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_4300064
_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         '[(C72 H60 Mo3 N3 P6 S13) Br]. 2[C H2 Cl2]'
_chemical_formula_sum            'C74 H64 Br Cl4 Mo3 N3 P6 S13'
_chemical_formula_weight         2107.41
_chemical_melting_point          316(1)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.570(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.309(4)
_cell_length_b                   24.971(8)
_cell_length_c                   26.206(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.56
_cell_volume                     8692(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52806
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.622
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   'Semi-empirical ellipsoidal'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             4224
_refine_diff_density_max         2.569
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.503
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         15259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.503
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          5.541
_refine_ls_shift/su_mean         0.085
_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          0.1230
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                10311
_reflns_number_total             15259
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300064
_journal_paper_doi 10.1021/ic9907056