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_4134547
_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
'C59 H63 N6 Na Ni2 O2, 1.75(C4 H8 O), 0.25(C5 H12)'
_chemical_formula_sum            'C67.25 H80 N6 Na Ni2 O3.75'
_chemical_formula_weight         1172.78
_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-2014/7
_cell_angle_alpha                112.663(4)
_cell_angle_beta                 92.988(4)
_cell_angle_gamma                99.314(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7288(7)
_cell_length_b                   15.5000(7)
_cell_length_c                   17.7274(9)
_cell_measurement_reflns_used    41104
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.874
_cell_measurement_theta_min      1.452
_cell_volume                     3159.7(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41104
_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         26.874
_diffrn_reflns_theta_min         1.452
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9144
_exptl_absorpt_correction_T_min  0.7802
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1245
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         13405
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8722
_reflns_number_total             13405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00758_si_002.cif
_cod_data_source_block           3Na-pd126
_cod_database_code               4134547
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              32117
_shelx_hkl_checksum              24551