Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Juan C Mareque-Rivas' _publ_contact_author_address ; School of Chemistry The University of Edinburgh West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email JUAN.MAREQUE@ED.AC.UK _publ_section_title ; Investigating the effect of hydrogen bonding environments in amide cleavage reactions at zinc(II) complexes with intramolecular amide oxygen co-ordination ; loop_ _publ_author_name 'Juan C. Mareque-Rivas' 'Simon Parsons' 'Emiliano Salvagni' #===END #Crystallographic information (CIF) data_r52113b _database_code_depnum_ccdc_archive 'CCDC 228550' # Referred to as 7(ClO4)2 in manuscript # Checkcif output under refine special details _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C21 H32 N6 O S Zn] (Cl O4)2' _chemical_formula_sum 'C21 H32 Cl2 N6 O9 S Zn' _chemical_formula_weight 680.86 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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0729(12) _cell_length_b 10.6189(12) _cell_length_c 14.2244(16) _cell_angle_alpha 87.826(2) _cell_angle_beta 85.209(2) _cell_angle_gamma 69.217(2) _cell_volume 1417.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10285 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4928 _reflns_number_gt 3847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio The H-atom parameters are of course less precise than others in the structure, but this refinement did converge, and so we prefer to retain this model because NH-atom positions are important for the discussion of H-bonding in the text. #=============================================================================== 029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.99 No action. #=============================================================================== 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 213_ALERT_2_C Atom C8 has ADP max/min Ratio ............. 3.70 oblate 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 352_ALERT_3_C Short N-H Bond (0.87A) N7 - H7N = 0.76 Ang. 432_ALERT_2_C Short Inter X...Y Contact O1P .. C6 = 2.93 Ang. 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 51.00 A**3 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 Cl O4 Noted - some of these can be traced to the lowish quality of the data. #=============================================================================== ; _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^)+(0.0424P)^2^+0.9169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment riding/refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4928 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _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 Zn Zn 0.28016(7) 0.68130(7) 0.23147(5) 0.0142(2) Uani 1 1 d . . . N1A N 0.4756(6) 0.5481(5) 0.1843(4) 0.0181(12) Uani 1 1 d . . . H1NB H 0.544(6) 0.581(5) 0.185(3) 0.002(14) Uiso 1 1 d . . . H1NA H 0.475(7) 0.521(7) 0.123(5) 0.04(2) Uiso 1 1 d . . . N1 N 0.0994(5) 0.6452(5) 0.1878(3) 0.0152(11) Uani 1 1 d . . . C1 C 0.1128(6) 0.6583(6) 0.0831(4) 0.0171(14) Uani 1 1 d . . . H1A H 0.0197 0.6730 0.0579 0.021 Uiso 1 1 calc R . . H1B H 0.1826 0.5739 0.0560 0.021 Uiso 1 1 calc R . . C1A C 0.5132(6) 0.4255(6) 0.2432(4) 0.0212(14) Uani 1 1 d . . . H1AA H 0.6174 0.3900 0.2488 0.025 Uiso 1 1 calc R . . H1AB H 0.4879 0.3560 0.2123 0.025 Uiso 1 1 calc R . . N2 N 0.2214(5) 0.8187(4) 0.1206(3) 0.0151(11) Uani 1 1 d . . . N2A N 0.3246(5) 0.5668(5) 0.3527(3) 0.0180(11) Uani 1 1 d . . . C2A C 0.4378(6) 0.4517(6) 0.3403(4) 0.0173(14) Uani 1 1 d . . . C2 C 0.1605(6) 0.7743(6) 0.0543(4) 0.0146(13) Uani 1 1 d . . . C3A C 0.4816(7) 0.3597(6) 0.4123(4) 0.0236(15) Uani 1 1 d . . . H3AA H 0.5642 0.2811 0.4033 0.028 Uiso 1 1 calc R . . C3 C 0.1473(6) 0.8308(6) -0.0341(4) 0.0216(15) Uani 1 1 d . . . H3A H 0.1037 0.7992 -0.0801 0.026 Uiso 1 1 calc R . . C4A C 0.4018(7) 0.3847(6) 0.4985(4) 0.0271(16) Uani 1 1 d . . . H4AA H 0.4268 0.3199 0.5480 0.033 Uiso 1 1 calc R . . C4 C 0.1976(7) 0.9335(6) -0.0555(4) 0.0229(15) Uani 1 1 d . . . H4A H 0.1952 0.9694 -0.1178 0.028 Uiso 1 1 calc R . . C5 C 0.2516(6) 0.9844(6) 0.0134(4) 0.0202(14) Uani 1 1 d . . . H5A H 0.2823 1.0584 0.0003 0.024 Uiso 1 1 calc R . . C5A C 0.2881(7) 0.5012(6) 0.5130(4) 0.0238(15) Uani 1 1 d . . . H5AA H 0.2336 0.5184 0.5720 0.029 Uiso 1 1 calc R . . C6 C 0.2604(6) 0.9257(6) 0.1027(4) 0.0154(13) Uani 1 1 d . . . C6A C 0.2534(7) 0.5952(6) 0.4384(4) 0.0211(14) Uani 1 1 d . . . N7 N 0.3073(5) 0.9795(5) 0.1752(4) 0.0164(12) Uani 1 1 d . . . H7N H 0.325(6) 1.042(6) 0.162(4) 0.013(18) Uiso 1 1 d . . . N7A N 0.1436(6) 0.7143(6) 0.4503(4) 0.0271(14) Uani 1 1 d . . . H7NB H 0.102(8) 0.748(7) 0.514(6) 0.06(3) Uiso 1 1 d . . . H7NA H 0.148(5) 0.781(5) 0.416(4) 0.002(14) Uiso 1 1 d . . . O8 O 0.2865(4) 0.8453(4) 0.3000(3) 0.0205(10) Uani 1 1 d . . . C8 C 0.3062(6) 0.9488(6) 0.2681(4) 0.0151(13) Uani 1 1 d . . . C9 C 0.3374(6) 1.0413(6) 0.3345(4) 0.0161(13) Uani 1 1 d . . . C10C C 0.3031(7) 1.0062(6) 0.4365(4) 0.0263(16) Uani 1 1 d . . . H10A H 0.2011 1.0218 0.4468 0.039 Uiso 1 1 calc R . . H10B H 0.3284 1.0629 0.4793 0.039 Uiso 1 1 calc R . . H10C H 0.3577 0.9112 0.4490 0.039 Uiso 1 1 calc R . . C10A C 0.2510(7) 1.1898(6) 0.3152(5) 0.0244(15) Uani 1 1 d . . . H10D H 0.1491 1.2046 0.3248 0.037 Uiso 1 1 calc R . . H10E H 0.2735 1.2129 0.2499 0.037 Uiso 1 1 calc R . . H10F H 0.2752 1.2467 0.3584 0.037 Uiso 1 1 calc R . . C10B C 0.4974(6) 1.0166(7) 0.3188(5) 0.0293(17) Uani 1 1 d . . . H10G H 0.5198 1.0390 0.2534 0.044 Uiso 1 1 calc R . . H10H H 0.5519 0.9217 0.3315 0.044 Uiso 1 1 calc R . . H10I H 0.5226 1.0734 0.3616 0.044 Uiso 1 1 calc R . . C11 C -0.0284(6) 0.7528(6) 0.2310(4) 0.0186(14) Uani 1 1 d . . . H11B H -0.0229 0.8414 0.2114 0.022 Uiso 1 1 calc R . . H11A H -0.0255 0.7459 0.3005 0.022 Uiso 1 1 calc R . . C12 C -0.1696(7) 0.7489(6) 0.2059(5) 0.0256(16) Uani 1 1 d . . . H12B H -0.1746 0.7582 0.1366 0.031 Uiso 1 1 calc R . . H12A H -0.2475 0.8264 0.2353 0.031 Uiso 1 1 calc R . . S13 S -0.19587(18) 0.59454(18) 0.24452(12) 0.0286(4) Uani 1 1 d . . . C14 C -0.0324(6) 0.4798(6) 0.1887(4) 0.0233(15) Uani 1 1 d . . . H14B H -0.0222 0.3862 0.2074 0.028 Uiso 1 1 calc R . . H14A H -0.0365 0.4876 0.1193 0.028 Uiso 1 1 calc R . . C15 C 0.0963(6) 0.5092(6) 0.2162(4) 0.0187(14) Uani 1 1 d . . . H15B H 0.0997 0.4999 0.2856 0.022 Uiso 1 1 calc R . . H15A H 0.1834 0.4401 0.1876 0.022 Uiso 1 1 calc R . . Cl1 Cl 0.37314(16) 1.28564(15) 0.01433(10) 0.0199(4) Uani 1 1 d . . . O1P O 0.4319(5) 1.2165(4) -0.0727(3) 0.0286(11) Uani 1 1 d . . . O2P O 0.4201(5) 1.1965(4) 0.0931(3) 0.0316(11) Uani 1 1 d . . . O3P O 0.2204(4) 1.3327(4) 0.0173(3) 0.0287(11) Uani 1 1 d . . . O4P O 0.4187(5) 1.3992(4) 0.0217(3) 0.0301(11) Uani 1 1 d . . . Cl2 Cl 0.89530(15) 0.11387(15) 0.31267(10) 0.0190(4) Uani 1 1 d . . . O5P O 0.9950(4) 0.0794(4) 0.2309(3) 0.0286(11) Uani 1 1 d . . . O6P O 0.8581(5) 0.2540(4) 0.3331(3) 0.0349(12) Uani 1 1 d . . . O7P O 0.9590(5) 0.0352(5) 0.3917(3) 0.0411(13) Uani 1 1 d . . . O8P O 0.7691(5) 0.0887(5) 0.2945(3) 0.0369(13) 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 Zn 0.0158(4) 0.0130(4) 0.0147(4) 0.0014(3) -0.0015(3) -0.0061(3) N1A 0.016(3) 0.022(3) 0.018(3) 0.002(2) -0.001(2) -0.010(3) N1 0.017(3) 0.014(3) 0.016(3) 0.002(2) -0.001(2) -0.008(2) C1 0.023(4) 0.012(3) 0.013(3) -0.001(2) -0.006(3) -0.002(3) C1A 0.019(4) 0.016(3) 0.024(4) 0.000(3) -0.002(3) -0.001(3) N2 0.017(3) 0.009(3) 0.020(3) 0.001(2) 0.001(2) -0.006(2) N2A 0.016(3) 0.017(3) 0.023(3) -0.001(2) 0.000(2) -0.008(2) C2A 0.019(3) 0.021(3) 0.018(3) 0.000(3) -0.007(3) -0.014(3) C2 0.013(3) 0.014(3) 0.018(3) 0.000(3) -0.003(3) -0.005(3) C3A 0.022(4) 0.020(4) 0.032(4) 0.005(3) -0.005(3) -0.011(3) C3 0.026(4) 0.024(4) 0.022(4) -0.004(3) -0.008(3) -0.016(3) C4A 0.041(4) 0.021(4) 0.025(4) 0.003(3) -0.006(3) -0.017(3) C4 0.028(4) 0.023(4) 0.015(3) 0.005(3) -0.004(3) -0.006(3) C5 0.023(4) 0.014(3) 0.024(4) 0.006(3) 0.004(3) -0.009(3) C5A 0.035(4) 0.026(4) 0.014(3) 0.000(3) 0.003(3) -0.016(3) C6 0.008(3) 0.018(3) 0.017(3) -0.001(3) -0.003(2) 0.000(3) C6A 0.022(4) 0.025(4) 0.021(4) -0.002(3) 0.002(3) -0.014(3) N7 0.020(3) 0.013(3) 0.018(3) 0.000(2) 0.002(2) -0.009(2) N7A 0.031(4) 0.020(3) 0.026(3) 0.001(3) 0.005(3) -0.006(3) O8 0.030(3) 0.016(2) 0.020(2) -0.0007(18) -0.0002(19) -0.013(2) C8 0.004(3) 0.014(3) 0.022(3) -0.002(3) 0.005(2) 0.002(2) C9 0.014(3) 0.013(3) 0.023(3) 0.003(3) -0.007(3) -0.006(3) C10C 0.037(4) 0.022(4) 0.026(4) -0.004(3) -0.007(3) -0.016(3) C10A 0.027(4) 0.016(3) 0.031(4) -0.006(3) -0.005(3) -0.008(3) C10B 0.017(4) 0.033(4) 0.038(4) -0.010(3) -0.002(3) -0.008(3) C11 0.021(4) 0.021(3) 0.016(3) -0.005(3) 0.000(3) -0.010(3) C12 0.019(4) 0.025(4) 0.031(4) -0.001(3) 0.005(3) -0.008(3) S13 0.0217(9) 0.0367(11) 0.0333(10) 0.0058(8) 0.0004(8) -0.0188(8) C14 0.025(4) 0.027(4) 0.026(4) 0.006(3) -0.006(3) -0.018(3) C15 0.025(4) 0.017(3) 0.017(3) -0.001(3) 0.002(3) -0.012(3) Cl1 0.0211(9) 0.0210(8) 0.0209(8) -0.0018(6) 0.0013(7) -0.0120(7) O1P 0.028(3) 0.032(3) 0.025(3) -0.010(2) 0.002(2) -0.011(2) O2P 0.042(3) 0.039(3) 0.022(3) 0.012(2) -0.010(2) -0.024(2) O3P 0.018(3) 0.034(3) 0.035(3) -0.013(2) 0.005(2) -0.011(2) O4P 0.043(3) 0.025(3) 0.030(3) -0.006(2) 0.003(2) -0.022(2) Cl2 0.0151(8) 0.0246(9) 0.0178(8) -0.0041(6) 0.0012(6) -0.0080(7) O5P 0.024(3) 0.038(3) 0.019(2) -0.005(2) 0.007(2) -0.006(2) O6P 0.036(3) 0.026(3) 0.042(3) -0.013(2) 0.011(2) -0.013(2) O7P 0.043(3) 0.048(3) 0.027(3) 0.016(2) -0.011(2) -0.010(3) O8P 0.018(3) 0.056(3) 0.043(3) -0.015(3) 0.003(2) -0.021(2) _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 N1A 2.050(5) . ? Zn O8 2.051(4) . ? Zn N2A 2.058(5) . ? Zn N2 2.082(5) . ? Zn N1 2.134(5) . ? N1A C1A 1.471(7) . ? N1A H1NB 0.87(5) . ? N1A H1NA 0.93(7) . ? N1 C1 1.489(7) . ? N1 C11 1.490(7) . ? N1 C15 1.494(7) . ? C1 C2 1.505(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1A C2A 1.505(8) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? N2 C6 1.336(7) . ? N2 C2 1.351(7) . ? N2A C6A 1.349(7) . ? N2A C2A 1.349(7) . ? C2A C3A 1.375(8) . ? C2 C3 1.368(8) . ? C3A C4A 1.389(8) . ? C3A H3AA 0.9500 . ? C3 C4 1.372(8) . ? C3 H3A 0.9500 . ? C4A C5A 1.363(9) . ? C4A H4AA 0.9500 . ? C4 C5 1.373(8) . ? C4 H4A 0.9500 . ? C5 C6 1.388(8) . ? C5 H5A 0.9500 . ? C5A C6A 1.407(8) . ? C5A H5AA 0.9500 . ? C6 N7 1.390(7) . ? C6A N7A 1.358(8) . ? N7 C8 1.350(7) . ? N7 