#------------------------------------------------------------------------------
#$Date: 2018-10-25 05:40:06 +0300 (Thu, 25 Oct 2018) $
#$Revision: 211615 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/12/2021280.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_2021280
loop_
_publ_author_name
'Owczarzak, Agata'
'Przyby\/l, Anna K.'
'Kubicki, Maciej'
_publ_section_title
;
Different cationic forms of (--)-cytisine in the crystal structures of
its simple inorganic salts
;
_journal_coeditor_code YF3149
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229618012585
_journal_volume 74
_journal_year 2018
_chemical_absolute_configuration syn
_chemical_formula_iupac 'C11 H15 N2 O +, Br -'
_chemical_formula_moiety 'C11 H15 N2 O +, Br -'
_chemical_formula_sum 'C11 H15 Br N2 O'
_chemical_formula_weight 271.16
_chemical_name_common
;
Cytisinium bromide
;
_chemical_name_systematic
;
6-Oxo-7,11-diazatricyclo[7.3.1.0^2,7^]trideca-2,4-dien-11-ium bromide
;
_space_group_crystal_system trigonal
_space_group_IT_number 145
_space_group_name_Hall 'P 32'
_space_group_name_H-M_alt 'P 32'
_symmetry_space_group_name_Hall 'P 32'
_symmetry_space_group_name_H-M 'P 32'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2013
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 7.3942(2)
_cell_length_b 7.3942(2)
_cell_length_c 17.4657(4)
_cell_measurement_reflns_used 4385
_cell_measurement_temperature 100.0(10)
_cell_measurement_theta_max 27.9210
_cell_measurement_theta_min 3.1570
_cell_volume 826.99(4)
_computing_cell_refinement
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_collection
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_reduction
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Agilent Xcalibur Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0505
_diffrn_reflns_av_unetI/netI 0.0509
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 9856
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.991
_diffrn_reflns_theta_min 3.181
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 3.703
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.76982
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.633
_exptl_crystal_description plate
_exptl_crystal_F_000 414
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.549
_refine_diff_density_min -0.250
_refine_ls_abs_structure_details
;
Flack x determined using 919 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack -0.016(7)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.996
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 144
_refine_ls_number_reflns 2153
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.996
_refine_ls_R_factor_all 0.0334
_refine_ls_R_factor_gt 0.0273
