#------------------------------------------------------------------------------
#$Date: 2019-06-18 16:09:15 +0300 (Tue, 18 Jun 2019) $
#$Revision: 216076 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021680.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_2021680
loop_
_publ_author_name
'Eugenia D. Voronova'
'Alexander A. Golovanov'
'Ivan S. Odin'
'Maksim A. Anisimov'
'Pavel V. Dorovatovskii'
'Yan V. Zubavichus'
'Anna V. Vologzhanina'
_publ_section_title
;
Peculiarities of supramolecular organization of cyclic ketones with
vinylacetylene fragments
;
_journal_coeditor_code JX3023
_journal_issue 12
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1674
_journal_page_last 1683
_journal_paper_doi 10.1107/S2053229618015838
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'C18 H20 O2'
_chemical_formula_moiety 'C18 H20 O2'
_chemical_formula_sum 'C18 H20 O2'
_chemical_formula_weight 268.34
_chemical_name_systematic
;
6-(3-Butylprop-2-yn-1-ylidene)-2-(furan-2-ylmethylene)cyclohexanone
;
_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 geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 84.218(3)
_cell_angle_beta 70.882(3)
_cell_angle_gamma 66.632(3)
_cell_formula_units_Z 2
_cell_length_a 9.2801(14)
_cell_length_b 9.5498(14)
_cell_length_c 9.6407(14)
_cell_measurement_reflns_used 2852
_cell_measurement_temperature 120
_cell_measurement_theta_max 34.66
_cell_measurement_theta_min 2.32
_cell_volume 740.63(19)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0315
_diffrn_reflns_av_unetI/netI 0.0558
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 13735
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 36.053
_diffrn_reflns_theta_min 2.325
_diffrn_source 'sealed tube'
_exptl_absorpt_coefficient_mu 0.077
_exptl_absorpt_correction_T_max 0.7471
_exptl_absorpt_correction_T_min 0.6691
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.203
_exptl_crystal_density_meas .
_exptl_crystal_description prism
_exptl_crystal_F_000 288
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_refine_diff_density_max 0.451
_refine_diff_density_min -0.324
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 182
_refine_ls_number_reflns 6779
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0903
_refine_ls_R_factor_gt 0.0577
_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^)+(0.0500P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1249
_refine_ls_wR_factor_ref 0.1390
_reflns_number_gt 4496
_reflns_number_total 6779
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file 5b.cif
_cod_data_source_block 5b
_cod_database_code 2021680
_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 0.970
_shelx_estimated_absorpt_t_max 0.985
_shelx_hkl_file
;
-1 0 0 128.89 2.20
-1 0 0 115.69 2.30
1 0 0 130.49 2.20
1 0 0 125.69 2.30
-2 0 0 14.30 0.60
2 0 0 14.80 0.60
2 0 0 14.80 0.40
-3 0 0 22.30 0.80
3 0 0 21.30 0.60
-4 0 0 44.50 1.40
4 0 0 44.30 1.40
4 0 0 43.50 1.00
-5 0 0 0.60 0.30
5 0 0 0.20 0.30
5 0 0 1.00 0.20
-6 0 0 20.60 1.20
6 0 0 21.90 1.20
6 0 0 21.40 0.60
-7 0 0 38.50 1.70
7 0 0 37.00 1.70
-8 0 0 10.10 1.20
8 0 0 9.80 1.20
-9 0 0 12.10 1.40
9 0 0 9.90 1.20
-10 0 0 21.80 1.70
10 0 0 28.80 2.00
