Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 1350 _publ_contact_author_name 'Ning-Hai Hu' _publ_contact_author_address ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun Institute of Applied Chemistry 5625 Renmin Street Changchun 130022 CHINA ; _publ_contact_author_fax 86-431-85685653 _publ_contact_author_email hunh@ciac.jl.cn _publ_requested_journal CrystEngComm _publ_section_title ; Supramolecular isomerism in zinc hydroxide coordination polymer with pyridine-2,4-dicarboxylic acid: two polymorphs with centrosymmetric two-dimensional and acentric three-dimensional coordination networks ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Li, Zhi-Gang' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; 'Wang, Guan-Hua' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; 'Jia, Heng-Qing' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; 'Hu, Ning-Hai' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; 'Xu, Jing-Wei' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; data_l009 _database_code_depnum_ccdc_archive 'CCDC 604691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 N O6 Zn2' _chemical_formula_sum 'C7 H5 N O6 Zn2' _chemical_formula_weight 329.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 7.7477(8) _cell_length_b 18.698(2) _cell_length_c 5.7744(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 836.51(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3194 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.94 _exptl_crystal_description tabular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1948 _exptl_absorpt_correction_T_max 0.7582 _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _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 Smart APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4528 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1593 _reflns_number_gt 1520 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 1997)' _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^)+(0.0393P)^2^] 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 (1983). Acta Cryst. A39, 876-881; 699 Friedel pairs,' _refine_ls_abs_structure_Flack 0.018(18) _refine_ls_number_reflns 1593 _refine_ls_number_parameters 145 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.032 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.85588(5) 0.46675(2) 1.00989(9) 0.01790(13) Uani 1 1 d . . . Zn2 Zn 0.57068(6) 0.48454(2) 0.53492(10) 0.01949(13) Uani 1 1 d . . . O1 O 1.0026(4) 0.46007(14) 0.6821(6) 0.0203(6) Uani 1 1 d . . . O2 O 1.1082(4) 0.37844(17) 0.4371(6) 0.0308(8) Uani 1 1 d . . . O3 O 1.0285(4) 0.11979(15) 0.6412(5) 0.0270(7) Uani 1 1 d . . . O4 O 0.8768(4) 0.09264(16) 0.9581(6) 0.0315(9) Uani 1 1 d . . . O5 O 0.7170(4) 0.44839(14) 1.2925(5) 0.0180(6) Uani 1 1 d . . . H5A H 0.8100 0.4470 1.3870 0.022 Uiso 1 1 d . . . O6 O 0.6545(3) 0.51174(14) 0.8519(5) 0.0177(6) Uani 1 1 d . . . H6A H 0.6778 0.5605 0.8327 0.021 Uiso 1 1 d . . . N1 N 0.8824(4) 0.35856(16) 0.9646(6) 0.0189(8) Uani 1 1 d . . . C1 C 1.0305(6) 0.3953(2) 0.6134(8) 0.0187(9) Uani 1 1 d . . . C2 C 0.9590(5) 0.3367(2) 0.7682(7) 0.0177(8) Uani 