#------------------------------------------------------------------------------
#$Date: 2021-04-23 12:50:23 +0300 (Fri, 23 Apr 2021) $
#$Revision: 264471 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022362.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_2022362
loop_
_publ_author_name
'Szczesio, Ma\/lgorzata'
'Gobis, Katarzyna'
'Korona-G\/lowniak, Izabela'
'Mazerant-Politowicz, Ida'
'Ziembicka, Dagmara'
'Foks, Henryk'
'G\/l\'owka, Marek'
'Olczak, Andrzej'
_publ_section_title
;
Synthesis, structure and biological activity of four new
picolinohydrazonamide derivatives
;
_journal_coeditor_code FM3063
_journal_issue 7
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 673
_journal_page_last 680
_journal_paper_doi 10.1107/S2053229620007822
_journal_volume 76
_journal_year 2020
_chemical_formula_iupac 'C6 H7 Cl N4'
_chemical_formula_moiety 'C6 H7 Cl N4'
_chemical_formula_sum 'C6 H7 Cl N4'
_chemical_formula_weight 170.61
_chemical_name_common
;
6-Chloropicolinohydrazonamide
;
_chemical_name_systematic
;
N'-Amino-6-chloropyridine-2-carboximidamide
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2014
_cell_angle_alpha 90.0
_cell_angle_beta 90.0
_cell_angle_gamma 90.0
_cell_formula_units_Z 4
_cell_length_a 3.77379(4)
_cell_length_b 5.63483(4)
_cell_length_c 32.9783(2)
_cell_measurement_reflns_used 16896
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 78.5140
_cell_measurement_theta_min 4.0280
_cell_volume 701.273(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9765
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy Dualflex Pilatus 300K'
_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 0.0514
_diffrn_reflns_av_sigmaI/netI 0.0470
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 41
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 19459
_diffrn_reflns_theta_full 66.9682
_diffrn_reflns_theta_max 78.6751
_diffrn_reflns_theta_min 4.0214
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 4.264
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_correction_T_min 0.22
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.616
_exptl_crystal_description plate
_exptl_crystal_F_000 352
_exptl_crystal_size_max 0.83
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.201
_refine_diff_density_min -0.217
_refine_ls_abs_structure_details
;
Flack x determined using 533 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.014(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 112
_refine_ls_number_reflns 1471
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0208
_refine_ls_R_factor_gt 0.0206
_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^)+(0.0336P)^2^+0.1754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0563
_refine_ls_wR_factor_ref 0.0564
_reflns_number_gt 1460
_reflns_number_total 1471
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file fm3063sup1.cif
_cod_data_source_block 6
_cod_database_code 2022362
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 3 33.4502 89.5284 40
0 0 3 22.2186 62.5135 2
0 0 -4 17562.1 692.469 17
0 0 -4 15819.0 748.509 28
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0 0 -5 120.298 108.468 15
