# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Elena A. Vinogradova' 'Olga Yu. Vassilyeva' 'Volodymyr N. Kokozay' 'Philip J. Squattrito' 'Jan Reedijk' 'Gerard A. Van Albada' 'Wolfgang Linert' 'Satish K. Tiwarye' 'Paul R. Raithby' _publ_contact_author_name 'Prof P Raithby' _publ_contact_author_address ; Prof P Raithby Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; _publ_contact_author_email 'p.r.raithby@bath.ac.uk' _publ_section_references ; Gilmore, C. J. (1983). MITHRIL. Computer Program for the Automatic Solution of Crystal Structures from X-ray Data. Department of Chemistry, University of Glasgow, Scotland. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation (1988). MSC/AFC Diffractometer Control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation (1991). TEXSAN. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ; data_LV221 #Compound 1 _database_code_CSD 159629 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Dec 10 16:40:02 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record 'modified by P. Squattrito 14 Dec. 1999' #------------------------------------------------------------------------------ _computing_data_collection ; MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1988) ; _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1991) ; _computing_structure_solution 'MITHRIL (Gilmore, 1983)' _computing_structure_refinement 'TEXSAN' _computing_publication_material 'TEXSAN' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #------------------------------------------------------------------------------ _cell_length_a 15.004(4) _cell_length_b 10.412(4) _cell_length_c 16.228(2) _cell_angle_alpha 90 _cell_angle_beta 112.69(1) _cell_angle_gamma 90 _cell_volume 2338(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 16.6 _cell_measurement_theta_max 20.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 580.25 _chemical_formula_sum 'C12 H33 Cl3 Cu2 N4 O3 Zn ' _chemical_formula_moiety 'C12 H33 Cl3 Cu2 N4 O3 Zn ' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 3.22 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North et al., 1968) ; _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_correction_T_min 0.458 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 296 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -2 1 3 -1 3 1 -2 _diffrn_reflns_number 4560 _reflns_number_total 4122 _diffrn_reflns_av_R_equivalents 0.058 _reflns_number_gt 2378 _reflns_threshold_expression I>3\s(I) _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.06346 _diffrn_orient_matrix_UB_12 0.04094 _diffrn_orient_matrix_UB_13 -0.00932 _diffrn_orient_matrix_UB_21 0.03438 _diffrn_orient_matrix_UB_22 0.07109 _diffrn_orient_matrix_UB_23 0.04153 _diffrn_orient_matrix_UB_31 0.00309 _diffrn_orient_matrix_UB_32 0.04995 _diffrn_orient_matrix_UB_33 -0.05147 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 'International Tables' H 0 132 0.000 0.000 'International Tables' Cl 0 12 0.132 0.159 'International Tables' Cu 0 8 0.263 1.266 'International Tables' N 0 16 0.004 0.003 'International Tables' O 0 12 0.008 0.006 'International Tables' Zn 0 4 0.222 1.431 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Zn2 0.76435(6) -0.09530(7) 0.85605(5) 0.0353(2) Uij ? ? Cu1 0.63830(6) -0.16033(8) 0.65270(5) 0.0326(2) Uij ? ? Cu3 0.78120(6) 0.09078(8) 0.70615(5) 0.0341(2) Uij ? ? Cl1 0.5871(1) 0.0834(2) 0.64044(10) 0.0399(5) Uij ? ? Cl2 0.7478(2) -0.0810(2) 0.9899(1) 0.0624(7) Uij ? ? Cl3 0.8228(1) 0.0965(2) 0.5855(1) 0.0585(6) Uij ? ? O1 0.7727(3) -0.0974(4) 0.7077(2) 0.031(1) Uij ? ? O2 0.6525(3) -0.1890(4) 0.7742(3) 0.048(1) Uij ? ? O3 0.8033(3) 0.0747(4) 0.8323(2) 0.038(1) Uij ? ? N1 0.8806(4) -0.2225(5) 0.8750(3) 0.048(2) Uij ? ? N2 0.5136(4) -0.2647(5) 0.6220(3) 0.038(2) Uij ? ? N3 0.7931(4) 0.2830(5) 0.7340(3) 0.040(2) Uij ? ? N4 0.6406(3) -0.1492(5) 0.5308(3) 0.035(2) Uij ? ? C1 0.8536(5) -0.1750(7) 0.7160(4) 0.043(2) Uij ? ? C2 0.8715(5) -0.2761(6) 0.7875(4) 0.046(2) Uij ? ? C3 0.9727(5) -0.1510(8) 0.9152(5) 0.074(3) Uij ? ? C4 0.8810(7) -0.3298(8) 0.9350(5) 0.097(4) Uij ? ? C5 0.5683(5) -0.2344(7) 0.7829(4) 0.058(3) Uij ? ? C6 0.5203(5) -0.3252(8) 0.7063(5) 0.066(3) Uij ? ? C7 0.5013(6) -0.3646(7) 0.5536(5) 0.074(3) Uij ? ? C8 0.4267(5) -0.1816(8) 0.5870(5) 0.064(3) Uij ? ? C9 0.8068(5) 0.1923(7) 0.8769(4) 0.050(2) Uij ? ? C10 0.7609(5) 0.2947(6) 0.8086(4) 0.046(2) Uij ? ? C11 0.7331(6) 0.3654(7) 0.6588(5) 0.071(3) Uij ? ? C12 0.8953(6) 0.3205(7) 0.7619(5) 0.071(3) Uij ? ? H1 0.9089 -0.1227 0.7312 