#------------------------------------------------------------------------------
#$Date: 2022-09-23 05:04:31 +0300 (Fri, 23 Sep 2022) $
#$Revision: 278102 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244164.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_2244164
loop_
_publ_author_name
'Archana, Sreeramapura D.'
'Kiran Kumar, Haruvegowda'
'Yathirajan, Hemmige S.'
'Foro, Sabine'
'Butcher, Ray J.'
_publ_section_title
;
 The structures of eleven (4-phenyl)piperazinium salts containing organic
 anions
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009057
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C10 H15 N2 +, C7 H4 Br O2 -, H2 O'
_chemical_formula_moiety         'C10 H15 N2 +, C7 H4 Br O2 -, H2 O'
_chemical_formula_sum            'C17 H21 Br N2 O3'
_chemical_formula_weight         381.27
_chemical_name_systematic
;
4-Phenylpiperazin-1-ium 4-bromobenzoate monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.69(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.183(2)
_cell_length_b                   37.748(7)
_cell_length_c                   7.506(2)
_cell_measurement_reflns_used    1437
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.77
_cell_volume                     1748.2(8)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur with Sapphire CCD
;
_diffrn_measurement_method
;
\w and \f scans
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6103
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.772
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisRED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       rod
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.607
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3170
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.2432
_refine_ls_R_factor_gt           0.1380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+10.0601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3076
_refine_ls_wR_factor_ref         0.3753
_reflns_number_gt                1374
_reflns_number_total             3170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8034sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2244164
_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   0.409
_shelx_estimated_absorpt_t_max   0.764
_shelx_hkl_file
;
   0   0  -2 146418. 627.148   5
   0   0   2 147476. 679.496   4
   0   0   2 151559. 814.088   3
   0   0   3-3.95927 24.7086   3
   0   0  -3 73.1154 22.0820   5
   0   0   3 104.834 34.7354   4
   0   0   4 899.521 95.3043   4
   0   0  -4 820.174 74.5802   5
   0   0  -5 108.433 36.7801   5
   0   0   5 143.264 44.9734   4
   0   0   5 31.5018 33.9525   3
   0   0   6 133.769 46.0586   4
   0   0   6 59.8886 45.0095   3
   0   0  -6 168.452 45.1077   5
   0   0   7 32.8816 46.6091   3
   0   0   8 141.380 70.7338   3
   0   0   9 203.730 91.7556   3
   0   1   1 15.4869 10.1737   4
   0   1   1 3.77849 8.35300   3
   0  -1   2 36057.3 317.951   4
   0  -1  -2 35142.0 319.572   5
   0   1   2 34340.0 386.385   4
   0   1  -2 35682.6 308.070   5
   0   1   2 36761.3 417.168   3
   0  -1   3 293.275 40.8736   4
   0   1  -3 247.317 35.6644   5
   0   1   3 349.488 52.9877   4
   0  -1  -3 280.363 37.0503   5
   0   1   3 146.149 35.3917   3
   0  -1   3 210.620 42.5646   3
   0  -1   4 1929.90 136.632   3
   0   1   4 1989.58 121.459   4
   0  -1  -4 1814.86 105.169   5
   0   1  -4 1888.98 100.943   5
   0   1   4 1830.19 134.091   3
   0  -1   4 2265.36 135.466   4
   0  -1   5 253.994 54.1095   4
   0   1  -5 199.253 42.0055   5
   0  -1  -5 278.779 49.6971   5
   0  -1   5 145.819 47.2208   3
   0   1   5 134.029 52.9279   3
   0   1   5 260.110 57.7303   4
   0   1   6 44.5610 41.4705   3
   0   1  -6 90.3747 37.9064   5
   0  -1  -6 127.632 45.2839   5
   0  -1   6 79.5785 46.9978   3
   0  -1   6 120.924 45.8614   4
   0  -1   7 1.35547 41.6860   3
   0   1   7 52.9260 56.0621   3
   0  -1   8 149.284 72.6567   3
   0   1   8 156.712 77.7925   3
   0  -1   9 222.623 89.1139   3
   0   1   9 119.244 89.6362   3
   0   2   1 252.676 23.1995   4
   0  -2  -1 219.592 20.2552   5
   0   2   1 258.677 25.3314   3
   0   2   2 1833.96 110.754   4
   0   2  -2 3237.06 101.957   5
   0  -2  -2 4827.58 117.701   5
   0   2   2 2088.03 116.913   3
   0   2   3 461.148 63.3804   4
   0   2  -3 341.255 42.1107   5
   0  -2   3 372.438 43.7581   4
   0  -2  -3 513.237 55.8118   5
   0   2   4 728.946 80.7793   4
   0  -2   4 1134.14 100.683   4
   0   2  -4 794.958 68.5244   5
   0  -2  -4 857.377 75.3710   5
   0  -2   4 533.825 71.5801   3
   0   2   4 272.458 59.3794   3
   0   2   5 393.957 64.5144   4
   0  -2   5 564.536 80.0849   4
   0   2  -5 360.092 54.9093   5
   0  -2  -5 417.462 60.2441   5
   0  -2   5 362.311 72.5700   3
   0   2   5 410.489 74.5060   3
