#------------------------------------------------------------------------------
#$Date: 2021-08-25 05:10:51 +0300 (Wed, 25 Aug 2021) $
#$Revision: 268201 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243906.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_2243906
loop_
_publ_author_name
'Xu, Xiaowen'
'Hoogenboom, Richard'
'Van Hecke, Kristof'
_publ_section_title
;
 Crystal structures of three
 <i>N</i>-(pyridine-2-carbonyl)pyridine-2-carboxamides as potential
 ligands for supramolecular chemistry
;
_journal_coeditor_code           VM2252
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021008562
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C12 H7 F2 N3 O2'
_chemical_formula_moiety         'C12 H7 F2 N3 O2'
_chemical_formula_sum            'C12 H7 F2 N3 O2'
_chemical_formula_weight         263.21
_chemical_name_systematic
;
3-Fluoro-<i>N</i>-(3-fluoropyridine-2-carbonyl)pyridine-2-carboxamide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.140(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7062(3)
_cell_length_b                   14.1190(5)
_cell_length_c                   11.2074(5)
_cell_measurement_reflns_used    1899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9110
_cell_measurement_theta_min      5.0350
_cell_volume                     1052.94(8)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015)
;
_computing_structure_solution
;
ShelXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5200
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.370
_diffrn_reflns_theta_min         5.063
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0954P)^2^+0.7955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                856
_reflns_number_total             1083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2252sup1.cif
_cod_data_source_block           3
_cod_database_code               2243906
_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   0.878
_shelx_estimated_absorpt_t_max   0.931
_shelx_hkl_file
;
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   3   4  -7 5439.34 972.892  17
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   3   4  -5 6211.54 1089.96   2
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   3 -12   7 1236.46 428.193  13
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   3 -13  -8 4929.95 618.734  13
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   3 -13  -6 920.273 442.404  13
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   3 -13  -4 2119.87 572.023   8
   3 -13  -4 3047.68 829.478  13
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   3  13   6 197.107 202.588  17
   3 -14  -7 198.476 184.362  13
   3 -14  -7 604.416 210.924  10
   3 -14  -5 13444.5 1284.53  13
   3 -14  -5 13904.0 1089.37  10
   3  14  -5 14988.4 1181.43  17
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   3 -14  -3 17994.7 1641.65  13
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   3 -15   4 2711.35 468.974  13
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   3 -16   1 3700.29 554.221  13
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   3  16   1 3291.91 498.879  17
   4   0 -12 25261.4 1743.80   4
   4   0 -10 908.922 606.261   4
   4   0  -8 284.416 303.667   4
   4   0  -8 194.649 2348.56  17
   4   0  -6 47035.4 3402.35   2
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   4   0  -6 41745.3 2216.86   3
   4   0  -6 48724.4 2598.21   4
   4   0  -6 41310.0 3101.45   1
   4   0  -4 81378.2 3930.53   2
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   4   0  -2 22133.4 1881.47   2
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   4   0   2 829.608 583.300   2
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   4   0   4 12792.2 1274.60   3
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   4   1 -13 2189.54 416.442   4
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   4   1 -11 634.273 448.034   4
   4  -1 -11 1156.38 489.260   4
   4   1  -9 1043.64 478.957   4
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   4   1  -7 2963.19 869.959   1
   4  -1  -7 3066.64 795.636   4
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   4   1  -7 2932.55 946.764   2
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   4  -1  -7 2814.52 919.892   1
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   4   1  -7 1495.32 715.357  17
   4   1  -5 18735.6 2051.93   2
   4  -1  -5 18871.3 2030.79   2
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   4   1  -3 43865.3 2736.67   2
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   4   1   3 10024.0 1583.22   2
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   4   1   5 62.2633 348.865   3
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   4   1   9 2587.25 551.253   3
   4   1  11 9056.24 685.663   3
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   4   2 -12 463.513 328.921   4
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   4   2  -8 7808.18 1192.84   4
