#------------------------------------------------------------------------------
#$Date: 2019-06-18 16:07:37 +0300 (Tue, 18 Jun 2019) $
#$Revision: 216070 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021674.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_2021674
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 'C23 H14 Br2 O'
_chemical_formula_moiety 'C23 H14 Br2 O'
_chemical_formula_sum 'C23 H14 Br2 O'
_chemical_formula_weight 466.16
_chemical_name_systematic
;
2,5-Bis[3-(4-bromophenyl)prop-2-yn-1-ylidene]cyclopentanone
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 39
_space_group_name_Hall 'A 2 -2b'
_space_group_name_H-M_alt 'A e m 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.098(3)
_cell_length_b 42.72(2)
_cell_length_c 6.135(3)
_cell_measurement_reflns_used 6354
_cell_measurement_temperature 120
_cell_measurement_theta_max 31
_cell_measurement_theta_min 2
_cell_volume 1860.3(15)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0879
_diffrn_reflns_av_unetI/netI 0.0959
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 60
_diffrn_reflns_limit_k_min -59
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 9371
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.500
_diffrn_reflns_theta_min 1.907
_exptl_absorpt_coefficient_mu 4.367
_exptl_absorpt_correction_T_max 0.737
_exptl_absorpt_correction_T_min 0.664
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.665
_exptl_crystal_description needle
_exptl_crystal_F_000 920
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.927
_refine_diff_density_min -1.090
_refine_ls_abs_structure_details
;
Flack x determined using 608 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.30(2)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.969
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 121
_refine_ls_number_reflns 2642
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.969
_refine_ls_R_factor_all 0.0966
_refine_ls_R_factor_gt 0.0635
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1478
_refine_ls_wR_factor_ref 0.1649
_reflns_number_gt 1928
_reflns_number_total 2642
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file 3b.cif
_cod_data_source_block 3b
_cod_original_cell_volume 1860.1(15)
_cod_original_sg_symbol_Hall 'A 2 -2c'
_cod_original_sg_symbol_H-M 'A b m 2'
_cod_database_code 2021674
_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 0.664
_shelx_estimated_absorpt_t_max 0.737
_shelx_hkl_file
;
0 0 -2 2055.99 159.38
0 0 -4 602.24 47.90
0 0 -6 113.69 13.20
0 0 -8 45.30 10.40
0 -1 -1 -0.10 1.10
0 -1 -1 -1.60 0.90
0 1 -1 0.40 1.00
0 -1 -3 2.40 2.50
0 1 -3 -2.30 2.30
0 -1 -5 -1.60 4.20
0 1 -5 -1.50 4.40
0 -1 -7 -8.80 6.50
0 1 -7 -3.20 7.00
0 2 0 -0.10 0.10
0 -2 -2 1650.83 127.39
0 -2 -2 1661.03 127.19
0 2 -2 1605.94 127.19
0 2 -4 602.44 47.00
0 -2 -4 576.64 46.90
0 -2 -6 259.07 23.00
0 2 -6 255.07 23.00
0 2 -8 75.59 12.50
0 -2 -8 74.59 12.60
0 -3 -1 1.30 0.90
0 3 -1 0.50 0.90
0 3 -1 0.50 0.90
0 -3 -1 0.30 1.10
