# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Fakun Zheng' _publ_contact_author_email ZFK@FJIRSM.AC.CN _publ_section_title ; Hydrothermal Syntheses, Crystal Structures and Luminescent Properties of Zinc(II) Coordination Polymers Constructed by Bifunctional Tetrazolate-5-carboxylate Ligands ; loop_ _publ_author_name 'Fakun Zheng.' 'Feng Chen.' 'Guo-Cong Guo.' 'Jin-Shun Huang.' 'Yan Li.' ; Ming-Sheng Wang ; 'Mei-Feng Wu.' 'A-Qing Wu.' 'Wei-Wei Zhou.' data_2 _database_code_depnum_ccdc_archive 'CCDC 733077' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn(N4CCOO)(H2O)3]2.2H2O' ; _chemical_name_common '[Zn(N4CCOO)(H2O)3]2.2H2O' _chemical_melting_point 'not measured' _chemical_formula_moiety '[Zn(N4CCOO)(H2O)3]2.2H2O' _chemical_formula_sum 'C4 H16 N8 O12 Zn2' _chemical_formula_weight 499.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.153(4) _cell_length_b 7.752(4) _cell_length_c 8.775(4) _cell_angle_alpha 97.048(3) _cell_angle_beta 112.728(4) _cell_angle_gamma 108.627(4) _cell_volume 408.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1487 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 25.35 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measure' _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_absorpt_coefficient_mu 3.020 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7726 _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 'fine-focus sealed tube' _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 2845 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1487 _reflns_number_gt 1390 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.1309P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1487 _refine_ls_number_parameters 142 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.079 _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 0.74823(4) 0.30222(3) 0.76910(3) 0.02182(11) Uani 1 1 d . . . O1W O 0.4155(3) 0.1375(2) 0.6359(2) 0.0319(4) Uani 1 1 d D . . H1WA H 0.356(4) 0.0200(15) 0.586(3) 0.048 Uiso 1 1 d D . . H1WB H 0.332(4) 0.187(3) 0.578(3) 0.048 Uiso 1 1 d D . . O1 O 0.8140(3) 0.2301(2) 0.5535(2) 0.0265(4) Uani 1 1 d . . . O2 O 1.0811(3) 0.2731(2) 0.4714(2) 0.0294(4) Uani 1 1 d . . . O2W O 0.7949(3) 0.0647(2) 0.8333(2) 0.0318(4) Uani 1 1 d D . . H2WA H 0.902(3) 0.047(4) 0.828(4) 0.048 Uiso 1 1 d D . . H2WB H 0.803(5) 0.052(4) 0.929(2) 0.048 Uiso 1 1 d D . . O3W O 0.6774(3) 0.5285(3) 0.6926(3) 0.0406(5) Uani 1 1 d D . . H3WA H 0.717(5) 0.589(4) 0.631(4) 0.061 Uiso 1 1 d D . . H3WB H 0.595(5) 0.571(4) 0.717(4) 0.061 Uiso 1 1 d D . . O4W O 0.1546(3) -0.0011(3) 0.8515(2) 0.0340(4) Uani 1 1 d D . . H4WB H 0.108(4) -0.071(3) 0.752(2) 0.051 Uiso 1 1 d D . . H4WA H 0.272(3) 0.089(3) 0.873(4) 0.051 Uiso 1 1 d D . . N1 N 1.0934(3) 0.4746(3) 0.8624(2) 0.0212(4) Uani 1 1 d . . . N2 N 1.2638(3) 0.6123(3) 0.9975(2) 0.0215(4) Uani 1 1 d . . . N3 N 1.4319(3) 0.6749(3) 0.9610(3) 0.0245(4) Uani 1 1 d . . . N4 N 1.3722(3) 0.5778(3) 0.8012(3) 0.0237(4) Uani 1 1 d . . . C1 C 1.1640(4) 0.4559(3) 0.7440(3) 0.0199(5) Uani 1 1 d . . . C2 C 1.0104(4) 0.3095(3) 0.5750(3) 0.0214(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 0.01725(16) 0.02503(16) 0.02018(16) 0.00186(11) 0.00955(12) 0.00518(12) O1W 0.0198(9) 0.0258(9) 0.0364(11) -0.0008(8) 0.0056(8) 0.0050(7) O1 0.0213(8) 0.0295(9) 0.0233(9) -0.0003(7) 0.0118(7) 0.0045(7) O2 0.0268(9) 0.0343(9) 0.0250(9) 0.0001(7) 0.0153(8) 0.0081(8) O2W 0.0367(10) 0.0353(10) 0.0339(11) 0.0148(8) 0.0208(9) 0.0191(8) O3W 0.0481(12) 0.0474(11) 0.0605(14) 0.0330(10) 0.0432(11) 0.0306(10) O4W 0.0281(10) 0.0378(10) 0.0289(10) 0.0017(8) 0.0157(8) 0.0041(8) N1 0.0173(9) 0.0224(10) 0.0200(10) 0.0009(8) 0.0091(8) 0.0044(8) N2 0.0176(9) 0.0232(10) 0.0188(10) 0.0014(8) 0.0085(8) 0.0037(8) N3 0.0193(10) 0.0251(10) 0.0259(11) 0.0023(8) 0.0129(9) 0.0037(8) N4 0.0203(10) 0.0274(10) 0.0223(10) 0.0036(8) 0.0121(8) 0.0065(8) C1 0.0170(11) 0.0225(11) 0.0208(12) 0.0036(9) 0.0100(10) 0.0077(9) C2 0.0239(12) 0.0209(11) 0.0201(12) 0.0052(9) 0.0109(10) 0.0090(10) _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 O1W 2.050(2) . ? Zn1 O2W 2.0785(19) . ? Zn1 O3W 2.093(2) . ? Zn1 N2 2.117(2) 2_767 ? Zn1 N1 2.148(2) . ? Zn1 O1 2.1701(17) . ? O1W H1WA 0.844(10) . ? O1W H1WB 0.844(10) . ? O1 C2 1.266(3) . ? O2 C2 1.243(3) . ? O2W H2WA 0.841(10) . ? O2W H2WB 0.843(10) . ? O3W H3WA 0.834(10) . ? O3W H3WB 0.840(10) . ? O4W H4WB 0.843(10) . ? O4W H4WA 0.838(10) . ? N1 N2 1.331(3) . ? N1 C1 1.331(3) . ? N2 N3 1.321(3) . ? N2 Zn1 2.117(2) 2_767 ? N3 N4 1.337(3) . ? N4 C1 1.330(3) . ? C1 C2 1.492(3) . ? 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 O1W Zn1 O2W 88.28(8) . . ? O1W Zn1 O3W 87.62(8) . . ? O2W Zn1 O3W 175.86(8) . . ? O1W Zn1 N2 94.04(8) . 2_767 ? O2W Zn1 N2 90.57(7) . 2_767 ? O3W Zn1 N2 90.28(8) . 