Electrochemical-hydrothermal synthesis and structure of [N(CH3)4]2[Co(H2O)4V12O28]
Wang, Xiqu; Liu, Lumei; Jacobson, Allan J.; Ross, Kent; Journal of Materials Chemistry 9 (1999) 859–; doi:10.1039/a809999e

data_7213003
_publ_section_title
;
 Electrochemical-hydrothermal synthesis and structure of
 [N(CH3)4]2[Co(H2O)4V12O28]
;
_journal_issue                   4
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              859
_journal_paper_doi               10.1039/a809999e
_journal_volume                  9
_journal_year                    1999
_chemical_formula_sum            'C8 H32 Co N2 O32 V12'
_chemical_formula_weight         1338.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                83.003(2)
_cell_angle_beta                 85.739(2)
_cell_angle_gamma                83.971(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6510(6)
_cell_length_b                   10.7485(10)
_cell_length_c                   13.4022(13)
_cell_measurement_temperature    293(2)
_cell_volume                     943.87(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5593
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    3.348
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_F_000             653
_refine_diff_density_max         1.006
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.230
_refine_ls_extinction_coef       0.0024(9)
_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_all   1.021
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_obs          0.0668
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1741
_refine_ls_wR_factor_obs         0.1419
_reflns_number_observed          2575
_reflns_number_total             3894
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809999esup1.cif
_cod_data_source_block           '[N(CH3)4]2[Co(H2O)4V12O28]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.0000P] 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^)+(0.0834P)^2^+0.0000P] 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        943.9(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213003