#------------------------------------------------------------------------------
#$Date: 2022-11-08 20:40:13 +0100 (Tue, 08 Nov 2022) $
#$Revision: 279111 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022673.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_2022673
loop_
_publ_author_name
'W\'ojcicka, Anna'
'Becan, Lilianna'
'Rembia\/lkowska, Nina'
'Pyra, Anna'
'Bryndal, Iwona'
_publ_section_title
;
Structure and cytotoxic properties of
1-hydroxy-5-methyl-7-phenylpyrido[3,4-d]pyridazin-4(3H)-one
and its mono- and disubstituted ethyl acetates
;
_journal_coeditor_code QF3056
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 559
_journal_page_last 569
_journal_paper_doi 10.1107/S2053229622009202
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C18 H17 N3 O4'
_chemical_formula_moiety 'C18 H17 N3 O4'
_chemical_formula_sum 'C18 H17 N3 O4'
_chemical_formula_weight 339.34
_chemical_name_systematic
;Ethyl
[1-(2-ethoxy-2-oxoethoxy)-5-methyl-4-oxo-7-phenyl-3,4-dihydropyrido[3,4-d]pyridazin-3-yl]acetate
;
_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
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 92.3150(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.4344(3)
_cell_length_b 13.0800(3)
_cell_length_c 7.01920(10)
_cell_measurement_reflns_used 1548
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 69.8
_cell_measurement_theta_min 2.5
_cell_volume 1599.37(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2014)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy DW system with a HyPix-Arc 150 detector'
_diffrn_measurement_method '\f scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0350
_diffrn_reflns_av_unetI/netI 0.0305
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 15272
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.656
_diffrn_reflns_theta_min 2.536
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 0.841
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73598
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.409
_exptl_crystal_description plate
_exptl_crystal_F_000 712
_exptl_crystal_size_max 0.170
_exptl_crystal_size_mid 0.030
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.307
_refine_diff_density_min -0.202
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 228
_refine_ls_number_reflns 3274
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.096
_refine_ls_R_factor_all 0.0593
_refine_ls_R_factor_gt 0.0500
_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^)+(0.0533P)^2^+0.7835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1184
_refine_ls_wR_factor_ref 0.1232
_reflns_number_gt 2878
_reflns_number_total 3274
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file qf3056sup1.cif
_cod_data_source_block 3
_cod_depositor_comments
'Adding full bibliography for 2022672--2022674.cif.'
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022673
_cod_database_fobs_code 2022673
_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 0.870
_shelx_estimated_absorpt_t_max 0.975
_shelx_hkl_file
;
0 0 -1-5.43229 29.6330 26
0 0 -1-0.26910 18.6568 24
0 0 -1 12.9037 10.5938 1
