# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Zheng, Fakun' _publ_contact_author_name 'Zheng, Fakun' _publ_contact_author_email zfk@fjirsm.ac.cn _publ_section_title ; Structures and photoluminescence of zinc(II) coordination polymers based on in situ generated 1H-tetrazolate-5-propionic acid ligands ; # Attachment '- polymer 1.CIF' #===================================================================== # corresponding information _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_phone '+86 591 8370 4827' _publ_contact_author_fax '+86 591 8371 4946' #===================================================================== data_14_1 _database_code_depnum_ccdc_archive 'CCDC 815796' #TrackingRef '- polymer 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn(N4CCH2CH2COO)]n' ; _chemical_name_common '[Zn(N4CCH2CH2COO)]n' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Zn(N4CCH2CH2COO)]n' _chemical_formula_sum 'C4 H4 N4 O2 Zn' _chemical_formula_weight 205.48 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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.822(10) _cell_length_b 10.44(2) _cell_length_c 8.870(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.396(13) _cell_angle_gamma 90.00 _cell_volume 619.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 3.0448 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Chip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 3.909 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7482 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4079 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.33 _reflns_number_total 1134 _reflns_number_gt 1013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0338P)^2^+0.2911P] 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 1134 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.26844(4) 0.24321(2) 0.22304(4) 0.02191(14) Uani 1 1 d . . . O1 O 0.1875(3) 0.27263(17) 0.4247(2) 0.0276(4) Uani 1 1 d . . . O2 O 0.0141(2) 0.32131(17) 0.5983(2) 0.0262(4) Uani 1 1 d . . . C1 C -0.4645(3) 0.4782(2) 0.2776(3) 0.0195(5) Uani 1 1 d . . . C2 C -0.3137(3) 0.4189(2) 0.4009(3) 0.0203(5) Uani 1 1 d . . . H2A H -0.3746 0.3490 0.4472 0.024 Uiso 1 1 calc R . . H2B H -0.2669 0.4819 0.4802 0.024 Uiso 1 1 calc R . . C3 C -0.1358(3) 0.3679(2) 0.3368(3) 0.0234(6) Uani 1 1 d . . . H3A H -0.1823 0.3006 0.2631 0.028 Uiso 1 1 calc R . . H3B H -0.0835 0.4366 0.2825 0.028 Uiso 1 1 calc R . . C4 C 0.0299(3) 0.3163(2) 0.4584(3) 0.0208(5) Uani 1 1 d . . . N1 N -0.6209(3) 0.41645(18) 0.1953(2) 0.0226(5) Uani 1 1 d . . . N2 N -0.7181(3) 0.5016(2) 0.0898(3) 0.0345(6) Uani 1 1 d . . . N3 N -0.6240(3) 0.6089(2) 0.1080(3) 0.0332(6) Uani 1 1 d . . . N4 N -0.4625(3) 0.59812(19) 0.2272(2) 0.0231(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 0.01812(19) 0.01523(19) 0.0299(2) -0.00211(11) -0.00124(14) 0.00000(10) O1 0.0217(9) 0.0312(10) 0.0284(11) -0.0004(8) 0.0018(8) 0.0078(8) O2 0.0231(9) 0.0301(10) 