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_4134546
_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
'C55 H53 N6 Na Ni2 O, 0.875(C4 H8 O), 0.125(C4 H10 O)'
_chemical_formula_sum            'C59 H61.25 N6 Na Ni2 O2'
_chemical_formula_weight         1026.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                80.688(2)
_cell_angle_beta                 82.043(2)
_cell_angle_gamma                81.867(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2900(3)
_cell_length_b                   18.5010(4)
_cell_length_c                   19.5019(5)
_cell_measurement_reflns_used    70438
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.959
_cell_measurement_theta_min      1.432
_cell_volume                     5001.4(2)
_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-2017 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70438
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.959
_diffrn_reflns_theta_min         1.432
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.7360
_exptl_absorpt_correction_T_min  0.5170
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             2161
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.490
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         21215
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+3.6144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17846
_reflns_number_total             21215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00758_si_002.cif
_cod_data_source_block           2Na-pd126
_cod_database_code               4134546
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.842
_shelx_res_checksum              59765
_shelx_hkl_checksum              31399