Reactivity of the [Mo3(μ3-S)(μ2-S2)3Br6]2- Anion toward the Imidodiphosphinochalcogenido Ligands [N(QPPh2)2]- (Q = S, Se): Synthesis and Characterization of [Mo3(μ3-S)(μ2-S2)3{N(QPPh2)2}3]Br
Virginie Béreau; Christopher G. Pernin; James A. Ibers; Inorganic Chemistry 39 (2000) 854–856; doi:10.1021/ic9907056

data_4300065
_publ_section_title
;
Reactivity of the [Mo3(\m3-S)(\m2-S2)3Br6]2- Anion toward the
Imidodiphosphinochalcogenido Ligands [N(QPPh2)2]- (Q = S, Se): Synthesis
and Characterization of [Mo3(\m3-S)(\m2-S2)3{N(QPPh2)2}3]Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              854
_journal_page_last               856
_journal_paper_doi               10.1021/ic9907056
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(C72 H60 Mo3 P6 S7 Se6) Br'
_chemical_formula_sum            'C72 H60 Br Mo3 N3 P6 S7 Se6'
_chemical_formula_weight         2218.96
_chemical_melting_point          315(1)
_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_hydrogens   geom
_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            12
_cell_length_a                   21.076(3)
_cell_length_b                   21.076(3)
_cell_length_c                   75.848(15)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      1.24
_cell_volume                     29178(8)
_computing_cell_refinement       'SAINT-Plus version 5.101 (Bruker, 1997)'
_computing_data_collection       'SMART version 5.101 (Bruker, 1997)'
_computing_data_reduction        'SAINT-Plus version 5.101 (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Standard-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            56780
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_correction_type   'Semi-empirical ellipsoidal'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             12960
_refine_diff_density_max         3.451
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.327
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.327
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                3065
_reflns_number_total             4668
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        29179(8)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4300065