#------------------------------------------------------------------------------
#$Date: 2022-09-13 03:48:08 +0200 (Tue, 13 Sep 2022) $
#$Revision: 277787 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022664.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_2022664
loop_
_publ_author_name
'Kayukova, Lyudmila A.'
'Vologzhanina, Anna V.'
'Yergaliyeva, Elmira M.'
'Baitursynova, Gulnur P.'
'Shulgau, Zarina T.'
'Sergazy, Shynggys'
_publ_section_title
;
Crystal structure and antidiabetic activity of 2-aminospiropyrazolinium
tosylates and the product of O-tosylation of
\b-(benzimidazol-1-yl)propioamidoxime
;
_journal_coeditor_code ZO3026
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229622008464
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C7 H14 N3 S +, C7 H7 O3 S -'
_chemical_formula_moiety 'C7 H14 N3 S +, C7 H7 O3 S -'
_chemical_formula_sum 'C14 H21 N3 O3 S2'
_chemical_formula_weight 343.46
_chemical_name_common
;
2-Amino-8-thia-1,5-diazaspiro[4.5]dec-1-en-5-ium tosylate
;
_chemical_name_systematic
;
2-Amino-8-thia-1,5-diazaspiro[4.5]dec-1-en-5-ium 4-methylbenzenesulfonate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 84.881(2)
_cell_angle_beta 79.671(2)
_cell_angle_gamma 84.660(2)
_cell_formula_units_Z 2
_cell_length_a 6.2286(4)
_cell_length_b 8.5209(4)
_cell_length_c 16.2157(7)
_cell_measurement_reflns_used 6761
_cell_measurement_temperature 295
_cell_measurement_theta_max 30.51
_cell_measurement_theta_min 2.41
_cell_volume 840.68(8)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_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
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type 'Bruker D8 Quest PHOTON area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0641
_diffrn_reflns_av_unetI/netI 0.0792
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 13223
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.542
_diffrn_reflns_theta_min 2.407
_exptl_absorpt_coefficient_mu 0.332
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.3894
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.357
_exptl_crystal_description plate
_exptl_crystal_F_000 364
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.695
_refine_diff_density_min -0.568
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 200
_refine_ls_number_reflns 4869
_refine_ls_number_restraints 18
_refine_ls_restrained_S_all 1.108
