# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Wang, Liying' 'Ma, Haiyan' _publ_contact_author_name 'Ma, Haiyan' _publ_contact_author_email haiyanma@ecust.edu.cn _publ_section_title ; Novel Zinc Complexes Supported by Multidentate Amino-Phenolate Ligands: Synthesis, Structure and Catalysis in Ring-Opening Polymerization of rac-Lactide ; # Attachment '- cd28470-4.cif' #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 772262' #TrackingRef '- cd28470-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H53 N3 O2 Si2 Zn' _chemical_formula_weight 609.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.0516(7) _cell_length_b 15.5157(9) _cell_length_c 18.0946(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3383.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6826 _cell_measurement_theta_min 4.836 _cell_measurement_theta_max 52.795 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.326 _exptl_crystal_size_min 0.265 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83755 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20151 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7318 _reflns_number_gt 6577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0353P)^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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(9) _chemical_absolute_configuration ad _refine_ls_number_reflns 7318 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.02656(3) 0.489291(17) 0.860565(16) 0.03447(9) Uani 1 1 d . . . Si1 Si 0.04267(7) 0.64232(5) 0.95942(4) 0.0413(2) Uani 1 1 d . . . Si2 Si -0.17977(7) 0.62151(5) 0.88731(5) 0.0397(2) Uani 1 1 d . . . N1 N -0.04479(17) 0.36399(12) 0.85382(11) 0.0313(5) Uani 1 1 d . . . N2 N 0.0480(2) 0.47977(14) 0.74286(12) 0.0425(6) Uani 1 1 d . . . N3 N -0.04445(19) 0.59242(13) 0.89772(13) 0.0386(5) Uani 1 1 d . . . O1 O 0.16666(15) 0.45166(11) 0.90186(11) 0.0402(5) Uani 1 1 d . . . O2 O -0.2789(2) 0.33955(16) 0.74025(12) 0.0670(7) Uani 1 1 d . . . C1 C 0.2082(2) 0.37179(16) 0.89990(14) 0.0338(6) Uani 1 1 d . . . C2 C 0.3244(2) 0.35725(17) 0.90072(15) 0.0358(6) Uani 1 1 d . . . C3 C 0.3616(2) 0.27249(18) 0.89706(15) 0.0413(7) Uani 1 1 d . . . H3 H 0.4378 0.2630 0.8959 0.050 Uiso 1 1 calc R . . C4 C 0.2925(3) 0.20177(17) 0.89500(16) 0.0411(7) Uani 1 1 d . . . C5 C 0.1800(2) 0.21691(17) 0.89671(15) 0.0396(7) Uani 1 1 d . . . H5 H 0.1316 0.1702 0.8962 0.048 Uiso 1 1 calc R . . C6 C 0.1365(2) 0.29986(16) 0.89920(15) 0.0345(6) Uani 1 1 d . . . C7 C 0.0143(2) 0.30977(16) 0.90949(15) 0.0381(6) Uani 1 1 d . . . H7A H 0.0013 0.3344 0.9580 0.046 Uiso 1 1 calc R . . H7B H -0.0189 0.2528 0.9091 0.046 Uiso 1 1 calc R . . C8 C -0.0206(3) 0.33532(15) 0.77696(13) 0.0361(6) Uani 1 1 d . . . H8A H -0.0724 0.2904 0.7629 0.043 Uiso 1 1 calc R . . H8B H 0.0537 0.3115 0.7747 0.043 Uiso 1 1 calc R . . C9 C -0.0299(3) 0.40971(17) 0.72332(15) 0.0459(7) Uani 1 1 d . . . H9A H -0.0139 0.3895 0.6737 0.055 Uiso 1 1 calc R . . H9B H -0.1052 0.4318 0.7238 0.055 Uiso 1 1 calc R . . C10 C -0.1662(2) 0.36522(16) 0.87028(16) 0.0360(6) Uani 1 1 d . . . H10A H -0.1995 0.4112 0.8415 0.043 Uiso 1 1 calc R . . H10B H -0.1754 0.3800 0.9220 0.043 Uiso 1 1 calc R . . C11 C -0.2313(2) 0.28374(16) 0.85570(16) 0.0356(6) Uani 1 1 d . . . C12 C -0.2432(2) 0.2209(2) 0.90957(17) 0.0433(7) Uani 1 1 d . . . H12 H -0.2081 0.2279 0.9550 0.052 Uiso 1 1 calc R . . C13 C -0.3063(3) 0.1482(2) 0.8968(2) 0.0542(8) Uani 1 1 d . . . H13 H -0.3132 0.1062 0.9331 0.065 Uiso 1 1 calc R . . C14 C -0.3587(3) 0.1384(2) 0.8305(2) 0.0606(9) Uani 1 1 d . . . H14 H -0.3999 0.0889 0.8216 0.073 Uiso 1 1 calc R . . C15 C -0.3515(3) 0.2006(2) 0.77659(19) 0.0561(9) Uani 1 1 d . . . H15 H -0.3886 0.1937 0.7319 0.067 Uiso 1 1 calc R . . C16 C -0.2886(2) 0.27343(19) 0.78951(16) 0.0437(7) Uani 1 1 d . . . C17 C 0.3385(3) 0.11118(17) 0.89278(19) 0.0560(9) Uani 1 1 d . . . H17A H 0.2784 0.0706 0.8918 0.084 Uiso 1 1 calc R . . H17B H 0.3832 0.1013 0.9359 0.084 Uiso 1 1 calc R . . H17C H 0.3832 0.1042 0.8493 0.084 Uiso 1 1 calc R . . C18 C 0.4080(2) 0.43191(19) 0.90822(18) 0.0467(8) Uani 1 1 d . . . C19 C 0.3995(3) 0.4932(2) 0.84228(19) 0.0670(10) Uani 1 1 d . . . H19A H 0.3251 0.5150 0.8388 0.101 Uiso 1 1 calc R . . H19B H 0.4178 0.4628 0.7977 0.101 Uiso 1 1 calc R . . H19C H 0.4501 0.5403 0.8489 0.101 Uiso 1 1 calc R . . C20 C 0.3847(3) 0.4820(2) 0.98004(19) 0.0659(10) Uani 1 1 d . . . H20A H 0.3102 0.5039 0.9790 0.099 Uiso 1 1 calc R . . H20B H 0.4359 0.5291 0.9843 0.099 Uiso 1 1 calc R . . H20C H 0.3933 0.4441 1.0216 0.099 Uiso 1 1 calc R . . C21 C 0.5284(3) 0.4006(2) 0.9124(2) 0.0735(11) Uani 1 1 d . . . H21A H 0.5771 0.4493 0.9173 0.110 Uiso 1 1 calc R . . H21B H 0.5466 0.3695 0.8682 0.110 Uiso 1 1 calc R . . H21C H 0.5371 0.3634 0.9544 0.110 Uiso 1 1 calc R . . C22 C 0.1626(3) 0.4568(2) 0.72267(17) 0.0543(8) Uani 1 1 d . . . H22A H 0.1846 0.4060 0.7493 0.081 Uiso 1 1 calc R . . H22B H 0.2113 0.5035 0.7350 0.081 Uiso 1 1 calc R . . H22C H 0.1665 0.4458 0.6705 0.081 Uiso 1 1 calc R . . C23 C 0.0180(4) 0.55988(19) 0.70333(19) 0.0666(10) Uani 1 1 d . . . H23A H 0.0250 0.5509 0.6510 0.100 Uiso 1 1 calc R . . H23B H 0.0668 0.6055 0.7184 0.100 Uiso 1 1 calc R . . H23C H -0.0572 0.5752 0.7149 0.100 Uiso 1 1 calc R . . C24 C -0.3588(4) 0.3483(3) 0.6833(2) 0.0857(13) Uani 1 1 d . . . H24A H -0.3511 0.3016 0.6489 0.129 Uiso 1 1 calc R . . H24B H -0.3476 0.4020 0.6581 0.129 Uiso 1 1 calc R . . H24C H -0.4319 0.3472 0.7044 0.129 Uiso 1 1 calc R . . C25 C -0.0106(3) 0.74463(19) 1.0016(2) 0.0646(10) Uani 1 1 d . . . H25A H -0.0134 0.7889 0.9645 0.097 Uiso 1 1 calc R . . H25B H 0.0381 0.7623 1.0408 0.097 Uiso 1 1 calc R . . H25C H -0.0837 0.7351 1.0211 0.097 Uiso 1 1 calc R . . C26 C 0.1747(3) 0.6717(2) 0.9122(2) 0.0622(10) Uani 1 1 d . . . H26A H 0.2052 0.6216 0.8886 0.093 Uiso 1 1 calc R . . H26B H 0.2266 0.6932 0.9480 0.093 Uiso 1 1 calc R . . H26C H 0.1604 0.7153 0.8759 0.093 Uiso 1 1 calc R . . C27 C 0.0723(3) 0.5711(2) 1.03966(18) 0.0580(9) Uani 1 1 d . . . H27A H 0.0050 0.5607 1.0666 0.087 Uiso 1 1 calc R . . H27B H 0.1254 0.5985 1.0715 0.087 Uiso 1 1 calc R . . H27C H 0.1019 0.5173 1.0223 0.087 Uiso 1 1 calc R . . C28 C -0.2641(3) 0.5911(2) 0.97031(19) 0.0623(10) Uani 1 1 d . . . H28A H -0.2573 0.5303 0.9791 0.093 Uiso 1 1 calc R . . H28B H -0.3406 0.6053 0.9617 0.093 Uiso 1 1 calc R . . H28C H -0.2376 0.6222 1.0127 0.093 Uiso 1 1 calc R . . C29 C -0.2527(3) 0.5760(2) 0.80458(18) 0.0611(9) Uani 1 1 d . . . H29A H -0.2402 0.6127 0.7627 0.092 Uiso 1 1 calc R . . H29B H -0.3308 0.5725 0.8144 0.092 Uiso 1 1 calc R . . H29C H -0.2243 0.5194 0.7942 0.092 Uiso 1 1 calc R . . C30 C -0.2004(3) 0.73965(19) 0.8709(2) 0.0718(11) Uani 1 1 d . . . H30A H -0.1862 0.7707 0.9158 0.108 Uiso 1 1 calc R . . H30B H -0.2755 0.7499 0.8553 0.108 Uiso 1 1 calc R . . H30C H -0.1503 0.7589 0.8331 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.03498(16) 0.02967(14) 0.03877(16) -0.00315(13) 0.00354(14) 0.00242(13) Si1 0.0410(5) 0.0332(4) 0.0497(5) -0.0069(3) 0.0036(4) -0.0001(4) Si2 0.0382(5) 0.0344(4) 0.0463(5) 0.0041(3) 0.0033(4) 0.0071(3) N1 0.0285(12) 0.0345(10) 0.0309(11) -0.0007(9) -0.0005(10) -0.0007(9) N2 0.0492(15) 0.0374(12) 0.0409(13) 0.0058(10) 0.0117(11) 0.0017(12) N3 0.0340(14) 0.0335(11) 0.0482(14) -0.0086(10) 0.0014(11) 0.0061(10) O1 0.0287(10) 0.0323(9) 0.0597(13) -0.0043(9) -0.0027(9) 0.0024(8) O2 0.0666(16) 0.0824(16) 0.0520(13) 0.0185(13) -0.0238(12) -0.0097(13) C1 0.0372(16) 0.0332(13) 0.0310(14) -0.0050(11) 0.0035(12) 0.0012(12) C2 0.0342(15) 0.0367(14) 0.0364(15) -0.0012(12) 0.0010(12) 0.0018(12) C3 0.0332(16) 0.0511(16) 0.0397(16) -0.0022(14) -0.0017(13) 0.0108(13) C4 0.0498(19) 0.0358(15) 0.0377(16) -0.0031(13) -0.0064(14) 0.0059(14) C5 0.0466(18) 0.0354(14) 0.0368(15) -0.0002(12) -0.0066(14) -0.0017(13) C6 0.0337(15) 0.0362(14) 0.0335(15) 0.0010(12) -0.0037(12) 0.0012(12) C7 0.0389(16) 0.0347(13) 0.0407(15) 0.0021(11) 0.0032(13) -0.0028(12) C8 0.0371(15) 0.0357(13) 0.0357(14) -0.0076(11) 0.0028(13) 0.0013(13) C9 0.0518(18) 0.0575(16) 0.0284(14) -0.0012(12) 0.0064(15) 0.0090(17) C10 0.0349(15) 0.0377(13) 0.0354(15) -0.0050(12) 0.0022(12) 0.0023(12) C11 0.0260(14) 0.0409(14) 0.0400(15) -0.0023(14) 0.0037(13) 0.0034(11) C12 0.0362(17) 0.0498(18) 0.0438(17) 0.0001(15) 0.0038(14) -0.0031(14) C13 0.053(2) 0.0427(17) 0.067(2) 0.0055(16) 0.0109(18) -0.0068(16) C14 0.045(2) 0.0499(19) 0.087(3) -0.0200(19) 0.0079(19) -0.0130(16) C15 0.044(2) 0.070(2) 0.055(2) -0.0198(18) -0.0042(16) -0.0053(17) C16 0.0352(17) 0.0542(17) 0.0418(17) -0.0043(14) -0.0012(13) 0.0018(14) C17 0.063(2) 0.0417(16) 0.064(2) -0.0060(16) -0.0092(17) 0.0153(16) C18 0.0311(16) 0.0470(17) 0.062(2) 0.0013(15) 0.0017(14) -0.0025(13) C19 0.051(2) 0.063(2) 0.087(3) 0.014(2) 0.0097(17) -0.0082(18) C20 0.052(2) 0.067(2) 0.079(2) -0.016(2) -0.0008(18) -0.0167(19) C21 0.0356(18) 0.072(2) 0.113(3) -0.002(2) -0.005(2) -0.003(2) C22 0.052(2) 0.0547(17) 0.056(2) -0.0044(16) 0.0143(16) -0.0029(16) C23 0.090(3) 0.0548(18) 0.055(2) 0.0162(16) 0.019(2) 0.012(2) C24 0.082(3) 0.117(3) 0.058(2) 0.007(2) -0.030(2) 0.010(3) C25 0.069(3) 0.0462(17) 0.079(2) -0.0207(16) 0.0024(19) 0.0042(18) C26 0.047(2) 0.058(2) 0.082(3) -0.0074(18) 0.0111(19) -0.0114(17) C27 0.069(2) 0.0529(19) 0.053(2) -0.0064(16) -0.0016(17) 0.0042(17) C28 0.053(2) 0.066(2) 0.068(2) 0.0046(19) 0.0143(18) -0.0030(18) C29 0.057(2) 0.066(2) 0.060(2) -0.0024(18) -0.0161(18) 0.0170(18) C30 0.073(3) 0.0429(17) 0.100(3) 0.014(2) 0.000(2) 0.0143(17) _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 Zn N3 1.935(2) . ? Zn O1 1.9366(18) . ? Zn N1 2.1293(19) . ? Zn N2 2.150(2) . ? Zn Si1 2.9790(8) . ? Si1 N3 1.717(2) . ? Si1 C27 1.859(3) . ? Si1 C26 1.862(3) . ? Si1 C25 1.875(3) . ? Si2 N3 1.703(2) . ? Si2 C30 1.874(3) . ? Si2 C28 1.874(3) . ? Si2 C29 1.874(3) . ? N1 C8 1.489(3) . ? N1 C7 1.493(3) . ? N1 C10 1.493(3) . ? N2 C22 1.473(4) . ? N2 C23 1.479(4) . ? N2 C9 1.479(4) . ? O1 C1 1.337(3) . ? O2 C16 1.364(4) . ? O2 C24 1.416(4) . ? C1 C6 1.411(4) . ? C1 C2 1.418(4) . ? C2 C3 1.391(4) . ? C2 C18 1.541(4) . ? C3 C4 1.378(4) . ? C3 H3 0.9300 . ? C4 C5 1.376(4) . ? C4 C17 1.512(4) . