#------------------------------------------------------------------------------
#$Date: 2023-07-01 03:50:37 +0200 (Sat, 01 Jul 2023) $
#$Revision: 284742 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022806.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_2022806
loop_
_publ_author_name
Vinaya,
'Richard, Austin S.'
'Murthy, Subbiah M.'
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
The synthesis, crystal structure and spectroscopic analysis of
(E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one
;
_journal_coeditor_code VM2285
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 674
_journal_page_last 677
_journal_paper_doi 10.1107/S2056989023005613
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C17 H13 Cl O3'
_chemical_formula_moiety 'C17 H13 Cl O3'
_chemical_formula_sum 'C17 H13 Cl O3'
_chemical_formula_weight 300.72
_chemical_name_systematic
(E)-3-(4-Chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_Hall 'P 2c -2n'
_space_group_name_H-M_alt 'P n a 21'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.8655(5)
_cell_length_b 14.3499(17)
_cell_length_c 16.4803(19)
_cell_measurement_reflns_used 9943
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 27.57
_cell_measurement_theta_min 2.47
_cell_volume 1387.1(3)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 200(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0375
_diffrn_reflns_av_unetI/netI 0.0265
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 17057
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.572
_diffrn_reflns_theta_min 2.472
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.282
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.788
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.440
_exptl_crystal_description 'cut block'
_exptl_crystal_F_000 624
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.230
_exptl_crystal_size_min 0.220
_refine_diff_density_max 0.214
_refine_diff_density_min -0.158
_refine_ls_abs_structure_details
;
Flack x determined using 1035 quotients [(I+)-(I-)]/[(I+)+(I-)]
[Parsons et al. (2013)
;
_refine_ls_abs_structure_Flack 0.01(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 190
_refine_ls_number_reflns 2896
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.065
_refine_ls_R_factor_all 0.0371
_refine_ls_R_factor_gt 0.0334
_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^)+(0.0322P)^2^+0.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0806
_refine_ls_wR_factor_ref 0.0827
_reflns_number_gt 2694
_reflns_number_total 2896
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2285sup1.cif
_cod_data_source_block I
_cod_database_code 2022806
_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 0.930
_shelx_estimated_absorpt_t_max 0.940
_shelx_hkl_file
;
1 0 0 0.57923 0.37981 2
1 0 0 1.38711 0.49641 4
1 0 0 0.61190 0.47702 5
-1 0 0 1.35458 0.58412 4
-1 0 0 0.15828 0.46680 5
-1 0 0 0.96563 0.41680 2
-2 0 0 927.860 34.1804 4
-2 0 0 876.875 34.1831 5
2 0 0 907.463 34.1297 4
2 0 0 887.307 34.2624 5
2 0 0 896.177 33.9166 2
3 0 0 -0.1606 0.89975 4
-3 0 0 1.42933 1.15907 4
-3 0 0 0.73019 1.09070 5
3 0 0 -0.6097 1.07783 5
3 0 0 0.68379 0.93136 2
4 0 0 94.2226 5.92927 5
4 0 0 99.1396 5.46071 4
-4 0 0 99.9583 5.63302 4
4 0 0 96.5769 5.24945 2
5 0 0 1.64574 1.90729 5
-5 0 0 1.21062 2.16025 4
5 0 0 -2.4627 2.55848 2
5 0 0 2.61776 1.85709 4
6 0 0 399.236 20.6874 5
6 0 0 422.468 18.3029 4
6 0 0 437.105 18.3847 2
7 0 0 -1.5539 2.60987 4
7 0 0 -0.1463 2.36984 2
7 0 0 -0.5227 1.36939 3
1 -1 0 17.9858 1.37353 2
1 -1 0 15.7444 1.14372 4
