#------------------------------------------------------------------------------
#$Date: 2024-05-04 04:52:17 +0300 (Sat, 04 May 2024) $
#$Revision: 291490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023116.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_2023116
loop_
_publ_author_name
'Gorbunov, Alexander'
'Bezzubov, Stanislav'
'Malakhova, Maria'
'Kovalev, Vladimir'
'Vatsouro, Ivan'
_publ_section_title
;
Synthesis and crystal structures of
5,17-dibromo-26,28-dihydroxy-25,27-dipropynyloxycalix[4]arene,
5,17-dibromo-26,28-dipropoxy-25,27-dipropynyloxycalix[4]arene and
25,27-bis(2-azidoethoxy)-5,17-dibromo-26,28-dihydroxycalix[4]arene
;
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024003785
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C32 H28 Br2 N6 O4'
_chemical_formula_moiety 'C32 H28 Br2 N6 O4'
_chemical_formula_sum 'C32 H28 Br2 N6 O4'
_chemical_formula_weight 720.42
_chemical_name_systematic
;
25,27-Bis(2-azidoethoxy)-5,17-dibromo-26,28-dihydroxycalix[4]arene
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_Hall '-R 3'
_space_group_name_H-M_alt 'R -3 :H'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 18
_cell_length_a 36.3261(7)
_cell_length_b 36.3261(7)
_cell_length_c 12.1054(4)
_cell_measurement_reflns_used 9927
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 28.311
_cell_measurement_theta_min 2.243
_cell_volume 13834.0(6)
_computing_cell_refinement
;
APEX3 (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker PHOTON III CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0473
_diffrn_reflns_av_unetI/netI 0.0353
_diffrn_reflns_limit_h_max 48
_diffrn_reflns_limit_h_min -47
_diffrn_reflns_limit_k_max 48
_diffrn_reflns_limit_k_min -48
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 45251
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.499
_diffrn_reflns_theta_min 1.802
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.4
_diffrn_source_power 0.07
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.685
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.5158
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.557
_exptl_crystal_description block
_exptl_crystal_F_000 6552
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.298
_refine_diff_density_min -1.122
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 399
_refine_ls_number_reflns 7804
_refine_ls_number_restraints 24
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0584
_refine_ls_R_factor_gt 0.0397
_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^)+(0.0383P)^2^+55.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0901
_refine_ls_wR_factor_ref 0.0974
_reflns_number_gt 6043
_reflns_number_total 7804
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5716.cif
_cod_data_source_block 3
_cod_original_cell_volume 13834.0(7)
_cod_original_sg_symbol_H-M 'R -3'
_cod_database_code 2023116
_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 0.437
_shelx_estimated_absorpt_t_max 0.775
_shelx_hkl_file
;
3 0 0 134.79 3.90
0 -3 0 135.59 4.80
3 -3 0 136.59 4.00
3 -3 0 131.29 4.20
2 2 0 20.90 1.70
2 -4 0 18.10 1.30
-4 2 0 21.00 1.50
2 2 0 22.20 1.30
2 -4 0 17.50 1.30
-2 -2 0 18.30 1.40
-2 4 0 20.40 1.50
4 -2 0 19.90 1.10
-2 4 0 21.60 1.40
4 -2 0 19.70 1.50
-5 1 0 352.96 9.40
4 -5 0 355.46 9.90
4 -5 0 340.37 9.70
1 4 0 316.17 9.70
1 4 0 351.66 9.80
-1 -4 0 332.07 9.80
-1 -4 0 349.27 9.80
-4 5 0 346.47 9.90
5 -1 0 358.46 10.00
5 -1 0 357.46 9.40
-4 5 0 330.07 9.70
-5 4 0 7.60 1.10
4 1 0 8.30 1.30
1 -5 0 8.10 1.40
1 -5 0 8.10 1.20
-5 4 0 6.40 1.30
4 1 0 7.40 1.40
5 -4 0 6.70 1.00
5 -4 0 6.60 1.30
-4 -1 0 8.20 1.40
-4 -1 0 8.70 1.30
-1 5 0 5.90 1.20
-1 5 0 9.50 1.40
-6 3 0 11.80 1.80
3 -6 0 13.50 1.60
3 3 0 15.00 1.60
3 -6 0 12.20 1.60
3 3 0 11.20 1.60
-3 6 0 12.10 1.60
-3 6 0 12.20 1.60
6 -3 0 9.90 1.60
-3 -3 0 15.10 1.60
6 -3 0 12.20 1.20
-3 -3 0 12.90 1.70
0 -6 0 28.20 2.30
-6 6 0 28.60 2.50
0 -6 0 32.50 2.60
6 0 0 32.60 2.70
-6 6 0 31.30 2.30
6 0 0 31.30 2.50
6 -6 0 27.90 2.20
0 6 0 29.50 2.40
0 6 0 29.10 2.40
-6 0 0 25.80 2.50
6 -6 0 29.20 2.60
-6 0 0 26.00 2.20
2 5 0 2.40 1.40
5 -7 0 2.40 1.40
-7 2 0 3.10 1.50
-7 2 0 2.60 1.40
2 5 0 0.30 1.20
-5 7 0 0.60 1.30
-5 7 0 1.20 1.30
7 -2 0 1.60 1.10
-2 -5 0 1.20 1.40
-2 -5 0 1.60 1.30
7 -2 0 -0.80 1.50
2 -7 0 130.79 5.00
-7 5 0 128.79 5.00
-7 5 0 121.79 4.40
2 -7 0 108.89 4.60
5 2 0 148.79 4.50
5 2 0 130.09 4.80
-2 7 0 131.29 5.00
7 -5 0 123.69 5.00
-5 -2 0 117.39 4.80
7 -5 0 120.69 4.30
-2 7 0 125.99 4.90
7 -8 0 820.42 22.30
1 7 0 844.12 22.60
-8 1 0 829.72 21.90
7 -8 0 840.42 22.80
1 7 0 789.72 22.60
-8 1 0 840.92 22.90
-7 8 0 825.62 22.70
-7 8 0 834.52 22.40
8 -1 0 819.92 22.80
-1 -7 0 793.12 22.50
8 -1 0 838.82 22.00
-1 -7 0 815.02 22.60
4 4 0 267.27 8.00
4 -8 0 248.98 8.30
4 4 0 260.07 8.40
-8 4 0 267.37 8.70
-8 4 0 258.57 7.80
4 -8 0 258.37 8.30
8 -4 0 270.57 8.60
-4 8 0 273.77 8.40
8 -4 0 257.37 7.50
-4 8 0 264.77 8.50
-4 -4 0 239.18 8.30
-8 7 0 6139.79 152.88
1 -8 0 5937.01 152.68
7 1 0 6106.19 152.18
7 1 0 6099.59 152.78
1 -8 0 6040.50 152.58
-8 7 0 5922.31 152.18
-7 -1 0 6107.59 151.98
8 -7 0 6032.80 152.08
8 -7 0 5902.81 152.78
-1 8 0 6015.20 152.58
-7 -1 0 5967.50 152.78
-1 8 0 5962.50 152.68
3 6 0 5239.68 134.99
-9 3 0 5328.57 134.19
-9 3 0 5329.27 135.29
6 -9 0 5176.88 134.79
3 6 0 5453.65 134.79
-3 -6 0 4792.92 134.89
-6 9 0 5309.67 134.89
-6 9 0 5299.97 135.19
-3 -6 0 5475.95 134.89
-6 9 0 5540.35 135.09
9 -3 0 5404.16 133.99
9 -3 0 5376.56 135.29
6 3 0 5204.88 131.29
-9 6 0 5231.78 131.39
-9 6 0 5267.57 132.29
3 -9 0 5297.57 131.99
3 -9 0 5154.98 131.99
6 3 0 5171.08 131.79
6 3 0 5219.88 132.09
9 -6 0 5170.28 132.29
9 -6 0 5300.87 131.09
-3 9 0 5114.69 132.09
-6 -3 0 4954.50 131.99
-3 9 0 5199.28 131.99
-9 9 0 3221.98 82.69
-9 9 0 3159.28 81.99
0 -9 0 2994.80 82.29
0 -9 0 3210.98 82.49
9 0 0 3323.77 81.89
9 0 0 3260.07 82.79
9 -9 0 3258.77 82.79
0 9 0 3058.89 82.39
-9 0 0 3214.38 82.69
-9 0 0 3223.58 81.49
0 9 0 3262.27 82.39
9 -9 0 3220.08 81.89
-10 2 0 2077.59 53.09
-10 2 0 2078.19 54.39
2 8 0 2100.39 53.99
8 -10 0 2016.80 53.69
2 8 0 1914.31 53.89
8 -10 0 2125.39 54.39
-8 10 0 2071.59 53.89
-2 -8 0 2043.90 54.09
-8 10 0 2122.29 54.29
10 -2 0 2073.89 54.39
-2 -8 0 2067.19 53.99
10 -2 0 2092.59 53.09
5 -10 0 1316.87 35.10
