#------------------------------------------------------------------------------
#$Date: 2024-11-23 04:04:23 +0100 (Sat, 23 Nov 2024) $
#$Revision: 296084 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023321.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_2023321
loop_
_publ_author_name
'Li, Kun'
'Yao, Jiali'
'Iitsuka, Hiroaki'
'Yonezawa, Noriyuki'
'Okamoto, Akiko'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
(2,7-diethoxynaphthalene-1,8-diyl)bis[(4-bromophenyl)methanone]
;
_journal_coeditor_code JP2015
_journal_issue 12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S205698902401123X
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C28 H22 Br2 O4'
_chemical_formula_moiety 'C28 H22 Br2 O4'
_chemical_formula_sum 'C28 H22 Br2 O4'
_chemical_formula_weight 582.27
_chemical_name_systematic
;
(2,7-Diethoxynaphthalene-1,8-diyl)bis[(4-bromophenyl)methanone]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 101.6109(9)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.74560(14)
_cell_length_b 24.4234(4)
_cell_length_c 13.0590(2)
_cell_measurement_reflns_used 38566
_cell_measurement_temperature 193(2)
_cell_measurement_theta_max 68.25
_cell_measurement_theta_min 3.46
_cell_volume 2419.87(7)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla et al., 2007)
;
_diffrn_ambient_temperature 193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54187
_diffrn_reflns_av_R_equivalents 0.0798
_diffrn_reflns_av_unetI/netI 0.0343
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 43148
_diffrn_reflns_theta_full 67.687
_diffrn_reflns_theta_max 68.250
_diffrn_reflns_theta_min 3.620
_exptl_absorpt_coefficient_mu 4.521
_exptl_absorpt_correction_T_max 0.636
_exptl_absorpt_correction_T_min 0.260
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
(NUMABS; Rigaku, 1999)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.598
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 1168
_exptl_crystal_size_max 0.600
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.972
_refine_diff_density_min -0.603
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 331
_refine_ls_number_reflns 4414
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.020
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_gt 0.0406
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+1.6111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1107
_refine_ls_wR_factor_ref 0.1130
_reflns_number_gt 4038
_reflns_number_total 4414
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jp2015.cif
_cod_data_source_block I
_cod_original_cell_volume 2419.86(8)
_cod_database_code 2023321
_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 0.172
_shelx_estimated_absorpt_t_max 0.661
_shelx_hkl_file
;
0 0 1 0.54 0.19
0 0 1 0.76 0.13
0 0 1 0.60 0.18
0 0 1 0.58 0.35
0 0 1 0.79 0.11
0 0 1 0.30 0.18
0 0 1 -0.06 0.47
0 0 -1 0.94 0.26
0 0 -1 0.44 0.32
0 0 -1 0.36 0.19
0 0 -1 0.01 0.20
0 0 -1 -0.01 0.12
0 0 -1 0.46 0.11
0 0 -1 0.53 0.24
0 0 -1 0.79 0.34
0 0 2 337.65 21.77
0 0 2 321.90 19.30
0 0 2 340.77 25.10
0 0 2 366.09 23.70
0 0 2 329.24 20.01
0 0 2 398.99 26.81
0 0 2 337.96 22.22
0 0 -2 333.61 21.21
0 0 -2 343.43 22.23
0 0 -2 368.82 24.85
0 0 -2 312.64 20.69
0 0 -2 354.81 23.15
0 0 -2 435.46 29.87
0 0 -2 360.21 24.09
0 0 -2 337.39 20.32
0 0 -2 349.80 22.97
0 0 3 -1.67 0.76
0 0 3 -0.65 0.72
0 0 3 -0.37 0.97
0 0 3 0.23 0.74
0 0 3 -0.00 0.38
0 0 3 -0.09 0.70
0 0 3 -0.00 0.70
0 0 -3 -2.31 1.63
0 0 -3 -1.53 0.71
0 0 -3 -1.50 1.44
0 0 -3 -1.23 0.73
0 0 -3 0.03 0.40
0 0 -3 -0.69 1.03
0 0 -3 -0.16 0.38
0 0 -3 -0.33 0.70
0 0 -3 1.07 0.80
0 0 410435.51 2663.75
0 0 410357.62 2613.25
0 0 410074.58 2572.10
0 0 4 9815.89 2531.02
0 0 410776.37 2752.06
0 0 410083.52 2533.63
0 0 410402.22 2660.14
0 0 4 9596.97 2444.14
0 0 -4 8859.50 2295.53
0 0 -410383.08 2650.00
0 0 -4 9980.91 2516.22
0 0 -410221.56 2616.46
0 0 -410157.20 2593.09
0 0 -4 9730.34 2496.70
0 0 -4 9960.25 2553.30
0 0 5 0.52 0.26
