#------------------------------------------------------------------------------
#$Date: 2024-08-14 04:53:19 +0300 (Wed, 14 Aug 2024) $
#$Revision: 294107 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312580.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_2312580
loop_
_publ_author_name
'Van Der Sluys, William G.'
_publ_section_title
;
Concerning the structures of Lewis base adducts of titanium(IV)
hexafluoroisopropoxide.
;
_journal_coeditor_code SON3002
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624006843
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Ti (C3 H F6 O1)3 Cl (C4 H8 O1)2]'
_chemical_formula_moiety 'C17 H19 Cl F18 O5 Ti'
_chemical_formula_sum 'C17 H19 Cl F18 O5 Ti'
_chemical_formula_weight 728.67
_chemical_name_systematic
Chloridotris(hexafluoroisopropoxido-\kO)bis(tetrahydrofuran-\kO)titanium(IV)
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 108.450(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.050(4)
_cell_length_b 10.701(3)
_cell_length_c 18.692(5)
_cell_measurement_reflns_used 9958
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 24.29
_cell_measurement_theta_min 2.22
_cell_volume 2665.9(13)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type 'Bruker APEX CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0582
_diffrn_reflns_av_unetI/netI 0.0335
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 67346
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.677
_diffrn_reflns_theta_min 2.223
_exptl_absorpt_coefficient_mu 0.575
_exptl_absorpt_correction_T_max 0.904
_exptl_absorpt_correction_T_min 0.864
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
[TWINABS (Sheldrick, 2015c) and
SADABS (Krause et al. (2015)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.816
_exptl_crystal_description block
_exptl_crystal_F_000 1448
_exptl_crystal_size_max 0.262
_exptl_crystal_size_mid 0.182
_exptl_crystal_size_min 0.180
_refine_diff_density_max 0.564
_refine_diff_density_min -0.707
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.984
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 379
_refine_ls_number_reflns 4968
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.984
_refine_ls_R_factor_all 0.0551
_refine_ls_R_factor_gt 0.0420
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1162
_refine_ls_wR_factor_ref 0.1229
_reflns_number_gt 3934
_reflns_number_total 4968
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file son3002.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2312580
_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 0.864
_shelx_estimated_absorpt_t_max 0.904
_shelx_hkl_file
;
2 0 0 373.826 9.51352
3 0 0 282.150 6.53485
4 0 0 31.4902 0.83772
5 0 0 29.5040 0.87352
6 0 0 98.1588 2.03567
7 0 0 229.592 4.49139
8 0 0 315.888 5.92882
9 0 0 17.3501 1.23273
10 0 0 21.3070 1.44068
11 0 0 50.6078 2.37221
12 0 0 170.605 5.05156
13 0 0 6.56076 1.38368
14 0 0 4.24016 2.80291
15 0 0 119.256 6.47816
16 0 0 5.52983 7.99506
0 1 0 0.13278 0.12979
1 1 0 1690.04 28.0952
2 1 0 6.84166 0.27459
3 1 0 2.76490 0.20420
4 1 0 729.854 9.28888
5 1 0 119.904 1.68373
6 1 0 82.1291 1.30863
7 1 0 584.598 7.92540
8 1 0 581.155 8.19428
9 1 0 32.1568 1.24040
10 1 0 6.96437 0.81343
11 1 0 80.5554 2.14222
12 1 0 14.6063 1.39846
13 1 0 2.23044 1.36369
14 1 0 290.237 6.51985
15 1 0 9.97162 2.49029
16 1 0 12.1493 7.09572
0 2 0 91.6680 1.97705
1 2 0 71.3883 1.01981
2 2 0 1576.23 19.0570
3 2 0 72.1936 1.18541
4 2 0 267.189 4.05265
5 2 0 24.6244 0.63420
6 2 0 243.894 3.28033
7 2 0 716.124 9.23419
8 2 0 1.05606 0.34804
9 2 0 1.76081 0.59035
10 2 0 118.074 2.72256
11 2 0 47.7826 1.83959
12 2 0 81.4562 2.55686
13 2 0 28.3172 1.98099
14 2 0 4.44161 2.00422
15 2 0 113.273 3.72211
16 2 0 2.35770 4.77697
0 3 0 0.14783 0.24221
1 3 0 1025.29 12.2069
2 3 0 116.896 1.53988
3 3 0 268.490 3.59135
4 3 0 125.213 1.98960
5 3 0 13.1951 0.53835
6 3 0 155.942 2.59839
7 3 0 42.6192 1.09916
8 3 0 19.6075 0.86505
9 3 0 1.57438 0.90518
10 3 0 8.29875 1.43131
11 3 0 35.3198 1.54944
12 3 0 5.39293 1.30293
13 3 0 31.9148 2.03794
14 3 0 61.3583 2.51172
15 3 0 2.40315 1.71833
0 4 0 383.354 7.58006
1 4 0 262.159 3.55301
2 4 0 0.43433 0.17973
3 4 0 1.92100 0.23117
4 4 0 102.670 1.53623
5 4 0 1.79865 0.40981
6 4 0 99.4143 1.85367
7 4 0 113.394 2.23804
8 4 0 2.69201 0.90271
9 4 0 195.811 4.02783
10 4 0 26.5362 1.61473
11 4 0 56.3823 2.29272
12 4 0 2.71080 1.64653
13 4 0 54.1424 2.42053
14 4 0 18.8073 2.21017
15 4 0 30.8512 4.80207
0 5 0 2.70542 0.47107
1 5 0 153.345 2.35882
2 5 0 17.1239 0.49869
3 5 0 128.484 1.88587
4 5 0 140.024 1.90261
5 5 0 139.545 2.14039
6 5 0 24.9754 1.29110
7 5 0 53.4133 1.75541
8 5 0 63.6532 2.26293
9 5 0 0.20849 0.92077
10 5 0 32.6610 1.67704
11 5 0 62.5296 2.88994
12 5 0 19.8349 1.88863
