Catalytic Four-Electron Reduction of O2 via Rate-Determining Proton-Coupled Electron Transfer to a Dinuclear Cobalt-μ-1,2-peroxo Complex
Shunichi Fukuzumi; Sukanta Mandal; Kentaro Mase; Kei Ohkubo; Hyejin Park; Jordi Benet-Buchholz; Wonwoo Nam; Antoni Llobet; Journal of the American Chemical Society 134 (2012) 9906–9909; doi:10.1021/ja303674n

data_4118102
_publ_section_title
;
 Catalytic Four-Electron Reduction of O2 via Rate-Determining
 Proton-Coupled Electron Transfer to a Dinuclear Cobalt-\m-1,2-peroxo
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9906
_journal_page_last               9909
_journal_paper_doi               10.1021/ja303674n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C45 H41 Co2 F12 N10 O13 P S2'
_chemical_formula_weight         1370.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.390(2)
_cell_angle_beta                 72.006(2)
_cell_angle_gamma                61.058(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0028(6)
_cell_length_b                   14.0551(6)
_cell_length_c                   16.0751(7)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.23
_cell_measurement_theta_min      2.43
_cell_volume                     2628.1(2)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55453
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         33.36
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       plate
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         19116
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+2.9037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2368
_reflns_number_gt                13635
_reflns_number_total             19116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303674n_si_002_2.cif
_cod_data_source_block           coclb_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4118102