0 0 -5 309.664 88.1769 17
0 0 5 36.9015 133.054 40
0 0 -5 69.9040 106.027 28
0 0 5 54.3557 103.873 2
0 0 -6 54256.4 2001.51 15
0 0 -6 50728.3 1804.60 17
0 0 6 52410.7 2065.51 40
0 0 -6 51689.2 1950.07 28
0 0 6 52224.0 2045.07 2
0 0 -7-20.7384 139.294 15
0 0 -7 49.9444 80.9199 17
0 0 7 77.1994 185.472 40
0 0 -7 18.2540 106.717 28
0 0 7 24.9645 133.762 2
0 0 -8 39809.0 1664.73 15
0 0 -8 37863.5 1579.21 28
0 0 8 37765.8 1695.50 2
0 0 -8 36817.6 1385.65 17
0 0 -9 133.092 149.279 15
0 0 -9 76.8165 72.6252 17
0 0 -9 45.4485 140.614 28
0 0 9 95.8968 162.930 2
0 0 -10 98128.2 3726.94 15
0 0 -10 102945. 3837.10 39
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0 0 -11 81.8192 146.135 28
0 0 -11 128.903 127.892 4
0 0 11 116.696 192.961 2
0 0 -12 92445.4 3563.93 39
0 0 12 86459.6 3254.55 16
0 0 -12 88128.5 2968.26 17
0 0 -12 82660.4 3317.15 28
0 0 -12 88669.8 3288.93 4
0 0 12 83839.0 3509.04 2
0 0 13 204.396 163.761 16
0 0 -13 206.435 89.8525 17
0 0 -13 44.7263 181.180 39
0 0 -13-32.3124 177.231 28
0 0 -13-30.2877 137.189 4
0 0 13 184.189 215.377 2
0 0 -14 508807. 16527.9 39
0 0 -14 489835. 16133.2 4
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0 0 -14 495359. 16223.1 28
0 0 -14 497698. 15721.3 17
0 0 14 497435. 16144.2 16
0 0 -15 183.572 84.0144 17
0 0 15-35.3032 136.925 16
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0 0 15-53.5526 177.119 2
0 0 -15 34.6241 145.987 4
0 0 -15 115.268 190.614 28
0 0 16 11067.3 1025.20 2
0 0 -16 11936.9 868.873 4
0 0 -16 11399.5 911.611 28
0 0 16 11645.0 883.715 16
0 0 -16 11102.5 589.035 17
0 0 17 37.7479 152.888 21
0 0 -17-14.5422 58.9018 17
0 0 17-42.3916 185.453 16
0 0 -17-27.4848 140.075 34
0 0 -17 179.490 196.307 28
0 0 -17 76.4342 134.051 4
0 0 -18 352318. 11858.1 17
0 0 18 379891. 12562.1 16
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0 0 18 385393. 12465.4 21
0 0 -18 380362. 12200.3 34
0 0 18 371679. 12081.6 31
0 0 -18 377189. 12691.5 28
0 0 18 380264. 12972.0 2
0 0 -18 378114. 12385.1 4
0 0 -19 77.4246 110.926 4
0 0 19 70.3528 164.551 2
0 0 19 301.768 179.686 23
0 0 -19 59.7412 144.042 22
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0 0 -19 115.169 79.3936 17
0 0 -19 95.1900 138.856 34
0 0 -19 208.687 202.343 28
0 0 19 132.509 131.509 31
0 0 19 50.1251 211.337 16
0 0 20 18823.1 1270.24 5
0 0 20 21546.4 1623.36 2
0 0 20 18076.6 1235.97 45
0 0 20 18677.8 1285.93 41
0 0 20 20675.1 1412.65 16
0 0 -20 17785.6 913.034 17
0 0 -20 21012.0 1189.61 34
0 0 -20 21156.3 1456.43 28
0 0 20 19607.1 1306.41 32
0 0 20 18691.1 1079.53 31
0 0 -20 19350.1 1121.89 22
0 0 20 21729.6 1349.87 21
0 0 20 20174.9 1198.98 23
0 0 21 59.2941 155.028 16
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0 0 21 95.7998 158.414 5
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0 0 -21-84.6332 197.913 43
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0 0 21 62.9043 132.601 31
0 0 21 40.0283 187.212 23
0 0 -21 240.206 170.229 22
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0 0 -22 8777.40 801.631 43
0 0 22 9062.99 884.918 41
0 0 22 8390.54 938.534 16
0 0 -22 8622.80 753.933 34
