#------------------------------------------------------------------------------ #$Date: 2011-01-03 12:48:23 +0000 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$URL: svn://www.crystallography.net/cod/cif/4/4308913.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308913 loop_ _publ_author_name 'Xian-Ming Zhang' 'Rui-Qin Fang' _publ_contact_author ; 'Zhang, Xian-Ming' School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; _publ_contact_author_email zhangxm@dns.sxtu.edu.cn _publ_contact_author_fax 86-357-2051402 _publ_contact_author_phone 86-357-2051402 _publ_section_title ; Hydrothermal Syntheses and Structures of Two Mixed-Valence Copper(I,II) 2-Pyrazinecarboxylate Coordination Polymers ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3955 _journal_page_last 3959 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C12 H14 Cu3 N6 O8' _chemical_formula_weight 560.91 _chemical_name_systematic ; ? ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.527(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.0895(12) _cell_length_b 9.5172(16) _cell_length_c 13.843(2) _cell_measurement_temperature 298(2) _cell_volume 918.3(3) _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2111 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.99 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.499 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_correction_T_min 0.5877 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour block _exptl_crystal_density_diffrn 2.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_description brown _exptl_crystal_F_000 558 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.889 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.238 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 955 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.197 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0739 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1690 _refine_ls_wR_factor_ref 0.2038 _reflns_number_gt 722 _reflns_number_total 955 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic050118msi20050125_030518_1.cif _[local]_cod_data_source_block a _[local]_cod_cif_authors_sg_H-M 'C 1 2/c 1' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4308913 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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 Cu1 Cu 1.0000 0.0000 0.0000 0.0342(6) Uani 1 4 d S . . Cu2 Cu 0.7833(2) 0.0000 0.46456(10) 0.0445(6) Uani 1 2 d S . . N1 N 0.9548(14) 0.0000 0.1381(7) 0.053(3) Uani 1 2 d S . . N2 N 0.8878(14) 0.0000 0.3271(6) 0.041(2) Uani 1 2 d S . . N3 N 0.7553(11) 0.1900(8) 0.4933(6) 0.0446(19) Uani 0.50 1 d PU . . C4 C 0.7553(11) 0.1900(8) 0.4933(6) 0.0446(19) Uani 0.50 1 d PU . . O1 O 1.0387(15) 0.1969(11) 0.0414(7) 0.035(2) Uani 0.50 1 d P . . O2 O 1.0115(17) 0.3437(11) 0.1651(8) 0.043(3) Uani 0.50 1 d P . . C1 C 1.0088(19) 0.2248(16) 0.1285(10) 0.029(3) Uani 0.50 1 d P . . C2 C 0.9412(16) 0.1173(10) 0.1852(6) 0.058(3) Uani 1 1 d . . . C3 C 0.9094(14) 0.1172(9) 0.2807(7) 0.051(2) Uani 1 1 d . . . H3A H 0.9032 0.2024 0.3129 0.061 Uiso 1 1 calc R . . O1W O 1.3292(16) -0.0621(11) 0.0550(8) 0.044(3) Uani 0.50 1 d P . . O2W O 0.889(2) 0.5000 0.3089(9) 0.125(5) Uani 1 2 d S . . 