#------------------------------------------------------------------------------ #$Date: 2019-11-17 10:44:50 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229411 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045404.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_7045404 loop_ _publ_author_name 'L\'opez-Vidal, E M' 'Prokofjevs, A.' 'Gibbs-Hall, I C' 'Dale, E. J.' 'Quintela, J. M.' 'Peinador, C.' _publ_section_title ; Studies towards the synthesis of Pd(ii)-containing [2] and [3]catenanes in aqueous media. ; _journal_issue 8 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2492 _journal_page_last 2496 _journal_paper_doi 10.1039/c7dt04792d _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C92 H108 Cl4 N8 O16 Pd2, 2(C36 H32 N4), 2(Cl4 Zn), 10(H2 O), 8(Cl)' _chemical_formula_sum 'C164 H192 Cl20 N16 O26 Pd2 Zn2' _chemical_formula_weight 3855.86 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2015-08-05 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2017-12-19 deposited with the CCDC. 2018-01-18 downloaded from the CCDC. ; _cell_angle_alpha 91.369(2) _cell_angle_beta 90.147(2) _cell_angle_gamma 97.5953(19) _cell_formula_units_Z 1 _cell_length_a 12.2761(4) _cell_length_b 19.5771(7) _cell_length_c 20.4123(8) _cell_measurement_reflns_used 9960 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.331 _cell_measurement_theta_min 2.301 _cell_volume 4861.2(3) _computing_cell_refinement 'SAINT V8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 V2014.11-0 (Bruker, 2014)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.02 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'QuazarTM optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.0932 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 58662 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.519 _diffrn_reflns_theta_min 0.998 _diffrn_source microsource _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6260 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1037 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.8398. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.317 _exptl_crystal_description needle _exptl_crystal_F_000 1988 _exptl_crystal_size_max 0.311 _exptl_crystal_size_mid 0.033 _exptl_crystal_size_min 0.01 _refine_diff_density_max 2.301 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.124 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1051 _refine_ls_number_reflns 20008 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0710 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1879 _refine_ls_wR_factor_ref 0.2055 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12458 _reflns_number_total 20008 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt04792d2.cif _cod_data_source_block cx0532 _cod_depositor_comments 'Adding full bibliography for 7045404--7045405.cif.' _cod_database_code 7045404 _shelxl_version_number 2013-4 _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 0.992 _shelx_estimated_absorpt_t_min 0.797 _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 O(H,H) groups 2.a Free rotating group: O1S(H1SA,H1SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB), O4S(H4SA,H4SB), O5S(H5SA,H5SB) 2.b Secondary CH2 refined with riding coordinates: C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A, H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C11(H11A,H11B), C18(H18A,H18B), C29(H29A, H29B), C36(H36A,H36B) 2.c Aromatic/amide H refined with riding coordinates: C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C73(H73), C74(H74), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C82(H82), C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35) ; _smtbx_masks_special_details ; Total solvent accessible volume / cell = 836.3 Ang^3^ [17.0%] Total electron count / cell = 302.5 The solvent masking procedure as implemented in Olex2 was used to remove the electronic contribution of solvent molecules from the refinement. As the exact solvent content is not known, only the atoms used in the refinement model are reported in the formula here. ; _shelx_res_file ; TITL cx0532_a.res in P-1 REM Old TITL cx0532 in P-1 REM SHELXT solution in P-1 REM R1 0.231, Rweak 0.014, Alpha 0.074, Orientation as input REM Formula found by SHELXT: C78 N28 O5S Cl10 Pd CELL 0.71073 12.2761 19.5771 20.4123 91.3686 90.1471 97.5953 ZERR 1 0.0004 0.0007 0.0008 0.002 0.002 0.0019 LATT 1 SFAC C H Cl N O Pd Zn UNIT 164 192 20 16 26 2 2 L.S. 10 PLAN 20 SIZE 0.01 0.033 0.311 TEMP -173.13 BOND $H acta wpdb -2 MORE -1 CONF fmap 2 acta 52 OMIT -1 6 1 OMIT 0 0 4 REM REM REM WGHT 0.115100 FVAR 0.07413 PD1 6 0.784859 0.119733 0.019092 11.00000 0.02287 0.02293 = 0.03090 -0.00549 -0.00989 0.00663 CL1 3 0.831105 0.224280 -0.028331 11.00000 0.02426 0.02407 = 0.02891 -0.00657 -0.00002 0.00569 CL2 3 0.745021 0.015795 0.071231 11.00000 0.04272 0.03077 = 0.04703 0.00666 -0.02021 0.00361 O1 5 1.040451 0.355283 0.483841 11.00000 0.03844 0.04954 = 0.05958 -0.01749 0.00236 0.00159 O2 5 0.812190 0.372222 0.461917 11.00000 0.02255 0.05410 = 0.04473 0.01255 0.00258 0.00606 O3 5 0.626748 0.395817 0.377886 11.00000 0.02411 0.03501 = 0.05201 0.00622 0.00723 0.00442 O4 5 0.615499 0.477745 0.261476 11.00000 0.02343 0.02303 = 0.05048 0.00673 0.00304 -0.00097 O5 5 0.829315 0.739428 0.145245 11.00000 0.01877 0.01859 = 0.03499 0.00307 0.00016 0.00459 O6 5 0.960660 0.879054 0.161397 11.00000 0.02297 0.01773 = 0.03902 0.00484 -0.00304 0.00168 O7 5 0.955041 0.984976 0.265125 11.00000 0.02027 0.02203 = 0.04604 -0.00755 -0.00438 0.00158 O8 5 0.836106 1.055399 0.361934 11.00000 0.03087 0.03109 = 0.04015 0.00042 -0.00923 0.00593 N5 4 0.860586 0.158606 0.101005 11.00000 0.01687 0.03311 = 0.03510 -0.00051 -0.00517 0.00445 N6 4 1.142089 0.277274 0.389637 11.00000 0.02711 0.03339 = 0.02717 -0.00681 -0.00776 0.00035 N7 4 0.598828 1.056888 0.339053 11.00000 0.03094 0.03205 = 0.03409 -0.00786 -0.00920 0.01020 N8 4 0.292847 0.921356 0.064291 11.00000 0.02364 0.02091 = 0.04121 -0.00538 -0.00935 0.01284 C37 1 0.803872 0.169973 0.155638 11.00000 0.02234 0.02135 = 0.03758 -0.00118 -0.00190 0.00770 AFIX 43 H37 2 0.725846 0.162266 0.154270 11.00000 -1.20000 AFIX 0 C38 1 0.856055 0.192465 0.213392 11.00000 0.01917 0.02156 = 0.02908 -0.00212 -0.00381 0.00272 AFIX 43 H38 2 0.814110 0.199408 0.251446 11.00000 -1.20000 AFIX 0 C39 1 0.970468 0.205093 0.216162 11.00000 0.02561 0.02155 = 0.02756 -0.00199 -0.00392 0.00327 C40 1 1.027656 0.193201 0.159112 11.00000 0.01482 0.05729 = 0.03200 -0.01370 -0.00248 0.00174 AFIX 43 H40 2 1.105691 0.201006 0.158742 11.00000 -1.20000 AFIX 0 C41 1 0.970395 0.170194 0.103668 11.00000 0.02372 0.07288 = 0.03584 -0.01506 0.00138 0.00141 AFIX 43 H41 2 1.010467 0.162028 0.065150 11.00000 -1.20000 AFIX 0 C42 1 1.029054 0.230194 0.276731 11.00000 0.02101 0.02124 = 0.03393 -0.00342 -0.00761 0.00612 C43 1 1.130926 0.272111 0.274259 11.00000 0.02736 0.02782 = 0.02782 0.00081 -0.00178 -0.00036 AFIX 43 H43 2 1.162784 0.284742 0.233202 11.00000 -1.20000 AFIX 0 C44 1 1.184320 0.294777 0.331568 11.00000 0.02106 0.02762 = 0.04436 -0.00511 -0.00547 -0.00475 AFIX 43 H44 2 1.252842 0.323555 0.329633 11.00000 -1.20000 AFIX 0 C45 1 1.045447 0.235121 0.394399 11.00000 0.02942 0.03638 = 0.02939 0.00099 -0.00149 -0.00212 AFIX 43 H45 2 1.017692 0.221414 0.436146 11.00000 -1.20000 AFIX 0 C46 1 0.987767 0.212308 0.338132 