#------------------------------------------------------------------------------
#$Date: 2025-03-14 05:12:06 +0200 (Fri, 14 Mar 2025) $
#$Revision: 298435 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312783.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_2312783
loop_
_publ_author_name
'Wang, Yan Juan'
'Zhang, Yao'
'Tang, Yuan Yuan'
'Chen, Xiao Gang'
_publ_section_title
;
Halogen-substituted benzylamine crown ether inclusion complexes.
;
_journal_coeditor_code JX3091
_journal_issue 4
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229625001986
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C7 H9 F N +, C2 H6 N O4 S2 -, C12 H24 O6'
_chemical_formula_moiety 'C7 H9 F N +, C2 H6 N O4 S2 -, C12 H24 O6'
_chemical_formula_sum 'C21 H39 F N2 O10 S2'
_chemical_formula_weight 562.66
_chemical_name_common
;
4-Fluorobenzylaminium di(methanesulfonyl)amidate--18-crown-6 (1/1)
;
_chemical_name_systematic
'4-Fluorobenzylaminium [(methanesulfonylazanidyl)sulfonyl]methane--1,4,7,10,13,16-hexaoxacyclooctadecane (1/1)'
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 105.4799(12)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.80545(9)
_cell_length_b 16.82204(19)
_cell_length_c 10.55058(13)
_cell_measurement_reflns_used 39584
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 74.7640
_cell_measurement_theta_min 2.5940
_cell_volume 1335.08(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(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 0.970
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy-DW diffractometer with a HyPix-Arc 150 detector'
_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 0.0249
_diffrn_reflns_av_unetI/netI 0.0105
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 46639
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.154
_diffrn_reflns_theta_min 4.348
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 2.358
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.89020
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2024)
;
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.400
_exptl_crystal_description block
_exptl_crystal_F_000 600
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.226
_refine_diff_density_min -0.229
_refine_ls_abs_structure_details
;
Flack x determined using 2392 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.018(6)
_refine_ls_extinction_coef 0.0039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 340
_refine_ls_number_reflns 5207
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.029
_refine_ls_R_factor_all 0.0207
_refine_ls_R_factor_gt 0.0206
_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^)+(0.0355P)^2^+0.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0557
_refine_ls_wR_factor_ref 0.0557
_reflns_number_gt 5177
_reflns_number_total 5207
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3091sup1.cif
_cod_data_source_block zy_241017_2_100k_auto
_cod_original_cell_volume 1335.07(3)
_cod_database_code 2312783
_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_hkl_file
;
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0 -19 -2 4153.95 193.663 130
0 -19 -3 1883.89 133.674 95
0 -19 -4 2150.74 130.522 93
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0 -18 0 19923.4 530.428 107
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0 -17 2 894.759 120.347 106
0 -17 -2 1093.29 126.240 107
0 -17 -2 1038.38 128.510 129
0 -17 -2 1074.49 132.229 130
0 -17 -2 1126.50 138.610 120
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0 -17 -3 5425.11 268.595 129
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8 5 -5 21033.7 626.807 66
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8 5 -4 11465.8 450.006 66
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8 5 -3 3443.45 262.001 123
8 5 -3 3063.60 250.351 84
8 5 -3 3060.93 233.392 66
8 5 -2 6039.84 338.672 84
8 5 -2 5815.16 310.652 124
8 5 -2 6190.09 338.617 123
8 5 -2 6329.05 356.507 126
8 5 -2 6222.41 357.754 102
8 5 -2 6569.38 320.512 58
8 5 -2 6398.31 363.053 113
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8 5 -1 12561.3 506.022 126
8 5 -1 12335.4 458.885 123
8 5 -1 12173.3 460.404 84
8 5 -1 12797.0 450.839 58
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8 5 -1 12506.1 499.604 102
8 5 -1 13087.3 524.967 101
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8 5 0 5084.06 301.878 102
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8 5 1 9580.34 375.896 102
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8 5 2 10083.6 408.786 82
8 5 2 9452.40 356.803 101
8 5 2 9768.48 386.799 112
-8 5 -2 8650.12 456.244 74
-8 5 -3 23181.9 695.605 74
8 5 3 24330.3 598.658 81
8 6 -9 11443.0 312.173 59
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8 6 -7 1581.71 150.839 84
8 6 -7 1571.67 144.284 85
8 6 -7 1353.41 143.697 124
8 6 -7 1669.66 153.811 123
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8 6 -7 1543.61 148.840 66
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8 6 -6 4697.28 247.364 85
8 6 -6 4735.31 276.101 84
8 6 -6 4495.86 268.534 124
