# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '- CIF.cif' _journal_coden_Cambridge 1350 #================================================= # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Professor Ming-Liang Tong School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 PR China ; _publ_contact_author_phone 86-20-8411-0966 _publ_contact_author_fax 81-20-8411-2245 _publ_contact_author_email tongml@mail.sysu.edu.cn _publ_requested_journal CrystEngComm _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to CrystEngComm. Ming-Liang Tong ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Spontaneous Resolution of Four-Coordinate of Zn Complexes in the Formation of Three-Dimensional Metal-Organic Frameworks ; loop_ _publ_author_name _publ_author_address 'Liu, Wen-Ting' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Ou, Yong-Cong' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Lin, Zhuojia' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; #============================================================ data_complex1a _database_code_depnum_ccdc_archive 'CCDC 777158' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 N8 Zn' _chemical_formula_weight 277.56 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.1103(6) _cell_length_b 8.7455(8) _cell_length_c 13.0119(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 922.92(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4326 _exptl_absorpt_correction_T_max 0.5810 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4206 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1963 _reflns_number_gt 1878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'PROCESS-AUTO (Rigaku, 1998)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^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 0.004(10) _refine_ls_number_reflns 1963 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0425 _refine_ls_wR_factor_gt 0.0419 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.97769(2) 0.40932(3) 0.881503(16) 0.01004(7) Uani 1 1 d . . . N1 N 1.1061(2) 0.3496(2) 1.00604(12) 0.0127(4) Uani 1 1 d . . . N2 N 1.2261(2) 0.2492(3) 1.00103(14) 0.0137(4) Uani 1 1 d . . . N3 N 1.26675(19) 0.2139(2) 1.09838(12) 0.0123(4) Uani 1 1 d . . . N4 N 1.06406(19) 0.3825(2) 1.10379(12) 0.0142(4) Uani 1 1 d . . . N5 N 1.0786(2) 0.3139(3) 1.75447(13) 0.0120(4) Uani 1 1 d . . . N6 N 1.05687(19) 0.1665(2) 1.74800(12) 0.0132(4) Uani 1 1 d . . . N7 N 1.07640(19) 0.1273(2) 1.64890(12) 0.0109(4) Uani 1 1 d . . . N8 N 1.1133(2) 0.3777(2) 1.66180(12) 0.0130(4) Uani 1 1 d . . . C1 C 1.1656(2) 0.2963(3) 1.15934(15) 0.0121(5) Uani 1 1 d . . . C2 C 1.1611(2) 0.2891(3) 1.27235(15) 0.0118(5) Uani 1 1 d . . . C3 C 1.2039(2) 0.1548(3) 1.32375(16) 0.0121(5) Uani 1 1 d . . . H3 H 1.2409 0.0686 1.2857 0.015 Uiso 1 1 calc R . . C4 C 1.1929(2) 0.1461(3) 1.42993(16) 0.0129(5) Uani 1 1 d . . . H4 H 1.2247 0.0551 1.4645 0.015 Uiso 1 1 calc R . . C5 C 1.1351(2) 0.2707(3) 1.48594(15) 0.0117(5) Uani 