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_4118101
_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            'C44.49 H38 Co2 F19.52 N10 O8.48 P2.51 S1.5'
_chemical_formula_weight         1462.72
_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                104.883(2)
_cell_angle_beta                 91.731(2)
_cell_angle_gamma                98.113(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3022(7)
_cell_length_b                   14.7258(10)
_cell_length_c                   18.4590(12)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.28
_cell_volume                     2672.9(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Apex DUO Kappa 4-axis goniometer'
_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  'Quazar MX multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76815
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'Metal ceramics X-ray Tube MCMB 50-0.6b'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_type              'Microfocus Source E025 IuS'
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.96
_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            orange
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.895
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         14141
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0554P)^2^+3.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                12118
_reflns_number_total             14141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303674n_si_002_1.cif
_cod_data_source_block           mo_co4eqce_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_original_formula_sum        'C44.49 H38 Co2 F19.52 N10 O8.48 P2.51 S1.50'
_cod_database_code               4118101