   0   2  -6 131.921 42.3770   5
   0  -2  -6 144.025 44.8556   5
   0  -2   6 56.9116 43.5370   3
   0  -2   6 119.044 46.3995   4
   0   2   6 56.0201 42.4286   3
   0  -2   7 30.1762 37.8172   3
   0   2   7 55.6318 47.7602   3
   0   2   8 157.394 76.5451   3
   0  -2   8 58.7127 66.1613   3
   0  -2   9 178.327 83.5953   3
   0  -3  -1 1220.84 49.4020   5
   0   3   2 6504.31 159.063   4
   0   3  -2 6610.15 117.731   5
   0  -3  -2 6502.67 145.563   5
   0  -3   2 6741.27 137.598   4
   0   3   2 6534.17 165.532   3
   0   3  -3 2157.68 87.9062   5
   0  -3   3 1999.13 90.1118   4
   0   3   3 2372.97 134.919   3
   0  -3  -3 2196.49 103.111   5
   0   3   3 2281.60 115.190   4
   0   3   4 1230.71 113.994   3
   0   3  -4 1467.24 86.0495   5
   0  -3  -4 1475.91 97.4606   5
   0   3   4 1375.04 103.846   4
   0  -3   4 1551.52 100.711   4
   0   3   5 88.5108 40.3406   4
   0  -3  -5 106.815 35.9525   5
   0  -3   5 62.5476 35.9418   3
   0   3   5 35.9902 32.2186   3
   0   3  -5 125.641 38.7505   5
   0  -3   5 179.503 48.9383   4
   0  -3  -6 115.637 44.4829   5
   0   3   6 78.2986 48.4595   3
   0  -3   6 80.7556 53.8739   3
   0  -3   6 170.476 51.6346   4
   0  -3  -7 22.0391 34.1337   5
   0   3   7 41.1814 49.3247   3
   0  -3   7 60.9259 40.4278   4
   0  -3   7-4.97127 35.2570   3
   0  -3   8 65.5367 66.3679   3
   0  -3   9 92.8035 84.5116   3
   0  -4  -1 2525.39 75.9994   5
   0   4  -2 230.583 21.8213   5
   0  -4   2 383.224 40.6967   4
   0   4   2 284.101 39.6878   4
   0   4   3 805.491 72.9781   4
   0  -4  -3 1083.81 75.8372   5
   0   4   3 777.075 78.4160   3
   0  -4   3 962.781 66.8015   4
   0   4  -3 811.513 54.7569   5
   0   4   4 1538.13 115.721   4
   0  -4   4 1700.19 103.692   4
   0   4   4 1321.17 110.775   3
   0  -4  -4 1648.33 104.335   5
   0   4  -4 1577.27 88.3683   5
   0  -4   5 71.0571 27.9254   4
   0  -4   5 9.52518 30.8796   3
   0   4   5 13.4723 33.2675   3
   0  -4  -5 52.7860 28.3902   5
   0   4  -5 33.7964 25.9084   5
   0  -4   6 339.163 85.1411   3
   0  -4   6 377.057 70.5399   4
   0   4   6 380.704 85.5297   3
   0  -4  -6 338.198 63.9632   5
   0  -4   7 64.0524 41.5215   4
   0   4   7 92.1131 61.3209   3
   0  -4  -7-1.22915 30.0625   5
   0  -4   7-9.35397 37.3473   3
   0  -4   8 50.9646 55.7651   3
   0  -4   9 79.1270 81.2725   3
   0  -5  -1 38.2041 14.7893   5
   0  -5  -2 138.686 27.9629   5
   0  -5   2 151.227 24.0362   4
   0   5  -3 610.541 44.8567   5
   0  -5  -3 649.977 57.8752   5
   0  -5   3 605.589 50.4968   4
   0  -5   4 1620.92 95.9212   4
   0   5  -4 1532.84 85.5457   5
   0  -5  -4 1608.82 103.653   5
   0   5   4 1633.93 132.443   3
   0  -5   5 238.715 52.7383   4
   0   5   5 204.313 59.4288   3
   0   5  -5 181.077 39.2264   5
   0  -5  -5 136.906 39.2131   5
   0  -5  -6 374.672 67.3492   5
   0   5   6 531.959 101.874   3
   0  -5   6 589.555 90.2909   4
   0  -5   6 369.882 82.0257   3
   0  -5   7 61.3931 39.9276   4
   0  -5  -7 57.8416 36.4725   5
   0  -5   7 9.92466 35.6036   3
   0  -5   8 12.4795 42.6841   3
   0  -5   9 137.406 86.1486   3
   0  -6   0 246.755 24.7041   2
   0  -6   0 269.946 23.5194   1
   0  -6  -1 3183.78 93.8332   5
   0  -6   2 995.860 54.5833   4
   0  -6  -2 921.818 61.9240   5
   0  -6   3 378.744 44.1645   4
   0  -6  -3 278.039 44.4406   5
   0  -6  -4 407.971 58.9125   5
   0   6  -4 258.458 39.8521   5
   0  -6   4 512.103 55.3800   4
   0  -6   5 407.820 60.9311   4
   0   6  -5 351.364 48.1760   5
   0  -6  -5 221.426 45.2023   5
   0  -6  -6 100.064 46.2899   5
   0  -6   6 88.1123 50.2094   3
   0  -6  -7 70.9899 44.7876   5
   0  -6   7 58.0022 52.7724   3
   0  -6   7 83.8317 45.2243   4
   0  -6   8-5.13596 44.1919   3
   0  -6   9 121.959 82.2533   3
   0  -7   0 9.91577 9.37680   1
   0  -7   0-3.18254 8.29541   2
   0  -7  -1 1058.50 57.9299   5
   0  -7   2 1655.44 69.2456   4
   0  -7  -2 1710.69 85.7705   5
   0  -7   3 3029.52 113.730   4
   0  -7  -3 2575.60 115.126   5
   0   7  -3 2842.31 87.9267   5
   0   7  -4 218.773 32.3790   5
   0  -7   4 194.251 35.8028   4
   0  -7  -4 235.416 45.2118   5
   0  -7  -5 232.219 45.5050   5
   0  -7   5 451.371 60.9840   4
   0  -7  -6 80.7047 44.7089   5
   0  -7   6 8.06743 36.7610   3
   0  -7   7 29.0147 38.0636   3
   0  -7  -7 99.9332 50.4549   5
   0  -7   7 78.6608 42.8291   4
   0  -7   8-55.9939 53.4415   3
   0  -7   9 98.9786 74.0655   3
   0  -8   0 3103.01 100.293   2
   0  -8   0 3454.00 95.9694   1
   0  -8  -1 3615.10 107.510   5
   0  -8   1 3894.16 80.6032   4
   0  -8   2 624.378 45.3644   4
   0  -8  -2 679.552 56.0342   5
   0  -8   3 900.356 66.6767   4
   0  -8  -3 716.063 68.6629   5
   0  -8  -4 129.321 35.4224   5
   0   8  -4 88.8757 21.8367   5
