η3-Silapropargyl/Alkynylsilyl Molybdenum Complexes: Synthesis, Structure, and Reactivity toward Methanol
Mako Yabe-Yoshida; Chizuko Kabuto; Kuninobu Kabuto; Eunsang Kwon; Hiroyuki Sakaba; Journal of the American Chemical Society 131 (2009) 9138–9139; doi:10.1021/ja9005833

data_4104637
_publ_section_title
;
 \h3-Silapropargyl/Alkynylsilyl Molybdenum Complexes: Synthesis,
 Structure, and Reactivity toward Methanol
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9138
_journal_page_last               9139
_journal_paper_doi               10.1021/ja9005833
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C29 H32 Mo O2 Si '
_chemical_formula_sum            'C29 H32 Mo O2 Si'
_chemical_formula_weight         536.60
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.962(2)
_cell_length_b                   17.016(4)
_cell_length_c                   17.214(5)
_cell_measurement_reflns_used    8598
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2625.1(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38127
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3384
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 4 parameters (Carruthers & Watkin, 1979)
    8355.7400    11560.6000    3415.8600    0.0000
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                2609
_reflns_number_total             3384
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9005833_si_002_2.cif
_cod_data_source_block           complex3b
_cod_original_cell_volume        2625.0(12)
_cod_original_formula_sum        'C29 H32 Mo O2 Si '
_cod_database_code               4104637