Reductive O<sub>2</sub> Binding at a Dihydride Complex Leading to Redox Interconvertible μ-1,2-Peroxo and μ-1,2-Superoxo Dinickel(II) Intermediates.
Duan, Peng-Cheng; Manz, Dennis-Helmut; Dechert, Sebastian; Demeshko, Serhiy; Meyer, Franc; Journal of the American Chemical Society 140 (2018) 4929–4939; doi:10.1021/jacs.8b01468

data_4132088
_publ_section_title
;
 Reductive O<sub>2</sub> Binding at a Dihydride Complex Leading to Redox
 Interconvertible \m-1,2-Peroxo and \m-1,2-Superoxo Dinickel(II)
 Intermediates.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4929
_journal_page_last               4939
_journal_paper_doi               10.1021/jacs.8b01468
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C39 H54 N6 Ni2 O'
_chemical_formula_sum            'C39 H54 N6 Ni2 O'
_chemical_formula_weight         740.30
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.320(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5261(8)
_cell_length_b                   16.4420(7)
_cell_length_c                   13.6294(6)
_cell_measurement_reflns_used    25752
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.744
_cell_measurement_theta_min      1.759
_cell_volume                     3654.7(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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25752
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.744
_diffrn_reflns_theta_min         1.759
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  0.7695
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0475P)^2^+1.1116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3483
_reflns_number_total             3872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01468_si_002.cif
_cod_data_source_block           4-dm273
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4132088
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.628
_shelx_estimated_absorpt_t_max   0.754
_shelx_res_checksum              21299
_shelx_hkl_checksum              53993