0.0515 Uij ? ? H2 0.8410 -0.2170 0.6609 0.0515 Uij ? ? H3 0.8195 -0.3353 0.7687 0.0545 Uij ? ? H4 0.9299 -0.3195 0.7955 0.0545 Uij ? ? H5 1.0245 -0.2071 0.9196 0.0863 Uij ? ? H6 0.9802 -0.1216 0.9723 0.0863 Uij ? ? H7 0.9721 -0.0804 0.8778 0.0863 Uij ? ? H8 0.8209 -0.3733 0.9114 0.1202 Uij ? ? H9 0.9317 -0.3873 0.9396 0.1202 Uij ? ? H10 0.8909 -0.2964 0.9924 0.1202 Uij ? ? H11 0.5850 -0.2790 0.8385 0.0691 Uij ? ? H12 0.5267 -0.1653 0.7811 0.0691 Uij ? ? H13 0.5573 -0.4019 0.7157 0.0794 Uij ? ? H14 0.4574 -0.3451 0.7034 0.0794 Uij ? ? H15 0.5609 -0.4071 0.5657 0.0909 Uij ? ? H16 0.4804 -0.3252 0.4962 0.0909 Uij ? ? H17 0.4541 -0.4251 0.5541 0.0909 Uij ? ? H18 0.4346 -0.1112 0.6263 0.0764 Uij ? ? H19 0.4194 -0.1504 0.5296 0.0764 Uij ? ? H20 0.3714 -0.2296 0.5823 0.0764 Uij ? ? H21 0.7719 0.1838 0.9150 0.0603 Uij ? ? H22 0.8717 0.2140 0.9118 0.0603 Uij ? ? H23 0.7792 0.3768 0.8359 0.0557 Uij ? ? H24 0.6927 0.2865 0.7866 0.0557 Uij ? ? H25 0.7502 0.3509 0.6093 0.0843 Uij ? ? H26 0.7444 0.4528 0.6768 0.0843 Uij ? ? H27 0.6673 0.3451 0.6438 0.0843 Uij ? ? H28 0.9157 0.3109 0.7144 0.0851 Uij ? ? H29 0.9028 0.4075 0.7817 0.0851 Uij ? ? H30 0.9338 0.2672 0.8110 0.0851 Uij ? ? H31 0.6600 -0.2451 0.5053 0.0416 Uij ? ? H32 0.6906 -0.0603 0.5334 0.0416 Uij ? ? H33 0.5815 -0.1306 0.4779 0.0416 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn2 0.0416(5) 0.0359(5) 0.0252(4) -0.0012(4) 0.0094(4) -0.0018(4) Cu1 0.0331(5) 0.0419(5) 0.0224(4) -0.0058(4) 0.0103(3) -0.0029(4) Cu3 0.0386(5) 0.0341(5) 0.0300(4) -0.0038(4) 0.0138(4) -0.0008(4) Cl1 0.0354(10) 0.045(1) 0.0373(9) 0.0035(9) 0.0117(8) -0.0052(9) Cl2 0.105(2) 0.054(1) 0.041(1) -0.013(1) 0.041(1) -0.0093(10) Cl3 0.074(1) 0.064(1) 0.052(1) -0.014(1) 0.041(1) -0.003(1) O1 0.027(2) 0.035(2) 0.031(2) 0.003(2) 0.009(2) -0.001(2) O2 0.046(3) 0.071(4) 0.023(2) -0.025(3) 0.011(2) 0.000(2) O3 0.060(3) 0.031(3) 0.023(2) -0.001(2) 0.015(2) -0.003(2) N1 0.057(4) 0.040(4) 0.036(3) 0.010(3) 0.007(3) -0.001(3) N2 0.036(4) 0.045(4) 0.033(3) -0.010(3) 0.011(3) -0.006(3) N3 0.044(4) 0.033(4) 0.038(3) -0.006(3) 0.009(3) 0.000(3) N4 0.043(3) 0.039(3) 0.022(3) 0.000(3) 0.010(3) -0.002(3) C1 0.038(4) 0.045(5) 0.042(4) 0.002(4) 0.011(3) -0.013(4) C2 0.055(5) 0.033(4) 0.046(4) 0.014(4) 0.016(4) -0.002(4) C3 0.057(6) 0.093(7) 0.049(5) 0.021(5) -0.005(4) -0.019(5) C4 0.17(1) 0.057(6) 0.066(6) 0.045(7) 0.053(7) 0.032(5) C5 0.062(5) 0.078(6) 0.039(4) -0.030(5) 0.023(4) -0.005(4) C6 0.060(5) 0.087(6) 0.044(5) -0.036(5) 0.013(4) 0.015(5) C7 0.084(7) 0.071(6) 0.069(6) -0.029(5) 0.031(5) -0.017(5) C8 0.046(5) 0.078(6) 0.070(6) -0.008(5) 0.024(4) 0.010(5) C9 0.061(5) 0.042(5) 0.041(4) 0.008(4) 0.012(4) 0.000(4) C10 0.049(5) 0.037(4) 0.047(5) 0.005(4) 0.014(4) -0.007(4) C11 0.101(7) 0.044(5) 0.057(5) -0.002(5) 0.017(5) 0.012(4) C12 0.060(6) 0.064(6) 0.094(7) -0.031(5) 0.036(5) -0.018(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 4F~o~^2^/\s^2^(F~o~^2^) ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details 'not applicable' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2378 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.031 _refine_ls_goodness_of_fit_ref 1.68 _refine_ls_shift/su_max 0.012 _refine_diff_density_min -0.48 _refine_diff_density_max 0.36 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn2 Cl2 2.283(2) ? ? yes Zn2 O2 1.952(4) ? ? yes Zn2 O3 1.948(4) ? ? yes Zn2 N1 2.116(5) ? ? yes Zn2 O1 2.459(4) ? ? yes Cu1 O1 1.975(4) ? ? yes Cu1 O2 1.923(4) ? ? yes Cu1 N2 2.052(5) ? ? yes Cu1 N4 1.995(4) ? ? yes Cu1 Cl1 2.636(2) ? ? yes Cu3 Cl3 2.274(2) ? ? yes Cu3 O1 1.965(4) ? ? yes Cu3 O3 1.950(4) ? ? yes Cu3 N3 2.044(5) ? ? yes Cu3 Cl1 2.688(2) ? ? yes O1 C1 1.421(7) ? ? yes O2 C5 1.406(7) ? ? yes O3 C9 1.413(7) ? ? yes N1 C2 1.482(7) ? ? yes N1 C3 1.481(9) ? ? yes N1 C4 1.481(9) ? ? yes N2 C6 1.474(7) ? ? yes N2 C7 1.480(8) ? ? yes N2 C8 1.483(8) ? ? yes N3 C10 1.472(8) ? ? yes N3 C11 1.479(8) ? ? yes N3 C12 1.474(8) ? ? yes C1 C2 1.512(9) ? ? yes C5 C6 1.506(9) ? ? yes C9 C10 1.500(8) ? ? yes N4 H31 1.16 ? ? no N4 H32 1.18 ? ? no N4 H33 0.99 ? ? no C1 H1 0.94 ? ? no C1 H2 0.95 ? ? no C2 H3 0.95 ? ? no C2 H4 0.95 ? ? no C3 H5 0.95 ? ? no C3 H6 0.94 ? ? no C3 H7 0.95 ? ? no C4 H8 0.95 ? ? no C4 H9 0.95 ? ? no C4 H10 0.95 ? ? no C5 H11 0.96 ? ? no C5 H12 0.95 ? ? no C6 H13 0.95 ? ? no C6 H14 0.95 ? ? no C7 H15 0.95 ? ? no C7 H16 0.95 ? ? no C7 H17 0.95 ? ? no C8 H18 0.95 ? ? no C8 H19 0.95 ? ? no C8 H20 0.95 ? ? no C9 H21 0.96 ? ? no C9 H22 0.95 ? ? no C10 H23 0.95 ? ? no C10 H24 0.95 ? ? no C11 