#------------------------------------------------------------------------------
#$Date: 2018-02-14 10:11:25 +0200 (Wed, 14 Feb 2018) $
#$Revision: 206432 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242383.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_2242383
loop_
_publ_author_name
'Lastovickova, Dominika N.'
'La Scala, John J.'
'Sausa, Rosario C.'
_publ_section_title
;
Synthesis and crystal structures of
(2E)-1,4-bis(4-chlorophenyl)but-2-ene-1,4-dione and
(2E)-1,4-bis(4-bromophenyl)but-2-ene-1,4-dione
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 352
_journal_page_last 356
_journal_paper_doi 10.1107/S205698901800230X
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'C16 H10 Br2 O2'
_chemical_formula_moiety 'C16 H10 Br2 O2'
_chemical_formula_sum 'C16 H10 Br2 O2'
_chemical_formula_weight 394.06
_chemical_name_systematic
;
(2E)-1,4-Bis(4-bromophenyl)but-2-ene-1,4-dione
;
_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'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha 90
_cell_angle_beta 97.827(5)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.4391(7)
_cell_length_b 3.9937(2)
_cell_length_c 12.7244(7)
_cell_measurement_reflns_used 2527
_cell_measurement_temperature 298.00(10)
_cell_measurement_theta_max 26.2050
_cell_measurement_theta_min 2.8490
_cell_volume 726.92(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 298.00(10)
_diffrn_detector_area_resol_mean 8.0945
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Agilent SuperNova, Dualflex, EosS2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0313
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 6231
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.369
_diffrn_reflns_theta_min 2.848
_exptl_absorpt_coefficient_mu 5.573
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.37033
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Bourhis et al., 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.800
_exptl_crystal_description irregular
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.355
_refine_diff_density_min -0.430
_refine_ls_extinction_coef 0.0047(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/4 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 92
_refine_ls_number_reflns 1470
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.078
_refine_ls_R_factor_all 0.0395
_refine_ls_R_factor_gt 0.0292
_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^)+(0.0234P)^2^+0.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0602
_refine_ls_wR_factor_ref 0.0650
_reflns_number_gt 1228
_reflns_number_total 1470
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zl2724sup1.cif
_cod_data_source_block 2
_cod_database_code 2242383
_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_hkl_file
;
-2 0 0 204.75 8.66
-3 0 0 574.41 18.14
-4 0 0 839.86 25.76
4 0 0 837.52 20.00
5 0 0 942.95 23.58
-5 0 0 981.72 30.68
-6 0 0 2281.25 53.82
6 0 0 2249.75 42.62
7 0 0 4058.73 65.81
-7 0 0 3980.80 79.75
8 0 0 1896.98 43.09
-8 0 0 1934.12 54.97
9 0 0 1927.42 45.27
-9 0 0 1904.60 57.14
-10 0 0 370.85 25.40
10 0 0 320.66 18.30
-11 0 0 7.52 4.85
11 0 0 14.63 5.37
12 0 0 246.36 17.80
-12 0 0 248.63 22.80
13 0 0 1711.61 50.18
-13 0 0 1621.39 61.20
-14 0 0 166.78 20.52
14 0 0 174.95 16.29
15 0 0 304.56 22.44
-15 0 0 317.79 28.81
-16 0 0 188.30 23.55
16 0 0 191.62 18.43
-17 0 0 24.47 10.48
17 0 0 27.99 8.52
0 -1 0 -0.55 1.00
0 1 0 -0.24 0.82
0 -1 0 -0.11 0.78
0 1 0 -1.33 1.06
0 -1 0 -0.10 0.67
-1 1 0 275.94 8.85
1 1 0 258.59 9.59
1 -1 0 251.81 8.11