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0 0 -22 8574.11 676.851 24
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0 0 -23-47.7266 193.304 43
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0 0 -24 1549.25 388.321 43
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0 0 -24 2352.64 416.746 34
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0 0 -28 971332. 30081.3 43
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0 0 30 56669.3 3047.90 21
0 0 30 56419.5 3050.91 23
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0 0 -41 64.7843 101.014 14
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-3 -5 4 1030.17 348.375 38
3 5 4 1286.20 234.955 32
-3 5 -4 1464.30 300.754 25
3 -5 -4 1438.80 269.072 22
-3 -5 5 14833.9 1167.64 38
3 5 5 19186.6 946.574 45
-3 5 -5 15699.3 1269.83 7
3 -5 -5 17164.0 996.958 22
-3 5 -5 15748.6 1027.35 25
3 -5 -6 19054.8 1046.48 22
-3 5 -6 20565.9 1139.86 25
-3 5 -7 1782.28 317.010 25
-3 -5 7 1686.48 368.586 38
-3 5 -8 7594.93 631.497 25
-3 -5 8 7896.13 731.678 38
-3 -5 9 25002.5 1386.21 38
-3 -5 12 434.420 147.741 38
-4 0 0 114282. 4221.25 12
-4 0 1 4696.18 667.470 26
-4 0 -1 4879.49 497.042 12
-4 0 1 5301.53 538.997 12
-4 0 -1 4783.68 578.776 13
-4 0 -1 4625.30 597.946 37
-4 0 2 20864.3 1466.28 26
-4 0 -2 22732.9 1442.32 37
-4 0 -2 23266.9 1221.59 12
-4 0 2 24555.7 1320.46 12
-4 0 -2 24728.7 1411.45 13
-4 0 -3 1865.58 407.264 37
-4 0 3 2167.25 451.507 38
-4 0 -3 1691.06 435.868 26
-4 0 3 1672.49 329.847 12
-4 0 -3 1610.22 344.344 13
-4 0 -3 1992.46 301.899 12
-4 0 -4 830.703 308.155 37
-4 0 4 861.680 355.825 38
-4 0 -4 398.513 282.932 26
-4 0 4 421.943 247.273 7
-4 0 -4 468.883 167.711 12
-4 0 4 659.122 231.206 12
-4 0 -4 567.472 270.618 13
-4 0 -5 1292.16 365.645 37
-4 0 5 1944.00 437.939 38
-4 0 -5 1493.26 427.061 26
-4 0 5 1807.28 411.924 7
-4 0 -5 1249.91 233.589 12
-4 0 5 1499.27 316.164 12
-4 0 -5 1347.95 347.400 13
-4 0 -6 150.844 220.103 37
-4 0 6 53.5608 250.611 38
-4 0 -6 463.629 295.456 26
-4 0 -6 298.649 134.520 12
-4 0 6 190.300 194.122 12
-4 0 -6 462.732 275.977 13
-4 0 6 199.171 217.966 7
-4 0 -7 64177.2 2978.15 37
-4 0 -7 64186.5 2482.75 12
-4 0 7 68624.3 2823.06 12
-4 0 -7 65430.0 2960.37 13
-4 0 -7 69055.8 3146.21 26
-4 0 7 67244.6 2965.35 7
-4 0 8 7535.60 753.294 7
-4 0 -8 6698.93 758.956 37
-4 0 8 6618.01 662.200 12
-4 0 -8 7168.50 778.413 13
-4 0 -9 22846.3 1514.71 37
-4 0 9 25980.8 1545.76 38
-4 0 9 23232.2 1371.81 12
-4 0 -9 26328.8 1604.74 13
-4 0 -10 46671.0 2295.52 37
-4 0 10 48177.9 2218.62 38
-4 0 10 46681.1 2099.34 12
-4 0 -10 49823.4 2406.94 13
-4 0 -11 87667.9 3595.26 37
-4 0 11 92909.3 3480.34 38
-4 0 11 95759.9 3424.38 7
-4 0 11 88754.0 3363.99 12
-4 0 -11 83461.4 3660.65 13
-4 0 -12 7560.59 816.588 37
-4 0 12 7806.02 723.066 38
4 0 -12 5480.40 510.560 24
-4 0 12 8638.55 718.461 7
-4 0 12 6645.37 667.662 12
-4 0 -12 7290.56 810.097 13
-4 0 13 1974.21 373.043 38
4 0 -13 1235.41 235.662 24
-4 0 13 1885.40 350.820 7
-4 0 13 2128.98 396.233 12
-4 0 -13 1677.03 396.048 13
-4 0 14 24527.5 1319.50 38
4 0 -14 18800.6 1055.05 24
-4 0 14 27781.5 1334.48 7
