#------------------------------------------------------------------------------ #$Date: 2024-10-24 01:06:42 +0300 (Thu, 24 Oct 2024) $ #$Revision: 295596 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572926.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_1572926 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 H82 O3 P4 Pd4' _chemical_formula_sum 'C84 H82 O3 P4 Pd4' _chemical_formula_weight 1688.97 _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 mixed _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 ; 2024-09-25 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 98.300(2) _cell_angle_beta 93.130(2) _cell_angle_gamma 116.152(3) _cell_formula_units_Z 2 _cell_length_a 13.6277(4) _cell_length_b 14.8406(4) _cell_length_c 20.3507(5) _cell_measurement_reflns_used 14589 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 71.0130 _cell_measurement_theta_min 3.6760 _cell_volume 3623.2(2) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _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 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -21.00 5.00 1.00 5.50 -- 0.00 -77.00 90.00 26 2 \w -21.00 14.00 1.00 5.50 -- 0.00 -77.00-150.00 35 3 \w -36.00 -8.00 1.00 5.50 -- 0.00 -57.00 -30.00 28 4 \w -69.00 -39.00 1.00 5.50 -- 0.00 -57.00 -30.00 30 5 \w -10.00 27.00 1.00 5.50 -- 0.00 -77.00 60.00 37 6 \w -14.00 28.00 1.00 5.50 -- 0.00 -77.00 0.00 42 7 \w 46.00 109.00 1.00 22.00 -- 54.00-125.00-150.00 63 8 \w 1.00 78.00 1.00 22.00 -- 54.00 -38.00 120.00 77 9 \w 32.00 125.00 1.00 22.00 -- 54.00 38.00 60.00 93 10 \w 28.00 80.00 1.00 22.00 -- 54.00-125.00 120.00 52 11 \w 97.00 123.00 1.00 22.00 -- 54.00 57.00 -60.00 26 12 \w 18.00 71.00 1.00 22.00 -- 54.00 -57.00 -90.00 53 13 \w -15.00 15.00 1.00 22.00 -- 54.00 -57.00 120.00 30 14 \w 37.00 123.00 1.00 22.00 -- 54.00 57.00 -90.00 86 15 \w 116.00 144.00 1.00 22.00 -- 108.00 111.00-120.00 28 16 \w 54.00 130.00 1.00 22.00 -- 108.00 -63.00 60.00 76 17 \w 107.00 133.00 1.00 22.00 -- 108.00 77.00 -90.00 26 18 \w 37.00 67.00 1.00 22.00 -- 108.00 -91.00 -60.00 30 19 \w 105.00 148.00 1.00 22.00 -- 108.00 111.00 90.00 43 20 \w 109.00 168.00 1.00 22.00 -- 108.00 63.00 60.00 59 21 \w 47.00 108.00 1.00 22.00 -- 108.00-111.00-180.00 61 22 \w 133.00 169.00 1.00 22.00 -- 108.00 77.00 30.00 36 23 \w 37.00 108.00 1.00 22.00 -- 108.00-111.00-120.00 71 24 \w 103.00 128.00 1.00 22.00 -- 108.00 77.00 30.00 25 25 \w 88.00 161.00 1.00 22.00 -- 108.00 63.00-180.00 73 26 \w 54.00 109.00 1.00 22.00 -- 108.00-111.00 -60.00 55 27 \w 48.00 129.00 1.00 22.00 -- 108.00 -50.00 -30.00 81 28 \w 143.00 177.00 1.00 22.00 -- 108.00 77.00 120.00 34 29 \w 48.00 104.00 1.00 22.00 -- 108.00 -91.00 -30.00 56 30 \w 60.00 109.00 1.00 22.00 -- 108.00-108.00 82.00 49 31 \w 103.00 129.00 1.00 22.00 -- 108.00 77.00 120.00 26 32 \w 109.00 165.00 1.00 22.00 -- 108.00 111.00 0.00 56 33 \w 87.00 174.00 1.00 22.00 -- 108.00 38.00 150.00 87 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1070219000 _diffrn_orient_matrix_UB_12 0.0363033000 _diffrn_orient_matrix_UB_13 0.0480578000 _diffrn_orient_matrix_UB_21 0.0682450000 _diffrn_orient_matrix_UB_22 0.0332767000 _diffrn_orient_matrix_UB_23 -0.0577728000 _diffrn_orient_matrix_UB_31 0.0059579000 _diffrn_orient_matrix_UB_32 0.1069495000 _diffrn_orient_matrix_UB_33 0.0176311000 _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 0.0291 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 25088 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.080 _diffrn_reflns_theta_max 67.080 _diffrn_reflns_theta_min 3.378 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.099 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.548 _exptl_crystal_description irregular _exptl_crystal_F_000 1708 _exptl_crystal_recrystallization_method 'crystallisation from dichloromethane and pentane' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.055 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 870 _refine_ls_number_reflns 12912 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0308 _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^)+(0.0341P)^2^+3.6378P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.0777 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11265 _reflns_number_total 12912 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05346j3.cif _cod_data_source_block ijsf21009 _cod_original_cell_volume 3623.25(19) _cod_database_code 1572926 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C84 H82 O3 P4 Pd4' _chemical_oxdiff_usercomment 'David Husbands DRH-01-131' _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 0.712 _shelx_estimated_absorpt_t_min 0.384 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All O(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O3-H3A = O1-H1 0.87 with sigma of 0.001 Pd4-H3A = H3A-Pd3 2.57 with sigma of 0.01 Pd1-H1 = H1-Pd2 2.57 with sigma of 0.01 3.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C64(H64A,H64B) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), 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) 3.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C35(H35A,H35B,H35C), C42(H42A,H42B, H42C), C56(H56A,H56B,H56C), C63(H63A,H63B,H63C), C77(H77A,H77B,H77C), C84(H84A, H84B,H84C) ; _shelx_res_file ; TITL ijsf21009_a.res in P-1 ijsf21009.res created by SHELXL-2018/3 at 08:28:14 on 25-Sep-2024 REM Old TITL ijsf21009 in P-1 REM SHELXT solution in P-1: R1 0.081, Rweak 0.004, Alpha 0.074 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C84 O3 P4 Pd4 CELL 1.54184 13.627734 14.840624 20.350735 98.2998 93.1304 116.1517 ZERR 2 0.000401 0.000411 0.000519 0.0022 0.0023 0.0029 LATT 1 SFAC C H O P Pd UNIT 168 164 6 8 8 DFIX 0.87 0.001 O3 H3a O1 H1 DFIX 2.57 0.01 Pd4 H3a H3a Pd3 DFIX 2.57 0.01 Pd1 H1 H1 Pd2 L.S. 8 PLAN 30 SIZE 0.04 0.07 0.13 TEMP -163 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 2 -1 3 OMIT 3 -5 4 REM REM REM WGHT 0.034100 3.637800 FVAR 2.79064 C1 1 0.249869 0.580636 0.578499 11.00000 0.01739 0.02941 = 0.03450 -0.00056 0.00109 0.00962 AFIX 23 H1A 2 0.217310 0.508477 0.584228 11.00000 -1.20000 H1B 2 0.199879 0.608718 0.594577 11.00000 -1.20000 AFIX 0 C2 1 0.251042 0.581833 0.504635 11.00000 0.02695 0.02958 = 0.03383 -0.00098 -0.00384 0.01991 C3 1 0.158272 0.518090 0.456968 11.00000 0.03390 0.03465 = 0.04122 -0.00376 -0.01059 0.01627 AFIX 43 H3 2 0.091617 0.473348 0.471202 11.00000 -1.20000 AFIX 0 C4 1 0.163689 0.520276 0.389257 11.00000 0.04780 0.04451 = 0.04742 -0.00884 -0.02164 0.02346 AFIX 43 H4 2 0.101117 0.475658 0.357466 11.00000 -1.20000 AFIX 0 C5 1 0.258307 0.586085 0.367613 11.00000 0.05158 0.04511 = 0.03072 -0.00163 -0.00535 0.03011 AFIX 43 H5 2 0.260359 0.588242 0.321259 11.00000 -1.20000 AFIX 0 C6 1 0.350893 0.649409 0.413695 11.00000 0.04473 0.04002 = 0.03078 0.00498 0.00216 0.02756 AFIX 43 H6 2 0.416873 0.694469 0.398982 11.00000 -1.20000 AFIX 0 C7 1 0.346587 0.646563 0.481785 11.00000 0.03108 0.02767 = 0.02867 0.00070 -0.00140 0.02020 C8 1 0.479406 0.850784 0.563541 11.00000 0.04892 0.02441 = 0.02712 0.00740 0.01145 0.01629 C9 1 0.386936 0.865823 0.540600 11.00000 0.06519 0.03787 = 0.04158 0.01468 0.01407 0.03254 AFIX 43 H9 2 0.322973 0.810271 0.515093 11.00000 -1.20000 AFIX 0 C10 1 0.391742 0.961090 0.555827 11.00000 0.06456 0.05396 = 0.04789 0.01286 0.00764 0.04065 AFIX 43 H10 2 0.331505 0.972427 0.541006 11.00000 -1.20000 AFIX 0 C11 1 0.486197 1.040207 0.593218 11.00000 0.07127 0.03972 = 0.04272 0.00674 0.01180 0.02132 AFIX 43 H11 2 