data_global
_journal_coden_Cambridge 182
loop_
_publ_author_name
'Schulz, A'
'Villinger, Alexander'
_publ_contact_author_name 'Schulz, A'
_publ_contact_author_email axel.schulz@uni-rostock.de
_publ_section_title
;
Preparation and Characterization of
[CF3SO3(SiMe3)2]+[B(C6F5)4]\^a
;
# Attachment 'silylsulfonat.cif'
data_sime2_cf3so3
_database_code_depnum_ccdc_archive 'CCDC 766935'
#TrackingRef 'silylsulfonat.cif'
_audit_author_name 'Villinger, A.'
_audit_creation_method SHELXL-97
#==============================================================================
# CHEMICAL DATA
_chemical_name_systematic
;
Bis(trimethylsilyl)trifluoromethylsulfonium tetrakis(pentafluorophenyl)borate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C24 B F20 -, C7 H18 F3 O3 S Si2 +'
_chemical_formula_sum 'C31 H18 B F23 O3 S Si2'
_chemical_formula_weight 974.50
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'
B B 0.0013 0.0007 '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'
Si Si 0.0817 0.0704 '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'
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.319(6)
_cell_length_b 13.300(7)
_cell_length_c 15.086(9)
_cell_angle_alpha 68.287(10)
_cell_angle_beta 82.484(12)
_cell_angle_gamma 76.86(2)
_cell_volume 1870.7(19)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9943
_cell_measurement_theta_min 6.861
_cell_measurement_theta_max 59.786
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.730
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 968
_exptl_absorpt_coefficient_mu 0.300
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8868
_exptl_absorpt_correction_T_max 0.9649
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# EXPERIMENTAL DATA
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 38916
_diffrn_reflns_av_R_equivalents 0.0259
_diffrn_reflns_av_sigmaI/netI 0.0254
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 1.45
_diffrn_reflns_theta_max 29.99
_reflns_number_total 10715
_reflns_number_gt 8535
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'Bruker Apex v7.51a'
_computing_cell_refinement 'Bruker Apex v7.51a'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material SHELXL-97
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 and with U~iso~(H) = 1.5 times U~eq~(C).
Torsion angles of all methyl groups were allowed to refine.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.3615P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10715
_refine_ls_number_parameters 556
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0494
_refine_ls_R_factor_gt 0.0360
_refine_ls_wR_factor_ref 0.1035
_refine_ls_wR_factor_gt 0.0978
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
#==============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
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
S S 0.79020(4) 0.66726(3) 0.82950(2) 0.03288(9) Uani 1 1 d . . .
Si1 Si 0.76520(4) 0.70475(3) 1.01647(3) 0.02907(9) Uani 1 1 d . . .
Si2 Si 0.98226(5) 0.74387(3) 0.65740(3) 0.03411(10) Uani 1 1 d . . .
O1 O 0.73511(11) 0.72945(9) 0.89372(7) 0.0345(2) Uani 1 1 d . . .
O2 O 0.83672(13) 0.74697(9) 0.73990(8) 0.0423(3) Uani 1 1 d . . .
O3 O 0.87865(14) 0.56604(10) 0.86899(8) 0.0478(3) Uani 1 1 d . . .
F1 F 0.58061(13) 0.58233(10) 0.87313(10) 0.0638(3) Uani 1 1 d . . .
F2 F 0.55941(15) 0.73598(10) 0.75594(12) 0.0773(4) Uani 1 1 d . . .
F3 F 0.67695(16) 0.58873(10) 0.73666(9) 0.0678(4) Uani 1 1 d . . .
C1 C 0.6392(2) 0.64299(14) 0.79576(14) 0.0477(4) Uani 1 1 d . . .
C2 C 0.7260(2) 0.56776(14) 1.08312(12) 0.0499(5) Uani 1 1 d . . .
H2A H 0.6336 0.5685 1.0736 0.075 Uiso 1 1 calc R . .
H2B H 0.7374 0.5486 1.1513 0.075 Uiso 1 1 calc R . .
H2C H 0.7861 0.5130 1.0601 0.075 Uiso 1 1 calc R . .
C3 C 0.64564(16) 0.82050(12) 1.03475(11) 0.0337(3) Uani 1 1 d . . .
H3A H 0.6660 0.8899 0.9881 0.051 Uiso 1 1 calc R . .
H3B H 0.6513 0.8193 1.0995 0.051 Uiso 1 1 calc R . .
H3C H 0.5554 0.8145 1.0265 0.051 Uiso 1 1 calc R . .
C4 C 0.94126(18) 0.71356(17) 1.00865(13) 0.0461(4) Uani 1 1 d . . .
