Low Coordinate, Monomeric Molybdenum and Tungsten(III) Complexes: Structure, Reactivity and Calculational Studies of (silox)3Mo and (silox)3ML (M = Mo, W; L = PMe3, CO; silox =tBu3SiO)
David S. Kuiper; Peter T. Wolczanski; Emil B. Lobkovsky; Thomas R. Cundari; Journal of the American Chemical Society 130 (2008) 12931–12943; doi:10.1021/ja802706u

data_4108389
_publ_section_title
;
 Low Coordinate, Monomeric Molybdenum and Tungsten(III) Complexes:
 Structure, Reactivity and Calculational Studies of (silox)3Mo and
 (silox)3ML (M = Mo, W; L = PMe3, CO; silox =tBu3SiO)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12931
_journal_page_last               12943
_journal_paper_doi               10.1021/ja802706u
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C39 H90 Mo O3 P Si3'
_chemical_formula_sum            'C39 H90 Mo O3 P Si3'
_chemical_formula_weight         818.29
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 108.588(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.422(3)
_cell_length_b                   12.7232(14)
_cell_length_c                   33.774(4)
_cell_measurement_reflns_used    7919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.40
_cell_volume                     9540(2)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and 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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            46866
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.8518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         11388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+3.7714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                8500
_reflns_number_total             11388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802706u_si_001_1.cif
_cod_data_source_block           dk6
_cod_original_cell_volume        9539.6(18)
_cod_database_code               4108389