0.0242(10) 0.0036(8) 0.0017(7) 0.0026(7) C1 0.0189(11) 0.0148(12) 0.0257(14) -0.0032(10) 0.0064(10) -0.0007(9) C2 0.0210(11) 0.0180(12) 0.0217(13) 0.0002(10) 0.0038(10) -0.0004(10) C3 0.0207(12) 0.0231(13) 0.0242(14) 0.0002(11) -0.0007(10) 0.0017(10) C4 0.0209(12) 0.0149(12) 0.0253(14) 0.0006(10) 0.0008(10) -0.0047(9) N1 0.0207(10) 0.0160(10) 0.0285(12) -0.0003(9) -0.0014(8) 0.0001(8) N2 0.0304(12) 0.0234(12) 0.0437(16) 0.0031(11) -0.0078(10) 0.0007(10) N3 0.0309(12) 0.0209(12) 0.0420(15) 0.0044(10) -0.0069(10) 0.0008(9) N4 0.0204(10) 0.0158(10) 0.0307(13) 0.0017(9) -0.0007(9) -0.0004(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 O2 1.982(3) 4_565 ? Zn1 N1 1.994(4) 1_655 ? Zn1 O1 1.997(4) . ? Zn1 N4 2.003(3) 2_545 ? O1 C4 1.257(3) . ? O2 C4 1.268(4) . ? O2 Zn1 1.982(3) 4_566 ? C1 N4 1.331(4) . ? C1 N1 1.334(3) . ? C1 C2 1.481(4) . ? C2 C3 1.533(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.500(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 N2 1.364(3) . ? N1 Zn1 1.994(4) 1_455 ? N2 N3 1.285(4) . ? N3 N4 1.372(3) . ? N4 Zn1 2.003(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 N1 123.39(9) 4_565 1_655 ? O2 Zn1 O1 100.71(12) 4_565 . ? N1 Zn1 O1 98.58(10) 1_655 . ? O2 Zn1 N4 109.49(13) 4_565 2_545 ? N1 Zn1 N4 117.62(14) 1_655 2_545 ? O1 Zn1 N4 101.91(10) . 2_545 ? C4 O1 Zn1 132.01(17) . . ? C4 O2 Zn1 107.35(16) . 4_566 ? N4 C1 N1 109.3(2) . . ? N4 C1 C2 126.1(2) . . ? N1 C1 C2 124.5(2) . . ? C1 C2 C3 110.9(2) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 113.4(2) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O1 C4 O2 119.3(2) . . ? O1 C4 C3 121.2(2) . . ? O2 C4 C3 119.4(2) . . ? C1 N1 N2 106.7(2) . . ? C1 N1 Zn1 130.71(18) . 1_455 ? N2 N1 Zn1 122.13(17) . 1_455 ? N3 N2 N1 108.6(2) . . ? N2 N3 N4 109.3(2) . . ? C1 N4 N3 106.02(19) . . ? C1 N4 Zn1 133.46(18) . 2 ? N3 N4 Zn1 120.20(17) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.717 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.069 #===================================================================== data_14_2 _database_code_depnum_ccdc_archive 'CCDC 815797' #TrackingRef '- polymer 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn2(C10N2H8)(N4CCH2CH2COO)(N3)(u2-OH)]n' ; _chemical_name_common '[Zn2(C10N2H8)(N4CCH2CH2COO)(N3)(u2-OH)]n' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Zn2(C10N2H8)(N4CCH2CH2COO)(N3)(u2-OH)]n' _chemical_formula_sum 'C14 H13 N9 O3 Zn2' _chemical_formula_weight 486.07 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(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.371(4) _cell_length_b 22.545(10) _cell_length_c 9.785(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.6030(10) _cell_angle_gamma 90.00 _cell_volume 1704.