# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jean-Luc Renaud' _publ_contact_author_email JEAN-LUC.RENAUD@UNIV-RENNES1.FR _publ_section_title ; Synthesis of New Amino- and Methylene-Bispyridines and their Coordination Chemistry with Mg(II) and Zn(II) ; _publ_requested_category FM loop_ _publ_author_name 'Jean-Luc Renaud' 'Jean-Francois Carpentier' 'Mohammed Kamal Elmkaddem' 'Cedric Fischmeister' ; T.Roisnel ; 'Christophe M Thomas' 'Zhanjiang Zheng.' # Attachment 'ligand2c.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-09-07 at 18:18:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\progs\wingx\files\archive.dat # CIF files read : job struct data_job3 _database_code_depnum_ccdc_archive 'CCDC 682251' _audit_creation_date 2006-09-07T18:18:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H53 N3' _chemical_formula_sum 'C40 H53 N3' _chemical_formula_weight 575.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0788(16) _cell_length_b 16.3324(17) _cell_length_c 14.8509(17) _cell_angle_alpha 90 _cell_angle_beta 99.069(7) _cell_angle_gamma 90 _cell_volume 3372.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.62 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thick 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 0.1213 _diffrn_reflns_av_unetI/netI 0.1105 _diffrn_reflns_number 34835 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.62 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 7758 _reflns_number_gt 4676 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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)' #----------------------------------------------------------------------------# # 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^)+(0.0523P)^2^+0.2331P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7758 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.153 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.245 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' 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 N1 N 0.34827(12) 0.09982(10) 0.25686(11) 0.0172(4) Uani 1 1 d . . . N2 N 0.60152(12) -0.03925(10) 0.34665(11) 0.0182(4) Uani 1 1 d . . . N3 N 0.47073(13) 0.03900(10) 0.36043(12) 0.0199(4) Uani 1 1 d . . . HN3 H 0.4862(19) 0.0197(16) 0.4200(18) 0.05 Uiso 1 1 d . . . C4 C 0.22580(14) 0.15668(12) 0.14210(13) 0.0156(4) Uani 1 1 d . . . C5 C 0.16838(15) 0.20204(13) -0.04150(13) 0.0190(5) Uani 1 1 d . . . C6 C 0.88101(15) -0.23500(12) 0.43819(13) 0.0170(4) Uani 1 1 d . . . C7 C 0.90460(15) -0.15668(12) 0.41065(13) 0.0173(4) Uani 1 1 d . . . H7 H 0.9697 -0.1392 0.4229 0.021 Uiso 1 1 calc R . . C8 C 0.78565(15) -0.25787(12) 0.42002(13) 0.0191(5) Uani 1 1 d . . . H8 H 0.7684 -0.3107 0.4389 0.023 Uiso 1 1 calc R . . C9 C 0.17414(15) 0.12017(12) -0.01555(13) 0.0192(5) Uani 1 1 d . . . H9 H 0.1579 0.0793 -0.0609 0.023 Uiso 1 1 calc R . . C10 C 0.19051(15) 0.26069(12) 0.02653(13) 0.0191(5) Uani 1 1 d . . . H10 H 0.1861 0.317 0.0102 0.023 Uiso 1 1 calc R . . C11 C 0.21906(15) 0.23974(12) 0.11813(13) 0.0165(4) Uani 1 1 d . . . C12 C 0.61039(15) -0.23811(12) 0.35837(14) 0.0210(5) Uani 1 1 d . . . H12 H 0.5718 -0.1996 0.3147 0.025 Uiso 1 1 calc R . . C13 C 0.71343(15) -0.20758(12) 0.37548(13) 0.0173(5) Uani 1 1 d . . . C14 C 0.65624(15) -0.06233(13) 0.20449(14) 0.0217(5) Uani 1 1 d . . . H14 H 0.6998 -0.0886 0.1711 0.026 Uiso 1 1 calc R . . C15 C 0.52145(15) 0.02556(12) 0.20981(14) 0.0213(5) Uani 1 1 d . . . H15 H 0.4727 0.0614 0.1812 0.026 Uiso 1 1 calc R . . C16 C 0.66335(14) -0.07439(12) 0.29767(14) 0.0174(4) Uani 1 1 d . . . C17 C 0.32294(16) 0.07514(12) 0.41071(14) 0.0198(5) Uani 1 1 d . . . H17 H 0.3472 0.0552 0.47 0.024 Uiso 1 1 calc R . . C18 C 0.19876(16) 0.13580(12) 0.30361(14) 0.0200(5) Uani 1 1 d . . . H18 H 0.1359 0.1581 0.2889 0.024 Uiso 1 1 calc R . . C19 C 0.37863(15) 0.07195(12) 0.34091(14) 0.0174(4) Uani 1 1 d . . . C20 C 0.20890(16) 0.00561(12) 0.09813(14) 0.0208(5) Uani 1 1 d . . . H20 H 0.2305 0.0011 0.1654 0.025 Uiso 1 1 calc R . . C21 C 0.13657(16) 0.22488(13) -0.14095(13) 0.0219(5) Uani 1 1 d . . . H21 H 0.1487 0.1763 -0.1785 0.026 Uiso 1 1 calc R . . C22 C 0.20292(15) 0.09583(12) 0.07481(13) 0.0175(5) Uani 1 1 d . . . C23 C 0.24005(15) 0.30746(12) 0.18901(14) 0.0187(5) Uani 1 1 d . . . H23 H 0.2657 0.2812 0.2487 0.022 Uiso 1 1 calc R . . C24 C 0.73867(14) -0.12910(12) 0.34845(13) 0.0156(4) Uani 1 1 d . . . C25 C 0.53142(15) 0.00850(12) 0.30246(13) 0.0176(5) Uani 1 1 d . . . C26 C 0.83529(15) -0.10360(12) 0.36576(13) 0.0167(4) Uani 1 1 d . . . C27 C 0.95534(15) -0.29173(12) 0.49078(14) 0.0205(5) Uani 1 1 d . . . H27 H 0.9299 -0.3488 0.4817 0.025 Uiso 1 1 calc R . . C28 C 0.60094(17) -0.32397(14) 0.31641(16) 0.0304(6) Uani 1 1 d . . . H28A H 0.5331 -0.3403 0.3061 0.046 Uiso 1 1 calc R . . H28B H 0.6382 -0.3629 0.3581 0.046 Uiso 1 1 calc R . . H28C H 0.6254 -0.3236 0.2582 0.046 Uiso 1 1 calc R . . C29 C 0.86422(16) -0.01709(12) 0.34267(14) 0.0214(5) Uani 1 1 d . . . H29 H 0.8143 0.004 0.2927 0.026 Uiso 1 1 calc R . . C30 C 0.58523(16) -0.01171(13) 0.16100(14) 0.0236(5) Uani 1 1 d . . . H30 H 0.5801 -0.0024 0.0973 0.028 Uiso 1 1 calc R . . C31 C 0.31515(16) 0.36806(13) 0.16669(15) 0.0270(5) Uani 1 1 d . . . H31A H 0.3261 0.41 0.2143 0.04 Uiso 1 1 calc R . . H31B H 0.2922 0.3941 0.1078 0.04 Uiso 1 1 calc R . . H31C H 0.3755 0.3391 0.1636 0.04 Uiso 1 1 calc R . . C32 C 1.05256(16) -0.28996(13) 0.45885(15) 0.0262(5) Uani 1 1 d . . . H32A H 1.0443 -0.3025 0.3936 0.039 Uiso 1 1 calc R . . H32B H 1.095 -0.3308 0.4928 0.039 Uiso 1 1 calc R . . H32C H 1.0811 -0.2354 0.4696 0.039 Uiso 1 1 calc R . . C33 C 0.23264(16) 0.10771(12) 0.39146(14) 0.0223(5) Uani 1 1 d . . . H33 H 0.1932 0.1112 0.4376 0.027 Uiso 1 1 calc R . . C34 C 0.02961(17) 0.24252(15) -0.16029(15) 0.0308(6) Uani 1 1 d . . . H34A H -0.0059 0.1959 -0.1407 0.046 Uiso 1 1 calc R . . H34B H 0.0099 0.2514 -0.2258 0.046 Uiso 1 1 calc R . . H34C H 0.0156 0.2917 -0.1269 0.046 Uiso 1 1 calc R . . C35 C 0.56724(17) -0.23832(14) 0.44664(15) 0.0297(6) Uani 1 1 d . . . H35A H 0.5006 -0.2578 0.434 0.045 Uiso 1 1 calc R . . H35B H 0.5685 -0.1826 0.4714 0.045 Uiso 1 1 calc R . . H35C H 0.605 -0.2747 0.4912 0.045 Uiso 1 1 calc R . . C36 C 0.96070(17) -0.01375(14) 0.30911(17) 0.0330(6) Uani 1 1 d . . . H36A H 0.9753 0.043 0.2948 0.05 Uiso 1 1 calc R . . H36B H 0.958 -0.0474 0.2542 0.05 Uiso 1 1 calc R . . H36C H 1.011 -0.0347 0.3567 0.05 Uiso 1 1 calc R . . C37 C 0.25835(15) 0.13050(11) 0.23855(13) 0.0158(4) Uani 1 1 d . . . C38 C 0.28336(18) -0.03800(13) 0.05135(16) 0.0306(6) Uani 1 1 d . . . H38A H 0.2857 -0.0961 0.0683 0.046 Uiso 1 1 calc R . . H38B H 0.3467 -0.0132 0.0706 0.046 Uiso 1 1 calc R . . H38C H 0.2656 -0.0329 -0.0149 0.046 Uiso 1 1 calc R . . C39 C 0.86383(19) 0.03822(13) 0.42577(16) 0.0336(6) Uani 1 1 d . . . H39A H 0.8008 0.0352 0.4458 0.05 Uiso 1 1 calc R . . H39B H 0.8767 0.0948 0.4095 0.05 Uiso 1 1 calc R . . H39C H 0.9137 0.02 0.4753 0.05 Uiso 1 1 calc R . . C40 C 0.11118(18) -0.03624(14) 0.07667(16) 0.0347(6) Uani 1 1 d . . . H40A H 0.1179 -0.0943 0.093 0.052 Uiso 1 1 calc R . . H40B H 0.0867 -0.0311 0.0114 0.052 Uiso 1 1 calc R . . H40C H 0.0661 -0.0102 0.1118 0.052 Uiso 1 1 calc R . . C41 C 0.96570(17) -0.27299(14) 0.59240(14) 0.0284(5) Uani 1 1 d . . . H41A H 0.9023 -0.2749 0.6117 0.043 Uiso 1 1 calc R . . H41B H 0.9935 -0.2183 0.6042 0.043 Uiso 1 1 calc R . . H41C H 1.0079 -0.3138 0.6267 0.043 Uiso 1 1 calc R . . C42 C 0.14744(17) 0.35211(13) 0.19999(15) 0.0265(5) Uani 1 1 d . . . H42A H 0.1617 0.3952 0.246 0.04 Uiso 1 1 calc R . . H42B H 0.1017 0.3132 0.2194 0.04 Uiso 1 1 calc R . . H42C H 0.1193 0.3766 0.1416 0.04 Uiso 1 1 calc R . . C43 C 0.1932(2) 0.29578(17) -0.17143(16) 0.0425(7) Uani 1 1 d . . . H43A H 0.1701 0.3076 -0.2359 0.064 Uiso 1 1 calc R . . H43B H 0.2616 0.2814 -0.1635 0.064 Uiso 1 1 calc R . . H43C H 0.1845 0.3442 -0.1347 0.064 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 N1 0.0182(10) 0.0156(8) 0.0181(9) 0.0009(7) 0.0035(7) 0.0016(7) N2 0.0169(10) 0.0178(9) 0.0193(9) 0.0016(7) 0.0012(8) 0.0011(7) N3 0.0202(10) 0.0246(10) 0.0148(9) 0.0022(8) 0.0027(8) 0.0058(8) C4 0.0118(11) 0.0188(10) 0.0167(11) 0.0013(8) 0.0032(8) 0.0020(8) C5 0.0172(12) 0.0255(11) 0.0148(11) 0.0018(9) 0.0038(9) 0.0048(9) C6 0.0198(12) 0.0184(10) 0.0140(10) -0.0007(8) 0.0060(9) 0.0010(9) C7 0.0162(11) 0.0210(11) 0.0147(11) -0.0004(8) 0.0026(8) -0.0011(9) C8 0.0208(12) 0.0167(10) 0.0204(11) 0.0008(9) 0.0052(9) 0.0006(9) C9 0.0188(12) 0.0228(11) 0.0161(11) -0.0052(9) 0.0031(9) 0.0017(9) C10 0.0192(12) 0.0190(10) 0.0198(11) 0.0013(9) 0.0052(9) 0.0039(9) C11 0.0152(11) 0.0184(10) 0.0169(11) 0.0002(8) 0.0060(9) 0.0013(9) C12 0.0173(12) 0.0219(11) 0.0233(12) 0.0034(9) 0.0015(9) -0.0010(9) C13 0.0184(12) 0.0203(10) 0.0140(10) -0.0002(8) 0.0046(9) -0.0003(9) C14 0.0192(12) 0.0264(11) 0.0207(11) 0.0024(9) 0.0068(9) 0.0024(10) C15 0.0190(12) 0.0229(11) 0.0221(12) 0.0048(9) 0.0038(9) 0.0039(9) C16 0.0144(11) 0.0168(10) 0.0205(11) 0.0000(8) 0.0013(9) -0.0022(9) C17 0.0261(13) 0.0201(11) 0.0131(10) -0.0006(8) 0.0026(9) 0.0008(9) C18 0.0203(12) 0.0204(11) 0.0196(11) 0.0001(9) 0.0045(9) 0.0037(9) C19 0.0187(12) 0.0139(10) 0.0188(11) -0.0012(8) 0.0006(9) -0.0002(9) C20 0.0276(13) 0.0188(10) 0.0149(10) -0.0006(8) 0.0003(9) 0.0005(9) C21 0.0269(13) 0.0253(11) 0.0134(11) -0.0011(9) 0.0031(9) 0.0039(10) C22 0.0181(12) 0.0170(10) 0.0179(11) -0.0004(8) 0.0043(9) 0.0023(9) C23 0.0240(12) 0.0172(10) 0.0154(11) -0.0002(8) 0.0045(9) -0.0001(9) C24 0.0168(11) 0.0205(10) 0.0097(10) -0.0006(8) 0.0027(8) 0.0024(9) C25 0.0167(11) 0.0158(10) 0.0204(11) -0.0012(8) 0.0034(9) -0.0012(9) C26 0.0195(12) 0.0170(10) 0.0142(10) -0.0002(8) 0.0045(9) 0.0008(9) C27 