#------------------------------------------------------------------------------
#$Date: 2022-09-23 03:06:54 +0100 (Fri, 23 Sep 2022) $
#$Revision: 278104 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244176.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_2244176
loop_
_publ_author_name
Vinaya
'Basavaraju, Yeriyur B.'
'Lakshmana, Beliyaiah'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
 Syntheses and crystal structures of benzyl
 <i>N</i>'-[(<i>E</i>)-2-hydroxybenzylidene]hydrazinecarboxylate and
 benzyl
 <i>N</i>'-[(<i>E</i>)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
;
_journal_coeditor_code           YK2176
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009100
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C15 H14 N2 O3'
_chemical_formula_sum            'C15 H14 N2 O3'
_chemical_formula_weight         270.28
_chemical_name_systematic
;
Benzyl <i>N</i>'-[(<i>E</i>)-2-hydroxybenzylidene]hydrazinecarboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 96.300(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.5017(12)
_cell_length_b                   14.047(4)
_cell_length_c                   10.567(3)
_cell_measurement_reflns_used    6841
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      74.41
_cell_measurement_theta_min      3.14
_cell_volume                     664.2(3)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>CIFFIX</i> (Parkin, 2013) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7271
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.635
_diffrn_reflns_theta_min         3.146
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.129
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1054 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.04(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2511
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.0531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                2425
_reflns_number_total             2511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2176sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2244176
_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   0.738
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_file
;
   1   0   0 0.13348 0.27974   7
   1   0   0 0.45466 0.28521  11
  -1   0   0 0.11131 0.19544  11
  -2   0   0 83.7500 4.33200   5
   2   0   0 78.2177 3.54241   7
   2   0   0 83.4202 3.43848   7
   2   0   0 83.5260 3.90793  11
   3   0   0 0.59898 0.93928  11
  -3   0   0 -0.1853 1.10383   5
   4   0   0 38.8545 2.65843   6
  -4   0   0 49.1963 4.75687  12
  -4   0   0 44.9839 3.56785   8
  -5   0   0 0.80102 1.24992  12
  -5   0   0 0.07827 0.82372   8
   0  -1   0 2332.15 94.3425   1
   0   1   0 2218.59 93.9210   1
  -1   1   0 1362.83 56.5745   5
   1   1   0 1416.30 57.1782  11
   1   1   0 1419.82 56.9355   7
  -2  -1   0 293.421 12.6759   5
   2  -1   0 289.230 12.1849  11
   2  -1   0 286.191 11.9158   7
   2   1   0 286.779 12.3612  11
   2   1   0 276.221 26.3855   2
   2   1   0 290.546 11.7405   7
  -2   1   0 287.204 13.0916   5
   2   1   0 302.207 11.7303   7
  -3  -1   0 38.6100 3.39768   5
   3  -1   0 39.5882 3.08621  11
   3  -1   0 37.0838 2.12801   6
   3   1   0 35.8544 2.76233  11
   3   1   0 34.0430 1.92183   6
  -3   1   0 39.7885 3.26784   5
   4  -1   0 133.440 6.29371   6
  -4  -1   0 132.916 8.16165  12
  -4  -1   0 137.025 7.29839   8
  -4   1   0 137.994 8.20930  12
  -4   1   0 138.155 7.19482   8
   4   1   0 131.126 6.24820   6
  -5  -1   0 27.7602 2.32425   8
  -5  -1   0 24.5942 2.98920  12
  -5   1   0 28.1395 3.10175  12
  -5   1   0 28.4021 2.30781   8
   0  -2   0 0.21530 0.18325   7
   0   2   0 0.09864 0.14414   7
  -1  -2   0 1247.11 49.5671  11
   1  -2   0 1201.12 50.4940   7
  -1  -2   0 1248.89 50.8956   5
   1   2   0 1257.00 49.6849   7
  -1   2   0 1253.31 50.2768   7
  -1   2   0 1198.40 50.5759   5
   1   2   0 1243.28 50.8202  11
  -2  -2   0 258.607 11.1630   5
   2  -2   0 252.153 10.5648  11
   2   2   0 236.170 10.6369  11
  -2   2   0 241.123 10.6682   5
  -3  -2   0 336.798 15.6209   5
  -3   2   0 334.277 15.4501   5
   4  -2   0 76.1135 4.07084   6
  -4  -2   0 79.8768 5.95809  12
  -4  -2   0 84.3940 5.20715   8
  -4   2   0 83.6279 6.05764  12
  -4   2   0 80.2821 4.92914   8
   4   2   0 78.8821 4.06212   6
  -5  -2   0 9.78238 1.88298  12
  -5   2   0 10.2442 1.44178   8
  -5   2   0 10.2277 1.79126  12
   0  -3   0 544.593 22.3989   7
   1  -3   0 7809.61 341.212   1
  -1  -3   0 8813.88 353.920   1
   1  -3   0 8386.06 344.580   1
  -1  -3   0 8005.50 353.468   1
   1   3   0 8476.84 355.258   1
  -1   3   0 8321.14 343.178   1
   1   3   0 8790.12 328.913   1
   2  -3   0 819.741 34.4386  11
  -2  -3   0 836.349 35.0275   5
   2  -3   0 839.995 34.1950   7
   2   3   0 785.684 34.7383  11
   2   3   0 905.054 56.4593   2
  -3  -3   0 8.11083 1.71871   5
   3  -3   0 7.78619 1.06669   6
   3   3   0 7.26537 0.79301   6
  -4  -3   0 28.2403 3.83864  12
   4  -3   0 27.5838 2.06395   6
  -4  -3   0 29.7223 3.21109   8
   4   3   0 27.5499 1.98892   6
  -4   3   0 29.1094 2.90887   8
  -4   3   0 32.5514 4.05106  12
  -5  -3   0 23.2099 2.07075   8
  -5  -3   0 13.2755 3.29968  12
  -5   3   0 17.7469 2.17213   8
   0  -4   0 18.4832 0.99897  11
   0  -4   0 19.6450 1.42123   7
   0   4   0 21.6564 3.66647   2
  -1  -4   0 586.643 24.4373  11
  -1  -4   0 583.189 24.5197   7
