# 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 _publ_contact_author_name 'Jean-Francois Carpentier' _publ_contact_author_email JEAN-FRANCOIS.CARPENTIER@UNIV-RENNES1.FR _publ_section_title ; Zinc and Enolato-Magnesium Complexes Based on Bi-, Tri- and Tetradentate Aminophenolate Ligands ; _publ_requested_category FM loop_ _publ_author_name 'Jean-Francois Carpentier' 'Miloud Bouyahyi' 'Osvaldo Casagrande Junior' 'Remy Fablet' 'Thierry Roisnel' ; C.M.Thomas ; 'Gang Zhao.' 'Zhanjiang Zheng.' # Attachment 'complex3_ZG01.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-01-12 at 17:07:03 # 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_job_1 _database_code_depnum_ccdc_archive 'CCDC 672301' _audit_creation_date 2007-01-12T17:07:03-00:00 _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 'C31 H49 N5 O Zn' _chemical_formula_sum 'C31 H49 N5 O Zn' _chemical_formula_weight 573.12 _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 31.6107(11) _cell_length_b 11.2967(3) _cell_length_c 17.4711(6) _cell_angle_alpha 90 _cell_angle_beta 96.688(2) _cell_angle_gamma 90 _cell_volume 6196.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.823 _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 0.814 _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 0.0831 _diffrn_reflns_av_unetI/netI 0.0678 _diffrn_reflns_number 28903 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.59 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 7145 _reflns_number_gt 5024 _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^)+(0.0531P)^2^+2.1426P] 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 7145 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.415 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.178943(8) 0.00382(2) 0.343427(16) 0.01889(9) Uani 1 d . . . C1 C 0.16934(8) 0.1390(2) 0.27157(14) 0.0250(5) Uani 1 d . . . H1A H 0.144 0.1831 0.2843 0.03 Uiso 1 calc R . . H1B H 0.1941 0.193 0.2806 0.03 Uiso 1 calc R . . C2 C 0.16278(9) 0.1077(2) 0.18638(15) 0.0321(6) Uani 1 d . . . H2A H 0.1583 0.1804 0.1558 0.048 Uiso 1 calc R . . H2B H 0.1378 0.0563 0.176 0.048 Uiso 1 calc R . . H2C H 0.188 0.0663 0.1724 0.048 Uiso 1 calc R . . N11 N 0.23072(6) 0.00925(15) 0.43036(12) 0.0193(4) Uani 1 d . . . N12 N 0.22582(6) 0.08330(15) 0.49051(11) 0.0191(4) Uani 1 d . . . C11 C 0.27744(8) -0.1568(2) 0.40431(16) 0.0285(6) Uani 1 d . . . H11A H 0.2594 -0.1559 0.3547 0.043 Uiso 0.5 calc PR . . H11B H 0.2746 -0.2333 0.4296 0.043 Uiso 0.5 calc PR . . H11C H 0.3072 -0.1445 0.3957 0.043 Uiso 0.5 calc PR . . H11D H 0.3014 -0.1999 0.4319 0.043 Uiso 0.5 calc PR . . H11E H 0.2862 -0.1225 0.3571 0.043 Uiso 0.5 calc PR . . H11F H 0.2536 -0.2113 0.391 0.043 Uiso 0.5 calc PR . . C12 C 0.26385(7) -0.06004(19) 0.45452(15) 0.0209(5) Uani 1 d . . . C13 C 0.28040(8) -0.0286(2) 0.52914(15) 0.0245(5) Uani 1 d . . . H13 H 0.3044 -0.0629 0.5589 0.029 Uiso 1 calc R . . C14 C 0.25533(7) 0.0614(2) 0.55136(14) 0.0220(5) Uani 1 d . . . C15 C 0.25681(8) 0.1288(2) 0.62509(15) 0.0293(6) Uani 1 d . . . H15A H 0.2338 0.1875 0.621 0.044 Uiso 0.5 calc PR . . H15B H 0.2843 0.1691 0.6354 0.044 Uiso 0.5 calc PR . . H15C H 0.2532 0.074 0.6673 0.044 Uiso 0.5 calc PR . . H15D H 0.2804 0.0996 0.6615 0.044 Uiso 0.5 calc PR . . H15E H 0.2299 0.1179 0.6471 0.044 Uiso 0.5 calc PR . . H15F H 0.261 0.2131 0.6151 0.044 Uiso 0.5 calc PR . . C16 C 0.18771(7) 0.15634(19) 0.48571(14) 0.0212(5) Uani 1 d . . . H16A H 0.1836 0.1958 0.4348 0.025 Uiso 1 calc R . . H16B H 0.1917 0.2187 0.5257 0.025 Uiso 1 calc R . . C17 C 0.14788(7) 0.08490(19) 0.49658(14) 0.0198(5) Uani 1 d . . . H17A H 0.1519 0.0467 0.5479 0.024 Uiso 1 calc R . . H17B H 0.1234 0.1396 0.4956 0.024 Uiso 1 calc R . . N21 N 0.13772(6) -0.00796(14) 0.43671(11) 0.0175(4) Uani 1 d . . . C21 C 0.09339(7) 0.00135(19) 0.39981(14) 0.0198(5) Uani 1 d . . . H21A H 0.0893 -0.0576 0.3577 0.024 Uiso 1 calc R . . H21B H 0.0895 0.0807 0.376 0.024 Uiso 1 calc R . . C22 C 0.05828(7) -0.0173(2) 0.45272(15) 0.0233(5) Uani 1 d . . . H22A H 0.0594 -0.0994 0.4726 0.028 Uiso 1 calc R . . H22B H 0.0627 0.0375 0.4972 0.028 Uiso 1 calc R . . N23 N 0.01719(6) 0.00484(16) 0.40920(13) 0.0238(4) Uani 1 d . . . N24 N 0.00505(7) 0.11953(17) 0.39421(15) 0.0336(5) Uani 1 d . . . C25 C -0.05337(10) 0.2193(3) 0.3136(2) 0.0659(12) Uani 1 d . . . H25A H -0.0382 0.2897 0.3351 0.099 Uiso 0.5 calc PR . . H25B H -0.0825 0.2195 0.3277 0.099 Uiso 0.5 calc PR . . H25C H -0.0543 0.22 0.2574 0.099 Uiso 0.5 calc PR . . H25D H -0.0784 0.1964 0.2784 0.099 Uiso 0.5 calc PR . . H25E H -0.0342 0.2666 0.2857 0.099 Uiso 0.5 calc PR . . H25F H -0.0624 0.2661 0.3561 0.099 Uiso 0.5 calc PR . . C26 C -0.03060(8) 0.1102(2) 0.34533(18) 0.0349(7) Uani 1 d . . . C27 C -0.04102(8) -0.0085(2) 0.33027(17) 0.0320(6) Uani 1 d . . . H27 H -0.0651 -0.0379 0.2983 0.038 Uiso 1 calc R . . C28 C -0.00975(8) -0.0731(2) 0.37069(16) 0.0288(6) Uani 1 d . . . C29 C -0.00330(9) -0.2041(2) 0.3785(2) 0.0537(10) Uani 1 d . . . H29A H 0.023 -0.2201 0.4124 0.081 Uiso 0.5 calc PR . . H29B H -0.0012 -0.2387 0.3276 0.081 Uiso 0.5 calc PR . . H29C H -0.0275 -0.2394 0.4006 0.081 Uiso 0.5 calc PR . . H29D H -0.0268 -0.2453 0.348 0.081 Uiso 0.5 calc PR . . H29E H -0.0026 -0.2268 0.4328 0.081 Uiso 0.5 calc PR . . H29F H 0.0237 -0.226 0.3598 0.081 Uiso 0.5 calc PR . . O31 O 0.17665(5) -0.16136(13) 0.32014(10) 0.0228(4) Uani 1 d . . . C31 C 0.15190(7) -0.24320(18) 0.34671(14) 0.0188(5) Uani 1 d . . . C32 C 0.13584(7) -0.23096(18) 0.41775(13) 0.0170(5) Uani 1 d . . . C33 C 0.14773(7) -0.12798(18) 0.47064(13) 0.0179(5) Uani 1 d . . . H33A H 0.1328 -0.1368 0.517 0.021 Uiso 1 calc R . . H33B H 0.1787 -0.132 0.4876 0.021 Uiso 1 calc R . . C34 C 0.11022(7) -0.31955(19) 0.44478(14) 0.0187(5) Uani 1 d . . . H34 H 0.0996 -0.3091 0.493 0.022 Uiso 1 calc R . . C35 C 0.14158(7) -0.34801(19) 0.30246(13) 0.0185(5) Uani 1 d . . . C36 C 0.15775(7) -0.3654(2) 0.22389(14) 0.0224(5) Uani 1 d . . . C36A C 0.13975(9) -0.2671(2) 0.16880(15) 0.0310(6) Uani 1 d . . . H36A H 0.1501 -0.278 0.1185 0.046 Uiso 1 calc R . . H36B H 0.1491 -0.1899 0.19 0.046 Uiso 1 calc R . . H36C H 0.1086 -0.2706 0.1627 0.046 Uiso 1 calc R . . C36B C 0.20671(8) -0.3636(2) 0.23229(15) 0.0271(6) Uani 1 d . . . H36D H 0.2165 -0.3748 0.1816 0.041 Uiso 1 calc R . . H36E H 0.2178 -0.4276 0.2669 0.041 Uiso 1 calc R . . H36F H 0.217 -0.2873 0.2537 0.041 Uiso 1 calc R . . C36C C 0.14337(9) -0.4842(2) 0.18719(16) 0.0308(6) Uani 1 d . . . H36G H 0.1543 -0.492 0.1372 0.046 Uiso 1 calc R . . H36H H 0.1122 -0.4875 0.1798 0.046 Uiso 1 calc R . . H36I H 0.1544 -0.549 0.2211 0.046 Uiso 1 calc R . . C37 C 0.11620(7) -0.43271(19) 0.33254(14) 0.0199(5) Uani 1 d . . . H37 H 0.1095 -0.5023 0.3031 0.024 Uiso 1 calc R . . C38 C 0.10004(7) -0.42198(18) 0.40290(14) 0.0195(5) Uani 1 d . . . C39 C 0.07216(8) -0.52125(19) 0.43003(15) 0.0236(5) Uani 1 d . . . C39A C 0.05763(8) -0.4941(2) 0.50874(15) 0.0269(5) Uani 1 d . . . H39A H 0.0826 -0.4816 0.5466 0.04 Uiso 1 calc R . . H39B H 0.041 -0.5608 0.525 0.04 Uiso 1 calc R . . H39C H 0.04 -0.4225 0.505 0.04 Uiso 1 calc R . . C39B C 0.03286(8) -0.5402(2) 0.37133(16) 0.0290(6) Uani 1 d . . . H39D H 0.0153 -0.6037 0.3893 0.043 Uiso 1 calc R . . H39E H 0.0419 -0.5622 0.3215 0.043 Uiso 1 calc R . . H39F H 0.0162 -0.4669 0.3657 0.043 Uiso 1 calc R . . C39C C 0.09789(9) -0.6370(2) 0.43773(18) 0.0368(7) Uani 1 d . . . H39G H 0.1232 -0.6259 0.475 0.055 Uiso 1 calc R . . H39H H 0.1066 -0.6585 0.3875 0.055 Uiso 1 calc R . . H39I H 0.0802 -0.7003 0.4555 0.055 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 0.01942(15) 0.01891(14) 0.01830(16) 0.00180(11) 0.00203(10) -0.00093(10) C1 0.0251(13) 0.0248(12) 0.0245(14) -0.0009(11) -0.0002(10) -0.0007(10) C2 0.0354(15) 0.0333(14) 0.0279(15) 0.0035(12) 0.0047(12) -0.0053(11) N11 0.0172(9) 0.0194(9) 0.0215(11) -0.0008(8) 0.0032(8) 0.0006(7) N12 0.0165(10) 0.0183(9) 0.0222(11) -0.0011(8) 0.0015(8) -0.0016(7) C11 0.0236(13) 0.0252(12) 0.0371(16) 0.0002(12) 0.0061(11) 0.0032(10) C12 0.0167(11) 0.0176(11) 0.0290(14) 0.0044(10) 0.0046(10) -0.0019(9) C13 0.0185(12) 0.0250(11) 0.0289(14) 0.0047(10) -0.0020(10) 0.0007(9) C14 0.0184(12) 0.0236(12) 0.0229(14) 0.0030(10) -0.0018(10) -0.0044(9) C15 0.0303(14) 0.0309(13) 0.0255(15) -0.0024(11) -0.0018(11) -0.0056(11) C16 0.0204(12) 0.0188(10) 0.0239(13) -0.0023(10) 0.0004(10) 0.0023(9) C17 0.0172(11) 0.0181(10) 0.0239(13) -0.0051(10) 0.0013(10) 0.0013(9) N21 0.0169(9) 0.0161(9) 0.0191(10) -0.0005(8) -0.0001(8) 0.0017(7) C21 0.0177(11) 0.0206(11) 0.0204(12) 0.0011(10) -0.0004(9) 0.0006(9) C22 0.0182(11) 0.0267(12) 0.0249(14) 0.0029(10) 0.0013(10) 0.0010(9) N23 0.0157(9) 0.0234(10) 0.0317(12) 0.0009(9) 0.0007(8) 0.0011(8) N24 0.0246(12) 0.0223(10) 0.0513(16) 0.0037(10) -0.0071(11) 0.0013(9) C25 0.0395(19) 0.0370(17) 0.111(3) 0.0236(19) -0.033(2) -0.0054(14) C26 0.0220(13) 0.0307(13) 0.0499(19) 0.0106(13) -0.0056(13) -0.0036(10) C27 0.0195(12) 0.0381(14) 0.0368(16) -0.0014(13) -0.0038(11) -0.0040(11) C28 0.0201(13) 0.0279(13) 0.0380(17) -0.0033(12) 0.0017(11) -0.0017(10) C29 0.0264(15) 0.0272(14) 0.104(3) -0.0131(17) -0.0084(17) 0.0021(12) O31 0.0258(9) 0.0190(8) 0.0251(10) -0.0018(7) 0.0093(7) -0.0039(6) C31 0.0157(11) 0.0184(10) 0.0227(13) 0.0019(10) 0.0033(9) 0.0022(8) C32 0.0170(11) 0.0145(10) 0.0194(12) 0.0003(9) 0.0019(9) 0.0023(8) C33 0.0186(11) 0.0190(10) 0.0159(12) 0.0029(9) 0.0012(9) 0.0014(9) C34 0.0173(11) 0.0209(11) 0.0186(12) 0.0018(10) 0.0054(9) 0.0037(9) C35 0.0187(11) 0.0203(11) 0.0165(12) -0.0007(9) 0.0022(9) 0.0025(9) C36 0.0266(13) 0.0216(11) 0.0199(13) -0.0007(10) 0.0062(10) 0.0015(9) C36A 0.0346(15) 0.0367(14) 0.0219(14) 0.0023(12) 0.0043(11) 0.0052(11) C36B 0.0275(13) 0.0276(12) 0.0276(15) -0.0019(11) 0.0096(11) 0.0022(10) C36C 0.0374(15) 0.0305(14) 0.0252(14) -0.0075(11) 0.0069(12) -0.0028(11) C37 0.0188(12) 0.0170(11) 0.0232(13) -0.0014(10) -0.0008(10) 0.0010(9) C38 0.0187(11) 0.0166(10) 0.0229(13) 0.0029(10) 0.0007(10) 0.0014(8) C39 0.0235(12) 0.0199(11) 0.0279(14) 0.0011(10) 0.0056(10) -0.0029(9) C39A 0.0269(13) 0.0270(12) 0.0279(14) 0.0064(11) 0.0074(11) -0.0050(10) C39B 0.0248(13) 0.0289(12) 0.0340(16) -0.0038(12) 0.0066(12) -0.0066(10) C39C 0.0377(16) 0.0204(12) 0.054(2) 0.0094(13) 0.0139(14) 0.0013(11) #----------------------------------------------------------------------------# # 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 O31 1.9094(15) . ? Zn1 C1 1.978(2) . ? Zn1 N11 2.100(2) . ? Zn1 N21 2.2059(19) . ? C1 C2 1.520(4) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? N11 C12 1.336(3) . ? N11 N12 1.366(3) . ? N12 C14 1.353(3) . ? N12 C16 1.454(3) . ? C11 C12 1.495(3) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C11 H11D 0.98 . ? C11 H11E 0.98 . ? C11 H11F 0.98 . ? C12 C13 1.393(4) . ? C13 C14 1.373(3) . ? C13 H13 0.95 . ? C14 C15 1.492(3) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C15 H15D 0.98 . ? C15 H15E 0.98 . ? C15 H15F 0.98 . ? C16 C17 1.526(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 N21 1.490(3) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? N21 C21 1.477(3) . ? N21 C33 1.499(3) . ? C21 C22 1.539(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 N23 1.448(3) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? N23 C28 1.349(3) . ? N23 N24 1.368(3) . ? N24 C26 1.336(3) . ? C25 C26 1.501(4) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C25 H25D 0.98 . ? C25 H25E 0.98 . ? C25 H25F 0.98 . ? C26 C27 1.398(3) . ? C27 C28 1.359(4) . ? C27 H27 0.95 . ? C28 C29 1.499(4) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C29 H29D 0.98 . ? C29 H29E 0.98 . ? C29 H29F 0.98 . ? O31 C31 1.329(3) . ? C31 C32 1.401(3) . ? C31 C35 1.431(3) . ? C32 C34 1.403(3) . ? C32 C33 1.506(3) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C38 1.387(3) . ? C34 H34 0.95 . ? C35 C37 1.390(3) . ? C35 C36 1.532(3) . ? C36 C36C 1.533(3) . ? C36 C36A 1.535(3) . ? C36 C36B 1.538(3) . ? C36A H36A 0.98 . ? C36A H36B 0.98 . ? C36A H36C 0.98 . ? C36B H36D 0.98 . ? C36B H36E 0.98 . ? C36B H36F 0.98 . ? C36C H36G 0.98 . ? C36C H36H 0.98 . ? C36C H36I 0.98 . ? C37 C38 1.390(3) . ? C37 H37 0.95 . ? C38 C39 1.535(3) . ? C39 C39B 1.531(4) . ? C39 C39A 1.531(4) . ? C39 C39C 1.537(3) . ? C39A H39A 0.98 . ? C39A H39B 0.98 . ? C39A H39C 0.98 . ? C39B H39D 0.98 . ? C39B H39E 0.98 . ? C39B H39F 0.98 . ? C39C H39G 0.98 . ? C39C H39H 0.98 . ? C39C H39I 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 O31 Zn1 C1 128.33(9) . . ? O31 Zn1 N11 100.93(7) . . ? C1 Zn1 N11 119.05(9) . . ? O31 Zn1 N21 95.01(6) . . ? C1 Zn1 N21 117.09(8) . . ? N11 Zn1 N21 86.86(7) . . ? C2 C1 Zn1 115.81(17) . . ? C2 C1 H1A 108.3 . . ? Zn1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? Zn1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? 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 . . ? C12 N11 N12 105.70(19) . . ? C12 N11 Zn1 136.69(16) . . ? N12 N11 Zn1 115.19(13) . . ? C14 N12 N11 111.28(18) . . ? C14 N12 C16 129.8(2) . . ? N11 N12 C16 118.06(19) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C12 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C12 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? N11 C12 C13 110.0(2) . . ? N11 C12 C11 120.7(2) . . ? C13 C12 C11 129.3(2) . . ? C14 C13 C12 106.7(2) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? N12 C14 C13 106.3(2) . . ? N12 C14 C15 122.3(2) . . ? C13 C14 C15 131.4(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C14 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C14 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? N12 C16 C17 112.50(18) . . ? N12 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N12 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N21 C17 C16 113.48(19) . . ? N21 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? N21 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C21 N21 C17 111.86(17) . . ? C21 N21 C33 112.52(16) . . ? C17 N21 C33 109.93(18) . . ? C21 N21 Zn1 106.59(14) . . ? C17 N21 Zn1 112.25(13) . . ? C33 N21 Zn1 103.37(12) . . ? N21 C21 C22 116.2(2) . . ? N21 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? N21 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.4 . . ? N23 C22 C21 109.0(2) . . ? N23 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? N23 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C28 N23 N24 112.1(2) . . ? C28 N23 C22 128.67(19) . . ? N24 N23 C22 118.58(19) . . ? C26 N24 N23 104.1(2) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 C25 H25D 109.5 . . ? H25A C25 H25D 141.1 . . ? H25B C25 H25D 56.3 . . ? H25C C25 H25D 56.3 . . ? C26 C25 H25E 109.5 . . ? H25A C25 H25E 56.3 . . ? H25B C25 H25E 141.1 . . ? H25C C25 H25E 56.3 . . ? H25D C25 H25E 109.5 . . ? C26 C25 H25F 109.5 . . ? H25A C25 H25F 56.3 . . ? H25B C25 H25F 56.3 . . ? H25C C25 H25F 141.1 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? N24 C26 C27 111.0(2) . . ? N24 C26 C25 120.2(2) . . ? C27 C26 C25 128.7(3) . . ? C28 C27 C26 106.0(2) . . ? C28 C27 H27 127 . . ? C26 C27 H27 127 . . ? N23 C28 C27 106.7(2) . . ? N23 C28 C29 121.9(2) . . ? C27 C28 C29 131.4(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29 H29D 109.5 . . ? H29A C29 H29D 141.1 . . ? H29B C29 H29D 56.3 . . ? H29C C29 H29D 56.3 . . ? C28 C29 H29E 109.5 . . ? H29A C29 H29E 56.3 . . ? H29B C29 H29E 141.1 . . ? H29C C29 H29E 56.3 . . ? H29D C29 H29E 109.5 . . ? C28 C29 H29F 109.5 . . ? H29A C29 H29F 56.3 . . ? H29B C29 H29F 56.3 . . ? H29C C29 H29F 141.1 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? C31 O31 Zn1 127.92(14) . . ? O31 C31 C32 122.0(2) . . ? O31 C31 C35 119.6(2) . . ? C32 C31 C35 118.48(19) . . ? C31 C32 C34 120.7(2) . . ? C31 C32 C33 121.96(19) . . ? C34 C32 C33 117.2(2) . . ? N21 C33 C32 115.46(18) . . ? N21 C33 H33A 108.4 . . ? C32 C33 H33A 108.4 . . ? N21 C33 H33B 108.4 . . ? C32 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C38 C34 C32 121.7(2) . . ? C38 C34 H34 119.2 . . ? C32 C34 H34 119.2 . . ? C37 C35 C31 118.1(2) . . ? C37 C35 C36 121.2(2) . . ? C31 C35 C36 120.76(19) . . ? C35 C36 C36C 111.94(19) . . ? C35 C36 C36A 109.32(19) . . ? C36C C36 C36A 107.5(2) . . ? C35 C36 C36B 110.5(2) . . ? C36C C36 C36B 107.33(19) . . ? C36A C36 C36B 110.2(2) . . ? C36 C36A H36A 109.5 . . ? C36 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C36 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C36 C36B H36D 109.5 . . ? C36 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C36 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C36 C36C H36G 109.5 . . ? C36 C36C H36H 109.5 . . ? H36G C36C H36H 109.5 . . ? C36 C36C H36I 109.5 . . ? H36G C36C H36I 109.5 . . ? H36H C36C H36I 109.5 . . ? C38 C37 C35 124.2(2) . . ? C38 C37 H37 117.9 . . ? C35 C37 H37 117.9 . . ? C34 C38 C37 116.9(2) . . ? C34 C38 C39 123.6(2) . . ? C37 C38 C39 119.5(2) . . ? C39B C39 C39A 109.0(2) . . ? C39B C39 C38 110.2(2) . . ? C39A C39 C38 111.98(19) . . ? C39B C39 C39C 108.6(2) . . ? C39A C39 C39C 107.6(2) . . ? C38 C39 C39C 109.34(19) . . ? C39 C39A H39A 109.5 . . ? C39 C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C39 C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C39 C39B H39D 109.5 . . ? C39 C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C39 C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C39 C39C H39G 109.5 . . ? C39 C39C H39H 109.5 . . ? H39G C39C H39H 109.5 . . ? C39 C39C H39I 109.5 . . ? H39G C39C H39I 109.5 . . ? H39H C39C H39I 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 O31 Zn1 C1 C2 -5.4(2) . . . . ? N11 Zn1 C1 C2 130.34(17) . . . . ? N21 Zn1 C1 C2 -127.33(18) . . . . ? O31 Zn1 N11 C12 19.6(2) . . . . ? C1 Zn1 N11 C12 -126.5(2) . . . . ? N21 Zn1 N11 C12 114.1(2) . . . . ? O31 Zn1 N11 N12 -139.61(14) . . . . ? C1 Zn1 N11 N12 74.31(17) . . . . ? N21 Zn1 N11 N12 -45.11(14) . . . . ? C12 N11 N12 C14 0.2(2) . . . . ? Zn1 N11 N12 C14 165.52(14) . . . . ? C12 N11 N12 C16 -170.08(18) . . . . ? Zn1 N11 N12 C16 -4.7(2) . . . . ? N12 N11 C12 C13 -1.1(2) . . . . ? Zn1 N11 C12 C13 -161.64(17) . . . . ? N12 N11 C12 C11 177.31(19) . . . . ? Zn1 N11 C12 C11 16.8(3) . . . . ? N11 C12 C13 C14 1.7(3) . . . . ? C11 C12 C13 C14 -176.6(2) . . . . ? N11 N12 C14 C13 0.9(2) . . . . ? C16 N12 C14 C13 169.6(2) . . . . ? N11 N12 C14 C15 -179.2(2) . . . . ? C16 N12 C14 C15 -10.4(4) . . . . ? C12 C13 C14 N12 -1.5(3) . . . . ? C12 C13 C14 C15 178.6(2) . . . . ? C14 N12 C16 C17 -95.2(3) . . . . ? N11 N12 C16 C17 73.0(3) . . . . ? N12 C16 C17 N21 -61.7(3) . . . . ? C16 C17 N21 C21 -127.2(2) . . . . ? C16 C17 N21 C33 107.0(2) . . . . ? C16 C17 N21 Zn1 -7.4(2) . . . . ? O31 Zn1 N21 C21 -86.46(13) . . . . ? C1 Zn1 N21 C21 51.62(15) . . . . ? N11 Zn1 N21 C21 172.83(13) . . . . ? O31 Zn1 N21 C17 150.74(14) . . . . ? C1 Zn1 N21 C17 -71.18(17) . . . . ? N11 Zn1 N21 C17 50.03(14) . . . . ? O31 Zn1 N21 C33 32.33(14) . . . . ? C1 Zn1 N21 C33 170.41(14) . . . . ? N11 Zn1 N21 C33 -68.38(13) . . . . ? C17 N21 C21 C22 -63.0(2) . . . . ? C33 N21 C21 C22 61.4(2) . . . . ? Zn1 N21 C21 C22 174.00(15) . . . . ? N21 C21 C22 N23 175.11(17) . . . . ? C21 C22 N23 C28 93.4(3) . . . . ? C21 C22 N23 N24 -76.4(3) . . . . ? C28 N23 N24 C26 0.4(3) . . . . ? C22 N23 N24 C26 171.8(2) . . . . ? N23 N24 C26 C27 0.6(3) . . . . ? N23 N24 C26 C25 -178.6(3) . . . . ? N24 C26 C27 C28 -1.3(3) . . . . ? C25 C26 C27 C28 177.8(3) . . . . ? N24 N23 C28 C27 -1.2(3) . . . . ? C22 N23 C28 C27 -171.5(2) . . . . ? N24 N23 C28 C29 -179.4(3) . . . . ? C22 N23 C28 C29 10.3(4) . . . . ? C26 C27 C28 N23 1.4(3) . . . . ? C26 C27 C28 C29 179.4(3) . . . . ? C1 Zn1 O31 C31 -121.6(2) . . . . ? N11 Zn1 O31 C31 96.82(19) . . . . ? N21 Zn1 O31 C31 9.1(2) . . . . ? Zn1 O31 C31 C32 -26.0(3) . . . . ? Zn1 O31 C31 C35 154.87(16) . . . . ? O31 C31 C32 C34 -179.2(2) . . . . ? C35 C31 C32 C34 0.0(3) . . . . ? O31 C31 C32 C33 -3.8(3) . . . . ? C35 C31 C32 C33 175.4(2) . . . . ? C21 N21 C33 C32 50.2(2) . . . . ? C17 N21 C33 C32 175.58(18) . . . . ? Zn1 N21 C33 C32 -64.41(19) . . . . ? C31 C32 C33 N21 57.9(3) . . . . ? C34 C32 C33 N21 -126.5(2) . . . . ? C31 C32 C34 C38 0.3(3) . . . . ? C33 C32 C34 C38 -175.3(2) . . . . ? O31 C31 C35 C37 178.9(2) . . . . ? C32 C31 C35 C37 -0.2(3) . . . . ? O31 C31 C35 C36 -1.6(3) . . . . ? C32 C31 C35 C36 179.2(2) . . . . ? C37 C35 C36 C36C -1.3(3) . . . . ? C31 C35 C36 C36C 179.3(2) . . . . ? C37 C35 C36 C36A 117.7(2) . . . . ? C31 C35 C36 C36A -61.7(3) . . . . ? C37 C35 C36 C36B -120.8(2) . . . . ? C31 C35 C36 C36B 59.8(3) . . . . ? C31 C35 C37 C38 0.2(3) . . . . ? C36 C35 C37 C38 -179.2(2) . . . . ? C32 C34 C38 C37 -0.4(3) . . . . ? C32 C34 C38 C39 -180.0(2) . . . . ? C35 C37 C38 C34 0.1(3) . . . . ? C35 C37 C38 C39 179.7(2) . . . . ? C34 C38 C39 C39B 120.7(2) . . . . ? C37 C38 C39 C39B -58.9(3) . . . . ? C34 C38 C39 C39A -0.8(3) . . . . ? C37 C38 C39 C39A 179.6(2) . . . . ? C34 C38 C39 C39C -119.9(3) . . . . ? C37 C38 C39 C39C 60.4(3) . . . . ? # Attachment 'complex4_ZG55.