#------------------------------------------------------------------------------
#$Date: 2026-08-29 16:29:29 +0100 (Sat, 29 Aug 2026) $
#$Revision: 306808 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/74/1577479.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_1577479
loop_
_publ_author_name
'Hamilton, Fiona'
'Harrison, William T. A.'
_publ_section_title
;
 Carnosinium bromide.
;
_journal_coeditor_code           TK4128
_journal_issue                   'Pt 7'
_journal_name_full               IUCrData
_journal_page_first              x260726
_journal_paper_doi               10.1107/S2414314626007261
_journal_volume                  11
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C9 H15 N4 O3 +, Br -'
_chemical_formula_moiety         'C9 H15 N4 O3 +, Br -'
_chemical_formula_sum            'C9 H15 Br N4 O3'
_chemical_formula_weight         307.16
_chemical_name_common            'Carnosinium bromide'
_chemical_name_systematic
'5-[(2<i>S</i>)-2-(3-Azaniumylpropanamido)-2-carboxylatoethyl]-1<i>H</i>-imidazol-3-ium bromide'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90.012(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.46611(13)
_cell_length_b                   28.6332(5)
_cell_length_c                   16.2890(4)
_cell_measurement_reflns_used    11802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4520
_cell_measurement_theta_min      2.4440
_cell_volume                     2549.43(10)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT </i>(Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18071
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.473
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.415
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2376 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.018(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         7858
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0529P)^2^+3.5341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                7654
_reflns_number_total             7858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk4128.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1577479
_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   0.579
_shelx_estimated_absorpt_t_max   0.882
_shelx_hkl_file
;
   0 -37   0 219.460 435.547   2
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   0 -37  -2 5231.88 677.430   2
   0 -37   2 5821.50 718.839   2
   0 -36   0 4244.15 612.625   2
   0 -36  -1 631.736 438.700   2
   0 -36   1 1141.37 546.862   2
   0 -36  -2 2078.77 533.029   2
   0 -36   2 1919.43 588.569   2
   0 -36   3 4475.09 661.612   2
   0 -36  -3 4766.02 629.839   2
   0 -36   4 3181.62 633.779   2
   0 -36   5 1365.21 542.857   2
   0 -35   0-77.5059 400.876   2
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   0 -35   1 3608.29 623.412   2
   0 -35  -2 16059.7 925.362   2
   0 -35   2 15263.6 965.730   2
   0 -35  -3 1317.65 442.035   2
   0 -35   3 1883.78 535.259   2
   0 -35   4 986.258 497.700   2
   0 -35  -4 857.215 434.701   2
   0 -35   5 5154.61 698.835   2
   0 -35   6 1277.14 516.287   2
   0 -35   7-111.617 490.493   2
   0 -34   0 5999.98 627.754   2
   0 -34   1 5399.35 645.645   2
   0 -34  -1 5015.94 608.659   2
   0 -34   2 704.654 437.896   2
   0 -34  -2 916.683 417.448   2
   0 -34   3 6541.02 700.212   2
   0 -34  -3 6535.79 660.755   2
   0 -34   4 36977.5 1393.01   2
   0 -34  -4 35029.7 1263.84   2
   0 -34   5 1659.86 520.878   2
   0 -34   6 4554.01 609.082   2
   0 -34   7 9749.78 869.353   2
   0 -34   8 20502.9 1158.94   2
   0 -33   0 1454.43 482.468   2
   0 -33  -1 4672.53 582.803   2
   0 -33   1 4329.37 589.773   2
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   0 -33   2 6408.74 658.254   2
   0 -33   3 680.562 454.199   2
   0 -33  -3 5.26621 361.595   2
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   0 -33   5 9238.06 801.628   2
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   0 -33   7 594.769 482.058   2
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   0 -32  -8 64.2495 346.284   1
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   1  12   1 3366.86 147.442   1
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   1  12   2 145669. 960.484   1
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   1  12   3 18966.6 414.624   1
   1  12   4 91055.6 1341.61   2
   1  12   4 90419.6 956.077   1
   1  12   5 10868.7 533.421   2
   1  12   5 9948.20 384.183   1
   1  12   6 161127. 1907.63   2
   1  12   6 163409. 1493.03   1
   1  12   6 166042. 1838.39   4
   1  12   7 10649.0 541.291   4
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   1  13  -4 53293.8 984.460   2
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   1  13  -3 23990.6 699.695   2
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   1  13  -1 8301.74 427.526   2
   1  13   0 18681.0 246.601   1
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   1  13   0 17529.6 572.639   2
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   1  13   1 24286.8 366.812   1
   1  13   1 25590.5 706.508   2
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   1  13   2 187035. 1114.06   1
   1  13   2 185432. 1845.96   2
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   1  13   3 9356.60 335.446   1
   1  13   3 8924.00 480.098   2
   1  13   4 47221.3 715.378   1
   1  13   4 46374.5 1009.12   6
   1  13   5 8145.06 362.741   1
   1  13   5 9147.87 496.519   2
   1  13   6 52629.4 868.453   1
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   2   9   4 51759.4 812.099   1
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   2  12   6 29581.3 700.485   1
   2  12   6 30748.6 855.475   4
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   2  24   8 41898.0 1367.29   4
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   2  26   8 20025.1 1005.02   4
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   2  26  10 21223.9 1075.14   4
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   2  27   8 4879.70 667.392   4
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   2  29   9 5841.03 742.480   4
   2  29  10 4640.10 667.048   4
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   4   5  -4 69857.0 1078.28   3
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   4   5  -1 18943.3 547.216   3
   4   5  -1 19884.4 660.342   1
   4   5   0 173272. 1431.03   3
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   4   5   4 62021.9 1014.15   4
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   4   6  -7 4502.12 340.780   1
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   4   6  -5 26820.8 743.513   3
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   4   6  -4 60890.1 990.449   3
   4   6  -4 60284.6 1015.73   1
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   4   6  -3 7427.41 415.606   1
   4   6  -2 3842.40 256.093   3
   4   6  -2 4054.59 312.460   1
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   4   6   0 2801.93 216.094   3
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   4   6   1 12835.1 403.557   3
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   4   6   2 5574.59 255.136   3
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   4   6   5 28946.2 814.903   4
   4   7 -16 2632.75 448.726   1
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   4   7 -10 21331.1 686.705   1
   4   7  -9 7155.54 535.920   3
   4   7  -9 6884.61 449.177   1
   4   7  -8 21107.5 724.244   3
   4   7  -8 22560.0 645.550   1
   4   7  -7 4543.43 352.974   1
   4   7  -7 5221.02 417.906   3
   4   7  -6 10731.2 443.109   1
   4   7  -6 10128.3 484.183   3
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   4   7  -4 88997.0 1196.31   3
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   4   7  -3 20286.2 592.751   3
   4   7  -3 21126.3 629.319   1
   4   7  -2 16410.0 464.298   3
   4   7  -2 17428.4 547.061   1
