#------------------------------------------------------------------------------
#$Date: 2023-05-06 11:47:15 +0100 (Sat, 06 May 2023) $
#$Revision: 283588 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244240.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2244240
loop_
_publ_author_name
'Wappelhorst, Jan Frederick'
'Wattenberg, Jonathan'
'Strohmann, Carsten'
_publ_section_title
;
Crystal structure of
trimeth-yl({tris-[(phenyl-sulfan-yl)meth-yl]sil-yl}meth-oxy)silane and
Hirshfeld surface analysis of 3-bromo-2,2-bis-(bromo-meth-yl)propan-1-ol.
;
_journal_coeditor_code VM2278
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 323
_journal_page_last 327
_journal_paper_doi 10.1107/S205698902300227X
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C26 H32 O S3 Si'
_chemical_formula_moiety 'C26 H32 O S3 Si'
_chemical_formula_sum 'C26 H32 O S3 Si'
_chemical_formula_weight 484.78
_chemical_name_systematic
;
Trimethyl({tris[(phenylsulfanyl)methyl]silyl}methoxy)silane
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha 90
_cell_angle_beta 96.939(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.0415(12)
_cell_length_b 6.9329(3)
_cell_length_c 27.7963(14)
_cell_measurement_reflns_used 9874
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 31.03
_cell_measurement_theta_min 2.24
_cell_volume 5173.0(4)
_computing_cell_refinement
;
SAINT V8.38A (Bruker, 2018)
;
_computing_data_reduction
;
SAINT V8.38A (Bruker, 2018)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'HELIOS mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0353
_diffrn_reflns_av_unetI/netI 0.0282
_diffrn_reflns_limit_h_max 39
_diffrn_reflns_limit_h_min -39
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 40629
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.049
_diffrn_reflns_theta_min 2.241
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.349
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.6714
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.245
_exptl_crystal_description block
_exptl_crystal_F_000 2064
_exptl_crystal_size_max 0.619
_exptl_crystal_size_mid 0.562
_exptl_crystal_size_min 0.457
_refine_diff_density_max 0.355
_refine_diff_density_min -0.241
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 340
_refine_ls_number_reflns 8253
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.031
_refine_ls_R_factor_all 0.0424
_refine_ls_R_factor_gt 0.0319
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+3.6217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0711
_refine_ls_wR_factor_ref 0.0773
_reflns_number_gt 6927
_reflns_number_total 8253
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2278sup1.cif
_cod_data_source_block 3
_cod_depositor_comments
'Adding full bibliography for 2244239--2244240.cif.'
_cod_database_code 2244240
_cod_database_fobs_code 2244240
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.813
_shelx_estimated_absorpt_t_max 0.857
_shelx_hkl_file
;
4 0 0 110.19 3.10
4 0 0 108.69 2.70
4 0 0 109.49 2.70
-4 0 0 109.59 2.80
-4 0 0 110.59 2.70
-4 0 0 105.89 3.30
-4 0 0 114.19 3.10
6 0 0 332.37 8.00
6 0 0 341.27 7.70
6 0 0 331.87 6.90
-6 0 0 334.27 7.60
-6 0 0 330.47 8.00
-6 0 0 341.37 6.90
6 0 0 327.87 6.90
-6 0 0 330.27 7.00
-8 0 0 7088.99 135.39
8 0 0 6665.63 134.99
-10 0 0 325.67 8.60
10 0 0 320.07 7.90
10 0 0 332.87 9.50
10 0 0 334.27 8.90
-10 0 0 334.77 8.10
-10 0 0 330.07 7.60
-10 0 0 320.97 8.00
-12 0 0 1151.88 21.90
-12 0 0 1159.98 22.90
12 0 0 1127.39 24.00
-12 0 0 1085.69 23.90
-12 0 0 1176.18 21.20
-12 0 0 1145.39 24.00
12 0 0 1141.89 21.80
14 0 0 27.10 2.50
-14 0 0 26.60 2.80
-14 0 0 23.70 2.00
-14 0 0 26.30 2.00
14 0 0 20.90 2.00
-14 0 0 22.10 2.10
-14 0 0 24.10 2.30
16 0 0 699.13 16.40
16 0 0 751.02 18.00
-16 0 0 720.13 17.30
-16 0 0 709.93 19.00
-16 0 0 715.73 15.80
-16 0 0 761.82 15.80
-16 0 0 733.03 16.50
-18 0 0 1.10 1.00
-18 0 0 1.20 0.80
-18 0 0 1.90 0.90
18 0 0 1.10 0.90
-20 0 0 4728.83 86.79
20 0 0 4781.42 83.99
-20 0 0 4764.62 80.39
-22 0 0 1895.71 43.30
22 0 0 2042.90 41.50
-22 0 0 2027.40 37.90
24 0 0 12.90 2.70
-24 0 0 7.40 1.80
-24 0 0 9.10 2.70
26 0 0 106.69 7.20
-26 0 0 105.29 8.40
-26 0 0 98.69 5.80
-28 0 0 123.39 6.90
-28 0 0 132.79 9.90
28 0 0 130.99 8.40
30 0 0 6.90 2.40
-30 0 0 4.10 1.90
32 0 0 28.80 4.80
-32 0 0 28.10 4.30
34 0 0 8.10 2.90
-34 0 0 6.30 2.50
36 0 0 5.90 2.80
-36 0 0 2.40 2.60
-38 0 0 76.09 7.30
-1 -1 0 35.90 1.40
1 -1 0 33.20 1.20
1 -1 0 33.30 1.70
-1 -1 0 32.80 1.50
1 -1 0 36.10 1.80
1 1 0 32.20 1.30
-1 1 0 36.20 1.20
1 1 0 32.80 1.70
1 1 0 31.40 1.50
-1 1 0 28.50 1.60
-3 -1 0 479.35 8.90
3 -1 0 484.75 10.30
3 -1 0 455.35 10.30
3 -1 0 465.55 10.00
-3 -1 0 487.95 8.90
3 -1 0 475.55 9.40
-3 1 0 468.35 10.30
-3 1 0 480.55 10.10
3 1 0 512.85 9.00
-3 1 0 477.45 9.40
3 1 0 497.95 8.80
-3 1 0 473.75 10.00
5 -1 0 13.50 1.30
-5 -1 0 11.20 1.10
-5 -1 0 11.90 0.80
5 -1 0 10.20 1.10
5 -1 0 12.20 1.50
5 -1 0 12.30 1.30
-5 1 0 10.00 1.10
5 1 0 11.20 1.00
5 1 0 10.60 0.90
-5 1 0 13.00 1.40
-5 1 0 12.00 1.20
-5 1 0 11.30 1.20
7 -1 0 457.25 11.60
7 -1 0 445.96 10.90
-7 -1 0 482.35 9.70
7 -1 0 451.55 10.90
7 -1 0 487.85 10.80
-7 1 0 477.85 11.10
7 1 0 463.45 8.90
7 1 0 472.05 8.60
7 1 0 470.35 10.40
-7 1 0 470.45 10.60
-7 1 0 450.35 10.90
-7 1 0 478.65 11.50
7 1 0 496.95 8.40
9 -1 0 243.98 7.50
-9 -1 0 246.38 6.30
9 -1 0 245.18 8.20
9 -1 0 227.68 8.30
-9 -1 0 218.78 8.60
-9 1 0 247.98 7.00
9 1 0 253.27 5.80
9 1 0 242.88 7.20
-9 1 0 247.98 8.00
9 1 0 246.48 5.50
-9 1 0 253.47 7.80
-9 1 0 251.57 7.50
-11 -1 0 220.58 5.40
11 -1 0 220.58 7.10
11 -1 0 215.88 7.40
11 -1 0 232.58 8.00
-11 -1 0 224.28 6.30
-11 -1 0 223.78 7.60
11 -1 0 225.78 8.20
11 1 0 220.88 6.00
11 1 0 222.98 5.50
-11 1 0 213.98 6.70
11 1 0 216.18 7.40
-11 1 0 224.08 7.40
-11 1 0 206.28 7.60
13 -1 0 147.59 6.90
-13 -1 0 138.29 6.30
-13 -1 0 142.19 5.30
13 -1 0 141.99 5.70
-13 -1 0 155.28 4.60
13 -1 0 140.49 6.10
-13 1 0 146.49 6.60
-13 1 0 154.08 6.90
13 1 0 150.28 4.60
13 1 0 128.69 9.30
-13 1 0 136.59 5.30
