#------------------------------------------------------------------------------
#$Date: 2024-10-31 04:58:08 +0200 (Thu, 31 Oct 2024) $
#$Revision: 295686 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312671.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_2312671
loop_
_publ_author_name
'Wzgarda-Raj, Kinga'
'Dominikowska, Justyna'
'Wojtulewski, Sławomir'
'Rybarczyk-Pirek, Agnieszka J'
_publ_section_title
;
 X-ray studies of three 3,6-bis(pyridin-2-yl)-1,2,4,5-tetrazine
 cocrystals: an unexpected molecular conformation stabilized by hydrogen
 bonds.
;
_journal_coeditor_code           DG3037
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              52
_journal_page_last               60
_journal_paper_doi               10.1107/S2053229622012256
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C12 H8 N6, 2C6 H5 N O3'
_chemical_formula_moiety         'C12 H8 N6, 2(C6 H5 N O3)'
_chemical_formula_sum            'C24 H18 N8 O6'
_chemical_formula_weight         514.46
_chemical_name_systematic
;
3,6-Bis(pyridin-2-yl)-1,2,4,5-tetrazine--4-carboxypyridine <i>N</i>-oxide (1/2)
;
_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     iterative
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.835(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.8067(2)
_cell_length_b                   21.3885(7)
_cell_length_c                   14.2669(6)
_cell_measurement_reflns_used    4366
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.1940
_cell_measurement_theta_min      3.8630
_cell_volume                     1105.78(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
olex2.solve (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4052
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
Rigaku OD SuperNova (Dual, Cu at home/near) diffractometer with an Atlas
detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10838
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.488
_diffrn_reflns_theta_min         3.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0682P)^2^+0.2944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                1806
_reflns_number_total             2048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3037sup1.cif
_cod_data_source_block           II
_cod_database_code               2312671
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
   0   0  -1-19.3787 70.9699   1
   0   0   1 5.25468 65.2680  21
   0   0   1-67.1056 86.1910  22
   0   0  -1 161.894 41.4568   2
   0   0  -2 31489.3 1006.19   1
   0   0   2 31941.4 1101.98  22
   0   0   2 30889.7 1103.70  21
   0   0  -2 29589.4 581.440   2
   0   0   3-279.936 319.309  22
   0   0  -3-11.5750 79.7621   2
   0   0  -4 8928.54 445.722   2
   0   0   4 9717.32 908.804  22
   0   0   5 781.540 515.758  22
   0   0  -5-74.8414 89.2605   2
   0   0   6 22880.3 1761.21  22
   0   0  -6 20560.2 750.434   2
   0   0   7 847.471 649.222  22
   0   0  -7-21.9460 265.540   5
   0   0  -8-355.584 311.251   4
   0   0  -8 288.425 274.943   5
   0   0   8 925.843 669.247  22
   0   0  -9-1112.97 491.040   4
   0   0   9-75.9933 493.956  22
   0   0  -9 242.785 324.473   5
   0   0  10 9473.30 1641.45  22
   0   0 -10 7467.37 1310.72   5
   0   0 -10 6861.41 1237.52   4
   0   0 -11 114.546 126.355   9
   0   0 -11-54.6723 173.902  15
   0   0 -12 124313. 2707.88  15
   0   0 -12 127370. 2434.67   9
   0   0 -12 131044. 2540.07   8
   0   0 -13 130.483 149.217  15
   0   0 -13-25.7818 158.796   9
   0   0 -14 1468.23 304.454  15
   0   0  14 1400.93 351.455  14
   0   0 -14 1160.18 333.514   6
   0   0 -14 1279.01 257.049   9
   0   0 -15-45.2707 202.197   6
   0   0  15 139.141 173.854  14
   0   0 -15-46.1120 106.850   9