0 0 -1-1.58796 23.2514 12
0 0 -1 13.9279 27.5265 13
0 0 -1 6.03846 25.3288 21
0 0 -1 13.4563 28.8268 16
0 0 -2 198074. 9571.17 29
0 0 -2 210138. 9575.22 26
0 0 -2 203341. 9571.34 24
0 0 -2 206810. 9574.21 21
0 0 -2 216457. 9575.80 16
0 0 -2 206301. 9574.70 14
0 0 -2 206154. 9575.62 13
0 0 2 207665. 9570.92 32
0 0 -2 215315. 9575.05 12
0 0 3 13.7179 23.3154 32
0 0 -3 52.4626 48.0681 18
0 0 -3 52.6105 48.0033 17
0 0 -3 22.1627 51.8785 26
0 0 -3 1.46167 43.6669 28
0 0 -3 62.0807 28.0632 29
0 0 -3-19.6141 55.0872 27
0 0 3 30.4349 22.4424 5
0 0 -3 68.1023 52.1005 13
0 0 -3-3.64012 49.3454 16
0 0 -3-6.46222 52.9552 14
0 0 -3 6.05555 29.1876 24
0 0 -4 29980.1 1418.36 14
0 0 -4 31437.2 1421.75 13
0 0 -4 30822.5 1416.78 28
0 0 -4 29608.7 1418.72 27
0 0 -4 29540.1 1411.85 9
0 0 -4 30897.6 1420.39 17
0 0 -5 94.4440 57.3777 27
0 0 -5-60.1566 60.3694 31
0 0 -5 30.4949 53.8825 19
0 0 -5 6.85564 56.4652 17
0 0 -5 15.1941 55.7340 18
0 0 -5 45.4370 56.9583 22
0 0 -5 3.10801 54.7026 23
0 0 -6 6407.68 329.665 18
0 0 -6 7004.03 334.302 31
0 0 -6 6706.95 330.218 23
0 0 -6 6470.15 334.106 22
0 0 -6 6224.49 325.811 19
0 0 -7 21.2675 49.9402 18
0 0 -7-10.0092 54.7201 31
0 0 -7-20.1363 50.8947 23
0 0 -7-79.8051 56.4062 22
0 0 -8 1770.97 108.055 35
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0 1 -1 6729.59 293.479 28
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0 1 -1 6491.07 294.873 16
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0 -6 1 1856.49 110.480 1
0 -6 -1 1806.65 105.954 1
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19 4 -2 174.177 46.2287 4
-19 4 2 118.910 49.9894 15
-19 4 2 133.381 43.6172 11
-19 -4 2 134.793 48.2057 25
19 4 -1 25.6158 38.6482 4
-19 4 1 24.1828 51.6155 15
-19 4 1 15.8627 43.5639 11
-19 -4 1 51.7181 49.6858 25
-19 4 0 135.532 56.1795 15
-19 -4 0 166.424 50.7568 25
19 -4 1 6.50248 39.8622 2
-19 -4 -1 50.0395 43.9126 16
-19 4 -1 26.8290 51.5587 15
-19 -4 -1-5.75980 45.4360 25
-19 -4 -2 79.4462 40.6294 16
-19 4 -2 46.9545 33.1683 12
-19 -4 -2 52.1444 44.6028 12
-19 4 -3 92.4416 38.4017 13
19 5 -3 30.8927 35.4847 4
19 -5 -3 80.8215 33.7720 2
19 5 -3 34.2798 34.5950 3
-19 5 3 21.0216 36.2517 15
19 5 -2 119.485 39.7630 4
-19 5 2 94.7017 44.8796 15
19 5 -1 714.056 54.7585 4
-19 5 1 695.615 67.6817 15
-19 -5 1 693.428 63.3107 25
19 -5 -1 738.540 69.1405 2
-19 5 0 861.847 71.7324 15
-19 -5 0 840.380 67.7190 25
19 -5 1 696.283 56.8085 2
-19 -5 -1 755.732 63.6185 16
-19 -5 -2 69.6618 40.1027 16
19 6 -3 32.1431 26.3222 3
-19 6 3 71.2809 29.9967 15
19 6 -3 84.0320 27.5844 4
19 -6 -2 289.289 45.1375 2
-19 6 2 297.855 44.1668 15
19 6 -2 245.206 37.7130 4
19 -6 -1 466.722 57.0033 2
-19 6 1 470.119 52.7893 15
19 -6 0 55.4530 43.1548 2
-19 6 0-7.17212 43.6246 15
19 -6 1 23.5247 32.2668 2
-19 -6 -1 117.864 40.4824 16
-19 -6 -2 119.303 35.7574 16
19 -7 -2 38.7706 30.4238 2
-19 7 2-9.06149 29.2875 15
19 -7 -1 476.450 50.2508 2
-19 7 1 610.718 48.2231 15
19 -7 0 1.77468 34.6441 2
-19 7 0 48.3330 33.4496 15
-19 -7 -1 288.782 40.5840 16
19 -8 -1 777.242 50.8044 2
20 0 -3 33.1691 38.4492 3
20 0 -2 70.1106 45.8155 3
