# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1775 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Chem. Commun. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Blue Photoluminescent Zinc Co-ordination Polymers with Supertetranuclear cores ; loop_ _publ_author_name _publ_author_address 'Tao Jun' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Shi, Jian-Xin' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Seik Weng Ng' ; Institute of Postgraduate Studies and Research University of Malaya 50603 Kuala Lumpur Malaysia ; #============================================================ data_complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H20 N2 O13 Zn4' _chemical_formula_weight 926.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y, -x, -z' 'y, x, -z' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' 'y, x, z' '-y, -x, z' '-y-1/2, x-1/2, -z-1/2' 'y-1/2, -x-1/2, -z-1/2' _cell_length_a 17.346(2) _cell_length_b 17.346(2) _cell_length_c 10.428(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3137.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5070 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 29.63 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 3.099 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6536 _exptl_absorpt_correction_T_max 0.7679 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens CCD area-detector diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11775 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 29.63 _reflns_number_total 2295 _reflns_number_gt 1845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; ? ; _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^)+(0.0475P)^2^+2.2713P] 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, U(H) = 1.5U~eq~(C).' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2295 _refine_ls_number_parameters 164 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.80044(2) 0.34146(2) 0.0000 0.0231(1) Uani 1 2 d S . . Zn2 Zn 0.81854(2) 0.18146(2) 0.14075(4) 0.0244(1) Uani 1 2 d S . . O1 O 0.8500(1) 0.3713(1) 0.1625(2) 0.029(1) Uani 1 1 d . . . O2 O 0.8554(2) 0.2594(1) 0.2666(2) 0.048(1) Uani 1 1 d . . . O3 O 0.9178(2) 0.1265(2) 0.1347(3) 0.027(1) Uani 0.50 1 d PD . 1 O4 O 0.9321(2) 0.2202(2) 0.0000 0.039(1) Uani 1 2 d SD . 1 O5 O 0.7636(1) 0.2364(1) 0.0000 0.020(1) Uani 1 4 d S . . N1 N 0.7177(2) 0.4280(2) 0.0000 0.029(1) Uani 1 2 d SD . . C1 C 0.7009(4) 0.4681(4) 0.0990(6) 0.056(3) Uani 0.50 1 d PD . . C2 C 0.6466(4) 0.5247(5) 0.1007(7) 0.057(3) Uani 0.50 1 d PD . . C1' C 0.6782(5) 0.4451(5) -0.1081(7) 0.056(3) Uani 0.50 1 d PD . . C2' C 0.6215(5) 0.5025(5) -0.1131(7) 0.057(3) Uani 0.50 1 d PD . . C3 C 0.6049(2) 0.5433(2) 0.0000 0.033(1) Uani 1 2 d SD . . C4 C 0.8606(2) 0.3309(1) 0.2612(2) 0.025(1) Uani 1 1 d . . . C5 C 0.8784(1) 0.3722(1) 0.3843(2) 0.022(1) Uani 1 1 d . . . C6 C 0.8954(2) 0.4506(1) 0.3848(2) 0.026(1) Uani 1 1 d . . . C7 C 0.9053(2) 0.4886(2) 0.5000 0.029(1) Uani 1 2 d S . . C8 C 0.8716(2) 0.3330(2) 0.5000 0.025(1) Uani 1 2 d S . . C9 C 0.9577(3) 0.1648(3) 0.0540(4) 0.024(1) Uani 0.50 1 d PD . 