# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- check cif.cif' _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jian Zhang' _publ_contact_author_email zhj@fjirsm.ac.cn loop_ _publ_author_name 'Jian Zhang' 'Hui Yang' 'Fei Wang' 'Yao Kang' data_1 #TrackingRef '- check cif.cif' _database_code_depnum_ccdc_archive 'CCDC 868807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C79 H79 N9 O42 Zn9' _chemical_formula_sum 'C79 H79 N9 O42 Zn9' _chemical_formula_weight 2415.04 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I23 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' '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+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, 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+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, 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+1/2, x+1/2' _cell_length_a 23.3024(2) _cell_length_b 23.3024(2) _cell_length_c 23.3024(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12653.25(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1428 _cell_measurement_theta_min 2.7586 _cell_measurement_theta_max 27.9115 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4360 _exptl_absorpt_coefficient_mu 1.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6234 _exptl_absorpt_correction_T_max 0.6234 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5486 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3492 _reflns_number_gt 2900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'XPREP in SHELXTL (Siemens, 1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1437P)^2^+5.6095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 3492 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2130 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Zn1 Zn 0.0000 0.5000 0.06322(4) 0.0281(3) Uani 1 2 d S . . Zn2 Zn 0.17884(6) 0.29240(5) 0.23701(5) 0.0589(4) Uani 1 1 d . . . O1 O 0.0544(3) 0.4359(3) 0.0466(3) 0.0522(16) Uani 1 1 d . . . O2 O 0.0649(3) 0.4421(3) -0.0479(2) 0.0491(15) Uani 1 1 d . . . O3 O 0.1690(3) 0.3044(3) 0.1555(3) 0.066(2) Uani 1 1 d . . . O4 O 0.2429(3) 0.2580(4) 0.1148(3) 0.072(2) Uani 1 1 d . . . O5 O 0.2625(5) 0.2665(5) -0.0986(5) 0.116(4) Uani 1 1 d . . . O6 O 0.2131(3) 0.3321(4) -0.1438(3) 0.066(2) Uani 1 1 d . . . O7 O 0.0000 0.5000 0.1468(3) 0.0386(16) Uiso 1 2 d S . . O8 O 0.2511(3) 0.2511(3) 0.2511(3) 0.044(2) Uani 1 3 d S . . C1 C 0.1222(3) 0.3771(3) 0.0015(5) 0.0421(18) Uani 1 1 d . . . C2 C 0.1372(4) 0.3523(4) 0.0532(4) 0.043(2) Uani 1 1 d . . . H2A