#------------------------------------------------------------------------------
#$Date: 2021-12-15 05:08:06 +0200 (Wed, 15 Dec 2021) $
#$Revision: 271437 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243948.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_2243948
loop_
_publ_author_name
'Schmidt, Annika'
'Krupp, Anna'
'Barth, Eva Rebecca'
'Strohmann, Carsten'
_publ_section_title
;
Crystal structures and Hirshfeld surface analyses of
bis(4,5-dihydrofuran-2-yl)dimethylsilane and
(4,5-dihydrofuran-2-yl)(methyl)diphenylsilane
;
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021012548
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C17 H18 O Si'
_chemical_formula_moiety 'C17 H18 O Si'
_chemical_formula_sum 'C17 H18 O Si'
_chemical_formula_weight 266.40
_chemical_name_systematic
;
(4,5-Dihydrofuran-2-yl)(methyl)diphenylsilane
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary iterative
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 102.219(2)
_cell_angle_beta 90.613(2)
_cell_angle_gamma 110.280(2)
_cell_formula_units_Z 2
_cell_length_a 8.7737(4)
_cell_length_b 9.1715(4)
_cell_length_c 9.8130(4)
_cell_measurement_reflns_used 8775
_cell_measurement_temperature 100
_cell_measurement_theta_max 36.28
_cell_measurement_theta_min 2.49
_cell_volume 720.85(6)
_computing_cell_refinement 'SAINT (Bruker, 2016)'
_computing_data_collection 'APEX2 (Bruker, 2018)'
_computing_data_reduction 'SAINT (Bruker, 2016)'
_computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material
;OLEX2 (Dolomanov et al., 2009),
CrystalExplorer21 (Spackman et al., 2021),
publCIF (Westrip, 2010), Mercury (Macrae et al., 2020)
;
_computing_structure_refinement 'SHELXL2014/7 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0296
_diffrn_reflns_av_unetI/netI 0.0328
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 20409
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 34.000
_diffrn_reflns_theta_min 2.789
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.4
_diffrn_source_power 0.07
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.152
_exptl_absorpt_correction_T_max 0.7471
_exptl_absorpt_correction_T_min 0.7127
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.227
_exptl_crystal_description plate
_exptl_crystal_F_000 284
_exptl_crystal_size_max 0.511
_exptl_crystal_size_mid 0.188
_exptl_crystal_size_min 0.074
_refine_diff_density_max 0.484
_refine_diff_density_min -0.268
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment
H_atoms_treated_by_a_mixture_of_independent_and_constrained_refinement.
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 5826
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0497
_refine_ls_R_factor_gt 0.0398
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.2951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0964
_refine_ls_wR_factor_ref 0.1049
_reflns_number_gt 4937
_reflns_number_total 5826
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2257sup1.cif
_cod_data_source_block 2
_cod_database_code 2243948
_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 0.926
_shelx_estimated_absorpt_t_max 0.989
_shelx_hkl_file
;
1 0 0 72.3108 3.15644 3
-2 0 0 228.932 8.33931 3
-2 0 0 232.323 7.53648 5
2 0 0 226.526 6.70416 7
2 0 0 238.000 7.43868 5
2 0 0 217.603 8.10335 3
-3 0 0 24.8295 3.30549 3
-3 0 0 25.4850 2.98350 5
3 0 0 26.1251 3.30875 3
3 0 0 21.6186 2.38543 7
3 0 0 16.7796 2.64772 5
3 0 0 23.8685 2.61305 4
-4 0 0 940.312 26.1093 3
4 0 0 976.020 22.2490 7