13 1 0 149.59 5.20
-13 1 0 148.49 6.10
-15 -1 0 6.00 1.10
15 -1 0 4.80 1.40
-15 -1 0 2.40 1.10
15 -1 0 3.80 1.20
-15 -1 0 11.20 1.70
-15 1 0 4.10 1.30
-15 1 0 5.80 1.30
15 1 0 5.40 1.20
15 1 0 4.90 1.00
-17 -1 0 1064.49 25.00
-17 -1 0 1003.60 20.30
-17 -1 0 1010.00 21.30
17 -1 0 1045.20 25.10
17 -1 0 1046.80 22.30
17 1 0 1049.00 21.80
-17 1 0 1041.70 21.70
-17 1 0 1049.89 25.30
17 1 0 998.10 20.50
19 -1 0 360.86 13.10
-19 -1 0 349.37 9.70
-19 -1 0 349.96 13.10
-19 -1 0 377.26 10.80
-19 1 0 366.66 11.50
-19 1 0 347.17 13.50
19 1 0 352.06 10.80
-19 1 0 363.36 10.60
-21 -1 0 169.98 9.30
-21 -1 0 167.88 6.50
21 -1 0 167.78 9.00
-21 -1 0 168.98 7.10
21 1 0 175.38 7.50
-21 1 0 168.98 9.40
-21 1 0 176.48 7.10
-21 1 0 167.18 7.50
-23 -1 0 40.60 3.60
23 -1 0 45.50 6.90
-23 -1 0 47.50 5.10
-23 -1 0 40.00 5.30
-23 1 0 42.90 3.60
-23 1 0 42.10 4.90
23 1 0 45.50 4.00
-23 1 0 50.29 4.10
-25 -1 0 74.69 6.80
25 -1 0 69.09 6.30
-25 -1 0 72.69 5.10
25 1 0 64.19 5.00
-25 1 0 69.49 4.70
-25 1 0 64.09 6.50
-27 -1 0 104.59 10.30
27 -1 0 112.19 8.30
-27 1 0 117.29 6.60
27 1 0 114.59 6.90
-27 1 0 87.09 7.80
-29 -1 0 505.55 16.20
29 -1 0 479.35 18.80
29 1 0 488.25 16.00
-29 1 0 462.45 20.00
-29 1 0 485.15 15.20
-31 -1 0 56.79 5.60
31 -1 0 52.29 6.20
31 1 0 44.50 5.20
-31 1 0 56.49 5.00
-33 -1 0 7.90 2.90
33 -1 0 7.20 2.70
33 1 0 5.40 2.10
-33 1 0 5.90 2.40
35 -1 0 2.30 2.40
-35 -1 0 3.80 2.70
-35 1 0 -0.30 1.60
35 1 0 -2.10 2.40
-37 -1 0 112.09 9.30
37 -1 0 132.49 10.60
-37 1 0 104.49 8.20
0 2 0 9999.00 180.28
2 -2 0 348.07 9.70
2 -2 0 354.56 9.30
2 -2 0 343.87 7.50
-2 -2 0 360.86 8.10
-2 -2 0 358.26 8.60
2 -2 0 353.46 9.20
2 2 0 352.46 8.60
-2 2 0 356.26 9.40
2 2 0 357.46 9.10
-2 2 0 348.07 9.30
2 2 0 358.76 7.90
-2 2 0 359.26 7.20
-2 2 0 356.86 9.20
4 -2 0 1018.50 21.70
4 -2 0 1096.79 19.80
4 -2 0 930.81 23.80
-4 -2 0 1076.49 18.40
-4 -2 0 1075.09 19.70
4 -2 0 1059.29 22.00
4 2 0 1078.79 18.20
-4 2 0 1016.00 23.80
4 2 0 1094.29 19.80
4 2 0 1095.99 18.10
-4 2 0 1076.79 19.40
-4 2 0 1099.59 21.70
6 -2 0 388.36 10.50
6 -2 0 384.36 9.60
-6 -2 0 394.66 8.60
6 -2 0 399.06 11.20
-6 2 0 384.06 10.60
-6 2 0 384.16 10.90
6 2 0 385.16 8.40
6 2 0 392.36 8.50
-6 2 0 379.16 9.40
-6 2 0 379.76 10.30
-8 -2 0 208.28 5.40
-8 -2 0 188.08 6.00
8 -2 0 202.78 7.90
8 -2 0 198.18 6.80
8 -2 0 195.38 7.10
-8 2 0 185.18 6.50
-8 2 0 200.58 7.70
-8 2 0 188.68 7.20
8 2 0 199.28 5.60
8 2 0 217.08 6.10
10 -2 0 455.85 12.20
10 -2 0 427.06 12.00
10 -2 0 442.66 13.30
-10 -2 0 455.25 9.50
-10 -2 0 433.26 11.30
-10 2 0 440.26 12.00
-10 2 0 451.55 13.00
-10 2 0 435.86 11.80
10 2 0 437.86 11.00
10 2 0 447.46 9.50
12 -2 0 233.48 9.60
-12 -2 0 243.08 6.20
12 -2 0 233.58 8.40
-12 -2 0 242.28 8.30
12 2 0 230.28 7.80
-12 2 0 219.68 7.90
12 2 0 234.58 5.90
-12 2 0 240.98 8.80
-14 -2 0 13.40 2.40
14 -2 0 14.80 2.70
14 -2 0 13.20 2.20
-14 -2 0 16.40 1.50
-14 2 0 17.50 2.10
-14 2 0 18.80 3.10
14 2 0 18.90 1.40
-16 -2 0 40.50 2.50
16 -2 0 36.90 3.40
16 -2 0 37.10 4.00
-16 -2 0 40.70 2.10
-16 -2 0 38.20 3.50
-16 2 0 38.60 3.80
-16 2 0 33.40 3.00
16 2 0 33.30 2.00
18 -2 0 33.70 4.20
-18 -2 0 32.70 2.00
-18 -2 0 31.60 3.60
18 -2 0 25.90 2.90
-18 -2 0 25.80 2.20
-18 -2 0 32.00 3.10
18 2 0 27.60 2.10
-18 2 0 25.40 6.20
-18 2 0 28.40 2.90
18 2 0 31.90 2.20
20 -2 0 176.38 8.00
-20 -2 0 168.38 7.50
-20 -2 0 179.38 6.30
-20 -2 0 184.58 10.40
-20 -2 0 191.98 5.90
20 -2 0 190.18 10.10
20 2 0 187.68 6.60
-20 2 0 171.08 9.40
-20 2 0 178.08 7.60
20 2 0 169.98 6.20
-22 -2 0 190.58 6.40
22 -2 0 210.38 9.10
22 -2 0 219.38 11.20
-22 -2 0 201.88 8.60
-22 2 0 196.98 9.10
22 2 0 199.48 7.10
-22 2 0 203.68 10.80
-22 2 0 186.98 8.10
24 -2 0 38.50 5.00
-24 -2 0 44.20 4.10
-24 2 0 34.00 3.60
-24 2 0 43.00 5.20
24 2 0 35.60 3.10
-24 2 0 44.30 4.40
-26 -2 0 223.58 10.00
-26 -2 0 238.18 8.20
26 -2 0 242.38 12.90
-26 -2 0 225.28 7.80
-26 2 0 224.18 10.30
26 2 0 228.68 8.50
-26 2 0 221.48 12.60
-26 2 0 246.08 9.80
28 -2 0 83.69 7.70
-28 -2 0 75.49 6.10
-28 -2 0 88.99 4.90
-28 2 0 85.19 9.00
-28 2 0 89.89 6.00
-28 2 0 79.09 6.00
28 2 0 82.49 5.00
30 -2 0 1.10 2.30
-30 -2 0 1.40 1.50
-30 2 0 -2.10 1.50
30 2 0 0.60 1.30
-30 2 0 -0.20 1.40
32 -2 0 25.00 5.20
-32 2 0 19.20 3.50
34 -2 0 29.50 6.00
-34 2 0 20.00 3.80
36 -2 0 16.00 4.70
-36 2 0 10.70 3.30
38 -2 0 -1.60 3.00
-38 2 0 0.70 2.30
-1 -3 0 575.04 13.30
1 -3 0 548.85 14.80
1 -3 0 547.75 11.00
-1 -3 0 564.54 13.60
-1 -3 0 561.04 15.10
1 -3 0 525.25 13.70
1 -3 0 557.74 13.90
1 3 0 566.54 14.20
-1 3 0 530.15 13.40
-1 3 0 550.44 10.10
1 3 0 567.44 12.90
-1 3 0 553.74 14.20
1 3 0 561.44 15.70
-1 3 0 556.54 14.30
3 -3 0 245.38 9.10
-3 -3 0 205.28 10.60
-3 -3 0 237.48 7.20
3 -3 0 243.48 8.60
3 -3 0 241.58 6.60
3 -3 0 236.48 8.30
-3 3 0 252.77 8.60
-3 3 0 242.08 6.00
-3 3 0 249.18 8.40
3 3 0 235.98 6.70
-3 3 0 239.38 8.60
3 3 0 236.98 7.60
3 3 0 211.48 11.60
5 -3 0 206.48 8.30
5 -3 0 205.38 7.90
5 -3 0 201.28 6.50
-5 -3 0 206.48 5.70
-5 -3 0 206.58 6.70
5 -3 0 217.68 10.10
5 3 0 210.38 5.50
-5 3 0 205.48 8.00
-5 3 0 213.28 6.20
5 3 0 215.88 7.50
5 3 0 207.08 6.80
-5 3 0 208.98 8.00
5 3 0 209.28 4.70
7 -3 0 254.67 8.10
7 -3 0 270.27 9.40
-7 -3 0 259.07 7.40
7 -3 0 270.57 10.10
7 3 0 253.27 7.40
-7 3 0 246.98 9.00
7 3 0 257.27 6.40
-7 3 0 259.87 7.80
7 3 0 249.48 8.30
9 -3 0 191.98 7.90
-9 -3 0 170.38 6.80
9 -3 0 187.28 7.20
9 -3 0 173.28 8.30
9 3 0 184.08 5.70
-9 3 0 180.48 6.80
9 3 0 179.58 5.70
-9 3 0 183.58 7.60
11 -3 0 149.19 7.10
11 -3 0 126.79 7.40
-11 -3 0 134.99 4.80
11 3 0 139.19 5.40
11 3 0 135.59 5.00
-11 3 0 138.29 6.30
-13 -3 0 928.51 17.90
13 -3 0 923.91 22.30
13 -3 0 921.91 24.40
-13 3 0 904.91 21.70
-13 3 0 922.71 22.00
13 3 0 925.01 18.00
13 3 0 899.81 20.10
15 -3 0 56.59 5.30
15 -3 0 54.59 4.50
-15 -3 0 52.59 2.70
-15 3 0 45.20 3.90
-15 3 0 49.40 4.20
15 3 0 56.09 2.70
17 -3 0 90.59 6.00
17 -3 0 91.79 7.10
-17 -3 0 91.39 3.70
-17 3 0 80.19 5.30
-17 3 0 86.99 6.40
17 3 0 90.29 3.60
19 -3 0 62.39 5.20
19 -3 0 60.39 6.00
19 3 0 55.59 2.90
-19 3 0 66.19 5.60
-19 3 0 57.59 4.60
