#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577308.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_1577308 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 'C37 H67 N4 P3 Pd, 2(C F3 O3 S), C6 H4 F2, 0.5(C4 H8 O)' _chemical_formula_sum 'C47 H75 F8 N4 O6.5 P3 Pd S2' _chemical_formula_weight 1215.54 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-10-13 _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.231(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.6307(4) _cell_length_b 14.8734(2) _cell_length_c 23.4810(4) _cell_measurement_reflns_used 10601 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 76.1950 _cell_measurement_theta_min 3.5350 _cell_volume 5576.65(19) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5700 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _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 -64.00 32.00 0.50 7.50 -- -38.50 57.00-180.00 192 2 \w -107.00 -12.00 0.50 7.50 -- -38.50 -57.00 30.00 190 3 \w -60.00 34.00 0.50 7.50 -- -38.50 38.00 -30.00 188 4 \w 46.00 97.00 0.50 7.50 -- 42.50-125.00 0.00 102 5 \w 6.00 54.00 0.50 7.50 -- 42.50 -99.00-120.00 96 6 \w 108.00 138.00 0.50 30.00 -- 111.00 -77.00 -90.00 60 7 \w 88.00 164.00 0.50 30.00 -- 111.00 30.00 60.00 152 8 \w 99.00 178.00 0.50 30.00 -- 111.00 45.00 0.00 158 9 \w 112.00 176.00 0.50 30.00 -- 111.00 77.00 -60.00 128 10 \w 50.00 75.00 0.50 30.00 -- 111.00 -94.00-180.00 50 11 \w 34.00 83.00 0.50 30.00 -- 111.00 -94.00 60.00 98 12 \w 48.00 75.00 0.50 30.00 -- 111.00 -94.00-120.00 54 13 \w 78.00 107.00 0.50 30.00 -- 111.00 -94.00-120.00 58 14 \w 80.00 107.00 0.50 30.00 -- 111.00 -94.00 150.00 54 15 \w 77.00 120.00 0.50 30.00 -- 111.00 -30.00-180.00 86 16 \w 31.00 39.00 0.50 30.00 -- 111.00 -94.00 -90.00 16 ; _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 -0.0756399000 _diffrn_orient_matrix_UB_12 -0.0283518000 _diffrn_orient_matrix_UB_13 0.0216488000 _diffrn_orient_matrix_UB_21 0.0491882000 _diffrn_orient_matrix_UB_22 0.0238929000 _diffrn_orient_matrix_UB_23 0.0640857000 _diffrn_orient_matrix_UB_31 -0.0342964000 _diffrn_orient_matrix_UB_32 0.0966914000 _diffrn_orient_matrix_UB_33 -0.0094918000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 0.965 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 25258 _diffrn_reflns_point_group_measured_fraction_full 0.965 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.245 _diffrn_reflns_theta_min 2.767 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.856 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 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 yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.448 _exptl_crystal_description plank _exptl_crystal_F_000 2528 _exptl_crystal_size_max 0.173 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.019 _refine_diff_density_max 1.414 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 883 _refine_ls_number_reflns 9837 _refine_ls_number_restraints 1140 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0531 _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^)+(0.0974P)^2^+3.1227P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1413 _refine_ls_wR_factor_ref 0.1512 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8245 _reflns_number_total 9837 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1291 _cod_original_formula_sum 'C47 H75 F8 N4 O6.50 P3 Pd S2' _cod_database_code 1577308 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C184 H304 N28 O40 Pd4 S12 P1 F1 ' _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 94.38 _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, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O7-C46 = O7-C49 1.44 with sigma of 0.02 C47-C48 1.54 with sigma of 0.02 C46-C47 = C48-C49 1.53 with sigma of 0.02 O7-C47 = O7-C48 = C46-C48 = C47-C49 2.38 with sigma of 0.04 F4A-S2A \\sim F4B-S2B with sigma of 0.04 C39A-F5A \\sim C39B-F6B with sigma of 0.02 F5A-S2A \\sim F6B-S2B with sigma of 0.04 F6A-S2A \\sim F5B-S2B with sigma of 0.04 C39A-S2A \\sim C39B-S2B with sigma of 0.02 C39A-F6A \\sim C39B-F5B with sigma of 0.02 C39A-F4A \\sim C39B-F4B with sigma of 0.02 O6A-S2A \\sim O5B-S2B with sigma of 0.02 O5A-S2A \\sim O6B-S2B with sigma of 0.02 O4A-S2A \\sim O4B-S2B with sigma of 0.02 F5A-F6A \\sim F6B-F5B with sigma of 0.04 F4A-F6A \\sim F4B-F5B with sigma of 0.04 C39A-O6A \\sim C39B-O5B with sigma of 0.04 C39A-O5A \\sim C39B-O6B with sigma of 0.04 O5A-O4A \\sim O6B-O4B with sigma of 0.04 C39A-O4A \\sim C39B-O4B with sigma of 0.04 O6A-O5A \\sim O5B-O6B with sigma of 0.04 O6A-O4A \\sim O5B-O4B with sigma of 0.04 F5A-F4A \\sim F6B-F4B with sigma of 0.04 C47-C49 \\sim C46-C48 with sigma of 0.04 O7-C47 \\sim O7-C48 with sigma of 0.04 C46-C47 \\sim C47-C48 \\sim C48-C49 with sigma of 0.02 O7-C46 \\sim O7-C49 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C19B \\sim C19A \\sim C18 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C19B \\sim C20 \\sim C19A \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A O3A \\sim S1A \\sim O1A \\sim O2A \\sim C38A \\sim F2A \\sim F1A \\sim F3A \\sim O2B \\sim S1B \\sim O3B \\sim O1B \\sim C38B \\sim F1B \\sim F3B \\sim F2B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C41B \\sim F8B \\sim C40B \\sim C42B \\sim F7B \\sim C45B \\sim C43B \\sim C44B \\sim C42A \\sim F7A \\sim C41A \\sim C40A \\sim F8A \\sim C43A \\sim C45A \\sim C44A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O4B \\sim O5B \\sim S2B \\sim C39B \\sim O6B \\sim F6B \\sim F4B \\sim F5B \\sim F6A \\sim C39A \\sim F5A \\sim F4A \\sim S2A \\sim O6A \\sim O5A \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A O7 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4. Rigid body (RIGU) restrains C39A, F5A, F4A, F6A, S2A, O6A, O5A, O4A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O3A, S1A, O1A, O2A, C38A, F2A, F1A, F3A, O2B, S1B, O3B, O1B, C38B, F1B, F3B, F2B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C41B, F8B, C40B, C42B, F7B, C45B, C43B, C44B, C42A, F7A, C41A, C40A, F8A, C43A, C45A, C44A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O4B, O5B, S2B, C39B, O6B, F6B, F4B, F5B, F6A, C39A, F5A, F4A, S2A, O6A, O5A, O4A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O7, C46, C47, C48, C49 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H18C)=Sof(H18D)=Sof(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19A)=1-FVAR(1) Sof(H18A)=Sof(H18B)=Sof(H20A)=Sof(H20B)=Sof(C19B)=Sof(H19B)=FVAR(1) Sof(O2B)=Sof(S1B)=Sof(O3B)=Sof(O1B)=Sof(C38B)=Sof(F1B)=Sof(F3B)=Sof(F2B)=1- FVAR(2) Sof(S1A)=Sof(F1A)=Sof(O1A)=Sof(F2A)=Sof(O2A)=Sof(O3A)=Sof(F3A)=Sof(C38A)= FVAR(2) Sof(O5B)=Sof(C39B)=Sof(F6B)=Sof(F4B)=Sof(F5B)=Sof(S2B)=Sof(O6B)=Sof(O4B)=1- FVAR(3) Sof(C39A)=Sof(O6A)=Sof(F5A)=Sof(F4A)=Sof(O5A)=Sof(O4A)=Sof(F6A)=Sof(S2A)= FVAR(3) Fixed Sof: F7A(0.72) F8A(0.72) C43A(0.72) H43A(0.72) C42A(0.72) C41A(0.72) C40A(0.72) H40A(0.72) C45A(0.72) H45A(0.72) C44A(0.72) H44A(0.72) F8B(0.28) F7B(0.28) C41B(0.28) C40B(0.28) C45B(0.28) H45B(0.28) C44B(0.28) H44B(0.28) C43B(0.28) H43B(0.28) C42B(0.28) H42B(0.28) O7(0.5) C46(0.5) H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5) 6.a Ternary CH refined with riding coordinates: C22(H22), C32(H32), C29(H29), C10(H10), C12(H12), C2(H2), C19B(H19B), C19A(H19A) 6.b Secondary CH2 refined with riding coordinates: C33(H33A,H33B), C34(H34A,H34B), C18(H18A,H18B), C18(H18C,H18D), C13(H13A, H13B), C35(H35A,H35B), C20(H20A,H20B), C20(H20C,H20D), C14(H14A,H14B), C36(H36A,H36B), C17(H17A,H17B), C37(H37A,H37B), C16(H16A,H16B), C15(H15A,H15B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B) 6.c Aromatic/amide H refined with riding coordinates: C43A(H43A), C40A(H40A), C45A(H45A), C44A(H44A), C45B(H45B), C44B(H44B), C43B(H43B), C42B(H42B) 6.d Fitted hexagon refined as free rotating group: C43A(C42A,C41A,C40A,C45A,C44A), C41B(C40B,C45B,C44B,C43B,C42B) 6.e Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C28(H28A,H28B, H28C), C23(H23A,H23B,H23C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C11(H11A,H11B,H11C), C3(H3A,H3B,H3C), C31(H31A,H31B,H31C) ; _shelx_res_file ; TITL jjw1291_a.res in P2(1)/c jjw1291.res created by SHELXL-2018/3 at 13:06:02 on 13-Oct-2020 REM Old TITL jjw1291 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.163, Rweak 0.019, Alpha 0.050 REM 0.473 for 432 systematic absences, Orientation as input REM Formula found by SHELXT: C49 N9 O6 S4 Pd CELL 1.54184 16.6307 14.8734 23.481 90 106.231 90 ZERR 4 0.0004 0.0002 0.0004 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O P Pd S UNIT 188 300 32 16 26 12 4 8 DFIX 1.44 O7 C46 O7 C49 DFIX 1.54 C47 C48 DFIX 1.53 C46 C47 C48 C49 SADI 0.04 F4A S2A F4B S2B SADI C39A F5A C39B F6B SADI 0.04 F5A S2A F6B S2B SADI 0.04 F6A S2A F5B S2B SADI C39A S2A C39B S2B SADI C39A F6A C39B F5B SADI C39A F4A C39B F4B SADI O6A S2A O5B S2B SADI O5A S2A O6B S2B SADI O4A S2A O4B S2B SADI 0.04 F5A F6A F6B F5B SADI 0.04 F4A F6A F4B F5B SADI 0.04 C39A O6A C39B O5B SADI 0.04 C39A O5A C39B O6B SADI 0.04 O5A O4A O6B O4B SADI 0.04 C39A O4A C39B O4B SADI 0.04 O6A O5A O5B O6B SADI 0.04 O6A O4A O5B O4B SADI 0.04 F5A F4A F6B F4B SADI 0.04 C47 C49 C46 C48 SADI 0.04 O7 C47 O7 C48 SADI C46 C47 C47 C48 C48 C49 SADI O7 C46 O7 C49 DANG 2.38 O7 C47 O7 C48 C46 C48 C47 C49 SIMU C19B C19A C18 C20 SIMU 0.01 0.01 2 C19B C20 C19A C18 SIMU O3A S1A O1A O2A C38A F2A F1A F3A O2B S1B O3B O1B C38B F1B F3B F2B SIMU C41B F8B C40B C42B F7B C45B C43B C44B C42A F7A C41A C40A F8A C43A C45A = C44A SIMU 0.01 0.01 2 O4B O5B S2B C39B O6B F6B F4B F5B F6A C39A F5A F4A S2A O6A = O5A O4A SIMU O7 C46 C47 C48 C49 RIGU C39A F5A F4A F6A S2A O6A O5A O4A RIGU O3A S1A O1A O2A C38A F2A F1A F3A O2B S1B O3B O1B C38B F1B F3B F2B RIGU C41B F8B C40B C42B F7B C45B C43B C44B C42A F7A C41A C40A F8A C43A C45A = C44A RIGU O4B O5B S2B C39B O6B F6B F4B F5B F6A C39A F5A F4A S2A O6A O5A O4A RIGU O7 C46 C47 C48 C49 L.S. 20 PLAN 14 CONF BOND $H list 4 MORE -1 fmap 2 TEMP 100 acta SHEL 1000 0.83 REM REM REM WGHT 0.097400 3.122700 FVAR 0.19027 0.36884 0.79463 0.58082 PD1 7 0.323237 0.687813 0.426535 11.00000 0.03801 0.02298 = 0.03081 0.00250 0.00650 -0.00190 P1 6 0.261844 0.828545 0.401019 11.00000 0.03280 0.02544 = 0.03666 0.00418 0.00600 -0.00018 P3 6 0.439080 0.780179 0.433177 11.00000 0.03403 0.02255 = 0.02927 0.00007 0.00714 0.00143 P2 6 0.374778 0.907342 0.418097 11.00000 0.03273 0.02212 = 0.04357 -0.00004 0.00695 0.00069 PART 1 S1A 8 0.165685 0.384329 0.304504 31.00000 0.04662 0.03561 = 0.05839 0.00212 -0.00023 -0.00252 C39A 1 0.367684 0.830350 0.201995 41.00000 0.07393 0.05293 = 0.05938 0.00530 0.02259 -0.00512 PART 0 N3 4 0.555229 0.835702 0.370435 11.00000 0.03807 0.02532 = 0.03370 0.00210 0.00901 0.00112 PART 1 O6A 5 0.219138 0.829180 0.132963 41.00000 0.05792 0.05263 = 0.07383 -0.01059 0.02023 -0.00609 PART 0 N4 4 0.513482 0.698530 0.348915 11.00000 0.04472 0.02668 = 0.02809 -0.00061 0.00821 0.00319 PART 1 F5A 3 0.382838 0.746821 0.193991 41.00000 0.08997 0.05658 = 0.09502 0.01980 0.03963 0.01019 F4A 3 0.442847 0.869187 0.215704 41.00000 0.06876 0.06902 = 0.06748 0.00669 0.00488 -0.01511 F1A 3 0.038022 0.330170 0.218871 31.00000 0.05589 0.08445 = 0.06566 -0.02509 0.00998 -0.02075 PART 0 N2 4 0.157992 0.793683 0.282245 11.00000 0.03270 0.03662 = 0.04044 0.00476 0.00336 -0.00101 N1 4 0.178036 0.936505 0.301368 11.00000 0.03942 0.03291 = 0.04206 0.00712 0.01152 0.00319 PART 1 O5A 5 0.283622 0.972936 0.159460 41.00000 0.06352 0.04461 = 0.06057 -0.00420 0.02064 0.00351 O1A 5 0.239470 0.432696 0.302774 31.00000 0.04366 0.05474 = 0.07182 0.00361 -0.00187 -0.00096 PART 0 C25 1 0.593454 0.805831 0.328785 11.00000 0.04133 0.03581 = 0.03335 0.00680 0.01048 0.00638 C27 1 0.567724 0.719491 0.315448 11.00000 0.04798 0.03702 = 0.02909 0.00503 0.01098 0.00821 C22 1 0.570820 0.923055 0.403116 11.00000 0.03811 0.02425 = 0.04903 -0.00224 0.01326 -0.00251 AFIX 13 H22 2 0.531653 0.926003 0.427440 11.00000 -1.20000 AFIX 0 C33 1 0.582868 0.703021 0.512236 11.00000 0.04585 0.03301 = 0.03474 -0.00041 0.00358 0.00456 AFIX 23 H33A 2 0.612532 0.709961 0.482327 11.00000 -1.20000 H33B 2 0.553882 0.645721 0.505717 11.00000 -1.20000 AFIX 0 C21 1 0.506277 0.770266 0.382227 11.00000 0.03501 0.02521 = 0.02946 0.00185 0.00695 0.00345 C34 1 0.645504 0.703819 0.573761 11.00000 0.04394 0.03503 = 0.03797 0.00260 0.00147 0.00786 AFIX 23 H34A 2 0.682745 0.652615 0.577499 11.00000 -1.20000 H34B 2 0.679184 0.757981 0.578208 11.00000 -1.20000 AFIX 0 C5 1 0.127886 0.928492 0.243762 11.00000 0.03557 0.04227 = 0.04198 0.01234 0.00635 0.00447 C32 1 0.519279 0.778814 0.506186 11.00000 0.03473 0.03050 = 0.03040 -0.00212 0.00554 0.00161 AFIX 13 H32 2 0.549760 0.835950 0.510673 11.00000 -1.20000 AFIX 0 PART 1 F2A 3 0.076146 0.458967 0.208081 31.00000 0.19133 0.10165 = 0.14840 0.03386 -0.08160 -0.01337 PART 0 C18 1 0.370310 0.556114 0.462404 11.00000 0.06425 0.02302 = 0.06330 0.01931 0.01816 0.00223 PART 1 AFIX 23 H18A 2 0.372216 0.509853 0.433693 21.00000 -1.20000 H18B 2 0.418933 0.556157 0.496793 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H18C 2 0.411527 0.528211 0.445896 -21.00000 -1.20000 H18D 2 0.382415 0.548821 0.505018 -21.00000 -1.20000 AFIX 0 PART 0 C29 1 0.473825 0.609939 0.352312 11.00000 0.06592 0.02690 = 0.03880 -0.00824 0.02244 -0.00541 AFIX 13 H29 2 0.438104 0.617542 0.378835 11.00000 -1.20000 AFIX 0 C26 1 0.648240 0.860393 0.301415 11.00000 0.04946 0.05023 = 0.04720 0.00685 0.02149 -0.00148 AFIX 137 H26A 2 0.614342 0.900945 0.272787 11.00000 -1.50000 H26B 2 0.678312 0.821159 0.282155 11.00000 -1.50000 H26C 2 0.687292 0.894159 0.331703 11.00000 -1.50000 AFIX 0 PART 1 O2A 5 0.111243 0.426387 0.333103 31.00000 0.07231 0.08000 = 0.07331 -0.02659 0.01769 -0.01466 PART 0 C8 1 0.061195 0.797942 0.175491 11.00000 0.04689 0.06005 = 0.03993 0.00068 0.00590 0.00163 AFIX 137 H8A 2 0.023784 0.842304 0.152764 11.00000 -1.50000 H8B 2 0.029297 0.749525 0.185313 11.00000 -1.50000 H8C 2 0.096360 0.775129 0.152606 11.00000 -1.50000 AFIX 0 C7 1 0.114984 0.840274 0.231873 11.00000 0.03664 0.05091 = 0.03719 0.00493 0.00862 0.00210 C1 1 0.196245 0.853234 0.324766 11.00000 0.03629 0.02785 = 0.04426 0.00335 0.00899 0.00017 C10 1 0.163661 0.694429 0.288938 11.00000 0.04148 0.03020 = 0.04612 0.00227 -0.00028 -0.00627 AFIX 13 H10 2 0.207792 0.681611 0.325519 11.00000 -1.20000 AFIX 0 C24 1 0.658377 0.925073 0.445443 11.00000 0.04782 0.03788 = 0.05087 -0.00576 0.01515 -0.00627 AFIX 137 H24A 2 0.669269 0.869449 0.466971 11.00000 -1.50000 H24B 2 0.662790 0.974020 0.472798 11.00000 -1.50000 H24C 2 0.698494 0.933026 0.423354 11.00000 -1.50000 AFIX 0 C28 1 0.590452 0.657443 0.272475 11.00000 0.06865 0.04659 = 0.04009 -0.00010 0.02570 0.00829 AFIX 137 H28A 2 0.613983 0.603245 0.292525 11.00000 -1.50000 H28B 2 0.630787 0.686044 0.256151 11.00000 -1.50000 H28C 2 0.541209 0.643115 0.241098 11.00000 -1.50000 AFIX 0 C13 1 0.233066 0.846363 0.512038 11.00000 0.04622 0.03533 = 0.04597 0.00375 0.01371 -0.00004 AFIX 23 H13A 2 0.237234 0.781539 0.516392 11.00000 -1.20000 H13B 2 0.289146 0.871188 0.525348 11.00000 -1.20000 AFIX 0 C12 1 0.193853 0.870406 0.446339 11.00000 0.03634 0.03735 = 0.04286 0.00338 0.01042 0.00121 AFIX 13 H12 2 0.191468 0.936099 0.443080 11.00000 -1.20000 AFIX 0 PART 1 F7A 3 0.873498 0.862697 0.517877 10.72000 0.09052 0.06628 = 0.13293 0.01985 0.04820 0.00286 PART 0 C35 1 0.602426 0.700220 0.622647 11.00000 0.04979 0.05494 = 0.03493 0.00775 0.00180 -0.00247 AFIX 23 H35A 2 0.643968 0.706089 0.660782 11.00000 -1.20000 H35B 2 0.575199 0.642344 0.621704 11.00000 -1.20000 AFIX 0 PART 1 O3A 5 0.180439 0.290681 0.317333 31.00000 0.07833 0.03946 = 0.13316 0.01175 -0.01869 -0.00286 PART 0 C2 1 0.206548 1.021336 0.333573 11.00000 0.04039 0.03047 = 0.05328 0.00714 0.00943 0.00391 AFIX 13 H2 2 0.242920 1.004427 0.372639 11.00000 -1.20000 AFIX 0 C20 1 0.225180 0.598116 0.438101 11.00000 0.05436 0.03777 = 0.06410 0.01173 0.01694 -0.01617 PART 1 AFIX 23 H20A 2 0.186412 0.623233 0.457965 21.00000 -1.20000 H20B 2 0.198322 0.560224 0.404555 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H20C 2 0.216119 0.597130 0.477150 -21.00000 -1.20000 H20D 2 0.173729 0.596501 0.405977 -21.00000 -1.20000 AFIX 0 PART 0 C23 1 0.551044 1.002610 0.360623 11.00000 0.05286 0.03211 = 0.06111 0.00564 0.01789 0.00048 AFIX 137 H23A 2 0.594167 1.008532 0.340920 11.00000 -1.50000 H23B 2 0.548346 1.056564 0.382453 11.00000 -1.50000 H23C 2 0.498156 0.992871 0.331716 11.00000 -1.50000 AFIX 0 C14 1 0.180127 0.883480 0.550154 11.00000 0.05747 0.05595 = 0.05125 0.00368 0.02300 0.00259 AFIX 23 H14A 2 0.180244 0.948648 0.548576 11.00000 -1.20000 H14B 2 0.204462 0.865465 0.591061 11.00000 -1.20000 AFIX 0 C36 1 0.537637 0.774669 0.615957 11.00000 0.04652 0.07600 = 0.03225 -0.00032 0.01148 0.00481 AFIX 23 H36A 2 0.508259 0.767395 0.646005 11.00000 -1.20000 H36B 2 0.565876 0.832400 0.622295 11.00000 -1.20000 AFIX 0 C17 1 0.104378 0.834706 0.424735 11.00000 0.04766 0.07894 = 0.05293 -0.00179 0.01386 -0.00822 AFIX 23 H17A 2 0.105021 0.769524 0.426152 11.00000 -1.20000 H17B 2 0.079630 0.852972 0.383928 11.00000 -1.20000 AFIX 0 C6 1 0.097017 1.004914 0.201441 11.00000 0.05179 0.05390 = 0.05290 0.01875 0.00847 0.01571 AFIX 137 H6A 2 0.137470 1.017798 0.180327 11.00000 -1.50000 H6B 2 0.089104 1.057228 0.223209 11.00000 -1.50000 H6C 2 0.044755 0.988540 0.173749 11.00000 -1.50000 AFIX 0 C4 1 0.259756 1.076755 0.303660 11.00000 0.05782 0.03805 = 0.06648 0.01133 0.01368 -0.00464 AFIX 137 H4A 2 0.303469 1.039807 0.296818 11.00000 -1.50000 H4B 2 0.284097 1.126330 0.328762 11.00000 -1.50000 H4C 2 0.225358 1.099182 0.266477 11.00000 -1.50000 AFIX 0 C37 1 0.474733 0.773685 0.555043 11.00000 0.04065 0.06636 = 0.03438 0.00086 0.01133 0.00482 AFIX 23 H37A 2 0.436942 0.824374 0.551455 11.00000 -1.20000 H37B 2 0.441766 0.718985 0.550373 11.00000 -1.20000 AFIX 0 C9 1 0.189640 0.650239 0.237977 11.00000 0.06017 0.03863 = 0.06344 -0.00244 0.01571 -0.00289 AFIX 137 H9A 2 0.210484 0.590839 0.249515 11.00000 -1.50000 H9B 2 0.232695 0.685511 0.228750 11.00000 -1.50000 H9C 2 0.142045 0.646631 0.203680 11.00000 -1.50000 AFIX 0 C30 1 0.539860 0.540849 0.380944 11.00000 0.08166 0.02672 = 0.05715 0.00452 0.01929 -0.00228 AFIX 137 H30A 2 0.513046 0.486034 0.387190 11.00000 -1.50000 H30B 2 0.573479 0.563379 0.418343 11.00000 -1.50000 H30C 2 0.574842 0.529410 0.355418 11.00000 -1.50000 AFIX 0 C11 1 0.082151 0.656227 0.296641 11.00000 0.06081 0.04988 = 0.05360 -0.00028 0.01312 -0.01758 AFIX 137 H11A 2 0.037181 0.668612 0.261762 11.00000 -1.50000 H11B 2 0.070355 0.683637 0.330441 11.00000 -1.50000 H11C 2 0.087654 0.592408 0.302565 11.00000 -1.50000 AFIX 0 C3 1 0.132943 1.073515 0.344588 11.00000 0.05053 0.04131 = 0.06445 0.00208 0.01107 0.01185 AFIX 137 H3A 2 0.096131 1.092715 0.307351 11.00000 -1.50000 H3B 2 0.153682 1.125130 0.368785 11.00000 -1.50000 H3C 2 0.102867 1.035413 0.364532 11.00000 -1.50000 AFIX 0 PART 1 F3A 3 0.145853 0.348148 0.192836 31.00000 0.07926 0.34249 = 0.11393 -0.10738 0.04762 -0.03436 PART 0 C16 1 0.051517 0.871305 0.463900 11.00000 0.03720 0.12159 = 0.06967 -0.00619 0.01849 -0.00087 AFIX 23 H16A 2 0.046390 0.936022 0.459157 11.00000 -1.20000 H16B 2 -0.004286 0.845721 0.450882 11.00000 -1.20000 AFIX 0 PART 1 C38A 1 0.103659 0.381720 0.227180 31.00000 0.05675 0.07256 = 0.05921 -0.00465 0.01981 -0.01745 PART 0 C31 1 0.417154 0.579679 0.292748 11.00000 0.06607 0.04955 = 0.06199 -0.01254 0.00888 -0.01737 AFIX 137 H31A 2 0.450532 0.554320 0.269384 11.00000 -1.50000 H31B 2 0.386544 0.630377 0.272303 11.00000 -1.50000 H31C 2 0.378592 0.535226 0.298935 11.00000 -1.50000 AFIX 0 C15 1 0.089881 0.849270 0.528812 11.00000 0.06523 0.08592 = 0.07035 -0.00686 0.03649 -0.01115 AFIX 23 H15A 2 0.089139 0.784695 0.534427 11.00000 -1.20000 H15B 2 0.056837 0.876781 0.552235 11.00000 -1.20000 AFIX 0 PART 1 F8A 3 0.813585 0.819599 0.401974 10.72000 0.15489 0.22038 = 0.11169 0.07398 0.06871 0.07934 C19B 1 0.297600 0.569507 0.472559 21.00000 0.06132 0.02164 = 0.04893 0.01601 0.02116 -0.00797 AFIX 13 H19B 2 0.303421 0.581636 0.514543 21.00000 -1.20000 AFIX 66 C43A 1 0.788211 0.675276 0.422028 10.72000 0.07031 0.16662 = 0.09103 -0.04330 0.00718 0.03104 AFIX 43 H43A 2 0.767154 0.661840 0.381926 10.72000 -1.20000 AFIX 65 C42A 1 0.815737 0.761826 0.439658 10.72000 0.06740 0.14084 = 0.06493 0.02434 0.02984 0.04859 C41A 1 0.847210 0.781908 0.499595 10.72000 0.05539 0.07370 = 0.07220 0.01820 0.03239 0.01322 C40A 1 0.851157 0.715440 0.541902 10.72000 0.07055 0.05380 = 0.08428 0.01606 0.04067 0.00750 AFIX 43 H40A 2 0.872215 0.728876 0.582004 10.72000 -1.20000 AFIX 65 C45A 1 0.823632 0.628890 0.524274 10.72000 0.08558 0.07600 = 0.13124 -0.00947 0.04026 -0.00666 AFIX 43 H45A 2 0.826273 0.584419 0.552581 10.72000 -1.20000 AFIX 65 C44A 1 0.792159 0.608807 0.464337 10.72000 0.06907 0.12439 = 0.15214 -0.04684 0.02268 -0.01381 AFIX 43 H44A 2 0.773742 0.550900 0.452542 10.72000 -1.20000 AFIX 0 O4A 5 0.331810 0.878208 0.093676 41.00000 0.06931 0.04395 = 0.05505 -0.00168 0.02121 0.00071 F6A 3 0.339907 0.835355 0.252070 41.00000 0.09597 0.07283 = 0.05144 0.01974 0.02992 -0.01045 PART 0 PART 2 C19A 1 0.289924 0.547530 0.430906 -21.00000 0.06482 0.01937 = 0.05211 0.00877 0.02038 -0.01299 AFIX 13 H19A 2 0.279265 0.513242 0.393901 -21.00000 -1.20000 AFIX 0 O2B 5 0.216488 0.286510 0.263088 -31.00000 0.05446 0.02862 = 0.11696 0.00880 0.02712 0.01577 S1B 8 0.171745 0.357369 0.283787 -31.00000 0.04572 0.08093 = 0.05017 0.01223 0.00854 0.00516 O3B 5 0.220903 0.447730 0.309386 -31.00000 0.04905 0.05802 = 0.08552 -0.00776 -0.00665 0.04825 O1B 5 0.123175 0.307294 0.314194 -31.00000 0.11200 0.14743 = 0.09648 0.06128 0.05254 0.01942 C38B 1 0.106017 0.404433 0.211581 -31.00000 0.03435 0.04082 = 0.05879 -0.01456 -0.00312 0.02907 F1B 3 0.060544 0.471596 0.214987 -31.00000 0.02912 0.04206 = 0.06385 -0.02175 -0.01363 0.02297 F3B 3 0.055344 0.329761 0.184655 -31.00000 0.07306 0.07115 = 0.10426 -0.02309 -0.03722 -0.00436 F2B 3 0.143230 0.422677 0.186564 -31.00000 0.04185 0.11967 = 0.04297 -0.00987 -0.01201 0.00924 F8B 3 0.836396 0.866837 0.416873 10.28000 0.07219 0.10482 = 0.15184 -0.01794 0.06124 -0.00513 F7B 3 0.855939 0.778789 0.530394 10.28000 0.19145 0.18605 = 0.14891 0.00060 0.06095 -0.01821 AFIX 66 C41B 1 0.828821 0.753949 0.432697 10.28000 0.06926 0.12192 = 0.12162 0.03809 0.02381 0.02516 C40B 1 0.832816 0.724127 0.489524 10.28000 0.08752 0.13520 = 0.12486 0.02476 0.03576 0.01562 C45B 1 0.801726 0.639800 0.497656 10.28000 0.07472 0.13248 = 0.12976 0.04198 0.05807 0.02700 AFIX 43 H45B 2 0.804399 0.619848 0.535678 10.28000 -1.20000 AFIX 65 C44B 1 0.766640 0.585294 0.448962 10.28000 0.09038 0.13831 = 0.14688 0.04164 0.04500 0.00641 AFIX 43 H44B 2 0.745838 0.528874 0.454403 10.28000 -1.20000 AFIX 65 C43B 1 0.762644 0.615115 0.392135 10.28000 0.08288 0.10277 = 0.14698 0.03887 0.04792 0.00397 AFIX 43 H43B 2 0.739169 0.578647 0.359555 10.28000 -1.20000 AFIX 65 C42B 1 0.793734 0.699441 0.384002 10.28000 0.05569 0.09552 = 0.12572 0.04503 0.02933 0.01088 AFIX 43 H42B 2 0.791061 0.719393 0.345980 10.28000 -1.20000 AFIX 0 PART 0 PART 1 S2A 8 0.291809 0.882986 0.139929 41.00000 0.05205 0.04210 = 0.04832 -0.00610 0.01770 -0.00693 PART 0 PART 2 O5B 5 0.337311 0.812780 0.262562 -41.00000 0.08396 0.05292 = 0.05254 0.00924 0.02405 -0.01871 C39B 1 0.321249 0.811179 0.149138 -41.00000 0.05597 0.03511 = 0.04867 -0.00453 0.02409 -0.00253 F6B 3 0.238436 0.801546 0.136405 -41.00000 0.04990 0.05355 = 0.06417 -0.00972 0.01448 -0.00157 F4B 3 0.342281 0.852368 0.105887 -41.00000 0.07400 0.04666 = 0.04915 0.00103 0.02469 -0.00045 F5B 3 0.351211 0.727098 0.154920 -41.00000 0.07362 0.03655 = 0.07673 -0.00424 0.02851 0.00064 S2B 8 0.360950 0.870305 0.220412 -41.00000 0.07173 0.04966 = 0.04276 -0.00300 0.01340 -0.02079 O6B 5 0.444207 0.893492 0.228655 -41.00000 0.06683 0.06298 = 0.05418 -0.00068 0.00829 -0.02155 O4B 5 0.315422 0.954927 0.207931 -41.00000 0.08572 0.04388 = 0.06500 -0.00922 0.02479 -0.00345 PART 0 PART -1 O7 5 0.069713 0.909117 -0.005935 10.50000 0.16938 0.26420 = 0.08720 0.02351 0.03285 0.03824 C46 1 0.051915 0.936489 0.045983 10.50000 0.11310 0.29063 = 0.09491 0.07248 0.04861 0.07313 AFIX 23 H46A 2 0.103796 0.948266 0.076406 10.50000 -1.20000 H46B 2 0.022531 0.888799 0.060033 10.50000 -1.20000 AFIX 0 C47 1 -0.001935 1.021309 0.034976 10.50000 0.07139 0.26352 = 0.10058 0.04253 -0.02860 0.03372 AFIX 23 H47A 2 0.030170 1.073709 0.052655 10.50000 -1.20000 H47B 2 -0.050075 1.015130 0.050336 10.50000 -1.20000 AFIX 0 C48 1 -0.028358 1.026940 -0.032775 10.50000 0.08630 0.26655 = 0.09894 0.09051 0.02427 -0.00207 AFIX 23 H48A 2 -0.001848 1.077754 -0.046114 10.50000 -1.20000 H48B 2 -0.088635 1.033226 -0.047942 10.50000 -1.20000 AFIX 0 C49 1 0.001154 0.937640 -0.053700 10.50000 0.12838 0.30372 = 0.11306 0.08521 0.04816 0.04329 AFIX 23 H49A 2 -0.043442 0.893369 -0.061873 10.50000 -1.20000 H49B 2 0.018727 0.946765 -0.089340 10.50000 -1.20000 AFIX 0 HKLF 4 REM jjw1291_a.res in P2(1)/c REM wR2 = 0.1512, GooF = S = 1.020, Restrained GooF = 1.006 for all data REM R1 = 0.0531 for 8245 Fo > 4sig(Fo) and 0.0636 for all 9837 data REM 883 parameters refined using 1140 restraints END WGHT 0.0972 3.1533 REM Highest difference peak 1.414, deepest hole -0.755, 1-sigma level 0.090 Q1 1 0.3109 0.6919 0.4585 11.00000 0.05 1.41 Q2 1 0.2642 0.6923 0.3993 11.00000 0.05 0.86 Q3 1 0.3275 0.6991 0.3913 11.00000 0.05 0.83 Q4 1 0.3367 0.6620 0.3915 11.00000 0.05 0.75 Q5 1 0.2463 0.8187 0.4287 11.00000 0.05 0.64 Q6 1 0.3188 0.7748 0.4296 11.00000 0.05 0.62 Q7 1 0.3850 0.6807 0.4601 11.00000 0.05 0.60 Q8 1 -0.0251 0.8807 -0.0887 11.00000 0.05 0.59 Q9 1 0.1036 0.8583 0.0264 11.00000 0.05 0.57 Q10 1 0.7847 0.6425 0.4295 11.00000 0.05 0.55 Q11 1 0.3885 0.8148 0.4149 11.00000 0.05 0.53 Q12 1 0.1267 0.3797 0.3314 11.00000 0.05 0.52 Q13 1 0.3695 0.8957 0.3830 11.00000 0.05 0.51 Q14 1 0.3706 0.9002 0.4563 11.00000 0.05 0.51 ; _shelx_res_checksum 90173 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.484 _oxdiff_exptl_absorpt_empirical_full_min 0.747 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.32324(2) 0.68781(2) 0.42653(2) 0.03123(11) Uani 1 1 d . . . . . P1 P 0.26184(6) 0.82854(6) 0.40102(4) 0.0324(2) Uani 1 1 d . . . . . P3 P 0.43908(6) 0.78018(6) 0.43318(4) 0.0290(2) Uani 1 1 d . . . . . P2 P 0.37478(6) 0.90734(6) 0.41810(4) 0.0336(2) Uani 1 1 d . . . . . S1A S 0.16568(15) 0.38433(14) 0.30450(14) 0.0499(6) Uani 0.795(7) 1 d . U P A 1 C39A C 0.3677(7) 0.8303(7) 0.2020(5) 0.0613(15) Uani 0.581(3) 1 d D U P B 1 N3 N 0.5552(2) 0.8357(2) 0.37043(14) 0.0326(7) Uani 1 1 d . . . . . O6A O 0.2191(6) 0.8292(6) 0.1330(6) 0.061(2) Uani 0.581(3) 1 d D U P B 1 N4 N 0.5135(2) 0.6985(2) 0.34891(14) 0.0336(7) Uani 1 1 d . . . . . F5A F 0.3828(5) 0.7468(4) 0.1940(3) 0.0777(15) Uani 0.581(3) 1 d D U P B 1 F4A F 0.4428(6) 0.8692(6) 0.2157(4) 0.071(2) Uani 0.581(3) 1 d D U P B 1 F1A F 0.0380(3) 0.3302(3) 0.2189(2) 0.0701(13) Uani 0.795(7) 1 d . U P A 1 N2 N 0.1580(2) 0.7937(2) 0.28224(15) 0.0380(7) Uani 1 1 d . . . . . N1 N 0.1780(2) 0.9365(2) 0.30137(15) 0.0381(7) Uani 1 1 d . . . . . O5A O 0.2836(4) 0.9729(4) 0.1595(3) 0.0556(14) Uani 0.581(3) 1 d D U P B 1 O1A O 0.2395(5) 0.4327(6) 0.3028(5) 0.060(2) Uani 0.795(7) 1 d . U P A 1 C25 C 0.5935(3) 0.8058(3) 0.32879(18) 0.0368(9) Uani 1 1 d . . . . . C27 C 0.5677(3) 0.7195(3) 0.31545(17) 0.0380(9) Uani 1 1 d . . . . . C22 C 0.5708(3) 0.9231(2) 0.40312(19) 0.0369(8) Uani 1 1 d . . . . . H22 H 0.531653 0.926003 0.427440 0.044 Uiso 1 1 calc R U . . . C33 C 0.5829(3) 0.7030(3) 0.51224(18) 0.0394(9) Uani 1 1 d . . . . . H33A H 0.612532 0.709961 0.482327 0.047 Uiso 1 1 calc R U . . . H33B H 0.553882 0.645721 0.505717 0.047 Uiso 1 1 calc R U . . . C21 C 0.5063(2) 0.7703(2) 0.38223(16) 0.0303(8) Uani 1 1 d . . . . . C34 C 0.6455(3) 0.7038(3) 0.57376(18) 0.0410(9) Uani 1 1 d . . . . . H34A H 0.682745 0.652615 0.577499 0.049 Uiso 1 1 calc R U . . . H34B H 0.679184 0.757981 0.578208 0.049 Uiso 1 1 calc R U . . . C5 C 0.1279(3) 0.9285(3) 0.24376(19) 0.0408(9) Uani 1 1 d . . . . . C32 C 0.5193(2) 0.7788(3) 0.50619(16) 0.0326(8) Uani 1 1 d . . . . . H32 H 0.549760 0.835950 0.510673 0.039 Uiso 1 1 calc R U . . . F2A F 0.0761(9) 0.4590(9) 0.2081(6) 0.173(6) Uani 0.795(7) 1 d . U P A 1 C18 C 0.3703(3) 0.5561(3) 0.4624(2) 0.0501(11) Uani 1 1 d . U . . . H18A H 0.372216 0.509853 0.433693 0.060 Uiso 0.369(11) 1 calc R U P C 1 H18B H 0.418933 0.556157 0.496793 0.060 Uiso 0.369(11) 1 calc R U P C 1 H18C H 0.411527 0.528211 0.445896 0.060 Uiso 0.631(11) 1 calc R U P C 2 H18D H 0.382415 0.548821 0.505018 0.060 Uiso 0.631(11) 1 calc R U P C 2 C29 C 0.4738(3) 0.6099(3) 0.35231(18) 0.0423(10) Uani 1 1 d . . . . . H29 H 0.438104 0.617542 0.378835 0.051 Uiso 1 1 calc R U . . . C26 C 0.6482(3) 0.8604(3) 0.3014(2) 0.0474(10) Uani 1 1 d . . . . . H26A H 0.614342 0.900945 0.272787 0.071 Uiso 1 1 calc R U . . . H26B H 0.678312 0.821159 0.282155 0.071 Uiso 1 1 calc R U . . . H26C H 0.687292 0.894159 0.331703 0.071 Uiso 1 1 calc R U . . . O2A O 0.1112(4) 0.4264(4) 0.3331(2) 0.0757(16) Uani 0.795(7) 1 d . U P A 1 C8 C 0.0612(3) 0.7979(3) 0.1755(2) 0.0502(11) Uani 1 1 d . . . . . H8A H 0.023784 0.842304 0.152764 0.075 Uiso 1 1 calc R U . . . H8B H 0.029297 0.749525 0.185313 0.075 Uiso 1 1 calc R U . . . H8C H 0.096360 0.775129 0.152606 0.075 Uiso 1 1 calc R U . . . C7 C 0.1150(3) 0.8403(3) 0.23187(18) 0.0419(9) Uani 1 1 d . . . . . C1 C 0.1962(3) 0.8532(3) 0.32477(18) 0.0366(8) Uani 1 1 d . . . . . C10 C 0.1637(3) 0.6944(3) 0.2889(2) 0.0418(10) Uani 1 1 d . . . . . H10 H 0.207792 0.681611 0.325519 0.050 Uiso 1 1 calc R U . . . C24 C 0.6584(3) 0.9251(3) 0.4454(2) 0.0452(10) Uani 1 1 d . . . . . H24A H 0.669269 0.869449 0.466971 0.068 Uiso 1 1 calc R U . . . H24B H 0.662790 0.974020 0.472798 0.068 Uiso 1 1 calc R U . . . H24C H 0.698494 0.933026 0.423354 0.068 Uiso 1 1 calc R U . . . C28 C 0.5905(3) 0.6574(3) 0.2725(2) 0.0497(11) Uani 1 1 d . . . . . H28A H 0.613983 0.603245 0.292525 0.074 Uiso 1 1 calc R U . . . H28B H 0.630787 0.686044 0.256151 0.074 Uiso 1 1 calc R U . . . H28C H 0.541209 0.643115 0.241098 0.074 Uiso 1 1 calc R U . . . C13 C 0.2331(3) 0.8464(3) 0.51204(19) 0.0423(9) Uani 1 1 d . . . . . H13A H 0.237234 0.781539 0.516392 0.051 Uiso 1 1 calc R U . . . H13B H 0.289146 0.871188 0.525348 0.051 Uiso 1 1 calc R U . . . C12 C 0.1939(3) 0.8704(3) 0.44634(18) 0.0390(9) Uani 1 1 d . . . . . H12 H 0.191468 0.936099 0.443080 0.047 Uiso 1 1 calc R U . . . F7A F 0.8735(4) 0.8627(4) 0.5179(3) 0.0931(16) Uani 0.72 1 d . U P D 1 C35 C 0.6024(3) 0.7002(3) 0.6226(2) 0.0486(11) Uani 1 1 d . . . . . H35A H 0.643968 0.706089 0.660782 0.058 Uiso 1 1 calc R U . . . H35B H 0.575199 0.642344 0.621704 0.058 Uiso 1 1 calc R U . . . O3A O 0.1804(5) 0.2907(4) 0.3173(4) 0.093(2) Uani 0.795(7) 1 d . U P A 1 C2 C 0.2065(3) 1.0213(3) 0.3336(2) 0.0421(9) Uani 1 1 d . . . . . H2 H 0.242920 1.004427 0.372639 0.051 Uiso 1 1 calc R U . . . C20 C 0.2252(3) 0.5981(3) 0.4381(2) 0.0520(11) Uani 1 1 d . U . . . H20A H 0.186412 0.623233 0.457965 0.062 Uiso 0.369(11) 1 calc R U P C 1 H20B H 0.198322 0.560224 0.404555 0.062 Uiso 0.369(11) 1 calc R U P C 1 H20C H 0.216119 0.597130 0.477150 0.062 Uiso 0.631(11) 1 calc R U P C 2 H20D H 0.173729 0.596501 0.405977 0.062 Uiso 0.631(11) 1 calc R U P C 2 C23 C 