4 0 0 939.471 25.5384 3
4 0 0 985.789 22.9618 4
4 0 0 966.222 23.5957 5
4 0 0 955.100 22.5295 2
-5 0 0 2464.46 54.1812 3
5 0 0 2492.21 48.4901 2
5 0 0 2479.88 47.9091 7
5 0 0 2450.34 53.2810 3
5 0 0 2467.65 49.9886 5
5 0 0 2569.14 49.5562 4
-6 0 0 11.7221 3.98513 3
6 0 0 4.74608 2.12355 5
6 0 0 3.20821 1.76137 7
6 0 0 6.43299 2.22831 2
6 0 0 2.63102 2.07659 3
6 0 0 5.18543 1.91823 4
-7 0 0 0.88939 1.98992 3
7 0 0 1.27150 2.21066 3
7 0 0 0.27548 1.58338 2
7 0 0 0.35379 1.46362 4
7 0 0 -0.5095 1.18676 7
8 0 0 1492.65 38.9822 4
8 0 0 1388.31 41.3662 6
8 0 0 1433.83 36.2616 7
8 0 0 1464.30 43.2590 3
9 0 0 18.5950 4.71594 7
9 0 0 12.6970 3.92835 4
9 0 0 14.6256 4.86798 6
10 0 0 35.9098 6.52752 7
10 0 0 29.5053 6.15164 4
10 0 0 39.3962 7.98106 6
11 0 0 160.857 14.2619 6
11 0 0 145.162 11.3824 7
11 0 0 139.230 10.6169 8
11 0 0 153.990 12.5782 4
12 0 0 60.1007 7.18512 8
12 0 0 49.3626 9.09681 6
12 0 0 53.2823 9.11783 4
12 0 0 49.2590 7.55189 7
13 0 0 132.323 11.1170 7
13 0 0 149.898 13.3411 4
13 0 0 91.9039 11.4113 6
13 -1 0 48.2350 9.12020 4
13 -1 0 53.1683 11.2533 6
12 -1 0 387.294 24.2426 6
12 -1 0 340.069 18.9521 7
12 -1 0 372.961 16.7549 8
12 -1 0 373.964 21.4376 4
11 -1 0 7.67400 3.53177 7
11 -1 0 9.71979 4.68430 6
11 -1 0 18.2780 5.03152 4
10 -1 0 7.80195 3.67759 4
10 -1 0 0.83659 2.88119 6
10 -1 0 -0.7911 1.72267 7
9 -1 0 22.5781 5.32034 7
9 -1 0 23.0308 5.24677 8
9 -1 0 18.2521 5.27414 4
9 -1 0 17.7594 5.92468 3
8 -1 0 5.58982 2.62264 7
8 -1 0 2.37722 1.97811 8
8 -1 0 6.95374 2.97694 4
7 -1 0 105.344 7.98461 7
7 -1 0 107.326 9.21556 3
7 -1 0 119.139 7.66641 2
7 -1 0 111.604 7.86970 8
7 -1 0 107.702 8.58290 4
6 -1 0 177.535 10.2584 4
6 -1 0 187.151 9.96950 7
6 -1 0 193.331 9.63547 8
6 -1 0 184.698 10.5772 5
6 -1 0 181.078 8.99675 2
6 -1 0 167.118 10.6727 3
5 -1 0 591.198 18.4784 4
5 -1 0 592.231 19.0383 5
5 -1 0 593.406 17.8891 7
5 -1 0 615.054 19.9217 3
5 -1 0 597.163 16.8259 2
4 -1 0 1447.18 32.3384 3
4 -1 0 1482.21 30.9430 7
4 -1 0 1438.70 31.8980 5
4 -1 0 1464.59 29.6439 2
4 -1 0 1448.91 31.3516 4
3 -1 0 955.522 21.2276 7
3 -1 0 980.191 19.9781 8
3 -1 0 977.496 21.9198 3
3 -1 0 919.792 21.8099 5
-3 1 0 999.604 21.4354 7
-3 1 0 977.713 20.7651 2
2 -1 0 491.689 10.7265 8
2 -1 0 498.559 11.5112 2
2 -1 0 500.959 12.1167 7
2 -1 0 489.716 12.3531 5
-2 1 0 511.810 12.1441 7
-2 1 0 486.285 10.7377 8
-2 1 0 514.604 11.7035 2
1 -1 0 318.644 7.89296 7
1 -1 0 312.374 7.00248 8
1 -1 0 374.229 8.32358 2
-1 1 0 349.368 8.16354 2
-1 1 0 364.627 8.12178 7
-1 1 0 333.686 7.20489 8
0 -1 0 2.14423 0.62100 8
0 1 0 0.02242 0.29038 2
0 1 0 0.14653 0.17725 7
0 1 0 0.35897 0.28083 8
-1 -1 0 256.753 6.18595 5
-1 -1 0 267.609 6.66564 6
1 1 0 250.817 5.88512 5
1 1 0 260.025 8.72616 3
1 1 0 248.122 6.28237 6
-2 -1 0 265.489 8.10248 5
-2 -1 0 260.683 10.6384 3
2 1 0 260.172 7.69629 5
2 1 0 257.680 7.09015 4
2 1 0 274.239 8.38488 6
2 1 0 254.921 10.2757 3
-3 -1 0 765.711 18.9288 5
-3 -1 0 749.238 22.5497 3
3 1 0 804.806 17.5651 4
3 1 0 797.433 22.4547 3
3 1 0 747.887 18.9622 6
3 1 0 811.555 18.4506 5
-4 -1 0 1772.56 42.3287 3
-4 -1 0 1749.31 37.0326 5
4 1 0 1761.25 35.6918 5
4 1 0 1711.25 40.9265 3
4 1 0 1734.34 34.5615 4
4 1 0 1748.85 33.9224 7
4 1 0 1708.10 36.9553 6
-5 -1 0 109.023 9.36897 3
5 1 0 106.310 8.84905 3
5 1 0 97.9465 7.33163 6
5 1 0 102.343 6.90858 5
5 1 0 103.334 6.58609 4
5 1 0 105.301 6.34502 7
-6 -1 0 443.621 21.3553 3
6 1 0 439.843 20.4161 3
6 1 0 463.457 17.2700 2
6 1 0 440.310 17.8825 6