21 -3 0 94.69 6.40
21 -3 0 84.29 7.40
21 3 0 82.89 4.00
-21 3 0 87.49 6.90
-21 3 0 83.19 5.70
23 -3 0 23.70 4.00
23 -3 0 26.10 5.10
-23 3 0 24.30 4.60
-23 3 0 24.80 3.80
25 -3 0 0.90 1.80
25 -3 0 1.20 1.80
-25 3 0 3.10 2.00
-25 3 0 3.40 2.10
-25 3 0 2.20 1.60
27 -3 0 9.90 3.60
-27 3 0 6.30 2.50
-27 3 0 11.90 2.70
29 -3 0 28.40 5.80
-29 3 0 31.70 6.90
-29 3 0 18.80 4.90
-29 3 0 21.80 3.60
31 -3 0 19.60 5.10
-31 3 0 21.00 3.90
33 -3 0 -3.50 2.30
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17 -3 -9 297.67 13.90
-17 -3 9 296.87 11.50
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15 -3 -9 192.38 10.70
-15 3 9 183.88 7.70
-13 -3 9 61.29 3.50
-13 -3 9 75.99 5.30
13 -3 -9 81.89 6.60
-13 3 9 68.99 4.40
-11 -3 9 13.00 2.00
11 -3 -9 16.70 3.50
-11 -3 9 10.30 2.30
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9 -3 -9 227.78 10.60
-9 -3 9 241.38 8.00
9 -3 -9 194.88 9.70
-9 -3 9 255.07 10.00
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7 -3 -9 747.63 20.90
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7 3 -9 742.23 20.80
5 -3 -9 13.10 2.70
-5 -3 9 14.70 2.70
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3 -3 -9 955.10 22.80
3 -3 -9 974.00 23.80
3 -3 -9 982.60 20.70
-3 3 9 968.30 19.20
3 3 -9 981.30 24.10
-1 -3 9 488.25 14.90
-1 -3 9 476.75 15.20
1 -3 -9 477.85 12.00
1 -3 -9 497.85 14.70
1 -3 -9 488.15 13.70
1 3 -9 464.55 14.70
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-1 3 9 485.35 10.80
1 -3 9 330.57 12.50
-1 -3 -9 355.26 11.70
-1 -3 -9 338.77 9.00
-1 -3 -9 348.97 10.60
1 -3 9 340.37 12.20
-1 3 -9 336.27 11.90
1 3 9 345.87 9.50
1 3 9 332.77 10.90
-1 3 -9 319.97 12.70
1 3 9 340.37 7.90
3 -3 9 15.10 2.70
3 -3 9 11.00 2.40
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3 -3 9 12.70 2.70
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-5 -3 -9 212.78 5.90
5 -3 9 211.58 9.40
5 -3 9 214.08 9.20
-5 -3 -9 223.18 7.80
-5 -3 -9 221.28 8.40
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5 3 9 206.28 7.90
5 3 9 209.48 6.20
-5 3 -9 210.08 9.90
-7 -3 -9 33.80 2.80
-7 -3 -9 29.80 2.90
7 -3 9 32.10 3.60
7 -3 9 26.70 3.30
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7 3 9 34.40 2.90
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9 -3 9 68.89 5.30
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11 -3 9 29.10 3.80
-11 -3 -9 23.40 2.60
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13 -3 9 104.09 8.40
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13 -3 9 95.79 7.00
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15 -3 9 19.20 3.40
-15 -3 -9 20.20 3.10
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17 -3 9 61.49 5.20
17 -3 9 63.69 6.10
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-19 -3 -9 171.68 8.80
19 -3 9 181.98 9.50
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21 -3 9 0.20 1.40
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23 -3 9 0.70 1.60
-23 -3 -9 5.80 2.40
23 -3 9 4.20 2.20
-23 3 -9 4.90 2.50
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25 -3 9 46.60 7.90
25 -3 9 33.40 5.00
-25 -3 -9 41.10 5.00
-25 3 -9 27.00 4.90
25 3 9 41.00 3.20
-25 3 -9 36.30 4.40
27 -3 9 3.90 2.00
-27 -3 -9 0.90 1.80
27 -3 9 5.90 2.10
-27 3 -9 4.40 2.40
27 3 9 5.00 1.60
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29 -3 9 31.00 6.10
-29 -3 -9 34.60 5.90
29 -3 9 36.20 6.50
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31 -3 9 11.50 4.60
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31 -3 9 22.30 4.10
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33 -3 9 4.50 3.30
-33 -3 -9 3.70 3.10
33 -3 9 0.70 2.10
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35 -3 9 -0.10 3.40
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34 -4 -9 26.60 11.00
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32 -4 -9 131.19 12.30
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-30 -4 9 19.20 4.10
30 -4 -9 23.70 6.50
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28 -4 -9 4.60 3.50
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26 -4 -9 18.50 4.90
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24 -4 -9 7.10 5.10
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22 -4 -9 48.00 7.50
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20 -4 -9 278.77 15.10
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18 -4 -9 158.78 11.00
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16 -4 -9 166.28 10.70
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-14 -4 9 264.37 7.20
-14 -4 9 249.88 7.20
-14 -4 9 278.07 11.40
14 -4 -9 259.67 13.20
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-12 -4 9 1069.89 21.90
-12 -4 9 1117.39 27.00
-12 -4 9 1051.89 21.20
12 -4 -9 1082.79 29.90
-12 4 9 1075.89 24.30
-10 -4 9 318.87 12.30
-10 -4 9 300.57 9.40
10 -4 -9 300.97 13.60
-10 -4 9 306.47 9.10
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8 -4 -9 6.20 1.40
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8 -4 -9 5.30 2.10
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6 -4 -9 21.70 2.20
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6 -4 -9 24.30 4.00
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4 -4 -9 356.56 13.50
4 4 -9 358.36 12.70
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2 -4 -9 267.87 9.30
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2 -4 -9 281.27 11.40
-2 -4 9 257.37 9.80
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0 -4 -9 12.60 2.20
0 -4 9 12.10 2.80
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0 -4 9 13.70 2.70
0 -4 -9 12.70 2.10
0 -4 -9 13.80 2.70
0 4 -9 11.60 2.80
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2 -4 9 257.17 11.10
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4 -4 9 73.29 5.50
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6 -4 9 67.49 5.50
-6 -4 -9 64.89 4.60
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8 -4 9 513.15 17.40
8 -4 9 508.85 17.30
-8 -4 -9 496.55 14.00
-8 -4 -9 520.95 12.40