1 1 0 256.69 10.43
1 -1 0 270.44 8.49
-1 -1 0 248.49 9.21
-1 -1 0 263.09 9.62
-1 1 0 270.31 10.39
1 -1 0 269.92 11.21
-1 1 0 265.79 6.63
2 1 0 9632.44 119.50
2 -1 0 9715.96 105.13
2 -1 0 9912.64 106.87
2 1 0 9761.93 109.36
-2 -1 0 9567.84 112.83
-2 -1 0 9999.00 102.78
-2 -1 0 9896.29 107.63
-2 1 0 9480.07 114.61
-3 -1 0 1047.22 22.78
-3 -1 0 1085.73 26.66
3 1 0 1097.17 21.41
3 1 0 1093.09 30.01
-3 1 0 1068.99 27.81
3 -1 0 1069.03 20.79
-4 -1 0 2037.14 42.76
4 -1 0 1894.21 32.59
4 1 0 1907.63 30.93
4 1 0 1895.74 45.48
-4 1 0 1962.57 43.69
-4 -1 0 1998.40 37.82
-5 1 0 1976.90 47.94
-5 -1 0 2017.70 42.67
5 1 0 1937.48 31.58
5 -1 0 2002.67 36.51
6 1 0 122.62 6.77
-6 -1 0 134.86 12.39
-6 1 0 115.16 11.73
-6 -1 0 130.91 10.83
6 -1 0 123.91 8.83
7 -1 0 183.63 11.70
7 1 0 179.97 8.75
-7 -1 0 212.87 16.93
-7 1 0 200.80 16.26
-7 -1 0 192.60 14.19
8 -1 0 16.06 4.31
-8 -1 0 15.03 4.73
-8 1 0 16.85 5.97
8 1 0 19.34 3.31
9 1 0 365.50 14.23
-9 -1 0 374.48 23.07
9 -1 0 405.24 20.04
-9 1 0 357.68 24.46
-10 1 0 669.14 35.23
-10 -1 0 628.31 31.49
10 -1 0 627.36 27.24
10 1 0 625.18 20.36
11 1 0 1790.75 48.52
-11 -1 0 1669.95 54.74
-11 1 0 1695.10 59.53
11 -1 0 1755.91 49.40
12 -1 0 171.49 15.74
12 1 0 179.57 15.19
-12 1 0 169.55 19.60
-12 -1 0 168.99 17.70
-13 1 0 110.36 16.21
13 1 0 95.99 11.90
-13 -1 0 93.70 14.20
13 -1 0 131.77 14.68
14 1 0 39.46 8.34
14 -1 0 45.92 10.11
-14 -1 0 45.19 11.44
-14 1 0 27.09 9.02
15 -1 0 47.06 9.80
15 1 0 32.04 8.34
-15 1 0 35.72 11.02
-15 -1 0 51.60 11.33
16 1 0 13.83 6.52
-16 1 0 13.61 8.75
-16 -1 0 2.43 5.90
16 -1 0 23.38 8.00
-17 1 0 43.10 12.55
17 -1 0 55.62 11.52
-17 -1 0 31.08 9.41
0 -2 0 51.81 5.30
0 2 0 55.16 5.62
0 -2 0 54.14 5.72
0 2 0 51.16 6.46
0 -2 0 55.32 6.52
1 -2 0 21.12 3.31
-1 2 0 21.79 2.37
-1 -2 0 17.69 3.54
1 -2 0 23.76 3.81
-1 2 0 20.51 2.86
1 -2 0 16.47 4.22
1 2 0 20.50 4.23
-1 2 0 23.05 4.48
-1 -2 0 21.90 3.95
1 2 0 15.51 3.49
-1 -2 0 27.05 4.38
2 -2 0 207.09 10.64
-2 2 0 211.05 13.05
-2 2 0 207.52 8.16
2 2 0 190.93 13.33
2 2 0 204.52 11.74
2 -2 0 220.01 13.85
-2 2 0 209.50 9.89
-2 -2 0 207.22 12.28
2 -2 0 215.51 10.28
-2 -2 0 215.95 11.76
-2 -2 0 208.93 11.96
3 2 0 81.69 9.34
-3 -2 0 78.75 6.87
3 2 0 88.27 7.76
-3 2 0 85.35 7.38
3 -2 0 79.43 8.51
3 -2 0 100.35 6.97
-3 -2 0 74.50 7.99
-3 2 0 85.30 8.55
3 -2 0 83.73 6.91
-3 2 0 86.41 4.55
-4 2 0 372.61 17.92
-4 -2 0 389.91 10.67
4 2 0 376.19 21.25
-4 -2 0 381.61 18.90
4 -2 0 364.36 14.68
-4 2 0 362.71 9.35
-4 2 0 387.62 18.27
4 2 0 384.94 15.87
-5 -2 0 121.44 7.28
5 2 0 118.54 8.65
-5 -2 0 112.17 11.39
5 2 0 117.81 12.88
5 -2 0 114.44 8.54
5 -2 0 108.08 10.43
-5 2 0 109.88 10.71
6 2 0 44.55 5.58
-6 -2 0 34.09 4.37
6 -2 0 37.94 5.24
-6 2 0 38.93 7.45
-6 -2 0 48.62 8.19
-7 2 0 21.41 5.72
7 2 0 33.19 5.06
-7 -2 0 22.92 5.83
7 -2 0 26.44 5.07
-7 -2 0 23.41 4.09
8 -2 0 2.13 2.63
-8 -2 0 -0.44 3.21
-8 2 0 -0.62 3.03
8 2 0 3.18 2.43
-8 -2 0 3.42 3.02
9 -2 0 379.90 20.46
-9 2 0 364.80 24.92
-9 -2 0 353.31 19.90
-9 -2 0 429.38 28.03
9 2 0 391.12 16.02
-10 -2 0 1.23 2.93
10 2 0 4.35 2.69
10 -2 0 0.74 2.76
-10 2 0 1.49 3.97
-10 -2 0 -3.04 5.88
11 -2 0 9.73 4.62
11 2 0 14.41 4.26
-11 -2 0 12.58 4.33
-11 2 0 8.62 5.62
12 2 0 12.35 4.15
12 -2 0 9.98 4.95
-13 2 0 1.97 4.93
13 2 0 0.72 3.02
13 -2 0 -2.85 4.41
-14 2 0 6.21 6.31
14 2 0 -0.65 5.06
14 -2 0 -3.34 5.72
15 2 0 10.46 5.87
15 -2 0 -4.51 6.44
-15 2 0 19.42 10.27
16 2 0 24.61 8.21
16 -2 0 25.71 8.53
-16 2 0 28.61 12.20
0 -3 0 -2.45 2.33
0 -3 0 -6.28 4.33
0 -3 0 -4.68 3.00
1 -3 0 67.66 9.06
1 -3 0 96.50 8.99