6 1 0 433.434 15.8699 4
6 1 0 433.000 15.0240 7
6 1 0 446.597 16.6117 5
-7 -1 0 241.154 16.4100 3
7 1 0 224.885 11.1560 7
7 1 0 230.573 12.3736 2
7 1 0 250.454 12.5591 4
7 1 0 246.415 13.9321 6
7 1 0 228.373 15.0973 3
-8 -1 0 343.334 21.1080 3
8 1 0 335.819 14.7259 7
8 1 0 329.559 17.5181 6
8 1 0 327.388 15.3926 2
8 1 0 340.761 16.2370 4
9 1 0 -2.5481 1.87809 6
9 1 0 0.42615 1.42861 7
9 1 0 -0.2446 1.52691 4
10 1 0 1.52752 2.32785 4
10 1 0 4.61990 2.34278 7
10 1 0 3.08111 2.32358 8
10 1 0 3.80175 2.94237 6
11 1 0 21.9210 7.02554 6
11 1 0 31.4182 6.00154 7
11 1 0 32.1133 6.44549 4
11 1 0 36.4085 6.81820 8
12 1 0 72.6360 11.2379 6
12 1 0 65.8092 7.69850 7
12 1 0 77.7443 9.18833 4
12 1 0 66.9093 8.04396 8
13 1 0 87.5414 9.93281 4
13 1 0 78.4572 9.77329 6
14 -2 0 22.0914 6.00950 7
14 -2 0 10.0614 8.07438 4
14 -2 0 8.71733 5.81561 6
13 -2 0 17.4878 4.73785 7
13 -2 0 20.7971 6.36538 4
13 -2 0 15.2665 5.84117 6
12 -2 0 16.3275 4.03951 8
12 -2 0 10.9810 5.34077 4
12 -2 0 13.4392 5.35865 6
12 -2 0 16.9014 4.99469 7
11 -2 0 4.24641 2.73133 7
11 -2 0 3.66733 3.09180 4
11 -2 0 3.37008 3.21809 6
10 -2 0 110.984 10.0524 8
10 -2 0 118.217 10.5432 7
10 -2 0 117.877 11.0882 4
9 -2 0 -2.0950 1.97638 8
9 -2 0 0.03737 1.72512 4
9 -2 0 -1.2864 2.34739 3
9 -2 0 -0.2975 1.96704 7
8 -2 0 316.998 18.2624 7
8 -2 0 289.686 13.1108 8
8 -2 0 278.519 12.5715 2
8 -2 0 312.914 15.8755 3
8 -2 0 285.009 15.5976 4
7 -2 0 1201.55 33.6698 4
7 -2 0 1226.22 33.6250 3
7 -2 0 1231.44 32.6309 7
7 -2 0 1198.55 29.4643 2
7 -2 0 1174.70 29.2463 8
6 -2 0 102.101 6.48427 8
6 -2 0 103.926 7.48149 7
6 -2 0 104.098 7.87383 4
6 -2 0 118.776 7.16667 2
6 -2 0 104.315 8.05121 5
5 -2 0 57.9187 5.48311 3
5 -2 0 55.0188 4.62737 2
5 -2 0 49.9647 5.03527 4
5 -2 0 53.0018 4.95847 7
5 -2 0 47.8833 3.99857 8
5 -2 0 53.1432 5.25782 5
-5 2 0 44.1388 4.61938 7
-5 2 0 46.0630 4.45202 2
4 -2 0 781.741 18.0871 8
4 -2 0 842.331 19.9726 2
4 -2 0 814.636 20.9309 7
4 -2 0 814.090 21.6818 5
4 -2 0 806.120 20.4936 3
-4 2 0 823.756 20.3509 2
-4 2 0 825.762 21.2698 7
3 -2 0 2051.97 35.3926 8
3 -2 0 1994.66 37.6107 2
3 -2 0 1967.50 38.3563 7
3 -2 0 2009.04 38.7921 5
-3 2 0 1976.08 35.9795 8
-3 2 0 1979.24 38.4012 7
-3 2 0 2037.51 37.8379 2
2 -2 0 6670.97 136.375 1
-2 2 0 6633.92 138.512 1
1 -2 0 2.50288 0.91144 8
1 -2 0 2.58956 0.68536 6
1 -2 0 1.20133 0.66503 7
1 -2 0 0.38147 0.86548 2
-1 2 0 3.28970 1.21531 2
-1 2 0 5.10880 1.17317 8
0 -2 0 464.207 10.4432 7
0 -2 0 461.684 8.81253 6
0 -2 0 450.483 13.1743 3
0 2 0 465.204 10.3238 7
0 2 0 461.587 8.93124 6
0 2 0 430.109 12.4709 2
0 2 0 451.548 11.3915 8
-1 -2 0 6944.39 129.516 1
1 2 0 6764.95 130.822 1
-2 -2 0 749.774 17.5896 6
-2 -2 0 803.694 17.0980 5
-2 -2 0 808.831 23.5337 3
2 2 0 816.232 14.8743 4
2 2 0 764.589 22.1269 3
2 2 0 770.909 15.8610 5
2 2 0 774.802 16.7278 6
-3 -2 0 730.129 18.4186 5
-3 -2 0 758.672 24.8530 3
3 2 0 766.548 23.7761 3
3 2 0 749.949 16.1919 4
3 2 0 748.240 18.2869 6
3 2 0 746.321 17.2560 5
-4 -2 0 13.1897 4.31088 3
-4 -2 0 14.6204 3.18502 5
4 2 0 13.6123 3.79786 3
4 2 0 10.4791 2.44792 5
4 2 0 10.5879 2.53099 6
4 2 0 11.5631 2.31731 4
-5 -2 0 12.9302 3.24058 5
-5 -2 0 15.8530 4.79254 3
5 2 0 12.3155 2.78371 4
5 2 0 10.5836 2.94055 6
5 2 0 20.0020 5.77369 3
5 2 0 10.5051 2.53243 7
5 2 0 8.66263 2.46823 5
-6 -2 0 152.146 13.2091 3
6 2 0 170.301 9.01481 4
6 2 0 169.980 9.38291 5
6 2 0 159.054 8.35808 7
6 2 0 162.610 10.0842 6
6 2 0 156.125 12.5357 3
-7 -2 0 66.4619 9.23431 3
7 2 0 63.1293 5.56150 7
7 2 0 60.8791 7.01961 2