1 C10 C 1.0391(1) 0.1372(1) 0.0293(3) 0.022(1) Uani 0.50 1 d PD . 1 C11 C 1.0897(1) 0.1879(1) -0.0305(4) 0.031(2) Uani 0.50 1 d PD . 1 C12 C 1.1650(2) 0.1650(2) -0.0557(6) 0.039(2) Uani 0.50 2 d SPD . 1 C13 C 1.0638(2) 0.0638(2) 0.0636(5) 0.020(1) Uani 0.50 2 d SPD . 1 H1 H 0.7274 0.4579 0.1746 0.083 Uiso 0.50 1 d PR . . H2 H 0.6388 0.5516 0.1768 0.086 Uiso 0.50 1 d PR . . H1' H 0.6891 0.4175 -0.1824 0.083 Uiso 0.50 1 d PR . . H2' H 0.5958 0.5133 -0.1893 0.086 Uiso 0.50 1 d PR . . H6 H 0.9002 0.4773 0.3079 0.039 Uiso 1 1 d R . . H7 H 0.9187 0.5405 0.5000 0.044 Uiso 1 2 d SR . . H8 H 0.8625 0.2802 0.5000 0.037 Uiso 1 2 d SR . . H11 H 1.0732 0.2370 -0.0536 0.047 Uiso 0.50 1 calc PR . 1 H12 H 1.1979 0.1893 -0.1136 0.059 Uiso 0.25 1 calc PR . 1 H13 H 1.0426 0.0335 0.1282 0.030 Uiso 0.25 1 calc PR . 1 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 0.0317(2) 0.0227(2) 0.0150(2) 0.000 0.000 0.0005(2) Zn2 0.0277(21 0.0277(2) 0.0177(2) 0.0004(1) -0.0004(1) 0.0098(2) O1 0.040(1) 0.032(1) 0.016(1) -0.001(1) -0.004(1) -0.001(1) O2 0.095(2) 0.027(1) 0.021(1) -0.004(1) -0.009(1) -0.009(1) O3 0.023(2) 0.032(2) 0.025(2) 0.002(2) 0.002(1) 0.003(1) O4 0.026(1) 0.028(1) 0.062(2) 0.000 0.000 0.007(1) O5 0.021(1) 0.021(1) 0.018(2) 0.000 0.000 0.002(1) N1 0.031(2) 0.026(2) 0.029(2) 0.000 0.000 0.003(1) C1 0.065(5) 0.065(6) 0.036(2) -0.022(3) -0.021(3) 0.036(4) C2 0.059(5) 0.073(5) 0.040(2) -0.023(3) -0.021(3) 0.035(4) C1' 0.065(5) 0.065(6) 0.036(2) -0.022(3) -0.021(3) 0.036(4) C2' 0.059(5) 0.073(5) 0.040(2) -0.023(3) -0.021(3) 0.035(4) C3 0.024(2) 0.023(2) 0.051(2) 0.000 0.000 -0.002(1) C4 0.028(1) 0.029(1) 0.017(1) -0.002(1) 0.002(1) 0.001(1) C5 0.025(1) 0.026(1) 0.016(1) 0.000(1) 0.000(1) 0.001(1) C6 0.033(1) 0.026(1) 0.018(1) 0.003(1) 0.002(1) -0.001(1) C7 0.040(2) 0.021(2) 0.026(2) 0.000 0.000 -0.004(2) C8 0.032(2) 0.024(2) 0.018(2) 0.000 0.000 -0.002(1) C9 0.018(2) 0.029(2) 0.024(2) -0.004(2) 0.000(2) 0.000(2) C10 0.019(2) 0.024(2) 0.022(4) -0.002(2) 0.000(2) 0.003(2) C11 0.031(2) 0.022(2) 0.041(5) 0.009(2) 0.003(2) 0.002(2) C12 0.029(2) 0.029(2) 0.059(5) 0.011(2) 0.011(2) -0.007(3) C13 0.022(2) 0.022(2) 0.015(3) 0.001(2) 0.001(2) -0.001(2) _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.970(2) . ? Zn1 O1 1.970(2) 10 ? Zn1 O5 1.931(1) . ? Zn1 N1 2.076(3) . ? Zn2 O2 1.989(2) . ? Zn2 O2 1.989(2) 14_665 ? Zn2 O3 1.969(3) . ? Zn2 O4 2.547(2) 5_665 ? Zn2 O5 1.993(2) . ? O1 C4 1.258(3) . ? O2 C4 1.245(3) . ? N1 C1 1.279(6) . ? N1 C1 1.279(6) 10 ? N1 C1' 1.352(6) . ? N1 C1' 1.352(6) 10 ? C1 C2 1.360(7) . ? C2 C3 1.316(6) . ? C1' C2' 1.400(7) . ? C2' C3 1.406(6) . ? C3 C2 1.316(6) 10 ? C3 C2' 1.406(6) 10 ? C3 C3 1.509(7) 13 ? C4 C5 1.502(3) . ? C5 C8 1.390(3) . ? C5 C6 1.393(3) . ? C6 C7 1.381(3) . ? C7 C6 1.381(3) 10_556 ? C8 C5 1.390(3) 10_556 ? C9 O4 1.199(5) . ? C9 O3 1.277(6) . ? C9 C10 1.512(5) . ? C10 C11 1.390(1) . ? C10 C13 1.390(1) . ? C11 C12 1.390(1) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 118.8(1) . 