#------------------------------------------------------------------------------
#$Date: 2019-02-15 05:36:39 +0200 (Fri, 15 Feb 2019) $
#$Revision: 213660 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021516.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_2021516
loop_
_publ_author_name
'Oliveira, Ana P. A.'
'Ferreira, Isabella P.'
'Despaigne, Angel A. Recio'
'da Silva, Jeferson G.'
'Vieira, Ana Carolina S.'
'Santos, Mariana S.'
'Alexandre-Moreira, Magna S.'
'Diniz, Renata'
'Beraldo, Heloisa'
_publ_section_title
;
Structural studies and antileishmanial activity of 2-acetylpyridine and
2-benzoylpyridine nitroimidazole-derived hydrazones
;
_journal_coeditor_code KY3160
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619001529
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C12 H12 N6 O3'
_chemical_formula_moiety 'C12 H12 N6 O3'
_chemical_formula_sum 'C12 H12 N6 O3'
_chemical_formula_weight 288.28
_chemical_melting_point 786.4(8)
_chemical_name_common
;
2-Acetylpyridine-2-nitroimidazole hydrazone
;
_chemical_name_systematic
;
2-(2-Nitro-1H-imidazol-1-yl)-N'-[1-(pyridin-2-\
yl)ethylidene]acetohydrazide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_symmetry_space_group_name_Hall '-I 2ya'
_symmetry_space_group_name_H-M 'I 1 2/a 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2017/1
_cell_angle_alpha 90
_cell_angle_beta 106.612(8)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 12.1890(10)
_cell_length_b 18.7185(11)
_cell_length_c 12.4701(9)
_cell_measurement_reflns_used 2902
_cell_measurement_temperature 270(2)
_cell_measurement_theta_max 28.1380
_cell_measurement_theta_min 2.2160
_cell_volume 2726.4(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008) and
ORTEP-3 For Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2017 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 270(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Xcalibur Gemini ultra diffractometer with an Atlas detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0360
_diffrn_reflns_av_unetI/netI 0.0326
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 9783
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.373
_diffrn_reflns_theta_min 2.022
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.106
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80689
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.405
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1200
_exptl_crystal_size_max 0.410
_exptl_crystal_size_mid 0.078
_exptl_crystal_size_min 0.024
_refine_diff_density_max 0.186
_refine_diff_density_min -0.199
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 203
_refine_ls_number_reflns 2786
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.052
_refine_ls_R_factor_all 0.0709
_refine_ls_R_factor_gt 0.0442
_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^)+(0.0541P)^2^+0.6451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1040
_refine_ls_wR_factor_ref 0.1192
_reflns_number_gt 1955
_reflns_number_total 2786
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ky3160sup1.cif
_cod_data_source_block 2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' value '512.55-514.05 /% C' was changed to
'786.4(8)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.
Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas
;
_cod_database_code 2021516
_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 0.958
_shelx_estimated_absorpt_t_max 0.997