   0   0 -15-84.4898 153.214  15
   0   0 -16 175.283 105.641  15
   0   0 -16-115.002 142.004   6
   0   0  16-61.0942 124.210  14
   0   0  17 38.2054 68.9645  14
   0   0 -17-14.1462 67.7278   6
   0   1   1 30253.9 774.850   5
   0   1   1 35931.8 847.693   3
   0  -1   1 28871.4 777.789  22
   0  -1  -1 30489.6 593.819  21
   0  -1   1 29056.5 889.798  21
   0   1   1 30686.1 768.882  22
   0   1   1 35771.2 793.719   4
   0   1   1 30322.4 613.479   2
   0  -1  -1 30755.2 653.716  20
   0   1   1 27946.0 583.598  21
   0   1  -1 31092.6 766.368   1
   0   1   2 20175.8 888.725  22
   0  -1   2 21221.0 932.093  22
   0   1  -2 19549.2 875.768   1
   0  -1   2 21148.9 992.344  21
   0   1   2 18703.8 586.850   2
   0   1   2 18931.7 798.398  21
   0  -1  -2 20029.3 603.874  19
   0  -1  -2 19217.4 769.788  21
   0  -1  -2 18633.3 574.146   2
   0  -1  -3 88184.9 1442.68   2
   0   1  -3 92247.4 2163.10   1
   0   1   3 95101.8 2373.97  22
   0   1  -3 87304.5 1043.28   2
   0  -1  -3 89720.6 1709.96  19
   0  -1   3 95790.2 2384.63  22
   0   1   4 1673.81 384.948  22
   0   1  -4 1877.73 467.519   1
   0   1  -4 2268.43 199.154   2
   0  -1  -4 2217.62 263.378   2
   0  -1   5 10161.8 1124.71  22
   0  -1  -5 9556.49 955.416   5
   0   1  -5 8297.74 392.093   2
   0   1   5 9340.85 1029.29  22
   0  -1  -5 8777.44 538.197   2
   0  -1  -6 5061.09 789.601   5
   0  -1  -6 5043.96 435.213   2
   0  -1   6 6972.71 1072.73  22
   0  -1  -6 4997.90 763.719   4
   0   1  -6 4010.48 267.195   2
   0   1   6 5686.52 903.132  22
   0  -1   7 94273.6 3851.54  22
   0   1   7 93080.9 3791.86  22
   0  -1  -7 92009.9 3563.59   5
   0  -1  -7 93264.0 3510.15   4
   0  -1   8 15289.3 1767.20  22
   0   1  -8 17433.1 1709.38   5
   0  -1  -8 17267.4 1656.61   4
   0  -1  -8 15886.4 1637.58   5
   0   1   8 15490.7 1752.73  22
   0   1   9 2318.49 865.918  22
   0  -1  -9 1623.02 497.900   4
   0   1  -9 1842.21 617.288   5
   0  -1  -9 1918.41 590.846   5
   0  -1   9 2761.10 823.251  22
   0   1  -9 2337.76 684.162   4
   0   1  10 13408.3 1871.29  22
   0   1 -10 16178.6 1973.42   5
   0   1 -10 14966.3 1835.77   4
   0  -1 -10 14743.4 1787.51   4
   0  -1 -10 15196.3 1912.54   5
   0  -1  10 16508.2 2047.27  22
   0  -1 -11 371.914 196.818   8
   0  -1 -11 92.1726 148.985   9
   0   1 -11 147.122 154.889  15
   0  -1 -11-37.9036 161.162  15
   0   1 -11 54.7121 121.481   9
   0  -1 -12 8576.22 723.620  15
   0  -1 -12 8501.69 674.390   8
   0  -1 -12 8959.82 644.648   9
   0   1 -12 8525.95 652.378   9
   0   1 -12 7475.83 679.339  15
   0  -1 -13 392.665 190.564   9
   0   1 -13 363.944 242.773  15
   0   1 -13 256.824 192.336   9
   0  -1 -13 85.9723 176.763   8
   0  -1 -13 261.791 187.479  15
   0   1 -14 7327.63 580.903   9
   0  -1  14 9777.82 760.829  14
   0  -1 -14 7459.36 716.111   6
   0   1 -14 8309.90 670.172  15
   0  -1 -14 7057.04 559.702   9
   0  -1 -14 8158.26 653.376  15
   0   1  14 8725.47 721.834  14
   0  -1 -14 7965.71 589.551   8
   0  -1 -15 2354.97 378.153   6
   0  -1  15 2579.58 380.734  14
   0  -1 -15 1964.62 270.680   9
   0   1 -15 2273.80 300.666   9
   0   1 -15 2277.13 378.505   6
   0   1  15 2696.96 374.185  14
   0  -1 -15 2463.33 317.000  15
   0   1 -15 2573.67 339.510  15
   0   1  16 11.6627 117.743  14
   0  -1 -16 220.763 160.548   6
   0  -1  16 195.414 134.293  14
   0  -1 -16 166.898 105.237  15
   0   1 -16 158.446 98.0373  15
   0   1 -16 99.9424 151.139   6
   0   1  17 993.363 146.466  14
   0  -1 -17 888.235 142.021   6
   0   1 -17 877.646 148.806   6
   0  -1  17 1181.30 158.920  14
   0   2   0 5.76223 54.9080   2
   0   2   0-71.7895 64.0453   1
   0   2   0 45.0068 84.3946   3