H25 0.95 ? ? no C11 H26 0.95 ? ? no C11 H27 0.95 ? ? no C12 H28 0.94 ? ? no C12 H29 0.95 ? ? no C12 H30 0.96 ? ? no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zn2 O2 107.4(1) ? ? ? yes Cl2 Zn2 O3 106.3(1) ? ? ? yes Cl2 Zn2 N1 106.8(2) ? ? ? yes O2 Zn2 O3 124.3(2) ? ? ? yes O2 Zn2 N1 103.3(2) ? ? ? yes O3 Zn2 N1 107.7(2) ? ? ? yes O3 Zn2 O1 71.5(1) ? ? ? yes O2 Zn2 O1 71.6(1) ? ? ? yes N1 Zn2 O1 77.6(2) ? ? ? yes Cl2 Zn2 O1 175.5(1) ? ? ? yes O1 Cu1 O2 84.1(2) ? ? ? yes O1 Cu1 N2 164.0(2) ? ? ? yes O1 Cu1 N4 91.4(2) ? ? ? yes O2 Cu1 N2 84.1(2) ? ? ? yes O2 Cu1 N4 171.2(2) ? ? ? yes N2 Cu1 N4 98.8(2) ? ? ? yes O2 Cu1 Cl1 98.1(1) ? ? ? yes O1 Cu1 Cl1 86.1(1) ? ? ? yes N4 Cu1 Cl1 89.2(1) ? ? ? yes N2 Cu1 Cl1 106.2(2) ? ? ? yes Cl3 Cu3 O1 94.5(1) ? ? ? yes Cl3 Cu3 O3 156.0(1) ? ? ? yes Cl3 Cu3 N3 97.7(2) ? ? ? yes O1 Cu3 O3 83.5(2) ? ? ? yes O1 Cu3 N3 167.0(2) ? ? ? yes O3 Cu3 N3 83.5(2) ? ? ? yes O3 Cu3 Cl1 97.7(1) ? ? ? yes O1 Cu3 Cl1 84.9(1) ? ? ? yes N3 Cu3 Cl1 96.0(2) ? ? ? yes Cl3 Cu3 Cl1 105.94(7) ? ? ? yes Cu1 O1 Cu3 112.7(2) ? ? ? yes Cu1 O1 C1 122.7(4) ? ? ? yes Cu3 O1 C1 120.7(4) ? ? ? yes Zn2 O2 Cu1 110.3(2) ? ? ? yes Zn2 O2 C5 132.0(4) ? ? ? yes Cu1 O2 C5 114.0(4) ? ? ? yes Zn2 O3 Cu3 110.1(2) ? ? ? yes Zn2 O3 C9 129.8(4) ? ? ? yes Cu3 O3 C9 114.9(4) ? ? ? yes Zn2 N1 C2 109.3(4) ? ? ? yes Zn2 N1 C3 109.0(4) ? ? ? yes Zn2 N1 C4 111.2(5) ? ? ? yes C2 N1 C3 109.7(6) ? ? ? yes C2 N1 C4 108.8(5) ? ? ? yes C3 N1 C4 108.9(6) ? ? ? yes Cu1 N2 C6 105.8(4) ? ? ? yes Cu1 N2 C7 113.1(4) ? ? ? yes Cu1 N2 C8 111.6(4) ? ? ? yes C6 N2 C7 109.9(6) ? ? ? yes C6 N2 C8 109.9(5) ? ? ? yes C7 N2 C8 106.6(5) ? ? ? yes Cu3 N3 C10 103.6(4) ? ? ? yes Cu3 N3 C11 114.4(4) ? ? ? yes Cu3 N3 C12 108.6(4) ? ? ? yes C10 N3 C11 110.0(6) ? ? ? yes C10 N3 C12 110.9(5) ? ? ? yes C11 N3 C12 109.3(6) ? ? ? yes O1 C1 C2 111.1(5) ? ? ? yes N1 C2 C1 113.4(5) ? ? ? yes O2 C5 C6 106.8(6) ? ? ? yes N2 C6 C5 109.7(6) ? ? ? yes O3 C9 C10 108.8(5) ? ? ? yes N3 C10 C9 110.2(5) ? ? ? yes Cu1 N4 H31 113.9974 ? ? ? no Cu1 N4 H32 105.2801 ? ? ? no Cu1 N4 H33 121.3278 ? ? ? no H31 N4 H32 116.3579 ? ? ? no H31 N4 H33 97 ? ? ? no H32 N4 H33 103 ? ? ? no O1 C1 H1 109 ? ? ? no O1 C1 H2 109 ? ? ? no C2 C1 H1 109 ? ? ? no C2 C1 H2 108 ? ? ? no H1 C1 H2 110 ? ? ? no N1 C2 H3 108 ? ? ? no N1 C2 H4 108 ? ? ? no C1 C2 H3 109 ? ? ? no C1 C2 H4 109 ? ? ? no H3 C2 H4 110 ? ? ? no N1 C3 H5 109 ? ? ? no N1 C3 H6 110 ? ? ? no N1 C3 H7 109 ? ? ? no H5 C3 H6 110 ? ? ? no H5 C3 H7 109 ? ? ? no H6 C3 H7 110 ? ? ? no N1 C4 H8 109 ? ? ? no N1 C4 H9 109 ? ? ? no N1 C4 H10 109 ? ? ? no H8 C4 H9 110 ? ? ? no H8 C4 H10 110 ? ? ? no H9 C4 H10 110 ? ? ? no O2 C5 H11 110 ? ? ? no O2 C5 H12 110 ? ? ? no C6 C5 H11 110 ? ? ? no C6 C5 H12 111 ? ? ? no H11 C5 H12 109 ? ? ? no N2 C6 H13 110 ? ? ? no N2 C6 H14 110 ? ? ? no C5 C6 H13 109 ? ? ? no C5 C6 H14 109 ? ? ? no H13 C6 H14 109 ? ? ? no N2 C7 H15 110 ? ? ? no N2 C7 H16 109 ? ? ? no N2 C7 H17 110 ? ? ? no H15 C7 H16 109 ? ? ? no H15 C7 H17 110 ? ? ? no H16 C7 H17 109 ? ? ? no N2 C8 H18 109 ? ? ? no N2 C8 H19 109 ? ? ? no N2 C8 H20 110 ? ? ? no H18 C8 H19 109 ? ? ? no H18 C8 H20 110 ? ? ? no H19 C8 H20 110 ? ? ? no O3 C9 H21 109 ? ? ? no O3 C9 H22 110 ? ? ? no C10 C9 H21 109 ? ? ? no C10 C9 H22 110 ? ? ? no H21 C9 H22 109 ? ? ? no N3 C10 H23 109 ? ? ? no N3 C10 H24 109 ? ? ? no C9 C10 H23 109 ? ? ? no C9 C10 H24 110 ? ? ? no H23 C10 H24 109 ? ? ? no N3 C11 H25 109 ? ? ? no N3 C11 H26 109 ? ? ? no N3 C11 H27 109 ? ? ? no H25 C11 H26 110 ? ? ? no H25 C11 H27 110 ? ? ? no H26 C11 H27 110 ? ? ? no N3 C12 H28 110 ? ? ? no N3 C12 H29 109 ? ? ? no N3 C12 H30 109 ? ? ? no H28 C12 H29 110 ? ? ? no H28 C12 H30 110 ? ? ? no H29 C12 H30 108 ? ? ? no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Zn2 O2 Cu1 O1 . . . . 16.0(2) no Zn2 O2 Cu1 N2 . . . . -174.9(3) no Zn2 O2 Cu1 N4 . . . . 76(1) no Zn2 O2 C5 C6 . . . . -167.0(4) no Zn2 O3 Cu3 Cl3 . . . . -102.7(3) no Zn2 O3 Cu3 O1 . . . . -16.3(2) no Zn2 O3 Cu3 N3 . . . . 162.8(2) no Zn2 O3 C9 C10 . . . . -133.3(5) no Zn2 N1 C2 C1 . . . . 48.9(7) no Cu1 O1 Cu3 Cl3 . . . . -100.1(2) no Cu1 O1 Cu3 O3 . . . . 103.9(2) no Cu1 O1 Cu3 N3 . . . . 100.0(8) no Cu1 O1 C1 C2 . . . . -72.9(6) no Cu1 O2 Zn2 Cl2 . . . . 162.0(2) no Cu1 O2 Zn2 O3 . . . . 37.3(3) no Cu1 O2 Zn2 N1 . . . . -85.3(3) no Cu1 O2 C5 C6 . . . . 37.3(7) no Cu1 N2 C6 C5 . . . . 36.8(7) no Cu3 O1 Cu1 O2 . . . . -104.2(2) no Cu3 O1 Cu1 N2 . . . . -146.9(6) no Cu3 O1 Cu1 N4 . . . . 83.4(2) no Cu3 O1 C1 C2 . . . . 