11.00000 0.02583 0.02936 = 0.03428 -0.00577 -0.00693 -0.00171 AFIX 43 H46 2 0.918994 0.184029 0.341486 11.00000 -1.20000 AFIX 0 C47 1 1.198517 0.306184 0.449595 11.00000 0.04283 0.04982 = 0.03164 -0.00524 -0.00994 -0.00894 AFIX 23 H47A 2 1.278725 0.315294 0.442146 11.00000 -1.20000 H47B 2 1.184963 0.273273 0.485673 11.00000 -1.20000 AFIX 0 C48 1 1.153789 0.372857 0.467302 11.00000 0.03005 0.04676 = 0.03920 -0.01546 -0.00441 -0.00966 AFIX 23 H48A 2 1.195040 0.396394 0.504994 11.00000 -1.20000 H48B 2 1.161023 0.404150 0.429720 11.00000 -1.20000 AFIX 0 C49 1 0.993579 0.413685 0.500913 11.00000 0.03323 0.04039 = 0.04402 -0.01193 -0.00720 0.00663 AFIX 23 H49A 2 1.000421 0.445629 0.463832 11.00000 -1.20000 H49B 2 1.033944 0.437426 0.538815 11.00000 -1.20000 AFIX 0 C50 1 0.874561 0.396537 0.518233 11.00000 0.06681 0.04328 = 0.03798 0.00064 0.00135 0.01706 AFIX 23 H50A 2 0.866480 0.360771 0.551995 11.00000 -1.20000 H50B 2 0.846748 0.438131 0.536622 11.00000 -1.20000 AFIX 0 C51 1 0.700161 0.362416 0.479247 11.00000 0.03522 0.08648 = 0.04935 0.00815 0.01434 0.00372 AFIX 23 H51A 2 0.681080 0.405372 0.500181 11.00000 -1.20000 H51B 2 0.688009 0.325527 0.511793 11.00000 -1.20000 AFIX 0 C52 1 0.627943 0.343980 0.423454 11.00000 0.04377 0.07471 = 0.03897 0.01352 0.00590 -0.02033 AFIX 23 H52A 2 0.650679 0.302814 0.400992 11.00000 -1.20000 H52B 2 0.552235 0.331142 0.439654 11.00000 -1.20000 AFIX 0 C53 1 0.542257 0.386829 0.332895 11.00000 0.02330 0.04305 = 0.05876 0.00460 0.00095 -0.00935 AFIX 23 H53A 2 0.474063 0.366679 0.354837 11.00000 -1.20000 H53B 2 0.559342 0.353793 0.298146 11.00000 -1.20000 AFIX 0 C54 1 0.523518 0.451695 0.302743 11.00000 0.01940 0.03074 = 0.09552 0.00649 0.01010 -0.00064 AFIX 23 H54A 2 0.455411 0.443942 0.276006 11.00000 -1.20000 H54B 2 0.513603 0.486413 0.337525 11.00000 -1.20000 AFIX 0 C55 1 0.617305 0.544343 0.243894 11.00000 0.01716 0.01762 = 0.03402 0.00375 -0.00205 0.00133 C56 1 0.538820 0.584997 0.260186 11.00000 0.01525 0.02646 = 0.03922 -0.00300 0.00337 0.00187 AFIX 43 H56 2 0.475105 0.566088 0.283166 11.00000 -1.20000 AFIX 0 C57 1 0.552071 0.655540 0.242890 11.00000 0.02340 0.02679 = 0.02919 -0.00374 -0.00098 0.01052 AFIX 43 H57 2 0.496876 0.683268 0.254570 11.00000 -1.20000 AFIX 0 C58 1 0.643174 0.684292 0.209624 11.00000 0.02016 0.02137 = 0.02946 -0.00058 -0.00382 0.00034 AFIX 43 H58 2 0.651242 0.731530 0.198504 11.00000 -1.20000 AFIX 0 C59 1 0.724688 0.642802 0.192151 11.00000 0.01489 0.01764 = 0.01978 -0.00519 -0.00267 0.00412 C60 1 0.822531 0.669989 0.158447 11.00000 0.01951 0.02120 = 0.02623 -0.00054 -0.00206 0.00297 C61 1 0.899752 0.629323 0.141478 11.00000 0.01719 0.02394 = 0.02601 0.00023 0.00264 0.00725 AFIX 43 H61 2 0.963817 0.648235 0.118824 11.00000 -1.20000 AFIX 0 C62 1 0.885194 0.559622 0.157279 11.00000 0.02458 0.02165 = 0.02751 -0.00668 -0.00288 0.01370 AFIX 43 H62 2 0.939646 0.531600 0.144930 11.00000 -1.20000 AFIX 0 C63 1 0.793221 0.530678 0.190489 11.00000 0.02086 0.01665 = 0.02674 -0.00595 -0.00651 0.00519 AFIX 43 H63 2 0.784633 0.483340 0.201276 11.00000 -1.20000 AFIX 0 C64 1 0.713766 0.571685 0.207811 11.00000 0.01837 0.02188 = 0.02564 -0.00194 -0.00427 -0.00006 C65 1 0.924583 0.767700 0.108586 11.00000 0.02292 0.02177 = 0.03149 -0.00046 0.00262 0.00609 AFIX 23 H65A 2 0.922968 0.745373 0.064500 11.00000 -1.20000 H65B 2 0.992327 0.758640 0.131360 11.00000 -1.20000 AFIX 0 C66 1 0.924782 0.843294 0.102389 11.00000 0.01860 0.02653 = 0.03239 0.00636 -0.00330 0.00489 AFIX 23 H66A 2 0.974007 0.860069 0.066201 11.00000 -1.20000 H66B 2 0.849686 0.852811 0.091524 11.00000 -1.20000 AFIX 0 C67 1 0.980547 0.951715 0.153218 11.00000 0.02449 0.02105 = 0.05213 0.00346 -0.00070 0.00191 AFIX 23 H67A 2 0.910215 0.969288 0.143989 11.00000 -1.20000 H67B 2 1.029533 0.961923 0.115254 11.00000 -1.20000 AFIX 0 C68 1 1.031941 0.987234 0.212651 11.00000 0.01838 0.02571 = 0.06278 0.00040 -0.00500 -0.00150 AFIX 23 H68A 2 1.095942 0.964785 0.225956 11.00000 -1.20000 H68B 2 1.058567 1.035840 0.202787 11.00000 -1.20000 AFIX 0 C69 1 1.003642 1.024128 0.320330 11.00000 0.02545 0.03943 = 0.06185 -0.01716 -0.01717 0.00517 AFIX 23 H69A 2 1.022849 1.072838 0.308045 11.00000 -1.20000 H69B 2 1.072302 1.006257 0.332927 11.00000 -1.20000 AFIX 0 C70 1 0.927254 1.020481 0.377750 11.00000 0.03540 0.03738 = 0.04308 -0.00600 -0.01891 0.00528 AFIX 23 H70A 2 0.901318 0.971759 0.387521 11.00000 -1.20000 H70B 2 0.966063 1.042513 0.416937 11.00000 -1.20000 AFIX 0 C71 1 0.759033 1.052368 0.412795 11.00000 0.03629 0.03267 = 0.03217 -0.00588 -0.00890 0.00319 AFIX 23 H71A 2 0.794895 1.073183 0.453360 11.00000 -1.20000 H71B 2 0.731036 1.003632 0.421299 11.00000 -1.20000 AFIX 0 C72 1 0.664150 1.090610 0.394730 11.00000 0.03544 0.03868 = 0.03171 -0.00862 -0.01625 0.00251 AFIX 23 H72A 2 0.615762 1.093051 0.433207 11.00000 -1.20000 H72B 2 0.693214 1.138352 0.383102 11.00000 -1.20000 AFIX 0 C73 1 0.646635 1.053573 0.279617 11.00000 0.03034 0.02071 = 0.04004 -0.00092 -0.00693 0.00531 AFIX 43 H73 2 0.722587 1.069566 0.274651 11.00000 -1.20000 AFIX 0 C74 1 0.584881 1.026988 0.226508 11.00000 0.03526 0.02199 = 0.03143 -0.00672 -0.00818 0.00678 AFIX 43 H74 2 0.618607 1.023912 0.184896 11.00000 -1.20000 AFIX 0 C75 1 0.472941 1.004470 0.233272 11.00000 0.03994 0.02655 = 0.04242 -0.01099 -0.01616 0.01992 C76 1 0.427378 1.008340 0.294745 11.00000 0.02317 0.05182 = 0.04751 -0.02025 -0.00572 0.01002 AFIX 43 H76 2 0.351889 0.992144 0.301349 11.00000 -1.20000 AFIX 0 C77 1 0.491608 1.035577 0.345811 11.00000 0.03439 0.05006 = 0.04643 -0.01605 -0.00956 0.01479 AFIX 43 H77 2 0.459114 1.039574 0.387681 11.00000 -1.20000 AFIX 0 C78 1 0.407761 0.976043 0.174720 11.00000 0.03074 0.02435 = 0.04170 -0.01197 -0.01609 0.01601 C79 1 0.445101 0.992920 0.112054 11.00000 0.03034 0.02704 = 0.04530 0.00285 -0.01996 0.00136 AFIX 43 H79 2 0.510600 1.023866 0.106292 11.00000 -1.20000 AFIX 0 C80 1 0.385645 0.964070 0.058295 11.00000 0.03992 0.02799 = 0.03537 0.00026 -0.01218 0.00117 AFIX 43 H80 2 0.412051 0.975169 0.015633 11.00000 -1.20000 AFIX 0 C81 1 0.253498 0.904447 0.124739 11.00000 0.02360 0.02678 = 0.03932 -0.01115 -0.01078 0.01545 AFIX 43 H81 2 0.186886 0.874142 0.128926 11.00000 -1.20000 AFIX 0 C82 1 0.310595 0.931438 0.180549 11.00000 0.02481 0.03052 = 0.04140 -0.01245 -0.00539 0.01674 AFIX 43 H82 2 0.283039 0.919323 0.222742 11.00000 -1.20000 AFIX 0 N1 4 0.772287 0.817443 0.325111 11.00000 0.03402 0.01769 = 0.03309 -0.00586 -0.00846 0.00454 N2 4 0.934110 0.488753 0.330678 11.00000 0.02529 0.02114 = 0.02695 0.00259 -0.00424 0.00387 N3 4 0.672126 0.402733 0.069599 11.00000 0.02445 0.01790 = 0.02512 -0.00127 -0.00401 0.00279 N4 4 0.471276 0.721118 0.076306 11.00000 0.01817 0.02112 = 0.04105 -0.00661 -0.01077 0.01099 C1 1 0.866083 0.805956 0.294431 11.00000 0.02426 0.02382 = 0.03307 -0.00250 -0.00141 -0.00391 AFIX 43 H1 2 0.904632 0.841174 0.268927 11.00000 -1.20000 AFIX 0 C2 1 0.906368 0.743814 0.299725 11.00000 0.01847 0.03082 = 0.02920 -0.00132 -0.00092 0.00106 AFIX 43 H2 2 0.972601 0.736646 0.278222 11.00000 -1.20000 AFIX 0 C3 1 0.849375 0.690748 0.337064 11.00000 0.02697 0.01791 = 0.02434 -0.00628 -0.00481 -0.00146 C4 1 0.754478 0.705877 0.370217 11.00000 0.03786 0.02763 = 0.02678 0.00021 -0.00210 0.00512 AFIX 43 H4 2 0.715123 0.672261 0.397113 11.00000 -1.20000 AFIX 0 C5 1 0.718273 0.769604 0.363763 11.00000 0.03647 0.02406 = 0.03647 -0.00261 -0.00037 0.00280 AFIX 43 H5 2 0.654872 0.779562 0.386799 11.00000 -1.20000 AFIX 0 C6 1 0.880835 0.621218 0.337476 11.00000 0.02415 0.02135 = 0.02156 -0.00373 -0.00651 0.00419 C7 1 0.983223 0.607562 0.315138 11.00000 0.01985 0.02396 = 0.04416 0.00428 -0.00728 -0.00391 AFIX 43 H7 2 1.036310 0.644323 0.301847 11.00000 -1.20000 AFIX 0 C8 1 1.007715 0.540154 0.312293 11.00000 0.01924 0.02620 = 0.03569 0.00350 -0.00590 0.00132 AFIX 43 H8 2 1.077553 0.531025 0.297092 11.00000 -1.20000 AFIX 0 C9 1 0.834606 0.499159 0.353949 11.00000 0.02154 0.02212 = 0.03186 0.00220 -0.00224 0.00113 AFIX 43 H9 2 0.783879 0.461313 0.367545 11.00000 -1.20000 AFIX 0 C10 1 0.807177 0.565562 0.357812 11.00000 0.01853 0.02516 = 0.02589 -0.00461 -0.00111 0.00039 AFIX 43 H10 2 0.737504 0.573193 0.374481 11.00000 -1.20000 AFIX 0 C11 1 0.956279 0.414556 0.321593 11.00000 0.02586 0.02076 = 0.03884 0.00294 -0.00134 0.00995 AFIX 23 H11A 2 1.036469 0.412939 0.319606 11.00000 -1.20000 H11B 2 0.926536 0.387144 0.359206 11.00000 -1.20000 AFIX 0 C12 1 0.902143 0.384538 0.258728 11.00000 0.02624 0.01493 = 0.03166 0.00466 -0.00283 0.00926 C13 1 0.958830 0.391914 0.200487 11.00000 0.01864 0.03052 = 0.02951 0.00196 0.00244 0.00846 AFIX 43 H13 2 1.034926 0.409064 0.200418 11.00000 -1.20000 AFIX 0 C14 1 0.903397 0.374004 0.142182 11.00000 0.02183 0.02248 = 0.03330 0.00128 0.00825 0.01075 AFIX 43 H14 2 0.941725 0.379157 0.101857 11.00000 -1.20000 AFIX 0 C15 1 0.792747 0.348677 0.142046 11.00000 0.02772 0.01126 = 0.03543 -0.00343 -0.00254 0.00647 C16 1 0.738679 0.336868 0.201303 11.00000 0.01536 0.01397 = 0.03180 -0.00206 0.00112 0.00177 AFIX 43 H16 2 0.663934 0.316712 0.202011 11.00000 -1.20000 AFIX 0 C17 1 0.795239 0.354877 0.259244 11.00000 0.02784 0.01379 = 0.03324 0.00115 0.00294 0.00685 AFIX 43 H17 2 0.759071 0.346454 0.299912 11.00000 -1.20000 AFIX 0 C18 1 0.726449 0.339569 0.078655 11.00000 0.02670 0.01607 = 0.03018 -0.00246 0.00147 0.00819 AFIX 23 H18A 2 0.775418 0.332998 0.041215 11.00000 -1.20000 H18B 2 0.670302 0.298461 0.080878 11.00000 -1.20000 AFIX 0 C19 1 0.573056 0.406812 0.097039 11.00000 0.01470 0.02241 = 0.03371 -0.00150 0.00027 -0.00106 AFIX 43 H19 2 0.534690 0.367798 0.117595 11.00000 -1.20000 AFIX 0 C20 1 0.527617 0.467356 0.095272 11.00000 0.01853 0.02287 = 0.02396 -0.00178 -0.00347 0.00294 AFIX 43 H20 2 0.457840 0.469806 0.114545 11.00000 -1.20000 AFIX 0 C21 1 0.583776 0.525904 0.065061 11.00000 0.01572 0.01839 = 0.02148 -0.00461 -0.00270 0.00122 C22 1 0.684576 0.517772 0.036045 11.00000 0.01962 0.02840 = 0.02620 0.00002 -0.00122 0.00135 AFIX 43 H22 2 0.723900 0.555179 0.013622 11.00000 -1.20000 AFIX 0 C23 1 0.727719 0.456564 0.039421 11.00000 0.02068 0.02414 = 0.02207 -0.00320 0.00421 0.00178 AFIX 43 H23 2 0.797097 0.452413 0.020320 11.00000 -1.20000 AFIX 0 C24 1 0.542710 0.593209 0.065873 11.00000 0.01779 0.02833 = 0.01984 -0.00654 -0.00712 0.00610 C25 1 0.442039 0.602433 0.096195 11.00000 0.01345 0.02131 = 0.03856 -0.00414 -0.00436 0.00270 AFIX 43 H25 2 0.395867 0.563883 0.112569 11.00000 -1.20000 AFIX 0 C26 1 0.411223 0.667069 0.101910 11.00000 0.01680 0.02759 = 0.04694 -0.00665 -0.00430 0.00470 AFIX 43 H26 2 0.345661 0.673271 0.124622 11.00000 -1.20000 AFIX 0 C27 1 0.564878 0.713229 0.042194 11.00000 0.03399 0.02236 = 0.03811 0.00362 -0.00844 0.00802 AFIX 43 H27 2 0.605199 0.751654 0.021761 11.00000 -1.20000 AFIX 0 C28 1 0.599737 0.650701 0.037667 11.00000 0.02183 0.02689 = 0.02903 0.00029 0.00010 0.00737 AFIX 43 H28 2 0.665395 0.646059 0.014414 11.00000 -1.20000 AFIX 0 C29 1 0.442510 0.792279 0.088791 11.00000 0.02453 0.02449 = 0.05418 -0.00722 -0.00440 0.01715 AFIX 23 H29A 2 0.363128 0.790298 0.098291 11.00000 -1.20000 H29B 2 0.459410 0.820798 0.049787 11.00000 -1.20000 AFIX 0 C30 1 0.510111 0.823256 0.147111 11.00000 0.02020 0.01770 = 0.04597 -0.00091 -0.00047 0.01410 C31 1 0.613895 0.857955 0.138422 11.00000 0.02430 0.02193 = 0.03398 0.00138 -0.00080 0.01011 AFIX 43 H31 2 0.639251 0.868069 0.095351 11.00000 -1.20000 AFIX 0 C32 1 0.682420 0.878500 0.191908 11.00000 0.02274 0.01717 = 0.05007 0.00180 0.00097 0.00338 AFIX 43 H32 2 0.754583 0.901361 0.185210 11.00000 -1.20000 AFIX 0 C33 1 0.644459 0.865314 0.255104 11.00000 0.02472 0.01593 = 0.04548 -0.00434 0.00130 0.00424 C34 1 0.536937 0.834494 0.263779 11.00000 0.02298 0.02222 = 0.04691 -0.00293 0.00701 0.00715 AFIX 43 H34 2 0.509249 0.827819 0.306896 11.00000 -1.20000 AFIX 0 C35 1 0.469417 0.813327 0.210468 11.00000 0.01272 0.02601 = 0.05468 -0.00452 0.00090 0.00851 AFIX 43 H35 2 0.396134 0.792262 0.217026 11.00000 -1.20000 AFIX 0 C36 1 0.722051 0.880128 0.311715 11.00000 0.02680 0.01477 = 0.05343 -0.00651 0.00495 0.00561 AFIX 23 H36A 2 0.779899 0.918436 0.301242 11.00000 -1.20000 H36B 2 0.681993 0.893955 0.350849 11.00000 -1.20000 AFIX 0 ZN1 7 0.436991 0.201032 0.184117 11.00000 0.02170 0.02888 = 0.05039 0.00774 -0.00195 0.00385 CL3 3 0.525320 0.180054 0.088852 11.00000 0.02792 0.04162 = 0.04677 0.00690 0.00112 0.00620 CL4 3 0.285277 0.121351 0.193442 11.00000 0.02267 0.03342 = 0.05476 0.00259 -0.00118 0.00044 CL5 3 0.376544 0.305761 0.180103 11.00000 0.03203 0.03740 = 0.09213 0.02588 0.02388 0.01653 CL6 3 0.556892 0.201881 0.269480 11.00000 0.03321 0.02458 = 0.05434 -0.00154 -0.00834 0.00468 AFIX 6 O1S 5 0.251411 0.470260 0.145636 11.00000 0.02080 0.01957 = 0.04902 0.00670 0.00815 -0.00148 H1SA 2 0.241117 0.478404 0.186884 11.00000 -1.50000 H1SB 2 0.290335 0.436575 0.141168 11.00000 -1.50000 AFIX 6 O2S 5 0.025578 0.569026 0.007926 11.00000 0.05144 0.07287 = 0.04177 0.01469 0.02238 0.03574 H2SA 2 -0.023596 0.595382 -0.001317 11.00000 -1.50000 H2SB 2 0.034587 0.568639 0.050001 11.00000 -1.50000 AFIX 6 O3S 5 0.164569 0.588894 0.116492 11.00000 0.02621 0.06714 = 0.09942 -0.01395 0.00472 0.00297 H3SA 2 0.142565 0.618361 0.090135 11.00000 -1.50000 H3SB 2 0.109800 0.557824 0.125572 11.00000 -1.50000 AFIX 6 O4S 5 0.280424 0.632762 0.327315 11.00000 0.07355 0.08582 = 0.07493 0.00539 -0.00073 0.01141 H4SA 2 0.267773 0.619400 0.286942 11.00000 -1.50000 H4SB 2 0.298509 0.677140 0.329234 11.00000 -1.50000 AFIX 6 O5S 5 0.457299 0.705056 0.392001 11.00000 0.08153 0.08727 = 0.07312 -0.00052 0.02728 0.00775 H5SA 2 0.492646 0.723072 0.426336 11.00000 -1.50000 H5SB 2 0.418676 0.734691 0.375803 11.00000 -1.50000 AFIX 0 CL7 3 0.573572 0.592450 0.458818 11.00000 0.07571 0.08763 = 0.10711 -0.01076 0.00380 -0.00256 CL8 3 0.244290 0.467541 0.302954 11.00000 0.03336 0.05246 = 0.06069 0.00478 -0.00049 0.01322 CL9 3 0.184534 0.716377 0.216332 11.00000 0.04061 0.06197 = 0.06141 0.01164 -0.00882 -0.00609 CL10 3 0.150072 0.358789 0.050839 11.00000 0.08265 0.19317 = 0.10833 -0.01008 0.01184 0.02953 HKLF 4 REM cx0532_a.res in P-1 REM R1 = 0.0710 for 12458 Fo > 4sig(Fo) and 0.1108 for all 20008 data REM 1051 parameters refined using 0 restraints END WGHT 0.1154 0.0000 REM Highest difference peak 2.301, deepest hole -1.258, 1-sigma level 0.124 Q1 1 0.9159 0.2820 0.1000 11.00000 0.05 2.30 Q2 1 0.3092 1.0285 0.1014 11.00000 0.05 1.94 Q3 1 0.3484 1.0395 0.0619 11.00000 0.05 1.57 Q4 1 0.1586 0.9518 0.1137 11.00000 0.05 1.07 Q5 1 0.5738 0.3574 0.2664 11.00000 0.05 1.06 Q6 1 1.0317 0.4053 0.4497 11.00000 0.05 1.04 Q7 1 0.4291 1.0346 0.1864 11.00000 0.05 0.92 Q8 1 0.9618 0.3856 0.0559 11.00000 0.05 0.87 Q9 1 0.3974 1.0088 0.0120 11.00000 0.05 0.77 Q10 1 0.7018 0.3171 0.4423 11.00000 0.05 0.74 Q11 