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_4104636
_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_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C30 H34 Mo O2 Si '
_chemical_formula_sum            'C30 H34 Mo O2 Si'
_chemical_formula_weight         550.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 115.3265(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.0724(5)
_cell_length_b                   16.3900(8)
_cell_length_c                   9.9887(5)
_cell_measurement_reflns_used    3421
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     1342.53(12)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.062
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17851
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       prism
_exptl_crystal_F_000             572.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.27
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2902 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5643
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.0053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                5624
_reflns_number_total             6076
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9005833_si_002_1.cif
_cod_data_source_block           complex3a
_cod_original_formula_sum        'C30 H34 Mo O2 Si '
_cod_database_code               4104636