#------------------------------------------------------------------------------
#$Date: 2025-02-21 05:00:08 +0200 (Fri, 21 Feb 2025) $
#$Revision: 297817 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312761.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_2312761
loop_
_publ_author_name
'Zhang, Yao'
'Wang, Yan Juan'
'Tang, Yuan Yuan'
'Chen, Xiao Gang'
_publ_section_title
;
Two nonlinear optically responsive crown ether inclusion compounds based
on a sulfonimide anion assembly.
;
_journal_coeditor_code EF3063
_journal_issue 3
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229625000294
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C7 H10 N +, C2 H3 F3 N O4 S2 -, C12 H24 O6'
_chemical_formula_moiety 'C7 H10 N +, C2 H3 F3 N O4 S2 -, C12 H24 O6'
_chemical_formula_sum 'C21 H37 F3 N2 O10 S2'
_chemical_formula_weight 598.64
_chemical_name_systematic
'Benzylammonium (methanesulfonyl)(trifluoromethylsulfonyl)azanide--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 105.4332(15)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.23545(13)
_cell_length_b 16.4434(2)
_cell_length_c 10.58330(14)
_cell_measurement_reflns_used 21354
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 72.0660
_cell_measurement_theta_min 2.6660
_cell_volume 1381.50(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
;
SHELXT2018 (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 0.978
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy-R 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 0.0301
_diffrn_reflns_av_unetI/netI 0.0166
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 26683
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 72.243
_diffrn_reflns_theta_min 4.334
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 2.422
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67854
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2024)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.439
_exptl_crystal_description prism
_exptl_crystal_F_000 632
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.685
_refine_diff_density_min -0.475
_refine_ls_abs_structure_details
;
Flack x determined using 2382 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.004(6)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 344
_refine_ls_number_reflns 5223
_refine_ls_number_restraints 29
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0359
_refine_ls_R_factor_gt 0.0356
_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^)+(0.0567P)^2^+0.7608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0974
_refine_ls_wR_factor_ref 0.0977
_reflns_number_gt 5175
_reflns_number_total 5223
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ef3063sup1.cif
_cod_data_source_block 18c6_metfsa_ba_100k_auto
_cod_database_code 2312761
_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 0.643
_shelx_estimated_absorpt_t_max 0.760
_shelx_hkl_file
;
0 -20 0 14.31 1.26
0 -20 -1 39.80 1.97
0 -20 1 38.82 1.95
0 -20 2 15.17 1.18
0 -19 0 -0.21 0.68
0 -19 1 13.86 1.50
0 -19 -1 16.19 1.90
0 -19 2 37.07 2.21
0 -19 -2 32.16 2.64
0 -19 3 46.18 2.26
0 -19 -3 39.91 2.82
0 -19 4 1.79 0.58
0 -18 0 14.89 2.08
0 -18 1 16.64 1.86
0 -18 -1 15.77 2.26
0 -18 2 27.82 2.22
0 -18 -2 22.09 2.60
0 -18 3 107.32 4.12
0 -18 4 66.74 2.90
0 -18 5 140.63 3.98
0 -17 0 0.15 1.08
0 -17 -1 52.97 4.22
0 -17 1 55.94 4.01
0 -17 2 58.09 3.45
0 -17 3 51.07 3.07
0 -17 4 4.97 1.07
0 -17 5 12.31 1.33
0 -17 5 13.20 1.26
0 -17 5 12.93 1.23
0 -17 6 92.80 3.45
0 -17 6 93.84 3.10
0 -16 0 175.44 7.85
0 -16 -1 79.57 4.80
0 -16 -2 250.15 9.05
0 -16 3 100.66 4.19
0 -16 3 101.98 4.21
0 -16 -4 163.17 6.10
0 -16 -4 168.74 7.16
0 -16 -4 165.53 5.89
0 -16 -4 165.14 6.89
0 -16 4 161.71 5.73
0 -16 4 162.21 5.39
0 -16 4 161.79 5.40
0 -16 -5 153.65 6.37
0 -16 -5 148.05 5.38
0 -16 -5 160.94 5.87
0 -16 -5 148.69 5.48
0 -16 5 139.20 5.35
0 -16 -5 157.51 6.44
0 -16 5 147.26 5.02
0 -16 5 145.54 4.85
0 -16 5 157.42 5.02
0 -16 -6 85.10 3.77
0 -16 6 73.44 3.56
0 -16 -6 84.46 3.93
0 -16 -6 85.15 3.72
0 -16 6 74.76 3.11
0 -16 6 76.59 3.10
0 -16 6 74.07 3.02
0 -16 -7 -0.37 0.60
0 -16 7 0.64 0.63
0 -15 0 0.54 0.98
0 -15 1 18.56 2.61
0 -15 -1 17.68 2.50
0 -15 -1 20.45 2.72
0 -15 -2 294.72 10.50
0 -15 -2 293.23 10.15
0 -15 -2 305.51 10.08
0 -15 2 284.57 9.83
0 -15 -3 63.39 4.56
0 -15 -3 67.25 3.89
0 -15 -3 64.93 4.49
0 -15 -3 64.99 4.49
0 -15 3 60.10 3.66
0 -15 3 59.90 3.38
0 -15 3 58.86 3.37
0 -15 -4 144.24 6.73
0 -15 -4 140.78 6.57
0 -15 4 137.25 5.20
0 -15 4 134.13 5.17
0 -15 -4 141.86 6.74
0 -15 -4 149.02 6.06
0 -15 -4 147.05 5.79
0 -15 -5 180.22 6.70
0 -15 -5 169.55 6.30
0 -15 -5 174.46 6.44
0 -15 5 163.53 6.28
0 -15 -5 166.80 7.10