_refine_ls_R_factor_all 0.1077
_refine_ls_R_factor_gt 0.0965
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+2.0384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2109
_refine_ls_wR_factor_ref 0.2184
_reflns_number_gt 4011
_reflns_number_total 4869
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zo3026sup1.cif
_cod_data_source_block 8
_cod_database_code 2022664
_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 0.925
_shelx_estimated_absorpt_t_max 0.987
_shelx_hkl_file
;
-1 0 0 11.60 1.30
-2 0 0 281.07 26.70
-3 0 0 625.24 60.69
-3 0 0 660.53 60.79
-4 0 0 86.09 8.60
-4 0 0 74.09 8.30
-5 0 0 66.19 7.50
-5 0 0 70.39 7.80
-6 0 0 59.09 7.20
-6 0 0 63.59 7.50
-7 0 0 1.20 1.20
-7 0 0 0.40 1.10
-7 0 0 0.70 1.30
-8 0 0 28.90 6.30
-8 0 0 37.60 6.60
-8 0 0 36.90 5.50
-8 1 0 -0.20 1.40
-7 1 0 3.60 1.70
-7 1 0 3.40 1.70
-6 1 0 25.60 4.10
-6 1 0 26.70 3.90
-5 1 0 52.09 6.00
-5 1 0 51.59 6.20
-4 1 0 38.90 4.50
-4 1 0 34.10 4.20
-3 1 0 375.46 37.90
-3 1 0 427.16 38.30
-2 1 0 966.40 90.89
1 -1 0 9999.00 958.70
0 -1 0 25.70 2.70
0 1 0 31.50 2.70
-1 -1 0 7333.27 715.13
1 1 0 7616.54 715.03
-2 -1 0 4161.28 396.56
2 1 0 3845.32 389.16
-3 -1 0 379.76 37.30
-3 -1 0 421.46 37.40
3 1 0 375.46 37.30
-4 -1 0 560.64 53.29
-4 -1 0 558.84 53.29
-5 -1 0 34.20 4.40
-5 -1 0 33.40 4.30
-5 -1 0 31.10 4.20
-6 -1 0 6.60 2.10
-6 -1 0 6.70 2.00
-6 -1 0 8.60 2.40
-7 -1 0 6.60 2.20
-7 -1 0 4.40 2.00
-7 -1 0 4.30 1.80
-8 -1 0 -0.60 1.50
-8 -1 0 2.40 1.90
-8 -1 0 1.60 1.60
-7 2 0 1.00 1.30
-7 2 0 1.10 1.00
-6 2 0 4.50 1.90
-6 2 0 3.40 1.60
-5 2 0 12.70 2.50
-5 2 0 15.80 3.20
-4 2 0 29.90 3.70
-4 2 0 23.90 3.20
3 -2 0 115.59 11.80
-3 2 0 123.99 11.80
2 -2 0 402.06 40.10
-2 2 0 449.16 40.40
1 -2 0 1685.63 198.48
-1 2 0 1840.02 205.18
-1 -2 0 3240.48 335.87
-2 -2 0 2.90 0.80
-2 -2 0 2.20 0.60
2 2 0 2.20 0.80
2 2 0 2.00 0.60
-3 -2 0 511.55 46.70
-3 -2 0 481.25 46.50
3 2 0 481.95 46.60
-4 -2 0 19.80 2.70
-4 -2 0 16.00 2.50
-5 -2 0 37.80 4.80
-5 -2 0 38.60 4.80
-6 -2 0 -0.10 0.90
-6 -2 0 0.90 1.10
-7 -2 0 6.80 2.20
-7 -2 0 7.30 2.20
-7 -2 0 6.50 2.20
-8 -2 0 6.80 2.60
-8 -2 0 5.90 2.50
-7 3 0 4.20 2.80
-7 3 0 0.80 1.50
-6 3 0 10.00 2.50
-6 3 0 14.60 2.80
-5 3 0 16.20 2.60
-5 3 0 19.30 3.70
4 -3 0 55.69 6.60
-4 3 0 72.99 7.20
-4 3 0 60.49 6.50
3 -3 0 12.60 2.00
-3 3 0 14.40 1.90
2 -3 0 39.40 4.10
-2 3 0 37.00 3.90
-2 3 0 35.70 4.20
1 -3 0 2541.35 297.77
-1 3 0 2862.21 310.67
