#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114246.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_4114246
loop_
_publ_author_name
'Dmitri V. Sevenard'
'Alexander A. Kolomeitsev'
'Berthold Hoge'
'Enno Lork'
'Gerd-Volker Röschenthaler'
_publ_contact_author
;
       Dmitri Sevenard
       Institut für Anorganische und Physikalische Chemie
       der Universität
       Postfach 330 440
       28334 Bremen
       Bundesrepublik Deutschland
;
_publ_contact_author_email       sevenard@chemie.uni-bremen.de
_publ_contact_author_fax         '049 421 2184267'
_publ_contact_author_phone       '049 421 2182493'
_publ_section_title
;
 Noncyclic [10-S-5] Sulfuranide Dioxide Salts with Three S-C Bonds: A New
 Class of Stable Hypervalent Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12366
_journal_page_last               12367
_journal_paper_doi               10.1021/ja030155h
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C15 H24 F9 K O8 S'
_chemical_formula_weight         574.50
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 118.474(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1268(11)
_cell_length_b                   15.632(3)
_cell_length_c                   9.5243(9)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.39
_cell_measurement_theta_min      4.44
_cell_volume                     1194.5(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.812
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4435
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9594
_exptl_absorpt_correction_T_min  0.7878
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0499
_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)+(0.0452P)²+1.4002P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                3521
_reflns_number_total             4124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030155h.cif
_cod_data_source_block           cd607
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4114246
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
S1 S 0.52873(12) 0.19404(8) 0.79141(11) 0.0243(3) Uani 1 1 d .
O1 O 0.5763(5) 0.2616(3) 0.7155(4) 0.0463(10) Uani 1 1 d .
O2 O 0.5321(4) 0.1941(3) 0.9447(3) 0.0397(8) Uani 1 1 d .
C1 C 0.7507(7) 0.1494(4) 0.8890(7) 0.0490(15) Uani 1 1 d .
F1 F 0.8220(5) 0.1438(3) 0.7962(6) 0.0927(16) Uani 1 1 d .
F2 F 0.8465(4) 0.2014(4) 1.0094(5) 0.1008(16) Uani 1 1 d .
F3 F 0.7686(4) 0.0721(3) 0.9565(4) 0.0695(12) Uani 1 1 d .
C2 C 0.3039(6) 0.2368(5) 0.6938(7) 0.0544(18) Uani 1 1 d .
F4 F 0.2360(5) 0.2547(3) 0.5374(4) 0.0823(13) Uani 1 1 d .
F5 F 0.3073(5) 0.3123(3) 0.7602(5) 0.0802(13) Uani 1 1 d .
F6 F 0.1949(4) 0.1892(3) 0.7133(5) 0.0905(14) Uani 1 1 d .
C3 C 0.4512(8) 0.0899(5) 0.6747(6) 0.0544(17) Uani 1 1 d .
F7 F 0.3200(7) 0.1010(4) 0.5374(5) 0.124(2) Uani 1 1 d .
F8 F 0.4191(8) 0.0351(3) 0.7578(6) 0.1119(19) Uani 1 1 d .
F9 F 0.5606(7) 0.0560(4) 0.6420(6) 0.1116(18) Uani 1 1 d .
K1 K 0.45191(10) 0.40220(7) 0.52743(9) 0.0273(2) Uani 1 1 d .
O3 O 0.7427(4) 0.4665(2) 0.7850(4) 0.0422(10) Uani 1 1 d .
C4 C 0.7271(8) 0.5442(4) 0.8547(6) 0.0556(17) Uani 1 1 d .
H4A H 0.7212 0.5934 0.7868 0.058(3) Uiso 1 1 calc R
H4B H 0.8248 0.5521 0.9615 0.058(3) Uiso 1 1 calc R
C5 C 0.5720(8) 0.5390(5) 0.8688(7) 0.0611(18) Uani 1 1 d .
H5A H 0.5732 0.4865 0.9274 0.058(3) Uiso 1 1 calc R
H5B H 0.5644 0.5890 0.9288 0.058(3) Uiso 1 1 calc R
O4 O 0.4321(5) 0.5376(3) 0.7124(4) 0.0468(10) Uani 1 1 d .
C6 C 0.2776(8) 0.5406(5) 0.7134(8) 0.0567(18) Uani 1 1 d .
