#------------------------------------------------------------------------------
#$Date: 2025-04-09 04:15:37 +0200 (Wed, 09 Apr 2025) $
#$Revision: 299231 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023462.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_2023462
loop_
_publ_author_name
'Faraj, Imane'
'El Ghayati, Lhoussaine'
'Blacque, Olivier'
'H\"okelek, Tuncer'
'Mazzah, Ahmed'
'Essassi, El Mokhtar'
'Sebbar, Nada Kheira'
_publ_section_title
;
 Synthesis and crystal structure of
 2-(2,4-dioxo-6-methylpyran-3-ylidene)-4-(4-hydroxyphenyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine
;
_journal_coeditor_code           HB8131
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989025003032
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C21 H18 N2 O4'
_chemical_formula_moiety         'C21 H18 N2 O4'
_chemical_formula_sum            'C21 H18 N2 O4'
_chemical_formula_weight         362.37
_chemical_name_systematic
4-(4-Hydroxyphenyl)-2-(6-methyl-2,4-dioxopyran-3-ylidene)-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_cell_angle_alpha                100.967(2)
_cell_angle_beta                 97.373(2)
_cell_angle_gamma                100.127(2)
_cell_formula_units_Z            2
_cell_length_a                   6.37570(10)
_cell_length_b                   7.75060(10)
_cell_length_c                   17.9997(4)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      79.1140
_cell_measurement_theta_min      2.5240
_cell_volume                     847.49(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.5-ac6-012 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5-ac6-012 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18745
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.437
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.315
_refine_ls_extinction_coef       0.0020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0570P)^2^+0.3065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3159
_reflns_number_total             3608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8131.cif
_cod_data_source_block           I
_cod_database_code               2023462
_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   0.923
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_file
;
   0   0  -1 2732.51 81.5766  10
   0   0  -1 2606.60 81.1302   7
   0   0  -1 2800.53 81.6189  13
   0   0  -2 8415.54 254.159  10
   0   0  -2 8709.19 254.151  13
   0   0  -2 8314.77 253.311   7
   0   0  -3 23074.3 679.925  13
   0   0  -3 22501.7 678.727   7
   0   0  -4 7.38896 12.1122  13
   0   0  -4 4.04802 9.60481   7
   0   0  -5 3434.10 109.737  13
   0   0  -6 705.526 31.4002  13
   0   0  -7 1502.57 56.7428  13
   0   0   8 3880.05 118.829  18
   0   0  -8 3942.55 127.921  13
   0   0   8 3755.74 118.930  14
   0   0   9 437.293 20.4075  18
   0   0   9 443.615 21.0568  14
   0   0  -9 468.692 29.4401  13
   0   0 -10 150.992 19.9953  13
   0   0  10 153.162 14.4568  14
   0   0 -11 1617.24 66.8679  13
   0   0  11 1630.37 56.5434  14
   0   0  12 2122.14 70.3833  49
   0   0 -12 2104.74 82.7359  13
   0   0  12 2019.97 71.5363  14
   0   0  12 2093.88 70.2460  55
   0   0  12 2186.66 70.5418  30
   0   0  13 534.524 24.4323  37
   0   0  13 549.586 27.9675  14
   0   0  13 587.083 26.0828  55
   0   0  13 570.097 25.6840  49
   0   0  13 533.818 25.3335  30
   0   0 -13 595.696 25.7720  20
   0   0  14 20.4482 15.3572  14
   0   0  14 12.2910 12.4479  30
   0   0 -14 1.82221 11.0543  20
   0   0  14 18.1691 10.9378  37
   0   0  14-3.88612 12.5620  55
   0   0  14 1.94072 12.0193  49
   0   0  15 446.687 23.4220  49
   0   0  15 432.489 24.5303  55
   0   0 -15 456.078 23.2162  20
   0   0  15 474.030 24.2720  30
   0   0  15 440.108 24.7827  29
   0   0  16 14.2095 12.6146  49
   0   0 -16 10.8500 11.5676  20
   0   0  16 5.61427 13.6932  29
   0   0  16 11.6094 13.1955  30
   0   0  16 17.2391 14.4840  55
   0   0  17 45.9390 14.0315  55
   0   0  17 41.4054 12.7858  49
   0   0  17 43.8988 13.2252  30
   0   0  17 40.5588 14.5950  29
   0   0 -17 49.4993 11.5092  20
   0   0  17 44.3166 15.0004  16
   0   0  18 12.4470 10.3919  54
   0   0  18 13.6706 12.0820  30
   0   0  18 20.9204 13.0853  29
   0   0  18 9.94942 11.9287  49
   0   0  18 12.2034 13.3936  16
   0   0 -18 8.70181 9.32851  20
   0   0  18 3.00034 10.5052  38
   0   0  19 104.281 10.7237  54
   0   0  19 102.244 12.5671  49
   0   0  19 93.6826 13.3153  16
   0   0 -19 65.7312 9.26968  25
   0   0  19 104.173 12.9593  30
   0   0  19 92.8038 13.3762  29
   0   0  19 101.084 10.5980  38
   0   0  20-1.16491 9.05239  49
   0   0  20 1.39394 9.29784  16
   0   0  20 10.8628 9.87773  29
   0   0  21 19.0017 6.78150  16
   0   0  21 20.9116 7.72275  29
   0   0  22 20.6174 5.15009  23
   0   0  22 22.9593 4.16500  29
   0   0  22 29.6905 5.15130  22
   0  -1  22-3.92847 4.99059  29
   0  -1  21 211.963 12.2768  29
   0  -1  21 185.397 11.8642  16
   0  -1  20 19.7148 8.24699  38
   0  -1  20 4.00834 9.66478  16
   0  -1  20 13.3924 8.44249  54
   0  -1  20 4.09973 10.2506  29
   0  -1  19 51.4766 11.3089  49
   0  -1  19 45.4662 10.3538  38
   0  -1  19 37.7263 12.7940  16
   0  -1  19 28.6732 10.6219  54
   0  -1  19 75.7385 13.0527  29
   0  -1  19 64.0658 13.4373  30
   0  -1  18-5.83943 11.7918  49
   0  -1  18-4.52548 11.6278  38
   0  -1  18 2.76640 12.9706  16
   0  -1  18 0.58689 11.6568  54
   0  -1  18-8.94010 13.4542  30
   0  -1  18 0.63536 12.8184  29
   0  -1  17 2239.18 75.9499  49
   0  -1  17 2244.44 75.9636  38
   0  -1  17 2111.09 77.0648  16
   0  -1  17 2242.65 76.8375  30
   0  -1  17 2434.98 77.2733  29
   0  -1  17 2293.69 76.3837  54
   0  -1  16 28.6603 12.7980  37
   0  -1  16 57.6114 14.7853  30
   0  -1  16 53.6364 14.2892  29
   0  -1  16 40.4346 12.4388  49
   0  -1  15 362.726 20.4615  49
   0  -1  15 335.282 21.4389  30
   0  -1  15 380.980 21.7371  29
   0  -1  15 324.533 20.1673  37
   0  -1  14 218.660 16.2859  49
   0  -1  14 206.245 16.8552  37
   0  -1  14 223.394 17.1096  30
   0  -1  14 228.874 16.9500  29
   0  -1  13 121.756 13.0121  49
   0  -1  13 116.520 13.1453  37
   0  -1  13 107.358 16.3601  14
   0  -1  13 132.815 14.0765  30
   0  -1  13 98.1912 13.5131  29
   0  -1  12 1267.41 45.6967  37
   0  -1  12 1307.24 46.3832  30
   0  -1  12 1354.58 46.2994  29
   0  -1  12 1250.47 47.1175  14
   0  -1  11 6271.89 193.711  14
   0  -1  11 6285.26 193.813  18
   0  -1  10 1586.24 54.2328  14
   0  -1  10 1603.30 54.0968  18
   0  -1   9 8519.93 256.100  14
   0   1  -9 8276.05 261.255  13
   0   1  -8 14146.1 429.226  13
   0   1  -7 22885.0 687.194  13
   0   1  -6 1973.99 63.3623  13
   0  -1   6 1900.99 60.6536   3
   0   1  -5 1674.46 53.1956  13
   0  -1   5 1608.05 52.5299   3
   0  -1   4 2318.45 73.0433   3
   0  -1   4 2351.60 74.2676   2
   0  -1   4 2310.01 74.1552   1
   0  -1   3 728.532 32.9291   9
   0  -1   3 753.892 26.0459   3
   0  -1   3 709.637 27.4862   2
   0  -1   3 687.365 27.3471   1
   0  -1   2 21.4134 3.40230   8
   0  -1   2 20.8692 14.2946   9
   0  -1   1 12636.7 389.714   9
   0  -1   1 12991.3 385.283  10
   0  -1   1 12890.8 385.419  11
   0  -1   0 1614.22 51.1381   3
   0  -1   0 1602.51 52.8466   2
   0  -1   0 1590.32 52.8374   1
   0  -1   0 1559.13 50.5736  13
   0  -1  -1 5703.70 175.376   7
   0  -1  -1 5748.73 176.046   1
   0  -1  -1 5716.32 176.054   2
   0  -1  -1 5823.36 174.601   3
   0  -1  -2 10751.2 329.064   7
   0  -1  -2 10994.2 328.720   1
   0  -1  -2 10831.4 327.185   3
   0  -1  -2 11018.2 328.819   2
   0  -1  -3 3750.24 114.479   3
   0  -1  -3 3672.95 116.256   2
   0  -1  -3 3602.13 118.274   7
   0  -1  -3 3822.87 116.290   1
   0  -1  -4 1086.18 39.9211  13
   0  -1  -4 866.630 34.3761   2
   0  -1  -4 1008.12 40.0085  10
   0  -1  -4 858.316 34.4580   1
   0  -1  -4 1007.94 32.6002   3
   0  -1  -5 1322.57 42.6585   3
   0  -1  -5 1332.47 51.6104  13
   0  -1  -6 47.7314 17.1397  13
   0  -1  -7 344.595 26.1850  13
   0   1   8 2832.15 90.5890  14
   0  -1  -8 2978.41 103.582  13
   0   1   9 3993.65 125.830  14
   0  -1  -9 4119.65 140.712  13
   0  -1 -10 712.954 43.0884  13
   0   1  10 753.541 30.5699  14
   0   1  11 3314.89 111.205  14
   0  -1 -11 3700.46 128.806  13
   0   1  11 3557.49 110.277  30
   0  -1 -11 3451.89 111.067  20
   0   1  11 3497.54 110.211  55
   0   1  12 687.087 31.6119  14
   0  -1 -12 779.434 46.2845  13
   0   1  12 712.680 29.8666  30
   0  -1 -12 719.396 30.6312  20
   0   1  12 717.844 29.7364  55
   0   1  13 7.49976 15.2261  14
   0  -1 -13-2.31496 18.1100  13
   0  -1 -13 6.66217 12.5596  20
   0   1  13-5.48634 11.7864  30
   0   1  13-4.91841 11.5542  55
   0  -1 -14 219.871 17.9028  20
   0   1  14 226.401 17.4114  30
   0   1  14 238.402 17.9672  55