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10 -4 9 238.38 11.50
10 -4 9 236.28 11.10
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12 -4 9 220.08 10.90
12 -4 9 202.08 10.90
-12 -4 -9 203.88 7.60
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-12 4 -9 194.68 10.50
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14 -4 9 6.20 2.30
-14 -4 -9 9.20 2.10
14 -4 9 6.10 2.30
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16 -4 9 13.30 3.40
-16 -4 -9 13.00 2.50
16 -4 9 16.40 4.00
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18 -4 9 65.89 6.10
18 -4 9 64.29 6.90
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20 -4 9 1.40 1.60
20 -4 9 0.40 1.30
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24 -4 9 1.10 2.70
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26 -4 9 25.80 5.70
26 -4 9 21.40 4.40
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28 -4 9 -0.40 1.80
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32 -4 9 6.80 4.80
32 -4 9 2.00 1.80
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29 -5 -9 2.00 2.80
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23 -5 -9 250.67 15.80
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21 -5 -9 4.40 2.60
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19 -5 -9 5.80 2.90
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17 -5 -9 652.33 24.60
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-17 5 9 648.24 18.80
15 -5 -9 600.14 22.90
-15 -5 9 577.74 18.70
-15 5 9 615.74 17.70
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13 -5 -9 0.80 2.00
-13 -5 9 0.60 0.90
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11 -5 -9 10.10 3.30
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11 -5 -9 10.00 2.80
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7 -5 -9 220.98 7.50
-7 -5 9 231.28 11.70
7 -5 -9 223.48 11.80
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5 -5 -9 133.69 9.30
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5 -5 -9 140.89 5.20
5 -5 -9 128.19 10.90
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3 -5 -9 25.20 4.50
3 -5 -9 26.00 3.60
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1 -5 -9 83.29 6.40
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1 -5 -9 83.89 5.10
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1 5 -9 86.09 5.40
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1 -5 9 245.38 10.80
1 -5 9 241.78 10.80
1 -5 9 267.27 12.20
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3 -5 9 252.17 12.00
-3 -5 -9 258.17 10.90
3 -5 9 257.37 14.70
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-5 -5 -9 219.38 9.60
5 -5 9 231.28 11.20
5 -5 9 231.58 11.60
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9 -5 9 339.67 14.80
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11 -5 9 45.40 5.30
11 -5 9 41.30 5.10
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13 -5 9 46.50 5.60
13 -5 9 53.29 5.70
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15 -5 9 23.20 4.40
-15 -5 -9 30.80 3.10
15 -5 9 20.90 4.80
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-15 5 -9 30.90 3.90
17 -5 9 92.09 8.60
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19 -5 9 95.69 8.90
19 -5 9 91.59 8.70
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29 -5 9 2.70 4.30
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14 -6 -9 39.50 5.80
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12 -6 -9 29.40 5.60
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10 -6 -9 141.19 10.40
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6 -6 -9 71.49 4.70
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4 -6 9 499.75 18.40
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12 -6 9 6.00 2.70
12 -6 9 10.40 3.20
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14 -6 9 13.40 3.40
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16 -6 9 -1.00 2.00
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22 -6 9 83.59 9.80
22 -6 9 62.09 7.30
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7 -3 -36 140.49 15.00
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7 3 -36 110.19 25.00
5 -3 -36 32.50 8.70
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1 -3 -36 8.50 5.30
1 3 -36 4.10 5.60
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6 -2 -38 16.10 6.30
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0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 33076
_shelx_res_file
;
b1352_0m.res created by SHELXL-2014/7
TITL b1352_0m_a.res in C2/c
REM Old TITL B1352_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.203, Rweak 0.007, Alpha 0.040, Orientation as input
REM Formula found by SHELXT: C25' O Si S3
CELL 0.71073 27.0415 6.9329 27.7963 90 96.939 90
ZERR 8 0.0012 0.0003 0.0014 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H O S Si
UNIT 208 256 8 24 8
L.S. 25
PLAN 8
SIZE 0.457 0.619 0.562
TEMP -173.15
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 0 0 4
REM
REM
REM
WGHT 0.027300 3.621700
FVAR 0.24743 0.49113
S1 4 0.293968 0.491361 0.538262 11.00000 0.01888 0.01749 =
0.01825 -0.00230 0.00277 -0.00061
S2 4 0.202381 0.781501 0.582692 11.00000 0.01735 0.03543 =
0.01493 -0.00211 0.00136 0.00120
S3 4 0.312158 1.146051 0.662845 11.00000 0.03324 0.02129 =
0.02207 -0.00615 0.00528 -0.00472
C8 1 0.304832 0.807435 0.603581 11.00000 0.01675 0.01620 =
0.01403 0.00046 0.00198 -0.00051
C7 1 0.306557 0.746422 0.550364 11.00000 0.01910 0.01699 =
0.01532 -0.00015 0.00216 -0.00017
AFIX 23
H7A 2 0.339926 0.777510 0.541249 11.00000 -1.20000
H7B 2 0.281862 0.823848 0.529384 11.00000 -1.20000
AFIX 0
C9 1 0.258311 0.729951 0.623892 11.00000 0.01824 0.01889 =
0.01448 -0.00015 0.00248 -0.00099
AFIX 23
H9A 2 0.255574 0.790369 0.655733 11.00000 -1.20000
H9B 2 0.261536 0.588858 0.628788 11.00000 -1.20000
AFIX 0
C16 1 0.305943 1.029927 0.603643 11.00000 0.02643 0.01735 =
0.01740 -0.00064 0.00581 -0.00184
AFIX 23
H16A 2 0.274866 1.076836 0.584795 11.00000 -1.20000