   4  -2  -8 6689.18 1135.21   4
   4   2  -8 5826.22 1396.38  17
   4  -2  -6 11722.8 1275.32   8
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   4  -2  -6 15629.8 2018.05   2
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   4  -2  -4 4201.07 1003.31   2
   4   2  -2 330085. 7304.06   2
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   4   2   0 108821. 4313.36   2
   4  -2   0 106034. 4278.32   2
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   4   2   2 68667.1 3822.25   2
   4  -2   2 76577.7 3962.96   2
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   4   2   4 30892.8 1799.81  20
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   4  -2   4 30907.7 1953.39   3
   4   2   4 33306.3 2034.21   3
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   4  -2   6 42644.9 2384.89   3
   4   2   6 45625.6 2492.48   3
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   4  -2   8 23655.3 1719.51   3
   4   2   8 21481.2 1627.15   3
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   4  -2  10-139.888 316.682   3
   4   2  10 19.5034 229.207   3
   4   3 -11 529.049 309.814   4
   4  -3 -11 469.773 414.250   4
   4   3  -9 2790.94 854.787   4
   4  -3  -9 2276.29 692.650   4
   4   3  -9 1665.45 1760.32  17
   4  -3  -7 214.077 249.015   8
   4   3  -7-32.6049 307.441   4
   4  -3  -7 47.6831 263.094   4
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   4   3  -7-19.1352 298.076   2
   4   3  -7 423.740 532.029  17
   4  -3  -5 1996.82 574.180   8
   4   3  -5 2597.65 586.230   4
   4  -3  -5 2336.21 540.316   4
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   4   3  -5 1661.26 563.494   2
   4  -3  -5 2347.26 814.923   2
   4   3  -5 1756.01 466.852   3
   4  -3  -5 1909.99 430.399   3
   4   3  -5 2125.83 575.488  17
   4  -3  -3 5170.84 1014.28   2
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   4   3  -3 4726.90 952.115   2
   4   3  -1 52372.1 2954.20   2
   4  -3  -1 51334.0 2881.57   2
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   4   3   1 1249.12 588.213   2
   4  -3   1 2351.92 759.897   2
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   4   3   3 7401.56 1380.05   2
   4  -3   3 8591.74 1445.95   2
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   4   3   5-17.8279 326.146  20
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   4  -3   5 67.7696 294.176   3
   4   3   5-203.620 252.168   3
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   4   3   7 92.9496 173.708  20
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   4  -3   7-586.974 351.788   3
   4   3   7 449.424 375.232   3
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   4  -3   9 468.154 293.022   3
   4   3   9 485.568 347.940   3
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   4   3  11 371.232 147.750   3
   4   4 -12 45.7125 175.839   4
   4  -4 -12 311.647 273.841   4
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   4   4 -10 495.349 398.610   4
   4  -4 -10 159.023 410.120   4
   4   4 -10-1092.43 2847.07  17
   4  -4  -8 8388.39 1114.18  10
   4   4  -8 8636.68 1243.34   4
   4  -4  -8 8458.58 1233.22   4
   4   4  -8 7965.03 1247.51  17
   4  -4  -8 7727.39 1142.75   8
   4  -4  -6 4503.44 902.715   8
   4   4  -6 4468.53 815.790   4
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   4   4  -6 4626.43 1116.09   2
   4  -4  -6 4708.37 1107.17   2
   4  -4  -6 4945.60 895.343   4
   4   4  -6 3687.07 871.116  17
   4   4  -4 37663.4 2790.26   2
   4  -4  -4 36097.2 2693.47   2
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   4   4  -2 15512.7 1654.26   2
   4  -4  -2 13493.4 1525.65   2
  -4   4   2 14176.6 1727.53  14
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  -4   4   0 5991.95 1123.90  14
   4   4   0 6357.17 1109.63   2
   4  -4   0 5882.11 1053.26   2
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  -4   4   0 7603.81 1155.03   5
  -4   4  -2 34074.8 2732.46  14
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   4   4   2 35191.5 2784.38   2
   4  -4   2 33339.4 2684.86   2
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  -4   4  -4 12479.3 1742.97  14
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   4   4   4 11377.9 1789.36   2
   4  -4   4 13211.6 1886.95   2
   4  -4   4 11808.0 1192.85   3
   4   4   4 10916.5 1156.77   3
  -4   4  -4 13728.2 1573.57  12
  -4   4  -4 12651.6 1723.63   5
   4   4   4 13787.5 1313.24  20
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  -4   4  -4 11121.0 1838.30   1
  -4  -4  -4 10956.0 1859.67   1
  -4   4  -6 883.178 582.696  12
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   4   4   6 1460.97 467.122  20
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   4  -4   6 1650.24 530.516   3
   4   4   6 1273.24 432.153   3
   4   4   8 693.808 325.525  20
  -4   4  -8-162.471 461.290  12
  -4  -4  -8 363.009 318.944  12
