#------------------------------------------------------------------------------
#$Date: 2025-05-03 21:19:38 +0200 (Sat, 03 May 2025) $
#$Revision: 299517 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023422.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_2023422
loop_
_publ_author_name
'Mohamed-Ezzat, Reham A'
'Kariuki, Benson M.'
'Al-Ashmawy, Aisha A K'
'Srour, Aladdin M.'
_publ_section_title
;
Synthesis and crystal structure of
5-{(E)-[(1H-indol-3-ylformamido)-imino]-meth-yl}-2-meth-oxy-phenyl
propane-1-sulfonate.
;
_journal_coeditor_code JP2017
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 310
_journal_page_last 313
_journal_paper_doi 10.1107/S2056989025002087
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C20 H21 N3 O5 S'
_chemical_formula_moiety 'C20 H21 N3 O5 S'
_chemical_formula_sum 'C20 H21 N3 O5 S'
_chemical_formula_weight 415.46
_chemical_name_systematic
;
5-{(E)-[(1H-Indol-3-ylformamido)imino]methyl}-2-methoxyphenyl
propane-1-sulfonate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 29
_space_group_name_Hall 'P 2c -2ac'
_space_group_name_H-M_alt 'P c a 21'
_atom_sites_solution_hydrogens mixed
_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 9.2969(5)
_cell_length_b 14.0662(7)
_cell_length_c 15.1168(7)
_cell_measurement_reflns_used 7123
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 28.6400
_cell_measurement_theta_min 3.8590
_cell_volume 1976.85(17)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 10.5082
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0274
_diffrn_reflns_av_unetI/netI 0.0291
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 16123
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.722
_diffrn_reflns_theta_min 3.633
_exptl_absorpt_coefficient_mu 0.202
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.618
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.396
_exptl_crystal_description block
_exptl_crystal_F_000 872
_exptl_crystal_size_max 0.340
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_min 0.090
_refine_diff_density_max 0.226
_refine_diff_density_min -0.233
_refine_ls_abs_structure_details
;
Flack x determined using 1389 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.05(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 272
_refine_ls_number_reflns 4696
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.052
_refine_ls_R_factor_all 0.0591
_refine_ls_R_factor_gt 0.0427
_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^)+(0.0461P)^2^+0.6044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1000
_refine_ls_wR_factor_ref 0.1109
_reflns_number_gt 3791
_reflns_number_total 4696
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jp2017.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023422.cif.'
_cod_database_code 2023422
_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 0.935
_shelx_estimated_absorpt_t_max 0.982
_shelx_hkl_file
;
0 0 -20 1278.80 215.758 5
0 0 -19 208.506 95.8334 5
0 0 -18 616.622 138.909 5
0 0 -17 491.293 125.852 5
0 0 -16 8182.32 423.031 5
0 0 -15 1101.15 157.383 5
0 0 -14 5237.64 307.573 5
0 0 -13 2071.56 191.758 5
0 0 -12 17090.9 492.999 5
0 0 -11 1384.15 146.142 5
0 0 -10 41206.8 679.722 5
0 0 -8 4556.52 199.415 5
0 0 -8 4132.98 153.679 4
0 0 -7 240.691 57.8191 5
0 0 -7 425.529 112.800 3
0 0 -7 264.759 43.5042 4
0 0 -6 28285.9 419.340 5
0 0 -6 28273.0 337.196 4
0 0 -6 28209.1 667.348 3
0 0 -5 85.0912 36.6326 5
0 0 -5 98.2173 25.8320 4
0 0 -5 107.855 61.3932 3
0 0 -4 244069. 989.450 5
0 0 -4 240761. 787.952 4
0 0 -4 241725. 1589.79 3
0 0 -3 10.7150 16.2619 5
0 0 -3-6.76673 31.7055 3
0 0 -3 16.4016 12.1405 4
0 0 3 61.8904 36.6594 2
0 0 3 37.0713 19.4461 5
0 0 3 23.2233 12.5858 4
0 0 4 242995. 1435.93 2
0 0 4 238915. 976.682 5
0 0 4 248422. 752.401 4
0 0 4 240033. 1654.48 3
0 0 5 118.272 79.8952 3
0 0 5 93.0543 49.8650 2
0 0 5 61.7140 31.9198 5
0 0 5 48.1357 19.0532 4
0 0 6 27686.6 600.787 2
0 0 6 26855.5 407.599 5
0 0 6 27264.5 694.011 3
0 0 6 27413.8 308.130 4
0 0 7 62.7933 33.4455 5
0 0 7 181.862 28.2519 1
0 0 7 183.134 70.5681 2
0 0 8 4093.72 273.727 2
0 0 8 3978.87 112.437 1
0 0 8 4092.14 188.626 5
0 0 9 112.562 26.1773 1
0 0 9 99.9298 62.5906 2
0 0 9 25.7460 33.0832 5
0 0 10 41647.8 981.489 2
0 0 10 40024.8 390.721 1
0 0 10 39607.8 660.795 5