-1 -3 0 80.38 8.86
-1 -3 0 74.12 9.01
-1 -3 0 84.30 9.02
-1 3 0 76.59 9.76
1 -3 0 95.62 9.05
1 3 0 90.53 9.91
2 3 0 258.90 17.88
2 -3 0 251.77 14.54
2 -3 0 255.18 14.16
-2 -3 0 271.23 16.64
2 -3 0 217.89 16.34
-2 3 0 267.98 18.15
2 3 0 239.88 15.80
-2 -3 0 272.69 16.32
-2 -3 0 260.89 16.57
-3 -3 0 480.39 23.73
3 3 0 471.89 25.95
3 -3 0 438.56 24.01
3 -3 0 459.84 19.96
-3 3 0 479.66 24.39
3 3 0 489.20 22.25
3 -3 0 507.03 19.85
-3 -3 0 507.48 22.11
-3 -3 0 514.42 23.32
-4 -3 0 161.74 12.10
-4 3 0 154.04 14.11
-4 -3 0 171.42 14.60
-4 -3 0 155.18 13.26
4 -3 0 138.82 13.80
4 3 0 155.58 12.46
4 -3 0 143.93 10.90
-5 -3 0 73.89 9.57
-5 3 0 58.29 9.44
-5 -3 0 73.83 10.56
5 -3 0 62.68 9.66
5 3 0 68.35 7.98
5 -3 0 84.19 8.71
6 -3 0 179.67 12.90
-6 3 0 177.82 15.67
6 3 0 191.43 13.25
-6 -3 0 181.43 17.15
6 -3 0 170.32 16.27
-6 -3 0 201.61 16.12
-7 -3 0 155.93 16.87
-7 3 0 134.17 13.81
7 -3 0 144.94 15.44
7 3 0 146.18 11.67
-8 3 0 3.85 4.23
8 -3 0 1.84 4.12
8 3 0 5.71 3.71
-8 -3 0 0.43 4.08
9 3 0 37.77 6.71
-9 3 0 20.18 8.00
-9 -3 0 26.29 8.61
9 -3 0 21.85 7.90
-10 -3 0 222.10 23.38
10 3 0 244.66 14.80
10 -3 0 233.15 22.65
-10 3 0 238.10 22.58
-11 3 0 137.44 17.95
11 3 0 155.55 11.94
-11 -3 0 152.53 21.10
11 -3 0 141.77 18.75
12 -3 0 18.83 8.07
12 3 0 22.02 5.22
-12 3 0 32.18 10.00
13 3 0 25.25 5.77
13 -3 0 13.70 8.36
-13 3 0 3.65 5.92
-14 3 0 5.29 5.75
14 -3 0 0.16 7.40
14 3 0 11.58 4.75
0 4 0 418.45 25.74
0 -4 0 427.20 25.59
-1 -4 0 348.11 22.71
1 -4 0 303.94 21.93
-1 4 0 364.10 24.43
1 4 0 355.84 23.16
-2 -4 0 95.73 11.93
-2 4 0 113.32 13.90
-2 -4 0 104.28 11.95
2 -4 0 85.24 11.82
2 4 0 92.16 11.58
-3 -4 0 7.80 4.14
-3 -4 0 7.65 4.86
-3 4 0 22.71 7.76
3 4 0 7.34 4.70
-4 -4 0 3.10 4.22
-4 4 0 5.66 5.73
4 4 0 7.22 4.77
4 -4 0 -8.77 5.62
-4 -4 0 -3.40 3.72
-5 4 0 182.15 18.07
-5 -4 0 164.00 16.64
5 4 0 168.43 14.41
5 -4 0 156.04 16.75
6 -4 0 115.16 15.32
-6 4 0 110.71 14.56
-6 -4 0 99.07 12.93
6 4 0 96.27 11.29
7 -4 0 96.46 14.57
-7 4 0 118.73 15.65
7 4 0 125.21 12.68
-7 -4 0 118.01 14.70
8 -4 0 180.64 20.61
-8 -4 0 193.88 19.54
8 4 0 217.83 16.19
-8 4 0 185.21 19.36
9 4 0 92.67 11.14
9 -4 0 68.83 14.23
-9 -4 0 94.96 14.45
-9 4 0 76.64 12.82
-10 4 0 28.57 8.84
10 -4 0 30.93 11.46
10 4 0 44.01 8.05
-10 -4 0 30.30 9.88
17 0 -1 2.98 5.74
-17 0 1 -1.71 6.27
-16 0 1 -2.05 4.90
16 0 -1 -1.70 3.63
-15 0 1 6.68 7.78
15 0 -1 -1.79 4.34
14 0 -1 3.90 4.98
-14 0 1 5.34 7.07
13 0 -1 -0.02 4.09
-13 0 1 5.29 5.09
-12 0 1 0.78 4.55
12 0 -1 1.21 3.22
11 0 -1 2.43 4.00
-11 0 1 5.05 4.55
-10 0 1 4.43 4.87
10 0 -1 0.66 2.60
-9 0 1 -3.11 3.94
9 0 -1 -1.93 3.01
8 0 -1 -0.77 1.95
-8 0 1 0.68 2.38
-7 0 1 3.13 3.11
7 0 -1 -1.60 2.39
-6 0 1 5.86 3.11
6 0 -1 -0.49 1.65
5 0 -1 0.26 1.71
5 0 -1 -0.78 1.73
-5 0 1 -0.38 1.59
-4 0 1 0.94 0.45
4 0 -1 -0.55 1.24
-4 0 1 0.67 1.61
4 0 -1 0.23 1.18
3 0 -1 2.89 1.70
-3 0 1 0.81 0.55
3 0 -1 1.29 1.12
-3 0 1 0.62 1.29
2 0 -1 0.75 0.53
-2 0 1 0.32 0.42
2 0 -1 0.06 0.69
-2 0 1 -0.01 0.53
-1 0 1 -0.35 0.61
1 0 -1 5.99 0.83
0 0 1 -0.51 0.37
-1 0 -1 0.17 0.51
-1 0 -1 1.02 0.76
1 0 1 -0.04 0.35
1 0 1 -0.12 0.47
-2 0 -1 2.55 1.32
-2 0 -1 -1.56 1.15
2 0 1 -0.83 0.95
2 0 1 1.20 0.65
3 0 1 0.60 0.49
-3 0 -1 1.20 1.46
-3 0 -1 -0.17 1.29
4 0 1 0.54 0.44
-4 0 -1 0.29 1.75
-4 0 -1 1.87 1.69
-5 0 -1 -2.32 2.81
-6 0 -1 -0.44 2.19
-7 0 -1 -3.12 3.57
8 0 1 4.82 3.10
-8 0 -1 -2.23 2.95
-9 0 -1 -4.19 5.19
9 0 1 -0.16 2.69
-10 0 -1 8.76 5.39
10 0 1 4.22 3.42
-11 0 -1 -3.89 5.72
11 0 1 -2.48 3.62
-12 0 -1 7.02 6.01
12 0 1 7.69 4.79
13 0 1 5.61 4.60
-13 0 -1 1.43 4.90