131.1(4) no Cu3 O3 Zn2 Cl2 . . . . -162.4(2) no Cu3 O3 Zn2 O2 . . . . -37.1(3) no Cu3 O3 Zn2 N1 . . . . 83.5(2) no Cu3 O3 C9 C10 . . . . 18.3(7) no Cu3 N3 C10 C9 . . . . 45.6(6) no Cl2 Zn2 O2 C5 . . . . 5.7(6) no Cl2 Zn2 O3 C9 . . . . -9.8(5) no Cl2 Zn2 N1 C2 . . . . 157.8(4) no Cl2 Zn2 N1 C3 . . . . -82.3(4) no Cl2 Zn2 N1 C4 . . . . 37.7(5) no Cl3 Cu3 O1 C1 . . . . 58.2(4) no Cl3 Cu3 O3 C9 . . . . 100.3(5) no Cl3 Cu3 N3 C10 . . . . 176.1(4) no Cl3 Cu3 N3 C11 . . . . 56.5(5) no Cl3 Cu3 N3 C12 . . . . -65.8(4) no O1 Cu1 O2 C5 . . . . 176.9(5) no O1 Cu1 N2 C6 . . . . 29.2(9) no O1 Cu1 N2 C7 . . . . -91.1(8) no O1 Cu1 N2 C8 . . . . 148.7(6) no O1 Cu3 O3 C9 . . . . -173.4(4) no O1 Cu3 N3 C10 . . . . -24(1) no O1 Cu3 N3 C11 . . . . -143.7(8) no O1 Cu3 N3 C12 . . . . 93.9(9) no O1 C1 C2 N1 . . . . -53.8(7) no O2 Zn2 O3 C9 . . . . 115.5(5) no O2 Zn2 N1 C2 . . . . 44.6(5) no O2 Zn2 N1 C3 . . . . 164.5(4) no O2 Zn2 N1 C4 . . . . -75.4(5) no O2 Cu1 O1 C1 . . . . 98.0(4) no O2 Cu1 N2 C6 . . . . -13.5(5) no O2 Cu1 N2 C7 . . . . -133.8(5) no O2 Cu1 N2 C8 . . . . 106.0(4) no O2 C5 C6 N2 . . . . -48.9(8) no O3 Zn2 O2 C5 . . . . -119.0(6) no O3 Zn2 N1 C2 . . . . -88.5(4) no O3 Zn2 N1 C3 . . . . 31.5(5) no O3 Zn2 N1 C4 . . . . 151.5(5) no O3 Cu3 O1 C1 . . . . -97.8(4) no O3 Cu3 N3 C10 . . . . -28.0(4) no O3 Cu3 N3 C11 . . . . -147.6(5) no O3 Cu3 N3 C12 . . . . 90.0(5) no O3 C9 C10 N3 . . . . -43.4(7) no N1 Zn2 O2 C5 . . . . 118.4(6) no N1 Zn2 O3 C9 . . . . -123.9(5) no N2 Cu1 O1 C1 . . . . 55.3(9) no N2 Cu1 O2 C5 . . . . -13.9(5) no N3 Cu3 O1 C1 . . . . -101.7(9) no N3 Cu3 O3 C9 . . . . 5.7(4) no N4 Cu1 O1 C1 . . . . -74.4(4) no N4 Cu1 O2 C5 . . . . -124(1) no N4 Cu1 N2 C6 . . . . 158.1(5) no N4 Cu1 N2 C7 . . . . 37.8(5) no N4 Cu1 N2 C8 . . . . -82.4(4) no C1 C2 N1 C3 . . . . -70.7(7) no C1 C2 N1 C4 . . . . 170.4(6) no C5 C6 N2 C7 . . . . 159.2(6) no C5 C6 N2 C8 . . . . -83.8(7) no C9 C10 N3 C11 . . . . 168.3(5) no C9 C10 N3 C12 . . . . -70.7(7) no #------------------------------------------------------------------------------ #===END #Compound 2 data_lena _database_code_CSD 159630 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H33 Br3 Cu2 N4 O3 Zn' _chemical_formula_weight 713.60 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.214(3) _cell_length_b 10.478(2) _cell_length_c 16.526(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.69(3) _cell_angle_gamma 90.00 _cell_volume 2412.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method ? _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 7.719 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3928 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 23.98 _reflns_number_total 3773 _reflns_number_observed 2555 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3762 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_obs 0.0679 _refine_ls_wR_factor_all 0.1966 _refine_ls_wR_factor_obs 0.1665 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Br1 Br 0.58275(8) 0.08736(11) 0.64092(8) 0.0468(4) Uani 1 d . . Br2 Br 0.75620(13) -0.07767(13) 0.99546(9) 0.0723(5) Uani 1 d . . Br3 Br 0.82536(11) 0.09720(14) 0.58305(9) 0.0639(4) Uani 1 d . . Cu1 Cu 0.64289(9) -0.16313(13) 0.65562(8) 0.0370(4) Uani 1 d . . Zn2 Zn 0.76985(9) -0.09496(12) 0.85514(8) 0.0394(4) Uani 1 d . . Cu3 Cu 0.78364(9) 0.09144(12) 0.70919(9) 0.0369(4) Uani 1 d . . O1 O 0.7754(5) -0.0949(6) 0.7100(4) 0.034(2) Uani 1 d . . O2 O 0.6613(6) -0.1921(9) 0.7750(5) 0.056(2) Uani 1 d . . O3 O 0.8067(5) 0.0745(7) 0.8324(5) 0.040(2) Uani 1 d . . N1 N 0.8844(8) -0.2181(9) 0.8736(6) 0.053(3) Uani 1 d . . N2 N 0.5216(6) -0.2714(9) 0.6269(6) 0.046(2) Uani 1 d . . N3 N 0.7971(7) 0.2821(9) 0.7372(6) 0.048(2) Uani 1 d . . N4 N 0.6436(6) -0.1526(9) 0.5362(5) 0.043(2) Uani 1 d . . H41N H 0.6606(6) -0.2202(9) 0.5121(5) 0.080 Uiso 1 d R . H42N H 0.6737(6) -0.0856(9) 0.5247(5) 0.080 Uiso 1 d R . H43N H 0.5814(6) -0.1401(9) 0.5005(5) 0.080 Uiso 1 d R . C1 C 0.8543(8) -0.1708(12) 0.7174(8) 0.048(3) Uani 1 d . . H1A H 0.9124(8) -0.1154(12) 0.7333(8) 0.080 Uiso 1 d R . H1B H 0.8417(8) -0.2122(12) 0.6593(8) 0.080 Uiso 1 d R . C2 C 0.8741(9) -0.2719(11) 0.7881(8) 0.053(3) Uani 1 d . . H2A H 0.8194(9) -0.3337(11) 0.7678(8) 0.080 Uiso 1 d R . H2B H 0.9338(9) -0.3201(11) 0.7960(8) 0.080 Uiso 1 d R . C3 C 0.9759(10) -0.1451(16) 0.9150(10) 0.080(5) Uani 1 d . . H3A H 1.0317(10) -0.2024(16) 0.9245(10) 0.080 Uiso 1 d R . H3B H 0.9756(10) -0.0734(16) 0.8750(10) 0.080 Uiso 1 d R . H3C H 0.9813(10) -0.1098(16) 0.9730(10) 0.080 Uiso 1 d R . C4 C 0.8860(14) -0.3261(14) 0.9312(10) 0.088(5) Uani 1 