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 C7 1.493(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.512(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.511(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.386(4) . ? C11 C16 1.392(4) . ? C12 C13 1.381(4) . ? C12 H12 0.9300 . ? C13 C14 1.364(5) . ? C13 H13 0.9300 . ? C14 C15 1.374(5) . ? C14 H14 0.9300 . ? C15 C16 1.380(4) . ? C15 H15 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.529(4) . ? C18 C21 1.532(4) . ? C18 C20 1.540(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? 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 N3 Zn O1 120.05(9) . . ? N3 Zn N1 126.61(9) . . ? O1 Zn N1 95.67(7) . . ? N3 Zn N2 117.00(9) . . ? O1 Zn N2 104.89(9) . . ? N1 Zn N2 85.93(8) . . ? N3 Zn Si1 32.99(7) . . ? O1 Zn Si1 87.23(6) . . ? N1 Zn Si1 142.04(6) . . ? N2 Zn Si1 129.91(6) . . ? N3 Si1 C27 110.94(13) . . ? N3 Si1 C26 109.55(15) . . ? C27 Si1 C26 109.81(17) . . ? N3 Si1 C25 115.92(14) . . ? C27 Si1 C25 104.55(16) . . ? C26 Si1 C25 105.78(16) . . ? N3 Si1 Zn 37.85(7) . . ? C27 Si1 Zn 90.45(10) . . ? C26 Si1 Zn 88.59(11) . . ? C25 Si1 Zn 153.77(12) . . ? N3 Si2 C30 113.85(15) . . ? N3 Si2 C28 111.35(14) . . ? C30 Si2 C28 107.53(17) . . ? N3 Si2 C29 115.94(14) . . ? C30 Si2 C29 100.35(17) . . ? C28 Si2 C29 106.93(16) . . ? C8 N1 C7 111.63(19) . . ? C8 N1 C10 112.4(2) . . ? C7 N1 C10 109.9(2) . . ? C8 N1 Zn 104.32(14) . . ? C7 N1 Zn 106.45(15) . . ? C10 N1 Zn 111.87(14) . . ? C22 N2 C23 108.2(3) . . ? C22 N2 C9 111.0(2) . . ? C23 N2 C9 110.3(2) . . ? C22 N2 Zn 112.02(18) . . ? C23 N2 Zn 113.08(18) . . ? C9 N2 Zn 102.19(15) . . ? Si2 N3 Si1 122.56(13) . . ? Si2 N3 Zn 127.18(13) . . ? Si1 N3 Zn 109.17(12) . . ? C1 O1 Zn 126.57(17) . . ? C16 O2 C24 119.3(3) . . ? O1 C1 C6 120.2(2) . . ? O1 C1 C2 121.1(2) . . ? C6 C1 C2 118.6(2) . . ? C3 C2 C1 117.9(3) . . ? C3 C2 C18 120.3(3) . . ? C1 C2 C18 121.8(2) . . ? C4 C3 C2 124.0(3) . . ? C4 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C5 C4 C3 117.3(2) . . ? C5 C4 C17 121.4(3) . . ? C3 C4 C17 121.3(3) . . ? C4 C5 C6 122.0(3) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 C7 118.1(2) . . ? C1 C6 C7 121.4(2) . . ? C6 C7 N1 116.4(2) . . ? C6 C7 H7A 108.2 . . ? N1 C7 H7A 108.2 . . ? C6 C7 H7B 108.2 . . ? N1 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 110.91(19) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C8 111.1(2) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N1 C10 C11 117.6(2) . . ? N1 C10 H10A 107.9 . . ? C11 C10 H10A 107.9 . . ? N1 C10 H10B 107.9 . . ? C11 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? C12 C11 C16 118.2(3) . . ? C12 C11 C10 121.3(3) . . ? C16 C11 C10 120.3(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 119.6(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? O2 C16 C15 123.5(3) . . ? O2 C16 C11 115.7(3) . . ? C15 C16 C11 120.8(3) . . ? C4 C17 H17A 109.5 . . ? C4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C21 107.5(3) . . ? C19 C18 C20 109.4(3) . . ? C21 C18 C20 106.9(3) . . ? C19 C18 C2 110.8(3) . . ? C21 C18 C2 112.7(2) . . ? C20 C18 C2 109.5(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C24 H24A 109.5 . . ? O2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 O1 Zn Si1 N3 -174.49(14) . . . . ? N1 Zn Si1 N3 -78.80(16) . . . . ? N2 Zn Si1 N3 78.36(16) . . . . ? N3 Zn Si1 C27 124.92(17) . . . . ? O1 Zn Si1 C27 -49.56(13) . . . . ? N1 Zn Si1 C27 46.12(15) . . . . ? N2 Zn Si1 C27 -156.71(14) . . . . ? N3 Zn Si1 C26 -125.27(17) . . . . ? O1 Zn Si1 C26 60.24(14) . . . . ? N1 Zn Si1 C26 155.93(15) . . . . ? N2 Zn Si1 C26 -46.91(15) . . . . ? N3 Zn Si1 C25 -0.8(3) . . . . ? O1 Zn Si1 C25 -175.3(3) . . . . ? N1 Zn Si1 C25 -79.6(3) . . . . ? N2 Zn Si1 C25 77.5(3) . . . . ? N3 Zn N1 C8 131.03(16) . . . . ? O1 Zn N1 C8 -94.48(16) . . . . ? N2 Zn N1 C8 10.10(16) . . . . ? Si1 Zn N1 C8 172.74(12) . . . . ? N3 Zn N1 C7 -110.81(17) . . . . ? O1 Zn N1 C7 23.68(16) . . . . ? N2 Zn N1 C7 128.26(16) . . . . ? Si1 Zn N1 C7 -69.10(18) . . . . ? N3 Zn N1 C10 9.2(2) . . . . ? O1 Zn N1 C10 143.71(17) . . . . ? N2 Zn N1 C10 -111.71(17) . . . . ? Si1 Zn N1 C10 50.9(2) . . . . ? N3 Zn N2 C22 130.02(18) . . . . ? O1 Zn N2 C22 -5.8(2) . . . . ? N1 Zn N2 C22 -100.58(19) . . . . ? Si1 Zn N2 C22 93.26(18) . . . . ? N3 Zn N2 C23 7.4(3) . . . . ? O1 Zn N2 C23 -128.4(2) . . . . ? N1 Zn N2 C23 136.8(2) . . . . ? Si1 Zn N2 C23 -29.3(3) . . . . ? N3 Zn N2 C9 -111.15(17) . . . . ? O1 Zn N2 C9 113.04(17) . . . . ? N1 Zn N2 C9 18.24(17) . . . . ? Si1 Zn N2 C9 -147.91(14) . . . . ? C30 Si2 N3 Si1 52.0(2) . . . . ? C28 Si2 N3 Si1 -69.7(2) . . . . ? C29 Si2 N3 Si1 167.72(16) . . . . ? C30 Si2 N3 Zn -141.25(19) . . . . ? C28 Si2 N3 Zn 96.98(19) . . . . ? C29 Si2 N3 Zn -25.6(2) . . . . ? C27 Si1 N3 Si2 107.44(18) . . . . ? C26 Si1 N3 Si2 -131.16(18) . . . . ? C25 Si1 N3 Si2 -11.6(2) . . . . ? Zn Si1 N3 Si2 168.8(2) . . . . ? C27 Si1 N3 Zn -61.39(17) . . . . ? C26 Si1 N3 Zn 60.01(16) . . . . ? C25 Si1 N3 Zn 179.59(14) . . . . ? O1 Zn N3 Si2 -161.80(13) . . . . ? N1 Zn N3 Si2 -36.9(2) . . . . ? N2 Zn N3 Si2 69.31(18) . . . . ? Si1 Zn N3 Si2 -168.2(3) . . . . ? O1 Zn N3 Si1 6.37(16) . . . . ? N1 Zn N3 Si1 131.26(11) . . . . ? N2 Zn N3 Si1 -122.53(12) . . . . ? N3 Zn O1 C1 157.6(2) . . . . ? N1 Zn O1 C1 19.1(2) . . . . ? N2 Zn O1 C1 -68.2(2) . . . . ? Si1 Zn O1 C1 161.1(2) . . . . ? Zn O1 C1 C6 -30.3(3) . . . . ? Zn O1 C1 C2 151.6(2) . . . . ? O1 C1 C2 C3 -178.7(2) . . . . ? C6 C1 C2 C3 3.1(4) . . . . ? O1 C1 C2 C18 3.4(4) . . . . ? C6 C1 C2 C18 -174.7(3) . . . . ? C1 C2 C3 C4 -2.1(4) . . . . ? C18 C2 C3 C4 175.8(3) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C2 C3 C4 C17 -178.6(3) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C17 C4 C5 C6 179.6(3) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? C4 C5 C6 C7 -173.2(3) . . . . ? O1 C1 C6 C5 179.6(2) . . . . ? C2 C1 C6 C5 -2.3(4) . . . . ? O1 C1 C6 C7 -7.3(4) . . . . ? C2 C1 C6 C7 170.9(2) . . . . ? C5 C6 C7 N1 -126.5(3) . . . . ? C1 C6 C7 N1 60.2(3) . . . . ? C8 N1 C7 C6 52.7(3) . . . . ? C10 N1 C7 C6 178.2(2) . . . . ? Zn N1 C7 C6 -60.5(2) . . . . ? C7 N1 C8 C9 -152.0(2) . . . . ? C10 N1 C8 C9 84.0(3) . . . . ? Zn N1 C8 C9 -37.5(3) . . . . ? C22 N2 C9 C8 75.1(3) . . . . ? C23 N2 C9 C8 -165.0(2) . . . . ? Zn N2 C9 C8 -44.5(2) . . . . ? N1 C8 C9 N2 59.1(3) . . . . ? C8 N1 C10 C11 53.4(3) . . . . ? C7 N1 C10 C11 -71.6(3) . . . . ? Zn N1 C10 C11 170.41(19) . . . . ? N1 C10 C11 C12 89.4(3) . . . . ? N1 C10 C11 C16 -96.0(3) . . . . ? C16 C11 C12 C13 2.8(4) . . . . ? C10 C11 C12 C13 177.5(3) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C12 C13 C14 C15 -1.3(5) . . . . ? C13 C14 C15 C16 1.1(5) . . . . ? C24 O2 C16 C15 19.0(5) . . . . ? C24 O2 C16 C11 -160.3(3) . . . . ? C14 C15 C16 O2 -178.2(3) . . . . ? C14 C15 C16 C11 1.1(5) . . . . ? C12 C11 C16 O2 176.4(3) . . . . ? C10 C11 C16 O2 1.6(4) . . . . ? C12 C11 C16 C15 -3.0(4) . . . . ? C10 C11 C16 C15 -177.8(3) . . . . ? C3 C2 C18 C19 119.2(3) . . . . ? C1 C2 C18 C19 -63.0(4) . . . . ? C3 C2 C18 C21 -1.2(4) . . . . ? C1 C2 C18 C21 176.6(3) . . . . ? C3 C2 C18 C20 -120.0(3) . . . . ? C1 C2 C18 C20 57.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.443 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.053 # End ======================================================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 772263' #TrackingRef '- cd28470-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H63 N3 O2 Si2 Zn' _chemical_formula_weight 679.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.9250(10) _cell_length_b 24.604(3) _cell_length_c 18.129(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.663(2) _cell_angle_gamma 90.00 _cell_volume 3961.