0.0200(12) 0.0176(10) 0.0241(12) 0.0028(9) 0.0042(9) 0.0009(9) C28 0.0256(14) 0.0315(13) 0.0337(14) -0.0068(11) 0.0033(11) -0.0040(11) C29 0.0194(12) 0.0190(11) 0.0247(12) 0.0058(9) 0.0005(9) 0.0004(9) C30 0.0240(13) 0.0315(12) 0.0151(11) 0.0058(9) 0.0025(9) 0.0007(10) C31 0.0277(14) 0.0250(12) 0.0295(13) -0.0055(10) 0.0084(10) -0.0048(10) C32 0.0226(13) 0.0262(12) 0.0305(13) 0.0058(10) 0.0066(10) 0.0071(10) C33 0.0256(13) 0.0235(11) 0.0195(11) -0.0013(9) 0.0084(9) 0.0023(10) C34 0.0284(14) 0.0423(14) 0.0208(12) 0.0088(10) 0.0013(10) 0.0024(11) C35 0.0255(14) 0.0364(13) 0.0289(13) -0.0002(11) 0.0096(11) -0.0046(11) C36 0.0316(15) 0.0236(12) 0.0464(15) 0.0102(11) 0.0141(12) -0.0003(11) C37 0.0188(12) 0.0117(9) 0.0168(11) -0.0013(8) 0.0025(9) -0.0014(8) C38 0.0373(15) 0.0225(12) 0.0317(14) -0.0043(10) 0.0045(11) 0.0073(11) C39 0.0369(16) 0.0194(12) 0.0432(15) -0.0023(11) 0.0024(12) -0.0013(11) C40 0.0391(16) 0.0284(13) 0.0359(15) 0.0034(11) 0.0040(12) -0.0071(11) C41 0.0327(14) 0.0310(13) 0.0214(12) 0.0046(10) 0.0043(10) 0.0105(11) C42 0.0300(14) 0.0245(12) 0.0257(13) -0.0068(10) 0.0071(10) 0.0039(10) C43 0.0463(18) 0.0617(18) 0.0193(13) 0.0112(12) 0.0049(12) -0.0170(14) #----------------------------------------------------------------------------# # 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 N1 C19 1.334(3) . ? N1 C37 1.349(3) . ? N2 C25 1.345(3) . ? N2 C16 1.347(2) . ? N3 C19 1.392(3) . ? N3 C25 1.397(2) . ? N3 HN3 0.93(3) . ? C4 C11 1.402(3) . ? C4 C22 1.410(3) . ? C4 C37 1.496(3) . ? C5 C9 1.390(3) . ? C5 C10 1.391(3) . ? C5 C21 1.521(3) . ? C6 C8 1.379(3) . ? C6 C7 1.399(3) . ? C6 C27 1.519(3) . ? C7 C26 1.394(3) . ? C7 H7 0.95 . ? C8 C13 1.391(3) . ? C8 H8 0.95 . ? C9 C22 1.397(3) . ? C9 H9 0.95 . ? C10 C11 1.399(3) . ? C10 H10 0.95 . ? C11 C23 1.523(3) . ? C12 C13 1.517(3) . ? C12 C35 1.529(3) . ? C12 C28 1.532(3) . ? C12 H12 1 . ? C13 C24 1.405(3) . ? C14 C30 1.377(3) . ? C14 C16 1.386(3) . ? C14 H14 0.95 . ? C15 C30 1.381(3) . ? C15 C25 1.389(3) . ? C15 H15 0.95 . ? C16 C24 1.497(3) . ? C17 C33 1.366(3) . ? C17 C19 1.396(3) . ? C17 H17 0.95 . ? C18 C37 1.379(3) . ? C18 C33 1.394(3) . ? C18 H18 0.95 . ? C20 C22 1.513(3) . ? C20 C38 1.523(3) . ? C20 C40 1.524(3) . ? C20 H20 1 . ? C21 C43 1.515(3) . ? C21 C34 1.516(3) . ? C21 H21 1 . ? C23 C31 1.522(3) . ? C23 C42 1.525(3) . ? C23 H23 1 . ? C24 C26 1.407(3) . ? C26 C29 1.524(3) . ? C27 C32 1.518(3) . ? C27 C41 1.524(3) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C36 1.520(3) . ? C29 C39 1.530(3) . ? C29 H29 1 . ? C30 H30 0.95 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33 0.95 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 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 C19 N1 C37 117.87(16) . . ? C25 N2 C16 118.06(17) . . ? C19 N3 C25 130.53(18) . . ? C19 N3 HN3 113.5(16) . . ? C25 N3 HN3 112.9(16) . . ? C11 C4 C22 120.21(18) . . ? C11 C4 C37 121.20(17) . . ? C22 C4 C37 118.58(17) . . ? C9 C5 C10 117.66(19) . . ? C9 C5 C21 120.03(18) . . ? C10 C5 C21 122.30(18) . . ? C8 C6 C7 117.35(19) . . ? C8 C6 C27 120.41(18) . . ? C7 C6 C27 122.16(19) . . ? C26 C7 C6 121.87(19) . . ? C26 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C6 C8 C13 123.33(19) . . ? C6 C8 H8 118.3 . . ? C13 C8 H8 118.3 . . ? C5 C9 C22 122.36(18) . . ? C5 C9 H9 118.8 . . ? C22 C9 H9 118.8 . . ? C5 C10 C11 122.33(19) . . ? C5 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C4 118.76(18) . . ? C10 C11 C23 119.28(18) . . ? C4 C11 C23 121.94(18) . . ? C13 C12 C35 110.84(18) . . ? C13 C12 C28 112.86(17) . . ? C35 C12 C28 109.03(17) . . ? C13 C12 H12 108 . . ? C35 C12 H12 108 . . ? C28 C12 H12 108 . . ? C8 C13 C24 118.40(19) . . ? C8 C13 C12 119.58(18) . . ? C24 C13 C12 122.01(18) . . ? C30 C14 C16 119.11(19) . . ? C30 C14 H14 120.4 . . ? C16 C14 H14 120.4 . . ? C30 C15 C25 117.3(2) . . ? C30 C15 H15 121.3 . . ? C25 C15 H15 121.3 . . ? N2 C16 C14 121.83(19) . . ? N2 C16 C24 116.68(17) . . ? C14 C16 C24 121.46(17) . . ? C33 C17 C19 118.18(19) . . ? C33 C17 H17 120.9 . . ? C19 C17 H17 120.9 . . ? C37 C18 C33 118.6(2) . . ? C37 C18 H18 120.7 . . ? C33 C18 H18 120.7 . . ? N1 C19 N3 118.52(17) . . ? N1 C19 C17 123.20(19) . . ? N3 C19 C17 118.28(18) . . ? C22 C20 C38 111.62(17) . . ? C22 C20 C40 111.91(18) . . ? C38 C20 C40 111.00(18) . . ? C22 C20 H20 107.3 . . ? C38 C20 H20 107.3 . . ? C40 C20 H20 107.3 . . ? C43 C21 C34 110.6(2) . . ? C43 C21 C5 112.92(19) . . ? C34 C21 C5 111.24(16) . . ? C43 C21 H21 107.3 . . ? C34 C21 H21 107.3 . . ? C5 C21 H21 107.3 . . ? C9 C22 C4 118.66(18) . . ? C9 C22 C20 119.62(17) . . ? C4 C22 C20 121.72(18) . . ? C31 C23 C11 112.78(16) . . ? C31 C23 C42 110.32(17) . . ? C11 C23 C42 110.18(18) . . ? C31 C23 H23 107.8 . . ? C11 C23 H23 107.8 . . ? C42 C23 H23 107.8 . . ? C13 C24 C26 119.90(18) . . ? C13 C24 C16 119.84(18) . . ? C26 C24 C16 120.21(17) . . ? N2 C25 C15 123.47(18) . . ? N2 C25 N3 112.28(17) . . ? C15 C25 N3 124.25(19) . . ? C7 C26 C24 119.14(18) . . ? C7 C26 C29 119.50(19) . . ? C24 C26 C29 121.21(18) . . ? C6 C27 C32 114.20(17) . . ? C6 C27 C41 109.72(16) . . ? C32 C27 C41 110.81(19) . . ? C6 C27 H27 107.3 . . ? C32 C27 H27 107.3 . . ? C41 C27 H27 107.3 . . ? C12 C28 H28A 109.5 . . ? C12 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C12 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C36 C29 C26 113.04(17) . . ? C36 C29 C39 111.12(19) . . ? C26 C29 C39 109.31(17) . . ? C36 C29 H29 107.7 . . ? C26 C29 H29 107.7 . . ? C39 C29 H29 107.7 . . ? C14 C30 C15 120.16(19) . . ? C14 C30 H30 119.9 . . ? C15 C30 H30 119.9 . . ? C23 C31 H31A 109.5 . . ? C23 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C23 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C18 119.59(19) . . ? C17 C33 H33 120.2 . . ? C18 C33 H33 120.2 . . ? C21 C34 H34A 109.5 . . ? C21 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C21 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C12 C35 H35A 109.5 . . ? C12 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C12 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C29 C36 H36A 109.5 . . ? C29 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C29 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 C18 122.52(19) . . ? N1 C37 C4 115.81(16) . . ? C18 C37 C4 121.65(19) . . ? C20 C38 H38A 109.5 . . ? C20 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C20 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C29 C39 H39A 109.5 . . ? C29 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C29 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C20 C40 H40A 109.5 . . ? C20 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C20 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C23 C42 H42A 109.5 . . ? C23 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C23 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C21 C43 H43A 109.5 . . ? C21 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C21 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? # Attachment 'complex7.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-05-15 at 18:22:57 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\progs\wingx\files\archive.dat # CIF files read : job struct data_job2 _database_code_depnum_ccdc_archive 'CCDC 682252' _audit_creation_date 2006-05-15T18:22:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H48 N6 Zn1' _chemical_formula_sum 'C36 H48 N6 Zn' _chemical_formula_weight 630.17 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.1083(2) _cell_length_b 13.1130(3) _cell_length_c 20.4550(4) _cell_angle_alpha 89.9580(10) _cell_angle_beta 89.9930(10) _cell_angle_gamma 89.9770(10) _cell_volume 3515.99(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.51 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thick 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 0.0298 _diffrn_reflns_av_unetI/netI 0.0579 _diffrn_reflns_number 52346 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 24633 _reflns_number_gt 21292 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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)' #----------------------------------------------------------------------------# # 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^)+(0.0000P)^2^+15.0954P] 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 24633 _refine_ls_number_parameters 1549 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.303 _refine_ls_restrained_S_all 1.303 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.005 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.037(12) _refine_diff_density_max 0.643 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.104 #----------------------------------------------------------------------------# # 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' 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 0.75441(6) 1.39946(5) 1.26535(4) 0.0179(2) Uani 1 1 d . . . Zn2 Zn 0.74921(6) 1.40355(5) 1.57834(4) 0.0177(2) Uani 1 1 d . . . Zn3 Zn 1.25061(6) 1.89483(6) 1.07834(4) 0.0180(2) Uani 1 1 d . . . Zn4 Zn 1.24547(6) 1.89912(5) 0.76541(4) 0.0177(2) Uani 1 1 d . . . N5 N 0.8300(4) 1.5268(4) 1.2241(3) 0.0141(11) Uani 1 1 d . . . N6 N 0.6195(4) 1.3473(4) 1.5480(3) 0.0197(12) Uani 1 1 d . . . N7 N 0.6901(5) 1.2707(4) 1.2221(3) 0.0179(12) Uani 1 1 d . . . N8 N 0.6956(4) 1.5315(4) 1.2905(3) 0.0178(12) Uani 1 1 d . . . N9 N 0.8097(5) 1.2716(4) 1.2977(3) 0.0168(12) Uani 1 1 d . . . N10 N 1.3794(4) 1.8239(4) 1.1207(3) 0.0203(12) Uani 1 1 d . . . N11 N 0.6204(4) 1.4738(4) 1.6208(3) 0.0191(12) Uani 1 1 d . . . N12 N 1.1907(5) 2.0272(4) 0.7981(3) 0.0172(12) Uani 1 1 d . . . N13 N 1.3800(4) 1.9508(4) 1.0483(3) 0.0186(12) Uani 1 1 d . . . N14 N 1.1210(4) 1.8369(4) 1.0511(3) 