#------------------------------------------------------------------------------
#$Date: 2019-02-15 05:36:39 +0200 (Fri, 15 Feb 2019) $
#$Revision: 213660 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021515.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_2021515
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_gt 513.35
_chemical_melting_point_lt 513.75
_chemical_name_common
;
2-Acetylpyridine-4-nitroimidazole hydrazone
;
_chemical_name_systematic
2-(4-Nitro-1H-imidazol-1-yl)-N'-[1-(pyridin-2-yl)ethylidene]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'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2017/1
_cell_angle_alpha 90
_cell_angle_beta 96.721(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.9284(4)
_cell_length_b 13.6918(7)
_cell_length_c 16.0601(12)
_cell_measurement_reflns_used 2324
_cell_measurement_temperature 270(2)
_cell_measurement_theta_max 28.8130
_cell_measurement_theta_min 3.7360
_cell_volume 1294.65(15)
_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 0.0265
_diffrn_reflns_av_unetI/netI 0.0270
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8641
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.372
_diffrn_reflns_theta_min 1.960
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.111
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.66554
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.479
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 600
_exptl_crystal_size_max 0.421
_exptl_crystal_size_mid 0.284
_exptl_crystal_size_min 0.057
_refine_diff_density_max 0.157
_refine_diff_density_min -0.208
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 215
_refine_ls_number_reflns 2653
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0580
_refine_ls_R_factor_gt 0.0406
_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^)+(0.0532P)^2^+0.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0985
_refine_ls_wR_factor_ref 0.1129
_reflns_number_gt 2015
_reflns_number_total 2653
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ky3160sup1.cif
_cod_data_source_block 1
_cod_database_code 2021515
_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 0.955
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
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0 0 4 39163.9 371.961 3
0 0 -4 40728.6 316.225 2
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0 0 -4 39132.5 382.236 3
0 0 -5 9.15406 15.7679 2
0 0 5 4.28468 12.1142 3
0 0 5-3.79058 13.4446 2
0 0 -5 22.4513 21.8244 3
0 0 -6 3037.58 130.715 3
0 0 -6 3063.11 108.802 2
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0 0 -7-0.06264 14.4227 2
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0 0 -8 18894.9 379.100 3
0 0 8 19579.3 377.403 3
0 0 -8 18822.7 309.176 2
