#------------------------------------------------------------------------------
#$Date: 2024-07-10 04:51:59 +0300 (Wed, 10 Jul 2024) $
#$Revision: 293350 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023195.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_2023195
loop_
_publ_author_name
'Abu-Zaied, Mamdouh A.'
'Nawwar, Galal A.'
'Elgemeie, Galal H.'
'Jones, Peter G.'
_publ_section_title
;
Crystal structures of four thioglycosides involving carbamimidothioate
groups
;
_journal_coeditor_code YZ2056
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024006455
_journal_volume 80
_journal_year 2024
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C23 H27 N3 O9 S'
_chemical_formula_moiety 'C23 H27 N3 O9 S'
_chemical_formula_sum 'C23 H27 N3 O9 S'
_chemical_formula_weight 521.53
_chemical_name_systematic
;
2',3',4',6'-Tetra-O-acetyl-\b-D-galactopyranosyl
N'-cyano-N-p-tolylcarbamimidothioate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.41967(5)
_cell_length_b 14.96519(12)
_cell_length_c 22.75622(16)
_cell_measurement_reflns_used 90210
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 80.0220
_cell_measurement_theta_min 3.5190
_cell_volume 2526.78(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Bruker XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3(Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0326
_diffrn_reflns_av_unetI/netI 0.0096
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 122360
_diffrn_reflns_theta_full 77.500
_diffrn_reflns_theta_max 80.615
_diffrn_reflns_theta_min 3.535
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.632
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.78082
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.371
_exptl_crystal_description prism
_exptl_crystal_F_000 1096
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.217
_refine_diff_density_min -0.182
_refine_ls_abs_structure_details
;
Flack x determined using 2334 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.004(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 334
_refine_ls_number_reflns 5508
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0228
_refine_ls_R_factor_gt 0.0226
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.7621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0592
_refine_ls_wR_factor_ref 0.0593
_reflns_number_gt 5458
_reflns_number_total 5508
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2056.cif
_cod_data_source_block 5dCu
_cod_database_code 2023195
_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 0.792
_shelx_estimated_absorpt_t_max 0.938
_shelx_hkl_file
;
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0 0 -7 29.4859 71.3986 22
0 0 8 101094. 3266.89 45
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0 0 8 102294. 3246.20 50
0 0 -8 109505. 3283.16 22
0 0 8 107595. 3220.85 7
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0 0 9 75.5262 69.4571 20
0 0 10 659769. 20230.3 43
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2 -9 -21 2083.42 112.734 137
2 -9 -21 2045.08 110.398 126
2 -9 -21 2421.04 131.117 106
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2 -9 -21 2001.90 115.837 99
2 -9 -21 2035.19 118.681 83
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2 -9 -23 2029.14 103.375 83
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2 -10 17 3389.84 306.561 30
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4 -4 -4 2146.07 158.599 35
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4 -4 -5 17724.6 693.588 46
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4 -4 -6 2046.29 125.270 81
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4 -4 -6 1647.33 223.596 47
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9 -3 2 1337.34 73.2810 92
-9 3 2 1305.65 71.8705 153
9 3 -2 1283.82 67.4632 149
9 -3 2 1255.31 62.3818 149
-9 3 2 1282.17 67.5689 144
-9 3 1 2978.70 119.717 6
-9 3 1 2924.02 120.524 153
-9 -3 -1 2752.23 118.455 153
9 3 -1 3109.64 119.201 149
9 -3 1 2827.81 110.098 149