0.0171(12) Uani 1 1 d . . . N15 N 0.8793(5) 1.4621(4) 1.5511(3) 0.0187(12) Uani 1 1 d . . . N16 N 1.1703(4) 1.7714(4) 0.7243(3) 0.0148(11) Uani 1 1 d . . . N17 N 1.3040(4) 1.7671(4) 0.7908(3) 0.0188(12) Uani 1 1 d . . . N18 N 0.4892(5) 1.2735(4) 1.4851(3) 0.0217(13) Uani 1 1 d . . . N19 N 0.8761(4) 1.3325(4) 1.6208(3) 0.0173(12) Uani 1 1 d . . . N20 N 0.6218(5) 1.6654(4) 1.3495(3) 0.0169(12) Uani 1 1 d . . . N21 N 0.8952(5) 1.1437(4) 1.3588(3) 0.0236(13) Uani 1 1 d . . . C22 C 0.5054(7) 1.6276(5) 1.4375(3) 0.0267(18) Uani 1 1 d . . . H22 H 0.4606 1.6507 1.4709 0.032 Uiso 1 1 calc R . . N23 N 1.1233(4) 1.9662(4) 1.1209(3) 0.0191(12) Uani 1 1 d . . . C24 C 0.7698(5) 1.6968(5) 1.2499(3) 0.0192(15) Uani 1 1 d . . . H24 H 0.7228 1.7416 1.2705 0.023 Uiso 1 1 calc R . . C25 C 0.9255(5) 1.3162(5) 1.3814(3) 0.0193(14) Uani 1 1 d . . . H25 H 0.9141 1.3862 1.372 0.023 Uiso 1 1 calc R . . C26 C 1.4237(5) 1.8080(5) 0.8759(3) 0.0218(15) Uani 1 1 d . . . H26 H 1.4176 1.8784 0.8657 0.026 Uiso 1 1 calc R . . N27 N 1.5108(4) 2.0253(4) 0.9851(3) 0.0193(12) Uani 1 1 d . . . C28 C 0.8385(6) 1.5788(5) 1.4662(3) 0.0234(15) Uani 1 1 d . . . H28 H 0.7678 1.5675 1.4732 0.028 Uiso 1 1 calc R . . C29 C 0.6297(5) 1.5645(5) 1.3402(3) 0.0162(14) Uani 1 1 d . . . N30 N 1.3099(5) 2.0279(4) 0.7217(3) 0.0186(12) Uani 1 1 d . . . C31 C 0.9114(5) 1.5308(5) 1.5036(3) 0.0174(14) Uani 1 1 d . . . C32 C 0.7496(5) 1.2092(5) 1.2582(3) 0.0150(13) Uani 1 1 d . . . C33 C 1.3696(6) 1.7341(5) 0.8404(3) 0.0184(14) Uani 1 1 d . . . C34 C 1.5487(5) 1.8832(6) 1.0918(3) 0.0208(15) Uani 1 1 d . . . H34 H 1.5929 1.9274 1.0684 0.025 Uiso 1 1 calc R . . C35 C 0.5758(6) 1.4906(5) 1.3761(3) 0.0219(15) Uani 1 1 d . . . H35 H 0.5814 1.4201 1.3661 0.026 Uiso 1 1 calc R . . N36 N 0.9870(5) 1.7527(4) 0.9946(3) 0.0197(12) Uani 1 1 d . . . C37 C 0.6083(6) 1.1243(5) 1.1746(4) 0.0240(16) Uani 1 1 d . . . H37 H 0.5614 1.0954 1.1444 0.029 Uiso 1 1 calc R . . C38 C 0.5894(5) 1.2842(5) 1.4998(3) 0.0150(13) Uani 1 1 d . . . C39 C 1.0747(5) 1.9823(5) 0.8815(3) 0.0194(14) Uani 1 1 d . . . H39 H 1.0871 1.9123 0.8725 0.023 Uiso 1 1 calc R . . C40 C 0.6632(5) 1.2276(5) 1.4645(3) 0.0202(14) Uani 1 1 d . . . H40 H 0.7331 1.2327 1.4762 0.024 Uiso 1 1 calc R . . C41 C 0.8733(7) 1.6452(6) 1.4173(4) 0.0252(18) Uani 1 1 d . . . H41 H 0.8251 1.6809 1.3913 0.03 Uiso 1 1 calc R . . N42 N 1.0130(5) 1.5458(4) 1.4949(3) 0.0207(13) Uani 1 1 d . . . C43 C 0.4765(6) 1.5518(7) 1.6704(4) 0.035(2) Uani 1 1 d . . . H43 H 0.448 1.6 1.6998 0.042 Uiso 1 1 calc R . . C44 C 1.4412(5) 1.8875(5) 1.0854(3) 0.0186(14) Uani 1 1 d . . . C45 C 1.2500(5) 2.0890(5) 0.7582(3) 0.0146(13) Uani 1 1 d . . . C46 C 1.2303(6) 1.6025(5) 0.7501(3) 0.0235(16) Uani 1 1 d . . . H46 H 1.2771 1.5573 0.7706 0.028 Uiso 1 1 calc R . . C47 C 0.9736(6) 1.6592(5) 1.4065(3) 0.0254(17) Uani 1 1 d . . . H47 H 0.9966 1.7016 1.3719 0.031 Uiso 1 1 calc R . . C48 C 1.1616(6) 1.7202(5) 0.9666(3) 0.0240(16) Uani 1 1 d . . . H48 H 1.232 1.7316 0.9746 0.029 Uiso 1 1 calc R . . C49 C 0.4513(5) 1.4154(6) 1.5919(3) 0.0205(14) Uani 1 1 d . . . H49 H 0.4068 1.3711 1.5688 0.025 Uiso 1 1 calc R . . C50 C 1.4174(6) 1.7543(6) 1.1623(4) 0.0269(17) Uani 1 1 d . . . C51 C 0.5828(6) 1.5444(6) 1.6626(4) 0.0274(17) Uani 1 1 d . . . C52 C 0.7404(6) 1.1032(5) 1.2553(3) 0.0220(15) Uani 1 1 d . . . H52 H 0.7833 1.0605 1.2809 0.026 Uiso 1 1 calc R . . C53 C 0.7643(5) 1.5900(5) 1.2577(3) 0.0176(14) Uani 1 1 d . . . C54 C 0.6186(6) 1.2299(5) 1.1797(3) 0.0204(15) Uani 1 1 d . . . C55 C 0.5161(6) 1.5232(6) 1.4253(4) 0.0209(16) Uani 1 1 d . . . H55 H 0.481 1.4752 1.4519 0.025 Uiso 1 1 calc R . . C56 C 1.4956(6) 1.6713(5) 0.9375(3) 0.0254(17) Uani 1 1 d . . . H56 H 1.5407 1.6482 0.9707 0.031 Uiso 1 1 calc R . . C57 C 0.9051(5) 1.5613(5) 1.1886(3) 0.0192(14) Uani 1 1 d . . . N58 N 1.1062(4) 2.1556(4) 0.8588(3) 0.0223(13) Uani 1 1 d . . . N59 N 1.3777(4) 1.6324(4) 0.8503(3) 0.0161(11) Uani 1 1 d . . . C60 C 1.0616(5) 1.9018(5) 1.0873(3) 0.0165(14) Uani 1 1 d . . . C61 C 0.9550(6) 1.9127(6) 1.0912(4) 0.0244(16) Uani 1 1 d . . . H61 H 0.9112 1.869 1.067 0.029 Uiso 1 1 calc R . . C62 C 1.3363(6) 2.0709(5) 0.9647(4) 0.0219(15) Uani 1 1 d . . . H62 H 1.2665 2.0661 0.9768 0.026 Uiso 1 1 calc R . . C63 C 1.1238(5) 2.0574(6) 0.8452(3) 0.0228(15) Uani 1 1 d . . . C64 C 0.9601(6) 1.1156(6) 1.4053(4) 0.0299(18) Uani 1 1 d . . . C65 C 1.5228(6) 1.7466(7) 1.1709(4) 0.035(2) Uani 1 1 d . . . H65 H 1.5507 1.699 1.2011 0.042 Uiso 1 1 calc R . . C66 C 0.9395(5) 1.3972(5) 1.5871(3) 0.0159(14) Uani 1 1 d . . . C67 C 1.3925(6) 2.1743(5) 0.6742(4) 0.0239(16) Uani 1 1 d . . . H67 H 1.44 2.2032 0.6444 0.029 Uiso 1 1 calc R . . C68 C 1.0442(6) 1.3861(6) 1.5916(4) 0.0250(16) Uani 1 1 d . . . H68 H 1.088 1.4303 1.5678 0.03 Uiso 1 1 calc R . . C69 C 0.8766(5) 1.2415(5) 1.3451(3) 0.0212(15) Uani 1 1 d . . . C70 C 1.2363(5) 1.7090(5) 0.7578(3) 0.0180(14) Uani 1 1 d . . . C71 C 1.0265(6) 1.6386(5) 0.9070(3) 0.0222(16) Uani 1 1 d . . . H71 H 1.0038 1.5941 0.8734 0.027 Uiso 1 1 calc R . . C72 C 0.9153(6) 1.2581(6) 1.6579(4) 0.0281(17) Uani 1 1 d . . . C73 C 0.8491(7) 1.7324(5) 1.2100(4) 0.0309(19) Uani 1 1 d . . . H73 H 0.8567 1.8036 1.2032 0.037 Uiso 1 1 calc R . . C74 C 1.2589(6) 2.1955(5) 0.7553(3) 0.0227(16) Uani 1 1 d . . . H74 H 1.2163 2.2387 0.7807 0.027 Uiso 1 1 calc R . . C75 C 1.4123(5) 2.0146(5) 0.9998(3) 0.0173(14) Uani 1 1 d . . . C76 C 1.0956(6) 1.7377(5) 0.6891(3) 0.0203(15) Uani 1 1 d . . . C77 C 1.0175(6) 1.2441(6) 1.6648(4) 0.0301(18) Uani 1 1 d . . . H77 H 1.0438 1.1912 1.6917 0.036 Uiso 1 1 calc R . . C78 C 0.5575(5) 1.4107(5) 1.5847(3) 0.0200(15) Uani 1 1 d . . . C79 C 0.5608(6) 1.6975(5) 1.4005(4) 0.0213(15) Uani 1 1 d . . . C80 C 1.4845(6) 1.7759(6) 0.9251(4) 0.0247(18) Uani 1 1 d . . . H80 H 1.5197 1.8242 0.9513 0.03 Uiso 1 1 calc R . . C81 C 1.0865(6) 1.7669(5) 1.0032(3) 0.0189(14) Uani 1 1 d . . . C82 C 1.3807(6) 2.0683(5) 0.6794(3) 0.0194(14) Uani 1 1 d . . . C83 C 1.0385(6) 1.5261(5) 1.1017(4) 0.0248(16) Uani 1 1 d . . . H83A H 1.0849 1.4739 1.0847 0.037 Uiso 1 1 calc R . . H83B H 1.0779 1.5857 1.1158 0.037 Uiso 1 1 calc R . . H83C H 0.9905 1.5464 1.0673 0.037 Uiso 1 1 calc R . . C84 C 1.1277(6) 1.6551(6) 0.9169(4) 0.0243(18) Uani 1 1 d . . . H84 H 1.1762 1.6219 0.8897 0.029 Uiso 1 1 calc R . . C85 C 1.1575(6) 1.6204(6) 1.4394(4) 0.0279(18) Uani 1 1 d . . . C86 C 0.9165(6) 1.6657(5) 1.1804(4) 0.0264(17) Uani 1 1 d . . . H86 H 0.9707 1.6914 1.1543 0.032 Uiso 1 1 calc R . . C87 C 0.9787(6) 1.4826(5) 1.1605(3) 0.0222(16) Uani 1 1 d . . . C88 C 0.9715(8) 1.0012(8) 1.4184(6) 0.049(3) Uani 1 1 d . . . C89 C 1.0413(6) 2.1833(6) 0.9049(4) 0.0299(18) Uani 1 1 d . . . C90 C 0.8437(7) 1.6776(6) 0.9395(4) 0.0303(18) Uani 1 1 d . . . C91 C 0.5318(6) 1.1588(5) 1.3997(4) 0.0295(18) Uani 1 1 d . . . H91 H 0.5097 1.1163 1.3648 0.035 Uiso 1 1 calc R . . C92 C 0.6358(7) 1.1665(6) 1.4144(4) 0.0260(18) Uani 1 1 d . . . H92 H 0.6854 1.13 1.39 0.031 Uiso 1 1 calc R . . C93 C 0.6677(5) 1.0621(5) 1.2145(3) 0.0196(14) Uani 1 1 d . . . H93 H 0.658 0.9903 1.2136 0.024 Uiso 1 1 calc R . . C94 C 0.9915(6) 1.2882(6) 1.4318(4) 0.0244(17) Uani 1 1 d . . . H94 H 1.0265 1.3389 1.4562 0.029 Uiso 1 1 calc R . . C95 C 1.0217(6) 1.8153(5) 0.6605(3) 0.0210(15) Uani 1 1 d . . . C96 C 1.0058(6) 1.1855(6) 1.4461(4) 0.0322(18) Uani 1 1 d . . . H96 H 1.0456 1.1644 1.4825 0.039 Uiso 1 1 calc R . . C97 C 1.0429(6) 1.6096(5) 1.4477(4) 0.0233(16) Uani 1 1 d . . . C98 C 1.3650(6) 2.1314(6) 0.9138(4) 0.0232(17) Uani 1 1 d . . . H98 H 1.3155 2.1661 0.8882 0.028 Uiso 1 1 calc R . . C99 C 1.0321(8) 2.2993(6) 0.9185(5) 0.043(3) Uani 1 1 d . . . C100 C 0.4613(6) 1.2132(6) 1.4360(3) 0.0218(15) Uani 1 1 d . . . C101 C 1.3922(9) 1.4266(7) 0.8580(6) 0.053(3) Uani 1 1 d . . . H10A H 1.3972 1.3537 0.8681 0.08 Uiso 1 1 calc R . . H10B H 1.4268 1.4406 0.8164 0.08 Uiso 1 1 calc R . . H10C H 1.3202 1.4461 0.8545 0.08 Uiso 1 1 calc R . . C102 C 0.4151(6) 1.4892(6) 1.6352(4) 0.0311(18) Uani 1 1 d . . . H102 H 0.3434 1.4959 1.6404 0.037 Uiso 1 1 calc R . . C103 C 0.9828(6) 2.0537(6) 1.1645(4) 0.0300(18) Uani 1 1 d . . . H103 H 0.9568 2.1063 1.1917 0.036 Uiso 1 1 calc R . . C104 C 1.4704(6) 2.1414(6) 0.9000(4) 0.0302(18) Uani 1 1 d . . . H104 H 1.4931 2.1856 0.8662 0.036 Uiso 1 1 calc R . . C105 C 1.1678(7) 2.1146(8) 1.1862(5) 0.048(3) Uani 1 1 d . . . C106 C 1.3876(7) 1.6295(8) 1.2521(4) 0.045(3) Uani 1 1 d . . . H10D H 1.3371 1.583 1.2711 0.067 Uiso 1 1 calc R . . H10E H 1.407 1.6807 1.2846 0.067 Uiso 1 1 calc R . . H10F H 1.4481 1.5907 1.2389 0.067 Uiso 1 1 calc R . . C107 C 1.1504(7) 1.5673(5) 0.7101(4) 0.0309(19) Uani 1 1 d . . . H107 H 1.1427 1.496 0.7032 0.037 Uiso 1 1 calc R . . C108 C 1.0557(6) 1.4587(6) 1.2164(4) 0.0323(19) Uani 1 1 d . . . H10G H 1.1055 1.4084 1.2011 0.048 Uiso 1 1 calc R . . H10H H 1.0188 1.4313 1.2542 0.048 Uiso 1 1 calc R . . H10I H 1.0911 1.5215 1.2291 0.048 Uiso 1 1 calc R . . C109 C 1.3328(5) 2.2351(5) 0.7136(3) 0.0204(15) Uani 1 1 d . . . H109 H 1.3425 2.3069 0.7122 0.025 Uiso 1 1 calc R . . C110 C 1.0071(6) 2.0101(6) 0.9313(4) 0.0255(18) Uani 1 1 d . . . H110 H 0.9707 1.9596 0.9551 0.031 Uiso 1 1 calc R . . C111 C 1.6554(7) 2.0847(7) 0.9207(4) 0.031(2) Uani 1 1 d . . . C112 C 1.5391(6) 2.0863(6) 0.9362(3) 0.0229(16) Uani 1 1 d . . . C113 C 0.9562(6) 1.6889(5) 0.9476(4) 0.0224(16) Uani 1 1 d . . . C114 C 1.4395(6) 1.6011(5) 0.9005(4) 0.0218(15) Uani 1 1 d . . . C115 C 1.0844(6) 1.3118(6) 1.6301(3) 0.0256(16) Uani 1 1 d . . . H115 H 1.1563 1.3047 1.6341 0.031 Uiso 1 1 calc R . . C116 C 0.9157(6) 1.9871(6) 1.1302(3) 0.0267(17) Uani 1 1 d . . . H116 H 0.8439 1.9946 1.1346 0.032 Uiso 1 1 calc R . . C117 C 0.9252(7) 1.3856(6) 1.1399(5) 0.046(3) Uani 1 1 d . . . H11A