Crystal Structure and Spectroscopic Characterization of K8(VO)2O(SO4)6
Søren B. Rasmussen; Rikke Mattsson Rasmussen; Rasmus Fehrmann; Kurt Nielsen; Inorganic Chemistry 42 (2003) 7123–7128; doi:10.1021/ic0301674

data_4312366
_publ_section_title
;
 Crystal Structure and Spectroscopic Characterization of K8(VO)2O(SO4)6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7123
_journal_page_last               7128
_journal_paper_doi               10.1021/ic0301674
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'K8 O27 S6 V2'
_chemical_formula_weight         1039.04
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.2860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5973(9)
_cell_length_b                   13.9288(9)
_cell_length_c                   14.0516(9)
_cell_measurement_temperature    568(2)
_cell_volume                     2661.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20232
_diffrn_reflns_theta_max         30.21
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.268
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         9624
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                7058
_reflns_number_total             9624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0301674.cif
_cod_data_source_block           shelxl
_cod_database_code               4312366