# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_HAK55 #TrackingRef 'HAK55_cifdep_Roisnel.cif' _audit_creation_date 2012-02-24T17:50:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H68 Cl2 N4 Zn' _chemical_formula_sum 'C60 H68 Cl2 N4 Zn' _chemical_formula_weight 981.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.239(3) _cell_length_b 26.022(3) _cell_length_c 15.3824(15) _cell_angle_alpha 90 _cell_angle_beta 101.558(6) _cell_angle_gamma 90 _cell_volume 10682(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5083 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 19.54 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.947 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.146 0.473 0.030 30 2 ' ' 2 0.353 1.027 -0.030 30 2 ' ' 3 0.646 0.973 0.030 30 2 ' ' 4 0.853 0.527 -0.030 30 2 ' ' 5 0.000 0.056 0.250 89 16 ' ' 6 0.500 0.556 0.250 89 16 ' ' 7 0.353 0.973 0.470 30 2 ' ' 8 0.853 0.473 0.470 30 2 ' ' 9 0.146 0.527 0.529 30 2 ' ' 10 0.646 1.027 0.529 30 2 ' ' 11 0.000 0.944 0.750 89 16 ' ' 12 0.500 0.444 0.750 89 16 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_unetI/netI 0.1063 _diffrn_reflns_number 52855 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 12142 _reflns_number_gt 4847 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12142 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2031 _refine_ls_R_factor_gt 0.1049 _refine_ls_wR_factor_ref 0.354 _refine_ls_wR_factor_gt 0.3045 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.317 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.098 _iucr_refine_instructions_details ; .res file for SHELXL : sqz.res ................................................................. TITL import in C 2/c CELL 0.71073 27.2390 26.0220 15.3824 90.000 101.558 90.000 ZERR 8.00 0.0030 0.0030 0.0015 0.000 0.006 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N CL ZN UNIT 480.00 544.00 32.00 16.00 8.00 MERG 2 EXYZ C21A C21B EXYZ C28A C28B EADP C1 > C5 eadp C21a > c29b EADP C51 c52 c53 c71 c55 c54 c56 c57 EADP C58 > c63 EADP C74 > C79 eadp C32A C32b eadp c33a c34a c33b c34b EADP C31A C31B EXYZ C31A C31B EXYZ C33a c33b EADP C17A C17B C18A C18B FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 1 WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.196600 FVAR 0.55281 MOLE 1 ZN1 5 0.367849 0.166389 0.628796 11.00000 0.06458 0.05717 = 0.05350 -0.00103 0.01178 -0.01212 CL1 4 0.336097 0.131269 0.497347 11.00000 0.07342 0.08465 = 0.06808 -0.02483 0.00256 0.00790 CL2 4 0.356365 0.125840 0.750216 11.00000 0.04685 0.06724 = 0.07813 0.02736 0.01197 -0.00179 C1 1 0.438428 0.195061 0.637396 11.00000 0.06995 0.09113 = 0.03496 0.00931 0.00815 -0.02615 C2 1 0.443249 0.246473 0.637826 11.00000 0.06995 0.09113 = 0.03496 0.00931 0.00815 -0.02615 C3 1 0.482858 0.274377 0.637712 11.00000 0.06995 0.09113 = 0.03496 0.00931 0.00815 -0.02615 AFIX 43 H3 2 0.481540 0.310847 0.635647 11.00000 -1.20000 AFIX 0 C4 1 0.482153 0.168178 0.640162 11.00000 0.06995 0.09113 = 0.03496 0.00931 0.00815 -0.02615 C5 1 0.526801 0.195972 0.643712 11.00000 0.06995 0.09113 = 0.03496 0.00931 0.00815 -0.02615 AFIX 43 H5 2 0.557909 0.178657 0.648143 11.00000 -1.20000 AFIX 0 C6 1 0.476921 0.111961 0.636382 11.00000 0.06256 0.11417 = 0.04807 0.02335 0.01229 0.01073 AFIX 43 H6 2 0.445465 0.097404 0.640375 11.00000 -1.20000 AFIX 0 C7 1 0.514406 0.080225 0.627569 11.00000 0.06689 0.11595 = 0.04366 0.02579 0.01034 0.01329 AFIX 43 H7 2 0.545469 0.095754 0.623769 11.00000 -1.20000 AFIX 0 C8 1 0.512281 0.024627 0.623260 11.00000 0.06692 0.15482 = 0.04227 0.03629 0.01572 0.02935 C9 1 0.469723 -0.004273 0.634958 11.00000 0.07379 0.12671 = 0.05833 0.03144 0.03140 0.03950 AFIX 43 H9 2 0.441585 0.013743 0.647385 11.00000 -1.20000 AFIX 0 C10 1 0.467282 -0.057520 0.629106 11.00000 0.08729 0.12856 = 0.05746 0.04077 0.02967 0.03040 AFIX 43 H10 2 0.438033 -0.075106 0.637551 11.00000 -1.20000 AFIX 0 C11 1 0.509377 -0.086009 0.610140 11.00000 0.09570 0.13181 = 0.06021 0.03218 0.03882 0.05394 C12 1 0.551450 -0.060113 0.598277 11.00000 0.09140 0.13723 = 0.06538 0.03504 0.02865 0.05527 AFIX 43 H12 2 0.579517 -0.078458 0.586321 11.00000 -1.20000 AFIX 0 C13 1 0.552621 -0.005866 0.604022 11.00000 0.06526 0.20030 = 0.03851 0.03605 0.00954 0.03683 AFIX 43 H13 2 0.581849 0.011370 0.594579 11.00000 -1.20000 AFIX 0 N14 3 0.507679 -0.138709 0.602673 11.00000 0.11364 0.13953 = 0.09878 0.05375 0.06506 0.05420 C15 1 0.470188 -0.167151 0.632543 11.00000 0.11328 0.13069 = 0.08396 0.04074 0.03753 0.04834 AFIX 23 H15A 2 0.460481 -0.148940 0.683038 11.00000 -1.20000 H15B 2 0.483850 -0.201130 0.654013 11.00000 -1.20000 AFIX 0 C16 1 0.422835 -0.174995 0.557883 11.00000 0.16463 0.08812 = 0.12133 0.02437 0.06988 0.02977 AFIX 33 H16A 2 0.397361 -0.193912 0.581733 11.00000 -1.50000 H16B 2 0.431958 -0.194564 0.509039 11.00000 -1.50000 H16C 2 0.409420 -0.141440 0.535948 11.00000 -1.50000 AFIX 0 PART 1 C17A 1 0.556184 -0.158572 0.594144 10.50000 0.10533 0.10906 = 0.06967 0.02168 0.02300 0.01821 AFIX 23 H17A 2 0.568625 -0.136799 0.550396 10.50000 -1.20000 H17B 2 0.550819 -0.193407 0.568100 10.50000 -1.20000 AFIX 0 C18A 1 0.599148 -0.162539 0.678489 10.50000 0.10533 0.10906 = 0.06967 0.02168 0.02300 0.01821 AFIX 33 H18A 2 0.629447 -0.176174 0.661602 10.50000 -1.50000 H18B 2 0.588714 -0.185569 0.721833 10.50000 -1.50000 H18C 2 0.606155 -0.128354 0.704783 10.50000 -1.50000 AFIX 0 PART 2 C17B 1 0.543719 -0.175487 0.585268 10.50000 0.10533 0.10906 = 0.06967 0.02168 0.02300 0.01821 AFIX 23 H17C 2 0.561983 -0.161904 0.540659 10.50000 -1.20000 H17D 2 0.526886 -0.207890 0.562426 10.50000 -1.20000 AFIX 0 C18B 1 0.580735 -0.185117 0.675636 10.50000 0.10533 0.10906 = 0.06967 0.02168 0.02300 0.01821 AFIX 33 H18D 2 0.605903 -0.210541 0.667168 10.50000 -1.50000 H18E 2 0.562053 -0.198007 0.719336 10.50000 -1.50000 H18F 2 0.597424 -0.152833 0.696981 10.50000 -1.50000 AFIX 0 PART 1 C21A 1 0.524441 