#------------------------------------------------------------------------------ #$Date: 2024-10-24 01:06:42 +0300 (Thu, 24 Oct 2024) $ #$Revision: 295596 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572927.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_1572927 loop_ _publ_author_name 'Husbands, David R.' 'Tanner, Theo' 'Whitwood, Adrian C.' 'Hodnett, Neil S.' 'Wheelhouse, Katherine M. P.' 'Fairlamb, Ian J. S.' _publ_section_title ; The ubiquitous P(o-tol)3 ligand promotes formation of catalytically-active higher order palladacyclic clusters ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05346J _journal_year 2024 _chemical_formula_moiety 'C84 H80 Cl2 O P4 Pd4, 1.435(C H2 Cl2), 0.295(C5 H12)' _chemical_formula_sum 'C86.91 H86.4 Cl4.87 O P4 Pd4' _chemical_formula_weight 1869.00 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-09-25 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-09-26 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 82.3154(14) _cell_angle_beta 83.1540(13) _cell_angle_gamma 82.3315(13) _cell_formula_units_Z 2 _cell_length_a 13.9903(2) _cell_length_b 15.1118(2) _cell_length_c 19.6632(3) _cell_measurement_reflns_used 29947 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 76.6730 _cell_measurement_theta_min 3.9330 _cell_volume 4061.19(10) _computing_cell_refinement 'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 42.70a 64-bit (release 22-09-2022))' _computing_data_reduction 'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 110.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -84.00 -21.00 0.50 5.15 -- -48.95 130.00-124.00 126 2 \w -119.00 -94.00 0.50 5.15 -- -48.95-130.00 163.00 50 3 \w -108.00 -65.00 0.50 5.15 -- -48.95-139.00 -10.00 86 4 \w -96.00 -70.00 0.50 5.15 -- -48.95 139.00 49.00 52 5 \w 38.00 98.00 0.50 5.15 -- 48.95-130.00 163.00 120 6 \w 42.00 100.00 0.50 5.15 -- 48.95-139.00 -10.00 116 7 \w 128.00 160.00 0.50 20.60 -- 107.75 139.00 49.00 64 8 \w 76.00 102.00 0.50 20.60 -- 107.75-130.00 163.00 52 9 \w 119.00 145.00 0.50 20.60 -- 107.75 130.00-124.00 52 10 \w 83.00 113.00 0.50 20.60 -- 107.75-139.00 -10.00 60 11 \w -61.00 -35.00 0.50 5.15 -- -48.95 37.00-180.00 52 12 \w -116.00 -26.00 0.50 5.15 -- -48.95 -77.00-150.00 180 13 \w -101.00 -76.00 0.50 5.15 -- -48.95 -77.00 90.00 50 14 \w -119.00 -74.00 0.50 5.15 -- -48.95-125.00-150.00 90 15 \w -118.00 -87.00 0.50 5.15 -- -48.95-125.00-180.00 62 16 \w -28.00 24.00 0.50 5.15 -- -48.95 37.00-180.00 104 17 \w -116.00 -83.00 0.50 5.15 -- -48.95-125.00 30.00 66 18 \w -20.00 58.00 0.50 5.15 -- 48.95 -57.00 150.00 156 19 \w 37.00 122.00 0.50 20.60 -- 107.75 -57.00 -60.00 170 20 \w 80.00 130.00 0.50 20.60 -- 107.75 -77.00 150.00 100 21 \w 38.00 106.00 0.50 20.60 -- 107.75 -99.00 150.00 136 22 \w 114.00 174.00 0.50 20.60 -- 107.75 125.00-180.00 120 23 \w 38.00 66.00 0.50 20.60 -- 107.75-125.00 0.00 56 24 \w 80.00 112.00 0.50 20.60 -- 107.75-125.00 0.00 64 25 \w 40.00 119.00 0.50 20.60 -- 107.75 -37.00 120.00 158 26 \w 35.00 61.00 0.50 20.60 -- 107.75 -77.00 150.00 52 27 \w 71.00 106.00 0.50 20.60 -- 107.75 -99.00-150.00 70 28 \w 102.00 177.00 0.50 20.60 -- 107.75 37.00-120.00 150 29 \w 40.00 105.00 0.50 20.60 -- 107.75 -99.00 90.00 130 30 \w 98.00 178.00 0.50 20.60 -- 107.75 37.00 -90.00 160 31 \w 33.00 119.00 0.50 20.60 -- 107.75 -19.00 90.00 172 32 \w 37.00 101.00 0.50 20.60 -- 107.75 -99.00 -30.00 128 33 \w 91.00 126.00 0.50 20.60 -- 107.75-144.00 94.56 70 34 \w 130.00 178.00 0.50 20.60 -- 107.75 19.00 -60.00 96 35 \w 41.00 110.00 0.50 20.60 -- 107.75 -37.00 -60.00 138 36 \w 113.00 139.00 0.50 20.60 -- 107.75 125.00 90.00 52 37 \w 125.00 167.00 0.50 20.60 -- 107.75 19.00 0.00 84 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0219357000 _diffrn_orient_matrix_UB_12 -0.0003585000 _diffrn_orient_matrix_UB_13 -0.0748955000 _diffrn_orient_matrix_UB_21 0.0909737000 _diffrn_orient_matrix_UB_22 0.0467263000 _diffrn_orient_matrix_UB_23 -0.0264972000 _diffrn_orient_matrix_UB_31 0.0609991000 _diffrn_orient_matrix_UB_32 -0.0924744000 _diffrn_orient_matrix_UB_33 -0.0024361000 _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 0.0414 _diffrn_reflns_av_unetI/netI 0.0387 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 50180 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.075 _diffrn_reflns_theta_max 67.075 _diffrn_reflns_theta_min 3.523 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.597 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024) 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_density_diffrn 1.528 _exptl_crystal_description sphere _exptl_crystal_F_000 1885 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad 0.024 _refine_diff_density_max 1.120 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 952 _refine_ls_number_reflns 14483 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0326 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.8381P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.0874 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12849 _reflns_number_total 14483 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05346j3.cif _cod_data_source_block ijsf22044 _cod_original_cell_volume 4061.19(11) _cod_original_formula_sum 'C86.91 H86.40 Cl4.87 O P4 Pd4' _cod_database_code 1572927 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C87.5 H87 Cl5.2 O1 P4 Pd4' _chemical_oxdiff_usercomment 'David Husbands DRH-03-75' _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 0.762 _shelx_estimated_absorpt_t_min 0.327 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C91-C90 = C90-C89 = C88-C89 = C88-C87 1.53 with sigma of 0.02 C21A-C20A 1.54 with sigma of 0.02 C88-C90 = C89-C91 2.48 with sigma of 0.04 C87-C89 2.48 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C18) = Uanis(C18A) Uanis(C19) = Uanis(C19A) Uanis(C61) = Uanis(C20) = Uanis(C20A) Uanis(C17A) = Uanis(C17) Uanis(C21) = Uanis(C21A) Uanis(C16A) = Uanis(C16) Uanis(Cl6) = Uanis(C89) Uanis(C86) = Uanis(C88) Uanis(Cl5) = Uanis(C87) Uanis(C89) = Uanis(Cl6) 4. Others Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)= Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1) Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)= Sof(C20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1) Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(Cl5)=Sof(Cl6)=FVAR(2) Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)= Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)= Sof(H91C)=FVAR(3) Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(Cl3)=Sof(Cl4)=FVAR(4) 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C64(H64A,H64B), C86(H86A,H86B), C85(H85A,H85B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B) 5.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A), C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60), C61(H61), C66(H66), C67(H67), C68(H68), C69(H69), C72(H72), C73(H73), C74(H74), C75(H75), C79(H79), C80(H80), C81(H81), C82(H82) 5.c Fitted hexagon refined as free rotating group: C15(C16A,C17A,C18A,C19A,C20A) 5.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C35(H35A,H35B, H35C), C42(H42A,H42B,H42C), C56(H56A,H56B,H56C), C63(H63A,H63B,H63C), C77(H77A, H77B,H77C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C), C91(H91A,H91B,H91C) ; _shelx_res_file ; TITL ijsf22044_a.res in P-1 ijsf22044.res created by SHELXL-2018/3 at 16:32:40 on 25-Sep-2024 REM Old TITL ijsf22044 in P-1 REM SHELXT solution in P-1: R1 0.077, Rweak 0.006, Alpha 0.094 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C86 F5 P6 Pd4 CELL 1.54184 13.990341 15.111766 19.663192 82.3154 83.154 82.3315 ZERR 2 0.000212 0.000243 0.000332 0.0014 0.0013 0.0013 LATT 1 SFAC C H Cl O P Pd UNIT 173.82 172.81 9.74 2 8 8 EADP C18 C18A EADP C19 C19A EADP C61 C20 C20A EADP C17A C17 EADP C21 C21A EADP C16A C16 DFIX 1.53 C91 C90 C90 C89 C88 C89 C88 C87 EADP Cl6 C89 DANG 2.48 C88 C90 C89 C91 DANG 2.48 C87 C89 EADP C86 C88 EADP Cl5 C87 EADP C89 Cl6 ISOR 0.01 0.02 C90 C91 DFIX 1.54 C21A C20A L.S. 9 0 0 PLAN 23 SIZE 0.03 0.05 0.15 TEMP -163 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 -1 2 REM REM REM WGHT 0.053700 1.838100 FVAR 0.35162 0.72411 0.59057 0.29452 0.84461 C1 1 0.266399 0.903560 0.698483 11.00000 0.02489 0.02716 = 0.03586 0.00102 -0.00489 -0.00422 AFIX 23 H1A 2 0.214941 0.885303 0.674734 11.00000 -1.20000 H1B 2 0.234324 0.937703 0.736244 11.00000 -1.20000 AFIX 0 C2 1 0.324780 0.964289 0.648148 11.00000 0.03128 0.02229 = 0.03050 -0.00584 -0.00265 -0.00236 C3 1 0.286465 1.023486 0.594631 11.00000 0.03850 0.02972 = 0.03987 -0.00167 -0.01071 -0.00683 AFIX 43 H3 2 0.219122 1.028645 0.589798 11.00000 -1.20000 AFIX 0 C4 1 0.346159 1.074908 0.548386 11.00000 0.05185 0.02784 = 0.03196 0.00168 -0.01167 -0.00523 AFIX 43 H4 2 0.319270 1.114177 0.511780 11.00000 -1.20000 AFIX 0 C5 1 0.443977 1.069733 0.554890 11.00000 0.04918 0.02700 = 0.02749 -0.00036 0.00195 -0.01079 AFIX 43 H5 2 0.484147 1.104698 0.522606 11.00000 -1.20000 AFIX 