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0115P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0451
_refine_ls_wR_factor_ref 0.0466
_reflns_number_gt 1987
_reflns_number_total 2153
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yf3149sup1.cif
_cod_data_source_block 1
_cod_original_cell_volume 826.99(5)
_cod_database_code 2021280
_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
;
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0 0 -3 10364.6 419.893 4
0 0 -3 10177.6 522.368 5
0 0 -4-114.627 67.6455 2
0 0 4 42.5153 121.426 9
0 0 4-47.1008 121.668 4
0 0 4 14.8343 63.5551 2
0 0 -4-15.7680 132.086 4
0 0 -4-110.262 120.408 1
0 0 -4-43.3112 118.647 9
0 0 -5 68.6014 144.744 4
0 0 5 250.528 159.946 4
0 0 5-12.9735 75.0541 2
0 0 -5-397.218 259.140 5
0 0 -5-21.1688 125.442 1
0 0 5 122.856 168.845 9
0 0 -5-104.208 130.579 9
0 0 -5-0.20536 67.6055 2
0 0 -5 98.7638 80.1206 8
0 0 6 102564. 3199.06 4
0 0 -6 106148. 3184.37 1
0 0 -6 104895. 2903.84 2
0 0 -6 95930.1 3466.67 5
0 0 6 100023. 3236.94 9
0 0 6 99755.3 2895.13 2
0 0 -6 105014. 2900.88 8
0 0 -6 107363. 3283.12 9
0 0 -6 108438. 3205.07 4
0 0 -7-56.0775 151.360 1
0 0 -7 388.841 201.886 9
0 0 -7 168.178 276.760 5
0 0 -7-8.30770 71.0584 2
0 0 -7 176.105 172.332 4
0 0 7-112.108 149.669 4
0 0 7 163.372 94.1886 2
0 0 7 99.8323 190.128 9
0 0 -7-47.3971 78.4017 8
0 0 8 29.3218 171.458 9
0 0 -8-31.1931 164.297 4
0 0 -8 45.1100 74.3808 8
0 0 -8 7.31302 159.151 9
0 0 -8-33.8726 83.0037 2
0 0 8 140.244 179.746 4
0 0 -8-15.4981 296.380 5
0 0 -8-2.56100 140.896 1
0 0 -9 26737.9 962.556 8
0 0 -9 25116.6 1574.29 5
0 0 -9 26752.2 1307.26 4
0 0 9 27695.1 1370.69 9
0 0 -9 27446.6 969.215 2
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0 0 -9 27812.0 1282.89 1
0 0 -10-61.9639 158.036 1
0 0 -10 73.6777 80.8805 8
0 0 -10-254.366 217.299 4
0 0 10 233.128 215.957 9
0 0 -10 158.066 368.835 5
0 0 -10 122.094 91.6742 2
0 0 -11 88.1318 81.7192 8
0 0 -11-192.967 269.498 5
0 0 -11-1.65293 226.749 4
0 0 11-119.887 208.040 9
0 0 -12 53886.5 1718.65 8
0 0 -12 52868.3 2764.03 5
0 0 -12 55422.1 2305.40 4
0 0 12 52168.4 2358.07 9
0 0 13 4.11088 246.532 9
0 0 -13 163.457 97.9406 8
0 0 -13-68.4998 235.040 4
0 0 -13 234.964 457.849 5
0 0 14-245.061 294.822 9
0 0 -14 2.19662 277.907 4
0 0 -14-52.2628 63.3358 8
0 0 -15 19796.6 1350.36 4
0 0 15 17960.9 1354.68 9
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0 0 16-27.8498 276.698 9
0 0 -16-10.8093 273.298 4
0 0 -16 558.272 465.942 5
0 0 17-154.800 337.730 9
0 0 -17 169.730 260.654 4
0 0 -17-41.3612 506.922 5
0 0 -18 16583.1 1846.25 5
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0 0 -19-15.4867 552.988 5
0 0 19 299.484 338.228 9
0 0 -19 748.439 420.518 4
0 0 -20-33.4919 437.903 5