0 0 5 -0.02 0.70
0 0 5 1.83 0.50
0 0 5 0.27 0.60
0 0 5 1.58 0.64
0 0 5 0.34 1.40
0 0 5 0.33 0.94
0 0 -5 1.76 0.54
0 0 -5 0.85 0.99
0 0 -5 0.38 1.10
0 0 -5 0.32 0.84
0 0 -5 0.09 0.63
0 0 -5 0.16 0.67
0 0 6 169.69 9.40
0 0 6 157.45 12.71
0 0 6 166.31 11.98
0 0 6 166.52 10.85
0 0 6 155.62 8.44
0 0 6 173.96 13.19
0 0 -6 162.57 11.46
0 0 -6 170.07 11.36
0 0 -6 161.11 11.01
0 0 -6 156.45 8.42
0 0 -6 161.29 11.21
0 0 -6 150.12 12.29
0 0 -6 163.32 11.33
0 0 7 -0.12 1.15
0 0 7 0.25 0.27
0 0 7 0.10 0.51
0 0 7 0.53 0.81
0 0 7 0.14 0.21
0 0 7 0.32 0.56
0 0 -7 9.29 1.27
0 0 -7 0.69 0.63
0 0 -7 0.61 0.36
0 0 -7 0.86 0.58
0 0 -7 0.31 0.56
0 0 -7 -0.10 0.61
0 0 8 1102.29 120.89
0 0 8 1051.78 120.53
0 0 8 1154.34 125.26
0 0 8 1144.48 123.14
0 0 8 1128.07 124.56
0 0 8 1094.12 117.90
0 0 -8 1074.18 116.52
0 0 -8 1147.69 131.32
0 0 -8 931.43 111.11
0 0 -8 1141.55 124.57
0 0 9 0.54 0.63
0 0 9 0.11 0.45
0 0 9 -0.15 0.66
0 0 -9 -0.07 0.66
0 0 -9 1.27 0.98
0 0 10 60.75 5.58
0 0 10 55.66 4.34
0 0 -10 56.74 6.74
0 0 -10 47.59 6.18
0 0 11 0.12 0.52
0 0 11 0.42 0.79
0 0 -11 0.06 1.04
0 0 -11 0.38 0.89
0 0 12 50.25 5.43
0 0 12 45.75 4.92
0 0 -12 33.45 7.37
0 0 -12 51.17 6.60
0 0 13 -0.58 1.40
0 0 -13 0.77 0.69
0 0 -13 0.51 0.81
0 0 14 29.93 3.51
0 0 -14 32.25 4.36
0 0 15 -0.09 0.41
0 1 -1 13.87 0.69
0 1 1 13.10 1.23
0 1 1 13.85 0.65
0 1 -1 12.38 0.59
0 1 1 12.23 0.64
0 1 -1 12.56 1.10
0 1 1 12.86 0.98
0 1 -1 13.01 0.53
0 1 1 11.64 0.57
0 1 -1 11.01 0.54
0 1 1 11.69 0.59
0 1 -1 11.78 0.75
0 1 1 12.29 0.71
0 1 -1 15.51 1.07
0 1 1 12.62 0.78
0 1 -1 11.90 0.49
0 -1 1 15.15 1.91
0 -1 1 13.09 0.79
0 -1 1 11.55 0.47
0 -1 1 12.11 0.69
0 -1 -1 11.71 0.58
0 -1 1 11.03 0.80
0 -1 -1 12.24 0.72
0 -1 -1 13.27 0.81
0 -1 1 12.85 0.70
0 -1 -1 12.83 0.60
0 -1 -1 12.78 0.73
0 -1 -1 12.90 0.94
0 -1 1 13.83 0.55
0 -1 -1 12.04 0.57
0 -1 -1 14.89 0.67
0 1 2 19.12 2.91
0 1 2 21.81 1.54
0 1 -2 19.90 2.23
0 1 -2 25.42 2.70
0 1 2 19.78 1.72
0 1 2 21.33 1.26
0 1 2 24.36 2.50
0 1 2 19.40 1.16
0 1 2 20.69 1.72
0 1 -2 21.31 1.63
0 1 -2 19.34 1.44
0 1 -2 20.49 1.59
0 1 -2 19.71 1.57
0 1 -2 23.28 2.44
0 -1 2 26.25 2.07
0 -1 2 19.65 1.05
0 -1 2 18.51 1.56
0 -1 2 21.20 1.83
0 -1 2 18.65 1.36
0 -1 2 21.38 1.65
0 -1 -2 22.09 1.59
0 -1 -2 19.95 1.73
0 -1 -2 22.30 1.68
0 -1 -2 21.16 1.20
0 -1 -2 21.41 1.79
0 -1 -2 21.71 1.85
0 -1 2 19.39 1.00
0 -1 -2 23.74 2.33
0 -1 -2 20.28 1.86
0 -1 2 23.24 1.86
0 1 3 5643.39 1083.40
0 1 3 5536.07 1084.41
0 1 3 5559.72 1055.86
0 1 -3 5330.10 1068.66
0 1 3 5266.19 998.47
0 1 3 5383.01 1036.83
0 1 -3 5115.55 982.21
0 1 -3 5549.37 1070.02
0 1 -3 5234.75 1032.54
0 1 3 5088.53 983.13
0 1 3 5554.68 1072.45
0 1 -3 5310.09 1011.14
0 1 -3 5393.84 1040.30
0 1 -3 5166.26 997.07
0 -1 3 5292.50 1002.61
0 -1 3 5461.51 1071.77
0 -1 3 5728.25 1112.32
0 -1 3 5385.63 1038.48
0 -1 3 5207.35 1023.76
0 -1 -3 5599.11 1089.90
0 -1 3 5144.33 986.38
0 -1 -3 5346.56 1024.44
0 -1 -3 5637.37 1086.85
0 -1 -3 5376.30 1020.64
0 -1 3 5451.37 1026.48
0 -1 -3 5382.70 1039.90
0 -1 -3 5541.99 1067.60
0 -1 -3 5354.14 1035.42
0 -1 -3 5367.80 1037.22
0 -1 3 5491.58 1065.47
0 -1 -3 5674.92 1107.29
0 1 -4 355.35 23.66
0 1 4 333.58 27.48
0 1 -4 360.05 27.67
0 1 4 339.73 28.37
0 1 4 347.24 28.78
0 1 4 311.28 20.33
0 1 4 380.13 33.91
0 1 4 359.57 25.14
0 1 -4 345.02 24.56
0 1 4 365.62 25.68
0 1 -4 354.22 25.62
0 1 -4 377.62 35.40
0 1 -4 357.01 25.82
0 1 -4 377.90 32.15
0 -1 4 370.75 29.88
0 -1 4 354.68 23.06
0 -1 4 334.12 21.10
0 -1 4 366.24 29.83
0 -1 4 373.10 27.53
0 -1 -4 372.90 26.35
0 -1 4 335.83 23.60
0 -1 -4 367.26 31.76
0 -1 4 380.80 27.95
0 -1 -4 353.60 25.40
0 -1 -4 324.34 29.11
0 -1 -4 349.53 25.37
0 -1 -4 360.30 23.26
0 -1 4 338.07 24.52
0 -1 -4 348.49 22.91
0 -1 -4 367.10 26.30
0 -1 -4 361.97 26.05
0 1 -5 1199.81 130.81
0 1 5 1180.78 130.72
0 1 5 1247.95 127.97
0 1 5 1320.54 139.08
0 1 5 1156.85 117.42
0 1 5 1242.45 132.63
0 1 5 1238.95 131.75
0 1 5 1323.14 145.65
0 1 5 1248.40 133.87
0 1 -5 1234.48 131.84
