#------------------------------------------------------------------------------
#$Date: 2018-09-26 06:29:44 +0300 (Wed, 26 Sep 2018) $
#$Revision: 211175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/01/8000142.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_8000142
loop_
_publ_author_name
'Mitsumoto, Kiyotaka'
'Koizumi, Satoshi'
'Shiga, Takuya'
'Nishikawa, Hiroyuki'
'Chi, Yun'
'Oshio, Hiroki'
_publ_section_title
;
 Alkoxo-bridged Cobalt(II) Cube and Its Radical Adduct
;
_journal_issue                   9
_journal_name_full               'Chemistry Letters'
_journal_page_first              1154
_journal_paper_doi               10.1246/cl.2007.1154
_journal_volume                  36
_journal_year                    2007
_chemical_formula_sum            'C32 H36 Co4 F24 N4 O12'
_chemical_formula_weight         1360.37
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.197(3)
_cell_length_b                   14.197(3)
_cell_length_c                   12.052(3)
_cell_measurement_reflns_used    1014
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.2275
_cell_measurement_theta_min      3.208
_cell_volume                     2429.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11464
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         265
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.6629
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(15)
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         1745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0190
_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/[σ²(Fo²)+(0.0340P)²+0.4290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                1709
_reflns_number_total             1745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-1154sup1.cif
_cod_data_source_block           '[Co4(heip)4(MeOH)4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2429.2(9)
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               8000142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H9 H 0.441(2) 0.258(2) 0.000(3) 0.062(11) Uiso 1 1 d . . .
Co1 Co 0.415826(19) 0.422964(19) 0.08552(3) 0.03254(12) Uani 1 1 d . . .
F1 F 0.11368(13) 0.52494(14) 0.1691(2) 0.1004(7) Uani 1 1 d . A .
F2 F 0.09284(14) 0.3874(2) 0.1148(3) 0.1421(12) Uani 1 1 d . A .
F3 F 0.0968(16) 0.442(2) 0.3045(13) 0.086(5) Uani 0.34(6) 1 d P A 1
F3' F 0.0800(8) 0.406(2) 0.272(3) 0.120(7) Uani 0.66(6) 1 d P A 2
F4 F 0.31776(12) 0.31628(12) 0.49657(18) 0.0719(5) Uani 1 1 d . A .
F5 F 0.42212(14) 0.23088(11) 0.41615(15) 0.0772(5) Uani 1 1 d . A .
F6 F 0.45845(12) 0.36529(13) 0.48337(12) 0.0692(5) Uani 1 1 d . A .
O1 O 0.27925(10) 0.44515(11) 0.11123(15) 0.0456(4) Uani 1 1 d . . .
O2 O 0.55865(10) 0.42543(10) 0.08332(13) 0.0320(3) Uani 1 1 d . . .
O3 O 0.40473(13) 0.27227(12) 0.04075(16) 0.0444(4) Uani 1 1 d . . .
N1 N 0.43699(13) 0.38138(13) 0.24705(15) 0.0371(4) Uani 1 1 d . . .
C1 C 0.13150(19) 0.4373(2) 0.1926(3) 0.0688(9) Uani 1 1 d . . .
C2 C 0.23738(16) 0.41882(16) 0.1994(2) 0.0476(6) Uani 1 1 d . A .
C3 C 0.27255(17) 0.38006(17) 0.2932(2) 0.0513(7) Uani 1 1 d . . .
H3 H 0.2285 0.3626 0.3489 0.062 Uiso 1 1 calc R A .
C4 C 0.36971(18) 0.36298(16) 0.3161(2) 0.0410(6) Uani 1 1 d . A .
C5 C 0.39153(19) 0.31902(18) 0.4283(2) 0.0531(6) Uani 1 1 d . . .
C6 C 0.53778(15) 0.37074(17) 0.27152(19) 0.0399(5) Uani 1 1 d . . .
H6A H 0.5478 0.3146 0.3188 0.048 Uiso 1 1 calc R . .
H6B H 0.5608 0.4268 0.3122 0.048 Uiso 1 1 calc R . .