0 0 -20-242.080 395.643 4
0 0 20-184.951 348.071 9
0 0 21 17615.6 1634.99 9
0 0 -21 17547.1 2052.02 5
0 0 22 232.368 396.558 9
0 0 23 832.177 536.203 9
1 -1 23 78.8740 371.932 9
1 -1 22 4962.51 941.046 9
0 1 22 6270.79 992.231 9
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0 1 21-47.0011 332.766 9
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0 -1 -20 2683.17 659.791 4
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4 -9 1 9678.47 1374.04 1
-9 5 1 10821.7 1393.18 2
-5 -4 -1 10954.7 1572.62 1
9 -5 -1 10997.1 1401.25 8
-4 9 0 1171.98 571.732 7
5 4 0 1366.67 670.577 7
-9 5 0 544.208 539.731 3
-5 -4 0-681.619 640.319 3
-5 -4 0 272.477 534.940 1
4 -9 0 62.3908 399.746 1
-9 5 0-98.6953 428.779 2
9 -5 0 456.631 436.169 8
5 4 -1-591.623 515.384 7
-5 -4 1 1071.83 591.962 1
-9 5 -1 92.0381 521.790 3
-5 -4 1 25.0206 507.539 3
4 -9 -1-208.544 421.193 1
-9 5 -1 376.975 449.939 2
9 -5 1 361.555 501.975 8
-5 -4 2 8076.63 1302.95 1
5 4 -2 4958.17 1094.54 7
-9 5 -2 5108.70 919.928 3
-5 -4 2 3907.96 918.843 3
4 -9 -2 4709.44 941.012 1
-9 5 -2 5917.11 1021.21 2
9 -5 2 5238.64 958.519 8
5 4 -3 451.647 607.071 7
-9 5 -3 1268.57 477.820 3
-5 -4 3 216.682 436.228 3
4 -9 -3-201.002 446.749 1
-9 5 -3 680.919 496.705 2
9 -5 3 470.962 368.982 8
-5 -4 3 867.048 513.667 1
5 4 -4 479.392 528.726 7
-5 -4 4 631.791 540.774 3
4 -9 -4 880.478 529.797 1
-5 -4 4 1509.71 645.984 1
-9 5 -4 532.193 490.798 2
9 -5 4 916.122 562.191 8
-9 5 -5 7023.17 1026.68 4
5 4 -5 6931.52 1201.61 7
-4 9 5 8411.02 1333.79 2
-5 -4 5 7047.03 1194.48 3
5 4 -5 6013.33 1192.77 6
-5 -4 5 8482.80 1285.93 1
4 -9 -5 6591.04 1086.75 1
-9 5 -5 6682.50 1035.40 2
9 -5 5 8741.54 1170.18 8
-9 5 -6 574.598 578.384 4
5 4 -6 344.221 524.297 7
-5 -4 6-1076.32 716.261 3
5 4 -6-789.778 695.789 6
-5 -4 6-191.969 450.668 1
9 -5 6 583.044 443.798 8
-9 5 -7 37.3815 488.035 4
5 4 -7-538.602 626.445 7
-5 -4 7 328.421 396.859 3
-5 -4 7 420.974 561.817 1
5 4 -7-131.066 662.466 6
-9 5 -8 5608.72 1016.48 4
-5 -4 8 5580.33 1032.97 1
5 4 -8 5232.45 1130.31 7
-5 -4 8 4153.67 891.793 3
5 4 -8 4528.29 1057.08 6
-9 5 -9 444.687 433.703 4
-5 -4 9-398.933 508.330 3
-5 -4 10 559.958 468.699 3
9 -5 10 640.797 489.796 9
-5 9 -9 2345.38 655.801 2
-5 9 -8-1031.07 733.379 7
-9 4 8 457.535 535.912 3
-5 9 -8 717.316 554.174 2
-5 9 -7 631.743 555.682 7
-5 9 -7 320.105 429.542 2
-9 4 7 54.8794 448.222 3
-5 9 -6 4879.23 955.714 7
5 -9 6 5180.63 1016.93 1
-5 9 -6 5472.99 1057.08 2
-9 4 6 5180.60 986.309 3
-5 9 -5-702.773 655.391 7
5 -9 5 625.935 680.798 1
-5 9 -5 217.064 425.406 2
4 5 5 1202.21 624.807 7
-9 4 5 703.950 625.602 3
-9 4 5-744.777 634.684 2
9 -4 -5-228.163 553.520 8
-5 9 -4 478.472 499.127 7
-5 9 -4 254.217 400.304 2
5 -9 4-139.306 422.586 1
