Probing Edge Site Reactivity of Oxidic Cobalt Water Oxidation Catalysts.
Ullman, Andrew M.; Brodsky, Casey N.; Li, Nancy; Zheng, Shao-Liang; Nocera, Daniel G.; Journal of the American Chemical Society 138 (2016) 4229–; doi:10.1021/jacs.6b00762

data_4124943
_publ_section_title
;
 Probing Edge Site Reactivity of Oxidic Cobalt Water Oxidation Catalysts.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4229
_journal_paper_doi               10.1021/jacs.6b00762
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C16 H16 Co N3 O2, C16 H15 Co N3 O2, 2.5(F6 P), 1.88(O), H2 O, F1.38 P0.5, 1.62(F)'
_chemical_formula_sum            'C32 H33 Co2 F18 N6 O6.88 P3'
_chemical_formula_weight         1164.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8026(17)
_cell_length_b                   26.903(3)
_cell_length_c                   18.9027(19)
_cell_measurement_temperature    100(2)
_cell_volume                     8528.9(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            156742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.431
_exptl_absorpt_coefficient_mu    1.023
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       block
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0699P)^2^+29.5450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             8731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00762_si_003.cif
_cod_data_source_block           12216_a
_cod_depositor_comments
'Adding full bibliography for 4124943--4124944.cif.'
_cod_original_cell_volume        8529.0(15)
_cod_database_code               4124943
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2B} of O2, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H1SA,H1SB} of O1S
2. Restrained distances
 O1-H0AA = O2-H2B = O2-H2A = O3-H1AA = O4-H3AA
 0.84 with sigma of 0.02
 P3A-F3 \\sim P3-F1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(P3) = Uanis(P3A)
Uanis(F2C) = Uanis(F2D)
Uanis(F1C) = Uanis(F3)
Uanis(F3D) = Uanis(F3C)
Uanis(F10) = Uanis(F10A)
Uanis(F13) = Uanis(F13A)
Uanis(O2S) = Uanis(O3S)
4. Others
 Sof(F2D)=Sof(F3D)=Sof(F3)=1-FVAR(1)
 Sof(P3A)=0.5*(1-FVAR(2))
 Sof(P3)=0.5*FVAR(2)
 Sof(F1C)=Sof(F2C)=Sof(F3C)=FVAR(1)
 Sof(F7B)=Sof(F9A)=Sof(F8B)=1-FVAR(2)
 Sof(F9)=Sof(F7A)=Sof(F8A)=Sof(O0AA)=FVAR(2)
 Sof(F10A)=Sof(F13A)=1-FVAR(3)
 Sof(F10)=Sof(F13)=FVAR(3)
 Sof(O3S)=1-FVAR(4)
 Sof(O2S)=FVAR(4)
 Fixed Sof: O4T(0.5) P4A(0.5)
5.a Free rotating group:
 O1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2AA), C3A(H3A), C4A(H4A), C8A(H8A), C9A(H9A), C10A(H10A),
 C11A(H11A), C14A(H14A), C15A(H15A), C1B(H1B), C2B(H2BA), C3B(H3B), C4B(H4B),
 C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C14B(H14B), C15B(H15B)
5.c Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              29180
_shelx_hkl_checksum              3831
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 'Co2 Hydrogen Bonded Dimer PF6'
_olex2_submission_special_instructions 'No special instructions were received'