1 1 d . . . C3 C 0.9759(5) 0.2655(2) 0.7115(8) 0.0205(9) Uani 1 1 d . . . H3 H 1.0266 0.2520 0.5722 0.025 Uiso 1 1 calc R . . C4 C 0.9165(5) 0.2144(2) 0.8640(8) 0.0185(9) Uani 1 1 d . . . C5 C 0.8383(5) 0.2366(2) 1.0677(7) 0.0220(10) Uani 1 1 d . . . H5 H 0.7976 0.2032 1.1740 0.026 Uiso 1 1 calc R . . C6 C 0.8215(5) 0.3089(2) 1.1106(7) 0.0220(9) Uani 1 1 d . . . H6 H 0.7661 0.3236 1.2453 0.026 Uiso 1 1 calc R . . C7 C 0.9426(5) 0.1354(2) 0.8161(8) 0.0189(9) 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 0.0217(2) 0.0133(2) 0.0187(2) -0.0020(2) -0.0008(2) -0.00013(14) Zn2 0.0271(3) 0.0161(2) 0.0153(2) 0.0005(3) -0.0012(2) -0.00007(15) O1 0.0245(16) 0.0142(14) 0.0220(16) 0.0008(12) 0.0061(13) -0.0036(12) O2 0.043(2) 0.0211(17) 0.0286(19) -0.0019(13) 0.0152(15) -0.0050(14) O3 0.0431(19) 0.0147(14) 0.0232(17) -0.0037(13) 0.0048(15) -0.0002(13) O4 0.0470(19) 0.0134(14) 0.034(3) 0.0031(13) 0.0104(14) 0.0022(13) O5 0.0227(15) 0.0161(13) 0.0151(14) -0.0057(11) 0.0129(12) -0.0027(11) O6 0.0170(16) 0.0147(14) 0.0214(16) -0.0003(12) -0.0004(12) -0.0022(11) N1 0.0249(17) 0.0136(16) 0.018(2) -0.0018(13) 0.0022(14) 0.0004(12) C1 0.021(2) 0.015(2) 0.021(2) -0.0003(17) -0.0003(18) -0.0006(16) C2 0.020(2) 0.0145(18) 0.019(2) -0.0005(16) 0.0020(16) -0.0004(15) C3 0.023(2) 0.017(2) 0.022(2) -0.0011(17) 0.0037(17) 0.0025(16) C4 0.018(2) 0.017(2) 0.021(2) -0.0004(18) -0.0020(18) -0.0028(15) C5 0.029(2) 0.0154(18) 0.021(3) 0.0027(17) 0.0015(18) -0.0035(15) C6 0.029(2) 0.021(2) 0.017(2) -0.0021(16) 0.0065(18) 0.0014(17) C7 0.021(2) 0.0143(19) 0.022(2) -0.0009(17) -0.0028(18) -0.0006(16) _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 O5 1.984(3) . ? Zn1 O6 1.994(3) . ? Zn1 O1 2.016(3) 2_765 ? Zn1 N1 2.050(3) . ? Zn1 O1 2.212(3) . ? Zn2 O5 1.924(3) 1_554 ? Zn2 O6 2.007(3) . ? Zn2 O6 2.041(3) 2_664 ? Zn2 O3 2.071(3) 3_455 ? Zn2 O4 2.109(3) 4_654 ? Zn2 Zn2 3.1416(4) 2_665 ? O1 C1 1.293(5) . ? O2 C1 1.224(5) . ? O3 C7 1.244(5) . ? O4 C7 1.254(5) . ? O5 H5A 0.9039 . ? O6 H6A 0.9360 . ? N1 C6 1.340(5) . ? N1 C2 1.344(5) . ? C1 C2 1.517(6) . ? C2 C3 1.378(6) . ? C3 C4 1.378(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 C7 1.516(6) . ? C5 C6 1.380(6) . ? C5 H5 0.9300 . ? C6 H6 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 O5 Zn1 O6 91.44(12) . . ? O5 Zn1 O1 90.38(13) . 2_765 ? O6 Zn1 O1 111.41(12) . 2_765 ? O5 Zn1 N1 89.33(12) . . ? O6 Zn1 N1 115.87(12) . . ? O1 Zn1 N1 132.71(13) 2_765 . ? O5 Zn1 O1 166.58(10) . . ? O6 Zn1 O1 91.98(12) . . ? O1 Zn1 O1 100.43(6) 2_765 . ? N1 Zn1 O1 77.50(12) . . ? O5 Zn2 O6 124.18(12) 1_554 . ? O5 Zn2 O6 97.98(12) 1_554 2_664 ? O6 Zn2 O6 137.73(10) . 2_664 ? O5 Zn2 O3 88.72(12) 1_554 3_455 ? O6 Zn2 O3 91.12(11) . 3_455 ? O6 Zn2 O3 92.90(11) 2_664 3_455 ? O5 Zn2 O4 94.00(12) 1_554 4_654 ? O6 Zn2 O4 83.49(12) . 4_654 ? O6 Zn2 O4 91.35(11) 2_664 4_654 ? O3 Zn2 O4 174.59(13) 3_455 4_654 ? C1 O1 Zn1 113.2(3) . 2_764 ? C1 O1 Zn1 113.7(3) . . ? Zn1 O1 Zn1 131.56(14) 2_764 . ? C7 O3 Zn2 123.1(3) . 3 ? C7 O4 Zn2 132.1(3) . 4_645 ? Zn2 O5 Zn1 148.97(15) 1_556 . ? Zn2 O5 H5A 92.3 1_556 . ? Zn1 O5 H5A 94.0 . . ? Zn1 O6 Zn2 124.29(14) . . ? Zn1 O6 Zn2 116.51(14) . 