0 C6 1 0.483530 1.013152 0.608871 11.00000 0.03504 0.02875 = 0.03043 -0.00540 0.00027 -0.00858 AFIX 43 H6 2 0.550584 1.009618 0.614204 11.00000 -1.20000 AFIX 0 C7 1 0.423369 0.961845 0.654906 11.00000 0.03071 0.02472 = 0.02448 -0.00453 -0.00108 -0.00465 C8 1 0.583800 0.842507 0.711234 11.00000 0.02609 0.03138 = 0.02945 0.00668 -0.00407 -0.00826 C9 1 0.652886 0.858856 0.752423 11.00000 0.03755 0.05228 = 0.03507 0.00616 -0.00975 -0.01826 AFIX 43 H9 2 0.633102 0.891535 0.790774 11.00000 -1.20000 AFIX 0 C10 1 0.749774 0.827867 0.737821 11.00000 0.03206 0.06405 = 0.05653 0.02176 -0.02222 -0.02234 AFIX 43 H10 2 0.795749 0.838516 0.766749 11.00000 -1.20000 AFIX 0 C11 1 0.780184 0.781893 0.681973 11.00000 0.02360 0.05576 = 0.06991 0.01362 -0.00514 -0.00342 AFIX 43 H11 2 0.847059 0.762290 0.671393 11.00000 -1.20000 AFIX 0 C12 1 0.712082 0.764295 0.641021 11.00000 0.03011 0.03887 = 0.05657 0.00293 0.00222 -0.00256 AFIX 43 H12 2 0.733208 0.732425 0.602394 11.00000 -1.20000 AFIX 0 C13 1 0.613570 0.792344 0.655356 11.00000 0.02746 0.02990 = 0.03826 0.00384 -0.00150 -0.00594 C14 1 0.543143 0.765338 0.612209 11.00000 0.03228 0.03821 = 0.03637 -0.00786 -0.00074 -0.00376 AFIX 137 H14A 2 0.504071 0.721888 0.640207 11.00000 -1.50000 H14B 2 0.578893 0.737880 0.572821 11.00000 -1.50000 H14C 2 0.500520 0.818627 0.595452 11.00000 -1.50000 AFIX 66 C15 1 0.453723 0.961456 0.795908 11.00000 0.04229 0.05043 = 0.03638 -0.01225 -0.00717 -0.00794 PART 2 C16A 1 0.494571 1.039529 0.769628 -21.00000 0.11259 0.03084 = 0.04588 -0.01066 -0.02337 0.00688 AFIX 43 H16A 2 0.515426 1.050231 0.721792 -21.00000 -1.20000 AFIX 65 C17A 1 0.504906 1.101945 0.813339 -21.00000 0.14230 0.04031 = 0.05386 -0.01588 -0.02746 0.00267 AFIX 43 H17A 2 0.532823 1.155304 0.795377 -21.00000 -1.20000 AFIX 65 C18A 1 0.474393 1.086287 0.883330 -21.00000 0.09464 0.06404 = 0.04918 -0.01548 -0.01680 -0.01184 AFIX 43 H18A 2 0.481457 1.128945 0.913204 -21.00000 -1.20000 AFIX 65 C19A 1 0.433545 1.008214 0.909611 -21.00000 0.05642 0.06248 = 0.04655 -0.01635 -0.01720 -0.00402 AFIX 43 H19A 2 0.412691 0.997514 0.957447 -21.00000 -1.20000 AFIX 65 C20A 1 0.423210 0.945798 0.865901 -21.00000 0.03186 0.03978 = 0.04494 0.00104 -0.01011 -0.00619 AFIX 0 PART 1 C16 1 0.447267 1.056779 0.775447 21.00000 0.11259 0.03084 = 0.04588 -0.01066 -0.02337 0.00688 AFIX 43 H16 2 0.447643 1.079337 0.727954 21.00000 -1.20000 AFIX 0 C17 1 0.440526 1.115938 0.824013 21.00000 0.14230 0.04031 = 0.05386 -0.01588 -0.02746 0.00267 AFIX 43 H17 2 0.435876 1.178880 0.810004 21.00000 -1.20000 AFIX 0 C18 1 0.440563 1.083446 0.892755 21.00000 0.09464 0.06404 = 0.04918 -0.01548 -0.01680 -0.01184 AFIX 43 H18 2 0.440569 1.123901 0.925811 21.00000 -1.20000 AFIX 0 C19 1 0.440593 0.993180 0.914115 21.00000 0.05642 0.06248 = 0.04655 -0.01635 -0.01720 -0.00402 AFIX 43 H19 2 0.435545 0.972320 0.962025 21.00000 -1.20000 AFIX 0 C20 1 0.448011 0.931347 0.865852 21.00000 0.03186 0.03978 = 0.04494 0.00104 -0.01011 -0.00619 C21 1 0.445912 0.834235 0.893181 21.00000 0.11652 0.07633 = 0.03105 0.01247 -0.03222 -0.05399 AFIX 137 H21A 2 0.382880 0.816089 0.887614 21.00000 -1.50000 H21B 2 0.456043 0.825428 0.942209 21.00000 -1.50000 H21C 2 0.497440 0.797601 0.867615 21.00000 -1.50000 AFIX 0 PART 2 C21A 1 0.393133 0.857302 0.883460 -21.00000 0.11652 0.07633 = 0.03105 0.01247 -0.03222 -0.05399 AFIX 137 H21D 2 0.448170 0.811951 0.873450 -21.00000 -1.50000 H21E 2 0.340624 0.851254 0.856194 -21.00000 -1.50000 H21F 2 0.370154 0.848520 0.932677 -21.00000 -1.50000 AFIX 0 PART 0 C22 1 0.168840 0.531297 0.767255 11.00000 0.03142 0.02874 = 0.04227 -0.00109 -0.00650 -0.00792 AFIX 23 H22A 2 0.115370 0.580481 0.773283 11.00000 -1.20000 H22B 2 0.169723 0.514202 0.720286 11.00000 -1.20000 AFIX 0 C23 1 0.148193 0.451755 0.818998 11.00000 0.03245 0.03071 = 0.04022 -0.00450 -0.00565 -0.01012 C24 1 0.055751 0.434102 0.847071 11.00000 0.03684 0.04182 = 0.05611 -0.00521 -0.00286 -0.01220 AFIX 43 H24 2 0.000926 0.474242 0.834093 11.00000 -1.20000 AFIX 0 C25 1 0.042841 0.358162 0.894005 11.00000 0.04331 0.05333 = 0.05253 -0.00172 0.00294 -0.02317 AFIX 43 H25 2 -0.020631 0.346953 0.913168 11.00000 -1.20000 AFIX 0 C26 1 0.122302 0.298711 0.912949 11.00000 0.05160 0.04363 = 0.04147 0.00248 -0.00252 -0.02325 AFIX 43 H26 2 0.112863 0.246347 0.944343 11.00000 -1.20000 AFIX 0 C27 1 0.214466 0.315076 0.886617 11.00000 0.04429 0.03279 = 0.03527 0.00025 -0.00184 -0.01311 AFIX 43 H27 2 0.268814 0.274397 0.899766 11.00000 -1.20000 AFIX 0 C28 1 0.227606 0.391856 0.840444 11.00000 0.03585 0.02765 = 0.03320 -0.00327 0.00042 -0.01101 C29 1 0.418067 0.397759 0.877730 11.00000 0.03407 0.02686 = 0.04300 0.00391 -0.00493 -0.01010 C30 1 0.497340 0.332769 0.870101 11.00000 0.03918 0.03712 = 0.04966 -0.00759 -0.00608 -0.00322 AFIX 43 H30 2 0.512751 0.307693 0.827776 11.00000 -1.20000 AFIX 0 C31 1 0.554303 0.304140 0.923938 11.00000 0.04484 0.05114 = 0.06161 -0.00588 -0.01601 0.00800 AFIX 43 H31 2 0.608680 0.259848 0.918393 11.00000 -1.20000 AFIX 0 C32 1 0.531647 0.340192 0.985324 11.00000 0.05017 0.05735 = 0.05378 -0.00243 -0.01991 -0.00239 AFIX 43 H32 2 0.571056 0.321186 1.021960 11.00000 -1.20000 AFIX 0 C33 1 0.451863 0.403945 0.994092 11.00000 0.05289 0.04389 = 0.04162 -0.00396 -0.01076 -0.00773 AFIX 43 H33 2 0.436327 0.427690 1.036948 11.00000 -1.20000 AFIX 0 C34 1 0.394062 0.433614 0.940448 11.00000 0.04556 0.03355 = 0.03816 -0.00165 -0.00570 -0.00934 C35 1 0.309813 0.503912 0.953189 11.00000 0.06664 0.04781 = 0.03633 -0.00940 -0.00780 0.00830 AFIX 137 H35A 2 0.314813 0.555771 0.917803 11.00000 -1.50000 H35B 2 0.310349 0.523019 0.998832 11.00000 -1.50000 H35C 2 0.249200 0.478902 0.951261 11.00000 -1.50000 AFIX 0 C36 1 0.392801 0.369130 0.736497 11.00000 0.04054 0.02252 = 0.03584 -0.00379 -0.00232 0.00024 C37 1 0.340513 0.305228 0.717624 11.00000 0.04988 0.03796 = 0.04683 -0.01028 -0.00029 -0.00996 AFIX 43 H37 2 0.280799 0.293323 0.743437 11.00000 -1.20000 AFIX 0 C38 1 0.374795 0.259312 0.661894 11.00000 0.07461 0.03912 = 0.05580 -0.01875 -0.00369 -0.00997 AFIX 43 H38 2 0.338896 0.215570 0.649955 11.00000 -1.20000 AFIX 0 C39 1 0.460877 0.276425 0.623323 11.00000 0.07009 0.04034 = 0.05097 -0.01708 0.00855 -0.00555 AFIX 43 H39 2 0.484290 0.244924 0.584828 11.00000 -1.20000 AFIX 0 C40 1 0.512466 0.339855 0.641391 11.00000 0.05089 0.03411 = 0.05625 -0.01106 0.01250 0.00013 AFIX 43 H40 2 0.571994 0.351112 0.615031 11.00000 -1.20000 AFIX 0 C41 1 0.479841 0.388052 0.697279 11.00000 0.04256 0.02655 = 0.04756 -0.00462 0.00225 -0.00049 C42 1 0.538932 0.457798 0.712711 11.00000 0.04461 0.04083 = 0.06134 -0.01418 0.01225 -0.00920 AFIX 137 H42A 2 0.607188 0.441793 0.696288 11.00000 -1.50000 H42B 2 0.532692 0.460353 0.762604 11.00000 -1.50000 H42C 2 0.515400 0.516672 0.689291 11.00000 -1.50000 AFIX 0 C43 1 0.321185 0.661104 0.601427 11.00000 0.02542 0.03931 = 0.03115 -0.00907 -0.00158 -0.00029 AFIX 23 H43A 2 0.361741 0.709127 0.581826 11.00000 -1.20000 H43B 2 0.354545 0.623531 0.638814 11.00000 -1.20000 AFIX 0 C44 1 0.312369 0.604006 0.546220 11.00000 0.02611 0.03391 = 0.02992 -0.00453 0.00563 -0.00795 C45 1 0.373187 0.525105 0.535552 11.00000 0.03075 0.04180 = 0.04371 -0.00946 0.00389 0.00067 AFIX 43 H45 2 0.423169 0.504620 0.564653 11.00000 -1.20000 AFIX 0 C46 1 0.361451 0.476258 0.482911 11.00000 0.04154 0.03795 = 0.06154 -0.01753 0.01581 -0.00359 AFIX 43 H46 2 0.402381 0.421851 0.476830 11.00000 -1.20000 AFIX 0 C47 1 0.290390 0.506395 0.439191 11.00000 0.03945 0.04587 = 0.04594 -0.02402 0.01341 -0.01948 AFIX 43 H47 2 0.284018 0.473707 0.402258 11.00000 -1.20000 AFIX 0 C48 1 0.228631 0.583991 0.449145 11.00000 0.03351 0.04278 = 0.03318 -0.01148 0.00490 -0.01582 AFIX 43 H48 2 0.179621 0.604602 0.419263 11.00000 -1.20000 AFIX 0 C49 1 0.238583 0.631567 0.502947 11.00000 0.02817 0.03033 = 0.02919 -0.00468 0.00469 -0.00890 C50 1 0.039023 0.711358 0.511177 11.00000 0.02474 0.03878 = 0.02911 -0.00993 -0.00049 -0.00748 C51 1 -0.007080 0.772949 0.462195 11.00000 0.02886 0.04245 = 0.03664 -0.00590 -0.00391 -0.00815 AFIX 43 H51 2 0.023527 0.823606 0.441017 11.00000 -1.20000 AFIX 0 C52 1 -0.097176 0.760850 0.444167 11.00000 0.02806 0.06093 = 0.04083 -0.01226 -0.00848 -0.00291 AFIX 43 H52 2 -0.128687 0.803542 0.411560 11.00000 -1.20000 AFIX 0 C53 1 -0.140342 0.686197 0.474125 11.00000 0.02670 0.06881 = 0.05138 -0.02028 -0.00493 -0.01435 AFIX 43 H53 2 -0.201174 0.676547 0.461353 11.00000 -1.20000 AFIX 0 C54 1 -0.094980 0.625267 0.522856 11.00000 0.03707 0.05099 = 0.05049 -0.01371 0.00257 -0.01968 AFIX 43 H54 2 -0.125611 0.574232 0.543117 11.00000 -1.20000 AFIX 0 C55 1 -0.005935 0.636806 0.542871 11.00000 0.03063 0.04159 = 0.03416 -0.00937 0.00196 -0.01151 C56 1 0.037605 0.569189 0.597049 11.00000 0.04128 0.04030 = 0.04704 -0.00049 -0.00065 -0.01858 AFIX 137 H56A 2 0.100602 0.541236 0.577951 11.00000 -1.50000 H56B 2 -0.005717 0.522823 0.611984 11.00000 -1.50000 H56C 2 0.046392 0.599308 0.636628 11.00000 -1.50000 AFIX 0 C57 1 0.192063 0.825645 