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 2.2553 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 2.854 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10966 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3107 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0400P)^2^+2.5121P] 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 3107 _refine_ls_number_parameters 253 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.112 _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 -0.02971(4) -0.040308(14) 0.66690(3) 0.02569(9) Uani 1 1 d . . . Zn2 Zn 0.13986(4) 0.093365(14) 0.73637(3) 0.02640(9) Uani 1 1 d . . . O1 O 0.2141(2) -0.05822(9) 0.6968(2) 0.0307(5) Uani 1 1 d . . . O2 O 0.3371(2) 0.02726(9) 0.8003(2) 0.0308(5) Uani 1 1 d . . . O3 O -0.0663(2) 0.04269(8) 0.6321(2) 0.0292(5) Uani 1 1 d . . . N1 N 0.8925(3) -0.08474(10) 1.0528(2) 0.0270(6) Uani 1 1 d . . . N2 N 1.0349(3) -0.11508(11) 1.0573(3) 0.0335(6) Uani 1 1 d . . . N3 N 1.0639(3) -0.10446(11) 0.9392(3) 0.0343(6) Uani 1 1 d . . . N4 N 0.9412(3) -0.06592(10) 0.8534(2) 0.0288(6) Uani 1 1 d . . . N5 N 0.3347(3) 0.16234(10) 0.8007(2) 0.0262(6) Uani 1 1 d . . . N6 N -0.0086(3) 0.17481(10) 0.6744(2) 0.0270(6) Uani 1 1 d . . . N7 N -0.1803(3) -0.09229(11) 0.4986(3) 0.0341(7) Uani 1 1 d . . . N8 N -0.3002(4) -0.10747(14) 0.5024(3) 0.0476(8) Uani 1 1 d . . . N9 N -0.4323(5) -0.1291(2) 0.5018(5) 0.1089(15) Uani 1 1 d U . . C1 C 0.8374(3) -0.05458(12) 0.9254(3) 0.0223(6) Uani 1 1 d . . . C2 C 0.6789(3) -0.01688(12) 0.8680(3) 0.0258(7) Uani 1 1 d . . . H2A H 0.6825 0.0081 0.7886 0.031 Uiso 1 1 calc R . . H2B H 0.6746 0.0086 0.9464 0.031 Uiso 1 1 calc R . . C3 C 0.5172(3) -0.05611(13) 0.8105(3) 0.0314(8) Uani 1 1 d . . . H3A H 0.5186 -0.0779 0.7255 0.038 Uiso 1 1 calc R . . H3B H 0.5262 -0.0850 0.8866 0.038 Uiso 1 1 calc R . . C4 C 0.3437(3) -0.02581(13) 0.7657(3) 0.0240(7) Uani 1 1 d . . . C5 C -0.1804(4) 0.17740(14) 0.6177(3) 0.0342(8) Uani 1 1 d . . . H5A H -0.2427 0.1422 0.5921 0.041 Uiso 1 1 calc R . . C6 C -0.2706(4) 0.23036(14) 0.5951(3) 0.0382(8) Uani 1 1 d . . . H6A H -0.3909 0.2312 0.5528 0.046 Uiso 1 1 calc R . . C7 C -0.1752(4) 0.28218(14) 0.6380(4) 0.0429(9) Uani 1 1 d . . . H7A H -0.2313 0.3185 0.6270 0.051 Uiso 1 1 calc R . . C8 C 0.0012(4) 0.27979(13) 0.6962(3) 0.0369(8) Uani 1 1 d . . . H8A H 0.0661 0.3144 0.7247 0.044 Uiso 1 1 calc R . . C9 C 0.0831(4) 0.22494(13) 0.7126(3) 0.0291(7) Uani 1 1 d . . . C10 C 0.2746(3) 0.21857(12) 0.7731(3) 0.0257(7) Uani 1 1 d . . . C11 C 0.3845(4) 0.26700(13) 0.7988(3) 0.0355(8) Uani 1 1 d . . . H11A H 0.3405 0.3052 0.7765 0.043 Uiso 1 1 calc R . . C12 C 0.5619(4) 0.25709(14) 0.8585(4) 0.0403(9) Uani 1 1 d . . . H12A H 0.6388 0.2887 0.8782 0.048 Uiso 1 1 calc R . . C13 C 0.6224(4) 0.19996(14) 0.8881(3) 0.0367(8) Uani 1 1 d . . . H13A H 0.7407 0.1924 0.9288 0.044 Uiso 1 1 calc R . . C14 C 0.5058(4) 0.15421(13) 0.8568(3) 0.0328(8) Uani 1 1 d . . . H14A H 0.5480 0.1156 0.8755 0.039 Uiso 1 1 calc 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 0.02316(15) 0.02521(17) 0.02612(15) 0.00048(12) 0.00659(12) -0.00186(12) Zn2 0.02402(16) 0.01987(16) 0.03289(16) 0.00052(13) 0.00823(13) 