0.5510(3) 1.0026(3) 0.3606(2) 0.0483(11) Uani 1 1 d . . . . . H23A H 0.594167 1.008532 0.340920 0.072 Uiso 1 1 calc R U . . . H23B H 0.548346 1.056564 0.382453 0.072 Uiso 1 1 calc R U . . . H23C H 0.498156 0.992871 0.331716 0.072 Uiso 1 1 calc R U . . . C14 C 0.1801(3) 0.8835(4) 0.5502(2) 0.0533(12) Uani 1 1 d . . . . . H14A H 0.180244 0.948648 0.548576 0.064 Uiso 1 1 calc R U . . . H14B H 0.204462 0.865465 0.591061 0.064 Uiso 1 1 calc R U . . . C36 C 0.5376(3) 0.7747(4) 0.61596(19) 0.0515(11) Uani 1 1 d . . . . . H36A H 0.508259 0.767395 0.646005 0.062 Uiso 1 1 calc R U . . . H36B H 0.565876 0.832400 0.622295 0.062 Uiso 1 1 calc R U . . . C17 C 0.1044(3) 0.8347(4) 0.4247(2) 0.0599(13) Uani 1 1 d . . . . . H17A H 0.105021 0.769524 0.426152 0.072 Uiso 1 1 calc R U . . . H17B H 0.079630 0.852972 0.383928 0.072 Uiso 1 1 calc R U . . . C6 C 0.0970(3) 1.0049(3) 0.2014(2) 0.0541(12) Uani 1 1 d . . . . . H6A H 0.137470 1.017798 0.180327 0.081 Uiso 1 1 calc R U . . . H6B H 0.089104 1.057228 0.223209 0.081 Uiso 1 1 calc R U . . . H6C H 0.044755 0.988540 0.173749 0.081 Uiso 1 1 calc R U . . . C4 C 0.2598(3) 1.0768(3) 0.3037(2) 0.0549(12) Uani 1 1 d . . . . . H4A H 0.303469 1.039807 0.296818 0.082 Uiso 1 1 calc R U . . . H4B H 0.284097 1.126330 0.328762 0.082 Uiso 1 1 calc R U . . . H4C H 0.225358 1.099182 0.266477 0.082 Uiso 1 1 calc R U . . . C37 C 0.4747(3) 0.7737(4) 0.55504(18) 0.0470(11) Uani 1 1 d . . . . . H37A H 0.436942 0.824374 0.551455 0.056 Uiso 1 1 calc R U . . . H37B H 0.441766 0.718985 0.550373 0.056 Uiso 1 1 calc R U . . . C9 C 0.1896(3) 0.6502(3) 0.2380(2) 0.0544(12) Uani 1 1 d . . . . . H9A H 0.210484 0.590839 0.249515 0.082 Uiso 1 1 calc R U . . . H9B H 0.232695 0.685511 0.228750 0.082 Uiso 1 1 calc R U . . . H9C H 0.142045 0.646631 0.203680 0.082 Uiso 1 1 calc R U . . . C30 C 0.5399(4) 0.5408(3) 0.3809(2) 0.0552(12) Uani 1 1 d . . . . . H30A H 0.513046 0.486034 0.387190 0.083 Uiso 1 1 calc R U . . . H30B H 0.573479 0.563379 0.418343 0.083 Uiso 1 1 calc R U . . . H30C H 0.574842 0.529410 0.355418 0.083 Uiso 1 1 calc R U . . . C11 C 0.0822(3) 0.6562(3) 0.2966(2) 0.0553(12) Uani 1 1 d . . . . . H11A H 0.037181 0.668612 0.261762 0.083 Uiso 1 1 calc R U . . . H11B H 0.070355 0.683637 0.330441 0.083 Uiso 1 1 calc R U . . . H11C H 0.087654 0.592408 0.302565 0.083 Uiso 1 1 calc R U . . . C3 C 0.1329(3) 1.0735(3) 0.3446(2) 0.0531(12) Uani 1 1 d . . . . . H3A H 0.096131 1.092715 0.307351 0.080 Uiso 1 1 calc R U . . . H3B H 0.153682 1.125130 0.368785 0.080 Uiso 1 1 calc R U . . . H3C H 0.102867 1.035413 0.364532 0.080 Uiso 1 1 calc R U . . . F3A F 0.1459(5) 0.3481(10) 0.1928(4) 0.174(5) Uani 0.795(7) 1 d . U P A 1 C16 C 0.0515(4) 0.8713(5) 0.4639(3) 0.0754(18) Uani 1 1 d . . . . . H16A H 0.046390 0.936022 0.459157 0.091 Uiso 1 1 calc R U . . . H16B H -0.004286 0.845721 0.450882 0.091 Uiso 1 1 calc R U . . . C38A C 0.1037(7) 0.3817(7) 0.2272(4) 0.062(2) Uani 0.795(7) 1 d . U P A 1 C31 C 0.4172(4) 0.5797(4) 0.2927(2) 0.0610(13) Uani 1 1 d . . . . . H31A H 0.450532 0.554320 0.269384 0.092 Uiso 1 1 calc R U . . . H31B H 0.386544 0.630377 0.272303 0.092 Uiso 1 1 calc R U . . . H31C H 0.378592 0.535226 0.298935 0.092 Uiso 1 1 calc R U . . . C15 C 0.0899(4) 0.8493(5) 0.5288(3) 0.0703(16) Uani 1 1 d . . . . . H15A H 0.089139 0.784695 0.534427 0.084 Uiso 1 1 calc R U . . . H15B H 0.056837 0.876781 0.552235 0.084 Uiso 1 1 calc R U . . . F8A F 0.8136(8) 0.8196(8) 0.4020(5) 0.156(5) Uani 0.72 1 d . U P D 1 C19B C 0.2976(8) 0.5695(7) 0.4726(6) 0.043(2) Uani 0.369(11) 1 d . U P C 1 H19B H 0.303421 0.581636 0.514543 0.051 Uiso 0.369(11) 1 calc R U P C 1 C43A C 0.7882(5) 0.6753(7) 0.4220(3) 0.112(3) Uani 0.72 1 d G U P D 1 H43A H 0.767154 0.661840 0.381926 0.135 Uiso 0.72 1 calc R U P D 1 C42A C 0.8157(5) 0.7618(5) 0.4397(2) 0.089(3) Uani 0.72 1 d G U P D 1 C41A C 0.8472(4) 0.7819(3) 0.4996(3) 0.0642(18) Uani 0.72 1 d G U P D 1 C40A C 0.8512(4) 0.7154(4) 0.5419(2) 0.0657(19) Uani 0.72 1 d G U P D 1 H40A H 0.872215 0.728876 0.582004 0.079 Uiso 0.72 1 calc R U P D 1 C45A C 0.8236(6) 0.6289(4) 0.5243(3) 0.096(3) Uani 0.72 1 d G U P D 1 H45A H 0.826273 0.584419 0.552581 0.115 Uiso 0.72 1 calc R U P D 1 C44A C 0.7922(6) 0.6088(5) 0.4643(4) 0.117(4) Uani 0.72 1 d G U P D 1 H44A H 0.773742 0.550900 0.452542 0.140 Uiso 0.72 1 calc R U P D 1 O4A O 0.3318(7) 0.8782(6) 0.0937(4) 0.0553(19) Uani 0.581(3) 1 d D U P B 1 F6A F 0.3399(8) 0.8354(6) 0.2521(4) 0.0715(19) Uani 0.581(3) 1 d D U P B 1 C19A C 0.2899(5) 0.5475(4) 0.4309(4) 0.0446(18) Uani 0.631(11) 1 d . U P C 2 H19A H 0.279265 0.513242 0.393901 0.054 Uiso 0.631(11) 1 calc R U P C 2 O2B O 0.2165(12) 0.2865(11) 0.2631(10) 0.066(5) Uani 0.205(7) 1 d . U P A 2 S1B S 0.1717(6) 0.3574(10) 0.2838(5) 0.060(3) Uani 0.205(7) 1 d . U P A 2 O3B O 0.221(3) 0.448(3) 0.309(2) 0.069(9) Uani 0.205(7) 1 d . U P A 2 O1B O 0.123(2) 0.307(2) 0.3142(13) 0.114(9) Uani 0.205(7) 1 d . U P A 2 C38B C 0.106(2) 0.404(3) 0.2116(17) 0.048(5) Uani 0.205(7) 1 d . U P A 2 F1B F 0.0605(13) 0.4716(16) 0.2150(12) 0.050(5) Uani 0.205(7) 1 d . U P A 2 F3B F 0.0553(15) 0.3298(14) 0.1847(13) 0.095(7) Uani 0.205(7) 1 d . U P A 2 F2B F 0.1432(13) 0.4227(17) 0.1866(8) 0.073(5) Uani 0.205(7) 1 d . U P A 2 F8B F 0.8364(15) 0.8668(14) 0.4169(12) 0.104(6) Uani 0.28 1 d . U P E 2 F7B F 0.856(2) 0.779(2) 0.5304(13) 0.173(9) Uani 0.28 1 d . U P E 2 C41B C 0.8288(14) 0.7539(12) 0.4327(11) 0.105(6) Uani 0.28 1 d G U P E 2 C40B C 0.8328(15) 0.7241(17) 0.4895(9) 0.115(6) Uani 0.28 1 d G U P E 2 C45B C 0.8017(16) 0.6398(18) 0.4977(8) 0.106(6) Uani 0.28 1 d G U P E 2 H45B H 0.804399 0.619848 0.535678 0.128 Uiso 0.28 1 calc R U P E 2 C44B C 0.7666(17) 0.5853(13) 0.4490(11) 0.123(7) Uani 0.28 1 d G U P E 2 H44B H 0.745838 0.528874 0.454403 0.147 Uiso 0.28 1 calc R U P E 2 C43B C 0.7626(13) 0.6151(13) 0.3921(9) 0.108(6) Uani 0.28 1 d G U P E 2 H43B H 0.739169 0.578647 0.359555 0.129 Uiso 0.28 1 calc R U P E 2 C42B C 0.7937(13) 0.6994(14) 0.3840(8) 0.092(5) Uani 0.28 1 d G U P E 2 H42B H 0.791061 0.719393 0.345980 0.110 Uiso 0.28 1 calc R U P E 2 S2A S 0.29181(13) 0.88299(13) 0.13993(9) 0.0467(5) Uani 0.581(3) 1 d D U P B 1 O5B O 0.3373(12) 0.8128(10) 0.2626(7) 0.062(2) Uani 0.419(3) 1 d D U P B 2 C39B C 0.3212(7) 0.8112(6) 0.1491(4) 0.0447(15) Uani 0.419(3) 1 d D U P B 2 F6B F 0.2384(6) 0.8015(7) 0.1364(6) 0.056(2) Uani 0.419(3) 1 d D U P B 2 F4B F 0.3423(8) 0.8524(7) 0.1059(5) 0.055(2) Uani 0.419(3) 1 d D U P B 2 F5B F 0.3512(5) 0.7271(4) 0.1549(4) 0.0608(16) Uani 0.419(3) 1 d D U P B 2 S2B S 0.3610(2) 0.8703(2) 0.22041(14) 0.0552(8) Uani 0.419(3) 1 d D U P B 2 O6B O 0.4442(9) 0.8935(10) 0.2287(7) 0.063(3) Uani 0.419(3) 1 d D U P B 2 O4B O 0.3154(6) 0.9549(5) 0.2079(4) 0.0641(19) Uani 0.419(3) 1 d D U P B 2 O7 O 0.0697(11) 0.9091(14) -0.0059(6) 0.174(7) Uani 0.5 1 d D U P F -1 C46 C 0.0519(19) 0.936(2) 0.0460(8) 0.162(9) Uani 0.5 1 d D U P F -1 H46A H 0.103796 0.948266 0.076406 0.195 Uiso 0.5 1 calc R U P F -1 H46B H 0.022531 0.888799 0.060033 0.195 Uiso 0.5 1 calc R U P F -1 C47 C -0.0019(17) 1.0213(18) 0.0350(8) 0.156(9) Uani 0.5 1 d D U P F -1 H47A H 0.030170 1.073709 0.052655 0.187 Uiso 0.5 1 calc R U P F -1 H47B H -0.050075 1.015130 0.050336 0.187 Uiso 0.5 1 calc R U P F -1 C48 C -0.0284(15) 1.0269(17) -0.0328(8) 0.151(8) Uani 0.5 1 d D U P F -1 H48A H -0.001848 1.077754 -0.046114 0.181 Uiso 0.5 1 calc R U P F -1 H48B H -0.088635 1.033226 -0.047942 0.181 Uiso 0.5 1 calc R U P F -1 C49 C 0.0012(18) 0.938(2) -0.0537(8) 0.179(10) Uani 0.5 1 d D U P F -1 H49A H -0.043442 0.893369 -0.061873 0.215 Uiso 0.5 1 calc R U P F -1 H49B H 0.018727 0.946765 -0.089340 0.215 Uiso 0.5 1 calc R U P F -1 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 0.03801(18) 0.02298(16) 0.03081(16) 0.00250(10) 0.00650(12) -0.00190(10) P1 0.0328(5) 0.0254(4) 0.0367(5) 0.0042(4) 