   4   7  -1 2912.95 243.431   3
   4   7  -1 3075.56 301.819   1
   4   7   0 111480. 1042.53   3
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   4   7   1 3695.64 220.662   3
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   4   7   2 16163.4 373.667   3
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   4   7   3 18278.1 411.357   3
   4   7   5 5595.01 427.005   4
   4   7   6 12696.4 539.458   4
   4   8 -15 6770.48 598.520   1
   4   8 -14 13603.1 674.130   1
   4   8 -13 5987.73 489.742   1
   4   8 -13 8151.24 655.114   3
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   7  -6   0 8377.97 788.629   1
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   7   0  -1 7054.87 695.826   1
   7   0   0 144.556 412.541   1
   7   0   1 2404.94 527.930   1
   7   0   2 171.763 419.643   1
   7   0   3 4478.85 630.776   1
   7   1  -3 1775.29 479.911   1
   7   1  -2 2473.85 493.178   1
   7   1  -1-132.466 403.733   1
   7   1   0 19329.0 998.588   1
   7   1   1 1050.66 445.961   1
   7   1   2 4807.59 620.083   1
   7   1   3 3884.17 639.166   1
   7   2  -3 776.337 447.629   1
   7   2  -2 9761.61 706.580   1
   7   2  -1 5363.60 613.920   1
   7   2   0 1405.63 471.935   1
   7   2   1 4023.91 577.197   1
   7   2   2 7853.78 733.772   1
   7   2   3 2889.23 566.001   1
   7   3  -3 5412.08 628.804   1
   7   3  -2 5937.17 588.471   1
   7   3  -1 3772.58 539.086   1
   7   3   0 1030.77 432.404   1
   7   3   1 4676.84 611.170   1
   7   3   2 5465.49 645.132   1
   7   3   3 4191.95 621.706   1
   7   4  -2 16254.2 886.513   1
   7   4  -1 1533.05 426.848   1
   7   4   0 11737.6 791.330   1
   7   4   1 1008.17 461.985   1
   7   4   2 13704.8 840.579   1
   7   5  -1 3062.57 517.457   1
   7   5   0 4992.00 560.348   1
   7   5   1 6381.05 672.747   1
   7   5   2 2070.82 470.331   1
   0   0   0    0.00    0.00   0
TITL 2016ncs0016w in P2(1)
REM P2(1) (#4 in standard setting)
CELL 0.71075   5.466114  28.633178  16.289050  90.0000  90.0123  90.0000
ZERR    8.00   0.000126   0.000551   0.000369   0.0000   0.0024   0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O Br
UNIT 72.00 112.00 32.00 24.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum              33913
_shelx_res_file
;
TITL 2016ncs0016wa_a.res in P2(1)
    fh010.res
    created by SHELXL-2019/3 at 14:55:17 on 18-Nov-2025
CELL 0.71073 5.46611 28.6332 16.2890 90 90.012 90
ZERR 8       0.00013  0.0005  0.0004  0.0  0.002 0.0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O Br
UNIT 72 120 32 24 8
RIGU
size 0.19 0.05 0.04
rem colourless block
temp -173
L.S. 5
isor 0.001 c6b c6c
PLAN  20
BOND $H
CONF
acta
htab
EQIV $1 -x+2, y-1/2, -z+1
EQIV $2 x-2, y, z
EQIV $3 x-1, y, z
HTAB N1A Br4_$3
EQIV $4 x-1, y, z-1
HTAB N2A Br2_$4
HTAB N3A O1A_$3
HTAB N4A O1B_$2
HTAB N4A O1C_$3
HTAB N4A O3A
HTAB N4A O2B_$3
HTAB C2A Br1_$1
HTAB C4A Br4_$2
HTAB C9A O3A_$3
EQIV $5 x+1, y, z
EQIV $6 x+1, y, z+1
HTAB N1B Br2
HTAB N2B Br4
HTAB N3B O1B_$3
EQIV $7 x, y, z+1
HTAB N4B O1A_$7
HTAB N4B O2A_$7
HTAB N4B O3B_$3
HTAB N4B O2D_$3
HTAB C2B O3A_$5
HTAB C3B Br3_$1
HTAB C4B Br2_$3
HTAB C5B Br2
HTAB C8B O3B_$3
HTAB C9B O2A_$6
EQIV $8 -x+2, y+1/2, -z+1
EQIV $9 x-2, y, z-1
HTAB N1C Br1_$4
HTAB N2C Br3
HTAB N3C O2C_$3
HTAB N4C O1D_$9
HTAB N4C O2D_$9
HTAB N4C O3C_$3
HTAB N4C O2A
HTAB C2C O3D_$3
HTAB C3C Br2_$8
HTAB C4C Br1_$9
HTAB C9C O2D_$4
EQIV $10 -x+3, y+1/2, -z+1
HTAB N1D Br3_$5
HTAB N2D Br1
HTAB N3D O1D_$3
HTAB N4D O2C
HTAB N4D O2B
HTAB N4D O1C_$5
HTAB N4D O3D
HTAB C3D Br4_$10
HTAB C4D Br3
HTAB C9D O3D_$3
mpla c6a o1a o2a
mpla c1a c2a c3a n1a n2a
mpla c5a c7a c8a n3a o3a
mpla c6b o1b o2b
mpla c1b c2b c3b n1b n2b
mpla c5b c7b c8b n3b o3b
mpla c6c o1c o2c
mpla c1c c2c c3c n1c n2c
mpla c5c c7c c8c n3c o3c
mpla c6d o1d o2d
mpla c1d c2d c3d n1d n2d
mpla c5d c7d c8d n3d o3d
fmap 2
htab
TWIN -1 0 0 0 -1 0 0 0 1 2
rem EXTI    0.000000
WGHT    0.052900    3.534100
BASF   0.21080
FVAR       3.53265
mole 1
C1A   1   -0.384630    0.328115   -0.069936    11.00000    0.01599    0.00901 =
         0.01219   -0.00122   -0.00162   -0.00346
C2A   1   -0.059612    0.287159   -0.105935    11.00000    0.01564    0.01562 =
         0.02082   -0.00710   -0.00071   -0.00360
AFIX  43
H2A   2    0.082943    0.268239   -0.103299    11.00000   -1.20000
AFIX   0
C3A   1   -0.364186    0.328900   -0.153270    11.00000    0.02312    0.01125 =
         0.01287   -0.00128   -0.00081   -0.00121
AFIX  43
H3A   2   -0.470595    0.344238   -0.190686    11.00000   -1.20000
AFIX   0
C4A   1   -0.571627    0.349001   -0.014190    11.00000    0.01577    0.01166 =
         0.01742   -0.00255    0.00642   -0.00347
AFIX  23
H4A1  2   -0.636412    0.324211    0.022169    11.00000   -1.20000
H4A2  2   -0.709365    0.360817   -0.047756    11.00000   -1.20000
AFIX   0
C5A   1   -0.473441    0.389239    0.039376    11.00000    0.02024    0.01004 =
         0.01071   -0.00140    0.00016    0.00133
AFIX  13
H5A   2   -0.353554    0.377286    0.080723    11.00000   -1.20000
AFIX   0
C6A   1   -0.351276    0.425012   -0.018210    11.00000    0.01858    0.00980 =
         0.00649   -0.00307   -0.00449   -0.00169
C7A   1   -0.696484    0.419821    0.159988    11.00000    0.02258    0.01242 =
         0.00875    0.00003   -0.00220   -0.00011
C8A   1   -0.930457    0.444613    0.187012    11.00000    0.01976    0.02696 =
         0.00781   -0.00008   -0.00134    0.00653
AFIX  23
H8A1  2   -0.907562    0.478773    0.181602    11.00000   -1.20000
H8A2  2   -1.066138    0.435311    0.150213    11.00000   -1.20000
AFIX   0
C9A   1   -0.999948    0.433165    0.275552    11.00000    0.02161    0.02389 =
         0.01082   -0.00541    0.00212   -0.00508
AFIX  23
H9A1  2   -1.167253    0.444823    0.286585    11.00000   -1.20000
H9A2  2   -1.000967    0.398846    0.282924    11.00000   -1.20000
AFIX   0
N1A   3   -0.189698    0.301605   -0.041749    11.00000    0.01715    0.01253 =
         0.01191   -0.00246   -0.00248   -0.00217
AFIX  43
H1A   2   -0.157361    0.295366    0.010027    11.00000   -1.20000
AFIX   0
N2A   3   -0.158928    0.303095   -0.172856    11.00000    0.02348    0.01801 =
         0.01645   -0.00244    0.00584   -0.00281
AFIX  43
H2A1  2   -0.103855    0.298192   -0.222880    11.00000   -1.20000
AFIX   0
N3A   3   -0.683888    0.410608    0.080072    11.00000    0.01962    0.01467 =
         0.00863   -0.00044   -0.00187    0.00330
AFIX  43
H3A1  2   -0.811156    0.417885    0.049550    11.00000   -1.20000
AFIX   0
N4A   3   -0.829840    0.454059    0.334647    11.00000    0.01348    0.01339 =
         0.01854    0.00195    0.00097   -0.00020
AFIX 137
H4A3  2   -0.871740    0.445109    0.386372    11.00000   -1.50000
H4A4  2   -0.837230    0.485733    0.330795    11.00000   -1.50000
H4A5  2   -0.674946    0.444306    0.323460    11.00000   -1.50000
AFIX   0
O1A   4   -0.121539    0.425848   -0.018981    11.00000    0.01924    0.02422 =
         0.01128    0.00164    0.00039   -0.00369
O2A   4   -0.487928    0.448425   -0.063151    11.00000    0.02106    0.01415 =
         0.01011    0.00243   -0.00456   -0.00010
O3A   4   -0.530607    0.411369    0.209406    11.00000    0.01906    0.03048 =
         0.01450   -0.00822   -0.00600    0.00467
mole 2
C1B   1    0.660236    0.329628    0.427661    11.00000    0.01691    0.00887 =
         0.01416   -0.00224   -0.00099    0.00100
C2B   1    0.672413    0.328481    0.344821    11.00000    0.02776    0.01018 =
         0.01700    0.00264    0.00426   -0.00060
AFIX  43
H2B   2    0.562893    0.343211    0.307660    11.00000   -1.20000
AFIX   0
C3B   1    0.982517    0.286549    0.392249    11.00000    0.02242    0.01603 =
         0.02068   -0.00579    0.00621    0.00212
AFIX  43
H3B   2    1.123696    0.267263    0.395021    11.00000   -1.20000
AFIX   0
C4B   1    0.484081    0.352955    0.484265    11.00000    0.01411    0.01213 =
         0.01465   -0.00305    0.00087   -0.00070
AFIX  23
H4B1  2    0.412884    0.329230    0.521459    11.00000   -1.20000