0 3 -3 -1.50 2.50
0 -3 -3 0.20 2.40
0 -3 -5 1.50 4.40
0 3 -5 -2.70 4.50
0 -3 -7 4.20 7.10
0 3 -7 4.10 7.40
0 4 0 314.67 22.90
0 -4 0 274.87 22.90
0 4 -2 961.30 76.29
0 -4 -2 987.80 76.19
0 -4 -2 989.30 76.49
0 -4 -4 325.87 26.10
0 4 -4 308.27 26.10
0 -4 -6 108.99 12.70
0 4 -6 104.79 12.80
0 4 -8 55.89 11.20
0 -4 -8 48.60 11.20
0 -5 -1 0.40 1.20
0 5 -1 0.20 1.10
0 5 -1 -0.90 1.00
0 -5 -1 0.80 0.90
0 -5 -3 0.30 2.90
0 -5 -3 2.10 2.40
0 5 -3 -1.20 2.70
0 5 -5 -4.90 4.60
0 -5 -5 0.60 4.30
0 5 -7 -5.60 6.70
0 -5 -7 -1.90 7.00
0 -6 0 148.39 11.30
0 -6 0 127.19 11.10
0 6 0 150.68 11.40
0 6 -2 41.00 4.60
0 -6 -2 38.30 4.40
0 -6 -2 44.80 4.90
0 -6 -4 182.38 15.80
0 6 -4 179.88 15.90
0 6 -6 119.99 13.40
0 -6 -6 109.59 12.90
0 -6 -8 18.60 9.10
0 6 -8 18.30 8.90
0 -7 -1 -1.50 1.30
0 -7 -1 -1.20 1.00
0 7 -1 1.00 1.60
0 7 1 0.20 1.30
0 7 -1 -0.70 1.10
0 -7 -3 -3.40 2.30
0 -7 -3 -1.70 2.90
0 7 -3 -2.70 2.60
0 -7 -5 -1.80 4.20
0 7 -5 -2.20 4.60
0 -7 -7 -3.10 6.70
0 7 -7 4.30 7.40
0 -8 0 70.49 6.40
0 8 0 82.29 6.60
0 -8 0 71.59 6.20
0 -8 -2 248.28 19.30
0 8 -2 228.88 19.10
0 -8 -2 241.18 19.60
0 8 -2 239.88 19.40
0 -8 -4 42.60 6.30
0 8 -4 57.69 7.10
0 -8 -6 64.39 9.40
0 8 -6 60.79 9.80
0 8 -8 6.30 8.50
0 -8 -8 -1.10 8.30
0 -9 -1 -1.60 1.60
0 9 -1 0.40 2.00
0 -9 -1 -1.00 1.20
0 9 -1 -0.40 1.30
0 9 1 1.90 1.70
0 9 -3 -1.40 2.70
0 -9 -3 -2.10 2.40
0 -9 -3 -0.10 3.10
0 9 -5 -1.40 4.80
0 -9 -5 0.10 4.30
0 -9 -7 -2.80 6.90
0 9 -7 -1.80 6.80
0 -10 0 253.77 20.30
0 -10 0 253.07 20.40
0 10 0 263.77 20.50
0 10 -2 117.29 10.80
0 -10 -2 128.29 10.60
0 -10 -2 135.09 11.20
0 10 -2 123.99 10.60
0 10 -4 27.50 5.30
0 -10 -4 16.40 4.40
0 -10 -4 24.90 5.70
0 10 -6 4.60 6.40
0 -10 -6 14.90 6.30
0 -10 -8 -1.10 8.40
0 10 -8 -4.20 8.20
0 11 -1 1.20 2.30
0 11 1 -2.90 2.00
0 -11 -1 1.40 1.80
0 11 -1 0.00 1.40
0 -11 -1 0.10 1.20
0 11 -3 -1.10 2.30
0 -11 -3 -1.40 2.50
0 -11 -3 1.10 3.20
0 11 -3 -3.20 2.80
0 -11 -5 -7.70 4.10
0 11 -5 -2.40 4.90
0 -11 -7 1.60 7.20
0 11 -7 -5.00 7.00
0 -12 0 272.47 22.10
0 12 0 279.07 22.20
0 -12 0 281.27 22.00
0 12 -2 412.26 32.00
0 12 2 360.86 31.80
0 12 -2 418.66 31.90
0 -12 -2 414.86 31.90
0 -12 -2 415.76 32.40
0 -12 -4 337.67 26.30
0 -12 -4 306.27 26.80
0 12 -4 309.87 26.30
0 -12 -6 81.79 10.90
0 12 -6 79.79 11.00
0 -12 -8 32.50 10.50
0 12 -8 21.20 9.70
0 13 -1 2.40 1.70
0 -13 -1 1.20 2.00
0 13 -1 -2.30 2.50
0 13 1 1.30 2.40
0 -13 -1 -0.30 1.40
0 -13 -3 -0.10 3.40
0 13 -3 1.00 2.60
0 13 -3 -0.40 3.10
0 -13 -3 -1.30 2.50
0 -13 -5 -0.80 4.50
0 13 -5 -3.60 5.00
0 -13 -7 2.40 7.30
0 13 -7 -3.80 7.50
0 -14 0 972.40 75.29
0 -14 0 963.40 75.49
0 14 0 972.50 75.59
0 -14 -2 1043.00 80.89
0 14 2 1002.30 80.39
0 -14 -2 1058.19 80.39
0 14 -2 1050.99 80.49
0 14 -2 1009.80 80.49
0 14 -4 352.96 28.30
0 -14 -4 346.37 28.10
0 -14 -4 323.77 28.70
0 14 -4 345.97 27.50
0 -14 -6 114.29 13.50
0 14 -6 127.59 14.10
0 -14 -8 53.49 11.50
0 14 -8 39.60 10.90
0 15 -1 -1.40 1.80
0 15 -1 0.00 2.80
0 -15 -1 -0.60 1.60
0 15 1 0.00 2.90
0 -15 -1 -0.90 2.20
0 15 -3 0.40 3.30