-20 0 1 17.5737 38.6102 11
20 0 -1 44.7419 40.8682 3
-20 0 0 840.646 68.6147 25
-20 0 0 755.510 67.7575 15
-20 0 -1-31.2157 40.9357 25
-20 0 -1 39.6627 48.0617 12
-20 0 -2 195.945 46.3066 12
-20 0 -3 47.3322 30.7102 12
20 1 -3 51.5885 38.9816 3
20 -1 -3 145.920 40.9370 3
20 -1 -2 128.362 45.3133 3
20 1 -2 63.9474 43.4449 3
-20 -1 1 53.1685 43.7872 25
-20 1 1-15.8108 45.5272 15
-20 1 1 66.0065 41.5373 11
20 -1 -1 82.7315 41.2548 3
20 1 -1 30.8388 40.6251 3
-20 1 0 85.7616 48.7610 15
-20 -1 0 106.395 46.6928 25
-20 1 0 38.2495 43.3543 12
-20 -1 -1 65.9547 44.1691 25
-20 1 -1 62.7654 44.4136 12
-20 -1 -1 69.3778 48.1625 12
-20 1 -2 41.1242 41.3197 12
-20 -1 -2 15.9495 40.6887 12
-20 -1 -3 299.434 34.7604 12
20 2 -3 1081.60 71.0033 3
-20 2 2 319.563 47.0258 15
20 2 -2 276.017 48.7023 3
20 -2 -2 438.769 50.8986 3
-20 -2 1 55.3298 42.8951 25
-20 2 1-11.1943 38.8567 11
20 2 -1-12.5685 38.1343 3
-20 2 0 362.494 55.3542 15
-20 -2 0 316.018 51.9361 25
-20 2 0 276.074 46.0604 12
-20 2 -1 407.207 48.5762 12
-20 -2 -1 347.965 56.1143 12
-20 2 -2 39.5679 36.9903 12
-20 -2 -2-67.2552 42.2633 12
-20 3 3 228.233 35.3841 15
20 3 -3 236.366 36.6441 3
-20 3 2 61.5679 40.5655 15
20 3 -2 81.2138 39.6446 3
-20 3 1 149.942 47.7674 15
20 3 -1 169.594 39.5794 3
-20 3 0 259.294 53.8135 15
-20 3 -1 41.7463 32.2232 12
-20 -3 -1-9.68503 43.0684 12
-20 -3 -2 19.4376 36.8879 12
20 4 -3 86.6913 28.1427 3
20 -4 -2 100.316 41.4896 2
20 4 -2 153.462 36.3239 3
-20 4 2 127.257 40.5233 15
20 -4 -1 214.031 46.3281 2
20 4 -1 226.552 37.2268 3
-20 4 1 170.294 46.4507 15
20 -4 0 16.2345 39.4030 2
-20 4 0 86.9575 45.1189 15
-20 -4 -1 72.3259 40.6285 12
-20 -4 -2 81.5491 32.5932 12
20 -5 -2 75.2614 34.8130 2
20 5 -2 67.1540 28.5985 3
-20 5 2 112.021 36.2877 15
20 -5 -1 1504.13 89.0531 2
-20 5 1 1638.21 90.4085 15
20 5 -1 1387.34 82.3789 3
20 -5 0 3.48737 34.2762 2
-20 5 0 107.888 39.0697 15
-20 -5 -1 148.181 35.5974 12
20 -6 -1 21.4100 30.4113 2
-20 6 1-4.75523 30.1727 15
20 -6 0 98.2106 29.0221 2
21 0 -2 18.7957 29.4629 3
-21 0 1 4.97655 32.1119 12
-21 0 0 71.4624 35.8318 12
-21 0 -1 69.7263 35.6178 12
21 1 -2 190.000 33.8067 3
21 1 -1 15.0385 27.0197 3
-21 1 0 72.3490 32.9078 12
-21 -1 0 182.811 40.7291 12
-21 1 -1 141.836 33.5781 12
-21 -1 -1 171.235 38.1286 12
21 2 -2 107.238 30.5752 3
-21 2 1 291.022 41.4643 15
21 -2 0 14.4293 28.4492 2
-21 -2 0 30.9913 37.4767 12
-21 -2 -1 328.348 41.6649 12
21 -3 -2 71.9849 27.9114 2
21 -3 -1 780.786 57.2964 2
-21 3 1 869.240 57.5352 15
21 -3 0 52.0384 27.5248 2
-21 -3 0 34.1056 34.2031 12
-21 -3 -1 72.9864 31.7543 12
21 -4 -1 99.4686 29.8016 2
-21 -4 0 179.954 33.3392 12
0 0 0 0.00 0.00 0
TITL pm13m_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 17.434400 13.079970 7.019158 90.0000 92.3150 90.0000
ZERR 5.00 0.000318 0.000280 0.000118 0.0000 0.0014 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 50.00 50.00 20.00 20.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 75357
_shelx_res_file
;
TITL pm13m.res in P2(1)/c
3.res
created by SHELXL-2018/1 at 09:14:19 on 21-Jun-2022
CELL 1.54184 17.4344 13.08 7.0192 90 92.315 90