H7N 0.76(6) . ? N7A H7NB 0.99(8) . ? N7A H7NA 0.86(5) . ? O8 C8 1.247(7) . ? C8 C9 1.516(8) . ? C9 C10C 1.526(8) . ? C9 C10A 1.534(8) . ? C9 C10B 1.536(8) . ? C10C H10A 0.9800 . ? C10C H10B 0.9800 . ? C10C H10C 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C10B H10G 0.9800 . ? C10B H10H 0.9800 . ? C10B H10I 0.9800 . ? C11 C12 1.510(8) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 S13 1.810(6) . ? C12 H12B 0.9900 . ? C12 H12A 0.9900 . ? S13 C14 1.805(6) . ? C14 C15 1.521(8) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? Cl1 O1P 1.435(4) . ? Cl1 O2P 1.437(4) . ? Cl1 O3P 1.437(4) . ? Cl1 O4P 1.445(4) . ? Cl2 O7P 1.429(4) . ? Cl2 O8P 1.434(4) . ? Cl2 O6P 1.435(4) . ? Cl2 O5P 1.439(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Zn O8 114.6(2) . . ? N1A Zn N2A 82.3(2) . . ? O8 Zn N2A 90.57(17) . . ? N1A Zn N2 104.01(19) . . ? O8 Zn N2 82.91(17) . . ? N2A Zn N2 172.36(19) . . ? N1A Zn N1 116.3(2) . . ? O8 Zn N1 128.61(17) . . ? N2A Zn N1 102.88(18) . . ? N2 Zn N1 78.39(18) . . ? C1A N1A Zn 110.0(4) . . ? C1A N1A H1NB 108(3) . . ? Zn N1A H1NB 113(3) . . ? C1A N1A H1NA 106(4) . . ? Zn N1A H1NA 111(4) . . ? H1NB N1A H1NA 108(5) . . ? C1 N1 C11 112.1(4) . . ? C1 N1 C15 110.7(4) . . ? C11 N1 C15 110.4(4) . . ? C1 N1 Zn 103.7(3) . . ? C11 N1 Zn 106.4(3) . . ? C15 N1 Zn 113.3(3) . . ? N1 C1 C2 110.7(4) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1A C1A C2A 112.0(5) . . ? N1A C1A H1AA 109.2 . . ? C2A C1A H1AA 109.2 . . ? N1A C1A H1AB 109.2 . . ? C2A C1A H1AB 109.2 . . ? H1AA C1A H1AB 107.9 . . ? C6 N2 C2 120.0(5) . . ? C6 N2 Zn 126.9(4) . . ? C2 N2 Zn 111.9(4) . . ? C6A N2A C2A 119.7(5) . . ? C6A N2A Zn 127.2(4) . . ? C2A N2A Zn 113.1(4) . . ? N2A C2A C3A 121.9(6) . . ? N2A C2A C1A 117.3(5) . . ? C3A C2A C1A 120.8(6) . . ? N2 C2 C3 121.1(5) . . ? N2 C2 C1 116.0(5) . . ? C3 C2 C1 122.9(5) . . ? C2A C3A C4A 118.2(6) . . ? C2A C3A H3AA 120.9 . . ? C4A C3A H3AA 120.9 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5A C4A C3A 120.8(6) . . ? C5A C4A H4AA 119.6 . . ? C3A C4A H4AA 119.6 . . ? C3 C4 C5 119.7(6) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 118.9(6) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C4A C5A C6A 118.4(6) . . ? C4A C5A H5AA 120.8 . . ? C6A C5A H5AA 120.8 . . ? N2 C6 C5 120.7(5) . . ? N2 C6 N7 119.1(5) . . ? C5 C6 N7 120.2(5) . . ? N2A C6A N7A 118.7(6) . . ? N2A C6A C5A 120.8(6) . . ? N7A C6A C5A 120.5(6) . . ? C8 N7 C6 129.1(5) . . ? C8 N7 H7N 115(4) . . ? C6 N7 H7N 115(4) . . ? C6A N7A H7NB 121(4) . . ? C6A N7A H7NA 117(4) . . ? H7NB N7A H7NA 109(6) . . ? C8 O8 Zn 130.3(4) . . ? O8 C8 N7 122.5(5) . . ? O8 C8 C9 119.6(5) . . ? N7 C8 C9 117.9(5) . . ? C8 C9 C10C 109.8(5) . . ? C8 C9 C10A 111.7(5) . . ? C10C C9 C10A 109.3(5) . . ? C8 C9 C10B 106.8(5) . . ? C10C C9 C10B 109.3(5) . . ? C10A C9 C10B 110.0(5) . . ? C9 C10C H10A 109.5 . . ? C9 C10C H10B 109.5 . . ? H10A C10C H10B 109.5 . . ? C9 C10C H10C 109.5 . . ? H10A C10C H10C 109.5 . . ? H10B C10C H10C 109.5 . . ? C9 C10A H10D 109.5 . . ? C9 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C9 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C9 C10B H10G 109.5 . . ? C9 C10B H10H 109.5 . . ? H10G C10B H10H 109.5 . . ? C9 C10B H10I 109.5 . . ? H10G C10B H10I 109.5 . . ? H10H C10B H10I 109.5 . . ? N1 C11 C12 115.1(5) . . ? N1 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? N1 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? H11B C11 H11A 107.5 . . ? C11 C12 S13 112.4(4) . . ? C11 C12 H12B 109.1 . . ? S13 C12 H12B 109.1 . . ? C11 C12 H12A 109.1 . . ? S13 C12 H12A 109.1 . . ? H12B C12 H12A 107.9 . . ? C14 S13 C12 97.0(3) . . ? C15 C14 S13 111.5(4) . . ? C15 C14 H14B 109.3 . . ? S13 C14 H14B 109.3 . . ? C15 C14 H14A 109.3 . . ? S13 C14 H14A 109.3 . . ? H14B C14 H14A 108.0 . . ? N1 C15 C14 115.4(5) . . ? N1 C15 H15B 108.4 . . ? C14 C15 H15B 108.4 . . ? N1 C15 H15A 108.4 . . ? C14 C15 H15A 108.4 . . ? H15B C15 H15A 107.5 . . ? O1P Cl1 O2P 110.3(3) . . ? O1P Cl1 O3P 109.5(3) . . ? O2P Cl1 O3P 109.1(3) . . ? O1P Cl1 O4P 110.1(3) . . ? O2P Cl1 O4P 108.7(3) . . ? O3P Cl1 O4P 109.3(3) . . ? O7P Cl2 O8P 110.1(3) . . ? O7P Cl2 O6P 109.1(3) . . ? O8P Cl2 O6P 109.1(3) . . ? O7P Cl2 O5P 109.5(3) . . ? O8P Cl2 O5P 109.6(3) . . ? O6P Cl2 O5P 109.5(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.878 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.105 #CRYSTALLOGRAPHIC INFORMATION (CIF) data_r85170 _database_code_depnum_ccdc_archive 'CCDC 250153' # Referred to as 2(ClO4)2CH3CN in manuscript # Checkcif output and final .res file under refine special details _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H28 N6 O Zn, 2(Cl O4), C2 H3 N' _chemical_formula_sum 'C25 H31 Cl2 N7 O9 Zn' _chemical_formula_weight 709.84 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8999(4) _cell_length_b 11.5861(4) _cell_length_c 14.3217(5) _cell_angle_alpha 72.3300(10) _cell_angle_beta 75.5930(10) _cell_angle_gamma 86.876(2) _cell_volume 1515.60(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6733 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28.5 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.780 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART APEX CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14264 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.96 _reflns_number_total 7045 _reflns_number_gt 6193 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The disordered ClO4- was treated using a pair of variable-metric rigid groups. 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? The H's are in calculated positions. 911_ALERT_3_B Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 53 912_ALERT_3_B Missing FCF Reflections Above STH/L=0.6 ........ 932 Coverage statistics: #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 3185 3182 3 23.01 0.550 0.996 4227 4209 18 25.24 0.600 0.990 5473 5420 53 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.969 6967 6753 214 29.84 0.700 0.877 8030 7045 985 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.68 mm Gorbitz has shown that use of a large crystal does not appear to affect data quality. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 10 H's involved in H-bonding were refined. 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl1 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl1' 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C1S 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl2 Mostly these are in the perchlorate & solvent MeCN. 301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. 302_ALERT_4_C Anion/Solvent Disorder ......................... 28.00 Perc. 430_ALERT_2_C Short Inter D...A Contact O1' .. O1' .. 2.87 Ang. 432_ALERT_2_C Short Inter X...Y Contact O3A .. C8 .. 2.97 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 Cl O4 Noted, no action. #TITL test2 in P-1 CELL 0.71073 9.8999 11.5861 14.3217 72.330 75.593 86.876 ZERR 2.00 0.0004 0.0004 0.0005 0.001 0.001 0.002 LATT 1 SFAC C H N O CL ZN UNIT 50 62 14 18 4 2 TEMP -123 ACTA L.S. 4 BOND FMAP 2 PLAN 20 WGHT 0.054900 1.400900 FVAR 0.52728 0.77357 0.58517 ZN 6 0.973683 0.209655 0.265868 11.00000 0.02362 0.02134 = 0.02741 -0.01023 -0.00540 -0.00220 N1 3 1.055577 0.342387 0.314948 11.00000 0.02819 0.02544 = 0.03067 -0.01199 -0.00518 -0.00310 C1 1 1.059592 0.285267 0.420807 11.00000 0.03078 0.03130 = 0.03479 -0.01527 -0.01011 -0.00378 AFIX 23 H1A 2 1.050392 0.348247 0.455607 11.00000 -1.20000 H1B 2 1.150844 0.246612 0.423271 11.00000 -1.20000 AFIX 0 N2 3 0.907035 0.128368 0.419081 11.00000 0.02093 0.02414 = 0.02651 -0.01013 -0.00733 0.00180 C2 1 0.944263 0.191140 0.475363 11.00000 0.02353 0.02600 = 0.03092 -0.01246 -0.01064 0.00374 C3 1 0.884039 0.167876 0.576679 11.00000 0.03300 0.03341 = 0.03065 -0.01547 -0.01315 0.00724 AFIX 43 H3A 2 0.910466 0.213982 0.614223 11.00000 -1.20000 AFIX 0 C4 1 0.783610 0.075509 0.623251 11.00000 0.03369 0.03786 = 0.02550 -0.00957 -0.00638 0.00557 AFIX 43 H4A 2 0.740035 0.058189 0.693209 11.00000 -1.20000 AFIX 0 C5 1 0.747522 0.009251 0.567696 11.00000 0.02855 0.02798 = 0.02898 -0.00558 -0.00605 0.00069 AFIX 43 H5A 2 0.680627 -0.055380 0.598802 11.00000 -1.20000 AFIX 0 C6 1 0.811367 0.039080 0.464598 11.00000 0.02131 0.02234 = 0.02819 -0.00955 -0.00736 0.00373 N7 3 0.772679 -0.029163 0.408976 11.00000 0.02234 0.02390 = 0.02961 -0.00854 -0.00519 -0.00414 H7N 2 0.704842 -0.073393 0.442297 11.00000 0.03032 O8 4 0.894962 0.063140 0.246808 11.00000 0.03110 0.02569 = 0.02755 -0.01270 -0.00161 -0.00686 C8 1 0.810535 -0.016482 0.308757 11.00000 0.02202 0.02273 = 0.03044 -0.01063 -0.00746 0.00213 C9 1 0.743642 -0.105347 0.272625 11.00000 0.03112 0.02554 = 0.03556 -0.01051 -0.01050 -0.00532 C10B 1 0.811659 -0.087654 0.160860 11.00000 0.08259 0.03693 = 0.03298 -0.01159 -0.01762 -0.01917 AFIX 33 H10A 2 0.911487 -0.103906 0.152176 11.00000 -1.50000 H10B 2 0.799162 -0.004074 0.121578 11.00000 -1.50000 H10C 2 0.767930 -0.143639 0.137179 11.00000 -1.50000 AFIX 0 C10A 1 0.587202 -0.079111 0.287974 11.00000 0.03940 0.04215 = 0.10420 -0.03724 -0.03954 0.00644 AFIX 33 H10D 2 0.545247 -0.090136 0.359800 11.00000 -1.50000 H10E 2 0.541872 -0.134962 0.265129 11.00000 -1.50000 H10F 2 0.574672 0.004506 0.248785 11.00000 -1.50000 AFIX 0 C11 1 1.194563 0.381363 0.247269 11.00000 0.03345 0.03619 = 0.04046 -0.01460 -0.00447 -0.01251 AFIX 23 H11A 2 1.257049 0.395291 0.287264 11.00000 -1.20000 H11B 2 1.186281 0.459311 0.196051 11.00000 -1.20000 AFIX 0 N12 3 1.175873 0.205981 0.188998 11.00000 0.02693 0.02725 = 0.03056 -0.00999 -0.00447 0.00217 C12 1 1.259655 0.290263 0.193936 11.00000 0.02715 0.03789 = 0.02476 -0.00417 -0.00680 -0.00324 C13 1 1.400450 0.296798 0.147526 11.00000 0.02826 0.06598 = 0.03786 -0.00868 -0.00328 -0.01036 AFIX 43 H13A 2 1.459465 0.356061 0.151710 11.00000 -1.20000 AFIX 0 C14 1 1.453811 0.215688 0.094982 11.00000 0.02962 0.08351 = 0.04807 -0.01803 0.00357 0.00663 AFIX 43 H14A 2 1.550642 0.218307 0.063578 11.00000 -1.20000 AFIX 0 C15 1 1.368991 0.132267 0.087862 11.00000 0.04728 0.05352 = 0.03607 -0.01423 0.00233 0.01846 AFIX 43 H15A 2 1.405076 0.077442 0.050577 11.00000 -1.20000 AFIX 0 C16 1 1.229249 0.128667 0.135873 11.00000 0.03947 0.03236 = 0.03572 -0.01204 -0.00741 0.01058 PART 1 21 AFIX 43 H16A 2 1.169158 0.070387 0.131438 21.00000 -1.20000 AFIX 0 PART 0 C21 1 0.954331 0.441042 0.303768 