1 0.2483 0.6902 0.1887 11.00000 0.05 0.71 Q12 1 0.9156 0.1913 0.3966 11.00000 0.05 0.68 Q13 1 0.5253 0.4278 0.3560 11.00000 0.05 0.67 Q14 1 0.0488 0.5565 0.1294 11.00000 0.05 0.66 Q15 1 0.1141 0.7951 0.2225 11.00000 0.05 0.64 Q16 1 0.2934 0.4808 0.1377 11.00000 0.05 0.63 Q17 1 0.2400 0.4830 0.1720 11.00000 0.05 0.60 Q18 1 0.3194 0.7105 0.3468 11.00000 0.05 0.58 Q19 1 0.3032 0.5501 0.3796 11.00000 0.05 0.57 Q20 1 0.2588 0.6849 0.3597 11.00000 0.05 0.57 ; _shelx_res_checksum 20824 _olex2_date_sample_data_collection 2015-08-04 _olex2_date_sample_submission 2015-07-27 _olex2_submission_original_sample_id cx0532 _olex2_submission_special_instructions 'No special instructions were received' 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 Pd1 Pd 0.78486(3) 0.11973(2) 0.01909(2) 0.02536(12) Uani 1 1 d . Cl1 Cl 0.83111(10) 0.22428(6) -0.02833(6) 0.0256(3) Uani 1 1 d . Cl2 Cl 0.74502(12) 0.01579(7) 0.07123(7) 0.0402(4) Uani 1 1 d . O1 O 1.0405(3) 0.3553(2) 0.4838(2) 0.0499(11) Uani 1 1 d . O2 O 0.8122(3) 0.3722(2) 0.46192(19) 0.0402(10) Uani 1 1 d . O3 O 0.6267(3) 0.39582(19) 0.37789(19) 0.0369(9) Uani 1 1 d . O4 O 0.6155(3) 0.47775(17) 0.26148(18) 0.0326(9) Uani 1 1 d . O5 O 0.8293(3) 0.73943(16) 0.14525(16) 0.0239(7) Uani 1 1 d . O6 O 0.9607(3) 0.87905(16) 0.16140(17) 0.0266(8) Uani 1 1 d . O7 O 0.9550(3) 0.98498(17) 0.26513(18) 0.0297(8) Uani 1 1 d . O8 O 0.8361(3) 1.05540(18) 0.36193(18) 0.0339(9) Uani 1 1 d . N5 N 0.8606(3) 0.1586(2) 0.1010(2) 0.0283(10) Uani 1 1 d . N6 N 1.1421(4) 0.2773(2) 0.3896(2) 0.0297(10) Uani 1 1 d . N7 N 0.5988(4) 1.0569(2) 0.3391(2) 0.0320(10) Uani 1 1 d . N8 N 0.2928(3) 0.9214(2) 0.0643(2) 0.0278(10) Uani 1 1 d . C37 C 0.8039(4) 0.1700(2) 0.1556(3) 0.0267(11) Uani 1 1 d . H37 H 0.7258 0.1623 0.1543 0.032 Uiso 1 1 calc R C38 C 0.8561(4) 0.1925(2) 0.2134(2) 0.0233(11) Uani 1 1 d . H38 H 0.8141 0.1994 0.2514 0.028 Uiso 1 1 calc R C39 C 0.9705(4) 0.2051(2) 0.2162(2) 0.0249(11) Uani 1 1 d . C40 C 1.0277(4) 0.1932(3) 0.1591(3) 0.0352(13) Uani 1 1 d . H40 H 1.1057 0.2010 0.1587 0.042 Uiso 1 1 calc R C41 C 0.9704(5) 0.1702(3) 0.1037(3) 0.0449(16) Uani 1 1 d . H41 H 1.0105 0.1620 0.0651 0.054 Uiso 1 1 calc R C42 C 1.0291(4) 0.2302(2) 0.2767(2) 0.0252(11) Uani 1 1 d . C43 C 1.1309(4) 0.2721(3) 0.2743(3) 0.0280(12) Uani 1 1 d . H43 H 1.1628 0.2847 0.2332 0.034 Uiso 1 1 calc R C44 C 1.1843(4) 0.2948(3) 0.3316(3) 0.0318(13) Uani 1 1 d . H44 H 1.2528 0.3236 0.3296 0.038 Uiso 1 1 calc R C45 C 1.0454(4) 0.2351(3) 0.3944(3) 0.0323(12) Uani 1 1 d . H45 H 1.0177 0.2214 0.4361 0.039 Uiso 1 1 calc R C46 C 0.9878(4) 0.2123(3) 0.3381(3) 0.0304(12) Uani 1 1 d . H46 H 0.9190 0.1840 0.3415 0.037 Uiso 1 1 calc R C47 C 1.1985(5) 0.3062(3) 0.4496(3) 0.0429(15) Uani 1 1 d . H47A H 1.2787 0.3153 0.4421 0.051 Uiso 1 1 calc R H47B H 1.1850 0.2733 0.4857 0.051 Uiso 1 1 calc R C48 C 1.1538(5) 0.3729(3) 0.4673(3) 0.0403(15) Uani 1 1 d . H48A H 1.1950 0.3964 0.5050 0.048 Uiso 1 1 calc R H48B H 1.1610 0.4041 0.4297 0.048 Uiso 1 1 calc R C49 C 0.9936(5) 0.4137(3) 0.5009(3) 0.0393(14) Uani 1 1 d . H49A H 1.0004 0.4456 0.4638 0.047 Uiso 1 1 calc R H49B H 1.0339 0.4374 0.5388 0.047 Uiso 1 1 calc R C50 C 0.8746(6) 0.3965(3) 0.5182(3) 0.0485(16) Uani 1 1 d . H50A H 0.8665 0.3608 0.5520 0.058 Uiso 1 1 calc R H50B H 0.8467 0.4381 0.5366 0.058 Uiso 1 1 calc R C51 C 0.7002(5) 0.3624(4) 0.4792(3) 0.0573(19) Uani 1 1 d . H51A H 0.6811 0.4054 0.5002 0.069 Uiso 1 1 calc R H51B H 0.6880 0.3255 0.5118 0.069 Uiso 1 1 calc R C52 C 0.6279(5) 0.3440(4) 0.4235(3) 0.0548(19) Uani 1 1 d . H52A H 0.6507 0.3028 0.4010 0.066 Uiso 1 1 calc R H52B H 0.5522 0.3311 0.4397 0.066 Uiso 1 1 calc R C53 C 0.5423(5) 0.3868(3) 0.3329(3) 0.0429(15) Uani 1 1 d . H53A H 0.4741 0.3667 0.3548 0.051 Uiso 1 1 calc R H53B H 0.5593 0.3538 0.2981 0.051 Uiso 1 1 calc R C54 C 0.5235(5) 0.4517(3) 0.3027(4) 0.0488(17) Uani 1 1 d . H54A H 0.4554 0.4439 0.2760 0.059 Uiso 1 1 calc R H54B H 0.5136 0.4864 0.3375 0.059 Uiso 1 1 calc R C55 C 0.6173(4) 0.5443(2) 0.2439(2) 0.0230(11) Uani 1 1 d . C56 C 0.5388(4) 0.5850(3) 0.2602(3) 0.0271(11) Uani 1 1 d . H56 H 0.4751 0.5661 0.2832 0.033 Uiso 1 1 calc R C57 C 0.5521(4) 0.6555(3) 0.2429(2) 0.0259(11) Uani 1 1 d . H57 H 0.4969 0.6833 0.2546 0.031 Uiso 1 1 calc R C58 C 0.6432(4) 0.6843(2) 0.2096(2) 0.0239(11) Uani 1 1 d . H58 H 0.6512 0.7315 0.1985 0.029 Uiso 1 1 calc R C59 C 0.7247(4) 0.6428(2) 0.1922(2) 0.0174(10) Uani 1 1 d . C60 C 0.8225(4) 0.6700(2) 0.1584(2) 0.0223(10) Uani 1 1 d . C61 C 0.8998(4) 0.6293(2) 0.1415(2) 0.0220(10) Uani 1 1 d . H61 H 0.9638 0.6482 0.1188 0.026 Uiso 1 1 calc R C62 C 0.8852(4) 0.5596(2) 0.1573(2) 0.0238(11) Uani 1 1 d . H62 H 0.9396 0.5316 0.1449 0.029 Uiso 1 1 calc R C63 C 0.7932(4) 0.5307(2) 0.1905(2) 0.0213(10) Uani 1 1 d . H63 H 0.7846 0.4833 0.2013 0.026 Uiso 1 1 calc R C64 C 0.7138(4) 0.5717(2) 0.2078(2) 0.0223(10) Uani 1 1 d . C65 C 0.9246(4) 0.7677(2) 0.1086(2) 0.0251(11) Uani 1 1 d . H65A H 0.9230 0.7454 0.0645 0.030 Uiso 1 1 calc R H65B H 0.9923 0.7586 0.1314 0.030 Uiso 1 1 calc R C66 C 0.9248(4) 0.8433(2) 0.1024(2) 0.0256(11) Uani 1 1 d . H66A H 0.9740 0.8601 0.0662 0.031 Uiso 1 1 calc R H66B H 0.8497 0.8528 0.0915 0.031 Uiso 1 1 calc R C67 C 0.9805(4) 0.9517(3) 0.1532(3) 0.0326(13) Uani 1 1 d . H67A H 0.9102 0.9693 0.1440 0.039 Uiso 1 1 calc R H67B H 1.0295 0.9619 0.1153 0.039 Uiso 1 1 calc R C68 C 1.0319(4) 0.9872(3) 0.2127(3) 0.0360(14) Uani 1 1 d . H68A H 1.0959 0.9648 0.2260 0.043 Uiso 1 1 calc R H68B H 1.0586 1.0358 0.2028 0.043 Uiso 1 1 calc R C69 C 1.0036(5) 1.0241(3) 0.3203(3) 0.0425(15) Uani 1 1 d . H69A H 1.0228 1.0728 0.3080 0.051 Uiso 1 1 calc R H69B H 1.0723 1.0063 0.3329 0.051 Uiso 1 1 calc R C70 C 0.9273(5) 1.0205(3) 0.3777(3) 0.0387(14) Uani 1 1 d . H70A H 0.9013 0.9718 0.3875 0.046 Uiso 1 1 calc R H70B H 0.9661 1.0425 0.4169 0.046 Uiso 1 1 calc R C71 C 0.7590(5) 1.0524(3) 0.4128(3) 0.0340(13) Uani 1 1 d . H71A H 0.7949 1.0732 0.4534 0.041 Uiso 1 1 calc R H71B H 0.7310 1.0036 0.4213 0.041 Uiso 1 1 calc R C72 C 0.6642(5) 1.0906(3) 0.3947(3) 0.0357(13) Uani 1 1 d . H72A H 0.6158 1.0931 0.4332 0.043 Uiso 1 1 calc R H72B H 0.6932 1.1384 0.3831 0.043 Uiso 1 1 calc R C73 C 0.6466(5) 1.0536(3) 0.2796(3) 0.0302(12) Uani 1 1 d . H73 H 0.7226 1.0696 0.2747 0.036 Uiso 1 1 calc R C74 C 0.5849(4) 1.0270(2) 0.2265(3) 0.0294(12) Uani 1 1 d . H74 H 0.6186 1.0239 0.1849 0.035 Uiso 1 1 calc R C75 C 0.4729(5) 1.0045(3) 0.2333(3) 0.0351(14) Uani 1 1 d . C76 C 0.4274(5) 1.0083(3) 0.2947(3) 0.0407(15) Uani 1 1 d . H76 H 0.3519 0.9921 0.3013 0.049 Uiso 1 1 calc R C77 C 0.4916(5) 1.0356(3) 0.3458(3) 0.0431(15) Uani 1 1 d . H77 H 0.4591 1.0396 0.3877 0.052 Uiso 1 1 calc R C78 C 0.4078(4) 0.9760(3) 0.1747(3) 0.0314(13) Uani 1 1 d . C79 C 0.4451(5) 0.9929(3) 0.1121(3) 0.0344(13) Uani 1 1 d . H79 H 0.5106 1.0239 0.1063 0.041 Uiso 1 1 calc R C80 C 0.3856(5) 0.9641(3) 0.0583(3) 0.0348(13) Uani 1 1 d . H80 H 0.4121 0.9752 0.0156 0.042 Uiso 1 1 calc R C81 C 0.2535(4) 0.9044(3) 0.1247(3) 0.0290(12) Uani 1 1 d . H81 H 0.1869 0.8741 0.1289 0.035 Uiso 1 1 calc R C82 C 0.3106(4) 0.9314(3) 0.1805(3) 0.0313(12) Uani 1 1 d . H82 H 0.2830 0.9193 0.2227 0.038 Uiso 1 1 calc R N1 N 0.7723(4) 0.8174(2) 0.3251(2) 0.0283(10) Uani 1 1 d . N2 N 0.9341(3) 0.4888(2) 0.3307(2) 0.0244(9) Uani 1 1 d . N3 N 0.6721(3) 0.40273(19) 0.06960(19) 0.0225(9) Uani 1 1 d . N4 N 0.4713(3) 0.7211(2) 0.0763(2) 0.0262(10) Uani 