10 ? O1 Zn1 O5 113.1(1) . . ? O1 Zn1 N1 96.4(1) . . ? O1 Zn1 O5 113.1(1) 10 . ? O1 Zn1 N1 96.4(1) 10 . ? O5 Zn1 N1 117.0(1) . . ? O2 Zn2 O2 90.1(1) . 14_665 ? O2 Zn2 O3 94.0(1) . . ? O2 Zn2 O4 172.1(1) . 5_665 ? O2 Zn2 O5 108.3(1) . . ? O2 Zn2 O3 117.4(1) 14_665 . ? O2 Zn2 O4 87.3(1) 14_665 5_665 ? O2 Zn2 O5 108.3(1) 14_665 . ? O3 Zn2 O4 80.7(1) . 5_665 ? O3 Zn2 O5 128.8(1) . . ? O4 Zn2 O5 79.6(1) 5_665 . ? C4 O1 Zn1 128.4(2) . . ? C4 O2 Zn2 132.1(2) . . ? Zn1 O5 Zn1 128.7(2) . 5_665 ? Zn1 O5 Zn2 107.0(1) . . ? Zn1 O5 Zn2 107.0(1) . 10 ? Zn1 O5 Zn2 107.0(1) 5_665 . ? Zn1 O5 Zn2 107.0(1) 5_665 10 ? Zn2 O5 Zn2 94.9(1) . 10 ? C1' N1 C1 115.9(4) . . ? N1 C1 C2 124.1(8) . . ? C1 C2 C3 123.2(8) . . ? C2 C3 C2' 115.6(4) . . ? C3 C2' C1' 118.1(7) . . ? C2' C1' N1 122.9(7) . . ? C1 N1 Zn1 123.5(4) . . ? C1 N1 Zn1 123.5(4) 10 . ? C1' N1 Zn1 120.6(4) . . ? C1' N1 Zn1 120.6(4) 10 . ? C2 C3 C3 124.2(4) . 13 ? C2 C3 C3 124.2(4) 10 13 ? C2' C3 C3 120.1(4) . 13 ? C2' C3 C3 120.1(4) 10 13 ? O1 C4 O2 125.5(2) . . ? O1 C4 C5 117.6(2) . . ? O2 C4 C5 116.8(2) . . ? C8 C5 C6 119.5(2) . . ? C8 C5 C4 119.5(2) . . ? C6 C5 C4 120.8(2) . . ? C7 C6 C5 119.7(2) . . ? C6 C7 C6 120.9(3) . 10_556 ? C5 C8 C5 120.6(3) 10_556 . ? O3 C9 O4 121.7(4) . . ? O3 C9 C10 116.9(4) . . ? O4 C9 C10 121.3(4) . . ? C9 O3 Zn2 104.1(3) . . ? C11 C10 C13 119.9(1) . . ? C11 C10 C9 117.8(2) . . ? C13 C10 C9 122.3(2) . . ? C10 C11 C12 119.9(1) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 29.63 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.527 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.082 _publ_section_exptl_refinement ; The lattice benzene-1,3-dicarboxylic acid lies on the Wyckoff 4f site, and is disordered. Within the aromatic ring, the C-C distances were fixed at 1.390+-0.001 and C^...^C^...^C distances at 2.408+-0.002 \%A. FLAT 0.01 restraints were imposed on the -C-CO~2~ unit as well as on the aromatic carbon atoms. The pyridine ring of the 4,4'-bipyridyl molecule is also disordered over two positions; the primed and umprimed atoms were restrained to have the same temperature factors, and the six independent atoms were retrained to be planar by a similar FLAT instruction. Pairs of bonds in the pyridyl ring were restrained by a SADI 0.01 instruction. ; #===========================================END data_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N4 O14 Zn4' _chemical_formula_weight 950.