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3515 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8422 _exptl_absorpt_correction_T_max 0.8708 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20329 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7020 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-9(Sheldrick,1990) _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0458P)^2^+0.6882P] 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_extinction_coef ? _refine_ls_number_reflns 7020 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.36029(4) 0.336077(17) 0.70049(2) 0.04209(14) Uani 1 1 d . . . Si1 Si 0.19454(12) 0.41198(5) 0.56806(6) 0.0599(3) Uani 1 1 d . . . Si2 Si 0.43968(14) 0.33244(5) 0.54440(6) 0.0668(3) Uani 1 1 d . . . C1 C 0.6132(3) 0.27841(14) 0.78268(17) 0.0397(8) Uani 1 1 d . . . C2 C 0.6815(4) 0.22773(14) 0.80441(17) 0.0420(8) Uani 1 1 d . . . C3 C 0.7754(4) 0.22625(14) 0.87040(18) 0.0475(9) Uani 1 1 d . . . H3 H 0.8184 0.1931 0.8853 0.057 Uiso 1 1 calc R . . C4 C 0.8091(4) 0.27119(15) 0.91548(19) 0.0476(9) Uani 1 1 d . . . C5 C 0.7478(4) 0.32007(14) 0.89134(18) 0.0447(9) Uani 1 1 d . . . H5 H 0.7712 0.3511 0.9194 0.054 Uiso 1 1 calc R . . C6 C 0.6517(3) 0.32472(13) 0.82609(17) 0.0378(8) Uani 1 1 d . . . C7 C 0.6620(4) 0.17752(14) 0.75423(19) 0.0476(9) Uani 1 1 d . . . C8 C 0.4955(4) 0.16262(15) 0.7373(2) 0.0602(10) Uani 1 1 d . . . H8A H 0.4866 0.1314 0.7054 0.090 Uiso 1 1 calc R . . H8B H 0.4424 0.1927 0.7132 0.090 Uiso 1 1 calc R . . H8C H 0.4533 0.1545 0.7827 0.090 Uiso 1 1 calc R . . C9 C 0.7291(4) 0.18990(16) 0.68124(19) 0.0635(11) Uani 1 1 d . . . H9A H 0.8340 0.1985 0.6915 0.095 Uiso 1 1 calc R . . H9B H 0.6773 0.2203 0.6572 0.095 Uiso 1 1 calc R . . H9C H 0.7179 0.1587 0.6494 0.095 Uiso 1 1 calc R . . C10 C 0.7426(5) 0.12711(15) 0.7896(2) 0.0727(12) Uani 1 1 d . . . H10A H 0.7029 0.1189 0.8356 0.109 Uiso 1 1 calc R . . H10B H 0.8486 0.1343 0.7985 0.109 Uiso 1 1 calc R . . H10C H 0.7266 0.0967 0.7565 0.109 Uiso 1 1 calc R . . C11 C 0.9110(4) 0.26675(17) 0.9875(2) 0.0691(12) Uani 1 1 d . . . H11A H 0.9514 0.2306 0.9924 0.104 Uiso 1 1 calc R . . H11B H 0.8541 0.2744 1.0285 0.104 Uiso 1 1 calc R . . H11C H 0.9920 0.2924 0.9870 0.104 Uiso 1 1 calc R . . C12 C 0.6042(3) 0.38065(13) 0.80035(17) 0.0411(8) Uani 1 1 d . . . H12A H 0.6467 0.4066 0.8369 0.049 Uiso 1 1 calc R . . H12B H 0.6481 0.3880 0.7545 0.049 Uiso 1 1 calc R . . C13 C 0.4103(4) 0.44798(14) 0.76305(18) 0.0456(9) Uani 1 1 d . . . H13A H 0.3024 0.4537 0.7556 0.055 Uiso 1 1 calc R . . H13B H 0.4495 0.4527 0.7154 0.055 Uiso 1 1 calc R . . C14 C 0.4781(3) 0.49190(13) 0.81523(17) 0.0371(8) Uani 1 1 d . . . C15 C 0.6244(3) 0.51125(14) 0.81246(18) 0.0417(8) Uani 1 1 d . . . C16 C 0.6905(3) 0.54614(14) 0.8680(2) 0.0468(9) Uani 1 1 d . . . C17 C 0.6000(4) 0.56388(14) 0.92097(19) 0.0494(9) Uani 1 1 d . . . H17 H 0.6416 0.5874 0.9576 0.059 Uiso 1 1 calc R . . C18 C 0.4511(4) 0.54857(14) 0.92241(17) 0.0431(9) Uani 1 1 d . . . C19 C 0.3937(3) 0.51189(14) 0.86974(18) 0.0424(8) Uani 1 1 d . . . H19 H 0.2950 0.5000 0.8706 0.051 Uiso 1 1 calc R . . C20 C 0.6655(5) 0.51783(19) 0.6848(2) 0.0886(15) Uani 1 1 d . . . H20A H 0.7282 0.5033 0.6495 0.106 Uiso 1 1 calc R . . H20B H 0.6785 0.5565 0.6880 0.106 Uiso 1 1 calc R . . H20C H 0.5621 0.5096 0.6694 0.106 Uiso 1 1 calc R . . C21 C 0.8578(4) 0.56261(19) 0.8725(3) 0.0825(14) Uani 1 1 d . . . C22 C 0.9024(5) 0.5954(2) 0.9433(4) 0.143(3) Uani 1 1 d . . . H22A H 1.0057 0.6064 0.9443 0.215 Uiso 1 1 calc R . . H22B H 0.8898 0.5733 0.9859 0.215 Uiso 1 1 calc R . . H22C H 0.8394 0.6270 0.9441 0.215 Uiso 1 1 calc R . . C23 C 0.8917(6) 0.5956(3) 0.8063(4) 0.172(3) Uani 1 1 d . . . H23A H 0.8327 0.6283 0.8041 0.158 Uiso 1 1 calc R . . H23B H 0.8672 0.5748 0.7620 0.158 Uiso 1 1 calc R . . H23C H 0.9967 0.6048 0.8106 0.158 Uiso 1 1 calc R . . C24 C 0.9524(5) 0.5101(3) 0.8775(4) 0.148(3) Uani 1 1 d . . . H24A H 1.0570 0.5192 0.8875 0.222 Uiso 1 1 calc R . . H24B H 0.9369 0.4908 0.8314 0.222 Uiso 1 1 calc R . . H24C H 0.9222 0.4877 0.9168 0.222 Uiso 1 1 calc R . . C25 C 0.3580(4) 0.57104(16) 0.98004(19) 0.0626(11) Uani 1 1 d . . . H25A H 0.2536 0.5706 0.9613 0.075 Uiso 1 1 calc R . . H25B H 0.3885 0.6077 0.9916 0.075 Uiso 1 1 calc R . . H25C H 0.3723 0.5492 1.0240 0.075 Uiso 1 1 calc R . . C26 C 0.3577(4) 0.37509(15) 0.85213(18) 0.0480(9) Uani 1 1 d . . . H26A H 0.3569 0.4055 0.8861 0.058 Uiso 1 1 calc R . . H26B H 0.4096 0.3450 0.8782 0.058 Uiso 1 1 calc R . . C27 C 0.1970(4) 0.35855(17) 0.8264(2) 0.0573(10) Uani 1 1 d . . . H27A H 0.1460 0.3479 0.8690 0.069 Uiso 1 1 calc R . . H27B H 0.1437 0.3894 0.8031 0.069 Uiso 1 1 calc R . . C28 C 0.2345(5) 0.26138(17) 0.8112(2) 0.0755(13) Uani 1 1 d . . . H28A H 0.3347 0.2643 0.8355 0.091 Uiso 1 1 calc R . . H28B H 0.2307 0.2323 0.7757 0.091 Uiso 1 1 calc R . . H28C H 0.1653 0.2540 0.8473 0.091 Uiso 1 1 calc R . . C29 C 0.0382(4) 0.3063(2) 0.7353(2) 0.0881(15) Uani 1 1 d . . . H29A H -0.0290 0.2955 0.7708 0.106 Uiso 1 1 calc R . . H29B H 0.0387 0.2789 0.6975 0.106 Uiso 1 1 calc R . . H29C H 0.0049 0.3402 0.7132 0.106 Uiso 1 1 calc R . . C30 C 0.0641(5) 0.4368(2) 0.6354(2) 0.0985(17) Uani 1 1 d . . . H30A H -0.0057 0.4085 0.6446 0.118 Uiso 1 1 calc R . . H30B H 0.0098 0.4680 0.6151 0.118 Uiso 1 1 calc R . . H30C H 0.1213 0.4467 0.6810 0.118 Uiso 1 1 calc R . . C31 C 0.2909(5) 0.47503(18) 0.5405(3) 0.0932(15) Uani 1 1 d . . . H31A H 0.3397 0.4923 0.5839 0.112 Uiso 1 1 calc R . . H31B H 0.2180 0.4994 0.5161 0.112 Uiso 1 1 calc R . . H31C H 0.3646 0.4658 0.5074 0.112 Uiso 1 1 calc R . . C32 C 0.0627(5) 0.3907(2) 0.4862(3) 0.1048(18) Uani 1 1 d . . . H32A H 0.1198 0.3793 0.4467 0.126 Uiso 1 1 calc R . . H32B H -0.0004 0.4208 0.4698 0.126 Uiso 1 1 calc R . . H32C H 0.0013 0.3611 0.5001 0.126 Uiso 1 1 calc R . . C33 C 0.4200(7) 0.3563(3) 0.4452(2) 0.135(2) Uani 1 1 d . . . H33A H 0.3210 0.3476 0.4226 0.162 Uiso 1 1 calc R . . H33B H 0.4938 0.3385 0.4186 0.162 Uiso 1 1 calc R . . H33C H 0.4350 0.3949 0.4438 0.162 Uiso 1 1 calc R . . C34 C 0.6405(5) 0.3468(2) 0.5781(2) 0.0908(15) Uani 1 1 d . . . H34A H 0.6565 0.3854 0.5800 0.109 Uiso 1 1 calc R . . H34B H 0.7051 0.3307 0.5448 0.109 Uiso 1 1 calc R . . H34C H 0.6630 0.3317 0.6267 0.109 Uiso 1 1 calc R . . C35 C 0.4101(5) 0.25752(18) 0.5393(2) 0.0914(15) Uani 1 1 d . . . H35A H 0.4224 0.2424 0.5883 0.110 Uiso 1 1 calc R . . H35B H 0.4824 0.2415 0.5099 0.110 Uiso 1 1 calc R . . H35C H 0.3103 0.2500 0.5169 0.110 Uiso 1 1 calc R . . N1 N 0.4383(3) 0.39073(11) 0.78745(13) 0.0385(7) Uani 1 1 d . . . N2 N 0.1927(3) 0.31272(13) 0.77300(16) 0.0518(8) Uani 1 1 d . . . N3 N 0.3178(3) 0.36233(12) 0.60029(14) 0.0519(8) Uani 1 1 d . . . O1 O 0.5182(2) 0.28281(9) 0.72090(12) 0.0451(6) Uani 1 1 d . . . O2 O 0.7072(2) 0.49404(10) 0.75594(13) 0.0547(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0412(2) 0.0486(3) 0.0369(2) -0.0051(2) 0.00594(16) -0.0042(2) Si1 0.0541(6) 0.0676(8) 0.0555(7) 0.0031(6) -0.0071(5) 0.0015(6) Si2 0.0804(8) 0.0826(9) 0.0396(6) 0.0013(6) 0.0163(5) 0.0132(7) C1 0.0404(19) 0.042(2) 0.038(2) -0.0080(16) 0.0098(15) -0.0023(17) C2 0.048(2) 0.037(2) 0.042(2) -0.0082(17) 0.0120(17) -0.0052(17) C3 0.052(2) 0.040(2) 0.050(2) -0.0012(18) 0.0053(17) 0.0032(18) C4 0.054(2) 0.044(2) 0.044(2) -0.0048(18) 0.0007(17) 0.0021(19) C5 0.050(2) 0.041(2) 0.043(2) -0.0160(17) 0.0025(16) 0.0003(18) C6 0.0384(18) 0.032(2) 0.0438(19) -0.0052(15) 0.0073(15) 0.0017(15) C7 0.057(2) 0.037(2) 0.049(2) -0.0096(17) 0.0089(17) -0.0011(18) C8 0.077(3) 0.046(2) 0.058(2) -0.018(2) 0.011(2) -0.015(2) C9 0.075(3) 0.060(3) 0.058(3) -0.018(2) 0.021(2) -0.001(2) C10 0.101(3) 0.039(2) 0.077(3) -0.011(2) 0.005(2) 0.008(2) C11 0.075(3) 0.064(3) 0.063(3) -0.008(2) -0.017(2) 0.003(2) C12 0.038(2) 0.037(2) 0.048(2) -0.0091(17) 0.0035(16) -0.0004(16) C13 0.044(2) 0.050(2) 0.042(2) -0.0029(18) 0.0033(16) 0.0051(18) C14 0.0368(18) 0.034(2) 0.0403(19) 0.0003(16) 0.0009(15) 0.0073(16) C15 0.0389(19) 0.036(2) 0.051(2) 0.0046(17) 0.0107(17) 0.0088(17) C16 0.0342(19) 0.041(2) 0.065(2) 0.0047(19) 0.0012(17) 0.0013(17) C17 0.051(2) 0.043(2) 0.052(2) -0.0073(18) -0.0116(18) 0.0057(19) C18 0.047(2) 0.041(2) 0.041(2) -0.0023(17) -0.0006(16) 0.0099(18) C19 0.0341(18) 0.042(2) 0.051(2) -0.0007(18) 0.0042(16) 0.0040(17) C20 0.108(4) 0.092(4) 0.072(3) 0.022(3) 0.042(3) -0.001(3) C21 0.038(2) 0.073(3) 0.135(4) -0.024(3) 0.000(3) -0.004(2) C22 0.051(3) 0.141(5) 0.231(7) -0.096(5) -0.020(4) -0.018(3) C23 0.092(4) 0.188(7) 0.242(8) 0.046(6) 0.049(5) -0.081(5) C24 0.042(3) 0.161(6) 0.234(7) -0.074(5) -0.026(3) 0.032(3) C25 0.072(3) 0.068(3) 0.048(2) -0.011(2) 0.0084(19) 0.020(2) C26 0.053(2) 0.051(2) 0.041(2) -0.0082(18) 0.0091(17) 0.0018(19) C27 0.054(2) 0.067(3) 0.053(2) -0.005(2) 0.0214(19) -0.006(2) C28 0.086(3) 0.068(3) 0.079(3) 0.002(3) 0.040(2) -0.014(3) C29 0.059(3) 0.115(4) 0.092(3) -0.012(3) 0.014(2) -0.035(3) C30 0.071(3) 0.125(5) 0.100(4) 0.011(3) 0.009(3) 0.036(3) C31 0.094(3) 0.075(3) 0.108(4) 0.015(3) -0.002(3) -0.003(3) C32 0.095(4) 0.110(4) 0.101(4) -0.003(3) -0.037(3) -0.003(3) C33 0.188(6) 0.168(6) 0.056(3) 0.019(3) 0.047(4) 0.061(5) C34 0.079(3) 0.104(4) 0.096(4) -0.004(3) 0.045(3) 0.000(3) C35 0.107(4) 0.095(4) 0.069(3) -0.024(3) -0.009(3) 0.015(3) N1 0.0404(16) 0.0361(17) 0.0392(16) -0.0044(13) 0.0057(12) -0.0015(13) N2 0.0497(18) 0.057(2) 0.0508(18) -0.0045(16) 0.0131(15) -0.0105(16) N3 0.0520(18) 0.064(2) 0.0400(17) 0.0017(15) 0.0062(14) 0.0066(16) O1 0.0527(14) 0.0432(15) 0.0387(13) -0.0100(11) 0.0015(11) 0.0031(12) O2 0.0538(15) 0.0526(17) 0.0616(16) 0.0057(13) 0.0263(13) 0.0089(13) _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 N3 1.930(3) . ? Zn1 O1 1.934(2) . ? Zn1 N1 2.136(2) . ? Zn1 N2 2.164(3) . ? Si1 N3 1.708(3) . ? Si1 C31 1.865(4) . ? Si1 C30 1.871(4) . ? Si1 C32 1.875(4) . ? Si2 N3 1.722(3) . ? Si2 C35 1.863(5) . ? Si2 C34 1.869(4) . ? Si2 C33 1.883(4) . ? C1 O1 1.341(3) . ? C1 C6 1.408(4) . ? C1 C2 1.426(5) . ? C2 C3 1.392(4) . ? C2 C7 1.534(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.375(4) . ? C4 C11 1.519(5) . ? C5 C6 1.396(4) . ? C5 H5 0.9300 . ? C6 C12 1.501(4) . ? C7 C8 1.531(5) . ? C7 C9 1.536(5) . ? C7 C10 1.541(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N1 1.497(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.490(4) . ? C13 C14 1.522(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.390(4) . ? C14 C15 1.396(4) . ? C15 O2 1.387(4) . ? C15 C16 1.407(5) . ? C16 C17 1.385(5) . ? C16 C21 1.542(5) . ? C17 C18 1.383(5) . ? C17 H17 0.9300 . ? C18 C19 1.376(4) . ? C18 C25 1.503(4) . ? C19 H19 0.9300 . ? C20 O2 1.431(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C23 1.504(7) . ? C21 C22 1.535(6) . ? C21 C24 1.540(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N1 1.486(4) . ? C26 C27 1.519(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N2 1.484(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N2 