#------------------------------------------------------------------------------
#$Date: 2025-03-14 05:12:06 +0200 (Fri, 14 Mar 2025) $
#$Revision: 298435 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312785.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_2312785
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_formula_iupac 'C7 H9 Br N +, C2 H6 N O4 S2 -, C12 H24 O6'
_chemical_formula_moiety 'C7 H9 Br N +, C2 H6 N O4 S2 -, C12 H24 O6'
_chemical_formula_sum 'C21 H39 Br N2 O10 S2'
_chemical_formula_weight 623.57
_chemical_name_common
;
4-Bromobenzylaminium di(methanesulfonyl)amidate--18-crown-6 (1/1)
;
_chemical_name_systematic
'4-Bromobenzylaminium [(methanesulfonylazanidyl)sulfonyl]methane--1,4,7,10,13,16-hexaoxacyclooctadecane (1/1)'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary 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 105.6590(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.02390(10)
_cell_length_b 17.69260(10)
_cell_length_c 15.1608(2)
_cell_measurement_reflns_used 19691
_cell_measurement_temperature 99.99(10)
_cell_measurement_theta_max 71.6840
_cell_measurement_theta_min 2.4710
_cell_volume 2847.24(5)
_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 99.99(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 0.986
_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 0.0381
_diffrn_reflns_av_unetI/netI 0.0241
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 28808
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.993
_diffrn_reflns_theta_min 3.926
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 3.799
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.56516
_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 1.455
_exptl_crystal_description plate
_exptl_crystal_F_000 1304
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.657
_refine_diff_density_min -0.774
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 339
_refine_ls_number_reflns 5514
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.079
_refine_ls_R_factor_all 0.0343
_refine_ls_R_factor_gt 0.0318
_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^)+(0.0508P)^2^+1.4365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0871
_refine_ls_wR_factor_ref 0.0885
_reflns_number_gt 5091
_reflns_number_total 5514
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3091sup1.cif
_cod_data_source_block zy-241018-2-100k_auto
_cod_database_code 2312785
_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 0.517
_shelx_estimated_absorpt_t_max 0.726
_shelx_hkl_file
;
0 0 1 0.74 0.30
0 0 -1 0.31 0.30
0 0 -2 3816.44 128.27
0 0 2 4026.86 127.82
0 0 -2 3798.95 128.41
0 0 2 3996.38 128.86
0 0 3 1.03 1.68
0 0 -3 0.52 0.86
0 0 -3 0.86 1.03
0 0 3 0.41 0.50
0 0 -4 9265.47 315.84
0 0 4 9999.00 314.58
0 0 -4 9370.13 315.55
0 0 4 9572.20 316.84
0 0 5 -1.49 2.32
0 0 -5 1.30 1.23
0 0 5 1.14 0.64
0 0 -5 -0.43 1.51
0 0 6 2239.76 71.55
0 0 6 2065.24 75.13
0 0 -6 2068.72 73.64
0 0 -7 0.67 1.58
0 0 -7 0.37 1.36
0 0 7 0.33 2.58
0 0 -7 -0.76 1.28
0 0 -8 1462.04 52.77
0 0 8 1474.50 55.70
0 0 8 1518.04 56.88
0 0 -8 1587.02 52.99
0 0 -9 1.08 1.81
0 0 -9 0.27 1.58
0 0 9 -0.54 3.40
0 0 10 26.63 3.74
0 0 10 21.30 5.10
0 0 -10 20.64 3.37
0 0 -10 23.40 3.54
0 0 10 19.24 4.55
0 0 11 -0.58 2.95
0 0 -11 1.17 1.74
0 0 11 0.35 2.08
0 0 -11 -1.08 1.90
0 0 -11 -0.36 2.31
0 0 -12 603.21 26.10
0 0 -12 581.85 24.94
0 0 -13 -2.02 2.84
0 0 -14 104.48 7.89
0 0 14 104.93 7.82
0 0 -14 104.03 7.22
0 0 -14 88.59 7.02
0 0 -15 -0.27 1.63
0 0 -15 1.17 1.96
0 0 -15 -0.33 1.95
0 0 15 -0.65 1.78
0 0 -16 3.56 1.61
0 0 -16 3.89 1.73
0 0 16 5.68 2.20
0 0 -16 4.73 1.82
0 0 -17 -0.89 1.25
0 0 17 -0.62 1.33
0 0 -17 1.03 1.21
0 -1 0 1.72 0.26
0 1 0 0.46 0.22
0 1 0 1.67 0.19
0 -1 0 1.21 0.18
0 -1 0 0.04 0.36
0 1 0 0.29 0.31
0 -1 1 12.57 0.71
0 -1 1 13.42 0.79
0 -1 1 12.64 0.63
0 1 -1 13.50 0.74
0 -1 1 11.61 0.65
0 -1 -1 12.70 1.01
0 1 -1 12.08 0.66
0 -1 1 14.10 0.76
0 1 -1 11.76 0.82
0 -1 1 14.11 0.85
0 1 -1 14.84 0.67
0 -1 -1 12.43 0.90
0 1 1 13.23 0.89
0 -1 1 12.59 0.68
0 1 -1 12.17 0.67
0 -1 1 11.72 0.64
0 1 1 12.54 1.07
0 -1 2 283.92 10.26
0 -1 -2 303.87 10.77
0 1 -2 313.51 10.53
0 -1 2 316.57 10.28
0 -1 2 293.54 10.54
0 -1 2 310.75 10.48
0 -1 -2 309.15 11.00
0 1 -2 308.33 10.58
0 -1 2 331.24 11.28
0 1 2 313.04 11.28
0 1 -3 30.97 1.94
0 -1 -3 28.63 2.14
0 -1 3 28.53 1.93