H 0.9753 1.3377 1.1219 0.069 Uiso 1 1 calc R . . H11B H 0.8741 1.4015 1.1064 0.069 Uiso 1 1 calc R . . H11C H 0.8916 1.3548 1.1779 0.069 Uiso 1 1 calc R . . C118 C 1.3427(7) 1.6814(7) 1.1935(4) 0.038(2) Uani 1 1 d . . . C119 C 0.3424(7) 1.2119(7) 1.4210(4) 0.032(2) Uani 1 1 d . . . C120 C 1.0850(6) 2.0404(6) 1.1573(4) 0.0284(17) Uani 1 1 d . . . C121 C 0.9941(6) 2.1135(6) 0.9454(4) 0.0297(18) Uani 1 1 d . . . H121 H 0.9542 2.135 0.9816 0.036 Uiso 1 1 calc R . . C122 C 1.1170(8) 2.1835(8) 1.2397(5) 0.049(2) Uani 1 1 d . . . H12A H 1.0604 2.2218 1.2203 0.074 Uiso 1 1 calc R . . H12B H 1.1678 2.2311 1.2571 0.074 Uiso 1 1 calc R . . H12C H 1.0912 2.1405 1.2753 0.074 Uiso 1 1 calc R . . C123 C 1.6912(8) 2.1929(8) 0.9013(7) 0.073(4) Uani 1 1 d . . . H12D H 1.6817 2.2393 0.9383 0.11 Uiso 1 1 calc R . . H12E H 1.6512 2.2171 0.8639 0.11 Uiso 1 1 calc R . . H12F H 1.7636 2.1909 0.8894 0.11 Uiso 1 1 calc R . . C124 C 0.5509(7) 1.3043(6) 1.1428(4) 0.036(2) Uani 1 1 d . . . C125 C 0.8322(6) 1.1831(8) 1.6862(5) 0.046(3) Uani 1 1 d . . . C126 C 0.5592(7) 1.8128(6) 1.4099(4) 0.035(2) Uani 1 1 d . . . C127 C 0.6101(9) 1.8731(7) 1.3575(5) 0.051(3) Uani 1 1 d . . . H12G H 0.6052 1.9459 1.3678 0.076 Uiso 1 1 calc R . . H12H H 0.5766 1.8596 1.3156 0.076 Uiso 1 1 calc R . . H12I H 0.6821 1.8533 1.3548 0.076 Uiso 1 1 calc R . . C130 C 0.8000(8) 1.1114(8) 1.6299(5) 0.053(3) Uani 1 1 d . . . H13A H 0.8602 1.0759 1.6129 0.079 Uiso 1 1 calc R . . H13B H 0.7686 1.1514 1.5949 0.079 Uiso 1 1 calc R . . H13C H 0.7508 1.0613 1.6464 0.079 Uiso 1 1 calc R . . C131 C 1.0489(8) 0.9690(8) 1.4601(6) 0.053(3) Uani 1 1 d . . . H13D H 1.0474 0.8945 1.4637 0.079 Uiso 1 1 calc R . . H13E H 1.0389 0.9993 1.5034 0.079 Uiso 1 1 calc R . . H13F H 1.1151 0.9906 1.4425 0.079 Uiso 1 1 calc R . . C132 C 0.4509(9) 1.8463(7) 1.4315(7) 0.067(4) Uani 1 1 d . . . H13G H 0.4262 1.8005 1.4658 0.1 Uiso 1 1 calc R . . H13H H 0.4046 1.8435 1.3939 0.1 Uiso 1 1 calc R . . H13I H 0.4535 1.9162 1.4483 0.1 Uiso 1 1 calc R . . C133 C 1.0831(6) 1.6332(5) 0.6806(4) 0.0238(16) Uani 1 1 d . . . H133 H 1.0287 1.6077 0.6547 0.029 Uiso 1 1 calc R . . C134 C 0.9439(7) 1.8395(6) 0.7164(4) 0.0311(18) Uani 1 1 d . . . H13J H 0.8941 1.8897 0.7008 0.047 Uiso 1 1 calc R . . H13K H 0.9805 1.8672 0.7542 0.047 Uiso 1 1 calc R . . H13L H 0.9084 1.7768 0.7291 0.047 Uiso 1 1 calc R . . C135 C 1.5460(8) 1.4507(7) 0.9320(7) 0.061(3) Uani 1 1 d . . . H13M H 1.5716 1.4957 0.9665 0.091 Uiso 1 1 calc R . . H13N H 1.5927 1.4526 0.8946 0.091 Uiso 1 1 calc R . . H13O H 1.5415 1.3807 0.9487 0.091 Uiso 1 1 calc R . . C136 C 1.4498(7) 1.9939(5) 0.6432(4) 0.0321(19) Uani 1 1 d . . . C137 C 0.9618(6) 1.7722(6) 0.6023(4) 0.0279(17) Uani 1 1 d . . . H13P H 0.9154 1.8245 0.5854 0.042 Uiso 1 1 calc R . . H13Q H 0.9224 1.7127 0.6166 0.042 Uiso 1 1 calc R . . H13R H 1.0095 1.7518 0.5678 0.042 Uiso 1 1 calc R . . C138 C 0.7555(8) 1.5578(10) 1.7150(6) 0.071(4) Uani 1 1 d . . . H13S H 0.7843 1.5224 1.6771 0.107 Uiso 1 1 calc R . . H13T H 0.7379 1.5078 1.7488 0.107 Uiso 1 1 calc R . . H13U H 0.8059 1.6059 1.7324 0.107 Uiso 1 1 calc R . . C140 C 1.2004(7) 2.1884(8) 1.1301(5) 0.052(3) Uani 1 1 d . . . H14A H 1.1401 2.2235 1.1129 0.077 Uiso 1 1 calc R . . H14B H 1.2329 2.1493 1.095 0.077 Uiso 1 1 calc R . . H14C H 1.2488 2.2387 1.1472 0.077 Uiso 1 1 calc R . . C141 C 1.5848(6) 1.8090(7) 1.1351(4) 0.0309(18) Uani 1 1 d . . . H141 H 1.6565 1.8016 1.1399 0.037 Uiso 1 1 calc R . . C142 C 0.8005(8) 1.7776(8) 0.9149(7) 0.070(4) Uani 1 1 d . . . H14D H 0.7265 1.7714 0.9098 0.105 Uiso 1 1 calc R . . H14E H 0.8314 1.7943 0.8725 0.105 Uiso 1 1 calc R . . H14F H 0.8158 1.8318 0.9463 0.105 Uiso 1 1 calc R . . C143 C 1.1335(7) 2.3445(7) 0.9352(5) 0.045(2) Uani 1 1 d . . . H14G H 1.1848 2.3206 0.9039 0.067 Uiso 1 1 calc R . . H14H H 1.1532 2.3234 0.9794 0.067 Uiso 1 1 calc R . . H14I H 1.1291 2.419 0.9332 0.067 Uiso 1 1 calc R . . C144 C 0.7462(10) 1.2424(10) 1.7160(7) 0.096(6) Uani 1 1 d . . . H14J H 0.7728 1.286 1.7509 0.144 Uiso 1 1 calc R . . H14K H 0.6958 1.1951 1.7341 0.144 Uiso 1 1 calc R . . H14L H 0.714 1.2849 1.6824 0.144 Uiso 1 1 calc R . . C145 C 0.6142(7) 1.6702(7) 1.7524(4) 0.040(2) Uani 1 1 d . . . H14M H 0.6657 1.7161 1.7707 0.06 Uiso 1 1 calc R . . H14N H 0.5948 1.6194 1.7853 0.06 Uiso 1 1 calc R . . H14O H 0.554 1.7097 1.7395 0.06 Uiso 1 1 calc R . . C146 C 0.8678(7) 0.9547(7) 1.4363(5) 0.046(2) Uani 1 1 d . . . H14P H 0.816 0.9783 1.4053 0.069 Uiso 1 1 calc R . . H14Q H 0.8488 0.9758 1.4806 0.069 Uiso 1 1 calc R . . H14R H 0.8724 0.8801 1.4345 0.069 Uiso 1 1 calc R . . C147 C 0.6125(10) 1.3921(9) 1.1168(6) 0.080(5) Uani 1 1 d . . . H14S H 0.6504 1.4238 1.1527 0.12 Uiso 1 1 calc R . . H14T H 0.5667 1.4425 1.097 0.12 Uiso 1 1 calc R . . H14U H 0.6605 1.3672 1.0837 0.12 Uiso 1 1 calc R . . C148 C 1.4411(7) 1.4862(6) 0.9106(4) 0.034(2) Uani 1 1 d . . . C150 C 0.2801(8) 1.2560(8) 1.4792(5) 0.051(3) Uani 1 1 d . . . H15A H 0.3047 1.3247 1.4895 0.076 Uiso 1 1 calc R . . H15B H 0.2885 1.2118 1.5175 0.076 Uiso 1 1 calc R . . H15C H 0.2077 1.2592 1.4673 0.076 Uiso 1 1 calc R . . C151 C 1.2436(7) 1.7387(10) 1.2149(6) 0.072(4) Uani 1 1 d . . . H15D H 1.2138 1.7736 1.1771 0.107 Uiso 1 1 calc R . . H15E H 1.2604 1.7889 1.2487 0.107 Uiso 1 1 calc R . . H15F H 1.1943 1.6895 1.2324 0.107 Uiso 1 1 calc R . . C152 C 1.2007(8) 1.5224(8) 1.4144(8) 0.072(4) Uani 1 1 d . . . H15G H 1.2748 1.5292 1.4093 0.108 Uiso 1 1 calc R . . H15H H 1.1699 1.5063 1.372 0.108 Uiso 1 1 calc R . . H15I H 1.1859 1.4676 1.4455 0.108 Uiso 1 1 calc R . . C153 C 0.4897(8) 1.2525(7) 1.0908(4) 0.044(2) Uani 1 1 d . . . H15J H 0.4469 1.3028 1.0684 0.066 Uiso 1 1 calc R . . H15K H 0.4462 1.2003 1.1108 0.066 Uiso 1 1 calc R . . H15L H 0.5358 1.2203 1.0593 0.066 Uiso 1 1 calc R . . C154 C 1.7189(8) 2.0423(8) 0.9796(5) 0.051(3) Uani 1 1 d . . . H15M H 1.7095 2.0866 1.0177 0.076 Uiso 1 1 calc R . . H15N H 1.7914 2.0404 0.9677 0.076 Uiso 1 1 calc R . . H15O H 1.6957 1.9732 0.9902 0.076 Uiso 1 1 calc R . . C155 C 0.8105(9) 1.5957(9) 0.8937(8) 0.079(4) Uani 1 1 d . . . H15P H 0.7359 1.5942 0.8917 0.118 Uiso 1 1 calc R . . H15Q H 0.8358 1.5297 0.9093 0.118 Uiso 1 1 calc R . . H15R H 0.8381 1.6095 0.8501 0.118 Uiso 1 1 calc R . . C156 C 0.6570(7) 1.6174(7) 1.6938(4) 0.036(2) Uani 1 1 d . . . C157 C 1.3748(9) 1.4669(8) 0.9756(5) 0.055(3) Uani 1 1 d . . . H15S H 1.4045 1.5051 1.012 0.082 Uiso 1 1 calc R . . H15T H 1.3749 1.3939 0.986 0.082 Uiso 1 1 calc R . . H15U H 1.3045 1.4897 0.9682 0.082 Uiso 1 1 calc R . . C160 C 0.9520(7) 2.3296(8) 0.9605(6) 0.052(3) Uani 1 1 d . . . H16A H 0.8883 2.2972 0.9464 0.078 Uiso 1 1 calc R . . H16B H 0.9444 2.4039 0.9587 0.078 Uiso 1 1 calc R . . H16C H 0.9679 2.3087 1.0053 0.078 Uiso 1 1 calc R . . C161 C 0.4768(9) 1.3495(8) 1.1933(5) 0.061(3) Uani 1 1 d . . . H16D H 0.5157 1.384 1.2277 0.092 Uiso 1 1 calc R . . H16E H 0.4359 1.2947 1.2126 0.092 Uiso 1 1 calc R . . H16F H 0.4317 1.3987 1.1717 0.092 Uiso 1 1 calc R . . C162 C 0.9970(10) 2.3477(8) 0.8448(6) 0.064(3) Uani 1 1 d . . . H16G H 1.0483 2.3298 0.8119 0.096 Uiso 1 1 calc R . . H16H H 0.9915 2.4221 0.8479 0.096 Uiso 1 1 calc R . . H16I H 0.9308 2.3192 0.8321 0.096 Uiso 1 1 calc R . . C163 C 1.3130(8) 1.6032(8) 1.1412(5) 0.055(3) Uani 1 1 d . . . H16J H 1.2844 1.6386 1.1032 0.083 Uiso 1 1 calc R . . H16K H 1.2621 1.5562 1.1591 0.083 Uiso 1 1 calc R . . H16L H 1.3737 1.5647 1.1279 0.083 Uiso 1 1 calc R . . C164 C 1.5102(7) 2.0465(7) 0.5909(4) 0.041(2) Uani 1 1 d . . . H16M H 1.5508 2.1013 0.6104 0.061 Uiso 1 1 calc R . . H16N H 1.4636 2.0752 0.5583 0.061 Uiso 1 1 calc R . . H16O H 1.5557 1.9972 0.5698 0.061 Uiso 1 1 calc R . . C165 C 0.6862(8) 1.6939(8) 1.6409(5) 0.058(3) Uani 1 1 d . . . H16P H 0.7141 1.6575 1.6031 0.087 Uiso 1 1 calc R . . H16Q H 0.7376 1.7411 1.658 0.087 Uiso 1 1 calc R . . H16R H 0.6255 1.7324 1.6275 0.087 Uiso 1 1 calc R . . C166 C 1.3880(10) 1.9078(9) 0.6163(6) 0.078(5) Uani 1 1 d . . . H16S H 1.3498 1.8752 0.6518 0.118 Uiso 1 1 calc R . . H16T H 1.4335 1.8577 0.596 0.118 Uiso 1 1 calc R . . H16U H 1.3403 1.934 0.5834 0.118 Uiso 1 1 calc R . . C170 C 1.0025(9) 0.9513(8) 1.3459(6) 0.062(3) Uani 1 1 d . . . H17A H 0.9513 0.9711 1.3133 0.093 Uiso 1 1 calc R . . H17B H 1.0048 0.8768 1.3494 0.093 Uiso 1 1 calc R . . H17C H 1.0696 0.9768 1.3325 0.093 Uiso 1 1 calc R . . C171 C 1.2538(10) 2.0574(10) 1.2158(7) 0.095(6) Uani 1 1 d . . . H17D H 1.2279 2.013 1.2506 0.143 Uiso 1 1 calc R . . H17E H 1.3032 2.1056 1.2341 0.143 Uiso 1 1 calc R . . H17F H 1.2871 2.0158 1.1822 0.143 Uiso 1 1 calc R . . C172 C 1.0746(8) 1.9129(6) 0.6401(5) 0.047(3) Uani 1 1 d . . . H17G H 1.0243 1.9605 0.6221 0.07 Uiso 1 1 calc R . . H17H H 1.1261 1.8975 0.6068 0.07 Uiso 1 1 calc R . . H17I H 1.1078 1.9438 0.6782 0.07 Uiso 1 1 calc R . . C180 C 0.7984(8) 1.6425(9) 1.0037(5) 0.059(3) Uani 1 1 d . . . H18A H 0.7243 1.6356 0.999 0.088 Uiso 1 1 calc R . . H18B H 0.8137 1.6927 1.0378 0.088 Uiso 1 1 calc R . . H18C H 0.8279 1.5765 1.0158 0.088 Uiso 1 1 calc R . . C181 C 0.8819(7) 1.1145(7) 1.7409(4) 0.043(2) Uani 1 1 d . . . H18D H 0.9368 1.0734 1.7219 0.065 Uiso 1 1 calc R . . H18E H 0.8299 1.0693 1.7595 0.065 Uiso 1 1 calc R . . H18F H 0.9098 1.1581 1.7755 0.065 Uiso 1 1 calc R . . C182 C 0.6241(9) 1.8314(8) 1.4753(5) 0.056(3) Uani 1 1 d . . . H18G H 0.5935 1.7931 1.5115 0.084 Uiso 1 1 calc R . . H18H H 0.6242 1.9043 1.4859 0.084 Uiso 1 1 calc R . . H18I H 0.6944 1.8081 1.4685 0.084 Uiso 1 1 calc R . . C183 C 1.5214(9) 1.9475(8) 0.6930(5) 0.060(3) Uani 1 1 d . . . H18J H 1.4815 1.913 0.727 0.089 Uiso 1 1 calc R . . H18K H 1.5628 2.0014 0.7129 0.089 Uiso 1 1 calc R . . H18L H 1.5661 1.8981 0.6714 0.089 Uiso 1 1 calc R . . C190 C 0.3102(9) 1.1069(8) 1.3993(8) 