7 2 0 57.9364 6.56657 6
7 2 0 52.7522 5.56592 4
-8 -2 0 249.735 19.1693 3
8 2 0 242.744 12.0008 7
8 2 0 251.419 14.5035 6
8 2 0 258.367 14.4712 8
8 2 0 253.556 12.9142 4
-9 -2 0 265.070 20.7294 3
9 2 0 294.824 13.6306 7
9 2 0 276.133 15.9513 8
9 2 0 296.216 16.7583 6
9 2 0 315.817 15.3267 4
10 2 0 79.2150 8.18882 4
10 2 0 89.3961 9.93909 7
10 2 0 80.7483 8.96239 8
10 2 0 89.9529 9.47189 6
11 2 0 15.5381 4.76032 8
11 2 0 27.1395 6.79302 6
11 2 0 13.1268 4.23832 4
11 2 0 13.6432 3.88279 7
12 2 0 -2.3110 2.79715 8
12 2 0 -3.2977 2.99261 6
14 -3 0 -5.1897 3.33923 7
14 -3 0 14.5719 8.21858 4
13 -3 0 198.330 18.3105 6
13 -3 0 194.790 15.2122 7
13 -3 0 203.800 17.0385 4
12 -3 0 -0.3884 2.31312 7
12 -3 0 2.31421 3.96353 4
11 -3 0 83.2778 9.60371 8
11 -3 0 84.8865 9.56123 7
11 -3 0 73.0713 10.5229 4
10 -3 0 95.5793 7.64146 8
10 -3 0 110.738 10.2206 3
10 -3 0 128.121 11.7790 4
10 -3 0 109.880 10.3599 7
9 -3 0 26.9498 5.69766 3
9 -3 0 26.9432 5.06804 2
9 -3 0 29.5942 6.97060 4
9 -3 0 25.0465 4.38194 8
9 -3 0 18.1566 4.61903 7
8 -3 0 375.270 18.3384 4
8 -3 0 366.112 16.9796 3
8 -3 0 361.441 17.3088 7
8 -3 0 382.160 14.0537 8
8 -3 0 367.666 15.0695 2
7 -3 0 400.973 16.7388 3
7 -3 0 404.179 15.4713 2
7 -3 0 450.631 18.2283 7
7 -3 0 411.182 28.5228 4
7 -3 0 399.211 14.0630 8
-7 3 0 406.665 16.3743 2
6 -3 0 30.8344 4.21751 3
6 -3 0 26.3661 3.14998 8
6 -3 0 41.1001 6.82657 4
6 -3 0 37.0711 6.21970 5
6 -3 0 23.6975 4.32671 7
6 -3 0 26.0401 4.39874 2
-6 3 0 27.7218 5.38288 7
-6 3 0 35.5380 5.59359 2
5 -3 0 1080.44 28.1980 7
5 -3 0 1109.01 28.7654 5
5 -3 0 1072.99 23.4558 8
5 -3 0 1068.23 28.1145 4
5 -3 0 1089.30 26.6479 2
-5 3 0 1065.81 26.9027 2
4 -3 0 1247.32 29.4001 4
4 -3 0 1301.01 30.0223 7
4 -3 0 1264.49 25.6440 8
4 -3 0 1278.97 29.0463 2
4 -3 0 1270.16 29.7970 5
-4 3 0 1285.86 26.6751 8
-4 3 0 1282.00 29.1571 2
-4 3 0 1228.72 29.4949 7
3 -3 0 5529.80 94.9009 2
3 -3 0 5712.22 90.6452 8
-3 3 0 5420.94 98.2349 7
-3 3 0 5624.03 91.4299 8
-3 3 0 5700.13 94.8543 2
2 -3 0 2942.34 49.8342 8
2 -3 0 2903.33 52.0598 7
2 -3 0 2726.07 49.4519 6
2 -3 0 2917.65 54.0319 2
-2 3 0 2973.85 53.7405 2
-2 3 0 2965.03 50.6100 8
-2 3 0 2880.56 51.8997 7
1 -3 0 323.253 7.93271 6
1 -3 0 298.607 11.5036 2
1 -3 0 304.141 9.60462 8
1 -3 0 288.079 10.8770 3
1 -3 0 317.741 9.82677 7
-1 3 0 307.632 11.4528 2
-1 3 0 305.016 9.53913 7
-1 3 0 299.970 8.39919 6
0 -3 0 8.10767 1.69905 7
0 -3 0 4.67859 1.95411 3
0 -3 0 7.09272 1.14823 6
0 3 0 3.22553 1.35578 3
0 3 0 8.13982 2.18677 2
0 3 0 8.34250 1.40971 6
0 3 0 5.34723 1.45853 7
0 3 0 7.08660 1.76821 8
-1 -3 0 3446.66 67.0135 3
-1 -3 0 3443.68 54.9802 5
-1 -3 0 3485.04 56.7660 6
1 3 0 3372.73 65.5643 3
1 3 0 3403.39 61.4228 8
1 3 0 3346.73 56.9314 7
1 3 0 3509.76 64.2146 2
-2 -3 0 654.569 18.3842 6
-2 -3 0 663.324 15.2759 5
2 3 0 682.622 13.7627 5
2 3 0 674.533 14.6640 6
2 3 0 655.045 22.0513 3
2 3 0 673.733 15.0948 7
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_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7471
_exptl_absorpt_correction_T_min 0.7127
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71084 8.776 9.173 9.812 102.196 90.631 110.268
)
;
_shelx_hkl_checksum 36527
_shelx_res_file
;
c0047_0m.res created by SHELXL-2014/7
TITL c0047_0m_a.res in P-1
REM Old TITL c0047_0m_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.096, Rweak 0.005, Alpha 0.030, Orientation as input
REM Formula found by SHELXT: C17 O Si
CELL 0.71073 8.7737 9.1715 9.813 102.219 90.613 110.28
