#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577305.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_1577305 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 H92 N4 P4 Pd2, 1.728(C F3 O3 S), C4 H10 O, 1.424(C6 H4 F2), C3.729 H2.305 F1.97 O0.817 S0.272' _chemical_formula_sum 'C88 H110 F10 N4 O7 P4 Pd2 S2' _chemical_formula_weight 1926.59 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-05-25 _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 121.4210(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.0433(3) _cell_length_b 16.79110(10) _cell_length_c 23.4811(2) _cell_measurement_reflns_used 21046 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.3010 _cell_measurement_theta_min 3.2820 _cell_volume 8762.45(16) _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 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5700 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _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 -39.00 -3.00 0.50 4.50 -- -38.50 31.00 -90.00 72 2 \w -112.00 -15.00 0.50 4.50 -- -38.50 -31.00 109.00 194 3 \w 1.00 27.00 0.50 4.50 -- -38.50 31.00 -90.00 52 4 \w 21.00 117.00 0.50 4.50 -- 42.50 31.00 -90.00 192 5 \w 117.00 172.00 0.50 18.00 -- 111.00 31.00 -90.00 110 6 \w 41.00 124.00 0.50 18.00 -- 111.00 -31.00 109.00 166 7 \w -33.00 -8.00 0.50 4.50 -- -38.50 125.00 -60.00 50 8 \w -82.00 -10.00 0.50 4.50 -- -38.50 125.00 -90.00 144 9 \w -55.00 -9.00 0.50 4.50 -- -38.50 125.00 0.00 92 10 \w 31.00 96.00 0.50 4.50 -- 42.50-125.00-180.00 130 11 \w -7.00 18.00 0.50 4.50 -- 42.50 -31.00 109.00 50 12 \w 98.00 129.00 0.50 18.00 -- 111.00 45.00 -60.00 62 13 \w 112.00 139.00 0.50 18.00 -- 111.00 125.00-150.00 54 14 \w 86.00 141.00 0.50 18.00 -- 111.00 -77.00-150.00 110 15 \w 50.00 112.00 0.50 18.00 -- 111.00-125.00 30.00 124 16 \w 70.00 97.00 0.50 18.00 -- 111.00 -61.00 150.00 54 17 \w 111.00 176.00 0.50 18.00 -- 111.00 77.00 30.00 130 18 \w 105.00 156.00 0.50 18.00 -- 111.00 77.00-180.00 102 19 \w 130.00 157.00 0.50 18.00 -- 111.00 77.00-150.00 54 20 \w 47.00 127.00 0.50 18.00 -- 111.00 -45.00 0.00 160 21 \w 39.00 92.00 0.50 18.00 -- 111.00 -30.00 -90.00 106 22 \w 58.00 108.00 0.50 18.00 -- 111.00-108.00-162.32 100 23 \w 42.00 112.00 0.50 18.00 -- 111.00-125.00 -30.00 140 24 \w 129.00 172.00 0.50 18.00 -- 111.00 77.00 150.00 86 25 \w 131.00 167.00 0.50 18.00 -- 111.00 45.00 -60.00 72 26 \w 107.00 138.00 0.50 18.00 -- 111.00 -61.00 150.00 62 27 \w 68.00 107.00 0.50 18.00 -- 111.00 -94.00 90.00 78 28 \w 90.00 165.00 0.50 18.00 -- 111.00 45.00 -30.00 150 29 \w 97.00 133.00 0.50 18.00 -- 111.00 -61.00 30.00 72 30 \w 79.00 106.00 0.50 18.00 -- 111.00 -94.00 0.00 54 31 \w 80.00 91.00 0.50 18.00 -- 111.00-125.00-150.00 22 ; _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 0.0271365000 _diffrn_orient_matrix_UB_12 0.0616712000 _diffrn_orient_matrix_UB_13 -0.0255569000 _diffrn_orient_matrix_UB_21 0.0047773000 _diffrn_orient_matrix_UB_22 0.0605209000 _diffrn_orient_matrix_UB_23 0.0518646000 _diffrn_orient_matrix_UB_31 0.0636160000 _diffrn_orient_matrix_UB_32 -0.0308371000 _diffrn_orient_matrix_UB_33 0.0506226000 _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 0.0446 _diffrn_reflns_av_unetI/netI 0.0301 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 40986 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.803 _diffrn_reflns_theta_min 3.299 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.096 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_correction_T_min 0.634 _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 orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.460 _exptl_crystal_description block _exptl_crystal_F_000 3984 _exptl_crystal_size_max 0.144 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.865 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 617 _refine_ls_number_reflns 9092 _refine_ls_number_restraints 911 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0431 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+12.3114P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1158 _refine_ls_wR_factor_ref 0.1188 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8436 _reflns_number_total 9092 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1213 _cod_database_code 1577305 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C88H110F10N4O7P4Pd2S2 _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. ; _shelx_estimated_absorpt_t_max 0.750 _shelx_estimated_absorpt_t_min 0.527 _reflns_odcompleteness_completeness 99.33 _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. Uiso/Uaniso restraints and constraints F1A \\sim F2A \\sim C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B \\sim C42B \\sim F1B \\sim F2B \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A S1A \\sim F3A \\sim F4A \\sim F5A \\sim O1A \\sim O2A \\sim O3A \\sim C36A \\sim S1B \\sim F3B \\sim F4B \\sim F5B \\sim O1B \\sim O2B \\sim O3B \\sim C36B: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 3A 3. Rigid body (RIGU) restrains F1A, F2A, C37B, C38B, C39B, C40B, C41B, C42B, F1B, F2B, C37A, C38A, C39A, C40A, C41A, C42A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 S1A, F3A, F4A, F5A, O1A, O2A, O3A, C36A, S1B, F3B, F4B, F5B, O1B, O2B, O3B, C36B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(F2A)=Sof(C42B)=Sof(H42B)=Sof(C37B)=Sof(C38B)=Sof(C39B)=Sof(H39B)= Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(F1A)=1-FVAR(1) Sof(F2B)=Sof(F1B)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)= Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(C39A)=FVAR(1) Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C36B)=Sof(F3B)=Sof(F5B)=Sof(F4B)=1- FVAR(2) Sof(S1A)=Sof(F4A)=Sof(F3A)=Sof(O3A)=Sof(F5A)=Sof(O1A)=Sof(O2A)=Sof(C36A)= FVAR(2) 5.a Ternary CH refined with riding