11.00000 0.04091 0.02353 = 0.03517 -0.01327 -0.00760 0.00191 AFIX 23 H21A 2 0.998500 0.517006 0.301058 11.00000 -1.20000 H21B 2 0.873300 0.420804 0.363052 11.00000 -1.20000 AFIX 0 N22 3 0.889911 0.357804 0.184380 11.00000 0.03012 0.02718 = 0.02298 -0.00593 -0.00439 0.00109 C22 1 0.905553 0.459352 0.208920 11.00000 0.03589 0.02707 = 0.02831 -0.00836 -0.00094 0.00465 C23 1 0.875012 0.572004 0.152716 11.00000 0.06999 0.03048 = 0.03643 -0.00914 -0.00735 0.01321 AFIX 43 H23A 2 0.891801 0.642753 0.168891 11.00000 -1.20000 AFIX 0 C24 1 0.818844 0.579336 0.071525 11.00000 0.08246 0.04446 = 0.03658 -0.00198 -0.01797 0.02650 AFIX 43 H24A 2 0.793348 0.655800 0.032867 11.00000 -1.20000 AFIX 0 C25 1 0.800010 0.477888 0.046865 11.00000 0.06066 0.05742 = 0.03015 -0.00637 -0.01623 0.01548 AFIX 43 H25A 2 0.760737 0.482983 -0.008365 11.00000 -1.20000 AFIX 0 C26 1 0.839075 0.366136 0.103677 11.00000 0.03906 0.03956 = 0.02569 -0.00752 -0.00646 0.00044 PART 2 AFIX 43 H26E 2 0.829716 0.295361 0.085247 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 21 N27 3 0.835521 0.266711 0.077792 21.00000 0.05736 0.04398 = 0.03235 -0.00955 -0.02105 -0.01106 AFIX 93 H27A 2 0.865655 0.198416 0.112805 21.00000 -1.20000 H27B 2 0.803013 0.268597 0.025489 21.00000 -1.20000 AFIX 0 PART 2 -21 N27' 3 1.153456 0.064393 0.107773 -21.00000 0.04204 AFIX 93 H27C 2 1.062048 0.069811 0.123217 -21.00000 -1.20000 H27D 2 1.193292 0.015240 0.073209 -21.00000 -1.20000 AFIX 0 PART 0 C10C 1 0.765381 -0.235339 0.333447 11.00000 0.03702 0.02420 = 0.03932 -0.01141 -0.00989 -0.00286 AFIX 33 H10G 2 0.722355 -0.247099 0.405235 11.00000 -1.50000 H10H 2 0.865512 -0.250405 0.324135 11.00000 -1.50000 H10I 2 0.722217 -0.291883 0.309979 11.00000 -1.50000 AFIX 9 PART 1 31 CL1 5 0.548715 0.269011 0.371464 31.00000 0.02505 0.02417 = 0.02997 -0.00893 -0.00685 0.00062 O1A 4 0.411152 0.229462 0.430016 31.00000 0.03379 0.05603 = 0.04796 -0.00530 -0.00311 -0.00955 O2A 4 0.542538 0.381678 0.296465 31.00000 0.05640 0.02891 = 0.04562 -0.00074 -0.01048 0.00139 O3A 4 0.609991 0.180796 0.323562 31.00000 0.06784 0.03885 = 0.05665 -0.02687 -0.01496 0.02088 O4A 4 0.631177 0.284109 0.435817 31.00000 0.04681 0.05676 = 0.06527 -0.02602 -0.03118 0.00360 AFIX 9 PART 2 -31 CL1' 5 0.543931 0.239612 0.392105 -31.00000 0.02447 0.03361 = 0.03683 -0.01376 -0.00846 0.00343 O1' 4 0.502437 0.129798 0.473330 -31.00000 0.03118 0.05739 = 0.04007 0.00179 -0.00206 -0.00774 O2' 4 0.620122 0.210557 0.303103 -31.00000 0.04785 0.03736 = 0.03682 -0.01080 0.00418 0.00227 O3' 4 0.630941 0.312198 0.419935 -31.00000 0.04750 0.06373 = 0.09107 -0.03922 -0.03135 -0.00525 O4' 4 0.422224 0.305891 0.372052 -31.00000 0.03569 0.06435 = 0.06947 -0.03610 -0.02970 0.02603 AFIX 0 PART 0 CL2 5 1.249924 0.771306 0.143928 11.00000 0.05581 0.05408 = 0.03326 -0.01619 -0.00514 -0.00972 O5A 4 1.127964 0.749260 0.223046 11.00000 0.08035 0.20682 = 0.05991 -0.05632 0.01492 -0.01912 O6A 4 1.234966 0.864416 0.056802 11.00000 0.15289 0.08776 = 0.06329 -0.00991 -0.04462 0.02035 O7A 4 1.359266 0.808078 0.175488 11.00000 0.08870 0.08573 = 0.11818 -0.04855 -0.04258 -0.01944 O8A 4 1.282950 0.664715 0.116111 11.00000 0.13023 0.04791 = 0.05565 -0.01967 -0.00610 -0.03043 N1S 3 0.192886 0.510530 0.470066 11.00000 0.05762 0.06654 = 0.10531 -0.05646 0.00167 -0.01764 C1S 1 0.300235 0.549556 0.427909 11.00000 0.05065 0.03713 = 0.05895 -0.02667 -0.01096 -0.00438 C2S 1 0.437738 0.599656 0.376216 11.00000 0.06065 0.06318 = 0.07009 -0.02422 0.00204 -0.01929 AFIX 137 H2S1 2 0.463024 0.654719 0.409601 11.00000 -1.50000 H2S2 2 0.439318 0.644421 0.305857 11.00000 -1.50000 H2S3 2 0.504717 0.534022 0.377911 11.00000 -1.50000 HKLF 4 REM test2 in P-1 REM R1 = 0.0454 for 6193 Fo > 4sig(Fo) and 0.0521 for all 7045 data REM 437 parameters refined using 0 restraints END WGHT 0.0549 1.4054 REM Highest difference peak 0.815, deepest hole -0.608, 1-sigma level 0.074 Q1 1 1.1968 0.7655 0.1135 11.00000 0.05 0.81 Q2 1 1.3093 0.7240 0.1425 11.00000 0.05 0.74 Q3 1 1.1875 0.8052 0.0432 11.00000 0.05 0.64 Q4 1 1.0392 0.2580 0.2594 11.00000 0.05 0.59 Q5 1 1.3136 0.8327 0.1250 11.00000 0.05 0.56 Q6 1 0.9050 0.1698 0.2733 11.00000 0.05 0.56 Q7 1 0.9835 0.1720 0.3277 11.00000 0.05 0.55 Q8 1 0.9539 0.2411 0.2102 11.00000 0.05 0.55 Q9 1 0.9172 0.2567 0.2850 11.00000 0.05 0.51 Q10 1 0.8997 0.2277 0.3017 11.00000 0.05 0.47 Q11 1 0.9382 0.2941 0.2162 11.00000 0.05 0.46 Q12 1 1.1453 0.8417 0.1886 11.00000 0.05 0.43 Q13 1 1.0849 0.1986 0.2240 11.00000 0.05 0.40 Q14 1 1.3579 0.6590 0.1378 11.00000 0.05 0.40 Q15 1 0.7995 0.5643 0.1443 11.00000 0.05 0.38 Q16 1 0.7986 -0.0977 0.2145 11.00000 0.05 0.38 Q17 1 0.6100 0.3016 0.3884 11.00000 0.05 0.38 Q18 1 1.0026 0.2351 0.4457 11.00000 0.05 0.37 Q19 1 1.1742 0.8564 0.0992 11.00000 0.05 0.36 Q20 1 0.9981 0.3765 0.3015 11.00000 0.05 0.36 ; _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^)+(0.0549P)^2^+1.4009P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7045 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.97368(3) 0.20966(2) 0.26587(2) 0.02350(9) Uani 1 1 d . . . N1 N 1.0556(2) 0.34239(18) 0.31495(16) 0.0275(4) Uani 1 1 d . . . C1 C 1.0596(3) 0.2853(2) 0.42081(19) 0.0305(5) Uani 1 1 d . . . H1A H 1.0504 0.3482 0.4556 0.037 Uiso 1 1 calc R . . H1B H 1.1508 0.2466 0.4233 0.037 Uiso 1 1 calc R . . N2 N 0.9070(2) 0.12837(17) 0.41908(15) 0.0230(4) Uani 1 1 d . . . C2 C 0.9443(2) 0.1911(2) 0.47536(18) 0.0253(5) Uani 1 1 d . . . C3 C 0.8840(3) 0.1679(2) 0.57668(19) 0.0303(5) Uani 1 1 d . . . H3A H 0.9105 0.2140 0.6142 0.036 Uiso 1 1 calc R . . C4 C 0.7836(3) 0.0755(2) 0.62325(19) 0.0327(5) Uani 1 1 d . . . H4A H 0.7400 0.0582 0.6932 0.039 Uiso 1 1 calc R . . C5 C 0.7475(3) 0.0093(2) 0.56770(19) 0.0294(5) Uani 1 1 d . . . H5A H 0.6806 -0.0554 0.5988 0.035 Uiso 1 1 calc R . . C6 C 0.8114(2) 0.0391(2) 0.46460(18) 0.0234(4) Uani 1 1 d . . . N7 N 0.7727(2) -0.02916(18) 0.40898(16) 0.0252(4) Uani 1 1 d . . . H7N H 0.705(3) -0.073(3) 0.442(2) 0.030(8) Uiso 1 1 d . . . O8 O 0.89496(18) 0.06314(15) 0.24681(12) 0.0278(4) Uani 1 1 d . . . C8 C 0.8105(2) -0.0165(2) 0.30876(18) 0.0243(5) Uani 1 1 d . . . C9 C 0.7436(3) -0.1053(2) 0.2726(2) 0.0298(5) Uani 1 1 d . . . C10B C 0.8117(4) -0.0877(3) 0.1609(2) 0.0491(8) Uani 1 1 d . . . H10A H 0.9115 -0.1039 0.1522 0.074 Uiso 1 1 calc R . . H10B H 0.7992 -0.0041 0.1216 0.074 Uiso 1 1 calc R . . H10C H 0.7679 -0.1436 0.1372 0.074 Uiso 1 1 calc R . . C10A C 0.5872(3) -0.0791(3) 0.2880(3) 0.0545(9) Uani 1 1 d . . . H10D H 0.5452 -0.0901 0.3598 0.082 Uiso 1 1 calc R . . H10E H 0.5419 -0.1350 0.2651 0.082 Uiso 1 1 calc R . . H10F H 0.5747 0.0045 0.2488 0.082 Uiso 1 1 calc R . . C11 C 1.1946(3) 0.3814(3) 0.2473(2) 0.0363(6) Uani 1 1 d . . . H11A H 1.2570 0.3953 0.2873 0.044 Uiso 1 1 calc R . . H11B H 1.1863 0.4593 0.1961 0.044 Uiso 1 1 calc R . . N12 N 1.1759(2) 0.20598(19) 0.18900(16) 0.0285(4) Uani 1 1 d . A . C12 C 1.2597(3) 0.2903(2) 0.19394(18) 0.0309(5) Uani 1 1 d . . . C13 C 1.4005(3) 0.2968(3) 0.1475(2) 0.0461(7) Uani 1 1 d . . . H13A H 1.4595 0.3561 0.1517 0.055 Uiso 1 1 calc R . . C14 C 1.4538(3) 0.2157(4) 0.0950(3) 0.0568(9) Uani 1 1 d . . . H14A H 1.5506 0.2183 0.0636 0.068 Uiso 1 1 calc R . . C15 C 1.3690(3) 0.1323(3) 0.0879(2) 0.0484(8) Uani 1 1 d . A . H15A H 1.4051 0.0774 0.0506 0.058 Uiso 1 1 calc R . . C16 C 1.2292(3) 0.1287(2) 0.1359(2) 0.0361(6) Uani 1 1 d . . . H16A H 1.1692 0.0704 0.1314 0.043 Uiso 0.774(7) 1 calc PR A 1 C21 C 0.9543(3) 0.4410(2) 0.3038(2) 0.0325(5) Uani 1 1 d . . . H21A H 0.9985 0.5170 0.3011 0.039 Uiso 1 1 calc R . . H21B H 0.8733 0.4208 0.3631 0.039 Uiso 1 1 calc R . . N22 N 0.8899(2) 0.35780(18) 0.18438(15) 0.0275(4) Uani 1 1 d . A . C22 C 0.9056(3) 0.4594(2) 0.20892(19) 0.0318(5) Uani 1 1 d . . . C23 C 0.8750(4) 0.5720(3) 0.1527(2) 0.0474(8) Uani 1 1 d . . . H23A H 0.8918 0.6428 0.1689 0.057 Uiso 1 1 calc R . . C24 C 0.8188(4) 0.5793(3) 0.0715(2) 0.0572(9) Uani 1 1 d . . . H24A H 0.7933 0.6558 0.0329 0.069 Uiso 1 1 calc R . . C25 C 0.8000(4) 0.4779(3) 0.0469(2) 0.0506(8) Uani 1 1 d . A . H25A H 0.7607 0.4830 -0.0084 0.061 Uiso 1 1 calc R . . C26 C 0.8391(3) 0.3661(3) 0.10368(19) 0.0355(6) Uani 1 1 d . . . H26E H 0.8297 0.2954 0.0852 0.043 Uiso 0.226(7) 1 calc PR A 2 N27 N 0.8355(4) 0.2667(3) 0.0778(2) 0.0426(10) Uani 0.774(7) 1 d P A 1 H27A H 0.8657 0.1984 0.1128 0.051 Uiso 0.774(7) 1 calc PR A 1 H27B H 0.8030 0.2686 0.0255 0.051 Uiso 0.774(7) 1 calc PR A 1 N27' N 1.1535(12) 0.0644(10) 0.1078(8) 0.042(3) Uiso 0.226(7) 1 d P A 2 H27C H 1.0620 0.0698 0.1232 0.050 Uiso 0.226(7) 1 calc PR A 2 H27D H 1.1933 0.0152 0.0732 0.050 Uiso 0.226(7) 1 calc PR A 2 C10C C 0.7654(3) -0.2353(2) 0.3334(2) 0.0328(5) Uani 1 1 d . . . H10G H 0.7224 -0.2471 0.4052 0.049 Uiso 1 1 calc R . . H10H H 0.8655 -0.2504 0.3241 0.049 Uiso 1 1 calc R . . H10I H 0.7222 -0.2919 0.3100 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.5487(2) 0.2690(2) 0.3715(2) 0.0262(4) Uani 0.585(3) 1 d PG B 1 O1A O 0.4112(3) 0.2295(3) 0.4300(2) 0.0491(10) Uani 0.585(3) 1 d PG B 1 O2A O 0.5425(3) 0.3817(3) 0.2965(2) 0.0464(10) Uani 0.585(3) 1 d PG B 1 O3A O 0.6100(7) 0.1808(3) 0.3236(4) 0.0524(18) Uani 0.585(3) 1 d PG B 1 O4A O 0.6312(6) 0.2841(6) 0.4358(4) 0.0514(16) Uani 0.585(3) 1 d PG B 1 Cl1' Cl 0.5439(3) 0.2396(3) 0.3921(3) 0.0308(7) Uani 0.415(3) 1 d PG B 2 O1' O 0.5024(4) 0.1298(4) 0.4733(3) 0.0475(14) Uani 0.415(3) 1 d PG B 2 O2' O 0.6201(10) 0.2106(7) 0.3031(5) 0.043(2) Uani 0.415(3) 1 d PG B 2 O3' O 0.6309(9) 0.3122(5) 0.4199(8) 0.061(3) Uani 0.415(3) 1 d PG B 2 O4' O 0.4222(5) 0.3059(4) 0.3721(4) 0.0507(16) Uani 0.415(3) 1 d PG B 2 Cl2 Cl 1.24992(9) 0.77131(7) 0.14393(5) 0.04763(19) Uani 1 1 d . . . O5A O 1.1280(4) 0.7493(5) 0.2230(2) 0.1170(15) Uani 1 1 d . . . O6A O 1.2350(5) 0.8644(3) 0.0568(2) 0.1016(12) Uani 1 1 d . . . O7A O 1.3593(4) 0.8081(3) 0.1755(3) 0.0893(10) Uani 1 1 d . . . O8A O 1.2829(4) 0.6647(2) 0.1161(2) 0.0788(9) Uani 1 1 d . . . N1S N 0.1929(4) 0.5105(3) 0.4701(3) 0.0727(10) Uani 1 1 d . . . C1S C 0.3002(4) 0.5496(3) 0.4279(3) 0.0463(7) Uani 1 1 d . . . C2S C 0.4377(4) 0.5997(4) 0.3762(3) 0.0662(10) Uani 1 1 d . . . H2S1 H 0.4630 0.6547 0.4096 0.099 Uiso 1 1 calc R . . H2S2 H 0.4393 0.6444 0.3059 0.099 Uiso 1 1 calc R . . H2S3 H 0.5047 0.5340 0.3779 0.099 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 0.02362(14) 0.02134(14) 0.02741(15) -0.01023(11) -0.00540(11) -0.00220(10) N1 