#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309505.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_4309505
loop_
_publ_author_name
'Mason R. Haneline'
'François P. Gabbaï'
_publ_section_title
;
Coordination of Nitroxide and Nitronyl-nitroxide Organic Radicals to
Trimeric Perfluoro-o-phenylene Mercury
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6248
_journal_page_last               6255
_journal_paper_doi               10.1021/ic050528a
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C49 H17 F24 Hg6 N2 O2'
_chemical_formula_weight         2325.19
_chemical_name_common
'2:1 trimeric perfluoro-o-phenylene mercury:NIT-Ph '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 115.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.963(4)
_cell_length_b                   15.835(3)
_cell_length_c                   20.652(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5295(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    17.460
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.313625
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    2.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4148
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0272
_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)+(0.0485P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3814
_reflns_number_total             4659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050528asi20050404_044012.cif
_cod_data_source_block           fsad
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5294.8(18)
_cod_database_code               4309505
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Hg1 Hg 0.57187(2) -0.26553(2) 0.049565(19) 0.04076(12) Uani 1 1 d . . .
Hg2 Hg 0.55822(2) -0.05091(2) 0.09810(2) 0.04201(12) Uani 1 1 d . . .
Hg3 Hg 0.37305(2) -0.16734(2) -0.00505(2) 0.04615(13) Uani 1 1 d . . .
F3 F 0.2401(4) -0.3051(5) -0.0954(4) 0.088(2) Uani 1 1 d . . .
F4 F 0.2549(4) -0.4602(4) -0.1421(5) 0.105(3) Uani 1 1 d . . .
F5 F 0.4028(4) -0.5237(4) -0.1150(4) 0.080(2) Uani 1 1 d . . .
F6 F 0.5404(3) -0.4350(4) -0.0380(4) 0.0678(18) Uani 1 1 d . . .
F9 F 0.7576(4) -0.3226(4) 0.1417(4) 0.0728(19) Uani 1 1 d . . .
F10 F 0.8948(4) -0.2364(5) 0.2255(5) 0.103(3) Uani 1 1 d . . .
F11 F 0.8860(4) -0.0706(5) 0.2485(5) 0.100(3) Uani 1 1 d . . .
F12 F 0.7400(4) 0.0101(4) 0.1926(4) 0.077(2) Uani 1 1 d . . .
F14 F 0.5029(4) 0.1378(3) 0.1028(3) 0.0625(16) Uani 1 1 d . . .
F16 F 0.3562(4) 0.2118(4) 0.0620(4) 0.0733(19) Uani 1 1 d . . .
F17 F 0.2146(4) 0.1209(4) -0.0096(4) 0.084(2) Uani 1 1 d . . .
F18 F 0.2236(4) -0.0434(4) -0.0350(4) 0.080(2) Uani 1 1 d . . .
O1 O 0.4931(4) -0.2064(4) 0.1362(3) 0.0456(16) Uani 1 1 d . . .
N1 N 0.4971(4) -0.2342(4) 0.1957(4) 0.0330(16) Uani 1 1 d . . .
C1 C 0.4637(6) -0.3228(6) -0.0218(5) 0.042(2) Uani 1 1 d . . .
C2 C 0.3853(6) -0.2879(6) -0.0373(5) 0.041(2) Uani 1 1 d . . .
C3 C 0.3177(6) -0.3361(7) -0.0787(6) 0.060(3) Uani 1 1 d . . .
C4 C 0.3231(6) -0.4138(7) -0.1053(6) 0.063(3) Uani 1 1 d . . .
C5 C 0.3980(7) -0.4467(6) -0.0902(6) 0.058(3) Uani 1 1 d . . .
C6 C 0.4676(6) -0.4000(6) -0.0496(5) 0.049(2) Uani 1 1 d . . .
C7 C 0.6702(5) -0.1138(6) 0.1348(5) 0.043(2) Uani 1 1 d . . .
C8 C 0.6752(5) -0.2011(6) 0.1201(5) 0.043(2) Uani 1 1 d . . .
C9 C 0.7514(6) -0.2395(6) 0.1519(6) 0.053(3) Uani 1 1 d . . .
C10 C 0.8225(6) -0.1962(8) 0.1952(6) 0.064(3) Uani 1 1 d . . .
C11 C 0.8175(6) -0.1123(7) 0.2069(6) 0.059(3) Uani 1 1 d . . .
C12 C 0.7419(6) -0.0729(6) 0.1777(6) 0.054(3) Uani 1 1 d . . .
C13 C 0.3691(6) -0.0425(5) 0.0223(5) 0.040(2) Uani 1 1 d . . .
C14 C 0.4417(6) 0.0052(6) 0.0587(5) 0.042(2) Uani 1 1 d . . .