coordinates: C2(H2), C12(H12), C9(H9) 5.b Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C15(H15A, H15B), C43(H43A,H43B) 5.c Aromatic/amide H refined with riding coordinates: C26(H26), C29(H29), C35(H35), C27(H27), C25(H25), C23(H23), C31(H31), C34(H34), C28(H28), C33(H33), C32(H32), C19(H19), C22(H22), C20(H20), C21(H21), C40A(H40A), C41A(H41A), C42A(H42A), C37A(H37A), C42B(H42B), C39B(H39B), C40B(H40B), C41B(H41B) 5.d Fitted hexagon refined as free rotating group: C40A(C41A,C42A,C37A,C38A,C39A), C42B(C37B,C38B,C39B,C40B,C41B) 5.e Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C44(H44A,H44B,H44C) ; _shelx_res_file ; TITL jjw1213_a.res in I2/a jjw1213.res created by SHELXL-2018/3 at 17:48:32 on 25-May-2020 REM Old TITL jjw1213 in I2/a REM SHELXT solution in I2/a: R1 0.097, Rweak 0.008, Alpha 0.044 REM 0.489 for 317 systematic absences, Orientation as input REM Formula found by SHELXT: C88 N4 O11 F6 S6 Pd2 CELL 1.54184 26.0433 16.7911 23.4811 90 121.421 90 ZERR 4 0.0003 0.0001 0.0002 0 0.001 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H F N O P Pd S UNIT 352 440 40 16 28 16 8 8 SIMU F2B F1B C40A C41A C42A C37A C38A C39A F2A C42B C37B C38B C39B C40B = C41B F1A RIGU F2B F1B C40A C41A C42A C37A C38A C39A F2A C42B C37B C38B C39B C40B = C41B F1A RIGU S1A F3A O3A O1A O2A C36A S1B O1B O2B O3B C36B F3B F5B F4B F5A F4A SIMU 0.01 0.01 3 S1A F3A O3A O1A O2A C36A S1B O1B O2B O3B C36B F3B F5B F4B = F5A F4A L.S. 10 PLAN 8 SIZE 0.06 0.09 0.144 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 TEMP 100 acta REM REM REM WGHT 0.079500 12.311400 FVAR 0.14491 0.71192 0.86377 PD1 7 0.333774 0.647024 0.564673 11.00000 0.01873 0.02288 = 0.01965 0.00080 0.01058 0.00178 P1 6 0.241511 0.699845 0.539428 11.00000 0.01858 0.02564 = 0.01969 -0.00054 0.01047 0.00052 P2 6 0.404225 0.584766 0.547577 11.00000 0.01996 0.02578 = 0.02214 -0.00007 0.01170 0.00265 PART 1 S1A 8 1.099176 0.560917 0.931530 31.00000 0.04690 0.03446 = 0.04404 -0.00935 0.03298 -0.00839 PART 0 O4 5 1.250000 0.303986 1.000000 10.50000 0.04477 0.03280 = 0.05951 0.00000 0.02537 0.00000 PART 1 F4A 3 1.099418 0.554069 1.042986 31.00000 0.06148 0.05978 = 0.03231 -0.00937 0.02120 -0.01668 F3A 3 1.045305 0.463466 0.971902 31.00000 0.06553 0.05460 = 0.03977 -0.00377 0.02463 -0.02466 O3A 5 1.109308 0.644419 0.938680 31.00000 0.04909 0.04305 = 0.04222 -0.00813 0.02958 -0.01358 PART 0 N1 4 0.371370 0.571066 0.698734 11.00000 0.02613 0.03073 = 0.02542 0.00610 0.01311 0.00106 N2 4 0.427581 0.673176 0.713298 11.00000 0.02406 0.02855 = 0.02028 0.00046 0.01084 0.00179 PART 1 F5A 3 1.012570 0.587446 0.954411 31.00000 0.04283 0.07814 = 0.05481 -0.01237 0.03230 -0.00665 PART 0 C1 1 0.380493 0.630616 0.666608 11.00000 0.02173 0.02871 = 0.01885 0.00445 0.01039 0.00478 PART 1 O1A 5 1.055014 0.534472 0.864653 31.00000 0.06907 0.05550 = 0.04028 -0.01162 0.03546 -0.02069 PART 0 C24 1 0.482797 0.574936 0.615382 11.00000 0.02370 0.02529 = 0.02788 -0.00266 0.01423 0.00187 C26 1 0.553648 0.534078 0.728725 11.00000 0.03261 0.02773 = 0.02602 0.00172 0.01320 0.00585 AFIX 43 H26 2 0.561322 0.512297 0.768846 11.00000 -1.20000 AFIX 0 C30 1 0.409513 0.630280 0.480395 11.00000 0.02008 0.03173 = 0.02336 0.00143 0.01067 0.00395 C29 1 0.530631 0.598836 0.608244 11.00000 0.02360 0.03129 = 0.02819 -0.00068 0.01504 0.00347 AFIX 43 H29 2 0.523120 0.620287 0.568084 11.00000 -1.20000 AFIX 0 C18 1 0.383812 0.480764 0.523339 11.00000 0.02490 0.02885 = 0.02529 -0.00151 0.01359 0.00017 C2 1 0.323910 0.510437 0.663255 11.00000 0.02950 0.03054 = 0.03473 0.00551 0.01655 0.00010 AFIX 13 H2 2 0.304516 0.522591 0.615580 11.00000 -1.20000 AFIX 0 C35 1 0.421045 0.712383 0.484925 11.00000 0.02408 0.03441 = 0.02978 -0.00080 0.01647 0.00112 AFIX 43 H35 2 0.425754 0.741272 0.521144 11.00000 -1.20000 AFIX 0 C27 1 0.601115 0.558866 0.721654 11.00000 0.02460 0.03211 = 0.03142 -0.00212 0.00820 0.00516 AFIX 43 H27 2 0.640547 0.554258 0.757295 11.00000 -1.20000 AFIX 0 C7 1 0.449393 0.638981 0.776222 11.00000 0.02697 0.03693 = 0.02506 0.00484 0.01337 0.00684 C25 1 0.494975 0.542051 0.675679 11.00000 0.02867 0.02448 = 0.03039 0.00101 0.01631 0.00411 AFIX 43 H25 2 0.463345 0.525255 0.680371 11.00000 -1.20000 AFIX 0 C23 1 0.426793 0.424903 0.531317 11.00000 0.02544 0.03193 = 0.03961 -0.00292 0.01791 0.00090 AFIX 43 H23 2 0.466531 0.440672 0.549104 11.00000 -1.20000 AFIX 0 C31 1 0.402456 0.587728 0.425889 11.00000 0.02275 0.03452 = 0.02552 -0.00159 0.01283 0.00408 AFIX 43 H31 2 0.395170 0.533211 0.422814 11.00000 -1.20000 AFIX 0 C10 1 0.435081 0.819373 0.733012 11.00000 0.03299 0.03350 = 0.03114 -0.00336 0.01634 0.00343 AFIX 137 H10A 2 0.397238 0.811955 0.730118 11.00000 -1.50000 H10B 2 0.434333 0.868536 0.711722 11.00000 -1.50000 H10C 2 0.466839 0.821029 0.779063 11.00000 -1.50000 AFIX 0 C17 1 0.278129 0.852638 0.594278 11.00000 0.02868 0.02922 = 0.02803 -0.00496 0.01595 -0.00357 AFIX 23 H17A 2 0.273798 0.870627 0.552733 11.00000 -1.20000 H17B 2 0.318165 0.830463 0.621800 11.00000 -1.20000 AFIX 0 C34 1 0.425373 0.750145 0.435182 11.00000 0.03011 0.03335 = 0.03828 0.00546 0.01957 0.00166 AFIX 43 H34 2 0.433552 0.804420 0.438350 11.00000 -1.20000 AFIX 0 C12 1 0.231160 0.788351 0.579706 11.00000 0.02139 0.02484 = 0.02248 -0.00136 0.01244 0.00171 AFIX 13 H12 2 0.191125 0.810621 0.549312 11.00000 -1.20000 AFIX 0 C9 1 0.445949 0.750339 0.698232 11.00000 0.02890 0.02785 = 0.02666 -0.00064 0.01523 -0.00075 AFIX 13 H9 2 0.419783 0.759197 0.650112 11.00000 -1.20000 AFIX 0 C3 1 0.274949 0.516943 0.680390 11.00000 0.03226 0.04092 = 0.04865 0.00551 0.02351 -0.00110 AFIX 137 H3A 2 0.243752 0.478938 0.654538 11.00000 -1.50000 H3B 2 0.258311 0.569702 0.670363 11.00000 -1.50000 H3C 2 0.292022 0.506277 0.727034 11.00000 -1.50000 AFIX 0 C28 1 0.589593 0.590317 0.661650 11.00000 0.02361 0.03577 = 0.03401 -0.00443 0.01543 0.00126 AFIX 43 H28 2 0.621431 0.605902 0.656898 11.00000 -1.20000 AFIX 0 C33 1 0.417564 0.707396 0.380555 11.00000 0.03152 0.04841 = 0.03221 0.00765 0.02116 0.00563 AFIX 43 H33 2 0.419941 0.733267 0.346982 11.00000 -1.20000 AFIX 0 C13 1 0.234116 0.761566 0.643804 11.00000 0.03205 0.03151 = 0.02573 0.00152 0.01672 0.00223 AFIX 23 H13A 2 0.272977 0.737534 0.673911 11.00000 -1.20000 H13B 2 0.203267 0.721949 0.633142 11.00000 -1.20000 AFIX 0 C14 1 0.224670 0.833283 0.677812 11.00000 0.03715 0.03837 = 0.03046 -0.00072 0.02182 0.00397 AFIX 23 H14A 2 0.184645 0.854823 0.648825 11.00000 -1.20000 H14B 2 0.227720 0.816129 0.718917 11.00000 -1.20000 AFIX 0 C32 1 0.406312 0.626820 0.376013 11.00000 0.02905 0.04506 = 0.02714 -0.00084 0.01668 0.00499 AFIX 43 H32 2 0.401267 0.598396 0.339439 11.00000 -1.20000 AFIX 0 C11 1 0.510465 0.751427 0.713652 11.00000 0.03185 0.03272 = 0.04096 -0.00594 0.02174 -0.00352 AFIX 137 H11A 2 0.517853 0.800611 0.698288 11.00000 -1.50000 H11B 2 0.516461 0.707649 0.691442 11.00000 -1.50000 H11C 2 0.537742 0.746706 0.760945 11.00000 -1.50000 AFIX 0 C5 1 0.413458 0.575813 0.767000 11.00000 0.02947 0.03883 = 0.02817 0.00703 0.01349 0.00744 C19 1 0.324544 0.456210 0.497324 11.00000 0.02519 0.03378 = 0.04169 -0.00530 0.01780 -0.00060 AFIX 43 H19 2 0.295490 0.492793 0.491845 11.00000 -1.20000 AFIX 0 C4 1 0.350507 0.427299 0.672714 11.00000 0.04340 0.03212 = 0.05095 0.00682 0.02611 0.00277 AFIX 137 H4A 2 0.371590 0.413557 0.719208 11.00000 -1.50000 H4B 2 0.377955 0.426294 0.657025 11.00000 -1.50000 H4C 2 0.318747 0.389620 0.647875 11.00000 -1.50000 AFIX 0 PART 1 F2B 3 0.762449 0.684717 0.708532 21.00000 0.04758 0.06324 = 0.12250 -0.03324 0.03506 0.00233 PART 0 C16 1 0.270407 0.923604 0.630455 11.00000 0.03570 0.03233 = 0.04116 -0.00977 0.02172 -0.00669 AFIX 23 H16A 2 0.302505 0.961634 0.642380 11.00000 -1.20000 H16B 2 0.232506 0.949924 0.600448 11.00000 -1.20000 AFIX 0 C8 1 0.505425 0.663812 0.838284 11.00000 0.03296 0.04782 = 0.02618 0.00252 0.01145 0.00406 AFIX 137 H8A 2 0.506641 0.640088 0.876168 11.00000 -1.50000 H8B 2 0.506095 0.720759 0.842247 11.00000 -1.50000 H8C 2 0.539725 0.646623 0.836518 11.00000 -1.50000 AFIX 0 C22 1 0.410732 0.346023 0.512928 11.00000 0.03635 0.03102 = 0.04999 -0.00160 0.02425 0.00638 AFIX 43 H22 2 0.439559 0.309403 0.517827 11.00000 -1.20000 AFIX 0 C6 1 0.416983 0.520023 0.818474 11.00000 0.04175 0.05564 = 0.03425 0.01720 0.01554 0.00271 AFIX 137 H6A 2 0.434353 0.470509 0.816370 11.00000 -1.50000 H6B 2 0.377283 0.510608 0.810157 11.00000 -1.50000 H6C 2 0.441578 0.543097 0.861975 11.00000 -1.50000 AFIX 0 PART 1 O2A 5 1.153398 0.515089 0.969220 31.00000 0.05714 0.05615 = 0.07581 -0.00294 0.03818 0.00769 PART 0 C15 1 0.271397 0.898068 0.693296 11.00000 0.03525 0.04252 = 0.03182 -0.01141 0.01725 0.00002 AFIX 23 H15A 2 0.263166 0.943794 0.712549 11.00000 -1.20000 H15B 2 0.311110 0.878187 0.725829 11.00000 -1.20000 AFIX 0 C20 1 0.308952 0.377230 0.479630 11.00000 0.03115 0.03870 = 0.05215 -0.00980 0.02265 -0.00593 AFIX 43 H20 2 0.269378 0.361078 0.462434 11.00000 -1.20000 AFIX 0 C21 1 0.351857 0.321812 0.487307 11.00000 0.04197 0.02910 = 0.04993 -0.00693 0.02627 -0.00537 AFIX 43 H21 2 0.341056 0.268909 0.475315 11.00000 -1.20000 AFIX 0 PART 1 C36A 1 1.061480 0.541703 0.976892 31.00000 0.04775 0.04562 = 0.03373 -0.00820 0.02379 -0.01390 PART 0 C43 1 1.211636 0.349995 0.942487 11.00000 0.08356 0.03974 = 0.08516 0.01862 0.05580 0.02157 AFIX 23 H43A 2 1.235390 0.387698 0.934447 11.00000 -1.20000 H43B 2 1.183557 0.379785 0.949628 11.00000 -1.20000 AFIX 0 PART 1 F1B 3 0.735801 0.601524 0.787020 21.00000 0.05962 0.07133 = 0.21973 -0.01695 0.08663 -0.01681 PART 0 C44 1 1.177895 0.296992 0.883530 11.00000 0.05998 0.06986 = 0.06435 0.02391 0.02331 0.01091 AFIX 137 H44A 2 1.150329 0.328196 0.845391 11.00000 -1.50000 H44B 2 1.155921 0.258163 0.892456 11.00000 -1.50000 H44C 2 1.205659 0.270409 0.874692 11.00000 -1.50000 AFIX 66 PART 1 C40A 1 0.832689 0.623823 0.882135 21.00000 0.06830 0.04334 = 0.14717 -0.00177 0.07881 0.00087 AFIX 43 H40A 2 0.823492 0.594291 0.909174 21.00000 -1.20000 AFIX 65 C41A 1 0.888965 0.659141 0.909257 21.00000 0.06930 0.04092 = 0.10162 -0.00869 0.06264 -0.00120 AFIX 43 H41A 2 0.917421 0.653239 0.954441 21.00000 -1.20000 AFIX 65 C42A 1 0.902711 0.703280 0.868845 21.00000 0.05525 0.03963 = 0.08330 -0.01385 0.04118 -0.01544 AFIX 43 H42A 2 0.940363 0.726910 0.886991 21.00000 -1.20000 AFIX 65 C37A 1 0.860181 0.712102 0.801311 21.00000 0.04329 0.03800 = 0.08679 -0.02207 0.03835 -0.01260 AFIX 43 H37A 2 0.869378 0.741634 0.774273 21.00000 -1.20000 AFIX 65 C38A 1 0.803905 0.676785 0.774189 21.00000 0.03589 0.03481 = 0.11610 -0.03124 0.04010 -0.00711 C39A 1 0.790158 0.632646 0.814600 21.00000 0.04909 0.03888 = 0.14935 -0.01889 0.06570 -0.00702 AFIX 0 PART 2 F2A 3 0.837754 0.733926 0.752530 -21.00000 0.10056 0.05185 = 0.06917 0.00666 0.04943 0.00915 AFIX 66 C42B 1 0.890708 0.694216 0.863024 -21.00000 0.02852 0.03538 = 0.05883 -0.01928 0.01998 -0.00988 AFIX 43 H42B 2 0.924594 0.720452 0.868904 -21.00000 -1.20000 AFIX 65 C37B 1 0.837855 0.694072 0.800812 -21.00000 0.04193 0.03153 = 0.06388 -0.00369 0.02726 -0.00468 C38B 1 0.787208 0.654860 0.792023 -21.00000 0.03469 0.03868 = 0.07333 -0.00013 0.02346 -0.00165 C39B 1 0.789413 0.615792 0.845446 -21.00000 0.05949 0.04276 = 0.08277 0.00184 0.04021 0.00466 AFIX 43 H39B 2 0.755527 0.589556 0.839565 -21.00000 -1.20000 AFIX 65 C40B 1 0.842265 0.615936 0.907657 -21.00000 0.07082 0.04341 = 0.07957 0.00164 0.03852 -0.00222 AFIX 43 H40B 2 0.843740 0.589796 0.943400 -21.00000 -1.20000 AFIX 65 C41B 1 0.892913 0.655147 0.916447 -21.00000 0.07212 0.05081 = 0.07174 -0.00325 0.03107 -0.01050 AFIX 43 H41B 2 0.928274 0.655244 0.958071 -21.00000 -1.20000 AFIX 0 F1A 3 0.740522 0.656122 