0 -15 5 159.74 5.62
0 -15 5 172.44 5.65
0 -15 5 167.66 5.66
0 -15 6 4.27 1.00
0 -15 6 4.21 0.98
0 -15 6 3.67 1.10
0 -15 -6 4.89 1.50
0 -15 6 3.21 0.92
0 -15 -6 3.51 1.06
0 -15 -6 3.69 1.23
0 -15 -6 3.98 1.29
0 -15 -6 4.51 1.18
0 -15 -7 80.40 3.79
0 -15 7 85.91 3.90
0 -15 -7 83.08 4.15
0 -15 7 86.33 3.26
0 -15 7 84.97 3.25
0 -15 -7 84.65 3.84
0 -15 -7 89.11 4.06
0 -15 -8 15.09 1.43
0 -15 8 12.72 1.35
0 -14 0 355.50 10.76
0 -14 0 362.61 11.43
0 -14 -1 105.96 5.50
0 -14 -1 112.47 5.57
0 -14 1 111.70 5.98
0 -14 1 112.17 5.37
0 -14 -1 111.62 5.81
0 -14 -1 119.34 6.26
0 -14 1 118.79 5.87
0 -14 2 1.65 1.30
0 -14 -2 2.97 1.48
0 -14 -2 1.46 1.17
0 -14 2 2.89 1.03
0 -14 2 1.79 0.87
0 -14 -2 4.18 1.60
0 -14 -2 1.49 1.28
0 -14 -3 102.19 5.86
0 -14 -3 106.43 4.86
0 -14 -3 100.03 5.89
0 -14 -3 111.05 5.87
0 -14 -3 101.71 4.81
0 -14 3 97.56 4.81
0 -14 -3 107.57 5.84
0 -14 3 106.92 4.58
0 -14 3 97.73 4.42
0 -14 3 104.71 5.39
0 -14 4 180.41 6.91
0 -14 4 183.95 6.64
0 -14 -4 190.39 7.06
0 -14 -4 200.12 8.23
0 -14 -4 189.87 7.19
0 -14 -4 190.40 8.08
0 -14 -4 198.09 8.28
0 -14 -4 193.98 8.03
0 -14 -5 78.92 4.54
0 -14 -5 71.33 4.77
0 -14 -5 81.84 4.46
0 -14 -5 80.09 5.02
0 -14 -5 84.27 5.21
0 -14 5 76.44 3.88
0 -14 5 85.98 4.03
0 -14 5 77.43 3.86
0 -14 -6 31.87 2.81
0 -14 -6 31.29 2.74
0 -14 -6 30.91 2.79
0 -14 6 27.65 2.57
0 -14 -6 29.07 3.02
0 -14 6 26.72 2.16
0 -14 6 32.89 2.41
0 -14 6 27.22 2.22
0 -14 -7 53.42 3.38
0 -14 -7 54.96 3.40
0 -14 -7 59.93 3.52
0 -14 7 51.38 3.24
0 -14 -7 52.82 3.63
0 -14 7 49.26 2.58
0 -14 7 50.69 2.69
0 -14 7 52.54 2.75
0 -14 8 0.56 0.69
0 -14 -8 0.71 0.73
0 -14 -8 1.39 0.84
0 -14 -8 1.10 0.78
0 -14 8 1.19 0.58
0 -14 8 1.56 0.60
0 -14 -8 1.53 0.98
0 -14 9 49.35 1.91
0 -13 0 0.57 0.92
0 -13 0 2.17 1.10
0 -13 0 0.69 0.89
0 -13 -1 16.21 2.19
0 -13 -1 16.87 2.21
0 -13 1 17.38 1.83
0 -13 1 16.65 1.76
0 -13 -1 17.51 2.41
0 -13 1 17.24 2.29
0 -13 1 17.91 2.18
0 -13 -1 18.77 2.44
0 -13 -2 16.80 1.98
0 -13 -2 16.15 2.31
0 -13 -2 18.89 2.63
0 -13 -2 15.20 2.25
0 -13 -2 18.79 1.99
0 -13 -2 21.88 2.59
0 -13 2 17.16 1.86
0 -13 2 14.59 2.26
0 -13 2 18.19 1.90
0 -13 -3 192.39 6.98
0 -13 -3 179.10 6.53
0 -13 -3 188.99 8.03
0 -13 -3 182.52 7.78
0 -13 -3 187.70 6.74
0 -13 -3 196.21 7.84
0 -13 3 186.76 6.83
0 -13 -3 182.47 7.69
0 -13 3 186.35 6.34
0 -13 3 185.96 6.31
0 -13 3 190.20 7.42
0 -13 4 220.65 7.33
0 -13 -4 236.45 7.99
0 -13 -4 233.36 8.93
0 -13 4 237.41 8.02
0 -13 -4 244.01 9.14
0 -13 -4 230.71 8.93
0 -13 -4 226.59 7.78
0 -13 -4 249.69 9.21
0 -13 4 222.97 7.14
0 -13 4 223.73 7.19
0 -13 5 8.81 1.68
0 -13 -5 11.01 1.77
0 -13 -5 7.02 1.62
0 -13 -5 8.83 1.91
0 -13 5 8.42 1.50
0 -13 -5 9.35 1.97
0 -13 -5 10.60 1.79
0 -13 -5 7.87 2.02
0 -13 6 326.61 8.87
0 -13 -6 361.85 11.31
0 -13 -6 346.12 11.15
0 -13 -6 360.41 10.38
0 -13 -6 356.54 11.04
0 -13 -6 341.69 10.33
0 -13 6 347.34 9.19
0 -13 6 351.76 9.24
0 -13 7 46.55 2.68
0 -13 -7 49.64 3.46
0 -13 -7 49.88 3.41
0 -13 -7 46.30 3.41
0 -13 -7 52.03 3.54
0 -13 7 47.67 3.33
0 -13 -7 42.09 3.50
0 -13 7 48.77 2.82
0 -13 7 50.71 2.90
0 -13 -8 6.49 1.32
0 -13 -8 8.64 1.45
0 -13 -8 8.63 1.48
0 -13 8 8.16 1.14
0 -13 8 6.25 1.31
0 -13 -8 9.96 1.66
0 -13 8 7.04 1.08
0 -13 8 9.29 1.29
0 -13 9 55.76 2.33
0 -13 -9 56.47 2.82
0 -13 -9 60.93 2.89
0 -13 9 55.02 2.30
0 -13 9 58.00 2.91
0 -13 -9 53.41 2.66
0 -13 9 47.55 2.34
0 -13 9 56.71 2.33
0 -12 0 112.16 5.43
0 -12 0 99.76 4.92
0 -12 0 113.86 5.03
0 -12 0 113.13 5.00
0 -12 -1 28.75 2.75
0 -12 -1 31.14 2.76
0 -12 1 27.84 2.18
0 -12 1 26.67 2.13
0 -12 -1 27.25 2.68
0 -12 1 28.60 2.53
0 -12 1 28.74 2.68
0 -12 -1 29.00 2.25
0 -12 -1 31.92 3.00
0 -12 -2 23.97 2.70
0 -12 2 30.42 2.70
0 -12 -2 26.13 2.30
0 -12 -2 32.98 3.11
0 -12 -2 29.40 2.30
0 -12 -2 30.43 2.85
0 -12 -2 27.03 2.25
0 -12 2 30.07 2.52
0 -12 -2 26.42 2.81
0 -12 2 30.22 2.32
0 -12 2 26.13 2.77
0 -12 2 30.90 2.37
0 -12 -3 103.40 5.50
0 -12 -3 94.10 4.63
0 -12 -3 96.23 4.54
0 -12 -3 88.77 5.17
0 -12 -3 96.94 4.59
0 -12 -3 90.16 5.09
0 -12 3 97.39 4.67
0 -12 -3 85.47 5.01
0 -12 3 89.60 4.11
0 -12 3 88.06 4.11
0 -12 3 97.67 5.07
0 -12 4 180.11 6.44
0 -12 -4 198.49 8.05
0 -12 4 198.61 7.16
0 -12 -4 191.25 7.91
0 -12 -4 194.48 7.97
0 -12 -4 195.31 7.11
0 -12 -4 201.43 7.32
0 -12 -4 190.53 7.94
0 -12 -4 202.42 7.14
0 -12 4 200.36 6.54
0 -12 4 185.86 6.36
0 -12 5 379.84 10.02
0 -12 -5 392.55 12.09
0 -12 5 408.11 11.18
0 -12 -5 386.54 12.14
0 -12 -5 401.23 11.23
0 -12 -5 399.61 12.00
0 -12 -5 376.25 10.86
0 -12 -5 382.39 11.92
0 -12 5 382.16 10.08
0 -12 5 383.01 10.06
0 -12 -6 58.34 4.31
0 -12 -6 63.40 4.10
0 -12 6 61.41 3.94
0 -12 -6 59.56 4.20
0 -12 -6 56.53 3.89
0 -12 -6 56.79 4.00
0 -12 -6 61.86 4.53
0 -12 6 55.12 3.23
0 -12 -7 53.66 3.71
0 -12 -7 51.60 3.63