  -4   4  -8 122.804 415.195  18
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   4  -4   8 441.098 386.219   3
   4   4   8-41.3513 254.014   3
   4   4  10 2862.54 424.876   3
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  -4   4 -10 2776.09 603.255  12
  -4  -4 -10 2470.77 532.314  18
   4  -4  10 2848.69 433.634   3
   4   5 -11 598.918 290.071   4
   4  -5 -11 632.280 325.822   4
   4  -5  -9 12850.9 1305.47  10
   4   5  -9 12289.5 1438.89   4
   4  -5  -9 11082.9 1356.83   4
   4   5  -9 14102.3 1794.53  17
   4  -5  -9 10248.9 1326.41   8
   4  -5  -7 397.071 356.403   8
   4   5  -7-108.341 293.060   4
   4  -5  -7 1083.81 463.687   4
   4   5  -7 338.211 472.745  17
   4  -5  -5 4212.61 832.375   8
   4  -5  -5 3048.21 628.021   4
  -4   5   5 5154.82 1194.59  14
   4   5  -5 3505.05 888.517   2
   4  -5  -5 3327.76 891.503   2
   4   5  -5 4344.14 795.133   4
   4   5  -5 4345.88 896.458  17
   4  -5  -3 27344.4 1901.23   8
   4   5  -3 27250.3 2301.45   2
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   4   5  -1 425.988 324.868   2
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   4   5   3 10084.1 1582.25   2
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   4   5   3 8627.59 974.461   3
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   4   7  -3 16975.5 1397.88  20
   4  -7  -3 15216.6 1700.59  13
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   4   7  -3 22363.1 1899.20  17
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   4  -8 -10 5548.98 737.587  10
   4   8 -10 6277.01 1637.71  17
   4   8  -8 23388.1 1920.09  17
   4  -8  -8 16925.6 1719.41   8
   4  -8  -6 5190.34 1014.35  13
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   4   8   2 3408.73 716.424  20
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   4   8   6 8793.09 1066.40  20
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   4   9  -1 5779.34 861.845  20
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   4   9  -1 6542.25 1115.52  17
   4  -9   1 79854.0 3305.45   8
   4  -9   1 73848.7 3923.60  13
   4   9   1 76018.7 3143.40  20
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   4   9   1 81066.4 3626.38  17
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   4 -11  -9 1857.72 379.486  10
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   4 -11  -5 3232.64 743.400  13
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   4 -11  -1 188.432 481.160  13
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   4  11   5 23013.4 1456.47  20
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   4 -11   7 1745.26 479.425  13
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   4 -12  -8 11476.3 871.097  10
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   4 -12  -6 2645.41 634.741   8
   4 -12  -6 3469.96 633.416  13
   4  12  -6 4050.74 739.775  17
   4 -12  -4 12265.7 1425.93  13
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   4 -12  -4 12831.7 1360.53   8
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   4  12   2 826.277 419.733  17
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   4  12   4 21555.0 1343.20  20
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   4  12   4 15387.5 1268.20  17
   4  12   6 21204.2 1100.98  20
   4 -12   6 23714.9 1513.15  13
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   4 -13  -7 10961.7 827.601  10
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   4  13  -5 4187.10 690.705  17
   4 -13  -3 15639.9 1547.74  13
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   4  13   3 431.774 352.825  17
   4 -13   5-280.492 298.586  13
   4  13   5 161.690 141.737  20
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   4 -14  -4 594.189 309.517  13
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   4  14   2 652.954 307.188  17
   4 -14   4 1566.54 376.516  13
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   4 -15  -3 19173.8 1175.38  13
   4  15  -3 19447.7 1106.69  17
   4 -15  -1 109.405 199.747  13
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   4  15   1 10763.2 829.560  17
   5   0 -11-60.4637 364.670   4
   5   0  -9 62.5125 452.479   4
   5   0  -7 309.813 432.223   4
   5   0  -7-259.174 2093.52  17
   5   0  -5 114.882 287.302   4
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   5   0  -5-395.391 775.339   2
   5   0  -5 204.653 309.303   3
   5   0  -5 830.725 585.172  17
   5   0  -3-640.856 364.072   4
   5   0  -3 551.957 493.227   2
   5   0  -3 21.9046 270.258   3
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   5   0  -1-1316.32 651.147   2
   5   0  -1-11.3501 250.634   3
   5   0  -1-1034.28 399.251  20
   5   0   1-163.830 321.013   2
   5   0   1-38.9086 359.353  20
   5   0   1 18.4221 210.990   3
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   5   0   3 437.620 506.294   2
   5   0   3-130.537 275.200   3
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   5   0   5 360.842 421.202   3