H4A H 0.9963 0.6521 0.9918 0.069 Uiso 1 1 calc R . .
H4B H 0.9663 0.7098 1.0704 0.069 Uiso 1 1 calc R . .
H4C H 0.9554 0.7836 0.9595 0.069 Uiso 1 1 calc R . .
C5 C 0.9237(2) 0.87264(14) 0.56159(12) 0.0468(4) Uani 1 1 d . . .
H5A H 0.8415 0.8683 0.5384 0.070 Uiso 1 1 calc R . .
H5B H 0.9919 0.8851 0.5091 0.070 Uiso 1 1 calc R . .
H5C H 0.9063 0.9338 0.5857 0.070 Uiso 1 1 calc R . .
C6 C 0.9999(3) 0.61688(16) 0.63359(16) 0.0595(6) Uani 1 1 d . . .
H6A H 1.0051 0.5542 0.6941 0.089 Uiso 1 1 calc R . .
H6B H 1.0814 0.6073 0.5937 0.089 Uiso 1 1 calc R . .
H6C H 0.9228 0.6206 0.6001 0.089 Uiso 1 1 calc R . .
C7 C 1.1185(3) 0.7482(2) 0.72194(17) 0.0681(6) Uani 1 1 d . . .
H7A H 1.0964 0.8149 0.7387 0.102 Uiso 1 1 calc R . .
H7B H 1.2008 0.7491 0.6813 0.102 Uiso 1 1 calc R . .
H7C H 1.1310 0.6829 0.7804 0.102 Uiso 1 1 calc R . .
B B 0.22856(13) 0.77422(10) 0.25865(9) 0.0178(2) Uani 1 1 d . . .
C8 C 0.06531(12) 0.78943(10) 0.27817(8) 0.0195(2) Uani 1 1 d . . .
C9 C -0.02177(13) 0.87063(10) 0.30512(8) 0.0225(2) Uani 1 1 d . . .
C10 C -0.15834(13) 0.87782(11) 0.31814(9) 0.0265(3) Uani 1 1 d . . .
C11 C -0.21542(13) 0.80390(12) 0.30005(10) 0.0289(3) Uani 1 1 d . . .
C12 C -0.13466(13) 0.72433(11) 0.26947(9) 0.0267(3) Uani 1 1 d . . .
C13 C 0.00068(13) 0.71891(10) 0.25989(9) 0.0219(2) Uani 1 1 d . . .
C14 C 0.24240(12) 0.80445(9) 0.14141(8) 0.0191(2) Uani 1 1 d . . .
C15 C 0.18817(12) 0.91025(10) 0.08202(9) 0.0214(2) Uani 1 1 d . . .
C16 C 0.18047(13) 0.94273(11) -0.01544(9) 0.0258(3) Uani 1 1 d . . .
C17 C 0.22753(15) 0.86670(12) -0.05961(9) 0.0292(3) Uani 1 1 d . . .
C18 C 0.28137(14) 0.76073(12) -0.00511(9) 0.0285(3) Uani 1 1 d . . .
C19 C 0.28812(13) 0.73200(10) 0.09253(9) 0.0229(2) Uani 1 1 d . . .
C20 C 0.29410(12) 0.85421(9) 0.29362(8) 0.0200(2) Uani 1 1 d . . .
C21 C 0.37526(12) 0.92734(10) 0.23955(9) 0.0225(2) Uani 1 1 d . . .
C22 C 0.42844(14) 0.99156(11) 0.27375(10) 0.0280(3) Uani 1 1 d . . .
C23 C 0.40516(15) 0.98177(11) 0.36800(11) 0.0318(3) Uani 1 1 d . . .
C24 C 0.32981(14) 0.90715(11) 0.42663(10) 0.0283(3) Uani 1 1 d . . .
C25 C 0.27668(13) 0.84637(10) 0.38894(9) 0.0228(2) Uani 1 1 d . . .
C26 C 0.30614(12) 0.64871(9) 0.32075(8) 0.0188(2) Uani 1 1 d . . .
C27 C 0.25259(13) 0.57124(10) 0.39742(8) 0.0222(2) Uani 1 1 d . . .
C28 C 0.32509(15) 0.47008(11) 0.45104(9) 0.0279(3) Uani 1 1 d . . .
C29 C 0.45834(15) 0.44229(10) 0.42890(10) 0.0288(3) Uani 1 1 d . . .
C30 C 0.51789(13) 0.51648(11) 0.35452(9) 0.0255(3) Uani 1 1 d . . .
C31 C 0.44217(12) 0.61679(10) 0.30349(9) 0.0218(2) Uani 1 1 d . . .