0 -12 -7 50.38 3.83
0 -12 7 52.42 3.07
0 -12 7 50.77 3.29
0 -12 7 55.65 3.18
0 -12 -8 73.38 4.04
0 -12 -8 60.58 3.67
0 -12 -8 72.65 4.00
0 -12 8 66.56 3.15
0 -12 8 64.51 3.74
0 -12 -8 64.04 4.04
0 -12 8 58.05 3.34
0 -12 8 61.16 3.05
0 -12 9 3.59 0.79
0 -12 9 4.90 0.86
0 -12 -9 3.99 1.01
0 -12 -9 4.68 1.09
0 -12 9 5.00 1.00
0 -12 9 4.49 1.05
0 -12 -9 4.86 1.04
0 -12 -9 4.27 1.08
0 -12 10 39.64 1.75
0 -11 0 0.38 0.83
0 -11 -1 71.33 3.95
0 -11 1 76.22 3.63
0 -11 1 69.42 3.28
0 -11 1 74.96 3.37
0 -11 -1 74.20 4.08
0 -11 -1 73.77 3.42
0 -11 -1 81.18 4.44
0 -11 2 346.26 8.76
0 -11 2 352.51 8.71
0 -11 2 379.87 9.49
0 -11 -2 367.01 10.26
0 -11 2 339.36 10.06
0 -11 -2 349.70 10.08
0 -11 -2 328.30 8.69
0 -11 -2 347.70 8.89
0 -11 -2 341.13 10.49
0 -11 -2 344.76 10.18
0 -11 -2 351.79 9.15
0 -11 -3 322.22 8.91
0 -11 -3 322.90 10.14
0 -11 -3 331.63 9.24
0 -11 -3 333.76 10.34
0 -11 -3 329.46 10.04
0 -11 3 338.10 9.35
0 -11 -3 347.14 10.34
0 -11 3 343.07 8.73
0 -11 3 328.53 8.59
0 -11 3 331.98 9.78
0 -11 4 490.36 11.51
0 -11 4 484.62 11.45
0 -11 4 461.07 11.41
0 -11 -4 500.92 12.32
0 -11 -4 488.96 12.47
0 -11 -4 479.28 13.27
0 -11 -4 488.70 13.36
0 -11 -4 491.39 13.43
0 -11 4 534.76 12.64
0 -11 4 502.09 12.33
0 -11 -4 494.64 13.45
0 -11 5 328.27 8.99
0 -11 5 338.28 9.04
0 -11 5 328.71 8.97
0 -11 -5 344.40 10.16
0 -11 -5 332.91 10.51
0 -11 -5 332.81 10.69
0 -11 -5 319.61 9.78
0 -11 -5 331.20 9.89
0 -11 -5 330.75 10.84
0 -11 5 349.63 10.03
0 -11 -5 313.33 10.51
0 -11 6 259.88 7.72
0 -11 6 267.11 7.85
0 -11 6 244.22 7.44
0 -11 -6 270.71 8.88
0 -11 -6 266.56 9.27
0 -11 -6 250.49 8.61
0 -11 -6 260.18 9.53
0 -11 6 259.43 8.59
0 -11 -6 262.54 9.39
0 -11 7 174.09 5.95
0 -11 -7 184.68 7.14
0 -11 7 174.05 5.99
0 -11 7 162.44 5.64
0 -11 -7 169.69 7.48
0 -11 7 175.64 6.87
0 -11 -7 172.12 6.93
0 -11 -7 166.71 7.14
0 -11 -8 118.93 5.33
0 -11 -8 111.85 5.20
0 -11 -8 113.68 5.22
0 -11 8 103.59 4.20
0 -11 8 108.63 5.05
0 -11 -8 96.96 5.26
0 -11 8 108.65 4.88
0 -11 8 109.09 4.33
0 -11 -9 60.86 3.43
0 -11 -9 61.21 3.38
0 -11 9 59.86 2.78
0 -11 9 60.02 2.78
0 -11 -9 52.34 3.28
0 -11 9 57.69 3.23
0 -11 -9 61.35 3.40
0 -11 9 57.31 3.34
0 -11 -10 -0.06 0.51
0 -11 10 0.18 0.48
0 -11 10 -0.06 0.54
0 -11 10 0.59 0.59
0 -10 0 516.89 11.61
0 -10 0 511.32 11.70
0 -10 0 510.37 12.24
0 -10 0 500.94 11.78
0 -10 0 505.69 10.47
0 -10 1 9.44 1.37
0 -10 1 10.23 1.33
0 -10 -1 9.88 1.65
0 -10 1 11.23 1.46
0 -10 1 7.91 1.40
0 -10 -1 9.11 1.19
0 -10 -1 10.59 1.72
0 -10 1 10.78 1.35
0 -10 -1 10.03 1.48
0 -10 -2 339.42 8.67
0 -10 2 352.95 9.05
0 -10 2 358.06 8.50
0 -10 2 327.70 8.24
0 -10 -3 151.65 6.11
0 -10 3 165.92 5.34
0 -10 -3 158.45 5.71
0 -10 -3 148.83 6.21
0 -10 3 164.40 6.16
0 -10 3 160.44 5.74
0 -10 3 160.13 5.29
0 -10 4 806.71 16.33
0 -10 -4 779.03 18.10
0 -10 -4 831.46 17.42
0 -10 4 860.15 17.61
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-9 1 5 84.85 3.46
-9 1 4 30.51 2.14
-9 1 4 31.84 2.13
-9 1 4 30.06 2.13
-9 1 3 37.61 2.35
-9 1 3 37.11 2.33
-9 1 3 39.98 2.46
-9 1 2 34.76 2.27
9 1 -2 36.63 2.95
9 1 -2 37.27 2.94
-9 1 2 35.44 2.27
-9 1 2 32.39 2.22
-9 1 1 66.87 3.07
9 1 -1 66.79 4.02
9 1 -1 64.37 3.94
-9 1 1 68.48 3.07
9 1 0 41.53 3.13
9 1 0 43.52 3.15
-9 1 0 38.41 2.22
9 1 1 25.73 2.38
9 1 1 25.27 2.33
-9 1 -1 27.16 1.77
9 1 2 52.20 2.98
-9 2 8 4.38 1.06
-9 2 8 4.73 0.73
-9 2 7 36.25 2.74
-9 2 7 39.48 3.21
-9 2 7 39.06 2.04
-9 2 7 38.16 2.03
-9 2 6 58.88 3.63
-9 2 6 62.96 4.24
-9 2 6 72.65 3.02
-9 2 6 73.91 3.01
-9 2 5 100.78 3.79
-9 2 5 100.59 3.74
-9 2 5 99.78 3.73
-9 2 4 35.06 2.27
-9 2 4 33.27 2.19
-9 2 4 34.49 2.21
-9 2 3 40.46 2.41
-9 2 3 42.79 2.45
-9 2 3 41.30 2.45
9 2 -2 6.15 1.42
-9 2 2 6.56 1.12
-9 2 2 5.74 1.11
-9 2 2 5.55 1.11
9 2 -2 7.54 1.54
9 2 -1 75.61 4.22
9 2 -1 78.86 4.25
-9 2 1 75.34 3.22
-9 2 1 71.65 3.18
9 2 0 45.56 3.22
9 2 0 45.30 3.21
-9 2 0 46.37 2.39
9 2 1 30.55 2.56
-9 2 -1 28.52 1.79
9 2 2 0.84 0.84
-9 3 8 7.63 1.27
-9 3 7 55.02 3.33
-9 3 7 57.29 3.76
-9 3 7 55.39 2.39
-9 3 7 54.21 2.37
-9 3 6 13.40 1.79
-9 3 6 11.26 1.85
-9 3 6 12.87 1.25
-9 3 6 12.63 1.26
-9 3 5 30.16 2.61
-9 3 5 30.03 2.92
-9 3 5 37.36 2.14
-9 3 5 35.95 2.13
-9 3 4 14.45 1.49
-9 3 4 15.86 1.53
-9 3 4 16.09 1.52
-9 3 3 20.35 1.70
-9 3 3 18.20 1.62
-9 3 3 18.71 1.66
9 3 -2 5.59 1.35
-9 3 2 5.39 1.01
9 3 -2 5.49 1.37
-9 3 2 3.70 0.92
9 3 -1 0.85 1.06
-9 3 1 1.01 0.67
-9 3 1 0.36 0.61
9 3 -1 1.61 1.11
9 3 0 15.61 1.95
-9 3 0 15.54 1.36
9 3 0 14.38 1.92
9 3 1 74.61 3.78
9 3 1 77.35 3.86
-9 3 -1 75.81 2.82
9 3 2 18.64 1.75
-9 4 8 3.13 0.90
-9 4 7 17.75 1.91
-9 4 7 16.01 1.22
-9 4 6 24.79 2.56
-9 4 6 25.60 2.37
-9 4 6 25.49 1.64
-9 4 6 24.75 1.63
-9 4 5 18.30 2.30
-9 4 5 20.07 2.15
-9 4 5 24.01 1.67
-9 4 5 23.67 1.69