4 5 4 517.148 535.883 7
-9 4 4 1322.12 608.127 3
-4 -5 -4-239.606 685.406 1
-9 4 4 178.955 501.485 2
9 -4 -4 562.812 504.642 8
-5 9 -3 5046.89 952.407 7
-5 9 -3 5894.31 1097.29 2
4 5 3 5396.30 1119.67 7
5 -9 3 5994.71 1066.45 1
-9 4 3 4764.24 939.753 3
-4 -5 -3 4667.59 1084.63 1
-9 4 3 7951.13 1243.13 2
9 -4 -3 4764.42 974.257 8
-5 9 -2 1264.97 582.191 2
4 5 2 195.670 492.511 7
5 -9 2-175.627 386.555 1
-9 4 2-64.8727 415.085 3
-4 -5 -2 33.0387 459.466 1
-9 4 2 898.024 645.631 2
9 -4 -2 712.852 445.361 8
5 -9 1 195.807 497.689 8
-5 9 -1-278.691 424.630 2
4 5 1 980.329 578.747 7
-4 -5 -1 194.997 598.828 1
5 -9 1-208.600 490.781 1
-9 4 1 365.236 489.462 3
-9 4 1 314.917 495.528 2
9 -4 -1-482.852 539.192 8
5 -9 0 6905.41 1207.20 8
-4 -5 0 9667.06 1452.77 1
-5 9 0 6889.95 1162.83 2
4 5 0 7782.21 1284.09 7
5 -9 0 5917.02 990.523 1
-9 4 0 7124.25 1151.34 3
-4 -5 0 5332.35 1013.71 3
-9 4 0 5922.52 1042.70 2
9 -4 0 6717.03 1100.28 8
-4 -5 1 542.546 475.891 1
5 -9 -1 2251.19 871.030 8
-5 9 1 1657.20 730.348 2
4 5 -1 1420.95 712.421 7
5 -9 -1 1034.49 468.664 1
-9 4 -1 474.502 478.118 3
-4 -5 1 799.282 390.934 3
-9 4 -1 2312.21 724.074 2
9 -4 1 637.186 508.915 8
5 -9 -2-896.094 696.765 8
-5 9 2-543.174 522.934 2
4 5 -2-310.199 494.752 7
5 -9 -2 440.094 417.380 1
-9 4 -2-605.560 467.766 3
-4 -5 2 371.493 415.362 3
-9 4 -2 366.000 359.043 2
-4 -5 2-304.910 459.958 1
9 -4 2-116.816 411.854 8
5 -9 -3 6496.26 1199.79 8
-5 9 3 4379.32 986.508 2
4 5 -3 6314.00 1226.25 7
-4 -5 3 3766.20 797.752 3
5 -9 -3 5704.61 972.573 1
-9 4 -3 5993.01 1053.32 3
-4 -5 3 5078.59 1048.72 1
-9 4 -3 5623.21 999.046 2
9 -4 3 4889.21 872.356 8
5 -9 -4 467.924 587.337 8
-5 9 4-107.509 437.054 2
4 5 -4 892.366 613.416 7
-4 -5 4 1545.67 618.468 3
-9 4 -4-60.4666 520.334 3
4 5 -4 1060.07 540.932 6
-9 4 -4 681.273 449.246 2
-4 -5 4 1513.38 584.143 1
9 -4 4 1183.91 546.569 8
5 -9 -5-41.7000 565.731 8
4 5 -5-210.396 505.430 7
-4 -5 5 776.097 594.286 3
-4 -5 5-292.427 526.515 1
4 5 -5 404.523 465.033 6
-9 4 -5-267.822 533.989 3
9 -4 5-576.468 465.859 8
-9 4 -6 8882.24 1203.78 4
4 5 -6 9780.88 1522.31 7
-4 -5 6 9537.66 1394.38 1
-4 -5 6 8960.78 1243.21 3
4 5 -6 6923.35 1242.19 6
9 -4 6 8570.33 1129.55 8
-9 4 -7 1214.87 464.094 4
-4 -5 7 649.409 485.653 3
4 5 -7-48.3271 484.465 6
-9 4 -8 1.62103 385.880 4
-4 -5 8 638.656 488.640 1
4 5 -8 49.6287 485.835 6
9 -4 8 314.475 404.146 9
-4 -5 9 3771.35 913.769 1
-9 4 -9 4707.01 940.845 4
4 5 -9 3860.99 996.701 6
9 -4 9 4962.79 908.475 9
9 -4 10 215.602 387.736 9
-4 -5 10-417.226 546.208 1
-6 9 -9 498.506 469.159 7
-6 9 -8 4671.76 990.108 7
-6 9 -8 4960.61 944.491 2
-6 9 -7 95.7139 425.094 7
-6 9 -7 398.121 472.128 2
6 -9 6 3226.28 868.412 1
-6 9 -6 1871.98 614.158 7