0.476566 11.00000 0.02432 0.03401 = 0.03301 0.00062 -0.00718 -0.00861 C58 1 0.260078 0.815685 0.419622 11.00000 0.03788 0.03880 = 0.04404 -0.00203 0.00226 -0.00978 AFIX 43 H58 2 0.287151 0.757019 0.410086 11.00000 -1.20000 AFIX 0 C59 1 0.288942 0.889367 0.376756 11.00000 0.04483 0.05416 = 0.05123 0.00261 0.01293 -0.01622 AFIX 43 H59 2 0.335544 0.881263 0.338128 11.00000 -1.20000 AFIX 0 C60 1 0.250097 0.974739 0.390036 11.00000 0.03888 0.04136 = 0.05415 0.01381 -0.00799 -0.01352 AFIX 43 H60 2 0.269994 1.025698 0.360751 11.00000 -1.20000 AFIX 0 C61 1 0.182067 0.985896 0.446143 11.00000 0.03186 0.03978 = 0.04494 0.00104 -0.01011 -0.00619 AFIX 43 H61 2 0.154874 1.045025 0.454363 11.00000 -1.20000 AFIX 0 C62 1 0.152065 0.912955 0.491122 11.00000 0.02528 0.03366 = 0.03600 0.00289 -0.01384 -0.00358 C63 1 0.079619 0.928714 0.552280 11.00000 0.03689 0.03028 = 0.03894 -0.00233 -0.01035 -0.00115 AFIX 137 H63A 2 0.110591 0.909195 0.594809 11.00000 -1.50000 H63B 2 0.025136 0.894320 0.551740 11.00000 -1.50000 H63C 2 0.055818 0.992918 0.550232 11.00000 -1.50000 AFIX 0 C64 1 0.190795 0.723952 0.886795 11.00000 0.03072 0.05120 = 0.02872 -0.00939 -0.00326 0.00475 AFIX 23 H64A 2 0.187057 0.658600 0.898201 11.00000 -1.20000 H64B 2 0.260139 0.731860 0.874762 11.00000 -1.20000 AFIX 0 C65 1 0.156086 0.767805 0.951155 11.00000 0.02742 0.04069 = 0.03144 -0.00897 -0.00063 -0.00641 C66 1 0.202312 0.746451 1.010991 11.00000 0.03204 0.05291 = 0.03201 -0.00715 -0.00390 -0.00437 AFIX 43 H66 2 0.259630 0.704937 1.011262 11.00000 -1.20000 AFIX 0 C67 1 0.165605 0.785178 1.070503 11.00000 0.04360 0.05718 = 0.03032 -0.00915 -0.00481 -0.00652 AFIX 43 H67 2 0.198270 0.770577 1.110939 11.00000 -1.20000 AFIX 0 C68 1 0.080775 0.845502 1.070859 11.00000 0.04586 0.04220 = 0.02667 -0.01037 0.00181 -0.00978 AFIX 43 H68 2 0.055139 0.871048 1.111782 11.00000 -1.20000 AFIX 0 C69 1 0.034330 0.867951 1.012040 11.00000 0.03469 0.03243 = 0.03128 -0.00690 0.00382 -0.00720 AFIX 43 H69 2 -0.023307 0.909063 1.012023 11.00000 -1.20000 AFIX 0 C70 1 0.072751 0.829703 0.952338 11.00000 0.02903 0.03169 = 0.02715 -0.00443 0.00144 -0.01038 C71 1 0.051897 0.968817 0.836353 11.00000 0.03846 0.02675 = 0.03247 -0.00846 0.00984 -0.00129 C72 1 0.125792 1.001465 0.865806 11.00000 0.04155 0.03581 = 0.04240 -0.01123 0.00931 -0.01152 AFIX 43 H72 2 0.151308 0.968011 0.905418 11.00000 -1.20000 AFIX 0 C73 1 0.161500 1.080592 0.838336 11.00000 0.05424 0.04837 = 0.05582 -0.01473 0.00286 -0.02145 AFIX 43 H73 2 0.211313 1.101382 0.858662 11.00000 -1.20000 AFIX 0 C74 1 0.124581 1.128971 0.781517 11.00000 0.06593 0.04310 = 0.05554 -0.00628 0.01253 -0.01847 AFIX 43 H74 2 0.148755 1.183863 0.762680 11.00000 -1.20000 AFIX 0 C75 1 0.052314 1.099155 0.750904 11.00000 0.06342 0.04026 = 0.04089 -0.00412 0.00979 -0.00916 AFIX 43 H75 2 0.027615 1.133825 0.711455 11.00000 -1.20000 AFIX 0 C76 1 0.015072 1.017564 0.777918 11.00000 0.04843 0.03248 = 0.03401 -0.00789 0.00554 -0.00017 C77 1 -0.061413 0.988791 0.741714 11.00000 0.05113 0.03902 = 0.04756 -0.00317 -0.00767 0.00026 AFIX 137 H77A 2 -0.125561 1.010175 0.763436 11.00000 -1.50000 H77B 2 -0.053989 0.923010 0.744833 11.00000 -1.50000 H77C 2 -0.054891 1.014305 0.693110 11.00000 -1.50000 AFIX 0 C78 1 -0.104333 0.853125 0.891400 11.00000 0.02668 0.04589 = 0.02896 -0.00590 -0.00195 -0.00311 C79 1 -0.163301 0.933043 0.901676 11.00000 0.03721 0.05454 = 0.05089 -0.01263 0.00909 0.00015 AFIX 43 H79 2 -0.135725 0.988116 0.894031 11.00000 -1.20000 AFIX 0 C80 1 -0.260947 0.933711 0.922737 11.00000 0.03994 0.07926 = 0.06565 -0.01609 0.01324 0.00830 AFIX 43 H80 2 -0.300600 0.988841 0.928645 11.00000 -1.20000 AFIX 0 C81 1 -0.300087 0.854252 0.935023 11.00000 0.02961 0.10525 = 0.04309 -0.00987 0.00498 -0.00617 AFIX 43 H81 2 -0.367123 0.854293 0.950296 11.00000 -1.20000 AFIX 0 C82 1 -0.243442 0.773889 0.925523 11.00000 0.03913 0.07565 = 0.03503 -0.00474 0.00019 -0.02525 AFIX 43 H82 2 -0.272134 0.719399 0.933956 11.00000 -1.20000 AFIX 0 C83 1 -0.144126 0.771634 0.903593 11.00000 0.03269 0.05555 = 0.02815 -0.00160 -0.00120 -0.01464 C84 1 -0.084760 0.682610 0.894488 11.00000 0.05298 0.04689 = 0.05854 -0.00373 0.00742 -0.02574 AFIX 137 H84A 2 -0.126267 0.634302 0.906554 11.00000 -1.50000 H84B 2 -0.032441 0.672906 0.924642 11.00000 -1.50000 H84C 2 -0.056895 0.682622 0.846337 11.00000 -1.50000 AFIX 0 CL1 3 0.440632 0.651359 0.790493 11.00000 0.02734 0.02612 = 0.04482 -0.00045 -0.00572 -0.00387 CL2 3 0.032950 0.775559 0.699360 11.00000 0.02542 0.04667 = 0.03071 -0.01074 -0.00345 0.00218 O1 4 0.237765 0.707281 0.739947 11.00000 0.02508 0.02212 = 0.02454 -0.00211 0.00021 -0.00466 P1 5 0.456132 0.885146 0.729577 11.00000 0.02642 0.02834 = 0.02368 -0.00208 -0.00311 -0.00868 P2 5 0.341173 0.433998 0.807232 11.00000 0.02975 0.02206 = 0.03305 -0.00189 -0.00086 -0.00506 P3 5 0.158566 0.726566 0.533274 11.00000 0.02388 0.02780 = 0.02566 -0.00362 -0.00223 -0.00614 P4 5 0.026281 0.853308 0.868782 11.00000 0.02467 0.02813 = 0.02632 -0.00661 0.00190 -0.00401 PD1 6 0.346633 0.790176 0.740411 11.00000 0.02174 0.02294 = 0.02392 -0.00081 -0.00222 -0.00491 PD2 6 0.296888 0.578322 0.774828 11.00000 0.02467 0.02084 = 0.02669 -0.00234 -0.00046 -0.00484 PD3 6 0.190294 0.718558 0.642128 11.00000 0.02159 0.02423 = 0.02454 -0.00433 -0.00137 -0.00326 PD4 6 0.121548 0.766445 0.801185 11.00000 0.02193 0.02477 = 0.02387 -0.00522 0.00061 -0.00402 PART 1 C86 1 0.901942 0.315302 0.762764 31.00000 0.11210 0.04001 = 0.03900 0.00138 -0.00518 -0.00164 AFIX 23 H86A 2 0.936703 0.274222 0.797749 31.00000 -1.20000 H86B 2 0.870971 0.368909 0.784430 31.00000 -1.20000 AFIX 0 CL5 3 0.984953 0.348292 0.692824 31.00000 0.15561 0.04583 = 0.04214 0.00541 0.02144 0.00880 CL6 3 0.814300 0.261992 0.736255 31.00000 0.16812 0.09716 = 0.06040 0.00030 -0.05128 -0.04336 PART 0 C85 1 0.715080 0.585153 0.782999 51.00000 0.05357 0.05788 = 0.05346 -0.00719 0.00147 -0.01027 AFIX 23 H85A 2 0.724132 0.641346 0.800890 51.00000 -1.20000 H85B 2 0.656292 0.596961 0.758161 51.00000 -1.20000 AFIX 0 CL3 3 0.817181 0.553268 0.725060 51.00000 0.07874 0.06522 = 0.06767 0.01066 0.01732 0.01398 CL4 3 0.699387 0.501853 0.851030 51.00000 0.12543 0.09465 = 0.04848 0.01564 0.01940 0.00786 PART 2 C87 1 0.944608 0.333247 0.713742 41.00000 0.15561 0.04583 = 0.04214 0.00541 0.02144 0.00880 AFIX 137 H87A 2 0.965094 0.299461 0.674230 41.00000 -1.50000 H87B 2 0.980702 0.306113 0.752617 41.00000 -1.50000 H87C 2 0.957606 0.395790 0.701101 41.00000 -1.50000 AFIX 0 C88 1 0.836837 0.330735 0.734307 41.00000 0.11210 0.04001 = 0.03900 0.00138 -0.00518 -0.00164 AFIX 23 H88A 2 0.817578 0.357492 0.777920 41.00000 -1.20000 H88B 2 0.799546 0.366400 0.698111 41.00000 -1.20000 AFIX 0 C89 1 0.814597 0.234994 0.743590 41.00000 0.16812 0.09716 = 0.06040 0.00030 -0.05128 -0.04336 AFIX 23 H89A 2 0.833815 0.208990 0.699660 41.00000 -1.20000 H89B 2 0.853551 0.199584 0.778963 41.00000 -1.20000 AFIX 0 C90 1 0.710084 0.227338 0.764916 41.00000 0.05899 0.08987 = 0.04919 -0.03090 -0.01398 0.01502 AFIX 23 H90A 2 0.673109 0.243706 0.724239 41.00000 -1.20000 H90B 2 0.684957 0.269783 0.798904 41.00000 -1.20000 AFIX 0 PART 0 C91 1 0.695625 0.131966 0.796683 41.00000 0.06104 0.10215 = 0.04962 -0.02479 -0.01787 0.00302 AFIX 137 H91A 2 0.704683 0.092320 0.760273 41.00000 -1.50000 H91B 2 0.629892 0.131321 0.820270 41.00000 -1.50000 H91C 2 0.742987 0.110830 0.829968 41.00000 -1.50000 AFIX 0 HKLF 4 REM ijsf22044_a.res in P-1 REM wR2 = 0.0874, GooF = S = 1.025, Restrained GooF = 1.026 for all data REM R1 = 0.0326 for 12849 Fo > 4sig(Fo) and 0.0374 for all 14483 data REM 952 parameters refined using 20 restraints END WGHT 0.0537 1.8384 REM Highest difference peak 1.120, deepest hole -0.813, 1-sigma level 0.092 Q1 1 0.3669 0.7420 0.7278 11.00000 0.05 1.12 Q2 1 0.0716 0.8138 0.8322 11.00000 0.05 0.80 Q3 1 0.3892 0.7779 0.7017 11.00000 0.05 0.80 Q4 1 0.1658 0.6631 0.6623 11.00000 0.05 0.80 Q5 1 0.4910 1.0030 0.8196 11.00000 0.05 0.79 Q6 1 0.3287 0.5545 0.7407 11.00000 0.05 0.79 Q7 1 0.2189 0.6611 0.6179 11.00000 0.05 0.78 Q8 1 0.0913 0.8235 0.8203 11.00000 0.05 0.77 Q9 1 0.7559 0.2986 0.7460 11.00000 0.05 0.75 Q10 1 0.1495 0.6833 0.6806 11.00000 0.05 0.74 Q11 1 0.2390 0.7034 0.6011 11.00000 0.05 0.73 Q12 1 0.2982 0.8139 0.7801 11.00000 0.05 0.71 Q13 1 0.1704 0.7739 0.7603 11.00000 0.05 0.71 Q14 1 0.8200 0.5748 0.7672 11.00000 0.05 0.67 Q15 1 0.5562 1.0602 0.7650 11.00000 0.05 0.66 Q16 1 0.3353 0.5565 0.8014 11.00000 0.05 0.65 Q17 1 0.1685 0.7781 0.6634 11.00000 0.05 0.65 Q18 1 0.3791 0.9173 0.9306 11.00000 0.05 0.64 Q19 1 0.2208 0.7822 0.6185 11.00000 0.05 0.64 Q20 1 0.2425 0.5912 0.8137 11.00000 0.05 0.64 Q21 1 0.1481 0.7154 0.7796 11.00000 0.05 0.63 Q22 1 0.0241 0.6402 0.5991 11.00000 0.05 0.61 Q23 1 0.7646 0.5035 0.8643 11.00000 0.05 0.61 ; _shelx_res_checksum 9265 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.273 _oxdiff_exptl_absorpt_empirical_full_min 0.769 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2664(2) 