#------------------------------------------------------------------------------
#$Date: 2024-08-09 04:46:27 +0300 (Fri, 09 Aug 2024) $
#$Revision: 294065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312568.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_2312568
loop_
_publ_author_name
'Jaconelli, Harry S.'
'Kennedy, Alan R.'
_publ_section_title
;
Salt forms of amides: protonation of acetanilide.
;
_journal_coeditor_code EF3058
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624007332
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C8 H10 N1 O1 +, I2 Br1 -, C8 H9 N1 O1, 0.5I2'
_chemical_formula_moiety 'C8 H10 N1 O1 +, I2 Br1 -, C8 H9 N1 O1, 0.5I2'
_chemical_formula_sum 'C16 H19 Br0.93 I3.07 N2 O2'
_chemical_formula_weight 735.18
_chemical_name_systematic
;
N-(1-Hydroxyethylidene)anilinium diiodobromide--\
N-phenylacetamide--diiodine (2/2/1)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 11
_space_group_name_Hall '-P 2yb'
_space_group_name_H-M_alt 'P 1 21/m 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 91.970(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.89560(10)
_cell_length_b 18.6224(4)
_cell_length_c 19.9632(4)
_cell_measurement_reflns_used 13599
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 71.4720
_cell_measurement_theta_min 2.3540
_cell_volume 2190.47(7)
_computing_cell_refinement
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_publication_material
;
SHELXL2018 in WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type 'Rigaku Synergy-i'
_diffrn_measurement_method ' omega scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0959
_diffrn_reflns_av_unetI/netI 0.0445
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 21645
_diffrn_reflns_theta_full 70.000
_diffrn_reflns_theta_max 71.536
_diffrn_reflns_theta_min 3.246
_diffrn_source 'microsource tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 36.463
_exptl_absorpt_correction_T_max 0.164
_exptl_absorpt_correction_T_min 0.014
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2023), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.229
_exptl_crystal_description 'broken needle'
_exptl_crystal_F_000 1361
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.055
_refine_diff_density_max 1.495
_refine_diff_density_min -1.862
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 245
_refine_ls_number_reflns 4338
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.076
_refine_ls_R_factor_all 0.0564
_refine_ls_R_factor_gt 0.0516
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1466
_refine_ls_wR_factor_ref 0.1508
_reflns_number_gt 3762
_reflns_number_total 4338
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ef3058.cif
_cod_data_source_block ACTHI2Br
_cod_original_sg_symbol_H-M 'P 21/m'
_cod_database_code 2312568
_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
;
0 0 2 459.117 44.7633 16
0 0 2 698.707 671.664 17
0 0 2 240.180 295.285 41
0 0 -2 565.043 54.2854 39
0 0 2 331.977 56.3974 7
0 0 2 626.512 773.295 1
0 0 3 890.521 342.604 41
0 0 -3 2266.41 130.394 39
0 0 3 1496.61 113.369 16
0 0 3 1546.51 469.333 17
0 0 3 790.298 676.025 1
0 0 4 2736.95 509.871 41
0 0 -4 4961.44 258.262 39
0 0 4 3884.37 244.056 16
0 0 4 3894.02 498.676 17
0 0 4 3543.19 739.243 1
0 0 5 291.097 79.4959 16
0 0 5 140.717 351.772 17
0 0 5 294.428 368.084 41
0 0 -5 329.263 77.0343 39
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0 0 -6 3661.47 238.851 39
0 0 6 3987.40 261.045 7
0 0 6 2963.27 602.582 1
0 0 7 173854. 8896.55 17
0 0 7 174862. 8775.61 16
0 0 -7 193268. 8794.34 37
0 0 7 186015. 8787.76 7
0 0 8 2289.63 491.099 1
0 0 -8 2082.02 191.396 37
0 0 8 2696.23 360.905 17
0 0 8 1893.67 179.832 16
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0 0 11 32626.7 2299.48 1
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0 0 12 1807.91 381.235 1
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0 0 -12 2137.32 241.511 37
0 0 -13 276.968 111.753 37
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0 0 13 186.738 71.2009 22
0 0 13 21.9292 249.953 1
0 0 -14 4546.73 369.270 37
0 0 14 3216.49 327.511 27
0 0 14 4400.28 273.741 22