14 0 1 2.24 5.13
-14 0 -1 -7.06 7.20
-15 0 -1 -1.84 7.33
15 0 1 5.87 5.78
16 0 1 8.11 6.69
-16 0 -1 3.41 7.21
17 0 1 -3.87 5.37
-17 0 -1 -2.56 5.68
-17 -1 1 82.67 15.38
17 1 -1 136.80 16.79
-17 1 1 99.97 17.80
17 -1 -1 107.64 15.97
-16 -1 1 71.55 13.20
16 1 -1 85.41 12.74
-16 1 1 90.83 16.70
16 -1 -1 73.41 13.15
15 -1 -1 317.35 24.65
-15 1 1 292.72 28.22
15 1 -1 293.24 21.82
-15 -1 1 253.56 24.73
14 1 -1 24.94 6.63
14 -1 -1 38.38 9.60
-14 1 1 27.71 9.81
-14 -1 1 14.29 5.14
13 -1 -1 114.23 14.23
13 1 -1 101.33 12.42
-13 1 1 87.43 14.52
-13 -1 1 93.87 13.69
12 1 -1 243.94 17.57
-12 1 1 254.56 23.10
-12 -1 1 262.65 21.90
12 -1 -1 263.42 19.61
-11 1 1 27.83 7.95
11 -1 -1 21.86 5.52
-11 -1 1 30.79 7.73
11 1 -1 24.20 6.14
-10 -1 1 655.67 31.80
10 -1 -1 716.63 29.44
10 1 -1 734.81 27.76
-10 1 1 646.42 33.53
9 -1 -1 1099.59 34.14
9 1 -1 1057.59 32.29
-9 -1 1 1021.96 37.24
-9 1 1 953.16 38.95
9 1 -1 993.48 24.36
-8 1 1 552.05 27.30
8 1 -1 575.97 29.81
-8 -1 1 542.17 25.12
8 1 -1 572.05 16.42
8 -1 -1 578.74 22.67
-7 -1 1 416.64 20.25
7 1 -1 421.89 12.89
-7 1 1 408.04 21.97
7 -1 -1 410.20 17.68
6 1 -1 19.78 2.70
-6 -1 1 19.94 4.30
6 -1 -1 13.53 3.24
-6 1 1 21.12 4.76
-5 -1 1 438.53 17.03
5 1 -1 441.37 12.04
-5 -1 1 458.00 21.21
-5 1 1 407.50 18.82
5 -1 -1 423.77 15.35
4 -1 -1 949.46 22.38
4 1 -1 972.68 18.91
-4 1 1 994.99 27.57
-4 -1 1 991.02 23.08
4 1 -1 935.39 29.79
3 -1 -1 2464.62 38.59
3 1 -1 2438.72 35.45
-3 -1 1 2378.07 36.14
-3 -1 1 2430.50 43.40
3 1 -1 2503.38 47.14
-3 1 1 2457.49 42.46
2 1 -1 9679.57 107.69
2 -1 -1 9711.56 110.50
-2 -1 1 9549.54 111.44
-2 1 1 9811.63 113.36
-2 1 1 9771.70 110.27
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10 -1 -12 121.09 16.66
10 1 -12 137.80 19.28
-10 -1 12 109.37 14.33
-10 1 12 100.99 11.58
-9 1 12 0.84 3.73
9 -1 -12 19.11 7.44
9 1 -12 11.59 7.97
-9 -1 12 -3.59 6.94
-8 1 12 8.19 4.82
8 -1 -12 12.71 6.57
8 1 -12 16.65 8.09
-8 -1 12 -4.90 7.62
-8 -1 12 1.45 3.59
-7 1 12 13.45 5.99
7 -1 -12 8.28 6.42
-7 -1 12 -7.20 8.50
7 1 -12 3.20 5.60
-7 -1 12 1.11 3.38
6 -1 -12 121.13 15.31
-6 -1 12 122.03 17.09
6 1 -12 143.93 17.17
6 -1 -12 121.55 14.19
-6 -1 12 132.60 13.78
-6 1 12 124.39 14.05
-5 1 12 99.47 13.14
5 -1 -12 103.68 14.43
-5 -1 12 122.75 17.15
5 -1 -12 116.28 13.66
5 1 -12 103.87 14.28
-5 -1 12 118.65 13.03
-4 1 12 90.49 12.70
4 -1 -12 73.46 12.33
-4 -1 12 76.64 14.12
4 1 -12 90.95 13.28
4 -1 -12 91.35 12.62
3 -1 -12 285.88 23.45
3 1 -12 283.75 23.06
-3 1 12 268.98 21.42
-3 -1 12 246.25 25.29
-2 1 12 29.22 8.41
2 -1 -12 48.04 10.55
-2 -1 12 20.71 8.26
2 1 -12 36.67 8.98
-1 1 12 4.85 4.45
1 -1 -12 11.01 6.31
-1 -1 12 0.27 5.62
0 1 12 -0.07 4.62
0 -1 -12 8.68 4.76
0 -1 12 -1.75 8.36
-1 -1 -12 213.50 20.67
-1 1 -12 227.11 24.41
1 1 12 223.79 19.26
1 -1 12 256.54 25.23
-2 -1 -12 28.73 9.13
-2 1 -12 28.27 11.40
2 1 12 33.01 7.90
-2 -1 -12 30.13 8.55
2 -1 12 22.37 8.76
-3 -1 -12 37.07 10.37
-3 1 -12 35.46 11.42
3 1 12 63.03 9.94
-3 -1 -12 63.51 12.17
3 -1 12 40.57 10.45
-4 -1 -12 31.96 9.68
-4 1 -12 29.09 9.59
4 1 12 26.37 7.34
-4 -1 -12 40.81 11.22
4 -1 12 21.70 7.58
-5 -1 -12 18.91 7.95
-5 1 -12 18.27 8.70
5 1 12 19.46 6.49
-5 -1 -12 19.27 8.33
5 -1 12 -0.80 7.42
-6 -1 -12 22.22 9.43
-6 1 -12 42.95 12.38
6 1 12 39.76 7.93
6 1 12 17.92 4.55
-6 -1 -12 20.36 8.03
6 -1 12 36.14 9.49
-7 -1 -12 15.27 9.19
-7 1 -12 16.43 8.55
-7 -1 -12 12.01 7.71
-8 -1 -12 0.58 6.23
-8 1 -12 21.04 11.26
-8 -1 -12 12.07 8.60
-9 -1 -12 -5.60 6.60
-9 1 -12 -4.59 6.90
-9 -1 -12 0.01 6.57
11 -2 -12 13.39 8.49
11 2 -12 4.34 7.98