0 0 10 40521.1 1127.94 3
0 0 11 1602.62 209.782 2
0 0 11 958.242 117.369 5
0 0 11 1816.04 87.0849 1
0 0 12 18930.1 731.225 2
0 0 12 17541.1 253.896 1
0 0 12 17082.0 491.447 5
0 1 -21-188.907 108.589 5
0 1 -20 15.1491 71.5002 5
0 -1 -20-266.038 118.001 5
0 -1 -19-143.798 93.6221 5
0 1 -19 72.5131 77.0257 5
0 -1 -18 56.9552 56.5721 5
0 1 -18 89.3646 63.1007 5
0 1 -17-34.3472 66.8206 5
0 -1 -17-33.0126 60.7909 5
0 1 -16-50.0439 71.2315 5
0 -1 -16 24.3186 67.1504 5
0 -1 -15-12.6159 62.0267 5
0 1 -15-19.7679 59.8269 5
0 1 -14 340.968 87.7633 5
0 -1 -14 357.270 94.4390 5
0 -1 -13-63.3509 78.6255 5
0 1 -13 8.51026 50.0707 5
0 -1 -12 2313.88 190.937 5
0 1 -12 2190.43 176.689 5
0 1 -11-78.8069 55.4825 5
0 -1 -11-18.4543 46.0666 5
0 -1 -11 2.12130 74.4640 3
0 -1 -10 4345.13 229.234 5
0 -1 -10 4044.79 338.059 3
0 1 -9-40.9359 32.1279 4
0 -1 -9-69.5205 79.4669 3
0 1 -8 3232.83 163.335 5
0 -1 -8 3454.81 281.684 3
0 1 -8 3003.95 143.292 4
0 -1 -7 58.2507 42.0955 5
0 1 -7 4.22651 28.0818 5
0 -1 -7-32.6695 60.2486 3
0 1 -7-4.69578 21.7615 4
0 1 -6 7472.77 309.898 2
0 1 -6 7761.68 211.140 5
0 -1 -6 7811.17 231.239 5
0 -1 -6 7047.73 346.567 3
0 1 -6 7546.41 194.714 4
0 -1 -5 9.69439 52.7854 3
0 1 -5-42.8839 58.2072 2
0 -1 -5 14.6132 25.2194 5
0 1 -5 43.8156 29.8015 5
0 1 -5-0.46153 18.3246 4
0 1 -4 130192. 1040.83 2
0 1 -4 130780. 673.711 5
0 1 -4 131253. 681.332 4
0 -1 -4 129311. 1250.22 3
0 1 -3 27.2856 33.9115 2
0 1 -3 16.1558 17.4721 5
0 1 -3-11.0076 15.6620 4
0 -1 3 23.9413 23.4863 2
0 -1 3 12.7218 12.7348 5
0 1 3 75.5620 29.5651 5
0 -1 3-12.2687 19.2142 4
0 -1 4 128709. 1028.84 2
0 -1 4 127218. 662.821 5
0 1 4 129935. 773.992 5
0 -1 4 131772. 661.849 4
0 -1 5 31.6417 35.0182 2
0 -1 5-3.86913 20.2329 5
0 1 5-3.30495 26.9469 5
0 -1 5-19.3661 44.6986 3
0 -1 5 10.5943 23.5135 4
0 -1 6 7634.72 311.569 2
0 1 6 7493.62 316.754 2
0 -1 6 7256.33 200.667 5
0 1 6 7533.45 225.835 5
0 -1 6 7709.06 186.940 4
0 -1 7-63.8512 55.2950 2
0 1 7 29.6483 43.9654 2
0 1 7 13.3064 21.5636 5
0 -1 7 0.09051 23.1753 5
0 -1 7-0.35134 23.4794 4
0 -1 8 3213.36 238.620 2
0 1 8 3266.91 176.854 5
0 -1 8 3218.64 160.457 5
0 1 8 3336.43 247.762 2
0 -1 9 17.2197 63.6496 3
0 -1 9 4.13216 21.0267 1
0 1 9 20.5762 49.3549 2
0 -1 9 3.77607 51.6353 2
0 -1 9 29.1775 36.1504 5
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0 1 10 4083.23 312.225 2
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0 -1 10 3875.97 150.584 1
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0 -1 10 3810.01 201.319 5
0 -1 10 3787.25 355.967 3
0 -1 11-32.5336 95.9695 3
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0 -1 11-40.3695 83.8924 2
0 -1 11-2.25113 24.2616 1
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0 -1 11-39.2383 46.6055 5
0 -1 12 2652.10 276.716 2
0 -1 12 2308.14 124.840 1
0 1 12 2483.23 192.127 5
0 -1 12 2427.24 181.274 5
0 -1 12 2560.91 331.543 3
0 -1 13 33.8379 99.7381 3
0 -1 13-26.1165 28.3356 1
0 -1 13-52.9076 47.6008 5
0 -1 14 341.258 54.2472 1
0 2 -20 544.847 150.741 5
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0 -2 -19-45.8323 76.1737 5
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0 2 -18 1556.79 207.448 5
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0 2 -17-42.7522 67.1255 5
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0 -2 -15-39.0463 79.4050 5
0 2 -15 3.04454 52.1323 5
0 -2 -14 1391.89 167.301 5
0 2 -14 1522.14 165.618 5
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0 -2 -11-16.4489 97.5203 3
0 -2 -10 21448.7 514.593 5
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0 -2 -9-30.2745 47.9327 5
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0 2 -9 20.4704 26.3160 4
0 -2 -9-18.1720 50.1580 3
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0 -2 -7 86.3167 69.4863 3
0 2 -7-36.6482 58.3587 2
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0 2 -7 12.9101 24.2714 4
0 2 -6 57308.1 853.716 2
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0 -2 -6 57003.6 1040.45 3
0 2 -6 58292.3 592.109 4
0 2 -5-10.3495 48.8288 2
0 2 -5 100.546 34.6650 5
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0 2 -4 256841. 1489.52 2
0 2 -4 260066. 881.459 5
0 2 -4 253042. 1079.96 4
0 2 -3-21.0038 34.5926 2
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0 -2 2 79692.1 641.787 2