  -1  -4   0 610.932 24.6573   5
   1  -4   0 587.290 24.4068   7
   1  -4   0 591.881 24.3486  11
   2  -4   0 1038.43 39.8678   7
   2  -4   0 1021.46 39.9927  11
  -2  -4   0 1043.09 40.8480   5
   2  -4   0 842.992 39.7734   6
   2   4   0 936.316 40.8121   6
   3  -4   0 25.4515 1.88834   6
  -3  -4   0 27.4855 3.12148   5
  -3  -4   0 24.5500 3.88939  12
  -3   4   0 24.1354 4.01114  12
   3   4   0 25.4443 1.53191   6
  -3   4   0 27.3977 3.87575   8
  -4  -4   0 17.5963 2.74185   8
   4  -4   0 15.9963 1.90641   6
  -4  -4   0 17.6760 3.03971  12
   4   4   0 14.2792 1.53719   6
  -4   4   0 18.3890 2.49049   8
  -4   4   0 13.6081 2.60618  12
  -5  -4   0 181.289 8.83986  12
  -5  -4   0 174.001 8.37687   8
  -5   4   0 181.182 8.43877  12
  -5   4   0 184.883 8.06440   8
   0  -5   0 42.6498 2.59561   7
  -1  -5   0 1209.48 51.1541   7
   1  -5   0 1224.04 50.7479  11
   1  -5   0 1186.53 50.9340   7
  -1  -5   0 1202.04 51.2071   5
   1   5   0 1381.44 66.9192   2
  -2  -5   0 233.424 10.5437   5
   2  -5   0 190.312 9.24723   6
   2  -5   0 218.908 9.65849  11
   2  -5   0 231.960 9.71994   7
   2   5   0 217.682 9.39946   6
  -3  -5   0 64.2452 7.62717  12
   3  -5   0 67.1321 3.44838   6
  -3  -5   0 51.0401 6.98945   5
  -3   5   0 64.3798 5.97543  12
   3   5   0 62.0797 3.19070   6
  -3   5   0 69.4673 4.19149   8
  -4  -5   0 81.2986 6.14278  12
  -4  -5   0 88.3214 5.30378   8
   4  -5   0 83.9228 4.32696   6
  -4   5   0 83.8683 5.62885  12
   4   5   0 87.8335 4.26911   6
  -4   5   0 88.5409 4.99177   8
  -5  -5   0 79.4001 4.57691  12
  -5  -5   0 73.7729 4.89430   8
  -5   5   0 74.0566 3.73664   8
  -5   5   0 77.9723 3.96093  12
   0  -6   0 173.216 7.49510  11
   0  -6   0 174.913 8.69418   7
   1  -6   0 478.213 20.4334   7
  -1  -6   0 479.705 20.8571   7
   1  -6   0 467.535 20.3068  11
  -1  -6   0 468.398 20.7836   5
   1   6   0 522.412 34.7941   2
  -2  -6   0 543.970 23.7712   5
   2  -6   0 558.955 22.6132   6
   2  -6   0 514.064 22.6458  11
   2  -6   0 541.751 22.9432   7
   2   6   0 524.293 22.6592   6
  -3  -6   0 60.9744 5.32425  12
  -3  -6   0 66.9080 5.33124   5
   3  -6   0 64.3161 3.44712   6
  -3   6   0 63.7169 3.94209   8
   3   6   0 61.2118 3.25090   6
  -3   6   0 62.0373 4.71382  12
  -4  -6   0 132.574 7.84442  12
  -4  -6   0 130.343 7.28806   8
   4  -6   0 125.682 6.10078   6
   4   6   0 126.818 5.99029   6
  -4   6   0 129.887 7.04117  12
  -4   6   0 129.470 6.47594   8
  -5  -6   0 6.82918 1.69123   8
  -5  -6   0 5.48089 1.36612  12
  -5   6   0 6.17851 0.89323  12
  -5   6   0 5.37296 0.80737   8
   0  -7   0 19.9685 1.25357  11
   0  -7   0 17.6040 1.65127   6
   0  -7   0 19.1243 2.23169   7
   0   7   0 17.3375 1.20683   6
  -1  -7   0 92.7815 5.19613   5
  -1  -7   0 89.3506 5.37776   7
   1  -7   0 90.8797 4.43325  11
   1  -7   0 93.8918 4.40801   6
   1  -7   0 96.2005 5.10222   7
   1   7   0 90.2737 4.19587   6
   2  -7   0 99.2674 5.44360   7
   2  -7   0 94.6199 4.59913   6
  -2  -7   0 91.8924 5.98644   5
   2   7   0 90.9291 4.38272   6
   3  -7   0 137.042 6.43748  13
  -3  -7   0 143.020 7.28090   4
  -3  -7   0 144.344 9.09906   5
   3  -7   0 146.738 6.51518   6
  -3  -7   0 141.076 8.45356  12
   3   7   0 127.233 6.25528  13
  -3   7   0 138.338 6.72631   8
  -3   7   0 118.094 6.97938  12
   3   7   0 141.211 6.36219   6
   4  -7   0 40.8842 2.61038   6
  -4  -7   0 44.7290 4.32324  12
  -4  -7   0 35.7596 3.54287   8
   4   7   0 36.1682 2.38388  13
  -4   7   0 43.8294 3.23358  12
   4   7   0 42.8859 2.54644   6
  -4   7   0 43.9144 2.75135   8
  -5  -7   0 2.04270 1.42193  12
  -5   7   0 1.61605 0.46827  12
  -5   7   0 1.26575 0.38909   8
   0  -8   0 41.4333 2.82681   5
   0  -8   0 40.9306 3.34382   7
   0  -8   0 36.7927 2.89742   6
   0  -8   0 40.7931 2.25189  11
   0   8   0 41.8576 2.18150   6
  -1  -8   0 67.3256 4.82495   7
   1  -8   0 61.4187 3.65365  11
   1  -8   0 63.3272 3.84788   5
   1  -8   0 67.4003 4.79114   7
  -1  -8   0 80.8959 6.07507   5
   1   8   0 73.0907 3.73809   6
   2  -8   0 93.9679 4.58048   6
   2  -8   0 81.8747 5.46713   7
  -2  -8   0 83.0351 5.92845   5
   2   8   0 87.7696 4.18661   6
   3  -8   0 492.156 19.9963   6
   3  -8   0 483.319 20.0984  13
  -3  -8   0 460.927 22.7805   5
   3  -8   0 460.655 20.2738   9
   3   8   0 434.127 20.1630  13
   3   8   0 445.140 20.4426   9
   3   8   0 471.533 19.7210   6
  -3   8   0 529.785 20.7958   8
   4  -8   0 101.357 4.98087  13
  -4  -8   0 106.799 6.50793  12
  -4  -8   0 95.0820 6.46246   8
   4   8   0 103.611 4.74831  13
  -4   8   0 103.795 5.12508  12
  -4   8   0 102.194 4.89524   8
   0  -9   0 177.314 9.65468   6
   0  -9   0 219.861 10.0008   5
   0  -9   0 220.814 10.9096   7
   0  -9   0 223.287 9.29830  11
   0   9   0 212.953 9.09864   6
  -1  -9   0 309.227 14.8046   5
   1  -9   0 319.645 14.8579   7
   1  -9   0 308.542 13.7029   6
  -1  -9   0 304.306 15.4599   7
   1   9   0 320.809 13.4018   6
  -2  -9   0 296.972 14.9845   5
  -2  -9   0 316.617 14.4421   4
   2  -9   0 264.086 14.1917   7
   2  -9   0 305.496 12.8766   6
  -2   9   0 277.221 12.7787  12
  -2   9   0 278.822 12.5342   8
   2   9   0 299.585 12.4781   6
  -3  -9   0 30.2864 3.22541   4
  -3  -9   0 26.1477 3.81657  12
   3  -9   0 33.5181 2.60194   6
   3  -9   0 25.0716 2.90355   9
   3  -9   0 30.9490 2.43021  13
   3   9   0 29.9094 2.28828   6
  -3   9   0 31.5625 2.25176  12