H16B 2 0.334031 1.072382 0.586435 11.00000 -1.20000
AFIX 0
C1 1 0.349507 0.394568 0.520763 11.00000 0.02336 0.02066 =
0.01563 -0.00037 0.00298 0.00350
C23 1 0.349882 0.725984 0.635685 11.00000 0.01782 0.02263 =
0.01771 -0.00099 0.00042 0.00003
C15 1 0.160045 0.700469 0.667013 11.00000 0.02247 0.02764 =
0.02444 -0.00263 0.00613 -0.00243
AFIX 43
H15 2 0.191368 0.650322 0.680526 11.00000 -1.20000
AFIX 0
C2 1 0.344093 0.232149 0.490743 11.00000 0.03075 0.02265 =
0.02246 -0.00400 0.00635 -0.00035
AFIX 43
H2 2 0.311743 0.185722 0.479324 11.00000 -1.20000
AFIX 0
C6 1 0.397217 0.462795 0.536799 11.00000 0.02285 0.03399 =
0.02552 -0.00906 0.00015 0.00405
AFIX 43
H6 2 0.401430 0.572807 0.557260 11.00000 -1.20000
AFIX 0
C17 1 0.250896 1.148667 0.679596 11.00000 0.03772 0.01573 =
0.02457 -0.00485 0.01025 -0.00084
C10 1 0.154402 0.773258 0.620289 11.00000 0.01798 0.02955 =
0.02188 -0.00655 0.00386 -0.00234
C22 1 0.243942 1.079873 0.725567 11.00000 0.04708 0.02246 =
0.02182 -0.00618 0.00951 -0.00351
AFIX 43
H22 2 0.271185 1.025764 0.745909 11.00000 -1.20000
AFIX 0
C18 1 0.210564 1.224185 0.649604 11.00000 0.04090 0.01917 =
0.03356 0.00026 0.01131 0.00430
AFIX 43
H18 2 0.214955 1.271219 0.618300 11.00000 -1.20000
AFIX 0
C14 1 0.120174 0.700215 0.694333 11.00000 0.02991 0.04321 =
0.02814 -0.00383 0.01290 -0.00804
AFIX 43
H14 2 0.124497 0.651476 0.726510 11.00000 -1.20000
AFIX 0
C3 1 0.385772 0.138545 0.477570 11.00000 0.04262 0.02797 =
0.03058 -0.00721 0.01024 0.00540
AFIX 43
H3 2 0.381821 0.027207 0.457552 11.00000 -1.20000
AFIX 0
C21 1 0.197427 1.090373 0.741554 11.00000 0.05799 0.02753 =
0.03133 -0.00973 0.02287 -0.00672
AFIX 43
H21 2 0.192984 1.045506 0.773039 11.00000 -1.20000
AFIX 0
C5 1 0.438550 0.368884 0.522668 11.00000 0.02304 0.05100 =
0.03677 -0.01080 0.00207 0.00782
AFIX 43
H5 2 0.470981 0.416678 0.533192 11.00000 -1.20000
AFIX 0
C11 1 0.107973 0.845272 0.600584 11.00000 0.02060 0.05934 =
0.02591 -0.00504 0.00046 0.00444
AFIX 43
H11 2 0.103592 0.896170 0.568621 11.00000 -1.20000
AFIX 0
C4 1 0.433061 0.206431 0.493424 11.00000 0.03474 0.04460 =
0.03466 -0.00673 0.00795 0.01633
AFIX 43
H4 2 0.461549 0.142208 0.484338 11.00000 -1.20000
AFIX 0
C20 1 0.157506 1.165945 0.711805 11.00000 0.04951 0.02588 =
0.05457 -0.01264 0.03021 -0.00091
AFIX 43
H20 2 0.125682 1.173834 0.722887 11.00000 -1.20000
AFIX 0
C19 1 0.163971 1.230474 0.665598 11.00000 0.04029 0.02462 =
0.05221 -0.00401 0.01303 0.00869
AFIX 43
H19 2 0.136283 1.279174 0.644863 11.00000 -1.20000
AFIX 0
C13 1 0.074371 0.770606 0.674789 11.00000 0.02123 0.07420 =
0.03964 -0.01332 0.01357 -0.00589
AFIX 43
H13 2 0.047097 0.770113 0.693362 11.00000 -1.20000
AFIX 0
C12 1 0.068460 0.841870 0.627971 11.00000 0.01830 0.08655 =
0.03945 -0.01127 0.00281 0.00526
AFIX 43
H12 2 0.036849 0.889158 0.614405 11.00000 -1.20000
AFIX 0
PART 1
SI1' 5 0.447850 0.855312 0.649560 21.00000 0.01566 0.02239 =
0.01895 -0.00256 0.00157 -0.00079
PART 2
SI1 5 0.447615 0.767685 0.659173 -21.00000 0.01662 0.02589 =
0.02081 -0.00310 0.00142 -0.00036
PART 1
C26' 1 0.492635 0.889687 0.605119 21.00000 0.02515 0.03577 =
0.03384 -0.00198 0.01181 -0.00406
AFIX 137
H26A 2 0.495024 0.770536 0.586571 21.00000 -1.50000
H26B 2 0.525439 0.921820 0.622212 21.00000 -1.50000
H26C 2 0.481208 0.994946 0.582991 21.00000 -1.50000
AFIX 0
PART 2
C25 1 0.452592 0.517763 0.683665 -21.00000 0.02929 0.02937 =
0.03148 0.00216 0.00165 0.00643
AFIX 137
H25A 2 0.426258 0.495906 0.704372 -21.00000 -1.50000
H25B 2 0.485202 0.500342 0.702742 -21.00000 -1.50000
H25C 2 0.448937 0.425399 0.656780 -21.00000 -1.50000
AFIX 0
C26 1 0.496275 0.819828 0.619415 -21.00000 0.02561 0.04199 =
0.04082 -0.00625 0.01147 -0.00754
AFIX 137
H26D 2 0.495305 0.721183 0.594066 -21.00000 -1.50000
H26E 2 0.529089 0.818962 0.638724 -21.00000 -1.50000
H26F 2 0.490163 0.946910 0.604431 -21.00000 -1.50000
AFIX 0
C24 1 0.449639 0.944054 0.709628 -21.00000 0.03233 0.03543 =
0.02718 -0.00721 -0.00239 -0.00128
AFIX 137
H24A 2 0.481852 0.934839 0.729847 -21.00000 -1.50000
H24B 2 0.422812 0.915671 0.729316 -21.00000 -1.50000
H24C 2 0.445324 1.074756 0.696357 -21.00000 -1.50000
AFIX 0
PART 1
C24' 1 0.442064 1.077679 0.685465 21.00000 0.02158 0.03657 =
0.04370 -0.01837 0.00206 -0.00309
AFIX 137
H24D 2 0.430732 1.184057 0.663657 21.00000 -1.50000
H24E 2 0.474530 1.110089 0.703233 21.00000 -1.50000
H24F 2 0.417871 1.056474 0.708490 21.00000 -1.50000
AFIX 0
C25' 1 0.465077 0.645246 0.689809 21.00000 0.02766 0.03780 =
0.03727 0.01254 -0.00028 0.00409
AFIX 137
H25D 2 0.442469 0.638034 0.714775 21.00000 -1.50000
H25E 2 0.499382 0.660657 0.705276 21.00000 -1.50000
H25F 2 0.462454 0.526433 0.670568 21.00000 -1.50000
AFIX 0
O1' 3 0.393299 0.812557 0.616182 21.00000 0.01273 0.02494 =
0.01638 0.00215 -0.00125 -0.00199
PART 2
O1 3 0.395379 0.787784 0.623395 -21.00000 0.01905 0.02207 =
0.01623 0.00332 0.00033 -0.00056
PART 0
H23A 2 0.347904 0.763210 0.670315 11.00000 0.02098
H23B 2 0.349661 0.584863 0.633164 11.00000 0.01888
HKLF 4
REM b1352_0m_a.res in C2/c
REM R1 = 0.0319 for 6927 Fo > 4sig(Fo) and 0.0424 for all 8253 data
REM 340 parameters refined using 0 restraints
END
WGHT 0.0272 3.6219
REM Highest difference peak 0.355, deepest hole -0.241, 1-sigma level 0.046
Q1 1 0.2814 0.7637 0.6107 11.00000 0.05 0.36
Q2 1 0.1300 0.8014 0.6120 11.00000 0.05 0.35
Q3 1 0.3277 0.7625 0.6164 11.00000 0.05 0.32
Q4 1 0.3018 0.7758 0.5775 11.00000 0.05 0.31
Q5 1 0.3713 0.4309 0.5277 11.00000 0.05 0.29
Q6 1 0.3486 0.3023 0.5090 11.00000 0.05 0.28
Q7 1 0.3487 0.3387 0.5001 11.00000 0.05 0.28
Q8 1 0.1382 0.6872 0.6765 11.00000 0.05 0.27
;
_shelx_res_checksum 34258
loop_
_space_group_symop_operation_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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 0.29397(2) 0.49136(4) 0.53826(2) 0.01817(6) Uani d 1 . .
S S2 0.20238(2) 0.78150(4) 0.58269(2) 0.02262(6) Uani d 1 . .
S S3 0.31216(2) 1.14605(4) 0.66285(2) 0.02538(7) Uani d 1 . .
C C8 0.30483(4) 0.80744(14) 0.60358(4) 0.01565(18) Uani d 1 . .
