Accessing Pincer Bis(carbene) Ni(IV) Complexes from Ni(II) via Halogen and Halogen Surrogates.
Martinez, Gabriel Espinosa; Ocampo, Cristian; Park, Yun Ji; Fout, Alison R.; Journal of the American Chemical Society 138 (2016) 4290–4293; doi:10.1021/jacs.5b12827

data_4130025
_publ_section_title
;
 Accessing Pincer Bis(carbene) Ni(IV) Complexes from Ni(II) via Halogen
 and Halogen Surrogates.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4290
_journal_page_last               4293
_journal_paper_doi               10.1021/jacs.5b12827
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C44 H45 Br N4 Ni'
_chemical_formula_sum            'C44 H45 Br N4 Ni'
_chemical_formula_weight         768.46
_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_date             2015-11-30
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) 
;
_cell_angle_alpha                111.4611(18)
_cell_angle_beta                 101.546(2)
_cell_angle_gamma                97.071(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6747(4)
_cell_length_b                   13.9513(7)
_cell_length_c                   16.8043(8)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.47
_cell_volume                     1810.91(15)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2014-4 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd47x
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.164
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  0.9369
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014) was used for absorption correction. 
wR2(int) was 0.1237 before and 0.0620 after correction. 
The Ratio of minimum to maximum transmission is 0.6661. 
The \l/2 correction factor is 0.00150. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             800
_exptl_crystal_id                cd47x
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1, 1, 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+2.1204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7131
_reflns_number_total             8022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12827_si_002.cif
_cod_data_source_block           cd47xsa
_cod_database_code               4130025
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.609
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C27(H27), C30(H30), C39(H39), C42(H42) 
2.b Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C15(H15), 
 C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C35(H35), 
 C36(H36), C37(H37) 
2.c Idealised Me refined as rotating group: 
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), 
 C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), 
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C) 
;
_olex2_submission_special_instructions 'No special instructions were received'