Organometallic Nickel(III) Complexes Relevant to Cross-Coupling and Carbon-Heteroatom Bond Formation Reactions.
Zheng, Bo; Tang, Fengzhi; Luo, Jia; Schultz, Jason W.; Rath, Nigam P.; Mirica, Liviu M.; Journal of the American Chemical Society 136 (2014) 6499–6504; doi:10.1021/ja5024749

data_4121686
_publ_section_title
;
 Organometallic Nickel(III) Complexes Relevant to Cross-Coupling and
 Carbon-Heteroatom Bond Formation Reactions.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6499
_journal_page_last               6504
_journal_paper_doi               10.1021/ja5024749
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'2(C28 H36 Cl F N4 Ni), 2(F6 P), 0.5(C4 H8 O), 0.5(C4 H10 O)'
_chemical_formula_sum            'C60 H81 Cl2 F14 N8 Ni2 O P2'
_chemical_formula_weight         1446.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                75.795(16)
_cell_angle_beta                 77.796(11)
_cell_angle_gamma                89.143(11)
_cell_formula_units_Z            2
_cell_length_a                   11.7748(19)
_cell_length_b                   15.072(3)
_cell_length_c                   19.717(5)
_cell_measurement_reflns_used    1195
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.10
_cell_measurement_theta_min      2.45
_cell_volume                     3313.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2594
_diffrn_reflns_av_unetI/netI     0.4447
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32800
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.395
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2012/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1502
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         11463
_refine_ls_number_restraints     881
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.3185
_refine_ls_R_factor_gt           0.1014
_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^)+(0.1209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.3069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3450
_reflns_number_total             11463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5024749_si_002.cif
_cod_data_source_block           l12813
_cod_depositor_comments
'Adding full bibliography for 4121684--4121687.cif.'
_cod_database_code               4121686
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-3
_shelx_res_checksum              8277
_shelx_hkl_checksum              54192