0.9036(2) 0.69848(17) 0.0295(7) Uani 1 1 d . . . . . H1A H 0.214941 0.885303 0.674734 0.035 Uiso 1 1 calc R U . . . H1B H 0.234324 0.937703 0.736244 0.035 Uiso 1 1 calc R U . . . C2 C 0.3248(2) 0.9643(2) 0.64815(17) 0.0279(6) Uani 1 1 d . . . . . C3 C 0.2865(3) 1.0235(2) 0.59463(19) 0.0355(7) Uani 1 1 d . . . . . H3 H 0.219122 1.028645 0.589798 0.043 Uiso 1 1 calc R U . . . C4 C 0.3462(3) 1.0749(2) 0.54839(18) 0.0371(8) Uani 1 1 d . . . . . H4 H 0.319270 1.114177 0.511780 0.044 Uiso 1 1 calc R U . . . C5 C 0.4440(3) 1.0697(2) 0.55489(17) 0.0347(8) Uani 1 1 d . . . . . H5 H 0.484147 1.104698 0.522606 0.042 Uiso 1 1 calc R U . . . C6 C 0.4835(3) 1.0132(2) 0.60887(17) 0.0311(7) Uani 1 1 d . . . . . H6 H 0.550584 1.009618 0.614204 0.037 Uiso 1 1 calc R U . . . C7 C 0.4234(2) 0.9618(2) 0.65491(16) 0.0265(6) Uani 1 1 d . . . . . C8 C 0.5838(2) 0.8425(2) 0.71123(17) 0.0294(7) Uani 1 1 d . . . . . C9 C 0.6529(3) 0.8589(3) 0.75242(19) 0.0410(8) Uani 1 1 d . . . . . H9 H 0.633102 0.891535 0.790774 0.049 Uiso 1 1 calc R U . . . C10 C 0.7498(3) 0.8279(3) 0.7378(2) 0.0506(11) Uani 1 1 d . . . . . H10 H 0.795749 0.838516 0.766749 0.061 Uiso 1 1 calc R U . . . C11 C 0.7802(3) 0.7819(3) 0.6820(2) 0.0518(11) Uani 1 1 d . . . . . H11 H 0.847059 0.762290 0.671393 0.062 Uiso 1 1 calc R U . . . C12 C 0.7121(3) 0.7643(3) 0.6410(2) 0.0433(9) Uani 1 1 d . . . . . H12 H 0.733208 0.732425 0.602394 0.052 Uiso 1 1 calc R U . . . C13 C 0.6136(2) 0.7923(2) 0.65536(18) 0.0325(7) Uani 1 1 d . . . . . C14 C 0.5431(3) 0.7653(2) 0.61221(19) 0.0356(7) Uani 1 1 d . . . . . H14A H 0.504071 0.721888 0.640207 0.053 Uiso 1 1 calc R U . . . H14B H 0.578893 0.737880 0.572821 0.053 Uiso 1 1 calc R U . . . H14C H 0.500520 0.818627 0.595452 0.053 Uiso 1 1 calc R U . . . C15 C 0.4537(3) 0.9615(3) 0.79591(19) 0.0419(8) Uani 1 1 d G . . . . C16A C 0.4946(10) 1.0395(6) 0.7696(5) 0.063(2) Uani 0.276(10) 1 d G . P A 2 H16A H 0.515426 1.050231 0.721792 0.075 Uiso 0.276(10) 1 calc R U P A 2 C17A C 0.5049(16) 1.1019(7) 0.8133(8) 0.078(3) Uani 0.276(10) 1 d G . P A 2 H17A H 0.532823 1.155304 0.795377 0.093 Uiso 0.276(10) 1 calc R U P A 2 C18A C 0.4744(16) 1.0863(10) 0.8833(8) 0.068(2) Uani 0.276(10) 1 d G . P A 2 H18A H 0.481457 1.128945 0.913204 0.081 Uiso 0.276(10) 1 calc R U P A 2 C19A C 0.4335(15) 1.0082(12) 0.9096(4) 0.0536(14) Uani 0.276(10) 1 d G . P A 2 H19A H 0.412691 0.997514 0.957447 0.064 Uiso 0.276(10) 1 calc R U P A 2 C20A C 0.4232(10) 0.9458(8) 0.8659(2) 0.0387(7) Uani 0.276(10) 1 d DG . P A 2 C16 C 0.4473(7) 1.0568(4) 0.7754(4) 0.063(2) Uani 0.724(10) 1 d . . P A 1 H16 H 0.447643 1.079337 0.727954 0.075 Uiso 0.724(10) 1 calc R U P A 1 C17 C 0.4405(9) 1.1159(5) 0.8240(4) 0.078(3) Uani 0.724(10) 1 d . . P A 1 H17 H 0.435876 1.178880 0.810004 0.093 Uiso 0.724(10) 1 calc R U P A 1 C18 C 0.4406(8) 1.0834(6) 0.8928(4) 0.068(2) Uani 0.724(10) 1 d . . P A 1 H18 H 0.440569 1.123901 0.925811 0.081 Uiso 0.724(10) 1 calc R U P A 1 C19 C 0.4406(7) 0.9932(6) 0.9141(3) 0.0536(14) Uani 0.724(10) 1 d . . P A 1 H19 H 0.435545 0.972320 0.962025 0.064 Uiso 0.724(10) 1 calc R U P A 1 C20 C 0.4480(4) 0.9313(4) 0.8659(3) 0.0387(7) Uani 0.724(10) 1 d . . P A 1 C21 C 0.4459(8) 0.8342(6) 0.8932(3) 0.070(3) Uani 0.724(10) 1 d . . P A 1 H21A H 0.382880 0.816089 0.887614 0.106 Uiso 0.724(10) 1 calc R U P A 1 H21B H 0.456043 0.825428 0.942209 0.106 Uiso 0.724(10) 1 calc R U P A 1 H21C H 0.497440 0.797601 0.867615 0.106 Uiso 0.724(10) 1 calc R U P A 1 C21A C 0.393(2) 0.8573(14) 0.8835(11) 0.070(3) Uani 0.276(10) 1 d D . P A 2 H21D H 0.448170 0.811951 0.873450 0.106 Uiso 0.276(10) 1 calc R U P A 2 H21E H 0.340624 0.851254 0.856194 0.106 Uiso 0.276(10) 1 calc R U P A 2 H21F H 0.370154 0.848520 0.932677 0.106 Uiso 0.276(10) 1 calc R U P A 2 C22 C 0.1688(2) 0.5313(2) 0.76726(19) 0.0338(7) Uani 1 1 d . . . . . H22A H 0.115370 0.580481 0.773283 0.041 Uiso 1 1 calc R U . . . H22B H 0.169723 0.514202 0.720286 0.041 Uiso 1 1 calc R U . . . C23 C 0.1482(3) 0.4518(2) 0.81900(19) 0.0337(7) Uani 1 1 d . . . . . C24 C 0.0558(3) 0.4341(3) 0.8471(2) 0.0445(9) Uani 1 1 d . . . . . H24 H 0.000926 0.474242 0.834093 0.053 Uiso 1 1 calc R U . . . C25 C 0.0428(3) 0.3582(3) 0.8940(2) 0.0492(10) Uani 1 1 d . . . . . H25 H -0.020631 0.346953 0.913168 0.059 Uiso 1 1 calc R U . . . C26 C 0.1223(3) 0.2987(3) 0.9129(2) 0.0448(9) Uani 1 1 d . . . . . H26 H 0.112863 0.246347 0.944343 0.054 Uiso 1 1 calc R U . . . C27 C 0.2145(3) 0.3151(2) 0.88662(19) 0.0373(8) Uani 1 1 d . . . . . H27 H 0.268814 0.274397 0.899766 0.045 Uiso 1 1 calc R U . . . C28 C 0.2276(3) 0.3919(2) 0.84044(18) 0.0319(7) Uani 1 1 d . . . . . C29 C 0.4181(3) 0.3978(2) 0.87773(19) 0.0347(7) Uani 1 1 d . . . . . C30 C 0.4973(3) 0.3328(2) 0.8701(2) 0.0418(8) Uani 1 1 d . . . . . H30 H 0.512751 0.307693 0.827776 0.050 Uiso 1 1 calc R U . . . C31 C 0.5543(3) 0.3041(3) 0.9239(2) 0.0530(10) Uani 1 1 d . . . . . H31 H 0.608680 0.259848 0.918393 0.064 Uiso 1 1 calc R U . . . C32 C 0.5316(3) 0.3402(3) 0.9853(2) 0.0533(10) Uani 1 1 d . . . . . H32 H 0.571056 0.321186 1.021960 0.064 Uiso 1 1 calc R U . . . C33 C 0.4519(3) 0.4039(3) 0.9941(2) 0.0456(9) Uani 1 1 d . . . . . H33 H 0.436327 0.427690 1.036948 0.055 Uiso 1 1 calc R U . . . C34 C 0.3941(3) 0.4336(2) 0.94045(19) 0.0388(8) Uani 1 1 d . . . . . C35 C 0.3098(4) 0.5039(3) 0.9532(2) 0.0510(10) Uani 1 1 d . . . . . H35A H 0.314813 0.555771 0.917803 0.077 Uiso 1 1 calc R U . . . H35B H 0.310349 0.523019 0.998832 0.077 Uiso 1 1 calc R U . . . H35C H 0.249200 0.478902 0.951261 0.077 Uiso 1 1 calc R U . . . C36 C 0.3928(3) 0.3691(2) 0.73650(18) 0.0334(7) Uani 1 1 d . . . . . C37 C 0.3405(3) 0.3052(3) 0.7176(2) 0.0444(9) Uani 1 1 d . . . . . H37 H 0.280799 0.293323 0.743437 0.053 Uiso 1 1 calc R U . . . C38 C 0.3748(4) 0.2593(3) 0.6619(2) 0.0553(11) Uani 1 1 d . . . . . H38 H 0.338896 0.215570 0.649955 0.066 Uiso 1 1 calc R U . . . C39 C 0.4609(4) 0.2764(3) 0.6233(2) 0.0540(11) Uani 1 1 d . . . . . H39 H 0.484290 0.244924 0.584828 0.065 Uiso 1 1 calc R U . . . C40 C 0.5125(3) 0.3399(3) 0.6414(2) 0.0485(10) Uani 1 1 d . . . . . H40 H 0.571994 0.351112 0.615031 0.058 Uiso 1 1 calc R U . . . C41 C 0.4798(3) 0.3881(2) 0.6973(2) 0.0398(8) Uani 1 1 d . . . . . C42 C 0.5389(3) 0.4578(3) 0.7127(2) 0.0493(10) Uani 1 1 d . . . . . H42A H 0.607188 0.441793 0.696288 0.074 Uiso 1 1 calc R U . . . H42B H 0.532692 0.460353 0.762604 0.074 Uiso 1 1 calc R U . . . H42C H 0.515400 0.516672 0.689291 0.074 Uiso 1 1 calc R U . . . C43 C 0.3212(2) 0.6611(2) 0.60143(17) 0.0319(7) Uani 1 1 d . . . . . H43A H 0.361741 0.709127 0.581826 0.038 Uiso 1 1 calc R U . . . H43B H 0.354545 0.623531 0.638814 0.038 Uiso 1 1 calc R U . . . C44 C 0.3124(2) 0.6040(2) 0.54622(17) 0.0302(7) Uani 1 1 d . . . . . C45 C 0.3732(3) 0.5251(2) 0.5356(2) 0.0394(8) Uani 1 1 d . . . . . H45 H 0.423169 0.504620 0.564653 0.047 Uiso 1 1 calc R U . . . C46 C 0.3615(3) 0.4763(3) 0.4829(2) 0.0478(10) Uani 1 1 d . . . . . H46 H 0.402381 0.421851 0.476830 0.057 Uiso 1 1 calc R U . . . C47 C 0.2904(3) 0.5064(3) 0.4392(2) 0.0422(9) Uani 1 1 d . . . . . H47 H 0.284018 0.473707 0.402258 0.051 Uiso 1 1 calc R U . . . C48 C 0.2286(3) 0.5840(2) 0.44914(18) 0.0355(7) Uani 1 1 d . . . . . H48 H 0.179621 0.604602 0.419263 0.043 Uiso 1 1 calc R U . . . C49 C 0.2386(2) 0.6316(2) 0.50295(17) 0.0293(7) Uani 1 1 d . . . . . C50 C 0.0390(2) 0.7114(2) 0.51118(17) 0.0302(7) Uani 1 1 d . . . . . C51 C -0.0071(3) 0.7729(2) 0.46219(18) 0.0355(7) Uani 1 1 d . . . . . H51 H 0.023527 0.823606 0.441017 0.043 Uiso 1 1 calc R U . . . C52 C -0.0972(3) 0.7609(3) 0.4442(2) 0.0425(9) Uani 1 1 d . . . . . H52 H -0.128687 0.803542 0.411560 0.051 Uiso 1 1 calc R U . . . C53 C -0.1403(3) 0.6862(3) 0.4741(2) 0.0469(9) Uani 1 1 d . . . . . H53 H -0.201174 0.676547 0.461353 0.056 Uiso 1 1 calc R U . . . C54 C -0.0950(3) 0.6253(3) 0.5229(2) 0.0447(9) Uani 1 1 d . . . . . H54 H -0.125611 0.574232 0.543117 0.054 Uiso 1 1 calc R U . . . C55 C -0.0059(3) 0.6368(2) 0.54287(18) 0.0348(7) Uani 1 1 d . . . . . C56 C 0.0376(3) 0.5692(3) 0.5970(2) 0.0424(8) Uani 1 1 d . . . . . H56A H 0.100602 0.541236 0.577951 0.064 Uiso 1 1 calc R U . . . H56B H -0.005717 0.522823 0.611984 0.064 Uiso 1 1 calc R U . . . H56C H 0.046392 0.599308 0.636628 0.064 Uiso 1 1 calc R U . . . C57 C 0.1921(2) 0.8256(2) 0.47657(17) 0.0301(7) Uani 1 1 d . . . . . C58 C 0.2601(3) 0.8157(3) 0.4196(2) 0.0406(8) Uani 1 1 d . . . . . H58 H 0.287151 0.757019 0.410086 0.049 Uiso 1 1 calc R U . . . C59 C 0.2889(3) 0.8894(3) 0.3768(2) 0.0514(10) Uani 1 1 d . . . . . H59 H 0.335544 0.881263 0.338128 0.062 Uiso 1 1 calc R U . . . C60 C 0.2501(3) 0.9747(3) 0.3900(2) 0.0455(9) Uani 1 1 d . . . . . H60 H 0.269994 1.025698 0.360751 0.055 Uiso 1 1 calc R U . . . C61 C 0.1821(3) 0.9859(3) 0.4461(2) 0.0387(7) Uani 1 1 d . . . . . H61 H 0.154874 1.045025 0.454363 0.046 Uiso 1 1 calc R U . . . C62 C 0.1521(2) 0.9130(2) 0.49112(18) 0.0314(7) Uani 1 1 d . . . . . C63 C 0.0796(3) 0.9287(2) 0.55228(18) 