0 0 14 4081.30 479.391 1
0 0 -15 160.387 102.181 37
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0 0 15-154.751 272.626 1
0 0 -16 58.3176 99.7950 37
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0 0 16 184.771 71.8894 22
0 0 16 306.919 229.235 1
0 0 -17 81.9770 109.141 37
0 0 17 279.314 208.095 1
0 0 17 379.180 81.0375 22
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0 0 18 1242.71 128.360 22
0 0 18 1629.31 213.256 27
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0 0 19 385.236 154.324 27
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0 0 21 2823.05 231.725 27
0 0 22 4785.27 301.476 27
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0 0 23 3512.58 233.376 27
0 0 24 998.923 102.600 27
0 0 24 651.166 93.7075 4
0 -1 0 290.096 51.9193 11
0 -1 0 302.041 53.2819 12
0 -1 1 2291.34 137.108 11
0 -1 1 1502.62 356.888 17
0 -1 1 2170.99 137.245 12
0 1 -1 2450.87 439.215 40
0 -1 -1 2039.36 121.467 37
0 -1 1 2235.74 147.076 8
0 -1 1 1611.35 541.896 1
0 -1 2 3208.58 201.794 12
0 -1 2 3143.46 199.829 11
0 -1 2 2168.70 442.402 17
0 -1 2 3137.40 181.233 16
0 1 2 3875.84 442.475 17
0 1 -2 4886.31 258.213 39
0 -1 -2 3252.46 181.842 37
0 -1 -2 2757.53 159.652 39
0 1 2 3221.63 770.352 41
0 1 2 4260.57 271.970 40
0 -1 2 2962.62 188.623 8
0 -1 2 2985.56 184.362 7
0 1 2 4027.42 924.996 1
0 -1 2 1824.70 647.225 1
0 -1 3 3610.97 222.515 16
0 1 3 3252.61 215.328 16
0 -1 3 2810.40 490.308 17
0 1 3 3246.41 418.908 17
0 1 3 2545.30 486.767 41
0 -1 -3 3584.95 200.881 39
0 -1 -3 4046.31 229.935 37
0 1 -3 5844.96 307.152 39
0 -1 3 4055.16 231.909 7
0 -1 3 4365.82 240.686 8
0 -1 3 2246.97 708.071 1
0 1 3 3322.77 775.731 1
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0 -1 4 147.142 70.0269 16
0 -1 4-85.7937 391.670 17
0 1 4 71.1867 65.2326 16
0 -1 4 124.110 205.131 41
0 1 -4 471.759 135.883 39
0 -1 -4 57.9506 42.5262 39
0 1 -4 103.320 270.208 40
0 -1 -4 160.889 71.2091 37
0 1 4 110.747 71.5864 40
0 1 4 139.841 354.007 41
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0 -1 4 21.5085 621.848 1
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0 -1 5 1865.97 449.883 17
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0 -1 -5 1442.52 115.797 39
0 1 -5 2283.29 210.345 39
0 -1 -5 1786.21 150.017 37
0 1 5 1852.76 176.021 7
0 -1 5 1706.37 164.274 7
0 1 5 1519.53 618.949 1
0 -1 5 1263.71 621.526 1
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0 -1 6 425.943 339.771 17
0 -1 6 358.600 91.9986 16
0 1 6 255.572 77.5132 16
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0 -1 -6 249.769 81.8615 37
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0 1 6 339.397 123.006 7
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0 1 6 294.014 475.787 1
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0 1 -7 2655.16 214.329 39
0 -1 -7 2302.42 193.062 37
0 1 7 2534.33 215.149 7
0 1 7 1415.22 469.539 1
0 -1 7 2273.62 545.360 1
0 -1 8 136356. 7495.99 1
0 1 8 119480. 7422.66 1
0 -1 -8 157914. 7236.25 37
0 1 8 148793. 7320.26 17
0 1 8 144946. 7216.13 16
0 -1 8 137014. 7327.45 17
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0 -1 14 6815.18 637.303 1
0 1 14 6298.17 615.289 1
0 1 -15 60614.6 2935.26 37
0 -1 -15 66988.9 2963.99 37
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0 -1 -16 4903.87 393.399 37
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0 -1 -17 646.289 149.561 37
0 1 -17 645.454 154.241 37
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0 -1 20 4180.95 308.141 4
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0 -1 20 3511.97 252.104 22
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0 -1 22 2827.63 229.720 4
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0 -1 24 146.856 75.6207 27
0 1 24 211.838 81.6681 27
0 -1 24 135.678 65.1793 4
0 1 24 176.414 68.4533 4
0 -2 0 343670. 15085.0 37
0 -2 0 269747. 15067.1 38
0 2 0 349836. 15224.8 40
0 -2 0 360304. 15087.2 17
0 -2 0 308721. 15086.9 13
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0 -2 1 3.62952 267.342 15
0 -2 -1 88.2801 62.3327 11
0 -2 1 14.1263 61.7755 13
0 -2 -1 19.8668 50.3607 37