   0  -8   4 89.3899 25.2757   4
   0  -8  -5 39.4687 29.6114   5
   0  -8   5 132.901 38.0139   4
   0  -8   6 104.101 48.2214   4
   0  -8  -6 33.2436 35.7513   5
   0  -8   7 7.21581 37.0925   3
   0  -8   7 71.9282 37.9011   4
   0  -8  -7 12.9025 36.2456   5
   0  -8  -8 56.5117 46.6617   5
   0  -8   8-53.3078 58.2321   3
   0  -8   9 15.4372 52.0128   3
   0  -9   0 25.9667 15.3075   2
   0  -9   0 30.4335 14.9585   1
   0  -9   1 1311.98 48.9184   4
   0  -9  -1 1318.52 70.0006   5
   0  -9   2 765.087 48.9639   4
   0  -9  -2 824.344 63.5713   5
   0  -9  -3 2108.85 111.118   5
   0   9  -3 2196.12 71.4319   5
   0  -9   3 2490.50 104.910   4
   0   9  -4 12.6253 14.6408   5
   0  -9  -4 51.3967 25.8544   5
   0  -9   4 13.3331 18.5119   4
   0  -9  -5 313.332 61.0195   5
   0  -9   5 266.128 50.7796   4
   0  -9   6 59.1095 39.2487   4
   0  -9  -6 39.4778 32.2834   5
   0  -9   7 69.9904 42.9236   4
   0  -9  -7 78.7578 46.2225   5
   0  -9   7 31.4926 42.5751   3
   0  -9   8 98.6160 52.7201   4
   0  -9  -8-35.8490 42.5463   5
   0  -9   8-18.0981 48.4180   3
   0  -9   9-2.90786 50.0041   3
   0 -10   0 1259.54 69.2455   2
   0 -10   0 1486.17 70.7813   1
   0 -10  -1 11231.7 200.642   5
   0 -10   1 10748.3 146.886   4
   0 -10  -2 351.947 42.9424   5
   0 -10   2 385.224 36.8212   4
   0 -10   3 895.786 67.9876   4
   0 -10  -3 719.523 72.9265   5
   0 -10   4 45.1266 24.2933   4
   0 -10  -4 70.7288 33.4944   5
   0 -10   5 1083.89 84.8115   4
   0 -10  -5 1332.42 112.875   5
   0 -10  -6 49.0626 36.3838   5
   0 -10   6 55.9141 31.4552   4
   0 -10  -7 218.657 62.2526   5
   0 -10   7 59.5042 60.2835   3
   0 -10   7 167.941 63.2449   4
   0 -10   8 119.820 50.4869   4
   0 -10   8 34.3184 49.7494   3
   0 -10  -8 15.0266 44.4829   5
   0 -10   9 6.72208 55.0161   3
   0 -11   0 43.3674 23.8766   2
   0 -11   0 49.3362 21.6187   1
   0 -11   1 4475.28 101.778   4
   0 -11  -1 4717.99 135.657   5
   0 -11  -2 165.791 32.8669   5
   0 -11   2 143.544 24.1416   4
   0 -11  -3 3380.50 148.248   5
   0 -11   3 3609.19 122.978   4
   0 -11   4 310.527 45.6993   4
   0 -11  -4 335.013 58.0140   5
   0 -11   5 271.861 54.0430   4
   0 -11  -5 250.368 59.9567   5
   0 -11   6 115.650 40.4255   4
   0 -11  -6 136.742 49.3099   5
   0 -11   7 423.698 80.2983   4
   0 -11  -7 383.634 77.7567   5
   0 -11   8 16.7936 45.0191   3
   0 -11  -8 89.2025 52.1561   5
   0 -11   9 25.0316 61.3374   3
   0 -12   0 8304.17 185.096   1
   0 -12   0 7729.15 194.863   2
   0 -12  -1 8915.48 190.041   5
   0 -12  -2 1330.25 85.4214   5
   0 -12   2 1356.87 65.5319   4
   0 -12  -3 658.163 70.6203   5
   0 -12   3 642.477 55.1921   4
   0 -12  -4 178.838 43.2855   5
   0 -12   4 132.977 34.4469   4
   0 -12  -5 23.2206 26.6166   5
   0 -12   5 20.0422 21.3065   4
   0 -12  -6 67.9544 39.1717   5
   0 -12   6 113.572 38.7616   4
   0 -12  -7 96.4308 53.9476   5
   0 -12   7 197.754 62.1419   4
   0 -12  -8 44.4887 40.2198   5
   0 -12   8-95.1435 65.5084   3
   0 -12   9 19.6074 53.6375   3
   0 -13   0 126.764 32.0131   2
   0 -13   0 142.904 31.4363   1
   0 -13  -1 537.255 55.6727   1
   0 -13  -1 592.238 55.9855   5
   0 -13   2 1519.18 70.9521   4
   0 -13  -2 1531.91 93.7489   5
   0 -13  -3 684.419 69.7762   5
   0 -13   3 670.012 52.5574   4
   0 -13  -4 142.274 38.9955   5
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   3   1   6 41.4525 36.3777   4
   3  -1   6 52.8742 38.0430   4
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   3  -5   2-36.0182 31.0561   3
   3   5   2 41.6499 25.1786   4
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   3  -5   7 94.2937 47.6496   4
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   7  -3  -1 44.7456 44.4042   5
   7   3   0 23.2667 47.9517   5
   7  -3   0 59.1703 51.5074   5
   7   3   1-75.5375 73.2731   5
   7  -3   1 31.8388 62.8618   5
   7  -3   2-47.5798 52.9905   4
   7  -3   3 15.4092 41.3147   4
   7   3   4 90.3989 45.7300   4
   7   4  -4 76.4396 45.7430   5
   7  -4  -4 0.77097 49.7064   5
   7   4  -3 38.5699 42.4947   5
   7  -4  -3-9.13662 37.6104   5
   7   4  -2 14.3479 45.5844   5
   7  -4  -2 68.3688 56.2801   5
   7   4  -1 87.8662 52.5169   5
   7  -4  -1 10.7519 43.2506   5
   7   4   0 74.3549 52.2567   5
   7  -4   0-2.62610 38.1911   5
   7  -4   0 51.4344 41.5953   4
   7  -4   1 76.9021 59.1577   5
   7  -4   1 252.655 74.6012   4
   7  -4   2-7.11178 48.8737   4
   7  -4   3 30.6420 46.9858   4
   7   5  -4 70.3870 47.1907   5
   7  -5  -4 67.0076 56.4293   5
   7   5  -3 25.8579 51.3778   5
   7  -5  -3-62.0747 48.3973   5
   7   5  -2 61.1241 51.9028   5
   7  -5  -2 50.2706 51.2318   5
   7   5  -1 1.93024 44.4352   5
   7  -5  -1-6.58061 42.8050   5
   7   5   0 83.5088 62.8762   5
   7  -5   0 5.29641 41.5344   5