-11 0 0 5.60 1.20
11 0 0 3.90 1.00
-12 0 0 5.10 1.20
12 0 0 4.20 1.10
-13 0 0 -0.80 0.70
13 0 0 1.10 0.80
12 -1 0 -0.10 0.80
-12 1 0 1.60 0.90
11 -1 0 9.60 1.50
-11 1 0 8.70 1.40
10 -1 0 -0.70 0.60
-10 1 0 0.50 0.60
9 -1 0 11.60 1.40
-9 1 0 11.60 1.30
8 -1 0 7.50 1.10
-8 1 0 10.50 1.20
7 -1 0 42.90 1.90
-7 1 0 46.10 2.00
6 -1 0 17.70 0.70
6 -1 0 17.90 1.10
-6 1 0 16.50 1.10
5 -1 0 2.90 0.50
5 -1 0 4.80 0.40
-5 1 0 3.10 0.50
4 -1 0 73.89 2.10
4 -1 0 72.09 1.70
-4 1 0 76.19 2.10
3 -1 0 26.40 1.00
3 -1 0 25.40 0.80
-3 1 0 24.00 0.90
2 -1 0 25.00 0.80
2 -1 0 27.30 0.80
-2 1 0 26.90 0.80
1 -1 0 1197.28 20.30
1 -1 0 1189.08 21.20
-1 1 0 1169.98 20.70
0 -1 0 257.97 4.20
0 -1 0 220.58 4.00
0 1 0 229.48 4.10
-1 -1 0 3.00 0.20
1 1 0 3.70 0.20
1 1 0 3.40 0.20
-2 -1 0 384.46 6.50
2 1 0 379.16 6.70
2 1 0 378.96 6.70
-3 -1 0 11.30 0.40
-3 -1 0 10.50 0.60
3 1 0 11.80 0.60
-4 -1 0 15.70 0.80
-4 -1 0 14.90 0.50
4 1 0 14.40 0.80
-5 -1 0 0.20 0.30
-5 -1 0 0.60 0.20
5 1 0 0.80 0.40
-6 -1 0 31.40 1.40
6 1 0 31.50 1.40
-7 -1 0 2.30 0.60
7 1 0 2.00 0.60
-8 -1 0 4.70 0.80
8 1 0 4.00 0.80
-9 -1 0 34.30 1.90
9 1 0 29.90 1.80
-10 -1 0 4.90 1.00
10 1 0 4.50 1.00
-11 -1 0 1.10 0.80
11 1 0 1.10 0.80
-12 -1 0 1.10 0.80
12 1 0 1.60 0.90
-13 -1 0 0.30 0.70
13 1 0 0.70 0.80
12 -2 0 20.30 2.20
-12 2 0 12.80 1.70
11 -2 0 0.50 0.80
-11 2 0 0.10 0.70
10 -2 0 -0.50 0.60
-10 2 0 0.30 0.60
9 -2 0 1.40 0.80
-9 2 0 1.00 0.60
8 -2 0 10.70 1.30
-8 2 0 10.30 1.30
7 -2 0 0.90 0.50
-7 2 0 0.10 0.40
6 -2 0 2.90 0.60
6 -2 0 2.60 0.40
-6 2 0 2.90 0.60
5 -2 0 50.49 1.60
5 -2 0 52.49 1.90
-5 2 0 53.29 1.90
4 -2 0 34.20 1.20
4 -2 0 33.10 1.40
-4 2 0 33.50 1.30
3 -2 0 127.49 2.80
3 -2 0 122.09 2.80
-3 2 0 123.39 2.80
2 -2 0 582.14 10.20
2 -2 0 593.34 10.40
-2 2 0 573.24 10.20
1 -2 0 188.08 3.70
1 -2 0 185.38 3.50
-1 2 0 187.88 3.50
0 -2 0 1078.29 18.90
0 2 0 1123.69 19.10
0 2 0 1127.19 18.90
-1 -2 0 1209.78 21.30
1 2 0 1212.88 21.60
1 2 0 1260.27 21.20
-2 -2 0 171.38 3.40
2 2 0 178.18 3.20
2 2 0 178.28 3.40
-3 -2 0 61.19 1.40
3 2 0 60.09 1.50
3 2 0 57.59 1.60
-4 -2 0 41.70 1.10
4 2 0 41.60 1.30
4 2 0 39.30 1.40
-5 -2 0 8.20 0.40
-5 -2 0 6.70 0.70
5 2 0 8.40 0.70
-6 -2 0 131.89 3.40
-6 -2 0 134.79 2.50
6 2 0 129.29 3.30
-7 -2 0 0.20 0.30
7 2 0 -0.60 0.30
-8 -2 0 0.70 0.40
8 2 0 1.50 0.50
-9 -2 0 33.40 1.90
9 2 0 31.40 1.80
-10 -2 0 33.00 2.00
10 2 0 33.80 2.00
-11 -2 0 4.60 1.00
11 2 0 4.70 1.00
-12 -2 0 0.30 0.60
12 2 0 1.30 0.90
-13 -2 0 4.20 1.20
13 2 0 1.50 0.90
-12 3 0 2.40 1.00
11 -3 0 0.60 0.90
-11 3 0 1.60 0.90
10 -3 0 0.70 0.80
-10 3 0 1.50 0.80
9 -3 0 0.50 0.70
-9 3 0 2.40 0.80
8 -3 0 3.00 0.70
-8 3 0 2.20 0.70
7 -3 0 52.59 2.30
-7 3 0 52.09 2.20
6 -3 0 0.30 0.40
6 -3 0 1.40 0.40
-6 3 0 0.30 0.40
5 -3 0 -0.20 0.30
5 -3 0 0.50 0.30
-5 3 0 -0.10 0.30
4 -3 0 37.60 1.50
4 -3 0 40.10 1.50
-4 3 0 34.90 1.40
3 -3 0 640.94 11.60
3 -3 0 634.54 11.40
-3 3 0 630.74 11.50
2 -3 0 0.60 0.30
2 -3 0 0.00 0.20
-2 3 0 0.10 0.20
1 -3 0 121.79 2.50
1 -3 0 125.39 2.90
-1 3 0 121.79 2.60
0 -3 0 7.20 0.60
0 3 0 6.50 0.30
0 3 0 6.80 0.40
-1 -3 0 48.10 1.50
1 3 0 49.90 1.10
1 3 0 49.30 1.20
-2 -3 0 0.00 0.20
2 3 0 0.20 0.20
2 3 0 0.10 0.10
-3 -3 0 7.50 0.60
3 3 0 7.70 0.50
3 3 0 7.90 0.60
