#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:40:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179802 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009885.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_7009885
loop_
_publ_author_name
'Caneschi, Andrea'
'Gatteschi, Dante'
'Lalioti, Nikolia'
'Sangregorio, Claudio'
'Sessoli, Roberta'
_publ_section_title
;
 Supramolecular interactions and magnetism of metal--radical
 chains †
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3907
_journal_paper_doi               10.1039/b004244g
_journal_year                    2000
_chemical_formula_sum            'C24 H21 Co F12 N2 O7'
_chemical_formula_weight         736.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL93
_cell_angle_alpha                90.08(2)
_cell_angle_beta                 89.93(2)
_cell_angle_gamma                120.030(10)
_cell_formula_units_Z            3
_cell_length_a                   11.295(3)
_cell_length_b                   11.294(2)
_cell_length_c                   20.570(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.33
_cell_measurement_theta_min      9.35
_cell_volume                     2271.8(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'enraf nonius cad4 diffractometer'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3413
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  3600
_diffrn_standards_number         38
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       'needle with an hexagonal base'
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.8
_exptl_crystal_size_min          0.2
_refine_diff_density_max         .264
_refine_diff_density_min         -.297
_refine_diff_density_rms         .057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_obs          0.0433
_refine_ls_shift/esd_max         0.019
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.0825P)²+0.4777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1345
_refine_ls_wR_factor_obs         0.1179
_reflns_number_observed          2616
_reflns_number_total             3413
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004244g.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0825P)^2^+0.4777P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0825P)^2^+0.4777P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P32
_cod_database_code               7009885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.59545(8) 0.47955(7) -0.20932(3) 0.0461(2) Uani 1 d . .
O2 O 0.7407(4) 0.3286(5) -0.4661(2) 0.0532(10) Uani 1 d . .
O3 O 0.7672(4) 0.5063(4) -0.2611(2) 0.0490(9) Uani 1 d . .
O4 O 0.4386(5) 0.4501(5) -0.1482(2) 0.0587(11) Uani 1 d . .
O5 O 0.4725(5) 0.2926(5) -0.2504(2) 0.0604(11) Uani 1 d . .
O6 O 0.7137(5) 0.6817(4) -0.1891(2) 0.0604(11) Uani 1 d . .
O7 O 0.5065(5) 0.5406(5) -0.2808(2) 0.0635(12) Uani 1 d . .
N8 N 0.7700(5) 0.4303(5) -0.3079(2) 0.0469(11) Uani 1 d . .
N9 N 0.7594(5) 0.3489(5) -0.4044(2) 0.0467(10) Uani 1 d . .
C10 C 0.6245(16) 0.8761(15) -0.5211(7) 0.145(5) Uani 1 d . .
H10A H 0.6237(96) 0.9602(43) -0.5262(39) 0.217 Uiso 1 calc R .
H10B H 0.5337(28) 0.8035(82) -0.5115(27) 0.217 Uiso 1 calc R .
H10C H 0.6559(70) 0.8555(120) -0.5606(13) 0.217 Uiso 1 calc R .
C11 C 0.7161(9) 0.7761(9) -0.4477(4) 0.074(2) Uani 1 d . .
C12 C 0.6356(9) 0.6480(10) -0.4717(4) 0.077(2) Uani 1 d . .
H12 H 0.5726(9) 0.6331(10) -0.5042(4) 0.092 Uiso 1 calc R .
C13 C 0.6474(8) 0.5373(8) -0.4473(3) 0.061(2) Uani 1 d . .
H13 H 0.5945(8) 0.4502(8) -0.4647(3) 0.073 Uiso 1 calc R .
C14 C 0.7384(6) 0.5597(6) -0.3975(3) 0.0477(12) Uani 1 d . .
C15 C 0.8160(7) 0.6905(7) -0.3728(3) 0.0572(15) Uani 1 d . .
H15 H 0.8747(7) 0.7057(7) -0.3381(3) 0.069 Uiso 1 calc R .