  -3   9   0 29.4924 2.01822   8
   3   9   0 29.6084 1.99778  13
   3   9   0 24.2915 2.19588   9
  -4  -9   0 53.1056 4.30143  12
   4  -9   0 52.0682 3.25325   6
  -4   9   0 56.7174 3.36689   8
  -4   9   0 53.1633 2.99796  12
   4   9   0 56.7230 2.98769   6
   4   9   0 48.7933 2.97553   9
   0 -10   0 361.774 16.8191   7
   0 -10   0 319.524 16.2220   6
   0 -10   0 354.600 15.7376   5
   1 -10   0 87.1772 5.22483   6
   1 -10   0 93.5556 5.41882   9
   1 -10   0 93.0531 5.05476  13
  -1 -10   0 90.8225 6.72306   4
   1 -10   0 93.1442 6.93823   7
  -1 -10   0 93.7902 6.13420   5
   1  10   0 93.2646 4.56225   6
   1  10   0 93.8650 4.53624   9
   1  10   0 93.2547 4.30560  13
   2 -10   0 478.476 19.6181   6
   2 -10   0 458.737 19.5640   9
  -2 -10   0 480.059 21.1284   4
  -2 -10   0 441.523 22.3219   5
   2 -10   0 448.183 19.3517  13
   2  10   0 458.436 18.9712   6
  -2  10   0 431.015 19.3775  12
   2  10   0 450.940 19.6495   9
   2  10   0 449.161 19.3417  13
  -3 -10   0 49.9859 4.25061   4
   3 -10   0 56.6333 3.66035   6
  -3 -10   0 49.8179 5.02089  12
   3 -10   0 50.7652 3.88467   9
   3 -10   0 58.1228 3.38453  13
  -3  10   0 50.0911 2.84907   8
   3  10   0 55.3678 2.91026  13
   3  10   0 51.7441 3.15006   9
   3  10   0 56.3635 3.12995   6
   4 -10   0 26.7366 2.26156  13
   4 -10   0 22.5615 2.43444   9
  -4 -10   0 23.5338 3.74849  12
   4  10   0 31.0018 1.84405  13
   4  10   0 35.2509 2.90444   6
   4  10   0 30.3950 2.04511   9
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   3   6   2 62.6445 4.06170   9
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   4   6   2 157.674 7.72773   9
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   4   1   3 55.1543 3.19591   6
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   4   4   3 21.4397 1.98781   6
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   2   5   3 1271.97 51.9622   6
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   4   5   3 124.734 6.15100   9
   4   5   3 133.213 6.20653   6
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   4   5   3 119.212 7.96038   3
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   4   6  -3 65.5180 3.21690   6
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   3   7   3 582.834 25.0848   6
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   4   7   3 69.6401 3.60918   6
   4   7   3 65.3255 3.83549   3
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   4   8  -3 17.8106 1.44663   6
   4   8  -3 20.3284 1.48653  13
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   3   8  -3 173.762 7.50308   6
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   3   7   5 77.3934 4.53259   3
   3   7   5 76.0087 4.17074   6
   3   7   5 67.9346 4.12922   9
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   2   9   5 6.49135 1.26053   3
   2   9   5 7.19794 1.03464  13
   2   9   5 5.00817 1.29497   6
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   3   9   5 30.1122 2.24976   9
   3   9   5 34.6815 2.33745   6
   3   9   5 30.5183 2.42026   3
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   2   0   6 18.0050 2.08406   6
   2   0   6 20.0001 2.28603   3
   3   0   6 0.88554 0.85144   3
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   3   0   6 0.51705 0.97363   9
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   1   1   6 10.6442 1.53390   6
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   2  -1   6 17.1933 2.82067   3
   2   1   6 18.8634 2.10048   6
   2   1   6 16.0751 2.05174   3
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   3  -1   6 13.7041 1.86333   3
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   3  -1   6 14.8315 2.52578   6
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   3   1   6 14.3669 2.06506   9
   3   1   6 13.6585 1.92085   3
   3   1   6 13.7945 1.68603  13
   3   1   6 12.3451 2.05799   6
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   4  -1   6 20.3125 1.72138   6
   4   1   6 19.2596 1.74074   6
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   4   1   6 22.2760 1.59908  13
   4   1   6 17.1770 1.88000   3
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   3  -2  -6 486.955 19.5874   6
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   3   2  -6 476.108 19.6413   6
   2  -2  -6 12.7647 2.27407   7
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   2  -2  -6 8.79537 1.30637   6
   2   2  -6 9.15843 1.39116   6
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   0   2  -6 67.6383 3.94050   6
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   1  -2   6 297.781 13.0371   3
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   2   2   6 39.5344 3.20639   9
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   2   2   6 45.6132 3.19272   3
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   4   2   6 84.4939 4.47339   3
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   4   2   6 94.6187 4.69309   9
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   3   3   6 15.0044 1.89074   3
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   2   4   6 20.0453 2.15872   6
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   3   4   6 18.7448 2.11637   3
   3   4   6 18.1000 2.00591   6
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   4  -4   6 6.37201 0.94556   9
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   4   4   6 5.41806 0.90181   6