H4B2  2    0.348939    0.366524    0.451570    11.00000   -1.20000
AFIX   0
C5B   1    0.603058    0.392034    0.536456    11.00000    0.01594    0.01378 =
         0.00739   -0.00093   -0.00218    0.00360
AFIX  13
H5B   2    0.720376    0.377801    0.576377    11.00000   -1.20000
AFIX   0
C6B   1    0.741596    0.426549    0.480225    11.00000    0.01334    0.00998 =
         0.00920   -0.00072   -0.00057   -0.00002
C7B   1    0.425974    0.425588    0.660548    11.00000    0.01115    0.01140 =
         0.01703   -0.00538   -0.00272   -0.00044
C8B   1    0.199278    0.448603    0.696173    11.00000    0.02371    0.01932 =
         0.00796    0.00152    0.00379    0.00375
AFIX  23
H8B1  2    0.226562    0.482655    0.701378    11.00000   -1.20000
H8B2  2    0.058520    0.443594    0.658944    11.00000   -1.20000
AFIX   0
C9B   1    0.143254    0.427945    0.779931    11.00000    0.01669    0.01901 =
         0.01255    0.00280   -0.00066    0.00202
AFIX  23
H9B1  2    0.101691    0.394475    0.773782    11.00000   -1.20000
H9B2  2    0.290168    0.430251    0.815254    11.00000   -1.20000
AFIX   0
N1B   3    0.854919    0.303482    0.455820    11.00000    0.02269    0.01188 =
         0.01120   -0.00291   -0.00200    0.00179
AFIX  43
H1B   2    0.890076    0.298643    0.507852    11.00000   -1.20000
AFIX   0
N2B   3    0.873246    0.301972    0.324457    11.00000    0.01990    0.01898 =
         0.01853   -0.00843    0.00296   -0.00394
AFIX  43
H2B1  2    0.922244    0.296079    0.274052    11.00000   -1.20000
AFIX   0
N3B   3    0.406414    0.414947    0.581200    11.00000    0.01295    0.01653 =
         0.01001   -0.00323   -0.00399    0.00327
AFIX  43
H3B1  2    0.270436    0.421988    0.555051    11.00000   -1.20000
AFIX   0
N4B   3   -0.061018    0.452438    0.819184    11.00000    0.02051    0.01418 =
         0.01563   -0.00244    0.00498   -0.00712
AFIX 137
H4B3  2   -0.084777    0.440727    0.870501    11.00000   -1.50000
H4B4  2   -0.199126    0.448348    0.788818    11.00000   -1.50000
H4B5  2   -0.025994    0.483447    0.822605    11.00000   -1.50000
AFIX   0
O1B   4    0.966588    0.427839    0.483466    11.00000    0.02030    0.02622 =
         0.01100    0.00472   -0.00230   -0.00086
O2B   4    0.607362    0.450595    0.432638    11.00000    0.02015    0.01449 =
         0.01494    0.00207   -0.00350    0.00091
O3B   4    0.609548    0.418179    0.702332    11.00000    0.01815    0.03903 =
         0.01552   -0.01020   -0.00829    0.00472
mole 3
C1C   1    0.146349    0.669140    0.319472    11.00000    0.01883    0.00525 =
         0.01432   -0.00176    0.00087    0.00150
C2C   1    0.156525    0.670602    0.401777    11.00000    0.01663    0.01267 =
         0.01311   -0.00230   -0.00186    0.00058
AFIX  43
H2C   2    0.047334    0.655617    0.438715    11.00000   -1.20000
AFIX   0
C3C   1    0.462214    0.713774    0.354496    11.00000    0.02653    0.01497 =
         0.02247   -0.00222    0.00165   -0.00217
AFIX  43
H3C   2    0.600378    0.733847    0.351904    11.00000   -1.20000
AFIX   0
C4C   1   -0.024879    0.645333    0.263428    11.00000    0.02276    0.01482 =
         0.00836   -0.00005   -0.00448    0.00154
AFIX  23
H4C1  2   -0.098117    0.668765    0.226096    11.00000   -1.20000
H4C2  2   -0.158958    0.631385    0.296104    11.00000   -1.20000
AFIX   0
C5C   1    0.096115    0.606787    0.211683    11.00000    0.01549    0.01360 =
         0.00785   -0.00200   -0.00339   -0.00639
AFIX  13
H5C   2    0.213853    0.621079    0.171984    11.00000   -1.20000
AFIX   0
C6C   1    0.232349    0.572120    0.268090    11.00000    0.01487    0.01136 =
         0.01046   -0.00080   -0.00005    0.00014
C7C   1   -0.078050    0.570985    0.087962    11.00000    0.02078    0.01301 =
         0.01537   -0.00143   -0.00255   -0.00287
C8C   1   -0.297325    0.547342    0.052069    11.00000    0.01090    0.01750 =
         0.02114    0.00002   -0.00690   -0.00303
AFIX  23
H8C1  2   -0.439478    0.551611    0.088965    11.00000   -1.20000
H8C2  2   -0.265369    0.513438    0.046878    11.00000   -1.20000
AFIX   0
C9C   1   -0.354702    0.567546   -0.031263    11.00000    0.01324    0.01365 =
         0.02287    0.00171   -0.00485   -0.00132
AFIX  23
H9C1  2   -0.395614    0.601055   -0.025275    11.00000   -1.20000
H9C2  2   -0.208148    0.565132   -0.066711    11.00000   -1.20000
AFIX   0
N1C   3    0.341454    0.696530    0.290628    11.00000    0.01930    0.00896 =
         0.01816    0.00183    0.00007   -0.00061
AFIX  43
H1C   2    0.377680    0.701450    0.238707    11.00000   -1.20000
AFIX   0
N2C   3    0.356416    0.698101    0.422951    11.00000    0.02466    0.01744 =
         0.01488   -0.00698   -0.00584   -0.00209
AFIX  43
H2C1  2    0.405214    0.704179    0.473316    11.00000   -1.20000
AFIX   0
N3C   3   -0.098747    0.583440    0.167149    11.00000    0.01904    0.01401 =
         0.00871    0.00084   -0.00015   -0.00415
AFIX  43
H3C1  2   -0.236078    0.577190    0.193104    11.00000   -1.20000
AFIX   0
N4C   3   -0.559475    0.543295   -0.070624    11.00000    0.01718    0.01525 =
         0.01655   -0.00087   -0.00176    0.00137
AFIX 137
H4C3  2   -0.574463    0.553281   -0.123423    11.00000   -1.50000
H4C4  2   -0.699998    0.549560   -0.042776    11.00000   -1.50000
H4C5  2   -0.531174    0.511977   -0.070125    11.00000   -1.50000
AFIX   0
O1C   4    0.103112    0.548346    0.314838    11.00000    0.02022    0.01191 =
         0.01702    0.00038    0.00018   -0.00084
O2C   4    0.460294    0.571668    0.264513    11.00000    0.02025    0.02635 =
         0.01300    0.00444   -0.00357   -0.00105
O3C   4    0.109654    0.577377    0.046854    11.00000    0.02114    0.03516 =
         0.02365   -0.01020    0.00465   -0.00757
mole 4
C1D   1    1.119606    0.666722    0.820247    11.00000    0.01545    0.00840 =
         0.01470   -0.00052   -0.00427    0.00297
C2D   1    1.137954    0.665620    0.903069    11.00000    0.01772    0.01426 =
         0.01375   -0.00060   -0.00312    0.00120
AFIX  43
H2D   2    1.029951    0.650016    0.939607    11.00000   -1.20000
AFIX   0
C3D   1    1.445597    0.707117    0.857491    11.00000    0.01955    0.01465 =
         0.02153   -0.00499   -0.00191    0.00518
AFIX  43
H3D   2    1.589908    0.725561    0.855240    11.00000   -1.20000
AFIX   0
C4D   1    0.932127    0.647276    0.764297    11.00000    0.01997    0.01122 =
         0.01062   -0.00133   -0.00854    0.00282
AFIX  23
H4D1  2    0.871802    0.672581    0.728162    11.00000   -1.20000
H4D2  2    0.792050    0.636108    0.797437    11.00000   -1.20000
AFIX   0
C5D   1    1.025533    0.606289    0.709738    11.00000    0.02132    0.01046 =
         0.00945    0.00063   -0.00368   -0.00146
AFIX  13
H5D   2    1.145552    0.618184    0.668399    11.00000   -1.20000
AFIX   0
C6D   1    1.149213    0.570762    0.766400    11.00000    0.01795    0.01211 =
         0.00551   -0.00407   -0.00186    0.00277
C7D   1    0.799397    0.577982    0.587846    11.00000    0.01700    0.01899 =
         0.00980    0.00141    0.00013   -0.00274
C8D   1    0.564587    0.554646    0.560649    11.00000    0.01553    0.02601 =
         0.01840   -0.00527   -0.00291   -0.00589
AFIX  23
H8D1  2    0.430611    0.564434    0.597742    11.00000   -1.20000
H8D2  2    0.583439    0.520389    0.565927    11.00000   -1.20000
AFIX   0
C9D   1    0.492941    0.566243    0.472306    11.00000    0.01750    0.02150 =
         0.02156    0.00052   -0.00131    0.00746
AFIX  23
H9D1  2    0.326172    0.554301    0.461277    11.00000   -1.20000
H9D2  2    0.490527    0.600568    0.465047    11.00000   -1.20000
AFIX   0
N1D   3    1.314008    0.692931    0.793230    11.00000    0.01719    0.01384 =
         0.01530   -0.00070   -0.00013   -0.00061
AFIX  43
H1D   2    1.346639    0.699361    0.741551    11.00000   -1.20000
AFIX   0
