#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/35/2203580.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2203580 loop_ _publ_author_name 'Guang-Qi Xiang' 'Nan-Wen Zhu' 'Mao-Lin Hu' 'Hong-Ping Xiao' 'Xiao-Xia Chen' _publ_section_title ; Polymeric bis(hydrogen pyrazine-2,3-dicarboxylato)copper(II) N,N'-dimethylformamide disolvate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m647 _journal_page_last m649 _journal_paper_doi 10.1107/S1600536804009249 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cu (C6 H3 N2 O4)2], 2C3 H7 N O' _chemical_formula_moiety 'C12 H6 Cu N4 O8, 2(C3 H7 N O)' _chemical_formula_sum 'C18 H20 Cu N6 O10' _chemical_formula_weight 543.94 _chemical_name_systematic ; bis(hydrogen pyrazine-2,3-dicarboxylate)copper(II) N,N'-dimethylformamide disolvate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 76.147(7) _cell_angle_beta 88.002(7) _cell_angle_gamma 70.902(7) _cell_formula_units_Z 1 _cell_length_a 6.289(2) _cell_length_b 7.679(3) _cell_length_c 12.686(5) _cell_measurement_reflns_used 1209 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.33 _cell_measurement_theta_min 2.89 _cell_volume 561.5(4) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics 'XP in SHELXTL (Bruker, 2002)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker SMART APEX area-detector' _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 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 4122 _diffrn_reflns_theta_full 25.20 _diffrn_reflns_theta_max 25.20 _diffrn_reflns_theta_min 1.66 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 279 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.287 _refine_diff_density_min -0.513 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2005 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.227 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0958 _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^)+(0.1029P)^2^+3.7409P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2619 _refine_ls_wR_factor_ref 0.2639 _reflns_number_gt 1921 _reflns_number_total 2005 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cv6298.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_Hall -P1 _cod_database_code 2203580 _cod_database_fobs_code 2203580 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu1 0.0000 1.0000 1.0000 0.0290(5) Uani d S 1 Cu O1 0.0967(11) 1.2188(8) 0.9691(6) 0.0465(18) Uani d . 1 O O2 0.3452(11) 1.3350(9) 0.8725(6) 0.0490(17) Uani d . 1 O O3 0.5703(13) 1.2231(11) 0.6681(5) 0.0534(18) Uani d . 1 O H3 0.6400 1.2951 0.6411 0.080 Uiso calc R 1 H O4 0.8282(12) 1.1286(10) 0.8050(6) 0.0558(19) Uani d . 1 O O5 0.7090(13) 0.4977(11) 0.5917(6) 0.061(2) Uani d . 1 O N1 0.2692(11) 0.8911(9) 0.9220(5) 0.0287(14) Uani d . 1 N N2 0.6376(14) 0.8056(11) 0.7955(7) 0.047(2) Uani d . 1 N N3 0.9427(12) 0.6665(11) 0.5937(6) 0.0415(18) Uani d . 1 N C1 0.2624(14) 1.2102(11) 0.9069(7) 0.0343(19) Uani d . 1 C C2 0.3676(13) 1.0197(10) 0.8793(6) 0.0265(16) Uani d . 1 C C3 0.5489(14) 0.9786(12) 0.8145(7) 0.0342(18) Uani d . 1 C C4 0.6645(15) 1.1206(12) 0.7632(7) 0.038(2) Uani d . 1 C C5 0.3548(15) 0.7167(11) 0.9025(7) 0.0365(19) Uani d . 1 C H5 0.2886 0.6243 0.9305 0.044 Uiso calc R 1 H C6 0.5396(16) 0.6772(13) 0.8411(8) 0.046(2) Uani d . 1 C H6 0.6001 0.5551 0.8305 0.055 Uiso calc R 1 H C7 0.8138(19) 0.8239(15) 0.5074(10) 0.063(3) Uani d . 