13 5 0 14.0261 1.66814
14 5 0 15.1511 1.87057
15 5 0 8.54036 2.40115
0 6 0 209.886 4.72879
1 6 0 90.0746 2.63205
2 6 0 290.475 5.08386
3 6 0 12.8656 0.90505
4 6 0 74.6997 1.87365
5 6 0 6.20382 0.52325
6 6 0 68.4936 2.01145
7 6 0 7.46930 1.01710
8 6 0 4.71603 1.42482
9 6 0 2.71935 1.22932
10 6 0 44.9157 2.23066
11 6 0 23.0112 2.82251
12 6 0 6.65471 2.54189
13 6 0 17.7078 4.56728
14 6 0 2.31986 4.71624
1 7 0 7.41697 0.94470
2 7 0 20.5408 1.24407
3 7 0 4.37188 0.82780
4 7 0 0.00000 0.77037
5 7 0 9.26773 0.94303
6 7 0 10.2532 1.39856
7 7 0 27.5999 1.45882
8 7 0 96.2715 2.96917
9 7 0 1.24567 0.90802
10 7 0 49.1518 2.28472
11 7 0 0.00000 3.91694
12 7 0 3.68185 4.13697
0 8 0 90.3517 2.77939
1 8 0 5.89693 1.09801
2 8 0 17.5659 1.07523
3 8 0 125.050 2.45481
4 8 0 47.6405 1.95918
5 8 0 5.09709 1.16858
6 8 0 0.49150 0.83117
7 8 0 43.6369 1.73458
8 8 0 10.8763 1.41593
9 8 0 9.95444 1.74251
10 8 0 3.22298 1.58851
11 8 0 3.21267 1.79308
12 8 0 0.00000 2.06468
1 9 0 57.8070 1.90496
2 9 0 8.47727 0.96168
3 9 0 25.7930 1.25527
4 9 0 3.37458 0.98842
5 9 0 2.94612 0.96716
6 9 0 4.01675 0.96279
7 9 0 2.15413 0.91746
8 9 0 3.03829 1.69888
9 9 0 33.1618 2.51154
10 9 0 8.51626 1.94591
11 9 0 6.87553 2.14847
0 10 0 33.3910 2.28564
1 10 0 88.1568 2.44979
2 10 0 10.3941 1.19890
3 10 0 15.7801 1.29502
4 10 0 0.44893 1.17523
5 10 0 28.1035 1.75443
6 10 0 45.5862 1.92250
7 10 0 30.8678 1.96018
8 10 0 3.35526 1.17112
9 10 0 3.30001 1.65444
10 10 0 0.97421 1.91073
0 11 0 0.00000 2.51373
1 11 0 22.7522 1.84207
2 11 0 22.2309 1.66796
3 11 0 7.38587 1.50469
4 11 0 1.58509 1.15049
5 11 0 2.45236 1.65599
6 11 0 5.69232 1.81642
7 11 0 1.83931 1.94758
8 11 0 26.9751 3.08687
9 11 0 7.42195 4.21231
0 12 0 213.841 8.08901
1 12 0 21.7319 2.81086
2 12 0 0.00000 1.92833
3 12 0 19.7845 2.14876
4 12 0 0.11634 1.81556
5 12 0 5.51754 3.20418
6 12 0 20.6569 7.35019
1 13 0 63.6319 9.95978
-12 0 1 0.39809 0.98238
-11 0 1 0.00000 0.84402
-10 0 1 0.39218 0.70734
-9 0 1 0.66919 0.72908
-8 0 1 0.08329 0.51473
-7 0 1 0.31391 0.50489
-6 0 1 0.26153 0.50434
-5 0 1 0.10461 0.29469
-4 0 1 0.08763 0.29456
-3 0 1 0.09097 0.40023
-2 0 1 0.85628 0.23561
1 0 1 0.03516 0.15188
2 0 1 0.05665 0.29852
3 0 1 0.55941 0.35265
4 0 1 0.26138 0.27925
5 0 1 0.26307 0.36619
6 0 1 0.09467 0.29163
7 0 1 0.29809 0.36466
8 0 1 0.07876 0.45473
9 0 1 0.33292 0.60204
10 0 1 0.10726 0.70948
11 0 1 0.23840 0.80890
12 0 1 0.83295 0.96560
13 0 1 0.50655 1.23000
14 0 1 0.14896 2.29127
-16 1 1 1.65216 3.81788
-15 1 1 4.12367 1.99010
-14 1 1 58.8394 2.67334
-13 1 1 57.1569 2.29395
-12 1 1 1.31279 1.11107
-11 1 1 0.78163 0.84842
-10 1 1 33.0135 1.30899
-9 1 1 120.448 2.39653
-8 1 1 26.2312 0.77205
-7 1 1 68.7203 1.17057
-6 1 1 11.9219 0.45110
-5 1 1 16.5874 0.47265
-4 1 1 135.414 1.93742
-3 1 1 555.769 7.44840
-2 1 1 27.2807 0.49370
-1 1 1 63.9195 1.11897
0 1 1 149.217 2.42055
1 1 1 53.7759 0.89266
2 1 1 268.640 3.44951
3 1 1 9.50884 0.30121
4 1 1 0.43437 0.19752
5 1 1 226.777 3.17199
6 1 1 8.21993 0.40548
7 1 1 33.7274 0.77507
8 1 1 10.3868 0.71140
9 1 1 1.15512 0.55187
10 1 1 15.4874 1.00173
11 1 1 0.38807 0.68734
12 1 1 3.78825 0.91863
13 1 1 79.5446 2.45573
14 1 1 2.41721 1.56115
15 1 1 13.5702 2.23376
-16 2 1 0.00000 3.11672
-15 2 1 18.7630 3.06583
-14 2 1 0.00000 1.67968
-13 2 1 63.1684 2.56333
-12 2 1 50.0367 2.15102
-11 2 1 77.9026 2.27412
-10 2 1 3.94460 1.02989
-9 2 1 48.7200 1.23602
-8 2 1 22.4307 0.67986
-7 2 1 70.1736 1.24232
-6 2 1 97.3104 1.66929
-5 2 1 352.700 5.31747
-4 2 1 48.6323 0.92029
-3 2 1 160.669 2.40715
-2 2 1 282.042 3.34468
-1 2 1 0.23209 0.12804
0 2 1 84.6909 1.24297
1 2 1 620.851 7.42849
2 2 1 155.827 2.02788
3 2 1 585.551 8.34526
4 2 1 0.80960 0.26875
5 2 1 101.095 1.46850
6 2 1 11.3596 0.47461
7 2 1 7.22810 0.42185
8 2 1 256.547 3.95456
9 2 1 0.38978 0.49762
10 2 1 12.6329 1.08208
11 2 1 76.0467 2.29600
12 2 1 67.9090 2.58019
13 2 1 15.6537 1.80345
14 2 1 1.76962 1.82449
15 2 1 0.00000 1.65542
-16 3 1 0.00000 6.32379
-15 3 1 8.96185 2.08525
-14 3 1 1.04010 1.64290
-13 3 1 61.5104 2.18796
-12 3 1 0.00000 1.23682
-11 3 1 3.86914 1.29515
-10 3 1 4.66456 1.04814
-9 3 1 23.1010 1.06357
-8 3 1 5.96970 0.81665
-7 3 1 28.4429 0.93533
-6 3 1 92.0204 1.64513
-5 3 1 3.60000 0.40309
-4 3 1 16.4736 0.55176
-3 3 1 59.6863 0.88256
-2 3 1 65.0568 0.90946
-1 3 1 332.091 4.20750
0 3 1 28.5114 0.55697
1 3 1 822.744 9.57153
2 3 1 475.475 5.69094
3 3 1 76.0780 1.11820
4 3 1 47.7600 0.94503
5 3 1 17.7110 0.60582
6 3 1 0.50194 0.35077
7 3 1 58.0377 1.23159
8 3 1 46.6761 1.30728
9 3 1 363.094 6.26520
10 3 1 2.22595 0.90548
11 3 1 1.77070 1.13335
12 3 1 110.838 3.09943
13 3 1 16.5520 1.68737
14 3 1 0.00000 1.68744
15 3 1 43.7887 3.10924
-15 4 1 37.6146 2.96881
-14 4 1 38.2052 2.54747
-13 4 1 37.8393 2.37859