-6 9 -6 2864.22 748.527 2
6 -9 5 5994.85 1166.83 8
6 -9 5 5926.65 1073.99 1
-6 9 -5 6010.53 1095.03 2
-9 3 5 5661.13 1089.27 3
6 -9 4-119.955 541.457 8
6 -9 4 954.103 548.633 1
-6 9 -4 727.114 437.301 2
-9 3 4-853.685 577.738 3
6 -9 3 24.7446 570.470 8
6 -9 3 561.341 428.445 1
-6 9 -3 1531.79 631.099 2
3 6 3 44.6390 470.182 7
-9 3 3 428.648 563.730 3
9 -3 -3 352.283 525.996 8
6 -9 2 2145.31 781.588 8
-3 -6 -2 4430.30 1112.67 1
6 -9 2 3655.33 790.595 1
-6 9 -2 2669.16 770.662 2
3 6 2 3419.57 907.079 7
-9 3 2 2104.77 663.938 3
9 -3 -2 3220.79 862.890 8
6 -9 1 299.094 466.332 8
-6 9 -1 746.279 526.335 2
6 -9 1 311.565 353.924 1
3 6 1 537.497 584.615 7
-9 3 1 951.668 562.308 3
9 -3 -1 366.492 381.874 8
-3 -6 -1-198.860 559.933 1
6 -9 0 1212.54 617.715 8
-6 9 0 1108.44 555.712 2
6 -9 0 1563.49 559.273 1
3 6 0 1433.69 651.098 7
-9 3 0 1687.54 628.894 3
-3 -6 0 2013.92 802.334 1
9 -3 0 1746.46 673.845 8
6 -9 -1 4668.39 1049.84 8
-6 9 1 5464.99 1019.49 2
6 -9 -1 4343.81 861.688 1
3 6 -1 5820.66 1145.26 7
-9 3 -1 4878.06 991.414 3
-3 -6 1 5501.47 1093.77 1
9 -3 1 7115.81 1126.73 8
6 -9 -2-155.541 497.740 8
-6 9 2 313.436 453.513 2
3 6 -2 1494.81 647.222 7
-9 3 -2 366.316 530.743 3
-3 -6 2 1547.31 689.970 1
9 -3 2 1378.14 608.249 8
-6 9 3 943.652 695.324 2
3 6 -3 36.3465 536.188 7
-9 3 -3 1060.20 597.547 3
-3 -6 3-309.606 513.130 1
9 -3 3 71.2609 391.808 8
-3 -6 4 4091.57 992.197 1
-9 3 -4 3960.11 950.122 3
9 -3 4 3860.66 826.542 8
-3 -6 5-27.4080 506.242 1
9 -3 5 59.1604 349.610 8
-3 -6 6 2583.92 791.669 1
9 -3 6 1598.30 558.830 8
-9 3 -6 3106.27 778.948 4
9 -3 7 5710.28 956.301 9
-9 3 -7 5408.67 1008.17 4
9 -3 8 582.125 375.058 9
-9 3 -8 1309.38 525.349 4
3 6 -9 212.031 474.536 6
9 -3 9-524.270 569.259 9
7 -9 8 117.196 437.036 8
7 -9 7 1838.18 681.983 8
-7 9 -7 3039.64 765.522 2
7 -9 6 782.184 622.203 8
-7 9 -6 711.831 533.986 2
7 -9 5 2549.00 871.104 8
7 -9 5 2091.32 707.037 1
-7 9 -5 2259.12 726.893 2
7 -9 4 6549.56 1183.96 8
7 -9 4 3892.08 849.283 1
-7 9 -4 4295.26 939.645 2
7 -9 3 839.271 573.133 8
7 -9 3 2817.92 776.723 1
-7 9 -3 2842.79 797.557 2
7 -9 2 2275.40 852.046 8
7 -9 2 2302.49 719.349 1
-7 9 -2 1757.22 652.592 2
7 -9 1 4512.13 856.040 1
9 -2 -1 3577.89 872.170 8
9 -2 0 881.297 494.313 8
9 -2 1 990.639 521.920 8
9 -2 2 2741.51 717.087 8
9 -2 3 906.151 608.104 8
9 -2 4 203.411 447.816 8
9 -2 5 1411.43 609.232 8
9 -2 6 234.835 367.084 9
9 -2 7 1237.93 541.740 9
-9 2 -7 2433.53 741.579 4
-10 5 2 5788.37 1082.24 3
-10 5 1 1444.50 624.272 3
5 -10 -2 1060.50 533.770 1
6 -10 0 1028.60 570.579 1
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 97937
_shelx_res_file
;
TITL ap90_hbr in P3(2)
CELL 0.71073 7.3942 7.3942 17.4657 90.000 90.000 120.000
