Ni(I)-X Complexes Bearing a Bulky α-Diimine Ligand: Synthesis, Structure, and Superior Catalytic Performance in the Hydrogen Isotope Exchange in Pharmaceuticals.
Zarate, Cayetana; Yang, Haifeng; Bezdek, Máté J; Hesk, David; Chirik, Paul J.; Journal of the American Chemical Society 141 (2019) 5034–5044; doi:10.1021/jacs.9b00939

data_4129045
_publ_section_title
;
 Ni(I)-X Complexes Bearing a Bulky \a-Diimine Ligand: Synthesis,
 Structure, and Superior Catalytic Performance in the Hydrogen Isotope
 Exchange in Pharmaceuticals.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5034
_journal_page_last               5044
_journal_paper_doi               10.1021/jacs.9b00939
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_sum            'C44 H72 Br2 N4 Ni2'
_chemical_formula_weight         934.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.3180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3155(4)
_cell_length_b                   12.3857(3)
_cell_length_c                   13.9317(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.16
_cell_measurement_theta_min      3.43
_cell_volume                     2226.27(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26427
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.161
_diffrn_reflns_theta_min         3.425
_exptl_absorpt_coefficient_mu    3.397
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3810 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8248
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0304P)^2^+0.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                8194
_reflns_number_total             8248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00939_si_002.cif
_cod_data_source_block           cz11
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4129045
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.599
_shelxl_version_number           2014-3
_shelx_res_checksum              75998
_shelx_hkl_checksum              29466