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0 -2 3 5.73148 28.7070 2
0 -2 3-5.21534 11.4814 5
0 -2 3 10.8954 21.9042 4
0 -2 4 253557. 1459.00 2
0 2 4 252124. 1154.55 5
0 2 5 38.2859 39.6175 5
0 -2 5 29.1716 19.9124 5
0 -2 5-3.26213 27.4476 4
0 -2 6 56728.6 838.299 2
0 -2 6 57237.6 530.366 5
0 2 6 58119.6 655.577 5
0 -2 6 58819.3 573.944 4
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0 2 7 1.05724 24.7529 5
0 -2 7-15.4760 23.8775 5
0 -2 7-20.1800 36.6920 4
0 -2 8 44639.9 871.667 2
0 -2 8 44248.6 565.431 5
0 2 8 45885.4 677.116 5
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0 -2 9 23.2448 28.9730 5
0 -2 9-101.860 96.4389 3
0 -2 10 21781.5 693.032 2
0 -2 10 20858.3 393.176 1
0 2 10 21288.3 715.688 2
0 2 10 22432.4 528.728 5
0 -2 10 20557.2 446.183 5
0 -2 10 21804.7 829.516 3
0 -2 11-67.2094 72.2094 2
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0 2 11-34.9475 67.6058 2
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0 -2 11-19.0164 37.4029 5
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0 -2 12 13105.7 336.767 1
0 -2 12 12659.0 398.685 5
0 -2 12 13049.1 729.080 3
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0 -2 13-49.8593 48.2476 5
0 -2 13 52.8870 37.3398 1
0 -2 14 1383.83 281.414 3
0 -2 14 1574.96 126.089 1
0 -2 15-418.802 218.428 3
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0 3 -19-7.87899 80.2374 5
0 -3 -19 41.8079 80.4244 5
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0 -3 -18 668.467 149.322 5
0 3 -17 14.2095 72.1309 5
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0 3 -15-15.4244 48.0239 5
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0 3 -14 1213.73 145.421 5
0 3 -13 8.85680 51.8071 5
0 -3 -13 30.6766 63.5577 5
0 3 -12 14583.6 433.171 5
0 -3 -12 14587.8 483.631 5
0 -3 -11 2.16344 66.0532 5
0 -3 -11-31.8012 93.2320 3
0 3 -11 26.4330 35.9363 4
0 3 -10 7379.05 407.001 2
0 -3 -10 7555.98 315.225 5
0 3 -10 7483.82 288.165 4
0 -3 -10 7945.12 503.977 3
0 -3 -9-40.0273 81.4811 3
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0 3 -9-35.0477 43.4332 4
0 3 -8 13282.5 307.539 5
0 -3 -8 12887.8 587.884 3
0 3 -8 12958.8 339.627 4
0 3 -7 27.1564 54.9149 2
0 3 -7 36.4706 33.2806 5
0 3 -7-10.8607 28.9338 4
0 3 -6 59670.4 886.486 2
0 3 -6 57531.3 518.041 5
0 3 -6 54880.5 629.516 4
0 -3 -5 32.1006 14.6274 1
0 3 -5 12.4457 42.6751 2
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0 3 -5 1.12207 20.9013 4
0 3 -4 24189.7 477.220 2
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0 3 -4 24616.1 255.838 5
0 3 -4 23976.7 368.024 4
0 3 -3 1.37148 31.8527 2
0 -3 -3 8.44475 26.8201 5
0 3 -3-7.95564 20.7822 4
0 3 -2 54751.9 594.876 2
0 -3 -2 53002.1 448.573 5
0 3 -2 53851.2 477.163 4
0 3 -1 24.9803 33.8732 2
0 -3 -1-13.8391 18.9019 5
0 3 -1 31.2578 25.3720 4
0 -3 -1 5.74433 14.6768 4
0 -3 0 2786.96 71.1176 5
0 3 0 2272.94 68.0732 5
0 -3 0 2517.61 86.6618 4
0 3 0 2337.62 86.4107 4
0 3 1 7.52969 15.5910 5
0 3 1-2.15175 13.8149 4
0 -3 2 53520.1 588.291 2
0 3 2 52473.1 450.435 5
0 3 2 52640.1 315.847 4
0 -3 3 53.3258 34.3053 2
0 3 3-3.43795 21.3337 5
0 -3 4 24674.6 479.737 2
0 3 4 24339.1 380.122 5
0 -3 4 24013.9 230.320 5
0 -3 4 25443.8 372.732 4
0 -3 5 6.16640 30.5202 2
0 3 5 34.3698 32.6781 5
0 -3 5 8.16013 17.7708 5
0 -3 5-3.06798 29.7394 4
0 -3 6 55884.0 854.851 2
0 -3 6 55042.3 489.604 5
0 3 6 56138.0 677.042 5
0 -3 6 58235.6 623.039 4
0 -3 7-64.3120 55.8962 2
0 -3 7 12.5958 23.2072 5
0 3 7-10.1458 25.7406 5
0 -3 7-26.5828 42.0518 4
0 -3 8 13032.8 472.028 2
0 -3 8 12805.0 290.466 5
0 3 8 13204.7 375.709 5
0 -3 8 13900.6 333.497 4
0 -3 9-4.77149 49.3668 2
0 3 9-12.1328 36.0404 5
0 -3 9-9.90120 25.1114 5
0 -3 9-14.4589 79.0489 3
0 -3 10 7853.26 415.655 2
0 3 10 7377.76 427.258 2
0 3 10 8054.16 328.466 5
0 -3 10 7390.52 257.989 5
0 -3 10 7152.27 479.853 3
0 -3 11-35.9337 54.0826 2
0 3 11 70.6189 59.9426 2
0 -3 11-22.4615 33.5262 1
0 -3 11-49.6259 37.6075 5
0 3 11 1.61643 41.6766 5
0 -3 11-31.2496 105.870 3
0 -3 12 15090.9 640.062 2
0 -3 12 13779.8 377.619 1
0 -3 12 12791.0 389.887 5
0 -3 12 15904.1 799.418 3
0 -3 13-63.2905 83.4999 3
0 -3 13-22.9973 33.4680 5
0 -3 13 36.1747 37.2343 1
0 -3 14 1247.87 269.485 3
0 -3 14 1146.37 135.391 5
0 -3 14 1322.51 131.764 1
0 -3 15 185.843 145.955 3
0 -3 16 410.996 177.686 3
0 -3 17-20.0435 120.389 3
0 4 -19 28.5313 64.7195 5