0 1 -5 1277.82 136.46
0 1 -5 1106.26 118.29
0 1 -5 1126.90 115.81
0 1 -5 1256.17 135.72
0 1 -5 1199.43 134.31
0 -1 5 1227.61 135.45
0 -1 5 1234.45 134.69
0 -1 5 1258.59 128.08
0 -1 -5 1114.94 124.31
0 -1 5 1150.90 117.78
0 -1 5 1241.79 132.27
0 -1 -5 1207.38 128.63
0 -1 5 1267.17 136.69
0 -1 -5 1175.53 126.60
0 -1 5 1265.55 139.64
0 -1 -5 1234.70 133.85
0 -1 -5 1243.63 132.32
0 -1 5 1243.75 130.28
0 -1 -5 1161.50 124.14
0 -1 -5 1260.54 127.93
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0 1 -6 786.87 73.51
0 1 6 831.37 77.12
0 1 -6 832.70 80.84
0 1 6 742.28 73.68
0 1 -6 798.44 76.11
0 1 -6 718.62 73.10
0 1 6 796.43 75.75
0 1 6 853.23 75.12
0 1 -6 768.95 72.66
0 1 -6 775.53 66.92
0 1 6 882.67 87.18
0 1 -6 784.06 73.62
0 1 6 716.61 63.13
0 -1 6 810.41 78.20
0 -1 -6 807.86 77.40
0 -1 6 841.38 81.97
0 -1 -6 799.79 75.00
0 -1 6 791.02 78.37
0 -1 -6 685.30 69.10
0 -1 -6 747.48 65.41
0 -1 6 792.76 75.13
0 -1 6 770.96 67.69
0 -1 -6 774.96 72.83
0 -1 6 849.30 73.17
0 -1 -6 764.50 72.52
0 -1 6 817.72 84.05
0 1 7 775.54 72.34
0 1 7 752.16 68.98
0 1 7 738.90 64.51
0 1 7 694.99 68.23
0 1 7 754.03 80.21
0 1 7 688.31 60.66
0 1 7 771.38 72.88
0 1 -7 742.24 63.40
0 1 -7 725.25 67.54
0 1 -7 757.01 77.09
0 1 -7 720.91 67.89
0 1 -7 716.42 67.50
0 1 -7 724.94 67.67
0 -1 7 737.95 70.64
0 -1 7 707.56 69.48
0 -1 7 712.05 67.22
0 -1 7 948.70 89.74
0 -1 -7 744.11 70.92
0 -1 7 749.24 69.07
0 -1 -7 735.05 71.26
0 -1 -7 725.16 67.83
0 -1 7 722.23 66.41
0 -1 7 744.27 64.85
0 -1 -7 564.17 57.75
0 -1 -7 734.86 68.83
0 -1 -7 720.32 63.77
0 1 -8 36.30 6.80
0 1 8 44.45 3.92
0 1 8 45.87 4.25
0 1 8 43.64 4.96
0 1 8 40.99 4.72
0 1 8 45.57 3.52
0 1 -8 42.58 3.77
0 1 -8 45.14 3.82
0 1 -8 42.27 3.71
0 -1 8 40.59 3.08
0 -1 8 42.79 4.37
0 -1 8 41.42 4.07
0 -1 -8 42.68 3.91
0 -1 -8 43.31 3.31
0 -1 -8 34.62 4.38
0 -1 8 42.27 4.24
0 -1 8 44.07 3.70
0 -1 -8 42.23 3.93
0 1 -9 217.20 24.69
0 1 9 295.93 25.35
0 1 -9 295.30 23.21
0 1 9 297.20 23.97
0 -1 -9 314.37 24.73
0 -1 9 311.79 25.45
0 -1 -9 309.65 24.81
0 -1 9 303.37 22.98
0 1 10 49.97 5.63
0 1 10 49.62 4.96
0 1 -10 47.99 4.24
0 1 -10 43.38 6.01
0 -1 10 54.72 7.93
0 -1 -10 36.74 5.34
0 -1 -10 48.97 4.68
0 -1 -10 49.82 4.59
0 -1 10 45.52 3.65
0 1 11 26.51 3.36
0 1 -11 19.39 3.87
0 1 11 25.30 2.58
0 1 -11 25.61 2.88
0 -1 -11 18.63 3.57
0 -1 11 25.71 5.53
0 -1 11 23.22 2.42
0 -1 -11 24.59 3.07
0 1 12 3.00 1.08
0 1 -12 5.35 1.29
0 1 12 5.61 1.49
0 1 -12 2.29 2.85
0 -1 12 3.99 2.63
0 -1 -12 2.15 2.58
0 -1 -12 4.04 1.38
0 1 -13 131.44 9.98
0 1 13 126.38 10.85
0 1 -13 96.67 9.70
0 -1 13 123.78 10.76
0 -1 -13 130.14 10.26
0 1 -14 0.15 1.13
0 1 14 0.20 0.76
0 1 -14 0.67 0.60
0 -1 14 1.43 0.80
0 -1 14 0.41 0.84
0 -1 -14 0.80 0.69
0 -1 15 28.01 3.91
0 -1 15 22.53 2.59
0 2 0 166.05 8.46
0 2 0 185.54 8.57
0 2 0 173.98 9.51
0 2 0 163.30 8.32
0 2 0 179.63 8.70
0 2 0 168.44 7.81
0 2 0 172.43 8.41
0 2 0 150.18 8.10
0 -2 0 180.25 9.71
0 -2 0 161.01 8.24
0 -2 0 187.19 10.10
0 -2 0 156.51 7.54
0 -2 0 185.27 9.53
0 -2 0 158.09 8.42
0 -2 0 166.47 8.46
0 -2 0 167.28 8.22
0 2 -1 81.42 3.50
0 2 1 89.21 3.78
0 2 -1 90.88 4.40
0 2 1 94.84 4.60
0 2 1 93.02 4.36
0 2 1 80.09 3.77
0 2 1 94.04 4.74
0 2 -1 82.88 3.70
0 2 1 95.82 4.49
0 2 -1 90.65 4.18
0 2 -1 84.96 3.39
0 2 1 93.14 4.98
0 2 -1 85.41 4.08
0 2 -1 99.93 5.30
0 -2 1 88.60 5.04
0 -2 1 84.89 3.73
0 -2 1 90.51 4.26
0 -2 -1 98.24 4.69
0 -2 -1 89.78 4.51
0 -2 -1 84.89 5.00
0 -2 -1 94.16 4.49
0 -2 1 84.05 3.49
0 -2 -1 88.12 3.72
0 -2 1 82.09 4.56
0 -2 -1 92.48 5.83
0 -2 -1 88.57 4.70
0 -2 -1 87.20 3.28
0 -2 1 86.29 3.41
0 -2 1 87.97 4.34
0 2 2 23.55 2.34
0 2 2 22.42 2.11
0 2 2 23.09 1.71
0 2 -2 23.10 1.94
0 2 2 22.98 2.23
0 2 -2 23.66 2.43
0 2 -2 20.40 1.19
0 2 -2 19.60 1.42
0 2 2 21.25 1.59
0 2 2 24.68 2.54
0 2 -2 23.64 2.40
0 2 2 23.87 1.69
0 2 2 34.14 3.29
0 2 -2 22.55 1.95
0 2 -2 26.69 3.21
0 -2 2 26.55 3.52
0 -2 2 22.91 1.31
0 -2 2 22.50 1.91
0 -2 -2 22.92 1.55
0 -2 -2 22.01 1.67
0 -2 2 23.59 3.54
0 -2 -2 24.99 2.22