-12 4 1 230.394 5.37182
-11 4 1 3.93539 1.17223
-10 4 1 18.4966 1.34646
-9 4 1 45.9486 1.68526
-8 4 1 12.2370 0.91548
-7 4 1 17.2444 1.22197
-6 4 1 0.43344 0.60002
-5 4 1 74.5415 1.49207
-4 4 1 196.687 2.62170
-3 4 1 74.2109 1.10008
-2 4 1 109.851 1.40358
-1 4 1 200.053 2.64849
0 4 1 8.23507 0.35205
1 4 1 0.60297 0.20338
2 4 1 4.62861 0.26861
3 4 1 153.147 2.00444
4 4 1 215.572 2.86413
5 4 1 279.390 4.01662
6 4 1 5.42949 0.56683
7 4 1 162.267 2.99133
8 4 1 597.324 9.23190
9 4 1 164.008 3.56700
10 4 1 205.464 4.73785
11 4 1 5.12391 1.38875
12 4 1 69.4474 2.84399
13 4 1 54.0950 2.58430
14 4 1 31.7575 2.20858
15 4 1 0.50507 3.60348
-15 5 1 1.41104 2.49810
-14 5 1 2.87374 1.69306
-13 5 1 82.5175 3.38779
-12 5 1 117.574 3.95751
-11 5 1 18.3368 1.46166
-10 5 1 52.2053 2.53024
-9 5 1 42.0635 1.92793
-8 5 1 8.41242 1.05189
-7 5 1 67.4477 1.67365
-6 5 1 352.268 5.99867
-5 5 1 87.5047 1.71309
-4 5 1 5.21566 0.53213
-3 5 1 6.47761 0.44216
-2 5 1 9.91068 0.52046
-1 5 1 1.86749 0.30603
0 5 1 267.014 3.70452
1 5 1 2.13701 0.26879
2 5 1 223.738 2.81706
3 5 1 74.0173 1.18901
4 5 1 233.863 3.09006
5 5 1 10.7290 0.54221
6 5 1 612.904 9.06287
7 5 1 234.313 4.11875
8 5 1 292.966 5.01541
9 5 1 7.03399 0.92928
10 5 1 4.67926 1.24612
11 5 1 1.68267 1.14682
12 5 1 49.6064 2.27221
13 5 1 18.6330 1.69632
14 5 1 0.56538 1.65038
-13 6 1 6.41138 2.46981
-12 6 1 0.00000 3.02420
-11 6 1 1.05054 2.74611
-10 6 1 0.00000 0.98569
-9 6 1 15.5621 1.81217
-8 6 1 334.636 6.23072
-7 6 1 152.189 3.60995
-6 6 1 342.557 5.09393
-5 6 1 7.46396 0.72476
-4 6 1 310.206 4.63679
-3 6 1 141.352 2.31039
-2 6 1 175.552 2.85791
-1 6 1 135.717 2.58094
0 6 1 39.8615 1.44521
1 6 1 261.376 4.22092
2 6 1 225.835 3.89993
3 6 1 7.78118 0.66872
4 6 1 30.7759 1.07535
5 6 1 250.316 4.05947
6 6 1 1.15155 0.56597
7 6 1 62.0661 1.90454
8 6 1 162.514 3.93132
9 6 1 6.78324 1.26562
10 6 1 18.6757 1.80709
11 6 1 1.78738 1.30300
12 6 1 36.0884 2.40689
13 6 1 9.32772 1.74863
-13 7 1 44.8904 4.92130
-12 7 1 60.0837 5.75077
-11 7 1 3.51999 3.98889
-10 7 1 13.8697 1.59527
-9 7 1 7.17130 1.22099
-8 7 1 61.8907 2.37123
-7 7 1 52.3930 1.82382
-6 7 1 295.333 5.80363
-5 7 1 6.08803 0.85538
-4 7 1 6.22458 0.78573
-3 7 1 5.68593 0.73729
-2 7 1 253.279 3.98541
-1 7 1 247.149 3.77966
0 7 1 268.090 4.28996
1 7 1 6.37623 0.83977
2 7 1 36.8575 1.14048
3 7 1 12.2926 0.91390
4 7 1 18.5846 1.10882
5 7 1 30.6628 1.39626
6 7 1 161.331 3.51388
7 7 1 52.6206 1.95454
8 7 1 33.3642 1.78637
9 7 1 9.03060 1.15898
10 7 1 28.2139 1.87255
11 7 1 2.32644 1.58780
12 7 1 22.6522 4.66272
-12 8 1 50.0542 4.32657
-11 8 1 68.4207 3.93830
-10 8 1 1.69391 1.11831
-9 8 1 8.74172 1.41605
-8 8 1 34.8392 2.01181
-7 8 1 123.171 2.65073
-6 8 1 39.5275 1.55235
-5 8 1 75.1757 1.82128
-4 8 1 6.55348 0.86369
-3 8 1 151.357 3.10568
-2 8 1 11.6693 1.05875
-1 8 1 38.4384 1.29178
0 8 1 41.6087 1.55202
1 8 1 126.730 2.65305
2 8 1 5.18948 0.92966
3 8 1 21.5644 1.20092
4 8 1 406.846 6.88836
5 8 1 184.397 3.46986
6 8 1 1.61702 0.72311
7 8 1 114.255 2.91227
8 8 1 55.9034 2.43705
9 8 1 1.43017 1.06588
10 8 1 13.6424 1.73262
11 8 1 33.8357 2.84813
12 8 1 12.8453 4.29092
-11 9 1 0.76154 1.78864
-10 9 1 8.38825 1.59056
-9 9 1 28.5870 2.06048
-8 9 1 1.88544 1.26723
-7 9 1 93.2369 2.50781
-6 9 1 62.0034 2.03366
-5 9 1 10.9574 1.20966
-4 9 1 10.0444 1.19484
-3 9 1 18.6517 1.34007
-2 9 1 213.956 3.99559
-1 9 1 131.857 2.94536
0 9 1 60.3589 1.76629
1 9 1 32.8354 1.39129
2 9 1 13.6771 1.08733
3 9 1 25.9133 1.40103
4 9 1 4.67675 1.03419
5 9 1 1.16549 1.00750
6 9 1 132.483 3.08895
7 9 1 102.800 2.85410
8 9 1 77.0679 2.92717
9 9 1 18.4894 2.23080
10 9 1 0.36401 2.29208
11 9 1 1.68733 2.84381
-11 10 1 15.0807 4.79887
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-3 1 21 19.4098 2.21902
-2 1 21 45.7366 3.09889
-1 1 21 1.14655 1.87836
0 1 21 0.00000 3.52780
-10 2 21 0.85966 2.38183
-9 2 21 1.15387 1.74521
-8 2 21 3.94150 1.71214
-7 2 21 6.61812 1.50717
-6 2 21 0.97346 1.71857
-5 2 21 2.02759 1.43309
-4 2 21 0.00000 1.53381
-3 2 21 18.9685 2.16313
-2 2 21 17.7788 2.28650
-1 2 21 7.85370 2.41719
0 2 21 16.1800 4.58557
-10 3 21 6.63822 2.66397
-9 3 21 4.54040 1.77351
-8 3 21 7.94742 1.76529
-7 3 21 0.00935 1.40543
-6 3 21 0.23493 1.74352
-5 3 21 1.21729 1.46431
-4 3 21 12.9835 1.96302
-3 3 21 0.52281 1.67176
-2 3 21 6.05615 2.64204
-1 3 21 27.2064 5.20770
0 3 21 0.00000 3.93206
1 3 21 18.7044 6.34545
-8 4 21 1.33173 1.78657
-7 4 21 25.2810 2.50934
-6 4 21 13.4723 2.68112
-5 4 21 0.85824 1.94692
-4 4 21 7.74499 2.45760
-3 4 21 21.5297 4.31562
-8 5 21 57.8825 7.05182
-7 5 21 1.99515 3.42978
-5 5 21 26.5641 4.80004
-4 5 21 1.88432 2.16047
-3 5 21 16.8808 4.25066
-2 5 21 8.82392 4.47272
-9 0 22 45.2883 6.37489
-8 0 22 24.0608 4.61864
-6 0 22 12.0868 3.40945
-5 0 22 19.7660 3.79631