1 1 d . C1 C 0.8661(4) 0.8060(3) 0.2944(3) 0.0277(12) Uani 1 1 d . H1 H 0.9046 0.8412 0.2689 0.033 Uiso 1 1 calc R C2 C 0.9064(4) 0.7438(3) 0.2997(2) 0.0264(11) Uani 1 1 d . H2 H 0.9726 0.7366 0.2782 0.032 Uiso 1 1 calc R C3 C 0.8494(4) 0.6907(2) 0.3371(2) 0.0236(11) Uani 1 1 d . C4 C 0.7545(5) 0.7059(3) 0.3702(3) 0.0307(12) Uani 1 1 d . H4 H 0.7151 0.6723 0.3971 0.037 Uiso 1 1 calc R C5 C 0.7183(5) 0.7696(3) 0.3638(3) 0.0325(12) Uani 1 1 d . H5 H 0.6549 0.7796 0.3868 0.039 Uiso 1 1 calc R C6 C 0.8808(4) 0.6212(2) 0.3375(2) 0.0223(10) Uani 1 1 d . C7 C 0.9832(4) 0.6076(3) 0.3151(3) 0.0299(12) Uani 1 1 d . H7 H 1.0363 0.6443 0.3018 0.036 Uiso 1 1 calc R C8 C 1.0077(4) 0.5402(3) 0.3123(3) 0.0272(11) Uani 1 1 d . H8 H 1.0776 0.5310 0.2971 0.033 Uiso 1 1 calc R C9 C 0.8346(4) 0.4992(3) 0.3539(2) 0.0253(11) Uani 1 1 d . H9 H 0.7839 0.4613 0.3675 0.030 Uiso 1 1 calc R C10 C 0.8072(4) 0.5656(2) 0.3578(2) 0.0235(11) Uani 1 1 d . H10 H 0.7375 0.5732 0.3745 0.028 Uiso 1 1 calc R C11 C 0.9563(4) 0.4146(2) 0.3216(3) 0.0278(11) Uani 1 1 d . H11A H 1.0365 0.4129 0.3196 0.033 Uiso 1 1 calc R H11B H 0.9265 0.3871 0.3592 0.033 Uiso 1 1 calc R C12 C 0.9021(4) 0.3845(2) 0.2587(2) 0.0236(11) Uani 1 1 d . C13 C 0.9588(4) 0.3919(3) 0.2005(2) 0.0257(11) Uani 1 1 d . H13 H 1.0349 0.4091 0.2004 0.031 Uiso 1 1 calc R C14 C 0.9034(4) 0.3740(2) 0.1422(3) 0.0251(11) Uani 1 1 d . H14 H 0.9417 0.3792 0.1019 0.030 Uiso 1 1 calc R C15 C 0.7927(4) 0.3487(2) 0.1420(2) 0.0245(11) Uani 1 1 d . C16 C 0.7387(4) 0.3369(2) 0.2013(2) 0.0204(10) Uani 1 1 d . H16 H 0.6639 0.3167 0.2020 0.025 Uiso 1 1 calc R C17 C 0.7952(4) 0.3549(2) 0.2592(3) 0.0246(11) Uani 1 1 d . H17 H 0.7591 0.3465 0.2999 0.029 Uiso 1 1 calc R C18 C 0.7264(4) 0.3396(2) 0.0787(2) 0.0239(11) Uani 1 1 d . H18A H 0.7754 0.3330 0.0412 0.029 Uiso 1 1 calc R H18B H 0.6703 0.2985 0.0809 0.029 Uiso 1 1 calc R C19 C 0.5731(4) 0.4068(2) 0.0970(2) 0.0240(11) Uani 1 1 d . H19 H 0.5347 0.3678 0.1176 0.029 Uiso 1 1 calc R C20 C 0.5276(4) 0.4674(2) 0.0953(2) 0.0218(10) Uani 1 1 d . H20 H 0.4578 0.4698 0.1145 0.026 Uiso 1 1 calc R C21 C 0.5838(4) 0.5259(2) 0.0651(2) 0.0187(10) Uani 1 1 d . C22 C 0.6846(4) 0.5178(3) 0.0360(2) 0.0249(11) Uani 1 1 d . H22 H 0.7239 0.5552 0.0136 0.030 Uiso 1 1 calc R C23 C 0.7277(4) 0.4566(2) 0.0394(2) 0.0225(10) Uani 1 1 d . H23 H 0.7971 0.4524 0.0203 0.027 Uiso 1 1 calc R C24 C 0.5427(4) 0.5932(2) 0.0659(2) 0.0218(10) Uani 1 1 d . C25 C 0.4420(4) 0.6024(2) 0.0962(2) 0.0245(11) Uani 1 1 d . H25 H 0.3959 0.5639 0.1126 0.029 Uiso 1 1 calc R C26 C 0.4112(4) 0.6671(3) 0.1019(3) 0.0304(12) Uani 1 1 d . H26 H 0.3457 0.6733 0.1246 0.036 Uiso 1 1 calc R C27 C 0.5649(4) 0.7132(3) 0.0422(3) 0.0311(12) Uani 1 1 d . H27 H 0.6052 0.7517 0.0218 0.037 Uiso 1 1 calc R C28 C 0.5997(4) 0.6507(2) 0.0377(2) 0.0256(11) Uani 1 1 d . H28 H 0.6654 0.6461 0.0144 0.031 Uiso 1 1 calc R C29 C 0.4425(4) 0.7923(3) 0.0888(3) 0.0333(13) Uani 1 1 d . H29A H 0.3631 0.7903 0.0983 0.040 Uiso 1 1 calc R H29B H 0.4594 0.8208 0.0498 0.040 Uiso 1 1 calc R C30 C 0.5101(4) 0.8233(2) 0.1471(3) 0.0269(12) Uani 1 1 d . C31 C 0.6139(4) 0.8580(2) 0.1384(3) 0.0261(11) Uani 1 1 d . H31 H 0.6393 0.8681 0.0954 0.031 Uiso 1 1 calc R C32 C 0.6824(4) 0.8785(2) 0.1919(3) 0.0299(12) Uani 1 1 d . H32 H 0.7546 0.9014 0.1852 0.036 Uiso 1 1 calc R C33 C 0.6445(4) 0.8653(2) 0.2551(3) 0.0287(12) Uani 1 1 d . C34 C 0.5369(4) 0.8345(3) 0.2638(3) 0.0304(12) Uani 1 1 d . H34 H 0.5092 0.8278 0.3069 0.036 Uiso 1 1 calc R C35 C 0.4694(4) 0.8133(3) 0.2105(3) 0.0307(12) Uani 1 1 d . H35 H 0.3961 0.7923 0.2170 0.037 Uiso 1 1 calc R C36 C 0.7221(4) 0.8801(2) 0.3117(3) 0.0315(12) Uani 1 1 d . H36A H 0.7799 0.9184 0.3012 0.038 Uiso 1 1 calc R H36B H 0.6820 0.8940 0.3508 0.038 Uiso 1 1 calc R Zn1 Zn 0.43699(5) 0.20103(3) 0.18412(3) 0.03351(18) Uani 1 1 d . Cl3 Cl 0.52532(11) 0.18005(7) 0.08885(7) 0.0385(3) Uani 1 1 d . Cl4 Cl 0.28528(11) 0.12135(7) 0.19344(7) 0.0372(3) Uani 1 1 d . Cl5 Cl 0.37654(12) 0.30576(8) 0.18010(9) 0.0523(5) Uani 1 1 d . Cl6 Cl 0.55689(11) 0.20188(7) 0.26948(7) 0.0374(3) Uani 1 1 d . O1S O 0.2514(3) 0.47026(17) 0.14564(18) 0.0301(8) Uani 1 1 d . H1SA H 0.2411 0.4784 0.1869 0.045 Uiso 1 1 d G H1SB H 0.2903 0.4366 0.1412 0.045 Uiso 1 1 d G O2S O 0.0256(4) 0.5690(3) 0.0079(2) 0.0526(12) Uani 1 1 d . H2SA H -0.0236 0.5954 -0.0013 0.079 Uiso 1 1 d G H2SB H 0.0346 0.5686 0.0500 0.079 Uiso 1 1 d G O3S O 0.1646(3) 0.5889(3) 0.1165(3) 0.0648(14) Uani 1 1 d . H3SA H 0.1426 0.6184 0.0901 0.097 Uiso 1 1 d G H3SB H 0.1098 0.5578 0.1256 0.097 Uiso 1 1 d G O4S O 0.2804(5) 0.6328(3) 0.3273(3) 0.0780(16) Uani 1 1 d . H4SA H 0.2678 0.6194 0.2869 0.117 Uiso 1 1 d G H4SB H 0.2985 0.6771 0.3292 0.117 Uiso 1 1 d G O5S O 0.4573(5) 0.7051(3) 0.3920(3) 0.0809(17) Uani 1 1 d . H5SA H 0.4926 0.7231 0.4263 0.121 Uiso 1 1 d G H5SB H 0.4187 0.7347 0.3758 0.121 Uiso 1 1 d G Cl7 Cl 0.5736(2) 0.59245(13) 0.45882(13) 0.0916(7) Uani 1 1 d . Cl8 Cl 0.24429(12) 0.46754(8) 0.30295(8) 0.0481(4) Uani 1 1 d . Cl9 Cl 0.18453(13) 0.71638(9) 0.21633(9) 0.0557(5) Uani 1 1 d . Cl10 Cl 0.1501(2) 0.3588(2) 0.05084(15) 0.1272(11) Uani 1 1 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 Pd1 0.0229(2) 0.0229(2) 0.0309(2) -0.00549(16) -0.00989(16) 0.00663(16) Cl1 0.0243(6) 0.0241(6) 0.0289(7) -0.0066(5) 0.0000(5) 0.0057(5) Cl2 0.0427(8) 0.0308(7) 0.0470(8) 0.0067(6) -0.0202(7) 0.0036(6) O1 0.038(2) 0.050(3) 0.060(3) -0.017(2) 0.002(2) 0.002(2) O2 0.023(2) 0.054(3) 0.045(2) 0.0125(19) 0.0026(17) 0.0061(19) O3 0.024(2) 0.035(2) 0.052(3) 0.0062(18) 0.0072(18) 0.0044(17) O4 0.0234(19) 0.0230(19) 0.050(2) 0.0067(16) 0.0030(17) -0.0010(15) O5 0.0188(17) 0.0186(17) 0.035(2) 0.0031(14) 0.0002(15) 0.0046(14) O6 0.0230(19) 0.0177(17) 0.039(2) 0.0048(15) -0.0030(15) 0.0017(14) O7 0.0203(18) 0.0220(18) 0.046(2) -0.0075(16) -0.0044(16) 0.0016(15) O8 0.031(2) 0.031(2) 0.040(2) 0.0004(16) -0.0092(17) 0.0059(17) N5 0.017(2) 0.033(2) 0.035(3) -0.0005(19) -0.0052(19) 0.0045(19) N6 0.027(2) 0.033(2) 0.027(2) -0.0068(19) -0.0078(19) 0.000(2) N7 0.031(3) 0.032(2) 0.034(3) -0.008(2) -0.009(2) 0.010(2) N8 0.024(2) 0.021(2) 0.041(3) -0.0054(19) -0.009(2) 0.0128(18) C37 0.022(3) 0.021(3) 0.038(3) -0.001(2) -0.002(2) 0.008(2) C38 0.019(3) 0.022(2) 0.029(3) -0.002(2) -0.004(2) 0.003(2) C39 0.026(3) 0.022(3) 0.028(3) -0.002(2) -0.004(2) 0.003(2) C40 0.015(3) 0.057(4) 0.032(3) -0.014(3) -0.002(2) 0.002(3) C41 0.024(3) 0.073(5) 0.036(3) -0.015(3) 0.001(2) 0.001(3) C42 0.021(3) 0.021(3) 0.034(3) -0.003(2) -0.008(2) 0.006(2) C43 0.027(3) 0.028(3) 0.028(3) 0.001(2) -0.002(2) 0.000(2) C44 0.021(3) 0.028(3) 0.044(3) -0.005(2) -0.005(2) -0.005(2) C45 0.029(3) 0.036(3) 0.029(3) 0.001(2) -0.001(2) -0.002(2) C46 0.026(3) 0.029(3) 0.034(3) -0.006(2) -0.007(2) -0.002(2) C47 0.043(4) 0.050(4) 0.032(3) -0.005(3) -0.010(3) -0.009(3) C48 0.030(3) 0.047(4) 0.039(3) -0.015(3) -0.004(3) -0.010(3) C49 0.033(3) 0.040(3) 0.044(4) -0.012(3) -0.007(3) 0.007(3) C50 0.067(5) 0.043(4) 0.038(4) 0.001(3) 0.001(3) 0.017(3) C51 0.035(4) 0.086(5) 0.049(4) 0.008(4) 0.014(3) 0.004(4) C52 0.044(4) 0.075(5) 0.039(4) 0.014(3) 0.006(3) -0.020(4) C53 0.023(3) 0.043(4) 0.059(4) 0.005(3) 0.001(3) -0.009(3) C54 0.019(3) 0.031(3) 0.096(5) 0.006(3) 0.010(3) -0.001(3) C55 0.017(2) 0.018(2) 0.034(3) 0.004(2) -0.002(2) 0.001(2) C56 0.015(2) 0.026(3) 0.039(3) -0.003(2) 0.003(2) 0.002(2) C57 0.023(3) 0.027(3) 