C C7 0.30656(4) 0.74642(14) 0.55036(4) 0.01713(18) Uani d 1 . .
H H7A 0.3399 0.7775 0.5412 0.021 Uiso calc 1 . .
H H7B 0.2819 0.8238 0.5294 0.021 Uiso calc 1 . .
C C9 0.25831(4) 0.72995(14) 0.62389(4) 0.01716(18) Uani d 1 . .
H H9A 0.2556 0.7904 0.6557 0.021 Uiso calc 1 . .
H H9B 0.2615 0.5889 0.6288 0.021 Uiso calc 1 . .
C C16 0.30594(4) 1.02993(15) 0.60364(4) 0.0201(2) Uani d 1 . .
H H16A 0.2749 1.0768 0.5848 0.024 Uiso calc 1 . .
H H16B 0.3340 1.0724 0.5864 0.024 Uiso calc 1 . .
C C1 0.34951(4) 0.39457(15) 0.52076(4) 0.0198(2) Uani d 1 . .
C C23 0.34988(4) 0.72598(16) 0.63568(4) 0.01953(19) Uani d 1 . .
C C15 0.16005(4) 0.70047(17) 0.66701(4) 0.0246(2) Uani d 1 . .
H H15 0.1914 0.6503 0.6805 0.029 Uiso calc 1 . .
C C2 0.34409(5) 0.23215(16) 0.49074(4) 0.0250(2) Uani d 1 . .
H H2 0.3117 0.1857 0.4793 0.030 Uiso calc 1 . .
C C6 0.39722(4) 0.46279(18) 0.53680(4) 0.0277(2) Uani d 1 . .
H H6 0.4014 0.5728 0.5573 0.033 Uiso calc 1 . .
C C17 0.25090(5) 1.14867(15) 0.67960(4) 0.0255(2) Uani d 1 . .
C C10 0.15440(4) 0.77326(17) 0.62029(4) 0.0230(2) Uani d 1 . .
C C22 0.24394(5) 1.07987(17) 0.72557(4) 0.0300(3) Uani d 1 . .
H H22 0.2712 1.0258 0.7459 0.036 Uiso calc 1 . .
C C18 0.21056(5) 1.22418(17) 0.64960(5) 0.0307(3) Uani d 1 . .
H H18 0.2150 1.2712 0.6183 0.037 Uiso calc 1 . .
C C14 0.12017(5) 0.7002(2) 0.69433(5) 0.0330(3) Uani d 1 . .
H H14 0.1245 0.6515 0.7265 0.040 Uiso calc 1 . .
C C3 0.38577(5) 0.13854(18) 0.47757(5) 0.0332(3) Uani d 1 . .
H H3 0.3818 0.0272 0.4576 0.040 Uiso calc 1 . .
C C21 0.19743(6) 1.09037(19) 0.74155(5) 0.0375(3) Uani d 1 . .
H H21 0.1930 1.0455 0.7730 0.045 Uiso calc 1 . .
C C5 0.43855(5) 0.3689(2) 0.52267(5) 0.0371(3) Uani d 1 . .
H H5 0.4710 0.4167 0.5332 0.044 Uiso calc 1 . .
C C11 0.10797(4) 0.8453(2) 0.60058(5) 0.0355(3) Uani d 1 . .
H H11 0.1036 0.8962 0.5686 0.043 Uiso calc 1 . .
C C4 0.43306(5) 0.2064(2) 0.49342(5) 0.0377(3) Uani d 1 . .
H H4 0.4615 0.1422 0.4843 0.045 Uiso calc 1 . .
C C20 0.15751(6) 1.16595(19) 0.71180(6) 0.0414(3) Uani d 1 . .
H H20 0.1257 1.1738 0.7229 0.050 Uiso calc 1 . .
C C19 0.16397(5) 1.23047(19) 0.66560(6) 0.0384(3) Uani d 1 . .
H H19 0.1363 1.2792 0.6449 0.046 Uiso calc 1 . .
C C13 0.07437(5) 0.7706(3) 0.67479(6) 0.0442(4) Uani d 1 . .
H H13 0.0471 0.7701 0.6934 0.053 Uiso calc 1 . .
C C12 0.06846(5) 0.8419(3) 0.62797(6) 0.0482(4) Uani d 1 . .
H H12 0.0368 0.8892 0.6144 0.058 Uiso calc 1 . .
Si Si1' 0.44785(2) 0.8553(2) 0.64956(3) 0.0190(2) Uani d 0.491(3) A 1
Si Si1 0.44762(2) 0.7677(2) 0.65917(3) 0.0212(2) Uani d 0.509(3) A 2
C C26' 0.49264(14) 0.8897(5) 0.60512(14) 0.0309(7) Uani d 0.491(3) A 1
H H26A 0.4950 0.7705 0.5866 0.046 Uiso calc 0.491(3) A 1
H H26B 0.5254 0.9218 0.6222 0.046 Uiso calc 0.491(3) A 1
H H26C 0.4812 0.9949 0.5830 0.046 Uiso calc 0.491(3) A 1
C C25 0.45259(9) 0.5178(4) 0.68366(9) 0.0302(6) Uani d 0.509(3) A 2
H H25A 0.4263 0.4959 0.7044 0.045 Uiso calc 0.509(3) A 2
H H25B 0.4852 0.5003 0.7027 0.045 Uiso calc 0.509(3) A 2
H H25C 0.4489 0.4254 0.6568 0.045 Uiso calc 0.509(3) A 2
C C26 0.49628(13) 0.8198(6) 0.61941(14) 0.0355(7) Uani d 0.509(3) A 2
H H26D 0.4953 0.7212 0.5941 0.053 Uiso calc 0.509(3) A 2
H H26E 0.5291 0.8190 0.6387 0.053 Uiso calc 0.509(3) A 2
H H26F 0.4902 0.9469 0.6044 0.053 Uiso calc 0.509(3) A 2
C C24 0.44964(10) 0.9441(4) 0.70963(9) 0.0321(6) Uani d 0.509(3) A 2
H H24A 0.4819 0.9348 0.7298 0.048 Uiso calc 0.509(3) A 2
H H24B 0.4228 0.9157 0.7293 0.048 Uiso calc 0.509(3) A 2
H H24C 0.4453 1.0748 0.6964 0.048 Uiso calc 0.509(3) A 2
C C24' 0.44206(10) 1.0777(4) 0.68546(11) 0.0341(7) Uani d 0.491(3) A 1
H H24D 0.4307 1.1841 0.6637 0.051 Uiso calc 0.491(3) A 1
H H24E 0.4745 1.1101 0.7032 0.051 Uiso calc 0.491(3) A 1
H H24F 0.4179 1.0565 0.7085 0.051 Uiso calc 0.491(3) A 1
C C25' 0.46508(10) 0.6452(4) 0.68981(11) 0.0346(7) Uani d 0.491(3) A 1
H H25D 0.4425 0.6380 0.7148 0.052 Uiso calc 0.491(3) A 1
H H25E 0.4994 0.6607 0.7053 0.052 Uiso calc 0.491(3) A 1
H H25F 0.4625 0.5264 0.6706 0.052 Uiso calc 0.491(3) A 1
O O1' 0.3933(5) 0.813(2) 0.6162(5) 0.0183(11) Uani d 0.491(3) A 1
O O1 0.3954(5) 0.788(2) 0.6234(5) 0.0193(11) Uani d 0.509(3) A 2
H H23A 0.3479(5) 0.7632(18) 0.6703(5) 0.021(3) Uiso d 1 . .