-11 -2 12 3.70 6.52
-10 2 12 9.94 4.21
10 -2 -12 39.04 11.39
10 2 -12 28.27 10.71
-10 -2 12 16.96 7.30
-9 2 12 -3.29 5.02
9 -2 -12 8.40 6.84
9 2 -12 5.19 7.28
-9 -2 12 15.05 7.05
-8 2 12 -6.89 6.26
8 -2 -12 6.09 6.87
8 2 -12 13.88 7.56
-8 -2 12 3.90 5.60
-7 2 12 20.70 7.55
7 -2 -12 31.86 12.12
7 2 -12 16.49 9.46
-7 -2 12 19.50 7.50
6 -2 -12 7.40 4.88
6 2 -12 1.18 4.99
-6 -2 12 12.13 5.55
5 -2 -12 40.89 9.87
5 2 -12 40.68 10.68
-5 -2 12 42.57 9.34
4 -2 -12 14.20 7.30
4 2 -12 13.31 6.23
-4 -2 12 9.95 4.94
3 -2 -12 12.74 7.44
3 2 -12 9.70 6.27
-3 -2 12 5.08 4.69
2 -2 -12 13.80 8.31
2 2 -12 8.33 6.64
1 2 -12 22.41 9.80
1 -2 -12 5.33 4.83
1 2 -12 6.98 5.85
0 2 -12 8.72 8.07
0 -2 -12 1.58 4.35
0 2 -12 1.78 6.62
-1 2 -12 6.28 6.59
-1 -2 -12 -3.10 5.17
-2 -2 -12 4.74 5.26
-2 2 -12 4.66 5.33
-2 -2 -12 12.94 7.65
3 2 12 10.58 6.76
-3 -2 -12 2.48 4.22
-3 2 -12 23.39 10.90
3 2 12 4.83 2.85
-3 -2 -12 13.24 7.56
4 2 12 17.22 6.95
-4 -2 -12 20.28 9.27
-4 2 -12 21.46 9.35
4 2 12 8.28 3.41
-4 -2 -12 16.08 7.78
5 2 12 -6.07 6.41
-5 -2 -12 4.79 6.19
-5 2 -12 8.36 6.48
5 2 12 -0.90 2.62
-5 -2 -12 -1.82 4.63
6 2 12 -5.34 5.80
-6 -2 -12 2.39 5.02
6 2 12 10.39 4.57
-6 -2 -12 4.71 7.50
-7 -2 -12 1.00 7.35
-7 2 -12 -0.56 6.05
7 2 12 3.29 4.13
-7 -2 -12 2.08 6.49
6 -3 -12 7.08 7.01
6 3 -12 22.97 10.83
-6 -3 12 8.85 7.12
5 -3 -12 14.17 7.94
5 3 -12 17.95 9.75
-5 -3 12 14.37 6.85
4 -3 -12 44.67 11.88
4 3 -12 30.85 11.07
-4 -3 12 46.13 11.55
3 -3 -12 6.16 6.39
3 3 -12 -11.38 7.71
-3 -3 12 -7.50 6.54
2 -3 -12 28.05 10.67
2 3 -12 27.69 9.87
1 -3 -12 2.29 6.32
1 3 -12 -1.26 5.90
0 -3 -12 -1.81 5.11
0 3 -12 14.85 9.19
1 3 12 30.93 7.14
-1 -3 -12 13.62 7.76
-1 3 -12 33.11 11.54
2 3 12 54.07 8.88
-2 -3 -12 57.87 14.51
-2 3 -12 49.36 13.36
12 0 -13 4.86 6.37
12 0 -13 -0.61 5.90
11 0 -13 -2.84 6.33
11 0 -13 14.39 8.14
10 0 -13 0.70 5.07
-10 0 13 10.23 5.69
10 0 -13 6.37 6.32
9 0 -13 1.22 4.21
-9 0 13 1.01 4.85
9 0 -13 -5.56 5.79
8 0 -13 4.33 4.97
-8 0 13 2.47 4.52
8 0 -13 -6.19 6.62
7 0 -13 0.83 4.70
-7 0 13 12.61 8.10
7 0 -13 0.13 4.89
6 0 -13 -4.84 5.47
6 0 -13 1.99 4.64
-5 0 13 10.25 6.89
5 0 -13 -2.53 4.69
5 0 -13 5.61 5.93
4 0 -13 -6.43 6.20
4 0 -13 4.79 4.51
-3 0 13 17.44 8.74
3 0 -13 15.42 7.70
-2 0 13 27.67 10.35
-1 0 13 17.48 9.00
0 0 13 33.45 10.50
1 0 13 19.21 7.86
-2 0 -13 3.25 6.29
2 0 13 16.35 8.59
-3 0 -13 -3.03 6.06
3 0 13 2.96 6.44
-4 0 -13 2.31 7.63
4 0 13 6.98 6.41
-5 0 -13 5.58 6.83
5 0 13 13.51 7.43
-6 0 -13 -2.39 5.15
6 0 13 -0.09 4.25
-7 0 -13 -3.83 6.25
-8 0 -13 -5.32 8.31
11 -1 -13 45.08 11.21
11 1 -13 49.94 13.43
-10 1 13 78.10 10.49
10 -1 -13 93.42 15.46
10 1 -13 96.31 17.10
-10 -1 13 100.32 14.37
-9 1 13 32.29 7.60
9 -1 -13 26.95 9.96
9 1 -13 37.57 11.81
-9 -1 13 0.04 5.57
-8 1 13 69.71 10.26
8 -1 -13 73.26 13.15
8 1 -13 64.95 14.03
-8 -1 13 84.44 14.06
7 -1 -13 -5.39 5.37
-7 -1 13 -10.13 8.68
7 1 -13 -2.39 5.33
-6 1 13 9.86 6.64
6 -1 -13 3.18 4.40
-6 -1 13 -4.51 9.28
6 1 -13 4.63 4.05
-6 -1 13 7.30 5.68
-5 1 13 21.51 7.08
5 -1 -13 24.93 8.58
-5 -1 13 16.98 7.90
5 1 -13 32.46 10.06
5 -1 -13 35.04 8.78
-4 1 13 41.23 9.51
4 -1 -13 62.44 12.48
-4 -1 13 39.39 11.18
4 1 -13 59.64 12.26
4 -1 -13 71.53 12.18
3 -1 -13 174.28 19.50
-3 -1 13 179.62 23.69
3 1 -13 207.05 21.03
-3 1 13 192.56 18.41
-2 1 13 29.65 8.49
2 -1 -13 43.24 9.76
-2 -1 13 7.71 8.73
2 1 -13 24.44 7.99
-1 1 13 8.27 5.62
1 -1 -13 9.85 5.95
0 1 13 12.60 6.70
0 -1 -13 8.76 5.89
0 -1 13 -2.04 8.49
-1 1 -13 5.48 7.91
1 1 13 12.66 6.51
-1 -1 -13 5.58 6.12
1 -1 13 -3.31 9.11
-2 -1 -13 15.33 9.25
-2 1 -13 17.18 8.92