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-03-07 at 16:43:18 # 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_job_2 _database_code_depnum_ccdc_archive 'CCDC 672302' _audit_creation_date 2007-03-07T16:43:18-00:00 _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 'C35 H62 N6 O1 Si2 Zn1' _chemical_formula_sum 'C35 H62 N6 O Si2 Zn' _chemical_formula_weight 704.46 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # 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 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7495(4) _cell_length_b 14.5448(5) _cell_length_c 14.7216(5) _cell_angle_alpha 62.3027(17) _cell_angle_beta 88.2672(17) _cell_angle_gamma 67.8521(17) _cell_volume 2030.70(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5339 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.50 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.696 _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 0.816 _exptl_absorpt_correction_T_max 0.946 #----------------------------------------------------------------------------# # 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 0.0379 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_number 19863 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 9258 _reflns_number_gt 7219 _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^)+(0.0480P)^2^+0.7946P] 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 9258 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.097 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.445 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 0.84092(2) 0.43536(2) 0.791540(19) 0.01583(8) Uani 1 d . . . N1 N 0.82343(16) 0.58263(15) 0.76777(14) 0.0181(4) Uani 1 d . . . Si1 Si 0.96242(6) 0.59683(5) 0.76257(5) 0.02135(14) Uani 1 d . . . C1A C 1.0334(3) 0.5861(3) 0.6497(3) 0.0507(9) Uani 1 d . . . H1A1 H 0.9745 0.6447 0.5845 0.076 Uiso 1 calc R . . H1A2 H 1.052 0.5107 0.6583 0.076 Uiso 1 calc R . . H1A3 H 1.1108 0.5975 0.6474 0.076 Uiso 1 calc R . . C1B C 1.0826(2) 0.4816(2) 0.8808(2) 0.0395(7) Uani 1 d . . . H1B1 H 1.0921 0.4072 0.8912 0.059 Uiso 1 calc R . . H1B2 H 1.0562 0.4886 0.9419 0.059 Uiso 1 calc R . . H1B3 H 1.1626 0.4883 0.8713 0.059 Uiso 1 calc R . . C1C C 0.9512(2) 0.7352(2) 0.7483(2) 0.0336(6) Uani 1 d . . . H1C1 H 0.8894 0.7986 0.6864 0.05 Uiso 1 calc R . . H1C2 H 1.0328 0.7389 0.7407 0.05 Uiso 1 calc R . . H1C3 H 0.9255 0.7405 0.8103 0.05 Uiso 1 calc R . . Si2 Si 0.68099(6) 0.69104(5) 0.74300(5) 0.01938(13) Uani 1 d . . . C2A C 0.6386(2) 0.8104(2) 0.60477(19) 0.0305(5) Uani 1 d . . . H2A1 H 0.6435 0.7801 0.557 0.046 Uiso 1 calc R . . H2A2 H 0.6969 0.847 0.5923 0.046 Uiso 1 calc R . . H2A3 H 0.5534 0.8665 0.5929 0.046 Uiso 1 calc R . . C2B C 0.6718(2) 0.7541(2) 0.8308(2) 0.0301(5) Uani 1 d . . . H2B1 H 0.6948 0.6935 0.9037 0.045 Uiso 1 calc R . . H2B2 H 0.5864 0.8101 0.8185 0.045 Uiso 1 calc R . . H2B3 H 0.7293 0.7916 0.8158 0.045 Uiso 1 calc R . . C2C C 0.5483(2) 0.6446(2) 0.76497(19) 0.0245(5) Uani 1 d . . . H2C1 H 0.5656 0.5815 0.8362 0.037 Uiso 1 calc R . . H2C2 H 0.5396 0.6196 0.7151 0.037 Uiso 1 calc R . . H2C3 H 0.4707 0.7085 0.755 0.037 Uiso 1 calc R . . N11 N 0.71672(16) 0.37520(15) 0.87385(14) 0.0176(4) Uani 1 d . . . N12 N 0.62683(16) 0.35588(16) 0.83736(14) 0.0185(4) Uani 1 d . . . C11 C 0.7736(2) 0.3837(2) 1.02809(19) 0.0291(5) Uani 1 d . . . H11A H 0.8393 0.4007 0.99 0.044 Uiso 0.5 calc PR . . H11B H 0.8118 0.3153 1.0963 0.044 Uiso 0.5 calc PR . . H11C H 0.7215 0.4481 1.0379 0.044 Uiso 0.5 calc PR . . H11D H 0.7424 0.3753 1.0927 0.044 Uiso 0.5 calc PR . . H11E H 0.7699 0.4607 0.9865 0.044 Uiso 0.5 calc PR . . H11F H 0.8602 0.328 1.0449 0.044 Uiso 0.5 calc PR . . C12 C 0.6947(2) 0.36377(19) 0.96723(17) 0.0206(5) Uani 1 d . . . C13 C 0.5912(2) 0.3370(2) 0.99038(19) 0.0259(5) Uani 1 d . . . H13 H 0.5564 0.3242 1.052 0.031 Uiso 1 calc R . . C14 C 0.5499(2) 0.3328(2) 0.90665(18) 0.0227(5) Uani 1 d . . . C15 C 0.4421(2) 0.3102(2) 0.8860(2) 0.0330(6) Uani 1 d . . . H15A H 0.4379 0.3163 0.8169 0.049 Uiso 0.5 calc PR . . H15B H 0.3644 0.366 0.8885 0.049 Uiso 0.5 calc PR . . H15C H 0.4533 0.2333 0.9391 0.049 Uiso 0.5 calc PR . . H15D H 0.3992 0.2941 0.9461 0.049 Uiso 0.5 calc PR . . H15E H 0.4726 0.2444 0.8745 0.049 Uiso 0.5 calc PR . . H15F H 0.3838 0.3771 0.8239 0.049 Uiso 0.5 calc PR . . C16 C 0.6111(2) 0.3712(2) 0.73232(18) 0.0218(5) Uani 1 d . . . H16A H 0.5548 0.4514 0.6841 0.026 Uiso 1 calc R . . H16B H 0.5703 0.3228 0.7325 0.026 Uiso 1 calc R . . C17 C 0.7315(2) 0.3423(2) 0.69152(18) 0.0204(5) Uani 1 d . . . H17A H 0.7932 0.2676 0.746 0.024 Uiso 1 calc R . . H17B H 0.7162 0.3341 0.6305 0.024 Uiso 1 calc R . . N21 N 0.78736(16) 0.42713(15) 0.66013(14) 0.0170(4) Uani 1 d . . . C21 C 0.70533(19) 0.54242(19) 0.57894(17) 0.0192(4) Uani 1 d . . . H21A H 0.7522 0.5909 0.5608 0.023 Uiso 1 calc R . . H21B H 0.6339 0.5732 0.6091 0.023 Uiso 1 calc R . . C22 C 0.6531(2) 0.5545(2) 0.47748(18) 0.0229(5) Uani 1 d . . . H22A H 0.7213 0.5369 0.4391 0.028 Uiso 1 calc R . . H22B H 0.613 0.5011 0.4935 0.028 Uiso 1 calc R . . N23 N 0.56162(16) 0.67168(16) 0.41456(14) 0.0199(4) Uani 1 d . . . N24 N 0.44631(16) 0.70233(17) 0.44152(15) 0.0222(4) Uani 1 d . . . C25 C 0.2587(2) 0.8796(3) 0.3857(3) 0.0474(8) Uani 1 d . . . H25A H 0.2276 0.8268 0.438 0.071 Uiso 1 calc R . . H25B H 0.2058 0.9182 0.3175 0.071 Uiso 1 calc R . . H25C H 0.2566 0.9362 0.405 0.071 Uiso 1 calc R . . C26 C 0.3905(2) 0.8145(2) 0.3805(2) 0.0289(5) Uani 1 d . . . C27 C 0.4698(3) 0.8556(2) 0.3159(2) 0.0340(6) Uani 1 d . . . H27 H 0.4513 0.9323 0.2653 0.041 Uiso 1 calc R . . C28 C 0.5795(2) 0.7625(2) 0.34070(19) 0.0272(5) Uani 1 d . . . C29 C 0.7013(3) 0.7506(3) 0.3029(2) 0.0417(7) Uani 1 d . . . H29A H 0.7596 0.6701 0.3382 0.063 Uiso 0.5 calc PR . . H29B H 0.7363 0.7943 0.3182 0.063 Uiso 0.5 calc PR . . H29C H 0.6877 0.7795 0.2275 0.063 Uiso 0.5 calc PR . . H29D H 0.6961 0.8258 0.2511 0.063 Uiso 0.5 calc PR . . H29E H 0.7194 0.7017 0.2711 0.063 Uiso 0.5 calc PR . . H29F H 0.768 0.7165 0.3618 0.063 Uiso 0.5 calc PR . . O31 O 1.00301(13) 0.30981(13) 0.83567(12) 0.0198(3) Uani 1 d . . . C31 C 1.03793(19) 0.23334(18) 0.80322(17) 0.0173(4) Uani 1 d . . . C32 C 0.99523(19) 0.26553(18) 0.69975(17) 0.0174(4) Uani 1 d . . . C33 C 0.90792(19) 0.38566(19) 0.62461(17) 0.0186(4) Uani 1 d . . . H33A H 0.9503 0.4364 0.6135 0.022 Uiso 1 calc R . . H33B H 0.8893 0.391 0.5568 0.022 Uiso 1 calc R . . C34 C 1.12057(19) 0.11784(18) 0.86992(17) 0.0175(4) Uani 1 d . . . C35 C 1.1703(2) 0.0754(2) 0.98445(18) 0.0228(5) Uani 1 d . . . C35A C 1.0607(2) 0.1005(2) 1.04264(19) 0.0312(6) Uani 1 d . . . H35A H 1.0075 0.1823 1.0064 0.047 Uiso 1 calc R . . H35B H 1.0937 0.0766 1.1141 0.047 Uiso 1 calc R . . H35C H 1.0114 0.0585 1.0443 0.047 Uiso 1 calc R . . C35B C 1.2524(2) 0.1358(2) 0.9870(2) 0.0298(5) Uani 1 d . . . H35D H 1.2034 0.2184 0.9495 0.045 Uiso 1 calc R . . H35E H 1.3243 0.1161 0.9537 0.045 Uiso 1 calc R . . H35F H 1.2817 0.1112 1.0595 0.045 Uiso 1 calc R . . C35C C 1.2504(2) -0.0530(2) 1.04462(19) 0.0312(6) Uani 1 d . . . H35G H 1.2007 -0.0939 1.0442 0.047 Uiso 1 calc R . . H35H H 1.279 -0.0757 1.1167 0.047 Uiso 1 calc R . . H35I H 1.3229 -0.0716 1.0114 0.047 Uiso 1 calc R . . C36 C 1.15966(19) 0.04437(19) 0.82837(17) 0.0185(4) Uani 1 d . . . H36 H 1.2163 -0.0322 0.8729 0.022 Uiso 1 calc R . . C37 C 1.1204(2) 0.07672(19) 0.72484(17) 0.0192(4) Uani 1 d . . . C38 C 1.1756(2) -0.00712(19) 0.68279(18) 0.0224(5) Uani 1 d . . . C38A C 1.1641(3) -0.1184(2) 0.7534(2) 0.0353(6) Uani 1 d . . . H38A H 1.2048 -0.1498 0.8248 0.053 Uiso 1 calc R . . H38B H 1.2044 -0.1728 0.7286 0.053 Uiso 1 calc R . . H38C H 1.0757 -0.1045 0.7525 0.053 Uiso 1 calc R . . C38B C 1.3134(2) -0.0295(2) 0.6794(2) 0.0340(6) Uani 1 d . . . H38D H 1.3206 0.0425 0.6345 0.051 Uiso 1 calc R . . H38E H 1.3496 -0.0817 0.6516 0.051 Uiso 1 calc R . . H38F H 1.3583 -0.0637 0.75 0.051 Uiso 1 calc R . . C38C C 1.1102(3) 0.0416(2) 0.5716(2) 0.0371(6) Uani 1 d . . . H38G H 1.1176 0.1132 0.5254 0.056 Uiso 1 calc R . . H38H H 1.0218 0.0559 0.5716 0.056 Uiso 1 calc R . . H38I H 1.1495 -0.013 0.5469 0.056 Uiso 1 calc R . . C39 C 1.03599(19) 0.18769(19) 0.66282(17) 0.0189(4) Uani 1 d . . . H39 H 1.0047 0.2119 0.5931 0.023 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 0.01439(13) 0.01924(14) 0.01663(13) -0.01016(11) 0.00280(9) -0.00783(10) N1 0.0162(9) 0.0207(10) 0.0217(10) -0.0129(8) 0.0040(7) -0.0087(8) Si1 0.0205(3) 0.0254(3) 0.0265(3) -0.0160(3) 0.0080(3) -0.0136(3) C1A 0.0574(19) 0.090(3) 0.062(2) -0.059(2) 0.0442(17) -0.060(2) C1B 0.0251(13) 0.0324(15) 0.0599(19) -0.0218(15) -0.0071(13) -0.0106(12) C1C 0.0325(14) 0.0285(14) 0.0446(16) -0.0174(13) 0.0029(12) -0.0176(12) Si2 0.0187(3) 0.0198(3) 0.0192(3) -0.0107(3) 0.0035(2) -0.0060(3) C2A 0.0273(13) 0.0278(13) 0.0269(13) -0.0094(11) 0.0044(11) -0.0073(11) C2B 0.0283(13) 0.0312(14) 0.0349(14) -0.0233(12) 0.0058(11) -0.0071(11) C2C 0.0183(11) 0.0281(13) 0.0284(13) -0.0172(11) 0.0063(10) -0.0064(10) N11 0.0185(9) 0.0214(10) 0.0170(9) -0.0102(8) 0.0031(7) -0.0111(8) N12 0.0188(9) 0.0241(10) 0.0177(9) -0.0117(8) 0.0039(7) -0.0120(8) C11 0.0418(15) 0.0364(14) 0.0201(12) -0.0158(11) 0.0076(11) -0.0244(13) C12 0.0238(11) 0.0218(12) 0.0189(11) -0.0111(10) 0.0044(9) -0.0105(10) C13 0.0293(13) 0.0348(14) 0.0254(12) -0.0197(11) 0.0145(10) -0.0189(11) C14 0.0200(11) 0.0272(12) 0.0265(12) -0.0164(11) 0.0084(10) -0.0114(10) C15 0.0233(12) 0.0504(17) 0.0386(15) -0.0265(14) 0.0115(11) -0.0224(12) C16 0.0202(11) 0.0301(13) 0.0218(12) -0.0154(11) 0.0045(9) -0.0135(10) C17 0.0205(11) 0.0278(12) 0.0217(11) -0.0164(10) 0.0066(9) -0.0130(10) N21 0.0146(9) 0.0210(9) 0.0170(9) -0.0112(8) 0.0031(7) -0.0065(8) C21 0.0152(10) 0.0245(12) 0.0183(11) -0.0124(10) 0.0008(9) -0.0058(9) C22 0.0194(11) 0.0284(13) 0.0210(12) -0.0144(10) 0.0003(9) -0.0065(10) N23 0.0150(9) 0.0268(10) 0.0184(9) -0.0117(9) 0.0017(7) -0.0082(8) N24 0.0141(9) 0.0324(11) 0.0239(10) -0.0182(9) 0.0026(8) -0.0076(8) C25 0.0266(14) 0.0456(18) 0.064(2) -0.0355(17) -0.0022(14) 0.0033(13) C26 0.0253(12) 0.0304(14) 0.0321(14) -0.0196(12) -0.0035(11) -0.0061(11) C27 0.0432(15) 0.0259(13) 0.0275(14) -0.0079(12) -0.0052(12) -0.0146(12) C28 0.0292(13) 0.0332(14) 0.0233(12) -0.0123(11) 0.0017(10) -0.0184(11) C29 0.0421(16) 0.059(2) 0.0376(16) -0.0229(15) 0.0151(13) -0.0359(16) O31 0.0177(8) 0.0221(8) 0.0233(8) -0.0152(7) 0.0001(6) -0.0062(7) C31 0.0131(10) 0.0222(11) 0.0200(11) -0.0118(10) 0.0050(8) -0.0088(9) C32 0.0137(10) 0.0204(11) 0.0188(11) -0.0099(9) 0.0039(8) -0.0073(9) C33 0.0170(10) 0.0239(12) 0.0172(11) -0.0121(10) 0.0052(9) -0.0084(9) C34 0.0139(10) 0.0214(11) 0.0184(11) -0.0088(9) 0.0030(8) -0.0095(9) C35 0.0231(12) 0.0241(12) 0.0196(12) -0.0105(10) 0.0014(9) -0.0083(10) C35A 0.0335(14) 0.0382(15) 0.0210(12) -0.0155(12) 0.0068(11) -0.0127(12) C35B 0.0257(13) 0.0321(14) 0.0302(14) -0.0153(12) -0.0044(11) -0.0100(11) C35C 0.0388(15) 0.0281(13) 0.0215(13) -0.0111(11) -0.0026(11) -0.0094(12) C36 0.0165(10) 0.0171(11) 0.0203(11) -0.0085(9) 0.0039(9) -0.0063(9) C37 0.0173(10) 0.0237(12) 0.0209(11) -0.0133(10) 0.0064(9) -0.0096(9) C38 0.0250(12) 0.0225(12) 0.0217(12) -0.0134(10) 0.0055(10) -0.0083(10) C38A 0.0536(17) 0.0305(14) 0.0363(15) -0.0228(13) 0.0174(13) -0.0235(13) C38B 0.0266(13) 0.0311(14) 0.0465(17) -0.0234(13) 0.0142(12) -0.0087(11) C38C 0.0397(15) 0.0384(16) 0.0324(15) -0.0271(13) 0.0039(12) -0.0025(13) C39 0.0159(10) 0.0260(12) 0.0162(11) -0.0116(10) 0.0039(8) -0.0086(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 N1 1.9310(17) . ? Zn1 O31 1.9323(15) . ? Zn1 N11 2.0575(16) . ? Zn1 N21 2.1210(17) . ? N1 Si2 1.7126(19) . ? N1 Si1 1.7168(17) . ? Si1 C1B 1.867(3) . ? Si1 C1C 1.877(2) . ? Si1 C1A 1.882(3) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C1C H1C1 0.98 . ? C1C H1C2 0.98 . ? C1C H1C3 0.98 . ? Si2 C2A 1.879(3) . ? Si2 C2B 1.882(2) . ? Si2 C2C 1.885(2) . ? C2A H2A1 0.98 . ? C2A H2A2 0.98 . ? C2A H2A3 0.98 . ? C2B H2B1 0.98 . ? C2B H2B2 0.98 . ? C2B H2B3 0.98 . ? C2C H2C1 0.98 . ? C2C H2C2 0.98 . ? C2C H2C3 0.98 . ? N11 C12 1.335(3) . ? N11 N12 1.372(2) . ? N12 C14 1.351(3) . ? N12 C16 1.463(3) . ? C11 C12 1.497(3) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C11 H11D 0.98 . ? C11 H11E 0.98 . ? C11 H11F 0.98 . ? C12 C13 1.397(3) . ? C13 C14 1.374(3) . ? C13 H13 0.95 . ? C14 C15 1.496(3) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C15 H15D 0.98 . ? C15 H15E 0.98 . ? C15 H15F 0.98 . ? C16 C17 1.508(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 N21 1.493(2) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? N21 C21 1.469(3) . ? N21 C33 1.499(3) . ? C21 C22 1.539(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 N23 1.459(3) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? N23 C28 1.353(3) . ? N23 N24 1.367(2) . ? N24 C26 1.329(3) . ? C25 C26 1.502(4) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 C27 1.402(4) . ? C27 C28 1.371(4) . ? C27 H27 0.95 . ? C28 C29 1.497(3) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C29 H29D 0.98 . ? C29 H29E 0.98 . ? C29 H29F 0.98 . ? O31 C31 1.331(2) . ? C31 C32 1.413(3) . ? C31 C34 1.422(3) . ? C32 C39 1.398(3) . ? C32 C33 1.500(3) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C36 1.396(3) . ? C34 C35 1.544(3) . ? C35 C35C 1.532(3) . ? C35 C35B 1.541(3) . ? C35 C35A 1.547(3) . ? C35A H35A 0.98 . ? C35A H35B 0.98 . ? C35A H35C 0.98 . ? C35B H35D 0.98 . ? C35B H35E 0.98 . ? C35B H35F 0.98 . ? C35C H35G 0.98 . ? C35C H35H 0.98 . ? C35C H35I 0.98 . ? C36 C37 1.403(3) . ? C36 H36 0.95 . ? C37 C39 1.379(3) . ? C37 C38 1.540(3) . ? C38 C38A 1.520(3) . ? C38 C38B 1.531(3) . ? C38 C38C 1.535(3) . ? C38A H38A 0.98 . ? C38A H38B 0.98 . ? C38A H38C 0.98 . ? C38B H38D 0.98 . ? C38B H38E 0.98 . ? C38B H38F 0.98 . ? C38C H38G 0.98 . ? C38C H38H 0.98 . ? C38C H38I 0.98 . ? C39 H39 0.95 . ? 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 N1 Zn1 O31 121.17(7) . . ? N1 Zn1 N11 116.17(7) . . ? O31 Zn1 N11 108.62(7) . . ? N1 Zn1 N21 116.65(7) . . ? O31 Zn1 N21 95.71(6) . . ? N11 Zn1 N21 93.50(7) . . ? Si2 N1 Si1 124.00(10) . . ? Si2 N1 Zn1 122.48(9) . . ? Si1 N1 Zn1 113.27(10) . . ? N1 Si1 C1B 112.25(11) . . ? N1 Si1 C1C 114.64(10) . . ? C1B Si1 C1C 106.53(12) . . ? N1 Si1 C1A 111.58(11) . . ? C1B Si1 C1A 105.21(15) . . ? C1C Si1 C1A 105.97(13) . . ? Si1 C1A H1A1 109.5 . . ? Si1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Si1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? Si1 C1B H1B1 109.5 . . ? Si1 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? Si1 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? Si1 C1C H1C1 109.5 . . ? Si1 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? Si1 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? N1 Si2 C2A 112.76(10) . . ? N1 Si2 C2B 112.64(10) . . ? C2A Si2 C2B 107.51(12) . . ? N1 Si2 C2C 113.32(10) . . ? C2A Si2 C2C 105.70(11) . . ? C2B Si2 C2C 104.27(11) . . ? Si2 C2A H2A1 109.5 . . ? Si2 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? Si2 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? Si2 C2B H2B1 109.5 . . ? Si2 C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? Si2 C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? Si2 C2C H2C1 109.5 . . ? Si2 C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? Si2 C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? C12 N11 N12 105.90(16) . . ? C12 N11 Zn1 126.75(14) . . ? N12 N11 Zn1 126.64(13) . . ? C14 N12 N11 110.96(17) . . ? C14 N12 C16 125.75(17) . . ? N11 N12 C16 122.97(16) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C12 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C12 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? N11 C12 C13 109.88(19) . . ? N11 C12 C11 120.14(18) . . ? C13 C12 C11 129.9(2) . . ? C14 C13 C12 106.55(19) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? N12 C14 C13 106.72(18) . . ? N12 C14 C15 122.3(2) . . ? C13 C14 C15 131.0(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C14 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C14 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? N12 C16 C17 114.06(18) . . ? N12 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? N12 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N21 C17 C16 115.13(18) . . ? N21 C17 H17A 108.5 . . ? C16 C17 H17A 108.5 . . ? N21 C17 H17B 108.5 . . ? C16 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C21 N21 C17 114.22(17) . . ? C21 N21 C33 109.79(16) . . ? C17 N21 C33 109.21(16) . . ? C21 N21 Zn1 108.75(12) . . ? C17 N21 Zn1 110.37(13) . . ? C33 N21 Zn1 104.01(12) . . ? N21 C21 C22 116.93(18) . . ? N21 C21 H21A 108.1 . . ? C22 C21 H21A 108.1 . . ? N21 C21 H21B 108.1 . . ? C22 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? N23 C22 C21 107.74(18) . . ? N23 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? N23 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C28 N23 N24 112.26(19) . . ? C28 N23 C22 128.61(19) . . ? N24 N23 C22 118.27(18) . . ? C26 N24 N23 104.63(18) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N24 C26 C27 111.0(2) . . ? N24 C26 C25 120.3(2) . . ? C27 C26 C25 128.7(3) . . ? C28 C27 C26 106.1(2) . . ? C28 C27 H27 127 . . ? C26 C27 H27 127 . . ? N23 C28 C27 106.0(2) . . ? N23 C28 C29 121.9(2) . . ? C27 C28 C29 132.1(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29 H29D 109.5 . . ? H29A C29 H29D 141.1 . . ? H29B C29 H29D 56.3 . . ? H29C C29 H29D 56.3 . . ? C28 C29 H29E 109.5 . . ? H29A C29 H29E 56.3 . . ? H29B C29 H29E 141.1 . . ? H29C C29 H29E 56.3 . . ? H29D C29 H29E 109.5 . . ? C28 C29 H29F 109.5 . . ? H29A C29 H29F 56.3 . . ? H29B C29 H29F 56.3 . . ? H29C C29 H29F 141.1 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? C31 O31 Zn1 124.89(13) . . ? O31 C31 C32 120.5(2) . . ? O31 C31 C34 121.68(19) . . ? C32 C31 C34 117.77(19) . . ? C39 C32 C31 121.3(2) . . ? C39 C32 C33 117.66(19) . . ? C31 C32 C33 121.02(19) . . ? N21 C33 C32 113.82(17) . . ? N21 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? N21 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C36 C34 C31 118.4(2) . . ? C36 C34 C35 120.5(2) . . ? C31 C34 C35 121.03(19) . . ? C35C C35 C35B 107.50(19) . . ? C35C C35 C34 112.67(18) . . ? C35B C35 C34 109.15(18) . . ? C35C C35 C35A 107.3(2) . . ? C35B C35 C35A 109.69(19) . . ? C34 C35 C35A 110.50(18) . . ? C35 C35A H35A 109.5 . . ? C35 C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C35 C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C35 C35B H35D 109.5 . . ? C35 C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C35 C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C35 C35C H35G 109.5 . . ? C35 C35C H35H 109.5 . . ? H35G C35C H35H 109.5 . . ? C35 C35C H35I 109.5 . . ? H35G C35C H35I 109.5 . . ? H35H C35C H35I 109.5 . . ? C34 C36 C37 124.0(2) . . ? C34 C36 H36 118 . . ? C37 C36 H36 118 . . ? C39 C37 C36 116.6(2) . . ? C39 C37 C38 122.5(2) . . ? C36 C37 C38 120.8(2) . . ? C38A C38 C38B 109.7(2) . . ? C38A C38 C38C 108.9(2) . . ? C38B C38 C38C 107.7(2) . . ? C38A C38 C37 110.20(18) . . ? C38B C38 C37 108.40(18) . . ? C38C C38 C37 111.9(2) . . ? C38 C38A H38A 109.5 . . ? C38 C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C38 C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? C38 C38B H38D 109.5 . . ? C38 C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C38 C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C38 C38C H38G 109.5 . . ? C38 C38C H38H 109.5 . . ? H38G C38C H38H 109.5 . . ? C38 C38C H38I 109.5 . . ? H38G C38C H38I 109.5 . . ? H38H C38C H38I 109.5 . . ? C37 C39 C32 121.8(2) . . ? C37 C39 H39 119.1 . . ? C32 C39 H39 119.1 . . ? 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 O31 Zn1 N1 Si2 -172.47(9) . . . . ? N11 Zn1 N1 Si2 -36.98(14) . . . . ? N21 Zn1 N1 Si2 71.84(13) . . . . ? O31 Zn1 N1 Si1 13.00(14) . . . . ? N11 Zn1 N1 Si1 148.48(9) . . . . ? N21 Zn1 N1 Si1 -102.70(10) . . . . ? Si2 N1 Si1 C1B 131.07(14) . . . . ? Zn1 N1 Si1 C1B -54.49(14) . . . . ? Si2 N1 Si1 C1C 9.34(18) . . . . ? Zn1 N1 Si1 C1C -176.22(11) . . . . ? Si2 N1 Si1 C1A -111.12(17) . . . . ? Zn1 N1 Si1 C1A 63.32(16) . . . . ? Si1 N1 Si2 C2A 64.20(16) . . . . ? Zn1 N1 Si2 C2A -109.74(13) . . . . ? Si1 N1 Si2 C2B -57.70(16) . . . . ? Zn1 N1 Si2 C2B 128.36(13) . . . . ? Si1 N1 Si2 C2C -175.78(12) . . . . ? Zn1 N1 Si2 C2C 10.28(16) . . . . ? N1 Zn1 N11 C12 -54.0(2) . . . . ? O31 Zn1 N11 C12 86.72(19) . . . . ? N21 Zn1 N11 C12 -176.06(19) . . . . ? N1 Zn1 N11 N12 114.98(17) . . . . ? O31 Zn1 N11 N12 -104.29(17) . . . . ? N21 Zn1 N11 N12 -7.07(18) . . . . ? C12 N11 N12 C14 0.0(2) . . . . ? Zn1 N11 N12 C14 -170.80(15) . . . . ? C12 N11 N12 C16 173.9(2) . . . . ? Zn1 N11 N12 C16 3.1(3) . . . . ? N12 N11 C12 C13 0.1(3) . . . . ? Zn1 N11 C12 C13 170.96(16) . . . . ? N12 N11 C12 C11 -177.7(2) . . . . ? Zn1 N11 C12 C11 -6.9(3) . . . . ? N11 C12 C13 C14 -0.2(3) . . . . ? C11 C12 C13 C14 177.4(2) . . . . ? N11 N12 C14 C13 -0.2(3) . . . . ? C16 N12 C14 C13 -173.9(2) . . . . ? N11 N12 C14 C15 179.0(2) . . . . ? C16 N12 C14 C15 5.3(4) . . . . ? C12 C13 C14 N12 0.3(3) . . . . ? C12 C13 C14 C15 -178.9(3) . . . . ? C14 N12 C16 C17 -153.1(2) . . . . ? N11 N12 C16 C17 33.9(3) . . . . ? N12 C16 C17 N21 -73.8(3) . . . . ? C16 C17 N21 C21 -58.4(2) . . . . ? C16 C17 N21 C33 178.21(18) . . . . ? C16 C17 N21 Zn1 64.5(2) . . . . ? N1 Zn1 N21 C21 -19.41(15) . . . . ? O31 Zn1 N21 C21 -148.62(12) . . . . ? N11 Zn1 N21 C21 102.26(13) . . . . ? N1 Zn1 N21 C17 -145.44(13) . . . . ? O31 Zn1 N21 C17 85.35(14) . . . . ? N11 Zn1 N21 C17 -23.77(14) . . . . ? N1 Zn1 N21 C33 97.54(13) . . . . ? O31 Zn1 N21 C33 -31.67(13) . . . . ? N11 Zn1 N21 C33 -140.79(13) . . . . ? C17 N21 C21 C22 -54.7(2) . . . . ? C33 N21 C21 C22 68.3(2) . . . . ? Zn1 N21 C21 C22 -178.46(14) . . . . ? N21 C21 C22 N23 172.28(16) . . . . ? C21 C22 N23 C28 91.6(3) . . . . ? C21 C22 N23 N24 -76.8(2) . . . . ? C28 N23 N24 C26 1.8(2) . . . . ? C22 N23 N24 C26 172.08(18) . . . . ? N23 N24 C26 C27 -0.7(3) . . . . ? N23 N24 C26 C25 178.4(2) . . . . ? N24 C26 C27 C28 -0.5(3) . . . . ? C25 C26 C27 C28 -179.6(2) . . . . ? N24 N23 C28 C27 -2.2(3) . . . . ? C22 N23 C28 C27 -171.2(2) . . . . ? N24 N23 C28 C29 176.7(2) . . . . ? C22 N23 C28 C29 7.7(4) . . . . ? C26 C27 C28 N23 1.6(3) . . . . ? C26 C27 C28 C29 -177.1(3) . . . . ? N1 Zn1 O31 C31 -141.79(15) . . . . ? N11 Zn1 O31 C31 79.82(16) . . . . ? N21 Zn1 O31 C31 -15.82(16) . . . . ? Zn1 O31 C31 C32 35.2(2) . . . . ? Zn1 O31 C31 C34 -145.94(15) . . . . ? O31 C31 C32 C39 176.68(17) . . . . ? C34 C31 C32 C39 -2.2(3) . . . . ? O31 C31 C32 C33 -1.2(3) . . . . ? C34 C31 C32 C33 179.99(17) . . . . ? C21 N21 C33 C32 -176.49(16) . . . . ? C17 N21 C33 C32 -50.5(2) . . . . ? Zn1 N21 C33 C32 67.28(18) . . . . ? C39 C32 C33 N21 123.44(19) . . . . ? C31 C32 C33 N21 -58.7(2) . . . . ? O31 C31 C34 C36 -175.72(17) . . . . ? C32 C31 C34 C36 3.1(3) . . . . ? O31 C31 C34 C35 1.9(3) . . . . ? C32 C31 C34 C35 -179.26(17) . . . . ? C36 C34 C35 C35C -6.4(3) . . . . ? C31 C34 C35 C35C 176.03(19) . . . . ? C36 C34 C35 C35B 112.9(2) . . . . ? C31 C34 C35 C35B -64.6(2) . . . . ? C36 C34 C35 C35A -126.4(2) . . . . ? C31 C34 C35 C35A 56.1(3) . . . . ? C31 C34 C36 C37 -1.4(3) . . . . ? C35 C34 C36 C37 -179.03(18) . . . . ? C34 C36 C37 C39 -1.4(3) . . . . ? C34 C36 C37 C38 175.35(18) . . . . ? C39 C37 C38 C38A -130.5(2) . . . . ? C36 C37 C38 C38A 52.9(3) . . . . ? C39 C37 C38 C38B 109.5(2) . . . . ? C36 C37 C38 C38B -67.1(3) . . . . ? C39 C37 C38 C38C -9.1(3) . . . . ? C36 C37 C38 C38C 174.3(2) . . . . ? C36 C37 C39 C32 2.5(3) . . . . ? C38 C37 C39 C32 -174.24(18) . . . . ? C31 C32 C39 C37 -0.7(3) . . . . ? C33 C32 C39 C37 177.19(18) . . . . ? # Attachment 'complex5_Jiang6.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-08-26 at 17:19:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : f:\progs\wingx\files\archive.dat # CIF files read : sq_renum sq struct data_sq_renum _database_code_depnum_ccdc_archive 'CCDC 672303' _audit_creation_date 2008-08-26T17:19:49-00:00 _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 'C30 H40 N2 O Zn' _chemical_formula_sum 'C30 H40 N2 O Zn' _chemical_formula_weight 510.