#------------------------------------------------------------------------------ #$Date: 2015-12-13 00:44:01 +0200 (Sun, 13 Dec 2015) $ #$Revision: 171462 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013257.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_2013257 loop_ _publ_author_name 'Trombe, Jean-Christian' 'Rozier, Patrick' 'Galy, Jean' _publ_section_title ; A new aquahydroxidocopper(II) oxovanadium(IV) vanadate, Cu(H~2~O)(OH)VO(VO~4~) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i50 _journal_page_last i52 _journal_paper_doi 10.1107/S0108270103008047 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'Cu (H2 O)(O H) V O (V O4)' _chemical_formula_moiety 'Cu1 H3 O7 V2' _chemical_formula_sum 'Cu H3 O7 V2' _chemical_formula_weight 280.45 _chemical_name_systematic ; aqua hydroxyl copper(II) oxo-vanadium(IV) vanadate ; _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 99.902(14) _cell_angle_beta 101.139(14) _cell_angle_gamma 101.495(13) _cell_formula_units_Z 2 _cell_length_a 5.1290(7) _cell_length_b 5.3070(10) _cell_length_c 10.3590(14) _cell_measurement_reflns_used 914 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.44 _cell_measurement_theta_min 6.17 _cell_volume 264.53(8) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius 1998)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1966)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Enraf-Nonius KappaCCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1972 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 6.17 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.416 _exptl_absorpt_correction_T_max 0.690 _exptl_absorpt_correction_T_min 0.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Sortav, Blessing, 1995 ; _exptl_crystal_colour blue-black _exptl_crystal_density_diffrn 3.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 268 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.979 _refine_diff_density_min -0.766 _refine_ls_extinction_coef 0.012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 95 _refine_ls_number_reflns 914 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.122 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0322 _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^)+(0.0373P)^2^+1.2774P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.0886 _reflns_number_gt 819 _reflns_number_total 914 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fa1011.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'Cu1 H3 O7 V2' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' 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 ; _cod_database_code 2013257 _cod_database_fobs_code 2013257 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 0.5000 0.5000 0.0000 0.0171(3) Uani d S 1 . . Cu Cu2 1.0000 0.5000 0.5000 0.0112(3) Uani d S 1 . . Cu V1 0.35925(17) 0.33092(16) 0.28053(8) 0.0097(3) Uani d . 1 . . V V2 0.82209(17) 0.92354(16) 0.33112(8) 0.0097(3) Uani d . 1 . . V O1 0.2810(8) 0.3489(8) 0.1168(4) 0.0189(9) Uani d . 1 . . O O2 0.5000(8) 0.0682(8) 0.2915(4) 0.0173(8) Uani d . 1 . . O O3 0.5815(8) 0.6165(7) 0.3739(4) 0.0149(8) Uani d . 1 . . O O4 0.0589(8) 0.2818(7) 0.3413(4) 0.0127(8) Uani d . 1 . . O O5 0.8394(9) 0.7799(8) 0.1833(4) 0.0203(9) Uani d . 1 . . O O6 1.1342(7) 0.8373(7) 0.4541(4) 0.0114(8) Uani d . 1 . . O H6 1.2927 0.8542 0.4126 0.016 Uiso d R 1 . . H O7 0.2872(9) 0.7689(8) -0.0090(4) 0.0218(9) Uani d . 