5 -10 0 1278.77 35.00
-10 5 0 1300.27 35.50
-10 5 0 1343.47 34.40
5 5 0 1371.46 34.70
5 5 0 1276.37 35.10
10 -5 0 1340.77 35.40
-5 -5 0 1238.78 35.10
10 -5 0 1316.47 34.00
-5 10 0 1319.57 35.30
-5 10 0 1340.27 35.20
8 2 0 1343.07 35.40
8 2 0 1331.17 34.80
2 -10 0 1347.37 35.40
-10 8 0 1330.77 35.50
-10 8 0 1289.77 34.60
2 -10 0 1302.67 35.10
8 2 0 1319.37 34.20
10 -8 0 1361.56 35.60
10 -8 0 1302.37 34.40
-2 10 0 1299.97 35.20
-2 10 0 1187.38 35.00
10 -11 0 3.50 2.00
1 10 0 4.30 2.20
1 10 0 0.30 2.00
-11 1 0 4.40 2.20
-11 1 0 1.40 1.70
10 -11 0 2.00 2.40
11 -1 0 5.00 2.00
-10 11 0 2.60 2.00
-1 -10 0 0.00 1.80
-10 11 0 1.10 1.80
-1 -10 0 3.20 2.50
7 -11 0 202.78 7.70
4 7 0 199.18 7.70
4 7 0 216.58 7.50
-11 4 0 207.78 6.90
-11 4 0 228.58 8.30
-7 11 0 203.88 7.70
-4 -7 0 209.58 7.70
11 -4 0 220.78 8.30
11 -4 0 203.28 6.60
-7 11 0 214.68 7.70
-7 11 0 196.98 7.90
-4 -7 0 218.78 7.90
-11 7 0 5188.58 133.59
4 -11 0 5364.16 134.29
7 4 0 5376.36 133.39
7 4 0 5333.57 132.49
4 -11 0 5067.99 133.19
-11 7 0 5158.08 132.49
7 4 0 5256.37 133.09
-4 11 0 5294.27 133.49
11 -7 0 5228.78 134.59
-7 -4 0 4951.60 133.29
-4 11 0 5281.47 133.39
11 -7 0 5188.68 132.09
10 1 0 1885.61 49.60
-11 10 0 1845.42 48.70
10 1 0 1915.71 48.80
1 -11 0 1802.42 49.10
-11 10 0 1874.81 49.60
1 -11 0 1817.42 49.30
-1 11 0 1894.01 49.30
11 -10 0 1871.31 49.60
-1 11 0 1788.62 49.20
11 -10 0 1833.42 48.40
-10 -1 0 1831.82 49.50
-10 -1 0 1923.41 48.30
3 9 0 160.58 6.90
9 -12 0 160.28 6.60
-12 3 0 160.08 5.90
-12 3 0 167.78 7.30
3 9 0 164.58 6.70
-9 12 0 159.88 6.80
12 -3 0 151.28 7.00
-9 12 0 151.58 6.60
12 -3 0 161.28 5.70
-3 -9 0 151.68 6.60
6 -12 0 582.24 17.70
-12 6 0 604.54 18.00
6 6 0 604.84 17.00
6 6 0 590.34 17.60
-12 6 0 601.24 16.70
6 6 0 582.84 17.60
-6 -6 0 529.75 17.40
12 -6 0 592.24 17.90
-6 12 0 619.24 17.90
12 -6 0 609.64 16.30
-6 12 0 606.54 17.60
-12 9 0 1456.45 38.00
3 -12 0 1454.75 38.60
-12 9 0 1420.06 38.90
3 -12 0 1386.66 38.70
9 3 0 1467.85 37.60
9 3 0 1475.35 38.80
9 3 0 1428.06 38.20
12 -9 0 1413.06 37.50
-9 -3 0 1430.16 38.80
12 -9 0 1414.46 38.90
-3 12 0 1345.17 38.60
-3 12 0 1467.95 38.70
0 -12 0 1116.79 31.10
-12 12 0 1129.69 31.50
0 -12 0 1125.29 31.30
12 0 0 1102.39 31.40
12 0 0 1118.29 30.40
-12 12 0 1120.49 30.70
12 -12 0 1102.49 30.40
0 12 0 1125.39 31.30
0 12 0 1153.18 31.20
-12 0 0 1096.69 29.90
12 -12 0 1131.29 31.60
2 11 0 2354.46 68.49
2 11 0 2715.23 68.69
11 -13 0 2616.24 69.19
-13 2 0 2614.44 67.29
11 -13 0 2672.03 69.19
-13 2 0 2667.73 69.29
-2 -11 0 2497.65 68.59
-11 13 0 2552.14 68.39
13 -2 0 2594.04 68.99
-2 -11 0 2692.23 68.89
13 -2 0 2768.32 67.59
-11 13 0 2691.03 68.99
5 8 0 3531.05 89.09
8 -13 0 3347.06 89.19
-13 5 0 3396.66 88.29
5 8 0 3487.35 89.49
-13 5 0 3473.05 89.99
-5 -8 0 3278.47 89.39
13 -5 0 3406.76 87.89
13 -5 0 3408.96 89.79
-8 13 0 3408.36 89.39
-8 13 0 3675.43 91.09
-8 13 0 3425.66 89.49
-5 -8 0 3631.94 89.59
5 -13 0 7.80 2.80
-13 8 0 3.70 2.00
8 5 0 0.30 2.40
8 5 0 5.80 2.60
5 -13 0 4.30 2.00
-13 8 0 5.10 2.60
8 5 0 5.10 2.00
13 -8 0 4.80 2.40
-8 -5 0 5.10 2.20
-5 13 0 3.80 2.30
13 -8 0 3.10 1.70
-5 13 0 3.50 2.30
2 -13 0 270.17 10.00
11 2 0 267.07 10.10
-13 11 0 253.57 9.10
2 -13 0 236.88 9.30
11 2 0 270.67 9.50
11 2 0 262.87 8.40
-2 13 0 271.87 9.90
13 -11 0 253.27 9.90
13 -11 0 251.17 8.70
1 13 0 -1.50 2.80
13 -14 0 -0.10 2.60
1 13 0 -0.20 2.50
-14 1 0 -2.20 3.00
13 -14 0 9.50 3.10
-14 1 0 -2.80 2.20
-13 14 0 -1.20 2.40
-13 14 0 0.50 2.80
-1 -13 0 1.00 3.10
-1 -13 0 -4.50 2.00
14 -1 0 4.60 2.60
14 -1 0 3.80 3.30
-14 4 0 1065.49 28.80
4 10 0 1092.09 29.70
4 10 0 977.40 29.80
10 -14 0 1086.09 29.80
-4 -10 0 1106.59 30.20
14 -4 0 1098.49 28.50
-10 14 0 1098.39 30.20
14 -4 0 1089.39 30.50
-10 14 0 1046.60 30.40
-4 -10 0 994.50 29.90
-10 14 0 1096.89 30.00
7 7 0 77.09 5.20
7 7 0 94.49 6.00
7 -14 0 86.69 5.50
-14 7 0 84.79 4.60
7 7 0 87.69 4.70
-7 14 0 74.79 5.30
-7 -7 0 78.39 5.30
14 -7 0 76.89 5.50
14 -7 0 79.79 3.90
-7 14 0 90.09 5.50
10 4 0 230.38 9.20
-14 10 0 223.08 8.20
10 4 0 236.58 9.00
10 4 0 213.18 7.60
4 -14 0 205.98 9.00
4 -14 0 228.78 8.70
-14 10 0 201.58 9.00
-4 14 0 223.88 8.80
14 -10 0 198.58 9.10
-10 -4 0 226.98 9.00
14 -10 0 218.68 7.60
-14 13 0 229.88 9.60
1 -14 0 227.58 9.10
1 -14 0 230.98 9.70
13 1 0 229.38 9.90
-14 13 0 218.08 8.90
13 1 0 241.68 9.20
14 -13 0 206.08 9.40
-1 14 0 213.38 9.20
14 -13 0 227.38 9.20
-1 14 0 236.58 9.30
12 -15 0 1.80 2.80
-15 3 0 10.90 2.90
3 12 0 2.20 2.60
3 12 0 2.70 2.80
-15 3 0 5.90 3.40
15 -3 0 2.40 3.20
-3 -12 0 -0.90 2.40
-12 15 0 2.40 2.70
15 -3 0 2.40 2.40
-3 -12 0 1.30 3.20
-12 15 0 2.70 2.80
6 9 0 655.13 21.30
-15 6 0 672.13 20.80
6 9 0 677.53 19.70
-15 6 0 674.73 19.00
9 -15 0 651.33 20.10
-9 15 0 688.33 21.30
15 -6 0 659.43 18.30
-9 15 0 683.63 20.60
-6 -9 0 657.63 20.20
15 -6 0 660.43 20.60
-9 15 0 674.93 20.20
9 6 0 184.48 8.60
9 6 0 198.38 8.70
6 -15 0 189.48 8.70
9 6 0 204.18 7.50
6 -15 0 212.68 8.40
-15 9 0 186.18 8.80
-15 9 0 191.68 7.70
-6 15 0 187.28 8.30
-6 15 0 208.88 8.80
15 -9 0 191.88 8.70
15 -9 0 190.88 6.90
-9 -6 0 192.88 8.50
3 -15 0 460.35 15.70
3 -15 0 470.55 15.30
12 3 0 482.35 13.90
12 3 0 470.95 15.70
-15 12 0 470.55 15.80
12 3 0 471.75 15.30
-15 12 0 467.65 14.90
-3 15 0 457.05 15.50
-12 -3 0 483.25 16.90
15 -12 0 481.85 15.90
-3 15 0 466.15 15.50
15 -12 0 466.75 14.20
15 0 0 72.29 6.50
15 0 0 80.89 6.00
0 -15 0 71.39 6.60
-15 15 0 85.49 6.00
0 -15 0 76.99 5.50
-15 15 0 71.89 6.00
-15 0 0 81.79 6.50
0 15 0 76.09 6.00
15 -15 0 78.19 6.30
0 15 0 79.69 6.00
15 -15 0 64.29 5.60
14 -16 0 186.08 8.50
2 14 0 187.28 8.60
-16 2 0 196.38 9.50
-16 2 0 178.08 7.40
14 -16 0 182.88 9.00
2 14 0 179.28 8.60
16 -2 0 175.68 9.00
-14 16 0 186.88 9.40
-2 -14 0 169.68 8.10
-2 -14 0 176.38 9.00
16 -2 0 200.58 7.60
-14 16 0 175.28 8.70
11 -16 0 215.48 9.40
-16 5 0 224.98 8.50
5 11 0 230.88 9.80
5 11 0 236.38 9.60
-16 5 0 218.58 10.20
-5 -11 0 222.88 9.50
-11 16 0 227.78 9.80
-5 -11 0 240.78 9.80
16 -5 0 221.28 10.00
16 -5 0 222.98 7.70
-11 16 0 231.18 9.50
-11 16 0 211.78 9.20
8 -16 0 26.10 4.30
8 8 0 20.10 4.50
8 8 0 18.80 3.80
8 8 0 24.20 3.60
-16 8 0 17.80 4.20
-16 8 0 22.70 3.40
-8 -8 0 22.50 3.70
-8 16 0 15.50 3.60
-8 16 0 22.20 3.90
-8 16 0 28.00 3.70
16 -8 0 25.70 4.40
16 -8 0 22.50 2.60
5 -16 0 724.33 21.80
11 5 0 759.22 22.10