_shelx_hkl_file
;
0 0 -2 222.233 24.2069 2
0 0 -2 301.297 35.5785 3
0 0 -2 184.037 18.2683 1
0 0 2 192.257 17.3051 1
0 0 2 213.597 23.5876 2
0 0 -4 46903.7 446.855 2
0 0 4 45706.7 446.136 2
0 0 4 47336.5 342.481 1
0 0 -4 45941.7 361.856 1
0 0 -4 46565.5 506.346 3
0 0 -6 73.2730 38.6027 3
0 0 -6 23.7310 17.9675 2
0 0 6 55.9321 18.7064 1
0 0 6 28.2065 26.7122 2
0 0 -8 184.123 49.3416 3
0 0 8 132.008 41.2373 2
0 0 8 143.901 38.3835 3
0 0 8 160.839 29.2778 1
0 0 10 11746.3 258.543 1
0 0 10 11864.5 377.834 2
0 0 10 11529.4 402.973 3
0 0 -10 11653.2 351.220 2
0 0 -12 239.596 60.8377 2
0 0 12 203.302 61.7893 3
0 0 -14-60.8629 49.3732 2
0 -1 -1 16116.9 133.193 1
0 1 1 15677.4 153.388 2
0 1 -1 15650.1 150.796 3
0 -1 -1 16663.3 147.459 3
0 1 3 1540.76 59.5126 1
0 -1 -3 1455.69 59.2353 1
0 -1 -3 1743.90 86.5223 3
0 -1 3 1388.90 55.9463 1
0 1 -3 1460.07 68.0230 2
0 -1 3 1441.41 67.6962 2
0 1 -3 1463.82 79.2323 3
0 -1 -3 1379.85 70.1049 2
0 1 3 1408.91 70.5583 2
0 -1 -5-12.7562 16.7085 2
0 -1 -5-42.3665 30.7540 3
0 1 5 21.9100 22.9088 2
0 1 5 33.6761 16.9283 1
0 1 -5-15.4045 23.6528 2
0 -1 -5 9.46693 15.8041 1
0 -1 5-6.97167 11.9250 1
0 -1 5 6.56611 20.5964 2
0 1 -5-8.98032 25.5904 3
0 -1 7 333.269 39.3097 1
0 -1 -7 39.1566 28.7032 2
0 -1 -7 302.152 43.1604 1
0 1 -7 119.102 35.4233 2
0 1 7 402.163 60.7388 2
0 1 7 303.729 37.9292 1
0 1 -7 404.459 70.1824 3
0 -1 7 335.690 54.4786 2
0 -1 -7 352.772 64.7813 3
0 -1 9 510.372 76.0855 2
0 -1 9 503.788 79.6158 3
0 1 9 547.020 56.4139 1
0 -1 9 542.283 53.5091 1
0 1 9 584.203 83.7197 2
0 1 9 531.873 84.0538 3
0 -1 11 1190.72 140.656 3
0 -1 11 881.607 71.1067 1
0 1 -11 1367.38 126.145 2
0 -1 -11 1215.61 125.034 2
0 1 11 1239.50 143.351 3
0 -1 11 1313.07 134.414 2
0 -1 -13-46.3100 37.9536 2
0 1 -13 66.1897 44.3109 2
0 -1 -15-1.10874 30.6450 2
0 1 -15 4.36805 27.6919 2
0 -2 0 1782.80 50.9087 1
0 2 2 60790.1 429.818 2
0 2 -2 57832.2 401.850 3
0 2 2 67053.1 377.550 1
0 -2 -2 66095.1 420.389 3
0 -2 -2 65525.1 375.735 1
0 -2 -4 38.6843 22.8509 2
0 2 4 12.0991 14.2626 1
0 -2 -4-0.22973 15.0211 1
0 2 -4 23.5241 17.8035 2
0 2 -4 18.8066 19.3271 3
0 -2 4-7.60949 17.6736 2
0 2 4 3.33200 17.8225 2
0 -2 -4 47.0018 26.6593 3
0 2 -6 1718.41 124.909 3
0 -2 -6 1590.29 105.483 2
0 2 6 1799.04 88.3148 1
0 -2 -6 1991.65 132.899 3
0 2 6 1677.28 112.687 2
0 -2 6 1662.97 104.712 2
0 2 -6 1683.16 100.538 2
0 -2 6 1663.21 82.0146 1
0 -2 -6 1639.27 89.6620 1
0 2 8 1038.80 108.603 3
0 2 8 1224.69 111.202 2
0 2 8 1257.07 82.0352 1
0 2 -8 1186.02 120.968 3
0 -2 8 1188.41 102.078 2
0 -2 -8 1289.42 124.535 3
0 -2 8 1143.24 112.812 3
0 -2 -8 1125.02 86.3379 1
0 -2 8 1232.41 78.9493 1
0 2 -8 614.262 72.7709 2
0 -2 10-3.13805 21.7069 2
0 -2 -10 44.7914 34.2339 2
0 2 10 79.3179 42.9728 2
0 -2 10 23.3895 39.2827 3
0 2 10-21.1422 16.7069 1
0 2 10-40.8325 53.3538 3
0 -2 10-4.67888 13.1195 1
0 -2 -12 60.9498 40.6765 2
0 -2 12 125.737 56.4669 3
0 2 -12 104.601 42.3107 2
0 2 12 37.7702 19.2590 1
0 -2 -14-14.6195 40.7255 2
0 2 -14 26.3887 30.7625 2
0 3 1 12095.2 184.071 2
0 -3 -1 11580.8 167.674 1
0 3 -1 12007.2 143.068 3
0 -3 1 12061.9 142.067 3
0 -3 -3 8924.47 204.137 2
0 -3 -3 10217.2 203.248 3
0 -3 -3 9640.08 178.877 1
0 3 -3 9739.82 185.734 2
0 3 3 9881.99 179.192 1
0 3 3 8709.73 202.430 2
0 3 -3 8903.18 194.805 3
0 -3 3 9104.59 195.651 3
0 3 5 6989.08 216.818 2
0 3 -5 6920.16 221.411 3
0 -3 5 6446.24 212.831 3
0 -3 -5 7687.13 231.574 3
0 -3 -5 6887.06 209.544 2
0 3 -5 7035.24 188.799 2
0 3 5 6916.65 216.991 3
