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_4085204
_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         'C48 H56 N4 Ni Si, O C4 H10'
_chemical_formula_sum            'C52 H66 N4 Ni O Si'
_chemical_formula_weight         849.88
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                106.393(6)
_cell_angle_beta                 110.407(6)
_cell_angle_gamma                93.967(7)
_cell_formula_units_Z            4
_cell_length_a                   15.1590(17)
_cell_length_b                   18.643(2)
_cell_length_c                   18.882(2)
_cell_measurement_reflns_used    7755
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.88
_cell_measurement_theta_min      2.23
_cell_volume                     4713.9(9)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm19ksa-sr
_diffrn_reflns_av_R_equivalents  0.1842
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            184757
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.656
_diffrn_reflns_theta_min         1.379
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.95961
_exptl_absorpt_correction_T_min  0.91393
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS v2012/1 (Bruker, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1824
_exptl_crystal_id                cm19ksa-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 (3 3 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.134
_platon_squeeze_details
; 
One diethylether molecule per asymmetric unit was squeezed out of the 
model.  The number of electrons squeezed from the model is consistant 
with this. 
;
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         17580
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11174
_reflns_number_total             17580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5007177_si_002.cif
_cod_data_source_block           cm19ksa-sr_3
_cod_depositor_comments
'Adding full bibliography for 4085202--4085205.cif.'
_cod_original_cell_volume        4714.0(9)
_cod_database_code               4085204
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2014-3
_shelx_res_checksum              44654
_shelx_hkl_checksum              71808