C7 C 0.59211(16) 0.35985(16) 0.16334(19) 0.0379(5) Uani 1 1 d . . .
H7A H 0.6600 0.3707 0.1769 0.045 Uiso 1 1 calc R . .
H7B H 0.5843 0.2950 0.1348 0.045 Uiso 1 1 calc R . .
C8 C 0.3948(2) 0.19147(17) 0.1110(2) 0.0548(7) Uani 1 1 d . . .
H8A H 0.4471 0.1895 0.1640 0.082 Uiso 1 1 calc R . .
H8B H 0.3954 0.1342 0.0656 0.082 Uiso 1 1 calc R . .
H8C H 0.3350 0.1954 0.1514 0.082 Uiso 1 1 calc R . .
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
O1 Co1 O2 166.93(7) . .
O1 Co1 O2 101.47(7) . 3_565
O2 Co1 O2 85.33(7) . 3_565
O1 Co1 N1 92.31(7) . .
O2 Co1 N1 82.60(7) . .
O2 Co1 N1 164.52(7) 3_565 .
O1 Co1 O2 90.44(6) . 2_665
O2 Co1 O2 79.45(6) . 2_665
O2 Co1 O2 81.48(6) 3_565 2_665
N1 Co1 O2 105.68(7) . 2_665
O1 Co1 O3 96.99(7) . .
O2 Co1 O3 94.86(6) . .
O2 Co1 O3 83.46(7) 3_565 .
N1 Co1 O3 87.92(7) . .
O2 Co1 O3 164.27(7) 2_665 .
C2 O1 Co1 122.59(15) . .
C7 O2 Co1 108.29(12) . .
C7 O2 Co1 125.83(13) . 4_655
Co1 O2 Co1 97.97(7) . 4_655
C7 O2 Co1 125.58(13) . 2_665
Co1 O2 Co1 100.54(6) . 2_665
Co1 O2 Co1 93.23(6) 4_655 2_665
C8 O3 Co1 129.60(17) . .
C4 N1 C6 124.7(2) . .
C4 N1 Co1 124.02(17) . .
C6 N1 Co1 111.22(14) . .
F3' C1 F2 96.2(19) . .
F3' C1 F1 112.5(12) . .
F2 C1 F1 106.4(3) . .
F3' C1 F3 28.6(8) . .
F2 C1 F3 123.9(14) . .
F1 C1 F3 95.4(10) . .
F3' C1 C2 117.5(6) . .
F2 C1 C2 111.2(3) . .
F1 C1 C2 111.6(2) . .
F3 C1 C2 107.1(9) . .
O1 C2 C3 130.1(2) . .
O1 C2 C1 111.3(2) . .
C3 C2 C1 118.5(2) . .
C2 C3 C4 126.0(2) . .
N1 C4 C3 123.7(2) . .
N1 C4 C5 120.3(2) . .
C3 C4 C5 116.0(2) . .
F6 C5 F5 106.6(2) . .
F6 C5 F4 105.5(2) . .
F5 C5 F4 107.3(2) . .
F6 C5 C4 112.7(2) . .
F5 C5 C4 110.7(2) . .
F4 C5 C4 113.6(2) . .
N1 C6 C7 109.39(18) . .
O2 C7 C6 110.18(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 1.9887(16) .
Co1 O2 2.0281(15) .
Co1 O2 2.0561(16) 3_565
Co1 N1 2.0565(19) .
Co1 O2 2.1828(15) 2_665
Co1 O3 2.2120(18) .
F1 C1 1.301(4) .
F2 C1 1.297(4) .
F3 C1 1.437(14) .
F3' C1 1.283(10) .
F4 C5 1.333(3) .
F5 C5 1.332(3) .
F6 C5 1.332(3) .
O1 C2 1.274(3) .
O2 C7 1.422(3) .
O2 Co1 2.0561(16) 4_655
O2 Co1 2.1828(15) 2_665
O3 C8 1.432(3) .
N1 C4 1.294(3) .
N1 C6 1.469(3) .
C1 C2 1.528(4) .
C2 C3 1.353(4) .
C3 C4 1.428(4) .
C4 C5 1.521(4) .
C6 C7 1.523(3) .
