#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577312.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1577312 loop_ _publ_author_name 'Fidelius, Jannis' 'Taube, Clemens' 'Schwedtmann, Kai' 'Hennersdorf, Felix' 'Gomila, Rosa Maria' 'Frontera, Antonio' 'Wolf, Robert' 'Weigand, Jan J.' _publ_section_title ; Imidazoliumyl-Substituted Di-and Iso-Tetraphosphanes and Their Metal-Mediated Fragmentation Reactions ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC02577C _journal_year 2026 _chemical_formula_moiety 'C70 H80 N4 P4 Pd2, 4(C H2 Cl2), 2(C F3 O3 S)' _chemical_formula_sum 'C76 H88 Cl8 F6 N4 O6 P4 Pd2 S2' _chemical_formula_weight 1951.90 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-07-26 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 100.7730(10) _cell_angle_beta 96.8500(10) _cell_angle_gamma 108.2840(10) _cell_formula_units_Z 2 _cell_length_a 14.2227(2) _cell_length_b 17.67070(10) _cell_length_c 18.94390(10) _cell_measurement_reflns_used 32283 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.6490 _cell_measurement_theta_min 2.3950 _cell_volume 4359.50(8) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2850 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 21.00 112.00 0.50 0.50 -- 42.50 38.00 -30.00 182 2 \w 94.00 140.00 0.50 2.00 -- 111.00 61.00 0.00 92 3 \w 106.00 139.00 0.50 2.00 -- 111.00 77.00 120.00 66 4 \w 41.00 125.00 0.50 2.00 -- 111.00 -45.00 60.00 168 5 \w 106.00 131.00 0.50 2.00 -- 111.00 -77.00 -30.00 50 6 \w 93.00 121.00 0.50 2.00 -- 111.00-125.00 30.00 56 7 \w 93.00 120.00 0.50 2.00 -- 111.00-125.00 90.00 54 8 \w 62.00 89.00 0.50 2.00 -- 111.00 -61.00 0.00 54 9 \w 51.00 102.00 0.50 2.00 -- 111.00-125.00 -30.00 102 10 \w 94.00 121.00 0.50 2.00 -- 111.00-125.00 -90.00 54 11 \w 80.00 134.00 0.50 2.00 -- 111.00 -61.00-180.00 108 12 \w 76.00 119.00 0.50 2.00 -- 111.00-125.00-180.00 86 13 \w 54.00 121.00 0.50 2.00 -- 111.00-125.00-150.00 134 14 \w 50.00 77.00 0.50 2.00 -- 111.00 -61.00-180.00 54 15 \w 44.00 131.00 0.50 2.00 -- 111.00 -45.00-180.00 174 16 \w 46.00 98.00 0.50 0.50 -- 42.50-125.00-120.00 104 17 \w 31.00 107.00 0.50 2.00 -- 111.00 -94.00-150.00 152 18 \w 39.00 86.00 0.50 2.00 -- 111.00 -77.00 -30.00 94 19 \w 49.00 121.00 0.50 2.00 -- 111.00-125.00 0.00 144 20 \w 62.00 88.00 0.50 2.00 -- 111.00 -94.00 120.00 52 21 \w 42.00 108.00 0.50 2.00 -- 111.00 -94.00 30.00 132 22 \w 40.00 68.00 0.50 2.00 -- 111.00-125.00 90.00 56 23 \w 31.00 101.00 0.50 2.00 -- 111.00 -94.00 90.00 140 24 \w 34.00 155.00 0.50 2.00 -- 111.00 -15.00 30.00 242 25 \w 34.00 154.00 0.50 2.00 -- 111.00 -15.00 150.00 240 26 \w 31.00 156.00 0.50 2.00 -- 111.00 -15.00 -90.00 250 27 \w -62.00 32.00 0.50 0.50 -- -38.50 57.00-150.00 188 28 \w -82.00 -5.00 0.50 0.50 -- -38.50 125.00 -30.00 154 29 \w -109.00 -12.00 0.50 0.50 -- -38.50 -57.00 60.00 194 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1054710000 _diffrn_orient_matrix_UB_12 0.0595239000 _diffrn_orient_matrix_UB_13 -0.0004709000 _diffrn_orient_matrix_UB_21 0.0447720000 _diffrn_orient_matrix_UB_22 -0.0259238000 _diffrn_orient_matrix_UB_23 0.0657384000 _diffrn_orient_matrix_UB_31 0.0193948000 _diffrn_orient_matrix_UB_32 -0.0687121000 _diffrn_orient_matrix_UB_33 -0.0528174000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 50554 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.732 _diffrn_reflns_theta_min 2.419 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.257 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_correction_T_min 0.313 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.487 _exptl_crystal_description block _exptl_crystal_F_000 1988 _exptl_crystal_size_max 0.213 _exptl_crystal_size_mid 0.178 _exptl_crystal_size_min 0.111 _refine_diff_density_max 1.416 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1067 _refine_ls_number_reflns 18157 _refine_ls_number_restraints 480 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0392 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+6.3455P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.1098 _reflns_Friedel_coverage 0.000 _reflns_number_gt 17199 _reflns_number_total 18157 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1091 _cod_database_code 1577312 _chemical_oxdiff_formula 'C152 H172 N8 O12 F12 P8 S4 Cl16 Pd4 ' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Cl6B-C75B \\sim C75B-Cl5B with sigma of 0.05 S2B-C72B \\sim S2A-C72A with sigma of 0.02 O5B-O6B \\sim O6B-O4B with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Cl7 \\sim Cl8A \\sim C76A: within 3A with sigma of 0.08 and sigma for terminal atoms of 0.01 Cl5A \\sim Cl6A \\sim C75A \\sim Cl5B \\sim Cl6B \\sim C75B: within 3A with sigma of 0.1 and sigma for terminal atoms of 0.01 S2A \\sim F4A \\sim F5A \\sim F6A \\sim O4A \\sim O5A \\sim O6A \\sim C72A \\sim S2B \\sim F4B \\sim F5B \\sim F6B \\sim O4B \\sim O5B \\sim O6B \\sim C72B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C76B) = Uanis(C76A) Uanis(O5B) = Uanis(O4B) = Uanis(O6B) = Uanis(O5A) = Uanis(O6A) = Uanis(O4A) 4. Rigid body (RIGU) restrains Cl7, Cl8A, Cl8B, C76A, C76B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 Cl5A, Cl6A, C75A, Cl5B, Cl6B, C75B with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 1 S2A, F4A, F5A, F6A, O4A, O5A, O6A, C72A, S2B, F4B, F5B, F6B, O4B, O5B, O6B, C72B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Same fragment restrains {Cl1, Cl2, C73} sigma for 1-2: 0.02, 1-3: 0.02 as {Cl7, Cl8A, C76A} 6. Others Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C72B)=1- FVAR(1) Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C72A)= FVAR(1) Fixed Sof: Cl5A(0.74) Cl6A(0.74) C75A(0.74) H75A(0.74) H75B(0.74) Cl5B(0.26) Cl6B(0.26) C75B(0.26) H75C(0.26) H75D(0.26) Cl8A(0.68) C76A(0.68) H76A(0.68) H76B(0.68) Cl8B(0.32) C76B(0.32) H76C(0.32) H76D(0.32) 7.a Ternary CH refined with riding coordinates: C2(H2), C9(H9), C19(H19), C26(H26) 7.b Secondary CH2 refined with riding coordinates: C73(H73A,H73B), C74(H74A,H74B), C75A(H75A,H75B), C75B(H75C,H75D), C76A(H76A, H76B), C76B(H76C,H76D) 7.c Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70) 7.d Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B, H28C) ; _shelx_res_file ; jjw1091.res created by SHELXL-2014/7 TITL jjw1091_a.res in P-1 REM Old TITL jjw1091 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.095, Rweak 0.007, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C75 N7 O4 F10 S Cl8 Pd2 CELL 1.54184 14.2227 17.6707 18.9439 100.773 96.85 108.284 ZERR 2 0.0002 0.0001 0.0001 0.001 0.001 0.001 LATT 1 SFAC C H Cl F N O P Pd S UNIT 152 176 16 12 8 12 8 4 4 SADI 0.05 Cl6B C75B C75B Cl5B SADI S2B C72B S2A C72A SADI O5B O6B O6B O4B SIMU 0.08 0.01 3 Cl7 Cl8A C76A SIMU 0.1 0.01 3 Cl5A > C75B SIMU S2A > C72B RIGU Cl7 Cl8A Cl8B C76A C76B RIGU 0.1 1 Cl5A Cl6A C75A Cl5B Cl6B C75B RIGU S2A F4A F5A F6A O4A O5A O6A C72A S2B F4B F5B F6B O4B O5B O6B C72B EADP C76B C76A EADP O5B O4B O6B O5A O6A O4A L.S. 10 PLAN 10 BOND $H LIST 6 MORE -1 CONF fmap 2 TEMP 100 acta OMIT 1 -1 3 REM REM REM WGHT 0.063800 6.345500 FVAR 0.26750 0.64300 PD1 8 0.274489 0.217358 0.217891 11.00000 0.01170 0.01361 = 0.01701 0.00348 0.00204 0.00282 PD2 8 0.452291 0.206811 0.223980 11.00000 0.01190 0.01399 = 0.01538 0.00424 0.00318 0.00319 P1 7 0.411445 0.315959 0.195222 11.00000 0.01597 0.01299 = 0.01709 0.00408 0.00296 0.00245 P2 7 0.312731 0.104744 0.239622 11.00000 0.01391 0.01440 = 0.01752 0.00538 0.00325 0.00277 P3 7 0.594414 0.176627 0.204113 11.00000 0.01350 0.01730 = 0.01717 0.00363 0.00340 0.00507 P4 7 0.115021 0.219813 0.183899 11.00000 0.01279 0.01824 = 0.02241 0.00294 0.00060 0.00405 N1 5 0.568463 0.472022 0.243572 11.00000 0.02015 0.01542 = 0.01848 0.00400 0.00537 0.00201 N2 5 0.444349 0.463581 0.302502 11.00000 0.01922 0.01502 = 0.01739 0.00262 0.00295 0.00332 N3 5 0.362703 0.081321 0.382313 11.00000 0.01823 0.01872 = 0.01958 0.00789 0.00385 0.00559 N4 5 0.207483 0.008461 0.329498 11.00000 0.01838 0.02095 = 0.02411 0.00936 0.00521 0.00286 C1 1 0.476366 0.422363 0.248585 11.00000 0.01912 0.01521 = 0.01729 0.00484 0.00265 0.00388 C2 1 0.632718 0.445749 0.194710 11.00000 0.02298 0.01738 = 0.02126 0.00320 0.00841 0.00474 AFIX 13 H2 2 0.591995 0.390972 0.164630 11.00000 -1.20000 AFIX 0 C3 1 0.723126 0.436947 0.239084 11.00000 0.02473 0.02728 = 0.03032 0.00601 0.00723 0.00788 AFIX 137 H3A 2 0.767879 0.490121 0.266537 11.00000 -1.50000 H3B 2 0.757973 0.412200 0.206693 11.00000 -1.50000 H3C 2 0.700745 0.402948 0.272105 11.00000 -1.50000 AFIX 0 