Unsymmetrical N-Aryl-1-(pyridin-2-yl)methanimine Ligands in Organonickel(II) Complexes: More Than a Blend of 2,2'-Bipyridine and N,N-Diaryl-α-diimines?
Biewer, Christian; Hamacher, Claudia; Kaiser, Andre; Vogt, Nicolas; Sandleben, Aaron; Chin, Mason T.; Yu, Siqi; Vicic, David A.; Klein, Axel; Inorganic chemistry 55 (2016) 12716–12727; doi:10.1021/acs.inorgchem.6b01874

data_4349043
_publ_section_title
;
 Unsymmetrical N-Aryl-1-(pyridin-2-yl)methanimine Ligands in
 Organonickel(II) Complexes: More Than a Blend of 2,2'-Bipyridine and
 N,N-Diaryl-\a-diimines?
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12716
_journal_page_last               12727
_journal_paper_doi               10.1021/acs.inorgchem.6b01874
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C22 H20 Br F3 N2 Ni'
_chemical_formula_sum            'C22 H20 Br F3 N2 Ni'
_chemical_formula_weight         508.02
_chemical_name_common            '[(2-CF3-PyMa)Ni(Mes)Br]'
_chemical_name_systematic        '[(2-CF3-PyMa)Ni(Mes)Br]'
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                82.802(6)
_cell_angle_beta                 68.130(6)
_cell_angle_gamma                78.740(7)
_cell_formula_units_Z            4
_cell_length_a                   11.7586(10)
_cell_length_b                   13.3830(11)
_cell_length_c                   15.4157(12)
_cell_measurement_reflns_used    33437
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.835
_cell_measurement_theta_min      1.554
_cell_volume                     2204.3(3)
_computing_cell_refinement       'X-AREA (STOE & Cie 2001)'
_computing_data_collection       'X-AREA (STOE & Cie 2001)'
_computing_data_reduction        'X-RED (STOE & Cie 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2132
_diffrn_reflns_av_unetI/netI     0.2522
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.835
_diffrn_reflns_theta_min         1.554
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.7574
_exptl_absorpt_correction_T_min  0.4792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001) 
was performed after optimizing the crystal shape 
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Octothorpe
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.745
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.745
_refine_ls_R_factor_all          0.2666
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2047
_reflns_number_total             9356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01874_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H40 Br2 F6 N4 Ni2'
_cod_original_formula_weight         1016.04
_cod_original_formula_moiety         'C44 H40 Br2 F6 N4 Ni2'
_cod_original_formula_units_Z            2
_cod_database_code               4349043
_shelx_shelxl_version_number     2014/7