0.0060(4) -0.0002(4) P3 0.0340(5) 0.0226(4) 0.0293(4) 0.0001(3) 0.0071(4) 0.0014(4) P2 0.0327(5) 0.0221(4) 0.0436(5) 0.0000(4) 0.0070(4) 0.0007(4) S1A 0.0466(10) 0.0356(10) 0.0584(14) 0.0021(8) -0.0002(9) -0.0025(7) C39A 0.074(3) 0.053(3) 0.059(3) 0.005(3) 0.023(3) -0.005(3) N3 0.0381(18) 0.0253(15) 0.0337(16) 0.0021(13) 0.0090(13) 0.0011(13) O6A 0.058(4) 0.053(4) 0.074(4) -0.011(4) 0.020(3) -0.006(3) N4 0.045(2) 0.0267(16) 0.0281(15) -0.0006(12) 0.0082(14) 0.0032(14) F5A 0.090(4) 0.057(3) 0.095(4) 0.020(3) 0.040(3) 0.010(3) F4A 0.069(3) 0.069(5) 0.067(5) 0.007(3) 0.005(3) -0.015(3) F1A 0.056(3) 0.084(3) 0.066(3) -0.025(2) 0.010(2) -0.021(2) N2 0.0327(18) 0.0366(18) 0.0404(18) 0.0048(14) 0.0034(14) -0.0010(14) N1 0.0394(19) 0.0329(17) 0.0421(18) 0.0071(14) 0.0115(15) 0.0032(14) O5A 0.064(4) 0.045(3) 0.061(3) -0.004(2) 0.021(3) 0.004(3) O1A 0.044(5) 0.055(5) 0.072(4) 0.004(4) -0.002(3) -0.001(4) C25 0.041(2) 0.036(2) 0.0333(19) 0.0068(16) 0.0105(17) 0.0064(17) C27 0.048(2) 0.037(2) 0.0291(18) 0.0050(16) 0.0110(17) 0.0082(18) C22 0.038(2) 0.0243(18) 0.049(2) -0.0022(16) 0.0133(17) -0.0025(16) C33 0.046(2) 0.033(2) 0.035(2) -0.0004(16) 0.0036(17) 0.0046(18) C21 0.035(2) 0.0252(18) 0.0295(17) 0.0018(14) 0.0069(15) 0.0035(15) C34 0.044(2) 0.035(2) 0.038(2) 0.0026(17) 0.0015(18) 0.0079(18) C5 0.036(2) 0.042(2) 0.042(2) 0.0123(18) 0.0064(17) 0.0045(18) C32 0.035(2) 0.0305(19) 0.0304(18) -0.0021(15) 0.0055(15) 0.0016(16) F2A 0.191(12) 0.102(7) 0.148(10) 0.034(6) -0.082(8) -0.013(6) C18 0.064(3) 0.0230(19) 0.063(3) 0.0193(18) 0.018(2) 0.0022(19) C29 0.066(3) 0.0269(19) 0.039(2) -0.0082(16) 0.022(2) -0.0054(19) C26 0.049(3) 0.050(3) 0.047(2) 0.007(2) 0.021(2) -0.001(2) O2A 0.072(4) 0.080(4) 0.073(3) -0.027(3) 0.018(3) -0.015(3) C8 0.047(3) 0.060(3) 0.040(2) 0.001(2) 0.006(2) 0.002(2) C7 0.037(2) 0.051(3) 0.037(2) 0.0049(19) 0.0086(17) 0.0021(19) C1 0.036(2) 0.0279(19) 0.044(2) 0.0034(16) 0.0090(17) 0.0002(16) C10 0.041(2) 0.030(2) 0.046(2) 0.0023(16) -0.0003(18) -0.0063(17) C24 0.048(3) 0.038(2) 0.051(2) -0.0058(19) 0.015(2) -0.0063(19) C28 0.069(3) 0.047(2) 0.040(2) 0.000(2) 0.026(2) 0.008(2) C13 0.046(3) 0.035(2) 0.046(2) 0.0038(18) 0.0137(19) 0.0000(18) C12 0.036(2) 0.037(2) 0.043(2) 0.0034(17) 0.0104(17) 0.0012(17) F7A 0.091(4) 0.066(3) 0.133(5) 0.020(3) 0.048(4) 0.003(3) C35 0.050(3) 0.055(3) 0.035(2) 0.0077(19) 0.0018(19) -0.002(2) O3A 0.078(5) 0.039(3) 0.133(6) 0.012(3) -0.019(4) -0.003(3) C2 0.040(2) 0.030(2) 0.053(2) 0.0071(18) 0.0094(19) 0.0039(17) C20 0.054(3) 0.038(2) 0.064(3) 0.012(2) 0.017(2) -0.016(2) C23 0.053(3) 0.032(2) 0.061(3) 0.006(2) 0.018(2) 0.0005(19) C14 0.057(3) 0.056(3) 0.051(3) 0.004(2) 0.023(2) 0.003(2) C36 0.047(3) 0.076(3) 0.032(2) 0.000(2) 0.0115(19) 0.005(2) C17 0.048(3) 0.079(4) 0.053(3) -0.002(3) 0.014(2) -0.008(3) C6 0.052(3) 0.054(3) 0.053(3) 0.019(2) 0.008(2) 0.016(2) C4 0.058(3) 0.038(2) 0.066(3) 0.011(2) 0.014(2) -0.005(2) C37 0.041(2) 0.066(3) 0.034(2) 0.001(2) 0.0113(18) 0.005(2) C9 0.060(3) 0.039(2) 0.063(3) -0.002(2) 0.016(2) -0.003(2) C30 0.082(4) 0.027(2) 0.057(3) 0.0045(19) 0.019(3) -0.002(2) C11 0.061(3) 0.050(3) 0.054(3) 0.000(2) 0.013(2) -0.018(2) C3 0.051(3) 0.041(2) 0.064(3) 0.002(2) 0.011(2) 0.012(2) F3A 0.079(5) 0.342(13) 0.114(5) -0.107(8) 0.048(4) -0.034(7) C16 0.037(3) 0.122(6) 0.070(3) -0.006(4) 0.018(3) -0.001(3) C38A 0.057(4) 0.073(6) 0.059(5) -0.005(3) 0.020(3) -0.017(4) C31 0.066(4) 0.050(3) 0.062(3) -0.013(2) 0.009(3) -0.017(3) C15 0.065(4) 0.086(4) 0.070(3) -0.007(3) 0.036(3) -0.011(3) F8A 0.155(10) 0.220(11) 0.112(7) 0.074(7) 0.069(7) 0.079(8) C19B 0.061(5) 0.022(4) 0.049(5) 0.016(4) 0.021(4) -0.008(4) C43A 0.070(6) 0.167(7) 0.091(7) -0.043(5) 0.007(6) 0.031(6) C42A 0.067(6) 0.141(6) 0.065(4) 0.024(4) 0.030(4) 0.049(5) C41A 0.055(5) 0.074(4) 0.072(4) 0.018(4) 0.032(4) 0.013(4) C40A 0.071(5) 0.054(4) 0.084(5) 0.016(4) 0.041(4) 0.007(4) C45A 0.086(8) 0.076(5) 0.131(7) -0.009(6) 0.040(7) -0.007(5) C44A 0.069(7) 0.124(8) 0.152(8) -0.047(6) 0.023(7) -0.014(6) O4A 0.069(4) 0.044(4) 0.055(4) -0.002(3) 0.021(3) 0.001(3) F6A 0.096(4) 0.073(5) 0.051(3) 0.020(3) 0.030(3) -0.010(4) C19A 0.065(4) 0.019(3) 0.052(4) 0.009(3) 0.020(3) -0.013(3) O2B 0.054(11) 0.029(7) 0.117(15) 0.009(8) 0.027(10) 0.016(7) S1B 0.046(4) 0.081(7) 0.050(5) 0.012(4) 0.009(3) 0.005(4) O3B 0.049(14) 0.058(11) 0.086(18) -0.008(10) -0.007(11) 0.048(9) O1B 0.112(19) 0.15(2) 0.096(16) 0.061(14) 0.053(14) 0.019(15) C38B 0.034(9) 0.041(9) 0.059(11) -0.015(7) -0.003(7) 0.029(6) F1B 0.029(7) 0.042(8) 0.064(10) -0.022(7) -0.014(6) 0.023(6) F3B 0.073(12) 0.071(9) 0.104(15) -0.023(10) -0.037(11) -0.004(8) F2B 0.042(8) 0.120(13) 0.043(7) -0.010(8) -0.012(6) 0.009(8) F8B 0.072(11) 0.105(10) 0.152(17) -0.018(9) 0.061(11) -0.005(9) F7B 0.19(2) 0.186(18) 0.149(14) 0.001(14) 0.061(17) -0.018(18) C41B 0.069(13) 0.122(11) 0.122(10) 0.038(9) 0.024(11) 0.025(11) C40B 0.088(12) 0.135(11) 0.125(10) 0.025(9) 0.036(10) 0.016(10) C45B 0.075(13) 0.132(11) 0.130(13) 0.042(10) 0.058(11) 0.027(10) C44B 0.090(15) 0.138(13) 0.147(13) 0.042(10) 0.045(12) 0.006(13) C43B 0.083(14) 0.103(12) 0.147(12) 0.039(11) 0.048(12) 0.004(11) C42B 0.056(11) 0.096(10) 0.126(11) 0.045(9) 0.029(11) 0.011(9) S2A 0.0521(11) 0.0421(10) 0.0483(10) -0.0061(8) 0.0177(8) -0.0069(8) O5B 0.084(5) 0.053(5) 0.053(5) 0.009(4) 0.024(4) -0.019(4) C39B 0.056(3) 0.035(3) 0.049(3) -0.005(3) 0.024(3) -0.003(3) F6B 0.050(4) 0.054(5) 0.064(4) -0.010(4) 0.014(3) -0.002(3) F4B 0.074(4) 0.047(5) 0.049(4) 0.001(3) 0.025(3) 0.000(4) F5B 0.074(4) 0.037(3) 0.077(4) -0.004(3) 0.029(3) 0.001(3) S2B 0.0717(18) 0.0497(17) 0.0428(15) -0.0030(13) 0.0134(13) -0.0208(14) O6B 0.067(4) 0.063(6) 0.054(5) -0.001(4) 0.008(4) -0.022(4) O4B 0.086(4) 0.044(4) 0.065(4) -0.009(3) 0.025(4) -0.003(3) O7 0.169(14) 0.264(19) 0.087(7) 0.024(10) 0.033(8) 0.038(12) C46 0.113(15) 0.29(3) 0.095(9) 0.072(13) 0.049(11) 0.073(15) C47 0.071(13) 0.26(3) 0.101(9) 0.043(13) -0.029(11) 0.034(13) C48 0.086(18) 0.27(3) 0.099(10) 0.091(13) 0.024(10) -0.002(14) C49 0.128(16) 0.30(3) 0.113(10) 0.085(14) 0.048(11) 0.043(18) 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' 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 10 -1 0 0.0137 -10 1 0 0.0137 0 1 -5 0.0097 0 -1 5 0.0097 0 1 0 0.0799 0 -1 0 0.0799 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 P3 77.47(3) . . ? C18 Pd1 P1 170.31(14) . . ? C18 Pd1 P3 107.52(14) . . ? C20 Pd1 P1 106.97(14) . . ? C20 Pd1 P3 169.29(14) . . ? C20 Pd1 C18 66.69(19) . . ? C19B Pd1 P1 136.3(3) . . ? C19B Pd1 P3 135.8(4) . . ? C19B Pd1 C18 35.0(4) . . ? C19B Pd1 C20 35.3(4) . . ? C19A Pd1 P1 140.9(2) . . ? C19A Pd1 P3 141.2(2) . . ? C19A Pd1 C18 35.8(2) . . ? C19A Pd1 C20 36.5(2) . . ? P2 P1 Pd1 98.29(5) . . ? C1 P1 Pd1 121.52(13) . . ? C1 P1 P2 108.60(13) . . ? C1 P1 C12 101.43(19) . . ? C12 P1 Pd1 116.43(14) . . ? C12 P1 P2 110.40(14) . . ? P2 P3 Pd1 98.23(5) . . ? C21 P3 Pd1 122.95(12) . . ? C21 P3 P2 108.93(12) . . ? C32 P3 Pd1 114.96(13) . . ? C32 P3 P2 110.94(13) . . ? C32 P3 C21 100.82(17) . . ? P3 P2 P1 85.40(5) . . ? O1A S1A C38A 103.5(6) . . ? O2A S1A O1A 117.3(5) . . ? O2A S1A O3A 115.2(5) . . ? O2A S1A C38A 102.9(4) . . ? O3A S1A O1A 113.4(5) . . ? O3A S1A C38A 101.8(5) . . ? F5A C39A F4A 104.1(9) . . ? F5A C39A F6A 107.5(8) . . ? F5A C39A S2A 114.7(8) . . ? F4A C39A F6A 106.6(10) . . ? F4A C39A S2A 113.7(7) . . ? F6A C39A S2A 109.7(8) . . ? C25 N3 C22 126.5(3) . . ? C21 N3 C25 109.7(3) . . ? C21 N3 C22 123.4(3) . . ? C27 N4 C29 126.8(3) . . ? C21 N4 C27 109.2(3) . . ? C21 N4 C29 123.9(3) . . ? C7 N2 C10 126.2(4) . . ? C1 N2 C7 109.1(4) . . ? C1 N2 C10 124.7(4) . . ? C5 N1 C2 126.4(3) . . ? C1 N1 C5 108.9(4) . . ? C1 N1 C2 124.7(3) . . ? N3 C25 C26 126.0(4) . . ? C27 C25 N3 106.8(4) . . ? C27 C25 C26 127.1(4) . . ? N4 C27 C28 124.9(4) . . ? C25 C27 N4 107.1(3) . . ? C25 