#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:10:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179234 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/54/4315464.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_4315464
loop_
_publ_author_name
'Fabrice Riblet'
'Ghenadie Novitchi'
'Rosario Scopelliti'
'Lothar Helm'
'Aurelian Gulea'
'André E. Merbach'
_publ_contact_author_address
;Ecole polytechnique fédérale de Lausanne
Institut des sciences et ingénierie chimiques
EPFL SB ISIC LCIB
BCH 3108 (Bât. BCH)
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       lothar.helm@epfl.ch
_publ_contact_author_fax         '+41 21 693 98 55'
_publ_contact_author_name        'Lothar Helm'
_publ_contact_author_phone       '+41 21 693 98 75'
_publ_section_title
;
 Isomerization Mechanisms of Stereolabile tris- and bis-Bidentate
 Octahedral Cobalt(II) Complexes: X-ray Structure and Variable Temperature
 and Pressure NMR Kinetic Investigations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4194
_journal_page_last               4211
_journal_paper_doi               10.1021/ic902494j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H16 Co F12 N2 O4'
_chemical_formula_sum            'C22 H16 Co F12 N2 O4'
_chemical_formula_weight         659.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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            4
_cell_length_a                   9.6976(9)
_cell_length_b                   16.3685(15)
_cell_length_c                   15.9331(18)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.0182
_cell_measurement_theta_min      2.47825
_cell_volume                     2529.1(4)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction KM4/Sapphire CCD'
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7626
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                1069
_reflns_number_total             1235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902494j_si_001_3.cif
_cod_data_source_block           nov36a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315464
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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
Co1 Co 1.0000 0.83315(3) 0.7500 0.01698(18) Uani 1 4 d S . .
O1 O 1.14826(12) 0.83539(8) 0.65746(8) 0.0198(3) Uani 1 1 d . . .
F1 F 1.32486(14) 0.93461(9) 0.56084(9) 0.0483(4) Uani 1 1 d . . .
F2 F 1.23789(13) 0.87985(9) 0.45030(8) 0.0506(4) Uani 1 1 d . . .
F3 F 1.34630(12) 0.80585(9) 0.54052(9) 0.0481(4) Uani 1 1 d . . .
N1 N 1.0000 0.70209(19) 0.7500 0.0174(7) Uani 1 4 d S . .
N2 N 1.0000 0.96552(18) 0.7500 0.0190(7) Uani 1 4 d S . .
C1 C 1.12629(19) 0.85480(11) 0.58216(12) 0.0203(4) Uani 1 1 d . . .
C2 C 1.0000 0.86561(16) 0.54172(18) 0.0235(6) Uani 1 2 d S . .
H2 H 1.0000 0.8810 0.4842 0.028 Uiso 1 2 calc SR . .
C3 C 1.2587(2) 0.86857(14) 0.53218(13) 0.0316(5) Uani 1 1 d . . .
C4 C 1.0000 0.65897(15) 0.67813(17) 0.0194(6) Uani 1 2 d S . .
H4 H 1.0000 0.6880 0.6265 0.023 Uiso 1 2 calc SR . .
C5 C 1.0000 0.57451(16) 0.67568(18) 0.0203(6) Uani 1 2 d S . .
H5 H 1.0000 0.5470 0.6232 0.024 Uiso 1 2 calc SR . .
C6 C 1.0000 0.5296(2) 0.7500 0.0184(8) Uani 1 4 d S . .
C7 C 1.0000 0.4380(2) 0.7500 0.0249(9) Uani 1 4 d S . .
H7A H 1.0000 0.4180 0.6920 0.037 Uiso 0.50 2 calc SPR . .
H7B H 0.9175 0.4180 0.7790 0.037 Uiso 0.25 1 calc PR . .
H7C H 1.0825 0.4180 0.7790 0.037 Uiso 0.25 1 calc PR . .
C8 C 0.8827(3) 1.00905(17) 0.7500 0.0282(7) Uani 1 2 d S . .
H8 H 0.7977 0.9803 0.7500 0.034 Uiso 1 2 calc SR . .
C9 C 0.8789(3) 1.09341(18) 0.7500 0.0328(7) Uani 1 2 d S . .
H9 H 0.7928 1.1210 0.7500 0.039 Uiso 1 2 calc SR . .
C10 C 1.0000 1.1377(2) 0.7500 0.0282(10) Uani 1 4 d S . .
C11 C 1.0000 1.2297(3) 0.7500 0.0490(14) Uani 1 4 d S . .
H11A H 1.0953 1.2496 0.7500 0.073 Uiso 0.50 2 calc SPR . .
H11B H 0.9524 1.2496 0.8002 0.073 Uiso 0.25 1 calc PR . .
H11C H 0.9524 1.2496 0.6998 0.073 Uiso 0.25 1 calc PR . .
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
_geom_angle_publ_flag
O1 Co1 O1 88.54(7) . 12_755 ?
O1 Co1 O1 91.42(7) . 10_557 ?
O1 Co1 O1 177.96(7) 12_755 10_557 ?
O1 Co1 O1 177.96(7) . 3_756 ?
O1 Co1 O1 91.42(7) 12_755 3_756 ?
O1 Co1 O1 88.54(7) 10_557 3_756 ?
O1 Co1 N1 91.02(4) . . ?
O1 Co1 N1 91.02(4) 12_755 . ?
O1 Co1 N1 91.02(4) 10_557 . ?
O1 Co1 N1 91.02(4) 3_756 . ?
O1 Co1 N2 88.98(4) . . ?