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   5   0   7 346.065 380.481   3
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   5   0   9 61.6294 257.344   3
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   5   1 -12 1421.00 354.941   4
   5  -1 -12 1635.82 431.572   4
   5   1 -10 1223.06 547.086   4
   5  -1 -10-39.9831 434.353   4
   5   1  -8 2784.23 842.748   4
   5  -1  -8 2555.04 724.061   4
   5   1  -8 2105.03 2725.62  17
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   5   1  -6 15046.7 1436.97   3
   5  -1  -6 14694.9 1424.86   3
   5   1  -6 15449.2 1613.28   4
   5  -1  -6 15628.6 1628.39   4
   5   1  -6 10782.1 1508.21  17
   5  -1  -4 1446.07 516.491   8
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   5   3 -10 442.451 384.153   4
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   5  -3  -4 271.626 437.041   2
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   5   3  -4 334.726 265.379   3
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   5  -3   0 16782.9 1414.97   3
   5   3   0 16141.1 1413.38   3
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   5  -3   2-732.749 600.121   2
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   5   3   2-1201.29 460.987   3
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   5   3   4 217.468 342.192   3
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   5   3   6 4280.74 655.143  20
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   5   3   6 3736.02 729.133   3
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   5  -3   8 1481.10 422.705   3
   5   3   8 858.490 322.715   3
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   5   4 -11 4722.47 668.906   4
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   5  -4  -9 13292.6 1401.50   4
   5   4  -9 13484.9 2506.58  17
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   5   4  -5 306.704 346.742   3
   5  -4  -5 186.606 261.894   3
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   5   4  -3 4649.37 824.821   4
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   5  -4  -1 521.903 429.415   2
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   5   4  -1 1030.39 426.177   3
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   5  -4   1 315.609 320.564   3
   5   4   1 568.670 320.450   3
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   5  -4   3 18799.8 1541.27   3
   5   4   3 20106.7 1615.71   3
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   5   4   3 22976.6 1721.63  20
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   5   4   7 488.368 275.390   3
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   5   4   9 883.290 251.665   3
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   5  -5  -8 10111.6 1235.55   8
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   5  -5  -6 2555.52 657.815   4
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   5   5  -2 5188.91 783.011   3
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   5   5   6 145.190 248.121   3
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   5  -6  -7 8375.43 1045.04   4
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   5  -6  -5 218.036 391.521   8
   5  -6  -5-152.033 312.719   4
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   5   6  -3 13618.7 1349.80  20
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   5  -6   9 680.022 219.468  13
   5  -7  -8 919.953 496.879   8
   5  -7  -8 466.089 281.079  10
   5   7  -8 677.041 471.271  17
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   5   7  -6 1038.81 556.137  17
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   5   7  -4 10237.9 1360.85  17
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   5   7  -2 843.087 421.848  20
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   5   7   8 4455.20 449.677  20
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   5  -8  -9 2221.48 428.615  10
   5   8  -9 3060.91 1072.75  17
   5  -8  -7 1990.12 648.135   8
   5   8  -7 1928.00 685.576  17
   5  -8  -5 639.907 495.320   8
   5   8  -5-74.2035 449.423  17
   5  -8  -3 4306.85 911.476   8
   5  -8  -3 2601.90 706.896  13
   5   8  -3 3130.05 666.968  20
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   5   8  -1 8441.71 1063.38  20
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   5   8  -1 7401.75 1107.27  17
   5  -8   1 15499.8 1541.06   8
   5  -8   1 11389.5 1567.89  13
   5   8   1 14176.4 1377.67  20
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   5   8   1 11397.4 1278.81  17
   5  -8   3 982.560 454.095   8
   5  -8   3 1008.16 597.928  13
   5   8   3 386.867 280.022  20
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   5   8   5 4434.27 726.173  20
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   5  -8   7-162.397 257.188  13
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   5  -9  -8 360.847 360.894   8