2_665 ? Zn2 O6 Zn2 101.80(12) . 2_665 ? Zn1 O6 H6A 108.3 . . ? Zn2 O6 H6A 101.6 . . ? Zn2 O6 H6A 101.1 2_665 . ? C6 N1 C2 118.4(3) . . ? C6 N1 Zn1 124.6(3) . . ? C2 N1 Zn1 116.8(3) . . ? O2 C1 O1 125.3(4) . . ? O2 C1 C2 119.0(4) . . ? O1 C1 C2 115.7(4) . . ? N1 C2 C3 122.4(4) . . ? N1 C2 C1 116.1(3) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 C7 120.9(4) . . ? C5 C4 C7 120.3(4) . . ? C6 C5 C4 119.1(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 122.2(4) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O3 C7 O4 126.8(4) . . ? O3 C7 C4 116.6(4) . . ? O4 C7 C4 116.6(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O2 0.94 2.10 2.800(4) 130 2_765 O6 H6A O4 0.94 2.28 2.742(4) 109 4_654 O5 H5A O1 0.90 2.28 3.163(4) 166 1_556 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.524 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.094 #End of the file data_l016 _database_code_depnum_ccdc_archive 'CCDC 606914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 N O6 Zn2' _chemical_formula_sum 'C7 H5 N O6 Zn2' _chemical_formula_weight 329.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.3424(11) _cell_length_b 6.7836(8) _cell_length_c 13.9741(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.688(2) _cell_angle_gamma 90.00 _cell_volume 870.25(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1719 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.03 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3099 _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 Smart APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4714 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.06 _reflns_number_total 1727 _reflns_number_gt 1437 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 1997)' _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^)+(0.0368P)^2^+0.4260P] 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_number_reflns 1727 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 0.39900(4) 0.70349(5) 0.87082(3) 0.01303(14) Uani 1 1 d . . . Zn2 Zn 0.41373(4) 1.19924(5) 0.87972(3) 0.01185(13) Uani 1 1 d . . . N1 N 0.1704(3) 0.6883(4) 0.8874(2) 0.0152(6) Uani 1 1 d . . . O1 O 0.4073(2) 0.7664(3) 1.01734(16) 0.0154(5) Uani 1 1 d . . . O2 O 0.2778(3) 0.8456(4) 1.13122(17) 0.0213(6) Uani 1 1 d . . . O3 O -0.2583(2) 0.8004(3) 1.04186(17) 0.0186(5) Uani 1 1 d . . . O4 O -0.3655(2) 0.6837(4) 0.89574(18) 0.0221(6) Uani 1 1 d . . . O5 O 0.3820(2) 0.9591(3) 0.80885(16) 0.0143(5) Uani 1 1 d . . . H5A H 0.4450 0.9605 0.7714 0.017 Uiso 1 1 d . . . O6 O 0.3990(2) 0.4456(3) 0.80963(15) 0.0130(5) Uani 1 1 d . . . H6A H 0.3210 0.4510 0.7580 0.016 Uiso 1 1 d . . . C1 C 0.2857(4) 0.7918(5) 1.0491(2) 0.0131(7) Uani 1 1 d . . . C2 C 0.1502(3) 0.7461(5) 0.9760(2) 0.0128(7) Uani 1 1 d . . . C3 C 0.0137(3) 0.7630(4) 0.9999(2) 0.0135(7) Uani 1 1 d . . . H3 H 0.0039 0.8058 1.0616 0.016 Uiso 1 1 calc R . . C4 C -0.1082(3) 0.7160(5) 0.9314(2) 0.0125(7) Uani 1 1 d . . . C5 C -0.0886(4) 0.6498(5) 0.8403(2) 0.0181(7) Uani 1 1 d . . . H5 H -0.1681 0.6131 0.7932 0.022 Uiso 1 1 calc R . . C6 C 0.0518(4) 0.6398(5) 0.8212(2) 