-9 3 1 2712.34 112.857 144
9 3 -1 2774.48 110.115 166
9 -3 1 2905.01 116.190 166
9 3 -1 2875.98 110.792 159
-9 -3 -1 2962.49 117.641 113
9 -3 1 3021.73 123.426 92
-9 3 0 887.615 60.5412 6
-9 -3 0 965.424 62.3995 6
9 3 0 872.327 57.7877 5
-9 -3 0 762.505 52.9668 144
-9 3 0 900.068 61.8891 153
-9 -3 0 860.475 57.1101 153
9 3 0 887.458 58.6352 149
9 -3 0 788.897 46.8946 149
9 3 0 834.979 47.5019 166
9 -3 0 845.317 55.6016 166
-9 3 0 706.454 46.9449 128
-9 -3 0 889.352 56.2495 113
9 -3 0 996.644 65.7554 92
-9 -3 1 3083.92 118.453 144
-9 -3 1 3098.96 117.482 153
9 3 1 3429.21 122.870 149
9 -3 -1 2382.57 102.147 149
9 3 1 2203.70 103.796 166
9 -3 -1 3291.57 119.179 166
-9 3 -1 3122.39 114.585 128
-9 3 -1 3207.43 121.713 104
-9 -3 1 3352.19 120.173 113
9 3 1 3334.70 124.547 4
-9 -3 1 3417.41 124.213 6
9 3 1 3079.50 121.045 5
9 3 2 1283.99 71.0308 4
-9 3 -2 1344.09 71.2719 6
-9 -3 2 1271.91 71.0737 6
9 3 2 1275.77 67.7472 5
-9 -3 2 1345.36 70.0535 144
-9 -3 2 1242.62 63.0092 153
9 3 2 1472.31 70.8128 149
9 -3 -2 1377.88 66.8230 166
-9 3 -2 1175.74 65.3138 128
-9 -3 2 1226.00 58.4676 104
-9 3 -2 1537.61 71.7915 104
-9 -3 2 1213.83 65.7767 113
-9 -3 2 1225.60 67.5440 94
9 3 3 3137.88 120.029 4
-9 3 -3 3393.65 119.987 6
-9 -3 3 2849.16 117.629 6
9 3 3 2924.95 116.971 5
-9 -3 3 3030.66 119.803 144
-9 3 -3 3004.56 119.562 153
-9 -3 3 2622.54 108.591 153
9 -3 -3 2912.95 109.123 139
9 -3 -3 2884.33 115.757 166
-9 3 -3 3052.56 119.746 128
-9 -3 3 2817.00 109.867 104
-9 -3 3 2935.52 114.315 113
-9 -3 3 3009.22 118.558 94
9 -3 -3 3345.04 124.982 92
9 3 4 358.440 40.3590 4
-9 3 -4 465.126 40.6516 6
-9 -3 4 381.605 40.2937 6
9 3 4 396.418 38.0444 5
-9 3 -4 453.056 44.5000 153
9 -3 -4 396.039 31.7164 139
9 -3 -4 420.126 36.4699 166
-9 3 -4 429.507 45.0911 128
-9 -3 4 365.170 33.1469 104
-9 -3 4 415.519 36.1068 113
-9 -3 4 437.367 41.0200 94
9 -3 -4 437.421 46.2347 92
9 -3 -5 3681.40 135.021 139
-9 3 -5 3910.29 141.434 153
9 3 5 3977.61 143.416 149
9 -3 -5 4120.83 140.083 166
9 -3 -5 4082.13 145.073 159
-9 3 -5 4216.19 148.033 128
-9 3 -5 3853.90 137.105 6
-9 -3 5 3755.61 137.658 6
-9 -3 5 4034.37 143.983 94
-9 3 -6 1593.33 74.5780 128
9 -3 -6 1528.93 64.0995 166
9 -3 -6 1358.30 67.9604 159
-9 -3 6 1565.15 71.9050 144
9 3 6 1625.24 68.8266 149
-9 -3 6 1633.90 70.2702 94
-9 -3 7 1073.80 54.0687 144
9 -3 -7 979.762 49.0487 159
9 -4 6 630.110 35.6695 149
9 4 -6 602.957 37.3815 159
-9 4 6 632.836 36.1604 123
-9 -4 -6 610.925 38.0281 131
-9 4 5 849.019 43.4132 123
-9 -4 -5 651.784 41.8536 131
9 4 -5 639.908 40.8649 159
-9 4 5 735.477 41.4411 153
9 4 -5 628.361 38.7882 149
-9 4 5 779.768 46.6888 144
9 -4 5 748.605 40.2829 149
-9 4 5 639.057 38.6084 6
-9 -4 -4 2044.28 89.0145 131
-9 4 4 2469.39 94.0375 123
9 4 -4 2379.78 91.4670 159
-9 4 4 2486.60 92.4968 6
-9 -4 -4 2267.99 91.0504 6
9 4 -4 2114.62 90.7690 5
-9 4 4 2414.61 93.9502 153
9 4 -4 2312.67 92.2205 149
9 -4 4 2359.92 89.0555 149
-9 4 4 2657.64 96.3495 144
9 4 -3 1305.46 71.7230 4
-9 4 3 1850.92 74.0548 6
-9 -4 -3 1493.91 70.9422 6
9 4 -3 1384.17 70.2733 5
-9 4 3 1677.76 73.6778 153
9 4 -3 1491.20 70.8360 149
9 -4 3 1464.96 63.9900 149
-9 4 3 1634.01 71.4338 144
9 4 -3 1358.99 64.6006 159
9 -4 3 1504.14 68.9334 166
-9 4 3 1520.78 72.0898 123
-9 4 3 1562.61 68.6981 104
9 -4 3 1731.72 74.9074 92
9 4 -2 1006.91 59.2299 4
-9 4 2 1061.44 59.2441 6
-9 -4 -2 1027.25 59.2362 6
-9 4 2 1068.80 58.9672 153
9 4 -2 993.010 56.9739 149
9 -4 2 860.903 45.8789 149
-9 4 2 1120.95 55.7479 144
9 4 -2 923.548 47.6320 159
9 -4 2 1021.48 54.4580 166
9 -4 2 908.015 46.2589 139
-9 4 2 1009.20 55.9532 104
-9 -4 -2 1102.59 58.9501 113
9 -4 2 862.351 59.6814 92
-9 4 1 1893.74 82.4075 6
-9 4 1 1838.88 84.0198 153
9 4 -1 1737.40 79.7899 149
-9 4 1 1553.13 71.8781 144
9 -4 1 1730.52 77.1176 166
9 -4 1 1689.78 71.1369 139
-9 4 1 1786.01 80.8430 104
-9 -4 -1 1645.00 80.5977 113
9 -4 1 1904.38 85.3885 92
-9 -4 0 544.242 48.9906 6
9 4 0 547.298 46.2467 5
-9 -4 0 491.971 40.9578 144
-9 -4 0 593.980 43.8960 153