0 -3 -5 6862.28 176.535 1
0 3 5 7305.45 175.906 1
0 -3 7 922.007 68.3136 1
0 3 7 988.106 73.6564 1
0 -3 -7 939.813 76.2238 1
0 -3 -7 866.157 97.3574 3
0 3 -7 725.606 70.4051 2
0 3 7 926.802 92.3496 2
0 3 7 835.400 90.6397 3
0 3 -7 881.923 96.5752 3
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0 3 9 2183.83 160.727 2
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0 -3 9 2087.11 109.771 1
0 -3 11 48.4063 19.5189 1
0 -3 -11 90.5616 39.9061 2
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0 -3 -13 81.6954 41.9088 2
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0 -4 0 157280. 686.217 1
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0 4 8 115.729 28.5586 1
0 4 8 294.852 60.0946 2
0 -4 8 263.754 61.5070 3
0 -4 -8 239.137 44.1325 1
0 -4 8 223.031 38.1493 1
0 4 -8 136.502 38.5622 2
0 4 -8 288.697 62.2446 3
0 -4 -8 282.321 60.0861 3
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0 -4 10 2378.63 124.234 1
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0 4 -12 9.45628 22.3934 2
0 -4 12-32.9291 42.7004 3
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0 4 -14 89.4146 45.6219 2
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0 -5 1 2050.36 66.5517 3
0 5 1 2341.74 102.994 2
0 -5 -1 1936.46 89.0927 1
0 5 3 34848.9 457.158 2
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0 -5 -3 35060.6 402.247 1
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0 5 -5 8254.73 220.154 2
0 5 5 8473.33 216.388 1
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0 5 -5 7525.38 235.711 3
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0 -5 -7 2530.29 162.824 3
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0 5 -7 300.774 52.3748 2
0 -5 -7 2054.29 118.395 1
0 5 7 912.788 77.4485 1
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0 -5 -13 845.909 123.505 2
0 -5 -15 13.0709 37.1561 2
0 -6 0 74495.4 403.975 3
0 -6 0 72516.1 574.171 1
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0 6 2 3829.85 147.012 2
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0 -6 2 3750.18 112.766 3
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0 -6 4 1245.76 86.0435 3
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0 6 -6 12026.8 330.570 3
0 6 6 12231.8 337.407 2
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0 -6 8 443.429 76.8994 3
0 -6 -8 426.655 75.2858 3
0 6 8 480.494 77.0681 2
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0 -6 -8 503.507 81.0724 2
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0 -6 -16-10.5027 36.5491 2
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0 -7 -3 135.964 33.5966 1
0 7 -3 159.536 30.5578 3
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0 -7 -5 3780.27 165.820 3
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0 -7 -7 494.223 77.1967 2
0 7 -7 10.3179 18.4735 2
0 -7 7 550.801 79.8636 3
0 -7 -7 627.260 84.9373 3
0 7 -7 624.630 84.0400 3
0 -7 -7 519.871 69.5048 1
0 7 7 548.057 80.5642 2
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0 -7 -9 326.687 69.6609 2
0 -7 11 487.406 65.6067 1
0 7 -11 466.375 76.7321 2
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0 -7 -11 432.987 90.2322 2
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0 -8 0 3520.95 151.173 1
0 -8 0 3497.01 103.196 3
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0 8 -4 6164.99 194.953 3
0 8 4 6183.58 235.844 2
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0 -8 -4 6485.94 220.313 1