0.0200(8) Uani 1 1 d . . . H6 H 0.0645 0.5977 0.7600 0.024 Uiso 1 1 calc R . . C7 C -0.2586(4) 0.7346(5) 0.9572(2) 0.0138(7) 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 0.0131(2) 0.0107(2) 0.0157(2) -0.00045(15) 0.00378(15) 0.00036(15) Zn2 0.0103(2) 0.0107(2) 0.0144(2) -0.00025(15) 0.00212(15) 0.00001(14) N1 0.0141(14) 0.0139(15) 0.0177(14) -0.0028(11) 0.0035(11) -0.0001(11) O1 0.0096(11) 0.0194(13) 0.0164(11) -0.0002(10) 0.0006(9) 0.0001(9) O2 0.0176(12) 0.0278(15) 0.0181(12) -0.0042(11) 0.0020(10) -0.0032(11) O3 0.0130(12) 0.0256(15) 0.0185(12) -0.0020(10) 0.0057(9) -0.0007(10) O4 0.0105(12) 0.0274(15) 0.0275(14) -0.0084(11) 0.0013(10) -0.0022(10) O5 0.0174(12) 0.0116(13) 0.0154(11) 0.0000(9) 0.0071(9) -0.0007(9) O6 0.0168(12) 0.0101(12) 0.0108(11) -0.0021(9) -0.0010(9) 0.0016(9) C1 0.0122(16) 0.0115(17) 0.0152(16) 0.0007(13) 0.0018(13) -0.0014(13) C2 0.0126(16) 0.0097(16) 0.0160(16) 0.0018(13) 0.0025(13) 0.0004(13) C3 0.0141(16) 0.0135(17) 0.0126(15) 0.0002(14) 0.0019(13) -0.0002(14) C4 0.0098(16) 0.0093(16) 0.0183(16) 0.0027(13) 0.0025(13) 0.0018(12) C5 0.0150(17) 0.0198(19) 0.0177(17) -0.0037(15) -0.0013(13) -0.0019(14) C6 0.0200(18) 0.025(2) 0.0153(17) -0.0041(15) 0.0033(14) 0.0001(16) C7 0.0144(16) 0.0074(16) 0.0194(17) 0.0029(14) 0.0024(13) 0.0008(13) _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 O5 1.931(2) . ? Zn1 O6 1.947(2) . ? Zn1 O1 2.079(2) . ? Zn1 O4 2.167(2) 1_655 ? Zn1 N1 2.193(3) . ? Zn2 O5 1.901(2) . ? Zn2 O6 1.929(2) 1_565 ? Zn2 O3 1.975(2) 3_577 ? Zn2 O1 2.007(2) 3_677 ? N1 C6 1.346(4) . ? N1 C2 1.346(4) . ? O1 C1 1.306(4) . ? O2 C1 1.219(4) . ? O3 C7 1.264(4) . ? O4 C7 1.239(4) . ? O5 H5A 0.8569 . ? O6 H6A 0.9263 . ? C1 C2 1.504(4) . ? C2 C3 1.382(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 C7 1.520(4) . ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 H6 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 O5 Zn1 O6 128.05(10) . . ? O5 Zn1 O1 104.02(9) . . ? O6 Zn1 O1 127.87(9) . . ? O5 Zn1 O4 97.13(10) . 1_655 ? O6 Zn1 O4 86.11(9) . 1_655 ? O1 Zn1 O4 90.18(9) . 1_655 ? O5 Zn1 N1 95.09(10) . . ? O6 Zn1 N1 94.79(10) . . ? O1 Zn1 N1 76.41(9) . . ? O4 Zn1 N1 163.71(10) 1_655 . ? O5 Zn2 O6 119.24(10) . 1_565 ? O5 Zn2 O3 103.34(10) . 3_577 ? O6 Zn2 O3 106.86(10) 1_565 3_577 ? O5 Zn2 O1 120.10(9) . 3_677 ? O6 Zn2 O1 103.58(9) 1_565 3_677 ? O3 Zn2 O1 101.69(10) 3_577 3_677 ? C6 N1 C2 117.8(3) . . ? C6 N1 Zn1 129.3(2) . . ? C2 N1 Zn1 112.9(2) . . ? C1 O1 Zn2 113.74(19) . 3_677 ? C1 O1 Zn1 119.10(19) . . ? Zn2 O1 Zn1 127.15(11) 3_677 . ? C7 O3 Zn2 130.2(2) . 3_577 ? C7 O4 Zn1 139.2(2) . 1_455 ? Zn2 O5 Zn1 122.95(12) . . ? Zn2 O5 H5A 104.5 . . ? Zn1 O5 H5A 106.0 . . ? Zn2 O6 Zn1 124.14(11) 1_545 . ? Zn2 O6 H6A 113.7 1_545 . ? Zn1 O6 H6A 104.0 . . ? O2 C1 O1 124.6(3) . . ? O2 C1 C2 120.7(3) . . ? O1 C1 C2 114.6(3) . . ? N1 C2 C3 122.7(3) . . ? N1 C2 C1 116.2(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 C7 119.7(3) . . ? C5 C4 C7 121.8(3) . . ? C6 C5 C4 118.7(3) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 122.9(3) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? O4 C7 O3 127.5(3) . . ? O4 