1.471(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N2 1.487(4) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 N3 Zn1 O1 118.60(11) . . ? N3 Zn1 N1 120.23(12) . . ? O1 Zn1 N1 96.15(9) . . ? N3 Zn1 N2 125.27(12) . . ? O1 Zn1 N2 103.77(11) . . ? N1 Zn1 N2 85.03(10) . . ? N3 Si1 C31 112.83(18) . . ? N3 Si1 C30 115.58(17) . . ? C31 Si1 C30 103.6(2) . . ? N3 Si1 C32 113.8(2) . . ? C31 Si1 C32 106.8(2) . . ? C30 Si1 C32 103.0(2) . . ? N3 Si2 C35 110.92(19) . . ? N3 Si2 C34 111.59(18) . . ? C35 Si2 C34 109.3(2) . . ? N3 Si2 C33 115.1(2) . . ? C35 Si2 C33 105.1(2) . . ? C34 Si2 C33 104.4(2) . . ? O1 C1 C6 120.1(3) . . ? O1 C1 C2 121.3(3) . . ? C6 C1 C2 118.6(3) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C7 120.8(3) . . ? C1 C2 C7 121.3(3) . . ? C4 C3 C2 124.2(3) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C11 121.5(3) . . ? C3 C4 C11 121.6(3) . . ? C4 C5 C6 122.2(3) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C12 118.0(3) . . ? C1 C6 C12 121.5(3) . . ? C8 C7 C2 111.3(3) . . ? C8 C7 C9 109.1(3) . . ? C2 C7 C9 108.7(3) . . ? C8 C7 C10 107.1(3) . . ? C2 C7 C10 112.4(3) . . ? C9 C7 C10 108.2(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C6 116.5(3) . . ? N1 C12 H12A 108.2 . . ? C6 C12 H12A 108.2 . . ? N1 C12 H12B 108.2 . . ? C6 C12 H12B 108.2 . . ? H12A C12 H12B 107.3 . . ? N1 C13 C14 116.2(3) . . ? N1 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C19 C14 C15 118.6(3) . . ? C19 C14 C13 118.9(3) . . ? C15 C14 C13 122.4(3) . . ? O2 C15 C14 119.4(3) . . ? O2 C15 C16 119.9(3) . . ? C14 C15 C16 120.6(3) . . ? C17 C16 C15 117.2(3) . . ? C17 C16 C21 120.5(3) . . ? C15 C16 C21 122.3(3) . . ? C18 C17 C16 123.6(3) . . ? C18 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C19 C18 C17 117.3(3) . . ? C19 C18 C25 122.0(3) . . ? C17 C18 C25 120.7(3) . . ? C18 C19 C14 122.3(3) . . ? C18 C19 H19 118.8 . . ? C14 C19 H19 118.8 . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 109.1(5) . . ? C23 C21 C24 110.3(5) . . ? C22 C21 C24 107.2(4) . . ? C23 C21 C16 111.6(4) . . ? C22 C21 C16 110.6(4) . . ? C24 C21 C16 107.8(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 110.1(3) . . ? N1 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? N1 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.2 . . ? N2 C27 C26 111.5(3) . . ? N2 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? N2 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 H29A 109.5 . . ? N2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C26 N1 C13 113.5(2) . . ? C26 N1 C12 112.5(2) . . ? C13 N1 C12 109.7(2) . . ? C26 N1 Zn1 105.75(19) . . ? C13 N1 Zn1 110.07(18) . . ? C12 N1 Zn1 104.85(18) . . ? C28 N2 C27 110.9(3) . . ? C28 N2 C29 107.8(3) . . ? C27 N2 C29 110.1(3) . . ? C28 N2 Zn1 110.9(2) . . ? C27 N2 Zn1 102.7(2) . . ? C29 N2 Zn1 114.5(2) . . ? Si1 N3 Si2 121.79(16) . . ? Si1 N3 Zn1 128.41(16) . . ? Si2 N3 Zn1 109.52(15) . . ? C1 O1 Zn1 127.1(2) . . ? C15 O2 C20 115.5(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.294 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.051 # End ======================================================================= data_7 _database_code_depnum_ccdc_archive 'CCDC 772264' #TrackingRef '- cd28470-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H28 Cl2 N2 O2 Zn' _chemical_formula_weight 476.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5566(12) _cell_length_b 18.482(2) _cell_length_c 12.2472(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.060(2) _cell_angle_gamma 90.00 _cell_volume 2271.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1141 _cell_measurement_theta_min 4.408 _cell_measurement_theta_max 36.050 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.123 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7298 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12375 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.1379 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4440 _reflns_number_gt 2056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0271P)^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_extinction_coef ? _refine_ls_number_reflns 4440 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.27077(6) 0.07671(3) 0.71803(5) 0.0634(2) Uani 1 1 d . . . Cl1 Cl 0.96776(13) 0.10636(8) 1.02672(12) 0.0824(5) Uani 1 1 d . . . Cl2 Cl 0.64455(14) -0.01544(7) 0.64375(12) 0.0731(4) Uani 1 1 d . . . O1 O 0.4332(3) 0.02174(16) 0.7413(3) 0.0563(9) Uani 1 1 d . . . O2 O 0.2028(4) 0.30315(18) 0.9154(3) 0.0753(11) Uani 1 1 d . . . N1 N 0.3506(3) 0.14066(19) 0.8712(3) 0.0425(10) Uani 1 1 d . . . N2 N 0.3035(5) 0.1740(2) 0.6313(4) 0.0659(13) Uani 1 1 d . . . C1 C 0.2530(5) 0.2742(3) 1.0227(5) 0.0547(14) Uani 1 1 d . . . C2 C 0.2841(6) 0.3144(3) 1.1229(6) 0.0767(18) Uani 1 1 d . . . H2 H 0.2737 0.3644 1.1197 0.092 Uiso 1 1 calc R . . C3 C 0.3303(6) 0.2799(4) 1.2267(5) 0.093(2) Uani 1 1 d . . . H3 H 0.3516 0.3071 1.2939 0.112 Uiso 1 1 calc R . . C4 C 0.3456(6) 0.2066(4) 1.2337(5) 0.098(2) Uani 1 1 d . . . H4 H 0.3758 0.1838 1.3048 0.118 Uiso 1 1 calc R . . C5 C 0.3157(5) 0.1671(3) 1.1340(5) 0.0682(16) Uani 1 1 d . . . H5 H 0.3257 0.1171 1.1385 0.082 Uiso 1 1 calc R . . C6 C 0.2708(4) 0.1997(3) 1.0267(4) 0.0483(13) Uani 1 1 d . . . C7 C 0.2398(4) 0.1542(2) 0.9189(4) 0.0537(13) Uani 1 1 d . . . H7A H 0.2066 0.1077 0.9348 0.064 Uiso 1 1 calc R . . H7B H 0.1682 0.1775 0.8599 0.064 Uiso 1 1 calc R . . C8 C 0.4030(4) 0.2073(2) 0.8352(4) 0.0484(13) Uani 1 1 d . . . H8A H 0.4928 0.1987 0.8329 0.058 Uiso 1 1 calc R . . H8B H 0.4070 0.2453 0.8909 0.058 Uiso 1 1 calc R . . C9 C 0.3159(5) 0.2317(3) 0.7180(4) 0.0599(15) Uani 1 1 d . . . H9A H 0.2281 0.2442 0.7218 0.072 Uiso 1 1 calc R . . H9B H 0.3541 0.2746 0.6950 0.072 Uiso 1 1 calc R . . C10 C 0.4570(4) 0.0974(2) 0.9531(4) 0.0492(13) Uani 1 1 d . . . H10A H 0.4179 0.0531 0.9704 0.059 Uiso 1 1 calc R . . H10B H 0.4905 0.1245 1.0242 0.059 Uiso 1 1 calc R . . C11 C 0.5722(5) 0.0782(2) 0.9120(4) 0.0448(12) Uani 1 1 d . . . C12 C 0.7010(5) 0.0964(2) 0.9786(4) 0.0485(13) Uani 1 1 d . . . H12 H 0.7139 0.1208 1.0476 0.058 Uiso 1 1 calc R . . C13 C 0.8086(5) 0.0792(3) 0.9445(4) 0.0521(13) Uani 1 1 d . . . C14 C 0.7922(5) 0.0442(2) 0.8434(5) 0.0551(14) Uani 1 1 d . . . H14 H 0.8657 0.0326 0.8203 0.066 Uiso 1 1 calc R . . C15 C 0.6662(5) 0.0261(2) 0.7755(4) 0.0467(13) Uani 1 1 d . . . C16 C 0.5500(5) 0.0413(2) 0.8064(4) 0.0470(13) Uani 1 1 d . . . C17 C 0.1873(6) 0.1884(3) 0.5282(5) 0.120(3) Uani 1 1 d . . . H17A H 0.1974 0.2349 0.4971 0.180 Uiso 1 1 calc R . . H17B H 0.1071 0.1878 0.5495 0.180 Uiso 1 1 calc R . . H17C H 0.1822 0.1517 0.4716 0.180 Uiso 1 1 calc R . . C18 C 0.4243(6) 0.1704(3) 0.5964(4) 0.093(2) Uani 1 1 d . . . H18A H 0.4198 0.1289 0.5482 0.139 Uiso 1 1 calc R . . H18B H 0.5010 0.1665 0.6633 0.139 Uiso 1 1 calc R . . H18C H 0.4311 0.2135 0.5547 0.139 Uiso 1 1 calc R . . C19 C 0.1747(6) 0.3787(3) 0.9046(5) 0.096(2) Uani 1 1 d . . . H19A H 0.1157 0.3911 0.9476 0.144 Uiso 1 1 calc R . . H19B H 0.1332 0.3905 0.8251 0.144 Uiso 1 1 calc R . . H19C H 0.2562 0.4055 0.9336 0.144 Uiso 1 1 calc R . . C20 C 0.0889(6) 0.0396(4) 0.6733(6) 0.119(3) Uani 1 1 d . . . H20A H 0.0375 0.0714 0.7063 0.143 Uiso 1 1 calc R . . H20B H 0.0526 0.0442 0.5905 0.143 Uiso 1 1 calc R . . C21 C 0.0646(7) -0.0324(4) 0.7019(6) 0.140(3) Uani 1 1 d . . . H21A H 0.1240 -0.0648 0.6805 0.209 Uiso 1 1 calc R . . H21B H -0.0259 -0.0454 0.6613 0.209 Uiso 1 1 calc R . . H21C H 0.0792 -0.0358 0.7830 0.209 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0479(4) 0.0571(4) 0.0761(5) -0.0188(3) 0.0061(3) -0.0015(3) Cl1 0.0455(9) 0.1022(13) 0.0915(11) -0.0042(9) 0.0097(8) -0.0014(8) Cl2 0.0834(11) 0.0646(10) 0.0800(10) -0.0172(8) 0.0381(9) -0.0029(8) O1 0.041(2) 0.047(2) 0.075(2) -0.0185(18) 0.0096(19) -0.0049(16) O2 0.094(3) 0.053(3) 0.082(3) 0.017(2) 0.032(2) 0.030(2) N1 0.035(2) 0.040(2) 0.054(3) 0.004(2) 0.015(2) 0.0046(18) N2 0.078(4) 0.057(3) 0.052(3) -0.004(2) 0.004(3) 0.010(3) C1 0.053(4) 0.049(4) 0.067(4) -0.002(3) 0.027(3) 0.010(3) C2 0.091(5) 0.053(4) 0.094(5) -0.007(4) 0.040(4) 0.014(3) C3 0.128(6) 0.072(5) 0.077(5) -0.018(4) 0.028(5) 0.021(4) C4 0.143(6) 0.100(6) 0.062(4) 0.004(4) 0.047(4) 0.029(5) C5 0.098(5) 0.046(4) 0.068(4) 0.007(3) 0.037(4) 0.015(3) C6 0.043(3) 0.048(3) 0.060(4) 0.000(3) 0.024(3) 0.003(2) C7 0.044(3) 0.043(3) 0.074(4) 0.000(3) 0.018(3) 0.002(2) C8 0.046(3) 0.048(3) 0.048(3) -0.001(2) 0.011(3) 0.000(2) C9 0.069(4) 0.051(3) 0.054(3) 0.011(3) 0.010(3) 0.017(3) C10 0.048(3) 0.044(3) 0.054(3) 0.008(2) 0.014(3) 0.011(2) C11 0.040(3) 0.037(3) 0.061(3) 0.010(3) 0.021(3) 0.007(2) C12 0.051(3) 0.039(3) 0.054(3) 0.004(2) 0.015(3) 0.003(2) C13 0.039(3) 0.048(3) 0.065(4) 0.009(3) 0.010(3) 0.006(3) C14 0.046(4) 0.050(3) 0.074(4) 0.009(3) 0.025(3) 0.004(3) C15 0.055(4) 0.038(3) 0.049(3) 0.002(2) 0.018(3) 0.005(2) C16 0.042(3) 0.032(3) 0.064(4) 0.004(3) 0.011(3) 0.002(2) C17 0.144(6) 0.096(5) 0.069(4) 0.004(4) -0.040(4) 0.029(5) C18 0.132(6) 0.088(5) 0.065(4) 0.008(3) 0.038(4) 0.013(4) C19 0.106(5) 0.064(4) 0.122(5) 0.027(4) 0.041(4) 0.033(4) C20 0.067(5) 0.092(6) 0.182(7) -0.028(5) 0.013(5) -0.004(4) C21 0.089(6) 0.171(9) 0.177(8) 0.001(7) 0.069(5) -0.030(6) _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 Zn O1 1.936(3) . ? Zn C20 1.950(6) . ? Zn N1 2.156(3) . ? Zn N2 2.170(4) . ? Cl1 C13 1.743(5) . ? Cl2 C15 1.737(5) . ? O1 C16 1.295(5) . ? O2 C1 1.364(5) . ? O2 C19 1.425(5) . ? N1 C8 1.473(5) . ? N1 C7 1.481(5) . ? N1 C10 1.486(5) . ? N2 C18 1.466(6) . ? N2 C9 1.482(5) . ? N2 C17 1.487(6) . ? C1 C2 1.384(6) . ? C1 C6 1.388(6) . ? C2 C3 1.370(7) . ? C2 H2 0.9300 . ? C3 C4 1.363(7) . ? C3 H3 0.9300 . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 C6 1.388(6) . ? C5 H5 0.9300 . ? C6 C7 1.513(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.514(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.497(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.393(6) . ? C11 C16 1.415(6) . ? C12 C13 1.364(6) . ? C12 H12 0.9300 . ? C13 C14 1.360(6) . ? C14 C15 1.373(6) . ? C14 H14 0.9300 . ? C15 C16 1.419(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.420(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 Zn C20 127.3(2) . . ? O1 Zn N1 94.01(13) . . ? C20 Zn N1 121.5(2) . . ? O1 Zn N2 103.80(16) . . ? C20 Zn N2 116.5(3) . . ? N1 Zn N2 83.88(15) . . ? C16 O1 Zn 125.1(3) . . ? C1 O2 C19 118.8(4) . . ? C8 N1 C7 113.1(3) . . ? C8 N1 C10 112.1(3) . . ? C7 N1 C10 110.4(3) . . ? C8 N1 Zn 106.3(3) . . ? C7 N1 Zn 107.0(3) . . ? C10 N1 Zn 107.6(3) . . ? C18 N2 C9 110.5(4) . . ? C18 N2 C17 108.9(5) . . ? C9 N2 C17 110.2(4) . . ? C18 N2 Zn 113.0(3) . . ? C9 N2 Zn 103.7(3) . . ? C17 N2 Zn 110.4(3) . . ? O2 C1 C2 123.8(5) . . ? O2 C1 C6 115.6(5) . . ? C2 C1 C6 120.6(5) . . ? C3 C2 C1 119.4(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 121.5(6) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 121.9(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 117.7(5) . . ? C1 C6 C7 122.0(5) . . ? C5 C6 C7 120.2(5) . . ? N1 C7 C6 117.0(4) . . ? N1 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? N1 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 111.0(4) . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C8 111.0(4) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N1 C10 C11 115.1(4) . . ? N1 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N1 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C16 120.5(4) . . ? C12 C11 C10 119.5(4) . . ? C16 C11 C10 120.0(4) . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.4(5) . . ? C14 C13 Cl1 119.4(4) . . ? C12 C13 Cl1 120.1(4) . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 123.1(5) . . ? C14 C15 Cl2 119.6(4) . . ? C16 C15 Cl2 117.4(4) . . ? O1 C16 C11 123.6(5) . . ? O1 C16 C15 121.2(5) . . ? C11 C16 C15 115.2(4) . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C19 H19A 109.5 . . ? O2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 Zn 119.9(5) . . ? C21 C20 H20A 107.4 . . ? Zn C20 H20A 107.4 . . ? C21 C20 H20B 107.4 . . ? Zn C20 H20B 107.4 . . ? H20A C20 H20B 106.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 C20 Zn O1 C16 -154.9(4) . . . . ? N1 Zn O1 C16 -19.4(4) . . . . ? N2 Zn O1 C16 65.2(4) . . . . ? O1 Zn N1 C8 93.9(3) . . . . ? C20 Zn N1 C8 -127.0(3) . . . . ? N2 Zn N1 C8 -9.5(3) . . . . ? O1 Zn N1 C7 -145.0(3) . . . . ? C20 Zn N1 C7 -5.9(4) . . . . ? N2 Zn N1 C7 111.6(3) . . . . ? O1 Zn N1 C10 -26.3(3) . . . . ? C20 Zn N1 C10 112.8(4) . . . . ? N2 Zn N1 C10 -129.8(3) . . . . ? O1 Zn N2 C18 8.7(4) . . . . ? C20 Zn N2 C18 -136.4(4) . . . . ? N1 Zn N2 C18 101.3(3) . . . . ? O1 Zn N2 C9 -111.0(3) . . . . ? C20 Zn N2 C9 103.9(4) . . . . ? N1 Zn N2 C9 -18.4(3) . . . . ? O1 Zn N2 C17 130.9(4) . . . . ? C20 Zn N2 C17 -14.1(5) . . . . ? N1 Zn N2 C17 -136.4(4) . . . . ? C19 O2 C1 C2 -2.9(8) . . . . ? C19 O2 C1 C6 176.5(4) . . . . ? O2 C1 C2 C3 178.0(5) . . . . ? C6 C1 C2 C3 -1.3(8) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C3 C4 C5 C6 0.2(9) . . . . ? O2 C1 C6 C5 -177.0(4) . . . . ? C2 C1 C6 C5 2.4(7) . . . . ? O2 C1 C6 C7 1.5(7) . . . . ? C2 C1 C6 C7 -179.1(5) . . . . ? C4 C5 C6 C1 -1.9(8) . . . . ? C4 C5 C6 C7 179.6(5) . . . . ? C8 N1 C7 C6 -62.2(5) . . . . ? C10 N1 C7 C6 64.3(5) . . . . ? Zn N1 C7 C6 -178.9(3) . . . . ? C1 C6 C7 N1 92.1(5) . . . . ? C5 C6 C7 N1 -89.5(6) . . . . ? C7 N1 C8 C9 -80.7(4) . . . . ? C10 N1 C8 C9 153.7(4) . . . . ? Zn N1 C8 C9 36.4(4) . . . . ? C18 N2 C9 C8 -77.5(5) . . . . ? C17 N2 C9 C8 162.1(4) . . . . ? Zn N2 C9 C8 43.9(5) . . . . ? N1 C8 C9 N2 -57.1(5) . . . . ? C8 N1 C10 C11 -55.0(5) . . . . ? C7 N1 C10 C11 177.9(4) . . . . ? Zn N1 C10 C11 61.4(4) . . . . ? N1 C10 C11 C12 125.0(4) . . . . ? N1 C10 C11 C16 -55.3(6) . . . . ? C16 C11 C12 C13 -0.3(7) . . . . ? C10 C11 C12 C13 179.4(4) . . . . ? C11 C12 C13 C14 0.7(7) . . . . ? C11 C12 C13 Cl1 177.2(3) . . . . ? C12 C13 C14 C15 -0.1(7) . . . . ? Cl1 C13 C14 C15 -176.6(3) . . . . ? C13 C14 C15 C16 -0.9(7) . . . . ? C13 C14 C15 Cl2 177.5(4) . . . . ? Zn O1 C16 C11 36.6(6) . . . . ? Zn O1 C16 C15 -144.0(3) . . . . ? C12 C11 C16 O1 178.9(4) . . . . ? C10 C11 C16 O1 -0.8(7) . . . . ? C12 C11 C16 C15 -0.6(6) . . . . ? C10 C11 C16 C15 179.7(4) . . . . ? C14 C15 C16 O1 -178.3(4) . . . . ? Cl2 C15 C16 O1 3.3(6) . . . . ? C14 C15 C16 C11 1.2(7) . . . . ? Cl2 C15 C16 C11 -177.2(3) . . . . ? O1 Zn C20 C21 27.7(8) . . . . ? N1 Zn C20 C21 -97.0(6) . . . . ? N2 Zn C20 C21 163.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.323 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.084 # End ======================================================================= data_9 _database_code_depnum_ccdc_archive 'CCDC 772265' #TrackingRef '- cd28470-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H55 N3 O Zn' _chemical_formula_weight 671.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2877(11) _cell_length_b 13.4436(18) _cell_length_c 18.389(2) _cell_angle_alpha 110.4870(10) _cell_angle_beta 90.143(2) _cell_angle_gamma 100.628(2) _cell_volume 1881.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3260 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.02 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8471 _exptl_absorpt_correction_T_max 0.8749 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9813 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6535 _reflns_number_gt 5126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick,1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0409P)^2^+0.7938P] 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_extinction_coef ? _refine_ls_number_reflns 6535 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.27666(4) 0.84127(3) 0.112216(17) 0.03890(11) Uani 1 1 d . . . C1 C 0.2990(5) 0.8409(3) 0.00572(16) 0.0614(9) Uani 1 1 d . . . H1A H 0.2048 0.7920 -0.0274 0.074 Uiso 1 1 calc R . . H1B H 0.2981 0.9130 0.0059 0.074 Uiso 1 1 calc R . . C2 C 0.4541(7) 0.8069(5) -0.0281(3) 0.127(2) Uani 1 1 d . . . H2A H 0.5481 0.8594 0.0010 0.191 Uiso 1 1 calc R . . H2B H 0.4537 0.8020 -0.0815 0.191 Uiso 1 1 calc R . . H2C H 0.4594 0.7375 -0.0254 0.191 Uiso 1 1 calc R . . C3 C 0.2115(3) 0.9791(2) 0.26739(15) 0.0426(7) Uani 1 1 d . . . H3A H 0.2160 1.0503 0.3066 0.051 Uiso 1 1 calc R . . H3B H 0.2265 0.9299 0.2938 0.051 Uiso 1 1 calc R . . C4 C 0.0452(4) 0.9404(2) 0.22223(16) 0.0456(7) Uani 1 1 d . . . H4A H -0.0399 0.9339 0.2573 0.055 Uiso 1 1 calc R . . H4B H 0.0255 0.9936 0.2005 0.055 Uiso 1 1 calc R . . C5 C 0.0035(4) 0.7453(2) 0.18917(19) 0.0570(8) Uani 1 1 d . . . H5A H -0.0981 0.7462 0.2142 0.085 Uiso 1 1 calc R . . H5B H 0.0919 0.7542 0.2261 0.085 Uiso 1 1 calc R . . H5C H -0.0042 0.6774 0.1470 0.085 Uiso 1 1 calc R . . C6 C -0.1003(4) 0.8187(3) 0.10081(19) 0.0652(9) Uani 1 1 d . . . H6A H -0.1089 0.7493 0.0602 0.098 Uiso 1 1 calc R . . H6B H -0.0781 0.8746 0.0789 0.098 Uiso 1 1 calc R . . H6C H -0.2018 0.8220 0.1258 0.098 Uiso 1 1 calc R . . C7 C 0.3575(4) 1.0768(2) 0.18705(15) 0.0402(6) Uani 1 1 d . . . H7A H 0.2653 1.0606 0.1494 0.048 Uiso 1 1 calc R . . H7B H 0.4571 1.0805 0.1597 0.048 Uiso 1 1 calc R . . C8 C 0.3602(4) 1.1880(2) 0.24776(15) 0.0407(7) Uani 1 1 d . . . C9 C 0.5014(4) 1.2453(2) 0.29464(17) 0.0512(8) Uani 1 1 d . . . H9 H 0.5955 1.2155 0.2862 0.061 Uiso 1 1 calc R . . C10 C 0.5101(5) 1.3451(3) 0.35378(18) 0.0633(10) Uani 1 1 d . . . C11 C 0.3687(6) 1.3865(3) 0.3644(2) 0.0739(12) Uani 1 1 d . . . H11 H 0.3684 1.4517 0.4048 0.089 Uiso 1 1 calc R . . C12 C 0.2283(5) 1.3343(3) 0.3170(2) 0.0707(11) Uani 1 1 d . . . H12 H 0.1355 1.3655 0.3252 0.085 Uiso 1 1 calc R . . C13 C 0.2215(4) 1.2351(2) 0.2565(2) 0.0539(8) Uani 1 1 d . . . C14 C 0.1039(6) 1.1985(3) 0.1265(3) 0.0974(14) Uani 1 1 d . . . H14A H 0.0952 1.2714 0.1332 0.146 Uiso 1 1 calc R . . H14B H 0.0207 1.1486 0.0880 0.146 Uiso 1 1 calc R . . H14C H 0.2107 1.1867 0.1098 0.146 Uiso 1 1 calc R . . C15 C -0.0768(5) 1.2007(4) 0.2294(4) 0.130(2) Uani 1 1 d . . . H15A H -0.0859 1.1921 0.2790 0.196 Uiso 1 1 calc R . . H15B H -0.1630 1.1498 0.1932 0.196 Uiso 1 1 calc R . . H15C H -0.0865 1.2731 0.2350 0.196 Uiso 1 1 calc R . . C16 C 0.6684(6) 1.4058(3) 0.4020(2) 0.1076(16) Uani 1 1 d . . . H16A H 0.7342 1.4466 0.3752 0.161 Uiso 1 1 calc R . . H16B H 0.7277 1.3553 0.4103 0.161 Uiso 1 1 calc R . . H16C H 0.6442 1.4543 0.4513 0.161 Uiso 1 1 calc R . . C17 C 0.5056(4) 0.9805(2) 0.24945(16) 0.0433(7) Uani 1 1 d . . . H17A H 0.5381 1.0455 0.2952 0.052 Uiso 1 1 calc R . . H17B H 0.5871 0.9827 0.2120 0.052 Uiso 1 1 calc R . . C18 C 0.5114(3) 0.8842(2) 0.27261(14) 0.0370(6) Uani 1 1 d . . . C19 C 0.5836(3) 0.9036(2) 0.34631(15) 0.0398(6) Uani 1 1 d . . . H19 H 0.6133 0.9747 0.3807 0.048 Uiso 1 1 calc R . . C20 C 0.6124(3) 0.8215(2) 0.37003(14) 0.0358(6) Uani 1 1 d . . . C21 C 0.5693(3) 0.7162(2) 0.31570(14) 0.0353(6) Uani 1 1 d . . . H21 H 0.5901 0.6597 0.3300 0.042 Uiso 1 1 calc R . . C22 C 0.4973(3) 0.6912(2) 0.24160(14) 0.0317(6) Uani 1 1 d . . . C23 C 0.4625(3) 0.7768(2) 0.21970(13) 0.0343(6) Uani 1 1 d . . . C24 C 0.4580(3) 0.5741(2) 0.18247(14) 0.0337(6) Uani 1 1 d . . . C25 C 0.5523(3) 0.5682(2) 0.10971(15) 0.0426(7) Uani 1 1 d . . . H25A H 0.5342 0.4944 0.0743 0.064 Uiso 1 1 calc R . . H25B H 0.6678 0.5942 0.1246 0.064 Uiso 1 1 calc R . . H25C H 