8 6 -6 4193.10 257.885 123
8 6 -6 4203.98 252.447 102
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8 6 -6 4319.22 255.561 66
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8 6 -5 1985.22 197.805 84
8 6 -5 1933.94 189.815 124
8 6 -5 2142.08 199.791 123
8 6 -5 2181.83 200.461 102
-8 6 5 2149.91 193.634 8
8 6 -5 2048.56 187.694 66
-8 6 5 2002.55 164.479 70
8 6 -4 4997.31 308.833 84
8 6 -4 4853.46 292.856 124
8 6 -4 5015.76 304.793 123
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8 6 -4 4700.14 300.318 102
-8 6 4 4951.94 248.147 70
8 6 -3 4364.05 271.638 66
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8 6 -3 4582.52 292.184 123
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8 6 -2 2414.87 227.621 113
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8 6 -2 2161.16 205.305 126
8 6 -2 2456.11 228.305 102
8 6 -2 2425.88 213.517 123
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8 6 -2 2473.10 196.556 58
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8 6 -1 6339.16 343.963 102
8 6 -1 5570.17 298.761 123
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-8 6 0 826.932 189.113 74
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8 7 -8 328.971 73.0084 139
-8 7 8 376.451 65.9035 70
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8 7 -7 12538.0 397.016 123
8 7 -7 12800.3 403.521 66
8 7 -6 13549.7 453.270 84
-8 7 6 13653.1 410.140 70
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8 7 -6 12263.2 436.070 124
8 7 -6 12967.0 444.017 123
8 7 -6 12623.5 428.000 66
8 7 -5 4576.20 276.294 84
-8 7 5 4846.21 240.804 70
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8 7 -5 4470.45 264.503 102
8 7 -5 4535.06 270.381 124
8 7 -5 4603.21 275.686 123
8 7 -5 5026.49 274.816 66
8 7 -4 6240.28 331.842 84
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8 7 -4 6357.49 335.821 102
8 7 -4 6604.40 332.426 124
8 7 -4 6344.28 332.754 123
8 7 -4 6483.91 317.706 66
8 7 -3 9324.48 407.042 84
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8 7 -3 9424.85 416.804 101
8 7 -3 9435.17 407.901 123
8 7 -3 9009.07 382.989 66
8 7 -2 1050.66 155.095 101
8 7 -2 939.989 147.785 102
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8 7 -2 1332.98 161.484 123
8 7 -2 1155.73 151.744 84
-8 7 2 1238.21 216.743 74
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8 7 -1 23362.5 684.602 101
8 7 -1 23109.1 671.159 102
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8 7 0 13604.3 473.541 102
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8 7 0 13336.4 466.077 112
-8 7 0 14470.5 472.119 8
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8 7 1 19195.6 564.232 82
-8 7 -1 18737.3 682.515 74
8 7 1 19477.8 556.054 101
8 7 1 17471.9 506.582 102
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8 7 2 339.631 75.2665 101
-8 7 -2 460.496 124.731 74
-8 7 -3 59.8168 60.2587 74
-8 8 8 672.489 74.3069 70
8 8 -8 677.968 75.1209 59
-8 8 7 3656.56 181.747 70
-8 8 7 3372.87 189.145 75
8 8 -7 3306.83 183.392 139
8 8 -7 3584.62 192.619 66
8 8 -6 202.696 76.6117 123
8 8 -6 267.332 80.3926 84
8 8 -6 300.079 76.0366 139
8 8 -6 200.672 77.3720 66
-8 8 6 307.619 74.0157 70
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8 8 -5 6356.83 305.987 123
8 8 -5 6339.98 306.740 84
8 8 -5 6491.92 299.869 102
8 8 -5 5595.70 251.774 139
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8 8 -4 3546.56 225.991 66
8 8 -4 3407.99 234.808 123
8 8 -4 3339.57 236.435 84
-8 8 4 3397.57 212.369 75
-8 8 4 3116.48 231.397 9
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8 8 -4 3399.52 234.836 102
-8 8 3 1899.02 177.190 8
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8 8 -3 1690.23 175.027 123
8 8 -3 1782.81 179.270 101
8 8 -3 1758.03 183.002 102
8 8 -3 1793.31 170.907 66
-8 8 2 21932.3 632.412 9
-8 8 2 22586.0 625.626 8
8 8 -2 20314.2 594.753 123
8 8 -2 20332.1 577.680 66
8 8 -2 21412.1 628.031 101
8 8 -2 20541.1 623.236 102
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-8 8 1 3850.87 238.543 8
-8 8 1 3424.87 226.794 9
8 8 -1 3806.99 252.797 101
8 8 -1 3780.68 248.591 102
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8 8 0 12235.0 438.927 101
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8 8 1 1602.53 150.378 101
-8 8 -2 4444.79 266.049 74
-8 9 7 6681.77 243.783 75
-8 9 7 6920.44 232.920 70
-8 9 6 2878.26 161.862 70
-8 9 6 2977.45 177.384 75
8 9 -6 2652.49 170.282 123
8 9 -6 2824.50 172.781 66
8 9 -6 2440.87 149.010 139
8 9 -6 2869.70 187.350 138
8 9 -5 3017.04 190.606 66
-8 9 5 2811.11 181.984 75
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8 9 -5 2840.53 193.497 123
8 9 -4 2047.32 173.654 102
8 9 -4 2172.46 171.971 66
-8 9 4 2010.00 155.520 75
8 9 -4 1956.24 173.237 123
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8 9 -3 7471.87 315.847 66
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8 9 -2 12995.1 450.406 102
8 9 -2 12475.5 415.641 66
8 9 -1 2658.05 175.510 138
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8 9 -1 3146.73 214.919 102
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8 10 -6 3855.49 178.483 66