   0  -2   0 71.8804 59.5280   1
   0   2   0 54.6151 47.4732  20
   0   2   0 2.08029 54.5589  21
   0  -2   0-0.48388 52.1199  20
   0   2   0 40.4978 49.6848   4
   0   2   0 38.3015 52.7970   5
   0   2   1 49111.4 791.752  19
   0   2  -1 50065.8 1056.76   1
   0   2  -1 52666.8 815.998   2
   0  -2   1 51653.0 1303.92  21
   0   2   1 51536.2 1078.08   4
   0   2   1 50947.2 1010.13   2
   0   2   1 53768.5 1195.95   3
   0  -2  -1 48125.0 931.047  20
   0   2   1 51558.8 998.602  20
   0   2   1 52352.4 1146.87   5
   0  -2   1 49219.2 1120.60  22
   0  -2   1 49463.4 1078.71   1
   0   2   2 30940.9 639.944  19
   0  -2  -2 32617.2 607.854  19
   0  -2  -2 36083.6 905.951  21
   0  -2   2 39099.3 1301.93  22
   0   2  -2 36441.7 1209.24   1
   0   2   2 33471.4 1191.98  22
   0  -2  -2 33768.9 912.020   2
   0  -2  -2 36876.3 1035.90  20
   0  -2   2 39276.4 1424.40  21
   0  -2  -3 543.714 172.184   2
   0  -2   3 1428.81 509.274  22
   0   2   3 663.316 296.352  22
   0  -2  -3 633.841 122.660  19
   0  -2  -3 643.460 227.506   4
   0   2  -3 550.016 277.368   1
   0  -2  -4 22515.0 815.941  19
   0  -2   4 23842.3 1471.19  22
   0  -2  -4 24585.8 1316.73   4
   0   2  -4 21799.3 1269.20   1
   0  -2  -4 21088.3 863.994   2
   0   2  -4 20424.5 531.631   2
   0   2   4 21543.6 1364.92  22
   0  -2  -5 32320.6 1135.10   2
   0   2  -5 33125.7 1804.90   1
   0  -2   5 36493.6 2011.47  22
   0   2   5 32444.6 1878.93  22
   0  -2  -5 34277.8 1758.84   4
   0  -2  -5 35206.3 1817.14   5
   0   2  -5 29306.7 615.798   2
   0  -2  -6 50065.3 2349.13   4
   0  -2   6 46104.0 2521.97  22
   0  -2  -6 49873.6 2400.92   5
   0   2   6 46775.3 2482.51  22
   0  -2  -6 48756.8 1471.50   2
   0  -2  -7 76757.6 3240.96   4
   0  -2  -7 75985.7 3269.29   5
   0   2   7 72213.8 3388.70  22
   0  -2   7 71258.6 3407.00  22
   0  -2  -8 5115.62 900.300   4
   0  -2   8 6190.90 1170.82  22
   0  -2  -8 5989.83 995.889   5
   0   2   8 5327.60 1034.10  22
   0   2  -9 8377.29 1307.30   5
   0  -2   9 8702.90 1407.60  22
   0  -2  -9 8863.71 1310.98   4
   0   2   9 8692.32 1433.05  22
   0  -2  -9 9229.87 1368.34   5
   0  -2 -10 5264.95 1022.00   4
   0   2 -10 5244.54 1118.69   4
   0   2  10 6485.88 1353.84  22
   0  -2 -10 4892.12 1118.17   5
   0  -2  10 4788.05 1160.69  22
   0   2 -10 5540.12 1206.32   5
   0   2 -11 21212.3 1111.19  15
   0  -2 -11 20662.1 1048.47   8
   0   2 -11 22794.1 1029.01   9
   0  -2 -11 21564.1 954.122   9
   0  -2 -11 20859.8 1090.37  15
   0  -2 -12 63072.7 1663.92   9
   0   2 -12 61485.3 1923.33  15
   0  -2 -12 62767.8 1916.99  15
   0  -2 -12 63945.8 1848.36   8
   0   2 -12 64728.3 1779.65   9
   0  -2 -13 32153.1 1284.92   8
   0  -2  13 34466.7 1447.85  14
   0  -2 -13 30175.9 1153.29   9
   0   2 -13 32476.5 1369.94  15
   0  -2 -13 31108.0 1321.20  15
   0   2 -13 32112.3 1244.24   9
   0  -2 -14 207.407 152.694   9
   0  -2 -14 234.612 232.283   6
   0  -2 -14 225.299 151.942   8
   0  -2 -14 254.642 178.404  15
   0  -2  14 27.2277 229.377  14
   0   2 -14 258.092 193.548  15
   0   2 -14 142.982 193.942   9
   0   2  15 561.176 203.524  14
   0  -2 -15 937.986 273.877   6
   0  -2 -15 740.106 169.336   9
   0   2 -15 772.820 223.323   9
   0   2 -15 600.087 186.997  15
   0  -2 -15 644.747 168.524   8
   0   2 -15 550.425 234.517   6
   0  -2 -15 734.921 196.210  15
   0  -2  15 633.750 214.556  14
   0  -2 -16 108.700 132.614   6
   0   2 -16 162.004 137.217   6
   0  -2  16 133.109 129.522  14
   0   2 -16 38.7570 91.1331  15
   0  -2 -16 15.2966 84.0079  15
   0   2  16 9.11680 107.727  14
   0   2 -17 3541.40 257.624   6
   0  -2 -17 3131.61 236.847   6
   0   3   0-47.5768 60.6406  20