1 . . O H7a 0.1252 0.7420 -0.0650 0.030 Uiso d R 1 . . H H7b 0.3161 0.8945 0.0630 0.030 Uiso d 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 0.0196(5) 0.0194(5) 0.0163(5) 0.0053(4) 0.0106(4) 0.0064(4) Cu2 0.0150(5) 0.0084(5) 0.0119(5) 0.0024(3) 0.0081(4) 0.0016(3) V1 0.0096(5) 0.0099(5) 0.0110(5) 0.0021(3) 0.0064(3) 0.0016(3) V2 0.0098(5) 0.0078(5) 0.0125(5) 0.0015(3) 0.0056(3) 0.0025(3) O1 0.018(2) 0.028(2) 0.0121(19) 0.0016(17) 0.0073(16) 0.0075(16) O2 0.0163(19) 0.0128(18) 0.024(2) 0.0033(15) 0.0084(16) 0.0040(15) O3 0.0151(19) 0.0150(19) 0.0151(19) -0.0006(15) 0.0073(15) 0.0054(15) O4 0.0152(19) 0.0118(17) 0.0128(18) 0.0030(15) 0.0077(15) 0.0029(14) O5 0.025(2) 0.020(2) 0.016(2) 0.0036(17) 0.0107(17) 0.0009(16) O6 0.0120(18) 0.0100(17) 0.0150(18) 0.0026(14) 0.0084(15) 0.0045(14) O7 0.023(2) 0.017(2) 0.024(2) 0.0062(17) 0.0059(17) 0.0015(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 O7 Cu1 O7 . 2_665 180.0 ? O7 Cu1 O1 . 2_665 90.59(17) yes O7 Cu1 O1 2_665 2_665 89.41(17) yes O7 Cu1 O1 . . 89.41(17) ? O7 Cu1 O1 2_665 . 90.59(17) ? O1 Cu1 O1 2_665 . 180.0 ? O7 Cu1 O5 . . 91.72(16) yes O7 Cu1 O5 2_665 . 88.28(16) yes O1 Cu1 O5 2_665 . 86.52(15) yes O1 Cu1 O5 . . 93.48(15) yes O7 Cu1 O5 . 2_665 88.28(16) ? O7 Cu1 O5 2_665 2_665 91.72(16) ? O1 Cu1 O5 2_665 2_665 93.48(15) ? O1 Cu1 O5 . 2_665 86.52(15) ? O5 Cu1 O5 . 2_665 180.0 ? O4 Cu2 O4 1_655 2_666 180.0000(10) ? O4 Cu2 O6 1_655 . 95.63(15) yes O4 Cu2 O6 2_666 . 84.37(15) yes O4 Cu2 O6 1_655 2_766 84.37(15) ? O4 Cu2 O6 2_666 2_766 95.63(15) ? O6 Cu2 O6 . 2_766 179.999(2) ? O4 Cu2 O3 1_655 2_766 84.89(14) yes O4 Cu2 O3 2_666 2_766 95.11(14) yes O6 Cu2 O3 . 2_766 105.92(13) yes O6 Cu2 O3 2_766 2_766 74.08(13) yes O4 Cu2 O3 1_655 . 95.11(14) ? O4 Cu2 O3 2_666 . 84.89(14) ? O6 Cu2 O3 . . 74.08(13) ? O6 Cu2 O3 2_766 . 105.92(13) ? O3 Cu2 O3 2_766 . 180.00(15) ? O1 V1 O2 . . 108.3(2) yes O1 V1 O3 . . 109.85(19) yes O2 V1 O3 . . 110.95(19) yes O1 V1 O4 . . 109.78(18) yes O2 V1 O4 . . 108.75(18) yes O3 V1 O4 . . 109.19(18) yes O5 V2 O2 . 1_565 102.8(2) yes O5 V2 O3 . . 97.96(18) yes O2 V2 O3 1_565 . 88.13(16) yes O5 V2 O4 . 1_665 98.45(18) yes O2 V2 O4 1_565 1_665 88.55(16) yes O3 V2 O4 . 1_665 163.58(15) yes O5 V2 O6 . . 102.55(19) yes O2 V2 O6 1_565 . 154.52(16) yes O3 V2 O6 . . 85.76(15) yes O4 V2 O6 1_665 . 90.38(15) yes O5 V2 O6 . 2_776 171.22(17) yes O2 V2 O6 1_565 2_776 82.41(15) yes O3 V2 O6 . 2_776 89.21(14) yes O4 V2 O6 1_665 2_776 74.42(13) yes O6 V2 O6 . 2_776 72.80(15) yes V1 O1 Cu1 . . 132.6(2) ? V1 O2 V2 . 1_545 150.3(2) ? V1 O3 V2 . . 134.8(2) ? V1 O3 Cu2 . . 108.03(18) ? V2 O3 Cu2 . . 90.26(14) ? V1 O4 Cu2 . 1_455 125.8(2) ? V1 O4 V2 . 1_445 123.7(2) ? Cu2 O4 V2 1_455 1_445 103.27(15) ? V2 O5 Cu1 . . 131.5(2) ? Cu2 O6 V2 . . 108.90(17) ? Cu2 O6 V2 . 2_776 93.28(14) ? V2 O6 V2 . 2_776 107.20(15) ? Cu2 O6 H6 . . 117.5 ? V2 O6 H6 . . 108.6 ? V2 O6 H6 2_776 . 120.1 ? Cu1 O7 H7a . . 123.6 ? Cu1 O7 H7b . . 118.1 ? H7a O7 H7b . . 113.9 ? 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 O7 . 1.965(4) yes Cu1 O7 2_665 1.966(4) ? Cu1 O1 2_665 1.967(4) yes Cu1 O1 . 1.967(4) ? Cu1 O5 . 2.359(4) yes Cu1 O5 2_665 2.359(4) ? Cu2 O4 1_655 1.953(3) yes Cu2 O4 2_666 1.953(3) yes Cu2 O6 . 1.958(3) yes Cu2 O6 2_766 1.958(3) ? Cu2 O3 2_766 2.534(4) yes Cu2 O3 . 2.534(4) ? V1 O1 . 1.690(4) yes V1 O2 . 1.704(4) yes V1 O3 . 1.707(4) yes V1 O4 . 1.763(4) yes V2 O5 . 1.617(4) yes V2 O2 1_565 1.959(4) yes V2 O3 . 2.008(4) yes V2 O4 1_665 2.016(4) yes V2 O6 . 2.025(4) yes V2 O6 2_776 2.309(4) yes O6 H6 . 0.9866 ? O7 H7a . 0.8866 ? O7 H7b . 0.8767 ? 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 _geom_hbond_publ_flag O6 H6 O2 1_665 0.99 2.13 2.979(5) 143.7 yes O6 H6 O3 1_655 0.99 2.18 2.967(5) 135.8 yes O7 H7a O1 2_565 0.89 1.98 2.812(6) 154.7 yes O7 H7b O2 1_565 0.88 2.32 3.114(6) 150.6 yes O7 H7b O1 1_565 0.88 2.43 3.138(6) 138.1 yes