0 -15 -3 -4.80 3.30
0 -15 -3 1.30 2.80
0 15 -3 0.10 3.00
0 15 -5 -3.60 5.00
0 -15 -5 -2.10 4.60
0 15 -7 1.90 7.90
0 -15 -7 -2.90 6.90
0 16 0 820.82 66.49
0 -16 0 847.32 66.49
0 -16 0 877.91 66.19
0 -16 -2 1271.27 100.89
0 16 -2 1322.67 100.49
0 -16 -2 1327.47 100.29
0 16 -2 1267.87 100.39
0 16 2 1263.17 100.39
0 16 -4 717.23 57.99
0 -16 -4 749.92 57.89
0 -16 -4 728.53 58.69
0 16 -4 727.93 57.39
0 16 -6 156.18 16.90
0 -16 -6 169.38 16.70
0 16 -8 60.49 12.30
0 -16 -8 62.09 11.80
0 17 1 -3.10 3.10
0 17 -1 -0.30 3.20
0 -17 1 1.10 2.10
0 -17 -1 -0.70 1.80
0 -17 -1 -0.60 2.40
0 17 -3 -1.90 3.50
0 -17 -3 0.10 2.70
0 17 3 -2.00 3.30
0 17 -3 -6.20 3.00
0 -17 -3 -0.40 3.90
0 17 -5 0.50 5.40
0 -17 -5 5.30 6.00
0 -17 -5 1.30 4.90
0 17 -7 -2.20 7.90
0 -17 -7 1.00 7.10
0 18 0 935.21 75.69
0 -18 0 969.10 75.59
0 -18 0 995.10 75.39
0 -18 -2 1624.84 125.79
0 18 -2 1597.84 125.09
0 -18 -2 1648.14 125.09
0 18 2 1530.95 125.19
0 18 -2 1648.24 125.29
0 18 -4 317.57 26.30
0 18 -4 325.37 25.80
0 -18 -4 312.57 27.00
0 -18 -4 302.37 26.00
0 -18 -6 203.38 19.30
0 18 -6 197.48 19.60
0 18 -8 42.60 11.60
0 -18 -8 63.09 11.50
0 -19 1 3.60 2.50
0 -19 -1 -0.20 2.00
0 19 1 -2.40 3.40
0 -19 -1 3.30 2.90
0 19 -1 3.20 3.60
0 19 -3 1.60 3.70
0 19 3 -5.40 3.70
0 -19 -3 0.50 2.80
0 -19 -3 0.10 4.00
0 19 -3 -1.00 3.60
0 -19 -5 -10.30 5.30
0 19 -5 -4.20 5.70
0 -19 -5 -1.40 4.80
0 19 -7 -4.00 7.70
0 -19 -7 -4.80 7.20
0 20 0 801.42 64.79
0 -20 0 845.82 64.69
0 -20 0 827.82 64.39
0 -20 -2 320.07 26.00
0 20 2 282.67 25.60
0 20 -2 346.77 25.80
0 -20 -2 322.07 25.10
0 20 -2 296.07 25.20
0 -20 -4 759.32 60.59
0 20 -4 755.02 59.29
0 -20 -4 745.13 59.49
0 20 -4 746.83 59.69
0 20 -6 125.19 14.90
0 -20 -6 122.49 14.30
0 20 -8 33.90 11.00
0 -20 -8 48.10 11.10
0 21 -1 -2.00 3.90
0 -21 -1 -1.70 2.90
0 -21 1 1.00 2.70
0 21 1 0.10 3.80
0 -21 -1 0.00 2.30
0 21 -3 -1.20 4.00
0 21 -3 0.60 3.90
0 -21 -3 2.70 4.20
0 -21 -3 -0.20 3.00
0 21 3 -4.20 4.20
0 -21 -5 -3.20 5.90
0 21 -5 -0.30 6.10
0 -21 -5 7.90 5.40
0 21 -7 2.10 8.40
0 -21 -7 -7.10 7.30
0 22 0 411.36 33.50
0 -22 0 419.06 33.30
0 -22 0 416.66 33.00
0 22 -2 145.19 12.90
0 -22 -2 146.79 13.70
0 22 -2 152.98 14.00
0 -22 -2 151.88 12.50
0 22 2 122.99 13.60
0 -22 -4 175.98 17.80
0 22 -4 166.78 16.50
0 22 -4 197.18 16.40
0 -22 -4 182.38 16.30
0 22 -6 71.39 11.30
0 -22 -6 84.69 11.30
0 22 -8 6.90 9.90
0 -22 -8 3.70 9.20
0 -23 1 3.60 3.50
0 -23 -1 -3.80 3.00
0 -23 -1 -3.40 2.50
0 -23 1 -0.90 3.00
0 23 -1 -4.70 4.10
0 23 1 1.40 4.00
0 23 3 -8.50 4.70
0 -23 -3 -1.20 3.00
0 -23 -3 -1.50 4.40
0 23 -3 1.90 4.20
0 23 -3 0.10 4.50
0 -23 -5 -2.00 5.30
0 23 -5 5.50 5.30
0 23 -5 1.30 6.20
0 -23 -5 5.80 7.00
0 23 -7 1.50 8.60
0 -23 -7 -4.70 7.40
0 -24 0 144.19 12.70
0 24 0 154.98 13.70
0 -24 0 142.59 12.90
0 -24 -2 65.19 7.10
0 24 2 70.19 8.40
0 24 -2 74.99 8.70
0 -24 -2 64.79 8.80
0 24 -4 44.00 7.80
0 -24 -4 55.49 9.20
0 24 4 52.09 7.80
0 24 -4 47.90 7.30
0 -24 -4 43.00 6.90
0 -24 -6 24.10 8.00
0 24 -6 38.70 9.50
0 24 -8 5.60 10.20
