#------------------------------------------------------------------------------
#$Date: 2023-07-29 05:03:55 +0300 (Sat, 29 Jul 2023) $
#$Revision: 285386 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022830.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_2022830
loop_
_publ_author_name
'Nasr, Tamer'
'Kariuki, Benson M.'
'Elansary, Mai M.'
'Elhaggar, Radwan'
'Zaghary, Wafaa'
_publ_section_title
;
 Synthesis and crystal structures of
 (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and
 (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine
;
_journal_coeditor_code           JQ2029
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              762
_journal_page_last               766
_journal_paper_doi               10.1107/S2056989023006412
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C9 H8 Cl N3 O3'
_chemical_formula_moiety         'C9 H8 Cl N3 O3'
_chemical_formula_sum            'C9 H8 Cl N3 O3'
_chemical_formula_weight         241.63
_chemical_name_common
;
<i>N</i>'-[(1<i>E</i>)-(4-Chloro-3-nitrophenyl)methylidene]acetohydrazide
;
_chemical_name_systematic
;
(<i>E</i>)-<i>N</i>'-(4-Chloro-3-nitrobenzylidene)acetohydrazide
;
_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   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 95.689(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.47170(10)
_cell_length_b                   11.9367(2)
_cell_length_c                   20.1382(3)
_cell_measurement_reflns_used    5559
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8600
_cell_measurement_theta_min      4.2770
_cell_volume                     1069.63(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.625
_diffrn_reflns_theta_min         4.311
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2107
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.2562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                1960
_reflns_number_total             2107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jq2029sup1.cif
_cod_data_source_block           IV
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022830
_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   0.412
_shelx_estimated_absorpt_t_max   0.832
_shelx_hkl_file
;
   0   0   2 22811.0 352.189   2
   0   0   3 3.71707 19.2816   2
   0   0   4 567.141 49.3067   2
   0   0   5 20.7899 26.5355   2
   0   0   6 180484. 2494.72   3
   0   0   6 178479. 2450.38   2
   0   0   7 11.5229 34.9257   3
   0   0   7 58.9763 27.5153   2
   0   0   8 1919.68 102.448   2
   0   0   8 1921.49 122.557   3
   0   0   9 44.5415 39.9204   3
   0   0  10 7164.15 268.779   3
   0   0  11-8.54601 39.0874   3
   0   0  12 5326.77 255.611   3
   0   0 -13 22.2937 32.8141   6
   0   0  13 59.4538 46.4520   3
   0   0 -14 11653.3 406.256   6
   0   0  14 11457.2 433.430   3
   0   0 -14 12571.5 269.035  18
   0   0 -15-15.4760 26.9674  18
   0   0  15 36.2244 41.2889   3
   0   0 -15 27.1216 35.7778   6
   0   0  16 222.448 75.6951   3
   0   0 -16 130.202 32.1058  18
   0   0 -16 174.084 31.2073  15
   0   0 -16 198.124 59.0214   6
   0   0 -17-54.8053 31.2869  18
   0   0 -17 12.7875 23.8528  15
   0   0  17 22.3547 48.3669   3
   0   0 -18 274.291 40.6111  15
   0   0 -18 310.459 43.6703  18
   0   0 -19-77.6879 36.0171  18
   0   0 -19 1.45841 25.0221  15
   0   0 -20 2903.63 120.941  15
   0   0 -20 2843.97 112.356   7
   0   0 -21 5.56711 20.1056   7
   0   0 -21-5.27183 23.6795  15
   0   0 -22 5708.37 161.463  15
   0   0 -22 5294.60 145.720   7
   0   0 -23 1.75177 14.1598   7
   0   0 -23 20.1526 19.3935  15
   0   0 -24-7.01825 14.5079  15
   0   0 -24 18.3516 10.9847   7
   0   1   0 18.0710 7.11201   5
   0   1   0 13.9446 5.24345   6
   0  -1   1 33154.5 445.891   3
   0   1  -1 32338.3 462.823   1
   0   1  -1 32444.0 471.124   6
   0   1   2 102267. 1556.15   2
   0  -1   2 117933. 1502.97   3
   0  -1   3 187027. 2448.37   3
   0   1   3 178400. 2502.72   2
   0  -1   3 183570. 2392.59   2
   0  -1   4 58869.3 810.027   2
   0  -1   4 56483.7 864.521   3
   0  -1   5 44493.1 654.919   2
   0  -1   5 44713.5 718.490   3
   0  -1   6 22678.6 443.525   3
   0  -1   6 22253.8 379.966   2
   0  -1   7 97095.7 1503.74   3
   0   1   7 106472. 1520.09   2
   0   1   8 18407.9 414.998   2
   0  -1   8 17580.6 413.277   3
   0   1   9 55865.6 1006.25   3
   0   1   9 56150.5 967.125   2
   0  -1  10 42344.1 805.452   3
   0   1  10 40397.1 807.694   3
   0   1  11 1869.89 143.742   3
   0  -1  11 2059.16 152.326   3
   0   1 -12 25877.4 620.123   6
   0   1  12 24179.0 617.880   3
   0   1 -13 4475.44 236.293   6
   0   1  13 4220.49 240.399   3
   0  -1  13 4682.93 255.353   3
   0   1 -14 5112.91 153.002  18
   0  -1  14 4868.97 272.299   3
   0  -1 -14 5363.40 256.792   6
   0   1  14 5391.46 290.364   3
   0   1 -14 4742.77 254.940   6
   0   1 -14 4588.85 142.142  15
   0  -1 -14 5113.43 155.148  18
   0  -1  15 3502.08 239.361   3
   0  -1 -15 3733.48 216.803   6
   0   1 -15 3625.56 130.411  18
   0   1 -15 3704.71 232.218   6
   0   1 -15 3172.73 121.531  15
   0  -1 -15 3944.82 136.397  18
   0   1  15 3645.32 249.979   3
   0  -1  16 1101.95 138.395   3
   0   1 -16 1108.28 72.2511  15
   0   1 -16 1269.92 76.7265  18
   0   1  16 1175.64 146.724   3
   0   1 -16 1185.46 136.719   6
   0  -1 -16 1298.47 79.1521  18
   0   1 -17 2592.32 114.686  18
   0   1 -17 2627.92 207.924   6
