Syntheses, modulated crystal structures of Ba6−2xU2+xAg4Se12 (x = 0 and 0.5), and crystal structure and spectroscopy of Sr4Th2.78Cu4S12
Mesbah, Adel; Prakash, Jai; Beard, Jessica C.; Malliakas, Christos D.; Lebègue, Sébastien; Ibers, James A.; Journal of Solid State Chemistry 268 (2018) 30–35; doi:10.1016/j.jssc.2018.08.025

data_1560713
_publ_section_title
;
 Syntheses, modulated crystal structures of Ba6&#x2212;2xU2+xAg4Se12
 (x&#x202F;=&#x202F;0 and 0.5), and crystal structure and spectroscopy of
 Sr4Th2.78Cu4S12
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              30
_journal_page_last               35
_journal_paper_doi               10.1016/j.jssc.2018.08.025
_journal_volume                  268
_journal_year                    2018
_chemical_formula_moiety         '0.5(Cu8 S24 Sr8 Th6)'
_chemical_formula_sum            'Cu4 S12 Sr4 Th3'
_chemical_formula_weight         1685.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2292(3)
_cell_length_b                   11.5252(4)
_cell_length_c                   11.1483(4)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.580
_cell_measurement_theta_min      2.542
_cell_volume                     1057.34(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20670
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.542
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    36.110
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.4422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0706 before and 0.0437 after correction. The Ratio of minimum to maximum transmission is 0.5919. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.294
_exptl_crystal_description       needle
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.639
_refine_diff_density_min         -3.139
_refine_diff_density_rms         0.450
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_coef       0.00079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3268
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+10.4653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2830
_reflns_number_total             3268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Sr4Cu4Th3S12_SUMP.CIF
_cod_data_source_block           mo_p8_0m_th_vacancies
_cod_database_code               1560713
_shelx_estimated_absorpt_t_max   0.465
_shelx_estimated_absorpt_t_min   0.024
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(3)
 0.51(3)
2. Others
 0.5*[Sof(Th1)]+1*[Sof(Th2)]+0.5*[Sof(Th3)]=1.5 with esd of 0.0001
;
_shelx_res_checksum              83197
_shelx_hkl_checksum              64216
_olex2_submission_special_instructions 'No special instructions were received'