N2D   3    1.340473    0.691074    0.924811    11.00000    0.02132    0.01722 =
         0.01624   -0.00398   -0.00850    0.00430
AFIX  43
H2D1  2    1.391867    0.695914    0.975300    11.00000   -1.20000
AFIX   0
N3D   3    0.815923    0.585969    0.668440    11.00000    0.01178    0.01721 =
         0.01009    0.00148   -0.00301   -0.00544
AFIX  43
H3D1  2    0.689357    0.578279    0.698960    11.00000   -1.20000
AFIX   0
N4D   3    0.666319    0.545358    0.412975    11.00000    0.00962    0.01402 =
         0.01711    0.00074   -0.00232    0.00100
AFIX 137
H4D3  2    0.621520    0.553349    0.361033    11.00000   -1.50000
H4D4  2    0.664180    0.513717    0.418170    11.00000   -1.50000
H4D5  2    0.819867    0.556165    0.423240    11.00000   -1.50000
AFIX   0
O1D   4    1.378219    0.569761    0.767769    11.00000    0.02169    0.02151 =
         0.01151    0.00298   -0.00519    0.00554
O2D   4    1.009758    0.547202    0.811280    11.00000    0.02956    0.01039 =
         0.01495    0.00032    0.00364   -0.00378
O3D   4    0.963419    0.587481    0.538079    11.00000    0.01071    0.03247 =
         0.01773   -0.00668    0.00128   -0.00577
mole 5
BR1   5    1.563787    0.701705    1.105727    11.00000    0.02183    0.02245 =
         0.01361    0.00415   -0.00456   -0.00421
mole 6
BR2   5    1.055353    0.298473    0.644193    11.00000    0.02296    0.02311 =
         0.01352    0.00390    0.00437    0.00704
mole 7
BR3   5    0.524139    0.703969    0.608639    11.00000    0.02482    0.02391 =
         0.01336    0.00374   -0.00294   -0.00326
mole 8
BR4   5    1.045194    0.290196    0.139943    11.00000    0.02308    0.02441 =
         0.01481    0.00428    0.00424    0.00115
HKLF 4
REM  2016ncs0016wa_a.res in P2(1)
REM wR2 = 0.0920, GooF = S = 1.056, Restrained GooF = 1.029 for all data
REM R1 = 0.0352 for 7654 Fo > 4sig(Fo) and 0.0364 for all 7858 data
REM 618 parameters refined using 445 restraints
END
WGHT      0.0527      3.6959
REM Instructions for potential hydrogen bonds
HTAB C2A Br1_$1
HTAB C4A Br4_$2
HTAB C9A O3A_$3
HTAB N1A Br4_$3
HTAB N2A Br2_$4
HTAB N3A O1A_$3
HTAB N4A O1B_$2
HTAB N4A O1C_$3
HTAB N4A O3A
HTAB N4A O2B_$3
HTAB C2B O3A_$5
HTAB C3B Br3_$1
HTAB C4B Br2_$3
HTAB C5B Br2
HTAB C8B O3B_$3
HTAB C9B O2A_$6
HTAB N1B Br2
HTAB N2B Br4
HTAB N3B O1B_$3
HTAB N4B O1A_$7
HTAB N4B O2A_$7
HTAB N4B O3B_$3
HTAB N4B O2D_$3
HTAB C2C O3D_$3
HTAB C3C Br2_$8
HTAB C4C Br1_$9
HTAB C9C O2D_$4
HTAB N1C Br1_$4
HTAB N2C Br3
HTAB N3C O2C_$3
HTAB N4C O1D_$9
HTAB N4C O2D_$9
HTAB N4C O3C_$3
HTAB N4C O2A
HTAB C3D Br4_$10
HTAB C4D Br3
HTAB C9D O3D_$3
HTAB N1D Br3_$5
HTAB N2D Br1
HTAB N3D O1D_$3
HTAB N4D O2C
HTAB N4D O2B
HTAB N4D O1C_$5
HTAB N4D O3D
REM Highest difference peak  0.847,  deepest hole -0.415,  1-sigma level  0.096
Q1    1  -0.0456  0.5897  0.0388  11.00000  0.05    0.85
Q2    1   0.6069  0.6838  0.6020  11.00000  0.05    0.81
Q3    1   0.4557  0.4098  0.7131  11.00000  0.05    0.71
Q4    1   1.1247  0.3109  0.1500  11.00000  0.05    0.71
Q5    1   0.4269  0.5425  0.4269  11.00000  0.05    0.68
Q6    1   1.1335  0.5803  0.5443  11.00000  0.05    0.67
Q7    1  -0.4475  0.5506  0.0605  11.00000  0.05    0.66
Q8    1  -1.0513  0.4541  0.3252  11.00000  0.05    0.65
Q9    1   0.1689  0.4526  0.8404  11.00000  0.05    0.64
Q10   1   1.0355  0.2723  0.6389  11.00000  0.05    0.61
Q11   1  -0.3757  0.4147  0.2012  11.00000  0.05    0.61
Q12   1  -0.3333  0.5438 -0.0863  11.00000  0.05    0.60
Q13   1  -0.0304  0.4304  0.7783  11.00000  0.05    0.59
Q14   1   0.5943  0.7176  0.6017  11.00000  0.05    0.59
Q15   1   0.0280  0.4486  0.6843  11.00000  0.05    0.55
Q16   1   1.4980  0.6880  1.1086  11.00000  0.05    0.52
Q17   1   0.4611  0.4534  0.4362  11.00000  0.05    0.52
Q18   1   0.2754  0.4211  0.6585  11.00000  0.05    0.48
Q19   1   0.3196  0.5718  0.2628  11.00000  0.05    0.46
Q20   1  -0.0300  0.5442  0.3111  11.00000  0.05    0.46
;
_shelx_res_checksum              17538
loop_
_space_group_symop_operation_xyz
'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
C C1A -0.3846(13) 0.3281(2) -0.0699(4) 0.0124(13) Uani d 1 . .
C C2A -0.0596(13) 0.2872(3) -0.1059(5) 0.0174(15) Uani d 1 . .
H H2A 0.082943 0.268239 -0.103299 0.021 Uiso calc 1 . .
C C3A -0.3642(14) 0.3289(2) -0.1533(5) 0.0157(15) Uani d 1 . .
H H3A -0.470595 0.344238 -0.190686 0.019 Uiso calc 1 . .
C C4A -0.5716(13) 0.3490(2) -0.0142(5) 0.0149(15) Uani d 1 . .
H H4A1 -0.636412 0.324211 0.022169 0.018 Uiso calc 1 . .
H H4A2 -0.709365 0.360817 -0.047756 0.018 Uiso calc 1 . .
C C5A -0.4734(13) 0.3892(2) 0.0394(4) 0.0137(14) Uani d 1 . .
H H5A -0.353554 0.377286 0.080723 0.016 Uiso calc 1 . .
C C6A -0.3513(13) 0.4250(2) -0.0182(4) 0.0116(12) Uani d 1 . .
C C7A -0.6965(13) 0.4198(2) 0.1600(4) 0.0146(13) Uani d 1 . .
C C8A -0.9305(14) 0.4446(3) 0.1870(4) 0.0182(14) Uani d 1 . .
H H8A1 -0.907562 0.478773 0.181602 0.022 Uiso calc 1 . .
H H8A2 -1.066138 0.435311 0.150213 0.022 Uiso calc 1 . .
C C9A -0.9999(14) 0.4332(2) 0.2756(4) 0.0188(15) Uani d 1 . .
H H9A1 -1.167253 0.444823 0.286585 0.023 Uiso calc 1 . .
H H9A2 -1.000967 0.398846 0.282924 0.023 Uiso calc 1 . .
N N1A -0.1897(11) 0.3016(2) -0.0417(4) 0.0139(12) Uani d 1 . .
H H1A -0.157361 0.295366 0.010027 0.017 Uiso calc 1 . .
N N2A -0.1589(12) 0.3031(2) -0.1729(4) 0.0193(14) Uani d 1 . .
H H2A1 -0.103855 0.298192 -0.222880 0.023 Uiso calc 1 . .
N N3A -0.6839(11) 0.41061(19) 0.0801(4) 0.0143(12) Uani d 1 . .
H H3A1 -0.811156 0.417885 0.049550 0.017 Uiso calc 1 . .
N N4A -0.8298(10) 0.45406(18) 0.3346(3) 0.0151(12) Uani d 1 . .
H H4A3 -0.871740 0.445109 0.386372 0.023 Uiso calc 1 . .
H H4A4 -0.837230 0.485733 0.330795 0.023 Uiso calc 1 . .
H H4A5 -0.674946 0.444306 0.323460 0.023 Uiso calc 1 . .
O O1A -0.1215(10) 0.42585(18) -0.0190(3) 0.0182(11) Uani d 1 . .
O O2A -0.4879(9) 0.44842(16) -0.0632(3) 0.0151(10) Uani d 1 . .
O O3A -0.5306(10) 0.41137(18) 0.2094(3) 0.0213(11) Uani d 1 . .
C C1B 0.6602(13) 0.3296(2) 0.4277(4) 0.0133(14) Uani d 1 . .
C C2B 0.6724(15) 0.3285(2) 0.3448(5) 0.0183(15) Uani d 1 . .
H H2B 0.562893 0.343211 0.307660 0.022 Uiso calc 1 . .
C C3B 0.9825(14) 0.2865(3) 0.3922(5) 0.0197(16) Uani d 1 . .
H H3B 1.123696 0.267263 0.395021 0.024 Uiso calc 1 . .
C C4B 0.4841(13) 0.3530(2) 0.4843(4) 0.0136(14) Uani d 1 . .
H H4B1 0.412884 0.329230 0.521459 0.016 Uiso calc 1 . .
H H4B2 0.348939 0.366524 0.451570 0.016 Uiso calc 1 . .
C C5B 0.6031(13) 0.3920(2) 0.5365(4) 0.0124(13) Uani d 1 . .
H H5B 0.720376 0.377801 0.576377 0.015 Uiso calc 1 . .
C C6B 0.7416(12) 0.4265(2) 0.4802(4) 0.0108(12) Uani d 1 . .
C C7B 0.4260(12) 0.4256(2) 0.6605(4) 0.0132(12) Uani d 1 . .
C C8B 0.1993(14) 0.4486(2) 0.6962(4) 0.0170(15) Uani d 1 . .
H H8B1 0.226562 0.482655 0.701378 0.020 Uiso calc 1 . .
H H8B2 0.058520 0.443594 0.658944 0.020 Uiso calc 1 . .
C C9B 0.1433(13) 0.4279(2) 0.7799(4) 0.0161(14) Uani d 1 . .
H H9B1 0.101691 0.394475 0.773782 0.019 Uiso calc 1 . .
H H9B2 0.290168 0.430251 0.815254 0.019 Uiso calc 1 . .
N N1B 0.8549(11) 0.3035(2) 0.4558(4) 0.0153(12) Uani d 1 . .
H H1B 0.890076 0.298643 0.507852 0.018 Uiso calc 1 . .
N N2B 0.8732(12) 0.3020(2) 0.3245(4) 0.0191(13) Uani d 1 . .
H H2B1 0.922244 0.296079 0.274052 0.023 Uiso calc 1 . .
N N3B 0.4064(11) 0.41495(19) 0.5812(4) 0.0132(11) Uani d 1 . .
H H3B1 0.270436 0.421988 0.555051 0.016 Uiso calc 1 . .
N N4B -0.0610(11) 0.45244(19) 0.8192(4) 0.0168(13) Uani d 1 . .
H H4B3 -0.084777 0.440727 0.870501 0.025 Uiso calc 1 . .
H H4B4 -0.199126 0.448348 0.788818 0.025 Uiso calc 1 . .
H H4B5 -0.025994 0.483447 0.822605 0.025 Uiso calc 1 . .
O O1B 0.9666(9) 0.42784(18) 0.4835(3) 0.0192(11) Uani d 1 . .
O O2B 0.6074(9) 0.45059(16) 0.4326(3) 0.0165(10) Uani d 1 . .
O O3B 0.6095(10) 0.41818(19) 0.7023(3) 0.0242(12) Uani d 1 . .
C C1C 0.1463(13) 0.6691(2) 0.3195(4) 0.0128(13) Uani d 1 . .
C C2C 0.1565(13) 0.6706(2) 0.4018(5) 0.0141(14) Uani d 1 . .
H H2C 0.047334 0.655617 0.438715 0.017 Uiso calc 1 . .
C C3C 0.4622(15) 0.7138(2) 0.3545(5) 0.0213(17) Uani d 1 . .