   0  -1 -17 2466.88 111.138  15
   0  -1  17 2702.91 221.171   3
   0  -1 -17 3058.73 124.528  18
   0   1  17 2793.71 232.451   3
   0   1 -17 2529.09 111.872  15
   0   1 -18 2662.89 116.117  18
   0   1 -18 2549.78 114.336  15
   0  -1 -18 2733.55 116.968  15
   0   1 -19 2414.61 112.065  15
   0   1 -19 2311.01 103.551   7
   0  -1 -19 2470.59 112.433  15
   0   1 -19 2443.33 110.008  18
   0   1 -20 6.53914 26.0273  18
   0  -1 -20 92.2407 25.9658   7
   0   1 -20 66.5579 28.5148  15
   0   1 -20 71.2122 26.9856   7
   0  -1 -20 79.6306 31.0584  15
   0  -1 -21 5539.31 151.995   7
   0   1 -21 5685.06 169.248  15
   0   1 -21 5179.93 154.708   7
   0  -1 -21 5446.28 164.626  15
   0   1 -22 14.7753 19.0053   7
   0  -1 -22 15.5946 15.9087   7
   0  -1 -22 11.3301 20.2476  15
   0   1 -22 30.3915 25.2742  15
   0  -1 -23-2.35068 16.8609  15
   0   1 -23 28.6357 20.4144  15
   0   1 -23 5.15057 14.4227   7
   0  -1 -23-14.2846 14.8699   7
   0   1 -24 90.1573 16.2296  10
   0  -1 -24 107.720 20.5575  15
   0   1 -24 98.1243 17.8828   7
   0   2   0 20698.3 339.764   5
   0   2   0 21169.8 339.471   1
   0   2   0 21531.1 352.039   2
   0   2   0 21524.4 324.138   6
   0   2  -1 102919. 1437.87   1
   0   2  -1 104488. 1435.06   6
   0   2   1 103613. 1477.17   2
   0   2   1 106994. 1406.88   4
   0   2  -2 4338.58 123.215   6
   0  -2   2 4437.88 92.0538   3
   0   2  -2 4155.04 111.426   1
   0  -2   3 25581.9 404.098   3
   0   2  -3 26138.7 421.407   1
   0  -2   4 21437.6 373.735   3
   0   2   4 23686.0 458.842   2
   0   2   5 81746.5 1208.52   2
   0  -2   5 73246.6 1106.61   3
   0   2   6 21680.4 463.597   2
   0  -2   6 19098.6 392.848   3
   0  -2   7 77873.7 1225.41   3
   0   2   7 83834.4 1291.44   2
   0   2   8 4751.69 199.232   3
   0  -2   8 4498.29 185.084   3
   0   2   8 4530.00 199.709   2
   0   2   9 2144.11 139.556   2
   0  -2   9 2469.01 143.453   3
   0   2   9 2267.99 145.311   3
   0   2 -10 895.151 98.2210   6
   0  -2  10 852.793 91.7860   3
   0   2  10 851.609 97.6680   3
   0   2  11 40095.7 847.990   3
   0  -2  11 41916.7 848.177   3
   0  -2  12 30978.6 704.165   3
   0   2 -12 30118.9 697.843   6
   0   2 -13 15282.6 479.230   6
   0  -2  13 15042.9 480.033   3
   0   2  13 14701.7 480.504   3
   0   2 -14 717.138 56.2128  18
   0   2  14 638.198 108.419   3
   0  -2  14 808.163 111.911   3
   0   2 -14 762.410 104.405   6
   0   2 -14 682.731 53.0516  15
   0  -2 -14 802.009 60.0819  18
   0   2 -14 748.296 42.4157  17
   0  -2 -15 2335.79 105.345  18
   0  -2  15 1865.70 169.788   3
   0   2 -15 2028.54 97.4606  18
   0   2 -15 2164.70 184.433   6
   0   2 -15 2219.42 76.9715  17
   0   2  15 1912.37 181.016   3
   0   2 -15 2049.33 94.4769  15
   0  -2  16 1913.88 176.861   3
   0   2 -16 2050.09 99.3417  18
   0   2 -16 1798.20 91.6076  15
   0   2  16 1913.94 188.523   3
   0   2 -16 1778.88 172.508   6
   0  -2 -17 3336.34 128.045  15
   0   2 -17 3405.23 242.368   6
   0   2 -17 3291.59 131.115  15
   0   2 -17 3409.39 131.713  18
   0   2 -18 956.765 67.7905   7
   0   2 -18 935.840 69.9726  15
   0   2 -18 986.710 70.1074  18
   0  -2 -18 1004.65 71.2034  15
   0   2 -19 4353.93 149.167  18
   0   2 -19 3951.91 140.310   7
   0  -2 -19 3940.51 143.883  15
   0   2 -19 4125.46 148.753  15
   0   2 -20 28.9368 25.4183  15
   0   2 -20 7.03814 23.7830  18
   0  -2 -20 68.5243 26.3787  15
   0  -2 -20 69.7410 22.1468   7
   0   2 -20 53.9609 25.3356   7
   0   2 -21-8.90457 23.9555  18
   0  -2 -21 27.9432 15.3310  19
   0   2 -21 34.1934 20.7330   7
   0   2 -21 83.6754 30.7524  15
   0  -2 -21 50.5056 25.7649  15
   0   2 -22 311.486 36.2493   7
   0  -2 -22 353.588 38.5743  15
   0  -2 -22 311.137 26.9491  19
   0   2 -22 360.037 41.3914  15
   0  -2 -23 430.083 37.3665  15
   0   2 -23 469.541 38.8681   7
   0   2 -23 532.509 44.4482  15
   0   2 -24-2.66251 8.98683  10
   0  -2 -24 3.08635 12.7501  15
   0   2 -24-0.70141 11.4940   7
   0   3   0 29.7337 14.2177   6
   0   3   0-6.24645 26.3853   2
   0   3   0 42.5393 21.2373   1
   0   3   0-5.23289 19.9185   5
   0   3   1 321792. 4285.44   2
   0   3  -1 314444. 4236.25   6
   0   3  -1 322278. 4244.69   1
   0   3   1 333712. 4197.10   4
   0   3   1 324092. 4233.57   5
   0   3  -2 7416.87 181.684   1
   0   3   2 7226.59 148.244   4
   0   3  -2 7251.16 182.351   6
   0  -3   3 3940.49 96.9469   3
   0   3  -3 3806.19 136.689   6
   0   3   3 3691.67 161.438   2
   0   3  -3 3834.40 125.879   1
   0  -3   4 25734.2 421.874   3
   0   3  -4 26833.9 495.814   6
   0   3   4 26608.8 540.024   2
   0   3  -5 12106.7 307.419   6
   0  -3   5 11489.7 249.667   3
   0   3  -6 36953.5 692.013   6
   0  -3   6 36522.9 625.842   3
   0   3  -7 18503.2 445.031   6
   0   3   7 19595.2 481.994   2
   0  -3   7 19014.7 398.647   3
   0   3  -8 20339.6 494.003   6
   0  -3   8 20330.7 447.711   3
   0   3   8 21261.6 493.370   3
   0   3   9 70.6974 39.3330   3
   0   3  -9 54.9531 42.0980   6
   0  -3   9 113.469 38.6110   3
   0  -3  10 18791.5 463.781   3
   0   3  10 17789.9 487.901   3
   0   3 -10 18482.3 494.770   6
   0   3  11 12328.0 409.090   3
   0  -3  11 13262.4 394.312   3
   0   3 -11 13790.1 429.238   6
   0  -3  12 32981.3 724.332   3
   0   3  12 31260.2 742.969   3
   0   3 -12 33763.7 769.209   6
   0  -3  13 1847.42 151.763   3
   0   3 -13 1854.00 87.9437  18
   0   3 -13 1858.40 161.137   6
