#------------------------------------------------------------------------------
#$Date: 2021-12-15 05:07:16 +0200 (Wed, 15 Dec 2021) $
#$Revision: 271436 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243946.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_2243946
loop_
_publ_author_name
'Pirnazarova, Nasiba'
'Yakubov, Ubaydullo'
'Allabergenova, Sevara'
'Tojiboev, Akmaljon'
'Turgunov, Kambarali'
'Elmuradov, Burkhon'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
3-methyl-4-oxo-N-phenyl-3,4-dihydroquinazoline-2-carbothioamide
;
_journal_coeditor_code WM5629
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021013116
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C16 H13 N3 O S'
_chemical_formula_moiety 'C16 H13 N3 O S'
_chemical_formula_sum 'C16 H13 N3 O S'
_chemical_formula_weight 295.35
_chemical_name_systematic
;
3-Methyl-4-oxo-N-phenyl-3,4-dihydroquinazoline-2-carbothioamide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 110.646(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 11.7685(3)
_cell_length_b 16.3641(3)
_cell_length_c 16.3798(3)
_cell_measurement_reflns_used 9141
_cell_measurement_temperature 566(2)
_cell_measurement_theta_max 71.1000
_cell_measurement_theta_min 2.6930
_cell_volume 2951.85(11)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020), Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 566(2)
_diffrn_detector_area_resol_mean 10.00000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0216
_diffrn_reflns_av_unetI/netI 0.0217
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 16801
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.415
_diffrn_reflns_theta_min 3.952
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.962
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.63892
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.329
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1232
_exptl_crystal_size_max 0.250
_exptl_crystal_size_mid 0.230
_exptl_crystal_size_min 0.200
_refine_diff_density_max 0.324
_refine_diff_density_min -0.425
_refine_ls_extinction_coef 0.00124(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 390
_refine_ls_number_reflns 5685
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.057
_refine_ls_R_factor_all 0.0496
_refine_ls_R_factor_gt 0.0424
_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^)+(0.0602P)^2^+0.6163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1153
_refine_ls_wR_factor_ref 0.1209
_reflns_number_gt 4788
_reflns_number_total 5685
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5629sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2243946
_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 0.640
_shelx_estimated_absorpt_t_max 0.695
_shelx_hkl_file
;
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0 0 1 8.30107 2.04247 8
0 0 -1 25.2393 2.59336 10
0 0 2 77436.5 1608.71 36
0 0 2 76494.7 1605.51 35
0 0 -2 89902.9 1599.92 9
0 0 -2 92575.4 1604.36 10
0 0 3-0.96438 5.67782 36
0 0 3 3.32047 4.47738 35
0 0 -3 9.38785 4.84677 10
0 0 4 50312.0 994.292 12
0 0 4 50519.7 985.898 35
0 0 4 52523.7 992.222 36
0 0 -4 51011.5 976.456 10
0 0 5 16.0520 10.4588 36
0 0 5 1.41989 8.35653 35
0 0 5 15.9115 9.71005 12
0 0 6 1425.05 66.3257 12
0 0 6 1421.80 61.8613 7
0 0 6 1477.68 61.4171 35
0 0 6 1501.70 65.3118 36
0 0 -6 1368.53 69.4000 31
0 0 7 15.6057 12.2942 12
0 0 7-2.10595 10.4408 35
0 0 7 21.7075 11.2403 7
0 0 -7 11.7055 14.1737 31
0 0 -8 22777.5 531.819 31
0 0 8 24016.5 527.292 12
0 0 9 3.63103 17.1616 12
0 0 -9 3.90942 16.5266 31
0 0 10 3886.05 156.837 12
0 0 10 3781.44 155.251 18
0 0 10 3996.54 160.909 17
0 0 11 4.79762 20.2818 12
0 0 11 4.82383 19.0757 18
0 0 11 19.5294 19.3071 17
0 0 12 48.7591 30.8590 12
0 0 12 85.4873 32.4619 18
0 0 12 70.5925 32.4882 17
0 0 13 5.84708 25.4794 12
0 0 13-5.74041 25.7397 18
0 0 13 35.1175 24.7434 17
0 0 14 200.918 47.6855 18
0 0 14 169.071 44.3446 17
0 0 15 5.85439 24.7510 23
0 0 15 63.3544 31.6301 18
0 0 15 5.86205 23.9966 17
0 0 16 90.2923 33.7212 17
0 0 17 4.47832 21.1661 17
0 0 18 745.853 59.9365 22
0 0 18 721.995 57.7483 17
0 -1 0 18.5952 2.94323 10
0 1 0 16.5092 2.35480 8
0 -1 -1 15632.9 303.962 10
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0 -1 1 15704.6 296.514 11
0 1 1 14877.9 302.805 8
0 -1 -1 15892.1 303.458 9
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0 -1 -2 10279.0 203.739 9
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0 -1 -2 10092.1 206.018 10
0 1 3 7057.27 150.483 34
0 -1 -3 7200.05 154.959 9
0 -1 -3 7338.75 159.486 10
0 -1 3 6979.88 153.189 7
0 1 4 52280.6 1020.51 12
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0 1 4 53701.8 1015.18 35
0 -1 -4 51941.7 1012.54 10
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0 -1 4 51477.1 1008.27 7
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0 -1 5 82452.4 1615.85 7
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0 1 6 4728.56 139.469 12
0 1 -6 4672.83 141.149 31
0 1 6 4704.03 137.196 36
0 1 6 4617.16 131.363 35
0 -1 6 4468.18 126.013 7
0 1 7 520.451 42.4334 12
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0 -1 -7 496.888 46.6633 31
0 1 7 662.160 42.6686 35
0 1 -7 522.682 43.5689 31
0 1 7 544.284 41.7875 36
0 1 7 500.293 39.5768 7
0 1 8 1716.13 85.5085 12
0 -1 8 1697.66 85.5709 12
0 1 8 1558.01 77.7393 7
0 -1 -8 1621.61 90.7347 31
0 1 8 1644.89 80.5519 36
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0 -1 -9 42.3617 20.0237 31
0 -1 9 29.2283 17.6968 12
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0 -1 10 46.3878 23.1646 12
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0 1 12 12038.6 356.290 12
0 -1 12 12071.2 357.539 12
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0 1 13 2882.37 152.089 12
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-10 3 17 133.515 28.1083 21
-10 -3 16 507.660 54.8814 25
-10 -3 16 512.510 54.2789 24
-10 3 16 468.159 52.1446 24
-10 3 16 459.230 51.4931 21
-10 -3 15-14.2696 28.4370 24
-10 3 15-23.2796 23.5989 24
-10 -3 15 18.9488 26.0149 25
-10 -3 14 182.819 41.4503 25
-10 3 13 10.5917 22.3874 30
-10 -3 13-5.32270 26.3847 30
-10 -3 13-16.6905 28.1982 25
-10 3 12 193.836 41.5926 30
-10 -3 12 223.378 45.9022 30
-10 -3 12 260.385 49.8519 25
-10 3 11 4446.57 193.022 30
-10 -3 11 4693.89 199.153 30
10 -3 -11 5045.20 232.125 1
-10 3 10 514.568 62.1722 30
-10 -3 10 456.402 60.3522 30
10 -3 -10 463.666 74.5988 1