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   5  -9  -8 771.102 324.924  10
   5   9  -8-54.6764 425.067  17
   5   9  -6 9168.18 1192.11  17
   5  -9  -6 6522.11 1014.83   8
   5  -9  -4 572.995 461.592   8
   5  -9  -4 614.742 443.661  13
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   5   9  -4 1077.44 610.430  17
   5  -9  -2 615.698 489.896   8
   5  -9  -2 149.685 528.138  13
   5   9  -2 36.0968 278.568  20
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   5   9  -2 437.513 421.564  17
   5  -9   0 30354.9 2123.11   8
   5  -9   0 22458.0 2125.75  13
   5   9   0 26426.2 1817.17  20
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   5   9   0 24025.3 1895.38  17
   5  -9   2 4002.51 703.399   8
   5  -9   2 3271.69 846.439  13
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   6   9  -1 806.278 385.152  20
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   6   9   1 1112.53 401.180  20
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   6  -9   3-375.200 215.283   8
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   6   9   3 128.545 193.341  20
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   6   9   5 396.893 153.318  20
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   6 -10  -4 7325.05 901.901   8
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   6 -10   0 54414.5 2254.54   8
   6  10   0 59347.5 2141.78  20
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   6 -10   2 521.720 261.739  13
   6  10   2-417.732 270.771  20
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   6  10   4 1911.35 320.920  20
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   6 -11  -5 1829.68 412.806   8
   6  11  -5 2663.81 463.320  17
   6 -11  -3 950.881 334.665   8
  -6  11   3 1193.90 317.676  18
   6  11  -3 1266.53 381.596  17
   6 -11  -1 1058.51 315.038   8
  -6  11   1 1789.28 435.049  18
   6  11  -1 1229.76 311.858  17
   6 -11   1 1135.51 277.507  13
   6  11   1 1282.09 299.327  20
  -6  11  -1 753.639 193.516  11
  -6  11  -1 1079.87 336.719  18
   6  11   3 419.664 166.211  20
  -6  11  -3 464.415 212.382  18
  -6  12   2 2224.54 373.742  18
  -6  12   0 3531.35 484.443  18
   7   0  -9-15.8542 182.495   4
   7   0  -7 655.722 368.060   4
   7   0  -5-80.7016 297.532   4
   7   0  -5 87.1316 405.380   3
   7   0  -3-233.919 365.492   4
   7   0  -3-17.6104 351.676   3
   7   0  -1-149.747 381.277   4
   7   0  -1-91.7152 349.159   3
   7   0   1-139.124 292.336   3
  -7   0  -1 261.517 553.756  18
   7   0   3-3.92540 264.908   3
  -7   0  -3-303.234 476.835  18
   7   0   5-355.330 266.222   3
  -7   0  -5-181.524 304.218  18
   7   1  -8 2249.05 497.352   4
   7  -1  -8 2359.76 520.399   4
   7   1  -6 236.011 312.671   4
   7  -1  -6 375.672 419.106   4
   7  -1  -4-1.24713 239.036   8
   7  -1  -4 378.964 444.690   4
   7  -1  -4 201.242 385.803   3
   7  -1  -2 1353.67 473.456   8
   7   1  -2 1821.95 459.259   8
   7   1  -2 830.167 396.431   4
   7  -1  -2 822.971 451.624   4
   7  -1  -2 1073.08 454.126   3
   7   1  -2 1025.02 446.999   3
   7   1   0 4203.48 806.413   4
   7  -1   0 5071.93 783.495   3
   7   1   0 4501.38 769.499   3
  -7   1   0 4119.73 962.360  18
   7  -1   0 4438.98 805.424   4
   7  -1   2 2507.55 574.517   3
   7   1   2 2243.37 592.444   3
  -7   1  -2 1757.13 785.494  18
  -7  -1  -2 1956.38 669.792  18
   7  -1   4 360.107 294.935   3
   7   1   4-74.3992 330.841   3
  -7   1  -4 173.618 354.448  18
  -7  -1  -4 175.503 399.832  18
   7   1   6 1107.86 237.927   3
   7  -1   6 781.344 229.386   3
  -7   1  -6 595.178 285.725  18
  -7  -1  -6 611.262 279.755  18
   7   2  -7 4186.52 705.234   4
   7  -2  -7 5093.89 771.413   4
   7   2  -5 1209.57 471.262   4
   7  -2  -5 1708.51 565.515   4
   7  -2  -3 4937.30 835.260   8
   7  -2  -3 4211.18 798.840   4
   7   2  -3 3959.54 747.323   3
   7  -2  -3 4179.52 731.577   3
   7   2  -3 5033.94 883.722   4
   7  -2  -1 6607.33 1003.29   8
   7  -2  -1 6625.78 882.303   3
   7   2  -1 5133.14 819.789   3
   7   2  -1 6796.06 1001.65   4
   7  -2  -1 6307.59 961.745   4
   7  -2   1 2166.16 554.599   3
   7   2   1 2790.12 601.869   3
  -7   2  -1 2452.36 755.574  18
  -7  -2  -1 1530.34 680.370  18
   7  -2   3 2311.96 499.556   3
   7   2   3 2358.78 523.020   3
  -7   2  -3 2125.78 756.844  18
  -7  -2  -3 3304.26 783.330  18
   7   2   5 10279.9 784.714   3
   7  -2   5 10025.8 777.662   3
  -7   2  -5 9236.48 1032.88  18
  -7  -2  -5 8836.10 1031.67  18
   7   3  -8 6243.88 712.904   4
   7  -3  -8 4818.48 641.652   4
   7   3  -6 1821.55 519.974   4
   7  -3  -6 1642.79 517.098   4
   7  -3  -4 9457.75 1092.05   8
   7   3  -4 7740.40 952.612   3
   7  -3  -4 7977.07 970.691   3
   7   3  -4 8581.55 1065.90   4
   7  -3  -4 7872.55 1031.23   4
   7  -3  -2 172.091 349.388   8
   7   3  -2-725.211 400.927   4
   7  -3  -2-296.553 385.420   4
   7  -3  -2-93.9145 285.575   3