-4 0 22 6.51542 2.65406
-3 0 22 109.364 6.73007
-9 1 22 6.22538 2.76596
-8 1 22 6.35426 2.17671
-7 1 22 16.3624 4.67752
-6 1 22 25.9648 3.76136
-5 1 22 1.37139 1.73362
-4 1 22 65.7926 4.10209
-3 1 22 8.13450 3.44204
-9 2 22 15.3751 4.49600
-8 2 22 33.8542 3.17118
-7 2 22 3.63855 2.32639
-6 2 22 0.26396 2.07273
-5 2 22 57.6854 3.98388
-4 2 22 0.35780 1.99430
-3 2 22 81.7547 5.75395
-2 2 22 35.8997 6.19295
-9 3 22 24.0078 6.20150
-8 3 22 2.58468 2.29317
-7 3 22 25.4804 3.42993
-6 3 22 5.01796 2.46656
-5 3 22 15.9379 2.98593
-4 3 22 28.6101 3.61023
-3 3 22 0.93052 3.94947
-2 3 22 9.58152 5.21684
-6 0 23 0.22571 3.72390
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 23474
_shelx_res_file
;
TITL 18084 in P2(1)/c
18084.res
created by SHELXL-2018/1 at 10:18:40 on 18-Mar-2018
CELL 0.71073 14.050 10.701 18.692 90.0000 108.450 90.0000
ZERR 4.00 0.004 0.003 0.005 0.0000 0.003 0.0000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H O F CL TI
UNIT 68 76 20 72 4 4
shel 20.0 0.820
TEMP -173.17
SIZE 0.18 0.182 0.262
acta
conf
wpdb -2
HTAB C2 Cl1
HTAB C5 Cl1
HTAB C10 F3
EQIV $1 -x+1, -y+1, -z+1
HTAB C10 F17_$1
EQIV $2 -x, y+1/2, -z+1/2
HTAB C11 F2_$2
EQIV $3 -x, -y+1, -z+1
HTAB C12 Cl1_$3
EQIV $4 x, y+1, z
HTAB C12 F9_$4
HTAB C13 Cl1_$3
HTAB C14 F12
HTAB C17 F15_$1
HTAB C17 O4
htab
L.S. 10 4
BOND $H
FMAP 2
PLAN 20
WGHT 0.090000 0.400000
FVAR 0.22080
TI1 6 0.237572 0.278769 0.526594 11.00000 0.01106 0.01397 =
0.01316 -0.00024 0.00517 -0.00076
CL1 5 0.083723 0.290341 0.549940 11.00000 0.01433 0.02145 =
0.02589 0.00001 0.01068 0.00055
F1 4 0.008394 0.353820 0.359533 11.00000 0.04287 0.03812 =
0.04250 -0.00456 -0.01195 0.01300
F2 4 -0.046292 0.206022 0.279296 11.00000 0.02993 0.06276 =
0.02947 -0.00689 -0.01006 -0.00963
F3 4 0.095565 0.292338 0.290466 11.00000 0.04561 0.04875 =
0.02981 0.01492 0.00062 -0.01202
F4 4 0.017233 -0.031749 0.333015 11.00000 0.05225 0.04226 =
0.06314 -0.02881 0.02091 -0.03017
F5 4 0.134413 0.045390 0.296249 11.00000 0.06565 0.05019 =
0.03633 -0.01306 0.03301 -0.00551
F6 4 0.170146 -0.035874 0.405412 11.00000 0.06423 0.02228 =
0.04485 -0.00430 0.01119 0.00183
F7 4 0.115862 -0.037925 0.540158 11.00000 0.02565 0.03210 =
0.05738 -0.00496 0.00669 -0.00830
F8 4 0.181421 -0.140421 0.642844 11.00000 0.06115 0.03430 =
0.08189 0.02563 0.03629 -0.00818
F9 4 0.265878 -0.111805 0.566070 11.00000 0.03746 0.02646 =
0.05470 -0.00984 0.01787 0.00362
F10 4 0.301037 -0.013014 0.760083 11.00000 0.06818 0.08820 =
0.02904 0.03276 0.02619 0.01564
F11 4 0.403870 -0.021029 0.696184 11.00000 0.03123 0.04709 =
0.03308 0.00639 0.00749 0.01886
F12 4 0.368591 0.155019 0.735638 11.00000 0.04290 0.05361 =
0.02491 -0.01036 -0.00102 0.00862
F13 4 0.359566 0.195877 0.376980 11.00000 0.03342 0.05524 =
0.02333 -0.00960 0.01195 0.00235
F14 4 0.509520 0.124175 0.421456 11.00000 0.04090 0.05537 =
0.05225 -0.00927 0.03076 0.01446
F15 4 0.481705 0.322225 0.421685 11.00000 0.05102 0.04410 =
0.04008 0.00628 0.03117 -0.01187
F16 4 0.596123 0.124687 0.570800 11.00000 0.02262 0.05882 =
0.05383 0.01129 0.01055 0.02396
F17 4 0.570085 0.322102 0.576302 11.00000 0.02238 0.04592 =
0.05077 0.00254 0.00202 -0.01498
F18 4 0.510191 0.195294 0.639387 11.00000 0.02577 0.05733 =
0.02516 0.01290 0.00385 0.00601
O1 3 0.178721 0.205010 0.434292 11.00000 0.01505 0.02055 =
0.01495 -0.00153 0.00263 -0.00227
O2 3 0.271981 0.138772 0.586660 11.00000 0.01602 0.01886 =
0.01825 0.00254 0.01002 -0.00053
O3 3 0.364569 0.290137 0.515039 11.00000 0.01454 0.01586 =
0.01538 0.00024 0.00549 0.00193
O4 3 0.210355 0.454462 0.473423 11.00000 0.01787 0.01589 =
0.01650 0.00149 0.00893 0.00243
O5 3 0.293436 0.402179 0.622143 11.00000 0.01789 0.02118 =
0.01496 -0.00472 0.00894 -0.00666
C1 1 0.036342 0.252686 0.329092 11.00000 0.02729 0.03621 =
0.02383 -0.00353 -0.00298 -0.00385
C2 1 0.087714 0.158030 0.390178 11.00000 0.01846 0.02490 =
0.01704 -0.00516 0.00514 -0.00782
AFIX 13
H2 2 0.044296 0.144049 0.422740 11.00000 -1.20000
AFIX 0
C3 1 0.102953 0.033693 0.355941 11.00000 0.03259 0.02869 =
0.02527 -0.00508 0.00927 -0.01001
C4 1 0.201693 -0.057624 0.596233 11.00000 0.03062 0.02115 =
0.04351 0.00696 0.01795 -0.00143
C5 1 0.241888 0.064565 0.635539 11.00000 0.02150 0.02130 =
0.02242 0.00661 0.01470 0.00445
AFIX 13
H5 2 0.186717 0.108028 0.648787 11.00000 -1.20000
AFIX 0
C6 1 0.330014 0.045726 0.707251 11.00000 0.03790 0.03802 =
0.02219 0.00979 0.01564 0.01245
C7 1 0.446028 0.210209 0.431680 11.00000 0.02476 0.03175 =
0.03146 -0.00450 0.01759 0.00066
C8 1 0.430503 0.197912 0.508632 11.00000 0.01420 0.01573 =
0.02553 0.00256 0.01060 0.00063
AFIX 13
H8 2 0.400039 0.114424 0.511673 11.00000 -1.20000
AFIX 0
C9 1 0.527830 0.209914 0.573905 11.00000 0.01935 0.03069 =
0.03166 0.00599 0.00993 0.00458