0.085(5) Uani 1 1 d . . . H19A H 0.3191 1.0587 1.4355 0.127 Uiso 1 1 calc R . . H19B H 0.3523 1.0854 1.3622 0.127 Uiso 1 1 calc R . . H19C H 0.2384 1.1082 1.3862 0.127 Uiso 1 1 calc R . . C191 C 0.3274(9) 1.2840(7) 1.3634(6) 0.056(3) Uani 1 1 d . . . H19D H 0.349 1.3528 1.3759 0.084 Uiso 1 1 calc R . . H19E H 0.2551 1.2852 1.3511 0.084 Uiso 1 1 calc R . . H19F H 0.3683 1.2605 1.3263 0.084 Uiso 1 1 calc R . . C192 C 1.1879(9) 1.7025(8) 1.3919(8) 0.078(5) Uani 1 1 d . . . H19G H 1.1607 1.7682 1.4066 0.118 Uiso 1 1 calc R . . H19H H 1.1604 1.6865 1.3485 0.118 Uiso 1 1 calc R . . H19I H 1.2625 1.7063 1.3895 0.118 Uiso 1 1 calc R . . C193 C 1.2018(8) 1.6563(9) 1.5038(5) 0.059(3) Uani 1 1 d . . . H19J H 1.17 1.721 1.5163 0.089 Uiso 1 1 calc R . . H19K H 1.2756 1.6658 1.4992 0.089 Uiso 1 1 calc R . . H19L H 1.1884 1.6051 1.5377 0.089 Uiso 1 1 calc R . . C194 C 1.6709(9) 2.0132(7) 0.8626(6) 0.055(3) Uani 1 1 d . . . H19M H 1.7436 2.0099 0.8517 0.082 Uiso 1 1 calc R . . H19N H 1.6326 2.039 0.8249 0.082 Uiso 1 1 calc R . . H19O H 1.6463 1.9449 0.874 0.082 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 0.0222(5) 0.0120(4) 0.0195(4) 0.0008(3) 0.0010(4) 0.0019(4) Zn2 0.0136(4) 0.0202(5) 0.0194(4) 0.0000(4) 0.0006(3) -0.0004(4) Zn3 0.0141(4) 0.0207(5) 0.0191(4) 0.0003(4) 0.0001(3) 0.0006(4) Zn4 0.0211(5) 0.0124(4) 0.0196(4) -0.0003(3) 0.0003(4) 0.0019(4) N5 0.011(3) 0.017(3) 0.014(3) 0.001(2) -0.004(2) 0.001(2) N6 0.012(3) 0.021(3) 0.026(3) 0.001(2) 0.002(2) 0.006(2) N7 0.023(3) 0.015(3) 0.015(3) -0.001(2) -0.003(2) -0.001(2) N8 0.020(3) 0.015(3) 0.019(3) 0.004(2) 0.008(2) 0.004(2) N9 0.029(3) 0.005(2) 0.016(3) -0.001(2) -0.004(2) -0.002(2) N10 0.016(3) 0.026(3) 0.019(3) 0.002(2) -0.001(2) 0.004(2) N11 0.012(3) 0.025(3) 0.021(3) -0.003(2) 0.001(2) -0.001(2) N12 0.024(3) 0.009(2) 0.018(3) 0.002(2) 0.004(2) -0.001(2) N13 0.008(3) 0.021(3) 0.027(3) 0.001(2) 0.002(2) 0.000(2) N14 0.019(3) 0.015(3) 0.017(3) -0.004(2) 0.001(2) -0.003(2) N15 0.023(3) 0.013(3) 0.020(3) 0.006(2) -0.001(2) 0.001(2) N16 0.012(3) 0.018(3) 0.014(3) -0.001(2) 0.003(2) 0.000(2) N17 0.019(3) 0.017(3) 0.021(3) -0.005(2) -0.005(2) 0.005(2) N18 0.017(3) 0.015(3) 0.033(3) 0.008(2) -0.002(3) 0.001(2) N19 0.018(3) 0.019(3) 0.015(3) 0.002(2) 0.003(2) 0.001(2) N20 0.025(3) 0.007(2) 0.018(3) -0.002(2) 0.012(2) -0.004(2) N21 0.021(3) 0.017(3) 0.034(3) 0.000(2) -0.009(3) -0.003(2) C22 0.045(5) 0.022(4) 0.013(3) 0.005(3) 0.015(3) 0.003(3) N23 0.017(3) 0.025(3) 0.016(3) -0.001(2) -0.001(2) 0.004(2) C24 0.024(4) 0.012(3) 0.021(3) -0.001(3) 0.013(3) 0.006(3) C25 0.022(4) 0.017(3) 0.018(3) 0.003(3) 0.001(3) -0.009(3) C26 0.020(4) 0.017(3) 0.029(4) -0.003(3) -0.006(3) 0.006(3) N27 0.014(3) 0.017(3) 0.027(3) -0.006(2) 0.002(2) -0.001(2) C28 0.020(4) 0.027(4) 0.024(4) 0.007(3) -0.003(3) 0.000(3) C29 0.022(4) 0.010(3) 0.016(3) 0.000(2) 0.006(3) 0.001(3) N30 0.022(3) 0.017(3) 0.017(3) 0.001(2) 0.006(2) -0.001(2) C31 0.024(4) 0.009(3) 0.019(3) 0.000(2) 0.001(3) 0.001(3) C32 0.016(3) 0.013(3) 0.016(3) -0.010(2) 0.006(3) 0.000(3) C33 0.027(4) 0.012(3) 0.016(3) -0.004(2) -0.004(3) 0.003(3) C34 0.011(3) 0.033(4) 0.018(3) 0.001(3) -0.001(3) 0.000(3) C35 0.028(4) 0.015(3) 0.022(4) 0.002(3) 0.005(3) 0.005(3) N36 0.020(3) 0.018(3) 0.021(3) 0.000(2) -0.005(2) -0.003(2) C37 0.024(4) 0.025(4) 0.023(4) -0.007(3) 0.001(3) -0.002(3) C38 0.015(3) 0.009(3) 0.022(3) 0.003(2) -0.001(3) 0.000(2) C39 0.016(4) 0.019(3) 0.022(4) 0.000(3) 0.002(3) -0.006(3) C40 0.015(3) 0.017(3) 0.029(4) 0.006(3) -0.007(3) 0.000(3) C41 0.038(5) 0.016(4) 0.022(4) 0.004(3) -0.008(3) 0.005(3) N42 0.019(3) 0.019(3) 0.024(3) -0.002(2) 0.004(2) -0.003(2) C43 0.020(4) 0.042(5) 0.044(5) -0.002(4) 0.012(4) 0.011(4) C44 0.016(3) 0.017(3) 0.024(4) -0.006(3) 0.002(3) -0.005(3) C45 0.013(3) 0.017(3) 0.014(3) 0.010(2) -0.006(2) 0.000(3) C46 0.029(4) 0.023(4) 0.019(4) 0.000(3) -0.012(3) 0.005(3) C47 0.040(5) 0.020(4) 0.016(4) 0.008(3) 0.006(3) -0.004(3) C48 0.025(4) 0.027(4) 0.020(4) -0.005(3) 0.005(3) 0.002(3) C49 0.011(3) 0.031(4) 0.019(3) -0.001(3) 0.002(3) -0.008(3) C50 0.022(4) 0.038(4) 0.021(4) 0.006(3) 0.003(3) 0.009(3) C51 0.019(4) 0.041(4) 0.022(4) -0.009(3) 0.000(3) 0.012(3) C52 0.028(4) 0.013(3) 0.025(4) -0.004(3) 0.013(3) 0.001(3) C53 0.017(4) 0.016(3) 0.019(3) -0.004(3) 0.004(3) 0.000(3) C54 0.026(4) 0.019(3) 0.016(3) -0.008(3) 0.003(3) 0.006(3) C55 0.017(4) 0.023(4) 0.023(4) 0.014(3) 0.006(3) -0.004(3) C56 0.041(5) 0.021(4) 0.014(3) -0.001(3) -0.014(3) 0.001(3) C57 0.017(3) 0.028(4) 0.013(3) -0.001(3) 0.001(3) 0.005(3) N58 0.014(3) 0.020(3) 0.033(3) 0.003(2) 0.011(3) -0.001(2) N59 0.017(3) 0.011(3) 0.020(3) 0.001(2) -0.012(2) -0.005(2) C60 0.019(4) 0.021(3) 0.009(3) 0.007(2) 0.007(3) 0.007(3) C61 0.024(4) 0.023(4) 0.026(4) 0.005(3) 0.001(3) 0.002(3) C62 0.018(4) 0.016(3) 0.032(4) -0.008(3) 0.007(3) 0.001(3) C63 0.013(3) 0.032(4) 0.024(4) -0.005(3) -0.003(3) 0.001(3) C64 0.030(5) 0.020(4) 0.039(5) 0.004(3) -0.010(4) -0.005(3) C65 0.023(4) 0.047(5) 0.035(4) 0.006(4) -0.008(3) 0.014(4) C66 0.020(4) 0.020(3) 0.008(3) -0.004(2) -0.003(2) 0.006(3) C67 0.025(4) 0.020(3) 0.026(4) 0.009(3) -0.001(3) -0.004(3) C68 0.022(4) 0.023(4) 0.030(4) -0.004(3) 0.001(3) -0.002(3) C69 0.013(3) 0.026(4) 0.025(4) 0.006(3) 0.002(3) -0.001(3) C70 0.019(4) 0.016(3) 0.019(3) 0.006(3) -0.002(3) 0.000(3) C71 0.036(5) 0.016(3) 0.015(3) -0.007(3) -0.002(3) -0.012(3) C72 0.025(4) 0.036(4) 0.023(4) 0.012(3) 0.004(3) 0.002(3) C73 0.060(6) 0.010(3) 0.023(4) -0.002(3) 0.003(4) -0.005(3) C74 0.026(4) 0.019(3) 0.024(4) 0.007(3) -0.014(3) 0.000(3) C75 0.017(3) 0.011(3) 0.024(4) -0.006(3) 0.001(3) 0.002(3) C76 0.025(4) 0.023(3) 0.013(3) 0.003(3) 0.001(3) 0.006(3) C77 0.031(4) 0.039(4) 0.020(4) 0.020(3) -0.002(3) 0.002(4) C78 0.015(4) 0.020(3) 0.025(4) 0.003(3) -0.008(3) -0.008(3) C79 0.019(4) 0.019(3) 0.026(4) -0.004(3) 0.009(3) 0.000(3) C80 0.025(4) 0.026(4) 0.024(4) -0.016(3) -0.006(3) -0.001(3) C81 0.026(4) 0.008(3) 0.022(3) 0.001(3) 0.001(3) 0.002(3) C82 0.023(4) 0.014(3) 0.021(3) 0.005(3) -0.005(3) 0.005(3) C83 0.024(4) 0.024(4) 0.026(4) 0.000(3) 0.012(3) 0.011(3) C84 0.031(5) 0.018(4) 0.024(4) -0.004(3) 0.008(3) 0.005(3) C85 0.030(4) 0.022(4) 0.032(4) -0.004(3) 0.013(3) 0.002(3) C86 0.030(4) 0.019(4) 0.030(4) 0.002(3) 0.018(3) 0.000(3) C87 0.037(4) 0.015(3) 0.015(3) 0.005(3) 0.005(3) 0.007(3) C88 0.038(6) 0.035(5) 0.074(8) 0.019(5) -0.017(5) -0.001(4) C89 0.025(4) 0.025(4) 0.040(5) -0.005(3) 0.011(4) -0.010(3) C90 0.033(5) 0.027(4) 0.030(4) 0.004(3) -0.012(4) 0.008(4) C91 0.041(5) 0.015(3) 0.032(4) 0.007(3) -0.009(4) 0.000(3) C92 0.028(4) 0.022(4) 0.028(4) -0.001(3) 0.004(3) -0.004(3) C93 0.014(3) 0.018(3) 0.027(4) -0.007(3) 0.001(3) 0.002(3) C94 0.024(4) 0.026(4) 0.024(4) 0.006(3) -0.007(3) -0.005(3) C95 0.031(4) 0.013(3) 0.018(3) -0.007(3) -0.012(3) 0.004(3) C96 0.021(4) 0.036(4) 0.039(5) 0.012(4) -0.002(3) 0.002(3) C97 0.036(5) 0.010(3) 0.024(4) -0.001(3) 0.007(3) -0.004(3) C98 0.026(4) 0.016(4) 0.028(4) 0.002(3) 0.000(3) -0.006(3) C99 0.042(6) 0.018(4) 0.070(7) -0.018(4) 0.019(5) -0.008(4) C100 0.019(4) 0.026(4) 0.020(4) 0.006(3) 0.000(3) -0.006(3) C101 0.063(7) 0.024(5) 0.073(7) 0.003(4) -0.031(6) -0.004(4) C102 0.016(4) 0.043(5) 0.035(4) -0.003(4) 0.002(3) 0.004(3) C103 0.031(4) 0.040(4) 0.020(4) -0.021(3) 0.002(3) 0.003(4) C104 0.037(5) 0.017(4) 0.036(5) -0.003(3) 0.016(4) -0.002(3) C105 0.024(5) 0.065(6) 0.054(6) -0.052(5) -0.013(4) 0.016(4) C106 0.037(5) 0.060(6) 0.038(5) 0.034(4) 0.005(4) 0.021(5) C107 0.056(6) 0.012(3) 0.025(4) 0.002(3) -0.010(4) -0.003(3) C108 0.035(5) 0.035(4) 0.026(4) 0.010(3) 0.002(3) 0.020(4) C109 0.014(3) 0.021(3) 0.027(4) 0.011(3) 0.001(3) 0.004(3) C110 0.020(4) 0.029(4) 0.027(4) -0.006(3) 0.012(3) -0.007(3) C111 0.025(4) 0.044(5) 0.025(4) 0.013(4) 0.005(3) 0.002(4) C112 0.022(4) 0.027(4) 0.020(4) -0.012(3) 0.004(3) -0.004(3) C113 0.034(4) 0.009(3) 0.024(4) 0.002(3) -0.006(3) -0.005(3) C114 0.021(4) 0.020(3) 0.025(4) 0.005(3) -0.014(3) -0.001(3) C115 0.022(4) 0.032(4) 0.023(4) -0.002(3) -0.009(3) 0.004(3) C116 0.024(4) 0.039(4) 0.017(3) -0.002(3) 0.011(3) 0.004(3) C117 0.046(6) 0.020(4) 0.071(7) -0.017(4) 0.033(5) -0.008(4) C118 0.033(5) 0.053(5) 0.029(4) 0.024(4) -0.001(4) 0.015(4) C119 0.029(5) 0.040(5) 0.028(4) -0.014(4) -0.007(4) 0.003(4) C120 0.027(4) 0.036(4) 0.022(4) -0.011(3) 0.000(3) -0.002(3) C121 0.015(4) 0.035(4) 0.039(5) -0.012(4) 0.008(3) -0.001(3) C122 0.055(7) 0.055(6) 0.038(5) -0.008(4) -0.013(5) 0.003(5) C123 0.040(6) 0.035(5) 0.146(13) 0.011(7) 0.045(7) 0.000(5) C124 0.049(6) 0.022(4) 0.036(5) -0.001(3) -0.021(4) 0.005(4) C125 0.017(4) 0.064(6) 0.057(6) 0.048(5) 0.009(4) 0.006(4) C126 0.050(6) 0.021(4) 0.034(4) -0.002(3) 0.036(4) -0.001(4) C127 0.070(7) 0.024(4) 0.058(6) 0.001(4) 0.025(5) -0.004(4) C130 0.037(6) 0.072(7) 0.049(6) 0.033(5) -0.015(4) -0.019(5) C131 0.036(5) 0.044(5) 0.079(8) 0.032(5) -0.012(5) -0.004(4) C132 0.066(8) 0.020(5) 0.114(10) -0.017(5) 0.022(7) 0.018(5) C133 0.027(4) 0.014(3) 0.031(4) -0.001(3) -0.016(3) -0.003(3) C134 0.040(5) 0.028(4) 0.026(4) -0.010(3) -0.003(3) 0.017(4) C135 0.042(6) 0.023(5) 0.118(10) 0.021(5) -0.018(6) 0.014(4) C136 0.049(5) 0.016(3) 0.031(4) 0.005(3) 0.021(4) -0.001(3) C137 0.025(4) 0.030(4) 0.029(4) -0.006(3) -0.016(3) 0.011(3) C138 0.034(6) 0.098(9) 0.081(8) -0.060(7) -0.030(5) 0.037(6) C140 0.032(5) 0.071(7) 0.053(6) -0.033(5) 0.016(4) -0.022(5) C141 0.015(4) 0.054(5) 0.024(4) 0.006(4) -0.001(3) 0.007(4) C142 0.031(6) 0.044(6) 0.136(12) 0.033(7) -0.015(6) 0.019(5) C143 0.030(5) 0.033(5) 0.071(7) -0.017(5) 0.007(5) -0.011(4) C144 0.080(9) 0.080(9) 0.129(12) 0.082(9) 0.064(9) 0.018(7) C145 0.039(5) 0.052(5) 0.029(4) -0.032(4) -0.003(4) 0.018(4) C146 0.029(5) 0.043(5) 0.065(7) 