H 0.1182 0.3629 0.0867 0.052 Uiso 1 1 calc R . . C3 C 0.1810(4) 0.3113(4) 0.0551(4) 0.045(2) Uani 1 1 d . . . C4 C 0.2080(4) 0.2931(4) 0.0076(4) 0.054(2) Uani 1 1 d . . . H4A H 0.2352 0.2639 0.0094 0.065 Uiso 1 1 calc R . . C5 C 0.1939(4) 0.3197(4) -0.0461(4) 0.050(2) Uani 1 1 d . . . C6 C 0.1504(4) 0.3601(4) -0.0489(4) 0.050(2) Uani 1 1 d . . . H6A H 0.1399 0.3758 -0.0841 0.060 Uiso 1 1 calc R . . C7 C 0.0763(3) 0.4218(3) -0.0019(5) 0.0395(18) Uani 1 1 d . . . C8 C 0.1981(4) 0.2894(4) 0.1153(4) 0.051(2) Uani 1 1 d . . . C9 C 0.2249(5) 0.3015(5) -0.1001(5) 0.064(3) Uani 1 1 d . . . C10 C 0.0090(6) 0.5344(8) 0.1780(8) 0.059(5) Uiso 0.50 1 d PD . . C11 C 0.0795(11) 0.6174(9) 0.2072(16) 0.122(11) Uiso 0.50 1 d PD . . C12 C 0.0228(13) 0.6468(15) 0.1996(16) 0.144(14) Uiso 0.50 1 d PD . . C13 C -0.0238(11) 0.6244(11) 0.2379(12) 0.111(10) Uiso 0.50 1 d PD . . C14 C 0.1105(11) 0.5143(11) 0.1717(12) 0.095(9) Uiso 0.50 1 d PD . . C15 C -0.0934(9) 0.5501(11) 0.1835(11) 0.083(7) Uiso 0.50 1 d PD . . N1 N 0.0665(7) 0.5559(8) 0.1930(9) 0.077(5) Uiso 0.50 1 d PD . . N2 N -0.0359(7) 0.5729(8) 0.2010(10) 0.089(6) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0256(6) 0.0342(6) 0.0246(5) 0.000 0.000 0.0025(6) Zn2 0.0850(9) 0.0345(6) 0.0572(7) 0.0009(5) 0.0296(6) 0.0024(6) O1 0.052(4) 0.064(4) 0.041(3) 0.005(3) 0.008(3) 0.023(3) O2 0.047(3) 0.061(4) 0.040(3) 0.019(3) 0.007(3) 0.028(3) O3 0.070(5) 0.079(5) 0.048(4) 0.012(3) 0.021(3) 0.030(4) O4 0.069(5) 0.087(6) 0.061(4) 0.007(4) -0.010(4) 0.050(4) O5 0.098(7) 0.144(10) 0.105(8) -0.009(7) 0.027(6) 0.066(7) O6 0.065(5) 0.084(5) 0.048(4) -0.018(4) 0.008(3) 0.013(4) O8 0.044(2) 0.044(2) 0.044(2) -0.007(2) -0.007(2) -0.007(2) C1 0.042(4) 0.034(4) 0.050(5) 0.004(4) -0.007(5) 0.002(3) C2 0.038(5) 0.050(5) 0.042(5) -0.002(4) 0.006(4) 0.020(4) C3 0.048(5) 0.047(5) 0.039(5) 0.007(4) 0.002(4) 0.016(4) C4 0.044(5) 0.065(6) 0.053(6) -0.012(5) 0.003(4) 0.027(4) C5 0.052(5) 0.058(6) 0.041(5) 0.004(4) -0.001(4) 0.023(4) C6 0.049(5) 0.058(6) 0.042(5) 0.008(4) 0.003(4) 0.013(4) C7 0.021(3) 0.047(4) 0.050(5) 0.011(5) 0.010(4) 0.005(3) C8 0.051(6) 0.045(5) 0.057(6) 0.012(4) -0.006(5) 0.008(4) C9 0.058(6) 0.081(8) 0.052(6) -0.001(6) 0.023(5) 0.025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O7 1.947(7) . ? Zn1 O1 1.998(6) . ? Zn1 O1 1.998(6) 2_565 ? Zn1 O2 2.057(6) 3 ? Zn1 O2 2.057(6) 4_565 ? Zn1 Zn1 2.947(2) 3 ? Zn2 O6 1.905(7) 22 ? Zn2 O3 1.934(7) . ? Zn2 O4 1.948(7) 5 ? Zn2 O8 1.967(4) . ? O1 C7 1.283(11) . ? O2 C7 1.203(11) . ? O2 Zn1 2.057(6) 3 ? O3 C8 1.207(12) . ? O4 