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_4132087
_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 H53 N6 Ni2 O2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C41 H57 N6 Ni2 O2.5'
_chemical_formula_weight         791.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.291(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3032(5)
_cell_length_b                   14.2469(4)
_cell_length_c                   17.1692(5)
_cell_measurement_reflns_used    53345
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.802
_cell_measurement_theta_min      1.920
_cell_volume                     3887.6(2)
_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 0.991
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53345
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.802
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.8761
_exptl_absorpt_correction_T_min  0.5050
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8239
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0427P)^2^+1.3077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6848
_reflns_number_total             8239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01468_si_002.cif
_cod_data_source_block           3-pd135b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C41 H57 N6 Ni2 O2.50'
_cod_database_code               4132087
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.642
_shelx_estimated_absorpt_t_max   0.815
_shelx_res_checksum              82302
_shelx_hkl_checksum              36464