d . . H4A H 0.9413(14) -0.3838(14) 0.9393(10) 0.080 Uiso 1 d R . H4B H 0.8922(14) -0.2931(14) 0.9900(10) 0.080 Uiso 1 d R . H4C H 0.8246(14) -0.3747(14) 0.9031(10) 0.080 Uiso 1 d R . C5 C 0.5841(10) -0.2423(15) 0.7879(9) 0.071(4) Uani 1 d . . H5A H 0.5389(10) -0.1721(15) 0.7862(9) 0.080 Uiso 1 d R . H5B H 0.6049(10) -0.2876(15) 0.8459(9) 0.080 Uiso 1 d R . C6 C 0.5319(12) -0.3354(18) 0.7074(9) 0.093(6) Uani 1 d . . H6A H 0.5730(12) -0.4128(18) 0.7156(9) 0.080 Uiso 1 d R . H6B H 0.4677(12) -0.3631(18) 0.7044(9) 0.080 Uiso 1 d R . C7 C 0.5090(12) -0.3670(16) 0.5577(11) 0.087(5) Uani 1 d . . H7A H 0.4495(12) -0.4181(16) 0.5455(11) 0.080 Uiso 1 d R . H7B H 0.5035(12) -0.3216(16) 0.5026(11) 0.080 Uiso 1 d R . H7C H 0.5659(12) -0.4251(16) 0.5775(11) 0.080 Uiso 1 d R . C8 C 0.4342(9) -0.1934(15) 0.5924(11) 0.076(4) Uani 1 d . . H8A H 0.3766(9) -0.2488(15) 0.5792(11) 0.080 Uiso 1 d R . H8B H 0.4375(9) -0.1284(15) 0.6378(11) 0.080 Uiso 1 d R . H8C H 0.4293(9) -0.1491(15) 0.5371(11) 0.080 Uiso 1 d R . C9 C 0.8073(10) 0.1906(11) 0.8778(7) 0.052(3) Uani 1 d . . H9A H 0.8746(10) 0.2144(11) 0.9174(7) 0.080 Uiso 1 d R . H9B H 0.7693(10) 0.1798(11) 0.9146(7) 0.080 Uiso 1 d R . C10 C 0.7651(9) 0.2905(12) 0.8107(8) 0.052(3) Uani 1 d . . H10A H 0.6936(9) 0.2820(12) 0.7859(8) 0.080 Uiso 1 d R . H10B H 0.7823(9) 0.3763(12) 0.8392(8) 0.080 Uiso 1 d R . C11 C 0.7406(12) 0.3639(14) 0.6652(10) 0.080(5) Uani 1 d . . H11A H 0.7517(12) 0.4550(14) 0.6846(10) 0.080 Uiso 1 d R . H11B H 0.7598(12) 0.3506(14) 0.6146(10) 0.080 Uiso 1 d R . H11C H 0.6710(12) 0.3427(14) 0.6461(10) 0.080 Uiso 1 d R . C12 C 0.8965(10) 0.3190(16) 0.7661(11) 0.080(5) Uani 1 d . . H12A H 0.9037(10) 0.4123(16) 0.7799(11) 0.080 Uiso 1 d R . H12B H 0.9354(10) 0.2693(16) 0.8204(11) 0.080 Uiso 1 d R . H12C H 0.9196(10) 0.2999(16) 0.7186(11) 0.080 Uiso 1 d 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 Br1 0.0442(7) 0.0467(7) 0.0504(7) -0.0077(5) 0.0198(5) 0.0066(5) Br2 0.1327(14) 0.0528(8) 0.0544(8) -0.0108(6) 0.0615(9) -0.0170(8) Br3 0.0905(10) 0.0628(9) 0.0607(9) -0.0045(7) 0.0536(8) -0.0181(7) Cu1 0.0434(8) 0.0394(8) 0.0335(7) -0.0046(6) 0.0211(6) -0.0076(6) Zn2 0.0537(8) 0.0324(7) 0.0352(7) -0.0020(5) 0.0210(6) -0.0013(6) Cu3 0.0478(8) 0.0310(7) 0.0373(7) 0.0000(6) 0.0227(6) -0.0050(6) O1 0.041(4) 0.028(4) 0.029(4) -0.002(3) 0.010(3) 0.003(3) O2 0.068(5) 0.071(6) 0.036(4) -0.014(4) 0.027(4) -0.032(5) O3 0.058(5) 0.028(4) 0.033(4) -0.004(3) 0.016(3) 0.001(3) N1 0.075(7) 0.042(6) 0.040(5) 0.007(5) 0.020(5) 0.012(5) N2 0.049(6) 0.053(6) 0.042(5) -0.009(5) 0.024(5) -0.014(5) N3 0.070(7) 0.032(5) 0.042(5) -0.007(4) 0.024(5) -0.006(5) N4 0.051(6) 0.051(6) 0.036(5) -0.014(4) 0.027(4) -0.003(5) C1 0.043(7) 0.051(8) 0.051(7) -0.003(6) 0.019(6) 0.004(6) C2 0.076(9) 0.036(7) 0.053(7) -0.013(6) 0.031(7) 0.011(6) C3 0.068(10) 0.085(11) 0.070(10) -0.011(9) 0.011(8) 0.019(9) C4 0.153(16) 0.051(9) 0.069(10) 0.019(8) 0.056(10) 0.034(10) C5 0.077(10) 0.081(11) 0.067(9) -0.017(8) 0.043(8) -0.032(8) C6 0.107(12) 0.124(15) 0.049(8) 0.006(9) 0.032(8) -0.059(12) C7 0.097(12) 0.081(11) 0.078(11) -0.019(9) 0.032(9) -0.045(10) C8 0.048(8) 0.085(11) 0.106(12) 0.022(9) 0.042(8) -0.005(8) C9 0.082(9) 0.029(6) 0.040(6) -0.005(5) 0.019(6) 0.011(6) C10 0.068(8) 0.037(7) 0.052(7) -0.004(6) 0.024(6) -0.001(6) C11 0.115(13) 0.045(8) 0.079(11) 0.003(8) 0.036(9) -0.004(8) C12 0.065(10) 0.071(10) 0.106(12) -0.025(9) 0.036(9) -0.029(8) _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 Br1 Cu1 2.758(2) . ? Br1 Cu3 2.801(2) . ? Br2 Zn2 2.417(2) . ? Br3 Cu3 2.412(2) . ? Cu1 O2 1.902(7) . ? Cu1 O1 1.982(7) . ? Cu1 N4 1.981(8) . ? Cu1 N2 2.053(9) . ? Zn2 O2 1.939(8) . ? Zn2 O3 1.943(7) . ? Zn2 N1 2.090(10) . ? Zn2 O1 2.434(7) . ? Cu3 O3 1.930(7) . ? Cu3 O1 1.956(7) . ? Cu3 N3 2.042(9) . ? O1 C1 1.404(13) . ? O2 C5 1.380(14) . ? O3 C9 1.427(12) . ? N1 C4 1.47(2) . ? N1 C2 1.469(14) . ? N1 C3 1.49(2) . ? N2 C6 1.44(2) . ? N2 C8 1.47(2) . ? N2 C7 1.47(2) . ? N3 C11 1.44(2) . ? N3 C12 1.44(2) . ? N3 C10 1.48(2) . ? C1 C2 1.52(2) . ? C5 C6 1.58(2) . ? C9 C10 1.47(2) . ? 