F4 F 0.02358(8) 0.94994(6) 0.32096(6) 0.02907(17) Uani 1 1 d . . .
F5 F -0.23558(9) 0.95665(8) 0.34718(6) 0.0373(2) Uani 1 1 d . . .
F6 F -0.34717(8) 0.80950(8) 0.31114(7) 0.0434(2) Uani 1 1 d . . .
F7 F -0.18844(9) 0.65270(8) 0.24929(7) 0.0384(2) Uani 1 1 d . . .
F8 F 0.07402(8) 0.63682(6) 0.23120(6) 0.02675(16) Uani 1 1 d . . .
F9 F 0.13689(8) 0.98911(6) 0.12026(5) 0.02744(17) Uani 1 1 d . . .
F10 F 0.12628(9) 1.04685(7) -0.06692(6) 0.0359(2) Uani 1 1 d . . .
F11 F 0.21774(11) 0.89510(9) -0.15359(6) 0.0438(2) Uani 1 1 d . . .
F12 F 0.32585(11) 0.68440(8) -0.04624(7) 0.0459(2) Uani 1 1 d . . .
F13 F 0.34064(9) 0.62530(6) 0.13878(6) 0.03194(18) Uani 1 1 d . . .
F14 F 0.41071(8) 0.93922(6) 0.14732(5) 0.02801(16) Uani 1 1 d . . .
F15 F 0.50613(10) 1.06014(7) 0.21581(7) 0.0413(2) Uani 1 1 d . . .
F16 F 0.45602(12) 1.04327(8) 0.40219(8) 0.0488(3) Uani 1 1 d . . .
F17 F 0.30688(10) 0.89487(8) 0.51933(6) 0.0406(2) Uani 1 1 d . . .
F18 F 0.20133(8) 0.77664(7) 0.45010(5) 0.02839(17) Uani 1 1 d . . .
F19 F 0.12269(8) 0.58957(7) 0.42630(6) 0.03030(17) Uani 1 1 d . . .
F20 F 0.26497(10) 0.39879(8) 0.52356(7) 0.0438(2) Uani 1 1 d . . .
F21 F 0.52972(10) 0.34438(7) 0.47911(7) 0.0447(2) Uani 1 1 d . . .
F22 F 0.64837(8) 0.49007(7) 0.33203(7) 0.0388(2) Uani 1 1 d . . .
F23 F 0.50681(8) 0.68604(6) 0.23184(6) 0.02859(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S 0.0470(2) 0.02632(16) 0.02255(15) -0.00947(13) 0.00362(14) -0.00338(14)
Si1 0.0379(2) 0.02638(18) 0.02142(17) -0.00785(14) 0.00196(15) -0.00620(15)
Si2 0.0454(2) 0.02616(19) 0.02667(19) -0.00810(15) 0.00371(17) -0.00412(16)
O1 0.0453(6) 0.0334(5) 0.0244(5) -0.0132(4) -0.0006(4) -0.0020(4)
O2 0.0580(7) 0.0317(5) 0.0306(5) -0.0101(4) 0.0130(5) -0.0061(5)
O3 0.0618(8) 0.0344(6) 0.0344(6) -0.0089(5) 0.0037(5) 0.0067(5)
F1 0.0678(8) 0.0520(7) 0.0815(9) -0.0351(6) 0.0235(7) -0.0268(6)
F2 0.0841(9) 0.0438(6) 0.1111(11) -0.0253(7) -0.0520(8) -0.0028(6)
F3 0.1118(11) 0.0580(7) 0.0558(7) -0.0362(6) 0.0013(7) -0.0353(7)
C1 0.0667(12) 0.0315(8) 0.0517(10) -0.0201(7) -0.0055(9) -0.0125(8)
C2 0.0847(14) 0.0312(8) 0.0321(8) -0.0089(6) 0.0064(8) -0.0172(8)
C3 0.0403(8) 0.0304(7) 0.0296(7) -0.0116(6) 0.0045(6) -0.0071(6)
C4 0.0386(9) 0.0556(10) 0.0434(9) -0.0195(8) -0.0035(7) -0.0031(8)
C5 0.0544(11) 0.0389(8) 0.0306(7) -0.0037(6) 0.0082(7) 0.0024(7)
C6 0.0840(15) 0.0387(9) 0.0585(11) -0.0277(9) 0.0281(11) -0.0172(9)
C7 0.0658(14) 0.0754(15) 0.0613(13) -0.0168(12) -0.0149(11) -0.0157(12)
B 0.0194(6) 0.0165(5) 0.0165(5) -0.0049(4) -0.0013(4) -0.0027(4)