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 17.096(7) _cell_length_b 11.183(6) _cell_length_c 18.607(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.520(10) _cell_angle_gamma 90.00 _cell_volume 3459(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 2.817 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.3333 _exptl_absorpt_correction_T_max 0.5060 _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 'Siemens R3m' _diffrn_measurement_method '\w-scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 7035 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.93 _reflns_number_total 6801 _reflns_number_gt 5418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+8.0332P] 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_number_reflns 6801 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.58657(3) 0.06306(4) -0.00090(3) 0.02682(13) Uani 1 d . . . Zn2 Zn 0.50043(3) 0.17578(4) 0.12963(3) 0.02893(13) Uani 1 d . . . Zn3 Zn 0.92370(3) 0.41748(4) 0.02119(3) 0.02797(13) Uani 1 d . . . Zn4 Zn 1.01780(3) 0.67075(4) 0.13106(3) 0.02971(13) Uani 1 d . . . N1 N 0.1913(2) -0.0248(3) 0.4538(2) 0.0331(8) Uani 1 d . . . N2 N 0.4392(2) 0.1291(3) 0.2082(2) 0.0307(8) Uani 1 d . . . N3 N 0.8604(2) 0.3979(3) 0.1092(2) 0.0315(8) Uani 1 d . . . N4 N 0.9172(2) 0.7089(3) 0.1682(2) 0.0353(9) Uani 1 d . . . O1 O 0.5312(2) 0.1912(3) -0.10110(19) 0.0420(8) Uani 1 d . . . O2 O 0.60413(19) 0.2479(3) 0.00713(18) 0.0365(7) Uani 1 d . . . O3 O 0.6017(2) 0.6906(3) -0.0011(2) 0.0492(9) Uani 1 d . . . O4 O 0.5209(2) 0.6520(3) -0.11240(18) 0.0429(8) Uani 1 d . . . O5 O 0.61032(19) 0.1370(3) 0.18271(18) 0.0440(8) Uani 1 d . . . O6 O 0.6535(2) 0.0181(3) 0.10217(17) 0.0411(8) Uani 1 d . . . O7 O 0.52839(17) -0.0908(2) -0.03568(15) 0.0277(6) Uani 1 d . . . H7 H 0.5535 -0.1428 -0.0057 0.120 Uiso 1 d R . . O8 O 1.1066(2) 0.6829(3) 0.21866(17) 0.0403(8) Uani 1 d . . . O9 O 1.1016(2) 0.4849(3) 0.2233(2) 0.0652(13) Uani 1 d . . . O10 O 1.3298(2) 0.4106(3) 0.4520(2) 0.0562(10) Uani 1 d . . . O11 O 1.32811(19) 0.6073(3) 0.43789(17) 0.0387(8) Uani 1 d . . . O12 O 1.01105(17) 0.5244(3) 0.07425(15) 0.0292(6) Uani 1 d . . . H12 H 1.0444 0.4776 0.1016 0.120 Uiso 1 d R . . O13 O 1.0246(2) 0.8150(3) 0.07509(17) 0.0444(9) Uani 1 d . . . O14 O 1.0291(2) 0.7500(3) -0.03819(18) 0.0418(8) Uani 1 d . . . C1 C 0.2272(3) -0.1093(4) 0.4207(3) 0.0391(11) Uani 1 d . . . H1A H 0.2142 -0.1915 0.4271 0.080 Uiso 1 d R . . C2 C 0.2813(3) -0.0838(4) 0.3782(3) 0.0396(11) Uani 1 d . . . H2A H 0.3044 -0.1477 0.3555 0.080 Uiso 1 d R . . C3 C 0.3025(3) 0.0353(4) 0.3675(2) 0.0289(9) Uani 1 d . . . C4 C 0.2700(3) 0.1214(4) 0.4072(3) 0.0370(11) Uani 1 d . . . H4A H 0.2857 0.2037 0.4057 0.080 Uiso 1 d R . . C5 C 0.2159(3) 0.0884(4) 0.4484(3) 0.0371(11) Uani 1 d . . . H5A H 0.1947 0.1495 0.4747 0.080 Uiso 1 d R . . C6 C 0.3526(2) 0.0677(4) 0.3149(2) 0.0279(9) Uani 1 d . . . C7 C 0.3836(3) -0.0198(4) 0.2751(3) 0.0366(11) Uani 1 d . . . H7A H 0.3749 -0.1029 0.2835 0.080 Uiso 1 d R . . C8 C 0.4263(3) 