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0 0 -9-0.49122 16.8656 2
0 0 -9 21.8728 24.4332 3
0 0 9-11.8558 27.4488 3
0 0 9 1.42223 13.6188 2
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0 0 -10 3827.55 193.659 3
0 0 10 3615.75 154.311 2
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0 0 -13-21.5299 28.0638 3
0 0 13 30.4751 23.2583 2
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0 0 -18-16.6202 38.7145 3
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0 0 -21 16.8787 43.2480 3
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0 -1 -3 140.591 14.7257 2
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0 -1 3 103.610 20.4234 2
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0 -1 6 9832.95 217.945 2
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-7 -4 6 1320.82 175.147 1
-7 4 6 1261.88 177.539 1
-7 -4 5 22.7469 38.1205 1
-7 4 5-9.63892 40.3806 1
-7 -4 4-5.16057 37.3306 1
-7 -4 4 105.376 62.2868 3
-7 4 4 126.705 60.1298 1
-7 4 3 152.923 67.5601 1
-7 -4 3 46.7493 50.9289 3
-7 4 2-7.57062 50.5815 1
-7 -4 2-25.7102 41.7935 3
-7 4 1 128.646 60.4478 1
-7 -4 1 67.2330 55.7948 3
-7 4 0 16.5885 35.6350 1
-7 -4 0-58.9711 60.2275 3
-7 4 -1-11.6994 42.7091 1
-7 -4 -1 15.6243 39.8903 3
-7 4 -2 357.123 102.974 1
-7 -4 -2 167.739 74.1568 3
-7 4 -2 324.963 105.910 3
-7 4 -3 187.940 78.8493 3
-7 4 -4 320.974 102.230 3
-7 4 -5-30.0267 52.4278 3
-7 -5 12-0.31389 30.3343 1
-7 -5 11 94.6081 56.6135 1
-7 -5 10 76.8462 48.0017 1
-7 -5 9 155.316 65.6748 1
-7 -5 8 177.800 70.0247 1
-7 -5 7 151.241 63.3623 1
-7 -5 6 11.9201 44.5141 1
-7 -5 6 56.6188 50.3908 3
-7 -5 5 18.5199 43.2473 3
-7 5 5 47.1062 36.3275 1
-7 -5 4 70.4506 63.8895 3
-7 5 4-90.2077 63.1109 1
-7 -5 3 264.338 86.1043 3
-7 5 3 142.953 64.3943 1
-7 5 2 22.5414 42.7860 1
-7 -5 2 11.3011 31.4944 3
-7 5 1 45.7743 39.0607 1
-7 -5 1 27.4296 36.3947 3
-7 5 0-58.4710 53.0814 1
-7 -5 0 55.4649 64.0848 3
-7 5 -1-4.84951 52.8177 1
-7 -5 -1 83.7988 61.4709 3
-7 5 -2 68.7028 57.8613 1
-7 5 -3 479.046 120.406 1
-7 5 -3 483.330 130.681 3
-7 5 -4 131.696 73.8853 3
-7 5 -5 21.8180 36.0803 3
-7 -6 11 10.6974 31.5948 1
-7 -6 10-0.61964 42.6087 1
-7 -6 9 93.6443 54.7141 1
-7 -6 8 12.0008 33.0581 1
-7 -6 8 60.8309 48.6419 3
-7 -6 7-10.2678 52.3088 3
-7 -6 6 148.719 71.4698 3
-7 -6 5 1691.29 210.194 3
-7 -6 4-62.7765 39.4913 3
-7 -6 3 513.538 119.026 3
-7 6 3 737.262 141.107 1
-7 -6 2 7.92385 44.2993 3
-7 6 2 194.406 77.2322 1
-7 6 1 180.703 72.8274 1
-7 -6 1 243.231 88.3060 3
-7 6 0 619.274 134.900 1
-7 -6 0 630.417 132.096 3
-7 6 -1-28.0481 48.5243 1
-7 6 -2-97.1540 64.3610 1
-7 6 -3 14.2621 46.2480 3
-7 6 -4 442.095 119.319 3
-7 6 -5-81.6270 69.9510 3
-7 -7 10-65.4658 50.4506 3
-7 -7 9 43.9442 45.6985 3
-7 -7 8-5.81531 34.7872 3
-7 -7 7 88.0289 57.2339 3