0.249126 0.640609 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C22A 1 0.562507 0.294521 0.636854 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H22A 2 0.551296 0.329130 0.630009 10.50000 -1.20000 AFIX 0 C23A 1 0.611697 0.282673 0.643687 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H23A 2 0.621825 0.247885 0.653769 10.50000 -1.20000 AFIX 0 C24A 1 0.648180 0.319607 0.636493 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C25A 1 0.637983 0.370748 0.607092 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H25A 2 0.603816 0.380798 0.591580 10.50000 -1.20000 AFIX 0 C26A 1 0.675562 0.409248 0.598655 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H26A 2 0.666211 0.442278 0.574629 10.50000 -1.20000 AFIX 0 C27A 1 0.724364 0.396202 0.626354 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C28A 1 0.729661 0.344277 0.663672 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H28A 2 0.763288 0.334469 0.687237 10.50000 -1.20000 AFIX 0 C29A 1 0.698146 0.310705 0.670114 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H29A 2 0.708556 0.278920 0.698236 10.50000 -1.20000 AFIX 0 PART 2 C21B 1 0.524441 0.249126 0.640609 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C22B 1 0.579252 0.265870 0.644898 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H22B 2 0.606364 0.242217 0.653661 10.50000 -1.20000 AFIX 0 C23B 1 0.585051 0.313150 0.635887 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H23B 2 0.555304 0.333200 0.625932 10.50000 -1.20000 AFIX 0 C24B 1 0.632350 0.341930 0.638738 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C25B 1 0.630648 0.393058 0.617822 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H25B 2 0.598949 0.409083 0.599169 10.50000 -1.20000 AFIX 0 C26B 1 0.671489 0.420749 0.622703 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H26B 2 0.669002 0.456854 0.613750 10.50000 -1.20000 AFIX 0 C27B 1 0.722725 0.395111 0.642657 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 C28B 1 0.729661 0.344277 0.663672 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H28B 2 0.761091 0.327462 0.680466 10.50000 -1.20000 AFIX 0 C29B 1 0.677873 0.318836 0.655523 10.50000 0.08087 0.10820 = 0.04588 0.00300 0.00538 -0.03255 AFIX 43 H29B 2 0.677839 0.282611 0.663181 10.50000 -1.20000 AFIX 0 PART 0 N30 3 0.763665 0.427648 0.627674 11.00000 0.05299 0.14941 = 0.14413 0.02104 0.00034 -0.03225 PART 1 C31A 1 0.815815 0.413685 0.661958 10.50000 0.08045 0.13550 = 0.16388 -0.01414 -0.02362 0.01508 AFIX 23 H31A 2 0.831335 0.401858 0.612539 10.50000 -1.20000 H31B 2 0.817282 0.385059 0.704793 10.50000 -1.20000 AFIX 0 C32A 1 0.845270 0.460096 0.708166 10.50000 0.05053 0.33768 = 0.18271 -0.08692 0.01106 -0.02960 AFIX 33 H32A 2 0.879863 0.449740 0.732689 10.50000 -1.50000 H32B 2 0.829424 0.472258 0.756207 10.50000 -1.50000 H32C 2 0.845237 0.487779 0.664959 10.50000 -1.50000 AFIX 0 PART 2 C31B 1 0.815815 0.413685 0.661958 10.50000 0.08045 0.13550 = 0.16388 -0.01414 -0.02362 0.01508 AFIX 23 H31C 2 0.822281 0.377814 0.645978 10.50000 -1.20000 H31D 2 0.838696 0.436779 0.637826 10.50000 -1.20000 AFIX 0 C32B 1 0.822786 0.419389 0.757938 10.50000 0.05053 0.33768 = 0.18271 -0.08692 0.01106 -0.02960 AFIX 33 H32D 2 0.857251 0.410113 0.785577 10.50000 -1.50000 H32E 2 0.799385 0.396751 0.780362 10.50000 -1.50000 H32F 2 0.816408 0.455136 0.772391 10.50000 -1.50000 AFIX 0 PART 1 C33A 1 0.755366 0.474153 0.584225 10.50000 0.12789 0.06323 = 0.41986 0.00911 -0.01808 -0.02620 AFIX 23 H33A 2 0.730401 0.464516 0.530642 10.50000 -1.20000 H33B 2 0.787005 0.478810 0.562784 10.50000 -1.20000 AFIX 0 C34A 1 0.741128 0.528046 0.597517 10.50000 0.12789 0.06323 = 0.41986 0.00911 -0.01808 -0.02620 AFIX 33 H34A 2 0.741191 0.547768 0.543265 10.50000 -1.50000 H34B 2 0.765229 0.543149 0.646785 10.50000 -1.50000 H34C 2 0.707537 0.528904 0.611303 10.50000 -1.50000 AFIX 0 PART 2 C33B 1 0.755366 0.474153 0.584225 10.50000 0.12789 0.06323 = 0.41986 0.00911 -0.01808 -0.02620 AFIX 23 H33C 2 0.786003 0.485775 0.564590 10.50000 -1.20000 H33D 2 0.727899 0.471084 0.531533 10.50000 -1.20000 AFIX 0 C34B 1 0.743930 0.504673 0.637776 10.50000 0.12789 0.06323 = 0.41986 0.00911 -0.01808 -0.02620 AFIX 33 H34D 2 0.737160 0.538412 0.609618 10.50000 -1.50000 H34E 2 0.771617 0.507590 0.689160 10.50000 -1.50000 H34F 2 0.713890 0.492364 0.657271 10.50000 -1.50000 AFIX 0 PART 0 C51 1 0.353030 0.244165 0.630996 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 C52 1 0.393978 0.274821 0.635872 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 C53 1 0.393417 0.325035 0.636069 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 AFIX 43 H53 2 0.423680 0.343886 0.640420 11.00000 -1.20000 AFIX 0 C54 1 0.308536 0.267208 0.622889 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 C55 1 0.305048 0.320869 0.619764 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 AFIX 43 H55 2 0.273657 0.338022 0.611126 11.00000 -1.20000 AFIX 0 C56 1 0.264663 0.230807 0.621073 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 AFIX 43 H56 2 0.272809 0.195782 0.634154 11.00000 -1.20000 AFIX 0 C57 1 0.221048 0.241364 0.605010 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 AFIX 43 H57 2 0.212474 0.276322 0.592187 11.00000 -1.20000 AFIX 0 C58 1 0.178566 0.204213 0.603308 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 C59 1 0.133901 0.219922 0.576496 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 AFIX 43 H59 2 0.128100 0.254607 0.558003 11.00000 -1.20000 AFIX 0 C60 1 0.094486 0.187845 0.573959 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 AFIX 43 H60 2 0.061840 0.201837 0.555583 11.00000 -1.20000 AFIX 0 C61 1 0.098273 0.134193 0.596968 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 C62 1 0.146401 0.115277 0.628325 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 AFIX 43 H62 2 0.152131 0.080725 0.647645 11.00000 -1.20000 AFIX 0 C63 1 0.188426 0.152175 0.629930 11.00000 0.09892 