0.0282(10) 0.0254(10) 0.0307(10) -0.0120(8) -0.0052(8) -0.0031(8) C1 0.0308(13) 0.0313(13) 0.0348(13) -0.0153(11) -0.0101(10) -0.0038(10) N2 0.0209(9) 0.0241(9) 0.0265(10) -0.0101(8) -0.0073(8) 0.0018(7) C2 0.0235(11) 0.0260(11) 0.0309(12) -0.0125(10) -0.0106(9) 0.0037(9) C3 0.0330(13) 0.0334(13) 0.0306(12) -0.0155(10) -0.0132(10) 0.0072(10) C4 0.0337(13) 0.0379(14) 0.0255(12) -0.0096(10) -0.0064(10) 0.0056(11) C5 0.0286(12) 0.0280(12) 0.0290(12) -0.0056(10) -0.0061(10) 0.0007(9) C6 0.0213(11) 0.0223(11) 0.0282(11) -0.0096(9) -0.0074(9) 0.0037(8) N7 0.0223(10) 0.0239(10) 0.0296(10) -0.0085(8) -0.0052(8) -0.0041(8) O8 0.0311(9) 0.0257(8) 0.0275(8) -0.0127(7) -0.0016(7) -0.0069(7) C8 0.0220(11) 0.0227(11) 0.0304(12) -0.0106(9) -0.0075(9) 0.0021(8) C9 0.0311(13) 0.0255(12) 0.0356(13) -0.0105(10) -0.0105(10) -0.0053(10) C10B 0.083(2) 0.0369(15) 0.0330(14) -0.0116(12) -0.0176(15) -0.0192(15) C10A 0.0394(16) 0.0422(17) 0.104(3) -0.0372(19) -0.0395(18) 0.0064(13) C11 0.0334(14) 0.0362(14) 0.0405(15) -0.0146(12) -0.0045(11) -0.0125(11) N12 0.0269(10) 0.0272(10) 0.0306(11) -0.0100(8) -0.0045(8) 0.0022(8) C12 0.0272(12) 0.0379(14) 0.0248(12) -0.0042(10) -0.0068(10) -0.0032(10) C13 0.0283(14) 0.066(2) 0.0379(15) -0.0087(14) -0.0033(12) -0.0104(13) C14 0.0296(15) 0.084(3) 0.0481(19) -0.0180(18) 0.0036(13) 0.0066(16) C15 0.0473(18) 0.0535(19) 0.0361(15) -0.0142(14) 0.0023(13) 0.0185(15) C16 0.0395(15) 0.0324(13) 0.0357(14) -0.0120(11) -0.0074(12) 0.0106(11) C21 0.0409(14) 0.0235(12) 0.0352(13) -0.0133(10) -0.0076(11) 0.0019(10) N22 0.0301(10) 0.0272(10) 0.0230(10) -0.0059(8) -0.0044(8) 0.0011(8) C22 0.0359(13) 0.0271(12) 0.0283(12) -0.0084(10) -0.0009(10) 0.0046(10) C23 0.070(2) 0.0305(14) 0.0364(15) -0.0091(12) -0.0074(14) 0.0132(14) C24 0.082(3) 0.0445(18) 0.0366(16) -0.0020(14) -0.0180(17) 0.0265(17) C25 0.061(2) 0.057(2) 0.0301(14) -0.0064(14) -0.0162(14) 0.0155(16) C26 0.0391(14) 0.0396(14) 0.0257(12) -0.0075(11) -0.0065(11) 0.0004(11) N27 0.057(2) 0.0440(19) 0.0324(16) -0.0096(13) -0.0211(15) -0.0111(15) C10C 0.0370(14) 0.0242(12) 0.0393(14) -0.0114(10) -0.0099(11) -0.0029(10) Cl1 0.0251(7) 0.0242(10) 0.0300(10) -0.0089(7) -0.0068(6) 0.0006(6) O1A 0.034(2) 0.056(2) 0.048(2) -0.0053(19) -0.0031(17) -0.0096(17) O2A 0.056(2) 0.0289(17) 0.046(2) -0.0007(15) -0.0105(17) 0.0014(16) O3A 0.068(4) 0.039(3) 0.057(3) -0.027(2) -0.015(3) 0.021(3) O4A 0.047(4) 0.057(3) 0.065(4) -0.026(3) -0.031(3) 0.004(2) Cl1' 0.0245(10) 0.0336(18) 0.0368(18) -0.0138(12) -0.0085(9) 0.0034(10) O1' 0.031(3) 0.057(3) 0.040(3) 0.002(2) -0.002(2) -0.008(2) O2' 0.048(4) 0.037(3) 0.037(3) -0.011(3) 0.004(3) 0.002(3) O3' 0.047(6) 0.064(5) 0.091(7) -0.039(4) -0.031(5) -0.005(4) O4' 0.036(3) 0.064(4) 0.069(4) -0.036(3) -0.030(3) 0.026(3) Cl2 0.0558(5) 0.0541(4) 0.0333(3) -0.0162(3) -0.0051(3) -0.0097(4) O5A 0.080(2) 0.207(5) 0.0599(19) -0.056(3) 0.0149(17) -0.019(3) O6A 0.153(4) 0.088(2) 0.0633(19) -0.0099(17) -0.045(2) 0.020(2) O7A 0.089(2) 0.086(2) 0.118(3) -0.049(2) -0.043(2) -0.0194(17) O8A 0.130(3) 0.0479(14) 0.0557(16) -0.0197(12) -0.0061(16) -0.0304(16) N1S 0.058(2) 0.067(2) 0.105(3) -0.056(2) 0.0017(19) -0.0176(16) C1S 0.0506(18) 0.0371(15) 0.0590(19) -0.0267(14) -0.0110(15) -0.0044(13) C2S 0.061(2) 0.063(2) 0.070(2) -0.024(2) 0.0020(19) -0.0193(19) _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 O8 2.0236(16) . ? Zn N22 2.026(2) . ? Zn N12 2.035(2) . ? Zn N2 2.057(2) . ? Zn N1 2.143(2) . ? N1 C1 1.468(3) . ? N1 C11 1.475(3) . ? N1 C21 1.477(3) . ? C1 C2 1.509(3) . ? N2 C6 1.335(3) . ? N2 C2 1.359(3) . ? C2 C3 1.372(3) . ? C3 C4 1.390(4) . ? C4 C5 1.376(4) . ? C5 C6 1.396(3) . ? C6 N7 1.405(3) . ? N7 C8 1.354(3) . ? O8 C8 1.247(3) . ? C8 C9 1.528(3) . ? C9 C10C 1.528(3) . ? C9 C10B 1.529(4) . ? C9 C10A 1.536(4) . ? C11 C12 1.511(4) . ? N12 C12 1.344(3) . ? N12 C16 1.350(3) . ? C12 C13 1.382(4) . ? C13 C14 1.381(5) . ? C14 C15 1.357(5) . ? C15 C16 1.380(4) . ? C16 N27' 1.293(11) . ? C21 C22 1.505(4) . ? N22 C26 1.347(3) . ? N22 C22 1.353(3) . ? C22 C23 1.372(4) . ? C23 C24 1.387(5) . ? C24 C25 1.360(5) . ? C25 C26 1.397(4) . ? C26 N27 1.317(4) . ? Cl1 O2A 1.426(2) . ? Cl1 O3A 1.426(2) . ? Cl1 O4A 1.426(2) . ? Cl1 O1A 1.426(2) . ? Cl1' O3' 1.436(3) . ? Cl1' O4' 1.436(3) . ? Cl1' O2' 1.436(3) . ? Cl1' O1' 1.436(3) . ? Cl2 O7A 1.403(3) . ? Cl2 O8A 1.407(3) . ? Cl2 O5A 1.409(3) . ? Cl2 O6A 1.414(3) . ? N1S C1S 1.125(4) . ? C1S C2S 1.436(5) . ? 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 O8 Zn N22 107.06(8) . . ? O8 Zn N12 100.10(8) . . ? N22 Zn N12 106.50(8) . . ? O8 Zn N2 87.50(7) . . ? N22 Zn N2 125.73(8) . . ? N12 Zn N2 122.31(8) . . ? O8 Zn N1 168.92(7) . . ? N22 Zn N1 82.13(8) . . ? N12 Zn N1 82.70(8) . . ? N2 Zn N1 82.01(8) . . ? C1 N1 C11 113.1(2) . . ? C1 N1 C21 112.3(2) . . ? C11 N1 C21 112.1(2) . . ? C1 N1 Zn 107.26(14) . . ? C11 N1 Zn 107.55(15) . . ? C21 N1 Zn 103.91(15) . . ? N1 C1 C2 111.66(19) . . ? C6 N2 C2 118.8(2) . . ? C6 N2 Zn 126.05(16) . . ? C2 N2 Zn 113.58(16) . . ? N2 C2 C3 122.2(2) . . ? N2 C2 C1 116.1(2) . . ? C3 C2 C1 121.7(2) . . ? C2 C3 C4 118.7(2) . . ? C5 C4 C3 119.8(2) . . ? C4 C5 C6 118.5(2) . . ? N2 C6 C5 122.1(2) . . ? N2 C6 N7 120.2(2) . . ? C5 C6 N7 117.7(2) . . ? C8 N7 C6 130.5(2) . . ? C8 O8 Zn 129.23(15) . . ? O8 C8 N7 123.2(2) . . ? O8 C8 C9 120.0(2) . . ? N7 C8 C9 116.7(2) . . ? C8 C9 C10C 109.8(2) . . ? C8 C9 C10B 109.3(2) . . ? C10C C9 C10B 109.1(2) . . ? C8 C9 C10A 107.9(2) . . ? C10C C9 C10A 110.3(2) . . ? C10B C9 C10A 110.4(3) . . ? N1 C11 C12 113.1(2) . . ? C12 N12 C16 119.6(2) . . ? C12 N12 Zn 114.31(17) . . ? C16 N12 Zn 126.12(18) . . ? N12 C12 C13 120.9(3) . . ? N12 C12 C11 118.2(2) . . ? C13 C12 C11 120.9(3) . . ? C14 C13 C12 118.8(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 118.7(3) . . ? N27' C16 N12 123.5(6) . . ? N27' C16 C15 113.4(6) . . ? N12 C16 C15 121.6(3) . . ? N1 C21 C22 110.5(2) . . ? C26 N22 C22 119.3(2) . . ? C26 N22 Zn 126.63(18) . . ? C22 N22 Zn 113.46(17) . . ? N22 C22 C23 122.3(3) . . ? N22 C22 C21 115.9(2) . . ? C23 C22 C21 121.8(3) . . ? C22 C23 C24 117.9(3) . . ? C25 C24 C23 120.5(3) . . ? C24 C25 C26 119.2(3) . . ? N27 C26 N22 117.4(3) . . ? N27 C26 C25 121.9(3) . . ? N22 C26 C25 120.6(3) . . ? O2A Cl1 O3A 109.5 . . ? O2A Cl1 O4A 109.5 . . ? O3A Cl1 O4A 109.5 . . ? O2A Cl1 O1A 109.5 . . ? O3A Cl1 O1A 109.5 . . ? O4A Cl1 O1A 109.5 . . ? O3' Cl1' O4' 109.5 . . ? O3' Cl1' O2' 109.5 . . ? O4' Cl1' O2' 109.5 . . ? O3' Cl1' O1' 109.5 . . ? O4' Cl1' O1' 109.5 . . ? O2' Cl1' O1' 109.5 . . ? O7A Cl2 O8A 111.0(2) . . ? O7A Cl2 O5A 109.7(2) . . ? O8A Cl2 O5A 108.7(2) . . ? O7A Cl2 O6A 106.7(2) . . ? O8A Cl2 O6A 107.7(2) . . ? O5A Cl2 O6A 113.0(3) . . ? N1S C1S C2S 178.7(4) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.815 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.074 #===END data_r83168 _database_code_depnum_ccdc_archive 'CCDC 250154' # Referred to as 3(ClO4)2CH3CN in manuscript # Checkcif output and final .res file under refine special details _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 N7 O Zn, 2(Cl O4), C2 H3 N' _chemical_formula_sum 'C25 H32 Cl2 N8 O9 Zn' _chemical_formula_weight 724.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0798(2) _cell_length_b 11.7300(3) _cell_length_c 14.2630(3) _cell_angle_alpha 71.3770(10) _cell_angle_beta 75.0580(10) _cell_angle_gamma 87.7060(10) _cell_volume 1542.42(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5258 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Smart APEX CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18392 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.88 _reflns_number_total 7310 _reflns_number_gt 6742 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? H positions were mostly calculated. 430_ALERT_2_B Short Inter D...A Contact O7B .. O7B .. 2.72 Ang. These atoms are part weight, being part of a disordered perchlorate. 911_ALERT_3_B Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 23 912_ALERT_3_B Missing FCF Reflections Above STH/L=0.6 ........ 791 #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 3231 3230 1 23.01 0.550 0.999 4295 4292 3 25.24 0.600 0.996 5569 5546 23 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.985 7104 6996 108 29.84 0.700 0.900 8124 7310 814 No problems here. 165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 10 One perchlorate is disordered over two sites and orientations; these were modelled as two intersecting variable-metric rigid groups. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.64 Ratio 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl2 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C1S 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for Cl1 302_ALERT_4_C Anion/Solvent Disorder ......................... 28.00 Perc. 432_ALERT_2_C Short Inter X...Y Contact O7A .. C8 .. 