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   4   4   6 6.65170 1.08283   9
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   3   5  -6 32.2355 2.34075   6
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   1   5   6 52.3833 3.19898   6
   1   5   6 51.0390 4.08409   9
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   2   5   6 23.4266 2.41325   3
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   4  -5   6 25.1015 1.54636  13
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   4   5   6 18.9924 1.63651   3
   4   5   6 23.1872 1.47793  13
   4   5   6 22.6779 1.57965   9
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   2   6   6 333.363 15.1724   9
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   1   7   6 63.5676 3.90353   3
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   1   7   6 62.8944 3.43388  13
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   2  -7   6 42.5966 2.90370   6
   2  -7   6 40.1400 2.84814   9
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   2   7   6 39.4877 3.08069   3
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   2   7   6 39.0428 2.90558   6
   2   7   6 41.8343 2.90216   9
   3  -7   6 27.5837 2.23105   9
   3  -7   6 27.5758 2.01320  13
   3  -7   6 26.8008 2.48550   6
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   3   7   6 27.9583 2.18380   9
   3   7   6 27.0625 2.56638   3
   3   7   6 30.7487 2.89542   6
   3   7   6 27.4195 1.93566  13
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   4  -7   6 3.68495 0.73530   9
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   4   7   6 3.52200 0.61985   9
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   3   8  -6 22.9314 1.92503   9
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   1   8  -6 39.4960 2.55457   9
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   0   8   6 19.5924 2.43262   9
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   0   8  -6 25.1018 1.58268  13
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   1   8   6 86.1280 4.21776  13
   1   8   6 82.6032 4.62465   9
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   1   8   6 87.1118 4.85221   3
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   2  -8   6 76.0476 4.29892   6
   2  -8   6 79.8861 4.28162   9
   2   8   6 75.6834 3.93493  13
   2   8   6 80.3077 4.37896   6
   2   8   6 74.6412 4.28219   9
   3  -8   6 24.1349 2.13564   6
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   3  -8   6 27.3384 1.87172  13
   3  -8   6 26.4016 2.14234   9
   3   8   6 27.4892 1.81983  13
   3   8   6 27.4292 2.19611   3
   3   8   6 26.0526 2.04998   9
   3   8   6 24.3970 2.11319   6
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   4  -8   6 3.12373 0.63716   9
   4   8   6 3.24330 0.51008   9
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   4   9  -6 3.06633 0.46618  13
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   3   9  -6 8.40958 1.06968  13
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   3   9  -6 8.22982 1.06272   6
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   2  -9  -6 280.055 14.3904   6
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   2   9  -6 259.285 11.3887   6
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   2   9  -6 235.136 10.5448   9
   1  -9  -6 336.559 16.2149   6
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   1   9  -6 336.714 14.6005   6
   1   9  -6 339.879 14.6542   9
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   1  -9   6 2.78909 1.61828   4
   1   9   6 6.03815 1.16914   9
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   2  -9   6 78.4401 4.25008   9
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   2  -9   6 76.0634 3.89606  13
   2   9   6 81.3355 3.92967  13
   2   9   6 77.2998 4.26257   9
   2   9   6 74.5637 4.41349   6
   2   9   6 83.7849 4.56793   3
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   3  -9   6 13.2333 1.61464   9
   3  -9   6 13.2742 1.93330  13
   3   9   6 12.4792 1.49415   3
   3   9   6 12.0128 1.61441  13
   3   9   6 13.1587 1.49381   9
   3 -10  -6 8.13407 1.67684   6
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   3  10  -6 5.94700 0.87342   9
   3  10  -6 7.30829 0.98409   6
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   2  -2   8 298.480 13.0959   9
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   2   2   8 293.201 12.7403  13
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   2   9   9 14.7268 1.42981   3
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   0 -11   9 3.12035 1.07107   4
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   2   2 -11 25.3116 2.34296   6
   2   2 -11 24.0882 3.21616   9
   2   2 -11 24.8986 2.07002  13
   1  -2 -11 33.3060 2.68625  13
   1  -2 -11 31.4529 3.02430   9
   1  -2 -11 41.7189 4.97074   6
   1   2 -11 31.3454 3.58572   6
  -1   2  11 31.9625 2.28150   3
   1   2 -11 27.0886 2.60774   9
   1   2 -11 32.8115 2.35459  13
   0  -2  11 244.327 11.5496   3
   0  -2 -11 253.000 11.7790   9
   0  -2 -11 252.997 10.9008  13
   0   2 -11 258.183 11.0795   9
   0   2 -11 248.136 10.8631  13
   0   2  11 253.023 11.3148   3
   1  -2  11 17.8432 1.70057   3
  -1  -2 -11 14.8874 2.83128   4
   1   2  11 18.2508 1.70475   3
  -1   2 -11 14.2364 2.34260   4
  -2  -2 -11 39.5375 2.80507   4
   2  -2  11 36.0558 2.23614   3
   2   2  11 37.5794 2.17777   3