-4 -3 0 36.20 1.20
4 3 0 36.70 1.20
4 3 0 36.30 1.30
-5 -3 0 28.00 1.00
5 3 0 28.40 1.10
5 3 0 28.40 1.20
-6 -3 0 22.80 0.80
-6 -3 0 21.80 1.20
6 3 0 21.10 1.10
-7 -3 0 0.30 0.40
-7 -3 0 0.20 0.20
7 3 0 -0.30 0.30
-8 -3 0 14.60 1.20
8 3 0 14.30 1.10
9 3 0 20.60 1.40
-10 -3 0 0.40 0.50
10 3 0 0.90 0.60
-11 -3 0 10.00 1.40
11 3 0 9.40 1.30
-12 -3 0 1.60 0.80
12 3 0 2.50 0.90
-13 -3 0 1.90 0.80
13 3 0 2.80 1.10
-14 -3 0 5.30 1.90
11 -4 0 0.40 0.80
-11 4 0 0.80 0.90
10 -4 0 1.50 0.90
-10 4 0 1.80 0.90
9 -4 0 2.70 1.00
-9 4 0 4.30 1.00
8 -4 0 0.90 0.60
-8 4 0 0.30 0.50
7 -4 0 11.70 1.30
-7 4 0 12.50 1.30
6 -4 0 0.90 0.40
6 -4 0 1.40 0.60
-6 4 0 0.80 0.50
5 -4 0 0.00 0.40
5 -4 0 0.20 0.30
-5 4 0 -0.20 0.30
4 -4 0 45.90 1.70
4 -4 0 45.40 1.80
-4 4 0 45.90 1.70
3 -4 0 24.80 1.10
3 -4 0 25.60 1.30
-3 4 0 24.30 1.10
2 -4 0 21.40 1.00
2 -4 0 23.60 1.20
-2 4 0 22.80 1.00
1 -4 0 3.30 0.40
1 -4 0 2.60 0.50
-1 4 0 2.20 0.30
0 -4 0 9.60 0.80
0 4 0 9.50 0.50
0 4 0 10.10 0.50
-1 -4 0 15.30 0.90
1 4 0 16.40 0.70
1 4 0 15.20 0.50
-2 -4 0 19.70 1.00
2 4 0 19.70 0.80
2 4 0 20.90 0.70
-3 -4 0 165.08 3.70
3 4 0 161.28 3.50
3 4 0 167.98 3.20
-4 -4 0 36.60 1.40
4 4 0 38.20 1.40
4 4 0 37.10 1.20
-5 -4 0 116.09 2.80
5 4 0 115.59 3.00
5 4 0 111.99 2.70
-6 -4 0 -0.20 0.20
6 4 0 -0.10 0.30
6 4 0 0.10 0.40
-7 -4 0 0.90 0.40
-7 -4 0 2.60 0.40
7 4 0 1.80 0.50
-8 -4 0 18.30 1.30
8 4 0 17.50 1.20
-9 -4 0 43.80 2.20
9 4 0 45.90 2.00
-10 -4 0 36.40 2.00
10 4 0 35.00 1.90
-11 -4 0 7.20 1.20
11 4 0 8.20 1.20
-12 -4 0 0.30 0.60
12 4 0 0.20 0.60
-13 -4 0 0.90 0.70
13 4 0 0.30 0.70
-14 -4 0 8.00 1.50
14 4 0 7.70 1.60
10 -5 0 0.20 0.90
-10 5 0 0.70 0.80
9 -5 0 8.10 1.40
-9 5 0 9.70 1.40
8 -5 0 15.60 1.70
-8 5 0 11.40 1.50
7 -5 0 4.00 0.90
-7 5 0 3.50 0.80
6 -5 0 12.10 1.20
6 -5 0 12.50 1.30
-6 5 0 11.60 1.20
5 -5 0 4.30 0.80
5 -5 0 4.60 0.80
-5 5 0 4.10 0.70
4 -5 0 75.99 2.60
4 -5 0 67.89 2.30
-4 5 0 75.19 2.40
3 -5 0 0.00 0.40
3 -5 0 0.40 0.30
-3 5 0 1.50 0.40
2 -5 0 118.19 3.40
2 -5 0 116.09 2.80
-2 5 0 114.09 2.80
1 -5 0 23.90 1.00
1 -5 0 21.70 1.30
-1 5 0 23.90 1.00
0 -5 0 35.00 1.60
0 5 0 32.10 1.00
0 5 0 34.40 1.10
-1 -5 0 57.09 2.00
1 5 0 58.89 1.60
1 5 0 57.49 1.40
-2 -5 0 -0.30 0.30
2 5 0 0.00 0.20
2 5 0 0.10 0.20
-3 -5 0 179.78 4.20
3 5 0 181.88 3.50
3 5 0 183.08 3.90
-4 -5 0 17.30 1.10
4 5 0 17.30 0.80
4 5 0 17.20 0.90
-5 -5 0 31.90 1.40
5 5 0 29.70 1.30
5 5 0 29.70 1.10
-6 -5 0 128.29 3.20
6 5 0 127.59 3.10
6 5 0 130.79 3.50
-7 -5 0 3.60 0.60
7 5 0 2.50 0.60
7 5 0 3.60 0.60
-8 -5 0 13.70 1.20
8 5 0 15.40 1.10
-9 -5 0 16.80 1.40
9 5 0 15.90 1.20
-10 -5 0 29.30 1.90
10 5 0 25.20 1.60
-11 -5 0 10.40 1.40
11 5 0 9.40 1.20
-12 -5 0 0.20 0.70
12 5 0 0.10 0.60
-13 -5 0 0.90 0.80
13 5 0 -0.30 0.70
-14 -5 0 0.60 0.80
14 5 0 -0.70 0.70
10 -6 0 7.70 1.50
9 -6 0 20.00 2.10
8 -6 0 4.00 1.10
-8 6 0 2.80 0.80
7 -6 0 9.70 1.40
-7 6 0 10.20 1.30
6 -6 0 0.80 0.60
-6 6 0 0.30 0.50
5 -6 0 3.60 0.80
5 -6 0 3.90 0.80
-5 6 0 4.70 0.80
4 -6 0 0.30 0.50
4 -6 0 0.70 0.60
-4 6 0 1.00 0.50
3 -6 0 27.90 1.70
3 -6 0 26.80 1.40
-3 6 0 24.80 1.30
2 -6 0 59.39 2.40
2 -6 0 59.29 1.90
-2 6 0 63.39 2.00
1 -6 0 22.30 1.50
-1 6 0 19.90 1.00
-1 6 0 22.20 0.90
0 -6 0 1.70 0.60
0 6 0 2.20 0.40
