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_1566617
_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         'C73 H85 N5 Ni2 Si4'
_chemical_formula_sum            'C73 H85 N5 Ni2 Si4'
_chemical_formula_weight         1262.25
_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                97.750(7)
_cell_angle_beta                 95.438(7)
_cell_angle_gamma                102.855(7)
_cell_formula_units_Z            4
_cell_length_a                   14.392(12)
_cell_length_b                   22.272(19)
_cell_length_c                   22.510(19)
_cell_measurement_reflns_used    2309
_cell_measurement_temperature    100
_cell_measurement_theta_max      17.82
_cell_measurement_theta_min      4.31
_cell_volume                     6912(10)
_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, 2018)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.773
_diffrn_measurement_device_type  'Rigaku R-AXIS IV'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41500
_diffrn_reflns_av_R_equivalents  0.1469
_diffrn_reflns_av_unetI/netI     0.1226
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.773
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            282646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        14.418
_diffrn_reflns_theta_max         22.231
_diffrn_reflns_theta_min         0.949
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            lightbrown
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680.00
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.36
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1542
_refine_ls_number_reflns         67846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1753
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1152P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29903
_reflns_number_total             67846
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1sc06935g2.cif
_cod_data_source_block           Ni2(SiPh2)4C(CNtBu)4(NtBu)
_cod_database_code               1566617
_shelx_res_checksum              42529
_shelx_hkl_checksum              32801