0.730934 -21.00000 0.05242 0.07471 = 0.07257 -0.01203 0.00462 0.00865 S1B 8 1.067818 0.576748 0.920752 -31.00000 0.05284 O1B 5 1.019878 0.617580 0.919059 -31.00000 0.05140 O2B 5 1.070666 0.515381 0.876364 -31.00000 0.04948 O3B 5 1.098280 0.645371 0.935178 -31.00000 0.04998 C36B 1 1.087509 0.502324 0.988709 -31.00000 0.05110 F3B 3 1.087862 0.566511 1.038789 -31.00000 0.04667 F5B 3 1.135869 0.459405 0.999043 -31.00000 0.05676 F4B 3 1.030556 0.480483 0.964197 -31.00000 0.04940 HKLF 4 REM jjw1213_a.res in I2/a REM wR2 = 0.1188, GooF = S = 1.054, Restrained GooF = 1.047 for all data REM R1 = 0.0431 for 8436 Fo > 4sig(Fo) and 0.0458 for all 9092 data REM 617 parameters refined using 911 restraints END WGHT 0.0795 12.3031 REM Highest difference peak 0.865, deepest hole -0.883, 1-sigma level 0.095 Q1 1 0.3159 0.5983 0.5438 11.00000 0.05 0.86 Q2 1 0.2391 0.6399 0.5389 11.00000 0.05 0.80 Q3 1 0.3302 0.6924 0.5475 11.00000 0.05 0.73 Q4 1 1.0184 0.5605 0.8464 11.00000 0.05 0.72 Q5 1 0.3307 0.5842 0.5695 11.00000 0.05 0.69 Q6 1 1.1307 0.5205 0.9241 11.00000 0.05 0.69 Q7 1 0.3401 0.7069 0.5751 11.00000 0.05 0.67 Q8 1 0.3007 0.6898 0.5615 11.00000 0.05 0.62 ; _shelx_res_checksum 81940 _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 2.770 _oxdiff_exptl_absorpt_empirical_full_min 0.714 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 0.33377(2) 0.64702(2) 0.56467(2) 0.02014(8) Uani 1 1 d . . . . . P1 P 0.24151(3) 0.69985(4) 0.53943(3) 0.02107(13) Uani 1 1 d . . . . . P2 P 0.40423(3) 0.58477(4) 0.54758(3) 0.02228(14) Uani 1 1 d . . . . . S1A S 1.09918(5) 0.56092(5) 0.93153(5) 0.0374(3) Uani 0.864(3) 1 d . U P A 1 O4 O 1.250000 0.30399(19) 1.000000 0.0466(8) Uani 1 2 d S T P . . F4A F 1.09942(19) 0.5541(3) 1.0430(3) 0.0527(9) Uani 0.864(3) 1 d . U P A 1 F3A F 1.04531(16) 0.4635(2) 0.97190(18) 0.0546(8) Uani 0.864(3) 1 d . U P A 1 O3A O 1.1093(2) 0.6444(4) 0.9387(4) 0.0420(9) Uani 0.864(3) 1 d . U P A 1 N1 N 0.37137(10) 0.57107(14) 0.69873(12) 0.0276(5) Uani 1 1 d . . . . . N2 N 0.42758(10) 0.67318(14) 0.71330(11) 0.0246(4) Uani 1 1 d . . . . . F5A F 1.01257(11) 0.58745(18) 0.95441(14) 0.0553(6) Uani 0.864(3) 1 d . U P A 1 C1 C 0.38049(12) 0.63062(16) 0.66661(12) 0.0232(5) Uani 1 1 d . . . . . O1A O 1.05501(18) 0.5345(2) 0.86465(18) 0.0516(8) Uani 0.864(3) 1 d . U P A 1 C24 C 0.48280(12) 0.57494(15) 0.61538(13) 0.0252(5) Uani 1 1 d . . . . . C26 C 0.55365(13) 0.53408(16) 0.72873(14) 0.0298(5) Uani 1 1 d . . . . . H26 H 0.561322 0.512297 0.768846 0.036 Uiso 1 1 calc R U . . . C30 C 0.40951(12) 0.63028(17) 0.48040(13) 0.0254(5) Uani 1 1 d . . . . . C29 C 0.53063(12) 0.59884(16) 0.60824(14) 0.0270(5) Uani 1 1 d . . . . . H29 H 0.523120 0.620287 0.568084 0.032 Uiso 1 1 calc R U . . . C18 C 0.38381(12) 0.48076(16) 0.52334(13) 0.0261(5) Uani 1 1 d . . . . . C2 C 0.32391(13) 0.51044(17) 0.66325(15) 0.0317(6) Uani 1 1 d . . . . . H2 H 0.304516 0.522591 0.615580 0.038 Uiso 1 1 calc R U . . . C35 C 0.42104(12) 0.71238(17) 0.48492(14) 0.0283(5) Uani 1 1 d . . . . . H35 H 0.425754 0.741272 0.521144 0.034 Uiso 1 1 calc R U . . . C27 C 0.60111(13) 0.55887(17) 0.72165(15) 0.0324(6) Uani 1 1 d . . . . . H27 H 0.640547 0.554258 0.757295 0.039 Uiso 1 1 calc R U . . . C7 C 0.44939(13) 0.63898(17) 0.77622(15) 0.0297(6) Uani 1 1 d . . . . . C25 C 0.49498(12) 0.54205(16) 0.67568(14) 0.0274(5) Uani 1 1 d . . . . . H25 H 0.463345 0.525255 0.680371 0.033 Uiso 1 1 calc R U . . . C23 C 0.42679(13) 0.42490(17) 0.53132(15) 0.0319(6) Uani 1 1 d . . . . . H23 H 0.466531 0.440672 0.549104 0.038 Uiso 1 1 calc R U . . . C31 C 0.40246(12) 0.58773(17) 0.42589(14) 0.0275(5) Uani 1 1 d . . . . . H31 H 0.395170 0.533211 0.422814 0.033 Uiso 1 1 calc R U . . . C10 C 0.43508(14) 0.81937(18) 0.73301(15) 0.0327(6) Uani 1 1 d . . . . . H10A H 0.397238 0.811955 0.730118 0.049 Uiso 1 1 calc R U . . . H10B H 0.434333 0.868536 0.711722 0.049 Uiso 1 1 calc R U . . . H10C H 0.466839 0.821029 0.779063 0.049 Uiso 1 1 calc R U . . . C17 C 0.27813(14) 0.85264(15) 0.59428(15) 0.0281(6) Uani 1 1 d . . . . . H17A H 0.273798 0.870627 0.552733 0.034 Uiso 1 1 calc R U . . . H17B H 0.318165 0.830463 0.621800 0.034 Uiso 1 1 calc R U . . . C34 C 0.42537(13) 0.75015(18) 0.43518(15) 0.0331(6) Uani 1 1 d . . . . . H34 H 0.433552 0.804420 0.438350 0.040 Uiso 1 1 calc R U . . . C12 C 0.23116(11) 0.78835(15) 0.57971(12) 0.0224(5) Uani 1 1 d . . . . . H12 H 0.191125 0.810621 0.549312 0.027 Uiso 1 1 calc R U . . . C9 C 0.44595(12) 0.75034(16) 0.69823(14) 0.0274(5) Uani 1 1 d . . . . . H9 H 0.419783 0.759197 0.650112 0.033 Uiso 1 1 calc R U . . . C3 C 0.27495(14) 0.5169(2) 0.68039(18) 0.0395(7) Uani 1 1 d . . . . . H3A H 0.243752 0.478938 0.654538 0.059 Uiso 1 1 calc R U . . . H3B H 0.258311 0.569702 0.670363 0.059 Uiso 1 1 calc R U . . . H3C H 0.292022 0.506277 0.727034 0.059 Uiso 1 1 calc R U . . . C28 C 0.58959(12) 0.59032(17) 0.66165(15) 0.0309(6) Uani 1 1 d . . . . . H28 H 0.621431 0.605902 0.656898 0.037 Uiso 1 1 calc R U . . . C33 C 0.41756(13) 0.7074(2) 0.38055(15) 0.0352(6) Uani 1 1 d . . . . . H33 H 0.419941 0.733267 0.346982 0.042 Uiso 1 1 calc R U . . . C13 C 0.23412(13) 0.76157(17) 0.64380(14) 0.0290(5) Uani 1 1 d . . . . . H13A H 0.272977 0.737534 0.673911 0.035 Uiso 1 1 calc R U . . . H13B H 0.203267 0.721949 0.633142 0.035 Uiso 1 1 calc R U . . . C14 C 0.22467(14) 0.83328(19) 0.67781(15) 0.0333(6) Uani 1 1 d . . . . . H14A H 0.184645 0.854823 0.648825 0.040 Uiso 1 1 calc R U . . . H14B H 0.227720 0.816129 0.718917 0.040 Uiso 1 1 calc R U . . . C32 C 0.40631(13) 0.6268(2) 0.37601(15) 0.0328(6) Uani 1 1 d . . . . . H32 H 0.401267 0.598396 0.339439 0.039 Uiso 1 1 calc R U . . . C11 C 0.51047(13) 0.75143(18) 0.71365(16) 0.0339(6) Uani 1 1 d . . . . . H11A H 0.517853 0.800611 0.698288 0.051 Uiso 1 1 calc R U . . . H11B H 0.516461 0.707649 