0 1 -3 30.77 2.09
0 -1 -3 32.19 2.45
0 1 3 32.29 2.86
0 -1 3 33.54 2.85
0 -1 3 35.56 1.61
0 -1 -4 8108.20 273.49
0 1 -4 8249.88 273.11
0 1 -4 8140.25 272.85
0 -1 -4 8018.65 273.09
0 -1 4 8321.72 274.25
0 1 4 8258.78 274.29
0 1 4 8443.31 271.89
0 -1 4 8786.39 272.11
0 -1 -5 333.95 14.07
0 1 -5 341.13 13.68
0 1 5 362.89 12.20
0 -1 5 373.79 12.44
0 -1 -5 341.90 13.61
0 1 -5 351.51 13.41
0 -1 5 352.43 14.93
0 1 5 357.49 15.15
0 1 6 1.11 2.70
0 -1 6 0.79 2.27
0 -1 -6 0.39 1.63
0 1 -6 1.01 1.44
0 1 -6 0.43 1.14
0 1 6 1.30 0.62
0 -1 -7 335.28 15.06
0 1 -7 349.17 14.72
0 -1 7 351.43 16.95
0 -1 7 334.57 16.19
0 1 7 365.59 16.82
0 1 -7 363.53 14.43
0 -1 -7 358.04 14.60
0 -1 -7 344.39 14.46
0 1 -7 358.94 14.30
0 1 8 161.96 10.89
0 -1 8 157.43 10.53
0 -1 -8 191.26 9.32
0 1 -8 176.18 8.84
0 1 -8 176.12 8.91
0 1 9 413.12 22.56
0 1 9 400.56 21.16
0 1 -9 454.41 18.58
0 -1 -9 419.31 18.60
0 -1 -9 435.52 18.66
0 1 -9 449.45 18.57
0 -1 10 426.03 17.31
0 1 10 351.85 20.61
0 -1 10 345.69 18.69
0 1 10 350.66 19.61
0 -1 -10 353.28 16.58
0 1 -10 357.10 16.31
0 1 -10 360.49 16.37
0 -1 -10 349.59 16.51
0 1 11 360.52 22.07
0 1 11 377.04 21.53
0 -1 -11 415.99 18.76
0 1 -11 413.46 18.46
0 1 -11 401.95 17.54
0 -1 -11 382.11 18.42
0 1 -11 390.44 18.15
0 -1 -11 409.65 17.74
0 1 12 180.74 13.67
0 1 12 196.58 11.31
0 -1 -12 155.81 9.74
0 1 -12 166.39 9.78
0 -1 -12 168.26 10.83
0 1 -12 170.97 10.65
0 1 -13 13.56 3.12
0 -1 -13 9.58 3.17
0 1 14 125.38 8.57
0 -1 14 118.17 8.36
0 -1 -14 124.29 8.11
0 1 -14 111.73 7.54
0 -1 -14 111.26 8.50
0 1 -14 109.89 8.10
0 1 -14 113.93 7.80
0 -1 -15 5.81 2.41
0 1 -15 10.29 2.57
0 -1 -15 7.34 2.23
0 1 -15 6.39 2.09
0 1 15 5.81 2.33
0 -1 15 3.58 2.27
0 1 -15 6.33 2.23
0 -1 -15 6.06 2.21
0 1 16 216.93 10.79
0 -1 16 220.67 10.97
0 1 -16 207.30 9.75
0 -1 -16 214.88 10.18
0 -1 -16 210.86 10.69
0 -1 -16 214.68 10.39
0 1 -16 195.48 9.79
0 1 17 1.41 1.36
0 -1 17 0.85 1.58
0 -1 -17 0.50 1.15
0 1 -17 -0.13 0.98
0 -1 -17 1.10 1.14
0 -2 0 44.84 1.71
0 -2 0 43.75 2.18
0 -2 0 39.94 1.67
0 -2 0 45.10 1.87
0 -2 0 45.30 1.90
0 2 0 45.14 1.70
0 -2 0 44.68 1.76
0 -2 1 9.81 0.83
0 -2 1 9.07 0.80
0 -2 1 12.96 0.72
0 -2 1 9.32 0.68
0 -2 -1 10.15 1.14
0 -2 1 10.48 0.69
0 -2 1 9.46 0.70
0 2 1 9.79 1.16
0 -2 1 9.95 0.92
0 -2 -2 109.70 4.59
0 2 -2 111.75 4.08
0 -2 2 109.48 4.21
0 -2 2 113.07 4.33
0 -2 2 107.93 4.08
0 -2 2 92.76 3.99
0 2 2 107.56 4.99
0 -2 2 109.49 4.06
0 -2 -2 112.82 4.90
0 -2 2 99.41 4.05
0 -2 2 117.12 3.84
0 -2 2 111.99 4.43
0 -2 2 109.83 4.27
0 -2 3 647.58 22.50
0 -2 3 695.63 22.52
0 2 3 681.35 24.07
0 -2 3 660.43 23.65
0 -2 -3 682.13 23.73
0 2 -3 703.08 22.83
0 -2 -3 674.32 23.33
0 -2 3 640.82 23.48
0 -2 3 671.31 22.61
0 -2 3 678.68 23.11
0 -2 3 681.40 22.82
0 -2 3 679.49 22.94
0 2 -3 683.10 22.90
0 -2 4 1450.73 46.74
0 -2 -4 1376.86 48.25
0 2 -4 1448.26 47.53
0 2 -4 1438.36 47.32
0 -2 -4 1362.24 47.78
0 -2 4 1421.80 47.27
0 -2 4 1434.15 47.69
0 -2 4 1378.44 48.58
0 2 4 1412.18 48.97
0 -2 4 1387.52 48.56
0 -2 -5 2.06 1.76
0 2 -5 3.04 1.26
0 -2 5 3.18 2.28
0 2 5 4.73 2.72
0 2 -5 3.06 1.25
0 -2 -5 2.05 1.34
0 2 5 2.43 0.59
0 -2 5 3.22 2.56
0 -2 5 2.56 1.57
0 2 -6 1709.44 58.63
0 -2 -6 1659.50 59.51
0 -2 6 1624.35 60.09
0 2 -6 1712.69 58.43
0 2 6 1762.12 56.58
0 -2 6 1667.01 60.08
0 2 6 1715.29 60.83
0 -2 6 1776.60 58.81
0 2 -6 1736.04 58.31
0 2 -7 146.11 7.66
0 -2 -7 161.34 8.20
0 -2 7 169.69 8.22
0 -2 7 148.26 9.32
0 -2 7 156.38 9.32
0 2 7 172.05 10.39
0 -2 -7 174.59 8.43
0 -2 -7 151.13 8.62
0 -2 8 1773.24 58.31
0 2 -8 1645.70 57.80
0 2 -8 1655.66 57.67
0 -2 -8 1663.01 58.26
0 -2 8 1610.01 59.91
0 -2 9 14.14 3.50
0 2 9 9.72 3.81
0 -2 -9 10.80 2.60
0 2 -9 13.25 2.56
0 -2 9 14.84 2.84
0 2 -9 14.64 2.64
0 -2 -9 13.81 2.73
0 -2 -10 160.94 9.70
0 2 -10 156.85 9.23
0 2 10 150.63 12.00
0 -2 10 167.06 9.58
0 2 10 171.16 13.71
0 -2 -10 163.22 9.73
0 2 -10 160.73 8.67
0 2 -10 160.79 9.22
0 -2 11 10.44 2.85
0 2 11 9.98 5.15
0 2 -11 10.84 2.42
0 -2 -11 13.49 2.83
0 2 11 13.17 4.47
0 -2 -11 12.56 3.31
0 2 -11 9.73 2.70
0 -2 -11 10.50 2.81
0 -2 -12 409.80 18.74
0 2 12 378.45 23.76
0 -2 -12 423.12 19.88
0 2 -12 403.85 19.06
0 2 -12 417.35 18.38
0 2 12 396.28 23.00
0 2 12 481.43 20.41
0 -2 12 488.87 20.06
0 -2 -13 69.64 6.81
0 2 -13 60.44 5.85
0 2 -14 25.99 3.52
0 -2 14 29.10 4.10
0 2 14 14.53 3.33
0 -2 -14 17.25 3.57
0 2 -14 22.14 3.20
0 -2 -14 18.18 3.33
0 -2 -15 38.19 4.55