0.0135(4) 0.2237(3) 0.0375(11) Uani 1 d . . . H8A H 0.4478 -0.0481 0.1979 0.080 Uiso 1 d R . . C9 C 0.4105(3) 0.2135(4) 0.2463(3) 0.0382(11) Uani 1 d . . . H9A H 0.4197 0.2958 0.2362 0.080 Uiso 1 d R . . C10 C 0.3677(3) 0.1871(4) 0.2995(3) 0.0380(11) Uani 1 d . . . H10A H 0.3487 0.2505 0.3258 0.080 Uiso 1 d R . . C11 C 0.5620(3) 0.2720(4) -0.0564(3) 0.0315(10) Uani 1 d . . . C12 C 0.5484(3) 0.4012(4) -0.0793(3) 0.0369(11) Uani 1 d . . . H12A H 0.5166 0.4201 -0.1276 0.080 Uiso 1 d R . . C13 C 0.5795(3) 0.4891(4) -0.0341(3) 0.0398(11) Uani 1 d . . . H13A H 0.6125 0.4667 0.0132 0.080 Uiso 1 d R . . C14 C 0.5678(3) 0.6212(4) -0.0500(3) 0.0371(11) Uani 1 d . . . C15 C 0.6627(3) 0.0739(4) 0.1616(2) 0.0321(10) Uani 1 d . . . C16 C 0.7446(3) 0.0703(4) 0.2138(2) 0.0390(11) Uani 1 d . . . H16A H 0.7913 0.0680 0.1936 0.080 Uiso 1 d R . . C17 C 0.7807(3) 0.3741(4) 0.0930(2) 0.0344(10) Uani 1 d . . . H17A H 0.7538 0.3618 0.0422 0.080 Uiso 1 d R . . C18 C 0.7361(3) 0.3683(4) 0.1459(3) 0.0360(10) Uani 1 d . . . H18A H 0.6798 0.3492 0.1318 0.080 Uiso 1 d R . . C19 C 0.7730(3) 0.3889(4) 0.2204(2) 0.0291(9) Uani 1 d . . . C20 C 0.8564(3) 0.4104(4) 0.2365(2) 0.0328(10) Uani 1 d . . . H20A H 0.8855 0.4216 0.2868 0.080 Uiso 1 d R . . C21 C 0.8963(3) 0.4146(4) 0.1807(2) 0.0333(10) Uani 1 d . . . H21A H 0.9530 0.4308 0.1933 0.080 Uiso 1 d R . . C22 C 0.8422(3) 0.6961(4) 0.1275(3) 0.0377(11) Uani 1 d . . . H22A H 0.8344 0.6779 0.0759 0.080 Uiso 1 d R . . C23 C 0.7747(3) 0.7078(4) 0.1571(3) 0.0408(11) Uani 1 d . . . H23A H 0.7217 0.6981 0.1262 0.080 Uiso 1 d R . . C24 C 0.7851(3) 0.7337(4) 0.2319(2) 0.0345(10) Uani 1 d . . . C25 C 0.8633(3) 0.7522(4) 0.2733(3) 0.0402(11) Uani 1 d . . . H25A H 0.8722 0.7744 0.3244 0.080 Uiso 1 d R . . C26 C 0.9269(3) 0.7388(4) 0.2409(3) 0.0361(10) Uani 1 d . . . H26A H 0.9805 0.7504 0.2704 0.080 Uiso 1 d R . . C27 C 1.1308(3) 0.5814(4) 0.2481(2) 0.0320(10) Uani 1 d . . . C28 C 1.1991(3) 0.5870(4) 0.3139(2) 0.0325(10) Uani 1 d . . . H28A H 1.2224 0.6638 0.3289 0.080 Uiso 1 d R . . C29 C 1.2301(3) 0.4943(4) 0.3540(3) 0.0382(11) Uani 1 d . . . H29A H 1.2067 0.4172 0.3402 0.080 Uiso 1 d R . . C30 C 1.3000(3) 0.5028(4) 0.4196(3) 0.0357(10) Uani 1 d . . . C31 C 1.0223(3) 0.8303(4) 0.0072(2) 0.0323(10) Uani 1 d . . . C32 C 1.0087(3) 0.9560(4) -0.0211(2) 0.0353(10) Uani 1 d . . . H32A H 1.0126 0.9740 -0.0706 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 Zn1 0.0300(3) 0.0246(2) 0.0251(3) -0.00170(19) 0.0050(2) -0.00151(19) Zn2 0.0312(3) 0.0286(3) 0.0267(3) -0.0022(2) 0.0063(2) 0.0013(2) Zn3 0.0274(3) 0.0273(3) 0.0272(3) -0.0033(2) 0.0021(2) -0.0003(2) Zn4 0.0360(3) 0.0282(3) 0.0242(3) 0.0001(2) 0.0056(2) -0.0005(2) N1 0.034(2) 0.0313(19) 0.037(2) 0.0011(16) 0.0153(17) 0.0017(16) N2 0.033(2) 0.0292(18) 0.0307(19) -0.0002(15) 0.0094(16) 0.0031(15) N3 0.0292(19) 0.035(2) 0.030(2) -0.0020(16) 0.0061(16) -0.0002(16) N4 