ZERR 4 0.0003 0.0003 0.0001 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 72 68 12 16
size 0.17 0.03 0.03
L.S. 4
PLAN 5
TEMP -173
fmap 2
HTAB 2.2
BOND $H
EQIV $3 -x, -y+1, -z+1
HTAB N3 O4_$3
EQIV $1 -x+1, y-1/2, -z+1/2
HTAB C14 O12_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C14 O12_$2
EQIV $4 -x+1, -y+1, -z
HTAB C13 O12_$4
EQIV $5 x, -y+3/2, z-1/2
HTAB C51 O4_$5
ACTA
CONF
mpla 8 C1 O1 C11 C12 O12 O13 C13 C14
mpla 10 C1 N2 N3 C4 C10 C9 C8 C7 N6 C5 C51 O1 O4 H3
MPLA 6 C71 C72 C73 C74 C75 C76
mpla 10 C1 N2 N3 C4 C10 C9 C8 C7 N6 C5
mpla 7 O1 C11 C12 O12 O13 C13 C14
WGHT 0.053300 0.783500
FVAR 2.81373
C1 1 0.204074 0.608290 0.335365 11.00000 0.02250 0.02511 =
0.02155 -0.00018 0.00322 -0.00027
O1 4 0.279739 0.599189 0.300552 11.00000 0.02303 0.02021 =
0.03258 0.00104 0.00612 0.00163
C11 1 0.308192 0.496531 0.315157 11.00000 0.02746 0.02010 =
0.02530 0.00168 0.00502 0.00204
AFIX 23
H111 2 0.280079 0.451875 0.222334 11.00000 -1.20000
H112 2 0.301025 0.469441 0.444930 11.00000 -1.20000
AFIX 0
C12 1 0.392222 0.498878 0.273773 11.00000 0.02757 0.02092 =
0.02350 -0.00290 0.00356 -0.00047
O12 4 0.426786 0.568076 0.204562 11.00000 0.02715 0.02422 =
0.03795 0.00234 0.00655 -0.00343
O13 4 0.423592 0.409252 0.325477 11.00000 0.02603 0.02247 =
0.03588 0.00332 0.00802 0.00227
C13 1 0.504804 0.397238 0.290321 11.00000 0.02383 0.02733 =
0.03585 -0.00008 0.00621 0.00272
AFIX 23
H131 2 0.534376 0.455913 0.343799 11.00000 -1.20000
H132 2 0.512733 0.393650 0.151615 11.00000 -1.20000
AFIX 0
C14 1 0.530610 0.299773 0.385707 11.00000 0.03720 0.03233 =
0.04415 0.00055 0.00573 0.00727
AFIX 137
H141 2 0.500106 0.242594 0.333566 11.00000 -1.50000
H142 2 0.523598 0.304973 0.523192 11.00000 -1.50000
H143 2 0.584979 0.288096 0.362658 11.00000 -1.50000
AFIX 0
N2 3 0.164131 0.527417 0.361062 11.00000 0.02406 0.02344 =
0.02567 -0.00035 0.00455 0.00041
N3 3 0.088599 0.541255 0.400056 11.00000 0.02369 0.02019 =
0.03080 -0.00054 0.00667 -0.00354
AFIX 43
H3 2 0.061443 0.485415 0.415974 11.00000 -1.20000
AFIX 0
C4 1 0.050784 0.631175 0.416989 11.00000 0.02518 0.02209 =
0.02144 0.00008 0.00183 -0.00026
O4 4 -0.017678 0.631370 0.460530 11.00000 0.02347 0.02420 =
0.03427 0.00168 0.00655 -0.00147
C5 1 0.066057 0.823467 0.395755 11.00000 0.02238 0.02325 =
0.02031 -0.00117 0.00253 -0.00211
C51 1 -0.016591 0.845563 0.433825 11.00000 0.02382 0.02329 =
0.03153 -0.00061 0.00542 0.00047
AFIX 137
H511 2 -0.029101 0.816888 0.557765 11.00000 -1.50000
H512 2 -0.049690 0.814526 0.333548 11.00000 -1.50000
H513 2 -0.024832 0.919671 0.434967 11.00000 -1.50000
AFIX 0
N6 3 0.110522 0.905268 0.374389 11.00000 0.02456 0.02149 =
0.02359 -0.00077 0.00374 -0.00066
C7 1 0.186309 0.893869 0.340034 11.00000 0.02324 0.02262 =
0.01869 -0.00017 0.00163 -0.00223
C71 1 0.230230 0.991014 0.323725 11.00000 0.02564 0.02396 =
0.02059 -0.00117 0.00382 -0.00216
C72 1 0.191083 1.083008 0.291547 11.00000 0.02562 0.02570 =
0.04016 -0.00013 0.00525 -0.00092
AFIX 43
H72 2 0.136623 1.083014 0.279027 11.00000 -1.20000
AFIX 0
C73 1 0.230942 1.174373 0.277688 11.00000 0.03292 0.02295 =
0.05460 0.00159 0.00419 0.00062
AFIX 43