C8 0.0190(5) 0.0208(5) 0.0165(5) -0.0047(4) -0.0016(4) -0.0025(4)
C9 0.0236(6) 0.0234(6) 0.0192(5) -0.0074(4) -0.0031(4) -0.0014(4)
C10 0.0224(6) 0.0287(6) 0.0211(6) -0.0060(5) -0.0015(5) 0.0046(5)
C11 0.0165(6) 0.0345(7) 0.0274(6) -0.0024(5) -0.0025(5) -0.0023(5)
C12 0.0249(6) 0.0272(6) 0.0258(6) -0.0035(5) -0.0053(5) -0.0085(5)
C13 0.0224(6) 0.0208(5) 0.0201(5) -0.0047(4) -0.0023(4) -0.0032(4)
C14 0.0191(5) 0.0196(5) 0.0181(5) -0.0054(4) -0.0007(4) -0.0048(4)
C15 0.0221(6) 0.0211(5) 0.0206(5) -0.0066(4) -0.0018(4) -0.0041(4)
C16 0.0264(6) 0.0250(6) 0.0213(6) -0.0009(5) -0.0045(5) -0.0066(5)
C17 0.0341(7) 0.0376(7) 0.0163(5) -0.0067(5) -0.0010(5) -0.0124(6)
C18 0.0334(7) 0.0325(7) 0.0234(6) -0.0150(5) 0.0032(5) -0.0079(5)
C19 0.0256(6) 0.0204(5) 0.0213(5) -0.0065(4) -0.0010(5) -0.0030(4)
C20 0.0191(5) 0.0180(5) 0.0216(5) -0.0071(4) -0.0039(4) 0.0005(4)
C21 0.0210(6) 0.0213(5) 0.0247(6) -0.0082(5) -0.0041(5) -0.0011(4)
C22 0.0253(6) 0.0202(6) 0.0377(7) -0.0075(5) -0.0058(5) -0.0052(5)
C23 0.0340(7) 0.0269(6) 0.0411(8) -0.0177(6) -0.0148(6) -0.0021(5)
C24 0.0318(7) 0.0282(6) 0.0263(6) -0.0134(5) -0.0093(5) 0.0022(5)
C25 0.0216(6) 0.0223(6) 0.0230(6) -0.0079(5) -0.0041(4) -0.0001(4)
C26 0.0208(6) 0.0175(5) 0.0177(5) -0.0060(4) -0.0029(4) -0.0023(4)
C27 0.0234(6) 0.0229(6) 0.0186(5) -0.0057(4) -0.0012(4) -0.0041(4)
C28 0.0354(7) 0.0230(6) 0.0198(6) 0.0004(5) -0.0034(5) -0.0075(5)
C29 0.0343(7) 0.0194(6) 0.0273(6) -0.0024(5) -0.0120(5) 0.0014(5)
C30 0.0214(6) 0.0246(6) 0.0285(6) -0.0082(5) -0.0057(5) 0.0002(5)
C31 0.0229(6) 0.0199(5) 0.0213(5) -0.0051(4) -0.0021(4) -0.0047(4)
F4 0.0279(4) 0.0273(4) 0.0354(4) -0.0176(3) -0.0039(3) 0.0004(3)
F5 0.0273(4) 0.0414(5) 0.0375(5) -0.0173(4) 0.0000(3) 0.0094(4)
F6 0.0164(4) 0.0498(6) 0.0560(6) -0.0113(5) -0.0023(4) -0.0029(4)
F7 0.0290(4) 0.0389(5) 0.0518(5) -0.0145(4) -0.0074(4) -0.0148(4)
F8 0.0264(4) 0.0239(4) 0.0332(4) -0.0134(3) -0.0009(3) -0.0057(3)
F9 0.0335(4) 0.0189(3) 0.0270(4) -0.0074(3) -0.0051(3) 0.0012(3)
F10 0.0440(5) 0.0282(4) 0.0258(4) 0.0030(3) -0.0114(3) -0.0038(4)
F11 0.0619(6) 0.0519(6) 0.0166(4) -0.0081(4) -0.0046(4) -0.0141(5)
F12 0.0681(7) 0.0438(5) 0.0308(4) -0.0246(4) 0.0019(4) -0.0035(5)
F13 0.0455(5) 0.0200(4) 0.0278(4) -0.0098(3) -0.0035(3) 0.0019(3)
F14 0.0310(4) 0.0286(4) 0.0245(4) -0.0076(3) 0.0032(3) -0.0118(3)
F15 0.0438(5) 0.0343(5) 0.0501(5) -0.0107(4) -0.0035(4) -0.0225(4)
F16 0.0647(7) 0.0439(5) 0.0540(6) -0.0254(5) -0.0181(5) -0.0198(5)
F17 0.0541(6) 0.0460(5) 0.0284(4) -0.0208(4) -0.0096(4) -0.0057(4)
F18 0.0314(4) 0.0318(4) 0.0209(3) -0.0086(3) 0.0006(3) -0.0064(3)