0.00103(12) O1 0.0216(9) 0.0320(11) 0.0369(10) -0.0043(9) 0.0093(8) -0.0006(8) O2 0.0253(9) 0.0289(10) 0.0344(10) -0.0014(8) 0.0073(8) 0.0070(8) O3 0.0282(10) 0.0249(10) 0.0309(9) 0.0001(8) 0.0071(8) -0.0014(8) N1 0.0244(11) 0.0280(12) 0.0272(11) 0.0050(9) 0.0083(9) 0.0026(9) N2 0.0265(11) 0.0413(14) 0.0338(12) 0.0089(11) 0.0126(9) 0.0140(10) N3 0.0287(11) 0.0417(14) 0.0364(12) 0.0131(11) 0.0167(10) 0.0114(11) N4 0.0286(11) 0.0289(12) 0.0283(11) 0.0059(10) 0.0102(9) 0.0024(10) N5 0.0293(11) 0.0221(11) 0.0258(10) -0.0002(9) 0.0089(9) 0.0009(9) N6 0.0307(11) 0.0231(12) 0.0274(10) 0.0040(9) 0.0114(9) 0.0024(9) N7 0.0341(13) 0.0367(14) 0.0256(11) -0.0053(10) 0.0049(10) -0.0028(11) N8 0.0438(15) 0.0663(19) 0.0340(13) -0.0182(13) 0.0163(11) -0.0080(14) N9 0.082(2) 0.159(4) 0.100(2) -0.048(2) 0.0510(19) -0.047(2) C1 0.0211(12) 0.0199(13) 0.0251(12) 0.0010(10) 0.0080(10) -0.0023(10) C2 0.0255(13) 0.0239(14) 0.0285(12) 0.0050(11) 0.0110(10) 0.0027(11) C3 0.0226(13) 0.0265(15) 0.0406(15) -0.0047(12) 0.0071(12) 0.0022(11) C4 0.0211(12) 0.0293(14) 0.0209(11) 0.0013(11) 0.0073(10) 0.0067(11) C5 0.0300(14) 0.0332(16) 0.0395(15) 0.0040(13) 0.0135(12) 0.0036(12) C6 0.0305(15) 0.0446(18) 0.0388(15) 0.0087(14) 0.0126(12) 0.0131(13) C7 0.0423(17) 0.0312(16) 0.0508(18) 0.0070(14) 0.0131(14) 0.0171(13) C8 0.0374(16) 0.0225(15) 0.0462(16) 0.0022(13) 0.0110(13) 0.0041(12) C9 0.0368(14) 0.0279(15) 0.0238(12) 0.0039(11) 0.0128(11) 0.0062(12) C10 0.0315(13) 0.0216(13) 0.0248(12) 0.0028(11) 0.0118(10) 0.0050(11) C11 0.0393(16) 0.0202(14) 0.0462(16) 0.0009(12) 0.0157(13) -0.0019(12) C12 0.0373(16) 0.0293(16) 0.0547(18) -0.0037(14) 0.0180(14) -0.0091(13) C13 0.0214(14) 0.0388(17) 0.0472(16) -0.0033(14) 0.0103(12) -0.0018(12) C14 0.0323(14) 0.0289(16) 0.0358(14) 0.0001(12) 0.0116(12) 0.0026(12) _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 O3 1.905(2) . ? Zn1 O1 1.989(2) . ? Zn1 N4 2.016(3) 1_455 ? Zn1 N7 2.020(2) . ? Zn2 O3 1.9926(19) . ? Zn2 O2 2.132(2) . ? Zn2 N5 2.165(2) . ? Zn2 N6 2.169(2) . ? Zn2 N1 2.190(3) 3_657 ? Zn2 N7 2.449(3) 3_556 ? O1 C4 1.266(3) . ? O2 C4 1.251(3) . ? N1 C1 1.336(3) . ? N1 N2 1.360(3) . ? N1 Zn2 2.190(3) 3_657 ? N2 N3 1.292(4) . ? N3 N4 1.360(3) . ? N4 C1 1.338(4) . ? N4 Zn1 2.016(3) 1_655 ? N5 C14 1.335(4) . ? N5 C10 1.353(3) . ? N6 C5 1.329(4) . ? N6 C9 1.336(4) . ? N7 N8 1.075(4) . ? N7 Zn2 2.449(3) 3_556 ? N8 N9 1.206(5) . ? C1 C2 1.492(4) . ? C2 C3 1.531(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.510(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.384(4) . ? C5 H5A 0.9300 . ? C6 C7 1.386(5) . ? C6 H6A 0.9300 . ? C7 C8 1.364(4) . ? C7 H7A 0.9300 . ? C8 C9 1.393(4) . ? C8 H8A 0.9300 . ? C9 C10 1.487(4) . ? C10 C11 1.387(4) . ? C11 C12 1.389(4) . ? C11 H11A 0.9300 . ? C12 C13 1.373(4) . ? C12 H12A 0.9300 . ? C13 C14 1.371(4) . ? C13 H13A 0.9300 . ? C14 H14A 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 O3 Zn1 O1 108.11(8) . . ? O3 Zn1 N4 112.10(9) . 