0 6 0 3.10 0.40
-1 -6 0 56.49 2.20
1 6 0 55.99 1.40
1 6 0 56.29 1.70
-2 -6 0 72.39 2.50
2 6 0 71.69 1.70
2 6 0 71.49 2.00
-3 -6 0 5.80 0.80
3 6 0 7.80 0.50
3 6 0 8.80 0.70
-4 -6 0 31.30 1.60
4 6 0 32.70 1.10
4 6 0 28.50 1.30
-5 -6 0 3.20 0.60
5 6 0 3.00 0.50
5 6 0 2.10 0.50
-6 -6 0 66.19 2.30
6 6 0 66.39 2.00
6 6 0 66.29 2.30
-7 -6 0 0.80 0.50
7 6 0 0.90 0.40
7 6 0 0.60 0.50
-8 -6 0 3.30 0.60
8 6 0 2.80 0.70
8 6 0 3.20 0.60
-9 -6 0 24.00 1.60
9 6 0 22.80 1.40
-10 -6 0 10.00 1.30
10 6 0 9.90 1.10
-11 -6 0 0.90 0.70
11 6 0 0.90 0.60
-12 -6 0 -0.60 0.50
12 6 0 -0.40 0.50
-13 -6 0 -0.50 0.60
13 6 0 0.80 0.70
-14 -6 0 4.90 1.30
14 6 0 4.70 1.20
9 -7 0 2.30 1.20
8 -7 0 1.00 0.90
7 -7 0 4.30 1.10
-7 7 0 3.00 0.90
6 -7 0 0.30 0.60
-6 7 0 0.80 0.50
5 -7 0 1.10 0.60
5 -7 0 0.20 0.60
-5 7 0 1.50 0.50
4 -7 0 10.70 1.10
4 -7 0 7.30 1.20
-4 7 0 8.20 1.00
3 -7 0 122.29 3.30
3 -7 0 118.29 3.90
-3 7 0 123.29 3.30
2 -7 0 33.40 1.90
-2 7 0 32.20 1.40
-2 7 0 31.70 1.30
1 -7 0 7.90 1.20
-1 7 0 8.30 0.70
-1 7 0 8.90 0.70
0 -7 0 76.79 2.90
0 7 0 77.29 2.00
0 7 0 77.39 2.20
-1 -7 0 10.70 1.30
1 7 0 10.90 0.70
1 7 0 12.20 0.60
-2 -7 0 40.50 2.00
2 7 0 41.20 1.50
2 7 0 40.40 1.20
-3 -7 0 29.80 1.70
3 7 0 30.40 1.30
3 7 0 29.90 1.00
-4 -7 0 1.00 0.60
4 7 0 0.70 0.30
4 7 0 0.50 0.30
-5 -7 0 14.90 1.30
5 7 0 14.10 0.80
5 7 0 14.40 1.00
-6 -7 0 11.80 1.20
6 7 0 9.30 1.10
6 7 0 13.00 0.80
-7 -7 0 328.37 7.20
7 7 0 335.57 6.80
7 7 0 333.47 7.30
-8 -7 0 11.10 1.10
8 7 0 11.60 1.30
8 7 0 11.90 1.00
-9 -7 0 4.80 0.90
9 7 0 3.80 0.70
-10 -7 0 1.40 0.70
10 7 0 1.60 0.60
-11 -7 0 1.20 0.70
11 7 0 1.30 0.60
-12 -7 0 0.30 0.70
12 7 0 0.70 0.60
-13 -7 0 0.50 0.70
13 7 0 0.40 0.70
-14 -7 0 0.90 0.80
14 7 0 0.60 0.80
8 -8 0 1.40 1.10
7 -8 0 25.00 2.30
6 -8 0 7.00 1.30
-6 8 0 5.00 1.10
5 -8 0 1.10 0.70
5 -8 0 1.10 0.70
-5 8 0 1.10 0.60
4 -8 0 2.00 0.80
-4 8 0 2.70 0.60
-4 8 0 1.90 0.60
3 -8 0 0.40 0.60
-3 8 0 1.00 0.50
-3 8 0 0.40 0.40
2 -8 0 1.50 0.70
-2 8 0 2.10 0.50
-2 8 0 1.40 0.40
1 -8 0 2.50 0.80
-1 8 0 1.30 0.40
-1 8 0 2.20 0.40
0 -8 0 70.29 3.00
0 8 0 64.59 1.80
0 8 0 63.59 2.00
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8 3 14 -0.20 1.00
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10 3 14 2.10 1.20
-2 -4 -14 0.30 1.00
-3 -4 -14 6.50 1.50
-4 -4 -14 0.10 0.90
-5 -4 -14 5.50 1.40
7 4 14 0.50 0.80
8 4 14 2.40 1.20
9 4 14 12.00 2.10
10 4 14 -0.20 0.90
1 5 14 5.90 1.20
-2 -5 -14 4.80 1.40
-3 -5 -14 8.40 1.70
-4 -5 -14 2.00 1.10
-5 -5 -14 1.10 1.10
-6 -5 -14 1.90 1.20
-7 -5 -14 3.30 1.20
-8 -5 -14 1.90 1.30
-9 -5 -14 3.00 1.30
-10 -5 -14 -0.80 0.90
1 6 14 0.40 0.70
2 6 14 10.00 1.50
-3 -6 -14 1.70 1.10
3 6 14 1.30 0.70
-4 -6 -14 -0.20 0.90
-5 -6 -14 0.70 1.00
-6 -6 -14 1.40 1.10
-7 -6 -14 0.10 0.90
-8 -6 -14 12.90 2.20
-9 -6 -14 8.40 1.90
-10 -6 -14 3.20 1.40
-3 -7 -14 -0.20 0.90
3 7 14 -1.10 0.60
-4 -7 -14 2.10 1.10
4 7 14 1.90 0.80
-5 -7 -14 0.40 1.00
5 7 14 -0.30 0.60
-6 -7 -14 1.70 1.10
-7 -7 -14 3.50 1.40
-8 -7 -14 0.50 1.10
-9 -7 -14 1.50 1.10
-4 -8 -14 2.40 1.30
4 8 14 1.30 0.70
-5 -8 -14 0.90 1.20
5 8 14 1.10 0.80
-6 -8 -14 -0.20 1.00
6 8 14 0.80 0.70
-7 -8 -14 1.70 1.30
-8 -8 -14 0.00 1.10
-1 3 -15 -0.30 1.60
-2 3 -15 0.00 1.00