ZERR 3 0.0002 0.0002 0.0004 0.00 0.00 0.00
LATT -1
SYMM -Y,X-Y, 0.66667+Z
SYMM -X+Y,-X, 0.33333+Z
SFAC C H N O BR
UNIT 33 45 6 3 3
omit 0 52
omit 0 1 -2
L.S. 4
FMAP 2
PLAN -5
bond $h
acta 50
conf
WGHT 0.011500
FVAR 3.28395
N1 3 0.685309 0.213049 0.193664 11.00000 0.01097 0.01603 =
0.01104 -0.00009 0.00217 0.00761
C2 1 0.557760 0.254574 0.148072 11.00000 0.01222 0.02115 =
0.01607 0.00323 0.00388 0.00883
O2 4 0.555946 0.421175 0.157621 11.00000 0.01534 0.01680 =
0.02508 0.00080 0.00091 0.01105
C3 1 0.429629 0.096961 0.093889 11.00000 0.01192 0.03058 =
0.01662 -0.00063 0.00055 0.00935
AFIX 43
H3 2 0.346778 0.120997 0.060058 11.00000 -1.20000
AFIX 0
C4 1 0.427979 -0.086315 0.091459 11.00000 0.01375 0.01980 =
0.01623 -0.00481 0.00394 0.00334
AFIX 43
H4 2 0.339920 -0.189647 0.057362 11.00000 -1.20000
AFIX 0
C5 1 0.556056 -0.121579 0.139219 11.00000 0.01801 0.01643 =
0.02532 -0.00308 0.00723 0.00808
AFIX 43
H5 2 0.555033 -0.247687 0.136407 11.00000 -1.20000
AFIX 0
C6 1 0.684364 0.027014 0.190601 11.00000 0.01536 0.01739 =
0.01624 0.00391 0.00370 0.01149
C7 1 0.831544 -0.003811 0.240591 11.00000 0.01836 0.02057 =
0.02276 0.01054 0.00835 0.01304
AFIX 13
H7 2 0.769339 -0.153371 0.251231 11.00000 -1.20000
AFIX 0
C8 1 0.869276 0.111002 0.316591 11.00000 0.02112 0.03422 =
0.01583 0.00716 0.00526 0.01940
AFIX 23
H8A 2 0.739286 0.058409 0.344616 11.00000 -1.20000
H8B 2 0.966717 0.091311 0.347724 11.00000 -1.20000
AFIX 0
C9 1 0.959358 0.342140 0.297774 11.00000 0.01756 0.02904 =
0.00847 -0.00546 -0.00407 0.01268
AFIX 13
H9 2 0.985945 0.418030 0.346262 11.00000 -1.20000
AFIX 0
C10 1 0.801083 0.373411 0.253249 11.00000 0.01440 0.01493 =
0.01900 -0.00685 -0.00271 0.00468
AFIX 23
H10A 2 0.701065 0.374019 0.289033 11.00000 -1.20000
H10B 2 0.872973 0.509457 0.228882 11.00000 -1.20000
AFIX 0
C11 1 1.168822 0.423918 0.256711 11.00000 0.02136 0.02663 =
0.01398 -0.00611 -0.00386 0.00915
AFIX 23
H11A 2 1.222983 0.569163 0.243016 11.00000 -1.20000
H11B 2 1.267850 0.416969 0.291276 11.00000 -1.20000
AFIX 0
N12 3 1.149252 0.302199 0.186564 11.00000 0.01244 0.02656 =
0.01511 0.00360 0.00398 0.01334
H12A 2 1.079072 0.329534 0.145802 11.00000 0.02426
H12B 2 1.262737 0.328625 0.169811 11.00000 0.01667
C13 1 1.040270 0.070818 0.198912 11.00000 0.02192 0.02333 =
0.01509 0.00042 0.00110 0.01801
AFIX 23
H13A 2 1.128443 0.035573 0.229101 11.00000 -1.20000
H13B 2 1.014917 0.000424 0.149913 11.00000 -1.20000
AFIX 0
BR1 5 1.053411 0.359788 0.014351 11.00000 0.02774 0.01807 =
0.01604 -0.00107 -0.00410 0.01132
HKLF 4
REM ap90_hbr in P3(2)
REM R1 = 0.0273 for 1987 Fo > 4sig(Fo) and 0.0334 for all 2153 data
REM 144 parameters refined using 1 restraints
END
WGHT 0.0106 0.0000
REM Highest difference peak 0.549, deepest hole -0.250, 1-sigma level 0.065