1_455 ? O1 Zn1 N4 106.43(9) . 1_455 ? O3 Zn1 N7 114.64(9) . . ? O1 Zn1 N7 106.60(10) . . ? N4 Zn1 N7 108.51(11) 1_455 . ? O3 Zn2 O2 99.79(8) . . ? O3 Zn2 N5 165.53(8) . . ? O2 Zn2 N5 90.27(9) . . ? O3 Zn2 N6 92.98(9) . . ? O2 Zn2 N6 165.88(8) . . ? N5 Zn2 N6 76.11(9) . . ? O3 Zn2 N1 92.02(9) . 3_657 ? O2 Zn2 N1 91.35(8) . 3_657 ? N5 Zn2 N1 98.16(9) . 3_657 ? N6 Zn2 N1 94.21(9) . 3_657 ? O3 Zn2 N7 85.32(9) . 3_556 ? O2 Zn2 N7 84.14(8) . 3_556 ? N5 Zn2 N7 85.39(9) . 3_556 ? N6 Zn2 N7 90.98(9) . 3_556 ? N1 Zn2 N7 174.29(9) 3_657 3_556 ? C4 O1 Zn1 125.57(18) . . ? C4 O2 Zn2 134.36(16) . . ? Zn1 O3 Zn2 115.06(9) . . ? C1 N1 N2 105.7(2) . . ? C1 N1 Zn2 143.1(2) . 3_657 ? N2 N1 Zn2 110.41(16) . 3_657 ? N3 N2 N1 110.0(2) . . ? N2 N3 N4 108.3(2) . . ? C1 N4 N3 106.6(2) . . ? C1 N4 Zn1 138.71(18) . 1_655 ? N3 N4 Zn1 114.59(19) . 1_655 ? C14 N5 C10 118.0(2) . . ? C14 N5 Zn2 126.20(19) . . ? C10 N5 Zn2 115.73(18) . . ? C5 N6 C9 119.5(2) . . ? C5 N6 Zn2 124.5(2) . . ? C9 N6 Zn2 115.60(18) . . ? N8 N7 Zn1 117.1(2) . . ? N8 N7 Zn2 119.8(2) . 3_556 ? Zn1 N7 Zn2 120.21(13) . 3_556 ? N7 N8 N9 174.3(4) . . ? N1 C1 N4 109.4(2) . . ? N1 C1 C2 125.4(3) . . ? N4 C1 C2 125.0(2) . . ? C1 C2 C3 110.0(2) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 117.5(2) . . ? C4 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? O2 C4 O1 125.4(2) . . ? O2 C4 C3 119.5(2) . . ? O1 C4 C3 115.2(2) . . ? N6 C5 C6 122.7(3) . . ? N6 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C7 117.6(3) . . ? C5 C6 H6A 121.2 . . ? C7 C6 H6A 121.2 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 119.3(3) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? N6 C9 C8 120.9(3) . . ? N6 C9 C10 116.4(2) . . ? C8 C9 C10 122.6(3) . . ? N5 C10 C11 122.1(3) . . ? N5 C10 C9 115.6(2) . . ? C11 C10 C9 122.3(2) . . ? C10 C11 C12 118.5(3) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 119.0(3) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? N5 C14 C13 123.2(3) . . ? N5 C14 H14A 118.4 . . ? C13 C14 H14A 118.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.702 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.090 #===================================================================== data_14_3 _database_code_depnum_ccdc_archive 'CCDC 815798' #TrackingRef '- polymer 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn2(C10N2H8)(N4CCH2CH2COO)2]n' ; _chemical_name_common '[Zn2(C10N2H8)(N4CCH2CH2COO)2]n' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Zn2(C10N2H8)(N4CCH2CH2COO)2]n' _chemical_formula_sum 'C18 H16 N10 O4 Zn2' _chemical_formula_weight 567.15 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' 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' H H 0.0000 0.0000 '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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.992(3) _cell_length_b 7.602(3) _cell_length_c 9.470(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.271(19) _cell_angle_gamma 90.00 _cell_volume 1041.