  -2   2 -11 35.4630 2.38610   4
   3  -3 -11 72.3880 3.59112  13
   3   3 -11 77.7401 3.33854  13
  -3   3  11 72.5803 4.34979  10
   2  -3 -11 60.6726 4.12865   6
   2  -3 -11 58.2848 3.92371   9
   2  -3 -11 61.2683 3.74866  13
   2   3 -11 59.9452 3.23352  13
   2   3 -11 56.8995 3.56931   6
   2   3 -11 58.8568 3.37075   9
  -2   3  11 61.8205 3.73190  10
   1  -3 -11 25.5963 2.65182   9
   1  -3 -11 26.4200 2.46277  13
   1  -3 -11 26.7847 2.88696   6
   1   3 -11 25.4470 2.23640   9
   1   3 -11 25.3873 2.43260   6
   1   3 -11 26.6846 1.99115  13
  -1   3  11 23.5099 2.00239   3
   0  -3 -11 70.7736 3.65488  13
   0  -3  11 67.8008 4.11868   3
   0  -3 -11 69.8276 4.29727   9
   0   3 -11 69.6838 3.84729   9
   0   3  11 68.8354 3.81174   3
   0   3 -11 69.8838 3.32881  13
  -1  -3 -11 5.92424 1.61554   4
  -1  -3 -11 7.22527 1.06461   9
   1  -3  11 7.80447 1.23977   3
  -1   3 -11 6.80705 1.38187   4
  -1   3 -11 6.74871 0.90048   9
   1   3  11 8.57156 1.25018   3
  -2  -3 -11 33.4550 2.67517   4
   2   3  11 32.7034 1.98602   3
  -2   3 -11 32.9371 2.32225   4
   3  -4 -11 22.2568 1.67936  13
   3   4 -11 23.9161 1.30496  13
  -3   4  11 21.4468 1.69994  10
   2  -4 -11 168.948 8.47021   6
   2  -4 -11 164.605 8.13262   9
   2   4 -11 171.425 7.52796   9
   2   4 -11 164.475 7.70288   6
  -2   4  11 172.606 8.04614  10
   1  -4 -11 19.8962 2.44577   9
   1  -4 -11 18.0047 2.24472  13
   1  -4 -11 19.6158 2.59966   6
   1   4 -11 17.9939 1.73426   9
   1   4 -11 17.1907 1.91626   6
   1   4 -11 16.0676 1.56762  13
   0  -4  11 4.24867 1.13163   3
   0  -4 -11 5.49600 1.35301   9
   0  -4 -11 4.29554 0.91229  13
   0   4 -11 4.88826 0.60908  13
   0   4  11 5.25504 1.00339   3
   0   4 -11 2.81141 0.79317   9
   1  -4  11 86.6975 4.39005   3
  -1  -4 -11 82.7811 5.34673   4
  -1  -4 -11 91.0071 4.13350   9
   1   4  11 84.9262 4.27676   3
  -1   4 -11 83.0589 3.76531   9
  -1   4 -11 79.1947 4.55110   4
  -2  -4 -11 13.0260 1.71195   4
  -2   4 -11 10.5511 1.10047   4
   2   4  11 8.70507 1.30907   3
   3  -5 -11 29.0065 1.97500  13
   3   5 -11 29.0717 1.48140  13
  -3   5  11 28.8426 1.97690  10
   2  -5 -11 110.246 5.39470  13
   2  -5 -11 102.662 5.98971   6
   2  -5 -11 109.551 5.58076   9
   2   5 -11 102.641 4.84611   9
   2   5 -11 96.4148 5.20263   6
   2   5 -11 104.599 4.68522  13
  -2   5  11 111.807 5.84092  10
   1  -5 -11 10.4566 1.54680  13
   1  -5 -11 9.33364 1.88199   6
   1  -5 -11 13.4317 2.08166   9
  -1  -5  11 9.60961 1.41189   4
   1   5 -11 11.5293 1.20338  13
   1   5 -11 10.9680 1.34025   9
   1   5 -11 10.4691 1.55129   6
   0  -5 -11 15.1950 2.19642   9
   0   5 -11 13.6218 1.34117   9
   0   5  11 12.4550 1.75382   3
  -1  -5 -11 25.4621 2.55131   9
   1  -5  11 26.3560 1.88030   3
  -1  -5 -11 31.5980 3.07017   4
   1   5  11 26.5587 1.84406   3
  -1   5 -11 24.1899 2.05695   4
  -1   5 -11 23.7385 1.73526   9
  -2  -5 -11 14.0177 1.71820   4
   2  -6 -11 70.9193 3.98378   9
   2  -6 -11 71.0970 3.86844  13
   2   6 -11 68.5324 3.30610   9
   2   6 -11 70.7508 3.23228  13
  -2   6  11 69.8838 3.93593  10
   1  -6 -11 113.640 5.57739  13
  -1  -6  11 84.9641 5.78414   4
   1  -6 -11 103.231 6.15229   6
   1  -6 -11 123.405 6.55649   9
   1   6 -11 97.4565 5.04473   6
   1   6 -11 103.739 4.88414  13
   1   6 -11 108.072 5.03099   9
   0  -6 -11 34.9073 3.94055   9
   0  -6 -11 28.9532 1.84338  13
   0   6  11 25.4456 1.87102   3
   0   6 -11 30.3587 2.27722   9
   0   6 -11 26.2998 1.38432  13
  -1  -6 -11 1.75467 1.17018   4
   1   6  11 0.01293 0.59320   3
   2  -7 -11 19.4895 2.93327   9
   2  -7 -11 18.1768 1.81128  13
   2   7 -11 19.7291 1.11290  13
   2   7 -11 17.7564 1.62206   9
  -2   7  11 20.5345 2.38666  10
   1  -7 -11 108.186 5.57754   9
   1  -7 -11 106.474 5.13617  13
  -1  -7  11 98.5671 4.93885   4
   1   7 -11 102.054 4.60423   9
   1   7 -11 101.346 4.41918  13
   0  -7 -11 13.9560 1.82416   9
   0  -7  11 13.4558 1.52227   4
   0   7 -11 13.9872 1.05755   9
   1  -7  11 8.28058 1.46874   4
  -1  -7 -11 12.4021 2.23551   4
   2  -8 -11 22.5604 1.80660  13
   2  -8 -11 22.6151 2.02002   9
   2   8 -11 22.4752 1.11256  13
   2   8 -11 22.1557 1.24612   9
  -1  -8  11 138.765 6.38362   4
   1  -8 -11 139.326 6.49188   9
   1  -8 -11 138.617 6.10066  13
   1   8 -11 133.497 5.88048  13
   1   8 -11 138.739 6.06646   9
   0  -8 -11 50.4688 2.93921   9
   0  -8  11 49.0961 2.81144   4
   0   8 -11 48.3066 2.32265   9
   1  -8  11 17.1754 1.44624   4
   1  -9 -11 67.6994 3.82347   9
   1   9 -11 61.3103 2.85506   9
   0  -9  11 20.6400 1.73711   4
   0  -9 -11 22.4179 2.04606   9
   0   9 -11 19.0669 1.13655   9
   2   0 -12 62.4857 3.24888  13
   2   0 -12 63.5316 3.37649   9
   1   0 -12 0.93258 0.86418   9
   1   0 -12 0.70108 0.82112  13
   0   0 -12 53.5795 2.60752  13
   0   0  12 60.3698 3.44528   3
   0   0 -12 56.9186 3.20971   9
   1   0  12 -0.0815 0.47973   3
  -1   0 -12 0.49311 0.87981   4
   2  -1 -12 13.4796 1.47113  13
   2  -1 -12 11.9513 1.52792   9
   2   1 -12 11.9506 1.37625   9
   2   1 -12 14.7085 1.34981  13
   1  -1 -12 24.0816 2.12887   9
   1  -1 -12 27.1608 2.41692  13
   1   1 -12 26.3182 2.08680   9
   1   1 -12 24.7357 2.21072  13
   0  -1 -12 32.9963 2.27403   9
   0  -1  12 34.2541 2.33436   3
   0  -1 -12 27.7766 1.73840  13
   0   1 -12 32.7497 2.12243   9
   0   1  12 35.2514 2.34460   3
   0   1 -12 28.5135 1.62719  13
  -1  -1 -12 62.3410 3.64368   4
