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_4104638
_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         'C31 H38 Mo O3 Si '
_chemical_formula_sum            'C31 H38 Mo O3 Si'
_chemical_formula_weight         582.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                100.000(3)
_cell_angle_beta                 96.530(3)
_cell_angle_gamma                99.907(3)
_cell_formula_units_Z            4
_cell_length_a                   11.3091(8)
_cell_length_b                   14.9091(11)
_cell_length_c                   18.1392(11)
_cell_measurement_reflns_used    6557
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2934.4(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38031
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.72
_refine_diff_density_min         -1.03
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     713
_refine_ls_number_reflns         13180
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0041Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                10505
_reflns_number_total             13180
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9005833_si_002_3.cif
_cod_data_source_block           complex5a
_cod_original_cell_volume        2934.4(3)
_cod_original_formula_sum        'C31 H38 Mo O3 Si '
_cod_database_code               4104638