C7 C4 118.3(3) . . ? O3 C7 C4 114.2(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O6 0.86 2.01 2.862(4) 175 2_656 O6 H6A O2 0.93 2.22 2.908(3) 130 4_575 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.496 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.142 # Attachment 'Compound1.cif' # File Zn2(OH)2(2,4-pyda) P21/c (1) -120 \%C data_l084 _database_code_depnum_ccdc_archive 'CCDC 649373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 N O6 Zn2' _chemical_formula_sum 'C7 H5 N O6 Zn2' _chemical_formula_weight 329.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.3365(11) _cell_length_b 6.7815(8) _cell_length_c 13.9607(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.704(2) _cell_angle_gamma 90.00 _cell_volume 868.55(18) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 1672 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.03 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.307 _exptl_absorpt_correction_T_max 0.798 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4671 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.03 _reflns_number_total 1711 _reflns_number_gt 1443 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0368P)^2^+0.4260P] 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_number_reflns 1711 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.39914(4) 0.70215(5) 0.87100(2) 0.01057(12) Uani 1 1 d . . . Zn2 Zn 0.41341(4) 1.19769(5) 0.87934(2) 0.00985(12) Uani 1 1 d . . . N1 N 0.1707(3) 0.6866(3) 0.88781(18) 0.0127(5) Uani 1 1 d . . . O1 O 0.4075(2) 0.7670(3) 1.01744(15) 0.0140(5) Uani 1 1 d . . . O2 O 0.2778(2) 0.8488(3) 1.13097(15) 0.0175(5) Uani 1 1 d . . . O3 O -0.2583(2) 0.8019(3) 1.04181(15) 0.0154(5) Uani 1 1 d . . . O4 O -0.3660(2) 0.6818(3) 0.89630(16) 0.0183(5) Uani 1 1 d . . . O5 O 0.3818(2) 0.9571(3) 0.80851(15) 0.0120(5) Uani 1 1 d . . . H5A H 0.4450 0.9605 0.7714 0.014 Uiso 1 1 d . . . O6 O 0.3996(2) 0.4440(3) 0.80928(14) 0.0112(5) Uani 1 1 d . . . H6A H 0.3210 0.4510 0.7580 0.013 Uiso 1 1 d . . . C1 C 0.2860(3) 0.7929(4) 1.0489(2) 0.0116(6) Uani 1 1 d . . . C2 C 0.1502(3) 0.7460(4) 0.9760(2) 0.0118(6) Uani 1 1 d . . . C3 C 0.0137(3) 0.7634(4) 1.0004(2) 0.0121(6) Uani 1 1 d . . . H3 H 0.0040 0.8064 1.0621 0.015 Uiso 1 1 calc R . . C4 C -0.1089(3) 0.7156(4) 0.9312(2) 0.0118(6) Uani 1 1 d . . . C5 C -0.0884(3) 0.6473(4) 0.8407(2) 0.0149(7) Uani 1 1 d . . . H5 H -0.1675 0.6087 0.7937 0.018 Uiso 1 1 calc R . . C6 C 0.0526(3) 0.6376(5) 0.8219(2) 0.0155(7) Uani 1 1 d . . . H6 H 0.0655 0.5953 0.7607 0.019 Uiso 1 1 calc R . . C7 C -0.2586(3) 0.7338(4) 0.9576(2) 0.0125(6) 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 0.0103(2) 0.0093(2) 0.0126(2) -0.00049(13) 0.00357(15) 0.00026(13) Zn2 0.0088(2) 0.0096(2) 0.0115(2) -0.00033(13) 0.00264(14) -0.00026(13) N1 0.0123(13) 0.0120(13) 0.0132(13) -0.0012(10) 0.0011(11) -0.0003(10) O1 0.0103(11) 0.0185(12) 0.0131(11) -0.0003(9) 0.0021(9) -0.0017(9) O2 0.0160(12) 0.0239(13) 0.0126(11) -0.0014(9) 0.0023(9) -0.0024(10) O3 0.0108(11) 0.0227(13) 0.0141(11) -0.0025(9) 0.0058(9) -0.0009(9) O4 0.0109(11) 0.0216(12) 0.0220(12) -0.0081(10) 