2_767 ? O1W Zn1 N1 169.41(7) . . ? O2W Zn1 N1 95.35(8) . . ? O3W Zn1 N1 88.59(8) . . ? N2 Zn1 N1 95.86(7) 2_767 . ? O1W Zn1 O1 94.27(7) . . ? O2W Zn1 O1 87.35(7) . . ? O3W Zn1 O1 92.39(7) . . ? N2 Zn1 O1 171.37(7) 2_767 . ? N1 Zn1 O1 76.01(7) . . ? Zn1 O1W H1WA 126.6(19) . . ? Zn1 O1W H1WB 117.8(19) . . ? H1WA O1W H1WB 107(2) . . ? C2 O1 Zn1 117.45(14) . . ? Zn1 O2W H2WA 117(2) . . ? Zn1 O2W H2WB 117(2) . . ? H2WA O2W H2WB 105(2) . . ? Zn1 O3W H3WA 128(2) . . ? Zn1 O3W H3WB 124(2) . . ? H3WA O3W H3WB 108(2) . . ? H4WB O4W H4WA 107(2) . . ? N2 N1 C1 105.39(17) . . ? N2 N1 Zn1 141.18(14) . . ? C1 N1 Zn1 113.00(15) . . ? N3 N2 N1 109.17(18) . . ? N3 N2 Zn1 128.38(15) . 2_767 ? N1 N2 Zn1 122.40(14) . 2_767 ? N2 N3 N4 109.09(18) . . ? C1 N4 N3 105.19(17) . . ? N4 C1 N1 111.15(19) . . ? N4 C1 C2 129.95(19) . . ? N1 C1 C2 118.90(19) . . ? O2 C2 O1 126.0(2) . . ? O2 C2 C1 119.8(2) . . ? O1 C2 C1 114.19(18) . . ? 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 O4W H4WB O2 0.843(10) 1.992(12) 2.809(3) 163(3) 2_656 O4W H4WA N3 0.838(10) 2.107(15) 2.879(3) 153(3) 2_767 O2W H2WA O4W 0.841(10) 1.895(12) 2.729(3) 171(3) 1_655 O2W H2WB O4W 0.843(10) 1.938(11) 2.775(3) 172(3) 2_657 O1W H1WB O2 0.844(10) 2.045(13) 2.867(3) 164(3) 1_455 O1W H1WA O1 0.844(10) 1.870(12) 2.705(3) 170(3) 2_656 O3W H3WA O2 0.834(10) 2.065(14) 2.861(2) 159(3) 2_766 O3W H3WB N4 0.840(10) 2.010(14) 2.806(3) 158(3) 1_455 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.344 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.060 # Attachment 'Complex_5.CIF' ## cif for 'Zn2(N4CCOO)2(2,2'-bpy)2(H2O)2.H2O' data_22 _database_code_depnum_ccdc_archive 'CCDC 733078' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Zn2(N4CCOO)2(2,2'-bpy)2(H2O)2.H2O' ; _chemical_name_common Zn2(N4CCOO)2(2,2'-bpy)2(H2O)2.H2O _chemical_melting_point 'not measured' _chemical_formula_moiety Zn2(N4CCOO)2(2,2'-bpy)2(H2O)2.H2O _chemical_formula_sum 'C24 H22 N12 O7 Zn2' _chemical_formula_weight 721.28 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.396(3) _cell_length_b 11.094(3) _cell_length_c 13.567(4) _cell_angle_alpha 83.399(9) _cell_angle_beta 81.828(7) _cell_angle_gamma 74.782(9) _cell_volume 1346.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3465 _cell_measurement_theta_min 3.0437 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.853 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4548 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 10119 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4881 _reflns_number_gt 3994 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4881 _refine_ls_number_parameters 426 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.146024(17) 0.075349(14) 0.190132(11) 0.01094(4) Uani 1 1 d . . . Zn2 Zn -0.110232(17) 0.379640(14) 0.356101(11) 0.01031(4) Uani 1 1 d . . . O1W O -0.02050(11) -0.02139(8) 0.22303(7) 0.0149(3) Uani 1 1 d D . . H1WA H -0.0125(16) -0.0716(7) 0.2747(4) 0.022 Uiso 1 1 d D . . H1WB H -0.0280(12) -0.0646(7) 0.1778(4) 0.022 Uiso 1 1 d D . . O1 O 0.12057(11) 0.07649(8) 0.03417(7) 0.0141(3) Uani 1 1 d . . . O2W O 0.06768(11) 0.46352(8) 0.34395(7) 0.0142(3) Uani 1 1 d D . . H2WA H 0.0777(12) 0.5071(7) 0.3884(4) 0.021 Uiso 1 1 d D . . H2WB H 0.0860(14) 0.5045(8) 0.2891(4) 0.021 Uiso 1 1 d D . . O2 O 0.02132(12) 0.19279(9) -0.09650(7) 0.0185(3) Uani 1 1 d . . . O3 O -0.10757(11) 0.37134(8) 0.51863(7) 0.0130(3) Uani 1 1 d . . . O3W O 0.14594(12) 0.57409(9) 0.16598(8) 0.0214(3) Uani 1 1 d . . . H3WB H 0.091(2) 0.6367(16) 0.1639(14) 0.049(6) Uiso 1 1 d . . . H3WA H 0.151(2) 0.5517(15) 0.1047(13) 0.040(5) Uiso 1 1 d . . . O4 O -0.04623(11) 0.23480(8) 0.64964(7) 0.0165(3) Uani 1 1 d . . . N1 N -0.00418(13) 0.25512(10) 0.15786(8) 0.0119(3) Uani 1 1 d . . . N2 N -0.08004(13) 0.36116(10) 0.19936(9) 0.0130(3) Uani 1 1 d . . . N3 N -0.14477(13) 0.44311(10) 0.12995(9) 0.0153(3) Uani 1 1 d . . . N4 N -0.11230(13) 0.39091(10) 0.04200(9) 0.0149(3) Uani 1 1 d . . . N5 N 0.02942(12) 0.19690(10) 0.38941(8) 0.0103(3) Uani 1 1 d . . . N6 N 0.12473(13) 0.09972(10) 0.34573(8) 0.0117(3) Uani 1 1 d . . . N7 N 0.19382(14) 0.02031(11) 0.41501(9) 0.0168(3) Uani 1 1 d . . . N8 N 0.14315(14) 0.06522(10) 0.50525(9) 0.0158(3) Uani 1 1 d . . . N9 N -0.31285(13) 0.31905(10) 0.37022(8) 0.0125(3) Uani 1 1 d . . . N10 N -0.27627(13) 0.55105(10) 0.35608(8) 0.0132(3) Uani 1 1 d . . . N11 N 0.33107(13) -0.08156(10) 0.16918(9) 0.0140(3) Uani 1 1 d . . . N12 N 0.33567(13) 0.15813(10) 0.15426(9) 0.0130(3) Uani 1 1 d . . . C1 C -0.02679(15) 0.27628(12) 0.06186(10) 0.0108(4) Uani 1 1 d . . . C2 C 0.04235(15) 0.17433(12) -0.00723(11) 0.0125(4) Uani 1 1 d . . . C3 C 0.04406(15) 0.17211(12) 0.48606(10) 0.0104(3) Uani 1 1 d . . . C4 C -0.04341(15) 0.26429(12) 0.55909(10) 0.0105(3) Uani 1 1 d . . . C5 C -0.32337(17) 0.20077(13) 0.37182(11) 0.0169(4) Uani 1 1 d . . . H5A H -0.2370 0.1363 0.3694 0.020 Uiso 1 1 calc R . . C6 C -0.45911(17) 0.17131(14) 0.37699(12) 0.0225(4) Uani 1 1 d . . . H6A H -0.4635 0.0884 0.3784 0.027 Uiso 1 1 calc R . . C7 C -0.58731(17) 0.26680(14) 0.38007(11) 0.0227(4) Uani 1 1 d . . . H7A H -0.6794 0.2492 0.3833 0.027 Uiso 1 1 calc R . . C8 C -0.57698(16) 