0.016(5) -0.005(5) -0.006(4) C147 0.086(9) 0.072(8) 0.080(8) 0.053(7) -0.061(7) -0.039(7) C148 0.051(6) 0.019(4) 0.032(4) 0.009(3) -0.032(4) -0.006(4) C150 0.050(6) 0.049(6) 0.054(6) -0.027(5) -0.012(5) -0.007(5) C151 0.030(5) 0.102(9) 0.082(8) 0.066(7) 0.032(5) 0.043(6) C152 0.028(6) 0.039(6) 0.148(12) -0.031(7) 0.022(7) 0.017(5) C153 0.058(7) 0.037(5) 0.036(5) 0.000(4) -0.014(4) -0.009(4) C154 0.049(6) 0.058(6) 0.045(6) 0.025(5) 0.007(5) -0.005(5) C155 0.035(6) 0.058(7) 0.143(12) -0.023(8) -0.054(7) -0.005(5) C156 0.028(5) 0.046(5) 0.034(5) -0.020(4) 0.007(4) 0.005(4) C157 0.078(8) 0.046(6) 0.041(5) 0.016(4) -0.019(5) -0.033(5) C160 0.028(5) 0.048(6) 0.081(8) -0.037(5) 0.006(5) -0.002(4) C161 0.072(8) 0.062(7) 0.050(6) -0.019(5) -0.023(5) 0.050(6) C162 0.066(8) 0.042(6) 0.083(8) -0.011(6) -0.005(6) 0.013(5) C163 0.056(7) 0.060(6) 0.050(6) 0.042(5) -0.025(5) -0.036(5) C164 0.046(6) 0.038(5) 0.037(5) 0.005(4) 0.016(4) -0.006(4) C165 0.052(7) 0.068(7) 0.053(6) -0.041(5) 0.025(5) -0.034(5) C166 0.086(9) 0.066(7) 0.083(8) -0.051(7) 0.066(7) -0.037(6) C170 0.062(8) 0.036(5) 0.089(9) 0.017(5) 0.011(6) 0.009(5) C171 0.070(9) 0.090(9) 0.126(12) -0.092(9) -0.058(8) 0.024(7) C172 0.053(6) 0.021(4) 0.066(6) 0.020(4) -0.035(5) -0.013(4) C180 0.033(6) 0.077(8) 0.066(7) -0.010(6) -0.012(5) -0.018(5) C181 0.046(6) 0.044(5) 0.040(5) 0.008(4) 0.008(4) -0.006(4) C182 0.084(9) 0.047(6) 0.038(5) -0.011(4) 0.016(5) -0.027(6) C183 0.068(7) 0.063(7) 0.048(6) 0.021(5) 0.030(5) 0.048(6) C190 0.044(7) 0.031(5) 0.179(15) -0.018(7) -0.047(8) 0.005(5) C191 0.055(7) 0.033(5) 0.081(8) -0.010(5) -0.025(6) 0.009(5) C192 0.038(6) 0.044(6) 0.153(13) 0.019(7) 0.049(8) -0.003(5) C193 0.034(6) 0.080(8) 0.064(7) 0.007(6) 0.011(5) -0.014(5) C194 0.056(7) 0.030(5) 0.079(8) 0.008(5) 0.022(6) 0.007(5) #----------------------------------------------------------------------------# # 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 N9 1.943(5) . ? Zn1 N8 1.964(5) . ? Zn1 N7 2.086(6) . ? Zn1 N5 2.117(6) . ? Zn1 C32 2.501(6) . ? Zn1 C53 2.506(7) . ? Zn2 N15 1.951(6) . ? Zn2 N6 1.955(6) . ? Zn2 N19 2.094(6) . ? Zn2 N11 2.110(6) . ? Zn2 C66 2.502(7) . ? Zn2 C78 2.518(7) . ? Zn3 N14 1.943(6) . ? Zn3 N13 1.947(6) . ? Zn3 N23 2.102(6) . ? Zn3 N10 2.112(6) . ? Zn3 C60 2.487(7) . ? Zn3 C44 2.504(7) . ? Zn4 N12 1.946(5) . ? Zn4 N17 1.963(5) . ? Zn4 N30 2.088(6) . ? Zn4 N16 2.118(6) . ? Zn4 C45 2.495(6) . ? Zn4 C70 2.501(7) . ? N5 C57 1.304(9) . ? N5 C53 1.379(8) . ? N6 C38 1.348(9) . ? N6 C78 1.385(9) . ? N7 C32 1.343(9) . ? N7 C54 1.385(9) . ? N8 C53 1.360(9) . ? N8 C29 1.402(8) . ? N9 C69 1.364(9) . ? N9 C32 1.395(8) . ? N10 C50 1.343(9) . ? N10 C44 1.368(9) . ? N11 C51 1.355(9) . ? N11 C78 1.382(9) . ? N12 C63 1.360(9) . ? N12 C45 1.388(8) . ? N13 C75 1.365(9) . ? N13 C44 1.382(9) . ? N14 C60 1.371(8) . ? N14 C81 1.416(9) . ? N15 C66 1.374(8) . ? N15 C31 1.390(9) . ? N16 C76 1.293(9) . ? N16 C70 1.373(8) . ? N17 C70 1.351(9) . ? N17 C33 1.398(9) . ? N18 C100 1.330(10) . ? N18 C38 1.355(9) . ? N19 C72 1.338(9) . ? N19 C66 1.372(9) . ? N20 C29 1.341(8) . ? N20 C79 1.380(8) . ? N21 C64 1.328(10) . ? N21 C69 1.335(9) . ? C22 C79 1.393(10) . ? C22 C55 1.398(10) . ? N23 C120 1.325(9) . ? N23 C60 1.357(9) . ? C24 C73 1.402(11) . ? C24 C53 1.411(9) . ? C25 C69 1.387(10) . ? C25 C94 1.395(10) . ? C26 C80 1.350(11) . ? C26 C33 1.404(10) . ? N27 C75 1.333(9) . ? N27 C112 1.334(10) . ? C28 C31 1.376(10) . ? C28 C41 1.401(11) . ? C29 C35 1.407(10) . ? N30 C45 1.347(8) . ? N30 C82 1.376(9) . ? C31 N42 1.358(9) . ? C32 C52 1.396(9) . ? C33 N59 1.353(8) . ? C34 C141 1.397(10) . ? C34 C44 1.416(10) . ? C35 C55 1.345(10) . ? N36 C81 1.329(9) . ? N36 C113 1.338(9) . ? C37 C93 1.393(10) . ? C37 C54 1.395(10) . ? C38 C40 1.418(10) . ? C39 C63 1.392(10) . ? C39 C110 1.399(10) . ? C40 C92 1.349(11) . ? C41 C47 1.346(12) . ? N42 C97 1.336(9) . ? C43 C102 1.357(12) . ? C43 C51 1.405(10) . ? C45 C74 1.403(9) . ? C46 C107 1.408(11) . ? C46 C70 1.408(10) . ? C47 C97 1.400(11) . ? C48 C81 1.381(10) . ? C48 C84 1.400(11) . ? C49 C102 1.395(10) . ? C49 C78 1.401(10) . ? C50 C65 1.396(11) . ? C50 C118 1.511(12) . ? C51 C156 1.508(12) . ? C52 C93 1.377(10) . ? C54 C124 1.519(10) . ? C56 C114 1.400(10) . ? C56 C80 1.403(11) . ? C57 C86 1.387(10) . ? C57 C87 1.525(9) . ? N58 C89 1.320(9) . ? N58 C63 1.338(9) . ? N59 C114 1.370(8) . ? C60 C61 1.407(10) . ? C61 C116 1.362(10) . ? C62 C98 1.361(10) . ? C62 C75 1.433(10) . ? C64 C96 1.377(12) . ? C64 C88 1.532(12) . ? C65 C141 1.367(12) . ? C66 C68 1.384(10) . ? C67 C109 1.377(10) . ? C67 C82 1.403(9) . ? C68 C115 1.359(10) . ? C71 C84 1.359(11) . ? C71 C113 1.405(10) . ? C72 C77 1.360(11) . ? C72 C125 1.576(11) . ? C73 C86 1.383(10) . ? C74 C109 1.392(10) . ? C76 C133 1.392(10) . ? C76 C95 1.521(9) . ? C77 C115 1.435(11) . ? C79 C126 1.526(10) . ? C82 C136 1.524(10) . ? C83 C87 1.544(9) . ? C85 C152 1.494(11) . ? C85 C192 1.504(13) . ? C85 C193 1.516(14) . ? C85 C97 1.518(11) . ? C87 C117 1.512(11) . ? C87 C108 1.557(10) . ? C88 C131 1.391(13) . ? C88 C146 1.534(14) . ? C88 C170 1.671(16) . ? C89 C121 1.382(11) . ? C89 C99 1.552(11) . ? C90 C155 1.490(14) . ? C90 C113 1.492(11) . ? C90 C180 1.511(14) . ? C90 C142 1.513(11) . ? C91 C100 1.383(11) . ? C91 C92 1.401(12) . ? C94 C96 1.390(11) . ? C95 C172 1.514(11) . ? C95 C137 1.535(9) . ? C95 C134 1.564(10) . ? C98 C104 1.416(11) . ? C99 C160 1.413(13) . ? C99 C143 1.496(13) . ? C99 C162 1.698(16) . ? C100 C119 1.590(11) . ? C101 C148 1.477(12) . ? C103 C120 1.358(11) . ? C103 C116 1.425(11) . ? C104 C112 1.371(12) . ? C105 C171 1.484(15) . ? C105 C140 1.560(15) . ? C105 C122 1.568(12) . ? C105 C120 1.572(12) . ? C106 C118 1.499(10) . ? C107 C133 1.373(10) . ? C110 C121 1.397(11) . ? C111 C194 1.527(14) . ? C111 C123 1.546(13) . ? C111 C112 1.558(11) . ? C111 C154 1.566(12) . ? C114 C148 1.521(10) . ? C118 C163 1.533(14) . ? C118 C151 1.563(12) . ? C119 C190 1.507(13) . ? C119 C191 1.523(14) . ? C119 C150 1.555(13) . ? C124 C153 1.495(12) . ? C124 C147 1.503(14) . ? C124 C161 1.537(13) . ? C125 C144 1.499(15) . ? C125 C130 1.546(15) . ? C125 C181 1.578(12) . ? C126 C127 1.489(12) . ? C126 C132 1.550(13) . ? C126 C182 1.604(14) . ? C135 C148 1.516(13) . ? C136 C166 1.496(13) . ? C136 C164 1.498(11) . ? C136 C183 1.512(13) . ? C138 C156 1.570(12) . ? C145 C156 1.493(10) . ? C148 C157 1.607(14) . ? C156 C165 1.524(14) . ? 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 N9 Zn1 N8 144.9(2) . . ? N9 Zn1 N7 66.2(2) . . ? N8 Zn1 N7 131.8(2) . . ? N9 Zn1 N5 129.9(2) . . ? N8 Zn1 N5 66.0(2) . . ? N7 Zn1 N5 131.2(2) . . ? N9 Zn1 C32 33.7(2) . . ? N8 Zn1 C32 152.3(2) . . ? N7 Zn1 C32 32.5(2) . . ? N5 Zn1 C32 140.8(2) . . ? N9 Zn1 C53 149.6(2) . . ? N8 Zn1 C53 32.7(2) . . ? N7 Zn1 C53 143.3(2) . . ? N5 Zn1 C53 33.4(2) . . ? C32 Zn1 C53 172.9(2) . . ? N15 Zn2 N6 144.9(2) . . ? N15 Zn2 N19 66.3(2) . . ? N6 Zn2 N19 130.9(2) . . ? N15 Zn2 N11 130.2(2) . . ? N6 Zn2 N11 66.4(2) . . ? N19 Zn2 N11 131.2(2) . . ? N15 Zn2 C66 33.1(2) . . ? N6 Zn2 C66 151.3(2) . . ? N19 Zn2 C66 33.3(2) . . ? N11 Zn2 C66 141.5(2) . . ? N15 Zn2 C78 150.7(2) . . ? N6 Zn2 C78 33.1(2) . . ? N19 Zn2 C78 142.0(2) . . ? N11 Zn2 C78 33.3(2) . . ? C66 Zn2 C78 172.9(2) . . ? N14 Zn3 N13 145.0(2) . . ? N14 Zn3 N23 66.3(2) . . ? N13 Zn3 N23 130.8(2) . . ? N14 Zn3 N10 130.1(2) . . ? N13 Zn3 N10 66.4(2) . . ? N23 Zn3 N10 131.3(2) . . ? N14 Zn3 C60 33.3(2) . . ? N13 Zn3 C60 151.3(2) . . ? N23 Zn3 C60 33.1(2) . . ? N10 Zn3 C60 141.5(2) . . ? N14 Zn3 C44 150.9(2) . . ? N13 Zn3 C44 33.3(2) . . ? N23 Zn3 C44 141.7(2) . . ? N10 Zn3 C44 33.1(2) . . ? C60 Zn3 C44 172.4(2) . . ? N12 Zn4 N17 144.5(2) . . ? N12 Zn4 N30 66.3(2) . . ? N17 Zn4 N30 131.9(2) . . ? N12 Zn4 N16 130.4(2) . . ? N17 Zn4 N16 65.8(2) . . ? N30 Zn4 N16 131.1(2) . . ? N12 Zn4 C45 33.6(2) . . ? N17 Zn4 C45 152.4(2) . . ? N30 Zn4 C45 32.7(2) . . ? N16 Zn4 C45 141.0(2) . . ? N12 Zn4 C70 149.8(2) . . ? N17 Zn4 C70 32.5(2) . . ? N30 Zn4 C70 143.0(2) . . ? N16 Zn4 C70 33.3(2) . . ? C45 Zn4 C70 172.9(2) . . ? C57 N5 C53 122.7(6) . . ? C57 N5 Zn1 148.1(5) . . ? C53 N5 Zn1 89.0(4) . . ? C38 N6 C78 126.5(6) . . ? C38 N6 Zn2 136.1(5) . . ? C78 N6 Zn2 96.4(4) . . ? C32 N7 C54 120.3(6) . . ? C32 N7 Zn1 91.0(4) . . ? C54 N7 Zn1 148.6(5) . . ? C53 N8 C29 126.3(6) . . ? C53 N8 Zn1 96.2(4) . . ? C29 N8 Zn1 134.8(4) . . ? C69 N9 C32 127.3(6) . . ? C69 N9 Zn1 136.9(5) . . ? C32 N9 Zn1 95.6(4) . . ? C50 N10 C44 121.8(6) . . ? C50 N10 Zn3 148.8(5) . . ? C44 N10 Zn3 89.4(4) . . ? C51 N11 C78 122.0(6) . . ? C51 N11 Zn2 148.2(5) . . ? C78 N11 Zn2 89.8(4) . . ? C63 N12 C45 127.4(6) . . ? C63 N12 Zn4 137.1(5) . . ? C45 N12 Zn4 95.4(4) . . ? C75 N13 C44 125.9(6) . . ? C75 N13 Zn3 136.9(5) . . ? C44 N13 Zn3 96.1(4) . . ? C60 N14 C81 126.5(6) . . ? C60 N14 Zn3 95.7(4) . . ? C81 N14 Zn3 137.0(5) . . ? C66 N15 C31 126.9(6) . . ? C66 N15 Zn2 96.1(4) . . ? C31 N15 Zn2 136.0(5) . . ? C76 N16 C70 123.4(6) . . ? C76 N16 Zn4 147.6(5) . . ? C70 N16 Zn4 88.8(4) . . ? C70 N17 C33 126.4(6) . . ? C70 N17 Zn4 96.2(4) . . ? C33 N17 Zn4 134.8(5) . . ? C100 N18 C38 119.6(6) . . ? C72 N19 C66 120.2(6) . . ? C72 N19 Zn2 149.7(5) . . ? C66 N19 Zn2 89.9(4) . . ? C29 N20 C79 116.9(5) . . ? C64 N21 C69 122.2(6) . . ? C79 C22 C55 119.6(6) . . ? C120 N23 C60 121.1(6) . . ? C120 N23 Zn3 149.4(5) . . ? C60 N23 Zn3 89.2(4) . . ? C73 C24 C53 115.7(6) . . ? C69 C25 C94 119.8(7) . . ? C80 C26 C33 118.0(7) . . ? C75 N27 C112 120.0(6) . . ? C31 C28 C41 117.0(7) . . ? N20 C29 N8 117.1(6) . . ? N20 C29 C35 124.6(6) . . ? N8 C29 C35 118.4(6) . . ? C45 N30 C82 120.9(6) . . ? C45 N30 Zn4 90.5(4) . . ? C82 N30 Zn4 148.6(4) . . ? N42 C31 C28 122.8(6) . . ? N42 C31 N15 118.8(6) . . ? C28 C31 N15 118.3(7) . . ? N7 C32 