   1  -1  12 60.4908 3.20517   3
  -1   1 -12 61.5454 3.50852   4
   1   1  12 59.5901 3.13517   3
   2  -2 -12 16.1633 1.48780  13
   2  -2 -12 15.7730 1.63601   9
   2   2 -12 15.4275 1.25946  13
   2   2 -12 15.0618 1.34910   9
   1  -2 -12 63.9043 3.31687  13
   1  -2 -12 61.4553 3.56954   9
   1   2 -12 62.8303 3.32349   9
   1   2 -12 61.3984 3.13285  13
   0  -2 -12 33.3370 2.14170  13
   0  -2 -12 37.9868 2.43803   9
   0   2  12 33.9132 2.19888   3
   0   2 -12 37.9578 2.19707   9
  -1  -2 -12 5.50937 1.16486   4
   1  -2  12 3.40600 0.75286   3
   1   2  12 3.38342 0.72835   3
  -1   2 -12 4.59575 0.94160   4
   2  -3 -12 13.8231 1.57326   9
   2  -3 -12 12.7968 1.37879  13
   2   3 -12 13.9761 1.24284   9
   2   3 -12 12.7435 1.07216  13
   1  -3 -12 49.6154 3.06934   9
   1  -3 -12 51.3950 2.82928  13
   1   3 -12 49.9370 2.75523   9
   1   3 -12 49.5789 2.51474  13
   0  -3 -12 69.2768 3.65691   9
   0   3 -12 66.7762 3.34034   9
   0   3  12 70.4949 3.51988   3
  -1  -3 -12 103.986 7.21511   4
   1  -3  12 124.924 5.56719   3
   1   3  12 122.048 5.59456   3
  -1   3 -12 110.820 5.91554   4
   2  -4 -12 30.3003 1.96527   9
   2  -4 -12 31.0848 2.00275  13
   2   4 -12 29.9571 1.63211   9
   2   4 -12 30.0567 1.57731  13
   1  -4 -12 8.21224 1.28392   9
  -1  -4  12 6.41370 0.92170   4
   1  -4 -12 6.42714 0.92792  13
   1   4 -12 6.90581 0.81203  13
   1   4 -12 6.44015 0.94901   9
   0  -4 -12 80.6436 3.85758   9
   0   4 -12 75.7784 3.47128   9
   0   4  12 69.7895 3.80429   3
   2  -5 -12 25.7200 1.71027   9
   2  -5 -12 27.6019 1.66815  13
   2   5 -12 25.9993 1.31318  13
   2   5 -12 26.8437 1.40136   9
   1  -5 -12 11.7276 1.28537  13
   1  -5 -12 12.6160 1.55102   9
   1   5 -12 12.5750 1.01528   9
   1   5 -12 11.1192 0.82064  13
   0  -5  12 53.7343 2.96164   4
   0  -5 -12 56.4428 2.93812   9
   0   5 -12 55.9564 2.59033   9
   1  -5  12 58.6269 2.95065   4
   1  -6 -12 61.4940 3.37149   9
   1  -6 -12 56.1782 2.65969  13
   1   6 -12 52.9180 2.44890  13
   1   6 -12 55.9402 2.78523   9
   0  -6 -12 60.5550 2.93930   9
   0  -6  12 63.0974 3.63190   4
   0   6 -12 60.6105 2.81762   9
   1  -7 -12 18.5133 1.57104   9
   1   7 -12 18.0959 1.06166   9
   0  -7  12 22.0609 1.43553   4
   1   0 -13 59.4245 2.80885   9
   1   0 -13 59.3005 2.70386  13
   0   0 -13 0.41852 0.32165   9
   1  -1 -13 34.2680 1.87109   9
   1  -1 -13 34.2317 1.86674  13
   1   1 -13 34.2399 1.86307   9
   0  -1 -13 56.5561 2.68106   9
   0   1 -13 54.0690 2.54940   9
   1  -2 -13 21.3401 1.45305   9
   1   2 -13 20.9910 1.28678   9
   0   0   0    0.00    0.00   0
;
_shelx_hkl_checksum              45189
_shelx_res_file
;
TITL c22010  - space group Pn
    c22010.res
    created by SHELXL-2019/2 at 09:06:19 on 26-Aug-2022
CELL  1.54184   4.5017  14.0470  10.5671   90.000   96.300   90.000
ZERR        2   0.0012   0.0041   0.0034    0.000    0.015    0.000
LATT -1
SYMM 1/2+X, -Y, 1/2+Z
SFAC C H N O
UNIT 30  28  4  6
TEMP -183
SIZE 0.41 0.23 0.015
REM FORM plate
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds
HTAB O1 N1
EQIV $1 x-1/2, -y+1, z+1/2
HTAB N2 O1_$1
EQIV $2 x+1/2, -y+1, z+1/2
HTAB C7 O3_$2
HTAB
REM Various planes for r.m.s. deviations and dihedrals:
MPLA C1 C2 C3 C4 C5 C6 C7 N1 N2 C8 O2 O3
MPLA C9 C10 C11 C12 C13 C14 C15
REM Various torsions:
RTAB tors C8 O2 C9 C10
RTAB tors O2 C9 C10 C11
FMAP 2
PLAN 20
REM EXTI    0.000624, SU = 0.0008 : not significant
WGHT    0.028300    0.053100
FVAR       1.13119
O1    4    0.752487    0.443874    0.346493    11.00000    0.03685    0.03125 =
         0.01377    0.00202    0.00897    0.00583
H1O   2    0.630541    0.478614    0.391105    11.00000   -1.50000
O2    4   -0.040671    0.675352    0.569974    11.00000    0.02685    0.02667 =
         0.02015    0.00221    0.00656    0.00455
O3    4    0.202102    0.642425    0.397800    11.00000    0.03171    0.02923 =
         0.01367    0.00075    0.00395    0.00053
N1    3    0.468779    0.494951    0.530760    11.00000    0.02354    0.02420 =
         0.01321   -0.00190    0.00409    0.00055
N2    3    0.272787    0.554768    0.580484    11.00000    0.02590    0.02755 =
         0.01165   -0.00011    0.00645    0.00442
H2N   2    0.242220    0.550835    0.659835    11.00000   -1.20000
C1    1    0.788676    0.361370    0.547514    11.00000    0.02173    0.02506 =
         0.01481   -0.00079    0.00287   -0.00078
C2    1    0.861215    0.370600    0.422167    11.00000    0.02463    0.02622 =
         0.01540   -0.00108    0.00253   -0.00101
C3    1    1.049284    0.304918    0.373109    11.00000    0.03220    0.03381 =
         0.01717   -0.00409    0.00621    0.00148
AFIX  43
H3    2    1.101603    0.312160    0.288959    11.00000   -1.20000
AFIX   0
C4    1    1.160216    0.228823    0.447386    11.00000    0.03037    0.03157 =
         0.02848   -0.00790    0.00528    0.00689
AFIX  43
H4    2    1.284895    0.183155    0.413092    11.00000   -1.20000
AFIX   0
C5    1    1.090695    0.218819    0.571317    11.00000    0.03126    0.02839 =
         0.02645    0.00176    0.00094    0.00612
AFIX  43
H5    2    1.168389    0.166681    0.621816    11.00000   -1.20000
AFIX   0
C6    1    0.908183    0.284858    0.621157    11.00000    0.02676    0.02896 =
         0.01737    0.00113    0.00243    0.00202
AFIX  43
H6    2    0.863234    0.278254    0.706480    11.00000   -1.20000
AFIX   0
C7    1    0.586563    0.427537    0.601233    11.00000    0.02331    0.02690 =