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description Chip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 2.356 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.9062 _exptl_absorpt_correction_T_max 0.9967 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.9705 _diffrn_reflns_number 2008 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.1761 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1898 _reflns_number_gt 950 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0200P)^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_number_reflns 1898 _refine_ls_number_parameters 154 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.991 _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 0.21399(2) 0.48960(5) -0.10048(4) 0.02463(8) Uani 1 1 d . . . O1 O -0.08419(13) 0.5795(3) 0.1549(2) 0.0439(8) Uani 1 1 d . . . O2 O -0.14435(17) 0.7575(4) -0.0248(3) 0.0758(11) Uani 1 1 d . . . N1 N 0.23449(13) 0.6613(3) 0.0676(2) 0.0245(7) Uani 1 1 d . . . N2 N 0.31600(15) 0.7580(4) 0.0939(3) 0.0352(9) Uani 1 1 d . . . N3 N 0.31658(15) 0.8764(3) 0.1934(2) 0.0275(8) Uani 1 1 d . . . N4 N 0.23619(14) 0.8601(3) 0.2401(2) 0.0233(7) Uani 1 1 d . . . N5 N 0.32246(15) 0.3195(3) -0.0691(3) 0.0313(8) Uani 1 1 d . . . C1 C 0.19304(17) 0.7275(4) 0.1607(3) 0.0221(9) Uani 1 1 d . . . C2 C 0.09842(18) 0.6633(4) 0.1730(3) 0.0306(10) Uani 1 1 d . . . H46A H 0.0912 0.5397 0.1468 0.037 Uiso 1 1 calc R . . H46B H 0.0952 0.6750 0.2735 0.037 Uiso 1 1 calc R . . C3 C 0.02021(18) 0.7675(4) 0.0735(4) 0.0419(11) Uani 1 1 d . . . H41A H 0.0282 0.7666 -0.0249 0.050 Uiso 1 1 calc R . . H41B H 0.0244 0.8888 0.1066 0.050 Uiso 1 1 calc R . . C4 C -0.0761(2) 0.6975(5) 0.0685(3) 0.0410(11) Uani 1 1 d . . . C5 C 0.3123(2) 0.1666(5) -0.1396(4) 0.0506(12) Uani 1 1 d . . . H30A H 0.2570 0.1440 -0.2092 0.061 Uiso 1 1 calc R . . C6 C 0.3808(2) 0.0397(5) -0.1135(3) 0.0524(12) Uani 1 1 d . . . H11A H 0.3695 -0.0669 -0.1631 0.063 Uiso 1 1 calc R . . C7 C 0.46442(17) 0.0679(4) -0.0168(3) 0.0262(9) Uani 1 1 d . . . C8 C 0.4734(3) 0.2258(5) 0.0575(4) 0.0672(10) Uani 1 1 d U . . H8A H 0.5278 0.2521 0.1282 0.081 Uiso 1 1 calc R . . C9 C 0.4007(2) 0.3452(5) 0.0259(4) 0.0653(10) Uani 1 1 d U . . H22A H 0.4089 0.4511 0.0768 0.078 Uiso 1 1 calc 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 0.01342(12) 0.02491(15) 0.03361(15) 0.0024(2) 0.00277(11) 0.00332(19) O1 0.0256(10) 0.0630(16) 0.0425(12) -0.0027(12) 0.0080(9) -0.0233(11) O2 0.0474(15) 0.090(2) 0.0830(18) 0.0299(18) 0.0051(13) -0.0016(17) N1 0.0090(10) 0.0381(14) 0.0290(12) 0.0023(12) 0.0095(9) 0.0003(11) N2 0.0185(12) 0.0449(16) 0.0406(15) 0.0058(14) 0.0048(11) -0.0005(13) N3 0.0280(12) 0.0347(14) 0.0211(12) -0.0059(12) 0.0089(10) -0.0082(12) N4 0.0065(10) 0.0323(14) 0.0251(12) 0.0070(12) -0.0066(9) -0.0053(11) N5 0.0101(11) 0.0280(14) 0.0502(15) -0.0025(13) -0.0016(11) -0.0007(12) C1 0.0150(13) 0.0228(15) 0.0272(15) 0.0019(14) 