C4 1 0.662205 0.501020 0.142150 11.00000 0.03853 0.02658 = 0.02643 0.01047 0.01586 0.00946 AFIX 137 H4A 2 0.603829 0.510758 0.120528 11.00000 -1.50000 H4B 2 0.688819 0.474755 0.104371 11.00000 -1.50000 H4C 2 0.712521 0.552328 0.168479 11.00000 -1.50000 AFIX 0 C5 1 0.594326 0.545949 0.294792 11.00000 0.02352 0.01556 = 0.02036 0.00292 0.00335 0.00341 C6 1 0.687510 0.618063 0.303171 11.00000 0.02754 0.01754 = 0.02903 0.00090 0.00926 -0.00174 AFIX 137 H6A 2 0.745614 0.601903 0.311115 11.00000 -1.50000 H6B 2 0.690655 0.660467 0.344246 11.00000 -1.50000 H6C 2 0.686298 0.638283 0.259552 11.00000 -1.50000 AFIX 0 C7 1 0.517006 0.540376 0.332287 11.00000 0.02147 0.01662 = 0.02124 0.00380 0.00361 0.00233 C8 1 0.509758 0.603360 0.393674 11.00000 0.02615 0.02089 = 0.02621 -0.00183 0.00711 0.00138 AFIX 137 H8A 2 0.463453 0.628259 0.376164 11.00000 -1.50000 H8B 2 0.575069 0.644643 0.412702 11.00000 -1.50000 H8C 2 0.486080 0.577774 0.431724 11.00000 -1.50000 AFIX 0 C9 1 0.348728 0.427183 0.327706 11.00000 0.01752 0.01787 = 0.02090 0.00342 0.00431 0.00200 AFIX 13 H9 2 0.308027 0.378295 0.289360 11.00000 -1.20000 AFIX 0 C10 1 0.370891 0.397476 0.396025 11.00000 0.02561 0.02649 = 0.02921 0.01239 0.01087 0.00859 AFIX 137 H10A 2 0.407943 0.360874 0.386474 11.00000 -1.50000 H10B 2 0.308583 0.369139 0.409327 11.00000 -1.50000 H10C 2 0.410147 0.443651 0.435421 11.00000 -1.50000 AFIX 0 C11 1 0.286608 0.483516 0.335926 11.00000 0.02273 0.02684 = 0.03077 0.00793 0.00580 0.00957 AFIX 137 H11A 2 0.314771 0.524942 0.380819 11.00000 -1.50000 H11B 2 0.218295 0.451964 0.336698 11.00000 -1.50000 H11C 2 0.287626 0.509128 0.295439 11.00000 -1.50000 AFIX 0 C12 1 0.393950 0.330331 0.102888 11.00000 0.02200 0.01840 = 0.01835 0.00506 0.00230 0.00344 C13 1 0.363536 0.259938 0.045302 11.00000 0.02024 0.01803 = 0.02210 0.00426 0.00219 0.00345 AFIX 43 H13 2 0.355307 0.209008 0.055475 11.00000 -1.20000 AFIX 0 C14 1 0.345605 0.265820 -0.026926 11.00000 0.03164 0.02602 = 0.01972 0.00073 0.00063 0.00558 AFIX 43 H14 2 0.326051 0.218902 -0.064803 11.00000 -1.20000 AFIX 0 C15 1 0.356794 0.341572 -0.042751 11.00000 0.04713 0.03196 = 0.01975 0.00816 -0.00075 0.00426 AFIX 43 H15 2 0.345545 0.345505 -0.091092 11.00000 -1.20000 AFIX 0 C16 1 0.384844 0.411263 0.014023 11.00000 0.06015 0.02214 = 0.02617 0.01038 0.00030 0.00581 AFIX 43 H16 2 0.391373 0.461875 0.003660 11.00000 -1.20000 AFIX 0 C17 1 0.403242 0.405769 0.086370 11.00000 0.04411 0.01651 = 0.02260 0.00500 -0.00042 0.00345 AFIX 43 H17 2 0.421894 0.452784 0.124047 11.00000 -1.20000 AFIX 0 C18 1 0.294285 0.062284 0.320241 11.00000 0.01632 0.01629 = 0.02155 0.00624 0.00507 0.00402 C19 1 0.467930 0.139902 0.394606 11.00000 0.01459 0.02142 = 0.02088 0.00800 0.00324 0.00365 AFIX 13 H19 2 0.479392 0.151319 0.347073 11.00000 -1.20000 AFIX 0 C20 1 0.545621 0.102452 0.419121 11.00000 0.02102 0.02919 = 0.02647 0.01132 0.00483 0.01072 AFIX 137 H20A 2 0.549887 0.104069 0.470372 11.00000 -1.50000 H20B 2 0.610284 0.133165 0.410586 11.00000 -1.50000 H20C 2 0.525596 0.046548 0.391838 11.00000 -1.50000 AFIX 0 C21 1 0.478842 0.221262 0.445146 11.00000 0.02302 0.02014 = 0.03185 0.00407 0.00600 0.00389 AFIX 137 H21A 2 0.431000 0.243159 0.424664 11.00000 -1.50000 H21B 2 0.545944 0.259235 0.450388 11.00000 -1.50000 H21C 2 0.466463 0.212698 0.492255 11.00000 -1.50000 AFIX 0 C22 1 0.319272 0.039982 0.431714 11.00000 0.02195 0.02330 = 0.02427 0.01220 0.00801 0.00752 C23 1 0.370778 0.045553 0.506777 11.00000 0.02871 0.03490 = 0.02467 0.01627 0.00608 0.01069 AFIX 137 H23A 2 0.418791 0.017715 0.503502 11.00000 -1.50000 H23B 2 0.321663 0.020367 0.533726 11.00000 -1.50000 H23C 2 0.405049 0.102163 0.531443 11.00000 -1.50000 AFIX 0 C24 1 0.222507 -0.006527 0.398509 11.00000 0.02446 0.02477 = 0.02571 0.01204 0.00816 0.00711 C25 1 0.145894 -0.065542 0.427854 11.00000 0.02972 0.03377 = 0.03822 0.02033 0.01248 0.00278 AFIX 137 H25A 2 0.081608 -0.059164 0.416529 11.00000 -1.50000 H25B 2 0.166125 -0.054774 0.479977 11.00000 -1.50000 H25C 2 0.140720 -0.120608 0.405913 11.00000 -1.50000 AFIX 0 C26 1 0.110304 -0.019486 0.276533 11.00000 0.01787 0.02424 = 0.02619 0.00699 0.00247 -0.00095 AFIX 13 H26 2 0.125377 0.000982 0.233044 11.00000 -1.20000 AFIX 0 C27 1 0.065078 -0.113220 0.251483 11.00000 0.02680 0.02687 = 0.04479 0.00486 0.00448 -0.00304 AFIX 137 H27A 2 0.116462 -0.134650 0.238308 11.00000 -1.50000 H27B 2 0.011599 -0.128540 0.209856 11.00000 -1.50000 H27C 2 0.038835 -0.135206 0.290588 11.00000 -1.50000 AFIX 0 C28 1 0.037220 0.018951 0.307059 11.00000 0.02040 0.03567 = 0.02939 0.00959 0.00463 0.00480 AFIX 137 H28A 2 0.018343 -0.001381 0.348765 11.00000 -1.50000 H28B 2 -0.021888 0.004967 0.270146 11.00000 -1.50000 H28C 2 0.069101 0.077517 0.321522 11.00000 -1.50000 AFIX 0 C29 1 0.281744 0.012376 0.167619 11.00000 0.01444 0.02109 = 0.02155 0.00368 0.00315 0.00477 C30 1 0.285302 -0.062604 0.179242 11.00000 0.02440 0.02145 = 0.02709 0.00401 0.00087 0.00631 AFIX 43 H30 2 0.299520 -0.068234 0.226793 11.00000 -1.20000 AFIX 0 C31 1 0.267819 -0.128907 0.120501 11.00000 0.03062 0.02105 = 0.04026 -0.00044 0.00118 0.00991 AFIX 43 H31 2 0.270348 -0.178540 0.128771 11.00000 -1.20000 AFIX 0 C32 1 0.246529 -0.120560 0.049310 11.00000 0.03067 0.03258 = 0.03228 -0.00991 0.00062 0.00982 AFIX 43 H32 2 0.234714 -0.164744 0.009906 11.00000 -1.20000 AFIX 0 C33 1 0.242911 -0.046778 0.037053 11.00000 0.02595 0.03940 = 0.02233 0.00089 0.00441 0.01115 AFIX 43 H33 2 0.227999 -0.041689 -0.010607 11.00000 -1.20000 AFIX 0 C34 1 0.261383 0.019747 0.095393 11.00000 0.01925 0.02780 = 0.02219 0.00597 0.00530 0.00837 AFIX 43 H34 2 0.260266 0.069528 0.086588 11.00000 -1.20000 AFIX 0 C35 1 0.662121 0.230768 0.142013 11.00000 0.01878 0.01685 = 0.01723 0.00283 0.00463 0.00496 C36 1 0.604512 0.247583 0.085987 11.00000 0.01760 0.02413 = 0.02150 0.00505 0.00334 0.00641 AFIX 43 H36 2 0.534699 0.229842 0.081168 11.00000 -1.20000 AFIX 0 C37 1 0.649617 0.290351 0.037296 11.00000 0.02736 0.02688 = 0.02070 0.00663 0.00291 0.01006 AFIX 43 H37 2 0.610353 0.301309 0.000334 11.00000 -1.20000 AFIX 0 C38 1 0.754143 0.316662 0.044336 11.00000 0.02775 0.02191 = 0.02287 0.00685 0.00925 0.00463 AFIX 43 H38 2 0.785170 0.345920 0.012421 11.00000 -1.20000 AFIX 0 C39 1 0.811701 0.299088 0.099046 11.00000 0.01830 0.02366 = 0.02586 0.00312 0.00737 0.00365 AFIX 43 H39 2 0.881408 0.316127 0.103221 11.00000 -1.20000 AFIX 0 C40 1 0.766702 0.256338 0.147786 11.00000 0.01750 0.02113 = 0.02153 0.00371 0.00272 0.00498 AFIX 43 H40 2 0.806182 0.244779 0.184191 11.00000 -1.20000 AFIX 0 C41 1 0.687804 0.199895 0.287249 11.00000 0.01573 0.02016 = 0.02137 0.00701 0.00592 0.00399 C42 1 0.694801 0.264746 0.344608 11.00000 0.02104 0.02283 = 0.02175 0.00575 0.00526 0.00640 AFIX 43 H42 2 0.653811 0.296006 0.339118 11.00000 -1.20000 AFIX 0 C43 1 0.762547 0.283238 0.410080 11.00000 0.02527 0.02670 = 0.02036 0.00257 0.00238 0.00433 AFIX 43 H43 2 0.766600 0.326718 0.447965 11.00000 -1.20000 AFIX 0 C44 1 0.823821 0.237134 0.418931 11.00000 0.01815 0.03499 = 0.02506 0.00726 -0.00195 0.00273 AFIX 43 H44 2 0.868818 0.249451 0.462771 11.00000 -1.20000 AFIX 0 C45 1 0.818025 0.172306 0.362144 11.00000 0.01843 0.03199 = 0.03239 0.01051 0.00159 0.00903 AFIX 43 H45 2 0.859442 0.141442 0.367916 11.00000 -1.20000 AFIX 0 C46 1 0.750451 0.153667 0.296870 11.00000 0.01772 0.02766 = 0.02404 0.00417 0.00376 0.00802 AFIX 43 H46 2 0.746671 0.110117 0.259156 11.00000 -1.20000 AFIX 0 C47 1 0.573897 0.068971 0.163506 11.00000 0.01453 0.02137 = 0.02245 0.00218 0.00142 0.00630 C48 1 0.589955 0.042474 0.093165 11.00000 0.02142 0.02416 = 0.02371 0.00234 0.00289 0.00751 AFIX 43 H48 2 0.613095 0.080215 0.065382 11.00000 -1.20000 AFIX 0 C49 1 0.571234 -0.040520 0.064804 11.00000 0.02667 0.02653 = 0.02867 -0.00333 0.00256 0.00881 AFIX 43 H49 2 0.581287 -0.057961 0.017764 11.00000 -1.20000 AFIX 0 C50 1 0.537829 -0.097502 0.105690 11.00000 0.02511 0.02093 = 0.03729 -0.00237 -0.00055 0.00797 AFIX 43 H50 2 0.526326 -0.152752 0.086515 11.00000 -1.20000 AFIX 0 C51 1 0.521699 -0.071462 0.175422 11.00000 0.02870 0.02088 = 0.03691 0.00838 0.00557 0.00745 AFIX 43 H51 2 0.499444 -0.109337 0.203254 11.00000 -1.20000 AFIX 0 C52 1 0.538726 0.011247 0.203908 11.00000 0.02697 0.02310 = 0.02729 0.00538 0.00672 0.00943 AFIX 43 H52 2 0.526495 0.028120 0.250372 11.00000 -1.20000 AFIX 0 C53 1 0.095714 0.260566 0.103817 11.00000 0.01870 0.02743 = 0.02849 0.00789 0.00225 0.00763 C54 1 0.021746 0.215668 0.041659 11.00000 0.02294 0.03168 = 0.02471 0.00413 0.00227 0.00669 AFIX 