11 5 0 743.63 22.40
11 5 0 733.13 20.70
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8 -15 -7 42.40 8.20
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8 1 16 62.49 12.40
2 6 -16 -8.00 12.50
6 -8 -16 -3.70 12.40
-8 2 -16 2.30 12.20
-6 8 16 23.00 9.70
8 -2 16 -17.40 13.30
-8 5 -16 122.89 18.80
3 -8 -16 142.89 19.10
5 3 -16 119.49 19.00
-3 8 16 127.59 15.20
8 -5 16 117.89 13.80
8 0 -16 21.00 23.40
-8 8 -16 17.00 14.10
0 -8 -16 20.20 13.20
0 8 16 51.69 12.10
8 -8 16 30.60 10.00
11 -3 -16 25.50 16.50
-8 11 -16 34.70 14.50
-3 -8 -16 13.40 13.60
3 8 16 20.10 11.50
-11 3 16 25.10 11.50
14 -6 -16 18.80 14.70
-8 14 -16 7.60 14.90
-6 -8 -16 13.30 12.70
6 8 16 24.60 11.60
-14 6 16 13.70 10.80
17 -9 -16 4.10 12.40
-9 -8 -16 12.90 10.90
-17 9 16 -4.20 11.20
9 8 16 8.20 11.00
-9 -5 -16 8.40 11.90
-5 14 -16 -5.40 14.50
14 -9 -16 16.60 14.40
9 5 16 10.80 11.00
-9 -2 -16 22.40 12.50
-2 11 -16 -12.20 14.00
11 -9 -16 -10.60 13.40
-11 9 16 4.10 11.30
9 2 16 7.90 10.00
-9 1 -16 7.00 12.10
1 8 -16 9.20 14.50
8 -9 -16 -2.40 12.50
9 -1 16 10.40 10.00
-8 9 16 22.90 9.70
4 5 -16 5.00 13.80
-9 4 -16 -19.80 11.20
5 -9 -16 -6.60 12.20
-5 9 16 15.10 10.00
9 -4 16 19.40 10.40
7 2 -16 28.30 19.90
2 -9 -16 10.50 12.70
-9 7 -16 0.20 12.20
9 -7 16 -4.20 9.80
-2 9 16 14.90 10.10
-1 -9 -16 45.10 14.30
10 -1 -16 65.99 27.10
-9 10 -16 38.70 14.80
1 9 16 60.49 12.80
-4 -9 -16 5.20 12.50
-9 13 -16 1.40 14.00
13 -4 -16 -13.30 13.30
4 9 16 16.30 11.20
-7 -9 -16 27.80 13.60
-9 16 -16 9.00 15.50
16 -7 -16 39.90 15.10
7 9 16 50.29 12.60
-16 7 16 59.79 13.00
-9 19 -16 65.89 19.50
19 -10 -16 23.10 15.80
-10 -9 -16 54.09 13.90
10 9 16 43.50 14.70
-19 10 16 39.00 12.40
16 -10 -16 28.90 14.80
-10 -6 -16 7.80 11.40
10 6 16 16.00 11.50
-16 10 16 7.00 10.70
13 -10 -16 0.30 13.10
-10 -3 -16 -20.10 11.30
-3 13 -16 -36.80 16.70
10 3 16 7.90 10.70
-13 10 16 8.80 9.60
0 10 -16 124.99 23.10
-10 0 -16 108.39 16.40
-10 10 16 112.69 14.50
10 0 16 140.49 16.00
3 7 -16 53.99 18.30
-10 3 -16 60.09 14.60
7 -10 -16 46.90 14.60
-7 10 16 71.69 12.30
10 -3 16 40.10 11.20
4 -10 -16 28.10 14.10
-10 6 -16 61.79 15.70
10 -6 16 28.70 10.80
-4 10 16 36.70 11.10
1 -10 -16 -35.60 11.00
-10 9 -16 5.90 13.20
10 -9 16 0.10 9.30
-1 10 16 4.50 10.20
12 -2 -16 36.40 15.60
-10 12 -16 38.20 13.60
-2 -10 -16 25.60 12.60
2 10 16 25.40 11.60
15 -5 -16 1.40 13.80
-5 -10 -16 3.70 11.80
-10 15 -16 20.00 14.20
5 10 16 12.80 11.50
18 -8 -16 15.40 14.70
-8 -10 -16 7.30 12.60
-18 8 16 6.60 15.50
8 10 16 30.50 13.40
-11 -7 -16 42.50 13.30
-7 18 -16 87.89 19.80
18 -11 -16 32.70 15.30
11 7 16 76.09 14.60
-18 11 16 45.80 12.20
-11 -4 -16 25.50 12.10
-4 15 -16 18.80 19.30
15 -11 -16 17.90 14.10
-15 11 16 16.70 10.70
11 4 16 10.40 11.80
12 -11 -16 20.90 14.30
-11 -1 -16 32.50 12.60
11 1 16 20.10 11.20
-12 11 16 31.20 10.90
-11 2 -16 19.00 12.40
11 -2 16 20.60 10.60
-9 11 16 25.10 10.60
-11 5 -16 18.70 13.30
6 -11 -16 14.40 13.50
-6 11 16 52.59 11.80
11 -5 16 26.20 11.60
8 3 -16 15.00 19.00
-11 8 -16 0.60 12.60
3 -11 -16 -7.80 12.80
-3 11 16 2.30 10.10
11 -8 16 -5.80 9.80
0 -11 -16 8.70 12.80
11 0 -16 -9.10 13.60
-11 11 -16 2.60 13.10
0 11 16 1.30 10.20
-3 -11 -16 11.60 12.70
14 -3 -16 -18.50 13.50
-11 14 -16 8.80 14.50
3 11 16 10.00 11.00
17 -6 -16 78.79 17.70
-6 -11 -16 59.79 14.60
-11 17 -16 80.49 18.60
6 11 16 74.19 15.30
17 -12 -16 30.10 15.70
-12 -5 -16 29.50 12.10
-5 17 -16 33.70 16.70
-17 12 16 26.30 11.50
12 5 16 28.60 12.90
14 -12 -16 6.70 14.10
-2 14 -16 19.50 17.10
-12 -2 -16 30.00 12.90
-14 12 16 5.30 10.30
12 2 16 28.30 11.80
-12 1 -16 -6.10 11.30
1 11 -16 16.40 17.90
11 -12 -16 28.40 14.10
12 -1 16 6.70 11.00
-11 12 16 9.50 10.40
-12 4 -16 41.60 14.10
12 -4 16 37.80 11.50
-8 12 16 13.60 10.40
7 5 -16 -25.70 12.40
5 -12 -16 -1.90 12.80
-12 7 -16 21.00 13.50
-5 12 16 8.60 10.30
12 -7 16 18.80 10.60
2 -12 -16 43.50 14.20
-12 10 -16 29.50 14.60
10 2 -16 43.30 16.10
12 -10 16 38.10 11.00
-2 12 16 28.20 11.60
-12 13 -16 16.90 13.30
13 -1 -16 35.00 16.40
-1 -12 -16 30.20 13.50
1 12 16 46.90 12.50
-4 -12 -16 31.10 13.10
-12 16 -16 56.09 17.00
16 -4 -16 44.40 15.60
4 12 16 40.70 12.60
19 -7 -16 76.59 18.90
-7 -12 -16 74.79 13.90
19 -13 -16 8.40 14.20
-13 -6 -16 5.70 12.10
-6 19 -16 -7.30 15.50
-19 13 16 4.60 10.30
13 6 16 6.80 13.00
16 -13 -16 31.90 15.90
-3 16 -16 69.39 18.80
-13 -3 -16 70.79 14.50
13 3 16 46.60 13.30
-16 13 16 73.09 13.30
-13 0 -16 18.80 12.50
13 -13 -16 26.90 14.80
0 13 -16 21.10 14.70
13 0 16 46.80 12.00
-13 13 16 28.30 11.10
10 -13 -16 10.90 13.70
-13 3 -16 15.90 11.60
3 10 -16 4.50 14.10
13 -3 16 -8.10 10.20
-10 13 16 0.40 10.70
-13 6 -16 20.90 13.30
6 7 -16 18.30 14.40
13 -6 16 5.50 10.70
-7 13 16 8.90 10.70
9 4 -16 -13.70 12.50
-13 9 -16 -8.30 12.00
4 -13 -16 31.10 17.10
-4 13 16 16.90 10.80
13 -9 16 21.30 11.00
1 -13 -16 -4.40 11.90
12 1 -16 17.00 14.30
-13 12 -16 27.90 14.70
-1 13 16 6.40 10.20
-13 15 -16 16.50 14.10
15 -2 -16 29.00 16.30
-2 -13 -16 -0.60 11.90
2 13 16 23.90 11.90
-5 -13 -16 0.20 12.00
18 -5 -16 22.10 16.40
-13 18 -16 -31.10 12.00
5 13 16 4.70 14.20
-14 -4 -16 60.29 13.00
18 -14 -16 79.19 17.40
-4 18 -16 45.80 18.60
14 4 16 47.00 13.40
-18 14 16 40.60 12.50
15 -14 -16 -16.10 12.70
-14 -1 -16 -1.90 10.90
-1 15 -16 -4.80 14.80
14 1 16 -0.70 11.00
-15 14 16 1.00 10.40
-14 2 -16 129.29 16.40
2 12 -16 93.29 20.50
12 -14 -16 127.89 19.80
-12 14 16 121.39 15.40
14 -2 16 158.98 16.80
-14 5 -16 18.80 12.80
9 -14 -16 2.80 13.30
-9 14 16 24.90 12.10
14 -5 16 29.80 11.50
-14 8 -16 5.70 13.00
6 -14 -16 -8.90 20.50
8 6 -16 4.80 14.10
-6 14 16 19.90 11.30
11 3 -16 0.70 15.90
3 -14 -16 -2.20 22.40
-14 11 -16 14.80 12.80
14 -11 16 7.60 10.60
-3 14 16 16.50 10.20
-14 14 -16 52.89 15.40
14 0 -16 84.59 18.80
0 -14 -16 62.59 15.40
0 14 16 41.20 12.50
17 -3 -16 13.40 15.30
-3 -14 -16 26.00 13.90
-14 17 -16 12.20 14.40
3 14 16 49.60 13.90
17 -15 -16 33.40 15.80
-15 -2 -16 41.60 12.30
-2 17 -16 24.00 16.90
-17 15 16 23.60 11.90
15 2 16 23.70 12.90
14 -15 -16 10.80 13.50
-15 1 -16 22.30 12.30
1 14 -16 6.20 14.60
15 -1 16 -1.10 10.40
-14 15 16 35.30 11.80
11 -15 -16 69.49 15.40
4 11 -16 57.39 16.90
-15 4 -16 84.69 15.40
15 -4 16 68.99 13.50
-11 15 16 82.49 13.50
8 -15 -16 14.10 12.40
7 8 -16 -6.40 12.20
-15 7 -16 13.40 11.90
-8 15 16 5.80 10.90
15 -7 16 -0.80 10.50
-15 10 -16 -0.30 11.70