H73 2 0.203789 1.236386 0.254404 11.00000 -1.20000
AFIX 0
C74 1 0.310591 1.175176 0.297867 11.00000 0.03259 0.02392 =
0.04150 -0.00117 0.00495 -0.00854
AFIX 43
H74 2 0.337833 1.237841 0.290086 11.00000 -1.20000
AFIX 0
C75 1 0.350119 1.084747 0.329258 11.00000 0.02416 0.03054 =
0.02892 -0.00091 0.00422 -0.00377
AFIX 43
H75 2 0.404570 1.085344 0.342154 11.00000 -1.20000
AFIX 0
C76 1 0.310463 0.992819 0.342047 11.00000 0.02539 0.02536 =
0.02442 -0.00111 0.00251 -0.00103
AFIX 43
H76 2 0.338009 0.930930 0.363338 11.00000 -1.20000
AFIX 0
C8 1 0.219772 0.798436 0.321427 11.00000 0.02037 0.02521 =
0.02353 0.00002 0.00342 -0.00068
AFIX 43
H8 2 0.272420 0.792202 0.293389 11.00000 -1.20000
AFIX 0
C9 1 0.174444 0.711656 0.344774 11.00000 0.02414 0.02147 =
0.01968 -0.00067 0.00182 -0.00021
C10 1 0.096292 0.723147 0.383387 11.00000 0.02355 0.02187 =
0.01859 0.00026 0.00168 -0.00171
HKLF 4
REM pm13m.res in P2(1)/c
REM R1 = 0.0500 for 2878 Fo > 4sig(Fo) and 0.0593 for all 3274 data
REM 228 parameters refined using 0 restraints
END
WGHT 0.0533 0.7835
REM Instructions for potential hydrogen bonds
HTAB C13 O12_$4
HTAB C14 O12_$1
HTAB C14 O12_$2
HTAB N3 O4_$3
HTAB C51 O4_$5
REM Highest difference peak 0.307, deepest hole -0.202, 1-sigma level 0.051
Q1 1 0.0758 0.6809 0.4027 11.00000 0.05 0.31
Q2 1 0.2113 0.9457 0.3527 11.00000 0.05 0.28
Q3 1 0.1352 0.7139 0.3658 11.00000 0.05 0.27
Q4 1 0.1903 0.6628 0.3485 11.00000 0.05 0.26
Q5 1 0.2107 0.8522 0.3658 11.00000 0.05 0.24
;
_shelx_res_checksum 90591
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 0.20407(9) 0.60829(14) 0.3354(2) 0.0230(4) Uani d 1 . .
O O1 0.27974(7) 0.59919(9) 0.30055(17) 0.0251(3) Uani d 1 . .
C C11 0.30819(10) 0.49653(14) 0.3152(2) 0.0242(4) Uani d 1 . .
H H111 0.280079 0.451875 0.222334 0.029 Uiso calc 1 . .
H H112 0.301025 0.469441 0.444930 0.029 Uiso calc 1 . .
C C12 0.39222(10) 0.49888(13) 0.2738(2) 0.0239(4) Uani d 1 . .
O O12 0.42679(7) 0.56808(10) 0.20456(18) 0.0296(3) Uani d 1 . .
O O13 0.42359(7) 0.40925(9) 0.32548(18) 0.0279(3) Uani d 1 . .
C C13 0.50480(10) 0.39724(15) 0.2903(3) 0.0289(4) Uani d 1 . .
H H131 0.534376 0.455913 0.343799 0.035 Uiso calc 1 . .
H H132 0.512733 0.393650 0.151615 0.035 Uiso calc 1 . .
C C14 0.53061(12) 0.29977(16) 0.3857(3) 0.0378(5) Uani d 1 . .
H H141 0.500106 0.242594 0.333566 0.057 Uiso calc 1 . .
H H142 0.523598 0.304973 0.523192 0.057 Uiso calc 1 . .
H H143 0.584979 0.288096 0.362658 0.057 Uiso calc 1 . .
N N2 0.16413(8) 0.52742(11) 0.3611(2) 0.0243(3) Uani d 1 . .
N N3 0.08860(8) 0.54126(11) 0.4001(2) 0.0247(3) Uani d 1 . .
H H3 0.061443 0.485415 0.415974 0.030 Uiso calc 1 . .
C C4 0.05078(10) 0.63117(13) 0.4170(2) 0.0229(4) Uani d 1 . .
O O4 -0.01768(7) 0.63137(10) 0.46053(18) 0.0272(3) Uani d 1 . .
C C5 0.06606(9) 0.82347(13) 0.3958(2) 0.0219(4) Uani d 1 . .
C C51 -0.01659(9) 0.84556(14) 0.4338(3) 0.0261(4) Uani d 1 . .
H H511 -0.029101 0.816888 0.557765 0.039 Uiso calc 1 . .
H H512 -0.049690 0.814526 0.333548 0.039 Uiso calc 1 . .
H H513 -0.024832 0.919671 0.434967 0.039 Uiso calc 1 . .
N N6 0.11052(8) 0.90527(11) 0.37439(19) 0.0231(3) Uani d 1 . .
