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_1566616
_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         'C83 H103 N7 Ni5 Si4'
_chemical_formula_sum            'C83 H103 N7 Ni5 Si4'
_chemical_formula_weight         1604.62
_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                89.5959(19)
_cell_angle_beta                 79.412(2)
_cell_angle_gamma                63.052(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9645(4)
_cell_length_b                   14.7686(3)
_cell_length_c                   24.4091(5)
_cell_measurement_reflns_used    28076
_cell_measurement_temperature    113
_cell_measurement_theta_max      31.28
_cell_measurement_theta_min      1.96
_cell_volume                     4394.3(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.898
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            83661
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.204
_diffrn_reflns_theta_min         1.678
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.882
_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            darkred
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1692.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     886
_refine_ls_number_reflns         25607
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0707P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15666
_reflns_number_total             25607
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1sc06935g2.cif
_cod_data_source_block           Ni5(CNtBu)5(NtBu)(CCNtBu)(SiPh2)4
_cod_database_code               1566616
_shelx_res_checksum              97862
_shelx_hkl_checksum              76096
_shelx_fab_checksum              48952