0.037(2) 0.038(2) 0.031(2) -0.0038(16) 0.0091(17) 0.0022(17) O1 0.055(2) 0.0277(16) 0.0425(19) -0.0007(15) 0.0088(17) 0.0016(15) O2 0.0390(18) 0.0296(16) 0.0377(18) 0.0058(14) 0.0029(15) 0.0015(13) O3 0.048(2) 0.0304(17) 0.061(2) 0.0039(17) -0.0024(18) -0.0009(15) O4 0.060(2) 0.0326(17) 0.0371(19) -0.0001(14) 0.0134(17) 0.0043(16) O5 0.0324(18) 0.063(2) 0.0333(18) -0.0061(16) 0.0004(15) 0.0098(16) O6 0.0468(19) 0.0420(18) 0.0289(17) -0.0024(14) -0.0022(15) 0.0106(16) O7 0.0300(15) 0.0262(14) 0.0266(15) -0.0009(12) 0.0060(12) -0.0001(12) O8 0.047(2) 0.0366(18) 0.0317(17) 0.0017(14) -0.0025(15) 0.0064(15) O9 0.067(3) 0.047(2) 0.060(3) 0.0216(19) -0.030(2) -0.022(2) O10 0.055(2) 0.053(2) 0.049(2) 0.0194(18) -0.0117(18) -0.0002(18) O11 0.0336(17) 0.047(2) 0.0312(17) -0.0063(14) -0.0017(14) 0.0006(15) O12 0.0299(15) 0.0312(16) 0.0248(15) -0.0002(12) 0.0031(12) -0.0006(12) O13 0.075(3) 0.0298(17) 0.0287(17) 0.0059(14) 0.0125(17) 0.0061(16) O14 0.059(2) 0.0294(17) 0.0352(18) 0.0020(14) 0.0070(16) 0.0098(15) C1 0.041(3) 0.028(2) 0.053(3) 0.003(2) 0.022(2) 0.000(2) C2 0.044(3) 0.030(2) 0.050(3) -0.004(2) 0.021(2) 0.000(2) C3 0.029(2) 0.030(2) 0.027(2) 0.0002(17) 0.0046(18) 0.0005(17) C4 0.044(3) 0.027(2) 0.044(3) -0.003(2) 0.017(2) -0.003(2) C5 0.038(3) 0.032(2) 0.046(3) -0.009(2) 0.020(2) -0.005(2) C6 0.027(2) 0.028(2) 0.029(2) 0.0012(17) 0.0075(18) -0.0007(17) C7 0.048(3) 0.028(2) 0.039(3) 0.0028(19) 0.019(2) 0.001(2) C8 0.047(3) 0.033(2) 0.036(3) 0.000(2) 0.018(2) 0.005(2) C9 0.044(3) 0.030(2) 0.046(3) -0.004(2) 0.022(2) -0.003(2) C10 0.042(3) 0.030(2) 0.049(3) -0.006(2) 0.025(2) -0.004(2) C11 0.037(2) 0.025(2) 0.035(2) 0.0059(18) 0.013(2) 0.0025(18) C12 0.047(3) 0.030(2) 0.035(2) 0.0067(19) 0.010(2) 0.004(2) C13 0.043(3) 0.033(2) 0.044(3) 0.008(2) 0.012(2) 0.004(2) C14 0.039(3) 0.029(2) 0.047(3) 0.001(2) 0.018(2) 0.003(2) C15 0.030(2) 0.035(2) 0.027(2) 0.0026(19) -0.0006(19) -0.0015(19) C16 0.031(2) 0.050(3) 0.033(2) -0.001(2) 0.002(2) 0.004(2) C17 0.032(2) 0.046(3) 0.024(2) -0.0054(19) 0.0042(19) -0.008(2) C18 0.029(2) 0.042(3) 0.036(3) -0.001(2) 0.006(2) -0.008(2) C19 0.030(2) 0.027(2) 0.031(2) 0.0015(17) 0.0084(19) -0.0012(17) C20 0.033(2) 0.037(2) 0.026(2) -0.0016(18) 0.0023(19) 0.0006(19) C21 0.025(2) 0.038(2) 0.036(2) 0.006(2) 0.0058(19) 0.0006(18) C22 0.035(3) 0.049(3) 0.028(2) -0.001(2) 0.004(2) 0.003(2) C23 0.038(3) 0.047(3) 0.034(3) -0.001(2) 0.001(2) 0.000(2) C24 0.038(3) 0.035(2) 0.032(2) 0.0002(19) 0.010(2) -0.002(2) C25 0.037(3) 0.050(3) 0.034(3) -0.013(2) 0.010(2) -0.003(2) C26 0.036(3) 0.040(3) 0.031(2) -0.007(2) 0.008(2) -0.006(2) C27 0.029(2) 0.038(2) 0.028(2) 0.0077(19) 0.0045(18) -0.0013(19) C28 0.030(2) 0.038(2) 0.027(2) -0.0041(19) 0.0022(19) 0.0010(19) C29 0.036(3) 0.040(3) 0.033(2) 0.002(2) -0.002(2) -0.005(2) C30 0.029(2) 0.047(3) 0.030(2) 0.003(2) 0.0050(19) -0.003(2) C31 0.033(2) 0.029(2) 