2.95 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3 Noted, but no action taken. #TITL R83168 in P-1 CELL 0.71073 10.0798 11.7300 14.2630 71.377 75.058 87.706 ZERR 2 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H Cl N O Zn UNIT 50 64 4 16 18 2 TEMP -123 OMIT 0 1 1 L.S. 6 ACTA RTAB D1 N17 O8 RTAB D2 N27 O8 FMAP 2 PLAN 10 HTAB WGHT 0.041500 0.847900 FVAR 0.17987 0.54928 ZN 6 0.023125 0.283211 0.732998 11.00000 0.01920 0.01675 = 0.01696 -0.00657 -0.00476 -0.00085 O8 5 0.110371 0.426909 0.750475 11.00000 0.02664 0.02133 = 0.01952 -0.00889 -0.00369 -0.00476 N1 4 -0.055131 0.159099 0.677883 11.00000 0.02284 0.01803 = 0.01952 -0.00615 -0.00665 -0.00114 C1 1 -0.060036 0.221980 0.571387 11.00000 0.02677 0.02429 = 0.02103 -0.00735 -0.01042 -0.00275 AFIX 23 H1A 2 -0.148883 0.261097 0.571208 11.00000 -1.20000 H1B 2 -0.053576 0.162852 0.534202 11.00000 -1.20000 AFIX 0 N2 4 0.093484 0.373785 0.575790 11.00000 0.01854 0.01855 = 0.01882 -0.00741 -0.00650 0.00102 C2 1 0.056634 0.316051 0.517329 11.00000 0.02318 0.01953 = 0.02026 -0.00738 -0.00981 0.00265 C3 1 0.117918 0.342943 0.413972 11.00000 0.03030 0.02582 = 0.02085 -0.00967 -0.01132 0.00353 AFIX 43 H3A 2 0.091117 0.299759 0.375191 11.00000 -1.20000 AFIX 0 C4 1 0.219936 0.434808 0.367789 11.00000 0.03029 0.02762 = 0.01670 -0.00519 -0.00533 0.00399 AFIX 43 H4A 2 0.264295 0.454637 0.296850 11.00000 -1.20000 AFIX 0 C5 1 0.256186 0.496705 0.425348 11.00000 0.02385 0.02102 = 0.02043 -0.00303 -0.00501 0.00064 AFIX 43 H5A 2 0.323774 0.561100 0.394707 11.00000 -1.20000 AFIX 0 C6 1 0.191237 0.462604 0.529917 11.00000 0.01850 0.01890 = 0.02045 -0.00707 -0.00707 0.00343 N7 4 0.230990 0.526979 0.587001 11.00000 0.01951 0.02073 = 0.02152 -0.00690 -0.00322 -0.00481 H7A 2 0.293874 0.573706 0.554178 11.00000 0.02665 C8 1 0.193228 0.510219 0.688157 11.00000 0.01860 0.02068 = 0.02238 -0.00890 -0.00642 0.00163 C9 1 0.255802 0.598232 0.725960 11.00000 0.02679 0.02180 = 0.02732 -0.01050 -0.01035 -0.00227 C10A 1 0.408343 0.570902 0.716171 11.00000 0.03672 0.04357 = 0.09487 -0.04263 -0.03951 0.01208 AFIX 33 H10A 2 0.415927 0.487659 0.757966 11.00000 -1.50000 H10B 2 0.451405 0.626024 0.739975 11.00000 -1.50000 H10C 2 0.454906 0.581608 0.644336 11.00000 -1.50000 AFIX 0 C10B 1 0.181038 0.581012 0.837716 11.00000 0.07163 0.03075 = 0.02264 -0.00971 -0.01202 -0.01566 AFIX 33 H10D 2 0.083902 0.598095 0.842993 11.00000 -1.50000 H10E 2 0.222764 0.636148 0.862279 11.00000 -1.50000 H10F 2 0.188516 0.497753 0.879524 11.00000 -1.50000 AFIX 0 C10C 1 0.240473 0.728151 0.661788 11.00000 0.03361 0.02034 = 0.02906 -0.00966 -0.00630 -0.00344 AFIX 33 H10G 2 0.142695 0.743907 0.669387 11.00000 -1.50000 H10H 2 0.285805 0.739876 0.589576 11.00000 -1.50000 H10I 2 0.283113 0.783773 0.685354 11.00000 -1.50000 AFIX 0 C11 1 -0.191739 0.113824 0.746924 11.00000 0.02673 0.02558 = 0.02720 -0.00826 -0.00640 -0.00751 AFIX 23 H11A 2 -0.182055 0.036803 0.799066 11.00000 -1.20000 H11B 2 -0.251290 0.097479 0.706840 11.00000 -1.20000 AFIX 0 N12 4 -0.178319 0.280236 0.814576 11.00000 0.02230 0.02077 = 0.01709 -0.00351 -0.00445 0.00141 C12 1 -0.260349 0.201431 0.800472 11.00000 0.02355 0.03007 = 0.01768 -0.00359 -0.00570 -0.00210 C13 1 -0.400563 0.193800 0.839170 11.00000 0.02268 0.06054 = 0.03024 -0.01334 -0.00487 -0.00821 AFIX 43 H13A 2 -0.456289 0.138579 0.827941 11.00000 -1.20000 AFIX 0 C14 1 -0.458889 0.269534 0.895501 11.00000 0.02163 0.08050 = 0.03774 -0.02188 -0.00096 0.00565 AFIX 43 H14A 2 -0.555850 0.267360 0.921521 11.00000 -1.20000 AFIX 0 C15 1 -0.378792 0.346011 0.913440 11.00000 0.03050 0.05044 = 0.02859 -0.01480 -0.00138 0.01144 AFIX 43 H15A 2 -0.418569 0.396067 0.953137 11.00000 -1.20000 AFIX 0 C16 1 -0.235939 0.350083 0.872375 11.00000 0.02970 0.02609 = 0.01681 -0.00325 -0.00405 0.00699 N17 4 -0.153117 0.421369 0.892121 11.00000 0.03631 0.02883 = 0.03327 -0.01793 0.00158 0.00195 H17A 2 -0.072923 0.434644 0.859918 11.00000 0.03674 H17B 2 -0.182954 0.473447 0.913764 11.00000 0.03298 C21 1 0.045311 0.062970 0.683809 11.00000 0.03218 0.01927 = 0.02309 -0.01026 -0.00919 0.00254 AFIX 23 H21A 2 0.126323 0.089205 0.624152 11.00000 -1.20000 H21B 2 0.002909 -0.010708 0.681971 11.00000 -1.20000 AFIX 0 N22 4 0.107503 0.133037 0.810121 11.00000 0.02040 0.02167 = 0.01758 -0.00589 -0.00503 0.00052 C22 1 0.089975 0.035853 0.781451 11.00000 0.02430 0.02269 = 0.02108 -0.00798 -0.00426 0.00265 C23 1 0.113342 -0.079301 0.836103 11.00000 0.04231 0.02311 = 0.02980 -0.00910 -0.00864 0.00717 AFIX 43 H23A 2 0.095184 -0.146234 0.816725 11.00000 -1.20000 AFIX 0 C24 1 0.164949 -0.094712 0.921534 11.00000 0.05117 0.03031 = 0.03001 -0.00350 -0.01367 0.01566 AFIX 43 H24A 2 0.184095 -0.173071 0.960126 11.00000 -1.20000 AFIX 0 C25 1 0.187707 0.001518 0.949422 11.00000 0.03699 0.04157 = 0.02237 -0.00502 -0.01246 0.00970 AFIX 43 H25A 2 0.224800 -0.008840 1.006299 11.00000 -1.20000 AFIX 0 C26 1 0.155754 0.117187 0.893137 11.00000 0.02066 0.03110 = 0.01903 -0.00611 -0.00413 -0.00055 N27 4 0.168189 0.213753 0.921876 11.00000 0.04081 0.03472 = 0.02322 -0.00830 -0.01514 -0.00408 H27A 2 0.164993 0.281335 0.885140 11.00000 0.03697 H27B 2 0.189084 0.204157 0.973484 11.00000 0.03649 CL1 3 0.254211 0.272370 0.139190 11.00000 0.04138 0.02793 = 0.02321 -0.01140 -0.01015 0.00044 O1A 5 0.357285 0.306309 0.177406 11.00000 0.06023 0.07814 = 0.07975 -0.04223 -0.03076 -0.00991 O2A 5 0.125836 0.259337 0.212604 11.00000 0.05027 0.10414 = 0.05283 -0.04715 0.00680 -0.00895 O3A 5 0.250573 0.365330 0.045206 11.00000 0.13128 0.03518 = 0.03286 -0.01615 -0.02967 0.02948 O4A 5 0.284391 0.163008 0.114775 11.00000 0.06527 0.02241 = 0.03804 -0.01043 -0.01072 0.00027 AFIX 9 PART 1 21 CL2 3 0.444667 0.232352 0.623312 21.00000 0.02218 0.02170 = 0.02547 -0.00749 -0.00521 0.00029 O5A 5 0.585818 0.269493 0.573563 21.00000 0.02584 0.05109 = 0.03611 -0.00866 -0.00224 -0.00774 O6A 5 0.373574 0.232452 0.548400 21.00000 0.04629 0.05659 = 0.05218 -0.01889 -0.02728 0.00120 O7A 5 0.382840 0.313951 0.676382 21.00000 0.05191 0.03395 = 0.04801 -0.02219 -0.00972 0.01617 O8A 5 0.436434 0.113516 0.694906 21.00000 0.04890 0.02322 = 0.04461 0.00073 -0.00885 -0.00398 AFIX 9 PART 2 -21 CL2B 3 0.453108 0.263938 0.603611 -21.00000 0.02124 0.02856 = 0.02845 -0.01061 -0.00618 0.00190 O5B 5 0.381299 0.283983 0.697988 -21.00000 0.03599 0.03499 = 0.03004 -0.00864 0.00044 0.00512 O6B 5 0.573178 0.196707 0.618022 -21.00000 0.03524 0.05070 = 0.04039 -0.02141 -0.01713 0.02086 O7B 5 0.494271 0.378164 0.524548 -21.00000 0.02662 0.04050 = 0.03420 -0.00049 -0.00162 -0.00290 O8B 5 0.363686 0.196898 0.573886 -21.00000 0.04078 0.05396 = 0.06462 -0.03164 -0.01820 -0.01100 AFIX 0 PART 0 N1S 4 0.192142 0.018889 0.455745 11.00000 0.05732 0.08529 = 0.09452 -0.06575 0.01122 -0.02703 C1S 1 0.301251 0.054119 0.419203 11.00000 0.05142 0.03693 = 0.04614 -0.02372 -0.00823 -0.00812 C2S 1 0.441144 0.100349 0.372499 11.00000 0.05208 0.06502 = 0.06242 -0.02210 -0.00329 -0.02116 AFIX 137 H2S1 2 0.460957 0.160629 0.401942 11.00000 -1.50000 H2S2 2 0.454122 0.137649 0.298523 11.00000 -1.50000 H2S3 2 0.503586 0.034241 0.385239 11.00000 -1.50000 HKLF 4 1 REM R83168 in P-1 REM R1 = 0.0349 for 6742 Fo > 4sig(Fo) and 0.0383 for all 7310 data REM 457 parameters refined using 0 restraints END WGHT 0.0414 0.8476 REM Highest difference peak 0.612, deepest hole -0.388, 1-sigma level 0.068 Q1 1 0.1589 0.3442 0.0761 11.00000 0.05 0.61 Q2 1 0.0134 0.2586 0.5421 11.00000 0.05 0.40 Q3 1 0.0625 0.2128 0.7738 11.00000 0.05 0.39 Q4 1 -0.2222 0.1627 0.7736 11.00000 0.05 0.38 Q5 1 0.0755 0.0430 0.7316 11.00000 0.05 0.36 Q6 1 0.1239 0.4258 0.5581 11.00000 0.05 0.35 Q7 1 0.2785 0.2141 0.1263 11.00000 0.05 0.34 Q8 1 0.3339 0.3337 0.1302 11.00000 0.05 0.34 Q9 1 0.6036 0.2204 0.6111 11.00000 0.05 0.34 Q10 1 -0.0577 0.1877 0.6319 11.00000 0.05 0.33 ; _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^)+(0.0415P)^2^+0.8479P] 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 riding/refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7310 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.005 _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 0.023125(19) 0.283211(17) 0.732998(14) 0.01728(7) Uani 1 1 d . . . O8 O 0.11037(13) 0.42691(11) 0.75048(9) 0.0222(3) Uani 1 1 d . . . N1 N -0.05513(15) 0.15910(13) 0.67788(11) 0.0198(3) Uani 1 1 d . . . C1 C -0.06004(19) 0.22198(17) 0.57139(13) 0.0231(4) Uani 1 1 d . . . H1A H -0.1489 0.2611 0.5712 0.028 Uiso 1 1 calc R . . H1B H -0.0536 0.1629 0.5342 0.028 Uiso 1 1 calc R . . N2 N 0.09348(14) 0.37378(13) 0.57579(11) 0.0180(3) Uani 1 1 d . . . C2 C 0.05663(18) 0.31605(16) 0.51733(13) 0.0200(3) Uani 1 1 d . . . C3 C 0.11792(19) 0.34294(17) 0.41397(14) 0.0243(4) Uani 1 1 d . . . H3A H 0.0911 0.2998 0.3752 0.029 Uiso 1 1 calc R . . C4 C 0.2199(2) 0.43481(17) 0.36779(14) 0.0256(4) Uani 1 1 d . . . H4A H 0.2643 0.4546 0.2968 0.031 Uiso 1 1 calc R . . C5 C 0.25619(19) 0.49671(16) 0.42535(13) 0.0228(4) Uani 1 1 d . . . H5A H 0.3238 0.5611 0.3947 0.027 Uiso 1 1 calc R . . C6 C 0.19124(17) 0.46260(15) 0.52992(13) 0.0188(3) Uani 1 1 d . . . N7 N 0.23099(16) 0.52698(14) 0.58700(12) 0.0208(3) Uani 1 1 d . . . H7A H 0.294(2) 0.574(2) 0.5542(18) 0.027(6) Uiso 1 1 d . . . C8 C 0.19323(17) 0.51022(16) 0.68816(13) 0.0199(3) Uani 1 1 d . . . C9 C 0.25580(19) 0.59823(16) 0.72596(14) 0.0239(4) Uani 1 1 d . . . C10A C 0.4083(2) 0.5709(2) 0.7162(2) 0.0493(7) Uani 1 1 d . . . H10A H 0.4159 0.4877 0.7580 0.074 Uiso 1 1 calc R . . H10B H 0.4514 0.6260 0.7400 0.074 Uiso 1 1 calc R . . H10C H 0.4549 0.5816 0.6443 0.074 Uiso 1 1 calc R . . C10B C 0.1810(3) 0.5810(2) 0.83772(16) 0.0409(6) Uani 1 1 d . . . H10D H 0.0839 0.5981 0.8430 0.061 Uiso 1 1 calc R . . H10E H 0.2228 0.6361 0.8623 0.061 Uiso 1 1 calc R . . H10F H 0.1885 0.4978 0.8795 0.061 Uiso 1 1 calc R . . C10C C 0.2405(2) 0.72815(17) 0.66179(15) 0.0275(4) Uani 1 1 d . . . H10G H 0.1427 0.7439 0.6694 0.041 Uiso 1 1 calc R . . H10H H 0.2858 0.7399 0.5896 0.041 Uiso 1 1 calc R . . H10I H 0.2831 0.7838 0.6854 0.041 Uiso 1 1 calc R . . C11 C -0.1917(2) 0.11382(17) 0.74692(15) 0.0264(4) Uani 1 1 d . . . H11A H -0.1821 0.0368 0.7991 0.032 Uiso 1 1 calc R . . H11B H -0.2513 0.0975 0.7068 0.032 Uiso 1 1 calc R . . N12 N -0.17832(15) 0.28024(13) 0.81458(11) 0.0208(3) Uani 1 1 d . . . C12 C -0.26035(19) 0.20143(18) 0.80047(13) 0.0246(4) Uani 1 1 d . . . C13 C -0.4006(2) 0.1938(2) 0.83917(16) 0.0382(5) Uani 1 1 d . . . H13A H -0.4563 0.1386 0.8279 0.046 Uiso 1 1 calc R . . C14 C -0.4589(2) 0.2695(3) 0.89550(19) 0.0473(6) Uani 1 1 d . . . H14A H -0.5559 0.2674 0.9215 0.057 Uiso 1 1 calc R . . C15 C -0.3788(2) 0.3460(2) 0.91344(16) 0.0375(5) Uani 1 1 d . . . H15A H -0.4186 0.3961 0.9531 0.045 Uiso 1 1 calc R . . C16 C -0.2359(2) 0.35008(17) 0.87238(13) 0.0256(4) Uani 1 1 d . . . N17 N -0.1531(2) 0.42137(17) 0.89212(14) 0.0329(4) Uani 1 1 d . . . H17A H -0.073(3) 0.435(2) 0.860(2) 0.037(7) Uiso 1 1 d . . . H17B H -0.183(3) 0.473(2) 0.9138(19) 0.033(7) Uiso 1 1 d . . . C21 C 0.0453(2) 0.06297(16) 0.68381(14) 0.0236(4) Uani 1 1 d . . . H21A H 0.1263 0.0892 0.6242 0.028 Uiso 1 1 calc R . . H21B H 0.0029 -0.0107 0.6820 0.028 Uiso 1 1 calc R . . N22 N 0.10750(15) 0.13304(13) 0.81012(11) 0.0199(3) Uani 1 1 d . . . C22 C 0.08997(19) 0.03585(16) 0.78145(14) 0.0228(4) Uani 1 1 d . . . C23 C 0.1133(2) -0.07930(18) 0.83610(16) 0.0319(4) Uani 1 1 d . . . H23A H 0.0952 -0.1462 0.8167 0.038 Uiso 1 1 calc R . . C24 C 0.1649(3) -0.0947(2) 0.92153(17) 0.0385(5) Uani 1 1 d . . . H24A H 0.1841 -0.1731 0.9601 0.046 Uiso 1 1 calc R . . C25 C 0.1877(2) 0.0015(2) 0.94942(15) 0.0342(5) Uani 1 1 d . . . H25A H 0.2248 -0.0088 1.0063 0.041 Uiso 1 1 calc R . . C26 C 0.15575(18) 0.11719(18) 0.89314(13) 0.0242(4) Uani 1 1 d . . . N27 N 0.1682(2) 0.21375(18) 0.92188(14) 0.0317(4) Uani 1 1 d . . . H27A H 0.165(3) 0.281(3) 0.885(2) 0.037(7) Uiso 1 1 d . . . H27B H 