F19 0.0248(4) 0.0322(4) 0.0245(4) -0.0016(3) 0.0051(3) -0.0052(3)
F20 0.0482(6) 0.0322(5) 0.0319(4) 0.0112(4) 0.0007(4) -0.0105(4)
F21 0.0451(5) 0.0259(4) 0.0455(5) 0.0046(4) -0.0162(4) 0.0062(4)
F22 0.0215(4) 0.0353(5) 0.0495(5) -0.0084(4) -0.0044(4) 0.0046(3)
F23 0.0222(4) 0.0261(4) 0.0305(4) -0.0025(3) 0.0030(3) -0.0065(3)
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
Least-squares planes (x,y,z in crystal coordinates) and deviations from them
(* indicates atom used to define plane)
2.6433 (0.0082) x + 3.6827 (0.0102) y + 14.8490 (0.0091) z = 20.0932 (0.0161)
* 0.0000 (0.0000) C2
* 0.0000 (0.0000) C3
* 0.0000 (0.0000) C4
-0.3817 (0.0011) Si1
Rms deviation of fitted atoms = 0.0000
7.2858 (0.0093) x - 0.4091 (0.0125) y - 9.1649 (0.0146) z = 1.2262 (0.0232)
Angle to previous plane (with approximate su) = 59.81 ( 0.08 )
* 0.0000 (0.0000) C5
* 0.0000 (0.0000) C6
* 0.0000 (0.0000) C7
-0.3989 (0.0013) Si2
Rms deviation of fitted atoms = 0.0000
;
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
S O3 1.4109(13) . ?
S O1 1.4769(12) . ?
S O2 1.4774(13) . ?
S C1 1.830(2) . ?
Si1 O1 1.8131(15) . ?
Si1 C3 1.8249(17) . ?
Si1 C4 1.833(2) . ?
Si1 C2 1.835(2) . ?
Si2 C6 1.818(2) . ?
Si2 C5 1.8204(18) . ?
Si2 O2 1.8240(14) . ?
Si2 C7 1.834(3) . ?
F1 C1 1.311(2) . ?
F2 C1 1.298(2) . ?
F3 C1 1.313(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
B C20 1.6443(19) . ?
B C8 1.651(2) . ?
B C26 1.6543(18) . ?
B C14 1.657(2) . ?
C8 C13 1.3871(18) . ?
C8 C9 1.3882(17) . ?
C9 F4 1.3524(16) . ?
C9 C10 1.383(2) . ?
C10 F5 1.3399(16) . ?
C10 C11 1.375(2) . ?
C11 F6 1.3363(17) . ?
C11 C12 1.374(2) . ?
C12 F7 1.3444(17) . ?
C12 C13 1.373(2) . ?
C13 F8 1.3567(15) . ?
C14 C19 1.3868(17) . ?
C14 C15 1.3915(17) . ?
C15 F9 1.3523(15) . ?
C15 C16 1.3783(19) . ?
C16 F10 1.3414(16) . ?
C16 C17 1.376(2) . ?
C17 F11 1.3369(17) . ?
C17 C18 1.370(2) . ?
C18 F12 1.3439(16) . ?
C18 C19 1.3851(19) . ?
C19 F13 1.3458(16) . ?
C20 C21 1.3847(19) . ?
C20 C25 1.3931(19) . ?
C21 F14 1.3510(16) . ?
C21 C22 1.3820(19) . ?
C22 F15 1.3408(17) . ?
C22 C23 1.373(2) . ?
C23 F16 1.3374(16) . ?
C23 C24 1.376(2) . ?
C24 F17 1.3418(17) . ?
C24 C25 1.3785(19) . ?
C25 F18 1.3502(16) . ?
C26 C27 1.3837(18) . ?
C26 C31 1.3905(19) . ?
C27 F19 1.3502(16) . ?
C27 C28 1.3856(18) . ?
C28 F20 1.3428(17) . ?
C28 C29 1.371(2) . ?
C29 F21 1.3388(15) . ?
C29 C30 1.373(2) . ?
C30 F22 1.3435(17) . ?
C30 C31 1.3809(18) . ?
C31 F23 1.3474(15) . ?
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
O3 S O1 116.77(8) . . ?
O3 S O2 116.76(8) . . ?
O1 S O2 106.64(8) . . ?