   7   3  -2 100.549 288.454   3
   7   3   0 303.360 278.707   4
   7  -3   0-86.4239 297.415   4
   7  -3   0-70.1786 271.123   3
   7   3   0 215.549 307.421   3
  -7   3   0-358.812 490.744  18
   7  -3   2 337.714 329.060   3
   7   3   2-15.8770 266.589   3
  -7   3  -2 319.436 495.987  18
  -7  -3  -2-314.287 509.757  18
   7   3   4-609.309 307.651   3
   7  -3   4 575.515 275.434   3
  -7   3  -4 158.601 375.260  18
  -7  -3  -4 310.990 329.559  18
   7   4  -7 318.974 239.016   4
   7  -4  -7 139.018 254.608   4
   7  -4  -5 2541.83 573.489   8
   7   4  -5 2593.21 555.274   4
   7  -4  -5 2951.88 631.073   4
   7  -4  -3 1.36469 320.798   8
   7   4  -3 160.549 243.386   4
   7  -4  -3-96.3559 301.243   4
   7   4  -3-73.1405 261.415   3
   7  -4  -3-38.7761 285.728   3
   7  -4  -1 619.514 467.480   8
   7   4  -1 1319.22 477.264   4
   7  -4  -1 1168.29 450.609   4
   7   4  -1 713.822 334.871   3
   7  -4  -1 980.589 414.952   3
  -7   4   1 70.1265 498.294  18
   7   4   1 826.971 379.696   4
   7  -4   1 1198.42 394.781   4
   7  -4   1 1778.72 469.561   3
   7   4   1 1585.00 452.190   3
  -7   4  -1 1586.34 608.728  18
   7   4   3 1593.63 436.704   4
   7  -4   3 2295.68 508.521   4
   7   4   3 2912.39 480.247   3
   7  -4   3 3632.83 535.877   3
  -7   4  -3 2584.48 649.808  18
  -7  -4  -3 1656.27 540.021  18
   7  -4   5 152.148 168.079   8
  -7  -4  -5 328.805 306.709  18
   7  -5  -6 310.858 230.491   8
   7   5  -6 274.064 163.195   4
   7  -5  -6 151.501 162.350   4
   7  -5  -4 388.173 342.433   8
   7   5  -4-461.997 258.395   4
   7  -5  -4-60.5300 249.734   4
   7  -5  -2 3159.31 682.852   8
   7   5  -2 1946.94 541.715   4
   7  -5  -2 2426.79 548.488   4
   7   5  -2 2030.11 451.224   3
   7  -5  -2 1834.32 445.125   3
   7  -5   0-12.3887 336.573   8
   7   5   0-362.142 266.932   4
   7  -5   0-346.162 333.366   4
   7   5   0 58.7146 234.330   3
   7  -5   0-261.331 373.885   3
  -7   5   0 779.831 487.041  18
   7  -5   2 1808.36 496.408   8
   7   5   2 667.339 307.103   4
   7  -5   2 999.691 338.635   4
   7   5   2 838.389 317.438   3
   7  -5   2 992.285 284.279   3
   7   5   2 1647.49 419.782  20
  -7   5  -2 1474.44 536.785  18
   7  -5   4-281.571 256.054   8
  -7   5  -4-64.6978 334.327  18
  -7  -5  -4 640.499 309.031  18
   7  -6  -5 1362.37 431.901   8
   7  -6  -3 3555.66 670.970   8
   7  -6  -1 84.2027 276.976   8
  -7   6   1-875.581 407.826  18
   7  -6   1 6915.13 879.015   8
  -7   6  -1 5219.60 868.395  18
   7  -6   3 956.981 300.075   8
  -7   6  -3 745.821 351.834  18
   7  -7  -6 823.096 264.304   8
   7  -7  -4 482.974 283.544   8
   7  -7  -2 6981.20 872.503   8
   7  -7   0 8255.60 943.770   8
  -7   7   0 7568.47 948.946  18
   7  -7   2 1269.27 371.603   8
  -7   7  -2 1157.70 406.726  18
   7  -8  -5 358.169 241.178   8
   7  -8  -3 58.6335 226.729   8
   7  -8  -1 15716.2 1173.93   8
  -7   8   1 12357.2 1012.02  18
   7  -8   1 3250.77 527.617   8
  -7   8  -1 4014.85 618.966  18
  -7   8  -3 13.4761 162.560  18
   7  -9  -4 1695.16 330.084   8
   7  -9  -2 1371.40 344.018   8
   7  -9   0 2396.35 391.565   8
  -7   9   0 2917.12 476.366  18
   8   0  -6-145.421 167.475   4
   8   0  -4 4542.20 614.556   4
   8   0  -2 2895.01 485.162   3
   8   0  -2 3232.64 546.657   4
   8   0   0 1277.23 283.617   8
   8   0   0 1352.75 353.316   4
   8   0   0 1491.09 367.476   3
   8   0   2 10918.7 734.906   3
   8   0   2 8438.62 690.633   4
   8   1  -5 5717.48 646.675   4
   8  -1  -5 4117.21 558.094   4
   8   1  -3 84.5732 226.704   4
   8  -1  -3 279.241 232.623   4
   8   1  -3 60.3752 226.352   3
   8  -1  -3-199.645 263.130   3
   8  -1  -1-401.973 213.851   8
   8   1  -1 165.815 244.141   4
   8  -1  -1-180.704 269.562   4
   8   1  -1 337.596 243.075   3
   8  -1  -1 0.71820 226.103   3
   8  -1   1 291.472 201.186   8
   8   1   1 894.733 275.337   4
   8  -1   1 142.568 177.335   4
   8   1   1 814.491 257.430   3
   8  -1   1 363.331 187.473   3
   8   2  -4 2170.47 434.511   4
   8  -2  -4 2175.53 426.328   4
   8  -2  -2-434.158 193.574   8
   8   2  -2 411.159 243.768   4
   8  -2  -2-322.080 293.147   4
   8   2  -2 418.787 210.255   3
   8  -2  -2 296.499 227.082   3
   8  -2   0-174.066 179.769   8
   8   2   0 250.792 232.420   4
   8  -2   0-152.549 242.264   4
   8   2   0-42.4811 173.134   3
   8  -2   0-13.2529 173.095   3
   8  -2   2 548.446 207.867   8
   8   2   2 758.006 224.311   4
   8  -2   2 384.099 188.704   4
   8   2   2 1039.04 240.910   3
   8  -2   2 995.346 248.147   3
   8  -3  -3 967.101 248.931   8
   8   3  -3 922.779 280.147   4
   8  -3  -3 1246.21 327.269   4
   8  -3  -1 83.5270 162.148   8
   8   3  -1 322.076 208.751   4
   8  -3  -1 159.982 185.216   4
   8   3  -1-35.9062 158.256   3
   8  -3  -1 464.911 233.106   3
   8  -3   1 287.768 150.089   8
   8   3   1 147.639 157.534   4
   8  -3   1 387.412 175.027   4
   8   3   1 334.657 174.869   3