2 -3 15 0.70 1.10
-3 3 -15 0.10 1.00
3 -3 15 3.80 1.30
-4 3 -15 -1.10 0.80
4 -3 15 -0.50 1.10
-5 3 -15 6.60 1.60
0 2 -15 0.80 1.20
-1 2 -15 -0.90 0.80
-2 2 -15 4.10 1.30
2 -2 15 4.30 1.40
-3 2 -15 8.80 1.60
3 -2 15 10.70 2.00
-4 2 -15 0.20 0.90
4 -2 15 0.40 0.90
-5 2 -15 2.00 1.10
5 -2 15 1.40 1.20
-6 2 -15 -1.50 0.80
6 -2 15 0.50 1.80
0 1 -15 0.50 0.90
-1 1 -15 2.90 1.20
-2 1 -15 13.10 1.80
2 -1 15 10.30 1.90
-3 1 -15 11.30 1.60
3 -1 15 12.20 2.10
-4 1 -15 9.40 1.50
4 -1 15 8.60 1.90
-5 1 -15 -0.30 0.90
5 -1 15 1.90 1.10
-6 1 -15 2.40 1.00
6 -1 15 0.50 1.00
-7 1 -15 0.20 0.90
7 -1 15 1.50 1.80
2 0 15 2.30 1.10
-3 0 -15 2.80 1.50
3 0 15 2.10 1.10
-4 0 -15 0.30 1.20
4 0 15 1.50 1.10
-5 0 -15 0.30 1.40
5 0 15 0.60 1.10
6 0 15 1.30 1.20
7 0 15 0.10 1.00
2 1 15 2.90 1.20
3 1 15 1.20 1.00
4 1 15 3.10 1.30
5 1 15 -0.30 0.80
6 1 15 0.90 1.10
7 1 15 1.20 1.20
8 1 15 0.40 1.00
-2 -2 -15 -0.50 1.00
3 2 15 4.10 1.30
4 2 15 0.10 0.80
5 2 15 0.60 1.10
6 2 15 0.60 1.00
7 2 15 8.10 1.80
8 2 15 6.00 1.70
-3 -3 -15 6.20 1.50
-4 -3 -15 11.50 2.00
5 3 15 1.00 1.00
6 3 15 0.00 1.00
7 3 15 7.30 1.80
8 3 15 1.70 1.20
-3 -4 -15 6.90 1.60
-4 -4 -15 3.40 1.30
-5 -4 -15 2.90 1.30
-6 -4 -15 -0.40 0.90
-7 -4 -15 1.10 1.20
-3 -5 -15 -1.20 0.90
-4 -5 -15 1.80 1.20
-5 -5 -15 2.10 1.30
-6 -5 -15 1.70 1.20
-7 -5 -15 -0.90 1.00
-8 -5 -15 0.00 1.00
-4 -6 -15 2.00 1.40
-5 -6 -15 -0.30 1.00
-6 -6 -15 0.80 1.20
-7 -6 -15 1.40 1.80
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 61134
_shelx_res_file
;
TITL hate_a.res in P-1
REM Old TITL hate in P-1
REM SHELXT solution in P-1
REM R1 0.128, Rweak 0.006, Alpha 0.040, Orientation as input
REM Formula found by SHELXT: C18 O2
CELL 0.71073 9.2801 9.5498 9.6407 84.218 70.882 66.632
ZERR 2 0.0014 0.0014 0.0014 0.003 0.003 0.003
LATT 1
SFAC C H O
UNIT 36 40 4
L.S. 4
PLAN 20
SIZE 0.2 0.3 0.4
TEMP -153.15
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.050000 0.150000
FVAR 0.56856
O1 3 0.236546 0.693765 0.127314 11.00000 0.02672 0.01583 =
0.03730 0.00517 -0.01998 -0.00810
O2 3 0.066105 0.312492 0.046098 11.00000 0.02583 0.01670 =
0.03972 0.00302 -0.02070 -0.00769
C1 1 0.338194 0.583731 0.167661 11.00000 0.01851 0.01701 =
0.01969 0.00204 -0.00800 -0.00700
C2 1 0.463802 0.604144 0.218906 11.00000 0.01881 0.01848 =
0.01916 0.00286 -0.00823 -0.00780
C3 1 0.601144 0.465998 0.244683 11.00000 0.02206 0.02107 =
0.03354 0.00460 -0.01623 -0.00825
AFIX 23
H3A 2 0.648467 0.493867 0.310791 11.00000 -1.20000
H3B 2 0.689832 0.426762 0.150235 11.00000 -1.20000
AFIX 0
C4 1 0.537852 0.342391 0.313224 11.00000 0.02926 0.02063 =
0.03063 0.00760 -0.01835 -0.01014
AFIX 23
H4A 2 0.451404 0.380771 0.408990 11.00000 -1.20000
H4B 2 0.629725 0.252388 0.331049 11.00000 -1.20000
AFIX 0
C5 1 0.466326 0.295347 0.212792 11.00000 0.02352 0.01499 =
0.02639 0.00316 -0.01231 -0.00632
AFIX 23
H5A 2 0.557566 0.240353 0.124699 11.00000 -1.20000
H5B 2 0.414760 0.223853 0.264900 11.00000 -1.20000
AFIX 0
C6 1 0.339685 0.428010 0.164751 11.00000 0.01862 0.01519 =
0.01848 0.00193 -0.00701 -0.00680
C7 1 0.225259 0.416447 0.114156 11.00000 0.01948 0.01479 =
0.02166 0.00174 -0.00762 -0.00624
AFIX 43
H7 2 0.150326 0.509884 0.090492 11.00000 -1.20000
