#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309506.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_4309506
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            'C31 H17 F12 Hg3 N2 O2'
_chemical_formula_weight         1279.24
_chemical_name_common
'1:1 trimeric perfluoro-o-phenylene mercury:NIT-Ph '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.559(3)
_cell_length_b                   11.559(3)
_cell_length_c                   44.627(14)
_cell_measurement_temperature    110(2)
_cell_volume                     5164(2)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            32596
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    13.441
_exptl_absorpt_correction_T_max  0.352
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.468
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3486
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.375
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0700P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                4446
_reflns_number_total             4893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050528asi20050404_044026.cif
_cod_data_source_block           c2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psiscan' changed to
'psi-scan' 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_database_code               4309506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
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 -0.14908(9) 0.45663(10) 0.250048(19) 0.0449(3) Uani 1 1 d . . .
Hg2 Hg -0.11639(11) 0.76719(9) 0.27438(3) 0.0467(3) Uani 1 1 d . . .
Hg3 Hg -0.39417(10) 0.45681(10) 0.298711(19) 0.0451(3) Uani 1 1 d . . .
F3 F -0.6013(16) 0.1559(18) 0.3131(5) 0.083(6) Uani 1 1 d . . .
F4 F -0.627(2) -0.0751(17) 0.2947(5) 0.091(6) Uani 1 1 d . . .
F5 F -0.446(2) -0.0750(17) 0.2556(6) 0.098(7) Uani 1 1 d . . .
F6 F -0.243(2) 0.1557(19) 0.2349(4) 0.079(5) Uani 1 1 d . . .
F9 F 0.1090(19) 0.5250(19) 0.2132(5) 0.084(6) Uani 1 1 d . . .
F10 F 0.3314(17) 0.761(2) 0.1986(4) 0.076(5) Uani 1 1 d . . .
F11 F 0.3542(18) 0.9920(18) 0.2170(5) 0.088(6) Uani 1 1 d . . .
F12 F 0.1616(17) 0.9995(18) 0.2515(4) 0.073(5) Uani 1 1 d . . .
F15 F -0.1619(17) 0.997(2) 0.2978(5) 0.082(5) Uani 1 1 d . . .
F16 F -0.361(2) 0.9936(17) 0.3314(4) 0.075(5) Uani 1 1 d . . .
F17 F -0.5698(16) 0.7623(19) 0.3502(4) 0.070(5) Uani 1 1 d . . .
F18 F -0.5853(18) 0.5259(18) 0.3359(5) 0.078(6) Uani 1 1 d . . .
C1 C -0.316(2) 0.276(2) 0.2641(6) 0.049(7) Uani 1 1 d . . .
C2 C -0.410(2) 0.276(2) 0.2849(5) 0.035(5) Uani 1 1 d . . .
C3 C -0.511(3) 0.155(3) 0.2937(6) 0.049(7) Uani 1 1 d . . .
C4 C -0.531(3) 0.032(3) 0.2840(8) 0.074(10) Uani 1 1 d . . .
C5 C -0.438(3) 0.032(4) 0.2639(7) 0.066(9) Uani 1 1 d . . .
C6 C -0.336(3) 0.154(3) 0.2547(6) 0.052(7) Uani 1 1 d . . .
C7 C 0.033(3) 0.763(3) 0.2488(8) 0.062(8) Uani 1 1 d . . .
C8 C 0.016(2) 0.639(2) 0.2390(6) 0.039(6) Uani 1 1 d . . .
C9 C 0.114(3) 0.642(3) 0.2227(6) 0.051(5) Uani 1 1 d . . .
C10 C 0.230(3) 0.760(3) 0.2147(6) 0.051(5) Uani 1 1 d . . .
C11 C 0.241(3) 0.878(3) 0.2255(7) 0.058(7) Uani 1 1 d . . .
C12 C 0.145(3) 0.878(3) 0.2412(7) 0.056(8) Uani 1 1 d . . .