1 1 d . . . C6 C 1.0928(2) 0.4071(4) 1.43493(15) 0.0147(4) Uani 1 1 d . . . H6 H 1.0550 0.4929 1.4730 0.018 Uiso 1 1 calc R . . C7 C 1.1065(2) 0.4159(3) 1.32911(15) 0.0145(5) Uani 1 1 d . . . H7 H 1.0787 0.5081 1.2947 0.017 Uiso 1 1 calc R . . C8 C 1.1114(2) 0.2589(3) 1.59792(14) 0.0112(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01465(11) 0.00910(13) 0.00636(10) 0.00037(10) 0.00014(8) 0.00009(9) N1 0.0142(9) 0.0141(12) 0.0097(9) 0.0003(8) 0.0000(6) -0.0005(8) N2 0.0185(8) 0.0135(11) 0.0092(8) 0.0008(7) -0.0021(6) 0.0002(8) N3 0.0157(8) 0.0132(12) 0.0080(9) 0.0007(7) -0.0006(6) 0.0002(7) N4 0.0160(8) 0.0184(12) 0.0080(8) -0.0009(7) -0.0004(6) 0.0016(7) N5 0.0150(9) 0.0115(12) 0.0094(9) 0.0010(7) 0.0009(6) -0.0009(7) N6 0.0175(9) 0.0119(12) 0.0103(8) -0.0014(7) 0.0006(6) 0.0003(7) N7 0.0145(7) 0.0104(12) 0.0080(8) -0.0014(6) 0.0013(5) 0.0005(6) N8 0.0161(8) 0.0132(13) 0.0096(8) 0.0016(7) 0.0020(6) -0.0004(7) C1 0.0140(10) 0.0132(14) 0.0092(9) 0.0001(9) 0.0011(7) -0.0020(9) C2 0.0113(10) 0.0152(14) 0.0088(10) 0.0002(9) 0.0008(7) -0.0009(9) C3 0.0130(9) 0.0130(14) 0.0103(10) -0.0032(9) 0.0018(7) 0.0005(9) C4 0.0128(10) 0.0123(14) 0.0135(10) 0.0015(8) 0.0005(7) 0.0002(8) C5 0.0124(10) 0.0138(14) 0.0088(9) -0.0004(9) 0.0004(7) -0.0021(9) C6 0.0201(10) 0.0125(13) 0.0116(10) -0.0020(10) 0.0031(7) 0.0005(11) C7 0.0169(10) 0.0120(14) 0.0145(10) 0.0029(11) -0.0005(7) 0.0023(10) C8 0.0108(9) 0.0102(13) 0.0127(11) 0.0003(8) -0.0001(7) 0.0007(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 Zn1 N7 1.996(2) 3_757 ? Zn1 N1 1.9960(17) . ? Zn1 N5 2.0245(18) 1_554 ? Zn1 N3 2.0386(17) 4_457 ? N1 N2 1.312(3) . ? N1 N4 1.348(2) . ? N2 N3 1.345(2) . ? N3 C1 1.350(3) . ? N3 Zn1 2.0386(17) 4_557 ? N4 C1 1.330(3) . ? N5 N6 1.303(3) . ? N5 N8 1.358(2) . ? N5 Zn1 2.0245(18) 1_556 ? N6 N7 1.344(2) . ? N7 C8 1.358(3) . ? N7 Zn1 1.996(2) 3_747 ? N8 C8 1.330(3) . ? C1 C2 1.472(3) . ? C2 C3 1.395(3) . ? C2 C7 1.404(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.392(3) . ? C4 H4 0.9500 . ? C5 C6 1.407(4) . ? C5 C8 1.473(3) . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? 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 N7 Zn1 N1 121.71(8) 3_757 . ? N7 Zn1 N5 108.72(8) 3_757 1_554 ? N1 Zn1 N5 110.12(7) . 1_554 ? N7 Zn1 N3 110.23(7) 3_757 4_457 ? N1 Zn1 N3 101.27(7) . 4_457 ? N5 Zn1 N3 103.06(7) 1_554 4_457 ? N2 N1 N4 112.18(16) . . ? N2 N1 Zn1 121.45(14) . . ? N4 N1 Zn1 125.31(14) . . ? N1 N2 N3 106.78(17) . . ? N2 N3 C1 106.37(17) . . ? N2 N3 Zn1 116.62(13) . 4_557 ? C1 N3 Zn1 135.80(14) . 4_557 ? C1 N4 N1 103.59(17) . . ? N6 N5 N8 112.13(17) . . ? N6 N5 Zn1 113.95(13) . 1_556 ? N8 N5 Zn1 129.75(16) . 1_556 ? N5 N6 N7 107.36(17) . . ? N6 N7 C8 106.08(18) . . ? N6 N7 Zn1 114.08(14) . 3_747 ? C8 N7 Zn1 139.33(14) . 