43 H54 2 -0.020547 0.162960 0.040193 11.00000 -1.20000 AFIX 0 C55 1 0.011383 0.249990 -0.018233 11.00000 0.03370 0.05165 = 0.02778 0.01215 -0.00079 0.00925 AFIX 43 H55 2 -0.037023 0.219586 -0.059876 11.00000 -1.20000 AFIX 0 C56 1 0.072374 0.328551 -0.016014 11.00000 0.04128 0.06464 = 0.04627 0.03485 0.00007 0.01126 AFIX 43 H56 2 0.065156 0.350917 -0.056178 11.00000 -1.20000 AFIX 0 C57 1 0.145031 0.374739 0.046357 11.00000 0.03874 0.04617 = 0.06128 0.03378 -0.00889 -0.00121 AFIX 43 H57 2 0.184843 0.428372 0.048370 11.00000 -1.20000 AFIX 0 C58 1 0.157597 0.340310 0.105313 11.00000 0.02648 0.03440 = 0.04535 0.01896 -0.00817 0.00074 AFIX 43 H58 2 0.207540 0.370431 0.146187 11.00000 -1.20000 AFIX 0 C59 1 0.014127 0.119509 0.158905 11.00000 0.01674 0.01993 = 0.02113 0.00271 0.00076 0.00493 C60 1 -0.080783 0.106311 0.177703 11.00000 0.01731 0.02281 = 0.02215 0.00274 0.00215 0.00551 AFIX 43 H60 2 -0.094623 0.149333 0.205626 11.00000 -1.20000 AFIX 0 C61 1 -0.154758 0.028547 0.154549 11.00000 0.01746 0.02870 = 0.02411 0.00487 0.00206 0.00260 AFIX 43 H61 2 -0.217876 0.019790 0.167173 11.00000 -1.20000 AFIX 0 C62 1 -0.134589 -0.035710 0.112815 11.00000 0.02361 0.02289 = 0.02691 0.00273 -0.00001 -0.00130 AFIX 43 H62 2 -0.184090 -0.087497 0.097598 11.00000 -1.20000 AFIX 0 C63 1 -0.040630 -0.022875 0.093708 11.00000 0.03027 0.02220 = 0.02979 -0.00088 0.00508 0.00775 AFIX 43 H63 2 -0.027302 -0.065881 0.065300 11.00000 -1.20000 AFIX 0 C64 1 0.033304 0.054114 0.117016 11.00000 0.01947 0.02545 = 0.02931 0.00179 0.00603 0.00632 AFIX 43 H64 2 0.096466 0.062304 0.104596 11.00000 -1.20000 AFIX 0 C65 1 0.075262 0.281471 0.254912 11.00000 0.01399 0.02030 = 0.02804 0.00118 -0.00030 0.00356 C66 1 0.026297 0.336029 0.240351 11.00000 0.02324 0.03022 = 0.03250 -0.00043 -0.00606 0.01352 AFIX 43 H66 2 0.013969 0.342764 0.193004 11.00000 -1.20000 AFIX 0 C67 1 -0.003928 0.380175 0.296692 11.00000 0.02317 0.03150 = 0.04465 -0.00242 -0.00327 0.01468 AFIX 43 H67 2 -0.036819 0.415980 0.286642 11.00000 -1.20000 AFIX 0 C68 1 0.014469 0.371241 0.366990 11.00000 0.02047 0.02827 = 0.04073 -0.00477 0.00726 0.00665 AFIX 43 H68 2 -0.006065 0.400839 0.404284 11.00000 -1.20000 AFIX 0 C69 1 0.063817 0.317903 0.382325 11.00000 0.02318 0.02586 = 0.03131 0.00202 0.00704 0.00333 AFIX 43 H69 2 0.076442 0.311998 0.429935 11.00000 -1.20000 AFIX 0 C70 1 0.094348 0.273344 0.326574 11.00000 0.01768 0.02144 = 0.03056 0.00448 0.00510 0.00463 AFIX 43 H70 2 0.127642 0.237970 0.337141 11.00000 -1.20000 AFIX 0 CL1 3 0.865610 0.513255 0.431799 11.00000 0.03975 0.06826 = 0.05096 -0.00995 0.00936 0.01875 CL2 3 0.650269 0.444323 0.438753 11.00000 0.03769 0.03522 = 0.03635 -0.00122 0.00575 0.01477 C73 1 0.767482 0.523633 0.473172 11.00000 0.05331 0.02901 = 0.06914 -0.00391 0.03383 0.00223 AFIX 23 H73A 2 0.759399 0.575048 0.468365 11.00000 -1.20000 H73B 2 0.785874 0.527320 0.525004 11.00000 -1.20000 AFIX 0 CL3 3 0.229843 0.185281 -0.231367 11.00000 0.06578 0.04187 = 0.03990 0.01065 0.01607 0.00719 CL4 3 0.251403 0.042077 -0.323653 11.00000 0.07644 0.04342 = 0.04165 0.01702 0.02188 0.01598 C74 1 0.300771 0.150015 -0.291745 11.00000 0.04343 0.04514 = 0.04106 0.02116 0.00792 0.00682 AFIX 23 H74A 2 0.370194 0.166519 -0.266702 11.00000 -1.20000 H74B 2 0.300229 0.175079 -0.333116 11.00000 -1.20000 AFIX 0 PART 1 CL5A 3 0.279275 -0.266323 0.403973 10.74000 0.12974 0.15390 = 0.09514 0.03110 0.01827 -0.00168 CL6A 3 0.398849 -0.132862 0.345159 10.74000 0.09561 0.06555 = 0.05488 0.01255 -0.00616 0.02277 C75A 1 0.297371 -0.224707 0.326461 10.74000 0.09732 0.10379 = 0.05682 -0.00131 0.01773 0.04130 AFIX 23 H75A 2 0.308340 -0.264406 0.288480 10.74000 -1.20000 H75B 2 0.236461 -0.215394 0.307781 10.74000 -1.20000 AFIX 0 PART 0 PART 2 CL5B 3 0.295193 -0.286522 0.388462 10.26000 0.10294 0.07399 = 0.08164 0.00598 0.02186 0.04823 CL6B 3 0.341694 -0.136466 0.361922 10.26000 0.12098 0.09874 = 0.08626 0.02825 0.00918 0.04479 C75B 1 0.368310 -0.201324 0.334455 10.26000 0.09772 0.08797 = 0.06299 0.00377 0.02473 0.02962 AFIX 23 H75C 2 0.440809 -0.188113 0.345592 10.26000 -1.20000 H75D 2 0.344927 -0.220458 0.281896 10.26000 -1.20000 AFIX 0 SAME 0.02 0.02 Cl1 Cl2 C73 PART 0 CL7 3 -0.029926 0.508829 0.146760 11.00000 0.11367 0.08045 = 0.15202 0.02714 0.02129 0.01652 PART 1 CL8A 3 0.014912 0.639084 0.278163 10.68000 0.13429 0.22120 = 0.22694 -0.00364 0.03213 0.00512 C76A 1 0.058780 0.594566 0.200572 10.68000 0.13143 0.13567 = 0.21203 0.01098 0.02163 -0.00054 AFIX 23 H76A 2 0.079525 0.634666 0.171686 10.68000 -1.20000 H76B 2 0.117365 0.581501 0.218071 10.68000 -1.20000 AFIX 0 PART 0 PART 2 CL8B 3 0.010489 0.668133 0.229929 10.32000 0.41537 0.08443 = 0.18404 -0.04016 -0.09097 0.10316 C76B 1 0.076921 0.581307 0.236504 10.32000 0.13143 0.13567 = 0.21203 0.01098 0.02163 -0.00054 AFIX 23 H76C 2 0.145514 0.596839 0.227852 10.32000 -1.20000 H76D 2 0.071614 0.560629 0.280369 10.32000 -1.20000 AFIX 0 PART 0 S1 9 0.223928 0.215901 0.501268 11.00000 0.02030 0.02271 = 0.02391 0.00539 0.00450 0.00282 F1 4 0.099302 0.190643 0.592877 11.00000 0.03834 0.07053 = 0.04072 0.01162 0.02100 0.00505 F2 4 0.088283 0.081586 0.514587 11.00000 0.04285 0.03623 = 0.06801 0.02120 0.01415 -0.00320 F3 4 0.025802 0.167766 0.480937 11.00000 0.02219 0.06452 = 0.05753 0.02237 0.00398 0.00533 O1 6 0.215213 0.177925 0.425476 11.00000 0.03234 0.03342 = 0.02505 0.00399 0.00437 0.00963 O2 6 0.225780 0.299470 0.515080 11.00000 0.03348 0.02387 = 0.03551 0.00543 0.00585 0.00564 O3 6 0.295969 0.201289 0.552615 11.00000 0.02568 0.03452 = 0.02783 0.00949 0.00371 0.00760 C71 1 0.102903 0.160945 0.523414 11.00000 0.02475 0.03601 = 0.03615 0.01056 0.00698 0.00166 PART 1 S2A 9 0.318156 0.616846 0.145272 21.00000 0.04106 0.02741 = 0.03134 0.01370 0.00703 0.00765 F4A 4 0.472224 0.702508 0.254333 21.00000 0.06487 0.05175 = 0.03713 0.00645 0.00457 0.00180 F5A 4 0.503277 0.612809 0.168722 21.00000 0.05045 0.05287 = 0.06550 0.02992 0.01616 0.02565 F6A 4 0.492671 0.727286 0.147654 21.00000 0.05811 0.02926 = 0.04502 0.01619 0.01433 0.00397 O4A 6 0.320619 0.581068 0.068813 21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 O5A 6 0.287442 0.558985 0.189813 21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 O6A 6 0.280967 0.685330 0.157990 21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 C72A 1 0.456087 0.664738 0.187563 21.00000 0.01505 0.01413 = 0.00576 -0.00316 -0.00318 0.00287 PART 0 PART 2 S2B 9 0.444692 0.659027 0.177512 -21.00000 0.11719 0.06028 = 0.09791 0.02412 -0.01160 0.02463 F4B 4 0.306239 0.583728 0.071451 -21.00000 0.05706 0.02830 = 0.04091 0.00906 -0.00047 0.00714 F5B 4 0.278545 0.544025 0.168710 -21.00000 0.09660 0.07190 = 0.07794 0.03482 0.02492 0.00062 F6B 4 0.265892 0.662164 0.155419 -21.00000 0.06332 0.09716 = 0.11070 0.02934 0.02951 0.04029 O4B 6 0.484301 0.728105 0.165548 -21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 O5B 6 0.490559 0.605651 0.181425 -21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 O6B 6 0.443749 0.682958 0.262189 -21.00000 0.07168 0.05757 = 0.05149 0.02122 0.00839 0.01801 C72B 1 0.301392 0.590788 0.145365 -21.00000 0.09127 0.07460 = 0.05060 0.02636 0.01994 0.02590 HKLF 4 REM jjw1091_a.res in P-1 REM R1 = 0.0392 for 17199 Fo > 4sig(Fo) and 0.0412 for all 18157 data REM 1067 parameters refined using 480 restraints END WGHT 0.0638 6.3455 REM Highest difference peak 1.416, deepest hole -1.533, 1-sigma level 0.100 Q1 1 0.3649 -0.1878 0.3263 11.00000 0.05 1.42 Q2 1 0.4936 0.6550 0.1392 11.00000 0.05 1.26 Q3 1 0.1244 0.5978 0.3995 11.00000 0.05 1.25 Q4 1 0.2618 -0.3365 0.3344 11.00000 0.05 1.11 Q5 1 -0.0178 0.4921 0.0525 11.00000 0.05 1.08 Q6 1 0.0194 0.6907 0.3869 11.00000 0.05 0.98 Q7 1 0.4539 -0.2123 0.3417 11.00000 0.05 0.93 Q8 1 0.0000 0.5000 0.0000 10.50000 0.05 0.86 Q9 1 -0.0131 0.5763 0.1790 11.00000 0.05 0.76 Q10 1 -0.0639 0.6760 0.2281 11.00000 0.05 0.70 ; _shelx_res_checksum 23033 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.836 _oxdiff_exptl_absorpt_empirical_full_min 0.833 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.27449(2) 0.21736(2) 0.21789(2) 0.01457(6) Uani 1 1 d . . . . . Pd2 Pd 0.45229(2) 0.20681(2) 0.22398(2) 0.01391(6) Uani 1 1 d . . . . . P1 P 0.41145(5) 0.31596(4) 0.19522(3) 0.01592(12) Uani 1 1 d . . . . . P2 P 0.31273(5) 0.10474(4) 0.23962(3) 0.01555(12) Uani 1 1 d . . . . . P3 P 0.59441(5) 0.17663(4) 0.20411(3) 0.01607(12) Uani 1 1 d . . . . . P4 P 0.11502(5) 0.21981(4) 0.18390(4) 0.01864(13) Uani 1 1 d . . . . . N1 N 0.56846(17) 0.47202(13) 0.24357(12) 