-4 0 14 23586.0 1388.31 12
-4 0 -14 22398.1 1353.54 13
-4 0 15 1757.19 335.630 38
-4 0 -15 1669.79 337.778 13
4 0 -15 1463.91 232.014 24
-4 0 16 816.977 229.582 38
-4 0 -16 578.573 213.384 13
4 0 -16 505.371 150.151 24
-4 0 -17 21083.6 1145.17 13
-4 0 -18 28851.3 1348.20 13
-4 0 -20 261.114 128.255 13
-4 1 22 6861.41 427.896 12
-4 1 21 16718.5 842.325 12
-4 -1 -21 16669.0 892.900 37
-4 1 20 1037.63 215.174 12
-4 -1 -20 1271.85 262.989 37
-4 1 19 33081.3 1542.28 12
-4 -1 -19 30528.6 1574.30 37
-4 1 18 1955.59 387.923 12
-4 -1 -18 1291.01 344.779 37
-4 1 17 18548.4 1023.78 7
-4 -1 -17 16478.1 1340.97 37
-4 1 16 43996.1 1626.54 7
-4 1 16 34780.7 2144.01 12
-4 1 15 6824.44 617.370 7
-4 1 15 7102.94 831.496 12
-4 -1 -15 7994.45 1313.22 37
4 1 -15 5838.75 474.709 35
-4 1 14 116858. 4087.19 7
-4 1 14 114349. 4331.57 12
-4 -1 -13 38987.0 2225.82 37
-4 -1 -13 40287.8 2249.80 26
-4 1 13 35527.8 1757.27 7
-4 1 13 37964.4 1894.94 12
-4 1 12 14063.8 1030.80 7
-4 1 12 13573.0 1042.67 12
-4 -1 -12 13290.0 1197.14 37
-4 1 11 41367.9 2134.84 7
-4 1 11 45512.0 2189.49 12
-4 -1 -11 46233.2 2421.37 37
-4 1 10 7347.27 749.691 7
-4 1 10 7320.14 727.812 12
-4 -1 -10 6741.50 820.295 37
-4 -1 -9 22231.5 1517.82 37
-4 -1 -9 19428.2 1617.46 26
-4 1 9 20210.2 1377.06 7
-4 1 9 21970.7 1355.17 12
-4 -1 -8 512.681 333.399 37
-4 -1 -8 354.995 288.007 26
-4 1 8 467.553 265.245 7
-4 1 8 731.805 285.165 12
-4 -1 -7 25595.6 1633.32 37
-4 -1 -7 25692.4 1792.87 26
-4 1 7 22466.4 1536.61 7
-4 1 7 23412.5 1431.54 12
-4 -1 -6 14709.2 1208.18 37
-4 1 6 17129.1 1144.09 12
-4 -1 -6 15180.7 1334.07 26
-4 -1 -5 10057.6 990.124 37
-4 -1 -5 12428.8 1188.72 26
-4 1 5 11744.5 924.016 12
-4 -1 -4 13230.5 1134.82 37
-4 1 4 13918.8 1016.21 12
-4 -1 -4 15057.9 1299.88 26
-4 1 4 14594.8 1255.17 7
-4 -1 -3 5181.73 695.303 37
-4 -1 -3 3728.27 651.912 26
-4 1 3 4512.69 554.119 12
-4 1 3 6062.64 817.600 7
-4 -1 -2 31377.3 1884.82 37
-4 1 2 34240.2 1751.37 12
-4 -1 -2 37168.5 2139.46 26
-4 1 2 34688.2 2192.88 7
-4 -1 -1 3554.24 564.224 37
-4 -1 -1 3159.51 621.832 26
-4 1 1 3693.39 481.026 12
-4 1 1 3103.09 421.249 13
-4 1 1 2496.63 580.483 7
-4 -1 0 38531.9 2129.75 26
-4 1 0 36121.7 1748.62 12
-4 1 0 30867.1 1669.52 13
-4 -1 0 34903.5 1922.05 37
-4 -1 1 3070.67 604.069 26
-4 1 -1 3047.10 436.893 12
-4 -1 1 2563.23 478.241 37
-4 -1 1 2961.22 615.552 38
-4 -1 2 35369.1 2075.75 26
-4 1 -2 36178.3 1751.84 12
-4 -1 2 39825.7 2461.98 38
-4 -1 3 2140.97 510.657 26
-4 1 -3 3213.26 415.158 12
-4 1 -3 3741.19 509.913 13
-4 -1 3 3107.94 680.435 38
-4 -1 4 16732.6 1283.41 26
-4 1 -4 17318.5 1022.62 12
-4 1 -4 16882.5 1159.29 13
-4 -1 5 14114.8 1131.86 26
-4 1 -5 14296.9 887.083 12
-4 1 -5 12954.2 1026.06 13
-4 1 -6 11666.2 784.560 12
-4 1 -6 11971.0 979.463 13
-4 -1 7 22791.7 1550.75 38
-4 1 -7 22749.1 1387.65 13
-4 1 -7 20478.1 1064.47 12
4 -1 -8 427.732 177.502 34
-4 -1 8 405.924 279.986 38
-4 1 -8 563.828 165.545 12
-4 1 -8 625.907 281.899 13
-4 -1 9 27466.9 1693.61 38
-4 1 -9 27254.6 1634.73 13
-4 1 -9 24784.0 1202.84 12
-4 -1 10 5761.31 711.041 38
-4 1 -10 6173.20 766.860 13
-4 -1 11 47506.7 2408.06 38
-4 1 -11 54016.5 2753.37 13