   0   3  13 1807.13 162.805   3
   0   3 -13 1766.21 82.2253  15
   0   3 -13 1892.01 91.1143  11
   0   3 -14 3162.21 95.7397  17
   0   3  14 2987.12 222.351   3
   0  -3  14 3125.34 203.510   3
   0   3 -14 2843.71 111.708  15
   0   3 -14 2913.96 210.998   6
   0   3 -14 3055.88 117.888  18
   0   3  14 3282.52 120.560  12
   0   3 -15 1012.33 53.5546  17
   0   3 -15 1151.25 73.9222  18
   0   3 -15 1118.25 136.355   6
   0   3  15 1149.98 73.4194  12
   0   3  15 983.054 135.390   3
   0   3 -15 1049.56 68.5404  15
   0   3 -16 18435.3 320.615  17
   0   3 -16 18457.8 601.318   6
   0   3 -16 17331.1 357.575  15
   0   3  16 18190.8 623.272   3
   0   3  16 18630.7 368.003  12
   0   3 -16 17847.8 364.586  18
   0   3 -17 2327.97 108.435  15
   0   3 -17 2596.17 89.6725  17
   0  -3 -17 2323.29 104.963  15
   0   3 -17 2381.06 110.325  18
   0   3 -17 2302.10 105.208   7
   0   3 -18 5674.15 140.584  17
   0   3 -18 5261.22 169.341  15
   0   3 -18 5423.94 168.194   7
   0   3 -18 5229.54 170.516  18
   0  -3 -18 5003.02 162.522  15
   0  -3 -19 7666.86 205.927  15
   0   3 -19 7928.18 213.634  15
   0   3 -19 8109.46 211.267   7
   0   3 -19 7410.30 206.955  18
   0   3 -20 1161.42 72.8559   7
   0   3 -20 1155.60 72.7610  18
   0  -3 -20 1071.76 68.0229  15
   0   3 -20 1339.76 79.0907  15
   0   3 -21 9539.85 220.998  18
   0  -3 -21 9244.21 191.737  19
   0   3 -21 9865.99 228.465  15
   0   3 -21 9687.11 221.481   7
   0   3 -22 369.331 37.3706   7
   0  -3 -22 330.690 28.7608  19
   0  -3 -22 366.793 36.7936  15
   0   3 -22 327.117 34.8017  18
   0   3 -22 392.065 40.3558  15
   0  -3 -23 1042.62 42.3333  19
   0   3 -23 1024.47 44.3094  10
   0  -3 -23 1081.88 54.1035  15
   0  -3 -24 440.984 28.1266  10
   0   3 -24 489.887 31.0796   7
   0   4   0 145914. 2023.70   1
   0   4   0 146174. 2032.91   5
   0   4   0 145113. 1984.49   6
   0   4  -1 12529.8 292.755   5
   0   4  -1 13168.5 269.948   6
   0   4   1 13053.5 282.275   5
   0   4   1 12972.0 281.112   1
   0   4  -1 13204.6 288.906   1
   0   4  -2 14043.0 325.502   5
   0   4   2 15112.6 352.654   2
   0   4   2 13857.6 292.339   5
   0   4   2 13333.5 255.229   4
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   2  12 -10 57.6012 16.8442  18
   2  12 -10 2.52695 10.6471  17
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   2  12  -9 97.3651 19.2952  18
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   2  12  -8 106.023 22.1611  18
   2  12  -8 89.3947 18.8200   8
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   2  12  -7 608.446 43.2691  18
   2  12  -7 628.580 44.7553   8
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   2  12  -6 1414.47 68.3276  18
   2  12  -6 1500.79 71.9663   8
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   2  12  -5 31.6471 16.9274  18
   2  12  -5 75.8126 23.3005   8
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   2  12  -4 3.62836 18.0652  18
   2  12  -4 2.23540 19.2269   8
   2  12  -3 1749.22 80.2303  18
   2  12  -3 1769.79 85.4917   8
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   2  12  -2 964.903 59.2884  18
   2  12  -2 999.080 66.0762   8
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   2  12  -1 35.8994 18.5605  18
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   2  12  -1 23.2123 22.7141   8
   2  12   0 483.934 43.0133  18
   2  12   0 526.031 50.7459   8
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   2  12   1 1057.87 61.5266  18
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   2  12   1 1074.29 69.9091   8
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   2  12   2 36.9994 19.1207  18
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   2  12   2 77.6547 27.4646   8
  -2  12  -3 64.4745 25.2098  11
   2  12   3 38.7755 19.1629  18
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   2  12   3 83.5383 28.6193   8
   2  12   4 87.7743 21.9133  18
  -2  12  -4 61.1059 20.1914  16
  -2  12  -4 69.2382 25.1764  11
   2  12   4 65.0644 26.9940   8
  -2  12  -5 13.6892 16.7259  16
  -2  12  -5 36.1582 21.5471  11
   2  12   5 34.6090 21.9743   8
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  -2  12  -6 246.317 28.6804  16
   2  12   6 245.356 33.4221   8
  -2  12  -7 31.0831 16.3673  16
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   2  12   7 75.0970 22.8663   8
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   2  12   8 36.2130 16.8157   8
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   2  12   9 4.58824 14.2293   8
  -2  13   7 28.8713 14.5875  11
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   2  13  -6 99.2109 17.1599  18
   2  13  -6 107.400 17.7683   8
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   2  13  -5-31.9782 15.7203  18
   2  13  -5 7.06191 12.3880   8
   2  13  -4 252.611 26.5435  18
   2  13  -4 258.014 28.2185   8
  -2  13   4 272.779 30.4040  11
   2  13  -3 61.6304 17.0180  18
  -2  13   3 33.1246 16.8030  11
   2  13  -3 25.1431 14.1471   8
   2  13  -2 4.49954 13.3721  18
  -2  13   2-14.6743 17.1825  11
   2  13  -2 11.9475 16.1786   8
   2  13  -1 951.330 48.6944  18
   2  13  -1 1053.15 56.8206   8
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   2  13   0 1465.19 68.4736   8
   2  13   0 1341.77 57.4318  18
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   2  13   1 67.5327 16.4071  18
   2  13   1 129.630 24.2892   8