0.11485 = 0.05510 -0.01442 0.00617 -0.01839 AFIX 43 H63 2 0.222045 0.140904 0.648850 11.00000 -1.20000 AFIX 0 N64 3 0.056390 0.104396 0.590760 11.00000 0.06876 0.08149 = 0.09000 0.01016 -0.00992 -0.00983 C65 1 0.059910 0.051825 0.612032 11.00000 0.06048 0.15063 = 0.10159 0.00771 -0.00709 -0.01062 AFIX 23 H65A 2 0.027414 0.039890 0.624086 11.00000 -1.20000 H65B 2 0.085607 0.046927 0.666822 11.00000 -1.20000 AFIX 0 C66 1 0.073776 0.018838 0.537085 11.00000 0.11392 0.09572 = 0.18223 0.01011 -0.00065 -0.01560 AFIX 33 H66A 2 0.075978 -0.017347 0.555103 11.00000 -1.50000 H66B 2 0.106178 0.030132 0.525479 11.00000 -1.50000 H66C 2 0.047973 0.022788 0.483094 11.00000 -1.50000 AFIX 0 C67 1 0.007740 0.122880 0.546396 11.00000 0.07128 0.11078 = 0.14435 -0.02725 -0.02784 0.00246 AFIX 23 H67A 2 -0.012997 0.093283 0.520572 11.00000 -1.20000 H67B 2 0.011967 0.145797 0.497048 11.00000 -1.20000 AFIX 0 C68 1 -0.019377 0.151686 0.607546 11.00000 0.09046 0.17480 = 0.17463 -0.03124 0.01480 0.01372 AFIX 33 H68A 2 -0.052132 0.162987 0.574381 11.00000 -1.50000 H68B 2 0.000427 0.181716 0.631826 11.00000 -1.50000 H68C 2 -0.024061 0.129090 0.656199 11.00000 -1.50000 AFIX 0 C71 1 0.351422 0.348607 0.630303 11.00000 0.09387 0.07257 = 0.04174 -0.00728 0.01664 -0.02154 C72 1 0.351421 0.405977 0.633862 11.00000 0.15904 0.06903 = 0.05628 0.00672 0.03051 -0.03132 AFIX 43 H72 2 0.381307 0.422671 0.626348 11.00000 -1.20000 AFIX 0 C73 1 0.315516 0.435033 0.645934 11.00000 0.17534 0.05821 = 0.09626 -0.00221 0.06617 -0.00962 AFIX 43 H73 2 0.286960 0.417335 0.657333 11.00000 -1.20000 AFIX 0 C74 1 0.311151 0.492307 0.645034 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 C75 1 0.268180 0.515325 0.656218 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 AFIX 43 H75 2 0.240938 0.494989 0.666478 11.00000 -1.20000 AFIX 0 C76 1 0.263881 0.567833 0.652781 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 AFIX 43 H76 2 0.233656 0.583048 0.662108 11.00000 -1.20000 AFIX 0 C77 1 0.302318 0.600050 0.636039 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 C78 1 0.348825 0.576034 0.631940 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 AFIX 43 H78 2 0.376739 0.596640 0.625914 11.00000 -1.20000 AFIX 0 C79 1 0.353962 0.522621 0.636657 11.00000 0.11888 0.07109 = 0.10003 -0.01243 0.04674 -0.01683 AFIX 43 H79 2 0.385083 0.506743 0.634369 11.00000 -1.20000 AFIX 0 N80 3 0.297829 0.652435 0.628202 11.00000 0.08526 0.07067 = 0.09327 -0.01357 0.03241 -0.01211 C81 1 0.250966 0.678641 0.637561 11.00000 0.10842 0.09749 = 0.08749 -0.01010 0.02615 -0.00063 AFIX 23 H81A 2 0.258797 0.714551 0.656687 11.00000 -1.20000 H81B 2 0.237022 0.661278 0.684518 11.00000 -1.20000 AFIX 0 C82 1 0.211563 0.678903 0.552073 11.00000 0.11136 0.11874 = 0.10284 -0.01541 0.02021 -0.00359 AFIX 33 H82A 2 0.181412 0.696535 0.562186 11.00000 -1.50000 H82B 2 0.203141 0.643453 0.533302 11.00000 -1.50000 H82C 2 0.224759 0.696889 0.505677 11.00000 -1.50000 AFIX 0 C83 1 0.335291 0.685608 0.601244 11.00000 0.11300 0.05493 = 0.07346 0.00287 0.02734 -0.00905 AFIX 23 H83A 2 0.318556 0.715426 0.567830 11.00000 -1.20000 H83B 2 0.353306 0.666355 0.561762 11.00000 -1.20000 AFIX 0 C84 1 0.371502 0.703898 0.680352 11.00000 0.15657 0.09780 = 0.07871 -0.01055 0.03658 -0.05895 AFIX 33 H84A 2 0.396717 0.725771 0.661443 11.00000 -1.50000 H84B 2 0.388016 0.674320 0.713309 11.00000 -1.50000 H84C 2 0.353701 0.723689 0.718581 11.00000 -1.50000 HKLF 4 REM import in C 2/c REM R1 = 0.1049 for 4847 Fo > 4sig(Fo) and 0.2031 for all 12142 data REM 451 parameters refined using 0 restraints END WGHT 0.1966 0.0000 REM Highest difference peak 1.32, deepest hole -0.84, 1-sigma level 0.10 Q1 1 0.2472 0.1999 0.6324 11.00000 0.05 1.21 Q2 1 0.2014 0.1710 0.6163 11.00000 0.05 0.81 Q3 1 0.8064 0.5023 0.5828 11.00000 0.05 0.80 Q4 1 0.3803 0.1631 0.5844 11.00000 0.05 0.77 Q5 1 0.1995 0.1175 0.6481 11.00000 0.05 0.75 Q6 1 0.1560 0.1932 0.5778 11.00000 0.05 0.71 Q7 1 0.4940 0.2609 0.6441 11.00000 0.05 0.71 Q8 1 0.2564 0.2595 0.5984 11.00000 0.05 0.68 Q9 1 0.5391 0.2242 0.6439 11.00000 0.05 0.60 Q10 1 0.3262 0.3397 0.6200 11.00000 0.05 0.59 Q11 1 0.5329 0.1679 0.6391 11.00000 0.05 0.55 Q12 1 0.4096 0.2568 0.6209 11.00000 0.05 0.48 Q13 1 0.7137 0.4229 0.6811 11.00000 0.05 0.45 Q14 1 0.7542 0.4568 0.6939 11.00000 0.05 0.44 Q15 1 0.6636 0.4395 0.6663 11.00000 0.05 0.39 Q16 1 0.5833 0.3231 0.6526 11.00000 0.05 0.38 Q17 1 0.1146 0.1708 0.5638 11.00000 0.05 0.38 Q18 1 0.3710 0.1193 0.6967 11.00000 0.05 0.37 Q19 1 0.5329 0.4328 0.6871 11.00000 0.05 0.37 Q20 1 0.6273 0.3594 0.6563 11.00000 0.05 0.37 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 '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_ _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.36785(3) 0.16639(3) 0.62880(5) 0.0584(3) Uani 1 1 d . . . Cl1 Cl 0.33610(7) 0.13127(7) 0.49735(12) 0.0770(6) Uani 1 1 d . . . Cl2 Cl 0.35637(6) 0.12584(6) 0.75022(11) 0.0641(5) Uani 1 1 d . . . C1 C 0.4384(3) 0.1951(3) 0.6374(4) 0.0657(9) Uani 1 1 d . . . C2 C 0.4432(3) 0.2465(3) 0.6378(4) 0.0657(9) Uani 1 1 d . D . C3 C 0.4829(3) 0.2744(3) 0.6377(4) 0.0657(9) Uani 1 1 d . . . H3 H 0.4815 0.3108 0.6356 0.079 Uiso 1 1 calc R A 1 C4 C 0.4822(3) 0.1682(3) 0.6402(4) 0.0657(9) Uani 1 1 d . D . C5 C 0.5268(3) 0.1960(3) 0.6437(4) 0.0657(9) Uani 1 1 d . . . H5 H 0.5579 0.1787 0.6481 0.079 Uiso 1 1 calc R B 1 C6 C 0.4769(3) 0.1120(3) 0.6364(4) 0.075(2) Uani 1 1 d . . . H6 H 0.4455 0.0974 0.6404 0.09 Uiso 1 1 calc R D . C7 C 0.5144(3) 0.0802(4) 0.6276(4) 0.076(2) Uani 1 1 d . D . H7 H 0.5455 0.0958 0.6238 0.091 Uiso 1 1 calc R . . C8 C 0.5123(3) 0.0246(4) 0.6233(4) 0.087(3) Uani 1 1 d . . . C9 C 0.4697(3) -0.0043(4) 0.6350(5) 0.084(2) Uani 1 1 d . D . H9 H 0.4416 0.0137 0.6474 0.1 Uiso 1 1 calc R . . C10 C 0.4673(3) -0.0575(4) 0.6291(5) 0.089(3) Uani 1 1 d . . . H10 H 0.438 -0.0751 0.6376 0.107 Uiso 1 1 calc R D . C11 C 0.5094(4) -0.0860(4) 0.6101(5) 