C16 C 0.8080(10) 0.7993(8) -0.3987(4) 0.079(2) Uani 1 d . .
H16 H 0.8643(10) 0.8874(8) -0.3830(4) 0.094 Uiso 1 calc R .
C17 C 0.7524(7) 0.4480(7) -0.3721(3) 0.0454(11) Uani 1 d . .
C18 C 0.7607(9) 0.2431(7) -0.3601(3) 0.068(2) Uani 1 d . .
C19 C 0.8523(13) 0.1934(10) -0.3876(4) 0.099(4) Uani 1 d . .
H19A H 0.8678(74) 0.1417(76) -0.3551(14) 0.149 Uiso 1 calc R .
H19B H 0.9382(33) 0.2705(10) -0.4003(38) 0.149 Uiso 1 calc R .
H19C H 0.8092(39) 0.1365(70) -0.4248(25) 0.149 Uiso 1 calc R .
C20 C 0.6095(14) 0.1290(8) -0.3566(5) 0.124(5) Uani 1 d . .
H20A H 0.5583(27) 0.1610(39) -0.3324(46) 0.186 Uiso 1 calc R .
H20B H 0.6030(18) 0.0502(40) -0.3355(48) 0.186 Uiso 1 calc R .
H20C H 0.5730(34) 0.1048(80) -0.3998(5) 0.186 Uiso 1 calc R .
C21 C 0.8122(11) 0.3258(9) -0.2975(3) 0.075(2) Uani 1 d . .
C22 C 0.9711(12) 0.4109(13) -0.2948(5) 0.102(3) Uani 1 d . .
H22A H 1.0067(12) 0.3515(19) -0.2853(41) 0.153 Uiso 1 calc R .
H22B H 0.9988(12) 0.4791(58) -0.2614(29) 0.153 Uiso 1 calc R .
H22C H 1.0058(13) 0.4546(71) -0.3360(14) 0.153 Uiso 1 calc R .
C23 C 0.7518(15) 0.2475(11) -0.2355(4) 0.117(5) Uani 1 d . .
H23A H 0.8011(65) 0.3033(39) -0.1990(4) 0.176 Uiso 1 calc R .
H23B H 0.7583(94) 0.1659(53) -0.2357(22) 0.176 Uiso 1 calc R .
H23C H 0.6575(31) 0.2232(88) -0.2325(23) 0.176 Uiso 1 calc R .
C24 C 0.3150(8) 0.3636(8) -0.1599(3) 0.064(2) Uani 1 d . .
C25 C 0.2112(10) 0.3758(11) -0.1163(5) 0.091(3) Uani 1 d . .
C26 C 0.2633(8) 0.2619(9) -0.2074(4) 0.072(2) Uani 1 d . .
H26 H 0.1689(8) 0.2078(9) -0.2113(4) 0.086 Uiso 1 calc R .
C27 C 0.3432(8) 0.2378(7) -0.2482(3) 0.067(2) Uani 1 d . .
C28 C 0.2725(11) 0.1276(12) -0.3014(5) 0.101(3) Uani 1 d . .
C29 C 0.5074(8) 0.6520(9) -0.2819(3) 0.069(2) Uani 1 d . .
C30 C 0.3992(12) 0.6554(13) -0.3241(6) 0.098(3) Uani 1 d . .
C31 C 0.5977(11) 0.7701(9) -0.2472(5) 0.095(3) Uani 1 d . .
H31 H 0.5904(11) 0.8481(9) -0.2523(5) 0.114 Uiso 1 calc R .
C32 C 0.6950(10) 0.7762(8) -0.2066(4) 0.076(2) Uani 1 d . .
C33 C 0.7998(19) 0.9187(10) -0.1753(10) 0.162(7) Uani 1 d . .
O8 O 0.7136(10) 0.8896(7) -0.4692(4) 0.120(3) Uani 1 d . .
F251 F 0.2517(7) 0.3995(9) -0.0554(3) 0.127(2) Uani 1 d . .