-1 1 0 14.9116 1.18667 4
1 -1 0 16.5876 0.90636 3
1 1 0 17.7102 1.43555 5
-1 1 0 16.8544 1.27378 2
-1 -1 0 16.7496 1.43709 5
1 1 0 16.0875 1.27173 4
2 1 0 2501.38 96.8601 2
2 -1 0 2439.69 97.1485 4
-2 1 0 2722.42 97.3044 4
2 1 0 2714.72 97.6075 5
-2 -1 0 2715.23 97.3720 4
2 -1 0 2575.41 97.2545 5
2 1 0 2531.68 97.3016 4
-2 -1 0 2631.32 97.5285 5
2 -1 0 2656.02 97.2639 2
-2 1 0 2617.37 97.1846 2
3 -1 0 74.0947 4.12015 4
3 1 0 68.4179 4.11582 4
3 -1 0 77.4559 4.41340 5
-3 -1 0 77.1902 4.33744 4
-3 1 0 72.5888 4.02469 2
-3 1 0 85.3311 4.39619 4
3 -1 0 80.6328 4.25628 2
3 1 0 75.8590 3.84743 2
3 1 0 73.2633 4.57781 5
-3 -1 0 71.9896 4.55640 5
-4 -1 0 27.2388 3.45821 5
-4 1 0 25.3127 3.11326 4
4 -1 0 22.8869 2.99750 2
4 -1 0 25.0706 3.12623 5
4 1 0 26.7370 2.87153 4
4 1 0 25.4691 3.37298 5
-4 -1 0 28.4467 3.16002 4
4 -1 0 28.5714 2.83045 4
4 1 0 27.3155 2.66456 2
5 1 0 -0.7456 1.95880 4
-5 1 0 4.61346 2.28677 4
5 1 0 1.94735 1.59966 2
5 -1 0 5.82072 2.00115 4
5 -1 0 0.52818 2.13037 5
5 -1 0 0.31254 1.80405 2
5 1 0 -1.5148 1.84915 5
6 1 0 37.4898 4.62168 4
6 1 0 28.0448 3.85466 2
7 1 0 21.3375 4.46641 4
7 1 0 28.2982 3.99857 2
7 -1 0 22.5929 4.18445 4
7 -1 0 31.1837 4.68454 2
0 -2 0 184.354 7.56207 3
0 2 0 189.665 7.57723 3
0 -2 0 205.634 7.71163 2
0 -2 0 180.528 7.57236 5
0 2 0 206.572 7.70273 2
1 -2 0 4047.02 155.342 1
-1 -2 0 3803.72 154.202 1
1 2 0 4172.97 152.302 1
-2 -2 0 243.127 10.0967 5
2 -2 0 232.941 9.50394 5
2 -2 0 241.555 9.83982 2
-2 2 0 238.452 9.73189 2
-2 2 0 226.848 9.61450 4
2 -2 0 219.225 9.06614 3
2 2 0 241.962 10.0644 5
2 -2 0 225.880 9.56844 4
2 2 0 227.400 9.76470 4
-3 2 0 437.721 17.0550 4
3 -2 0 434.777 17.1714 2
3 -2 0 425.488 16.9899 5
-3 2 0 404.060 17.2031 2
3 2 0 417.465 17.5023 5
3 -2 0 421.025 16.8769 4
-3 -2 0 423.262 17.5085 5
3 -2 0 396.451 15.9809 3
3 2 0 420.411 16.3439 2
3 2 0 416.898 17.1082 4
4 2 0 65.9047 3.83058 2
4 2 0 62.2195 4.32888 4
4 2 0 62.7598 4.92598 5
4 -2 0 72.3535 4.71361 5
-4 -2 0 70.8849 5.17083 5
-4 2 0 71.1231 4.61857 4
4 -2 0 67.4055 3.29584 3
-4 2 0 65.2885 4.22215 2
4 -2 0 64.5578 4.22434 4
5 2 0 97.2825 5.53830 2
5 -2 0 108.178 6.79593 5
5 -2 0 105.164 6.60068 2
5 2 0 92.5148 7.05686 5
5 2 0 99.6139 6.34928 4
5 -2 0 100.973 4.85977 3
-5 -2 0 98.4423 7.19202 5
-5 2 0 102.923 6.47548 4
5 -2 0 101.498 6.07733 4
6 -2 0 4.72717 1.88174 3
6 -2 0 8.06474 2.65739 4
6 -2 0 -1.3611 2.51274 2
6 -2 0 4.53200 2.84362 5
6 2 0 6.39734 2.91232 4
6 2 0 4.84648 2.22466 2
-6 2 0 -0.8560 2.52827 4
7 2 0 10.6888 3.47889 4
7 -2 0 3.95957 2.96422 4
7 -2 0 -0.3316 2.77078 2
7 -2 0 5.80531 2.23126 3
0 3 0 1.14274 0.77959 2
0 -3 0 -0.0552 0.67673 5
0 -3 0 -0.3836 0.71696 2
0 -3 0 -1.3582 0.65612 3
0 3 0 -0.7355 0.70159 3
-1 3 0 2077.93 79.0877 3
1 -3 0 2095.94 79.1969 3
-1 3 0 2158.51 79.5110 2
-1 -3 0 2113.96 79.0761 2
1 -3 0 2147.41 79.5549 2
-1 3 0 1978.62 79.2948 4
1 3 0 2182.82 79.0982 2
-1 -3 0 2232.91 79.6584 5
1 3 0 2147.72 79.5727 5
2 -3 0 530.952 21.1826 3
2 3 0 604.510 22.2063 5
-2 3 0 512.421 20.7043 3
-2 -3 0 596.857 22.1931 5
-2 3 0 554.308 21.6044 4
2 -3 0 572.716 21.9158 2
2 -3 0 533.004 21.4940 4
2 3 0 537.104 21.7837 4
-2 3 0 527.778 20.7313 3
-2 3 0 567.370 21.7997 2
-3 -3 0 632.728 24.4279 5
3 -3 0 596.317 23.3475 5
-3 3 0 572.671 23.5062 4
3 -3 0 571.996 22.7950 3
3 -3 0 579.641 23.4046 4
3 3 0 608.002 24.1778 5
-3 3 0 594.487 23.6367 2
3 -3 0 605.723 23.8631 2
4 -3 0 41.9756 3.99649 2
4 3 0 42.9880 4.08942 5
-4 -3 0 48.9906 4.46171 5
4 3 0 41.8064 2.80462 2
4 -3 0 38.7664 2.80942 3
4 3 0 44.1601 3.64371 4
4 -3 0 40.2646 3.62364 5