C10 1 0.247607 0.483997 0.410101 11.00000 0.02116 0.02078 =
0.01829 0.00603 0.01153 -0.00028
AFIX 23
H10A 2 0.236777 0.412906 0.374522 11.00000 -1.20000
H10B 2 0.320045 0.504382 0.428445 11.00000 -1.20000
AFIX 0
C11 1 0.186449 0.596116 0.372912 11.00000 0.02527 0.02585 =
0.02884 0.01078 0.00918 0.00221
AFIX 23
H11A 2 0.224154 0.649274 0.347877 11.00000 -1.20000
H11B 2 0.122329 0.570331 0.335365 11.00000 -1.20000
AFIX 0
C12 1 0.168823 0.662959 0.438481 11.00000 0.02981 0.01806 =
0.04651 0.00633 0.01844 0.00289
AFIX 23
H12A 2 0.111163 0.720959 0.421247 11.00000 -1.20000
H12B 2 0.229079 0.710321 0.467785 11.00000 -1.20000
AFIX 0
C13 1 0.146951 0.557548 0.484322 11.00000 0.02277 0.01547 =
0.03012 0.00086 0.01327 0.00680
AFIX 23
H13A 2 0.165042 0.580831 0.538235 11.00000 -1.20000
H13B 2 0.075085 0.534296 0.465743 11.00000 -1.20000
AFIX 0
C14 1 0.253137 0.426298 0.684410 11.00000 0.02886 0.02777 =
0.01794 -0.00469 0.01497 -0.00366
AFIX 23
H14A 2 0.249614 0.348035 0.711704 11.00000 -1.20000
H14B 2 0.185126 0.463146 0.665311 11.00000 -1.20000
AFIX 0
C15 1 0.325922 0.517234 0.735359 11.00000 0.03750 0.03727 =
0.02269 -0.01169 0.01234 -0.01210
AFIX 23
H15A 2 0.380907 0.472747 0.773328 11.00000 -1.20000
H15B 2 0.291513 0.572981 0.761594 11.00000 -1.20000
AFIX 0
C16 1 0.365104 0.589926 0.680968 11.00000 0.02707 0.02197 =
0.02468 -0.00533 0.00594 -0.00651
AFIX 23
H16A 2 0.316295 0.653889 0.653447 11.00000 -1.20000
H16B 2 0.429902 0.630870 0.707385 11.00000 -1.20000
AFIX 0
C17 1 0.377612 0.488434 0.628648 11.00000 0.02229 0.02602 =
0.02355 -0.00578 0.01057 -0.01134
AFIX 23
H17A 2 0.373852 0.523353 0.578781 11.00000 -1.20000
H17B 2 0.442781 0.445263 0.650081 11.00000 -1.20000
AFIX 0
HKLF 4
REM 18084 in P2(1)/c
REM R1 = 0.0420 for 3934 Fo > 4sig(Fo) and 0.0551 for all 4968 data
REM 379 parameters refined using 0 restraints
END
WGHT 0.0695 0.8199
REM Instructions for potential hydrogen bonds
HTAB C2 Cl1
HTAB C5 Cl1
HTAB C10 F3
HTAB C10 F17_$1
HTAB C11 F2_$2
HTAB C12 Cl1_$3
HTAB C12 F9_$4
HTAB C13 Cl1_$3
HTAB C14 F12
HTAB C17 F15_$1
HTAB C17 O4
REM Highest difference peak 0.564, deepest hole -0.707, 1-sigma level 0.076
Q1 1 0.1864 0.2611 0.4747 11.00000 0.05 0.56
Q2 1 0.2341 0.3793 0.5248 11.00000 0.05 0.54
Q3 1 0.2543 0.2153 0.5741 11.00000 0.05 0.48
Q4 1 0.0814 0.1997 0.5529 11.00000 0.05 0.48
Q5 1 0.2470 0.2016 0.5572 11.00000 0.05 0.46
Q6 1 0.2573 0.3509 0.5678 11.00000 0.05 0.44
Q7 1 0.2774 0.3126 0.5789 11.00000 0.05 0.40
Q8 1 0.0857 0.3777 0.5436 11.00000 0.05 0.33
Q9 1 0.1553 0.2824 0.4209 11.00000 0.05 0.32
Q10 1 0.0852 0.0904 0.3791 11.00000 0.05 0.32
Q11 1 0.2265 0.0041 0.6171 11.00000 0.05 0.31
Q12 1 0.2631 0.0885 0.6063 11.00000 0.05 0.31
Q13 1 0.2535 0.0966 0.5499 11.00000 0.05 0.31
Q14 1 0.2138 0.6514 0.4088 11.00000 0.05 0.31
Q15 1 0.0904 0.6471 0.3967 11.00000 0.05 0.29
Q16 1 0.1788 -0.1613 0.5983 11.00000 0.05 0.29
Q17 1 0.0375 0.2820 0.5001 11.00000 0.05 0.29
Q18 1 0.4415 0.1923 0.4729 11.00000 0.05 0.29
Q19 1 0.1290 0.2856 0.5964 11.00000 0.05 0.28
Q20 1 0.0655 0.2195 0.2626 11.00000 0.05 0.28
;
_shelx_res_checksum 63581
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ti Ti1 0.23757(3) 0.27877(4) 0.52659(2) 0.01242(14) Uani d 1 . .
Cl Cl1 0.08372(4) 0.29034(6) 0.54994(3) 0.01954(17) Uani d 1 . .
F F1 0.00839(14) 0.35382(17) 0.35953(10) 0.0471(5) Uani d 1 . .
F F2 -0.04629(13) 0.20602(18) 0.27930(10) 0.0453(5) Uani d 1 . .
F F3 0.09556(14) 0.29234(17) 0.29047(10) 0.0440(5) Uani d 1 . .
F F4 0.01723(15) -0.03175(17) 0.33302(11) 0.0519(5) Uani d 1 . .
F F5 0.13441(15) 0.04539(17) 0.29625(10) 0.0468(5) Uani d 1 . .
F F6 0.17015(15) -0.03587(15) 0.40541(10) 0.0452(5) Uani d 1 . .
F F7 0.11586(12) -0.03793(16) 0.54016(10) 0.0399(4) Uani d 1 . .
F F8 0.18142(16) -0.14042(17) 0.64284(12) 0.0559(6) Uani d 1 . .
F F9 0.26588(13) -0.11180(16) 0.56607(10) 0.0388(4) Uani d 1 . .
F F10 0.30104(16) -0.0130(2) 0.76008(10) 0.0593(6) Uani d 1 . .
F F11 0.40387(12) -0.02103(17) 0.69618(9) 0.0378(4) Uani d 1 . .
F F12 0.36859(14) 0.15502(18) 0.73564(9) 0.0432(5) Uani d 1 . .
F F13 0.35957(13) 0.19588(17) 0.37698(9) 0.0366(4) Uani d 1 . .
F F14 0.50952(14) 0.12417(18) 0.42146(10) 0.0458(5) Uani d 1 . .
F F15 0.48170(14) 0.32223(16) 0.42168(10) 0.0411(5) Uani d 1 . .
F F16 0.59612(12) 0.12469(18) 0.57080(10) 0.0455(5) Uani d 1 . .
F F17 0.57008(12) 0.32210(17) 0.57630(10) 0.0419(5) Uani d 1 . .
F F18 0.51019(12) 0.19529(17) 0.63939(9) 0.0371(4) Uani d 1 . .
O O1 0.17872(12) 0.20501(15) 0.43429(9) 0.0173(4) Uani d 1 . .
O O2 0.27198(12) 0.13877(15) 0.58666(9) 0.0166(4) Uani d 1 . .
O O3 0.36457(12) 0.29014(15) 0.51504(9) 0.0151(4) Uani d 1 . .
O O4 0.21035(12) 0.45446(15) 0.47342(9) 0.0159(4) Uani d 1 . .
O O5 0.29344(12) 0.40218(15) 0.62214(9) 0.0171(4) Uani d 1 . .