2 1 13 28.00 8.40
-2 -1 -13 15.09 6.85
2 -1 13 10.25 6.20
-3 -1 -13 51.77 13.19
-3 1 -13 68.11 15.30
3 1 13 66.09 10.68
-3 -1 -13 71.16 13.18
3 -1 13 60.33 12.84
-4 -1 -13 14.39 8.37
-4 1 -13 20.40 9.55
4 1 13 17.91 6.96
-4 -1 -13 28.25 9.26
4 -1 13 25.36 9.90
-5 -1 -13 17.42 9.32
-5 1 -13 2.54 6.40
5 1 13 11.54 5.17
-5 -1 -13 7.19 5.92
5 -1 13 -3.67 6.37
-6 -1 -13 13.39 9.70
-6 1 -13 5.07 7.95
6 1 13 0.93 3.83
-6 -1 -13 3.41 6.00
6 -1 13 -16.03 10.07
-7 -1 -13 23.60 10.16
-7 1 -13 9.81 6.31
-7 -1 -13 27.72 11.06
-9 2 13 -9.47 5.98
9 -2 -13 -3.06 5.96
9 2 -13 25.00 10.85
-9 -2 13 15.13 8.08
-8 2 13 76.33 11.40
8 -2 -13 92.28 16.12
8 2 -13 106.55 18.09
-8 -2 13 113.26 15.39
-7 2 13 114.18 14.34
7 -2 -13 115.69 17.82
7 2 -13 151.23 21.62
-7 -2 13 133.23 16.69
-6 2 13 83.70 13.20
6 -2 -13 88.61 15.70
6 2 -13 88.70 15.25
-6 -2 13 123.67 15.68
-5 2 13 63.67 11.52
5 -2 -13 55.91 12.65
5 2 -13 56.51 12.47
-5 -2 13 63.00 11.40
-4 2 13 39.04 9.32
4 -2 -13 47.86 12.19
4 2 -13 46.34 11.77
-4 -2 13 46.97 10.43
-3 2 13 -3.72 6.47
3 -2 -13 7.32 8.70
3 2 -13 -2.28 5.47
-2 2 13 15.40 6.98
2 -2 -13 18.90 8.65
2 2 -13 21.69 8.65
-1 2 13 82.12 13.44
1 2 -13 93.74 17.32
1 -2 -13 69.33 14.16
1 2 -13 84.77 14.75
0 2 13 51.09 10.82
0 2 -13 53.09 13.68
0 -2 -13 43.82 12.12
0 2 -13 63.36 13.19
-1 -2 -13 52.97 12.75
1 2 13 47.76 10.21
-1 2 -13 44.85 14.63
-1 -2 -13 63.32 14.15
2 2 13 10.03 5.40
-2 -2 -13 17.51 9.44
-2 2 -13 16.72 10.21
-2 -2 -13 16.56 8.63
3 2 13 20.50 6.08
-3 -2 -13 51.35 13.03
-3 2 -13 41.03 12.84
-3 -2 -13 38.72 11.70
4 2 13 -2.39 5.64
-4 -2 -13 11.62 7.87
-4 2 -13 8.96 8.30
-4 -2 -13 5.27 6.21
5 2 13 -16.87 7.97
-5 -2 -13 7.33 6.40
-5 2 -13 5.90 8.14
-5 -2 -13 7.29 7.86
-10 0 14 37.44 8.71
10 0 -14 28.83 9.94
-9 0 14 15.99 7.00
9 0 -14 11.21 6.63
-8 0 14 17.23 7.28
8 0 -14 4.94 4.97
-7 0 14 59.39 11.42
7 0 -14 33.67 10.21
6 0 -14 182.24 20.91
-6 0 14 178.13 19.36
5 0 -14 210.67 22.00
-5 0 14 262.27 23.52
-4 0 14 28.94 10.50
4 0 -14 21.97 9.01
-3 0 14 70.87 13.36
3 0 -14 65.53 12.84
-2 0 14 20.20 9.98
-1 0 14 4.03 7.71
0 0 14 76.64 14.35
-1 0 -14 172.94 23.46
1 0 14 184.95 19.85
-2 0 -14 19.76 9.12
2 0 14 38.70 10.44
-3 0 -14 18.83 10.05
3 0 14 28.85 9.45
-4 0 -14 23.76 9.24
4 0 14 23.30 8.49
-5 0 -14 29.30 11.32
5 0 14 26.01 7.85
-6 0 -14 -4.82 6.53
6 0 14 -1.11 5.31
-9 1 14 46.29 8.71
9 -1 -14 42.25 11.66
9 1 -14 66.71 14.41
-9 -1 14 55.30 12.24
-8 1 14 45.15 8.94
8 -1 -14 62.74 12.97
8 1 -14 46.08 11.78
-8 -1 14 52.02 13.17
-7 1 14 17.64 6.87
7 -1 -14 8.99 6.39
-7 -1 14 5.08 8.57
7 1 -14 21.74 8.54
-6 1 14 -1.94 4.42
6 -1 -14 3.47 4.95
-6 -1 14 -13.04 10.48
6 1 -14 -5.68 7.12
-5 1 14 9.64 6.32
5 -1 -14 -0.13 4.99
-5 -1 14 -10.98 8.99
5 1 -14 1.55 5.23
-4 1 14 53.10 9.53
4 -1 -14 37.20 9.97
-4 -1 14 29.24 10.52
4 1 -14 59.74 13.37
4 -1 -14 45.14 10.74
-3 1 14 30.04 8.38
3 -1 -14 34.01 10.11
-3 -1 14 29.71 10.13
3 1 -14 36.42 9.91
-2 1 14 26.70 8.67
2 -1 -14 31.84 9.52
-2 -1 14 11.41 10.31
2 1 -14 41.06 11.53
-1 1 14 87.06 12.84
1 -1 -14 112.88 16.44
-1 -1 14 83.76 16.14
0 1 -14 8.09 9.41
0 1 14 2.40 5.22
0 -1 -14 -1.30 6.15
0 -1 14 -7.95 10.45
-1 1 -14 11.00 7.76
1 1 14 13.06 5.89
-1 -1 -14 -4.48 6.65
1 -1 14 -4.67 11.18
-2 -1 -14 5.71 5.57
-2 1 -14 3.61 6.37
2 1 14 13.28 6.63
-2 -1 -14 15.74 8.53
-3 -1 -14 14.59 8.51
-3 1 -14 9.99 8.35
3 1 14 15.79 6.76
-3 -1 -14 18.93 8.67
3 -1 14 -4.38 7.40
-4 -1 -14 -1.72 6.10
-4 1 -14 7.82 8.93
4 1 14 21.24 8.02
-4 -1 -14 12.09 6.84
4 -1 14 -10.71 9.15
-5 -1 -14 15.91 7.71
-5 1 -14 9.82 8.16
5 1 14 15.56 6.78