         0.01139    0.00014    0.00345   -0.00039
AFIX  43
H7    2    0.542993    0.420844    0.686734    11.00000   -1.20000
AFIX   0
C8    1    0.150917    0.625823    0.505058    11.00000    0.02124    0.02311 =
         0.01445   -0.00191    0.00186   -0.00209
C9    1   -0.160728    0.760465    0.505457    11.00000    0.02160    0.02785 =
         0.02560    0.00177    0.00092    0.00371
AFIX  23
H9A   2   -0.343944    0.780464    0.542188    11.00000   -1.20000
H9B   2   -0.215620    0.746317    0.414103    11.00000   -1.20000
AFIX   0
C10   1    0.062988    0.839811    0.518596    11.00000    0.01945    0.02524 =
         0.02428   -0.00176    0.00086    0.00634
C11   1    0.169805    0.872559    0.639547    11.00000    0.02535    0.03856 =
         0.02899   -0.00670    0.00099    0.00677
AFIX  43
H11   2    0.100670    0.844554    0.712731    11.00000   -1.20000
AFIX   0
C12   1    0.376347    0.945779    0.653257    11.00000    0.02866    0.03889 =
         0.05033   -0.01868   -0.00675    0.00613
AFIX  43
H12   2    0.448310    0.967698    0.736024    11.00000   -1.20000
AFIX   0
C13   1    0.478663    0.987200    0.548254    11.00000    0.02398    0.02524 =
         0.07415   -0.00343   -0.00389    0.00339
AFIX  43
H13   2    0.619778    1.037661    0.558367    11.00000   -1.20000
AFIX   0
C14   1    0.374202    0.954721    0.427475    11.00000    0.02793    0.03393 =
         0.05518    0.01552    0.00422    0.00390
AFIX  43
H14   2    0.444340    0.982844    0.354578    11.00000   -1.20000
AFIX   0
C15   1    0.167434    0.881217    0.413144    11.00000    0.02507    0.03100 =
         0.02895    0.00528    0.00123    0.00549
AFIX  43
H15   2    0.096956    0.859121    0.330295    11.00000   -1.20000
AFIX   0
HKLF 4
REM  c22010  - space group Pn
REM wR2 = 0.0629, GooF = S = 1.040, Restrained GooF = 1.040 for all data
REM R1 = 0.0242 for 2425 Fo > 4sig(Fo) and 0.0257 for all 2511 data
REM 187 parameters refined using 2 restraints
END
WGHT      0.0283      0.0531
REM Instructions for potential hydrogen bonds
HTAB O1 N1
HTAB N2 O1_$1
HTAB C7 O3_$2
REM Highest difference peak  0.129,  deepest hole -0.129,  1-sigma level  0.031
Q1    1   0.5297  0.5099  0.4675  11.00000  0.05    0.13
Q2    1   0.8014  0.3600  0.4832  11.00000  0.05    0.12
Q3    1   0.9442  0.4476  0.4005  11.00000  0.05    0.12
Q4    1   0.9414  0.3436  0.6044  11.00000  0.05    0.11
Q5    1   0.4053  0.4358  0.5558  11.00000  0.05    0.11
Q6    1  -0.1365  0.6243  0.5149  11.00000  0.05    0.11
Q7    1   0.6431  0.4920  0.5773  11.00000  0.05    0.10
Q8    1   0.0893  0.5576  0.5251  11.00000  0.05    0.10
Q9    1  -0.1958  0.5870  0.6703  11.00000  0.05    0.10
Q10   1  -0.2908  0.7609  0.5729  11.00000  0.05    0.09
Q11   1   1.0164  0.3502  0.4203  11.00000  0.05    0.09
Q12   1   1.3347  0.3876  0.3441  11.00000  0.05    0.09
Q13   1   0.0165  0.6627  0.3109  11.00000  0.05    0.09
Q14   1   1.1554  0.4069  0.5506  11.00000  0.05    0.09
Q15   1   0.1481  0.4931  0.5414  11.00000  0.05    0.09
Q16   1   0.9461  0.3015  0.8137  11.00000  0.05    0.09
Q17   1   1.1167  0.3683  0.5075  11.00000  0.05    0.08
Q18   1  -0.0852  0.6757  0.6625  11.00000  0.05    0.08
Q19   1   0.1444  0.5048  0.6393  11.00000  0.05    0.08
Q20   1   0.8905  0.4186  0.5816  11.00000  0.05    0.08
;
_shelx_res_checksum              19977
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, 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
O O1 0.7525(3) 0.44387(9) 0.34649(11) 0.0268(3) Uani d 1 . .
H H1O 0.631(6) 0.4786(18) 0.391(3) 0.040 Uiso d 1 . .
O O2 -0.0407(3) 0.67535(9) 0.56997(11) 0.0243(3) Uani d 1 . .
O O3 0.2021(3) 0.64243(9) 0.39780(11) 0.0248(3) Uani d 1 . .
N N1 0.4688(3) 0.49495(10) 0.53076(13) 0.0202(3) Uani d 1 . .
N N2 0.2728(3) 0.55477(11) 0.58048(13) 0.0214(3) Uani d 1 . .
H H2N 0.242(5) 0.5508(15) 0.660(2) 0.026 Uiso d 1 . .
C C1 0.7887(3) 0.36137(13) 0.54751(15) 0.0205(3) Uani d 1 . .
C C2 0.8612(4) 0.37060(12) 0.42217(16) 0.0221(4) Uani d 1 . .
C C3 1.0493(4) 0.30492(14) 0.37311(16) 0.0275(4) Uani d 1 . .
H H3 1.101603 0.312160 0.288959 0.033 Uiso calc 1 . .
C C4 1.1602(4) 0.22882(14) 0.44739(19) 0.0300(4) Uani d 1 . .
H H4 1.284895 0.183155 0.413092 0.036 Uiso calc 1 . .
C C5 1.0907(4) 0.21882(14) 0.57132(18) 0.0289(4) Uani d 1 . .
H H5 1.168389 0.166681 0.621816 0.035 Uiso calc 1 . .
C C6 0.9082(4) 0.28486(13) 0.62116(15) 0.0244(4) Uani d 1 . .
H H6 0.863234 0.278254 0.706480 0.029 Uiso calc 1 . .
C C7 0.5866(4) 0.42754(12) 0.60123(15) 0.0204(3) Uani d 1 . .
H H7 0.542993 0.420844 0.686734 0.025 Uiso calc 1 . .
C C8 0.1509(4) 0.62582(12) 0.50506(15) 0.0196(3) Uani d 1 . .
C C9 -0.1607(4) 0.76046(13) 0.50546(17) 0.0251(4) Uani d 1 . .
H H9A -0.343944 0.780464 0.542188 0.030 Uiso calc 1 . .
H H9B -0.215620 0.746317 0.414103 0.030 Uiso calc 1 . .
C C10 0.0630(4) 0.83981(12) 0.51860(17) 0.0231(4) Uani d 1 . .
C C11 0.1698(4) 0.87256(14) 0.63955(19) 0.0311(4) Uani d 1 . .
H H11 0.100670 0.844554 0.712731 0.037 Uiso calc 1 . .
C C12 0.3763(5) 0.94578(15) 0.6533(2) 0.0401(5) Uani d 1 . .
H H12 0.448310 0.967698 0.736024 0.048 Uiso calc 1 . .
C C13 0.4787(5) 0.98720(14) 0.5483(3) 0.0418(6) Uani d 1 . .
H H13 0.619778 1.037661 0.558367 0.050 Uiso calc 1 . .
C C14 0.3742(5) 0.95472(15) 0.4275(2) 0.0390(5) Uani d 1 . .
H H14 0.444340 0.982844 0.354578 0.047 Uiso calc 1 . .
C C15 0.1674(4) 0.88122(13) 0.41314(18) 0.0285(4) Uani d 1 . .