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   2  13   2 210.600 28.6159   8
   2  13   3 445.527 37.7418   8
  -2  13  -3 464.311 38.1826  11
  -2  13  -4 211.688 27.9616  11
   2  13   4 197.092 25.4437   8
   2  13   5 353.106 31.3997   8
  -2  13  -5 361.972 31.4167  11
   2  13   6 937.177 46.6318   8
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   3   0 -21 20.4373 11.6602  15
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  -3   0  13-16.8194 22.7550  19
   3   0 -13-1.35644 28.1949   8
  -3   0  13-4.64954 17.6826  12
   3   0 -12 349.446 47.9115   8
  -3   0  12 397.183 39.6260  12
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  -3   0  11 8.99063 21.2662  19
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   3   0 -11-16.3815 27.3900   8
  -3   0  11 26.8463 18.3655  12
   3   0 -10 21311.1 417.911   8
  -3   0  10 21249.9 372.744  12
  -3   0  10 21040.2 380.348  19
  -3   0   9 40.5243 21.8001  19
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   3   0  -9 17.6458 27.4182   8
  -3   0   9 19.2705 16.7742  12
  -3   0   8 12579.2 499.036   3
  -3   0   8 12745.8 253.608  19
   3   0  -8 13023.8 289.028   8
  -3   0   7-14.2668 17.0726  19
  -3   0   7 20.3117 16.6825  10
   3   0  -7-19.3511 23.0396   8
  -3   0   6 8298.20 181.317  19
  -3   0   6 8069.37 184.371  10
   3   0  -6 7607.10 203.342   8
   3   0  -6 8126.69 341.723   2
  -3   0   6 7995.59 297.227   4
  -3   0   5 22.9767 15.1673  19
  -3   0   5-0.84545 12.5124  10
  -3   0   5-15.2204 31.4974   4
   3   0  -5 4.75474 31.4157   2
  -3   0   4 1084.89 54.8116  19
  -3   0   4 1090.14 58.2458  10
  -3   0   4 969.017 92.3989   4
   3   0  -3 14.7066 34.3598   2
  -3   0   3-12.3876 15.1453  10
  -3   0   3 15.1564 24.2054   4
   3   0  -2 16766.2 499.995   2
  -3   0   2 16610.6 419.721   4
   3   0  -1 223.341 54.6132   2
  -3   0   1 57.8976 26.8751   4
   3   0   0 7309.63 311.175   2
   3   0   1 38.7611 33.7091   2
  -3   0  -1-0.76265 12.7220  10
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   3   0   2 9855.02 371.363   2
   3   0   3-26.7904 29.3233   2
  -3   0  -3 3.91586 16.5949  10
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   3   0   4 876.264 113.121   2
  -3   0  -5-5.30081 14.0461  19
  -3   0  -5 4.11843 15.6280  10
  -3   0  -5 42.9526 17.8123  13
   3   0   6 5416.48 284.752   2
  -3   0  -6 5637.96 159.556  10
  -3   0  -6 5502.99 156.239  13
   3   0   7 47.7981 37.6618   2
  -3   0  -7 8.57647 19.7496  10
  -3   0  -7 49.4771 23.8921  13
   3   0   8 8057.51 364.322   2
  -3   0  -8 8435.17 217.477  10
  -3   0  -8 8310.36 213.688  13
   3   0   9-12.2616 50.2014   2
  -3   0  -9 46.7374 32.2447  10
  -3   0  -9 31.2381 25.3657  13
  -3   0 -10 44581.3 734.120  10
  -3   0 -11 22.2736 27.3790  10
  -3   0 -12 11970.1 285.286  10
  -3   0 -13-27.7851 33.2262  10
  -3   0 -14 7569.78 206.564  10
  -3   0 -15 30.2796 27.2943  10
  -3   0 -15 26.9453 21.6061  13
  -3   0 -16 1973.71 86.2912  10
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  -3   0 -18 1688.49 66.6317  10
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   3  -1 -21 101.210 18.6718  15
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   3   1 -20 89.6722 19.2713  15
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  -3   1  19 706.492 49.5930  12
  -3  -1  19 713.197 48.5532  12
  -3   1  18 379.505 40.4414  12
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  -3   1  17-7.74742 22.3253  12
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  -3  -1  15 634.537 51.1420  12
  -3   1  14 1674.45 91.1291  19
   3   1 -14 1470.76 89.9987   8
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   3   1 -13 65.2875 32.4549   8
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   3   1 -12 3802.62 148.026   8
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   3  -1 -11 1243.77 82.2039   8
   3   1 -11 1392.48 87.3127   8
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   3  -1 -10 38.6402 27.3033   8
   3   1 -10 30.5911 24.1562   8
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   3  -1  -9 137.489 31.0198   8
   3   1  -9 128.182 31.1579   8
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   3   1  -9 85.7627 54.9242   2
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   3  -1  -8 596.532 54.1662   8
   3   1  -8 509.805 50.1235   8
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  -3   1   8 611.514 42.8661  12
   3   1  -8 537.362 80.7925   2
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  -3  -1   7-11.0246 32.1315   3
   3  -1  -7 33.7020 23.8112   8
   3   1  -7 45.9974 23.9104   8
  -3   1   7 35.3691 14.9982  12
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   3   1  -7 4.22074 30.3163   2
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  -3   1   6 3225.19 106.732  10
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   3  -1  -6 3338.57 121.902   8
   3   1  -6 3379.06 125.700   8
  -3   1   6 3370.37 190.464   4
   3   1  -6 3248.76 203.501   2
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  -3  -1   5 1647.55 72.0233  10
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   3   1  -5 1503.37 80.1039   8
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   3   1  -5 1414.55 133.295   2
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   3   1  -4 1794.23 146.970   2