H H3C 0.600378 0.733847 0.351904 0.026 Uiso calc 1 . .
C C4C -0.0249(14) 0.6453(2) 0.2634(4) 0.0153(14) Uani d 1 . .
H H4C1 -0.098117 0.668765 0.226096 0.018 Uiso calc 1 . .
H H4C2 -0.158958 0.631385 0.296104 0.018 Uiso calc 1 . .
C C5C 0.0961(13) 0.6068(2) 0.2117(4) 0.0123(13) Uani d 1 . .
H H5C 0.213853 0.621079 0.171984 0.015 Uiso calc 1 . .
C C6C 0.2323(12) 0.5721(2) 0.2681(4) 0.0122(12) Uani d 1 . .
C C7C -0.0780(14) 0.5710(2) 0.0880(4) 0.0164(13) Uani d 1 . .
C C8C -0.2973(12) 0.5473(2) 0.0521(4) 0.0165(14) Uani d 1 . .
H H8C1 -0.439478 0.551611 0.088965 0.020 Uiso calc 1 . .
H H8C2 -0.265369 0.513438 0.046878 0.020 Uiso calc 1 . .
C C9C -0.3547(13) 0.5675(2) -0.0313(4) 0.0166(14) Uani d 1 . .
H H9C1 -0.395614 0.601055 -0.025275 0.020 Uiso calc 1 . .
H H9C2 -0.208148 0.565132 -0.066711 0.020 Uiso calc 1 . .
N N1C 0.3415(11) 0.69653(19) 0.2906(4) 0.0155(12) Uani d 1 . .
H H1C 0.377680 0.701450 0.238707 0.019 Uiso calc 1 . .
N N2C 0.3564(12) 0.6981(2) 0.4230(4) 0.0190(13) Uani d 1 . .
H H2C1 0.405214 0.704179 0.473316 0.023 Uiso calc 1 . .
N N3C -0.0987(11) 0.58344(19) 0.1671(4) 0.0139(12) Uani d 1 . .
H H3C1 -0.236078 0.577190 0.193104 0.017 Uiso calc 1 . .
N N4C -0.5595(11) 0.5433(2) -0.0706(4) 0.0163(12) Uani d 1 . .
H H4C3 -0.574463 0.553281 -0.123423 0.024 Uiso calc 1 . .
H H4C4 -0.699998 0.549560 -0.042776 0.024 Uiso calc 1 . .
H H4C5 -0.531174 0.511977 -0.070125 0.024 Uiso calc 1 . .
O O1C 0.1031(9) 0.54835(16) 0.3148(3) 0.0164(11) Uani d 1 . .
O O2C 0.4603(9) 0.57167(18) 0.2645(3) 0.0199(11) Uani d 1 . .
O O3C 0.1097(10) 0.57738(19) 0.0469(3) 0.0266(13) Uani d 1 . .
C C1D 1.1196(13) 0.6667(2) 0.8202(4) 0.0128(13) Uani d 1 . .
C C2D 1.1380(14) 0.6656(2) 0.9031(5) 0.0152(14) Uani d 1 . .
H H2D 1.029951 0.650016 0.939607 0.018 Uiso calc 1 . .
C C3D 1.4456(13) 0.7071(3) 0.8575(4) 0.0186(15) Uani d 1 . .
H H3D 1.589908 0.725561 0.855240 0.022 Uiso calc 1 . .
C C4D 0.9321(13) 0.6473(2) 0.7643(4) 0.0139(14) Uani d 1 . .
H H4D1 0.871802 0.672581 0.728162 0.017 Uiso calc 1 . .
H H4D2 0.792050 0.636108 0.797437 0.017 Uiso calc 1 . .
C C5D 1.0255(13) 0.6063(2) 0.7097(4) 0.0137(13) Uani d 1 . .
H H5D 1.145552 0.618184 0.668399 0.016 Uiso calc 1 . .
C C6D 1.1492(13) 0.5708(2) 0.7664(4) 0.0119(12) Uani d 1 . .
C C7D 0.7994(13) 0.5780(2) 0.5878(4) 0.0153(13) Uani d 1 . .
C C8D 0.5646(14) 0.5546(3) 0.5606(4) 0.0200(15) Uani d 1 . .
H H8D1 0.430611 0.564434 0.597742 0.024 Uiso calc 1 . .
H H8D2 0.583439 0.520389 0.565927 0.024 Uiso calc 1 . .
C C9D 0.4929(14) 0.5662(2) 0.4723(4) 0.0202(15) Uani d 1 . .
H H9D1 0.326172 0.554301 0.461277 0.024 Uiso calc 1 . .
H H9D2 0.490527 0.600568 0.465047 0.024 Uiso calc 1 . .
N N1D 1.3140(11) 0.69293(19) 0.7932(4) 0.0154(13) Uani d 1 . .
H H1D 1.346639 0.699361 0.741551 0.019 Uiso calc 1 . .
N N2D 1.3405(12) 0.6911(2) 0.9248(4) 0.0183(13) Uani d 1 . .
H H2D1 1.391867 0.695914 0.975300 0.022 Uiso calc 1 . .
N N3D 0.8159(10) 0.58597(19) 0.6684(4) 0.0130(12) Uani d 1 . .
H H3D1 0.689357 0.578279 0.698960 0.016 Uiso calc 1 . .
N N4D 0.6663(10) 0.54536(18) 0.4130(3) 0.0136(11) Uani d 1 . .
H H4D3 0.621520 0.553349 0.361033 0.020 Uiso calc 1 . .
H H4D4 0.664180 0.513717 0.418170 0.020 Uiso calc 1 . .
H H4D5 0.819867 0.556165 0.423240 0.020 Uiso calc 1 . .
O O1D 1.3782(10) 0.56976(17) 0.7678(3) 0.0182(11) Uani d 1 . .
O O2D 1.0098(10) 0.54720(16) 0.8113(3) 0.0183(11) Uani d 1 . .
O O3D 0.9634(9) 0.58748(18) 0.5381(3) 0.0203(11) Uani d 1 . .
Br Br1 1.56379(13) 0.70170(2) 1.10573(4) 0.01930(16) Uani d 1 . .
Br Br2 1.05535(14) 0.29847(2) 0.64419(5) 0.0199(2) Uani d 1 . .
Br Br3 0.52414(14) 0.70397(2) 0.60864(4) 0.02070(17) Uani d 1 . .
Br Br4 1.04519(14) 0.29020(2) 0.13994(5) 0.0208(2) 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
C1A 0.016(3) 0.009(3) 0.012(3) -0.003(2) -0.002(3) -0.001(2)
C2A 0.016(3) 0.016(3) 0.021(4) -0.004(3) -0.001(3) -0.007(3)
C3A 0.023(4) 0.011(3) 0.013(3) -0.001(3) -0.001(3) -0.001(2)
C4A 0.016(3) 0.012(3) 0.017(4) -0.003(2) 0.006(3) -0.003(2)
C5A 0.020(3) 0.010(3) 0.011(3) 0.001(2) 0.000(3) -0.001(2)
C6A 0.019(3) 0.010(3) 0.006(3) -0.002(2) -0.004(3) -0.003(2)
C7A 0.023(3) 0.012(3) 0.009(3) 0.000(3) -0.002(3) 0.000(2)
C8A 0.020(3) 0.027(3) 0.008(3) 0.007(3) -0.001(3) 0.000(3)
C9A 0.022(3) 0.024(3) 0.011(3) -0.005(3) 0.002(3) -0.005(3)
N1A 0.017(3) 0.013(3) 0.012(3) -0.002(2) -0.002(2) -0.002(2)
N2A 0.023(3) 0.018(3) 0.016(3) -0.003(3) 0.006(3) -0.002(3)
N3A 0.020(3) 0.015(3) 0.009(3) 0.003(2) -0.002(2) 0.000(2)
N4A 0.013(3) 0.013(2) 0.019(3) 0.000(2) 0.001(2) 0.002(2)
O1A 0.019(2) 0.024(3) 0.011(3) -0.004(2) 0.000(2) 0.002(2)
O2A 0.021(2) 0.014(2) 0.010(2) -0.0001(19) -0.005(2) 0.0024(17)
O3A 0.019(3) 0.030(3) 0.014(3) 0.005(2) -0.006(2) -0.008(2)
C1B 0.017(3) 0.009(3) 0.014(3) 0.001(2) -0.001(3) -0.002(2)
C2B 0.028(4) 0.010(3) 0.017(3) -0.001(3) 0.004(3) 0.003(3)
C3B 0.022(3) 0.016(3) 0.021(4) 0.002(3) 0.006(3) -0.006(3)
C4B 0.014(3) 0.012(3) 0.015(3) -0.001(2) 0.001(3) -0.003(2)
C5B 0.016(3) 0.014(3) 0.007(3) 0.004(2) -0.002(3) -0.001(2)
C6B 0.0133(15) 0.0100(15) 0.0092(16) 0.0000(11) -0.0006(11) -0.0007(11)
C7B 0.011(3) 0.011(3) 0.017(3) 0.000(2) -0.003(3) -0.005(2)
C8B 0.024(4) 0.019(3) 0.008(3) 0.004(3) 0.004(3) 0.002(2)
C9B 0.017(3) 0.019(3) 0.013(3) 0.002(3) -0.001(3) 0.003(3)
N1B 0.023(3) 0.012(3) 0.011(3) 0.002(2) -0.002(2) -0.003(2)
N2B 0.020(3) 0.019(3) 0.019(3) -0.004(2) 0.003(3) -0.008(3)
N3B 0.013(3) 0.017(3) 0.010(3) 0.003(2) -0.004(2) -0.003(2)