   7  -5   0-57.9175 45.5449   4
   7  -5   1 74.6764 49.5748   5
   7  -5   1 211.519 72.4751   4
   7  -5   2-33.1564 47.7098   4
   7  -5   3 14.0625 42.9213   4
   7   6  -4 45.4718 71.5004   5
   7  -6  -4 42.1050 47.6864   5
   7   6  -3 10.4808 51.9529   5
   7  -6  -3-8.76547 38.7366   5
   7   6  -2 51.4706 50.2619   5
   7  -6  -2-5.82959 38.2036   5
   7   6  -1 8.09433 45.5002   5
   7  -6  -1-0.10490 38.8910   5
   7   6   0 76.5790 63.2197   5
   7  -6   0 12.4738 51.8187   5
   7  -6   0-76.6691 49.5652   4
   7  -6   1 108.009 67.9959   5
   7  -6   1 205.115 69.8825   4
   7  -6   2 6.17535 49.5761   4
   7  -6   3-88.6389 61.3514   4
   7   7  -4 214.602 83.4593   5
   7  -7  -4-52.2046 58.4573   5
   7   7  -3 67.9001 51.7357   5
   7  -7  -3-3.83351 50.9913   5
   7   7  -2-59.5242 46.3133   5
   7  -7  -2-29.1920 45.1269   5
   7   7  -1 46.6450 50.9254   5
   7  -7  -1-1.57047 36.4547   5
   7   7   0 85.3342 56.1972   5
   7  -7   0 59.1583 44.8922   5
   7  -7   1 179.179 63.9488   4
   7  -7   2 112.743 66.1989   4
   7  -7   3-33.7640 57.3747   4
   7   8  -4-4.21931 44.0745   5
   7  -8  -4-72.3124 55.3408   5
   7   8  -3-15.0602 42.7561   5
   7  -8  -3-11.9114 36.8228   5
   7   8  -2 16.5482 52.3344   5
   7  -8  -2 18.2207 42.9170   5
   7   8  -1 50.5325 54.2301   5
   7  -8  -1 51.3490 40.1664   5
   7   8   0 46.4869 57.5391   5
   7  -8   0 100.054 50.7276   5
   7  -8   0-92.2218 59.5815   4
   7  -8   1 183.377 72.3279   4
   7  -8   2 192.721 72.2369   4
   7  -8   3-28.3822 63.0621   4
   7   9  -4-28.0627 48.6722   5
   7  -9  -4-63.2606 44.8136   5
   7   9  -3-19.4613 42.0400   5
   7  -9  -3-13.3049 48.1484   5
   7   9  -2 152.036 68.2027   5
   7  -9  -2 61.6131 41.3833   5
   7  -9  -1-112.284 60.4355   4
   7   9  -1 62.4253 62.7962   5
   7  -9  -1-12.9104 38.4021   5
   7  -9   0-41.8846 56.9526   4
   7   9   0 21.8286 52.7818   5
   7  -9   0 78.9701 52.7579   5
   7  -9   1 171.044 76.1605   4
   7  -9   2 189.972 71.2428   4
   7  -9   3-88.1079 63.0377   4
   7  10  -4 137.167 61.7934   5
   7 -10  -4-7.55659 42.5277   5
   7  10  -3-24.2721 50.4418   5
   7 -10  -3 27.9482 50.7685   5
   7  10  -2 81.3278 73.8835   5
   7 -10  -2 33.1851 43.3809   5
   7 -10  -1-105.508 59.3018   4
   7 -10  -1-31.2552 35.8957   5
   7 -10   0-97.9578 61.0929   4
   7  10   0 36.1762 50.7836   5
   7 -10   0 60.7913 58.9229   5
   7 -10   1 327.902 82.4295   4
   7 -10   2 359.071 93.0727   4
   7 -10   3-49.2771 53.8621   4
   7  11  -4 55.9237 54.1399   5
   7 -11  -4 27.0674 47.4344   5
   7  11  -3 57.0022 59.3410   5
   7 -11  -3 43.3321 53.2546   5
   7  11  -2 106.517 68.9868   5
   7 -11  -2-24.5447 43.8285   5
   7  11  -1 31.0267 45.4304   5
   7 -11  -1-31.8457 42.4823   5
   7 -11   0-81.9888 55.1420   4
   7 -11   0 41.0815 54.5903   5
   7 -11   1 220.427 77.9798   4
   7 -11   2 346.029 93.4611   4
   7 -11   3-114.771 69.6019   4
   7  12  -4-2.68714 46.3511   5
   7  12  -3 97.4530 69.0921   5
   7 -12  -3 59.0863 56.4722   5
   7  12  -2 99.6080 58.0515   5
   7 -12  -2 20.3000 46.4599   5
   7 -12  -1-138.020 70.4161   4
   7  12  -1 39.4154 55.0271   5
   7 -12  -1-62.3319 52.1657   5
   7 -12   0-144.059 59.3854   4
   7 -12   1 146.228 61.4634   4
   7 -12   2 254.155 81.6298   4
   7  13  -3 122.797 63.4107   5
   7 -13  -3-59.1950 51.5527   5
   7  13  -2 81.7319 73.2866   5
   7 -13  -2 64.2660 50.5707   5
   7  13  -1 39.2973 43.2648   5
   7 -13  -1 4.79404 49.2682   5
   7 -13   0-168.144 72.7003   4
   7 -13   1 110.587 63.0477   4
   7 -13   2 293.145 81.4050   4
   7  14  -3 98.9981 73.3524   5
   7 -14  -3-44.9769 44.2035   5
   7  14  -2 140.386 70.9528   5
   7 -14  -2 15.7681 42.5692   5
   7  14  -1-185.456 69.1502   5
   7 -14  -1-11.1564 38.5467   5
   7 -14   0-144.807 76.6920   4
   7 -14   1 59.8008 60.3799   4
   7 -14   2 281.738 89.1572   4
   7  15  -3 80.2700 61.8648   5
   7 -15  -3 19.5912 46.5710   5
   7  15  -2 82.4262 63.4020   5
   7 -15  -2-34.2641 47.1753   5
   7  15  -1-172.709 86.4799   5
   7 -15  -1-95.1118 56.8743   5
   7 -15   0-70.2570 62.1739   4
   7 -15   1 68.9988 54.6155   4
   7 -15   2 201.439 87.6971   4
   7  16  -3 67.5595 69.9848   5
   7 -16  -3 21.7026 44.6200   5
   7  16  -2 151.402 83.8227   5
   7 -16  -2-108.097 60.7016   5
   7 -16  -1-173.153 82.0206   4
   7 -16   0-122.009 71.7813   4
   7 -16   1-7.02729 41.4708   4
   7 -16   2 295.672 97.4099   4
   7  17  -3 58.9322 65.6068   5
   7 -17  -3 15.8432 52.7812   5
   7  17  -2 71.8215 49.1947   5
   7 -17  -2-36.9081 46.9197   5
   7 -17   0-140.578 70.6492   4
   7 -17   1-81.9268 61.4160   4
   7 -18  -3 18.9824 62.0503   5
   7  18  -2-154.362 73.4699   5
   7 -18  -2-9.99792 44.2468   5
   7 -18  -1-155.229 81.9378   4