H H23B 0.3497(5) 0.5849(19) 0.6332(5) 0.019(3) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.01888(11) 0.01749(11) 0.01825(12) -0.00061(9) 0.00277(9) -0.00230(9)
S2 0.01735(11) 0.03543(15) 0.01493(12) 0.00120(10) 0.00136(9) -0.00211(10)
S3 0.03324(15) 0.02129(12) 0.02207(13) -0.00472(11) 0.00528(11) -0.00615(10)
C8 0.0167(4) 0.0162(4) 0.0140(4) -0.0005(3) 0.0020(3) 0.0005(3)
C7 0.0191(4) 0.0170(4) 0.0153(4) -0.0002(4) 0.0022(3) -0.0002(3)
C9 0.0182(4) 0.0189(4) 0.0145(4) -0.0010(4) 0.0025(3) -0.0002(3)
C16 0.0264(5) 0.0174(4) 0.0174(5) -0.0018(4) 0.0058(4) -0.0006(4)
C1 0.0234(5) 0.0207(5) 0.0156(5) 0.0035(4) 0.0030(4) -0.0004(4)
C23 0.0178(4) 0.0226(5) 0.0177(5) 0.0000(4) 0.0004(4) -0.0010(4)
C15 0.0225(5) 0.0276(5) 0.0244(5) -0.0024(4) 0.0061(4) -0.0026(4)
C2 0.0308(6) 0.0227(5) 0.0225(5) -0.0004(4) 0.0063(4) -0.0040(4)
C6 0.0228(5) 0.0340(6) 0.0255(6) 0.0040(5) 0.0001(4) -0.0091(5)
C17 0.0377(6) 0.0157(4) 0.0246(5) -0.0008(4) 0.0103(5) -0.0049(4)
C10 0.0180(5) 0.0295(5) 0.0219(5) -0.0023(4) 0.0039(4) -0.0065(4)
C22 0.0471(7) 0.0225(5) 0.0218(6) -0.0035(5) 0.0095(5) -0.0062(4)
C18 0.0409(7) 0.0192(5) 0.0336(7) 0.0043(5) 0.0113(5) 0.0003(4)
C14 0.0299(6) 0.0432(7) 0.0281(6) -0.0080(5) 0.0129(5) -0.0038(5)
C3 0.0426(7) 0.0280(6) 0.0306(6) 0.0054(5) 0.0102(5) -0.0072(5)
C21 0.0580(9) 0.0275(6) 0.0313(7) -0.0067(6) 0.0229(6) -0.0097(5)
C5 0.0230(6) 0.0510(8) 0.0368(7) 0.0078(6) 0.0021(5) -0.0108(6)
C11 0.0206(5) 0.0593(9) 0.0259(6) 0.0044(6) 0.0005(4) -0.0050(6)
C4 0.0347(7) 0.0446(7) 0.0347(7) 0.0163(6) 0.0080(5) -0.0067(6)
C20 0.0495(8) 0.0259(6) 0.0546(9) -0.0009(6) 0.0302(7) -0.0126(6)
C19 0.0403(7) 0.0246(6) 0.0522(9) 0.0087(5) 0.0130(6) -0.0040(6)
C13 0.0212(6) 0.0742(11) 0.0396(8) -0.0059(6) 0.0136(5) -0.0133(7)
C12 0.0183(6) 0.0866(12) 0.0394(8) 0.0053(7) 0.0028(5) -0.0113(8)
Si1' 0.0157(3) 0.0224(5) 0.0190(3) -0.0008(3) 0.0016(2) -0.0026(3)
Si1 0.0166(3) 0.0259(6) 0.0208(3) -0.0004(3) 0.0014(2) -0.0031(3)
C26' 0.0251(13) 0.0358(18) 0.0338(18) -0.0041(13) 0.0118(12) -0.0020(13)
C25 0.0293(12) 0.0294(13) 0.0315(13) 0.0064(10) 0.0017(10) 0.0022(10)
C26 0.0256(13) 0.042(2) 0.041(2) -0.0075(14) 0.0115(13) -0.0063(14)
C24 0.0323(12) 0.0354(13) 0.0272(12) -0.0013(10) -0.0024(9) -0.0072(10)
C24' 0.0216(11) 0.0366(14) 0.0437(16) -0.0031(10) 0.0021(10) -0.0184(12)
C25' 0.0277(12) 0.0378(16) 0.0373(15) 0.0041(11) -0.0003(10) 0.0125(12)
O1' 0.0127(13) 0.025(3) 0.016(3) -0.0020(18) -0.0013(17) 0.0021(18)
O1 0.0191(16) 0.022(3) 0.016(3) -0.0006(15) 0.0003(18) 0.0033(17)
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'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 S1 C7 . . 105.85(5) y
C10 S2 C9 . . 103.65(5) y
C17 S3 C16 . . 104.74(5) y
C9 C8 C7 . . 112.14(8) ?
C9 C8 C16 . . 111.46(8) ?
C16 C8 C7 . . 105.78(8) ?
C23 C8 C7 . . 110.11(8) ?
C23 C8 C9 . . 106.65(8) ?
C23 C8 C16 . . 110.77(8) ?
S1 C7 H7A . . 108.6 ?
S1 C7 H7B . . 108.6 ?
C8 C7 S1 . . 114.55(7) ?
C8 C7 H7A . . 108.6 ?
C8 C7 H7B . . 108.6 ?
H7A C7 H7B . . 107.6 ?
S2 C9 H9A . . 109.5 ?
S2 C9 H9B . . 109.5 ?
C8 C9 S2 . . 110.82(7) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 108.1 ?
S3 C16 H16A . . 108.2 ?
S3 C16 H16B . . 108.2 ?
C8 C16 S3 . . 116.27(7) ?
C8 C16 H16A . . 108.2 ?
C8 C16 H16B . . 108.2 ?
H16A C16 H16B . . 107.4 ?
C2 C1 S1 . . 116.04(8) ?
C6 C1 S1 . . 124.56(8) ?
C6 C1 C2 . . 119.31(10) ?
C8 C23 H23A . . 109.5(7) ?
C8 C23 H23B . . 109.2(7) ?
O1' C23 C8 . . 104.4(4) ?
O1' C23 H23A . . 112.6(10) ?
O1' C23 H23B . . 112.1(10) ?
O1 C23 C8 . . 114.3(4) ?
O1 C23 H23A . . 108.0(10) ?
O1 C23 H23B . . 106.8(10) ?
H23A C23 H23B . . 108.9(11) ?
C10 C15 H15 . . 119.8 ?
C10 C15 C14 . . 120.49(11) ?
C14 C15 H15 . . 119.8 ?
C1 C2 H2 . . 119.9 ?
C3 C2 C1 . . 120.28(11) ?
C3 C2 H2 . . 119.9 ?
C1 C6 H6 . . 120.2 ?
C5 C6 C1 . . 119.65(11) ?
C5 C6 H6 . . 120.2 ?
C22 C17 S3 . . 118.00(10) ?
C18 C17 S3 . . 122.37(10) ?
C18 C17 C22 . . 119.57(12) ?
C15 C10 S2 . . 124.22(9) ?
C15 C10 C11 . . 119.28(11) ?
C11 C10 S2 . . 116.50(10) ?
C17 C22 H22 . . 119.9 ?
C21 C22 C17 . . 120.19(13) ?
C21 C22 H22 . . 119.9 ?
C17 C18 H18 . . 120.1 ?
C19 C18 C17 . . 119.75(13) ?
C19 C18 H18 . . 120.1 ?
C15 C14 H14 . . 119.9 ?
C13 C14 C15 . . 120.15(13) ?
C13 C14 H14 . . 119.9 ?
C2 C3 H3 . . 119.8 ?
C4 C3 C2 . . 120.38(12) ?
C4 C3 H3 . . 119.8 ?
C22 C21 H21 . . 119.9 ?
C20 C21 C22 . . 120.13(13) ?
C20 C21 H21 . . 119.9 ?
C6 C5 H5 . . 119.6 ?
C4 C5 C6 . . 120.88(12) ?
C4 C5 H5 . . 119.6 ?
C10 C11 H11 . . 120.2 ?
C12 C11 C10 . . 119.60(13) ?
C12 C11 H11 . . 120.2 ?
C3 C4 C5 . . 119.50(12) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
C21 C20 H20 . . 120.1 ?
C21 C20 C19 . . 119.90(13) ?
C19 C20 H20 . . 120.1 ?
C18 C19 C20 . . 120.43(14) ?
C18 C19 H19 . . 119.8 ?
C20 C19 H19 . . 119.8 ?
C14 C13 H13 . . 120.2 ?
C14 C13 C12 . . 119.53(12) ?
C12 C13 H13 . . 120.2 ?
C11 C12 H12 . . 119.5 ?
C13 C12 C11 . . 120.94(13) ?
C13 C12 H12 . . 119.5 ?
C26' Si1' C24' . . 110.96(16) ?
C26' Si1' C25' . . 111.49(15) ?
C24' Si1' C25' . . 111.01(15) ?
O1' Si1' C26' . . 104.9(5) ?
