Formation of New μ-Thioalkylidene and μ-Borohydride Dimolybdenum Complexes from the μ-Alkylidyne Precursor [Mo2Cp2(μ-SMe)3(μ-CCH2Ph)]
Le Goff, Alan; Le Roy, Christine; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Organometallics 26 (2007) 3607–; doi:10.1021/om7003496

data_4073472
_publ_section_title
;
 Formation of New \m-Thioalkylidene and \m-Borohydride Dimolybdenum
 Complexes from the \m-Alkylidyne Precursor [Mo2Cp2(\m-SMe)3(\m-CCH2Ph)]
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3607
_journal_paper_doi               10.1021/om7003496
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C20 H27 B Mo2 S2'
_chemical_formula_weight         534.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-04-12T17:50:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.602(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5128(7)
_cell_length_b                   30.503(2)
_cell_length_c                   7.8636(6)
_cell_measurement_temperature    170(2)
_cell_volume                     2035.3(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type
;
X-CALIBUR-2 CCD 4-circle diffractometer
;
_diffrn_measurement_method
;
4 omega-scans with kappa -79 deg (chi -58.3 deg), phi 0, 90, 180, 270 deg
1 phi-scan
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25391
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         3.46
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.8240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
        Scale3 Abspack program including interframe scaling, empirical
        absorption correction (Blessing) and detector sensitivity correction.
;
_exptl_crystal_colour            'dark mauve'
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate, main faces <1 0 0>'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+14.6823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.129
_reflns_number_gt                3727
_reflns_number_total             4926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7003496-file001.cif
_cod_data_source_block           b1a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4073472