   0  -1 -15 171.398 16.6102  20
   0   1  15 161.226 15.8021  30
   0   1  15 127.530 16.0222  55
   0  -1 -16 160.240 16.3966  20
   0   1  16 164.715 15.4691  30
   0   1  16 122.886 16.1999  55
   0   1  17 432.112 22.3743  55
   0   1  17 390.547 21.4871  30
   0  -1 -17 393.892 21.7619  20
   0   1  17 404.784 23.1678  16
   0   1  18 19.7787 10.9530  30
   0   1  18 26.7869 9.32094  38
   0  -1 -18 30.2885 10.7755  20
   0   1  18 14.4696 12.0620  16
   0   1  19 70.3898 10.3867  30
   0   1  19 76.7982 11.9230  29
   0   1  19 69.2762 11.2659  16
   0  -1 -19 85.8103 9.19437  25
   0   1  20 8.31054 8.65517  29
   0   1  20 19.4893 7.90934  49
   0  -1 -20 16.2072 5.48032  25
   0   1  20 14.6046 7.53804  16
   0   1  21 220.278 10.3295  29
   0  -2  22 141.551 8.17291  29
   0  -2  22 121.102 8.77030  35
   0  -2  21 58.4594 8.98417  29
   0  -2  21 55.4890 7.19894  38
   0  -2  21 40.6544 8.32180  16
   0  -2  20 12.3347 9.18995  54
   0  -2  20 0.45757 10.2101  29
   0  -2  20 19.8246 9.23445  38
   0  -2  20 26.6157 10.3017  16
   0  -2  19 483.710 23.0911  54
   0  -2  19 459.447 23.0446  29
   0  -2  19 485.378 22.5607  38
   0  -2  19 464.995 22.7042  16
   0  -2  18 1138.78 42.7461  54
   0  -2  18 1100.19 42.8515  16
   0  -2  18 1174.25 43.5265  29
   0  -2  18 1138.45 42.3592  38
   0  -2  17 1301.98 47.8963  30
   0  -2  17 1279.96 47.3955  29
   0  -2  17 1294.78 47.5858  54
   0  -2  17 1254.90 45.9713  49
   0  -2  17 1246.10 44.8933  41
   0  -2  17 1252.38 47.4119  16
   0  -2  17 1213.23 46.7102  37
   0  -2  17 1227.84 46.8455  38
   0  -2  16 589.029 27.0923  29
   0  -2  16 613.041 28.3247  54
   0  -2  16 538.872 25.9529  49
   0  -2  16 555.432 25.1834  41
   0  -2  16 603.977 27.7517  16
   0  -2  16 566.037 27.2866  37
   0  -2  16 525.329 27.1402  38
   0  -2  15 344.767 21.3088  29
   0  -2  15 379.690 21.6464  38
   0  -2  15 356.300 21.8600  37
   0  -2  15 366.180 21.9162  54
   0  -2  15 342.075 19.1396  41
   0  -2  15 343.812 19.9926  49
   0  -2  14 102.569 14.1676  29
   0  -2  14 125.789 14.9442  37
   0  -2  14 119.760 13.5261  49
   0  -2  14 132.084 12.9823  41
   0  -2  14 129.557 15.2813  38
   0  -2  13 442.221 21.8887  55
   0  -2  13 432.632 22.4397  31
   0  -2  13 409.174 22.2594  32
   0  -2  13 422.501 20.4764  49
   0  -2  13 422.661 21.8319  29
   0  -2  13 432.899 22.0744  37
   0  -2  13 434.232 22.4447  38
   0  -2  13 424.273 20.9082  41
   0  -2  12 84.6446 12.4060  32
   0  -2  12 94.0033 12.5628  31
   0  -2  12 87.1763 12.0891  55
   0  -2  12 67.6023 12.9898  14
   0  -2  12 75.9180 13.1336  18
   0  -2  12 113.160 12.6832  29
   0  -2  12 98.7535 12.8016  37
   0  -2  11 1493.52 52.5539  14
   0  -2  11 1596.70 53.1880  18
   0  -2  11 1470.05 55.6822   8
   0  -2  10 2460.28 77.8517  18
   0  -2  10 2343.95 77.5080  14
   0  -2   9 2338.09 79.4939   3
   0  -2   9 2517.55 78.7924  14
   0  -2   9 2511.07 79.1484  18
   0  -2   9 2500.33 81.3247   8
   0  -2   8 1994.12 67.9697   3
   0  -2   8 2079.89 65.5492  18
   0  -2   8 2002.77 66.7608   8
   0  -2   7 5132.69 161.027   8
   0  -2   7 5489.36 164.476   3
   0  -2   6 3266.18 101.810   1
   0  -2   6 3280.67 102.151   2
   0  -2   6 2985.04 94.5829   8
   0  -2   6 3036.07 99.4014   3
   0   2  -5 5535.99 168.509  12
   0  -2   5 6241.59 178.272   1
   0  -2   5 6211.26 175.739   3
   0  -2   5 6198.38 178.352   2
   0  -2   5 5377.89 168.641   8
   0  -2   5 5815.54 170.093  11
   0  -2   4 20666.8 598.731   1
   0  -2   4 20359.6 598.747   2
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   1  -5  -5 2081.12 69.6811  17
   1  -5  -5 2122.00 75.3791  15
   1  -5  -5 1950.76 68.8516  20
   1  -5  -4 2092.86 68.6223  50
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   1  -5  -4 1980.89 67.0904  44
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   1  -5  -4 2002.96 82.3959   3
   1  -5  -4 1894.88 102.893   9
   1  -5  -4 1931.36 88.9071   2
   1  -5  -4 1924.97 65.6690   6
   1  -5  -4 2107.01 69.1558   5
   1  -5  -4 1853.21 86.6990   1
   1  -5  -4 2056.46 66.8642  25
   1  -5  -4 2109.58 73.6613  15
   1  -5  -4 2017.77 67.1289  17
   1  -5  -4 1987.15 66.5871  20
   1  -5  -3 41.1975 16.2746  12
   1  -5  -3 23.1188 11.9224  50
   1  -5  -3 20.0024 24.6770   2
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   1  -5  -3 72.7829 34.9735   9
   1  -5  -3 34.8247 13.7236   5
   1  -5  -3 4.36847 12.8469  27
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   1  -5  -3 19.3025 19.6942   3
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   1  -5  -3 31.5152 13.3970  26
   1  -5  -2 485.338 30.0053  12
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   1  -5  -2 536.367 53.7806   9
   1  -5  -2 537.349 38.0671   3
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   1  -5   0 746.388 33.7972   5
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   1  -5   0 625.745 56.6743   9
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   1  -5   0 761.663 52.5669   2
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   1  -5   1-0.67313 13.3193   5
   1  -5   1 6.61208 31.0982   9
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   1  -5   2 1087.38 64.1478   2
   1  -5   2 1104.23 56.4658   3
   1  -5   2 1163.05 44.5341  15
   1  -5   2 1105.13 63.2077   1
   1  -5   2 1030.91 68.6474   9
   1  -5   3 191.394 37.6879   9
   1  -5   4 14.8882 25.3905   2
   1  -5   4-9.66015 24.3613   1
   1  -5   4 3.21133 30.9533   9
   1  -5   4 1.33363 13.5983   5
   1  -5   5 2172.22 72.1233  27
   1  -5   5 1984.43 94.1787   2
   1  -5   5 1980.11 93.9050   1
   1  -5   5 2146.84 88.1317   3
   1  -5   5 2155.81 72.2140  26
   1  -5   5 2099.25 102.554   9
   1  -5   5 2212.33 73.8623   5
   1  -5   6 161.349 14.8706  38
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   1  -5   6 164.079 15.0274  22
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   1  -5   6 197.853 38.5431   9
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   1  -3  12 1587.32 56.4670  32
   1  -3  12 1632.97 55.6572  16
   1  -3  12 1541.84 56.6707  37
   1  -3  12 1680.32 56.6910  24
   1  -3  12 1589.85 55.5389  29
   1  -3  12 1544.85 56.4314  28
   1  -3  12 1671.47 56.4328  30
   1  -3  12 1653.51 55.3311  55
   1  -3  13 1129.41 43.6571  54
   1  -3  13 1120.51 42.3625  41
   1  -3  13 1089.68 41.9481  24
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   1  -3  13 1107.80 41.4463  29
   1  -3  13 1133.11 42.3365  32
   1  -3  13 1129.14 42.5614  31
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   1  -3  13 1088.23 41.2867  16
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   1  -3  13 1151.02 43.4337  38
   1  -3  14 79.1110 15.5773  38
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   1  -3  14 95.2940 13.2293  29
   1  -3  14 68.3459 15.6530  37
   1  -3  14 83.0007 11.9017  40
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   1  -3  16 1902.88 64.9855  37
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   1  -3  21-1.65555 6.57186  23
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   1  -2 -11 1538.53 54.0550  20
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   1  -2 -10 113.967 25.0299  13
   1  -2 -10 109.344 13.5936  20
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   1  -2  -9 153.268 26.2719  13
  -1   2   8 403.947 19.6287  14
   1  -2  -8 377.788 27.8137   7
   1  -2  -8 397.230 32.1427  13
   1  -2  -7 1694.58 67.1893  13
   1  -2  -7 1583.86 57.5743   1
  -1   2   7 1545.11 52.7667  14
   1  -2  -7 1654.46 64.2496   7
   1  -2  -7 1556.73 57.3535   2
   1  -2  -6 1934.40 69.8021   2
   1  -2  -6 1944.81 69.5447   1
   1  -2  -6 1886.91 72.9513   7
   1  -2  -6 2094.93 76.8314  13
   1  -2  -5 92.8170 17.4869   1
   1  -2  -5 102.962 18.0191   2
   1  -2  -5 113.027 19.3381   7
   1  -2  -5 106.147 19.4533  13
   1  -2  -4 5286.42 174.150   1
   1  -2  -4 5834.01 174.843   7
   1  -2  -4 5289.99 174.279   2
   1  -2  -3 2476.07 88.4542   1
   1  -2  -3 2400.63 88.8515   2
   1  -2  -3 2679.23 85.2517   3
   1  -2  -3 2570.53 86.9078   7
   1  -2  -2 64099.3 2000.22   2
   1  -2  -2 65767.7 2000.40   1
   1  -2  -2 69287.6 1997.68   3
   1  -2  -2 67769.1 1998.96  13
   1  -2  -1 54587.7 1650.73   2
   1  -2  -1 54559.2 1647.48   3
   1  -2  -1 55210.7 1650.86   1
   1  -2  -1 56054.5 1646.84  12
   1  -2   0 364.098 19.8039  12
   1  -2   0 369.122 27.4169   1
   1  -2   0 303.094 20.9115   7
   1  -2   0 385.724 27.1839   2
   1  -2   1 194639. 5802.13  12
   1  -2   1 194026. 5808.00   2
   1  -2   1 197061. 5803.39   8
   1  -2   1 194764. 5802.83   7
   1  -2   1 194263. 5807.98   1
   1  -2   2 5594.95 172.701   7
   1  -2   2 5663.18 174.180   8
   1  -2   3 23531.7 734.056   1