C C1 0.0363(2) 0.2527(3) 0.32909(16) 0.0317(7) Uani d 1 . .
C C2 0.08771(19) 0.1580(2) 0.39018(14) 0.0202(6) Uani d 1 . .
H H2 0.044296 0.144049 0.422740 0.024 Uiso calc 1 . .
C C3 0.1030(2) 0.0337(3) 0.35594(15) 0.0288(6) Uani d 1 . .
C C4 0.2017(2) -0.0576(3) 0.59623(17) 0.0303(7) Uani d 1 . .
C C5 0.24189(19) 0.0646(2) 0.63554(14) 0.0199(5) Uani d 1 . .
H H5 0.186717 0.108028 0.648787 0.024 Uiso calc 1 . .
C C6 0.3300(2) 0.0457(3) 0.70725(15) 0.0313(7) Uani d 1 . .
C C7 0.4460(2) 0.2102(3) 0.43168(16) 0.0273(6) Uani d 1 . .
C C8 0.43050(18) 0.1979(2) 0.50863(14) 0.0175(5) Uani d 1 . .
H H8 0.400039 0.114424 0.511673 0.021 Uiso calc 1 . .
C C9 0.5278(2) 0.2099(3) 0.57390(16) 0.0268(6) Uani d 1 . .
C C10 0.24761(19) 0.4840(2) 0.41010(13) 0.0188(5) Uani d 1 . .
H H10A 0.236777 0.412906 0.374522 0.023 Uiso calc 1 . .
H H10B 0.320045 0.504382 0.428445 0.023 Uiso calc 1 . .
C C11 0.1864(2) 0.5961(3) 0.37291(15) 0.0265(6) Uani d 1 . .
H H11A 0.224154 0.649274 0.347877 0.032 Uiso calc 1 . .
H H11B 0.122329 0.570331 0.335365 0.032 Uiso calc 1 . .
C C12 0.1688(2) 0.6630(2) 0.43848(17) 0.0300(7) Uani d 1 . .
H H12A 0.111163 0.720959 0.421247 0.036 Uiso calc 1 . .
H H12B 0.229079 0.710321 0.467785 0.036 Uiso calc 1 . .
C C13 0.14695(19) 0.5575(2) 0.48432(15) 0.0216(6) Uani d 1 . .
H H13A 0.165042 0.580831 0.538235 0.026 Uiso calc 1 . .
H H13B 0.075085 0.534296 0.465743 0.026 Uiso calc 1 . .
C C14 0.2531(2) 0.4263(2) 0.68441(14) 0.0231(6) Uani d 1 . .
H H14A 0.249614 0.348035 0.711704 0.028 Uiso calc 1 . .
H H14B 0.185126 0.463146 0.665311 0.028 Uiso calc 1 . .
C C15 0.3259(2) 0.5172(3) 0.73536(15) 0.0318(7) Uani d 1 . .
H H15A 0.380907 0.472747 0.773328 0.038 Uiso calc 1 . .
H H15B 0.291513 0.572981 0.761594 0.038 Uiso calc 1 . .
C C16 0.3651(2) 0.5899(2) 0.68097(15) 0.0251(6) Uani d 1 . .
H H16A 0.316295 0.653889 0.653447 0.030 Uiso calc 1 . .
H H16B 0.429902 0.630870 0.707385 0.030 Uiso calc 1 . .
C C17 0.3776(2) 0.4884(2) 0.62865(15) 0.0232(6) Uani d 1 . .
H H17A 0.373852 0.523353 0.578781 0.028 Uiso calc 1 . .
H H17B 0.442781 0.445263 0.650081 0.028 Uiso calc 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
Ti1 0.0111(2) 0.0140(2) 0.0132(2) -0.00076(17) 0.00517(17) -0.00024(16)
Cl1 0.0143(3) 0.0214(3) 0.0259(3) 0.0006(2) 0.0107(2) 0.0000(2)
F1 0.0429(11) 0.0381(11) 0.0425(11) 0.0130(9) -0.0119(8) -0.0046(8)
F2 0.0299(10) 0.0628(13) 0.0295(10) -0.0096(9) -0.0101(8) -0.0069(8)
F3 0.0456(11) 0.0488(11) 0.0298(10) -0.0120(9) 0.0006(8) 0.0149(8)
F4 0.0522(12) 0.0423(11) 0.0631(13) -0.0302(9) 0.0209(10) -0.0288(10)
F5 0.0657(13) 0.0502(11) 0.0363(10) -0.0055(10) 0.0330(10) -0.0131(8)
F6 0.0642(13) 0.0223(9) 0.0449(11) 0.0018(9) 0.0112(10) -0.0043(8)
F7 0.0256(9) 0.0321(9) 0.0574(12) -0.0083(7) 0.0067(8) -0.0050(8)
F8 0.0612(14) 0.0343(11) 0.0819(15) -0.0082(9) 0.0363(12) 0.0256(10)
F9 0.0375(10) 0.0265(9) 0.0547(11) 0.0036(8) 0.0179(9) -0.0098(8)
F10 0.0682(14) 0.0882(16) 0.0290(10) 0.0156(12) 0.0262(10) 0.0328(10)
F11 0.0312(9) 0.0471(10) 0.0331(9) 0.0189(8) 0.0075(7) 0.0064(8)
F12 0.0429(11) 0.0536(12) 0.0249(9) 0.0086(9) -0.0010(8) -0.0104(8)
F13 0.0334(10) 0.0552(11) 0.0233(9) 0.0023(8) 0.0119(7) -0.0096(7)
F14 0.0409(11) 0.0554(12) 0.0523(11) 0.0145(9) 0.0308(9) -0.0093(9)
F15 0.0510(11) 0.0441(10) 0.0401(10) -0.0119(9) 0.0312(9) 0.0063(8)
F16 0.0226(9) 0.0588(12) 0.0538(11) 0.0240(9) 0.0105(8) 0.0113(9)
F17 0.0224(9) 0.0459(11) 0.0508(11) -0.0150(8) 0.0020(8) 0.0025(8)
F18 0.0258(9) 0.0573(11) 0.0252(9) 0.0060(8) 0.0038(7) 0.0129(8)
O1 0.0151(9) 0.0205(9) 0.0149(9) -0.0023(7) 0.0026(7) -0.0015(7)
O2 0.0160(9) 0.0189(9) 0.0182(9) -0.0005(7) 0.0100(7) 0.0025(7)
O3 0.0145(9) 0.0159(9) 0.0154(9) 0.0019(7) 0.0055(7) 0.0002(6)
O4 0.0179(9) 0.0159(9) 0.0165(9) 0.0024(7) 0.0089(7) 0.0015(7)
O5 0.0179(9) 0.0212(9) 0.0150(8) -0.0067(7) 0.0089(7) -0.0047(7)
C1 0.0273(16) 0.0362(16) 0.0238(15) -0.0039(13) -0.0030(12) -0.0035(13)
C2 0.0185(13) 0.0249(14) 0.0170(13) -0.0078(11) 0.0051(10) -0.0052(10)
C3 0.0326(16) 0.0287(15) 0.0253(15) -0.0100(13) 0.0093(12) -0.0051(12)
C4 0.0306(16) 0.0211(14) 0.0435(17) -0.0014(12) 0.0180(14) 0.0070(12)