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8 10 -5 3266.09 200.194 138
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8 10 -2 14079.5 431.635 101
8 10 -2 14746.6 451.362 102
8 10 -2 14917.4 427.769 66
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8 10 -1 299.760 81.1769 101
8 10 -1 289.008 80.9690 102
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8 11 -5 1928.69 137.417 138
8 11 -5 1877.14 119.779 66
8 11 -4 399.083 79.6452 138
8 11 -4 328.504 67.3831 66
8 11 -3 1524.09 127.979 138
8 11 -3 1549.96 121.522 66
8 11 -2 2566.70 152.935 66
8 11 -1 17917.7 423.791 66
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-9 -5 4 7782.95 275.964 11
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-9 -3 5 21844.4 514.719 11
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-9 -1 3 17009.4 468.540 11
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9 0 -7 1446.70 126.443 123
9 0 -6 5635.82 265.198 84
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9 0 -6 5365.60 251.310 123
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9 0 -5 3512.07 208.549 123
-9 0 5 3589.44 205.179 8
9 0 -4 372.429 88.5187 84
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9 0 -3 8870.03 353.546 102
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9 1 -6 8855.15 334.626 84
9 1 -5 22130.8 573.359 123
-9 1 5 23304.6 582.359 8
9 1 -5 23149.1 600.652 84
-9 1 4 20101.8 503.709 11
-9 1 4 18638.9 515.456 8
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9 1 -4 17936.6 505.745 123
9 1 -4 18755.4 532.862 84
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9 1 -3 16118.6 494.575 102
9 1 -3 14697.3 432.126 123
9 1 -3 15621.8 462.789 84
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9 1 -1 32.1773 56.9801 101
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9 2 -7 4207.96 203.546 123
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9 2 -6 4518.58 233.393 102
9 2 -6 4589.89 234.554 84
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9 2 -5 183.291 72.2312 123
9 2 -5 132.597 71.6756 102
9 2 -5 144.270 75.3265 84
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-9 2 4 5723.61 267.019 8
9 2 -4 6026.73 283.509 84
9 2 -4 5492.19 261.430 123
9 2 -4 5636.10 285.175 102
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-9 2 3 545.100 93.9777 8
9 2 -3 286.280 88.4179 84
9 2 -3 368.480 81.4614 123
9 2 -3 486.984 102.003 102
9 2 -2 305.874 72.6023 84
9 2 -2 332.504 85.5306 102
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9 2 -1 871.245 116.615 101
9 2 -1 671.293 94.6901 102
-9 2 1 680.300 115.690 74
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9 2 0 1424.97 122.538 101
9 2 1 2821.55 175.368 82
9 3 -7 4200.07 197.477 84
9 3 -7 4332.32 200.391 123
9 3 -6 7037.18 283.309 102
9 3 -6 7080.32 283.646 123
9 3 -6 6795.49 282.757 84
-9 3 6 7085.84 279.936 8
-9 3 5 19454.9 514.356 8
9 3 -5 19066.8 525.624 102
9 3 -5 18684.9 508.470 123
9 3 -5 19116.2 523.122 84
-9 3 4 23972.5 593.795 8
9 3 -4 23269.8 611.888 102
9 3 -4 23590.8 586.511 123
9 3 -4 23936.6 600.845 84
9 3 -3 19865.9 559.455 102
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-9 3 3 20749.1 539.532 8
9 3 -3 20069.8 533.834 84
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9 3 -2 10071.5 381.279 101
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9 3 -1 14310.9 416.195 102
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9 4 -6 6660.68 270.396 84
9 4 -6 6889.93 270.071 123
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9 4 -5 6807.33 290.453 102
9 4 -5 6949.92 289.969 84
9 4 -5 6795.87 282.309 123
9 4 -5 5909.67 234.889 66
-9 4 4 1614.36 143.196 8
9 4 -4 1751.50 159.023 102
9 4 -4 1777.13 155.263 84
9 4 -4 1758.50 150.164 123
9 4 -4 1530.11 121.829 66
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9 4 -3 1843.30 163.851 102
9 4 -3 1660.63 159.636 101
9 4 -3 1677.16 142.579 123
9 4 -3 1612.54 144.574 84
9 4 -3 1366.75 114.902 66
9 4 -2 85.2637 67.4200 101
9 4 -2 105.721 67.3794 102
9 4 -2 125.538 56.8612 123
9 4 -2 151.587 51.4559 66
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9 4 -1 1668.80 146.539 101
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9 4 0 1406.81 132.695 82
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9 5 -6 4390.73 204.630 84
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9 5 -5 19508.4 507.243 102
9 5 -5 20603.6 505.656 101
9 5 -5 20593.3 515.780 84
9 5 -5 19491.5 500.615 123
9 5 -5 18598.6 456.004 66
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9 5 -4 8522.68 324.680 102
9 5 -4 8600.17 324.736 101
9 5 -4 8058.44 311.310 84
9 5 -4 7856.65 300.099 123
9 5 -4 7808.24 272.396 66
-9 5 3 32408.5 700.336 8
9 5 -3 33120.8 731.977 101
9 5 -3 31972.9 716.847 102
9 5 -3 31590.2 675.556 123
9 5 -3 32174.9 689.704 84
-9 5 2 15009.6 418.630 8
9 5 -2 15280.4 452.826 101
9 5 -2 15149.5 436.622 102
9 5 -1 9488.10 263.561 66
9 5 -1 11800.3 369.064 101
-9 5 0 1177.71 136.958 74
9 6 -5 873.575 91.6930 66
9 6 -5 1027.12 108.317 84
9 6 -5 1090.92 110.789 123