-10 -3 9 658.229 71.2248 32
10 -3 -9 639.041 87.5192 1
10 -3 -8 3294.42 183.656 1
10 -3 -7 11397.9 377.467 1
-10 -3 7 11178.9 343.240 28
10 -3 -6 1088.90 105.143 1
-10 -3 6 1010.33 87.3284 28
10 -3 -5 1521.43 123.542 1
-10 -3 5 1548.48 107.175 28
-10 -3 4 4124.45 180.561 28
10 3 -4 4004.76 207.863 1
10 -3 -4 4286.82 209.523 1
-10 -3 3 10413.2 316.651 28
10 3 -3 9372.12 347.450 1
10 -3 -3 9895.18 347.755 1
-10 -3 2 1457.53 101.089 28
10 3 -2 1409.03 122.926 1
10 -3 -2 1286.89 114.242 1
10 -3 -1 180.326 55.6952 1
10 3 -1 168.661 53.1233 1
-10 -3 1 205.678 42.9497 28
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10 3 0 1036.90 108.345 1
10 -3 0 997.908 104.148 1
-10 -3 -1 2905.12 144.534 28
10 3 1 2805.01 175.045 1
10 3 2 161.736 57.0560 1
10 3 3 255.464 66.5276 1
10 3 4 781.162 89.0787 1
10 -3 4 756.579 80.6225 2
10 3 4 840.161 84.6922 2
10 -3 5 493.912 62.3332 2
10 3 5 478.833 68.1195 1
10 3 5 414.558 60.0202 2
10 3 6 184.562 43.8580 1
10 -3 6 130.060 36.7949 2
10 3 6 131.788 35.3771 2
10 -3 6 103.510 31.6436 18
10 -3 7 7.13780 21.3403 2
10 3 7 36.1390 22.5991 2
10 -3 7 25.0377 20.7087 18
10 3 8 93.7935 21.8985 17
10 -3 8 97.6371 22.6771 17
10 -3 8 97.8546 21.6757 18
-10 -4 17 9.31656 19.9646 25
-10 -4 16 625.737 58.6005 25
-10 -4 16 514.592 52.4510 24
10 -4 -15 211.027 47.0118 1
-10 -4 15 271.056 44.0889 24
-10 -4 15 276.487 43.8982 25
-10 -4 14 19.8087 22.8131 24
-10 -4 14-10.0488 21.8938 25
-10 4 13 59.3409 27.1578 30
-10 -4 13 4.99725 25.8750 30
-10 -4 13 5.40007 22.8304 25
-10 -4 12 18231.7 477.179 25
-10 4 12 16897.7 458.414 30
-10 -4 12 17538.1 463.411 30
-10 4 11 5.38391 27.2880 30
-10 -4 11 5.45151 27.0233 30
-10 -4 11 5.20133 23.9609 32
-10 -4 10 145.218 40.2323 32
-10 4 10 97.5105 33.9172 30
-10 -4 10 71.4708 34.4199 30
10 -4 -10 68.1448 47.3739 1
-10 -4 9 4890.93 203.678 32
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-10 -4 9 5451.03 212.538 30
10 -4 -9 5192.39 236.804 1
10 -4 -8 926.287 100.555 1
10 -4 -7 526.968 76.5176 1
-10 -4 7 597.797 69.5328 28
10 -4 -6 5834.82 248.280 1
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10 -4 -5 420.047 70.1322 1
-10 -4 5 749.542 74.2756 28
10 -4 -4 529.173 77.1883 1
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10 -4 -3 94.5470 42.8710 1
10 4 -3 197.644 54.2073 1
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-10 -4 2 699.555 72.5554 28
10 -4 -2 636.978 84.6288 1
10 4 -2 669.269 90.3819 1
10 -4 -1 80.1543 41.5145 1
10 4 -1 103.835 50.6838 1
-10 -4 1 116.969 34.3771 28
10 4 0 15.8807 38.4634 1
-10 -4 0 60.6364 31.9185 28
10 4 1 187.091 60.0319 1
-10 -4 -1 118.904 36.2155 28
-10 -4 -2 3990.01 173.463 28
10 4 2 3941.43 204.020 1
-10 -4 -3 177.423 37.3351 28
10 4 3 162.880 51.9521 1
10 4 4 1610.21 120.399 1
10 -4 4 1259.88 98.7924 2
10 4 4 1424.62 104.344 2
10 4 5 62.3943 33.9243 1
10 -4 5 43.3357 30.1209 2
10 -4 6 387.407 48.0346 2
10 -4 6 330.546 47.2851 18
10 -4 7 3.47515 16.8304 18
10 -4 8 59.5347 18.3847 18
-10 -5 17 8.20619 15.8347 25
10 -5 -16 518.369 60.0383 1
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-10 -5 15 666.853 62.9757 25
-10 -5 14 292.402 46.2744 25
-10 -5 13 123.122 33.4893 25
-10 -5 13 106.457 31.7729 32
-10 -5 12 907.285 78.7582 32
-10 -5 12 1018.14 86.2379 25
-10 -5 11 2724.15 141.514 32
-10 -5 10 2483.38 135.628 32
10 -5 -10 2417.25 159.858 1
-10 -5 9 83.6454 32.8513 32
10 -5 -9 89.2500 45.1817 1
-10 -5 8 16.9525 28.0113 32
10 -5 -8-7.35621 43.2856 1
10 -5 -7 5187.44 233.202 1
-10 -5 7 5123.71 209.827 28
10 -5 -6 446.480 71.4209 1
-10 -5 6 404.135 60.2970 28
10 -5 -5 557.960 76.3198 1
-10 -5 5 563.957 67.4390 28
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10 -5 -4 1246.58 110.911 1
-10 -5 3 656.708 70.5317 28
10 -5 -3 560.565 77.3247 1
-10 -5 2 1611.93 110.983 28
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10 5 -1 526.640 81.0229 1
-10 -5 0 2705.64 142.669 28
10 5 0 2497.28 162.778 1
-10 -5 -1 4064.03 176.431 28
10 5 1 3670.93 197.101 1
10 5 2 43.3021 41.1010 1
-10 -5 -2 104.996 33.7815 28
10 5 3 121.222 47.7850 1
-10 -5 -3 98.7915 32.2406 28
-10 -5 -4 1081.28 79.8242 28
10 5 4 873.908 90.2321 1
-10 -5 -5 275.714 40.1517 28
10 5 5 165.720 45.3960 1
10 -5 6 4.17503 22.4986 18
10 -5 7 84.4061 24.3111 18
10 -6 -17 54.2027 23.1230 1
-10 -6 16 257.148 35.6893 25
10 -6 -16 187.899 38.8660 1
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-10 -6 14 241.723 40.5601 25
-10 -6 14 261.197 41.8574 32
-10 -6 13-9.52959 26.1659 25
-10 -6 13 9.12571 22.6181 32
-10 -6 12 700.942 67.8400 32
-10 -6 12 572.283 63.8418 25
-10 -6 11 323.249 52.6188 32
-10 -6 10 467.034 61.0914 32
10 -6 -10 467.700 78.4851 1
-10 -6 9 2232.68 129.366 32
10 -6 -9 2135.79 146.797 1
-10 -6 8 2629.95 141.530 32
10 -6 -8 2412.69 155.001 1
-10 -6 7 1028.60 88.5287 28
10 -6 -7 1127.23 106.090 1
-10 -6 6 523.554 66.5962 28
10 -6 -6 388.135 67.6609 1
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10 -6 -5 977.247 98.1181 1
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10 -6 -4 338.354 62.7356 1
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-10 -6 1 669.402 72.0270 28
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10 6 0 216.392 57.5574 1
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10 6 1 548.747 77.6535 1
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10 6 2 246.028 56.6176 1
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10 6 3 50.3466 39.9403 1
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10 6 4 5.66198 29.9205 1
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10 -6 6 84.0194 27.4013 18
10 -6 7 11.5784 15.8971 18
10 -7 -16 670.420 62.5158 1
10 -7 -15 78.4438 35.1529 1
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-10 -7 12 28.7002 22.6093 32
-10 -7 11 294.855 49.6855 32
-10 -7 11 433.779 56.4050 25
-10 -7 10 638.567 68.9327 32
10 -7 -10 596.082 82.3427 1
-10 -7 9 170.388 41.1876 32
10 -7 -9 154.556 48.2133 1
-10 -7 8-5.61489 29.6703 32
10 -7 -8-6.97705 33.7903 1
-10 -7 7 3931.00 173.530 28
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10 -7 -7 3420.31 181.459 1
-10 -7 6 186.044 42.6935 28
10 -7 -6 190.310 49.3691 1
-10 -7 5 493.554 62.9825 28
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10 7 2 521.400 71.7271 1
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10 7 3 500.639 67.2774 1
-10 -7 -4 153.724 33.8483 28
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10 -7 6 16.6678 19.9323 18