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0 -8 -8 472.496 77.3179 3
0 8 -8 433.744 78.6385 3
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0 -8 -14 160.255 76.3574 2
0 -9 1 2616.92 92.3886 3
0 9 1 2975.65 153.369 2
0 -9 -1 2505.67 133.657 1
0 -9 1 2690.71 136.221 1
0 -9 -3 134.871 27.7135 3
0 -9 3 126.665 26.2267 3
0 9 -3 112.142 29.4556 3
0 9 3 115.366 35.1469 2
0 -9 -3 84.0413 32.8214 1
0 9 5 83.2740 32.3005 2
0 9 -5 64.9163 28.5199 3
0 -9 -5 71.0653 33.6092 1
0 -9 5-2.78106 18.1560 3
0 -9 -5 22.9838 28.0134 2
0 -9 -5 78.7343 30.8200 3
0 9 -7 3640.73 200.724 3
0 -9 -7 3794.82 190.630 1
0 -9 -7 3734.78 221.416 2
0 9 7 3841.02 189.775 1
0 -9 -7 4116.15 211.131 3
0 -9 7 3535.59 191.031 3
0 -9 -9 361.801 82.0670 2
0 -9 9 307.687 64.1582 3
0 9 9 315.075 58.9900 1
0 -9 -9 248.580 55.2927 1
0 -9 11 971.176 128.194 3
0 -9 -11 1146.35 146.359 2
0 9 -11 1206.47 122.729 2
0 -9 -11 1028.35 116.809 1
0 9 -13 132.395 44.6390 2
0 -9 13 154.477 61.8160 3
0 -9 -13 82.8490 59.1519 2
0 -9 -15 203.604 79.4586 2
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0 -10 0 1637.69 75.1440 3
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0 -10 2 5506.21 207.024 1
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0 -10 2 5111.23 147.905 3
0 -10 -2 5025.88 208.612 1
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0 10 -4 3132.08 146.956 3
0 -10 4 3202.24 145.569 3
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14 -8 -8-0.18055 44.7350 2
14 8 -6 71.5381 60.6233 2
14 -8 -6 17.2435 47.6197 3
14 -8 -6-22.4161 30.9111 2
14 -8 -4 82.8557 67.3204 3
14 8 -4 19.6715 25.4595 2
14 -8 -2 53.5132 57.6225 3
14 8 -2 18.7434 35.4139 2
14 8 0 63.4968 58.9681 2
14 -9 -9-51.9326 37.8045 2
14 9 -7 134.449 77.3283 2
14 -9 -7 45.9318 32.5642 2
14 -9 -5 108.369 71.0651 3
14 9 -5 6.20914 40.8323 2
14 -9 -3 74.6250 62.2644 3
14 9 -3 64.5997 47.5703 2
14 9 -1 66.5904 39.2769 2
14 -10 -8 56.4230 55.1175 2
14 10 -6-41.5014 45.1108 2
14 -10 -6 122.081 65.8190 2
14 10 -4 19.9109 50.5839 2
14 10 -2 88.8226 68.6953 2
14 -11 -9 94.4786 65.9642 2
14 -11 -7 57.2197 38.4919 2
-14 -11 5 265.554 88.9814 1
14 11 -5 240.171 83.2632 2
14 11 -3-9.79302 38.1180 2
-14 -11 3 52.2819 64.3844 1
14 -12 -8 213.651 86.2301 2
-14 -12 6 4.24314 48.5914 1
14 12 -4-145.156 84.7342 2
-14 -12 4-60.7152 56.8084 1
-14 -13 5 166.368 77.8906 1
15 0 -9-165.788 76.1118 3
15 0 -9-12.1609 40.6595 2
15 0 -7 20.8773 64.8998 3
15 0 -7-50.2241 48.8966 2
15 0 -5 39.9202 75.5344 3
15 0 -5 35.4021 39.5648 2
15 0 -3 106.026 77.3107 3
15 0 -1-51.6447 59.9659 3
15 0 1-17.5469 52.0869 3
15 -1 -10 315.938 99.6413 2
15 1 -8 477.179 122.675 3
15 -1 -8 350.754 112.817 3
15 -1 -8 667.457 131.786 2
15 1 -8 583.444 119.943 2
15 1 -6 91.9026 53.1279 3
15 -1 -6 88.5665 64.8837 3
15 -1 -6 13.3289 38.7470 2
15 1 -6-30.4592 49.0885 2
15 1 -4 12.3408 66.6650 3
15 -1 -4 53.2392 67.4638 3
15 -1 -4-20.3346 43.2641 2
15 1 -4 152.964 68.8439 2
15 1 -2 9.12508 43.5583 3
15 -1 -2 90.5124 72.2785 3
15 -1 0-128.823 71.5598 3
15 1 0-7.53060 45.6841 3
15 2 -9 87.8930 49.6453 3
15 -2 -9 364.131 108.378 2
15 2 -9 369.090 112.959 2
15 2 -7 9.07405 51.3153 3
15 -2 -7 34.4786 52.5890 3
15 -2 -7 4.87802 35.7449 2
15 2 -7 8.36302 46.5508 2
15 2 -5 6.95343 44.2723 3
15 -2 -5-1.39458 56.6453 3
15 -2 -5-18.9517 36.8329 2
15 2 -5 126.689 67.0156 2
15 2 -3-49.2829 68.3532 3
15 -2 -3 63.1123 61.4684 3
15 2 -3 47.8085 47.7094 2
15 2 -1 61.6389 61.2081 3
15 -2 -1 6.17739 64.1812 3
