#------------------------------------------------------------------------------ #$Date: 2022-09-15 15:52:48 +0300 (Thu, 15 Sep 2022) $ #$Revision: 277877 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/00/95/7009557.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_7009557 loop_ _publ_author_name 'Daniela Belli Dell'Amico' 'Rocco Alessio' 'Fausto Calderazzo' 'Fabrizio Della Pina' 'Ulli Englert' 'Guido Pampaloni' 'Vincenzo Passarelli' _publ_section_title ; Synproportionation reactions between copper(II) trihalogenoacetates Cu(CX3CO2)2, X = F, Cl or Br, and copper in the presence of carbon monoxide ; _journal_issue 13 _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_page_first 2067 _journal_page_last 2075 _journal_paper_doi 10.1039/b001889i _journal_year 2000 _chemical_formula_sum 'C12 H2 Cl18 Cu2 O12' _chemical_formula_weight 1103.38 _chemical_name_common ' chloroacetato derivative Cu2(CCl3COO)4(CCl3COOH)2' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall 'P -1' _space_group_name_H-M_alt 'P -1' _atom_type_scat_source International_Tables_for_Xray_Crystallography _cell_angle_alpha 79.00(2) _cell_angle_beta 67.62(3) _cell_angle_gamma 73.08(2) _cell_formula_units_Z 1.00 _cell_length_a 9.354(4) _cell_length_b 9.650(1) _cell_length_c 10.875(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 203 _cell_measurement_theta_max 12 _cell_measurement_theta_min 9 _cell_volume 864.9(6) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_structure_solution none _diffrn_ambient_temperature 203 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6832 _diffrn_reflns_theta_max 45.0 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.687 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_type empirical _exptl_crystal_colour blue-green _exptl_crystal_density_diffrn 2.12 _exptl_crystal_density_meas ? _exptl_crystal_description platelet _exptl_crystal_F_000 534 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.7142 _refine_diff_density_min -0.7309 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.952 _refine_ls_hydrogen_treatment riding _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 2748 _refine_ls_number_restraints 4 _refine_ls_R_factor_obs 0.069 _refine_ls_shift/esd_max 0.022 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.075 _reflns_number_observed 2748 _reflns_number_total 3384 _reflns_observed_criterion >1.0\s(I) _cod_data_source_file b001889i.txt _cod_data_source_block GP32_22119 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 7009557 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z 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 Cu 0.0216(3) 0.0268(3) 0.0164(3) -0.0078(2) -0.0044(2) 0.0006(3) O11 0.039(2) 0.033(2) 0.026(2) -0.019(2) -0.009(2) -0.000(2) C12 0.024(3) 0.025(3) 0.025(3) -0.006(2) -0.011(2) -0.001(2) O13 0.033(2) 0.032(2) 0.024(2) -0.012(2) -0.002(2) -0.006(2) C14 0.038(3) 0.037(3) 0.024(3) -0.018(2) -0.006(2) -0.001(3) Cl15 0.073(1) 0.0679(9) 0.048(1) -0.0511(7) -0.0009(8) -0.0153(8) Cl16 0.085(1) 0.060(1) 0.0268(7) -0.0433(7) -0.0145(7) -0.0033(7) Cl17 0.054(1) 0.043(1) 0.062(1) 0.008(1) -0.004(1) -0.007(1) O21 0.029(2) 0.043(3) 0.031(2) -0.010(2) -0.014(2) 0.008(2) C22 0.030(3) 0.030(3) 0.028(3) -0.005(2) -0.015(2) -0.001(2) O23 0.029(2) 0.040(3) 0.032(2) -0.007(2) -0.016(2) 0.005(2) C24 0.041(4) 0.033(4) 0.042(4) -0.012(3) -0.027(3) 0.015(4) Cl25 0.054(1) 0.057(1) 0.108(2) -0.023(1) -0.047(1) 0.053(1) Cl26 0.027(1) 0.097(2) 0.072(2) -0.003(1) -0.017(1) 0.025(2) Cl27 0.107(2) 0.100(2) 0.084(1) -0.018(1) -0.065(1) -0.021(1) O31 0.034(2) 0.038(2) 0.021(2) -0.018(2) -0.003(2) -0.000(2) C32 0.033(3) 0.033(3) 0.032(3) -0.010(3) -0.009(2) -0.001(3) O33 