Cu~3~V~10~O~28~·24H~2~O and CuNa~4~V~10~O~28~·23H~2~O
Iida, Akifumi; Ozeki, Tomoji; Acta Crystallographica Section C 59 (2003) i41–i44; doi:10.1107/S0108270103008552

data_2013242
_publ_section_title
;
 Cu~3~V~10~O~28~&#x00B7;24H~2~O and CuNa~4~V~10~O~28~&#x00B7;23H~2~O
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i41
_journal_page_last               i44
_journal_paper_doi               10.1107/S0108270103008552
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         '(Cu 2+)3, (V10 O28 6-), 24(H2 O)'
_chemical_formula_sum            'Cu3 H48 O52 V10'
_chemical_formula_weight         1580.40
_chemical_name_common            'tricopper decavanadate icositetrahydrate'
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.662(2)
_cell_angle_beta                 95.579(3)
_cell_angle_gamma                102.064(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8567(5)
_cell_length_b                   10.7189(6)
_cell_length_c                   11.5492(7)
_cell_measurement_reflns_used    5734
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.85
_cell_volume                     1024.14(10)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku Corporation, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku Corporation, 1998)'
_computing_molecular_graphics
'ATOMS (Dowty, 1999) and ORTEP-III (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Ultrax rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9090
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.833
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             781
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.968
_refine_ls_extinction_coef       0.0433(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.342
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                4486
_reflns_number_total             4688
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bc1014.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H48 Cu3 O52 V10'
_cod_database_code               2013242
_cod_database_fobs_code          2013242