Versatile Tautomerization of EH<sub>2</sub>-Substituted Silylenes (E = N, P, As) in the Coordination Sphere of Nickel.
Hadlington, Terrance J.; Szilvási, Tibor; Driess, Matthias; Journal of the American Chemical Society 141 (2019) 3304–3314; doi:10.1021/jacs.9b00159

data_4128495
_publ_section_title
;
 Versatile Tautomerization of EH<sub>2</sub>-Substituted Silylenes (E = N,
 P, As) in the Coordination Sphere of Nickel.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3304
_journal_page_last               3314
_journal_paper_doi               10.1021/jacs.9b00159
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C58 H110 N8 Ni Si4'
_chemical_formula_sum            'C58 H110 N8 Ni Si4'
_chemical_formula_weight         1090.60
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 101.5110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5510(2)
_cell_length_b                   16.6693(2)
_cell_length_c                   26.9463(3)
_cell_measurement_reflns_used    12193
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5410
_cell_measurement_theta_min      3.0950
_cell_volume                     6404.50(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25490
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.993
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         12073
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+5.4352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10397
_reflns_number_total             12073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00159_si_002.cif
_cod_data_source_block           SiNi_Ph3BNH2Li
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4128495
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              15684
_shelx_hkl_checksum              78167