0.488997 1.105893 0.603326 11.00000 -1.20000 AFIX 0 C12 1 0.574718 1.029411 0.616189 11.00000 0.07089 0.04681 = 0.03963 0.00432 0.01235 0.03713 AFIX 43 H12 2 0.638343 1.086507 0.640760 11.00000 -1.20000 AFIX 0 C13 1 0.570870 0.931799 0.603001 11.00000 0.05304 0.03267 = 0.03960 0.00752 0.01165 0.01448 C14 1 0.665202 0.920060 0.631822 11.00000 0.03772 0.03940 = 0.06964 0.01070 0.01279 0.01341 AFIX 137 H14A 2 0.638473 0.862902 0.655936 11.00000 -1.50000 H14B 2 0.715413 0.983039 0.662916 11.00000 -1.50000 H14C 2 0.704455 0.906434 0.595780 11.00000 -1.50000 AFIX 0 C15 1 0.579846 0.720299 0.513330 11.00000 0.02237 0.03441 = 0.02438 0.00304 0.00615 0.01200 C16 1 0.627096 0.790341 0.471369 11.00000 0.03410 0.04701 = 0.03391 0.01219 0.00807 0.01234 AFIX 43 H16 2 0.600460 0.838814 0.466967 11.00000 -1.20000 AFIX 0 C17 1 0.710383 0.791500 0.436417 11.00000 0.03312 0.06666 = 0.03959 0.01389 0.01357 0.01517 AFIX 43 H17 2 0.740777 0.839560 0.407897 11.00000 -1.20000 AFIX 0 C18 1 0.748552 0.723098 0.443214 11.00000 0.02472 0.08068 = 0.02661 -0.00256 0.00824 0.01637 AFIX 43 H18 2 0.806390 0.723273 0.419119 11.00000 -1.20000 AFIX 0 C19 1 0.704992 0.652373 0.484746 11.00000 0.03562 0.05711 = 0.04486 -0.01341 -0.00353 0.02856 AFIX 43 H19 2 0.732786 0.604443 0.488051 11.00000 -1.20000 AFIX 0 C20 1 0.620090 0.650598 0.522114 11.00000 0.02650 0.03493 = 0.03065 -0.00319 0.00238 0.01595 C21 1 0.582438 0.577698 0.570651 11.00000 0.04414 0.03414 = 0.04987 -0.00031 0.00068 0.02629 AFIX 137 H21A 2 0.618283 0.614490 0.616053 11.00000 -1.50000 H21B 2 0.602385 0.522282 0.557954 11.00000 -1.50000 H21C 2 0.502232 0.549049 0.569420 11.00000 -1.50000 AFIX 0 C22 1 0.367409 0.645522 0.870527 11.00000 0.01671 0.02602 = 0.02864 0.00774 0.00340 0.00690 AFIX 23 H22A 2 0.294912 0.642007 0.856463 11.00000 -1.20000 H22B 2 0.354382 0.577654 0.879627 11.00000 -1.20000 AFIX 0 C23 1 0.421118 0.724146 0.933851 11.00000 0.02236 0.02424 = 0.02679 0.01191 0.00667 0.01046 C24 1 0.364726 0.758447 0.977326 11.00000 0.02810 0.03518 = 0.03140 0.01151 0.00996 0.01439 AFIX 43 H24 2 0.286714 0.730158 0.968583 11.00000 -1.20000 AFIX 0 C25 1 0.421109 0.833563 1.033368 11.00000 0.03420 0.03202 = 0.03580 0.00831 0.01844 0.01430 AFIX 43 H25 2 0.381680 0.857814 1.062026 11.00000 -1.20000 AFIX 0 C26 1 0.535423 0.874021 1.048164 11.00000 0.03511 0.02916 = 0.02845 0.00231 0.00389 0.00806 AFIX 43 H26 2 0.573333 0.923547 1.087659 11.00000 -1.20000 AFIX 0 C27 1 0.593041 0.841445 1.004886 11.00000 0.02501 0.02931 = 0.02619 0.00547 -0.00046 0.01122 AFIX 43 H27 2 0.671015 0.869668 1.013934 11.00000 -1.20000 AFIX 0 C28 1 0.536375 0.767354 0.948208 11.00000 0.02087 0.02196 = 0.02715 0.00994 0.00656 0.01136 C29 1 0.623168 0.623625 0.898420 11.00000 0.01368 0.02327 = 0.03408 0.00850 0.00005 0.00429 C30 1 0.613960 0.601469 0.961783 11.00000 0.03374 0.03560 = 0.04428 0.01602 0.00835 0.01963 AFIX 43 H30 2 0.592495 0.639569 0.994317 11.00000 -1.20000 AFIX 0 C31 1 0.635844 0.523369 0.978994 11.00000 0.04269 0.04591 = 0.05553 0.02851 0.01029 0.02268 AFIX 43 H31 2 0.630129 0.509421 1.023122 11.00000 -1.20000 AFIX 0 C32 1 0.665391 0.467330 0.932277 11.00000 0.03017 0.03351 = 0.07259 0.02389 0.01236 0.02000 AFIX 43 H32 2 0.680474 0.414433 0.943718 11.00000 -1.20000 AFIX 0 C33 1 0.673131 0.488241 0.868338 11.00000 0.02113 0.02666 = 0.06331 0.01049 0.00723 0.01382 AFIX 43 H33 2 0.693158 0.448555 0.836058 11.00000 -1.20000 AFIX 0 C34 1 0.652526 0.565785 0.849432 11.00000 0.01409 0.02177 = 0.04838 0.00505 0.00147 0.00612 C35 1 0.661200 0.584479 0.779017 11.00000 0.03288 0.03457 = 0.04372 0.00573 0.01087 0.02176 AFIX 137 H35A 2 0.588117 0.567952 0.756773 11.00000 -1.50000 H35B 2 0.689676 0.541211 0.754487 11.00000 -1.50000 H35C 2 0.711476 0.656490 0.779775 11.00000 -1.50000 AFIX 0 C36 1 0.731923 0.834275 0.883529 11.00000 0.01586 0.02259 = 0.02197 0.00298 0.00437 0.00675 C37 1 0.824300 0.828575 0.912632 11.00000 0.02106 0.02693 = 0.03182 0.00603 0.00504 0.01317 AFIX 43 H37 2 0.814941 0.767535 0.927081 11.00000 -1.20000 AFIX 0 C38 1 0.927682 0.909229 0.920627 11.00000 0.01910 0.03325 = 0.04008 0.00653 -0.00047 0.01132 AFIX 43 H38 2 0.988829 0.904875 0.941924 11.00000 -1.20000 AFIX 0 C39 1 0.942516 0.996276 0.897756 11.00000 0.01439 0.03140 = 0.05375 0.01091 0.00261 0.00299 AFIX 43 H39 2 1.014459 1.051412 0.901697 11.00000 -1.20000 AFIX 0 C40 1 0.852553 1.003888 0.868870 11.00000 0.02501 0.02410 = 0.04821 0.01067 0.00302 0.00657 AFIX 43 H40 2 0.863676 1.064602 0.853302 11.00000 -1.20000 AFIX 0 C41 1 0.745935 0.923937 0.862255 11.00000 0.02063 0.02578 = 0.02902 0.00375 -0.00015 0.01078 C42 1 0.650870 0.938315 0.833752 11.00000 0.02852 0.02727 = 0.05366 0.01588 -0.00487 0.00852 AFIX 137 H42A 2 0.611556 0.885764 0.793688 11.00000 -1.50000 H42B 2 0.678669 1.006110 0.821757 11.00000 -1.50000 H42C 2 0.600380 0.932447 0.867220 11.00000 -1.50000 AFIX 0 C43 1 0.311758 0.423931 0.739552 11.00000 0.01886 0.01901 = 0.03475 0.00617 0.00180 0.00891 AFIX 23 H43A 2 0.316087 0.386450 0.696325 11.00000 -1.20000 H43B 2 0.385124 0.482949 0.755050 11.00000 -1.20000 AFIX 0 C44 1 0.284610 0.354968 0.789642 11.00000 0.02395 0.01735 = 0.02940 0.00095 -0.00185 0.00936 C45 1 0.364731 0.346322 0.830165 11.00000 0.02312 0.02874 = 0.03784 0.00469 -0.00279 0.01056 AFIX 43 H45 2 0.440597 0.386237 0.826987 11.00000 -1.20000 AFIX 0 C46 1 0.334335 0.279849 0.875041 11.00000 0.02923 0.04211 = 0.04101 0.01183 -0.00122 0.01884 AFIX 43 H46 2 0.389530 0.273124 0.901469 11.00000 -1.20000 AFIX 0 C47 1 0.224866 0.223387 0.881738 11.00000 0.03726 0.04518 = 0.04700 0.02755 0.00332 0.01599 AFIX 43 H47 2 0.205017 0.179226 0.913399 11.00000 -1.20000 AFIX 0 C48 1 0.143433 0.231102 0.842101 11.00000 0.02479 0.04016 = 0.05323 0.02615 0.00382 0.00835 AFIX 43 H48 2 0.067779 0.191625 0.846011 11.00000 -1.20000 AFIX 0 C49 1 0.174048 0.297310 0.796651 11.00000 0.02276 0.02193 = 0.03622 0.00866 0.00012 0.00843 C50 1 -0.034383 0.307869 0.786504 11.00000 0.02112 0.02211 = 0.03250 0.01225 0.00505 0.01022 C51 1 -0.140511 0.232483 0.758451 11.00000 0.01984 0.02660 = 0.03930 0.00963 0.00566 0.00946 AFIX 43 H51 2 -0.149859 0.187807 0.717577 11.00000 -1.20000 AFIX 0 C52 1 -0.231836 0.222257 0.789484 11.00000 0.01942 0.03055 = 0.05481 0.01639 0.00990 0.00809 AFIX 43 H52 2 -0.303277 0.171349 0.769623 11.00000 -1.20000 AFIX 0 C53 1 -0.219218 0.285329 0.848622 11.00000 0.03123 0.03287 = 0.05377 0.02005 0.02477 0.01714 AFIX 43 H53 2 -0.281859 0.278324 0.869917 11.00000 -1.20000 AFIX 0 C54 1 -0.115320 0.359319 0.877459 11.00000 0.03749 0.03265 = 0.03712 0.01225 0.01702 0.01347 AFIX 43 H54 2 -0.107588 0.401965 0.918972 11.00000 -1.20000 AFIX 0 C55 1 -0.021743 0.373127 0.847433 11.00000 0.02728 0.02851 = 0.03272 0.01184 0.00834 0.00996 C56 1 0.089272 0.455725 0.880704 11.00000 0.03243 0.04616 = 0.03277 -0.00451 0.00707 0.00507 AFIX 137 H56A 2 0.135105 0.424569 0.894869 11.00000 -1.50000 H56B 2 0.079798 0.496483 0.919927 11.00000 -1.50000 H56C 2 0.125224 0.499924 0.848988 11.00000 -1.50000 AFIX 0 C57 1 0.026530 0.215542 0.671157 11.00000 0.01582 0.01585 = 0.03838 0.00244 0.00671 0.00341 C58 1 0.043919 0.130156 0.673798 11.00000 0.02597 0.02212 = 0.05868 0.00939 0.01160 0.00973 AFIX 43 H58 2 0.084483 0.128030 0.712519 11.00000 -1.20000 AFIX 0 C59 1 0.002357 0.048247 0.620229 11.00000 0.03912 0.02220 = 0.07663 0.00090 0.02165 0.00991 AFIX 43 H59 2 0.015201 -0.009323 0.622095 11.00000 -1.20000 AFIX 0 C60 1 -0.057344 0.050802 0.564585 11.00000 0.03527 0.03056 = 0.05381 -0.01270 0.01497 