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_4132086
_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 -, C28 H40 K O8 +, 3(C4 H8 O)'
_chemical_formula_sum            'C79 H117 K N6 Ni2 O13'
_chemical_formula_weight         1515.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2912(2)
_cell_length_b                   25.8683(4)
_cell_length_c                   27.1074(4)
_cell_measurement_reflns_used    65467
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.722
_cell_measurement_theta_min      1.502
_cell_volume                     7917.6(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-2016 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65467
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         1.502
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.8007
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7668
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+7.3377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6102
_reflns_number_total             7668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01468_si_002.cif
_cod_data_source_block           2b-pd212c
_cod_database_code               4132086
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.756
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              66325
_shelx_hkl_checksum              55735