AFIX 0
C8 1 0.201640 0.282373 0.091369 11.00000 0.01807 0.01712 =
0.02336 0.00155 -0.00971 -0.00661
C9 1 0.277161 0.128613 0.101307 11.00000 0.02176 0.01611 =
0.02964 0.00136 -0.01318 -0.00583
AFIX 43
H9 2 0.373746 0.076529 0.129415 11.00000 -1.20000
AFIX 0
C10 1 0.184368 0.061082 0.061780 11.00000 0.02912 0.01628 =
0.03770 0.00110 -0.01778 -0.00853
AFIX 43
H10 2 0.206110 -0.044704 0.058776 11.00000 -1.20000
AFIX 0
C11 1 0.059363 0.176371 0.029334 11.00000 0.03115 0.02003 =
0.04341 0.00152 -0.02188 -0.01183
AFIX 43
H11 2 -0.022486 0.163945 -0.001184 11.00000 -1.20000
AFIX 0
C12 1 0.443790 0.748135 0.241160 11.00000 0.02296 0.02060 =
0.02574 0.00246 -0.01186 -0.00958
AFIX 43
H12 2 0.350117 0.827495 0.224171 11.00000 -1.20000
AFIX 0
C13 1 0.550115 0.792312 0.287798 11.00000 0.02592 0.02062 =
0.02646 0.00196 -0.01148 -0.01021
C14 1 0.634625 0.838266 0.325806 11.00000 0.02722 0.02371 =
0.02810 0.00048 -0.01198 -0.01109
C15 1 0.738839 0.889564 0.376135 11.00000 0.02914 0.02586 =
0.03380 -0.00151 -0.01503 -0.01380
AFIX 23
H15A 2 0.667413 0.966353 0.457333 11.00000 -1.20000
H15B 2 0.795241 0.940170 0.294594 11.00000 -1.20000
AFIX 0
C16 1 0.868734 0.761201 0.429006 11.00000 0.02263 0.02725 =
0.02839 -0.00065 -0.00915 -0.01152
AFIX 23
H16A 2 0.813377 0.708255 0.508794 11.00000 -1.20000
H16B 2 0.943502 0.686082 0.347089 11.00000 -1.20000
AFIX 0
C17 1 0.969629 0.820463 0.484714 11.00000 0.02960 0.04264 =
0.03450 -0.00284 -0.01438 -0.01750
AFIX 23
H17A 2 0.893667 0.901322 0.561265 11.00000 -1.20000
H17B 2 1.030812 0.867024 0.402749 11.00000 -1.20000
AFIX 0
C18 1 1.091772 0.697002 0.548214 11.00000 0.02935 0.06550 =
0.03731 0.00461 -0.01577 -0.01531
AFIX 137
H18A 2 1.168573 0.617282 0.472566 11.00000 -1.50000
H18B 2 1.031803 0.652476 0.631406 11.00000 -1.50000
H18C 2 1.153891 0.741443 0.581715 11.00000 -1.50000
AFIX 0
HKLF 4
REM hate_a.res in P-1
REM R1 = 0.0577 for 4496 Fo > 4sig(Fo) and 0.0903 for all 6779 data
REM 182 parameters refined using 0 restraints
END
WGHT 0.0792 0.0176
REM Highest difference peak 0.451, deepest hole -0.324, 1-sigma level 0.058
Q1 1 0.4000 0.6000 0.1982 11.00000 0.05 0.45
Q2 1 0.2526 0.2056 0.0960 11.00000 0.05 0.44
Q3 1 0.4554 0.6751 0.2238 11.00000 0.05 0.43
Q4 1 0.4032 0.3650 0.1924 11.00000 0.05 0.42
Q5 1 0.1983 0.3553 0.1120 11.00000 0.05 0.40
Q6 1 0.2823 0.4285 0.1490 11.00000 0.05 0.39
Q7 1 0.3519 0.5001 0.1586 11.00000 0.05 0.38
Q8 1 0.6247 0.7788 0.3136 11.00000 0.05 0.37
Q9 1 0.5770 0.3989 0.2778 11.00000 0.05 0.37
Q10 1 0.5351 0.5330 0.2246 11.00000 0.05 0.36
Q11 1 0.5821 0.8562 0.2808 11.00000 0.05 0.36
Q12 1 0.1213 0.1140 0.0489 11.00000 0.05 0.35
Q13 1 0.5022 0.3088 0.2733 11.00000 0.05 0.34
Q14 1 0.4816 0.7825 0.2719 11.00000 0.05 0.33
Q15 1 0.2348 0.0933 0.0727 11.00000 0.05 0.33
Q16 1 0.7018 0.8635 0.3442 11.00000 0.05 0.31
Q17 1 0.8079 0.8178 0.4095 11.00000 0.05 0.31
Q18 1 0.9327 0.7758 0.4470 11.00000 0.05 0.31
Q19 1 0.2762 0.6601 0.1720 11.00000 0.05 0.29
Q20 1 0.1363 0.2983 0.0648 11.00000 0.05 0.27
;
_shelx_res_checksum 68326
_shelxl_version_number 2.014
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
O O1 0.23655(10) 0.69376(8) 0.12731(9) 0.02436(17) Uani d 1 . .