0.38913(14) 0.37832(11) 0.0199(4) Uani 1 1 d . . . H8A H -0.6620 0.4550 0.3799 0.024 Uiso 1 1 calc R . . C9 C -0.43808(16) 0.41205(13) 0.37412(10) 0.0128(4) Uani 1 1 d . . . C10 C -0.41797(16) 0.54125(13) 0.37254(10) 0.0142(4) Uani 1 1 d . . . C11 C -0.53559(17) 0.64602(13) 0.38550(10) 0.0175(4) Uani 1 1 d . . . H11A H -0.6327 0.6378 0.3965 0.021 Uiso 1 1 calc R . . C12 C -0.50742(18) 0.76313(14) 0.38196(11) 0.0216(4) Uani 1 1 d . . . H12A H -0.5850 0.8341 0.3919 0.026 Uiso 1 1 calc R . . C13 C -0.36197(18) 0.77247(14) 0.36345(11) 0.0219(4) Uani 1 1 d . . . H13A H -0.3400 0.8500 0.3599 0.026 Uiso 1 1 calc R . . C14 C -0.25010(17) 0.66470(13) 0.35033(11) 0.0172(4) Uani 1 1 d . . . H14A H -0.1524 0.6713 0.3369 0.021 Uiso 1 1 calc R . . C15 C 0.32092(17) -0.19983(13) 0.17398(10) 0.0160(4) Uani 1 1 d . . . H15A H 0.2286 -0.2165 0.1937 0.019 Uiso 1 1 calc R . . C16 C 0.44135(18) -0.29875(14) 0.15094(12) 0.0224(4) Uani 1 1 d . . . H16A H 0.4299 -0.3799 0.1541 0.027 Uiso 1 1 calc R . . C17 C 0.57891(18) -0.27489(14) 0.12312(11) 0.0222(5) Uani 1 1 d . . . H17A H 0.6621 -0.3398 0.1079 0.027 Uiso 1 1 calc R . . C18 C 0.59091(17) -0.15159(13) 0.11817(11) 0.0195(4) Uani 1 1 d . . . H18A H 0.6826 -0.1332 0.1002 0.023 Uiso 1 1 calc R . . C19 C 0.46499(16) -0.05712(13) 0.14033(10) 0.0134(4) Uani 1 1 d . . . C20 C 0.46813(16) 0.07680(13) 0.13375(10) 0.0138(4) Uani 1 1 d . . . C21 C 0.59734(18) 0.11733(14) 0.10633(12) 0.0237(4) Uani 1 1 d . . . H21A H 0.6878 0.0600 0.0916 0.028 Uiso 1 1 calc R . . C22 C 0.58945(18) 0.24296(14) 0.10131(13) 0.0287(5) Uani 1 1 d . . . H22B H 0.6749 0.2717 0.0841 0.034 Uiso 1 1 calc R . . C23 C 0.45395(18) 0.32628(14) 0.12194(12) 0.0256(5) Uani 1 1 d . . . H23A H 0.4464 0.4119 0.1182 0.031 Uiso 1 1 calc R . . C24 C 0.32901(17) 0.28030(13) 0.14842(11) 0.0189(4) Uani 1 1 d . . . H24A H 0.2374 0.3365 0.1626 0.023 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 0.01173(8) 0.00943(7) 0.01067(8) -0.00132(6) 0.00002(7) -0.00139(6) Zn2 0.01013(7) 0.00934(7) 0.01053(8) -0.00100(6) -0.00052(6) -0.00109(6) O1W 0.0204(5) 0.0140(4) 0.0113(5) -0.0007(4) 0.0007(4) -0.0076(4) O1 0.0169(5) 0.0123(4) 0.0109(5) -0.0033(4) 0.0000(4) 0.0001(4) O2W 0.0171(5) 0.0151(4) 0.0123(5) -0.0012(4) -0.0020(4) -0.0071(4) O2 0.0290(5) 0.0169(5) 0.0088(5) -0.0012(4) -0.0050(4) -0.0029(4) O3 0.0146(5) 0.0126(4) 0.0097(5) -0.0023(4) -0.0008(4) 0.0006(4) O3W 0.0322(6) 0.0167(5) 0.0141(5) 0.0012(4) -0.0042(5) -0.0042(4) O4 0.0249(5) 0.0171(5) 0.0077(5) -0.0003(4) 0.0016(4) -0.0078(4) N1 0.0147(6) 0.0109(5) 0.0110(6) -0.0026(4) -0.0002(5) -0.0049(4) N2 0.0139(6) 0.0107(5) 0.0129(6) -0.0018(4) 0.0004(5) -0.0012(5) N3 0.0170(6) 0.0130(6) 0.0138(6) -0.0009(5) -0.0023(5) 0.0001(5) N4 0.0195(6) 0.0094(5) 0.0149(6) -0.0005(5) -0.0043(5) -0.0011(5) N5 0.0101(5) 0.0090(5) 0.0123(6) -0.0024(4) 0.0013(5) -0.0042(4) N6 0.0125(6) 0.0085(5) 0.0142(6) -0.0021(4) -0.0015(5) -0.0021(4) N7 0.0189(6) 0.0144(6) 0.0150(6) -0.0027(5) -0.0048(5) 0.0020(5) N8 0.0215(6) 0.0118(6) 0.0111(6) -0.0013(5) -0.0029(5) 0.0018(5) N9 0.0127(6) 0.0142(5) 0.0098(6) 0.0001(4) 0.0000(5) -0.0031(5) N10 0.0134(6) 0.0128(5) 0.0131(6) -0.0006(5) -0.0029(5) -0.0021(5) N11 0.0170(6) 0.0099(5) 0.0148(6) -0.0024(4) -0.0021(5) -0.0022(5) N12 0.0135(6) 0.0103(5) 0.0135(6) -0.0035(4) 0.0024(5) -0.0010(5) C1 0.0110(6) 0.0118(6) 0.0099(6) -0.0006(5) -0.0008(6) -0.0036(5) C2 0.0111(6) 0.0092(6) 0.0182(7) -0.0025(5) -0.0017(6) -0.0037(5) C3 0.0119(6) 0.0095(6) 0.0110(6) 0.0003(5) -0.0032(5) -0.0042(5) C4 0.0087(6) 0.0106(6) 0.0141(7) -0.0038(5) -0.0003(6) -0.0053(5) C5 0.0197(7) 0.0125(7) 0.0167(7) -0.0022(6) 0.0004(6) -0.0017(6) C6 0.0254(8) 0.0207(7) 0.0241(8) -0.0006(6) 0.0009(7) -0.0130(6) C7 0.0177(7) 0.0319(8) 0.0231(8) -0.0008(6) -0.0037(7) -0.0142(6) C8 0.0114(7) 0.0268(8) 0.0201(8) -0.0006(6) -0.0037(6) -0.0021(6) C9 0.0148(7) 0.0165(7) 0.0064(6) -0.0010(5) -0.0008(6) -0.0025(6) C10 0.0147(7) 0.0195(7) 0.0086(7) 0.0002(5) -0.0039(6) -0.0039(6) C11 0.0124(7) 0.0220(7) 0.0126(7) -0.0018(6) 0.0024(6) 0.0036(6) C12 0.0228(8) 0.0162(7) 0.0194(8) -0.0030(6) -0.0047(7) 0.0082(7) C13 0.0283(8) 0.0112(7) 0.0244(8) -0.0033(6) -0.0061(7) 0.0004(6) C14 0.0167(7) 0.0140(7) 0.0216(8) -0.0011(6) -0.0046(6) -0.0038(6) C15 0.0176(7) 0.0131(7) 0.0157(7) -0.0014(6) -0.0007(6) -0.0017(6) C16 0.0297(9) 0.0141(7) 0.0205(8) -0.0025(6) -0.0024(7) -0.0003(7) C17 0.0205(8) 0.0146(7) 0.0234(8) -0.0022(6) 0.0001(7) 0.0089(7) C18 0.0138(7) 0.0215(7) 0.0202(8) -0.0003(6) -0.0012(6) -0.0002(6) C19 0.0142(7) 0.0142(7) 0.0093(7) -0.0012(5) -0.0001(6) 0.0000(6) C20 0.0155(7) 0.0159(7) 0.0092(7) -0.0032(5) -0.0011(6) -0.0017(6) C21 0.0182(8) 0.0225(8) 0.0297(9) -0.0057(7) 0.0018(7) -0.0049(6) C22 0.0207(8) 0.0288(8) 0.0405(10) -0.0053(7) 0.0041(8) -0.0159(6) C23 0.0290(8) 0.0169(7) 0.0323(9) -0.0055(6) 0.0061(8) -0.0118(6) C24 0.0219(8) 0.0151(7) 0.0192(7) -0.0054(6) 0.0016(7) -0.0041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1W 2.0909(11) . ? Zn1 