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0 -2 1-11.8369 121.422 8
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0 -2 1 235.761 487.069 1
0 2 1 601.756 347.283 1
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0 -2 2 18583.0 923.785 12
0 -2 2 11398.7 1035.46 17
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0 -2 2 18928.3 923.440 11
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0 -2 -2 16161.7 905.060 37
0 -2 2 19639.2 931.388 7
0 2 2 27243.1 1481.46 1
0 -2 3 3540.83 469.667 17
0 -2 3 640.400 419.965 15
0 -2 3 4503.08 287.192 11
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0 -2 3 4447.23 288.834 12
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0 2 3 4523.24 565.685 41
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0 -2 -3 4534.39 269.168 37
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0 -2 3 4166.56 289.895 8
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0 -2 3 2370.23 623.713 1
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0 -2 4 14154.7 1020.91 17
0 -2 4 16108.1 854.861 14
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0 -2 -4 15561.6 827.044 39
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0 -2 4 14334.6 857.294 8
0 2 4 20511.1 1396.94 1
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0 -2 6 9163.75 923.196 1
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0 -2 -11 41938.7 1963.39 37
0 -2 11 35238.4 2157.44 1
0 2 11 31299.2 2098.18 1
0 -2 11 32733.1 1929.49 16
0 -2 11 37063.3 2032.75 17
0 2 11 42936.8 1954.71 16
0 2 -12 14105.8 851.368 37
0 -2 -12 14740.2 845.192 37
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0 -2 -13 30.1242 87.5589 37
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0 -2 13 72.9492 204.055 27
0 -2 13 69.1761 68.3432 22
0 2 13 82.1646 70.9079 22
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0 2 14 23771.1 1185.16 16
0 2 14 15377.1 1048.83 30
0 2 -14 22537.5 1202.37 37
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0 -2 14 21283.8 1078.25 22
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0 -2 15 1414.20 141.533 25
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0 -2 -16 37.0741 90.7393 37
0 2 -16-36.3603 91.5709 37
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6 -8 7 211.299 92.3346 23
6 8 7 121.725 49.0129 33
6 -8 8 456.702 86.5854 23
6 8 8 303.086 57.0901 33
6 8 9 4646.28 267.024 33
-6 -9 10 869.054 90.1507 20
-6 -9 9 113.803 59.4412 20
6 -9 -9 168.681 143.291 34
-6 -9 8 495.602 87.6786 20
6 -9 -8 271.559 191.729 34
-6 -9 7 163.303 70.3813 20
6 -9 -7-22.6442 191.945 34
-6 -9 6 3570.36 246.726 20
6 -9 -6 2895.55 344.934 34
-6 -9 5 4154.25 290.757 20
6 -9 -5 4193.43 393.581 34
-6 -9 4 268.011 96.9328 20
6 -9 -4 33.6159 209.905 34
-6 -9 3 363.417 115.552 20
6 -9 -3 534.212 230.371 34
6 -9 -2 389.683 232.087 34
6 -9 -1 159.843 205.665 34
6 9 0 337.113 71.9541 33
6 -9 0 158.164 210.565 34
6 9 1 5742.90 346.182 33
6 9 2 246.982 64.8982 33
6 9 3 91.4510 53.2632 33
6 9 4 273.703 61.3804 33
6 9 5 37.7341 41.3460 33
6 9 6 4017.20 245.524 33
6 9 7 1035.25 92.7735 33
6 9 8 160.871 39.7442 33
-6 -10 9 74.5482 50.4083 20
-6 -10 8 424.986 71.5969 20
6 -10 -8 291.333 133.150 34
-6 -10 7 70.5294 62.8655 20
6 -10 -7 122.398 138.717 34
-6 -10 6 1405.06 133.756 20
6 -10 -6 664.647 196.390 34
-6 -10 5 901.392 117.403 20
6 -10 -5 746.444 206.191 34
-6 -10 4 61.7266 74.2791 20
6 -10 -4-69.6046 185.786 34
-6 -10 3 32.3925 73.6754 20
6 -10 -3 84.8686 175.061 34
-6 -10 2 2488.27 208.942 20
6 -10 -2 2787.87 307.837 34
6 -10 -1 809.353 208.491 34
6 10 -1 515.401 75.1099 33
6 10 0 172.788 52.9567 33
6 10 1 513.638 73.1395 33
6 10 2 21.0262 39.2882 33
6 10 3 470.837 66.7985 33
6 10 4 185.369 47.0886 33
6 10 5 66.5908 35.7976 33
6 10 6-8.67445 32.4018 33
6 10 7 73.5857 29.4848 33
-6 -11 7 171.114 54.5198 20
-6 -11 6 2457.40 155.665 20
6 -11 -6 1144.66 195.236 34
-6 -11 5 1791.22 137.422 20
6 -11 -5 1101.14 192.232 34
-6 -11 4 398.608 81.2289 20
6 -11 -4 282.410 142.838 34
6 11 -3 134.621 42.7069 33
-6 -11 3 339.147 73.2884 20
6 -11 -3 254.747 144.643 34
6 11 -2 180.996 49.8432 33
-6 -11 2 361.479 79.2306 20
6 -11 -2 481.171 161.780 34