9 4 0 606.586 47.6551 149
9 -4 0 516.968 39.9706 166
9 -4 0 603.544 38.6822 139
-9 4 0 584.834 45.9137 104
-9 -4 0 702.306 47.9438 113
9 -4 0 603.266 53.0513 92
9 4 1 2031.25 91.0471 4
-9 -4 1 2154.38 91.1185 6
9 4 1 2026.65 88.2174 5
-9 -4 1 1961.81 84.0078 153
9 4 1 2195.94 90.7229 149
9 -4 -1 2039.85 81.7945 139
9 -4 -1 2113.64 84.6081 166
-9 4 -1 1940.97 81.2505 128
-9 -4 1 2040.02 88.1303 113
9 -4 -1 1976.22 94.3084 92
-9 -4 2 847.142 53.8146 144
-9 4 -2 887.967 55.5079 153
-9 -4 2 695.094 43.4844 153
9 -4 -2 885.035 48.1426 139
9 -4 -2 883.259 48.6628 166
-9 4 -2 890.399 52.0562 128
-9 -4 2 923.936 52.5352 113
9 4 2 920.043 56.0142 4
-9 4 -2 778.250 54.3696 6
-9 -4 2 872.822 55.0720 6
9 4 2 886.215 52.7168 5
9 4 3 1718.42 77.4761 4
-9 4 -3 1742.72 76.8960 6
-9 -4 3 1616.85 75.6962 6
9 4 3 1564.25 72.9953 5
-9 -4 3 1638.98 77.1058 144
-9 4 -3 1690.08 76.2455 153
9 -4 -3 1641.12 70.3269 139
9 -4 -3 1616.40 69.9980 166
-9 4 -3 1653.69 76.0157 128
-9 -4 3 1637.38 74.3215 113
-9 -4 3 1738.55 74.0998 94
9 -4 -3 1748.29 80.4035 92
9 4 4 2334.21 93.2707 4
-9 4 -4 2451.66 91.2658 6
-9 -4 4 2193.77 91.1649 6
9 -4 -4 2293.48 88.9992 139
-9 4 -4 2303.89 92.0107 153
9 4 4 2602.73 94.6093 149
9 -4 -4 2184.00 86.5438 166
-9 4 -4 2398.24 95.8437 128
-9 -4 4 2298.63 91.8494 113
-9 -4 4 2351.02 92.2925 94
9 -4 -4 2339.81 96.5302 92
-9 4 -5 859.005 51.3940 128
9 -4 -5 839.697 46.8503 159
9 -4 -5 806.050 42.6325 139
-9 -4 5 763.143 42.2480 6
-9 4 -6 890.361 47.9355 128
-9 -4 6 766.506 45.0460 144
-9 5 5 2672.58 95.3386 123
-9 5 4 3325.33 110.940 123
9 -5 4 2982.88 106.518 166
-9 5 4 3136.18 110.258 153
9 5 -4 2822.43 108.423 149
-9 5 4 3078.30 108.997 144
-9 5 3 6030.68 180.793 123
9 -5 3 4913.99 174.494 166
-9 5 3 5598.97 178.805 6
-9 -5 -3 4675.89 175.531 6
-9 5 3 5665.18 181.482 153
9 5 -3 5292.28 179.280 149
-9 5 3 5266.66 176.187 144
9 -5 2 724.493 40.1394 139
9 -5 2 733.515 41.1799 166
-9 5 2 959.182 49.9578 6
-9 -5 -2 832.090 47.8794 6
-9 5 2 955.177 50.1203 153
9 5 -2 961.822 49.3699 149
-9 5 1 627.205 43.9874 153
-9 -5 -1 515.863 38.3477 153
9 5 -1 651.916 42.6316 149
9 -5 1 532.753 34.5263 166
9 -5 1 586.248 35.9276 139
-9 5 1 669.583 44.1201 6
9 -5 1 702.119 47.1670 92
-9 -5 0 135.917 24.4139 153
9 -5 0 150.024 21.3074 166
9 -5 0 130.461 24.1608 139
-9 5 0 157.734 27.6183 123
9 -5 0 151.823 32.5842 92
9 5 0 188.289 29.4993 5
-9 5 -1 940.333 48.5152 123
-9 -5 1 682.732 44.7803 144
-9 5 -1 922.371 51.7057 153
9 -5 -1 878.657 45.2777 139
9 5 1 866.348 51.3924 4
-9 -5 1 773.651 50.7033 6
9 5 1 879.085 49.0723 5
9 -5 -1 1020.23 56.2819 92
-9 -5 2 527.573 40.1455 144
-9 5 -2 765.510 43.3382 153
9 -5 -2 599.204 38.2824 139
9 5 2 629.462 41.3028 149
-9 -5 2 661.675 43.1314 113
-9 5 -2 730.679 44.0231 6
-9 -5 2 725.402 44.2088 6
-9 5 -3 5476.98 174.797 6
-9 -5 3 5152.00 174.145 6
-9 5 -3 5310.14 173.667 153
9 -5 -3 5208.37 173.410 139
9 5 3 5816.21 176.279 149
-9 5 -3 5082.21 171.189 123
-9 5 -3 5275.36 174.711 128
-9 5 -4 2844.61 94.9094 128
9 -5 -4 2778.96 91.5954 139
-9 6 1 2245.89 83.3744 6
0 0 0 0.00 0.00 0
TITL elg_m4 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 7.419673 14.965186 22.756217 90.0000 90.0000 90.0000
ZERR 4.00 0.000026 0.000061 0.000081 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O S
UNIT 92.00 108.00 12.00 20.00 4.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.1; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 63669
_shelx_res_file
;
TITL elg_m4 in P2(1)2(1)2(1)
shelx.res
created by SHELXL-2019/3 at 09:44:32 on 21-Jun-2024
CELL 1.54184 7.419673 14.965186 22.756217 90.0000 90.0000 90.0000
ZERR 4.00 0.00005 0.00012 0.00016 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O S
UNIT 92 108 12 36 4
TEMP -173
SIZE 0.15 0.05 0.04
OMIT -4 16 10
L.S. 6
FMAP 2
PLAN 10
ACTA 155
BOND $H
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z
HTAB N1 N3_$1
HTAB C14 O1_$1
HTAB C4 O7_$1
HTAB C5 N3_$1
EQIV $2 -x, y-1/2, -z+3/2
HTAB C1 O10_$2
HTAB C25 O9_$2
EQIV $3 x+1/2, -y+1/2, -z+2