1 C H7A 0.7033 0.7880 0.4755 0.094 Uiso calc R 1 H H7B 0.9132 0.8565 0.4529 0.094 Uiso calc R 1 H H7C 0.7396 0.9315 0.5368 0.094 Uiso calc R 1 H C8 1.130(2) 0.6860(18) 0.6458(11) 0.070(3) Uani d . 1 C H8A 1.1839 0.5825 0.7087 0.105 Uiso calc R 1 H H8B 1.0831 0.8039 0.6675 0.105 Uiso calc R 1 H H8C 1.2489 0.6845 0.5960 0.105 Uiso calc R 1 H C9 0.8722(17) 0.5201(14) 0.6298(8) 0.048(2) Uani d . 1 C H9 0.9525 0.4263 0.6889 0.058 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.0306(8) 0.0205(7) 0.0411(9) -0.0138(6) 0.0114(6) -0.0112(6) O1 0.061(4) 0.034(3) 0.069(4) -0.035(3) 0.034(4) -0.034(3) O2 0.057(4) 0.032(3) 0.067(5) -0.025(3) 0.018(3) -0.015(3) O3 0.069(5) 0.062(5) 0.040(4) -0.045(4) -0.003(3) 0.000(3) O4 0.052(4) 0.057(4) 0.063(5) -0.034(4) -0.011(3) 0.004(4) O5 0.067(5) 0.062(5) 0.062(5) -0.038(4) 0.008(4) -0.006(4) N1 0.032(3) 0.023(3) 0.035(4) -0.012(3) 0.004(3) -0.008(3) N2 0.051(5) 0.039(4) 0.060(5) -0.021(4) 0.018(4) -0.022(4) N3 0.038(4) 0.039(4) 0.047(5) -0.011(3) 0.001(3) -0.010(3) C1 0.034(4) 0.026(4) 0.050(5) -0.013(3) 0.000(4) -0.015(4) C2 0.030(4) 0.020(4) 0.033(4) -0.010(3) -0.002(3) -0.008(3) C3 0.034(4) 0.027(4) 0.044(5) -0.013(3) -0.002(4) -0.009(4) C4 0.041(5) 0.031(5) 0.046(5) -0.016(4) 0.009(4) -0.013(4) C5 0.046(5) 0.020(4) 0.046(5) -0.013(4) 0.003(4) -0.010(4) C6 0.054(6) 0.029(5) 0.061(6) -0.015(4) 0.014(5) -0.024(4) C7 0.059(7) 0.044(6) 0.080(8) -0.020(5) -0.011(6) -0.002(6) C8 0.062(7) 0.068(8) 0.082(9) -0.032(6) -0.006(6) -0.006(7) C9 0.051(6) 0.045(6) 0.051(6) -0.021(5) 0.015(5) -0.008(5) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O1 . 2_577 180.000(2) no O1 Cu1 N1 . . 83.7(3) yes O1 Cu1 N1 2_577 . 96.3(3) yes O1 Cu1 N1 . 2_577 96.3(3) no O1 Cu1 N1 2_577 2_577 83.7(3) no N1 Cu1 N1 . 2_577 180.000(2) no O4 Cu1 O1 1_455 . 84.8(3) yes O4 Cu1 N1 1_455 . 81.1(3) yes C1 O1 Cu1 . . 115.3(5) ? C4 O3 H3 . . 109.5 ? C2 N1 C5 . . 118.3(7) ? C2 N1 Cu1 . . 111.4(5) ? C5 N1 Cu1 . . 130.2(6) ? C6 N2 C3 . . 116.7(8) ? C9 N3 C8 . . 121.8(9) ? C9 N3 C7 . . 119.7(9) ? C8 N3 C7 . . 118.1(9) ? O2 C1 O1 . . 126.8(8) ? O2 C1 C2 . . 118.7(7) ? O1 C1 C2 . . 114.4(7) ? N1 C2 C3 . . 121.3(7) ? N1 C2 C1 . . 114.6(7) ? C3 C2 C1 . . 124.2(7) ? N2 C3 C2 . . 121.2(7) ? N2 C3 C4 . . 115.7(7) ? C2 C3 C4 . . 123.1(7) ? O4 C4 O3 . . 125.8(8) ? O4 C4 C3 . . 122.4(8) ? O3 C4 C3 . . 111.7(7) ? N1 C5 C6 . . 119.4(8) ? N1 C5 H5 . . 120.3 ? C6 C5 H5 . . 120.3 ? N2 C6 C5 . . 123.2(8) ? N2 C6 H6 . . 118.4 ? C5 C6 H6 . . 118.4 ? N3 C7 H7A . . 109.5 ? N3 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? N3 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? N3 C8 H8A . . 109.5 ? N3 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? N3 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O5 C9 N3 . . 125.2(10) ? O5 C9 H9 . . 117.4 ? N3 C9 H9 . . 117.4 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 . 1.919(5) yes Cu1 O1 2_577 1.919(5) ? Cu1 N1 . 1.974(6) yes Cu1 N1 2_577 1.974(6) ? Cu1 O4 1_455 2.565(5) yes Cu1 O4 2_677 2.565(5) ? O1 C1 . 1.279(10) ? O2 C1 . 1.221(10) ? O3 C4 . 1.311(11) ? O3 H3 . 0.8200 ? O4 C4 . 1.200(11) ? O5 C9 . 1.228(12) ? N1 C2 . 1.332(10) ? N1 C5 . 1.351(10) ? N2 C6 . 1.337(12) ? N2 C3 . 1.339(11) ? N3 C9 . 1.317(12) ? N3 C8 . 1.438(13) ? N3 C7 . 1.451(13) ? C1 C2 . 1.515(10) ? C2 C3 . 1.377(11) ? C3 C4 . 1.512(12) ? C5 C6 . 1.367(12) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? C9 H9 . 0.9300 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3 O5 1_565 0.82 1.72 2.512(9) 162 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139066640