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # 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 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9651(2) _cell_length_b 17.5917(2) _cell_length_c 21.1494(3) _cell_angle_alpha 76.8990(10) _cell_angle_beta 79.3830(10) _cell_angle_gamma 67.2880(10) _cell_volume 4641.00(11) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8539 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.16 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.815 _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 0.783 _exptl_absorpt_correction_T_max 0.976 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.018 0.000 0.000 734 25 ' ' 2 0.111 0.714 0.407 7 1 ' ' 3 0.180 0.679 0.574 7 1 ' ' 4 0.250 0.185 0.465 25 1 ' ' 5 0.750 0.815 0.535 25 2 ' ' 6 0.819 0.321 0.426 7 1 ' ' 7 0.889 0.286 0.593 7 0 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_unetI/netI 0.1476 _diffrn_reflns_number 62706 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.65 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 18987 _reflns_number_gt 10056 _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^)+(0.1614P)^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 18987 _refine_ls_number_parameters 940 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.2911 _refine_ls_wR_factor_gt 0.2698 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.244 _refine_diff_density_min -1.351 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.16559(6) -0.60731(5) 0.69210(4) 0.0267(2) Uani 1 d . . . C1 C 0.1352(5) -0.7055(4) 0.6830(3) 0.0313(16) Uani 1 d . . . H1A H 0.192 -0.7573 0.6993 0.038 Uiso 1 calc R . . H1B H 0.0696 -0.7053 0.7105 0.038 Uiso 1 calc R . . C2 C 0.1246(6) -0.7063(5) 0.6135(4) 0.044(2) Uani 1 d . . . H2A H 0.0721 -0.6533 0.5959 0.065 Uiso 1 calc R . . H2B H 0.1028 -0.7527 0.6125 0.065 Uiso 1 calc R . . H2C H 0.1919 -0.7135 0.587 0.065 Uiso 1 calc R . . N11 N 0.0928(4) -0.4980(3) 0.6236(3) 0.0274(13) Uani 1 d . . . C12 C 0.0268(5) -0.4327(4) 0.6510(3) 0.0273(15) Uani 1 d . . . C13 C -0.0253(5) -0.3556(4) 0.6144(3) 0.0292(16) Uani 1 d . . . H13 H -0.0699 -0.3094 0.6348 0.035 Uiso 1 calc R . . C14 C -0.0095(6) -0.3490(5) 0.5475(4) 0.0373(18) Uani 1 d . . . H14 H -0.0448 -0.2977 0.521 0.045 Uiso 1 calc R . . C15 C 0.0582(6) -0.4173(5) 0.5179(4) 0.0373(18) Uani 1 d . . . H15 H 0.0694 -0.4136 0.4718 0.045 Uiso 1 calc R . . C16 C 0.1074(5) -0.4894(5) 0.5588(3) 0.0316(16) Uani 1 d . . . H16 H 0.1547 -0.536 0.5398 0.038 Uiso 1 calc R . . C17 C 0.0071(5) -0.4485(4) 0.7251(3) 0.0287(16) Uani 1 d . . . H17A H -0.009 -0.396 0.7415 0.034 Uiso 1 calc R . . H17B H -0.0543 -0.4657 0.7384 0.034 Uiso 1 calc R . . N21 N 0.0980(4) -0.5140(4) 0.7551(3) 0.0279(13) Uani 1 d . . . C22 C 0.0652(5) -0.5364(4) 0.8264(3) 0.0272(15) Uani 1 d . . . H22A H 0.0366 -0.485 0.846 0.033 Uiso 1 calc R . . H22B H 0.1276 -0.5749 0.8481 0.033 Uiso 1 calc R . . C23 C -0.0161(6) -0.5776(4) 0.8398(3) 0.0306(16) Uani 1 d . . . C24 C 0.0156(6) -0.6618(5) 0.8371(3) 0.0368(18) Uani 1 d . . . H24 H 0.0868 -0.6925 0.8247 0.044 Uiso 1 calc R . . C25 C -0.0566(7) -0.7013(6) 0.8525(4) 0.049(2) Uani 1 d . . . H25 H -0.0349 -0.7588 0.8498 0.058 Uiso 1 calc R . . C26 C -0.1606(7) -0.6573(6) 0.8719(4) 0.052(2) Uani 1 d . . . H26 H -0.2099 -0.6845 0.8822 0.063 Uiso 1 calc R . . C27 C -0.1908(7) -0.5759(6) 0.8758(4) 0.053(2) Uani 1 d . . . H27 H -0.2618 -0.546 0.8893 0.064 Uiso 1 calc R . . C28 C -0.1191(6) -0.5339(6) 0.8602(4) 0.043(2) Uani 1 d . . . H28 H -0.1412 -0.4765 0.8637 0.052 Uiso 1 calc R . . O31 O 0.3087(3) -0.6127(3) 0.6906(2) 0.0265(10) Uani 1 d . . . C32 C 0.3377(5) -0.6093(4) 0.7461(3) 0.0239(15) Uani 1 d . . . C33 C 0.2799(5) -0.5417(4) 0.7778(3) 0.0257(15) Uani 1 d . . . C34 C 0.3103(5) -0.5293(4) 0.8324(3) 0.0300(16) Uani 1 d . . . H34 H 0.2709 -0.4807 0.8511 0.036 Uiso 1 calc R . . C35 C 0.4011(5) -0.5899(5) 0.8603(3) 0.0290(16) Uani 1 d . . . C36 C 0.4363(5) -0.5750(5) 0.9201(3) 0.0319(16) Uani 1 d . . . C37 C 0.3600(8) -0.5797(8) 0.9769(5) 0.077(3) Uani 1 d . . . H37A H 0.3434 -0.6299 0.9806 0.116 Uiso 1 calc R . . H37B H 0.2963 -0.5299 0.9717 0.116 Uiso 1 calc R . . H37C H 0.3893 -0.5824 1.0164 0.116 Uiso 1 calc R . . C38 C 0.4499(11) -0.4898(7) 0.9061(5) 0.087(4) Uani 1 d . . . H38A H 0.3821 -0.4449 0.8995 0.131 Uiso 1 calc R . . H38B H 0.4987 -0.4867 0.8667 0.131 Uiso 1 calc R . . H38C H 0.4775 -0.4836 0.9432 0.131 Uiso 1 calc R . . C39 C 0.5442(8) -0.6372(8) 0.9339(6) 0.090(4) Uani 1 d . . . H39A H 0.5683 -0.6218 0.9681 0.136 Uiso 1 calc R . . H39B H 0.5927 -0.6368 0.894 0.136 Uiso 1 calc R . . H39C H 0.5412 -0.6934 0.9485 0.136 Uiso 1 calc R . . C40 C 0.4547(5) -0.6562(4) 0.8298(3) 0.0301(17) Uani 1 d . . . H40 H 0.5154 -0.6969 0.8478 0.036 Uiso 1 calc R . . C41 C 0.4278(5) -0.6698(4) 0.7732(3) 0.0307(16) Uani 1 d . . . C42 C 0.4938(5) -0.7476(4) 0.7433(3) 0.0260(15) Uani 1 d . . . C43 C 0.5462(6) -0.7203(5) 0.6765(3) 0.0376(18) Uani 1 d . . . H43A H 0.4925 -0.6826 0.6482 0.056 Uiso 1 calc R . . H43B H 0.5889 -0.7696 0.6565 0.056 Uiso 1 calc R . . H43C H 0.5906 -0.6911 0.6819 0.056 Uiso 1 calc R . . C44 C 0.5813(6) -0.8094(4) 0.7855(4) 0.0362(18) Uani 1 d . . . H44A H 0.6238 -0.78 0.7935 0.054 Uiso 1 calc R . . H44B H 0.6256 -0.8555 0.7625 0.054 Uiso 1 calc R . . H44C H 0.5499 -0.8316 0.8273 0.054 Uiso 1 calc R . . C45 C 0.4274(6) -0.7964(5) 0.7344(4) 0.0381(18) Uani 1 d . . . H45A H 0.39 -0.8109 0.7765 0.057 Uiso 1 calc R . . H45B H 0.4732 -0.8477 0.7178 0.057 Uiso 1 calc R . . H45C H 0.3771 -0.7617 0.7032 0.057 Uiso 1 calc R . . C46 C 0.1820(5) -0.4763(4) 0.7497(3) 0.0269(15) Uani 1 d . . . H46A H 0.1996 -0.4549 0.7033 0.032 Uiso 1 calc R . . H46B H 0.1548 -0.4287 0.7738 0.032 Uiso 1 calc R . . Zn2 Zn -0.13961(6) -0.08243(5) 0.65511(4) 0.0277(2) Uani 1 d . . . C101 C -0.2632(5) 0.0215(4) 0.6538(4) 0.0324(17) Uani 1 d . . . H10A H -0.3064 0.0191 0.6964 0.039 Uiso 1 calc R . . H10B H -0.24 0.0694 0.6483 0.039 Uiso 1 calc R . . C102 C -0.3309(7) 0.0369(5) 0.5991(5) 0.057(2) Uani 1 d . . . H10C H -0.2903 0.0438 0.5566 0.085 Uiso 1 calc R . . H10D H -0.3928 0.0877 0.6025 0.085 Uiso 1 calc R . . H10E H -0.3525 -0.011 0.6035 0.085 Uiso 1 calc R . . N111 N -0.0417(4) -0.1051(3) 0.5667(3) 0.0294(13) Uani 1 d . . . C112 C 0.0596(5) -0.1175(4) 0.5694(3) 0.0253(15) Uani 1 d . . . C113 C 0.1349(6) -0.1400(4) 0.5188(3) 0.0318(16) Uani 1 d . . . H113 H 0.2062 -0.1517 0.5225 0.038 Uiso 1 calc R . . C114 C 0.1041(6) -0.1454(5) 0.4613(4) 0.0381(18) Uani 1 d . . . H114 H 0.1542 -0.1594 0.4248 0.046 Uiso 1 calc R . . C115 C 0.0016(6) -0.1303(5) 0.4578(4) 0.0370(18) Uani 1 d . . . H115 H -0.0204 -0.1336 0.4189 0.044 Uiso 1 calc R . . C116 C -0.0691(5) -0.1103(4) 0.5111(3) 0.0281(16) Uani 1 d . . . H116 H -0.1404 -0.0997 0.5085 0.034 Uiso 1 calc R . . C117 C 0.0846(5) -0.1034(4) 0.6299(3) 0.0297(16) Uani 1 d . . . H11A H 0.0781 -0.0443 0.6246 0.036 Uiso 1 calc R . . H11B H 0.1578 -0.1391 0.637 0.036 Uiso 1 calc R . . N121 N 0.0146(4) -0.1226(3) 0.6881(3) 0.0233(12) Uani 1 d . . . C122 C 0.0268(6) -0.0903(4) 0.7452(3) 0.0309(16) Uani 1 d . . . H12A H -0.0188 -0.1055 0.7836 0.037 Uiso 1 calc R . . H12B H 0.0998 -0.1185 0.7558 0.037 Uiso 1 calc R . . C123 C 0.0008(5) 0.0020(4) 0.7339(3) 0.0263(15) Uani 1 d . . . C124 C -0.1004(5) 0.0587(4) 0.7330(4) 0.0339(17) Uani 1 d . . . H124 H -0.1564 0.0389 0.7398 0.041 Uiso 1 calc R . . C125 C -0.1217(6) 0.1436(5) 0.7225(4) 0.0369(18) Uani 1 d . . . H125 H -0.1919 0.1815 0.7216 0.044 Uiso 1 calc R . . C126 C -0.0407(6) 0.1746(4) 0.7131(4) 0.0350(17) Uani 1 d . . . H126 H -0.0557 0.2331 0.7057 0.042 Uiso 1 calc R . . C127 C 0.0616(5) 0.1189(4) 0.7148(3) 0.0322(17) Uani 1 d . . . H127 H 0.1171 0.1391 0.7091 0.039 Uiso 1 calc R . . C128 C 0.0825(5) 0.0335(4) 0.7247(3) 0.0295(16) Uani 1 d . . . H128 H 0.1527 -0.0043 0.7254 0.035 Uiso 1 calc R . . O131 O -0.1557(3) -0.1918(3) 0.6878(2) 0.0272(10) Uani 1 d . . . C132 C -0.1266(5) -0.2299(4) 0.7488(3) 0.0255(15) Uani 1 d . . . C133 C -0.0256(5) -0.2428(4) 0.7613(3) 0.0234(14) Uani 1 d . . . C134 C 0.0055(5) -0.2789(4) 0.8236(3) 0.0270(15) Uani 1 d . . . H134 H 0.074 -0.2871 0.8314 0.032 Uiso 1 calc R . . C135 C -0.0593(6) -0.3025(4) 0.8735(3) 0.0332(17) Uani 1 d . . . C136 C -0.0258(6) -0.3334(5) 0.9426(3) 0.0348(17) Uani 1 d . . . C137 C -0.0303(8) -0.2562(5) 0.9695(4) 0.054(2) Uani 1 d . . . H13A H -0.0045 -0.2749 1.0125 0.081 Uiso 1 calc R . . H13B H -0.1027 -0.2169 0.9733 0.081 Uiso 1 calc R . . H13C H 0.0133 -0.2284 0.9394 0.081 Uiso 1 calc R . . C138 C 0.0856(6) -0.3963(5) 0.9456(4) 0.0429(19) Uani 1 d . . . H13D H 0.0958 -0.4409 0.9216 0.064 Uiso 1 calc R . . H13E H 0.0978 -0.4205 0.9913 0.064 Uiso 1 calc R . . H13F H 0.1349 -0.368 0.9259 0.064 Uiso 1 calc R . . C139 C -0.0948(7) -0.3767(5) 0.9892(4) 0.047(2) Uani 1 d . . . H13G H -0.0957 -0.4226 0.9707 0.071 Uiso 1 calc R . . H13H H -0.166 -0.3361 0.9951 0.071 Uiso 1 calc R . . H13I H -0.0667 -0.3989 1.0315 0.071 Uiso 1 calc R . . C140 C -0.1561(5) -0.2937(4) 0.8584(3) 0.0299(16) Uani 1 d . . . H140 H -0.2008 -0.3125 0.8925 0.036 Uiso 1 calc R . . C141 C -0.1935(5) -0.2595(4) 0.7972(3) 0.0278(15) Uani 1 d . . . C142 C -0.3023(5) -0.2500(4) 0.7855(3) 0.0314(17) Uani 1 d . . . C143 C -0.3565(6) -0.2952(6) 0.8442(4) 0.047(2) Uani 1 d . . . H14A H -0.4245 -0.2898 0.8336 0.07 Uiso 1 calc R . . H14B H -0.3666 -0.2696 0.8828 0.07 Uiso 1 calc R . . H14C H -0.3126 -0.3545 0.8534 0.07 Uiso 1 calc R . . C144 C -0.2971(6) -0.2891(5) 0.7277(4) 0.0399(19) Uani 1 d . . . H14D H -0.2649 -0.2621 0.6887 0.06 Uiso 1 calc R . . H14E H -0.3678 -0.2816 0.7207 0.06 Uiso 1 calc R . . H14F H -0.2552 -0.3489 0.7364 0.06 Uiso 1 calc R . . C145 C -0.3722(6) -0.1547(5) 0.7718(4) 0.0421(19) Uani 1 d . . . H14G H -0.3432 -0.1274 0.7315 0.063 Uiso 1 calc R . . H14H H -0.3737 -0.1283 0.8083 0.063 Uiso 1 calc R . . H14I H -0.4433 -0.149 0.7672 0.063 Uiso 1 calc R . . C146 C 0.0468(5) -0.2157(4) 0.7065(3) 0.0254(15) Uani 1 d . . . H14J H 0.1183 -0.2391 0.7199 0.031 Uiso 1 calc R . . H14K H 0.0487 -0.2392 0.6677 0.031 Uiso 1 calc R . . Zn3 Zn 0.48128(6) -0.30359(5) 0.57560(4) 0.0278(2) Uani 1 d . . . C201 C 0.6082(6) -0.2955(5) 0.5206(4) 0.0404(19) Uani 1 d . . . H20A H 0.6481 -0.2784 0.5452 0.048 Uiso 1 calc R . . H20B H 0.653 -0.351 0.5093 0.048 Uiso 1 calc R . . C202 C 0.5806(7) -0.2321(6) 0.4580(4) 0.061(3) Uani 1 d . . . H20C H 0.54 -0.2484 0.4341 0.091 Uiso 1 calc R . . H20D H 0.6449 -0.2305 0.4308 0.091 Uiso 1 calc R . . H20E H 0.5393 -0.1766 0.4691 0.091 Uiso 1 calc R . . N211 N 0.4004(4) -0.3622(3) 0.5384(3) 0.0285(13) Uani 1 d . . . C212 C 0.3982(5) -0.4346(4) 0.5749(3) 0.0244(15) Uani 1 d . . . C213 C 0.3647(5) -0.4877(4) 0.5535(4) 0.0313(16) Uani 1 d . . . H213 H 0.364 -0.5387 0.5804 0.038 Uiso 1 calc R . . C214 C 0.3319(6) -0.4647(5) 0.4913(4) 0.0367(18) Uani 1 d . . . H214 H 0.3123 -0.5014 0.4741 0.044 Uiso 1 calc R . . C215 C 0.3283(5) -0.3863(5) 0.4540(3) 0.0365(18) Uani 1 d . . . H215 H 0.3018 -0.3675 0.4127 0.044 Uiso 1 calc R . . C216 C 0.3640(6) -0.3381(5) 0.4792(4) 0.0352(17) Uani 1 d . . . H216 H 0.3631 -0.2857 0.4541 0.042 Uiso 1 calc R . . C217 C 0.4437(5) -0.4603(4) 0.6393(3) 0.0252(15) Uani 1 d . . . H21A H 0.4001 -0.4859 0.6726 0.03 Uiso 1 calc R . . H21B H 0.5147 -0.503 0.6346 0.03 Uiso 1 calc R . . N221 N 0.4493(4) -0.3880(3) 0.6618(2) 0.0227(12) Uani 1 d . . . C222 C 0.5168(5) -0.4198(4) 0.7172(3) 0.0270(15) Uani 1 d . . . H22C H 0.5201 -0.3714 0.7319 0.032 Uiso 1 calc R . . H22D H 0.4834 -0.4499 0.7544 0.032 Uiso 1 calc R . . C223 C 0.6257(5) -0.4770(4) 0.7001(3) 0.0308(16) Uani 1 d . . . C224 C 0.6974(5) -0.4458(4) 0.6577(3) 0.0295(16) Uani 1 d . . . H224 H 0.6745 -0.3886 0.6374 0.035 Uiso 1 calc R . . C225 C 0.8014(5) -0.4967(4) 0.6447(3) 0.0315(16) Uani 1 d . . . H225 H 0.8488 -0.4746 0.616 0.038 Uiso 1 calc R . . C226 C 0.8351(6) -0.5807(5) 0.6746(4) 0.0390(18) Uani 1 d . . . H226 H 0.9058 -0.6161 0.6669 0.047 Uiso 1 calc R . . C227 C 0.7650(6) -0.6113(5) 0.7149(4) 0.0409(19) Uani 1 d . . . H227 H 0.7882 -0.6685 0.7349 0.049 Uiso 1 calc R . . C228 C 0.6610(5) -0.5617(4) 0.7276(3) 0.0315(16) Uani 1 d . . . H228 H 0.614 -0.5853 0.755 0.038 Uiso 1 calc R . . O231 O 0.3730(3) -0.2037(3) 0.6013(2) 0.0272(11) Uani 1 d . . . C232 C 0.3575(5) -0.1962(4) 0.6633(4) 0.0286(16) Uani 1 d . . . C233 C 0.3383(5) -0.2622(4) 0.7111(3) 0.0254(15) Uani 1 d . . . C234 C 0.3185(5) -0.2563(4) 0.7777(4) 0.0312(17) Uani 1 d . . . H234 H 0.3063 -0.301 0.8085 0.037 Uiso 1 calc R . . C235 C 0.3161(5) -0.1878(5) 0.7997(3) 0.0316(17) Uani 1 d . . . C236 C 0.2867(5) -0.1764(5) 0.8718(4) 0.0352(17) Uani 1 d . . . C237 C 0.2962(9) -0.2589(6) 0.9157(4) 0.068(3) Uani 1 d . . . H23A H 0.2904 -0.2527 0.9613 0.101 Uiso 1 calc R . . H23B H 0.3641 -0.3011 0.9045 0.101 Uiso 1 calc R . . H23C H 0.2403 -0.2766 0.9099 0.101 Uiso 1 calc R . . C238 C 0.1747(6) -0.1182(6) 0.8804(4) 0.049(2) Uani 1 d . . . H23D H 0.129 -0.1438 0.8709 0.073 Uiso 1 calc R . . H23E H 0.1658 -0.0652 0.8503 0.073 Uiso 1 calc R . . H23F H 0.1564 -0.1078 0.9254 0.073 Uiso 1 calc R . . C239 C 0.3579(7) -0.1433(6) 0.8935(4) 0.054(2) Uani 1 d . . . H23G H 0.3483 -0.1493 0.9412 0.081 Uiso 1 calc R . . H23H H 0.3411 -0.0841 0.8742 0.081 Uiso 1 calc R . . H23I H 0.4307 -0.1751 0.8792 0.081 Uiso 1 calc R . . C240 C 0.3378(5) -0.1248(4) 0.7520(3) 0.0301(16) Uani 1 d . . . H240 H 0.3393 -0.0781 0.7667 0.036 Uiso 1 calc R . . C241 C 0.3569(5) -0.1254(4) 0.6861(3) 0.0259(15) Uani 1 d . . . C242 C 0.3826(5) -0.0539(4) 0.6360(4) 0.0330(17) Uani 1 d . . . C243 C 0.3029(6) -0.0156(5) 0.5860(4) 0.0377(18) Uani 1 d . . . H24A H 0.2334 0.0107 0.6082 0.057 Uiso 1 calc R . . H24B H 0.3024 -0.0596 0.5649 0.057 Uiso 1 calc R . . H24C H 0.322 0.0266 0.553 0.057 Uiso 1 calc R . . C244 C 0.3820(6) 0.0149(5) 0.6674(4) 0.0397(18) Uani 1 d . . . H24D H 0.4015 0.0565 0.6339 0.06 Uiso 1 calc R . . H24E H 0.4321 -0.0086 0.7 0.06 Uiso 1 calc R . . H24F H 0.3119 0.0416 0.6887 0.06 Uiso 1 calc R . . C245 C 0.4932(6) -0.0911(5) 0.5996(4) 0.0384(18) Uani 1 d . . . H24G H 0.5114 -0.046 0.5698 0.058 Uiso 1 calc R . . H24H H 0.4936 -0.1319 0.5747 0.058 Uiso 1 calc R . . H24I H 0.5443 -0.1188 0.6315 0.058 Uiso 1 calc R . . C246 C 0.3421(5) -0.3375(4) 0.6889(3) 0.0272(15) Uani 1 d . . . H24J H 0.294 -0.3199 0.6549 0.033 Uiso 1 calc R . . H24K H 0.3171 -0.3731 0.7261 0.033 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 0.0316(4) 0.0201(4) 0.0331(5) 0.0067(3) -0.0145(3) -0.0159(3) C1 0.030(4) 0.027(4) 0.038(4) -0.003(3) -0.016(3) -0.008(3) C2 0.048(5) 0.042(5) 0.054(5) -0.014(4) 0.000(4) -0.029(4) N11 0.024(3) 0.024(3) 0.034(4) -0.001(3) -0.010(2) -0.008(2) C12 0.026(3) 0.027(4) 0.036(4) 0.000(3) -0.013(3) -0.016(3) C13 0.030(4) 0.024(4) 0.036(4) 0.003(3) -0.014(3) -0.013(3) C14 0.046(4) 0.030(4) 0.035(5) 0.008(3) -0.011(3) -0.017(4) C15 0.057(5) 0.031(4) 0.029(4) 0.008(3) -0.015(4) -0.023(4) C16 0.035(4) 0.030(4) 0.032(4) 0.002(3) -0.013(3) -0.013(3) C17 0.027(3) 0.025(4) 0.030(4) 0.006(3) -0.010(3) -0.008(3) N21 0.029(3) 0.035(3) 0.030(3) -0.001(3) -0.011(2) -0.021(3) C22 0.029(3) 0.027(4) 0.027(4) 0.001(3) -0.011(3) -0.012(3) C23 0.039(4) 0.029(4) 0.026(4) 0.002(3) -0.004(3) -0.018(3) C24 0.035(4) 0.044(5) 0.034(4) 0.003(4) -0.010(3) -0.020(4) C25 0.053(5) 0.051(5) 0.050(5) -0.002(4) -0.007(4) -0.031(4) C26 0.056(5) 0.082(7) 0.040(5) -0.003(5) -0.007(4) -0.051(5) C27 0.045(5) 0.070(7) 0.051(6) -0.005(5) -0.003(4) -0.030(5) C28 0.042(4) 0.053(5) 0.037(5) 0.000(4) -0.009(4) -0.022(4) O31 0.032(2) 0.026(3) 0.027(3) 0.003(2) -0.009(2) -0.018(2) C32 0.031(3) 0.020(4) 0.024(4) 0.005(3) -0.011(3) -0.015(3) C33 0.030(3) 0.022(4) 0.030(4) 0.007(3) -0.008(3) -0.019(3) C34 0.030(3) 0.031(4) 0.034(4) 0.004(3) -0.009(3) -0.019(3) C35 0.028(3) 0.038(4) 0.024(4) 0.004(3) -0.008(3) -0.018(3) C36 0.037(4) 0.034(4) 0.032(4) -0.002(3) -0.012(3) -0.019(3) C37 0.059(6) 0.133(11) 0.053(6) -0.023(6) -0.011(5) -0.045(7) C38 0.172(12) 0.073(7) 0.061(7) 0.018(6) -0.067(7) -0.084(8) C39 0.063(7) 0.113(10) 0.102(9) -0.048(8) -0.058(6) -0.001(6) C40 0.032(4) 0.028(4) 0.032(4) 0.013(3) -0.018(3) -0.017(3) C41 0.027(3) 0.030(4) 0.035(4) 0.009(3) -0.009(3) -0.016(3) C42 0.025(3) 0.023(4) 0.026(4) 0.007(3) -0.008(3) -0.008(3) C43 0.043(4) 0.030(4) 0.032(4) 0.004(3) 0.000(3) -0.011(3) C44 0.035(4) 0.027(4) 0.039(5) 0.003(3) -0.009(3) -0.005(3) C45 0.042(4) 0.023(4) 0.045(5) -0.003(3) -0.008(4) -0.008(3) C46 0.027(3) 0.022(4) 0.036(4) 0.003(3) -0.009(3) -0.015(3) Zn2 0.0288(4) 0.0215(4) 0.0330(5) 0.0059(3) -0.0103(3) -0.0122(3) C101 0.030(4) 0.023(4) 0.039(4) 0.009(3) -0.011(3) -0.009(3) C102 0.047(5) 0.041(5) 0.073(7) -0.012(5) -0.024(5) 0.003(4) N111 0.036(3) 0.019(3) 0.039(4) 0.004(3) -0.011(3) -0.017(3) C112 0.033(4) 0.018(3) 0.026(4) 0.012(3) -0.014(3) -0.016(3) C113 0.036(4) 0.029(4) 0.029(4) 0.007(3) -0.008(3) -0.015(3) C114 0.042(4) 0.032(4) 0.035(4) 0.006(3) -0.010(3) -0.011(3) C115 0.054(5) 0.032(4) 0.034(4) 0.004(3) -0.014(4) -0.027(4) C116 0.033(4) 0.028(4) 0.025(4) 0.002(3) -0.013(3) -0.012(3) C117 0.034(4) 0.027(4) 0.033(4) 0.009(3) -0.013(3) -0.019(3) N121 0.027(3) 0.015(3) 0.032(3) 0.005(2) -0.006(2) -0.016(2) C122 0.040(4) 0.020(4) 0.038(4) 0.003(3) -0.011(3) -0.019(3) C123 0.037(4) 0.021(4) 0.026(4) 0.003(3) -0.013(3) -0.016(3) C124 0.032(4) 0.021(4) 0.052(5) -0.005(3) -0.006(3) -0.013(3) C125 0.030(4) 0.032(4) 0.048(5) -0.015(4) 0.001(3) -0.009(3) C126 0.044(4) 0.020(4) 0.046(5) -0.002(3) -0.008(4) -0.017(3) C127 0.034(4) 0.020(4) 0.043(4) 0.006(3) -0.013(3) -0.013(3) C128 0.027(3) 0.014(3) 0.045(5) 0.001(3) -0.007(3) -0.008(3) O131 0.032(2) 0.024(3) 0.029(3) 0.006(2) -0.014(2) -0.014(2) C132 0.039(4) 0.013(3) 0.026(4) 0.005(3) -0.009(3) -0.012(3) C133 0.032(3) 0.016(3) 0.027(4) 0.006(3) -0.012(3) -0.014(3) C134 0.030(3) 0.024(4) 0.032(4) 0.005(3) -0.014(3) -0.015(3) C135 0.045(4) 0.023(4) 0.032(4) 0.005(3) -0.010(3) -0.016(3) C136 0.051(4) 0.032(4) 0.027(4) 0.008(3) -0.016(3) -0.022(4) C137 0.077(6) 0.050(6) 0.041(5) -0.001(4) -0.018(4) -0.028(5) C138 0.051(5) 0.036(5) 0.037(5) 0.006(4) -0.013(4) -0.014(4) C139 0.057(5) 0.052(5) 0.033(5) 0.019(4) -0.020(4) -0.028(4) C140 0.033(4) 0.022(4) 0.035(4) 0.003(3) -0.006(3) -0.014(3) C141 0.031(4) 0.028(4) 0.028(4) 0.003(3) -0.009(3) -0.017(3) C142 0.031(4) 0.030(4) 0.034(4) 0.008(3) -0.005(3) -0.018(3) C143 0.039(4) 0.059(6) 0.045(5) 0.001(4) -0.002(4) -0.028(4) C144 0.034(4) 0.044(5) 0.052(5) -0.003(4) -0.012(4) -0.024(4) C145 0.031(4) 0.054(5) 0.047(5) -0.012(4) -0.005(3) -0.020(4) C146 0.027(3) 0.013(3) 0.036(4) 0.007(3) -0.011(3) -0.010(3) Zn3 0.0291(4) 0.0255(4) 0.0309(5) 0.0046(3) -0.0081(3) -0.0152(3) C201 0.037(4) 0.041(5) 0.039(5) 0.004(4) -0.009(3) -0.013(4) C202 0.057(6) 0.077(7) 0.039(5) 0.012(5) -0.014(4) -0.021(5) N211 0.034(3) 0.026(3) 0.027(3) 0.006(3) -0.009(3) -0.016(3) C212 0.024(3) 0.023(4) 0.028(4) 0.003(3) -0.007(3) -0.012(3) C213 0.025(3) 0.028(4) 0.039(4) 0.002(3) -0.005(3) -0.012(3) C214 0.036(4) 0.043(5) 0.040(5) -0.006(4) -0.005(3) -0.024(4) C215 0.036(4) 0.054(5) 0.022(4) -0.002(4) -0.010(3) -0.018(4) C216 0.039(4) 0.033(4) 0.034(4) 0.003(3) -0.014(3) -0.014(3) C217 0.030(3) 0.020(3) 0.029(4) 0.007(3) -0.013(3) -0.015(3) N221 0.027(3) 0.021(3) 0.023(3) 0.005(2) -0.011(2) -0.013(2) C222 0.030(3) 0.022(4) 0.029(4) 0.004(3) -0.014(3) -0.009(3) C223 0.035(4) 0.031(4) 0.029(4) -0.001(3) -0.015(3) -0.011(3) C224 0.032(4) 0.023(4) 0.038(4) 0.001(3) -0.011(3) -0.016(3) C225 0.034(4) 0.030(4) 0.036(4) 0.001(3) -0.015(3) -0.015(3) C226 0.032(4) 0.035(4) 0.049(5) -0.007(4) -0.011(3) -0.008(3) C227 0.038(4) 0.029(4) 0.048(5) 0.002(4) -0.005(4) -0.007(3) C228 0.035(4) 0.018(4) 0.040(4) 0.009(3) -0.011(3) -0.011(3) O231 0.035(3) 0.032(3) 0.019(3) 0.007(2) -0.014(2) -0.019(2) C232 0.021(3) 0.019(4) 0.046(5) 0.007(3) -0.012(3) -0.011(3) C233 0.023(3) 0.026(4) 0.024(4) 0.006(3) -0.004(3) -0.010(3) C234 0.024(3) 0.028(4) 0.039(4) 0.008(3) -0.012(3) -0.011(3) C235 0.027(3) 0.036(4) 0.028(4) 0.005(3) -0.012(3) -0.010(3) C236 0.032(4) 0.034(4) 0.035(4) -0.003(3) -0.010(3) -0.008(3) C237 0.108(8) 0.050(6) 0.032(5) -0.002(4) -0.008(5) -0.017(6) C238 0.042(5) 0.066(6) 0.031(5) -0.015(4) -0.010(4) -0.006(4) C239 0.046(5) 0.086(7) 0.039(5) -0.021(5) -0.009(4) -0.025(5) C240 0.025(3) 0.030(4) 0.037(4) 0.000(3) -0.011(3) -0.011(3) C241 0.023(3) 0.024(4) 0.028(4) 0.001(3) -0.010(3) -0.006(3) C242 0.034(4) 0.024(4) 0.047(5) 0.001(3) -0.010(3) -0.018(3) C243 0.041(4) 0.027(4) 0.044(5) 0.009(3) -0.013(4) -0.016(3) C244 0.045(4) 0.033(4) 0.046(5) -0.001(4) -0.014(4) -0.018(4) C245 0.044(4) 0.041(5) 0.043(5) -0.007(4) 0.003(4) -0.032(4) C246 0.023(3) 0.025(4) 0.029(4) 0.009(3) -0.010(3) -0.009(3) #----------------------------------------------------------------------------# # 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 O31 1.959(4) . ? Zn1 C1 1.988(7) . ? Zn1 N11 2.146(5) . ? Zn1 N21 2.167(6) . ? C1 C2 1.507(10) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? N11 C16 1.328(9) . ? N11 C12 1.339(9) . ? C12 C13 1.392(9) . ? C12 C17 1.521(9) . ? C13 C14 1.377(10) . ? C13 H13 0.95 . ? C14 C15 1.405(11) . ? C14 H14 0.95 . ? C15 C16 1.371(10) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 N21 1.475(8) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? N21 C22 1.501(8) . ? N21 C46 1.532(7) . ? C22 C23 1.521(9) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C28 1.383(10) . ? C23 C24 1.385(10) . ? C24 C25 1.387(10) . ? C24 H24 0.95 . ? C25 C26 1.390(12) . ? C25 H25 0.95 . ? C26 C27 1.346(13) . ? C26 H26 0.95 . ? C27 C28 1.414(11) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? O31 C32 1.331(7) . ? C32 C33 1.389(9) . ? C32 C41 1.414(9) . ? C33 C34 1.388(9) . ? C33 C46 1.524(9) . ? C34 C35 1.428(9) . ? C34 H34 0.95 . ? C35 C40 1.350(10) . ? C35 C36 1.546(9) . ? C36 C37 1.462(12) . ? C36 C39 1.516(11) . ? C36 C38 1.538(11) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 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 C41 1.414(10) . ? C40 H40 0.95 . ? C41 C42 1.524(10) . ? C42 C43 1.532(9) . ? C42 C45 1.545(10) . ? C42 C44 1.553(9) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? Zn2 C101 1.970(7) . ? Zn2 O131 1.976(4) . ? Zn2 N111 2.122(6) . ? Zn2 N121 2.186(5) . ? C101 C102 1.539(11) . ? C101 H10A 0.99 . ? C101 H10B 0.99 . ? C102 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? N111 C116 1.333(8) . ? N111 C112 1.356(8) . ? C112 C113 1.367(10) . ? C112 C117 1.482(9) . ? C113 C114 1.394(10) . ? C113 H113 0.95 . ? C114 C115 1.365(10) . ? C114 H114 0.95 . ? C115 C116 1.368(10) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 N121 1.486(8) . ? C117 H11A 0.99 . ? C117 H11B 0.99 . ? N121 C146 1.499(8) . ? N121 C122 1.507(9) . ? C122 C123 1.491(9) . ? C122 H12A 0.99 . ? C122 H12B 0.99 . ? C123 C124 1.380(9) . ? C123 C128 1.417(9) . ? C124 C125 1.379(10) . ? C124 H124 0.95 . ? C125 C126 1.398(10) . ? C125 H125 0.95 . ? C126 C127 1.387(10) . ? C126 H126 0.95 . ? C127 C128 1.387(9) . ? C127 H127 0.95 . ? C128 H128 0.95 . ? O131 C132 1.366(7) . ? C132 C133 1.404(9) . ? C132 C141 1.406(9) . ? C133 C134 1.396(9) . ? C133 C146 1.511(9) . ? C134 C135 1.358(9) . ? C134 H134 0.95 . ? C135 C140 1.389(9) . ? C135 C136 1.533(10) . ? C136 C138 1.525(10) . ? C136 C139 1.535(10) . ? C136 C137 1.561(11) . ? C137 H13A 0.98 . ? C137 H13B 0.98 . ? C137 H13C 0.98 . ? C138 H13D 0.98 . ? C138 H13E 0.98 . ? C138 H13F 0.98 . ? C139 H13G 0.98 . ? C139 H13H 0.98 . ? C139 H13I 0.98 . ? C140 C141 1.401(9) . ? C140 H140 0.95 . ? C141 C142 1.525(9) . ? C142 C144 1.509(10) . ? C142 C143 1.555(10) . ? C142 C145 1.570(10) . ? C143 H14A 0.98 . ? C143 H14B 0.98 . ? C143 H14C 0.98 . ? C144 H14D 0.98 . ? C144 H14E 0.98 . ? C144 H14F 0.98 . ? C145 H14G 0.98 . ? C145 H14H 0.98 . ? C145 H14I 0.98 . ? C146 H14J 0.99 . ? C146 H14K 0.99 . ? Zn3 O231 1.935(5) . ? Zn3 C201 1.969(7) . ? Zn3 N211 2.134(6) . ? Zn3 N221 2.171(5) . ? C201 C202 1.527(11) . ? C201 H20A 0.99 . ? C201 H20B 0.99 . ? C202 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? N211 C212 1.339(8) . ? N211 C216 1.353(9) . ? C212 C213 1.382(9) . ? C212 C217 1.509(9) . ? C213 C214 1.393(10) . ? C213 H213 0.95 . ? C214 C215 1.412(10) . ? C214 H214 0.95 . ? C215 C216 1.372(10) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 N221 1.489(8) . ? C217 H21A 0.99 . ? C217 H21B 0.99 . ? N221 C246 1.498(8) . ? N221 C222 1.510(8) . ? C222 C223 1.495(9) . ? C222 H22C 0.99 . ? C222 H22D 0.99 . ? C223 C228 1.395(9) . ? C223 C224 1.408(9) . ? C224 C225 1.395(10) . ? C224 H224 0.95 . ? C225 C226 1.398(10) . ? C225 H225 0.95 . ? C226 C227 1.366(10) . ? C226 H226 0.95 . ? C227 C228 1.387(10) . ? C227 H227 0.95 . ? C228 H228 0.95 . ? O231 C232 1.319(8) . ? C232 C241 1.430(10) . ? C232 C233 1.432(9) . ? C233 C234 1.404(10) . ? C233 C246 1.481(10) . ? C234 C235 1.373(10) . ? C234 H234 0.95 . ? C235 C240 1.405(9) . ? C235 C236 1.544(10) . ? C236 C238 1.507(10) . ? C236 C237 1.507(11) . ? C236 C239 1.508(11) . ? C237 H23A 0.98 . ? C237 H23B 0.98 . ? C237 H23C 0.98 . ? C238 H23D 0.98 . ? C238 H23E 0.98 . ? C238 H23F 0.98 . ? C239 H23G 0.98 . ? C239 H23H 0.98 . ? C239 H23I 0.98 . ? C240 C241 1.373(9) . ? C240 H240 0.95 . ? C241 C242 1.561(9) . ? C242 C244 1.502(10) . ? C242 C243 1.530(10) . ? C242 C245 1.554(10) . ? C243 H24A 0.98 . ? C243 H24B 0.98 . ? C243 H24C 0.98 . ? C244 H24D 0.98 . ? C244 H24E 0.98 . ? C244 H24F 0.98 . ? C245 H24G 0.98 . ? C245 H24H 0.98 . ? C245 H24I 0.98 . ? C246 H24J 0.99 . ? C246 H24K 0.99 . ? 