N11 2.1256(11) . ? Zn1 N6 2.1335(13) . ? Zn1 N1 2.1583(11) . ? Zn1 O1 2.1612(12) . ? Zn1 N12 2.1829(14) . ? Zn2 O2W 2.0954(11) . ? Zn2 N10 2.1196(11) . ? Zn2 N2 2.1314(13) . ? Zn2 N5 2.1442(11) . ? Zn2 N9 2.1567(14) . ? Zn2 O3 2.1998(12) . ? O1W H1WA 0.843(6) . ? O1W H1WB 0.842(7) . ? O1 C2 1.2618(15) . ? O2W H2WA 0.845(7) . ? O2W H2WB 0.846(6) . ? O2 C2 1.2399(18) . ? O3 C4 1.2820(15) . ? O3W H3WB 0.748(16) . ? O3W H3WA 0.885(18) . ? O4 C4 1.2328(17) . ? N1 C1 1.3338(18) . ? N1 N2 1.3442(15) . ? N2 N3 1.3262(16) . ? N3 N4 1.3471(17) . ? N4 C1 1.3348(16) . ? N5 C3 1.3274(18) . ? N5 N6 1.3434(15) . ? N6 N7 1.3281(16) . ? N7 N8 1.3504(17) . ? N8 C3 1.3263(16) . ? N9 C5 1.3391(19) . ? N9 C9 1.3451(17) . ? N10 C14 1.3383(19) . ? N10 C10 1.349(2) . ? N11 C15 1.3339(19) . ? N11 C19 1.351(2) . ? N12 C24 1.3339(18) . ? N12 C20 1.3454(17) . ? C1 C2 1.5049(19) . ? C3 C4 1.5044(18) . ? C5 C6 1.388(2) . ? C5 H5A 0.9300 . ? C6 C7 1.379(2) . ? C6 H6A 0.9300 . ? C7 C8 1.383(2) . ? C7 H7A 0.9300 . ? C8 C9 1.386(2) . ? C8 H8A 0.9300 . ? C9 C10 1.492(2) . ? C10 C11 1.3859(19) . ? C11 C12 1.387(2) . ? C11 H11A 0.9300 . ? C12 C13 1.383(2) . ? C12 H12A 0.9300 . ? C13 C14 1.379(2) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.382(2) . ? C15 H15A 0.9300 . ? C16 C17 1.379(2) . ? C16 H16A 0.9300 . ? C17 C18 1.395(2) . ? C17 H17A 0.9300 . ? C18 C19 1.3816(19) . ? C18 H18A 0.9300 . ? C19 C20 1.486(2) . ? C20 C21 1.391(2) . ? C21 C22 1.370(2) . ? C21 H21A 0.9300 . ? C22 C23 1.376(2) . ? C22 H22B 0.9300 . ? C23 C24 1.386(2) . ? C23 H23A 0.9300 . ? C24 H24A 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 O1W Zn1 N11 98.21(5) . . ? O1W Zn1 N6 87.66(4) . . ? N11 Zn1 N6 104.10(4) . . ? O1W Zn1 N1 94.90(5) . . ? N11 Zn1 N1 158.71(4) . . ? N6 Zn1 N1 93.09(4) . . ? O1W Zn1 O1 87.52(4) . . ? N11 Zn1 O1 87.65(4) . . ? N6 Zn1 O1 167.83(4) . . ? N1 Zn1 O1 76.20(4) . . ? O1W Zn1 N12 174.27(4) . . ? N11 Zn1 N12 76.06(5) . . ? N6 Zn1 N12 93.71(5) . . ? N1 Zn1 N12 90.59(5) . . ? O1 Zn1 N12 92.18(4) . . ? O2W Zn2 N10 94.97(5) . . ? O2W Zn2 N2 91.57(4) . . ? N10 Zn2 N2 97.63(4) . . ? O2W Zn2 N5 92.21(4) . . ? N10 Zn2 N5 166.47(4) . . ? N2 Zn2 N5 93.62(4) . . ? O2W Zn2 N9 172.10(4) . . ? N10 Zn2 N9 77.16(5) . . ? N2 Zn2 N9 90.18(5) . . ? N5 Zn2 N9 95.37(5) . . ? O2W Zn2 O3 86.03(4) . . ? N10 Zn2 O3 92.11(4) . . ? N2 Zn2 O3 170.14(4) . . ? N5 Zn2 O3 76.95(4) . . ? N9 Zn2 O3 93.51(4) . . ? Zn1 O1W H1WA 114.6(10) . . ? Zn1 O1W H1WB 115.2(7) . . ? H1WA O1W H1WB 104.8(8) . . ? C2 O1 Zn1 118.06(9) . . ? Zn2 O2W H2WA 122.0(7) . . ? Zn2 O2W H2WB 117.0(9) . . ? H2WA O2W H2WB 105.0(8) . . ? C4 O3 Zn2 115.11(8) . . ? H3WB O3W H3WA 102.0(17) . . ? C1 N1 N2 104.90(10) . . ? C1 N1 Zn1 112.55(8) . . ? N2 N1 Zn1 142.38(9) . . ? N3 N2 N1 109.44(11) . . ? N3 N2 Zn2 126.71(8) . . ? N1 N2 Zn2 123.40(8) . . ? N2 N3 N4 108.85(10) . . ? C1 N4 N3 105.09(11) . . ? C3 N5 N6 104.60(10) . . ? C3 N5 Zn2 112.65(8) . . ? N6 N5 Zn2 142.14(9) . . ? N7 N6 N5 109.37(11) . . ? N7 N6 Zn1 126.66(8) . . ? N5 N6 Zn1 123.84(8) . . ? N6 N7 N8 108.76(10) . . ? C3 N8 N7 104.65(11) . . ? C5 N9 C9 118.79(13) . . ? C5 N9 Zn2 126.27(9) . . ? C9 N9 Zn2 114.89(10) . . ? C14 N10 C10 118.94(11) . . ? C14 N10 Zn2 124.84(10) . . ? C10 N10 Zn2 115.91(9) . . ? C15 N11 C19 118.62(12) . . ? C15 N11 Zn1 124.22(10) . . ? C19 N11 Zn1 116.87(9) . . ? C24 N12 C20 118.92(13) . . ? C24 N12 Zn1 125.49(10) . . ? C20 N12 Zn1 115.56(10) . . ? N1 C1 N4 111.72(12) . . ? N1 C1 C2 118.98(11) . . ? N4 C1 C2 129.30(12) . . ? O2 C2 O1 126.46(12) . . ? O2 C2 C1 119.49(11) . . ? O1 C2 C1 114.03(12) . . ? N8 C3 N5 112.62(11) . . ? N8 C3 C4 127.62(12) . . ? N5 C3 C4 119.72(11) . . ? O4 C4 O3 125.52(12) . . ? O4 C4 C3 120.02(11) . . ? O3 C4 C3 114.44(12) . . ? N9 C5 C6 122.11(13) . . ? N9 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C7 C6 C5 119.04(15) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C6 C7 C8 119.05(15) . . ? C6 C7 H7A 120.5 . . ? C8 C7 H7A 120.5 . . ? C7 C8 C9 119.02(13) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? N9 C9 C8 121.98(14) . . ? N9 C9 C10 115.86(13) . . ? C8 C9 C10 122.16(12) . . ? N10 C10 C11 121.21(14) . . ? N10 C10 C9 115.66(11) . . ? C11 C10 C9 123.12(14) . . ? C10 C11 C12 119.52(15) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 118.84(13) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 118.75(15) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? N10 C14 C13 122.71(15) . . ? N10 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? N11 C15 C16 122.98(15) . . ? N11 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C17 C16 C15 118.75(15) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? C16 C17 C18 118.76(13) . . ? C16 C17 H17A 120.6 . . ? C18 C17 H17A 120.6 . . ? C19 C18 C17 119.24(15) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? N11 C19 C18 121.63(13) . . ? N11 C19 C20 116.02(11) . . ? C18 C19 C20 122.36(14) . . ? N12 C20 C21 121.53(13) . . ? N12 C20 C19 115.34(13) . . ? C21 C20 C19 