-9 4 4 14.99 1.41
-9 4 4 14.63 1.42
-9 4 3 15.63 1.44
-9 4 3 14.38 1.41
9 4 -3 13.09 1.76
-9 4 2 31.67 1.99
-9 4 2 29.76 1.96
9 4 -2 32.84 2.71
9 4 -2 31.63 2.68
9 4 -1 2.06 1.19
-9 4 1 3.49 0.80
-9 4 1 4.44 0.87
9 4 -1 3.76 1.29
9 4 0 7.22 1.41
9 4 0 7.99 1.51
-9 4 0 7.18 0.95
-9 4 0 6.78 0.95
9 4 1 30.61 2.39
-9 4 -1 26.72 1.59
-9 5 7 7.21 1.22
-9 5 6 20.32 1.38
-9 5 6 20.28 2.23
-9 5 6 19.91 2.08
-9 5 5 9.73 1.05
-9 5 5 9.75 1.09
-9 5 5 8.85 1.62
-9 5 5 9.58 1.52
-9 5 4 23.47 1.64
-9 5 4 24.35 1.67
-9 5 4 23.42 2.21
-9 5 4 25.69 2.46
-9 5 3 2.00 0.72
-9 5 3 3.14 0.79
9 5 -3 3.62 1.11
-9 5 2 48.83 2.36
-9 5 2 51.79 2.43
9 5 -2 50.96 3.20
9 5 -2 51.85 3.26
-9 5 1 24.37 1.58
-9 5 1 23.16 1.57
9 5 -1 24.54 2.28
9 5 -1 24.06 2.27
-9 5 0 11.42 1.06
9 5 0 11.07 1.61
9 5 0 10.55 1.56
9 5 1 111.20 4.35
-9 6 7 15.52 1.65
-9 6 6 37.75 2.63
-9 6 5 45.39 2.98
-9 6 4 0.48 0.51
-9 6 4 -0.28 0.80
-9 6 3 117.98 3.67
9 6 -3 122.26 4.82
9 6 -2 25.24 2.20
9 6 -2 24.77 2.22
9 6 -1 22.42 2.09
9 6 -1 20.24 2.01
9 6 0 54.53 3.06
-9 7 6 12.37 1.51
-9 7 5 6.28 1.19
-9 7 4 8.42 0.98
-9 7 4 8.29 1.33
-9 7 3 6.41 0.85
9 7 -2 62.57 3.24
9 7 -1 8.73 1.36
9 7 0 83.84 3.61
-9 8 5 60.26 3.08
-9 8 4 51.70 2.11
-9 8 4 48.91 2.78
-9 8 3 29.67 1.58
10 -2 -3 56.77 3.01
10 -2 -2 108.74 4.19
-10 -1 4 31.07 1.60
-10 -1 3 51.14 2.07
10 -1 -3 51.66 2.93
10 -1 -2 15.86 1.69
-10 0 4 58.75 2.25
10 0 -4 56.79 3.00
-10 0 3 72.58 2.52
10 0 -3 68.78 3.46
10 0 -2 66.54 3.30
-10 1 4 33.10 1.65
10 1 -4 35.71 2.36
-10 1 3 51.01 2.08
10 1 -3 55.00 3.05
10 1 -2 18.11 1.82
10 2 -2 108.05 4.21
0 0 0 0.00 0.00
TITL 18C6_MeTFSA_BA_100K_auto in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 8.235448 16.443424 10.583299 90.0000 105.4332 90.0000
ZERR 16.00 0.000127 0.000215 0.000140 0.0000 0.0015 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O F S
UNIT 16.00 16.00 16.00 16.00 16.00 16.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 88826
_shelx_res_file
;
TITL 18c6_metfsa_ba_100k_auto_a.res in P2(1)
18c6_metfsa_ba_100k_auto.res
created by SHELXL-2018/3 at 22:12:03 on 06-Feb-2025
REM Old TITL 18C6_MeTFSA_BA_100K_auto in P2(1)
REM SHELXT solution in P2(1): R1 0.098, Rweak 0.035, Alpha 0.002
REM 2.885 for 4 systematic absences, Orientation as input
REM Flack x = 0.050 ( 0.010 ) from 1385 Parsons' quotients
REM Formula found by SHELXT: C4 N1 O7 F6 S1
CELL 1.54184 8.235448 16.443424 10.583299 90 105.4332 90
ZERR 2 0.000127 0.000215 0.00014 0 0.0015 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H F N O S
UNIT 42 74 6 4 20 4
DELU 0.001 0.002 S2 C21
ISOR 0.001 0.001 S2 C21
SIMU 0.001 0.001 2 S2 C21
RIGU 0.001 0.001 S2 C21
DFIX 1.54 0.001 C2 C1
DFIX 1.54 0.001 C6 C5
DFIX 1.54 0.001 C4 C3
DFIX 1.54 0.001 C8 C7
SADI N1 H1c N1 H1e N1 H1d
L.S. 5
PLAN 5
SIZE 0.2 0.16 0.12
TEMP -173
CONF
HTAB N1 O3
HTAB N1 O1
HTAB N1 O5
BOND $H
MORE -1
fmap 2
acta
OMIT -3 0 2
REM
REM
REM
WGHT 0.056700 0.760800
FVAR 0.74513
S1 6 1.084573 0.230838 0.977086 11.00000 0.03381 0.04724 =
0.02599 0.00319 0.00866 -0.00478
S2 6 0.832868 0.212993 1.109096 11.00000 0.02984 0.02200 =
0.02306 0.00190 0.00697 -0.00107
F1 3 0.767937 0.358174 1.001484 11.00000 0.05263 0.03166 =
0.06231 0.01950 0.01915 0.00490
F2 3 0.577201 0.268025 0.923565 11.00000 0.04363 0.06598 =
0.04089 0.00467 -0.00923 0.00524
F3 3 0.602717 0.321350 1.114947 11.00000 0.03942 0.04799 =
0.04666 0.00476 0.01641 0.01294
O7 5 1.148829 0.174148 0.898589 11.00000 0.05171 0.09814 =
0.06044 -0.02788 0.03398 -0.00840
O8 5 1.043037 0.310461 0.924477 11.00000 0.04099 0.06608 =
0.04604 0.03173 0.00477 -0.00736
O9 5 0.722316 0.149723 1.127341 11.00000 0.04605 0.03466 =
0.03496 0.00336 0.01583 -0.00938
O10 5 0.934743 0.251575 1.224820 11.00000 0.04091 0.03347 =
0.02566 -0.00222 0.00265 0.00214
N2 4 0.926427 0.184735 1.007272 11.00000 0.03410 0.02991 =
0.02775 -0.00189 0.00720 -0.00291
C20 1 1.240078 0.243097 1.125324 11.00000 0.03265 0.04801 =
0.03681 0.01242 -0.00101 -0.01131
AFIX 137
H20A 2 1.336274 0.272417 1.109291 11.00000 -1.50000
H20B 2 1.277071 0.189573 1.162799 11.00000 -1.50000
H20C 2 1.193828 0.274153 1.186759 11.00000 -1.50000
AFIX 0
C21 1 0.688718 0.292563 1.033477 11.00000 0.02850 0.03001 =
0.02686 0.00119 0.00694 -0.00087
O1 5 0.688667 0.561858 0.704657 11.00000 0.02310 0.02637 =
0.03222 -0.00326 0.00274 0.00012
O2 5 0.453666 0.454519 0.765024 11.00000 0.03591 0.02874 =
0.01902 -0.00295 0.00917 0.00041
O3 5 0.151595 0.423579 0.571430 11.00000 0.03248 0.02073 =
0.02710 -0.00088 0.01037 -0.00528
O4 5 0.146271 0.446503 0.304046 11.00000 0.03342 0.02601 =
0.02383 0.00063 0.00069 0.00027
O5 5 0.377686 0.555187 0.244463 11.00000 0.04823 0.02998 =
0.01999 0.00027 0.01356 0.00487