9 6 -4 1410.16 126.637 123
9 6 -4 1688.27 137.291 101
9 6 -4 1460.85 133.413 102
9 6 -4 1507.20 116.691 66
-9 6 4 1541.71 129.842 8
9 6 -3 963.485 97.1195 66
9 6 -3 1064.08 118.122 101
9 6 -3 1128.59 121.033 102
-9 6 3 1187.56 116.136 8
9 6 -2 1238.68 102.059 66
9 6 -2 1450.91 134.530 101
9 6 -1 303.700 72.0719 101
9 7 -5 24523.7 500.476 66
9 7 -4 9651.64 284.300 66
9 7 -3 4913.16 193.795 66
9 7 -3 5205.72 220.355 101
9 7 -2 11652.8 303.527 66
9 7 -2 12283.2 356.481 101
9 8 -4 9745.64 262.528 66
9 8 -3 4026.87 160.746 66
0 0 0 0.00 0.00 0
TITL ZY_241017_2_100K_auto in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 7.802799 16.822550 10.548150 90.0000 105.4580 90.0000
ZERR 19.00 0.000051 0.000090 0.000061 0.0000 0.0006 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O S
UNIT 19.00 19.00 19.00 19.00 19.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 44290
_shelx_res_file
;
TITL zy_241017_2_100k_auto_a.res in P2(1)
zy_241017_2_100k_auto.res
created by SHELXL-2018/3 at 12:03:31 on 03-Feb-2025
REM Old TITL ZY_241017_2_100K_auto in P2(1)
REM SHELXT solution in P2(1): R1 0.079, Rweak 0.037, Alpha 0.004
REM 4.282 for 8 systematic absences, Orientation as input
REM Flack x = 0.036 ( 0.009 ) from 1321 Parsons' quotients
REM Formula found by SHELXT: C22 N2 O10 S2
CELL 1.54184 7.805446 16.822035 10.550584 90 105.4799 90
ZERR 2 0.000086 0.000191 0.00013 0 0.0012 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H F N O S
UNIT 42 78 2 4 20 4
L.S. 5
PLAN 10
TEMP -173
CONF
HTAB N1 O1
HTAB N1 O3
HTAB N1 O5
BOND $H
MORE -1
fmap 2
acta
REM
REM
REM
WGHT 0.035500 0.268400
EXTI 0.003927
FVAR 7.96231
C1 1 0.092374 0.225322 0.467436 11.00000 0.02274 0.01868 =
0.03734 -0.00341 0.00966 -0.00704
AFIX 23
H1A 2 -0.010401 0.197792 0.485985 11.00000 -1.20000
H1B 2 0.176539 0.184581 0.452681 11.00000 -1.20000
AFIX 0
C2 1 0.030601 0.276351 0.347229 11.00000 0.02019 0.02474 =
0.03268 -0.00578 0.00200 -0.00421
AFIX 23
H2A 2 -0.045564 0.245068 0.274155 11.00000 -1.20000
H2B 2 -0.039387 0.321860 0.365810 11.00000 -1.20000
AFIX 0
C3 1 0.142441 0.347880 0.191808 11.00000 0.03557 0.02213 =
0.01991 -0.00004 -0.00409 0.00091
AFIX 23
H3A 2 0.078083 0.397242 0.201574 11.00000 -1.20000
H3B 2 0.065187 0.315638 0.120623 11.00000 -1.20000
AFIX 0
C4 1 0.312089 0.367799 0.158419 11.00000 0.04388 0.02169 =
0.01494 -0.00006 0.00452 0.00059
AFIX 23
H4A 2 0.378871 0.318480 0.152790 11.00000 -1.20000
H4B 2 0.285660 0.394854 0.072027 11.00000 -1.20000
AFIX 0
C5 1 0.584082 0.437954 0.234670 11.00000 0.03291 0.02938 =
0.02134 0.00478 0.01311 0.00308
AFIX 23
H5A 2 0.564899 0.464256 0.148063 11.00000 -1.20000
H5B 2 0.653692 0.388832 0.234010 11.00000 -1.20000
AFIX 0
C6 1 0.683706 0.492622 0.341830 11.00000 0.03124 0.02493 =
0.02736 0.00778 0.01336 -0.00078
AFIX 23
H6A 2 0.791094 0.513488 0.320187 11.00000 -1.20000
H6B 2 0.607539 0.538146 0.351023 11.00000 -1.20000
AFIX 0
C7 1 0.820947 0.496396 0.570446 11.00000 0.01941 0.01928 =
0.02916 -0.00276 0.00943 -0.00263
AFIX 23
H7A 2 0.740509 0.539034 0.584466 11.00000 -1.20000
H7B 2 0.927543 0.521433 0.553610 11.00000 -1.20000
AFIX 0
C8 1 0.874187 0.444051 0.690182 11.00000 0.01558 0.02623 =
0.02500 -0.00513 0.00335 -0.00140
AFIX 23
H8A 2 0.927482 0.394165 0.668543 11.00000 -1.20000
H8B 2 0.963585 0.471522 0.760973 11.00000 -1.20000
AFIX 0
C9 1 0.761502 0.376643 0.847636 11.00000 0.02530 0.02180 =
0.01847 0.00106 -0.00019 0.00378
AFIX 23
H9A 2 0.844514 0.404613 0.921587 11.00000 -1.20000
H9B 2 0.819781 0.327331 0.829203 11.00000 -1.20000
AFIX 0
C10 1 0.592548 0.356589 0.883579 11.00000 0.03182 0.02489 =
0.01525 0.00101 0.00594 0.00443
AFIX 23
H10A 2 0.620282 0.328196 0.968833 11.00000 -1.20000
H10B 2 0.526988 0.405842 0.891914 11.00000 -1.20000
AFIX 0
C11 1 0.321508 0.285962 0.805706 11.00000 0.02554 0.02963 =
0.02590 0.01002 0.01336 0.00478
AFIX 23
H11A 2 0.248485 0.334021 0.806204 11.00000 -1.20000
H11B 2 0.341848 0.259286 0.892096 11.00000 -1.20000
AFIX 0
C12 1 0.227445 0.230691 0.697644 11.00000 0.02634 0.02466 =
0.03297 0.01066 0.00992 -0.00182
AFIX 23
H12A 2 0.306808 0.186097 0.689914 11.00000 -1.20000
H12B 2 0.120160 0.208465 0.717667 11.00000 -1.20000
AFIX 0
O1 5 0.177959 0.274514 0.576632 11.00000 0.02426 0.01839 =
0.02489 0.00317 0.00671 -0.00242
O2 5 0.184673 0.304205 0.312176 11.00000 0.02293 0.02411 =
0.02017 0.00135 0.00019 -0.00301
O3 5 0.416706 0.418760 0.258252 11.00000 0.03011 0.02212 =
0.01688 -0.00058 0.00649 0.00014
O4 5 0.733017 0.448565 0.461328 11.00000 0.02682 0.01977 =
0.02043 0.00126 0.00697 -0.00121
O5 5 0.718780 0.426481 0.733438 11.00000 0.01786 0.02114 =
0.01888 0.00169 0.00373 0.00197
O6 5 0.487126 0.307426 0.782340 11.00000 0.02295 0.02508 =
0.01933 0.00024 0.00890 -0.00036
C13 1 0.252714 0.454426 0.540884 11.00000 0.01728 0.01654 =
0.02597 0.00203 0.00778 0.00174
AFIX 23
H13A 2 0.236442 0.449615 0.630469 11.00000 -1.20000
H13B 2 0.140140 0.438240 0.477465 11.00000 -1.20000
AFIX 0
C14 1 0.291022 0.540053 0.515973 11.00000 0.01394 0.01597 =
0.02021 0.00091 0.00664 0.00225
C15 1 0.234121 0.572854 0.390183 11.00000 0.02118 0.01851 =