0.0019(10) -0.0018(9) O5 0.0138(11) 0.0107(11) 0.0131(11) -0.0012(8) 0.0071(9) -0.0020(8) O6 0.0125(11) 0.0098(11) 0.0101(10) -0.0004(8) -0.0009(9) 0.0003(8) C1 0.0103(15) 0.0106(15) 0.0140(15) 0.0042(11) 0.0028(12) -0.0002(12) C2 0.0129(16) 0.0086(14) 0.0144(15) -0.0001(12) 0.0039(12) -0.0003(12) C3 0.0134(16) 0.0111(15) 0.0117(15) 0.0007(13) 0.0023(13) -0.0006(13) C4 0.0110(16) 0.0080(15) 0.0161(15) 0.0031(11) 0.0017(13) 0.0001(11) C5 0.0119(16) 0.0163(17) 0.0150(16) -0.0031(13) -0.0012(13) -0.0018(13) C6 0.0168(16) 0.0174(17) 0.0127(15) -0.0046(12) 0.0038(13) -0.0004(13) C7 0.0135(16) 0.0060(14) 0.0184(16) 0.0033(12) 0.0037(13) 0.0012(12) 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 O5 1.930(2) . ? Zn1 O6 1.9516(19) . ? Zn1 O1 2.078(2) . ? Zn1 O4 2.160(2) 1_655 ? Zn1 N1 2.191(3) . ? Zn2 O5 1.902(2) . ? Zn2 O6 1.928(2) 1_565 ? Zn2 O3 1.975(2) 3_577 ? Zn2 O1 2.009(2) 3_677 ? N1 C6 1.340(4) . ? N1 C2 1.343(4) . ? O1 C1 1.303(4) . ? O2 C1 1.222(4) . ? O3 C7 1.262(4) . ? O4 C7 1.242(4) . ? O5 H5A 0.8549 . ? O6 H6A 0.9265 . ? C1 C2 1.505(4) . ? C2 C3 1.384(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 C7 1.516(4) . ? C5 C6 1.391(4) . ? C5 H5 0.9300 . ? C6 H6 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 O5 Zn1 O6 127.67(9) . . ? O5 Zn1 O1 103.87(8) . . ? O6 Zn1 O1 128.41(9) . . ? O5 Zn1 O4 97.38(9) . 1_655 ? O6 Zn1 O4 85.96(8) . 1_655 ? O1 Zn1 O4 90.07(8) . 1_655 ? O5 Zn1 N1 95.16(9) . . ? O6 Zn1 N1 94.95(9) . . ? O1 Zn1 N1 76.36(9) . . ? O4 Zn1 N1 163.40(9) 1_655 . ? O5 Zn2 O6 119.35(9) . 1_565 ? O5 Zn2 O3 103.41(9) . 3_577 ? O6 Zn2 O3 107.14(9) 1_565 3_577 ? O5 Zn2 O1 120.22(9) . 3_677 ? O6 Zn2 O1 103.23(9) 1_565 3_677 ? O3 Zn2 O1 101.47(9) 3_577 3_677 ? C6 N1 C2 117.7(3) . . ? C6 N1 Zn1 129.1(2) . . ? C2 N1 Zn1 113.0(2) . . ? C1 O1 Zn2 113.76(18) . 3_677 ? C1 O1 Zn1 118.99(19) . . ? Zn2 O1 Zn1 127.23(11) 3_677 . ? C7 O3 Zn2 130.1(2) . 3_577 ? C7 O4 Zn1 139.4(2) . 1_455 ? Zn2 O5 Zn1 122.79(11) . . ? Zn2 O5 H5A 103.5 . . ? Zn1 O5 H5A 106.8 . . ? Zn2 O6 Zn1 123.97(10) 1_545 . ? Zn2 O6 H6A 113.9 1_545 . ? Zn1 O6 H6A 103.2 . . ? O2 C1 O1 124.6(3) . . ? O2 C1 C2 120.5(3) . . ? O1 C1 C2 114.8(3) . . ? N1 C2 C3 123.1(3) . . ? N1 C2 C1 116.0(3) . . ? C3 C2 C1 120.9(3) . . ? C4 C3 C2 119.0(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 C7 119.2(3) . . ? C5 C4 C7 122.5(3) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 123.0(3) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? O4 C7 O3 127.4(3) . . ? O4 C7 C4 118.1(3) . . ? O3 C7 C4 114.5(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O6 0.85 2.00 2.850(3) 174 2_656 O6 H6A O2 0.93 2.21 2.901(3) 131 4_575 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.437 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.096 # End of the file # Attachment 'Compound2.cif' # File Zn2(OH)2(2,4-pyda) Pna21 (2) -120 \%C data_l085 _database_code_depnum_ccdc_archive 'CCDC 649374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 N O6 Zn2' _chemical_formula_sum 'C7 H5 N O6 Zn2' _chemical_formula_weight 329.