C8 1.276(12) . ? O4 Zn2 1.948(7) 9 ? O5 C9 1.197(14) . ? O6 C9 1.274(14) . ? O6 Zn2 1.905(7) 19_554 ? O7 C10 1.102(18) . ? O7 C10 1.102(18) 2_565 ? O8 Zn2 1.967(4) 9 ? O8 Zn2 1.967(4) 5 ? C1 C2 1.383(14) . ? C1 C6 1.403(14) . ? C1 C7 1.495(10) . ? C2 C3 1.400(12) . ? C2 H2A 0.9300 . ? C3 C4 1.343(12) . ? C3 C8 1.544(13) . ? C4 C5 1.435(13) . ? C4 H4A 0.9300 . ? C5 C6 1.383(13) . ? C5 C9 1.512(13) . ? C6 H6A 0.9300 . ? C10 N1 1.472(10) . ? C10 N2 1.480(10) . ? C10 C10 1.66(4) 2_565 ? C11 C12 1.498(10) . ? C11 N1 1.501(10) . ? C12 C13 1.499(10) . ? C13 N2 1.502(10) . ? C14 N1 1.497(10) . ? C14 C15 1.58(4) 2_565 ? C15 N2 1.497(10) . ? C15 C14 1.58(4) 2_565 ? 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 O7 Zn1 O1 101.16(17) . . ? O7 Zn1 O1 101.16(17) . 2_565 ? O1 Zn1 O1 157.7(3) . 2_565 ? O7 Zn1 O2 99.97(16) . 3 ? O1 Zn1 O2 86.7(3) . 3 ? O1 Zn1 O2 89.4(3) 2_565 3 ? O7 Zn1 O2 99.97(16) . 4_565 ? O1 Zn1 O2 89.4(3) . 4_565 ? O1 Zn1 O2 86.7(3) 2_565 4_565 ? O2 Zn1 O2 160.1(3) 3 4_565 ? O7 Zn1 Zn1 180.0 . 3 ? O1 Zn1 Zn1 78.84(17) . 3 ? O1 Zn1 Zn1 78.84(17) 2_565 3 ? O2 Zn1 Zn1 80.03(16) 3 3 ? O2 Zn1 Zn1 80.03(16) 4_565 3 ? O6 Zn2 O3 118.1(3) 22 . ? O6 Zn2 O4 101.9(4) 22 5 ? O3 Zn2 O4 104.0(4) . 5 ? O6 Zn2 O8 113.2(4) 22 . ? O3 Zn2 O8 109.6(3) . . ? O4 Zn2 O8 109.0(3) 5 . ? C7 O1 Zn1 127.9(5) . . ? C7 O2 Zn1 125.1(5) . 3 ? C8 O3 Zn2 130.9(6) . . ? C8 O4 Zn2 128.4(7) . 9 ? C9 O6 Zn2 114.7(6) . 19_554 ? C10 O7 C10 97(2) . 2_565 ? C10 O7 Zn1 131.3(11) . . ? C10 O7 Zn1 131.3(11) 2_565 . ? Zn2 O8 Zn2 110.9(3) 9 5 ? Zn2 O8 Zn2 110.9(3) 9 . ? Zn2 O8 Zn2 110.9(3) 5 . ? C2 C1 C6 119.6(7) . . ? C2 C1 C7 121.1(9) . . ? C6 C1 C7 119.3(9) . . ? C1 C2 C3 119.8(8) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 122.2(8) . . ? C4 C3 C8 121.6(8) . . ? C2 C3 C8 116.2(8) . . ? C3 C4 C5 118.3(7) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? C6 C5 C4 120.3(8) . . ? C6 C5 C9 120.1(9) . . ? C4 C5 C9 119.6(8) . . ? C5 C6 C1 119.7(8) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? O2 C7 O1 126.7(7) . . ? O2 C7 C1 118.6(9) . . ? O1 C7 C1 114.7(8) . . ? O3 C8 O4 129.2(9) . . ? O3 C8 C3 117.7(8) . . ? O4 C8 C3 113.1(9) . . ? O5 C9 O6 124.2(10) . . ? O5 C9 C5 121.2(11) . . ? O6 C9 C5 113.8(9) . . ? O7 C10 N1 125.3(15) . . ? O7 C10 N2 123.1(15) . . ? N1 C10 N2 110.5(15) . . ? O7 C10 C10 41.3(11) . 2_565 ? N1 C10 C10 124.1(16) . 2_565 ? N2 C10 C10 114.1(16) . 2_565 ? C12 C11 N1 103(2) . . ? C11 C12 C13 114.1(15) . . ? C12 C13 N2 94(2) . . ? N1 C14 C15 113(2) . 2_565 ? N2 C15 C14 128(2) . 