C C7 0.18631(9) 0.89387(13) 0.3400(2) 0.0215(3) Uani d 1 . .
C C71 0.23023(10) 0.99101(14) 0.3237(2) 0.0233(4) Uani d 1 . .
C C72 0.19108(11) 1.08301(14) 0.2915(3) 0.0304(4) Uani d 1 . .
H H72 0.136623 1.083014 0.279027 0.036 Uiso calc 1 . .
C C73 0.23094(11) 1.17437(16) 0.2777(3) 0.0368(5) Uani d 1 . .
H H73 0.203789 1.236386 0.254404 0.044 Uiso calc 1 . .
C C74 0.31059(11) 1.17518(15) 0.2979(3) 0.0326(4) Uani d 1 . .
H H74 0.337833 1.237841 0.290086 0.039 Uiso calc 1 . .
C C75 0.35012(10) 1.08475(14) 0.3293(3) 0.0278(4) Uani d 1 . .
H H75 0.404570 1.085344 0.342154 0.033 Uiso calc 1 . .
C C76 0.31046(10) 0.99282(14) 0.3420(2) 0.0250(4) Uani d 1 . .
H H76 0.338009 0.930930 0.363338 0.030 Uiso calc 1 . .
C C8 0.21977(10) 0.79844(13) 0.3214(2) 0.0230(4) Uani d 1 . .
H H8 0.272420 0.792202 0.293389 0.028 Uiso calc 1 . .
C C9 0.17444(9) 0.71166(13) 0.3448(2) 0.0217(3) Uani d 1 . .
C C10 0.09629(9) 0.72315(13) 0.3834(2) 0.0213(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
C1 0.0225(9) 0.0251(9) 0.0215(8) -0.0003(7) 0.0032(6) -0.0002(7)
O1 0.0230(6) 0.0202(6) 0.0326(7) 0.0016(5) 0.0061(5) 0.0010(5)
C11 0.0275(9) 0.0201(9) 0.0253(8) 0.0020(7) 0.0050(6) 0.0017(7)
C12 0.0276(9) 0.0209(8) 0.0235(8) -0.0005(7) 0.0036(6) -0.0029(7)
O12 0.0272(7) 0.0242(7) 0.0380(7) -0.0034(5) 0.0065(5) 0.0023(5)
O13 0.0260(7) 0.0225(7) 0.0359(7) 0.0023(5) 0.0080(5) 0.0033(5)
C13 0.0238(9) 0.0273(10) 0.0358(10) 0.0027(7) 0.0062(7) -0.0001(8)
C14 0.0372(11) 0.0323(11) 0.0442(11) 0.0073(9) 0.0057(8) 0.0005(9)
N2 0.0241(7) 0.0234(8) 0.0257(7) 0.0004(6) 0.0045(5) -0.0003(6)
N3 0.0237(8) 0.0202(7) 0.0308(8) -0.0035(6) 0.0067(6) -0.0005(6)
C4 0.0252(9) 0.0221(9) 0.0214(8) -0.0003(7) 0.0018(6) 0.0001(6)
O4 0.0235(6) 0.0242(6) 0.0343(7) -0.0015(5) 0.0066(5) 0.0017(5)
C5 0.0224(8) 0.0232(9) 0.0203(8) -0.0021(7) 0.0025(6) -0.0012(6)
C51 0.0238(9) 0.0233(9) 0.0315(9) 0.0005(7) 0.0054(7) -0.0006(7)
N6 0.0246(7) 0.0215(7) 0.0236(7) -0.0007(6) 0.0037(5) -0.0008(6)
C7 0.0232(8) 0.0226(9) 0.0187(8) -0.0022(7) 0.0016(6) -0.0002(6)
C71 0.0256(9) 0.0240(9) 0.0206(8) -0.0022(7) 0.0038(6) -0.0012(7)
C72 0.0256(9) 0.0257(10) 0.0402(10) -0.0009(7) 0.0052(7) -0.0001(8)
C73 0.0329(11) 0.0230(10) 0.0546(13) 0.0006(8) 0.0042(9) 0.0016(9)
C74 0.0326(10) 0.0239(10) 0.0415(11) -0.0085(7) 0.0049(8) -0.0012(8)
C75 0.0242(9) 0.0305(10) 0.0289(9) -0.0038(7) 0.0042(7) -0.0009(7)
C76 0.0254(9) 0.0254(9) 0.0244(8) -0.0010(7) 0.0025(6) -0.0011(7)
C8 0.0204(8) 0.0252(9) 0.0235(8) -0.0007(7) 0.0034(6) 0.0000(7)
C9 0.0241(8) 0.0215(9) 0.0197(7) -0.0002(7) 0.0018(6) -0.0007(6)
C10 0.0236(8) 0.0219(9) 0.0186(7) -0.0017(7) 0.0017(6) 0.0003(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_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
N2 C1 O1 . . 119.35(16) ?