H6A H 0.2739 0.5916 0.7732 0.058(3) Uiso 1 1 calc R
H6B H 0.2652 0.4891 0.7673 0.058(3) Uiso 1 1 calc R
C7 C 0.1377(8) 0.5444(5) 0.5448(7) 0.0555(17) Uani 1 1 d .
H7A H 0.0301 0.5523 0.5448 0.058(3) Uiso 1 1 calc R
H7B H 0.1543 0.5932 0.4877 0.058(3) Uiso 1 1 calc R
O5 O 0.1365(4) 0.4665(3) 0.4679(4) 0.0462(10) Uani 1 1 d .
C8 C 0.0070(6) 0.4656(5) 0.3054(7) 0.0569(18) Uani 1 1 d .
H8A H 0.0205 0.5152 0.2478 0.058(3) Uiso 1 1 calc R
H8B H -0.1027 0.4706 0.3019 0.058(3) Uiso 1 1 calc R
C9 C 0.0135(6) 0.3849(4) 0.2256(6) 0.0489(16) Uani 1 1 d .
H9A H 0.0082 0.3349 0.2869 0.058(3) Uiso 1 1 calc R
H9B H -0.0822 0.3820 0.1165 0.058(3) Uiso 1 1 calc R
O6 O 0.1655(4) 0.3842(3) 0.2189(4) 0.0436(10) Uani 1 1 d .
C10 C 0.1824(7) 0.3090(4) 0.1418(6) 0.0514(16) Uani 1 1 d .
H10A H 0.0862 0.3039 0.0333 0.058(3) Uiso 1 1 calc R
H10B H 0.1853 0.2575 0.2036 0.058(3) Uiso 1 1 calc R
C11 C 0.3390(7) 0.3156(5) 0.1320(6) 0.0525(16) Uani 1 1 d .
H11A H 0.3456 0.2683 0.0660 0.058(3) Uiso 1 1 calc R
H11B H 0.3418 0.3704 0.0814 0.058(3) Uiso 1 1 calc R
O7 O 0.4757(4) 0.3110(3) 0.2889(4) 0.0417(9) Uani 1 1 d .
C12 C 0.6327(7) 0.3083(5) 0.2908(6) 0.0518(16) Uani 1 1 d .
H12A H 0.6481 0.3606 0.2405 0.058(3) Uiso 1 1 calc R
H12B H 0.6379 0.2580 0.2301 0.058(3) Uiso 1 1 calc R
C13 C 0.7647(7) 0.3026(4) 0.4589(6) 0.0480(15) Uani 1 1 d .
H13A H 0.7408 0.2547 0.5129 0.058(3) Uiso 1 1 calc R
H13B H 0.8738 0.2918 0.4634 0.058(3) Uiso 1 1 calc R
O8 O 0.7703(4) 0.3816(2) 0.5377(4) 0.0387(10) Uani 1 1 d .
C14 C 0.8977(5) 0.3815(4) 0.7004(6) 0.0505(17) Uani 1 1 d .
H14A H 1.0079 0.3742 0.7056 0.058(3) Uiso 1 1 calc R
H14B H 0.8800 0.3331 0.7577 0.058(3) Uiso 1 1 calc R
C15 C 0.8944(5) 0.4630(4) 0.7778(6) 0.0460(15) Uani 1 1 d .