O O2 0.06610(10) 0.31249(8) 0.04610(9) 0.02500(17) Uani d 1 . .
C C1 0.33819(12) 0.58373(11) 0.16766(11) 0.01795(18) Uani d 1 . .
C C2 0.46380(12) 0.60414(11) 0.21891(11) 0.01820(18) Uani d 1 . .
C C3 0.60114(13) 0.46600(12) 0.24468(13) 0.0239(2) Uani d 1 . .
H H3A 0.6485 0.4939 0.3108 0.029 Uiso calc 1 . .
H H3B 0.6898 0.4268 0.1502 0.029 Uiso calc 1 . .
C C4 0.53785(15) 0.34239(12) 0.31322(13) 0.0248(2) Uani d 1 . .
H H4A 0.4514 0.3808 0.4090 0.030 Uiso calc 1 . .
H H4B 0.6297 0.2524 0.3310 0.030 Uiso calc 1 . .
C C5 0.46633(13) 0.29535(11) 0.21279(12) 0.0210(2) Uani d 1 . .
H H5A 0.5576 0.2404 0.1247 0.025 Uiso calc 1 . .
H H5B 0.4148 0.2239 0.2649 0.025 Uiso calc 1 . .
C C6 0.33968(12) 0.42801(11) 0.16475(11) 0.01714(18) Uani d 1 . .
C C7 0.22526(12) 0.41645(11) 0.11416(11) 0.01856(18) Uani d 1 . .
H H7 0.1503 0.5099 0.0905 0.022 Uiso calc 1 . .
C C8 0.20164(12) 0.28237(11) 0.09137(11) 0.01880(18) Uani d 1 . .
C C9 0.27716(13) 0.12861(11) 0.10131(12) 0.0217(2) Uani d 1 . .
H H9 0.3737 0.0765 0.1294 0.026 Uiso calc 1 . .
C C10 0.18437(14) 0.06108(12) 0.06178(13) 0.0259(2) Uani d 1 . .
H H10 0.2061 -0.0447 0.0588 0.031 Uiso calc 1 . .
C C11 0.05936(15) 0.17637(13) 0.02933(14) 0.0282(2) Uani d 1 . .
H H11 -0.0225 0.1639 -0.0012 0.034 Uiso calc 1 . .
C C12 0.44379(13) 0.74814(12) 0.24116(12) 0.0217(2) Uani d 1 . .
H H12 0.3501 0.8275 0.2242 0.026 Uiso calc 1 . .
C C13 0.55011(14) 0.79231(12) 0.28780(12) 0.0232(2) Uani d 1 . .
C C14 0.63463(14) 0.83827(13) 0.32581(13) 0.0250(2) Uani d 1 . .
C C15 0.73884(15) 0.88956(13) 0.37614(14) 0.0270(2) Uani d 1 . .
H H15A 0.6674 0.9664 0.4573 0.032 Uiso calc 1 . .
H H15B 0.7952 0.9402 0.2946 0.032 Uiso calc 1 . .
C C16 0.86873(14) 0.76120(13) 0.42901(13) 0.0250(2) Uani d 1 . .
H H16A 0.8134 0.7083 0.5088 0.030 Uiso calc 1 . .
H H16B 0.9435 0.6861 0.3471 0.030 Uiso calc 1 . .
C C17 0.96963(16) 0.82046(16) 0.48471(15) 0.0330(3) Uani d 1 . .
H H17A 0.8937 0.9013 0.5613 0.040 Uiso calc 1 . .
H H17B 1.0308 0.8670 0.4027 0.040 Uiso calc 1 . .
C C18 1.09177(17) 0.69700(19) 0.54821(16) 0.0439(4) Uani d 1 . .
H H18A 1.1686 0.6173 0.4726 0.066 Uiso calc 1 . .
H H18B 1.0318 0.6525 0.6314 0.066 Uiso calc 1 . .
