#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/84/2008492.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_2008492 loop_ _publ_author_name 'Huai-Ming Hu' 'De-Liang Long' 'Hui-Yi Zeng' 'Wen-Dan Cheng' 'Jin-Shun Huang' _publ_section_title ; A redetermination of bis(2-aminomethylpyridine)diperchloratocopper(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900049 _journal_paper_doi 10.1107/S0108270199099485 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Cu (Cl O4)2 (C6 H8 N2)2]' _chemical_formula_sum 'C12 H16 Cl2 Cu N4 O8' _chemical_formula_weight 478.73 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 106.71(3) _cell_angle_beta 108.96(3) _cell_angle_gamma 95.64(3) _cell_formula_units_Z 1 _cell_length_a 7.6235(15) _cell_length_b 7.9661(16) _cell_length_c 7.9712(16) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.7 _cell_measurement_theta_min 13.0 _cell_volume 428.6(2) _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'XP (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _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 0.016 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1812 _diffrn_reflns_theta_full 25.97 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_min 2.73 _diffrn_standards_decay_% none _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.639 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_type 'empirical via \y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour Violet _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 243 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.513 _refine_diff_density_min -0.371 _refine_ls_extinction_coef 0.003(4) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 125 _refine_ls_number_reflns 1682 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.036 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0432P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.083 _reflns_number_gt 1357 _reflns_number_total 1682 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0091.cif _cod_data_source_block QA0091 _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. 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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0432P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0432P)^2^] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 428.56(15) _cod_database_code 2008492 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 0 0 0 .0244(2) Uani d S 1 . . Cu N1 -.0321(4) .1069(3) .2449(3) .0259(6) Uani d . 1 . . N N2 .1910(4) .2323(3) .1006(4) .0290(6) Uani d . 1 . . N H2A .2876 .2156 .0607 .035 Uiso calc R 1 . . H H2C .1362 .3146 .0578 .035 Uiso calc R 1 . . H C1 -.1791(5) .0553(5) .2899(5) .0358(8) Uani d . 1 . . C H1A -.2770 -.0393 .2011 .043 Uiso calc R 1 . . H C2 -.1900(5) .1373(5) .4625(5) .0404(8) Uani d . 1 . . C H2B -.2934 .0991 .4900 .049 Uiso calc R 1 . . H C3 -.0452(5) .2765(5) .5932(5) .0372(8) Uani d . 1 . . C H3A -.0484 .3330 .7115 .045 Uiso calc R 1 . . H C4 .1048(5) .3320(4) .5481(4) .0335(7) Uani d . 1 . . C H4A .2037 .4267 .6350 .040 Uiso calc R 1 . . H C5 .1066(4) .2450(4) .3718(4) .0260(7) Uani d . 1 . . C C6 .2634(5) .2970(4) .3093(4) .0315(7) Uani d . 1 . . C H6A .3067 .4263 .3582 .038 Uiso calc R 1 . . H H6B .3698 .2441 .3575 .038 Uiso calc R 1 . . H Cl1 .34552(10) -.27558(10) .09599(11) .0287(2) Uani d . 1 . . Cl O11 .1710(4) -.4066(3) .0010(4) .0478(7) Uani d . 1 . . O O12 .3049(4) -.1019(3) .1598(4) .0501(7) Uani d . 1 . . O O13 .4387(4) -.2783(4) -.0320(4) .0650(9) Uani d . 1 . . O O14 .4613(4) -.3120(4) .2551(4) .0659(9) Uani d . 1 . . O 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 .0214(3) .0264(3) .0237(3) .0013(2) .0099(2) .0053(2) N1 .0245(13) .0301(14) .0233(13) .0040(11) .0112(11) .0075(11) N2 .0293(14) .0266(14) .0333(15) .0050(12) .0166(12) .0081(12) C1 .0284(17) .041(2) .0346(18) -.0019(15) .0147(15) .0072(15) C2 .039(2) .052(2) .0369(19) .0113(17) .0221(16) .0151(17) C3 .043(2) .043(2) .0284(18) .0162(17) .0173(16) .0094(16) C4 .0356(18) .0325(18) .0257(17) .0082(15) .0061(15) .0058(14) C5 .0248(15) .0261(16) .0272(16) .0078(13) .0080(13) .0104(13) C6 .0270(17) .0264(17) .0339(18) .0002(14) .0095(14) .0036(14) Cl1 .0218(4) .0286(4) .0350(5) .0047(3) .0118(3) .0084(4) O11 .0302(13) .0418(15) .0600(17) -.0061(11) .0151(13) .0070(13) O12 .0574(17) .0322(14) .0528(17) .0185(13) .0137(14) .0075(12) O13 .0523(18) .076(2) .068(2) -.0033(16) .0449(17) .0063(17) O14 .0574(19) .072(2) .0604(19) .0297(17) -.0006(15) .0314(17) 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' 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 N1 Cu1 N1 2 . 180.0 N1 Cu1 N2 2 . 98.79(10) N1 Cu1 N2 . . 81.21(10) N1 Cu1 N2 2 2 81.21(10) N1 Cu1 N2 . 2 98.79(10) N2 Cu1 N2 . 2 180.0 N1 Cu1 O12 2 . 87.61(10) N1 Cu1 O12 . . 92.39(10) N2 Cu1 O12 . . 80.09(10) N2 Cu1 O12 2 . 99.91(10) C5 N1 C1 . . 118.5(3) C5 N1 Cu1 . . 115.2(2) C1 N1 Cu1 . . 126.3(2) C6 N2 Cu1 . . 109.25(19) N1 C1 C2 . . 122.4(3) C3 C2 C1 . . 118.6(3) C2 C3 C4 . . 119.5(3) C3 C4 C5 . . 119.0(3) N1 C5 C4 . . 121.8(3) N1 C5 C6 . . 115.3(3) C4 C5 C6 . . 122.9(3) N2 C6 C5 . . 108.9(3) O14 Cl1 O13 . . 110.90(19) O14 Cl1 O11 . . 110.06(19) O13 Cl1 O11 . . 108.91(17) O14 Cl1 O12 . . 108.36(18) O13 Cl1 O12 . . 109.48(18) O11 Cl1 O12 . . 109.11(17) Cl1 O12 Cu1 . . 125.93(16) 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 N1 2 1.998(2) ? Cu1 N1 . 1.998(2) ? Cu1 N2 . 2.012(3) ? Cu1 N2 2 2.012(3) ? Cu1 O12 . 2.593(3) ? N1 C5 . 1.337(4) ? N1 C1 . 1.345(4) ? N2 C6 . 1.481(4) ? C1 C2 . 1.377(5) ? C2 C3 . 1.372(5) ? C3 C4 . 1.375(5) ? C4 C5 . 1.382(4) ? C5 C6 . 1.502(4) ? Cl1 O14 . 1.416(3) ? Cl1 O13 . 1.417(3) ? Cl1 O11 . 1.432(3) ? Cl1 O12 . 1.432(2) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139056580