Competing H2 versus Intramolecular C-H Activation at a Dinuclear Nickel Complex via Metal-Metal Cooperative Oxidative Addition.
Stevens, Hendrik; Duan, Peng-Cheng; Dechert, Sebastian; Meyer, Franc; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00758

data_4134548
_publ_section_title
;
 Competing H2 versus Intramolecular C-H Activation at a Dinuclear Nickel
 Complex via Metal-Metal Cooperative Oxidative Addition.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00758
_journal_year                    2020
_chemical_formula_moiety         'C64 H63 K N6 Ni2 O2.50, C4 H8 O'
_chemical_formula_sum            'C68 H71 K N6 Ni2 O3.5'
_chemical_formula_weight         1184.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.1870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.8579(5)
_cell_length_b                   14.7943(3)
_cell_length_c                   25.3281(4)
_cell_measurement_reflns_used    71528
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.782
_cell_measurement_theta_min      1.325
_cell_volume                     11515.5(4)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            71528
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.782
_diffrn_reflns_theta_min         1.325
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7248
_exptl_absorpt_correction_T_min  0.6210
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.420
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10855
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0506P)^2^+16.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9203
_reflns_number_total             10855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00758_si_002.cif
_cod_data_source_block           5K-hs-jw12
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C68 H71 K N6 Ni2 O3.50'
_cod_database_code               4134548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.735
_shelx_res_checksum              31702
_shelx_hkl_checksum              93768