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  -3   1   3 7159.59 171.770  10
  -3  -1   3 7259.98 169.812  10
   3  -1  -3 6797.74 313.233   2
  -3   1   3 6830.08 266.426   4
   3   1  -3 6518.54 291.831   2
  -3   1   2 4347.02 126.636  10
   3  -1  -2 4384.95 246.702   2
   3   1  -2 4255.52 230.138   2
  -3   1   2 4242.08 202.085   4
  -3   1   1 24747.8 415.771  10
   3  -1  -1 24493.1 643.390   2
   3   1  -1 23958.0 622.647   2
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   3  -1   0 83919.5 1505.16   2
   3   1   0 81781.6 1493.72   2
  -3   1  -1 26252.6 442.592  10
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   3  -1   1 24665.4 643.710   2
   3   1   1 24719.7 653.864   2
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  -3   1  -2 15273.9 299.368  10
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   3  -1   2 16274.5 490.423   2
   3   1   2 16856.9 508.526   2
  -3   1  -3 1016.55 60.1311  10
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   3  -1   3 1032.87 116.040   2
   3   1   3 1093.32 124.798   2
  -3  -1  -4 5564.34 147.674  19
  -3   1  -4 5455.90 154.050  10
  -3  -1  -4 5620.31 154.010  10
  -3   1  -4 6000.88 147.664  16
   3   1   4 5604.42 288.408   2
  -3   1  -4 5339.18 153.502  13
   3  -1   4 6075.98 288.227   2
  -3  -1  -5 3226.79 108.452  19
   3   1   5 3073.75 215.175   2
  -3   1  -5 3134.36 112.379  10
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  -3   1  -5 3090.54 100.613  16
  -3   1  -5 2926.51 110.279  13
   3  -1   5 2845.95 198.801   2
   3  -1   6 30032.7 751.415   2
  -3  -1  -6 31621.0 515.326  19
   3   1   6 30873.0 789.702   2
  -3   1  -6 30423.2 523.838  10
  -3  -1  -6 31981.9 525.194  10
  -3   1  -6 31357.3 530.494  13
  -3   1  -6 31827.6 522.048   7
  -3  -1  -7 17384.6 329.463  19
   3  -1   7 16137.9 520.954   2
   3   1   7 16950.3 559.900   2
  -3   1  -7 16706.5 341.463  10
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  -3   1  -7 17131.5 346.619  13
  -3   1  -7 17856.2 338.874   7
  -3  -1  -8 53486.3 817.943  19
   3   1   8 52619.2 1168.14   2
  -3   1  -8 54616.6 848.873  10
  -3  -1  -8 54542.2 844.623  10
   3  -1   8 51440.0 1109.17   2
  -3   1  -8 54814.7 855.003  13
  -3   1  -8 55733.5 838.907   7
   3  -1   9 974.381 124.248   2
  -3   1  -9 1201.25 77.9982  10
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   3   1   9 849.240 130.441   2
  -3  -1  -9 1016.84 62.6727  19
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  -3   1 -10 1766.09 96.1734  10
  -3  -1 -10 1940.47 100.245  10
  -3   1 -11 23286.2 445.581  10
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  -3  -1 -13 338.704 45.9853  10
  -3   1 -14 2185.94 101.513  10
  -3  -1 -14 2011.93 97.9967  10
  -3   1 -15 295.794 37.6685  10
  -3  -1 -15 324.624 41.4852  10
  -3   1 -15 268.126 38.4394  13
  -3  -1 -16 331.585 37.6102  10
  -3   1 -16 322.525 36.4616  10
  -3   1 -16 345.221 37.8867  13
  -3   1 -17 1242.94 62.3391  10
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  -3   1 -19 129.698 17.0871  10
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  -3   2  20 72.4214 20.8228  12
  -3  -2  20 74.1776 18.1501  12
  -3   2  19 2954.42 103.565  12
  -3  -2  19 2770.51 92.6300  12
  -3   2  18 153.057 32.1703  12
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  -3   2  17 699.100 54.6191  12
  -3  -2  17 675.080 48.7693  12
  -3   2  16 732.236 56.9270  12
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   3   2 -15 509.637 53.5179   8
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  -3  -2  15 440.481 46.9347  19
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   3   2 -14 308.013 45.0387   8
  -3   2  14 500.352 48.1255  12
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   3   2 -13 26400.9 508.291   8
  -3   2  13 27019.9 469.094  12
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  -3  -2  13 26202.8 469.537  19
  -3   2  12 86.1691 30.1073  19
  -3  -2  12 89.4829 25.9526  19
   3   2 -12 71.0072 32.4989   8
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  -3   2  11 1832.74 203.728   3
  -3  -2  11 1566.88 184.682   3
  -3  -2  11 1628.98 78.6686  19
   3   2 -11 1670.00 95.5284   8
  -3   2  11 1664.59 79.8515  12
  -3   2  11 1460.50 82.4138  19
  -3   2  10 55.0650 23.5153  19
  -3  -2  10 82.7240 22.3551  19
  -3   2  10 105.946 56.0105   3
  -3  -2  10 79.5381 47.5413   3
   3   2 -10 33.2856 26.8178   8
  -3   2  10 69.3290 22.4677  12
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  -3   2   9 4994.63 308.954   3
  -3  -2   9 4394.39 291.975   3
   3   2  -9 4751.49 162.399   8
  -3   2   9 4620.50 133.784  12
  -3   2   9 4472.94 140.070  19
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   4   7 -11 25.6004 17.5072   8
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   4   7 -10 18.9425 19.6943   8
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  -4  -7   9 106.166 18.3311  19
  -4   7   9 84.9183 21.4682  14
   4   7  -9 120.962 26.6713   8
  -4   7   8 2202.08 85.4458  11
  -4   7   8 2340.66 82.0187  16
   4   7  -8 2269.83 98.0086   8
  -4   7   8 2166.64 89.3164  14
  -4  -7   8 2252.64 75.8614  19
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   4   7  -7 2910.68 115.255   8
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  -4   7   6 41.0299 19.1345  11