0.0353(7) Uani 1 1 d . . . . . H63A H 0.110591 0.909195 0.594809 0.053 Uiso 1 1 calc R U . . . H63B H 0.025136 0.894320 0.551740 0.053 Uiso 1 1 calc R U . . . H63C H 0.055818 0.992918 0.550232 0.053 Uiso 1 1 calc R U . . . C64 C 0.1908(3) 0.7240(3) 0.88679(18) 0.0373(8) Uani 1 1 d . . . . . H64A H 0.187057 0.658600 0.898201 0.045 Uiso 1 1 calc R U . . . H64B H 0.260139 0.731860 0.874762 0.045 Uiso 1 1 calc R U . . . C65 C 0.1561(2) 0.7678(2) 0.95115(18) 0.0327(7) Uani 1 1 d . . . . . C66 C 0.2023(3) 0.7465(3) 1.01099(18) 0.0388(8) Uani 1 1 d . . . . . H66 H 0.259630 0.704937 1.011262 0.047 Uiso 1 1 calc R U . . . C67 C 0.1656(3) 0.7852(3) 1.07050(19) 0.0432(9) Uani 1 1 d . . . . . H67 H 0.198270 0.770577 1.110939 0.052 Uiso 1 1 calc R U . . . C68 C 0.0808(3) 0.8455(2) 1.07086(18) 0.0377(8) Uani 1 1 d . . . . . H68 H 0.055139 0.871048 1.111782 0.045 Uiso 1 1 calc R U . . . C69 C 0.0343(3) 0.8680(2) 1.01204(17) 0.0328(7) Uani 1 1 d . . . . . H69 H -0.023307 0.909063 1.012023 0.039 Uiso 1 1 calc R U . . . C70 C 0.0728(2) 0.8297(2) 0.95234(16) 0.0289(7) Uani 1 1 d . . . . . C71 C 0.0519(3) 0.9688(2) 0.83635(18) 0.0335(7) Uani 1 1 d . . . . . C72 C 0.1258(3) 1.0015(2) 0.8658(2) 0.0398(8) Uani 1 1 d . . . . . H72 H 0.151308 0.968011 0.905418 0.048 Uiso 1 1 calc R U . . . C73 C 0.1615(3) 1.0806(3) 0.8383(2) 0.0513(10) Uani 1 1 d . . . . . H73 H 0.211313 1.101382 0.858662 0.062 Uiso 1 1 calc R U . . . C74 C 0.1246(4) 1.1290(3) 0.7815(2) 0.0553(11) Uani 1 1 d . . . . . H74 H 0.148755 1.183863 0.762680 0.066 Uiso 1 1 calc R U . . . C75 C 0.0523(3) 1.0992(3) 0.7509(2) 0.0492(10) Uani 1 1 d . . . . . H75 H 0.027615 1.133825 0.711455 0.059 Uiso 1 1 calc R U . . . C76 C 0.0151(3) 1.0176(2) 0.77792(19) 0.0392(8) Uani 1 1 d . . . . . C77 C -0.0614(3) 0.9888(3) 0.7417(2) 0.0464(9) Uani 1 1 d . . . . . H77A H -0.125561 1.010175 0.763436 0.070 Uiso 1 1 calc R U . . . H77B H -0.053989 0.923010 0.744833 0.070 Uiso 1 1 calc R U . . . H77C H -0.054891 1.014305 0.693110 0.070 Uiso 1 1 calc R U . . . C78 C -0.1043(2) 0.8531(2) 0.89140(17) 0.0339(7) Uani 1 1 d . . . . . C79 C -0.1633(3) 0.9330(3) 0.9017(2) 0.0486(10) Uani 1 1 d . . . . . H79 H -0.135725 0.988116 0.894031 0.058 Uiso 1 1 calc R U . . . C80 C -0.2609(3) 0.9337(4) 0.9227(3) 0.0639(13) Uani 1 1 d . . . . . H80 H -0.300600 0.988841 0.928645 0.077 Uiso 1 1 calc R U . . . C81 C -0.3001(3) 0.8543(4) 0.9350(2) 0.0601(13) Uani 1 1 d . . . . . H81 H -0.367123 0.854293 0.950296 0.072 Uiso 1 1 calc R U . . . C82 C -0.2434(3) 0.7739(3) 0.9255(2) 0.0488(10) Uani 1 1 d . . . . . H82 H -0.272134 0.719399 0.933956 0.059 Uiso 1 1 calc R U . . . C83 C -0.1441(3) 0.7716(3) 0.90359(18) 0.0384(8) Uani 1 1 d . . . . . C84 C -0.0848(3) 0.6826(3) 0.8945(2) 0.0523(10) Uani 1 1 d . . . . . H84A H -0.126267 0.634302 0.906554 0.078 Uiso 1 1 calc R U . . . H84B H -0.032441 0.672906 0.924642 0.078 Uiso 1 1 calc R U . . . H84C H -0.056895 0.682622 0.846337 0.078 Uiso 1 1 calc R U . . . Cl1 Cl 0.44063(6) 0.65136(5) 0.79049(4) 0.03288(17) Uani 1 1 d . . . . . Cl2 Cl 0.03295(6) 0.77556(6) 0.69936(4) 0.03425(17) Uani 1 1 d . . . . . O1 O 0.23777(15) 0.70728(13) 0.73995(10) 0.0240(4) Uani 1 1 d . . . . . P1 P 0.45613(6) 0.88515(5) 0.72958(4) 0.02570(16) Uani 1 1 d . . . . . P2 P 0.34117(6) 0.43400(5) 0.80723(4) 0.02843(17) Uani 1 1 d . . . . . P3 P 0.15857(6) 0.72657(5) 0.53327(4) 0.02549(16) Uani 1 1 d . . . . . P4 P 0.02628(6) 0.85331(5) 0.86878(4) 0.02636(16) Uani 1 1 d . . . . . Pd1 Pd 0.34663(2) 0.79018(2) 0.74041(2) 0.02286(6) Uani 1 1 d . . . . . Pd2 Pd 0.29689(2) 0.57832(2) 0.77483(2) 0.02409(6) Uani 1 1 d . . . . . Pd3 Pd 0.19029(2) 0.71856(2) 0.64213(2) 0.02336(6) Uani 1 1 d . . . . . Pd4 Pd 0.12155(2) 0.76645(2) 0.80118(2) 0.02344(6) Uani 1 1 d . . . . . C86 C 0.9019(8) 0.3153(5) 0.7628(4) 0.065(2) Uani 0.591(5) 1 d . . P B 1 H86A H 0.936703 0.274222 0.797749 0.078 Uiso 0.591(5) 1 calc R U P B 1 H86B H 0.870971 0.368909 0.784430 0.078 Uiso 0.591(5) 1 calc R U P B 1 Cl5 Cl 0.9850(3) 0.34829(14) 0.69282(11) 0.0867(11) Uani 0.591(5) 1 d . . P B 1 Cl6 Cl 0.8143(3) 0.2620(2) 0.7363(2) 0.1037(13) Uani 0.591(5) 1 d . . P B 1 C85 C 0.7151(4) 0.5852(4) 0.7830(3) 0.0552(13) Uani 0.845(4) 1 d . . P . . H85A H 0.724132 0.641346 0.800890 0.066 Uiso 0.845(4) 1 calc R U P . . H85B H 0.656292 0.596961 0.758161 0.066 Uiso 0.845(4) 1 calc R U P . . Cl3 Cl 0.81718(13) 0.55327(10) 0.72506(8) 0.0764(6) Uani 0.845(4) 1 d . . P . . Cl4 Cl 0.69939(17) 0.50185(13) 0.85103(8) 0.0960(8) Uani 0.845(4) 1 d . . P . . C87 C 0.9446(16) 0.3332(14) 0.7137(12) 0.0867(11) Uani 0.295(7) 1 d D . P C 2 H87A H 0.965094 0.299461 0.674230 0.130 Uiso 0.295(7) 1 calc R U P C 2 H87B H 0.980702 0.306113 0.752617 0.130 Uiso 0.295(7) 1 calc R U P C 2 H87C H 0.957606 0.395790 0.701101 0.130 Uiso 0.295(7) 1 calc R U P C 2 C88 C 0.8368(14) 0.3307(11) 0.7343(8) 0.065(2) Uani 0.295(7) 1 d D . P C 2 H88A H 0.817578 0.357492 0.777920 0.078 Uiso 0.295(7) 1 calc R U P C 2 H88B H 0.799546 0.366400 0.698111 0.078 Uiso 0.295(7) 1 calc R U P C 2 C89 C 0.8146(19) 0.2350(17) 0.744(3) 0.1037(13) Uani 0.295(7) 1 d D . P C 2 H89A H 0.833815 0.208990 0.699660 0.124 Uiso 0.295(7) 1 calc R U P C 2 H89B H 0.853551 0.199584 0.778963 0.124 Uiso 0.295(7) 1 calc R U P C 2 C90 C 0.7101(12) 0.2273(11) 0.7649(8) 0.065(5) Uani 0.295(7) 1 d D U P C 2 H90A H 0.673109 0.243706 0.724239 0.079 Uiso 0.295(7) 1 calc R U P C 2 H90B H 0.684957 0.269783 0.798904 0.079 Uiso 0.295(7) 1 calc R U P C 2 C91 C 0.6956(13) 0.1320(11) 0.7967(8) 0.070(5) Uani 0.295(7) 1 d D U P . . H91A H 0.704683 0.092320 0.760273 0.105 Uiso 0.295(7) 1 calc R U P C 2 H91B H 0.629892 0.131321 0.820270 0.105 Uiso 0.295(7) 1 calc R U P C 2 H91C H 0.742987 0.110830 0.829968 0.105 Uiso 0.295(7) 1 calc R U P C 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 C1 0.0249(16) 0.0272(15) 0.0359(17) 0.0010(13) -0.0049(13) -0.0042(12) C2 0.0313(17) 0.0223(14) 0.0305(16) -0.0058(12) -0.0026(13) -0.0024(12) C3 0.0385(19) 0.0297(16) 0.0399(19) -0.0017(14) -0.0107(15) -0.0068(14) C4 0.052(2) 0.0278(16) 0.0320(17) 0.0017(13) -0.0117(16) -0.0052(15) C5 0.049(2) 0.0270(16) 0.0275(16) -0.0004(13) 0.0019(15) -0.0108(15) C6 0.0350(18) 0.0288(15) 0.0304(17) -0.0054(13) 0.0003(14) -0.0086(13) C7 0.0307(16) 0.0247(14) 0.0245(15) -0.0045(12) -0.0011(12) -0.0047(12) C8 0.0261(16) 0.0314(16) 0.0295(16) 0.0067(13) -0.0041(13) -0.0083(13) C9 0.038(2) 0.052(2) 0.0351(19) 0.0062(16) -0.0097(15) -0.0183(17) C10 0.032(2) 0.064(3) 0.057(3) 0.022(2) -0.0222(18) -0.0223(18) C11 0.0236(18) 0.056(2) 0.070(3) 0.014(2) -0.0051(18) -0.0034(17) C12 0.0301(18) 0.0389(19) 0.057(2) 0.0029(17) 0.0022(17) -0.0026(15) C13 0.0275(17) 0.0299(16) 0.0383(18) 0.0038(14) -0.0015(14) -0.0059(13) C14 0.0323(18) 0.0382(18) 0.0364(18) -0.0079(14) -0.0007(14) -0.0038(14) C15 0.042(2) 0.050(2) 0.0364(19) -0.0123(16) -0.0072(16) -0.0079(17) C16A 0.113(7) 0.031(3) 0.046(3) -0.011(2) -0.023(4) 0.007(3) C17A 0.142(9) 0.040(3) 0.054(4) -0.016(3) -0.027(5) 0.003(4) C18A 0.095(8) 0.064(3) 0.049(3) -0.015(3) -0.017(4) -0.012(4) C19A 0.056(3) 0.062(4) 0.047(2) -0.016(2) -0.017(2) -0.004(3) C20A 0.0319(16) 0.0398(15) 0.0449(15) 0.0010(12) -0.0101(12) -0.0062(12) C16 0.113(7) 0.031(3) 0.046(3) -0.011(2) -0.023(4) 0.007(3) C17 0.142(9) 0.040(3) 0.054(4) -0.016(3) -0.027(5) 0.003(4) C18 0.095(8) 0.064(3) 0.049(3) -0.015(3) -0.017(4) -0.012(4) C19 0.056(3) 0.062(4) 0.047(2) -0.016(2) -0.017(2) -0.004(3) C20 0.0319(16) 0.0398(15) 0.0449(15) 0.0010(12) -0.0101(12) -0.0062(12) C21 0.117(8) 0.076(5) 0.031(3) 0.012(3) -0.032(4) -0.054(5) C21A 0.117(8) 0.076(5) 0.031(3) 0.012(3) -0.032(4) -0.054(5) C22 0.0314(17) 0.0287(16) 0.0423(19) -0.0011(14) -0.0065(14) -0.0079(13) C23 0.0325(18) 0.0307(16) 0.0402(19) -0.0045(14) -0.0057(14) -0.0101(14) C24 0.037(2) 0.042(2) 0.056(2) -0.0052(17) -0.0029(17) -0.0122(16) C25 0.043(2) 0.053(2) 0.053(2) -0.0017(19) 0.0029(18) -0.0232(19) C26 0.052(2) 0.044(2) 0.041(2) 0.0025(16) -0.0025(17) -0.0233(18) C27 0.044(2) 0.0328(17) 0.0353(18) 0.0003(14) -0.0018(15) -0.0131(15) C28 0.0359(18) 0.0277(16) 0.0332(17) -0.0033(13) 0.0004(14) -0.0110(13) C29 0.0341(18) 0.0269(16) 0.0430(19) 0.0039(14) -0.0049(15) -0.0101(14) C30 0.039(2) 0.0371(18) 0.050(2) -0.0076(16) -0.0061(17) -0.0032(16) C31 0.045(2) 0.051(2) 0.062(3) -0.006(2) -0.016(2) 0.0080(19) C32 0.050(2) 0.057(2) 0.054(3) -0.002(2) -0.020(2) -0.002(2) C33 0.053(2) 0.044(2) 0.042(2) -0.0040(16) -0.0108(18) -0.0077(18) C34 0.046(2) 0.0336(17) 0.0382(19) -0.0016(14) -0.0057(16) -0.0093(15) C35 0.067(3) 0.048(2) 0.036(2) -0.0094(17) -0.0078(19) 0.008(2) C36 0.0405(19) 0.0225(15) 0.0358(18) -0.0038(13) -0.0023(15) 0.0002(13) C37 0.050(2) 0.0380(19) 0.047(2) -0.0103(16) -0.0003(18) -0.0100(17) C38 0.075(3) 0.039(2) 0.056(3) -0.0188(19) -0.004(2) -0.010(2) C39 0.070(3) 0.040(2) 0.051(2) -0.0171(18) 0.009(2) -0.006(2) C40 0.051(2) 0.0341(19) 0.056(2) -0.0111(17) 0.0125(19) 0.0001(17) C41 0.043(2) 0.0266(16) 0.048(2) -0.0046(15) 0.0022(16) -0.0005(15) C42 