0.5138 0.6122 0.0848 0.064 Uiso 1 1 calc R . . C26 C 0.5155(4) 0.4942(2) 0.21500(16) 0.0435(7) Uani 1 1 d . . . H26A H 0.4598 0.4951 0.2609 0.065 Uiso 1 1 calc R . . H26B H 0.6321 0.5152 0.2278 0.065 Uiso 1 1 calc R . . H26C H 0.4902 0.4224 0.1765 0.065 Uiso 1 1 calc R . . C27 C 0.2717(3) 0.53481(19) 0.16389(14) 0.0338(6) Uani 1 1 d . . . C28 C 0.1967(4) 0.4884(2) 0.08933(16) 0.0447(7) Uani 1 1 d . . . H28 H 0.2598 0.4852 0.0471 0.054 Uiso 1 1 calc R . . C29 C 0.0288(4) 0.4466(2) 0.07628(18) 0.0529(8) Uani 1 1 d . . . H29 H -0.0186 0.4146 0.0255 0.064 Uiso 1 1 calc R . . C30 C -0.0679(4) 0.4520(2) 0.1373(2) 0.0562(8) Uani 1 1 d . . . H30 H -0.1804 0.4240 0.1284 0.067 Uiso 1 1 calc R . . C31 C 0.0040(4) 0.4995(2) 0.21209(19) 0.0519(8) Uani 1 1 d . . . H31 H -0.0604 0.5041 0.2541 0.062 Uiso 1 1 calc R . . C32 C 0.1712(3) 0.5404(2) 0.22501(16) 0.0430(7) Uani 1 1 d . . . H32 H 0.2177 0.5726 0.2759 0.052 Uiso 1 1 calc R . . C33 C 0.6829(3) 0.8403(2) 0.45225(14) 0.0402(6) Uani 1 1 d . . . C34 C 0.7495(4) 0.9606(2) 0.49894(16) 0.0531(8) Uani 1 1 d . . . H34A H 0.8289 0.9900 0.4702 0.080 Uiso 1 1 calc R . . H34B H 0.8008 0.9681 0.5479 0.080 Uiso 1 1 calc R . . H34C H 0.6604 0.9991 0.5079 0.080 Uiso 1 1 calc R . . C35 C 0.5420(4) 0.7994(3) 0.49552(16) 0.0580(9) Uani 1 1 d . . . H35A H 0.4519 0.8350 0.4949 0.087 Uiso 1 1 calc R . . H35B H 0.5804 0.8152 0.5484 0.087 Uiso 1 1 calc R . . H35C H 0.5057 0.7226 0.4702 0.087 Uiso 1 1 calc R . . C36 C 0.8270(3) 0.7815(2) 0.44742(14) 0.0395(6) Uani 1 1 d . . . C37 C 0.9552(4) 0.7969(2) 0.40210(16) 0.0488(7) Uani 1 1 d . . . H37 H 0.9498 0.8405 0.3728 0.059 Uiso 1 1 calc R . . C38 C 1.0907(4) 0.7501(3) 0.39881(18) 0.0604(9) Uani 1 1 d . . . H38 H 1.1757 0.7631 0.3683 0.072 Uiso 1 1 calc R . . C39 C 1.1001(5) 0.6842(3) 0.4406(2) 0.0698(10) Uani 1 1 d . . . H39 H 1.1907 0.6517 0.4384 0.084 Uiso 1 1 calc R . . C40 C 0.9752(5) 0.6671(3) 0.4853(2) 0.0802(12) Uani 1 1 d . . . H40 H 0.9806 0.6222 0.5135 0.096 Uiso 1 1 calc R . . C41 C 0.8402(4) 0.7155(3) 0.4893(2) 0.0641(9) Uani 1 1 d . . . H41 H 0.7569 0.7033 0.5208 0.077 Uiso 1 1 calc R . . N1 N 0.3447(3) 0.98435(16) 0.21534(12) 0.0358(5) Uani 1 1 d . . . N2 N 0.0353(3) 0.83474(18) 0.15872(13) 0.0433(6) Uani 1 1 d . . . N3 N 0.0813(4) 1.1814(2) 0.2010(2) 0.0752(9) Uani 1 1 d . . . O1 O 0.3902(2) 0.75476(14) 0.15004(9) 0.0429(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0455(2) 0.03807(19) 0.03306(17) 0.01199(13) -0.00322(13) 0.00944(14) C1 0.090(3) 0.054(2) 0.0419(17) 0.0202(15) -0.0034(17) 0.0112(18) C2 0.139(5) 0.170(5) 0.096(3) 0.066(4) 0.061(3) 0.049(4) C3 0.0519(19) 0.0369(16) 0.0385(14) 0.0125(12) 0.0058(13) 0.0095(13) C4 0.0468(18) 0.0394(16) 0.0544(17) 0.0195(14) 0.0078(14) 0.0119(14) C5 0.059(2) 0.0417(18) 0.070(2) 0.0229(16) 0.0080(17) 0.0038(15) C6 0.051(2) 0.070(2) 0.069(2) 0.0179(18) -0.0108(17) 0.0124(17) C7 0.0448(17) 0.0375(15) 0.0424(15) 0.0194(13) -0.0006(13) 0.0082(13) C8 0.0474(18) 0.0338(15) 0.0460(16) 0.0206(13) 0.0049(13) 0.0079(13) C9 0.063(2) 0.0378(17) 0.0548(18) 0.0197(15) -0.0035(16) 0.0085(15) C10 0.101(3) 0.0369(18) 0.0509(18) 0.0188(15) -0.0082(19) 0.0041(19) C11 0.133(4) 0.044(2) 0.051(2) 0.0198(17) 0.026(2) 0.025(2) C12 0.087(3) 0.052(2) 0.092(3) 0.039(2) 0.041(2) 0.034(2) C13 0.054(2) 0.0407(18) 0.078(2) 0.0322(17) 0.0170(17) 0.0148(15) C14 0.097(3) 0.091(3) 0.125(4) 0.065(3) -0.031(3) 0.017(3) C15 0.059(3) 0.095(4) 0.256(7) 0.079(4) 0.031(4) 0.028(3) C16 0.148(4) 0.062(3) 0.086(3) 0.012(2) -0.050(3) -0.016(3) C17 0.0468(18) 0.0346(15) 0.0462(16) 0.0138(13) -0.0085(13) 0.0037(13) C18 0.0417(16) 0.0304(14) 0.0367(14) 0.0103(11) -0.0068(12) 0.0052(12) C19 0.0431(17) 0.0315(15) 0.0376(14) 0.0052(12) -0.0060(12) 0.0039(12) C20 0.0337(15) 0.0392(15) 0.0325(13) 0.0105(12) -0.0058(11) 0.0070(12) C21 0.0361(15) 0.0355(15) 0.0376(14) 0.0171(12) -0.0021(12) 0.0071(12) C22 0.0288(14) 0.0327(14) 0.0326(13) 0.0108(11) 0.0001(11) 0.0057(11) C23 0.0343(15) 0.0367(15) 0.0314(13) 0.0119(11) -0.0017(11) 0.0063(12) C24 0.0341(15) 0.0333(14) 0.0339(13) 0.0106(11) 0.0009(11) 0.0098(12) C25 0.0421(17) 0.0418(16) 0.0402(15) 0.0102(13) 0.0074(13) 0.0079(13) C26 0.0467(18) 0.0372(16) 0.0492(16) 0.0160(13) 0.0004(13) 0.0135(13) C27 0.0357(15) 0.0267(13) 0.0397(14) 0.0111(11) 0.0014(12) 0.0091(11) C28 0.0442(18) 0.0424(17) 0.0422(15) 0.0099(13) -0.0023(13) 0.0061(14) C29 0.050(2) 0.0413(17) 0.0564(18) 0.0056(15) -0.0157(16) 0.0055(14) C30 0.0351(18) 0.0385(17) 0.091(3) 0.0185(17) -0.0048(17) 0.0061(14) C31 0.0415(19) 0.0465(18) 0.071(2) 0.0238(16) 0.0166(16) 0.0110(15) C32 0.0421(18) 0.0408(16) 0.0458(16) 0.0143(13) 0.0044(13) 0.0100(13) C33 0.0398(16) 0.0477(17) 0.0311(13) 0.0125(12) -0.0026(12) 0.0069(13) C34 0.058(2) 0.0539(19) 0.0374(15) 0.0028(14) -0.0125(14) 0.0138(16) C35 0.051(2) 0.084(2) 0.0436(17) 0.0282(17) 0.0034(14) 0.0136(17) C36 0.0393(16) 0.0424(16) 0.0314(13) 0.0090(12) -0.0108(12) 0.0034(13) C37 0.053(2) 0.0539(19) 0.0417(16) 0.0168(14) 0.0035(14) 0.0161(15) C38 0.055(2) 0.068(2) 0.0531(19) 0.0121(17) 0.0046(16) 0.0200(18) C39 0.052(2) 0.070(2) 0.086(3) 0.021(2) -0.016(2) 0.0211(19) C40 0.065(3) 0.090(3) 0.110(3) 0.065(3) -0.013(2) 0.017(2) C41 0.048(2) 0.085(3) 0.077(2) 0.050(2) -0.0009(17) 0.0120(18) N1 0.0408(13) 0.0317(12) 0.0369(11) 0.0143(10) -0.0006(10) 0.0082(10) N2 0.0428(14) 0.0373(13) 0.0485(13) 0.0143(11) -0.0021(11) 0.0067(11) N3 0.0474(18) 0.0577(18) 0.132(3) 0.0465(19) 0.0053(18) 0.0134(14) O1 0.0581(13) 0.0361(10) 0.0324(9) 0.0085(8) -0.0117(9) 0.0122(9) _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 1.9205(17) . ? Zn1 C1 1.966(3) . ? Zn1 N1 2.158(2) . ? Zn1 N2 2.176(2) . ? C1 C2 1.507(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N1 1.471(3) . ? C3 C4 1.512(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.478(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N2 1.478(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.479(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N1 1.494(3) . ? C7 C8 1.516(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.380(4) . ? C8 C13 1.395(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C10 C11 1.374(5) . ? C10 C16 1.506(5) . ? C11 C12 1.368(5) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 H12 0.9300 . ? C13 N3 1.443(4) . ? C14 N3 1.472(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N3 1.446(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N1 1.489(3) . ? C17 C18 1.506(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.398(3) . ? C18 C23 1.412(3) . ? C19 C20 1.377(4) . ? C19 H19 0.9300 . ? C20 C21 1.397(3) . ? C20 C33 1.538(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9300 . ? C22 C23 1.420(3) . ? C22 C24 1.542(3) . ? C23 O1 1.324(3) . ? C24 C27 1.533(4) . ? C24 C25 1.537(3) . ? C24 C26 1.541(3) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.382(4) . ? C27 C32 1.390(4) . ? C28 C29 1.387(4) . ? C28 H28 0.9300 . ? C29 C30 1.370(4) . ? C29 H29 0.9300 . ? C30 C31 1.376(4) . ? C30 H30 0.9300 . ? C31 C32 1.380(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.534(4) . ? C33 C36 1.535(4) . ? C33 C35 1.541(4) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 1.382(4) . ? C36 C37 1.383(4) . ? C37 C38 1.377(4) . ? C37 H37 0.9300 . ? C38 C39 1.372(5) . ? C38 H38 0.9300 . ? C39 C40 1.359(5) . ? C39 H39 0.9300 . ? C40 C41 1.385(5) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? 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 C1 120.79(11) . . ? O1 Zn1 N1 94.18(7) . . ? C1 Zn1 N1 123.81(11) . . ? O1 Zn1 N2 107.09(8) . . ? C1 Zn1 N2 119.60(12) . . ? N1 Zn1 N2 83.46(8) . . ? C2 C1 Zn1 113.2(3) . . ? C2 C1 H1A 108.9 . . ? Zn1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? Zn1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 110.9(2) . . ? N1 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 111.6(2) . . ? N2 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 117.1(2) . . ? N1 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? N1 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? C9 C8 C13 118.7(3) . . ? C9 C8 C7 120.4(3) . . ? C13 C8 C7 120.9(3) . . ? C8 C9 C10 123.4(3) . . ? C8 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C11 C10 C9 116.7(3) . . ? C11 C10 C16 121.9(4) . . ? C9 C10 C16 121.3(4) . . ? C12 C11 C10 121.7(3) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 118.1(3) . . ? C8 C13 N3 118.6(3) . . ? C12 C13 N3 123.3(3) . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 116.7(2) . . ? N1 C17 H17A 108.1 . . ? C18 C17 H17A 108.1 . . ? N1 C17 H17B 108.1 . . ? C18 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C19 C18 C23 119.9(2) . . ? C19 C18 C17 117.8(2) . . ? C23 C18 C17 122.0(2) . . ? C20 C19 C18 122.6(2) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 116.6(2) . . ? C19 C20 C33 123.6(2) . . ? C21 C20 C33 119.8(2) . . ? C22 C21 C20 123.8(2) . . ? C22 C21 H21 118.1 . . ? C20 C21 H21 118.1 . . ? C21 C22 C23 118.5(2) . . ? C21 C22 C24 121.9(2) . . ? C23 C22 C24 119.5(2) . . ? O1 C23 C18 121.8(2) . . ? O1 C23 C22 119.7(2) . . ? C18 C23 C22 118.5(2) . . ? C27 C24 C25 112.9(2) . . ? C27 C24 C26 105.9(2) . . ? C25 C24 C26 106.4(2) . . ? C27 C24 C22 110.60(19) . . ? C25 C24 C22 109.3(2) . . ? C26 C24 C22 111.8(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 117.2(3) . . ? C28 C27 C24 124.1(2) . . ? C32 C27 C24 118.7(2) . . ? C27 C28 C29 121.2(3) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.0(3) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 121.7(3) . . ? C31 C32 H32 119.2 . . ? C27 C32 H32 119.2 . . ? C34 C33 C36 106.9(2) . . ? C34 C33 C20 112.2(2) . . ? C36 C33 C20 110.2(2) . . ? C34 C33 C35 108.0(2) . . ? C36 C33 C35 111.8(2) . . ? C20 C33 C35 107.7(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 116.6(3) . . ? C41 C36 C33 123.1(3) . . ? C37 C36 C33 120.2(2) . . ? C38 C37 C36 122.3(3) . . ? C38 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? C39 C38 C37 119.8(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.1(3) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 121.0(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C36 C41 C40 121.1(3) . . ? C36 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C3 N1 C17 112.2(2) . . ? C3 N1 C7 113.6(2) . . ? C17 N1 C7 112.0(2) . . ? C3 N1 Zn1 105.75(15) . . ? C17 N1 Zn1 107.73(15) . . ? C7 N1 Zn1 104.80(14) . . ? C5 N2 C4 110.8(2) . . ? C5 N2 C6 108.8(2) . . ? C4 N2 C6 109.3(2) . . ? C5 N2 Zn1 108.97(17) . . ? C4 N2 Zn1 105.36(16) . . ? C6 N2 Zn1 113.57(19) . . ? C13 N3 C15 115.7(4) . . ? C13 N3 C14 112.7(3) . . ? C15 N3 C14 111.5(4) . . ? C23 O1 Zn1 129.95(16) . . ? 