ZERR 2 0.0004 0.0004 0.0004 0.002 0.002 0.002
LATT 1
SFAC C H O Si
UNIT 34 36 2 2
EQIV $1 2-X,1-Y,1-Z
EQIV $2 +X,1+Y,+Z
L.S. 20
PLAN 2
SIZE 0.074 0.188 0.511
TEMP -173.15
CONF
HTAB C17 O1_$1
HTAB C15 O1_$2
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT -3 68
OMIT 0 0 1
OMIT 1 0 0
OMIT 0 1 0
REM
REM
REM
WGHT 0.039100 0.295100
FVAR 1.51595
SI1 4 0.698544 0.375349 0.342971 11.00000 0.01095 0.01317 =
0.01416 0.00181 0.00118 0.00328
O1 3 0.924169 0.222375 0.285398 11.00000 0.02024 0.01986 =
0.03135 0.01027 0.00828 0.01132
C1 1 0.863665 0.328973 0.243558 11.00000 0.01121 0.01338 =
0.01769 0.00197 0.00019 0.00398
C2 1 0.939452 0.388135 0.139243 11.00000 0.01557 0.02273 =
0.01984 0.00544 0.00399 0.00837
C3 1 1.074239 0.324503 0.101082 11.00000 0.01756 0.03091 =
0.02720 0.00506 0.00781 0.01037
H3A 2 1.181738 0.409864 0.124132 11.00000 0.03493
H3B 2 1.068050 0.281524 0.005219 11.00000 0.03717
C4 1 1.045740 0.200144 0.190816 11.00000 0.01937 0.02248 =
0.03182 0.00193 0.00508 0.01158
H4A 2 1.003369 0.090655 0.132870 11.00000 0.03669
H4B 2 1.143461 0.212872 0.249763 11.00000 0.03363
C5 1 0.507110 0.194772 0.298396 11.00000 0.01145 0.01496 =
0.01697 0.00359 0.00201 0.00418
C6 1 0.447469 0.117764 0.158863 11.00000 0.01435 0.01761 =
0.01687 0.00151 0.00231 0.00440
H6 2 0.497636 0.161072 0.085724 11.00000 0.02099
C7 1 0.312737 -0.023891 0.125622 11.00000 0.01504 0.01858 =
0.02167 -0.00136 0.00042 0.00439
H7 2 0.276082 -0.071582 0.029041 11.00000 0.02991
C8 1 0.234856 -0.091845 0.231868 11.00000 0.01582 0.01651 =
0.03070 0.00356 0.00226 0.00300
H8 2 0.140651 -0.195353 0.208766 11.00000 0.02802
C9 1 0.289603 -0.016168 0.370536 11.00000 0.01979 0.02097 =
0.02705 0.00877 0.00523 0.00189
H9 2 0.231665 -0.063307 0.449633 11.00000 0.03400
C10 1 0.424477 0.125712 0.403459 11.00000 0.01711 0.01974 =
0.01920 0.00561 0.00246 0.00256
H10 2 0.459502 0.174138 0.500697 11.00000 0.02466
C11 1 0.680032 0.551984 0.287400 11.00000 0.01379 0.01491 =
0.01776 0.00239 0.00378 0.00554
C12 1 0.546675 0.543713 0.202696 11.00000 0.01762 0.01852 =
0.02144 0.00463 0.00166 0.00709
H12 2 0.458793 0.446644 0.168988 11.00000 0.02115
C13 1 0.537311 0.679913 0.166686 11.00000 0.02521 0.02493 =
0.02486 0.00843 0.00201 0.01269
H13 2 0.446816 0.670169 0.110602 11.00000 0.02850
C14 1 0.662190 0.826260 0.213366 11.00000 0.03027 0.02063 =
0.02651 0.01002 0.00830 0.01326
H14 2 0.656005 0.920275 0.190808 11.00000 0.02907
C15 1 0.797325 0.836984 0.295788 11.00000 0.02430 0.01589 =
0.02923 0.00551 0.00699 0.00581
C16 1 0.805430 0.701452 0.332896 11.00000 0.01688 0.01686 =
0.02650 0.00418 0.00192 0.00432
H16 2 0.902003 0.711211 0.392171 11.00000 0.02853
C17 1 0.761693 0.428548 0.533831 11.00000 0.02050 0.02374 =
0.01606 0.00246 0.00011 0.00395
H17A 2 0.779085 0.341484 0.560702 11.00000 0.04226
H17B 2 0.678272 0.458920 0.584475 11.00000 0.04145
H15 2 0.885982 0.938092 0.329414 11.00000 0.02798
H17C 2 0.863462 0.523920 0.557392 11.00000 0.04453
H2 2 0.916125 0.467335 0.101446 11.00000 0.02790
HKLF 4
REM c0047_0m_a.res in P-1
REM R1 = 0.0398 for 4937 Fo > 4sig(Fo) and 0.0497 for all 5826 data
REM 244 parameters refined using 0 restraints
END
WGHT 0.0391 0.2951
REM Highest difference peak 0.484, deepest hole -0.268, 1-sigma level 0.055
Q1 1 0.6223 0.5550 0.2479 11.00000 0.05 0.48
Q2 1 0.6844 0.4559 0.3099 11.00000 0.05 0.45
;
_shelx_res_checksum 70266
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Si Si1 0.69854(3) 0.37535(3) 0.34297(3) 0.01325(7) Uani d 1 . .