0.00372 AFIX 43 H60 2 -0.087376 -0.005897 0.528397 11.00000 -1.20000 AFIX 0 C61 1 -0.073743 0.134155 0.560984 11.00000 0.03314 0.03704 = 0.03640 -0.00297 0.00646 0.00490 AFIX 43 H61 2 -0.114508 0.134848 0.521835 11.00000 -1.20000 AFIX 0 C62 1 -0.032090 0.218944 0.613488 11.00000 0.02071 0.02501 = 0.03736 0.00226 0.00777 0.00545 C63 1 -0.052260 0.308594 0.606427 11.00000 0.03935 0.03653 = 0.03274 0.00505 -0.00690 0.01558 AFIX 137 H63A 2 0.017108 0.366408 0.601471 11.00000 -1.50000 H63B 2 -0.080975 0.327623 0.646397 11.00000 -1.50000 H63C 2 -0.106121 0.290458 0.566790 11.00000 -1.50000 AFIX 0 C64 1 0.364641 0.836092 0.766752 11.00000 0.01486 0.01668 = 0.04254 0.00224 0.00260 0.00483 AFIX 23 H64A 2 0.395612 0.841493 0.813128 11.00000 -1.20000 H64B 2 0.419892 0.835559 0.737274 11.00000 -1.20000 AFIX 0 C65 1 0.350808 0.930730 0.763544 11.00000 0.02134 0.01937 = 0.02621 0.00254 0.00527 0.00738 C66 1 0.436795 1.024178 0.758239 11.00000 0.02363 0.02390 = 0.04279 0.00434 0.00866 0.00778 AFIX 43 H66 2 0.509500 1.031070 0.758354 11.00000 -1.20000 AFIX 0 C67 1 0.418126 1.106648 0.752837 11.00000 0.03448 0.02254 = 0.06073 0.01224 0.01279 0.00641 AFIX 43 H67 2 0.477949 1.170165 0.749741 11.00000 -1.20000 AFIX 0 C68 1 0.312282 1.097640 0.751878 11.00000 0.04628 0.02340 = 0.05771 0.01181 0.00757 0.01727 AFIX 43 H68 2 0.299364 1.154163 0.746357 11.00000 -1.20000 AFIX 0 C69 1 0.225491 1.006428 0.758952 11.00000 0.02912 0.02440 = 0.05041 0.00771 0.00782 0.01341 AFIX 43 H69 2 0.153321 1.000512 0.760087 11.00000 -1.20000 AFIX 0 C70 1 0.245728 0.923491 0.764378 11.00000 0.02322 0.01507 = 0.03175 0.00298 0.00438 0.00742 C71 1 0.022916 0.785671 0.717580 11.00000 0.01997 0.01989 = 0.03257 0.00463 0.00174 0.01080 C72 1 -0.053780 0.807692 0.749490 11.00000 0.02596 0.03725 = 0.03591 0.01176 0.00563 0.01842 AFIX 43 H72 2 -0.046926 0.820178 0.797038 11.00000 -1.20000 AFIX 0 C73 1 -0.140363 0.811668 0.712694 11.00000 0.02331 0.03954 = 0.04870 0.01431 0.00625 0.01930 AFIX 43 H73 2 -0.191783 0.827776 0.734849 11.00000 -1.20000 AFIX 0 C74 1 -0.150643 0.792094 0.644150 11.00000 0.02959 0.03269 = 0.04674 0.00847 -0.00722 0.01584 AFIX 43 H74 2 -0.210442 0.793132 0.618565 11.00000 -1.20000 AFIX 0 C75 1 -0.074346 0.770825 0.612030 11.00000 0.04275 0.03401 = 0.03531 0.00467 -0.00321 0.02372 AFIX 43 H75 2 -0.082543 0.757483 0.564453 11.00000 -1.20000 AFIX 0 C76 1 0.013574 0.768557 0.647646 11.00000 0.03141 0.02386 = 0.03358 0.00397 0.00227 0.01628 C77 1 0.096743 0.749574 0.609768 11.00000 0.06628 0.08102 = 0.02571 0.00937 0.00705 0.05616 AFIX 137 H77A 2 0.103075 0.690882 0.622381 11.00000 -1.50000 H77B 2 0.168616 0.810224 0.620779 11.00000 -1.50000 H77C 2 0.072606 0.735273 0.561519 11.00000 -1.50000 AFIX 0 C78 1 0.113192 0.793965 0.853588 11.00000 0.01881 0.03303 = 0.03332 0.01002 0.00690 0.02055 C79 1 0.183680 0.877288 0.903440 11.00000 0.02516 0.03862 = 0.03416 0.00507 0.00290 0.01693 AFIX 43 H79 2 0.239411 0.936001 0.890941 11.00000 -1.20000 AFIX 0 C80 1 0.173344 0.875381 0.970819 11.00000 0.03747 0.05491 = 0.03364 0.00385 0.00087 0.02994 AFIX 43 H80 2 0.221895 0.931993 1.004259 11.00000 -1.20000 AFIX 0 C81 1 0.091225 0.789750 0.988603 11.00000 0.06286 0.06300 = 0.03583 0.02050 0.01310 0.04919 AFIX 43 H81 2 0.082857 0.787647 1.034479 11.00000 -1.20000 AFIX 0 C82 1 0.021966 0.707958 0.939942 11.00000 0.04969 0.04367 = 0.05242 0.02478 0.02395 0.03251 AFIX 43 H82 2 -0.034135 0.650176 0.953112 11.00000 -1.20000 AFIX 0 C83 1 0.030948 0.706583 0.871850 11.00000 0.02807 0.03174 = 0.04543 0.01560 0.01200 0.01997 C84 1 -0.045402 0.614946 0.820449 11.00000 0.02930 0.03399 = 0.06363 0.02044 0.01722 0.01014 AFIX 137 H84A 2 -0.105895 0.626395 0.801801 11.00000 -1.50000 H84B 2 -0.075509 0.554585 0.841504 11.00000 -1.50000 H84C 2 -0.004692 0.603979 0.784455 11.00000 -1.50000 AFIX 0 O1 3 0.549501 0.727850 0.710033 11.00000 0.03211 0.03132 = 0.01472 0.00411 0.00141 0.02210 H1 2 0.581179 0.688889 0.700276 11.00000 -1.20000 O2 3 0.321352 0.621392 0.723577 11.00000 0.01195 0.01537 = 0.02898 0.00387 0.00337 0.00628 O3 3 0.090624 0.545889 0.709318 11.00000 0.02603 0.00983 = 0.03012 0.00300 -0.00024 0.00904 H3A 2 0.073365 0.536528 0.666245 11.00000 -1.20000 P1 4 0.459420 0.718351 0.549977 11.00000 0.02261 0.02121 = 0.02419 0.00487 0.00359 0.01180 P2 4 0.594369 0.726762 0.878104 11.00000 0.01474 0.01925 = 0.02517 0.00578 0.00198 0.00771 P3 4 0.084156 0.323430 0.742126 11.00000 0.01386 0.01527 = 0.02980 0.00622 0.00245 0.00448 P4 4 0.143327 0.794582 0.767182 11.00000 0.01526 0.01751 = 0.02920 0.00498 0.00357 0.00891 PD1 5 0.396517 0.658168 0.638916 11.00000 0.01459 0.01800 = 0.02367 0.00347 0.00262 0.00755 PD2 5 0.461168 0.678134 0.794654 11.00000 0.01244 0.01712 = 0.02410 0.00481 0.00222 0.00624 PD3 5 0.198582 0.476266 0.724902 11.00000 0.01228 0.01373 = 0.02463 0.00364 0.00301 0.00549 PD4 5 0.226558 0.699049 0.740366 11.00000 0.01205 0.01438 = 0.02668 0.00403 0.00221 0.00610 HKLF 4 REM ijsf21009_a.res in P-1 REM wR2 = 0.0777, GooF = S = 1.025, Restrained GooF = 1.025 for all data REM R1 = 0.0308 for 11265 Fo > 4sig(Fo) and 0.0378 for all 12912 data REM 870 parameters refined using 6 restraints END WGHT 0.0342 3.6514 REM Highest difference peak 1.055, deepest hole -0.681, 1-sigma level 0.088 Q1 1 0.1169 0.4614 0.6788 11.00000 0.05 1.06 Q2 1 0.3643 0.5816 0.6210 11.00000 0.05 0.82 Q3 1 0.6798 1.0154 0.6224 11.00000 0.05 0.78 Q4 1 0.1474 0.6788 0.6877 11.00000 0.05 0.73 Q5 1 0.4664 0.9146 0.5727 11.00000 0.05 0.73 Q6 1 0.5293 0.7221 0.7354 11.00000 0.05 0.69 Q7 1 0.5778 0.7238 0.7155 11.00000 0.05 0.62 Q8 1 0.4570 0.7006 0.8397 11.00000 0.05 0.58 Q9 1 0.5406 0.6999 0.3688 11.00000 0.05 0.57 Q10 1 0.6376 0.9157 0.5844 11.00000 0.05 0.57 Q11 1 0.0974 0.5576 0.7420 11.00000 0.05 0.56 Q12 1 0.1213 0.5304 0.7039 11.00000 0.05 0.56 Q13 1 0.2031 0.4885 0.7590 11.00000 0.05 0.54 Q14 1 0.1364 0.6011 0.7189 11.00000 0.05 0.53 Q15 1 0.3045 0.6387 0.8188 11.00000 0.05 0.50 Q16 1 0.2331 0.7408 0.7771 11.00000 0.05 0.46 Q17 1 0.3225 0.8557 0.5521 11.00000 0.05 0.45 Q18 1 0.4341 0.7458 0.6590 11.00000 0.05 0.43 Q19 1 0.1265 0.4651 0.7723 11.00000 0.05 0.43 Q20 1 0.4738 0.6431 0.7429 11.00000 0.05 0.42 Q21 1 0.0413 0.5204 0.7168 11.00000 0.05 0.42 Q22 1 0.5397 0.8653 0.5686 11.00000 0.05 0.42 Q23 1 0.5803 0.7601 0.9176 11.00000 0.05 0.42 Q24 1 0.2854 0.6373 0.7146 11.00000 0.05 0.41 Q25 1 0.4566 0.6384 0.6827 11.00000 0.05 0.41 Q26 1 0.6750 0.7825 0.8825 11.00000 0.05 0.40 Q27 1 0.1719 0.7633 0.7605 11.00000 0.05 0.40 Q28 1 0.2815 0.5731 0.7587 11.00000 0.05 0.39 Q29 1 0.4783 0.7014 0.6437 11.00000 0.05 0.38 Q30 1 0.1871 0.3958 0.7191 11.00000 0.05 0.38 ; _shelx_res_checksum 53811 _olex2_date_sample_data_collection 2021-01-28 _olex2_date_sample_submission 2021-01-25 _olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount' _olex2_submission_original_sample_id DRH-01-131 _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 2.275 _oxdiff_exptl_absorpt_empirical_full_min 0.603 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 0.2499(3) 0.5806(3) 0.57850(19) 0.0283(8) Uani 1 1 d . . . . . H1A H 0.217310 0.508477 0.584228 0.034 Uiso 1 1 calc R U . . . H1B H 0.199879 0.608718 0.594577 0.034 Uiso 1 1 calc R U . . . C2 C 0.2510(3) 0.5818(3) 0.5046(2) 0.0286(8) Uani 1 1 d . . . . . C3 C 0.1583(4) 0.5181(3) 0.4570(2) 0.0382(10) Uani 1 1 d . . . . . H3 H 0.091617 0.473348 0.471202 0.046 Uiso 1 1 calc R U . . . C4 C 0.1637(4) 0.5203(4) 0.3893(2) 0.0487(13) Uani 1 1 d . . . . . H4 H 0.101117 0.475658 