   1  -2   3 23712.2 730.855   3
   1  -2   3 24036.0 734.262   2
   1  -2   3 24950.4 737.298   9
   1  -2   3 24976.6 729.521   8
   1  -2   3 24418.4 726.969   7
   1  -2   4 463.612 27.5857   1
   1  -2   4 436.495 24.1800   3
   1  -2   4 442.603 22.6662   8
   1  -2   4 463.839 17.9562   7
   1  -2   4 441.976 27.5648   2
   1  -2   4 495.586 33.0920   9
   1  -2   5 38.8811 13.4627   3
   1  -2   5 47.8632 12.1431   8
   1  -2   5 74.1561 22.1776   9
   1  -2   5 42.5821 5.25162   7
   1  -2   5 65.7975 16.5897   2
   1  -2   5 43.4945 16.0405   1
   1  -2   6 818.293 34.3291   8
   1  -2   6 822.621 37.2671   2
  -1   2  -6 810.057 27.3541  13
   1  -2   6 791.383 36.8647   1
   1  -2   7 80.9293 14.3973   8
   1  -2   7 71.9261 15.7492   1
   1  -2   7 98.5721 16.0951   2
   1  -2   8 55.7766 14.0466   8
   1  -2   8 57.4973 12.1707   1
   1  -2   8 40.4694 12.0981   2
   1  -2   8 50.0061 9.46685  16
   1  -2   9 691.120 33.0784   8
   1  -2   9 622.422 25.5065  16
   1  -2  10 46.2461 14.5136   8
   1  -2  10 49.2989 10.3585  16
   1  -2  11-6.17670 10.8625  16
   1  -2  11 3.11998 10.1724  24
   1  -2  11 6.14630 10.5004  28
   1  -2  11 0.51523 10.8100  37
   1  -2  11-1.36019 13.3170   8
   1  -2  12 1951.12 65.6019  16
   1  -2  12 1846.44 64.6620  32
   1  -2  12 1864.40 64.8296  31
   1  -2  12 1941.05 75.2413   8
   1  -2  12 1873.72 65.2159  24
   1  -2  12 1967.09 65.4339  37
   1  -2  12 1963.60 65.2008  41
   1  -2  12 1865.74 64.7547  55
   1  -2  12 2008.64 64.0067  49
   1  -2  12 1983.98 64.7032  29
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   1  -1   1 661.368 29.9822   9
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   2  -6  19 910.291 29.3325  41
   2  -5 -17-3.33323 3.49476  25
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   2  -5 -11 1565.74 56.5511  20
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   2  -5 -11 1452.22 95.0318   9
   2  -5 -11 1569.67 54.1376  34
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   2  -5 -10 10.9634 11.2905  34
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   2  -5  -9 280.768 33.6274  12
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   2  -5  -7 50.6698 18.1256  15
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   2  -5  -7 62.7950 12.1490  34
   2  -5  -7 43.2226 13.3173  20
   2  -5  -7 61.7220 22.6622  12
   2  -5  -7 40.4071 13.0790  44
   2  -5  -7 64.8245 15.2253  50
   2  -5  -7 71.9630 38.8959   9
   2  -5  -7 63.9889 12.2419  42
   2  -5  -6 3038.04 101.537  50
   2  -5  -6 3099.62 119.303  12
   2  -5  -6 3066.48 100.753  44
   2  -5  -6 3157.37 99.7154  39
   2  -5  -6 3161.00 147.116   9
   2  -5  -6 3135.08 105.465  15
   2  -5  -6 3035.19 121.079   1
   2  -5  -6 3093.87 99.6962  34
   2  -5  -6 3231.19 101.313   5
   2  -5  -6 2995.66 100.692  20
   2  -5  -6 3063.70 100.535  25
   2  -5  -6 3113.76 122.743   2
   2  -5  -6 3144.26 99.6056  42
   2  -5  -5 1804.39 66.5411  50
   2  -5  -5 1911.24 65.8381  53
   2  -5  -5 1934.91 81.9778  12
   2  -5  -5 1909.86 66.4130  44
   2  -5  -5 1955.40 65.1769  39
   2  -5  -5 1767.69 102.295   9
   2  -5  -5 2018.81 70.2755  15
   2  -5  -5 2142.31 89.7414   1
   2  -5  -5 1935.62 64.6876  34
   2  -5  -5 2062.50 67.7815   5
   2  -5  -5 1855.82 64.6221   6
   2  -5  -5 1939.57 65.8832  20
   2  -5  -5 1978.15 65.1932  42
   2  -5  -5 2039.83 89.9962   2
   2  -5  -5 1956.87 65.9615  25
   2  -5  -4 1276.49 59.1381  12
   2  -5  -4 1243.23 44.6003  42
   2  -5  -4 1191.20 48.4314  15
   2  -5  -4 1388.93 84.4488   9
   2  -5  -4 1206.95 43.6293  34
   2  -5  -4 1385.19 48.2790   5
   2  -5  -4 1157.86 44.0254   6
   2  -5  -4 1261.70 45.0683  25
   2  -5  -4 1234.65 67.7459   2
   2  -5  -4 1218.36 44.3265  39
   2  -5  -4 1194.88 46.4434  50
   2  -5  -4 1266.58 45.8156  53
   2  -5  -4 1428.63 69.6242   1
   2  -5  -4 1242.36 45.8259  44
   2  -5  -3 1330.45 47.7807  39
   2  -5  -3 1367.98 46.8685  34
   2  -5  -3 1354.20 64.2973   7
   2  -5  -3 1467.49 61.7918  12
   2  -5  -3 1365.46 71.1064   1
   2  -5  -3 1332.36 51.4281  15
   2  -5  -3 1299.22 85.2043   9
   2  -5  -3 1339.35 48.9114  44
   2  -5  -3 1470.78 73.4373   2
   2  -5  -3 1435.15 49.8317  50
   2  -5  -3 1353.99 49.2155  53
   2  -5  -3 1404.35 48.3949  25
   2  -5  -3 1364.94 47.9749  42
   2  -5  -3 1355.04 51.0140   5
   2  -5  -3 1227.31 47.6415   6
   2  -5  -2 99.3756 18.3464  12
   2  -5  -2 108.050 30.4868   2
   2  -5  -2 129.685 30.4561   1
   2  -5  -2 111.956 15.1453  27
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   2  -5  -2 107.962 17.3306   5
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   2  -5  -1 437.390 23.6832  27
   2  -5  -1 469.697 43.4357   1
   2  -5  -1 357.647 40.9092   2
   2  -5  -1 425.750 22.4069  50
   2  -5  -1 451.212 23.1465  53
   2  -5  -1 382.295 22.3440  44
   2  -5  -1 476.226 25.5780   5
   2  -5  -1 460.831 21.6715   6
   2  -5  -1 445.220 21.3872  42
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   2  -5  -1 451.999 21.1722  25
   2  -5  -1 440.287 28.5542  12
   2  -5  -1 478.280 34.1642   7
   2  -5  -1 392.766 23.4303  15
   2  -5   0 34.7729 18.2703   7
   2  -5   0 24.5509 25.4494   1
   2  -5   0-11.1576 28.3447   2
   2  -5   0 15.9253 9.93259  25
   2  -5   0 16.7519 10.3205  39
   2  -5   0 18.6772 11.8273  12
   2  -5   0 15.3485 12.4063  53
   2  -5   0 11.8421 12.1905  50
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   2  -5   0 20.3285 15.7109   5
   2  -5   0 10.3918 10.3788  42
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   2  -5   1 4202.25 157.480   1
   2  -5   1 4065.65 131.902  27
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   2  -5   1 4259.76 132.360  53
   2  -5   1 4134.26 157.662   2
   2  -5   1 4109.09 132.096  26
   2  -5   1 4431.39 134.298   5
   2  -5   1 4031.08 130.860   6
   2  -5   1 4241.28 130.806  39
   2  -5   1 4088.96 142.760   7
   2  -5   2 9285.40 326.067   9
   2  -5   2 9814.82 318.217   1
   2  -5   2 9511.72 290.814  44
   2  -5   2 9222.31 300.038   7
   2  -5   2 9566.70 290.223  42
   2  -5   2 9389.69 291.390  26
   2  -5   2 9928.08 319.664   2
   2  -5   2 9410.57 290.273  39
   2  -5   2 9678.41 289.966  28
   2  -5   2 9356.46 291.207  27
   2  -5   2 9898.21 293.386   5
   2  -5   3 936.405 65.6629   9
   2  -5   3 945.022 35.6934   6
   2  -5   3 902.809 37.0882  53
   2  -5   3 902.601 36.6975  26
   2  -5   3 904.270 36.5570  27
   2  -5   3 977.445 35.3954  28
   2  -5   3 961.925 35.6144  42
   2  -5   3 899.016 35.9716  44
   2  -5   3 937.990 35.5307  39
   2  -5   4 4149.54 164.543   9
   2  -5   4 4319.18 158.059   1
   2  -5   4 4175.95 132.175  26
   2  -5   4 4265.89 130.671  32
   2  -5   4 4193.95 130.577  31
   2  -5   4 4362.13 132.644  53
   2  -5   4 4021.43 130.977  36
   2  -5   4 4129.58 131.962  27
   2  -5   4 4165.66 130.889  28
   2  -5   4 4296.60 134.061   5
   2  -5   4 4065.24 131.056   6
   2  -5   4 4211.97 158.100   2
   2  -5   4 4037.89 131.280  44
   2  -5   5 1169.26 45.2030   5
   2  -5   5 1090.14 41.9609   6
   2  -5   5 1187.23 42.0561  31
   2  -5   5 1190.61 42.0856  32
   2  -5   5 1155.36 42.4224  42
   2  -5   5 1144.69 42.0298  28
   2  -5   5 1069.54 42.6623  27
   2  -5   5 1235.90 71.6648   9
   2  -5   5 1180.02 43.4588  26
   2  -5   5 1202.76 42.7390  39
   2  -5   5 1240.20 66.4299   2
   2  -5   5 1104.93 42.3454  36
   2  -5   5 1289.59 66.3048   1
   2  -5   5 1234.97 42.7796  44
   2  -5   5 1141.79 43.6317  53
   2  -5   6 65.2619 12.0343  43
   2  -5   6 76.2233 12.6416  42
   2  -5   6 75.9292 11.4717  41
   2  -5   6 63.5845 12.0101  40
   2  -5   6 71.1766 11.9249  38
   2  -5   6 66.8783 12.0625  39
   2  -5   6 63.0161 11.0632  37
   2  -5   6 77.5873 12.8291  36
   2  -5   6 61.9053 11.3030   6
   2  -5   6 60.8852 12.0215  32
   2  -5   6 59.5100 15.9432   5
   2  -5   6 50.6422 11.9885  31
   2  -5   6 38.4373 26.4356   2
   2  -5   6 29.3917 27.1260   1
   2  -5   6 70.6355 12.2112  28
   2  -5   6 60.8066 13.2182  27
   2  -5   6 86.9185 32.3557   9
   2  -5   6 68.2681 10.9866  23
   2  -5   6 78.9696 13.4892  26
   2  -5   6 70.0839 10.9555  22
   2  -5   6 70.1276 10.3581  21
   2  -5   6 84.5695 14.2739  53
   2  -5   6 78.7896 11.9690  44
   2  -5   7 987.091 39.1014  36
   2  -5   7 1059.30 38.4064  37
   2  -5   7 1089.02 41.5175   5
   2  -5   7 962.062 38.4717   6
   2  -5   7 1103.74 39.4577  32
   2  -5   7 1054.39 39.1024  31
   2  -5   7 950.787 36.6370  51
   2  -5   7 1045.31 40.4106  53
   2  -5   7 1071.46 60.2787   1
   2  -5   7 1119.70 62.1404   2
   2  -5   7 1062.75 39.6782  27
   2  -5   7 1036.06 38.9965  28
   2  -5   7 1009.47 39.6432  26
   2  -5   7 1046.46 70.5328   9