0.0189(4) Uani 1 1 d . . . . . N2 N 0.44435(17) 0.46358(13) 0.30250(12) 0.0181(4) Uani 1 1 d . . . . . N3 N 0.36270(17) 0.08132(13) 0.38231(12) 0.0185(4) Uani 1 1 d . . . . . N4 N 0.20748(18) 0.00846(14) 0.32950(13) 0.0214(4) Uani 1 1 d . . . . . C1 C 0.4764(2) 0.42236(15) 0.24858(14) 0.0176(5) Uani 1 1 d . . . . . C2 C 0.6327(2) 0.44575(16) 0.19471(15) 0.0209(5) Uani 1 1 d . . . . . H2 H 0.5920 0.3910 0.1646 0.025 Uiso 1 1 calc R . . . . C3 C 0.7231(2) 0.43695(19) 0.23908(17) 0.0276(6) Uani 1 1 d . . . . . H3A H 0.7679 0.4901 0.2665 0.041 Uiso 1 1 calc GR . . . . H3B H 0.7580 0.4122 0.2067 0.041 Uiso 1 1 calc GR . . . . H3C H 0.7007 0.4029 0.2721 0.041 Uiso 1 1 calc GR . . . . C4 C 0.6622(3) 0.50102(19) 0.14215(17) 0.0295(6) Uani 1 1 d . . . . . H4A H 0.6038 0.5108 0.1205 0.044 Uiso 1 1 calc GR . . . . H4B H 0.6888 0.4748 0.1044 0.044 Uiso 1 1 calc GR . . . . H4C H 0.7125 0.5523 0.1685 0.044 Uiso 1 1 calc GR . . . . C5 C 0.5943(2) 0.54595(16) 0.29479(15) 0.0209(5) Uani 1 1 d . . . . . C6 C 0.6875(2) 0.61806(17) 0.30317(17) 0.0273(6) Uani 1 1 d . . . . . H6A H 0.7456 0.6019 0.3111 0.041 Uiso 1 1 calc GR . . . . H6B H 0.6907 0.6605 0.3442 0.041 Uiso 1 1 calc GR . . . . H6C H 0.6863 0.6383 0.2596 0.041 Uiso 1 1 calc GR . . . . C7 C 0.5170(2) 0.54038(16) 0.33229(15) 0.0209(5) Uani 1 1 d . . . . . C8 C 0.5098(2) 0.60336(17) 0.39367(16) 0.0269(6) Uani 1 1 d . . . . . H8A H 0.4635 0.6283 0.3762 0.040 Uiso 1 1 calc GR . . . . H8B H 0.5751 0.6446 0.4127 0.040 Uiso 1 1 calc GR . . . . H8C H 0.4861 0.5778 0.4317 0.040 Uiso 1 1 calc GR . . . . C9 C 0.3487(2) 0.42718(16) 0.32771(14) 0.0199(5) Uani 1 1 d . . . . . H9 H 0.3080 0.3783 0.2894 0.024 Uiso 1 1 calc R . . . . C10 C 0.3709(2) 0.39748(18) 0.39602(16) 0.0259(6) Uani 1 1 d . . . . . H10A H 0.4079 0.3609 0.3865 0.039 Uiso 1 1 calc GR . . . . H10B H 0.3086 0.3691 0.4093 0.039 Uiso 1 1 calc GR . . . . H10C H 0.4101 0.4437 0.4354 0.039 Uiso 1 1 calc GR . . . . C11 C 0.2866(2) 0.48352(18) 0.33593(17) 0.0263(6) Uani 1 1 d . . . . . H11A H 0.3148 0.5249 0.3808 0.039 Uiso 1 1 calc GR . . . . H11B H 0.2183 0.4520 0.3367 0.039 Uiso 1 1 calc GR . . . . H11C H 0.2876 0.5091 0.2954 0.039 Uiso 1 1 calc GR . . . . C12 C 0.3940(2) 0.33033(16) 0.10289(14) 0.0205(5) Uani 1 1 d . . . . . C13 C 0.3635(2) 0.25994(16) 0.04530(15) 0.0211(5) Uani 1 1 d . . . . . H13 H 0.3553 0.2090 0.0555 0.025 Uiso 1 1 calc R . . . . C14 C 0.3456(2) 0.26582(18) -0.02693(16) 0.0279(6) Uani 1 1 d . . . . . H14 H 0.3261 0.2189 -0.0648 0.033 Uiso 1 1 calc R . . . . C15 C 0.3568(3) 0.3416(2) -0.04275(17) 0.0356(7) Uani 1 1 d . . . . . H15 H 0.3455 0.3455 -0.0911 0.043 Uiso 1 1 calc R . . . . C16 C 0.3848(3) 0.4113(2) 0.01402(18) 0.0382(8) Uani 1 1 d . . . . . H16 H 0.3914 0.4619 0.0037 0.046 Uiso 1 1 calc R . . . . C17 C 0.4032(3) 0.40577(17) 0.08637(16) 0.0300(6) Uani 1 1 d . . . . . H17 H 0.4219 0.4528 0.1240 0.036 Uiso 1 1 calc R . . . . C18 C 0.29428(19) 0.06228(15) 0.32024(14) 0.0181(5) Uani 1 1 d . . . . . C19 C 0.46793(19) 0.13990(16) 0.39461(14) 0.0192(5) Uani 1 1 d . . . . . H19 H 0.4794 0.1513 0.3471 0.023 Uiso 1 1 calc R . . . . C20 C 0.5456(2) 0.10245(18) 0.41912(16) 0.0244(5) Uani 1 1 d . . . . . H20A H 0.5499 0.1041 0.4704 0.037 Uiso 1 1 calc GR . . . . H20B H 0.6103 0.1332 0.4106 0.037 Uiso 1 1 calc GR . . . . H20C H 0.5256 0.0465 0.3918 0.037 Uiso 1 1 calc GR . . . . C21 C 0.4788(2) 0.22126(17) 0.44515(17) 0.0261(6) Uani 1 1 d . . . . . H21A H 0.4310 0.2432 0.4247 0.039 Uiso 1 1 calc GR . . . . H21B H 0.5459 0.2592 0.4504 0.039 Uiso 1 1 calc GR . . . . H21C H 0.4665 0.2127 0.4923 0.039 Uiso 1 1 calc GR . . . . C22 C 0.3193(2) 0.03998(17) 0.43171(15) 0.0220(5) Uani 1 1 d . . . . . C23 C 0.3708(2) 0.0456(2) 0.50678(16) 0.0281(6) Uani 1 1 d . . . . . H23A H 0.4188 0.0177 0.5035 0.042 Uiso 1 1 calc GR . . . . H23B H 0.3217 0.0204 0.5337 0.042 Uiso 1 1 calc GR . . . . H23C H 0.4050 0.1022 0.5314 0.042 Uiso 1 1 calc GR . . . . C24 C 0.2225(2) -0.00653(17) 0.39851(16) 0.0242(5) Uani 1 1 d . . . . . C25 C 0.1459(3) -0.0655(2) 0.42785(19) 0.0337(7) Uani 1 1 d . . . . . H25A H 0.0816 -0.0592 0.4165 0.051 Uiso 1 1 calc GR . . . . H25B H 0.1661 -0.0548 0.4800 0.051 Uiso 1 1 calc GR . . . . H25C H 0.1407 -0.1206 0.4059 0.051 Uiso 1 1 calc GR . . . . C26 C 0.1103(2) -0.01949(17) 0.27653(16) 0.0248(6) Uani 1 1 d . . . . . H26 H 0.1254 0.0010 0.2330 0.030 Uiso 1 1 calc R . . . . C27 C 0.0651(3) -0.1132(2) 0.2515(2) 0.0365(7) Uani 1 1 d . . . . . H27A H 0.1165 -0.1346 0.2383 0.055 Uiso 1 1 calc GR . . . . H27B H 0.0116 -0.1285 0.2099 0.055 Uiso 1 1 calc GR . . . . H27C H 0.0388 -0.1352 0.2906 0.055 Uiso 1 1 calc GR . . . . C28 C 0.0372(2) 0.0190(2) 0.30706(17) 0.0294(6) Uani 1 1 d . . . . . H28A H 0.0183 -0.0014 0.3488 0.044 Uiso 1 1 calc GR . . . . H28B H -0.0219 0.0050 0.2701 0.044 Uiso 1 1 calc GR . . . . H28C H 0.0691 0.0775 0.3215 0.044 Uiso 1 1 calc GR . . . . C29 C 0.28174(19) 0.01238(16) 0.16762(15) 0.0196(5) Uani 1 1 d . . . . . C30 C 0.2853(2) -0.06260(17) 0.17924(16) 0.0253(6) Uani 1 1 d . . . . . H30 H 0.2995 -0.0682 0.2268 0.030 Uiso 1 1 calc R . . . . C31 C 0.2678(2) -0.12891(19) 0.12050(19) 0.0320(6) Uani 1 1 d . . . . . H31 H 0.2703 -0.1785 0.1288 0.038 Uiso 1 1 calc R . . . . C32 C 0.2465(3) -0.1206(2) 0.04931(18) 0.0351(7) Uani 1 1 d . . . . . H32 H 0.2347 -0.1647 0.0099 0.042 Uiso 1 1 calc R . . . . C33 C 0.2429(2) -0.0468(2) 0.03705(17) 0.0302(6) Uani 1 1 d . . . . . H33 H 0.2280 -0.0417 -0.0106 0.036 Uiso 1 1 calc R . . . . C34 C 0.2614(2) 0.01975(18) 0.09539(15) 0.0229(5) Uani 1 1 d . . . . . H34 H 0.2603 0.0695 0.0866 0.027 Uiso 1 1 calc R . . . . C35 C 0.6621(2) 0.23077(15) 0.14201(14) 0.0180(5) Uani 1 1 d . . . . . C36 C 0.6045(2) 0.24758(17) 0.08599(15) 0.0214(5) Uani 1 1 d . . . . . H36 H 0.5347 0.2298 0.0812 0.026 Uiso 1 1 calc R . . . . C37 C 0.6496(2) 0.29035(18) 0.03730(15) 0.0248(5) Uani 1 1 d . . . . . H37 H 0.6104 0.3013 0.0003 0.030 Uiso 1 1 calc R . . . . C38 C 0.7541(2) 0.31666(17) 0.04434(15) 0.0245(5) Uani 1 1 d . . . . . H38 H 0.7852 0.3459 0.0124 0.029 Uiso 1 1 calc R . . . . C39 C 0.8117(2) 0.29909(17) 0.09905(16) 0.0236(5) Uani 1 1 d . . . . . H39 H 0.8814 0.3161 0.1032 0.028 Uiso 1 1 calc R . . . . C40 C 0.7667(2) 0.25634(16) 0.14779(15) 0.0207(5) Uani 1 1 d . . . . . H40 H 0.8062 0.2448 0.1842 0.025 Uiso 1 1 calc R . . . . C41 C 0.68780(19) 0.19989(16) 0.28725(15) 0.0191(5) Uani 1 1 d . . . . . C42 C 0.6948(2) 0.26475(17) 0.34461(15) 0.0220(5) Uani 1 1 d . . . . . H42 H 0.6538 0.2960 0.3391 0.026 Uiso 1 1 calc R . . . . C43 C 0.7625(2) 0.28324(18) 0.41008(15) 0.0258(6) Uani 1 1 d . . . . . H43 H 0.7666 0.3267 0.4480 0.031 Uiso 1 1 calc R . . . . C44 C 0.8238(2) 0.23713(19) 0.41893(16) 0.0282(6) Uani 1 1 d . . . . . H44 H 0.8688 0.2495 0.4628 0.034 Uiso 1 1 calc R . . . . C45 C 0.8180(2) 0.17231(19) 0.36214(17) 0.0274(6) Uani 1 1 d . . . . . H45 H 0.8594 0.1414 0.3679 0.033 Uiso 1 1 calc R . . . . C46 C 0.7505(2) 0.15367(18) 0.29687(16) 0.0234(5) Uani 1 1 d . . . . . H46 H 0.7467 0.1101 0.2592 0.028 Uiso 1 1 calc R . . . . C47 C 0.57390(19) 0.06897(16) 0.16351(15) 0.0200(5) Uani 1 1 d . . . . . C48 C 0.5900(2) 0.04247(17) 0.09317(16) 0.0238(5) Uani 1 1 d . . . . . H48 H 0.6131 0.0802 0.0654 0.029 Uiso 1 1 calc R . . . . C49 C 0.5712(2) -0.04052(19) 0.06480(17) 0.0290(6) Uani 1 1 d . . . . . H49 H 0.5813 -0.0580 0.0178 0.035 Uiso 1 1 calc R . . . . C50 C 0.5378(2) -0.09750(18) 0.10569(18) 0.0296(6) Uani 1 1 d . . . . . H50 H 0.5263 -0.1528 0.0865 0.036 Uiso 1 1 calc R . . . . C51 C 0.5217(2) -0.07146(18) 0.17542(18) 0.0289(6) Uani 1 1 d . . . . . H51 H 0.4994 -0.1093 0.2033 0.035 Uiso 1 1 calc R . . . . C52 C 0.5387(2) 0.01125(18) 0.20391(16) 0.0255(6) Uani 1 1 d . . . . . H52 H 0.5265 0.0281 0.2504 0.031 Uiso 1 1 calc R . . . . C53 C 0.0957(2) 0.26057(18) 0.10382(16) 0.0250(5) Uani 1 1 d . . . . . C54 C 0.0217(2) 0.21567(19) 0.04166(16) 0.0277(6) Uani 1 1 d . . . . . H54 H -0.0205 0.1630 0.0402 0.033 Uiso 1 1 calc R . . . . C55 C 0.0114(3) 0.2500(2) -0.01823(19) 0.0392(8) Uani 1 1 d . . . . . H55 H -0.0370 0.2196 -0.0599 0.047 Uiso 1 1 calc R . . . . C56 C 0.0724(3) 0.3286(3) -0.0160(2) 0.0501(10) Uani 1 1 d . . . . . H56 H 0.0652 0.3509 -0.0562 0.060 Uiso 1 1 calc R . . . . C57 C 0.1450(3) 0.3747(3) 0.0464(2) 0.0513(11) Uani 1 1 d . . . . . H57 H 0.1848 0.4284 0.0484 0.062 Uiso 1 1 calc R . . . . C58 C 0.1576(3) 0.3403(2) 0.1053(2) 0.0378(8) Uani 1 1 d . . . . . H58 H 0.2075 0.3704 0.1462 0.045 Uiso 1 1 calc R . . . . C59 C 0.0141(2) 0.11951(16) 0.15890(15) 