0 -2 -2 23.91 2.12
0 -2 -2 20.85 1.49
0 -2 2 22.12 2.45
0 -2 -2 24.04 2.80
0 -2 2 22.94 2.43
0 -2 2 23.60 1.78
0 2 -3 140.08 8.86
0 2 -3 127.20 11.25
0 2 3 149.17 9.40
0 2 3 133.07 10.29
0 2 3 139.81 10.57
0 2 3 153.43 13.65
0 2 -3 129.25 9.45
0 2 3 143.72 8.64
0 2 3 145.05 11.55
0 2 -3 155.43 14.18
0 2 3 123.30 13.63
0 2 3 134.85 7.98
0 2 -3 134.72 9.80
0 2 -3 142.41 7.46
0 2 -3 147.12 13.45
0 -2 3 138.93 11.41
0 -2 3 133.66 14.37
0 -2 -3 141.11 9.48
0 -2 3 129.24 12.80
0 -2 -3 140.16 8.43
0 -2 3 152.60 10.51
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TITL Yonezawa_170116_5_
yonezawa_170116_5_.res
created by SHELXL-2019/3 at 04:23:31 on 14-Nov-2024
CELL 1.54187 7.7456 24.42337 13.05895 90 101.6109 90
ZERR 4 0.00014 0.00044 0.00024 0 0.0009 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H O Br
UNIT 112 88 16 8
L.S. 10
PLAN 2
SIZE 0.6 0.3 0.1
TEMP -80
CONF
WPDB -2
HTAB
BOND $H
LIST 4
fmap 2
acta
MORE -1
REM
REM
REM
WGHT 0.067400 1.611100
FVAR 0.33508
BR1 4 0.965761 1.034038 0.364309 11.00000 0.04527 0.03872 =
0.07174 0.00497 0.00611 -0.01329
BR2 4 -0.399296 0.968230 -0.112545 11.00000 0.05820 0.05951 =
0.05055 0.00419 -0.00315 0.02283
O1 3 0.545697 0.830551 0.504306 11.00000 0.04686 0.03669 =
0.02990 0.00202 -0.00066 -0.00343
O2 3 0.069541 0.759461 -0.008881 11.00000 0.04930 0.03521 =
0.03605 -0.00286 -0.00544 -0.00483
O3 3 0.207204 0.884060 0.309266 11.00000 0.02523 0.04251 =
0.04693 -0.00259 0.00709 0.00388
O4 3 0.396792 0.857765 0.114712 11.00000 0.03097 0.04178 =
0.03769 -0.00115 0.00846 -0.00621
C1 1 0.397826 0.808137 0.336380 11.00000 0.02208 0.03271 =
0.03272 0.00154 0.00859 -0.00163
C2 1 0.486486 0.790042 0.433746 11.00000 0.02543 0.03742 =
0.03284 -0.00032 0.00646 -0.00287
C3 1 0.506894 0.734199 0.458397 11.00000 0.03176 0.03818 =
0.03273 0.00546 0.00561 -0.00053
AFIX 43
H3 2 0.573259 0.722794 0.524202 11.00000 -1.20000
AFIX 0
C4 1 0.429578 0.696385 0.386043 11.00000 0.03016 0.03383 =
0.04086 0.00614 0.00844 0.00088
AFIX 43
H4 2 0.439489 0.658560 0.403185 11.00000 -1.20000
AFIX 0
C5 1 0.252133 0.672687 0.214276 11.00000 0.03385 0.02713 =
0.04532 -0.00045 0.01057 -0.00126
AFIX 43
H5 2 0.260856 0.635155 0.233735 11.00000 -1.20000
AFIX 0
C6 1 0.160172 0.686545 0.118069 11.00000 0.03302 0.03104 =
0.04388 -0.00546 0.00641 -0.00359
AFIX 43
H6 2 0.102926 0.659242 0.071504 11.00000 -1.20000
AFIX 0
C7 1 0.150844 0.742676 0.088017 11.00000 0.02812 0.03511 =
0.03496 -0.00009 0.00485 -0.00128
C8 1 0.231816 0.783252 0.155474 11.00000 0.02587 0.03133 =
0.03517 -0.00071 0.00672 0.00015
C9 1 0.322298 0.769083 0.258774 11.00000 0.02056 0.03106 =
0.03391 -0.00009 0.00805 -0.00044
C10 1 0.335605 0.712442 0.286668 11.00000 0.02565 0.03265 =
0.03749 0.00094 0.00907 0.00028
C11 1 0.642560 0.815964 0.606114 11.00000 0.03014 0.04763 =
0.02914 0.00157 0.00222 -0.00046
AFIX 23
H11A 2 0.750029 0.795168 0.600616 11.00000 -1.20000
H11B 2 0.569300 0.793170 0.643391 11.00000 -1.20000
AFIX 0
C12 1 0.690431 0.869035 0.662972 11.00000 0.05512 0.05294 =
0.04156 -0.00292 -0.00681 -0.00687
C13 1 -0.024950 0.720766 -0.081910 11.00000 0.03274 0.04000 =
0.03376 -0.00749 0.00717 -0.00678
AFIX 23
H13A 2 -0.112423 0.700710 -0.050432 11.00000 -1.20000
H13B 2 0.057209 0.693956 -0.102999 11.00000 -1.20000
AFIX 0
C14 1 -0.115361 0.753422 -0.174390 11.00000 0.03594 0.05305 =
0.03448 -0.00275 0.00622 -0.00894
C15 1 0.359982 0.868341 0.325366 11.00000 0.02623 0.03546 =
0.02695 -0.00225 0.00590 0.00176
C16 1 0.508507 0.908054 0.336836 11.00000 0.02698 0.03074 =
0.02767 0.00113 0.00295 0.00238
C17 1 0.483751 0.961483 0.367127 11.00000 0.03234 0.03420 =
0.04064 -0.00100 0.00861 0.00459
AFIX 43
H17 2 0.372901 0.972407 0.380858 11.00000 -1.20000
AFIX 0
C18 1 0.621031 0.999003 0.377377 11.00000 0.04222 0.02855 =
0.04706 -0.00241 0.00608 0.00286
AFIX 43
H18 2 0.606068 1.035412 0.399668 11.00000 -1.20000
AFIX 0
C19 1 0.779375 0.982475 0.354630 11.00000 0.03242 0.03203 =
0.03886 0.00563 0.00009 -0.00488