Q1 1 0.8920 0.2787 0.0097 11.00000 0.05 0.55
Q2 1 0.9781 0.4389 0.0201 11.00000 0.05 0.35
Q3 1 0.9838 0.1993 0.0199 11.00000 0.05 0.34
Q4 1 1.0191 0.2993 -0.0463 11.00000 0.05 0.29
Q5 1 1.0568 0.3732 0.0786 11.00000 0.05 0.29
;
_shelx_res_checksum 81869
_shelxl_version_number .2013
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
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
N N1 0.6853(6) 0.2130(6) 0.19366(19) 0.0123(9) Uani d 1
C C2 0.5578(8) 0.2546(8) 0.1481(3) 0.0163(11) Uani d 1
O O2 0.5559(5) 0.4212(5) 0.15762(17) 0.0177(8) Uani d 1
C C3 0.4296(8) 0.0970(9) 0.0939(3) 0.0203(12) Uani d 1
H H3 0.3468 0.1210 0.0601 0.024 Uiso calc 1
C C4 0.4280(8) -0.0863(9) 0.0915(3) 0.0188(13) Uani d 1
H H4 0.3399 -0.1896 0.0574 0.023 Uiso calc 1
C C5 0.5561(8) -0.1216(8) 0.1392(3) 0.0202(13) Uani d 1
H H5 0.5550 -0.2477 0.1364 0.024 Uiso calc 1
C C6 0.6844(8) 0.0270(7) 0.1906(3) 0.0149(11) Uani d 1
C C7 0.8315(7) -0.0038(9) 0.2406(3) 0.0191(12) Uani d 1
H H7 0.7693 -0.1534 0.2512 0.023 Uiso calc 1
C C8 0.8693(8) 0.1110(8) 0.3166(3) 0.0212(12) Uani d 1
H H8A 0.7393 0.0584 0.3446 0.025 Uiso calc 1
H H8B 0.9667 0.0913 0.3477 0.025 Uiso calc 1
C C9 0.9594(8) 0.3421(8) 0.2978(3) 0.0179(11) Uani d 1
H H9 0.9859 0.4180 0.3463 0.021 Uiso calc 1
C C10 0.8011(7) 0.3734(7) 0.2532(2) 0.0173(11) Uani d 1
H H10A 0.7011 0.3740 0.2890 0.021 Uiso calc 1
H H10B 0.8730 0.5095 0.2289 0.021 Uiso calc 1
C C11 1.1688(8) 0.4239(8) 0.2567(3) 0.0219(13) Uani d 1
H H11A 1.2230 0.5692 0.2430 0.026 Uiso calc 1
H H11B 1.2679 0.4170 0.2913 0.026 Uiso calc 1
N N12 1.1493(7) 0.3022(7) 0.1866(2) 0.0164(10) Uani d 1
H H12A 1.079(7) 0.330(6) 0.146(3) 0.024(14) Uiso d 1
H H12B 1.263(8) 0.329(8) 0.170(3) 0.017(14) Uiso d 1
C C13 1.0403(7) 0.0708(8) 0.1989(3) 0.0171(11) Uani d 1
H H13A 1.1284 0.0356 0.2291 0.021 Uiso calc 1
H H13B 1.0149 0.0004 0.1499 0.021 Uiso calc 1
Br Br1 1.05341(7) 0.35979(7) 0.01435(2) 0.02068(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
N1 0.011(2) 0.016(2) 0.011(2) 0.008(2) 0.0022(16) -0.0001(17)
C2 0.012(3) 0.021(3) 0.016(3) 0.009(2) 0.004(2) 0.003(2)
O2 0.0153(18) 0.0168(19) 0.0251(19) 0.0110(16) 0.0009(14) 0.0008(15)
C3 0.012(3) 0.031(3) 0.017(3) 0.009(3) 0.001(2) -0.001(2)
C4 0.014(3) 0.020(3) 0.016(3) 0.003(2) 0.004(2) -0.005(2)
C5 0.018(3) 0.016(3) 0.025(3) 0.008(3) 0.007(2) -0.003(2)
C6 0.015(3) 0.017(3) 0.016(3) 0.011(2) 0.004(2) 0.004(2)
C7 0.018(3) 0.021(3) 0.023(3) 0.013(3) 0.008(2) 0.011(2)
C8 0.021(3) 0.034(3) 0.016(3) 0.019(3) 0.005(2) 0.007(2)
C9 0.018(3) 0.029(3) 0.008(2) 0.013(3) -0.004(2) -0.005(2)
C10 0.014(3) 0.015(3) 0.019(3) 0.005(2) -0.003(2) -0.007(2)
C11 0.021(3) 0.027(3) 0.014(3) 0.009(3) -0.004(2) -0.006(2)