0 -24 -8 1.80 8.80
0 -25 1 0.10 3.90
0 25 -1 1.60 4.90
0 -25 -1 -7.50 3.30
0 -25 1 0.40 3.50
0 25 1 -1.90 4.70
0 -25 -1 -0.60 2.90
0 25 -3 6.60 4.60
0 -25 -3 2.00 3.50
0 -25 -3 -0.50 4.90
0 25 3 -0.50 5.10
0 25 -3 -1.20 4.90
0 25 -5 4.40 6.80
0 -25 -5 -1.30 7.20
0 25 -5 1.90 5.90
0 -25 -5 -3.40 5.30
0 25 -7 0.00 9.10
0 -25 -7 8.80 8.00
0 -26 0 9.40 4.00
0 26 0 11.00 4.90
0 -26 0 3.40 3.60
0 -26 -2 37.70 7.10
0 -26 2 42.30 5.70
0 -26 -2 37.90 5.30
0 26 2 38.00 6.80
0 26 -2 37.60 7.10
0 -26 -4 53.89 7.30
0 26 -4 34.50 7.90
0 26 -4 44.20 7.80
0 -26 -4 50.69 9.70
0 26 4 45.00 8.00
0 26 -6 21.40 8.70
0 -26 -6 18.70 7.70
0 27 -1 -2.00 4.90
0 27 1 2.60 4.80
0 -27 -1 -7.90 2.90
0 -27 -1 3.80 4.00
0 -27 1 1.50 4.10
0 -27 1 2.60 3.90
0 27 -3 -0.10 5.40
0 27 -3 2.50 4.70
0 -27 -3 -0.60 3.50
0 27 3 -6.60 5.40
0 -27 -3 3.80 5.20
0 27 -5 13.00 7.10
0 -27 -5 11.10 8.20
0 27 -5 -7.80 6.20
0 -27 -5 -11.40 5.30
0 -27 -7 -2.80 7.80
0 27 -7 5.60 9.50
0 -28 0 33.50 5.60
0 28 0 34.30 6.60
0 -28 0 38.00 5.60
0 -28 -2 88.29 11.50
0 28 -2 80.79 11.30
0 28 2 107.49 11.20
0 -28 -2 97.59 9.80
0 -28 2 123.29 10.10
0 28 -4 43.80 8.00
0 28 4 31.80 7.80
0 -28 -4 37.90 9.30
0 28 -4 34.20 7.70
0 -28 -4 36.10 6.70
0 28 -6 40.60 9.90
0 -28 -6 25.50 8.30
0 -28 -6 23.20 10.90
0 -29 1 -7.20 4.10
0 -29 1 0.30 4.30
0 -29 -1 2.70 4.10
0 -29 -1 -6.30 3.30
0 29 -1 -0.20 5.40
0 29 1 11.00 5.50
0 -29 -3 3.90 4.10
0 29 -3 1.10 6.00
0 29 3 0.70 6.00
0 -29 -3 -2.10 5.60
0 29 -5 -7.40 6.70
0 29 -5 -4.40 7.40
0 -29 -5 -3.10 5.90
0 -29 -5 -6.50 8.00
0 -29 -7 8.00 8.50
0 29 -7 -4.90 9.80
0 30 0 253.47 23.20
0 -30 0 269.47 22.40
0 -30 0 269.57 22.20
0 30 2 151.88 16.60
0 30 -2 162.48 17.10
0 -30 -2 167.38 15.10
0 -30 2 213.28 15.50
0 -30 -2 154.38 16.80
0 -30 -4 101.29 12.00
0 30 4 104.99 12.50
0 30 -4 108.09 12.90
0 30 -4 109.49 13.00
0 -30 -4 123.49 15.20
0 -30 -6 142.19 16.10
0 30 -6 126.29 16.40
0 -30 -6 140.79 19.10
0 30 -6 146.99 17.40
0 -31 1 0.50 4.50
0 -31 -1 -4.30 4.20
0 -31 1 -4.80 4.60
0 31 1 1.00 5.40
0 31 -1 2.70 5.70
0 -31 -1 -1.70 3.60
0 31 3 -0.90 6.30
0 -31 3 -5.20 5.60
0 -31 -3 -3.20 4.00
0 -31 -3 4.30 6.10
0 31 -3 -4.20 6.30
0 31 -5 11.90 7.80
0 -31 -5 -9.10 8.60
0 31 5 8.10 7.40
0 -31 -5 1.90 6.20
0 31 -5 3.70 7.80
0 31 -7 -5.80 9.90
0 -31 -7 -4.70 8.30
0 32 0 955.00 74.69
0 -32 0 931.51 74.29
0 -32 0 942.91 73.89
0 -32 -2 270.77 22.50
0 32 2 289.17 23.90
0 32 -2 275.47 24.30
0 -32 -2 256.27 24.20
0 32 -4 194.68 18.80
0 32 -4 186.08 17.60
0 -32 -4 170.08 19.40
0 -32 -4 168.38 16.70
0 32 4 166.58 17.90
0 32 -6 55.79 12.10
0 -32 -6 69.39 15.00
0 -32 -6 72.89 11.20
0 32 -6 73.69 13.60
0 -33 -1 -1.90 4.70
0 -33 1 -2.50 4.70
0 33 -1 7.90 6.10
0 33 1 1.20 5.80
0 -33 -1 2.50 4.10
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9 -4 -2 21.40 8.50
-9 4 -2 8.90 13.00
-9 -4 -2 29.40 14.20
9 -4 2 0.60 10.20
9 4 -2 12.40 7.40
-9 5 -1 32.40 13.50
9 -5 -1 41.00 9.30
-9 -5 -1 64.79 15.60
9 -5 1 28.10 10.40
9 5 -1 27.20 9.90
-9 -5 -1 24.00 18.40
9 5 -1 34.40 12.50
-9 5 1 38.90 12.80
