Hydride transfer reactions in dimolybdenum compounds: a simple route to the novel μ-η1∶η1-tetrahydroboride complex [Mo2Cp2(μ-SMe)3(μ-BH4)]
Schollhammer, Philippe; Cabon, Nolwenn; Pétillon, François Y.; Talarmin, Jean; Muir, Kenneth W.; Chemical Communications  (2000) 2137–; doi:10.1039/b006457m

data_7111092
_publ_section_title
;
 Hydride transfer reactions in dimolybdenum compounds: a simple route to
 the novel \m-\h1&#x2236;\h1-tetrahydroboride complex
 [Mo2Cp2(\m-SMe)3(\m-BH4)]
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2137
_journal_paper_doi               10.1039/b006457m
_journal_year                    2000
_chemical_formula_moiety         'C13 H23 B1 Mo2 S3'
_chemical_formula_sum            'C13 H23 B Mo2 S3'
_chemical_formula_weight         478.18
_chemical_name_systematic
;
 ?
;
_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                 100.774(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7445(13)
_cell_length_b                   10.4279(7)
_cell_length_c                   14.1960(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      15.4
_cell_volume                     1707.9(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0113
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8632
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.8444
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   7
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0235P)^2^+2.5813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                2373
_reflns_number_total             3366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006457msup1.cif
_cod_data_source_block           km2199
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7111092
_exptl_absorpt_factor_mur        0.000
_exptl_absorpt_correction_t_ave  0.9332
_exptl_absorpt_rmerge_before     0.0256
_exptl_absorpt_rmerge_after      0.0120
_exptl_absorpt_theta_corr_max    1.0000
_exptl_absorpt_theta_corr_min    0.9994