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_4128486
_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         'C37 H68 N6 Ni Si2'
_chemical_formula_sum            'C37 H68 N6 Ni Si2'
_chemical_formula_weight         711.86
_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                 113.769(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5126(4)
_cell_length_b                   11.6650(2)
_cell_length_c                   20.9368(4)
_cell_measurement_reflns_used    8524
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3310
_cell_measurement_theta_min      2.6010
_cell_volume                     4137.79(15)
_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 0.994
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16315
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.996
_diffrn_reflns_theta_min         2.697
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49575
_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            red
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0653P)^2^+1.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6888
_reflns_number_total             7811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00159_si_002.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        4137.78(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4128486
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              40894
_shelx_hkl_checksum              95491