9 -5 -3 47.70 10.00
-9 5 -3 34.50 14.30
9 -5 3 15.20 12.30
9 5 -3 49.30 9.90
-9 -5 -3 44.30 14.80
9 -6 0 6.90 8.50
-9 6 0 -8.10 11.40
-9 -6 0 20.50 12.30
9 -6 -2 13.50 8.30
-9 6 -2 4.00 11.90
9 -6 2 -2.70 10.70
-9 -6 -2 -10.90 13.20
9 6 -2 2.20 7.10
9 -7 -1 69.29 11.50
-9 7 -1 93.69 15.60
-9 7 1 87.99 15.00
9 7 -1 91.99 14.60
9 -7 1 80.39 12.80
-9 -7 -1 34.80 13.20
-9 7 -3 87.09 16.50
9 -7 -3 69.39 12.20
9 7 -3 76.79 12.10
9 -7 3 69.99 15.00
-9 8 0 15.60 12.00
-9 -8 0 20.30 12.60
9 8 0 16.30 12.80
9 -8 0 -0.70 9.10
-9 8 -2 6.40 11.90
9 -8 -2 -1.60 7.80
9 -8 2 -16.40 10.90
-9 9 -1 91.39 15.90
9 -9 -1 71.39 12.10
9 9 1 112.39 17.40
-9 -9 -1 59.49 14.60
9 9 -1 80.99 14.50
9 -9 1 89.59 13.80
-9 9 1 79.89 14.90
-9 9 -3 73.89 15.30
9 -9 -3 71.29 12.10
9 -9 3 50.19 14.60
9 -10 0 -13.40 8.70
9 10 0 -20.80 11.50
-9 -10 0 9.00 12.20
-9 10 0 5.20 11.50
9 10 2 4.90 13.50
9 -10 -2 -3.80 7.90
-9 10 -2 -5.70 11.80
9 10 -2 -1.00 12.20
9 -10 2 -15.90 11.20
-9 -10 -2 -16.10 10.80
-9 11 -1 135.09 18.80
9 11 1 126.29 18.90
9 -11 -1 111.99 15.20
9 11 -1 134.59 17.50
-9 11 1 136.69 17.50
9 -11 1 96.99 16.00
-9 -11 -1 120.99 18.10
-9 11 -3 44.40 13.70
9 11 3 15.30 15.70
9 -11 -3 17.90 9.20
9 -11 3 13.60 13.00
-9 12 0 7.40 11.80
-9 -12 0 2.60 12.70
9 12 0 4.60 12.40
9 -12 0 1.90 9.50
9 -12 -2 8.70 8.70
-9 12 -2 -4.40 11.90
9 12 2 1.50 13.50
9 -12 2 -17.40 11.50
9 12 -2 18.70 12.60
-9 -12 -2 -19.00 10.40
9 -13 -1 46.60 11.40
-9 13 -1 56.09 14.30
9 13 1 70.99 15.00
9 13 -1 79.99 14.30
-9 13 1 57.19 13.10
-9 -13 -1 52.79 14.10
9 -13 1 50.09 13.10
9 13 3 9.20 15.20
9 -13 -3 25.60 9.80
-9 13 -3 30.70 13.60
9 -13 3 37.50 13.50
-9 -14 0 15.90 13.20
9 -14 0 9.80 10.30
-9 14 0 2.20 11.40
9 14 0 21.30 12.90
-9 14 -2 9.30 12.10
9 -14 -2 -4.20 8.40
9 14 2 14.80 14.80
-9 -14 -2 -25.90 10.50
9 14 -2 -1.40 11.70
9 -14 2 -19.70 11.60
9 15 1 31.90 13.40
9 -15 -1 -4.30 9.00
-9 15 -1 10.50 11.70
-9 -15 -1 10.20 12.30
9 -15 1 -3.10 11.10
-9 15 1 3.20 11.10
9 15 -1 0.30 11.20
9 15 3 42.90 16.70
9 -15 -3 0.60 8.80
-9 15 -3 -2.30 11.70
9 -15 3 -18.00 12.80
-9 -15 -3 17.50 13.00
-9 16 0 26.70 12.10
9 16 0 -2.50 12.10
9 -16 0 0.10 10.40
-9 -16 0 12.50 13.10
9 -16 -2 32.90 10.90
-9 16 -2 38.90 13.00
9 16 2 36.60 14.80
-9 -16 -2 1.70 12.00
9 16 -2 45.10 14.20
9 -16 2 11.70 13.00
9 -17 -1 -2.50 9.90
-9 17 -1 -2.00 11.70
9 17 1 22.10 13.60
-9 17 1 7.00 11.40
9 -17 1 -2.90 11.10
-9 -17 -1 11.60 12.40
9 17 -1 -5.20 10.90
9 17 3 -2.70 14.40
9 -17 -3 -2.30 9.30
-9 17 -3 -12.40 11.60
9 -17 3 -12.00 13.20
-9 -17 -3 3.30 12.20
9 -18 0 14.50 11.70
-9 -18 0 27.80 14.00
9 18 0 20.90 13.20
-9 18 0 14.00 12.20
-9 18 -2 19.40 12.60
9 18 2 16.80 14.20
9 -18 -2 20.20 10.50
9 -18 2 -13.10 12.30
-9 -18 -2 23.90 12.90
9 18 -2 14.90 12.20
9 -19 -1 13.20 11.20
-9 -19 1 18.20 13.50
-9 19 -1 7.50 12.30
9 19 1 12.90 13.20
-9 -19 -1 29.60 13.90
9 -19 1 7.30 11.90
-9 19 1 30.70 12.10
9 19 -1 21.60 12.20
-9 -20 0 27.30 13.50
9 -20 0 -7.40 11.70
-9 20 0 20.70 12.30
9 20 0 8.30 12.20
9 -20 -2 5.30 10.40