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 Cu1 Br1 Cu3 73.10(5) . . ? O2 Cu1 O1 83.6(3) . . ? O2 Cu1 N4 169.9(4) . . ? O1 Cu1 N4 91.2(3) . . ? O2 Cu1 N2 84.0(3) . . ? O1 Cu1 N2 163.9(3) . . ? N4 Cu1 N2 99.4(4) . . ? O2 Cu1 Br1 98.6(3) . . ? O1 Cu1 Br1 86.4(2) . . ? N4 Cu1 Br1 89.6(3) . . ? N2 Cu1 Br1 105.7(3) . . ? O2 Zn2 O3 125.5(3) . . ? O2 Zn2 N1 101.9(4) . . ? O3 Zn2 N1 107.7(4) . . ? O2 Zn2 Br2 108.5(2) . . ? O3 Zn2 Br2 105.1(2) . . ? N1 Zn2 Br2 107.1(3) . . ? O2 Zn2 O1 71.6(3) . . ? O3 Zn2 O1 71.4(3) . . ? N1 Zn2 O1 77.7(3) . . ? Br2 Zn2 O1 174.9(2) . . ? O3 Cu3 O1 83.4(3) . . ? O3 Cu3 N3 83.8(3) . . ? O1 Cu3 N3 167.3(3) . . ? O3 Cu3 Br3 156.1(2) . . ? O1 Cu3 Br3 94.1(2) . . ? N3 Cu3 Br3 97.7(3) . . ? O3 Cu3 Br1 97.5(2) . . ? O1 Cu3 Br1 85.7(2) . . ? N3 Cu3 Br1 95.7(3) . . ? Br3 Cu3 Br1 106.01(7) . . ? C1 O1 Cu3 120.7(7) . . ? C1 O1 Cu1 120.9(6) . . ? Cu3 O1 Cu1 114.4(3) . . ? C1 O1 Zn2 106.3(6) . . ? Cu3 O1 Zn2 92.0(3) . . ? Cu1 O1 Zn2 90.9(3) . . ? C5 O2 Cu1 116.2(8) . . ? C5 O2 Zn2 129.7(7) . . ? Cu1 O2 Zn2 110.8(4) . . ? C9 O3 Cu3 115.8(6) . . ? C9 O3 Zn2 128.2(7) . . ? Cu3 O3 Zn2 110.1(3) . . ? C4 N1 C2 107.1(10) . . ? C4 N1 C3 109.1(12) . . ? C2 N1 C3 110.9(10) . . ? C4 N1 Zn2 111.4(9) . . ? C2 N1 Zn2 109.6(7) . . ? C3 N1 Zn2 108.7(8) . . ? C6 N2 C8 111.3(11) . . ? C6 N2 C7 109.4(12) . . ? C8 N2 C7 105.2(11) . . ? C6 N2 Cu1 106.8(8) . . ? C8 N2 Cu1 111.8(8) . . ? C7 N2 Cu1 112.3(8) . . ? C11 N3 C12 108.3(12) . . ? C11 N3 C10 111.0(11) . . ? C12 N3 C10 111.0(10) . . ? C11 N3 Cu3 115.0(8) . . ? C12 N3 Cu3 109.5(8) . . ? C10 N3 Cu3 102.0(7) . . ? O1 C1 C2 111.2(9) . . ? N1 C2 C1 112.6(9) . . ? O2 C5 C6 106.0(11) . . ? N2 C6 C5 108.7(12) . . ? O3 C9 C10 107.6(9) . . ? C9 C10 N3 112.8(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu3 Br1 Cu1 O2 86.7(2) . . . . ? Cu3 Br1 Cu1 O1 3.8(2) . . . . ? Cu3 Br1 Cu1 N4 -87.4(3) . . . . ? Cu3 Br1 Cu1 N2 172.9(3) . . . . ? Cu1 Br1 Cu3 O3 -86.6(2) . . . . ? Cu1 Br1 Cu3 O1 -3.8(2) . . . . ? Cu1 Br1 Cu3 N3 -171.1(3) . . . . ? Cu1 Br1 Cu3 Br3 89.18(6) . . . . ? O3 Cu3 O1 C1 -98.6(7) . . . . ? N3 Cu3 O1 C1 -99.6(18) . . . . ? Br3 Cu3 O1 C1 57.6(7) . . . . ? Br1 Cu3 O1 C1 163.4(7) . . . . ? O3 Cu3 O1 Cu1 103.6(4) . . . . ? N3 Cu3 O1 Cu1 102.6(16) . . . . ? Br3 Cu3 O1 Cu1 -100.2(3) . . . . ? Br1 Cu3 O1 Cu1 5.6(3) . . . . ? O3 Cu3 O1 Zn2 11.8(3) . . . . ? N3 Cu3 O1 Zn2 10.7(17) . . . . ? Br3 Cu3 O1 Zn2 167.9(2) . . . . ? Br1 Cu3 O1 Zn2 -86.3(2) . . . . ? O2 Cu1 O1 C1 97.5(8) . . . . ? N4 Cu1 O1 C1 -73.9(8) . . . . ? N2 Cu1 O1 C1 57.5(15) . . . . ? Br1 Cu1 O1 C1 -163.4(7) . . . . ? O2 Cu1 O1 Cu3 -104.7(4) . . . . ? N4 Cu1 O1 Cu3 83.9(4) . . . . ? N2 Cu1 O1 Cu3 -144.8(10) . . . . ? Br1 Cu1 O1 Cu3 -5.7(3) . . . . ? O2 Cu1 O1 Zn2 -12.1(3) . . . . ? N4 Cu1 O1 Zn2 176.5(3) . . . . ? N2 Cu1 O1 Zn2 -52.2(12) . . . . ? Br1 Cu1 O1 Zn2 86.9(2) . . . . ? O2 Zn2 O1 C1 -110.2(7) . . . . ? O3 Zn2 O1 C1 110.6(7) . . . . ? N1 Zn2 O1 C1 -3.0(7) . . . . ? Br2 Zn2 O1 C1 158.3(17) . . . . ? O2 Zn2 O1 Cu3 126.9(4) . . . . ? O3 Zn2 O1 Cu3 -12.2(3) . . . . ? N1 Zn2 O1 Cu3 -125.9(4) . . . . ? Br2 Zn2 O1 Cu3 35.4(20) . . . . ? O2 Zn2 O1 Cu1 12.5(3) . . . . ? O3 Zn2 O1 Cu1 -126.7(3) . . . . ? N1 Zn2 O1 Cu1 119.6(4) . . . . ? Br2 Zn2 O1 Cu1 -79.1(19) . . . . ? O1 Cu1 O2 C5 177.8(10) . . . . ? N4 Cu1 O2 C5 -123.4(21) . . . . ? N2 Cu1 O2 C5 -12.6(10) . . . . ? Br1 Cu1 O2 C5 92.4(10) . . . . ? O1 Cu1 O2 Zn2 16.4(4) . . . . ? N4 Cu1 O2 Zn2 75.1(22) . . . . ? N2 Cu1 O2 Zn2 -174.0(5) . . . . ? Br1 Cu1 O2 Zn2 -69.0(4) . . . . ? O3 Zn2 O2 C5 -122.5(12) . . . . ? N1 Zn2 O2 C5 115.4(12) . . . . ? Br2 Zn2 O2 C5 2.5(13) . . . . ? O1 Zn2 O2 C5 -172.1(13) . . . . ? O3 Zn2 O2 Cu1 35.6(6) . . . . ? N1 Zn2 O2 Cu1 -86.5(5) . . . . ? Br2 Zn2 O2 Cu1 160.7(3) . . . . ? O1 Zn2 O2 Cu1 -13.9(4) . . . . ? O1 Cu3 O3 C9 -171.1(8) . . . . ? N3 Cu3 O3 C9 8.6(8) . . . . ? Br3 Cu3 O3 C9 103.7(9) . . . . ? Br1 Cu3 O3 C9 -86.4(8) . . . . ? O1 Cu3 O3 Zn2 -15.8(3) . . . . ? N3 Cu3 O3 Zn2 164.0(4) . . . . ? Br3 Cu3 O3 Zn2 -101.0(6) . . . . ? Br1 Cu3 O3 Zn2 69.0(3) . . . . ? O2 Zn2 O3 C9 115.1(9) . . . . ? N1 Zn2 O3 C9 -125.3(9) . . . . ? Br2 Zn2 O3 C9 -11.4(9) . . . . ? O1 Zn2 O3 C9 164.7(9) . . . . ? O2 Zn2 O3 Cu3 -36.4(6) . . . . ? N1 Zn2 O3 Cu3 83.2(4) . . . . ? Br2 Zn2 O3 Cu3 -162.9(3) . . . . ? O1 Zn2 O3 Cu3 13.2(3) . . . . ? O2 Zn2 N1 C4 -74.1(9) . . . . ? O3 Zn2 N1 C4 152.3(9) . . . . ? Br2 Zn2 N1 C4 39.7(10) . . . . ? O1 Zn2 N1 C4 -142.0(10) . . . . ? O2 Zn2 N1 C2 44.2(8) . . . . ? O3 Zn2 N1 C2 -89.4(8) . . . . ? Br2 Zn2 N1 C2 158.1(7) . . . . ? O1 Zn2 N1 C2 -23.7(7) . . . . ? O2 Zn2 N1 C3 165.6(8) . . . . ? O3 Zn2 N1 C3 32.0(9) . . . . ? Br2 Zn2 N1 C3 -80.5(8) . . . . ? O1 Zn2 N1 C3 97.8(8) . . . . ? O2 Cu1 N2 C6 -15.4(10) . . . . ? O1 Cu1 N2 C6 24.6(18) . . . . ? N4 Cu1 N2 C6 155.0(10) . . . . ? Br1 Cu1 N2 C6 -112.7(10) . . . . ? O2 Cu1 N2 C8 106.6(9) . . . . ? O1 Cu1 N2 C8 146.7(12) . . . . ? N4 Cu1 N2 C8 -82.9(9) . . . . ? Br1 Cu1 N2 C8 9.4(9) . . . . ? O2 Cu1 N2 C7 -135.4(10) . . . . ? O1 