   2  -5   7 1021.44 39.3369  38
   2  -5   7 1008.64 38.0183  44
   2  -5   7 994.839 39.3183  54
   2  -5   7 1069.52 38.8976  23
   2  -5   7 959.800 38.3316  22
   2  -5   7 1027.07 38.8461  40
   2  -5   7 1053.22 39.3531  39
   2  -5   7 1044.32 39.4250  42
   2  -5   7 1082.58 39.2261  41
   2  -5   7 1116.58 39.3104  43
   2  -5   8 225.860 17.3503  31
   2  -5   8 277.935 18.0611  32
   2  -5   8 239.021 18.6983   5
   2  -5   8 243.755 15.6933   6
   2  -5   8 257.598 17.2416  27
   2  -5   8 254.630 17.2063  28
   2  -5   8 281.225 35.7266   2
   2  -5   8 249.017 34.3841   1
   2  -5   8 235.071 17.4784  54
   2  -5   8 247.704 15.2085  24
   2  -5   8 234.996 17.1170  26
   2  -5   8 218.678 17.1664  53
   2  -5   8 237.837 15.3522  51
   2  -5   8 262.332 17.6479  41
   2  -5   8 261.638 16.8095  43
   2  -5   8 230.577 17.1892  42
   2  -5   8 242.729 16.6063  40
   2  -5   8 233.257 16.9489  39
   2  -5   8 247.750 17.3559  38
   2  -5   8 259.812 16.1542  23
   2  -5   8 279.973 16.4494  22
   2  -5   8 234.066 16.8680  37
   2  -5   8 260.103 17.6010  36
   2  -5   9 2116.86 91.5141   2
   2  -5   9 2187.57 70.4758   5
   2  -5   9 2027.58 67.8594   6
   2  -5   9 2053.31 69.4580  28
   2  -5   9 1995.90 68.8804  22
   2  -5   9 1994.21 68.7348  23
   2  -5   9 2000.53 68.4506  40
   2  -5   9 2055.43 69.2900  39
   2  -5   9 2088.38 70.2131  38
   2  -5   9 2022.76 69.0346  53
   2  -5   9 1987.79 67.6204  51
   2  -5   9 2012.99 89.5358   1
   2  -5   9 2041.56 70.4011  54
   2  -5   9 2102.83 68.0987  24
   2  -5   9 2094.35 68.5410  43
   2  -5   9 2034.08 69.8509  41
   2  -5   9 1992.60 69.1479  42
   2  -5   9 1993.43 69.4200  36
   2  -5   9 2112.11 69.3878  37
   2  -5  10 1543.29 53.5602  41
   2  -5  10 1449.91 52.3445  42
   2  -5  10 1386.80 68.1884   1
   2  -5  10 1523.45 51.7310  24
   2  -5  10 1466.40 53.7879  38
   2  -5  10 1432.96 52.9897  36
   2  -5  10 1490.32 53.1031  37
   2  -5  10 1441.57 51.9878   5
   2  -5  10 1456.36 52.3539  39
   2  -5  10 1480.21 54.2617  54
   2  -5  10 1438.84 52.0680  22
   2  -5  10 1455.39 52.0999  23
   2  -5  10 1497.18 70.3538   2
   2  -5  11 88.1200 15.7430  54
   2  -5  11 100.958 14.0476  22
   2  -5  11 107.860 14.6789  36
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   2  -5  11 117.012 15.6981  41
   2  -5  11 97.3322 14.6677  42
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   2  -5  11 85.5721 14.2232  39
   2  -5  11 112.689 16.0144  38
   2  -5  12 52.6695 14.6406  38
   2  -5  12 61.0363 14.5451  54
   2  -5  12 40.1474 12.6744  22
   2  -5  12 54.9297 15.0704  32
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   2  -5  12 49.9468 13.8802  36
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   2  -5  13 17.7852 14.2443  38
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   2  -5  17 939.180 35.6408  41
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   2  -5  19 6.86498 7.75803  41
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   3   0   6 377.632 34.3849   8
   3   0   6 415.137 18.7402   4
   3   0   6 425.438 30.6080   1
   3   0   6 450.226 31.2103   2
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   3   0   7 5.98929 10.9876  16
   3   0   7 27.5308 14.2766   2
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   3   0   8 83.7646 13.1363  55
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   3   0  11 517.523 44.6948   8
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   3   0  15 235.255 16.4869  55
   3   0  16 104.786 9.49321  41
   3   0  16 132.251 13.4847  30
   3   0  16 97.6514 12.7879  55
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   3   0  17 30.7764 9.81278  55
   3   0  18 377.818 15.4651  55
   3   0  18 353.747 16.3605  38
   3   0  19-1.76571 4.40480  54
   3   0  19 0.60935 3.81600  30
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   3   1 -13 3823.68 125.140  19
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   3   1 -12 58.3520 19.9341  12
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   3   1 -12-4.67091 13.4352  19
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   3   1 -11 2603.58 98.8941  12
   3   1 -11 2580.09 85.4364  19
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   3   1 -10 824.769 43.5887   2
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   3   1 -10 759.734 32.3162  19
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   3   1 -10 807.528 40.0731   7
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   3   1  -9 229.703 24.3349  12
   3   1  -9 244.168 14.6616   4
   3   1  -9 272.694 23.6397   7
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   3   1  -8 644.251 36.8929   7
   3   1  -8 725.272 39.1231  12
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   3   1  -7 65.6205 18.2205  12
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   3   1  -5 15852.9 484.097   8
   3   1  -4 539.728 29.3565   8
   3   1  -3 155.075 18.7797   8
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   3   1   4 2714.30 110.054   8
   3   1   4 2938.51 92.0232   4
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   3   1   5 260.992 31.1256   8
   3   1   5 289.902 15.3111   4
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   3   1   6 16.2918 22.4381   8
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   3   1   7 737.259 42.2006   2
   3   1   7 867.616 54.3445   8
   3   1   7 855.494 32.6161  16
   3   1   7 741.587 41.9531   1
   3   1   8 370.701 20.3703  16
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   3   1  17 7.03838 7.73392  30
   3   1  18 22.1080 5.28926  38
   3   1  18 25.9728 5.48989  54
   3   1  18 13.3265 5.02936  30
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   3   2  -9 820.651 40.2193   7
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   3   2  -4 4719.15 151.862   8
   3   2  -3 1626.07 62.3171   8
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   3   2  -2 93.6661 16.5652   8
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   3   2   6 117.337 10.5220   4
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   3   2   7 14.2518 24.3532   8
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   3   2   8 460.091 43.5175   8
   3   2   8 513.573 25.9541  55
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   3   2  11 1659.89 84.9284   8
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   3   2  12 91.9117 15.6855  30
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   3   2  15 158.560 11.2726  49
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   3   2  16 1095.95 36.5025  49
   3   2  16 1106.52 37.7071  30
   3   2  17 44.6728 5.29868  30
   3   2  17 59.6355 5.53773  55
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   4  -5  -6 1252.03 76.5759   2
   4  -5  -6 1372.44 71.2734   7
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   4  -5   1 913.000 70.6787   1
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   4  -5   1 953.941 45.2443   4
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   4  -5   1 937.443 63.5780   9
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   4  -5   3 3932.93 179.213   2
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   4  -5   3 4476.36 141.074  21
   4  -5   3 3760.86 176.758   1
   4  -5   3 4476.67 146.608   4
   4  -5   3 4608.92 141.145  28
   4  -5   3 4485.72 140.816  39
   4  -5   3 4681.91 172.186   9
   4  -5   3 4561.40 140.923  36
   4  -5   4 236.026 44.6580   2
   4  -5   4 183.305 41.8820   1
   4  -5   4 286.029 19.2863  39
   4  -5   4 300.324 36.6634   9
   4  -5   4 245.547 26.0275   4
   4  -5   4 290.776 19.9940  42
   4  -5   4 273.878 25.7675   5
   4  -5   4 271.637 19.5757  28
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   4  -5   5 1100.39 40.4062  28
   4  -5   5 1031.22 40.6235  39
   4  -5   5 981.051 37.4095  41
   4  -5   5 941.469 44.5915   5
   4  -5   5 907.536 67.7656   1
   4  -5   5 1039.04 40.4438  36
   4  -5   5 1025.73 40.7298  42
   4  -5   5 1044.77 40.8468  31
   4  -5   5 1050.52 40.8953  32
   4  -5   5 1075.09 46.1350   4
   4  -5   6 52.3498 13.9309  28
   4  -5   6 91.0220 18.6785   5
   4  -5   6 61.3390 11.7706  41
   4  -5   6 81.5500 30.6589   2
   4  -5   6 100.095 31.4254   1
   4  -5   6 62.0585 14.0989  37
   4  -5   6 48.7780 13.4602  36
   4  -5   6 49.5731 14.6293  42
   4  -5   6 83.9813 15.1785  31
   4  -5   6 75.7189 15.0514  32
   4  -5   6 59.3080 13.5694  51
   4  -5   6 63.4168 14.7241  39
   4  -5   6 86.7442 20.3517   4
   4  -5   7 523.271 48.7084   1
   4  -5   7 492.746 48.7172   2
   4  -5   7 583.038 25.5201  24
   4  -5   7 558.833 27.2178  36
   4  -5   7 577.411 27.1456  37
   4  -5   7 572.155 26.3109  51
   4  -5   7 568.318 27.5148  31