HTAB C10 O9_$3
EQIV $4 x-1/2, -y+1/2, -z+2
HTAB C10 O3_$4
HTAB C12 O8_$3
WGHT 0.029900 0.762100
FVAR 3.48997
C1 1 0.377179 0.229358 0.768869 11.00000 0.01316 0.01949 =
0.01427 -0.00158 0.00153 0.00016
AFIX 13
H1 2 0.305463 0.178029 0.753220 11.00000 -1.20000
AFIX 0
C2 1 0.411737 0.218010 0.835388 11.00000 0.01402 0.01640 =
0.01528 -0.00184 0.00003 0.00198
AFIX 13
H2 2 0.493541 0.266236 0.850011 11.00000 -1.20000
AFIX 0
C3 1 0.231508 0.221862 0.867231 11.00000 0.01487 0.01990 =
0.01185 -0.00125 0.00026 -0.00123
AFIX 13
H3 2 0.156595 0.168623 0.856807 11.00000 -1.20000
AFIX 0
C4 1 0.130896 0.307646 0.852112 11.00000 0.01253 0.01801 =
0.01775 -0.00292 0.00088 -0.00192
AFIX 13
H4 2 0.008592 0.307059 0.870571 11.00000 -1.20000
AFIX 0
C5 1 0.113764 0.315520 0.785683 11.00000 0.01244 0.02108 =
0.01768 -0.00031 0.00025 0.00026
AFIX 13
H5 2 0.036670 0.265711 0.770640 11.00000 -1.20000
AFIX 0
C6 1 0.038593 0.403501 0.764579 11.00000 0.01556 0.02495 =
0.02417 0.00272 0.00024 0.00162
AFIX 23
H6A 2 0.115147 0.453474 0.778348 11.00000 -1.20000
H6B 2 0.034706 0.404828 0.721102 11.00000 -1.20000
AFIX 0
C7 1 0.671600 0.129120 0.855303 11.00000 0.01662 0.02664 =
0.01672 -0.00404 -0.00255 0.00313
C8 1 0.731687 0.035739 0.867532 11.00000 0.02703 0.02551 =
0.04755 -0.00439 -0.01014 0.00806
AFIX 137
H8A 2 0.706042 0.020803 0.908620 11.00000 -1.50000
H8B 2 0.861516 0.030769 0.860319 11.00000 -1.50000
H8C 2 0.666942 -0.005650 0.841684 11.00000 -1.50000
AFIX 0
C9 1 0.156085 0.175537 0.964770 11.00000 0.01569 0.02292 =
0.01756 0.00262 0.00181 0.00327
C10 1 0.183040 0.200091 1.027714 11.00000 0.02146 0.03753 =
0.01605 0.00033 0.00109 0.00341
AFIX 137
H10A 2 0.304948 0.223927 1.033097 11.00000 -1.50000
H10B 2 0.167381 0.146942 1.052348 11.00000 -1.50000
H10C 2 0.094493 0.245531 1.039034 11.00000 -1.50000
AFIX 0
C11 1 0.181913 0.418271 0.926386 11.00000 0.02245 0.02048 =
0.02189 -0.00468 0.00150 0.00108
C12 1 0.305712 0.490395 0.945854 11.00000 0.02898 0.02241 =
0.02430 -0.00408 -0.00284 -0.00344
AFIX 137
H12A 2 0.395173 0.465700 0.973058 11.00000 -1.50000
H12B 2 0.236442 0.537242 0.965739 11.00000 -1.50000
H12C 2 0.367223 0.515843 0.911615 11.00000 -1.50000
AFIX 0
C13 1 -0.234612 0.481866 0.767754 11.00000 0.02022 0.01927 =
0.02873 -0.00503 -0.00570 0.00270
C14 1 -0.421943 0.482029 0.792440 11.00000 0.01930 0.02626 =
0.04945 -0.00638 -0.00067 0.00338
AFIX 137
H14A 2 -0.489544 0.431364 0.776357 11.00000 -1.50000
H14B 2 -0.482462 0.537927 0.781767 11.00000 -1.50000
H14C 2 -0.416279 0.476901 0.835333 11.00000 -1.50000
AFIX 0
C15 1 0.561942 0.204508 0.659546 11.00000 0.01415 0.01783 =
0.01555 0.00048 -0.00010 0.00019
C16 1 0.868941 0.197243 0.652291 11.00000 0.01662 0.03045 =
0.01268 -0.00395 0.00301 0.00127
C21 1 0.368925 0.167012 0.576306 11.00000 0.01273 0.02123 =
0.01611 -0.00045 -0.00201 0.00277
C22 1 0.460362 0.205671 0.529718 11.00000 0.01618 0.02569 =
0.02059 0.00233 -0.00343 -0.00333
AFIX 43
H22 2 0.543454 0.252860 0.536484 11.00000 -1.20000
AFIX 0
C23 1 0.429472 0.174801 0.472932 11.00000 0.01863 0.03118 =
0.01670 0.00468 -0.00132 -0.00027
AFIX 43
H23 2 0.494441 0.200514 0.441181 11.00000 -1.20000
AFIX 0
C24 1 0.305731 0.107194 0.461567 11.00000 0.01915 0.02551 =
0.01926 -0.00153 -0.00283 0.00456
C25 1 0.213431 0.069816 0.509010 11.00000 0.01801 0.02291 =
0.02282 -0.00212 -0.00267 0.00002
AFIX 43
H25 2 0.128093 0.023630 0.502222 11.00000 -1.20000
AFIX 0
C26 1 0.244634 0.099246 0.566137 11.00000 0.01488 0.02360 =
0.01967 0.00067 0.00031 0.00002
AFIX 43
H26 2 0.181204 0.073110 0.598069 11.00000 -1.20000
AFIX 0
C27 1 0.269593 0.075771 0.399655 11.00000 0.03280 0.03458 =
0.02096 -0.00371 -0.00384 0.00024
AFIX 137
H27A 2 0.259841 0.010468 0.399217 11.00000 -1.50000
H27B 2 0.368852 0.094415 0.374026 11.00000 -1.50000
H27C 2 0.156622 0.102027 0.385524 11.00000 -1.50000
AFIX 0
S1 5 0.595629 0.234769 0.733601 11.00000 0.01212 0.02639 =
0.01402 -0.00383 0.00099 -0.00190
O1 4 0.287682 0.311309 0.757912 11.00000 0.01384 0.01917 =