10 5 -16 27.90 16.30
5 -15 -16 -7.70 15.70
-5 15 16 21.30 10.30
15 -10 16 9.30 11.30
13 2 -16 16.20 14.30
-15 13 -16 23.80 14.10
-2 15 16 9.00 10.50
-1 -15 -16 -7.60 21.80
-15 16 -16 0.60 12.90
16 -1 -16 5.80 14.80
1 15 16 1.60 11.60
0 16 -16 13.90 15.40
-16 0 -16 28.20 12.90
16 -16 -16 14.50 13.10
16 0 16 -2.00 11.00
-16 16 16 25.20 11.30
3 13 -16 1.10 14.20
-16 3 -16 -10.50 10.90
13 -16 -16 15.10 13.20
-13 16 16 9.40 10.80
16 -3 16 -6.30 10.20
6 10 -16 47.70 17.00
10 -16 -16 18.10 13.70
-16 6 -16 29.60 13.50
-10 16 16 49.20 13.10
16 -6 16 32.00 12.40
9 7 -16 28.90 16.90
7 -16 -16 27.50 14.50
-16 9 -16 40.90 14.50
-7 16 16 48.40 12.40
16 -9 16 52.99 11.70
12 4 -16 20.30 15.80
4 -16 -16 57.19 15.10
-16 12 -16 45.00 13.50
16 -12 16 26.50 11.20
-4 16 16 35.80 12.00
-16 15 -16 8.90 13.40
1 -16 -16 21.60 17.50
15 1 -16 32.80 15.10
-1 16 16 49.10 13.70
-16 18 -16 6.80 15.00
18 -2 -16 46.70 18.10
2 15 -16 -5.70 14.60
-17 2 -16 7.80 11.40
15 -17 -16 11.20 13.30
17 -2 16 6.00 11.40
-15 17 16 0.20 11.70
-17 5 -16 21.00 12.70
5 12 -16 -0.50 13.70
12 -17 -16 -10.40 11.70
17 -5 16 8.30 11.60
-12 17 16 16.00 10.90
8 9 -16 35.60 16.80
9 -17 -16 33.10 14.00
-17 8 -16 44.00 14.00
-9 17 16 38.80 12.70
17 -8 16 15.30 11.70
6 -17 -16 60.29 15.20
11 6 -16 14.10 14.10
-17 11 -16 44.80 14.30
-6 17 16 43.90 12.90
17 -11 16 19.40 11.90
-17 14 -16 8.80 12.40
14 3 -16 3.00 15.10
3 -17 -16 4.70 13.20
-3 17 16 -1.00 11.00
17 0 -16 -1.30 15.90
-17 17 -16 28.70 13.40
0 -17 -16 27.40 13.50
0 17 16 9.60 15.60
14 -18 -16 -18.70 12.30
-18 4 -16 24.10 12.50
4 14 -16 -16.20 13.50
-14 18 16 7.30 10.40
18 -4 16 10.50 11.50
-18 7 -16 39.30 13.40
11 -18 -16 -5.80 12.40
7 11 -16 -21.50 13.30
18 -7 16 10.60 12.00
-11 18 16 -0.70 10.70
10 8 -16 -9.80 14.30
-18 10 -16 12.70 12.40
8 -18 -16 16.50 13.70
18 -10 16 12.00 11.20
-8 18 16 -13.10 10.30
-18 13 -16 100.99 16.10
5 -18 -16 79.99 17.30
13 5 -16 65.69 18.40
-5 18 16 64.19 14.70
-18 16 -16 24.80 13.30
16 2 -16 -15.10 15.30
2 -18 -16 9.40 12.80
-19 6 -16 89.49 14.40
6 13 -16 69.79 18.60
13 -19 -16 61.09 14.90
-13 19 16 71.19 14.40
19 -6 16 37.70 13.00
9 10 -16 -12.80 13.90
-19 9 -16 -11.70 12.10
10 -19 -16 19.40 13.90
19 -9 16 26.40 12.20
-10 19 16 2.30 11.30
-19 12 -16 67.39 15.30
7 -19 -16 53.99 16.00
12 7 -16 73.99 19.20
-7 19 16 70.19 15.00
19 -12 16 44.20 12.90
0 -1 -17 23.00 13.60
-1 1 -17 16.20 15.10
1 0 -17 -12.30 13.60
0 1 17 25.50 11.30
2 -2 -17 65.49 17.50
0 2 -17 47.00 15.80
-2 0 -17 74.69 26.40
2 0 17 20.50 12.60
-2 2 17 40.80 11.40
-1 -2 -17 1.30 15.40
-2 3 -17 1.30 14.40
3 -1 -17 9.50 13.60
1 2 17 12.70 10.30
-1 4 -17 -23.10 13.10
4 -3 -17 13.00 13.80
3 1 17 14.80 10.20
-4 3 17 44.60 11.90
2 1 -17 71.99 17.10
1 -3 -17 54.99 17.10
-3 2 -17 39.10 25.70
-1 3 17 56.99 12.20
3 -2 17 58.99 15.60
5 -2 -17 -7.80 13.30
-2 -3 -17 70.19 26.40
-3 5 -17 29.10 15.90
2 3 17 38.20 11.40
6 -4 -17 -23.60 11.50
-2 6 -17 5.80 14.30
-6 4 17 21.30 11.80
4 2 17 16.30 11.20
1 3 -17 14.70 14.80
3 -4 -17 23.40 14.80
-3 4 17 24.00 11.00
4 0 -17 36.90 15.80
0 -4 -17 22.00 14.10
0 4 17 17.70 11.00
-4 7 -17 4.00 14.60
7 -3 -17 26.80 14.80
3 4 17 24.50 11.40
8 -5 -17 -8.50 13.50
-3 8 -17 7.50 15.00
-5 -3 -17 -9.20 22.40
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5 3 17 11.10 10.90
0 5 -17 24.80 15.80
-5 0 -17 2.50 17.30
5 -5 -17 14.00 14.20
-5 5 17 23.60 11.00
5 0 17 15.00 10.70
2 -5 -17 37.50 16.00
3 2 -17 3.60 14.20
-2 5 17 31.80 11.00
5 -3 17 29.00 12.70
-5 6 -17 116.79 24.10
6 -1 -17 132.69 19.60
-1 -5 -17 129.39 20.40
1 5 17 153.68 16.20
-5 9 -17 17.70 15.50
9 -4 -17 7.00 13.60
4 5 17 31.10 12.00
7 -6 -17 -1.90 12.50
-6 -1 -17 35.30 14.50
-1 7 -17 -5.30 15.00
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2 4 -17 -15.00 13.50
4 -6 -17 0.60 13.50
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6 -2 17 16.00 11.10
1 -6 -17 62.49 16.40
5 1 -17 32.60 15.70
-1 6 17 58.79 12.30
-2 -6 -17 30.10 14.50
8 -2 -17 12.70 14.30
-6 8 -17 22.30 15.20
2 6 17 39.90 12.40
-7 -2 -17 -6.30 12.10
-2 9 -17 -20.00 13.20
9 -7 -17 7.30 13.00
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-9 7 17 -0.70 10.60
1 6 -17 2.30 13.60
6 -7 -17 6.60 14.00
-7 1 -17 18.90 13.00
-6 7 17 12.90 10.60
7 -1 17 -2.60 11.30
3 -7 -17 22.50 15.20
-7 4 -17 49.50 18.60
4 3 -17 40.30 16.20
7 -4 17 38.60 14.50
-3 7 17 47.20 12.10
0 -7 -17 5.60 13.50
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8 -8 -17 -0.10 12.90
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0 8 -17 -9.90 15.10
-8 8 17 14.90 10.40
8 0 17 2.60 10.80
-8 3 -17 65.39 15.90
5 -8 -17 45.00 15.40
3 5 -17 20.20 16.30
8 -3 17 56.59 13.00
-5 8 17 47.50 11.30
-8 6 -17 7.80 14.10
6 2 -17 14.10 14.90
2 -8 -17 19.20 14.70
-2 8 17 -1.70 9.90
-9 2 -17 20.90 14.10
7 -9 -17 11.80 14.90
2 7 -17 21.20 14.10
9 -2 17 11.30 11.90
-7 9 17 8.60 10.00
5 4 -17 -1.00 13.50
-9 5 -17 -16.40 13.00
4 -9 -17 -4.60 13.30
9 -5 17 -6.90 12.10
-4 9 17 6.40 9.30
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 27373
_shelx_res_file
;
TITL mo_ga597_0m_a.res in R-3
mo_ga597_0m.res
created by SHELXL-2018/3 at 13:00:58 on 25-Mar-2024
REM Old TITL mo_GA597_0m in R-3
REM SHELXT solution in R-3
REM R1 0.130, Rweak 0.009, Alpha 0.042, Orientation as input
REM Formula found by SHELXT: C114 O13 Br6
CELL 0.71073 36.3261 36.3261 12.1054 90 90 120
ZERR 18 0.0007 0.0007 0.0004 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Br N O
UNIT 576 504 36 108 72
SIMU 0.01 0.005 2 N6 N5 N4
SIMU 0.01 0.005 2 N1 N2 N3
L.S. 7
PLAN 1
SIZE 0.1 0.13 0.37
TEMP -173.15
CONF
HTAB O3 O4
HTAB O1 O2
BOND $H
list 4
MORE -1
ABIN
fmap 2
acta
OMIT -2 57
OMIT -2 4 0
OMIT 0 3 0
OMIT -3 6 0
REM
REM
REM
WGHT 0.038300 55.034100
FVAR 0.09132
BR2 3 0.778077 0.644224 0.118445 11.00000 0.02212 0.02979 =
0.02155 0.00350 -0.00145 0.00975
BR1 3 0.947473 0.640868 1.047457 11.00000 0.02894 0.03163 =
0.04687 -0.00860 -0.00821 0.01439
O4 5 0.733440 0.533221 0.693603 11.00000 0.01827 0.02723 =
0.02532 0.00346 0.00567 0.01162
O3 5 0.767017 0.531953 0.496460 11.00000 0.03720 0.03980 =
0.02486 0.00862 0.00950 0.02727
AFIX 147
H3 2 0.754079 0.534255 0.551158 11.00000 -1.50000
AFIX 0
O1 5 0.812145 0.536261 0.715612 11.00000 0.02916 0.04235 =
0.02673 -0.00677 -0.00100 0.02491
AFIX 147
H1 2 0.821251 0.526224 0.667258 11.00000 -1.50000
AFIX 0