C15 C 0.4347(6) 0.0894(6) 0.0704(5) 0.048(2) Uani 1 1 d . . .
C16 C 0.3596(7) 0.1288(6) 0.0497(6) 0.050(3) Uani 1 1 d . . .
C17 C 0.2889(7) 0.0826(7) 0.0146(6) 0.058(3) Uani 1 1 d . . .
C18 C 0.2953(6) -0.0009(6) 0.0009(6) 0.048(2) Uani 1 1 d . . .
C21 C 0.5000 0.0826(9) 0.2500 0.053(4) Uani 1 2 d S . .
H21A H 0.5000 0.1413 0.2500 0.063 Uiso 1 2 calc SR . .
C22 C 0.5704(7) 0.0408(6) 0.2639(6) 0.058(3) Uani 1 1 d . . .
H22A H 0.6186 0.0707 0.2735 0.069 Uiso 1 1 calc R . .
C23 C 0.5714(5) -0.0485(6) 0.2639(5) 0.048(2) Uani 1 1 d . . .
H23A H 0.6198 -0.0777 0.2732 0.057 Uiso 1 1 calc R . .
C24 C 0.5000 -0.0910(8) 0.2500 0.039(3) Uani 1 2 d S . .
C25 C 0.5000 -0.1853(7) 0.2500 0.030(3) Uani 1 2 d S . .
C26 C 0.5117(6) -0.3257(5) 0.2181(5) 0.037(2) Uani 1 1 d . . .
C27 C 0.4593(7) -0.3822(6) 0.1556(6) 0.059(3) Uani 1 1 d . . .
H27A H 0.4783 -0.3784 0.1188 0.089 Uiso 1 1 calc R . .
H27B H 0.4027 -0.3644 0.1365 0.089 Uiso 1 1 calc R . .
H27C H 0.4637 -0.4396 0.1719 0.089 Uiso 1 1 calc R . .
C28 C 0.6032(6) -0.3410(6) 0.2400(6) 0.060(3) Uani 1 1 d . . .
H28A H 0.6134 -0.3402 0.1981 0.090 Uiso 1 1 calc R . .
H28B H 0.6187 -0.3949 0.2632 0.090 Uiso 1 1 calc R . .
H28C H 0.6350 -0.2974 0.2725 0.090 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'
Hg Hg -2.3894 9.2266 '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
C8 Hg1 C1 176.1(4) . . ?
C8 Hg1 O1 86.2(3) . . ?
C1 Hg1 O1 91.3(3) . . ?
C7 Hg2 C14 176.4(4) . . ?
C7 Hg2 O1 86.3(3) . . ?
C14 Hg2 O1 90.7(3) . . ?
C7 Hg2 C23 90.3(3) . . ?
C14 Hg2 C23 90.5(3) . . ?
O1 Hg2 C23 66.31(19) . . ?
C2 Hg3 C13 173.8(4) . . ?
C2 Hg3 O1 89.4(3) . . ?
C13 Hg3 O1 91.6(3) . . ?
N1 O1 Hg3 139.7(5) . . ?
N1 O1 Hg1 130.4(5) . . ?
Hg3 O1 Hg1 77.95(15) . . ?
N1 O1 Hg2 132.5(5) . . ?
Hg3 O1 Hg2 76.04(14) . . ?
Hg1 O1 Hg2 75.46(15) . . ?
O1 N1 C25 124.6(7) . . ?
O1 N1 C26 123.8(7) . . ?
C25 N1 C26 111.0(7) . . ?
C6 C1 C2 118.8(8) . . ?
C6 C1 Hg1 119.2(7) . . ?
C2 C1 Hg1 121.7(6) . . ?
C3 C2 C1 116.7(9) . . ?
C3 C2 Hg3 121.6(7) . . ?
C1 C2 Hg3 121.6(6) . . ?
C4 C3 F3 117.4(9) . . ?
C4 C3 C2 123.5(10) . . ?
F3 C3 C2 119.1(9) . . ?
F4 C4 C5 119.5(9) . . ?
F4 C4 C3 120.8(10) . . ?
C5 C4 C3 119.5(9) . . ?
F5 C5 C4 119.1(9) . . ?
F5 C5 C6 122.0(10) . . ?
C4 C5 C6 118.9(9) . . ?
F6 C6 C1 121.2(9) . . ?
F6 C6 C5 116.3(9) . . ?
C1 C6 C5 122.5(9) . . ?
C12 C7 C8 117.9(8) . . ?
C12 C7 Hg2 120.1(7) . . ?
C8 C7 Hg2 122.0(6) . . ?
C9 C8 C7 117.9(8) . . ?
C9 C8 Hg1 121.5(8) . . ?
C7 C8 Hg1 120.5(6) . . ?