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 O31 Zn1 C1 121.8(2) . . ? O31 Zn1 N11 106.00(19) . . ? C1 Zn1 N11 112.3(2) . . ? O31 Zn1 N21 94.40(19) . . ? C1 Zn1 N21 134.1(3) . . ? N11 Zn1 N21 79.0(2) . . ? C2 C1 Zn1 112.9(5) . . ? C2 C1 H1A 109 . . ? Zn1 C1 H1A 109 . . ? C2 C1 H1B 109 . . ? Zn1 C1 H1B 109 . . ? H1A C1 H1B 107.8 . . ? 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 . . ? C16 N11 C12 118.8(6) . . ? C16 N11 Zn1 127.0(5) . . ? C12 N11 Zn1 114.3(4) . . ? N11 C12 C13 122.6(6) . . ? N11 C12 C17 116.2(6) . . ? C13 C12 C17 121.2(6) . . ? C14 C13 C12 117.3(7) . . ? C14 C13 H13 121.4 . . ? C12 C13 H13 121.4 . . ? C13 C14 C15 120.9(7) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 116.7(7) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? N11 C16 C15 123.8(7) . . ? N11 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? N21 C17 C12 111.9(5) . . ? N21 C17 H17A 109.2 . . ? C12 C17 H17A 109.2 . . ? N21 C17 H17B 109.2 . . ? C12 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 N21 C22 108.1(5) . . ? C17 N21 C46 107.8(5) . . ? C22 N21 C46 107.6(5) . . ? C17 N21 Zn1 106.9(4) . . ? C22 N21 Zn1 121.8(4) . . ? C46 N21 Zn1 103.9(4) . . ? N21 C22 C23 113.9(5) . . ? N21 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N21 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 119.8(7) . . ? C28 C23 C22 120.8(7) . . ? C24 C23 C22 119.2(6) . . ? C23 C24 C25 120.0(7) . . ? C23 C24 H24 120 . . ? C25 C24 H24 120 . . ? C24 C25 C26 120.5(8) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.4(8) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 121.4(8) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C23 C28 C27 118.9(8) . . ? C23 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C32 O31 Zn1 117.5(4) . . ? O31 C32 C33 119.1(6) . . ? O31 C32 C41 122.7(6) . . ? C33 C32 C41 118.2(6) . . ? C34 C33 C32 122.7(6) . . ? C34 C33 C46 118.4(6) . . ? C32 C33 C46 118.9(6) . . ? C33 C34 C35 119.8(7) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C40 C35 C34 116.6(6) . . ? C40 C35 C36 123.6(6) . . ? C34 C35 C36 119.7(7) . . ? C37 C36 C39 110.8(8) . . ? C37 C36 C38 110.6(8) . . ? C39 C36 C38 103.7(8) . . ? C37 C36 C35 109.6(6) . . ? C39 C36 C35 111.2(6) . . ? C38 C36 C35 110.9(6) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 C41 125.2(6) . . ? C35 C40 H40 117.4 . . ? C41 C40 H40 117.4 . . ? C32 C41 C40 117.5(6) . . ? C32 C41 C42 121.9(6) . . ? C40 C41 C42 120.6(6) . . ? C41 C42 C43 108.5(5) . . ? C41 C42 C45 112.0(5) . . ? C43 C42 C45 108.9(6) . . ? C41 C42 C44 112.5(6) . . ? C43 C42 C44 107.7(6) . . ? C45 C42 C44 107.1(6) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 N21 110.5(5) . . ? C33 C46 H46A 109.5 . . ? N21 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? N21 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C101 Zn2 O131 120.0(2) . . ? C101 Zn2 N111 118.5(3) . . ? O131 Zn2 N111 101.2(2) . . ? C101 Zn2 N121 133.7(3) . . ? O131 Zn2 N121 94.63(18) . . ? N111 Zn2 N121 79.0(2) . . ? C102 C101 Zn2 113.3(5) . . ? C102 C101 H10A 108.9 . . ? Zn2 C101 H10A 108.9 . . ? C102 C101 H10B 108.9 . . ? Zn2 C101 H10B 108.9 . . ? H10A C101 H10B 107.7 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C116 N111 C112 118.5(6) . . ? C116 N111 Zn2 127.0(5) . . ? C112 N111 Zn2 114.5(4) . . ? N111 C112 C113 122.2(6) . . ? N111 C112 C117 116.5(6) . . ? C113 C112 C117 121.3(6) . . ? C112 C113 C114 118.0(7) . . ? C112 C113 H113 121 . . ? C114 C113 H113 121 . . ? C115 C114 C113 119.8(7) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 119.0(7) . . ? C114 C115 H115 120.5 . . ? C116 C115 H115 120.5 . . ? N111 C116 C115 122.5(6) . . ? N111 C116 H116 118.8 . . ? C115 C116 H116 118.8 . . ? C112 C117 N121 112.2(5) . . ? C112 C117 H11A 109.2 . . ? N121 C117 H11A 109.2 . . ? C112 C117 H11B 109.2 . . ? N121 C117 H11B 109.2 . . ? H11A C117 H11B 107.9 . . ? C117 N121 C146 108.2(5) . . ? C117 N121 C122 110.3(5) . . ? C146 N121 C122 107.6(5) . . ? C117 N121 Zn2 106.3(4) . . ? C146 N121 Zn2 104.2(3) . . ? C122 N121 Zn2 119.7(4) . . ? C123 C122 N121 114.3(5) . . ? C123 C122 H12A 108.7 . . ? N121 C122 H12A 108.7 . . ? C123 C122 H12B 108.7 . . ? N121 C122 H12B 108.7 . . ? H12A C122 H12B 107.6 . . ? C124 C123 C128 118.0(6) . . ? C124 C123 C122 122.8(6) . . ? C128 C123 C122 119.2(6) . . ? C125 C124 C123 121.3(6) . . ? C125 C124 H124 119.4 . . ? C123 C124 H124 119.4 . . ? C124 C125 C126 120.6(7) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? C127 C126 C125 119.3(6) . . ? C127 C126 H126 120.3 . . ? C125 C126 H126 120.3 . . ? C128 C127 C126 119.8(6) . . ? C128 C127 H127 120.1 . . ? C126 C127 H127 120.1 . . ? C127 C128 C123 121.0(6) . . ? C127 C128 H128 119.5 . . ? C123 C128 H128 119.5 . . ? C132 O131 Zn2 115.8(4) . . ? O131 C132 C133 118.5(6) . . ? O131 C132 C141 121.3(6) . . ? C133 C132 C141 120.2(6) . . ? C134 C133 C132 120.0(6) . . ? C134 C133 C146 121.3(6) . . ? C132 C133 C146 118.7(6) . . ? C135 C134 C133 121.9(6) . . ? C135 C134 H134 119.1 . . ? C133 C134 H134 119.1 . . ? C134 C135 C140 116.6(6) . . ? C134 C135 C136 119.9(6) . . ? C140 C135 C136 123.4(6) . . ? C138 C136 C135 113.8(6) . . ? C138 C136 C139 105.5(6) . . ? C135 C136 C139 113.0(6) . . ? C138 C136 C137 106.7(7) . . ? C135 C136 C137 107.9(6) . . ? C139 C136 C137 109.7(7) . . ? C136 C137 H13A 109.5 . . ? C136 C137 H13B 109.5 . . ? H13A C137 H13B 109.5 . . ? C136 C137 H13C 109.5 . . ? H13A C137 H13C 109.5 . . ? H13B C137 H13C 109.5 . . ? C136 C138 H13D 109.5 . . ? C136 C138 H13E 109.5 . . ? H13D C138 H13E 109.5 . . ? C136 C138 H13F 109.5 . . ? H13D C138 H13F 109.5 . . ? H13E C138 H13F 109.5 . . ? C136 C139 H13G 109.5 . . ? C136 C139 H13H 109.5 . . ? H13G C139 H13H 109.5 . . ? C136 C139 H13I 109.5 . . ? H13G C139 H13I 109.5 . . ? H13H C139 H13I 109.5 . . ? C135 C140 C141 125.5(6) . . ? C135 C140 H140 117.3 . . ? C141 C140 H140 117.3 . . ? C140 C141 C132 115.5(6) . . ? C140 C141 C142 122.0(6) . . ? C132 C141 C142 122.4(6) . . ? C144 C142 C141 110.8(6) . . ? C144 C142 C143 105.7(6) . . ? C141 C142 C143 112.4(6) . . ? C144 C142 C145 108.9(6) . . ? C141 C142 C145 109.7(6) . . ? C143 C142 C145 109.2(6) . . ? C142 C143 H14A 109.5 . . ? C142 C143 H14B 109.5 . . ? H14A C143 H14B 109.5 . . ? C142 C143 H14C 109.5 . . ? H14A C143 H14C 109.5 . . ? H14B C143 H14C 109.5 . . ? C142 C144 H14D 109.5 . . ? C142 C144 H14E 109.5 . . ? H14D C144 H14E 109.5 . . ? C142 C144 H14F 109.5 . . ? H14D C144 H14F 109.5 . . ? H14E C144 H14F 109.5 . . ? C142 C145 H14G 109.5 . . ? C142 C145 H14H 109.5 . . ? H14G C145 H14H 109.5 . . ? C142 C145 H14I 109.5 . . ? H14G C145 H14I 109.5 . . ? H14H C145 H14I 109.5 . . ? N121 C146 C133 113.0(5) . . ? N121 C146 H14J 109 . . ? C133 C146 H14J 109 . . ? N121 C146 H14K 109 . . ? C133 C146 H14K 109 . . ? H14J C146 H14K 107.8 . . ? O231 Zn3 C201 119.7(3) . . ? O231 Zn3 N211 104.4(2) . . ? C201 Zn3 N211 114.9(3) . . ? O231 Zn3 N221 95.30(19) . . ? C201 Zn3 N221 135.0(3) . . ? N211 Zn3 N221 78.2(2) . . ? C202 C201 Zn3 110.8(5) . . ? C202 C201 H20A 109.5 . . ? Zn3 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? Zn3 C201 H20B 109.5 . . ? H20A C201 H20B 108.1 . . ? C201 C202 H20C 109.5 . . ? C201 C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C201 C202 H20E 109.5 . . ? H20C C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? C212 N211 C216 119.0(6) . . ? C212 N211 Zn3 114.7(4) . . ? C216 N211 Zn3 125.8(5) . . ? N211 C212 C213 122.6(6) . . ? N211 C212 C217 116.9(6) . . ? C213 C212 C217 120.3(6) . . ? C212 C213 C214 118.4(6) . . ? C212 C213 H213 120.8 . . ? C214 C213 H213 120.8 . . ? C213 C214 C215 119.3(7) . . ? C213 C214 H214 120.4 . . ? C215 C214 H214 120.4 . . ? C216 C215 C214 118.0(7) . . ? C216 C215 H215 121 . . ? C214 C215 H215 121 . . ? N211 C216 C215 122.6(7) . . ? N211 C216 H216 118.7 . . ? C215 C216 H216 118.7 . . ? N221 C217 C212 111.9(5) . . ? N221 C217 H21A 109.2 . . ? C212 C217 H21A 109.2 . . ? N221 C217 H21B 109.2 . . ? C212 C217 H21B 109.2 . . ? H21A C217 H21B 107.9 . . ? C217 N221 C246 108.7(5) . . ? C217 N221 C222 109.3(5) . . ? C246 N221 C222 106.7(5) . . ? C217 N221 Zn3 107.4(4) . . ? C246 N221 Zn3 102.8(4) . . ? C222 N221 Zn3 121.2(4) . . ? C223 C222 N221 114.1(5) . . ? C223 C222 H22C 108.7 . . ? N221 C222 H22C 108.7 . . ? C223 C222 H22D 108.7 . . ? N221 C222 H22D 108.7 . . ? H22C C222 H22D 107.6 . . ? C228 C223 C224 117.8(6) . . ? C228 C223 C222 121.6(6) . . ? C224 C223 C222 120.5(6) . . ? C225 C224 C223 121.5(7) . . ? C225 C224 H224 119.2 . . ? C223 C224 H224 119.2 . . ? C224 C225 C226 119.2(7) . . ? C224 C225 H225 120.4 . . ? C226 C225 H225 120.4 . . ? C227 C226 C225 119.2(7) . . ? C227 C226 H226 120.4 . . ? C225 C226 H226 120.4 . . ? C226 C227 C228 122.2(7) . . ? C226 C227 H227 118.9 . . ? C228 C227 H227 118.9 . . ? C227 C228 C223 120.0(7) . . ? C227 C228 H228 120 . . ? C223 C228 H228 120 . . ? C232 O231 Zn3 118.1(4) . . ? O231 C232 C241 124.1(6) . . ? O231 C232 C233 118.2(6) . . ? C241 C232 C233 117.7(6) . . ? C234 C233 C232 120.5(6) . . ? C234 C233 C246 120.8(6) . . ? C232 C233 C246 118.6(6) . . ? C235 C234 C233 122.0(6) . . ? C235 C234 H234 119 . . ? C233 C234 H234 119 . . ? C234 C235 C240 116.4(6) . . ? C234 C235 C236 123.3(6) . . ? C240 C235 C236 120.3(7) . . ? C238 C236 C237 108.1(7) . . ? C238 C236 C239 110.7(7) . . ? C237 C236 C239 106.9(7) . . ? C238 C236 C235 108.8(6) . . ? C237 C236 C235 110.6(6) . . ? C239 C236 C235 111.6(6) . . ? C236 C237 H23A 109.5 . . ? C236 C237 H23B 109.5 . . ? H23A C237 H23B 109.5 . . ? C236 C237 H23C 109.5 . . ? H23A C237 H23C 109.5 . . ? H23B C237 H23C 109.5 . . ? C236 C238 H23D 109.5 . . ? C236 C238 H23E 109.5 . . ? H23D C238 H23E 109.5 . . ? C236 C238 H23F 109.5 . . ? H23D C238 H23F 109.5 . . ? H23E C238 H23F 109.5 . . ? C236 C239 H23G 109.5 . . ? C236 C239 H23H 109.5 . . ? H23G C239 H23H 109.5 . . ? C236 C239 H23I 109.5 . . ? H23G C239 H23I 109.5 . . ? H23H C239 H23I 109.5 . . ? C241 C240 C235 125.2(7) . . ? C241 C240 H240 117.4 . . ? C235 C240 H240 117.4 . . ? C240 C241 C232 118.1(6) . . ? C240 C241 C242 122.4(6) . . ? C232 C241 C242 119.4(6) . . ? C244 C242 C243 108.3(6) . . ? C244 C242 C245 107.8(6) . . ? C243 C242 C245 108.8(6) . . ? C244 C242 C241 113.2(6) . . ? C243 C242 C241 109.6(5) . . ? C245 C242 C241 109.0(6) . . ? C242 C243 H24A 109.5 . . ? C242 C243 H24B 109.5 . . ? H24A C243 H24B 109.5 . . ? C242 C243 H24C 109.5 . . ? H24A C243 H24C 109.5 . . ? H24B C243 H24C 109.5 . . ? C242 C244 H24D 109.5 . . ? C242 C244 H24E 109.5 . . ? H24D C244 H24E 109.5 . . ? C242 C244 H24F 109.5 . . ? H24D C244 H24F 109.5 . . ? H24E C244 H24F 109.5 . . ? C242 C245 H24G 109.5 . . ? C242 C245 H24H 109.5 . . ? H24G C245 H24H 109.5 . . ? C242 C245 H24I 109.5 . . ? H24G C245 H24I 109.5 . . ? H24H C245 H24I 109.5 . . ? C233 C246 N221 113.2(5) . . ? C233 C246 H24J 108.9 . . ? N221 C246 H24J 108.9 . . ? C233 C246 H24K 108.9 . . ? N221 C246 H24K 108.9 . . ? H24J C246 H24K 107.8 . . ? 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 O31 Zn1 C1 C2 -93.9(5) . . . . ? N11 Zn1 C1 C2 33.2(6) . . . . ? N21 Zn1 C1 C2 129.6(5) . . . . ? O31 Zn1 N11 C16 75.5(6) . . . . ? C1 Zn1 N11 C16 -59.6(6) . . . . ? N21 Zn1 N11 C16 167.0(6) . . . . ? O31 Zn1 N11 C12 -103.9(4) . . . . ? C1 Zn1 N11 C12 120.9(5) . . . . ? N21 Zn1 N11 C12 -12.5(4) . . . . ? C16 N11 C12 C13 -1.5(9) . . . . ? Zn1 N11 C12 C13 178.0(5) . . . . ? C16 N11 C12 C17 175.5(6) . . . . ? Zn1 N11 C12 C17 -5.0(7) . . . . ? N11 C12 C13 C14 2.3(9) . . . . ? C17 C12 C13 C14 -174.6(6) . . . . ? C12 C13 C14 C15 -1.2(10) . . . . ? C13 C14 C15 C16 -0.5(10) . . . . ? C12 N11 C16 C15 -0.4(10) . . . . ? Zn1 N11 C16 C15 -179.8(5) . . . . ? C14 C15 C16 N11 1.3(11) . . . . ? N11 C12 C17 N21 29.3(8) . . . . ? C13 C12 C17 N21 -153.6(6) . . . . ? C12 C17 N21 C22 -169.7(5) . . . . ? C12 C17 N21 C46 74.2(7) . . . . ? C12 C17 N21 Zn1 -37.0(6) . . . . ? O31 Zn1 N21 C17 132.1(4) . . . . ? C1 Zn1 N21 C17 -83.8(5) . . . . ? N11 Zn1 N21 C17 26.6(4) . . . . ? O31 Zn1 N21 C22 -103.2(4) . . . . ? C1 Zn1 N21 C22 40.9(6) . . . . ? N11 Zn1 N21 C22 151.4(4) . . . . ? O31 Zn1 N21 C46 18.2(4) . . . . ? C1 Zn1 N21 C46 162.3(4) . . . . ? N11 Zn1 N21 C46 -87.3(4) . . . . ? C17 N21 C22 C23 65.7(7) . . . . ? C46 N21 C22 C23 -178.1(6) . . . . ? Zn1 N21 C22 C23 -58.5(7) . . . . ? N21 C22 C23 C28 -105.9(8) . . . . ? N21 C22 C23 C24 79.8(8) . . . . ? C28 C23 C24 C25 2.4(11) . . . . ? C22 C23 C24 C25 176.7(7) . . . . ? C23 C24 C25 C26 -1.2(12) . . . . ? C24 C25 C26 C27 -0.2(13) . . . . ? C25 C26 C27 C28 0.4(13) . . . . ? C24 C23 C28 C27 -2.2(11) . . . . ? C22 C23 C28 C27 -176.4(7) . . . . ? C26 C27 C28 C23 0.8(12) . . . . ? C1 Zn1 O31 C32 -110.8(5) . . . . ? N11 Zn1 O31 C32 119.3(4) . . . . ? N21 Zn1 O31 C32 39.5(4) . . . . ? Zn1 O31 C32 C33 -56.0(7) . . . . ? Zn1 O31 C32 C41 126.8(5) . . . . ? O31 C32 C33 C34 -173.8(6) . . . . ? C41 C32 C33 C34 3.6(9) . . . . ? O31 C32 C33 C46 3.2(8) . . . . ? C41 C32 C33 C46 -179.4(5) . . . . ? C32 C33 C34 C35 -3.7(9) . . . . ? C46 C33 C34 C35 179.4(6) . . . . ? C33 C34 C35 C40 1.8(9) . . . . ? C33 C34 C35 C36 178.5(6) . . . . ? C40 C35 C36 C37 -115.5(9) . . . . ? C34 C35 C36 C37 68.0(9) . . . . ? C40 C35 C36 C39 7.4(10) . . . . ? C34 C35 C36 C39 -169.1(8) . . . . ? C40 C35 C36 C38 122.2(9) . . . . ? C34 C35 C36 C38 -54.3(10) . . . . ? C34 C35 C40 C41 -0.2(10) . . . . ? C36 C35 C40 C41 -176.7(6) . . . . ? O31 C32 C41 C40 175.5(6) . . . . ? C33 C32 C41 C40 -1.8(9) . . . . ? O31 C32 C41 C42 -5.0(9) . . . . ? C33 C32 C41 C42 177.8(5) . . . . ? C35 C40 C41 C32 0.2(10) . . . . ? C35 C40 C41 C42 -179.4(6) . . . . ? C32 C41 C42 C43 67.2(8) . . . . ? C40 C41 C42 C43 -113.3(7) . . . . ? C32 C41 C42 C45 -53.1(8) . . . . ? C40 C41 C42 C45 126.5(6) . . . . ? C32 C41 C42 C44 -173.8(6) . . . . ? C40 C41 C42 C44 5.7(8) . . . . ? C34 C33 C46 N21 -116.2(6) . . . . ? C32 C33 C46 N21 66.7(7) . . . . ? C17 N21 C46 C33 -178.1(5) . . . . ? C22 N21 C46 C33 65.6(7) . . . . ? Zn1 N21 C46 C33 -64.8(6) . . . . ? O131 Zn2 C101 C102 -74.5(6) . . . . ? N111 Zn2 C101 C102 50.1(6) . . . . ? N121 Zn2 C101 C102 152.6(5) . . . . ? C101 Zn2 N111 C116 -58.7(6) . . . . ? O131 Zn2 N111 C116 74.7(6) . . . . ? N121 Zn2 N111 C116 167.3(6) . . . . ? C101 Zn2 N111 C112 123.2(5) . . . . ? O131 Zn2 N111 C112 -103.4(4) . . . . ? N121 Zn2 N111 C112 -10.8(4) . . . . ? C116 N111 C112 C113 -4.1(9) . . . . ? Zn2 N111 C112 C113 174.2(5) . . . . ? C116 N111 C112 C117 174.5(6) . . . . ? Zn2 N111 C112 C117 -7.2(7) . . . . ? N111 C112 C113 C114 3.8(10) . . . . ? C117 C112 C113 C114 -174.7(6) . . . . ? C112 C113 C114 C115 -1.7(10) . . . . ? C113 C114 C115 C116 -0.1(11) . . . . ? C112 N111 C116 C115 2.2(10) . . . . ? Zn2 N111 C116 C115 -175.9(5) . . . . ? C114 C115 C116 N111 -0.1(11) . . . . ? N111 C112 C117 N121 30.8(8) . . . . ? C113 C112 C117 N121 -150.6(6) . . . . ? C112 C117 N121 C146 74.7(7) . . . . ? C112 C117 N121 C122 -167.8(5) . . . . ? C112 C117 N121 Zn2 -36.7(6) . . . . ? C101 Zn2 N121 C117 -93.7(5) . . . . ? O131 Zn2 N121 C117 125.8(4) . . . . ? N111 Zn2 N121 C117 25.4(4) . . . . ? C101 Zn2 N121 C146 152.1(4) . . . . ? O131 Zn2 N121 C146 11.6(4) . . . . ? N111 Zn2 N121 C146 -88.9(4) . . . . ? C101 Zn2 N121 C122 32.0(6) . . . . ? O131 Zn2 N121 C122 -108.5(4) . . . . ? N111 Zn2 N121 C122 151.0(4) . . . . ? C117 N121 C122 C123 60.3(7) . . . . ? C146 N121 C122 C123 178.2(5) . . . . ? Zn2 N121 C122 C123 -63.4(7) . . . . ? N121 C122 C123 C124 73.7(9) . . . . ? N121 C122 C123 C128 -107.4(7) . . . . ? C128 C123 C124 C125 1.0(11) . . . . ? C122 C123 C124 C125 180.0(7) . . . . ? C123 C124 C125 C126 -0.7(12) . . . . ? C124 C125 C126 C127 -0.3(11) . . . . ? C125 C126 C127 C128 0.9(11) . . . . ? C126 C127 C128 C123 -0.6(11) . . . . ? C124 C123 C128 C127 -0.3(10) . . . . ? C122 C123 C128 C127 -179.3(7) . . . . ? C101 Zn2 O131 C132 -104.2(5) . . . . ? N111 Zn2 O131 C132 123.4(4) . . . . ? N121 Zn2 O131 C132 43.7(5) . . . . ? Zn2 O131 C132 C133 -54.3(7) . . . . ? Zn2 O131 C132 C141 128.9(6) . . . . ? O131 C132 C133 C134 177.8(6) . . . . ? C141 C132 C133 C134 -5.3(10) . . . . ? O131 C132 C133 C146 -1.3(9) . . . . ? C141 C132 C133 C146 175.6(6) . . . . ? C132 C133 C134 C135 0.1(10) . . . . ? C146 C133 C134 C135 179.2(6) . . . . ? C133 C134 C135 C140 3.8(10) . . . . ? C133 C134 C135 C136 -173.6(6) . . . . ? C134 C135 C136 C138 -46.0(9) . . . . ? C140 C135 C136 C138 136.8(7) . . . . ? C134 C135 C136 C139 -166.4(7) . . . . ? C140 C135 C136 C139 16.4(10) . . . . ? C134 C135 C136 C137 72.2(9) . . . . ? C140 C135 C136 C137 -105.0(8) . . . . ? C134 C135 C140 C141 -2.9(11) . . . . ? C136 C135 C140 C141 174.4(7) . . . . ? C135 C140 C141 C132 -2.0(11) . . . . ? C135 C140 C141 C142 -178.3(7) . . . . ? O131 C132 C141 C140 -177.2(6) . . . . ? C133 C132 C141 C140 6.0(10) . . . . ? O131 C132 C141 C142 -0.9(10) . . . . ? C133 C132 C141 C142 -177.7(6) . . . . ? C140 C141 C142 C144 -127.4(7) . . . . ? C132 C141 C142 C144 56.5(9) . . . . ? C140 C141 C142 C143 -9.5(10) . . . . ? C132 C141 C142 C143 174.5(7) . . . . ? C140 C141 C142 C145 112.2(7) . . . . ? C132 C141 C142 C145 -63.8(9) . . . . ? C117 N121 C146 C133 -174.4(5) . . . . ? C122 N121 C146 C133 66.4(6) . . . . ? Zn2 N121 C146 C133 -61.6(6) . . . . ? C134 C133 C146 N121 -108.9(7) . . . . ? C132 C133 C146 N121 70.2(8) . . . . ? O231 Zn3 C201 C202 -55.0(7) . . . . ? N211 Zn3 C201 C202 70.5(7) . . . . ? N221 Zn3 C201 C202 168.8(5) . . . . ? O231 Zn3 N211 C212 -111.8(5) . . . . ? C201 Zn3 N211 C212 115.1(5) . . . . ? N221 Zn3 N211 C212 -19.3(5) . . . . ? O231 Zn3 N211 C216 76.6(6) . . . . ? C201 Zn3 N211 C216 -56.5(6) . . . . ? N221 Zn3 N211 C216 169.1(6) . . . . ? C216 N211 C212 C213 3.0(10) . . . . ? Zn3 N211 C212 C213 -169.2(5) . . . . ? C216 N211 C212 C217 177.6(6) . . . . ? Zn3 N211 C212 C217 5.4(7) . . . . ? N211 C212 C213 C214 0.0(10) . . . . ? C217 C212 C213 C214 -174.4(6) . . . . ? C212 C213 C214 C215 -3.7(10) . . . . ? C213 C214 C215 C216 4.2(10) . . . . ? C212 N211 C216 C215 -2.4(10) . . . . ? Zn3 N211 C216 C215 168.9(5) . . . . ? C214 C215 C216 N211 -1.2(11) . . . . ? N211 C212 C217 N221 20.1(8) . . . . ? C213 C212 C217 N221 -165.2(6) . . . . ? C212 C217 N221 C246 76.7(6) . . . . ? C212 C217 N221 C222 -167.2(5) . . . . ? C212 C217 N221 Zn3 -33.9(6) . . . . ? O231 Zn3 N221 C217 131.9(4) . . . . ? C201 Zn3 N221 C217 -85.3(5) . . . . ? N211 Zn3 N221 C217 28.2(4) . . . . ? O231 Zn3 N221 C246 17.3(4) . . . . ? C201 Zn3 N221 C246 160.1(5) . . . . ? N211 Zn3 N221 C246 -86.4(4) . . . . ? O231 Zn3 N221 C222 -101.6(5) . . . . ? C201 Zn3 N221 C222 41.2(6) . . . . ? N211 Zn3 N221 C222 154.7(5) . . . . ? C217 N221 C222 C223 58.4(7) . . . . ? C246 N221 C222 C223 175.9(5) . . . . ? Zn3 N221 C222 C223 -67.2(7) . . . . ? N221 C222 C223 C228 -112.3(7) . . . . ? N221 C222 C223 C224 70.8(8) . . . . ? C228 C223 C224 C225 -1.8(10) . . . . ? C222 C223 C224 C225 175.2(6) . . . . ? C223 C224 C225 C226 0.0(10) . . . . ? C224 C225 C226 C227 1.1(11) . . . . ? C225 C226 C227 C228 -0.2(12) . . . . ? C226 C227 C228 C223 -1.6(12) . . . . ? C224 C223 C228 C227 2.6(10) . . . . ? C222 C223 C228 C227 -174.4(7) . . . . ? C201 Zn3 O231 C232 -111.4(5) . . . . ? N211 Zn3 O231 C232 118.3(4) . . . . ? N221 Zn3 O231 C232 39.1(4) . . . . ? Zn3 O231 C232 C241 126.7(6) . . . . ? Zn3 O231 C232 C233 -54.3(7) . . . . ? O231 C232 C233 C234 -178.3(5) . . . . ? C241 C232 C233 C234 0.8(9) . . . . ? O231 C232 C233 C246 3.0(9) . . . . ? C241 C232 C233 C246 -177.9(6) . . . . ? C232 C233 C234 C235 0.3(10) . . . . ? C246 C233 C234 C235 179.0(6) . . . . ? C233 C234 C235 C240 -1.8(10) . . . . ? C233 C234 C235 C236 175.4(6) . . . . ? C234 C235 C236 C238 -100.0(8) . . . . ? C240 C235 C236 C238 77.1(8) . . . . ? C234 C235 C236 C237 18.6(10) . . . . ? C240 C235 C236 C237 -164.3(7) . . . . ? C234 C235 C236 C239 137.5(7) . . . . ? C240 C235 C236 C239 -45.4(9) . . . . ? C234 C235 C240 C241 2.5(10) . . . . ? C236 C235 C240 C241 -174.8(6) . . . . ? C235 C240 C241 C232 -1.5(10) . . . . ? C235 C240 C241 C242 -178.7(6) . . . . ? O231 C232 C241 C240 178.8(6) . . . . ? C233 C232 C241 C240 -0.2(9) . . . . ? O231 C232 C241 C242 -3.9(9) . . . . ? C233 C232 C241 C242 177.1(5) . . . . ? C240 C241 C242 C244 -1.2(9) . . . . ? C232 C241 C242 C244 -178.3(6) . . . . ? C240 C241 C242 C243 -122.2(7) . . . . ? C232 C241 C242 C243 60.6(8) . . . . ? C240 C241 C242 C245 118.8(7) . . . . ? C232 C241 C242 C245 -58.4(8) . . . . ? C234 C233 C246 N221 -111.7(6) . . . . ? C232 C233 C246 N221 67.0(7) . . . . ? C217 N221 C246 C233 -178.3(5) . . . . ? C222 N221 C246 C233 63.8(6) . . . . ? Zn3 N221 C246 C233 -64.7(5) . . . . ? # Attachment 'complex6_ZG57.