Na~2.9~KMo~12~S~14~: a novel quaternary reduced molybdenum sulfide containing Mo~12~ clusters with a channel structure
Gougeon, Patrick; Gall, Philippe; Salloum, Diala; Acta Crystallographica Section E 69 (2013) i38–; doi:10.1107/S1600536813013603

data_2238004
_publ_section_title
;
 Na~2.9~KMo~12~S~14~: a novel quaternary reduced molybdenum sulfide
 containing Mo~12~ clusters with a channel structure
;
_journal_coeditor_code           RU2051
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i38
_journal_paper_doi               10.1107/S1600536813013603
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Na2.90 K Mo12 S14'
_chemical_formula_moiety         'K Mo12 Na2.90 S14'
_chemical_formula_sum            'K Mo12 Na2.9 S14'
_chemical_formula_weight         1705.89
_chemical_name_systematic
;
Trisodium potassium dodecamolybdenum tetradecasulfide
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                   9.36640(10)
_cell_length_b                   9.36640(10)
_cell_length_c                   16.2981(2)
_cell_measurement_reflns_used    5780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.76
_cell_measurement_theta_min      3.54
_cell_volume                     1238.26(2)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37291
_diffrn_reflns_theta_full        39.76
_diffrn_reflns_theta_max         39.76
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    7.242
_exptl_absorpt_correction_T_max  0.5719
_exptl_absorpt_correction_T_min  0.5498
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multi-faceted crystal'
_exptl_crystal_F_000             1558
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.743
_refine_diff_density_min         -1.840
_refine_ls_extinction_coef       0.00032(9)
_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   1.132
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         2536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0290P)^2^+4.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                2376
_reflns_number_total             2536
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ru2051.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -31c'
_cod_original_formula_sum        'K Mo12 Na2.90 S14'
_cod_database_code               2238004
_cod_database_fobs_code          2238004