-4 3 0 44.6189 3.60025 2
-4 3 0 41.2887 3.67121 4
4 -3 0 41.0570 3.36958 4
5 -3 0 67.8379 5.03567 4
-5 -3 0 69.5969 6.32967 5
5 3 0 69.6306 6.18326 5
5 3 0 65.6365 5.41612 4
5 -3 0 69.2844 4.24980 3
-5 3 0 74.6053 5.48723 4
5 3 0 71.8370 4.33565 2
5 -3 0 61.5088 5.62103 2
5 -3 0 70.2510 5.40094 5
6 -3 0 -5.2420 2.68525 2
6 -3 0 -0.0089 2.48412 4
6 -3 0 0.26263 2.00840 3
6 3 0 -5.0414 3.31851 4
6 3 0 -3.4647 1.85164 2
-6 3 0 -3.1655 2.84580 4
-7 3 0 12.3495 3.81904 4
7 3 0 0.70128 1.87274 2
7 -3 0 5.41949 3.20541 2
7 -3 0 1.33322 2.61765 4
7 -3 0 4.14358 2.44151 3
7 3 0 -1.7592 4.42178 4
1 4 0 9543.23 368.298 1
-1 4 0 9583.88 371.249 1
1 -4 0 9742.69 371.906 1
-1 -4 0 9999.99 369.123 1
2 -4 0 80.5044 4.27816 3
2 4 0 88.2454 4.96510 5
-2 4 0 81.0535 5.25363 2
2 -4 0 81.4384 4.80170 2
2 -4 0 80.1355 4.36618 4
-2 4 0 79.0869 3.84165 3
2 4 0 86.2290 4.02624 2
-2 4 0 78.9454 4.50149 4
-2 -4 0 91.4566 5.07119 5
-3 4 0 3.20620 1.62974 2
3 -4 0 7.09852 3.15511 2
3 -4 0 5.19290 1.89196 4
3 4 0 3.65937 1.78295 4
3 4 0 3.41391 1.11053 2
3 -4 0 7.78414 1.67221 5
-3 4 0 4.92171 1.76399 4
3 -4 0 5.16380 1.58991 3
3 4 0 5.14990 1.89704 5
-3 -4 0 3.34457 1.94991 5
4 -4 0 6.13530 1.74389 5
4 4 0 7.98417 1.48033 2
4 -4 0 8.74318 2.01692 4
-4 -4 0 5.32797 2.47427 5
4 4 0 6.21820 2.39250 5
4 4 0 8.79413 2.32530 4
-4 4 0 7.36670 2.41101 4
4 -4 0 13.7045 2.31009 3
4 -4 0 11.7561 2.81229 2
-4 4 0 9.72849 2.13991 2
-5 4 0 132.716 7.65801 4
5 4 0 132.215 7.89188 4
5 4 0 130.567 12.2209 5
5 -4 0 134.711 7.49553 5
5 4 0 128.924 6.14183 2
5 -4 0 125.483 6.67298 3
5 -4 0 126.633 7.97160 2
-5 -4 0 123.301 8.54279 5
5 -4 0 130.465 7.13600 4
-5 4 0 112.864 7.39995 2
6 4 0 143.345 8.67062 4
6 -4 0 131.691 9.02149 2
-6 4 0 154.512 8.75799 4
-6 -4 0 141.830 9.93752 5
6 4 0 134.502 6.83671 2
6 -4 0 132.293 7.81177 4
6 -4 0 139.876 8.56619 5
6 -4 0 142.452 7.47353 3
-7 4 0 9.52331 3.81297 4
7 -4 0 9.84670 3.10041 3
7 -4 0 5.95758 2.98662 4
7 -4 0 8.33475 4.23609 2
0 -5 0 3.40238 1.32143 5
0 -5 0 4.78382 1.50923 2
0 5 0 1.71948 1.25359 2
0 5 0 2.93559 1.32492 3
1 -5 0 12.6460 2.10074 3
-1 5 0 11.7227 1.99004 2
-1 -5 0 10.0211 1.71333 2
1 5 0 11.4982 1.74223 2
-1 -5 0 15.1397 2.38374 5
-1 5 0 12.8963 2.06271 4
1 5 0 8.29773 1.78089 5
-1 5 0 11.6488 1.84328 3
1 -5 0 11.0149 2.02486 2
1 5 0 8.41868 1.56982 3
-2 -5 0 1632.05 57.6032 5
2 -5 0 1516.39 57.0830 2
-2 5 0 1436.36 55.9703 3
2 5 0 1453.98 56.0014 2
-2 5 0 1437.33 56.7942 2
2 5 0 1495.77 57.0494 5
-2 5 0 1489.02 56.6731 4
2 -5 0 1469.16 56.3821 3
3 -5 0 469.580 19.9433 2
-3 5 0 451.817 17.9751 3
3 -5 0 459.814 19.2765 4
-3 5 0 479.230 19.7336 2
3 -5 0 486.577 19.1424 3
3 5 0 505.377 19.9819 4
3 5 0 465.469 18.5661 2
-3 5 0 483.382 19.5043 4
3 5 0 461.898 20.0667 5
-3 -5 0 495.093 20.3377 5
4 5 0 21.4115 2.17911 2
4 -5 0 22.1301 3.29960 5
-4 5 0 30.0681 3.67782 4
-4 5 0 24.1498 3.41177 2
4 -5 0 25.0916 2.97633 4
4 -5 0 25.5191 3.10215 3
4 5 0 29.0823 4.28696 5
4 -5 0 26.6776 3.92294 2
-4 -5 0 27.7286 4.07089 5
4 5 0 25.3948 3.57082 4
5 5 0 2.32308 1.43238 2
5 5 0 5.87658 1.60040 2
5 5 0 1.38478 2.70661 4
-5 5 0 5.67854 3.21003 4
5 -5 0 6.75415 2.50668 5
5 -5 0 7.46128 2.48166 3
5 -5 0 3.30978 2.16483 4
-5 5 0 -1.9298 2.12341 2
-5 -5 0 3.47448 3.11811 5
5 -5 0 5.15067 2.86949 2
6 -5 0 37.7758 4.59393 3
-6 -5 0 41.7149 6.57845 5
6 -5 0 34.5567 5.66196 2
6 -5 0 43.7262 4.61757 4
-6 5 0 37.1977 5.38320 4
6 -5 0 44.4776 5.15953 5
6 5 0 50.7529 5.62856 4
7 -5 0 11.5296 3.74671 5
-7 5 0 14.7943 4.44270 4
7 -5 0 8.04377 3.83377 2
7 -5 0 20.0921 4.09544 4
7 -5 0 17.0909 3.82399 3