0.189(3) 0.204(2) 0.973(2) 0.036(7) Uiso 1 1 d . . . Cl1 Cl 0.25421(5) 0.27237(4) 0.13919(3) 0.02967(11) Uani 1 1 d . . . O1A O 0.3573(2) 0.3063(2) 0.17741(18) 0.0657(6) Uani 1 1 d . . . O2A O 0.1258(2) 0.2593(2) 0.21260(16) 0.0672(6) Uani 1 1 d . . . O3A O 0.2506(3) 0.36533(16) 0.04521(13) 0.0643(6) Uani 1 1 d . . . O4A O 0.28439(19) 0.16301(13) 0.11477(12) 0.0422(4) Uani 1 1 d . . . Cl2 Cl 0.44467(19) 0.23235(16) 0.62331(16) 0.0233(4) Uani 0.549(2) 1 d PG A 1 O5A O 0.5858(2) 0.2695(3) 0.5736(2) 0.0398(8) Uani 0.549(2) 1 d PG A 1 O6A O 0.3736(4) 0.2325(4) 0.5484(3) 0.0485(12) Uani 0.549(2) 1 d PG A 1 O7A O 0.3828(5) 0.3140(3) 0.6764(3) 0.0434(12) Uani 0.549(2) 1 d PG A 1 O8A O 0.4364(3) 0.1135(2) 0.69491(19) 0.0422(8) Uani 0.549(2) 1 d PG A 1 Cl2B Cl 0.4531(2) 0.26394(19) 0.6036(2) 0.0258(5) Uani 0.451(2) 1 d PG A 2 O5B O 0.3813(6) 0.2840(4) 0.6980(3) 0.0360(13) Uani 0.451(2) 1 d PG A 2 O6B O 0.5732(3) 0.1967(3) 0.6180(2) 0.0396(9) Uani 0.451(2) 1 d PG A 2 O7B O 0.4943(3) 0.3782(3) 0.5245(2) 0.0377(9) Uani 0.451(2) 1 d PG A 2 O8B O 0.3637(6) 0.1969(3) 0.5739(5) 0.0487(15) Uani 0.451(2) 1 d PG A 2 N1S N 0.1921(3) 0.0189(3) 0.4557(2) 0.0751(9) Uani 1 1 d . . . C1S C 0.3013(3) 0.0541(2) 0.41920(19) 0.0428(5) Uani 1 1 d . . . C2S C 0.4411(3) 0.1003(3) 0.3725(2) 0.0610(8) Uani 1 1 d . . . H2S1 H 0.4610 0.1606 0.4019 0.091 Uiso 1 1 calc R . . H2S2 H 0.4541 0.1376 0.2985 0.091 Uiso 1 1 calc R . . H2S3 H 0.5036 0.0342 0.3852 0.091 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 0.01920(11) 0.01675(11) 0.01696(10) -0.00657(7) -0.00476(7) -0.00085(7) O8 0.0266(6) 0.0213(6) 0.0195(6) -0.0089(5) -0.0037(5) -0.0048(5) N1 0.0228(7) 0.0180(7) 0.0195(7) -0.0062(6) -0.0067(6) -0.0011(5) C1 0.0268(9) 0.0243(9) 0.0210(8) -0.0074(7) -0.0104(7) -0.0028(7) N2 0.0185(7) 0.0186(7) 0.0188(7) -0.0074(5) -0.0065(5) 0.0010(5) C2 0.0232(8) 0.0195(8) 0.0203(8) -0.0074(6) -0.0098(6) 0.0027(6) C3 0.0303(9) 0.0258(9) 0.0208(8) -0.0097(7) -0.0113(7) 0.0035(7) C4 0.0303(9) 0.0276(9) 0.0167(8) -0.0052(7) -0.0053(7) 0.0040(7) C5 0.0239(9) 0.0210(8) 0.0204(8) -0.0030(7) -0.0050(7) 0.0006(7) C6 0.0185(8) 0.0189(8) 0.0204(8) -0.0071(6) -0.0071(6) 0.0034(6) N7 0.0195(7) 0.0207(7) 0.0215(7) -0.0069(6) -0.0032(6) -0.0048(6) C8 0.0186(8) 0.0207(8) 0.0224(8) -0.0089(7) -0.0064(6) 0.0016(6) C9 0.0268(9) 0.0218(9) 0.0273(9) -0.0105(7) -0.0103(7) -0.0023(7) C10A 0.0367(12) 0.0436(13) 0.095(2) -0.0426(14) -0.0395(14) 0.0121(10) C10B 0.0716(16) 0.0308(11) 0.0226(9) -0.0097(8) -0.0120(10) -0.0157(11) C10C 0.0336(10) 0.0203(9) 0.0291(9) -0.0097(7) -0.0063(8) -0.0034(7) C11 0.0267(9) 0.0256(9) 0.0272(9) -0.0083(7) -0.0064(7) -0.0075(7) N12 0.0223(7) 0.0208(7) 0.0171(7) -0.0035(6) -0.0045(5) 0.0014(6) C12 0.0235(9) 0.0301(10) 0.0177(8) -0.0036(7) -0.0057(7) -0.0021(7) C13 0.0227(10) 0.0605(15) 0.0302(10) -0.0133(10) -0.0049(8) -0.0082(9) C14 0.0216(10) 0.0805(19) 0.0377(12) -0.0219(12) -0.0010(9) 0.0056(11) C15 0.0305(11) 0.0504(13) 0.0286(10) -0.0148(10) -0.0014(8) 0.0114(9) C16 0.0297(9) 0.0261(9) 0.0168(8) -0.0033(7) -0.0041(7) 0.0070(7) N17 0.0363(10) 0.0288(9) 0.0333(9) -0.0179(8) 0.0016(8) 0.0020(8) C21 0.0322(10) 0.0193(8) 0.0231(8) -0.0103(7) -0.0092(7) 0.0025(7) N22 0.0204(7) 0.0217(7) 0.0176(7) -0.0059(6) -0.0050(5) 0.0005(5) C22 0.0243(9) 0.0227(9) 0.0211(8) -0.0080(7) -0.0043(7) 0.0027(7) C23 0.0423(11) 0.0231(9) 0.0298(10) -0.0091(8) -0.0086(8) 0.0072(8) C24 0.0512(13) 0.0303(11) 0.0300(10) -0.0035(9) -0.0137(9) 0.0157(10) C25 0.0370(11) 0.0416(12) 0.0224(9) -0.0050(8) -0.0125(8) 0.0097(9) C26 0.0207(8) 0.0311(10) 0.0190(8) -0.0061(7) -0.0041(6) -0.0005(7) N27 0.0408(10) 0.0347(10) 0.0232(8) -0.0083(8) -0.0151(7) -0.0041(8) Cl1 0.0414(3) 0.0279(2) 0.0232(2) -0.01140(18) -0.01015(19) 0.00044(19) O1A 0.0602(13) 0.0781(15) 0.0797(15) -0.0422(12) -0.0308(11) -0.0099(11) O2A 0.0503(11) 0.1041(18) 0.0528(12) -0.0471(12) 0.0068(9) -0.0089(11) O3A 0.131(2) 0.0352(9) 0.0329(9) -0.0161(8) -0.0297(11) 0.0295(11) O4A 0.0653(11) 0.0224(7) 0.0380(8) -0.0104(6) -0.0107(8) 0.0003(7) Cl2 0.0222(6) 0.0217(8) 0.0255(8) -0.0075(6) -0.0052(5) 0.0003(5) O5A 0.0258(14) 0.051(2) 0.0361(16) -0.0087(14) -0.0022(12) -0.0077(13) O6A 0.046(3) 0.057(3) 0.052(3) -0.019(2) -0.027(2) 0.0012(19) O7A 0.052(3) 0.034(2) 0.048(2) -0.0222(18) -0.010(2) 0.0162(18) O8A 0.0489(18) 0.0232(14) 0.0446(17) 0.0007(12) -0.0089(13) -0.0040(12) Cl2B 0.0212(7) 0.0286(12) 0.0285(10) -0.0106(8) -0.0062(6) 0.0019(7) O5B 0.036(2) 0.035(2) 0.030(2) -0.0086(19) 0.0004(17) 0.0051(19) O6B 0.0352(19) 0.051(2) 0.040(2) -0.0214(18) -0.0171(16) 0.0209(18) O7B 0.0266(16) 0.0405(19) 0.0342(18) -0.0005(15) -0.0016(13) -0.0029(14) O8B 0.041(3) 0.054(3) 0.065(4) -0.032(3) -0.018(2) -0.011(2) N1S 0.0573(16) 0.085(2) 0.095(2) -0.0657(18) 0.0112(14) -0.0270(14) C1S 0.0514(14) 0.0369(12) 0.0461(13) -0.0237(11) -0.0082(11) -0.0081(10) C2S 0.0521(16) 0.0650(19) 0.0624(18) -0.0221(15) -0.0033(14) -0.0212(14) _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 N22 2.0399(15) . ? Zn O8 2.0437(12) . ? Zn N12 2.0590(15) . ? Zn N2 2.0924(14) . ? Zn N1 2.1218(15) . ? O8 C8 1.253(2) . ? N1 C11 1.474(2) . ? N1 C1 1.474(2) . ? N1 C21 1.482(2) . ? C1 C2 1.513(2) . ? N2 C6 1.341(2) . ? N2 C2 1.354(2) . ? C2 C3 1.380(2) . ? C3 C4 1.392(3) . ? C4 C5 1.375(3) . ? C5 C6 1.396(2) . ? C6 N7 1.407(2) . ? N7 C8 1.344(2) . ? C8 C9 1.529(2) . ? C9 C10B 1.529(3) . ? C9 C10C 1.532(3) . ? C9 C10A 1.538(3) . ? C11 C12 1.513(3) . ? N12 C16 1.354(2) . ? N12 C12 1.358(2) . ? C12 C13 1.373(3) . ? C13 C14 1.397(4) . ? C14 C15 1.354(4) . ? C15 C16 1.404(3) . ? C16 N17 1.343(3) . ? C21 C22 1.507(2) . ? N22 C26 1.350(2) . ? N22 C22 1.360(2) . ? C22 C23 1.373(3) . ? C23 C24 1.402(3) . ? C24 C25 1.356(3) . ? C25 C26 1.411(3) . ? C26 N27 1.342(3) . ? Cl1 O1A 1.4138(19) . ? Cl1 O2A 1.4174(19) . ? Cl1 O4A 1.4349(16) . ? Cl1 O3A 1.4408(17) . ? Cl2 O6A 1.4315(19) . ? Cl2 O5A 1.4315(19) . ? Cl2 O8A 1.4315(19) . ? Cl2 O7A 1.4315(19) . ? Cl2B O7B 1.441(2) . ? Cl2B O6B 1.441(2) . ? Cl2B O5B 1.441(2) . ? Cl2B O8B 1.441(2) . ? N1S C1S 1.120(3) . ? C1S C2S 1.440(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N22 Zn O8 106.67(6) . . ? N22 Zn N12 107.04(6) . . ? O8 Zn N12 102.85(6) . . ? N22 Zn N2 124.29(6) . . ? O8 Zn N2 85.23(5) . . ? N12 Zn N2 123.33(6) . . ? N22 Zn N1 82.44(6) . . ? O8 Zn N1 166.46(5) . . ? N12 Zn N1 83.43(6) . . ? N2 Zn N1 81.32(6) . . ? C8 O8 Zn 131.66(11) . . ? C11 N1 C1 112.81(14) . . ? C11 N1 C21 111.86(14) . . ? C1 N1 C21 111.73(14) . . ? C11 N1 Zn 107.42(11) . . ? C1 N1 Zn 108.23(11) . . ? C21 N1 Zn 104.26(10) . . ? N1 C1 C2 110.80(14) . . ? C6 N2 C2 118.03(15) . . ? C6 N2 Zn 126.95(12) . . ? C2 N2 Zn 113.20(11) . . ? N2 C2 C3 122.66(17) . . ? N2 C2 C1 115.94(15) . . ? C3 C2 C1 121.37(16) . . ? C2 C3 C4 118.49(17) . . ? C5 C4 C3 119.69(17) . . ? C4 C5 C6 118.38(17) . . ? N2 C6 C5 122.70(16) . . ? N2 C6 N7 120.15(15) . . ? C5 C6 N7 117.14(16) . . ? C8 N7 C6 130.38(16) . . ? O8 C8 N7 122.70(16) . . ? O8 C8 C9 120.15(15) . . ? N7 C8 C9 117.15(15) . . ? C10B C9 C8 109.62(15) . . ? C10B C9 C10C 108.57(16) . . ? C8 C9 C10C 110.09(15) . . ? C10B C9 C10A 110.3(2) . . ? C8 C9 C10A 107.55(15) . . ? C10C C9 C10A 110.73(17) . . ? N1 C11 C12 112.78(15) . . ? C16 N12 C12 118.94(16) . . ? C16 N12 Zn 128.43(13) . . ? C12 N12 Zn 112.49(12) . . ? N12 C12 C13 122.20(19) . . ? N12 C12 C11 117.81(16) . . ? C13 C12 C11 119.83(19) . . ? C12 C13 C14 118.1(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 118.9(2) . . ? N17 C16 N12 118.56(18) . . ? N17 C16 C15 120.37(19) . . ? N12 C16 C15 121.0(2) . . ? N1 C21 C22 109.95(14) . . ? C26 N22 C22 119.04(16) . . ? C26 N22 Zn 127.31(13) . . ? C22 N22 Zn 112.72(11) . . ? N22 C22 C23 122.78(17) . . ? N22 C22 C21 115.46(15) . . ? C23 C22 C21 121.76(18) . . ? C22 C23 C24 117.7(2) . . ? C25 C24 C23 120.43(19) . . ? C24 C25 C26 119.37(19) . . ? N27 C26 N22 118.00(17) . . ? N27 C26 C25 121.40(18) . . ? N22 C26 C25 120.57(18) . . ? O1A Cl1 O2A 109.12(13) . . ? O1A Cl1 O4A 111.73(13) . . ? O2A Cl1 O4A 110.47(13) . . ? O1A Cl1 O3A 108.16(14) . . ? O2A Cl1 O3A 110.40(15) . . ? O4A Cl1 O3A 106.93(10) . . ? O6A Cl2 O5A 109.5 . . ? O6A Cl2 O8A 109.5 . . ? O5A Cl2 O8A 109.5 . . ? O6A Cl2 O7A 109.5 . . ? O5A Cl2 O7A 109.5 . . ? O8A Cl2 O7A 109.5 . . ? O7B Cl2B O6B 109.5 . . ? O7B Cl2B O5B 109.5 . . ? O6B Cl2B O5B 109.5 . . ? O7B Cl2B O8B 109.5 . . ? O6B Cl2B O8B 109.5 . . ? O5B Cl2B O8B 109.5 . . ? N1S C1S C2S 179.5(3) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.612 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.068 #===END data_r4193 _database_code_depnum_ccdc_archive 'CCDC 250155' # Referred to as 5(ClO4)CH3CN in manuscript #Note to referee: final res file and checkcif output are under #_refine_special_details. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[ZnL4L5(ClO4)](ClO4).MeCN' _chemical_formula_sum 'C29 H34 Cl2 N6 O9 S Zn' _chemical_formula_weight 778.95 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' S S 0.1246 0.1234 '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 10.5300(6) _cell_length_b 12.0767(7) _cell_length_c 13.7292(8) _cell_angle_alpha 88.6410(10) _cell_angle_beta 73.0370(10) _cell_angle_gamma 88.0690(10) _cell_volume 1668.83(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7782 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker Smart Apex CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14951 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.78 _reflns_number_total 7775 _reflns_number_gt 6869 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.89 911_ALERT_3_B Missing FCF Refl. Between TH(Min) & STH/L=0.6 .. 48 912_ALERT_3_B Missing FCF Reflections Above STH/L=0.6 ........ 873 The data set is 99.3% complete to 0.84 Ang (2theta=50). 761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? 762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ? These are (mostly) in calculated positions. 242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Cl1 Inspection of a thermal ellipsoid plot does not reveal anything unusual about this atom. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The notation used is intended to correspond to that used in the manuscript. 062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.88 Noted, no action 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.72 The highest peaks are in the region of the perchlorate anion. This may suffer from unmodelled disorder. 