Na~3.88~Mo~15~Se~19~: a novel ternary reduced molybdenum selenide containing Mo~6~ and Mo~9~ clusters
Salloum, Diala; Gougeon, Patrick; Gall, Philippe; Acta Crystallographica Section E 69 (2013) i67–i68; doi:10.1107/S1600536813025907

data_2238670
_publ_section_title
;
 Na~3.88~Mo~15~Se~19~: a novel ternary reduced molybdenum selenide
 containing Mo~6~ and Mo~9~ clusters
;
_journal_coeditor_code           RU2054
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i67
_journal_page_last               i68
_journal_paper_doi               10.1107/S1600536813025907
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Na3.88 Mo15 Se19'
_chemical_formula_moiety         'Mo15 Na3.88 Se19'
_chemical_formula_sum            'Mo15 Na3.88 Se19'
_chemical_formula_weight         3028.54
_chemical_name_systematic
;
Tetrasodium pentadecamolybdenum nonadecaselenide
;
_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                   9.86470(10)
_cell_length_b                   9.86470(10)
_cell_length_c                   19.5957(3)
_cell_measurement_reflns_used    26001
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      1.70
_cell_volume                     1651.43(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) and PLATON (Spek, 2009)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25999
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    26.467
_exptl_absorpt_correction_T_max  0.2148
_exptl_absorpt_correction_T_min  0.1110
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multi-faceted crystal'
_exptl_crystal_F_000             2637
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.691
_refine_diff_density_min         -1.807
_refine_ls_extinction_coef       0.00058(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0435P)^2^+3.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                2116
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ru2054.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               2238670