#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308914.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_4308914 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 'C10 H8 Br Cu2 N4 O5' _chemical_formula_weight 471.19 _chemical_name_systematic ; Hydrothermal Syntheses and Structures of Two Mixed-valence Copper(I,II) 2-Pyrazinecarboxylate Coordination Polymers ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.156(3) _cell_length_b 7.7171(17) _cell_length_c 26.148(6) _cell_measurement_temperature 298(2) _cell_volume 2654.7(10) _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 0.959 _diffrn_measured_fraction_theta_max 0.959 _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 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 17271 _diffrn_reflns_theta_full 28.34 _diffrn_reflns_theta_max 28.34 _diffrn_reflns_theta_min 1.56 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.244 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.3681 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour block _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_description black _exptl_crystal_F_000 1832 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.418 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.194 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 3188 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0560 _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^)+(0.0831P)^2^+4.1204P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1499 _refine_ls_wR_factor_ref 0.1712 _reflns_number_gt 1935 _reflns_number_total 3188 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic050118msi20050125_030518_2.cif _[local]_cod_data_source_block a _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 4308914 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-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 Br1 Br 0.83385(6) 0.27342(10) 0.06347(3) 0.0358(2) Uani 1 1 d . . . C1 C 0.6093(6) 0.2127(9) -0.0260(2) 0.0316(16) Uani 1 1 d . . . H1A H 0.6116 0.1170 -0.0044 0.038 Uiso 1 1 calc R . . C2 C 0.5988(6) 0.1906(9) -0.0788(2) 0.0257(15) Uani 1 1 d . . . C3 C 0.5999(5) 0.4791(9) -0.0919(2) 0.0293(16) Uani 1 1 d . . . H3A H 0.5953 0.5740 -0.1137 0.035 Uiso 1 1 calc R . . C4 C 0.6091(6) 0.5047(9) -0.0399(2) 0.0308(16) Uani 1 1 d . . . H4A H 0.6107 0.6177 -0.0275 0.037 Uiso 1 1 calc R . . C5 C 0.5927(6) 0.0112(10) -0.1031(2) 0.0360(19) Uani 1 1 d . . . C6 C 0.6233(6) 0.4940(9) 0.2235(2) 0.0261(15) Uani 1 1 d . . . H6A H 0.6245 0.5901 0.2450 0.031 Uiso 1 1 calc R . . C7 C 0.6288(6) 0.5159(9) 0.1709(2) 0.0274(16) Uani 1 1 d . . . H7A H 0.6328 0.6277 0.1578 0.033 Uiso 1 1 calc R . . C8 C 0.6223(6) 0.2246(8) 0.1589(2) 0.0254(15) Uani 1 1 d . . . H8A H 0.6212 0.1292 0.1372 0.030 Uiso 1 1 calc R . . C9 C 0.6172(5) 0.1974(8) 0.2111(2) 0.0225(14) Uani 1 1 d . . . C10 C 0.6106(6) 0.0264(9) 0.2362(2) 0.0266(15) Uani 1 1 d . . . Cu1 Cu 0.66386(8) 0.41641(13) 0.06450(3) 0.0358(3) Uani 1 1 d . . . Cu2 Cu 0.61152(7) 0.25972(9) 0.31664(3) 0.0248(2) Uani 1 1 d . . . N1 N 0.6160(5) 0.3745(7) -0.00673(19) 0.0271(13) Uani 1 1 d . . . N2 N 0.5973(4) 0.3186(7) -0.11111(19) 0.0250(13) Uani 1 1 d . . . N3 N 0.6163(4) 0.3360(7) 0.24328(19) 0.0233(12) Uani 1 1 d . . . N4 N 0.6286(5) 0.3837(7) 0.13850(19) 0.0262(13) Uani 1 1 d . . . O1 O 0.5975(4) 0.0120(6) -0.15251(16) 0.0317(12) Uani 1 1 d . . . O2 O 0.5843(7) -0.1180(7) -0.0774(2) 0.072(2) Uani 1 1 d . . . O3 O 0.6126(5) -0.1069(6) 0.21037(18) 0.0469(15) Uani 1 1 d . . . O4 O 0.6036(4) 0.0304(6) 