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_1566614
_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         'C66 H72 N4 Ni Si4'
_chemical_formula_sum            'C66 H72 N4 Ni Si4'
_chemical_formula_weight         1092.36
_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                80.502(2)
_cell_angle_beta                 78.053(3)
_cell_angle_gamma                71.215(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7807(4)
_cell_length_b                   11.8079(3)
_cell_length_c                   22.9033(7)
_cell_measurement_reflns_used    15654
_cell_measurement_temperature    113
_cell_measurement_theta_max      31.21
_cell_measurement_theta_min      1.86
_cell_volume                     2934.25(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28326
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.246
_diffrn_reflns_theta_min         1.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     676
_refine_ls_number_reflns         15917
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0679P)^2^+1.6180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11734
_reflns_number_total             15917
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1sc06935g2.cif
_cod_data_source_block           Ni(NHC)2(SI4Ph8)
_cod_database_code               1566614
_shelx_res_checksum              50877
_shelx_hkl_checksum              11559