3_747 ? C8 N8 N5 103.40(19) . . ? N4 C1 N3 111.08(18) . . ? N4 C1 C2 123.5(2) . . ? N3 C1 C2 125.4(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 120.6(2) . . ? C7 C2 C1 120.0(2) . . ? C4 C3 C2 120.5(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 119.91(19) . . ? C4 C5 C8 120.4(2) . . ? C6 C5 C8 119.6(2) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N8 C8 N7 111.03(17) . . ? N8 C8 C5 124.2(2) . . ? N7 C8 C5 124.7(2) . . ? 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 N7 Zn1 N1 N2 -135.54(18) 3_757 . . . ? N5 Zn1 N1 N2 -6.6(2) 1_554 . . . ? N3 Zn1 N1 N2 101.94(18) 4_457 . . . ? N7 Zn1 N1 N4 57.2(2) 3_757 . . . ? N5 Zn1 N1 N4 -173.93(17) 1_554 . . . ? N3 Zn1 N1 N4 -65.4(2) 4_457 . . . ? N4 N1 N2 N3 -0.3(3) . . . . ? Zn1 N1 N2 N3 -169.13(14) . . . . ? N1 N2 N3 C1 0.4(2) . . . . ? N1 N2 N3 Zn1 -168.98(15) . . . 4_557 ? N2 N1 N4 C1 0.0(3) . . . . ? Zn1 N1 N4 C1 168.35(16) . . . . ? N8 N5 N6 N7 -0.2(2) . . . . ? Zn1 N5 N6 N7 159.18(11) 1_556 . . . ? N5 N6 N7 C8 0.3(2) . . . . ? N5 N6 N7 Zn1 -173.15(12) . . . 3_747 ? N6 N5 N8 C8 0.0(2) . . . . ? Zn1 N5 N8 C8 -155.25(14) 1_556 . . . ? N1 N4 C1 N3 0.3(2) . . . . ? N1 N4 C1 C2 -177.5(2) . . . . ? N2 N3 C1 N4 -0.4(3) . . . . ? Zn1 N3 C1 N4 165.93(16) 4_557 . . . ? N2 N3 C1 C2 177.3(2) . . . . ? Zn1 N3 C1 C2 -16.4(4) 4_557 . . . ? N4 C1 C2 C3 148.3(2) . . . . ? N3 C1 C2 C3 -29.1(3) . . . . ? N4 C1 C2 C7 -28.8(3) . . . . ? N3 C1 C2 C7 153.7(2) . . . . ? C7 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C4 -177.22(19) . . . . ? C2 C3 C4 C5 1.5(3) . . . . ? C3 C4 C5 C6 -2.0(3) . . . . ? C3 C4 C5 C8 175.5(2) . . . . ? C4 C5 C6 C7 1.0(3) . . . . ? C8 C5 C6 C7 -176.51(19) . . . . ? C5 C6 C7 C2 0.5(3) . . . . ? C3 C2 C7 C6 -0.9(3) . . . . ? C1 C2 C7 C6 176.2(2) . . . . ? N5 N8 C8 N7 0.2(2) . . . . ? N5 N8 C8 C5 177.05(19) . . . . ? N6 N7 C8 N8 -0.3(2) . . . . ? Zn1 N7 C8 N8 170.51(15) 3_747 . . . ? N6 N7 C8 C5 -177.16(18) . . . . ? Zn1 N7 C8 C5 -6.3(3) 3_747 . . . ? C4 C5 C8 N8 155.6(2) . . . . ? C6 C5 C8 N8 -26.9(3) . . . . ? C4 C5 C8 N7 -27.9(3) . . . . ? C6 C5 C8 N7 149.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.402 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.070 #=================================================END data_complex1b _database_code_depnum_ccdc_archive 'CCDC 777159' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H4 N8 Zn' _chemical_formula_weight 277.56 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.1094(3) _cell_length_b 8.7499(4) _cell_length_c 13.0128(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 923.34(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4328 _exptl_absorpt_correction_T_max 0.6063 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4715 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1960 _reflns_number_gt 1873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'PROCESS-AUTO (Rigaku, 1998)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.3125P] 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 0.015(13) _refine_ls_number_reflns 1960 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.02226(3) 0.59063(3) 0.118511(17) 0.00938(8) Uani 1 1 d . . . N1 N -0.1060(2) 0.6504(3) -0.00611(14) 0.0119(5) Uani 1 1 d . . . N2 N -0.2251(3) 0.7503(3) -0.00088(16) 0.0133(4) Uani 1 1 d . . . N3 N -0.2668(2) 0.7860(3) -0.09837(14) 0.0127(4) Uani 1 1 d . . . N4 N -0.0644(2) 0.6176(3) -0.10390(13) 0.0132(5) Uani 1 1 d . . . N5 N -0.0784(3) 0.6863(3) -0.75466(14) 0.0124(5) Uani 1 1 d . . . N6 N -0.0574(2) 0.8337(3) -0.74806(13) 0.0116(5) Uani 1 1 d . . . N7 N -0.0762(2) 0.8725(3) -0.64878(13) 0.0109(4) Uani 1 1 d . . . N8 N -0.1141(2) 0.6220(3) -0.66206(14) 0.0126(5) Uani 1 1 d . . . C1 C -0.1659(3) 0.7035(3) -0.15904(17) 0.0108(5) Uani 1 1 d . . . C2 C -0.1608(3) 0.7103(3) -0.27281(17) 0.0117(5) Uani 1 1 d . . . C3 C -0.2049(3) 0.8453(3) -0.32343(18) 0.0121(5) Uani 1 1 d . . . H3 H -0.2430 0.9309 -0.2853 0.015 Uiso 1 1 calc R . . C4 C -0.1927(3) 0.8536(3) -0.43024(17) 0.0125(5) Uani 1 1 d . . . H4 H -0.2234 0.9448 -0.4650 0.015 Uiso 1 1 calc R . . C5 C -0.1359(3) 0.7290(3) -0.48590(17) 0.0110(5) Uani 1 1 d . . . C6 C -0.0921(3) 0.5939(4) -0.43524(16) 0.0146(5) Uani 1 1 d . . . H6 H -0.0532 0.5088 -0.4735 0.018 Uiso 1 1 calc R . . C7 C -0.1055(3) 0.5840(4) -0.32874(17) 0.0143(5) Uani 1 1 d . . . H7 H -0.0773 0.4919 -0.2943 0.017 Uiso 1 1 calc R . . C8 C -0.1124(3) 0.7405(3) -0.59834(16) 0.0110(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01350(12) 0.00864(14) 0.00599(11) 0.00043(10) 0.00001(10) 0.00005(10) N1 0.0087(10) 0.0167(13) 0.0102(9) 0.0001(9) -0.0009(8) 0.0018(9) N2 0.0171(10) 0.0143(12) 0.0087(8) 0.0013(7) -0.0014(7) 0.0005(9) N3 0.0177(10) 0.0132(13) 0.0072(9) 0.0013(8) -0.0013(7) 0.0017(8) N4 0.0134(9) 0.0173(14) 0.0088(8) -0.0006(8) -0.0001(7) 0.0009(8) N5 0.0193(11) 0.0111(13) 0.0069(8) 0.0007(8) 0.0012(8) 0.0005(9) N6 0.0148(10) 0.0099(13) 0.0101(8) -0.0018(8) 0.0018(8) -0.0006(8) N7 0.0118(8) 0.0125(13) 0.0084(8) -0.0012(7) 0.0011(7) 0.0006(8) N8 0.0135(10) 0.0149(14) 0.0095(8) 0.0021(8) 0.0013(7) -0.0014(9) C1 0.0112(11) 0.0110(15) 0.0103(10) 0.0011(9) -0.0005(9) -0.0016(10) C2 0.0086(11) 0.0158(16) 0.0107(10) -0.0002(10) 0.0005(9) 0.0008(10) C3 0.0118(11) 0.0138(15) 0.0107(10) -0.0029(10) 0.0019(9) -0.0010(11) C4 0.0166(12) 0.0106(15) 0.0104(10) 0.0016(9) 0.0000(9) -0.0015(10) C5 0.0096(11) 0.0147(16) 0.0086(10) 0.0005(10) 0.0010(8) -0.0027(11) C6 0.0175(11) 0.0144(15) 0.0121(10) -0.0024(11) 0.0027(9) 0.0024(14) C7 0.0191(12) 0.0111(15) 0.0127(10) 0.0025(11) 0.0009(9) -0.0009(13) C8 0.0134(11) 0.0095(14) 0.0102(11) 0.0007(9) 0.0005(9) 0.0007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.996(2) . ? Zn1 N7 1.998(2) 3_544 ? Zn1 N5 2.023(2) 1_556 ? Zn1 N3 2.039(2) 4_565 ? N1 N2 1.305(3) . ? N1 N4 1.347(3) . ? N2 N3 1.349(3) . ? N3 C1 1.348(3) . ? N3 Zn1 2.039(2) 4_465 ? N4 C1 1.325(3) . ? N5 N6 1.304(3) . ? N5 N8 1.361(3) . ? N5 Zn1 2.023(2) 1_554 ? N6 N7 1.344(3) . ? N7 C8 1.360(3) . ? N7 Zn1 1.998(2) 3_554 ? N8 C8 1.327(3) . ? C1 C2 1.482(3) . ? C2 C7 1.397(4) . ? C2 C3 1.400(4) . ? C3 C4 1.395(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.399(4) . ? C5 C8 1.479(3) . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? 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 N1 Zn1 N7 121.65(9) . 3_544 ? N1 Zn1 N5 110.14(8) . 1_556 ? N7 Zn1 N5 108.84(9) 3_544 1_556 ? N1 Zn1 N3 101.18(9) . 4_565 ? N7 Zn1 N3 110.33(8) 3_544 4_565 ? N5 Zn1 N3 102.96(9) 1_556 4_565 ? N2 N1 N4 112.16(19) . . ? N2 N1 Zn1 121.26(16) . . ? N4 N1 Zn1 125.53(16) . . ? N1 N2 N3 107.0(2) . . ? C1 N3 N2 105.9(2) . . ? C1 N3 Zn1 135.89(16) . 4_465 ? N2 N3 Zn1 116.96(15) . 4_465 ? C1 N4 N1 103.6(2) . . ? N6 N5 N8 112.22(19) . . ? N6 N5 Zn1 114.25(16) . 1_554 ? N8 N5 Zn1 129.60(19) . 1_554 ? N5 N6 N7 107.35(19) . . ? N6 N7 C8 105.9(2) . . ? N6 N7 Zn1 113.95(16) . 3_554 ? C8 N7 Zn1 139.75(16) . 3_554 ? C8 N8 N5 103.2(2) . . ? N4 C1 N3 111.3(2) . . ? N4 C1 C2 123.1(2) . . ? N3 C1 C2 125.5(2) . . ? C7 C2 C3 120.3(2) . . ? C7 C2 C1 119.9(3) . . ? C3 C2 C1 119.8(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 C8 120.4(3) . . ? C6 C5 C8 119.4(2) . . ? C7 C6 C5 120.1(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 119.6(3) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? N8 C8 N7 111.32(19) . . ? N8 C8 C5 124.3(3) . . ? N7 C8 C5 124.2(2) . . ? 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 N7 Zn1 N1 N2 135.6(2) 3_544 . . . ? N5 Zn1 N1 N2 6.5(3) 1_556 . . . ? N3 Zn1 N1 N2 -101.9(2) 4_565 . . . ? N7 Zn1 N1 N4 -57.0(2) 3_544 . . . ? N5 Zn1 N1 N4 173.9(2) 1_556 . . . ? N3 Zn1 N1 N4 65.5(2) 4_565 . . . ? N4 N1 N2 N3 0.4(3) . . . . ? Zn1 N1 N2 N3 169.32(17) . . . . ? N1 N2 N3 C1 -0.5(3) . . . . ? N1 N2 N3 Zn1 168.94(18) . . . 4_465 ? N2 N1 N4 C1 -0.1(3) . . . . ? Zn1 N1 N4 C1 -168.49(19) . . . . ? N8 N5 N6 N7 1.0(3) . . . . ? Zn1 N5 N6 N7 -158.88(14) 1_554 . . . ? N5 N6 N7 C8 -1.2(3) . . . . ? N5 N6 N7 Zn1 173.00(15) . . . 3_554 ? N6 N5 N8 C8 -0.4(3) . . . . ? Zn1 N5 N8 C8 155.60(18) 1_554 . . . ? N1 N4 C1 N3 -0.2(3) . . . . ? N1 N4 C1 C2 177.4(2) . . . . ? N2 N3 C1 N4 0.4(3) . . . . ? Zn1 N3 C1 N4 -165.97(19) 4_465 . . . ? N2 N3 C1 C2 -177.1(3) . . . . ? Zn1 N3 C1 C2 16.5(4) 4_465 . . . ? N4 C1 C2 C7 28.7(4) . . . . ? N3 C1 C2 C7 -154.1(3) . . . . ? N4 C1 C2 C3 -148.7(3) . . . . ? N3 C1 C2 C3 28.5(4) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 177.1(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 0.7(4) . . . . ? C3 C4 C5 C8 -176.0(2) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C8 C5 C6 C7 176.7(2) . . . . ? C5 C6 C7 C2 -0.9(4) . . . . ? C3 C2 C7 C6 1.0(4) . . . . ? C1 C2 C7 C6 -176.4(2) . . . . ? N5 N8 C8 N7 -0.4(3) . . . . ? N5 N8 C8 C5 -176.6(2) . . . . ? N6 N7 C8 N8 1.0(3) . . . . ? Zn1 N7 C8 N8 -170.79(18) 3_554 . . . ? N6 N7 C8 C5 177.2(2) . . . . ? Zn1 N7 C8 C5 5.5(4) 3_554 . . . ? C4 C5 C8 N8 -156.0(3) . . . . ? C6 C5 C8 N8 27.3(4) . . . . ? C4 C5 C8 N7 28.3(4) . . . . ? C6 C5 C8 N7 -148.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.405 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.082 #_eof #End of Crystallographic Information File