0.357466 0.058 Uiso 1 1 calc R U . . . C5 C 0.2583(4) 0.5861(3) 0.3676(2) 0.0408(11) Uani 1 1 d . . . . . H5 H 0.260359 0.588242 0.321259 0.049 Uiso 1 1 calc R U . . . C6 C 0.3509(4) 0.6494(3) 0.4137(2) 0.0357(10) Uani 1 1 d . . . . . H6 H 0.416873 0.694469 0.398982 0.043 Uiso 1 1 calc R U . . . C7 C 0.3466(3) 0.6466(3) 0.48178(19) 0.0273(8) Uani 1 1 d . . . . . C8 C 0.4794(4) 0.8508(3) 0.56354(19) 0.0331(9) Uani 1 1 d . . . . . C9 C 0.3869(4) 0.8658(3) 0.5406(2) 0.0437(11) Uani 1 1 d . . . . . H9 H 0.322973 0.810271 0.515093 0.052 Uiso 1 1 calc R U . . . C10 C 0.3917(5) 0.9611(4) 0.5558(2) 0.0499(12) Uani 1 1 d . . . . . H10 H 0.331505 0.972427 0.541006 0.060 Uiso 1 1 calc R U . . . C11 C 0.4862(5) 1.0402(4) 0.5932(2) 0.0526(13) Uani 1 1 d . . . . . H11 H 0.488997 1.105893 0.603326 0.063 Uiso 1 1 calc R U . . . C12 C 0.5747(5) 1.0294(4) 0.6162(2) 0.0488(12) Uani 1 1 d . . . . . H12 H 0.638343 1.086507 0.640760 0.059 Uiso 1 1 calc R U . . . C13 C 0.5709(4) 0.9318(3) 0.6030(2) 0.0433(11) Uani 1 1 d . . . . . C14 C 0.6652(4) 0.9201(4) 0.6318(3) 0.0502(12) Uani 1 1 d . . . . . H14A H 0.638473 0.862902 0.655936 0.075 Uiso 1 1 calc R U . . . H14B H 0.715413 0.983039 0.662916 0.075 Uiso 1 1 calc R U . . . H14C H 0.704455 0.906434 0.595780 0.075 Uiso 1 1 calc R U . . . C15 C 0.5798(3) 0.7203(3) 0.51333(18) 0.0275(8) Uani 1 1 d . . . . . C16 C 0.6271(4) 0.7903(4) 0.4714(2) 0.0400(10) Uani 1 1 d . . . . . H16 H 0.600460 0.838814 0.466967 0.048 Uiso 1 1 calc R U . . . C17 C 0.7104(4) 0.7915(4) 0.4364(2) 0.0485(12) Uani 1 1 d . . . . . H17 H 0.740777 0.839560 0.407897 0.058 Uiso 1 1 calc R U . . . C18 C 0.7486(4) 0.7231(4) 0.4432(2) 0.0480(13) Uani 1 1 d . . . . . H18 H 0.806390 0.723273 0.419119 0.058 Uiso 1 1 calc R U . . . C19 C 0.7050(4) 0.6524(4) 0.4847(2) 0.0460(12) Uani 1 1 d . . . . . H19 H 0.732786 0.604443 0.488051 0.055 Uiso 1 1 calc R U . . . C20 C 0.6201(3) 0.6506(3) 0.5221(2) 0.0310(9) Uani 1 1 d . . . . . C21 C 0.5824(4) 0.5777(3) 0.5707(2) 0.0407(10) Uani 1 1 d . . . . . H21A H 0.618283 0.614490 0.616053 0.061 Uiso 1 1 calc R U . . . H21B H 0.602385 0.522282 0.557954 0.061 Uiso 1 1 calc R U . . . H21C H 0.502232 0.549049 0.569420 0.061 Uiso 1 1 calc R U . . . C22 C 0.3674(3) 0.6455(3) 0.87053(18) 0.0245(8) Uani 1 1 d . . . . . H22A H 0.294912 0.642007 0.856463 0.029 Uiso 1 1 calc R U . . . H22B H 0.354382 0.577654 0.879627 0.029 Uiso 1 1 calc R U . . . C23 C 0.4211(3) 0.7241(3) 0.93385(18) 0.0236(8) Uani 1 1 d . . . . . C24 C 0.3647(3) 0.7584(3) 0.9773(2) 0.0307(9) Uani 1 1 d . . . . . H24 H 0.286714 0.730158 0.968583 0.037 Uiso 1 1 calc R U . . . C25 C 0.4211(3) 0.8336(3) 1.0334(2) 0.0335(9) Uani 1 1 d . . . . . H25 H 0.381680 0.857814 1.062026 0.040 Uiso 1 1 calc R U . . . C26 C 0.5354(3) 0.8740(3) 1.0482(2) 0.0337(9) Uani 1 1 d . . . . . H26 H 0.573333 0.923547 1.087659 0.040 Uiso 1 1 calc R U . . . C27 C 0.5930(3) 0.8414(3) 1.00489(18) 0.0274(8) Uani 1 1 d . . . . . H27 H 0.671015 0.869668 1.013934 0.033 Uiso 1 1 calc R U . . . C28 C 0.5364(3) 0.7674(3) 0.94821(18) 0.0220(7) Uani 1 1 d . . . . . C29 C 0.6232(3) 0.6236(3) 0.89842(19) 0.0250(8) Uani 1 1 d . . . . . C30 C 0.6140(3) 0.6015(3) 0.9618(2) 0.0353(9) Uani 1 1 d . . . . . H30 H 0.592495 0.639569 0.994317 0.042 Uiso 1 1 calc R U . . . C31 C 0.6358(4) 0.5234(4) 0.9790(3) 0.0448(11) Uani 1 1 d . . . . . H31 H 0.630129 0.509421 1.023122 0.054 Uiso 1 1 calc R U . . . C32 C 0.6654(4) 0.4673(3) 0.9323(3) 0.0416(11) Uani 1 1 d . . . . . H32 H 0.680474 0.414433 0.943718 0.050 Uiso 1 1 calc R U . . . C33 C 0.6731(3) 0.4882(3) 0.8683(2) 0.0356(10) Uani 1 1 d . . . . . H33 H 0.693158 0.448555 0.836058 0.043 Uiso 1 1 calc R U . . . C34 C 0.6525(3) 0.5658(3) 0.8494(2) 0.0291(9) Uani 1 1 d . . . . . C35 C 0.6612(4) 0.5845(3) 0.7790(2) 0.0346(9) Uani 1 1 d . . . . . H35A H 0.588117 0.567952 0.756773 0.052 Uiso 1 1 calc R U . . . H35B H 0.689676 0.541211 0.754487 0.052 Uiso 1 1 calc R U . . . H35C H 0.711476 0.656490 0.779775 0.052 Uiso 1 1 calc R U . . . C36 C 0.7319(3) 0.8343(3) 0.88353(17) 0.0209(7) Uani 1 1 d . . . . . C37 C 0.8243(3) 0.8286(3) 0.91263(19) 0.0256(8) Uani 1 1 d . . . . . H37 H 0.814941 0.767535 0.927081 0.031 Uiso 1 1 calc R U . . . C38 C 0.9277(3) 0.9092(3) 0.9206(2) 0.0312(9) Uani 1 1 d . . . . . H38 H 0.988829 0.904875 0.941924 0.037 Uiso 1 1 calc R U . . . C39 C 0.9425(3) 0.9963(3) 0.8978(2) 0.0357(10) Uani 1 1 d . . . . . H39 H 1.014459 1.051412 0.901697 0.043 Uiso 1 1 calc R U . . . C40 C 0.8526(3) 1.0039(3) 0.8689(2) 0.0338(9) Uani 1 1 d . . . . . H40 H 0.863676 1.064602 0.853302 0.041 Uiso 1 1 calc R U . . . C41 C 0.7459(3) 0.9239(3) 0.86226(18) 0.0254(8) Uani 1 1 d . . . . . C42 C 0.6509(3) 0.9383(3) 0.8338(2) 0.0375(10) Uani 1 1 d . . . . . H42A H 0.611556 0.885764 0.793688 0.056 Uiso 1 1 calc R U . . . H42B H 0.678669 1.006110 0.821757 0.056 Uiso 1 1 calc R U . . . H42C H 0.600380 0.932447 0.867220 0.056 Uiso 1 1 calc R U . . . C43 C 0.3118(3) 0.4239(3) 0.73955(19) 0.0240(8) Uani 1 1 d . . . . . H43A H 0.316087 0.386450 0.696325 0.029 Uiso 1 1 calc R U . . . H43B H 0.385124 0.482949 0.755050 0.029 Uiso 1 1 calc R U . . . C44 C 0.2846(3) 0.3550(3) 0.78964(18) 0.0242(8) Uani 1 1 d . . . . . C45 C 0.3647(3) 0.3463(3) 0.8302(2) 0.0308(9) Uani 1 1 d . . . . . H45 H 0.440597 0.386237 0.826987 0.037 Uiso 1 1 calc R U . . . C46 C 0.3343(3) 0.2798(3) 0.8750(2) 0.0363(10) Uani 1 1 d . . . . . H46 H 0.389530 0.273124 0.901469 0.044 Uiso 1 1 calc R U . . . C47 C 0.2249(4) 0.2234(4) 0.8817(2) 0.0422(11) Uani 1 1 d . . . . . H47 H 0.205017 0.179226 0.913399 0.051 Uiso 1 1 calc R U . . . C48 C 0.1434(4) 0.2311(3) 0.8421(2) 0.0399(11) Uani 1 1 d . . . . . H48 H 0.067779 0.191625 0.846011 0.048 Uiso 1 1 calc R U . . . C49 C 0.1740(3) 0.2973(3) 0.7967(2) 0.0274(8) Uani 1 1 d . . . . . C50 C -0.0344(3) 0.3079(3) 0.78650(19) 0.0242(8) Uani 1 1 d . . . . . C51 C -0.1405(3) 0.2325(3) 0.7585(2) 0.0285(8) Uani 1 1 d . . . . . H51 H -0.149859 0.187807 0.717577 0.034 Uiso 1 1 calc R U . . . C52 C -0.2318(3) 0.2223(3) 0.7895(2) 0.0350(10) Uani 1 1 d . . . . . H52 H -0.303277 0.171349 0.769623 0.042 Uiso 1 1 calc R U . . . C53 C -0.2192(4) 0.2853(3) 0.8486(2) 0.0362(10) Uani 1 1 d . . . . . H53 H -0.281859 0.278324 0.869917 0.043 Uiso 1 1 calc R U . . . C54 C -0.1153(4) 0.3593(3) 0.8775(2) 0.0355(9) Uani 1 1 d . . . . . H54 H -0.107588 0.401965 0.918972 0.043 Uiso 1 1 calc R U . . . C55 C -0.0217(3) 0.3731(3) 0.8474(2) 0.0297(8) Uani 1 1 d . . . . . C56 C 0.0893(4) 0.4557(4) 0.8807(2) 0.0431(11) Uani 1 1 d . . . . . H56A H 0.135105 0.424569 0.894869 0.065 Uiso 1 1 calc R U . . . H56B H 0.079798 0.496483 0.919927 0.065 Uiso 1 1 calc R U . . . H56C H 0.125224 0.499924 0.848988 0.065 Uiso 1 1 calc R U . . . C57 C 0.0265(3) 0.2155(3) 0.6712(2) 0.0249(8) Uani 1 1 d . . . . . C58 C 0.0439(3) 0.1302(3) 0.6738(2) 0.0356(10) Uani 1 1 d . . . . . H58 H 0.084483 0.128030 0.712519 0.043 Uiso 1 1 calc R U . . . C59 C 0.0024(4) 0.0482(3) 0.6202(3) 0.0478(12) Uani 1 1 d . . . . . H59 H 0.015201 -0.009323 0.622095 0.057 Uiso 1 1 calc R U . . . C60 C -0.0573(4) 0.0508(3) 0.5646(2) 0.0460(12) Uani 1 1 d . . . . . H60 H -0.087376 -0.005897 0.528397 0.055 Uiso 1 1 calc R U . . . C61 C -0.0737(4) 0.1342(3) 0.5610(2) 0.0407(11) Uani 1 1 d . . . . . H61 H -0.114508 0.134848 0.521835 0.049 Uiso 1 1 calc R U . . . C62 C -0.0321(3) 0.2189(3) 0.6135(2) 0.0298(9) Uani 1 1 d . . . . . C63 C -0.0523(4) 0.3086(3) 0.6064(2) 0.0375(10) Uani 1 1 d . . . . . H63A H 0.017108 0.366408 0.601471 0.056 