123.11(12) . . ? C22 C21 C20 119.09(14) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C21 C22 C23 119.43(16) . . ? C21 C22 H22B 120.3 . . ? C23 C22 H22B 120.3 . . ? C22 C23 C24 118.82(14) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? N12 C24 C23 122.20(13) . . ? N12 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.559 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.088 # Attachment 'Polymer_11.CIF' ## cif for '[Zn(N4CCH2COO)(H2O)]n' data_86 _database_code_depnum_ccdc_archive 'CCDC 733079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn(N4CCH2COO)(H2O)]n' ; _chemical_name_common (Zn(N4CCH2COO)(H2O))n _chemical_melting_point 'not measured' _chemical_formula_moiety '[Zn(N4CCH2COO)(H2O)]n' _chemical_formula_sum 'C3 H4 N4 O3 Zn' _chemical_formula_weight 209.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 12.7076(15) _cell_length_b 12.7076(15) _cell_length_c 7.7157(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1246.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1138 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 25.33 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 3.899 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.6697 _exptl_absorpt_correction_T_max 0.9997 _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 'fine-focus sealed tube' _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 _diffrn_reflns_number 1313 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.33 _reflns_number_total 1138 _reflns_number_gt 954 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX was applied to restrain the bond distances of O1W-H1WA and O1W-H1WB, and the H1WA...H1WB separation. ; _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^)+(0.0624P)^2^+0.3303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0196(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1138 _refine_ls_number_parameters 107 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _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 0.50618(2) 0.71232(2) 0.12807(3) 0.01571(8) Uani 1 1 d . . . O1 O 0.68488(13) 0.58788(13) 0.2090(2) 0.0199(4) Uani 1 1 d . . . O1W O 0.42557(15) 0.59452(16) -0.0189(2) 0.0345(5) Uani 1 1 d D . . H1WA H 0.4151(17) 0.603(2) -0.1267(10) 0.052 Uiso 1 1 d D . . H1WB H 0.3650(7) 0.589(3) 0.025(2) 0.052 Uiso 1 1 d D . . O2 O 0.63052(13) 0.67769(14) -0.0183(2) 0.0237(4) Uani 1 1 d . . . C1 C 0.83885(18) 0.47952(18) -0.0079(3) 0.0163(5) Uani 1 1 d . . . C2 C 0.7858(2) 0.57926(19) -0.0578(3) 0.0216(6) Uani 1 1 d . . . H2A H 0.7599 0.5714 -0.1754 0.026 Uiso 1 1 calc R . . H2B H 0.8384 0.6346 -0.0593 0.026 Uiso 1 1 calc R . . C3 C 0.69487(18) 0.61598(17) 0.0546(3) 0.0162(5) Uani 1 1 d . . . N4 N 0.88550(17) 0.41612(16) -0.1201(2) 0.0205(5) Uani 1 1 d . . . N3 N 0.92564(16) 0.33759(16) -0.0223(3) 0.0211(5) Uani 1 1 d . . . N2 N 0.90564(17) 0.35179(16) 0.1418(2) 0.0219(5) Uani 1 1 d . . . N1 N 0.85033(16) 0.44239(15) 0.1543(2) 0.0175(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 0.01809(14) 0.01829(14) 0.01076(15) 0.00248(10) 0.00110(10) 0.00261(10) O1 0.0217(8) 0.0237(8) 0.0144(8) 0.0042(7) 0.0058(7) 0.0039(7) O1W 0.0458(11) 0.0434(11) 0.0143(8) -0.0003(8) -0.0020(8) -0.0210(9) O2 0.0233(8) 0.0279(9) 0.0199(8) 0.0020(7) 0.0012(7) 0.0099(7) C1 0.0171(11) 0.0201(11) 0.0117(10) 0.0024(9) 0.0013(9) 0.0026(9) C2 0.0253(12) 0.0243(12) 0.0151(10) 0.0046(10) 0.0057(10) 0.0100(10) C3 0.0159(11) 0.0131(10) 0.0196(11) -0.0005(9) -0.0001(9) -0.0007(9) N4 0.0239(10) 0.0247(10) 0.0130(9) 0.0010(8) 0.0000(8) 0.0085(9) N3 0.0233(10) 0.0241(10) 0.0158(9) -0.0009(9) 0.0023(9) 0.0060(9) N2 0.0304(11) 0.0221(10) 0.0132(9) 0.0009(8) 0.0023(9) 0.0088(9) N1 0.0233(10) 0.0166(9) 0.0126(9) -0.0015(8) 0.0022(8) 0.0045(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 1.9913(17) . ? Zn1 N1 2.027(2) 7_576 ? Zn1 N3 2.061(2) 6_565 ? Zn1 O1 2.0894(16) 7_576 ? Zn1 O1W 2.1391(19) . ? O1 C3 1.250(3) . ? O1 Zn1 2.0893(16) 8_756 ? O1W H1WA 0.850(8) . ? O1W H1WB 0.844(8) . ? O2 C3 1.265(3) . ? C1 N4 1.323(3) . ? C1 N1 1.345(3) . ? C1 C2 1.486(3) . ? C2 C3 1.518(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N4 N3 1.351(3) . ? N3 N2 1.304(3) . ? N3 Zn1 2.061(2) 6_655 ? N2 N1 1.352(3) . ? N1 Zn1 2.027(2) 8_756 ? 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 134.44(8) . 7_576 ? O2 Zn1 N3 109.89(8) . 6_565 ? N1 Zn1 N3 115.63(8) 7_576 6_565 ? O2 Zn1 O1 94.88(7) . 7_576 ? N1 Zn1 O1 86.89(7) 7_576 7_576 ? N3 Zn1 O1 90.12(7) 6_565 7_576 ? O2 Zn1 O1W 85.69(7) . . ? N1 Zn1 O1W 88.44(8) 7_576 . ? N3 Zn1 O1W 95.33(8) 6_565 . ? O1 Zn1 O1W 173.98(7) 7_576 . ? C3 O1 Zn1 130.68(15) . 8_756 ? Zn1 O1W H1WA 120(2) . . ? Zn1 O1W H1WB 106.5(18) . . ? H1WA O1W H1WB 104.9(16) . . ? C3 O2 Zn1 113.45(15) . . ? N4 C1 N1 110.3(2) . . ? N4 C1 C2 123.6(2) . . ? N1 C1 C2 126.1(2) . . ? C1 C2 C3 117.36(19) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? O1 C3 O2 122.3(2) . . ? O1 C3 C2 122.3(2) . . ? O2 C3 C2 115.4(2) . . ? C1 N4 N3 104.69(18) . . ? N2 N3 N4 111.50(19) . . ? N2 N3 Zn1 126.02(16) . 