0 2 -15 37.22 3.89
0 -2 -15 33.35 4.20
0 -2 15 36.30 4.42
0 2 15 44.42 4.77
0 -2 -15 42.54 4.38
0 2 -15 36.02 3.70
0 -2 -16 68.30 5.43
0 -2 -16 66.32 5.18
0 2 16 69.21 5.35
0 -2 16 74.51 5.69
0 -2 -16 62.87 4.88
0 -2 -17 2.81 1.43
0 2 17 3.11 1.54
0 -2 17 4.94 1.72
0 -2 -17 4.55 1.56
0 -3 0 1.00 0.45
0 3 0 0.38 0.39
0 -3 0 0.47 0.44
0 3 0 0.32 0.38
0 -3 0 0.98 0.54
0 -3 0 0.60 0.64
0 -3 0 0.85 0.60
0 -3 0 0.65 1.07
0 -3 1 126.77 4.53
0 -3 -1 123.18 4.74
0 -3 1 123.22 4.74
0 3 1 123.07 5.17
0 -3 1 123.28 4.49
0 -3 1 128.50 4.98
0 -3 1 122.21 4.55
0 -3 -1 125.81 5.26
0 -3 -1 123.53 4.89
0 -3 1 128.07 4.81
0 -3 1 123.21 4.49
0 -3 2 1548.49 51.74
0 -3 2 1534.73 51.70
0 -3 2 1548.73 52.13
0 -3 2 1732.11 51.85
0 -3 2 1566.12 51.86
0 -3 2 1551.46 52.08
0 3 -2 1602.24 51.52
0 -3 -2 1540.38 52.36
0 3 2 1548.35 52.86
0 -3 2 1585.84 52.02
0 -3 -2 1570.49 52.80
0 -3 3 4867.09 158.69
0 3 -3 4965.78 158.69
0 -3 -3 4763.65 159.99
0 -3 -3 4880.65 159.53
0 3 -3 5085.67 158.71
0 -3 3 4743.64 158.15
0 -3 3 4895.48 158.61
0 3 3 5020.57 160.36
0 -3 3 4926.17 158.89
0 -3 3 5045.68 159.08
0 -3 3 4962.88 159.20
0 -3 3 4379.81 158.19
0 -3 3 5046.53 158.18
0 -3 4 104.58 4.89
0 -3 4 97.52 4.83
0 -3 4 119.92 5.34
0 -3 4 125.39 5.28
0 -3 4 117.66 5.09
0 -3 -4 119.31 5.62
0 3 -4 123.09 4.97
0 -3 4 117.94 4.64
0 -3 4 119.40 4.77
0 -3 -4 107.14 5.98
0 3 -4 115.40 5.03
0 3 4 119.20 6.65
0 -3 5 54.93 4.14
0 3 5 66.12 5.15
0 -3 5 56.82 3.43
0 3 -5 62.93 3.55
0 3 -5 59.33 3.53
0 -3 -5 62.54 4.48
0 3 -5 61.82 3.39
0 -3 5 47.12 3.63
0 -3 5 47.35 3.67
0 -3 6 828.79 33.35
0 3 -6 1013.31 33.25
0 3 6 986.42 35.98
0 -3 6 957.48 34.32
0 -3 6 966.50 33.39
0 -3 -6 992.43 33.85
0 3 -6 982.22 32.99
0 -3 6 881.36 33.50
0 -3 -6 938.13 34.47
0 3 -7 188.25 8.51
0 -3 -7 171.20 8.80
0 -3 -7 167.77 8.85
0 3 7 169.31 10.66
0 -3 -7 171.13 9.51
0 -3 7 180.61 8.62
0 3 -8 1139.90 41.13
0 -3 -8 1138.43 41.98
0 3 -8 1103.62 40.88
0 3 9 12.85 4.48
0 3 -9 13.48 2.24
0 -3 9 15.58 2.89
0 -3 -9 9.93 2.56
0 3 -9 13.05 2.35
0 -3 -9 15.46 3.04
0 3 10 19.23 4.89
0 -3 -10 12.19 2.77
0 3 -10 12.79 2.38
0 -3 10 11.77 2.74
0 -3 -10 15.72 3.19
0 3 -10 13.93 2.73
0 3 10 8.40 5.00
0 3 11 106.72 11.61
0 3 11 90.08 9.86
0 -3 -11 92.39 7.60
0 3 -11 98.99 7.20
0 3 -11 101.29 6.73
0 -3 -11 99.23 7.93
0 -3 -11 107.08 7.31
0 -3 11 114.89 7.77
0 3 12 166.05 14.76
0 -3 12 182.60 10.54
0 3 -12 150.99 9.03
0 3 12 166.99 13.87
0 -3 -12 162.14 9.83
0 -3 -12 182.03 11.17
0 3 -12 162.30 9.84
0 3 13 16.28 5.59
0 3 13 31.13 6.48
0 3 -13 28.36 3.74
0 -3 13 34.57 4.57
0 3 13 36.83 4.91
0 -3 -13 29.99 4.76
0 -3 -14 130.04 8.51
0 -3 -14 120.06 9.07
0 -3 14 137.65 9.05
0 3 14 129.39 8.76
0 -3 -15 12.35 2.93
0 -3 -15 9.78 2.45
0 -3 -15 10.58 2.87
0 -3 15 14.11 3.17
0 3 15 15.44 3.03
0 -3 -16 36.17 3.81
0 -3 -16 38.61 3.67
0 3 16 31.64 3.70
0 -3 16 36.22 4.04
0 -3 -16 35.37 3.95
0 -3 -17 0.18 1.20
0 -3 -17 0.98 1.25
0 4 0 291.98 10.03
0 -4 0 289.73 10.14
0 -4 0 294.70 10.16
0 -4 0 312.93 10.55
0 -4 0 308.51 10.47
0 -4 0 299.38 10.25
0 4 0 290.61 10.02
0 -4 0 292.08 10.14
0 -4 -1 733.86 24.52
0 -4 1 743.97 24.44
0 -4 1 766.95 24.40
0 -4 -1 747.29 24.38
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-12 -7 -1 63.63 3.33
-12 8 9 21.59 3.42
-12 8 8 88.05 6.69
-12 8 7 6.63 2.46
-12 8 6 152.69 8.01
12 8 -6 116.98 6.74
-12 8 5 70.58 5.25
12 8 -5 58.95 4.50
-12 8 4 1.79 1.68
12 8 -4 -0.21 1.31
-12 8 3 145.69 7.58
12 8 -3 129.66 7.41
-12 -8 2 67.02 3.63
-12 8 2 85.70 5.10
-12 -8 1 63.60 3.41
-12 8 1 68.19 4.42
-12 9 8 139.44 8.27
-12 9 7 -1.12 1.92
-12 9 6 34.81 4.01
-12 9 5 35.22 3.44
-12 9 5 36.35 4.04
-12 9 4 370.63 15.11
12 9 -3 8.73 1.79
-12 9 3 9.59 2.03
13 0 -10 0.64 1.38
13 0 -9 54.09 4.53
13 0 -8 -0.78 1.58
13 0 -7 163.71 9.10
13 0 -6 1.37 1.59
13 0 -5 8.91 2.34
13 0 -4 -0.77 1.70
13 0 -3 172.98 9.13
13 0 -2 0.84 1.30
13 -1 -10 8.07 1.98
13 1 -9 125.88 7.33
13 -1 -9 133.78 7.61
13 1 -8 5.31 1.99
13 -1 -8 3.12 1.87
13 1 -7 4.52 1.98
13 -1 -7 6.98 2.17
13 1 -6 31.26 3.74
13 -1 -6 28.32 3.56
13 -1 -5 100.24 6.60
13 1 -5 98.38 6.67
13 1 -4 2.86 1.80
13 -1 -4 1.49 1.72
-13 1 4 0.77 1.48
-13 1 3 89.36 5.43
13 1 -3 96.81 6.31
13 -1 -3 86.47 5.82
13 1 -2 12.23 2.30
-13 1 2 12.62 2.15
-13 1 1 43.13 3.33
13 1 -1 39.98 3.53
13 2 -9 1.29 1.33
13 -2 -9 1.66 1.74
13 -2 -8 3.52 1.77
13 2 -8 2.62 1.59
13 2 -7 -1.53 1.50
13 -2 -7 -0.26 1.69
-13 2 6 45.61 3.98
13 -2 -6 40.13 4.07