Uiso 1 1 calc R U . . . H63B H -0.080975 0.327623 0.646397 0.056 Uiso 1 1 calc R U . . . H63C H -0.106121 0.290458 0.566790 0.056 Uiso 1 1 calc R U . . . C64 C 0.3646(3) 0.8361(3) 0.7668(2) 0.0260(8) Uani 1 1 d . . . . . H64A H 0.395612 0.841493 0.813128 0.031 Uiso 1 1 calc R U . . . H64B H 0.419892 0.835559 0.737274 0.031 Uiso 1 1 calc R U . . . C65 C 0.3508(3) 0.9307(3) 0.76354(18) 0.0231(8) Uani 1 1 d . . . . . C66 C 0.4368(3) 1.0242(3) 0.7582(2) 0.0313(9) Uani 1 1 d . . . . . H66 H 0.509500 1.031070 0.758354 0.038 Uiso 1 1 calc R U . . . C67 C 0.4181(4) 1.1066(3) 0.7528(2) 0.0409(11) Uani 1 1 d . . . . . H67 H 0.477949 1.170165 0.749741 0.049 Uiso 1 1 calc R U . . . C68 C 0.3123(4) 1.0976(3) 0.7519(2) 0.0414(11) Uani 1 1 d . . . . . H68 H 0.299364 1.154163 0.746357 0.050 Uiso 1 1 calc R U . . . C69 C 0.2255(3) 1.0064(3) 0.7590(2) 0.0340(9) Uani 1 1 d . . . . . H69 H 0.153321 1.000512 0.760087 0.041 Uiso 1 1 calc R U . . . C70 C 0.2457(3) 0.9235(3) 0.76438(19) 0.0240(8) Uani 1 1 d . . . . . C71 C 0.0229(3) 0.7857(3) 0.71758(19) 0.0236(8) Uani 1 1 d . . . . . C72 C -0.0538(3) 0.8077(3) 0.7495(2) 0.0309(9) Uani 1 1 d . . . . . H72 H -0.046926 0.820178 0.797038 0.037 Uiso 1 1 calc R U . . . C73 C -0.1404(3) 0.8117(3) 0.7127(2) 0.0346(9) Uani 1 1 d . . . . . H73 H -0.191783 0.827776 0.734849 0.041 Uiso 1 1 calc R U . . . C74 C -0.1506(3) 0.7921(3) 0.6442(2) 0.0361(10) Uani 1 1 d . . . . . H74 H -0.210442 0.793132 0.618565 0.043 Uiso 1 1 calc R U . . . C75 C -0.0743(4) 0.7708(3) 0.6120(2) 0.0356(10) Uani 1 1 d . . . . . H75 H -0.082543 0.757483 0.564453 0.043 Uiso 1 1 calc R U . . . C76 C 0.0136(3) 0.7686(3) 0.6476(2) 0.0285(8) Uani 1 1 d . . . . . C77 C 0.0967(4) 0.7496(4) 0.6098(2) 0.0492(13) Uani 1 1 d . . . . . H77A H 0.103075 0.690882 0.622381 0.074 Uiso 1 1 calc R U . . . H77B H 0.168616 0.810224 0.620779 0.074 Uiso 1 1 calc R U . . . H77C H 0.072606 0.735273 0.561519 0.074 Uiso 1 1 calc R U . . . C78 C 0.1132(3) 0.7940(3) 0.85359(19) 0.0245(8) Uani 1 1 d . . . . . C79 C 0.1837(3) 0.8773(3) 0.9034(2) 0.0320(9) Uani 1 1 d . . . . . H79 H 0.239411 0.936001 0.890941 0.038 Uiso 1 1 calc R U . . . C80 C 0.1733(4) 0.8754(4) 0.9708(2) 0.0393(10) Uani 1 1 d . . . . . H80 H 0.221895 0.931993 1.004259 0.047 Uiso 1 1 calc R U . . . C81 C 0.0912(4) 0.7897(4) 0.9886(2) 0.0446(12) Uani 1 1 d . . . . . H81 H 0.082857 0.787647 1.034479 0.054 Uiso 1 1 calc R U . . . C82 C 0.0220(4) 0.7080(4) 0.9399(2) 0.0419(11) Uani 1 1 d . . . . . H82 H -0.034135 0.650176 0.953112 0.050 Uiso 1 1 calc R U . . . C83 C 0.0309(3) 0.7066(3) 0.8719(2) 0.0315(9) Uani 1 1 d . . . . . C84 C -0.0454(4) 0.6149(3) 0.8204(2) 0.0422(11) Uani 1 1 d . . . . . H84A H -0.105895 0.626395 0.801801 0.063 Uiso 1 1 calc R U . . . H84B H -0.075509 0.554585 0.841504 0.063 Uiso 1 1 calc R U . . . H84C H -0.004692 0.603979 0.784455 0.063 Uiso 1 1 calc R U . . . O1 O 0.5495(2) 0.72785(19) 0.71003(11) 0.0233(5) Uani 1 1 d D . . . . H1 H 0.5812(9) 0.6889(8) 0.7003(6) 0.028 Uiso 1 1 d D U . . . O2 O 0.32135(18) 0.62139(17) 0.72358(12) 0.0187(5) Uani 1 1 d . . . . . O3 O 0.0906(2) 0.54589(16) 0.70932(12) 0.0219(5) Uani 1 1 d D . . . . H3A H 0.0734(10) 0.5365(9) 0.66624(17) 0.026 Uiso 1 1 d D U . . . P1 P 0.45942(8) 0.71835(7) 0.54998(4) 0.02189(19) Uani 1 1 d . . . . . P2 P 0.59437(7) 0.72676(7) 0.87810(4) 0.01957(18) Uani 1 1 d . . . . . P3 P 0.08416(7) 0.32343(6) 0.74213(5) 0.02024(18) Uani 1 1 d . . . . . P4 P 0.14333(7) 0.79458(6) 0.76718(5) 0.02001(18) Uani 1 1 d . . . . . Pd1 Pd 0.39652(2) 0.65817(2) 0.63892(2) 0.01874(6) Uani 1 1 d D . . . . Pd2 Pd 0.46117(2) 0.67813(2) 0.79465(2) 0.01797(6) Uani 1 1 d D . . . . Pd3 Pd 0.19858(2) 0.47627(2) 0.72490(2) 0.01701(6) Uani 1 1 d D . . . . Pd4 Pd 0.22656(2) 0.69905(2) 0.74037(2) 0.01766(6) Uani 1 1 d D . . . . 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 0.0174(18) 0.029(2) 0.034(2) -0.0006(16) 0.0011(16) 0.0096(16) C2 0.027(2) 0.030(2) 0.034(2) -0.0010(16) -0.0038(16) 0.0199(17) C3 0.034(2) 0.035(2) 0.041(2) -0.0038(19) -0.0106(19) 0.016(2) C4 0.048(3) 0.045(3) 0.047(3) -0.009(2) -0.022(2) 0.023(2) C5 0.052(3) 0.045(3) 0.031(2) -0.0016(19) -0.005(2) 0.030(2) C6 0.045(3) 0.040(2) 0.031(2) 0.0050(18) 0.0022(19) 0.028(2) C7 0.031(2) 0.0277(19) 0.0287(19) 0.0007(15) -0.0014(16) 0.0202(18) C8 0.049(3) 0.0244(19) 0.027(2) 0.0074(16) 0.0115(18) 0.0163(19) C9 0.065(3) 0.038(2) 0.042(2) 0.015(2) 0.014(2) 0.033(2) C10 0.065(3) 0.054(3) 0.048(3) 0.013(2) 0.008(2) 0.041(3) C11 0.071(4) 0.040(3) 0.043(3) 0.007(2) 0.012(3) 0.021(3) C12 0.071(4) 0.047(3) 0.040(3) 0.004(2) 0.012(2) 0.037(3) C13 0.053(3) 0.033(2) 0.040(2) 0.0075(19) 0.012(2) 0.014(2) C14 0.038(3) 0.039(3) 0.070(3) 0.011(2) 0.013(2) 0.013(2) C15 0.0224(19) 0.034(2) 0.0244(18) 0.0030(16) 0.0062(15) 0.0120(17) C16 0.034(2) 0.047(3) 0.034(2) 0.0122(19) 0.0081(18) 0.012(2) C17 0.033(3) 0.067(3) 0.040(3) 0.014(2) 0.014(2) 0.015(2) C18 0.025(2) 0.081(4) 0.027(2) -0.003(2) 0.0082(18) 0.016(2) C19 0.036(3) 0.057(3) 0.045(3) -0.013(2) -0.004(2) 0.029(2) C20 0.026(2) 0.035(2) 0.031(2) -0.0032(17) 0.0024(16) 0.0160(18) C21 0.044(3) 0.034(2) 0.050(3) 0.000(2) 0.001(2) 0.026(2) C22 0.0167(18) 0.0260(19) 0.0286(19) 0.0077(15) 0.0034(15) 0.0069(15) C23 0.0224(19) 0.0242(18) 0.0268(18) 0.0119(15) 0.0067(15) 0.0105(16) C24 0.028(2) 0.035(2) 0.031(2) 0.0115(17) 0.0100(16) 0.0144(18) C25 0.034(2) 0.032(2) 0.036(2) 0.0083(17) 0.0184(18) 0.0143(19) C26 0.035(2) 0.029(2) 0.028(2) 0.0023(16) 0.0039(17) 0.0081(18) C27 0.025(2) 0.029(2) 0.0262(19) 0.0055(15) -0.0005(15) 0.0112(17) C28 0.0209(18) 0.0220(17) 0.0272(18) 0.0099(14) 0.0066(15) 0.0114(15) C29 0.0137(17) 0.0233(18) 0.034(2) 0.0085(15) 0.0001(15) 0.0043(15) C30 0.034(2) 0.036(2) 0.044(2) 0.0160(19) 0.0083(19) 0.0196(19) C31 0.043(3) 0.046(3) 0.056(3) 0.029(2) 0.010(2) 0.023(2) C32 0.030(2) 0.034(2) 0.073(3) 0.024(2) 0.012(2) 0.020(2) C33 0.021(2) 0.027(2) 0.063(3) 0.0105(19) 0.0072(19) 0.0138(17) C34 0.0141(18) 0.0218(18) 0.048(2) 0.0051(17) 0.0015(16) 0.0061(15) C35 0.033(2) 0.035(2) 0.044(2) 0.0057(18) 0.0109(19) 0.0218(19) C36 0.0159(17) 0.0226(18) 0.0220(17) 0.0030(14) 0.0044(14) 0.0067(15) C37 0.0211(19) 0.0269(19) 0.032(2) 0.0060(16) 0.0050(15) 0.0132(16) C38 0.0191(19) 0.033(2) 0.040(2) 0.0065(17) -0.0005(16) 0.0113(17) C39 0.0144(19) 0.031(2) 0.054(3) 0.0109(19) 0.0026(18) 0.0030(17) C40 0.025(2) 0.024(2) 0.048(2) 0.0107(18) 0.0030(18) 0.0066(17) C41 0.0206(19) 0.0258(19) 0.0290(19) 0.0038(15) -0.0002(15) 0.0108(16) C42 0.029(2) 0.027(2) 0.054(3) 0.0159(19) -0.0049(19) 0.0085(18) C43 0.0189(18) 0.0190(17) 0.035(2) 0.0062(15) 0.0018(15) 0.0089(15) C44 0.0239(19) 0.0173(17) 0.0294(19) 0.0010(14) -0.0018(15) 0.0094(15) C45 0.023(2) 0.029(2) 0.038(2) 0.0047(17) -0.0028(17) 0.0106(17) C46 0.029(2) 0.042(2) 0.041(2) 0.0118(19) -0.0012(18) 0.019(2) C47 0.037(2) 0.045(3) 0.047(3) 0.028(2) 0.003(2) 0.016(2) C48 0.025(2) 0.040(2) 0.053(3) 0.026(2) 0.0038(19) 0.0083(19) C49 0.0228(19) 0.0219(18) 0.036(2) 0.0087(16) 0.0001(16) 0.0084(16) C50 0.0211(19) 0.0221(18) 0.0325(19) 0.0123(15) 0.0050(15) 0.0102(15) C51 0.0198(19) 0.0266(19) 0.039(2) 0.0096(17) 0.0057(16) 0.0095(16) C52 0.019(2) 0.031(2) 0.055(3) 0.0164(19) 0.0099(18) 0.0081(17) C53 0.031(2) 0.033(2) 0.054(3) 0.020(2) 0.025(2) 0.0171(19) C54 0.037(2) 0.033(2) 0.037(2) 0.0123(18) 0.0170(19) 0.0135(19) C55 0.027(2) 0.029(2) 0.033(2) 0.0118(16) 0.0083(16) 0.0100(17) C56 0.032(2) 0.046(3) 0.033(2) -0.0045(19) 0.0071(19) 0.005(2) C57 0.0158(18) 0.0158(17) 0.038(2) 0.0024(15) 0.0067(15) 