-7 -7 6 68.8416 62.6940 3
-7 -7 5 34.9223 44.3866 3
-7 -7 4 127.531 64.6429 3
-7 -7 3 132.333 66.2728 3
-7 -7 2 34.1424 43.1086 3
-7 -7 1 3.53550 37.8647 3
-7 7 -3-52.2350 56.1866 3
-7 7 -4 162.731 82.6385 3
-7 -8 9-2.12270 30.7797 3
-7 -8 8 104.015 58.8176 3
-7 -8 7 8.37465 34.6497 3
-7 -8 6 150.614 65.5569 3
-7 -8 5-19.6929 41.9347 3
-7 -8 4 214.219 87.8713 3
-7 -8 3 73.6737 57.2109 3
-7 -8 2 114.450 64.6382 3
-7 -9 7-2.92455 30.8221 3
-7 -9 6 188.447 74.0411 3
-7 -9 5 87.2493 59.3026 3
0 0 0 0.00 0.00 0
TITL H2Ac4NO2Im-b in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 5.928446 13.691827 16.060125 90.0000 96.7208 90.0000
ZERR 3.00 0.000447 0.000750 0.001232 0.0000 0.0072 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 36.00 36.00 18.00 9.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 68470
_shelx_res_file
;
TITL H2Ac4NO2Im in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 14:14:20 on 21-Dec-2018
CELL 0.71073 5.9284 13.6918 16.0601 90.000 96.721 90.000
ZERR 4.00 0.0004 0.0007 0.0012 0.000 0.007 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O
UNIT 48 48 24 12
MERG 2
SHEL 20 0.8
EQIV $1 -x, -y, -z+1
HTAB N3 O1_$1
EQIV $2 -x, -y+1, -z+1
HTAB C9 O3_$2
EQIV $3 x-1, y, z
HTAB C9 N5_$3
EQIV $4 x+1, y, z
HTAB C10 N2_$4
HTAB C13 N1
EQIV $5 x-2, -y+1/2, z-1/2
HTAB C6 O2_$5
MPLA 6 O1 N2 N3 C9 C7 C8
FMAP 2
PLAN 8
SIZE 0.057 0.284 0.421
ACTA
BOND $H
CONF
LIST 4
L.S. 10
TEMP -3.15
WGHT 0.053200 0.177600
FVAR 3.64263 0.49229
C2 1 -0.725267 0.145859 0.305940 11.00000 0.03431 0.03779 =
0.03573 -0.00788 0.00172 -0.00173
C3 1 -0.697880 0.244313 0.287519 11.00000 0.04145 0.04010 =
0.05585 0.00222 -0.00625 -0.00503
AFIX 43
H3 2 -0.561957 0.276128 0.304993 11.00000 -1.20000
AFIX 0
C4 1 -0.874580 0.293664 0.243179 11.00000 0.05583 0.04541 =
0.06079 0.00787 -0.00603 -0.00104
AFIX 43
H4 2 -0.861256 0.359725 0.231202 11.00000 -1.20000
AFIX 0
C5 1 -1.070642 0.244121 0.216878 11.00000 0.04520 0.05762 =
0.04952 -0.00047 -0.00626 0.00886
AFIX 43
H5 2 -1.192383 0.275746 0.186430 11.00000 -1.20000
AFIX 0
C6 1 -1.083818 0.147361 0.236251 11.00000 0.03394 0.05919 =
0.04572 -0.00994 -0.00523 -0.00405
AFIX 43
H6 2 -1.217041 0.114171 0.217563 11.00000 -1.20000
AFIX 0
C7 1 -0.544574 0.089113 0.356545 11.00000 0.03560 0.03280 =
0.03686 -0.00587 0.00454 -0.00322
C8 1 -0.039248 0.149121 0.482089 11.00000 0.03378 0.02947 =
0.04229 -0.00071 0.00120 0.00179
C9 1 -0.059351 0.257726 0.465434 11.00000 0.02677 0.02948 =
0.05484 -0.00156 -0.00379 -0.00058
AFIX 23
H9A 2 -0.063787 0.269209 0.405665 11.00000 -1.20000
H9B 2 -0.201123 0.281109 0.482746 11.00000 -1.20000
AFIX 0
C10 1 0.352569 0.297266 0.508589 11.00000 0.02915 0.03935 =
0.06432 -0.01523 0.00419 0.00307
AFIX 43
H10 2 0.411275 0.244078 0.482246 11.00000 -1.20000
AFIX 0