13 2 -6 45.44 4.31
13 2 -5 7.58 2.17
13 -2 -5 7.92 2.15
-13 2 5 5.20 1.86
13 2 -4 19.12 3.02
-13 2 4 22.80 2.78
13 2 -3 8.66 2.23
-13 2 3 7.47 1.92
-13 2 2 54.67 4.04
13 2 -2 51.95 4.36
-13 2 1 100.27 5.34
13 2 -1 85.01 5.41
13 -3 -9 1.12 1.42
13 -3 -8 3.30 1.75
13 3 -8 3.26 1.58
-13 3 7 96.26 5.92
13 3 -7 84.44 5.88
13 -3 -7 91.65 6.01
-13 3 6 47.27 4.06
13 3 -6 46.02 4.25
-13 3 5 205.78 9.66
13 3 -5 188.56 9.91
13 3 -4 14.81 2.62
-13 3 4 10.37 2.20
13 3 -3 2.54 1.60
-13 3 3 -0.57 1.41
13 3 -2 3.79 1.59
-13 3 2 6.65 1.75
-13 3 1 134.99 6.56
13 3 -1 121.78 6.69
13 4 -8 2.67 1.46
13 4 -7 20.00 2.71
-13 4 7 26.52 3.12
13 4 -6 7.09 1.89
-13 4 6 5.96 1.95
-13 4 5 68.94 4.94
13 4 -5 69.85 5.08
-13 4 4 34.18 3.36
13 4 -4 28.42 3.26
-13 4 3 290.62 12.03
13 4 -3 261.42 12.12
13 4 -2 0.20 1.28
-13 4 2 -0.51 1.26
13 4 -1 12.48 1.97
-13 5 7 13.18 2.58
-13 5 6 5.91 2.01
13 5 -6 5.59 1.58
-13 5 5 2.58 1.68
13 5 -5 2.78 1.44
-13 5 4 2.46 1.64
13 5 -4 0.20 1.26
-13 5 3 19.19 2.48
13 5 -3 15.81 2.30
-13 5 2 3.30 1.43
13 5 -2 2.80 1.34
-13 6 5 130.38 6.87
0 0 0 0.00 0.00
TITL zy-241018-2-100k_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 11.023933 17.692631 15.160799 90.0000 105.6593 90.0000
ZERR 32.00 0.000116 0.000142 0.000162 0.0000 0.0011 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O S Br
UNIT 32.00 32.00 32.00 32.00 32.00 32.00
REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 43872
_shelx_res_file
;
TITL zy-241018-2-100k_auto_a.res in P2(1)/n
zy-241018-2-100k_auto.res
created by SHELXL-2018/3 at 09:03:35 on 10-Mar-2025
REM Old TITL zy-241018-2-100k_auto_a.res in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.114, Rweak 0.009, Alpha 0.031
REM 0.761 for 202 systematic absences, Orientation as input
REM Formula found by SHELXT: C21 Br N O11 S2
CELL 1.54184 11.0239 17.6926 15.1608 90 105.659 90
ZERR 4 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br N O S
UNIT 84 156 4 8 40 8
L.S. 4
PLAN 5
SIZE 0.1 0.2 0.09
TEMP -173
CONF
HTAB N1 O5
HTAB N1 O3
HTAB N1 O1
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.050800 1.436500
FVAR 0.38168
BR1 3 0.337174 0.742969 0.331836 11.00000 0.03376 0.01420 =
0.02924 0.00379 0.00087 0.00154
N1 4 0.308747 0.354050 0.351844 11.00000 0.01650 0.01314 =
0.01804 0.00007 0.00300 -0.00048
H1C 2 0.333340 0.360220 0.304585 11.00000 0.01743
H1D 2 0.229795 0.365155 0.336834 11.00000 0.02591
H1E 2 0.318802 0.309709 0.368812 11.00000 0.01945
C13 1 0.380897 0.403516 0.428648 11.00000 0.02004 0.01474 =
0.01976 -0.00067 -0.00046 -0.00132
AFIX 23
H13A 2 0.470927 0.388931 0.445248 11.00000 -1.20000
H13B 2 0.349015 0.395539 0.483047 11.00000 -1.20000
AFIX 0
C14 1 0.368880 0.485844 0.402654 11.00000 0.01660 0.01497 =
0.01806 -0.00163 -0.00156 -0.00100
C15 1 0.277192 0.529978 0.425121 11.00000 0.01701 0.01972 =
0.02926 -0.00005 0.00629 -0.00270
AFIX 43
H15 2 0.221622 0.507739 0.455919 11.00000 -1.20000
AFIX 0
C16 1 0.266140 0.606286 0.402932 11.00000 0.01671 0.01887 =
0.03242 -0.00150 0.00389 0.00318
AFIX 43
H16 2 0.203343 0.636355 0.418212 11.00000 -1.20000
AFIX 0
C17 1 0.347970 0.637881 0.358226 11.00000 0.01919 0.01354 =
0.02165 0.00106 -0.00303 -0.00041
C18 1 0.440717 0.595381 0.335427 11.00000 0.02223 0.01907 =
0.02036 -0.00149 0.00389 -0.00393
AFIX 43
H18 2 0.496335 0.617875 0.304857 11.00000 -1.20000
AFIX 0
C19 1 0.450546 0.519180 0.358263 11.00000 0.01817 0.01834 =
0.02225 -0.00341 0.00418 0.00087
AFIX 43
H19 2 0.513926 0.489367 0.343374 11.00000 -1.20000
AFIX 0
S1 6 0.817369 0.034562 0.361503 11.00000 0.01542 0.01646 =
0.01862 0.00089 0.00139 0.00016
S2 6 0.726554 0.091396 0.186601 11.00000 0.01695 0.03051 =
0.01878 0.00411 0.00369 0.00524
O7 5 0.784321 0.163551 0.217230 11.00000 0.02627 0.02564 =
0.03450 0.00935 0.00724 0.00202
O8 5 0.729017 0.068604 0.095679 11.00000 0.03083 0.05687 =
0.01961 0.00184 0.00595 0.00992
O9 5 0.721789 0.075601 0.391350 11.00000 0.02545 0.02805 =
0.02364 -0.00031 0.00792 0.00699
O10 5 0.847840 -0.038948 0.402841 11.00000 0.02373 0.01880 =
0.03038 0.00640 0.00368 0.00179
N2 4 0.783269 0.022823 0.253220 11.00000 0.02007 0.02073 =
0.02005 -0.00196 0.00325 0.00334
C20 1 0.956861 0.088808 0.391683 11.00000 0.02508 0.02983 =
0.02492 0.00254 -0.00239 -0.01059
AFIX 137
H20A 2 0.987827 0.091793 0.458557 11.00000 -1.50000
H20B 2 0.939317 0.139835 0.366298 11.00000 -1.50000