   4  -5   7 547.947 27.1501  32
   4  -5   7 527.896 27.8992  39
   4  -5   7 575.868 25.9250  41
   4  -5   7 543.516 30.2718   5
   4  -5   7 538.108 27.9213  42
   4  -5   7 576.577 27.1923  28
   4  -5   8 1902.76 66.5313  41
   4  -5   8 1993.41 68.1350  32
   4  -5   8 2056.96 68.3556  31
   4  -5   8 1969.54 66.9988  51
   4  -5   8 1915.24 67.8456  36
   4  -5   8 1988.53 68.0092  37
   4  -5   8 1725.37 89.8336   1
   4  -5   8 2030.49 67.6607  28
   4  -5   8 2010.95 66.9219  24
   4  -5   8 1707.46 90.4612   2
   4  -5   8 1877.46 68.6726   5
   4  -5   9 72.2834 14.3569  28
   4  -5   9 84.2887 13.5826  41
   4  -5   9 62.2543 15.0494  32
   4  -5   9 57.2464 11.0392  54
   4  -5   9 84.7255 14.5591  51
   4  -5   9 73.5007 13.3056   5
   4  -5   9 62.5920 12.3663  24
   4  -5   9 77.4517 11.1045  38
   4  -5   9 93.9858 14.9976  37
   4  -5   9 78.1502 14.7420  36
   4  -5   9 83.3940 15.1426  31
   4  -5  10 45.5681 13.4186  36
   4  -5  10 32.8446 10.6141  38
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   4  -5  10 39.2896 13.9409  28
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   4  -5  10 36.1635 13.8035  32
   4  -5  10 64.8750 12.8349  51
   4  -5  10 46.9800 10.7992  54
   4  -5  10 54.7797 12.4610  24
   4  -5  11 211.532 15.1204  38
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   4  -5  11 251.210 18.2066  32
   4  -5  11 266.059 17.3913  41
   4  -5  11 230.211 17.9279  28
   4  -5  11 219.408 15.4747  54
   4  -5  12 620.276 26.9998  38
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   4  -5  12 694.659 28.7643  31
   4  -5  12 659.608 28.1972  24
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   4  -5  12 709.382 29.1986  28
   4  -5  12 629.905 27.2836  54
   4  -5  13 2306.65 76.3638  24
   4  -5  13 2324.98 75.8947  38
   4  -5  13 2367.31 77.5300  37
   4  -5  13 2452.78 76.8560  32
   4  -5  13 2392.57 76.7494  31
   4  -5  13 2272.79 75.9182  54
   4  -5  13 2334.39 77.2702  41
   4  -5  14 171.113 14.2366  41
   4  -5  14 180.388 14.5762  37
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   4  -5  14 157.598 12.9272  32
   4  -5  14 175.020 13.1395  31
   4  -5  15 260.214 14.8507  37
   4  -5  15 229.910 13.2589  32
   4  -5  15 238.784 13.4527  31
   4  -5  16 326.606 15.2371  37
   4  -5  17 176.400 9.10400  37
   4  -5  17 190.204 9.36623  41
   4  -4 -17 35.3848 6.16986  34
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   4  -4 -16 59.5091 8.58609  34
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   4  -4 -15 5.84881 9.15305  19
   4  -4 -15 12.0973 7.08698  25
   4  -4 -14 183.466 14.9055  34
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   4  -4 -14 180.707 14.7116  19
   4  -4 -14 161.380 12.0827  25
   4  -4 -13 24.5222 10.1339  25
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   4  -4 -13 39.2569 12.2744  34
   4  -4 -13 30.2264 12.2548  19
   4  -4 -13 34.2935 9.24736  21
   4  -4 -12 128.849 13.5297  25
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   4  -4 -12 130.260 15.6578  34
   4  -4 -12 112.361 12.2065  21
   4  -4 -12 132.774 14.7346  19
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   4  -4 -11 277.230 19.4004  34
   4  -4 -11 243.664 17.3314  25
   4  -4 -11 263.928 18.3248  19
   4  -4 -11 259.685 31.4370   7
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   4  -4 -10 2010.75 70.3039  34
   4  -4 -10 2009.76 69.4713  25
   4  -4 -10 2016.81 94.5297  12
   4  -4 -10 2161.42 70.6189  19
   4  -4 -10 1955.31 91.1380   7
   4  -4  -9 563.836 27.2899  34
   4  -4  -9 644.747 45.2002   7
   4  -4  -9 568.186 26.3703  25
   4  -4  -9 642.873 46.8848  12
   4  -4  -9 566.112 27.1360  19
   4  -4  -8 1023.73 61.3332  12
   4  -4  -8 997.101 38.9136  19
   4  -4  -8 1081.19 39.4115  25
   4  -4  -8 995.772 58.0546   7
   4  -4  -8 1000.34 41.0859   4
   4  -4  -7 412.557 37.9143  12
   4  -4  -7 254.891 41.3818   1
   4  -4  -7 294.123 41.4792   2
   4  -4  -7 374.441 37.5614   7
   4  -4  -7 449.147 22.1731  19
   4  -4  -7 309.598 24.8924   5
   4  -4  -7 428.388 22.5614  25
   4  -4  -7 373.582 49.3267   9
   4  -4  -7 449.008 26.9484   4
   4  -4  -6 74.6287 25.1860  12
   4  -4  -6 60.5573 32.2402   1
   4  -4  -6 48.5778 31.3076   2
   4  -4  -6 79.4510 18.1875   5
   4  -4  -6 77.8735 17.8138   4
   4  -4  -6 87.2581 13.1192  19
   4  -4  -6 110.119 14.1885  21
   4  -4  -6 78.2464 13.9519  25
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   4  -4  -6 45.6562 36.2508   9
   4  -4  -5 25.5880 21.5286  12
   4  -4  -5 3.26616 29.5487   1
   4  -4  -5-6.62151 29.6811   2
   4  -4  -5-16.4833 17.1989   5
   4  -4  -5 3.47288 16.3342   4
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   4  -4  -5 4.40026 12.4155  25
   4  -4  -5 4.74131 9.82867  36
   4  -4  -5 19.7310 32.1469   9
   4  -4  -4 18.6806 31.1054   9
   4  -4  -4 5.22715 10.3169  36
   4  -4  -4 12.2504 21.1451  12
   4  -4  -4-39.6348 30.5475   1
   4  -4  -4-13.3754 31.3235   2
   4  -4  -4-2.35731 21.1348   7
   4  -4  -4 13.6093 10.3213  19
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   4  -4  -4 2.52169 11.4736  21
   4  -4  -4 12.3344 16.8337   5
   4  -4  -4 2.61351 17.9398   4
   4  -4  -3 1.25071 12.4213  21
   4  -4  -3-7.00679 17.1342   4
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   4  -2   3 821.560 51.3294   1
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   4   0 -12 386.495 19.3841  34
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   4   0 -12 369.818 23.6357  19
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   4   0 -11 240.615 31.2800  12
   4   0 -11 302.503 28.7401   7
   4   0 -11 263.518 20.8143  19
   4   0 -10 2302.16 80.7386  19
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   4   0  -9 1107.04 41.1020   4
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   5  -1  -2 1550.73 52.1996  34
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  -7   0  -1 932.968 32.5636  47
  -7   0  -2 105.348 10.7232  56
   7   0   2 131.955 12.9967   4
  -7   0  -3 194.315 11.2446  56
   7   0   4 46.7976 6.19937  24
  -7   0  -4 70.8071 10.0838  20
  -7   0  -5 569.847 21.9729  20
  -7   0  -6 2.76899 6.19431  46
  -7   0  -6 12.8654 6.41900  20
  -7   0  -7 57.6848 5.30011  46
  -7   0  -7 61.4467 5.06273  20
   7   1 -12 30.3896 6.32283  48
   7   1 -12 28.7424 5.29712  19
  -7  -1  12 26.6445 5.55178  47
   7   1 -11 7.08364 7.23277  48
   7   1 -11 9.43456 6.05669  19
  -7  -1  11-2.43052 6.86987  47
   7   1 -10 26.3404 8.91714  48
  -7  -1  10 26.9771 8.17809  47
   7   1 -10 21.0457 7.75141  19
  -7  -1  10 15.7596 7.80690  18
   7   1  -9-4.83386 9.63912  48
  -7  -1   9-4.62842 7.75218  56
   7   1  -9-4.00445 8.93532   4
   7   1  -9-9.12236 8.10968  19
   7   1  -8 11.7646 8.53891  19
   7   1  -8 4.60489 10.4524  48
  -7  -1   8-4.28790 9.21445  47
   7   1  -8 13.3546 10.3306   4
  -7  -1   8 20.8923 8.67172  56
   7   1  -7 426.042 20.2786  48
  -7  -1   7 467.605 19.6564  47
  -7  -1   7 425.032 19.3370  56
   7   1  -7 413.460 20.8208   4
   7   1  -7 412.210 19.1801  19
  -7  -1   6-0.39170 9.74956  47
  -7  -1   6-6.73030 10.3518  56
   7   1  -6-7.00693 9.76394  19
   7   1  -6-8.07483 11.0952   4
  -7  -1   5 5.93943 9.77755  47
   7   1  -5 15.4897 10.6695   4
   7   1  -5 12.8697 10.0443  19
  -7  -1   4 64.3011 10.6819  47
  -7  -1   4 62.3301 11.9775  56
   7   1  -4 38.3061 11.8920   4
   7   1  -4 70.8421 11.1380  19
  -7  -1   3 797.065 30.2784  56
  -7  -1   3 774.171 29.3211  47
  -7  -1   2 358.321 18.3208  56
   7   1  -2 354.564 19.5581   4
  -7  -1   2 341.858 16.9377  47
  -7  -1   1 5.70784 10.0340  56
   7   1  -1 10.9545 10.6754   4
  -7  -1   1-11.3886 8.26027  47
  -7  -1   0 113.624 11.3807  56
   7   1   0 118.540 12.6890   4
  -7  -1   0 130.816 9.69655  47
  -7  -1  -1 2.96929 8.03876  56
   7   1   1 8.12412 9.63770   4
  -7  -1  -1-1.73014 5.99189  47
  -7  -1  -2 453.244 17.5611  56
  -7  -1  -3 660.632 23.8446  46
  -7  -1  -4 20.2297 6.08761  46
  -7  -1  -4 22.2507 7.16249  20
  -7  -1  -5 25.5400 5.59054  20
  -7  -2  11 8.14672 4.37423  47
  -7  -2  10 64.6965 7.27758  47
  -7  -2   9 66.5811 7.16011  56
  -7  -2   9 93.5426 8.21149  47
  -7  -2   8 4.55571 7.02345  56
  -7  -2   7 27.0322 8.52951  47
  -7  -2   7 40.5306 8.40377  56
   7   2  -7 25.4760 8.52727   4
   7   2  -6 248.704 14.8333   4
  -7  -2   6 278.940 14.0065  47
   7   2  -5 18.0173 9.00029   4
  -7  -2   5 22.7985 8.58259  47
  -7  -2   4 15.7856 9.24979  56
  -7  -2   4 16.4391 8.43341  47
  -7  -2   3-6.65384 7.83051  47
   7   2  -3 8.80573 9.01871   4
  -7  -2   3 10.5864 9.06152  56
  -7  -2   2 214.185 11.9873  47
  -7  -2   2 186.204 11.5019  20
   7   2  -2 198.577 13.0623   4