0 4 -18 1480.73 195.172 5
0 -4 -18 1757.32 237.943 5
0 4 -17-22.9522 53.7890 5
0 -4 -17 1.83543 46.6606 5
0 -4 -16 498.256 131.046 5
0 4 -16 466.133 104.663 5
0 -4 -15-112.704 81.4276 5
0 4 -15 10.5184 60.3924 5
0 -4 -14 5846.41 347.009 5
0 4 -14 5943.66 309.386 5
0 -4 -13 28.7320 59.1730 5
0 4 -13 22.2480 48.1713 5
0 4 -12 4818.61 369.188 2
0 -4 -12 5394.50 302.035 5
0 4 -12 5501.27 284.087 4
0 -4 -11-5.52768 81.7607 3
0 4 -11 12.9750 75.1464 2
0 -4 -11 20.2653 52.7276 5
0 4 -11-1.09942 40.7385 4
0 4 -10 12217.6 525.313 2
0 -4 -10 12320.4 413.217 5
0 4 -10 12426.2 340.458 5
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11 -1 7 221.818 148.572 1
11 1 7 63.2309 112.477 1
11 1 8 1304.46 273.436 1
-11 2 -10 308.051 157.978 2
11 -2 -10 198.714 106.694 1
11 -2 -9 139.121 124.751 1
11 2 -9 298.083 106.749 1
11 -2 -8 107.409 104.460 1
-11 2 -8 435.564 154.039 2
11 2 -8 296.807 131.569 1
-11 2 -7 141.163 87.1220 2
11 2 -7 77.0973 90.5708 1
11 -2 -7 159.086 112.173 1
-11 2 -6 61.8113 93.5227 2
11 2 -6 129.099 113.830 1
11 -2 -6 36.3878 94.1937 1
-11 2 -5 287.214 128.170 2
11 2 -5 347.820 137.317 1
11 -2 -5 276.315 148.155 1
-11 2 -4-3.96056 56.1612 2
11 2 -4 225.070 127.408 1
11 -2 -4 445.862 156.779 1
-11 2 -3 26.8481 61.8876 2
11 2 -3-35.5409 74.1889 1
11 2 -2-67.6061 100.744 1
-11 2 -2 61.5245 51.8116 2
11 2 -1 369.641 153.885 1
11 -2 -1 40.3989 119.124 1
-11 2 -1 301.581 108.010 2
11 -2 0 644.806 198.702 1
11 2 0 519.834 180.442 1
-11 2 0 731.532 150.157 2
11 -2 1 454.258 169.170 1
11 2 1 60.9262 98.2138 1
11 -2 2-74.1617 149.876 1
11 2 2-125.078 143.435 1
11 -2 3-66.0267 148.638 1
11 2 3-175.879 125.773 1
11 -2 4 262.695 155.929 1
11 2 4 254.685 145.064 1
11 -2 5 187.805 110.423 1
11 2 5 503.127 168.572 1
11 -2 6-251.026 150.871 1
11 2 6 93.0073 97.7238 1
11 -2 7 44.0516 121.538 1
11 2 7-84.9922 106.410 1
11 2 8 533.243 198.749 1
11 -3 -10 1826.03 287.334 1
11 -3 -9 137.702 110.545 1
-11 3 -9-7.00826 89.3276 2
-11 3 -8 701.105 201.585 2
11 3 -8 810.332 195.293 1
11 -3 -8 544.713 173.730 1
-11 3 -7 576.822 171.871 2
11 3 -7 487.487 154.266 1
11 -3 -7 382.470 158.940 1
-11 3 -6 157.173 104.354 2
11 3 -6 147.969 110.629 1
11 -3 -6-34.9364 76.8784 1
-11 3 -5 353.475 124.603 2
11 3 -5 442.625 160.348 1
11 -3 -5 441.634 172.434 1
-11 3 -4 448.381 144.866 2
11 3 -4 385.228 147.735 1
11 -3 -4 175.594 114.554 1
11 3 -3 184.258 103.791 1
11 -3 -3 258.827 139.342 1
-11 3 -3 315.135 130.545 2
11 3 -2 1941.37 305.245 1
11 -3 -2 2384.75 346.279 1
-11 3 -2 1902.42 260.077 2
11 3 -1 106.622 106.214 1
11 -3 -1 101.223 132.283 1
-11 3 -1 203.463 102.659 2
11 3 0 1192.82 243.557 1
11 -3 0 1120.00 246.296 1
-11 3 0 976.172 183.554 2
11 3 1 187.931 133.435 1
11 -3 1 20.5204 134.901 1
-11 3 1 32.3432 58.4859 2
11 -3 2 2411.90 367.293 1
11 3 2 2448.98 341.499 1
-11 3 2 2116.54 252.121 2
11 3 3-12.3524 114.796 1
11 -3 3 148.812 123.035 1
11 3 4 351.113 151.356 1
11 -3 4 467.916 168.103 1
11 -3 5 292.557 147.727 1
11 3 5 389.036 170.079 1
11 -3 6 157.218 131.935 1
11 3 6 17.1593 103.983 1
11 3 7 320.281 149.827 1
11 3 8 639.860 189.922 1
11 -4 -10 78.5660 87.9431 1
11 -4 -9-11.2399 106.014 1
-11 4 -8-28.3521 85.4876 2
11 -4 -8-254.526 132.166 1
-11 4 -7-115.554 110.557 2
11 -4 -7 192.848 141.744 1
-11 4 -6 629.201 181.861 2
11 -4 -6 486.859 172.277 1
11 4 -6 384.514 157.345 1
11 -4 -5 1417.52 284.725 1
11 4 -5 1135.21 233.017 1
-11 4 -5 1504.91 260.622 2
11 -4 -4 199.964 146.089 1
11 4 -4 302.150 136.638 1
-11 4 -4 306.165 127.560 2
11 -4 -3 82.9137 105.746 1
11 4 -3 158.212 119.947 1
-11 4 -3 2.14462 75.5659 2
11 -4 -2 361.504 152.156 1
11 4 -2 83.4110 115.316 1
-11 4 -2 208.766 101.955 2
11 -4 -1 306.229 150.560 1
11 4 -1 77.1762 79.6096 1
-11 4 -1 197.992 88.2125 2
11 4 0 241.345 123.912 1
-11 4 0 245.324 124.123 2
11 4 1 56.2573 92.2150 1
11 -4 1 115.266 119.970 1
-11 4 1 143.073 67.0813 2
11 4 2 200.196 124.521 1
11 -4 2 21.3614 124.667 1
-11 4 2 265.589 100.306 2
11 4 3-70.8203 94.6598 1
11 -4 3 34.1818 107.755 1
-11 4 3 26.9941 60.4116 2
11 4 4 341.915 148.360 1
11 4 5 1489.65 262.524 1
11 4 6 584.590 182.697 1
11 4 7 344.141 158.396 1
11 -5 -9 170.439 129.710 1
11 -5 -8 552.156 186.105 1
-11 5 -7 40.4174 82.5344 2
11 -5 -7 236.637 143.166 1
11 -5 -6 136.716 104.294 1
-11 5 -6 16.9024 93.5240 2
11 -5 -5 219.875 131.301 1