0.691442 0.051 Uiso 1 1 calc R U . . . H11C H 0.537742 0.746706 0.760945 0.051 Uiso 1 1 calc R U . . . C5 C 0.41346(13) 0.57581(18) 0.76700(15) 0.0329(6) Uani 1 1 d . . . . . C19 C 0.32454(13) 0.45621(18) 0.49732(16) 0.0334(6) Uani 1 1 d . . . . . H19 H 0.295490 0.492793 0.491845 0.040 Uiso 1 1 calc R U . . . C4 C 0.35051(16) 0.42730(19) 0.67271(19) 0.0414(7) Uani 1 1 d . . . . . H4A H 0.371590 0.413557 0.719208 0.062 Uiso 1 1 calc R U . . . H4B H 0.377955 0.426294 0.657025 0.062 Uiso 1 1 calc R U . . . H4C H 0.318747 0.389620 0.647875 0.062 Uiso 1 1 calc R U . . . F2B F 0.76245(18) 0.6847(3) 0.7085(3) 0.0822(15) Uani 0.712(7) 1 d . U P B 1 C16 C 0.27041(14) 0.92360(18) 0.63045(16) 0.0356(6) Uani 1 1 d . . . . . H16A H 0.302505 0.961634 0.642380 0.043 Uiso 1 1 calc R U . . . H16B H 0.232506 0.949924 0.600448 0.043 Uiso 1 1 calc R U . . . C8 C 0.50542(15) 0.6638(2) 0.83828(15) 0.0375(6) Uani 1 1 d . . . . . H8A H 0.506641 0.640088 0.876168 0.056 Uiso 1 1 calc R U . . . H8B H 0.506095 0.720759 0.842247 0.056 Uiso 1 1 calc R U . . . H8C H 0.539725 0.646623 0.836518 0.056 Uiso 1 1 calc R U . . . C22 C 0.41073(16) 0.34602(18) 0.51293(19) 0.0383(7) Uani 1 1 d . . . . . H22 H 0.439559 0.309403 0.517827 0.046 Uiso 1 1 calc R U . . . C6 C 0.41698(16) 0.5200(2) 0.81847(17) 0.0459(8) Uani 1 1 d . . . . . H6A H 0.434353 0.470509 0.816370 0.069 Uiso 1 1 calc R U . . . H6B H 0.377283 0.510608 0.810157 0.069 Uiso 1 1 calc R U . . . H6C H 0.441578 0.543097 0.861975 0.069 Uiso 1 1 calc R U . . . O2A O 1.15340(16) 0.5151(2) 0.9692(2) 0.0614(8) Uani 0.864(3) 1 d . U P A 1 C15 C 0.27140(14) 0.8981(2) 0.69330(15) 0.0366(6) Uani 1 1 d . . . . . H15A H 0.263166 0.943794 0.712549 0.044 Uiso 1 1 calc R U . . . H15B H 0.311110 0.878187 0.725829 0.044 Uiso 1 1 calc R U . . . C20 C 0.30895(15) 0.3772(2) 0.47963(18) 0.0402(7) Uani 1 1 d . . . . . H20 H 0.269378 0.361078 0.462434 0.048 Uiso 1 1 calc R U . . . C21 C 0.35186(15) 0.32181(19) 0.48731(18) 0.0392(7) Uani 1 1 d . . . . . H21 H 0.341056 0.268909 0.475315 0.047 Uiso 1 1 calc R U . . . C36A C 1.06148(19) 0.5417(3) 0.97689(19) 0.0412(7) Uani 0.864(3) 1 d . U P A 1 C43 C 1.2116(2) 0.3500(2) 0.9425(3) 0.0638(12) Uani 1 1 d . . . . . H43A H 1.235390 0.387698 0.934447 0.077 Uiso 1 1 calc R U . . . H43B H 1.183557 0.379785 0.949628 0.077 Uiso 1 1 calc R U . . . F1B F 0.7358(2) 0.6015(3) 0.7870(4) 0.110(2) Uani 0.712(7) 1 d . U P B 1 C44 C 1.1779(2) 0.2970(3) 0.8835(2) 0.0691(12) Uani 1 1 d . . . . . H44A H 1.150329 0.328196 0.845391 0.104 Uiso 1 1 calc R U . . . H44B H 1.155921 0.258163 0.892456 0.104 Uiso 1 1 calc R U . . . H44C H 1.205659 0.270409 0.874692 0.104 Uiso 1 1 calc R U . . . C40A C 0.8327(3) 0.6238(4) 0.8821(4) 0.075(2) Uani 0.712(7) 1 d G U P B 1 H40A H 0.823492 0.594291 0.909174 0.091 Uiso 0.712(7) 1 calc R U P B 1 C41A C 0.8890(3) 0.6591(6) 0.9093(3) 0.062(2) Uani 0.712(7) 1 d G U P B 1 H41A H 0.917421 0.653239 0.954441 0.074 Uiso 0.712(7) 1 calc R U P B 1 C42A C 0.90271(19) 0.7033(5) 0.8688(3) 0.0570(19) Uani 0.712(7) 1 d G U P B 1 H42A H 0.940363 0.726910 0.886991 0.068 Uiso 0.712(7) 1 calc R U P B 1 C37A C 0.8602(2) 0.7121(3) 0.8013(3) 0.0539(16) Uani 0.712(7) 1 d G U P B 1 H37A H 0.869378 0.741634 0.774273 0.065 Uiso 0.712(7) 1 calc R U P B 1 C38A C 0.80390(19) 0.6768(3) 0.7742(3) 0.0620(16) Uani 0.712(7) 1 d G U P B 1 C39A C 0.79016(19) 0.6326(3) 0.8146(4) 0.072(2) Uani 0.712(7) 1 d G U P B 1 F2A F 0.8378(5) 0.7339(5) 0.7525(5) 0.071(3) Uani 0.288(7) 1 d . U P B 2 C42B C 0.8907(6) 0.6942(11) 0.8630(8) 0.042(3) Uani 0.288(7) 1 d G U P B 2 H42B H 0.924594 0.720452 0.868904 0.051 Uiso 0.288(7) 1 calc R U P B 2 C37B C 0.8379(7) 0.6941(7) 0.8008(6) 0.046(3) Uani 0.288(7) 1 d G U P B 2 C38B C 0.7872(5) 0.6549(7) 0.7920(5) 0.051(3) Uani 0.288(7) 1 d G U P B 2 C39B C 0.7894(6) 0.6158(8) 0.8454(7) 0.060(4) Uani 0.288(7) 1 d G U P B 2 H39B H 0.755527 0.589556 0.839565 0.072 Uiso 0.288(7) 1 calc R U P B 2 C40B C 0.8423(8) 0.6159(13) 0.9077(6) 0.065(4) Uani 0.288(7) 1 d G U P B 2 H40B H 0.843740 0.589796 0.943400 0.078 Uiso 0.288(7) 1 calc R U P B 2 C41B C 0.8929(6) 0.6551(16) 0.9164(6) 0.068(6) Uani 0.288(7) 1 d G U P B 2 H41B H 0.928274 0.655244 0.958071 0.082 Uiso 0.288(7) 1 calc R U P B 2 F1A F 0.7405(6) 0.6561(7) 0.7309(6) 0.080(4) Uani 0.288(7) 1 d . U P B 2 S1B S 1.0678(5) 0.5767(5) 0.9208(4) 0.0528(13) Uiso 0.136(3) 1 d . U P A 2 O1B O 1.0199(9) 0.6176(12) 0.9191(10) 0.0514(18) Uiso 0.136(3) 1 d . U P A 2 O2B O 1.0707(12) 0.5154(17) 0.8764(15) 0.049(2) Uiso 0.136(3) 1 d . U P A 2 O3B O 1.098(2) 0.645(3) 0.935(3) 0.050(2) Uiso 0.136(3) 1 d . U P A 2 C36B C 1.0875(14) 0.5023(19) 0.9887(15) 0.0511(18) Uiso 0.136(3) 1 d . U P A 2 F3B F 1.0879(14) 0.567(2) 1.039(2) 0.047(2) Uiso 0.136(3) 1 d . U P A 2 F5B F 1.1359(8) 0.4594(10) 0.9990(9) 0.057(2) Uiso 0.136(3) 1 d . U P A 2 F4B F 1.0306(11) 0.4805(16) 0.9642(15) 0.049(2) Uiso 0.136(3) 1 d . U P A 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 0.01873(12) 0.02288(12) 0.01965(12) 0.00080(6) 0.01058(9) 0.00178(6) P1 0.0186(3) 0.0256(3) 0.0197(3) -0.0005(2) 0.0105(2) 0.0005(2) P2 0.0200(3) 0.0258(3) 0.0221(3) -0.0001(2) 0.0117(2) 0.0027(2) S1A 0.0469(6) 0.0345(4) 0.0440(5) -0.0094(3) 0.0330(4) -0.0084(4) O4 0.0448(18) 0.0328(16) 0.060(2) 0.000 0.0254(17) 0.000 F4A 0.061(2) 0.060(2) 0.0323(12) -0.0094(14) 0.0212(15) -0.0167(15) F3A 0.0655(19) 0.0546(17) 0.0398(13) -0.0038(12) 0.0246(14) -0.0247(13) O3A 0.049(2) 0.0430(14) 0.0422(15) -0.0081(11) 0.0296(18) -0.0136(18) N1 0.0261(11) 0.0307(11) 0.0254(11) 0.0061(9) 0.0131(9) 0.0011(9) N2 0.0241(10) 0.0285(11) 0.0203(10) 0.0005(8) 0.0108(9) 0.0018(8) F5A 0.0428(11) 0.0781(15) 0.0548(13) -0.0124(11) 0.0323(10) -0.0066(11) C1 0.0217(12) 0.0287(12) 0.0188(11) 0.0044(9) 0.0104(10) 0.0048(10) O1A 0.069(2) 0.0555(19) 0.0403(15) -0.0116(13) 