0.045(2) 0.041(2) 0.061(3) -0.0142(18) 0.0123(19) -0.0092(17) C43 0.0254(16) 0.0393(17) 0.0311(17) -0.0091(14) -0.0016(13) -0.0003(13) C44 0.0261(16) 0.0339(16) 0.0299(16) -0.0045(13) 0.0056(13) -0.0080(13) C45 0.0308(18) 0.0418(19) 0.044(2) -0.0095(16) 0.0039(15) 0.0007(15) C46 0.042(2) 0.0379(19) 0.062(3) -0.0175(18) 0.0158(19) -0.0036(16) C47 0.039(2) 0.046(2) 0.046(2) -0.0240(17) 0.0134(17) -0.0195(16) C48 0.0335(18) 0.0428(19) 0.0332(18) -0.0115(15) 0.0049(14) -0.0158(15) C49 0.0282(16) 0.0303(16) 0.0292(16) -0.0047(13) 0.0047(13) -0.0089(13) C50 0.0247(16) 0.0388(17) 0.0291(16) -0.0099(13) -0.0005(13) -0.0075(13) C51 0.0289(17) 0.0424(19) 0.0366(18) -0.0059(15) -0.0039(14) -0.0082(14) C52 0.0281(18) 0.061(2) 0.041(2) -0.0123(17) -0.0085(15) -0.0029(17) C53 0.0267(18) 0.069(3) 0.051(2) -0.020(2) -0.0049(16) -0.0143(18) C54 0.037(2) 0.051(2) 0.050(2) -0.0137(18) 0.0026(17) -0.0197(17) C55 0.0306(17) 0.0416(18) 0.0342(18) -0.0094(14) 0.0020(14) -0.0115(14) C56 0.041(2) 0.0403(19) 0.047(2) -0.0005(16) -0.0007(17) -0.0186(16) C57 0.0243(16) 0.0340(16) 0.0330(17) 0.0006(13) -0.0072(13) -0.0086(13) C58 0.038(2) 0.0388(19) 0.044(2) -0.0020(16) 0.0023(16) -0.0098(15) C59 0.045(2) 0.054(2) 0.051(2) 0.0026(19) 0.0129(19) -0.0162(19) C60 0.039(2) 0.041(2) 0.054(2) 0.0138(17) -0.0080(17) -0.0135(16) C61 0.0319(16) 0.0398(15) 0.0449(15) 0.0010(12) -0.0101(12) -0.0062(12) C62 0.0253(16) 0.0337(17) 0.0360(17) 0.0029(13) -0.0138(13) -0.0036(13) C63 0.0369(18) 0.0303(16) 0.0389(18) -0.0023(14) -0.0103(15) -0.0011(14) C64 0.0307(18) 0.051(2) 0.0287(17) -0.0094(15) -0.0033(14) 0.0047(15) C65 0.0274(17) 0.0407(18) 0.0314(17) -0.0090(14) -0.0006(13) -0.0064(14) C66 0.0320(18) 0.053(2) 0.0320(18) -0.0071(16) -0.0039(14) -0.0044(16) C67 0.044(2) 0.057(2) 0.0303(18) -0.0092(16) -0.0048(15) -0.0065(18) C68 0.046(2) 0.0422(19) 0.0267(17) -0.0104(14) 0.0018(15) -0.0098(16) C69 0.0347(18) 0.0324(16) 0.0313(17) -0.0069(13) 0.0038(14) -0.0072(14) C70 0.0290(16) 0.0317(16) 0.0271(16) -0.0044(13) 0.0014(13) -0.0104(13) C71 0.0385(19) 0.0267(15) 0.0325(17) -0.0085(13) 0.0098(14) -0.0013(14) C72 0.042(2) 0.0358(18) 0.042(2) -0.0112(15) 0.0093(16) -0.0115(15) C73 0.054(3) 0.048(2) 0.056(3) -0.0147(19) 0.003(2) -0.0215(19) C74 0.066(3) 0.043(2) 0.056(3) -0.0063(19) 0.013(2) -0.018(2) C75 0.063(3) 0.040(2) 0.041(2) -0.0041(17) 0.0098(19) -0.0092(19) C76 0.048(2) 0.0325(17) 0.0340(18) -0.0079(14) 0.0055(16) -0.0002(15) C77 0.051(2) 0.039(2) 0.048(2) -0.0032(17) -0.0077(18) 0.0003(17) C78 0.0267(17) 0.0459(19) 0.0290(16) -0.0059(14) -0.0019(13) -0.0031(14) C79 0.037(2) 0.055(2) 0.051(2) -0.0126(19) 0.0091(17) 0.0002(18) C80 0.040(2) 0.079(3) 0.066(3) -0.016(2) 0.013(2) 0.008(2) C81 0.030(2) 0.105(4) 0.043(2) -0.010(2) 0.0050(17) -0.006(2) C82 0.039(2) 0.076(3) 0.035(2) -0.0047(19) 0.0002(16) -0.025(2) C83 0.0327(18) 0.056(2) 0.0282(17) -0.0016(15) -0.0012(14) -0.0146(16) C84 0.053(3) 0.047(2) 0.059(3) -0.0037(19) 0.007(2) -0.0257(19) Cl1 0.0273(4) 0.0261(3) 0.0448(4) -0.0005(3) -0.0057(3) -0.0039(3) Cl2 0.0254(4) 0.0467(4) 0.0307(4) -0.0107(3) -0.0034(3) 0.0022(3) O1 0.0251(10) 0.0221(10) 0.0245(10) -0.0021(8) 0.0002(8) -0.0047(8) P1 0.0264(4) 0.0283(4) 0.0237(4) -0.0021(3) -0.0031(3) -0.0087(3) P2 0.0298(4) 0.0221(4) 0.0331(4) -0.0019(3) -0.0009(3) -0.0051(3) P3 0.0239(4) 0.0278(4) 0.0257(4) -0.0036(3) -0.0022(3) -0.0061(3) P4 0.0247(4) 0.0281(4) 0.0263(4) -0.0066(3) 0.0019(3) -0.0040(3) Pd1 0.02174(11) 0.02294(11) 0.02392(11) -0.00081(8) -0.00222(8) -0.00491(8) Pd2 0.02467(12) 0.02084(11) 0.02669(12) -0.00234(8) -0.00046(9) -0.00484(8) Pd3 0.02159(11) 0.02423(11) 0.02454(12) -0.00433(8) -0.00137(8) -0.00326(8) Pd4 0.02193(11) 0.02477(11) 0.02387(12) -0.00522(8) 0.00061(8) -0.00402(8) C86 0.112(7) 0.040(3) 0.039(4) 0.001(3) -0.005(4) -0.002(4) Cl5 0.156(3) 0.0458(11) 0.0421(13) 0.0054(9) 0.0214(13) 0.0088(13) Cl6 0.168(3) 0.097(3) 0.0604(18) 0.0003(19) -0.0513(16) -0.043(2) C85 0.054(3) 0.058(3) 0.053(3) -0.007(2) 0.001(2) -0.010(2) Cl3 0.0787(11) 0.0652(9) 0.0677(10) 0.0107(7) 0.0173(8) 0.0140(7) Cl4 0.1254(17) 0.0946(12) 0.0485(9) 0.0156(8) 0.0194(9) 0.0079(11) C87 0.156(3) 0.0458(11) 0.0421(13) 0.0054(9) 0.0214(13) 0.0088(13) C88 0.112(7) 0.040(3) 0.039(4) 0.001(3) -0.005(4) -0.002(4) C89 0.168(3) 0.097(3) 0.0604(18) 0.0003(19) -0.0513(16) -0.043(2) C90 0.059(8) 0.090(9) 0.049(7) -0.031(6) -0.014(6) 0.015(7) C91 0.061(9) 0.102(12) 0.050(8) -0.025(8) -0.018(7) 0.003(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 -1 0.0712 -1 -1 1 0.0462 1 0 -1 0.0467 1 -1 -1 0.0238 -1 1 1 0.0153 1 1 2 0.0041 -1 -1 -2 0.0075 1 0 1 0.0323 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 H1A C1 H1B 107.7 . . ? C2 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? C2 C1 Pd1 113.9(2) . . ? Pd1 C1 H1A 108.8 . . ? Pd1 C1 H1B 108.8 . . ? C3 C2 C1 123.9(3) . . ? C3 C2 C7 117.7(3) . . ? C7 C2 C1 118.4(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 119.5 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.5 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(3) . . ? C6 C5 H5 120.1 . . ? C5 C6 H6 120.5 . . ? C7 C6 C5 119.0(3) . . ? C7 C6 H6 120.5 . . ? C2 C7 P1 110.3(2) . . ? C6 C7 C2 122.1(3) . . ? C6 C7 P1 127.6(3) . . ? C9 C8 C13 119.3(3) . . ? C9 C8 P1 120.6(3) . . ? C13 C8 P1 120.1(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C9 C10 H10 119.7 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.3(4) . . ? C12 C11 H11 120.3 . . ? C11 C12 H12 119.2 . . ? C11 C12 C13 121.5(4) . . ? C13 C12 H12 119.2 . . ? C8 C13 C14 122.6(3) . . ? C12 C13 C8 118.6(3) . . ? C12 C13 C14 118.8(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16A C15 C20A 120.0 . . ? C16A C15 P1 112.1(4) . . ? C20A C15 P1 127.7(4) . . ? C16 C15 P1 119.2(4) . . ? C20 C15 C16 117.9(4) . . ? C20 C15 P1 122.5(4) . . ? C15 C16A H16A 120.0 . . ? C17A C16A C15 120.0 . . ? C17A C16A H16A 120.0 . . ? C16A C17A H17A 120.0 . . ? C16A C17A C18A 120.0 . . ? C18A C17A H17A 120.0 . . ? C17A C18A H18A 120.0 . . ? C19A C18A C17A 120.0 . . ? C19A C18A H18A 120.0 . . ? C18A C19A H19A 120.0 . . ? C20A C19A C18A 120.0 . . ? C20A C19A H19A 120.0 . . ? C15 C20A C21A 111.0(11) . . ? C19A C20A C15 120.0 . . ? C19A C20A C21A 128.7(10) . . ? C15 C16 H16 119.6 . . ? C17 C16 C15 120.7(6) . . ? C17 C16 H16 119.6 . . ? C16 C17 H17 120.1 . . ? C18 C17 C16 119.8(7) . . ? C18 C17 H17 120.1 . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.7(6) . . ? C19 C18 H18 119.7 . . ? C18 C19 H19 119.7 . . ? C18 C19 C20 120.7(6) . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 120.0(5) . . ? C15 C20 C21 122.5(5) . . ? C19 C20 C21 117.5(6) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20A C21A H21D 109.5 . . ? C20A C21A H21E 109.5 . . ? C20A C21A H21F 109.5 . . ? H21D C21A H21E 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? H22A C22 H22B 107.6 . . ? C23 C22 H22A 108.7 . . ? C23 C22 H22B 108.7 . . ? C23 C22 Pd2 114.0(2) . . ? Pd2 C22 H22A 108.7 . . ? Pd2 C22 H22B 108.7 . . ? C24 C23 C22 124.2(3) . . ? C24 C23 C28 118.1(3) . . ? C28 C23 C22 117.7(3) . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.5(4) . . ? C25 C24 H24 119.7 . . ? C24 C25 H25 119.9 . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.4(4) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.4(4) . . ? C28 C27 H27 120.3 . . ? C23 C28 P2 111.3(2) . . ? C27 C28 C23 121.2(3) . . ? C27 C28 P2 127.2(3) . . ? C30 C29 C34 119.9(3) . . ? C30 C29 P2 120.5(3) . . ? C34 C29 P2 119.5(3) . . ? C29 C30 H30 119.8 . . ? C29 C30 C31 120.4(4) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 120.1 . . ? C32 C31 C30 119.7(4) . . ? C32 C31 H31 120.1 . . ? C31 C32 H32 119.8 . . ? C31 C32 C33 120.5(4) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.5(4) . . ? C34 C33 H33 119.8 . . ? C29 C34 C35 123.5(3) . . ? C33 C34 C29 118.9(3) . . ? C33 C34 C35 117.6(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C41 119.5(3) . . ? C37 C36 P2 119.3(3) . . ? C41 C36 P2 120.9(3) . . ? C36 C37 H37 119.7 . . ? C38 C37 C36 120.6(4) . . ? C38 C37 H37 119.7 . . ? C37 C38 H38 119.7 . . ? C37 C38 C39 120.5(4) . . ? C39 C38 H38 119.7 . . ? C38 C39 H39 120.4 . . ? C40 C39 C38 119.1(4) . . ? C40 C39 H39 120.4 . . ? C39 C40 H40 119.0 . . ? C39 C40 C41 122.0(4) . . ? C41 C40 H40 119.0 . . ? C36 C41 C42 122.9(3) . . ? C40 C41 C36 118.2(4) . . ? C40 C41 C42 118.9(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? H43A C43 H43B 107.8 . . ? C44 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C44 C43 Pd3 112.9(2) . . ? Pd3 C43 H43A 109.0 . . ? Pd3 C43 H43B 109.0 . . ? C45 C44 C43 123.8(3) . . ? C45 C44 C49 118.1(3) . . ? C49 C44 C43 118.0(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45 119.7 . . ? C45 C46 H46 119.9 . . ? C47 C46 C45 120.3(3) . . ? C47 C46 H46 119.9 . . ? C46 C47 H47 119.9 . . ? C48 C47 C46 120.1(3) . . ? C48 C47 H47 119.9 . . ? C47 C48 H48 120.2 . . ? C47 C48 C49 119.7(4) . . ? C49 C48 H48 120.2 . . ? C44 C49 P3 110.6(2) . . ? C48 C49 C44 121.1(3) . . ? C48 