F252 F 0.0914(7) 0.2713(10) -0.1168(5) 0.176(4) Uani 1 d . .
F253 F 0.2022(11) 0.4826(12) -0.1346(4) 0.174(4) Uani 1 d . .
F281 F 0.3035(9) 0.0294(7) -0.2957(3) 0.135(3) Uani 1 d . .
F282 F 0.3157(11) 0.1756(9) -0.3588(3) 0.162(4) Uani 1 d . .
F283 F 0.1430(9) 0.0680(12) -0.3011(5) 0.218(6) Uani 1 d . .
F301 F 0.4526(10) 0.7679(11) -0.3607(5) 0.196(5) Uani 1 d . .
F302 F 0.3545(10) 0.5660(11) -0.3694(5) 0.175(4) Uani 1 d . .
F303 F 0.3049(11) 0.6471(19) -0.2947(5) 0.259(9) Uani 1 d . .
F331 F 0.8625(11) 1.0050(9) -0.2236(6) 0.186(4) Uani 1 d . .
F332 F 0.7269(13) 0.9813(9) -0.1554(5) 0.185(4) Uani 1 d . .
F333 F 0.8695(15) 0.9185(8) -0.1353(7) 0.291(10) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co .3494 .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
O6 Co1 O5 166.6(2) . . ?
O6 Co1 O4 95.0(2) . . ?
O5 Co1 O4 90.0(2) . . ?
O6 Co1 O7 85.8(2) . . ?
O5 Co1 O7 81.9(2) . . ?
O4 Co1 O7 88.1(2) . . ?
O6 Co1 O3 84.3(2) . . ?
O5 Co1 O3 92.4(2) . . ?
O4 Co1 O3 172.7(2) . . ?
O7 Co1 O3 99.1(2) . . ?
O6 Co1 O2 95.5(2) . 2_655 ?
O5 Co1 O2 97.2(2) . 2_655 ?
O4 Co1 O2 87.6(2) . 2_655 ?
O7 Co1 O2 175.6(2) . 2_655 ?
O3 Co1 O2 85.2(2) . 2_655 ?
N9 O2 Co1 129.7(4) . 3_664 ?
N8 O3 Co1 127.3(4) . . ?
C24 O4 Co1 122.5(4) . . ?
C27 O5 Co1 120.8(4) . . ?
C32 O6 Co1 127.5(5) . . ?
C29 O7 Co1 125.6(5) . . ?
O3 N8 C17 124.5(5) . . ?
O3 N8 C21 122.5(5) . . ?
C17 N8 C21 112.6(5) . . ?
O2 N9 C17 124.4(5) . . ?
O2 N9 C18 121.4(5) . . ?
C17 N9 C18 113.0(4) . . ?
C12 C11 O8 124.2(8) . . ?
C12 C11 C16 120.5(7) . . ?
O8 C11 C16 115.2(8) . . ?
C11 C12 C13 120.2(7) . . ?
C14 C13 C12 119.5(7) . . ?
C15 C14 C13 118.9(6) . . ?
C15 C14 C17 120.8(5) . . ?
C13 C14 C17 120.3(6) . . ?
C14 C15 C16 121.3(6) . . ?
C11 C16 C15 119.5(7) . . ?
N9 C17 N8 106.5(5) . . ?
N9 C17 C14 129.0(5) . . ?
N8 C17 C14 124.4(5) . . ?
N9 C18 C19 110.4(5) . . ?
N9 C18 C21 100.2(5) . . ?
C19 C18 C21 114.9(8) . . ?
N9 C18 C20 104.1(7) . . ?
C19 C18 C20 112.6(8) . . ?
C21 C18 C20 113.3(7) . . ?
N8 C21 C23 111.0(6) . . ?
N8 C21 C18 100.8(5) . . ?
C23 C21 C18 115.7(8) . . ?
N8 C21 C22 104.0(7) . . ?
C23 C21 C22 112.0(9) . . ?
C18 C21 C22 112.1(7) . . ?
O4 C24 C26 128.0(7) . . ?