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   4   7  -6 57.4241 30.2144   8
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   4   7  -5 18.6183 26.7692   8
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   4   7  -4 3557.55 136.339   8
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   4   7  -2 109.366 31.4321   8
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   4   7  -1 147.503 35.9212   8
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  -4  -7  -4 1818.36 75.9620  19
  -4   7  -4 1739.29 83.1610  16
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   4   8 -10 72.5159 20.1619   8
   4   8  -9 442.656 38.4762   8
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   4   8  -8 1258.19 65.5049   8
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   4   8  -7 1714.71 79.0437   8
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   4   8  -6 22.1731 22.8687   8
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   4   8  -5 29.2255 22.2181   8
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   4   8  -4 670.595 54.7090   8
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   4   8  -3 430.819 45.1502   8
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   4   8  -2 464.589 47.6307   8
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   4   8  -1 93.0617 26.9343   8
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   4   9  -9 28.3587 14.8080   8
   4   9  -8 549.066 37.7875   8
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   4   9  -7 1014.41 53.2902   8
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   4   9  -6 401.661 35.5614   8
  -4   9   6 316.985 27.1414  11
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   4   9  -5 204.686 27.9310   8
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   4   9  -4 506.925 41.8322   8
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   4   9  -3 1129.94 61.1344   8
  -4  -9   2-1.80212 10.1264  19
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   4   9  -2 13.4123 18.1955   8
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   4   9  -1 1160.29 62.7085   8
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   4   9   0 105.594 23.9896   8
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  -5  -3   2 336.978 31.1025  19
  -5   3   2 319.737 31.2335  16
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  -5   4   7 221.651 24.1985  16
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  -5   4   6 629.477 39.4968  16
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  -5   4   3 63.4971 18.7365  16
  -5  -4   2 1508.76 60.4758  19
  -5   4   2 1496.22 62.7697  16
  -5  -4   1 121.713 20.1557  19
  -5   4   1 146.214 22.2558  16
  -5  -4   0 88.4704 16.8050  19
  -5   4   0 93.9727 19.7024  16
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  -5   4  -1 1802.34 67.6840  16
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  -5   4  -2 3916.58 99.5853  10
  -5   4  -2 4094.43 105.423  16
  -5   4  -3 5396.10 116.683  10
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  -5  -4  -4 221.294 21.1424  19
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  -5   5   7 36.7271 12.9288  16
  -5  -5   6 53.4143 12.4722  19
  -5   5   6 18.7888 12.2583  16
  -5   5   5 185.254 22.2325  16
  -5  -5   5 240.110 22.5176  19
  -5  -5   4 140.982 19.1208  19
  -5   5   4 94.2238 18.3618  16
  -5  -5   3 635.186 36.5125  19
  -5   5   3 653.003 40.1465  16
  -5  -5   2 54.2607 14.1994  19
  -5   5   2 85.4259 19.4213  16
  -5  -5   1 274.652 25.4069  19
  -5   5   1 256.599 26.7314  16
  -5  -5   0 499.935 32.7841  19
  -5   5   0 494.024 34.4722  16
  -5  -5  -1 540.249 33.3969  19
  -5   5  -1 502.930 34.1188  16
  -5  -5  -2 1508.14 55.3465  19
  -5   5  -2 1604.81 58.7852  16
  -5  -5  -3 311.509 24.0592  19
  -5  -6   5 16.3443 8.48246  19
  -5  -6   4 82.6628 13.3671  19
  -5   6   4 80.3583 15.7031  16
  -5  -6   3 637.328 33.1323  19
  -5   6   3 632.381 36.4046  16
  -5  -6   2 21.9849 10.8852  19
  -5   6   2 50.6349 15.0036  16
  -5  -6   1 254.143 21.6337  19
  -5   6   1 263.921 24.4911  16
  -5  -6   0 52.7283 12.5893  19
  -5   6   0 35.3219 12.8620  16
  -5  -6  -1 339.503 23.5235  19
   0   0   0    0.00    0.00   0
TITL bmk2260b_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   4.471717  11.936678  20.138209  90.0000  95.6888  90.0000
ZERR    2.00   0.000068   0.000200   0.000314   0.0000   0.0015   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 36.00 20.00 8.00 4.00
SIZE 0.06 0.21 0.34
TREF
HKLF 4
END
;
_shelx_hkl_checksum              73122
_shelx_res_file
;
TITL bmk2260b in P2(1)/c
    shelx.res
    created by SHELXL-2018/1 at 17:13:06 on 09-Jan-2023
CELL  1.54184   4.4717  11.9367  20.1382   90.000   95.689   90.000
ZERR     4.00   0.0001   0.0002   0.0003    0.000    0.002    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    CL
UNIT  36 32 12 12 4
MERG   2
simu .01 n1 > o2a
isor .01 n1 > o2a
eadp c1 c1a
exyz c1 c1a
EQIV $1 -x, -y+2, -z+1
HTAB N3 O3_$1
MPLA C1 N1 O1 O2
MPLA C1 C2 C3 C4 C5 C6 C7 C8 C9 N2 N3 O3 CL1
MPLA C1 N1A O1A O2A
FMAP   2
PLAN   10
SIZE     0.060   0.210   0.340
ACTA
BOND   $H
LIST   4
L.S.   4
WGHT    0.062800    0.256200
FVAR       6.60187   0.83717
PART  1
C1    1    1.168664    0.640785    0.655664    21.00000    0.03989    0.04477 =
         0.05654    0.01065    0.00392   -0.00019
N1    3    1.248032    0.529161    0.632306    21.00000    0.06276    0.04812 =