-9 20 -2 28.20 12.80
9 20 2 23.80 14.70
-9 -20 -2 27.50 13.60
9 -20 2 6.20 13.00
9 20 -2 -8.50 11.50
9 21 1 25.40 13.10
-9 21 -1 20.60 12.70
-9 -21 1 15.10 13.50
9 -21 -1 20.80 11.90
-9 21 1 24.30 12.10
9 -21 1 7.40 12.70
-9 -21 -1 58.19 14.80
9 21 -1 22.90 12.50
-9 22 0 -1.30 11.40
-9 -22 0 22.70 14.10
9 22 0 9.30 12.60
9 -22 0 5.30 12.20
-9 22 -2 19.30 12.80
9 -22 -2 -0.40 10.40
9 22 2 9.70 13.60
-9 -22 -2 12.00 13.40
9 -22 2 -15.40 12.60
9 22 -2 72.59 14.50
-9 -23 1 60.49 15.60
9 23 1 71.19 15.80
-9 23 -1 63.99 15.10
9 -23 -1 65.59 15.10
-9 23 1 56.69 13.90
9 23 -1 66.59 14.60
-9 -23 -1 76.49 16.10
9 -23 1 30.00 14.40
-9 -24 0 18.80 13.40
-9 24 0 -5.40 11.60
9 24 0 12.70 12.90
9 -24 0 -12.00 12.10
9 -24 -2 -2.00 10.70
9 24 2 -3.80 13.60
-9 24 -2 -4.20 12.30
9 24 -2 -22.50 11.90
-9 -24 -2 6.70 13.80
9 -24 2 -12.00 12.80
9 -25 -1 36.40 13.60
-9 25 -1 32.90 13.40
9 25 1 26.10 14.10
-9 -25 1 45.10 14.80
9 25 -1 45.80 14.10
9 -25 1 3.10 12.80
-9 25 1 31.30 12.40
-9 -25 -1 51.79 14.60
-9 -26 0 2.90 13.40
9 -26 0 -19.10 11.40
-9 26 0 -6.20 11.70
9 26 0 -1.50 12.10
9 27 1 54.99 14.80
-9 27 -1 29.90 13.50
9 -27 -1 13.10 13.20
9 -27 1 11.80 13.50
9 27 -1 28.70 13.60
-9 27 1 19.10 12.50
9 28 0 -4.40 13.00
10 -1 -1 0.70 9.80
-10 1 -1 -4.00 14.20
-10 -1 -1 10.40 14.20
-10 2 0 73.89 16.90
-10 3 -1 25.40 15.20
10 -3 -1 -7.80 8.10
10 3 -1 6.50 13.10
-10 4 0 13.90 14.20
10 -4 0 2.00 8.50
-10 5 -1 35.90 15.40
10 -5 -1 -14.10 8.00
-10 5 1 -6.30 12.70
10 5 -1 -13.60 12.70
-10 6 0 9.70 13.80
10 -6 0 5.40 9.10
10 6 0 10.30 14.50
-10 7 -1 9.00 13.30
10 7 1 26.70 15.90
-10 7 1 5.90 13.50
10 7 -1 -10.10 12.90
10 -8 0 -2.20 9.00
10 8 0 -3.10 14.00
-10 8 0 20.10 13.70
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 97998
_shelx_res_file
;
TITL 217_d.res in Abm2
REM Old TITL
REM SHELXT solution in Abm2
REM R1 0.105, Rweak 0.016, Alpha 0.104, Orientation as input
REM Flack x = 0.344 ( 0.022 ) from Parsons' quotients
REM Formula found by SHELXT: C23 Br2 O3
CELL 0.71073 7.0976 42.7178 6.1349 90 90 90
ZERR 4 0.0034 0.0197 0.003 0 0 0
LATT -5
SYMM -X,-Y,+Z
SYMM +X,0.5-Y,+Z
SYMM -X,0.5+Y,+Z
SFAC C H Br O
UNIT 92 56 8 4
L.S. 10
PLAN 20
TEMP -153.15
BOND $H
LIST 6
fmap 2
ACTA
OMIT 0 2 0
REM
REM
REM
WGHT 0.100000
FVAR 0.17981
BR2 3 0.200373 0.529317 -0.275975 11.00000 0.02442 0.02260 =
0.02908 -0.00849 -0.00134 -0.00207
C20 1 0.175753 0.594168 -0.179932 11.00000 0.01540 0.02872 =
0.01932 0.00229 -0.00270 -0.00383
AFIX 43
H20 2 0.124980 0.596260 -0.322468 11.00000 -1.20000
AFIX 0
C19 1 0.228723 0.564884 -0.097835 11.00000 0.01537 0.02134 =
0.01727 -0.00049 0.00694 0.00293
C9 1 0.283911 0.644090 0.303742 11.00000 0.01751 0.02387 =
0.02301 0.00254 0.00410 -0.00040
C16 1 0.269396 0.617301 0.165817 11.00000 0.01447 0.02225 =
0.01770 -0.00030 0.00676 -0.00721
C21 1 0.200114 0.620208 -0.045075 11.00000 0.01496 0.01951 =
0.02393 0.00349 0.00470 -0.00118
AFIX 43
H21 2 0.168551 0.640393 -0.098848 11.00000 -1.20000
AFIX 0
C17 1 0.322381 0.587492 0.243627 11.00000 0.01650 0.02464 =