6 11 -1 51.0823 34.5826 33
-6 -11 1 55.0693 59.4374 20
6 11 0 301.667 54.3359 33
6 11 2 270.134 48.2207 33
6 11 3 53.4792 30.5606 33
6 11 4 124.637 34.4812 33
6 11 5 75.2121 29.2575 33
-6 -12 5 445.666 65.3188 20
-6 -12 4 93.3140 44.2313 20
6 -12 -4 108.209 93.8126 34
-6 -12 3 32.1106 44.6727 20
6 -12 -3-26.7822 71.3880 21
6 -12 -3 58.0292 99.5604 34
6 -12 -2 2843.33 159.540 21
-6 -12 2 1290.36 128.705 20
6 12 -1 62.3571 32.1288 33
-6 -12 1 75.8093 51.0748 20
6 -12 0 966.801 94.7940 21
6 12 0 296.478 46.2495 33
6 -12 1 670.693 81.1740 21
6 12 1 264.872 42.6271 33
6 -12 2 40.2868 55.3549 21
7 0 -7 38.7739 89.0179 23
7 0 -6 9.35620 131.102 5
7 0 -6 8.99881 269.845 6
7 0 -6 70.6912 101.271 23
7 0 -5 256.068 156.199 5
7 0 -5 560.544 298.081 6
7 0 -5 183.661 117.971 23
7 0 -4 3828.92 284.963 23
7 0 -4 3225.05 325.889 5
7 0 -3 275.731 161.990 5
7 0 -3 510.371 314.702 6
7 0 -3 324.309 133.125 23
7 0 -2 437.001 174.248 5
7 0 -2 581.654 333.874 6
7 0 -2 609.280 142.155 23
7 0 -1-10.9983 153.472 5
7 0 -1-26.7716 117.595 23
7 0 0 1003.82 207.646 5
7 0 0 837.968 157.939 23
7 0 1 3476.43 291.747 23
7 0 1 3970.18 358.933 5
7 0 2 130.000 152.583 5
7 0 2 177.429 127.545 23
7 0 3 1495.24 221.554 5
7 0 3 1125.31 166.023 23
7 0 4 235.990 156.354 5
7 0 4 212.530 121.836 23
7 1 -7 451.034 111.993 23
7 1 -6 134.119 103.261 23
7 -1 -6 267.477 111.607 23
7 1 -5 2016.11 200.417 23
7 -1 -5 2817.60 221.092 23
7 1 -5 1538.03 231.638 5
7 1 -5 1908.04 336.669 6
7 -1 -5 1747.84 355.256 6
7 -1 -5 1965.40 250.905 5
7 1 -4-19.1056 136.600 5
7 -1 -4 190.007 154.393 5
7 1 -4 243.951 286.058 6
7 -1 -4-250.128 332.283 6
7 1 -4 224.837 105.488 23
7 -1 -4 43.4628 126.545 23
7 1 -3 215.613 151.092 5
7 -1 -3 76.0222 152.839 5
7 1 -3 284.958 297.005 6
7 -1 -3-229.289 347.563 6
7 1 -3 17.5156 106.298 23
7 -1 -3 155.756 125.788 23
7 1 -2 2046.89 203.953 23
7 -1 -2 2425.91 227.509 23
7 1 -2 1877.00 368.884 6
7 -1 -2 1863.35 396.428 6
7 1 -2 1965.72 254.301 5
7 -1 -2 2086.65 278.435 5
7 1 -1 819.225 184.897 5
7 -1 -1 1198.68 206.168 5
7 1 -1 749.430 145.707 23
7 -1 -1 894.775 163.417 23
7 1 0 2611.22 245.654 23
7 -1 0 3271.45 267.081 23
7 1 0 2970.19 302.553 5
7 -1 0 3039.85 319.036 5
7 1 1-41.2757 144.574 5
7 -1 1-33.8525 159.368 5
7 1 1 101.808 116.243 23
7 -1 1-107.805 141.093 23
7 1 2 61.3418 136.746 5
7 -1 2 22.1528 157.060 5
7 1 2 40.5441 110.770 23
7 -1 2 6.56267 128.193 23
7 1 3 80.5276 142.727 5
7 -1 3 21.5176 151.949 5
7 1 3 77.1892 107.471 23
7 -1 3-88.6528 128.964 23
7 -1 4 7411.66 485.015 23
7 1 4 8227.15 554.395 5
7 -1 4 8700.88 570.468 5
7 2 -6 56.4642 84.9300 23
7 -2 -6 114.990 95.2080 23
7 2 -5 120.094 117.647 5
7 -2 -5 144.286 134.401 5
7 2 -5 164.980 246.996 6
7 -2 -5 53.5778 292.397 6
7 2 -5 125.784 91.2174 23
7 -2 -5 146.329 110.557 23
7 2 -4 3407.86 258.701 23
7 2 -4 2743.98 377.675 6
7 -2 -4 3154.65 409.934 6
7 2 -4 3065.81 302.118 5
7 -2 -4 3777.67 336.532 5
7 2 -3 280.112 134.013 5
7 -2 -3 311.797 158.342 5
7 2 -3 43.9126 272.925 6
7 -2 -3 192.826 312.912 6
7 2 -3 328.171 115.949 23
7 -2 -3 475.536 135.733 23
7 2 -2-26.8416 127.379 5
7 -2 -2 51.5745 148.556 5
7 2 -2 137.361 279.868 6
7 -2 -2 233.231 327.818 6
7 2 -2 53.0277 99.4319 23
7 -2 -2 63.8432 120.776 23
7 2 -1 368.822 151.230 5
7 -2 -1 531.194 172.071 5
7 2 -1 588.813 125.383 23
7 -2 -1 600.168 142.838 23
7 2 0 904.058 176.920 5
7 -2 0 1272.73 211.752 5
7 2 0 730.497 139.657 23
7 -2 0 1304.84 176.667 23
7 -2 1 3505.64 284.901 23
7 2 1 3249.86 318.969 5
7 -2 1 4107.67 354.320 5
7 2 2 213.653 139.499 5
7 -2 2 166.306 148.169 5
7 -2 2 121.358 124.491 23
7 2 3 321.148 141.923 5
7 -2 3 342.794 149.966 5
7 -2 3 376.702 139.576 23
7 -2 4-105.957 121.129 23
7 3 -5 3129.25 235.019 23
7 -3 -5 3781.60 255.212 23
7 -3 -4 313.787 139.193 5
7 3 -4 295.585 96.7274 23
7 -3 -4 370.418 112.883 23
7 3 -3 749.310 146.276 5
7 -3 -3 857.409 174.769 5
7 3 -3 652.558 269.824 6
7 -3 -3 492.845 310.810 6
7 3 -3 832.262 123.101 23
7 -3 -3 908.397 151.322 23
7 -3 -2 2542.14 221.342 23
7 -3 -2 2449.05 261.673 5
7 3 -1 995.979 169.709 5
7 -3 -1 1112.98 194.610 5
7 -3 -1 1001.76 163.064 23
7 -3 0 4368.69 327.702 23