-11 5 -5-52.4947 79.2599 2
11 -5 -4 790.087 235.817 1
-11 5 -4 735.189 198.819 2
11 -5 -3 1077.52 255.534 1
11 5 -3 1101.91 218.095 1
-11 5 -3 1283.57 237.934 2
11 5 -2-60.9228 91.2160 1
-11 5 -2 131.936 97.4975 2
11 -5 -1 103.387 102.048 1
11 5 -1 93.3325 98.8015 1
-11 5 -1 47.5058 73.7182 2
11 5 0 632.740 188.585 1
-11 5 0 569.140 159.045 2
11 5 1 128.213 103.158 1
-11 5 1 65.3772 69.9415 2
11 5 2 183.722 119.735 1
-11 5 2 261.957 116.277 2
11 5 3 1318.02 251.589 1
-11 5 3 1139.99 207.590 2
11 5 4 851.719 203.934 1
-11 5 4 916.753 196.102 2
11 5 5 280.766 127.280 1
11 5 6-92.2006 94.0276 1
11 -6 -9 341.240 168.678 1
11 -6 -8 299.325 146.967 1
11 -6 -7-1.39698 78.9085 1
11 -6 -6 201.363 137.138 1
-11 6 -6 181.106 138.985 2
11 -6 -5 438.128 157.042 1
-11 6 -5 381.717 150.908 2
11 -6 -4 382.557 152.650 1
-11 6 -4 517.092 173.702 2
11 -6 -3 32.7574 109.845 1
-11 6 -3-66.0950 96.0168 2
11 -6 -2 310.464 153.044 1
-11 6 -2 195.737 110.531 2
-11 6 -1 234.358 120.936 2
-11 6 0 12.5051 67.7347 2
-11 6 1 319.879 120.609 2
-11 6 2 198.105 71.1307 2
-11 6 3 67.6503 74.3621 2
-11 6 4 875.506 194.211 2
-11 6 5 197.077 97.9062 2
-11 7 -5 598.084 184.707 2
-11 7 -4 637.057 200.556 2
-11 7 -3 191.327 129.629 2
-11 7 -2 249.279 123.871 2
-11 7 -1 1082.58 241.685 2
-11 7 0 10.9473 104.647 2
-11 7 1 235.308 117.798 2
-11 7 2 380.245 135.408 2
-11 7 3 446.510 152.316 2
-11 7 4 639.365 175.818 2
-11 7 5-148.761 102.117 2
-11 8 -3 605.936 186.335 2
-11 8 -2 159.033 112.364 2
-11 8 -1 112.781 95.4971 2
-11 8 0-18.1805 67.0555 2
-11 8 1 222.056 125.264 2
-11 8 2-29.8777 76.7691 2
-11 8 3 339.907 139.901 2
-11 8 4 409.159 130.676 2
-11 8 5-42.1019 74.8223 2
-11 8 6 298.439 128.682 2
-11 9 0-64.4765 83.7947 2
-11 9 1 695.413 201.795 2
-11 9 2 36.9489 71.2060 2
-11 9 3 1233.90 261.329 2
-11 9 4 169.219 142.588 2
-11 9 5 296.682 143.661 2
-12 3 -6-148.355 109.918 2
-12 3 -5-154.493 104.054 2
-12 4 -6 43.3747 86.5528 2
-12 4 -5 625.833 166.270 2
-12 4 -4 179.211 116.115 2
-12 4 -3 423.571 143.824 2
-12 5 -5 833.835 219.341 2
-12 5 -4 104.780 71.4410 2
-12 5 -3 79.5560 84.5465 2
-12 5 -2-52.6418 85.2133 2
-12 6 -4 353.904 157.456 2
-12 6 -3 517.680 171.664 2
-12 6 -2 178.940 107.891 2
-12 6 -1 69.4971 93.8003 2
0 0 0 0.00 0.00 0
TITL bmk2266_auto in Pca2(1)
REM Pca2(1) (#29 in standard setting)
CELL 0.71073 9.296898 14.066152 15.116790 90.0000 90.0000 90.0000
ZERR 8.00 0.000477 0.000679 0.000686 0.0000 0.0000 0.0000
LATT -1
SYMM -x,-y, z+1/2
SYMM x+1/2,-y, z
SYMM -x+1/2, y, z+1/2
SFAC C H N O
UNIT 88.00 80.00 8.00 8.00
SIZE 0.09 0.14 0.34
TREF
HKLF 4
END
;
_shelx_hkl_checksum 88235
_shelx_res_file
;
TITL bmk2266 in Pca2(1)
shelx.res
created by SHELXL-2019/3 at 15:03:18 on 20-Jan-2025
CELL 0.71073 9.2969 14.0662 15.1168 90.000 90.000 90.000
ZERR 4.00 0.0005 0.0007 0.0007 0.000 0.000 0.000
LATT -1
SYMM - X, - Y, 1/2 + Z
SYMM 1/2 + X, - Y, Z
SYMM 1/2 - X, Y, 1/2 + Z
SFAC C H N O S
UNIT 80 84 12 20 4
MERG 2
dfix .86 .01 n1 h1 n2 h2a
EQIV $1 x-1/2, -y+1, z
HTAB C10 O1_$1
EQIV $2 -x+1, -y+1, z-1/2
HTAB C18 O1_$2
HTAB N2 O1_$1
EQIV $3 -x, -y+1, z+1/2
HTAB N1 O4_$3
MPLA C1 C2 C3 C4 C5 C6 C7 C8 N1
MPLA C9 C10 N2 N3 O1
MPLA C11 C12 C13 C14 C15 C16 C17 O2
CONF C20 C19 C18 S1
FMAP 2
PLAN 5
SIZE 0.090 0.140 0.340
ACTA
BOND $H
LIST 4
L.S. 4
TEMP 23.00
WGHT 0.046100 0.604400
FVAR 3.81647
C1 1 -0.065918 0.209447 0.706642 11.00000 0.04294 0.05282 =
0.05275 0.01618 -0.00353 -0.01179
C2 1 -0.084860 0.110907 0.708815 11.00000 0.07471 0.06367 =
0.07085 0.02427 -0.00962 -0.02754
AFIX 43
H2 2 -0.168430 0.084058 0.731600 11.00000 -1.20000
AFIX 0
C3 1 0.023036 0.055578 0.676488 11.00000 0.10012 0.04001 =
0.07434 0.00984 -0.01983 -0.01118
AFIX 43
H3 2 0.013852 -0.010235 0.678105 11.00000 -1.20000
AFIX 0
C4 1 0.145990 0.095642 0.641308 11.00000 0.08275 0.04556 =
0.05875 -0.00606 -0.00633 0.00849
AFIX 43
H4 2 0.218451 0.055961 0.620438 11.00000 -1.20000
AFIX 0
C5 1 0.164470 0.192714 0.636217 11.00000 0.05260 0.04366 =
0.05000 -0.00107 -0.00700 0.00154
AFIX 43
H5 2 0.246976 0.218411 0.610950 11.00000 -1.20000
AFIX 0
C6 1 0.057377 0.251243 0.669587 11.00000 0.03480 0.03975 =
0.03380 0.00504 -0.00446 -0.00362
C7 1 0.036210 0.352961 0.675568 11.00000 0.03103 0.04064 =
0.04129 0.00597 0.00014 0.00160
C8 1 -0.094638 0.366046 0.714939 11.00000 0.03546 0.05344 =