0.01827 -0.00304 0.00261 0.00166
AFIX 43
H15 2 0.174579 0.540349 0.318265 11.00000 -1.20000
AFIX 0
C16 1 0.263859 0.652802 0.369176 11.00000 0.02684 0.02108 =
0.01904 0.00432 0.00840 0.00442
AFIX 43
H16 2 0.225820 0.675520 0.283818 11.00000 -1.20000
AFIX 0
C17 1 0.349930 0.697730 0.475818 11.00000 0.01944 0.01341 =
0.03133 0.00178 0.00996 -0.00088
C18 1 0.410144 0.667805 0.600895 11.00000 0.02359 0.02217 =
0.02438 -0.00551 0.00094 -0.00217
AFIX 43
H18 2 0.471632 0.700546 0.671864 11.00000 -1.20000
AFIX 0
C19 1 0.378154 0.587916 0.620330 11.00000 0.02196 0.02191 =
0.01711 0.00125 0.00340 0.00324
AFIX 43
H19 2 0.416500 0.565899 0.706183 11.00000 -1.20000
AFIX 0
F1 3 0.370754 0.776709 0.457658 11.00000 0.03674 0.01536 =
0.04667 0.00409 0.01283 -0.00454
N1 4 0.397057 0.399619 0.528478 11.00000 0.01696 0.01374 =
0.01743 0.00144 0.00348 0.00047
C20 1 0.773136 0.620512 -0.126626 11.00000 0.02192 0.03491 =
0.02014 -0.00254 0.00016 0.00720
AFIX 137
H20A 2 0.680694 0.658341 -0.119465 11.00000 -1.50000
H20B 2 0.718713 0.568831 -0.155602 11.00000 -1.50000
H20C 2 0.833561 0.640230 -0.190743 11.00000 -1.50000
AFIX 0
C21 1 1.382874 0.624883 0.060621 11.00000 0.02463 0.04787 =
0.08018 -0.03535 0.02470 -0.01388
AFIX 137
H21A 2 1.416737 0.593259 0.141486 11.00000 -1.50000
H21B 2 1.333859 0.675937 0.078879 11.00000 -1.50000
H21C 2 1.487832 0.634272 0.028394 11.00000 -1.50000
AFIX 0
N2 4 1.072264 0.547011 0.009275 11.00000 0.01897 0.01890 =
0.01963 0.00294 0.00451 0.00050
O7 5 0.835105 0.574077 0.114219 11.00000 0.02696 0.04010 =
0.02659 0.00461 0.01365 -0.00231
O8 5 1.000883 0.688388 0.065043 11.00000 0.02481 0.02377 =
0.02627 -0.00598 0.00718 -0.00016
O9 5 1.306384 0.501246 -0.087612 11.00000 0.02624 0.02469 =
0.02658 -0.00067 0.00753 0.00822
O10 5 1.156878 0.625390 -0.170036 11.00000 0.05942 0.04373 =
0.04854 0.02949 0.03960 0.03079
S1 6 0.928491 0.609968 0.027816 11.00000 0.01657 0.02229 =
0.01400 -0.00003 0.00407 0.00056
S2 6 1.221349 0.573052 -0.059699 11.00000 0.02237 0.01846 =
0.02541 0.00234 0.01158 0.00383
H1C 2 0.360133 0.350362 0.541060 11.00000 0.02414
H1D 2 0.409642 0.404705 0.444539 11.00000 0.02837
H1E 2 0.496989 0.408677 0.591248 11.00000 0.03114
HKLF 4
REM zy_241017_2_100k_auto_a.res in P2(1)
REM wR2 = 0.0557, GooF = S = 1.029, Restrained GooF = 1.029 for all data
REM R1 = 0.0206 for 5177 Fo > 4sig(Fo) and 0.0207 for all 5207 data
REM 340 parameters refined using 1 restraints
END
WGHT 0.0355 0.2684
REM Highest difference peak 0.226, deepest hole -0.229, 1-sigma level 0.033
Q1 1 1.2997 0.6105 -0.0210 11.00000 0.05 0.23
Q2 1 0.8513 0.6103 -0.0501 11.00000 0.05 0.20
Q3 1 0.8519 0.4626 0.6241 11.00000 0.05 0.18
Q4 1 1.1745 0.5820 -0.1404 11.00000 0.05 0.18
Q5 1 0.2873 0.5483 0.4466 11.00000 0.05 0.17
Q6 1 1.3558 0.6586 -0.0056 11.00000 0.05 0.16
Q7 1 0.2913 0.5676 0.5600 11.00000 0.05 0.15
Q8 1 0.3596 0.6804 0.5355 11.00000 0.05 0.15
Q9 1 0.2113 0.2512 0.6323 11.00000 0.05 0.15
Q10 1 1.0054 0.5757 0.0165 11.00000 0.05 0.14
;
_shelx_res_checksum 48964
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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 0.0924(3) 0.22532(12) 0.4674(2) 0.0259(4) Uani d 1 . .
H H1A -0.010401 0.197792 0.485985 0.031 Uiso calc 1 . .
H H1B 0.176539 0.184581 0.452681 0.031 Uiso calc 1 . .
C C2 0.0306(3) 0.27635(13) 0.3472(2) 0.0268(4) Uani d 1 . .
H H2A -0.045564 0.245068 0.274155 0.032 Uiso calc 1 . .
H H2B -0.039387 0.321860 0.365810 0.032 Uiso calc 1 . .
C C3 0.1424(3) 0.34788(12) 0.1918(2) 0.0281(4) Uani d 1 . .
H H3A 0.078083 0.397242 0.201574 0.034 Uiso calc 1 . .
H H3B 0.065187 0.315638 0.120623 0.034 Uiso calc 1 . .
C C4 0.3121(3) 0.36780(12) 0.15842(19) 0.0275(4) Uani d 1 . .
H H4A 0.378871 0.318480 0.152790 0.033 Uiso calc 1 . .
H H4B 0.285660 0.394854 0.072027 0.033 Uiso calc 1 . .
C C5 0.5841(3) 0.43795(13) 0.23467(19) 0.0268(4) Uani d 1 . .
H H5A 0.564899 0.464256 0.148063 0.032 Uiso calc 1 . .
H H5B 0.653692 0.388832 0.234010 0.032 Uiso calc 1 . .
C C6 0.6837(3) 0.49262(13) 0.3418(2) 0.0268(4) Uani d 1 . .
H H6A 0.791094 0.513488 0.320187 0.032 Uiso calc 1 . .
H H6B 0.607539 0.538146 0.351023 0.032 Uiso calc 1 . .
C C7 0.8209(3) 0.49640(11) 0.57045(19) 0.0221(4) Uani d 1 . .
H H7A 0.740509 0.539034 0.584466 0.026 Uiso calc 1 . .
H H7B 0.927543 0.521433 0.553610 0.026 Uiso calc 1 . .
C C8 0.8742(3) 0.44405(12) 0.69018(19) 0.0227(4) Uani d 1 . .
H H8A 0.927482 0.394165 0.668543 0.027 Uiso calc 1 . .
H H8B 0.963585 0.471522 0.760973 0.027 Uiso calc 1 . .
C C9 0.7615(3) 0.37664(12) 0.84764(19) 0.0230(4) Uani d 1 . .
H H9A 0.844514 0.404613 0.921587 0.028 Uiso calc 1 . .
H H9B 0.819781 0.327331 0.829203 0.028 Uiso calc 1 . .
C C10 0.5925(3) 0.35659(13) 0.88358(18) 0.0241(4) Uani d 1 . .
H H10A 0.620282 0.328196 0.968833 0.029 Uiso calc 1 . .
H H10B 0.526988 0.405842 0.891914 0.029 Uiso calc 1 . .
C C11 0.3215(3) 0.28596(13) 0.8057(2) 0.0258(4) Uani d 1 . .
H H11A 0.248485 0.334021 0.806204 0.031 Uiso calc 1 . .
H H11B 0.341848 0.259286 0.892096 0.031 Uiso calc 1 . .
C C12 0.2274(3) 0.23069(12) 0.6976(2) 0.0276(4) Uani d 1 . .