O3 S C1 109.95(9) . . ?
O1 S C1 101.89(8) . . ?
O2 S C1 102.98(9) . . ?
O1 Si1 C3 99.67(6) . . ?
O1 Si1 C4 102.33(7) . . ?
C3 Si1 C4 115.91(9) . . ?
O1 Si1 C2 104.08(7) . . ?
C3 Si1 C2 115.65(9) . . ?
C4 Si1 C2 115.76(10) . . ?
C6 Si2 C5 117.16(11) . . ?
C6 Si2 O2 105.66(8) . . ?
C5 Si2 O2 97.95(8) . . ?
C6 Si2 C7 114.58(13) . . ?
C5 Si2 C7 114.32(12) . . ?
O2 Si2 C7 104.26(11) . . ?
S O1 Si1 132.16(7) . . ?
S O2 Si2 135.01(8) . . ?
F2 C1 F1 110.10(18) . . ?
F2 C1 F3 111.15(17) . . ?
F1 C1 F3 109.74(15) . . ?
F2 C1 S 110.41(13) . . ?
F1 C1 S 108.30(14) . . ?
F3 C1 S 107.06(15) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C20 B C8 113.44(10) . . ?
C20 B C26 103.22(10) . . ?
C8 B C26 111.98(10) . . ?
C20 B C14 113.28(10) . . ?
C8 B C14 100.98(9) . . ?
C26 B C14 114.37(9) . . ?
C13 C8 C9 112.99(12) . . ?
C13 C8 B 118.51(10) . . ?
C9 C8 B 128.33(11) . . ?
F4 C9 C10 114.84(11) . . ?
F4 C9 C8 120.98(12) . . ?
C10 C9 C8 124.18(12) . . ?
F5 C10 C11 119.72(12) . . ?
F5 C10 C9 120.72(13) . . ?
C11 C10 C9 119.55(12) . . ?
F6 C11 C12 120.29(13) . . ?
F6 C11 C10 120.87(13) . . ?
C12 C11 C10 118.84(12) . . ?
F7 C12 C13 120.67(12) . . ?
F7 C12 C11 119.93(13) . . ?
C13 C12 C11 119.40(13) . . ?
F8 C13 C12 115.96(11) . . ?
F8 C13 C8 119.09(11) . . ?
C12 C13 C8 124.94(12) . . ?
C19 C14 C15 112.92(11) . . ?
C19 C14 B 127.36(11) . . ?
C15 C14 B 119.18(10) . . ?
F9 C15 C16 115.64(11) . . ?
F9 C15 C14 119.44(11) . . ?
C16 C15 C14 124.91(12) . . ?
F10 C16 C17 120.06(12) . . ?
F10 C16 C15 120.66(12) . . ?
C17 C16 C15 119.27(12) . . ?
F11 C17 C18 120.66(13) . . ?
F11 C17 C16 120.54(13) . . ?
C18 C17 C16 118.78(12) . . ?
F12 C18 C17 119.95(12) . . ?
F12 C18 C19 120.07(13) . . ?
C17 C18 C19 119.97(12) . . ?
F13 C19 C18 114.64(11) . . ?
F13 C19 C14 121.20(11) . . ?
C18 C19 C14 124.14(12) . . ?
C21 C20 C25 113.17(11) . . ?
C21 C20 B 127.22(11) . . ?
C25 C20 B 119.47(11) . . ?
F14 C21 C22 114.56(12) . . ?
F14 C21 C20 121.09(11) . . ?
C22 C21 C20 124.33(13) . . ?
F15 C22 C23 120.32(12) . . ?
F15 C22 C21 120.01(13) . . ?
C23 C22 C21 119.63(13) . . ?
F16 C23 C22 120.35(14) . . ?
F16 C23 C24 120.72(14) . . ?
C22 C23 C24 118.93(12) . . ?
F17 C24 C23 120.20(12) . . ?
F17 C24 C25 120.41(13) . . ?
C23 C24 C25 119.38(13) . . ?
F18 C25 C24 116.16(12) . . ?
F18 C25 C20 119.37(11) . . ?
C24 C25 C20 124.46(13) . . ?
C27 C26 C31 113.46(11) . . ?
C27 C26 B 126.61(11) . . ?
C31 C26 B 119.62(11) . . ?
F19 C27 C26 121.66(11) . . ?
F19 C27 C28 114.31(11) . . ?
C26 C27 C28 124.03(12) . . ?
F20 C28 C29 120.01(12) . . ?
F20 C28 C27 120.28(13) . . ?
C29 C28 C27 119.70(12) . . ?
F21 C29 C28 120.58(13) . . ?
F21 C29 C30 120.35(13) . . ?