0.0355(14) -0.0207(14) C24 0.0237(12) 0.0253(12) 0.0279(13) -0.0027(10) 0.0142(11) 0.0019(9) C26 0.0326(14) 0.0277(13) 0.0260(13) 0.0017(10) 0.0132(11) 0.0059(11) C30 0.0201(12) 0.0317(13) 0.0234(12) 0.0014(10) 0.0107(10) 0.0039(10) C29 0.0236(12) 0.0313(13) 0.0282(13) -0.0007(10) 0.0150(11) 0.0035(10) C18 0.0249(12) 0.0289(13) 0.0253(12) -0.0015(10) 0.0136(10) 0.0002(10) C2 0.0295(14) 0.0305(14) 0.0347(15) 0.0055(11) 0.0165(12) 0.0001(11) C35 0.0241(12) 0.0344(14) 0.0298(13) -0.0008(11) 0.0165(11) 0.0011(10) C27 0.0246(13) 0.0321(14) 0.0314(14) -0.0021(11) 0.0082(11) 0.0052(10) C7 0.0270(14) 0.0369(14) 0.0251(14) 0.0048(10) 0.0134(12) 0.0068(10) C25 0.0287(13) 0.0245(12) 0.0304(13) 0.0010(10) 0.0163(11) 0.0041(10) C23 0.0254(13) 0.0319(14) 0.0396(15) -0.0029(11) 0.0179(12) 0.0009(11) C31 0.0228(12) 0.0345(14) 0.0255(13) -0.0016(10) 0.0128(10) 0.0041(10) C10 0.0330(14) 0.0335(14) 0.0311(14) -0.0034(11) 0.0163(12) 0.0034(11) C17 0.0287(14) 0.0292(14) 0.0280(14) -0.0050(10) 0.0159(12) -0.0036(10) C34 0.0301(14) 0.0334(14) 0.0383(15) 0.0055(12) 0.0196(13) 0.0017(11) C12 0.0214(11) 0.0248(11) 0.0225(11) -0.0014(9) 0.0124(10) 0.0017(9) C9 0.0289(13) 0.0279(13) 0.0267(13) -0.0006(10) 0.0152(11) -0.0008(10) C3 0.0323(15) 0.0409(16) 0.0486(18) 0.0055(13) 0.0235(14) -0.0011(12) C28 0.0236(13) 0.0358(14) 0.0340(14) -0.0044(11) 0.0154(12) 0.0013(11) C33 0.0315(14) 0.0484(17) 0.0322(14) 0.0076(12) 0.0212(12) 0.0056(12) C13 0.0320(14) 0.0315(13) 0.0257(13) 0.0015(10) 0.0167(11) 0.0022(11) C14 0.0371(15) 0.0384(15) 0.0305(14) -0.0007(12) 0.0218(13) 0.0040(12) C32 0.0290(14) 0.0451(16) 0.0271(14) -0.0008(12) 0.0167(12) 0.0050(12) C11 0.0318(14) 0.0327(14) 0.0410(16) -0.0059(12) 0.0217(13) -0.0035(11) C5 0.0295(14) 0.0388(15) 0.0282(14) 0.0070(11) 0.0135(12) 0.0074(11) C19 0.0252(13) 0.0338(14) 0.0417(16) -0.0053(12) 0.0178(12) -0.0006(11) C4 0.0434(17) 0.0321(15) 0.0510(19) 0.0068(13) 0.0261(16) 0.0028(13) F2B 0.048(2) 0.063(3) 0.123(4) -0.033(2) 0.035(2) 0.0023(18) C16 0.0357(15) 0.0323(14) 0.0412(16) -0.0098(12) 0.0217(13) -0.0067(11) C8 0.0330(15) 0.0478(17) 0.0262(14) 0.0025(12) 0.0115(12) 0.0041(13) C22 0.0363(17) 0.0310(15) 0.0500(19) -0.0016(12) 0.0242(15) 0.0064(11) C6 0.0418(18) 0.056(2) 0.0343(16) 0.0172(15) 0.0155(14) 0.0027(15) O2A 0.0571(16) 0.0561(16) 0.0758(18) -0.0029(14) 0.0382(14) 0.0077(13) C15 0.0353(15) 0.0425(16) 0.0318(15) -0.0114(12) 0.0172(13) 0.0000(12) C20 0.0311(15) 0.0387(16) 0.0521(19) -0.0098(14) 0.0227(15) -0.0059(12) C21 0.0420(17) 0.0291(14) 0.0499(18) -0.0069(13) 0.0263(15) -0.0054(12) C36A 0.0478(16) 0.0456(16) 0.0337(14) -0.0082(13) 0.0238(13) -0.0139(14) C43 0.084(3) 0.040(2) 0.085(3) 0.0186(19) 0.056(3) 0.0216(19) F1B 0.060(2) 0.071(3) 0.220(7) -0.017(3) 0.087(3) -0.017(2) C44 0.060(3) 0.070(3) 0.064(3) 0.024(2) 0.023(2) 0.011(2) C40A 0.068(4) 0.043(4) 0.147(6) -0.002(5) 0.079(4) 0.001(4) C41A 0.069(4) 0.041(4) 0.102(5) -0.009(4) 0.063(4) -0.001(3) C42A 0.055(4) 0.040(3) 0.083(4) -0.014(3) 0.041(3) -0.015(3) C37A 0.043(3) 0.038(3) 0.087(4) -0.022(3) 0.038(3) -0.013(2) C38A 0.036(3) 0.035(3) 0.116(4) -0.031(3) 0.040(3) -0.007(2) C39A 0.049(3) 0.039(4) 0.149(6) -0.019(4) 0.066(4) -0.007(3) F2A 0.101(8) 0.052(5) 0.069(6) 0.007(4) 0.049(6) 0.009(5) C42B 0.029(5) 0.035(7) 0.059(6) -0.019(5) 0.020(5) -0.010(5) C37B 0.042(7) 0.032(6) 0.064(6) -0.004(5) 0.027(5) -0.005(5) C38B 0.035(6) 0.039(7) 0.073(6) 0.000(6) 0.023(5) -0.002(5) C39B 0.059(7) 0.043(7) 0.083(8) 0.002(6) 0.040(6) 0.005(6) C40B 0.071(8) 0.043(8) 0.080(8) 0.002(7) 0.039(6) -0.002(6) C41B 0.072(9) 0.051(12) 0.072(9) -0.003(9) 0.031(8) -0.010(9) F1A 0.052(6) 0.075(7) 0.073(6) -0.012(5) 0.005(5) 0.009(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' 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 12 -8 -6 0.0497 16 0 -12 0.0782 6 8 4 0.0421 0 9 8 0.0326 9 -9 -4 0.0422 -3 6 12 0.0389 0 -5 -12 0.0451 0 4 -5 0.0459 -13 3 -2 0.0616 -15 -5 8 0.0541 1 -7 9 0.0371 15 1 -3 0.0526 1 11 1 0.0279 -7 -5 -7 0.0383 -2 -9 -7 0.0293 -9 2 15 0.0433 0 -1 13 0.0331 -11 -7 -1 0.0364 1 -11 3 0.0275 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 P1 53.53(3) . 2_556 ? P2 Pd1 P1 107.09(2) . 2_556 ? P2 Pd1 P1 158.58(2) . . ? C1 Pd1 P1 104.63(7) . . ? C1 Pd1 P1 156.70(7) . 2_556 ? C1 Pd1 P2 95.70(7) . . ? Pd1 P1 Pd1 108.01(2) . 2_556 ? P1 P1 Pd1 62.30(3) 2_556 2_556 ? P1 P1 Pd1 64.17(3) 2_556 . ? C12 P1 Pd1 124.34(8) . 2_556 ? C12 P1 Pd1 125.45(8) . . ? C12 P1 P1 126.75(8) . 2_556 ? C24 P2 Pd1 121.07(8) . . ? C30 P2 Pd1 112.60(9) . . ? C30 P2 C24 103.66(12) . . ? C30 P2 C18 105.80(12) . . ? C18 P2 Pd1 110.87(9) . . ? C18 P2 C24 101.33(12) . . ? O3A S1A O1A 115.1(3) . . ? O3A S1A O2A 113.2(3) . . ? O3A S1A C36A 103.3(3) . . ? O1A S1A C36A 102.4(2) . . ? O2A S1A O1A 118.2(2) . . ? O2A S1A C36A 101.6(2) . . ? C43 O4 C43 114.0(5) 2_757 . ? C1 N1 C2 122.4(2) . . ? C1 N1 C5 109.8(2) . . ? C5 N1 C2 127.8(2) . . ? C1 N2 C7 109.7(2) . . ? C1 N2 C9 122.6(2) . . ? C7 N2 C9 127.2(2) . . ? N1 C1 Pd1 125.5(2) . . ? N1 C1 N2 106.8(2) . . ? N2 C1 Pd1 127.59(19) . . ? C29 C24 P2 122.1(2) . . ? C25 C24 P2 118.6(2) . . ? C25 C24 C29 119.3(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C25 C26 C27 119.7(3) . . ? C35 C30 P2 117.2(2) . . ? C31 C30 P2 123.2(2) . . ? C31 C30 C35 119.6(3) . . ? C24 C29 H29 120.2 . . ? C28 C29 C24 119.6(3) . . ? C28 C29 H29 120.2 . . ? C23 C18 P2 121.2(2) . . ? C19 C18 P2 119.7(2) . . ? C19 C18 C23 119.2(3) . . ? N1 C2 H2 106.4 . . ? N1 C2 C3 111.7(3) . . ? N1 C2 C4 111.5(2) . . ? C3 C2 H2 106.4 . . ? C4 C2 H2 106.4 . . ? C4 C2 C3 113.9(3) . . ? C30 C35 H35 120.2 . . ? C34 C35 C30 119.6(3) . . ? C34 C35 H35 120.2 . . ? C26 C27 H27 120.0 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? N2 C7 C8 124.8(3) . . ? C5 C7 N2 106.6(3) . . ? C5 C7 C8 128.3(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25 119.6 . . ? C18 C23 H23 119.7 . . ? C22 C23 C18 120.6(3) . . ? C22 C23 H23 119.7 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H17A C17 H17B 108.1 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? C12 C17 C16 110.5(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C35 C34 H34 119.8 . . ? C35 C34 C33 120.3(3) . . ? C33 C34 H34 119.8 . . ? P1 C12 H12 108.5 . . ? C17 C12 P1 111.55(17) . . ? C17 C12 H12 108.5 . . ? C17 C12 C13 111.2(2) . . ? C13 C12 P1 108.61(18) . . ? C13 C12 H12 108.5 . . ? N2 C9 C10 111.2(2) . . ? N2 C9 H9 106.9 . . ? N2 C9 C11 113.9(2) . . ? C10 C9 H9 106.9 . . ? C11 C9 C10 110.7(2) . . ? C11 C9 H9 106.9 . . ? 