0.0034(14) C58 0.026(2) 0.0221(19) 0.059(3) 0.0094(18) 0.0116(19) 0.0097(17) C59 0.039(3) 0.022(2) 0.077(4) 0.001(2) 0.022(3) 0.010(2) C60 0.035(3) 0.031(2) 0.054(3) -0.013(2) 0.015(2) 0.004(2) C61 0.033(2) 0.037(2) 0.036(2) -0.0030(19) 0.0065(19) 0.005(2) C62 0.0207(19) 0.0250(19) 0.037(2) 0.0023(16) 0.0078(16) 0.0055(16) C63 0.039(2) 0.037(2) 0.033(2) 0.0050(18) -0.0069(18) 0.016(2) C64 0.0149(18) 0.0167(17) 0.043(2) 0.0022(15) 0.0026(16) 0.0048(15) C65 0.0213(19) 0.0194(17) 0.0262(18) 0.0025(14) 0.0053(15) 0.0074(15) C66 0.024(2) 0.0239(19) 0.043(2) 0.0043(17) 0.0087(17) 0.0078(17) C67 0.034(2) 0.023(2) 0.061(3) 0.012(2) 0.013(2) 0.0064(18) C68 0.046(3) 0.023(2) 0.058(3) 0.0118(19) 0.008(2) 0.017(2) C69 0.029(2) 0.024(2) 0.050(3) 0.0077(18) 0.0078(19) 0.0134(18) C70 0.0232(19) 0.0151(16) 0.0318(19) 0.0030(14) 0.0044(15) 0.0074(15) C71 0.0200(18) 0.0199(17) 0.0326(19) 0.0046(15) 0.0017(15) 0.0108(15) C72 0.026(2) 0.037(2) 0.036(2) 0.0118(18) 0.0056(17) 0.0184(18) C73 0.023(2) 0.040(2) 0.049(3) 0.0143(19) 0.0062(18) 0.0193(19) C74 0.030(2) 0.033(2) 0.047(2) 0.0085(19) -0.0072(19) 0.0158(19) C75 0.043(3) 0.034(2) 0.035(2) 0.0047(18) -0.0032(19) 0.024(2) C76 0.031(2) 0.0239(19) 0.034(2) 0.0040(16) 0.0023(17) 0.0163(17) C77 0.066(3) 0.081(4) 0.026(2) 0.009(2) 0.007(2) 0.056(3) C78 0.0188(18) 0.033(2) 0.033(2) 0.0100(16) 0.0069(15) 0.0205(16) C79 0.025(2) 0.039(2) 0.034(2) 0.0051(18) 0.0029(17) 0.0169(18) C80 0.037(2) 0.055(3) 0.034(2) 0.004(2) 0.0009(19) 0.030(2) C81 0.063(3) 0.063(3) 0.036(2) 0.020(2) 0.013(2) 0.049(3) C82 0.050(3) 0.044(3) 0.052(3) 0.025(2) 0.024(2) 0.033(2) C83 0.028(2) 0.032(2) 0.045(2) 0.0156(18) 0.0120(18) 0.0200(18) C84 0.029(2) 0.034(2) 0.064(3) 0.020(2) 0.017(2) 0.0101(19) O1 0.0321(14) 0.0313(13) 0.0147(11) 0.0041(10) 0.0014(10) 0.0221(12) O2 0.0119(11) 0.0154(11) 0.0290(13) 0.0039(9) 0.0034(9) 0.0063(9) O3 0.0260(13) 0.0098(11) 0.0301(13) 0.0030(9) -0.0002(10) 0.0090(10) P1 0.0226(5) 0.0212(4) 0.0242(4) 0.0049(3) 0.0036(4) 0.0118(4) P2 0.0147(4) 0.0192(4) 0.0252(4) 0.0058(3) 0.0020(3) 0.0077(4) P3 0.0139(4) 0.0153(4) 0.0298(5) 0.0062(3) 0.0025(3) 0.0045(3) P4 0.0153(4) 0.0175(4) 0.0292(5) 0.0050(3) 0.0036(3) 0.0089(4) Pd1 0.01459(13) 0.01800(12) 0.02367(13) 0.00347(10) 0.00262(10) 0.00755(10) Pd2 0.01244(12) 0.01712(12) 0.02410(13) 0.00481(9) 0.00222(9) 0.00624(10) Pd3 0.01228(12) 0.01373(12) 0.02463(13) 0.00364(9) 0.00301(9) 0.00549(10) Pd4 0.01205(12) 0.01438(12) 0.02668(13) 0.00403(9) 0.00221(9) 0.00610(10) 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' 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 0 0 1 0.0084 0 0 -1 0.0318 0 1 0 0.0381 0 -1 0 0.0283 1 1 0 0.0368 -1 1 0 0.0551 -1 0 0 0.0722 1 0 0 0.0492 2 -5 2 0.0052 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 107.2 . . ? C2 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? C2 C1 Pd1 117.4(3) . . ? Pd1 C1 H1A 107.9 . . ? Pd1 C1 H1B 107.9 . . ? C3 C2 C1 122.3(4) . . ? C7 C2 C1 119.7(3) . . ? C7 C2 C3 118.0(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 119.6 . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(4) . . ? C6 C5 H5 120.1 . . ? C5 C6 H6 120.2 . . ? C5 C6 C7 119.7(4) . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 121.3(4) . . ? C2 C7 P1 111.7(3) . . ? C6 C7 P1 126.9(3) . . ? C9 C8 P1 116.5(3) . . ? C13 C8 C9 119.6(4) . . ? C13 C8 P1 123.0(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 C8 119.6(5) . . ? C10 C9 H9 120.2 . . ? C9 C10 H10 120.7 . . ? C9 C10 C11 118.6(5) . . ? C11 C10 H10 120.7 . . ? C10 C11 H11 118.1 . . ? C12 C11 C10 123.8(5) . . ? C12 C11 H11 118.1 . . ? C11 C12 H12 120.6 . . ? C11 C12 C13 118.8(5) . . ? C13 C12 H12 120.6 . . ? C8 C13 C12 119.4(5) . . ? C8 C13 C14 122.5(4) . . ? C12 C13 C14 118.1(5) . . ? 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 . . ? C16 C15 P1 117.5(3) . . ? C20 C15 C16 119.8(4) . . ? C20 C15 P1 122.5(3) . . ? C15 C16 H16 118.9 . . ? C17 C16 C15 122.2(5) . . ? C17 C16 H16 118.9 . . ? C16 C17 H17 120.6 . . ? C18 C17 C16 118.7(5) . . ? C18 C17 H17 120.6 . . ? C17 C18 H18 119.3 . . ? C17 C18 C19 121.3(4) . . ? C19 C18 H18 119.3 . . ? C18 C19 H19 119.5 . . ? C18 C19 C20 121.1(4) . . ? C20 C19 H19 119.5 . . ? C15 C20 C19 116.9(4) . . ? C15 C20 C21 124.5(4) . . ? C19 C20 C21 118.6(4) . . ? 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 . . ? H22A C22 H22B 107.9 . . ? C23 C22 H22A 109.1 . . ? C23 C22 H22B 109.1 . . ? C23 C22 Pd2 112.3(2) . . ? Pd2 C22 H22A 109.1 . . ? Pd2 C22 H22B 109.1 . . ? C24 C23 C22 124.3(3) . . ? C24 C23 C28 118.4(4) . . ? C28 C23 C22 117.3(3) . . ? C23 C24 H24 119.7 . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C24 C25 H25 119.7 . . ? C24 C25 C26 120.6(4) . . ? C26 C25 H25 119.7 . . ? C25 C26 H26 120.2 . . ? C27 C26 C25 119.5(4) . . ? C27 C26 H26 120.2 . . ? C26 C27 H27 120.2 . . ? C26 C27 C28 119.7(4) . . ? C28 C27 H27 120.2 . . ? C23 C28 P2 110.6(3) . . ? C27 C28 C23 121.3(4) . . ? C27 C28 P2 127.5(3) . . ? C30 C29 C34 119.9(4) . . ? C30 C29 P2 119.4(3) . . ? C34 C29 P2 120.7(3) . . ? C29 C30 H30 119.6 . . ? C29 C30 C31 120.8(4) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.4(4) . . ? C33 C32 H32 120.3 . . ? C32 C33 H33 118.9 . . ? C32 C33 C34 122.3(4) . . ? C34 C33 H33 118.9 . . ? C29 C34 C35 122.4(3) . . ? C33 C34 C29 117.7(4) . . ? C33 C34 C35 119.9(4) . . ? 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 P2 119.6(3) . . ? C41 C36 C37 119.2(3) . . ? C41 C36 P2 121.1(3) . . ? C36 C37 H37 119.3 . . ? C38 C37 C36 121.3(3) . . ? C38 C37 H37 119.3 . . ? C37 C38 H38 120.1 . . ? C37 C38 C39 119.7(4) . . ? C39 C38 H38 120.1 . . ? C38 C39 H39 120.0 . . ? C38 C39 C40 120.0(4) . . ? C40 C39 H39 120.0 . . ? C39 C40 H40 119.4 . . ? C39 C40 C41 121.2(4) . . ? C41 C40 H40 119.4 . . ? C36 C41 C40 118.4(3) . . ? C36 C41 C42 122.6(3) . . ? C40 C41 C42 119.0(3) . . ? 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 112.7(3) . . ? Pd3 C43 H43A 109.0 . . ? Pd3 C43 H43B 109.0 . . ? C45 C44 C43 123.1(3) . . ? C45 C44 C49 118.5(3) . . ? C49 C44 C43 118.5(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 C44 120.4(4) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 119.7 . . ? C47 C46 C45 120.7(4) . . ? C47 C46 H46 119.7 . . ? C46 C47 H47 120.0 . . ? C46 C47 C48 120.0(4) . . ? C48 C47 H47 120.0 . . ? C47 C48 H48 120.4 . . ? C47 C48 C49 119.3(4) . . ? C49 C48 H48 120.4 . . ? C44 C49 P3 111.5(3) . . ? C48 C49 C44 121.2(4) . . ? C48 C49 P3 127.3(3) . . ? C51 C50 C55 118.9(4) . . ? C51 C50 P3 119.9(3) . . ? C55 C50 P3 121.2(3) . . ? C50 C51 H51 119.5 . . ? C52 C51 C50 121.0(4) . . ? C52 C51 H51 119.5 . . ? C51 C52 H52 120.0 . . ? C53 C52 C51 120.0(4) . . ? C53 C52 H52 120.0 . . ? C52 C53 H53 120.0 . . ? C52 C53 C54 120.0(4) . . ? C54 C53 H53 120.0 . . ? C53 C54 H54 119.1 . . ? C53 C54 C55 121.8(4) . . ? C55 C54 H54 119.1 . . ? C50 C55 C56 122.0(4) . . ? C54 C55 C50 118.4(4) . . ? C54 C55 C56 119.6(4) . . ? 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(4) . . ? C58 C57 P3 119.6(3) . . ? C62 C57 P3 120.9(3) . . ? C57 C58 H58 119.8 . . ? C59 C58 C57 120.5(4) . . ? C59 C58 H58 119.8 . . ? C58 C59 H59 120.1 . . ? C60 C59 C58 119.8(4) . . ? C60 C59 H59 120.1 . . ? C59 C60 H60 119.8 . . ? C61 C60 C59 120.4(4) . . ? C61 C60 H60 119.8 . . ? C60 C61 H61 119.1 . . ? C60 C61 C62 121.7(4) . . ? C62 C61 H61 119.1 . . ? C57 C62 C63 122.6(3) . . ? C61 C62 C57 118.1(4) . . ? C61 C62 C63 119.3(4) . . ? 