   0   3   0-9.00695 95.1502   1
   0  -3   0-24.5479 87.5358  20
   0   3   0 30.8290 77.8098  21
   0  -3   0 199.521 104.124   1
   0   3   1 75875.8 1316.04  19
   0   3  -1 78741.6 1265.09   2
   0  -3   1 73503.7 1545.66  22
   0  -3  -1 71703.6 1312.89  20
   0   3   1 78201.6 1421.80  20
   0   3  -1 71425.2 1426.45   1
   0   3  -2-217.862 200.151   1
   0  -3  -2-8.92493 119.314  20
   0  -3  -2 46.5738 124.928   2
   0   3   2-48.1808 80.7611  19
   0   3  -2 10.0978 75.1103   2
   0   3   2-36.7679 161.913  22
   0   3  -3 12839.4 926.913   1
   0  -3  -3 11849.1 670.461   2
   0  -3   3 12717.1 921.364  22
   0  -3  -3 12936.4 665.028  21
   0   3   3 11875.2 901.585  22
   0  -3  -3 13533.3 843.646   4
   0   3   4 582.312 345.521  22
   0  -3  -4 595.699 295.939   4
   0   3  -4 517.522 266.839   1
   0  -3  -4 563.505 254.457   5
   0  -3  -4 565.834 202.505   2
   0  -3   4 663.791 380.985  22
   0  -3   5 50122.3 2368.81  22
   0  -3  -5 45446.9 2007.60   4
   0   3  -5 46327.5 2122.13   1
   0  -3  -5 44299.4 2087.97   5
   0  -3  -5 43580.0 1446.24   2
   0   3   5 44768.7 2233.29  22
   0  -3  -6 6119.46 825.608   4
   0  -3  -6 5827.04 852.231   5
   0  -3   6 6444.07 1005.01  22
   0   3  -6 6442.63 929.925   1
   0  -3  -6 6781.42 605.309   2
   0   3   6 4911.13 857.088  22
   0  -3  -7 26945.5 1973.58   5
   0  -3   7 28148.9 2143.76  22
   0   3   7 25231.0 2015.62  22
   0  -3  -7 25524.2 1207.99   2
   0  -3  -7 24698.6 1811.60   4
   0  -3  -8 675.677 403.238   4
   0   3   8 615.924 419.368  22
   0  -3  -8 698.117 389.264   5
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   1   2  -7 128641. 4141.83   1
   1  -2  -7 121213. 3919.37   5
   1  -2  -7 124551. 3147.68   4
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   1   2  -6 24357.8 1684.00   1
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   2   6  -2 159556. 5183.69   1
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   2   7 -14 842.854 222.246   7
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   2   7 -13 34889.9 1352.21   7
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   2   7  -4 128637. 4852.96   1
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   2  -7  -3 115470. 4314.73  20
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   2   7  -3 110991. 4488.28   1
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   2   8 -11 56916.6 1851.76   7
   2  -8 -10 25414.3 1163.69   6
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   2   8  -3 204004. 6289.88   1
   2  -8  -3 198535. 5874.07  20
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   2   8  -2 617.004 377.383   1
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   2  -8   1 10190.0 1470.16  20
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   2  -9 -15 368.664 209.965   8
   2  -9 -14 5713.53 490.790   6
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   2  -9 -14 6248.24 582.971   8
   2   9 -14 5905.56 494.549   7
   2  -9 -13 28658.9 1139.54   6
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   2  -9 -13 29493.2 1279.22   8
   2   9 -13 29442.7 1211.59   7
   2  -9 -12 6418.30 577.137   6
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   2  -9 -12 7537.57 702.560   8
   2   9 -12 6509.71 651.278   7
   2  -9 -11 10713.0 761.131   6
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   2  -9 -11 10869.9 828.681   8
   2   9 -11 11934.8 865.687   7
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   2   9 -10 147.603 220.372   7
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   2  -9  -9 6497.89 647.690   8
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   2  -9  -8 28314.5 1163.77   6