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 . . ? C29 C28 H28 119.7 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.7 . . ? C34 C33 H33 119.9 . . ? C32 C33 C34 120.1(3) . . ? C32 C33 H33 119.9 . . ? C12 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C12 C13 C14 109.9(2) . . ? H13A C13 H13B 108.2 . . ? C14 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C15 C14 C13 111.0(2) . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.9 . . ? 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 . . ? N1 C5 C6 125.0(3) . . ? C7 C5 N1 107.0(2) . . ? C7 C5 C6 128.0(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.0 . . ? 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 . . ? C17 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C15 C16 C17 112.1(3) . . ? C15 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? 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 . . ? C23 C22 H22 120.0 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 120.0 . . ? 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 . . ? C14 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 C14 111.1(2) . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C19 C20 H20 119.6 . . ? C19 C20 C21 120.7(3) . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? F4A C36A S1A 110.6(3) . . ? F4A C36A F3A 104.7(4) . . ? F3A C36A S1A 111.0(3) . . ? F5A C36A S1A 111.2(3) . . ? F5A C36A F4A 109.9(3) . . ? F5A C36A F3A 109.3(3) . . ? O4 C43 H43A 109.7 . . ? O4 C43 H43B 109.7 . . ? O4 C43 C44 110.0(3) . . ? H43A C43 H43B 108.2 . . ? C44 C43 H43A 109.7 . . ? C44 C43 H43B 109.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41A C40A H40A 120.0 . . ? C41A C40A C39A 120.0 . . ? C39A C40A H40A 120.0 . . ? C40A C41A H41A 120.0 . . ? C42A C41A C40A 120.0 . . ? C42A C41A H41A 120.0 . . ? C41A C42A H42A 120.0 . . ? C37A C42A C41A 120.0 . . ? C37A C42A H42A 120.0 . . ? C42A C37A H37A 120.0 . . ? C38A C37A C42A 120.0 . . ? C38A C37A H37A 120.0 . . ? F2B C38A C37A 120.4(5) . . ? F2B C38A C39A 119.6(5) . . ? C37A C38A C39A 120.0 . . ? F1B C39A C40A 122.1(7) . . ? F1B C39A C38A 117.9(7) . . ? C38A C39A C40A 120.0 . . ? C37B C42B H42B 120.0 . . ? C37B C42B C41B 120.0 . . ? C41B C42B H42B 120.0 . . ? F2A C37B C42B 117.4(12) . . ? F2A C37B C38B 122.5(12) . . ? C42B C37B C38B 120.0 . . ? C39B C38B C37B 120.0 . . ? F1A C38B C37B 115.0(12) . . ? F1A C38B C39B 125.0(12) . . ? C38B C39B H39B 120.0 . . ? C40B C39B C38B 120.0 . . ? C40B C39B H39B 120.0 . . ? C39B C40B H40B 120.0 . . ? C39B C40B C41B 120.0 . . ? C41B C40B H40B 120.0 . . ? C42B C41B H41B 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? O1B S1B O2B 133.0(15) . . ? O1B S1B C36B 101.2(14) . . ? O2B S1B C36B 92.5(16) . . ? O3B S1B O1B 89(2) . . ? O3B S1B O2B 122(3) . . ? O3B S1B C36B 120(3) . . ? F3B C36B S1B 94(2) . . ? F5B C36B S1B 109(2) . . ? F5B C36B F3B 125(3) . . ? F4B C36B S1B 94(2) . . ? F4B C36B F3B 95(3) . . ? F4B C36B F5B 131(3) . . ? 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 2.3295(6) . ? Pd1 P1 2.3683(6) 2_556 ? Pd1 P2 2.3213(6) . ? Pd1 C1 2.061(2) . ? P1 P1 2.1160(12) 2_556 ? P1 C12 1.855(2) . ? P2 C24 1.831(3) . ? P2 C30 1.822(3) . ? P2 C18 1.828(3) . ? S1A O3A 1.420(7) . ? S1A O1A 1.450(4) . ? S1A O2A 1.438(4) . ? S1A C36A 1.815(4) . ? O4 C43 1.418(5) 2_757 ? O4 C43 1.418(5) . ? F4A C36A 1.352(6) . ? F3A C36A 1.366(5) . ? N1 C1 1.346(3) . ? N1 C2 1.478(4) . ? N1 C5 1.395(4) . ? N2 C1 1.347(4) . ? N2 C7 1.400(4) . ? N2 C9 1.486(3) . ? F5A C36A 1.338(5) . ? C24 C29 1.400(4) . ? C24 C25 1.394(4) . ? C26 H26 0.9300 . ? C26 C27 1.394(4) . ? C26 C25 1.386(4) . ? C30 C35 1.403(4) . ? C30 C31 1.392(4) . ? C29 H29 0.9300 . ? C29 C28 1.394(4) . ? C18 C23 1.396(4) . ? C18 C19 1.394(4) . ? C2 H2 0.9800 . ? C2 C3 1.528(4) . ? C2 C4 1.522(4) . ? C35 H35 0.9300 . ? C35 C34 1.384(4) . ? C27 H27 0.9300 . ? C27 C28 1.383(4) . ? C7 C5 1.355(4) . ? C7 C8 1.487(4) . ? C25 H25 0.9300 . ? C23 H23 0.9300 . ? C23 C22 1.388(4) . ? C31 H31 0.9300 . ? C31 C32 1.391(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 C9 1.527(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C12 1.530(4) . ? C17 C16 1.536(4) . ? C34 H34 0.9300 . ? C34 C33 1.389(4) . ? C12 H12 0.9800 . ? C12 C13 1.534(3) . ? C9 H9 0.9800 . ? C9 C11 1.523(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C28 H28 0.9300 . ? C33 H33 0.9300 . ? C33 C32 1.377(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.534(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.528(4) . ? C32 H32 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C5 C6 1.494(4) . ? C19 H19 0.9300 . ? C19 C20 1.386(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? F2B C38A 1.351(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C15 1.524(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C22 H22 0.9300 . ? C22 C21 1.384(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C20 H20 0.9300 . ? C20 C21 1.392(5) . ? C21 H21 0.9300 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.487(7) . ? F1B C39A 1.319(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C40A H40A 0.9300 . ? C40A C41A 1.3900 . ? C40A C39A 1.3900 . ? C41A H41A 0.9300 . ? C41A C42A 1.3900 . ? C42A H42A 0.9300 . ? C42A C37A 1.3900 . ? C37A H37A 0.9300 . ? C37A C38A 1.3900 . ? C38A C39A 1.3900 . ? F2A C37B 1.315(15) . ? C42B H42B 0.9300 . ? C42B C37B 1.3900 . ? C42B C41B 1.3900 . ? C37B C38B 1.3900 . ? C38B C39B 1.3900 . ? C38B F1A 1.311(14) . ? C39B H39B 0.9300 . ? C39B C40B 1.3900 . ? C40B H40B 0.9300 . ? C40B C41B 1.3900 . ? C41B H41B 0.9300 . ? S1B O1B 1.41(2) . ? S1B O2B 1.49(3) . ? S1B O3B 1.34(6) . ? S1B C36B 1.88(3) . ? C36B F3B 1.59(5) . ? C36B F5B 1.36(4) . ? C36B F4B 1.33(4) . ? 