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-08-27 at 16:09:53 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : f:\progs\wingx\files\archive.dat # CIF files read : sq struct data_sq _database_code_depnum_ccdc_archive 'CCDC 672304' _audit_creation_date 2008-08-27T16:09:53-00:00 _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 'C34 H53 N3 O Si2 Zn' _chemical_formula_sum 'C34 H53 N3 O Si2 Zn' _chemical_formula_weight 641.34 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 15.2406(8) _cell_length_b 10.5921(6) _cell_length_c 48.038(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7754.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8500 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.02 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.722 _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 0.749 _exptl_absorpt_correction_T_max 0.958 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.382 0.287 0.470 224 27 ' ' 2 0.882 -0.287 0.470 224 27 ' ' 3 0.118 0.287 0.970 224 27 ' ' 4 0.618 -0.287 0.970 224 28 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_unetI/netI 0.0799 _diffrn_reflns_number 67188 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 4.1 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 17364 _reflns_number_gt 13933 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0958P)^2^+29.1824P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0070(5) _refine_ls_number_reflns 17364 _refine_ls_number_parameters 745 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2364 _refine_ls_wR_factor_gt 0.2289 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.109(19) _refine_diff_density_max 0.869 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 0.44081(5) 0.79945(8) 0.818328(16) 0.0223(2) Uani 1 d . . . Si1 Si 0.07131(13) 0.4160(2) 0.62537(5) 0.0229(4) Uani 1 d . . . Si2 Si 0.22660(13) 0.42402(18) 0.66484(4) 0.0183(4) Uani 1 d . . . C1 C 0.0194(6) 0.5521(8) 0.64586(19) 0.0335(19) Uani 1 d . . . H1A H 0.0009 0.5217 0.6642 0.05 Uiso 1 calc R . . H1B H -0.0318 0.584 0.6357 0.05 Uiso 1 calc R . . H1C H 0.0624 0.6201 0.6481 0.05 Uiso 1 calc R . . C2 C 0.0963(6) 0.4858(7) 0.5909(2) 0.034(2) Uani 1 d . . . H2A H 0.1411 0.5514 0.593 0.051 Uiso 1 calc R . . H2B H 0.0429 0.5231 0.5831 0.051 Uiso 1 calc R . . H2C H 0.1181 0.4198 0.5784 0.051 Uiso 1 calc R . . C3 C -0.0153(5) 0.2947(7) 0.6208(2) 0.0274(15) Uani 1 d . . . H3A H 0.009 0.222 0.6108 0.041 Uiso 1 calc R . . H3B H -0.0641 0.3305 0.6101 0.041 Uiso 1 calc R . . H3C H -0.0365 0.2675 0.6391 0.041 Uiso 1 calc R . . C4 C 0.2753(5) 0.5746(8) 0.6519(2) 0.036(2) Uani 1 d . . . H4A H 0.3189 0.556 0.6375 0.055 Uiso 1 calc R . . H4B H 0.3038 0.6189 0.6674 0.055 Uiso 1 calc R . . H4C H 0.2289 0.628 0.6441 0.055 Uiso 1 calc R . . C5 C 0.1662(6) 0.4643(9) 0.69750(19) 0.0338(19) Uani 1 d . . . H5A H 0.1375 0.5465 0.6953 0.051 Uiso 1 calc R . . H5B H 0.2077 0.468 0.7131 0.051 Uiso 1 calc R . . H5C H 0.1219 0.3995 0.7012 0.051 Uiso 1 calc R . . C6 C 0.3191(5) 0.3191(8) 0.67645(18) 0.0310(18) Uani 1 d . . . H6A H 0.2952 0.247 0.6868 0.047 Uiso 1 calc R . . H6B H 0.3588 0.367 0.6885 0.047 Uiso 1 calc R . . H6C H 0.3513 0.2886 0.6601 0.047 Uiso 1 calc R . . N1 N 0.1625(4) 0.3495(6) 0.64063(13) 0.0200(13) Uani 1 d . . . N11 N 0.2480(4) 0.0213(6) 0.63641(13) 0.0183(12) Uani 1 d . . . C12 C 0.2358(4) -0.0145(7) 0.66610(15) 0.0172(14) Uani 1 d . . . H12A H 0.2692 0.0458 0.6778 0.021 Uiso 1 calc R . . H12B H 0.2619 -0.0991 0.669 0.021 Uiso 1 calc R . . C13 C 0.1435(5) -0.0175(7) 0.67628(15) 0.0185(14) Uani 1 d . . . C14 C 0.0929(5) 0.0917(7) 0.67838(16) 0.0233(16) Uani 1 d . . . H14 H 0.1154 0.1707 0.6723 0.028 Uiso 1 calc R . . C15 C 0.0065(6) 0.0825(8) 0.68984(16) 0.0285(18) Uani 1 d . . . H15 H -0.0278 0.1568 0.692 0.034 Uiso 1 calc R . . C16 C -0.0279(6) -0.0322(10) 0.69788(17) 0.034(2) Uani 1 d . . . H16 H -0.0861 -0.0372 0.7049 0.041 Uiso 1 calc R . . C17 C 0.0231(6) -0.1401(8) 0.69567(16) 0.0307(18) Uani 1 d . . . H17 H 0.0007 -0.2194 0.7016 0.037 Uiso 1 calc R . . C18 C 0.1072(6) -0.1313(8) 0.68472(17) 0.0316(19) Uani 1 d . . . H18 H 0.1412 -0.206 0.6829 0.038 Uiso 1 calc R . . N21 N 0.3320(4) 0.2033(5) 0.60351(12) 0.0185(12) Uani 1 d . . . C22 C 0.3608(5) 0.2886(7) 0.58477(17) 0.0254(16) Uani 1 d . . . H22 H 0.3297 0.3657 0.5826 0.03 Uiso 1 calc R . . C23 C 0.4347(5) 0.2662(8) 0.56862(16) 0.0317(19) Uani 1 d . . . H23 H 0.4549 0.3284 0.5559 0.038 Uiso 1 calc R . . C24 C 0.4788(5) 0.1532(8) 0.57119(17) 0.0288(17) Uani 1 d . . . H24 H 0.5288 0.135 0.5601 0.035 Uiso 1 calc R . . C25 C 0.4479(5) 0.0677(8) 0.59031(16) 0.0268(17) Uani 1 d . . . H25 H 0.4769 -0.011 0.5927 0.032 Uiso 1 calc R . . C26 C 0.3749(5) 0.0962(7) 0.60612(15) 0.0207(15) Uani 1 d . . . C27 C 0.3428(4) 0.0085(7) 0.62874(15) 0.0189(15) Uiso 1 d . . . H27A H 0.3534 -0.0795 0.6227 0.023 Uiso 1 calc R . . H27B H 0.3785 0.0232 0.6456 0.023 Uiso 1 calc R . . O31 O 0.1425(3) 0.1434(5) 0.58922(10) 0.0172(10) Uiso 1 d . . . C32 C 0.1717(4) 0.0422(7) 0.57479(15) 0.0177(14) Uani 1 d . . . C33 C 0.1670(4) 0.0398(6) 0.54493(14) 0.0135(13) Uiso 1 d . . . C34 C 0.1312(5) 0.1596(7) 0.52872(15) 0.0218(15) Uani 1 d . . . C35 C 0.1951(5) 0.2661(8) 0.53284(17) 0.0247(16) Uiso 1 d . . . H35A H 0.1726 0.3424 0.5238 0.037 Uiso 1 calc R . . H35B H 0.2518 0.2433 0.5246 0.037 Uiso 1 calc R . . H35C H 0.2026 0.282 0.5528 0.037 Uiso 1 calc R . . C36 C 0.0391(5) 0.1885(9) 0.53855(19) 0.037(2) Uani 1 d . . . H36A H 0.0399 0.206 0.5586 0.056 Uiso 1 calc R . . H36B H 0.0011 0.1158 0.5349 0.056 Uiso 1 calc R . . H36C H 0.0166 0.2625 0.5286 0.056 Uiso 1 calc R . . C37 C 0.1263(6) 0.1299(8) 0.49700(17) 0.034(2) Uani 1 d . . . H37A H 0.1075 0.2056 0.4869 0.051 Uiso 1 calc R . . H37B H 0.084 0.0617 0.4938 0.051 Uiso 1 calc R . . H37C H 0.1843 0.1038 0.4903 0.051 Uiso 1 calc R . . C38 C 0.1964(5) -0.0683(7) 0.53190(17) 0.0214(15) Uani 1 d . . . H38 H 0.1923 -0.0716 0.5122 0.026 Uiso 1 calc R . . C39 C 0.2310(5) -0.1706(8) 0.54513(16) 0.0240(16) Uani 1 d . . . C40 C 0.2593(6) -0.2890(7) 0.52786(17) 0.0296(18) Uani 1 d . . . C41 C 0.1747(7) -0.3556(7) 0.51750(19) 0.038(2) Uani 1 d . . . H41A H 0.1366 -0.2938 0.5083 0.056 Uiso 1 calc R . . H41B H 0.1436 -0.3927 0.5334 0.056 Uiso 1 calc R . . H41C H 0.1903 -0.4223 0.5043 0.056 Uiso 1 calc R . . C42 C 0.3152(6) -0.2493(9) 0.50329(19) 0.041(2) Uani 1 d . . . H42A H 0.3593 -0.1881 0.5095 0.061 Uiso 1 calc R . . H42B H 0.2779 -0.2107 0.489 0.061 Uiso 1 calc R . . H42C H 0.3447 -0.3236 0.4955 0.061 Uiso 1 calc R . . C43 C 0.3102(7) -0.3822(9) 0.54611(19) 0.044(2) Uani 1 d . . . H43A H 0.3246 -0.4576 0.5352 0.067 Uiso 1 calc R . . H43B H 0.2741 -0.4062 0.5621 0.067 Uiso 1 calc R . . H43C H 0.3645 -0.3424 0.5526 0.067 Uiso 1 calc R . . C44 C 0.2342(5) -0.1680(6) 0.57397(15) 0.0197(14) Uani 1 d . . . H44 H 0.2565 -0.2387 0.5839 0.024 Uiso 1 calc R . . C45 C 0.2049(4) -0.0624(6) 0.58856(16) 0.0156(14) Uani 1 d . . . C46 C 0.1953(5) -0.0709(7) 0.61985(18) 0.0235(15) Uani 1 d . . . H46A H 0.1326 -0.0589 0.6246 0.028 Uiso 1 calc R . . H46B H 0.2119 -0.1572 0.6257 0.028 Uiso 1 calc R . . Zn2 Zn 0.20678(5) 0.20529(7) 0.621107(15) 0.01744(19) Uani 1 d . . . Si11 Si 0.46224(14) 0.5830(2) 0.77409(5) 0.0304(5) Uani 1 d . . . Si12 Si 0.30508(13) 0.5906(2) 0.81277(5) 0.0300(5) Uani 1 d . . . C101 C 0.4052(6) 0.5380(13) 0.7406(2) 0.053(3) Uani 1 d . . . H10A H 0.3596 0.4752 0.7445 0.079 Uiso 1 calc R . . H10B H 0.4481 0.5022 0.7276 0.079 Uiso 1 calc R . . H10C H 0.3784 0.6131 0.7323 0.079 Uiso 1 calc R . . C102 C 0.5110(6) 0.4328(9) 0.7886(2) 0.044(2) Uani 1 d . . . H10D H 0.5517 0.4536 0.8037 0.065 Uiso 1 calc R . . H10E H 0.5427 0.3882 0.7738 0.065 Uiso 1 calc R . . H10F H 0.464 0.3788 0.7958 0.065 Uiso 1 calc R . . C103 C 0.5543(5) 0.6900(9) 0.76360(17) 0.035(2) Uani 1 d . . . H10G H 0.5345 0.7459 0.7486 0.053 Uiso 1 calc R . . H10H H 0.6039 0.6393 0.7571 0.053 Uiso 1 calc R . . H10I H 0.5725 0.7408 0.7796 0.053 Uiso 1 calc R . . C104 C 0.2560(6) 0.4614(8) 0.7911(2) 0.037(2) Uani 1 d . . . H10J H 0.2297 0.4977 0.7743 0.056 Uiso 1 calc R . . H10K H 0.2107 0.4176 0.8019 0.056 Uiso 1 calc R . . H10L H 0.3019 0.4012 0.7858 0.056 Uiso 1 calc R . . C105 C 0.2177(5) 0.7117(8) 0.8175(2) 0.0354(19) Uani 1 d . . . H10M H 0.239 0.7783 0.8299 0.053 Uiso 1 calc R . . H10N H 0.1656 0.6721 0.8256 0.053 Uiso 1 calc R . . H10O H 0.2026 0.7484 0.7994 0.053 Uiso 1 calc R . . C106 C 0.3289(6) 0.5212(10) 0.8478(2) 0.041(2) Uani 1 d . . . H10P H 0.3636 0.444 0.8456 0.062 Uiso 1 calc R . . H10Q H 0.2736 0.501 0.8572 0.062 Uiso 1 calc R . . H10R H 0.3619 0.5822 0.859 0.062 Uiso 1 calc R . . N101 N 0.3973(4) 0.6556(7) 0.79817(14) 0.0290(15) Uani 1 d . . . N111 N 0.4841(4) 0.9824(7) 0.80393(14) 0.0271(15) Uani 1 d . . . C112 C 0.4754(5) 1.0173(9) 0.77365(17) 0.0313(19) Uani 1 d . . . H11A H 0.5035 1.1004 0.7706 0.038 Uiso 1 calc R . . H11B H 0.5076 0.9544 0.7623 0.038 Uiso 1 calc R . . C113 C 0.3833(5) 1.0237(9) 0.76367(17) 0.0301(18) Uani 1 d . . . C114 C 0.3473(6) 1.1457(10) 0.75711(18) 0.035(2) Uani 1 d . . . H114 H 0.3809 1.2202 0.7599 0.042 Uiso 1 calc R . . C115 C 0.2622(6) 1.1526(11) 0.74654(18) 0.043(2) Uani 1 d . . . H115 H 0.2372 1.2323 0.7422 0.051 Uiso 1 calc R . . C116 C 0.2135(6) 1.0419(10) 0.74236(17) 0.037(2) Uani 1 d . . . H116 H 0.1559 1.0472 0.7349 0.045 Uiso 1 calc R . . C117 C 0.2478(6) 0.9268(11) 0.74883(18) 0.041(2) Uani 1 d . . . H117 H 0.214 0.8525 0.7461 0.05 Uiso 1 calc R . . C118 C 0.3320(6) 0.9184(10) 0.75948(17) 0.036(2) Uani 1 d . . . H118 H 0.355 0.8376 0.764 0.043 Uiso 1 calc R . . N121 N 0.5652(4) 0.7956(6) 0.83664(13) 0.0242(14) Uani 1 d . . . C122 C 0.5925(5) 0.7082(7) 0.85520(16) 0.0226(15) Uani 1 d . . . H122 H 0.5605 0.6318 0.8572 0.027 Uiso 1 calc R . . C123 C 0.6661(5) 0.7285(7) 0.87128(17) 0.0261(16) Uani 1 d . . . H123 H 0.6845 0.6661 0.8842 0.031 Uiso 1 calc R . . C124 C 0.7125(5) 0.8381(9) 0.86862(17) 0.0324(18) Uani 1 d . . . H124 H 0.7637 0.8518 0.8795 0.039 Uiso 1 calc R . . C125 C 0.6838(5) 0.9310(8) 0.84955(18) 0.0306(18) Uani 1 d . . . H125 H 0.7151 1.008 0.8474 0.037 Uiso 1 calc R . . C126 C 0.6100(5) 0.9076(8) 0.83419(16) 0.0260(17) Uani 1 d . . . C127 C 0.5789(5) 0.9917(8) 0.81122(18) 0.0285(18) Uani 1 d . . . H12C H 0.5917 1.0802 0.8165 0.034 Uiso 1 calc R . . H12D H 0.6137 0.9726 0.7943 0.034 Uiso 1 calc R . . O131 O 0.3755(3) 0.8607(5) 0.85014(11) 0.0242(11) Uani 1 d . . . C132 C 0.4039(4) 0.9569(7) 0.86499(16) 0.0218(16) Uani 1 d . . . C133 C 0.3986(4) 0.9596(7) 0.89457(16) 0.0224(15) Uani 1 d . . . C134 C 0.3635(5) 0.8501(7) 0.91132(16) 0.0227(15) Uani 1 d . . . C135 C 0.4252(6) 0.7329(9) 0.9073(2) 0.036(2) Uani 1 d . . . H13A H 0.4299 0.713 0.8874 0.055 Uiso 1 calc R . . H13B H 0.4006 0.6602 0.9172 0.055 Uiso 1 calc R . . H13C H 0.4835 0.7522 0.9148 0.055 Uiso 1 calc R . . C136 C 0.2702(5) 0.8092(7) 0.90047(17) 0.0251(16) Uani 1 d . . . H13D H 0.2298 0.8809 0.9017 0.038 Uiso 1 calc R . . H13E H 0.248 0.7395 0.9119 0.038 Uiso 1 calc R . . H13F H 0.2747 0.7816 0.881 0.038 Uiso 1 calc R . . C137 C 0.3567(6) 0.8704(8) 0.94205(17) 0.0306(18) Uani 1 d . . . H13G H 0.415 0.8625 0.9505 0.046 Uiso 1 calc R . . H13H H 0.3173 0.8069 0.9501 0.046 Uiso 1 calc R . . H13I H 0.3333 0.9549 0.9457 0.046 Uiso 1 calc R . . C138 C 0.4275(5) 1.0677(7) 0.90861(16) 0.0216(16) Uani 1 d . . . H138 H 0.4234 1.068 0.9283 0.026 Uiso 1 calc R . . C139 C 0.4629(5) 1.1783(7) 0.89540(16) 0.0220(15) Uani 1 d . . . C140 C 0.4877(6) 1.2926(7) 0.91235(18) 0.033(2) Uani 1 d . . . C141 C 0.5475(7) 1.2529(8) 0.93684(19) 0.040(2) Uani 1 d . . . H14A H 0.5144 1.1993 0.9497 0.059 Uiso 1 calc R . . H14B H 0.568 1.3284 0.9467 0.059 Uiso 1 calc R . . H14C H 0.5981 1.2059 0.9296 0.059 Uiso 1 calc R . . C142 C 0.4053(6) 1.3558(9) 0.9236(2) 0.041(2) Uani 1 d . . . H14D H 0.3699 1.3875 0.9081 0.062 Uiso 1 calc R . . H14E H 0.4218 1.4263 0.9357 0.062 Uiso 1 calc R . . H14F H 0.3709 1.2943 0.9343 0.062 Uiso 1 calc R . . C143 C 0.5408(7) 1.3880(9) 0.8948(2) 0.044(2) Uani 1 d . . . H14G H 0.5897 1.3443 0.8857 0.067 Uiso 1 calc R . . H14H H 0.5638 1.4545 0.907 0.067 Uiso 1 calc R . . H14I H 0.5027 1.4256 0.8806 0.067 Uiso 1 calc R . . C144 C 0.4678(5) 1.1680(8) 0.86655(16) 0.0279(17) Uani 1 d . . . H144 H 0.4933 1.2364 0.8566 0.033 Uiso 1 calc R . . C145 C 0.4390(5) 1.0678(8) 0.85152(18) 0.0265(18) Uani 1 d . . . C146 C 0.4312(5) 1.0754(7) 0.82055(17) 0.0233(15) Uani 1 d . . . H14J H 0.4485 1.1615 0.8147 0.028 Uiso 1 calc R . . H14K H 0.3686 1.0643 0.8156 0.028 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 0.0200(4) 0.0270(5) 0.0200(4) -0.0033(4) -0.0013(3) 0.0005(3) Si1 0.0200(9) 0.0205(10) 0.0281(11) -0.0029(9) 0.0023(8) 0.0020(8) Si2 0.0222(9) 0.0107(9) 0.0221(10) -0.0025(8) 0.0010(8) -0.0027(8) C1 0.031(4) 0.028(4) 0.041(5) -0.004(4) 0.001(4) 0.013(4) C2 0.044(5) 0.010(4) 0.048(6) 0.005(4) 0.005(4) 0.010(4) C3 0.028(3) 0.021(3) 0.034(4) -0.006(4) 0.001(4) 0.001(3) C4 0.023(4) 0.025(4) 0.061(6) -0.003(4) -0.009(4) -0.011(3) C5 0.035(4) 0.033(5) 0.034(5) -0.004(4) -0.002(4) 0.000(4) C6 0.026(4) 0.033(4) 0.034(4) 0.008(4) -0.006(3) -0.014(3) N1 0.018(3) 0.017(3) 0.025(3) -0.005(3) 0.003(2) 0.005(2) N11 0.018(3) 0.015(3) 0.021(3) -0.006(2) -0.004(2) 0.007(2) C12 0.024(3) 0.013(3) 0.015(3) -0.003(3) -0.002(3) 0.006(3) C13 0.026(3) 0.015(3) 0.014(4) 0.005(3) 0.000(3) -0.007(3) C14 0.029(4) 0.023(4) 0.019(4) 0.001(3) -0.006(3) -0.005(3) C15 0.039(4) 0.028(4) 0.018(4) 0.007(3) 0.002(3) 0.006(4) C16 0.029(4) 0.056(6) 0.017(4) 0.001(4) 0.002(3) -0.010(4) C17 0.037(4) 0.033(5) 0.022(4) -0.002(3) 0.000(3) -0.018(4) C18 0.051(5) 0.027(4) 0.018(4) 0.006(3) 0.002(3) -0.013(4) N21 0.023(3) 0.015(3) 0.017(3) -0.003(2) 0.002(2) 0.001(2) C22 0.026(4) 0.020(4) 0.029(4) -0.008(3) 0.000(3) 0.000(3) C23 0.033(4) 0.039(5) 0.023(4) 0.010(3) 0.005(3) -0.021(4) C24 0.031(4) 0.022(4) 0.034(4) -0.006(3) 0.009(3) 0.015(3) C25 0.026(4) 0.028(4) 0.027(4) -0.003(3) 0.001(3) 0.003(3) C26 0.023(3) 0.019(4) 0.020(4) -0.004(3) -0.004(3) 0.004(3) C32 0.019(3) 0.015(4) 0.019(4) -0.004(3) 0.005(3) 0.001(3) C34 0.035(4) 0.011(3) 0.020(4) -0.009(3) 0.000(3) 0.002(3) C36 0.030(4) 0.051(6) 0.030(5) 0.005(4) -0.006(3) 0.019(4) C37 0.056(5) 0.023(4) 0.024(4) 0.006(3) -0.012(4) 0.012(4) C38 0.023(4) 0.019(4) 0.022(4) -0.006(3) -0.004(3) -0.004(3) C39 0.025(4) 0.022(4) 0.025(4) 0.005(3) 0.008(3) 0.006(3) C40 0.046(5) 0.014(4) 0.030(4) 0.006(3) 0.004(4) -0.002(3) C41 0.071(6) 0.004(4) 0.038(5) 0.000(3) 0.013(4) 0.000(4) C42 0.049(5) 0.037(5) 0.036(5) 0.025(4) 0.015(4) 0.021(4) C43 0.071(7) 0.028(5) 0.035(5) 0.013(4) 0.017(4) 0.020(5) C44 0.029(4) 0.008(3) 0.023(4) -0.004(3) 0.002(3) 0.003(3) C45 0.017(3) 0.007(3) 0.023(4) 0.006(3) 0.003(3) 0.005(2) C46 0.030(4) 0.022(3) 0.019(4) 0.003(4) -0.001(3) 0.014(3) Zn2 0.0205(4) 0.0126(4) 0.0192(4) -0.0004(4) 0.0013(3) 0.0003(3) Si11 0.0227(10) 0.0406(13) 0.0280(12) -0.0117(10) -0.0034(9) 0.0003(10) Si12 0.0174(9) 0.0388(13) 0.0337(13) -0.0088(10) -0.0011(8) -0.0040(9) C101 0.038(5) 0.089(8) 0.032(5) -0.027(6) -0.003(4) 0.000(5) C102 0.030(4) 0.047(6) 0.054(6) -0.012(5) -0.011(4) 0.002(4) C103 0.030(4) 0.055(6) 0.020(4) -0.009(4) -0.003(3) -0.010(4) C104 0.032(4) 0.030(5) 0.050(6) -0.015(4) 0.001(4) 0.004(4) C105 0.021(3) 0.048(5) 0.038(5) -0.013(4) -0.001(4) -0.001(3) C106 0.042(5) 0.046(6) 0.036(5) 0.008(4) -0.004(4) -0.002(4) N101 0.022(3) 0.040(4) 0.025(3) -0.006(3) -0.001(3) 0.003(3) N111 0.024(3) 0.038(4) 0.019(3) 0.006(3) 0.003(2) -0.003(3) C112 0.028(4) 0.045(5) 0.021(4) 0.002(4) -0.003(3) 0.019(4) C113 0.027(4) 0.042(5) 0.021(4) -0.007(4) 0.005(3) 0.004(4) C114 0.031(4) 0.047(6) 0.026(4) -0.008(4) 0.002(3) 0.008(4) C115 0.034(4) 0.070(7) 0.024(4) 0.000(5) 0.005(3) 0.011(5) C116 0.030(4) 0.060(6) 0.021(4) 0.003(4) -0.006(3) 0.008(4) C117 0.028(4) 0.071(7) 0.024(5) -0.006(4) -0.010(3) 0.005(5) C118 0.039(5) 0.051(6) 0.018(4) 0.013(4) -0.003(3) -0.002(4) N121 0.017(3) 0.033(4) 0.023(3) -0.008(3) -0.004(2) 0.002(3) C122 0.022(3) 0.015(3) 0.030(4) 0.003(3) -0.005(3) 0.001(3) C123 0.028(4) 0.022(4) 0.028(4) -0.003(3) 0.002(3) -0.002(3) C124 0.024(4) 0.043(5) 0.030(4) 0.006(4) -0.008(3) 0.005(4) C125 0.025(4) 0.033(4) 0.034(4) 0.006(4) -0.006(3) -0.007(3) C126 0.019(3) 0.039(5) 0.020(4) 0.002(3) 0.004(3) 0.003(3) C127 0.021(3) 0.035(4) 0.030(4) 0.008(3) 0.002(3) -0.010(3) O131 0.031(3) 0.020(3) 0.021(2) -0.006(2) -0.001(2) -0.001(2) C132 0.015(3) 0.021(4) 0.030(4) -0.008(3) 0.000(3) 0.004(3) C133 0.016(3) 0.022(4) 0.029(4) -0.003(3) -0.002(3) 0.001(3) C134 0.021(3) 0.021(4) 0.026(4) 0.006(3) 0.002(3) -0.008(3) C135 0.044(5) 0.028(4) 0.037(5) 0.000(4) 0.007(4) 0.007(4) C136 0.030(4) 0.017(4) 0.028(4) -0.001(3) 0.004(3) 0.001(3) C137 0.038(4) 0.027(4) 0.027(4) -0.002(3) 0.001(3) -0.009(4) C138 0.026(4) 0.021(4) 0.018(4) 0.005(3) -0.001(3) -0.006(3) C139 0.027(4) 0.011(3) 0.028(4) 0.001(3) -0.004(3) -0.004(3) C140 0.044(5) 0.021(4) 0.033(4) 0.003(3) -0.016(4) -0.025(4) C141 0.063(6) 0.018(4) 0.038(5) -0.005(4) -0.019(4) -0.020(4) C142 0.051(5) 0.036(5) 0.037(5) -0.009(4) -0.010(4) -0.010(4) C143 0.059(6) 0.040(5) 0.035(5) 0.002(4) -0.018(4) -0.027(5) C144 0.029(4) 0.032(4) 0.022(4) 0.009(3) 0.001(3) -0.005(4) C145 0.028(4) 0.030(4) 0.021(4) 0.004(3) -0.001(3) 0.001(3) C146 0.027(4) 0.022(4) 0.021(4) -0.003(3) -0.001(3) 0.008(3) #----------------------------------------------------------------------------# # 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 N101 1.923(7) . ? Zn1 O131 1.936(5) . ? Zn1 N121 2.091(6) . ? Zn1 N111 2.160(7) . ? Si1 N1 1.721(6) . ? Si1 C2 1.853(10) . ? Si1 C3 1.854(7) . ? Si1 C1 1.917(8) . ? Si2 N1 1.712(6) . ? Si2 C4 1.866(9) . ? Si2 C5 1.868(9) . ? Si2 C6 1.879(9) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? N1 Zn2 1.916(6) . ? N11 C12 1.487(9) . ? N11 C46 1.494(10) . ? N11 C27 1.497(8) . ? N11 Zn2 2.175(6) . ? C12 C13 1.490(9) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C18 1.387(11) . ? C13 C14 1.393(11) . ? C14 C15 1.431(12) . ? C14 H14 0.95 . ? C15 C16 1.378(13) . ? C15 H15 0.95 . ? C16 C17 1.386(13) . ? C16 H16 0.95 . ? C17 C18 1.389(12) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? N21 C26 1.315(9) . ? N21 C22 1.348(10) . ? N21 Zn2 2.087(6) . ? C22 C23 1.389(11) . ? C22 H22 0.95 . ? C23 C24 1.377(12) . ? C23 H23 0.95 . ? C24 C25 1.372(12) . ? C24 H24 0.95 . ? C25 C26 1.381(10) . ? C25 H25 0.95 . ? C26 C27 1.511(10) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? O31 C32 1.352(8) . ? O31 Zn2 1.933(5) . ? C32 C45 1.385(10) . ? C32 C33 1.437(10) . ? C33 C38 1.380(10) . ? C33 C34 1.586(10) . ? C34 C35 1.504(11) . ? C34 C36 1.512(11) . ? C34 C37 1.557(11) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.362(11) . ? C38 H38 0.95 . ? C39 C44 1.387(10) . ? C39 C40 1.564(11) . ? C40 C42 1.515(11) . ? C40 C43 1.531(12) . ? C40 C41 1.553(13) . ? 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 . ? C44 C45 1.394(10) . ? C44 H44 0.95 . ? C45 C46 1.513(11) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? Si11 N101 1.705(7) . ? Si11 C103 1.872(9) . ? Si11 C102 1.889(10) . ? Si11 C101 1.891(9) . ? Si12 N101 1.716(7) . ? Si12 C105 1.862(8) . ? Si12 C106 1.873(10) . ? Si12 C104 1.875(9) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? C103 H10G 0.98 . ? C103 H10H 0.98 . ? C103 H10I 0.98 . ? C104 H10J 0.98 . ? C104 H10K 0.98 . ? C104 H10L 0.98 . ? C105 H10M 0.98 . ? C105 H10N 0.98 . ? C105 H10O 0.98 . ? C106 H10P 0.98 . ? C106 H10Q 0.98 . ? C106 H10R 0.98 . ? N111 C127 1.491(9) . ? N111 C146 1.503(10) . ? N111 C112 1.507(10) . ? C112 C113 1.485(11) . ? C112 H11A 0.99 . ? C112 H11B 0.99 . ? C113 C118 1.377(13) . ? C113 C114 1.440(13) . ? C114 C115 1.395(12) . ? C114 H114 0.95 . ? C115 C116 1.402(15) . ? C115 H115 0.95 . ? C116 C117 1.362(14) . ? C116 H116 0.95 . ? C117 C118 1.384(12) . ? C117 H117 0.95 . ? C118 H118 0.95 . ? N121 C122 1.350(9) . ? N121 C126 1.374(11) . ? C122 C123 1.379(11) . ? C122 H122 0.95 . ? C123 C124 1.366(12) . ? C123 H123 0.95 . ? C124 C125 1.414(11) . ? C124 H124 0.95 . ? C125 C126 1.368(11) . ? C125 H125 0.95 . ? C126 C127 1.495(11) . ? C127 H12C 0.99 . ? C127 H12D 0.99 . ? O131 C132 1.317(9) . ? C132 C133 1.424(11) . ? C132 C145 1.443(12) . ? C133 C138 1.400(11) . ? C133 C134 1.509(11) . ? C134 C137 1.496(11) . ? C134 C135 1.569(12) . ? C134 C136 1.576(10) . ? C135 H13A 0.98 . ? C135 H13B 0.98 . ? C135 H13C 0.98 . ? C136 H13D 0.98 . ? C136 H13E 0.98 . ? C136 H13F 0.98 . ? C137 H13G 0.98 . ? C137 H13H 0.98 . ? C137 H13I 0.98 . ? C138 C139 1.437(10) . ? C138 H138 0.95 . ? C139 C144 1.392(11) . ? C139 C140 1.507(10) . ? C140 C142 1.522(14) . ? C140 C143 1.545(12) . ? C140 C141 1.547(12) . ? C141 H14A 0.98 . ? C141 H14B 0.98 . ? C141 H14C 0.98 . ? C142 H14D 0.98 . ? C142 H14E 0.98 . ? C142 H14F 0.98 . ? C143 H14G 0.98 . ? C143 H14H 0.98 . ? C143 H14I 0.98 . ? C144 C145 1.357(12) . ? C144 H144 0.95 . ? C145 C146 1.495(11) . ? C146 H14J 0.99 . ? C146 H14K 0.99 . ? 