C20 1 0.806398 0.929627 0.323790 11.00000 0.02731 0.03631 =
0.04976 -0.00055 0.00676 0.00104
AFIX 43
H20 2 0.916284 0.919065 0.308167 11.00000 -1.20000
AFIX 0
C21 1 0.670816 0.892689 0.316219 11.00000 0.02943 0.03043 =
0.04365 -0.00186 0.00673 0.00239
AFIX 43
H21 2 0.688291 0.855973 0.296535 11.00000 -1.20000
AFIX 0
C22 1 0.249128 0.839335 0.110436 11.00000 0.03233 0.03353 =
0.02644 -0.00296 0.00675 -0.00340
C23 1 0.090749 0.870512 0.058579 11.00000 0.03308 0.03070 =
0.03010 -0.00202 0.00441 -0.00133
C24 1 0.107622 0.909484 -0.016293 11.00000 0.04098 0.03891 =
0.03986 0.00436 0.01236 -0.00067
AFIX 43
H24 2 0.219855 0.916307 -0.032517 11.00000 -1.20000
AFIX 0
C25 1 -0.037857 0.938378 -0.067296 11.00000 0.05735 0.03948 =
0.03963 0.00934 0.01289 0.00586
AFIX 43
H25 2 -0.027117 0.964235 -0.120001 11.00000 -1.20000
AFIX 0
C26 1 -0.198953 0.929156 -0.040622 11.00000 0.04277 0.03762 =
0.03548 -0.00154 0.00010 0.00968
C27 1 -0.219378 0.892218 0.036211 11.00000 0.03303 0.04417 =
0.03856 -0.00180 0.00506 0.00043
AFIX 43
H27 2 -0.330361 0.887427 0.055432 11.00000 -1.20000
AFIX 0
C28 1 -0.072968 0.862276 0.084567 11.00000 0.03507 0.03844 =
0.03374 0.00422 0.00572 -0.00241
AFIX 43
H28 2 -0.084796 0.835830 0.136056 11.00000 -1.20000
AFIX 0
H12A 2 0.754710 0.890067 0.619907 11.00000 0.08670
H12B 2 0.767261 0.862776 0.729497 11.00000 0.07674
H12C 2 0.581639 0.886675 0.674776 11.00000 0.07645
H14A 2 -0.197598 0.780078 -0.160647 11.00000 0.05443
H14B 2 -0.175188 0.732528 -0.223224 11.00000 0.06680
H14C 2 -0.028070 0.772158 -0.201706 11.00000 0.05950
HKLF 4
REM Yonezawa_170116_5_
REM wR2 = 0.1130, GooF = S = 1.020, Restrained GooF = 1.020 for all data
REM R1 = 0.0406 for 4038 Fo > 4sig(Fo) and 0.0429 for all 4414 data
REM 331 parameters refined using 0 restraints
END
WGHT 0.0674 1.6111
REM Instructions for potential hydrogen bonds
EQIV $1 x, -y+3/2, z-1/2
HTAB C13 O3_$1
EQIV $2 x+1, y, z
HTAB C20 O3_$2
EQIV $3 x-1, y, z
HTAB C27 O4_$3
EQIV $4 -x+2, -y+2, -z+1
HTAB C12 Br1_$4
REM Highest difference peak 0.972, deepest hole -0.603, 1-sigma level 0.078
Q1 1 -0.3115 0.9841 -0.1381 11.00000 0.05 0.97
Q2 1 0.9711 0.9950 0.3618 11.00000 0.05 0.95
;
_shelx_res_checksum 16253
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+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
Br Br1 0.96576(4) 1.03404(2) 0.36431(3) 0.05270(14) Uani d 1 . .
Br Br2 -0.39930(5) 0.96823(2) -0.11254(3) 0.05806(14) Uani d 1 . .
O O1 0.5457(2) 0.83055(7) 0.50431(13) 0.0390(4) Uani d 1 . .
O O2 0.0695(2) 0.75946(7) -0.00888(13) 0.0421(4) Uani d 1 . .
O O3 0.2072(2) 0.88406(7) 0.30927(14) 0.0383(4) Uani d 1 . .
O O4 0.3968(2) 0.85776(7) 0.11471(13) 0.0366(4) Uani d 1 . .
C C1 0.3978(3) 0.80814(9) 0.33638(17) 0.0287(5) Uani d 1 . .
C C2 0.4865(3) 0.79004(10) 0.43375(18) 0.0318(5) Uani d 1 . .
C C3 0.5069(3) 0.73420(10) 0.45840(19) 0.0343(5) Uani d 1 . .
H H3 0.573259 0.722794 0.524202 0.041 Uiso calc 1 . .
C C4 0.4296(3) 0.69638(10) 0.38604(19) 0.0348(5) Uani d 1 . .
H H4 0.439489 0.658560 0.403185 0.042 Uiso calc 1 . .
C C5 0.2521(3) 0.67269(9) 0.2143(2) 0.0351(5) Uani d 1 . .
H H5 0.260856 0.635155 0.233735 0.042 Uiso calc 1 . .
C C6 0.1602(3) 0.68654(10) 0.1181(2) 0.0362(5) Uani d 1 . .
H H6 0.102926 0.659242 0.071504 0.043 Uiso calc 1 . .
C C7 0.1508(3) 0.74268(10) 0.08802(18) 0.0329(5) Uani d 1 . .
C C8 0.2318(3) 0.78325(9) 0.15547(18) 0.0307(5) Uani d 1 . .
C C9 0.3223(3) 0.76908(9) 0.25877(17) 0.0282(5) Uani d 1 . .
C C10 0.3356(3) 0.71244(9) 0.28667(19) 0.0315(5) Uani d 1 . .
C C11 0.6426(3) 0.81596(11) 0.60611(18) 0.0362(5) Uani d 1 . .
H H11A 0.750029 0.795168 0.600616 0.043 Uiso calc 1 . .
H H11B 0.569300 0.793170 0.643391 0.043 Uiso calc 1 . .
C C12 0.6904(5) 0.86904(13) 0.6630(2) 0.0522(7) Uani d 1 . .
C C13 -0.0250(3) 0.72077(10) -0.08191(18) 0.0354(5) Uani d 1 . .
H H13A -0.112423 0.700710 -0.050432 0.043 Uiso calc 1 . .
H H13B 0.057209 0.693956 -0.102999 0.043 Uiso calc 1 . .