-4 -1 12 19368.6 1316.26 38
-4 1 -12 22304.0 1764.41 13
-4 -1 13 36581.9 1763.99 38
-4 1 -13 23053.2 1801.93 13
-4 -1 14 121416. 4242.64 38
-4 1 -14 92745.1 4270.41 13
-4 -1 15 7933.18 710.776 38
-4 1 -15 6668.44 710.193 13
-4 -1 16 42188.1 1878.47 38
-4 1 -16 38929.0 1908.02 13
-4 -1 17 16584.6 964.589 38
-4 1 -17 15791.6 992.053 13
-4 -1 18 2986.45 352.226 38
-4 1 -18 2410.85 349.185 13
-4 -1 19 30350.0 1269.50 38
-4 1 -19 24303.2 1243.35 13
-4 1 -20 193.744 124.219 13
-4 1 -21 17714.5 831.873 13
-4 -2 -20 31858.4 1309.18 37
-4 2 20 31651.8 1230.10 12
-4 -2 -19 32632.5 1459.61 37
-4 2 19 34490.5 1373.34 12
-4 -2 -18 2866.04 372.827 37
-4 2 18 2912.96 320.643 12
-4 -2 -17 19271.2 1174.31 37
-4 2 17 22620.6 1119.60 12
-4 2 16 22899.3 1212.83 12
-4 -2 -16 23562.7 1300.25 26
-4 -2 -15 2624.26 490.234 37
-4 -2 -15 3480.25 527.003 26
-4 2 15 4241.14 520.067 12
-4 2 15 3936.12 426.949 7
-4 -2 -14 23285.4 1609.56 37
-4 -2 -14 25906.3 1644.51 26
-4 2 14 23696.6 1382.13 12
-4 2 14 23280.3 1269.23 7
-4 -2 -13 113.556 289.710 37
-4 -2 -13 337.892 395.316 26
-4 2 13 536.888 229.065 12
-4 2 13 728.714 233.496 7
-4 -2 -12 23473.2 1512.66 37
-4 -2 -12 21288.9 2486.38 26
-4 2 12 21009.5 1260.30 12
-4 2 12 20276.0 1245.41 7
-4 -2 -11 2117.63 457.013 37
-4 -2 -11 3367.56 892.910 26
-4 2 11 2402.94 408.876 12
-4 2 11 1860.00 380.487 7
-4 -2 -10 1410.22 379.511 37
-4 -2 -10 1240.42 522.450 26
-4 2 10 1210.73 323.883 12
-4 2 10 1636.27 353.322 7
-4 -2 -9 113853. 4560.43 37
-4 2 9 116184. 4331.74 12
-4 2 9 105959. 4442.33 7
-4 -2 -8 37342.5 1992.19 37
-4 -2 -8 39274.9 2256.46 26
-4 2 8 37318.2 1808.18 12
-4 2 8 32523.2 1913.17 7
-4 -2 -7 19517.1 1328.74 37
-4 -2 -7 19311.6 1478.73 26
-4 2 7 19125.3 1170.66 12
-4 2 7 17882.1 1321.00 7
-4 -2 -6 19703.6 1348.10 37
-4 -2 -6 21992.3 1571.08 26
-4 2 6 23058.2 1279.92 12
-4 2 6 20415.9 1450.47 7
-4 -2 -5 12549.0 1016.14 37
-4 -2 -5 10898.7 1084.12 26
-4 2 5 12359.6 879.011 12
-4 2 5 11823.0 1073.64 7
-4 2 4 4839.87 519.482 12
-4 -2 -4 4356.27 688.223 26
-4 -2 -4 3775.07 557.214 37
4 2 -3 14118.2 781.594 46
-4 -2 -3 14285.1 1082.14 37
-4 -2 -3 13955.3 1224.46 26
-4 2 3 14898.6 973.208 12
-4 2 2 15656.1 1378.87 7
4 2 -2 14835.4 802.826 46
-4 -2 -2 17673.5 1322.86 26
-4 -2 -2 16694.8 1165.27 37
-4 2 2 16757.8 1038.54 12
-4 -2 -1 14589.1 1075.86 37
-4 2 1 13588.5 919.233 12
-4 2 1 13867.7 1372.36 7
-4 -2 -1 12945.3 1135.08 26
-4 2 0 42846.4 1972.33 12
-4 -2 0 45290.9 2352.68 26
-4 2 0 47434.3 2986.66 7
-4 -2 1 13437.3 1126.75 26
-4 -2 1 15989.6 1785.89 38
-4 2 -1 14666.2 922.255 12
4 -2 -2 16750.5 954.625 22
-4 -2 2 18690.5 1313.34 26
-4 2 -2 18671.7 1045.35 12
-4 -2 3 13649.5 1097.55 26
-4 2 -3 14223.2 879.184 12
-4 -2 4 5042.16 643.633 26
-4 -2 4 5086.65 778.657 38
-4 2 -4 4909.84 471.193 12
-4 -2 5 14271.0 1065.16 26
-4 -2 5 14920.4 1291.70 38
-4 2 -5 13915.1 834.644 12
-4 2 -5 14337.4 947.972 13
-4 -2 6 23133.0 1376.37 26
-4 -2 6 23310.1 1620.38 38
-4 2 -6 22111.3 1107.96 12
-4 2 -6 22104.9 1270.18 13
-4 -2 7 18085.3 1371.55 38
-4 2 -7 17034.5 909.520 12
-4 -2 8 35894.8 2017.81 38
-4 2 -8 34171.2 1473.67 12
-4 -2 9 105427. 4175.51 38