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 N101 Zn1 O131 119.1(3) . . ? N101 Zn1 N121 120.6(3) . . ? O131 Zn1 N121 98.1(2) . . ? N101 Zn1 N111 130.9(3) . . ? O131 Zn1 N111 96.3(2) . . ? N121 Zn1 N111 82.8(3) . . ? N1 Si1 C2 112.2(4) . . ? N1 Si1 C3 109.9(3) . . ? C2 Si1 C3 108.5(4) . . ? N1 Si1 C1 115.0(4) . . ? C2 Si1 C1 104.1(4) . . ? C3 Si1 C1 106.7(4) . . ? N1 Si2 C4 113.3(4) . . ? N1 Si2 C5 113.2(3) . . ? C4 Si2 C5 106.3(4) . . ? N1 Si2 C6 110.9(3) . . ? C4 Si2 C6 107.8(4) . . ? C5 Si2 C6 104.8(4) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 N1 Si1 124.2(4) . . ? Si2 N1 Zn2 119.9(3) . . ? Si1 N1 Zn2 113.7(3) . . ? C12 N11 C46 106.1(6) . . ? C12 N11 C27 109.5(5) . . ? C46 N11 C27 109.2(5) . . ? C12 N11 Zn2 121.1(4) . . ? C46 N11 Zn2 104.5(4) . . ? C27 N11 Zn2 106.1(4) . . ? N11 C12 C13 116.0(6) . . ? N11 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N11 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C18 C13 C14 118.6(7) . . ? C18 C13 C12 119.4(7) . . ? C14 C13 C12 121.9(7) . . ? C13 C14 C15 118.7(7) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 121.2(8) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.5(8) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 119.4(8) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 122.5(8) . . ? C13 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C26 N21 C22 118.7(6) . . ? C26 N21 Zn2 115.1(5) . . ? C22 N21 Zn2 124.1(5) . . ? N21 C22 C23 121.5(7) . . ? N21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 119.6(7) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 117.8(7) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 120.0(7) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? N21 C26 C25 122.5(7) . . ? N21 C26 C27 115.9(6) . . ? C25 C26 C27 121.5(7) . . ? N11 C27 C26 115.7(6) . . ? N11 C27 H27A 108.4 . . ? C26 C27 H27A 108.4 . . ? N11 C27 H27B 108.4 . . ? C26 C27 H27B 108.4 . . ? H27A C27 H27B 107.4 . . ? C32 O31 Zn2 120.5(4) . . ? O31 C32 C45 120.6(7) . . ? O31 C32 C33 120.6(6) . . ? C45 C32 C33 118.7(6) . . ? C38 C33 C32 116.8(6) . . ? C38 C33 C34 123.6(6) . . ? C32 C33 C34 119.6(6) . . ? C35 C34 C36 114.1(7) . . ? C35 C34 C37 108.1(7) . . ? C36 C34 C37 107.6(7) . . ? C35 C34 C33 108.2(6) . . ? C36 C34 C33 109.2(6) . . ? C37 C34 C33 109.6(6) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C33 125.0(7) . . ? C39 C38 H38 117.5 . . ? C33 C38 H38 117.5 . . ? C38 C39 C44 117.7(7) . . ? C38 C39 C40 119.8(7) . . ? C44 C39 C40 122.4(7) . . ? C42 C40 C43 109.9(7) . . ? C42 C40 C41 110.1(7) . . ? C43 C40 C41 108.2(7) . . ? C42 C40 C39 110.3(7) . . ? C43 C40 C39 110.7(7) . . ? C41 C40 C39 107.7(7) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 C45 120.5(7) . . ? C39 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C32 C45 C44 121.3(7) . . ? C32 C45 C46 119.1(6) . . ? C44 C45 C46 118.9(6) . . ? N11 C46 C45 116.0(6) . . ? N11 C46 H46A 108.3 . . ? C45 C46 H46A 108.3 . . ? N11 C46 H46B 108.3 . . ? C45 C46 H46B 108.3 . . ? H46A C46 H46B 107.4 . . ? N1 Zn2 O31 118.7(2) . . ? N1 Zn2 N21 121.9(2) . . ? O31 Zn2 N21 98.0(2) . . ? N1 Zn2 N11 130.6(2) . . ? O31 Zn2 N11 96.3(2) . . ? N21 Zn2 N11 82.2(2) . . ? N101 Si11 C103 110.1(4) . . ? N101 Si11 C102 111.0(4) . . ? C103 Si11 C102 108.3(4) . . ? N101 Si11 C101 115.1(4) . . ? C103 Si11 C101 105.5(5) . . ? C102 Si11 C101 106.4(5) . . ? N101 Si12 C105 111.1(4) . . ? N101 Si12 C106 111.5(4) . . ? C105 Si12 C106 107.4(5) . . ? N101 Si12 C104 113.2(4) . . ? C105 Si12 C104 106.6(4) . . ? C106 Si12 C104 106.8(5) . . ? Si11 C101 H10A 109.5 . . ? Si11 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? Si11 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? Si11 C102 H10D 109.5 . . ? Si11 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? Si11 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? Si11 C103 H10G 109.5 . . ? Si11 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? Si11 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? Si12 C104 H10J 109.5 . . ? Si12 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? Si12 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? Si12 C105 H10M 109.5 . . ? Si12 C105 H10N 109.5 . . ? H10M C105 H10N 109.5 . . ? Si12 C105 H10O 109.5 . . ? H10M C105 H10O 109.5 . . ? H10N C105 H10O 109.5 . . ? Si12 C106 H10P 109.5 . . ? Si12 C106 H10Q 109.5 . . ? H10P C106 H10Q 109.5 . . ? Si12 C106 H10R 109.5 . . ? H10P C106 H10R 109.5 . . ? H10Q C106 H10R 109.5 . . ? Si11 N101 Si12 124.9(4) . . ? Si11 N101 Zn1 120.0(4) . . ? Si12 N101 Zn1 113.2(4) . . ? C127 N111 C146 110.6(6) . . ? C127 N111 C112 107.2(6) . . ? C146 N111 C112 107.7(6) . . ? C127 N111 Zn1 106.3(5) . . ? C146 N111 Zn1 104.7(4) . . ? C112 N111 Zn1 120.1(6) . . ? C113 C112 N111 114.0(7) . . ? C113 C112 H11A 108.8 . . ? N111 C112 H11A 108.8 . . ? C113 C112 H11B 108.8 . . ? N111 C112 H11B 108.8 . . ? H11A C112 H11B 107.7 . . ? C118 C113 C114 118.6(8) . . ? C118 C113 C112 123.2(9) . . ? C114 C113 C112 118.2(8) . . ? C115 C114 C113 118.7(9) . . ? C115 C114 H114 120.6 . . ? C113 C114 H114 120.6 . . ? C114 C115 C116 120.1(10) . . ? C114 C115 H115 120 . . ? C116 C115 H115 120 . . ? C117 C116 C115 120.8(8) . . ? C117 C116 H116 119.6 . . ? C115 C116 H116 119.6 . . ? C116 C117 C118 119.8(10) . . ? C116 C117 H117 120.1 . . ? C118 C117 H117 120.1 . . ? C113 C118 C117 121.9(9) . . ? C113 C118 H118 119.1 . . ? C117 C118 H118 119.1 . . ? C122 N121 C126 119.7(6) . . ? C122 N121 Zn1 124.7(5) . . ? C126 N121 Zn1 113.4(5) . . ? N121 C122 C123 120.9(7) . . ? N121 C122 H122 119.6 . . ? C123 C122 H122 119.6 . . ? C124 C123 C122 120.1(8) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 119.5(7) . . ? C123 C124 H124 120.3 . . ? C125 C124 H124 120.3 . . ? C126 C125 C124 118.5(8) . . ? C126 C125 H125 120.7 . . ? C124 C125 H125 120.7 . . ? C125 C126 N121 121.3(7) . . ? C125 C126 C127 123.4(7) . . ? N121 C126 C127 114.9(7) . . ? N111 C127 C126 116.1(6) . . ? N111 C127 H12C 108.3 . . ? C126 C127 H12C 108.3 . . ? N111 C127 H12D 108.2 . . ? C126 C127 H12D 108.3 . . ? H12C C127 H12D 107.4 . . ? C132 O131 Zn1 121.2(5) . . ? O131 C132 C133 122.5(7) . . ? O131 C132 C145 120.6(7) . . ? C133 C132 C145 116.9(7) . . ? C138 C133 C132 118.6(7) . . ? C138 C133 C134 118.9(7) . . ? C132 C133 C134 122.5(7) . . ? C137 C134 C133 116.1(7) . . ? C137 C134 C135 106.0(7) . . ? C133 C134 C135 109.3(6) . . ? C137 C134 C136 107.6(6) . . ? C133 C134 C136 110.8(6) . . ? C135 C134 C136 106.4(7) . . ? C134 C135 H13A 109.5 . . ? C134 C135 H13B 109.5 . . ? H13A C135 H13B 109.5 . . ? C134 C135 H13C 109.5 . . ? H13A C135 H13C 109.5 . . ? H13B C135 H13C 109.5 . . ? C134 C136 H13D 109.5 . . ? C134 C136 H13E 109.5 . . ? H13D C136 H13E 109.5 . . ? C134 C136 H13F 109.5 . . ? H13D C136 H13F 109.5 . . ? H13E C136 H13F 109.5 . . ? C134 C137 H13G 109.5 . . ? C134 C137 H13H 109.5 . . ? H13G C137 H13H 109.5 . . ? C134 C137 H13I 109.5 . . ? H13G C137 H13I 109.5 . . ? H13H C137 H13I 109.5 . . ? C133 C138 C139 124.9(7) . . ? C133 C138 H138 117.6 . . ? C139 C138 H138 117.6 . . ? C144 C139 C138 113.4(7) . . ? C144 C139 C140 125.9(7) . . ? C138 C139 C140 120.7(7) . . ? C139 C140 C142 109.8(7) . . ? C139 C140 C143 111.3(7) . . ? C142 C140 C143 109.8(8) . . ? C139 C140 C141 109.9(7) . . ? C142 C140 C141 109.6(8) . . ? C143 C140 C141 106.4(7) . . ? C140 C141 H14A 109.5 . . ? C140 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C140 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C140 C142 H14D 109.5 . . ? C140 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C140 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? C140 C143 H14G 109.5 . . ? C140 C143 H14H 109.5 . . ? H14G C143 H14H 109.5 . . ? C140 C143 H14I 109.5 . . ? H14G C143 H14I 109.5 . . ? H14H C143 H14I 109.5 . . ? C145 C144 C139 124.9(8) . . ? C145 C144 H144 117.5 . . ? C139 C144 H144 117.5 . . ? C144 C145 C132 121.2(8) . . ? C144 C145 C146 120.8(7) . . ? C132 C145 C146 117.4(7) . . ? C145 C146 N111 116.8(6) . . ? C145 C146 H14J 108.1 . . ? N111 C146 H14J 108.1 . . ? C145 C146 H14K 108.1 . . ? N111 C146 H14K 108.1 . . ? H14J C146 H14K 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Si2 N1 Si1 -58.9(5) . . . . ? C5 Si2 N1 Si1 62.2(6) . . . . ? C6 Si2 N1 Si1 179.7(4) . . . . ? C4 Si2 N1 Zn2 103.2(5) . . . . ? C5 Si2 N1 Zn2 -135.7(4) . . . . ? C6 Si2 N1 Zn2 -18.2(5) . . . . ? C2 Si1 N1 Si2 97.0(5) . . . . ? C3 Si1 N1 Si2 -142.1(4) . . . . ? C1 Si1 N1 Si2 -21.7(6) . . . . ? C2 Si1 N1 Zn2 -66.1(5) . . . . ? C3 Si1 N1 Zn2 54.8(5) . . . . ? C1 Si1 N1 Zn2 175.2(4) . . . . ? C46 N11 C12 C13 -57.2(7) . . . . ? C27 N11 C12 C13 -174.9(6) . . . . ? Zn2 N11 C12 C13 61.4(7) . . . . ? N11 C12 C13 C18 115.4(8) . . . . ? N11 C12 C13 C14 -66.5(9) . . . . ? C18 C13 C14 C15 1.7(11) . . . . ? C12 C13 C14 C15 -176.4(7) . . . . ? C13 C14 C15 C16 -2.1(11) . . . . ? C14 C15 C16 C17 2.1(12) . . . . ? C15 C16 C17 C18 -1.7(12) . . . . ? C14 C13 C18 C17 -1.3(12) . . . . ? C12 C13 C18 C17 176.8(7) . . . . ? C16 C17 C18 C13 1.3(12) . . . . ? C26 N21 C22 C23 -0.8(11) . . . . ? Zn2 N21 C22 C23 -163.5(6) . . . . ? N21 C22 C23 C24 1.7(12) . . . . ? C22 C23 C24 C25 -1.3(12) . . . . ? C23 C24 C25 C26 0.3(12) . . . . ? C22 N21 C26 C25 -0.3(11) . . . . ? Zn2 N21 C26 C25 163.9(6) . . . . ? C22 N21 C26 C27 176.2(6) . . . . ? Zn2 N21 C26 C27 -19.6(8) . . . . ? C24 C25 C26 N21 0.6(12) . . . . ? C24 C25 C26 C27 -175.7(7) . . . . ? C12 N11 C27 C26 -150.9(6) . . . . ? C46 N11 C27 C26 93.4(7) . . . . ? Zn2 N11 C27 C26 -18.7(7) . . . . ? N21 C26 C27 N11 26.6(9) . . . . ? C25 C26 C27 N11 -156.9(7) . . . . ? Zn2 O31 C32 C45 42.0(8) . . . . ? Zn2 O31 C32 C33 -139.5(5) . . . . ? O31 C32 C33 C38 -178.5(6) . . . . ? C45 C32 C33 C38 0.0(10) . . . . ? O31 C32 C33 C34 2.8(10) . . . . ? C45 C32 C33 C34 -178.7(6) . . . . ? C38 C33 C34 C35 -112.2(7) . . . . ? C32 C33 C34 C35 66.4(8) . . . . ? C38 C33 C34 C36 123.0(7) . . . . ? C32 C33 C34 C36 -58.3(8) . . . . ? C38 C33 C34 C37 5.5(10) . . . . ? C32 C33 C34 C37 -175.9(7) . . . . ? C32 C33 C38 C39 -1.5(11) . . . . ? C34 C33 C38 C39 177.1(7) . . . . ? C33 C38 C39 C44 2.3(12) . . . . ? C33 C38 C39 C40 178.2(7) . . . . ? C38 C39 C40 C42 48.5(10) . . . . ? C44 C39 C40 C42 -135.8(8) . . . . ? C38 C39 C40 C43 170.3(7) . . . . ? C44 C39 C40 C43 -14.0(11) . . . . ? C38 C39 C40 C41 -71.6(9) . . . . ? C44 C39 C40 C41 104.1(9) . . . . ? C38 C39 C44 C45 -1.6(11) . . . . ? C40 C39 C44 C45 -177.4(7) . . . . ? O31 C32 C45 C44 179.1(6) . . . . ? C33 C32 C45 C44 0.7(10) . . . . ? O31 C32 C45 C46 9.3(10) . . . . ? C33 C32 C45 C46 -169.2(6) . . . . ? C39 C44 C45 C32 0.1(11) . . . . ? C39 C44 C45 C46 170.0(7) . . . . ? C12 N11 C46 C45 -173.7(5) . . . . ? C27 N11 C46 C45 -55.8(7) . . . . ? Zn2 N11 C46 C45 57.3(6) . . . . ? C32 C45 C46 N11 -68.7(8) . . . . ? C44 C45 C46 N11 121.2(7) . . . . ? Si2 N1 Zn2 O31 -168.4(3) . . . . ? Si1 N1 Zn2 O31 -4.5(4) . . . . ? Si2 N1 Zn2 N21 -46.5(5) . . . . ? Si1 N1 Zn2 N21 117.3(3) . . . . ? Si2 N1 Zn2 N11 62.3(5) . . . . ? Si1 N1 Zn2 N11 -133.9(3) . . . . ? C32 O31 Zn2 N1 179.7(5) . . . . ? C32 O31 Zn2 N21 46.5(5) . . . . ? C32 O31 Zn2 N11 -36.5(5) . . . . ? C26 N21 Zn2 N1 140.4(5) . . . . ? C22 N21 Zn2 N1 -56.4(6) . . . . ? C26 N21 Zn2 O31 -88.5(5) . . . . ? C22 N21 Zn2 O31 74.8(6) . . . . ? C26 N21 Zn2 N11 6.9(5) . . . . ? C22 N21 Zn2 N11 170.1(6) . . . . ? C12 N11 Zn2 N1 6.4(6) . . . . ? C46 N11 Zn2 N1 125.7(5) . . . . ? C27 N11 Zn2 N1 -118.9(4) . . . . ? C12 N11 Zn2 O31 -130.5(5) . . . . ? C46 N11 Zn2 O31 -11.2(5) . . . . ? C27 N11 Zn2 O31 104.1(4) . . . . ? C12 N11 Zn2 N21 132.2(5) . . . . ? C46 N11 Zn2 N21 -108.5(5) . . . . ? C27 N11 Zn2 N21 6.9(4) . . . . ? C103 Si11 N101 Si12 179.0(5) . . . . ? C102 Si11 N101 Si12 -61.1(6) . . . . ? C101 Si11 N101 Si12 59.9(7) . . . . ? C103 Si11 N101 Zn1 -18.0(6) . . . . ? C102 Si11 N101 Zn1 101.9(5) . . . . ? C101 Si11 N101 Zn1 -137.1(6) . . . . ? C105 Si12 N101 Si11 -141.9(5) . . . . ? C106 Si12 N101 Si11 98.4(6) . . . . ? C104 Si12 N101 Si11 -22.0(6) . . . . ? C105 Si12 N101 Zn1 54.2(5) . . . . ? C106 Si12 N101 Zn1 -65.6(5) . . . . ? C104 Si12 N101 Zn1 174.0(4) . . . . ? O131 Zn1 N101 Si11 -168.6(3) . . . . ? N121 Zn1 N101 Si11 -47.5(5) . . . . ? N111 Zn1 N101 Si11 61.1(6) . . . . ? O131 Zn1 N101 Si12 -3.7(5) . . . . ? N121 Zn1 N101 Si12 117.3(4) . . . . ? N111 Zn1 N101 Si12 -134.0(4) . . . . ? N101 Zn1 N111 C127 -116.3(5) . . . . ? O131 Zn1 N111 C127 105.8(5) . . . . ? N121 Zn1 N111 C127 8.4(5) . . . . ? N101 Zn1 N111 C146 126.6(5) . . . . ? O131 Zn1 N111 C146 -11.3(5) . . . . ? N121 Zn1 N111 C146 -108.7(5) . . . . ? N101 Zn1 N111 C112 5.4(7) . . . . ? O131 Zn1 N111 C112 -132.4(5) . . . . ? N121 Zn1 N111 C112 130.2(5) . . . . ? C127 N111 C112 C113 -174.9(7) . . . . ? C146 N111 C112 C113 -55.8(9) . . . . ? Zn1 N111 C112 C113 63.8(9) . . . . ? N111 C112 C113 C118 -72.5(10) . . . . ? N111 C112 C113 C114 109.8(9) . . . . ? C118 C113 C114 C115 -0.6(12) . . . . ? C112 C113 C114 C115 177.2(8) . . . . ? C113 C114 C115 C116 -0.3(13) . . . . ? C114 C115 C116 C117 0.8(13) . . . . ? C115 C116 C117 C118 -0.5(14) . . . . ? C114 C113 C118 C117 0.9(13) . . . . ? C112 C113 C118 C117 -176.7(8) . . . . ? C116 C117 C118 C113 -0.4(14) . . . . ? N101 Zn1 N121 C122 -56.1(7) . . . . ? O131 Zn1 N121 C122 74.8(6) . . . . ? N111 Zn1 N121 C122 170.1(6) . . . . ? N101 Zn1 N121 C126 140.5(5) . . . . ? O131 Zn1 N121 C126 -88.6(5) . . . . ? N111 Zn1 N121 C126 6.7(5) . . . . ? C126 N121 C122 C123 -1.6(11) . . . . ? Zn1 N121 C122 C123 -164.0(6) . . . . ? N121 C122 C123 C124 0.1(12) . . . . ? C122 C123 C124 C125 0.8(12) . . . . ? C123 C124 C125 C126 -0.2(13) . . . . ? C124 C125 C126 N121 -1.3(12) . . . . ? C124 C125 C126 C127 -173.0(8) . . . . ? C122 N121 C126 C125 2.3(11) . . . . ? Zn1 N121 C126 C125 166.6(6) . . . . ? C122 N121 C126 C127 174.6(7) . . . . ? Zn1 N121 C126 C127 -21.1(8) . . . . ? C146 N111 C127 C126 90.9(9) . . . . ? C112 N111 C127 C126 -151.9(7) . . . . ? Zn1 N111 C127 C126 -22.2(8) . . . . ? C125 C126 C127 N111 -157.7(8) . . . . ? N121 C126 C127 N111 30.1(10) . . . . ? N101 Zn1 O131 C132 178.3(5) . . . . ? N121 Zn1 O131 C132 46.4(6) . . . . ? N111 Zn1 O131 C132 -37.2(6) . . . . ? Zn1 O131 C132 C133 -139.1(6) . . . . ? Zn1 O131 C132 C145 43.4(9) . . . . ? O131 C132 C133 C138 -177.7(7) . . . . ? C145 C132 C133 C138 -0.2(10) . . . . ? O131 C132 C133 C134 2.6(11) . . . . ? C145 C132 C133 C134 -179.9(7) . . . . ? C138 C133 C134 C137 4.1(10) . . . . ? C132 C133 C134 C137 -176.2(7) . . . . ? C138 C133 C134 C135 -115.7(8) . . . . ? C132 C133 C134 C135 64.0(9) . . . . ? C138 C133 C134 C136 127.3(7) . . . . ? C132 C133 C134 C136 -53.0(9) . . . . ? C132 C133 C138 C139 -0.1(11) . . . . ? C134 C133 C138 C139 179.6(7) . . . . ? C133 C138 C139 C144 -1.2(11) . . . . ? C133 C138 C139 C140 176.7(7) . . . . ? C144 C139 C140 C142 107.9(9) . . . . ? C138 C139 C140 C142 -69.8(9) . . . . ? C144 C139 C140 C143 -13.8(12) . . . . ? C138 C139 C140 C143 168.5(8) . . . . ? C144 C139 C140 C141 -131.5(9) . . . . ? C138 C139 C140 C141 50.9(11) . . . . ? C138 C139 C144 C145 3.0(12) . . . . ? C140 C139 C144 C145 -174.8(8) . . . . ? C139 C144 C145 C132 -3.5(13) . . . . ? C139 C144 C145 C146 168.1(7) . . . . ? O131 C132 C145 C144 179.4(7) . . . . ? C133 C132 C145 C144 1.9(11) . . . . ? O131 C132 C145 C146 7.6(10) . . . . ? C133 C132 C145 C146 -170.0(6) . . . . ? C144 C145 C146 N111 120.7(8) . . . . ? C132 C145 C146 N111 -67.4(9) . . . . ? C127 N111 C146 C145 -56.1(9) . . . . ? C112 N111 C146 C145 -173.0(7) . . . . ? Zn1 N111 C146 C145 58.0(7) . . . . ? # Attachment 'complex7_ZG56.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-08-27 at 09:41:10 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : f:\progs\wingx\files\archive.dat # CIF files read : job_renum struct data_job_renum _database_code_depnum_ccdc_archive 'CCDC 672305' _audit_creation_date 2008-08-27T09:41:10-00:00 _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 'C58 H72 N2 O2 Zn' _chemical_formula_sum 'C58 H72 N2 O2 Zn' _chemical_formula_weight 894.55 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # 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 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.646(2) _cell_length_b 14.508(3) _cell_length_c 16.750(4) _cell_angle_alpha 85.050(10) _cell_angle_beta 75.882(10) _cell_angle_gamma 80.339(10) _cell_volume 2470.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8229 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.33 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.540 _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 0.823 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------------# # 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 0.0512 _diffrn_reflns_av_unetI/netI 0.0595 _diffrn_reflns_number 33514 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 11241 _reflns_number_gt 8736 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0281P)^2^+1.1081P] 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 11241 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.3 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 0.26795(2) 0.372515(15) 0.784635(13) 0.01643(6) Uani 1 d . . . O1 O 0.30981(11) 0.47106(8) 0.83606(7) 0.0182(3) Uani 1 d . . . N1 N 0.09346(14) 0.44174(10) 0.75427(9) 0.0155(3) Uani 1 d . . . C1 C 0.13237(17) 0.47354(12) 0.66527(11) 0.0170(4) Uani 1 d . . . H1A H 0.1585 0.4172 0.6321 0.02 Uiso 1 calc R . . H1B H 0.2111 0.5042 0.6578 0.02 Uiso 1 calc R . . C2 C 0.03163(16) 0.53998(13) 0.62953(11) 0.0169(4) Uani 1 d . . . C3 C 0.04854(18) 0.63261(13) 0.61259(12) 0.0215(4) Uani 1 d . . . H3 H 0.1164 0.655 0.6295 0.026 Uiso 1 calc R . . C4 C -0.03203(19) 0.69336(14) 0.57124(13) 0.0260(4) Uani 1 d . . . H4 H -0.0174 0.7564 0.5588 0.031 Uiso 1 calc R . . C5 C -0.13380(18) 0.66272(14) 0.54804(12) 0.0241(4) Uani 1 d . . . H5 H -0.1896 0.7046 0.5203 0.029 Uiso 1 calc R . . C6 C -0.15327(18) 0.57076(13) 0.56569(12) 0.0222(4) Uani 1 d . . . H6 H -0.2236 0.5493 0.5508 0.027 Uiso 1 calc R . . C7 C -0.07049(17) 0.50954(13) 0.60516(11) 0.0198(4) Uani 1 d . . . H7 H -0.0834 0.446 0.6158 0.024 Uiso 1 calc R . . N11 N 0.32397(15) 0.25641(10) 0.85728(9) 0.0186(3) Uani 1 d . . . C11 C -0.02235(17) 0.39164(13) 0.77118(11) 0.0184(4) Uani 1 d . . . H11A H -0.0982 0.4373 0.7619 0.022 Uiso 1 calc R . . H11B H -0.0419 0.3719 0.8304 0.022 Uiso 1 calc R . . C12 C -0.01410(18) 0.30657(13) 0.72253(11) 0.0198(4) Uani 1 d . . . C13 C -0.1330(2) 0.27989(14) 0.71881(13) 0.0265(4) Uani 1 d . . . H13 H -0.2135 0.3162 0.7443 0.032 Uiso 1 calc R . . C14 C -0.1340(2) 0.20101(15) 0.67817(14) 0.0355(5) Uani 1 d . . . H14 H -0.2151 0.1838 0.6755 0.043 Uiso 1 calc R . . C15 C -0.0170(3) 0.14682(15) 0.64122(14) 0.0383(6) Uani 1 d . . . H15 H -0.0182 0.0926 0.6135 0.046 Uiso 1 calc R . . C16 C 0.1003(2) 0.17177(14) 0.64486(13) 0.0321(5) Uani 1 d . . . H16 H 0.1803 0.1345 0.62 0.038 Uiso 1 calc R . . C17 C 0.1023(2) 0.25158(13) 0.68497(11) 0.0231(4) Uani 1 d . . . H17 H 0.1839 0.2687 0.6867 0.028 Uiso 1 calc R . . C21 C 0.05145(17) 0.52418(12) 0.80984(11) 0.0179(4) Uani 1 d . . . H21A H -0.0312 0.5596 0.7991 0.022 Uiso 1 calc R . . H21B H 0.0318 0.4993 0.8677 0.022 Uiso 1 calc R . . C22 C 0.14747(17) 0.59166(13) 0.80147(11) 0.0173(4) Uani 1 d . A . C23 C 0.27457(17) 0.56086(12) 0.81388(10) 0.0159(4) Uani 1 d . . . C24 C 0.36181(17) 0.62683(13) 0.80540(11) 0.0172(4) Uani 1 d . . . C25 C 0.50636(17) 0.59352(13) 0.80921(11) 0.0202(4) Uani 1 d . . . C26 C 0.56977(18) 0.51976(14) 0.74439(12) 0.0265(4) Uani 1 d . . . H26A H 0.5638 0.5468 0.6895 0.04 Uiso 1 calc R . . H26B H 0.5237 0.4653 0.757 0.04 Uiso 1 calc R . . H26C H 0.6621 0.5003 0.7455 0.04 Uiso 1 calc R . . C27 C 0.51468(19) 0.55216(14) 0.89553(12) 0.0255(4) Uani 1 d . . . H27A H 0.6062 0.5281 0.8959 0.038 Uiso 1 calc R . . H27B H 0.4624 0.501 0.9102 0.038 Uiso 1 calc R . . H27C H 0.4807 0.601 0.9356 0.038 Uiso 1 calc R . . C28 C 0.58787(19) 0.67370(15) 0.78940(13) 0.0294(5) Uani 1 d . . . H28A H 0.5514 0.7219 0.8298 0.044 Uiso 1 calc R . . H28B H 0.5857 0.7009 0.734 0.044 Uiso 1 calc R . . H28C H 0.6787 0.6496 0.7917 0.044 Uiso 1 calc R . . C29 C 0.31258(17) 0.72063(13) 0.79355(11) 0.0199(4) Uani 1 d . . . H29 H 0.3702 0.7652 0.7891 0.024 Uiso 1 calc R . . C30 C 0.18309(18) 0.75378(13) 0.78778(11) 0.0198(4) Uani 1 d . A . C31 C 0.12773(18) 0.85828(13) 0.78059(12) 0.0221(4) Uani 1 d . . . C32A C 0.1041(10) 0.8849(10) 0.6962(7) 0.055(3) Uani 0.5 d P A 1 H32A H 0.051 0.8421 0.6826 0.082 Uiso 0.5 calc PR A 1 H32B H 0.1882 0.8808 0.6556 0.082 Uiso 0.5 calc PR A 1 H32C H 0.0575 0.9491 0.6954 0.082 Uiso 0.5 calc PR A 1 C33A C 0.2088(6) 0.9235(4) 0.8036(5) 0.0562(19) Uani 0.5 d P A 1 H33A H 0.1677 0.9885 0.7967 0.084 Uiso 0.5 calc PR A 1 H33B H 0.2973 0.9143 0.7678 0.084 Uiso 0.5 calc PR A 1 H33C H 0.2139 0.9101 0.8611 0.084 Uiso 0.5 calc PR A 1 C34A C -0.0127(6) 0.8811(4) 0.8438(4) 0.0397(15) Uani 0.5 d P A 1 H34A H -0.0037 0.8637 0.9001 0.06 Uiso 0.5 calc PR A 1 H34B H -0.0745 0.8454 0.8302 0.06 Uiso 0.5 calc PR A 1 H34C H -0.0454 0.9482 0.8393 0.06 Uiso 0.5 calc PR A 1 C32B C 0.0527(9) 0.8773(9) 0.7126(6) 0.035(2) Uani 0.5 d P A 2 H32D H -0.0225 0.8432 0.7265 0.052 Uiso 0.5 calc PR A 2 H32E H 0.1107 0.8563 0.6603 0.052 Uiso 0.5 calc PR A 2 H32F H 0.0217 0.9446 0.7073 0.052 Uiso 0.5 calc PR A 2 C33B C 0.2433(6) 0.9172(4) 0.7545(3) 0.0317(12) Uani 0.5 d P A 2 H33D H 0.2077 0.9837 0.7494 0.048 Uiso 0.5 calc PR A 2 H33E H 0.2994 0.8969 0.7014 0.048 Uiso 0.5 calc PR A 2 H33F H 0.295 0.9077 0.7964 0.048 Uiso 0.5 calc PR A 2 C34B C 0.0464(6) 0.8856(4) 0.8618(4) 0.0354(13) Uani 0.5 d P A 2 H34D H 0.0105 0.9523 0.8591 0.053 Uiso 0.5 calc PR A 2 H34E H 0.1002 0.8742 0.9026 0.053 Uiso 0.5 calc PR A 2 H34F H -0.0255 0.8486 0.878 0.053 Uiso 0.5 calc PR A 2 C35 C 0.10386(17) 0.68649(13) 0.78978(11) 0.0191(4) Uani 1 d . . . H35 H 0.0172 0.7058 0.783 0.023 Uiso 1 calc R A . O51 O 0.38231(12) 0.32652(9) 0.68480(8) 0.0209(3) Uani 1 d . . . C51 C 0.23705(19) 0.24805(14) 0.94186(11) 0.0232(4) Uani 1 d . . . H51A H 0.2578 0.292 0.9771 0.028 Uiso 1 calc R . . H51B H 0.2588 0.1839 0.9652 0.028 Uiso 1 calc R . . C52 C 0.09088(19) 0.26716(14) 0.94726(11) 0.0250(4) Uani 1 d . . . C53 C 0.0185(2) 0.34948(15) 0.98269(11) 0.0276(5) Uani 1 d . . . H53 H 0.0628 0.3939 0.9986 0.033 Uiso 1 calc R . . C54 C -0.1179(2) 0.36733(17) 0.99511(12) 0.0343(5) Uani 1 d . . . H54 H -0.1656 0.4234 1.0193 0.041 Uiso 1 calc R . . C55 C -0.1826(2) 0.30355(18) 0.97221(13) 0.0388(6) Uani 1 d . . . H55 H -0.2752 0.3158 0.9802 0.047 Uiso 1 calc R . . C56 C -0.1129(2) 0.22100(18) 0.93731(13) 0.0382(6) Uani 1 d . . . H56 H -0.1581 0.1772 0.9212 0.046 Uiso 1 calc R . . C57 C 0.0226(2) 0.20241(15) 0.92602(12) 0.0316(5) Uani 1 d . . . H57 H 0.0692 0.1451 0.9036 0.038 Uiso 1 calc R . . C61 C 0.45964(18) 0.26631(13) 0.86523(12) 0.0215(4) Uani 1 d . . . H61A H 0.4536 0.3257 0.8919 0.026 Uiso 1 calc R . . H61B H 0.5163 0.2717 0.8091 0.026 Uiso 1 calc R . . C62 C 0.52655(19) 0.18805(13) 0.91323(13) 0.0247(4) Uani 1 d . . . C63 C 0.5090(2) 0.19080(16) 0.99810(13) 0.0325(5) Uani 1 d . . . H63 H 0.4536 0.2421 1.0263 0.039 Uiso 1 calc R . . C64 C 0.5711(2) 0.11992(17) 1.04224(16) 0.0430(6) Uani 1 d . . . H64 H 0.5577 0.1228 1.1002 0.052 Uiso 1 calc R . . C65 C 0.6520(2) 0.04526(17) 1.00223(18) 0.0473(7) Uani 1 d . . . H65 H 0.6941 -0.0034 1.0326 0.057 Uiso 1 calc R . . C66 C 0.6719(2) 0.04117(16) 0.91831(18) 0.0459(7) Uani 1 d . . . H66 H 0.7279 -0.0103 0.8908 0.055 Uiso 1 calc R . . C67 C 0.6101(2) 0.11249(15) 0.87350(15) 0.0345(5) Uani 1 d . . . H67 H 0.625 0.1096 0.8154 0.041 Uiso 1 calc R . . C71 C 0.32726(18) 0.17331(13) 0.80878(11) 0.0197(4) Uani 1 d . . . H71A H 0.239 0.1752 0.7987 0.024 Uiso 1 calc R . . H71B H 0.3448 0.116 0.8434 0.024 Uiso 1 calc R . . C72 C 0.42636(17) 0.16453(13) 0.72666(11) 0.0179(4) Uani 1 d . B . C73 C 0.44649(17) 0.24010(12) 0.66940(11) 0.0167(4) Uani 1 d . . . C74 C 0.53814(16) 0.22273(13) 0.59234(11) 0.0168(4) Uani 1 d . . . C75 C 0.56643(17) 0.30183(13) 0.52726(11) 0.0185(4) Uani 1 d . . . C76 C 0.65739(19) 0.26565(14) 0.44644(12) 0.0259(4) Uani 1 d . . . H76A H 0.743 0.2379 0.4563 0.039 Uiso 1 calc R . . H76B H 0.6682 0.3178 0.4053 0.039 Uiso 1 calc R . . H76C H 0.619 0.2182 0.4261 0.039 Uiso 1 calc R . . C77 C 0.6327(2) 0.37228(13) 0.55945(12) 0.0250(4) Uani 1 d . . . H77A H 0.5747 0.3983 0.6099 0.037 Uiso 1 calc R . . H77B H 0.6503 0.4229 0.5176 0.037 Uiso 1 calc R . . H77C H 0.7153 0.3406 0.5714 0.037 Uiso 1 calc R . . C78 C 0.43953(19) 0.35186(16) 0.50415(12) 0.0300(5) Uani 1 d . . . H78A H 0.3988 0.3066 0.4827 0.045 Uiso 1 calc R . . H78B H 0.4605 0.4016 0.4619 0.045 Uiso 1 calc R . . H78C H 0.3787 0.3791 0.5532 0.045 Uiso 1 calc R . . C79 C 0.60427(17) 0.13219(13) 0.57824(12) 0.0207(4) Uani 1 d . . . H79 H 0.6651 0.1213 0.5269 0.025 Uiso 1 calc R . . C80 C 0.58673(17) 0.05682(13) 0.63468(12) 0.0212(4) Uani 1 d . B . C81 C 0.6637(2) -0.04149(14) 0.61532(16) 0.0342(5) Uani 1 d . . . C82A C 0.7756(7) -0.0458(6) 0.5493(5) 0.0327(16) Uani 0.5 d P B 1 H82A H 0.8323 -0.0026 0.5576 0.049 Uiso 0.5 calc PR B 1 H82B H 0.7485 -0.0281 0.4975 0.049 Uiso 0.5 calc PR B 1 H82C H 0.8236 -0.1097 0.5468 0.049 Uiso 0.5 calc PR B 1 C83A C 0.7243(4) -0.0799(3) 0.6995(3) 0.0320(10) Uani 0.5 d P B 1 H83A H 0.6516 -0.0841 0.7479 0.048 Uiso 0.5 calc PR B 1 H83B H 0.779 -0.0358 0.7091 0.048 Uiso 0.5 calc PR B 1 H83C H 0.7772 -0.1418 0.69 0.048 Uiso 0.5 calc PR B 1 C84A C 0.5731(4) -0.1107(3) 0.6140(3) 0.0310(10) Uani 0.5 d P B 1 H84A H 0.6237 -0.1736 0.6068 0.047 Uiso 0.5 calc PR B 1 H84B H 0.53 -0.0934 0.5683 0.047 Uiso 0.5 calc PR B 1 H84C H 0.5066 -0.11 0.6661 0.047 Uiso 0.5 calc PR B 1 C82B C 0.8092(7) -0.0342(6) 0.5689(6) 0.0330(17) Uani 0.5 d P B 2 H82D H 0.8553 -0.0142 0.6068 0.05 Uiso 0.5 calc PR B 2 H82E H 0.8099 0.0116 0.5223 0.05 Uiso 0.5 calc PR B 2 H82F H 0.8533 -0.0955 0.5486 0.05 Uiso 0.5 calc PR B 2 C83B C 0.6500(5) -0.1078(3) 0.6777(3) 0.0380(11) Uani 0.5 d P B 2 H83D H 0.7015 -0.1675 0.6582 0.057 Uiso 0.5 calc PR B 2 H83E H 0.5574 -0.1151 0.6969 0.057 Uiso 0.5 calc PR B 2 H83F H 0.6811 -0.0887 0.7233 0.057 Uiso 0.5 calc PR B 2 C84B C 0.6055(5) -0.0733(3) 0.5384(3) 0.0394(12) Uani 0.5 d P B 2 H84D H 0.6438 -0.138 0.5252 0.059 Uiso 0.5 calc PR B 2 H84E H 0.6291 -0.0318 0.4895 0.059 Uiso 0.5 calc PR B 2 H84F H 0.5099 -0.0685 0.5558 0.059 Uiso 0.5 calc PR B 2 C85 C 0.49572(17) 0.07519(13) 0.70844(12) 0.0198(4) Uani 1 d . . . H85 H 0.4799 0.0251 0.7482 0.024 Uiso 1 calc R B . 