O2 5 0.829088 0.504911 0.526108 11.00000 0.03732 0.02884 =
0.03785 0.00505 0.01255 0.02326
C16 1 0.750077 0.606979 0.331050 11.00000 0.02186 0.02674 =
0.02436 0.00062 -0.00110 0.01352
AFIX 43
H16 2 0.735357 0.622450 0.332302 11.00000 -1.20000
AFIX 0
C15 1 0.774336 0.609622 0.240705 11.00000 0.01972 0.02556 =
0.01969 0.00228 -0.00179 0.00769
C3 1 0.905566 0.610470 0.937691 11.00000 0.02468 0.02123 =
0.02983 0.00027 -0.00201 0.00981
C2 1 0.865004 0.604830 0.948456 11.00000 0.02823 0.02408 =
0.02247 0.00173 0.00353 0.01503
AFIX 43
H2 2 0.858609 0.617607 1.008329 11.00000 -1.20000
AFIX 0
C24 1 0.788702 0.572431 0.881735 11.00000 0.02439 0.02945 =
0.01890 0.00273 0.00424 0.01604
AFIX 23
H24A 2 0.784545 0.580534 0.956822 11.00000 -1.20000
H24B 2 0.768569 0.541658 0.872265 11.00000 -1.20000
AFIX 0
C10 1 0.890564 0.600716 0.360265 11.00000 0.03044 0.03528 =
0.02675 0.00672 0.00824 0.02405
AFIX 43
H10 2 0.889258 0.612151 0.290757 11.00000 -1.20000
AFIX 0
C20 1 0.764554 0.644271 0.636639 11.00000 0.03093 0.03959 =
0.02991 0.01238 0.01160 0.02625
AFIX 43
H20 2 0.760226 0.660610 0.582331 11.00000 -1.20000
AFIX 0
C17 1 0.747166 0.581466 0.420943 11.00000 0.02158 0.03018 =
0.02247 0.00292 0.00149 0.01436
C11 1 0.857712 0.560954 0.391133 11.00000 0.02758 0.03142 =
0.02762 -0.00304 0.00282 0.02227
C14 1 0.795796 0.587211 0.235242 11.00000 0.01957 0.02770 =
0.02078 -0.00301 0.00070 0.00926
AFIX 43
H14 2 0.812203 0.589504 0.171789 11.00000 -1.20000
AFIX 0
C19 1 0.745684 0.600238 0.623113 11.00000 0.02466 0.03689 =
0.02362 0.00687 0.00880 0.02150
C25 1 0.844643 0.562617 0.783227 11.00000 0.02973 0.02891 =
0.02134 0.00308 0.00158 0.01893
C28 1 0.752168 0.577328 0.706227 11.00000 0.02135 0.02844 =
0.02365 0.00409 0.00844 0.01674
C13 1 0.793334 0.561360 0.322597 11.00000 0.02239 0.02674 =
0.02398 -0.00309 -0.00132 0.01282
C8 1 0.927314 0.607636 0.530157 11.00000 0.02741 0.03856 =
0.03458 -0.00723 -0.00080 0.02267
AFIX 43
H8 2 0.950790 0.624029 0.577501 11.00000 -1.20000
AFIX 0
C1 1 0.833814 0.580527 0.871736 11.00000 0.02465 0.02557 =
0.02379 0.00459 0.00536 0.01613
C5 1 0.886167 0.569892 0.770410 11.00000 0.03561 0.03507 =
0.02460 0.00524 0.00638 0.02676
C23 1 0.778524 0.597059 0.796970 11.00000 0.02232 0.03019 =
0.02142 0.00451 0.00767 0.01739
C22 1 0.796949 0.641034 0.806680 11.00000 0.02843 0.03324 =
0.02574 0.00150 0.00834 0.01922
AFIX 43
H22 2 0.814878 0.655309 0.867784 11.00000 -1.20000
AFIX 0
C21 1 0.789263 0.664175 0.727482 11.00000 0.03408 0.02879 =
0.03519 0.00472 0.01238 0.02082
AFIX 43
H21 2 0.801203 0.693985 0.736316 11.00000 -1.20000
AFIX 0
C7 1 0.895770 0.567760 0.563462 11.00000 0.03064 0.03929 =
0.02777 -0.00107 0.00341 0.02833
C4 1 0.916275 0.593689 0.849282 11.00000 0.02569 0.03850 =
0.03065 0.00657 0.00592 0.02055
AFIX 43
H4 2 0.944407 0.598510 0.842644 11.00000 -1.20000
AFIX 0
C26 1 0.861663 0.544772 0.492105 11.00000 0.02989 0.02778 =
0.02921 0.00243 0.00838 0.02094
C27 1 0.768926 0.558531 0.415138 11.00000 0.02290 0.02806 =
0.02438 0.00333 0.00058 0.01344
C18 1 0.720061 0.578393 0.519929 11.00000 0.02386 0.04338 =
0.02621 0.00968 0.00513 0.02242
AFIX 23
H18A 2 0.700519 0.548016 0.536836 11.00000 -1.20000
H18B 2 0.702496 0.591249 0.500219 11.00000 -1.20000
AFIX 0
C31 1 0.690601 0.509252 0.733950 11.00000 0.02037 0.03686 =
0.03228 0.01058 0.00791 0.01182
AFIX 23
H31A 2 0.674011 0.522648 0.709611 11.00000 -1.20000
H31B 2 0.690578 0.508623 0.815710 11.00000 -1.20000
AFIX 0
C9 1 0.925036 0.623988 0.428145 11.00000 0.02601 0.03320 =
0.04076 0.00215 0.00811 0.01875
AFIX 43
H9 2 0.947183 0.651128 0.405307 11.00000 -1.20000
AFIX 0
N4 4 0.664692 0.465479 0.568741 11.00000 0.04698 0.05161 =
0.04488 -0.00256 -0.01558 0.01296
C6 1 0.897732 0.550285 0.675926 11.00000 0.04323 0.05163 =
0.02616 0.00176 0.00289 0.03857
AFIX 23
H6A 2 0.878111 0.519168 0.676259 11.00000 -1.20000
H6B 2 0.926863 0.555358 0.687975 11.00000 -1.20000
AFIX 0
C12 1 0.817985 0.537810 0.321132 11.00000 0.03376 0.03370 =
0.02669 -0.00495 0.00049 0.02146
AFIX 23
H12A 2 0.799872 0.508657 0.350041 11.00000 -1.20000
H12B 2 0.825950 0.535615 0.244215 11.00000 -1.20000
AFIX 0
C32 1 0.670997 0.464854 0.689117 11.00000 0.02644 0.03816 =
0.04438 0.00924 -0.00145 0.00935
AFIX 23
H32A 2 0.689825 0.453040 0.704496 11.00000 -1.20000
H32B 2 0.643333 0.446505 0.725666 11.00000 -1.20000
AFIX 0
C29 1 0.835262 0.470480 0.490168 11.00000 0.05525 0.03299 =
0.04836 0.00507 0.01475 0.03237
AFIX 23
H29A 2 0.860714 0.472574 0.526160 11.00000 -1.20000
H29B 2 0.839456 0.471768 0.409152 11.00000 -1.20000
AFIX 0
N5 4 0.680065 0.449671 0.510347 11.00000 0.06562 0.07068 =
0.05892 -0.00980 -0.00195 0.01483
C30 1 0.796718 0.429882 0.521339 11.00000 0.06698 0.03226 =
0.07232 0.00394 0.00763 0.02960
AFIX 23
H30A 2 0.797717 0.405718 0.486638 11.00000 -1.20000
H30B 2 0.770974 0.429853 0.494378 11.00000 -1.20000
AFIX 0
N6 4 0.692060 0.435481 0.445431 11.00000 0.10320 0.10563 =
0.08012 -0.02048 0.01607 0.02867
N1 4 0.794693 0.424958 0.644786 11.00000 0.06597 0.06346 =
0.07369 0.03044 0.01634 0.04358
N2 4 0.765670 0.424810 0.688846 11.00000 0.07548 0.09621 =
0.06327 -0.00414 -0.00624 0.06250
N3 4 0.740142 0.424528 0.742450 11.00000 0.09814 0.15127 =
0.07423 -0.01074 -0.00835 0.08219
HKLF 4
REM mo_ga597_0m_a.res in R-3
REM wR2 = 0.0974, GooF = S = 1.031, Restrained GooF = 1.053 for all data
REM R1 = 0.0397 for 6043 Fo > 4sig(Fo) and 0.0584 for all 7804 data
REM 399 parameters refined using 24 restraints
END
WGHT 0.0383 55.0443
REM Highest difference peak 1.298, deepest hole -1.122, 1-sigma level 0.079
Q1 1 0.9524 0.6425 0.9833 11.00000 0.05 1.30
;
_shelx_res_checksum 72674
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39 2 1 2.0839 0.5970
39 2 4 -1.3158 0.1258
39 3 -3 -2.5767 1.2626
39 3 0 4.0325 1.6796
39 3 3 -0.1887 0.7456
39 4 -1 -1.1540 -0.0247
39 4 2 -5.0910 0.6009
39 5 -2 -2.7341 0.4614
39 5 1 1.3217 0.1786
40 1 -3 -2.2110 1.4416
40 1 0 3.3432 1.6877
40 1 3 0.5417 0.6244
40 2 -1 -0.7059 -0.3140
40 2 2 -5.2595 0.3484
40 3 -2 -2.4293 0.5950
40 3 1 2.0687 0.5513
40 4 0 4.5524 1.1325
41 1 -2 -1.7871 0.6463
41 1 1 2.3256 0.8328
41 2 0 3.9691 1.2923
0 0 0 0.0 0.0
;
_shelx_fab_checksum 62141
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.77808(2) 0.64422(2) 0.11845(2) 0.02592(8) Uani d 1 . .