C11 1 0.323594 0.425845 0.575787 11.00000 0.04005 0.02671 =
0.03964 -0.00121 -0.00382 0.00073
C12 1 0.106706 0.396834 0.552689 11.00000 0.03632 0.02734 =
0.03963 0.00250 0.00465 0.00653
AFIX 43
H12 2 -0.026307 0.427527 0.563994 11.00000 -1.20000
AFIX 0
C13 1 -0.564605 -0.019512 0.359239 11.00000 0.06300 0.03392 =
0.05891 -0.00232 -0.01401 -0.00234
N1 3 -0.917279 0.097572 0.280337 11.00000 0.03871 0.04309 =
0.04485 -0.00811 -0.00004 -0.00654
N2 3 -0.384964 0.140637 0.395271 11.00000 0.03054 0.03310 =
0.04191 -0.00202 0.00059 0.00213
N3 3 -0.210675 0.094741 0.444075 11.00000 0.03543 0.02677 =
0.04750 -0.00014 -0.00342 -0.00019
AFIX 43
H3N 2 -0.211003 0.032352 0.450253 11.00000 -1.20000
AFIX 0
N4 3 0.127530 0.312837 0.509318 11.00000 0.02605 0.02800 =
0.04565 -0.00259 0.00139 0.00224
N5 3 0.479580 0.364458 0.548627 11.00000 0.03105 0.03992 =
0.06160 -0.00981 -0.00292 0.00006
N6 3 0.391566 0.511905 0.622355 11.00000 0.06513 0.02729 =
0.04915 0.00153 -0.01627 0.00156
O1 4 0.121962 0.112478 0.525378 11.00000 0.04577 0.03298 =
0.06561 0.00405 -0.01720 0.00147
O2 4 0.594714 0.527163 0.641287 11.00000 0.07107 0.04323 =
0.10050 -0.00883 -0.03981 -0.00601
O3 4 0.240559 0.566453 0.640576 11.00000 0.08792 0.03421 =
0.06788 -0.01047 -0.00121 0.01381
PART 1
H13A 2 -0.407628 -0.051395 0.357228 21.00000 0.04153
H13B 2 -0.666526 -0.044429 0.313323 21.00000 0.03004
H13C 2 -0.582833 -0.037494 0.418135 21.00000 0.07216
PART 2
H14D 2 -0.483557 -0.049583 0.402014 -21.00000 0.03986
H13F 2 -0.483747 -0.045891 0.315262 -21.00000 0.04670
H13E 2 -0.746253 -0.031625 0.362912 -21.00000 0.07191
HKLF 4
REM H2Ac4NO2Im in P2(1)/c
REM wR2 = 0.1129, GooF = S = 1.054, Restrained GooF = 1.054 for all data
REM R1 = 0.0406 for 2015 Fo > 4sig(Fo) and 0.0580 for all 2653 data
REM 215 parameters refined using 0 restraints
END
WGHT 0.0532 0.1776
REM Highest difference peak 0.157, deepest hole -0.208, 1-sigma level 0.041
Q1 1 -0.6578 0.1781 0.2831 11.00000 0.05 0.16
Q2 1 -0.1623 0.1197 0.5711 11.00000 0.05 0.15
Q3 1 -0.8923 0.0374 0.2991 11.00000 0.05 0.15
Q4 1 -0.8850 -0.0419 0.3941 11.00000 0.05 0.13
Q5 1 0.2229 0.4392 0.5424 11.00000 0.05 0.12
Q6 1 -0.8118 0.1035 0.2737 11.00000 0.05 0.12
Q7 1 0.3922 0.3796 0.5979 11.00000 0.05 0.12
Q8 1 -0.6411 0.1269 0.3273 11.00000 0.05 0.11
;
_shelx_res_checksum 56403
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 C2 -0.7253(3) 0.14586(11) 0.30594(9) 0.0361(4) Uani d 1 . .
C C3 -0.6979(3) 0.24431(12) 0.28752(11) 0.0467(4) Uani d 1 . .
H H3 -0.561957 0.276128 0.304993 0.056 Uiso calc 1 . .
C C4 -0.8746(3) 0.29366(13) 0.24318(12) 0.0550(5) Uani d 1 . .
H H4 -0.861256 0.359725 0.231202 0.066 Uiso calc 1 . .
C C5 -1.0706(3) 0.24412(14) 0.21688(11) 0.0517(5) Uani d 1 . .
H H5 -1.192383 0.275746 0.186430 0.062 Uiso calc 1 . .