0.01745 0.00114 0.00123 0.00054
O2 4 0.489148 0.131930 0.846388 11.00000 0.01557 0.01840 =
0.01938 -0.00051 -0.00139 0.00162
O3 4 0.269770 0.222226 0.929229 11.00000 0.01677 0.02632 =
0.01229 -0.00099 0.00048 -0.00280
O4 4 0.233692 0.382959 0.873747 11.00000 0.01573 0.01819 =
0.01813 -0.00324 0.00041 -0.00224
O6 4 -0.140071 0.411672 0.788265 11.00000 0.01491 0.02328 =
0.03294 0.00422 0.00065 0.00272
O7 4 0.766115 0.193868 0.852720 11.00000 0.01672 0.02891 =
0.02478 -0.00148 -0.00292 -0.00091
O8 4 0.046872 0.123707 0.946386 11.00000 0.03551 0.04063 =
0.02101 0.00475 -0.00051 -0.01900
O9 4 0.053060 0.392286 0.953567 11.00000 0.03111 0.03861 =
0.03669 -0.01680 0.01575 -0.00960
O10 4 -0.172440 0.535604 0.734242 11.00000 0.03093 0.02723 =
0.03940 0.00707 0.00100 0.00751
N1 3 0.398974 0.196266 0.635881 11.00000 0.01194 0.02481 =
0.01558 -0.00165 0.00062 0.00026
H01 2 0.302408 0.202342 0.657723 11.00000 0.02805
N2 3 0.707747 0.190094 0.628016 11.00000 0.01190 0.02826 =
0.01538 -0.00283 -0.00089 0.00048
N3 3 1.017426 0.203036 0.668018 11.00000 0.01484 0.04655 =
0.01871 -0.00540 0.00064 0.00088
HKLF 4
REM elg_m4 in P2(1)2(1)2(1)
REM wR2 = 0.0593, GooF = S = 1.038, Restrained GooF = 1.038 for all data
REM R1 = 0.0226 for 5458 Fo > 4sig(Fo) and 0.0228 for all 5508 data
REM 334 parameters refined using 0 restraints
END
WGHT 0.0299 0.7618
REM Highest difference peak 0.217, deepest hole -0.182, 1-sigma level 0.034
Q1 1 0.0120 0.4263 0.9248 11.00000 0.05 0.22
Q2 1 0.1853 0.2635 0.8580 11.00000 0.05 0.22
Q3 1 0.3987 0.2246 0.8035 11.00000 0.05 0.20
Q4 1 0.2867 0.0952 0.4303 11.00000 0.05 0.19
Q5 1 0.1167 0.3148 0.8201 11.00000 0.05 0.18
Q6 1 0.8230 0.0363 0.8982 11.00000 0.05 0.17
Q7 1 0.0703 0.1832 1.0436 11.00000 0.05 0.17
Q8 1 0.3208 0.2288 0.8529 11.00000 0.05 0.16
Q9 1 0.1725 0.1856 0.9990 11.00000 0.05 0.16
Q10 1 0.3242 0.1246 0.5708 11.00000 0.05 0.16
;
_shelx_res_checksum 71048
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.37718(19) 0.22936(11) 0.76887(7) 0.0156(3) Uani d 1 . .
H H1 0.305463 0.178029 0.753220 0.019 Uiso calc 1 . .
C C2 0.4117(2) 0.21801(10) 0.83539(6) 0.0152(3) Uani d 1 . .
H H2 0.493541 0.266236 0.850011 0.018 Uiso calc 1 . .
C C3 0.2315(2) 0.22186(10) 0.86723(6) 0.0155(3) Uani d 1 . .
H H3 0.156595 0.168623 0.856807 0.019 Uiso calc 1 . .
C C4 0.1309(2) 0.30765(11) 0.85211(7) 0.0161(3) Uani d 1 . .
H H4 0.008592 0.307059 0.870571 0.019 Uiso calc 1 . .
C C5 0.1138(2) 0.31552(11) 0.78568(7) 0.0171(3) Uani d 1 . .
H H5 0.036670 0.265711 0.770640 0.020 Uiso calc 1 . .
C C6 0.0386(2) 0.40350(11) 0.76458(8) 0.0216(3) Uani d 1 . .
H H6A 0.115147 0.453474 0.778348 0.026 Uiso calc 1 . .
H H6B 0.034706 0.404828 0.721102 0.026 Uiso calc 1 . .
C C7 0.6716(2) 0.12912(12) 0.85530(7) 0.0200(3) Uani d 1 . .
C C8 0.7317(3) 0.03574(13) 0.86753(10) 0.0334(4) Uani d 1 . .
H H8A 0.706042 0.020803 0.908620 0.050 Uiso calc 1 . .
H H8B 0.861516 0.030769 0.860319 0.050 Uiso calc 1 . .
H H8C 0.666942 -0.005650 0.841684 0.050 Uiso calc 1 . .
C C9 0.1561(2) 0.17554(11) 0.96477(7) 0.0187(3) Uani d 1 . .
C C10 0.1830(2) 0.20009(13) 1.02771(7) 0.0250(4) Uani d 1 . .
H H10A 0.304948 0.223927 1.033097 0.038 Uiso calc 1 . .
H H10B 0.167381 0.146942 1.052348 0.038 Uiso calc 1 . .
H H10C 0.094493 0.245531 1.039034 0.038 Uiso calc 1 . .
C C11 0.1819(2) 0.41827(11) 0.92639(8) 0.0216(3) Uani d 1 . .
C C12 0.3057(3) 0.49040(12) 0.94585(8) 0.0252(4) Uani d 1 . .
H H12A 0.395173 0.465700 0.973058 0.038 Uiso calc 1 . .
H H12B 0.236442 0.537242 0.965739 0.038 Uiso calc 1 . .
H H12C 0.367223 0.515843 0.911615 0.038 Uiso calc 1 . .
C C13 -0.2346(2) 0.48187(11) 0.76775(8) 0.0227(3) Uani d 1 . .
C C14 -0.4219(3) 0.48203(13) 0.79244(10) 0.0317(4) Uani d 1 . .
H H14A -0.489544 0.431364 0.776357 0.048 Uiso calc 1 . .
H H14B -0.482462 0.537927 0.781767 0.048 Uiso calc 1 . .
H H14C -0.416279 0.476901 0.835333 0.048 Uiso calc 1 . .
C C15 0.5619(2) 0.20451(10) 0.65955(7) 0.0158(3) Uani d 1 . .
C C16 0.8689(2) 0.19724(12) 0.65229(7) 0.0199(3) Uani d 1 . .