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 0.01828(11) 0.01563(11) 0.01449(10) -0.00078(8) -0.00435(8) 0.00075(8) O1 0.0204(6) 0.0155(6) 0.0191(6) -0.0001(5) -0.0076(5) 0.0002(5) N1 0.0170(7) 0.0144(7) 0.0152(7) -0.0015(6) -0.0030(6) -0.0033(6) C1 0.0164(8) 0.0165(9) 0.0170(9) 0.0001(7) -0.0030(7) -0.0013(7) C2 0.0156(8) 0.0199(9) 0.0139(8) 0.0003(7) -0.0022(7) -0.0008(7) C3 0.0188(9) 0.0227(10) 0.0252(10) 0.0024(8) -0.0095(8) -0.0050(8) C4 0.0265(10) 0.0184(10) 0.0339(11) 0.0054(9) -0.0111(9) -0.0026(8) C5 0.0206(9) 0.0236(10) 0.0278(10) 0.0020(8) -0.0097(8) 0.0019(8) C6 0.0185(9) 0.0262(10) 0.0233(10) -0.0005(8) -0.0082(8) -0.0029(8) C7 0.0204(9) 0.0191(9) 0.0212(9) -0.0003(8) -0.0065(8) -0.0041(7) N11 0.0242(8) 0.0166(8) 0.0156(7) -0.0008(6) -0.0065(6) -0.0017(6) C11 0.0179(9) 0.0199(9) 0.0176(9) -0.0003(7) -0.0041(7) -0.0041(7) C12 0.0302(10) 0.0165(9) 0.0145(8) 0.0026(7) -0.0090(8) -0.0045(8) C13 0.0322(11) 0.0218(10) 0.0300(11) 0.0025(9) -0.0151(9) -0.0072(8) C14 0.0544(14) 0.0250(11) 0.0392(13) 0.0056(10) -0.0301(11) -0.0158(10) C15 0.0726(17) 0.0184(11) 0.0325(12) -0.0027(9) -0.0280(12) -0.0070(11) C16 0.0510(14) 0.0212(11) 0.0243(11) -0.0047(9) -0.0144(10) 0.0037(10) C17 0.0315(10) 0.0199(10) 0.0190(9) 0.0007(8) -0.0098(8) -0.0021(8) C21 0.0167(9) 0.0179(9) 0.0183(9) -0.0043(7) -0.0031(7) -0.0003(7) C22 0.0165(9) 0.0193(9) 0.0157(8) -0.0039(7) -0.0030(7) -0.0011(7) C23 0.0186(9) 0.0169(9) 0.0115(8) -0.0014(7) -0.0035(7) -0.0003(7) C24 0.0179(9) 0.0192(9) 0.0142(8) 0.0009(7) -0.0043(7) -0.0020(7) C25 0.0174(9) 0.0231(10) 0.0209(9) 0.0014(8) -0.0067(7) -0.0028(7) C26 0.0174(9) 0.0335(12) 0.0269(10) -0.0030(9) -0.0052(8) 0.0015(8) C27 0.0240(10) 0.0270(11) 0.0283(11) 0.0023(9) -0.0127(8) -0.0039(8) C28 0.0217(10) 0.0336(12) 0.0351(12) 0.0045(10) -0.0109(9) -0.0066(9) C29 0.0204(9) 0.0203(10) 0.0215(9) 0.0007(8) -0.0075(8) -0.0064(7) C30 0.0227(9) 0.0180(9) 0.0197(9) -0.0001(8) -0.0073(8) -0.0027(7) C31 0.0253(10) 0.0165(9) 0.0263(10) -0.0002(8) -0.0112(8) -0.0012(8) C32A 0.095(9) 0.026(4) 0.030(4) -0.001(3) -0.010(5) 0.021(6) C33A 0.035(3) 0.019(3) 0.123(7) -0.008(4) -0.036(4) -0.001(2) C34A 0.040(4) 0.022(3) 0.042(4) 0.000(2) 0.009(3) 0.006(3) C32B 0.053(5) 0.017(3) 0.040(6) -0.002(4) -0.029(4) 0.006(4) C33B 0.033(3) 0.016(2) 0.045(3) 0.005(2) -0.011(3) -0.001(2) C34B 0.044(4) 0.018(2) 0.035(3) -0.001(2) 0.000(3) 0.010(3) C35 0.0161(9) 0.0207(10) 0.0203(9) -0.0035(8) -0.0061(7) 0.0012(7) O51 0.0246(7) 0.0166(7) 0.0169(6) -0.0002(5) -0.0026(5) 0.0061(5) C51 0.0329(11) 0.0230(10) 0.0138(9) 0.0008(8) -0.0064(8) -0.0043(8) C52 0.0329(11) 0.0293(11) 0.0121(9) 0.0032(8) -0.0024(8) -0.0091(9) C53 0.0339(11) 0.0341(12) 0.0144(9) -0.0010(8) -0.0043(8) -0.0062(9) C54 0.0345(12) 0.0465(14) 0.0162(10) -0.0017(10) 0.0019(9) -0.0019(10) C55 0.0296(11) 0.0566(16) 0.0255(11) 0.0037(11) 0.0044(9) -0.0126(11) C56 0.0393(13) 0.0498(15) 0.0279(11) 0.0042(11) -0.0024(10) -0.0247(11) C57 0.0412(12) 0.0308(12) 0.0211(10) 0.0021(9) 0.0008(9) -0.0141(10) C61 0.0280(10) 0.0194(10) 0.0199(9) 0.0005(8) -0.0117(8) -0.0034(8) C62 0.0324(11) 0.0179(10) 0.0305(11) 0.0020(8) -0.0196(9) -0.0062(8) C63 0.0424(12) 0.0311(12) 0.0315(12) 0.0056(10) -0.0218(10) -0.0109(10) C64 0.0537(15) 0.0447(15) 0.0442(14) 0.0205(12) -0.0356(12) -0.0215(12) C65 0.0550(16) 0.0298(13) 0.0754(19) 0.0234(13) -0.0520(15) -0.0168(12) C66 0.0467(14) 0.0215(12) 0.084(2) -0.0077(12) -0.0459(14) 0.0011(10) C67 0.0389(12) 0.0250(11) 0.0491(14) -0.0078(10) -0.0309(11) 0.0021(9) C71 0.0259(10) 0.0157(9) 0.0179(9) -0.0002(7) -0.0075(8) -0.0016(7) C72 0.0198(9) 0.0179(9) 0.0182(9) -0.0018(7) -0.0092(7) -0.0011(7) C73 0.0175(9) 0.0160(9) 0.0180(9) -0.0023(7) -0.0091(7) 0.0015(7) C74 0.0135(8) 0.0191(9) 0.0201(9) -0.0039(7) -0.0075(7) -0.0019(7) C75 0.0156(8) 0.0224(10) 0.0176(9) -0.0040(8) -0.0043(7) -0.0014(7) C76 0.0260(10) 0.0294(11) 0.0214(10) -0.0075(9) 0.0018(8) -0.0090(8) C77 0.0349(11) 0.0190(10) 0.0226(10) -0.0016(8) -0.0077(9) -0.0067(8) C78 0.0212(10) 0.0451(13) 0.0212(10) 0.0089(9) -0.0067(8) -0.0003(9) C79 0.0144(8) 0.0219(10) 0.0268(10) -0.0085(8) -0.0040(8) -0.0028(7) C80 0.0180(9) 0.0170(9) 0.0311(10) -0.0070(8) -0.0092(8) -0.0015(7) C81 0.0242(10) 0.0166(10) 0.0605(15) -0.0132(10) -0.0055(10) -0.0006(8) C82A 0.029(4) 0.023(3) 0.039(4) -0.007(3) 0.000(3) 0.006(3) C83A 0.035(2) 0.021(2) 0.038(2) -0.0067(19) -0.016(2) 0.0130(18) C84A 0.037(2) 0.018(2) 0.042(3) -0.0088(19) -0.015(2) -0.0007(17) C82B 0.020(3) 0.020(3) 0.056(5) 0.002(3) -0.007(3) 0.005(2) C83B 0.037(3) 0.020(2) 0.046(3) 0.004(2) 0.003(2) 0.0050(19) C84B 0.042(3) 0.024(2) 0.057(3) -0.023(2) -0.021(2) 0.006(2) C85 0.0210(9) 0.0165(9) 0.0252(10) 0.0004(8) -0.0119(8) -0.0028(7) #----------------------------------------------------------------------------# # 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 O1 1.8969(13) . ? Zn1 O51 1.9106(12) . ? Zn1 N11 2.0826(16) . ? Zn1 N1 2.1130(15) . ? O1 C23 1.340(2) . ? N1 C11 1.491(2) . ? N1 C1 1.500(2) . ? N1 C21 1.519(2) . ? C1 C2 1.518(2) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 C3 1.382(3) . ? C2 C7 1.397(2) . ? C3 C4 1.387(3) . ? C3 H3 0.95 . ? C4 C5 1.385(3) . ? C4 H4 0.95 . ? C5 C6 1.380(3) . ? C5 H5 0.95 . ? C6 C7 1.387(3) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? N11 C51 1.499(2) . ? N11 C71 1.502(2) . ? N11 C61 1.514(2) . ? C11 C12 1.516(2) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C17 1.394(3) . ? C12 C13 1.401(3) . ? C13 C14 1.384(3) . ? C13 H13 0.95 . ? C14 C15 1.390(3) . ? C14 H14 0.95 . ? C15 C16 1.374(3) . ? C15 H15 0.95 . ? C16 C17 1.394(3) . ? C16 H16 0.95 . ? C17 H17 0.95 . ? C21 C22 1.505(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C35 1.389(2) . ? C22 C23 1.411(2) . ? C23 C24 1.418(3) . ? C24 C29 1.389(3) . ? C24 C25 1.549(2) . ? C25 C28 1.532(3) . ? C25 C27 1.534(3) . ? C25 C26 1.543(3) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? 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 C30 1.406(2) . ? C29 H29 0.95 . ? C30 C35 1.387(3) . ? C30 C31 1.537(3) . ? C31 C34B 1.470(6) . ? C31 C32A 1.502(13) . ? C31 C33A 1.513(6) . ? C31 C32B 1.525(12) . ? C31 C33B 1.569(6) . ? C31 C34A 1.608(6) . ? C32A H32A 0.98 . ? C32A H32B 0.98 . ? C32A H32C 0.98 . ? C33A H33A 0.98 . ? C33A H33B 0.98 . ? C33A H33C 0.98 . ? C34A H34A 0.98 . ? C34A H34B 0.98 . ? C34A H34C 0.98 . ? C32B H32D 0.98 . ? C32B H32E 0.98 . ? C32B H32F 0.98 . ? C33B H33D 0.98 . ? C33B H33E 0.98 . ? C33B H33F 0.98 . ? C34B H34D 0.98 . ? C34B H34E 0.98 . ? C34B H34F 0.98 . ? C35 H35 0.95 . ? O51 C73 1.337(2) . ? C51 C52 1.516(3) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 C57 1.396(3) . ? C52 C53 1.401(3) . ? C53 C54 1.397(3) . ? C53 H53 0.95 . ? C54 C55 1.372(3) . ? C54 H54 0.95 . ? C55 C56 1.392(3) . ? C55 H55 0.95 . ? C56 C57 1.392(3) . ? C56 H56 0.95 . ? C57 H57 0.95 . ? C61 C62 1.514(3) . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C62 C63 1.391(3) . ? C62 C67 1.395(3) . ? C63 C64 1.386(3) . ? C63 H63 0.95 . ? C64 C65 1.377(4) . ? C64 H64 0.95 . ? C65 C66 1.374(4) . ? C65 H65 0.95 . ? C66 C67 1.395(3) . ? C66 H66 0.95 . ? C67 H67 0.95 . ? C71 C72 1.516(2) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 C85 1.398(2) . ? C72 C73 1.402(3) . ? C73 C74 1.429(2) . ? C74 C79 1.392(2) . ? C74 C75 1.528(3) . ? C75 C77 1.535(3) . ? C75 C76 1.536(2) . ? C75 C78 1.543(3) . ? C76 H76A 0.98 . ? C76 H76B 0.98 . ? C76 H76C 0.98 . ? C77 H77A 0.98 . ? C77 H77B 0.98 . ? C77 H77C 0.98 . ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? C79 C80 1.389(3) . ? C79 H79 0.95 . ? C80 C85 1.387(3) . ? C80 C81 1.539(3) . ? C81 C83B 1.356(5) . ? C81 C82A 1.411(9) . ? C81 C84A 1.509(5) . ? C81 C82B 1.572(9) . ? C81 C84B 1.687(5) . ? C81 C83A 1.704(5) . ? C82A H82A 0.98 . ? C82A H82B 0.98 . ? C82A H82C 0.98 . ? C83A H83A 0.98 . ? C83A H83B 0.98 . ? C83A H83C 0.98 . ? C84A H84A 0.98 . ? C84A H84B 0.98 . ? C84A H84C 0.98 . ? C82B H82D 0.98 . ? C82B H82E 0.98 . ? C82B H82F 0.98 . ? C83B H83D 0.98 . ? C83B H83E 0.98 . ? C83B H83F 0.98 . ? C84B H84D 0.98 . ? C84B H84E 0.98 . ? C84B H84F 0.98 . ? C85 H85 0.95 . ? 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 O1 Zn1 O51 119.62(6) . . ? O1 Zn1 N11 101.61(6) . . ? O51 Zn1 N11 94.39(6) . . ? O1 Zn1 N1 99.11(5) . . ? O51 Zn1 N1 106.95(6) . . ? N11 Zn1 N1 137.39(6) . . ? C23 O1 Zn1 121.14(11) . . ? C11 N1 C1 111.85(13) . . ? C11 N1 C21 105.02(13) . . ? C1 N1 C21 111.43(14) . . ? C11 N1 Zn1 118.76(11) . . ? C1 N1 Zn1 105.61(10) . . ? C21 N1 Zn1 103.92(10) . . ? N1 C1 C2 117.70(14) . . ? N1 C1 H1A 107.9 . . ? C2 C1 H1A 107.9 . . ? N1 C1 H1B 107.9 . . ? C2 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C3 C2 C7 118.16(17) . . ? C3 C2 C1 118.91(16) . . ? C7 C2 C1 122.60(16) . . ? C2 C3 C4 121.00(18) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.38(19) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.29(18) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 120.20(18) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 120.94(18) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C51 N11 C71 110.66(14) . . ? C51 N11 C61 108.82(14) . . ? C71 N11 C61 111.44(14) . . ? C51 N11 Zn1 115.40(11) . . ? C71 N11 Zn1 105.13(11) . . ? C61 N11 Zn1 105.29(11) . . ? N1 C11 C12 118.39(14) . . ? N1 C11 H11A 107.7 . . ? C12 C11 H11A 107.7 . . ? N1 C11 H11B 107.7 . . ? C12 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C17 C12 C13 118.49(17) . . ? C17 C12 C11 124.63(17) . . ? C13 C12 C11 116.81(16) . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.4(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.86(19) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.2(2) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 120.67(19) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C22 C21 N1 116.68(14) . . ? C22 C21 H21A 108.1 . . ? N1 C21 H21A 108.1 . . ? C22 C21 H21B 108.1 . . ? N1 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C35 C22 C23 120.40(17) . . ? C35 C22 C21 118.36(16) . . ? C23 C22 C21 120.90(16) . . ? O1 C23 C22 120.04(16) . . ? O1 C23 C24 120.92(15) . . ? C22 C23 C24 119.00(16) . . ? C29 C24 C23 117.58(16) . . ? C29 C24 C25 122.30(16) . . ? C23 C24 C25 120.12(16) . . ? C28 C25 C27 107.58(16) . . ? C28 C25 C26 106.86(16) . . ? C27 C25 C26 110.13(16) . . ? C28 C25 C24 112.06(16) . . ? C27 C25 C24 110.62(15) . . ? C26 C25 C24 109.51(15) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 C30 124.23(17) . . ? C24 C29 H29 117.9 . . ? C30 C29 H29 117.9 . . ? C35 C30 C29 116.38(17) . . ? C35 C30 C31 120.15(16) . . ? C29 C30 C31 123.47(17) . . ? C34B C31 C32A 129.8(5) . . ? C34B C31 C33A 79.6(4) . . ? C32A C31 C33A 110.7(6) . . ? C34B C31 C32B 112.9(4) . . ? C33A C31 C32B 125.9(5) . . ? C34B C31 C30 107.8(3) . . ? C32A C31 C30 110.9(5) . . ? C33A C31 C30 114.5(3) . . ? C32B C31 C30 110.8(5) . . ? C34B C31 C33B 109.7(3) . . ? C32A C31 C33B 86.0(5) . . ? C32B C31 C33B 105.9(4) . . ? C30 C31 C33B 109.7(2) . . ? C32A C31 C34A 105.8(5) . . ? C33A C31 C34A 103.8(4) . . ? C32B C31 C34A 86.1(4) . . ? C30 C31 C34A 110.6(3) . . ? C33B C31 C34A 130.0(3) . . ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? C31 C33A H33A 109.5 . . ? C31 C33A H33B 109.5 . . ? C31 C33A H33C 109.5 . . ? C31 C34A H34A 109.5 . . ? C31 C34A H34B 109.5 . . ? C31 C34A H34C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31 C33B H33D 109.5 . . ? C31 C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31 C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C31 C34B H34D 109.5 . . ? C31 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C31 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C30 C35 C22 121.96(17) . . ? C30 C35 H35 119 . . ? C22 C35 H35 119 . . ? C73 O51 Zn1 129.00(11) . . ? N11 C51 C52 116.05(15) . . ? N11 C51 H51A 108.3 . . ? C52 C51 H51A 108.3 . . ? N11 C51 H51B 108.3 . . ? C52 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? C57 C52 C53 118.05(19) . . ? C57 C52 C51 123.00(18) . . ? C53 C52 C51 118.65(18) . . ? C54 C53 C52 121.2(2) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C55 C54 C53 119.8(2) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.2(2) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C57 C56 C55 120.2(2) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C52 120.7(2) . . ? C56 C57 H57 119.7 . . ? C52 C57 H57 119.7 . . ? N11 C61 C62 116.36(16) . . ? N11 C61 H61A 108.2 . . ? C62 C61 H61A 108.2 . . ? N11 C61 H61B 108.2 . . ? C62 C61 H61B 108.2 . . ? H61A C61 H61B 107.3 . . ? C63 C62 C67 118.10(19) . . ? C63 C62 C61 120.80(18) . . ? C67 C62 C61 121.08(19) . . ? C64 C63 C62 121.1(2) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C65 C64 C63 120.1(2) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C66 C65 C64 120.0(2) . . ? C66 C65 H65 120 . . ? C64 C65 H65 120 . . ? C65 C66 C67 120.1(2) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C62 120.5(2) . . ? C66 C67 H67 119.7 . . ? C62 C67 H67 119.7 . . ? N11 C71 C72 116.76(15) . . ? N11 C71 H71A 108.1 . . ? C72 C71 H71A 108.1 . . ? N11 C71 H71B 108.1 . . ? C72 C71 H71B 108.1 . . ? H71A C71 H71B 107.3 . . ? C85 C72 C73 120.37(16) . . ? C85 C72 C71 116.61(17) . . ? C73 C72 C71 122.98(15) . . ? O51 C73 C72 122.03(15) . . ? O51 C73 C74 119.83(16) . . ? C72 C73 C74 118.13(15) . . ? C79 C74 C73 118.58(17) . . ? C79 C74 C75 120.29(16) . . ? C73 C74 C75 121.12(15) . . ? C74 C75 C77 109.81(15) . . ? C74 C75 C76 112.10(15) . . ? C77 C75 C76 108.02(15) . . ? C74 C75 C78 111.10(15) . . ? C77 C75 C78 110.01(16) . . ? C76 C75 C78 105.69(15) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 C74 124.03(17) . . ? C80 C79 H79 118 . . ? C74 C79 H79 118 . . ? C85 C80 C79 116.28(16) . . ? C85 C80 C81 122.35(18) . . ? C79 C80 C81 121.37(18) . . ? C83B C81 C82A 122.6(4) . . ? C83B C81 C84A 63.0(3) . . ? C82A C81 C84A 115.1(4) . . ? C83B C81 C80 116.6(3) . . ? C82A C81 C80 116.0(4) . . ? C84A C81 C80 111.3(2) . . ? C83B C81 C82B 114.9(4) . . ? C84A C81 C82B 133.1(4) . . ? C80 C81 C82B 110.1(4) . . ? C83B C81 C84B 109.1(3) . . ? C82A C81 C84B 78.5(3) . . ? C84A C81 C84B 48.5(2) . . ? C80 C81 C84B 103.7(2) . . ? C82B C81 C84B 100.6(4) . . ? C82A C81 C83A 104.3(4) . . ? C84A C81 C83A 102.8(3) . . ? C80 C81 C83A 105.6(2) . . ? C82B C81 C83A 86.3(4) . . ? C84B C81 C83A 145.3(3) . . ? C81 C82A H82A 109.5 . . ? C81 C82A H82B 109.5 . . ? C81 C82A H82C 109.5 . . ? C81 C83A H83A 109.5 . . ? C81 C83A H83B 109.5 . . ? C81 C83A H83C 109.5 . . ? C81 C84A H84A 109.5 . . ? C81 C84A H84B 109.5 . . ? C81 C84A H84C 109.5 . . ? C81 C82B H82D 109.5 . . ? C81 C82B H82E 109.5 . . ? H82D C82B H82E 109.5 . . ? C81 C82B H82F 109.5 . . ? H82D C82B H82F 109.5 . . ? H82E C82B H82F 109.5 . . ? C81 C83B H83D 109.5 . . ? C81 C83B H83E 109.5 . . ? H83D C83B H83E 109.5 . . ? C81 C83B H83F 109.5 . . ? H83D C83B H83F 109.5 . . ? H83E C83B H83F 109.5 . . ? C81 C84B H84D 109.5 . . ? C81 C84B H84E 109.5 . . ? H84D C84B H84E 109.5 . . ? C81 C84B H84F 109.5 . . ? H84D C84B H84F 109.5 . . ? H84E C84B H84F 109.5 . . ? C80 C85 C72 122.60(18) . . ? C80 C85 H85 118.7 . . ? C72 C85 H85 118.7 . . ? 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 O51 Zn1 O1 C23 85.97(13) . . . . ? N11 Zn1 O1 C23 -172.10(12) . . . . ? N1 Zn1 O1 C23 -29.55(13) . . . . ? O1 Zn1 N1 C11 -134.85(12) . . . . ? O51 Zn1 N1 C11 100.25(12) . . . . ? N11 Zn1 N1 C11 -16.47(15) . . . . ? O1 Zn1 N1 C1 98.70(11) . . . . ? O51 Zn1 N1 C1 -26.20(11) . . . . ? N11 Zn1 N1 C1 -142.92(10) . . . . ? O1 Zn1 N1 C21 -18.70(11) . . . . ? O51 Zn1 N1 C21 -143.60(10) . . . . ? N11 Zn1 N1 C21 99.68(12) . . . . ? C11 N1 C1 C2 59.57(19) . . . . ? C21 N1 C1 C2 -57.65(19) . . . . ? Zn1 N1 C1 C2 -169.87(13) . . . . ? N1 C1 C2 C3 107.41(19) . . . . ? N1 C1 C2 C7 -79.3(2) . . . . ? C7 C2 C3 C4 -1.1(3) . . . . ? C1 C2 C3 C4 172.47(17) . . . . ? C2 C3 C4 C5 1.8(3) . . . . ? C3 C4 C5 C6 -0.7(3) . . . . ? C4 C5 C6 C7 -0.9(3) . . . . ? C5 C6 C7 C2 1.6(3) . . . . ? C3 C2 C7 C6 -0.5(3) . . . . ? C1 C2 C7 C6 -173.89(16) . . . . ? O1 Zn1 N11 C51 72.08(13) . . . . ? O51 Zn1 N11 C51 -166.46(12) . . . . ? N1 Zn1 N11 C51 -45.44(16) . . . . ? O1 Zn1 N11 C71 -165.72(10) . . . . ? O51 Zn1 N11 C71 -44.26(11) . . . . ? N1 Zn1 N11 C71 76.76(13) . . . . ? O1 Zn1 N11 C61 -47.91(11) . . . . ? O51 Zn1 N11 C61 73.55(11) . . . . ? N1 Zn1 N11 C61 -165.43(10) . . . . ? C1 N1 C11 C12 56.8(2) . . . . ? C21 N1 C11 C12 177.79(15) . . . . ? Zn1 N1 C11 C12 -66.64(18) . . . . ? N1 C11 C12 C17 23.5(3) . . . . ? N1 C11 C12 C13 -159.49(17) . . . . ? C17 C12 C13 C14 -0.4(3) . . . . ? C11 C12 C13 C14 -177.63(18) . . . . ? C12 C13 C14 C15 0.6(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C15 C16 C17 C12 0.6(3) . . . . ? C13 C12 C17 C16 -0.2(3) . . . . ? C11 C12 C17 C16 176.79(18) . . . . ? C11 N1 C21 C22 -176.02(15) . . . . ? C1 N1 C21 C22 -54.7(2) . . . . ? Zn1 N1 C21 C22 58.54(17) . . . . ? N1 C21 C22 C35 128.41(17) . . . . ? N1 C21 C22 C23 -58.2(2) . . . . ? Zn1 O1 C23 C22 44.0(2) . . . . ? Zn1 O1 C23 C24 -138.26(14) . . . . ? C35 C22 C23 O1 171.02(16) . . . . ? C21 C22 C23 O1 -2.2(2) . . . . ? C35 C22 C23 C24 -6.8(3) . . . . ? C21 C22 C23 C24 -179.97(15) . . . . ? O1 C23 C24 C29 -171.24(15) . . . . ? C22 C23 C24 C29 6.5(2) . . . . ? O1 C23 C24 C25 8.9(2) . . . . ? C22 C23 C24 C25 -173.32(15) . . . . ? C29 C24 C25 C28 -6.1(2) . . . . ? C23 C24 C25 C28 173.74(16) . . . . ? C29 C24 C25 C27 113.96(19) . . . . ? C23 C24 C25 C27 -66.2(2) . . . . ? C29 C24 C25 C26 -124.47(19) . . . . ? C23 C24 C25 C26 55.3(2) . . . . ? C23 C24 C29 C30 -1.4(3) . . . . ? C25 C24 C29 C30 178.45(17) . . . . ? C24 C29 C30 C35 -3.6(3) . . . . ? C24 C29 C30 C31 175.67(17) . . . . ? C35 C30 C31 C34B 76.7(3) . . . . ? C29 C30 C31 C34B -102.6(3) . . . . ? C35 C30 C31 C32A -70.7(5) . . . . ? C29 C30 C31 C32A 110.1(4) . . . . ? C35 C30 C31 C33A 163.1(4) . . . . ? C29 C30 C31 C33A -16.1(4) . . . . ? C35 C30 C31 C32B -47.3(4) . . . . ? C29 C30 C31 C32B 133.4(4) . . . . ? C35 C30 C31 C33B -163.9(3) . . . . ? C29 C30 C31 C33B 16.8(3) . . . . ? C35 C30 C31 C34A 46.3(3) . . . . ? C29 C30 C31 C34A -132.9(3) . . . . ? C29 C30 C35 C22 3.5(3) . . . . ? C31 C30 C35 C22 -175.84(16) . . . . ? C23 C22 C35 C30 1.6(3) . . . . ? C21 C22 C35 C30 175.00(16) . . . . ? O1 Zn1 O51 C73 120.16(14) . . . . ? N11 Zn1 O51 C73 14.15(15) . . . . ? N1 Zn1 O51 C73 -128.52(14) . . . . ? C71 N11 C51 C52 -75.3(2) . . . . ? C61 N11 C51 C52 161.98(16) . . . . ? Zn1 N11 C51 C52 43.9(2) . . . . ? N11 C51 C52 C57 77.6(2) . . . . ? N11 C51 C52 C53 -108.9(2) . . . . ? C57 C52 C53 C54 -1.2(3) . . . . ? C51 C52 C53 C54 -175.01(18) . . . . ? C52 C53 C54 C55 -0.1(3) . . . . ? C53 C54 C55 C56 0.5(3) . . . . ? C54 C55 C56 C57 0.5(3) . . . . ? C55 C56 C57 C52 -1.8(3) . . . . ? C53 C52 C57 C56 2.1(3) . . . . ? C51 C52 C57 C56 175.69(19) . . . . ? C51 N11 C61 C62 57.9(2) . . . . ? C71 N11 C61 C62 -64.4(2) . . . . ? Zn1 N11 C61 C62 -177.81(13) . . . . ? N11 C61 C62 C63 -88.7(2) . . . . ? N11 C61 C62 C67 93.0(2) . . . . ? C67 C62 C63 C64 -0.9(3) . . . . ? C61 C62 C63 C64 -179.29(19) . . . . ? C62 C63 C64 C65 0.2(3) . . . . ? C63 C64 C65 C66 0.3(4) . . . . ? C64 C65 C66 C67 -0.1(4) . . . . ? C65 C66 C67 C62 -0.7(4) . . . . ? C63 C62 C67 C66 1.2(3) . . . . ? C61 C62 C67 C66 179.5(2) . . . . ? C51 N11 C71 C72 -171.24(15) . . . . ? C61 N11 C71 C72 -50.0(2) . . . . ? Zn1 N11 C71 C72 63.54(17) . . . . ? N11 C71 C72 C85 137.16(17) . . . . ? N11 C71 C72 C73 -45.0(2) . . . . ? Zn1 O51 C73 C72 6.8(2) . . . . ? Zn1 O51 C73 C74 -173.60(12) . . . . ? C85 C72 C73 O51 -179.75(16) . . . . ? C71 C72 C73 O51 2.5(3) . . . . ? C85 C72 C73 C74 0.7(3) . . . . ? C71 C72 C73 C74 -177.12(16) . . . . ? O51 C73 C74 C79 179.52(15) . . . . ? C72 C73 C74 C79 -0.9(2) . . . . ? O51 C73 C74 C75 1.1(2) . . . . ? C72 C73 C74 C75 -179.27(16) . . . . ? C79 C74 C75 C77 -112.80(18) . . . . ? C73 C74 C75 C77 65.5(2) . . . . ? C79 C74 C75 C76 7.3(2) . . . . ? C73 C74 C75 C76 -174.38(16) . . . . ? C79 C74 C75 C78 125.27(18) . . . . ? C73 C74 C75 C78 -56.4(2) . . . . ? C73 C74 C79 C80 0.1(3) . . . . ? C75 C74 C79 C80 178.49(17) . . . . ? C74 C79 C80 C85 0.9(3) . . . . ? C74 C79 C80 C81 -179.66(17) . . . . ? C85 C80 C81 C83B -7.6(4) . . . . ? C79 C80 C81 C83B 173.0(3) . . . . ? C85 C80 C81 C82A -163.9(3) . . . . ? C79 C80 C81 C82A 16.7(4) . . . . ? C85 C80 C81 C84A 62.0(3) . . . . ? C79 C80 C81 C84A -117.4(3) . . . . ? C85 C80 C81 C82B -140.7(4) . . . . ? C79 C80 C81 C82B 39.9(4) . . . . ? C85 C80 C81 C84B 112.4(3) . . . . ? C79 C80 C81 C84B -67.0(3) . . . . ? C85 C80 C81 C83A -48.9(3) . . . . ? C79 C80 C81 C83A 131.7(2) . . . . ? C79 C80 C85 C72 -1.2(3) . . . . ? C81 C80 C85 C72 179.42(17) . . . . ? C73 C72 C85 C80 0.4(3) . . . . ? C71 C72 C85 C80 178.31(16) . . . . ? # Attachment 'complex10_Jiqng5.