O1 Co1 N2 88.98(4) 12_755 . ?
O1 Co1 N2 88.98(4) 10_557 . ?
O1 Co1 N2 88.98(4) 3_756 . ?
N1 Co1 N2 180.000(1) . . ?
C1 O1 Co1 124.64(12) . . ?
C4 N1 C4 116.7(3) . 10_557 ?
C4 N1 Co1 121.65(16) . . ?
C4 N1 Co1 121.64(16) 10_557 . ?
C8 N2 C8 115.9(3) 3_756 . ?
C8 N2 Co1 122.07(16) 3_756 . ?
C8 N2 Co1 122.07(16) . . ?
O1 C1 C2 128.36(19) . . ?
O1 C1 C3 113.06(17) . . ?
C2 C1 C3 118.58(19) . . ?
C1 C2 C1 122.8(3) . 12_755 ?
C1 C2 H2 118.6 . . ?
C1 C2 H2 118.6 12_755 . ?
F2 C3 F1 107.15(17) . . ?
F2 C3 F3 107.41(18) . . ?
F1 C3 F3 106.34(17) . . ?
F2 C3 C1 113.79(17) . . ?
F1 C3 C1 110.15(17) . . ?
F3 C3 C1 111.62(17) . . ?
N1 C4 C5 123.3(3) . . ?
N1 C4 H4 118.4 . . ?
C5 C4 H4 118.4 . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C5 116.3(3) . 10_557 ?
C5 C6 C7 121.85(17) . . ?
C5 C6 C7 121.85(17) 10_557 . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 123.6(3) . . ?
N2 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C9 116.6(4) 3_756 . ?
C9 C10 C11 121.71(19) 3_756 . ?
C9 C10 C11 121.70(19) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.0597(13) . ?
Co1 O1 2.0597(13) 12_755 ?
Co1 O1 2.0597(13) 10_557 ?
Co1 O1 2.0598(13) 3_756 ?
Co1 N1 2.145(3) . ?
Co1 N2 2.167(3) . ?
O1 C1 1.259(2) . ?
F1 C3 1.338(2) . ?
F2 C3 1.333(2) . ?
F3 C3 1.339(3) . ?
N1 C4 1.345(3) . ?
N1 C4 1.345(3) 10_557 ?
N2 C8 1.342(3) 3_756 ?
N2 C8 1.342(3) . ?
C1 C2 1.395(2) . ?
C1 C3 1.528(3) . ?
C2 C1 1.395(2) 12_755 ?
C2 H2 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9500 . ?
C6 C5 1.394(3) 10_557 ?
C6 C7 1.499(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.381(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(4) . ?
C9 H9 0.9500 . ?
C10 C9 1.380(4) 3_756 ?
C10 C11 1.505(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C1 16.12(17) 12_755 . . . ?
O1 Co1 O1 C1 -161.83(12) 10_557 . . . ?
N1 Co1 O1 C1 107.12(14) . . . . ?
N2 Co1 O1 C1 -72.88(14) . . . . ?
O1 Co1 N1 C4 -44.28(3) . . . . ?
O1 Co1 N1 C4 44.28(3) 12_755 . . . ?
O1 Co1 N1 C4 -135.72(3) 10_557 . . . ?
O1 Co1 N1 C4 135.72(3) 3_756 . . . ?
O1 Co1 N1 C4 135.72(3) . . . 10_557 ?
O1 Co1 N1 C4 -135.72(3) 12_755 . . 10_557 ?
O1 Co1 N1 C4 44.28(3) 10_557 . . 10_557 ?
O1 Co1 N1 C4 -44.28(3) 3_756 . . 10_557 ?
O1 Co1 N2 C8 -45.72(3) . . . 3_756 ?
O1 Co1 N2 C8 -134.28(3) 12_755 . . 3_756 ?
O1 Co1 N2 C8 45.72(3) 10_557 . . 3_756 ?
O1 Co1 N2 C8 134.28(3) 3_756 . . 3_756 ?
O1 Co1 N2 C8 134.28(3) . . . . ?
O1 Co1 N2 C8 45.72(3) 12_755 . . . ?
O1 Co1 N2 C8 -134.28(3) 10_557 . . . ?
O1 Co1 N2 C8 -45.72(3) 3_756 . . . ?
Co1 O1 C1 C2 -11.3(3) . . . . ?
Co1 O1 C1 C3 167.79(12) . . . . ?
O1 C1 C2 C1 -0.6(4) . . . 12_755 ?
C3 C1 C2 C1 -179.72(17) . . . 12_755 ?
O1 C1 C3 F2 172.67(17) . . . . ?
C2 C1 C3 F2 -8.1(3) . . . . ?
O1 C1 C3 F1 -67.0(2) . . . . ?
C2 C1 C3 F1 112.2(2) . . . . ?
O1 C1 C3 F3 50.9(2) . . . . ?
C2 C1 C3 F3 -129.9(2) . . . . ?
C4 N1 C4 C5 -0.001(1) 10_557 . . . ?
Co1 N1 C4 C5 180.0 . . . . ?
N1 C4 C5 C6 0.000(1) . . . . ?
C4 C5 C6 C5 0.001(1) . . . 10_557 ?
C4 C5 C6 C7 180.0 . . . . ?
C8 N2 C8 C9 0.0 3_756 . . . ?
Co1 N2 C8 C9 180.0 . . . . ?
N2 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C9 0.0 . . . 3_756 ?
C8 C9 C10 C11 180.0 . . . . ?
