Na~4.25~Mo~15~S~19~: a novel ternary reduced molybdenum sulfide containing Mo~6~ and Mo~9~ clusters
Salloum, D.; Gougeon, P.; Gall, P.; Acta Crystallographica Section E 70 (2014) i30–; doi:10.1107/S160053681401201X

data_2239626
_publ_section_title
;
 Na~4.25~Mo~15~S~19~: a novel ternary reduced molybdenum sulfide
 containing Mo~6~ and Mo~9~ clusters
;
_journal_coeditor_code           RU2060
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i30
_journal_paper_doi               10.1107/S160053681401201X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Na4.25 Mo15 S19'
_chemical_formula_sum            'Mo15 Na4.25 S19'
_chemical_formula_weight         2145.95
_chemical_name_systematic
;
Tetrasodium pentadecamolybdenum nonadecasulfide
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   9.53400(10)
_cell_length_b                   9.53400(10)
_cell_length_c                   18.9803(3)
_cell_measurement_reflns_used    16576
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.15
_cell_volume                     1494.11(3)
_computing_cell_refinement       'COLLECT (Nonius, 1998)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16576
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    7.443
_exptl_absorpt_correction_T_max  0.5914
_exptl_absorpt_correction_T_min  0.3631
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaar & Tompa, 1965)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multi-faceted crystal'
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.851
_refine_ls_extinction_coef       0.00266(19)
_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   1.130
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0337P)^2^+5.1576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                1322
_reflns_number_total             1500
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ru2060sup1.cf
_cod_data_source_block           I
_cod_database_code               2239626
_cod_database_fobs_code          2239626