C13 C -0.377(2) 0.641(2) 0.3095(6) 0.041(6) Uani 1 1 d . . .
C14 C -0.273(3) 0.761(3) 0.3003(6) 0.047(6) Uani 1 1 d . . .
C15 C -0.268(3) 0.879(3) 0.3077(7) 0.055(7) Uani 1 1 d . . .
C16 C -0.365(3) 0.876(2) 0.3240(6) 0.043(6) Uani 1 1 d . . .
C17 C -0.468(3) 0.763(3) 0.3335(7) 0.061(6) Uani 1 1 d . . .
C18 C -0.476(3) 0.645(3) 0.3258(7) 0.061(6) Uani 1 1 d . . .
N1 N -0.0524(18) 0.553(2) 0.3364(5) 0.047(5) Uani 1 1 d . . .
N2 N 0.0526(18) 0.606(2) 0.3794(5) 0.045(5) Uani 1 1 d . . .
O1 O -0.115(2) 0.559(2) 0.3135(4) 0.059(5) Uani 1 1 d . . .
O2 O 0.114(2) 0.6726(18) 0.4026(4) 0.056(5) Uani 1 1 d . . .
C21 C 0.000(4) 0.778(3) 0.3582(10) 0.069(3) Uani 1 1 d . . .
C22 C 0.086(3) 0.878(3) 0.3400(8) 0.069(3) Uani 1 1 d . . .
H22A H 0.1458 0.8676 0.3279 0.083 Uiso 1 1 calc R . .
C23 C 0.082(3) 0.996(3) 0.3401(8) 0.069(3) Uani 1 1 d . . .
H23A H 0.1379 1.0650 0.3273 0.083 Uiso 1 1 calc R . .
C24 C 0.001(4) 1.013(3) 0.3576(10) 0.069(3) Uani 1 1 d . . .
H24A H 0.0019 1.0944 0.3574 0.083 Uiso 1 1 calc R . .
C25 C -0.082(3) 0.917(3) 0.3756(8) 0.069(3) Uani 1 1 d . . .
H25A H -0.1390 0.9301 0.3881 0.083 Uiso 1 1 calc R . .
C26 C -0.085(3) 0.792(3) 0.3759(8) 0.069(3) Uani 1 1 d . . .
H26A H -0.1442 0.7222 0.3882 0.083 Uiso 1 1 calc R . .
C27 C 0.000(2) 0.648(2) 0.3579(7) 0.044(5) Uani 1 1 d . . .
C28 C 0.014(3) 0.463(3) 0.3754(8) 0.069(5) Uani 1 1 d . . .
C29 C -0.014(3) 0.444(3) 0.3402(8) 0.069(5) Uani 1 1 d . . .
C30 C 0.128(3) 0.441(3) 0.3829(8) 0.075(6) Uani 1 1 d . . .
H30A H 0.1430 0.4493 0.4042 0.112 Uiso 1 1 calc R . .
H30B H 0.2073 0.5061 0.3728 0.112 Uiso 1 1 calc R . .
H30C H 0.1068 0.3530 0.3767 0.112 Uiso 1 1 calc R . .
C31 C -0.099(3) 0.384(3) 0.3946(8) 0.075(6) Uani 1 1 d . . .
H31A H -0.0713 0.4002 0.4151 0.112 Uiso 1 1 calc R . .
H31B H -0.1343 0.2905 0.3901 0.112 Uiso 1 1 calc R . .
H31C H -0.1666 0.4071 0.3911 0.112 Uiso 1 1 calc R . .
C32 C 0.107(4) 0.485(5) 0.3222(12) 0.120(16) Uani 1 1 d . . .
H32A H 0.0845 0.4747 0.3013 0.180 Uiso 1 1 calc R . .
H32B H 0.1449 0.4295 0.3271 0.180 Uiso 1 1 calc R . .
