#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:55:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179353 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/50/4325022.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_4325022
loop_
_publ_author_name
'Victor I. Ovcharenko'
'Sergei V. Fokin'
'Elena Yu. Fursova'
'Olga V. Kuznetsova'
'Eugene V. Tretyakov'
'Galina V. Romanenko'
'Artem S. Bogomyakov'
_publ_section_title
;
 "Jumping Crystals": Oxygen-Evolving Metal-Nitroxide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4307
_journal_page_last               4312
_journal_paper_doi               10.1021/ic1022483
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C32 H36 Co F12 N8 O8'
_chemical_formula_weight         947.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.507(7)
_cell_angle_beta                 99.757(8)
_cell_angle_gamma                99.793(7)
_cell_formula_units_Z            1
_cell_length_a                   7.129(3)
_cell_length_b                   11.317(5)
_cell_length_c                   13.153(6)
_cell_measurement_reflns_used    2140
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.78
_cell_volume                     997.1(8)
_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      295(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7703
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       prizm
_exptl_crystal_F_000             483
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         2870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0568P)²+0.0182P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                2326
_reflns_number_total             2870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022483_si_001_01.cif
_cod_data_source_block           CoL
_cod_original_cell_volume        997.2(8)
_cod_database_code               4325022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Co Co 0.0000 0.0000 0.0000 0.0442(3) Uani 1 2 d S
O1 O -0.1490(4) 0.1273(2) -0.04755(19) 0.0541(7) Uani 1 1 d .
C1 C -0.2373(8) 0.3180(5) -0.0416(4) 0.0669(13) Uani 1 1 d .
F1 F -0.230(4) 0.3431(18) -0.1332(14) 0.123(8) Uani 0.50 1 d P
F2 F -0.425(3) 0.2566(18) -0.0483(14) 0.093(5) Uani 0.50 1 d P
F3 F -0.214(2) 0.4281(12) 0.0377(14) 0.053(2) Uani 0.50 1 d P
F1A F -0.401(2) 0.259(2) -0.0839(17) 0.159(9) Uani 0.50 1 d P
F2A F -0.246(3) 0.4129(19) 0.0185(18) 0.120(8) Uani 0.50 1 d P
F3A F -0.168(4) 0.3684(15) -0.1159(16) 0.108(6) Uani 0.50 1 d P
C2 C -0.0938(6) 0.2416(4) -0.0073(3) 0.0524(10) Uani 1 1 d .
C3 C 0.0824(6) 0.3059(4) 0.0610(3) 0.0634(12) Uani 1 1 d .
H3A H 0.1006 0.3915 0.0850 0.076 Uiso 1 1 calc R
C4 C 0.2314(6) 0.2516(4) 0.0955(3) 0.0524(10) Uani 1 1 d .
C5 C 0.4086(7) 0.3368(5) 0.1768(4) 0.0691(13) Uani 1 1 d .
F4 F 0.453(2) 0.441(2) 0.1446(19) 0.084(5) Uani 0.50 1 d P
F5 F 0.367(3) 0.3676(19) 0.2698(14) 0.141(8) Uani 0.50 1 d P
F6 F 0.576(2) 0.2943(12) 0.1792(9) 0.063(3) Uani 0.50 1 d P
F4A F 0.447(3) 0.4550(18) 0.1726(19) 0.093(6) Uani 0.50 1 d P
F5A F 0.380(3) 0.3413(15) 0.2745(11) 0.086(5) Uani 0.50 1 d P
F6A F 0.553(3) 0.2917(19) 0.1753(16) 0.135(7) Uani 0.50 1 d P
O2 O 0.2396(3) 0.1399(2) 0.07391(19) 0.0499(7) Uani 1 1 d .
O01 O 0.2631(4) -0.3102(3) -0.4376(2) 0.0678(8) Uani 1 1 d .
N1 N 0.1233(4) -0.2658(3) -0.4782(2) 0.0491(8) Uani 1 1 d .
C01 C 0.0354(6) -0.3018(4) -0.5949(3) 0.0534(10) Uani 1 1 d .
C02 C 0.1642(7) -0.2186(4) -0.6431(4) 0.0836(15) Uani 1 1 d .
H02A H 0.2864 -0.2436 -0.6425 0.125 Uiso 1 1 calc R
H02B H 0.1868 -0.1343 -0.6021 0.125 Uiso 1 1 calc R
H02C H 0.1011 -0.2251 -0.7152 0.125 Uiso 1 1 calc R
C03 C 0.0315(7) -0.4378(4) -0.6411(3) 0.0772(14) Uani 1 1 d .