N4B 0.021(3) 0.014(3) 0.016(3) -0.007(2) 0.005(3) -0.002(2)
O1B 0.020(2) 0.026(3) 0.011(3) -0.001(2) -0.002(2) 0.005(2)
O2B 0.020(2) 0.014(2) 0.015(2) 0.0009(19) -0.004(2) 0.0021(18)
O3B 0.018(3) 0.039(3) 0.016(3) 0.005(2) -0.008(2) -0.010(2)
C1C 0.019(3) 0.005(3) 0.014(3) 0.002(2) 0.001(3) -0.002(2)
C2C 0.017(3) 0.013(3) 0.013(3) 0.001(3) -0.002(3) -0.002(2)
C3C 0.027(4) 0.015(4) 0.022(4) -0.002(3) 0.002(3) -0.002(3)
C4C 0.023(4) 0.015(3) 0.008(3) 0.002(3) -0.004(3) 0.000(2)
C5C 0.015(3) 0.014(3) 0.008(3) -0.006(2) -0.003(3) -0.002(2)
C6C 0.0149(16) 0.0114(15) 0.0105(16) 0.0001(11) -0.0001(11) -0.0008(11)
C7C 0.021(3) 0.013(3) 0.015(3) -0.003(3) -0.003(3) -0.001(2)
C8C 0.011(3) 0.018(3) 0.021(3) -0.003(3) -0.007(3) 0.000(3)
C9C 0.013(3) 0.014(3) 0.023(4) -0.001(3) -0.005(3) 0.002(3)
N1C 0.019(3) 0.009(3) 0.018(3) -0.001(2) 0.000(2) 0.002(2)
N2C 0.025(3) 0.017(3) 0.015(3) -0.002(3) -0.006(3) -0.007(2)
N3C 0.019(3) 0.014(3) 0.009(3) -0.004(2) 0.000(2) 0.001(2)
N4C 0.017(3) 0.015(3) 0.017(3) 0.001(2) -0.002(2) -0.001(2)
O1C 0.020(2) 0.012(2) 0.017(3) -0.0008(19) 0.000(2) 0.0004(18)
O2C 0.020(3) 0.026(3) 0.013(3) -0.001(2) -0.004(2) 0.004(2)
O3C 0.021(3) 0.035(3) 0.024(3) -0.008(2) 0.005(2) -0.010(2)
C1D 0.015(3) 0.008(3) 0.015(3) 0.003(2) -0.004(3) -0.001(2)
C2D 0.018(3) 0.014(3) 0.014(3) 0.001(3) -0.003(3) -0.001(3)
C3D 0.020(3) 0.015(3) 0.022(4) 0.005(3) -0.002(3) -0.005(3)
C4D 0.020(3) 0.011(3) 0.011(3) 0.003(3) -0.009(3) -0.001(2)
C5D 0.021(3) 0.010(3) 0.009(3) -0.001(2) -0.004(3) 0.001(2)
C6D 0.018(3) 0.012(3) 0.006(3) 0.003(2) -0.002(3) -0.004(2)
C7D 0.017(3) 0.019(3) 0.010(3) -0.003(3) 0.000(3) 0.001(2)
C8D 0.016(3) 0.026(4) 0.018(3) -0.006(3) -0.003(3) -0.005(3)
C9D 0.017(3) 0.021(3) 0.022(4) 0.007(3) -0.001(3) 0.001(3)
N1D 0.017(3) 0.014(3) 0.015(3) -0.001(2) 0.000(2) -0.001(2)
N2D 0.021(3) 0.017(3) 0.016(3) 0.004(2) -0.009(3) -0.004(2)
N3D 0.012(3) 0.017(3) 0.010(3) -0.005(2) -0.003(2) 0.001(2)
N4D 0.010(2) 0.014(2) 0.017(3) 0.001(2) -0.002(2) 0.001(2)
O1D 0.022(3) 0.022(2) 0.012(3) 0.006(2) -0.005(2) 0.003(2)
O2D 0.030(3) 0.010(2) 0.015(2) -0.004(2) 0.004(2) 0.0003(17)
O3D 0.011(2) 0.032(3) 0.018(3) -0.006(2) 0.001(2) -0.007(2)
Br1 0.0218(3) 0.0225(3) 0.0136(3) -0.0042(4) -0.0046(3) 0.0042(3)
Br2 0.0230(4) 0.0231(4) 0.0135(4) 0.0070(3) 0.0044(3) 0.0039(3)
Br3 0.0248(3) 0.0239(3) 0.0134(4) -0.0033(4) -0.0029(3) 0.0037(3)
Br4 0.0231(4) 0.0244(5) 0.0148(4) 0.0011(3) 0.0042(3) 0.0043(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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3A C1A N1A . . 106.0(6) ?
C3A C1A C4A . . 131.0(7) ?
N1A C1A C4A . . 123.0(6) ?
N2A C2A N1A . . 109.1(7) ?
N2A C2A H2A . . 125.5 ?
N1A C2A H2A . . 125.5 ?
C1A C3A N2A . . 106.8(7) ?
C1A C3A H3A . . 126.6 ?
N2A C3A H3A . . 126.6 ?
C1A C4A C5A . . 113.9(6) ?
C1A C4A H4A1 . . 108.8 ?
C5A C4A H4A1 . . 108.8 ?
C1A C4A H4A2 . . 108.8 ?
C5A C4A H4A2 . . 108.8 ?
H4A1 C4A H4A2 . . 107.7 ?
N3A C5A C6A . . 109.8(5) ?
N3A C5A C4A . . 107.2(6) ?
C6A C5A C4A . . 107.6(5) ?
N3A C5A H5A . . 110.7 ?
C6A C5A H5A . . 110.7 ?
C4A C5A H5A . . 110.7 ?
O2A C6A O1A . . 125.8(6) ?
O2A C6A C5A . . 117.2(6) ?
O1A C6A C5A . . 116.9(6) ?
O3A C7A N3A . . 124.1(7) ?
O3A C7A C8A . . 121.2(6) ?
N3A C7A C8A . . 114.7(6) ?
C9A C8A C7A . . 112.4(6) ?
C9A C8A H8A1 . . 109.1 ?
C7A C8A H8A1 . . 109.1 ?
C9A C8A H8A2 . . 109.1 ?
C7A C8A H8A2 . . 109.1 ?
H8A1 C8A H8A2 . . 107.9 ?
N4A C9A C8A . . 112.0(6) ?
N4A C9A H9A1 . . 109.2 ?
C8A C9A H9A1 . . 109.2 ?
N4A C9A H9A2 . . 109.2 ?
C8A C9A H9A2 . . 109.2 ?
H9A1 C9A H9A2 . . 107.9 ?
C2A N1A C1A . . 108.7(6) ?
C2A N1A H1A . . 125.6 ?
C1A N1A H1A . . 125.6 ?
C2A N2A C3A . . 109.5(6) ?
C2A N2A H2A1 . . 125.3 ?
C3A N2A H2A1 . . 125.3 ?
C7A N3A C5A . . 124.6(7) ?
C7A N3A H3A1 . . 117.7 ?
C5A N3A H3A1 . . 117.7 ?
C9A N4A H4A3 . . 109.5 ?
C9A N4A H4A4 . . 109.5 ?
H4A3 N4A H4A4 . . 109.5 ?
C9A N4A H4A5 . . 109.5 ?
H4A3 N4A H4A5 . . 109.5 ?
H4A4 N4A H4A5 . . 109.5 ?
C2B C1B N1B . . 106.3(6) ?
C2B C1B C4B . . 131.3(7) ?
N1B C1B C4B . . 122.4(6) ?
C1B C2B N2B . . 107.1(7) ?
C1B C2B H2B . . 126.5 ?
N2B C2B H2B . . 126.5 ?
N2B C3B N1B . . 106.7(7) ?
N2B C3B H3B . . 126.6 ?
N1B C3B H3B . . 126.6 ?
C1B C4B C5B . . 113.1(6) ?
C1B C4B H4B1 . . 109.0 ?
C5B C4B H4B1 . . 109.0 ?
C1B C4B H4B2 . . 109.0 ?
C5B C4B H4B2 . . 109.0 ?
H4B1 C4B H4B2 . . 107.8 ?
N3B C5B C6B . . 111.8(5) ?
N3B C5B C4B . . 106.9(5) ?
C6B C5B C4B . . 110.0(5) ?
N3B C5B H5B . . 109.4 ?
C6B C5B H5B . . 109.4 ?
C4B C5B H5B . . 109.4 ?
O1B C6B O2B . . 125.9(6) ?
O1B C6B C5B . . 118.9(6) ?
O2B C6B C5B . . 115.2(6) ?
O3B C7B N3B . . 124.2(6) ?
O3B C7B C8B . . 121.9(6) ?
N3B C7B C8B . . 113.9(6) ?
C9B C8B C7B . . 109.8(6) ?
C9B C8B H8B1 . . 109.7 ?
C7B C8B H8B1 . . 109.7 ?
C9B C8B H8B2 . . 109.7 ?
C7B C8B H8B2 . . 109.7 ?
H8B1 C8B H8B2 . . 108.2 ?
N4B C9B C8B . . 111.1(6) ?
N4B C9B H9B1 . . 109.4 ?
C8B C9B H9B1 . . 109.4 ?
N4B C9B H9B2 . . 109.4 ?
C8B C9B H9B2 . . 109.4 ?
H9B1 C9B H9B2 . . 108.0 ?
C3B N1B C1B . . 109.9(6) ?
C3B N1B H1B . . 125.0 ?
C1B N1B H1B . . 125.0 ?
C3B N2B C2B . . 109.9(6) ?
C3B N2B H2B1 . . 125.0 ?
C2B N2B H2B1 . . 125.0 ?
C7B N3B C5B . . 122.0(6) ?
C7B N3B H3B1 . . 119.0 ?
C5B N3B H3B1 . . 119.0 ?
C9B N4B H4B3 . . 109.5 ?
C9B N4B H4B4 . . 109.5 ?
H4B3 N4B H4B4 . . 109.5 ?
C9B N4B H4B5 . . 109.5 ?
H4B3 N4B H4B5 . . 109.5 ?
H4B4 N4B H4B5 . . 109.5 ?
C2C C1C N1C . . 106.6(7) ?
C2C C1C C4C . . 131.2(6) ?
N1C C1C C4C . . 122.2(6) ?