0.0202(5) Uani 1 1 d . . . . . C60 C -0.0808(2) 0.10631(17) 0.17770(15) 0.0216(5) Uani 1 1 d . . . . . H60 H -0.0946 0.1493 0.2056 0.026 Uiso 1 1 calc R . . . . C61 C -0.1548(2) 0.02855(18) 0.15455(16) 0.0251(5) Uani 1 1 d . . . . . H61 H -0.2179 0.0198 0.1672 0.030 Uiso 1 1 calc R . . . . C62 C -0.1346(2) -0.03571(18) 0.11282(16) 0.0276(6) Uani 1 1 d . . . . . H62 H -0.1841 -0.0875 0.0976 0.033 Uiso 1 1 calc R . . . . C63 C -0.0406(2) -0.02287(18) 0.09371(17) 0.0288(6) Uani 1 1 d . . . . . H63 H -0.0273 -0.0659 0.0653 0.035 Uiso 1 1 calc R . . . . C64 C 0.0333(2) 0.05411(18) 0.11702(16) 0.0256(6) Uani 1 1 d . . . . . H64 H 0.0965 0.0623 0.1046 0.031 Uiso 1 1 calc R . . . . C65 C 0.0753(2) 0.28147(16) 0.25491(16) 0.0224(5) Uani 1 1 d . . . . . C66 C 0.0263(2) 0.33603(19) 0.24035(18) 0.0297(6) Uani 1 1 d . . . . . H66 H 0.0140 0.3428 0.1930 0.036 Uiso 1 1 calc R . . . . C67 C -0.0039(2) 0.3802(2) 0.2967(2) 0.0343(7) Uani 1 1 d . . . . . H67 H -0.0368 0.4160 0.2866 0.041 Uiso 1 1 calc R . . . . C68 C 0.0145(2) 0.37124(19) 0.36699(19) 0.0319(7) Uani 1 1 d . . . . . H68 H -0.0061 0.4008 0.4043 0.038 Uiso 1 1 calc R . . . . C69 C 0.0638(2) 0.31790(18) 0.38232(17) 0.0285(6) Uani 1 1 d . . . . . H69 H 0.0764 0.3120 0.4299 0.034 Uiso 1 1 calc R . . . . C70 C 0.0943(2) 0.27334(17) 0.32657(16) 0.0239(5) Uani 1 1 d . . . . . H70 H 0.1276 0.2380 0.3371 0.029 Uiso 1 1 calc R . . . . Cl1 Cl 0.86561(8) 0.51326(7) 0.43180(6) 0.0563(3) Uani 1 1 d D . . . . Cl2 Cl 0.65027(6) 0.44432(5) 0.43875(4) 0.03736(17) Uani 1 1 d D . . . . C73 C 0.7675(3) 0.5236(2) 0.4732(3) 0.0536(11) Uani 1 1 d D . . . . H73A H 0.7594 0.5750 0.4684 0.064 Uiso 1 1 calc R . . . . H73B H 0.7859 0.5273 0.5250 0.064 Uiso 1 1 calc R . . . . Cl3 Cl 0.22984(9) 0.18528(6) -0.23137(5) 0.0513(2) Uani 1 1 d . . . . . Cl4 Cl 0.25140(9) 0.04208(6) -0.32365(5) 0.0531(2) Uani 1 1 d . . . . . C74 C 0.3008(3) 0.1500(2) -0.2917(2) 0.0437(8) Uani 1 1 d . . . . . H74A H 0.3702 0.1665 -0.2667 0.052 Uiso 1 1 calc R . . . . H74B H 0.3002 0.1751 -0.3331 0.052 Uiso 1 1 calc R . . . . Cl5A Cl 0.2793(4) -0.2663(3) 0.4040(3) 0.1386(16) Uani 0.74 1 d . U P A 1 Cl6A Cl 0.3988(2) -0.13286(13) 0.34516(11) 0.0753(5) Uani 0.74 1 d . U P A 1 C75A C 0.2974(8) -0.2247(6) 0.3265(5) 0.087(2) Uani 0.74 1 d . U P A 1 H75A H 0.3083 -0.2644 0.2885 0.104 Uiso 0.74 1 calc R . P A 1 H75B H 0.2365 -0.2154 0.3078 0.104 Uiso 0.74 1 calc R . P A 1 Cl5B Cl 0.2952(9) -0.2865(6) 0.3885(6) 0.0833(17) Uani 0.26 1 d D U P B 2 Cl6B Cl 0.3417(8) -0.1365(5) 0.3619(5) 0.1004(18) Uani 0.26 1 d D U P B 2 C75B C 0.368(2) -0.2013(14) 0.3345(14) 0.085(3) Uani 0.26 1 d D U P B 2 H75C H 0.4408 -0.1881 0.3456 0.102 Uiso 0.26 1 calc R . P B 2 H75D H 0.3449 -0.2205 0.2819 0.102 Uiso 0.26 1 calc R . P B 2 Cl7 Cl -0.02993(19) 0.50883(13) 0.14676(15) 0.1199(7) Uani 1 1 d D U . . . Cl8A Cl 0.0149(5) 0.6391(5) 0.2782(4) 0.216(3) Uani 0.68 1 d D U P C 1 C76A C 0.0588(14) 0.5946(12) 0.2006(10) 0.176(5) Uani 0.68 1 d D U P C 1 H76A H 0.0795 0.6347 0.1717 0.212 Uiso 0.68 1 calc R . P C 1 H76B H 0.1174 0.5815 0.2181 0.212 Uiso 0.68 1 calc R . P C 1 Cl8B Cl 0.0105(15) 0.6681(6) 0.2299(8) 0.247(9) Uani 0.32 1 d . U P C 2 C76B C 0.077(4) 0.581(3) 0.237(3) 0.176(5) Uani 0.32 1 d . U P C 2 H76C H 0.1455 0.5968 0.2279 0.212 Uiso 0.32 1 calc R . P C 2 H76D H 0.0716 0.5606 0.2804 0.212 Uiso 0.32 1 calc R . P C 2 S1 S 0.22393(5) 0.21590(4) 0.50127(4) 0.02342(13) Uani 1 1 d . . . . . F1 F 0.09930(17) 0.19064(17) 0.59288(13) 0.0522(6) Uani 1 1 d . . . . . F2 F 0.08828(18) 0.08159(14) 0.51459(15) 0.0516(6) Uani 1 1 d . . . . . F3 F 0.02580(15) 0.16777(16) 0.48094(14) 0.0496(5) Uani 1 1 d . . . . . O1 O 0.21521(17) 0.17792(14) 0.42548(12) 0.0312(5) Uani 1 1 d . . . . . O2 O 0.22578(18) 0.29947(13) 0.51508(13) 0.0323(5) Uani 1 1 d . . . . . O3 O 0.29597(16) 0.20129(14) 0.55261(12) 0.0298(4) Uani 1 1 d . . . . . C71 C 0.1029(2) 0.1609(2) 0.52341(19) 0.0341(7) Uani 1 1 d . . . . . S2A S 0.31816(13) 0.61685(10) 0.14527(10) 0.0333(5) Uani 0.643(6) 1 d D U P D 1 F4A F 0.4722(4) 0.7025(3) 0.2543(3) 0.0567(12) Uani 0.643(6) 1 d . U P D 1 F5A F 0.5033(5) 0.6128(4) 0.1687(4) 0.0517(14) Uani 0.643(6) 1 d . U P D 1 F6A F 0.4927(5) 0.7273(3) 0.1477(3) 0.0454(11) Uani 0.643(6) 1 d . U P D 1 O4A O 0.3206(14) 0.5811(12) 0.0688(10) 0.0604(12) Uani 0.643(6) 1 d . U P D 1 O5A O 0.2874(9) 0.5590(6) 0.1898(5) 0.0604(12) Uani 0.643(6) 1 d . U P D 1 O6A O 0.2810(9) 0.6853(5) 0.1580(5) 0.0604(12) Uani 0.643(6) 1 d . U P D 1 C72A C 0.4561(5) 0.6647(5) 0.1876(4) 0.0134(11) Uani 0.643(6) 1 d D U P D 1 S2B S 0.4447(7) 0.6590(6) 0.1775(5) 0.095(3) Uani 0.357(6) 1 d D U P D 2 F4B F 0.3062(14) 0.5837(12) 0.0715(12) 0.045(3) Uani 0.357(6) 1 d . U P D 2 F5B F 0.2785(15) 0.5440(10) 0.1687(7) 0.086(4) Uani 0.357(6) 1 d . U P D 2 F6B F 0.2659(13) 0.6622(9) 0.1554(11) 0.086(4) Uani 0.357(6) 1 d . U P D 2 O4B O 0.4843(16) 0.7281(12) 0.1655(9) 0.0604(12) Uani 0.357(6) 1 d D U P D 2 O5B O 0.4906(18) 0.6057(12) 0.1814(11) 0.0604(12) Uani 0.357(6) 1 d D U P D 2 O6B O 0.4437(11) 0.6830(8) 0.2622(8) 0.0604(12) Uani 0.357(6) 1 d D U P D 2 C72B C 0.3014(14) 0.5908(16) 0.1454(12) 0.071(4) Uani 0.357(6) 1 d D U P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01170(9) 0.01361(9) 0.01701(9) 0.00348(6) 0.00204(6) 0.00282(6) Pd2 0.01190(9) 0.01399(9) 0.01538(9) 0.00424(6) 0.00318(6) 0.00319(6) P1 0.0160(3) 0.0130(3) 0.0171(3) 0.0041(2) 0.0030(2) 0.0024(2) P2 0.0139(3) 0.0144(3) 0.0175(3) 0.0054(2) 0.0032(2) 0.0028(2) P3 0.0135(3) 0.0173(3) 0.0172(3) 0.0036(2) 0.0034(2) 0.0051(2) P4 0.0128(3) 0.0182(3) 0.0224(3) 0.0029(2) 0.0006(2) 0.0040(2) N1 0.0202(11) 0.0154(10) 0.0185(10) 0.0040(8) 0.0054(8) 0.0020(8) N2 0.0192(10) 0.0150(10) 0.0174(10) 0.0026(8) 0.0029(8) 0.0033(8) N3 0.0182(10) 0.0187(10) 0.0196(10) 0.0079(8) 0.0039(8) 0.0056(8) N4 0.0184(11) 0.0210(11) 0.0241(11) 0.0094(9) 0.0052(9) 0.0029(9) C1 0.0191(12) 0.0152(11) 0.0173(11) 0.0048(9) 0.0027(9) 0.0039(9) C2 0.0230(13) 0.0174(11) 0.0213(12) 0.0032(10) 0.0084(10) 0.0047(10) C3 0.0247(14) 0.0273(14) 0.0303(14) 0.0060(11) 0.0072(12) 0.0079(11) C4 0.0385(17) 0.0266(14) 0.0264(14) 0.0105(11) 0.0159(13) 0.0095(12) C5 0.0235(13) 0.0156(11) 0.0204(12) 0.0029(9) 0.0034(10) 0.0034(10) C6 0.0275(14) 0.0175(12) 0.0290(14) 0.0009(10) 0.0093(11) -0.0017(11) C7 0.0215(13) 0.0166(12) 0.0212(12) 0.0038(10) 0.0036(10) 0.0023(10) C8 0.0261(14) 0.0209(13) 0.0262(14) -0.0018(11) 0.0071(11) 0.0014(11) C9 0.0175(12) 0.0179(11) 0.0209(12) 0.0034(9) 0.0043(10) 0.0020(9) C10 0.0256(14) 0.0265(13) 0.0292(14) 0.0124(11) 0.0109(11) 0.0086(11) C11 0.0227(13) 0.0268(14) 0.0308(14) 0.0079(11) 0.0058(11) 0.0096(11) C12 0.0220(12) 0.0184(12) 0.0184(12) 0.0051(10) 0.0023(10) 0.0034(10) C13 0.0202(12) 0.0180(12) 0.0221(13) 0.0043(10) 0.0022(10) 0.0035(10) C14 0.0316(15) 0.0260(14) 0.0197(13) 0.0007(11) 0.0006(11) 0.0056(12) C15 0.0471(19) 0.0320(16) 0.0198(13) 0.0082(12) -0.0008(13) 0.0043(14) C16 0.060(2) 0.0221(14) 0.0262(15) 0.0104(12) 0.0003(15) 0.0058(14) C17 0.0441(18) 0.0165(12) 0.0226(14) 0.0050(10) -0.0004(12) 0.0035(12) C18 0.0163(12) 0.0163(11) 0.0215(12) 0.0062(9) 0.0051(9) 0.0040(9) C19 0.0146(11) 0.0214(12) 0.0209(12) 0.0080(10) 0.0032(9) 0.0037(10) C20 0.0210(13) 0.0292(14) 0.0265(13) 0.0113(11) 0.0048(11) 0.0107(11) C21 0.0230(13) 0.0201(13) 0.0318(14) 0.0041(11) 0.0060(11) 0.0039(10) C22 0.0219(13) 0.0233(13) 0.0243(13) 0.0122(10) 0.0080(11) 0.0075(10) C23 0.0287(14) 0.0349(15) 0.0247(14) 0.0163(12) 0.0061(11) 0.0107(12) C24 0.0245(13) 0.0248(13) 0.0257(13) 0.0120(11) 0.0082(11) 0.0071(11) C25 0.0297(15) 0.0338(16) 0.0382(17) 0.0203(13) 0.0125(13) 0.0028(13) C26 0.0179(12) 0.0242(13) 0.0262(13) 0.0070(11) 0.0025(11) -0.0009(10) C27 0.0268(15) 0.0269(15) 0.0448(18) 0.0049(13) 0.0045(14) -0.0030(12) C28 0.0204(13) 0.0357(16) 0.0294(14) 0.0096(12) 0.0046(11) 0.0048(12) C29 0.0144(11) 0.0211(12) 0.0215(12) 0.0037(10) 0.0031(9) 0.0048(9) C30 0.0244(13) 0.0215(13) 0.0271(14) 0.0040(11) 0.0009(11) 0.0063(11) C31 0.0306(15) 0.0210(13) 0.0403(17) -0.0004(12) 0.0012(13) 0.0099(12) C32 0.0307(16) 0.0326(16) 0.0323(16) -0.0099(13) 0.0006(13) 0.0098(13) C33 0.0259(14) 0.0394(17) 0.0223(13) 0.0009(12) 0.0044(11) 0.0112(12) C34 0.0192(12) 0.0278(13) 0.0222(13) 0.0060(11) 0.0053(10) 0.0084(10) C35 0.0188(12) 0.0169(11) 0.0172(11) 0.0028(9) 0.0046(9) 0.0050(9) C36 0.0176(12) 0.0241(13) 0.0215(12) 0.0050(10) 0.0033(10) 0.0064(10) C37 0.0274(14) 0.0269(13) 0.0207(12) 0.0066(10) 0.0029(11) 0.0101(11) C38 0.0277(14) 0.0219(12) 0.0229(13) 0.0068(10) 0.0092(11) 