K2Na8(UO2)8Mo4O24[(S,Mo)O4], the first uranium molybdosulfate: synthesis, crystal structure, and comparison to related compounds
Sergey V. Krivovichev; Journal of GeoSciences 59 (2014) 115–121; doi:10.3190/jgeosci.166

data_1566325
_publ_section_title
;
 K2Na8(UO2)8Mo4O24[(S,Mo)O4], the first uranium molybdosulfate: synthesis,
 crystal structure, and comparison to related compounds
;
_journal_name_full               'Journal of GeoSciences'
_journal_page_first              115
_journal_page_last               121
_journal_paper_doi               10.3190/jgeosci.166
_journal_volume                  59
_journal_year                    2014
_chemical_formula_sum            'K0.68 Mo2.08 Na4.32 O22 S0.42 U4'
_chemical_formula_weight         1643.13
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.282(4)
_cell_length_b                   12.1170(18)
_cell_length_c                   13.6174(17)
_cell_measurement_temperature    293(2)
_cell_volume                     3844.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14743
_diffrn_reflns_theta_full        27.31
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    35.287
_exptl_crystal_density_diffrn    5.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5588
_refine_diff_density_max         3.239
_refine_diff_density_min         -4.255
_refine_diff_density_rms         0.539
_refine_ls_extinction_coef       0.000138(10)
_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   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0415P)^2^+643.0607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                2837
_reflns_number_total             4237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jgeosci.166_krivovichev_hsk4b.cif
_cod_data_source_block           hsk4b
_cod_original_cell_volume        3845.0(9)
_cod_database_code               1566325