H15A H 0.9904 0.4659 0.8868 0.058(3) Uiso 1 1 calc R
H15B H 0.9014 0.5120 0.7153 0.058(3) 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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O2 S1 O1 129.2(2)
O2 S1 C3 114.4(3)
O1 S1 C3 116.4(3)
O2 S1 C1 90.1(2)
O1 S1 C1 90.5(2)
C3 S1 C1 89.1(3)
O2 S1 C2 89.5(2)
O1 S1 C2 90.6(2)
C3 S1 C2 90.1(3)
C1 S1 C2 178.9(3)
F1 C1 F2 106.5(5)
F1 C1 F3 105.9(5)
F2 C1 F3 104.9(5)
F1 C1 S1 116.2(4)
F2 C1 S1 107.6(4)
F3 C1 S1 114.9(4)
F6 C2 F5 106.3(5)
F6 C2 F4 107.0(5)
F5 C2 F4 103.6(5)
F6 C2 S1 115.9(5)
F5 C2 S1 107.5(4)
F4 C2 S1 115.5(4)
F8 C3 F9 107.7(7)
F8 C3 F7 109.7(6)
F9 C3 F7 105.1(5)
F8 C3 S1 109.7(4)
F9 C3 S1 112.0(5)
F7 C3 S1 112.4(5)
C15 O3 C4 111.8(4)
O3 C4 C5 107.9(5)
O4 C5 C4 108.8(4)
C6 O4 C5 113.0(4)
O4 C6 C7 109.7(4)
O5 C7 C6 108.1(5)
C7 O5 C8 111.5(4)
O5 C8 C9 110.3(4)
O6 C9 C8 107.8(5)
C9 O6 C10 112.0(4)
O6 C10 C11 108.6(5)
O7 C11 C10 108.7(4)
C11 O7 C12 112.9(4)
O7 C12 C13 108.1(4)
O8 C13 C12 108.8(5)
C14 O8 C13 112.0(4)
O8 C14 C15 109.9(4)
O3 C15 C14 108.0(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 O2 1.446(3)
S1 O1 1.457(4)
S1 C3 1.908(6)
S1 C1 1.913(5)
S1 C2 1.924(6)
C1 F1 1.327(7)
C1 F2 1.336(8)
C1 F3 1.341(7)
C2 F6 1.324(7)
C2 F5 1.333(8)
C2 F4 1.342(6)
C3 F8 1.290(8)
C3 F9 1.292(7)
C3 F7 1.296(7)
O3 C15 1.419(6)
O3 C4 1.424(7)
C4 C5 1.486(9)
C5 O4 1.427(7)
O4 C6 1.415(7)
C6 C7 1.502(9)
C7 O5 1.419(8)
O5 C8 1.431(6)
C8 C9 1.489(9)
C9 O6 1.419(6)
O6 C10 1.433(7)
C10 C11 1.480(8)
C11 O7 1.421(6)
O7 C12 1.425(6)
C12 C13 1.478(8)
C13 O8 1.433(7)
O8 C14 1.427(5)
C14 C15 1.479(8)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O2 S1 C1 F1 -173.4(5)
O1 S1 C1 F1 -44.2(5)
C3 S1 C1 F1 72.2(5)
C2 S1 C1 F1 115(14)
O2 S1 C1 F2 -54.2(4)
O1 S1 C1 F2 75.0(4)
C3 S1 C1 F2 -168.6(4)
C2 S1 C1 F2 -126(14)
O2 S1 C1 F3 62.2(5)
O1 S1 C1 F3 -168.6(5)
C3 S1 C1 F3 -52.2(5)
C2 S1 C1 F3 -10(15)
O2 S1 C2 F6 -57.6(5)
O1 S1 C2 F6 173.2(5)
C3 S1 C2 F6 56.8(5)
C1 S1 C2 F6 14(15)
O2 S1 C2 F5 61.0(4)
O1 S1 C2 F5 -68.2(4)
C3 S1 C2 F5 175.4(4)
C1 S1 C2 F5 133(14)
O2 S1 C2 F4 176.1(6)
O1 S1 C2 F4 46.9(6)
C3 S1 C2 F4 -69.5(6)
C1 S1 C2 F4 -112(14)
O2 S1 C3 F8 -2.0(6)
O1 S1 C3 F8 177.8(5)
C1 S1 C3 F8 87.7(5)
C2 S1 C3 F8 -91.5(5)
O2 S1 C3 F9 -121.6(5)
O1 S1 C3 F9 58.2(6)
C1 S1 C3 F9 -31.9(5)
C2 S1 C3 F9 148.9(5)
O2 S1 C3 F7 120.4(5)
O1 S1 C3 F7 -59.8(6)
C1 S1 C3 F7 -149.9(5)
C2 S1 C3 F7 30.9(5)
C15 O3 C4 C5 -175.6(4)
O3 C4 C5 O4 -66.4(7)
C4 C5 O4 C6 -174.6(6)
C5 O4 C6 C7 176.5(6)
O4 C6 C7 O5 65.3(7)
C6 C7 O5 C8 -179.4(4)
C7 O5 C8 C9 177.5(5)
O5 C8 C9 O6 -65.0(5)
C8 C9 O6 C10 -179.2(4)
C9 O6 C10 C11 176.9(4)
O6 C10 C11 O7 67.4(6)
C10 C11 O7 C12 174.2(5)
C11 O7 C12 C13 -179.3(5)
O7 C12 C13 O8 -68.1(6)
C12 C13 O8 C14 -178.8(4)
C13 O8 C14 C15 -178.0(4)
C4 O3 C15 C14 -178.6(4)
O8 C14 C15 O3 66.2(5)
