Direct metal-carbon bonding in symmetric bis(C-H) agostic Nickel(I) complexes
He, Weiying; Beattie, D. Dawson; Zhou, Hao; Bowes, Eric G.; Schafer, Laurel L.; Love, Jennifer; Kennepohl, Pierre; Chemical Science  (2021) –; doi:10.1039/D1SC03578A

data_1565129
_publ_section_title
;
 Direct metal-carbon bonding in symmetric bis(C-H) agostic Nickel(I)
 complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03578A
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C23 H27 N O'
_chemical_formula_sum            'C23 H27 N O'
_chemical_formula_weight         333.45
_chemical_name_systematic
'N-(1-(1,3,3-Trimethyl-2-oxabicyclo[2.2.2]octan-5-yl) benzophenone imine'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.736(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3648(10)
_cell_length_b                   8.5788(8)
_cell_length_c                   10.6319(9)
_cell_measurement_reflns_used    5644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.52
_cell_volume                     928.81(15)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, TWINABS V2012/1 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2018-3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Quest/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_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2935
_diffrn_reflns_point_group_measured_fraction_full 0.536
_diffrn_reflns_point_group_measured_fraction_max 0.536
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.294
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.745210
_exptl_absorpt_correction_T_min  0.593114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0173P)^2^+1.4074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                2474
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03578a2.cif
_cod_data_source_block           twin5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1565129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.985
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              47817
_shelx_hkl_checksum              72108