O6 5 0.685726 0.581734 0.436212 11.00000 0.03526 0.02948 =
0.03867 0.00204 0.01746 0.00130
C1 1 0.724513 0.516911 0.824475 11.00000 0.03485 0.03079 =
0.02963 -0.00532 -0.00621 0.00545
AFIX 23
H1A 2 0.806065 0.546922 0.894600 11.00000 -1.20000
H1B 2 0.773600 0.463343 0.813018 11.00000 -1.20000
AFIX 0
C2 1 0.557201 0.505670 0.860952 11.00000 0.04247 0.02890 =
0.02013 -0.00408 0.00286 0.00591
AFIX 23
H2A 2 0.577717 0.480569 0.948823 11.00000 -1.20000
H2B 2 0.501804 0.558952 0.862534 11.00000 -1.20000
AFIX 0
C3 1 0.303140 0.433606 0.797479 11.00000 0.04390 0.03519 =
0.02443 0.00292 0.01873 0.00061
AFIX 23
H3A 2 0.237075 0.483133 0.803116 11.00000 -1.20000
H3B 2 0.329223 0.405490 0.883251 11.00000 -1.20000
AFIX 0
C4 1 0.202448 0.377167 0.688869 11.00000 0.04360 0.02718 =
0.03360 0.00687 0.01679 -0.00479
AFIX 23
H4A 2 0.273244 0.330754 0.676507 11.00000 -1.20000
H4B 2 0.102446 0.355575 0.712863 11.00000 -1.20000
AFIX 0
C5 1 0.050029 0.375867 0.466477 11.00000 0.03620 0.02466 =
0.03996 -0.00867 0.01081 -0.01216
AFIX 23
H5A 2 -0.051806 0.356191 0.489899 11.00000 -1.20000
H5B 2 0.114447 0.328107 0.449662 11.00000 -1.20000
AFIX 0
C6 1 -0.000584 0.429841 0.343579 11.00000 0.03392 0.03043 =
0.03796 -0.00948 -0.00255 -0.00284
AFIX 23
H6A 2 -0.084048 0.401355 0.272704 11.00000 -1.20000
H6B 2 -0.051579 0.481123 0.363656 11.00000 -1.20000
AFIX 0
C7 1 0.108365 0.490630 0.183474 11.00000 0.06029 0.02656 =
0.02196 -0.00145 -0.00840 0.00394
AFIX 23
H7A 2 0.054165 0.543086 0.193587 11.00000 -1.20000
H7B 2 0.030015 0.458949 0.113644 11.00000 -1.20000
AFIX 0
C8 1 0.274388 0.505699 0.146916 11.00000 0.06665 0.03104 =
0.01762 -0.00057 0.00785 0.00574
AFIX 23
H8A 2 0.331400 0.453341 0.141289 11.00000 -1.20000
H8B 2 0.251651 0.533033 0.060624 11.00000 -1.20000
AFIX 0
C9 1 0.532320 0.575361 0.212990 11.00000 0.05572 0.05059 =
0.03276 0.01243 0.02662 0.01279
AFIX 23
H9A 2 0.507446 0.604061 0.127753 11.00000 -1.20000
H9B 2 0.595337 0.525067 0.205796 11.00000 -1.20000
AFIX 0
C10 1 0.635276 0.628228 0.317697 11.00000 0.04988 0.03894 =
0.04611 0.01417 0.03110 0.00498
AFIX 23
H10A 2 0.735857 0.647876 0.292412 11.00000 -1.20000
H10B 2 0.568536 0.676013 0.330935 11.00000 -1.20000
AFIX 0
C11 1 0.791726 0.626372 0.541749 11.00000 0.02779 0.02735 =
0.05718 -0.00678 0.02077 -0.00440
AFIX 23
H11A 2 0.732453 0.675518 0.560184 11.00000 -1.20000
H11B 2 0.895359 0.643710 0.518688 11.00000 -1.20000
AFIX 0
C12 1 0.835399 0.572592 0.658895 11.00000 0.02196 0.03321 =
0.05167 -0.01245 0.00782 -0.00059
AFIX 23
H12A 2 0.875287 0.519280 0.635623 11.00000 -1.20000
H12B 2 0.926611 0.597488 0.728510 11.00000 -1.20000
AFIX 0
N1 4 0.365673 0.544992 0.512965 11.00000 0.02420 0.01754 =
0.01802 -0.00100 0.00606 -0.00170
H1C 2 0.458923 0.548476 0.561898 11.00000 0.02366
H1D 2 0.376004 0.547759 0.439631 11.00000 0.02874
H1E 2 0.325276 0.502078 0.527178 11.00000 0.03286
C13 1 0.243629 0.608080 0.530822 11.00000 0.02432 0.01890 =
0.02765 0.00049 0.01089 0.00118
AFIX 23
H13A 2 0.235025 0.606031 0.622306 11.00000 -1.20000
H13B 2 0.131051 0.595535 0.472299 11.00000 -1.20000
AFIX 66
C18 1 0.448779 0.815749 0.573548 11.00000 0.03852 0.02661 =
0.03036 -0.00149 -0.00174 -0.01224
AFIX 43
H18 2 0.521209 0.846953 0.641039 11.00000 -1.20000
AFIX 65
C19 1 0.399632 0.738213 0.600492 11.00000 0.03347 0.02411 =
0.02193 0.00116 0.00410 -0.00276
AFIX 43
H19 2 0.438471 0.716424 0.686398 11.00000 -1.20000
AFIX 65
C14 1 0.293656 0.692558 0.501742 11.00000 0.01931 0.01660 =
0.02143 -0.00134 0.00798 0.00095
C15 1 0.236827 0.724438 0.376047 11.00000 0.03496 0.02008 =
0.02222 -0.00267 0.00321 0.00270
AFIX 43
H15 2 0.164397 0.693234 0.308556 11.00000 -1.20000
AFIX 65
C16 1 0.285973 0.801974 0.349101 11.00000 0.04275 0.02555 =
0.02406 0.00413 0.01109 0.00487
AFIX 43
H16 2 0.247132 0.823762 0.263195 11.00000 -1.20000
AFIX 65
C17 1 0.391949 0.847630 0.447850 11.00000 0.03583 0.02205 =
0.03774 0.00441 0.01314 -0.00374
AFIX 43
H17 2 0.425538 0.900622 0.429434 11.00000 -1.20000
AFIX 0
HKLF 4
REM 18c6_metfsa_ba_100k_auto_a.res in P2(1)
REM wR2 = 0.0977, GooF = S = 1.056, Restrained GooF = 1.070 for all data
REM R1 = 0.0356 for 5175 Fo > 4sig(Fo) and 0.0359 for all 5223 data
REM 344 parameters refined using 29 restraints
END
WGHT 0.0568 0.7608
REM Highest difference peak 0.685, deepest hole -0.475, 1-sigma level 0.051
Q1 1 0.7355 0.2531 1.0578 11.00000 0.05 0.68
Q2 1 0.9894 0.2456 0.9713 11.00000 0.05 0.43
Q3 1 1.3138 0.1962 1.0953 11.00000 0.05 0.31
Q4 1 0.1993 0.4966 0.1520 11.00000 0.05 0.29
Q5 1 1.1534 0.2331 1.2218 11.00000 0.05 0.28
;
_shelx_res_checksum 18275
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
S S1 1.08457(11) 0.23084(6) 0.97709(8) 0.0355(2) Uani d 1 . .