7 -3 0 4850.61 381.651 5
7 3 1 72.7486 115.520 5
7 -3 1 104.953 135.292 5
7 -3 1-54.6654 120.842 23
7 3 2 202.362 122.312 5
7 -3 2 178.069 135.053 5
7 -3 2-35.7660 117.737 23
7 -3 3 247.609 120.526 23
7 -3 4 6691.25 420.424 23
7 -4 -4 4665.58 308.418 23
7 -4 -3 423.912 109.013 23
7 -4 -2 98.3476 100.795 23
7 -4 -1 199.719 112.425 23
7 -4 0 281.926 118.210 23
7 -4 1 3811.49 284.567 23
7 -4 2 234.001 115.740 23
7 -4 3 890.077 142.500 23
7 -5 -1 829.733 126.092 23
7 -5 0 2881.00 227.603 23
7 -5 1 72.1884 96.3751 23
0 0 0 0.00 0.00 0
TITL ACT_BrI_orange_smartabscorr in P2(1)/m
REM P2(1)/m (#11 in standard setting)
CELL 1.54184 5.895595 18.642444 19.963184 90.0000 91.9697 90.0000
ZERR 4.00 0.000123 0.000402 0.000393 0.0000 0.0018 0.0000
LATT 1
SYMM -x, y+1/2,-z
SFAC C H N O Br I
UNIT 64.00 80.00 8.00 8.00 8.00 24.00
REM CrysAlisPro recorded range (K): Min=99.4; max=100.5; aver:99.9
TEMP -173
SIZE 0.06 0.08 0.24
TREF
HKLF 4
END
;
_shelx_hkl_checksum 26007
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/m
shelx.res
created by SHELXL-2018/3 at 15:17:26 on 29-May-2024
CELL 1.54184 5.8956 18.6224 19.9632 90.000 91.970 90.000
ZERR 4.00 0.0001 0.0004 0.0004 0.000 0.002 0.000
LATT 1
SYMM - X, 1/2 + Y, - Z
SFAC I BR O N C H
UNIT 12.276 3.724 8 8 64 76
MERG 2
OMIT -3.00 180.00
dfix .88 .01 n1 h1n n2 h2n
EADP Br3 I5
eadp br1 i7
EQIV $1 -x, -y+1, -z+2
HTAB N1 Br2
HTAB N2 Br1
HTAB O1 O1_$1
EQIV $2 -x-1, -y+1, -z+1
HTAB O2 O2_$2
FMAP 2
PLAN 20
ACTA 140.00
BOND $H
CONF
L.S. 10
TEMP -173.00
WGHT 0.106600
FVAR 1.35654 0.87187 0.73403
I1 1 -0.354723 0.250000 0.679633 10.50000 0.04086 0.07465 =
0.05239 0.00000 0.00112 0.00000
I2 1 0.018897 0.250000 0.764172 10.50000 0.04076 0.06223 =
0.05250 0.00000 0.00154 0.00000
I3 1 0.799821 0.250000 1.143083 10.50000 0.06083 0.05679 =
0.05734 0.00000 -0.00900 0.00000
I4 1 0.606325 0.250000 1.015969 10.50000 0.04260 0.04803 =
0.05671 0.00000 -0.00342 0.00000
PART 1
I5 1 0.258341 0.250000 0.277781 20.50000 0.12093 0.05873 =
0.04240 0.00000 -0.00161 0.00000
PART 0
I6 1 0.213827 0.250000 0.415349 10.50000 0.06478 0.05045 =
0.04563 0.00000 -0.00932 0.00000
PART 1
BR1 2 0.187233 0.250000 0.562323 30.50000 0.03988 0.05678 =
0.04523 0.00000 0.00476 0.00000
PART 0
BR2 2 0.453019 0.250000 0.868158 10.50000 0.04678 0.04704 =
0.04602 0.00000 0.00235 0.00000
PART 2
BR3 2 0.376987 0.250000 0.278569 -20.50000 0.12093 0.05873 =
0.04240 0.00000 -0.00161 0.00000
I7 1 0.163457 0.250000 0.567184 -30.50000 0.03988 0.05678 =
0.04523 0.00000 0.00476 0.00000
PART 0
O1 3 0.168297 0.498361 0.966074 11.00000 0.04970 0.05293 =
0.04909 0.00108 0.00638 0.00218
AFIX 3
H1H 6 0.076093 0.499548 0.999810 10.50000 -1.20000
AFIX 0
O2 3 -0.323895 0.496881 0.533509 11.00000 0.05065 0.06802 =
0.05602 0.00447 -0.01493 0.00227
AFIX 3
H2H 6 -0.446965 0.490872 0.508030 10.50000 -1.20000
AFIX 0
N1 4 0.379795 0.425142 0.903318 11.00000 0.04466 0.04810 =
0.05252 0.00234 0.00493 0.00157
N2 4 -0.064177 0.421592 0.580140 11.00000 0.04679 0.05903 =
0.05890 0.00393 -0.00960 -0.00477
C1 5 0.071512 0.373088 0.963747 11.00000 0.04089 0.05098 =
0.05884 0.00448 0.00594 0.00199
AFIX 137
H1A 6 0.098353 0.362739 1.011495 11.00000 -1.50000
H1B 6 0.113691 0.331174 0.937228 11.00000 -1.50000
H1C 6 -0.089496 0.384005 0.955193 11.00000 -1.50000
AFIX 0
C2 5 0.212672 0.436534 0.944298 11.00000 0.04426 0.05103 =
0.04141 0.00216 -0.00012 0.00685
C3 5 0.541926 0.473520 0.877395 11.00000 0.04695 0.05460 =
0.03986 0.00565 -0.00544 -0.00235
C4 5 0.536231 0.547818 0.887008 11.00000 0.04671 0.05509 =
0.05405 0.00556 -0.00008 0.00699
AFIX 43
H4 6 0.419452 0.569179 0.911890 11.00000 -1.20000
AFIX 0
C5 5 0.705192 0.590274 0.859419 11.00000 0.04965 0.05401 =
0.05399 0.00475 -0.00335 -0.00300
AFIX 43
H5 6 0.702697 0.640867 0.865450 11.00000 -1.20000
AFIX 0
C6 5 0.875915 0.559129 0.823412 11.00000 0.05008 0.06319 =
0.05055 0.00791 -0.00533 -0.00822
AFIX 43
H6 6 0.991771 0.588384 0.805864 11.00000 -1.20000
AFIX 0
C7 5 0.879158 0.485712 0.812774 11.00000 0.04795 0.06669 =
0.04399 0.00580 -0.00248 0.00160
AFIX 43
H7 6 0.994642 0.464790 0.787078 11.00000 -1.20000
AFIX 0
C8 5 0.711626 0.442409 0.840020 11.00000 0.04521 0.05545 =