0 -6 0 96.7710 5.47703 2
0 6 0 104.220 5.31757 2
0 -6 0 94.4506 5.16126 5
0 -6 0 97.6560 5.17660 3
1 6 0 1638.16 59.4737 2
-1 -6 0 1606.41 59.9722 5
1 -6 0 1597.59 60.0667 2
-1 6 0 1513.32 59.3788 3
-1 6 0 1511.12 59.6699 4
1 6 0 1574.24 59.8198 5
-1 6 0 1601.57 59.9129 2
1 6 0 1504.19 59.2287 3
-1 -6 0 1656.82 59.6029 2
1 -6 0 1528.87 59.5593 3
2 6 0 319.314 12.8440 2
-2 6 0 306.058 13.5566 2
2 6 0 309.321 12.6105 3
2 6 0 297.154 13.6574 5
-2 6 0 311.635 13.4204 4
-2 6 0 309.979 13.4437 3
2 -6 0 316.751 13.8924 2
-2 -6 0 322.032 14.0038 5
3 -6 0 116.475 7.17827 2
3 6 0 121.786 7.16222 5
3 6 0 120.727 7.01161 4
3 6 0 121.306 5.75928 2
-3 -6 0 124.627 7.41355 5
-3 6 0 119.379 5.47555 3
-3 6 0 120.111 5.43885 3
3 -6 0 124.947 6.52157 3
-3 6 0 122.515 6.91725 2
-4 -6 0 121.236 7.95564 5
4 6 0 123.225 5.81000 2
4 -6 0 115.680 6.64259 4
4 -6 0 128.120 6.80024 3
4 6 0 112.312 7.63788 5
4 -6 0 128.116 7.88903 2
4 6 0 121.459 7.48694 4
4 -6 0 113.982 8.42889 5
-4 6 0 135.121 7.41400 4
-4 6 0 113.391 9.30135 2
5 -6 0 33.9734 5.13097 2
5 6 0 24.9902 2.46259 2
-5 -6 0 27.8516 5.49695 5
-5 6 0 23.1819 4.48896 4
-5 6 0 25.7806 4.51710 2
5 -6 0 25.0126 3.94081 3
5 -6 0 28.7517 3.83437 5
5 6 0 30.5041 4.54784 4
5 -6 0 26.4422 3.63768 4
5 6 0 20.9030 2.51004 2
6 -6 0 9.64994 5.55168 2
-6 6 0 3.36709 3.41757 4
6 -6 0 5.39485 2.97203 3
6 -6 0 -1.0055 2.40121 5
-6 -6 0 7.35710 4.02356 5
6 -6 0 3.51022 3.24867 4
7 -6 0 8.11734 4.11556 2
7 -6 0 2.22374 3.16947 3
-7 -6 0 -5.0801 3.50810 5
-7 6 0 -0.1897 3.69228 4
0 -7 0 2.40092 1.64602 3
0 -7 0 2.05464 1.67735 2
0 7 0 4.33542 1.56513 2
0 -7 0 3.32060 1.60520 5
0 7 0 7.33835 1.84099 3
1 7 0 1888.57 73.9854 5
-1 7 0 1924.22 74.1357 4
1 -7 0 2043.39 74.6772 2
-1 -7 0 1991.02 73.8826 2
1 7 0 1892.02 73.5303 3
1 7 0 2028.96 73.7968 2
-1 -7 0 1961.68 74.4575 5
-1 7 0 1936.47 74.1556 2
1 -7 0 2002.29 73.9998 3
-1 7 0 1860.47 73.6087 3
2 -7 0 19.8416 2.99727 3
2 7 0 15.1857 3.06537 5
-2 -7 0 16.6366 3.33167 5
2 7 0 17.0608 3.82252 3
2 -7 0 20.0047 3.39570 2
-2 7 0 18.0424 2.93963 2
-2 7 0 24.3900 3.82494 4
-2 7 0 16.5418 2.62955 3
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2 -3 20 10.1961 3.98580 2
-2 3 20 7.19909 6.77509 4
-2 3 20 7.75024 3.91776 3
2 -3 20 8.07044 4.04151 3
2 3 20 4.10254 3.06323 4
2 3 20 3.60040 3.69507 3
-2 -3 20 6.24311 4.50982 4
-2 -3 20 7.00079 3.76145 3
0 -4 20 129.347 9.46609 2
0 -4 20 142.676 9.98722 3
0 4 20 144.185 10.0903 4
1 -4 20 32.2200 5.86343 2
1 -4 20 43.3633 6.80902 3
-1 4 20 21.2222 5.04031 3
-1 -4 20 33.2377 5.79402 2
-1 -4 20 31.6472 5.94120 3
1 4 20 29.1748 5.83453 3
1 4 20 21.6707 4.83863 4
2 -4 20 19.2226 5.01588 3
2 -4 20 20.3401 4.98555 2
-2 4 20 20.6409 4.85080 3
-2 -4 20 13.2222 3.84369 2
2 4 20 28.2111 4.85581 4
-2 -4 20 22.8297 8.33024 4
-2 -4 20 16.1446 4.28485 3
2 4 20 21.1952 4.87886 3
0 -5 20 7.37029 3.61977 2
0 5 20 -0.3087 3.78356 3
0 5 20 1.86586 3.75837 4
1 -5 20 11.5633 4.47404 3
-1 5 20 2.82243 4.09969 4
1 -5 20 9.56324 4.05772 2
1 5 20 5.09218 3.99082 3
1 5 20 3.10230 3.64219 4
-1 -5 20 5.54596 3.44500 2
-1 -5 20 11.4491 4.14758 3
0 6 20 101.940 9.10132 4
0 6 20 106.866 8.86125 3
0 -6 20 119.822 8.99653 2
-1 6 20 7.81258 4.37029 3
1 -6 20 18.6845 4.97884 3
-1 6 20 11.9167 5.10886 4
1 -6 20 23.9631 7.95473 2
-1 -6 20 19.0526 4.35981 2
1 6 20 17.6813 4.80103 3
1 6 20 20.2006 4.88216 4
-1 -6 20 37.6690 6.19202 3
0 0 21 5.63134 4.41919 3
0 0 21 2.02342 3.80834 4
1 0 21 30.5773 5.86779 3
-1 0 21 14.8247 4.89832 4
1 0 21 8.54809 3.92218 4
-1 0 21 14.6249 4.57989 3
0 -1 21 112.369 9.30583 3
0 1 21 94.1822 8.44803 4
