#------------------------------------------------------------------------------
#$Date: 2017-04-08 04:28:15 +0300 (Sat, 08 Apr 2017) $
#$Revision: 195271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/56/1545698.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1545698
loop_
_publ_author_name
'Nguyen, Andy Ich'
'Wang, Jianing'
'Levine, Daniel S.'
'Ziegler, Micah S.'
'Tilley, T. Don'
_publ_section_title
;
 Synthetic Control and Empirical Prediction of Redox Potentials for Co4O4
 Cubanes over a 1.4 V Range: Implications for Catalyst Design and
 Evaluation of High-Valent Intermediates in Water Oxidation
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC00627F
_journal_year                    2017
_chemical_formula_moiety         'C28 H20 Co4 F12 N4 O12'
_chemical_formula_sum            'C28 H20 Co4 F12 N4 O12'
_chemical_formula_weight         1068.20
_chemical_name_common            ain834
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   22.0726(4)
_cell_length_b                   22.0726(4)
_cell_length_c                   22.0726(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.26
_cell_volume                     10753.8(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.461
_diffrn_reflns_theta_min         2.260
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
; 
 Flack x determined using 811 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0162P)²+16.0965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1803
_reflns_number_total             1847
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc00627f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        10753.8(6)
_cod_database_code               1545698
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.829
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.62519(15) 0.34730(14) 0.21395(14) 0.0197(7) Uani 1 1 d . . . . .
C2 C 0.62433(18) 0.27914(16) 0.19838(17) 0.0314(8) Uani 1 1 d . . . . .
C3 C 0.46522(16) 0.40025(16) 0.24937(17) 0.0263(7) Uani 1 1 d . . . . .
H3 H 0.4876 0.3759 0.2218 0.032 Uiso 1 1 calc R U . . .
N1 N 0.49551(12) 0.43749(12) 0.28726(12) 0.0184(5) Uani 1 1 d . . . . .
O1 O 0.66742(9) 0.45306(9) 0.27925(9) 0.0165(4) Uani 1 1 d . . . . .
O2 O 0.59287(10) 0.36039(10) 0.25880(10) 0.0203(5) Uani 1 1 d . . . . .
O3 O 0.65825(10) 0.37865(9) 0.18027(10) 0.0199(5) Uani 1 1 d . . . . .
Co1 Co 0.58351(2) 0.44564(2) 0.28342(2) 0.01603(11) Uani 1 1 d . . . . .
F1 F 0.6456(5) 0.2658(5) 0.1469(5) 0.059(3) Uani 0.61(3) 1 d . . P A 1
F2 F 0.6566(4) 0.2492(3) 0.2418(4) 0.049(2) Uani 0.61(3) 1 d . . P A 1
F3 F 0.5696(3) 0.2548(5) 0.2049(5) 0.052(3) Uani 0.61(3) 1 d . . P A 1
F1A F 0.6750(9) 0.2535(7) 0.204(2) 0.114(11) Uani 0.39(3) 1 d . . P A 2
F3A F 0.6138(19) 0.2719(10) 0.1381(9) 0.114(9) Uani 0.39(3) 1 d . . P A 2
F2A F 0.5811(12) 0.2508(8) 0.2195(12) 0.108(7) Uani 0.39(3) 1 d . U P A 2
C5 C 0.37048(17) 0.43170(18) 0.28907(19) 0.0356(9) Uani 1 1 d . . . . .
H5 H 0.3275 0.4298 0.2896 0.043 Uiso 1 1 calc R U . . .
C6 C 0.40099(16) 0.46990(18) 0.32811(18) 0.0324(8) Uani 1 1 d . . . . .
H6 H 0.3795 0.4947 0.3560 0.039 Uiso 1 1 calc R U . . .
C7 C 0.46340(15) 0.47127(16) 0.32575(15) 0.0256(7) Uani 1 1 d . . . . .
H7 H 0.4844 0.4974 0.3527 0.031 Uiso 1 1 calc R U . . .
C4 C 0.40319(18) 0.39643(18) 0.24929(18) 0.0338(9) Uani 1 1 d . . . . .
H4 H 0.3830 0.3698 0.2221 0.041 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 C1 O2 132.4(3) . .
O3 C1 C2 114.5(3) . .
O2 C1 C2 113.2(3) . .
F2A C2 F1A 114.8(13) . .
F1 C2 F3 109.9(7) . .
F2A C2 F3A 100.3(13) . .
F1A C2 F3A 101.5(11) . .
F1 C2 F2 109.0(6) . .
F3 C2 F2 101.6(6) . .
