Metalation-Induced Denitrogenative Reductive Coupling of Isocyanides on a Silylene-Bridged Nickel Cluster
Shimamoto, Kento; Sunada, Yusuke; Chemical Science  (2022) –; doi:10.1039/D1SC06935G

data_1566615
_publ_section_title
;
 Metalation-Induced Denitrogenative Reductive Coupling of Isocyanides on a
 Silylene-Bridged Nickel Cluster
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06935G
_journal_year                    2022
_chemical_formula_moiety         'C34 H29 N2 Si2'
_chemical_formula_sum            'C34 H29 N2 Si2'
_chemical_formula_weight         521.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                77.219(5)
_cell_angle_beta                 79.312(6)
_cell_angle_gamma                79.801(6)
_cell_formula_units_Z            2
_cell_length_a                   10.310(3)
_cell_length_b                   12.326(3)
_cell_length_c                   12.941(3)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    100
_cell_measurement_theta_max      15.49
_cell_measurement_theta_min      1.65
_cell_volume                     1560.0(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41260
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45326
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        14.333
_diffrn_reflns_theta_max         15.500
_diffrn_reflns_theta_min         1.232
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             550.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7039
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.9661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6260
_reflns_number_total             7039
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1sc06935g2.cif
_cod_data_source_block           disilylketenimine
_cod_original_cell_volume        1560.0(6)
_cod_database_code               1566615
_shelx_res_checksum              36448
_shelx_hkl_checksum              53255