0 -1 21 91.3079 8.47337 4
0 1 21 117.205 9.22871 3
1 -1 21 146.864 10.2210 3
-1 1 21 117.510 11.7435 3
1 -1 21 129.023 8.95300 4
-1 1 21 127.948 9.93816 4
1 1 21 115.709 8.82397 4
1 1 21 139.686 9.90305 3
-1 -1 21 139.401 10.3061 4
-1 -1 21 122.917 9.42124 3
0 2 21 10.4102 4.18484 3
0 -2 21 10.3263 4.48958 3
0 -2 21 3.56674 3.76527 4
0 2 21 10.0404 4.23507 4
-1 2 21 125.379 9.96962 4
1 -2 21 115.061 9.09146 3
1 2 21 111.335 8.52057 4
-1 -2 21 110.494 9.03165 3
1 2 21 113.152 9.16444 3
-1 -2 21 126.303 9.75436 4
0 3 21 95.4431 8.36330 3
0 3 21 97.4219 8.72405 4
0 -3 21 97.3355 8.51032 3
0 -3 21 85.3432 8.17906 2
1 -3 21 67.4114 7.80670 3
-1 3 21 85.5987 8.87255 3
-1 -3 21 76.6553 8.50741 3
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 68324
_shelx_res_file
;
TITL m22275 : space group Pna2(1)
m22275.res
created by SHELXL-2019/2 at 15:23:04 on 14-Jun-2023
CELL 0.71073 5.8655 14.3499 16.4803 90.000 90.000 90.000
ZERR 4 0.0005 0.0017 0.0019 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 1/2+Z
SYMM 1/2+X, 1/2-Y, Z
SYMM 1/2-X, 1/2+Y, 1/2+Z
SFAC C H CL O
UNIT 68 52 4 12
TEMP -73
SIZE 0.26 0.23 0.22
REM FORM cut block
REM COLR pale yellow
REM Diffraction pattern looked modulated at 90K, but all satellites seemed
REM to have disappeared by about 180K. Data were collected with the crystal
REM at 200K.
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds:
EQIV $1 x-1/2, -y+3/2, z
HTAB C5 O3_$1
EQIV $2 x-1, y, z-1
HTAB C5 Cl1_$2
HTAB
REM Conformation-defining torsional angles:
RTAB tors C3 C2 C1 C10
RTAB tors C3 C2 C1 O1
RTAB tors C2 C1 C10 C11
RTAB tors C1 C10 C11 C12
RTAB tors C10 C11 C12 C17
REM Dihedral between benzene ring planes:
MPLA C2 C3 C4 C7 C8 C9
MPLA C12 > C17
REM Dihedral between benzene ring planes in pi-pi interactions:
EQIV $3 1-x, 1-y, 0.5+z
MPLA C2 C3 C4 C7 C8 C9
MPLA C12_$3 C13_$3 C14_$3 C15_$3 C16_$3 C17_$3
REM Estimate of SU for pi-pi centroid distances:
MPLA 6 C2 C3 C4 C7 C8 C9 C12_$3 C13_$3 C14_$3 C15_$3 C16_$3 C17_$3
REM Deviation from plane in the dihydrodioxin ring:
MPLA 8 C2 C3 C4 O2 O3 C7 C8 C9 C5 C6
REM Deviation from plane of whole molecule
MPLA Cl1 > C17
FMAP 2
PLAN 20
REM EXTI 0.000000 not needed.
WGHT 0.032200 0.466600
FVAR 0.90159
CL1 3 0.860561 0.657101 0.915064 11.00000 0.06625 0.07448 =
0.03235 0.00482 -0.02483 -0.00458
O1 4 -0.009552 0.593701 0.488762 11.00000 0.03239 0.09386 =
0.02520 0.00009 -0.00001 -0.00572
O2 4 0.003011 0.573180 0.189140 11.00000 0.04139 0.05865 =
0.02481 0.00177 -0.00818 -0.01050
O3 4 0.439935 0.641287 0.142560 11.00000 0.04399 0.06340 =
0.02538 0.00587 0.00402 -0.00249
C1 1 0.190299 0.611217 0.472467 11.00000 0.03452 0.04417 =
0.02263 -0.00171 -0.00280 0.00048
C2 1 0.263371 0.618975 0.386460 11.00000 0.02831 0.03398 =
0.02337 0.00058 -0.00104 0.00105
C3 1 0.107989 0.593071 0.326408 11.00000 0.03119 0.03812 =
0.02606 0.00146 -0.00107 -0.00093
AFIX 43
H3 2 -0.038161 0.570520 0.341626 11.00000 -1.20000
AFIX 0
C4 1 0.163735 0.599762 0.245028 11.00000 0.03130 0.03272 =
0.02586 0.00071 -0.00580 -0.00010
C5 1 0.041354 0.614311 0.111066 11.00000 0.05261 0.06116 =
0.02207 0.00414 -0.01008 -0.00251
AFIX 23
H5A 2 0.008461 0.681919 0.113519 11.00000 -1.20000
H5B 2 -0.062554 0.585853 0.070731 11.00000 -1.20000
AFIX 0
C6 1 0.282892 0.599459 0.085568 11.00000 0.05910 0.06175 =
0.02173 -0.00051 -0.00070 0.00474
AFIX 23
H6A 2 0.313824 0.531780 0.081738 11.00000 -1.20000
H6B 2 0.306758 0.627076 0.031178 11.00000 -1.20000
AFIX 0
C7 1 0.377807 0.632998 0.222090 11.00000 0.03255 0.03744 =
0.02594 0.00396 0.00136 0.00317