0.05977 0.00794 0.00621 0.00521
AFIX 43
H8 2 -0.136701 0.424788 0.726252 11.00000 -1.20000
AFIX 0
C9 1 0.133167 0.426325 0.643899 11.00000 0.03216 0.03894 =
0.03719 -0.00065 0.00088 0.00041
C10 1 0.087946 0.660720 0.574321 11.00000 0.03419 0.04189 =
0.05891 0.00234 0.00857 -0.00209
AFIX 43
H10 2 -0.007127 0.668033 0.592203 11.00000 -1.20000
AFIX 0
C11 1 0.162951 0.739664 0.532221 11.00000 0.03696 0.03689 =
0.05067 0.00033 0.00360 0.00025
C12 1 0.301725 0.729406 0.498050 11.00000 0.03617 0.03539 =
0.04181 0.00152 -0.00090 0.00495
AFIX 43
H12 2 0.349555 0.671639 0.503558 11.00000 -1.20000
AFIX 0
C13 1 0.367105 0.803729 0.456722 11.00000 0.03240 0.03805 =
0.04254 -0.00368 0.00189 0.00084
C14 1 0.299514 0.891811 0.446498 11.00000 0.04039 0.03168 =
0.05381 -0.00040 0.00336 -0.00171
C15 1 0.162382 0.902293 0.480356 11.00000 0.04331 0.03246 =
0.07053 0.00101 0.00484 0.00562
AFIX 43
H15 2 0.114956 0.960221 0.475005 11.00000 -1.20000
AFIX 0
C16 1 0.095336 0.826708 0.522265 11.00000 0.03504 0.04305 =
0.07237 -0.00133 0.01111 0.00664
AFIX 43
H16 2 0.002673 0.834642 0.544236 11.00000 -1.20000
AFIX 0
C17 1 0.305022 1.049061 0.389462 11.00000 0.06971 0.03393 =
0.07900 0.00917 0.01289 0.00336
AFIX 137
H17A 2 0.219977 1.038851 0.354718 11.00000 -1.50000
H17B 2 0.368862 1.091027 0.358372 11.00000 -1.50000
H17C 2 0.278991 1.077006 0.445144 11.00000 -1.50000
AFIX 0
C18 1 0.697837 0.694900 0.341669 11.00000 0.03935 0.05334 =
0.05413 -0.00205 0.00607 0.00741
AFIX 23
H18A 2 0.728048 0.668857 0.285233 11.00000 -1.20000
H18B 2 0.766370 0.743790 0.358143 11.00000 -1.20000
AFIX 0
C19 1 0.702048 0.617272 0.409911 11.00000 0.07916 0.08865 =
0.06286 0.02080 0.00834 0.03261
AFIX 23
H19A 2 0.691877 0.645464 0.468136 11.00000 -1.20000
H19B 2 0.620706 0.575250 0.400642 11.00000 -1.20000
AFIX 0
C20 1 0.836724 0.560098 0.407695 11.00000 0.10667 0.09670 =
0.07837 0.01845 0.01023 0.05279
AFIX 137
H20A 2 0.841089 0.524917 0.353344 11.00000 -1.50000
H20B 2 0.837658 0.516757 0.456748 11.00000 -1.50000
H20C 2 0.918286 0.601747 0.411564 11.00000 -1.50000
AFIX 0
N1 3 -0.153947 0.280856 0.735031 11.00000 0.03441 0.07114 =
0.07852 0.02237 0.01474 -0.00498
N2 3 0.070041 0.510137 0.622772 11.00000 0.03141 0.03940 =
0.05958 0.00952 0.00670 0.00054
N3 3 0.151863 0.581840 0.586738 11.00000 0.03428 0.03785 =
0.05208 0.00338 0.00456 -0.00258
O1 4 0.264074 0.413536 0.637052 11.00000 0.02967 0.04467 =
0.06422 0.00727 0.00185 -0.00006
O2 4 0.374977 0.960644 0.404495 11.00000 0.05258 0.03565 =
0.07964 0.01056 0.01257 0.00122
O3 4 0.508860 0.792827 0.424813 11.00000 0.03119 0.04688 =
0.04878 -0.00454 0.00420 0.00072
O4 4 0.423603 0.674390 0.317573 11.00000 0.04890 0.09252 =
0.07594 -0.02993 -0.00666 -0.00023
O5 4 0.532730 0.820399 0.265307 11.00000 0.12563 0.09152 =
0.06386 0.02948 0.01965 0.05156
S1 5 0.529152 0.746975 0.328864 11.00000 0.04425 0.05553 =
0.04199 0.00178 0.00155 0.01259
H2A 2 -0.020905 0.519565 0.622353 11.00000 0.05148
H1 2 -0.242945 0.280237 0.750081 11.00000 0.09721
HKLF 4
REM bmk2266 in Pca2(1)
REM wR2 = 0.1109, GooF = S = 1.052, Restrained GooF = 1.052 for all data
REM R1 = 0.0427 for 3791 Fo > 4sig(Fo) and 0.0591 for all 4696 data
REM 272 parameters refined using 3 restraints
END
WGHT 0.0461 0.6045
REM Highest difference peak 0.226, deepest hole -0.233, 1-sigma level 0.042
Q1 1 0.7846 0.6696 0.3998 11.00000 0.05 0.23
Q2 1 0.0429 -0.0909 0.6609 11.00000 0.05 0.21
Q3 1 0.5556 1.0901 0.3319 11.00000 0.05 0.20
Q4 1 0.1972 1.0801 0.3291 11.00000 0.05 0.19
Q5 1 0.4683 0.9154 0.4941 11.00000 0.05 0.19
;
_shelx_res_checksum 64307
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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 -0.0659(4) 0.2094(3) 0.7066(3) 0.0495(9) Uani d 1 . .
C C2 -0.0849(6) 0.1109(3) 0.7088(3) 0.0697(13) Uani d 1 . .
H H2 -0.168430 0.084058 0.731600 0.084 Uiso calc 1 . .
C C3 0.0230(6) 0.0556(3) 0.6765(3) 0.0715(13) Uani d 1 . .
H H3 0.013852 -0.010235 0.678105 0.086 Uiso calc 1 . .
C C4 0.1460(5) 0.0956(3) 0.6413(3) 0.0624(11) Uani d 1 . .
H H4 0.218451 0.055961 0.620438 0.075 Uiso calc 1 . .
C C5 0.1645(4) 0.1927(2) 0.6362(3) 0.0488(8) Uani d 1 . .
H H5 0.246976 0.218411 0.610950 0.059 Uiso calc 1 . .
C C6 0.0574(4) 0.2512(2) 0.6696(2) 0.0361(7) Uani d 1 . .
C C7 0.0362(3) 0.3530(2) 0.6756(2) 0.0377(7) Uani d 1 . .
