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_4300063
_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_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(C8 H20 N)2 (Br6 Mo3 S7)'
_chemical_formula_sum            'C16 H40 Br6 Mo3 N2 S7'
_chemical_formula_weight         1252.20
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.928(13)
_cell_length_b                   12.769(9)
_cell_length_c                   29.50(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.38
_cell_volume                     7130(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1119
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52783
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    8.187
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   'semi-empirical ellipsoidal'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4784
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0344
_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 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                4069
_reflns_number_total             6282
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        7131(9)
_cod_database_code               4300063
_journal_paper_doi 10.1021/ic9907056