H H18C 1.1539 0.7414 0.5817 0.066 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
O1 0.0267(4) 0.0158(3) 0.0373(4) -0.0081(3) -0.0200(3) 0.0052(3)
O2 0.0258(4) 0.0167(3) 0.0397(5) -0.0077(3) -0.0207(3) 0.0030(3)
C1 0.0185(4) 0.0170(4) 0.0197(4) -0.0070(3) -0.0080(3) 0.0020(3)
C2 0.0188(4) 0.0185(4) 0.0192(4) -0.0078(3) -0.0082(4) 0.0029(3)
C3 0.0221(5) 0.0211(5) 0.0335(6) -0.0082(4) -0.0162(4) 0.0046(4)
C4 0.0293(5) 0.0206(5) 0.0306(6) -0.0101(4) -0.0184(5) 0.0076(4)
C5 0.0235(5) 0.0150(4) 0.0264(5) -0.0063(4) -0.0123(4) 0.0032(4)
C6 0.0186(4) 0.0152(4) 0.0185(4) -0.0068(3) -0.0070(3) 0.0019(3)
C7 0.0195(4) 0.0148(4) 0.0217(5) -0.0062(3) -0.0076(4) 0.0017(3)
C8 0.0181(4) 0.0171(4) 0.0234(5) -0.0066(3) -0.0097(4) 0.0015(3)
C9 0.0218(5) 0.0161(4) 0.0296(5) -0.0058(4) -0.0132(4) 0.0014(4)
C10 0.0291(5) 0.0163(4) 0.0377(6) -0.0085(4) -0.0178(5) 0.0011(4)
C11 0.0312(6) 0.0200(5) 0.0434(7) -0.0118(4) -0.0219(5) 0.0015(4)
C12 0.0230(5) 0.0206(5) 0.0257(5) -0.0096(4) -0.0119(4) 0.0025(4)
C13 0.0259(5) 0.0206(5) 0.0265(5) -0.0102(4) -0.0115(4) 0.0020(4)
C14 0.0272(5) 0.0237(5) 0.0281(5) -0.0111(4) -0.0120(4) 0.0005(4)
C15 0.0291(6) 0.0259(5) 0.0338(6) -0.0138(4) -0.0150(5) -0.0015(4)
C16 0.0226(5) 0.0272(5) 0.0284(5) -0.0115(4) -0.0091(4) -0.0007(4)
C17 0.0296(6) 0.0426(7) 0.0345(6) -0.0175(5) -0.0144(5) -0.0028(5)
C18 0.0293(7) 0.0655(10) 0.0373(7) -0.0153(7) -0.0158(6) 0.0046(7)
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'
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
C11 O2 C8 . . 106.96(8)
O1 C1 C2 . . 120.48(9)
O1 C1 C6 . . 120.95(9)
C6 C1 C2 . . 118.56(8)
C1 C2 C3 . . 119.03(9)
C12 C2 C1 . . 116.87(9)
C12 C2 C3 . . 124.09(9)
C2 C3 H3A . . 109.6
C2 C3 H3B . . 109.6
C2 C3 C4 . . 110.44(9)
H3A C3 H3B . . 108.1
C4 C3 H3A . . 109.6
C4 C3 H3B . . 109.6
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
C3 C4 C5 . . 110.80(9)
H4A C4 H4B . . 108.1
C5 C4 H4A . . 109.5
C5 C4 H4B . . 109.5
C4 C5 H5A . . 108.9
C4 C5 H5B . . 108.9
H5A C5 H5B . . 107.7
C6 C5 C4 . . 113.29(8)
C6 C5 H5A . . 108.9
C6 C5 H5B . . 108.9
C1 C6 C5 . . 119.92(9)
C7 C6 C1 . . 115.73(8)
C7 C6 C5 . . 124.33(9)
C6 C7 H7 . . 115.7
C6 C7 C8 . . 128.70(9)
C8 C7 H7 . . 115.7
O2 C8 C7 . . 113.56(8)
C9 C8 O2 . . 108.80(9)
C9 C8 C7 . . 137.64(10)
C8 C9 H9 . . 126.5
C8 C9 C10 . . 107.02(9)
C10 C9 H9 . . 126.5
C9 C10 H10 . . 126.8
C11 C10 C9 . . 106.45(9)
C11 C10 H10 . . 126.8
O2 C11 H11 . . 124.6
C10 C11 O2 . . 110.78(10)
C10 C11 H11 . . 124.6
C2 C12 H12 . . 117.1
C2 C12 C13 . . 125.79(10)
C13 C12 H12 . . 117.1
C14 C13 C12 . . 176.18(12)
C13 C14 C15 . . 177.80(12)
C14 C15 H15A . . 108.8
C14 C15 H15B . . 108.8
C14 C15 C16 . . 113.67(9)
H15A C15 H15B . . 107.7
C16 C15 H15A . . 108.8
C16 C15 H15B . . 108.8
C15 C16 H16A . . 109.3
C15 C16 H16B . . 109.3
H16A C16 H16B . . 107.9
C17 C16 C15 . . 111.74(10)
C17 C16 H16A . . 109.3
C17 C16 H16B . . 109.3
C16 C17 H17A . . 109.0
C16 C17 H17B . . 109.0
C16 C17 C18 . . 113.00(12)
H17A C17 H17B . . 107.8
C18 C17 H17A . . 109.0
C18 C17 H17B . . 109.0
C17 C18 H18A . . 109.5
C17 C18 H18B . . 109.5
C17 C18 H18C . . 109.5
H18A C18 H18B . . 109.5
H18A C18 H18C . . 109.5
H18B C18 H18C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O1 C1 . 1.2317(12)
O2 C8 . 1.3793(12)
O2 C11 . 1.3540(13)
C1 C2 . 1.4892(14)
C1 C6 . 1.4847(13)
C2 C3 . 1.4947(14)
C2 C12 . 1.3424(14)
C3 H3A . 0.9900
C3 H3B . 0.9900
C3 C4 . 1.5211(15)
C4 H4A . 0.9900
C4 H4B . 0.9900
C4 C5 . 1.5248(15)
C5 H5A . 0.9900
C5 H5B . 0.9900
C5 C6 . 1.5026(13)
C6 C7 . 1.3494(14)
C7 H7 . 0.9500
C7 C8 . 1.4306(14)
C8 C9 . 1.3623(14)
C9 H9 . 0.9500
C9 C10 . 1.4169(15)
C10 H10 . 0.9500
C10 C11 . 1.3457(15)
C11 H11 . 0.9500
C12 H12 . 0.9500
C12 C13 . 1.4187(15)
C13 C14 . 1.1982(15)
C14 C15 . 1.4635(15)
C15 H15A . 0.9900
C15 H15B . 0.9900
C15 C16 . 1.5231(16)
C16 H16A . 0.9900
C16 H16B . 0.9900
C16 C17 . 1.5154(16)
C17 H17A . 0.9900
C17 H17B . 0.9900
C17 C18 . 1.5161(19)
C18 H18A . 0.9800
C18 H18B . 0.9800
C18 H18C . 0.9800
_cod_database_fobs_code 2021680