0.0046(11) C39 0.0183(12) 0.0237(13) 0.0259(13) 0.0031(10) 0.0074(10) 0.0037(10) C40 0.0175(12) 0.0211(12) 0.0215(12) 0.0037(10) 0.0027(10) 0.0050(10) C41 0.0157(11) 0.0202(12) 0.0214(12) 0.0070(10) 0.0059(9) 0.0040(9) C42 0.0210(12) 0.0228(12) 0.0218(12) 0.0057(10) 0.0053(10) 0.0064(10) C43 0.0253(14) 0.0267(13) 0.0204(13) 0.0026(10) 0.0024(11) 0.0043(11) C44 0.0181(13) 0.0350(15) 0.0251(14) 0.0073(12) -0.0019(11) 0.0027(11) C45 0.0184(13) 0.0320(15) 0.0324(15) 0.0105(12) 0.0016(11) 0.0090(11) C46 0.0177(12) 0.0277(13) 0.0240(13) 0.0042(11) 0.0038(10) 0.0080(10) C47 0.0145(11) 0.0214(12) 0.0224(12) 0.0022(10) 0.0014(9) 0.0063(9) C48 0.0214(13) 0.0242(13) 0.0237(13) 0.0023(10) 0.0029(10) 0.0075(10) C49 0.0267(14) 0.0265(14) 0.0287(14) -0.0033(11) 0.0026(11) 0.0088(11) C50 0.0251(14) 0.0209(13) 0.0373(16) -0.0024(12) -0.0006(12) 0.0080(11) C51 0.0287(15) 0.0209(13) 0.0369(16) 0.0084(12) 0.0056(12) 0.0074(11) C52 0.0270(14) 0.0231(13) 0.0273(14) 0.0054(11) 0.0067(11) 0.0094(11) C53 0.0187(12) 0.0274(14) 0.0285(14) 0.0079(11) 0.0023(11) 0.0076(11) C54 0.0229(14) 0.0317(15) 0.0247(14) 0.0041(11) 0.0023(11) 0.0067(11) C55 0.0337(17) 0.052(2) 0.0278(15) 0.0122(14) -0.0008(13) 0.0092(15) C56 0.041(2) 0.065(3) 0.046(2) 0.035(2) 0.0001(17) 0.0113(18) C57 0.039(2) 0.046(2) 0.061(3) 0.034(2) -0.0089(18) -0.0012(16) C58 0.0265(15) 0.0344(17) 0.0453(19) 0.0190(14) -0.0082(14) 0.0007(13) C59 0.0167(12) 0.0199(12) 0.0211(12) 0.0027(10) 0.0008(10) 0.0049(10) C60 0.0173(12) 0.0228(13) 0.0221(12) 0.0027(10) 0.0021(10) 0.0055(10) C61 0.0175(12) 0.0287(14) 0.0241(13) 0.0049(11) 0.0021(10) 0.0026(11) C62 0.0236(14) 0.0229(13) 0.0269(14) 0.0027(11) 0.0000(11) -0.0013(11) C63 0.0303(15) 0.0222(13) 0.0298(14) -0.0009(11) 0.0051(12) 0.0078(12) C64 0.0195(13) 0.0254(14) 0.0293(14) 0.0018(11) 0.0060(11) 0.0063(11) C65 0.0140(11) 0.0203(12) 0.0280(13) 0.0012(10) -0.0003(10) 0.0036(10) C66 0.0232(14) 0.0302(15) 0.0325(15) -0.0004(12) -0.0061(12) 0.0135(12) C67 0.0232(14) 0.0315(15) 0.0446(18) -0.0024(13) -0.0033(13) 0.0147(12) C68 0.0205(13) 0.0283(14) 0.0407(17) -0.0048(13) 0.0073(12) 0.0067(11) C69 0.0232(14) 0.0259(14) 0.0313(15) 0.0020(11) 0.0070(12) 0.0033(11) C70 0.0177(12) 0.0214(12) 0.0306(14) 0.0045(11) 0.0051(11) 0.0046(10) Cl1 0.0397(5) 0.0683(6) 0.0510(5) -0.0100(5) 0.0094(4) 0.0187(4) Cl2 0.0377(4) 0.0352(4) 0.0364(4) -0.0012(3) 0.0057(3) 0.0148(3) C73 0.053(2) 0.0290(17) 0.069(3) -0.0039(17) 0.034(2) 0.0022(16) Cl3 0.0658(6) 0.0419(5) 0.0399(4) 0.0106(4) 0.0161(4) 0.0072(4) Cl4 0.0764(7) 0.0434(5) 0.0417(5) 0.0170(4) 0.0219(5) 0.0160(5) C74 0.043(2) 0.045(2) 0.0411(19) 0.0212(16) 0.0079(16) 0.0068(16) Cl5A 0.130(3) 0.154(3) 0.095(2) 0.031(2) 0.018(2) -0.002(2) Cl6A 0.0956(15) 0.0655(10) 0.0549(9) 0.0126(8) -0.0062(9) 0.0228(11) C75A 0.097(4) 0.104(4) 0.057(3) -0.001(3) 0.018(3) 0.041(4) Cl5B 0.103(3) 0.074(3) 0.082(4) 0.006(3) 0.022(3) 0.048(3) Cl6B 0.121(4) 0.099(3) 0.086(3) 0.028(3) 0.009(3) 0.045(3) C75B 0.098(5) 0.088(5) 0.063(5) 0.004(5) 0.025(5) 0.030(5) Cl7 0.1137(16) 0.0804(11) 0.152(2) 0.0271(12) 0.0213(14) 0.0165(11) Cl8A 0.134(4) 0.221(5) 0.227(6) -0.004(4) 0.032(4) 0.005(4) C76A 0.131(7) 0.136(7) 0.212(9) 0.011(7) 0.022(7) -0.001(6) Cl8B 0.42(2) 0.084(5) 0.184(11) -0.040(6) -0.091(12) 0.103(9) C76B 0.131(7) 0.136(7) 0.212(9) 0.011(7) 0.022(7) -0.001(6) S1 0.0203(3) 0.0227(3) 0.0239(3) 0.0054(2) 0.0045(2) 0.0028(2) F1 0.0383(12) 0.0705(16) 0.0407(12) 0.0116(11) 0.0210(10) 0.0050(11) F2 0.0429(12) 0.0362(11) 0.0680(15) 0.0212(11) 0.0141(11) -0.0032(9) F3 0.0222(9) 0.0645(15) 0.0575(14) 0.0224(11) 0.0040(9) 0.0053(9) O1 0.0323(11) 0.0334(11) 0.0250(10) 0.0040(9) 0.0044(9) 0.0096(9) O2 0.0335(12) 0.0239(10) 0.0355(11) 0.0054(9) 0.0059(9) 0.0056(9) O3 0.0257(10) 0.0345(11) 0.0278(10) 0.0095(9) 0.0037(8) 0.0076(9) C71 0.0247(15) 0.0360(17) 0.0362(16) 0.0106(13) 0.0070(13) 0.0017(12) S2A 0.0411(8) 0.0274(8) 0.0313(7) 0.0137(6) 0.0070(5) 0.0077(6) F4A 0.065(3) 0.052(3) 0.037(2) 0.0065(17) 0.0046(18) 0.002(2) F5A 0.050(3) 0.053(2) 0.065(4) 0.030(2) 0.016(2) 0.026(2) F6A 0.058(2) 0.0293(16) 0.045(3) 0.016(2) 0.014(2) 0.0040(15) O4A 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) O5A 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) O6A 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) C72A 0.0151(19) 0.014(2) 0.0058(17) -0.0032(15) -0.0032(14) 0.0029(16) S2B 0.117(5) 0.060(3) 0.098(5) 0.024(3) -0.012(3) 0.025(3) F4B 0.057(7) 0.028(3) 0.041(4) 0.009(3) 0.000(4) 0.007(4) F5B 0.097(8) 0.072(7) 0.078(8) 0.035(6) 0.025(7) 0.001(6) F6B 0.063(7) 0.097(8) 0.111(8) 0.029(7) 0.030(6) 0.040(7) O4B 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) O5B 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) O6B 0.072(3) 0.058(2) 0.051(2) 0.0212(16) 0.0084(17) 0.0180(18) C72B 0.091(7) 0.075(7) 0.051(6) 0.026(5) 0.020(5) 0.026(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 6 -4 8 0.1008 0 -5 -2 0.0574 0 -1 0 0.0498 1 -5 4 0.0480 -2 -5 0 0.0813 0 -2 5 0.0706 5 -5 -2 0.0902 5 -3 1 0.0831 1 3 5 0.0860 0 -4 -5 0.0739 8 1 2 0.1008 9 1 -3 0.0895 1 9 -8 0.0625 -6 9 -5 0.0927 -7 6 -6 0.1039 -9 7 1 0.1120 -9 1 -1 0.1144 -9 2 4 0.1155 7 5 -5 0.0792 8 2 -6 0.0820 -6 -1 9 0.1034 0 8 -10 0.0720 -6 5 8 0.1077 6 3 -9 0.0803 -5 -2 11 0.1013 3 8 -9 0.0612 0 -10 6 0.0589 -1 10 -8 0.0700 -2 7 -10 0.0864 2 -5 4 0.0638 0 1 0 0.0611 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 Pd2 56.153(16) . . ? P2 Pd1 Pd2 56.168(16) . . ? P2 Pd1 P1 112.22(2) . . ? P4 Pd1 Pd2 166.787(19) . . ? P4 Pd1 P1 119.30(2) . . ? P4 Pd1 P2 125.61(2) . . ? P1 Pd2 Pd1 56.070(16) . . ? P2 Pd2 Pd1 56.030(16) . . ? P2 Pd2 P1 112.00(2) . . ? P3 Pd2 Pd1 166.977(18) . . ? P3 Pd2 P1 125.95(2) . . ? P3 Pd2 P2 119.27(2) . . ? Pd1 P1 Pd2 67.777(17) . . ? C1 P1 Pd1 127.94(9) . . ? C1 P1 Pd2 122.31(8) . . ? C12 P1 Pd1 113.48(9) . . ? C12 P1 Pd2 123.22(9) . . ? C12 P1 C1 101.37(12) . . ? Pd1 P2 Pd2 67.802(17) . . ? C18 P2 Pd1 125.79(8) . . ? C18 P2 Pd2 128.34(9) . . ? C29 P2 Pd1 121.25(9) . . ? C29 P2 Pd2 110.48(9) . . ? C29 P2 C18 101.59(12) . . ? C35 P3 Pd2 114.00(9) . . ? C35 P3 C47 103.26(12) . . ? C41 P3 Pd2 113.89(9) . . ? C41 P3 C35 105.46(12) . . ? C41 P3 C47 103.07(12) . . ? C47 P3 Pd2 115.82(9) . . ? C53 P4 Pd1 115.64(9) . . ? C53 P4 C59 102.21(13) . . ? C53 P4 C65 104.06(13) . . ? C59 P4 Pd1 115.21(9) . . ? C65 P4 Pd1 113.69(9) . . ? C65 P4 C59 104.55(12) . . ? C1 N1 C2 123.6(2) . . ? C1 N1 C5 109.1(2) . . ? C5 N1 C2 127.1(2) . . ? C1 N2 C7 109.4(2) . . ? C1 N2 C9 123.5(2) . . ? C7 N2 C9 127.0(2) . . ? C18 N3 C19 124.1(2) . . ? C18 N3 C22 109.5(2) . . ? C22 N3 C19 126.4(2) . . ? C18 N4 C24 108.9(2) . . ? C18 N4 C26 123.6(2) . . ? C24 N4 C26 127.1(2) . . ? N1 C1 P1 125.76(19) . . ? N2 C1 P1 126.71(19) . . ? N2 C1 N1 107.4(2) . . ? N1 C2 H2 106.8 . . ? N1 C2 C3 110.7(2) . . ? N1 C2 C4 112.5(2) . . ? C3 C2 H2 106.8 . . ? C3 C2 C4 112.8(2) . . ? C4 C2 H2 106.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 125.0(2) . . ? C7 C5 N1 107.1(2) . . ? C7 C5 C6 127.8(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 125.3(2) . . ? C5 C7 N2 106.9(2) . . ? C5 C7 C8 127.7(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9 106.6 . . ? N2 C9 C10 109.7(2) . . ? N2 C9 C11 113.1(2) . . ? C10 C9 H9 106.6 . . ? C10 C9 C11 113.9(2) . . ? C11 C9 H9 106.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P1 117.1(2) . . ? C17 C12 P1 124.0(2) . . ? C17 C12 C13 118.7(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.2 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.3(3) . . ? C17 C16 H16 119.8 . . ? C12 C17 H17 119.7 . . ? C16 C17 C12 120.6(3) . . ? C16 C17 H17 119.7 . . ? N3 C18 P2 126.58(19) . . ? N3 C18 N4 107.3(2) . . ? N4 C18 P2 126.0(2) . . ? N3 C19 H19 106.6 . . ? N3 C19 C20 112.1(2) . . ? N3 C19 C21 110.5(2) . . ? C20 C19 H19 106.6 . . ? C21 C19 H19 106.6 . . ? C21 C19 C20 114.0(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 125.5(3) . . ? C24 C22 N3 107.1(2) . . ? C24 C22 C23 127.4(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C25 125.0(3) . . ? C22 C24 N4 107.2(2) . . ? C22 C24 C25 127.8(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N4 C26 H26 106.9 . . ? N4 C26 C27 112.0(3) . . ? N4 C26 C28 110.8(2) . . ? C27 C26 H26 106.9 . . ? C28 C26 H26 106.9 . . ? C28 C26 C27 112.9(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P2 124.4(2) . . ? C30 C29 C34 118.6(3) . . ? C34 C29 P2 116.8(2) . . ? C29 C30 H30 119.6 . . ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 120.2 . . ? C30 C31 C32 119.7(3) . . ? C32 C31 H31 120.2 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.4(3) . . ? C34 C33 H33 119.8 . . ? C29 C34 H34 119.8 . . ? C33 C34 C29 120.4(3) . . ? C33 C34 H34 119.8 . . ? C36 C35 P3 117.1(2) . . ? C36 C35 C40 118.8(2) . . ? C40 C35 P3 124.1(2) . . ? C35 C36 H36 119.4 . . ? C37 C36 C35 121.2(3) . . ? C37 C36 H36 119.4 . . ? C36 C37 H37 120.3 . . ? C36 C37 C38 119.4(3) . . ? C38 C37 H37 120.3 . . ? C37 C38 H38 120.1 . . ? C39 C38 C37 119.7(3) . . ? C39 C38 H38 120.1 . . ? C38 C39 H39 119.6 . . ? C38 C39 C40 120.9(3) . . ? C40 C39 H39 119.6 . . ? C35 C40 H40 120.1 . . ? C39 C40 C35 119.9(3) . . ? C39 C40 H40 120.1 . . ? C42 C41 P3 118.5(2) . . ? C42 C41 C46 118.6(3) . . ? C46 C41 P3 122.9(2) . . ? C41 C42 H42 119.7 . . ? C43 C42 C41 120.7(3) . . ? C43 C42 H42 119.7 . . ? C42 C43 H43 119.9 . . ? C44 C43 C42 120.2(3) . . ? C44 C43 H43 119.9 . . ? C43 C44 H44 120.1 . . ? C43 C44 C45 119.9(3) . . ? C45 C44 H44 120.1 . . ? C44 C45 H45 120.0 . . ? C46 C45 C44 120.0(3) . . ? C46 C45 H45 120.0 . . ? C41 C46 H46 119.7 . . ? C45 C46 C41 120.6(3) . . ? C45 C46 H46 119.7 . . ? C48 C47 P3 122.6(2) . . ? C52 C47 P3 118.4(2) . . ? C52 C47 C48 119.0(3) . . ? C47 C48 H48 120.1 . . ? C49 C48 C47 119.8(3) . . ? C49 C48 H48 120.1 . . ? C48 C49 H49 119.6 . . ? C50 C49 C48 120.9(3) . . ? C50 C49 H49 119.6 . . ? C49 C50 H50 120.3 . . ? C49 C50 C51 119.4(3) . . ? C51 C50 H50 120.3 . . ? C50 C51 H51 119.9 . . ? C50 C51 C52 120.2(3) . . ? C52 C51 H51 119.9 . . ? C47 C52 H52 119.7 . . ? C51 C52 C47 120.6(3) . . ? C51 C52 H52 119.7 . . ? C54 C53 P4 122.7(2) . . ? C54 C53 C58 119.1(3) . . ? C58 C53 P4 118.2(2) . . ? C53 C54 H54 120.0 . . ? C55 C54 C53 120.0(3) . . ? C55 C54 H54 120.0 . . ? C54 C55 H55 119.8 . . ? C56 C55 C54 120.4(3) . . ? C56 C55 H55 119.8 . . ? C55 C56 H56 119.9 . . ? C55 C56 C57 120.2(3) . . ? C57 C56 H56 119.9 . . ? C56 C57 H57 120.1 . . ? C58 C57 C56 119.7(3) . . ? C58 C57 H57 120.1 . . ? C53 C58 H58 119.7 . . ? C57 C58 C53 120.6(3) . . ? C57 C58 H58 119.7 . . ? C60 C59 P4 123.4(2) . . ? C64 C59 P4 117.5(2) . . ? C64 C59 C60 119.1(3) . . ? C59 C60 H60 120.0 . . ? C61 C60 C59 119.9(3) . . ? C61 C60 H60 120.0 . . ? C60 C61 H61 119.9 . . ? C62 C61 C60 120.3(3) . . ? C62 C61 H61 119.9 . . ? C61 C62 H62 120.0 . . ? C61 C62 C63 120.1(3) . . ? C63 C62 H62 120.0 . . ? C62 C63 H63 120.1 . . ? C64 C63 C62 119.9(3) . . ? C64 C63 H63 120.1 . . ? C59 C64 H64 119.6 . . ? C63 C64 C59 120.8(3) . . ? C63 C64 H64 119.6 . . ? C66 C65 P4 122.8(2) . . ? C70 C65 P4 118.2(2) . . ? C70 C65 C66 118.9(3) . . ? C65 C66 H66 119.9 . . ? C67 C66 C65 120.1(3) . . ? C67 C66 H66 119.9 . . ? C66 C67 H67 119.7 . . ? C68 C67 C66 120.5(3) . . ? C68 C67 H67 119.7 . . ? C67 C68 H68 120.0 . . ? C67 C68 C69 119.9(3) . . ? C69 C68 H68 120.0 . . ? C68 C69 H69 119.9 . . ? C68 C69 C70 120.1(3) . . ? C70 C69 H69 119.9 . . ? C65 C70 H70 119.8 . . ? C69 C70 C65 120.3(3) . . ? C69 C70 H70 119.8 . . ? Cl1 C73 Cl2 115.7(2) . . ? Cl1 C73 H73A 108.3 . . ? Cl1 C73 H73B 108.3 . . ? Cl2 C73 H73A 108.3 . . ? Cl2 C73 H73B 108.3 . . ? H73A C73 H73B 107.4 . . ? Cl3 C74 Cl4 111.4(2) . . ? Cl3 C74 H74A 109.4 . . ? Cl3 C74 H74B 109.4 . . ? Cl4 C74 H74A 109.4 . . ? Cl4 C74 H74B 109.4 . . ? H74A C74 H74B 108.0 . . ? Cl5A C75A H75A 108.9 . . ? Cl5A C75A H75B 108.9 . . ? Cl6A C75A Cl5A 113.3(5) . . ? Cl6A C75A H75A 108.9 . . ? Cl6A C75A H75B 108.9 . . ? H75A C75A H75B 107.7 . . ? Cl5B C75B H75C 111.4 . . ? Cl5B C75B H75D 111.4 . . ? Cl6B C75B Cl5B 101.7(15) . . ? Cl6B C75B H75C 111.4 . . ? Cl6B C75B H75D 111.4 . . ? H75C C75B H75D 109.3 . . ? Cl7 C76A Cl8A 112.7(10) . . ? Cl7 C76A H76A 109.0 . . ? Cl7 C76A H76B 109.0 . . ? Cl8A C76A H76A 109.0 . . ? Cl8A C76A H76B 109.0 . . ? H76A C76A H76B 107.8 . . ? Cl7 C76B Cl8B 86.2(19) . . ? Cl7 C76B H76C 114.3 . . ? Cl7 C76B H76D 114.3 . . ? Cl8B C76B H76C 114.3 . . ? Cl8B C76B H76D 114.3 . . ? H76C C76B H76D 111.4 . . ? O1 S1 O2 114.76(14) . . ? O1 S1 O3 115.72(14) . . ? O1 S1 C71 103.91(15) . . ? O2 S1 O3 114.49(14) . . ? O2 S1 C71 102.68(15) . . ? O3 S1 C71 102.82(15) . . ? F1 C71 S1 110.8(2) . . ? F2 C71 S1 111.3(2) . . ? F2 C71 F1 107.8(3) . . ? F2 C71 F3 107.5(3) . . ? F3 C71 S1 111.6(2) . . ? F3 C71 F1 107.7(3) . . ? O4A S2A C72A 102.2(8) . . ? O5A S2A O4A 115.7(9) . . ? O5A S2A O6A 114.9(6) . . ? O5A S2A C72A 99.3(5) . . ? O6A S2A O4A 117.3(8) . . ? O6A S2A C72A 103.7(5) . . ? F4A C72A S2A 113.1(4) . . ? F4A C72A F5A 119.0(7) . . ? F4A C72A F6A 106.1(6) . . ? F5A C72A S2A 110.1(6) . . ? F5A C72A F6A 103.6(5) . . ? F6A C72A S2A 103.0(5) . . ? O4B S2B O5B 124.5(16) . . ? O4B S2B O6B 101.1(10) . . ? O4B S2B C72B 125.2(14) . . ? O5B S2B O6B 96.3(10) . . ? O5B S2B C72B 103.9(14) . . ? O6B S2B C72B 97.3(10) . . ? F4B C72B S2B 93.0(14) . . ? F4B C72B F6B 97.1(18) . . ? F5B C72B S2B 115(2) . . ? F5B C72B F4B 125(2) . . ? F5B C72B F6B 124(2) . . ? F6B C72B S2B 94.0(13) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Pd2 2.5840(2) . ? Pd1 P1 2.3161(6) . ? Pd1 P2 2.3146(6) . ? Pd1 P4 2.2988(6) . ? Pd2 P1 2.3183(6) . ? Pd2 P2 2.3183(6) . ? Pd2 P3 2.3011(6) . ? P1 C1 1.840(3) . ? P1 C12 1.813(3) . ? P2 C18 1.834(3) . ? P2 C29 1.814(3) . ? P3 C35 1.827(3) . ? P3 C41 1.825(3) . ? P3 C47 1.829(3) . ? P4 C53 1.824(3) . ? P4 C59 1.831(3) . ? P4 C65 1.827(3) . ? N1 C1 1.354(3) . ? N1 C2 1.488(3) . ? N1 C5 1.387(3) . ? N2 C1 1.350(3) . ? N2 C7 1.387(3) . ? N2 C9 1.487(3) . ? N3 C18 1.348(3) . ? N3 C19 1.490(3) . ? N3 C22 1.379(3) . ? N4 C18 1.355(3) . ? N4 C24 1.387(4) . ? N4 C26 1.489(4) . ? C2 H2 0.9800 . ? C2 C3 1.517(4) . ? C2 C4 1.526(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.490(4) . ? C5 C7 1.367(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.489(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9 0.9800 . ? C9 C10 1.520(4) . ? C9 C11 1.524(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.402(4) . ? C12 C17 1.396(4) . ? C13 H13 0.9300 . ? C13 C14 1.391(4) . ? C14 H14 0.9300 . ? C14 C15 1.391(4) . ? C15 H15 0.9300 . ? C15 C16 1.388(5) . ? C16 H16 0.9300 . ? C16 C17 1.392(4) . ? C17 H17 0.9300 . ? C19 H19 0.9800 . ? C19 C20 1.525(4) . ? C19 C21 1.522(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.491(4) . ? C22 C24 1.362(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.494(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26 0.9800 . ? C26 C27 1.532(4) . ? C26 C28 1.522(4) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.398(4) . ? C29 C34 1.403(4) . ? C30 H30 0.9300 . ? C30 C31 1.392(4) . ? C31 H31 0.9300 . ? C31 C32 1.392(5) . ? C32 H32 0.9300 . ? C32 C33 1.382(5) . ? C33 H33 0.9300 . ? C33 C34 1.387(4) . ? C34 H34 0.9300 . ? C35 C36 1.396(4) . ? C35 C40 1.396(4) . ? C36 H36 0.9300 . ? C36 C37 1.390(4) . ? C37 H37 0.9300 . ? C37 C38 1.393(4) . ? C38 H38 0.9300 . ? C38 C39 1.385(4) . ? C39 H39 0.9300 . ? C39 C40 1.390(4) . ? C40 H40 0.9300 . ? C41 C42 1.393(4) . ? C41 C46 1.403(4) . ? C42 H42 0.9300 . ? C42 C43 1.393(4) . ? C43 H43 0.9300 . ? C43 C44 1.383(4) . ? C44 H44 0.9300 . ? C44 C45 1.391(5) . ? C45 H45 0.9300 . ? C45 C46 1.388(4) . ? C46 H46 0.9300 . ? C47 C48 1.398(4) . ? C47 C52 1.393(4) . ? C48 H48 0.9300 . ? C48 C49 1.392(4) . ? C49 H49 0.9300 . ? C49 C50 1.385(5) . ? C50 H50 0.9300 . ? C50 C51 1.386(5) . ? C51 H51 0.9300 . ? C51 C52 1.392(4) . ? C52 H52 0.9300 . ? C53 C54 1.398(4) . ? C53 C58 1.401(4) . ? C54 H54 0.9300 . ? C54 C55 1.397(5) . ? C55 H55 0.9300 . ? C55 C56 1.377(6) . ? C56 H56 0.9300 . ? C56 C57 1.396(6) . ? C57 H57 0.9300 . ? C57 C58 1.387(5) . ? C58 H58 0.9300 . ? C59 C60 1.397(4) . ? C59 C64 1.395(4) . ? C60 H60 0.9300 . ? C60 C61 1.395(4) . ? C61 H61 0.9300 . ? C61 C62 1.385(4) . ? C62 H62 0.9300 . ? C62 C63 1.387(4) . ? C63 H63 0.9300 . ? C63 C64 1.385(4) . ? C64 H64 0.9300 . ? C65 C66 1.402(4) . ? C65 C70 1.395(4) . ? C66 H66 0.9300 . ? C66 C67 1.393(5) . ? C67 H67 0.9300 . ? C67 C68 1.374(5) . ? C68 H68 0.9300 . ? C68 C69 1.391(5) . ? C69 H69 0.9300 . ? C69 C70 1.392(4) . ? C70 H70 0.9300 . ? Cl1 C73 1.721(4) . ? Cl2 C73 1.761(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? Cl3 C74 1.766(4) . ? Cl4 C74 1.767(4) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? Cl5A C75A 1.772(11) . ? Cl6A C75A 1.742(11) . ? C75A H75A 0.9700 . ? C75A H75B 0.9700 . ? Cl5B C75B 2.06(3) . ? Cl6B C75B 1.35(2) . ? C75B H75C 0.9700 . ? C75B H75D 0.9700 . ? Cl7 C76A 1.686(15) . ? Cl7 C76B 2.05(5) . ? Cl8A C76A 1.806(16) . ? C76A H76A 0.9700 . ? C76A H76B 0.9700 . ? Cl8B C76B 2.05(5) . ? C76B H76C 0.9700 . ? C76B H76D 0.9700 . ? S1 O1 1.440(2) . ? S1 O2 1.442(2) . ? S1 O3 1.444(2) . ? S1 