C1C C2C N2C . . 107.3(6) ?
C1C C2C H2C . . 126.3 ?
N2C C2C H2C . . 126.3 ?
N1C C3C N2C . . 108.3(7) ?
N1C C3C H3C . . 125.8 ?
N2C C3C H3C . . 125.8 ?
C1C C4C C5C . . 113.5(6) ?
C1C C4C H4C1 . . 108.9 ?
C5C C4C H4C1 . . 108.9 ?
C1C C4C H4C2 . . 108.9 ?
C5C C4C H4C2 . . 108.9 ?
H4C1 C4C H4C2 . . 107.7 ?
N3C C5C C4C . . 106.8(6) ?
N3C C5C C6C . . 110.8(5) ?
C4C C5C C6C . . 110.0(6) ?
N3C C5C H5C . . 109.7 ?
C4C C5C H5C . . 109.7 ?
C6C C5C H5C . . 109.7 ?
O1C C6C O2C . . 126.2(7) ?
O1C C6C C5C . . 116.3(6) ?
O2C C6C C5C . . 117.4(6) ?
O3C C7C N3C . . 123.4(7) ?
O3C C7C C8C . . 121.3(6) ?
N3C C7C C8C . . 115.3(6) ?
C7C C8C C9C . . 110.2(6) ?
C7C C8C H8C1 . . 109.6 ?
C9C C8C H8C1 . . 109.6 ?
C7C C8C H8C2 . . 109.6 ?
C9C C8C H8C2 . . 109.6 ?
H8C1 C8C H8C2 . . 108.1 ?
N4C C9C C8C . . 111.8(5) ?
N4C C9C H9C1 . . 109.3 ?
C8C C9C H9C1 . . 109.3 ?
N4C C9C H9C2 . . 109.3 ?
C8C C9C H9C2 . . 109.3 ?
H9C1 C9C H9C2 . . 107.9 ?
C3C N1C C1C . . 108.8(6) ?
C3C N1C H1C . . 125.6 ?
C1C N1C H1C . . 125.6 ?
C3C N2C C2C . . 108.9(7) ?
C3C N2C H2C1 . . 125.5 ?
C2C N2C H2C1 . . 125.5 ?
C7C N3C C5C . . 122.7(6) ?
C7C N3C H3C1 . . 118.6 ?
C5C N3C H3C1 . . 118.6 ?
C9C N4C H4C3 . . 109.5 ?
C9C N4C H4C4 . . 109.5 ?
H4C3 N4C H4C4 . . 109.5 ?
C9C N4C H4C5 . . 109.5 ?
H4C3 N4C H4C5 . . 109.5 ?
H4C4 N4C H4C5 . . 109.5 ?
C2D C1D N1D . . 106.0(7) ?
C2D C1D C4D . . 131.0(6) ?
N1D C1D C4D . . 123.0(6) ?
C1D C2D N2D . . 107.7(6) ?
C1D C2D H2D . . 126.1 ?
N2D C2D H2D . . 126.1 ?
N2D C3D N1D . . 108.1(6) ?
N2D C3D H3D . . 125.9 ?
N1D C3D H3D . . 125.9 ?
C1D C4D C5D . . 114.1(6) ?
C1D C4D H4D1 . . 108.7 ?
C5D C4D H4D1 . . 108.7 ?
C1D C4D H4D2 . . 108.7 ?
C5D C4D H4D2 . . 108.7 ?
H4D1 C4D H4D2 . . 107.6 ?
N3D C5D C6D . . 111.2(5) ?
N3D C5D C4D . . 107.9(6) ?
C6D C5D C4D . . 107.5(6) ?
N3D C5D H5D . . 110.0 ?
C6D C5D H5D . . 110.0 ?
C4D C5D H5D . . 110.0 ?
O1D C6D O2D . . 125.8(7) ?
O1D C6D C5D . . 117.9(6) ?
O2D C6D C5D . . 116.2(6) ?
O3D C7D N3D . . 123.8(7) ?
O3D C7D C8D . . 121.3(6) ?
N3D C7D C8D . . 114.9(6) ?
C7D C8D C9D . . 113.4(6) ?
C7D C8D H8D1 . . 108.9 ?
C9D C8D H8D1 . . 108.9 ?
C7D C8D H8D2 . . 108.9 ?
C9D C8D H8D2 . . 108.9 ?
H8D1 C8D H8D2 . . 107.7 ?
N4D C9D C8D . . 111.3(6) ?
N4D C9D H9D1 . . 109.4 ?
C8D C9D H9D1 . . 109.4 ?
N4D C9D H9D2 . . 109.4 ?
C8D C9D H9D2 . . 109.4 ?
H9D1 C9D H9D2 . . 108.0 ?
C3D N1D C1D . . 109.4(6) ?
C3D N1D H1D . . 125.3 ?
C1D N1D H1D . . 125.3 ?
C3D N2D C2D . . 108.8(7) ?
C3D N2D H2D1 . . 125.6 ?
C2D N2D H2D1 . . 125.6 ?
C7D N3D C5D . . 125.3(6) ?
C7D N3D H3D1 . . 117.3 ?
C5D N3D H3D1 . . 117.4 ?
C9D N4D H4D3 . . 109.5 ?
C9D N4D H4D4 . . 109.5 ?
H4D3 N4D H4D4 . . 109.5 ?
C9D N4D H4D5 . . 109.5 ?
H4D3 N4D H4D5 . . 109.5 ?
H4D4 N4D H4D5 . . 109.5 ?
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
C1A C3A . 1.362(10) ?
C1A N1A . 1.386(9) ?
C1A C4A . 1.492(9) ?
C2A N2A . 1.300(10) ?
C2A N1A . 1.330(9) ?
C2A H2A . 0.9500 ?
C3A N2A . 1.381(9) ?
C3A H3A . 0.9500 ?
C4A C5A . 1.542(10) ?
C4A H4A1 . 0.9900 ?
C4A H4A2 . 0.9900 ?
C5A N3A . 1.462(8) ?
C5A C6A . 1.541(9) ?
C5A H5A . 1.0000 ?
C6A O2A . 1.242(8) ?
C6A O1A . 1.256(9) ?
C7A O3A . 1.236(9) ?
C7A N3A . 1.330(8) ?
C7A C8A . 1.528(9) ?
C8A C9A . 1.527(9) ?
C8A H8A1 . 0.9900 ?
C8A H8A2 . 0.9900 ?
C9A N4A . 1.466(9) ?
C9A H9A1 . 0.9900 ?
C9A H9A2 . 0.9900 ?
N1A H1A . 0.8800 ?
N2A H2A1 . 0.8800 ?
N3A H3A1 . 0.8800 ?
N4A H4A3 . 0.9100 ?
N4A H4A4 . 0.9100 ?
N4A H4A5 . 0.9100 ?
C1B C2B . 1.351(10) ?
C1B N1B . 1.380(10) ?
C1B C4B . 1.491(9) ?
C2B N2B . 1.375(9) ?
C2B H2B . 0.9500 ?
C3B N2B . 1.331(11) ?
C3B N1B . 1.339(9) ?
C3B H3B . 0.9500 ?
C4B C5B . 1.548(9) ?
C4B H4B1 . 0.9900 ?
C4B H4B2 . 0.9900 ?
C5B N3B . 1.455(8) ?
C5B C6B . 1.546(8) ?
C5B H5B . 1.0000 ?
C6B O1B . 1.232(8) ?
C6B O2B . 1.270(8) ?
C7B O3B . 1.231(9) ?
C7B N3B . 1.332(9) ?
C7B C8B . 1.519(9) ?
C8B C9B . 1.518(8) ?
C8B H8B1 . 0.9900 ?
C8B H8B2 . 0.9900 ?
C9B N4B . 1.465(8) ?
C9B H9B1 . 0.9900 ?
C9B H9B2 . 0.9900 ?
N1B H1B . 0.8800 ?
N2B H2B1 . 0.8800 ?
N3B H3B1 . 0.8800 ?
N4B H4B3 . 0.9100 ?
N4B H4B4 . 0.9100 ?
N4B H4B5 . 0.9100 ?
C1C C2C . 1.342(10) ?
C1C N1C . 1.405(9) ?
C1C C4C . 1.474(11) ?
C2C N2C . 1.390(10) ?
C2C H2C . 0.9500 ?
C3C N1C . 1.327(10) ?
C3C N2C . 1.334(9) ?
C3C H3C . 0.9500 ?
C4C C5C . 1.538(9) ?
C4C H4C1 . 0.9900 ?
C4C H4C2 . 0.9900 ?
C5C N3C . 1.452(9) ?
C5C C6C . 1.544(10) ?
C5C H5C . 1.0000 ?
C6C O1C . 1.242(8) ?
C6C O2C . 1.247(8) ?
C7C O3C . 1.239(8) ?
C7C N3C . 1.343(9) ?
C7C C8C . 1.495(10) ?
C8C C9C . 1.508(10) ?
C8C H8C1 . 0.9900 ?
C8C H8C2 . 0.9900 ?
C9C N4C . 1.465(9) ?
C9C H9C1 . 0.9900 ?
C9C H9C2 . 0.9900 ?
N1C H1C . 0.8800 ?
N2C H2C1 . 0.8800 ?
N3C H3C1 . 0.8800 ?
N4C H4C3 . 0.9100 ?
N4C H4C4 . 0.9100 ?
N4C H4C5 . 0.9100 ?
C1D C2D . 1.353(10) ?
C1D N1D . 1.373(9) ?
C1D C4D . 1.480(11) ?
C2D N2D . 1.372(10) ?
C2D H2D . 0.9500 ?
C3D N2D . 1.321(9) ?
C3D N1D . 1.333(10) ?
C3D H3D . 0.9500 ?
C4D C5D . 1.558(9) ?
C4D H4D1 . 0.9900 ?
C4D H4D2 . 0.9900 ?
C5D N3D . 1.450(9) ?
C5D C6D . 1.531(10) ?
C5D H5D . 1.0000 ?