-4 2 -9 105720. 3947.76 13
4 -2 -10 1468.42 294.366 34
-4 -2 10 2572.09 481.413 38
-4 2 -10 1969.22 410.507 13
4 -2 -11 3763.41 434.194 34
-4 -2 11 3791.88 539.731 38
-4 2 -11 5011.76 674.566 13
-4 -2 12 22907.6 1432.67 38
-4 2 -12 32152.3 1987.82 13
-4 -2 13 1090.49 299.590 38
-4 2 -13 643.831 403.411 13
-4 -2 14 26077.9 1364.48 38
-4 2 -14 21957.4 1492.23 13
-4 -2 15 3784.36 438.540 38
-4 2 -15 3552.69 483.791 13
-4 -2 16 17317.1 964.266 38
-4 2 -16 16745.7 1014.59 13
-4 -2 17 20842.4 1014.50 38
-4 2 -17 18848.0 1038.28 13
-4 -2 18 3437.67 328.648 38
-4 2 -18 4088.67 379.637 13
-4 -2 19 37539.2 1404.82 38
-4 2 -19 35641.1 1469.39 13
-4 2 -20 31361.6 1229.91 13
-4 -3 -15 5927.12 460.456 26
-4 -3 -14 6345.94 439.846 37
-4 -3 -14 7125.27 558.447 26
-4 -3 -13 13580.4 768.195 37
-4 -3 -13 15733.9 957.241 26
-4 -3 -12 4058.04 395.161 37
-4 -3 -12 3961.71 504.247 26
-4 -3 -11 939.371 224.213 37
-4 -3 -11 990.587 327.867 26
-4 3 11 1117.60 188.896 12
-4 -3 -10 202.773 147.864 37
-4 -3 -10 101.484 237.455 26
-4 3 10 386.007 142.960 12
-4 -3 -9 4286.07 465.967 37
-4 -3 -9 4750.47 619.655 26
-4 3 9 4387.76 389.969 12
-4 -3 -8 17950.6 1064.90 37
-4 3 8 19226.2 953.761 12
-4 -3 -8 19435.8 1289.20 26
-4 3 7 56957.7 2597.97 7
-4 3 7 62071.8 2335.06 12
-4 -3 -7 65474.9 2781.28 26
-4 3 6 5519.70 442.041 12
-4 3 6 4435.30 552.984 7
-4 -3 -6 4217.35 558.746 26
-4 3 5 26661.6 1203.51 12
-4 3 5 26084.0 1510.81 7
-4 -3 -5 25913.6 1504.98 26
-4 3 4 37714.9 1542.83 12
-4 3 4 34188.4 1871.19 7
-4 -3 -4 36812.7 1859.72 26
-4 3 3 10563.3 640.636 12
-4 3 3 10745.2 923.225 7
-4 -3 -3 9809.29 840.994 26
-4 3 2 17947.6 898.153 12
-4 -3 -2 17165.2 1121.88 26
-4 3 1 14124.1 754.940 12
-4 -3 -1 13628.0 961.401 26
-4 3 0 40422.7 1642.46 12
-4 -3 0 39765.1 1910.70 26
-4 3 -1 14982.1 763.360 12
-4 -3 1 13742.1 932.736 26
-4 3 -2 18640.0 882.112 12
-4 -3 2 18025.1 1072.60 26
-4 -3 3 10035.4 1019.07 38
-4 3 -3 8889.16 539.984 12
-4 -3 4 45825.8 2361.91 38
-4 -3 5 22678.6 1451.40 38
-4 -3 6 4351.96 585.650 38
-4 -3 7 62241.4 2744.57 38
-4 -3 8 20223.1 1239.69 38
-4 -3 9 7327.01 668.933 38
-4 -3 10 1191.68 271.461 38
-4 -3 11 1255.49 269.729 38
-4 -3 12 4652.97 449.738 38
-4 -3 13 17329.7 905.991 38
-4 -3 14 8792.09 543.115 38
0 0 0 0.00 0.00 0
TITL a_1961_1 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 3.773790 5.634830 32.978318 90.0000 90.0000 90.0000
ZERR 4.00 0.000038 0.000042 0.000241 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N Cl
UNIT 28.00 28.00 12.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 8498
_shelx_res_file
;
TITL a_1961_1_a.res in P2(1)2(1)2(1)
CELL 1.54184 3.7738 5.6349 32.9787 90 90 90
ZERR 4 0 0 0.0002 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Cl N
UNIT 24 28 4 16
L.S. 14
ACTA
BOND $H
FMAP -2
PLAN 5
HTAB N4 N42
HTAB N4 N2_$1
HTAB N2 N3_$2
HTAB N2 N2_$1
HTAB N4 N42
HTAB N4 N2_$1
HTAB N2 N3_$2
HTAB N2 N2_$1
HTAB N4 N42
HTAB N4 N2_$1
HTAB N2 N3_$2
EQIV $2 x+1/2, -y+1/2, -z+1
HTAB N2 N2_$1
EQIV $1 x+1/2, -y+3/2, -z+1
HTAB
CONF
HTAB N2 N2_$1
HTAB N2 N3_$2
HTAB N4 N2_$1
HTAB N4 N42
HTAB N2 N2_$1
HTAB N2 N3_$2
HTAB N4 N2_$1
HTAB N4 N42