H03A H 0.1623 -0.4489 -0.6400 0.116 Uiso 1 1 calc R
H03B H -0.0424 -0.4636 -0.7133 0.116 Uiso 1 1 calc R
H03C H -0.0278 -0.4868 -0.5993 0.116 Uiso 1 1 calc R
C04 C -0.1657(6) -0.2701(4) -0.5918(3) 0.0537(10) Uani 1 1 d .
C05 C -0.3127(6) -0.3706(4) -0.5678(4) 0.0763(14) Uani 1 1 d .
H05A H -0.4339 -0.3447 -0.5670 0.114 Uiso 1 1 calc R
H05B H -0.2627 -0.3835 -0.4995 0.114 Uiso 1 1 calc R
H05C H -0.3334 -0.4465 -0.6218 0.114 Uiso 1 1 calc R
C06 C -0.2544(7) -0.2262(5) -0.6860(3) 0.0852(16) Uani 1 1 d .
H06A H -0.3787 -0.2086 -0.6774 0.128 Uiso 1 1 calc R
H06B H -0.2712 -0.2897 -0.7504 0.128 Uiso 1 1 calc R
H06C H -0.1695 -0.1525 -0.6898 0.128 Uiso 1 1 calc R
N2 N -0.1127(4) -0.1663(3) -0.4925(2) 0.0470(8) Uani 1 1 d .
O02 O -0.2224(4) -0.0912(3) -0.4701(2) 0.0676(8) Uani 1 1 d .
C07 C 0.0460(5) -0.1777(3) -0.4272(3) 0.0425(9) Uani 1 1 d .
C08 C 0.1047(5) -0.1126(3) -0.3152(3) 0.0415(9) Uani 1 1 d .
C09 C -0.0066(5) -0.0919(3) -0.2434(3) 0.0452(9) Uani 1 1 d .
H09A H -0.1420 -0.1144 -0.2592 0.054 Uiso 1 1 calc R
N3 N 0.1044(4) -0.0336(3) -0.1440(2) 0.0463(8) Uani 1 1 d .
C010 C 0.2849(5) -0.0186(3) -0.1579(3) 0.0489(10) Uani 1 1 d .
H01A H 0.3936 0.0197 -0.1034 0.059 Uiso 1 1 calc R
N4 N 0.2945(4) -0.0641(3) -0.2588(2) 0.0458(8) Uani 1 1 d .
C011 C 0.4698(5) -0.0531(4) -0.3035(3) 0.0648(12) Uani 1 1 d .
H01E H 0.5826 -0.0163 -0.2470 0.097 Uiso 1 1 calc R
H01B H 0.4603 -0.0019 -0.3528 0.097 Uiso 1 1 calc R
H01C H 0.4812 -0.1339 -0.3401 0.097 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
O2 Co O2 180.0 . 2
O2 Co O1 89.90(10) . 2
O2 Co O1 90.10(10) 2 2
O2 Co O1 90.10(10) . .
O2 Co O1 89.90(10) 2 .
O1 Co O1 180.0 2 .
O2 Co N3 91.40(10) . .
O2 Co N3 88.60(10) 2 .
O1 Co N3 88.34(11) 2 .
O1 Co N3 91.66(11) . .
O2 Co N3 88.60(10) . 2
O2 Co N3 91.40(10) 2 2
O1 Co N3 91.66(11) 2 2
O1 Co N3 88.34(11) . 2
N3 Co N3 180.0 . 2
C2 O1 Co 122.7(3) . .
F2A C1 F1A 109.3(15) . .
F2A C1 F1 106.5(14) . .
F1A C1 F1 85.9(15) . .
F2A C1 F3A 97.8(13) . .
F1A C1 F3A 106.3(16) . .
F1 C1 F3A 20.4(19) . .
F2A C1 F2 96.3(13) . .
F1A C1 F2 22.4(16) . .
F1 C1 F2 107.4(14) . .
F3A C1 F2 127.3(13) . .
F2A C1 F3 10.2(18) . .
F1A C1 F3 118.6(12) . .
F1 C1 F3 110.0(10) . .
F3A C1 F3 98.2(9) . .
F2 C1 F3 103.8(9) . .
F2A C1 C2 120.1(12) . .
F1A C1 C2 115.1(10) . .
F1 C1 C2 114.7(10) . .
F3A C1 C2 105.9(11) . .
F2 C1 C2 110.0(9) . .
F3 C1 C2 110.5(8) . .