15 2 1 129.239 91.7534 3
15 -3 -10 747.416 150.318 2
15 3 -8 1.56914 29.2304 3
15 -3 -8-6.15887 56.7618 3
15 3 -8 50.8364 45.5844 2
15 3 -6 18.4570 31.5476 3
15 -3 -6 47.8309 76.2681 3
15 -3 -6-57.4757 55.3471 2
15 3 -6-80.8770 67.3521 2
15 3 -4 506.014 129.283 3
15 -3 -4 361.513 123.274 3
15 3 -4 642.402 118.312 2
15 3 -2-111.738 62.8955 3
15 -3 -2 13.9536 49.7917 3
15 3 0 396.810 123.368 3
15 3 2-8.15530 60.8513 3
15 4 -9 47.4689 46.0685 3
15 -4 -9 63.9847 65.2167 2
15 4 -9-64.3862 75.4701 2
15 4 -7 9.20230 39.7873 3
15 -4 -7-39.2890 78.6365 3
15 -4 -7 119.418 77.7031 2
15 4 -7-94.6178 56.3225 2
15 4 -5 94.3153 38.4218 2
15 4 -5 101.651 44.0429 3
15 -4 -5 133.936 86.0106 3
15 -4 -5 74.6157 30.6838 2
15 4 -3 205.449 69.1736 2
15 -4 -3 122.747 86.9964 3
15 4 -1 152.947 73.5425 3
15 4 1 113.111 84.2672 3
15 5 -8 98.4123 75.4854 3
15 -5 -8-4.28703 42.0697 2
15 5 -8 43.0661 52.2107 2
15 5 -6-9.08176 25.9644 2
15 5 -6-48.4816 51.6924 3
15 -5 -6-10.7171 45.6857 3
15 -5 -6-134.610 72.8165 2
15 5 -4 189.096 49.1262 3
15 -5 -4 192.056 82.4700 3
15 5 -2 83.0328 56.7971 3
15 5 0 482.648 123.605 3
15 5 2 35.7729 56.7693 3
15 6 -9 140.048 78.7310 3
15 -6 -9-56.3395 67.2999 2
15 6 -7 112.681 77.6696 2
15 6 -7 15.9913 35.3393 3
15 -6 -7-52.4119 56.6726 2
15 6 -5 33.7970 43.0350 2
15 6 -5-2.14567 35.9329 3
15 6 -3 26.3914 45.1285 3
15 6 -3 70.3324 52.2499 2
15 6 -1 60.2161 56.5063 3
15 6 1-301.583 94.2819 3
15 -7 -8-7.95495 47.5543 2
15 7 -6-10.7760 39.5330 2
15 7 -4 67.1528 46.9485 2
15 7 -2-74.4717 54.6762 2
15 -8 -9 76.9379 67.8102 2
15 -8 -7 47.5864 38.5387 2
15 8 -5-26.8970 34.3017 2
15 8 -3 43.0058 50.2315 2
15 -9 -8 69.5931 66.9574 2
15 9 -6 56.8263 54.6991 2
15 9 -4 9.24328 33.9554 2
15 9 -2 18.7873 38.6850 2
15 10 -3 32.1900 35.1330 2
15 11 -2 104.538 70.4587 2
16 0 -8 119.144 76.8865 2
16 0 -6 18.4053 40.5199 3
16 0 -6 40.0584 34.3762 2
16 0 -4 138.179 87.4019 3
16 1 -7 33.6634 48.8324 3
16 -1 -7-52.5962 46.5899 2
16 1 -7 4.06225 53.5141 2
16 1 -5-9.26804 37.9856 3
16 1 -3-89.5659 81.9767 3
16 2 -8-42.5522 63.7560 3
16 2 -8 3.80601 38.1401 2
16 2 -6 50.6391 67.9125 3
16 2 -6-14.8665 37.3550 2
16 2 -4 201.007 97.3699 3
16 2 -2 67.9880 64.3438 3
16 3 -9-27.0475 58.3863 3
16 3 -7-139.127 65.4709 3
16 3 -7-95.2870 79.8026 2
16 3 -5 49.1715 69.9561 3
16 3 -5 199.258 86.7729 2
16 3 -3-74.6859 72.1531 3
16 3 -1 192.533 100.060 3
16 4 -8 71.0374 54.8148 3
16 -4 -8-153.097 87.1285 2
16 4 -6-6.97797 46.6505 3
16 4 -6 85.3876 44.4005 2
16 4 -4-31.8372 68.3322 3
16 4 -2-25.6417 54.4806 3
16 5 -7 21.9168 39.6790 3
16 5 -7-88.1683 71.6419 2
16 5 -5 25.9634 52.1756 3
16 5 -5-58.0581 63.2782 2
16 5 -3-18.1036 53.6728 3
16 6 -6-17.2952 40.7253 2
16 6 -4-96.0188 65.8744 2
16 7 -5 7.11333 44.8596 2
0 0 0 0.00 0.00 0
TITL H2Ac2NO2Im in I2/a
REM I2/a (#15 in standard setting)
CELL 0.71073 12.188959 18.718454 12.470102 90.0000 106.6120 90.0000
ZERR 8.00 0.000968 0.001089 0.000886 0.0000 0.0082 0.0000
LATT 2
SYMM -x+1/2, y,-z
SFAC C H N O
UNIT 96.00 96.00 48.00 24.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 14344
_shelx_res_file
;
TITL H2Ac2NO2Im in I2/a
shelx.res
created by SHELXL-2018/3 at 14:22:37 on 21-Dec-2018
CELL 0.71073 12.1890 18.7185 12.4701 90.000 106.612 90.000
ZERR 8.00 0.0010 0.0011 0.0009 0.000 0.008 0.000
LATT 2
SYMM 1/2 - X, Y, - Z
SFAC C H N O
UNIT 96 96 48 24
MERG 2
SHEL 20 0.8
EQIV $1 -x+3/2, y, -z+1
HTAB C9 O2_$1
EQIV $2 -x+1, -y, -z+1
HTAB N3 O1_$2
MPLA 6 C7 C8 C9 N2 N3 O1
FMAP 2