0.093(3) Uani 1 1 d . C . C12 C 0.5515(4) -0.0601(4) 0.5983(5) 0.096(3) Uani 1 1 d . . . H12 H 0.5795 -0.0785 0.5863 0.115 Uiso 1 1 calc R D . C13 C 0.5526(3) -0.0059(5) 0.6040(4) 0.101(3) Uani 1 1 d . D . H13 H 0.5818 0.0114 0.5946 0.122 Uiso 1 1 calc R . . N14 N 0.5077(3) -0.1387(4) 0.6027(5) 0.111(3) Uani 1 1 d . . . C15 C 0.4702(4) -0.1672(4) 0.6325(6) 0.107(3) Uani 1 1 d . C . H15A H 0.4605 -0.1489 0.683 0.128 Uiso 1 1 calc R . . H15B H 0.4838 -0.2011 0.654 0.128 Uiso 1 1 calc R . . C16 C 0.4228(4) -0.1750(3) 0.5579(7) 0.119(4) Uani 1 1 d . . . H16A H 0.3974 -0.1939 0.5817 0.178 Uiso 1 1 calc R C . H16B H 0.432 -0.1946 0.509 0.178 Uiso 1 1 calc R . . H16C H 0.4094 -0.1414 0.5359 0.178 Uiso 1 1 calc R . . C17A C 0.5562(15) -0.1586(14) 0.594(3) 0.094(6) Uani 0.5 1 d P C 1 H17A H 0.5686 -0.1368 0.5504 0.113 Uiso 0.5 1 calc PR C 1 H17B H 0.5508 -0.1934 0.5681 0.113 Uiso 0.5 1 calc PR C 1 C18A C 0.5991(11) -0.1625(10) 0.6785(18) 0.094(6) Uani 0.5 1 d P C 1 H18A H 0.6294 -0.1762 0.6616 0.141 Uiso 0.5 1 calc PR C 1 H18B H 0.5887 -0.1856 0.7218 0.141 Uiso 0.5 1 calc PR C 1 H18C H 0.6062 -0.1284 0.7048 0.141 Uiso 0.5 1 calc PR C 1 C17B C 0.5437(16) -0.1755(13) 0.585(3) 0.094(6) Uani 0.5 1 d P C 2 H17C H 0.562 -0.1619 0.5407 0.113 Uiso 0.5 1 calc PR C 2 H17D H 0.5269 -0.2079 0.5624 0.113 Uiso 0.5 1 calc PR C 2 C18B C 0.5807(10) -0.1851(10) 0.6756(16) 0.094(6) Uani 0.5 1 d P C 2 H18D H 0.6059 -0.2105 0.6672 0.141 Uiso 0.5 1 calc PR C 2 H18E H 0.5621 -0.198 0.7193 0.141 Uiso 0.5 1 calc PR C 2 H18F H 0.5974 -0.1528 0.697 0.141 Uiso 0.5 1 calc PR C 2 C21A C 0.5244(3) 0.2491(3) 0.6406(4) 0.0793(11) Uani 0.5 1 d P D 1 C22A C 0.5625(6) 0.2945(8) 0.6369(10) 0.0793(11) Uani 0.5 1 d P D 1 H22A H 0.5513 0.3291 0.63 0.095 Uiso 0.5 1 calc PR D 1 C23A C 0.6117(6) 0.2827(8) 0.6437(9) 0.0793(11) Uani 0.5 1 d P D 1 H23A H 0.6218 0.2479 0.6538 0.095 Uiso 0.5 1 calc PR D 1 C24A C 0.6482(8) 0.3196(7) 0.6365(11) 0.0793(11) Uani 0.5 1 d P D 1 C25A C 0.6380(7) 0.3707(7) 0.6071(11) 0.0793(11) Uani 0.5 1 d P D 1 H25A H 0.6038 0.3808 0.5916 0.095 Uiso 0.5 1 calc PR D 1 C26A C 0.6756(8) 0.4092(8) 0.5987(10) 0.0793(11) Uani 0.5 1 d P D 1 H26A H 0.6662 0.4423 0.5746 0.095 Uiso 0.5 1 calc PR D 1 C27A C 0.7244(12) 0.3962(13) 0.6264(12) 0.0793(11) Uani 0.5 1 d P D 1 C28A C 0.7297(3) 0.3443(3) 0.6637(4) 0.0793(11) Uani 0.5 1 d P D 1 H28A H 0.7633 0.3345 0.6872 0.095 Uiso 0.5 1 calc PR D 1 C29A C 0.6981(6) 0.3107(8) 0.6701(10) 0.0793(11) Uani 0.5 1 d P D 1 H29A H 0.7086 0.2789 0.6982 0.095 Uiso 0.5 1 calc PR D 1 C21B C 0.5244(3) 0.2491(3) 0.6406(4) 0.0793(11) Uani 0.5 1 d P D 2 C22B C 0.5793(7) 0.2659(7) 0.6449(9) 0.0793(11) Uani 0.5 1 d P D 2 H22B H 0.6064 0.2422 0.6537 0.095 Uiso 0.5 1 calc PR D 2 C23B C 0.5851(8) 0.3131(8) 0.6359(9) 0.0793(11) Uani 0.5 1 d P D 2 H23B H 0.5553 0.3332 0.6259 0.095 Uiso 0.5 1 calc PR D 2 C24B C 0.6324(7) 0.3419(8) 0.6387(11) 0.0793(11) Uani 0.5 1 d P D 2 C25B C 0.6306(7) 0.3931(7) 0.6178(10) 0.0793(11) Uani 0.5 1 d P D 2 H25B H 0.5989 0.4091 0.5992 0.095 Uiso 0.5 1 calc PR D 2 C26B C 0.6715(8) 0.4207(9) 0.6227(10) 0.0793(11) Uani 0.5 1 d P D 2 H26B H 0.669 0.4569 0.6137 0.095 Uiso 0.5 1 calc PR D 2 C27B C 0.7227(12) 0.3951(14) 0.6427(12) 0.0793(11) Uani 0.5 1 d P D 2 C28B C 0.7297(3) 0.3443(3) 0.6637(4) 0.0793(11) Uani 0.5 1 d P D 2 H28B H 0.7611 0.3275 0.6805 0.095 Uiso 0.5 1 calc PR D 2 C29B C 0.6779(7) 0.3188(8) 0.6555(11) 0.0793(11) Uani 0.5 1 d P D 2 H29B H 0.6778 0.2826 0.6632 0.095 Uiso 0.5 1 calc PR D 2 N30 N 0.7637(2) 0.4276(4) 0.6277(6) 0.118(3) Uani 1 1 d . . . C31A C 0.8158(3) 0.4137(4) 0.6620(9) 0.133(4) Uani 0.5 1 d P D 1 H31A H 0.8313 0.4019 0.6125 0.16 Uiso 0.5 1 calc PR D 1 H31B H 0.8173 0.3851 0.7048 0.16 Uiso 0.5 1 calc PR D 1 C32A C 0.8453(7) 0.4601(13) 0.7082(19) 0.192(12) Uani 0.5 1 d P D 1 H32A H 0.8799 0.4497 0.7327 0.288 Uiso 0.5 1 calc PR D 1 H32B H 0.8294 0.4723 0.7562 0.288 Uiso 0.5 1 calc PR D 1 H32C H 0.8452 0.4878 0.665 0.288 Uiso 0.5 1 calc PR D 1 C31B C 0.8158(3) 0.4137(4) 0.6620(9) 0.133(4) Uani 0.5 1 d P D 2 H31C H 0.8223 0.3778 0.646 0.16 Uiso 0.5 1 calc PR D 2 H31D H 0.8387 0.4368 0.6378 0.16 Uiso 0.5 1 calc PR D 2 C32B C 0.8228(7) 0.4194(14) 0.758(2) 0.192(12) Uani 0.5 1 d P D 2 H32D H 0.8573 0.4101 0.7856 0.288 Uiso 0.5 1 calc PR D 2 H32E H 0.7994 0.3968 0.7804 0.288 Uiso 0.5 1 calc PR D 2 H32F H 0.8164 0.4551 0.7724 0.288 Uiso 0.5 1 calc PR D 2 C33A C 0.7554(5) 0.4742(5) 0.5842(15) 0.214(8) Uani 0.5 1 d P D 1 H33A H 0.7304 0.4645 0.5306 0.257 Uiso 0.5 1 calc PR D 1 H33B H 0.787 0.4788 0.5628 0.257 Uiso 0.5 1 calc PR D 1 C34A C 0.7411(11) 0.5280(8) 0.598(3) 0.214(8) Uani 0.5 1 d P D 1 H34A H 0.7412 0.5478 0.5433 0.321 Uiso 0.5 1 calc PR D 1 H34B H 0.7652 0.5431 0.6468 0.321 Uiso 0.5 1 calc PR D 1 H34C H 0.7075 0.5289 0.6113 0.321 Uiso 0.5 1 calc PR D 1 C33B C 0.7554(5) 0.4742(5) 0.5842(15) 0.214(8) Uani 0.5 1 d P D 2 H33C H 0.786 0.4858 0.5646 0.257 Uiso 0.5 1 calc PR D 2 H33D H 0.7279 0.4711 0.5315 0.257 Uiso 0.5 1 calc PR D 2 C34B C 0.7439(12) 0.5047(11) 0.638(3) 0.214(8) Uani 0.5 1 d P D 2 H34D H 0.7372 0.5384 0.6096 0.321 Uiso 0.5 1 calc PR D 2 H34E H 0.7716 0.5076 0.6892 0.321 Uiso 0.5 1 calc PR D 2 H34F H 0.7139 0.4924 0.6573 0.321 Uiso 0.5 1 calc PR D 2 C51 C 0.3530(3) 0.2442(3) 0.6310(4) 0.0690(7) Uani 1 1 d . D . C52 C 0.3940(3) 0.2748(3) 0.6359(4) 0.0690(7) Uani 1 1 d . . . C53 C 0.3934(3) 0.3250(3) 0.6361(4) 0.0690(7) Uani 1 1 d . D . H53 H 0.4237 0.3439 0.6404 0.083 Uiso 1 1 calc R . . C54 C 0.3085(3) 0.2672(3) 0.6229(4) 0.0690(7) Uani 1 1 d . . . C55 C 0.3050(3) 0.3209(3) 0.6198(4) 0.0690(7) Uani 1 1 d . D . H55 H 0.2737 0.338 0.6111 0.083 Uiso 1 1 calc R . . C56 C 0.2647(3) 0.2308(3) 0.6211(4) 0.0690(7) Uani 1 1 d . D . H56 H 0.2728 0.1958 0.6342 0.083 Uiso 1 1 calc R . . C57 C 0.2210(3) 0.2414(3) 0.6050(4) 0.0690(7) Uani 1 1 d . . . H57 H 0.2125 0.2763 0.5922 0.083 Uiso 1 1 calc R D . C58 C 0.1786(3) 0.2042(4) 0.6033(5) 