6_655 ? N4 N3 Zn1 122.48(15) . 6_655 ? N3 N2 N1 106.75(18) . . ? C1 N1 N2 106.78(18) . . ? C1 N1 Zn1 125.98(16) . 8_756 ? N2 N1 Zn1 127.12(15) . 8_756 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.541 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.107 # Attachment 'Polymer_2.CIF' ## cif for '[Zn3(N4CCH2COO)2CL2(H2O)2(2,2'-bpy)2]n' data_43 _database_code_depnum_ccdc_archive 'CCDC 733080' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn3(N4CCH2COO)2CL2(H2O)2(2,2'-bpy)2]n' ; _chemical_name_common "[Zn3(N4CCH2COO)2CL2(H2O)2(2,2'-bpy)2]n" _chemical_melting_point 'not measured' _chemical_formula_moiety "[Zn3(N4CCH2COO)2CL2(H2O)2(2,2'-bpy)2]n" _chemical_formula_sum 'C26 H24 Cl2 N12 O6 Zn3' _chemical_formula_weight 867.58 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' Cl Cl 0.1484 0.1585 '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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.118(3) _cell_length_b 44.164(7) _cell_length_c 6.6646(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6510.1(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3360 _cell_measurement_theta_min 3.2255 _cell_measurement_theta_max 27.4758 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 2.418 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8086 _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 'fine-focus sealed tube' _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 11904 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3596 _reflns_number_gt 2413 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^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 mixed _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 0.053(9) _refine_ls_number_reflns 3596 _refine_ls_number_parameters 229 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.009 _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 0.2500 0.2500 0.40850(5) 0.04304(10) Uani 1 2 d S . . Zn2 Zn 0.054103(9) 0.208252(5) 0.99003(4) 0.03313(5) Uani 1 1 d . . . Cl1 Cl 0.19362(3) 0.282104(16) 0.21860(13) 0.0756(2) Uani 1 1 d . . . O1W O 0.08340(5) 0.23447(3) 1.2356(2) 0.0442(4) Uani 1 1 d D . . H1WA H 0.11640(16) 0.24422(12) 1.2442(19) 0.066 Uiso 1 1 d D . . H1WB H 0.0856(5) 0.22155(10) 1.3301(7) 0.066 Uiso 1 1 d D . . O1 O 0.02767(6) 0.24639(3) 0.8081(2) 0.0372(4) Uani 1 1 d . . . O2 O 0.03456(6) 0.28726(3) 0.6183(2) 0.0380(4) Uani 1 1 d . . . N5 N 0.07298(8) 0.16571(4) 1.1307(3) 0.0457(5) Uani 1 1 d . . . N6 N 0.01119(8) 0.17624(3) 0.7943(3) 0.0408(5) Uani 1 1 d . . . N1 N 0.13462(7) 0.21135(4) 0.8289(3) 0.0393(5) Uani 1 1 d . . . N2 N 0.17113(8) 0.18728(4) 0.7770(3) 0.0544(6) Uani 1 1 d . . . N3 N 0.20868(8) 0.19635(4) 0.6400(3) 0.0551(6) Uani 1 1 d . . . N4 N 0.19834(6) 0.22606(4) 0.5972(3) 0.0383(5) Uani 1 1 d . . . C1 C 0.10235(13) 0.16301(6) 1.3004(4) 0.0861(10) Uani 1 1 d . . . H1A H 0.1180 0.1805 1.3587 0.103 Uiso 1 1 calc R . . C2 C 0.11168(19) 0.13551(8) 1.3993(7) 0.1244(11) Uani 1 1 d U . . H2A H 0.1302 0.1341 1.5242 0.149 Uiso 1 1 calc R . . C3 C 0.09009(18) 0.10958(9) 1.2908(7) 0.1318(12) Uani 1 1 d U . . H3A H 0.0988 0.0903 1.3393 0.158 Uiso 1 1 calc R . . C4 C 0.05750(13) 0.11232(6) 1.1207(5) 0.0806(9) Uani 1 1 d U . . H4A H 0.0411 0.0955 1.0571 0.097 Uiso 1 1 calc R . . C5 C 0.04943(9) 0.14163(4) 1.0438(3) 0.0428(6) Uani 1 1 d . . . C6 C 0.01494(10) 0.14753(5) 0.8577(3) 0.0456(7) Uani 1 1 d . . . C7 C -0.01244(15) 0.12460(7) 0.7450(6) 0.0942(9) Uani 1 1 d U . . H7A H -0.0075 0.1044 0.7798 0.113 Uiso 1 1 calc R . . C8 C -0.04527(18) 0.13224(9) 0.5891(7) 0.1348(12) Uani 1 1 d U . . H8A H -0.0685 0.1175 0.5260 0.162 Uiso 1 1 calc R . . C9 C -0.04658(17) 0.16216(7) 0.5140(6) 0.1078(10) Uani 1 1 d U . . H9A H -0.0657 0.1672 0.3943 0.129 Uiso 1 1 calc R . . C10 C -0.01792(12) 0.18295(6) 0.6288(4) 0.0688(8) Uani 1 1 d . . . H10A H -0.0189 0.2031 0.5881 0.083 Uiso 1 1 calc R . . C11 C 0.15328(7) 0.23451(4) 0.7184(3) 0.0319(5) Uani 1 1 d . . . C12 C 0.12642(8) 0.26511(4) 0.7221(3) 0.0355(5) Uani 1 1 d . . . H12A H 0.1417 0.2763 0.6077 0.043 Uiso 1 1 calc R . . H12B H 0.1403 0.2754 0.8422 0.043 Uiso 1 1 calc R . . C13 C 0.05730(7) 0.26639(4) 0.7180(3) 0.0309(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 0.02829(14) 0.0599(2) 0.04093(17) 0.000 0.000 -0.00108(16) Zn2 0.03289(9) 0.02967(9) 0.03683(10) 0.00026(11) 0.00047(10) 0.00037(10) Cl1 0.0686(4) 0.0797(4) 0.0785(4) -0.0014(4) -0.0283(3) -0.0035(3) O1W 0.0387(7) 0.0387(7) 0.0553(8) -0.0009(8) -0.0034(7) -0.0044(6) O1 0.0349(7) 0.0325(7) 0.0442(8) 0.0106(6) 0.0055(6) 0.0039(6) O2 0.0362(6) 0.0275(7) 0.0504(8) 0.0074(6) -0.0085(6) 0.0027(6) N5 0.0510(10) 0.0365(9) 0.0496(10) 0.0029(9) -0.0013(9) 0.0007(9) N6 0.0556(10) 0.0266(8) 0.0403(10) -0.0050(8) 0.0014(8) -0.0121(7) N1 0.0351(8) 0.0336(9) 0.0492(10) 0.0031(8) 0.0071(8) 0.0055(7) N2 0.0505(9) 0.0381(9) 0.0744(14) 0.0088(10) 0.0168(10) 0.0165(8) N3 0.0507(10) 0.0451(10) 0.0695(13) -0.0011(10) 