C6D O1D . 1.252(9) ?
C6D O2D . 1.253(8) ?
C7D O3D . 1.239(8) ?
C7D N3D . 1.336(9) ?
C7D C8D . 1.513(10) ?
C8D C9D . 1.528(11) ?
C8D H8D1 . 0.9900 ?
C8D H8D2 . 0.9900 ?
C9D N4D . 1.480(8) ?
C9D H9D1 . 0.9900 ?
C9D H9D2 . 0.9900 ?
N1D H1D . 0.8800 ?
N2D H2D1 . 0.8800 ?
N3D H3D1 . 0.8800 ?
N4D H4D3 . 0.9100 ?
N4D H4D4 . 0.9100 ?
N4D H4D5 . 0.9100 ?
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
N1A H1A Br4 1_455 0.88 2.39 3.242(7) 162 yes
N2A H2A1 Br2 1_454 0.88 2.33 3.205(6) 171 yes
N3A H3A1 O1A 1_455 0.88 2.04 2.918(9) 172 yes
N4A H4A3 O1B 1_355 0.91 1.88 2.771(7) 167 yes
N4A H4A4 O1C 1_455 0.91 1.84 2.744(7) 171 yes
N4A H4A5 O3A . 0.91 2.23 2.887(7) 129 yes
N4A H4A5 O2B 1_455 0.91 2.36 2.875(8) 116 yes
C2A H2A Br1 2_746 0.95 2.71 3.651(8) 170 yes
C4A H4A1 Br4 1_355 0.99 2.77 3.678(6) 153 yes
C9A H9A1 O3A 1_455 0.99 2.54 3.156(10) 120 yes
N1B H1B Br2 . 0.88 2.40 3.261(7) 167 yes
N2B H2B1 Br4 . 0.88 2.29 3.167(6) 173 yes
N3B H3B1 O1B 1_455 0.88 2.04 2.907(8) 170 yes
N4B H4B3 O1A 1_556 0.91 1.86 2.764(7) 171 yes
N4B H4B4 O3B 1_455 0.91 1.96 2.798(8) 153 yes
N4B H4B5 O2D 1_455 0.91 1.85 2.744(7) 169 yes
C2B H2B O3A 1_655 0.95 2.58 3.425(10) 149 yes
C3B H3B Br3 2_746 0.95 2.64 3.587(8) 171 yes
C4B H4B1 Br2 1_455 0.99 2.93 3.836(6) 152 yes
C5B H5B Br2 . 1.00 3.12 4.046(7) 155 yes
C8B H8B2 O3B 1_455 0.99 2.66 3.341(9) 127 yes
C9B H9B2 O2A 1_656 0.99 2.38 3.307(9) 156 yes
N1C H1C Br1 1_454 0.88 2.39 3.251(6) 165 yes
N2C H2C1 Br3 . 0.88 2.30 3.165(7) 168 yes
N3C H3C1 O2C 1_455 0.88 2.03 2.905(7) 171 yes
N4C H4C3 O1D 1_354 0.91 1.85 2.760(8) 176 yes
N4C H4C4 O3C 1_455 0.91 1.96 2.808(7) 154 yes
N4C H4C5 O2A . 0.91 1.84 2.747(7) 176 yes
C2C H2C O3D 1_455 0.95 2.58 3.422(9) 148 yes
C3C H3C Br2 2_756 0.95 2.64 3.583(8) 172 yes
C4C H4C1 Br1 1_354 0.99 2.85 3.776(8) 155 yes
C9C H9C2 O2D 1_454 0.99 2.37 3.300(8) 156 yes
N1D H1D Br3 1_655 0.88 2.38 3.234(6) 165 yes
N2D H2D1 Br1 . 0.88 2.33 3.204(7) 173 yes
N3D H3D1 O1D 1_455 0.88 2.05 2.926(7) 172 yes
N4D H4D3 O2C . 0.91 1.88 2.772(8) 167 yes
N4D H4D4 O2B . 0.91 1.85 2.751(7) 171 yes
N4D H4D5 O1C 1_655 0.91 2.36 2.875(7) 116 yes
N4D H4D5 O3D . 0.91 2.22 2.871(8) 128 yes
C3D H3D Br4 2_856 0.95 2.72 3.662(8) 170 yes
C4D H4D1 Br3 . 0.99 2.86 3.746(7) 149 yes
C9D H9D1 O3D 1_455 0.99 2.53 3.146(8) 120 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
N1A C1A C3A N2A . . . . -0.1(7) ?
C4A C1A C3A N2A . . . . -178.7(7) ?
C3A C1A C4A C5A . . . . -111.9(9) ?
N1A C1A C4A C5A . . . . 69.7(8) ?
C1A C4A C5A N3A . . . . 171.1(6) ?
C1A C4A C5A C6A . . . . 53.0(8) ?
N3A C5A C6A O2A . . . . -45.5(8) ?
C4A C5A C6A O2A . . . . 70.9(7) ?
N3A C5A C6A O1A . . . . 138.7(6) ?
C4A C5A C6A O1A . . . . -105.0(7) ?
O3A C7A C8A C9A . . . . -32.0(9) ?
N3A C7A C8A C9A . . . . 151.1(6) ?
C7A C8A C9A N4A . . . . 69.9(8) ?
N2A C2A N1A C1A . . . . 0.4(8) ?
C3A C1A N1A C2A . . . . -0.2(7) ?
C4A C1A N1A C2A . . . . 178.6(6) ?
N1A C2A N2A C3A . . . . -0.5(8) ?
C1A C3A N2A C2A . . . . 0.3(8) ?
O3A C7A N3A C5A . . . . 0.1(10) ?
C8A C7A N3A C5A . . . . 176.9(6) ?
C6A C5A N3A C7A . . . . -112.3(7) ?
C4A C5A N3A C7A . . . . 131.0(7) ?
N1B C1B C2B N2B . . . . -0.2(8) ?
C4B C1B C2B N2B . . . . 179.6(7) ?
C2B C1B C4B C5B . . . . -114.5(9) ?
N1B C1B C4B C5B . . . . 65.3(8) ?
C1B C4B C5B N3B . . . . 173.6(6) ?
C1B C4B C5B C6B . . . . 52.1(8) ?
N3B C5B C6B O1B . . . . 130.1(7) ?
C4B C5B C6B O1B . . . . -111.3(7) ?
N3B C5B C6B O2B . . . . -51.5(8) ?
C4B C5B C6B O2B . . . . 67.1(7) ?
O3B C7B C8B C9B . . . . -43.6(9) ?
N3B C7B C8B C9B . . . . 137.0(6) ?
C7B C8B C9B N4B . . . . 174.7(6) ?
N2B C3B N1B C1B . . . . 0.7(8) ?
C2B C1B N1B C3B . . . . -0.3(8) ?
C4B C1B N1B C3B . . . . 179.9(6) ?
N1B C3B N2B C2B . . . . -0.8(8) ?
C1B C2B N2B C3B . . . . 0.6(8) ?
O3B C7B N3B C5B . . . . 1.6(10) ?
C8B C7B N3B C5B . . . . -179.0(5) ?
C6B C5B N3B C7B . . . . -104.2(7) ?
C4B C5B N3B C7B . . . . 135.4(6) ?
N1C C1C C2C N2C . . . . -0.6(8) ?
C4C C1C C2C N2C . . . . 179.7(7) ?
C2C C1C C4C C5C . . . . -114.8(8) ?
N1C C1C C4C C5C . . . . 65.5(8) ?
C1C C4C C5C N3C . . . . 173.7(6) ?
C1C C4C C5C C6C . . . . 53.4(7) ?
N3C C5C C6C O1C . . . . -51.6(8) ?
C4C C5C C6C O1C . . . . 66.3(8) ?
N3C C5C C6C O2C . . . . 130.7(7) ?
C4C C5C C6C O2C . . . . -111.4(7) ?
O3C C7C C8C C9C . . . . -46.7(9) ?
N3C C7C C8C C9C . . . . 134.8(6) ?
C7C C8C C9C N4C . . . . 176.5(5) ?
N2C C3C N1C C1C . . . . 1.1(8) ?
C2C C1C N1C C3C . . . . -0.3(8) ?
C4C C1C N1C C3C . . . . 179.4(6) ?
N1C C3C N2C C2C . . . . -1.4(8) ?
C1C C2C N2C C3C . . . . 1.2(8) ?
O3C C7C N3C C5C . . . . 1.6(11) ?
C8C C7C N3C C5C . . . . -179.9(6) ?
C4C C5C N3C C7C . . . . 137.8(6) ?
C6C C5C N3C C7C . . . . -102.4(7) ?
N1D C1D C2D N2D . . . . 0.2(8) ?
C4D C1D C2D N2D . . . . -176.8(7) ?
C2D C1D C4D C5D . . . . -112.1(8) ?
N1D C1D C4D C5D . . . . 71.2(8) ?
C1D C4D C5D N3D . . . . 170.9(6) ?
C1D C4D C5D C6D . . . . 50.8(7) ?
N3D C5D C6D O1D . . . . 138.7(6) ?
C4D C5D C6D O1D . . . . -103.3(7) ?
N3D C5D C6D O2D . . . . -45.6(8) ?
C4D C5D C6D O2D . . . . 72.4(7) ?
O3D C7D C8D C9D . . . . -29.2(10) ?
N3D C7D C8D C9D . . . . 152.5(6) ?
C7D C8D C9D N4D . . . . 68.2(8) ?
N2D C3D N1D C1D . . . . -0.4(8) ?
C2D C1D N1D C3D . . . . 0.1(8) ?
C4D C1D N1D C3D . . . . 177.5(6) ?
N1D C3D N2D C2D . . . . 0.6(8) ?
C1D C2D N2D C3D . . . . -0.5(8) ?
O3D C7D N3D C5D . . . . -0.5(11) ?
C8D C7D N3D C5D . . . . 177.7(6) ?
C6D C5D N3D C7D . . . . -113.2(7) ?
C4D C5D N3D C7D . . . . 129.1(7) ?