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_4108390
_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 O3 P Si3 W)2'
_chemical_formula_sum            'C78 H180 O6 P2 Si6 W2'
_chemical_formula_weight         1812.40
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.760(4)
_cell_angle_beta                 80.022(4)
_cell_angle_gamma                76.894(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9564(11)
_cell_length_b                   20.4690(17)
_cell_length_c                   21.6634(17)
_cell_measurement_reflns_used    8858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     5001.4(7)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            144395
_diffrn_reflns_theta_full        31.10
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.443
_exptl_absorpt_correction_T_max  0.6408
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         31033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          1.066
_refine_ls_shift/su_mean         0.048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.0782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                21805
_reflns_number_total             31033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802706u_si_001_2.cif
_cod_data_source_block           dk10
_cod_database_code               4108390