C C6 -1.0838(3) 0.14736(13) 0.23625(10) 0.0471(4) Uani d 1 . .
H H6 -1.217041 0.114171 0.217563 0.056 Uiso calc 1 . .
C C7 -0.5446(3) 0.08911(11) 0.35655(9) 0.0351(4) Uani d 1 . .
C C8 -0.0392(3) 0.14912(10) 0.48209(10) 0.0354(4) Uani d 1 . .
C C9 -0.0594(3) 0.25773(10) 0.46543(11) 0.0377(4) Uani d 1 . .
H H9A -0.063787 0.269209 0.405665 0.045 Uiso calc 1 . .
H H9B -0.201123 0.281109 0.482746 0.045 Uiso calc 1 . .
C C10 0.3526(3) 0.29727(11) 0.50859(12) 0.0444(4) Uani d 1 . .
H H10 0.411275 0.244078 0.482246 0.053 Uiso calc 1 . .
C C11 0.3236(3) 0.42585(10) 0.57579(9) 0.0361(4) Uani d 1 . .
C C12 0.1067(3) 0.39683(10) 0.55269(9) 0.0344(4) Uani d 1 . .
H H12 -0.026307 0.427527 0.563994 0.041 Uiso calc 1 . .
C C13 -0.5646(4) -0.01951(13) 0.35924(16) 0.0536(5) Uani d 1 . .
N N1 -0.9173(2) 0.09757(10) 0.28034(9) 0.0426(3) Uani d 1 . .
N N2 -0.3850(2) 0.14064(9) 0.39527(8) 0.0355(3) Uani d 1 . .
N N3 -0.2107(2) 0.09474(9) 0.44407(8) 0.0372(3) Uani d 1 . .
H H3N -0.211003 0.032352 0.450253 0.045 Uiso calc 1 . .
N N4 0.1275(2) 0.31284(8) 0.50932(8) 0.0335(3) Uani d 1 . .
N N5 0.4796(2) 0.36446(9) 0.54863(9) 0.0449(4) Uani d 1 . .
N N6 0.3916(3) 0.51191(10) 0.62235(9) 0.0490(4) Uani d 1 . .
O O1 0.1220(2) 0.11248(8) 0.52538(8) 0.0500(3) Uani d 1 . .
O O2 0.5947(3) 0.52716(9) 0.64129(10) 0.0755(5) Uani d 1 . .
O O3 0.2406(3) 0.56645(8) 0.64058(8) 0.0642(4) Uani d 1 . .
H H13A -0.408(8) -0.051(3) 0.357(3) 0.042(14) Uiso d 0.49(7) A 1
H H13B -0.667(6) -0.044(2) 0.313(3) 0.030(15) Uiso d 0.49(7) A 1
H H13C -0.583(10) -0.037(4) 0.418(4) 0.07(2) Uiso d 0.49(7) A 1
H H14D -0.484(9) -0.050(3) 0.402(3) 0.040(13) Uiso d 0.51(7) A 2
H H13F -0.484(8) -0.046(3) 0.315(3) 0.047(15) Uiso d 0.51(7) A 2
H H13E -0.746(10) -0.032(3) 0.363(3) 0.07(2) Uiso d 0.51(7) A 2
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 0.0343(9) 0.0378(8) 0.0357(8) -0.0017(7) 0.0017(7) -0.0079(7)
C3 0.0415(10) 0.0401(9) 0.0558(11) -0.0050(7) -0.0062(8) 0.0022(8)
C4 0.0558(12) 0.0454(10) 0.0608(12) -0.0010(9) -0.0060(9) 0.0079(9)
C5 0.0452(11) 0.0576(11) 0.0495(10) 0.0089(9) -0.0063(8) -0.0005(9)