   8  -3   1 804.253 211.600   3
   8  -4  -2 12006.4 896.426   8
   8  -4   0 337.295 176.482   8
   8  -5  -1 4602.81 531.064   8
   0   0   0    0.00    0.00   0
TITL RH065 in I2/a
REM I2/a (#15 in standard setting)
CELL 1.54184   6.706183  14.119024  11.207425  90.0000  97.1403  90.0000
ZERR    4.00   0.000318   0.000505   0.000502   0.0000   0.0044   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O F
UNIT 40.00 40.00 8.00 8.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum              90054
_shelx_res_file
;
TITL RH065 in I2/a #15
    rh065.res
    created by SHELXL-2018/3 at 15:06:26 on 18-Aug-2020
REM reset to I2/a #15
CELL 1.54184 6.706183 14.119024 11.207425 90 97.1403 90
ZERR 4 0.000318 0.000505 0.000502 0 0.0044 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H F N O
UNIT 48 28 8 12 8
L.S. 30
PLAN  20
SIZE 0.06 0.089 0.11
TEMP -173(2)
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./RH065.hkl">
REM </olex2.extras>
WGHT    0.095400    0.795500
FVAR       4.89728
F1    3    0.101207    0.499420    0.141901    11.00000    0.05507    0.01909 =
         0.02920    0.00706   -0.00022   -0.00624
O1    5    0.164869    0.539962    0.379773    11.00000    0.04039    0.01568 =
         0.03164    0.00226    0.00056    0.00159
N1    4    0.059643    0.296743    0.332922    11.00000    0.01899    0.01706 =
         0.02539    0.00140    0.00380    0.00165
N2    4    0.250000    0.410711    0.500000    10.50000    0.02540    0.01409 =
         0.02621    0.00000    0.00421    0.00000
C2    1    0.061200    0.410861    0.177089    11.00000    0.02618    0.01652 =
         0.03086    0.00479    0.00417    0.00116
C1    1    0.094474    0.385672    0.297927    11.00000    0.02030    0.01673 =
         0.02779    0.00206    0.00228    0.00221
C5    1   -0.010378    0.233754    0.249379    11.00000    0.01877    0.01745 =
         0.02697    0.00083    0.00580    0.00073
AFIX  43
H5    2   -0.037842    0.171355    0.274533    11.00000   -1.20000
AFIX   0
C4    1   -0.045254    0.254748    0.127300    11.00000    0.02131    0.02229 =
         0.02583   -0.00222    0.00143    0.00249
AFIX  43
H4    2   -0.094044    0.207588    0.070604    11.00000   -1.20000
AFIX   0
C3    1   -0.007484    0.345573    0.090221    11.00000    0.02759    0.02394 =
         0.02217    0.00285    0.00141    0.00393
AFIX  43
H3    2   -0.028177    0.362470    0.007558    11.00000   -1.20000
AFIX   0
C6    1    0.171134    0.454732    0.394364    11.00000    0.02219    0.01623 =
         0.02590    0.00088    0.00507    0.00137
H2    2    0.250000    0.350707    0.500000    10.50000   -1.20000
HKLF 4
REM  RH065 in I2/a #15
REM wR2 = 0.1612, GooF = S = 1.039, Restrained GooF = 1.039 for all data
REM R1 = 0.0553 for 856 Fo > 4sig(Fo) and 0.0712 for all 1083 data
REM 88 parameters refined using 0 restraints
END
WGHT      0.0954      0.7955
REM Highest difference peak  0.292,  deepest hole -0.319,  1-sigma level  0.076
Q1    1   0.0635  0.4185  0.4816  11.00000  0.05    0.29
Q2    1   0.0000  0.1459  0.2593  11.00000  0.05    0.25
Q3    1  -0.0657  0.4279  0.2591  11.00000  0.05    0.24
Q4    1   0.1013  0.5876  0.1419  11.00000  0.05    0.24
Q5    1   0.2282  0.2983  0.3628  11.00000  0.05    0.24
Q6    1   0.1220  0.0728  0.2675  11.00000  0.05    0.23
Q7    1   0.1113  0.2705  0.4082  11.00000  0.05    0.23
Q8    1   0.3783  0.4906  0.2649  11.00000  0.05    0.23
Q9    1   0.2640  0.5089  0.0813  11.00000  0.05    0.23
Q10   1   0.2500  0.4271  0.0000  10.50000  0.05    0.22
Q11   1  -0.2500  0.1734  0.0000  10.50000  0.05    0.22
Q12   1   0.2500  0.3160  0.5000  10.50000  0.05    0.22
Q13   1   0.0757  0.5942  0.3214  11.00000  0.05    0.21
Q14   1  -0.0116  0.5543  0.0776  11.00000  0.05    0.21
Q15   1  -0.1821  0.4406  0.0231  11.00000  0.05    0.19
Q16   1   0.1976  0.4429 -0.0270  11.00000  0.05    0.19
Q17   1  -0.2665  0.1445  0.2562  11.00000  0.05    0.19
Q18   1   0.1669  0.4345 -0.0486  11.00000  0.05    0.19
Q19   1   0.0096  0.5785  0.3972  11.00000  0.05    0.19
Q20   1  -0.1850  0.1565 -0.0533  11.00000  0.05    0.18
;
_shelx_res_checksum              48074
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
F F1 0.1012(3) 0.49942(9) 0.14190(14) 0.0349(5) Uani d 1 . .
O O1 0.1649(3) 0.53996(11) 0.37977(16) 0.0296(5) Uani d 1 . .
N N1 0.0596(3) 0.29674(13) 0.33292(17) 0.0204(5) Uani d 1 . .
N N2 0.250000 0.41071(19) 0.500000 0.0218(6) Uani d 1 . .
C C2 0.0612(4) 0.41086(16) 0.1771(2) 0.0245(6) Uani d 1 . .
C C1 0.0945(3) 0.38567(15) 0.2979(2) 0.0217(5) Uani d 1 . .
C C5 -0.0104(3) 0.23375(15) 0.2494(2) 0.0208(5) Uani d 1 . .
H H5 -0.037842 0.171355 0.274533 0.025 Uiso calc 1 . .
C C4 -0.0453(3) 0.25475(16) 0.1273(2) 0.0233(5) Uani d 1 . .
H H4 -0.094044 0.207588 0.070604 0.028 Uiso calc 1 . .
C C3 -0.0075(4) 0.34557(16) 0.0902(2) 0.0247(6) Uani d 1 . .
H H3 -0.028177 0.362470 0.007558 0.030 Uiso calc 1 . .
C C6 0.1711(3) 0.45473(15) 0.3944(2) 0.0213(5) Uani d 1 . .
