Sc~0.43(2)~Rb~2~Mo~15~S~19~, a partially Sc-filled variant of Rb~2~Mo~15~S~19~
Gougeon, Patrick; Al Rahal Al Orabi, Rabih; Gautier, Régis; Potel, Michel; Acta Crystallographica Section C 68 (2012) i25–i28; doi:10.1107/S0108270112016605

data_2018476
_publ_section_title
;
 Sc~0.43(2)~Rb~2~Mo~15~S~19~, a partially Sc-filled variant of
 Rb~2~Mo~15~S~19~
;
_journal_coeditor_code           FN3104
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i25
_journal_page_last               i28
_journal_paper_doi               10.1107/S0108270112016605
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'Sc0.43(2) Rb2 Mo15 S19'
_chemical_formula_moiety         'Mo15 Rb2 S19 Sc0.43'
_chemical_formula_sum            'Mo15 Rb2 S19 Sc0.43'
_chemical_formula_weight         2238.365
_chemical_name_systematic
'scandium dirubidium pentadecamolybdenum nonadecasulfide'
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.51730(10)
_cell_length_b                   9.51730(10)
_cell_length_c                   56.0061(9)
_cell_measurement_reflns_used    22338
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.76
_cell_measurement_theta_min      2.18
_cell_volume                     4393.33(10)
_computing_cell_refinement       'COLLECT (Nonius, 1998)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            13057
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    10.922
_exptl_absorpt_correction_T_max  0.4630
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multi-faceted
_exptl_crystal_F_000             6102
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.884
_refine_ls_extinction_coef       0.000087(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0000P)^2^+69.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                1383
_reflns_number_total             1431
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3104.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2018476
_cod_database_fobs_code          2018476