-10 -7 -6 20.1037 15.4805 28
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10 -8 -16 101.594 27.5652 1
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10 -8 -15 1970.77 109.069 1
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10 -8 -14 15.3194 27.5336 1
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-10 -8 12 1009.06 77.4752 32
-10 -8 11 19.4465 27.1905 32
10 -8 -11 25.6949 31.8451 1
-10 -8 10-15.3126 29.5470 32
10 -8 -10-13.1482 35.4277 1
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10 -8 -9 536.584 73.9181 1
-10 -8 8 261.063 48.6419 32
10 -8 -8 217.746 53.7526 1
-10 -8 7 1194.13 93.6244 32
-10 -8 7 1215.63 92.6583 28
-10 -8 6 3445.62 162.566 32
-10 -8 6 3150.88 154.468 28
-10 -8 5 460.456 61.3628 28
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10 -8 5 160.353 30.7735 26
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10 -8 5 128.425 29.5892 18
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10 -8 6 87.3055 22.7885 18
10 -9 -15 697.623 60.8255 1
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10 -9 -14-11.4064 21.6389 3
10 -9 -14 22.0152 26.3230 1
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10 -9 -13 105.144 32.4487 3
10 -9 -13 95.2441 34.7759 1
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10 -9 -12 1919.93 121.253 1
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10 -9 -11 1457.48 108.353 1
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-10 -9 10 212.515 41.6324 20
10 -9 -10 191.098 47.3819 1
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-10 -9 9 812.918 76.0701 20
-10 -9 9 852.995 75.7575 32
10 -9 -9 804.870 83.5796 1
-10 -9 8 2573.37 134.632 32
-10 9 7 3519.24 154.094 29
-10 -9 7 4062.85 173.707 32
-10 -9 6 363.659 53.9346 32
-10 -9 6 433.158 56.8166 28
-10 -9 5 1891.07 113.903 32
-10 -9 5 1647.87 106.838 28
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10 -9 4 27.9211 19.1775 26
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10 -9 5 17.0613 17.0009 18
10 -10 -14 49.1358 21.6648 3
10 -10 -14 96.0112 26.8745 1
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10 -10 -13 4.17775 23.7800 1
10 -10 -13 23.4299 22.9813 3
-10 -10 13 36.0588 20.2047 32
10 -10 -12 348.827 49.2731 3
10 -10 -12 450.886 57.1304 1
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10 -10 -11 94.5703 34.9246 1
10 -10 -11 67.4675 30.1675 3
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-10 -10 10 46.7380 25.0243 20
10 -10 -10 56.4090 32.0803 3
-10 -10 10 69.4673 26.3803 32
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-10 10 8 3171.23 139.796 29
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-10 10 7 674.605 63.1016 29
-10 -10 7 761.557 75.9780 20
-10 -10 6 62.5531 28.7827 32
-10 10 6 92.2930 28.2690 29
-10 -10 6 10.9233 25.1783 20
-10 -10 5 1919.35 111.209 32
-10 -10 5 1856.73 116.418 20
-10 -10 4 1678.59 102.730 28
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-10 -10 3 459.715 56.0123 28
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-10 -10 2-4.69560 24.3113 28
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10 -10 2 899.498 74.7460 26
10 -10 3 47.4407 25.3078 26
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10 -10 4 61.1414 22.4689 26
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10 -11 -13 157.763 30.0318 3
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10 -11 -12 34.5872 23.3402 3
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10 -11 -11 235.933 40.2928 3
-10 -11 11 247.758 37.1545 32
-10 -11 10 18.2729 20.0697 20
10 -11 -10-9.27697 25.4727 3
-10 -11 10 15.0878 18.6982 32
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10 -11 -9 1037.86 83.5710 3
-10 -11 9 1233.82 80.6422 32
-10 -11 8 1012.34 75.2745 32
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10 -11 -2 178.732 42.5372 26
10 -11 -1 155.995 40.1497 26
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10 -11 0 152.612 38.3637 26
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10 -11 1 24.7096 27.1848 26
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10 -11 2 213.651 36.8191 26
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10 -11 3 27.0005 19.8259 26
-10 -12 12-2.44231 14.6011 32
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-10 -12 8 85.9187 27.1080 20
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-10 12 5 1002.59 70.3536 29
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-10 12 4 58.5585 23.2285 29
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10 -12 -2 12.3982 23.5216 26
10 -12 -1 409.932 50.2980 26
10 -12 0 2221.31 109.149 26
10 -12 1 281.790 40.2984 26
10 -12 2 92.5339 25.2597 26
-10 13 10 2.13431 11.0503 29
-10 13 9-2.47725 12.8260 29
-10 -13 9-5.53951 15.7635 20
-10 13 8 407.952 39.7966 29
-10 -13 8 493.029 46.7758 20
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-10 13 5 451.496 44.6996 29
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-10 13 4 117.234 25.9326 29
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10 -13 -2 46.3668 22.1726 26
-10 13 1 121.995 24.3523 29
10 -13 -1 86.3609 26.0391 26
-10 13 0 339.859 33.9704 29
10 -13 0 283.263 36.1662 26
10 -13 1 747.473 52.5931 26
-10 14 8 108.366 19.6793 29
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-10 -14 7 57.1458 19.6319 20
-10 14 6 59.6055 18.1958 29
-10 -14 6 43.4130 19.0456 20
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-10 14 4 14.4699 14.1930 29
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-11 0 17 200.245 31.7639 24
-11 0 16-3.32127 17.1957 25
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-11 0 14-4.66459 22.0463 30
-11 0 14 4.42679 21.9436 25
-11 0 13 40.9145 25.3637 30
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11 0 -10 75.2440 49.0216 1
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11 0 -9 297.833 64.3001 1
11 0 -8 30.7610 40.6407 1
11 0 -7 6042.49 261.209 1
11 0 -6 411.919 76.5577 1
11 0 -5 5626.62 255.477 1
11 0 -4 7.84716 46.9135 1
11 0 -3 362.285 73.8198 1
11 0 -2-31.4778 45.5563 1
11 0 -1 4181.29 213.565 1
11 0 0 75.5725 57.0544 1
11 0 1 6079.26 255.140 1
11 0 2-13.2617 38.3837 1
11 0 3 2931.28 155.538 1
11 0 4 5.06009 29.2907 2
11 0 4 4.97403 28.7925 1
11 0 5 2042.76 110.585 2
11 0 6-6.58694 22.2874 2
-11 -1 17 327.351 36.1590 25
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-11 -1 16 599.478 53.0671 25