         0.07494    0.00867   -0.00194    0.00609
O1    4    1.253396    0.451428    0.672926    21.00000    0.13671    0.05232 =
         0.09105    0.01884   -0.01695    0.00842
O2    4    1.295816    0.516303    0.575431    21.00000    0.17138    0.07000 =
         0.09662   -0.00504    0.04909    0.02867
PART  2
same .001 c1 > o2
C1A   1    1.168664    0.640785    0.655664   -21.00000    0.03989    0.04477 =
         0.05654    0.01065    0.00392   -0.00019
N1A   3    1.242000    0.522243    0.646421   -21.00000    0.07099    0.05543 =
         0.07818    0.01464    0.00681    0.00162
O1A   4    1.033823    0.454268    0.647107   -21.00000    0.12248    0.07709 =
         0.14563   -0.00545    0.00318   -0.01507
O2A   4    1.499514    0.494580    0.647535   -21.00000    0.07199    0.06048 =
         0.13811   -0.00669    0.00982    0.02675
PART  0
C2    1    1.300399    0.687342    0.714546    11.00000    0.03617    0.05691 =
         0.05092    0.01771    0.00136   -0.00120
C3    1    1.221557    0.794763    0.731095    11.00000    0.04572    0.06254 =
         0.04351    0.00483   -0.00461   -0.00523
AFIX  43
H3    2    1.313563    0.828395    0.769479    11.00000   -1.20000
AFIX   0
C4    1    1.005675    0.852545    0.690636    11.00000    0.04456    0.04965 =
         0.04640    0.00180    0.00031   -0.00022
AFIX  43
H4    2    0.952715    0.924666    0.702441    11.00000   -1.20000
AFIX   0
C5    1    0.866672    0.804682    0.632683    11.00000    0.03432    0.04646 =
         0.04211    0.00841    0.00215   -0.00185
C6    1    0.953877    0.698022    0.614539    11.00000    0.04177    0.04619 =
         0.04613    0.00486   -0.00047   -0.00281
AFIX  43
H6    2    0.868744    0.665462    0.575164    11.00000   -1.20000
AFIX   0
C7    1    0.629285    0.866554    0.592891    11.00000    0.03560    0.04369 =
         0.04468    0.00525    0.00158    0.00025
AFIX  43
H7    2    0.572080    0.936881    0.606968    11.00000   -1.20000
AFIX   0
C8    1    0.121261    0.856075    0.449847    11.00000    0.04180    0.04901 =
         0.04216    0.00147   -0.00029   -0.00222
C9    1    0.201003    0.746322    0.421252    11.00000    0.07857    0.06217 =
         0.06284   -0.01604   -0.01159    0.01094
AFIX 137
H9A   2    0.062133    0.729457    0.383109    11.00000   -1.50000
H9B   2    0.191210    0.688737    0.454244    11.00000   -1.50000
H9C   2    0.401094    0.749991    0.407961    11.00000   -1.50000
AFIX   0
N2    3    0.500505    0.825100    0.539268    11.00000    0.03591    0.04477 =
         0.04439    0.00670    0.00036    0.00276
N3    3    0.277378    0.889961    0.507213    11.00000    0.03960    0.04289 =
         0.04431    0.00058   -0.00440    0.00491
AFIX  43
H3A   2    0.235971    0.953659    0.524035    11.00000   -1.20000
AFIX   0
O3    4   -0.078027    0.917084    0.423454    11.00000    0.05219    0.05908 =
         0.04944   -0.00164   -0.01377    0.00664
CL1   5    1.563695    0.617680    0.768027    11.00000    0.05022    0.07783 =
         0.07354    0.02911   -0.01338    0.00357
HKLF 4
REM  bmk2260b in P2(1)/c
REM R1 =  0.0383 for    1960 Fo > 4sig(Fo)  and  0.0403 for all    2107 data
REM    174 parameters refined using    132 restraints
END
WGHT      0.0628      0.2562
REM Highest difference peak  0.295,  deepest hole -0.265,  1-sigma level  0.044
Q1    1   1.1125  0.4997  0.5836  11.00000  0.05    0.30
Q2    1   1.4523  0.5138  0.6117  11.00000  0.05    0.27
Q3    1   1.4658  0.4992  0.6826  11.00000  0.05    0.26
Q4    1   0.7612  0.8382  0.6118  11.00000  0.05    0.15
Q5    1  -0.1266  0.8848  0.4211  11.00000  0.05    0.15
Q6    1   0.8715  0.7604  0.6190  11.00000  0.05    0.14
Q7    1   0.3663  0.6997  0.4457  11.00000  0.05    0.14
Q8    1   1.1989  0.6610  0.6911  11.00000  0.05    0.14
Q9    1   1.3873  0.6007  0.7938  11.00000  0.05    0.13
Q10   1   1.2031  0.7186  0.7313  11.00000  0.05    0.12
;
_shelx_res_checksum              45453
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
C C1 1.1687(3) 0.64078(14) 0.65566(9) 0.0471(4) Uani d 0.837(4) A 1
N N1 1.2480(5) 0.52916(17) 0.63231(17) 0.0625(7) Uani d 0.837(4) A 1
O O1 1.2534(7) 0.45143(16) 0.67293(12) 0.0952(8) Uani d 0.837(4) A 1
O O2 1.2958(7) 0.51630(18) 0.57543(12) 0.1103(10) Uani d 0.837(4) A 1
C C1A 1.1687(3) 0.64078(14) 0.65566(9) 0.0471(4) Uani d 0.163(4) A 2
N N1A 1.2420(17) 0.5222(3) 0.6464(8) 0.068(3) Uani d 0.163(4) A 2
O O1A 1.034(2) 0.4543(3) 0.6471(9) 0.116(4) Uani d 0.163(4) A 2
O O2A 1.4995(17) 0.4946(6) 0.6475(7) 0.090(3) Uani d 0.163(4) A 2
C C2 1.3004(3) 0.68734(15) 0.71455(8) 0.0482(4) Uani d 1 . .
C C3 1.2216(4) 0.79476(16) 0.73109(8) 0.0512(4) Uani d 1 . .
H H3 1.313563 0.828395 0.769479 0.061 Uiso calc 1 . .
C C4 1.0057(4) 0.85255(15) 0.69064(8) 0.0472(4) Uani d 1 . .
H H4 0.952715 0.924666 0.702441 0.057 Uiso calc 1 . .
C C5 0.8667(3) 0.80468(13) 0.63268(7) 0.0411(3) Uani d 1 . .
C C6 0.9539(3) 0.69802(13) 0.61454(8) 0.0450(4) Uani d 1 . .
H H6 0.868744 0.665462 0.575164 0.054 Uiso calc 1 A 1
C C7 0.6293(3) 0.86655(13) 0.59289(8) 0.0415(3) Uani d 1 . .
H H7 0.572080 0.936881 0.606968 0.050 Uiso calc 1 . .
C C8 0.1213(3) 0.85608(14) 0.44985(8) 0.0446(3) Uani d 1 . .
C C9 0.2010(5) 0.74632(18) 0.42125(11) 0.0691(5) Uani d 1 . .
H H9A 0.062133 0.729457 0.383109 0.104 Uiso calc 1 . .
H H9B 0.191210 0.688737 0.454244 0.104 Uiso calc 1 . .