C C21 0.3689(2) 0.16701(11) 0.57631(7) 0.0167(3) Uani d 1 . .
C C22 0.4604(2) 0.20567(12) 0.52972(7) 0.0208(3) Uani d 1 . .
H H22 0.543454 0.252860 0.536484 0.025 Uiso calc 1 . .
C C23 0.4295(2) 0.17480(12) 0.47293(7) 0.0222(3) Uani d 1 . .
H H23 0.494441 0.200514 0.441181 0.027 Uiso calc 1 . .
C C24 0.3057(2) 0.10719(11) 0.46157(7) 0.0213(3) Uani d 1 . .
C C25 0.2134(2) 0.06982(12) 0.50901(7) 0.0212(3) Uani d 1 . .
H H25 0.128093 0.023630 0.502222 0.025 Uiso calc 1 . .
C C26 0.2446(2) 0.09925(11) 0.56614(7) 0.0194(3) Uani d 1 . .
H H26 0.181204 0.073110 0.598069 0.023 Uiso calc 1 . .
C C27 0.2696(3) 0.07577(14) 0.39966(8) 0.0294(4) Uani d 1 . .
H H27A 0.259841 0.010468 0.399217 0.044 Uiso calc 1 . .
H H27B 0.368852 0.094415 0.374026 0.044 Uiso calc 1 . .
H H27C 0.156622 0.102027 0.385524 0.044 Uiso calc 1 . .
S S1 0.59563(5) 0.23477(3) 0.73360(2) 0.01751(9) Uani d 1 . .
O O1 0.28768(14) 0.31131(7) 0.75791(5) 0.0168(2) Uani d 1 . .
O O2 0.48915(15) 0.13193(8) 0.84639(5) 0.0178(2) Uani d 1 . .
O O3 0.26977(15) 0.22223(8) 0.92923(5) 0.0185(2) Uani d 1 . .
O O4 0.23369(15) 0.38296(7) 0.87375(5) 0.0173(2) Uani d 1 . .
O O6 -0.14007(16) 0.41167(8) 0.78826(6) 0.0237(3) Uani d 1 . .
O O7 0.76611(16) 0.19387(9) 0.85272(5) 0.0235(3) Uani d 1 . .
O O8 0.0469(2) 0.12371(10) 0.94639(6) 0.0324(3) Uani d 1 . .
O O9 0.0531(2) 0.39229(10) 0.95357(7) 0.0355(3) Uani d 1 . .
O O10 -0.17244(19) 0.53560(9) 0.73424(7) 0.0325(3) Uani d 1 . .
N N1 0.39897(18) 0.19627(9) 0.63588(6) 0.0174(3) Uani d 1 . .
H H01 0.302(3) 0.2023(15) 0.6577(10) 0.028(6) Uiso d 1 . .
N N2 0.70775(18) 0.19009(10) 0.62802(6) 0.0185(3) Uani d 1 . .
N N3 1.0174(2) 0.20304(12) 0.66802(6) 0.0267(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 0.0132(7) 0.0195(7) 0.0143(6) 0.0002(6) 0.0015(5) -0.0016(6)
C2 0.0140(7) 0.0164(7) 0.0153(7) 0.0020(6) 0.0000(6) -0.0018(5)
C3 0.0149(7) 0.0199(7) 0.0119(6) -0.0012(6) 0.0003(5) -0.0012(5)
C4 0.0125(7) 0.0180(7) 0.0178(7) -0.0019(6) 0.0009(5) -0.0029(6)
C5 0.0124(7) 0.0211(7) 0.0177(7) 0.0003(6) 0.0002(6) -0.0003(6)
C6 0.0156(7) 0.0249(8) 0.0242(8) 0.0016(6) 0.0002(6) 0.0027(7)
C7 0.0166(7) 0.0266(9) 0.0167(7) 0.0031(7) -0.0026(6) -0.0040(6)
C8 0.0270(9) 0.0255(9) 0.0476(11) 0.0081(7) -0.0101(9) -0.0044(8)
C9 0.0157(7) 0.0229(8) 0.0176(7) 0.0033(6) 0.0018(6) 0.0026(6)
C10 0.0215(8) 0.0375(9) 0.0161(7) 0.0034(7) 0.0011(6) 0.0003(7)
C11 0.0224(8) 0.0205(8) 0.0219(8) 0.0011(7) 0.0015(7) -0.0047(6)
C12 0.0290(9) 0.0224(8) 0.0243(8) -0.0034(7) -0.0028(7) -0.0041(7)
C13 0.0202(8) 0.0193(7) 0.0287(8) 0.0027(6) -0.0057(7) -0.0050(7)
C14 0.0193(9) 0.0263(9) 0.0494(11) 0.0034(7) -0.0007(8) -0.0064(8)
C15 0.0142(7) 0.0178(7) 0.0155(7) 0.0002(6) -0.0001(6) 0.0005(6)
C16 0.0166(8) 0.0304(8) 0.0127(7) 0.0013(7) 0.0030(6) -0.0040(6)
C21 0.0127(7) 0.0212(8) 0.0161(7) 0.0028(6) -0.0020(6) -0.0005(6)
C22 0.0162(7) 0.0257(8) 0.0206(8) -0.0033(6) -0.0034(6) 0.0023(6)
C23 0.0186(8) 0.0312(9) 0.0167(7) -0.0003(7) -0.0013(6) 0.0047(6)
C24 0.0192(8) 0.0255(8) 0.0193(8) 0.0046(7) -0.0028(6) -0.0015(6)
C25 0.0180(8) 0.0229(8) 0.0228(8) 0.0000(7) -0.0027(6) -0.0021(6)
C26 0.0149(7) 0.0236(8) 0.0197(7) 0.0000(6) 0.0003(6) 0.0007(6)
C27 0.0328(10) 0.0346(10) 0.0210(8) 0.0002(8) -0.0038(8) -0.0037(7)
S1 0.01212(16) 0.02639(18) 0.01402(15) -0.00190(14) 0.00099(13) -0.00383(14)
O1 0.0138(5) 0.0192(5) 0.0174(5) 0.0005(4) 0.0012(4) 0.0011(4)
O2 0.0156(5) 0.0184(6) 0.0194(5) 0.0016(4) -0.0014(4) -0.0005(4)
O3 0.0168(5) 0.0263(6) 0.0123(5) -0.0028(5) 0.0005(4) -0.0010(4)
O4 0.0157(5) 0.0182(5) 0.0181(5) -0.0022(4) 0.0004(4) -0.0032(4)
O6 0.0149(6) 0.0233(6) 0.0329(6) 0.0027(5) 0.0007(5) 0.0042(5)
O7 0.0167(5) 0.0289(6) 0.0248(6) -0.0009(5) -0.0029(5) -0.0015(5)
O8 0.0355(8) 0.0406(8) 0.0210(6) -0.0190(6) -0.0005(5) 0.0048(5)
O9 0.0311(7) 0.0386(8) 0.0367(7) -0.0096(6) 0.0157(6) -0.0168(6)
O10 0.0309(7) 0.0272(6) 0.0394(7) 0.0075(5) 0.0010(6) 0.0071(6)
N1 0.0119(6) 0.0248(7) 0.0156(6) 0.0003(5) 0.0006(5) -0.0016(5)
N2 0.0119(6) 0.0283(7) 0.0154(6) 0.0005(5) -0.0009(5) -0.0028(5)
N3 0.0148(7) 0.0465(9) 0.0187(7) 0.0009(7) 0.0006(5) -0.0054(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'
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
O1 C1 C2 . . 110.21(12) ?