   7 -18   1-46.0218 54.7387   4
   7 -19  -3-91.2840 59.6773   5
   7  19  -2-214.202 88.5715   5
   7 -19  -2-52.2413 65.9353   5
   7 -19   1-88.3054 65.8373   4
   7 -20  -3-74.7180 50.9145   5
   7 -21  -3-48.1415 44.8771   5
   8  -7   0 99.5186 76.4726   5
   0   0   0    0.00    0.00   0
;
_shelx_hkl_checksum              64980
_shelx_res_file
;
TITL HP3 IN P21/C
    shelx.res
    created by SHELXL-2018/3 at 17:23:02 on 26-Dec-2021
CELL  0.71073  6.18300 37.74800  7.50600 90.00000 93.69000 90.00000
ZERR 4  0.00200  0.00700  0.00200  0.00000  0.04000  0.00000
LATT 1
SYMM -X, Y+ 0.50000, -Z+ 0.50000
SFAC C H BR N O
UNIT 68 84 4 8 12
SHEL 38 0.83
SIZE 0.46 0.20 0.12
L.S. 25
rem damp 50
CONF
ACTA
BOND $H
htab
HTAB N2 O2
HTAB N2 O3
EQIV $1 -x+2, -y+1, -z+1
HTAB C8 O3_$1
EQIV $2 -x+2, -y+1, -z
HTAB C8 O2_$2
EQIV $3 -x+1, -y+1, -z+1
HTAB C9 O3_$3
HTAB O2 N2
HTAB O3 O2_$1
DFIX 0.82 0.02 O3 H31 O3 H32
dfix 1.297 .02 h31 h32
omit     1   2   3   !    625.55         26.01       7.18       0.016       2.25
omit     0   0   4   !    625.28         76.98       6.75       0.028       1.87
omit     1   2   4   !   1442.18        390.31       6.60       0.063       1.75
omit     2   1   0   !    669.60        126.49       5.26       0.036       3.07
omit    -1   0   2   !    794.46         67.91       5.16       0.026       3.30
omit     1   0   4   !   2642.45       1198.30       5.02       0.111       1.76
omit     2   1   5   !    173.03          4.37       5.00       0.007       1.31
omit     2   1   6   !    382.22          0.44       4.82       0.002       1.13
omit     3   3   5   !    413.38         26.15       4.80       0.016       1.17
omit    -1   3   1   !    261.38         22.62       4.80       0.015       4.58
omit    -3   2   1   !    602.94        180.75       4.72       0.043       2.01
omit     2   3   5   !    193.28          7.07       4.72       0.009       1.31
omit     0   2   2   !   2504.38        103.36       4.68       0.033       3.67
omit     0  21   1   !    134.98          5.43       4.23       0.007       1.75
omit    -2   3   2   !    639.04        246.85       4.04       0.050       2.41
bump
WGHT    0.128200   10.060101
FVAR       1.16462   0.68276
N1    4    0.703420    0.400202    0.229540    11.00000    0.04370    0.05019 =
         0.04586   -0.00502    0.00151    0.00251
N2    4    0.774396    0.475430    0.266075    11.00000    0.06277    0.05603 =
         0.05178    0.00026    0.01114   -0.00296
AFIX  23
H2N1  2    0.816948    0.495983    0.221941    21.00000   -1.20000
H2N2  2    0.734325    0.479226    0.376244    11.00000   -1.20000
AFIX   0
C1    1    0.652629    0.364897    0.264423    11.00000    0.05423    0.05258 =
         0.04829   -0.01050   -0.00132    0.00662
C2    1    0.451042    0.349858    0.200804    11.00000    0.06638    0.08460 =
         0.07572    0.02072   -0.02083   -0.00514
AFIX  43
H2    2    0.347995    0.364177    0.140653    11.00000   -1.20000
AFIX   0
C3    1    0.405919    0.315138    0.225930    11.00000    0.09172    0.07659 =
         0.11255    0.00368   -0.01768   -0.02133
AFIX  43
H3    2    0.275365    0.305737    0.179024    11.00000   -1.20000
AFIX   0
C4    1    0.552264    0.293755    0.320440    11.00000    0.11870    0.06675 =
         0.11581    0.01584   -0.01488   -0.00989
AFIX  43
H4    2    0.518855    0.270118    0.340272    11.00000   -1.20000
AFIX   0
C5    1    0.745013    0.307125    0.384615    11.00000    0.12676    0.06213 =
         0.13380    0.00952   -0.02084    0.01241
AFIX  43
H5    2    0.846262    0.292510    0.444957    11.00000   -1.20000
AFIX   0
C6    1    0.789806    0.341796    0.360679    11.00000    0.08508    0.06797 =
         0.11699    0.00028   -0.01452   -0.00356
AFIX  43
H6    2    0.919874    0.350644    0.411615    11.00000   -1.20000
AFIX   0
C7    1    0.893627    0.414835    0.332123    11.00000    0.03940    0.06022 =
         0.06781   -0.00292   -0.00033    0.00333
AFIX  23
H7A   2    0.863266    0.416060    0.457161    11.00000   -1.20000
H7B   2    1.015626    0.398972    0.321899    11.00000   -1.20000
AFIX   0
C8    1    0.952982    0.450248    0.271125    11.00000    0.05571    0.08370 =
         0.06077    0.00357    0.00990   -0.00376
AFIX  23
H8A   2    1.070611    0.459306    0.349995    11.00000   -1.20000
H8B   2    1.005544    0.448322    0.152505    11.00000   -1.20000
AFIX   0
C9    1    0.588624    0.461345    0.153248    11.00000    0.05403    0.06791 =
         0.06610    0.00580    0.00467    0.00262
AFIX  23
H9A   2    0.628083    0.459435    0.030616    11.00000   -1.20000
H9B   2    0.466823    0.477483    0.156218    11.00000   -1.20000
AFIX   0
C10   1    0.525532    0.426003    0.218903    11.00000    0.06457    0.06025 =
