Oxidation State of Uranium in A6Cu12U2S15 (A = K, Rb, Cs) Compounds
Christos D. Malliakas; Jiyong Yao; Daniel M. Wells; Geng Bang Jin; S. Skanthakumar; Eun Sang Choi; Mahalingam Balasubramanian; L. Soderholm; Donald E. Ellis; Mercouri G. Kanatzidis; James A. Ibers; Inorganic Chemistry 51 (2012) 6153–6163; doi:10.1021/ic300172k

data_4329332
_publ_section_title
;
 Oxidation State of Uranium in A6Cu12U2S15 (A = K, Rb, Cs) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6153
_journal_page_last               6163
_journal_paper_doi               10.1021/ic300172k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Cu12 K6 S15 U2'
_chemical_formula_weight         1954.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.5520(3)
_cell_length_b                   18.5520(3)
_cell_length_c                   18.5520(3)
_cell_measurement_reflns_used    96482
_cell_measurement_temperature    100.0(3)
_cell_volume                     6385.17(18)
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      ' 180 frames, detector distance = 60 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            85030
_diffrn_reflns_theta_full        35.05
_diffrn_reflns_theta_max         35.05
_diffrn_reflns_theta_min         3.11
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    19.676
_exptl_absorpt_correction_T_max  0.1433
_exptl_absorpt_correction_T_min  0.0729
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape
_exptl_crystal_density_diffrn    4.066
_exptl_crystal_F_000             7086
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.245
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.356
_refine_ls_extinction_coef       0.000085(16)
_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   1.190
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         4841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0481P)^2^+128.6468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                4735
_reflns_number_total             4841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300172k_si_003_2.cif
_cod_data_source_block           K6Cu12U2S15_100K
_cod_database_code               4329332