0.029(3) -0.004(2) -0.001(2) 0.011(2) C58 0.020(3) 0.021(2) 0.029(3) -0.001(2) -0.004(2) 0.000(2) C59 0.015(2) 0.018(2) 0.020(2) -0.0052(18) -0.0027(18) 0.0041(18) C60 0.020(2) 0.021(2) 0.026(3) -0.001(2) -0.002(2) 0.003(2) C61 0.017(2) 0.024(3) 0.026(3) 0.000(2) 0.003(2) 0.007(2) C62 0.025(3) 0.022(2) 0.028(3) -0.007(2) -0.003(2) 0.014(2) C63 0.021(3) 0.017(2) 0.027(3) -0.0060(19) -0.007(2) 0.005(2) C64 0.018(2) 0.022(2) 0.026(3) -0.002(2) -0.004(2) 0.000(2) C65 0.023(3) 0.022(3) 0.031(3) 0.000(2) 0.003(2) 0.006(2) C66 0.019(3) 0.027(3) 0.032(3) 0.006(2) -0.003(2) 0.005(2) C67 0.024(3) 0.021(3) 0.052(4) 0.003(2) -0.001(2) 0.002(2) C68 0.018(3) 0.026(3) 0.063(4) 0.000(3) -0.005(3) -0.001(2) C69 0.025(3) 0.039(3) 0.062(4) -0.017(3) -0.017(3) 0.005(3) C70 0.035(3) 0.037(3) 0.043(3) -0.006(3) -0.019(3) 0.005(3) C71 0.036(3) 0.033(3) 0.032(3) -0.006(2) -0.009(2) 0.003(2) C72 0.035(3) 0.039(3) 0.032(3) -0.009(2) -0.016(2) 0.003(3) C73 0.030(3) 0.021(3) 0.040(3) -0.001(2) -0.007(2) 0.005(2) C74 0.035(3) 0.022(3) 0.031(3) -0.007(2) -0.008(2) 0.007(2) C75 0.040(3) 0.027(3) 0.042(3) -0.011(2) -0.016(3) 0.020(2) C76 0.023(3) 0.052(4) 0.048(4) -0.020(3) -0.006(3) 0.010(3) C77 0.034(3) 0.050(4) 0.046(4) -0.016(3) -0.010(3) 0.015(3) C78 0.031(3) 0.024(3) 0.042(3) -0.012(2) -0.016(2) 0.016(2) C79 0.030(3) 0.027(3) 0.045(4) 0.003(2) -0.020(3) 0.001(2) C80 0.040(3) 0.028(3) 0.035(3) 0.000(2) -0.012(3) 0.001(3) C81 0.024(3) 0.027(3) 0.039(3) -0.011(2) -0.011(2) 0.015(2) C82 0.025(3) 0.031(3) 0.041(3) -0.012(2) -0.005(2) 0.017(2) N1 0.034(3) 0.018(2) 0.033(2) -0.0059(18) -0.008(2) 0.0045(19) N2 0.025(2) 0.021(2) 0.027(2) 0.0026(17) -0.0042(18) 0.0039(18) N3 0.024(2) 0.018(2) 0.025(2) -0.0013(16) -0.0040(17) 0.0028(17) N4 0.018(2) 0.021(2) 0.041(3) -0.0066(18) -0.0108(19) 0.0110(18) C1 0.024(3) 0.024(3) 0.033(3) -0.003(2) -0.001(2) -0.004(2) C2 0.018(3) 0.031(3) 0.029(3) -0.001(2) -0.001(2) 0.001(2) C3 0.027(3) 0.018(2) 0.024(3) -0.0063(19) -0.005(2) -0.001(2) C4 0.038(3) 0.028(3) 0.027(3) 0.000(2) -0.002(2) 0.005(2) C5 0.036(3) 0.024(3) 0.036(3) -0.003(2) 0.000(2) 0.003(2) C6 0.024(3) 0.021(2) 0.022(3) -0.0037(19) -0.007(2) 0.004(2) C7 0.020(3) 0.024(3) 0.044(3) 0.004(2) -0.007(2) -0.004(2) C8 0.019(3) 0.026(3) 0.036(3) 0.003(2) -0.006(2) 0.001(2) C9 0.022(3) 0.022(3) 0.032(3) 0.002(2) -0.002(2) 0.001(2) C10 0.019(2) 0.025(3) 0.026(3) -0.005(2) -0.001(2) 0.000(2) C11 0.026(3) 0.021(3) 0.039(3) 0.003(2) -0.001(2) 0.010(2) C12 0.026(3) 0.015(2) 0.032(3) 0.005(2) -0.003(2) 0.009(2) C13 0.019(3) 0.031(3) 0.030(3) 0.002(2) 0.002(2) 0.008(2) C14 0.022(3) 0.022(3) 0.033(3) 0.001(2) 0.008(2) 0.011(2) C15 0.028(3) 0.011(2) 0.035(3) -0.003(2) -0.003(2) 0.006(2) C16 0.015(2) 0.014(2) 0.032(3) -0.0021(19) 0.001(2) 0.0018(19) C17 0.028(3) 0.014(2) 0.033(3) 0.001(2) 0.003(2) 0.007(2) C18 0.027(3) 0.016(2) 0.030(3) -0.002(2) 0.001(2) 0.008(2) C19 0.015(2) 0.022(3) 0.034(3) -0.002(2) 0.000(2) -0.001(2) C20 0.019(2) 0.023(2) 0.024(3) -0.002(2) -0.003(2) 0.003(2) C21 0.016(2) 0.018(2) 0.021(2) -0.0046(18) -0.0027(19) 0.0012(19) C22 0.020(3) 0.028(3) 0.026(3) 0.000(2) -0.001(2) 0.001(2) C23 0.021(3) 0.024(3) 0.022(3) -0.003(2) 0.004(2) 0.002(2) C24 0.018(2) 0.028(3) 0.020(2) -0.007(2) -0.0071(19) 0.006(2) C25 0.013(2) 0.021(2) 0.039(3) -0.004(2) -0.004(2) 0.003(2) C26 0.017(3) 0.028(3) 0.047(3) -0.007(2) -0.004(2) 0.005(2) C27 0.034(3) 0.022(3) 0.038(3) 0.004(2) -0.008(2) 0.008(2) C28 0.022(3) 0.027(3) 0.029(3) 0.000(2) 0.000(2) 0.007(2) C29 0.025(3) 0.024(3) 0.054(4) -0.007(2) -0.004(2) 0.017(2) C30 0.020(3) 0.018(2) 0.046(3) -0.001(2) 0.000(2) 0.014(2) C31 0.024(3) 0.022(3) 0.034(3) 0.001(2) -0.001(2) 0.010(2) C32 0.023(3) 0.017(2) 0.050(4) 0.002(2) 0.001(2) 0.003(2) C33 0.025(3) 0.016(2) 0.045(3) -0.004(2) 0.001(2) 0.004(2) C34 0.023(3) 0.022(3) 0.047(3) -0.003(2) 0.007(2) 0.007(2) C35 0.013(2) 0.026(3) 0.055(4) -0.005(2) 0.001(2) 0.009(2) C36 0.027(3) 0.015(2) 0.053(4) -0.007(2) 0.005(2) 0.006(2) Zn1 0.0217(3) 0.0289(3) 0.0504(4) 0.0077(3) -0.0019(3) 0.0038(3) Cl3 0.0279(7) 0.0416(8) 0.0468(9) 0.0069(6) 0.0011(6) 0.0062(6) Cl4 0.0227(7) 0.0334(7) 0.0548(9) 0.0026(6) -0.0012(6) 0.0004(6) Cl5 0.0320(8) 0.0374(8) 0.0921(13) 0.0259(8) 0.0239(8) 0.0165(7) Cl6 0.0332(8) 0.0246(7) 0.0543(9) -0.0015(6) -0.0083(6) 0.0047(6) O1S 0.0208(19) 0.0196(18) 0.049(2) 0.0067(16) 0.0082(17) -0.0015(15) O2S 0.051(3) 0.073(3) 0.042(3) 0.015(2) 0.022(2) 0.036(2) O3S 0.026(2) 0.067(3) 0.099(4) -0.014(3) 0.005(2) 0.003(2) O4S 0.074(4) 0.086(4) 0.075(4) 0.005(3) -0.001(3) 0.011(4) O5S 0.082(5) 0.087(4) 0.073(4) -0.001(3) 0.027(3) 0.008(3) Cl7 0.0757(15) 0.0876(16) 0.1071(19) -0.0108(13) 0.0038(13) -0.0026(13) Cl8 0.0334(8) 0.0525(9) 0.0607(10) 0.0048(8) -0.0005(7) 0.0132(7) Cl9 0.0406(9) 0.0620(11) 0.0614(11) 0.0116(8) -0.0088(8) -0.0061(8) Cl10 0.0826(18) 0.193(3) 0.108(2) -0.010(2) 0.0118(16) 0.030(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl1 Pd1 Cl2 176.99(5) . . N5 Pd1 Cl1 88.82(13) . . N5 Pd1 Cl2 88.30(13) . . N5 Pd1 N8 179.24(17) . 2_665 N8 Pd1 Cl1 91.92(12) 2_665 . N8 Pd1 Cl2 90.95(12) 2_665 . C49 O1 C48 110.8(4) . . C51 O2 C50 108.3(5) . . C53 O3 C52 116.2(4) . . C55 O4 C54 114.8(4) . . C60 O5 C65 115.6(4) . . C66 O6 C67 112.0(4) . . C68 O7 C69 109.8(4) . . C71 O8 C70 111.8(4) . . C37 N5 Pd1 121.4(3) . . C41 N5 Pd1 120.1(4) . . C41 N5 C37 118.4(5) . . C44 N6 C45 121.0(4) . . C44 N6 C47 119.5(5) . . C45 N6 C47 119.4(5) . . C73 N7 C72 119.1(5) . . C77 N7 C72 120.5(5) . . C77 N7 C73 120.2(5) . . C80 N8 Pd1 118.3(4) . 2_665 C80 N8 C81 120.1(5) . . C81 N8 Pd1 121.6(3) . 2_665 N5 C37 H37 119.2 . . N5 C37 C38 121.6(5) . . C38 C37 H37 119.2 . . C37 C38 H38 120.0 . . C37 C38 C39 120.1(5) . . C39 C38 H38 120.0 . . C38 C39 C42 121.6(5) . . C40 C39 C38 117.4(4) . . C40 C39 C42 121.0(5) . . C39 C40 H40 120.3 . . C41 C40 C39 119.3(5) . . C41 C40 H40 120.3 . . N5 C41 C40 123.1(5) . . N5 C41 H41 118.4 . . C40 C41 H41 118.4 . . C43 C42 C39 120.7(5) . . C46 C42 C39 121.8(5) . . C46 C42 C43 117.5(5) . . C42 C43 H43 120.2 . . C44 C43 C42 119.6(5) . . C44 C43 H43 120.2 . . N6 C44 C43 121.4(5) . . N6 C44 H44 119.3 . . C43 C44 H44 119.3 . . N6 C45 H45 120.2 . . N6 C45 C46 119.5(5) . . C46 C45 H45 120.2 . . C42 C46 H46 119.6 . . C45 C46 C42 120.8(5) . . C45 C46 H46 119.6 . . N6 C47 H47A 110.2 . . N6 C47 H47B 110.2 . . N6 C47 C48 107.8(5) . . H47A C47 H47B 108.5 . . C48 C47 H47A 110.2 . . C48 C47 H47B 110.2 . . O1 C48 C47 107.3(4) . . O1 C48 H48A 110.3 . . O1 C48 H48B 110.3 . . C47 C48 H48A 110.3 . . C47 C48 H48B 110.3 . . H48A C48 H48B 108.5 . . O1 C49 H49A 109.3 . . O1 C49 H49B 109.3 . . O1 C49 C50 111.8(5) . . H49A C49 H49B 107.9 . . C50 C49 H49A 109.3 . . C50 C49 H49B 109.3 . . O2 C50 C49 110.3(5) . . O2 C50 H50A 109.6 . . O2 C50 H50B 109.6 . . C49 C50 H50A 109.6 . . C49 C50 H50B 109.6 . . H50A C50 H50B 108.1 . . O2 C51 H51A 109.0 . . O2 C51 H51B 109.0 . . O2 C51 C52 112.8(5) . . H51A C51 H51B 107.8 . . C52 C51 H51A 109.0 . . C52 C51 H51B 109.0 . . O3 C52 C51 114.6(6) . . O3 C52 H52A 108.6 . . O3 C52 H52B 108.6 . . C51 C52 H52A 108.6 . . C51 C52 H52B 108.6 . . H52A C52 H52B 107.6 . . O3 C53 H53A 109.1 . . O3 C53 H53B 109.1 . . O3 C53 C54 112.5(5) . . H53A C53 H53B 107.8 . . C54 C53 H53A 109.1 . . C54 C53 H53B 109.1 . . O4 C54 C53 111.0(5) . . O4 C54 H54A 109.4 . . O4 C54 H54B 109.4 . . C53 C54 H54A 109.4 . . C53 C54 H54B 109.4 . . H54A C54 H54B 108.0 . . O4 C55 