F9 C9 C8 119.3(9) . . ?
F9 C9 C10 118.1(9) . . ?
C8 C9 C10 122.6(10) . . ?
F10 C10 C11 120.5(10) . . ?
F10 C10 C9 120.4(10) . . ?
C11 C10 C9 119.0(10) . . ?
F11 C11 C10 119.0(10) . . ?
F11 C11 C12 121.3(10) . . ?
C10 C11 C12 119.7(9) . . ?
F12 C12 C7 119.8(9) . . ?
F12 C12 C11 117.3(9) . . ?
C7 C12 C11 122.9(10) . . ?
C18 C13 C14 117.2(8) . . ?
C18 C13 Hg3 120.9(7) . . ?
C14 C13 Hg3 121.7(6) . . ?
C15 C14 C13 118.8(8) . . ?
C15 C14 Hg2 119.9(7) . . ?
C13 C14 Hg2 121.3(7) . . ?
F14 C15 C14 120.4(9) . . ?
F14 C15 C16 117.0(9) . . ?
C14 C15 C16 122.5(9) . . ?
F16 C16 C17 120.9(9) . . ?
F16 C16 C15 120.2(10) . . ?
C17 C16 C15 118.9(9) . . ?
F17 C17 C18 121.1(10) . . ?
F17 C17 C16 119.8(10) . . ?
C18 C17 C16 118.9(9) . . ?
F18 C18 C17 116.6(9) . . ?
F18 C18 C13 119.8(9) . . ?
C17 C18 C13 123.7(10) . . ?
C22 C21 C22 121.0(14) 2_655 . ?
C21 C22 C23 120.2(10) . . ?
C24 C23 C22 118.9(10) . . ?
C24 C23 Hg2 97.9(5) . . ?
C22 C23 Hg2 90.9(6) . . ?
C23 C24 C23 120.8(12) . 2_655 ?
C23 C24 C25 119.6(6) . . ?
C23 C24 C25 119.6(6) 2_655 . ?
N1 C25 N1 109.6(10) . 2_655 ?
N1 C25 C24 125.2(5) . . ?
N1 C25 C24 125.2(5) 2_655 . ?
N1 C26 C27 110.1(7) . . ?
N1 C26 C28 105.4(7) . . ?
C27 C26 C28 110.6(8) . . ?
N1 C26 C26 100.7(5) . 2_655 ?
C27 C26 C26 115.3(8) . 2_655 ?
C28 C26 C26 113.8(9) . 2_655 ?
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
Hg1 C8 2.066(9) . ?
Hg1 C1 2.071(9) . ?
Hg1 O1 2.877(6) . ?
Hg2 C7 2.071(9) . ?
Hg2 C14 2.088(9) . ?
Hg2 O1 2.975(6) . ?
Hg2 C23 3.328(10) . ?
Hg3 C2 2.065(9) . ?
Hg3 C13 2.066(8) . ?
Hg3 O1 2.846(6) . ?
F3 C3 1.374(12) . ?
F4 C4 1.347(11) . ?
F5 C5 1.339(11) . ?
F6 C6 1.342(10) . ?
F9 C9 1.345(11) . ?
F10 C10 1.334(11) . ?
F11 C11 1.331(11) . ?
F12 C12 1.353(11) . ?
F14 C15 1.351(10) . ?
F16 C16 1.345(11) . ?
F17 C17 1.349(11) . ?
F18 C18 1.354(11) . ?
O1 N1 1.277(9) . ?
N1 C25 1.346(9) . ?
N1 C26 1.508(10) . ?
C1 C6 1.365(13) . ?
C1 C2 1.414(12) . ?
C2 C3 1.374(13) . ?
C3 C4 1.369(14) . ?
C4 C5 1.347(14) . ?
C5 C6 1.380(13) . ?
C7 C12 1.370(13) . ?
C7 C8 1.427(13) . ?
C8 C9 1.377(13) . ?
C9 C10 1.381(14) . ?
C10 C11 1.361(15) . ?
C11 C12 1.374(14) . ?
C13 C18 1.370(12) . ?
C13 C14 1.409(13) . ?
C14 C15 1.370(13) . ?
C15 C16 1.376(13) . ?
C16 C17 1.370(14) . ?
C17 C18 1.368(14) . ?
C21 C22 1.344(12) 2_655 ?
C21 C22 1.344(12) . ?
C22 C23 1.413(13) . ?
C23 C24 1.364(10) . ?
C24 C23 1.364(10) 2_655 ?
C24 C25 1.492(17) . ?
C25 N1 1.346(9) 2_655 ?
C26 C27 1.518(12) . ?
C26 C28 1.522(13) . ?
C26 C26 1.547(17) 2_655 ?
