#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:42:22 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178912 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/41/4114112.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_4114112
loop_
_publ_author_name
'Mitsukimi Tsunoda'
'François P. Gabbaï'
_publ_section_title
;
 Hexacoordination of a Dimethyl Sulfide Molecule
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10492
_journal_page_last               10493
_journal_paper_doi               10.1021/ja036197n
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C20 H6 F12 Hg3 S'
_chemical_formula_weight         1108.08
_chemical_name_common            (o-C6F4Hg)3-(Me2S)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                   11.151(2)
_cell_length_b                   10.743(2)
_cell_length_c                   17.987(4)
_cell_measurement_temperature    120(2)
_cell_volume                     2154.8(7)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1408
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12935
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    21.530
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.397707
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    3.416
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.858
_refine_diff_density_min         -1.879
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0702
_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)+(0.0300P)²+150.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                1357
_reflns_number_total             1690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036197nsi20030516_034445_2.cif
_cod_data_source_block           compound3
_cod_database_code               4114112
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, 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
Hg1 Hg 0.7500 0.5000 0.13399(6) 0.0184(3) Uani 1 2 d S
Hg2 Hg 0.60121(7) 0.43539(8) 0.30664(4) 0.0167(3) Uani 1 1 d .
S S 0.8475(8) 0.2500 0.2500 0.023(2) Uani 1 2 d S
F3 F 0.3298(11) 0.3782(12) 0.2645(6) 0.0254(13) Uani 1 1 d .
F4 F 0.2212(10) 0.3266(12) 0.1348(6) 0.0254(13) Uani 1 1 d .
F5 F 0.3490(11) 0.3267(12) 0.0068(6) 0.0254(13) Uani 1 1 d .
F6 F 0.5814(11) 0.3954(11) 0.0071(6) 0.0254(13) Uani 1 1 d .
F8 F 0.5358(11) 0.3805(12) 0.4756(6) 0.0254(13) Uani 1 1 d .
F9 F 0.6423(11) 0.4428(12) 0.6039(6) 0.0254(13) Uani 1 1 d .
C1 C 0.583(2) 0.422(2) 0.1382(12) 0.0210(17) Uani 1 1 d .
C2 C 0.511(2) 0.4113(19) 0.2056(12) 0.0210(17) Uani 1 1 d .
C3 C 0.398(2) 0.382(2) 0.2023(12) 0.0210(17) Uani 1 1 d .
C4 C 0.338(2) 0.353(2) 0.1355(12) 0.0210(17) Uani 1 1 d .
C5 C 0.406(2) 0.359(2) 0.0707(12) 0.0210(17) Uani 1 1 d .
C6 C 0.522(2) 0.389(2) 0.0739(12) 0.0210(17) Uani 1 1 d .
C7 C 0.699(2) 0.4680(19) 0.4037(12) 0.0210(17) Uani 1 1 d .
C8 C 0.640(2) 0.440(2) 0.4722(12) 0.0210(17) Uani 1 1 d .
C9 C 0.6985(19) 0.4688(19) 0.5398(12) 0.0210(17) Uani 1 1 d .
C10 C 0.953(2) 0.247(2) 0.1749(11) 0.0210(17) Uani 1 1 d .
H10A H 0.9109 0.2457 0.1284 0.031 Uiso 1 1 calc R
H10B H 1.0028 0.1747 0.1790 0.031 Uiso 1 1 calc R
H10C H 1.0025 0.3206 0.1771 0.031 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C1 Hg1 C1 175.8(12) 2_665
C1 Hg1 S 90.6(6) 2_665
C1 Hg1 S 86.9(6) .
C7 Hg2 C2 176.1(8) .
C7 Hg2 S 86.0(6) .
C2 Hg2 S 93.0(6) .
C10 S C10 97.8(15) 4
C10 S Hg2 106.5(7) 4
C10 S Hg2 137.3(7) .
C10 S Hg1 129.0(7) 4
C10 S Hg1 76.8(7) .
Hg2 S Hg1 60.59(9) .
C6 C1 C2 114(2) .
C6 C1 Hg1 121.4(16) .
C2 C1 Hg1 124.3(16) .
C3 C2 C1 121(2) .
C3 C2 Hg2 122.3(17) .
C1 C2 Hg2 116.7(16) .
C2 C3 F3 121(2) .
C2 C3 C4 124(2) .
F3 C3 C4 115.2(19) .
F4 C4 C5 122(2) .
F4 C4 C3 121(2) .
C5 C4 C3 116(2) .
C6 C5 F5 123(2) .
C6 C5 C4 120(2) .
F5 C5 C4 116(2) .
C5 C6 F6 116(2) .
C5 C6 C1 125(2) .
F6 C6 C1 118.7(19) .
C7 C7 C8 120.1(13) 2_665
C7 C7 Hg2 122.2(6) 2_665
C8 C7 Hg2 116.7(16) .
F8 C8 C9 118.0(19) .
F8 C8 C7 123(2) .
C9 C8 C7 119(2) .
C9 C9 F9 120.6(11) 2_665
C9 C9 C8 120.5(13) 2_665
F9 C9 C8 118.6(19) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 C1 2.04(2) 2_665
Hg1 C1 2.04(2) .
Hg1 S 3.571(3) .
Hg2 C7 2.09(2) .
Hg2 C2 2.09(2) .
Hg2 S 3.543(7) .
S C10 1.79(2) 4
S C10 1.79(2) .
F3 C3 1.35(2) .
F4 C4 1.33(2) .
F5 C5 1.36(2) .
F6 C6 1.37(2) .
F8 C8 1.33(2) .
F9 C9 1.34(2) .
C1 C6 1.39(3) .
C1 C2 1.46(3) .
C2 C3 1.30(3) .
C3 C4 1.41(3) .
C4 C5 1.39(3) .
C5 C6 1.34(3) .
C7 C7 1.34(4) 2_665
C7 C8 1.43(3) .
C8 C9 1.41(3) .
C9 C9 1.33(4) 2_665