0.0909(11) Uani 1 1 d . D . C59 C 0.1339(3) 0.2199(4) 0.5765(5) 0.0909(11) Uani 1 1 d . . . H59 H 0.1281 0.2546 0.558 0.109 Uiso 1 1 calc R D . C60 C 0.0945(4) 0.1878(4) 0.5740(5) 0.0909(11) Uani 1 1 d . D . H60 H 0.0618 0.2018 0.5556 0.109 Uiso 1 1 calc R . . C61 C 0.0983(3) 0.1342(4) 0.5970(5) 0.0909(11) Uani 1 1 d . . . C62 C 0.1464(3) 0.1153(4) 0.6283(5) 0.0909(11) Uani 1 1 d . D . H62 H 0.1521 0.0807 0.6476 0.109 Uiso 1 1 calc R . . C63 C 0.1884(3) 0.1522(4) 0.6299(5) 0.0909(11) Uani 1 1 d . . . H63 H 0.222 0.1409 0.6489 0.109 Uiso 1 1 calc R D . N64 N 0.0564(2) 0.1044(3) 0.5908(4) 0.0837(19) Uani 1 1 d . D . C65 C 0.0599(3) 0.0518(4) 0.6120(6) 0.107(3) Uani 1 1 d . . . H65A H 0.0274 0.0399 0.6241 0.129 Uiso 1 1 calc R D . H65B H 0.0856 0.0469 0.6668 0.129 Uiso 1 1 calc R . . C66 C 0.0738(4) 0.0188(4) 0.5371(9) 0.135(4) Uani 1 1 d . D . H66A H 0.076 -0.0173 0.5551 0.202 Uiso 1 1 calc R . . H66B H 0.1062 0.0301 0.5255 0.202 Uiso 1 1 calc R . . H66C H 0.048 0.0228 0.4831 0.202 Uiso 1 1 calc R . . C67 C 0.0077(3) 0.1229(4) 0.5464(7) 0.116(4) Uani 1 1 d . . . H67A H -0.013 0.0933 0.5206 0.139 Uiso 1 1 calc R D . H67B H 0.012 0.1458 0.497 0.139 Uiso 1 1 calc R . . C68 C -0.0194(4) 0.1517(5) 0.6075(9) 0.148(5) Uani 1 1 d . D . H68A H -0.0521 0.163 0.5744 0.222 Uiso 1 1 calc R . . H68B H 0.0004 0.1817 0.6318 0.222 Uiso 1 1 calc R . . H68C H -0.0241 0.1291 0.6562 0.222 Uiso 1 1 calc R . . C71 C 0.3514(3) 0.3486(3) 0.6303(4) 0.0690(7) Uani 1 1 d . . . C72 C 0.3514(4) 0.4060(3) 0.6339(5) 0.094(3) Uani 1 1 d . D . H72 H 0.3813 0.4227 0.6263 0.112 Uiso 1 1 calc R . . C73 C 0.3155(5) 0.4350(3) 0.6459(6) 0.105(3) Uani 1 1 d . . . H73 H 0.287 0.4173 0.6573 0.125 Uiso 1 1 calc R D . C74 C 0.3112(4) 0.4923(3) 0.6450(6) 0.0932(11) Uani 1 1 d . D . C75 C 0.2682(4) 0.5153(3) 0.6562(6) 0.0932(11) Uani 1 1 d . . . H75 H 0.2409 0.495 0.6665 0.112 Uiso 1 1 calc R D . C76 C 0.2639(4) 0.5678(3) 0.6528(6) 0.0932(11) Uani 1 1 d . D . H76 H 0.2337 0.583 0.6621 0.112 Uiso 1 1 calc R . . C77 C 0.3023(4) 0.6001(3) 0.6360(6) 0.0932(11) Uani 1 1 d . . . C78 C 0.3488(4) 0.5760(3) 0.6319(5) 0.0932(11) Uani 1 1 d . D . H78 H 0.3767 0.5966 0.6259 0.112 Uiso 1 1 calc R . . C79 C 0.3540(4) 0.5226(3) 0.6367(5) 0.0932(11) Uani 1 1 d . . . H79 H 0.3851 0.5067 0.6344 0.112 Uiso 1 1 calc R D . N80 N 0.2978(3) 0.6524(2) 0.6282(4) 0.0810(18) Uani 1 1 d . D . C81 C 0.2510(4) 0.6786(3) 0.6376(6) 0.097(3) Uani 1 1 d . . . H81A H 0.2588 0.7146 0.6567 0.116 Uiso 1 1 calc R D . H81B H 0.237 0.6613 0.6845 0.116 Uiso 1 1 calc R . . C82 C 0.2116(4) 0.6789(4) 0.5521(6) 0.111(3) Uani 1 1 d . D . H82A H 0.1814 0.6965 0.5622 0.167 Uiso 1 1 calc R . . H82B H 0.2031 0.6435 0.5333 0.167 Uiso 1 1 calc R . . H82C H 0.2248 0.6969 0.5057 0.167 Uiso 1 1 calc R . . C83 C 0.3353(3) 0.6856(3) 0.6012(5) 0.079(2) Uani 1 1 d . . . H83A H 0.3186 0.7154 0.5678 0.095 Uiso 1 1 calc R D . H83B H 0.3533 0.6664 0.5618 0.095 Uiso 1 1 calc R . . C84 C 0.3715(4) 0.7039(3) 0.6804(6) 0.109(3) Uani 1 1 d . D . H84A H 0.3967 0.7258 0.6614 0.164 Uiso 1 1 calc R . . H84B H 0.388 0.6743 0.7133 0.164 Uiso 1 1 calc R . . H84C H 0.3537 0.7237 0.7186 0.164 Uiso 1 1 calc R . . 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 Zn1 0.0646(5) 0.0572(5) 0.0535(5) -0.0010(3) 0.0118(4) -0.0121(4) Cl1 0.0734(11) 0.0847(13) 0.0681(11) -0.0248(9) 0.0026(9) 0.0079(10) Cl2 0.0468(8) 0.0672(10) 0.0781(11) 0.0274(8) 0.0120(8) -0.0018(7) C1 0.0700(18) 0.091(2) 0.0350(14) 0.0093(15) 0.0081(14) -0.0261(18) C2 0.0700(18) 0.091(2) 0.0350(14) 0.0093(15) 0.0081(14) -0.0261(18) C3 0.0700(18) 0.091(2) 0.0350(14) 0.0093(15) 0.0081(14) -0.0261(18) C4 0.0700(18) 0.091(2) 0.0350(14) 0.0093(15) 0.0081(14) -0.0261(18) C5 0.0700(18) 0.091(2) 0.0350(14) 0.0093(15) 0.0081(14) -0.0261(18) C6 0.063(4) 0.114(6) 0.048(4) 0.023(4) 0.012(3) 0.011(4) C7 0.067(5) 0.116(7) 0.044(4) 0.026(4) 0.010(3) 0.013(5) C8 0.067(5) 0.155(9) 0.042(4) 0.036(5) 0.016(3) 0.029(5) C9 0.074(5) 0.127(8) 0.058(4) 0.031(5) 0.031(4) 0.040(5) C10 0.087(5) 0.129(8) 0.057(4) 0.041(5) 0.030(4) 0.030(6) C11 0.096(6) 0.132(8) 0.060(5) 0.032(5) 0.039(4) 0.054(6) C12 0.091(6) 0.137(9) 0.065(5) 0.035(5) 0.029(5) 0.055(6) C13 0.065(5) 0.200(11) 0.039(4) 0.036(5) 0.010(4) 0.037(6) N14 0.114(6) 0.140(7) 0.099(5) 0.054(5) 0.065(5) 0.054(6) C15 0.113(7) 0.131(8) 0.084(6) 0.041(6) 0.038(6) 0.048(6) C16 0.165(10) 0.088(7) 0.121(8) 0.024(6) 0.070(8) 0.030(7) C17A 0.105(16) 0.109(17) 0.070(5) 0.022(10) 0.023(9) 0.018(10) C18A 0.105(16) 0.109(17) 0.070(5) 0.022(10) 0.023(9) 0.018(10) C17B 0.105(16) 0.109(17) 0.070(5) 0.022(10) 0.023(9) 0.018(10) C18B 0.105(16) 0.109(17) 0.070(5) 0.022(10) 0.023(9) 0.018(10) C21A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C22A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C23A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C24A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C25A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C26A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C27A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C28A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C29A 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C21B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C22B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C23B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C24B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C25B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C26B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C27B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C28B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) C29B 0.081(2) 0.108(3) 0.0459(17) 0.0030(19) 0.0054(18) -0.033(2) N30 0.053(4) 0.149(8) 0.144(7) 0.021(6) 0.000(4) -0.032(5) C31A 0.080(6) 0.136(9) 0.164(11) -0.014(8) -0.024(7) 0.015(6) C32A 0.051(9) 0.34(4) 0.18(2) -0.09(2) 0.011(10) -0.030(12) C31B 0.080(6) 0.136(9) 0.164(11) -0.014(8) -0.024(7) 