PLAN 8
SIZE 0.024 0.078 0.410
ACTA
BOND $H
CONF
LIST 4
L.S. 10
TEMP -3.15
WGHT 0.054100 0.645100
FVAR 1.61562 0.69450
C2 1 0.770837 0.008431 0.225600 11.00000 0.03741 0.03909 =
0.04041 -0.00758 0.01812 -0.00223
C3 1 0.790825 0.078016 0.199889 11.00000 0.06905 0.04389 =
0.06726 -0.00863 0.04672 -0.00366
AFIX 43
H3 2 0.757108 0.115674 0.227470 11.00000 -1.20000
AFIX 0
C4 1 0.860401 0.091188 0.133721 11.00000 0.09057 0.05103 =
0.08377 -0.00538 0.06149 -0.01120
AFIX 43
H4 2 0.875073 0.137819 0.116056 11.00000 -1.20000
AFIX 0
C5 1 0.908347 0.034624 0.093679 11.00000 0.07251 0.07008 =
0.07216 -0.00929 0.05504 -0.00770
AFIX 43
H5 2 0.955965 0.042029 0.048257 11.00000 -1.20000
AFIX 0
C6 1 0.884612 -0.032559 0.121966 11.00000 0.07018 0.06145 =
0.06741 -0.01364 0.04661 0.00297
AFIX 43
H6 2 0.917051 -0.070744 0.094242 11.00000 -1.20000
AFIX 0
C7 1 0.697220 -0.008465 0.299072 11.00000 0.03653 0.03456 =
0.04064 -0.00535 0.01773 -0.00048
C8 1 0.527352 0.092540 0.424698 11.00000 0.04554 0.03147 =
0.05091 0.00414 0.03017 0.00380
C9 1 0.543738 0.162127 0.369378 11.00000 0.05073 0.03045 =
0.05160 0.00274 0.03270 0.00318
AFIX 23
H9A 2 0.624798 0.172736 0.386342 11.00000 -1.20000
H9B 2 0.512995 0.157673 0.288837 11.00000 -1.20000
AFIX 0
C10 1 0.500478 0.244658 0.514574 11.00000 0.05152 0.03514 =
0.05610 -0.00101 0.02625 0.00710
C11 1 0.356647 0.298354 0.416939 11.00000 0.06277 0.05613 =
0.09587 0.00744 0.03074 0.02919
AFIX 43
H11 2 0.293877 0.328786 0.395097 11.00000 -1.20000
AFIX 0
C12 1 0.391580 0.254497 0.346202 11.00000 0.05006 0.04953 =
0.06621 0.00957 0.01764 0.01227
AFIX 43
H12 2 0.357589 0.249125 0.269746 11.00000 -1.20000
AFIX 0
C13 1 0.683869 -0.083879 0.331584 11.00000 0.06247 0.03782 =
0.06680 -0.00002 0.03944 0.00452
AFIX 33
H13A 2 0.728623 -0.114641 0.298954 21.00000 -1.50000
H13B 2 0.709665 -0.088178 0.411602 21.00000 -1.50000
H13C 2 0.604720 -0.097396 0.305138 21.00000 -1.50000
AFIX 0
N1 3 0.817510 -0.047033 0.187176 11.00000 0.05535 0.04637 =
0.05735 -0.01040 0.03482 0.00128
N2 3 0.649095 0.046002 0.328401 11.00000 0.04312 0.03612 =
0.04822 -0.00049 0.02921 0.00157
N3 3 0.581076 0.035835 0.398026 11.00000 0.05222 0.02891 =
0.05837 0.00551 0.03826 0.00501
AFIX 43
H3N 2 0.573246 -0.005884 0.423779 11.00000 -1.20000
AFIX 0
N4 3 0.485708 0.220228 0.409306 11.00000 0.04484 0.02876 =
0.05125 0.00494 0.02520 0.00412
N5 3 0.424809 0.292076 0.523084 11.00000 0.06764 0.04749 =
0.07992 -0.00522 0.03495 0.01826
N6 3 0.593139 0.223250 0.607350 11.00000 0.06983 0.05604 =
0.05536 -0.00908 0.02478 0.01133
O1 4 0.467490 0.088548 0.488103 11.00000 0.07197 0.03669 =
0.07706 0.01238 0.05814 0.01036
O2 4 0.673539 0.193215 0.587742 11.00000 0.05997 0.12183 =
0.06719 0.00163 0.02196 0.03374
O3 4 0.586352 0.234789 0.700729 11.00000 0.13505 0.10341 =
0.05704 -0.02104 0.02517 0.04531
H13D 2 0.636891 -0.094734 0.386005 -21.00000 0.01104
H13F 2 0.641035 -0.108263 0.255340 -21.00000 0.05896
H13E 2 0.768042 -0.106306 0.370057 -21.00000 0.05057
HKLF 4
REM H2Ac2NO2Im in I2/a
REM wR2 = 0.1192, GooF = S = 1.052, Restrained GooF = 1.052 for all data
REM R1 = 0.0442 for 1955 Fo > 4sig(Fo) and 0.0709 for all 2786 data
REM 203 parameters refined using 0 restraints
END
WGHT 0.0541 0.6451
REM Highest difference peak 0.186, deepest hole -0.199, 1-sigma level 0.039
Q1 1 0.6211 0.2784 0.6669 11.00000 0.05 0.19
Q2 1 0.7042 0.1236 0.1822 11.00000 0.05 0.16
Q3 1 0.4180 0.0429 0.4983 11.00000 0.05 0.14
Q4 1 0.8018 0.0434 0.2362 11.00000 0.05 0.13