O1' Si1' C24' . . 108.7(6) ?
O1' Si1' C25' . . 109.6(4) ?
C26 Si1 C25 . . 112.00(15) ?
C26 Si1 C24 . . 111.33(15) ?
C24 Si1 C25 . . 110.04(13) ?
O1 Si1 C25 . . 108.8(5) ?
O1 Si1 C26 . . 104.2(5) ?
O1 Si1 C24 . . 110.4(6) ?
Si1' C26' H26A . . 109.5 ?
Si1' C26' H26B . . 109.5 ?
Si1' C26' H26C . . 109.5 ?
H26A C26' H26B . . 109.5 ?
H26A C26' H26C . . 109.5 ?
H26B C26' H26C . . 109.5 ?
Si1 C25 H25A . . 109.5 ?
Si1 C25 H25B . . 109.5 ?
Si1 C25 H25C . . 109.5 ?
H25A C25 H25B . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
Si1 C26 H26D . . 109.5 ?
Si1 C26 H26E . . 109.5 ?
Si1 C26 H26F . . 109.5 ?
H26D C26 H26E . . 109.5 ?
H26D C26 H26F . . 109.5 ?
H26E C26 H26F . . 109.5 ?
Si1 C24 H24A . . 109.5 ?
Si1 C24 H24B . . 109.5 ?
Si1 C24 H24C . . 109.5 ?
H24A C24 H24B . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
Si1' C24' H24D . . 109.5 ?
Si1' C24' H24E . . 109.5 ?
Si1' C24' H24F . . 109.5 ?
H24D C24' H24E . . 109.5 ?
H24D C24' H24F . . 109.5 ?
H24E C24' H24F . . 109.5 ?
Si1' C25' H25D . . 109.5 ?
Si1' C25' H25E . . 109.5 ?
Si1' C25' H25F . . 109.5 ?
H25D C25' H25E . . 109.5 ?
H25D C25' H25F . . 109.5 ?
H25E C25' H25F . . 109.5 ?
C23 O1' Si1' . . 123.7(7) y
C23 O1 Si1 . . 123.6(7) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C7 . 1.8244(10) y
S1 C1 . 1.7661(11) y
S2 C9 . 1.8188(10) ?
S2 C10 . 1.7625(12) y
S3 C16 . 1.8214(11) y
S3 C17 . 1.7742(13) y
C8 C7 . 1.5446(14) ?
C8 C9 . 1.5367(14) ?
C8 C16 . 1.5428(14) ?
C8 C23 . 1.5286(14) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C1 C2 . 1.3986(15) ?
C1 C6 . 1.3957(15) ?
O1 C23 . 1.384(15) y
O1' C23 . 1.479(14) y
C23 H23A . 1.004(14) ?
C23 H23B . 0.981(13) ?
C15 H15 . 0.9500 ?
C15 C10 . 1.3845(16) ?
C15 C14 . 1.3918(16) ?
C2 H2 . 0.9500 ?
C2 C3 . 1.3875(17) ?
C6 H6 . 0.9500 ?
C6 C5 . 1.3905(17) ?
C17 C22 . 1.3977(17) ?
C17 C18 . 1.3925(18) ?
C10 C11 . 1.3998(16) ?
C22 H22 . 0.9500 ?
C22 C21 . 1.3856(19) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.3865(19) ?
C14 H14 . 0.9500 ?
C14 C13 . 1.380(2) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.384(2) ?
C21 H21 . 0.9500 ?
C21 C20 . 1.381(2) ?
C5 H5 . 0.9500 ?
C5 C4 . 1.3864(19) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3850(19) ?
C4 H4 . 0.9500 ?
C20 H20 . 0.9500 ?
C20 C19 . 1.391(2) ?
C19 H19 . 0.9500 ?
C13 H13 . 0.9500 ?
C13 C12 . 1.383(2) ?
C12 H12 . 0.9500 ?
Si1' C26' . 1.847(4) ?
Si1' C24' . 1.853(3) ?
Si1' C25' . 1.861(3) ?
O1 Si1 . 1.632(12) y
O1' Si1' . 1.672(13) y
Si1 C25 . 1.861(3) ?
Si1 C26 . 1.853(4) ?
Si1 C24 . 1.856(3) ?
C26' H26A . 0.9800 ?
C26' H26B . 0.9800 ?
C26' H26C . 0.9800 ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C26 H26D . 0.9800 ?
C26 H26E . 0.9800 ?
C26 H26F . 0.9800 ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
C24' H24D . 0.9800 ?
C24' H24E . 0.9800 ?
C24' H24F . 0.9800 ?
C25' H25D . 0.9800 ?
C25' H25E . 0.9800 ?
C25' H25F . 0.9800 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S1 C1 C2 C3 . . . . -175.92(10) ?
S1 C1 C6 C5 . . . . 176.56(10) ?
S2 C10 C11 C12 . . . . 179.49(12) ?
S3 C17 C22 C21 . . . . 175.84(9) ?
S3 C17 C18 C19 . . . . -176.99(9) ?
C8 C23 O1' Si1' . . . . 151.5(9) ?
C8 C23 O1 Si1 . . . . 163.9(8) ?
C7 S1 C1 C2 . . . . -153.61(8) ?
C7 S1 C1 C6 . . . . 29.86(11) ?
C7 C8 C9 S2 . . . . -49.35(10) ?
C7 C8 C16 S3 . . . . -172.59(7) ?
C7 C8 C23 O1' . . . . 60.9(7) ?
C7 C8 C23 O1 . . . . 60.3(8) ?
C9 S2 C10 C15 . . . . -12.64(11) ?
C9 S2 C10 C11 . . . . 167.62(10) ?
C9 C8 C7 S1 . . . . -47.38(10) ?
C9 C8 C16 S3 . . . . 65.28(10) ?
C9 C8 C23 O1' . . . . -177.2(7) ?
C9 C8 C23 O1 . . . . -177.8(8) ?
C16 S3 C17 C22 . . . . 129.90(9) ?
C16 S3 C17 C18 . . . . -53.05(11) ?
C16 C8 C7 S1 . . . . -169.08(7) ?
C16 C8 C9 S2 . . . . 69.04(9) ?
C16 C8 C23 O1' . . . . -55.8(7) ?
C16 C8 C23 O1 . . . . -56.3(8) ?
C1 S1 C7 C8 . . . . -115.70(7) ?
C1 C2 C3 C4 . . . . -0.9(2) ?
C1 C6 C5 C4 . . . . -1.0(2) ?
C23 C8 C7 S1 . . . . 71.19(9) ?
C23 C8 C9 S2 . . . . -169.94(7) ?
C23 C8 C16 S3 . . . . -53.29(11) ?
C15 C10 C11 C12 . . . . -0.3(2) ?
C15 C14 C13 C12 . . . . -0.2(2) ?
C2 C1 C6 C5 . . . . 0.14(18) ?
C2 C3 C4 C5 . . . . 0.1(2) ?
C6 C1 C2 C3 . . . . 0.80(18) ?
C6 C5 C4 C3 . . . . 0.9(2) ?
C17 S3 C16 C8 . . . . -81.99(9) ?
C17 C22 C21 C20 . . . . 1.09(18) ?
C17 C18 C19 C20 . . . . 1.48(19) ?
C10 S2 C9 C8 . . . . -157.51(7) ?
C10 C15 C14 C13 . . . . 0.8(2) ?
C10 C11 C12 C13 . . . . 0.9(2) ?
C22 C17 C18 C19 . . . . 0.02(17) ?
C22 C21 C20 C19 . . . . 0.4(2) ?
C18 C17 C22 C21 . . . . -1.30(17) ?
C14 C15 C10 S2 . . . . 179.72(10) ?
C14 C15 C10 C11 . . . . -0.55(18) ?
C14 C13 C12 C11 . . . . -0.6(3) ?
C21 C20 C19 C18 . . . . -1.7(2) ?
C26' Si1' O1' C23 . . . . 163.0(10) ?
C25 Si1 O1 C23 . . . . 47.9(13) ?
C26 Si1 O1 C23 . . . . 167.5(11) ?
C24 Si1 O1 C23 . . . . -72.9(12) ?
C24' Si1' O1' C23 . . . . -78.3(11) ?
C25' Si1' O1' C23 . . . . 43.2(13) ?