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-21 at 09:45:24 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job_3 _database_code_depnum_ccdc_archive 'CCDC 672306' _audit_creation_date 2006-11-21T09:45:24-00:00 _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 'C38 H47 Mg N3 O2' _chemical_formula_sum 'C38 H47 Mg N3 O2' _chemical_formula_weight 602.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4793(6) _cell_length_b 22.4925(13) _cell_length_c 15.5746(9) _cell_angle_alpha 90 _cell_angle_beta 108.702(4) _cell_angle_gamma 90 _cell_volume 3477.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3761 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.08 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.087 _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 0.981 _exptl_absorpt_correction_T_max 0.997 #----------------------------------------------------------------------------# # 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 0.087 _diffrn_reflns_av_unetI/netI 0.0837 _diffrn_reflns_number 35729 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.69 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8082 _reflns_number_gt 4998 _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^)+(0.0571P)^2^+1.1791P] 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 8082 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.385 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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 Mg1 Mg 0.82565(7) 0.24500(3) 0.72607(5) 0.01442(17) Uani 1 d . . . N1 N 0.91125(17) 0.19627(7) 0.84944(12) 0.0162(4) Uani 1 d . . . C1 C 0.8481(2) 0.18794(9) 0.91126(15) 0.0213(5) Uani 1 d . . . H1 H 0.7606 0.2042 0.9 0.026 Uiso 1 calc R . . C2 C 0.9057(2) 0.15667(10) 0.99029(16) 0.0241(5) Uani 1 d . . . H2 H 0.8582 0.1512 1.0324 0.029 Uiso 1 calc R . . C3 C 1.0337(2) 0.13332(9) 1.00743(15) 0.0250(5) Uani 1 d . . . H3 H 1.0751 0.1113 1.0613 0.03 Uiso 1 calc R . . C4 C 1.1002(2) 0.14239(9) 0.94538(15) 0.0208(5) Uani 1 d . . . H4 H 1.1887 0.1274 0.9564 0.025 Uiso 1 calc R . . C5 C 1.0361(2) 0.17379(8) 0.86623(14) 0.0158(4) Uani 1 d . . . C6 C 1.0965(2) 0.18256(9) 0.79164(14) 0.0171(4) Uani 1 d . . . H6A H 1.1959 0.184 0.818 0.021 Uiso 1 calc R . . H6B H 1.0726 0.1484 0.7495 0.021 Uiso 1 calc R . . N11 N 0.83476(17) 0.19760(7) 0.60626(12) 0.0184(4) Uani 1 d . . . C11 C 0.7303(2) 0.16794(10) 0.54837(16) 0.0247(5) Uani 1 d . . . H11 H 0.6491 0.1645 0.5628 0.03 Uiso 1 calc R . . C12 C 0.7361(2) 0.14241(11) 0.46938(17) 0.0314(6) Uani 1 d . . . H12 H 0.6601 0.1223 0.4299 0.038 Uiso 1 calc R . . C13 C 0.8551(3) 0.14656(11) 0.44843(17) 0.0323(6) Uani 1 d . . . H13 H 0.8617 0.1298 0.394 0.039 Uiso 1 calc R . . C14 C 0.9635(2) 0.17549(10) 0.50829(16) 0.0251(5) Uani 1 d . . . H14 H 1.0465 0.1781 0.4961 0.03 Uiso 1 calc R . . C15 C 0.9507(2) 0.20062(9) 0.58606(14) 0.0179(5) Uani 1 d . . . C16 C 1.0643(2) 0.23528(9) 0.65109(14) 0.0173(4) Uani 1 d . . . H16A H 1.1513 0.2161 0.6557 0.021 Uiso 1 calc R . . H16B H 1.0655 0.2761 0.6278 0.021 Uiso 1 calc R . . N17 N 1.04819(16) 0.23783(7) 0.74114(11) 0.0143(4) Uani 1 d . . . O21 O 0.84476(13) 0.32908(6) 0.72362(10) 0.0177(3) Uani 1 d . . . C21 C 0.9403(2) 0.36709(9) 0.72284(14) 0.0146(4) Uani 1 d . . . C22 C 1.0774(2) 0.35009(9) 0.75419(14) 0.0151(4) Uani 1 d . . . C24 C 0.9082(2) 0.42678(9) 0.69144(14) 0.0156(4) Uani 1 d . . . C25 C 0.7611(2) 0.44827(9) 0.66074(15) 0.0180(5) Uani 1 d . . . C23 C 1.1194(2) 0.28950(9) 0.79495(14) 0.0160(4) Uani 1 d . . . H23A H 1.2171 0.2847 0.8052 0.019 Uiso 1 calc R . . H23B H 1.1058 0.2883 0.855 0.019 Uiso 1 calc R . . C27 C 0.6686(2) 0.41154(10) 0.58168(16) 0.0245(5) Uani 1 d . . . H27A H 0.5765 0.4271 0.5651 0.037 Uiso 1 calc R . . H27B H 0.6693 0.3699 0.6003 0.037 Uiso 1 calc R . . H27C H 0.7011 0.4143 0.5294 0.037 Uiso 1 calc R . . C26 C 0.7064(2) 0.44435(10) 0.74122(16) 0.0221(5) Uani 1 d . . . H26A H 0.6126 0.4579 0.7221 0.033 Uiso 1 calc R . . H26B H 0.7609 0.4696 0.7908 0.033 Uiso 1 calc R . . H26C H 0.7109 0.4031 0.7621 0.033 Uiso 1 calc R . . C28 C 0.7488(2) 0.51319(9) 0.62829(17) 0.0257(5) Uani 1 d . . . H28A H 0.654 0.5253 0.6093 0.038 Uiso 1 calc R . . H28B H 0.7833 0.5168 0.577 0.038 Uiso 1 calc R . . H28C H 0.8014 0.5388 0.6779 0.038 Uiso 1 calc R . . C29 C 1.0144(2) 0.46552(9) 0.69679(14) 0.0169(4) Uani 1 d . . . H29 H 0.9928 0.5052 0.6763 0.02 Uiso 1 calc R . . C30 C 1.1502(2) 0.44979(9) 0.73024(14) 0.0166(4) Uani 1 d . . . C31 C 1.1788(2) 0.39088(9) 0.75651(14) 0.0165(4) Uani 1 d . . . H31 H 1.27 0.378 0.7766 0.02 Uiso 1 calc R . . C32 C 1.2630(2) 0.49503(10) 0.73579(16) 0.0223(5) Uani 1 d . . . C33 C 1.3922(2) 0.47924(11) 0.81154(19) 0.0352(6) Uani 1 d . . . H33A H 1.4218 0.4393 0.801 0.053 Uiso 1 calc R . . H33B H 1.3754 0.4801 0.8699 0.053 Uiso 1 calc R . . H33C H 1.4626 0.5082 0.8124 0.053 Uiso 1 calc R . . C34 C 1.2929(3) 0.49496(14) 0.64568(19) 0.0485(8) Uani 1 d . . . H34A H 1.3188 0.4548 0.6332 0.073 Uiso 1 calc R . . H34B H 1.3667 0.5226 0.6495 0.073 Uiso 1 calc R . . H34C H 1.2122 0.5074 0.5967 0.073 Uiso 1 calc R . . C35 C 1.2221(3) 0.55743(10) 0.7550(2) 0.0462(8) Uani 1 d . . . H35A H 1.1392 0.569 0.7074 0.069 Uiso 1 calc R . . H35B H 1.2941 0.5855 0.7561 0.069 Uiso 1 calc R . . H35C H 1.2068 0.5579 0.8138 0.069 Uiso 1 calc R . . O41 O 0.64829(14) 0.22867(7) 0.72461(11) 0.0254(4) Uani 1 d . . . C41 C 0.5196(2) 0.24326(10) 0.69680(15) 0.0202(5) Uani 1 d . . . C42 C 0.4684(3) 0.29530(11) 0.7106(2) 0.0334(6) Uani 1 d . . . H42A H 0.527(3) 0.3278(13) 0.7451(19) 0.05 Uiso 1 d . . . H42B H 0.373(3) 0.3020(12) 0.6887(19) 0.05 Uiso 1 d . . . C43 C 0.4299(2) 0.19353(9) 0.64761(15) 0.0176(5) Uani 1 d . . . C44 C 0.4001(2) 0.14658(9) 0.69811(15) 0.0182(5) Uani 1 d . . . C45 C 0.4562(2) 0.14711(10) 0.80029(15) 0.0232(5) Uani 1 d . . . H45A H 0.5091 0.1834 0.8204 0.035 Uiso 0.5 calc PR . . H45B H 0.514 0.1123 0.8211 0.035 Uiso 0.5 calc PR . . H45C H 0.3819 0.146 0.8256 0.035 Uiso 0.5 calc PR . . H45D H 0.4276 0.1111 0.8244 0.035 Uiso 0.5 calc PR . . H45E H 0.4227 0.1822 0.8237 0.035 Uiso 0.5 calc PR . . H45F H 0.5548 0.1484 0.8191 0.035 Uiso 0.5 calc PR . . C46 C 0.3214(2) 0.09972(9) 0.65274(16) 0.0232(5) Uani 1 d . . . H46 H 0.2981 0.069 0.6869 0.028 Uiso 1 calc R . . C47 C 0.2753(2) 0.09628(10) 0.55816(17) 0.0262(5) Uani 1 d . . . C48 C 0.1911(3) 0.04426(11) 0.51003(19) 0.0387(7) Uani 1 d . . . H48A H 0.1779 0.0165 0.5549 0.058 Uiso 0.5 calc PR . . H48B H 0.2375 0.0239 0.4729 0.058 Uiso 0.5 calc PR . . H48C H 0.1034 0.0587 0.471 0.058 Uiso 0.5 calc PR . . H48D H 0.168 0.0495 0.4443 0.058 Uiso 0.5 calc PR . . H48E H 0.1083 0.0421 0.5263 0.058 Uiso 0.5 calc PR . . H48F H 0.2424 0.0074 0.5282 0.058 Uiso 0.5 calc PR . . C49 C 0.3091(2) 0.14219(10) 0.50987(16) 0.0243(5) Uani 1 d . . . H49 H 0.2803 0.1402 0.4456 0.029 Uiso 1 calc R . . C50 C 0.3841(2) 0.19114(9) 0.55299(16) 0.0208(5) Uani 1 d . . . C51 C 0.4161(2) 0.24041(10) 0.49675(17) 0.0281(5) Uani 1 d . . . H51A H 0.469 0.2713 0.537 0.042 Uiso 0.5 calc PR . . H51B H 0.332 0.2576 0.457 0.042 Uiso 0.5 calc PR . . H51C H 0.468 0.2241 0.4599 0.042 Uiso 0.5 calc PR . . H51D H 0.377 0.2308 0.4322 0.042 Uiso 0.5 calc PR . . H51E H 0.514 0.2444 0.5122 0.042 Uiso 0.5 calc PR . . H51F H 0.378 0.2779 0.5094 0.042 Uiso 0.5 calc PR . . 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 Mg1 0.0134(3) 0.0137(3) 0.0163(4) 0.0008(3) 0.0049(3) -0.0001(3) N1 0.0169(9) 0.0153(8) 0.0171(10) 0.0003(7) 0.0063(8) -0.0020(7) C1 0.0231(12) 0.0220(11) 0.0202(13) -0.0017(9) 0.0089(10) -0.0055(9) C2 0.0316(13) 0.0239(12) 0.0191(13) 0.0002(10) 0.0116(10) -0.0089(10) C3 0.0392(14) 0.0183(11) 0.0148(12) 0.0024(9) 0.0048(10) -0.0029(10) C4 0.0241(12) 0.0154(10) 0.0200(12) -0.0006(9) 0.0031(10) 0.0015(9) C5 0.0181(11) 0.0114(9) 0.0167(12) -0.0017(8) 0.0038(9) -0.0020(8) C6 0.0159(11) 0.0154(10) 0.0202(12) 0.0009(9) 0.0059(9) 0.0028(8) N11 0.0182(9) 0.0182(9) 0.0176(10) 0.0004(7) 0.0042(8) 0.0010(7) C11 0.0219(12) 0.0255(12) 0.0245(13) -0.0026(10) 0.0042(10) 0.0001(9) C12 0.0337(14) 0.0324(13) 0.0232(14) -0.0089(11) 0.0020(11) -0.0050(11) C13 0.0432(16) 0.0326(14) 0.0217(14) -0.0072(11) 0.0115(12) -0.0021(11) C14 0.0337(13) 0.0258(12) 0.0194(13) -0.0011(10) 0.0138(11) 0.0001(10) C15 0.0218(11) 0.0164(10) 0.0160(12) 0.0028(8) 0.0066(9) 0.0027(8) C16 0.0183(11) 0.0170(10) 0.0190(12) 0.0015(9) 0.0094(9) 0.0004(8) N17 0.0170(9) 0.0121(8) 0.0144(9) -0.0003(7) 0.0060(7) -0.0002(7) O21 0.0159(8) 0.0138(7) 0.0247(9) 0.0017(6) 0.0083(6) -0.0005(6) C21 0.0152(10) 0.0163(10) 0.0135(11) -0.0021(8) 0.0063(8) -0.0023(8) C22 0.0187(11) 0.0149(10) 0.0128(11) -0.0016(8) 0.0064(9) -0.0020(8) C24 0.0182(11) 0.0172(10) 0.0133(11) -0.0010(8) 0.0074(9) 0.0011(8) C25 0.0188(11) 0.0161(10) 0.0208(12) 0.0020(9) 0.0090(9) 0.0040(8) C23 0.0125(10) 0.0168(10) 0.0175(11) -0.0004(9) 0.0031(9) -0.0010(8) C27 0.0200(12) 0.0240(12) 0.0279(14) 0.0014(10) 0.0055(10) 0.0051(9) C26 0.0228(12) 0.0207(11) 0.0275(13) 0.0019(10) 0.0145(10) 0.0042(9) C28 0.0271(13) 0.0193(11) 0.0333(15) 0.0059(10) 0.0135(11) 0.0062(9) C29 0.0218(11) 0.0128(10) 0.0178(12) 0.0007(8) 0.0090(9) 0.0005(8) C30 0.0201(11) 0.0164(10) 0.0163(12) -0.0033(8) 0.0103(9) -0.0035(8) C31 0.0159(11) 0.0187(10) 0.0157(12) -0.0022(9) 0.0063(9) 0.0000(8) C32 0.0217(12) 0.0207(11) 0.0267(13) -0.0019(9) 0.0110(10) -0.0068(9) C33 0.0233(13) 0.0348(14) 0.0451(17) 0.0039(12) 0.0076(12) -0.0122(11) C34 0.0543(19) 0.0618(19) 0.0373(18) -0.0073(15) 0.0255(15) -0.0357(16) C35 0.0325(15) 0.0174(12) 0.089(3) -0.0083(13) 0.0208(16) -0.0085(11) O41 0.0131(8) 0.0252(8) 0.0355(10) 0.0062(7) 0.0047(7) -0.0016(6) C41 0.0151(11) 0.0244(11) 0.0214(12) 0.0044(9) 0.0065(9) -0.0023(9) C42 0.0228(13) 0.0262(13) 0.0520(18) -0.0077(12) 0.0129(13) -0.0031(11) C43 0.0119(10) 0.0171(10) 0.0250(13) 0.0031(9) 0.0075(9) 0.0042(8) C44 0.0146(11) 0.0181(10) 0.0235(12) 0.0021(9) 0.0085(9) 0.0036(8) C45 0.0213(12) 0.0246(11) 0.0255(13) 0.0035(10) 0.0098(10) -0.0001(9) C46 0.0233(12) 0.0171(11) 0.0299(14) 0.0036(10) 0.0094(10) 0.0013(9) C47 0.0235(12) 0.0203(11) 0.0329(15) -0.0012(10) 0.0064(11) -0.0003(9) C48 0.0442(16) 0.0266(13) 0.0403(17) -0.0029(12) 0.0065(13) -0.0095(12) C49 0.0213(12) 0.0260(12) 0.0233(13) 0.0008(10) 0.0038(10) 0.0012(9) C50 0.0143(11) 0.0215(11) 0.0254(13) 0.0043(9) 0.0046(9) 0.0025(9) C51 0.0258(12) 0.0279(12) 0.0282(14) 0.0062(10) 0.0054(10) -0.0020(10) #----------------------------------------------------------------------------# # 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 Mg1 O41 1.8876(16) . ? Mg1 O21 1.9032(15) . ? Mg1 N1 2.1430(18) . ? Mg1 N11 2.1777(19) . ? Mg1 N17 2.2734(17) . ? N1 C1 1.345(3) . ? N1 C5 1.348(3) . ? C1 C2 1.377(3) . ? C1 H1 0.95 . ? C2 C3 1.385(3) . ? C2 H2 0.95 . ? C3 C4 1.376(3) . ? C3 H3 0.95 . ? C4 C5 1.392(3) . ? C4 H4 0.95 . ? C5 C6 1.504(3) . ? C6 N17 1.471(2) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? N11 C11 1.350(3) . ? N11 C15 1.351(3) . ? C11 C12 1.377(3) . ? C11 H11 0.95 . ? C12 C13 1.390(3) . ? C12 H12 0.95 . ? C13 C14 1.380(3) . ? C13 H13 0.95 . ? C14 C15 1.382(3) . ? C14 H14 0.95 . ? C15 C16 1.509(3) . ? C16 N17 1.466(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? N17 C23 1.486(2) . ? O21 C21 1.319(2) . ? C21 C22 1.415(3) . ? C21 C24 1.431(3) . ? C22 C31 1.396(3) . ? C22 C23 1.508(3) . ? C24 C29 1.395(3) . ? C24 C25 1.538(3) . ? C25 C28 1.537(3) . ? C25 C26 1.539(3) . ? C25 C27 1.540(3) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.396(3) . ? C29 H29 0.95 . ? C30 C31 1.391(3) . ? C30 C32 1.541(3) . ? C31 H31 0.95 . ? C32 C35 1.525(3) . ? C32 C33 1.526(3) . ? C32 C34 1.533(3) . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? O41 C41 1.319(2) . ? C41 C42 1.333(3) . ? C41 C43 1.503(3) . ? C42 H42A 1.00(3) . ? C42 H42B 0.96(3) . ? C43 C50 1.397(3) . ? C43 C44 1.410(3) . ? C44 C46 1.384(3) . ? C44 C45 1.509(3) . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C45 H45D 0.98 . ? C45 H45E 0.98 . ? C45 H45F 0.98 . ? C46 C47 1.397(3) . ? C46 H46 0.95 . ? C47 C49 1.389(3) . ? C47 C48 1.512(3) . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C48 H48D 0.98 . ? C48 H48E 0.98 . ? C48 H48F 0.98 . ? C49 C50 1.394(3) . ? C49 H49 0.95 . ? C50 C51 1.515(3) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C51 H51D 0.98 . ? C51 H51E 0.98 . ? C51 H51F 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 O41 Mg1 O21 107.61(7) . . ? O41 Mg1 N1 92.22(7) . . ? O21 Mg1 N1 120.65(7) . . ? O41 Mg1 N11 102.00(7) . . ? O21 Mg1 N11 115.82(7) . . ? N1 Mg1 N11 113.39(7) . . ? O41 Mg1 N17 163.93(7) . . ? O21 Mg1 N17 87.80(6) . . ? N1 Mg1 N17 75.56(6) . . ? N11 Mg1 N17 74.24(7) . . ? C1 N1 C5 118.60(18) . . ? C1 N1 Mg1 123.55(14) . . ? C5 N1 Mg1 117.84(13) . . ? N1 C1 C2 122.4(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.0(2) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.64(19) . . ? N1 C5 C6 115.08(18) . . ? C4 C5 C6 123.21(19) . . ? N17 C6 C5 111.46(16) . . ? N17 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N17 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108 . . ? C11 N11 C15 117.81(19) . . ? C11 N11 Mg1 124.41(15) . . ? C15 N11 Mg1 117.69(14) . . ? N11 C11 C12 123.0(2) . . ? N11 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 118.8(2) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 118.6(2) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N11 C15 C14 122.1(2) . . ? N11 C15 C16 116.39(18) . . ? C14 C15 C16 121.48(19) . . ? N17 C16 C15 110.75(17) . . ? N17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 N17 C6 110.65(15) . . ? C16 N17 C23 112.29(16) . . ? C6 N17 C23 109.56(16) . . ? C16 N17 Mg1 109.44(12) . . ? C6 N17 Mg1 106.31(12) . . ? C23 N17 Mg1 108.39(11) . . ? C21 O21 Mg1 136.81(13) . . ? O21 C21 C22 120.76(18) . . ? O21 C21 C24 121.01(18) . . ? C22 C21 C24 118.22(18) . . ? C31 C22 C21 120.81(18) . . ? C31 C22 C23 117.82(18) . . ? C21 C22 C23 121.08(17) . . ? C29 C24 C21 118.04(18) . . ? C29 C24 C25 121.54(18) . . ? C21 C24 C25 120.21(17) . . ? C28 C25 C24 111.74(17) . . ? C28 C25 C26 107.98(17) . . ? C24 C25 C26 109.06(17) . . ? C28 C25 C27 106.38(18) . . ? C24 C25 C27 113.01(17) . . ? C26 C25 C27 108.49(18) . . ? N17 C23 C22 116.32(17) . . ? N17 C23 H23A 108.2 . . ? C22 C23 H23A 108.2 . . ? N17 C23 H23B 108.2 . . ? C22 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 C30 124.26(19) . . ? C24 C29 H29 117.9 . . ? C30 C29 H29 117.9 . . ? C31 C30 C29 116.68(18) . . ? C31 C30 C32 121.58(19) . . ? C29 C30 C32 121.73(18) . . ? C30 C31 C22 121.90(19) . . ? C30 C31 H31 119.1 . . ? C22 C31 H31 119.1 . . ? C35 C32 C33 107.4(2) . . ? C35 C32 C34 109.5(2) . . ? C33 C32 C34 108.4(2) . . ? C35 C32 C30 111.12(18) . . ? C33 C32 C30 111.37(18) . . ? C34 C32 C30 109.03(19) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 O41 Mg1 148.74(14) . . ? O41 C41 C42 126.0(2) . . ? O41 C41 C43 112.88(18) . . ? C42 C41 C43 121.1(2) . . ? C41 C42 H42A 121.4(16) . . ? C41 C42 H42B 120.6(17) . . ? H42A C42 H42B 118(2) . . ? C50 C43 C44 119.8(2) . . ? C50 C43 C41 120.88(19) . . ? C44 C43 C41 119.1(2) . . ? C46 C44 C43 119.2(2) . . ? C46 C44 C45 120.74(19) . . ? C43 C44 C45 120.06(19) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C45 H45D 109.5 . . ? H45A C45 H45D 141.1 . . ? H45B C45 H45D 56.3 . . ? H45C C45 H45D 56.3 . . ? C44 C45 H45E 109.5 . . ? H45A C45 H45E 56.3 . . ? H45B C45 H45E 141.1 . . ? H45C C45 H45E 56.3 . . ? H45D C45 H45E 109.5 . . ? C44 C45 H45F 109.5 . . ? H45A C45 H45F 56.3 . . ? H45B C45 H45F 56.3 . . ? H45C C45 H45F 141.1 . . ? H45D C45 H45F 109.5 . . ? H45E C45 H45F 109.5 . . ? C44 C46 C47 121.9(2) . . ? C44 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C49 C47 C46 117.9(2) . . ? C49 C47 C48 121.1(2) . . ? C46 C47 C48 121.0(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C48 H48D 109.5 . . ? H48A C48 H48D 141.1 . . ? H48B C48 H48D 56.3 . . ? H48C C48 H48D 56.3 . . ? C47 C48 H48E 109.5 . . ? H48A C48 H48E 56.3 . . ? H48B C48 H48E 141.1 . . ? H48C C48 H48E 56.3 . . ? H48D C48 H48E 109.5 . . ? C47 C48 H48F 109.5 . . ? H48A C48 H48F 56.3 . . ? H48B C48 H48F 56.3 . . ? H48C C48 H48F 141.1 . . ? H48D C48 H48F 109.5 . . ? H48E C48 H48F 109.5 . . ? C47 C49 C50 121.9(2) . . ? C47 C49 H49 119 . . ? C50 C49 H49 119 . . ? C49 C50 C43 119.2(2) . . ? C49 C50 C51 119.6(2) . . ? C43 C50 C51 121.1(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C51 H51D 109.5 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? C50 C51 H51E 109.5 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.3 . . ? H51D C51 H51E 109.5 . . ? C50 C51 H51F 109.5 . . ? H51A C51 H51F 56.3 . . ? H51B C51 H51F 56.3 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 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 O41 Mg1 N1 C1 -26.02(17) . . . . ? O21 Mg1 N1 C1 86.00(17) . . . . ? N11 Mg1 N1 C1 -130.11(16) . . . . ? N17 Mg1 N1 C1 164.54(17) . . . . ? O41 Mg1 N1 C5 155.21(15) . . . . ? O21 Mg1 N1 C5 -92.77(15) . . . . ? N11 Mg1 N1 C5 51.12(16) . . . . ? N17 Mg1 N1 C5 -14.23(14) . . . . ? C5 N1 C1 C2 -0.9(3) . . . . ? Mg1 N1 C1 C2 -179.66(16) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 -1.2(3) . . . . ? C1 N1 C5 C4 0.1(3) . . . . ? Mg1 N1 C5 C4 178.94(15) . . . . ? C1 N1 C5 C6 177.17(18) . . . . ? Mg1 N1 C5 C6 -4.0(2) . . . . ? C3 C4 C5 N1 1.0(3) . . . . ? C3 C4 C5 C6 -175.86(19) . . . . ? N1 C5 C6 N17 31.1(2) . . . . ? C4 C5 C6 N17 -151.93(19) . . . . ? O41 Mg1 N11 C11 2.75(18) . . . . ? O21 Mg1 N11 C11 -113.77(17) . . . . ? N1 Mg1 N11 C11 100.51(17) . . . . ? N17 Mg1 N11 C11 166.65(18) . . . . ? O41 Mg1 N11 C15 179.25(14) . . . . ? O21 Mg1 N11 C15 62.73(16) . . . . ? N1 Mg1 N11 C15 -82.99(16) . . . . ? N17 Mg1 N11 C15 -16.85(14) . . . . ? C15 N11 C11 C12 -1.8(3) . . . . ? Mg1 N11 C11 C12 174.67(18) . . . . ? N11 C11 C12 C13 0.8(4) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? C12 C13 C14 C15 -1.4(4) . . . . ? C11 N11 C15 C14 1.2(3) . . . . ? Mg1 N11 C15 C14 -175.53(16) . . . . ? C11 N11 C15 C16 178.65(18) . . . . ? Mg1 N11 C15 C16 1.9(2) . . . . ? C13 C14 C15 N11 0.4(3) . . . . ? C13 C14 C15 C16 -176.9(2) . . . . ? N11 C15 C16 N17 23.9(2) . . . . ? C14 C15 C16 N17 -158.66(19) . . . . ? C15 C16 N17 C6 80.8(2) . . . . ? C15 C16 N17 C23 -156.48(16) . . . . ? C15 C16 N17 Mg1 -36.07(18) . . . . ? C5 C6 N17 C16 -158.59(16) . . . . ? C5 C6 N17 C23 77.1(2) . . . . ? C5 C6 N17 Mg1 -39.84(18) . . . . ? O41 Mg1 N17 C16 106.9(3) . . . . ? O21 Mg1 N17 C16 -89.24(13) . . . . ? N1 Mg1 N17 C16 148.30(13) . . . . ? N11 Mg1 N17 C16 28.39(12) . . . . ? O41 Mg1 N17 C6 -12.7(3) . . . . ? O21 Mg1 N17 C6 151.22(13) . . . . ? N1 Mg1 N17 C6 28.76(12) . . . . ? N11 Mg1 N17 C6 -91.15(13) . . . . ? O41 Mg1 N17 C23 -130.4(3) . . . . ? O21 Mg1 N17 C23 33.52(13) . . . . ? N1 Mg1 N17 C23 -88.94(13) . . . . ? N11 Mg1 N17 C23 151.15(13) . . . . ? O41 Mg1 O21 C21 -179.39(19) . . . . ? N1 Mg1 O21 C21 77.0(2) . . . . ? N11 Mg1 O21 C21 -66.1(2) . . . . ? N17 Mg1 O21 C21 5.2(2) . . . . ? Mg1 O21 C21 C22 -21.6(3) . . . . ? Mg1 O21 C21 C24 159.20(16) . . . . ? O21 C21 C22 C31 -177.62(19) . . . . ? C24 C21 C22 C31 1.6(3) . . . . ? O21 C21 C22 C23 -4.0(3) . . . . ? C24 C21 C22 C23 175.20(18) . . . . ? O21 C21 C24 C29 176.77(18) . . . . ? C22 C21 C24 C29 -2.4(3) . . . . ? O21 C21 C24 C25 2.0(3) . . . . ? C22 C21 C24 C25 -177.23(18) . . . . ? C29 C24 C25 C28 6.3(3) . . . . ? C21 C24 C25 C28 -179.09(19) . . . . ? C29 C24 C25 C26 -113.0(2) . . . . ? C21 C24 C25 C26 61.6(2) . . . . ? C29 C24 C25 C27 126.2(2) . . . . ? C21 C24 C25 C27 -59.1(3) . . . . ? C16 N17 C23 C22 58.9(2) . . . . ? C6 N17 C23 C22 -177.70(17) . . . . ? Mg1 N17 C23 C22 -62.09(19) . . . . ? C31 C22 C23 N17 -135.17(19) . . . . ? C21 C22 C23 N17 51.0(3) . . . . ? C21 C24 C29 C30 0.5(3) . . . . ? C25 C24 C29 C30 175.19(19) . . . . ? C24 C29 C30 C31 2.4(3) . . . . ? C24 C29 C30 C32 -179.0(2) . . . . ? C29 C30 C31 C22 -3.3(3) . . . . ? C32 C30 C31 C22 178.08(19) . . . . ? C21 C22 C31 C30 1.4(3) . . . . ? C23 C22 C31 C30 -172.45(19) . . . . ? C31 C30 C32 C35 -148.6(2) . . . . ? C29 C30 C32 C35 32.8(3) . . . . ? C31 C30 C32 C33 -28.9(3) . . . . ? C29 C30 C32 C33 152.5(2) . . . . ? C31 C30 C32 C34 90.7(3) . . . . ? C29 C30 C32 C34 -87.9(3) . . . . ? O21 Mg1 O41 C41 34.1(3) . . . . ? N1 Mg1 O41 C41 157.3(3) . . . . ? N11 Mg1 O41 C41 -88.2(3) . . . . ? N17 Mg1 O41 C41 -162.8(3) . . . . ? Mg1 O41 C41 C42 -56.9(4) . . . . ? Mg1 O41 C41 C43 124.5(3) . . . . ? O41 C41 C43 C50 -97.7(2) . . . . ? C42 C41 C43 C50 83.6(3) . . . . ? O41 C41 C43 C44 77.6(2) . . . . ? C42 C41 C43 C44 -101.1(3) . . . . ? C50 C43 C44 C46 -2.3(3) . . . . ? C41 C43 C44 C46 -177.72(19) . . . . ? C50 C43 C44 C45 176.32(19) . . . . ? C41 C43 C44 C45 0.9(3) . . . . ? C43 C44 C46 C47 2.8(3) . . . . ? C45 C44 C46 C47 -175.9(2) . . . . ? C44 C46 C47 C49 -0.9(3) . . . . ? C44 C46 C47 C48 179.1(2) . . . . ? C46 C47 C49 C50 -1.4(3) . . . . ? C48 C47 C49 C50 178.6(2) . . . . ? C47 C49 C50 C43 1.8(3) . . . . ? C47 C49 C50 C51 -179.0(2) . . . . ? C44 C43 C50 C49 0.1(3) . . . . ? C41 C43 C50 C49 175.43(19) . . . . ? C44 C43 C50 C51 -179.11(19) . . . . ? C41 C43 C50 C51 -3.8(3) . . . . ?