N2 C1 C9 . . 124.47(15) ?
O1 C1 C9 . . 116.16(15) ?
C1 O1 C11 . . 113.92(13) ?
O1 C11 C12 . . 107.68(14) ?
O1 C11 H111 . . 110.2 ?
C12 C11 H111 . . 110.2 ?
O1 C11 H112 . . 110.2 ?
C12 C11 H112 . . 110.2 ?
H111 C11 H112 . . 108.5 ?
O12 C12 O13 . . 124.33(16) ?
O12 C12 C11 . . 126.99(16) ?
O13 C12 C11 . . 108.68(14) ?
C12 O13 C13 . . 116.01(13) ?
O13 C13 C14 . . 106.99(15) ?
O13 C13 H131 . . 110.3 ?
C14 C13 H131 . . 110.3 ?
O13 C13 H132 . . 110.3 ?
C14 C13 H132 . . 110.3 ?
H131 C13 H132 . . 108.6 ?
C13 C14 H141 . . 109.5 ?
C13 C14 H142 . . 109.5 ?
H141 C14 H142 . . 109.5 ?
C13 C14 H143 . . 109.5 ?
H141 C14 H143 . . 109.5 ?
H142 C14 H143 . . 109.5 ?
C1 N2 N3 . . 116.83(15) ?
C4 N3 N2 . . 127.43(14) ?
C4 N3 H3 . . 116.3 ?
N2 N3 H3 . . 116.3 ?
O4 C4 N3 . . 119.87(16) ?
O4 C4 C10 . . 124.68(16) ?
N3 C4 C10 . . 115.45(15) ?
N6 C5 C10 . . 121.09(15) ?
N6 C5 C51 . . 115.55(15) ?
C10 C5 C51 . . 123.36(15) ?
C5 C51 H511 . . 109.5 ?
C5 C51 H512 . . 109.5 ?
H511 C51 H512 . . 109.5 ?
C5 C51 H513 . . 109.5 ?
H511 C51 H513 . . 109.5 ?
H512 C51 H513 . . 109.5 ?
C5 N6 C7 . . 120.34(15) ?
N6 C7 C8 . . 122.05(15) ?
N6 C7 C71 . . 115.20(15) ?
C8 C7 C71 . . 122.75(15) ?
C72 C71 C76 . . 118.69(16) ?
C72 C71 C7 . . 119.84(15) ?
C76 C71 C7 . . 121.47(16) ?
C73 C72 C71 . . 120.68(17) ?
C73 C72 H72 . . 119.7 ?
C71 C72 H72 . . 119.7 ?
C72 C73 C74 . . 120.02(18) ?
C72 C73 H73 . . 120.0 ?
C74 C73 H73 . . 120.0 ?
C75 C74 C73 . . 119.96(17) ?
C75 C74 H74 . . 120.0 ?
C73 C74 H74 . . 120.0 ?
C74 C75 C76 . . 120.26(17) ?
C74 C75 H75 . . 119.9 ?
C76 C75 H75 . . 119.9 ?
C75 C76 C71 . . 120.39(17) ?
C75 C76 H76 . . 119.8 ?
C71 C76 H76 . . 119.8 ?
C7 C8 C9 . . 118.59(15) ?
C7 C8 H8 . . 120.7 ?
C9 C8 H8 . . 120.7 ?
C8 C9 C10 . . 119.50(16) ?
C8 C9 C1 . . 123.25(15) ?
C10 C9 C1 . . 117.24(15) ?
C9 C10 C5 . . 118.40(15) ?
C9 C10 C4 . . 118.54(15) ?
C5 C10 C4 . . 123.01(15) ?
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 N2 . 1.283(2) ?
C1 O1 . 1.3565(19) ?
C1 C9 . 1.450(2) ?
O1 C11 . 1.434(2) ?
C11 C12 . 1.505(2) ?
C11 H111 . 0.9900 ?
C11 H112 . 0.9900 ?
C12 O12 . 1.201(2) ?
C12 O13 . 1.338(2) ?
O13 C13 . 1.456(2) ?
C13 C14 . 1.501(3) ?
C13 H131 . 0.9900 ?
C13 H132 . 0.9900 ?
C14 H141 . 0.9800 ?
C14 H142 . 0.9800 ?
C14 H143 . 0.9800 ?
N2 N3 . 1.368(2) ?
N3 C4 . 1.356(2) ?