0.04900 0.00008 -0.00735 0.00583
AFIX 43
H8 6 0.713507 0.391949 0.833071 11.00000 -1.20000
AFIX 0
C9 5 -0.351451 0.372288 0.504174 11.00000 0.04554 0.07478 =
0.06084 0.00657 -0.00761 -0.00862
AFIX 137
H9A 6 -0.498372 0.362062 0.523622 11.00000 -1.50000
H9B 6 -0.253279 0.329991 0.508838 11.00000 -1.50000
H9C 6 -0.374370 0.384069 0.456578 11.00000 -1.50000
AFIX 0
C10 5 -0.242583 0.434182 0.539850 11.00000 0.04820 0.06509 =
0.04805 0.00506 -0.00478 -0.00811
C11 5 0.075131 0.469271 0.618671 11.00000 0.04734 0.07124 =
0.04533 0.00089 -0.00419 -0.00849
C12 5 0.026182 0.541554 0.628290 11.00000 0.05375 0.07106 =
0.05905 0.00939 -0.01298 -0.01584
AFIX 43
H12 6 -0.107929 0.562506 0.609158 11.00000 -1.20000
AFIX 0
C13 5 0.180303 0.582338 0.666936 11.00000 0.07679 0.07668 =
0.05182 -0.00054 -0.01060 -0.01265
AFIX 43
H13 6 0.150763 0.631944 0.673515 11.00000 -1.20000
AFIX 0
C14 5 0.372764 0.552794 0.695595 11.00000 0.05505 0.11368 =
0.04438 -0.00025 -0.00393 -0.02180
AFIX 43
H14 6 0.475421 0.581829 0.721396 11.00000 -1.20000
AFIX 0
C15 5 0.417486 0.480373 0.686867 11.00000 0.04927 0.10690 =
0.05591 -0.00905 -0.01277 0.00649
AFIX 43
H15 6 0.550402 0.459333 0.706665 11.00000 -1.20000
AFIX 0
C16 5 0.266102 0.439186 0.648973 11.00000 0.04633 0.08708 =
0.05123 -0.00594 -0.00672 0.00302
AFIX 43
H16 6 0.294132 0.389301 0.643721 11.00000 -1.20000
AFIX 0
H1N 6 0.408320 0.379774 0.895210 11.00000 0.04671
H2N 6 -0.008504 0.378019 0.584390 11.00000 0.05093
HKLF 4
REM shelxt_a.res in P2(1)/m
REM wR2 = 0.1508, GooF = S = 1.077, Restrained GooF = 1.076 for all data
REM R1 = 0.0516 for 3762 Fo > 4sig(Fo) and 0.0564 for all 4338 data
REM 245 parameters refined using 2 restraints
END
WGHT 0.1066 0.0000
REM Highest difference peak 1.495, deepest hole -1.862, 1-sigma level 0.195
Q1 1 0.2207 0.2500 0.2645 10.50000 0.05 1.40
Q2 1 0.7220 0.2760 1.0491 11.00000 0.05 1.28
Q3 1 -0.2634 0.2766 0.7058 11.00000 0.05 1.16
Q4 1 0.4901 0.2500 1.0761 10.50000 0.05 1.14
Q5 1 0.6803 0.2820 1.1128 11.00000 0.05 1.11
Q6 1 -0.0808 0.2784 0.7363 11.00000 0.05 1.08
Q7 1 0.0674 0.2500 0.4759 10.50000 0.05 1.06
Q8 1 0.3323 0.2812 0.4446 11.00000 0.05 1.04
Q9 1 0.4948 0.2813 0.9852 11.00000 0.05 1.03
Q10 1 -0.4871 0.2680 0.6397 11.00000 0.05 0.99
Q11 1 0.1338 0.2770 0.7940 11.00000 0.05 0.98
Q12 1 0.1027 0.2821 0.3853 11.00000 0.05 0.94
Q13 1 0.9109 0.2500 1.0854 10.50000 0.05 0.93
Q14 1 -0.1271 0.2500 0.8131 10.50000 0.05 0.87
Q15 1 0.9161 0.2830 1.1739 11.00000 0.05 0.86
Q16 1 0.2971 0.2500 0.9447 10.50000 0.05 0.82
Q17 1 0.3282 0.2500 0.4927 10.50000 0.05 0.82
Q18 1 0.3483 0.2500 0.3614 10.50000 0.05 0.81
Q19 1 0.0642 0.2720 0.5319 11.00000 0.05 0.79
Q20 1 0.3066 0.2751 0.5021 11.00000 0.05 0.78
;
_shelx_res_checksum 91624
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
I I1 -0.35472(12) 0.250000 0.67963(3) 0.0560(2) Uani d 1 . .
I I2 0.01890(11) 0.250000 0.76417(3) 0.05183(19) Uani d 1 . .
I I3 0.79982(13) 0.250000 1.14308(3) 0.0586(2) Uani d 1 . .
I I4 0.60633(11) 0.250000 1.01597(3) 0.04923(19) Uani d 1 . .
I I5 0.2583(5) 0.250000 0.27778(5) 0.0741(7) Uani d 0.872(9) A 1
I I6 0.21383(12) 0.250000 0.41535(3) 0.0539(2) Uani d 1 . .
Br Br1 0.187(3) 0.250000 0.5623(9) 0.0472(13) Uani d 0.734(9) A 1
Br Br2 0.45302(18) 0.250000 0.86816(5) 0.0466(2) Uani d 1 . .
Br Br3 0.377(5) 0.250000 0.2786(6) 0.0741(7) Uani d 0.128(9) A 2
I I7 0.163(5) 0.250000 0.5672(16) 0.0472(13) Uani d 0.266(9) A 2
O O1 0.1683(9) 0.4984(2) 0.9661(2) 0.0505(10) Uani d 1 . .
H H1H 0.076093 0.499548 0.999810 0.061 Uiso d 0.5 . .
O O2 -0.3239(9) 0.4969(3) 0.5335(3) 0.0586(12) Uani d 1 . .
H H2H -0.446965 0.490872 0.508030 0.070 Uiso d 0.5 . .
N N1 0.3798(10) 0.4251(3) 0.9033(3) 0.0484(12) Uani d 1 . .
N N2 -0.0642(11) 0.4216(3) 0.5801(3) 0.0552(14) Uani d 1 . .
C C1 0.0715(12) 0.3731(3) 0.9637(4) 0.0501(14) Uani d 1 . .
H H1A 0.098353 0.362739 1.011495 0.075 Uiso calc 1 . .
H H1B 0.113691 0.331174 0.937228 0.075 Uiso calc 1 . .
H H1C -0.089496 0.384005 0.955193 0.075 Uiso calc 1 . .
C C2 0.2127(12) 0.4365(3) 0.9443(3) 0.0456(13) Uani d 1 . .
C C3 0.5419(12) 0.4735(3) 0.8774(3) 0.0473(14) Uani d 1 . .