C28 C29 C30 119.06(12) . . ?
F22 C30 C29 119.60(12) . . ?
F22 C30 C31 121.06(12) . . ?
C29 C30 C31 119.34(12) . . ?
F23 C31 C30 116.35(12) . . ?
F23 C31 C26 119.27(11) . . ?
C30 C31 C26 124.37(12) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S O1 Si1 3.63(14) . . . . ?
O2 S O1 Si1 -128.98(11) . . . . ?
C1 S O1 Si1 123.41(11) . . . . ?
C3 Si1 O1 S -176.83(10) . . . . ?
C4 Si1 O1 S 63.76(13) . . . . ?
C2 Si1 O1 S -57.13(13) . . . . ?
O3 S O2 Si2 6.19(15) . . . . ?
O1 S O2 Si2 138.81(11) . . . . ?
C1 S O2 Si2 -114.36(13) . . . . ?
C6 Si2 O2 S 48.10(16) . . . . ?
C5 Si2 O2 S 169.29(13) . . . . ?
C7 Si2 O2 S -73.03(15) . . . . ?
O3 S C1 F2 -177.53(14) . . . . ?
O1 S C1 F2 57.99(16) . . . . ?
O2 S C1 F2 -52.42(16) . . . . ?
O3 S C1 F1 61.86(13) . . . . ?
O1 S C1 F1 -62.61(13) . . . . ?
O2 S C1 F1 -173.02(11) . . . . ?
O3 S C1 F3 -56.41(15) . . . . ?
O1 S C1 F3 179.12(12) . . . . ?
O2 S C1 F3 68.71(14) . . . . ?
C20 B C8 C13 -174.00(10) . . . . ?
C26 B C8 C13 -57.65(14) . . . . ?
C14 B C8 C13 64.46(13) . . . . ?
C20 B C8 C9 11.06(16) . . . . ?
C26 B C8 C9 127.41(13) . . . . ?
C14 B C8 C9 -110.47(13) . . . . ?
C13 C8 C9 F4 -176.61(10) . . . . ?
B C8 C9 F4 -1.44(18) . . . . ?
C13 C8 C9 C10 3.56(17) . . . . ?
B C8 C9 C10 178.73(11) . . . . ?
F4 C9 C10 F5 -1.97(17) . . . . ?
C8 C9 C10 F5 177.87(11) . . . . ?
F4 C9 C10 C11 177.32(11) . . . . ?
C8 C9 C10 C11 -2.84(19) . . . . ?
F5 C10 C11 F6 -0.08(19) . . . . ?
C9 C10 C11 F6 -179.37(12) . . . . ?
F5 C10 C11 C12 179.39(12) . . . . ?
C9 C10 C11 C12 0.10(19) . . . . ?
F6 C11 C12 F7 0.96(19) . . . . ?
C10 C11 C12 F7 -178.52(12) . . . . ?
F6 C11 C12 C13 -179.03(12) . . . . ?
C10 C11 C12 C13 1.49(19) . . . . ?
F7 C12 C13 F8 -1.24(17) . . . . ?
C11 C12 C13 F8 178.74(11) . . . . ?
F7 C12 C13 C8 179.45(12) . . . . ?
C11 C12 C13 C8 -0.6(2) . . . . ?
C9 C8 C13 F8 178.85(10) . . . . ?
B C8 C13 F8 3.17(16) . . . . ?
C9 C8 C13 C12 -1.86(18) . . . . ?
B C8 C13 C12 -177.54(11) . . . . ?
C20 B C14 C19 131.06(13) . . . . ?
C8 B C14 C19 -107.30(14) . . . . ?
C26 B C14 C19 13.13(17) . . . . ?
C20 B C14 C15 -58.02(15) . . . . ?
C8 B C14 C15 63.62(13) . . . . ?
C26 B C14 C15 -175.95(11) . . . . ?
C19 C14 C15 F9 178.57(11) . . . . ?
B C14 C15 F9 6.39(17) . . . . ?
C19 C14 C15 C16 -0.69(19) . . . . ?
B C14 C15 C16 -172.86(12) . . . . ?
F9 C15 C16 F10 0.70(18) . . . . ?
C14 C15 C16 F10 179.98(12) . . . . ?
F9 C15 C16 C17 -178.46(12) . . . . ?
C14 C15 C16 C17 0.8(2) . . . . ?
F10 C16 C17 F11 -1.2(2) . . . . ?
C15 C16 C17 F11 178.01(12) . . . . ?
F10 C16 C17 C18 -179.46(13) . . . . ?
C15 C16 C17 C18 -0.3(2) . . . . ?