N9 107.1(5) . . ? N7 C32 C52 121.6(7) . . ? N9 C32 C52 131.1(6) . . ? N7 C32 Zn1 56.5(3) . . ? N9 C32 Zn1 50.6(3) . . ? C52 C32 Zn1 176.4(5) . . ? N59 C33 N17 117.5(6) . . ? N59 C33 C26 124.3(6) . . ? N17 C33 C26 118.3(6) . . ? C141 C34 C44 115.0(7) . . ? C55 C35 C29 117.6(6) . . ? C81 N36 C113 118.7(6) . . ? C93 C37 C54 118.9(7) . . ? N6 C38 N18 120.7(6) . . ? N6 C38 C40 119.6(6) . . ? N18 C38 C40 119.7(6) . . ? C63 C39 C110 119.8(7) . . ? C92 C40 C38 121.0(7) . . ? C47 C41 C28 121.3(7) . . ? C97 N42 C31 118.2(6) . . ? C102 C43 C51 119.1(7) . . ? N10 C44 N13 108.1(6) . . ? N10 C44 C34 121.1(6) . . ? N13 C44 C34 130.7(6) . . ? N10 C44 Zn3 57.5(3) . . ? N13 C44 Zn3 50.6(3) . . ? C34 C44 Zn3 178.0(5) . . ? N30 C45 N12 107.8(5) . . ? N30 C45 C74 121.4(6) . . ? N12 C45 C74 130.7(6) . . ? N30 C45 Zn4 56.8(3) . . ? N12 C45 Zn4 50.9(3) . . ? C74 C45 Zn4 176.5(5) . . ? C107 C46 C70 115.6(6) . . ? C41 C47 C97 118.2(7) . . ? C81 C48 C84 116.1(7) . . ? C102 C49 C78 115.7(7) . . ? N10 C50 C65 119.8(7) . . ? N10 C50 C118 117.2(7) . . ? C65 C50 C118 122.8(7) . . ? N11 C51 C43 118.6(7) . . ? N11 C51 C156 117.9(6) . . ? C43 C51 C156 123.3(7) . . ? C93 C52 C32 118.4(7) . . ? N8 C53 N5 108.7(5) . . ? N8 C53 C24 130.5(6) . . ? N5 C53 C24 120.5(6) . . ? N8 C53 Zn1 51.2(3) . . ? N5 C53 Zn1 57.6(3) . . ? C24 C53 Zn1 177.2(5) . . ? N7 C54 C37 119.8(6) . . ? N7 C54 C124 117.3(6) . . ? C37 C54 C124 122.9(7) . . ? C35 C55 C22 120.3(7) . . ? C114 C56 C80 119.4(7) . . ? N5 C57 C86 119.4(6) . . ? N5 C57 C87 116.9(6) . . ? C86 C57 C87 123.6(6) . . ? C89 N58 C63 121.7(6) . . ? C33 N59 C114 116.9(6) . . ? N23 C60 N14 108.7(6) . . ? N23 C60 C61 120.1(6) . . ? N14 C60 C61 131.1(7) . . ? N23 C60 Zn3 57.7(3) . . ? N14 C60 Zn3 51.0(3) . . ? C61 C60 Zn3 176.1(5) . . ? C116 C61 C60 118.8(7) . . ? C98 C62 C75 119.4(7) . . ? N58 C63 N12 122.6(7) . . ? N58 C63 C39 119.3(6) . . ? N12 C63 C39 118.0(6) . . ? N21 C64 C96 121.9(7) . . ? N21 C64 C88 117.3(7) . . ? C96 C64 C88 120.3(8) . . ? C141 C65 C50 118.5(7) . . ? N19 C66 N15 107.7(6) . . ? N19 C66 C68 120.1(6) . . ? N15 C66 C68 132.2(7) . . ? N19 C66 Zn2 56.8(3) . . ? N15 C66 Zn2 50.8(3) . . ? C68 C66 Zn2 175.8(5) . . ? C109 C67 C82 117.8(7) . . ? C115 C68 C66 119.9(7) . . ? N21 C69 N9 122.9(7) . . ? N21 C69 C25 118.8(6) . . ? N9 C69 C25 118.3(6) . . ? N17 C70 N16 109.1(6) . . ? N17 C70 C46 130.7(6) . . ? N16 C70 C46 120.0(6) . . ? N17 C70 Zn4 51.3(3) . . ? N16 C70 Zn4 57.9(3) . . ? C46 C70 Zn4 177.2(5) . . ? C84 C71 C113 118.5(6) . . ? N19 C72 C77 122.3(7) . . ? N19 C72 C125 113.5(7) . . ? C77 C72 C125 124.0(7) . . ? C86 C73 C24 121.2(6) . . ? C109 C74 C45 117.1(7) . . ? N27 C75 N13 121.9(6) . . ? N27 C75 C62 120.5(6) . . ? N13 C75 C62 117.6(6) . . ? N16 C76 C133 119.7(6) . . ? N16 C76 C95 117.8(6) . . ? C133 C76 C95 122.4(7) . . ? C72 C77 C115 117.9(7) . . ? N11 C78 N6 107.4(6) . . ? N11 C78 C49 120.7(6) . . ? N6 C78 C49 131.8(6) . . ? N11 C78 Zn2 56.9(3) . . ? N6 C78 Zn2 50.5(3) . . ? C49 C78 Zn2 176.9(5) . . ? N20 C79 C22 120.8(6) . . ? N20 C79 C126 114.0(6) . . ? C22 C79 C126 125.2(6) . . ? C26 C80 C56 120.0(7) . . ? N36 C81 C48 124.4(7) . . ? N36 C81 N14 119.8(6) . . ? C48 C81 N14 115.8(7) . . ? N30 C82 C67 120.2(6) . . ? N30 C82 C136 117.5(6) . . ? C67 C82 C136 122.1(7) . . ? C71 C84 C48 120.9(7) . . ? C152 C85 C192 107.1(9) . . ? C152 C85 C193 114.8(9) . . ? C192 C85 C193 103.8(9) . . ? C152 C85 C97 109.5(7) . . ? C192 C85 C97 113.7(8) . . ? C193 C85 C97 108.1(7) . . ? C73 C86 C57 120.1(7) . . ? C117 C87 C57 112.4(7) . . ? C117 C87 C83 109.2(6) . . ? C57 C87 C83 111.4(5) . . ? C117 C87 C108 109.7(7) . . ? C57 C87 C108 105.6(6) . . ? C83 C87 C108 108.5(7) . . ? C131 C88 C64 118.3(9) . . ? C131 C88 C146 112.3(9) . . ? C64 C88 C146 110.2(8) . . ? C131 C88 C170 104.4(9) . . ? C64 C88 C170 104.7(8) . . ? C146 C88 C170 105.8(9) . . ? N58 C89 C121 122.3(7) . . ? N58 C89 C99 116.6(7) . . ? C121 C89 C99 120.5(7) . . ? C155 C90 C113 115.5(8) . . ? C155 C90 C180 102.2(9) . . ? C113 C90 C180 108.8(7) . . ? C155 C90 C142 107.8(9) . . ? C113 C90 C142 108.6(7) . . ? C180 C90 C142 114.0(9) . . ? C100 C91 C92 119.8(7) . . ? C40 C92 C91 117.8(8) . . ? C52 C93 C37 120.9(7) . . ? C96 C94 C25 119.6(7) . . ? C172 C95 C76 112.3(7) . . ? C172 C95 C137 109.4(6) . . ? C76 C95 C137 112.1(5) . . ? C172 C95 C134 109.2(7) . . ? C76 C95 C134 105.7(6) . . ? C137 C95 C134 107.9(6) . . ? C64 C96 C94 117.3(7) . . ? N42 C97 C47 122.3(7) . . ? N42 C97 C85 115.5(7) . . ? C47 C97 C85 122.1(7) . . ? C62 C98 C104 118.4(8) . . ? C160 C99 C143 114.2(8) . . ? C160 C99 C89 116.3(8) . . ? C143 C99 C89 111.1(8) . . ? C160 C99 C162 103.5(9) . . ? C143 C99 C162 107.2(8) . . ? C89 C99 C162 103.2(7) . . ? N18 C100 C91 122.0(7) . . ? N18 C100 C119 114.9(6) . . ? C91 C100 C119 123.0(7) . . ? C43 C102 C49 123.8(7) . . ? C120 C103 C116 118.5(6) . . ? C112 C104 C98 118.9(7) . . ? C171 C105 C140 113.9(11) . . ? C171 C105 C122 109.1(8) . . ? C140 C105 C122 105.8(8) . . ? C171 C105 C120 111.4(9) . . ? C140 C105 C120 107.3(7) . . ? C122 C105 C120 109.1(7) . . ? C133 C107 C46 121.8(7) . . ? C67 C109 C74 122.6(7) . . ? C121 C110 C39 118.8(7) . . ? C194 C111 C123 108.9(8) . . ? C194 C111 C112 107.2(8) . . ? C123 C111 C112 109.7(7) . . ? C194 C111 C154 108.1(8) . . ? C123 C111 C154 111.2(9) . . ? C112 C111 C154 111.6(7) . . ? N27 C112 C104 122.6(7) . . ? N27 C112 C111 114.6(6) . . ? C104 C112 C111 122.7(7) . . ? N36 C113 C71 121.4(7) . . ? N36 C113 C90 116.1(7) . . ? C71 C113 C90 122.4(7) . . ? N59 C114 C56 121.3(6) . . ? N59 C114 C148 113.9(6) . . ? C56 C114 C148 124.8(6) . . ? C68 C115 C77 119.5(7) . . ? C61 C116 C103 119.6(7) . . ? C106 C118 C50 111.7(8) . . ? C106 C118 C163 110.7(8) . . ? C50 C118 C163 107.0(7) . . ? C106 C118 C151 108.7(7) . . ? C50 C118 C151 110.7(7) . . ? C163 C118 C151 107.9(9) . . ? C190 C119 C191 107.7(9) . . ? C190 C119 C150 114.7(10) . . ? C191 C119 C150 107.0(8) . . ? C190 C119 C100 110.0(7) . . ? C191 C119 C100 105.6(8) . . ? C150 C119 C100 111.3(7) . . ? N23 C120 C103 121.9(7) . . ? N23 C120 C105 113.9(6) . . ? C103 C120 C105 124.1(7) . . ? C89 C121 C110 117.7(7) . . ? C153 C124 C147 112.7(8) . . ? C153 C124 C54 112.0(7) . . ? C147 C124 C54 110.7(8) . . ? C153 C124 C161 108.3(8) . . ? C147 C124 C161 106.3(9) . . ? C54 C124 C161 106.4(7) . . ? C144 C125 C130 114.4(10) . . ? C144 C125 C72 110.2(8) . . ? C130 C125 C72 107.2(7) . . ? C144 C125 C181 108.5(8) . . ? C130 C125 C181 107.1(8) . . ? C72 C125 C181 109.3(7) . . ? C127 C126 C79 115.3(6) . . ? C127 C126 C132 117.7(9) . . ? C79 C126 C132 109.3(7) . . ? C127 C126 C182 106.3(8) . . ? C79 C126 C182 104.5(7) . . ? C132 C126 C182 101.9(8) . . ? C107 C133 C76 119.3(7) . . ? C166 C136 C164 111.7(8) . . ? C166 C136 C183 106.3(9) . . ? C164 C136 C183 109.8(8) . . ? C166 C136 C82 109.9(8) . . ? C164 C136 C82 111.5(6) . . ? C183 C136 C82 107.4(7) . . ? C65 C141 C34 123.7(7) . . ? C101 C148 C135 116.2(9) . . ? C101 C148 C114 114.8(6) . . ? C135 C148 C114 110.9(7) . . ? C101 C148 C157 106.5(8) . . ? C135 C148 C157 101.8(8) . . ? C114 C148 C157 105.1(7) . . ? C145 C156 C51 113.0(7) . . ? C145 C156 C165 111.0(8) . . ? C51 C156 C165 106.2(7) . . ? C145 C156 C138 108.6(7) . . ? C51 C156 C138 109.4(7) . . ? C165 C156 C138 108.5(9) . . ? # Attachment 'complex6.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-10-30 at 14:18:22 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\progs\wingx\files\archive.dat # CIF files read : job struct data_job1 _database_code_depnum_ccdc_archive 'CCDC 682253' _audit_creation_date 2006-10-30T14:18:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H58 N6 Zn2' _chemical_formula_sum 'C40 H58 N6 Zn2' _chemical_formula_weight 753.66 _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 25.7160(19) _cell_length_b 9.9469(12) _cell_length_c 15.7295(14) _cell_angle_alpha 90 _cell_angle_beta 96.67 _cell_angle_gamma 90 _cell_volume 3996.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5253 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.39 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.235 _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 0.574 _exptl_absorpt_correction_T_max 0.884 #----------------------------------------------------------------------------# # 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 0.0534 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_number 18459 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4595 _reflns_number_gt 3779 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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)' #----------------------------------------------------------------------------# # 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^)+(0.0604P)^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 4595 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.398 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # 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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.531629(8) 0.16222(2) 0.336168(12) 0.01333(9) Uani 1 d . . . C1 C 0.58012(8) 0.2552(2) 0.42304(13) 0.0241(4) Uani 1 d . . . H1A H 0.5816 0.3515 0.4075 0.029 Uiso 1 calc R . . H1B H 0.5661 0.2494 0.4789 0.029 Uiso 1 calc R . . C2 C 0.63562(9) 0.1985(3) 0.43285(14) 0.0315(5) Uani 1 d . . . H2A H 0.6574 0.2488 0.4772 0.047 Uiso 1 calc R . . H2B H 0.6504 0.2066 0.3784 0.047 Uiso 1 calc R . . H2C H 0.6347 0.1035 0.4493 0.047 Uiso 1 calc R . . N10 N 0.54739(6) 0.16859(14) 0.19658(9) 0.0124(3) Uani 1 d . . . N11 N 0.62951(6) 0.26317(16) 0.18015(9) 0.0154(3) Uani 1 d . . . C11 C 0.57740(7) 0.27474(18) 0.16890(10) 0.0134(4) Uani 1 d . . . C12 C 0.55251(8) 0.3907(2) 0.13427(11) 0.0176(4) Uani 1 d . . . H12 H 0.5154 