-5 -1 -14 21.11 8.89
5 -1 14 11.55 7.20
-6 2 14 6.35 5.67
6 -2 -14 -3.74 6.29
6 2 -14 3.72 6.62
-6 -2 14 -0.07 5.16
-5 2 14 -5.03 7.00
5 -2 -14 16.95 9.85
5 2 -14 -5.00 8.48
-4 2 14 5.46 5.49
4 -2 -14 11.43 7.80
4 2 -14 5.46 7.03
-3 2 14 -3.61 7.63
3 -2 -14 6.80 7.46
3 2 -14 19.34 9.03
-2 2 14 1.66 6.07
2 2 -14 1.99 5.59
1 2 -14 1.83 5.94
-1 2 14 -8.19 6.69
1 -2 -14 5.94 7.09
1 2 -14 3.45 6.78
0 2 14 -1.99 5.65
0 2 -14 12.17 8.77
0 -2 -14 3.88 7.56
0 2 -14 5.15 6.77
-1 -2 -14 0.16 5.81
1 2 14 3.14 5.85
-1 -2 -14 0.52 5.48
-1 2 -14 6.70 6.22
-2 -2 -14 9.56 8.55
2 2 14 2.44 5.34
-2 2 -14 13.51 9.43
-2 -2 -14 4.92 6.34
-8 0 15 12.83 7.95
8 0 -15 -1.84 7.74
-7 0 15 12.39 8.47
7 0 -15 4.10 6.34
-6 0 15 11.65 8.20
6 0 -15 8.60 6.94
-5 0 15 16.27 9.43
5 0 -15 4.49 5.39
-4 0 15 23.82 11.15
4 0 -15 3.44 8.07
-3 0 15 19.33 9.46
3 0 -15 4.34 7.39
-2 0 15 21.14 10.33
-1 0 15 23.60 11.22
0 0 15 5.86 7.74
-1 0 -15 19.19 10.17
1 0 15 19.78 8.87
-2 0 -15 4.31 6.65
2 0 15 -1.39 5.16
-3 0 -15 2.42 8.69
3 0 15 6.90 7.31
-7 1 15 60.98 10.34
7 -1 -15 42.88 12.03
7 1 -15 61.28 14.35
-7 -1 15 22.38 11.98
-6 1 15 -1.13 4.53
6 -1 -15 1.53 6.24
-6 -1 15 4.87 8.92
6 1 -15 0.33 4.31
-5 1 15 15.07 7.44
5 -1 -15 0.84 6.30
-5 -1 15 -6.66 10.52
5 1 -15 -1.94 5.69
-4 1 15 -0.45 4.52
4 -1 -15 23.25 9.53
-4 -1 15 -17.05 14.57
4 1 -15 7.73 6.62
-3 1 15 14.33 6.78
3 -1 -15 7.24 6.05
3 1 -15 9.47 7.27
3 -1 -15 19.30 8.48
-2 1 15 35.96 8.58
2 -1 -15 47.08 12.02
-2 -1 15 35.19 12.82
2 1 -15 40.90 11.50
-1 1 15 11.44 7.08
1 -1 -15 9.63 7.15
-1 -1 15 13.49 9.70
1 1 -15 15.41 7.92
0 1 -15 17.93 10.93
0 1 15 29.60 9.08
0 -1 -15 22.97 9.39
0 -1 15 6.29 9.43
-1 -1 -15 17.08 9.58
-1 1 -15 22.54 11.69
1 1 15 8.67 6.33
-1 -1 -15 6.85 7.61
-2 -1 -15 -8.49 6.75
-2 1 -15 0.20 6.82
2 1 15 0.78 4.69
-2 -1 -15 1.70 6.44
2 -1 15 -3.46 9.07
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 77426
_shelx_res_file
;
TITL ds4bc11_a.res in P2(1)/c
(2).res created by SHELXL-2016/4 at 14:33:36 on 31-Jan-2018
REM Old TITL DS4B C1 1 in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.154, Rweak 0.539, Alpha 0.032, Orientation as input
REM Formula found by SHELXT: C8 O Br
CELL 0.71073 14.4391 3.9937 12.7244 90 97.827 90
ZERR 2 0.0007 0.0002 0.0007 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br O
UNIT 32 20 4 4
L.S. 4
PLAN 4
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.023400 0.438200
EXTI 0.004715
FVAR 0.73056
BR1 3 0.069046 0.863436 0.668373 11.00000 0.04334 0.05040 =
0.07061 0.00106 0.02309 0.00725
C1 1 0.310594 0.387550 0.511009 11.00000 0.03537 0.03801 =
0.03343 0.00106 0.00567 -0.00099
C2 1 0.321220 0.454307 0.618763 11.00000 0.03796 0.06015 =
0.03404 -0.00011 0.00122 0.00884
AFIX 43
H2 2 0.377230 0.400535 0.660470 11.00000 -1.20000
AFIX 0
C3 1 0.250302 0.598963 0.665294 11.00000 0.04646 0.05978 =
0.03589 -0.00261 0.00816 0.01195
AFIX 43
H3 2 0.258517 0.646056 0.737543 11.00000 -1.20000
AFIX 0
C4 1 0.167273 0.672609 0.603389 11.00000 0.03709 0.03439 =
0.04866 0.00281 0.01576 0.00086
C5 1 0.153750 0.607315 0.496221 11.00000 0.03710 0.05142 =
0.04874 0.00343 0.00023 0.00544
AFIX 43
H5 2 0.097052 0.657253 0.455312 11.00000 -1.20000
AFIX 0
C6 1 0.225769 0.466592 0.450661 11.00000 0.04393 0.04914 =
0.03282 -0.00057 0.00302 0.00308
AFIX 43
H6 2 0.217497 0.423632 0.378154 11.00000 -1.20000
AFIX 0
C7 1 0.385852 0.239855 0.456991 11.00000 0.03947 0.04801 =
0.03823 -0.00569 0.00599 -0.00159
C8 1 0.467237 0.075959 0.521828 11.00000 0.03640 0.05136 =
0.03569 -0.00642 0.00602 -0.00045
AFIX 43