H20C 2 1.020890 0.064913 0.366952 11.00000 -1.50000
AFIX 0
C21 1 0.565787 0.099838 0.184236 11.00000 0.01648 0.04085 =
0.02850 0.00705 0.00333 0.00742
AFIX 137
H21A 2 0.558941 0.111936 0.245789 11.00000 -1.50000
H21B 2 0.522485 0.051996 0.163815 11.00000 -1.50000
H21C 2 0.526886 0.140258 0.141793 11.00000 -1.50000
AFIX 0
O1 5 0.388626 0.217978 0.454467 11.00000 0.03300 0.01554 =
0.02760 0.00268 0.00070 -0.00008
O2 5 0.130838 0.258231 0.421436 11.00000 0.03114 0.03426 =
0.02053 -0.00094 0.00777 -0.00846
O3 5 0.040515 0.385508 0.309674 11.00000 0.01537 0.03025 =
0.02990 -0.00440 0.00231 -0.00066
O4 5 0.160419 0.415414 0.166751 11.00000 0.03119 0.01437 =
0.02532 0.00201 0.00369 0.00239
O5 5 0.418519 0.380925 0.201832 11.00000 0.03043 0.02328 =
0.02366 -0.00164 0.01213 -0.00043
O6 5 0.513041 0.260225 0.323174 11.00000 0.01907 0.02704 =
0.03244 -0.00100 0.00458 0.00295
C1 1 0.295180 0.171373 0.477081 11.00000 0.04881 0.02164 =
0.02404 0.00608 -0.00102 -0.01063
AFIX 23
H1A 2 0.335284 0.137661 0.528860 11.00000 -1.20000
H1B 2 0.253174 0.139575 0.423869 11.00000 -1.20000
AFIX 0
C2 1 0.200938 0.220759 0.502714 11.00000 0.04519 0.03425 =
0.02001 0.00257 0.00703 -0.01686
AFIX 23
H2A 2 0.143966 0.190068 0.528818 11.00000 -1.20000
H2B 2 0.243920 0.258275 0.549119 11.00000 -1.20000
AFIX 0
C3 1 0.036747 0.307329 0.437002 11.00000 0.03047 0.04369 =
0.03355 -0.00824 0.01683 -0.01361
AFIX 23
H3A 2 0.076445 0.349515 0.477473 11.00000 -1.20000
H3B 2 -0.019009 0.279439 0.467056 11.00000 -1.20000
AFIX 0
C4 1 -0.038170 0.337420 0.346087 11.00000 0.01814 0.04294 =
0.04151 -0.00990 0.00981 -0.00711
AFIX 23
H4A 2 -0.069536 0.295024 0.303408 11.00000 -1.20000
H4B 2 -0.111661 0.366223 0.353724 11.00000 -1.20000
AFIX 0
C5 1 -0.023577 0.408744 0.218694 11.00000 0.01949 0.02928 =
0.03684 -0.00435 -0.00577 0.00824
AFIX 23
H5A 2 -0.101822 0.436001 0.219186 11.00000 -1.20000
H5B 2 -0.046932 0.363798 0.178819 11.00000 -1.20000
AFIX 0
C6 1 0.059998 0.459253 0.181951 11.00000 0.03244 0.01955 =
0.03534 0.00023 -0.00370 0.00966
AFIX 23
H6A 2 0.011392 0.482592 0.123790 11.00000 -1.20000
H6B 2 0.093913 0.500149 0.226324 11.00000 -1.20000
AFIX 0
C7 1 0.243388 0.458365 0.128670 11.00000 0.04243 0.01947 =
0.02207 0.00341 0.00066 -0.00561
AFIX 23
H7A 2 0.280909 0.500177 0.170575 11.00000 -1.20000
H7B 2 0.196183 0.480440 0.069324 11.00000 -1.20000
AFIX 0
C8 1 0.344559 0.407610 0.114993 11.00000 0.04552 0.02569 =
0.02024 -0.00014 0.01100 -0.01071
AFIX 23
H8A 2 0.306556 0.364239 0.076000 11.00000 -1.20000
H8B 2 0.398813 0.435498 0.083665 11.00000 -1.20000
AFIX 0
C9 1 0.516293 0.331020 0.191936 11.00000 0.04229 0.02724 =
0.04541 -0.00526 0.03044 -0.00102
AFIX 23
H9A 2 0.571659 0.357509 0.160307 11.00000 -1.20000
H9B 2 0.478831 0.286740 0.154487 11.00000 -1.20000
AFIX 0
C10 1 0.591644 0.305440 0.284426 11.00000 0.02137 0.02823 =
0.05606 -0.00607 0.01658 0.00090
AFIX 23
H10A 2 0.665380 0.275752 0.278935 11.00000 -1.20000
H10B 2 0.622480 0.349713 0.324071 11.00000 -1.20000
AFIX 0
C11 1 0.577818 0.228802 0.409453 11.00000 0.02581 0.02637 =
0.03667 -0.00476 -0.00452 0.01166
AFIX 23
H11A 2 0.604034 0.269444 0.455557 11.00000 -1.20000
H11B 2 0.654113 0.201621 0.404314 11.00000 -1.20000
AFIX 0
C12 1 0.490586 0.175532 0.437836 11.00000 0.03948 0.01788 =
0.03277 0.00057 -0.00482 0.00901
AFIX 23
H12A 2 0.457940 0.137857 0.388901 11.00000 -1.20000
H12B 2 0.535924 0.148289 0.494122 11.00000 -1.20000
AFIX 0
HKLF 4
REM zy-241018-2-100k_auto_a.res in P2(1)/n
REM wR2 = 0.0885, GooF = S = 1.079, Restrained GooF = 1.079 for all data
REM R1 = 0.0318 for 5091 Fo > 4sig(Fo) and 0.0343 for all 5514 data
REM 339 parameters refined using 0 restraints
END
WGHT 0.0508 1.4365
REM Highest difference peak 0.657, deepest hole -0.774, 1-sigma level 0.065
Q1 1 0.2360 0.7435 0.2756 11.00000 0.05 0.66
Q2 1 0.2016 0.6791 0.2846 11.00000 0.05 0.64
Q3 1 0.4410 0.7454 0.3871 11.00000 0.05 0.63
Q4 1 0.0508 0.5401 0.5200 11.00000 0.05 0.51
Q5 1 0.9202 0.0409 0.4205 11.00000 0.05 0.39
;
_shelx_res_checksum 8900
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.33717(2) 0.74297(2) 0.33184(2) 0.02722(8) Uani d 1 . .
N N1 0.30875(15) 0.35405(9) 0.35184(11) 0.0162(3) Uani d 1 . .
H H1C 0.333(2) 0.3602(12) 0.3046(16) 0.017(5) Uiso d 1 . .
H H1D 0.230(2) 0.3652(13) 0.3368(16) 0.026(6) Uiso d 1 . .
H H1E 0.319(2) 0.3097(14) 0.3688(15) 0.019(6) Uiso d 1 . .