F11 C17 C18 F12 0.5(2) . . . . ?
C16 C17 C18 F12 178.80(13) . . . . ?
F11 C17 C18 C19 -178.57(13) . . . . ?
C16 C17 C18 C19 -0.3(2) . . . . ?
F12 C18 C19 F13 -0.24(19) . . . . ?
C17 C18 C19 F13 178.83(13) . . . . ?
F12 C18 C19 C14 -178.69(13) . . . . ?
C17 C18 C19 C14 0.4(2) . . . . ?
C15 C14 C19 F13 -178.27(11) . . . . ?
B C14 C19 F13 -6.9(2) . . . . ?
C15 C14 C19 C18 0.08(19) . . . . ?
B C14 C19 C18 171.48(12) . . . . ?
C8 B C20 C21 -125.98(12) . . . . ?
C26 B C20 C21 112.62(13) . . . . ?
C14 B C20 C21 -11.61(16) . . . . ?
C8 B C20 C25 58.51(14) . . . . ?
C26 B C20 C25 -62.88(13) . . . . ?
C14 B C20 C25 172.88(10) . . . . ?
C25 C20 C21 F14 175.16(10) . . . . ?
B C20 C21 F14 -0.59(18) . . . . ?
C25 C20 C21 C22 -3.52(17) . . . . ?
B C20 C21 C22 -179.26(12) . . . . ?
F14 C21 C22 F15 1.26(17) . . . . ?
C20 C21 C22 F15 -179.99(11) . . . . ?
F14 C21 C22 C23 -176.43(12) . . . . ?
C20 C21 C22 C23 2.3(2) . . . . ?
F15 C22 C23 F16 2.3(2) . . . . ?
C21 C22 C23 F16 179.95(12) . . . . ?
F15 C22 C23 C24 -177.17(12) . . . . ?
C21 C22 C23 C24 0.5(2) . . . . ?
F16 C23 C24 F17 -0.3(2) . . . . ?
C22 C23 C24 F17 179.16(12) . . . . ?
F16 C23 C24 C25 178.82(12) . . . . ?
C22 C23 C24 C25 -1.7(2) . . . . ?
F17 C24 C25 F18 0.58(18) . . . . ?
C23 C24 C25 F18 -178.52(11) . . . . ?
F17 C24 C25 C20 179.42(11) . . . . ?
C23 C24 C25 C20 0.3(2) . . . . ?
C21 C20 C25 F18 -179.00(10) . . . . ?
B C20 C25 F18 -2.89(16) . . . . ?
C21 C20 C25 C24 2.18(18) . . . . ?
B C20 C25 C24 178.29(11) . . . . ?
C20 B C26 C27 107.10(13) . . . . ?
C8 B C26 C27 -15.27(16) . . . . ?
C14 B C26 C27 -129.38(12) . . . . ?
C20 B C26 C31 -66.17(13) . . . . ?
C8 B C26 C31 171.45(10) . . . . ?
C14 B C26 C31 57.35(14) . . . . ?
C31 C26 C27 F19 178.08(11) . . . . ?
B C26 C27 F19 4.45(18) . . . . ?
C31 C26 C27 C28 -1.62(18) . . . . ?
B C26 C27 C28 -175.25(12) . . . . ?
F19 C27 C28 F20 1.30(18) . . . . ?
C26 C27 C28 F20 -178.98(12) . . . . ?
F19 C27 C28 C29 -179.64(12) . . . . ?
C26 C27 C28 C29 0.1(2) . . . . ?
F20 C28 C29 F21 -0.1(2) . . . . ?
C27 C28 C29 F21 -179.16(12) . . . . ?
F20 C28 C29 C30 -179.93(13) . . . . ?
C27 C28 C29 C30 1.0(2) . . . . ?
F21 C29 C30 F22 0.3(2) . . . . ?
C28 C29 C30 F22 -179.86(12) . . . . ?
F21 C29 C30 C31 179.74(12) . . . . ?
C28 C29 C30 C31 -0.4(2) . . . . ?
F22 C30 C31 F23 -0.98(18) . . . . ?
C29 C30 C31 F23 179.60(11) . . . . ?
F22 C30 C31 C26 178.11(12) . . . . ?
C29 C30 C31 C26 -1.3(2) . . . . ?
C27 C26 C31 F23 -178.69(10) . . . . ?
B C26 C31 F23 -4.57(16) . . . . ?
C27 C26 C31 C30 2.24(18) . . . . ?
B C26 C31 C30 176.36(11) . . . . ?
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full 29.99
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max 0.392
_refine_diff_density_min -0.446
_refine_diff_density_rms 0.054
#===================== End of CIF submission =================================