C1 F1 F1A 44.8(9) . .
F1A F2 C1 61(4) . .
F2 F1A C1 96(4) . .
F2 F1A F1 142(5) . .
C1 F1A F1 49.2(11) . .
O1 C2 C3 128.2(4) . .
O1 C2 C1 114.7(4) . .
C3 C2 C1 117.1(4) . .
C4 C3 C2 124.5(4) . .
O2 C4 C3 128.9(4) . .
O2 C4 C5 114.3(4) . .
C3 C4 C5 116.7(4) . .
F6A C5 F5 115.1(14) . .
F6A C5 F5A 103.3(13) . .
F5 C5 F5A 14.9(16) . .
F6A C5 F4A 111.6(13) . .
F5 C5 F4A 91.3(14) . .
F5A C5 F4A 104.6(13) . .
F6A C5 F4 104.3(12) . .
F5 C5 F4 107.8(15) . .
F5A C5 F4 121.1(13) . .
F4A C5 F4 16(2) . .
F6A C5 F6 3.8(14) . .
F5 C5 F6 113.4(12) . .
F5A C5 F6 102.3(11) . .
F4A C5 F6 108.6(11) . .
F4 C5 F6 102.0(10) . .
F6A C5 C4 110.8(10) . .
F5 C5 C4 110.6(9) . .
F5A C5 C4 109.1(8) . .
F4A C5 C4 116.4(10) . .
F4 C5 C4 107.9(9) . .
F6 C5 C4 114.5(7) . .
C4 O2 Co 122.8(3) . .
O01 N1 C07 126.6(3) . .
O01 N1 C01 122.5(3) . .
C07 N1 C01 110.7(3) . .
N1 C01 C02 105.5(3) . .
N1 C01 C03 109.9(3) . .
C02 C01 C03 111.4(4) . .
N1 C01 C04 99.5(3) . .
C02 C01 C04 114.0(4) . .
C03 C01 C04 115.2(3) . .
N2 C04 C06 110.2(3) . .
N2 C04 C05 104.7(3) . .
C06 C04 C05 111.5(4) . .
N2 C04 C01 100.0(3) . .
C06 C04 C01 115.1(4) . .
C05 C04 C01 114.1(4) . .
O02 N2 C07 126.5(3) . .
O02 N2 C04 122.7(3) . .
C07 N2 C04 110.1(3) . .
N1 C07 N2 109.5(3) . .
N1 C07 C08 126.7(3) . .
N2 C07 C08 123.4(3) . .
C09 C08 N4 105.4(3) . .
C09 C08 C07 128.9(3) . .
N4 C08 C07 125.7(3) . .
C08 C09 N3 111.3(3) . .
C010 N3 C09 104.1(3) . .
C010 N3 Co 129.6(2) . .
C09 N3 Co 125.8(2) . .
N3 C010 N4 112.6(3) . .
C010 N4 C08 106.6(3) . .
C010 N4 C011 126.7(3) . .
C08 N4 C011 126.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co O2 2.054(2) .
Co O2 2.054(2) 2
Co O1 2.069(3) 2
Co O1 2.069(3) .
Co N3 2.132(3) .
Co N3 2.132(3) 2
O1 C2 1.252(4) .
C1 F2A 1.20(2) .
C1 F1A 1.213(18) .
C1 F1 1.304(19) .
C1 F3A 1.353(19) .
C1 F2 1.377(19) .
C1 F3 1.405(17) .
C1 C2 1.520(6) .
F1 F1A 1.72(3) .
F2 F1A 0.53(4) .
C2 C3 1.392(5) .
C3 C4 1.376(6) .
C4 O2 1.248(4) .
C4 C5 1.533(6) .
C5 F6A 1.23(2) .
C5 F5 1.296(19) .
C5 F5A 1.328(16) .
C5 F4A 1.33(2) .
C5 F4 1.34(2) .
C5 F6 1.358(18) .
O01 N1 1.280(4) .
N1 C07 1.330(4) .
N1 C01 1.495(5) .
C01 C02 1.514(6) .
C01 C03 1.521(5) .
C01 C04 1.541(6) .
C04 N2 1.498(4) .
C04 C06 1.513(6) .
C04 C05 1.534(6) .
N2 O02 1.271(4) .
N2 C07 1.343(4) .
C07 C08 1.451(5) .
C08 C09 1.340(5) .
C08 N4 1.384(4) .
C09 N3 1.368(4) .
N3 C010 1.318(4) .
C010 N4 1.333(4) .
N4 C011 1.467(5) .