C49 P3 128.1(3) . . ? C51 C50 C55 119.9(3) . . ? C51 C50 P3 120.4(3) . . ? C55 C50 P3 119.6(3) . . ? C50 C51 H51 119.6 . . ? C52 C51 C50 120.8(3) . . ? C52 C51 H51 119.6 . . ? C51 C52 H52 120.3 . . ? C53 C52 C51 119.3(4) . . ? C53 C52 H52 120.3 . . ? C52 C53 H53 120.0 . . ? C52 C53 C54 120.0(3) . . ? C54 C53 H53 120.0 . . ? C53 C54 H54 119.1 . . ? C53 C54 C55 121.8(4) . . ? C55 C54 H54 119.1 . . ? C50 C55 C56 123.1(3) . . ? C54 C55 C50 118.2(3) . . ? C54 C55 C56 118.8(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C62 119.5(3) . . ? C58 C57 P3 119.8(3) . . ? C62 C57 P3 120.7(3) . . ? C57 C58 H58 119.4 . . ? C59 C58 C57 121.2(4) . . ? C59 C58 H58 119.4 . . ? C58 C59 H59 120.1 . . ? C60 C59 C58 119.9(4) . . ? C60 C59 H59 120.1 . . ? C59 C60 H60 120.2 . . ? C59 C60 C61 119.7(4) . . ? C61 C60 H60 120.2 . . ? C60 C61 H61 119.0 . . ? C60 C61 C62 122.0(3) . . ? C62 C61 H61 119.0 . . ? C57 C62 C63 122.3(3) . . ? C61 C62 C57 117.7(3) . . ? C61 C62 C63 120.0(3) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? H64A C64 H64B 107.1 . . ? C65 C64 H64A 107.7 . . ? C65 C64 H64B 107.7 . . ? C65 C64 Pd4 118.3(2) . . ? Pd4 C64 H64A 107.7 . . ? Pd4 C64 H64B 107.7 . . ? C66 C65 C64 122.3(3) . . ? C66 C65 C70 118.1(3) . . ? C70 C65 C64 119.5(3) . . ? C65 C66 H66 119.6 . . ? C65 C66 C67 120.7(3) . . ? C67 C66 H66 119.6 . . ? C66 C67 H67 120.0 . . ? C66 C67 C68 120.1(3) . . ? C68 C67 H67 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 C67 120.1(3) . . ? C69 C68 H68 120.0 . . ? C68 C69 H69 120.3 . . ? C68 C69 C70 119.3(3) . . ? C70 C69 H69 120.3 . . ? C65 C70 C69 121.7(3) . . ? C65 C70 P4 111.8(2) . . ? C69 C70 P4 126.5(3) . . ? C72 C71 P4 116.6(3) . . ? C76 C71 C72 119.2(3) . . ? C76 C71 P4 123.3(3) . . ? C71 C72 H72 119.3 . . ? C73 C72 C71 121.5(4) . . ? C73 C72 H72 119.3 . . ? C72 C73 H73 120.3 . . ? C74 C73 C72 119.3(4) . . ? C74 C73 H73 120.3 . . ? C73 C74 H74 119.5 . . ? C73 C74 C75 121.0(4) . . ? C75 C74 H74 119.5 . . ? C74 C75 H75 119.7 . . ? C74 C75 C76 120.6(4) . . ? C76 C75 H75 119.7 . . ? C71 C76 C75 118.3(4) . . ? C71 C76 C77 123.9(3) . . ? C75 C76 C77 117.8(4) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77B 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 C83 119.7(3) . . ? C79 C78 P4 120.3(3) . . ? C83 C78 P4 119.8(3) . . ? C78 C79 H79 119.4 . . ? C80 C79 C78 121.2(4) . . ? C80 C79 H79 119.4 . . ? C79 C80 H80 120.4 . . ? C81 C80 C79 119.3(4) . . ? C81 C80 H80 120.4 . . ? C80 C81 H81 119.6 . . ? C80 C81 C82 120.8(4) . . ? C82 C81 H81 119.6 . . ? C81 C82 H82 119.6 . . ? C81 C82 C83 120.9(4) . . ? C83 C82 H82 119.6 . . ? C78 C83 C82 118.1(4) . . ? C78 C83 C84 122.7(3) . . ? C82 C83 C84 119.2(4) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84B 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? Pd1 Cl1 Pd2 84.34(2) . . ? Pd3 Cl2 Pd4 84.67(2) . . ? Pd2 O1 Pd1 105.94(9) . . ? Pd2 O1 Pd3 113.65(9) . . ? Pd2 O1 Pd4 117.41(9) . . ? Pd3 O1 Pd1 110.92(9) . . ? Pd4 O1 Pd1 103.46(9) . . ? Pd4 O1 Pd3 105.02(9) . . ? C7 P1 C8 106.57(15) . . ? C7 P1 C15 102.59(16) . . ? C7 P1 Pd1 102.31(11) . . ? C8 P1 C15 105.20(17) . . ? C8 P1 Pd1 118.68(11) . . ? C15 P1 Pd1 119.53(13) . . ? C28 P2 C29 103.50(16) . . ? C28 P2 C36 106.37(16) . . ? C28 P2 Pd2 103.18(11) . . ? C29 P2 Pd2 121.38(11) . . ? C36 P2 C29 106.34(16) . . ? C36 P2 Pd2 114.50(11) . . ? C49 P3 C50 104.53(15) . . ? C49 P3 C57 105.99(15) . . ? C49 P3 Pd3 102.23(11) . . ? C50 P3 Pd3 121.79(11) . . ? C57 P3 C50 104.72(15) . . ? C57 P3 Pd3 115.95(11) . . ? C70 P4 C71 105.06(16) . . ? C70 P4 C78 102.45(15) . . ? C70 P4 Pd4 105.91(11) . . ? C71 P4 Pd4 105.37(10) . . ? C78 P4 C71 109.18(16) . . ? C78 P4 Pd4 126.98(12) . . ? C1 Pd1 Cl1 178.72(10) . . ? C1 Pd1 O1 94.04(11) . . ? C1 Pd1 P1 80.84(10) . . ? O1 Pd1 Cl1 84.70(6) . . ? O1 Pd1 P1 173.49(6) . . ? P1 Pd1 Cl1 100.41(3) . . ? C22 Pd2 Cl1 172.93(10) . . ? C22 Pd2 O1 90.01(11) . . ? C22 Pd2 P2 81.82(9) . . ? O1 Pd2 Cl1 84.87(6) . . ? O1 Pd2 P2 171.64(6) . . ? P2 Pd2 Cl1 103.42(3) . . ? C43 Pd3 Cl2 174.67(10) . . ? C43 Pd3 O1 91.92(11) . . ? C43 Pd3 P3 81.28(10) . . ? O1 Pd3 Cl2 84.82(6) . . ? O1 Pd3 P3 173.03(6) . . ? P3 Pd3 Cl2 102.08(3) . . ? C64 Pd4 Cl2 164.85(12) . . ? C64 Pd4 O1 90.59(11) . . ? C64 Pd4 P4 84.16(10) . . ? O1 Pd4 Cl2 84.87(6) . . ? O1 Pd4 P4 164.86(6) . . ? P4 Pd4 Cl2 103.64(3) . . ? H86A C86 H86B 108.1 . . ? Cl5 C86 H86A 109.5 . . ? Cl5 C86 H86B 109.5 . . ? Cl6 C86 H86A 109.5 . . ? Cl6 C86 H86B 109.5 . . ? Cl6 C86 Cl5 110.8(5) . . ? H85A C85 H85B 108.0 . . ? Cl3 C85 H85A 109.5 . . ? Cl3 C85 H85B 109.5 . . ? Cl4 C85 H85A 109.5 . . ? Cl4 C85 H85B 109.5 . . ? Cl4 C85 Cl3 110.9(3) . . ? H87A C87 H87B 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? C87 C88 H88A 109.8 . . ? C87 C88 H88B 109.8 . . ? H88A C88 H88B 108.2 . . ? C89 C88 C87 109.6(15) . . ? C89 C88 H88A 109.8 . . ? C89 C88 H88B 109.8 . . ? C88 C89 H89A 109.1 . . ? C88 C89 H89B 109.1 . . ? H89A C89 H89B 107.8 . . ? C90 C89 C88 112(2) . . ? C90 C89 H89A 109.1 . . ? C90 C89 H89B 109.1 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? C89 C90 C91 110.7(15) . . ? H90A C90 H90B 108.1 . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91B 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? 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 C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.501(5) . ? C1 Pd1 2.051(3) . ? C2 C3 1.396(5) . ? C2 C7 1.397(5) . ? C3 H3 0.9500 . ? C3 C4 1.390(5) . ? C4 H4 0.9500 . ? C4 C5 1.380(6) . ? C5 H5 0.9500 . ? C5 C6 1.391(5) . ? C6 H6 0.9500 . ? C6 C7 1.391(5) . ? C7 P1 1.809(3) . ? C8 C9 1.398(5) . ? C8 C13 1.409(5) . ? C8 P1 1.827(3) . ? C9 H9 0.9500 . ? C9 C10 1.383(6) . ? C10 H10 0.9500 . ? C10 C11 1.372(7) . ? C11 H11 0.9500 . ? C11 C12 1.391(6) . ? C12 H12 0.9500 . ? C12 C13 1.394(5) . ? C13 C14 1.502(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16A 1.3900 . ? C15 C20A 1.3900 . ? C15 C16 1.437(8) . ? C15 C20 1.386(7) . ? C15 P1 1.848(4) . ? C16A H16A 0.9500 . ? C16A C17A 1.3900 . ? C17A H17A 0.9500 . ? C17A C18A 1.3900 . ? C18A H18A 0.9500 . ? C18A C19A 1.3900 . ? C19A H19A 0.9500 . ? C19A C20A 1.3900 . ? C20A C21A 1.441(15) . ? C16 H16 0.9500 . ? C16 C17 1.380(9) . ? C17 H17 0.9500 . ? C17 C18 1.375(10) . ? C18 H18 0.9500 . ? C18 C19 1.373(10) . ? C19 H19 0.9500 . ? C19 C20 1.404(8) . ? C20 C21 1.497(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.503(5) . ? C22 Pd2 2.042(3) . ? C23 C24 1.390(5) . ? C23 C28 1.405(5) . ? C24 H24 0.9500 . ? C24 C25 1.391(6) . ? C25 H25 0.9500 . ? C25 C26 1.387(6) . ? C26 H26 0.9500 . ? C26 C27 1.372(6) . ? C27 H27 0.9500 . ? C27 C28 1.393(5) . ? C28 P2 1.808(3) . ? C29 C30 1.388(5) . ? C29 C34 1.400(5) . ? C29 P2 1.837(4) . ? C30 H30 0.9500 . ? C30 C31 1.389(6) . ? C31 H31 0.9500 . ? C31 C32 1.376(7) . ? C32 H32 0.9500 . ? C32 C33 1.384(6) . ? C33 H33 0.9500 . ? C33 C34 1.396(6) . ? C34 C35 1.499(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.398(5) . ? C36 C41 1.403(5) . ? C36 P2 1.831(3) . ? C37 H37 0.9500 . ? C37 C38 1.379(6) . ? C38 H38 0.9500 . ? C38 C39 1.380(7) . ? C39 H39 0.9500 . ? C39 C40 1.379(7) . ? C40 H40 0.9500 . ? C40 C41 1.397(6) . ? C41 C42 1.505(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.500(5) . ? C43 Pd3 2.040(3) . ? C44 C45 1.394(5) . ? C44 C49 1.401(5) . ? C45 H45 0.9500 . ? C45 C46 1.386(6) . ? C46 H46 0.9500 . ? C46 C47 1.383(6) . ? C47 H47 0.9500 . ? C47 C48 1.382(5) . ? C48 H48 0.9500 . ? C48 C49 1.386(5) . ? C49 P3 1.820(3) . ? C50 C51 1.399(5) . ? C50 C55 1.400(5) . ? C50 P3 1.828(3) . ? C51 H51 0.9500 . ? C51 C52 1.390(5) . ? C52 H52 0.9500 . ? C52 C53 1.380(6) . ? C53 H53 0.9500 . ? C53 C54 1.386(6) . ? C54 H54 0.9500 . ? C54 C55 1.389(5) . ? C55 C56 1.499(5) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.391(5) . ? C57 C62 1.415(5) . ? C57 P3 1.822(3) . ? C58 H58 0.9500 . ? C58 C59 1.379(6) . ? C59 H59 0.9500 . ? C59 C60 1.377(6) . ? C60 H60 0.9500 . ? C60 C61 1.381(6) . ? C61 H61 0.9500 . ? C61 C62 1.396(5) . ? C62 C63 1.501(5) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 C65 1.506(5) . ? C64 Pd4 2.029(3) . ? C65 C66 1.390(5) . ? C65 C70 1.394(5) . ? C66 H66 0.9500 . ? C66 C67 1.391(5) . ? C67 H67 0.9500 . ? C67 C68 1.397(6) . ? C68 H68 0.9500 . ? C68 C69 1.375(5) . ? C69 H69 0.9500 . ? C69 C70 1.396(5) . ? C70 P4 1.813(3) . ? C71 C72 1.415(6) . ? C71 C76 1.393(5) . ? C71 P4 1.843(3) . ? C72 H72 0.9500 . ? C72 C73 1.376(6) . ? C73 H73 0.9500 . ? C73 C74 1.367(7) . ? C74 H74 0.9500 . ? C74 C75 1.388(7) . ? C75 H75 0.9500 . ? C75 C76 1.416(6) . ? C76 C77 1.493(6) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.393(5) . ? C78 C83 1.399(5) . ? C78 P4 1.829(4) . ? C79 H79 0.9500 . ? C79 C80 1.379(6) . ? C80 H80 0.9500 . ? C80 C81 1.366(8) . ? C81 H81 0.9500 . ? C81 C82 1.381(7) . ? C82 H82 0.9500 . ? C82 C83 1.402(5) . ? C83 C84 1.504(6) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? Cl1 Pd1 2.4738(7) . ? Cl1 Pd2 2.4876(8) . ? Cl2 Pd3 2.4529(8) . ? Cl2 Pd4 2.4569(8) . ? O1 Pd1 2.099(2) . ? O1 Pd2 2.0736(19) . ? O1 Pd3 2.087(2) . ? O1 Pd4 2.080(2) . ? P1 Pd1 2.2089(8) . ? P2 Pd2 2.2155(8) . ? P3 Pd3 2.2217(8) . ? P4 Pd4 2.2008(8) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C86 Cl5 1.755(9) . ? C86 Cl6 1.718(11) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C85 Cl3 1.774(5) . ? C85 Cl4 1.725(6) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C87 C88 1.518(17) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C88 C89 1.503(18) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C89 C90 1.488(19) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C90 C91 1.522(16) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? 