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_4128492
_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         'C46 H90 As Li N7 Ni Si2'
_chemical_formula_sum            'C46 H90 As Li N7 Ni Si2'
_chemical_formula_weight         937.99
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                91.496(3)
_cell_angle_beta                 102.225(2)
_cell_angle_gamma                103.698(3)
_cell_formula_units_Z            4
_cell_length_a                   15.7427(4)
_cell_length_b                   18.0180(6)
_cell_length_c                   20.4069(6)
_cell_measurement_reflns_used    13064
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5410
_cell_measurement_theta_min      2.4910
_cell_volume                     5478.5(3)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         2.532
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80965
_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    1.137
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         20683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15558
_reflns_number_total             20683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00159_si_002.cif
_cod_data_source_block           compound_12
_cod_database_code               4128492
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              68959
_shelx_hkl_checksum              82566