Water Oxidation Catalysis by Co(II) Impurities in Co(III)4O4 Cubanes.
Ullman, Andrew M.; Liu, Yi; Huynh, Michael; Bediako, D. Kwabena; Wang, Hongsen; Anderson, Bryce L.; Powers, David C.; Breen, John J.; Abruña, Héctor D; Nocera, Daniel G.; Journal of the American Chemical Society  (2014) 141204115603004–; doi:10.1021/ja5110393

data_4123020
_publ_section_title
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 Water Oxidation Catalysis by Co(II) Impurities in Co(III)4O4 Cubanes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141204115603004
_journal_paper_doi               10.1021/ja5110393
_journal_year                    2014
_chemical_formula_moiety         'C28 H32 Co4 N4 O12, F6 P, C2 H3 N'
_chemical_formula_sum            'C30 H35 Co4 F6 N5 O12 P'
_chemical_formula_weight         1044.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2399(15)
_cell_length_b                   16.7691(13)
_cell_length_c                   24.620(2)
_cell_measurement_reflns_used    9231
_cell_measurement_temperature    15
_cell_measurement_theta_max      16.69
_cell_measurement_theta_min      2.37
_cell_volume                     7943.3(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Si 1 1 1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70744
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.968
_diffrn_reflns_theta_min         0.962
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.7938.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8092
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0663P)^2^+3.3313P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6658
_reflns_number_total             8092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5110393_si_002.cif
_cod_data_source_block           Co4O4OAc4py4PF6
_cod_depositor_comments
;

2020-09-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         553.77
_cod_original_formula_moiety
'0.53(C28 H32 Co4 N4 O12), 0.53(F6 P), 0.53(C2 H3 N)'
_cod_original_formula_units_Z            15
_cod_original_formula_sum        'C16 H18.67 Co2.13 F3.20 N2.67 O6.40 P0.53'
_cod_database_code               4123020
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C012(H012), C013(H013), C016(H016), C017(H017), C018(H018),
 C019(H019), C01A(H01A), C01B(H01B), C01D(H01F), C01E(H01G), C01F(H01H),
 C01G(H01I), C01H(H01J)
3.b Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C01C(H01C,H01D,H01E), C01I(H01K,H01L,H01M), C01L(H01Q,
 H01R,H01S), C01M(H01N,H01O,H01P)
;
_shelx_res_checksum              38809
_shelx_hkl_checksum              20261