Br Br1 0.94747(2) 0.64087(2) 1.04746(3) 0.03614(9) Uani d 1 . .
O O4 0.73344(6) 0.53322(6) 0.69360(15) 0.0235(4) Uani d 1 . .
O O3 0.76702(7) 0.53195(7) 0.49646(16) 0.0304(5) Uani d 1 . .
H H3 0.754079 0.534255 0.551158 0.046 Uiso calc 1 . .
O O1 0.81215(6) 0.53626(7) 0.71561(16) 0.0296(4) Uani d 1 . .
H H1 0.821251 0.526224 0.667258 0.044 Uiso calc 1 . .
O O2 0.82909(7) 0.50491(6) 0.52611(17) 0.0317(5) Uani d 1 . .
C C16 0.75008(8) 0.60698(9) 0.3311(2) 0.0237(5) Uani d 1 . .
H H16 0.735357 0.622450 0.332302 0.028 Uiso calc 1 . .
C C15 0.77434(8) 0.60962(9) 0.2407(2) 0.0233(5) Uani d 1 . .
C C3 0.90557(9) 0.61047(9) 0.9377(2) 0.0260(6) Uani d 1 . .
C C2 0.86500(9) 0.60483(9) 0.9485(2) 0.0241(5) Uani d 1 . .
H H2 0.858609 0.617607 1.008329 0.029 Uiso calc 1 . .
C C24 0.78870(8) 0.57243(9) 0.8817(2) 0.0231(5) Uani d 1 . .
H H24A 0.784545 0.580534 0.956822 0.028 Uiso calc 1 . .
H H24B 0.768569 0.541658 0.872265 0.028 Uiso calc 1 . .
C C10 0.89056(9) 0.60072(9) 0.3603(2) 0.0274(6) Uani d 1 . .
H H10 0.889258 0.612151 0.290757 0.033 Uiso calc 1 . .
C C20 0.76455(9) 0.64427(10) 0.6366(2) 0.0296(6) Uani d 1 . .
H H20 0.760226 0.660610 0.582331 0.036 Uiso calc 1 . .
C C17 0.74717(8) 0.58147(9) 0.4209(2) 0.0241(5) Uani d 1 . .
C C11 0.85771(9) 0.56095(9) 0.3911(2) 0.0255(6) Uani d 1 . .
C C14 0.79580(8) 0.58721(9) 0.2352(2) 0.0238(5) Uani d 1 . .
H H14 0.812203 0.589504 0.171789 0.029 Uiso calc 1 . .
C C19 0.74568(9) 0.60024(9) 0.6231(2) 0.0257(6) Uani d 1 . .
C C25 0.84464(9) 0.56262(9) 0.7832(2) 0.0248(6) Uani d 1 . .
C C28 0.75217(8) 0.57733(9) 0.7062(2) 0.0226(5) Uani d 1 . .
C C13 0.79333(8) 0.56136(9) 0.3226(2) 0.0241(5) Uani d 1 . .
C C8 0.92731(9) 0.60764(10) 0.5302(2) 0.0308(6) Uani d 1 . .
H H8 0.950790 0.624029 0.577501 0.037 Uiso calc 1 . .
C C1 0.83381(9) 0.58053(9) 0.8717(2) 0.0231(5) Uani d 1 . .
C C5 0.88617(9) 0.56989(9) 0.7704(2) 0.0277(6) Uani d 1 . .
C C23 0.77852(8) 0.59706(9) 0.7970(2) 0.0227(5) Uani d 1 . .
C C22 0.79695(9) 0.64103(9) 0.8067(2) 0.0274(6) Uani d 1 . .
H H22 0.814878 0.655309 0.867784 0.033 Uiso calc 1 . .
C C21 0.78926(10) 0.66417(10) 0.7275(2) 0.0304(6) Uani d 1 . .
H H21 0.801203 0.693985 0.736316 0.037 Uiso calc 1 . .
C C7 0.89577(9) 0.56776(10) 0.5635(2) 0.0277(6) Uani d 1 . .
C C4 0.91627(9) 0.59369(10) 0.8493(2) 0.0296(6) Uani d 1 . .
H H4 0.944407 0.598510 0.842644 0.036 Uiso calc 1 . .
C C26 0.86166(9) 0.54477(9) 0.4921(2) 0.0261(6) Uani d 1 . .
C C27 0.76893(9) 0.55853(9) 0.4151(2) 0.0248(6) Uani d 1 . .
C C18 0.72006(9) 0.57839(10) 0.5199(2) 0.0287(6) Uani d 1 . .
H H18A 0.700519 0.548016 0.536836 0.034 Uiso calc 1 . .
H H18B 0.702496 0.591249 0.500219 0.034 Uiso calc 1 . .
C C31 0.69060(9) 0.50925(10) 0.7339(2) 0.0309(6) Uani d 1 . .
H H31A 0.674011 0.522648 0.709611 0.037 Uiso calc 1 . .
H H31B 0.690578 0.508623 0.815710 0.037 Uiso calc 1 . .
C C9 0.92504(9) 0.62399(10) 0.4281(3) 0.0316(6) Uani d 1 . .
H H9 0.947183 0.651128 0.405307 0.038 Uiso calc 1 . .
N N4 0.66469(11) 0.46548(11) 0.5687(3) 0.0530(8) Uani d 1 . .
C C6 0.89773(11) 0.55028(11) 0.6759(2) 0.0337(7) Uani d 1 . .
H H6A 0.878111 0.519168 0.676259 0.040 Uiso calc 1 . .
H H6B 0.926863 0.555358 0.687975 0.040 Uiso calc 1 . .
C C12 0.81799(9) 0.53781(10) 0.3211(2) 0.0293(6) Uani d 1 . .
H H12A 0.799872 0.508657 0.350041 0.035 Uiso calc 1 . .
H H12B 0.825950 0.535615 0.244215 0.035 Uiso calc 1 . .
C C32 0.67100(10) 0.46485(11) 0.6891(3) 0.0393(7) Uani d 1 . .
H H32A 0.689825 0.453040 0.704496 0.047 Uiso calc 1 . .
H H32B 0.643333 0.446505 0.725666 0.047 Uiso calc 1 . .
C C29 0.83526(12) 0.47048(10) 0.4902(3) 0.0410(8) Uani d 1 . .
H H29A 0.860714 0.472574 0.526160 0.049 Uiso calc 1 . .
H H29B 0.839456 0.471768 0.409152 0.049 Uiso calc 1 . .
N N5 0.68006(13) 0.44967(14) 0.5103(3) 0.0736(11) Uani d 1 . .
C C30 0.79672(14) 0.42988(11) 0.5213(4) 0.0551(10) Uani d 1 . .
H H30A 0.797717 0.405718 0.486638 0.066 Uiso calc 1 . .
H H30B 0.770974 0.429853 0.494378 0.066 Uiso calc 1 . .
N N6 0.69206(17) 0.43548(18) 0.4454(4) 0.1068(16) Uani d 1 . .
N N1 0.79469(12) 0.42496(12) 0.6448(3) 0.0627(10) Uani d 1 . .
N N2 0.76567(14) 0.42481(14) 0.6888(3) 0.0696(10) Uani d 1 . .