C6 0.0339(10) 0.0592(11) 0.0457(9) -0.0041(8) -0.0052(8) -0.0099(8)
C7 0.0356(9) 0.0328(8) 0.0369(8) -0.0032(7) 0.0045(7) -0.0059(6)
C8 0.0338(9) 0.0295(7) 0.0423(8) 0.0018(6) 0.0012(7) -0.0007(7)
C9 0.0268(8) 0.0295(7) 0.0548(10) -0.0006(6) -0.0038(7) -0.0016(7)
C10 0.0292(9) 0.0393(8) 0.0643(11) 0.0031(7) 0.0042(8) -0.0152(8)
C11 0.0401(10) 0.0267(7) 0.0396(8) 0.0007(6) -0.0038(7) -0.0012(6)
C12 0.0363(9) 0.0273(7) 0.0396(8) 0.0065(6) 0.0047(7) 0.0025(6)
C13 0.0630(16) 0.0339(9) 0.0589(13) -0.0023(9) -0.0140(13) -0.0023(9)
N1 0.0387(8) 0.0431(7) 0.0449(7) -0.0065(6) 0.0000(6) -0.0081(6)
N2 0.0305(7) 0.0331(7) 0.0419(7) 0.0021(5) 0.0006(6) -0.0020(6)
N3 0.0354(8) 0.0268(6) 0.0475(8) -0.0002(5) -0.0034(6) -0.0001(6)
N4 0.0261(7) 0.0280(6) 0.0457(7) 0.0022(5) 0.0014(6) -0.0026(5)
N5 0.0311(8) 0.0399(7) 0.0616(9) 0.0001(6) -0.0029(6) -0.0098(7)
N6 0.0651(11) 0.0273(7) 0.0492(8) 0.0016(7) -0.0163(8) 0.0015(6)
O1 0.0458(7) 0.0330(5) 0.0656(8) 0.0015(5) -0.0172(6) 0.0040(5)
O2 0.0711(11) 0.0432(7) 0.1005(11) -0.0060(7) -0.0398(9) -0.0088(7)
O3 0.0879(11) 0.0342(6) 0.0679(9) 0.0138(7) -0.0012(8) -0.0105(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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 5 1 0.2488
-1 0 -5 0.0167
1 0 5 0.0407
5 1 2 0.0786
-5 -1 -2 0.0956
0 -5 -1 0.1528
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 116.26(14)
C3 C2 C7 121.83(14)
C4 C3 C2 119.02(16)
C4 C3 H3 120.5
C2 C3 H3 120.5
C5 C4 C3 118.99(17)
C5 C4 H4 120.5
C3 C4 H4 120.5
C6 C5 C4 118.66(17)
C6 C5 H5 120.7
C4 C5 H5 120.7
N1 C6 C5 123.97(16)
N1 C6 H6 118.0
C5 C6 H6 118.0
N2 C7 C2 114.94(13)
N2 C7 C13 126.23(16)
C2 C7 C13 118.82(15)
O1 C8 N3 121.96(13)
O1 C8 C9 122.98(14)
N3 C8 C9 115.05(13)
N4 C9 C8 112.63(12)
N4 C9 H9A 109.1
C8 C9 H9A 109.1
N4 C9 H9B 109.1
C8 C9 H9B 109.1
H9A C9 H9B 107.8
N5 C10 N4 113.34(14)
N5 C10 H10 123.3
N4 C10 H10 123.3
C12 C11 N5 112.98(13)
C12 C11 N6 125.85(15)
N5 C11 N6 121.17(14)
C11 C12 N4 104.38(13)
C11 C12 H12 127.8
N4 C12 H12 127.8
C7 C13 H13A 110(2)
C7 C13 H13B 112.1(19)
H13A C13 H13B 108(3)
C7 C13 H13C 107(3)
H13A C13 H13C 97(4)
H13B C13 H13C 121(4)
C7 C13 H14D 116(2)
C7 C13 H13F 108(2)