C C14 -0.1154(4) 0.75342(13) -0.1744(2) 0.0413(6) Uani d 1 . .
C C15 0.3600(3) 0.86834(9) 0.32537(17) 0.0295(5) Uani d 1 . .
C C16 0.5085(3) 0.90805(9) 0.33684(17) 0.0288(5) Uani d 1 . .
C C17 0.4838(4) 0.96148(10) 0.3671(2) 0.0356(6) Uani d 1 . .
H H17 0.372901 0.972407 0.380858 0.043 Uiso calc 1 . .
C C18 0.6210(3) 0.99900(10) 0.3774(2) 0.0397(6) Uani d 1 . .
H H18 0.606068 1.035412 0.399668 0.048 Uiso calc 1 . .
C C19 0.7794(3) 0.98247(10) 0.35463(19) 0.0354(5) Uani d 1 . .
C C20 0.8064(3) 0.92963(10) 0.3238(2) 0.0379(5) Uani d 1 . .
H H20 0.916284 0.919065 0.308167 0.046 Uiso calc 1 . .
C C21 0.6708(3) 0.89269(10) 0.31622(19) 0.0346(5) Uani d 1 . .
H H21 0.688291 0.855973 0.296535 0.042 Uiso calc 1 . .
C C22 0.2491(3) 0.83933(9) 0.11044(17) 0.0306(5) Uani d 1 . .
C C23 0.0907(3) 0.87051(9) 0.05858(18) 0.0316(5) Uani d 1 . .
C C24 0.1076(4) 0.90948(10) -0.0163(2) 0.0393(6) Uani d 1 . .
H H24 0.219855 0.916307 -0.032517 0.047 Uiso calc 1 . .
C C25 -0.0379(4) 0.93838(11) -0.0673(2) 0.0450(6) Uani d 1 . .
H H25 -0.027117 0.964235 -0.120001 0.054 Uiso calc 1 . .
C C26 -0.1990(4) 0.92916(10) -0.04062(19) 0.0397(6) Uani d 1 . .
C C27 -0.2194(4) 0.89222(10) 0.0362(2) 0.0389(6) Uani d 1 . .
H H27 -0.330361 0.887427 0.055432 0.047 Uiso calc 1 . .
C C28 -0.0730(3) 0.86228(10) 0.08457(19) 0.0359(5) Uani d 1 . .
H H28 -0.084796 0.835830 0.136056 0.043 Uiso calc 1 . .
H H12A 0.755(6) 0.8901(17) 0.620(3) 0.087(13) Uiso d 1 . .
H H12B 0.767(5) 0.8628(16) 0.729(3) 0.077(11) Uiso d 1 . .
H H12C 0.582(6) 0.8867(16) 0.675(3) 0.076(12) Uiso d 1 . .
H H14A -0.198(4) 0.7801(14) -0.161(3) 0.054(9) Uiso d 1 . .
H H14B -0.175(5) 0.7325(17) -0.223(3) 0.067(11) Uiso d 1 . .
H H14C -0.028(5) 0.7722(14) -0.202(3) 0.060(9) Uiso 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 0.0453(2) 0.03872(19) 0.0717(2) -0.01329(11) 0.00611(17) 0.00497(12)
Br2 0.0582(3) 0.0595(2) 0.0506(2) 0.02283(14) -0.00315(16) 0.00419(13)
O1 0.0469(11) 0.0367(9) 0.0299(8) -0.0034(7) -0.0007(7) 0.0020(7)
O2 0.0493(11) 0.0352(9) 0.0360(9) -0.0048(8) -0.0054(8) -0.0029(7)
O3 0.0252(9) 0.0425(9) 0.0469(10) 0.0039(7) 0.0071(7) -0.0026(7)
O4 0.0310(10) 0.0418(9) 0.0377(9) -0.0062(7) 0.0085(7) -0.0011(7)
C1 0.0221(12) 0.0327(11) 0.0327(11) -0.0016(9) 0.0086(9) 0.0015(9)
C2 0.0254(12) 0.0374(12) 0.0328(11) -0.0029(9) 0.0065(9) -0.0003(9)
C3 0.0318(13) 0.0382(12) 0.0327(12) -0.0005(10) 0.0056(10) 0.0055(9)
C4 0.0302(13) 0.0338(12) 0.0409(13) 0.0009(10) 0.0084(10) 0.0061(10)
C5 0.0339(13) 0.0271(11) 0.0453(13) -0.0013(9) 0.0106(11) -0.0005(9)
C6 0.0330(14) 0.0310(12) 0.0439(13) -0.0036(10) 0.0064(10) -0.0055(10)
C7 0.0281(13) 0.0351(12) 0.0350(12) -0.0013(9) 0.0048(10) -0.0001(9)
C8 0.0259(12) 0.0313(11) 0.0352(12) 0.0001(9) 0.0067(9) -0.0007(9)
C9 0.0206(12) 0.0311(11) 0.0339(12) -0.0004(8) 0.0080(9) -0.0001(8)
C10 0.0256(12) 0.0327(12) 0.0375(12) 0.0003(9) 0.0091(9) 0.0009(9)
C11 0.0301(13) 0.0476(14) 0.0291(11) -0.0005(10) 0.0022(10) 0.0016(10)
C12 0.055(2) 0.0529(17) 0.0416(15) -0.0069(14) -0.0068(14) -0.0029(13)
C13 0.0327(13) 0.0400(13) 0.0338(12) -0.0068(10) 0.0072(10) -0.0075(10)
C14 0.0359(15) 0.0530(16) 0.0345(13) -0.0089(13) 0.0062(11) -0.0027(11)
C15 0.0262(13) 0.0355(12) 0.0269(10) 0.0018(9) 0.0059(9) -0.0022(8)
C16 0.0270(12) 0.0307(11) 0.0277(10) 0.0024(9) 0.0029(9) 0.0011(8)
C17 0.0323(14) 0.0342(13) 0.0406(14) 0.0046(9) 0.0086(11) -0.0010(9)
C18 0.0422(15) 0.0286(11) 0.0471(14) 0.0029(10) 0.0061(11) -0.0024(10)
C19 0.0324(13) 0.0320(11) 0.0389(13) -0.0049(10) 0.0001(10) 0.0056(10)
C20 0.0273(13) 0.0363(13) 0.0498(14) 0.0010(10) 0.0068(10) -0.0005(10)
C21 0.0294(13) 0.0304(11) 0.0436(13) 0.0024(9) 0.0067(10) -0.0019(9)
C22 0.0323(13) 0.0335(11) 0.0264(11) -0.0034(9) 0.0068(9) -0.0030(9)
C23 0.0331(13) 0.0307(11) 0.0301(11) -0.0013(9) 0.0044(9) -0.0020(9)
C24 0.0410(15) 0.0389(13) 0.0399(13) -0.0007(11) 0.0124(11) 0.0044(10)
C25 0.0573(18) 0.0395(13) 0.0396(14) 0.0059(12) 0.0129(12) 0.0093(11)
C26 0.0428(15) 0.0376(13) 0.0355(12) 0.0097(11) 0.0001(11) -0.0015(10)
C27 0.0330(14) 0.0442(13) 0.0386(13) 0.0004(11) 0.0051(10) -0.0018(10)
C28 0.0351(14) 0.0384(12) 0.0337(12) -0.0024(10) 0.0057(10) 0.0042(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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
C2 O1 C11 . . 119.16(19) ?