C C13 0.38090(17) 0.40352(10) 0.42865(12) 0.0193(4) Uani d 1 . .
H H13A 0.470927 0.388931 0.445248 0.023 Uiso calc 1 . .
H H13B 0.349015 0.395539 0.483047 0.023 Uiso calc 1 . .
C C14 0.36888(16) 0.48584(10) 0.40265(12) 0.0178(4) Uani d 1 . .
C C15 0.27719(17) 0.52998(10) 0.42512(14) 0.0220(4) Uani d 1 . .
H H15 0.221622 0.507739 0.455919 0.026 Uiso calc 1 . .
C C16 0.26614(17) 0.60629(11) 0.40293(14) 0.0232(4) Uani d 1 . .
H H16 0.203343 0.636355 0.418212 0.028 Uiso calc 1 . .
C C17 0.34797(17) 0.63788(10) 0.35823(13) 0.0198(4) Uani d 1 . .
C C18 0.44072(18) 0.59538(10) 0.33543(13) 0.0209(4) Uani d 1 . .
H H18 0.496335 0.617875 0.304857 0.025 Uiso calc 1 . .
C C19 0.45055(17) 0.51918(10) 0.35826(12) 0.0198(4) Uani d 1 . .
H H19 0.513926 0.489367 0.343374 0.024 Uiso calc 1 . .
S S1 0.81737(4) 0.03456(2) 0.36150(3) 0.01746(11) Uani d 1 . .
S S2 0.72655(4) 0.09140(3) 0.18660(3) 0.02230(12) Uani d 1 . .
O O7 0.78432(13) 0.16355(8) 0.21723(10) 0.0290(3) Uani d 1 . .
O O8 0.72902(14) 0.06860(10) 0.09568(10) 0.0359(4) Uani d 1 . .
O O9 0.72179(13) 0.07560(8) 0.39135(9) 0.0255(3) Uani d 1 . .
O O10 0.84784(13) -0.03895(7) 0.40284(10) 0.0250(3) Uani d 1 . .
N N2 0.78327(15) 0.02282(9) 0.25322(11) 0.0207(3) Uani d 1 . .
C C20 0.95686(19) 0.08881(12) 0.39168(14) 0.0284(4) Uani d 1 . .
H H20A 0.987827 0.091793 0.458557 0.043 Uiso calc 1 . .
H H20B 0.939317 0.139835 0.366298 0.043 Uiso calc 1 . .
H H20C 1.020890 0.064913 0.366952 0.043 Uiso calc 1 . .
C C21 0.56579(18) 0.09984(13) 0.18424(14) 0.0291(4) Uani d 1 . .
H H21A 0.558941 0.111936 0.245789 0.044 Uiso calc 1 . .
H H21B 0.522485 0.051996 0.163815 0.044 Uiso calc 1 . .
H H21C 0.526886 0.140258 0.141793 0.044 Uiso calc 1 . .
O O1 0.38863(13) 0.21798(7) 0.45447(10) 0.0268(3) Uani d 1 . .
O O2 0.13084(14) 0.25823(8) 0.42144(10) 0.0285(3) Uani d 1 . .
O O3 0.04051(12) 0.38551(8) 0.30967(10) 0.0259(3) Uani d 1 . .
O O4 0.16042(13) 0.41541(7) 0.16675(9) 0.0244(3) Uani d 1 . .
O O5 0.41852(13) 0.38093(7) 0.20183(9) 0.0249(3) Uani d 1 . .
O O6 0.51304(13) 0.26023(8) 0.32317(10) 0.0266(3) Uani d 1 . .
C C1 0.2952(2) 0.17137(12) 0.47708(14) 0.0336(5) Uani d 1 . .
H H1A 0.335284 0.137661 0.528860 0.040 Uiso calc 1 . .
H H1B 0.253174 0.139575 0.423869 0.040 Uiso calc 1 . .
C C2 0.2009(2) 0.22076(13) 0.50271(14) 0.0335(5) Uani d 1 . .
H H2A 0.143966 0.190068 0.528818 0.040 Uiso calc 1 . .
H H2B 0.243920 0.258275 0.549119 0.040 Uiso calc 1 . .
C C3 0.0367(2) 0.30733(14) 0.43700(15) 0.0343(5) Uani d 1 . .
H H3A 0.076445 0.349515 0.477473 0.041 Uiso calc 1 . .
H H3B -0.019009 0.279439 0.467056 0.041 Uiso calc 1 . .
C C4 -0.03817(19) 0.33742(13) 0.34609(16) 0.0339(5) Uani d 1 . .
H H4A -0.069536 0.295024 0.303408 0.041 Uiso calc 1 . .
H H4B -0.111661 0.366223 0.353724 0.041 Uiso calc 1 . .
C C5 -0.02358(19) 0.40874(12) 0.21869(15) 0.0311(5) Uani d 1 . .
H H5A -0.101822 0.436001 0.219186 0.037 Uiso calc 1 . .
H H5B -0.046932 0.363798 0.178819 0.037 Uiso calc 1 . .
C C6 0.0600(2) 0.45925(11) 0.18195(15) 0.0316(5) Uani d 1 . .
H H6A 0.011392 0.482592 0.123790 0.038 Uiso calc 1 . .
H H6B 0.093913 0.500149 0.226324 0.038 Uiso calc 1 . .
C C7 0.2434(2) 0.45837(11) 0.12867(14) 0.0296(5) Uani d 1 . .
H H7A 0.280909 0.500177 0.170575 0.035 Uiso calc 1 . .
H H7B 0.196183 0.480440 0.069324 0.035 Uiso calc 1 . .
C C8 0.3446(2) 0.40761(12) 0.11499(14) 0.0301(5) Uani d 1 . .
H H8A 0.306556 0.364239 0.076000 0.036 Uiso calc 1 . .
H H8B 0.398813 0.435498 0.083665 0.036 Uiso calc 1 . .
C C9 0.5163(2) 0.33102(12) 0.19194(17) 0.0347(5) Uani d 1 . .
H H9A 0.571659 0.357509 0.160307 0.042 Uiso calc 1 . .
H H9B 0.478831 0.286740 0.154487 0.042 Uiso calc 1 . .
C C10 0.5916(2) 0.30544(12) 0.28443(17) 0.0340(5) Uani d 1 . .
H H10A 0.665380 0.275752 0.278935 0.041 Uiso calc 1 . .
H H10B 0.622480 0.349713 0.324071 0.041 Uiso calc 1 . .
C C11 0.5778(2) 0.22880(12) 0.40945(16) 0.0321(5) Uani d 1 . .
H H11A 0.604034 0.269444 0.455557 0.039 Uiso calc 1 . .
H H11B 0.654113 0.201621 0.404314 0.039 Uiso calc 1 . .
C C12 0.4906(2) 0.17553(11) 0.43784(15) 0.0329(5) Uani d 1 . .
H H12A 0.457940 0.137857 0.388901 0.039 Uiso calc 1 . .