125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.35 Ratio 232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn - N31 .. 5.37 su 241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O1A 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C1S 244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 432_ALERT_2_C Short Inter X...Y Contact O7A .. C1 .. 3.01 Ang. 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 35.00 A**3 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 7 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C2 H3 N Noted, no action Final res file: #TITL r4193 in P-1 CELL 0.71073 10.5300 12.0767 13.7292 88.641 73.037 88.069 ZERR 2.00 0.0006 0.0007 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H N O CL ZN S UNIT 58 68 12 18 4 2 2 TEMP -123 L.S. 8 BOND FMAP 2 PLAN 10 ACTA WGHT 0.057900 1.635800 FVAR 0.42814 ZN 6 0.239476 0.748521 0.252594 11.00000 0.01592 0.01978 = 0.02383 -0.00102 -0.00640 0.00267 N1 3 0.140471 0.678858 0.144467 11.00000 0.02025 0.02250 = 0.02191 0.00143 -0.00701 -0.00006 C1 1 0.107153 0.568087 0.191649 11.00000 0.02253 0.02536 = 0.02523 0.00224 -0.00940 -0.00503 AFIX 23 H1A 2 0.076092 0.521351 0.145362 11.00000 -1.20000 H1B 2 0.034646 0.575457 0.256172 11.00000 -1.20000 AFIX 0 C1OB 1 0.575743 0.668995 0.487237 11.00000 0.02543 0.03897 = 0.02630 -0.00062 -0.01102 0.00279 AFIX 33 H1OA 2 0.492319 0.656360 0.540639 11.00000 -1.50000 H1OB 2 0.640911 0.698228 0.517651 11.00000 -1.50000 H1OC 2 0.609971 0.598890 0.453641 11.00000 -1.50000 AFIX 0 N2 3 0.298629 0.581549 0.253436 11.00000 0.02153 0.02075 = 0.02071 0.00021 -0.00787 -0.00046 C2 1 0.228133 0.513982 0.212495 11.00000 0.02455 0.02459 = 0.02020 0.00205 -0.00702 -0.00275 C3 1 0.263727 0.404779 0.191415 11.00000 0.03675 0.02305 = 0.03082 -0.00156 -0.01314 -0.00343 AFIX 43 H3A 2 0.212807 0.359647 0.162105 11.00000 -1.20000 AFIX 0 C4 1 0.376400 0.361858 0.214101 11.00000 0.04312 0.02084 = 0.03302 -0.00344 -0.01252 0.00598 AFIX 43 H4A 2 0.403318 0.286548 0.200412 11.00000 -1.20000 AFIX 0 C5 1 0.448337 0.428745 0.256283 11.00000 0.03116 0.02495 = 0.03020 -0.00212 -0.01198 0.00790 AFIX 43 H5A 2 0.525261 0.400508 0.272298 11.00000 -1.20000 AFIX 0 C6 1 0.406289 0.539358 0.275283 11.00000 0.02234 0.02304 = 0.02027 -0.00096 -0.00588 0.00171 N7 3 0.479654 0.605832 0.319446 11.00000 0.01991 0.02595 = 0.02951 -0.00518 -0.01287 0.00719 H7N 2 0.547708 0.580639 0.325414 11.00000 0.02033 O8 4 0.354853 0.766243 0.351675 11.00000 0.02087 0.02355 = 0.03505 -0.00502 -0.01282 0.00558 C8 1 0.451565 0.709235 0.358214 11.00000 0.01837 0.02356 = 0.02095 -0.00061 -0.00541 0.00080 C9 1 0.550723 0.752807 0.408576 11.00000 0.01719 0.02673 = 0.02583 -0.00487 -0.00835 0.00244 C10C 1 0.496531 0.861280 0.461081 11.00000 0.02825 0.03409 = 0.04558 -0.01585 -0.01856 0.00715 AFIX 33 H10A 2 0.480212 0.914798 0.410999 11.00000 -1.50000 H10B 2 0.561322 0.890830 0.491699 11.00000 -1.50000 H10C 2 0.413158 0.848068 0.514357 11.00000 -1.50000 AFIX 0 C10A 1 0.680720 0.773493 0.323266 11.00000 0.02489 0.04118 = 0.02922 -0.00087 -0.00744 -0.00646 AFIX 33 H10D 2 0.663184 0.826961 0.273607 11.00000 -1.50000 H10E 2 0.714915 0.703592 0.289257 11.00000 -1.50000 H10F 2 0.746612 0.803062 0.352760 11.00000 -1.50000 AFIX 0 C11 1 0.231297 0.670394 0.039123 11.00000 0.02573 0.03129 = 0.02318 0.00183 -0.00568 -0.00168 AFIX 23 H11A 2 0.313667 0.630095 0.041836 11.00000 -1.20000 H11B 2 0.255926 0.746078 0.012635 11.00000 -1.20000 AFIX 0 C12 1 0.174572 0.612160 -0.035595 11.00000 0.03607 0.04148 = 0.02232 -0.00290 -0.00731 -0.00087 AFIX 23 H12A 2 0.156321 0.534495 -0.012436 11.00000 -1.20000 H12B 2 0.241789 0.610753 -0.103238 11.00000 -1.20000 AFIX 0 S13 7 0.023129 0.678612 -0.048084 11.00000 0.04249 0.05054 = 0.02796 0.00239 -0.01974 -0.00300 C14 1 -0.066454 0.691124 0.085383 11.00000 0.02721 0.03930 = 0.03127 -0.00257 -0.01564 0.00123 AFIX 23 H14A 2 -0.147942 0.737437 0.092471 11.00000 -1.20000 H14B 2 -0.093664 0.616771 0.114306 11.00000 -1.20000 AFIX 0 C15 1 0.016841 0.742522 0.144945 11.00000 0.02255 0.02910 = 0.02864 -0.00288 -0.01128 0.00520 AFIX 23 H15A 2 0.041304 0.817592 0.116615 11.00000 -1.20000 H15B 2 -0.038385 0.751079 0.216444 11.00000 -1.20000 AFIX 0 N21 3 0.068360 0.755034 0.382176 11.00000 0.01849 0.02517 = 0.02299 0.00158 -0.00843 0.00119 C22 1 0.024090 0.678744 0.454120 11.00000 0.02681 0.03124 = 0.02892 0.00836 -0.01045 -0.00148 AFIX 43 H22A 2 0.068447 0.608289 0.447491 11.00000 -1.20000 AFIX 0 C23 1 -0.085655 0.697850 0.539685 11.00000 0.02933 0.04317 = 0.02656 0.01182 -0.00797 -0.00891 AFIX 43 H23A 2 -0.114318 0.641279 0.589851 11.00000 -1.20000 AFIX 0 C24 1 -0.150705 0.798449 0.550061 11.00000 0.02022 0.04747 = 0.02076 -0.00057 -0.00527 -0.00543 AFIX 43 H24A 2 -0.225412 0.812361 0.607381 11.00000 -1.20000 AFIX 0 C25 1 -0.106399 0.881506 0.475269 11.00000 0.01652 0.03389 = 0.02099 -0.00402 -0.00725 -0.00143 C26' 1 0.005124 0.855946 0.392849 11.00000 0.01565 0.02626 = 0.01993 -0.00174 -0.00812 -0.00120 C26 1 -0.169403 0.989451 0.479645 11.00000 0.01610 0.03876 = 0.02885 -0.01187 -0.00454 0.00266 AFIX 43 H26A 2 -0.243876 1.007600 0.535897 11.00000 -1.20000 AFIX 0 C27' 1 0.057761 0.938922 0.315983 11.00000 0.01780 0.02234 = 0.01962 -0.00293 -0.00780 0.00085 C27 1 -0.124168 1.065270 0.404946 11.00000 0.02205 0.02855 = 0.03620 -0.00998 -0.00924 0.00692 AFIX 43 H27A 2 -0.169595 1.135003 0.408051 11.00000 -1.20000 AFIX 0 C28 1 -0.008798 1.042721 0.320874 11.00000 0.02121 0.02411 = 0.02848 -0.00438 -0.00886 0.00302 C29 1 0.044290 1.120198 0.243004 11.00000 0.03344 0.02184 = 0.03914 -0.00043 -0.01226 0.00520 AFIX 43 H29A 2 0.001306 1.190499 0.242158 11.00000 -1.20000 AFIX 0 C30 1 0.158689 1.093481 0.168223 11.00000 0.03542 0.02623 = 0.03377 0.00763 -0.00557 -0.00226 AFIX 43 H30A 2 0.195577 1.145147 0.115044 11.00000 -1.20000 AFIX 0 N31 3 0.171780 0.913170 0.241789 11.00000 0.01745 0.02338 = 0.02209 -0.00113 -0.00510 0.00050 C31 1 0.220901 0.989570 0.170653 11.00000 0.02509 0.02664 = 0.02522 0.00094 -0.00314 -0.00050 AFIX 43 H31A 2 0.301495 0.972987 0.119381 11.00000 -1.20000 AFIX 0 CL1 5 0.544065 0.783339 0.058012 11.00000 0.02185 0.05002 = 0.02529 -0.00143 -0.00130 0.00076 O1A 4 0.425878 0.801137 0.139506 11.00000 0.03190 0.05197 = 0.05289 -0.00168 0.01417 -0.00504 O2A 4 0.572481 0.665930 0.054792 11.00000 0.08732 0.06041 = 0.09567 -0.01668 -0.00760 0.03569 O3A 4 0.519915 0.821930 -0.033764 11.00000 0.08427 0.10444 = 0.03745 0.01883 -0.02736 -0.03206 O4A 4 0.648859 0.841921 0.075755 11.00000 0.04041 0.10503 = 0.06397 0.01228 -0.02272 -0.02372 CL2 5 0.795639 0.398395 0.340712 11.00000 0.02258 0.03148 = 0.03341 0.00834 -0.00358 0.00670 O5A 4 0.738401 0.301210 0.310307 11.00000 0.04997 0.03999 = 0.07087 -0.00272 -0.01769 -0.00411 O6A 4 0.747730 0.407772 0.447508 11.00000 0.04341 0.08277 = 0.03589 0.00814 -0.01034 0.00576 O7A 4 0.935714 0.384523 0.305189 11.00000 0.02220 0.04585 = 0.06360 0.01915 -0.00050 0.00720 O8A 4 0.751734 0.491753 0.290820 11.00000 0.04762 0.04028 = 0.04108 -0.00098 -0.01736 0.02239 N1S 3 -0.442195 0.909283 0.711968 11.00000 0.06786 0.07388 = 0.05296 0.00737 -0.00598 0.02511 C1S 1 -0.550967 0.913451 0.758751 11.00000 0.06619 0.03971 = 0.04214 0.00649 -0.01599 0.01019 C2S 1 -0.690972 0.919027 0.820804 11.00000 0.06711 0.04976 = 0.06865 0.00422 -0.01251 -0.00642 AFIX 137 H2S1 2 -0.733699 0.849869 0.814276 11.00000 -1.50000 H2S2 2 -0.736778 0.981349 0.797112 11.00000 -1.50000 H2S3 2 -0.695647 0.929572 0.892335 11.00000 -1.50000 HKLF 4 REM r4193 in P-1 REM R1 = 0.0436 for 6869 Fo > 4sig(Fo) and 0.0495 for all 7775 data REM 438 parameters refined using 0 restraints END WGHT 0.0579 1.6357 REM Highest difference peak 1.324, deepest hole -0.487, 1-sigma level 0.083 Q1 1 0.8545 0.5034 0.4038 11.00000 0.05 1.32 Q2 1 0.7577 0.3291 0.4295 11.00000 0.05 0.94 Q3 1 0.6389 0.7234 0.0188 11.00000 0.05 0.73 Q4 1 0.8130 0.4376 0.3754 11.00000 0.05 0.65 Q5 1 0.2173 0.6836 0.2414 11.00000 0.05 0.62 Q6 1 0.5683 0.9024 0.1216 11.00000 0.05 0.61 Q7 1 0.6997 0.4413 0.3172 11.00000 0.05 0.61 Q8 1 0.2742 0.8028 0.2574 11.00000 0.05 0.56 Q9 1 0.2391 0.7791 0.1993 11.00000 0.05 0.56 Q10 1 0.2617 0.6929 0.2129 11.00000 0.05 0.50 ; _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^)+(0.0579P)^2^+1.6358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment 'riding/refall/rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7775 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Zn Zn 0.23948(2) 0.74852(2) 0.25259(2) 0.01978(9) Uani 1 1 d . . . N1 N 0.14047(19) 0.67886(16) 0.14447(15) 0.0214(4) Uani 1 1 d . . . C1 C 0.1072(2) 0.56809(19) 0.19165(18) 0.0238(5) Uani 1 1 d . . . H1A H 0.0761 0.5214 0.1454 0.029 Uiso 1 1 calc R . . H1B H 0.0346 0.5755 0.2562 0.029 Uiso 1 1 calc R . . C1OB C 0.5757(3) 0.6690(2) 0.48724(19) 0.0296(5) Uani 1 1 d . . . H1OA H 0.4923 0.6564 0.5406 0.044 Uiso 1 1 calc R . . H1OB H 0.6409 0.6982 0.5177 0.044 Uiso 1 1 calc R . . H1OC H 0.6100 0.5989 0.4536 0.044 Uiso 1 1 calc R . . N2 N 0.29863(19) 0.58155(16) 0.25344(14) 0.0206(4) Uani 1 1 d . . . C2 C 0.2281(2) 0.51398(19) 0.21249(17) 0.0230(5) Uani 1 1 d . . . C3 C 0.2637(3) 0.4048(2) 0.1914(2) 0.0294(5) Uani 1 1 d . . . H3A H 0.2128 0.3596 0.1621 0.035 Uiso 1 1 calc R . . C4 C 0.3764(3) 0.3619(2) 0.2141(2) 0.0321(6) Uani 1 1 d . . . H4A H 0.4033 0.2865 0.2004 0.039 Uiso 1 1 calc R . . C5 C 0.4483(3) 0.4287(2) 0.2563(2) 0.0283(5) Uani 1 1 d . . . H5A H 0.5253 0.4005 0.2723 0.034 Uiso 1 1 calc R . . C6 C 0.4063(2) 0.53936(19) 0.27528(17) 0.0220(4) Uani 1 1 d . . . N7 N 0.4797(2) 0.60583(17) 0.31945(16) 0.0240(4) Uani 1 1 d . . . H7N H 0.548(3) 0.581(2) 0.325(2) 0.020(7) Uiso 1 1 d . . . O8 O 0.35485(16) 0.76624(13) 0.35168(13) 0.0256(4) Uani 1 1 d . . . C8 C 0.4516(2) 0.70924(19) 0.35821(17) 0.0211(4) Uani 1 1 d . . . C9 C 0.5507(2) 0.75281(19) 0.40858(18) 0.0228(5) Uani 1 1 d . . . C10C C 0.4965(3) 0.8613(2) 0.4611(2) 0.0343(6) Uani 1 1 d . . . H10A H 0.4802 0.9148 0.4110 0.051 Uiso 1 1 calc R . . H10B H 0.5613 0.8908 0.4917 0.051 Uiso 1 1 calc R . . H10C H 0.4132 0.8481 0.5144 0.051 Uiso 1 1 calc R . . C10A C 0.6807(3) 0.7735(2) 0.3233(2) 0.0317(5) Uani 1 1 d . . . H10D H 0.6632 0.8270 0.2736 0.048 Uiso 1 1 calc R . . H10E H 0.7149 0.7036 0.2893 0.048 Uiso 1 1 calc R . . H10F H 0.7466 0.8031 0.3528 