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   2  -9  -8 28643.7 1289.54   8
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   2  -9  -7 4680.42 997.880  20
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   2   9  -7 3965.60 980.430   1
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   2  -9  -6 3746.72 901.285  20
   2   9  -6 3363.15 940.101   1
  -2   9   6 4749.09 1306.51  19
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  -4 -13   8 213.226 118.003   9
  -4 -13   8 64.4390 66.0646  10
   4 -13  -8 60.1891 68.8571  17
  -4 -13   7 1523.32 218.386   9
  -4 -13   7 1702.41 190.452  10
   4 -13  -7 1883.71 206.823  17
  -4 -13   6 268.026 131.493   9
  -4 -13   6 386.343 121.656  10
   4 -13  -6 581.387 133.781  17
  -4 -13   6 268.754 115.090  16
  -4 -13   5 2824.34 259.575  10
   4 -13  -5 2489.71 235.315  17
  -4 -13   5 2509.79 279.919  16
  -4 -13   5 2263.17 268.067   9
  -4 -13   4 20958.1 657.883  10
   4 -13  -4 19271.0 607.989  17
  -4 -13   4 20336.1 780.446  16
  -4 -13   4 19116.7 732.152   9
  -4 -13   3 1824.66 229.859   9
  -4 -13   3 2454.15 226.991  10
   4 -13  -3 1985.59 178.943  17
  -4 -13   3 2342.42 283.123  16
  -4 -13   2 63.2463 86.5448   9
  -4 -13   2 226.612 83.4723  10
  -4 -13   2 182.741 117.733  16
  -4 -13   1 823.475 140.658   9
  -4 -13   1 991.803 174.431  16
  -4 -14   7 8653.23 357.190  10
   4 -14  -7 9358.16 384.992  17
  -4 -14   6 402.828 124.487   9
  -4 -14   6 288.458 89.3185  10
   4 -14  -6 326.876 90.2214  17
  -4 -14   6 402.273 115.041  16
  -4 -14   5 8258.08 377.771  10
   4 -14  -5 7914.18 370.784  17
  -4 -14   5 8255.25 438.382  16
  -4 -14   4 14534.2 491.075  10
   4 -14  -4 12976.4 444.005  17
  -4 -14   4 14788.1 596.852  16
  -4 -14   3 1141.21 137.816  10
  -4 -14   3 1444.75 195.626  16
  -4 -14   2-1.17496 79.0762  16
   0   0   0    0.00    0.00   0
TITL exp_3062 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   3.806743  21.388506  14.266923  90.0000 107.8350  90.0000
ZERR    5.00   0.000168   0.000704   0.000601   0.0000   0.0047   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 55.00 50.00 5.00 5.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum              84216
_shelx_res_file
;
TITL
    exp_3062.res
    created by SHELXL-2018/3 at 15:18:41 on 06-Dec-2022
CELL 1.54184 3.8067 21.3885 14.2669 90 107.835 90
ZERR 2 0.0002 0.0007 0.0006 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 48 36 16 12
EQIV $1 +X,0.5-Y,-0.5+Z
EQIV $2 -X,1-Y,1-Z
L.S. 5
PLAN  1
HTAB C12 N2_$2
HTAB C12 N32_$2
HTAB O142 O11_$1
HTAB O142 N11_$1
CONF
BOND
BOND $H
fmap 2
acta
MERG 2
OMIT 0 137
REM <olex2.extras>
REM <HklSrc "%.\\exp_3062.hkl">
REM </olex2.extras>
WGHT    0.068200    0.294400
FVAR       6.67847
O11   4    0.048173    0.365039    0.881974    11.00000    0.02876    0.01437 =
         0.01198   -0.00182    0.00581    0.00144
O141  4   -0.132752    0.284628    0.445416    11.00000    0.02165    0.01638 =
         0.01289    0.00141    0.00122    0.00004
O142  4    0.156469    0.201333    0.531354    11.00000    0.02928    0.01422 =
         0.01417   -0.00036    0.00386    0.00505
N11   3    0.045826    0.339483    0.797004    11.00000    0.01509    0.01235 =
         0.01136   -0.00119    0.00303   -0.00223
N1    3    1.150990    0.448885    0.470447    11.00000    0.01712    0.01368 =
         0.01578    0.00017    0.00337   -0.00041
N2    3    0.737207    0.535492    0.435535    11.00000    0.01771    0.01259 =
         0.01647    0.00003    0.00366    0.00128
N32   3    0.566224    0.510144    0.241117    11.00000    0.01637    0.01390 =
         0.01737    0.00125    0.00354    0.00026