C7 O2 C13 . . 119.96(19) ?
C2 C1 C9 . . 119.5(2) ?
C2 C1 C15 . . 116.8(2) ?
C9 C1 C15 . . 122.8(2) ?
O1 C2 C1 . . 115.1(2) ?
O1 C2 C3 . . 122.8(2) ?
C1 C2 C3 . . 122.1(2) ?
C4 C3 C2 . . 118.9(2) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
C3 C4 C10 . . 121.4(2) ?
C3 C4 H4 . . 119.3 ?
C10 C4 H4 . . 119.3 ?
C6 C5 C10 . . 122.1(2) ?
C6 C5 H5 . . 119.0 ?
C10 C5 H5 . . 119.0 ?
C5 C6 C7 . . 118.9(2) ?
C5 C6 H6 . . 120.5 ?
C7 C6 H6 . . 120.5 ?
O2 C7 C8 . . 116.2(2) ?
O2 C7 C6 . . 122.4(2) ?
C8 C7 C6 . . 121.4(2) ?
C7 C8 C9 . . 119.9(2) ?
C7 C8 C22 . . 117.7(2) ?
C9 C8 C22 . . 121.5(2) ?
C1 C9 C10 . . 117.9(2) ?
C1 C9 C8 . . 124.1(2) ?
C10 C9 C8 . . 118.1(2) ?
C4 C10 C5 . . 120.3(2) ?
C4 C10 C9 . . 120.1(2) ?
C5 C10 C9 . . 119.6(2) ?
O1 C11 C12 . . 106.0(2) ?
O1 C11 H11A . . 110.5 ?
C12 C11 H11A . . 110.5 ?
O1 C11 H11B . . 110.5 ?
C12 C11 H11B . . 110.5 ?
H11A C11 H11B . . 108.7 ?
C11 C12 H12A . . 106(2) ?
C11 C12 H12B . . 111(2) ?
H12A C12 H12B . . 108(3) ?
C11 C12 H12C . . 109(2) ?
H12A C12 H12C . . 114(3) ?
H12B C12 H12C . . 109(3) ?
O2 C13 C14 . . 106.2(2) ?
O2 C13 H13A . . 110.5 ?
C14 C13 H13A . . 110.5 ?
O2 C13 H13B . . 110.5 ?
C14 C13 H13B . . 110.5 ?
H13A C13 H13B . . 108.7 ?
C13 C14 H14A . . 116(2) ?
C13 C14 H14B . . 112(3) ?
H14A C14 H14B . . 105(3) ?
C13 C14 H14C . . 108(2) ?
H14A C14 H14C . . 107(3) ?
H14B C14 H14C . . 109(3) ?
O3 C15 C16 . . 121.0(2) ?
O3 C15 C1 . . 119.2(2) ?
C16 C15 C1 . . 119.8(2) ?
C17 C16 C21 . . 119.4(2) ?
C17 C16 C15 . . 119.5(2) ?
C21 C16 C15 . . 121.0(2) ?
C16 C17 C18 . . 120.0(2) ?
C16 C17 H17 . . 120.0 ?
C18 C17 H17 . . 120.0 ?
C19 C18 C17 . . 118.9(2) ?
C19 C18 H18 . . 120.6 ?
C17 C18 H18 . . 120.6 ?
C18 C19 C20 . . 122.0(2) ?
C18 C19 Br1 . . 119.22(18) ?
C20 C19 Br1 . . 118.8(2) ?
C21 C20 C19 . . 118.5(2) ?
C21 C20 H20 . . 120.8 ?
C19 C20 H20 . . 120.8 ?
C20 C21 C16 . . 121.2(2) ?
C20 C21 H21 . . 119.4 ?
C16 C21 H21 . . 119.4 ?
O4 C22 C23 . . 120.8(2) ?
O4 C22 C8 . . 118.3(2) ?
C23 C22 C8 . . 120.9(2) ?
C24 C23 C28 . . 119.3(2) ?
C24 C23 C22 . . 119.1(2) ?
C28 C23 C22 . . 121.6(2) ?
C25 C24 C23 . . 120.4(2) ?
C25 C24 H24 . . 119.8 ?
C23 C24 H24 . . 119.8 ?
C26 C25 C24 . . 119.1(2) ?
C26 C25 H25 . . 120.5 ?
C24 C25 H25 . . 120.5 ?
C25 C26 C27 . . 122.1(2) ?
C25 C26 Br2 . . 118.88(19) ?
C27 C26 Br2 . . 119.0(2) ?
C26 C27 C28 . . 118.1(2) ?
C26 C27 H27 . . 120.9 ?
C28 C27 H27 . . 120.9 ?
C27 C28 C23 . . 120.9(2) ?
C27 C28 H28 . . 119.6 ?
C23 C28 H28 . . 119.6 ?
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
Br1 C19 . 1.901(2) ?
Br2 C26 . 1.901(3) ?
O1 C2 . 1.367(3) ?
O1 C11 . 1.434(3) ?
O2 C7 . 1.358(3) ?
O2 C13 . 1.434(3) ?
O3 C15 . 1.221(3) ?
O4 C22 . 1.220(3) ?
C1 C2 . 1.390(3) ?
C1 C9 . 1.428(3) ?
C1 C15 . 1.501(3) ?
C2 C3 . 1.403(3) ?
C3 C4 . 1.370(3) ?
C3 H3 . 0.9500 ?
C4 C10 . 1.410(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.357(4) ?
C5 C10 . 1.417(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.424(3) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.389(3) ?
C8 C9 . 1.432(3) ?
C8 C22 . 1.507(3) ?
C9 C10 . 1.429(3) ?
C11 C12 . 1.503(4) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 H12A . 0.97(5) ?