C8 1 0.531260 0.660096 0.281019 11.00000 0.02883 0.04095 =
0.03304 0.00340 0.00138 -0.00262
AFIX 43
H8 2 0.675979 0.683954 0.265581 11.00000 -1.20000
AFIX 0
C9 1 0.476070 0.652802 0.362429 11.00000 0.03028 0.03803 =
0.03048 -0.00116 -0.00593 -0.00332
AFIX 43
H9 2 0.584046 0.671004 0.402365 11.00000 -1.20000
AFIX 0
C10 1 0.362754 0.623044 0.537201 11.00000 0.03264 0.04890 =
0.02680 -0.00150 -0.00198 -0.00147
AFIX 43
H10 2 0.511960 0.643759 0.523877 11.00000 -1.20000
AFIX 0
C11 1 0.309041 0.604645 0.614360 11.00000 0.02911 0.04027 =
0.02469 -0.00315 -0.00119 -0.00044
AFIX 43
H11 2 0.158246 0.583195 0.624038 11.00000 -1.20000
AFIX 0
C12 1 0.456277 0.613798 0.685699 11.00000 0.03162 0.03300 =
0.02459 -0.00169 0.00053 0.00230
C13 1 0.673771 0.653336 0.682586 11.00000 0.03236 0.03959 =
0.02595 0.00105 -0.00239 -0.00053
AFIX 43
H13 2 0.737075 0.671519 0.631943 11.00000 -1.20000
AFIX 0
C14 1 0.797923 0.666085 0.753983 11.00000 0.03214 0.03871 =
0.03316 0.00098 -0.00691 0.00031
AFIX 43
H14 2 0.945533 0.693264 0.752293 11.00000 -1.20000
AFIX 0
C15 1 0.704734 0.638979 0.826700 11.00000 0.04159 0.03935 =
0.02550 0.00002 -0.01166 0.00598
C16 1 0.492693 0.598161 0.831583 11.00000 0.04304 0.04158 =
0.02560 0.00329 -0.00052 0.00232
AFIX 43
H16 2 0.432553 0.578743 0.882366 11.00000 -1.20000
AFIX 0
C17 1 0.369639 0.586122 0.761024 11.00000 0.03365 0.03621 =
0.02921 0.00133 0.00206 -0.00050
AFIX 43
H17 2 0.222733 0.558409 0.763644 11.00000 -1.20000
AFIX 0
HKLF 4
REM m22275 : space group Pna2(1)
REM wR2 = 0.0827, GooF = S = 1.065, Restrained GooF = 1.065 for all data
REM R1 = 0.0334 for 2694 Fo > 4sig(Fo) and 0.0371 for all 2896 data
REM 190 parameters refined using 1 restraints
END
WGHT 0.0322 0.4666
REM Instructions for potential hydrogen bonds
HTAB C5 O3_$1
HTAB C5 Cl1_$2
REM Highest difference peak 0.214, deepest hole -0.158, 1-sigma level 0.036
Q1 1 0.8755 0.5818 0.9159 11.00000 0.05 0.21
Q2 1 0.8470 0.7368 0.9188 11.00000 0.05 0.20
Q3 1 0.2429 0.6648 0.0844 11.00000 0.05 0.18
Q4 1 0.2636 0.6045 0.4279 11.00000 0.05 0.18
Q5 1 0.1901 0.6611 0.2451 11.00000 0.05 0.16
Q6 1 0.7493 0.6607 0.7168 11.00000 0.05 0.16
Q7 1 0.5077 0.6618 0.8310 11.00000 0.05 0.15
Q8 1 0.1210 0.5579 0.0966 11.00000 0.05 0.15
Q9 1 0.1377 0.5941 0.2865 11.00000 0.05 0.14
Q10 1 0.3675 0.6158 0.3697 11.00000 0.05 0.14
Q11 1 0.6994 0.6418 0.9189 11.00000 0.05 0.14
Q12 1 0.4275 0.6146 0.2739 11.00000 0.05 0.13
Q13 1 0.2748 0.6106 0.5035 11.00000 0.05 0.13
Q14 1 0.0062 0.5219 0.3331 11.00000 0.05 0.13
Q15 1 0.6945 0.6706 0.9185 11.00000 0.05 0.12
Q16 1 0.0150 0.6518 0.4837 11.00000 0.05 0.12
Q17 1 0.1035 0.5609 0.3280 11.00000 0.05 0.12
Q18 1 0.3816 0.6700 0.0787 11.00000 0.05 0.12
Q19 1 0.5704 0.6543 0.1322 11.00000 0.05 0.12
Q20 1 0.7015 0.6888 0.8183 11.00000 0.05 0.12
;
_shelx_res_checksum 23305
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'
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
Cl Cl1 0.86056(16) 0.65710(6) 0.91506(5) 0.0577(3) Uani d 1 . .
O O1 -0.0096(3) 0.59370(18) 0.48876(12) 0.0505(6) Uani d 1 . .
O O2 0.0030(3) 0.57318(14) 0.18914(12) 0.0416(5) Uani d 1 . .
O O3 0.4399(4) 0.64129(16) 0.14256(12) 0.0443(5) Uani d 1 . .
C C1 0.1903(5) 0.6112(2) 0.47247(15) 0.0338(6) Uani d 1 . .
C C2 0.2634(4) 0.61897(18) 0.38646(15) 0.0286(5) Uani d 1 . .
C C3 0.1080(4) 0.59307(18) 0.32641(17) 0.0318(5) Uani d 1 . .
H H3 -0.038161 0.570520 0.341626 0.038 Uiso calc 1 . .
C C4 0.1637(4) 0.59976(17) 0.24503(16) 0.0300(5) Uani d 1 . .
C C5 0.0414(6) 0.6143(2) 0.11107(17) 0.0453(7) Uani d 1 . .
H H5A 0.008461 0.681919 0.113519 0.054 Uiso calc 1 . .