O O1 0.92417(10) 0.22237(9) 0.28540(9) 0.02194(16) Uani d 1 . .
C C1 0.86366(11) 0.32897(11) 0.24356(10) 0.01447(16) Uani d 1 . .
C C2 0.93945(12) 0.38813(13) 0.13924(11) 0.01886(18) Uani d 1 . .
C C3 1.07424(14) 0.32450(15) 0.10108(13) 0.0250(2) Uani d 1 . .
H H3A 1.182(2) 0.410(2) 0.1241(18) 0.035(4) Uiso d 1 . .
H H3B 1.068(2) 0.282(2) 0.0052(19) 0.037(4) Uiso d 1 . .
C C4 1.04574(14) 0.20014(14) 0.19082(13) 0.0241(2) Uani d 1 . .
H H4A 1.003(2) 0.091(2) 0.1329(18) 0.037(4) Uiso d 1 . .
H H4B 1.143(2) 0.213(2) 0.2498(17) 0.034(4) Uiso d 1 . .
C C5 0.50711(11) 0.19477(11) 0.29840(10) 0.01461(16) Uani d 1 . .
C C6 0.44747(12) 0.11776(12) 0.15886(10) 0.01701(17) Uani d 1 . .
H H6 0.4976(18) 0.1611(17) 0.0857(15) 0.021(3) Uiso d 1 . .
C C7 0.31274(12) -0.02389(13) 0.12562(11) 0.01983(19) Uani d 1 . .
H H7 0.276(2) -0.0716(19) 0.0290(17) 0.030(4) Uiso d 1 . .
C C8 0.23486(13) -0.09184(13) 0.23187(13) 0.0221(2) Uani d 1 . .
H H8 0.1407(19) -0.1954(19) 0.2088(16) 0.028(4) Uiso d 1 . .
C C9 0.28960(13) -0.01617(13) 0.37054(12) 0.0235(2) Uani d 1 . .
H H9 0.232(2) -0.063(2) 0.4496(17) 0.034(4) Uiso d 1 . .
C C10 0.42448(12) 0.12571(13) 0.40346(11) 0.01958(18) Uani d 1 . .
H H10 0.4595(19) 0.1741(18) 0.5007(16) 0.025(4) Uiso d 1 . .
C C11 0.68003(11) 0.55198(11) 0.28740(10) 0.01557(16) Uani d 1 . .
C C12 0.54668(13) 0.54371(13) 0.20270(11) 0.01901(18) Uani d 1 . .
H H12 0.4588(18) 0.4466(18) 0.1690(15) 0.021(3) Uiso d 1 . .
C C13 0.53731(15) 0.67991(14) 0.16669(12) 0.0236(2) Uani d 1 . .
H H13 0.447(2) 0.6702(19) 0.1106(17) 0.029(4) Uiso d 1 . .
C C14 0.66219(15) 0.82626(14) 0.21337(12) 0.0239(2) Uani d 1 . .
H H14 0.6560(19) 0.9203(19) 0.1908(17) 0.029(4) Uiso d 1 . .
C C15 0.79733(14) 0.83698(13) 0.29579(13) 0.0234(2) Uani d 1 . .
C C16 0.80543(13) 0.70145(12) 0.33290(12) 0.02067(19) Uani d 1 . .
H H16 0.902(2) 0.7112(19) 0.3922(17) 0.029(4) Uiso d 1 . .
C C17 0.76169(14) 0.42855(14) 0.53383(11) 0.02152(19) Uani d 1 . .
H H17A 0.779(2) 0.341(2) 0.5607(19) 0.042(5) Uiso d 1 . .
H H17B 0.678(2) 0.459(2) 0.5845(19) 0.041(5) Uiso d 1 . .
H H15 0.886(2) 0.9381(19) 0.3294(16) 0.028(4) Uiso d 1 . .
H H17C 0.863(2) 0.524(2) 0.5574(19) 0.045(5) Uiso d 1 . .