C56 124.7(4) . . O4 C55 C64 114.4(4) . . C56 C55 C64 120.8(4) . . C55 C56 H56 119.9 . . C55 C56 C57 120.3(5) . . C57 C56 H56 119.9 . . C56 C57 H57 119.4 . . C58 C57 C56 121.2(5) . . C58 C57 H57 119.4 . . C57 C58 H58 120.4 . . C57 C58 C59 119.2(4) . . C59 C58 H58 120.4 . . C58 C59 C60 121.9(4) . . C58 C59 C64 121.3(4) . . C64 C59 C60 116.8(4) . . O5 C60 C59 114.2(4) . . C61 C60 O5 124.5(4) . . C61 C60 C59 121.2(4) . . C60 C61 H61 119.9 . . C60 C61 C62 120.1(5) . . C62 C61 H61 119.9 . . C61 C62 H62 119.3 . . C63 C62 C61 121.3(4) . . C63 C62 H62 119.3 . . C62 C63 H63 120.5 . . C62 C63 C64 119.0(4) . . C64 C63 H63 120.5 . . C59 C64 C55 117.2(4) . . C63 C64 C55 121.2(4) . . C63 C64 C59 121.6(4) . . O5 C65 H65A 109.8 . . O5 C65 H65B 109.8 . . O5 C65 C66 109.5(4) . . H65A C65 H65B 108.2 . . C66 C65 H65A 109.8 . . C66 C65 H65B 109.8 . . O6 C66 C65 111.1(4) . . O6 C66 H66A 109.4 . . O6 C66 H66B 109.4 . . C65 C66 H66A 109.4 . . C65 C66 H66B 109.4 . . H66A C66 H66B 108.0 . . O6 C67 H67A 109.4 . . O6 C67 H67B 109.4 . . O6 C67 C68 111.1(4) . . H67A C67 H67B 108.0 . . C68 C67 H67A 109.4 . . C68 C67 H67B 109.4 . . O7 C68 C67 110.7(4) . . O7 C68 H68A 109.5 . . O7 C68 H68B 109.5 . . C67 C68 H68A 109.5 . . C67 C68 H68B 109.5 . . H68A C68 H68B 108.1 . . O7 C69 H69A 109.3 . . O7 C69 H69B 109.3 . . O7 C69 C70 111.6(4) . . H69A C69 H69B 108.0 . . C70 C69 H69A 109.3 . . C70 C69 H69B 109.3 . . O8 C70 C69 108.5(5) . . O8 C70 H70A 110.0 . . O8 C70 H70B 110.0 . . C69 C70 H70A 110.0 . . C69 C70 H70B 110.0 . . H70A C70 H70B 108.4 . . O8 C71 H71A 109.6 . . O8 C71 H71B 109.6 . . O8 C71 C72 110.4(5) . . H71A C71 H71B 108.1 . . C72 C71 H71A 109.6 . . C72 C71 H71B 109.6 . . N7 C72 C71 112.2(4) . . N7 C72 H72A 109.2 . . N7 C72 H72B 109.2 . . C71 C72 H72A 109.2 . . C71 C72 H72B 109.2 . . H72A C72 H72B 107.9 . . N7 C73 H73 120.1 . . N7 C73 C74 119.7(5) . . C74 C73 H73 120.1 . . C73 C74 H74 119.8 . . C73 C74 C75 120.4(5) . . C75 C74 H74 119.8 . . C74 C75 C78 119.3(5) . . C76 C75 C74 118.1(5) . . C76 C75 C78 122.6(5) . . C75 C76 H76 120.3 . . C77 C76 C75 119.4(6) . . C77 C76 H76 120.3 . . N7 C77 C76 122.2(6) . . N7 C77 H77 118.9 . . C76 C77 H77 118.9 . . C79 C78 C75 120.0(5) . . C82 C78 C75 121.8(5) . . C82 C78 C79 118.2(5) . . C78 C79 H79 120.4 . . C80 C79 C78 119.2(5) . . C80 C79 H79 120.4 . . N8 C80 C79 122.2(5) . . N8 C80 H80 118.9 . . C79 C80 H80 118.9 . . N8 C81 H81 119.9 . . N8 C81 C82 120.1(5) . . C82 C81 H81 119.9 . . C78 C82 C81 120.2(5) . . C78 C82 H82 119.9 . . C81 C82 H82 119.9 . . C1 N1 C36 120.1(4) . . C5 N1 C1 120.9(5) . . C5 N1 C36 118.7(5) . . C8 N2 C9 122.2(4) . . C8 N2 C11 120.4(4) . . C9 N2 C11 117.3(4) . . C19 N3 C18 119.5(4) . . C23 N3 C18 118.8(4) . . C23 N3 C19 121.4(4) . . C26 N4 C27 120.5(4) . . C26 N4 C29 120.4(4) . . C27 N4 C29 119.0(4) . . N1 C1 H1 119.6 . . N1 C1 C2 120.9(5) . . C2 C1 H1 119.6 . . C1 C2 H2 119.9 . . C1 C2 C3 120.2(5) . . C3 C2 H2 119.9 . . C2 C3 C6 122.2(5) . . C4 C3 C2 117.0(5) . . C4 C3 C6 120.6(4) . . C3 C4 H4 119.8 . . C5 C4 C3 120.4(5) . . C5 C4 H4 119.8 . . N1 C5 C4 120.5(5) . . N1 C5 H5 119.7 . . C4 C5 H5 119.7 . . C7 C6 C3 121.6(4) . . C10 C6 C3 120.8(5) . . C10 C6 C7 117.5(5) . . C6 C7 H7 120.0 . . C8 C7 C6 120.1(5) . . C8 C7 H7 120.0 . . N2 C8 C7 120.2(5) . . N2 C8 H8 119.9 . . C7 C8 H8 119.9 . . N2 C9 H9 120.3 . . N2 C9 C10 119.4(4) . . C10 C9 H9 120.3 . . C6 C10 H10 119.7 . . C9 C10 C6 120.6(5) . . C9 C10 H10 119.7 . . N2 C11 H11A 109.8 . . N2 C11 H11B 109.8 . . H11A C11 H11B 108.3 . . C12 C11 N2 109.2(4) . . C12 C11 H11A 109.8 . . C12 C11 H11B 109.8 . . C13 C12 C11 119.6(5) . . C17 C12 C11 119.8(5) . . C17 C12 C13 120.4(5) . . C12 C13 H13 120.4 . . C12 C13 C14 119.1(5) . . C14 C13 H13 120.4 . . C13 C14 H14 119.7 . . C15 C14 C13 120.6(5) . . C15 C14 H14 119.7 . . C14 C15 C16 119.5(5) . . C14 C15 C18 121.3(5) . . C16 C15 C18 119.0(4) . . C15 C16 H16 120.4 . . C17 C16 C15 119.1(4) . . C17 C16 H16 120.4 . . C12 C17 C16 120.9(5) . . C12 C17 H17 119.6 . . C16 C17 H17 119.6 . . N3 C18 C15 108.3(4) . . N3 C18 H18A 110.0 . . N3 C18 H18B 110.0 . . C15 C18 H18A 110.0 . . C15 C18 H18B 110.0 . . H18A C18 H18B 108.4 . . N3 C19 H19 119.9 . . N3 C19 C20 120.2(4) . . C20 C19 H19 119.9 . . C19 C20 H20 119.7 . . C19 C20 C21 120.6(4) . . C21 C20 H20 119.7 . . C20 C21 C24 122.8(4) . . C22 C21 C20 116.4(4) . . C22 C21 C24 120.7(4) . . C21 C22 H22 119.4 . . C23 C22 C21 121.2(4) . . C23 C22 H22 119.4 . . N3 C23 C22 120.2(5) . . N3 C23 H23 119.9 . . C22 C23 H23 119.9 . . C25 C24 C21 121.3(4) . . C28 C24 C21 122.4(4) . . C28 C24 C25 116.3(4) . . C24 C25 H25 120.1 . . C26 C25 C24 119.9(5) . . C26 C25 H25 120.1 . . N4 C26 C25 121.2(5) . . N4 C26 H26 119.4 . . C25 C26 H26 119.4 . . N4 C27 H27 120.1 . . C28 C27 N4 119.8(5) . . C28 C27 H27 120.1 . . C24 C28 H28 119.0 . . C27 C28 C24 122.0(5) . . C27 C28 H28 119.0 . . N4 C29 H29A 110.2 . . N4 C29 H29B 110.2 . . N4 C29 C30 107.6(4) . . H29A C29 H29B 108.5 . . C30 C29 H29A 110.2 . . C30 C29 H29B 110.2 . . C31 C30 C29 120.6(5) . . C31 C30 C35 119.5(5) . . C35 C30 C29 119.8(5) . . C30 C31 H31 119.5 . . C30 C31 C32 121.0(5) . . C32 C31 H31 119.5 . . C31 C32 H32 120.2 . . C33 C32 C31 119.6(5) . . C33 C32 H32 120.2 . . C32 C33 C36 119.4(5) . . C34 C33 C32 119.1(5) . . C34 C33 C36 121.4(5) . . C33 C34 H34 119.5 . . C35 C34 C33 121.1(5) . . C35 C34 H34 119.5 . . C30 C35 H35 120.3 . . C34 C35 C30 119.4(5) . . C34 C35 H35 120.3 . . N1 C36 C33 108.7(4) . . N1 C36 H36A 109.9 . . N1 C36 H36B 109.9 . . C33 C36 H36A 109.9 . . C33 C36 H36B 109.9 . . H36A C36 H36B 108.3 . . Cl4 Zn1 Cl3 109.16(6) . . Cl5 Zn1 Cl3 109.46(6) . . Cl5 Zn1 Cl4 106.75(6) . . Cl5 Zn1 Cl6 108.94(7) . . Cl6 Zn1 Cl3 109.10(6) . . Cl6 Zn1 Cl4 113.36(6) . . H1SA O1S H1SB 109.5 . . H2SA O2S H2SB 109.4 . . H3SA O3S H3SB 109.5 . . H4SA O4S H4SB 109.5 . . H5SA O5S H5SB 109.4 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 Cl1 2.2888(13) . Pd1 Cl2 2.3142(14) . Pd1 N5 1.996(4) . Pd1 N8 2.044(4) 2_665 O1 C48 1.432(7) . O1 C49 1.384(7) . O2 C50 1.417(7) . O2 C51 1.410(7) . O3 C52 1.394(7) . O3 C53 1.375(7) . O4 C54 1.455(7) . O4 C55 1.358(6) . O5 C60 1.384(6) . O5 C65 1.445(6) . O6 C66 1.418(6) . O6 C67 1.425(6) . O7 C68 1.427(7) . O7 C69 1.431(6) . O8 C70 1.426(6) . O8 C71 1.403(7) . N5 C37 1.346(6) . N5 C41 1.338(7) . N6 C44 1.329(7) . N6 C45 1.358(6) . N6 C47 1.469(6) . N7 C72 1.480(6) . N7 C73 1.353(7) . N7 C77 1.336(7) . N8 Pd1 2.044(4) 2_665 N8 C80 1.329(7) . N8 C81 1.359(7) . C37 H37 0.9500 . C37 C38 1.375(7) . C38 H38 0.9500 . C38 C39 1.394(7) . C39 C40 1.392(7) . C39 C42 1.470(7) . C40 H40 0.9500 . C40 C41 1.366(7) . C41 H41 0.9500 . C42 C43 1.404(7) . C42 C46 1.388(7) . C43 H43 0.9500 . C43 C44 1.375(7) . C44 H44 0.9500 . C45 H45 0.9500 . C45 C46 1.381(7) . C46 H46 0.9500 . C47 H47A 0.9900 . C47 H47B 0.9900 . C47 C48 1.518(8) . C48 H48A 0.9900 . C48 H48B 0.9900 . C49 H49A 0.9900 . C49 H49B 0.9900 . C49 C50 1.500(9) . C50 H50A 0.9900 . C50 H50B 0.9900 . C51 H51A 0.9900 . C51 H51B 0.9900 . C51 C52 1.450(9) . C52 H52A 0.9900 . C52 H52B 0.9900 . C53 H53A 0.9900 . C53 H53B 0.9900 . C53 C54 1.469(8) . C54 H54A 0.9900 . C54 H54B 0.9900 . C55 C56 1.365(7) . C55 C64 1.445(7) . C56 H56 0.9500 . C56 C57 1.422(7) . C57 H57 0.9500 . C57 C58 1.373(7) . C58 H58 0.9500 . C58 C59 1.411(7) . C59 C60 1.432(6) . C59 C64 1.425(6) . C60 C61 1.357(7) . C61 H61 0.9500 . C61 C62 1.398(7) . C62 H62 0.9500 . C62 C63 