2_565 ? C10 N1 C14 108.9(17) . . ? C10 N1 C11 124.1(17) . . ? C14 N1 C11 123.6(19) . . ? C10 N2 C15 108.5(17) . . ? C10 N2 C13 123.9(18) . . ? C15 N2 C13 127.5(19) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 2059.7 51.9 2 0.000 0.184 0.500 24.8 -1.4 3 0.000 0.500 0.316 24.8 -1.3 4 0.000 0.500 0.684 24.8 -1.3 5 0.000 0.816 0.500 24.8 -1.4 6 0.500 0.500 0.500 2059.7 51.9 7 0.184 0.500 0.000 24.8 -1.5 8 0.316 0.000 0.500 24.8 -1.5 9 0.500 0.316 0.000 24.8 -1.4 10 0.500 0.684 0.000 24.8 -1.4 11 0.500 0.000 0.184 24.8 -1.3 12 0.500 0.000 0.816 24.8 -1.3 13 0.684 0.000 0.500 24.8 -1.5 14 0.816 0.500 0.000 24.8 -1.5 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.216 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.124 #end data_2 #TrackingRef '- check cif.cif' _database_code_depnum_ccdc_archive 'CCDC 868808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C156 H162 Cu3 N14 O86 Zn15' _chemical_formula_sum 'C156 H162 Cu3 N14 O86 Zn15' _chemical_formula_weight 4780.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I23 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' '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+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, 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+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, 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+1/2, x+1/2' _cell_length_a 23.3483(2) _cell_length_b 23.3483(2) _cell_length_c 23.3483(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12728.17(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1547 _cell_measurement_theta_min 2.7532 _cell_measurement_theta_max 27.6593 _exptl_crystal_description cube _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3754 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6228 _exptl_absorpt_correction_T_max 0.6228 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5422 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3479 _reflns_number_gt 2848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'XPREP in SHELXTL (Siemens, 1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 3479 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 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 0.5000 1.0000 0.93843(4) 0.0326(2) Uani 0.50 2 d SP . . Zn1 Zn 0.5000 1.0000 0.93843(4) 0.0326(2) Uani 0.50 2 d SP . . Zn2 Zn 0.70604(3) 0.81759(3) 0.76031(3) 0.0461(2) Uani 1 1 d . . . O1 O 0.56290(18) 0.94596(18) 0.95175(17) 0.0529(11) Uani 1 1 d . . . O2 O 0.5563(2) 0.93479(18) 1.04596(17) 0.0531(11) Uani 1 1 d . . . O3 O 0.6956(2) 0.83064(18) 0.84180(17) 0.0590(12) Uani 1 1 d . . . O4 O 0.7394(2) 0.75647(19) 0.88191(17) 0.0568(12) Uani 1 1 d . . . O5 O 0.7286(3) 0.7345(3) 1.0942(2) 0.117(3) Uani 1 1 d . . . O6 O 0.6661(2) 0.7858(2) 1.1402(2) 0.0700(14) Uani 1 1 d . . . O7 O 0.5000 1.0000 0.8517(2) 0.076(2) Uani 1 2 d S . . O8 O 0.74587(18) 0.74587(18) 0.74587(18) 0.0432(16) Uani 1 3 d S . . C1 C 0.6206(2) 0.8765(2) 0.9959(3) 0.0408(13) Uani 1 1 d . . . C2 C 0.6455(2) 0.8612(2) 0.9436(3) 0.0410(14) Uani 1 1 d . . . H2A H 0.6346 0.8802 0.9103 0.049 Uiso 1 1 calc R . . C3 C 0.6860(2) 0.8182(2) 0.9407(2) 0.0384(12) Uani 1 1 d . . . C4 C 0.7014(2) 0.7903(2) 0.9899(2) 0.0496(15) Uani 1 1 d . . . H4A H 0.7290 0.7617 0.9883 0.060 Uiso 1 1 calc R . . C5 C 0.6765(3) 0.8039(3) 1.0426(2) 0.0483(15) Uani 1 1 d . . . C6 C 0.6362(3) 0.8463(3) 1.0444(3) 0.0503(16) Uani 1 1 d . . . H6A H 0.6188 0.8551 1.0791 0.060 Uiso 1 1 calc R . . C7 C 0.5767(2) 0.9232(2) 0.9984(3) 0.0404(12) Uani 1 1 d . . . C8 C 0.7081(2) 0.8004(2) 0.8828(2) 0.0399(13) Uani 1 1 d . . . C9 C 0.6942(3) 0.7724(3) 1.0949(3) 0.064(2) 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 Cu1 0.0341(5) 0.0269(4) 0.0368(5) 0.000 0.000 0.0034(4) Zn1 0.0341(5) 0.0269(4) 0.0368(5) 0.000 0.000 0.0034(4) Zn2 0.0315(4) 0.0649(5) 0.0421(4) 0.0149(4) 0.0008(3) 0.0028(3) O1 0.057(3) 0.056(3) 0.046(3) 0.013(2) 0.004(2) 0.024(2) O2 0.067(3) 0.046(3) 0.047(3) 0.003(2) 0.007(2) 0.021(2) O3 0.079(3) 0.058(3) 0.040(2) 0.014(2) 0.012(2) 0.019(2) O4 0.072(3) 0.054(3) 0.045(3) -0.007(2) -0.001(2) 0.028(2) O5 0.136(6) 0.144(6) 0.072(4) 0.020(4) 0.000(4) 0.100(5) O6 0.093(4) 0.065(3) 0.052(3) 0.014(2) -0.013(3) 0.022(3) O7 0.127(6) 0.062(4) 0.038(3) 0.000 0.000 0.026(5) O8 0.0432(16) 0.0432(16) 0.0432(16) 0.0006(18) 0.0006(18) 0.0006(18) C1 0.046(3) 0.041(3) 0.036(3) 0.002(3) 0.001(3) 0.011(2) C2 0.049(4) 0.035(3) 0.038(3) 0.018(3) -0.001(3) 0.014(3) C3 0.038(3) 0.046(3) 0.032(3) 0.002(3) 0.008(2) 0.011(3) C4 0.050(3) 0.052(4) 0.046(4) 0.000(3) 0.006(3) 0.023(3) C5 0.064(4) 0.049(4) 0.032(3) 0.003(3) -0.004(3) 0.017(3) C6 0.070(4) 0.049(4) 0.033(3) -0.003(3) 0.011(3) 0.007(3) C7 0.040(3) 0.038(3) 0.043(3) 0.007(3) 0.008(3) 0.008(2) C8 0.031(3) 0.043(3) 0.046(3) 0.005(3) 0.010(3) 0.001(3) C9 0.073(5) 0.079(5) 0.038(4) 0.008(3) -0.004(3) 0.029(4) _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 O1 1.961(4) . ? Cu1 O1 1.961(4) 2_675 ? Cu1 O7 2.026(6) . ? Cu1 O2 2.045(4) 4_577 ? Cu1 O2 2.045(4) 3_657 ? Cu1 Zn1 2.8753(16) 3_657 ? Cu1 Cu1 2.8753(16) 3_657 ? Zn2 O6 1.916(4) 