H H12A 0.306808 0.186097 0.689914 0.033 Uiso calc 1 . .
H H12B 0.120160 0.208465 0.717667 0.033 Uiso calc 1 . .
O O1 0.17796(18) 0.27451(8) 0.57663(13) 0.0225(3) Uani d 1 . .
O O2 0.18467(18) 0.30420(8) 0.31218(13) 0.0235(3) Uani d 1 . .
O O3 0.41671(19) 0.41876(8) 0.25825(12) 0.0230(3) Uani d 1 . .
O O4 0.73302(18) 0.44856(8) 0.46133(13) 0.0222(3) Uani d 1 . .
O O5 0.71878(17) 0.42648(8) 0.73344(12) 0.0195(3) Uani d 1 . .
O O6 0.48713(17) 0.30743(8) 0.78234(13) 0.0218(3) Uani d 1 . .
C C13 0.2527(2) 0.45443(11) 0.54088(19) 0.0195(4) Uani d 1 . .
H H13A 0.236442 0.449615 0.630469 0.023 Uiso calc 1 . .
H H13B 0.140140 0.438240 0.477465 0.023 Uiso calc 1 . .
C C14 0.2910(2) 0.54005(11) 0.51597(18) 0.0163(3) Uani d 1 . .
C C15 0.2341(2) 0.57285(12) 0.39018(18) 0.0198(4) Uani d 1 . .
H H15 0.174579 0.540349 0.318265 0.024 Uiso calc 1 . .
C C16 0.2639(3) 0.65280(12) 0.36918(19) 0.0219(4) Uani d 1 . .
H H16 0.225820 0.675520 0.283818 0.026 Uiso calc 1 . .
C C17 0.3499(3) 0.69773(11) 0.4758(2) 0.0208(4) Uani d 1 . .
C C18 0.4101(3) 0.66781(12) 0.6009(2) 0.0244(4) Uani d 1 . .
H H18 0.471632 0.700546 0.671864 0.029 Uiso calc 1 . .
C C19 0.3782(3) 0.58792(11) 0.62033(18) 0.0207(4) Uani d 1 . .
H H19 0.416500 0.565899 0.706183 0.025 Uiso calc 1 . .
F F1 0.37075(17) 0.77671(7) 0.45766(13) 0.0326(3) Uani d 1 . .
N N1 0.3971(2) 0.39962(9) 0.52848(16) 0.0163(3) Uani d 1 . .
C C20 0.7731(3) 0.62051(13) -0.12663(18) 0.0267(4) Uani d 1 . .
H H20A 0.680694 0.658341 -0.119465 0.040 Uiso calc 1 . .
H H20B 0.718713 0.568831 -0.155602 0.040 Uiso calc 1 . .
H H20C 0.833561 0.640230 -0.190743 0.040 Uiso calc 1 . .
C C21 1.3829(3) 0.62488(17) 0.0606(3) 0.0488(7) Uani d 1 . .
H H21A 1.416737 0.593259 0.141486 0.073 Uiso calc 1 . .
H H21B 1.333859 0.675937 0.078879 0.073 Uiso calc 1 . .
H H21C 1.487832 0.634272 0.028394 0.073 Uiso calc 1 . .
N N2 1.0723(2) 0.54701(9) 0.00928(15) 0.0193(3) Uani d 1 . .
O O7 0.83510(19) 0.57408(10) 0.11422(14) 0.0300(3) Uani d 1 . .
O O8 1.00088(18) 0.68839(8) 0.06504(13) 0.0249(3) Uani d 1 . .
O O9 1.30638(19) 0.50125(8) -0.08761(14) 0.0257(3) Uani d 1 . .
O O10 1.1569(3) 0.62539(11) -0.17004(18) 0.0457(5) Uani d 1 . .
S S1 0.92849(5) 0.60997(3) 0.02782(4) 0.01762(10) Uani d 1 . .
S S2 1.22135(6) 0.57305(3) -0.05970(4) 0.02108(11) Uani d 1 . .
H H1C 0.360(3) 0.3504(16) 0.541(2) 0.024(6) Uiso d 1 . .
H H1D 0.410(3) 0.4047(16) 0.445(3) 0.028(6) Uiso d 1 . .
H H1E 0.497(4) 0.4087(16) 0.591(3) 0.031(7) 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 0.0227(9) 0.0187(9) 0.0373(11) -0.0070(8) 0.0097(8) -0.0034(8)
C2 0.0202(9) 0.0247(10) 0.0327(11) -0.0042(8) 0.0020(8) -0.0058(9)
C3 0.0356(11) 0.0221(10) 0.0199(9) 0.0009(8) -0.0041(8) 0.0000(8)
C4 0.0439(12) 0.0217(10) 0.0149(9) 0.0006(8) 0.0045(8) -0.0001(7)
C5 0.0329(11) 0.0294(11) 0.0213(9) 0.0031(9) 0.0131(8) 0.0048(8)
C6 0.0312(11) 0.0249(10) 0.0274(10) -0.0008(8) 0.0134(8) 0.0078(8)
C7 0.0194(9) 0.0193(9) 0.0292(10) -0.0026(7) 0.0094(8) -0.0028(8)
C8 0.0156(8) 0.0262(10) 0.0250(9) -0.0014(7) 0.0034(7) -0.0051(8)
C9 0.0253(10) 0.0218(10) 0.0185(9) 0.0038(8) -0.0002(7) 0.0011(7)
C10 0.0318(10) 0.0249(9) 0.0153(9) 0.0044(8) 0.0059(7) 0.0010(7)
C11 0.0255(10) 0.0296(11) 0.0259(10) 0.0048(8) 0.0134(8) 0.0100(8)
C12 0.0263(10) 0.0247(10) 0.0330(11) -0.0018(8) 0.0099(8) 0.0107(9)
O1 0.0243(7) 0.0184(6) 0.0249(7) -0.0024(5) 0.0067(5) 0.0032(5)
O2 0.0229(7) 0.0241(7) 0.0202(6) -0.0030(5) 0.0002(5) 0.0014(5)