C5 0.0215(13) 0.0213(13) 0.0224(13) 0.0044(11) 0.0147(11) 0.0066(10)
C6 0.0379(17) 0.0380(17) 0.0222(14) 0.0124(14) 0.0156(13) 0.0098(13)
C7 0.0248(15) 0.0317(16) 0.0315(16) 0.0007(12) 0.0176(13) -0.0045(12)
C8 0.0142(12) 0.0157(12) 0.0255(14) 0.0006(10) 0.0106(10) 0.0026(10)
C9 0.0193(14) 0.0307(16) 0.0317(16) 0.0046(12) 0.0099(12) 0.0060(12)
C10 0.0212(13) 0.0208(13) 0.0183(13) -0.0003(11) 0.0115(10) 0.0060(10)
C11 0.0253(15) 0.0259(14) 0.0288(15) 0.0022(12) 0.0092(12) 0.0108(11)
C12 0.0298(16) 0.0181(14) 0.0465(18) 0.0029(12) 0.0184(14) 0.0063(12)
C13 0.0228(14) 0.0155(13) 0.0301(14) 0.0068(11) 0.0133(11) 0.0009(10)
C14 0.0289(15) 0.0278(14) 0.0179(13) -0.0037(12) 0.0150(11) -0.0047(11)
C15 0.0375(17) 0.0373(17) 0.0227(14) -0.0121(14) 0.0123(13) -0.0117(12)
C16 0.0271(15) 0.0220(14) 0.0247(14) -0.0065(12) 0.0059(11) -0.0053(11)
C17 0.0223(14) 0.0260(14) 0.0235(14) -0.0113(11) 0.0106(11) -0.0058(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
O1 Ti1 O2 . . 100.14(8) y
O1 Ti1 O3 . . 94.69(7) y
O2 Ti1 O3 . . 92.72(7) y
O1 Ti1 O4 . . 88.84(7) y
O2 Ti1 O4 . . 170.98(7) y
O3 Ti1 O4 . . 85.68(7) y
O1 Ti1 O5 . . 167.56(7) y
O2 Ti1 O5 . . 92.10(7) y
O3 Ti1 O5 . . 86.87(7) y
O4 Ti1 O5 . . 78.95(6) y
O1 Ti1 Cl1 . . 91.72(6) y
O2 Ti1 Cl1 . . 90.52(5) y
O3 Ti1 Cl1 . . 172.19(6) y
O4 Ti1 Cl1 . . 90.02(5) y
O5 Ti1 Cl1 . . 85.92(5) y
C2 O1 Ti1 . . 140.75(15) y
C5 O2 Ti1 . . 142.97(15) y
C8 O3 Ti1 . . 130.80(15) y
C13 O4 C10 . . 109.58(17) ?
C13 O4 Ti1 . . 129.17(14) y
C10 O4 Ti1 . . 120.92(13) y
C14 O5 C17 . . 108.95(17) ?
C14 O5 Ti1 . . 129.22(14) y
C17 O5 Ti1 . . 121.54(13) y
F3 C1 F2 . . 107.2(2) ?
F3 C1 F1 . . 106.9(2) ?
F2 C1 F1 . . 107.0(2) ?
F3 C1 C2 . . 112.9(2) ?
F2 C1 C2 . . 112.0(2) ?
F1 C1 C2 . . 110.6(2) ?
O1 C2 C3 . . 110.1(2) ?
O1 C2 C1 . . 109.6(2) ?
C3 C2 C1 . . 111.2(2) ?
O1 C2 H2 . . 108.6 ?
C3 C2 H2 . . 108.6 ?
C1 C2 H2 . . 108.6 ?
F6 C3 F5 . . 106.6(2) ?
F6 C3 F4 . . 107.4(2) ?
F5 C3 F4 . . 106.5(2) ?
F6 C3 C2 . . 111.3(2) ?
F5 C3 C2 . . 113.5(2) ?
F4 C3 C2 . . 111.1(2) ?
F9 C4 F8 . . 107.4(2) ?
F9 C4 F7 . . 107.4(2) ?
F8 C4 F7 . . 106.8(2) ?
F9 C4 C5 . . 112.3(2) ?
F8 C4 C5 . . 112.3(2) ?
F7 C4 C5 . . 110.3(2) ?
O2 C5 C4 . . 108.8(2) ?
O2 C5 C6 . . 109.0(2) ?
C4 C5 C6 . . 112.7(2) ?
O2 C5 H5 . . 108.8 ?
C4 C5 H5 . . 108.8 ?
C6 C5 H5 . . 108.8 ?
F12 C6 F11 . . 107.2(2) ?
F12 C6 F10 . . 107.5(2) ?
F11 C6 F10 . . 107.3(2) ?
F12 C6 C5 . . 110.5(2) ?
F11 C6 C5 . . 113.0(2) ?
F10 C6 C5 . . 111.1(2) ?
F13 C7 F15 . . 106.8(2) ?
F13 C7 F14 . . 107.5(2) ?
F15 C7 F14 . . 107.5(2) ?
F13 C7 C8 . . 110.3(2) ?
F15 C7 C8 . . 112.4(2) ?
F14 C7 C8 . . 112.1(2) ?
O3 C8 C9 . . 109.0(2) ?
O3 C8 C7 . . 108.6(2) ?
C9 C8 C7 . . 112.8(2) ?
O3 C8 H8 . . 108.8 ?
C9 C8 H8 . . 108.8 ?
C7 C8 H8 . . 108.8 ?
F18 C9 F17 . . 106.6(2) ?
F18 C9 F16 . . 107.7(2) ?
F17 C9 F16 . . 107.3(2) ?
F18 C9 C8 . . 110.2(2) ?
F17 C9 C8 . . 112.3(2) ?
F16 C9 C8 . . 112.5(2) ?
O4 C10 C11 . . 104.20(19) ?
O4 C10 H10A . . 110.9 ?
C11 C10 H10A . . 110.9 ?
O4 C10 H10B . . 110.9 ?
C11 C10 H10B . . 110.9 ?
H10A C10 H10B . . 108.9 ?
C12 C11 C10 . . 102.6(2) ?
C12 C11 H11A . . 111.2 ?
C10 C11 H11A . . 111.2 ?
C12 C11 H11B . . 111.2 ?
C10 C11 H11B . . 111.2 ?
H11A C11 H11B . . 109.2 ?
C11 C12 C13 . . 102.9(2) ?
C11 C12 H12A . . 111.2 ?
C13 C12 H12A . . 111.2 ?
C11 C12 H12B . . 111.2 ?
C13 C12 H12B . . 111.2 ?
H12A C12 H12B . . 109.1 ?
O4 C13 C12 . . 104.0(2) ?
O4 C13 H13A . . 111.0 ?
C12 C13 H13A . . 111.0 ?
O4 C13 H13B . . 111.0 ?
C12 C13 H13B . . 111.0 ?
H13A C13 H13B . . 109.0 ?
O5 C14 C15 . . 105.0(2) ?
O5 C14 H14A . . 110.7 ?
C15 C14 H14A . . 110.7 ?
O5 C14 H14B . . 110.7 ?
C15 C14 H14B . . 110.7 ?
H14A C14 H14B . . 108.8 ?
C14 C15 C16 . . 103.0(2) ?
C14 C15 H15A . . 111.2 ?
C16 C15 H15A . . 111.2 ?
C14 C15 H15B . . 111.2 ?
C16 C15 H15B . . 111.2 ?
H15A C15 H15B . . 109.1 ?
C17 C16 C15 . . 101.9(2) ?
C17 C16 H16A . . 111.4 ?
C15 C16 H16A . . 111.4 ?
C17 C16 H16B . . 111.4 ?
C15 C16 H16B . . 111.4 ?
H16A C16 H16B . . 109.2 ?
O5 C17 C16 . . 104.4(2) ?
O5 C17 H17A . . 110.9 ?
C16 C17 H17A . . 110.9 ?