1.382(7) . C63 H63 0.9500 . C63 C64 1.384(7) . C65 H65A 0.9900 . C65 H65B 0.9900 . C65 C66 1.488(6) . C66 H66A 0.9900 . C66 H66B 0.9900 . C67 H67A 0.9900 . C67 H67B 0.9900 . C67 C68 1.481(8) . C68 H68A 0.9900 . C68 H68B 0.9900 . C69 H69A 0.9900 . C69 H69B 0.9900 . C69 C70 1.500(8) . C70 H70A 0.9900 . C70 H70B 0.9900 . C71 H71A 0.9900 . C71 H71B 0.9900 . C71 C72 1.515(8) . C72 H72A 0.9900 . C72 H72B 0.9900 . C73 H73 0.9500 . C73 C74 1.373(7) . C74 H74 0.9500 . C74 C75 1.395(8) . C75 C76 1.380(8) . C75 C78 1.491(7) . C76 H76 0.9500 . C76 C77 1.360(8) . C77 H77 0.9500 . C78 C79 1.392(8) . C78 C82 1.389(8) . C79 H79 0.9500 . C79 C80 1.383(7) . C80 H80 0.9500 . C81 H81 0.9500 . C81 C82 1.392(7) . C82 H82 0.9500 . N1 C1 1.354(7) . N1 C5 1.347(7) . N1 C36 1.475(6) . N2 C8 1.323(6) . N2 C9 1.350(6) . N2 C11 1.520(6) . N3 C18 1.495(6) . N3 C19 1.351(6) . N3 C23 1.341(6) . N4 C26 1.326(6) . N4 C27 1.369(7) . N4 C29 1.498(6) . C1 H1 0.9500 . C1 C2 1.379(7) . C2 H2 0.9500 . C2 C3 1.414(7) . C3 C4 1.410(7) . C3 C6 1.463(7) . C4 H4 0.9500 . C4 C5 1.388(7) . C5 H5 0.9500 . C6 C7 1.395(7) . C6 C10 1.393(7) . C7 H7 0.9500 . C7 C8 1.392(7) . C8 H8 0.9500 . C9 H9 0.9500 . C9 C10 1.386(7) . C10 H10 0.9500 . C11 H11A 0.9900 . C11 H11B 0.9900 . C11 C12 1.513(7) . C12 C13 1.380(7) . C12 C17 1.363(7) . C13 H13 0.9500 . C13 C14 1.384(7) . C14 H14 0.9500 . C14 C15 1.383(7) . C15 C16 1.391(7) . C15 C18 1.521(7) . C16 H16 0.9500 . C16 C17 1.384(7) . C17 H17 0.9500 . C18 H18A 0.9900 . C18 H18B 0.9900 . C19 H19 0.9500 . C19 C20 1.376(7) . C20 H20 0.9500 . C20 C21 1.413(6) . C21 C22 1.400(7) . C21 C24 1.471(6) . C22 H22 0.9500 . C22 C23 1.376(7) . C23 H23 0.9500 . C24 C25 1.414(7) . C24 C28 1.383(7) . C25 H25 0.9500 . C25 C26 1.370(7) . C26 H26 0.9500 . C27 H27 0.9500 . C27 C28 1.350(7) . C28 H28 0.9500 . C29 H29A 0.9900 . C29 H29B 0.9900 . C29 C30 1.517(7) . C30 C31 1.376(7) . C30 C35 1.396(8) . C31 H31 0.9500 . C31 C32 1.395(7) . C32 H32 0.9500 . C32 C33 1.391(8) . C33 C34 1.390(7) . C33 C36 1.494(7) . C34 H34 0.9500 . C34 C35 1.388(7) . C35 H35 0.9500 . C36 H36A 0.9900 . C36 H36B 0.9900 . Zn1 Cl3 2.2839(16) . Zn1 Cl4 2.2774(14) . Zn1 Cl5 2.2740(16) . Zn1 Cl6 2.2764(15) . O1S H1SA 0.8659 . O1S H1SB 0.8673 . O2S H2SA 0.8675 . O2S H2SB 0.8660 . O3S H3SA 0.8663 . O3S H3SB 0.8685 . O4S H4SA 0.8660 . O4S H4SB 0.8677 . O5S H5SA 0.8661 . O5S H5SB 0.8671 . 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 Pd1 N5 C37 C38 175.7(4) . Pd1 N5 C41 C40 -176.4(5) . Pd1 N8 C80 C79 -178.4(4) 2_665 Pd1 N8 C81 C82 177.7(3) 2_665 O1 C49 C50 O2 -67.9(6) . O2 C51 C52 O3 -66.7(8) . O3 C53 C54 O4 67.6(7) . O4 C55 C56 C57 175.9(4) . O4 C55 C64 C59 -175.4(4) . O4 C55 C64 C63 3.2(6) . O5 C60 C61 C62 179.8(4) . O5 C65 C66 O6 77.5(5) . O6 C67 C68 O7 -70.6(6) . O7 C69 C70 O8 -67.3(6) . O8 C71 C72 N7 66.1(6) . N5 C37 C38 C39 1.0(7) . N6 C45 C46 C42 2.0(8) . N6 C47 C48 O1 65.5(6) . N7 C73 C74 C75 1.1(7) . N8 C81 C82 C78 0.3(7) . C37 N5 C41 C40 -0.2(9) . C37 C38 C39 C40 -0.8(7) . C37 C38 C39 C42 179.0(4) . C38 C39 C40 C41 0.1(8) . C38 C39 C42 C43 -149.8(5) . C38 C39 C42 C46 31.8(7) . C39 C40 C41 N5 0.4(10) . C39 C42 C43 C44 -179.8(5) . C39 C42 C46 C45 178.4(5) . C40 C39 C42 C43 30.0(7) . C40 C39 C42 C46 -148.4(5) . C41 N5 C37 C38 -0.5(7) . C42 C39 C40 C41 -179.7(5) . C42 C43 C44 N6 0.7(8) . C43 C42 C46 C45 -0.1(8) . C44 N6 C45 C46 -2.7(8) . C44 N6 C47 C48 89.8(6) . C45 N6 C44 C43 1.3(8) . C45 N6 C47 C48 -87.7(6) . C46 C42 C43 C44 -1.3(7) . C47 N6 C44 C43 -176.2(5) . C47 N6 C45 C46 174.8(5) . C48 O1 C49 C50 179.8(5) . C49 O1 C48 C47 179.8(5) . C50 O2 C51 C52 174.3(6) . C51 O2 C50 C49 -175.0(5) . C52 O3 C53 C54 159.9(6) . C53 O3 C52 C51 -165.5(6) . C54 O4 C55 C56 -2.5(7) . C54 O4 C55 C64 174.8(4) . C55 O4 C54 C53 -165.6(5) . C55 C56 C57 C58 0.1(7) . C56 C55 C64 C59 2.0(7) . C56 C55 C64 C63 -179.3(5) . C56 C57 C58 C59 0.3(7) . C57 C58 C59 C60 -178.9(4) . C57 C58 C59 C64 0.6(7) . C58 C59 C60 O5 0.2(6) . C58 C59 C60 C61 -179.4(4) . C58 C59 C64 C55 -1.7(6) . C58 C59 C64 C63 179.7(4) . C59 C60 C61 C62 -0.5(7) . C60 O5 C65 C66 -175.9(4) . C60 C59 C64 C55 177.8(4) . C60 C59 C64 C63 -0.8(6) . C60 C61 C62 C63 -0.3(7) . C61 C62 C63 C64 0.6(7) . C62 C63 C64 C55 -178.5(4) . C62 C63 C64 C59 0.1(7) . C64 C55 C56 C57 -1.2(7) . C64 C59 C60 O5 -179.2(4) . C64 C59 C60 C61 1.1(7) . C65 O5 C60 C59 -177.2(4) . C65 O5 C60 C61 2.4(6) . C66 O6 C67 C68 -172.4(4) . C67 O6 C66 C65 169.4(4) . C68 O7 C69 C70 -177.4(5) . C69 O7 C68 C67 -175.5(4) . C70 O8 C71 C72 179.3(4) . C71 O8 C70 C69 178.2(4) . C72 N7 C73 C74 -175.3(5) . C72 N7 C77 C76 175.8(6) . C73 N7 C72 C71 -64.6(6) . C73 N7 C77 C76 1.8(9) . C73 C74 C75 C76 -1.4(8) . C73 C74 C75 C78 179.8(5) . C74 C75 C76 C77 1.9(8) . C74 C75 C78 C79 -22.1(7) . C74 C75 C78 C82 156.6(5) . C75 C76 C77 N7 -2.2(9) . C75 C78 C79 C80 177.6(5) . C75 C78 C82 C81 -178.2(5) . C76 C75 C78 C79 159.2(5) . C76 C75 C78 C82 -22.2(8) . C77 N7 C72 C71 121.4(6) . C77 N7 C73 C74 -1.2(7) . C78 C75 C76 C77 -179.3(5) . C78 C79 C80 N8 1.0(8) . C79 C78 C82 C81 0.4(7) . C80 N8 C81 C82 -0.4(7) . C81 N8 C80 C79 -0.2(8) . C82 C78 C79 C80 -1.0(8) . N1 C1 C2 C3 0.5(7) . N2 C9 C10 C6 0.5(7) . N2 C11 C12 C13 88.2(5) . N2 C11 C12 C17 -87.0(5) . N3 C19 C20 C21 -0.2(7) . N4 C27 C28 C24 0.9(8) . N4 C29 C30 C31 87.7(6) . N4 C29 C30 C35 -88.8(5) . C1 N1 C5 C4 -3.5(7) . C1 N1 C36 C33 89.1(5) . C1 C2 C3 C4 -2.9(7) . C1 C2 C3 C6 172.1(4) . C2 C3 C4 C5 2.2(7) . C2 C3 C6 C7 16.5(7) . C2 C3 C6 C10 -160.8(5) . C3 C4 C5 N1 0.9(8) . C3 C6 C7 C8 -175.9(4) . C3 C6 C10 C9 175.6(4) . C4 C3 C6 C7 -168.7(5) . C4 C3 C6 C10 14.0(7) . C5 N1 C1 C2 2.7(7) . C5 N1 C36 C33 -85.3(6) . C6 C3 C4 C5 -172.9(4) . C6 C7 C8 N2 0.1(8) . C7 C6 C10 C9 -1.8(7) . C8 N2 C9 C10 1.2(7) . C8 N2 C11 C12 -96.7(5) . C9 N2 C8 C7 -1.4(7) . C9 N2 C11 C12 79.1(5) . C10 C6 C7 C8 1.5(7) . C11 N2 C8 C7 174.2(4) . C11 N2 C9 C10 -174.6(4) . C11 C12 C13 C14 -170.0(4) . C11 C12 C17 C16 169.8(4) . C12 C13 C14 C15 -0.3(7) . C13 C12 C17 C16 -5.4(7) . C13 C14 C15 C16 -4.3(7) . C13 C14 C15 C18 170.1(4) . C14 C15 C16 C17 4.1(7) . C14 C15 C18 N3 -94.5(5) . C15 C16 C17 C12 0.7(7) . C16 C15 C18 N3 79.9(5) . C17 C12 C13 C14 5.2(7) . C18 N3 C19 C20 172.9(4) . C18 N3 C23 C22 -173.6(4) . C18 C15 C16 C17 -170.4(4) . C19 N3 C18 C15 -87.1(5) . C19 N3 C23 C22 0.3(7) . C19 C20 C21 C22 1.8(6) . C19 C20 C21 C24 -175.5(4) . C20 C21 C22 C23 -2.5(7) . C20 C21 C24 C25 -1.4(7) . C20 C21 C24 C28 178.2(4) . C21 C22 C23 N3 1.5(7) . C21 C24 C25 C26 173.5(4) . C21 C24 C28 C27 -175.8(4) . C22 C21 C24 C25 -178.7(4) . C22 C21 C24 C28 1.0(7) . C23 N3 C18 C15 86.8(5) . C23 N3 C19 C20 -0.9(7) . C24 C21 C22 C23 174.9(4) . C24 C25 C26 N4 3.7(7) . C25 C24 C28 C27 3.9(7) . C26 N4 C27 C28 -3.7(7) . C26 N4 C29 C30 94.3(5) . C27 N4 C26 C25 1.4(7) . C27 N4 C29 C30 -80.9(6) . C28 C24 C25 C26 -6.2(7) . C29 N4 C26 C25 -173.8(4) . C29 N4 C27 C28 171.5(4) . C29 C30 C31 C32 -171.3(4) . C29 C30 C35 C34 172.2(4) . C30 C31 C32 C33 -1.6(7) . C31 C30 C35 C34 -4.3(7) . C31 C32 C33 C34 -2.8(7) . C31 C32 C33 C36 173.1(4) . C32 C33 C34 C35 3.6(7) . C32 C33 C36 N1 -91.4(5) . C33 C34 C35 C30 -0.1(7) . C34 C33 C36 N1 84.4(6) . C35 C30 C31 C32 5.2(7) . C36 N1 C1 C2 -171.5(4) . C36 N1 C5 C4 170.9(5) . C36 C33 C34 C35 -172.2(5) . loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 0.000 0.000 0.000 139.7 34.3 2 -0.730 0.000 0.500 676.8 247.6 3 0.358 0.494 0.432 9.9 10.3 4 0.642 0.506 0.568 9.9 10.4