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-11 -1 15 174.152 36.6919 24
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-11 1 14 18.4118 23.8360 30
-11 -1 14 9.23585 21.8307 30
-11 -1 14 27.1960 22.9781 25
-11 1 14 46.3529 23.1453 25
-11 1 13 70.7544 31.1655 30
-11 -1 13 40.5667 30.3375 30
-11 -1 13 93.5030 35.2934 25
-11 1 13 54.9109 26.5132 25
-11 -1 12 621.172 66.2090 25
-11 1 12 597.419 66.7715 30
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11 -1 -11 1029.84 105.898 1
-11 1 11 1386.25 100.530 30
-11 -1 11 1224.37 95.2375 30
11 -1 -10 713.950 89.1565 1
-11 1 10 676.222 75.3120 30
-11 -1 10 828.009 78.9664 30
11 -1 -9 623.699 84.3427 1
11 -1 -8 91.7537 45.0245 1
11 1 -8 92.9823 45.6265 1
11 1 -7 2126.53 152.597 1
11 -1 -7 919.476 103.985 1
11 1 -6 2760.05 172.333 1
11 -1 -6 3006.57 178.133 1
-11 -1 6 2561.95 136.432 28
11 1 -5 12378.9 407.944 1
11 -1 -5 11950.4 399.510 1
-11 -1 5 12176.7 354.696 28
11 1 -4 410.527 76.0184 1
11 -1 -4 497.116 82.1081 1
11 -1 -3 116.824 48.7526 1
11 1 -3 142.691 59.8768 1
11 1 -2 7.90968 43.4359 1
11 -1 -2-7.76854 42.6608 1
11 1 -1 1124.37 114.983 1
11 -1 -1 1074.99 109.887 1
11 1 0 1972.48 145.015 1
11 -1 0 2075.13 145.797 1
11 1 1 577.852 86.4753 1
11 -1 1 401.095 70.7064 1
11 1 2-13.3970 36.7857 1
11 -1 2 51.6911 38.0211 1
11 1 3 1106.12 97.1657 1
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-13 -8 6 73.7720 20.3481 32
-13 -8 5 488.331 40.7076 20
-13 -8 5 642.718 46.5141 32
-13 -8 4 838.113 52.0218 32
-14 0 11 2.40831 13.4680 30
-14 0 10 164.397 27.3414 30
14 0 -9 3.93207 22.3817 1
-14 0 9-28.1505 19.0535 30
14 0 -8 2436.22 122.374 1
-14 0 8 3261.78 118.944 30
14 0 -7-8.36908 23.4017 1
-14 0 7 20.6305 15.8831 30
14 0 -6 62.0405 29.0519 1
-14 0 6 125.883 25.7645 30
14 0 -5 3.97735 26.5848 1
14 0 -4 2901.67 125.582 1
14 0 -3-3.35361 17.7212 1
-14 1 11 366.016 35.5908 30
-14 -1 11 387.530 36.0083 30
14 -1 -10 29.5929 22.1161 1
-14 1 10 10.3533 14.4769 30
-14 -1 10 10.4286 14.3194 30
14 -1 -9 163.312 36.6338 1
-14 1 9 184.404 29.4534 30
-14 -1 9 224.539 31.0752 30
14 1 -8 388.963 52.2330 1
14 -1 -8 385.200 49.0992 1
-14 1 8 381.622 40.4871 30
-14 -1 8 415.770 41.4250 30
14 1 -7 24.3862 25.0483 1
14 -1 -7 33.4676 26.1583 1
-14 1 7 17.3343 18.8243 30
-14 -1 7 8.72117 18.6908 30
14 1 -6 12.1104 25.9508 1
14 -1 -6 4.11553 23.8232 1
-14 1 6-20.0772 20.1070 30
-14 -1 6 2.88353 18.7860 30
14 -1 -5 410.054 50.2736 1
14 1 -5 315.482 45.3953 1
14 1 -4 109.626 35.6129 1
14 -1 -4 7.32487 24.7955 1
14 1 -3 3.30514 22.3662 1
14 -1 -3-9.82077 17.2985 1
14 -2 -10 131.681 32.9665 1
-14 2 10 176.870 25.9434 30
-14 -2 10 199.059 27.4380 30
-14 -2 10 184.714 26.9239 25
-14 2 9 1182.63 64.7487 30
-14 -2 9 1209.88 65.9262 30
-14 -2 8 340.819 37.3524 30
-14 2 8 266.334 34.2528 30
14 -2 -8 347.681 48.1181 1
-14 2 7 942.573 60.1341 30
-14 -2 7 1089.28 63.7423 30
-14 2 6 389.904 39.9799 30
-14 -2 6 459.654 42.2077 30
14 2 -6 330.735 44.5838 1
14 -2 -6 334.559 45.8910 1
-14 -2 5 52.3837 18.3545 32
14 2 -5 88.5034 28.3948 1
14 -2 -5 53.0531 27.1860 1
14 2 -4 387.279 44.6421 1
14 -2 -4 321.183 42.2563 1
14 2 -3 40.5747 21.8897 1
14 -2 -3 30.6764 19.4630 1
14 -3 -10 10.4588 20.5139 1
-14 -3 10-4.65596 12.7841 25
-14 3 9 146.013 24.5226 30
-14 -3 9 174.933 26.1055 30
14 -3 -9 104.257 31.1043 1
-14 3 8-9.68390 16.3829 30
-14 -3 8-2.46720 16.0733 30
14 -3 -8 34.5298 23.9880 1
-14 3 7 277.600 31.8046 30
-14 -3 7 379.852 37.3406 30
14 -3 -7 291.704 42.5582 1
-14 3 6 48.6852 17.8446 30
-14 -3 6 44.4868 19.3902 30
14 -3 -6 33.5998 24.6549 1
-14 -3 6 52.3702 17.4512 32
-14 3 5 268.181 30.2231 30
-14 -3 5 197.282 27.9411 30
14 -3 -5 200.488 34.5212 1
-14 -3 5 222.668 29.2745 32
14 -3 -4 79.6156 26.7627 1
-14 -3 4 91.0750 20.9017 32
-14 -4 9 1585.95 72.1938 25
14 -4 -9 1086.75 72.9338 1
-14 -4 8 1124.56 57.8598 32
14 -4 -8 912.479 67.4962 1
-14 -4 7 56.2834 17.8266 32
14 -4 -7 31.3900 23.0358 1
-14 -4 6 263.922 30.4994 32
14 -4 -6 265.056 37.6814 1
-14 -4 5 239.630 28.8183 32
0 0 0 0.00 0.00 0
TITL exp_137_ACP-8 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 11.768625 16.363891 16.379514 90.0000 110.6452 90.0000
ZERR 13.00 0.000251 0.000305 0.000312 0.0000 0.0023 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 143.00 130.00 13.00 13.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 53957
_shelx_res_file
;
TITL asr8.res in P2(1)/n
1.res
created by SHELXL-2018/3 at 07:49:42 on 12-Nov-2021
REM Old TITL exp_137_ACP-8 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.285, Rweak 0.066, Alpha 0.028
REM 1.143 for 222 systematic absences, Orientation as input
REM Formula found by SHELXT: C32 N6 O4
CELL 1.54184 11.7685 16.3641 16.3798 90 110.646 90
ZERR 8 0.0003 0.0003 0.0003 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O S
UNIT 128 104 24 8 8
ACTA
TEMP 293
SIZE 0.23 0.25 0.20
L.S. 4 0 0
PLAN 10
CONF
BOND
list 6
fmap 2 53
mpla N1A C2A N3A C4A C4A' C5A C6A C7A C8A C8A' O1A C9A C10A
mpla N1B C2B N3B C4B C4B' C5B C6B C7B C8B C8B' O1B C9B C10B
MORE -1
BOND $H
REM
REM
REM
REM #####
WGHT 0.060200 0.616300
EXTI 0.001236
FVAR 2.94788
S1A 5 0.467705 0.626489 0.890464 11.00000 0.05010 0.11320 =
0.05262 0.02201 0.01779 -0.00128
O1A 4 0.697658 0.593236 0.651545 11.00000 0.08516 0.05821 =
0.10945 -0.00771 0.06684 0.00799
N1A 3 0.487518 0.755269 0.721591 11.00000 0.04274 0.04785 =
0.05404 0.00254 0.02669 0.00153
N1B 3 0.227745 0.736986 0.572123 11.00000 0.05460 0.05076 =
0.04346 0.00072 0.02565 0.00334
S1B 5 0.042191 0.865966 0.636417 11.00000 0.05363 0.19355 =
0.05915 -0.02263 0.01654 0.03819
O1B 4 0.301207 0.907026 0.416995 11.00000 0.09073 0.05646 =
0.07735 0.00998 0.05129 -0.00401
C2A 1 0.490050 0.678015 0.738527 11.00000 0.03866 0.04756 =
0.04690 0.00019 0.02008 -0.00148
C2B 1 0.222795 0.814886 0.583758 11.00000 0.04226 0.05386 =
0.03803 -0.00233 0.01519 0.00379
N3A 3 0.559881 0.621759 0.716229 11.00000 0.04988 0.04221 =
0.06253 -0.00131 0.03044 -0.00135
N3B 3 0.249245 0.874025 0.534169 11.00000 0.04953 0.04433 =
0.04644 -0.00443 0.01949 -0.00045
C4A 1 0.637879 0.644704 0.672168 11.00000 0.05206 0.05194 =
0.06331 -0.00682 0.03327 -0.00198
C4B 1 0.280376 0.853680 0.461795 11.00000 0.04890 0.05033 =
0.04836 0.00020 0.02293 -0.00232
C4A' 1 0.638810 0.731614 0.654274 11.00000 0.04689 0.05115 =
0.05688 -0.00301 0.02903 -0.00345
C4B' 1 0.287024 0.766396 0.447188 11.00000 0.04446 0.04890 =