WGHT 0.033600 0.175400
FVAR 12.36927
C4 1 0.485801 0.568339 0.568714 11.00000 0.00857 0.01025 =
0.01147 0.00069 -0.00066 0.00145
C41 1 0.345713 0.487055 0.608680 11.00000 0.00862 0.01179 =
0.01117 0.00069 -0.00106 0.00294
C43 1 0.305580 0.560482 0.676369 11.00000 0.01198 0.01579 =
0.00998 -0.00118 -0.00180 0.00347
C44 1 0.129449 0.350068 0.684456 11.00000 0.01352 0.01870 =
0.01118 0.00397 0.00158 0.00453
AFIX 43
H44 2 0.060601 0.309207 0.710618 11.00000 -1.20000
AFIX 0
C45 1 0.060687 0.203035 0.651553 11.00000 0.01178 0.01272 =
0.01845 0.00345 0.00106 0.00060
AFIX 43
H45 2 -0.057942 0.060038 0.655293 11.00000 -1.20000
AFIX 0
C46 1 0.170022 0.270793 0.613096 11.00000 0.01179 0.01201 =
0.01376 -0.00014 -0.00113 0.00153
AFIX 43
H46 2 0.127148 0.174208 0.590761 11.00000 -1.20000
AFIX 0
CL43 3 0.408071 0.751951 0.716494 11.00000 0.02054 0.02074 =
0.00985 -0.00299 -0.00066 0.00060
N2 4 0.595890 0.509261 0.501198 11.00000 0.01566 0.01210 =
0.00855 -0.00078 0.00134 0.00034
H2A 2 0.789323 0.591183 0.504469 11.00000 -1.20000
H2B 2 0.650561 0.382198 0.487607 11.00000 -1.20000
N3 4 0.458209 0.423211 0.538530 11.00000 0.01270 0.01127 =
0.00917 0.00093 0.00025 0.00045
N4 4 0.634018 0.788748 0.568243 11.00000 0.01895 0.01292 =
0.00916 -0.00135 0.00166 -0.00378
H4A 2 0.764154 0.840534 0.547762 11.00000 -1.20000
H4B 2 0.657856 0.847016 0.591478 11.00000 -1.20000
N42 4 0.411550 0.632816 0.640063 11.00000 0.01091 0.01279 =
0.01158 -0.00032 0.00032 0.00172
HKLF 4
REM a_1961_1_a.res in P2(1)2(1)2(1)
REM R1 = 0.0206 for 1460 Fo > 4sig(Fo) and 0.0208 for all 1471 data
REM 112 parameters refined using 0 restraints
END
WGHT 0.0336 0.1754
REM Instructions for potential hydrogen bonds
HTAB N2 N2_$1
HTAB N2 N3_$2
HTAB N4 N2_$1
HTAB N4 N42
REM Highest difference peak 0.201, deepest hole -0.217, 1-sigma level 0.043
Q1 1 0.4502 0.6846 0.7197 11.00000 0.05 -0.20
Q2 1 0.4095 0.5290 0.5872 11.00000 0.05 0.20
Q3 1 0.4101 0.7711 0.6985 11.00000 0.05 -0.20
Q4 1 0.5422 0.7397 0.5950 11.00000 0.05 -0.19
Q5 1 0.4137 0.6802 0.6703 11.00000 0.05 -0.18
;
_shelx_res_checksum 55275
_shelxl_version_number 2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
C C4 0.4858(4) 0.5683(3) 0.56871(5) 0.0101(3) Uani d 1 . .
C C41 0.3457(4) 0.4871(3) 0.60868(5) 0.0105(3) Uani d 1 . .
C C43 0.3056(4) 0.5605(3) 0.67637(5) 0.0126(3) Uani d 1 . .
C C44 0.1294(5) 0.3501(3) 0.68446(5) 0.0145(3) Uani d 1 . .
H H44 0.0606 0.3092 0.7106 0.017 Uiso calc 1 . .
C C45 0.0607(5) 0.2030(3) 0.65155(5) 0.0143(3) Uani d 1 . .
H H45 -0.0579 0.0600 0.6553 0.017 Uiso calc 1 . .
C C46 0.1700(4) 0.2708(3) 0.61310(5) 0.0125(3) Uani d 1 . .
H H46 0.1271 0.1742 0.5908 0.015 Uiso calc 1 . .
Cl Cl43 0.40807(11) 0.75195(7) 0.71649(2) 0.01704(13) Uani d 1 . .
N N2 0.5959(4) 0.5093(3) 0.50120(4) 0.0121(3) Uani d 1 . .
H H2A 0.789(6) 0.591(4) 0.5045(6) 0.015 Uiso d 1 . .
H H2B 0.651(6) 0.382(4) 0.4876(6) 0.015 Uiso d 1 . .
N N3 0.4582(4) 0.4232(2) 0.53853(4) 0.0110(3) Uani d 1 . .
N N4 0.6340(4) 0.7887(2) 0.56824(4) 0.0137(3) Uani d 1 . .
H H4A 0.764(6) 0.841(4) 0.5478(6) 0.016 Uiso d 1 . .
H H4B 0.658(6) 0.847(4) 0.5915(7) 0.016 Uiso d 1 . .