O4 C24 C25 114.7(7) . . ?
C26 C24 C25 117.3(8) . . ?
F252 C25 F251 107.2(10) . . ?
F252 C25 F253 108.3(11) . . ?
F251 C25 F253 105.4(9) . . ?
F252 C25 C24 114.7(9) . . ?
F251 C25 C24 111.8(8) . . ?
F253 C25 C24 109.1(9) . . ?
C27 C26 C24 123.5(7) . . ?
O5 C27 C26 129.9(7) . . ?
O5 C27 C28 111.9(7) . . ?
C26 C27 C28 118.1(8) . . ?
F283 C28 F282 108.7(11) . . ?
F283 C28 F281 105.8(11) . . ?
F282 C28 F281 103.4(10) . . ?
F283 C28 C27 114.8(9) . . ?
F282 C28 C27 112.0(9) . . ?
F281 C28 C27 111.3(9) . . ?
O7 C29 C31 125.6(7) . . ?
O7 C29 C30 115.8(8) . . ?
C31 C29 C30 118.6(8) . . ?
F303 C30 F302 108.9(13) . . ?
F303 C30 F301 108.8(11) . . ?
F302 C30 F301 98.8(10) . . ?
F303 C30 C29 114.2(10) . . ?
F302 C30 C29 113.8(9) . . ?
F301 C30 C29 111.3(9) . . ?
C32 C31 C29 123.1(7) . . ?
O6 C32 C31 128.2(8) . . ?
O6 C32 C33 113.3(8) . . ?
C31 C32 C33 118.5(8) . . ?
F333 C33 F331 115.4(18) . . ?
F333 C33 F332 112.0(19) . . ?
F331 C33 F332 94.7(8) . . ?
F333 C33 C32 117.2(9) . . ?
F331 C33 C32 107.3(14) . . ?
F332 C33 C32 107.7(13) . . ?
C11 O8 C10 119.2(9) . . ?
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 O6 2.028(4) . ?
Co1 O5 2.040(4) . ?
Co1 O4 2.057(5) . ?
Co1 O7 2.085(5) . ?
Co1 O3 2.097(4) . ?
Co1 O2 2.111(4) 2_655 ?
O2 N9 1.287(6) . ?
O2 Co1 2.108(4) 3_664 ?
O3 N8 1.300(6) . ?
O4 C24 1.264(9) . ?
O5 C27 1.270(9) . ?
O6 C32 1.241(9) . ?
O7 C29 1.253(10) . ?
N8 C17 1.366(7) . ?
N8 C21 1.493(9) . ?
N9 C17 1.337(8) . ?
N9 C18 1.510(8) . ?
C10 O8 1.423(14) . ?
C11 C12 1.358(12) . ?
C11 O8 1.371(9) . ?
C11 C16 1.375(12) . ?
C12 C13 1.414(11) . ?
C13 C14 1.383(9) . ?
C14 C15 1.382(9) . ?
C14 C17 1.446(9) . ?
C15 C16 1.383(10) . ?
C18 C19 1.511(10) . ?
C18 C21 1.525(10) . ?
C18 C20 1.543(15) . ?
C21 C23 1.506(10) . ?
C21 C22 1.56(2) . ?
C24 C26 1.393(10) . ?
C24 C25 1.535(12) . ?
C25 F252 1.274(12) . ?
C25 F251 1.315(12) . ?
C25 F253 1.315(13) . ?
C26 C27 1.356(11) . ?
C27 C28 1.545(11) . ?
C28 F283 1.267(14) . ?
C28 F282 1.289(14) . ?
C28 F281 1.325(14) . ?
C29 C31 1.402(12) . ?
C29 C30 1.516(11) . ?
C30 F303 1.187(13) . ?
C30 F302 1.276(13) . ?
C30 F301 1.333(13) . ?
C31 C32 1.356(12) . ?
C32 C33 1.580(15) . ?
C33 F333 1.14(2) . ?
C33 F331 1.32(2) . ?
C33 F332 1.39(2) . ?