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 O1 Zn1 C1 C2 -22.8(4) . . . . ? N1 Zn1 C1 C2 97.3(3) . . . . ? N2 Zn1 C1 C2 -159.9(3) . . . . ? N1 C3 C4 N2 55.9(3) . . . . ? N1 C7 C8 C9 76.9(3) . . . . ? N1 C7 C8 C13 -104.2(3) . . . . ? C13 C8 C9 C10 4.2(4) . . . . ? C7 C8 C9 C10 -176.9(3) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C8 C9 C10 C16 -178.4(3) . . . . ? C9 C10 C11 C12 -2.7(5) . . . . ? C16 C10 C11 C12 175.6(3) . . . . ? C10 C11 C12 C13 1.3(5) . . . . ? C9 C8 C13 C12 -5.4(4) . . . . ? C7 C8 C13 C12 175.7(3) . . . . ? C9 C8 C13 N3 172.1(3) . . . . ? C7 C8 C13 N3 -6.8(4) . . . . ? C11 C12 C13 C8 2.9(5) . . . . ? C11 C12 C13 N3 -174.6(3) . . . . ? N1 C17 C18 C19 -132.0(3) . . . . ? N1 C17 C18 C23 54.7(4) . . . . ? C23 C18 C19 C20 1.1(4) . . . . ? C17 C18 C19 C20 -172.4(3) . . . . ? C18 C19 C20 C21 1.5(4) . . . . ? C18 C19 C20 C33 -176.5(3) . . . . ? C19 C20 C21 C22 -1.5(4) . . . . ? C33 C20 C21 C22 176.6(2) . . . . ? C20 C21 C22 C23 -1.0(4) . . . . ? C20 C21 C22 C24 177.6(2) . . . . ? C19 C18 C23 O1 178.4(2) . . . . ? C17 C18 C23 O1 -8.4(4) . . . . ? C19 C18 C23 C22 -3.6(4) . . . . ? C17 C18 C23 C22 169.5(2) . . . . ? C21 C22 C23 O1 -178.4(2) . . . . ? C24 C22 C23 O1 3.0(4) . . . . ? C21 C22 C23 C18 3.6(4) . . . . ? C24 C22 C23 C18 -175.1(2) . . . . ? C21 C22 C24 C27 115.1(3) . . . . ? C23 C22 C24 C27 -66.3(3) . . . . ? C21 C22 C24 C25 -120.0(3) . . . . ? C23 C22 C24 C25 58.6(3) . . . . ? C21 C22 C24 C26 -2.6(3) . . . . ? C23 C22 C24 C26 176.0(2) . . . . ? C25 C24 C27 C28 6.3(3) . . . . ? C26 C24 C27 C28 -109.7(3) . . . . ? C22 C24 C27 C28 129.1(3) . . . . ? C25 C24 C27 C32 -177.2(2) . . . . ? C26 C24 C27 C32 66.8(3) . . . . ? C22 C24 C27 C32 -54.5(3) . . . . ? C32 C27 C28 C29 -1.8(4) . . . . ? C24 C27 C28 C29 174.7(2) . . . . ? C27 C28 C29 C30 1.2(4) . . . . ? C28 C29 C30 C31 -0.1(4) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C30 C31 C32 C27 -0.3(4) . . . . ? C28 C27 C32 C31 1.3(4) . . . . ? C24 C27 C32 C31 -175.4(2) . . . . ? C19 C20 C33 C34 -11.6(4) . . . . ? C21 C20 C33 C34 170.4(2) . . . . ? C19 C20 C33 C36 -130.7(3) . . . . ? C21 C20 C33 C36 51.4(3) . . . . ? C19 C20 C33 C35 107.1(3) . . . . ? C21 C20 C33 C35 -70.9(3) . . . . ? C34 C33 C36 C41 106.7(3) . . . . ? C20 C33 C36 C41 -131.0(3) . . . . ? C35 C33 C36 C41 -11.3(4) . . . . ? C34 C33 C36 C37 -70.4(3) . . . . ? C20 C33 C36 C37 51.8(3) . . . . ? C35 C33 C36 C37 171.5(2) . . . . ? C41 C36 C37 C38 -0.5(4) . . . . ? C33 C36 C37 C38 176.9(3) . . . . ? C36 C37 C38 C39 1.0(5) . . . . ? C37 C38 C39 C40 -0.5(5) . . . . ? C38 C39 C40 C41 -0.4(6) . . . . ? C37 C36 C41 C40 -0.4(5) . . . . ? C33 C36 C41 C40 -177.7(3) . . . . ? C39 C40 C41 C36 0.9(6) . . . . ? C4 C3 N1 C17 -158.2(2) . . . . ? C4 C3 N1 C7 73.4(3) . . . . ? C4 C3 N1 Zn1 -41.0(2) . . . . ? C18 C17 N1 C3 56.7(3) . . . . ? C18 C17 N1 C7 -174.1(2) . . . . ? C18 C17 N1 Zn1 -59.3(3) . . . . ? C8 C7 N1 C3 49.6(3) . . . . ? C8 C7 N1 C17 -78.9(3) . . . . ? C8 C7 N1 Zn1 164.6(2) . . . . ? O1 Zn1 N1 C3 -91.10(16) . . . . ? C1 Zn1 N1 C3 137.08(18) . . . . ? N2 Zn1 N1 C3 15.64(15) . . . . ? O1 Zn1 N1 C17 29.10(17) . . . . ? C1 Zn1 N1 C17 -102.7(2) . . . . ? N2 Zn1 N1 C17 135.84(17) . . . . ? O1 Zn1 N1 C7 148.57(16) . . . . ? C1 Zn1 N1 C7 16.8(2) . . . . ? N2 Zn1 N1 C7 -104.68(16) . . . . ? C3 C4 N2 C5 79.8(3) . . . . ? C3 C4 N2 C6 -160.3(2) . . . . ? C3 C4 N2 Zn1 -37.9(2) . . . . ? O1 Zn1 N2 C5 -14.65(19) . . . . ? C1 Zn1 N2 C5 127.6(2) . . . . ? N1 Zn1 N2 C5 -107.04(18) . . . . ? O1 Zn1 N2 C4 104.26(16) . . . . ? C1 Zn1 N2 C4 -113.52(19) . . . . ? N1 Zn1 N2 C4 11.87(16) . . . . ? O1 Zn1 N2 C6 -136.14(19) . . . . ? C1 Zn1 N2 C6 6.1(2) . . . . ? N1 Zn1 N2 C6 131.5(2) . . . . ? C8 C13 N3 C15 152.4(3) . . . . ? C12 C13 N3 C15 -30.2(5) . . . . ? C8 C13 N3 C14 -77.6(4) . . . . ? C12 C13 N3 C14 99.8(4) . . . . ? C18 C23 O1 Zn1 -20.1(4) . . . . ? C22 C23 O1 Zn1 161.93(18) . . . . ? C1 Zn1 O1 C23 141.7(2) . . . . ? N1 Zn1 O1 C23 7.8(2) . . . . ? N2 Zn1 O1 C23 -76.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.361 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.049 # End ======================================================================= data_10 _database_code_depnum_ccdc_archive 'CCDC 772266' #TrackingRef '- cd28470-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H33 Cl2 N3 O Zn' _chemical_formula_weight 503.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.3448(17) _cell_length_b 9.4596(10) _cell_length_c 16.1050(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.982(2) _cell_angle_gamma 90.00 _cell_volume 2466.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3665 _cell_measurement_theta_min 4.995 _cell_measurement_theta_max 49.296 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.421 _exptl_crystal_size_mid 0.369 _exptl_crystal_size_min 0.210 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7719 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13064 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4831 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0514P)^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_extinction_coef ? _refine_ls_number_reflns 4831 _refine_ls_number_parameters 288 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.11359(2) 0.46719(4) 0.38903(2) 0.04417(15) Uani 1 1 d . A . Cl1 Cl 0.49819(5) 0.70783(10) 0.61041(6) 0.0584(3) Uani 1 1 d . . . Cl2 Cl 0.17473(6) 0.82248(10) 0.59190(6) 0.0631(3) Uani 1 1 d . . . O1 O 0.15902(13) 0.6407(2) 0.44255(14) 0.0503(6) Uani 1 1 d . . . N1 N 0.23213(14) 0.3856(3) 0.36922(14) 0.0341(5) Uani 1 1 d . . . N2 N 0.12385(16) 0.3108(3) 0.48777(15) 0.0474(7) Uani 1 1 d . . . N3 N 0.28042(16) 0.0252(3) 0.31991(15) 0.0420(6) Uani 1 1 d . . . C1 C 0.31934(17) 0.1145(3) 0.26577(17) 0.0369(7) Uani 1 1 d . . . C2 C 0.3843(2) 0.0687(4) 0.22590(19) 0.0474(8) Uani 1 1 d . . . H2 H 0.4040 -0.0229 0.2355 0.057 Uiso 1 1 calc R . . C3 C 0.4206(2) 0.1546(4) 0.1724(2) 0.0508(9) Uani 1 1 d . . . H3 H 0.4647 0.1205 0.1475 0.061 Uiso 1 1 calc R . . C4 C 0.3926(2) 0.2907(3) 0.15510(18) 0.0430(7) Uani 1 1 d . . . C5 C 0.32715(18) 0.3366(3) 0.19496(17) 0.0385(7) Uani 1 1 d . . . H5 H 0.3069 0.4275 0.1839 0.046 Uiso 1 1 calc R . . C6 C 0.29067(17) 0.2532(3) 0.25040(16) 0.0340(6) Uani 1 1 d . . . C7 C 0.21700(17) 0.3121(3) 0.28666(17) 0.0373(7) Uani 1 1 d . . . H7A H 0.1889 0.3779 0.2462 0.045 Uiso 1 1 calc R . . H7B H 0.1792 0.2346 0.2918 0.045 Uiso 1 1 calc R . . C8 C 0.26013(18) 0.2888(3) 0.44008(17) 0.0393(7) Uani 1 1 d . . . H8A H 0.2877 0.3427 0.4871 0.047 Uiso 1 1 calc R . . H8B H 0.2993 0.2213 0.4232 0.047 Uiso 1 1 calc R . . C9 C 0.1876(2) 0.2113(4) 0.4664(2) 0.0493(8) Uani 1 1 d . . . H9A H 0.1637 0.1500 0.4212 0.059 Uiso 1 1 calc R . . H9B H 0.2064 0.1526 0.5147 0.059 Uiso 1 1 calc R . . C10 C 0.28803(18) 0.5085(3) 0.36638(19) 0.0392(7) Uani 1 1 d . . . H10A H 0.2645 0.5715 0.3218 0.047 Uiso 1 1 calc R . . H10B H 0.3407 0.4752 0.3527 0.047 Uiso 1 1 calc R . . C11 C 0.30291(18) 0.5906(3) 0.44722(18) 0.0376(7) Uani 1 1 d . . . C12 C 0.38232(19) 0.6085(3) 0.48728(19) 0.0400(7) Uani 1 1 d . . . H12 H 0.4261 0.5662 0.4655 0.048 Uiso 1 1 calc R . . C13 C 0.39770(19) 0.6881(3) 0.55906(19) 0.0428(7) Uani 1 1 d . . . C14 C 0.3337(2) 0.7541(3) 0.59140(19) 0.0439(8) Uani 1 1 d . . . H14 H 0.3439 0.8098 0.6393 0.053 Uiso 1 1 calc R . . C15 C 0.2553(2) 0.7360(3) 0.55187(19) 0.0422(7) Uani 1 1 d . . . C16 C 0.23437(19) 0.6547(3) 0.47817(19) 0.0408(7) Uani 1 1 d . . . C17 C 0.0437(2) 0.2355(5) 0.4878(3) 0.0811(13) Uani 1 1 d . . . H17A H 0.0506 0.1608 0.5286 0.122 Uiso 1 1 calc R . . H17B H 0.0263 0.1964 0.4333 0.122 Uiso 1 1 calc R . . H17C H 0.0028 0.3009 0.5017 0.122 Uiso 1 1 calc R . . C18 C 0.1492(2) 0.3737(5) 0.5710(2) 0.0660(11) Uani 1 1 d . . . H18A H 0.1504 0.3017 0.6132 0.099 Uiso 1 1 calc R . . H18B H 0.1104 0.4458 0.5812 0.099 Uiso 1 1 calc R . . H18C H 0.2032 0.4145 0.5730 0.099 Uiso 1 1 calc R . . C19 C 0.2154(2) -0.0618(4) 0.2759(2) 0.0701(11) Uani 1 1 d . . . H19A H 0.1758 -0.0026 0.2427 0.105 Uiso 1 1 calc R . . H19B H 0.1885 -0.1133 0.3158 0.105 Uiso 1 1 calc R . . H19C H 0.2388 -0.1271 0.2401 0.105 Uiso 1 1 calc R . . C20 C 0.0165(2) 0.4661(6) 0.3032(2) 0.0798(13) Uani 1 1 d D . . H20A H -0.0151 0.3834 0.3148 0.096 Uiso 0.55(3) 1 calc PR A 1 H20B H -0.0161 0.5473 0.3152 0.096 Uiso 0.55(3) 1 calc PR A 1 H20C H -0.0304 0.4942 0.3290 0.096 Uiso 0.45(3) 1 d PR A 2 H20D H 0.0079 0.3705 0.2839 0.096 Uiso 0.45(3) 1 d PR A 2 C22 C 0.3386(2) -0.0601(4) 0.3752(2) 0.0646(10) Uani 1 1 d . . . H22A H 0.3572 -0.1378 0.3443 0.097 Uiso 1 1 calc R . . H22B H 0.3120 -0.0959 0.4204 0.097 Uiso 1 