F2A C2 C1 114.9(8) . .
F1A C2 C1 113.8(6) . .
F1 C2 C1 115.0(5) . .
F3 C2 C1 112.4(5) . .
F3A C2 C1 109.5(10) . .
F2 C2 C1 108.0(4) . .
N1 C3 C4 122.2(3) . .
N1 C3 H3 118.9 . .
C4 C3 H3 118.9 . .
C7 N1 C3 118.1(3) . .
C7 N1 Co1 120.3(2) . .
C3 N1 Co1 121.5(2) . .
Co1 O1 Co1 93.34(9) 42_545 .
Co1 O1 Co1 98.16(9) 42_545 19_654
Co1 O1 Co1 92.98(9) . 19_654
C1 O2 Co1 119.8(2) . .
C1 O3 Co1 119.6(2) . 19_654
O1 Co1 O1 86.42(9) 19_654 .
O1 Co1 O1 81.82(9) 19_654 42_545
O1 Co1 O1 86.10(9) . 42_545
O1 Co1 N1 93.32(10) 19_654 .
O1 Co1 N1 179.58(11) . .
O1 Co1 N1 94.19(10) 42_545 .
O1 Co1 O2 91.31(10) 19_654 .
O1 Co1 O2 88.06(9) . .
O1 Co1 O2 171.24(9) 42_545 .
N1 Co1 O2 91.62(10) . .
O1 Co1 O3 171.24(9) 19_654 42_545
O1 Co1 O3 88.41(9) . 42_545
O1 Co1 O3 90.79(9) 42_545 42_545
N1 Co1 O3 91.90(10) . 42_545
O2 Co1 O3 95.57(9) . 42_545
O1 Co1 Co1 87.53(6) 19_654 42_545
O1 Co1 Co1 43.28(6) . 42_545
O1 Co1 Co1 43.40(6) 42_545 42_545
N1 Co1 Co1 137.05(8) . 42_545
O2 Co1 Co1 131.32(7) . 42_545
O3 Co1 Co1 83.86(7) 42_545 42_545
O1 Co1 Co1 43.38(6) 19_654 19_654
O1 Co1 Co1 43.63(7) . 19_654
O1 Co1 Co1 87.31(6) 42_545 19_654
N1 Co1 Co1 136.07(8) . 19_654
O2 Co1 Co1 83.95(7) . 19_654
O3 Co1 Co1 132.02(7) 42_545 19_654
Co1 Co1 Co1 62.733(18) 42_545 19_654
O1 Co1 Co1 41.07(6) 19_654 28_455
O1 Co1 Co1 84.21(6) . 28_455
O1 Co1 Co1 40.77(6) 42_545 28_455
N1 Co1 Co1 95.81(7) . 28_455
O2 Co1 Co1 132.03(7) . 28_455
O3 Co1 Co1 131.29(7) 42_545 28_455
Co1 Co1 Co1 58.634(9) 42_545 28_455
Co1 Co1 Co1 58.633(9) 19_654 28_455
C4 C5 C6 119.1(3) . .
C4 C5 H5 120.4 . .
C6 C5 H5 120.4 . .
C7 C6 C5 118.5(4) . .
C7 C6 H6 120.8 . .
C5 C6 H6 120.8 . .
N1 C7 C6 122.9(3) . .
N1 C7 H7 118.6 . .
C6 C7 H7 118.6 . .
C3 C4 C5 119.2(4) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O3 1.251(4) .
C1 O2 1.254(4) .
C1 C2 1.543(5) .
C2 F2A 1.233(16) .
C2 F1A 1.260(13) .
C2 F1 1.264(10) .
C2 F3 1.329(9) .
C2 F3A 1.36(2) .
C2 F2 1.364(7) .
C3 N1 1.350(4) .
C3 C4 1.372(5) .
C3 H3 0.9500 .
N1 C7 1.334(4) .
N1 Co1 1.952(3) .
O1 Co1 1.858(2) 42_545
O1 Co1 1.862(2) .
O1 Co1 1.869(2) 19_654
O2 Co1 1.969(2) .
O3 Co1 1.979(2) 19_654
Co1 O1 1.858(2) 19_654
Co1 O1 1.869(2) 42_545
Co1 O3 1.979(2) 42_545
Co1 Co1 2.7059(7) 42_545
Co1 Co1 2.7059(7) 19_654
Co1 Co1 2.8169(8) 28_455
C5 C4 1.378(6) .
C5 C6 1.381(6) .
C5 H5 0.9500 .
C6 C7 1.379(5) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C4 H4 0.9500 .