O1 C1 S1 . . 107.63(10) ?
C2 C1 S1 . . 106.90(10) ?
O1 C1 H1 . . 110.7 ?
C2 C1 H1 . . 110.7 ?
S1 C1 H1 . . 110.7 ?
O2 C2 C3 . . 107.65(12) ?
O2 C2 C1 . . 109.67(12) ?
C3 C2 C1 . . 108.45(12) ?
O2 C2 H2 . . 110.3 ?
C3 C2 H2 . . 110.3 ?
C1 C2 H2 . . 110.3 ?
O3 C3 C2 . . 107.07(12) ?
O3 C3 C4 . . 108.34(12) ?
C2 C3 C4 . . 110.77(12) ?
O3 C3 H3 . . 110.2 ?
C2 C3 H3 . . 110.2 ?
C4 C3 H3 . . 110.2 ?
O4 C4 C5 . . 108.77(13) ?
O4 C4 C3 . . 108.72(12) ?
C5 C4 C3 . . 109.29(12) ?
O4 C4 H4 . . 110.0 ?
C5 C4 H4 . . 110.0 ?
C3 C4 H4 . . 110.0 ?
O1 C5 C6 . . 103.30(12) ?
O1 C5 C4 . . 110.99(12) ?
C6 C5 C4 . . 114.51(14) ?
O1 C5 H5 . . 109.3 ?
C6 C5 H5 . . 109.3 ?
C4 C5 H5 . . 109.3 ?
O6 C6 C5 . . 107.22(13) ?
O6 C6 H6A . . 110.3 ?
C5 C6 H6A . . 110.3 ?
O6 C6 H6B . . 110.3 ?
C5 C6 H6B . . 110.3 ?
H6A C6 H6B . . 108.5 ?
O7 C7 O2 . . 123.14(16) ?
O7 C7 C8 . . 126.27(16) ?
O2 C7 C8 . . 110.58(15) ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O8 C9 O3 . . 122.97(15) ?
O8 C9 C10 . . 125.85(16) ?
O3 C9 C10 . . 111.15(14) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
O9 C11 O4 . . 123.36(16) ?
O9 C11 C12 . . 124.96(16) ?
O4 C11 C12 . . 111.67(15) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
O10 C13 O6 . . 122.86(16) ?
O10 C13 C14 . . 126.39(17) ?
O6 C13 C14 . . 110.75(15) ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
N2 C15 N1 . . 120.77(14) ?
N2 C15 S1 . . 116.54(12) ?
N1 C15 S1 . . 122.69(12) ?
N3 C16 N2 . . 173.22(16) ?
C22 C21 C26 . . 120.15(15) ?
C22 C21 N1 . . 121.13(14) ?
C26 C21 N1 . . 118.72(14) ?
C21 C22 C23 . . 119.44(15) ?
C21 C22 H22 . . 120.3 ?
C23 C22 H22 . . 120.3 ?
C24 C23 C22 . . 121.54(15) ?
C24 C23 H23 . . 119.2 ?
C22 C23 H23 . . 119.2 ?
C23 C24 C25 . . 118.15(15) ?
C23 C24 C27 . . 121.17(16) ?
C25 C24 C27 . . 120.67(16) ?
C26 C25 C24 . . 120.94(16) ?
C26 C25 H25 . . 119.5 ?
C24 C25 H25 . . 119.5 ?
C21 C26 C25 . . 119.78(15) ?
C21 C26 H26 . . 120.1 ?
C25 C26 H26 . . 120.1 ?
C24 C27 H27A . . 109.5 ?
C24 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C24 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C15 S1 C1 . . 106.58(7) ?
C1 O1 C5 . . 112.40(11) ?
C7 O2 C2 . . 116.73(13) ?
C9 O3 C3 . . 117.27(12) ?
C11 O4 C4 . . 116.87(12) ?
C13 O6 C6 . . 114.65(14) ?
C15 N1 C21 . . 123.34(13) ?
C15 N1 H01 . . 120.3(15) ?
C21 N1 H01 . . 116.0(15) ?
C15 N2 C16 . . 120.18(13) ?
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 O1 . 1.4168(19) ?
C1 C2 . 1.545(2) ?
C1 S1 . 1.8105(15) ?
C1 H1 . 1.0000 ?
C2 O2 . 1.4325(18) ?
C2 C3 . 1.522(2) ?