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 107.3 . . ? C65 C64 H64A 108.1 . . ? C65 C64 H64B 108.1 . . ? C65 C64 Pd4 116.9(2) . . ? Pd4 C64 H64A 108.1 . . ? Pd4 C64 H64B 108.1 . . ? C66 C65 C64 123.7(3) . . ? C70 C65 C64 118.1(3) . . ? C70 C65 C66 118.2(3) . . ? C65 C66 H66 119.5 . . ? C67 C66 C65 120.9(4) . . ? C67 C66 H66 119.5 . . ? C66 C67 H67 119.9 . . ? C66 C67 C68 120.3(4) . . ? C68 C67 H67 119.9 . . ? C67 C68 H68 120.0 . . ? C69 C68 C67 120.1(4) . . ? C69 C68 H68 120.0 . . ? C68 C69 H69 120.6 . . ? C68 C69 C70 118.9(4) . . ? C70 C69 H69 120.6 . . ? C65 C70 C69 121.5(3) . . ? C65 C70 P4 111.9(3) . . ? C69 C70 P4 126.4(3) . . ? C72 C71 C76 119.5(3) . . ? C72 C71 P4 119.6(3) . . ? C76 C71 P4 120.4(3) . . ? C71 C72 H72 119.6 . . ? C73 C72 C71 120.9(4) . . ? C73 C72 H72 119.6 . . ? C72 C73 H73 120.4 . . ? C74 C73 C72 119.2(4) . . ? C74 C73 H73 120.4 . . ? C73 C74 H74 119.9 . . ? C73 C74 C75 120.3(4) . . ? C75 C74 H74 119.9 . . ? C74 C75 H75 119.3 . . ? C76 C75 C74 121.4(4) . . ? C76 C75 H75 119.3 . . ? C71 C76 C77 122.5(4) . . ? C75 C76 C71 118.6(4) . . ? C75 C76 C77 118.9(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(4) . . ? C79 C78 P4 118.5(3) . . ? C83 C78 P4 121.2(3) . . ? C78 C79 H79 119.5 . . ? C80 C79 C78 121.1(4) . . ? C80 C79 H79 119.5 . . ? C79 C80 H80 120.4 . . ? C81 C80 C79 119.1(4) . . ? C81 C80 H80 120.4 . . ? C80 C81 H81 120.0 . . ? C82 C81 C80 120.0(4) . . ? C82 C81 H81 120.0 . . ? C81 C82 H82 118.8 . . ? C81 C82 C83 122.4(4) . . ? C83 C82 H82 118.8 . . ? C78 C83 C84 121.7(4) . . ? C82 C83 C78 117.7(4) . . ? C82 C83 C84 120.6(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 O1 H1 104.8(8) . . ? Pd2 O1 H1 106.3(8) . . ? Pd2 O1 Pd1 92.89(10) . . ? Pd1 O2 Pd2 99.66(9) . . ? Pd1 O2 Pd4 108.52(10) . . ? Pd3 O2 Pd1 121.79(11) . . ? Pd3 O2 Pd2 116.91(11) . . ? Pd3 O2 Pd4 97.35(9) . . ? Pd4 O2 Pd2 112.94(10) . . ? Pd3 O3 H3A 106.8(8) . . ? Pd3 O3 Pd4 91.77(9) . . ? Pd4 O3 H3A 107.2(8) . . ? C7 P1 C8 106.59(18) . . ? C7 P1 C15 103.46(18) . . ? C7 P1 Pd1 105.50(13) . . ? C8 P1 Pd1 106.37(13) . . ? C15 P1 C8 106.06(19) . . ? C15 P1 Pd1 127.38(13) . . ? C28 P2 C29 107.66(17) . . ? C28 P2 C36 103.58(17) . . ? C28 P2 Pd2 101.91(12) . . ? C29 P2 Pd2 114.33(12) . . ? C36 P2 C29 103.55(16) . . ? C36 P2 Pd2 124.38(12) . . ? C49 P3 C50 105.96(17) . . ? C49 P3 C57 105.61(18) . . ? C49 P3 Pd3 101.11(12) . . ? C50 P3 Pd3 119.60(12) . . ? C57 P3 C50 103.99(17) . . ? C57 P3 Pd3 119.02(12) . . ? C70 P4 C71 101.70(17) . . ? C70 P4 C78 106.81(18) . . ? C70 P4 Pd4 104.45(12) . . ? C71 P4 C78 106.82(17) . . ? C71 P4 Pd4 124.71(12) . . ? C78 P4 Pd4 110.74(11) . . ? C1 Pd1 O1 173.73(13) . . ? C1 Pd1 O2 91.84(13) . . ? C1 Pd1 P1 84.52(12) . . ? C1 Pd1 Pd2 131.84(11) . . ? O1 Pd1 Pd2 43.33(6) . . ? O2 Pd1 O1 83.66(9) . . ? O2 Pd1 P1 167.88(7) . . ? O2 Pd1 Pd2 40.39(6) . . ? P1 Pd1 O1 100.77(7) . . ? P1 Pd1 Pd2 143.33(3) . . ? C22 Pd2 O1 171.09(12) . . ? C22 Pd2 O2 91.69(12) . . ? C22 Pd2 P2 81.40(10) . . ? C22 Pd2 Pd1 131.47(10) . . ? O1 Pd2 P2 103.49(7) . . ? O1 Pd2 Pd1 43.78(6) . . ? O2 Pd2 O1 83.67(9) . . ? O2 Pd2 P2 172.70(7) . . ? O2 Pd2 Pd1 39.95(6) . . ? P2 Pd2 Pd1 147.09(3) . . ? C43 Pd3 O2 91.53(12) . . ? C43 Pd3 O3 174.67(12) . . ? C43 Pd3 P3 82.30(10) . . ? C43 Pd3 Pd4 130.67(10) . . ? O2 Pd3 O3 83.14(9) . . ? O2 Pd3 P3 170.32(7) . . ? O2 Pd3 Pd4 41.55(6) . . ? O3 Pd3 P3 102.98(7) . . ? O3 Pd3 Pd4 44.20(6) . . ? P3 Pd3 Pd4 141.25(3) . . ? C64 Pd4 O2 91.50(12) . . ? C64 Pd4 O3 174.02(12) . . ? C64 Pd4 P4 82.46(11) . . ? C64 Pd4 Pd3 130.44(10) . . ? O2 Pd4 O3 82.57(9) . . ? O2 Pd4 P4 173.06(7) . . ? O2 Pd4 Pd3 41.10(6) . . ? O3 Pd4 P4 103.50(7) . . ? O3 Pd4 Pd3 44.04(6) . . ? P4 Pd4 Pd3 143.40(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 C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.507(5) . ? C1 Pd1 2.031(4) . ? C2 C3 1.408(5) . ? C2 C7 1.388(6) . ? C3 H3 0.9500 . ? C3 C4 1.388(7) . ? C4 H4 0.9500 . ? C4 C5 1.374(7) . ? C5 H5 0.9500 . ? C5 C6 1.388(6) . ? C6 H6 0.9500 . ? C6 C7 1.396(5) . ? C7 P1 1.822(4) . ? C8 C9 1.439(6) . ? C8 C13 1.391(6) . ? C8 P1 1.838(4) . ? C9 H9 0.9500 . ? C9 C10 1.374(6) . ? C10 H10 0.9500 . ? C10 C11 1.385(7) . ? C11 H11 0.9500 . ? C11 C12 1.353(7) . ? C12 H12 0.9500 . ? C12 C13 1.412(6) . ? C13 C14 1.474(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.397(6) . ? C15 C20 1.395(6) . ? C15 P1 1.830(4) . ? C16 H16 0.9500 . ? C16 C17 1.367(6) . ? C17 H17 0.9500 . ? C17 C18 1.348(7) . ? C18 H18 0.9500 . ? C18 C19 1.389(7) . ? C19 H19 0.9500 . ? C19 C20 1.412(6) . ? C20 C21 1.511(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.506(5) . ? C22 Pd2 2.034(4) . ? C23 C24 1.386(5) . ? C23 C28 1.404(5) . ? C24 H24 0.9500 . ? C24 C25 1.384(6) . ? C25 H25 0.9500 . ? C25 C26 1.396(6) . ? C26 H26 0.9500 . ? C26 C27 1.383(6) . ? C27 H27 0.9500 . ? C27 C28 1.387(5) . ? C28 P2 1.821(4) . ? C29 C30 1.375(5) . ? C29 C34 1.411(6) . ? C29 P2 1.834(4) . ? C30 H30 0.9500 . ? C30 C31 1.402(6) . ? C31 H31 0.9500 . ? C31 C32 1.366(7) . ? C32 H32 0.9500 . ? C32 C33 1.380(6) . ? C33 H33 0.9500 . ? C33 C34 1.397(5) . ? C34 C35 1.500(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.403(5) . ? C36 C41 1.395(5) . ? C36 P2 1.834(3) . ? C37 H37 0.9500 . ? C37 C38 1.370(5) . ? C38 H38 0.9500 . ? C38 C39 1.371(6) . ? C39 H39 0.9500 . ? C39 C40 1.387(6) . ? C40 H40 0.9500 . ? C40 C41 1.396(5) . ? C41 C42 1.503(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.494(5) . ? C43 Pd3 2.036(3) . ? C44 C45 1.394(5) . ? C44 C49 1.395(5) . ? C45 H45 0.9500 . ? C45 C46 1.386(6) . ? C46 H46 0.9500 . ? C46 C47 1.378(6) . ? C47 H47 0.9500 . ? C47 C48 1.391(6) . ? C48 H48 0.9500 . ? C48 C49 1.392(5) . ? C49 P3 1.810(4) . ? C50 C51 1.403(5) . ? C50 C55 1.410(5) . ? C50 P3 1.836(4) . ? C51 H51 0.9500 . ? C51 C52 1.385(6) . ? C52 H52 0.9500 . ? C52 C53 1.365(6) . ? C53 H53 0.9500 . ? C53 C54 1.381(6) . ? C54 H54 0.9500 . ? C54 C55 1.390(6) . ? C55 C56 1.505(6) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.396(5) . ? C57 C62 1.403(6) . ? C57 P3 1.835(4) . ? C58 H58 0.9500 . ? C58 C59 1.389(6) . ? C59 H59 0.9500 . ? C59 C60 1.373(7) . ? C60 H60 0.9500 . ? C60 C61 1.361(7) . ? C61 H61 0.9500 . ? C61 C62 1.401(6) . ? C62 C63 1.497(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 C65 1.507(5) . ? C64 Pd4 2.041(3) . ? C65 C66 1.390(5) . ? C65 C70 1.389(5) . ? C66 H66 0.9500 . ? C66 C67 1.373(6) . ? C67 H67 0.9500 . ? C67 C68 1.387(6) . ? C68 H68 0.9500 . ? C68 C69 1.384(6) . ? C69 H69 0.9500 . ? C69 C70 1.392(5) . ? C70 P4 1.816(4) . ? C71 C72 1.391(5) . ? C71 C76 1.398(5) . ? C71 P4 1.822(4) . ? C72 H72 0.9500 . ? C72 C73 1.391(5) . ? C73 H73 0.9500 . ? C73 C74 1.370(6) . ? C74 H74 0.9500 . ? C74 C75 1.383(6) . ? C75 H75 0.9500 . ? C75 C76 1.382(5) . ? C76 C77 1.507(6) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.402(6) . ? C78 C83 1.407(5) . ? C78 P4 1.828(4) . ? C79 H79 0.9500 . ? C79 C80 1.389(6) . ? C80 H80 0.9500 . ? C80 C81 1.386(7) . ? C81 H81 0.9500 . ? C81 C82 1.373(7) . ? C82 H82 0.9500 . ? C82 C83 1.396(6) . ? C83 C84 1.500(6) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? O1 H1 0.8697(10) . ? O1 Pd1 2.202(2) . ? O1 Pd2 2.184(2) . ? O2 Pd1 2.070(2) . ? O2 Pd2 2.089(2) . ? O2 Pd3 2.070(2) . ? O2 Pd4 2.088(2) . ? O3 H3A 0.8698(10) . ? O3 Pd3 2.172(2) . ? O3 Pd4 2.178(2) . ? P1 Pd1 2.1840(9) . ? P2 Pd2 2.2033(9) . ? P3 Pd3 2.2069(9) . ? P4 Pd4 2.2037(9) . ? Pd1 Pd2 3.1785(4) . ? Pd3 Pd4 3.1227(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -178.7(4) . . . . ? C1 C2 C7 C6 179.7(4) . . . . ? C1 C2 C7 P1 2.0(4) . . . . ? C2 C3 C4 C5 -1.6(7) . . . . ? C2 