C27 C28 128.0(4) . . ? N3 C22 H22 106.9 . . ? N3 C22 C24 110.5(3) . . ? N3 C22 C23 111.4(3) . . ? C24 C22 H22 106.9 . . ? C24 C22 C23 113.9(4) . . ? C23 C22 H22 106.9 . . ? H33A C33 H33B 108.1 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 C34 110.8(3) . . ? N3 C21 P3 125.6(3) . . ? N3 C21 N4 107.2(3) . . ? N4 C21 P3 127.1(3) . . ? C33 C34 H34A 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C35 C34 C33 112.0(4) . . ? C35 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? N1 C5 C6 125.7(4) . . ? C7 C5 N1 107.7(4) . . ? C7 C5 C6 126.5(4) . . ? P3 C32 H32 107.9 . . ? C33 C32 P3 113.3(3) . . ? C33 C32 H32 107.9 . . ? C33 C32 C37 111.2(3) . . ? C37 C32 P3 108.6(3) . . ? C37 C32 H32 107.9 . . ? Pd1 C18 H18A 116.4 . . ? Pd1 C18 H18B 116.4 . . ? Pd1 C18 H18C 116.5 . . ? Pd1 C18 H18D 116.5 . . ? H18A C18 H18B 113.4 . . ? H18C C18 H18D 113.5 . . ? C19B C18 Pd1 71.7(5) . . ? C19B C18 H18A 116.4 . . ? C19B C18 H18B 116.4 . . ? C19A C18 Pd1 71.3(3) . . ? C19A C18 H18C 116.5 . . ? C19A C18 H18D 116.5 . . ? N4 C29 H29 106.8 . . ? N4 C29 C30 110.3(4) . . ? N4 C29 C31 112.6(4) . . ? C30 C29 H29 106.8 . . ? C30 C29 C31 113.1(4) . . ? C31 C29 H29 106.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? N2 C7 C8 125.3(4) . . ? C5 C7 N2 107.2(4) . . ? C5 C7 C8 127.5(4) . . ? N2 C1 P1 127.7(3) . . ? N2 C1 N1 107.1(4) . . ? N1 C1 P1 125.3(3) . . ? N2 C10 H10 107.2 . . ? N2 C10 C9 111.6(4) . . ? N2 C10 C11 110.5(4) . . ? C9 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C11 C10 C9 112.8(4) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? H13A C13 H13B 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C14 C13 C12 110.6(4) . . ? P1 C12 H12 107.8 . . ? C13 C12 P1 109.9(3) . . ? C13 C12 H12 107.8 . . ? C17 C12 P1 112.6(3) . . ? C17 C12 C13 110.6(4) . . ? C17 C12 H12 107.8 . . ? C34 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C34 C35 C36 111.5(4) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? N1 C2 H2 106.6 . . ? N1 C2 C4 111.8(4) . . ? N1 C2 C3 111.2(4) . . ? C4 C2 H2 106.6 . . ? C4 C2 C3 113.6(4) . . ? C3 C2 H2 106.6 . . ? Pd1 C20 H20A 116.4 . . ? Pd1 C20 H20B 116.4 . . ? Pd1 C20 H20C 116.5 . . ? Pd1 C20 H20D 116.5 . . ? H20A C20 H20B 113.4 . . ? H20C C20 H20D 113.5 . . ? C19B C20 Pd1 71.8(5) . . ? C19B C20 H20A 116.4 . . ? C19B C20 H20B 116.4 . . ? C19A C20 Pd1 71.2(3) . . ? C19A C20 H20C 116.5 . . ? C19A C20 H20D 116.5 . . ? 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 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C13 C14 C15 111.2(4) . . ? H14A C14 H14B 108.0 . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C35 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C37 C36 C35 111.8(4) . . ? C37 C36 H36A 109.3 . . ? C37 C36 H36B 109.3 . . ? C12 C17 H17A 109.6 . . ? C12 C17 H17B 109.6 . . ? C12 C17 C16 110.2(4) . . ? H17A C17 H17B 108.1 . . ? C16 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? 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 . . ? 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 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? C36 C37 C32 110.8(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 . . ? C17 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C15 C16 C17 112.0(5) . . ? C15 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? F1A C38A S1A 112.3(6) . . ? F1A C38A F3A 104.7(9) . . ? F2A C38A S1A 112.4(9) . . ? F2A C38A F1A 106.0(11) . . ? F2A C38A F3A 109.3(12) . . ? F3A C38A S1A 111.8(9) . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 C14 110.9(5) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? Pd1 C19B H19B 112.0 . . ? C18 C19B Pd1 73.3(5) . . ? C18 C19B C20 131.9(10) . . ? C18 C19B H19B 112.0 . . ? C20 C19B Pd1 72.9(5) . . ? C20 C19B H19B 112.0 . . ? C42A C43A H43A 120.0 . . ? C42A C43A C44A 120.0 . . ? C44A C43A H43A 120.0 . . ? F8A C42A C43A 119.5(9) . . ? F8A C42A C41A 120.4(9) . . ? C41A C42A C43A 120.0 . . ? F7A C41A C42A 121.7(5) . . ? F7A C41A C40A 118.3(5) . . ? C40A C41A C42A 120.0 . . ? C41A C40A H40A 120.0 . . ? C41A C40A C45A 120.0 . . ? C45A C40A H40A 120.0 . . ? C40A C45A H45A 120.0 . . ? C40A C45A C44A 120.0 . . ? C44A C45A H45A 120.0 . . ? C43A C44A H44A 120.0 . . ? C45A C44A C43A 120.0 . . ? C45A C44A H44A 120.0 . . ? Pd1 C19A H19A 116.4 . . ? C18 C19A Pd1 72.9(3) . . ? C18 C19A C20 125.4(7) . . ? C18 C19A H19A 116.4 . . ? C20 C19A Pd1 72.3(3) . . ? C20 C19A H19A 116.4 . . ? O2B S1B O3B 118.7(14) . . ? O2B S1B C38B 101.1(14) . . ? O3B S1B C38B 98(2) . . ? O1B S1B O2B 101.7(19) . . ? O1B S1B O3B 123(3) . . ? O1B S1B C38B 112(2) . . ? F1B C38B S1B 116(3) . . ? F1B C38B F3B 111(3) . . ? F3B C38B S1B 103(3) . . ? F2B C38B S1B 109(3) . . ? F2B C38B F1B 107(4) . . ? F2B C38B F3B 110(3) . . ? C40B C41B F8B 121.9(17) . . ? C40B C41B C42B 120.0 . . ? C42B C41B F8B 115.3(17) . . ? F7B C40B C41B 117(2) . . ? F7B C40B C45B 122(2) . . ? C41B C40B C45B 120.0 . . ? C40B C45B H45B 120.0 . . ? C44B C45B C40B 120.0 . . ? C44B C45B H45B 120.0 . . ? C45B C44B H44B 120.0 . . ? C45B C44B C43B 120.0 . . ? C43B C44B H44B 120.0 . . ? C44B C43B H43B 120.0 . . ? C42B C43B C44B 120.0 . . ? C42B C43B H43B 120.0 . . ? C41B C42B H42B 120.0 . . ? C43B C42B C41B 120.0 . . ? C43B C42B H42B 120.0 . . ? O6A S2A C39A 103.1(6) . . ? O6A S2A O5A 114.1(5) . . ? O6A S2A O4A 116.6(7) . . ? O5A S2A C39A 104.6(5) . . ? O4A S2A C39A 102.8(5) . . ? O4A S2A O5A 113.4(5) . . ? F6B C39B F5B 104.7(8) . . ? F6B C39B S2B 109.9(8) . . ? F4B C39B F6B 111.0(11) . . ? F4B C39B F5B 110.0(9) . . ? F4B C39B S2B 112.0(8) . . ? F5B C39B S2B 109.0(8) . . ? O5B S2B C39B 104.1(8) . . ? O5B S2B O4B 115.1(9) . . ? O6B S2B O5B 120.3(11) . . ? O6B S2B C39B 109.6(7) . . ? O6B S2B O4B 104.8(8) . . ? O4B S2B C39B 101.3(5) . . ? C46 O7 C49 106.5(16) . . ? O7 C46 H46A 109.5 . . ? O7 C46 H46B 109.5 . . ? O7 C46 C47 110.6(13) . . ? H46A C46 H46B 108.1 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C46 C47 H47A 111.4 . . ? C46 C47 H47B 111.4 . . ? C46 C47 C48 101.9(10) . . ? H47A C47 H47B 109.3 . . ? C48 C47 H47A 111.4 . . ? C48 C47 H47B 111.4 . . ? C47 C48 H48A 110.7 . . ? C47 C48 H48B 110.7 . . ? C47 C48 C49 105.0(11) . . ? H48A C48 H48B 108.8 . . ? C49 C48 H48A 110.7 . . ? C49 C48 H48B 110.7 . . ? O7 C49 C48 105.2(14) . . ? O7 C49 H49A 110.7 . . ? O7 C49 H49B 110.7 . . ? C48 C49 H49A 110.7 . . ? C48 C49 H49B 110.7 . . ? H49A C49 H49B 108.8 . . ? 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 P1 2.3326(10) . ? Pd1 P3 2.3357(10) . ? Pd1 C18 2.189(4) . ? Pd1 C20 2.182(4) . ? Pd1 C19B 2.169(9) . ? Pd1 C19A 2.169(6) . ? P1 P2 2.1543(14) . ? P1 C1 1.854(4) . ? P1 C12 1.863(4) . ? P3 P2 2.1528(13) . ? P3 C21 1.857(4) . ? P3 C32 1.855(4) . ? S1A O1A 1.433(9) . ? S1A O2A 1.415(6) . ? S1A O3A 1.432(6) . ? S1A C38A 1.821(10) . ? C39A F5A 1.292(12) . ? C39A F4A 1.332(13) . ? C39A F6A 1.380(13) . ? C39A S2A 1.817(10) . ? N3 C25 1.380(5) . ? N3 C22 1.494(5) . ? N3 C21 1.346(5) . ? O6A S2A 1.420(10) . ? N4 C27 1.387(5) . ? N4 C21 1.348(5) . ? N4 C29 1.486(5) . ? F1A C38A 1.303(10) . ? N2 C7 1.385(6) . ? N2 C1 1.353(6) . ? N2 C10 1.485(5) . ? N1 C5 1.382(5) . ? N1 C1 1.354(5) . ? N1 C2 1.479(6) . ? O5A S2A 1.433(6) . ? C25 C27 1.362(6) . ? C25 C26 1.493(6) . ? C27 C28 1.492(6) . ? C22 H22 0.9800 . ? C22 C24 1.517(6) . ? C22 C23 1.523(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.527(6) . ? C33 C32 1.525(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 C35 1.514(6) . ? C5 C7 1.346(6) . ? C5 C6 1.503(6) . ? C32 H32 0.9800 . ? C32 C37 1.532(5) . ? F2A C38A 1.271(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C18 H18D 0.9700 . ? C18 C19B 1.311(14) . ? C18 C19A 1.341(9) . ? C29 H29 0.9800 . ? C29 C30 1.517(7) . ? C29 C31 1.520(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 C7 1.512(6) . ? C10 H10 0.9800 . ? C10 C9 1.530(7) . ? C10 C11 