18_466 ? Zn2 O3 1.942(4) . ? Zn2 O8 1.945(2) . ? Zn2 O4 1.970(4) 9 ? O1 C7 1.254(7) . ? O2 C7 1.237(7) . ? O2 Zn1 2.045(4) 3_657 ? O2 Cu1 2.045(4) 3_657 ? O3 C8 1.224(7) . ? O4 C8 1.260(7) . ? O4 Zn2 1.970(4) 5 ? O5 C9 1.195(8) . ? O6 C9 1.282(8) . ? O6 Zn2 1.916(4) 24_665 ? O8 Zn2 1.945(2) 5 ? O8 Zn2 1.945(2) 9 ? C1 C6 1.383(8) . ? C1 C2 1.398(8) . ? C1 C7 1.498(7) . ? C2 C3 1.382(7) . ? C2 H2A 0.9300 . ? C3 C4 1.369(8) . ? C3 C8 1.505(8) . ? C4 C5 1.398(8) . ? C4 H4A 0.9300 . ? C5 C6 1.367(8) . ? C5 C9 1.484(8) . ? C6 H6A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 161.7(2) . 2_675 ? O1 Cu1 O7 99.13(12) . . ? O1 Cu1 O7 99.13(12) 2_675 . ? O1 Cu1 O2 88.23(18) . 4_577 ? O1 Cu1 O2 88.53(18) 2_675 4_577 ? O7 Cu1 O2 100.27(12) . 4_577 ? O1 Cu1 O2 88.53(18) . 3_657 ? O1 Cu1 O2 88.23(18) 2_675 3_657 ? O7 Cu1 O2 100.27(12) . 3_657 ? O2 Cu1 O2 159.5(2) 4_577 3_657 ? O1 Cu1 Zn1 80.87(12) . 3_657 ? O1 Cu1 Zn1 80.87(12) 2_675 3_657 ? O7 Cu1 Zn1 180.000(1) . 3_657 ? O2 Cu1 Zn1 79.73(12) 4_577 3_657 ? O2 Cu1 Zn1 79.73(12) 3_657 3_657 ? O1 Cu1 Cu1 80.87(12) . 3_657 ? O1 Cu1 Cu1 80.87(12) 2_675 3_657 ? O7 Cu1 Cu1 180.000(1) . 3_657 ? O2 Cu1 Cu1 79.73(12) 4_577 3_657 ? O2 Cu1 Cu1 79.73(12) 3_657 3_657 ? Zn1 Cu1 Cu1 0.0 3_657 3_657 ? O6 Zn2 O3 114.7(2) 18_466 . ? O6 Zn2 O8 117.2(3) 18_466 . ? O3 Zn2 O8 111.42(16) . . ? O6 Zn2 O4 100.9(2) 18_466 9 ? O3 Zn2 O4 101.47(19) . 9 ? O8 Zn2 O4 109.12(17) . 9 ? C7 O1 Cu1 127.0(3) . . ? C7 O2 Zn1 124.7(4) . 3_657 ? C7 O2 Cu1 124.7(4) . 3_657 ? Zn1 O2 Cu1 0.00(5) 3_657 3_657 ? C8 O3 Zn2 130.2(4) . . ? C8 O4 Zn2 130.0(4) . 5 ? C9 O6 Zn2 115.0(4) . 24_665 ? Zn2 O8 Zn2 110.19(19) 5 9 ? Zn2 O8 Zn2 110.19(19) 5 . ? Zn2 O8 Zn2 110.19(19) 9 . ? C6 C1 C2 118.4(5) . . ? C6 C1 C7 121.2(6) . . ? C2 C1 C7 120.4(5) . . ? C3 C2 C1 120.9(5) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C4 C3 C2 118.9(5) . . ? C4 C3 C8 122.3(5) . . ? C2 C3 C8 118.6(5) . . ? C3 C4 C5 121.5(5) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C6 C5 C4 118.5(5) . . ? C6 C5 C9 121.8(5) . . ? C4 C5 C9 119.7(5) . . ? C5 C6 C1 121.7(5) . . ? C5 C6 H6A 119.1 . . ? C1 C6 H6A 119.1 . . ? O2 C7 O1 126.0(5) . . ? O2 C7 C1 117.2(5) . . ? O1 C7 C1 116.7(5) . . ? O3 C8 O4 126.5(5) . . ? O3 C8 C3 117.5(5) . . ? O4 C8 C3 116.0(5) . . ? O5 C9 O6 122.4(6) . . ? O5 C9 C5 123.0(6) . . ? O6 C9 C5 114.4(6) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.020 -0.004 -0.001 7976.4 982.0 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.753 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.082 #end