Insertion of Isonitriles into the M-C Bonds of Group 4 Dialkyl Complexes.
Chen, Jiawei; Yassin, Nadine; Gunasekara, Thilina; Norton, Jack R.; Rauch, Michael; Journal of the American Chemical Society 140 (2018) 8980–8989; doi:10.1021/jacs.8b05377

data_4132654
_publ_section_title
;
 Insertion of Isonitriles into the M-C Bonds of Group 4 Dialkyl Complexes.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8980
_journal_page_last               8989
_journal_paper_doi               10.1021/jacs.8b05377
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C27 H51 N3 Si Ti'
_chemical_formula_weight         493.69
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.740(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.297(4)
_cell_length_b                   15.025(5)
_cell_length_c                   19.462(7)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.43
_cell_volume                     2948.0(18)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.726
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4481
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.910
_exptl_crystal_size_mid          0.840
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.1811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5359
_reflns_number_total             6022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05377_si_001.cif
_cod_data_source_block           cytis10
_cod_original_cell_volume        2948.2(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132654
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              58656
_shelx_hkl_checksum              4898