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_4085203
_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         'C44.68 H47.03 Cl0.33 N4 Ni, C6 H6'
_chemical_formula_sum            'C50.17 H53.01 Cl0.33 N4 Ni'
_chemical_formula_weight         782.43
_chemical_name_systematic
; 
? 
;
_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   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                103.115(4)
_cell_angle_beta                 98.614(4)
_cell_angle_gamma                103.025(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6588(7)
_cell_length_b                   15.3314(14)
_cell_length_c                   16.5973(15)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.49
_cell_volume                     2043.2(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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  cd48ksa
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         2.470
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.98391
_exptl_absorpt_correction_T_min  0.93881
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             831
_exptl_crystal_id                cd48ksa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2, 1, -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         7526
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0187P)^2^+1.6686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6398
_reflns_number_total             7526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5007177_si_002.cif
_cod_data_source_block           cd48ksa_2
_cod_depositor_comments
'Adding full bibliography for 4085202--4085205.cif.'
_cod_database_code               4085203
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2014-3
_shelx_res_checksum              73215
_shelx_hkl_checksum              15316