         0.04479   -0.00290   -0.01249    0.00374
AFIX  23
H10A  2    0.471137    0.428689    0.336512    11.00000   -1.20000
H10B  2    0.408395    0.416774    0.140070    11.00000   -1.20000
AFIX   0
BR1   3    0.970812    0.723395    0.173562    11.00000    0.26635    0.06255 =
         0.16876   -0.00063   -0.02043   -0.01545
O1    5    0.628929    0.555786    0.322199    11.00000    0.09095    0.13062 =
         0.12304    0.03707    0.03592   -0.02844
O2    5    0.908111    0.542611    0.168722    11.00000    0.09795    0.06330 =
         0.07183    0.00535    0.01517   -0.00525
AFIX  83
H2O   2    0.853628    0.522821    0.170738   -21.00000   -1.20000
AFIX   0
C11   1    0.832487    0.603055    0.221869    11.00000    0.05214    0.07355 =
         0.03279   -0.00477    0.00642    0.00389
C12   1    1.016266    0.615505    0.146538    11.00000    0.06948    0.07414 =
         0.04719   -0.00312    0.00847    0.00360
AFIX  43
H12   2    1.115409    0.599557    0.104078    11.00000   -1.20000
AFIX   0
C13   1    1.052646    0.650766    0.134261    11.00000    0.08451    0.06950 =
         0.06016    0.00043   -0.00338   -0.01549
AFIX  43
H13   2    1.177707    0.658367    0.083258    11.00000   -1.20000
AFIX   0
C14   1    0.919436    0.674690    0.191068    11.00000    0.12779    0.06747 =
         0.07074    0.00576    0.01245    0.01071
C15   1    0.740777    0.663793    0.277028    11.00000    0.11028    0.09038 =
         0.08919   -0.01571    0.00572    0.03594
AFIX  43
H15   2    0.650657    0.680550    0.324796    11.00000   -1.20000
AFIX   0
C16   1    0.694242    0.628077    0.292904    11.00000    0.07925    0.10217 =
         0.05965    0.00920    0.00975    0.00622
AFIX  43
H16   2    0.572770    0.620785    0.349992    11.00000   -1.20000
AFIX   0
C17   1    0.787105    0.564311    0.237641    11.00000    0.05778    0.08886 =
         0.03708    0.00832   -0.01275   -0.00874
O3    5    0.720717    0.479631    0.633509    11.00000    0.08056    0.07348 =
         0.06423   -0.00587    0.01047   -0.01463
H31   2    0.829655    0.475549    0.695802    11.00000   -1.50000
H32   2    0.697177    0.500362    0.634746    11.00000   -1.50000
HKLF 4
REM  HP3 IN P21/C
REM wR2 = 0.3753, GooF = S = 1.030, Restrained GooF = 1.033 for all data
REM R1 = 0.1380 for 1374 Fo > 4sig(Fo) and 0.2432 for all 3170 data
REM 215 parameters refined using 7 restraints
END
WGHT      0.1278     10.0983
REM Instructions for potential hydrogen bonds
HTAB N2 O2
HTAB N2 O3
HTAB C8 O3_$1
HTAB C8 O2_$2
HTAB C9 O3_$3
HTAB O2 N2
HTAB O3 O2_$1
REM Highest difference peak  0.486,  deepest hole -0.607,  1-sigma level  0.096
Q1    1   0.9632  0.7524  0.1631  11.00000  0.05    0.49
Q2    1   0.7972  0.7175  0.2886  11.00000  0.05    0.43
Q3    1   0.9086  0.6959  0.1905  11.00000  0.05    0.35
Q4    1   0.9263  0.2964  0.3656  11.00000  0.05    0.34
Q5    1   0.6012  0.4934  0.1648  11.00000  0.05    0.34
Q6    1   0.7273  0.2604  0.3353  11.00000  0.05    0.32
Q7    1   0.8488  0.3797  0.3675  11.00000  0.05    0.31
Q8    1   0.8371  0.3614  0.3424  11.00000  0.05    0.30
Q9    1   0.5810  0.2573  0.3190  11.00000  0.05    0.29
Q10   1   0.5944  0.2435  0.3346  11.00000  0.05    0.29
Q11   1   0.4478  0.3995  0.2015  11.00000  0.05    0.27
Q12   1   0.6478  0.6726  0.1379  11.00000  0.05    0.26
Q13   1   0.7386  0.3422  0.2519  11.00000  0.05    0.26
Q14   1   0.5457  0.5565  0.1212  11.00000  0.05    0.26
Q15   1   0.6249  0.3667  0.3259  11.00000  0.05    0.26
Q16   1   0.6177  0.4174  0.2743  11.00000  0.05    0.26
Q17   1   0.6472  0.5998  0.3493  11.00000  0.05    0.26
Q18   1   1.1977  0.7089  0.1717  11.00000  0.05    0.26
Q19   1   1.3678  0.6981  0.1590  11.00000  0.05    0.25
Q20   1   1.1565  0.5775  0.2168  11.00000  0.05    0.24
;
_shelx_res_checksum              56935
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
N N1 0.7034(12) 0.4002(2) 0.2295(10) 0.047(2) Uani d 1 . .
N N2 0.7744(14) 0.4754(2) 0.2661(11) 0.057(2) Uani d 1 . .
H H2N1 0.816948 0.495983 0.221941 0.068 Uiso calc 0.68(16) . .
H H2N2 0.734325 0.479226 0.376244 0.068 Uiso calc 1 . .
C C1 0.6526(17) 0.3649(3) 0.2644(14) 0.052(3) Uani d 1 . .
C C2 0.4510(19) 0.3499(3) 0.2008(17) 0.077(4) Uani d 1 . .
H H2 0.347995 0.364177 0.140653 0.092 Uiso calc 1 . .
C C3 0.406(2) 0.3151(4) 0.226(2) 0.095(4) Uani d 1 . .
H H3 0.275365 0.305737 0.179024 0.114 Uiso calc 1 . .
C C4 0.552(3) 0.2938(4) 0.320(2) 0.101(5) Uani d 1 . .
H H4 0.518855 0.270118 0.340272 0.122 Uiso calc 1 . .
C C5 0.745(3) 0.3071(4) 0.385(2) 0.109(5) Uani d 1 . .
H H5 0.846262 0.292510 0.444957 0.131 Uiso calc 1 . .
C C6 0.790(2) 0.3418(3) 0.361(2) 0.091(4) Uani d 1 . .
H H6 0.919874 0.350644 0.411615 0.109 Uiso calc 1 . .
C C7 0.8936(15) 0.4148(3) 0.3321(15) 0.056(3) Uani d 1 . .