Q5 1 0.7987 0.1277 0.2858 11.00000 0.05 0.13
Q6 1 0.3796 0.2407 0.2333 11.00000 0.05 0.12
Q7 1 0.6377 0.1539 0.5047 11.00000 0.05 0.12
Q8 1 0.6515 0.0877 0.2879 11.00000 0.05 0.12
;
_shelx_res_checksum 14472
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C2 0.77084(13) 0.00843(8) 0.22560(13) 0.0375(4) Uani d 1
C C3 0.79083(17) 0.07802(10) 0.19989(16) 0.0544(5) Uani d 1
H H3 0.757108 0.115674 0.227470 0.065 Uiso calc 1
C C4 0.8604(2) 0.09119(11) 0.13372(19) 0.0675(6) Uani d 1
H H4 0.875073 0.137819 0.116056 0.081 Uiso calc 1
C C5 0.90835(19) 0.03462(12) 0.09368(18) 0.0645(6) Uani d 1
H H5 0.955965 0.042029 0.048257 0.077 Uiso calc 1
C C6 0.88461(18) -0.03256(11) 0.12197(17) 0.0608(6) Uani d 1
H H6 0.917051 -0.070744 0.094242 0.073 Uiso calc 1
C C7 0.69722(13) -0.00847(8) 0.29907(13) 0.0359(4) Uani d 1
C C8 0.52735(14) 0.09254(8) 0.42470(14) 0.0392(4) Uani d 1
C C9 0.54374(15) 0.16213(8) 0.36938(14) 0.0405(4) Uani d 1
H H9A 0.624798 0.172736 0.386342 0.049 Uiso calc 1
H H9B 0.512995 0.157673 0.288837 0.049 Uiso calc 1
C C10 0.50048(15) 0.24466(9) 0.51457(15) 0.0453(4) Uani d 1
C C11 0.35665(19) 0.29835(11) 0.4169(2) 0.0699(6) Uani d 1
H H11 0.293877 0.328786 0.395097 0.084 Uiso calc 1
C C12 0.39158(16) 0.25450(10) 0.34620(17) 0.0551(5) Uani d 1
H H12 0.357589 0.249125 0.269746 0.066 Uiso calc 1
C C13 0.68387(19) -0.08388(9) 0.33158(19) 0.0513(5) Uani d 1
H H13A 0.728623 -0.114641 0.298954 0.077 Uiso calc 0.69(3)
H H13B 0.709665 -0.088178 0.411602 0.077 Uiso calc 0.69(3)
H H13C 0.604720 -0.097396 0.305138 0.077 Uiso calc 0.69(3)
N N1 0.81751(13) -0.04703(8) 0.18718(13) 0.0491(4) Uani d 1
N N2 0.64909(11) 0.04600(7) 0.32840(11) 0.0391(3) Uani d 1
N N3 0.58108(12) 0.03583(7) 0.39803(12) 0.0418(4) Uani d 1
H H3N 0.573246 -0.005884 0.423779 0.050 Uiso calc 1
N N4 0.48571(12) 0.22023(7) 0.40931(12) 0.0392(4) Uani d 1
N N5 0.42481(15) 0.29208(8) 0.52308(16) 0.0621(5) Uani d 1
N N6 0.59314(15) 0.22325(9) 0.60735(14) 0.0590(5) Uani d 1
O O1 0.46749(11) 0.08855(6) 0.48810(11) 0.0543(4) Uani d 1
O O2 0.67354(13) 0.19321(10) 0.58774(13) 0.0822(5) Uani d 1
O O3 0.58635(18) 0.23479(10) 0.70073(13) 0.0990(6) Uani d 1
H H13D 0.637(4) -0.095(2) 0.386(3) 0.011(13) Uiso d 0.31(3)
H H13F 0.641(5) -0.108(3) 0.255(6) 0.06(2) Uiso d 0.31(3)
H H13E 0.768(6) -0.106(3) 0.370(5) 0.05(2) Uiso d 0.31(3)
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
C2 0.0374(9) 0.0391(9) 0.0404(9) -0.0022(7) 0.0181(7) -0.0076(7)
C3 0.0691(13) 0.0439(11) 0.0673(13) -0.0037(9) 0.0467(11) -0.0086(9)
C4 0.0906(16) 0.0510(12) 0.0838(15) -0.0112(11) 0.0615(13) -0.0054(10)
C5 0.0725(14) 0.0701(14) 0.0722(14) -0.0077(11) 0.0550(12) -0.0093(11)
C6 0.0702(14) 0.0615(13) 0.0674(13) 0.0030(10) 0.0466(11) -0.0136(10)
C7 0.0365(9) 0.0346(9) 0.0406(9) -0.0005(7) 0.0177(7) -0.0054(7)
C8 0.0455(10) 0.0315(9) 0.0509(10) 0.0038(7) 0.0302(8) 0.0041(7)
C9 0.0507(10) 0.0304(9) 0.0516(10) 0.0032(7) 0.0327(8) 0.0027(7)
C10 0.0515(11) 0.0351(10) 0.0561(11) 0.0071(8) 0.0263(9) -0.0010(8)
C11 0.0628(14) 0.0561(13) 0.0959(18) 0.0292(10) 0.0307(14) 0.0074(11)
C12 0.0501(11) 0.0495(11) 0.0662(13) 0.0123(9) 0.0176(10) 0.0096(9)
C13 0.0625(13) 0.0378(10) 0.0668(13) 0.0045(9) 0.0394(12) 0.0000(9)
N1 0.0554(9) 0.0464(9) 0.0573(9) 0.0013(7) 0.0348(8) -0.0104(7)
N2 0.0431(8) 0.0361(8) 0.0482(8) 0.0016(6) 0.0292(7) -0.0005(6)
N3 0.0522(9) 0.0289(7) 0.0584(9) 0.0050(6) 0.0383(7) 0.0055(6)
N4 0.0448(8) 0.0288(7) 0.0513(9) 0.0041(6) 0.0252(7) 0.0049(6)