O3 0.0301(7) 0.0221(7) 0.0169(6) 0.0001(6) 0.0065(5) -0.0006(5)
O4 0.0268(7) 0.0198(7) 0.0204(6) -0.0012(5) 0.0070(5) 0.0013(5)
O5 0.0179(6) 0.0211(7) 0.0189(6) 0.0020(5) 0.0037(5) 0.0017(5)
O6 0.0229(7) 0.0251(7) 0.0193(6) -0.0004(5) 0.0089(5) 0.0002(5)
C13 0.0173(9) 0.0165(9) 0.0260(9) 0.0017(7) 0.0078(7) 0.0020(7)
C14 0.0139(8) 0.0160(8) 0.0202(8) 0.0023(6) 0.0066(7) 0.0009(7)
C15 0.0212(8) 0.0185(8) 0.0183(8) 0.0017(8) 0.0026(7) -0.0030(7)
C16 0.0268(10) 0.0211(9) 0.0190(9) 0.0044(7) 0.0084(8) 0.0043(7)
C17 0.0194(9) 0.0134(8) 0.0313(10) -0.0009(7) 0.0100(8) 0.0018(7)
C18 0.0236(10) 0.0222(10) 0.0244(9) -0.0022(8) 0.0009(8) -0.0055(8)
C19 0.0220(9) 0.0219(10) 0.0171(8) 0.0032(7) 0.0034(7) 0.0012(7)
F1 0.0367(7) 0.0154(5) 0.0467(7) -0.0045(5) 0.0128(6) 0.0041(5)
N1 0.0170(7) 0.0137(7) 0.0174(8) 0.0005(6) 0.0035(6) 0.0014(6)
C20 0.0219(9) 0.0349(12) 0.0201(9) 0.0072(9) 0.0002(7) -0.0025(8)
C21 0.0246(11) 0.0479(16) 0.0802(19) -0.0139(11) 0.0247(12) -0.0354(14)
N2 0.0190(8) 0.0189(7) 0.0196(7) 0.0005(6) 0.0045(6) 0.0029(6)
O7 0.0270(7) 0.0401(8) 0.0266(7) -0.0023(7) 0.0137(6) 0.0046(7)
O8 0.0248(7) 0.0238(7) 0.0263(7) -0.0002(6) 0.0072(6) -0.0060(6)
O9 0.0262(7) 0.0247(7) 0.0266(7) 0.0082(6) 0.0075(6) -0.0007(6)
O10 0.0594(11) 0.0437(10) 0.0485(10) 0.0308(9) 0.0396(9) 0.0295(8)
S1 0.0166(2) 0.0223(2) 0.01400(19) 0.00056(18) 0.00407(15) -0.00003(17)
S2 0.0224(2) 0.0185(2) 0.0254(2) 0.00383(17) 0.01158(17) 0.00234(18)
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'
F F 0.0727 0.0534 '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
H1A C1 H1B . . 108.3 ?
C2 C1 H1A . . 109.9 ?
C2 C1 H1B . . 109.9 ?
O1 C1 H1A . . 109.9 ?
O1 C1 H1B . . 109.9 ?
O1 C1 C2 . . 108.99(16) ?
C1 C2 H2A . . 110.2 ?
C1 C2 H2B . . 110.2 ?
H2A C2 H2B . . 108.5 ?
O2 C2 C1 . . 107.68(16) ?
O2 C2 H2A . . 110.2 ?
O2 C2 H2B . . 110.2 ?
H3A C3 H3B . . 108.4 ?
C4 C3 H3A . . 110.0 ?
C4 C3 H3B . . 110.0 ?
O2 C3 H3A . . 110.0 ?
O2 C3 H3B . . 110.0 ?
O2 C3 C4 . . 108.42(17) ?
C3 C4 H4A . . 109.9 ?
C3 C4 H4B . . 109.9 ?
H4A C4 H4B . . 108.3 ?
O3 C4 C3 . . 109.12(16) ?
O3 C4 H4A . . 109.9 ?
O3 C4 H4B . . 109.9 ?
H5A C5 H5B . . 108.3 ?
C6 C5 H5A . . 110.0 ?
C6 C5 H5B . . 110.0 ?
O3 C5 H5A . . 110.0 ?
O3 C5 H5B . . 110.0 ?
O3 C5 C6 . . 108.69(15) ?
C5 C6 H6A . . 110.1 ?
C5 C6 H6B . . 110.1 ?
H6A C6 H6B . . 108.4 ?
O4 C6 C5 . . 108.11(16) ?
O4 C6 H6A . . 110.1 ?
O4 C6 H6B . . 110.1 ?
H7A C7 H7B . . 108.4 ?
C8 C7 H7A . . 110.0 ?
C8 C7 H7B . . 110.0 ?
O4 C7 H7A . . 110.0 ?
O4 C7 H7B . . 110.0 ?
O4 C7 C8 . . 108.30(15) ?
C7 C8 H8A . . 110.0 ?
C7 C8 H8B . . 110.0 ?
H8A C8 H8B . . 108.3 ?
O5 C8 C7 . . 108.65(15) ?
O5 C8 H8A . . 110.0 ?
O5 C8 H8B . . 110.0 ?
H9A C9 H9B . . 108.3 ?
C10 C9 H9A . . 110.0 ?
C10 C9 H9B . . 110.0 ?
O5 C9 H9A . . 110.0 ?
O5 C9 H9B . . 110.0 ?
O5 C9 C10 . . 108.68(15) ?
C9 C10 H10A . . 110.1 ?
C9 C10 H10B . . 110.1 ?
H10A C10 H10B . . 108.4 ?
O6 C10 C9 . . 108.10(15) ?
O6 C10 H10A . . 110.1 ?
O6 C10 H10B . . 110.1 ?
H11A C11 H11B . . 108.4 ?
C12 C11 H11A . . 110.1 ?
C12 C11 H11B . . 110.1 ?
O6 C11 H11A . . 110.1 ?
O6 C11 H11B . . 110.1 ?
O6 C11 C12 . . 107.91(16) ?
C11 C12 H12A . . 110.0 ?
C11 C12 H12B . . 110.0 ?
H12A C12 H12B . . 108.4 ?
O1 C12 C11 . . 108.56(16) ?
O1 C12 H12A . . 110.0 ?
O1 C12 H12B . . 110.0 ?
C1 O1 C12 . . 112.10(15) ?
C3 O2 C2 . . 112.88(15) ?
C5 O3 C4 . . 112.03(15) ?
C7 O4 C6 . . 112.35(15) ?
C9 O5 C8 . . 111.16(14) ?
C11 O6 C10 . . 112.71(14) ?
H13A C13 H13B . . 107.8 ?
C14 C13 H13A . . 109.0 ?