1 calc R . . H22C H 0.3851 -0.0031 0.3975 0.097 Uiso 1 1 calc R . . C23 C 0.4308(2) 0.3847(4) 0.0965(2) 0.0644(10) Uani 1 1 d . . . H23A H 0.4600 0.4601 0.1277 0.097 Uiso 1 1 calc R . . H23B H 0.3883 0.4234 0.0557 0.097 Uiso 1 1 calc R . . H23C H 0.4687 0.3309 0.0686 0.097 Uiso 1 1 calc R . . C21 C 0.0167(9) 0.467(3) 0.2143(7) 0.106(7) Uani 0.55(3) 1 d PD A 1 H21A H -0.0382 0.4852 0.1867 0.173 Uiso 0.55(3) 1 calc PR A 1 H21B H 0.0350 0.3767 0.1967 0.173 Uiso 0.55(3) 1 calc PR A 1 H21C H 0.0533 0.5394 0.1999 0.173 Uiso 0.55(3) 1 calc PR A 1 C21' C 0.0203(14) 0.561(5) 0.236(2) 0.133(17) Uani 0.45(3) 1 d PD A 2 H21D H 0.0726 0.5512 0.2155 0.189 Uiso 0.45(3) 1 calc PR A 2 H21E H 0.0142 0.6562 0.2545 0.189 Uiso 0.45(3) 1 calc PR A 2 H21F H -0.0234 0.5398 0.1911 0.189 Uiso 0.45(3) 1 calc PR A 2 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 Zn 0.0361(2) 0.0578(3) 0.0383(2) -0.00397(17) 0.00384(15) 0.00712(17) Cl1 0.0517(5) 0.0591(6) 0.0618(5) -0.0080(4) -0.0013(4) -0.0084(4) Cl2 0.0629(6) 0.0615(6) 0.0686(6) -0.0179(5) 0.0225(5) 0.0107(5) O1 0.0442(13) 0.0489(14) 0.0570(14) -0.0082(11) 0.0041(11) 0.0107(11) N1 0.0366(13) 0.0355(14) 0.0299(12) -0.0011(10) 0.0033(10) 0.0047(11) N2 0.0453(15) 0.0654(19) 0.0324(14) 0.0001(13) 0.0083(11) -0.0028(13) N3 0.0547(16) 0.0360(14) 0.0357(13) 0.0006(11) 0.0077(12) -0.0026(12) C1 0.0407(16) 0.0401(18) 0.0291(15) -0.0063(13) 0.0021(12) -0.0005(14) C2 0.058(2) 0.0420(19) 0.0429(18) -0.0056(15) 0.0101(15) 0.0085(15) C3 0.053(2) 0.058(2) 0.0442(19) -0.0078(17) 0.0170(16) 0.0072(17) C4 0.0492(18) 0.049(2) 0.0319(16) -0.0063(14) 0.0089(13) -0.0063(15) C5 0.0487(18) 0.0364(17) 0.0302(15) -0.0013(13) 0.0044(13) 0.0014(13) C6 0.0366(15) 0.0381(17) 0.0262(14) -0.0037(12) 0.0007(12) 0.0022(13) C7 0.0388(16) 0.0428(18) 0.0294(15) -0.0005(13) 0.0021(12) 0.0050(13) C8 0.0422(17) 0.0436(18) 0.0310(15) -0.0005(13) 0.0007(13) 0.0039(14) C9 0.059(2) 0.050(2) 0.0382(17) 0.0035(15) 0.0051(15) -0.0047(16) C10 0.0398(16) 0.0392(18) 0.0396(16) -0.0025(14) 0.0098(13) 0.0020(13) C11 0.0439(17) 0.0328(16) 0.0374(16) -0.0004(13) 0.0099(13) 0.0014(13) C12 0.0445(17) 0.0349(17) 0.0426(17) -0.0006(14) 0.0134(14) -0.0003(14) C13 0.0471(18) 0.0366(18) 0.0445(18) 0.0039(14) 0.0057(14) -0.0063(14) C14 0.060(2) 0.0345(17) 0.0391(17) -0.0053(14) 0.0144(15) -0.0064(15) C15 0.0517(19) 0.0320(17) 0.0461(18) -0.0019(14) 0.0180(15) 0.0025(14) C16 0.0429(18) 0.0344(17) 0.0464(18) 0.0006(14) 0.0112(14) 0.0018(14) C17 0.062(3) 0.111(4) 0.073(3) 0.006(3) 0.021(2) -0.026(3) C18 0.082(3) 0.082(3) 0.0341(18) -0.0042(19) 0.0111(18) 0.004(2) C19 0.072(3) 0.074(3) 0.065(2) 0.000(2) 0.009(2) -0.026(2) C20 0.050(2) 0.130(4) 0.057(2) 0.004(3) -0.0018(18) 0.006(2) C22 0.086(3) 0.054(2) 0.053(2) 0.0166(19) 0.009(2) 0.003(2) C23 0.076(3) 0.070(3) 0.052(2) 0.0028(19) 0.0259(19) -0.008(2) C21 0.061(6) 0.20(2) 0.050(6) 0.023(8) 0.005(5) 0.006(10) C21' 0.100(13) 0.17(3) 0.11(2) 0.11(2) -0.067(14) -0.040(18) _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 Zn O1 1.952(2) . ? Zn C20 1.954(4) . ? Zn N1 2.150(2) . ? Zn N2 2.162(3) . ? Cl1 C13 1.743(3) . ? Cl2 C15 1.748(3) . ? O1 C16 1.291(4) . ? N1 C10 1.483(4) . ? N1 C8 1.485(3) . ? N1 C7 1.490(3) . ? N2 C18 1.473(4) . ? N2 C9 1.480(4) . ? N2 C17 1.490(4) . ? N3 C1 1.425(4) . ? N3 C19 1.449(4) . ? N3 C22 1.454(4) . ? C1 C2 1.384(4) . ? C1 C6 1.403(4) . ? C2 C3 1.377(4) . ? C2 H2 0.9300 . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 C23 1.494(4) . ? C5 C6 1.387(4) . ? C5 H5 0.9300 . ? C6 C7 1.516(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.503(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.506(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.377(4) . ? C11 C16 1.423(4) . ? C12 C13 1.373(4) . ? C12 H12 0.9300 . ? C13 C14 1.381(4) . ? C14 C15 1.359(5) . ? C14 H14 0.9300 . ? C15 C16 1.416(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21' 1.419(14) . ? C20 C21 1.432(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9600 . ? C20 H20D 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? 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 Zn C20 122.58(17) . . ? O1 Zn N1 94.13(9) . . ? C20 Zn N1 123.57(14) . . ? O1 Zn N2 105.36(10) . . ? C20 Zn N2 119.28(16) . . ? N1 Zn N2 83.34(9) . . ? C16 O1 Zn 124.26(19) . . ? C10 N1 C8 112.4(2) . . ? C10 N1 C7 111.4(2) . . ? C8 N1 C7 113.1(2) . . ? C10 N1 Zn 107.15(17) . . ? C8 N1 Zn 107.17(16) . . ? C7 N1 Zn 104.99(16) . . ? C18 N2 C9 110.5(3) . . ? C18 N2 C17 109.2(3) . . ? C9 N2 C17 110.1(3) . . ? C18 N2 Zn 112.1(2) . . ? C9 N2 Zn 104.43(17) . . ? C17 N2 Zn 110.4(2) . . ? C1 N3 C19 113.4(2) . . ? C1 N3 C22 113.2(3) . . ? C19 N3 C22 110.9(3) . . ? C2 C1 C6 118.0(3) . . ? C2 C1 N3 122.3(3) . . ? C6 C1 N3 119.7(2) . . ? C3 C2 C1 122.0(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 116.9(3) . . ? C3 C4 C23 121.7(3) . . ? C5 C4 C23 121.4(3) . . ? C6 C5 C4 123.1(3) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C5 C6 C1 118.9(2) . . ? C5 C6 C7 118.3(3) . . ? C1 C6 C7 122.7(3) . . ? N1 C7 C6 118.2(2) . . ? N1 C7 H7A 107.8 . . ? C6 C7 H7A 107.8 . . ? N1 C7 H7B 107.8 . . ? C6 C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? N1 C8 C9 110.3(2) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N2 C9 C8 111.3(3) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N1 C10 C11 113.8(2) . . ? N1 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N1 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 121.3(3) . . ? C12 C11 C10 119.8(3) . . ? C16 C11 C10 118.8(3) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 Cl1 120.6(2) . . ? C14 C13 Cl1 119.1(2) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 124.3(3) . . ? C14 C15 Cl2 118.5(2) . . ? C16 C15 Cl2 117.2(2) . . ? O1 C16 C15 122.2(3) . . ? O1 C16 C11 123.3(3) . . ? C15 C16 C11 114.5(3) . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21' C20 C21 39.0(15) . . ? C21' C20 Zn 115.0(12) . . ? C21 C20 Zn 126.4(6) . . ? C21' C20 H20A 137.6 . . ? C21 C20 H20A 105.7 . . ? Zn C20 H20A 105.7 . . ? C21' C20 H20B 74.6 . . ? C21 C20 H20B 105.7 . . ? Zn C20 H20B 105.7 . . ? H20A C20 H20B 106.2 . . ? C21' C20 H20C 106.2 . . ? C21 C20 H20C 122.9 . . ? Zn C20 H20C 108.2 . . ? H20A C20 H20C 70.2 . . ? H20B C20 H20C 36.8 . . ? C21' C20 H20D 111.5 . . ? C21 C20 H20D 72.6 . . ? Zn C20 H20D 107.6 . . ? H20A C20 H20D 40.9 . . ? H20B C20 H20D 138.6 . . ? H20C C20 H20D 108.1 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C21 H20D 38.7 . . ? C20 C21 H21A 109.5 . . ? H20D C21 H21A 106.4 . . ? C20 C21 H21B 109.5 . . ? H20D C21 H21B 74.9 . . ? C20 C21 H21C 109.5 . . ? H20D C21 H21C 139.4 . . ? C20 C21' H21D 109.5 . . ? C20 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C20 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 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 C20 Zn O1 C16 -157.3(2) . . . . ? N1 Zn O1 C16 -22.5(2) . . . . ? N2 Zn O1 C16 61.7(2) . . . . ? O1 Zn N1 C10 -24.85(18) . . . . ? C20 Zn N1 C10 109.2(2) . . . . ? N2 Zn N1 C10 -129.85(18) . . . . ? O1 Zn N1 C8 96.04(18) . . . . ? C20 Zn N1 C8 -129.9(2) . . . . ? N2 Zn N1 C8 -8.96(18) . . . . ? O1 Zn N1 C7 -143.39(18) . . . . ? C20 Zn N1 C7 -9.3(3) . . . . ? N2 Zn N1 C7 111.60(18) . . . . ? O1 Zn N2 C18 8.7(2) . . . . ? C20 Zn N2 C18 -133.9(3) . . . . ? N1 Zn N2 C18 101.2(2) . . . . ? O1 Zn N2 C9 -110.97(19) . . . . ? C20 Zn N2 C9 106.4(2) . . . . ? N1 Zn N2 C9 -18.50(19) . . . . ? O1 Zn N2 C17 130.7(2) . . . . ? C20 Zn N2 C17 -11.9(3) . . . . ? N1 Zn N2 C17 -136.8(2) . . . . ? C19 N3 C1 C2 -85.6(4) . . . . ? C22 N3 C1 C2 41.8(4) . . . . ? C19 N3 C1 C6 93.2(3) . . . . ? C22 N3 C1 C6 -139.4(3) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? N3 C1 C2 C3 178.7(3) . . . . ? C1 C2 C3 C4 -1.1(5) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C2 C3 C4 C23 -179.4(3) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C23 C4 C5 C6 -179.3(3) . . . . ? C4 C5 C6 C1 -1.7(4) . . . . ? C4 C5 C6 C7 -177.0(3) . . . . ? C2 C1 C6 C5 1.4(4) . . . . ? N3 C1 C6 C5 -177.5(2) . . . . ? C2 C1 C6 C7 176.5(3) . . . . ? N3 C1 C6 C7 -2.3(4) . . . . ? C10 N1 C7 C6 59.0(3) . . . . ? C8 N1 C7 C6 -68.8(3) . . . . ? Zn N1 C7 C6 174.7(2) . . . . ? C5 C6 C7 N1 -93.8(3) . . . . ? C1 C6 C7 N1 91.0(3) . . . . ? C10 N1 C8 C9 152.8(2) . . . . ? C7 N1 C8 C9 -79.9(3) . . . . ? Zn N1 C8 C9 35.4(3) . . . . ? C18 N2 C9 C8 -76.7(3) . . . . ? C17 N2 C9 C8 162.6(3) . . . . ? Zn N2 C9 C8 44.1(3) . . . . ? N1 C8 C9 N2 -55.8(3) . . . . ? C8 N1 C10 C11 -54.1(3) . . . . ? C7 N1 C10 C11 177.7(2) . . . . ? Zn N1 C10 C11 63.4(3) . . . . ? N1 C10 C11 C12 122.4(3) . . . . ? N1 C10 C11 C16 -60.9(4) . . . . ? C16 C11 C12 C13 0.6(4) . . . . ? C10 C11 C12 C13 177.1(3) . . . . ? C11 C12 C13 C14 -1.3(4) . . . . ? C11 C12 C13 Cl1 178.9(2) . . . . ? C12 C13 C14 C15 1.4(5) . . . . ? Cl1 C13 C14 C15 -178.8(2) . . . . ? C13 C14 C15 C16 -0.9(5) . . . . ? C13 C14 C15 Cl2 -178.8(2) . . . . ? Zn O1 C16 C15 -143.2(2) . . . . ? Zn O1 C16 C11 36.9(4) . . . . ? C14 C15 C16 O1 -179.8(3) . . . . ? Cl2 C15 C16 O1 -1.8(4) . . . . ? C14 C15 C16 C11 0.2(4) . . . . ? Cl2 C15 C16 C11 178.1(2) . . . . ? C12 C11 C16 O1 179.9(3) . . . . ? C10 C11 C16 O1 3.4(4) . . . . ? C12 C11 C16 C15 0.0(4) . . . . ? C10 C11 C16 C15 -176.6(3) . . . . ? O1 Zn C20 C21' 52(2) . . . . ? N1 Zn C20 C21' -70(2) . . . . ? N2 Zn C20 C21' -172(2) . . . . ? O1 Zn C20 C21 95.4(15) . . . . ? N1 Zn C20 C21 -26.4(16) . . . . ? N2 Zn C20 C21 -128.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.566 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.070 # End =======================================================================