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 7.6827(6) _cell_length_b 18.7212(14) _cell_length_c 5.7833(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 831.81(11) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 3848 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 25.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3760 _exptl_absorpt_correction_T_max 0.6043 _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4343 _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1577 _reflns_number_gt 1546 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Bruker, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0369P)^2^+0.0620P] 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 (1983). Acta Cryst. A39, 876-881; 679 Friedel pairs,' _refine_ls_abs_structure_Flack 0.021(15) _refine_ls_number_reflns 1577 _refine_ls_number_parameters 139 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.005 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.85735(4) 0.466304(16) 1.00989(7) 0.01088(11) Uani 1 1 d . . . Zn2 Zn 0.57247(4) 0.484952(17) 0.53486(8) 0.01198(11) Uani 1 1 d . . . O1 O 1.0013(3) 0.45970(11) 0.6804(4) 0.0125(5) Uani 1 1 d . . . O2 O 1.1090(3) 0.37795(12) 0.4365(4) 0.0129(3) Uani 1 1 d . . . O3 O 1.0300(3) 0.11954(13) 0.6412(4) 0.0170(5) Uani 1 1 d . . . O4 O 0.8738(3) 0.09248(12) 0.9569(4) 0.0183(6) Uani 1 1 d . . . O5 O 0.7197(3) 0.44756(12) 1.2928(4) 0.0129(3) Uani 1 1 d . . . H5A H 0.7450 0.4450 1.4310 0.015 Uiso 1 1 d . . . O6 O 0.6545(3) 0.51226(12) 0.8538(4) 0.0117(5) Uani 1 1 d . . . H6A H 0.6778 0.5605 0.8327 0.014 Uiso 1 1 d . . . N1 N 0.8836(4) 0.35808(14) 0.9659(5) 0.0132(7) Uani 1 1 d . . . C1 C 1.0296(4) 0.39477(18) 0.6115(6) 0.0129(7) Uani 1 1 d . . . C2 C 0.9593(4) 0.33690(18) 0.7678(6) 0.0108(6) Uani 1 1 d . . . C3 C 0.9782(5) 0.26497(17) 0.7119(6) 0.0137(7) Uani 1 1 d . . . H3 H 1.0304 0.2514 0.5736 0.016 Uiso 1 1 calc R . . C4 C 0.9180(4) 0.21396(19) 0.8660(6) 0.0124(7) Uani 1 1 d . . . C5 C 0.8386(4) 0.23633(17) 1.0691(6) 0.0151(8) Uani 1 1 d . . . H5 H 0.7960 0.2031 1.1744 0.018 Uiso 1 1 calc R . . C6 C 0.8238(5) 0.30912(17) 1.1130(6) 0.0142(7) Uani 1 1 d . . . H6 H 0.7705 0.3241 1.2491 0.017 Uiso 1 1 calc R . . C7 C 0.9418(4) 0.13487(17) 0.8167(6) 0.0133(7) 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 0.01312(19) 0.00832(17) 0.01121(19) -0.00103(19) -0.00057(18) 0.00013(11) Zn2 0.0169(2) 0.00972(17) 0.0093(2) 0.00017(19) -0.00069(17) 0.00000(12) O1 0.0161(13) 0.0104(11) 0.0110(12) 0.0002(9) 0.0020(10) -0.0015(9) O2 0.0199(9) 0.0096(7) 0.0092(8) -0.0014(6) 0.0095(7) -0.0021(7) O3 0.0274(14) 0.0114(11) 0.0120(13) 0.0001(10) 0.0012(11) 0.0007(10) O4 0.0302(14) 0.0069(11) 0.0180(18) 0.0027(9) 0.0067(10) 0.0025(10) O5 0.0199(9) 0.0096(7) 0.0092(8) -0.0014(6) 0.0095(7) -0.0021(7) O6 0.0120(12) 0.0110(11) 0.0120(12) -0.0008(9) -0.0002(9) 0.0009(9) N1 0.0175(13) 0.0082(12) 0.0139(19) -0.0015(11) 0.0006(11) 0.0007(10) C1 0.0100(16) 0.0115(15) 0.0171(17) 0.0013(13) -0.0029(13) -0.0002(12) C2 0.0128(15) 0.0126(15) 0.0071(15) 0.0006(13) 0.0005(12) 0.0012(12) C3 0.0152(17) 0.0121(16) 0.0139(16) -0.0025(13) 0.0007(14) -0.0001(13) C4 0.0147(17) 0.0093(15) 0.0134(18) -0.0008(14) -0.0025(14) 