0.015(6) C32B 0.051(9) 0.34(4) 0.18(2) -0.09(2) 0.011(10) -0.030(12) C33A 0.128(8) 0.063(7) 0.42(2) 0.009(11) -0.018(11) -0.026(7) C34A 0.128(8) 0.063(7) 0.42(2) 0.009(11) -0.018(11) -0.026(7) C33B 0.128(8) 0.063(7) 0.42(2) 0.009(11) -0.018(11) -0.026(7) C34B 0.128(8) 0.063(7) 0.42(2) 0.009(11) -0.018(11) -0.026(7) C51 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C52 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C53 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C54 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C55 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C56 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C57 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C58 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) C59 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) C60 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) C61 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) C62 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) C63 0.099(2) 0.115(3) 0.0551(18) -0.0144(19) 0.0062(18) -0.018(2) N64 0.069(4) 0.081(5) 0.090(5) 0.010(4) -0.010(3) -0.010(4) C65 0.060(5) 0.151(10) 0.102(7) 0.008(7) -0.007(5) -0.011(6) C66 0.114(8) 0.096(8) 0.182(12) 0.010(8) -0.001(8) -0.016(6) C67 0.071(5) 0.111(7) 0.144(9) -0.027(6) -0.028(6) 0.002(5) C68 0.090(7) 0.175(12) 0.175(12) -0.031(10) 0.015(8) 0.014(8) C71 0.0939(17) 0.0726(17) 0.0417(12) -0.0073(12) 0.0166(14) -0.0215(15) C72 0.159(9) 0.069(5) 0.056(4) 0.007(4) 0.031(5) -0.031(6) C73 0.175(10) 0.058(5) 0.096(6) -0.002(4) 0.066(7) -0.010(6) C74 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) C75 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) C76 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) C77 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) C78 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) C79 0.119(3) 0.071(2) 0.100(2) -0.012(2) 0.047(2) -0.017(2) N80 0.085(4) 0.071(4) 0.093(5) -0.014(3) 0.032(4) -0.012(4) C81 0.108(7) 0.097(6) 0.087(6) -0.010(5) 0.026(6) -0.001(5) C82 0.111(7) 0.119(8) 0.103(7) -0.015(6) 0.020(6) -0.004(6) C83 0.113(6) 0.055(4) 0.073(5) 0.003(4) 0.027(5) -0.009(4) C84 0.157(9) 0.098(7) 0.079(6) -0.011(5) 0.037(6) -0.059(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Zn1 C1 2.042(7) . ? Zn1 C51 2.065(8) . ? Zn1 Cl2 2.2212(17) . ? Zn1 Cl1 2.2296(18) . ? C1 C2 1.344(10) . ? C1 C4 1.375(10) . ? C2 C3 1.301(8) . ? C2 C52 1.526(10) . ? C3 C21A 1.302(10) . ? C3 H3 0.95 . ? C4 C5 1.407(9) . ? C4 C6 1.470(10) . ? C5 C21A 1.385(11) . ? C5 H5 0.95 . ? C6 C7 1.341(10) . ? C6 H6 0.95 . ? C7 C8 1.449(12) . ? C7 H7 0.95 . ? C8 C9 1.423(12) . ? C8 C13 1.433(11) . ? C9 C10 1.389(12) . ? C9 H9 0.95 . ? C10 C11 1.443(11) . ? C10 H10 0.95 . ? C11 C12 1.373(13) . ? C11 N14 1.376(12) . ? C12 C13 1.414(13) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? N14 C15 1.411(12) . ? N14 C17B 1.43(5) . ? N14 C17A 1.45(5) . ? C15 C16 1.559(14) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17A C18A 1.57(3) . ? C17A H17A 0.99 . ? C17A H17B 0.99 . ? C18A H18A 0.98 . ? C18A H18B 0.98 . ? C18A H18C 0.98 . ? C17B C18B 1.57(3) . ? C17B H17C 0.99 . ? C17B H17D 0.99 . ? C18B H18D 0.98 . ? C18B H18E 0.98 . ? C18B H18F 0.98 . ? C21A C22A 1.580(19) . ? C22A C23A 1.36(3) . ? C22A H22A 0.95 . ? C23A C24A 1.40(2) . ? C23A H23A 0.95 . ? C24A C29A 1.38(2) . ? C24A C25A 1.42(3) . ? C25A C26A 1.46(3) . ? C25A H25A 0.95 . ? C26A C27A 1.36(4) . ? C26A H26A 0.95 . ? C27A N30 1.34(3) . ? C27A C28A 1.46(3) . ? C28A C29A 1.243(18) . ? C28A H28A 0.95 . ? C29A H29A 0.95 . ? C22B C23B 1.25(2) . ? C22B H22B 0.95 . ? C23B C24B 1.48(2) . ? C23B H23B 0.95 . ? C24B C29B 1.36(3) . ? C24B C25B 1.37(3) . ? C25B C26B 1.31(2) . ? C25B H25B 0.95 . ? C26B C27B 1.52(4) . ? C26B H26B 0.95 . ? C27B N30 1.45(3) . ? C29B H29B 0.95 . ? N30 C33A 1.379(15) . ? N30 C31A 1.459(11) . ? C31A C32A 1.54(3) . ? C31A H31A 0.99 . ? C31A H31B 0.99 . ? C32A H32A 0.98 . ? C32A H32B 0.98 . ? C32A H32C 0.98 . ? C32B H32D 0.98 . ? C32B H32E 0.98 . ? C32B H32F 0.98 . ? C33A C34A 1.48(3) . ? C33A H33A 0.99 . ? C33A H33B 0.99 . ? C34A H34A 0.98 . ? C34A H34B 0.98 . ? C34A H34C 0.98 . ? C34B H34D 0.98 . ? C34B H34E 0.98 . ? C34B H34F 0.98 . ? C51 C54 1.335(10) . ? C51 C52 1.361(10) . ? C52 C53 1.307(9) . ? C53 C71 1.285(11) . ? C53 H53 0.95 . ? C54 C55 1.400(10) . ? C54 C56 1.521(10) . ? C55 C71 1.436(10) . ? C55 H55 0.95 . ? C56 C57 1.196(10) . ? C56 H56 0.95 . ? C57 C58 1.504(11) . ? C57 H57 0.95 . ? C58 C59 1.271(11) . ? C58 C63 1.425(12) . ? C59 C60 1.354(11) . ? C59 H59 0.95 . ? C60 C61 1.439(12) . ? C60 H60 0.95 . ? C61 N64 1.367(10) . ? C61 C62 1.393(12) . ? C62 C63 1.490(12) . ? C62 H62 0.95 . ? C63 H63 0.95 . ? N64 C65 1.405(11) . ? N64 C67 1.446(10) . ? C65 C66 1.544(14) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 H66A 0.98 . ? C66 H66B 0.98 . ? C66 H66C 0.98 . ? C67 C68 1.507(14) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 H68A 0.98 . ? C68 H68B 0.98 . ? C68 H68C 0.98 . ? C71 C72 1.494(11) . ? C72 C73 1.279(12) . ? C72 H72 0.95 . ? C73 C74 1.495(12) . ? C73 H73 0.95 . ? C74 C75 1.356(12) . ? C74 C79 1.435(11) . ? C75 C76 1.372(10) . ? C75 H75 0.95 . ? C76 C77 1.405(11) . ? C76 H76 0.95 . ? C77 N80 1.372(10) . ? C77 C78 1.425(12) . ? C78 C79 1.397(11) . ? C78 H78 0.95 . ? C79 H79 0.95 . ? N80 C83 1.459(10) . ? N80 C81 1.479(11) . ? C81 C82 1.522(12) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? C83 C84 1.483(11) . ? C83 H83A 0.99 . ? C83 H83B 0.99 . ? C84 H84A 0.98 . ? C84 H84B 0.98 . ? C84 H84C 0.98 . ? 