0 -3 0 32.10 3.50
0 3 0 33.90 3.60
-1 -3 0 238.48 20.90
1 3 0 216.58 20.90
1 3 0 201.48 20.50
-2 -3 0 3078.59 332.67
2 3 0 2893.51 321.07
-3 -3 0 248.38 22.50
-3 -3 0 233.78 22.60
3 3 0 219.78 22.70
3 3 0 234.68 22.50
-4 -3 0 111.69 11.20
-4 -3 0 110.39 11.00
4 3 0 105.19 11.10
-5 -3 0 56.09 6.20
-5 -3 0 51.09 6.20
-6 -3 0 27.90 4.00
-6 -3 0 25.30 4.00
-7 -3 0 1.70 1.40
-7 -3 0 1.00 1.60
-7 -3 0 1.40 1.50
-8 -3 0 0.20 2.10
-8 -3 0 0.40 1.40
-7 4 0 8.60 2.60
-6 4 0 0.30 1.10
-6 4 0 2.70 1.30
5 -4 0 13.90 2.80
-5 4 0 16.00 2.40
-5 4 0 13.70 2.90
4 -4 0 24.40 3.50
-4 4 0 32.70 4.00
-4 4 0 24.90 3.30
3 -4 0 99.69 10.20
-3 4 0 96.69 9.90
-3 4 0 103.99 10.50
2 -4 0 129.99 12.50
-2 4 0 114.19 12.50
-2 4 0 128.99 12.10
1 -4 0 131.19 13.20
-1 4 0 138.99 13.10
0 -4 0 453.35 37.30
0 4 0 396.06 37.30
0 4 0 334.37 37.00
1 4 0 897.21 84.29
1 4 0 903.01 84.79
-2 -4 0 333.67 28.70
-2 -4 0 305.47 29.10
2 4 0 299.57 29.30
2 4 0 278.07 28.80
-3 -4 0 22.80 3.10
-3 -4 0 27.40 2.80
3 4 0 24.90 3.20
3 4 0 23.90 2.90
-4 -4 0 42.40 4.90
-4 -4 0 46.40 4.70
4 4 0 43.90 4.90
4 4 0 35.40 4.90
-5 -4 0 11.90 2.70
-5 -4 0 13.30 2.40
-6 -4 0 33.40 4.60
-6 -4 0 34.40 4.50
-7 -4 0 -0.30 1.00
-7 -4 0 -0.20 1.00
-8 -4 0 1.40 1.40
-6 5 0 2.60 1.30
-6 5 0 1.00 1.60
5 -5 0 40.30 5.50
-5 5 0 45.10 5.90
-5 5 0 47.80 5.20
4 -5 0 3.20 1.40
-4 5 0 3.00 1.20
3 -5 0 0.00 0.90
-3 5 0 -0.10 0.80
-3 5 0 2.80 1.00
2 -5 0 10.30 2.20
-2 5 0 7.60 1.70
-2 5 0 11.60 1.70
-2 5 0 6.60 1.70
1 -5 0 1239.88 120.59
-1 5 0 1326.57 120.49
0 -5 0 867.71 71.89
0 5 0 739.83 71.79
0 5 0 680.33 71.39
-1 -5 0 229.08 19.40
1 5 0 187.98 18.90
1 5 0 184.48 19.50
-2 -5 0 381.76 34.80
2 5 0 345.57 35.00
-3 -5 0 0.80 0.40
-3 -5 0 0.40 0.70
3 5 0 0.20 0.40
3 5 0 -0.30 0.50
-4 -5 0 20.90 3.00
-4 -5 0 22.70 2.50
4 5 0 20.30 2.90
4 5 0 18.60 3.10
-5 -5 0 33.20 4.50
-5 -5 0 36.10 4.10
-6 -5 0 -0.90 0.50
-6 -5 0 0.30 1.00
-7 -5 0 2.80 1.50
-7 -5 0 4.30 2.00
-8 -5 0 3.40 1.60
-6 6 0 0.30 1.00
-6 6 0 4.20 1.80
-6 6 0 3.50 1.40
5 -6 0 6.70 2.10
-5 6 0 6.20 1.90
-5 6 0 9.30 2.50
-5 6 0 10.30 2.10
4 -6 0 49.80 6.40
-4 6 0 55.59 5.80
-4 6 0 46.60 6.40
-4 6 0 57.39 6.50
3 -6 0 49.50 6.30
-3 6 0 51.89 5.70
-3 6 0 56.69 6.20
-3 6 0 52.69 6.30
2 -6 0 638.74 58.69
-2 6 0 701.13 58.29
-2 6 0 518.05 58.59
-2 6 0 602.64 58.39
1 -6 0 34.80 4.10
-1 6 0 25.90 3.50
-1 6 0 36.60 3.90
0 -6 0 13.60 2.30
-1 -6 0 946.21 77.39
1 6 0 766.22 76.79