0.04251 -0.00300 0.01981 -0.00179
C5A 1 0.715016 0.763341 0.612893 11.00000 0.06458 0.06890 =
0.08549 0.00045 0.05131 -0.00230
AFIX 43
H5A 2 0.767186 0.728822 0.597752 11.00000 -1.20000
AFIX 0
C5B 1 0.319314 0.738047 0.377764 11.00000 0.06579 0.06486 =
0.05121 -0.00450 0.03350 0.00009
AFIX 43
H5B 2 0.336243 0.775028 0.340470 11.00000 -1.20000
AFIX 0
C6A 1 0.712785 0.845210 0.594689 11.00000 0.07043 0.07377 =
0.08993 0.00876 0.05111 -0.01282
AFIX 43
H6A 2 0.763410 0.866124 0.567158 11.00000 -1.20000
AFIX 0
C6B 1 0.325952 0.655899 0.364811 11.00000 0.08479 0.07341 =
0.06481 -0.01701 0.04287 0.00456
AFIX 43
H6B 2 0.347755 0.637057 0.318813 11.00000 -1.20000
AFIX 0
C7A 1 0.635342 0.896855 0.617189 11.00000 0.06994 0.05442 =
0.08429 0.01234 0.03713 -0.00779
AFIX 43
H7A 2 0.633301 0.952178 0.603750 11.00000 -1.20000
AFIX 0
C7B 1 0.300244 0.600601 0.420115 11.00000 0.09516 0.05192 =
0.08673 -0.01655 0.04757 0.00333
AFIX 43
H7B 2 0.304581 0.544836 0.410662 11.00000 -1.20000
AFIX 0
C8A 1 0.561541 0.867103 0.659163 11.00000 0.05796 0.04849 =
0.07329 0.00570 0.03388 0.00091
AFIX 43
H8A 2 0.510698 0.902433 0.674732 11.00000 -1.20000
AFIX 0
C8B 1 0.268437 0.627231 0.488717 11.00000 0.08570 0.04802 =
0.07145 -0.00128 0.04248 0.00143
AFIX 43
H8B 2 0.251967 0.589664 0.525684 11.00000 -1.20000
AFIX 0
C8A' 1 0.562612 0.783977 0.678534 11.00000 0.04088 0.04728 =
0.04981 0.00010 0.02217 -0.00280
C8B' 1 0.260942 0.711061 0.502701 11.00000 0.05043 0.04683 =
0.04421 -0.00175 0.02271 0.00168
C9A 1 0.555010 0.534290 0.734306 11.00000 0.08493 0.04440 =
0.09872 0.00249 0.05045 -0.00259
AFIX 137
H9AA 2 0.543485 0.503622 0.682028 11.00000 -1.50000
H9AB 2 0.488631 0.524014 0.754066 11.00000 -1.50000
H9AC 2 0.629728 0.517988 0.778655 11.00000 -1.50000
AFIX 0
C9B 1 0.241075 0.961669 0.551068 11.00000 0.08682 0.04604 =
0.06872 -0.01135 0.02700 0.00357
AFIX 137
H9BA 2 0.308740 0.989779 0.544197 11.00000 -1.50000
H9BB 2 0.242392 0.969168 0.609523 11.00000 -1.50000
H9BC 2 0.166757 0.983288 0.510518 11.00000 -1.50000
AFIX 0
C10A 1 0.408970 0.648856 0.786435 11.00000 0.04124 0.05134 =
0.05176 0.00513 0.02283 -0.00052
C10B 1 0.185309 0.842071 0.658645 11.00000 0.05009 0.06555 =
0.04351 -0.00627 0.02028 0.00818
N11A 3 0.292564 0.645975 0.735047 11.00000 0.04145 0.05608 =
0.04530 0.00996 0.02168 -0.00122
N11B 3 0.278991 0.842350 0.734043 11.00000 0.04754 0.05367 =
0.04153 -0.00449 0.02215 0.00713
H11A 2 0.270944 0.665685 0.681565 11.00000 0.05618
H11B 2 0.345320 0.821149 0.730841 11.00000 0.05957
C12A 1 0.191831 0.624176 0.760174 11.00000 0.03847 0.05335 =
0.05002 0.01409 0.02127 0.00321
C12B 1 0.286411 0.862103 0.820165 11.00000 0.05598 0.04625 =
0.04147 -0.00175 0.02413 0.00350
C13A 1 0.174300 0.658313 0.831988 11.00000 0.05699 0.05867 =
0.06842 0.00516 0.03484 0.00538
AFIX 43
H13A 2 0.231162 0.694273 0.868105 11.00000 -1.20000
AFIX 0
C13B 1 0.188894 0.880315 0.844674 11.00000 0.06187 0.07701 =
0.05200 -0.00440 0.02799 0.01442
AFIX 43
H13B 2 0.110617 0.880890 0.803547 11.00000 -1.20000
AFIX 0
C14A 1 0.071042 0.638230 0.849344 11.00000 0.06475 0.08075 =
0.07758 0.01543 0.04607 0.01503
AFIX 43
H14A 2 0.058768 0.660791 0.897690 11.00000 -1.20000
AFIX 0
C14B 1 0.208764 0.897849 0.931658 11.00000 0.08424 0.09098 =
0.05879 -0.00710 0.04265 0.01450
AFIX 43
H14B 2 0.143062 0.910500 0.948369 11.00000 -1.20000
AFIX 0
C15A 1 -0.013637 0.585499 0.796307 11.00000 0.05007 0.09498 =
0.08490 0.03035 0.03800 0.00723
AFIX 43
H15A 2 -0.083359 0.573110 0.808191 11.00000 -1.20000
AFIX 0
C15B 1 0.322954 0.896839 0.993009 11.00000 0.09556 0.08746 =
0.04611 -0.01089 0.03288 -0.00384
AFIX 43
H15B 2 0.335113 0.909440 1.050847 11.00000 -1.20000
AFIX 0
C16A 1 0.004992 0.551067 0.725555 11.00000 0.04862 0.08879 =
0.07418 0.01925 0.01867 -0.01367
AFIX 43
H16A 2 -0.051928 0.514896 0.689846 11.00000 -1.20000
AFIX 0
C16B 1 0.419371 0.877089 0.968521 11.00000 0.07360 0.11561 =
0.04732 -0.01263 0.01735 -0.00500
AFIX 43
H16B 2 0.497078 0.875101 1.010346 11.00000 -1.20000
AFIX 0
C17A 1 0.108453 0.570036 0.707122 11.00000 0.05075 0.07294 =
0.05205 0.00982 0.02035 -0.00690
AFIX 43
H17A 2 0.121368 0.546455 0.659469 11.00000 -1.20000
AFIX 0
C17B 1 0.402697 0.860094 0.882560 11.00000 0.05562 0.08835 =
0.04903 -0.00825 0.02066 0.00100
AFIX 43
H17B 2 0.468896 0.847365 0.866451 11.00000 -1.20000
REM #####
AFIX 0
HKLF 4
REM asr8.res in P2(1)/n
REM wR2 = 0.1209, GooF = S = 1.057, Restrained GooF = 1.057 for all data
REM R1 = 0.0424 for 4788 Fo > 4sig(Fo) and 0.0496 for all 5685 data
REM 390 parameters refined using 0 restraints
END
WGHT 0.0602 0.6162
REM Highest difference peak 0.324, deepest hole -0.425, 1-sigma level 0.037
Q1 1 0.0632 0.8136 0.6485 11.00000 0.05 0.32
Q2 1 0.0944 0.9008 0.6408 11.00000 0.05 0.29
Q3 1 0.6240 0.5995 0.6036 11.00000 0.05 0.25
Q4 1 0.4519 0.6635 0.7624 11.00000 0.05 0.18
Q5 1 0.6022 0.7593 0.6607 11.00000 0.05 0.17
Q6 1 0.3575 0.8988 0.8599 11.00000 0.05 0.15
Q7 1 0.1285 0.6205 0.7165 11.00000 0.05 0.15
Q8 1 0.2186 0.8443 0.5554 11.00000 0.05 0.15
Q9 1 0.1634 0.9600 0.5781 11.00000 0.05 0.15
Q10 1 0.2602 0.7405 0.4627 11.00000 0.05 0.15
;
_shelx_res_checksum 82559
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
S S1A 0.46771(5) 0.62649(4) 0.89046(3) 0.07206(19) Uani d 1 . .
O O1A 0.69766(15) 0.59324(9) 0.65155(11) 0.0755(4) Uani d 1 . .
N N1A 0.48752(12) 0.75527(8) 0.72159(9) 0.0456(3) Uani d 1 . .
N N1B 0.22774(13) 0.73699(9) 0.57212(9) 0.0474(3) Uani d 1 . .
S S1B 0.04219(5) 0.86597(6) 0.63642(4) 0.1030(3) Uani d 1 . .
O O1B 0.30121(15) 0.90703(8) 0.41700(10) 0.0690(4) Uani d 1 . .
C C2A 0.49005(14) 0.67801(10) 0.73853(10) 0.0430(4) Uani d 1 . .
C C2B 0.22279(15) 0.81489(10) 0.58376(10) 0.0444(4) Uani d 1 . .
N N3A 0.55988(13) 0.62176(8) 0.71623(10) 0.0487(3) Uani d 1 . .
N N3B 0.24924(13) 0.87402(8) 0.53417(9) 0.0461(3) Uani d 1 . .
C C4A 0.63788(17) 0.64470(11) 0.67217(12) 0.0523(4) Uani d 1 . .
C C4B 0.28038(16) 0.85368(11) 0.46179(11) 0.0476(4) Uani d 1 . .
C C4A' 0.63881(16) 0.73161(11) 0.65427(12) 0.0488(4) Uani d 1 . .
C C4B' 0.28702(15) 0.76640(10) 0.44719(10) 0.0441(4) Uani d 1 . .
C C5A 0.7150(2) 0.76334(13) 0.61289(15) 0.0663(5) Uani d 1 . .
H H5A 0.767186 0.728822 0.597752 0.080 Uiso calc 1 . .
C C5B 0.31931(18) 0.73805(12) 0.37776(12) 0.0572(5) Uani d 1 . .
H H5B 0.336243 0.775028 0.340470 0.069 Uiso calc 1 . .
C C6A 0.7128(2) 0.84521(14) 0.59469(16) 0.0719(6) Uani d 1 . .