  -7  -2   2 232.822 12.4997  56
  -7  -2   1 26.2670 7.08270  47
  -7  -2   1 20.1968 7.42031  20
  -7  -2   1 17.4798 7.48857  56
   7   2  -1 14.4257 8.47134   4
  -7  -2   0 295.584 12.3782  56
  -7  -2   0 286.942 12.9461  20
  -7  -2  -1 38.4573 5.41571  56
  -7  -2  -1 46.3139 6.91942  20
  -7  -2  -2 3.41777 5.41357  20
  -7  -2  -3 172.922 8.03594  20
  -7  -3   8 49.7647 5.02093  56
  -7  -3   8 63.2327 5.59430  47
  -7  -3   7 188.960 9.24208  56
  -7  -3   6 654.111 22.5799  47
  -7  -3   5 1306.36 42.4760  56
  -7  -3   5 1350.24 42.4489  47
  -7  -3   4 683.441 23.3831  56
  -7  -3   3 606.258 21.0745  56
  -7  -3   2 35.7341 4.93109  56
   7   3  -2 20.0847 4.80533  55
  -8   3   4-1.68143 3.60607  56
   8  -3  -3-2.08489 3.75391  37
  -8   3   2 40.2929 5.33308  56
   8  -3  -2 102.785 5.39654  37
  -8   3   1 7.54407 4.10755  56
  -8   2   5 10.2952 4.40548  56
  -8   2   3 4.36296 5.29555  56
   8  -2  -3 15.0497 3.73910  37
  -8   2   2 93.2177 6.99184  56
  -8   2   1 70.9387 6.22070  56
  -8   1   5 12.4185 4.51629  56
  -8   1   3 23.4585 5.16846  56
  -8   1   2 65.3518 6.17815  56
  -8   1   1 78.1920 5.68738  56
  -8   1   0 56.2016 4.73760  20
  -8   0   4 34.9370 4.34761  56
   0   0   0    0.00    0.00   0
TITL NKS3008 in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184   6.375336   7.749475  18.000022 101.0023  97.3683 100.1168
ZERR    2.00   0.000145   0.000152   0.000244   0.0015   0.0016   0.0018
LATT  1
SFAC C H N O
UNIT 42.00 36.00 4.00 8.00
REM  CrysAlisPro recorded range (K): Min=159.9; max=160.1; aver:160.0
TEMP -113
SIZE 0.02 0.03 0.10
TREF
HKLF 4
END
;
_shelx_hkl_checksum              66772
_shelx_res_file
;
TITL nks3008_a.res in P-1
    nks3008.res
    created by SHELXL-2018/3 at 15:33:15 on 02-Sep-2024
CELL 1.54184 6.3757 7.7506 17.9997 100.967 97.373 100.127
ZERR 2 0.0001 0.0001 0.0004 0.002 0.002 0.002
LATT 1
SFAC C H N O
UNIT 42 36 4 8
EQIV $1 2-X,2-Y,1-Z
EQIV $2 1-X,1-Y,1-Z
L.S. 10 0 0
PLAN  20
SIZE 0.02 0.03 0.1
TEMP -113.15(10)
CONF
HTAB O4 O3_$1
HTAB N2 O1
HTAB N1 O4_$2
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\NKS3008.hkl">
REM </olex2.extras>
WGHT    0.057000    0.306500
EXTI    0.002041
FVAR       2.79142
O1    4    0.650549    0.666567    0.035385    11.00000    0.03198    0.04024 =
         0.02190    0.00373    0.00279   -0.00442
O2    4    1.178670    0.945550    0.188391    11.00000    0.02885    0.03568 =
         0.02685    0.00617    0.00398    0.00070
O3    4    1.037774    0.890408    0.288864    11.00000    0.03160    0.04683 =
         0.02165    0.00707    0.00182   -0.00401
O4    4    0.583609    0.879026    0.634414    11.00000    0.03525    0.03878 =
         0.02246    0.00366    0.00439    0.00072
H4    2    0.708742    0.951970    0.659146    11.00000    0.06036
N1    3    0.479325    0.442135    0.285081    11.00000    0.02980    0.02876 =
         0.02576    0.00852    0.00344    0.00227
H1    2    0.462015    0.363073    0.316777    11.00000    0.04083
N2    3    0.462585    0.587603    0.147289    11.00000    0.02496    0.02931 =
         0.02154    0.00506    0.00535    0.00124
H2    2    0.478020    0.574227    0.095832    11.00000    0.04358
C1    1    0.275311    0.494010    0.168610    11.00000    0.02417    0.02516 =
         0.02578    0.00247    0.00689    0.00253
C2    1    0.083897    0.453580    0.116166    11.00000    0.02850    0.02913 =
         0.02745    0.00341    0.00356    0.00521
AFIX  43
H2A   2    0.081763    0.494087    0.069522    11.00000   -1.20000
AFIX   0
C3    1   -0.103450    0.355267    0.130891    11.00000    0.02511    0.03239 =
         0.03681    0.00056    0.00243    0.00311
AFIX  43
H3    2   -0.232941    0.326686    0.094441    11.00000   -1.20000
AFIX   0
C4    1   -0.099242    0.299006    0.199810    11.00000    0.02754    0.03083 =
         0.04068    0.00351    0.01144    0.00115
AFIX  43
H4A   2   -0.227750    0.234648    0.211340    11.00000   -1.20000
AFIX   0
C5    1    0.091283    0.336310    0.251707    11.00000    0.03221    0.02961 =
         0.02936    0.00535    0.01046    0.00229
AFIX  43
H5    2    0.091044    0.296638    0.298496    11.00000   -1.20000
AFIX   0
C6    1    0.284785    0.431078    0.237158    11.00000    0.02596    0.02434 =
         0.02511    0.00222    0.00560    0.00321
C7    1    0.631619    0.612095    0.321499    11.00000    0.02531    0.03126 =
         0.02413    0.00563    0.00550    0.00259
AFIX  13
H7    2    0.781572    0.592843    0.318419    11.00000   -1.20000
AFIX   0
C8    1    0.590863    0.755218    0.276610    11.00000    0.02652    0.02843 =
         0.02306    0.00339    0.00610    0.00156
AFIX  23
H8A   2    0.441204    0.773084    0.277664    11.00000   -1.20000
H8B   2    0.690582    0.870450    0.301855    11.00000   -1.20000
AFIX   0
C9    1    0.622517    0.704518    0.195207    11.00000    0.02571    0.02468 =
         0.02329    0.00581    0.00474    0.00374
C10   1    0.808318    0.781091    0.166653    11.00000    0.02581    0.02566 =
         0.02171    0.00475    0.00495    0.00240
C11   1    0.805687    0.756996    0.084997    11.00000    0.02761    0.02678 =
         0.02372    0.00527    0.00481    0.00201
C12   1    0.994110    0.846069    0.060802    11.00000    0.02574    0.03029 =
         0.01838    0.00558    0.00643    0.00062
AFIX  43
H12   2    0.994265    0.840831    0.007649    11.00000   -1.20000
AFIX   0
C13   1    1.169719    0.936422    0.111664    11.00000    0.02841    0.02872 =
         0.02445    0.00720    0.00641    0.00462
C14   1    1.002477    0.872052    0.218934    11.00000    0.02762    0.02785 =
         0.02369    0.00605    0.00595    0.00247
C15   1    1.370415    1.034843    0.093587    11.00000    0.03086    0.04836 =
         0.05516    0.02426    0.01461    0.00727
AFIX 137
H15A  2    1.398618    1.160599    0.121192    11.00000   -1.50000
H15B  2    1.354219    1.028990    0.038227    11.00000   -1.50000
H15C  2    1.491521    0.980219    0.109353    11.00000   -1.50000
AFIX   0
C16   1    0.617018    0.677269    0.405438    11.00000    0.02872    0.03164 =
         0.02326    0.00760    0.00376    0.00335
C17   1    0.420807    0.665846    0.431979    11.00000    0.02578    0.04550 =
         0.02523    0.00296    0.00099    0.00231
AFIX  43
H17   2    0.290729    0.610431    0.397254    11.00000   -1.20000
AFIX   0
C18   1    0.411561    0.733949    0.508296    11.00000    0.02660    0.04644 =
         0.02713    0.00661    0.00564    0.00374
AFIX  43
H18   2    0.276168    0.724100    0.525576    11.00000   -1.20000
AFIX   0
C19   1    0.600719    0.816574    0.559391    11.00000    0.03260    0.02897 =
         0.02188    0.00662    0.00375    0.00299
C20   1    0.798038    0.828612    0.534054    11.00000    0.02856    0.04129 =
         0.02547    0.00620    0.00039   -0.00354
AFIX  43
H20   2    0.927986    0.884150    0.568830    11.00000   -1.20000
AFIX   0
C21   1    0.804778    0.759013    0.457512    11.00000    0.02615    0.04274 =
         0.02691    0.00784    0.00471   -0.00014
AFIX  43
H21   2    0.940413    0.767471    0.440438    11.00000   -1.20000
AFIX   0
HKLF 4
REM  nks3008_a.res in P-1
REM wR2 = 0.1146, GooF = S = 1.076, Restrained GooF = 1.076 for all data
REM R1 = 0.0412 for 3159 Fo > 4sig(Fo) and 0.0467 for all 3608 data
REM 258 parameters refined using 0 restraints
END
WGHT      0.0570      0.3065
REM Highest difference peak  0.452,  deepest hole -0.315,  1-sigma level  0.046
Q1    1   1.3639  0.9564  0.0556  11.00000  0.05    0.45
Q2    1   0.9244  0.8203  0.0726  11.00000  0.05    0.37
Q3    1   1.0545  0.8726  0.0769  11.00000  0.05    0.33
Q4    1   1.0233  0.8046  0.0591  11.00000  0.05    0.29
Q5    1   0.7311  0.7325  0.1811  11.00000  0.05    0.25
Q6    1   0.8118  0.7615  0.1363  11.00000  0.05    0.24
Q7    1   0.3594  0.5348  0.1613  11.00000  0.05    0.23
Q8    1   0.2715  0.4786  0.2046  11.00000  0.05    0.21
Q9    1   1.3455  1.0328  0.2209  11.00000  0.05    0.20
Q10   1   0.1829  0.4590  0.1413  11.00000  0.05    0.19
Q11   1   0.8601  0.8325  0.1853  11.00000  0.05    0.19
Q12   1   0.6206  0.6871  0.2980  11.00000  0.05    0.18
Q13   1   0.1930  0.3817  0.2402  11.00000  0.05    0.18
Q14   1   0.6066  0.7227  0.2368  11.00000  0.05    0.18
Q15   1   1.3617  1.1161  0.0563  11.00000  0.05    0.17
Q16   1   0.5295  0.7383  0.4206  11.00000  0.05    0.16
Q17   1   0.2911  0.4180  0.1860  11.00000  0.05    0.16
Q18   1   0.4343  0.7092  0.4761  11.00000  0.05    0.15
Q19   1  -0.0762  0.3248  0.1616  11.00000  0.05    0.15
Q20   1   0.8915  0.9689  0.5830  11.00000  0.05    0.15
;
_shelx_res_checksum              24576
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.65055(17) 0.66657(15) 0.03539(6) 0.0334(3) Uani d 1 . .