Cu1 N2 C7 -95.3(14) . . . . ? N4 Cu1 N2 C7 35.1(10) . . . . ? Br1 Cu1 N2 C7 127.4(9) . . . . ? O3 Cu3 N3 C11 -148.5(10) . . . . ? O1 Cu3 N3 C11 -147.5(15) . . . . ? Br3 Cu3 N3 C11 55.4(10) . . . . ? Br1 Cu3 N3 C11 -51.6(10) . . . . ? O3 Cu3 N3 C12 89.3(9) . . . . ? O1 Cu3 N3 C12 90.4(19) . . . . ? Br3 Cu3 N3 C12 -66.7(9) . . . . ? Br1 Cu3 N3 C12 -173.7(9) . . . . ? O3 Cu3 N3 C10 -28.3(7) . . . . ? O1 Cu3 N3 C10 -27.2(21) . . . . ? Br3 Cu3 N3 C10 175.7(7) . . . . ? Br1 Cu3 N3 C10 68.7(7) . . . . ? Cu3 O1 C1 C2 130.9(8) . . . . ? Cu1 O1 C1 C2 -72.7(10) . . . . ? Zn2 O1 C1 C2 28.4(10) . . . . ? C4 N1 C2 C1 170.1(12) . . . . ? C3 N1 C2 C1 -70.9(13) . . . . ? Zn2 N1 C2 C1 49.1(12) . . . . ? O1 C1 C2 N1 -53.2(13) . . . . ? Cu1 O2 C5 C6 34.6(15) . . . . ? Zn2 O2 C5 C6 -168.2(10) . . . . ? C8 N2 C6 C5 -85.9(15) . . . . ? C7 N2 C6 C5 158.2(13) . . . . ? Cu1 N2 C6 C5 36.5(15) . . . . ? O2 C5 C6 N2 -46.6(18) . . . . ? Cu3 O3 C9 C10 14.4(13) . . . . ? Zn2 O3 C9 C10 -135.7(9) . . . . ? O3 C9 C10 N3 -41.0(14) . . . . ? C11 N3 C10 C9 168.5(11) . . . . ? C12 N3 C10 C9 -71.0(14) . . . . ? Cu3 N3 C10 C9 45.5(11) . . . . ? _refine_diff_density_max 1.744 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.219 #===END #Compound 3 data_pr9905 _database_code_CSD 159631 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H33 Cu2 N7 O3 S3 Zn' _chemical_formula_weight 672.13 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmc2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 14.288(3) _cell_length_b 19.827(4) _cell_length_c 10.079(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2855.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description Block _exptl_crystal_colour 'Dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 2.559 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.6286 _exptl_absorpt_correction_T_max 0.7839 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method 'Omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2703 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2703 _reflns_number_gt 1789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction TeXsan _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 2703 _refine_ls_number_parameters 176 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.296 _refine_ls_shift/su_mean 0.014 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 Cu1 Cu 0.38082(9) -0.67486(5) -0.46769(12) 0.0318(3) Uani 1 1 d . . . Zn2 Zn 0.5000 -0.57564(8) -0.29250(17) 0.0270(4) Uani 1 2 d S . . O1 O 0.5000 -0.6889(4) -0.3731(9) 0.032(3) Uani 1 2 d S . . C1 C 0.5000 -0.7301(6) -0.2626(15) 0.031(4) Uani 1 2 d SD . . H1 H 0.537(5) -0.771(2) -0.262(9) 0.037 Uiso 1 1 d D . . C2 C 0.4572(13) -0.6962(9) -0.148(2) 0.035(5) Uani 0.50 1 d P A -1 H2A H 0.3898 -0.6892 -0.1661 0.042 Uiso 0.50 1 calc PR A -1 H2B H 0.4624 -0.7260 -0.0695 0.042 Uiso 0.50 1 calc PR A -1 C2' C 0.5426 -0.6976 -0.1477 0.033 Uiso 0.00 1 d P A -2 H2'A H 0.6103 -0.6914 -0.1646 0.040 Uiso 0.00 1 calc PR A -2 H2'B H 0.5358 -0.7276 -0.0697 0.040 Uiso 0.00 1 calc PR A -2 N1 N 0.5000 -0.6312(5) -0.1169(11) 0.029(3) Uani 1 2 d S . . C3 C 0.4196(9) -0.6126(10) -0.0402(14) 0.112(7) Uani 1 1 d . A . H3A H 0.4103 -0.6455 0.0312 0.168 Uiso 1 1 calc R . . H3B H 0.3642 -0.6119 -0.0974 0.168 Uiso 1 1 calc R . . H3C H 0.4293 -0.5678 -0.0017 0.168 Uiso 1 1 calc R . . O2 O 0.3867(5) -0.5865(3) -0.3930(7) 0.0327(18) Uani 1 1 d . . . C4 C 0.3031(7) -0.5477(5) -0.4059(10) 0.037(3) Uani 1 1 d . A . H4A H 0.3180 -0.4989 -0.4090 0.044 Uiso 1 1 calc R . . H4B H 0.2609 -0.5560 -0.3297 0.044 Uiso 1 1 calc R . . C5 C 0.2570(8) -0.5696(5) -0.5336(10) 0.038(3) Uani 1 1 d . . . H5A H 0.1922 -0.5521 -0.5371 0.045 Uiso 1 1 calc R A . H5B H 0.2919 -0.5510 -0.6101 0.045 Uiso 1 1 calc R . . N2 N 0.2557(6) -0.6453(4) -0.5415(9) 0.037(2) Uani 1 1 d . A . C6 C 0.1806(7) -0.6713(5) -0.4542(15) 0.052(3) Uani 1 1 d . . . H6A H 0.1201 -0.6536 -0.4839 0.079 Uiso 1 1 calc R A . H6B H 0.1924 -0.6569 -0.3627 0.079 Uiso 1 1 calc R . . H6C H 0.1797 -0.7207 -0.4582 0.079 Uiso 1 1 calc R . . C7 C 0.2370(7) -0.6660(6) -0.6810(11) 0.046(3) Uani 1 1 d . . . H7A H 0.1766 -0.6475 -0.7096 0.069 Uiso 1 1 calc R A . H7B H 0.2352 -0.7153 -0.6866 0.069 Uiso 1 1 calc R . . H7C H 0.2868 -0.6487 -0.7387 0.069 Uiso 1 1 calc R . . N10 N 0.3595(7) -0.7683(4) -0.4992(10) 0.049(3) Uani 1 1 d . . . C10 C 0.3512(7) -0.8246(6) -0.5289(10) 0.037(3) Uani 1 1 d . A . S1 S 0.3393(2) -0.90412(14) -0.5657(4) 0.0582(10) Uani 1 1 d . . . N20 N 0.5000 -0.4801(6) -0.2282(13) 0.039(4) Uani 1 