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 C1 Zn1 C51 79.9(3) . . ? C1 Zn1 Cl2 114.11(17) . . ? C51 Zn1 Cl2 113.01(18) . . ? C1 Zn1 Cl1 113.43(19) . . ? C51 Zn1 Cl1 112.02(18) . . ? Cl2 Zn1 Cl1 118.26(8) . . ? C2 C1 C4 115.0(7) . . ? C2 C1 Zn1 117.0(6) . . ? C4 C1 Zn1 127.9(6) . . ? C3 C2 C1 129.5(8) . . ? C3 C2 C52 117.2(7) . . ? C1 C2 C52 113.3(6) . . ? C2 C3 C21A 115.7(8) . . ? C2 C3 H3 122.1 . . ? C21A C3 H3 122.1 . . ? C1 C4 C5 118.5(7) . . ? C1 C4 C6 115.4(6) . . ? C5 C4 C6 126.1(7) . . ? C21A C5 C4 118.6(8) . . ? C21A C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C7 C6 C4 123.2(8) . . ? C7 C6 H6 118.4 . . ? C4 C6 H6 118.4 . . ? C6 C7 C8 126.5(8) . . ? C6 C7 H7 116.7 . . ? C8 C7 H7 116.7 . . ? C9 C8 C13 114.3(9) . . ? C9 C8 C7 123.2(8) . . ? C13 C8 C7 122.5(9) . . ? C10 C9 C8 123.3(8) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C9 C10 C11 119.7(9) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 N14 119.5(9) . . ? C12 C11 C10 119.5(10) . . ? N14 C11 C10 120.9(10) . . ? C11 C12 C13 119.4(9) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C8 123.8(9) . . ? C12 C13 H13 118.1 . . ? C8 C13 H13 118.1 . . ? C11 N14 C15 120.7(8) . . ? C11 N14 C17B 131.9(15) . . ? C15 N14 C17B 106.1(15) . . ? C11 N14 C17A 110.3(15) . . ? C15 N14 C17A 125.1(16) . . ? N14 C15 C16 112.0(7) . . ? N14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N14 C17A C18A 119(2) . . ? N14 C17A H17A 107.5 . . ? C18A C17A H17A 107.5 . . ? N14 C17A H17B 107.5 . . ? C18A C17A H17B 107.5 . . ? H17A C17A H17B 107 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? N14 C17B C18B 107(2) . . ? N14 C17B H17C 110.4 . . ? C18B C17B H17C 110.4 . . ? N14 C17B H17D 110.4 . . ? C18B C17B H17D 110.4 . . ? H17C C17B H17D 108.6 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C3 C21A C5 122.6(7) . . ? C3 C21A C22A 101.2(10) . . ? C5 C21A C22A 136.2(11) . . ? C23A C22A C21A 118.1(19) . . ? C23A C22A H22A 120.9 . . ? C21A C22A H22A 120.9 . . ? C22A C23A C24A 123(2) . . ? C22A C23A H23A 118.6 . . ? C24A C23A H23A 118.6 . . ? C29A C24A C23A 121.2(17) . . ? C29A C24A C25A 113.2(17) . . ? C23A C24A C25A 124.9(19) . . ? C24A C25A C26A 125.4(19) . . ? C24A C25A H25A 117.3 . . ? C26A C25A H25A 117.3 . . ? C27A C26A C25A 118(2) . . ? C27A C26A H26A 121.2 . . ? C25A C26A H26A 121.2 . . ? N30 C27A C26A 125(3) . . ? N30 C27A C28A 123(3) . . ? C26A C27A C28A 112(2) . . ? C29A C28A C27A 131.7(17) . . ? C29A C28A H28A 114.2 . . ? C27A C28A H28A 114.2 . . ? C28A C29A C24A 119.9(17) . . ? C28A C29A H29A 120 . . ? C24A C29A H29A 120 . . ? C23B C22B H22B 122.7 . . ? C22B C23B C24B 128(2) . . ? C22B C23B H23B 115.8 . . ? C24B C23B H23B 115.8 . . ? C29B C24B C25B 117.6(18) . . ? C29B C24B C23B 123(2) . . ? C25B C24B C23B 119.7(17) . . ? C26B C25B C24B 122(2) . . ? C26B C25B H25B 119 . . ? C24B C25B H25B 119 . . ? C25B C26B C27B 120(2) . . ? C25B C26B H26B 119.9 . . ? C27B C26B H26B 119.9 . . ? N30 C27B C26B 114(2) . . ? C24B C29B H29B 116.1 . . ? C27A N30 C33A 118.3(16) . . ? C33A N30 C27B 122.1(16) . . ? C27A N30 C31A 124.7(17) . . ? C33A N30 C31A 116.6(9) . . ? C27B N30 C31A 121.3(16) . . ? N30 C31A C32A 110.5(12) . . ? N30 C31A H31A 109.5 . . ? C32A C31A H31A 109.5 . . ? N30 C31A H31B 109.5 . . ? C32A C31A H31B 109.5 . . ? H31A C31A H31B 108.1 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? H32D C32B H32E 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N30 C33A C34A 142(3) . . ? N30 C33A H33A 101.5 . . ? C34A C33A H33A 101.5 . . ? N30 C33A H33B 101.5 . . ? C34A C33A H33B 101.5 . . ? H33A C33A H33B 104.6 . . ? C33A C34A H34A 109.5 . . ? C33A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C33A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? H34D C34B H34E 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C54 C51 C52 117.4(7) . . ? C54 C51 Zn1 128.0(6) . . ? C52 C51 Zn1 114.5(6) . . ? C53 C52 C51 125.2(8) . . ? C53 C52 C2 119.6(7) . . ? C51 C52 C2 115.2(7) . . ? C71 C53 C52 119.2(8) . . ? C71 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C51 C54 C55 120.3(7) . . ? C51 C54 C56 114.7(7) . . ? C55 C54 C56 125.0(8) . . ? C54 C55 C71 116.5(8) . . ? C54 C55 H55 121.8 . . ? C71 C55 H55 121.8 . . ? C57 C56 C54 127.2(8) . . ? C57 C56 H56 116.4 . . ? C54 C56 H56 116.4 . . ? C56 C57 C58 125.8(8) . . ? C56 C57 H57 117.1 . . ? C58 C57 H57 117.1 . . ? C59 C58 C63 120.8(9) . . ? C59 C58 C57 118.8(9) . . ? C63 C58 C57 120.4(8) . . ? C58 C59 C60 120.8(10) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C59 C60 C61 125.0(9) . . ? C59 C60 H60 117.5 . . ? C61 C60 H60 117.5 . . ? N64 C61 C62 122.6(9) . . ? N64 C61 C60 121.0(8) . . ? C62 C61 C60 116.4(8) . . ? C61 C62 C63 116.4(9) . . ? C61 C62 H62 121.8 . . ? C63 C62 H62 121.8 . . ? C58 C63 C62 120.5(8) . . ? C58 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C61 N64 C65 121.3(7) . . ? C61 N64 C67 121.2(8) . . ? C65 N64 C67 116.6(7) . . ? N64 C65 C66 112.5(9) . . ? N64 C65 H65A 109.1 . . ? C66 C65 H65A 109.1 . . ? N64 C65 H65B 109.1 . . ? C66 C65 H65B 109.1 . . ? H65A C65 H65B 107.8 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N64 C67 C68 112.9(9) . . ? N64 C67 H67A 109 . . ? C68 C67 H67A 109 . . ? N64 C67 H67B 109 . . ? C68 C67 H67B 109 . . ? H67A C67 H67B 107.8 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C53 C71 C55 121.2(7) . . ? C53 C71 C72 118.7(8) . . ? C55 C71 C72 120.0(8) . . ? C73 C72 C71 127.0(9) . . ? C73 C72 H72 116.5 . . ? C71 C72 H72 116.5 . . ? C72 C73 C74 130.5(10) . . ? C72 C73 H73 114.7 . . ? C74 C73 H73 114.7 . . ? C75 C74 C79 120.4(8) . . ? C75 C74 C73 120.5(9) . . ? C79 C74 C73 119.0(9) . . ? C74 C75 C76 120.3(9) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C75 C76 C77 122.7(9) . . ? C75 C76 H76 118.6 . . ? C77 C76 H76 118.6 . . ? N80 C77 C76 123.5(9) . . ? N80 C77 C78 119.7(8) . . ? C76 C77 C78 116.6(8) . . ? C79 C78 C77 121.0(9) . . ? C79 C78 H78 119.5 . . ? C77 C78 H78 119.5 . . ? C78 C79 C74 118.5(9) . . ? C78 C79 H79 120.8 . . ? C74 C79 H79 120.8 . . ? C77 N80 C83 123.9(7) . . ? C77 N80 C81 120.9(7) . . ? C83 N80 C81 114.9(7) . . ? N80 C81 C82 113.0(8) . . ? N80 C81 H81A 109 . . ? C82 C81 H81A 109 . . ? N80 C81 H81B 109 . . ? C82 C81 H81B 109 . . ? H81A C81 H81B 107.8 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N80 C83 C84 110.2(6) . . ? N80 C83 H83A 109.6 . . ? C84 C83 H83A 109.6 . . ? N80 C83 H83B 109.6 . . ? C84 C83 H83B 109.6 . . ? H83A C83 H83B 108.1 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? 