O O2 1.17867(16) 0.94555(14) 0.18839(6) 0.0314(2) Uani d 1 . .
O O3 1.03777(17) 0.89041(15) 0.28886(6) 0.0352(3) Uani d 1 . .
O O4 0.58361(18) 0.87903(15) 0.63441(6) 0.0335(3) Uani d 1 . .
H H4 0.709(4) 0.952(3) 0.6591(14) 0.060(7) Uiso d 1 . .
N N1 0.47933(19) 0.44213(16) 0.28508(7) 0.0283(3) Uani d 1 . .
H H1 0.462(3) 0.363(3) 0.3168(11) 0.041(5) Uiso d 1 . .
N N2 0.46259(18) 0.58760(16) 0.14729(7) 0.0257(3) Uani d 1 . .
H H2 0.478(3) 0.574(3) 0.0958(12) 0.044(5) Uiso d 1 . .
C C1 0.2753(2) 0.49401(18) 0.16861(8) 0.0255(3) Uani d 1 . .
C C2 0.0839(2) 0.45358(19) 0.11617(8) 0.0289(3) Uani d 1 . .
H H2A 0.081763 0.494087 0.069522 0.035 Uiso calc 1 . .
C C3 -0.1035(2) 0.3553(2) 0.13089(9) 0.0330(3) Uani d 1 . .
H H3 -0.232941 0.326686 0.094441 0.040 Uiso calc 1 . .
C C4 -0.0992(2) 0.2990(2) 0.19981(9) 0.0337(3) Uani d 1 . .
H H4A -0.227750 0.234648 0.211340 0.040 Uiso calc 1 . .
C C5 0.0913(2) 0.33631(19) 0.25171(8) 0.0306(3) Uani d 1 . .
H H5 0.091044 0.296638 0.298496 0.037 Uiso calc 1 . .
C C6 0.2848(2) 0.43108(18) 0.23716(8) 0.0257(3) Uani d 1 . .
C C7 0.6316(2) 0.61210(19) 0.32150(8) 0.0272(3) Uani d 1 . .
H H7 0.781572 0.592843 0.318419 0.033 Uiso calc 1 . .
C C8 0.5909(2) 0.75522(18) 0.27661(8) 0.0266(3) Uani d 1 . .
H H8A 0.441204 0.773084 0.277664 0.032 Uiso calc 1 . .
H H8B 0.690582 0.870450 0.301855 0.032 Uiso calc 1 . .
C C9 0.6225(2) 0.70452(17) 0.19521(7) 0.0246(3) Uani d 1 . .
C C10 0.8083(2) 0.78109(18) 0.16665(7) 0.0247(3) Uani d 1 . .
C C11 0.8057(2) 0.75700(18) 0.08500(8) 0.0265(3) Uani d 1 . .
C C12 0.9941(2) 0.84607(18) 0.06080(7) 0.0252(3) Uani d 1 . .
H H12 0.994265 0.840831 0.007649 0.030 Uiso calc 1 . .
C C13 1.1697(2) 0.93642(18) 0.11166(8) 0.0270(3) Uani d 1 . .
C C14 1.0025(2) 0.87205(18) 0.21893(8) 0.0266(3) Uani d 1 . .
C C15 1.3704(3) 1.0348(2) 0.09359(11) 0.0425(4) Uani d 1 . .
H H15A 1.398618 1.160599 0.121192 0.064 Uiso calc 1 . .
H H15B 1.354219 1.028990 0.038227 0.064 Uiso calc 1 . .
H H15C 1.491521 0.980219 0.109353 0.064 Uiso calc 1 . .
C C16 0.6170(2) 0.67727(19) 0.40544(8) 0.0281(3) Uani d 1 . .
C C17 0.4208(2) 0.6658(2) 0.43198(8) 0.0337(3) Uani d 1 . .
H H17 0.290729 0.610431 0.397254 0.040 Uiso calc 1 . .
C C18 0.4116(2) 0.7339(2) 0.50830(8) 0.0340(3) Uani d 1 . .
H H18 0.276168 0.724100 0.525576 0.041 Uiso calc 1 . .
C C19 0.6007(2) 0.81657(19) 0.55939(8) 0.0282(3) Uani d 1 . .
C C20 0.7980(2) 0.8286(2) 0.53405(8) 0.0336(3) Uani d 1 . .
H H20 0.927986 0.884150 0.568830 0.040 Uiso calc 1 . .
C C21 0.8048(2) 0.7590(2) 0.45751(8) 0.0328(3) Uani d 1 . .
H H21 0.940413 0.767471 0.440438 0.039 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 0.0320(5) 0.0402(6) 0.0219(5) -0.0044(4) 0.0028(4) 0.0037(4)
O2 0.0288(5) 0.0357(5) 0.0268(5) 0.0007(4) 0.0040(4) 0.0062(4)
O3 0.0316(5) 0.0468(6) 0.0216(5) -0.0040(4) 0.0018(4) 0.0071(4)
O4 0.0352(6) 0.0388(6) 0.0225(5) 0.0007(5) 0.0044(4) 0.0037(4)
N1 0.0298(6) 0.0288(6) 0.0258(6) 0.0023(5) 0.0034(5) 0.0085(5)
N2 0.0250(6) 0.0293(6) 0.0215(6) 0.0012(4) 0.0054(4) 0.0051(4)
C1 0.0242(6) 0.0252(6) 0.0258(6) 0.0025(5) 0.0069(5) 0.0025(5)
C2 0.0285(7) 0.0291(7) 0.0274(7) 0.0052(5) 0.0036(5) 0.0034(5)
C3 0.0251(7) 0.0324(7) 0.0368(8) 0.0031(6) 0.0024(6) 0.0006(6)
C4 0.0275(7) 0.0308(7) 0.0407(8) 0.0011(6) 0.0114(6) 0.0035(6)
C5 0.0322(7) 0.0296(7) 0.0294(7) 0.0023(6) 0.0105(6) 0.0054(5)
C6 0.0260(6) 0.0243(6) 0.0251(6) 0.0032(5) 0.0056(5) 0.0022(5)
C7 0.0253(6) 0.0313(7) 0.0241(6) 0.0026(5) 0.0055(5) 0.0056(5)
C8 0.0265(6) 0.0284(7) 0.0231(6) 0.0016(5) 0.0061(5) 0.0034(5)
C9 0.0257(6) 0.0247(6) 0.0233(6) 0.0037(5) 0.0047(5) 0.0058(5)
C10 0.0258(7) 0.0257(6) 0.0217(6) 0.0024(5) 0.0049(5) 0.0048(5)
C11 0.0276(7) 0.0268(6) 0.0237(6) 0.0020(5) 0.0048(5) 0.0053(5)
C12 0.0257(6) 0.0303(7) 0.0184(6) 0.0006(5) 0.0064(5) 0.0056(5)
C13 0.0284(7) 0.0287(7) 0.0244(6) 0.0046(5) 0.0064(5) 0.0072(5)
C14 0.0276(7) 0.0278(7) 0.0237(6) 0.0025(5) 0.0060(5) 0.0061(5)
C15 0.0309(8) 0.0484(9) 0.0552(10) 0.0073(7) 0.0146(7) 0.0243(8)
C16 0.0287(7) 0.0316(7) 0.0233(6) 0.0034(5) 0.0038(5) 0.0076(5)
C17 0.0258(7) 0.0455(8) 0.0252(7) 0.0023(6) 0.0010(5) 0.0030(6)
C18 0.0266(7) 0.0464(9) 0.0271(7) 0.0037(6) 0.0056(5) 0.0066(6)
C19 0.0326(7) 0.0290(7) 0.0219(6) 0.0030(5) 0.0037(5) 0.0066(5)
C20 0.0286(7) 0.0413(8) 0.0255(7) -0.0035(6) 0.0004(5) 0.0062(6)
C21 0.0261(7) 0.0427(8) 0.0269(7) -0.0001(6) 0.0047(5) 0.0078(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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 0 0.0200
0 0 0 0.0050
0 -1 0 0.0145
0 1 0 0.0010
3 0 1 0.0411
-3 0 -1 0.0411
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
C13 O2 C14 . . 122.21(11) ?
C19 O4 H4 . . 109.6(16) ?