H H15 0.096956 0.859121 0.330295 0.034 Uiso calc 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
O1 0.0369(8) 0.0313(7) 0.0138(5) 0.0058(5) 0.0090(5) 0.0020(5)
O2 0.0269(6) 0.0267(6) 0.0202(6) 0.0045(5) 0.0066(5) 0.0022(5)
O3 0.0317(6) 0.0292(6) 0.0137(5) 0.0005(5) 0.0040(4) 0.0007(5)
N1 0.0235(7) 0.0242(7) 0.0132(6) 0.0005(5) 0.0041(5) -0.0019(5)
N2 0.0259(8) 0.0276(8) 0.0117(6) 0.0044(6) 0.0064(5) -0.0001(5)
C1 0.0217(8) 0.0251(8) 0.0148(7) -0.0008(6) 0.0029(6) -0.0008(6)
C2 0.0246(8) 0.0262(9) 0.0154(7) -0.0010(7) 0.0025(6) -0.0011(7)
C3 0.0322(10) 0.0338(10) 0.0172(8) 0.0015(7) 0.0062(7) -0.0041(7)
C4 0.0304(10) 0.0316(10) 0.0285(9) 0.0069(8) 0.0053(7) -0.0079(8)
C5 0.0313(9) 0.0284(9) 0.0265(9) 0.0061(7) 0.0009(7) 0.0018(7)
C6 0.0268(8) 0.0290(9) 0.0174(8) 0.0020(7) 0.0024(7) 0.0011(6)
C7 0.0233(8) 0.0269(8) 0.0114(7) -0.0004(6) 0.0035(6) 0.0001(6)
C8 0.0212(8) 0.0231(8) 0.0144(8) -0.0021(6) 0.0019(6) -0.0019(6)
C9 0.0216(8) 0.0278(9) 0.0256(8) 0.0037(7) 0.0009(7) 0.0018(7)
C10 0.0194(7) 0.0252(9) 0.0243(8) 0.0063(6) 0.0009(6) -0.0018(7)
C11 0.0254(9) 0.0386(11) 0.0290(9) 0.0068(8) 0.0010(7) -0.0067(8)
C12 0.0287(10) 0.0389(11) 0.0503(13) 0.0061(8) -0.0067(9) -0.0187(9)
C13 0.0240(9) 0.0252(10) 0.0741(16) 0.0034(8) -0.0039(10) -0.0034(10)
C14 0.0279(10) 0.0339(11) 0.0552(12) 0.0039(8) 0.0042(9) 0.0155(10)
C15 0.0251(9) 0.0310(10) 0.0290(9) 0.0055(7) 0.0012(7) 0.0053(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 O1 H1O . . 107.5(17) ?
C8 O2 C9 . . 114.27(13) ?
C7 N1 N2 . . 118.33(14) ?
C8 N2 N1 . . 117.65(14) ?
C8 N2 H2N . . 121.3(14) ?
N1 N2 H2N . . 120.8(15) ?
C6 C1 C2 . . 118.71(16) ?
C6 C1 C7 . . 119.42(15) ?
C2 C1 C7 . . 121.85(15) ?
O1 C2 C3 . . 118.50(16) ?
O1 C2 C1 . . 121.20(16) ?
C3 C2 C1 . . 120.30(16) ?
C4 C3 C2 . . 119.79(17) ?
C4 C3 H3 . . 120.1 ?
C2 C3 H3 . . 120.1 ?
C3 C4 C5 . . 120.55(17) ?
C3 C4 H4 . . 119.7 ?
C5 C4 H4 . . 119.7 ?
C6 C5 C4 . . 119.83(17) ?
C6 C5 H5 . . 120.1 ?
C4 C5 H5 . . 120.1 ?
C5 C6 C1 . . 120.81(16) ?
C5 C6 H6 . . 119.6 ?
C1 C6 H6 . . 119.6 ?
N1 C7 C1 . . 118.70(14) ?
N1 C7 H7 . . 120.7 ?
C1 C7 H7 . . 120.7 ?
O3 C8 O2 . . 125.21(16) ?
O3 C8 N2 . . 126.12(17) ?
O2 C8 N2 . . 108.67(14) ?
O2 C9 C10 . . 110.94(13) ?
O2 C9 H9A . . 109.5 ?
C10 C9 H9A . . 109.5 ?
O2 C9 H9B . . 109.5 ?
C10 C9 H9B . . 109.5 ?
H9A C9 H9B . . 108.0 ?
C15 C10 C11 . . 119.09(18) ?
C15 C10 C9 . . 121.48(16) ?
C11 C10 C9 . . 119.43(17) ?
C12 C11 C10 . . 120.1(2) ?
C12 C11 H11 . . 119.9 ?
C10 C11 H11 . . 119.9 ?
C13 C12 C11 . . 120.7(2) ?
C13 C12 H12 . . 119.7 ?
C11 C12 H12 . . 119.7 ?
C12 C13 C14 . . 119.5(2) ?
C12 C13 H13 . . 120.2 ?
C14 C13 H13 . . 120.2 ?
C15 C14 C13 . . 120.0(2) ?
C15 C14 H14 . . 120.0 ?
C13 C14 H14 . . 120.0 ?
C10 C15 C14 . . 120.53(19) ?
C10 C15 H15 . . 119.7 ?
C14 C15 H15 . . 119.7 ?
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
O1 C2 . 1.361(2) ?
O1 H1O . 0.90(3) ?
O2 C8 . 1.352(2) ?
O2 C9 . 1.451(2) ?
O3 C8 . 1.204(2) ?
N1 C7 . 1.283(2) ?
N1 N2 . 1.365(2) ?
N2 C8 . 1.355(2) ?
N2 H2N . 0.87(2) ?
C1 C6 . 1.399(2) ?
C1 C2 . 1.405(2) ?
C1 C7 . 1.459(2) ?
C2 C3 . 1.390(3) ?
C3 C4 . 1.386(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.387(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.381(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
C9 C10 . 1.498(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C15 . 1.384(3) ?
C10 C11 . 1.393(3) ?
C11 C12 . 1.383(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.376(4) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.388(4) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.387(3) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1O N1 . 0.90(3) 1.73(3) 2.546(2) 148(2) yes
N2 H2N O1 2_465 0.87(2) 1.97(2) 2.8225(19) 168(2) yes
C7 H7 O3 2_565 0.95 2.43 3.271(2) 146.8 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
C7 N1 N2 C8 . . . . 179.79(15) ?
C6 C1 C2 O1 . . . . -179.68(16) ?
C7 C1 C2 O1 . . . . 2.1(2) ?
C6 C1 C2 C3 . . . . -0.3(2) ?
C7 C1 C2 C3 . . . . -178.51(16) ?
O1 C2 C3 C4 . . . . -179.13(17) ?
C1 C2 C3 C4 . . . . 1.4(3) ?
C2 C3 C4 C5 . . . . -1.5(3) ?
C3 C4 C5 C6 . . . . 0.3(3) ?
C4 C5 C6 C1 . . . . 0.9(3) ?
C2 C1 C6 C5 . . . . -0.9(3) ?
C7 C1 C6 C5 . . . . 177.40(16) ?
N2 N1 C7 C1 . . . . 178.01(14) ?
C6 C1 C7 N1 . . . . -177.06(15) ?
C2 C1 C7 N1 . . . . 1.2(2) ?
C9 O2 C8 O3 . . . . -7.2(2) ?
C9 O2 C8 N2 . . . . 173.15(13) ?
N1 N2 C8 O3 . . . . -1.1(3) ?
N1 N2 C8 O2 . . . . 178.58(13) ?
C8 O2 C9 C10 . . . . -78.01(18) ?
O2 C9 C10 C15 . . . . 119.80(18) ?
O2 C9 C10 C11 . . . . -59.9(2) ?
C15 C10 C11 C12 . . . . 0.3(3) ?
C9 C10 C11 C12 . . . . -179.98(17) ?
C10 C11 C12 C13 . . . . 0.1(3) ?
C11 C12 C13 C14 . . . . -0.3(3) ?
C12 C13 C14 C15 . . . . 0.2(3) ?
C11 C10 C15 C14 . . . . -0.4(3) ?
C9 C10 C15 C14 . . . . 179.89(17) ?
C13 C14 C15 C10 . . . . 0.2(3) ?

_cod_database_fobs_code 2244176