H H12B 0.535924 0.148289 0.494122 0.039 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.03376(14) 0.01420(12) 0.02924(13) 0.00154(7) 0.00087(10) 0.00379(7)
N1 0.0165(8) 0.0131(8) 0.0180(8) -0.0005(6) 0.0030(6) 0.0001(6)
C13 0.0200(9) 0.0147(8) 0.0198(9) -0.0013(7) -0.0005(7) -0.0007(7)
C14 0.0166(8) 0.0150(8) 0.0181(8) -0.0010(7) -0.0016(7) -0.0016(7)
C15 0.0170(9) 0.0197(9) 0.0293(10) -0.0027(7) 0.0063(7) -0.0001(8)
C16 0.0167(9) 0.0189(9) 0.0324(10) 0.0032(7) 0.0039(8) -0.0015(8)
C17 0.0192(9) 0.0135(8) 0.0217(9) -0.0004(7) -0.0030(7) 0.0011(7)
C18 0.0222(9) 0.0191(9) 0.0204(9) -0.0039(7) 0.0039(7) -0.0015(7)
C19 0.0182(9) 0.0183(9) 0.0222(9) 0.0009(7) 0.0042(7) -0.0034(7)
S1 0.0154(2) 0.0165(2) 0.0186(2) 0.00016(16) 0.00139(16) 0.00089(16)
S2 0.0170(2) 0.0305(3) 0.0188(2) 0.00524(18) 0.00369(17) 0.00411(18)
O7 0.0263(7) 0.0256(7) 0.0345(8) 0.0020(6) 0.0072(6) 0.0094(6)
O8 0.0308(8) 0.0569(10) 0.0196(7) 0.0099(7) 0.0059(6) 0.0018(7)
O9 0.0254(7) 0.0281(7) 0.0236(7) 0.0070(6) 0.0079(5) -0.0003(6)
O10 0.0237(7) 0.0188(7) 0.0304(7) 0.0018(5) 0.0037(6) 0.0064(5)
N2 0.0201(8) 0.0207(8) 0.0200(8) 0.0033(6) 0.0032(6) -0.0020(6)
C20 0.0251(10) 0.0298(11) 0.0249(10) -0.0106(8) -0.0024(8) 0.0025(8)
C21 0.0165(9) 0.0408(12) 0.0285(10) 0.0074(8) 0.0033(8) 0.0070(9)
O1 0.0330(8) 0.0155(6) 0.0276(7) -0.0001(6) 0.0007(6) 0.0027(5)
O2 0.0311(8) 0.0343(8) 0.0205(7) -0.0085(6) 0.0078(6) -0.0009(6)
O3 0.0154(6) 0.0303(7) 0.0299(7) -0.0007(5) 0.0023(5) -0.0044(6)
O4 0.0312(8) 0.0144(6) 0.0253(7) 0.0024(5) 0.0037(6) 0.0020(5)
O5 0.0304(7) 0.0233(7) 0.0237(7) -0.0004(6) 0.0121(6) -0.0016(5)
O6 0.0191(7) 0.0270(7) 0.0324(8) 0.0030(5) 0.0046(6) -0.0010(6)
C1 0.0488(13) 0.0216(10) 0.0240(10) -0.0106(9) -0.0010(9) 0.0061(8)
C2 0.0452(13) 0.0342(11) 0.0200(10) -0.0169(10) 0.0070(9) 0.0026(8)
C3 0.0305(11) 0.0437(13) 0.0335(11) -0.0136(10) 0.0168(9) -0.0082(10)
C4 0.0181(10) 0.0429(13) 0.0415(12) -0.0071(9) 0.0098(9) -0.0099(10)
C5 0.0195(10) 0.0293(11) 0.0368(12) 0.0082(8) -0.0058(8) -0.0044(9)
C6 0.0324(11) 0.0195(10) 0.0353(11) 0.0097(8) -0.0037(9) 0.0002(8)
C7 0.0424(12) 0.0195(9) 0.0221(10) -0.0056(9) 0.0007(9) 0.0034(8)
C8 0.0455(13) 0.0257(10) 0.0202(9) -0.0107(9) 0.0110(9) -0.0001(8)
C9 0.0423(13) 0.0272(11) 0.0454(13) -0.0010(9) 0.0304(11) -0.0053(9)
C10 0.0214(10) 0.0282(11) 0.0561(14) 0.0009(8) 0.0166(10) -0.0061(10)
C11 0.0258(10) 0.0264(10) 0.0367(12) 0.0117(9) -0.0045(9) -0.0048(9)
C12 0.0395(12) 0.0179(9) 0.0328(11) 0.0090(9) -0.0048(9) 0.0006(8)
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'
Br Br -0.6763 1.2805 '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
H1C N1 H1D . . 106(2) ?
H1C N1 H1E . . 110(2) ?
H1D N1 H1E . . 110(2) ?
C13 N1 H1C . . 111.2(15) ?
C13 N1 H1D . . 111.0(15) ?
C13 N1 H1E . . 108.3(15) ?
N1 C13 H13A . . 109.3 ?
N1 C13 H13B . . 109.3 ?
N1 C13 C14 . . 111.73(14) ?
H13A C13 H13B . . 107.9 ?
C14 C13 H13A . . 109.3 ?
C14 C13 H13B . . 109.3 ?
C15 C14 C13 . . 119.85(17) ?
C15 C14 C19 . . 119.22(16) ?
C19 C14 C13 . . 120.91(16) ?
C14 C15 H15 . . 119.7 ?
C16 C15 C14 . . 120.57(18) ?
C16 C15 H15 . . 119.7 ?
C15 C16 H16 . . 120.5 ?
C17 C16 C15 . . 119.02(17) ?
C17 C16 H16 . . 120.5 ?
C16 C17 Br1 . . 119.12(14) ?
C16 C17 C18 . . 121.68(17) ?
C18 C17 Br1 . . 119.16(14) ?
C17 C18 H18 . . 120.7 ?
C17 C18 C19 . . 118.53(18) ?
C19 C18 H18 . . 120.7 ?
C14 C19 H19 . . 119.5 ?
C18 C19 C14 . . 120.97(17) ?
C18 C19 H19 . . 119.5 ?
O9 S1 N2 . . 113.41(8) ?
O9 S1 C20 . . 107.62(10) ?
O10 S1 O9 . . 114.81(8) ?
O10 S1 N2 . . 106.98(8) ?
O10 S1 C20 . . 107.04(9) ?
N2 S1 C20 . . 106.52(9) ?
O7 S2 N2 . . 113.89(8) ?
O7 S2 C21 . . 106.49(10) ?
O8 S2 O7 . . 115.66(10) ?
O8 S2 N2 . . 106.69(9) ?
O8 S2 C21 . . 106.33(10) ?
N2 S2 C21 . . 107.25(9) ?
S2 N2 S1 . . 119.73(10) ?
S1 C20 H20A . . 109.5 ?
S1 C20 H20B . . 109.5 ?
S1 C20 H20C . . 109.5 ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21B . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C12 O1 C1 . . 112.99(16) ?
C3 O2 C2 . . 112.93(17) ?
C4 O3 C5 . . 110.53(15) ?
C6 O4 C7 . . 112.82(16) ?
C8 O5 C9 . . 111.44(16) ?
C10 O6 C11 . . 112.95(17) ?
O1 C1 H1A . . 109.9 ?
O1 C1 H1B . . 109.9 ?
O1 C1 C2 . . 108.83(16) ?
H1A C1 H1B . . 108.3 ?
C2 C1 H1A . . 109.9 ?
C2 C1 H1B . . 109.9 ?