H H6A 0.763410 0.866124 0.567158 0.086 Uiso calc 1 . .
C C6B 0.3260(2) 0.65590(14) 0.36481(14) 0.0699(6) Uani d 1 . .
H H6B 0.347755 0.637057 0.318813 0.084 Uiso calc 1 . .
C C7A 0.6353(2) 0.89685(13) 0.61719(15) 0.0669(5) Uani d 1 . .
H H7A 0.633301 0.952178 0.603750 0.080 Uiso calc 1 . .
C C7B 0.3002(2) 0.60060(13) 0.42011(16) 0.0738(6) Uani d 1 . .
H H7B 0.304581 0.544836 0.410662 0.089 Uiso calc 1 . .
C C8A 0.56154(18) 0.86710(11) 0.65916(14) 0.0570(5) Uani d 1 . .
H H8A 0.510698 0.902433 0.674732 0.068 Uiso calc 1 . .
C C8B 0.2684(2) 0.62723(12) 0.48872(14) 0.0644(5) Uani d 1 . .
H H8B 0.251967 0.589664 0.525684 0.077 Uiso calc 1 . .
C C8A' 0.56261(15) 0.78398(10) 0.67853(11) 0.0443(4) Uani d 1 . .
C C8B' 0.26094(16) 0.71106(10) 0.50270(11) 0.0455(4) Uani d 1 . .
C C9A 0.5550(2) 0.53429(12) 0.73431(16) 0.0712(6) Uani d 1 . .
H H9AA 0.543485 0.503622 0.682028 0.107 Uiso calc 1 . .
H H9AB 0.488631 0.524014 0.754066 0.107 Uiso calc 1 . .
H H9AC 0.629728 0.517988 0.778655 0.107 Uiso calc 1 . .
C C9B 0.2411(2) 0.96167(12) 0.55107(14) 0.0673(5) Uani d 1 . .
H H9BA 0.308740 0.989779 0.544197 0.101 Uiso calc 1 . .
H H9BB 0.242392 0.969168 0.609523 0.101 Uiso calc 1 . .
H H9BC 0.166757 0.983288 0.510518 0.101 Uiso calc 1 . .
C C10A 0.40897(15) 0.64886(10) 0.78644(11) 0.0464(4) Uani d 1 . .
C C10B 0.18531(16) 0.84207(12) 0.65864(11) 0.0520(4) Uani d 1 . .
N N11A 0.29256(13) 0.64598(9) 0.73505(9) 0.0459(3) Uani d 1 . .
N N11B 0.27899(14) 0.84235(9) 0.73404(9) 0.0458(3) Uani d 1 . .
H H11A 0.2709(18) 0.6657(12) 0.6816(13) 0.056(5) Uiso d 1 . .
H H11B 0.3453(19) 0.8211(12) 0.7308(13) 0.060(6) Uiso d 1 . .
C C12A 0.19183(15) 0.62418(10) 0.76017(11) 0.0458(4) Uani d 1 . .
C C12B 0.28641(16) 0.86210(10) 0.82016(10) 0.0460(4) Uani d 1 . .
C C13A 0.17430(18) 0.65831(12) 0.83199(13) 0.0579(5) Uani d 1 . .
H H13A 0.231162 0.694273 0.868105 0.070 Uiso calc 1 . .
C C13B 0.1889(2) 0.88031(13) 0.84467(13) 0.0615(5) Uani d 1 . .
H H13B 0.110617 0.880890 0.803547 0.074 Uiso calc 1 . .
C C14A 0.0710(2) 0.63823(14) 0.84934(16) 0.0687(6) Uani d 1 . .
H H14A 0.058768 0.660791 0.897690 0.082 Uiso calc 1 . .
C C14B 0.2088(2) 0.89785(15) 0.93166(14) 0.0733(6) Uani d 1 . .
H H14B 0.143062 0.910500 0.948369 0.088 Uiso calc 1 . .
C C15A -0.01364(19) 0.58550(15) 0.79631(16) 0.0728(6) Uani d 1 . .
H H15A -0.083359 0.573110 0.808191 0.087 Uiso calc 1 . .
C C15B 0.3230(2) 0.89684(15) 0.99301(13) 0.0743(6) Uani d 1 . .
H H15B 0.335113 0.909440 1.050847 0.089 Uiso calc 1 . .
C C16A 0.00499(18) 0.55107(15) 0.72556(15) 0.0713(6) Uani d 1 . .
H H16A -0.051928 0.514896 0.689846 0.086 Uiso calc 1 . .
C C16B 0.4194(2) 0.87709(17) 0.96852(14) 0.0799(7) Uani d 1 . .
H H16B 0.497078 0.875101 1.010346 0.096 Uiso calc 1 . .
C C17A 0.10845(17) 0.57004(13) 0.70712(12) 0.0580(5) Uani d 1 . .
H H17A 0.121368 0.546455 0.659469 0.070 Uiso calc 1 . .
C C17B 0.40270(19) 0.86009(14) 0.88256(12) 0.0637(5) Uani d 1 . .
H H17B 0.468896 0.847365 0.866451 0.076 Uiso calc 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
S1A 0.0501(3) 0.1132(5) 0.0526(3) -0.0013(3) 0.0178(2) 0.0220(3)
O1A 0.0852(10) 0.0582(8) 0.1095(12) 0.0080(7) 0.0668(10) -0.0077(8)
N1A 0.0427(7) 0.0479(8) 0.0540(8) 0.0015(6) 0.0267(6) 0.0025(6)
N1B 0.0546(8) 0.0508(8) 0.0435(7) 0.0033(6) 0.0257(6) 0.0007(6)
S1B 0.0536(3) 0.1936(8) 0.0591(3) 0.0382(4) 0.0165(3) -0.0226(4)
O1B 0.0907(10) 0.0565(8) 0.0774(9) -0.0040(7) 0.0513(8) 0.0100(7)
C2A 0.0387(8) 0.0476(9) 0.0469(8) -0.0015(6) 0.0201(7) 0.0002(7)
C2B 0.0423(9) 0.0539(10) 0.0380(8) 0.0038(7) 0.0152(7) -0.0023(7)
N3A 0.0499(8) 0.0422(7) 0.0625(9) -0.0013(6) 0.0304(7) -0.0013(6)
N3B 0.0495(8) 0.0443(7) 0.0464(7) -0.0005(6) 0.0195(6) -0.0044(6)
C4A 0.0521(10) 0.0519(10) 0.0633(11) -0.0020(8) 0.0333(9) -0.0068(8)
C4B 0.0489(9) 0.0503(9) 0.0484(9) -0.0023(7) 0.0229(8) 0.0002(7)
C4A' 0.0469(9) 0.0512(9) 0.0569(10) -0.0034(7) 0.0290(8) -0.0030(7)
C4B' 0.0445(9) 0.0489(9) 0.0425(8) -0.0018(7) 0.0198(7) -0.0030(7)
C5A 0.0646(12) 0.0689(13) 0.0855(14) -0.0023(10) 0.0513(11) 0.0005(10)
C5B 0.0658(12) 0.0649(11) 0.0512(10) 0.0001(9) 0.0335(9) -0.0045(8)
C6A 0.0704(14) 0.0738(14) 0.0899(15) -0.0128(11) 0.0511(12) 0.0088(11)
C6B 0.0848(15) 0.0734(13) 0.0648(12) 0.0046(11) 0.0429(11) -0.0170(10)
C7A 0.0699(13) 0.0544(11) 0.0843(14) -0.0078(10) 0.0371(11) 0.0123(10)
C7B 0.0952(17) 0.0519(11) 0.0867(15) 0.0033(11) 0.0476(13) -0.0166(10)
C8A 0.0580(11) 0.0485(10) 0.0733(12) 0.0009(8) 0.0339(10) 0.0057(8)
C8B 0.0857(15) 0.0480(10) 0.0714(13) 0.0014(9) 0.0425(11) -0.0013(8)
C8A' 0.0409(8) 0.0473(9) 0.0498(9) -0.0028(7) 0.0222(7) 0.0001(7)
C8B' 0.0504(9) 0.0468(9) 0.0442(8) 0.0017(7) 0.0227(7) -0.0018(7)
C9A 0.0849(15) 0.0444(10) 0.0987(16) -0.0026(10) 0.0505(13) 0.0025(10)
C9B 0.0868(15) 0.0460(10) 0.0687(12) 0.0036(10) 0.0270(11) -0.0114(9)
C10A 0.0412(9) 0.0513(9) 0.0518(9) -0.0005(7) 0.0228(7) 0.0051(7)
C10B 0.0501(10) 0.0655(11) 0.0435(9) 0.0082(8) 0.0203(8) -0.0063(8)
N11A 0.0415(7) 0.0561(8) 0.0453(8) -0.0012(6) 0.0217(6) 0.0100(6)
N11B 0.0475(8) 0.0537(8) 0.0415(7) 0.0071(6) 0.0222(6) -0.0045(6)
C12A 0.0385(8) 0.0533(9) 0.0500(9) 0.0032(7) 0.0213(7) 0.0141(7)
C12B 0.0560(10) 0.0462(9) 0.0415(8) 0.0035(7) 0.0241(8) -0.0018(6)
C13A 0.0570(11) 0.0587(11) 0.0684(11) 0.0054(9) 0.0348(9) 0.0052(9)
C13B 0.0619(12) 0.0770(13) 0.0520(10) 0.0144(10) 0.0280(9) -0.0044(9)
C14A 0.0647(13) 0.0808(14) 0.0776(14) 0.0150(11) 0.0461(12) 0.0154(11)
C14B 0.0842(16) 0.0910(15) 0.0588(12) 0.0145(12) 0.0426(12) -0.0071(11)
C15A 0.0501(11) 0.0950(16) 0.0849(15) 0.0072(11) 0.0380(11) 0.0303(13)
C15B 0.0956(17) 0.0875(15) 0.0461(10) -0.0038(13) 0.0329(11) -0.0109(10)
C16A 0.0486(11) 0.0888(15) 0.0742(13) -0.0137(10) 0.0187(10) 0.0193(11)
C16B 0.0736(15) 0.116(2) 0.0473(11) -0.0050(13) 0.0174(10) -0.0126(11)
C17A 0.0507(10) 0.0729(12) 0.0521(10) -0.0069(9) 0.0203(8) 0.0098(9)
C17B 0.0556(11) 0.0883(15) 0.0490(10) 0.0010(10) 0.0207(9) -0.0083(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
S S 0.3331 0.5567 '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
C2A N1A C8A' . . 117.91(14) ?