H32C H 0.1712 0.5763 0.3264 0.180 Uiso 1 1 calc R . .
C33 C -0.127(4) 0.318(3) 0.3315(9) 0.078(10) Uani 1 1 d . . .
H33A H -0.1365 0.3147 0.3101 0.117 Uiso 1 1 calc R . .
H33B H -0.2065 0.3092 0.3406 0.117 Uiso 1 1 calc R . .
H33C H -0.1144 0.2460 0.3381 0.117 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 176.4(10) . . ?
C8 Hg1 O1 87.2(8) . . ?
C1 Hg1 O1 89.2(9) . . ?
C7 Hg2 C14 177.1(9) . . ?
C7 Hg2 O1 88.0(8) . . ?
C14 Hg2 O1 89.9(8) . . ?
C7 Hg2 C22 93.2(10) . . ?
C14 Hg2 C22 87.7(9) . . ?
O1 Hg2 C22 62.6(6) . . ?
C13 Hg3 C2 176.3(9) . . ?
C13 Hg3 O1 90.5(7) . . ?
C2 Hg3 O1 90.0(7) . . ?
C6 C1 C2 118(2) . . ?
C6 C1 Hg1 122(2) . . ?
C2 C1 Hg1 120.7(18) . . ?
C3 C2 C1 117(2) . . ?
C3 C2 Hg3 123.0(19) . . ?
C1 C2 Hg3 120.4(18) . . ?
C2 C3 F3 116(2) . . ?
C2 C3 C4 125(3) . . ?
F3 C3 C4 118(3) . . ?
F4 C4 C3 120(3) . . ?
F4 C4 C5 122(3) . . ?
C3 C4 C5 118(3) . . ?
F5 C5 C6 122(3) . . ?
F5 C5 C4 121(4) . . ?
C6 C5 C4 117(3) . . ?
C5 C6 C1 125(3) . . ?
C5 C6 F6 118(2) . . ?
C1 C6 F6 117(2) . . ?
C12 C7 C8 120(3) . . ?
C12 C7 Hg2 120(2) . . ?
C8 C7 Hg2 120(2) . . ?
C9 C8 C7 117(3) . . ?
C9 C8 Hg1 120(2) . . ?
C7 C8 Hg1 123(2) . . ?
C8 C9 F9 121(3) . . ?
C8 C9 C10 124(3) . . ?
F9 C9 C10 115(2) . . ?
F10 C10 C9 123(3) . . ?
F10 C10 C11 121(3) . . ?
C9 C10 C11 116(2) . . ?
C12 C11 F11 123(3) . . ?
C12 C11 C10 122(3) . . ?
F11 C11 C10 115(3) . . ?
C11 C12 C7 121(3) . . ?
C11 C12 F12 119(2) . . ?
C7 C12 F12 119(3) . . ?
C14 C13 C18 117(2) . . ?
C14 C13 Hg3 123.6(17) . . ?
C18 C13 Hg3 120(2) . . ?
C13 C14 C15 121(2) . . ?
C13 C14 Hg2 120.1(18) . . ?
C15 C14 Hg2 119(2) . . ?
C16 C15 F15 122(2) . . ?
C16 C15 C14 119(3) . . ?
F15 C15 C14 119(3) . . ?
C17 C16 C15 122(2) . . ?
C17 C16 F16 118(2) . . ?
C15 C16 F16 120(2) . . ?
C16 C17 C18 119(3) . . ?
C16 C17 F17 121(3) . . ?
C18 C17 F17 120(3) . . ?
C17 C18 C13 122(3) . . ?
C17 C18 F18 118(2) . . ?
C13 C18 F18 120(3) . . ?
O1 N1 C27 124(2) . . ?
O1 N1 C29 122(2) . . ?
C27 N1 C29 113(2) . . ?
O2 N2 C27 125(2) . . ?
O2 N2 C28 122(2) . . ?
C27 N2 C28 112(2) . . ?