S S2 0.83287(10) 0.21299(5) 1.10910(7) 0.02498(18) Uani d 1 . .
F F1 0.7679(3) 0.35817(14) 1.0015(3) 0.0481(6) Uani d 1 . .
F F2 0.5772(3) 0.26802(19) 0.9236(3) 0.0541(7) Uani d 1 . .
F F3 0.6027(3) 0.32135(15) 1.1149(2) 0.0437(6) Uani d 1 . .
O O7 1.1488(5) 0.1741(3) 0.8986(4) 0.0665(11) Uani d 1 . .
O O8 1.0430(4) 0.3105(2) 0.9245(3) 0.0523(8) Uani d 1 . .
O O9 0.7223(4) 0.14972(17) 1.1273(3) 0.0376(6) Uani d 1 . .
O O10 0.9347(3) 0.25157(16) 1.2248(2) 0.0345(6) Uani d 1 . .
N N2 0.9264(4) 0.18473(19) 1.0073(3) 0.0308(6) Uani d 1 . .
C C20 1.2401(5) 0.2431(3) 1.1253(4) 0.0411(9) Uani d 1 . .
H H20A 1.336274 0.272417 1.109291 0.062 Uiso calc 1 . .
H H20B 1.277071 0.189573 1.162799 0.062 Uiso calc 1 . .
H H20C 1.193828 0.274153 1.186759 0.062 Uiso calc 1 . .
C C21 0.6887(4) 0.2926(2) 1.0335(3) 0.0285(5) Uani d 1 . .
O O1 0.6887(3) 0.56186(15) 0.7047(2) 0.0281(5) Uani d 1 . .
O O2 0.4537(3) 0.45452(15) 0.7650(2) 0.0275(5) Uani d 1 . .
O O3 0.1516(3) 0.42358(14) 0.5714(2) 0.0263(5) Uani d 1 . .
O O4 0.1463(3) 0.44650(15) 0.3040(2) 0.0291(5) Uani d 1 . .
O O5 0.3777(4) 0.55519(16) 0.2445(2) 0.0319(5) Uani d 1 . .
O O6 0.6857(3) 0.58173(16) 0.4362(3) 0.0330(6) Uani d 1 . .
C C1 0.7245(4) 0.5169(2) 0.8245(3) 0.0346(8) Uani d 1 . .
H H1A 0.806065 0.546922 0.894600 0.041 Uiso calc 1 . .
H H1B 0.773600 0.463343 0.813018 0.041 Uiso calc 1 . .
C C2 0.5572(4) 0.5057(2) 0.8610(3) 0.0315(8) Uani d 1 . .
H H2A 0.577717 0.480569 0.948823 0.038 Uiso calc 1 . .
H H2B 0.501804 0.558952 0.862534 0.038 Uiso calc 1 . .
C C3 0.3031(5) 0.4336(2) 0.7975(3) 0.0327(8) Uani d 1 . .
H H3A 0.237075 0.483133 0.803116 0.039 Uiso calc 1 . .
H H3B 0.329223 0.405490 0.883251 0.039 Uiso calc 1 . .
C C4 0.2024(5) 0.3772(2) 0.6889(3) 0.0335(8) Uani d 1 . .
H H4A 0.273244 0.330754 0.676507 0.040 Uiso calc 1 . .
H H4B 0.102446 0.355575 0.712863 0.040 Uiso calc 1 . .
C C5 0.0500(5) 0.3759(2) 0.4665(3) 0.0335(8) Uani d 1 . .
H H5A -0.051806 0.356191 0.489899 0.040 Uiso calc 1 . .
H H5B 0.114447 0.328107 0.449662 0.040 Uiso calc 1 . .
C C6 -0.0006(5) 0.4298(2) 0.3436(3) 0.0364(9) Uani d 1 . .
H H6A -0.084048 0.401355 0.272704 0.044 Uiso calc 1 . .
H H6B -0.051579 0.481123 0.363656 0.044 Uiso calc 1 . .
C C7 0.1084(4) 0.4906(2) 0.1835(3) 0.0400(9) Uani d 1 . .
H H7A 0.054165 0.543086 0.193587 0.048 Uiso calc 1 . .
H H7B 0.030015 0.458949 0.113644 0.048 Uiso calc 1 . .
C C8 0.2744(5) 0.5057(2) 0.1469(3) 0.0391(9) Uani d 1 . .
H H8A 0.331400 0.453341 0.141289 0.047 Uiso calc 1 . .
H H8B 0.251651 0.533033 0.060624 0.047 Uiso calc 1 . .
C C9 0.5323(6) 0.5754(3) 0.2130(4) 0.0435(10) Uani d 1 . .
H H9A 0.507446 0.604061 0.127753 0.052 Uiso calc 1 . .
H H9B 0.595337 0.525067 0.205796 0.052 Uiso calc 1 . .
C C10 0.6353(6) 0.6282(3) 0.3177(4) 0.0415(9) Uani d 1 . .
H H10A 0.735857 0.647876 0.292412 0.050 Uiso calc 1 . .
H H10B 0.568536 0.676013 0.330935 0.050 Uiso calc 1 . .
C C11 0.7917(5) 0.6264(2) 0.5417(4) 0.0356(8) Uani d 1 . .
H H11A 0.732453 0.675518 0.560184 0.043 Uiso calc 1 . .
H H11B 0.895359 0.643710 0.518688 0.043 Uiso calc 1 . .
C C12 0.8354(4) 0.5726(2) 0.6589(4) 0.0360(8) Uani d 1 . .
H H12A 0.875287 0.519280 0.635623 0.043 Uiso calc 1 . .
H H12B 0.926611 0.597488 0.728510 0.043 Uiso calc 1 . .
N N1 0.3657(4) 0.54499(16) 0.5130(3) 0.0198(5) Uani d 1 . .
H H1C 0.459(4) 0.548(3) 0.562(4) 0.024(10) Uiso d 1 . .
H H1D 0.376(5) 0.548(3) 0.440(3) 0.029(11) Uiso d 1 . .
H H1E 0.325(5) 0.502(2) 0.527(4) 0.033(11) Uiso d 1 . .
C C13 0.2436(4) 0.60808(19) 0.5308(3) 0.0229(6) Uani d 1 . .
H H13A 0.235025 0.606031 0.622306 0.027 Uiso calc 1 . .
H H13B 0.131051 0.595535 0.472299 0.027 Uiso calc 1 . .
C C18 0.4488(3) 0.81575(12) 0.57355(18) 0.0339(8) Uani d 1 . .
H H18 0.521209 0.846953 0.641039 0.041 Uiso calc 1 . .
C C19 0.3996(3) 0.73821(12) 0.60049(15) 0.0271(7) Uani d 1 . .
H H19 0.438471 0.716424 0.686398 0.033 Uiso calc 1 . .
C C14 0.2937(3) 0.69256(9) 0.50174(18) 0.0186(6) Uani d 1 . .
C C15 0.2368(3) 0.72444(12) 0.37605(16) 0.0266(7) Uani d 1 . .
H H15 0.164397 0.693234 0.308556 0.032 Uiso calc 1 . .
C C16 0.2860(3) 0.80197(12) 0.34910(15) 0.0304(7) Uani d 1 . .