N3 H3 . 0.8800 ?
C4 O4 . 1.244(2) ?
C4 C10 . 1.465(2) ?
C5 N6 . 1.333(2) ?
C5 C10 . 1.418(2) ?
C5 C51 . 1.504(2) ?
C51 H511 . 0.9800 ?
C51 H512 . 0.9800 ?
C51 H513 . 0.9800 ?
N6 C7 . 1.361(2) ?
C7 C8 . 1.386(2) ?
C7 C71 . 1.490(2) ?
C71 C72 . 1.397(2) ?
C71 C76 . 1.400(2) ?
C72 C73 . 1.388(3) ?
C72 H72 . 0.9500 ?
C73 C74 . 1.390(3) ?
C73 H73 . 0.9500 ?
C74 C75 . 1.382(3) ?
C74 H74 . 0.9500 ?
C75 C76 . 1.392(2) ?
C75 H75 . 0.9500 ?
C76 H76 . 0.9500 ?
C8 C9 . 1.397(2) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.408(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
N3 H3 O4 3_566 0.88 1.93 2.7717(19) 159.9 yes
C14 H141 O12 2_645 0.98 2.63 3.190(2) 116.2 yes
C14 H142 O12 3_666 0.98 2.65 3.411(3) 134.7 yes
C13 H132 O12 3_665 0.99 2.80 3.746(2) 160.6 yes
C51 H512 O4 4_575 0.98 2.79 3.335(2) 115.8 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 C1 O1 C11 . . . . -5.8(2) ?
C9 C1 O1 C11 . . . . 172.95(14) ?
C1 O1 C11 C12 . . . . -179.80(13) ?
O1 C11 C12 O12 . . . . -13.6(2) ?
O1 C11 C12 O13 . . . . 167.01(13) ?
O12 C12 O13 C13 . . . . -1.0(2) ?
C11 C12 O13 C13 . . . . 178.39(13) ?
C12 O13 C13 C14 . . . . 171.25(15) ?
O1 C1 N2 N3 . . . . 178.51(13) ?
C9 C1 N2 N3 . . . . -0.1(2) ?
C1 N2 N3 C4 . . . . -0.8(2) ?
N2 N3 C4 O4 . . . . -177.17(15) ?
N2 N3 C4 C10 . . . . 2.1(2) ?
C10 C5 N6 C7 . . . . 0.0(2) ?
C51 C5 N6 C7 . . . . 179.79(14) ?
C5 N6 C7 C8 . . . . 1.6(2) ?
C5 N6 C7 C71 . . . . -178.54(14) ?
N6 C7 C71 C72 . . . . -17.4(2) ?
C8 C7 C71 C72 . . . . 162.49(16) ?
N6 C7 C71 C76 . . . . 161.87(15) ?
C8 C7 C71 C76 . . . . -18.2(2) ?
C76 C71 C72 C73 . . . . 0.1(3) ?
C7 C71 C72 C73 . . . . 179.41(17) ?
C71 C72 C73 C74 . . . . -0.7(3) ?
C72 C73 C74 C75 . . . . 0.8(3) ?
C73 C74 C75 C76 . . . . -0.4(3) ?
C74 C75 C76 C71 . . . . -0.2(3) ?
C72 C71 C76 C75 . . . . 0.3(2) ?
C7 C71 C76 C75 . . . . -178.98(15) ?
N6 C7 C8 C9 . . . . -2.0(2) ?
C71 C7 C8 C9 . . . . 178.07(15) ?
C7 C8 C9 C10 . . . . 1.0(2) ?
C7 C8 C9 C1 . . . . -177.68(15) ?
N2 C1 C9 C8 . . . . 178.16(16) ?
O1 C1 C9 C8 . . . . -0.5(2) ?
N2 C1 C9 C10 . . . . -0.5(2) ?
O1 C1 C9 C10 . . . . -179.14(13) ?
C8 C9 C10 C5 . . . . 0.5(2) ?
C1 C9 C10 C5 . . . . 179.22(14) ?
C8 C9 C10 C4 . . . . -176.93(14) ?
C1 C9 C10 C4 . . . . 1.8(2) ?
N6 C5 C10 C9 . . . . -1.0(2) ?
C51 C5 C10 C9 . . . . 179.22(14) ?
N6 C5 C10 C4 . . . . 176.29(15) ?
C51 C5 C10 C4 . . . . -3.5(2) ?
O4 C4 C10 C9 . . . . 176.72(15) ?
N3 C4 C10 C9 . . . . -2.5(2) ?
O4 C4 C10 C5 . . . . -0.6(3) ?
N3 C4 C10 C5 . . . . -179.77(15) ?