N12 0.012(2) 0.027(3) 0.015(2) 0.013(2) 0.004(2) 0.0036(19)
C13 0.022(3) 0.023(3) 0.015(2) 0.018(3) 0.001(2) 0.000(2)
Br1 0.0277(3) 0.0181(3) 0.0160(2) 0.0113(3) -0.0041(3) -0.0011(2)
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'
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'
Br Br -0.2901 2.4595 '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
C6 N1 C2 122.6(4)
C6 N1 C10 122.6(4)
C2 N1 C10 114.3(4)
O2 C2 N1 119.2(4)
O2 C2 C3 124.2(5)
N1 C2 C3 116.6(4)
C4 C3 C2 120.6(5)
C4 C3 H3 119.7
C2 C3 H3 119.7
C3 C4 C5 120.5(5)
C3 C4 H4 119.7
C5 C4 H4 119.7
C6 C5 C4 120.7(5)
C6 C5 H5 119.7
C4 C5 H5 119.7
C5 C6 N1 119.0(4)
C5 C6 C7 121.7(4)
N1 C6 C7 119.3(4)
C6 C7 C8 111.5(4)
C6 C7 C13 110.1(4)
C8 C7 C13 109.9(4)
C6 C7 H7 108.4
C8 C7 H7 108.4
C13 C7 H7 108.4
C9 C8 C7 107.0(4)
C9 C8 H8A 110.3
C7 C8 H8A 110.3
C9 C8 H8B 110.3
C7 C8 H8B 110.3
H8A C8 H8B 108.6
C10 C9 C8 110.1(4)
C10 C9 C11 113.9(4)
C8 C9 C11 109.4(4)
C10 C9 H9 107.8
C8 C9 H9 107.8
C11 C9 H9 107.8
N1 C10 C9 114.7(4)
N1 C10 H10A 108.6
C9 C10 H10A 108.6
N1 C10 H10B 108.6
C9 C10 H10B 108.6
H10A C10 H10B 107.6
N12 C11 C9 112.0(4)
N12 C11 H11A 109.2
C9 C11 H11A 109.2
N12 C11 H11B 109.2
C9 C11 H11B 109.2
H11A C11 H11B 107.9
C11 N12 C13 114.0(4)
C11 N12 H12A 113(3)
C13 N12 H12A 108(2)
C11 N12 H12B 112(4)
C13 N12 H12B 103(3)
H12A N12 H12B 106(4)
N12 C13 C7 110.4(4)
N12 C13 H13A 109.6
C7 C13 H13A 109.6
N12 C13 H13B 109.6
C7 C13 H13B 109.6
H13A C13 H13B 108.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C6 1.373(6)
N1 C2 1.381(6)
N1 C10 1.486(5)
C2 O2 1.250(5)
C2 C3 1.431(7)
C3 C4 1.350(7)
C3 H3 0.9300
C4 C5 1.381(7)
C4 H4 0.9300
C5 C6 1.368(7)
C5 H5 0.9300
C6 C7 1.499(6)
C7 C8 1.524(6)
C7 C13 1.538(6)
C7 H7 0.9800
C8 C9 1.528(7)
C8 H8A 0.9700
C8 H8B 0.9700
C9 C10 1.516(6)
C9 C11 1.530(7)
C9 H9 0.9800
C10 H10A 0.9700
C10 H10B 0.9700
C11 N12 1.484(6)
C11 H11A 0.9700
C11 H11B 0.9700
N12 C13 1.498(6)
N12 H12A 0.96(5)
N12 H12B 0.81(5)
C13 H13A 0.9700
C13 H13B 0.9700
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
C6 N1 C2 O2 175.0(4)
C10 N1 C2 O2 3.0(6)
C6 N1 C2 C3 -3.0(6)
C10 N1 C2 C3 -175.0(4)
O2 C2 C3 C4 -174.4(5)
N1 C2 C3 C4 3.5(7)
C2 C3 C4 C5 -2.5(7)
C3 C4 C5 C6 1.0(8)
C4 C5 C6 N1 -0.5(7)
C4 C5 C6 C7 -177.3(4)
C2 N1 C6 C5 1.6(7)
C10 N1 C6 C5 173.0(4)
C2 N1 C6 C7 178.5(4)
C10 N1 C6 C7 -10.2(6)
C5 C6 C7 C8 -150.1(4)
N1 C6 C7 C8 33.1(6)
C5 C6 C7 C13 87.5(6)
N1 C6 C7 C13 -89.2(5)
C6 C7 C8 C9 -58.9(5)
C13 C7 C8 C9 63.5(5)
C7 C8 C9 C10 63.4(5)
C7 C8 C9 C11 -62.4(5)
C6 N1 C10 C9 14.5(6)
C2 N1 C10 C9 -173.5(4)
C8 C9 C10 N1 -41.3(5)
C11 C9 C10 N1 81.9(5)
C10 C9 C11 N12 -67.0(6)
C8 C9 C11 N12 56.6(5)
C9 C11 N12 C13 -51.1(6)
C11 N12 C13 C7 51.0(6)
C6 C7 C13 N12 65.8(5)
C8 C7 C13 N12 -57.5(5)
_cod_database_fobs_code 2021280