C C8 -0.0946(4) 0.3660(3) 0.7149(3) 0.0496(8) Uani d 1 . .
H H8 -0.136701 0.424788 0.726252 0.059 Uiso calc 1 . .
C C9 0.1332(3) 0.4263(2) 0.6439(2) 0.0361(6) Uani d 1 . .
C C10 0.0879(4) 0.6607(2) 0.5743(3) 0.0450(8) Uani d 1 . .
H H10 -0.007127 0.668033 0.592203 0.054 Uiso calc 1 . .
C C11 0.1630(4) 0.7397(2) 0.5322(2) 0.0415(7) Uani d 1 . .
C C12 0.3017(3) 0.7294(2) 0.4981(2) 0.0378(7) Uani d 1 . .
H H12 0.349555 0.671639 0.503558 0.045 Uiso calc 1 . .
C C13 0.3671(3) 0.8037(2) 0.4567(2) 0.0377(7) Uani d 1 . .
C C14 0.2995(4) 0.8918(2) 0.4465(2) 0.0420(7) Uani d 1 . .
C C15 0.1624(4) 0.9023(2) 0.4804(3) 0.0488(9) Uani d 1 . .
H H15 0.114956 0.960221 0.475005 0.059 Uiso calc 1 . .
C C16 0.0953(4) 0.8267(2) 0.5223(3) 0.0502(9) Uani d 1 . .
H H16 0.002673 0.834642 0.544236 0.060 Uiso calc 1 . .
C C17 0.3050(5) 1.0491(2) 0.3895(3) 0.0609(11) Uani d 1 . .
H H17A 0.219977 1.038851 0.354718 0.091 Uiso calc 1 . .
H H17B 0.368862 1.091027 0.358372 0.091 Uiso calc 1 . .
H H17C 0.278991 1.077006 0.445144 0.091 Uiso calc 1 . .
C C18 0.6978(4) 0.6949(3) 0.3417(3) 0.0489(9) Uani d 1 . .
H H18A 0.728048 0.668857 0.285233 0.059 Uiso calc 1 . .
H H18B 0.766370 0.743790 0.358143 0.059 Uiso calc 1 . .
C C19 0.7020(5) 0.6173(4) 0.4099(3) 0.0769(14) Uani d 1 . .
H H19A 0.691877 0.645464 0.468136 0.092 Uiso calc 1 . .
H H19B 0.620706 0.575250 0.400642 0.092 Uiso calc 1 . .
C C20 0.8367(6) 0.5601(4) 0.4077(4) 0.0939(18) Uani d 1 . .
H H20A 0.841089 0.524917 0.353344 0.141 Uiso calc 1 . .
H H20B 0.837658 0.516757 0.456748 0.141 Uiso calc 1 . .
H H20C 0.918286 0.601747 0.411564 0.141 Uiso calc 1 . .
N N1 -0.1539(3) 0.2809(3) 0.7350(3) 0.0614(9) Uani d 1 . .
N N2 0.0700(3) 0.5101(2) 0.6228(2) 0.0435(6) Uani d 1 . .
N N3 0.1519(3) 0.58184(19) 0.58674(19) 0.0414(6) Uani d 1 . .
O O1 0.2641(2) 0.41354(16) 0.63705(17) 0.0462(6) Uani d 1 . .
O O2 0.3750(3) 0.96064(16) 0.40450(19) 0.0560(7) Uani d 1 . .
O O3 0.5089(2) 0.79283(17) 0.42481(16) 0.0423(5) Uani d 1 . .
O O4 0.4236(3) 0.6744(2) 0.3176(2) 0.0725(9) Uani d 1 . .
O O5 0.5327(4) 0.8204(3) 0.2653(2) 0.0937(12) Uani d 1 . .
S S1 0.52915(9) 0.74697(7) 0.32886(7) 0.0473(2) Uani d 1 . .
H H2A -0.0209(16) 0.520(3) 0.622(3) 0.051(11) Uiso d 1 . .
H H1 -0.243(2) 0.280(4) 0.750(4) 0.097(17) Uiso 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 0.0429(19) 0.053(2) 0.053(2) -0.0118(17) -0.0035(16) 0.0162(18)
C2 0.075(3) 0.064(3) 0.071(3) -0.028(2) -0.010(2) 0.024(2)
C3 0.100(4) 0.040(2) 0.074(3) -0.011(2) -0.020(3) 0.010(2)
C4 0.083(3) 0.046(2) 0.059(2) 0.008(2) -0.006(2) -0.0061(19)
C5 0.053(2) 0.0437(19) 0.050(2) 0.0015(16) -0.0070(17) -0.0011(16)
C6 0.0348(16) 0.0397(16) 0.0338(15) -0.0036(13) -0.0045(12) 0.0050(13)
C7 0.0310(16) 0.0406(16) 0.0413(16) 0.0016(13) 0.0001(13) 0.0060(14)
C8 0.0355(18) 0.053(2) 0.060(2) 0.0052(15) 0.0062(15) 0.0079(19)
C9 0.0322(16) 0.0389(16) 0.0372(15) 0.0004(13) 0.0009(12) -0.0007(13)
C10 0.0342(17) 0.0419(17) 0.059(2) -0.0021(14) 0.0086(15) 0.0023(16)
C11 0.0370(18) 0.0369(16) 0.0507(19) 0.0002(13) 0.0036(14) 0.0003(14)
C12 0.0362(16) 0.0354(15) 0.0418(16) 0.0050(12) -0.0009(14) 0.0015(14)
C13 0.0324(16) 0.0380(16) 0.0425(17) 0.0008(12) 0.0019(13) -0.0037(13)
C14 0.0404(18) 0.0317(15) 0.054(2) -0.0017(13) 0.0034(15) -0.0004(15)
C15 0.043(2) 0.0325(16) 0.071(2) 0.0056(14) 0.0048(17) 0.0010(16)
C16 0.0350(18) 0.0430(18) 0.072(3) 0.0066(15) 0.0111(17) -0.0013(17)
C17 0.070(3) 0.0339(18) 0.079(3) 0.0034(17) 0.013(2) 0.009(2)
C18 0.0393(18) 0.053(2) 0.054(2) 0.0074(15) 0.0061(15) -0.0021(17)
C19 0.079(3) 0.089(3) 0.063(3) 0.033(3) 0.008(2) 0.021(2)
C20 0.107(4) 0.097(4) 0.078(3) 0.053(3) 0.010(3) 0.018(3)
N1 0.0344(18) 0.071(2) 0.079(2) -0.0050(16) 0.0147(16) 0.0224(19)
N2 0.0314(14) 0.0394(14) 0.0596(17) 0.0005(12) 0.0067(13) 0.0095(14)
N3 0.0343(14) 0.0379(14) 0.0521(16) -0.0026(12) 0.0046(12) 0.0034(12)
O1 0.0297(12) 0.0447(12) 0.0642(15) -0.0001(10) 0.0019(11) 0.0073(12)
O2 0.0526(15) 0.0357(12) 0.0796(19) 0.0012(10) 0.0126(13) 0.0106(13)
O3 0.0312(11) 0.0469(13) 0.0488(13) 0.0007(10) 0.0042(9) -0.0045(11)
O4 0.0489(16) 0.093(2) 0.076(2) -0.0002(15) -0.0067(15) -0.0299(18)
O5 0.126(3) 0.092(2) 0.064(2) 0.052(2) 0.020(2) 0.0295(19)
S1 0.0443(4) 0.0555(5) 0.0420(4) 0.0126(4) 0.0015(4) 0.0018(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 C1 C2 . . 130.3(4) ?