H H16 0.247132 0.823762 0.263195 0.036 Uiso calc 1 . .
C C17 0.3919(3) 0.84763(10) 0.4479(2) 0.0312(7) Uani d 1 . .
H H17 0.425538 0.900622 0.429434 0.037 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
S1 0.0338(4) 0.0472(6) 0.0260(4) -0.0048(4) 0.0087(3) 0.0032(4)
S2 0.0298(4) 0.0220(3) 0.0231(3) -0.0011(3) 0.0070(3) 0.0019(3)
F1 0.0526(14) 0.0317(12) 0.0623(16) 0.0049(11) 0.0191(12) 0.0195(11)
F2 0.0436(13) 0.0660(17) 0.0409(13) 0.0052(12) -0.0092(10) 0.0047(12)
F3 0.0394(12) 0.0480(14) 0.0467(13) 0.0129(10) 0.0164(10) 0.0048(11)
O7 0.0517(19) 0.098(3) 0.060(2) -0.0084(19) 0.0340(17) -0.028(2)
O8 0.0410(16) 0.066(2) 0.0460(17) -0.0074(14) 0.0048(13) 0.0317(15)
O9 0.0460(16) 0.0347(14) 0.0350(14) -0.0094(12) 0.0158(12) 0.0034(11)
O10 0.0409(14) 0.0335(14) 0.0257(12) 0.0021(11) 0.0027(10) -0.0022(10)
N2 0.0341(16) 0.0299(15) 0.0278(14) -0.0029(12) 0.0072(12) -0.0019(12)
C20 0.0326(18) 0.048(2) 0.0368(19) -0.0113(17) -0.0010(15) 0.0124(18)
C21 0.0285(9) 0.0300(9) 0.0269(9) -0.0009(8) 0.0069(8) 0.0012(8)
O1 0.0231(11) 0.0264(12) 0.0322(12) 0.0001(9) 0.0027(9) -0.0033(10)
O2 0.0359(12) 0.0287(12) 0.0190(10) 0.0004(10) 0.0092(9) -0.0030(9)
O3 0.0325(12) 0.0207(11) 0.0271(11) -0.0053(10) 0.0104(10) -0.0009(9)
O4 0.0334(12) 0.0260(12) 0.0238(11) 0.0003(10) 0.0007(10) 0.0006(9)
O5 0.0482(15) 0.0300(12) 0.0200(11) 0.0049(11) 0.0136(10) 0.0003(9)
O6 0.0353(13) 0.0295(13) 0.0387(14) 0.0013(11) 0.0175(11) 0.0020(11)
C1 0.0349(19) 0.0308(19) 0.0296(17) 0.0055(15) -0.0062(14) -0.0053(14)
C2 0.042(2) 0.0289(18) 0.0201(15) 0.0059(15) 0.0029(14) -0.0041(13)
C3 0.044(2) 0.0352(19) 0.0244(16) 0.0006(16) 0.0187(15) 0.0029(14)
C4 0.044(2) 0.0272(18) 0.0336(19) -0.0048(15) 0.0168(16) 0.0069(14)
C5 0.0362(19) 0.0247(18) 0.040(2) -0.0122(14) 0.0108(16) -0.0087(14)
C6 0.0339(19) 0.0304(19) 0.0380(19) -0.0028(15) -0.0025(16) -0.0095(15)
C7 0.060(3) 0.0266(18) 0.0220(16) 0.0039(17) -0.0084(17) -0.0014(14)
C8 0.067(3) 0.0310(19) 0.0176(15) 0.0057(18) 0.0078(16) -0.0006(14)
C9 0.056(2) 0.051(2) 0.0328(19) 0.013(2) 0.0266(18) 0.0124(18)
C10 0.050(2) 0.039(2) 0.046(2) 0.0050(18) 0.0311(19) 0.0142(17)
C11 0.0278(18) 0.0274(18) 0.057(2) -0.0044(15) 0.0208(17) -0.0068(17)
C12 0.0220(16) 0.0332(19) 0.052(2) -0.0006(14) 0.0078(15) -0.0125(17)
N1 0.0242(14) 0.0175(13) 0.0180(13) -0.0017(11) 0.0061(11) -0.0010(10)
C13 0.0243(16) 0.0189(14) 0.0276(16) 0.0012(12) 0.0109(13) 0.0005(12)
C18 0.039(2) 0.0266(18) 0.0304(18) -0.0122(15) -0.0017(14) -0.0015(14)
C19 0.0335(17) 0.0241(15) 0.0219(14) -0.0028(13) 0.0041(12) 0.0012(13)
C14 0.0193(14) 0.0166(14) 0.0214(14) 0.0010(11) 0.0080(11) -0.0013(11)
C15 0.0350(16) 0.0201(16) 0.0222(14) 0.0027(13) 0.0032(12) -0.0027(12)
C16 0.043(2) 0.0256(17) 0.0241(16) 0.0049(14) 0.0111(14) 0.0041(13)
C17 0.0358(18) 0.0221(16) 0.0377(19) -0.0037(14) 0.0131(15) 0.0044(14)
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
O7 S1 N2 . . 104.5(2) ?
O7 S1 C20 . . 107.3(2) ?
O8 S1 O7 . . 117.1(2) ?
O8 S1 N2 . . 112.73(18) ?
O8 S1 C20 . . 106.6(2) ?
N2 S1 C20 . . 108.26(17) ?
O9 S2 O10 . . 117.09(16) ?
O9 S2 N2 . . 109.11(16) ?
O9 S2 C21 . . 102.72(17) ?
O10 S2 N2 . . 116.04(16) ?
O10 S2 C21 . . 102.95(16) ?
N2 S2 C21 . . 107.37(16) ?
S2 N2 S1 . . 125.0(2) ?
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 ?
F1 C21 S2 . . 112.7(2) ?
F2 C21 S2 . . 112.7(3) ?
F2 C21 F1 . . 106.8(3) ?
F2 C21 F3 . . 107.9(3) ?
F3 C21 S2 . . 111.6(2) ?
F3 C21 F1 . . 104.6(3) ?
C12 O1 C1 . . 111.8(3) ?
C3 O2 C2 . . 111.7(2) ?
C4 O3 C5 . . 111.0(2) ?
C6 O4 C7 . . 111.3(2) ?
C8 O5 C9 . . 111.3(3) ?
C11 O6 C10 . . 112.7(3) ?
O1 C1 H1A . . 110.3 ?
O1 C1 H1B . . 110.3 ?
O1 C1 C2 . . 107.3(3) ?
H1A C1 H1B . . 108.5 ?
C2 C1 H1A . . 110.3 ?
C2 C1 H1B . . 110.3 ?
O2 C2 C1 . . 107.5(3) ?
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 . . 110.2 ?
O2 C3 H3B . . 110.2 ?
O2 C3 C4 . . 107.4(3) ?
H3A C3 H3B . . 108.5 ?
C4 C3 H3A . . 110.2 ?
C4 C3 H3B . . 110.2 ?
O3 C4 C3 . . 107.7(3) ?
O3 C4 H4A . . 110.2 ?
O3 C4 H4B . . 110.2 ?
C3 C4 H4A . . 110.2 ?
C3 C4 H4B . . 110.2 ?
H4A C4 H4B . . 108.5 ?
O3 C5 H5A . . 110.1 ?
O3 C5 H5B . . 110.1 ?
O3 C5 C6 . . 108.1(3) ?
H5A C5 H5B . . 108.4 ?
C6 C5 H5A . . 110.1 ?
C6 C5 H5B . . 110.1 ?
O4 C6 C5 . . 107.6(3) ?
O4 C6 H6A . . 110.2 ?
O4 C6 H6B . . 110.2 ?
C5 C6 H6A . . 110.2 ?