N N42 0.4116(4) 0.6328(2) 0.64006(4) 0.0118(3) 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
C4 0.0086(7) 0.0102(7) 0.0115(7) 0.0015(6) -0.0007(6) 0.0007(6)
C41 0.0086(8) 0.0118(7) 0.0112(7) 0.0029(6) -0.0011(6) 0.0007(6)
C43 0.0120(8) 0.0158(8) 0.0100(7) 0.0035(7) -0.0018(6) -0.0012(6)
C44 0.0135(8) 0.0187(8) 0.0112(7) 0.0045(7) 0.0016(7) 0.0040(6)
C45 0.0118(8) 0.0127(7) 0.0184(7) 0.0006(6) 0.0011(6) 0.0035(6)
C46 0.0118(8) 0.0120(7) 0.0138(7) 0.0015(7) -0.0011(6) -0.0001(6)
Cl43 0.0205(2) 0.0207(2) 0.00985(19) 0.0006(2) -0.00066(13) -0.00299(15)
N2 0.0157(7) 0.0121(7) 0.0085(6) 0.0003(6) 0.0013(6) -0.0008(5)
N3 0.0127(7) 0.0113(6) 0.0092(6) 0.0004(6) 0.0002(5) 0.0009(5)
N4 0.0190(7) 0.0129(7) 0.0092(6) -0.0038(6) 0.0017(6) -0.0013(5)
N42 0.0109(7) 0.0128(6) 0.0116(6) 0.0017(6) 0.0003(5) -0.0003(5)
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'
Cl Cl 0.3639 0.7018 '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'
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
N3 C4 N4 . . 126.95(15)
N3 C4 C41 . . 117.23(14)
N4 C4 C41 . . 115.81(14)
N42 C41 C46 . . 122.76(15)
N42 C41 C4 . . 115.28(14)
C46 C41 C4 . . 121.92(14)
N42 C43 C44 . . 125.55(15)
N42 C43 Cl43 . . 115.23(13)
C44 C43 Cl43 . . 119.21(12)
C43 C44 C45 . . 116.72(15)
C43 C44 H44 . . 121.6
C45 C44 H44 . . 121.6
C46 C45 C44 . . 119.62(16)
C46 C45 H45 . . 120.2
C44 C45 H45 . . 120.2
C45 C46 C41 . . 118.51(16)
C45 C46 H46 . . 120.7
C41 C46 H46 . . 120.7
N3 N2 H2A . . 112.3(13)
N3 N2 H2B . . 104.6(14)
H2A N2 H2B . . 108(2)
C4 N3 N2 . . 114.95(13)
C4 N4 H4A . . 122.5(14)
C4 N4 H4B . . 113.0(15)
H4A N4 H4B . . 121(2)
C43 N42 C41 . . 116.83(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C4 N3 . 1.292(2)
C4 N4 . 1.362(2)
C4 C41 . 1.492(2)
C41 N42 . 1.344(2)
C41 C46 . 1.395(2)
C43 N42 . 1.327(2)
C43 C44 . 1.385(3)
C43 Cl43 . 1.7506(16)
C44 C45 . 1.390(2)
C44 H44 . 0.9300
C45 C46 . 1.387(2)
C45 H45 . 0.9300
C46 H46 . 0.9300
N2 N3 . 1.4216(17)
N2 H2A . 0.87(2)
N2 H2B . 0.87(2)
N4 H4A . 0.88(2)
N4 H4B . 0.84(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N4 H4B N42 . 0.84(2) 2.21(2) 2.662(2) 113.8(19)
N4 H4A N2 4_566 0.88(2) 2.21(2) 3.095(2) 176.4(19)
N2 H2B N3 4_556 0.87(2) 2.25(2) 3.0862(19) 162(2)
N2 H2A N2 4_566 0.87(2) 2.54(2) 3.306(2) 147.5(19)
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
N3 C4 C41 N42 . . . . 173.55(15)
N4 C4 C41 N42 . . . . -5.7(2)
N3 C4 C41 C46 . . . . -4.3(2)
N4 C4 C41 C46 . . . . 176.46(15)
N42 C43 C44 C45 . . . . 0.3(3)
Cl43 C43 C44 C45 . . . . -178.87(13)
C43 C44 C45 C46 . . . . 0.3(2)
C44 C45 C46 C41 . . . . -0.3(2)
N42 C41 C46 C45 . . . . -0.4(3)
C4 C41 C46 C45 . . . . 177.31(15)
N4 C4 N3 N2 . . . . -0.8(2)
C41 C4 N3 N2 . . . . -179.96(14)
C44 C43 N42 C41 . . . . -1.0(3)
Cl43 C43 N42 C41 . . . . 178.26(12)
C46 C41 N42 C43 . . . . 1.0(2)
C4 C41 N42 C43 . . . . -176.86(14)