H H2 0.9161(19) 0.4673(19) 0.1014(16) 0.028(4) 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
Si1 0.01095(11) 0.01317(12) 0.01416(12) 0.00328(9) 0.00118(8) 0.00181(9)
O1 0.0202(3) 0.0199(3) 0.0313(4) 0.0113(3) 0.0083(3) 0.0103(3)
C1 0.0112(3) 0.0134(4) 0.0177(4) 0.0040(3) 0.0002(3) 0.0020(3)
C2 0.0156(4) 0.0227(5) 0.0198(4) 0.0084(3) 0.0040(3) 0.0054(4)
C3 0.0176(4) 0.0309(6) 0.0272(5) 0.0104(4) 0.0078(4) 0.0051(4)
C4 0.0194(4) 0.0225(5) 0.0318(6) 0.0116(4) 0.0051(4) 0.0019(4)
C5 0.0114(3) 0.0150(4) 0.0170(4) 0.0042(3) 0.0020(3) 0.0036(3)
C6 0.0144(4) 0.0176(4) 0.0169(4) 0.0044(3) 0.0023(3) 0.0015(3)
C7 0.0150(4) 0.0186(4) 0.0217(4) 0.0044(3) 0.0004(3) -0.0014(3)
C8 0.0158(4) 0.0165(4) 0.0307(5) 0.0030(3) 0.0023(4) 0.0036(4)
C9 0.0198(4) 0.0210(5) 0.0270(5) 0.0019(4) 0.0052(4) 0.0088(4)
C10 0.0171(4) 0.0197(4) 0.0192(4) 0.0026(3) 0.0025(3) 0.0056(4)
C11 0.0138(4) 0.0149(4) 0.0178(4) 0.0055(3) 0.0038(3) 0.0024(3)
C12 0.0176(4) 0.0185(4) 0.0214(4) 0.0071(3) 0.0017(3) 0.0046(3)
C13 0.0252(5) 0.0249(5) 0.0249(5) 0.0127(4) 0.0020(4) 0.0084(4)
C14 0.0303(5) 0.0206(5) 0.0265(5) 0.0133(4) 0.0083(4) 0.0100(4)
C15 0.0243(5) 0.0159(4) 0.0292(5) 0.0058(4) 0.0070(4) 0.0055(4)
C16 0.0169(4) 0.0169(4) 0.0265(5) 0.0043(3) 0.0019(4) 0.0042(4)
C17 0.0205(4) 0.0237(5) 0.0161(4) 0.0040(4) 0.0001(3) 0.0025(4)
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'
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
C5 Si1 C1 . . 108.44(4) ?
C11 Si1 C1 . . 105.50(4) ?
C11 Si1 C5 . . 113.08(4) ?
C17 Si1 C1 . . 109.26(5) ?
C17 Si1 C5 . . 110.48(5) ?
C17 Si1 C11 . . 109.89(5) ?
C1 O1 C4 . . 107.48(8) ?
O1 C1 Si1 . . 117.13(7) ?
C2 C1 Si1 . . 129.71(8) ?
C2 C1 O1 . . 113.10(9) ?
C1 C2 C3 . . 110.25(9) ?
C1 C2 H2 . . 123.6(9) ?
C3 C2 H2 . . 126.0(9) ?
C2 C3 H3A . . 111.2(10) ?
C2 C3 H3B . . 112.3(11) ?
C2 C3 C4 . . 101.51(9) ?
H3A C3 H3B . . 105.5(14) ?
C4 C3 H3A . . 112.9(10) ?
C4 C3 H3B . . 113.7(11) ?
O1 C4 C3 . . 106.70(8) ?
O1 C4 H4A . . 108.8(10) ?
O1 C4 H4B . . 107.0(10) ?
C3 C4 H4A . . 111.5(10) ?
C3 C4 H4B . . 114.2(10) ?
H4A C4 H4B . . 108.4(14) ?
C6 C5 Si1 . . 121.29(7) ?
C10 C5 Si1 . . 120.94(7) ?
C10 C5 C6 . . 117.64(9) ?
C5 C6 H6 . . 120.3(9) ?
C7 C6 C5 . . 121.26(9) ?
C7 C6 H6 . . 118.4(9) ?
C6 C7 H7 . . 118.2(10) ?
C8 C7 C6 . . 119.98(10) ?
C8 C7 H7 . . 121.8(10) ?
C7 C8 H8 . . 120.4(9) ?
C9 C8 C7 . . 119.76(10) ?
C9 C8 H8 . . 119.8(9) ?
C8 C9 H9 . . 120.5(9) ?
C8 C9 C10 . . 120.10(10) ?
C10 C9 H9 . . 119.4(9) ?
C5 C10 H10 . . 121.0(9) ?
C9 C10 C5 . . 121.24(10) ?
C9 C10 H10 . . 117.7(9) ?
C12 C11 Si1 . . 123.40(7) ?
C12 C11 C16 . . 117.71(9) ?
C16 C11 Si1 . . 118.89(8) ?
C11 C12 H12 . . 121.5(9) ?
C13 C12 C11 . . 121.09(10) ?
C13 C12 H12 . . 117.4(9) ?
C12 C13 H13 . . 118.8(10) ?
C14 C13 C12 . . 120.16(10) ?
C14 C13 H13 . . 121.0(10) ?
C13 C14 H14 . . 120.8(10) ?
C13 C14 C15 . . 119.80(10) ?
C15 C14 H14 . . 119.4(10) ?
C14 C15 C16 . . 119.92(10) ?