C7 P1 C8 -107.5(3) . . . . ? C2 C7 P1 C15 140.9(3) . . . . ? C2 C7 P1 Pd1 5.3(3) . . . . ? C3 C2 C7 C6 0.5(6) . . . . ? C3 C2 C7 P1 -177.2(3) . . . . ? C3 C4 C5 C6 1.8(7) . . . . ? C4 C5 C6 C7 -0.8(6) . . . . ? C5 C6 C7 C2 -0.4(6) . . . . ? C5 C6 C7 P1 177.0(3) . . . . ? C6 C7 P1 C8 74.9(4) . . . . ? C6 C7 P1 C15 -36.7(4) . . . . ? C6 C7 P1 Pd1 -172.3(3) . . . . ? C7 C2 C3 C4 0.4(6) . . . . ? C8 C9 C10 C11 -0.1(7) . . . . ? C9 C8 C13 C12 -4.3(6) . . . . ? C9 C8 C13 C14 175.9(4) . . . . ? C9 C8 P1 C7 22.3(4) . . . . ? C9 C8 P1 C15 132.1(3) . . . . ? C9 C8 P1 Pd1 -89.9(3) . . . . ? C9 C10 C11 C12 -0.3(8) . . . . ? C10 C11 C12 C13 -1.5(8) . . . . ? C11 C12 C13 C8 3.8(7) . . . . ? C11 C12 C13 C14 -176.4(5) . . . . ? C13 C8 C9 C10 2.4(6) . . . . ? C13 C8 P1 C7 -167.8(4) . . . . ? C13 C8 P1 C15 -58.1(4) . . . . ? C13 C8 P1 Pd1 79.9(4) . . . . ? C15 C16 C17 C18 -0.5(7) . . . . ? C16 C15 C20 C19 -2.8(6) . . . . ? C16 C15 C20 C21 174.4(4) . . . . ? C16 C15 P1 C7 78.9(3) . . . . ? C16 C15 P1 C8 -33.1(4) . . . . ? C16 C15 P1 Pd1 -159.2(3) . . . . ? C16 C17 C18 C19 0.0(7) . . . . ? C17 C18 C19 C20 -0.9(7) . . . . ? C18 C19 C20 C15 2.3(6) . . . . ? C18 C19 C20 C21 -175.1(4) . . . . ? C20 C15 C16 C17 2.0(7) . . . . ? C20 C15 P1 C7 -96.6(3) . . . . ? C20 C15 P1 C8 151.5(3) . . . . ? C20 C15 P1 Pd1 25.4(4) . . . . ? C22 C23 C24 C25 -177.8(3) . . . . ? C22 C23 C28 C27 179.0(3) . . . . ? C22 C23 C28 P2 7.4(4) . . . . ? C23 C24 C25 C26 -1.9(6) . . . . ? C23 C28 P2 C29 -100.4(3) . . . . ? C23 C28 P2 C36 150.3(3) . . . . ? C23 C28 P2 Pd2 20.2(3) . . . . ? C24 C23 C28 C27 1.0(5) . . . . ? C24 C23 C28 P2 -170.6(3) . . . . ? C24 C25 C26 C27 2.6(6) . . . . ? C25 C26 C27 C28 -1.5(6) . . . . ? C26 C27 C28 C23 -0.3(6) . . . . ? C26 C27 C28 P2 169.8(3) . . . . ? C27 C28 P2 C29 88.7(3) . . . . ? C27 C28 P2 C36 -20.6(4) . . . . ? C27 C28 P2 Pd2 -150.7(3) . . . . ? C28 C23 C24 C25 0.1(6) . . . . ? C29 C30 C31 C32 -0.8(7) . . . . ? C30 C29 C34 C33 -1.1(6) . . . . ? C30 C29 C34 C35 178.5(4) . . . . ? C30 C29 P2 C28 -8.7(4) . . . . ? C30 C29 P2 C36 100.5(3) . . . . ? C30 C29 P2 Pd2 -121.2(3) . . . . ? C30 C31 C32 C33 -0.1(7) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C32 C33 C34 C29 0.1(6) . . . . ? C32 C33 C34 C35 -179.4(4) . . . . ? C34 C29 C30 C31 1.5(6) . . . . ? C34 C29 P2 C28 170.0(3) . . . . ? C34 C29 P2 C36 -80.7(3) . . . . ? C34 C29 P2 Pd2 57.6(3) . . . . ? C36 C37 C38 C39 -2.3(6) . . . . ? C37 C36 C41 C40 2.0(5) . . . . ? C37 C36 C41 C42 -176.9(4) . . . . ? C37 C36 P2 C28 100.0(3) . . . . ? C37 C36 P2 C29 -12.3(3) . . . . ? C37 C36 P2 Pd2 -145.0(2) . . . . ? C37 C38 C39 C40 2.3(7) . . . . ? C38 C39 C40 C41 -0.2(7) . . . . ? C39 C40 C41 C36 -2.0(6) . . . . ? C39 C40 C41 C42 177.0(4) . . . . ? C41 C36 C37 C38 0.1(6) . . . . ? C41 C36 P2 C28 -76.8(3) . . . . ? C41 C36 P2 C29 170.9(3) . . . . ? C41 C36 P2 Pd2 38.2(4) . . . . ? C43 C44 C45 C46 -179.0(4) . . . . ? C43 C44 C49 C48 179.5(4) . . . . ? C43 C44 C49 P3 -1.7(4) . . . . ? C44 C45 C46 C47 -1.8(7) . . . . ? C44 C49 P3 C50 -148.0(3) . . . . ? C44 C49 P3 C57 102.0(3) . . . . ? C44 C49 P3 Pd3 -22.6(3) . . . . ? C45 C44 C49 C48 -1.1(6) . . . . ? C45 C44 C49 P3 177.7(3) . . . . ? C45 C46 C47 C48 1.5(7) . . . . ? C46 C47 C48 C49 -0.9(7) . . . . ? C47 C48 C49 C44 0.8(7) . . . . ? C47 C48 C49 P3 -177.8(4) . . . . ? C48 C49 P3 C50 30.6(4) . . . . ? C48 C49 P3 C57 -79.3(4) . . . . ? C48 C49 P3 Pd3 156.1(4) . . . . ? C49 C44 C45 C46 1.6(6) . . . . ? C50 C51 C52 C53 -0.7(6) . . . . ? C51 C50 C55 C54 0.5(5) . . . . ? C51 C50 C55 C56 179.9(4) . . . . ? C51 C50 P3 C49 -118.0(3) . . . . ? C51 C50 P3 C57 -6.9(3) . . . . ? C51 C50 P3 Pd3 128.9(3) . . . . ? C51 C52 C53 C54 0.0(6) . . . . ? C52 C53 C54 C55 1.0(6) . . . . ? C53 C54 C55 C50 -1.2(6) . . . . ? C53 C54 C55 C56 179.3(4) . . . . ? C55 C50 C51 C52 0.4(5) . . . . ? C55 C50 P3 C49 64.5(3) . . . . ? C55 C50 P3 C57 175.6(3) . . . . ? C55 C50 P3 Pd3 -48.6(3) . . . . ? C57 C58 C59 C60 -0.7(7) . . . . ? C58 C57 C62 C61 1.7(6) . . . . ? C58 C57 C62 C63 -178.9(4) . . . . ? C58 C57 P3 C49 9.2(4) . . . . ? C58 C57 P3 C50 -102.1(3) . . . . ? C58 C57 P3 Pd3 121.8(3) . . . . ? C58 C59 C60 C61 1.6(7) . . . . ? C59 C60 C61 C62 -0.8(7) . . . . ? C60 C61 C62 C57 -0.9(6) . . . . ? C60 C61 C62 C63 179.6(4) . . . . ? C62 C57 C58 C59 -0.9(6) . . . . ? C62 C57 P3 C49 -169.0(3) . . . . ? C62 C57 P3 C50 79.7(3) . . . . ? C62 C57 P3 Pd3 -56.4(3) . . . . ? C64 C65 C66 C67 177.4(4) . . . . ? C64 C65 C70 C69 -177.5(4) . . . . ? C64 C65 C70 P4 -1.5(4) . . . . ? C65 C66 C67 C68 -0.7(7) . . . . ? C65 C70 P4 C71 -145.8(3) . . . . ? C65 C70 P4 C78 102.4(3) . . . . ? C65 C70 P4 Pd4 -15.0(3) . . . . ? C66 C65 C70 C69 1.1(6) . . . . ? C66 C65 C70 P4 177.0(3) . . . . ? C66 C67 C68 C69 2.5(7) . . . . ? C67 C68 C69 C70 -2.5(7) . . . . ? C68 C69 C70 C65 0.7(6) . . . . ? C68 C69 C70 P4 -174.7(3) . . . . ? C69 C70 P4 C71 29.9(4) . . . . ? C69 C70 P4 C78 -81.9(4) . . . . ? C69 C70 P4 Pd4 160.8(3) . . . . ? C70 C65 C66 C67 -1.1(6) . . . . ? C71 C72 C73 C74 1.0(6) . . . . ? C72 C71 C76 C75 -2.1(6) . . . . ? C72 C71 C76 C77 176.8(4) . . . . ? C72 C71 P4 C70 -94.4(3) . . . . ? C72 C71 P4 C78 17.4(4) . . . . ? C72 C71 P4 Pd4 148.6(3) . . . . ? C72 C73 C74 C75 -1.4(6) . . . . ? C73 C74 C75 C76 0.1(6) . . . . ? C74 C75 C76 C71 1.7(6) . . . . ? C74 C75 C76 C77 -177.3(4) . . . . ? C76 C71 C72 C73 0.8(6) . . . . ? C76 C71 P4 C70 78.1(3) . . . . ? C76 C71 P4 C78 -170.1(3) . . . . ? C76 C71 P4 Pd4 -38.8(4) . . . . ? C78 C79 C80 C81 -0.5(6) . . . . ? C79 C78 C83 C82 1.3(5) . . . . ? C79 C78 C83 C84 -179.1(4) . . . . ? C79 C78 P4 C70 -13.1(3) . . . . ? C79 C78 P4 C71 -121.3(3) . . . . ? C79 C78 P4 Pd4 100.0(3) . . . . ? C79 C80 C81 C82 0.5(6) . . . . ? C80 C81 C82 C83 0.4(7) . . . . ? C81 C82 C83 C78 -1.3(6) . . . . ? C81 C82 C83 C84 179.1(4) . . . . ? C83 C78 C79 C80 -0.4(6) . . . . ? C83 C78 P4 C70 175.6(3) . . . . ? C83 C78 P4 C71 67.4(3) . . . . ? C83 C78 P4 Pd4 -71.2(3) . . . . ? P1 C8 C9 C10 172.7(4) . . . . ? P1 C8 C13 C12 -173.8(3) . . . . ? P1 C8 C13 C14 6.4(6) . . . . ? P1 C15 C16 C17 -173.6(4) . . . . ? P1 C15 C20 C19 172.6(3) . . . . ? P1 C15 C20 C21 -10.2(6) . . . . ? P2 C29 C30 C31 -179.7(3) . . . . ? P2 C29 C34 C33 -179.9(3) . . . . ? P2 C29 C34 C35 -0.3(5) . . . . ? P2 C36 C37 C38 -176.7(3) . . . . ? P2 C36 C41 C40 178.8(3) . . . . ? P2 C36 C41 C42 -0.1(5) . . . . ? P3 C50 C51 C52 -177.1(3) . . . . ? P3 C50 C55 C54 178.0(3) . . . . ? P3 C50 C55 C56 -2.6(5) . . . . ? P3 C57 C58 C59 -179.1(3) . . . . ? P3 C57 C62 C61 179.8(3) . . . . ? P3 C57 C62 C63 -0.7(5) . . . . ? P4 C71 C72 C73 173.4(3) . . . . ? P4 C71 C76 C75 -174.6(3) . . . . ? P4 C71 C76 C77 4.3(5) . . . . ? P4 C78 C79 C80 -171.8(3) . . . . ? P4 C78 C83 C82 172.4(3) . . . . ? P4 C78 C83 C84 -8.0(5) . . . . ? Pd1 C1 C2 C3 169.6(3) . . . . ? Pd1 C1 C2 C7 -9.5(5) . . . . ? Pd2 C22 C23 C24 141.9(3) . . . . ? Pd2 C22 C23 C28 -36.0(4) . . . . ? Pd3 C43 C44 C45 -150.1(3) . . . . ? Pd3 C43 C44 C49 29.2(4) . . . . ? Pd4 C64 C65 C66 -158.2(3) . . . . ? Pd4 C64 C65 C70 20.2(5) . . . . ? 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 0.0140 0.0013 0.9958 0.0494 -0.0565 0.0178 -0.0140 -0.0013 -0.9958 -0.0494 0.0565 -0.0178 -0.0024 1.0029 -0.0192 0.0352 0.0343 0.1069 0.0024 -1.0029 0.0192 -0.0352 -0.0343 -0.1069 0.9978 1.0101 -0.0625 0.1404 0.1053 0.1129 -1.0026 0.9957 0.0240 -0.0700 -0.0367 0.1009 -1.0002 -0.0072 0.0433 -0.1052 -0.0710 -0.0060 1.0002 0.0072 -0.0433 0.1052 0.0710 0.0060 2.0405 -4.9975 2.0014 0.1331 -0.1427 -0.4870