C13   1   -0.152160    0.342220    0.623218    11.00000    0.01198    0.01253 =
         0.01305    0.00251    0.00106   -0.00157
AFIX  43
H13   2   -0.279926    0.362247    0.564875    11.00000   -1.20000
AFIX   0
C12   1   -0.142242    0.368409    0.712272    11.00000    0.01365    0.01044 =
         0.01526    0.00204    0.00249   -0.00109
AFIX  43
H12   2   -0.264466    0.405830    0.714041    11.00000   -1.20000
AFIX   0
C141  1    0.008013    0.257573    0.522716    11.00000    0.01207    0.01260 =
         0.01519    0.00020    0.00319   -0.00325
C15   1    0.219187    0.257468    0.708814    11.00000    0.01225    0.01141 =
         0.01685    0.00046    0.00363   -0.00076
AFIX  43
H15   2    0.341600    0.219858    0.708654    11.00000   -1.20000
AFIX   0
C16   1    0.227427    0.284801    0.796621    11.00000    0.01297    0.01169 =
         0.01511    0.00194    0.00123    0.00039
AFIX  43
H16   2    0.357243    0.265892    0.855793    11.00000   -1.20000
AFIX   0
C14   1    0.028062    0.285931    0.620085    11.00000    0.01062    0.01138 =
         0.01431   -0.00022    0.00315   -0.00356
C3    1    0.891013    0.484557    0.408300    11.00000    0.01291    0.00980 =
         0.01799    0.00214    0.00505   -0.00109
C35   1    0.739683    0.396013    0.171794    11.00000    0.01766    0.01389 =
         0.02254   -0.00397    0.00668   -0.00087
AFIX  43
H35   2    0.797713    0.358080    0.148287    11.00000   -1.20000
AFIX   0
C34   1    0.529994    0.440193    0.107202    11.00000    0.01815    0.01991 =
         0.01716   -0.00178    0.00544   -0.00254
AFIX  43
H34   2    0.444011    0.432303    0.039907    11.00000   -1.20000
AFIX   0
C33   1    0.451560    0.496308    0.145165    11.00000    0.01805    0.01490 =
         0.01642    0.00142    0.00244   -0.00009
AFIX  43
H33   2    0.311986    0.525837    0.101626    11.00000   -1.20000
AFIX   0
C36   1    0.861519    0.409147    0.271791    11.00000    0.01514    0.01324 =
         0.02060   -0.00049    0.00417    0.00025
AFIX  43
H36   2    1.000670    0.380298    0.316770    11.00000   -1.20000
AFIX   0
C31   1    0.768695    0.467041    0.302805    11.00000    0.01230    0.01266 =
         0.01623    0.00016    0.00456   -0.00140
H142  2    0.098079    0.179373    0.461469    11.00000    0.04245
HKLF 4
REM
REM wR2 = 0.1110, GooF = S = 1.068, Restrained GooF = 1.068 for all data
REM R1 = 0.0421 for 1806 Fo > 4sig(Fo) and 0.0475 for all 2048 data
REM 176 parameters refined using 0 restraints
END
WGHT      0.0682      0.2944
REM Highest difference peak  0.241,  deepest hole -0.296,  1-sigma level  0.058
Q1    1   0.4773  0.2083  0.5637  11.00000  0.05    0.24
;
_shelx_res_checksum              30034
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
O O11 0.0482(3) 0.36504(5) 0.88197(8) 0.0185(3) Uani d 1 . .
O O141 -0.1328(3) 0.28463(5) 0.44542(8) 0.0179(3) Uani d 1 . .
O O142 0.1565(3) 0.20133(5) 0.53135(8) 0.0199(3) Uani d 1 . .
N N11 0.0458(3) 0.33948(6) 0.79700(9) 0.0132(3) Uani d 1 . .
N N1 1.1510(3) 0.44888(6) 0.47045(10) 0.0159(3) Uani d 1 . .
N N2 0.7372(4) 0.53549(6) 0.43554(10) 0.0159(3) Uani d 1 . .
N N32 0.5662(3) 0.51014(6) 0.24112(10) 0.0162(3) Uani d 1 . .
C C13 -0.1522(4) 0.34222(7) 0.62322(11) 0.0131(3) Uani d 1 . .
H H13 -0.279926 0.362247 0.564875 0.016 Uiso calc 1 . .
C C12 -0.1422(4) 0.36841(7) 0.71227(11) 0.0136(3) Uani d 1 . .
H H12 -0.264466 0.405830 0.714041 0.016 Uiso calc 1 . .
C C141 0.0080(4) 0.25757(7) 0.52272(11) 0.0135(3) Uani d 1 . .
C C15 0.2192(4) 0.25747(7) 0.70881(11) 0.0137(3) Uani d 1 . .
H H15 0.341600 0.219858 0.708654 0.016 Uiso calc 1 . .
C C16 0.2274(4) 0.28480(7) 0.79662(11) 0.0139(3) Uani d 1 . .
H H16 0.357243 0.265892 0.855793 0.017 Uiso calc 1 . .
