Nickel(II) Pincer Carbene Complexes: Oxidative Addition of an Aryl C‒H Bond to Form a Ni(II) Hydride
Matson, Ellen M.; Espinosa Martinez, Gabriel; Ibrahim, Abdulrahman D.; Jackson, Bailey J.; Bertke, Jeffrey A.; Fout, Alison R.; Organometallics 34 (2015) 399–; doi:10.1021/om5007177

data_4085205
_publ_contact_author
; 
Alison R. Fout 
University of Illinois 
A406 CLSL, Box 54-6 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Nickel(II) Pincer Carbene Complexes: Oxidative Addition of an Aryl C--H
 Bond to Form a Ni(II) Hydride
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              399
_journal_paper_doi               10.1021/om5007177
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C44 H46 N4 Ni'
_chemical_formula_sum            'C51 H61 N4 Ni O'
_chemical_formula_weight         804.74
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   21.7945(18)
_cell_length_b                   21.7945(18)
_cell_length_c                   41.104(4)
_cell_measurement_reflns_used    8777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.37
_cell_volume                     16909(3)
_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
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd40jsa-sr
_diffrn_reflns_av_R_equivalents  0.1611
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            71783
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.431
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.97623
_exptl_absorpt_correction_T_min  0.90984
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7758
_exptl_crystal_id                cd40jsa-sr
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) 
with the (4, -4, 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.052
_platon_squeeze_details
; 
There were a total of 63 electrons squeezed out per asymmetric 
unit.  This corresponds to a single THF molecule and a half 
hexane in each asymmetric unit. 
;
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         6851
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0604P)^2^+10.8816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4547
_reflns_number_total             6851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5007177_si_002.cif
_cod_data_source_block           cd40jsa-sr_4
_cod_depositor_comments
'Adding full bibliography for 4085202--4085205.cif.'
_cod_original_cell_volume        16908(3)
_cod_database_code               4085205
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2014-3
_shelx_res_checksum              57612
_shelx_hkl_checksum              1486