0.0011(12) C5 0.0186(16) 0.0097(14) 0.017(2) 0.0012(14) -0.0002(14) -0.0009(12) C6 0.0219(17) 0.0116(16) 0.0091(16) -0.0044(13) 0.0048(14) -0.0010(14) C7 0.0140(16) 0.0101(15) 0.0158(19) -0.0018(14) -0.0031(14) -0.0002(12) 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 O5 1.979(2) . ? Zn1 O6 1.996(2) . ? Zn1 O1 2.018(2) 2_765 ? Zn1 N1 2.052(3) . ? Zn1 O1 2.207(3) . ? Zn2 O5 1.931(2) 1_554 ? Zn2 O6 2.015(2) . ? Zn2 O6 2.034(2) 2_664 ? Zn2 O3 2.076(2) 3_455 ? Zn2 O4 2.104(2) 4_654 ? Zn2 Zn2 3.1494(7) 2_665 ? O1 C1 1.298(4) . ? O2 C1 1.223(4) . ? O3 C7 1.254(4) . ? O4 C7 1.249(4) . ? O5 H5A 0.8242 . ? O6 H6A 0.9288 . ? N1 C6 1.333(4) . ? N1 C2 1.345(4) . ? C1 C2 1.511(5) . ? C2 C3 1.392(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.388(5) . ? C4 C7 1.519(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9300 . ? C6 H6 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 O5 Zn1 O6 91.88(10) . . ? O5 Zn1 O1 90.29(11) . 2_765 ? O6 Zn1 O1 110.20(9) . 2_765 ? O5 Zn1 N1 88.85(10) . . ? O6 Zn1 N1 116.51(10) . . ? O1 Zn1 N1 133.28(10) 2_765 . ? O5 Zn1 O1 166.30(9) . . ? O6 Zn1 O1 91.44(10) . . ? O1 Zn1 O1 101.00(5) 2_765 . ? N1 Zn1 O1 77.78(10) . . ? O5 Zn2 O6 124.92(10) 1_554 . ? O5 Zn2 O6 97.94(10) 1_554 2_664 ? O6 Zn2 O6 137.10(8) . 2_664 ? O5 Zn2 O3 88.01(9) 1_554 3_455 ? O6 Zn2 O3 90.98(9) . 3_455 ? O6 Zn2 O3 92.40(10) 2_664 3_455 ? O5 Zn2 O4 94.38(10) 1_554 4_654 ? O6 Zn2 O4 83.81(9) . 4_654 ? O6 Zn2 O4 91.91(9) 2_664 4_654 ? O3 Zn2 O4 174.74(10) 3_455 4_654 ? O5 Zn2 Zn2 159.65(8) 1_554 2_665 ? O6 Zn2 Zn2 39.17(7) . 2_665 ? O6 Zn2 Zn2 99.49(7) 2_664 2_665 ? O3 Zn2 Zn2 80.86(7) 3_455 2_665 ? O4 Zn2 Zn2 95.46(7) 4_654 2_665 ? O5 Zn2 Zn2 66.81(7) 1_554 2_664 ? O6 Zn2 Zn2 154.91(7) . 2_664 ? O6 Zn2 Zn2 38.73(7) 2_664 2_664 ? O3 Zn2 Zn2 112.63(7) 3_455 2_664 ? O4 Zn2 Zn2 72.63(7) 4_654 2_664 ? Zn2 Zn2 Zn2 133.32(2) 2_665 2_664 ? C1 O1 Zn1 113.8(2) . 2_764 ? C1 O1 Zn1 113.7(2) . . ? Zn1 O1 Zn1 130.80(11) 2_764 . ? C7 O3 Zn2 122.7(2) . 3 ? C7 O4 Zn2 131.7(2) . 4_645 ? Zn2 O5 Zn1 147.98(13) 1_556 . ? Zn2 O5 H5A 57.1 1_556 . ? Zn1 O5 H5A 133.3 . . ? Zn1 O6 Zn2 123.28(11) . . ? Zn1 O6 Zn2 116.59(12) . 2_665 ? Zn2 O6 Zn2 102.10(10) . 2_665 ? Zn1 O6 H6A 109.1 . . ? Zn2 O6 H6A 100.7 . . ? Zn2 O6 H6A 102.0 2_665 . ? C6 N1 C2 119.4(3) . . ? C6 N1 Zn1 124.5(2) . . ? C2 N1 Zn1 116.1(2) . . ? O2 C1 O1 125.4(3) . . ? O2 C1 C2 119.3(3) . . ? O1 C1 C2 115.4(3) . . ? N1 C2 C3 121.9(3) . . ? N1 C2 C1 116.9(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 118.8(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 C7 120.7(3) . . ? C5 C4 C7 120.4(3) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N1 C6 C5 121.9(3) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? O3 C7 O4 127.3(3) . . ? O3 C7 C4 116.1(3) . . ? O4 C7 C4 116.5(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O2 0.93 2.09 2.785(3) 130 2_765 O6 H6A O4 0.93 2.29 2.752(3) 110 4_654 O5 H5A O1 0.82 2.46 3.124(3) 139 1_556 O5 H5A O3 0.82 2.38 2.786(3) 111 3_456 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.863 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.133 # End of the file