C2B N1B C8B' . . 117.44(14) ?
N1A C2A N3A . . 124.89(14) ?
N1A C2A C10A . . 116.71(14) ?
N3A C2A C10A . . 118.39(14) ?
N1B C2B N3B . . 125.33(14) ?
N1B C2B C10B . . 116.84(15) ?
N3B C2B C10B . . 117.83(15) ?
C2A N3A C4A . . 121.39(14) ?
C2A N3A C9A . . 122.23(15) ?
C4A N3A C9A . . 116.35(15) ?
C2B N3B C4B . . 121.15(14) ?
C2B N3B C9B . . 122.32(15) ?
C4B N3B C9B . . 116.47(15) ?
O1A C4A N3A . . 120.23(17) ?
O1A C4A C4A' . . 125.05(17) ?
N3A C4A C4A' . . 114.72(14) ?
O1B C4B N3B . . 120.52(16) ?
O1B C4B C4B' . . 124.74(16) ?
N3B C4B C4B' . . 114.73(14) ?
C8A' C4A' C5A . . 119.71(17) ?
C8A' C4A' C4A . . 119.49(15) ?
C5A C4A' C4A . . 120.80(16) ?
C8B' C4B' C5B . . 120.06(16) ?
C8B' C4B' C4B . . 119.62(14) ?
C5B C4B' C4B . . 120.33(16) ?
C6A C5A C4A' . . 120.07(19) ?
C6A C5A H5A . . 120.0 ?
C4A' C5A H5A . . 120.0 ?
C6B C5B C4B' . . 119.92(18) ?
C6B C5B H5B . . 120.0 ?
C4B' C5B H5B . . 120.0 ?
C5A C6A C7A . . 120.17(18) ?
C5A C6A H6A . . 119.9 ?
C7A C6A H6A . . 119.9 ?
C5B C6B C7B . . 120.16(18) ?
C5B C6B H6B . . 119.9 ?
C7B C6B H6B . . 119.9 ?
C8A C7A C6A . . 120.58(19) ?
C8A C7A H7A . . 119.7 ?
C6A C7A H7A . . 119.7 ?
C8B C7B C6B . . 120.80(19) ?
C8B C7B H7B . . 119.6 ?
C6B C7B H7B . . 119.6 ?
C7A C8A C8A' . . 120.18(18) ?
C7A C8A H8A . . 119.9 ?
C8A' C8A H8A . . 119.9 ?
C7B C8B C8B' . . 119.73(19) ?
C7B C8B H8B . . 120.1 ?
C8B' C8B H8B . . 120.1 ?
N1A C8A' C4A' . . 121.56(15) ?
N1A C8A' C8A . . 119.17(15) ?
C4A' C8A' C8A . . 119.26(16) ?
C4B' C8B' N1B . . 121.68(15) ?
C4B' C8B' C8B . . 119.33(16) ?
N1B C8B' C8B . . 118.99(16) ?
N3A C9A H9AA . . 109.5 ?
N3A C9A H9AB . . 109.5 ?
H9AA C9A H9AB . . 109.5 ?
N3A C9A H9AC . . 109.5 ?
H9AA C9A H9AC . . 109.5 ?
H9AB C9A H9AC . . 109.5 ?
N3B C9B H9BA . . 109.5 ?
N3B C9B H9BB . . 109.5 ?
H9BA C9B H9BB . . 109.5 ?
N3B C9B H9BC . . 109.5 ?
H9BA C9B H9BC . . 109.5 ?
H9BB C9B H9BC . . 109.5 ?
N11A C10A C2A . . 112.34(14) ?
N11A C10A S1A . . 127.74(13) ?
C2A C10A S1A . . 119.91(12) ?
N11B C10B C2B . . 111.73(14) ?
N11B C10B S1B . . 130.79(13) ?
C2B C10B S1B . . 117.47(13) ?
C10A N11A C12A . . 126.80(14) ?
C10A N11A H11A . . 119.1(13) ?
C12A N11A H11A . . 113.5(13) ?
C10B N11B C12B . . 131.43(15) ?
C10B N11B H11B . . 114.1(13) ?
C12B N11B H11B . . 114.0(13) ?
C17A C12A C13A . . 120.63(17) ?
C17A C12A N11A . . 117.17(16) ?
C13A C12A N11A . . 122.12(17) ?
C13B C12B C17B . . 119.80(16) ?
C13B C12B N11B . . 125.03(17) ?
C17B C12B N11B . . 115.15(16) ?
C14A C13A C12A . . 119.0(2) ?
C14A C13A H13A . . 120.5 ?
C12A C13A H13A . . 120.5 ?
C12B C13B C14B . . 119.2(2) ?
C12B C13B H13B . . 120.4 ?
C14B C13B H13B . . 120.4 ?
C15A C14A C13A . . 121.0(2) ?
C15A C14A H14A . . 119.5 ?
C13A C14A H14A . . 119.5 ?
C15B C14B C13B . . 121.2(2) ?
C15B C14B H14B . . 119.4 ?
C13B C14B H14B . . 119.4 ?
C14A C15A C16A . . 119.72(19) ?
C14A C15A H15A . . 120.1 ?
C16A C15A H15A . . 120.1 ?
C14B C15B C16B . . 119.32(19) ?
C14B C15B H15B . . 120.3 ?
C16B C15B H15B . . 120.3 ?
C15A C16A C17A . . 120.3(2) ?
C15A C16A H16A . . 119.9 ?
C17A C16A H16A . . 119.9 ?
C15B C16B C17B . . 120.8(2) ?
C15B C16B H16B . . 119.6 ?
C17B C16B H16B . . 119.6 ?
C12A C17A C16A . . 119.35(19) ?
C12A C17A H17A . . 120.3 ?
C16A C17A H17A . . 120.3 ?
C16B C17B C12B . . 119.6(2) ?
C16B C17B H17B . . 120.2 ?
C12B C17B H17B . . 120.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1A C10A . 1.6385(17) ?
O1A C4A . 1.219(2) ?
N1A C2A . 1.292(2) ?
N1A C8A' . 1.392(2) ?
N1B C2B . 1.293(2) ?
N1B C8B' . 1.392(2) ?
S1B C10B . 1.6401(18) ?
O1B C4B . 1.220(2) ?
C2A N3A . 1.367(2) ?
C2A C10A . 1.511(2) ?
C2B N3B . 1.368(2) ?
C2B C10B . 1.510(2) ?
N3A C4A . 1.404(2) ?
N3A C9A . 1.467(2) ?
N3B C4B . 1.399(2) ?
N3B C9B . 1.470(2) ?
C4A C4A' . 1.453(3) ?