0.28531(16) 0.0302(11) Uani 1 1 d . . . O1W O 0.7809(4) 0.2598(6) 0.3210(2) 0.0406(13) 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 Br1 0.0482(5) 0.0397(5) 0.0195(4) 0.0014(3) 0.0014(3) 0.0109(3) C1 0.053(5) 0.033(4) 0.009(3) 0.004(3) 0.000(3) 0.002(4) C2 0.041(4) 0.026(4) 0.010(3) -0.002(3) 0.000(3) 0.000(3) C3 0.043(5) 0.026(4) 0.019(3) 0.003(3) -0.003(3) 0.001(3) C4 0.048(5) 0.030(4) 0.014(3) -0.003(3) 0.001(3) 0.002(4) C5 0.069(6) 0.023(4) 0.015(3) -0.001(3) 0.004(3) 0.003(4) C6 0.051(4) 0.020(3) 0.007(3) 0.000(2) -0.003(3) 0.002(3) C7 0.048(5) 0.021(3) 0.013(3) 0.008(3) 0.001(3) 0.003(3) C8 0.044(4) 0.018(3) 0.015(3) -0.002(2) -0.002(3) -0.004(3) C9 0.033(4) 0.020(3) 0.014(3) 0.004(2) -0.001(3) 0.003(3) C10 0.045(4) 0.023(4) 0.012(3) 0.002(3) -0.002(3) 0.001(3) Cu1 0.0536(6) 0.0459(6) 0.0079(4) -0.0001(4) 0.0002(4) 0.0055(4) Cu2 0.0443(5) 0.0230(5) 0.0071(4) 0.0013(3) 0.0006(3) -0.0007(4) N1 0.043(4) 0.026(3) 0.012(2) -0.001(2) -0.002(2) 0.003(3) N2 0.045(4) 0.022(3) 0.008(2) 0.002(2) 0.003(2) -0.001(3) N3 0.038(3) 0.021(3) 0.011(2) -0.001(2) 0.002(2) 0.003(2) N4 0.038(3) 0.029(3) 0.011(2) 0.001(2) 0.000(2) 0.003(3) O1 0.056(3) 0.027(3) 0.012(2) -0.0006(19) 0.000(2) -0.001(2) O2 0.173(8) 0.022(3) 0.021(3) 0.005(2) -0.002(4) 0.002(4) O3 0.102(5) 0.019(3) 0.019(3) 0.000(2) 0.001(3) -0.002(3) O4 0.052(3) 0.029(3) 0.009(2) 0.0002(19) -0.002(2) -0.003(2) O1W 0.045(3) 0.038(3) 0.039(3) 0.009(2) -0.001(2) 0.005(2) 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' Br Br -0.2901 2.4595 '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 Cu1 Br1 Cu1 116.88(4) . 8_755 ? N1 C1 C2 119.2(6) . . ? N2 C2 C1 123.5(6) . . ? N2 C2 C5 114.6(6) . . ? C1 C2 C5 121.9(6) . . ? N2 C3 C4 120.3(6) . . ? N1 C4 C3 122.7(6) . . ? O2 C5 O1 124.3(7) . . ? O2 C5 C2 121.5(6) . . ? O1 C5 C2 114.2(6) . . ? N3 C6 C7 120.1(6) . . ? N4 C7 C6 122.6(6) . . ? N4 C8 C9 122.3(6) . . ? N3 C9 C8 119.5(6) . . ? N3 C9 C10 115.2(5) . . ? C8 C9 C10 125.3(6) . . ? O3 C10 O4 124.7(6) . . ? O3 C10 C9 120.0(6) . . ? O4 C10 C9 115.3(6) . . ? N1 Cu1 N4 143.9(3) . . ? N1 Cu1 Br1 101.62(18) . . ? N4 Cu1 Br1 99.33(17) . . ? N1 Cu1 Br1 99.02(16) . 8_765 ? N4 Cu1 Br1 97.92(16) . 8_765 ? Br1 Cu1 Br1 115.63(4) . 8_765 ? O1 Cu2 O4 171.5(2) 7_566 . ? O1 Cu2 N2 82.7(2) 7_566 7_566 ? O4 Cu2 N2 96.8(2) . 7_566 ? O1 Cu2 N3 97.7(2) 7_566 . ? O4 Cu2 N3 82.32(19) . . ? N2 Cu2 N3 176.3(3) 7_566 . ? O1 Cu2 O1W 94.2(2) 7_566 . ? O4 Cu2 O1W 94.3(2) . . ? N2 Cu2 O1W 92.6(2) 7_566 . ? N3 Cu2 O1W 91.0(2) . . ? C4 N1 C1 116.8(5) . . ? C4 N1 Cu1 120.5(5) . . ? C1 N1 Cu1 121.3(4) . . ? C2 N2 C3 117.3(6) . . ? C2 N2 Cu2 112.6(4) . 7_565 ? C3 N2 Cu2 129.4(4) . 7_565 ? C6 N3 C9 118.7(5) . . ? C6 N3 Cu2 130.0(4) . . ? C9 N3 Cu2 111.2(4) . . ? C7 N4 C8 116.8(5) . . ? C7 N4 Cu1 121.2(4) . . ? C8 N4 Cu1 120.9(4) . . ? C5 O1 Cu2 115.0(4) . 7_565 ? C10 O4 Cu2 115.8(4) . . ? 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 Br1 Cu1 2.4939(13) . ? Br1 Cu1 2.7554(14) 8_755 ? C1 N1 1.349(9) . ? C1 C2 1.398(8) . ? C2 N2 1.300(8) . ? C2 C5 1.526(10) . ? C3 N2 1.337(9) . ? C3 C4 1.379(9) . ? C4 N1 1.331(8) . ? C5 O2 1.208(9) . ? C5 O1 1.293(8) . ? C6 N3 1.327(8) . ? C6 C7 1.389(8) . ? C7 N4 1.325(8) . ? C8 N4 1.342(8) . ? C8 C9 1.381(9) . ? C9 N3 1.361(8) . ? C9 C10 1.477(9) . ? C10 O3 1.231(8) . ? C10 O4 1.287(7) . ? Cu1 N1 1.993(5) . ? Cu1 N4 2.006(5) . ? Cu1 Br1 2.7554(14) 8_765 ? Cu2 O1 1.947(5) 7_566 ? Cu2 O4 1.953(5) . ? Cu2 N2 1.992(5) 7_566 ? Cu2 N3 2.008(5) . ? Cu2 O1W 2.231(6) . ? N2 Cu2 1.992(5) 7_565 ? O1 Cu2 1.947(5) 7_565 ?