C C4 0.5362(13) 0.5478(4) 0.8870(4) 0.0520(16) Uani d 1 . .
H H4 0.419452 0.569179 0.911890 0.062 Uiso calc 1 . .
C C5 0.7052(13) 0.5903(4) 0.8594(4) 0.0527(15) Uani d 1 . .
H H5 0.702697 0.640867 0.865450 0.063 Uiso calc 1 . .
C C6 0.8759(14) 0.5591(4) 0.8234(4) 0.0548(16) Uani d 1 . .
H H6 0.991771 0.588384 0.805864 0.066 Uiso calc 1 . .
C C7 0.8792(13) 0.4857(4) 0.8128(4) 0.0530(15) Uani d 1 . .
H H7 0.994642 0.464790 0.787078 0.064 Uiso calc 1 . .
C C8 0.7116(13) 0.4424(4) 0.8400(3) 0.0501(15) Uani d 1 . .
H H8 0.713507 0.391949 0.833071 0.060 Uiso calc 1 . .
C C9 -0.3515(13) 0.3723(4) 0.5042(4) 0.0606(18) Uani d 1 . .
H H9A -0.498372 0.362062 0.523622 0.091 Uiso calc 1 . .
H H9B -0.253279 0.329991 0.508838 0.091 Uiso calc 1 . .
H H9C -0.374370 0.384069 0.456578 0.091 Uiso calc 1 . .
C C10 -0.2426(14) 0.4342(4) 0.5399(4) 0.0539(16) Uani d 1 . .
C C11 0.0751(14) 0.4693(4) 0.6187(4) 0.0548(16) Uani d 1 . .
C C12 0.0262(15) 0.5416(4) 0.6283(4) 0.0616(19) Uani d 1 . .
H H12 -0.107929 0.562506 0.609158 0.074 Uiso calc 1 . .
C C13 0.1803(17) 0.5823(5) 0.6669(4) 0.069(2) Uani d 1 . .
H H13 0.150763 0.631944 0.673515 0.082 Uiso calc 1 . .
C C14 0.3728(16) 0.5528(6) 0.6956(4) 0.071(2) Uani d 1 . .
H H14 0.475421 0.581829 0.721396 0.085 Uiso calc 1 . .
C C15 0.4175(16) 0.4804(5) 0.6869(4) 0.071(2) Uani d 1 . .
H H15 0.550402 0.459333 0.706665 0.085 Uiso calc 1 . .
C C16 0.2661(14) 0.4392(5) 0.6490(4) 0.0617(19) Uani d 1 . .
H H16 0.294132 0.389301 0.643721 0.074 Uiso calc 1 . .
H H1N 0.408(13) 0.3798(12) 0.895(3) 0.047(19) Uiso d 1 . .
H H2N -0.009(13) 0.3780(18) 0.584(4) 0.05(2) 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
I1 0.0409(4) 0.0747(4) 0.0524(4) 0.000 0.0011(3) 0.000
I2 0.0408(4) 0.0622(3) 0.0525(4) 0.000 0.0015(3) 0.000
I3 0.0608(5) 0.0568(3) 0.0573(4) 0.000 -0.0090(3) 0.000
I4 0.0426(4) 0.0480(3) 0.0567(4) 0.000 -0.0034(3) 0.000
I5 0.1209(18) 0.0587(4) 0.0424(4) 0.000 -0.0016(6) 0.000
I6 0.0648(5) 0.0505(3) 0.0456(3) 0.000 -0.0093(3) 0.000
Br1 0.040(3) 0.0568(5) 0.045(2) 0.000 0.0048(19) 0.000
Br2 0.0468(6) 0.0470(4) 0.0460(5) 0.000 0.0023(4) 0.000
Br3 0.1209(18) 0.0587(4) 0.0424(4) 0.000 -0.0016(6) 0.000
I7 0.040(3) 0.0568(5) 0.045(2) 0.000 0.0048(19) 0.000
O1 0.050(3) 0.053(2) 0.049(2) 0.002(2) 0.006(2) 0.0011(18)
O2 0.051(3) 0.068(3) 0.056(3) 0.002(2) -0.015(2) 0.004(2)
N1 0.045(3) 0.048(2) 0.053(3) 0.002(2) 0.005(3) 0.002(2)
N2 0.047(4) 0.059(3) 0.059(3) -0.005(3) -0.010(3) 0.004(2)
C1 0.041(4) 0.051(3) 0.059(4) 0.002(3) 0.006(3) 0.004(3)
C2 0.044(4) 0.051(3) 0.041(3) 0.007(3) 0.000(3) 0.002(2)
C3 0.047(4) 0.055(3) 0.040(3) -0.002(3) -0.005(3) 0.006(2)
C4 0.047(4) 0.055(3) 0.054(4) 0.007(3) 0.000(3) 0.006(3)
C5 0.050(4) 0.054(3) 0.054(4) -0.003(3) -0.003(3) 0.005(3)
C6 0.050(4) 0.063(4) 0.051(4) -0.008(3) -0.005(3) 0.008(3)
C7 0.048(4) 0.067(4) 0.044(3) 0.002(3) -0.002(3) 0.006(3)
C8 0.045(4) 0.055(3) 0.049(4) 0.006(3) -0.007(3) 0.000(3)
C9 0.046(4) 0.075(4) 0.061(4) -0.009(3) -0.008(3) 0.007(3)
C10 0.048(4) 0.065(4) 0.048(4) -0.008(3) -0.005(3) 0.005(3)
C11 0.047(4) 0.071(4) 0.045(3) -0.008(3) -0.004(3) 0.001(3)
C12 0.054(5) 0.071(4) 0.059(4) -0.016(4) -0.013(4) 0.009(3)
C13 0.077(6) 0.077(4) 0.052(4) -0.013(4) -0.011(4) -0.001(3)
C14 0.055(5) 0.114(7) 0.044(4) -0.022(5) -0.004(3) 0.000(4)
C15 0.049(5) 0.107(6) 0.056(4) 0.006(4) -0.013(4) -0.009(4)
C16 0.046(4) 0.087(5) 0.051(4) 0.003(4) -0.007(3) -0.006(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.3257 6.8362 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
I5 I6 Br1 . . 177.6(4) ?