0.0146(10) 0.0103(9) N4 0.0294(8) 0.0434(10) 0.0421(9) -0.0057(8) 0.0025(7) 0.0046(7) C1 0.133(2) 0.0431(13) 0.0822(17) 0.0099(13) -0.0703(14) 0.0052(14) C2 0.147(2) 0.1056(18) 0.120(2) 0.0137(17) -0.0484(17) -0.0105(17) C3 0.154(2) 0.1037(19) 0.137(2) 0.0054(18) -0.0354(18) -0.0105(17) C4 0.1022(17) 0.0524(13) 0.0871(17) 0.0131(13) -0.0261(14) -0.0138(12) C5 0.0567(12) 0.0294(10) 0.0422(13) 0.0032(9) -0.0016(10) 0.0064(10) C6 0.0557(12) 0.0403(12) 0.0408(12) 0.0020(10) -0.0017(10) -0.0117(10) C7 0.1208(18) 0.0700(15) 0.0917(17) 0.0004(15) -0.0239(16) -0.0198(13) C8 0.162(2) 0.111(2) 0.131(2) -0.0052(18) -0.0417(18) -0.0242(17) C9 0.143(2) 0.0819(16) 0.0981(18) 0.0018(16) -0.0441(15) -0.0281(14) C10 0.0951(17) 0.0556(13) 0.0556(14) 0.0236(12) -0.0361(12) -0.0317(12) C11 0.0225(7) 0.0331(10) 0.0401(10) -0.0018(9) 0.0027(8) -0.0006(8) C12 0.0345(9) 0.0300(9) 0.0420(11) 0.0017(10) -0.0009(9) -0.0002(8) C13 0.0292(8) 0.0289(9) 0.0345(10) -0.0033(9) 0.0035(8) -0.0035(7) _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 N4 2.0015(17) 14 ? Zn1 N4 2.0015(17) . ? Zn1 Cl1 2.2731(8) 14 ? Zn1 Cl1 2.2731(8) . ? Zn2 N1 2.0842(17) . ? Zn2 O1W 2.1069(15) . ? Zn2 N5 2.1411(18) . ? Zn2 N6 2.1452(16) . ? Zn2 O2 2.1484(14) 6 ? Zn2 O1 2.1561(13) . ? O1W H1WA 0.849(4) . ? O1W H1WB 0.851(4) . ? O1 C13 1.253(2) . ? O2 C13 1.243(2) . ? O2 Zn2 2.1484(13) 6_554 ? N5 C1 1.309(3) . ? N5 C5 1.318(3) . ? N6 C10 1.311(3) . ? N6 C6 1.339(3) . ? N1 C11 1.326(2) . ? N1 N2 1.379(2) . ? N2 N3 1.298(3) . ? N3 N4 1.362(3) . ? N4 C11 1.336(2) . ? C1 C2 1.397(5) . ? C1 H1A 0.9300 . ? C2 C3 1.436(6) . ? C2 H2A 0.9300 . ? C3 C4 1.349(6) . ? C3 H3A 0.9300 . ? C4 C5 1.404(3) . ? C4 H4A 0.9300 . ? C5 C6 1.479(3) . ? C6 C7 1.399(4) . ? C7 C8 1.311(6) . ? C7 H7A 0.9300 . ? C8 C9 1.413(5) . ? C8 H8A 0.9300 . ? C9 C10 1.353(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.476(3) . ? C12 C13 1.530(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 N4 Zn1 N4 102.12(10) 14 . ? N4 Zn1 Cl1 111.48(5) 14 14 ? N4 Zn1 Cl1 109.49(5) . 14 ? N4 Zn1 Cl1 109.49(5) 14 . ? N4 Zn1 Cl1 111.48(5) . . ? Cl1 Zn1 Cl1 112.33(4) 14 . ? N1 Zn2 O1W 95.82(6) . . ? N1 Zn2 N5 96.70(7) . . ? O1W Zn2 N5 94.71(6) . . ? N1 Zn2 N6 96.19(7) . . ? O1W Zn2 N6 166.10(6) . . ? N5 Zn2 N6 76.95(7) . . ? N1 Zn2 O2 168.22(6) . 6 ? O1W Zn2 O2 85.47(5) . 6 ? N5 Zn2 O2 94.86(6) . 6 ? N6 Zn2 O2 84.20(6) . 6 ? N1 Zn2 O1 83.72(6) . . ? O1W Zn2 O1 95.21(5) . . ? N5 Zn2 O1 169.97(6) . . ? N6 Zn2 O1 93.03(6) . . ? O2 Zn2 O1 84.50(5) 6 . ? Zn2 O1W H1WA 126.5(8) . . ? Zn2 O1W H1WB 102.9(4) . . ? H1WA O1W H1WB 104.0(10) . . ? C13 O1 Zn2 132.71(12) . . ? C13 O2 Zn2 130.60(11) . 6_554 ? C1 N5 C5 120.14(19) . . ? C1 N5 Zn2 123.70(15) . . ? C5 N5 Zn2 116.00(15) . . ? C10 N6 C6 120.67(19) . . ? C10 N6 Zn2 125.44(14) . . ? C6 N6 Zn2 113.88(14) . . ? C11 N1 N2 105.85(16) . . ? C11 N1 Zn2 127.05(12) . . ? N2 N1 Zn2 125.39(12) . . ? N3 N2 N1 108.26(16) . . ? N2 N3 N4 109.69(17) . . ? C11 N4 N3 105.54(16) . . ? C11 N4 Zn1 131.17(14) . . ? N3 N4 Zn1 122.99(13) . . ? N5 C1 C2 124.0(3) . . ? N5 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 114.0(4) . . ? C1 C2 H2A 123.0 . . ? C3 C2 H2A 123.0 . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 117.2(3) . . ? C3 C4 H4A 121.4 . . ? C5 C4 H4A 121.4 . . ? N5 C5 C4 122.2(2) . . ? N5 C5 C6 115.48(18) . . ? C4 C5 C6 122.3(2) . . ? N6 C6 C7 119.3(2) . . ? N6 C6 C5 117.60(18) . . ? C7 C6 C5 123.1(2) . . ? C8 C7 C6 118.6(3) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? C7 C8 C9 122.2(4) . . ? C7 C8 H8A 118.9 . . ? C9 C8 H8A 118.9 . . ? C10 C9 C8 115.1(4) . . ? C10 C9 H9A 122.4 . . ? C8 C9 H9A 122.4 . . ? N6 C10 C9 123.5(3) . . ? N6 C10 H10A 118.2 . . ? C9 C10 H10A 118.2 . . ? N1 C11 N4 110.63(16) . . ? N1 C11 C12 124.87(17) . . ? N4 C11 C12 124.46(18) . . ? C11 C12 C13 115.82(15) . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? C11 C12 H12B 108.3 . . ? C13 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O2 C13 O1 124.57(16) . . ? O2 C13 C12 116.20(16) . . ? O1 C13 C12 119.20(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.846 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.114 # Attachment 'Polymer_3.CIF' ## cif for '[Zn2(N4CCH2COO)2(4,4'-bpy)]n' data_14 _database_code_depnum_ccdc_archive 'CCDC 733081' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Zn2(N4CCH2COO)2(4,4'-bpy)]n' ; _chemical_name_common "[Zn2(N4CCH2COO)2(4,4'-bpy)]n" _chemical_melting_point 'not measured' _chemical_formula_moiety "[Zn2(N4CCH2COO)2(4,4'-bpy)]n" _chemical_formula_sum 'C16 H12 N10 O4 Zn2' _chemical_formula_weight 539.10 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 13.515(3) _cell_length_b 6.7465(13) _cell_length_c 10.667(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.33(3) _cell_angle_gamma 90.00 _cell_volume 972.