Cs~6~Mo~27~S~31~: a novel ternary reduced molybdenum sulfide containing Mo~9~ and Mo~18~ clusters
Picard, S.; Salloum, D.; Gougeon, P.; Potel, M.; Acta Crystallographica Section C 59 (2003) i112–i114; doi:10.1107/S0108270103006243

data_2013547
_publ_section_title
;
 Cs~6~Mo~27~S~31~: a novel ternary reduced molybdenum sulfide
 containing Mo~9~ and Mo~18~ clusters
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i112
_journal_page_last               i114
_journal_paper_doi               10.1107/S0108270103006243
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'Cs6 Mo27 S31'
_chemical_formula_moiety         'Cs6 Mo27 S31'
_chemical_formula_sum            'Cs6 Mo27 S31'
_chemical_formula_weight         4381.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     isomor
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.44240(5)
_cell_length_b                   9.44240(5)
_cell_length_c                   110.0790(7)
_cell_measurement_reflns_used    94508
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.55
_cell_volume                     8499.63(8)
_computing_cell_refinement       COLLECT
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       198
_diffrn_reflns_limit_l_min       -198
_diffrn_reflns_number            85183
_diffrn_reflns_theta_full        39.98
_diffrn_reflns_theta_max         39.98
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.686
_exptl_absorpt_correction_T_max  0.4535
_exptl_absorpt_correction_T_min  0.2749
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaar & Tompa, 1965)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             11760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.455
_refine_diff_density_min         -2.811
_refine_ls_extinction_coef       0.000148(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0133P)^2^+67.7286P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                4683
_reflns_number_total             5858
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bc1009.cif
_cod_data_source_block           I
_cod_original_cell_volume        8499.62(8)
_cod_original_sg_symbol_Hall     '-R 32"c'
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2013547
_cod_database_fobs_code          2013547