0.033(2) 0.0041(19) 0.0024(19) 0.0041(18) C32 0.046(3) 0.029(2) 0.028(2) 0.0056(18) 0.003(2) 0.006(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 Zn1 O7 2.017(3) . ? Zn1 O6 2.053(3) . ? Zn1 O2 2.089(3) . ? Zn1 N1 2.191(4) 4_655 ? Zn1 O7 2.247(3) 3_655 ? Zn1 O1 2.366(3) . ? Zn1 C11 2.549(4) . ? Zn2 O7 1.949(3) 3_655 ? Zn2 O5 1.956(3) . ? Zn2 O4 1.972(3) 3_665 ? Zn2 N2 2.054(4) . ? Zn3 O12 1.986(3) . ? Zn3 O11 1.991(3) 4_565 ? Zn3 O14 2.035(3) 3_765 ? Zn3 N3 2.175(4) . ? Zn3 O12 2.397(3) 3_765 ? Zn4 O12 1.937(3) . ? Zn4 O13 1.939(3) . ? Zn4 O8 1.955(3) . ? Zn4 N4 2.043(4) . ? N1 C5 1.345(6) . ? N1 C1 1.352(6) . ? N1 Zn1 2.191(4) 4_556 ? N2 C9 1.341(6) . ? N2 C8 1.355(6) . ? N3 C21 1.342(6) . ? N3 C17 1.351(6) . ? N4 C22 1.336(6) . ? N4 C26 1.366(6) . ? O1 C11 1.258(5) . ? O2 C11 1.260(5) . ? O3 C14 1.233(6) . ? O4 C14 1.294(6) . ? O4 Zn2 1.972(3) 3_665 ? O5 C15 1.272(5) . ? O6 C15 1.247(5) . ? O7 Zn2 1.949(3) 3_655 ? O7 Zn1 2.247(3) 3_655 ? O7 O3 2.754(4) 1_545 ? O8 C27 1.286(5) . ? O9 C27 1.232(6) . ? O9 O12 2.876(5) . ? O10 C30 1.241(6) . ? O11 C30 1.279(6) . ? O11 Zn3 1.991(3) 4_666 ? O12 Zn3 2.397(3) 3_765 ? O13 C31 1.267(5) . ? O14 C31 1.256(5) . ? O14 Zn3 2.035(3) 3_765 ? C1 C2 1.380(7) . ? C2 C3 1.406(6) . ? C3 C4 1.404(6) . ? C3 C6 1.489(6) . ? C4 C5 1.383(6) . ? C6 C10 1.402(6) . ? C6 C7 1.403(6) . ? C7 C8 1.383(6) . ? C9 C10 1.393(6) . ? C11 C12 1.509(6) . ? C12 C13 1.322(7) . ? C13 C14 1.511(6) . ? C15 C16 1.507(6) . ? C16 C16 1.316(9) 2_655 ? C17 C18 1.381(6) . ? C18 C19 1.401(6) . ? C19 C20 1.407(6) . ? C19 C19 1.495(8) 2_655 ? C20 C21 1.370(6) . ? C22 C23 1.395(7) . ? C23 C24 1.391(6) . ? C24 C25 1.393(7) . ? C24 C24 1.508(9) 2_655 ? C25 C26 1.370(7) . ? C27 C28 1.484(6) . ? C28 C29 1.314(6) . ? C29 C30 1.499(6) . ? C31 C32 1.500(6) . ? C32 C32 1.335(9) 3_775 ? 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 O6 102.49(13) . . ? O7 Zn1 O2 156.77(12) . . ? O6 Zn1 O2 97.82(13) . . ? O7 Zn1 N1 95.50(13) . 4_655 ? O6 Zn1 N1 89.11(14) . 4_655 ? O2 Zn1 N1 95.97(13) . 4_655 ? O7 Zn1 O7 79.29(12) . 3_655 ? O6 Zn1 O7 94.98(12) . 3_655 ? O2 Zn1 O7 87.88(12) . 3_655 ? N1 Zn1 O7 173.96(12) 4_655 3_655 ? O7 Zn1 O1 100.80(12) . . ? O6 Zn1 O1 156.52(12) . . ? O2 Zn1 O1 58.77(12) . . ? N1 Zn1 O1 91.55(13) 4_655 . ? O7 Zn1 O1 86.46(12) 3_655 . ? O7 Zn1 C11 129.05(14) . . ? O6 Zn1 C11 127.27(14) . . ? O2 Zn1 C11 29.46(13) . . ? N1 Zn1 C11 95.46(14) 4_655 . ? O7 Zn1 C11 85.61(12) 3_655 . ? O1 Zn1 C11 29.36(13) . . ? O7 Zn2 O5 110.88(13) 3_655 . ? O7 Zn2 O4 109.39(13) 3_655 3_665 ? O5 Zn2 O4 114.69(15) . 3_665 ? O7 Zn2 N2 116.77(14) 3_655 . ? O5 Zn2 N2 99.99(15) . . ? O4 Zn2 N2 104.96(14) 3_665 . ? O12 Zn3 O11 148.80(13) . 4_565 ? O12 Zn3 O14 104.62(13) . 3_765 ? O11 Zn3 O14 102.49(14) 4_565 3_765 ? O12 Zn3 N3 97.77(13) . . ? O11 Zn3 N3 96.29(14) 4_565 . ? O14 Zn3 N3 92.25(14) 3_765 . ? O12 Zn3 O12 77.23(12) . 