C14 C13 H13B . . 109.0 ?
N1 C13 H13A . . 109.0 ?
N1 C13 H13B . . 109.0 ?
N1 C13 C14 . . 112.72(15) ?
C15 C14 C13 . . 121.04(17) ?
C19 C14 C13 . . 119.61(16) ?
C19 C14 C15 . . 119.31(17) ?
C14 C15 H15 . . 119.7 ?
C16 C15 C14 . . 120.59(18) ?
C16 C15 H15 . . 119.7 ?
C15 C16 H16 . . 121.1 ?
C17 C16 C15 . . 117.85(18) ?
C17 C16 H16 . . 121.1 ?
C18 C17 C16 . . 123.57(18) ?
F1 C17 C16 . . 118.27(18) ?
F1 C17 C18 . . 118.11(18) ?
C17 C18 H18 . . 121.1 ?
C17 C18 C19 . . 117.82(18) ?
C19 C18 H18 . . 121.1 ?
C14 C19 C18 . . 120.85(17) ?
C14 C19 H19 . . 119.6 ?
C18 C19 H19 . . 119.6 ?
C13 N1 H1C . . 106.1(16) ?
C13 N1 H1D . . 107.7(16) ?
C13 N1 H1E . . 111.2(17) ?
H1C N1 H1D . . 110(2) ?
H1C N1 H1E . . 107(2) ?
H1D N1 H1E . . 114(2) ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
S1 C20 H20A . . 109.5 ?
S1 C20 H20B . . 109.5 ?
S1 C20 H20C . . 109.5 ?
H21A C21 H21B . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
S2 N2 S1 . . 119.92(10) ?
N2 S1 C20 . . 106.68(9) ?
O7 S1 C20 . . 106.71(9) ?
O7 S1 N2 . . 106.90(9) ?
O7 S1 O8 . . 115.87(9) ?
O8 S1 C20 . . 106.36(10) ?
O8 S1 N2 . . 113.74(8) ?
N2 S2 C21 . . 106.07(11) ?
O9 S2 C21 . . 106.32(11) ?
O9 S2 N2 . . 107.15(9) ?
O10 S2 C21 . . 107.97(15) ?
O10 S2 N2 . . 113.47(9) ?
O10 S2 O9 . . 115.26(9) ?
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 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C1 C2 . 1.500(3) ?
C1 O1 . 1.431(2) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 O2 . 1.428(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.496(3) ?
C3 O2 . 1.428(2) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4 O3 . 1.432(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.503(3) ?
C5 O3 . 1.431(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C6 O4 . 1.424(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.505(3) ?
C7 O4 . 1.422(2) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C8 O5 . 1.436(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.505(3) ?
C9 O5 . 1.432(2) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C10 O6 . 1.426(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C11 C12 . 1.502(3) ?
C11 O6 . 1.426(2) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C12 O1 . 1.435(2) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.508(2) ?
C13 N1 . 1.488(2) ?
C14 C15 . 1.396(3) ?
C14 C19 . 1.387(3) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.393(3) ?
C16 H16 . 0.9500 ?
C16 C17 . 1.373(3) ?
C17 C18 . 1.373(3) ?
C17 F1 . 1.358(2) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.392(3) ?
C19 H19 . 0.9500 ?
N1 H1C . 0.90(3) ?
N1 H1D . 0.92(3) ?
N1 H1E . 0.89(3) ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
C20 S1 . 1.7613(19) ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C21 S2 . 1.763(2) ?
N2 S1 . 1.5926(16) ?
N2 S2 . 1.5899(16) ?
O7 S1 . 1.4428(14) ?
O8 S1 . 1.4475(14) ?
O9 S2 . 1.4459(14) ?
O10 S2 . 1.4391(16) ?
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 H1C O1 . 0.90(3) 2.02(3) 2.842(2) 152(2) yes
N1 H1D O3 . 0.92(3) 1.99(3) 2.914(2) 175(2) yes
N1 H1E O5 . 0.89(3) 1.99(3) 2.879(2) 179(3) 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
C1 C2 O2 C3 . . . . 174.75(15) ?
C2 C1 O1 C12 . . . . 175.10(16) ?
C3 C4 O3 C5 . . . . 177.98(16) ?
C4 C3 O2 C2 . . . . -175.00(16) ?
C5 C6 O4 C7 . . . . -177.13(15) ?
C6 C5 O3 C4 . . . . 178.90(15) ?
C7 C8 O5 C9 . . . . -179.99(15) ?
C8 C7 O4 C6 . . . . -177.64(15) ?
C9 C10 O6 C11 . . . . -178.98(15) ?
C10 C9 O5 C8 . . . . -176.84(15) ?
C11 C12 O1 C1 . . . . 178.08(15) ?
C12 C11 O6 C10 . . . . -176.71(15) ?
O1 C1 C2 O2 . . . . 68.9(2) ?
O2 C3 C4 O3 . . . . -63.5(2) ?
O3 C5 C6 O4 . . . . 68.7(2) ?
O4 C7 C8 O5 . . . . -75.47(18) ?
O5 C9 C10 O6 . . . . 67.23(19) ?
O6 C11 C12 O1 . . . . -67.8(2) ?
C13 C14 C15 C16 . . . . 177.39(17) ?
C13 C14 C19 C18 . . . . -177.91(17) ?
C14 C15 C16 C17 . . . . -0.2(3) ?
C15 C14 C19 C18 . . . . -0.4(3) ?
C15 C16 C17 C18 . . . . 1.0(3) ?
C15 C16 C17 F1 . . . . -176.39(17) ?
C16 C17 C18 C19 . . . . -1.5(3) ?
C17 C18 C19 C14 . . . . 1.1(3) ?
C19 C14 C15 C16 . . . . -0.1(3) ?
F1 C17 C18 C19 . . . . 175.93(17) ?
N1 C13 C14 C15 . . . . 91.3(2) ?
N1 C13 C14 C19 . . . . -91.2(2) ?
S1 N2 S2 C21 . . . . 78.68(15) ?
S1 N2 S2 O9 . . . . -168.06(10) ?
S1 N2 S2 O10 . . . . -39.68(15) ?
S2 N2 S1 C20 . . . . 76.98(13) ?
S2 N2 S1 O7 . . . . -169.15(10) ?
S2 N2 S1 O8 . . . . -39.96(13) ?
_cod_database_fobs_code 2312783