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 C12 C17 37.7(2) . . . . ? Pd1 P1 C12 C17 -123.41(17) 2_556 . . . ? Pd1 P1 C12 C13 113.66(17) 2_556 . . . ? Pd1 P1 C12 C13 -85.25(18) . . . . ? Pd1 P2 C24 C29 -128.4(2) . . . . ? Pd1 P2 C24 C25 52.1(2) . . . . ? Pd1 P2 C30 C35 54.8(2) . . . . ? Pd1 P2 C30 C31 -124.9(2) . . . . ? Pd1 P2 C18 C23 -158.8(2) . . . . ? Pd1 P2 C18 C19 20.2(3) . . . . ? P1 P1 C12 C17 -44.5(2) 2_556 . . . ? P1 P1 C12 C13 -167.45(14) 2_556 . . . ? P1 C12 C13 C14 -179.08(19) . . . . ? P2 C24 C29 C28 179.7(2) . . . . ? P2 C24 C25 C26 -179.3(2) . . . . ? P2 C30 C35 C34 -179.8(2) . . . . ? P2 C30 C31 C32 179.1(2) . . . . ? P2 C18 C23 C22 179.8(3) . . . . ? P2 C18 C19 C20 -179.2(3) . . . . ? O3A S1A C36A F4A -67.6(4) . . . . ? O3A S1A C36A F3A 176.7(4) . . . . ? O3A S1A C36A F5A 54.8(4) . . . . ? N2 C7 C5 N1 1.5(3) . . . . ? N2 C7 C5 C6 -179.0(3) . . . . ? C1 N1 C2 C3 -113.4(3) . . . . ? C1 N1 C2 C4 117.8(3) . . . . ? C1 N1 C5 C7 -0.9(3) . . . . ? C1 N1 C5 C6 179.6(3) . . . . ? C1 N2 C7 C5 -1.6(3) . . . . ? C1 N2 C7 C8 172.2(3) . . . . ? C1 N2 C9 C10 112.4(3) . . . . ? C1 N2 C9 C11 -121.7(3) . . . . ? O1A S1A C36A F4A 172.6(3) . . . . ? O1A S1A C36A F3A 56.8(4) . . . . ? O1A S1A C36A F5A -65.1(3) . . . . ? C24 P2 C30 C35 -77.8(2) . . . . ? C24 P2 C30 C31 102.5(2) . . . . ? C24 P2 C18 C23 -29.1(3) . . . . ? C24 P2 C18 C19 150.0(2) . . . . ? C24 C29 C28 C27 -0.4(4) . . . . ? C26 C27 C28 C29 1.1(4) . . . . ? C30 P2 C24 C29 -0.9(2) . . . . ? C30 P2 C24 C25 179.5(2) . . . . ? C30 P2 C18 C23 78.8(3) . . . . ? C30 P2 C18 C19 -102.2(2) . . . . ? C30 C35 C34 C33 0.9(4) . . . . ? C30 C31 C32 C33 0.5(4) . . . . ? C29 C24 C25 C26 1.1(4) . . . . ? C18 P2 C24 C29 108.6(2) . . . . ? C18 P2 C24 C25 -71.0(2) . . . . ? C18 P2 C30 C35 176.0(2) . . . . ? C18 P2 C30 C31 -3.7(3) . . . . ? C18 C23 C22 C21 -0.9(5) . . . . ? C18 C19 C20 C21 -0.2(5) . . . . ? C2 N1 C1 Pd1 -2.1(4) . . . . ? C2 N1 C1 N2 -178.5(2) . . . . ? C2 N1 C5 C7 177.4(3) . . . . ? C2 N1 C5 C6 -2.1(5) . . . . ? C35 C30 C31 C32 -0.6(4) . . . . ? C35 C34 C33 C32 -0.9(4) . . . . ? C27 C26 C25 C24 -0.3(4) . . . . ? C7 N2 C1 Pd1 -175.30(19) . . . . ? C7 N2 C1 N1 1.0(3) . . . . ? C7 N2 C9 C10 -58.7(3) . . . . ? C7 N2 C9 C11 67.2(3) . . . . ? C25 C24 C29 C28 -0.8(4) . . . . ? C25 C26 C27 C28 -0.8(4) . . . . ? C23 C18 C19 C20 -0.1(5) . . . . ? C23 C22 C21 C20 0.6(5) . . . . ? C31 C30 C35 C34 -0.1(4) . . . . ? C17 C12 C13 C14 57.8(3) . . . . ? C17 C16 C15 C14 -54.5(3) . . . . ? C34 C33 C32 C31 0.2(4) . . . . ? C12 C17 C16 C15 54.3(3) . . . . ? C12 C13 C14 C15 -57.5(3) . . . . ? C9 N2 C1 Pd1 12.2(4) . . . . ? C9 N2 C1 N1 -171.4(2) . . . . ? C9 N2 C7 C5 170.4(2) . . . . ? C9 N2 C7 C8 -15.8(4) . . . . ? C13 C14 C15 C16 56.1(3) . . . . ? C5 N1 C1 Pd1 176.34(19) . . . . ? C5 N1 C1 N2 -0.1(3) . . . . ? C5 N1 C2 C3 68.5(4) . . . . ? C5 N1 C2 C4 -60.3(4) . . . . ? C19 C18 C23 C22 0.7(5) . . . . ? C19 C20 C21 C22 0.0(6) . . . . ? F2B C38A C39A F1B -1.7(5) . . . . ? F2B C38A C39A C40A 179.6(5) . . . . ? C16 C17 C12 P1 -177.4(2) . . . . ? C16 C17 C12 C13 -56.0(3) . . . . ? C8 C7 C5 N1 -172.0(3) . . . . ? C8 C7 C5 C6 7.5(5) . . . . ? O2A S1A C36A F4A 49.9(4) . . . . ? O2A S1A C36A F3A -65.8(3) . . . . ? O2A S1A C36A F5A 172.3(3) . . . . ? C43 O4 C43 C44 174.2(5) 2_757 . . . ? C40A C41A C42A C37A 0.0 . . . . ? C41A C40A C39A F1B -178.6(5) . . . . ? C41A C40A C39A C38A 0.0 . . . . ? C41A C42A C37A C38A 0.0 . . . . ? C42A C37A C38A F2B -179.6(5) . . . . ? C42A C37A C38A C39A 0.0 . . . . ? C37A C38A C39A F1B 178.7(5) . . . . ? C37A C38A C39A C40A 0.0 . . . . ? C39A C40A C41A C42A 0.0 . . . . ? F2A C37B C38B C39B -177.9(13) . . . . ? F2A C37B C38B F1A 4.3(13) . . . . ? C42B C37B C38B C39B 0.0 . . . . ? C42B C37B C38B F1A -177.7(14) . . . . ? C37B C42B C41B C40B 0.0 . . . . ? C37B C38B C39B C40B 0.0 . . . . ? C38B C39B C40B C41B 0.0 . . . . ? C39B C40B C41B C42B 0.0 . . . . ? C41B C42B C37B F2A 178.0(12) . . . . ? C41B C42B C37B C38B 0.0 . . . . ? F1A C38B C39B C40B 177.5(16) . . . . ? O1B S1B C36B F3B -48(2) . . . . ? O1B S1B C36B F5B -177.2(19) . . . . ? O1B S1B C36B F4B 47(2) . . . . ? O2B S1B C36B F3B 178(2) . . . . ? O2B S1B C36B F5B 48(2) . . . . ? O2B S1B C36B F4B -87(2) . . . . ? O3B S1B C36B F3B 48(4) . . . . ? O3B S1B C36B F5B -82(4) . . . . ? O3B S1B C36B F4B 143(3) . . . . ? 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 11.6517 -7.8830 -5.9692 -0.0174 -0.7310 0.6821 15.6927 -0.0614 -12.1965 0.7338 -0.5613 0.3828 6.0039 8.3598 4.1297 0.5729 0.7488 0.3332 -0.3924 8.7987 7.8563 0.3312 0.9381 0.1014 8.5284 -9.4053 -3.6635 -0.2550 -0.7185 0.6471 -2.6448 6.3677 11.6036 0.0244 0.9746 0.2228 0.4543 -5.3516 -11.5427 -0.0227 -0.9204 -0.3904 0.0000 4.0000 -5.0000 0.3745 -0.0172 -0.3765 -13.0001 3.0000 -2.0001 -0.1166 0.0157 -1.0208 -15.0002 -5.0000 7.9999 -0.9199 0.0406 -0.3951 1.0000 -7.0000 9.0000 -0.6346 0.0479 0.7351 15.0001 1.0000 -2.9999 0.5454 -0.0234 0.7715 0.9998 11.0000 1.0000 0.6800 0.7224 -0.2250 -6.9998 -5.0000 -7.0000 -0.3194 -0.6991 -0.6455 -1.9998 -9.0000 -6.9999 -0.4304 -0.9173 -0.2040 -9.0004 2.0000 14.9999 -0.5042 0.8560 0.1251 -0.0002 -1.0000 12.9999 -0.3939 0.6137 0.6889 -10.9999 -7.0000 -1.0000 -0.7046 -0.5281 -0.5345 1.0001 -11.0000 3.0000 -0.7279 -0.5054 0.5547