C14 C15 H15 . . 121.1(9) ?
C16 C15 H15 . . 119.0(9) ?
C11 C16 H16 . . 119.7(9) ?
C15 C16 C11 . . 121.32(10) ?
C15 C16 H16 . . 118.9(9) ?
Si1 C17 H17A . . 109.9(11) ?
Si1 C17 H17B . . 108.7(11) ?
Si1 C17 H17C . . 110.5(11) ?
H17A C17 H17B . . 112.2(15) ?
H17A C17 H17C . . 109.4(15) ?
H17B C17 H17C . . 106.1(15) ?
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
Si1 C1 . 1.8743(10) ?
Si1 C5 . 1.8720(9) ?
Si1 C11 . 1.8715(10) ?
Si1 C17 . 1.8591(11) ?
O1 C1 . 1.3897(12) ?
O1 C4 . 1.4603(13) ?
C1 C2 . 1.3356(14) ?
C2 C3 . 1.5082(15) ?
C2 H2 . 0.961(16) ?
C3 H3A . 0.981(17) ?
C3 H3B . 0.933(18) ?
C3 C4 . 1.5398(18) ?
C4 H4A . 0.982(17) ?
C4 H4B . 0.987(17) ?
C5 C6 . 1.4023(14) ?
C5 C10 . 1.4014(13) ?
C6 H6 . 0.934(15) ?
C6 C7 . 1.3926(14) ?
C7 H7 . 0.956(16) ?
C7 C8 . 1.3919(16) ?
C8 H8 . 0.998(16) ?
C8 C9 . 1.3854(17) ?
C9 H9 . 1.023(16) ?
C9 C10 . 1.3944(15) ?
C10 H10 . 0.960(15) ?
C11 C12 . 1.3988(14) ?
C11 C16 . 1.4050(14) ?
C12 H12 . 0.944(15) ?
C12 C13 . 1.3962(15) ?
C13 H13 . 0.928(16) ?
C13 C14 . 1.3861(17) ?
C14 H14 . 0.953(16) ?
C14 C15 . 1.3909(17) ?
C15 C16 . 1.3911(15) ?
C15 H15 . 0.969(16) ?
C16 H16 . 0.990(16) ?
C17 H17A . 0.950(18) ?
C17 H17B . 0.975(19) ?
C17 H17C . 0.992(19) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C15 H15 O1 1_565 0.969(16) 2.640(16) 3.3422(13) 129.6(12)
C17 H17C O1 2_766 0.992(19) 2.584(19) 3.5168(14) 156.5(15)
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
Si1 C1 C2 C3 . . . . 175.12(8) ?
Si1 C5 C6 C7 . . . . 174.69(8) ?
Si1 C5 C10 C9 . . . . -174.66(9) ?
Si1 C11 C12 C13 . . . . 178.63(8) ?
Si1 C11 C16 C15 . . . . -179.42(8) ?
O1 C1 C2 C3 . . . . -2.00(12) ?
C1 Si1 C5 C6 . . . . -51.23(9) ?
C1 Si1 C5 C10 . . . . 124.48(8) ?
C1 Si1 C11 C12 . . . . 109.11(9) ?
C1 Si1 C11 C16 . . . . -71.17(9) ?
C1 O1 C4 C3 . . . . 8.95(11) ?
C1 C2 C3 C4 . . . . 7.17(12) ?
C2 C3 C4 O1 . . . . -9.52(11) ?
C4 O1 C1 Si1 . . . . 177.92(7) ?
C4 O1 C1 C2 . . . . -4.57(12) ?
C5 Si1 C1 O1 . . . . -70.80(8) ?
C5 Si1 C1 C2 . . . . 112.17(10) ?
C5 Si1 C11 C12 . . . . -9.26(10) ?
C5 Si1 C11 C16 . . . . 170.46(8) ?
C5 C6 C7 C8 . . . . -0.15(16) ?
C6 C5 C10 C9 . . . . 1.20(15) ?
C6 C7 C8 C9 . . . . 1.46(16) ?
C7 C8 C9 C10 . . . . -1.42(17) ?
C8 C9 C10 C5 . . . . 0.07(17) ?
C10 C5 C6 C7 . . . . -1.15(15) ?
C11 Si1 C1 O1 . . . . 167.77(7) ?
C11 Si1 C1 C2 . . . . -9.26(11) ?
C11 Si1 C5 C6 . . . . 65.41(9) ?
C11 Si1 C5 C10 . . . . -118.88(9) ?
C11 C12 C13 C14 . . . . 0.82(17) ?
C12 C11 C16 C15 . . . . 0.31(15) ?
C12 C13 C14 C15 . . . . 0.27(17) ?
C13 C14 C15 C16 . . . . -1.03(17) ?
C14 C15 C16 C11 . . . . 0.74(17) ?
C16 C11 C12 C13 . . . . -1.09(15) ?
C17 Si1 C1 O1 . . . . 49.68(8) ?
C17 Si1 C1 C2 . . . . -127.35(10) ?
C17 Si1 C5 C6 . . . . -170.95(8) ?
C17 Si1 C5 C10 . . . . 4.76(10) ?
C17 Si1 C11 C12 . . . . -133.23(9) ?
C17 Si1 C11 C16 . . . . 46.49(9) ?
_cod_database_fobs_code 2243948