C C14 0.0281(4) 0.28593(7) 0.62008(11) 0.0123(3) Uani d 1 . .
C C3 0.8910(4) 0.48456(7) 0.40830(11) 0.0135(3) Uani d 1 . .
C C35 0.7397(4) 0.39601(7) 0.17179(12) 0.0179(3) Uani d 1 . .
H H35 0.797713 0.358080 0.148287 0.021 Uiso calc 1 . .
C C34 0.5300(4) 0.44019(8) 0.10720(12) 0.0184(3) Uani d 1 . .
H H34 0.444011 0.432303 0.039907 0.022 Uiso calc 1 . .
C C33 0.4516(4) 0.49631(7) 0.14517(11) 0.0171(3) Uani d 1 . .
H H33 0.311986 0.525837 0.101626 0.021 Uiso calc 1 . .
C C36 0.8615(4) 0.40915(7) 0.27179(12) 0.0166(3) Uani d 1 . .
H H36 1.000670 0.380298 0.316770 0.020 Uiso calc 1 . .
C C31 0.7687(4) 0.46704(7) 0.30281(11) 0.0137(3) Uani d 1 . .
H H142 0.098(7) 0.1794(12) 0.4615(19) 0.042(7) 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
O11 0.0288(6) 0.0144(5) 0.0120(5) 0.0014(4) 0.0058(4) -0.0018(4)
O141 0.0216(6) 0.0164(5) 0.0129(5) 0.0000(4) 0.0012(4) 0.0014(4)
O142 0.0293(6) 0.0142(5) 0.0142(5) 0.0050(4) 0.0039(5) -0.0004(4)
N11 0.0151(6) 0.0124(6) 0.0114(6) -0.0022(5) 0.0030(5) -0.0012(5)
N1 0.0171(6) 0.0137(6) 0.0158(6) -0.0004(5) 0.0034(5) 0.0002(5)
N2 0.0177(6) 0.0126(6) 0.0165(6) 0.0013(5) 0.0037(5) 0.0000(5)
N32 0.0164(6) 0.0139(6) 0.0174(6) 0.0003(5) 0.0035(5) 0.0012(5)
C13 0.0120(6) 0.0125(7) 0.0130(7) -0.0016(5) 0.0011(5) 0.0025(5)
C12 0.0137(7) 0.0104(7) 0.0153(7) -0.0011(5) 0.0025(5) 0.0020(5)
C141 0.0121(6) 0.0126(7) 0.0152(7) -0.0033(5) 0.0032(5) 0.0002(5)
C15 0.0123(6) 0.0114(7) 0.0168(7) -0.0008(5) 0.0036(5) 0.0005(5)
C16 0.0130(7) 0.0117(7) 0.0151(7) 0.0004(5) 0.0012(5) 0.0019(5)
C14 0.0106(7) 0.0114(7) 0.0143(8) -0.0036(5) 0.0032(5) -0.0002(5)
C3 0.0129(7) 0.0098(7) 0.0180(8) -0.0011(5) 0.0050(6) 0.0021(5)
C35 0.0177(7) 0.0139(7) 0.0225(8) -0.0009(6) 0.0067(6) -0.0040(6)
C34 0.0181(7) 0.0199(8) 0.0172(7) -0.0025(6) 0.0054(6) -0.0018(6)
C33 0.0181(7) 0.0149(7) 0.0164(7) -0.0001(6) 0.0024(6) 0.0014(6)
C36 0.0151(7) 0.0132(7) 0.0206(8) 0.0002(6) 0.0042(6) -0.0005(6)
C31 0.0123(7) 0.0127(7) 0.0162(7) -0.0014(5) 0.0046(6) 0.0002(6)
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
C141 O142 H142 . . 110.8(13) ?
O11 N11 C12 . . 118.81(13) ?
O11 N11 C16 . . 119.79(12) ?
C12 N11 C16 . . 121.40(13) ?
N2 N1 C3 3_766 . 117.99(13) ?
N1 N2 C3 3_766 . 117.63(13) ?
C33 N32 C31 . . 117.46(13) ?
C12 C13 H13 . . 119.8 ?
C12 C13 C14 . . 120.40(13) ?
C14 C13 H13 . . 119.8 ?
N11 C12 C13 . . 119.73(14) ?
N11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
O141 C141 O142 . . 125.21(14) ?
O141 C141 C14 . . 122.18(14) ?
O142 C141 C14 . . 112.61(13) ?
C16 C15 H15 . . 119.9 ?
C16 C15 C14 . . 120.17(14) ?
C14 C15 H15 . . 119.9 ?
N11 C16 C15 . . 120.00(13) ?
N11 C16 H16 . . 120.0 ?
C15 C16 H16 . . 120.0 ?