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.0132 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 2.517 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5962 _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 'fine-focus sealed tube' _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 6394 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1759 _reflns_number_gt 1452 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.4789P] 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 1759 _refine_ls_number_parameters 145 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.191 _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 0.82705(2) 0.02630(4) 0.53945(2) 0.02489(7) Uani 1 1 d . . . O1 O 0.96601(13) 0.1991(3) 0.52730(15) 0.0326(5) Uani 1 1 d . . . O2 O 1.09345(12) 0.2011(3) 0.39897(17) 0.0359(5) Uani 1 1 d . . . N1 N 0.79692(15) 0.1435(3) 0.36694(18) 0.0277(6) Uani 1 1 d . . . N2 N 0.70911(15) 0.1077(4) 0.30419(19) 0.0327(6) Uani 1 1 d . . . N3 N 0.70799(15) 0.2107(3) 0.20063(18) 0.0327(6) Uani 1 1 d . . . N4 N 0.79408(14) 0.3144(3) 0.19440(17) 0.0265(5) Uani 1 1 d . . . N5 N 0.69955(15) -0.1625(3) 0.53018(19) 0.0296(6) Uani 1 1 d . . . C1 C 0.84744(17) 0.2700(4) 0.2978(2) 0.0239(6) Uani 1 1 d . . . C2 C 0.94719(17) 0.3544(4) 0.3272(2) 0.0292(7) Uani 1 1 d . . . H2A H 0.9392 0.4902 0.3552 0.035 Uiso 1 1 calc R . . H2B H 0.9848 0.3575 0.2509 0.035 Uiso 1 1 calc R . . C3 C 1.00604(17) 0.2418(4) 0.4263(2) 0.0258(6) Uani 1 1 d . . . C4 C 0.6187(3) -0.1384(6) 0.5890(4) 0.0924(12) Uani 1 1 d U . . H4A H 0.6141 -0.0299 0.6424 0.111 Uiso 1 1 calc R . . C5 C 0.5377(3) -0.2638(7) 0.5779(5) 0.1008(13) Uani 1 1 d U . . H5A H 0.4802 -0.2342 0.6203 0.121 Uiso 1 1 calc R . . C6 C 0.54150(19) -0.4293(4) 0.5059(2) 0.0328(7) Uani 1 1 d . . . C7 C 0.6267(2) -0.4559(5) 0.4468(3) 0.0587(10) Uani 1 1 d . . . H7A H 0.6348 -0.5655 0.3953 0.070 Uiso 1 1 calc R . . C8 C 0.7031(2) -0.3203(5) 0.4624(4) 0.0731(11) Uani 1 1 d . . . H8A H 0.7614 -0.3452 0.4206 0.088 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 0.02373(13) 0.03079(16) 0.02017(12) 0.00064(12) 0.00071(10) -0.00101(13) O1 0.0355(9) 0.0416(11) 0.0207(8) 0.0028(8) -0.0004(7) -0.0051(9) O2 0.0229(8) 0.0374(10) 0.0476(10) 0.0134(8) 0.0040(8) -0.0003(8) N1 0.0260(10) 0.0326(12) 0.0244(10) 0.0026(9) -0.0015(8) -0.0036(9) N2 0.0291(11) 0.0408(13) 0.0278(10) 0.0056(9) -0.0055(9) -0.0078(10) N3 0.0279(10) 0.0436(13) 0.0265(10) 0.0053(10) -0.0030(9) -0.0032(10) N4 0.0230(10) 0.0332(12) 0.0234(9) 0.0024(9) -0.0001(8) -0.0019(9) N5 0.0255(10) 0.0316(12) 0.0318(10) -0.0002(9) 0.0026(9) -0.0046(9) C1 0.0238(11) 0.0255(13) 0.0225(11) 0.0002(10) 0.0042(9) 0.0027(11) C2 0.0259(12) 0.0357(15) 0.0260(12) 0.0047(11) -0.0020(10) -0.0026(11) C3 0.0258(12) 0.0238(13) 0.0277(12) -0.0021(10) -0.0002(10) -0.0043(11) C4 0.072(2) 0.082(2) 0.126(2) -0.0627(18) 0.0457(18) -0.0380(18) C5 0.075(2) 0.096(2) 0.134(2) -0.057(2) 0.0502(19) -0.0324(19) C6 0.0312(13) 0.0292(14) 0.0384(14) -0.0038(11) 0.0060(11) -0.0080(12) C7 0.0375(15) 0.0498(18) 0.090(2) -0.0383(16) 0.0231(15) -0.0170(14) C8 0.0380(16) 0.070(2) 0.113(2) -0.0520(18) 0.0377(16) -0.0198(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 O2 1.9766(18) 3_756 ? Zn1 N4 2.030(2) 4_566 ? Zn1 N1 2.035(2) . ? Zn1 N5 2.143(2) . ? Zn1 O1 2.2167(18) . ? O1 C3 1.251(3) . ? O2 C3 1.254(3) . ? O2 Zn1 1.9766(18) 3_756 ? N1 C1 1.327(3) . ? N1 N2 1.371(3) . ? N2 N3 1.305(3) . ? N3 N4 1.361(3) . ? N4 C1 1.337(3) . ? N4 Zn1 2.030(2) 4_565 ? N5 C4 1.284(4) . ? N5 C8 1.289(4) . ? C1 C2 1.490(3) . ? C2 C3 1.512(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.386(6) . ? C4 H4A 0.9300 . ? C5 C6 1.357(5) . ? C5 H5A 0.9300 . ? C6 C7 1.337(4) . ? C6 C6 1.476(5) 3_646 ? C7 C8 1.386(5) . ? C7 H7A 0.9300 . ? C8 H8A 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 O2 Zn1 N4 105.56(8) 3_756 4_566 ? O2 Zn1 N1 134.26(8) 3_756 . ? N4 Zn1 N1 119.17(8) 4_566 . ? O2 Zn1 N5 89.10(8) 3_756 . ? N4 Zn1 N5 99.26(8) 4_566 . ? N1 Zn1 N5 92.61(8) . . ? O2 Zn1 O1 88.44(7) 3_756 . ? N4 Zn1 O1 88.36(8) 4_566 . ? N1 Zn1 O1 83.96(8) . . ? N5 Zn1 O1 172.37(7) . . ? C3 O1 Zn1 123.75(15) . . ? C3 O2 Zn1 126.93(17) . 3_756 ? C1 N1 N2 107.02(19) . . ? C1 N1 Zn1 131.12(16) . . ? N2 N1 Zn1 121.73(16) . . ? N3 N2 N1 108.2(2) . . ? N2 N3 N4 108.79(18) . . ? C1 N4 N3 106.86(19) . . ? C1 N4 Zn1 131.73(16) . 4_565 ? N3 N4 Zn1 121.07(14) . 4_565 ? C4 N5 C8 115.0(3) . . ? C4 N5 Zn1 126.5(2) . . ? C8 N5 Zn1 118.48(19) . . ? N1 C1 N4 109.1(2) . . ? N1 C1 C2 127.1(2) . . ? N4 C1 C2 123.8(2) . . ? C1 C2 C3 114.5(2) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? O1 C3 O2 125.3(2) . . ? O1 C3 C2 119.1(2) . . ? O2 C3 C2 115.5(2) . . ? N5 C4 C5 124.1(4) . . ? N5 C4 H4A 118.0 . . ? C5 C4 H4A 118.0 . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C7 C6 C5 114.9(3) . . ? C7 C6 C6 122.3(3) . 3_646 ? C5 C6 C6 122.8(3) . 3_646 ? C6 C7 C8 120.2(3) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? N5 C8 C7 125.1(3) . . ? N5 C8 H8A 117.4 . . ? C7 C8 H8A 117.4 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.216 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.097