η3-Silaallyl/Alkenylsilyl Molybdenum Complex: Synthesis, Structure, and Reactivity toward Primary Amines To Form Mo‒N‒Si Three-Membered Cyclic Complexes
Sakaba, Hiroyuki; Tonosaki, Hiroki; Isozaki, Kazuyoshi; Kwon, Eunsang; Organometallics 34 (2015) 1029–; doi:10.1021/om500996r

data_4085597
_publ_section_title
;
 \h3-Silaallyl/Alkenylsilyl Molybdenum Complex: Synthesis, Structure, and
 Reactivity toward Primary Amines To Form Mo--N--Si Three-Membered Cyclic
 Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1029
_journal_paper_doi               10.1021/om500996r
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C27 H33 Mo N O2 Si'
_chemical_formula_sum            'C27 H33 Mo N O2 Si'
_chemical_formula_weight         527.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.580(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.170(3)
_cell_length_b                   14.916(5)
_cell_length_c                   19.000(7)
_cell_measurement_reflns_used    6612
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.31
_cell_volume                     2596.2(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36759
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         3.315
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5905
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0497P)^2^+4.7223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                5512
_reflns_number_total             5905
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500996r_si_002.cif
_cod_data_source_block           complex5b
_cod_depositor_comments
'Adding full bibliography for 4085595--4085597.cif.'
_cod_original_cell_volume        2596.3(17)
_cod_database_code               4085597