N1 O1 Hg3 135.1(15) . . ?
N1 O1 Hg2 138.2(16) . . ?
Hg3 O1 Hg2 75.2(5) . . ?
N1 O1 Hg1 134.0(16) . . ?
Hg3 O1 Hg1 74.2(4) . . ?
Hg2 O1 Hg1 73.5(4) . . ?
C26 C21 C22 122(3) . . ?
C26 C21 C27 120(3) . . ?
C22 C21 C27 119(3) . . ?
C21 C22 C23 118(3) . . ?
C21 C22 Hg2 97(2) . . ?
C23 C22 Hg2 91(2) . . ?
C24 C23 C22 122(3) . . ?
C23 C24 C25 121(3) . . ?
C24 C25 C26 120(3) . . ?
C21 C26 C25 118(3) . . ?
N2 C27 N1 109(2) . . ?
N2 C27 C21 125(3) . . ?
N1 C27 C21 126(3) . . ?
C31 C28 N2 108(3) . . ?
C31 C28 C30 111(3) . . ?
N2 C28 C30 111(2) . . ?
C31 C28 C29 116(2) . . ?
N2 C28 C29 101(3) . . ?
C30 C28 C29 109(3) . . ?
C33 C29 C32 115(4) . . ?
C33 C29 N1 108(2) . . ?
C32 C29 N1 107(3) . . ?
C33 C29 C28 115(3) . . ?
C32 C29 C28 114(3) . . ?
N1 C29 C28 96(2) . . ?
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 2.08(2) . ?
Hg1 C1 2.11(3) . ?
Hg1 O1 3.020(17) . ?
Hg2 C7 2.09(3) . ?
Hg2 C14 2.12(3) . ?
Hg2 O1 2.974(19) . ?
Hg2 C22 3.56(3) . ?
Hg3 C13 2.09(2) . ?
Hg3 C2 2.10(2) . ?
Hg3 O1 2.90(2) . ?
F3 C3 1.36(3) . ?
F4 C4 1.27(4) . ?
F5 C5 1.24(4) . ?
F6 C6 1.38(3) . ?
F9 C9 1.39(3) . ?
F10 C10 1.36(3) . ?
F11 C11 1.36(3) . ?
F12 C12 1.39(3) . ?
F15 C15 1.37(3) . ?
F16 C16 1.38(3) . ?
F17 C17 1.39(3) . ?
F18 C18 1.40(4) . ?
C1 C6 1.38(4) . ?
C1 C2 1.43(3) . ?
C2 C3 1.36(3) . ?
C3 C4 1.39(4) . ?
C4 C5 1.40(4) . ?
C5 C6 1.37(4) . ?
C7 C12 1.36(4) . ?
C7 C8 1.41(4) . ?
C8 C9 1.33(3) . ?
C9 C10 1.39(4) . ?
C10 C11 1.40(4) . ?
C11 C12 1.32(4) . ?
C13 C14 1.37(3) . ?
C13 C18 1.37(4) . ?
C14 C15 1.38(4) . ?
C15 C16 1.33(4) . ?
C16 C17 1.33(4) . ?
C17 C18 1.37(4) . ?
N1 O1 1.28(3) . ?
N1 C27 1.35(4) . ?
N1 C29 1.55(4) . ?
N2 O2 1.27(3) . ?
N2 C27 1.34(4) . ?
N2 C28 1.50(4) . ?
C21 C26 1.33(5) . ?
C21 C22 1.36(5) . ?
C21 C27 1.50(4) . ?
C22 C23 1.40(4) . ?
C23 C24 1.31(5) . ?
C24 C25 1.32(5) . ?
C25 C26 1.43(4) . ?
C28 C31 1.44(5) . ?
C28 C30 1.50(4) . ?
C28 C29 1.60(4) . ?
C29 C33 1.44(4) . ?
C29 C32 1.47(5) . ?