H8 2 0.471561 0.081856 0.595399 11.00000 -1.20000
AFIX 0
O1 4 0.381624 0.247808 0.361318 11.00000 0.05907 0.10870 =
0.03218 -0.00710 0.00777 0.02324
HKLF 4
REM ds4bc11_a.res in P2(1)/c
REM R1 = 0.0292 for 1228 Fo > 4sig(Fo) and 0.0395 for all 1470 data
REM 92 parameters refined using 0 restraints
END
WGHT 0.0234 0.4382
REM Highest difference peak 0.355, deepest hole -0.430, 1-sigma level 0.059
Q1 1 0.0559 0.8106 0.6016 11.00000 0.05 0.36
Q2 1 0.0789 1.1808 0.6596 11.00000 0.05 0.24
Q3 1 0.4228 0.1272 0.4918 11.00000 0.05 0.23
Q4 1 0.2796 0.5196 0.4794 11.00000 0.05 0.22
;
_shelx_res_checksum 30722
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
Br Br1 0.06905(2) 0.86344(8) 0.66837(3) 0.05337(16) Uani d 1
C C1 0.31059(19) 0.3876(7) 0.5110(2) 0.0355(6) Uani d 1
C C2 0.3212(2) 0.4543(8) 0.6188(2) 0.0444(7) Uani d 1
H H2 0.377230 0.400535 0.660470 0.053 Uiso calc 1
C C3 0.2503(2) 0.5990(8) 0.6653(2) 0.0471(8) Uani d 1
H H3 0.258517 0.646056 0.737543 0.057 Uiso calc 1
C C4 0.1673(2) 0.6726(6) 0.6034(2) 0.0391(7) Uani d 1
C C5 0.1538(2) 0.6073(7) 0.4962(2) 0.0463(7) Uani d 1
H H5 0.097052 0.657253 0.455312 0.056 Uiso calc 1
C C6 0.2258(2) 0.4666(8) 0.4507(2) 0.0422(7) Uani d 1
H H6 0.217497 0.423632 0.378154 0.051 Uiso calc 1
C C7 0.3859(2) 0.2399(8) 0.4570(2) 0.0418(7) Uani d 1
C C8 0.4672(2) 0.0760(7) 0.5218(2) 0.0410(7) Uani d 1
H H8 0.471561 0.081856 0.595399 0.049 Uiso calc 1
O O1 0.38162(17) 0.2478(7) 0.36132(17) 0.0665(7) Uani d 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0433(2) 0.0504(2) 0.0706(3) 0.00725(15) 0.02309(16) 0.00106(17)
C1 0.0354(15) 0.0380(14) 0.0334(15) -0.0010(12) 0.0057(12) 0.0011(12)
C2 0.0380(17) 0.0601(19) 0.0340(16) 0.0088(14) 0.0012(13) -0.0001(14)
C3 0.0465(18) 0.0598(19) 0.0359(16) 0.0119(15) 0.0082(13) -0.0026(15)
C4 0.0371(16) 0.0344(15) 0.0487(18) 0.0009(12) 0.0158(13) 0.0028(13)
C5 0.0371(16) 0.0514(18) 0.0487(18) 0.0054(14) 0.0002(13) 0.0034(15)
C6 0.0439(17) 0.0491(17) 0.0328(15) 0.0031(14) 0.0030(13) -0.0006(13)
C7 0.0395(16) 0.0480(16) 0.0382(17) -0.0016(13) 0.0060(13) -0.0057(13)
C8 0.0364(16) 0.0514(18) 0.0357(15) -0.0005(13) 0.0060(12) -0.0064(14)
O1 0.0591(15) 0.109(2) 0.0322(12) 0.0232(14) 0.0078(11) -0.0071(12)
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
C2 C1 C6 . 118.3(3)
C2 C1 C7 . 123.1(3)
C6 C1 C7 . 118.7(3)
C1 C2 H2 . 119.4
C3 C2 C1 . 121.2(3)
C3 C2 H2 . 119.4
C2 C3 H3 . 120.5
C4 C3 C2 . 119.0(3)
C4 C3 H3 . 120.5
C3 C4 Br1 . 118.8(2)
C3 C4 C5 . 121.5(3)
C5 C4 Br1 . 119.7(2)
C4 C5 H5 . 120.6
C4 C5 C6 . 118.8(3)
C6 C5 H5 . 120.6
C1 C6 H6 . 119.4
C5 C6 C1 . 121.3(3)
C5 C6 H6 . 119.4
C1 C7 C8 . 119.3(2)
O1 C7 C1 . 121.0(3)
O1 C7 C8 . 119.7(3)
C7 C8 H8 . 119.0
C8 C8 C7 3_656 121.9(4)
C8 C8 H8 3_656 119.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Br1 C4 . 1.896(3)
C1 C2 . 1.385(4)
C1 C6 . 1.390(4)
C1 C7 . 1.485(4)
C2 H2 . 0.9300
C2 C3 . 1.378(4)
C3 H3 . 0.9300
C3 C4 . 1.374(4)
C4 C5 . 1.376(4)
C5 H5 . 0.9300
C5 C6 . 1.377(4)
C6 H6 . 0.9300
C7 C8 . 1.492(4)
C7 O1 . 1.211(3)
C8 C8 3_656 1.310(5)
C8 H8 . 0.9300
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_4
_geom_torsion
Br1 C4 C5 C6 . -179.6(2)
C1 C2 C3 C4 . 1.0(5)
C1 C7 C8 C8 3_656 175.8(3)
C2 C1 C6 C5 . -0.1(4)
C2 C1 C7 C8 . 16.0(4)
C2 C1 C7 O1 . -164.7(3)
C2 C3 C4 Br1 . 178.8(2)
C2 C3 C4 C5 . -0.5(5)
C3 C4 C5 C6 . -0.4(5)
C4 C5 C6 C1 . 0.6(5)
C6 C1 C2 C3 . -0.8(5)
C6 C1 C7 C8 . -164.8(3)
C6 C1 C7 O1 . 14.5(4)
C7 C1 C2 C3 . 178.4(3)
C7 C1 C6 C5 . -179.3(3)
O1 C7 C8 C8 3_656 -3.5(6)
_cod_database_fobs_code 2242383