H H5B -0.062554 0.585853 0.070731 0.054 Uiso calc 1 . .
C C6 0.2829(6) 0.5995(2) 0.08557(18) 0.0475(8) Uani d 1 . .
H H6A 0.313824 0.531780 0.081738 0.057 Uiso calc 1 . .
H H6B 0.306758 0.627076 0.031178 0.057 Uiso calc 1 . .
C C7 0.3778(5) 0.63300(19) 0.22209(16) 0.0320(6) Uani d 1 . .
C C8 0.5313(5) 0.66010(18) 0.28102(18) 0.0343(6) Uani d 1 . .
H H8 0.675979 0.683954 0.265581 0.041 Uiso calc 1 . .
C C9 0.4761(5) 0.65280(18) 0.36243(17) 0.0329(6) Uani d 1 . .
H H9 0.584046 0.671004 0.402365 0.040 Uiso calc 1 . .
C C10 0.3628(5) 0.62304(19) 0.53720(16) 0.0361(6) Uani d 1 . .
H H10 0.511960 0.643759 0.523877 0.043 Uiso calc 1 . .
C C11 0.3090(5) 0.60465(18) 0.61436(15) 0.0314(6) Uani d 1 . .
H H11 0.158246 0.583195 0.624038 0.038 Uiso calc 1 . .
C C12 0.4563(4) 0.61380(17) 0.68570(15) 0.0297(5) Uani d 1 . .
C C13 0.6738(4) 0.65334(18) 0.68259(17) 0.0326(5) Uani d 1 . .
H H13 0.737075 0.671519 0.631943 0.039 Uiso calc 1 . .
C C14 0.7979(5) 0.66609(18) 0.75398(18) 0.0347(6) Uani d 1 . .
H H14 0.945533 0.693264 0.752293 0.042 Uiso calc 1 . .
C C15 0.7047(5) 0.63898(18) 0.82670(18) 0.0355(6) Uani d 1 . .
C C16 0.4927(5) 0.59816(19) 0.83158(18) 0.0367(6) Uani d 1 . .
H H16 0.432553 0.578743 0.882366 0.044 Uiso calc 1 . .
C C17 0.3696(5) 0.58612(18) 0.76102(16) 0.0330(6) Uani d 1 . .
H H17 0.222733 0.558409 0.763644 0.040 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
Cl1 0.0663(5) 0.0745(5) 0.0324(4) -0.0046(4) -0.0248(4) 0.0048(4)
O1 0.0324(10) 0.0939(18) 0.0252(10) -0.0057(11) 0.0000(9) 0.0001(10)
O2 0.0414(11) 0.0586(12) 0.0248(9) -0.0105(10) -0.0082(9) 0.0018(9)
O3 0.0440(11) 0.0634(14) 0.0254(10) -0.0025(10) 0.0040(9) 0.0059(9)
C1 0.0345(14) 0.0442(15) 0.0226(13) 0.0005(12) -0.0028(11) -0.0017(12)
C2 0.0283(12) 0.0340(13) 0.0234(12) 0.0011(10) -0.0010(10) 0.0006(10)
C3 0.0312(12) 0.0381(13) 0.0261(13) -0.0009(10) -0.0011(11) 0.0015(11)
C4 0.0313(13) 0.0327(12) 0.0259(12) -0.0001(11) -0.0058(11) 0.0007(10)
C5 0.0526(18) 0.0612(18) 0.0221(13) -0.0025(15) -0.0101(13) 0.0041(13)
C6 0.0591(19) 0.062(2) 0.0217(13) 0.0047(16) -0.0007(14) -0.0005(13)
C7 0.0326(14) 0.0374(13) 0.0259(13) 0.0032(11) 0.0014(11) 0.0040(10)
C8 0.0288(13) 0.0410(14) 0.0330(14) -0.0026(11) 0.0014(12) 0.0034(12)
C9 0.0303(12) 0.0380(14) 0.0305(13) -0.0033(10) -0.0059(11) -0.0012(11)
C10 0.0326(13) 0.0489(16) 0.0268(14) -0.0015(13) -0.0020(11) -0.0015(13)
C11 0.0291(13) 0.0403(14) 0.0247(13) -0.0004(11) -0.0012(10) -0.0031(11)
C12 0.0316(13) 0.0330(13) 0.0246(13) 0.0023(10) 0.0005(11) -0.0017(11)
C13 0.0324(13) 0.0396(13) 0.0259(13) -0.0005(10) -0.0024(11) 0.0010(11)
C14 0.0321(13) 0.0387(14) 0.0332(14) 0.0003(11) -0.0069(12) 0.0010(12)
C15 0.0416(15) 0.0393(13) 0.0255(12) 0.0060(11) -0.0117(12) 0.0000(11)
C16 0.0430(15) 0.0416(14) 0.0256(13) 0.0023(12) -0.0005(12) 0.0033(12)
C17 0.0337(13) 0.0362(13) 0.0292(14) -0.0005(10) 0.0021(11) 0.0013(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'
Cl Cl 0.1484 0.1585 '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'
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
C4 O2 C5 . . 112.4(2) ?
C7 O3 C6 . . 114.7(2) ?
O1 C1 C10 . . 121.2(2) ?
O1 C1 C2 . . 120.0(2) ?
C10 C1 C2 . . 118.8(2) ?
C3 C2 C9 . . 118.4(2) ?
C3 C2 C1 . . 117.9(2) ?
C9 C2 C1 . . 123.7(2) ?
C4 C3 C2 . . 121.0(2) ?
C4 C3 H3 . . 119.5 ?
C2 C3 H3 . . 119.5 ?
O2 C4 C3 . . 118.0(2) ?
O2 C4 C7 . . 122.1(3) ?
C3 C4 C7 . . 119.9(2) ?
O2 C5 C6 . . 110.0(3) ?