1.527(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C12 1.540(6) . ? C13 C14 1.524(6) . ? C12 H12 0.9800 . ? C12 C17 1.527(7) . ? F7A C41A 1.309(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 C36 1.522(7) . ? C2 H2 0.9800 . ? C2 C4 1.518(6) . ? C2 C3 1.531(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20 H20D 0.9700 . ? C20 C19B 1.320(14) . ? C20 C19A 1.362(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.530(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 C37 1.518(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C16 1.538(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? F3A C38A 1.307(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C15 1.515(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? F8A C42A 1.227(11) . ? C19B H19B 0.9800 . ? C43A H43A 0.9300 . ? C43A C42A 1.3900 . ? C43A C44A 1.3900 . ? C42A C41A 1.3900 . ? C41A C40A 1.3900 . ? C40A H40A 0.9300 . ? C40A C45A 1.3900 . ? C45A H45A 0.9300 . ? C45A C44A 1.3900 . ? C44A H44A 0.9300 . ? O4A S2A 1.425(10) . ? C19A H19A 0.9800 . ? O2B S1B 1.45(2) . ? S1B O3B 1.60(5) . ? S1B O1B 1.43(3) . ? S1B C38B 1.88(4) . ? C38B F1B 1.27(4) . ? C38B F3B 1.43(4) . ? C38B F2B 1.00(5) . ? F8B C41B 1.73(3) . ? F7B C40B 1.23(3) . ? C41B C40B 1.3900 . ? C41B C42B 1.3900 . ? C40B C45B 1.3900 . ? C45B H45B 0.9300 . ? C45B C44B 1.3900 . ? C44B H44B 0.9300 . ? C44B C43B 1.3900 . ? C43B H43B 0.9300 . ? C43B C42B 1.3900 . ? C42B H42B 0.9300 . ? O5B S2B 1.443(11) . ? C39B F6B 1.333(13) . ? C39B F4B 1.314(13) . ? C39B F5B 1.339(11) . ? C39B S2B 1.842(10) . ? S2B O6B 1.387(14) . ? S2B O4B 1.456(9) . ? O7 C46 1.393(14) . ? O7 C49 1.422(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 C47 1.527(13) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 C48 1.530(13) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 C49 1.543(13) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? 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 N2 19.6(4) . . . . ? Pd1 P1 C1 N1 -160.3(3) . . . . ? Pd1 P1 C12 C13 39.5(3) . . . . ? Pd1 P1 C12 C17 -84.3(4) . . . . ? Pd1 P3 C21 N3 157.4(3) . . . . ? Pd1 P3 C21 N4 -20.3(4) . . . . ? Pd1 P3 C32 C33 86.0(3) . . . . ? Pd1 P3 C32 C37 -38.0(3) . . . . ? Pd1 C18 C19B C20 47.1(10) . . . . ? Pd1 C18 C19A C20 -52.4(5) . . . . ? Pd1 C20 C19B C18 -47.2(11) . . . . ? Pd1 C20 C19A C18 52.7(5) . . . . ? P1 C12 C17 C16 179.8(4) . . . . ? P3 C32 C37 C36 -178.6(3) . . . . ? P2 P1 C1 N2 132.2(3) . . . . ? P2 P1 C1 N1 -47.6(4) . . . . ? P2 P1 C12 C13 -71.4(3) . . . . ? P2 P1 C12 C17 164.8(3) . . . . ? P2 P3 C21 N3 43.6(4) . . . . ? P2 P3 C21 N4 -134.1(3) . . . . ? P2 P3 C32 C33 -163.6(3) . . . . ? P2 P3 C32 C37 72.3(3) . . . . ? N3 C25 C27 N4 0.6(5) . . . . ? N3 C25 C27 C28 179.4(4) . . . . ? F5A C39A S2A O6A 58.7(9) . . . . ? F5A C39A S2A O5A 178.4(7) . . . . ? F5A C39A S2A O4A -62.9(9) . . . . ? F4A C39A S2A O6A 178.4(9) . . . . ? F4A C39A S2A O5A -62.0(9) . . . . ? F4A C39A S2A O4A 56.7(10) . . . . ? N1 C5 C7 N2 -0.5(5) . . . . ? N1 C5 C7 C8 177.2(4) . . . . ? O1A S1A C38A F1A 171.9(7) . . . . ? O1A S1A C38A F2A -68.8(11) . . . . ? O1A S1A C38A F3A 54.5(10) . . . . ? C25 N3 C22 C24 -67.6(5) . . . . ? C25 N3 C22 C23 60.1(5) . . . . ? C25 N3 C21 P3 -177.5(3) . . . . ? C25 N3 C21 N4 0.6(4) . . . . ? C27 N4 C21 P3 177.8(3) . . . . ? C27 N4 C21 N3 -0.2(4) . . . . ? C27 N4 C29 C30 65.7(5) . . . . ? C27 N4 C29 C31 -61.8(6) . . . . ? C22 N3 C25 C27 173.4(4) . . . . ? C22 N3 C25 C26 -9.9(7) . . . . ? C22 N3 C21 P3 8.2(5) . . . . ? C22 N3 C21 N4 -173.7(3) . . . . ? C33 C34 C35 C36 -54.1(5) . . . . ? C33 C32 C37 C36 56.1(5) . . . . ? C21 P3 C32 C33 -48.4(3) . . . . ? C21 P3 C32 C37 -172.4(3) . . . . ? C21 N3 C25 C27 -0.7(5) . . . . ? C21 N3 C25 C26 176.0(4) . . . . ? C21 N3 C22 C24 105.7(4) . . . . ? C21 N3 C22 C23 -126.6(4) . . . . ? C21 N4 C27 C25 -0.2(5) . . . . ? C21 N4 C27 C28 -179.1(4) . . . . ? C21 N4 C29 C30 -109.2(4) . . . . ? C21 N4 C29 C31 123.4(4) . . . . ? C34 C33 C32 P3 -178.3(3) . . . . ? C34 C33 C32 C37 -55.7(5) . . . . ? C34 C35 C36 C37 54.4(6) . . . . ? C5 N1 C1 P1 179.9(3) . . . . ? C5 N1 C1 N2 0.1(5) . . . . ? C5 N1 C2 C4 -61.5(6) . . . . ? C5 N1 C2 C3 66.6(5) . . . . ? C32 P3 C21 N3 -73.2(4) . . . . ? C32 P3 C21 N4 109.1(4) . . . . ? C32 C33 C34 C35 54.9(5) . . . . ? C29 N4 C27 C25 -175.7(4) . . . . ? C29 N4 C27 C28 5.4(7) . . . . ? C29 N4 C21 P3 -6.5(6) . . . . ? C29 N4 C21 N3 175.4(4) . . . . ? C26 C25 C27 N4 -176.1(4) . . . . ? C26 C25 C27 C28 2.7(8) . . . . ? O2A S1A C38A F1A -65.5(9) . . . . ? O2A S1A C38A F2A 53.8(11) . . . . ? O2A S1A C38A F3A 177.1(9) . . . . ? C7 N2 C1 P1 179.7(3) . . . . ? C7 N2 C1 N1 -0.4(5) . . . . ? C7 N2 C10 C9 50.4(6) . . . . ? C7 N2 C10 C11 -76.0(5) . . . . ? C1 P1 C12 C13 173.7(3) . . . . ? C1 P1 C12 C17 49.8(4) . . . . ? C1 N2 C7 C5 0.6(5) . . . . ? C1 N2 C7 C8 -177.2(4) . . . . ? C1 N2 C10 C9 -128.1(4) . . . . ? C1 N2 C10 C11 105.6(5) . . . . ? C1 N1 C5 C7 0.3(5) . . . . ? C1 N1 C5 C6 -177.1(4) . . . . ? C1 N1 C2 C4 119.8(4) . . . . ? C1 N1 C2 C3 -112.1(5) . . . . ? C10 N2 C7 C5 -178.1(4) . . . . ? C10 N2 C7 C8 4.1(7) . . . . ? C10 N2 C1 P1 -1.6(6) . . . . ? C10 N2 C1 N1 178.3(4) . . . . ? C13 C12 C17 C16 56.4(6) . . . . ? C13 C14 C15 C16 -55.6(7) . . . . ? C12 P1 C1 N2 -111.5(4) . . . . ? C12 P1 C1 N1 68.7(4) . . . . ? C12 C13 C14 C15 56.6(5) . . . . ? C12 C17 C16 C15 -56.1(7) . . . . ? F7A C41A C40A C45A 179.8(7) . . . . ? C35 C36 C37 C32 -55.2(6) . . . . ? O3A S1A C38A F1A 54.1(9) . . . . ? O3A S1A C38A F2A 173.4(11) . . . . ? O3A S1A C38A F3A -63.3(10) . . . . ? C2 N1 C5 C7 -178.6(4) . . . . ? C2 N1 C5 C6 4.0(7) . . . . ? C2 N1 C1 P1 -1.2(6) . . . . ? C2 N1 C1 N2 178.9(4) . . . . ? C14 C13 C12 P1 177.7(3) . . . . ? C14 C13 C12 C17 -57.4(5) . . . . ? C17 C16 C15 C14 55.4(8) . . . . ? C6 C5 C7 N2 176.9(4) . . . . ? C6 C5 C7 C8 -5.4(8) . . . . ? F8A C42A C41A F7A 1.7(9) . . . . ? F8A C42A C41A C40A -178.5(10) . . . . ? C43A C42A C41A F7A -179.8(7) . . . . ? C43A C42A C41A C40A 0.0 . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C42A C41A C40A C45A 0.0 . . . . ? C41A C40A C45A C44A 0.0 . . . . ? C40A C45A C44A C43A 0.0 . . . . ? C44A C43A C42A F8A 178.5(10) . . . . ? C44A C43A C42A C41A 0.0 . . . . ? F6A C39A S2A O6A -62.4(9) . . . . ? F6A C39A S2A O5A 57.3(9) . . . . ? F6A C39A S2A O4A 176.0(9) . . . . ? O2B S1B C38B F1B -178(3) . . . . ? O2B S1B C38B F3B 61(3) . . . . ? O2B S1B C38B F2B -56(3) . . . . ? O3B S1B C38B F1B -56(4) . . . . ? O3B S1B C38B F3B -178(3) . . . . ? O3B S1B C38B F2B 66(3) . . . . ? O1B S1B C38B F1B 75(4) . . . . ? O1B S1B C38B F3B -47(3) . . . . ? O1B S1B C38B F2B -163(3) . . . . ? F8B C41B C40B F7B -12(3) . . . . ? F8B C41B C40B C45B 160(2) . . . . ? F8B C41B C42B C43B -161.5(19) . . . . ? F7B C40B C45B C44B 172(3) . . . . ? C41B C40B C45B C44B 0.0 . . . . ? C40B C41B C42B C43B 0.0 . . . . ? C40B C45B C44B C43B 0.0 . . . . ? C45B C44B C43B C42B 0.0 . . . . ? C44B C43B C42B C41B 0.0 . . . . ? C42B C41B C40B F7B -172(3) . . . . ? C42B C41B C40B C45B 0.0 . . . . ? F6B C39B S2B O5B 60.1(11) . . . . ? F6B C39B S2B O6B -170.0(10) . . . . ? F6B C39B S2B O4B -59.7(9) . . . . ? F4B C39B S2B O5B -176.1(12) . . . . ? F4B C39B S2B O6B -46.2(12) . . . . ? F4B C39B S2B O4B 64.2(10) . . . . ? F5B C39B S2B O5B -54.2(11) . . . . ? F5B C39B S2B O6B 75.7(10) . . . . ? F5B C39B S2B O4B -173.9(7) . . . . ? O7 C46 C47 C48 12(4) . . . . ? C46 O7 C49 C48 34(3) . . . . ? C46 C47 C48 C49 9(4) . . . . ? C47 C48 C49 O7 -26(3) . . . . ? C49 O7 C46 C47 -29(4) . . . . ? 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 10.0001 -1.0000 -0.0002 -0.7281 0.4680 -0.4397 -10.0001 1.0000 0.0002 0.7281 -0.4680 0.4397 -0.0000 1.0000 -4.9999 -0.1366 -0.2965 0.1442 0.0000 -1.0000 4.9999 0.1366 0.2965 -0.1442 -0.0000 1.0000 0.0000 -0.0284 0.0239 0.0967 0.0000 -1.0000 -0.0000 0.0284 -0.0239 -0.0967