N N3 0.74014(17) 0.42453(19) 0.7425(4) 0.0991(13) 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
Br2 0.02212(13) 0.02979(15) 0.02155(13) 0.00975(11) -0.00145(10) 0.00350(11)
Br1 0.02894(16) 0.03163(16) 0.04687(19) 0.01439(13) -0.00821(13) -0.00860(13)
O4 0.0183(9) 0.0272(10) 0.0253(9) 0.0116(8) 0.0057(7) 0.0035(8)
O3 0.0372(12) 0.0398(12) 0.0249(10) 0.0273(10) 0.0095(9) 0.0086(9)
O1 0.0292(10) 0.0423(12) 0.0267(10) 0.0249(10) -0.0010(8) -0.0068(9)
O2 0.0373(11) 0.0288(11) 0.0378(12) 0.0233(10) 0.0125(9) 0.0051(9)
C16 0.0219(13) 0.0267(14) 0.0244(13) 0.0135(11) -0.0011(10) 0.0006(11)
C15 0.0197(12) 0.0256(13) 0.0197(12) 0.0077(11) -0.0018(10) 0.0023(10)
C3 0.0247(14) 0.0212(13) 0.0298(14) 0.0098(11) -0.0020(11) 0.0003(11)
C2 0.0282(14) 0.0241(13) 0.0225(13) 0.0150(12) 0.0035(11) 0.0017(10)
C24 0.0244(13) 0.0294(14) 0.0189(12) 0.0160(12) 0.0042(10) 0.0027(10)
C10 0.0304(15) 0.0353(15) 0.0268(14) 0.0241(13) 0.0082(11) 0.0067(12)
C20 0.0309(15) 0.0396(16) 0.0299(15) 0.0263(14) 0.0116(12) 0.0124(13)
C17 0.0216(13) 0.0302(14) 0.0225(13) 0.0144(11) 0.0015(10) 0.0029(11)
C11 0.0276(14) 0.0314(14) 0.0276(14) 0.0223(12) 0.0028(11) -0.0030(11)
C14 0.0196(12) 0.0277(14) 0.0208(12) 0.0093(11) 0.0007(10) -0.0030(11)
C19 0.0247(13) 0.0369(15) 0.0236(13) 0.0215(12) 0.0088(11) 0.0069(11)
C25 0.0297(14) 0.0289(14) 0.0213(13) 0.0189(12) 0.0016(11) 0.0031(11)
C28 0.0214(12) 0.0284(14) 0.0236(13) 0.0167(11) 0.0084(10) 0.0041(11)
C13 0.0224(13) 0.0267(14) 0.0240(13) 0.0128(11) -0.0013(10) -0.0031(11)
C8 0.0274(15) 0.0386(17) 0.0346(16) 0.0227(14) -0.0008(12) -0.0072(13)
C1 0.0246(13) 0.0256(13) 0.0238(13) 0.0161(11) 0.0054(11) 0.0046(11)
C5 0.0356(16) 0.0351(15) 0.0246(13) 0.0268(13) 0.0064(12) 0.0052(12)
C23 0.0223(13) 0.0302(14) 0.0214(12) 0.0174(11) 0.0077(10) 0.0045(11)
C22 0.0284(14) 0.0332(15) 0.0257(14) 0.0192(13) 0.0083(11) 0.0015(11)
C21 0.0341(16) 0.0288(15) 0.0352(16) 0.0208(13) 0.0124(13) 0.0047(12)
C7 0.0306(15) 0.0393(16) 0.0278(14) 0.0283(14) 0.0034(11) -0.0011(12)
C4 0.0257(14) 0.0385(16) 0.0307(15) 0.0205(13) 0.0059(12) 0.0066(13)
C26 0.0299(14) 0.0278(14) 0.0292(14) 0.0209(12) 0.0084(11) 0.0024(11)
C27 0.0229(13) 0.0281(14) 0.0244(13) 0.0134(11) 0.0006(10) 0.0033(11)
C18 0.0239(14) 0.0434(17) 0.0262(14) 0.0224(13) 0.0051(11) 0.0097(12)
C31 0.0204(13) 0.0369(16) 0.0323(15) 0.0118(12) 0.0079(11) 0.0106(13)
C9 0.0260(14) 0.0332(16) 0.0408(17) 0.0188(13) 0.0081(13) 0.0022(13)
N4 0.0470(18) 0.0516(19) 0.0449(18) 0.0130(15) -0.0156(15) -0.0026(15)
C6 0.0432(18) 0.0516(19) 0.0262(15) 0.0386(16) 0.0029(13) 0.0018(13)
C12 0.0338(15) 0.0337(15) 0.0267(14) 0.0215(13) 0.0005(12) -0.0049(12)
C32 0.0264(15) 0.0382(18) 0.0444(19) 0.0094(14) -0.0015(14) 0.0092(15)
C29 0.055(2) 0.0330(17) 0.0484(19) 0.0324(17) 0.0147(16) 0.0051(14)
N5 0.066(2) 0.071(2) 0.059(2) 0.0148(19) -0.0020(19) -0.0098(19)
C30 0.067(3) 0.0323(18) 0.072(3) 0.0296(19) 0.008(2) 0.0039(18)
N6 0.103(3) 0.106(3) 0.080(3) 0.029(3) 0.016(3) -0.020(3)
N1 0.066(2) 0.063(2) 0.074(2) 0.0436(19) 0.0163(19) 0.0304(19)
N2 0.075(2) 0.096(3) 0.063(2) 0.063(2) -0.0062(19) -0.004(2)
N3 0.098(3) 0.151(4) 0.074(3) 0.082(3) -0.008(2) -0.011(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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C28 O4 C31 . . 114.6(2) ?
C27 O3 H3 . . 109.5 ?
C25 O1 H1 . . 109.5 ?
C26 O2 C29 . . 113.0(2) ?
C15 C16 H16 . . 120.1 ?
C15 C16 C17 . . 119.8(2) ?
C17 C16 H16 . . 120.1 ?
C16 C15 Br2 . . 119.7(2) ?
C16 C15 C14 . . 121.8(2) ?
C14 C15 Br2 . . 118.5(2) ?
C2 C3 Br1 . . 120.1(2) ?
C4 C3 Br1 . . 118.5(2) ?
C4 C3 C2 . . 121.3(3) ?
C3 C2 H2 . . 120.0 ?
C1 C2 C3 . . 120.0(3) ?
C1 C2 H2 . . 120.0 ?
H24A C24 H24B . . 107.8 ?
C1 C24 H24A . . 109.0 ?
C1 C24 H24B . . 109.0 ?
C1 C24 C23 . . 112.8(2) ?
C23 C24 H24A . . 109.0 ?
C23 C24 H24B . . 109.0 ?
C11 C10 H10 . . 119.2 ?
C9 C10 H10 . . 119.2 ?
C9 C10 C11 . . 121.5(3) ?
C19 C20 H20 . . 119.6 ?
C21 C20 H20 . . 119.6 ?
C21 C20 C19 . . 120.8(3) ?
C16 C17 C27 . . 118.3(2) ?
C16 C17 C18 . . 119.6(2) ?
C27 C17 C18 . . 122.1(2) ?
C10 C11 C26 . . 117.3(3) ?
C10 C11 C12 . . 120.8(3) ?
C26 C11 C12 . . 121.8(3) ?
C15 C14 H14 . . 120.1 ?
C15 C14 C13 . . 119.9(2) ?
C13 C14 H14 . . 120.1 ?
C20 C19 C18 . . 120.9(2) ?
C28 C19 C20 . . 117.6(3) ?
C28 C19 C18 . . 121.4(3) ?
O1 C25 C1 . . 116.0(2) ?
O1 C25 C5 . . 122.6(2) ?
C5 C25 C1 . . 121.3(3) ?
C19 C28 O4 . . 118.2(2) ?
C23 C28 O4 . . 119.3(2) ?
C23 C28 C19 . . 122.4(3) ?
C14 C13 C27 . . 118.9(2) ?
C14 C13 C12 . . 121.1(2) ?
C27 C13 C12 . . 119.9(2) ?
C7 C8 H8 . . 119.6 ?
C7 C8 C9 . . 120.7(3) ?
C9 C8 H8 . . 119.6 ?
C2 C1 C24 . . 121.9(2) ?
C2 C1 C25 . . 118.4(2) ?
C25 C1 C24 . . 119.7(2) ?
C25 C5 C6 . . 121.3(3) ?
C4 C5 C25 . . 118.8(3) ?
C4 C5 C6 . . 119.8(3) ?
C28 C23 C24 . . 122.3(2) ?
C22 C23 C24 . . 119.8(3) ?
C22 C23 C28 . . 117.9(2) ?
C23 C22 H22 . . 119.8 ?
C21 C22 C23 . . 120.5(3) ?
C21 C22 H22 . . 119.8 ?
C20 C21 C22 . . 120.6(3) ?
C20 C21 H21 . . 119.7 ?
C22 C21 H21 . . 119.7 ?
C8 C7 C26 . . 118.0(3) ?
C8 C7 C6 . . 120.8(3) ?
C26 C7 C6 . . 121.2(3) ?
C3 C4 C5 . . 120.2(3) ?
C3 C4 H4 . . 119.9 ?
C5 C4 H4 . . 119.9 ?
C11 C26 O2 . . 118.9(3) ?
C7 C26 O2 . . 118.5(3) ?
C7 C26 C11 . . 122.6(3) ?
O3 C27 C17 . . 122.8(2) ?
O3 C27 C13 . . 116.0(2) ?
C13 C27 C17 . . 121.2(2) ?
C17 C18 C19 . . 113.8(2) ?
C17 C18 H18A . . 108.8 ?
C17 C18 H18B . . 108.8 ?
C19 C18 H18A . . 108.8 ?
C19 C18 H18B . . 108.8 ?
H18A C18 H18B . . 107.7 ?
O4 C31 H31A . . 110.0 ?
O4 C31 H31B . . 110.0 ?
O4 C31 C32 . . 108.4(2) ?
H31A C31 H31B . . 108.4 ?
C32 C31 H31A . . 110.0 ?
C32 C31 H31B . . 110.0 ?
C10 C9 C8 . . 119.8(3) ?
C10 C9 H9 . . 120.1 ?
C8 C9 H9 . . 120.1 ?
N5 N4 C32 . . 117.2(4) ?
C5 C6 C7 . . 113.5(2) ?
C5 C6 H6A . . 108.9 ?
C5 C6 H6B . . 108.9 ?