C71 1.832(3) . ? F1 C71 1.336(4) . ? F2 C71 1.326(4) . ? F3 C71 1.332(4) . ? S2A O4A 1.477(18) . ? S2A O5A 1.442(10) . ? S2A O6A 1.458(10) . ? S2A C72A 1.881(7) . ? F4A C72A 1.272(8) . ? F5A C72A 1.319(10) . ? F6A C72A 1.452(8) . ? S2B O4B 1.25(2) . ? S2B O5B 1.31(2) . ? S2B O6B 1.583(17) . ? S2B C72B 1.966(17) . ? F4B C72B 1.39(3) . ? F5B C72B 0.99(3) . ? F6B C72B 1.49(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 P1 C1 N1 164.27(18) . . . . ? Pd1 P1 C1 N2 -11.5(3) . . . . ? Pd1 P1 C12 C13 -51.6(2) . . . . ? Pd1 P1 C12 C17 124.6(3) . . . . ? Pd1 P2 C18 N3 -92.7(2) . . . . ? Pd1 P2 C18 N4 84.2(2) . . . . ? Pd1 P2 C29 C30 -167.8(2) . . . . ? Pd1 P2 C29 C34 17.9(2) . . . . ? Pd1 P4 C53 C54 122.9(2) . . . . ? Pd1 P4 C53 C58 -57.4(3) . . . . ? Pd1 P4 C59 C60 140.9(2) . . . . ? Pd1 P4 C59 C64 -41.1(2) . . . . ? Pd1 P4 C65 C66 136.0(2) . . . . ? Pd1 P4 C65 C70 -44.3(2) . . . . ? Pd2 P1 C1 N1 78.5(2) . . . . ? Pd2 P1 C1 N2 -97.3(2) . . . . ? Pd2 P1 C12 C13 26.4(3) . . . . ? Pd2 P1 C12 C17 -157.4(2) . . . . ? Pd2 P2 C18 N3 -4.0(3) . . . . ? Pd2 P2 C18 N4 172.87(18) . . . . ? Pd2 P2 C29 C30 116.4(2) . . . . ? Pd2 P2 C29 C34 -57.9(2) . . . . ? Pd2 P3 C35 C36 -32.6(2) . . . . ? Pd2 P3 C35 C40 146.9(2) . . . . ? Pd2 P3 C41 C42 -30.6(2) . . . . ? Pd2 P3 C41 C46 147.2(2) . . . . ? Pd2 P3 C47 C48 113.2(2) . . . . ? Pd2 P3 C47 C52 -65.3(2) . . . . ? P1 C12 C13 C14 178.0(2) . . . . ? P1 C12 C17 C16 -177.5(3) . . . . ? P2 C29 C30 C31 -175.1(2) . . . . ? P2 C29 C34 C33 176.2(2) . . . . ? P3 C35 C36 C37 178.3(2) . . . . ? P3 C35 C40 C39 -178.3(2) . . . . ? P3 C41 C42 C43 177.9(2) . . . . ? P3 C41 C46 C45 -177.9(2) . . . . ? P3 C47 C48 C49 -178.8(2) . . . . ? P3 C47 C52 C51 179.9(2) . . . . ? P4 C53 C54 C55 -179.3(3) . . . . ? P4 C53 C58 C57 -179.0(3) . . . . ? P4 C59 C60 C61 177.9(2) . . . . ? P4 C59 C64 C63 -177.6(2) . . . . ? P4 C65 C66 C67 178.7(2) . . . . ? P4 C65 C70 C69 -178.8(2) . . . . ? N1 C5 C7 N2 -1.0(3) . . . . ? N1 C5 C7 C8 178.9(3) . . . . ? N3 C22 C24 N4 -1.2(3) . . . . ? N3 C22 C24 C25 176.7(3) . . . . ? C1 P1 C12 C13 168.0(2) . . . . ? C1 P1 C12 C17 -15.9(3) . . . . ? C1 N1 C2 C3 -108.9(3) . . . . ? C1 N1 C2 C4 123.9(3) . . . . ? C1 N1 C5 C6 -176.3(3) . . . . ? C1 N1 C5 C7 0.9(3) . . . . ? C1 N2 C7 C5 0.7(3) . . . . ? C1 N2 C7 C8 -179.2(3) . . . . ? C1 N2 C9 C10 98.0(3) . . . . ? C1 N2 C9 C11 -133.7(3) . . . . ? C2 N1 C1 P1 -2.1(4) . . . . ? C2 N1 C1 N2 174.4(2) . . . . ? C2 N1 C5 C6 9.0(4) . . . . ? C2 N1 C5 C7 -173.7(2) . . . . ? C5 N1 C1 P1 -177.01(19) . . . . ? C5 N1 C1 N2 -0.5(3) . . . . ? C5 N1 C2 C3 65.1(3) . . . . ? C5 N1 C2 C4 -62.1(4) . . . . ? C6 C5 C7 N2 176.2(3) . . . . ? C6 C5 C7 C8 -3.9(5) . . . . ? C7 N2 C1 P1 176.34(19) . . . . ? C7 N2 C1 N1 -0.1(3) . . . . ? C7 N2 C9 C10 -77.1(3) . . . . ? C7 N2 C9 C11 51.2(3) . . . . ? C9 N2 C1 P1 0.5(4) . . . . ? C9 N2 C1 N1 -176.0(2) . . . . ? C9 N2 C7 C5 176.4(2) . . . . ? C9 N2 C7 C8 -3.5(4) . . . . ? C12 P1 C1 N1 -63.5(2) . . . . ? C12 P1 C1 N2 120.7(2) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C13 C12 C17 C16 -1.4(5) . . . . ? C13 C14 C15 C16 -0.8(5) . . . . ? C14 C15 C16 C17 1.0(6) . . . . ? C15 C16 C17 C12 0.1(6) . . . . ? C17 C12 C13 C14 1.7(4) . . . . ? C18 P2 C29 C30 -22.4(3) . . . . ? C18 P2 C29 C34 163.2(2) . . . . ? C18 N3 C19 C20 -127.4(3) . . . . ? C18 N3 C19 C21 104.3(3) . . . . ? C18 N3 C22 C23 -179.6(3) . . . . ? C18 N3 C22 C24 1.1(3) . . . . ? C18 N4 C24 C22 1.0(3) . . . . ? C18 N4 C24 C25 -177.0(3) . . . . ? C18 N4 C26 C27 125.7(3) . . . . ? C18 N4 C26 C28 -107.1(3) . . . . ? C19 N3 C18 P2 -1.8(4) . . . . ? C19 N3 C18 N4 -179.1(2) . . . . ? C19 N3 C22 C23 -1.0(4) . . . . ? C19 N3 C22 C24 179.7(2) . . . . ? C22 N3 C18 P2 176.9(2) . . . . ? C22 N3 C18 N4 -0.5(3) . . . . ? C22 N3 C19 C20 54.1(3) . . . . ? C22 N3 C19 C21 -74.1(3) . . . . ? C23 C22 C24 N4 179.4(3) . . . . ? C23 C22 C24 C25 -2.6(5) . . . . ? C24 N4 C18 P2 -177.7(2) . . . . ? C24 N4 C18 N3 -0.3(3) . . . . ? C24 N4 C26 C27 -63.0(4) . . . . ? C24 N4 C26 C28 64.2(4) . . . . ? C26 N4 C18 P2 -5.0(4) . . . . ? C26 N4 C18 N3 172.4(2) . . . . ? C26 N4 C24 C22 -171.4(3) . . . . ? C26 N4 C24 C25 10.6(5) . . . . ? C29 P2 C18 N3 124.1(2) . . . . ? C29 P2 C18 N4 -59.0(2) . . . . ? C29 C30 C31 C32 0.0(5) . . . . ? C30 C29 C34 C33 1.5(4) . . . . ? C30 C31 C32 C33 0.1(5) . . . . ? C31 C32 C33 C34 0.6(5) . . . . ? C32 C33 C34 C29 -1.4(4) . . . . ? C34 C29 C30 C31 -0.8(4) . . . . ? C35 P3 C41 C42 95.1(2) . . . . ? C35 P3 C41 C46 -87.1(2) . . . . ? C35 P3 C47 C48 -12.2(3) . . . . ? C35 P3 C47 C52 169.3(2) . . . . ? C35 C36 C37 C38 0.2(4) . . . . ? C36 C35 C40 C39 1.2(4) . . . . ? C36 C37 C38 C39 0.8(4) . . . . ? C37 C38 C39 C40 -0.8(4) . . . . ? C38 C39 C40 C35 -0.2(4) . . . . ? C40 C35 C36 C37 -1.2(4) . . . . ? C41 P3 C35 C36 -158.2(2) . . . . ? C41 P3 C35 C40 21.3(3) . . . . ? C41 P3 C47 C48 -121.8(2) . . . . ? C41 P3 C47 C52 59.7(2) . . . . ? C41 C42 C43 C44 -0.1(4) . . . . ? C42 C41 C46 C45 -0.1(4) . . . . ? C42 C43 C44 C45 0.3(4) . . . . ? C43 C44 C45 C46 -0.4(5) . . . . ? C44 C45 C46 C41 0.3(4) . . . . ? C46 C41 C42 C43 0.0(4) . . . . ? C47 P3 C35 C36 93.9(2) . . . . ? C47 P3 C35 C40 -86.6(2) . . . . ? C47 P3 C41 C42 -156.9(2) . . . . ? C47 P3 C41 C46 20.9(3) . . . . ? C47 C48 C49 C50 -0.7(4) . . . . ? C48 C47 C52 C51 1.3(4) . . . . ? C48 C49 C50 C51 0.8(5) . . . . ? C49 C50 C51 C52 0.2(5) . . . . ? C50 C51 C52 C47 -1.2(5) . . . . ? C52 C47 C48 C49 -0.3(4) . . . . ? C53 P4 C59 C60 -92.8(2) . . . . ? C53 P4 C59 C64 85.2(2) . . . . ? C53 P4 C65 C66 9.3(3) . . . . ? C53 P4 C65 C70 -171.0(2) . . . . ? C53 C54 C55 C56 -1.2(6) . . . . ? C54 C53 C58 C57 0.7(6) . . . . ? C54 C55 C56 C57 -0.2(7) . . . . ? C55 C56 C57 C58 1.9(7) . . . . ? C56 C57 C58 C53 -2.2(7) . . . . ? C58 C53 C54 C55 1.0(5) . . . . ? C59 P4 C53 C54 -3.1(3) . . . . ? C59 P4 C53 C58 176.6(3) . . . . ? C59 P4 C65 C66 -97.6(3) . . . . ? C59 P4 C65 C70 82.2(2) . . . . ? C59 C60 C61 C62 -0.1(4) . . . . ? C60 C59 C64 C63 0.5(4) . . . . ? C60 C61 C62 C63 -0.2(5) . . . . ? C61 C62 C63 C64 0.6(5) . . . . ? C62 C63 C64 C59 -0.8(5) . . . . ? C64 C59 C60 C61 0.0(4) . . . . ? C65 P4 C53 C54 -111.7(3) . . . . ? C65 P4 C53 C58 68.0(3) . . . . ? C65 P4 C59 C60 15.4(3) . . . . ? C65 P4 C59 C64 -166.6(2) . . . . ? C65 C66 C67 C68 0.5(5) . . . . ? C66 C65 C70 C69 0.9(4) . . . . ? C66 C67 C68 C69 0.1(5) . . . . ? C67 C68 C69 C70 -0.2(5) . . . . ? C68 C69 C70 C65 -0.3(4) . . . . ? C70 C65 C66 C67 -1.0(4) . . . . ? O1 S1 C71 F1 -179.2(2) . . . . ? O1 S1 C71 F2 60.9(3) . . . . ? O1 S1 C71 F3 -59.2(3) . . . . ? O2 S1 C71 F1 -59.3(3) . . . . ? O2 S1 C71 F2 -179.3(2) . . . . ? O2 S1 C71 F3 60.7(3) . . . . ? O3 S1 C71 F1 59.8(3) . . . . ? O3 S1 C71 F2 -60.1(3) . . . . ? O3 S1 C71 F3 179.8(2) . . . . ? O4A S2A C72A F4A 177.6(9) . . . . ? O4A S2A C72A F5A -46.4(9) . . . . ? O4A S2A C72A F6A 63.5(9) . . . . ? O5A S2A C72A F4A -63.4(7) . . . . ? O5A S2A C72A F5A 72.5(6) . . . . ? O5A S2A C72A F6A -177.5(5) . . . . ? O6A S2A C72A F4A 55.2(7) . . . . ? O6A S2A C72A F5A -168.8(6) . . . . ? O6A S2A C72A F6A -58.8(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 6.3929 -4.0456 7.7851 0.4298 0.9029 -0.0092 -0.0013 -4.9915 -1.9995 -0.2963 -0.0021 0.4486 -0.0005 -0.9987 0.0003 -0.0595 0.0259 0.0686 0.9960 -4.9991 4.0048 -0.1944 0.4375 0.1513 -2.0046 -4.9919 -0.0008 -0.5086 0.0396 0.3042 -0.0042 -2.0031 5.0033 -0.1220 0.3806 -0.1267 5.0039 -4.9961 -1.9937 0.2313 0.2225 0.5456 5.0031 -3.0019 1.0073 0.3485 0.3680 0.2501 0.9994 2.9897 5.0029 0.2810 0.2961 -0.4503 0.0011 -3.9894 -5.0014 -0.2350 -0.2253 0.5383 7.9313 0.7208 2.1510 0.8784 0.4778 -0.0093 8.5219 0.8584 -2.7660 0.9512 0.1775 0.2524 1.4513 9.2861 -7.5579 0.7094 -0.6726 -0.2107 -6.3590 9.3171 -5.1112 -0.1137 -0.8622 -0.4936 -7.4003 6.0708 -5.8575 -0.4164 -0.8738 -0.2513 -8.6301 7.1881 0.9871 -0.4828 -0.5078 -0.7134 -8.8280 1.2693 -0.5579 -0.8553 -0.4648 -0.2290 -8.9022 1.7197 4.3791 -0.8386 -0.1553 -0.5221 6.6113 4.8989 -4.5443 0.9910 -0.1297 0.0316 7.6562 2.0622 -6.2665 0.9332 -0.1226 0.3378 -6.4532 -1.3512 9.4180 -0.7655 0.3652 -0.5297 -0.0161 7.9751 -10.2063 0.4778 -0.8784 -0.0092 -5.9747 5.4644 8.4836 -0.3089 0.1485 -0.9394 6.0208 3.4972 -8.8656 0.8474 -0.4039 0.3447 -4.6559 -1.7727 11.1622 -0.6018 0.5713 -0.5581 2.5315 7.6365 -9.1748 0.7259 -0.6878 0.0090 -0.4867 -10.3303 5.8885 -0.6690 0.6331 0.3894 -1.3660 10.0225 -7.8619 0.4562 -0.8378 -0.2999 -2.3965 7.2378 -10.4679 0.1830 -0.9831 0.0091 1.9970 -5.0001 4.0060 -0.0889 0.4824 0.1707 0.0005 0.9987 -0.0003 0.0595 -0.0259 -0.0686