O2 C5 H5A . . 109.7 ?
C6 C5 H5A . . 109.7 ?
O2 C5 H5B . . 109.7 ?
C6 C5 H5B . . 109.7 ?
H5A C5 H5B . . 108.2 ?
O3 C6 C5 . . 111.2(2) ?
O3 C6 H6A . . 109.4 ?
C5 C6 H6A . . 109.4 ?
O3 C6 H6B . . 109.4 ?
C5 C6 H6B . . 109.4 ?
H6A C6 H6B . . 108.0 ?
O3 C7 C8 . . 118.5(3) ?
O3 C7 C4 . . 122.0(3) ?
C8 C7 C4 . . 119.5(3) ?
C7 C8 C9 . . 120.5(2) ?
C7 C8 H8 . . 119.7 ?
C9 C8 H8 . . 119.7 ?
C8 C9 C2 . . 120.7(2) ?
C8 C9 H9 . . 119.7 ?
C2 C9 H9 . . 119.7 ?
C11 C10 C1 . . 120.1(3) ?
C11 C10 H10 . . 119.9 ?
C1 C10 H10 . . 119.9 ?
C10 C11 C12 . . 127.4(3) ?
C10 C11 H11 . . 116.3 ?
C12 C11 H11 . . 116.3 ?
C13 C12 C17 . . 118.7(2) ?
C13 C12 C11 . . 123.0(2) ?
C17 C12 C11 . . 118.2(2) ?
C14 C13 C12 . . 119.9(3) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C15 C14 C13 . . 119.4(3) ?
C15 C14 H14 . . 120.3 ?
C13 C14 H14 . . 120.3 ?
C14 C15 C16 . . 122.1(3) ?
C14 C15 Cl1 . . 118.6(2) ?
C16 C15 Cl1 . . 119.3(2) ?
C15 C16 C17 . . 118.5(3) ?
C15 C16 H16 . . 120.8 ?
C17 C16 H16 . . 120.8 ?
C16 C17 C12 . . 121.5(3) ?
C16 C17 H17 . . 119.3 ?
C12 C17 H17 . . 119.3 ?
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
Cl1 C15 . 1.739(3) ?
O1 C1 . 1.229(3) ?
O2 C4 . 1.372(3) ?
O2 C5 . 1.433(3) ?
O3 C7 . 1.366(3) ?
O3 C6 . 1.446(4) ?
C1 C10 . 1.480(4) ?
C1 C2 . 1.485(3) ?
C2 C3 . 1.396(4) ?
C2 C9 . 1.396(4) ?
C3 C4 . 1.384(4) ?
C3 H3 . 0.9500 ?
C4 C7 . 1.395(4) ?
C5 C6 . 1.493(5) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.380(4) ?
C8 C9 . 1.384(4) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C11 . 1.336(4) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.465(4) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.397(4) ?
C12 C17 . 1.399(4) ?
C13 C14 . 1.396(4) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.373(4) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.377(4) ?
C16 C17 . 1.379(4) ?
C16 H16 . 0.9500 ?
C17 H17 . 0.9500 ?
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
C5 H5A O3 3_465 0.99 2.61 3.595(4) 172 yes
C5 H5B Cl1 1_454 0.99 2.80 3.455(3) 124 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
O1 C1 C2 C3 . . . . -8.9(4) ?
C10 C1 C2 C3 . . . . 169.9(2) ?
O1 C1 C2 C9 . . . . 169.5(3) ?
C10 C1 C2 C9 . . . . -11.7(4) ?
C9 C2 C3 C4 . . . . 0.7(4) ?
C1 C2 C3 C4 . . . . 179.1(2) ?
C5 O2 C4 C3 . . . . 158.0(3) ?
C5 O2 C4 C7 . . . . -21.8(4) ?
C2 C3 C4 O2 . . . . -180.0(2) ?
C2 C3 C4 C7 . . . . -0.1(4) ?
C4 O2 C5 C6 . . . . 50.4(3) ?
C7 O3 C6 C5 . . . . 38.6(4) ?
O2 C5 C6 O3 . . . . -60.1(4) ?
C6 O3 C7 C8 . . . . 171.8(3) ?
C6 O3 C7 C4 . . . . -9.4(4) ?
O2 C4 C7 O3 . . . . 0.2(4) ?
C3 C4 C7 O3 . . . . -179.6(3) ?
O2 C4 C7 C8 . . . . 179.0(2) ?
C3 C4 C7 C8 . . . . -0.8(4) ?
O3 C7 C8 C9 . . . . -179.9(3) ?
C4 C7 C8 C9 . . . . 1.3(4) ?
C7 C8 C9 C2 . . . . -0.8(4) ?
C3 C2 C9 C8 . . . . -0.2(4) ?
C1 C2 C9 C8 . . . . -178.6(3) ?
O1 C1 C10 C11 . . . . 7.4(4) ?
C2 C1 C10 C11 . . . . -171.3(3) ?
C1 C10 C11 C12 . . . . -179.0(2) ?
C10 C11 C12 C13 . . . . 6.8(4) ?
C10 C11 C12 C17 . . . . -176.7(3) ?
C17 C12 C13 C14 . . . . -1.2(4) ?
C11 C12 C13 C14 . . . . 175.3(2) ?
C12 C13 C14 C15 . . . . 0.4(4) ?
C13 C14 C15 C16 . . . . 0.9(4) ?
C13 C14 C15 Cl1 . . . . -179.0(2) ?
C14 C15 C16 C17 . . . . -1.3(4) ?
Cl1 C15 C16 C17 . . . . 178.7(2) ?
C15 C16 C17 C12 . . . . 0.4(4) ?
C13 C12 C17 C16 . . . . 0.8(4) ?
C11 C12 C17 C16 . . . . -175.8(2) ?
_cod_database_fobs_code 2022806