O5 C17 H17B . . 110.9 ?
C16 C17 H17B . . 110.9 ?
H17A C17 H17B . . 108.9 ?
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
Ti1 O1 . 1.8386(17) y
Ti1 O2 . 1.8426(17) y
Ti1 O3 . 1.8679(17) y
Ti1 O4 . 2.1043(17) y
Ti1 O5 . 2.1593(17) y
Ti1 Cl1 . 2.3399(9) y
F1 C1 . 1.338(3) ?
F2 C1 . 1.334(3) ?
F3 C1 . 1.332(4) ?
F4 C3 . 1.341(3) ?
F5 C3 . 1.330(3) ?
F6 C3 . 1.322(3) ?
F7 C4 . 1.341(3) ?
F8 C4 . 1.335(3) ?
F9 C4 . 1.338(3) ?
F10 C6 . 1.338(3) ?
F11 C6 . 1.329(3) ?
F12 C6 . 1.327(4) ?
F13 C7 . 1.326(3) ?
F14 C7 . 1.337(3) ?
F15 C7 . 1.335(3) ?
F16 C9 . 1.338(3) ?
F17 C9 . 1.334(3) ?
F18 C9 . 1.333(3) ?
O1 C2 . 1.379(3) ?
O2 C5 . 1.374(3) ?
O3 C8 . 1.384(3) ?
O4 C13 . 1.472(3) ?
O4 C10 . 1.472(3) ?
O5 C14 . 1.469(3) ?
O5 C17 . 1.475(3) ?
C1 C2 . 1.526(4) ?
C2 C3 . 1.521(4) ?
C2 H2 . 1.0000 ?
C4 C5 . 1.518(4) ?
C5 C6 . 1.523(4) ?
C5 H5 . 1.0000 ?
C7 C8 . 1.527(4) ?
C8 C9 . 1.523(4) ?
C8 H8 . 1.0000 ?
C10 C11 . 1.511(4) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.506(4) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.506(4) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.511(4) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 C16 . 1.515(4) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 C17 . 1.509(4) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
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
_geom_hbond_publ_flag
C2 H2 Cl1 . 1.00 2.75 3.321(3) 116.5 yes
C5 H5 Cl1 . 1.00 2.76 3.329(3) 116.5 yes
C10 H10A F3 . 0.99 2.47 3.278(3) 138.7 yes
C10 H10B F17 3_666 0.99 2.43 3.243(3) 138.6 yes
C11 H11B F2 2 0.99 2.53 3.132(3) 119.1 yes
C12 H12A Cl1 3_566 0.99 2.96 3.657(3) 128.7 yes
C12 H12B F9 1_565 0.99 2.58 3.361(3) 135.6 yes
C13 H13B Cl1 3_566 0.99 2.86 3.500(3) 123.2 yes
C14 H14A F12 . 0.99 2.61 3.315(3) 128.7 yes
C17 H17A F15 3_666 0.99 2.62 3.174(3) 115.5 yes
C17 H17A O4 . 0.99 2.61 3.124(3) 112.0 yes
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
O2 Ti1 O1 C2 . . . . 85.1(2) ?
O3 Ti1 O1 C2 . . . . 178.7(2) ?
O4 Ti1 O1 C2 . . . . -95.8(2) ?
O5 Ti1 O1 C2 . . . . -84.6(4) ?
Cl1 Ti1 O1 C2 . . . . -5.8(2) ?
O1 Ti1 O2 C5 . . . . -99.1(3) ?
O3 Ti1 O2 C5 . . . . 165.7(3) ?
O5 Ti1 O2 C5 . . . . 78.7(3) ?
Cl1 Ti1 O2 C5 . . . . -7.2(3) ?
O1 Ti1 O3 C8 . . . . -64.4(2) ?
O2 Ti1 O3 C8 . . . . 36.0(2) ?
O4 Ti1 O3 C8 . . . . -152.9(2) ?
O5 Ti1 O3 C8 . . . . 128.0(2) ?
Ti1 O1 C2 C3 . . . . -135.4(2) ?
Ti1 O1 C2 C1 . . . . 102.0(3) ?
F3 C1 C2 O1 . . . . 51.3(3) ?
F2 C1 C2 O1 . . . . 172.5(2) ?
F1 C1 C2 O1 . . . . -68.3(3) ?
F3 C1 C2 C3 . . . . -70.6(3) ?
F2 C1 C2 C3 . . . . 50.5(3) ?
F1 C1 C2 C3 . . . . 169.7(2) ?
O1 C2 C3 F6 . . . . 41.1(3) ?
C1 C2 C3 F6 . . . . 162.8(2) ?
O1 C2 C3 F5 . . . . -79.2(3) ?
C1 C2 C3 F5 . . . . 42.4(3) ?
O1 C2 C3 F4 . . . . 160.8(2) ?
C1 C2 C3 F4 . . . . -77.6(3) ?
Ti1 O2 C5 C4 . . . . 106.6(3) ?
Ti1 O2 C5 C6 . . . . -130.1(2) ?
F9 C4 C5 O2 . . . . 51.7(3) ?
F8 C4 C5 O2 . . . . 172.9(2) ?
F7 C4 C5 O2 . . . . -68.0(3) ?
F9 C4 C5 C6 . . . . -69.3(3) ?
F8 C4 C5 C6 . . . . 51.9(3) ?
F7 C4 C5 C6 . . . . 171.0(2) ?
O2 C5 C6 F12 . . . . 53.2(3) ?
C4 C5 C6 F12 . . . . 174.1(2) ?
O2 C5 C6 F11 . . . . -67.0(3) ?
C4 C5 C6 F11 . . . . 53.9(3) ?
O2 C5 C6 F10 . . . . 172.4(2) ?
C4 C5 C6 F10 . . . . -66.8(3) ?
Ti1 O3 C8 C9 . . . . -119.1(2) ?
Ti1 O3 C8 C7 . . . . 117.6(2) ?
F13 C7 C8 O3 . . . . -60.6(3) ?
F15 C7 C8 O3 . . . . 58.5(3) ?
F14 C7 C8 O3 . . . . 179.7(2) ?
F13 C7 C8 C9 . . . . 178.4(2) ?
F15 C7 C8 C9 . . . . -62.5(3) ?
F14 C7 C8 C9 . . . . 58.7(3) ?
O3 C8 C9 F18 . . . . 60.8(3) ?
C7 C8 C9 F18 . . . . -178.4(2) ?
O3 C8 C9 F17 . . . . -57.8(3) ?
C7 C8 C9 F17 . . . . 62.9(3) ?
O3 C8 C9 F16 . . . . -179.0(2) ?
C7 C8 C9 F16 . . . . -58.2(3) ?
C13 O4 C10 C11 . . . . -11.7(3) ?
Ti1 O4 C10 C11 . . . . 162.37(15) ?
O4 C10 C11 C12 . . . . 32.5(3) ?
C10 C11 C12 C13 . . . . -41.1(3) ?
C10 O4 C13 C12 . . . . -13.9(3) ?
Ti1 O4 C13 C12 . . . . 172.74(16) ?
C11 C12 C13 O4 . . . . 33.9(3) ?
C17 O5 C14 C15 . . . . -8.2(3) ?
Ti1 O5 C14 C15 . . . . 177.99(17) ?
O5 C14 C15 C16 . . . . 30.3(3) ?
C14 C15 C16 C17 . . . . -40.6(3) ?
C14 O5 C17 C16 . . . . -17.4(3) ?
Ti1 O5 C17 C16 . . . . 157.00(16) ?
C15 C16 C17 O5 . . . . 35.7(3) ?