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 C1 C2 C3 C4 -177.3(3) . . . . ? C1 C2 C7 C6 177.4(3) . . . . ? C1 C2 C7 P1 -2.8(4) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C2 C7 P1 C8 151.7(2) . . . . ? C2 C7 P1 C15 -98.0(2) . . . . ? C2 C7 P1 Pd1 26.4(2) . . . . ? C3 C2 C7 C6 -2.6(5) . . . . ? C3 C2 C7 P1 177.2(2) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C7 0.8(5) . . . . ? C5 C6 C7 C2 0.9(5) . . . . ? C5 C6 C7 P1 -178.9(2) . . . . ? C6 C7 P1 C8 -28.5(3) . . . . ? C6 C7 P1 C15 81.8(3) . . . . ? C6 C7 P1 Pd1 -153.7(3) . . . . ? C7 C2 C3 C4 2.7(5) . . . . ? C8 C9 C10 C11 1.2(6) . . . . ? C9 C8 C13 C12 -3.0(5) . . . . ? C9 C8 C13 C14 174.9(3) . . . . ? C9 C8 P1 C7 118.0(3) . . . . ? C9 C8 P1 C15 9.6(3) . . . . ? C9 C8 P1 Pd1 -127.4(3) . . . . ? C9 C10 C11 C12 -1.8(6) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C8 2.4(5) . . . . ? C11 C12 C13 C14 -175.6(3) . . . . ? C13 C8 C9 C10 1.3(5) . . . . ? C13 C8 P1 C7 -62.2(3) . . . . ? C13 C8 P1 C15 -170.7(3) . . . . ? C13 C8 P1 Pd1 52.4(3) . . . . ? C15 C16A C17A C18A 0.0 . . . . ? C15 C16 C17 C18 0.4(14) . . . . ? C16A C15 C20A C19A 0.0 . . . . ? C16A C15 C20A C21A -173.7(14) . . . . ? C16A C15 P1 C7 -41.5(7) . . . . ? C16A C15 P1 C8 69.8(7) . . . . ? C16A C15 P1 Pd1 -153.7(7) . . . . ? C16A C17A C18A C19A 0.0 . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A C15 0.0 . . . . ? C18A C19A C20A C21A 172.5(18) . . . . ? C20A C15 C16A C17A 0.0 . . . . ? C20A C15 P1 C7 143.3(8) . . . . ? C20A C15 P1 C8 -105.4(8) . . . . ? C20A C15 P1 Pd1 31.1(8) . . . . ? C16 C15 C20 C19 -2.8(8) . . . . ? C16 C15 C20 C21 175.0(7) . . . . ? C16 C15 P1 C7 -11.6(6) . . . . ? C16 C15 P1 C8 99.7(5) . . . . ? C16 C15 P1 Pd1 -123.8(5) . . . . ? C16 C17 C18 C19 -4.5(15) . . . . ? C17 C18 C19 C20 4.9(13) . . . . ? C18 C19 C20 C15 -1.1(11) . . . . ? C18 C19 C20 C21 -179.0(8) . . . . ? C20 C15 C16 C17 3.2(11) . . . . ? C20 C15 P1 C7 161.7(4) . . . . ? C20 C15 P1 C8 -87.0(4) . . . . ? C20 C15 P1 Pd1 49.5(4) . . . . ? C22 C23 C24 C25 179.1(4) . . . . ? C22 C23 C28 C27 -178.0(3) . . . . ? C22 C23 C28 P2 7.4(4) . . . . ? C23 C24 C25 C26 -0.5(6) . . . . ? C23 C28 P2 C29 143.7(3) . . . . ? C23 C28 P2 C36 -104.4(3) . . . . ? C23 C28 P2 Pd2 16.4(3) . . . . ? C24 C23 C28 C27 2.3(5) . . . . ? C24 C23 C28 P2 -172.4(3) . . . . ? C24 C25 C26 C27 1.2(6) . . . . ? C25 C26 C27 C28 -0.2(6) . . . . ? C26 C27 C28 C23 -1.6(5) . . . . ? C26 C27 C28 P2 172.2(3) . . . . ? C27 C28 P2 C29 -30.5(4) . . . . ? C27 C28 P2 C36 81.3(3) . . . . ? C27 C28 P2 Pd2 -157.8(3) . . . . ? C28 C23 C24 C25 -1.2(6) . . . . ? C29 C30 C31 C32 0.3(7) . . . . ? C30 C29 C34 C33 1.0(6) . . . . ? C30 C29 C34 C35 -180.0(4) . . . . ? C30 C29 P2 C28 111.8(3) . . . . ? C30 C29 P2 C36 0.0(3) . . . . ? C30 C29 P2 Pd2 -133.3(3) . . . . ? C30 C31 C32 C33 0.8(7) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C32 C33 C34 C29 0.1(6) . . . . ? C32 C33 C34 C35 -179.0(4) . . . . ? C34 C29 C30 C31 -1.2(6) . . . . ? C34 C29 P2 C28 -65.7(3) . . . . ? C34 C29 P2 C36 -177.6(3) . . . . ? C34 C29 P2 Pd2 49.2(3) . . . . ? C36 C37 C38 C39 -0.7(7) . . . . ? C37 C36 C41 C40 -1.8(5) . . . . ? C37 C36 C41 C42 178.1(4) . . . . ? C37 C36 P2 C28 2.7(3) . . . . ? C37 C36 P2 C29 112.6(3) . . . . ? C37 C36 P2 Pd2 -110.6(3) . . . . ? C37 C38 C39 C40 0.3(7) . . . . ? C38 C39 C40 C41 -0.6(7) . . . . ? C39 C40 C41 C36 1.3(6) . . . . ? C39 C40 C41 C42 -178.5(4) . . . . ? C41 C36 C37 C38 1.5(6) . . . . ? C41 C36 P2 C28 177.1(3) . . . . ? C41 C36 P2 C29 -73.0(3) . . . . ? C41 C36 P2 Pd2 63.9(3) . . . . ? C43 C44 C45 C46 -179.2(4) . . . . ? C43 C44 C49 C48 177.4(3) . . . . ? C43 C44 C49 P3 -7.7(4) . . . . ? C44 C45 C46 C47 1.5(6) . . . . ? C44 C49 P3 C50 -146.6(2) . . . . ? C44 C49 P3 C57 103.0(2) . . . . ? C44 C49 P3 Pd3 -18.8(2) . . . . ? C45 C44 C49 C48 -2.7(5) . . . . ? C45 C44 C49 P3 172.2(3) . . . . ? C45 C46 C47 C48 -2.1(6) . . . . ? C46 C47 C48 C49 0.3(5) . . . . ? C47 C48 C49 C44 2.1(5) . . . . ? C47 C48 C49 P3 -171.8(3) . . . . ? C48 C49 P3 C50 27.8(3) . . . . ? C48 C49 P3 C57 -82.5(3) . . . . ? C48 C49 P3 Pd3 155.6(3) . . . . ? C49 C44 C45 C46 0.9(5) . . . . ? C50 C51 C52 C53 -1.3(6) . . . . ? C51 C50 C55 C54 1.7(5) . . . . ? C51 C50 C55 C56 -178.4(3) . . . . ? C51 C50 P3 C49 -114.2(3) . . . . ? C51 C50 P3 C57 -2.9(3) . . . . ? C51 C50 P3 Pd3 131.1(2) . . . . ? C51 C52 C53 C54 1.5(6) . . . . ? C52 C53 C54 C55 -0.1(6) . . . . ? C53 C54 C55 C50 -1.5(6) . . . . ? C53 C54 C55 C56 178.6(4) . . . . ? C55 C50 C51 C52 -0.4(5) . . . . ? C55 C50 P3 C49 64.9(3) . . . . ? C55 C50 P3 C57 176.2(3) . . . . ? C55 C50 P3 Pd3 -49.8(3) . . . . ? C57 C58 C59 C60 -0.1(7) . . . . ? C58 C57 C62 C61 1.1(5) . . . . ? C58 C57 C62 C63 -179.0(3) . . . . ? C58 C57 P3 C49 5.9(3) . . . . ? C58 C57 P3 C50 -104.3(3) . . . . ? C58 C57 P3 Pd3 118.5(3) . . . . ? C58 C59 C60 C61 -0.3(7) . . . . ? C59 C60 C61 C62 1.1(6) . . . . ? C60 C61 C62 C57 -1.5(5) . . . . ? C60 C61 C62 C63 178.6(3) . . . . ? C62 C57 C58 C59 -0.4(6) . . . . ? C62 C57 P3 C49 -172.0(3) . . . . ? C62 C57 P3 C50 77.8(3) . . . . ? C62 C57 P3 Pd3 -59.4(3) . . . . ? C64 C65 C66 C67 -177.0(4) . . . . ? C64 C65 C70 C69 176.0(3) . . . . ? C64 C65 C70 P4 -5.2(4) . . . . ? C65 C66 C67 C68 0.7(6) . . . . ? C65 C70 P4 C71 -108.8(3) . . . . ? C65 C70 P4 C78 137.2(3) . . . . ? C65 C70 P4 Pd4 2.5(3) . . . . ? C66 C65 C70 C69 -1.7(5) . . . . ? C66 C65 C70 P4 177.1(3) . . . . ? C66 C67 C68 C69 -1.2(6) . . . . ? C67 C68 C69 C70 0.1(5) . . . . ? C68 C69 C70 C65 1.3(5) . . . . ? C68 C69 C70 P4 -177.3(3) . . . . ? C69 C70 P4 C71 70.0(3) . . . . ? C69 C70 P4 C78 -44.1(3) . . . . ? C69 C70 P4 Pd4 -178.8(3) . . . . ? C70 C65 C66 C67 0.7(6) . . . . ? C71 C72 C73 C74 0.3(6) . . . . ? C72 C71 C76 C75 -1.0(5) . . . . ? C72 C71 C76 C77 178.8(3) . . . . ? C72 C71 P4 C70 21.1(3) . . . . ? C72 C71 P4 C78 130.4(3) . . . . ? C72 C71 P4 Pd4 -90.5(3) . . . . ? C72 C73 C74 C75 -0.5(7) . . . . ? C73 C74 C75 C76 0.0(6) . . . . ? C74 C75 C76 C71 0.8(6) . . . . ? C74 C75 C76 C77 -179.0(4) . . . . ? C76 C71 C72 C73 0.5(5) . . . . ? C76 C71 P4 C70 -170.3(3) . . . . ? C76 C71 P4 C78 -61.0(3) . . . . ? C76 C71 P4 Pd4 78.1(3) . . . . ? C78 C79 C80 C81 1.3(7) . . . . ? C79 C78 C83 C82 0.5(5) . . . . ? C79 C78 C83 C84 -179.2(4) . . . . ? C79 C78 P4 C70 92.9(3) . . . . ? C79 C78 P4 C71 -18.1(3) . . . . ? C79 C78 P4 Pd4 -145.9(3) . . . . ? C79 C80 C81 C82 -1.1(7) . . . . ? C80 C81 C82 C83 0.6(7) . . . . ? C81 C82 C83 C78 -0.2(6) . . . . ? C81 C82 C83 C84 179.4(4) . . . . ? C83 C78 C79 C80 -1.0(6) . . . . ? C83 C78 P4 C70 -82.2(3) . . . . ? C83 C78 P4 C71 166.8(3) . . . . ? C83 C78 P4 Pd4 39.0(3) . . . . ? P1 C8 C9 C10 -178.9(3) . . . . ? P1 C8 C13 C12 177.2(3) . . . . ? P1 C8 C13 C14 -4.9(4) . . . . ? P1 C15 C16A C17A -175.6(6) . . . . ? P1 C15 C20A C19A 174.9(7) . . . . ? P1 C15 C20A C21A 1.2(16) . . . . ? P1 C15 C16 C17 176.8(7) . . . . ? P1 C15 C20 C19 -176.2(5) . . . . ? P1 C15 C20 C21 1.6(8) . . . . ? P2 C29 C30 C31 -178.7(3) . . . . ? P2 C29 C34 C33 178.5(3) . . . . ? P2 C29 C34 C35 -2.5(5) . . . . ? P2 C36 C37 C38 176.0(3) . . . . ? P2 C36 C41 C40 -176.2(3) . . . . ? P2 C36 C41 C42 3.6(5) . . . . ? P3 C50 C51 C52 178.7(3) . . . . ? P3 C50 C55 C54 -177.4(3) . . . . ? P3 C50 C55 C56 2.5(5) . . . . ? P3 C57 C58 C59 -178.2(3) . . . . ? P3 C57 C62 C61 179.0(3) . . . . ? P3 C57 C62 C63 -1.1(4) . . . . ? P4 C71 C72 C73 169.6(3) . . . . ? P4 C71 C76 C75 -169.4(3) . . . . ? P4 C71 C76 C77 10.4(5) . . . . ? P4 C78 C79 C80 -176.1(4) . . . . ? P4 C78 C83 C82 175.6(3) . . . . ? P4 C78 C83 C84 -4.1(5) . . . . ? Pd1 C1 C2 C3 154.0(3) . . . . ? Pd1 C1 C2 C7 -26.0(4) . . . . ? Pd2 C22 C23 C24 148.1(3) . . . . ? Pd2 C22 C23 C28 -31.6(4) . . . . ? Pd3 C43 C44 C45 -144.9(3) . . . . ? Pd3 C43 C44 C49 35.0(4) . . . . ? Pd4 C64 C65 C66 -176.5(3) . . . . ? Pd4 C64 C65 C70 5.9(5) . . . . ? C87 C88 C89 C90 179(3) . . . . ? C88 C89 C90 C91 -161(2) . . . . ? 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 1.0000 1.0000 -1.0000 0.0526 0.1642 -0.0290 -1.0000 -1.0000 1.0000 -0.0526 -0.1642 0.0290 1.0000 0.0000 -1.0001 0.0530 0.1175 0.0634 1.0000 -0.9999 -1.0002 0.0533 0.0708 0.1559 -1.0000 0.9999 1.0002 -0.0533 -0.0708 -0.1559 1.0000 1.0000 2.0000 -0.1721 0.0847 -0.0363 -1.0000 -1.0000 -2.0000 0.1721 -0.0847 0.0363 1.0000 0.0000 0.9999 -0.0968 0.0645 0.0586