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 Cu1 0.0519(12) 0.0332(11) 0.0222(10) 0.000 0.0192(8) 0.000 Cu2 0.0621(11) 0.0413(10) 0.0337(9) 0.000 0.0184(7) 0.000 N1 0.038(5) 0.104(10) 0.018(5) 0.000 0.008(4) 0.000 N2 0.059(6) 0.048(6) 0.022(5) 0.000 0.021(5) 0.000 N3 0.048(4) 0.055(5) 0.033(4) -0.012(4) 0.013(3) 0.007(4) C4 0.048(4) 0.055(5) 0.033(4) -0.012(4) 0.013(3) 0.007(4) O1 0.046(6) 0.031(6) 0.033(5) 0.005(4) 0.021(5) -0.005(5) O2 0.075(8) 0.024(6) 0.036(6) 0.008(5) 0.024(6) 0.000(5) C1 0.033(7) 0.035(9) 0.019(7) 0.002(6) 0.008(6) 0.013(6) C2 0.093(7) 0.052(6) 0.029(4) 0.000(4) 0.015(5) -0.037(6) C3 0.080(7) 0.041(5) 0.034(4) 0.001(4) 0.015(4) -0.024(5) O1W 0.053(7) 0.043(6) 0.036(6) -0.008(5) 0.011(5) 0.002(5) O2W 0.142(12) 0.172(15) 0.071(8) 0.000 0.041(8) 0.000 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 O1 180.0(6) 5_755 . ? O1 Cu1 O1 34.8(6) 5_755 6 ? O1 Cu1 O1 145.2(6) . 6 ? O1 Cu1 O1 145.2(6) 5_755 2_755 ? O1 Cu1 O1 34.8(6) . 2_755 ? O1 Cu1 O1 180.0(9) 6 2_755 ? O1 Cu1 N1 76.1(3) 5_755 5_755 ? O1 Cu1 N1 103.9(3) . 5_755 ? O1 Cu1 N1 103.9(3) 6 5_755 ? O1 Cu1 N1 76.1(3) 2_755 5_755 ? O1 Cu1 N1 103.9(3) 5_755 . ? O1 Cu1 N1 76.1(3) . . ? O1 Cu1 N1 76.1(3) 6 . ? O1 Cu1 N1 103.9(3) 2_755 . ? N1 Cu1 N1 180.0(5) 5_755 . ? O1 Cu1 O1W 66.1(4) 5_755 2_755 ? O1 Cu1 O1W 113.9(4) . 2_755 ? O1 Cu1 O1W 86.2(4) 6 2_755 ? O1 Cu1 O1W 93.8(4) 2_755 2_755 ? N1 Cu1 O1W 90.7(4) 5_755 2_755 ? N1 Cu1 O1W 89.3(4) . 2_755 ? O1 Cu1 O1W 113.9(4) 5_755 6 ? O1 Cu1 O1W 66.1(4) . 6 ? O1 Cu1 O1W 93.8(4) 6 6 ? O1 Cu1 O1W 86.2(4) 2_755 6 ? N1 Cu1 O1W 89.3(4) 5_755 6 ? N1 Cu1 O1W 90.7(4) . 6 ? O1W Cu1 O1W 180.0(5) 2_755 6 ? O1 Cu1 O1W 86.2(4) 5_755 . ? O1 Cu1 O1W 93.8(4) . . ? O1 Cu1 O1W 66.1(4) 6 . ? O1 Cu1 O1W 113.9(4) 2_755 . ? N1 Cu1 O1W 89.3(4) 5_755 . ? N1 Cu1 O1W 90.7(4) . . ? O1W Cu1 O1W 151.4(5) 2_755 . ? O1W Cu1 O1W 28.6(5) 6 . ? O1 Cu1 O1W 93.8(4) 5_755 5_755 ? O1 Cu1 O1W 86.2(4) . 5_755 ? O1 Cu1 O1W 113.9(4) 6 5_755 ? O1 Cu1 O1W 66.1(4) 2_755 5_755 ? N1 Cu1 O1W 90.7(4) 5_755 5_755 ? N1 Cu1 O1W 89.3(4) . 5_755 ? O1W Cu1 O1W 28.6(5) 2_755 5_755 ? O1W Cu1 O1W 151.4(5) 6 5_755 ? O1W Cu1 O1W 180.0(5) . 5_755 ? C4 Cu2 N3 0.00(12) 6 6 ? C4 Cu2 N3 150.5(5) 6 . ? N3 Cu2 N3 150.5(5) 6 . ? C4 Cu2 N2 104.7(3) 6 . ? N3 Cu2 N2 104.7(3) 6 . ? N3 Cu2 N2 104.7(3) . . ? C4 Cu2 Cu2 94.1(2) 6 5_756 ? N3 Cu2 Cu2 94.1(2) 6 5_756 ? N3 Cu2 Cu2 94.1(2) . 5_756 ? N2 Cu2 Cu2 78.2(3) . 5_756 ? C2 N1 C2 117.6(10) 6 . ? C2 N1 Cu1 121.2(5) 6 . ? C2 N1 Cu1 121.2(5) . . ? C3 N2 C3 116.7(11) 6 . ? C3 N2 Cu2 121.4(5) 6 . ? C3 N2 Cu2 121.4(5) . . ? C4 N3 N3 0.0(10) 7_656 7_656 ? C4 N3 Cu2 175.7(10) 7_656 . ? N3 N3 Cu2 175.7(10) 7_656 . ? O1 O1 C1 141.6(14) 2_755 . ? O1 O1 Cu1 72.6(3) 2_755 . ? C1 O1 Cu1 115.5(9) . . ? O2 C1 O1 125.2(13) . . ? O2 C1 C2 114.4(11) . . ? O1 C1 C2 119.8(12) . . ? N1 C2 C3 121.2(8) . . ? N1 C2 C1 106.1(9) . . ? C3 C2 C1 131.1(9) . . ? N2 C3 C2 121.6(8) . . ? O1W O1W Cu1 75.7(3) 6 . ? 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 Cu1 O1 1.964(10) 5_755 ? Cu1 O1 1.964(10) . ? Cu1 O1 1.964(10) 6 ? Cu1 O1 1.964(10) 2_755 ? Cu1 N1 1.995(9) 5_755 ? Cu1 N1 1.995(9) . ? Cu1 O1W 2.393(11) 2_755 ? Cu1 O1W 2.393(11) 6 ? Cu1 O1W 2.393(11) . ? Cu1 O1W 2.393(11) 5_755 ? Cu2 C4 1.870(7) 6 ? Cu2 N3 1.870(7) 6 ? Cu2 N3 1.870(7) . ? Cu2 N2 2.164(9) . ? Cu2 Cu2 3.050(3) 5_756 ? N1 C2 1.305(10) 6 ? N1 C2 1.305(10) . ? N2 C3 1.310(9) 6 ? N2 C3 1.310(9) . ? N3 C4 1.162(15) 7_656 ? N3 N3 1.162(15) 7_656 ? O1 O1 1.18(2) 2_755 ? O1 C1 1.290(16) . ? O2 C1 1.238(17) . ? C1 C2 1.424(16) . ? C2 C3 1.382(13) . ? O1W O1W 1.18(2) 6 ?