0.097(3) 0.051(3) 0.031(2) -0.049(2) -0.015(2) 0.003(2) C34 0.030(3) 0.029(3) 0.029(3) -0.012(2) -0.010(2) 0.000(3) Cl35 0.0667(9) 0.086(1) 0.044(1) -0.0565(7) -0.0125(7) 0.0062(9) Cl36 0.084(1) 0.067(1) 0.0264(9) -0.028(1) 0.0011(9) -0.0090(8) Cl37 0.058(1) 0.056(1) 0.095(2) 0.005(1) -0.031(1) 0.019(1) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Cu 0.39675(9) 0.43902(8) 0.10041(7) 0.0222(2) Ueq O11 0.3877(5) 0.6027(5) 0.1929(4) 0.031(1) Ueq C12 0.4623(7) 0.6985(7) 0.1369(6) 0.024(2) Ueq O13 0.5595(5) 0.7051(5) 0.0209(4) 0.030(1) Ueq C14 0.4234(8) 0.8277(7) 0.2199(6) 0.032(2) Ueq Cl15 0.5767(2) 0.9184(2) 0.1621(2) 0.0597(6) Ueq Cl16 0.3903(2) 0.7625(2) 0.3890(2) 0.0532(6) Ueq Cl17 0.2489(3) 0.9446(2) 0.2012(2) 0.0622(8) Ueq O21 0.5867(5) 0.3332(5) 0.1439(4) 0.035(1) Ueq C22 0.7227(7) 0.3566(7) 0.0766(6) 0.029(2) Ueq O23 0.2370(5) 0.5637(5) 0.0281(4) 0.034(1) Ueq C24 0.847(1) 0.288(1) 0.1423(8) 0.037(3) Ueq Cl25 0.8174(3) 0.1266(3) 0.2395(3) 0.0739(9) Ueq Cl26 1.0412(3) 0.2725(4) 0.0301(3) 0.073(1) Ueq Cl27 0.8140(4) 0.4136(4) 0.2584(3) 0.087(1) Ueq O31 0.2437(5) 0.3525(5) 0.2832(4) 0.031(1) Ueq C32 0.2256(8) 0.3652(7) 0.3964(7) 0.033(2) Ueq O33 0.2608(7) 0.4640(6) 0.4384(5) 0.056(2) Ueq C34 0.1645(7) 0.2527(7) 0.5088(6) 0.029(2) Ueq Cl35 0.0377(2) 0.1789(2) 0.4734(2) 0.0605(6) Ueq Cl36 0.0673(3) 0.3217(3) 0.6651(2) 0.0623(8) Ueq Cl37 0.3362(3) 0.1172(3) 0.5101(3) 0.0763(9) Ueq H 0.2808 0.5405 0.3783 0.0507 Uiso C24a 0.870(5) 0.233(5) 0.112(4) 0.05(1) Uiso Cl25a 0.793(3) 0.231(3) 0.291(3) 0.155(9) Uiso Cl26a 1.000(1) 0.344(1) 0.101(1) 0.062(3) Uiso Cl27a 0.948(2) 0.104(1) 0.016(1) 0.070(4) Uiso loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cu Cu O11 82.0(1) ? Cu Cu O13 85.9(1) ? Cu Cu O21 83.0(1) ? Cu Cu O23 85.6(1) ? Cu Cu O31 170.7(1) ? O11 Cu O13 167.9(1) ? O11 Cu O21 87.5(2) ? O11 Cu O23 90.5(2) ? O11 Cu O31 90.1(1) ? O13 Cu O21 90.1(2) ? O13 Cu O23 89.5(2) ? O13 Cu O31 101.8(1) ? O21 Cu O23 168.5(1) ? O21 Cu O31 91.8(1) ? O23 Cu O31 99.5(1) ? Cu O11 C12 123.4(3) ? O11 C12 O13 127.5(5) ? O11 C12 C14 115.8(4) ? O13 C12 C14 116.7(4) ? Cu O13 C12 121.1(3) ? C12 C14 Cl15 111.9(3) ? C12 C14 Cl16 109.4(3) ? C12 C14 Cl17 105.3(3) ? Cl15 C14 Cl16 109.5(3) ? Cl15 C14 Cl17 110.2(3) ? Cl16 C14 Cl17 110.5(3) ? Cu O21 C22 122.2(3) ? O21 C22 O23 128.8(5) ? O21 C22 C24 114.2(5) ? O23 C22 C24 116.8(5) ? Cu O23 C22 120.2(3) ? C22 C24 Cl25 112.9(5) ? C22 C24 Cl26 112.8(5) ? C22 C24 Cl27 104.6(5) ? Cl25 C24 Cl26 113.0(5) ? Cl25 C24 Cl27 105.2(5) ? Cl26 C24 Cl27 107.5(5) ? Cu O31 C32 129.2(3) ? O31 C32 O33 127.4(5) ? O31 C32 C34 120.4(5) ? O33 C32 C34 112.1(4) ? C32 O33 H 114.49 ? C32 C34 Cl35 110.3(4) ? C32 C34 Cl36 113.4(4) ? C32 C34 Cl37 104.4(4) ? Cl35 C34 Cl36 109.4(3) ? Cl35 C34 Cl37 109.4(3) ? Cl36 C34 Cl37 109.7(3) ? Cl25a C24a Cl26a 90(2) ? Cl25a C24a Cl27a 132(3) ? Cl26a C24a Cl27a 115(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu Cu 2.648(1) ? Cu O11 1.995(3) ? Cu O13 1.949(3) ? Cu O21 1.956(3) ? Cu O23 1.945(3) ? Cu O31 2.143(3) ? O11 C12 1.244(5) ? C12 O13 1.245(5) ? C12 C14 1.555(7) ? C14 Cl15 1.747(5) ? C14 Cl16 1.764(5) ? C14 Cl17 1.754(6) ? O21 C22 1.265(6) ? C22 O23 1.240(6) ? C22 C24 1.522(9) ? C24 Cl25 1.739(8) ? C24 Cl26 1.738(9) ? C24 Cl27 1.79(1) ? O31 C32 1.202(6) ? C32 O33 1.300(6) ? C32 C34 1.524(7) ? O33 H 0.9000 ? C34 Cl35 1.734(5) ? C34 Cl36 1.750(5) ? C34 Cl37 1.754(5) ? C24a Cl25a 1.80(5) ? C24a Cl26a 1.80(4) ? C24a Cl27a 1.60(4) ? H O11 1.9440 ? loop_ _cod_changelog_entry_id _cod_changelog_entry_author _cod_changelog_entry_date _cod_changelog_entry_text 1 'Vaitkus, Antanas' 2022-09-15T15:50:00+03:00 ; Added an explicit space group operation list and updated space group information. ;