H H7A 0.863266 0.416060 0.457161 0.067 Uiso calc 1 . .
H H7B 1.015626 0.398972 0.321899 0.067 Uiso calc 1 . .
C C8 0.9530(18) 0.4502(3) 0.2711(16) 0.066(3) Uani d 1 . .
H H8A 1.070611 0.459306 0.349995 0.080 Uiso calc 1 . .
H H8B 1.005544 0.448322 0.152505 0.080 Uiso calc 1 . .
C C9 0.5886(17) 0.4613(3) 0.1532(15) 0.063(3) Uani d 1 . .
H H9A 0.628083 0.459435 0.030616 0.075 Uiso calc 1 . .
H H9B 0.466823 0.477483 0.156218 0.075 Uiso calc 1 . .
C C10 0.5255(17) 0.4260(3) 0.2189(14) 0.057(3) Uani d 1 . .
H H10A 0.471137 0.428689 0.336512 0.069 Uiso calc 1 . .
H H10B 0.408395 0.416774 0.140070 0.069 Uiso calc 1 . .
Br Br1 0.9708(5) 0.72340(4) 0.1736(4) 0.1674(14) Uani d 1 . .
O O1 0.6289(16) 0.5558(3) 0.3222(15) 0.114(4) Uani d 1 . .
O O2 0.9081(15) 0.5426(2) 0.1687(11) 0.077(2) Uani d 1 . .
H H2O 0.853628 0.522821 0.170738 0.093 Uiso calc 0.32(16) . .
C C11 0.8325(17) 0.6031(3) 0.2219(13) 0.053(3) Uani d 1 . .
C C12 1.0163(19) 0.6155(3) 0.1465(14) 0.063(3) Uani d 1 . .
H H12 1.115409 0.599557 0.104078 0.076 Uiso calc 1 . .
C C13 1.053(2) 0.6508(3) 0.1343(16) 0.072(3) Uani d 1 . .
H H13 1.177707 0.658367 0.083258 0.086 Uiso calc 1 . .
C C14 0.919(3) 0.6747(4) 0.1911(19) 0.088(4) Uani d 1 . .
C C15 0.741(3) 0.6638(4) 0.277(2) 0.097(5) Uani d 1 . .
H H15 0.650657 0.680550 0.324796 0.116 Uiso calc 1 . .
C C16 0.694(2) 0.6281(4) 0.2929(17) 0.080(4) Uani d 1 . .
H H16 0.572770 0.620785 0.349992 0.096 Uiso calc 1 . .
C C17 0.787(2) 0.5643(4) 0.2376(14) 0.062(3) Uani d 1 . .
O O3 0.7207(13) 0.4796(2) 0.6335(11) 0.073(2) Uani d 1 . .
H H31 0.830(14) 0.4755(18) 0.696(17) 0.109 Uiso d 1 . .
H H32 0.697(5) 0.5004(5) 0.635(5) 0.109 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
N1 0.044(5) 0.050(5) 0.046(5) 0.003(4) 0.002(4) -0.005(4)
N2 0.063(6) 0.056(5) 0.052(5) -0.003(5) 0.011(4) 0.000(4)
C1 0.054(6) 0.053(6) 0.048(6) 0.007(5) -0.001(5) -0.010(5)
C2 0.066(8) 0.085(9) 0.076(8) -0.005(7) -0.021(7) 0.021(7)
C3 0.092(10) 0.077(9) 0.113(12) -0.021(8) -0.018(9) 0.004(9)
C4 0.119(13) 0.067(9) 0.116(12) -0.010(9) -0.015(10) 0.016(9)
C5 0.127(13) 0.062(9) 0.134(14) 0.012(9) -0.021(11) 0.010(9)
C6 0.085(9) 0.068(8) 0.117(12) -0.004(7) -0.015(8) 0.000(8)
C7 0.039(6) 0.060(7) 0.068(7) 0.003(5) 0.000(5) -0.003(6)
C8 0.056(7) 0.084(9) 0.061(7) -0.004(6) 0.010(6) 0.004(6)
C9 0.054(7) 0.068(7) 0.066(7) 0.003(6) 0.005(6) 0.006(6)
C10 0.065(7) 0.060(7) 0.045(6) 0.004(6) -0.012(5) -0.003(5)
Br1 0.266(3) 0.0626(11) 0.169(2) -0.0154(13) -0.020(2) -0.0006(12)
O1 0.091(7) 0.131(9) 0.123(8) -0.028(6) 0.036(7) 0.037(7)
O2 0.098(6) 0.063(5) 0.072(6) -0.005(5) 0.015(5) 0.005(4)
C11 0.052(6) 0.074(7) 0.033(5) 0.004(6) 0.006(5) -0.005(5)
C12 0.069(7) 0.074(8) 0.047(6) 0.004(6) 0.008(6) -0.003(6)
C13 0.085(9) 0.069(8) 0.060(8) -0.015(7) -0.003(6) 0.000(7)
C14 0.128(13) 0.067(8) 0.071(9) 0.011(9) 0.012(9) 0.006(7)
C15 0.110(12) 0.090(11) 0.089(10) 0.036(9) 0.006(10) -0.016(9)
C16 0.079(9) 0.102(11) 0.060(7) 0.006(8) 0.010(6) 0.009(8)
C17 0.058(7) 0.089(9) 0.037(6) -0.009(7) -0.013(5) 0.008(6)
O3 0.081(6) 0.073(5) 0.064(5) -0.015(4) 0.010(4) -0.006(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 N1 C10 . . 117.8(8) ?
C1 N1 C7 . . 116.2(8) ?
C10 N1 C7 . . 110.5(7) ?
C8 N2 C9 . . 109.8(8) ?
C8 N2 H2N1 . . 109.7 ?
C9 N2 H2N1 . . 109.7 ?
C8 N2 H2N2 . . 109.7 ?
C9 N2 H2N2 . . 109.7 ?
H2N1 N2 H2N2 . . 108.2 ?
C6 C1 N1 . . 124.0(10) ?
C6 C1 C2 . . 114.6(10) ?
N1 C1 C2 . . 121.3(9) ?
C3 C2 C1 . . 121.5(11) ?
C3 C2 H2 . . 119.3 ?
C1 C2 H2 . . 119.3 ?
C2 C3 C4 . . 120.3(13) ?
C2 C3 H3 . . 119.8 ?
C4 C3 H3 . . 119.8 ?
C5 C4 C3 . . 120.0(14) ?