N5 0.0676(11) 0.0475(10) 0.0799(13) 0.0183(8) 0.0350(10) -0.0052(8)
N6 0.0698(12) 0.0560(10) 0.0554(11) 0.0113(8) 0.0248(9) -0.0091(8)
O1 0.0720(9) 0.0367(7) 0.0771(9) 0.0104(6) 0.0581(8) 0.0124(6)
O2 0.0600(9) 0.1218(14) 0.0672(10) 0.0337(9) 0.0220(8) 0.0016(9)
O3 0.1351(16) 0.1034(14) 0.0570(10) 0.0453(12) 0.0252(10) -0.0210(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 1 -2 0.0070
0 -1 2 0.0168
1 0 0 0.1906
-1 0 0 0.1946
0 1 2 0.0010
0 -1 -2 0.0246
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 C2 C3 121.90(15)
N1 C2 C7 116.67(14)
C3 C2 C7 121.42(14)
C4 C3 C2 119.53(17)
C4 C3 H3 120.2
C2 C3 H3 120.2
C3 C4 C5 118.96(19)
C3 C4 H4 120.5
C5 C4 H4 120.5
C6 C5 C4 118.39(18)
C6 C5 H5 120.8
C4 C5 H5 120.8
N1 C6 C5 123.95(17)
N1 C6 H6 118.0
C5 C6 H6 118.0
N2 C7 C2 114.37(14)
N2 C7 C13 125.58(15)
C2 C7 C13 120.05(14)
O1 C8 N3 122.52(14)
O1 C8 C9 121.91(14)
N3 C8 C9 115.57(13)
N4 C9 C8 110.22(12)
N4 C9 H9A 109.6
C8 C9 H9A 109.6
N4 C9 H9B 109.6
C8 C9 H9B 109.6
H9A C9 H9B 108.1
N5 C10 N4 114.05(17)
N5 C10 N6 122.67(17)
N4 C10 N6 123.23(15)
N5 C11 C12 111.35(17)
N5 C11 H11 124.3
C12 C11 H11 124.3
N4 C12 C11 106.24(18)
N4 C12 H12 126.9
C11 C12 H12 126.9
C7 C13 H13A 109.5
C7 C13 H13B 109.5
H13A C13 H13B 109.5
C7 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C7 C13 H13D 120(2)
H13A C13 H13D 130.8
H13B C13 H13D 51.3
H13C C13 H13D 58.6
C7 C13 H13F 103(3)
H13A C13 H13F 63.3
H13B C13 H13F 146.7
H13C C13 H13F 51.9
H13D C13 H13F 107(4)
C7 C13 H13E 109(3)
H13A C13 H13E 51.3
H13B C13 H13E 61.4
H13C C13 H13E 141.3
H13D C13 H13E 105(4)
H13F C13 H13E 113(4)
C6 N1 C2 117.27(16)
C7 N2 N3 118.58(13)
C8 N3 N2 118.27(13)
C8 N3 H3N 120.9
N2 N3 H3N 120.9
C10 N4 C12 105.05(14)
C10 N4 C9 129.77(14)
C12 N4 C9 124.58(15)
C10 N5 C11 103.31(16)
O3 N6 O2 123.90(19)
O3 N6 C10 118.36(18)
O2 N6 C10 117.73(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C2 N1 1.337(2)
C2 C3 1.380(2)
C2 C7 1.488(2)
C3 C4 1.364(3)
C3 H3 0.9300
C4 C5 1.371(3)
C4 H4 0.9300
C5 C6 1.359(3)
C5 H5 0.9300
C6 N1 1.336(2)
C6 H6 0.9300
C7 N2 1.2806(19)
C7 C13 1.490(2)
C8 O1 1.2219(19)
C8 N3 1.3381(19)
C8 C9 1.514(2)
C9 N4 1.4603(19)
C9 H9A 0.9700
C9 H9B 0.9700
C10 N5 1.306(2)
C10 N4 1.353(2)
C10 N6 1.424(3)
C11 N5 1.352(3)
C11 C12 1.359(3)
C11 H11 0.9300
C12 N4 1.353(2)
C12 H12 0.9300
C13 H13A 0.9600
C13 H13B 0.9600
C13 H13C 0.9600
C13 H13D 1.03(5)
C13 H13F 1.05(7)
C13 H13E 1.09(6)
N2 N3 1.3744(18)
N3 H3N 0.8600
N6 O3 1.210(2)
N6 O2 1.214(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C9 H9A O2 2_656 0.97 2.42 3.383(2) 174.5 yes
N3 H3N O1 5_656 0.86 2.04 2.8754(17) 163.8 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
N1 C2 C3 C4 -0.2(3)
C7 C2 C3 C4 178.91(18)
C2 C3 C4 C5 0.4(3)
C3 C4 C5 C6 -0.1(4)
C4 C5 C6 N1 -0.3(4)
N1 C2 C7 N2 -176.10(15)
C3 C2 C7 N2 4.7(2)
N1 C2 C7 C13 3.4(2)
C3 C2 C7 C13 -175.77(18)
O1 C8 C9 N4 3.8(2)
N3 C8 C9 N4 -177.26(15)
N5 C11 C12 N4 -0.9(2)
C5 C6 N1 C2 0.5(3)
C3 C2 N1 C6 -0.2(3)
C7 C2 N1 C6 -179.41(16)
C2 C7 N2 N3 -178.82(13)
C13 C7 N2 N3 1.7(3)
O1 C8 N3 N2 -178.23(16)
C9 C8 N3 N2 2.9(2)
C7 N2 N3 C8 -177.34(15)
N5 C10 N4 C12 -0.9(2)
N6 C10 N4 C12 -178.17(17)
N5 C10 N4 C9 -172.15(16)
N6 C10 N4 C9 10.6(3)
C11 C12 N4 C10 1.0(2)
C11 C12 N4 C9 172.87(16)
C8 C9 N4 C10 58.8(2)
C8 C9 N4 C12 -110.96(18)
N4 C10 N5 C11 0.3(2)
N6 C10 N5 C11 177.63(18)
C12 C11 N5 C10 0.4(2)
N5 C10 N6 O3 19.1(3)
N4 C10 N6 O3 -163.87(18)
N5 C10 N6 O2 -162.24(19)
N4 C10 N6 O2 14.8(3)
_cod_database_fobs_code 2021516