0.3981 0.1276 0.021 Uiso 1 calc R . . C13 C 0.58324(8) 0.4935(2) 0.11023(12) 0.0205(4) Uani 1 d . . . H13 H 0.5674 0.5735 0.0866 0.025 Uiso 1 calc R . . C14 C 0.63739(8) 0.4811(2) 0.12037(12) 0.0200(4) Uani 1 d . . . H14 H 0.6589 0.5514 0.1033 0.024 Uiso 1 calc R . . C15 C 0.65920(8) 0.3645(2) 0.15578(12) 0.0181(4) Uani 1 d . . . C16 C 0.71794(9) 0.3400(2) 0.17228(15) 0.0252(5) Uani 1 d . . . C17 C 0.73118(9) 0.2069(3) 0.13284(19) 0.0401(6) Uani 1 d . . . H17A H 0.711 0.1348 0.1559 0.06 Uiso 1 calc R . . H17B H 0.7687 0.1886 0.1466 0.06 Uiso 1 calc R . . H17C H 0.7225 0.2113 0.0706 0.06 Uiso 1 calc R . . C18 C 0.74985(9) 0.4506(3) 0.13589(18) 0.0399(6) Uani 1 d . . . H18A H 0.7416 0.5372 0.1608 0.06 Uiso 1 calc R . . H18B H 0.7412 0.4542 0.0736 0.06 Uiso 1 calc R . . H18C H 0.7873 0.4315 0.1498 0.06 Uiso 1 calc R . . C19 C 0.73276(10) 0.3336(3) 0.27034(17) 0.0476(8) Uani 1 d . . . H19A H 0.7248 0.42 0.2959 0.071 Uiso 1 calc R . . H19B H 0.7702 0.3146 0.283 0.071 Uiso 1 calc R . . H19C H 0.7126 0.2622 0.2943 0.071 Uiso 1 calc R . . N20 N 0.56107(6) -0.01563(15) 0.28250(9) 0.0117(3) Uani 1 d . . . C21 C 0.57176(7) 0.04364(19) 0.20907(10) 0.0123(4) Uani 1 d . . . C22 C 0.60166(7) -0.02000(19) 0.15225(11) 0.0137(4) Uani 1 d . . . H22 H 0.61 0.0243 0.1021 0.016 Uiso 1 calc R . . C23 C 0.61862(8) -0.14840(19) 0.17117(11) 0.0155(4) Uani 1 d . . . H23 H 0.6384 -0.1952 0.1332 0.019 Uiso 1 calc R . . C24 C 0.60692(7) -0.2101(2) 0.24597(11) 0.0160(4) Uani 1 d . . . H24 H 0.6185 -0.2993 0.2589 0.019 Uiso 1 calc R . . C25 C 0.57821(7) -0.14085(19) 0.30189(11) 0.0137(4) Uani 1 d . . . C26 C 0.56736(7) -0.2046(2) 0.38652(11) 0.0146(4) Uani 1 d . . . C27 C 0.53801(9) -0.3369(2) 0.36829(14) 0.0257(5) Uani 1 d . . . H27A H 0.5312 -0.3783 0.4224 0.039 Uiso 1 calc R . . H27B H 0.5593 -0.3978 0.3377 0.039 Uiso 1 calc R . . H27C H 0.5047 -0.3193 0.3331 0.039 Uiso 1 calc R . . C28 C 0.62006(8) -0.2313(2) 0.44048(11) 0.0221(4) Uani 1 d . . . H28A H 0.6139 -0.2725 0.495 0.033 Uiso 1 calc R . . H28B H 0.6388 -0.1461 0.4515 0.033 Uiso 1 calc R . . H28C H 0.6411 -0.2921 0.4094 0.033 Uiso 1 calc R . . C29 C 0.53446(8) -0.1144(2) 0.43777(12) 0.0204(4) Uani 1 d . . . H29A H 0.5287 -0.1594 0.4913 0.031 Uiso 1 calc R . . H29B H 0.5007 -0.0964 0.4041 0.031 Uiso 1 calc R . . H29C H 0.5529 -0.0293 0.4508 0.031 Uiso 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 0.01278(14) 0.01447(14) 0.01297(13) -0.00245(7) 0.00254(9) -0.00034(9) C1 0.0222(11) 0.0235(11) 0.0260(10) -0.0081(8) -0.0002(8) -0.0026(9) C2 0.0228(12) 0.0442(14) 0.0264(11) -0.0023(10) -0.0016(9) -0.0055(11) N10 0.0129(8) 0.0109(8) 0.0137(7) 0.0019(5) 0.0035(6) 0.0004(6) N11 0.0150(8) 0.0163(9) 0.0151(7) -0.0007(6) 0.0029(6) -0.0012(7) C11 0.0160(9) 0.0120(9) 0.0126(8) -0.0031(7) 0.0039(6) -0.0016(8) C12 0.0175(10) 0.0155(10) 0.0206(9) 0.0015(7) 0.0052(7) 0.0022(8) C13 0.0260(11) 0.0135(10) 0.0233(9) 0.0040(7) 0.0078(8) 0.0029(9) C14 0.0234(11) 0.0139(10) 0.0243(9) -0.0001(7) 0.0103(8) -0.0052(8) C15 0.0179(10) 0.0197(10) 0.0178(9) -0.0024(7) 0.0063(7) -0.0021(8) C16 0.0175(11) 0.0251(12) 0.0335(11) 0.0014(9) 0.0051(9) -0.0058(9) C17 0.0190(12) 0.0297(13) 0.0731(18) -0.0010(13) 0.0115(12) 0.0007(11) C18 0.0218(12) 0.0321(14) 0.0683(17) 0.0041(12) 0.0155(11) -0.0073(11) C19 0.0239(13) 0.077(2) 0.0393(14) 0.0062(13) -0.0068(11) -0.0130(13) N20 0.0105(7) 0.0129(8) 0.0115(6) -0.0004(5) 0.0005(5) -0.0011(6) C21 0.0094(8) 0.0133(9) 0.0137(8) -0.0002(6) -0.0009(6) -0.0010(7) C22 0.0129(9) 0.0167(10) 0.0118(7) -0.0006(7) 0.0025(6) -0.0007(8) C23 0.0133(9) 0.0184(10) 0.0150(8) -0.0032(7) 0.0026(7) 0.0015(8) C24 0.0159(9) 0.0132(9) 0.0184(8) -0.0001(7) -0.0001(7) 0.0036(8) C25 0.0113(9) 0.0170(10) 0.0121(8) 0.0005(7) -0.0014(7) -0.0020(8) C26 0.0145(9) 0.0160(9) 0.0130(8) 0.0042(7) 0.0010(7) 0.0015(8) C27 0.0342(13) 0.0203(12) 0.0231(10) 0.0053(8) 0.0059(9) -0.0064(9) C28 0.0183(10) 0.0310(12) 0.0170(9) 0.0077(8) 0.0019(8) 0.0070(9) C29 0.0219(10) 0.0246(11) 0.0162(8) 0.0070(8) 0.0086(7) 0.0046(9) #----------------------------------------------------------------------------# # 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 1.9703(19) . ? Zn1 N10 2.0386(16) 2_655 ? Zn1 N20 2.1363(15) . ? Zn1 N10 2.2794(15) . ? Zn1 Zn1 2.9951(4) 2_655 ? C1 C2 1.526(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? N10 C21 1.396(2) . ? N10 C11 1.406(2) . ? N10 Zn1 2.0386(16) 2_655 ? N11 C11 1.336(2) . ? N11 C15 1.347(2) . ? C11 C12 1.399(3) . ? C12 C13 1.372(3) . ? C12 H12 0.95 . ? C13 C14 1.389(3) . ? C13 H13 0.95 . ? C14 C15 1.377(3) . ? C14 H14 0.95 . ? C15 C16 1.522(3) . ? C16 C17 1.518(3) . ? C16 C18 1.523(3) . ? C16 C19 1.547(3) . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? N20 C25 1.345(2) . ? N20 C21 1.353(2) . ? C21 C22 1.396(2) . ? C22 C23 1.371(3) . ? C22 H22 0.95 . ? C23 C24 1.391(3) . ? C23 H23 0.95 . ? C24 C25 1.394(3) . ? C24 H24 0.95 . ? C25 C26 1.529(2) . ? C26 C29 1.527(3) . ? C26 C27 1.527(3) . ? C26 C28 1.536(2) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 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 N10 133.85(8) . 2_655 ? C1 Zn1 N20 115.98(7) . . ? N10 Zn1 N20 108.33(6) 2_655 . ? C1 Zn1 N10 119.08(8) . . ? N10 Zn1 N10 92.25(6) 2_655 . ? N20 Zn1 N10 62.07(5) . . ? C1 Zn1 Zn1 149.46(7) . 2_655 ? N10 Zn1 Zn1 49.50(4) 2_655 2_655 ? N20 Zn1 Zn1 79.78(4) . 2_655 ? N10 Zn1 Zn1 42.85(4) . 2_655 ? C2 C1 Zn1 113.94(15) . . ? C2 C1 H1A 108.8 . . ? Zn1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? Zn1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C21 N10 C11 117.30(15) . . ? C21 N10 Zn1 115.22(11) . 2_655 ? C11 N10 Zn1 120.78(12) . 2_655 ? C21 N10 Zn1 88.10(10) . . ? C11 N10 Zn1 118.97(11) . . ? Zn1 N10 Zn1 87.65(6) 2_655 . ? C11 N11 C15 119.40(17) . . ? N11 C11 C12 121.96(17) . . ? N11 C11 N10 118.18(16) . . ? C12 C11 N10 119.80(17) . . ? C13 C12 C11 118.02(18) . . ? C13 C12 H12 121 . . ? C11 C12 H12 121 . . ? C12 C13 C14 120.25(19) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 118.52(18) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? N11 C15 C14 121.84(18) . . ? N11 C15 C16 114.57(17) . . ? C14 C15 C16 123.58(18) . . ? C17 C16 C15 109.60(18) . . ? C17 C16 C18 108.7(2) . . ? C15 C16 C18 112.80(18) . . ? C17 C16 C19 109.3(2) . . ? C15 C16 C19 107.54(19) . . ? C18 C16 C19 108.9(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 N20 C21 120.23(15) . . ? C25 N20 Zn1 143.07(12) . . ? C21 N20 Zn1 95.34(11) . . ? N20 C21 N10 112.07(15) . . ? N20 C21 C22 122.03(17) . . ? N10 C21 C22 125.82(16) . . ? C23 C22 C21 117.92(16) . . ? C23 C22 H22 121 . . ? C21 C22 H22 121 . . ? C22 C23 C24 120.02(17) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C23 C24 C25 119.85(18) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N20 C25 C24 119.90(17) . . ? N20 C25 C26 119.59(16) . . ? C24 C25 C26 120.49(17) . . ? C29 C26 C27 108.27(17) . . ? C29 C26 C25 112.57(16) . . ? C27 C26 C25 109.27(15) . . ? C29 C26 C28 108.49(15) . . ? C27 C26 C28 109.90(17) . . ? C25 C26 C28 108.31(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 N10 Zn1 C1 C2 170.04(13) 2_655 . . . ? N20 Zn1 C1 C2 7.67(19) . . . . ? N10 Zn1 C1 C2 -63.34(18) . . . . ? Zn1 Zn1 C1 C2 -108.25(17) 2_655 . . . ? C1 Zn1 N10 C21 96.50(12) . . . . ? N10 Zn1 N10 C21 -118.91(9) 2_655 . . . ? N20 Zn1 N10 C21 -9.31(9) . . . . ? Zn1 Zn1 N10 C21 -115.34(11) 2_655 . . . ? C1 Zn1 N10 C11 -23.91(16) . . . . ? N10 Zn1 N10 C11 120.69(12) 2_655 . . . ? N20 Zn1 N10 C11 -129.72(14) . . . . ? Zn1 Zn1 N10 C11 124.25(15) 2_655 . . . ? C1 Zn1 N10 Zn1 -148.16(8) . . . 2_655 ? N10 Zn1 N10 Zn1 -3.56(8) 2_655 . . 2_655 ? N20 Zn1 N10 Zn1 106.03(7) . . . 2_655 ? C15 N11 C11 C12 -1.5(3) . . . . ? C15 N11 C11 N10 -178.68(15) . . . . ? C21 N10 C11 N11 -19.3(2) . . . . ? Zn1 N10 C11 N11 -169.29(12) 2_655 . . . ? Zn1 N10 C11 N11 84.72(17) . . . . ? C21 N10 C11 C12 163.45(16) . . . . ? Zn1 N10 C11 C12 13.5(2) 2_655 . . . ? Zn1 N10 C11 C12 -92.49(17) . . . . ? N11 C11 C12 C13 1.1(3) . . . . ? N10 C11 C12 C13 178.21(16) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C13 C14 C15 -0.7(3) . . . . ? C11 N11 C15 C14 0.8(3) . . . . ? C11 N11 C15 C16 179.67(16) . . . . ? C13 C14 C15 N11 0.3(3) . . . . ? C13 C14 C15 C16 -178.44(18) . . . . ? N11 C15 C16 C17 53.1(2) . . . . ? C14 C15 C16 C17 -128.1(2) . . . . ? N11 C15 C16 C18 174.32(18) . . . . ? C14 C15 C16 C18 -6.8(3) . . . . ? N11 C15 C16 C19 -65.6(2) . . . . ? C14 C15 C16 C19 113.2(2) . . . . ? C1 Zn1 N20 C25 64.0(2) . . . . ? N10 Zn1 N20 C25 -102.7(2) 2_655 . . . ? N10 Zn1 N20 C25 174.7(2) . . . . ? Zn1 Zn1 N20 C25 -143.7(2) 2_655 . . . ? C1 Zn1 N20 C21 -101.06(12) . . . . ? N10 Zn1 N20 C21 92.24(11) 2_655 . . . ? N10 Zn1 N20 C21 9.64(9) . . . . ? Zn1 Zn1 N20 C21 51.26(9) 2_655 . . . ? C25 N20 C21 N10 175.23(15) . . . . ? Zn1 N20 C21 N10 -15.12(15) . . . . ? C25 N20 C21 C22 -1.6(3) . . . . ? Zn1 N20 C21 C22 168.00(15) . . . . ? C11 N10 C21 N20 135.98(16) . . . . ? Zn1 N10 C21 N20 -72.41(16) 2_655 . . . ? Zn1 N10 C21 N20 14.09(14) . . . . ? C11 N10 C21 C22 -47.3(2) . . . . ? Zn1 N10 C21 C22 104.32(18) 2_655 . . . ? Zn1 N10 C21 C22 -169.17(17) . . . . ? N20 C21 C22 C23 2.5(3) . . . . ? N10 C21 C22 C23 -173.95(17) . . . . ? C21 C22 C23 C24 -1.4(3) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? C21 N20 C25 C24 -0.3(3) . . . . ? Zn1 N20 C25 C24 -162.96(15) . . . . ? C21 N20 C25 C26 177.97(16) . . . . ? Zn1 N20 C25 C26 15.3(3) . . . . ? C23 C24 C25 N20 1.3(3) . . . . ? C23 C24 C25 C26 -176.93(17) . . . . ? N20 C25 C26 C29 2.9(2) . . . . ? C24 C25 C26 C29 -178.82(17) . . . . ? N20 C25 C26 C27 123.28(19) . . . . ? C24 C25 C26 C27 -58.5(2) . . . . ? N20 C25 C26 C28 -117.01(19) . . . . ? C24 C25 C26 C28 61.2(2) . . . . ?