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_4134549
_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         'C51 H43 N6 Ni2 -, 0.5(C12 H24 Na O3 +)'
_chemical_formula_sum            'C57 H55 N6 Na0.5 Ni2 O1.5'
_chemical_formula_weight         976.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.0510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7413(5)
_cell_length_b                   10.6411(2)
_cell_length_c                   20.9606(4)
_cell_measurement_reflns_used    71859
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.786
_cell_measurement_theta_min      1.544
_cell_volume                     5882.98(19)
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71859
_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         25.786
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9215
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             2050
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         11100
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0423P)^2^+2.1589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8846
_reflns_number_total             11100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00758_si_002.cif
_cod_data_source_block           6Na-hs281b_sq
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C57 H55 N6 Na0.50 Ni2 O1.50'
_cod_database_code               4134549
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.853
_shelx_res_checksum              82736
_shelx_hkl_checksum              71379
_shelx_fab_checksum              68030