C5 C6 H6B . . 110.2 ?
H6A C6 H6B . . 108.5 ?
O4 C7 H7A . . 110.1 ?
O4 C7 H7B . . 110.1 ?
O4 C7 C8 . . 108.0(3) ?
H7A C7 H7B . . 108.4 ?
C8 C7 H7A . . 110.1 ?
C8 C7 H7B . . 110.1 ?
O5 C8 C7 . . 108.2(3) ?
O5 C8 H8A . . 110.1 ?
O5 C8 H8B . . 110.1 ?
C7 C8 H8A . . 110.1 ?
C7 C8 H8B . . 110.1 ?
H8A C8 H8B . . 108.4 ?
O5 C9 H9A . . 109.9 ?
O5 C9 H9B . . 109.9 ?
O5 C9 C10 . . 109.1(3) ?
H9A C9 H9B . . 108.3 ?
C10 C9 H9A . . 109.9 ?
C10 C9 H9B . . 109.9 ?
O6 C10 C9 . . 108.4(3) ?
O6 C10 H10A . . 110.0 ?
O6 C10 H10B . . 110.0 ?
C9 C10 H10A . . 110.0 ?
C9 C10 H10B . . 110.0 ?
H10A C10 H10B . . 108.4 ?
O6 C11 H11A . . 110.1 ?
O6 C11 H11B . . 110.1 ?
O6 C11 C12 . . 108.0(3) ?
H11A C11 H11B . . 108.4 ?
C12 C11 H11A . . 110.1 ?
C12 C11 H11B . . 110.1 ?
O1 C12 C11 . . 108.5(3) ?
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 ?
H1C N1 H1D . . 107(4) ?
H1C N1 H1E . . 108(4) ?
H1D N1 H1E . . 112(4) ?
C13 N1 H1C . . 115(3) ?
C13 N1 H1D . . 109(3) ?
C13 N1 H1E . . 105(3) ?
N1 C13 H13A . . 109.0 ?
N1 C13 H13B . . 109.0 ?
N1 C13 C14 . . 112.7(2) ?
H13A C13 H13B . . 107.8 ?
C14 C13 H13A . . 109.0 ?
C14 C13 H13B . . 109.0 ?
C19 C18 H18 . . 120.0 ?
C19 C18 C17 . . 120.0 ?
C17 C18 H18 . . 120.0 ?
C18 C19 H19 . . 120.0 ?
C18 C19 C14 . . 120.0 ?
C14 C19 H19 . . 120.0 ?
C19 C14 C13 . . 119.76(17) ?
C15 C14 C13 . . 120.23(17) ?
C15 C14 C19 . . 120.0 ?
C14 C15 H15 . . 120.0 ?
C16 C15 C14 . . 120.0 ?
C16 C15 H15 . . 120.0 ?
C15 C16 H16 . . 120.0 ?
C15 C16 C17 . . 120.0 ?
C17 C16 H16 . . 120.0 ?
C18 C17 H17 . . 120.0 ?
C16 C17 C18 . . 120.0 ?
C16 C17 H17 . . 120.0 ?
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
S1 O7 . 1.440(4) ?
S1 O8 . 1.428(3) ?
S1 N2 . 1.611(3) ?
S1 C20 . 1.753(4) ?
S2 O9 . 1.429(3) ?
S2 O10 . 1.435(3) ?
S2 N2 . 1.553(3) ?
S2 C21 . 1.804(4) ?
F1 C21 . 1.350(4) ?
F2 C21 . 1.338(4) ?
F3 C21 . 1.339(4) ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
O1 C1 . 1.429(4) ?
O1 C12 . 1.427(4) ?
O2 C2 . 1.416(4) ?
O2 C3 . 1.414(4) ?
O3 C4 . 1.423(4) ?
O3 C5 . 1.433(4) ?
O4 C6 . 1.408(5) ?
O4 C7 . 1.428(4) ?
O5 C8 . 1.409(5) ?
O5 C9 . 1.438(5) ?
O6 C10 . 1.433(5) ?
O6 C11 . 1.425(5) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C1 C2 . 1.5378(14) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.5372(14) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.5377(14) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.5369(14) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.484(7) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C11 C12 . 1.487(6) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
N1 H1C . 0.81(3) ?
N1 H1D . 0.80(3) ?
N1 H1E . 0.81(3) ?
N1 C13 . 1.491(4) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.504(3) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.3900 ?
C18 C17 . 1.3900 ?
C19 H19 . 0.9500 ?
C19 C14 . 1.3900 ?
C14 C15 . 1.3900 ?
C15 H15 . 0.9500 ?
C15 C16 . 1.3900 ?
C16 H16 . 0.9500 ?
C16 C17 . 1.3900 ?
C17 H17 . 0.9500 ?
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 . 0.81(3) 2.10(3) 2.898(4) 174(4) yes
N1 H1D O5 . 0.80(3) 2.07(3) 2.874(4) 175(4) yes
N1 H1E O3 . 0.81(3) 2.07(3) 2.839(4) 158(4) 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
O7 S1 N2 S2 . . . . 168.3(3) ?
O8 S1 N2 S2 . . . . -63.5(3) ?
O9 S2 N2 S1 . . . . -168.9(2) ?
O9 S2 C21 F1 . . . . -177.1(3) ?
O9 S2 C21 F2 . . . . -56.1(3) ?
O9 S2 C21 F3 . . . . 65.5(3) ?
O10 S2 N2 S1 . . . . -34.0(3) ?
O10 S2 C21 F1 . . . . 60.9(3) ?
O10 S2 C21 F2 . . . . -178.2(3) ?
O10 S2 C21 F3 . . . . -56.6(3) ?
N2 S2 C21 F1 . . . . -62.1(3) ?
N2 S2 C21 F2 . . . . 58.8(3) ?
N2 S2 C21 F3 . . . . -179.5(2) ?
C20 S1 N2 S2 . . . . 54.1(3) ?
C21 S2 N2 S1 . . . . 80.5(3) ?
O1 C1 C2 O2 . . . . 66.6(3) ?
O2 C3 C4 O3 . . . . -66.7(4) ?
O3 C5 C6 O4 . . . . 67.9(3) ?
O4 C7 C8 O5 . . . . -63.4(4) ?
O5 C9 C10 O6 . . . . 66.3(4) ?
O6 C11 C12 O1 . . . . -71.0(3) ?
C1 O1 C12 C11 . . . . -174.6(3) ?
C2 O2 C3 C4 . . . . -179.0(3) ?
C3 O2 C2 C1 . . . . 173.9(3) ?
C4 O3 C5 C6 . . . . 179.8(3) ?
C5 O3 C4 C3 . . . . -177.4(3) ?
C6 O4 C7 C8 . . . . -179.6(3) ?
C7 O4 C6 C5 . . . . 174.9(3) ?
C8 O5 C9 C10 . . . . 179.3(3) ?
C9 O5 C8 C7 . . . . -177.0(3) ?
C10 O6 C11 C12 . . . . 179.8(3) ?
C11 O6 C10 C9 . . . . 177.5(3) ?
C12 O1 C1 C2 . . . . -177.4(3) ?
N1 C13 C14 C19 . . . . -87.8(3) ?
N1 C13 C14 C15 . . . . 91.0(3) ?
C13 C14 C15 C16 . . . . -178.8(2) ?
C18 C19 C14 C13 . . . . 178.8(2) ?
C18 C19 C14 C15 . . . . 0.0 ?
C19 C18 C17 C16 . . . . 0.0 ?
C19 C14 C15 C16 . . . . 0.0 ?
C14 C15 C16 C17 . . . . 0.0 ?
C15 C16 C17 C18 . . . . 0.0 ?
C17 C18 C19 C14 . . . . 0.0 ?
_cod_database_fobs_code 2312761