Br3 I6 I7 . . 166.4(9) ?
C2 O1 H1H . . 115.3 ?
C10 O2 H2H . . 104.0 ?
C2 N1 C3 . . 130.4(6) ?
C2 N1 H1N . . 115(5) ?
C3 N1 H1N . . 114(5) ?
C10 N2 C11 . . 130.7(6) ?
C10 N2 H2N . . 121(5) ?
C11 N2 H2N . . 109(5) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 N1 . . 121.9(6) ?
O1 C2 C1 . . 120.3(6) ?
N1 C2 C1 . . 117.7(5) ?
C8 C3 C4 . . 120.4(7) ?
C8 C3 N1 . . 115.8(6) ?
C4 C3 N1 . . 123.8(7) ?
C3 C4 C5 . . 119.0(7) ?
C3 C4 H4 . . 120.5 ?
C5 C4 H4 . . 120.5 ?
C6 C5 C4 . . 120.5(6) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C7 C6 C5 . . 120.5(7) ?
C7 C6 H6 . . 119.7 ?
C5 C6 H6 . . 119.7 ?
C6 C7 C8 . . 119.7(8) ?
C6 C7 H7 . . 120.1 ?
C8 C7 H7 . . 120.1 ?
C3 C8 C7 . . 119.8(6) ?
C3 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
C10 C9 H9A . . 109.5 ?
C10 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C10 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
O2 C10 N2 . . 121.0(7) ?
O2 C10 C9 . . 120.7(7) ?
N2 C10 C9 . . 118.3(7) ?
C16 C11 C12 . . 120.2(7) ?
C16 C11 N2 . . 115.6(7) ?
C12 C11 N2 . . 124.2(7) ?
C11 C12 C13 . . 117.9(8) ?
C11 C12 H12 . . 121.0 ?
C13 C12 H12 . . 121.0 ?
C14 C13 C12 . . 121.8(9) ?
C14 C13 H13 . . 119.1 ?
C12 C13 H13 . . 119.1 ?
C13 C14 C15 . . 119.8(8) ?
C13 C14 H14 . . 120.1 ?
C15 C14 H14 . . 120.1 ?
C16 C15 C14 . . 119.1(8) ?
C16 C15 H15 . . 120.4 ?
C14 C15 H15 . . 120.4 ?
C11 C16 C15 . . 121.1(8) ?
C11 C16 H16 . . 119.4 ?
C15 C16 H16 . . 119.4 ?
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
I1 I2 . 2.7285(9) ?
I3 I4 . 2.7462(9) ?
I5 I6 . 2.7678(12) ?
I6 Br3 . 2.926(17) ?
I6 Br1 . 2.944(18) ?
I6 I7 . 3.06(3) ?
O1 C2 . 1.261(8) ?
O1 H1H . 0.8802 ?
O2 C10 . 1.267(9) ?
O2 H2H . 0.8788 ?
N1 C2 . 1.319(9) ?
N1 C3 . 1.424(9) ?
N1 H1N . 0.878(10) ?
N2 C10 . 1.323(10) ?
N2 C11 . 1.418(9) ?
N2 H2N . 0.878(10) ?
C1 C2 . 1.504(9) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C3 C8 . 1.395(10) ?
C3 C4 . 1.397(9) ?
C4 C5 . 1.399(10) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.384(11) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.384(10) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.400(11) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
C9 C10 . 1.489(10) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C11 C16 . 1.379(11) ?
C11 C12 . 1.391(11) ?
C12 C13 . 1.396(11) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.369(14) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.386(14) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.382(11) ?
C15 H15 . 0.9500 ?
C16 H16 . 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_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N Br2 . 0.878(10) 2.492(14) 3.367(5) 175(7) yes
N2 H2N Br1 . 0.878(10) 2.69(2) 3.546(10) 164(7) yes
O1 H1H O1 3_567 0.88 1.62 2.442(10) 155.0 yes
O2 H2H O2 3_466 0.88 1.58 2.434(10) 164.0 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
C3 N1 C2 O1 . . . . 2.3(11) ?
C3 N1 C2 C1 . . . . -178.8(6) ?
C2 N1 C3 C8 . . . . 173.9(7) ?
C2 N1 C3 C4 . . . . -6.8(11) ?
C8 C3 C4 C5 . . . . -0.9(10) ?
N1 C3 C4 C5 . . . . 179.7(6) ?
C3 C4 C5 C6 . . . . -0.3(10) ?
C4 C5 C6 C7 . . . . 1.5(11) ?
C5 C6 C7 C8 . . . . -1.6(11) ?
C4 C3 C8 C7 . . . . 0.9(10) ?
N1 C3 C8 C7 . . . . -179.7(6) ?
C6 C7 C8 C3 . . . . 0.3(10) ?
C11 N2 C10 O2 . . . . -4.2(13) ?
C11 N2 C10 C9 . . . . 178.2(8) ?
C10 N2 C11 C16 . . . . -172.1(8) ?
C10 N2 C11 C12 . . . . 9.7(14) ?
C16 C11 C12 C13 . . . . 2.5(12) ?
N2 C11 C12 C13 . . . . -179.3(8) ?
C11 C12 C13 C14 . . . . -0.9(14) ?
C12 C13 C14 C15 . . . . -0.5(14) ?
C13 C14 C15 C16 . . . . 0.2(14) ?
C12 C11 C16 C15 . . . . -2.9(13) ?
N2 C11 C16 C15 . . . . 178.8(8) ?
C14 C15 C16 C11 . . . . 1.5(14) ?