O2 C2 C1 . . 107.50(17) ?
O2 C2 H2A . . 110.2 ?
O2 C2 H2B . . 110.2 ?
C1 C2 H2A . . 110.2 ?
C1 C2 H2B . . 110.2 ?
H2A C2 H2B . . 108.5 ?
O2 C3 H3A . . 110.1 ?
O2 C3 H3B . . 110.1 ?
O2 C3 C4 . . 108.05(17) ?
H3A C3 H3B . . 108.4 ?
C4 C3 H3A . . 110.1 ?
C4 C3 H3B . . 110.1 ?
O3 C4 C3 . . 108.99(16) ?
O3 C4 H4A . . 109.9 ?
O3 C4 H4B . . 109.9 ?
C3 C4 H4A . . 109.9 ?
C3 C4 H4B . . 109.9 ?
H4A C4 H4B . . 108.3 ?
O3 C5 H5A . . 109.7 ?
O3 C5 H5B . . 109.7 ?
O3 C5 C6 . . 109.73(16) ?
H5A C5 H5B . . 108.2 ?
C6 C5 H5A . . 109.7 ?
C6 C5 H5B . . 109.7 ?
O4 C6 C5 . . 108.65(16) ?
O4 C6 H6A . . 110.0 ?
O4 C6 H6B . . 110.0 ?
C5 C6 H6A . . 110.0 ?
C5 C6 H6B . . 110.0 ?
H6A C6 H6B . . 108.3 ?
O4 C7 H7A . . 109.9 ?
O4 C7 H7B . . 109.9 ?
O4 C7 C8 . . 108.75(16) ?
H7A C7 H7B . . 108.3 ?
C8 C7 H7A . . 109.9 ?
C8 C7 H7B . . 109.9 ?
O5 C8 C7 . . 109.48(16) ?
O5 C8 H8A . . 109.8 ?
O5 C8 H8B . . 109.8 ?
C7 C8 H8A . . 109.8 ?
C7 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.2 ?
O5 C9 H9A . . 109.8 ?
O5 C9 H9B . . 109.8 ?
O5 C9 C10 . . 109.39(17) ?
H9A C9 H9B . . 108.2 ?
C10 C9 H9A . . 109.8 ?
C10 C9 H9B . . 109.8 ?
O6 C10 C9 . . 108.22(17) ?
O6 C10 H10A . . 110.1 ?
O6 C10 H10B . . 110.1 ?
C9 C10 H10A . . 110.1 ?
C9 C10 H10B . . 110.1 ?
H10A C10 H10B . . 108.4 ?
O6 C11 H11A . . 110.1 ?
O6 C11 H11B . . 110.1 ?
O6 C11 C12 . . 108.03(17) ?
H11A C11 H11B . . 108.4 ?
C12 C11 H11A . . 110.1 ?
C12 C11 H11B . . 110.1 ?
O1 C12 C11 . . 108.54(16) ?
O1 C12 H12A . . 110.0 ?
O1 C12 H12B . . 110.0 ?
C11 C12 H12A . . 110.0 ?
C11 C12 H12B . . 110.0 ?
H12A C12 H12B . . 108.4 ?
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
Br1 C17 . 1.8988(18) ?
N1 H1C . 0.84(2) ?
N1 H1D . 0.86(3) ?
N1 H1E . 0.82(2) ?
N1 C13 . 1.501(2) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.505(2) ?
C14 C15 . 1.390(3) ?
C14 C19 . 1.392(3) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.389(3) ?
C16 H16 . 0.9500 ?
C16 C17 . 1.384(3) ?
C17 C18 . 1.386(3) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.389(3) ?
C19 H19 . 0.9500 ?
S1 O9 . 1.4490(14) ?
S1 O10 . 1.4434(13) ?
S1 N2 . 1.5957(16) ?
S1 C20 . 1.7650(19) ?
S2 O7 . 1.4461(15) ?
S2 O8 . 1.4435(15) ?
S2 N2 . 1.5944(16) ?
S2 C21 . 1.769(2) ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
O1 C1 . 1.432(3) ?
O1 C12 . 1.430(3) ?
O2 C2 . 1.429(3) ?
O2 C3 . 1.421(3) ?
O3 C4 . 1.428(3) ?
O3 C5 . 1.430(2) ?
O4 C6 . 1.421(2) ?
O4 C7 . 1.426(2) ?
O5 C8 . 1.429(2) ?
O5 C9 . 1.432(2) ?
O6 C10 . 1.418(3) ?
O6 C11 . 1.423(3) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C1 C2 . 1.487(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.500(3) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.495(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.489(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.494(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C11 C12 . 1.490(3) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
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 O5 . 0.84(2) 2.06(2) 2.889(2) 171(2) yes
N1 H1D O3 . 0.86(3) 2.05(3) 2.905(2) 175(2) yes
N1 H1E O1 . 0.82(2) 2.09(3) 2.873(2) 158(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
Br1 C17 C18 C19 . . . . 177.59(13) ?
N1 C13 C14 C15 . . . . 94.6(2) ?
N1 C13 C14 C19 . . . . -87.0(2) ?
C13 C14 C15 C16 . . . . 178.98(17) ?
C13 C14 C19 C18 . . . . -179.06(16) ?
C14 C15 C16 C17 . . . . -0.1(3) ?
C15 C14 C19 C18 . . . . -0.7(3) ?
C15 C16 C17 Br1 . . . . -177.69(14) ?
C15 C16 C17 C18 . . . . -0.2(3) ?
C16 C17 C18 C19 . . . . 0.1(3) ?
C17 C18 C19 C14 . . . . 0.3(3) ?
C19 C14 C15 C16 . . . . 0.6(3) ?
O7 S2 N2 S1 . . . . 40.13(14) ?
O8 S2 N2 S1 . . . . 168.98(11) ?
O9 S1 N2 S2 . . . . 43.89(14) ?
O10 S1 N2 S2 . . . . 171.49(10) ?
C20 S1 N2 S2 . . . . -74.30(13) ?
C21 S2 N2 S1 . . . . -77.42(13) ?
O1 C1 C2 O2 . . . . 69.6(2) ?
O2 C3 C4 O3 . . . . -67.3(2) ?
O3 C5 C6 O4 . . . . 69.5(2) ?
O4 C7 C8 O5 . . . . -64.3(2) ?
O5 C9 C10 O6 . . . . 66.3(2) ?
O6 C11 C12 O1 . . . . -66.1(2) ?
C1 O1 C12 C11 . . . . 176.56(16) ?
C2 O2 C3 C4 . . . . -174.65(16) ?
C3 O2 C2 C1 . . . . 179.84(16) ?
C4 O3 C5 C6 . . . . 179.75(17) ?
C5 O3 C4 C3 . . . . 173.76(17) ?
C6 O4 C7 C8 . . . . -179.76(16) ?
C7 O4 C6 C5 . . . . 178.06(16) ?
C8 O5 C9 C10 . . . . 179.36(16) ?
C9 O5 C8 C7 . . . . 179.28(16) ?
C10 O6 C11 C12 . . . . -173.32(16) ?
C11 O6 C10 C9 . . . . 176.32(17) ?
C12 O1 C1 C2 . . . . 174.02(16) ?
_cod_database_fobs_code 2312785