C2 H2 . 1.0000 ?
C3 O3 . 1.4391(17) ?
C3 C4 . 1.524(2) ?
C3 H3 . 1.0000 ?
C4 O4 . 1.4472(18) ?
C4 C5 . 1.522(2) ?
C4 H4 . 1.0000 ?
C5 O1 . 1.4382(18) ?
C5 C6 . 1.508(2) ?
C5 H5 . 1.0000 ?
C6 O6 . 1.436(2) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 O7 . 1.198(2) ?
C7 O2 . 1.370(2) ?
C7 C8 . 1.493(2) ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 O8 . 1.197(2) ?
C9 O3 . 1.362(2) ?
C9 C10 . 1.492(2) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 O9 . 1.203(2) ?
C11 O4 . 1.364(2) ?
C11 C12 . 1.485(2) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 O10 . 1.200(2) ?
C13 O6 . 1.347(2) ?
C13 C14 . 1.499(3) ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C15 N2 . 1.316(2) ?
C15 N1 . 1.329(2) ?
C15 S1 . 1.7628(16) ?
C16 N3 . 1.162(2) ?
C16 N2 . 1.322(2) ?
C21 C22 . 1.385(2) ?
C21 C26 . 1.390(2) ?
C21 N1 . 1.442(2) ?
C22 C23 . 1.391(2) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.390(2) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.396(2) ?
C24 C27 . 1.509(2) ?
C25 C26 . 1.392(2) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
N1 H01 . 0.88(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
N1 H01 N3 1_455 0.88(2) 2.13(2) 2.926(2) 151(2) yes
C14 H14A O1 1_455 0.98 2.48 3.433(2) 165.0 yes
C4 H4 O7 1_455 1.00 2.50 3.1976(19) 126.1 yes
C5 H5 N3 1_455 1.00 2.52 3.243(2) 128.8 yes
C1 H1 O10 3_546 1.00 2.37 3.274(2) 150.6 yes
C25 H25 O9 3_546 0.95 2.59 3.420(2) 146.8 yes
C10 H10A O9 4_557 0.98 2.55 3.103(2) 115.6 yes
C10 H10C O3 4_457 0.98 2.56 3.423(2) 146.7 yes
C12 H12A O8 4_557 0.98 2.53 3.483(2) 163.2 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
O1 C1 C2 O2 . . . . 175.42(11) ?
S1 C1 C2 O2 . . . . -67.89(14) ?
O1 C1 C2 C3 . . . . 58.12(16) ?
S1 C1 C2 C3 . . . . 174.81(10) ?
O2 C2 C3 O3 . . . . 68.36(15) ?
C1 C2 C3 O3 . . . . -173.05(12) ?
O2 C2 C3 C4 . . . . -173.70(12) ?
C1 C2 C3 C4 . . . . -55.11(16) ?
O3 C3 C4 O4 . . . . 52.97(15) ?
C2 C3 C4 O4 . . . . -64.20(15) ?
O3 C3 C4 C5 . . . . 171.55(12) ?
C2 C3 C4 C5 . . . . 54.39(16) ?
O4 C4 C5 O1 . . . . 62.77(16) ?
C3 C4 C5 O1 . . . . -55.79(16) ?
O4 C4 C5 C6 . . . . -53.70(17) ?
C3 C4 C5 C6 . . . . -172.26(13) ?
O1 C5 C6 O6 . . . . 177.48(12) ?
C4 C5 C6 O6 . . . . -61.70(17) ?
C26 C21 C22 C23 . . . . -1.3(2) ?
N1 C21 C22 C23 . . . . 179.15(15) ?
C21 C22 C23 C24 . . . . 1.4(3) ?
C22 C23 C24 C25 . . . . -0.7(3) ?
C22 C23 C24 C27 . . . . 178.40(17) ?
C23 C24 C25 C26 . . . . -0.1(3) ?
C27 C24 C25 C26 . . . . -179.24(16) ?
C22 C21 C26 C25 . . . . 0.5(2) ?
N1 C21 C26 C25 . . . . -179.94(15) ?
C24 C25 C26 C21 . . . . 0.2(3) ?
N2 C15 S1 C1 . . . . -169.42(13) ?
N1 C15 S1 C1 . . . . 10.56(16) ?
O1 C1 S1 C15 . . . . -83.79(11) ?
C2 C1 S1 C15 . . . . 157.82(10) ?
C2 C1 O1 C5 . . . . -61.91(15) ?
S1 C1 O1 C5 . . . . -178.15(9) ?
C6 C5 O1 C1 . . . . -175.75(13) ?
C4 C5 O1 C1 . . . . 61.07(16) ?
O7 C7 O2 C2 . . . . -2.0(2) ?
C8 C7 O2 C2 . . . . 178.69(14) ?
C3 C2 O2 C7 . . . . -141.14(13) ?
C1 C2 O2 C7 . . . . 101.05(15) ?
O8 C9 O3 C3 . . . . 12.5(2) ?
C10 C9 O3 C3 . . . . -165.64(13) ?
C2 C3 O3 C9 . . . . -142.40(13) ?
C4 C3 O3 C9 . . . . 98.09(15) ?
O9 C11 O4 C4 . . . . -3.1(2) ?
C12 C11 O4 C4 . . . . 175.72(14) ?
C5 C4 O4 C11 . . . . 142.86(14) ?
C3 C4 O4 C11 . . . . -98.22(15) ?
O10 C13 O6 C6 . . . . -3.0(2) ?
C14 C13 O6 C6 . . . . 176.98(14) ?
C5 C6 O6 C13 . . . . -172.35(14) ?
N2 C15 N1 C21 . . . . 3.4(2) ?
S1 C15 N1 C21 . . . . -176.61(12) ?
C22 C21 N1 C15 . . . . -50.1(2) ?
C26 C21 N1 C15 . . . . 130.35(17) ?
N1 C15 N2 C16 . . . . -179.01(17) ?
S1 C15 N2 C16 . . . . 1.0(2) ?