H14D C13 H13F 97(4)
C7 C13 H13E 104(2)
H14D C13 H13E 109(4)
H13F C13 H13E 124(3)
C6 N1 C2 117.44(15)
C7 N2 N3 119.24(13)
C8 N3 N2 118.87(12)
C8 N3 H3N 120.6
N2 N3 H3N 120.6
C10 N4 C12 106.68(13)
C10 N4 C9 127.66(13)
C12 N4 C9 125.37(13)
C10 N5 C11 102.62(13)
O2 N6 O3 124.08(15)
O2 N6 C11 118.66(15)
O3 N6 C11 117.26(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C2 N1 1.3388(19)
C2 C3 1.394(2)
C2 C7 1.486(2)
C3 C4 1.373(2)
C3 H3 0.9300
C4 C5 1.369(3)
C4 H4 0.9300
C5 C6 1.365(3)
C5 H5 0.9300
C6 N1 1.333(2)
C6 H6 0.9300
C7 N2 1.2814(19)
C7 C13 1.493(2)
C8 O1 1.2219(18)
C8 N3 1.3471(19)
C8 C9 1.513(2)
C9 N4 1.4528(19)
C9 H9A 0.9700
C9 H9B 0.9700
C10 N5 1.309(2)
C10 N4 1.352(2)
C10 H10 0.9300
C11 C12 1.355(2)
C11 N5 1.359(2)
C11 N6 1.428(2)
C12 N4 1.3576(19)
C12 H12 0.9300
C13 H13A 1.03(5)
C13 H13B 0.96(4)
C13 H13C 1.00(6)
C13 H14D 0.89(4)
C13 H13F 0.97(5)
C13 H13E 1.10(6)
N2 N3 1.3738(17)
N3 H3N 0.8600
N6 O2 1.225(2)
N6 O3 1.2273(19)
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 H3N O1 3_556 0.86 2.08 2.9166(16) 165.0 yes
C9 H9A O3 3_566 0.97 2.56 3.069(2) 113.1 yes
C9 H9B N5 1_455 0.97 2.54 3.500(2) 168.2 yes
C10 H10 N2 1_655 0.93 2.41 3.316(2) 164.4 yes
C13 H13B N1 . 0.96(4) 2.47(3) 2.815(3) 101(2) yes
C6 H6 O2 4_365 0.93 2.48 3.315(2) 148.8 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 1.3(3)
C7 C2 C3 C4 -177.52(15)
C2 C3 C4 C5 -1.4(3)
C3 C4 C5 C6 0.4(3)
C4 C5 C6 N1 0.7(3)
N1 C2 C7 N2 -165.52(13)
C3 C2 C7 N2 13.3(2)
N1 C2 C7 C13 13.5(2)
C3 C2 C7 C13 -167.62(18)
O1 C8 C9 N4 -2.5(2)
N3 C8 C9 N4 178.82(13)
N5 C11 C12 N4 0.35(18)
N6 C11 C12 N4 179.25(14)
C5 C6 N1 C2 -0.9(2)
C3 C2 N1 C6 -0.2(2)
C7 C2 N1 C6 178.69(13)
C2 C7 N2 N3 179.66(12)
C13 C7 N2 N3 0.7(3)
O1 C8 N3 N2 -179.03(14)
C9 C8 N3 N2 -0.4(2)
C7 N2 N3 C8 177.57(14)
N5 C10 N4 C12 0.4(2)
N5 C10 N4 C9 174.38(15)
C11 C12 N4 C10 -0.42(17)
C11 C12 N4 C9 -174.60(14)
C8 C9 N4 C10 52.4(2)
C8 C9 N4 C12 -134.66(15)
N4 C10 N5 C11 -0.16(19)
C12 C11 N5 C10 -0.13(19)
N6 C11 N5 C10 -179.08(14)
C12 C11 N6 O2 177.51(16)
N5 C11 N6 O2 -3.7(2)
C12 C11 N6 O3 -2.8(2)
N5 C11 N6 O3 176.00(15)
_cod_database_fobs_code 2021515