H H2 0.250000 0.351(3) 0.500000 0.026 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
F1 0.0551(11) 0.0191(7) 0.0292(9) -0.0062(6) -0.0002(7) 0.0071(6)
O1 0.0404(10) 0.0157(8) 0.0316(10) 0.0016(7) 0.0006(8) 0.0023(7)
N1 0.0190(9) 0.0171(9) 0.0254(10) 0.0017(7) 0.0038(7) 0.0014(7)
N2 0.0254(13) 0.0141(12) 0.0262(15) 0.000 0.0042(11) 0.000
C2 0.0262(11) 0.0165(10) 0.0309(13) 0.0012(9) 0.0042(10) 0.0048(9)
C1 0.0203(11) 0.0167(11) 0.0278(12) 0.0022(8) 0.0023(9) 0.0021(9)
C5 0.0188(10) 0.0174(10) 0.0270(12) 0.0007(8) 0.0058(9) 0.0008(8)
C4 0.0213(11) 0.0223(11) 0.0258(12) 0.0025(8) 0.0014(9) -0.0022(9)
C3 0.0276(11) 0.0239(12) 0.0222(12) 0.0039(9) 0.0014(10) 0.0028(9)
C6 0.0222(11) 0.0162(10) 0.0259(12) 0.0014(8) 0.0051(9) 0.0009(9)
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'
F F 0.0727 0.0534 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -8 4 0.0377
3 -6 -3 0.0466
3 1 -5 0.0572
-3 5 4 0.0346
0 -4 -6 0.0228
-2 -7 -3 0.0187
-1 1 7 0.0371
3 7 0 0.0440
1 6 5 0.0377
-2 5 -5 0.0264
4 -1 3 0.0579
-2 8 2 0.0279
1 9 -2 0.0348
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
C5 N1 C1 . . 118.5(2) ?
C6 N2 C6 2_556 . 126.6(3) ?
C6 N2 H2 2_556 . 116.71(13) ?
C6 N2 H2 . . 116.71(13) ?
F1 C2 C1 . . 120.5(2) ?
F1 C2 C3 . . 118.4(2) ?
C3 C2 C1 . . 121.1(2) ?
N1 C1 C2 . . 120.7(2) ?
N1 C1 C6 . . 117.0(2) ?
C2 C1 C6 . . 122.3(2) ?
N1 C5 H5 . . 118.3 ?
N1 C5 C4 . . 123.4(2) ?
C4 C5 H5 . . 118.3 ?
C5 C4 H4 . . 120.7 ?
C3 C4 C5 . . 118.6(2) ?
C3 C4 H4 . . 120.7 ?
C2 C3 C4 . . 117.8(2) ?
C2 C3 H3 . . 121.1 ?
C4 C3 H3 . . 121.1 ?
O1 C6 N2 . . 124.3(2) ?
O1 C6 C1 . . 123.0(2) ?
N2 C6 C1 . . 112.68(19) ?
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
F1 C2 . 1.348(2) ?
O1 C6 . 1.214(3) ?
N1 C1 . 1.344(3) ?
N1 C5 . 1.334(3) ?
N2 C6 2_556 1.383(3) ?
N2 C6 . 1.383(3) ?
N2 H2 . 0.85(4) ?
C2 C1 . 1.391(3) ?
C2 C3 . 1.378(3) ?
C1 C6 . 1.498(3) ?
C5 H5 . 0.9500 ?
C5 C4 . 1.391(3) ?
C4 H4 . 0.9500 ?
C4 C3 . 1.381(3) ?
C3 H3 . 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_D
_geom_hbond_site_symmetry_H
_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 H2 N1 ? ? ? 0.84(4) 2.265(15) 2.671(2) 109.8(10) yes
N2 H2 N1 . . 2_556 0.84(4) 2.265(15) 2.671(2) 109.8(10) yes
C4 H4 O1 . . 4_445 0.95 2.49 3.135(3) 125 yes
C5 H5 O1 . . 4_445 0.95 2.61 3.207(3) 122 yes
C3 H3 F1 . . 5_565 0.95 2.58 3.398(3) 145 yes
C5 H5 F1 . . 4_445 0.95 2.66 3.604(3) 176 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
F1 C2 C1 N1 . . . . -178.3(2) ?
F1 C2 C1 C6 . . . . 1.3(4) ?
F1 C2 C3 C4 . . . . 179.1(2) ?
N1 C1 C6 O1 . . . . -162.6(2) ?
N1 C1 C6 N2 . . . . 17.9(3) ?
N1 C5 C4 C3 . . . . -0.6(3) ?
C2 C1 C6 O1 . . . . 17.8(4) ?
C2 C1 C6 N2 . . . . -161.7(2) ?
C1 N1 C5 C4 . . . . 1.4(3) ?
C1 C2 C3 C4 . . . . 1.0(4) ?
C5 N1 C1 C2 . . . . -1.0(3) ?
C5 N1 C1 C6 . . . . 179.41(19) ?
C5 C4 C3 C2 . . . . -0.6(3) ?
C3 C2 C1 N1 . . . . -0.2(4) ?
C3 C2 C1 C6 . . . . 179.3(2) ?
C6 N2 C6 O1 2_556 . . . 1.68(18) ?
C6 N2 C6 C1 2_556 . . . -178.8(2) ?