2 d S . . C20 C 0.5000 -0.4223(8) -0.2069(14) 0.032(4) Uani 1 2 d S A . S2 S 0.5000 -0.34069(17) -0.1836(4) 0.0362(10) Uani 1 2 d S . . N50 N 0.5000 0.0836(9) -0.147(2) 0.081(6) Uani 1 2 d S . . C51 C 0.5000 0.0459(11) -0.227(2) 0.065(6) Uani 1 2 d S . . C52 C 0.5000 -0.0081(12) -0.326(2) 0.085(7) Uani 1 2 d S . . H52A H 0.5155 0.0107 -0.4133 0.127 Uiso 0.50 1 calc PR . . H52B H 0.4379 -0.0289 -0.3295 0.127 Uiso 0.50 1 calc PR . . H52C H 0.5466 -0.0421 -0.3016 0.127 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0426(7) 0.0200(5) 0.0328(6) -0.0025(6) -0.0052(8) -0.0034(6) Zn2 0.0356(10) 0.0224(8) 0.0228(8) -0.0045(8) 0.000 0.000 O1 0.052(7) 0.022(5) 0.023(5) 0.002(4) 0.000 0.000 C1 0.048(10) 0.006(6) 0.038(10) 0.010(6) 0.000 0.000 C2 0.032(12) 0.039(12) 0.033(11) 0.008(9) 0.006(10) -0.012(9) N1 0.032(7) 0.023(6) 0.031(7) 0.000(5) 0.000 0.000 C3 0.049(9) 0.24(2) 0.052(9) 0.057(12) 0.017(8) 0.034(12) O2 0.032(4) 0.019(3) 0.047(5) -0.005(3) -0.011(4) 0.004(3) C4 0.033(7) 0.035(6) 0.043(6) -0.003(5) -0.004(5) -0.004(5) C5 0.048(7) 0.025(5) 0.041(6) 0.001(5) -0.008(6) -0.003(5) N2 0.043(6) 0.031(5) 0.037(5) -0.004(4) -0.001(5) -0.017(4) C6 0.041(6) 0.044(6) 0.073(9) 0.004(7) -0.009(9) -0.007(6) C7 0.035(7) 0.047(7) 0.056(8) -0.011(6) -0.016(6) -0.009(6) N10 0.076(8) 0.020(4) 0.052(7) -0.006(5) 0.003(6) -0.016(5) C10 0.018(5) 0.052(7) 0.040(6) 0.011(6) -0.009(5) 0.008(5) S1 0.065(2) 0.0259(15) 0.083(3) -0.0141(16) -0.007(2) -0.0014(15) N20 0.053(9) 0.035(9) 0.030(7) -0.006(7) 0.000 0.000 C20 0.032(9) 0.039(9) 0.024(8) 0.002(8) 0.000 0.000 S2 0.058(3) 0.0233(19) 0.027(2) -0.0031(16) 0.000 0.000 N50 0.037(10) 0.090(14) 0.118(18) -0.003(13) 0.000 0.000 C51 0.059(14) 0.067(14) 0.071(15) -0.005(12) 0.000 0.000 C52 0.095(17) 0.096(17) 0.063(16) 0.006(14) 0.000 0.000 _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 Cu1 N10 1.904(8) . ? Cu1 O2 1.910(6) . ? Cu1 O1 1.971(5) . ? Cu1 N2 2.023(9) . ? Cu1 S2 2.781(3) 2_644 ? Zn2 O2 1.921(7) . ? Zn2 O2 1.921(7) 4_655 ? Zn2 N20 2.002(12) . ? Zn2 N1 2.085(11) . ? Zn2 O1 2.387(9) . ? O1 C1 1.381(16) . ? O1 Cu1 1.971(5) 4_655 ? C1 C2' 1.457(14) . ? C1 C2 1.47(2) . ? C1 C2 1.47(2) 4_655 ? C2 N1 1.46(2) . ? C2' N1 1.483(10) . ? N1 C3 1.433(15) 4_655 ? N1 C3 1.433(15) . ? N1 C2 1.46(2) 4_655 ? O2 C4 1.428(12) . ? C4 C5 1.510(13) . ? C5 N2 1.502(11) . ? N2 C6 1.481(14) . ? N2 C7 1.489(13) . ? N10 C10 1.163(13) . ? C10 S1 1.628(12) . ? N20 C20 1.166(18) . ? C20 S2 1.635(16) . ? S2 Cu1 2.781(3) 3_545 ? S2 Cu1 2.781(3) 2_645 ? N50 C51 1.10(2) . ? C51 C52 1.46(3) . ? 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 N10 Cu1 O2 165.0(4) . . ? N10 Cu1 O1 94.7(4) . . ? O2 Cu1 O1 84.3(3) . . ? N10 Cu1 N2 94.6(4) . . ? O2 Cu1 N2 85.3(3) . . ? O1 Cu1 N2 169.1(4) . . ? N10 Cu1 S2 94.3(3) . 2_644 ? O2 Cu1 S2 100.3(2) . 2_644 ? O1 Cu1 S2 82.3(3) . 2_644 ? N2 Cu1 S2 102.8(3) . 2_644 ? O2 Zn2 O2 114.8(4) . 4_655 ? O2 Zn2 N20 106.0(3) . . ? O2 Zn2 N20 106.0(3) 4_655 . ? O2 Zn2 N1 112.9(2) . . ? O2 Zn2 N1 112.9(2) 4_655 . ? N20 Zn2 N1 103.0(5) . . ? O2 Zn2 O1 73.5(2) . . ? O2 Zn2 O1 73.5(2) 4_655 . ? N20 Zn2 O1 179.0(5) . . ? N1 Zn2 O1 78.0(4) . . ? C1 O1 Cu1 118.3(3) . . ? C1 O1 Cu1 118.3(3) . 4_655 ? Cu1 O1 Cu1 119.5(5) . 4_655 ? C1 O1 Zn2 106.4(8) . . ? Cu1 O1 Zn2 91.8(3) . . ? Cu1 O1 Zn2 91.8(3) 4_655 . ? O1 C1 C2' 112.3(9) . . ? O1 C1 C2 111.3(11) . . ? C2' C1 C2 49.3(9) . . ? O1 C1 C2 111.3(11) . 4_655 ? C2' C1 C2 1.0(7) . 4_655 ? C2 C1 C2 49.2(16) . 4_655 ? N1 C2 C1 113.4(13) . . ? C1 C2' N1 112.8(5) . . ? C3 N1 C3 106.6(15) 4_655 . ? C3 N1 C2 90.4(11) 4_655 4_655 ? C3 N1 C2 132.7(13) . 4_655 ? C3 N1 C2 132.7(13) 4_655 . ? C3 N1 C2 90.4(11) . . ? C2 N1 C2 49.6(16) 4_655 . ? C3 N1 C2' 90.7(9) 4_655 . ? C3 N1 C2' 132.1(10) . . ? C2 N1 C2' 0.7(8) 4_655 . ? C2 N1 C2' 49.0(8) . . ? C3 N1 Zn2 108.8(8) 4_655 . ? C3 N1 Zn2 108.8(8) . . ? C2 N1 Zn2 106.5(10) 4_655 . ? C2 N1 Zn2 106.5(10) . . ? C2' N1 Zn2 106.9(6) . . ? C4 O2 Cu1 114.9(6) . . ? C4 O2 Zn2 133.9(6) . . ? Cu1 O2 Zn2 110.3(3) . . ? O2 C4 C5 106.7(8) . . ? N2 C5 C4 109.8(8) . . ? C6 N2 C7 109.6(8) . . ? C6 N2 C5 109.0(8) . . ? C7 N2 C5 109.1(8) . . ? C6 N2 Cu1 108.7(7) . . ? C7 N2 Cu1 115.3(7) . . ? C5 N2 Cu1 105.0(6) . . ? C10 N10 Cu1 173.8(9) . . ? N10 C10 S1 178.2(10) . . ? C20 N20 Zn2 171.8(13) . . ? N20 C20 S2 177.6(14) . . ? C20 S2 Cu1 102.8(4) . 3_545 ? C20 S2 Cu1 102.8(4) . 2_645 ? Cu1 S2 Cu1 75.53(11) 3_545 2_645 ? N50 C51 C52 176(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.689 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.129