C6 N1 H1 . . 110.6(12) ?
C6 N1 C7 . . 123.76(12) ?
C7 N1 H1 . . 113.6(12) ?
C1 N2 H2 . . 120.6(13) ?
C9 N2 H2 . . 114.0(13) ?
C9 N2 C1 . . 125.33(11) ?
C2 C1 N2 . . 117.37(12) ?
C2 C1 C6 . . 120.69(12) ?
C6 C1 N2 . . 121.73(12) ?
C1 C2 H2A . . 119.5 ?
C3 C2 C1 . . 121.03(13) ?
C3 C2 H2A . . 119.5 ?
C2 C3 H3 . . 120.5 ?
C2 C3 C4 . . 118.99(14) ?
C4 C3 H3 . . 120.5 ?
C3 C4 H4A . . 119.9 ?
C5 C4 C3 . . 120.29(13) ?
C5 C4 H4A . . 119.9 ?
C4 C5 H5 . . 119.1 ?
C4 C5 C6 . . 121.83(13) ?
C6 C5 H5 . . 119.1 ?
N1 C6 C1 . . 122.60(12) ?
N1 C6 C5 . . 119.93(12) ?
C5 C6 C1 . . 117.06(13) ?
N1 C7 H7 . . 108.1 ?
N1 C7 C8 . . 109.11(11) ?
N1 C7 C16 . . 113.14(11) ?
C8 C7 H7 . . 108.1 ?
C16 C7 H7 . . 108.1 ?
C16 C7 C8 . . 110.02(11) ?
C7 C8 H8A . . 109.2 ?
C7 C8 H8B . . 109.2 ?
H8A C8 H8B . . 107.9 ?
C9 C8 C7 . . 112.11(11) ?
C9 C8 H8A . . 109.2 ?
C9 C8 H8B . . 109.2 ?
N2 C9 C8 . . 116.72(12) ?
N2 C9 C10 . . 119.55(12) ?
C10 C9 C8 . . 123.66(12) ?
C9 C10 C11 . . 120.11(12) ?
C9 C10 C14 . . 120.03(12) ?
C14 C10 C11 . . 119.74(12) ?
O1 C11 C10 . . 124.06(12) ?
O1 C11 C12 . . 119.13(12) ?
C12 C11 C10 . . 116.80(12) ?
C11 C12 H12 . . 119.3 ?
C13 C12 C11 . . 121.42(12) ?
C13 C12 H12 . . 119.3 ?
O2 C13 C15 . . 112.37(13) ?
C12 C13 O2 . . 121.51(12) ?
C12 C13 C15 . . 126.11(13) ?
O2 C14 C10 . . 117.90(11) ?
O3 C14 O2 . . 114.04(12) ?
O3 C14 C10 . . 128.03(13) ?
C13 C15 H15A . . 109.5 ?
C13 C15 H15B . . 109.5 ?
C13 C15 H15C . . 109.5 ?
H15A C15 H15B . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C17 C16 C7 . . 122.38(12) ?
C17 C16 C21 . . 118.19(13) ?
C21 C16 C7 . . 119.36(12) ?
C16 C17 H17 . . 119.4 ?
C18 C17 C16 . . 121.16(13) ?
C18 C17 H17 . . 119.4 ?
C17 C18 H18 . . 120.1 ?
C17 C18 C19 . . 119.86(14) ?
C19 C18 H18 . . 120.1 ?
O4 C19 C18 . . 117.69(13) ?
O4 C19 C20 . . 122.47(13) ?
C20 C19 C18 . . 119.81(13) ?
C19 C20 H20 . . 120.2 ?
C19 C20 C21 . . 119.66(13) ?
C21 C20 H20 . . 120.2 ?
C16 C21 H21 . . 119.3 ?
C20 C21 C16 . . 121.32(14) ?
C20 C21 H21 . . 119.3 ?
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 C11 . 1.2484(17) ?
O2 C13 . 1.3626(16) ?
O2 C14 . 1.3933(16) ?
O3 C14 . 1.2260(17) ?
O4 H4 . 0.90(3) ?
O4 C19 . 1.3702(17) ?
N1 H1 . 0.92(2) ?
N1 C6 . 1.3963(18) ?
N1 C7 . 1.4717(18) ?
N2 H2 . 0.93(2) ?
N2 C1 . 1.4206(17) ?
N2 C9 . 1.3254(17) ?
C1 C2 . 1.3914(19) ?
C1 C6 . 1.4086(19) ?
C2 H2A . 0.9500 ?
C2 C3 . 1.384(2) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.390(2) ?
C4 H4A . 0.9500 ?
C4 C5 . 1.384(2) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.4027(19) ?
C7 H7 . 1.0000 ?
C7 C8 . 1.5295(19) ?
C7 C16 . 1.5195(18) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C8 C9 . 1.4922(18) ?
C9 C10 . 1.4300(18) ?
C10 C11 . 1.4434(18) ?
C10 C14 . 1.4341(19) ?
C11 C12 . 1.4375(18) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.3414(19) ?
C13 C15 . 1.478(2) ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
C16 C17 . 1.390(2) ?
C16 C21 . 1.390(2) ?
C17 H17 . 0.9500 ?
C17 C18 . 1.387(2) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.389(2) ?
C19 C20 . 1.386(2) ?
C20 H20 . 0.9500 ?
C20 C21 . 1.390(2) ?
C21 H21 . 0.9500 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 N2 2.5882(16) . . yes
O1 O1 2.8900(16) . 2_665 yes
O2 C5 3.1976(18) . 1_665 yes
O3 C8 2.8223(17) . . yes
O3 O4 2.7598(16) . 2_776 yes
O1 H2 1.80(2) . . yes
O1 H2 2.65(2) . 2_665 yes
O2 H4 2.67(2) . 2_776 yes
O3 H8B 2.24 . . yes
O3 H4 1.86(3) . 2_776 yes
O4 H1 2.21(2) . 2_666 yes
N1 N2 2.9107(17) . . yes
N1 H17 2.72 . . yes
C2 C11 3.272(2) . 1_455 yes
C2 C10 3.3849(19) . 1_455 yes
C3 C10 3.400(2) . 1_455 yes
C1 H15A 2.84 . 1_445 yes
C1 H8A 2.59 . . yes
C2 H12 2.79 . 2_665 yes
C6 H8A 2.59 . . yes
C11 H2 2.36(2) . . yes
C14 H8B 2.64 . . yes
C14 H4 2.65(2) . 2_776 yes
C17 H1 2.90(2) . . yes
C19 H1 2.88(2) . 2_666 yes
H1 H5 2.2962 . . yes
H2 H2A 2.45 . . yes
H4 H20 2.32 . . yes
H7 H21 2.35 . . yes
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
O4 H4 O3 2_776 0.90(3) 1.86(3) 2.7597(15) 178(2) yes
N1 H1 O4 2_666 0.92(2) 2.21(2) 3.1028(16) 165.2(17) yes
N2 H2 O1 . 0.93(2) 1.80(2) 2.5882(15) 140.8(18) 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
O1 C11 C12 C13 . . . . -176.20(14) ?
O4 C19 C20 C21 . . . . 178.55(14) ?
N1 C7 C8 C9 . . . . -60.37(14) ?
N1 C7 C16 C17 . . . . -40.57(19) ?
N1 C7 C16 C21 . . . . 142.47(14) ?
N2 C1 C2 C3 . . . . 176.89(12) ?
N2 C1 C6 N1 . . . . -5.7(2) ?
N2 C1 C6 C5 . . . . -178.41(12) ?
N2 C9 C10 C11 . . . . 11.1(2) ?
N2 C9 C10 C14 . . . . -164.86(13) ?
C1 N2 C9 C8 . . . . -6.8(2) ?
C1 N2 C9 C10 . . . . 176.18(12) ?
C1 C2 C3 C4 . . . . 1.0(2) ?
C2 C1 C6 N1 . . . . 169.01(13) ?
C2 C1 C6 C5 . . . . -3.7(2) ?
C2 C3 C4 C5 . . . . -1.9(2) ?
C3 C4 C5 C6 . . . . 0.1(2) ?
C4 C5 C6 N1 . . . . -170.18(13) ?
C4 C5 C6 C1 . . . . 2.7(2) ?
C6 N1 C7 C8 . . . . -21.39(17) ?
C6 N1 C7 C16 . . . . 101.43(15) ?
C6 C1 C2 C3 . . . . 1.9(2) ?
C7 N1 C6 C1 . . . . 59.64(19) ?
C7 N1 C6 C5 . . . . -127.87(14) ?
C7 C8 C9 N2 . . . . 78.98(15) ?
C7 C8 C9 C10 . . . . -104.10(15) ?
C7 C16 C17 C18 . . . . -176.98(14) ?
C7 C16 C21 C20 . . . . 176.77(14) ?
C8 C7 C16 C17 . . . . 81.74(17) ?
C8 C7 C16 C21 . . . . -95.22(15) ?
C8 C9 C10 C11 . . . . -165.74(13) ?
C8 C9 C10 C14 . . . . 18.3(2) ?
C9 N2 C1 C2 . . . . 147.66(14) ?
C9 N2 C1 C6 . . . . -37.4(2) ?
C9 C10 C11 O1 . . . . -2.4(2) ?
C9 C10 C11 C12 . . . . 176.74(12) ?
C9 C10 C14 O2 . . . . -179.54(12) ?
C9 C10 C14 O3 . . . . 2.7(2) ?
C10 C11 C12 C13 . . . . 4.6(2) ?
C11 C10 C14 O2 . . . . 4.5(2) ?
C11 C10 C14 O3 . . . . -173.28(14) ?
C11 C12 C13 O2 . . . . 1.0(2) ?
C11 C12 C13 C15 . . . . -179.05(14) ?
C13 O2 C14 O3 . . . . 179.40(13) ?
C13 O2 C14 C10 . . . . 1.33(19) ?
C14 O2 C13 C12 . . . . -4.2(2) ?
C14 O2 C13 C15 . . . . 175.86(12) ?
C14 C10 C11 O1 . . . . 173.61(13) ?
C14 C10 C11 C12 . . . . -7.29(19) ?
C16 C7 C8 C9 . . . . 174.97(11) ?
C16 C17 C18 C19 . . . . 0.5(2) ?
C17 C16 C21 C20 . . . . -0.3(2) ?
C17 C18 C19 O4 . . . . -178.94(14) ?
C17 C18 C19 C20 . . . . -0.8(2) ?
C18 C19 C20 C21 . . . . 0.5(2) ?
C19 C20 C21 C16 . . . . 0.1(2) ?
C21 C16 C17 C18 . . . . 0.0(2) ?