0.01176 0.00036 -0.00071 0.00103
AFIX 43
H17 2 0.373720 0.585341 0.385848 11.00000 -1.20000
AFIX 0
C7 1 0.316947 0.692921 0.557395 11.00000 0.01867 0.02593 =
0.01275 -0.00174 0.00243 0.00054
AFIX 43
H7 2 0.367774 0.690499 0.699652 11.00000 -1.20000
AFIX 0
C18 1 0.299300 0.561130 0.111373 11.00000 0.01948 0.01927 =
0.01889 -0.00037 0.00041 -0.00135
AFIX 43
H18 2 0.331514 0.540913 0.164049 11.00000 -1.20000
AFIX 0
C8 1 0.295328 0.666107 0.426921 11.00000 0.02598 0.02311 =
0.02653 0.00180 -0.00073 0.00086
O1 4 0.369771 0.750000 0.815141 10.50000 0.01738 0.03259 =
0.01479 0.00000 -0.00143 0.00000
C5 1 0.308979 0.750000 0.626112 10.50000 0.00735 0.02001 =
0.01399 0.00000 0.00469 0.00000
C6 1 0.269120 0.721859 0.490522 11.00000 0.01597 0.02742 =
0.00971 0.00096 -0.00157 -0.00566
C23 1 0.189124 0.731784 0.274411 11.00000 0.03948 0.03150 =
0.00728 -0.00013 -0.00515 -0.00199
AFIX 23
H23A 2 0.059327 0.723686 0.256749 11.00000 -1.20000
H23B 2 0.267639 0.723685 0.153540 11.00000 -1.20000
AFIX 0
HKLF 4
REM 217_d.res in Abm2
REM R1 = 0.0635 for 1928 Fo > 4sig(Fo) and 0.0966 for all 2642 data
REM 121 parameters refined using 1 restraints
END
WGHT 0.0717 2.8343
REM Highest difference peak 1.927, deepest hole -1.090, 1-sigma level 0.159
Q1 1 0.1984 0.5482 -0.2719 11.00000 0.05 1.93
Q2 1 0.1997 0.5095 -0.2672 11.00000 0.05 1.84
Q3 1 0.2084 0.5676 -0.2611 11.00000 0.05 0.72
Q4 1 0.2822 0.5977 0.1614 11.00000 0.05 0.64
Q5 1 0.3178 0.5442 -0.1852 11.00000 0.05 0.61
Q6 1 0.2110 0.6124 -0.1361 11.00000 0.05 0.60
Q7 1 0.1691 0.4911 -0.2687 11.00000 0.05 0.59
Q8 1 0.2102 0.6125 -0.4222 11.00000 0.05 0.58
Q9 1 0.2238 0.5804 -0.1389 11.00000 0.05 0.55
Q10 1 0.3239 0.5114 -0.3311 11.00000 0.05 0.55
Q11 1 0.2341 0.6482 -0.2822 11.00000 0.05 0.54
Q12 1 0.3297 0.5142 -0.1912 11.00000 0.05 0.53
Q13 1 0.3051 0.5710 0.2595 11.00000 0.05 0.49
Q14 1 0.3015 0.6841 0.4236 11.00000 0.05 0.48
Q15 1 0.0542 0.5196 -0.3593 11.00000 0.05 0.45
Q16 1 0.1639 0.6481 -0.2833 11.00000 0.05 0.45
Q17 1 0.3147 0.5827 0.1574 11.00000 0.05 0.45
Q18 1 0.0667 0.5127 -0.2747 11.00000 0.05 0.45
Q19 1 0.3704 0.5102 0.1365 11.00000 0.05 0.45
Q20 1 0.2230 0.6532 0.0953 11.00000 0.05 0.44
;
_shelx_res_checksum 77305
_shelxl_version_number 2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, z'
'-x, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1, z+1/2'
'-x, y+1, 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
Br Br2 0.20037(10) 0.52932(2) -0.27597(19) 0.0254(2) Uani d 1 . .
C C20 0.1758(11) 0.5942(2) -0.1799(16) 0.0211(17) Uani d 1 . .
H H20 0.1250 0.5963 -0.3225 0.025 Uiso calc 1 . .
C C19 0.2287(12) 0.56488(19) -0.0978(15) 0.0180(16) Uani d 1 . .
C C9 0.2839(11) 0.6441(2) 0.3037(16) 0.0215(17) Uani d 1 . .
C C16 0.2694(11) 0.61730(19) 0.1658(13) 0.0181(17) Uani d 1 . .
C C21 0.2001(11) 0.62021(19) -0.0451(15) 0.0195(16) Uani d 1 . .
H H21 0.1686 0.6404 -0.0988 0.023 Uiso calc 1 . .
C C17 0.3224(9) 0.58749(17) 0.2436(18) 0.0176(15) Uani d 1 . .