C5 C4 H4 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
C6 C5 C4 . . 119.8(15) ?
C6 C5 H5 . . 120.1 ?
C4 C5 H5 . . 120.1 ?
C5 C6 C1 . . 123.7(13) ?
C5 C6 H6 . . 118.2 ?
C1 C6 H6 . . 118.2 ?
C8 C7 N1 . . 112.7(9) ?
C8 C7 H7A . . 109.0 ?
N1 C7 H7A . . 109.0 ?
C8 C7 H7B . . 109.0 ?
N1 C7 H7B . . 109.0 ?
H7A C7 H7B . . 107.8 ?
N2 C8 C7 . . 113.5(9) ?
N2 C8 H8A . . 108.9 ?
C7 C8 H8A . . 108.9 ?
N2 C8 H8B . . 108.9 ?
C7 C8 H8B . . 108.9 ?
H8A C8 H8B . . 107.7 ?
N2 C9 C10 . . 110.1(9) ?
N2 C9 H9A . . 109.6 ?
C10 C9 H9A . . 109.6 ?
N2 C9 H9B . . 109.6 ?
C10 C9 H9B . . 109.6 ?
H9A C9 H9B . . 108.2 ?
N1 C10 C9 . . 113.8(9) ?
N1 C10 H10A . . 108.8 ?
C9 C10 H10A . . 108.8 ?
N1 C10 H10B . . 108.8 ?
C9 C10 H10B . . 108.8 ?
H10A C10 H10B . . 107.7 ?
C17 O2 H2O . . 109.5 ?
C12 C11 C16 . . 117.6(11) ?
C12 C11 C17 . . 121.9(10) ?
C16 C11 C17 . . 120.4(11) ?
C13 C12 C11 . . 120.4(11) ?
C13 C12 H12 . . 119.8 ?
C11 C12 H12 . . 119.8 ?
C14 C13 C12 . . 123.0(13) ?
C14 C13 H13 . . 118.5 ?
C12 C13 H13 . . 118.5 ?
C13 C14 C15 . . 119.1(13) ?
C13 C14 Br1 . . 122.7(13) ?
C15 C14 Br1 . . 118.1(12) ?
C14 C15 C16 . . 120.5(13) ?
C14 C15 H15 . . 119.7 ?
C16 C15 H15 . . 119.7 ?
C15 C16 C11 . . 119.2(12) ?
C15 C16 H16 . . 120.4 ?
C11 C16 H16 . . 120.4 ?
O1 C17 O2 . . 123.8(12) ?
O1 C17 C11 . . 116.9(12) ?
O2 C17 C11 . . 119.3(10) ?
H31 O3 H32 . . 109(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
N1 C1 . 1.398(12) ?
N1 C10 . 1.467(12) ?
N1 C7 . 1.471(12) ?
N2 C8 . 1.456(13) ?
N2 C9 . 1.481(13) ?
N2 H2N1 . 0.8900 ?
N2 H2N2 . 0.8900 ?
C1 C6 . 1.387(16) ?
C1 C2 . 1.424(15) ?
C2 C3 . 1.356(17) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.38(2) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.35(2) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.352(17) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.467(14) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.483(14) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
Br1 C14 . 1.872(14) ?
O1 C17 . 1.242(13) ?
O2 C17 . 1.244(14) ?
O2 H2O . 0.8200 ?
C11 C12 . 1.384(14) ?
C11 C16 . 1.402(16) ?
C11 C17 . 1.495(16) ?
C12 C13 . 1.354(16) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.312(18) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.38(2) ?
C15 C16 . 1.385(19) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
O3 H31 . 0.81(2) ?
O3 H32 . 0.796(19) ?
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
N2 H2N1 O2 . 0.89 1.90 2.780(11) 170.2 yes
N2 H2N2 O3 . 0.89 1.94 2.803(12) 163.6 yes
C8 H8A O3 3_766 0.97 2.64 3.377(14) 132.9 yes
C8 H8B O2 3_765 0.97 2.53 3.475(14) 165.9 yes
C9 H9B O3 3_666 0.97 2.59 3.403(14) 141.8 yes
O2 H2O N2 . 0.82 2.00 2.780(11) 158.8 yes
O3 H31 O2 3_766 0.81(2) 1.98(2) 2.782(12) 170(7) 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
C10 N1 C1 C6 . . . . -147.2(11) ?
C7 N1 C1 C6 . . . . -12.7(15) ?
C10 N1 C1 C2 . . . . 33.1(14) ?
C7 N1 C1 C2 . . . . 167.6(10) ?
C6 C1 C2 C3 . . . . -3.4(18) ?
N1 C1 C2 C3 . . . . 176.3(12) ?
C1 C2 C3 C4 . . . . 3(2) ?
C2 C3 C4 C5 . . . . -2(3) ?
C3 C4 C5 C6 . . . . 2(3) ?
C4 C5 C6 C1 . . . . -3(3) ?
N1 C1 C6 C5 . . . . -175.8(14) ?
C2 C1 C6 C5 . . . . 4(2) ?
C1 N1 C7 C8 . . . . 172.4(9) ?
C10 N1 C7 C8 . . . . -50.0(11) ?
C9 N2 C8 C7 . . . . -55.9(12) ?
N1 C7 C8 N2 . . . . 53.6(12) ?
C8 N2 C9 C10 . . . . 55.7(11) ?
C1 N1 C10 C9 . . . . -170.7(9) ?
C7 N1 C10 C9 . . . . 52.4(11) ?
N2 C9 C10 N1 . . . . -55.9(12) ?
C16 C11 C12 C13 . . . . -3.5(15) ?
C17 C11 C12 C13 . . . . -180.0(10) ?
C11 C12 C13 C14 . . . . -0.2(19) ?
C12 C13 C14 C15 . . . . 4(2) ?
C12 C13 C14 Br1 . . . . -180.0(9) ?
C13 C14 C15 C16 . . . . -4(2) ?
Br1 C14 C15 C16 . . . . 179.6(11) ?
C14 C15 C16 C11 . . . . 1(2) ?
C12 C11 C16 C15 . . . . 3.2(17) ?
C17 C11 C16 C15 . . . . 179.7(11) ?
C12 C11 C17 O1 . . . . 173.4(10) ?
C16 C11 C17 O1 . . . . -3.0(15) ?
C12 C11 C17 O2 . . . . -5.8(15) ?
C16 C11 C17 O2 . . . . 177.8(10) ?

_cod_database_fobs_code 2244164