C4B C4B' . 1.455(2) ?
C4A' C8A' . 1.396(2) ?
C4A' C5A . 1.401(2) ?
C4B' C8B' . 1.392(2) ?
C4B' C5B . 1.399(2) ?
C5A C6A . 1.371(3) ?
C5A H5A . 0.9300 ?
C5B C6B . 1.367(3) ?
C5B H5B . 0.9300 ?
C6A C7A . 1.385(3) ?
C6A H6A . 0.9300 ?
C6B C7B . 1.387(3) ?
C6B H6B . 0.9300 ?
C7A C8A . 1.373(3) ?
C7A H7A . 0.9300 ?
C7B C8B . 1.375(3) ?
C7B H7B . 0.9300 ?
C8A C8A' . 1.396(2) ?
C8A H8A . 0.9300 ?
C8B C8B' . 1.399(2) ?
C8B H8B . 0.9300 ?
C9A H9AA . 0.9600 ?
C9A H9AB . 0.9600 ?
C9A H9AC . 0.9600 ?
C9B H9BA . 0.9600 ?
C9B H9BB . 0.9600 ?
C9B H9BC . 0.9600 ?
C10A N11A . 1.332(2) ?
C10B N11B . 1.334(2) ?
N11A C12A . 1.430(2) ?
N11A H11A . 0.88(2) ?
N11B C12B . 1.420(2) ?
N11B H11B . 0.87(2) ?
C12A C17A . 1.379(3) ?
C12A C13A . 1.382(3) ?
C12B C13B . 1.375(2) ?
C12B C17B . 1.390(3) ?
C13A C14A . 1.382(3) ?
C13A H13A . 0.9300 ?
C13B C14B . 1.390(3) ?
C13B H13B . 0.9300 ?
C14A C15A . 1.372(3) ?
C14A H14A . 0.9300 ?
C14B C15B . 1.365(3) ?
C14B H14B . 0.9300 ?
C15A C16A . 1.374(3) ?
C15A H15A . 0.9300 ?
C15B C16B . 1.369(3) ?
C15B H15B . 0.9300 ?
C16A C17A . 1.389(3) ?
C16A H16A . 0.9300 ?
C16B C17B . 1.380(3) ?
C16B H16B . 0.9300 ?
C17A H17A . 0.9300 ?
C17B H17B . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
N1A H11A N1B 1_555 ? ? 0.88(2) 2.05(2) 2.913(2) 166.7(18) yes
N1B H11B N1A 1_555 . . 0.87(2) 2.04(2) 2.907(2) 171.6(19) yes
C9A H9AB S1A . . . 0.96 2.87 3.424(2) 118 yes
C13B H13B S1B . . . 0.93 2.58 3.243(3) 129 yes
C7A H7A O1B 3_676 . . 0.93 2.49 3.386(3) 162 yes
C7B H7B O1A 3_666 . . 0.93 2.47 3.385(3) 166 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
C8A' N1A C2A N3A . . . . -1.0(3) ?
C8A' N1A C2A C10A . . . . 179.14(14) ?
C8B' N1B C2B N3B . . . . -1.0(3) ?
C8B' N1B C2B C10B . . . . 179.33(14) ?
N1A C2A N3A C4A . . . . 0.6(3) ?
C10A C2A N3A C4A . . . . -179.57(16) ?
N1A C2A N3A C9A . . . . -177.51(18) ?
C10A C2A N3A C9A . . . . 2.4(3) ?
N1B C2B N3B C4B . . . . 2.7(3) ?
C10B C2B N3B C4B . . . . -177.67(15) ?
N1B C2B N3B C9B . . . . 179.73(17) ?
C10B C2B N3B C9B . . . . -0.6(2) ?
C2A N3A C4A O1A . . . . -178.66(18) ?
C9A N3A C4A O1A . . . . -0.5(3) ?
C2A N3A C4A C4A' . . . . 0.9(3) ?
C9A N3A C4A C4A' . . . . 179.10(17) ?
C2B N3B C4B O1B . . . . 178.41(17) ?
C9B N3B C4B O1B . . . . 1.2(3) ?
C2B N3B C4B C4B' . . . . -2.6(2) ?
C9B N3B C4B C4B' . . . . -179.78(16) ?
O1A C4A C4A' C8A' . . . . 177.6(2) ?
N3A C4A C4A' C8A' . . . . -1.9(3) ?
O1A C4A C4A' C5A . . . . -2.2(3) ?
N3A C4A C4A' C5A . . . . 178.19(18) ?
O1B C4B C4B' C8B' . . . . -179.87(18) ?
N3B C4B C4B' C8B' . . . . 1.1(2) ?
O1B C4B C4B' C5B . . . . 0.1(3) ?
N3B C4B C4B' C5B . . . . -178.91(16) ?
C8A' C4A' C5A C6A . . . . -1.4(3) ?
C4A C4A' C5A C6A . . . . 178.5(2) ?
C8B' C4B' C5B C6B . . . . -0.4(3) ?
C4B C4B' C5B C6B . . . . 179.66(18) ?
C4A' C5A C6A C7A . . . . 0.1(4) ?
C4B' C5B C6B C7B . . . . 0.3(3) ?
C5A C6A C7A C8A . . . . 1.1(4) ?
C5B C6B C7B C8B . . . . -0.3(4) ?
C6A C7A C8A C8A' . . . . -0.9(3) ?
C6B C7B C8B C8B' . . . . 0.5(4) ?
C2A N1A C8A' C4A' . . . . -0.1(2) ?
C2A N1A C8A' C8A . . . . 179.82(16) ?
C5A C4A' C8A' N1A . . . . -178.49(18) ?
C4A C4A' C8A' N1A . . . . 1.6(3) ?
C5A C4A' C8A' C8A . . . . 1.5(3) ?
C4A C4A' C8A' C8A . . . . -178.35(17) ?
C7A C8A C8A' N1A . . . . 179.63(18) ?
C7A C8A C8A' C4A' . . . . -0.4(3) ?
C5B C4B' C8B' N1B . . . . -179.59(16) ?
C4B C4B' C8B' N1B . . . . 0.4(3) ?
C5B C4B' C8B' C8B . . . . 0.6(3) ?
C4B C4B' C8B' C8B . . . . -179.50(18) ?
C2B N1B C8B' C4B' . . . . -0.5(2) ?
C2B N1B C8B' C8B . . . . 179.35(18) ?
C7B C8B C8B' C4B' . . . . -0.6(3) ?
C7B C8B C8B' N1B . . . . 179.5(2) ?
N1A C2A C10A N11A . . . . 75.1(2) ?
N3A C2A C10A N11A . . . . -104.80(18) ?
N1A C2A C10A S1A . . . . -103.97(17) ?
N3A C2A C10A S1A . . . . 76.14(19) ?
N1B C2B C10B N11B . . . . 83.6(2) ?
N3B C2B C10B N11B . . . . -96.12(19) ?
N1B C2B C10B S1B . . . . -96.53(18) ?
N3B C2B C10B S1B . . . . 83.78(19) ?
C2A C10A N11A C12A . . . . -177.47(15) ?
S1A C10A N11A C12A . . . . 1.5(3) ?
C2B C10B N11B C12B . . . . -179.09(17) ?
S1B C10B N11B C12B . . . . 1.0(3) ?
C10A N11A C12A C17A . . . . -133.70(19) ?
C10A N11A C12A C13A . . . . 49.3(3) ?
C10B N11B C12B C13B . . . . 5.4(3) ?
C10B N11B C12B C17B . . . . -176.2(2) ?
C17A C12A C13A C14A . . . . -0.8(3) ?
N11A C12A C13A C14A . . . . 176.03(17) ?
C17B C12B C13B C14B . . . . 1.1(3) ?
N11B C12B C13B C14B . . . . 179.36(19) ?
C12A C13A C14A C15A . . . . -0.3(3) ?
C12B C13B C14B C15B . . . . -0.4(4) ?
C13A C14A C15A C16A . . . . 1.0(3) ?
C13B C14B C15B C16B . . . . -0.9(4) ?
C14A C15A C16A C17A . . . . -0.6(3) ?
C14B C15B C16B C17B . . . . 1.5(4) ?
C13A C12A C17A C16A . . . . 1.2(3) ?
N11A C12A C17A C16A . . . . -175.84(17) ?
C15A C16A C17A C12A . . . . -0.4(3) ?
C15B C16B C17B C12B . . . . -0.8(4) ?
C13B C12B C17B C16B . . . . -0.5(3) ?
N11B C12B C17B C16B . . . . -179.0(2) ?
_cod_database_fobs_code 2243946