H H17 0.3737 0.5853 0.3858 0.021 Uiso calc 1 . .
C C7 0.3169(12) 0.6929(2) 0.5574(14) 0.0191(16) Uani d 1 . .
H H7 0.3678 0.6905 0.6997 0.023 Uiso calc 1 . .
C C18 0.2993(11) 0.56113(19) 0.1114(14) 0.0192(15) Uani d 1 . .
H H18 0.3315 0.5409 0.1640 0.023 Uiso calc 1 . .
C C8 0.2953(13) 0.6661(2) 0.4269(17) 0.0252(19) Uani d 1 . .
O O1 0.3698(13) 0.7500 0.8151(15) 0.022(2) Uani d 1 . .
C C5 0.3090(15) 0.7500 0.626(2) 0.014(2) Uani d 1 . .
C C6 0.2691(11) 0.7219(2) 0.4905(15) 0.0177(15) Uani d 1 . .
C C23 0.1891(13) 0.7318(2) 0.2744(12) 0.026(2) Uani d 1 . .
H H23A 0.0593 0.7237 0.2567 0.031 Uiso calc 1 . .
H H23B 0.2676 0.7237 0.1535 0.031 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
Br2 0.0244(4) 0.0226(4) 0.0291(4) -0.0021(3) -0.0013(6) -0.0085(5)
C20 0.015(4) 0.029(4) 0.019(4) -0.004(3) -0.003(3) 0.002(3)
C19 0.015(4) 0.021(4) 0.017(4) 0.003(3) 0.007(3) 0.000(3)
C9 0.018(4) 0.024(4) 0.023(4) 0.000(3) 0.004(3) 0.003(3)
C16 0.014(3) 0.022(4) 0.018(4) -0.007(3) 0.007(3) 0.000(3)
C21 0.015(4) 0.020(4) 0.024(4) -0.001(3) 0.005(3) 0.003(3)
C17 0.016(3) 0.025(3) 0.012(4) 0.001(2) -0.001(3) 0.000(4)
C7 0.019(4) 0.026(4) 0.013(4) 0.001(3) 0.002(3) -0.002(3)
C18 0.019(4) 0.019(3) 0.019(4) -0.001(3) 0.000(3) 0.000(3)
C8 0.026(5) 0.023(4) 0.027(5) 0.001(4) -0.001(4) 0.002(3)
O1 0.017(5) 0.033(5) 0.015(4) 0.000 -0.001(4) 0.000
C5 0.007(5) 0.020(5) 0.014(5) 0.000 0.005(4) 0.000
C6 0.016(3) 0.027(4) 0.010(4) -0.006(3) -0.002(3) 0.001(3)
C23 0.039(5) 0.032(4) 0.007(4) -0.002(4) -0.005(3) 0.000(3)
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'
Br Br -0.2901 2.4595 '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
C19 C20 H20 . . 121.1
C21 C20 H20 . . 121.1
C21 C20 C19 . . 117.7(8)
C20 C19 Br2 . . 118.9(7)
C18 C19 Br2 . . 118.9(6)
C18 C19 C20 . . 122.2(8)
C8 C9 C16 . . 177.7(10)
C21 C16 C9 . . 120.4(8)
C21 C16 C17 . . 119.3(8)
C17 C16 C9 . . 120.3(8)
C20 C21 H21 . . 119.2
C16 C21 C20 . . 121.6(8)
C16 C21 H21 . . 119.2
C16 C17 H17 . . 120.0
C18 C17 C16 . . 120.0(9)
C18 C17 H17 . . 120.0
C8 C7 H7 . . 118.4
C6 C7 H7 . . 118.4
C6 C7 C8 . . 123.2(8)
C19 C18 C17 . . 119.1(8)
C19 C18 H18 . . 120.4
C17 C18 H18 . . 120.4
C9 C8 C7 . . 175.5(10)
O1 C5 C6 . 3_565 126.1(6)
O1 C5 C6 . . 126.1(6)
C6 C5 C6 . 3_565 107.7(11)
C7 C6 C5 . . 121.6(8)
C7 C6 C23 . . 128.5(8)
C5 C6 C23 . . 109.7(8)
C6 C23 C23 . 3_565 106.4(5)
C6 C23 H23A . . 110.5
C6 C23 H23B . . 110.5
C23 C23 H23A 3_565 . 110.5
C23 C23 H23B 3_565 . 110.5
H23A C23 H23B . . 108.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Br2 C19 . 1.882(8)
C20 H20 . 0.9500
C20 C19 . 1.400(12)
C20 C21 . 1.397(12)
C19 C18 . 1.387(12)
C9 C16 . 1.427(12)
C9 C8 . 1.209(13)
C16 C21 . 1.390(12)
C16 C17 . 1.411(11)
C21 H21 . 0.9500
C17 H17 . 0.9500
C17 C18 . 1.398(12)
C7 H7 . 0.9500
C7 C8 . 1.406(12)
C7 C6 . 1.346(12)
C18 H18 . 0.9500
O1 C5 . 1.237(14)
C5 C6 . 1.489(12)
C5 C6 3_565 1.489(12)
C6 C23 . 1.503(12)
C23 C23 3_565 1.556(18)
C23 H23A . 0.9900
C23 H23B . 0.9900
_cod_database_fobs_code 2021674