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 C51 Zn1 C1 C2 -1.8(5) . . . . ? Cl2 Zn1 C1 C2 -112.7(4) . . . . ? Cl1 Zn1 C1 C2 107.9(5) . . . . ? C51 Zn1 C1 C4 -179.7(6) . . . . ? Cl2 Zn1 C1 C4 69.5(6) . . . . ? Cl1 Zn1 C1 C4 -69.9(6) . . . . ? C4 C1 C2 C3 2.4(10) . . . . ? Zn1 C1 C2 C3 -175.7(5) . . . . ? C4 C1 C2 C52 -179.3(5) . . . . ? Zn1 C1 C2 C52 2.6(7) . . . . ? C1 C2 C3 C21A -2.6(10) . . . . ? C52 C2 C3 C21A 179.1(6) . . . . ? C2 C1 C4 C5 0.4(8) . . . . ? Zn1 C1 C4 C5 178.3(4) . . . . ? C2 C1 C4 C6 -177.8(5) . . . . ? Zn1 C1 C4 C6 0.0(8) . . . . ? C1 C4 C5 C21A -2.6(9) . . . . ? C6 C4 C5 C21A 175.4(6) . . . . ? C1 C4 C6 C7 171.7(6) . . . . ? C5 C4 C6 C7 -6.4(10) . . . . ? C4 C6 C7 C8 -180.0(6) . . . . ? C6 C7 C8 C9 -5.1(11) . . . . ? C6 C7 C8 C13 173.0(6) . . . . ? C13 C8 C9 C10 0.5(10) . . . . ? C7 C8 C9 C10 178.7(6) . . . . ? C8 C9 C10 C11 -0.1(11) . . . . ? C9 C10 C11 C12 0.1(11) . . . . ? C9 C10 C11 N14 -179.0(7) . . . . ? N14 C11 C12 C13 178.6(7) . . . . ? C10 C11 C12 C13 -0.6(12) . . . . ? C11 C12 C13 C8 1.1(12) . . . . ? C9 C8 C13 C12 -1.0(10) . . . . ? C7 C8 C13 C12 -179.2(7) . . . . ? C12 C11 N14 C15 166.5(8) . . . . ? C10 C11 N14 C15 -14.4(12) . . . . ? C12 C11 N14 C17B 1(3) . . . . ? C10 C11 N14 C17B -179(2) . . . . ? C12 C11 N14 C17A 8(2) . . . . ? C10 C11 N14 C17A -173.2(18) . . . . ? C11 N14 C15 C16 90.7(11) . . . . ? C17B N14 C15 C16 -100.8(18) . . . . ? C17A N14 C15 C16 -114(2) . . . . ? C11 N14 C17A C18A 77(2) . . . . ? C15 N14 C17A C18A -80(2) . . . . ? C17B N14 C17A C18A -115(9) . . . . ? C11 N14 C17B C18B 81(3) . . . . ? C15 N14 C17B C18B -85.5(18) . . . . ? C17A N14 C17B C18B 66(8) . . . . ? C2 C3 C21A C5 -0.1(10) . . . . ? C2 C3 C21A C22A 178.5(7) . . . . ? C4 C5 C21A C3 2.5(10) . . . . ? C4 C5 C21A C22A -175.5(9) . . . . ? C3 C21A C22A C23A 176.3(11) . . . . ? C5 C21A C22A C23A -5.4(19) . . . . ? C21A C22A C23A C24A 176.5(12) . . . . ? C22A C23A C24A C29A 159.4(15) . . . . ? C22A C23A C24A C25A -11(3) . . . . ? C29A C24A C25A C26A 9(2) . . . . ? C23A C24A C25A C26A -179.4(15) . . . . ? C24A C25A C26A C27A -4(3) . . . . ? C25A C26A C27A N30 -176.4(16) . . . . ? C25A C26A C27A C28A -2(2) . . . . ? N30 C27A C28A C29A 178.3(16) . . . . ? C26A C27A C28A C29A 4(3) . . . . ? C27A C28A C29A C24A 2(3) . . . . ? C23A C24A C29A C28A -179.3(16) . . . . ? C25A C24A C29A C28A -8(2) . . . . ? C22B C23B C24B C29B -2(3) . . . . ? C22B C23B C24B C25B 172.9(16) . . . . ? C29B C24B C25B C26B -7(3) . . . . ? C23B C24B C25B C26B 177.3(15) . . . . ? C24B C25B C26B C27B 7(2) . . . . ? C25B C26B C27B N30 167.5(15) . . . . ? C26A C27A N30 C33A -12(3) . . . . ? C28A C27A N30 C33A 174.6(17) . . . . ? C26A C27A N30 C27B 103(19) . . . . ? C28A C27A N30 C27B -70(16) . . . . ? C26A C27A N30 C31A 176.7(16) . . . . ? C28A C27A N30 C31A 3(3) . . . . ? C26B C27B N30 C27A -81(17) . . . . ? C26B C27B N30 C33A -11(2) . . . . ? C26B C27B N30 C31A 165.9(12) . . . . ? C27A N30 C31A C32A -144.0(19) . . . . ? C33A N30 C31A C32A 44(2) . . . . ? C27B N30 C31A C32A -132.9(19) . . . . ? C27A N30 C33A C34A 87(3) . . . . ? C27B N30 C33A C34A 77(3) . . . . ? C31A N30 C33A C34A -100(2) . . . . ? C1 Zn1 C51 C54 176.1(6) . . . . ? Cl2 Zn1 C51 C54 -71.8(6) . . . . ? Cl1 Zn1 C51 C54 64.8(6) . . . . ? C1 Zn1 C51 C52 0.6(5) . . . . ? Cl2 Zn1 C51 C52 112.6(5) . . . . ? Cl1 Zn1 C51 C52 -110.8(5) . . . . ? C54 C51 C52 C53 2.3(10) . . . . ? Zn1 C51 C52 C53 178.4(5) . . . . ? C54 C51 C52 C2 -175.5(5) . . . . ? Zn1 C51 C52 C2 0.6(7) . . . . ? C3 C2 C52 C53 -1.4(9) . . . . ? C1 C2 C52 C53 180.0(6) . . . . ? C3 C2 C52 C51 176.4(6) . . . . ? C1 C2 C52 C51 -2.1(8) . . . . ? C51 C52 C53 C71 -0.8(11) . . . . ? C2 C52 C53 C71 176.8(6) . . . . ? C52 C51 C54 C55 -0.1(9) . . . . ? Zn1 C51 C54 C55 -175.6(4) . . . . ? C52 C51 C54 C56 -178.0(5) . . . . ? Zn1 C51 C54 C56 6.6(9) . . . . ? C51 C54 C55 C71 -3.1(9) . . . . ? C56 C54 C55 C71 174.5(5) . . . . ? C51 C54 C56 C57 -171.4(7) . . . . ? C55 C54 C56 C57 10.8(11) . . . . ? C54 C56 C57 C58 179.6(6) . . . . ? C56 C57 C58 C59 -173.0(8) . . . . ? C56 C57 C58 C63 5.9(11) . . . . ? C63 C58 C59 C60 1.1(13) . . . . ? C57 C58 C59 C60 -179.9(6) . . . . ? C58 C59 C60 C61 -2.4(13) . . . . ? C59 C60 C61 N64 -178.7(7) . . . . ? C59 C60 C61 C62 3.4(12) . . . . ? N64 C61 C62 C63 179.1(7) . . . . ? C60 C61 C62 C63 -3.0(10) . . . . ? C59 C58 C63 C62 -1.1(12) . . . . ? C57 C58 C63 C62 180.0(6) . . . . ? C61 C62 C63 C58 2.1(11) . . . . ? C62 C61 N64 C65 -3.1(13) . . . . ? C60 C61 N64 C65 179.2(8) . . . . ? C62 C61 N64 C67 -171.1(8) . . . . ? C60 C61 N64 C67 11.2(12) . . . . ? C61 N64 C65 C66 -78.6(10) . . . . ? C67 N64 C65 C66 90.0(10) . . . . ? C61 N64 C67 C68 -88.5(12) . . . . ? C65 N64 C67 C68 102.9(11) . . . . ? C52 C53 C71 C55 -2.8(10) . . . . ? C52 C53 C71 C72 177.8(6) . . . . ? C54 C55 C71 C53 4.7(9) . . . . ? C54 C55 C71 C72 -175.9(6) . . . . ? C53 C71 C72 C73 -165.7(9) . . . . ? C55 C71 C72 C73 14.8(11) . . . . ? C71 C72 C73 C74 -175.9(7) . . . . ? C72 C73 C74 C75 177.4(10) . . . . ? C72 C73 C74 C79 -5.8(15) . . . . ? C79 C74 C75 C76 5.1(14) . . . . ? C73 C74 C75 C76 -178.1(8) . . . . ? C74 C75 C76 C77 1.4(14) . . . . ? C75 C76 C77 N80 176.8(8) . . . . ? C75 C76 C77 C78 -6.5(13) . . . . ? N80 C77 C78 C79 -177.8(7) . . . . ? C76 C77 C78 C79 5.4(12) . . . . ? C77 C78 C79 C74 0.5(12) . . . . ? C75 C74 C79 C78 -5.9(13) . . . . ? C73 C74 C79 C78 177.2(7) . . . . ? C76 C77 N80 C83 -173.0(8) . . . . ? C78 C77 N80 C83 10.5(12) . . . . ? C76 C77 N80 C81 0.2(13) . . . . ? C78 C77 N80 C81 -176.3(7) . . . . ? C77 N80 C81 C82 -83.8(10) . . . . ? C83 N80 C81 C82 90.0(9) . . . . ? C77 N80 C83 C84 -91.6(9) . . . . ? C81 N80 C83 C84 94.9(9) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 869745'