N1 C1 C6 . . 107.9(3) ?
C2 C1 C6 . . 121.8(4) ?
C3 C2 C1 . . 117.8(4) ?
C3 C2 H2 . . 121.1 ?
C1 C2 H2 . . 121.1 ?
C2 C3 C4 . . 121.0(4) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C5 C4 C3 . . 121.9(4) ?
C5 C4 H4 . . 119.0 ?
C3 C4 H4 . . 119.0 ?
C4 C5 C6 . . 118.6(4) ?
C4 C5 H5 . . 120.7 ?
C6 C5 H5 . . 120.7 ?
C5 C6 C1 . . 118.8(3) ?
C5 C6 C7 . . 135.0(3) ?
C1 C6 C7 . . 106.1(3) ?
C8 C7 C6 . . 106.3(3) ?
C8 C7 C9 . . 126.9(3) ?
C6 C7 C9 . . 126.7(3) ?
N1 C8 C7 . . 109.9(3) ?
N1 C8 H8 . . 125.0 ?
C7 C8 H8 . . 125.0 ?
O1 C9 N2 . . 122.3(3) ?
O1 C9 C7 . . 122.4(3) ?
N2 C9 C7 . . 115.3(3) ?
N3 C10 C11 . . 120.3(3) ?
N3 C10 H10 . . 119.8 ?
C11 C10 H10 . . 119.8 ?
C16 C11 C12 . . 118.1(3) ?
C16 C11 C10 . . 120.3(3) ?
C12 C11 C10 . . 121.6(3) ?
C13 C12 C11 . . 120.2(3) ?
C13 C12 H12 . . 119.9 ?
C11 C12 H12 . . 119.9 ?
C12 C13 C14 . . 122.1(3) ?
C12 C13 O3 . . 119.4(3) ?
C14 C13 O3 . . 118.6(3) ?
O2 C14 C15 . . 125.1(3) ?
O2 C14 C13 . . 116.9(3) ?
C15 C14 C13 . . 117.9(3) ?
C14 C15 C16 . . 120.2(3) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C11 C16 C15 . . 121.6(3) ?
C11 C16 H16 . . 119.2 ?
C15 C16 H16 . . 119.2 ?
O2 C17 H17A . . 109.5 ?
O2 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
O2 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C19 C18 S1 . . 113.9(3) ?
C19 C18 H18A . . 108.8 ?
S1 C18 H18A . . 108.8 ?
C19 C18 H18B . . 108.8 ?
S1 C18 H18B . . 108.8 ?
H18A C18 H18B . . 107.7 ?
C20 C19 C18 . . 113.5(4) ?
C20 C19 H19A . . 108.9 ?
C18 C19 H19A . . 108.9 ?
C20 C19 H19B . . 108.9 ?
C18 C19 H19B . . 108.9 ?
H19A C19 H19B . . 107.7 ?
C19 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C19 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C8 N1 C1 . . 109.7(3) ?
C8 N1 H1 . . 117(4) ?
C1 N1 H1 . . 131(4) ?
C9 N2 N3 . . 119.5(3) ?
C9 N2 H2A . . 124(3) ?
N3 N2 H2A . . 115(3) ?
C10 N3 N2 . . 116.1(3) ?
C14 O2 C17 . . 117.6(3) ?
C13 O3 S1 . . 117.6(2) ?
O5 S1 O4 . . 117.3(3) ?
O5 S1 O3 . . 108.98(19) ?
O4 S1 O3 . . 108.43(17) ?
O5 S1 C18 . . 111.2(2) ?
O4 S1 C18 . . 109.37(19) ?
O3 S1 C18 . . 100.09(16) ?
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 N1 . 1.365(5) ?
C1 C2 . 1.398(6) ?
C1 C6 . 1.405(5) ?
C2 C3 . 1.360(7) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.381(7) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.378(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.387(5) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.447(5) ?
C7 C8 . 1.367(5) ?
C7 C9 . 1.451(4) ?
C8 N1 . 1.354(5) ?
C8 H8 . 0.9300 ?
C9 O1 . 1.235(4) ?
C9 N2 . 1.355(4) ?
C10 N3 . 1.273(4) ?
C10 C11 . 1.458(5) ?
C10 H10 . 0.9300 ?
C11 C16 . 1.385(5) ?
C11 C12 . 1.397(5) ?
C12 C13 . 1.361(5) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.398(4) ?
C13 O3 . 1.412(4) ?
C14 O2 . 1.354(4) ?
C14 C15 . 1.382(5) ?
C15 C16 . 1.386(5) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
C17 O2 . 1.422(4) ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
C18 C19 . 1.503(6) ?
C18 S1 . 1.742(3) ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
C19 C20 . 1.488(6) ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9600 ?
N1 H1 . 0.858(14) ?
N2 N3 . 1.376(4) ?
N2 H2A . 0.856(13) ?
O3 S1 . 1.599(3) ?
O4 S1 . 1.426(3) ?
O5 S1 . 1.411(3) ?
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
C10 H10 O1 3_465 0.93 2.51 3.325(4) 146.4 yes
C18 H18A O1 2_664 0.97 2.52 3.467(5) 164.3 yes
N2 H2A O1 3_465 0.856(13) 2.221(18) 3.048(4) 163(4) yes
N1 H1 O4 2_565 0.858(14) 2.07(3) 2.870(5) 156(5) 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
C20 C19 C18 S1 . . . . 168.2(4) ?