Synthesis, characterization and C‒H amination reactivity of nickel iminyl complexes
Dong, Yuyang; Lukens, James T.; Clarke, Ryan M.; Zheng, Shao-Liang; Lancaster, Kyle M.; Betley, Theodore A.; Chemical Science 11 (2020) 1260–1268; doi:10.1039/C9SC04879K

data_1556863
_publ_section_title
;
 Synthesis, characterization and C--H amination reactivity of nickel
 iminyl complexes
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1260
_journal_page_last               1268
_journal_paper_doi               10.1039/C9SC04879K
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C45 H49 F5 N3 Ni'
_chemical_formula_weight         785.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1294(9)
_cell_length_b                   16.6197(8)
_cell_length_c                   15.8282(8)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.626
_cell_measurement_theta_min      2.791
_cell_volume                     3716.9(4)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CMOS area detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41286
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.214
_diffrn_reflns_theta_max         67.214
_diffrn_reflns_theta_min         3.856
_diffrn_source                   'I/mS microfocus tube'
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       needle
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         6222
_refine_ls_number_restraints     1015
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+12.3867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                3085
_reflns_number_total             6222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04879k2.cif
_cod_data_source_block           LNiNAd
_cod_depositor_comments
;Adding full bibliography for 1556860--1556864.cif.

 Adding full bibliography for 1556860--1556864.cif.
;
_cod_database_code               1556863
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              73740