C7 C6 H6A . . 108.9 ?
C7 C6 H6B . . 108.9 ?
H6A C6 H6B . . 107.7 ?
C11 C12 C13 . . 110.4(2) ?
C11 C12 H12A . . 109.6 ?
C11 C12 H12B . . 109.6 ?
C13 C12 H12A . . 109.6 ?
C13 C12 H12B . . 109.6 ?
H12A C12 H12B . . 108.1 ?
C31 C32 H32A . . 109.8 ?
C31 C32 H32B . . 109.8 ?
N4 C32 C31 . . 109.5(3) ?
N4 C32 H32A . . 109.8 ?
N4 C32 H32B . . 109.8 ?
H32A C32 H32B . . 108.2 ?
O2 C29 H29A . . 110.1 ?
O2 C29 H29B . . 110.1 ?
O2 C29 C30 . . 107.8(3) ?
H29A C29 H29B . . 108.5 ?
C30 C29 H29A . . 110.1 ?
C30 C29 H29B . . 110.1 ?
N6 N5 N4 . . 172.0(6) ?
C29 C30 H30A . . 109.7 ?
C29 C30 H30B . . 109.7 ?
C29 C30 N1 . . 109.6(3) ?
H30A C30 H30B . . 108.2 ?
N1 C30 H30A . . 109.7 ?
N1 C30 H30B . . 109.7 ?
N2 N1 C30 . . 116.2(4) ?
N3 N2 N1 . . 171.8(5) ?
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
Br2 C15 . 1.902(3) ?
Br1 C3 . 1.903(3) ?
O4 C28 . 1.401(3) ?
O4 C31 . 1.436(3) ?
O3 H3 . 0.8400 ?
O3 C27 . 1.356(3) ?
O1 H1 . 0.8400 ?
O1 C25 . 1.360(3) ?
O2 C26 . 1.397(3) ?
O2 C29 . 1.444(3) ?
C16 H16 . 0.9500 ?
C16 C15 . 1.377(4) ?
C16 C17 . 1.399(4) ?
C15 C14 . 1.382(4) ?
C3 C2 . 1.389(4) ?
C3 C4 . 1.380(4) ?
C2 H2 . 0.9500 ?
C2 C1 . 1.388(4) ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C24 C1 . 1.518(4) ?
C24 C23 . 1.523(4) ?
C10 H10 . 0.9500 ?
C10 C11 . 1.388(4) ?
C10 C9 . 1.378(4) ?
C20 H20 . 0.9500 ?
C20 C19 . 1.400(4) ?
C20 C21 . 1.374(4) ?
C17 C27 . 1.408(4) ?
C17 C18 . 1.519(4) ?
C11 C26 . 1.394(4) ?
C11 C12 . 1.515(4) ?
C14 H14 . 0.9500 ?
C14 C13 . 1.387(4) ?
C19 C28 . 1.399(4) ?
C19 C18 . 1.522(4) ?
C25 C1 . 1.408(4) ?
C25 C5 . 1.404(4) ?
C28 C23 . 1.397(4) ?
C13 C27 . 1.400(4) ?
C13 C12 . 1.517(4) ?
C8 H8 . 0.9500 ?
C8 C7 . 1.383(4) ?
C8 C9 . 1.391(4) ?
C5 C4 . 1.382(4) ?
C5 C6 . 1.514(4) ?
C23 C22 . 1.394(4) ?
C22 H22 . 0.9500 ?
C22 C21 . 1.392(4) ?
C21 H21 . 0.9500 ?
C7 C26 . 1.394(4) ?
C7 C6 . 1.519(4) ?
C4 H4 . 0.9500 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C31 H31A . 0.9900 ?
C31 H31B . 0.9900 ?
C31 C32 . 1.501(5) ?
C9 H9 . 0.9500 ?
N4 C32 . 1.477(4) ?
N4 N5 . 1.209(5) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C32 H32A . 0.9900 ?
C32 H32B . 0.9900 ?
C29 H29A . 0.9900 ?
C29 H29B . 0.9900 ?
C29 C30 . 1.488(5) ?
N5 N6 . 1.139(6) ?
C30 H30A . 0.9900 ?
C30 H30B . 0.9900 ?
C30 N1 . 1.502(5) ?
N1 N2 . 1.179(5) ?
N2 N3 . 1.128(6) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O3 H3 O4 . 0.84 1.87 2.691(3) 164.1 yes
O1 H1 O2 . 0.84 1.95 2.764(3) 161.5 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Br2 C15 C14 C13 . . . . -179.3(2) ?
Br1 C3 C2 C1 . . . . -176.2(2) ?
Br1 C3 C4 C5 . . . . 177.3(2) ?
O4 C28 C23 C24 . . . . 1.7(4) ?
O4 C28 C23 C22 . . . . 179.5(2) ?
O4 C31 C32 N4 . . . . -69.0(3) ?
O1 C25 C1 C2 . . . . 174.8(2) ?
O1 C25 C1 C24 . . . . -4.4(4) ?
O1 C25 C5 C4 . . . . -173.5(3) ?
O1 C25 C5 C6 . . . . 3.1(4) ?
O2 C29 C30 N1 . . . . -69.2(4) ?
C16 C15 C14 C13 . . . . -0.3(4) ?
C16 C17 C27 O3 . . . . -177.9(3) ?
C16 C17 C27 C13 . . . . 0.7(4) ?
C16 C17 C18 C19 . . . . -109.8(3) ?
C15 C16 C17 C27 . . . . -1.0(4) ?
C15 C16 C17 C18 . . . . -179.5(3) ?
C15 C14 C13 C27 . . . . 0.0(4) ?
C15 C14 C13 C12 . . . . -177.4(2) ?
C3 C2 C1 C24 . . . . 178.3(2) ?
C3 C2 C1 C25 . . . . -0.9(4) ?
C2 C3 C4 C5 . . . . -1.5(4) ?
C24 C23 C22 C21 . . . . 177.5(2) ?
C10 C11 C26 O2 . . . . 179.7(2) ?
C10 C11 C26 C7 . . . . 3.3(4) ?
C10 C11 C12 C13 . . . . -66.7(3) ?
C20 C19 C28 O4 . . . . -180.0(2) ?
C20 C19 C28 C23 . . . . -4.0(4) ?
C20 C19 C18 C17 . . . . 80.6(3) ?
C17 C16 C15 Br2 . . . . 179.8(2) ?
C17 C16 C15 C14 . . . . 0.8(4) ?
C11 C10 C9 C8 . . . . -0.1(4) ?
C14 C13 C27 O3 . . . . 178.5(2) ?
C14 C13 C27 C17 . . . . -0.2(4) ?
C14 C13 C12 C11 . . . . 100.8(3) ?
C19 C20 C21 C22 . . . . 1.7(4) ?
C19 C28 C23 C24 . . . . -174.3(2) ?
C19 C28 C23 C22 . . . . 3.5(4) ?
C25 C5 C4 C3 . . . . -1.1(4) ?
C25 C5 C6 C7 . . . . 67.5(4) ?
C28 O4 C31 C32 . . . . 165.3(2) ?
C28 C19 C18 C17 . . . . -97.7(3) ?
C28 C23 C22 C21 . . . . -0.4(4) ?
C8 C7 C26 O2 . . . . -178.4(2) ?
C8 C7 C26 C11 . . . . -2.0(4) ?
C8 C7 C6 C5 . . . . 75.5(4) ?
C1 C24 C23 C28 . . . . 106.9(3) ?
C1 C24 C23 C22 . . . . -70.9(3) ?
C1 C25 C5 C4 . . . . 2.7(4) ?
C1 C25 C5 C6 . . . . 179.4(3) ?
C5 C25 C1 C2 . . . . -1.7(4) ?
C5 C25 C1 C24 . . . . 179.1(2) ?
C23 C24 C1 C2 . . . . 107.3(3) ?
C23 C24 C1 C25 . . . . -73.5(3) ?
C23 C22 C21 C20 . . . . -2.2(4) ?
C21 C20 C19 C28 . . . . 1.3(4) ?
C21 C20 C19 C18 . . . . -177.0(2) ?
C7 C8 C9 C10 . . . . 1.5(4) ?
C4 C3 C2 C1 . . . . 2.5(4) ?
C4 C5 C6 C7 . . . . -115.9(3) ?
C26 O2 C29 C30 . . . . -174.4(3) ?
C26 C11 C12 C13 . . . . 108.9(3) ?
C26 C7 C6 C5 . . . . -102.6(3) ?
C27 C17 C18 C19 . . . . 71.7(4) ?
C27 C13 C12 C11 . . . . -76.6(3) ?
C18 C17 C27 O3 . . . . 0.6(4) ?
C18 C17 C27 C13 . . . . 179.2(3) ?
C18 C19 C28 O4 . . . . -1.6(4) ?
C18 C19 C28 C23 . . . . 174.4(2) ?
C31 O4 C28 C19 . . . . -86.8(3) ?
C31 O4 C28 C23 . . . . 97.1(3) ?
C9 C10 C11 C26 . . . . -2.2(4) ?
C9 C10 C11 C12 . . . . 173.6(2) ?
C9 C8 C7 C26 . . . . -0.5(4) ?
C9 C8 C7 C6 . . . . -178.6(2) ?
C6 C5 C4 C3 . . . . -177.8(3) ?
C6 C7 C26 O2 . . . . -0.2(4) ?
C6 C7 C26 C11 . . . . 176.2(2) ?
C12 C11 C26 O2 . . . . 3.9(4) ?
C12 C11 C26 C7 . . . . -172.5(2) ?
C12 C13 C27 O3 . . . . -4.0(4) ?
C12 C13 C27 C17 . . . . 177.2(3) ?
C29 O2 C26 C11 . . . . 90.4(3) ?
C29 O2 C26 C7 . . . . -93.0(3) ?
C29 C30 N1 N2 . . . . 115.8(4) ?
N5 N4 C32 C31 . . . . 125.4(4) ?