C12 H12B . 0.96(4) ?
C12 H12C . 0.99(4) ?
C13 C14 . 1.498(4) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14A . 0.95(4) ?
C14 H14B . 0.87(4) ?
C14 H14C . 0.94(4) ?
C15 C16 . 1.489(3) ?
C16 C17 . 1.388(3) ?
C16 C21 . 1.389(3) ?
C17 C18 . 1.390(4) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.379(4) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.381(3) ?
C20 C21 . 1.373(3) ?
C20 H20 . 0.9500 ?
C21 H21 . 0.9500 ?
C22 C23 . 1.486(3) ?
C23 C24 . 1.389(3) ?
C23 C28 . 1.392(4) ?
C24 C25 . 1.382(4) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.380(4) ?
C25 H25 . 0.9500 ?
C26 C27 . 1.382(4) ?
C27 C28 . 1.390(4) ?
C27 H27 . 0.9500 ?
C28 H28 . 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_D
_geom_hbond_site_symmetry_H
_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
C20 H20 O3 1_555 1_555 1_655 0.95 2.41 3.339(3) 167 y
C27 H27 O4 1_555 1_555 1_455 0.95 2.50 3.439(3) 170 y
C11 H11B Cg2 1_555 1_555 4_576 0.99 2.75 3.632(3) 148 y
C11 H13B Cg5 1_555 1_555 4_576 0.99 2.89 3.838(3) 162 y
C14 H14C Cg2 1_555 1_555 4_575 0.98 2.78(4) 3.631(3) 151(3) y
C14 H14C Cg5 1_555 1_555 4_575 0.98 2.85(4) 3.632(3) 141(3) y
C12 H12A Br1 1_555 1_555 3_776 0.97(4) 2.82(5) 3.634(4) 141(3) y
C26 Br2 Cg3 1_555 1_555 3_575 1.901(3) 3.8749(11) 5.626(3) 152.17(9) y
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
C11 O1 C2 C1 . . . . -178.5(2) ?
C11 O1 C2 C3 . . . . 4.0(3) ?
C9 C1 C2 O1 . . . . -176.65(19) ?
C15 C1 C2 O1 . . . . -7.0(3) ?
C9 C1 C2 C3 . . . . 0.9(3) ?
C15 C1 C2 C3 . . . . 170.5(2) ?
O1 C2 C3 C4 . . . . 174.1(2) ?
C1 C2 C3 C4 . . . . -3.3(4) ?
C2 C3 C4 C10 . . . . 2.2(4) ?
C10 C5 C6 C7 . . . . 1.5(4) ?
C13 O2 C7 C8 . . . . -176.9(2) ?
C13 O2 C7 C6 . . . . 5.8(4) ?
C5 C6 C7 O2 . . . . 176.3(2) ?
C5 C6 C7 C8 . . . . -0.8(4) ?
O2 C7 C8 C9 . . . . -179.3(2) ?
C6 C7 C8 C9 . . . . -2.0(4) ?
O2 C7 C8 C22 . . . . -10.2(3) ?
C6 C7 C8 C22 . . . . 167.1(2) ?
C2 C1 C9 C10 . . . . 2.5(3) ?
C15 C1 C9 C10 . . . . -166.5(2) ?
C2 C1 C9 C8 . . . . -178.6(2) ?
C15 C1 C9 C8 . . . . 12.5(3) ?
C7 C8 C9 C1 . . . . -175.0(2) ?
C22 C8 C9 C1 . . . . 16.3(3) ?
C7 C8 C9 C10 . . . . 4.0(3) ?
C22 C8 C9 C10 . . . . -164.7(2) ?
C3 C4 C10 C5 . . . . -178.0(2) ?
C3 C4 C10 C9 . . . . 1.2(4) ?
C6 C5 C10 C4 . . . . 179.8(2) ?
C6 C5 C10 C9 . . . . 0.5(4) ?
C1 C9 C10 C4 . . . . -3.5(3) ?
C8 C9 C10 C4 . . . . 177.4(2) ?
C1 C9 C10 C5 . . . . 175.8(2) ?
C8 C9 C10 C5 . . . . -3.3(3) ?
C2 O1 C11 C12 . . . . 179.0(2) ?
C7 O2 C13 C14 . . . . 173.3(2) ?
C2 C1 C15 O3 . . . . -114.3(2) ?
C9 C1 C15 O3 . . . . 54.9(3) ?
C2 C1 C15 C16 . . . . 64.1(3) ?
C9 C1 C15 C16 . . . . -126.6(2) ?
O3 C15 C16 C17 . . . . 23.4(3) ?
C1 C15 C16 C17 . . . . -155.0(2) ?
O3 C15 C16 C21 . . . . -155.7(2) ?
C1 C15 C16 C21 . . . . 25.9(3) ?
C21 C16 C17 C18 . . . . -0.5(4) ?
C15 C16 C17 C18 . . . . -179.5(2) ?
C16 C17 C18 C19 . . . . 1.5(4) ?
C17 C18 C19 C20 . . . . -1.1(4) ?
C17 C18 C19 Br1 . . . . 178.12(18) ?
C18 C19 C20 C21 . . . . -0.3(4) ?
Br1 C19 C20 C21 . . . . -179.53(19) ?
C19 C20 C21 C16 . . . . 1.3(4) ?
C17 C16 C21 C20 . . . . -1.0(4) ?
C15 C16 C21 C20 . . . . 178.1(2) ?
C7 C8 C22 O4 . . . . -118.5(2) ?
C9 C8 C22 O4 . . . . 50.5(3) ?
C7 C8 C22 C23 . . . . 59.3(3) ?
C9 C8 C22 C23 . . . . -131.8(2) ?
O4 C22 C23 C24 . . . . 23.3(3) ?
C8 C22 C23 C24 . . . . -154.3(2) ?
O4 C22 C23 C28 . . . . -155.5(2) ?
C8 C22 C23 C28 . . . . 26.8(3) ?
C28 C23 C24 C25 . . . . -2.4(4) ?
C22 C23 C24 C25 . . . . 178.8(2) ?
C23 C24 C25 C26 . . . . 1.9(4) ?
C24 C25 C26 C27 . . . . 0.5(4) ?
C24 C25 C26 Br2 . . . . -179.1(2) ?
C25 C26 C27 C28 . . . . -2.5(4) ?
Br2 C26 C27 C28 . . . . 177.15(18) ?
C26 C27 C28 C23 . . . . 2.0(4) ?
C24 C23 C28 C27 . . . . 0.4(4) ?
C22 C23 C28 C27 . . . . 179.2(2) ?