0.0034(12) -0.0012(13) C2 0.0281(15) 0.0337(18) 0.0295(15) 0.0028(15) 0.0069(12) -0.0120(15) C3 0.0185(15) 0.0335(18) 0.071(2) 0.0035(18) 0.0070(15) -0.0045(16) C4 0.0318(16) 0.043(2) 0.0538(19) -0.0094(18) 0.0212(14) -0.0089(17) C5 0.0297(17) 0.049(2) 0.056(2) -0.0263(18) -0.0198(16) 0.0181(18) C6 0.0464(18) 0.048(2) 0.0446(18) -0.0283(17) -0.0210(16) 0.0262(17) C7 0.0182(13) 0.0218(15) 0.0380(16) -0.0036(14) 0.0062(13) -0.0030(13) C8 0.0564(15) 0.0588(16) 0.0738(16) -0.0120(13) -0.0050(12) 0.0066(13) C9 0.0600(15) 0.0528(15) 0.0749(16) -0.0121(13) 0.0031(12) 0.0063(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 O1 1.9494(19) 3_565 ? Zn1 N4 1.990(2) 4_575 ? Zn1 N1 2.019(2) . ? Zn1 N5 2.037(2) . ? Zn1 C4 2.592(3) 3_565 ? O1 C4 1.241(4) . ? O1 Zn1 1.9494(19) 3_565 ? O2 C4 1.249(4) . ? N1 C1 1.305(4) . ? N1 N2 1.391(3) . ? N2 N3 1.301(4) . ? N3 N4 1.394(3) . ? N4 C1 1.321(3) . ? N4 Zn1 1.990(2) 4_576 ? N5 C9 1.291(4) . ? N5 C5 1.329(4) . ? C1 C2 1.533(4) . ? C2 C3 1.519(4) . ? C2 H46A 0.9700 . ? C2 H46B 0.9700 . ? C3 C4 1.527(4) . ? C3 H41A 0.9700 . ? C3 H41B 0.9700 . ? C4 Zn1 2.592(3) 3_565 ? C5 C6 1.383(5) . ? C5 H30A 0.9300 . ? C6 C7 1.361(4) . ? C6 H11A 0.9300 . ? C7 C8 1.380(5) . ? C7 C7 1.458(5) 3_655 ? C8 C9 1.390(5) . ? C8 H8A 0.9300 . ? C9 H22A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N4 108.00(8) 3_565 4_575 ? O1 Zn1 N1 108.47(9) 3_565 . ? N4 Zn1 N1 101.88(10) 4_575 . ? O1 Zn1 N5 124.77(10) 3_565 . ? N4 Zn1 N5 100.87(10) 4_575 . ? N1 Zn1 N5 110.22(9) . . ? O1 Zn1 C4 27.32(9) 3_565 3_565 ? N4 Zn1 C4 134.55(9) 4_575 3_565 ? N1 Zn1 C4 102.89(10) . 3_565 ? N5 Zn1 C4 105.39(10) . 3_565 ? C4 O1 Zn1 106.56(17) . 3_565 ? C1 N1 N2 103.2(2) . . ? C1 N1 Zn1 141.33(18) . . ? N2 N1 Zn1 115.26(18) . . ? N3 N2 N1 109.4(2) . . ? N2 N3 N4 109.1(2) . . ? C1 N4 N3 102.8(2) . . ? C1 N4 Zn1 135.7(2) . 4_576 ? N3 N4 Zn1 121.41(16) . 4_576 ? C9 N5 C5 116.4(3) . . ? C9 N5 Zn1 123.3(2) . . ? C5 N5 Zn1 120.04(18) . . ? N1 C1 N4 115.5(2) . . ? N1 C1 C2 122.9(2) . . ? N4 C1 C2 121.6(3) . . ? C3 C2 C1 111.4(2) . . ? C3 C2 H46A 109.3 . . ? C1 C2 H46A 109.3 . . ? C3 C2 H46B 109.3 . . ? C1 C2 H46B 109.3 . . ? H46A C2 H46B 108.0 . . ? C2 C3 C4 114.0(3) . . ? C2 C3 H41A 108.8 . . ? C4 C3 H41A 108.8 . . ? C2 C3 H41B 108.8 . . ? C4 C3 H41B 108.8 . . ? H41A C3 H41B 107.7 . . ? O1 C4 O2 121.7(3) . . ? O1 C4 C3 119.2(2) . . ? O2 C4 C3 119.1(3) . . ? O1 C4 Zn1 46.12(13) . 3_565 ? O2 C4 Zn1 75.7(2) . 3_565 ? C3 C4 Zn1 164.6(2) . 3_565 ? N5 C5 C6 122.6(3) . . ? N5 C5 H30A 118.7 . . ? C6 C5 H30A 118.7 . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H11A 119.3 . . ? C5 C6 H11A 119.3 . . ? C6 C7 C8 115.4(3) . . ? C6 C7 C7 121.8(3) . 3_655 ? C8 C7 C7 122.5(3) . 3_655 ? C7 C8 C9 119.5(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? N5 C9 C8 124.7(4) . . ? N5 C9 H22A 117.7 . . ? C8 C9 H22A 117.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.166 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.161