H H9C 0.401094 0.749991 0.407961 0.104 Uiso calc 1 . .
N N2 0.5005(3) 0.82510(11) 0.53927(6) 0.0419(3) Uani d 1 . .
N N3 0.2774(3) 0.88996(11) 0.50721(7) 0.0428(3) Uani d 1 . .
H H3A 0.235971 0.953659 0.524035 0.051 Uiso calc 1 . .
O O3 -0.0780(3) 0.91708(11) 0.42345(6) 0.0548(3) Uani d 1 . .
Cl Cl1 1.56369(10) 0.61768(4) 0.76803(3) 0.0685(2) Uani 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
C1 0.0399(7) 0.0448(8) 0.0565(9) -0.0002(6) 0.0039(7) 0.0106(7)
N1 0.0628(13) 0.0481(11) 0.0749(17) 0.0061(10) -0.0019(10) 0.0087(10)
O1 0.137(2) 0.0523(11) 0.0910(15) 0.0084(12) -0.0170(14) 0.0188(10)
O2 0.171(2) 0.0700(13) 0.0966(17) 0.0287(14) 0.0491(17) -0.0050(11)
C1A 0.0399(7) 0.0448(8) 0.0565(9) -0.0002(6) 0.0039(7) 0.0106(7)
N1A 0.071(5) 0.055(5) 0.078(5) 0.002(4) 0.007(4) 0.015(4)
O1A 0.122(8) 0.077(6) 0.146(8) -0.015(6) 0.003(7) -0.005(6)
O2A 0.072(5) 0.060(5) 0.138(7) 0.027(4) 0.010(5) -0.007(5)
C2 0.0362(7) 0.0569(9) 0.0509(9) -0.0012(6) 0.0014(6) 0.0177(7)
C3 0.0457(8) 0.0625(10) 0.0435(8) -0.0052(7) -0.0046(7) 0.0048(7)
C4 0.0446(8) 0.0496(9) 0.0464(8) -0.0002(7) 0.0003(6) 0.0018(7)
C5 0.0343(7) 0.0465(8) 0.0421(7) -0.0018(6) 0.0021(6) 0.0084(6)
C6 0.0418(7) 0.0462(8) 0.0461(8) -0.0028(6) -0.0005(6) 0.0049(6)
C7 0.0356(7) 0.0437(8) 0.0447(8) 0.0003(6) 0.0016(6) 0.0053(6)
C8 0.0418(7) 0.0490(8) 0.0422(8) -0.0022(6) -0.0003(6) 0.0015(6)
C9 0.0786(13) 0.0622(11) 0.0628(11) 0.0109(10) -0.0116(10) -0.0160(9)
N2 0.0359(6) 0.0448(7) 0.0444(7) 0.0028(5) 0.0004(5) 0.0067(5)
N3 0.0396(6) 0.0429(7) 0.0443(7) 0.0049(5) -0.0044(5) 0.0006(5)
O3 0.0522(6) 0.0591(7) 0.0494(6) 0.0066(5) -0.0138(5) -0.0016(5)
Cl1 0.0502(3) 0.0778(4) 0.0735(3) 0.0036(2) -0.0134(2) 0.0291(2)
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'
Cl Cl 0.3639 0.7018 '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
C6 C1 C2 . . 121.62(15) ?
C6 C1 N1 . . 115.56(19) ?
C2 C1 N1 . . 122.81(18) ?
O2 N1 O1 . . 123.0(2) ?
O2 N1 C1 . . 119.7(2) ?
O1 N1 C1 . . 117.3(3) ?
C6 C1A C2 . . 121.62(15) ?
C6 C1A N1A . . 123.4(6) ?
C2 C1A N1A . . 114.4(6) ?
O2A N1A O1A . . 122.9(3) ?
O2A N1A C1A . . 119.4(3) ?
O1A N1A C1A . . 117.0(3) ?
C3 C2 C1 . . 118.81(14) ?
C3 C2 C1A . . 118.81(14) ?
C3 C2 Cl1 . . 118.12(13) ?
C1 C2 Cl1 . . 123.06(14) ?
C1A C2 Cl1 . . 123.06(14) ?
C2 C3 C4 . . 120.07(16) ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C3 C4 C5 . . 121.15(16) ?
C3 C4 H4 . . 119.4 ?
C5 C4 H4 . . 119.4 ?
C4 C5 C6 . . 118.90(14) ?
C4 C5 C7 . . 119.45(14) ?
C6 C5 C7 . . 121.64(14) ?
C1A C6 C5 . . 119.37(15) ?
C1 C6 C5 . . 119.37(15) ?
C1 C6 H6 . . 120.3 ?
C5 C6 H6 . . 120.3 ?
N2 C7 C5 . . 120.71(14) ?
N2 C7 H7 . . 119.6 ?
C5 C7 H7 . . 119.6 ?
O3 C8 N3 . . 118.88(15) ?
O3 C8 C9 . . 123.02(15) ?
N3 C8 C9 . . 118.10(15) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C7 N2 N3 . . 115.24(13) ?
C8 N3 N2 . . 121.54(13) ?
C8 N3 H3A . . 119.2 ?
N2 N3 H3A . . 119.2 ?
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
C1 C6 . 1.385(2) ?
C1 C2 . 1.387(2) ?
C1 N1 . 1.468(3) ?
N1 O2 . 1.196(4) ?
N1 O1 . 1.236(3) ?
C1A C6 . 1.385(2) ?
C1A C2 . 1.387(2) ?
C1A N1A . 1.469(3) ?
N1A O2A . 1.196(4) ?
N1A O1A . 1.236(4) ?
C2 C3 . 1.379(3) ?
C2 Cl1 . 1.7281(15) ?
C3 C4 . 1.384(2) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.390(2) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.391(2) ?
C5 C7 . 1.465(2) ?
C6 H6 . 0.9300 ?
C7 N2 . 1.273(2) ?
C7 H7 . 0.9300 ?
C8 O3 . 1.230(2) ?
C8 N3 . 1.351(2) ?
C8 C9 . 1.489(3) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
N2 N3 . 1.3726(17) ?
N3 H3A . 0.8600 ?
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
N3 H3A O3 3_576 0.86 2.04 2.8803(18) 166.9 yes
C3 H3 O1 2_856 0.93 2.61 3.442(3) 149.3 yes
C9 H9A O1A 3_666 0.96 2.30 2.906(8) 120.0 yes

_cod_database_fobs_code 2022830