3_765 ? O11 Zn3 O12 84.29(12) 4_565 3_765 ? O14 Zn3 O12 97.37(12) 3_765 3_765 ? N3 Zn3 O12 170.01(12) . 3_765 ? O12 Zn4 O13 114.42(14) . . ? O12 Zn4 O8 116.69(13) . . ? O13 Zn4 O8 104.92(15) . . ? O12 Zn4 N4 114.43(14) . . ? O13 Zn4 N4 99.73(16) . . ? O8 Zn4 N4 104.75(15) . . ? C5 N1 C1 116.1(4) . . ? C5 N1 Zn1 120.7(3) . 4_556 ? C1 N1 Zn1 122.6(3) . 4_556 ? C9 N2 C8 117.4(4) . . ? C9 N2 Zn2 120.6(3) . . ? C8 N2 Zn2 122.0(3) . . ? C21 N3 C17 116.9(4) . . ? C21 N3 Zn3 122.6(3) . . ? C17 N3 Zn3 120.3(3) . . ? C22 N4 C26 117.7(4) . . ? C22 N4 Zn4 124.0(3) . . ? C26 N4 Zn4 118.0(3) . . ? C11 O1 Zn1 83.4(3) . . ? C11 O2 Zn1 95.9(3) . . ? C14 O4 Zn2 117.3(3) . 3_665 ? C15 O5 Zn2 129.0(3) . . ? C15 O6 Zn1 129.3(3) . . ? Zn2 O7 Zn1 134.91(15) 3_655 . ? Zn2 O7 Zn1 106.47(13) 3_655 3_655 ? Zn1 O7 Zn1 100.71(12) . 3_655 ? Zn2 O7 O3 77.45(12) 3_655 1_545 ? Zn1 O7 O3 121.26(14) . 1_545 ? Zn1 O7 O3 115.73(14) 3_655 1_545 ? C27 O8 Zn4 113.8(3) . . ? C27 O9 O12 107.8(3) . . ? C30 O11 Zn3 105.6(3) . 4_666 ? Zn4 O12 Zn3 136.21(16) . . ? Zn4 O12 Zn3 101.35(12) . 3_765 ? Zn3 O12 Zn3 102.77(12) . 3_765 ? Zn4 O12 O9 69.74(12) . . ? Zn3 O12 O9 123.99(14) . . ? Zn3 O12 O9 121.14(14) 3_765 . ? C31 O13 Zn4 131.0(3) . . ? C31 O14 Zn3 130.5(3) . 3_765 ? N1 C1 C2 123.7(4) . . ? C1 C2 C3 120.4(4) . . ? C4 C3 C2 115.4(4) . . ? C4 C3 C6 122.5(4) . . ? C2 C3 C6 122.0(4) . . ? C5 C4 C3 120.4(4) . . ? N1 C5 C4 123.7(4) . . ? C10 C6 C7 116.5(4) . . ? C10 C6 C3 121.9(4) . . ? C7 C6 C3 121.6(4) . . ? C8 C7 C6 120.2(4) . . ? N2 C8 C7 122.9(4) . . ? N2 C9 C10 123.1(4) . . ? C9 C10 C6 119.9(4) . . ? O1 C11 O2 121.7(4) . . ? O1 C11 C12 119.2(4) . . ? O2 C11 C12 119.1(4) . . ? O1 C11 Zn1 67.2(2) . . ? O2 C11 Zn1 54.6(2) . . ? C12 C11 Zn1 172.7(3) . . ? C13 C12 C11 121.3(4) . . ? C12 C13 C14 126.0(5) . . ? O3 C14 O4 125.5(4) . . ? O3 C14 C13 116.9(5) . . ? O4 C14 C13 117.5(4) . . ? O6 C15 O5 126.9(4) . . ? O6 C15 C16 117.6(4) . . ? O5 C15 C16 115.5(4) . . ? C16 C16 C15 123.2(6) 2_655 . ? N3 C17 C18 123.1(4) . . ? C17 C18 C19 120.1(4) . . ? C18 C19 C20 116.0(4) . . ? C18 C19 C19 122.3(5) . 2_655 ? C20 C19 C19 121.6(5) . 2_655 ? C21 C20 C19 120.2(4) . . ? N3 C21 C20 123.6(4) . . ? N4 C22 C23 122.6(4) . . ? C24 C23 C22 119.4(4) . . ? C23 C24 C25 117.7(4) . . ? C23 C24 C24 121.2(5) . 2_655 ? C25 C24 C24 120.9(5) . 2_655 ? C26 C25 C24 119.9(4) . . ? N4 C26 C25 122.5(4) . . ? O9 C27 O8 123.5(4) . . ? O9 C27 C28 121.2(4) . . ? O8 C27 C28 115.3(4) . . ? C29 C28 C27 124.8(4) . . ? C28 C29 C30 123.4(4) . . ? O10 C30 O11 123.0(4) . . ? O10 C30 C29 120.0(4) . . ? O11 C30 C29 116.9(4) . . ? O14 C31 O13 126.0(4) . . ? O14 C31 C32 117.8(4) . . ? O13 C31 C32 116.2(4) . . ? C32 C32 C31 121.5(5) 3_775 . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 26.93 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 0.444 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.103