0.048 Uiso 1 1 calc R . . C11 C 0.2313(2) 0.6704(2) 0.03912(18) 0.0271(5) Uani 1 1 d . . . H11A H 0.3137 0.6301 0.0418 0.032 Uiso 1 1 calc R . . H11B H 0.2559 0.7461 0.0126 0.032 Uiso 1 1 calc R . . C12 C 0.1746(3) 0.6122(2) -0.0356(2) 0.0335(6) Uani 1 1 d . . . H12A H 0.1563 0.5345 -0.0124 0.040 Uiso 1 1 calc R . . H12B H 0.2418 0.6108 -0.1032 0.040 Uiso 1 1 calc R . . S13 S 0.02313(8) 0.67861(7) -0.04808(5) 0.03832(17) Uani 1 1 d . . . C14 C -0.0665(3) 0.6911(2) 0.0854(2) 0.0311(5) Uani 1 1 d . . . H14A H -0.1479 0.7374 0.0925 0.037 Uiso 1 1 calc R . . H14B H -0.0937 0.6168 0.1143 0.037 Uiso 1 1 calc R . . C15 C 0.0168(2) 0.7425(2) 0.14494(19) 0.0260(5) Uani 1 1 d . . . H15A H 0.0413 0.8176 0.1166 0.031 Uiso 1 1 calc R . . H15B H -0.0384 0.7511 0.2164 0.031 Uiso 1 1 calc R . . N21 N 0.06836(19) 0.75503(16) 0.38218(15) 0.0218(4) Uani 1 1 d . . . C22 C 0.0241(3) 0.6787(2) 0.45412(19) 0.0286(5) Uani 1 1 d . . . H22A H 0.0684 0.6083 0.4475 0.034 Uiso 1 1 calc R . . C23 C -0.0857(3) 0.6979(2) 0.5397(2) 0.0331(6) Uani 1 1 d . . . H23A H -0.1143 0.6413 0.5899 0.040 Uiso 1 1 calc R . . C24 C -0.1507(2) 0.7984(2) 0.55006(19) 0.0295(5) Uani 1 1 d . . . H24A H -0.2254 0.8124 0.6074 0.035 Uiso 1 1 calc R . . C25 C -0.1064(2) 0.8815(2) 0.47527(17) 0.0233(5) Uani 1 1 d . . . C26' C 0.0051(2) 0.85595(19) 0.39285(17) 0.0199(4) Uani 1 1 d . . . C26 C -0.1694(2) 0.9895(2) 0.47964(19) 0.0282(5) Uani 1 1 d . . . H26A H -0.2439 1.0076 0.5359 0.034 Uiso 1 1 calc R . . C27' C 0.0578(2) 0.93892(18) 0.31598(17) 0.0194(4) Uani 1 1 d . . . C27 C -0.1242(2) 1.0653(2) 0.4049(2) 0.0288(5) Uani 1 1 d . . . H27A H -0.1696 1.1350 0.4081 0.035 Uiso 1 1 calc R . . C28 C -0.0088(2) 1.0427(2) 0.32087(19) 0.0243(5) Uani 1 1 d . . . C29 C 0.0443(3) 1.1202(2) 0.2430(2) 0.0313(5) Uani 1 1 d . . . H29A H 0.0013 1.1905 0.2422 0.038 Uiso 1 1 calc R . . C30 C 0.1587(3) 1.0935(2) 0.1682(2) 0.0329(6) Uani 1 1 d . . . H30A H 0.1956 1.1451 0.1150 0.039 Uiso 1 1 calc R . . N31 N 0.17178(18) 0.91317(16) 0.24179(15) 0.0211(4) Uani 1 1 d . . . C31 C 0.2209(2) 0.9896(2) 0.17065(19) 0.0266(5) Uani 1 1 d . . . H31A H 0.3015 0.9730 0.1194 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.54406(6) 0.78334(6) 0.05801(5) 0.03360(15) Uani 1 1 d . . . O1A O 0.4259(2) 0.80114(19) 0.13951(18) 0.0511(6) Uani 1 1 d . . . O2A O 0.5725(3) 0.6659(2) 0.0548(3) 0.0858(10) Uani 1 1 d . . . O3A O 0.5199(3) 0.8219(3) -0.03376(19) 0.0730(9) Uani 1 1 d . . . O4A O 0.6489(2) 0.8419(3) 0.0758(2) 0.0679(8) Uani 1 1 d . . . Cl2 Cl 0.79564(6) 0.39840(5) 0.34071(5) 0.03045(14) Uani 1 1 d . . . O5A O 0.7384(2) 0.30121(19) 0.3103(2) 0.0535(6) Uani 1 1 d . . . O6A O 0.7477(2) 0.4078(2) 0.44751(17) 0.0546(6) Uani 1 1 d . . . O7A O 0.93571(19) 0.38452(18) 0.30519(18) 0.0470(6) Uani 1 1 d . . . O8A O 0.7517(2) 0.49175(17) 0.29082(16) 0.0426(5) Uani 1 1 d . . . N1S N -0.4422(4) 0.9093(3) 0.7120(3) 0.0681(10) Uani 1 1 d . . . C1S C -0.5510(4) 0.9135(3) 0.7588(3) 0.0497(8) Uani 1 1 d . . . C2S C -0.6910(4) 0.9190(3) 0.8208(3) 0.0634(10) Uani 1 1 d . . . H2S1 H -0.7337 0.8499 0.8143 0.095 Uiso 1 1 calc R . . H2S2 H -0.7368 0.9813 0.7971 0.095 Uiso 1 1 calc R . . H2S3 H -0.6956 0.9296 0.8923 0.095 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 0.01592(13) 0.01978(14) 0.02383(15) -0.00102(10) -0.00640(10) 0.00267(9) N1 0.0202(9) 0.0225(9) 0.0219(9) 0.0014(7) -0.0070(7) -0.0001(7) C1 0.0225(11) 0.0254(11) 0.0252(11) 0.0022(9) -0.0094(9) -0.0050(9) C1OB 0.0254(12) 0.0390(14) 0.0263(12) -0.0006(10) -0.0110(10) 0.0028(10) N2 0.0215(9) 0.0207(9) 0.0207(9) 0.0002(7) -0.0079(7) -0.0005(7) C2 0.0245(11) 0.0246(11) 0.0202(11) 0.0020(9) -0.0070(9) -0.0027(9) C3 0.0368(14) 0.0231(12) 0.0308(13) -0.0016(10) -0.0131(11) -0.0034(10) C4 0.0431(15) 0.0208(11) 0.0330(13) -0.0034(10) -0.0125(12) 0.0060(10) C5 0.0312(13) 0.0250(12) 0.0302(13) -0.0021(10) -0.0120(10) 0.0079(10) C6 0.0223(11) 0.0230(11) 0.0203(10) -0.0010(8) -0.0059(9) 0.0017(9) N7 0.0199(9) 0.0260(10) 0.0295(11) -0.0052(8) -0.0129(8) 0.0072(8) O8 0.0209(8) 0.0236(8) 0.0351(9) -0.0050(7) -0.0128(7) 0.0056(6) C8 0.0184(10) 0.0236(11) 0.0209(11) -0.0006(8) -0.0054(8) 0.0008(8) C9 0.0172(10) 0.0267(11) 0.0258(11) -0.0049(9) -0.0084(9) 0.0024(9) C10C 0.0283(13) 0.0341(14) 0.0456(16) -0.0159(12) -0.0186(12) 0.0072(11) C10A 0.0249(12) 0.0412(15) 0.0292(13) -0.0009(11) -0.0074(10) -0.0065(11) C11 0.0257(12) 0.0313(12) 0.0232(12) 0.0018(10) -0.0057(9) -0.0017(10) C12 0.0361(14) 0.0415(15) 0.0223(12) -0.0029(11) -0.0073(11) -0.0009(11) S13 0.0425(4) 0.0505(4) 0.0280(3) 0.0024(3) -0.0197(3) -0.0030(3) C14 0.0272(12) 0.0393(14) 0.0313(13) -0.0026(11) -0.0156(11) 0.0012(11) C15 0.0225(11) 0.0291(12) 0.0286(12) -0.0029(10) -0.0113(10) 0.0052(9) N21 0.0185(9) 0.0252(10) 0.0230(9) 0.0016(8) -0.0084(8) 0.0012(7) C22 0.0268(12) 0.0312(13) 0.0289(13) 0.0084(10) -0.0105(10) -0.0015(10) C23 0.0293(13) 0.0432(15) 0.0266(13) 0.0118(11) -0.0080(10) -0.0089(11) C24 0.0202(11) 0.0475(15) 0.0208(11) -0.0006(10) -0.0053(9) -0.0054(10) C25 0.0165(10) 0.0339(12) 0.0210(11) -0.0040(9) -0.0073(9) -0.0014(9) C26' 0.0156(10) 0.0263(11) 0.0199(10) -0.0017(8) -0.0081(8) -0.0012(8) C26 0.0161(10) 0.0388(14) 0.0289(12) -0.0119(10) -0.0045(9) 0.0027(9) C27' 0.0178(10) 0.0223(10) 0.0196(10) -0.0029(8) -0.0078(8) 0.0008(8) C27 0.0220(11) 0.0286(12) 0.0362(14) -0.0100(10) -0.0092(10) 0.0069(9) C28 0.0212(11) 0.0241(11) 0.0285(12) -0.0044(9) -0.0089(9) 0.0030(9) C29 0.0334(13) 0.0218(11) 0.0391(14) -0.0004(10) -0.0123(11) 0.0052(10) C30 0.0354(14) 0.0262(12) 0.0338(14) 0.0076(10) -0.0056(11) -0.0023(10) N31 0.0175(9) 0.0234(9) 0.0221(9) -0.0011(7) -0.0051(7) 0.0005(7) C31 0.0251(12) 0.0266(12) 0.0252(12) 0.0009(9) -0.0031(9) -0.0005(9) Cl1 0.0218(3) 0.0500(4) 0.0253(3) -0.0014(3) -0.0013(2) 0.0008(3) O1A 0.0319(11) 0.0520(13) 0.0529(14) -0.0017(11) 0.0142(10) -0.0050(10) O2A 0.087(2) 0.0604(18) 0.096(2) -0.0167(16) -0.0076(19) 0.0357(16) O3A 0.084(2) 0.104(2) 0.0374(13) 0.0188(14) -0.0274(14) -0.0321(18) O4A 0.0404(13) 0.105(2) 0.0640(17) 0.0123(15) -0.0227(12) -0.0237(14) Cl2 0.0226(3) 0.0315(3) 0.0334(3) 0.0083(2) -0.0036(2) 0.0067(2) O5A 0.0500(14) 0.0400(12) 0.0709(17) -0.0027(11) -0.0177(12) -0.0041(10) O6A 0.0434(13) 0.0828(18) 0.0359(12) 0.0081(11) -0.0103(10) 0.0058(12) O7A 0.0222(9) 0.0458(12) 0.0636(14) 0.0192(10) -0.0005(9) 0.0072(8) O8A 0.0476(12) 0.0403(11) 0.0411(11) -0.0010(9) -0.0174(10) 0.0224(9) N1S 0.068(2) 0.074(2) 0.0530(19) 0.0074(16) -0.0060(17) 0.0251(18) C1S 0.066(2) 0.0397(17) 0.0421(18) 0.0065(14) -0.0160(17) 0.0102(16) C2S 0.067(2) 0.050(2) 0.069(3) 0.0042(18) -0.013(2) -0.0064(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 O8 2.0900(17) . ? Zn N2 2.0911(19) . ? Zn N31 2.1062(19) . ? Zn N21 2.132(2) . ? Zn O1A 2.219(2) . ? Zn N1 2.2405(19) . ? N1 C1 1.480(3) . ? N1 C11 1.487(3) . ? N1 C15 1.488(3) . ? C1 C2 1.510(3) . ? C1OB C9 1.535(3) . ? N2 C6 1.337(3) . ? N2 C2 1.356(3) . ? C2 C3 1.373(3) . ? C3 C4 1.393(4) . ? C4 C5 1.372(4) . ? C5 C6 1.399(3) . ? C6 N7 1.395(3) . ? N7 C8 1.358(3) . ? O8 C8 1.234(3) . ? C8 C9 1.523(3) . ? C9 C10C 1.522(3) . ? C9 C10A 1.543(3) . ? C11 C12 1.524(4) . ? C12 S13 1.812(3) . ? S13 C14 1.807(3) . ? C14 C15 1.517(3) . ? N21 C22 1.326(3) . ? N21 C26' 1.359(3) . ? C22 C23 1.404(4) . ? C23 C24 1.364(4) . ? C24 C25 1.408(4) . ? C25 C26' 1.404(3) . ? C25 C26 1.437(3) . ? C26' C27' 1.439(3) . ? C26 C27 1.348(4) . ? C27' N31 1.361(3) . ? C27' C28 1.409(3) . ? C27 C28 1.434(3) . ? C28 C29 1.404(4) . ? C29 C30 1.370(4) . ? C30 C31 1.400(3) . ? N31 C31 1.329(3) . ? Cl1 O4A 1.412(3) . ? Cl1 O3A 1.421(3) . ? Cl1 O1A 1.424(2) . ? Cl1 O2A 1.438(3) . ? Cl2 O6A 1.411(2) . ? Cl2 O7A 1.417(2) . ? Cl2 O8A 1.4377(19) . ? Cl2 O5A 1.460(2) . ? N1S C1S 1.138(5) . ? C1S C2S 1.472(5) . ? 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 O8 Zn N2 84.10(7) . . ? O8 Zn N31 100.98(7) . . ? N2 Zn N31 174.90(7) . . ? O8 Zn N21 87.88(7) . . ? N2 Zn N21 101.70(7) . . ? N31 Zn N21 79.14(7) . . ? O8 Zn O1A 81.44(9) . . ? N2 Zn O1A 94.92(8) . . ? N31 Zn O1A 85.42(8) . . ? N21 Zn O1A 159.21(9) . . ? O8 Zn N1 163.20(7) . . ? N2 Zn N1 79.17(7) . . ? N31 Zn N1 95.74(7) . . ? N21 Zn N1 96.97(7) . . ? O1A Zn N1 98.36(9) . . ? C1 N1 C11 111.45(19) . . ? C1 N1 C15 110.00(18) . . ? C11 N1 C15 110.62(18) . . ? C1 N1 Zn 100.00(13) . . ? C11 N1 Zn 112.42(14) . . ? C15 N1 Zn 111.93(14) . . ? N1 C1 C2 109.75(18) . . ? C6 N2 C2 118.4(2) . . ? C6 N2 Zn 127.28(16) . . ? C2 N2 Zn 113.53(15) . . ? N2 C2 C3 122.8(2) . . ? N2 C2 C1 114.8(2) . . ? C3 C2 C1 122.4(2) . . ? C2 C3 C4 118.3(2) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 118.7(2) . . ? N2 C6 N7 120.0(2) . . ? N2 C6 C5 122.0(2) . . ? N7 C6 C5 118.0(2) . . ? C8 N7 C6 129.9(2) . . ? C8 O8 Zn 128.51(15) . . ? O8 C8 N7 123.3(2) . . ? O8 C8 C9 121.4(2) . . ? N7 C8 C9 115.31(19) . . ? C10C C9 C8 109.21(19) . . ? C10C C9 C1OB 109.4(2) . . ? C8 C9 C1OB 111.0(2) . . ? C10C C9 C10A 109.7(2) . . ? C8 C9 C10A 107.14(19) . . ? C1OB C9 C10A 110.4(2) . . ? N1 C11 C12 115.0(2) . . ? C11 C12 S13 112.93(19) . . ? C14 S13 C12 98.90(12) . . ? C15 C14 S13 111.91(18) . . ? N1 C15 C14 115.1(2) . . ? C22 N21 C26' 118.2(2) . . ? C22 N21 Zn 129.05(17) . . ? C26' N21 Zn 112.52(15) . . ? N21 C22 C23 122.7(2) . . ? C24 C23 C22 119.3(2) . . ? C23 C24 C25 119.6(2) . . ? C26' C25 C24 117.4(2) . . ? C26' C25 C26 119.3(2) . . ? C24 C25 C26 123.3(2) . . ? N21 C26' C25 122.8(2) . . ? N21 C26' C27' 117.4(2) . . ? C25 C26' C27' 119.9(2) . . ? C27 C26 C25 120.8(2) . . ? N31 C27' C28 122.9(2) . . ? N31 C27' C26' 117.78(19) . . ? C28 C27' C26' 119.3(2) . . ? C26 C27 C28 121.3(2) . . ? C29 C28 C27' 117.4(2) . . ? C29 C28 C27 123.3(2) . . ? C27' C28 C27 119.3(2) . . ? C30 C29 C28 119.4(2) . . ? C29 C30 C31 119.6(2) . . ? C31 N31 C27' 118.0(2) . . ? C31 N31 Zn 128.81(16) . . ? C27' N31 Zn 113.05(15) . . ? N31 C31 C30 122.7(2) . . ? O4A Cl1 O3A 110.06(17) . . ? O4A Cl1 O1A 109.72(17) . . ? O3A Cl1 O1A 108.26(18) . . ? O4A Cl1 O2A 111.1(2) . . ? O3A Cl1 O2A 110.9(2) . . ? O1A Cl1 O2A 106.72(17) . . ? Cl1 O1A Zn 154.07(15) . . ? O6A Cl2 O7A 112.78(15) . . ? O6A Cl2 O8A 110.91(14) . . ? O7A Cl2 O8A 110.61(13) . . ? O6A Cl2 O5A 108.73(16) . . ? O7A Cl2 O5A 107.50(14) . . ? O8A Cl2 O5A 106.00(14) . . ? N1S C1S C2S 179.0(4) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 1.324 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.083