C13 C14 C141 . . 119.64(13) ?
C15 C14 C13 . . 118.30(13) ?
C15 C14 C141 . . 122.06(13) ?
N1 C3 N2 . . 124.38(14) ?
N1 C3 C31 . . 117.72(14) ?
N2 C3 C31 . . 117.90(13) ?
C34 C35 H35 . . 120.4 ?
C36 C35 H35 . . 120.4 ?
C36 C35 C34 . . 119.20(14) ?
C35 C34 H34 . . 120.7 ?
C33 C34 C35 . . 118.59(15) ?
C33 C34 H34 . . 120.7 ?
N32 C33 C34 . . 123.37(14) ?
N32 C33 H33 . . 118.3 ?
C34 C33 H33 . . 118.3 ?
C35 C36 H36 . . 121.0 ?
C35 C36 C31 . . 117.92(14) ?
C31 C36 H36 . . 121.0 ?
N32 C31 C3 . . 115.54(13) ?
N32 C31 C36 . . 123.46(14) ?
C36 C31 C3 . . 121.00(13) ?
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
O11 N11 . 1.3273(16) ?
O141 C141 . 1.2150(19) ?
O142 C141 . 1.3187(19) ?
O142 H142 . 1.06(3) ?
N11 C12 . 1.3515(19) ?
N11 C16 . 1.359(2) ?
N1 N2 3_766 1.3200(18) ?
N1 C3 . 1.3454(19) ?
N2 C3 . 1.349(2) ?
N32 C33 . 1.336(2) ?
N32 C31 . 1.343(2) ?
C13 H13 . 0.9300 ?
C13 C12 . 1.378(2) ?
C13 C14 . 1.393(2) ?
C12 H12 . 0.9300 ?
C141 C14 . 1.496(2) ?
C15 H15 . 0.9300 ?
C15 C16 . 1.374(2) ?
C15 C14 . 1.392(2) ?
C16 H16 . 0.9300 ?
C3 C31 . 1.481(2) ?
C35 H35 . 0.9300 ?
C35 C34 . 1.389(2) ?
C35 C36 . 1.387(2) ?
C34 H34 . 0.9300 ?
C34 C33 . 1.386(2) ?
C33 H33 . 0.9300 ?
C36 H36 . 0.9300 ?
C36 C31 . 1.396(2) ?
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
C12 H12 N2 3_566 0.93 2.65 3.2978(19) 127.4 yes
C12 H12 N32 3_566 0.93 2.33 3.2329(19) 165.0 yes
O142 H142 O11 4_565 1.06(3) 1.45(3) 2.4878(15) 165(2) yes
O142 H142 N11 4_565 1.06(3) 2.33(3) 3.3549(17) 162(2) 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
O11 N11 C12 C13 . . . . -179.15(12) ?
O11 N11 C16 C15 . . . . 178.60(13) ?
O141 C141 C14 C13 . . . . 6.8(2) ?
O141 C141 C14 C15 . . . . -173.91(13) ?
O142 C141 C14 C13 . . . . -172.98(13) ?
O142 C141 C14 C15 . . . . 6.3(2) ?
N1 N2 C3 N1 3_766 . . . -0.2(2) ?
N1 N2 C3 C31 3_766 . . . -179.57(12) ?
N1 C3 C31 N32 . . . . -167.38(13) ?
N1 C3 C31 C36 . . . . 12.7(2) ?
N2 N1 C3 N2 3_766 . . . 0.2(2) ?
N2 N1 C3 C31 3_766 . . . 179.58(12) ?
N2 C3 C31 N32 . . . . 12.00(19) ?
N2 C3 C31 C36 . . . . -167.89(14) ?
C12 N11 C16 C15 . . . . -0.6(2) ?
C12 C13 C14 C141 . . . . 178.80(13) ?
C12 C13 C14 C15 . . . . -0.5(2) ?
C16 N11 C12 C13 . . . . 0.1(2) ?
C16 C15 C14 C13 . . . . 0.0(2) ?
C16 C15 C14 C141 . . . . -179.32(13) ?
C14 C13 C12 N11 . . . . 0.5(2) ?
C14 C15 C16 N11 . . . . 0.6(2) ?
C35 C34 C33 N32 . . . . -0.3(2) ?
C35 C36 C31 N32 . . . . 0.5(2) ?
C35 C36 C31 C3 . . . . -179.58(13) ?
C34 C35 C36 C31 . . . . -0.5(2) ?
C33 N32 C31 C3 . . . . 179.71(12) ?
C33 N32 C31 C36 . . . . -0.4(2) ?
C36 C35 C34 C33 . . . . 0.4(2) ?
C31 N32 C33 C34 . . . . 0.3(2) ?

_cod_database_fobs_code 2312671