1 6 0 747.23 77.49
-2 -6 0 2.40 0.50
-2 -6 0 6.00 1.40
2 6 0 2.00 0.60
2 6 0 2.90 1.20
-3 -6 0 64.69 7.00
3 6 0 59.49 7.30
3 6 0 67.79 6.60
-4 -6 0 191.58 18.70
-4 -6 0 195.08 17.90
4 6 0 172.38 18.90
-5 -6 0 30.90 4.00
-5 -6 0 30.30 3.30
5 6 0 23.70 4.00
-6 -6 0 7.80 2.10
-6 -6 0 5.50 1.40
-7 -6 0 -0.40 0.90
-7 -6 0 0.80 1.40
-6 7 0 -0.70 1.90
-6 7 0 1.70 1.60
-5 7 0 2.10 1.70
-5 7 0 2.30 1.50
-5 7 0 5.10 1.90
4 -7 0 30.50 4.60
-4 7 0 34.40 4.70
-4 7 0 31.10 3.90
-4 7 0 28.50 4.50
3 -7 0 3.40 1.60
-3 7 0 3.80 1.50
-3 7 0 3.70 1.40
-3 7 0 4.60 1.60
2 -7 0 9.70 2.40
-2 7 0 12.30 2.60
-2 7 0 5.70 1.60
-2 7 0 10.00 2.00
1 -7 0 203.68 19.20
-1 7 0 205.98 19.00
-1 7 0 187.18 18.60
-1 7 0 174.28 19.00
0 -7 0 703.43 63.99
0 7 0 707.53 63.39
0 7 0 609.34 63.99
1 7 0 74.59 7.20
1 7 0 70.89 8.10
2 7 0 128.89 13.30
2 7 0 156.18 14.60
-3 -7 0 5.50 0.90
-3 -7 0 6.90 1.80
3 7 0 7.00 1.10
3 7 0 3.80 1.70
-4 -7 0 11.50 1.40
-4 -7 0 8.90 2.20
4 7 0 7.90 2.30
-5 -7 0 14.80 3.00
-5 -7 0 18.30 2.10
5 7 0 17.70 3.70
-6 -7 0 1.90 2.60
-6 -7 0 3.00 0.90
-7 -7 0 2.80 1.10
5 -8 0 0.20 1.70
-5 8 0 -1.00 1.50
-5 8 0 0.40 1.30
-5 8 0 -0.10 1.20
4 -8 0 7.20 2.40
-4 8 0 6.20 2.00
-4 8 0 16.50 3.10
-4 8 0 10.10 2.10
3 -8 0 8.30 2.40
-3 8 0 7.60 1.90
-3 8 0 11.50 2.50
-3 8 0 8.40 2.50
2 -8 0 77.49 8.70
-2 8 0 73.29 8.60
-2 8 0 74.79 8.00
-2 8 0 77.99 8.20
1 -8 0 63.99 7.30
-1 8 0 59.59 7.10
-1 8 0 61.09 6.50
-1 8 0 66.09 7.10
0 -8 0 39.00 5.10
0 8 0 38.90 4.80
0 8 0 40.10 5.10
0 8 0 42.10 4.30
-1 -8 0 89.79 8.40
1 8 0 69.89 7.40
1 8 0 68.99 8.40
-2 -8 0 8.30 2.10
2 8 0 6.30 2.20
-3 -8 0 30.10 4.20
3 8 0 30.10 4.50
-4 -8 0 69.69 7.50
4 8 0 62.59 8.00
-5 -8 0 28.30 4.00
5 8 0 23.40 4.60
-6 -8 0 16.30 1.90
-6 -8 0 11.80 3.00
-7 -8 0 0.50 0.80
-5 9 0 2.50 1.70
4 -9 0 8.20 2.40
-4 9 0 15.30 3.00
-4 9 0 7.30 2.20
-4 9 0 4.50 2.00
3 -9 0 6.30 3.20
-3 9 0 6.50 1.70
-3 9 0 1.40 1.40
-3 9 0 5.10 2.10
2 -9 0 1.10 1.10
-2 9 0 0.20 1.20
-2 9 0 -0.10 0.70
-2 9 0 -1.50 0.90
1 -9 0 13.20 2.80
-1 9 0 9.10 1.60
-1 9 0 7.30 2.10
-1 9 0 9.90 2.30
0 -9 0 130.19 13.40
0 9 0 119.59 13.10
0 9 0 123.19 13.50
0 9 0 139.39 12.70
-1 -9 0 0.50 1.30
1 9 0 0.30 1.10
-2 -9 0 39.40 4.70
2 9 0 26.20 4.60
-3 -9 0 29.30 4.30
3 9 0 29.90 4.60
-4 -9 0 5.40 2.00
4 9 0 5.00 2.30
-5 -9 0 3.30 2.00
5 9 0 1.40 1.80
-4 10 0 3.30 1.50
-4 10 0 0.00 1.60
-3 10 0 1.90 1.60
-3 10 0 5.70 1.50
2 -10 0 22.60 3.70
-2 10 0 23.20 4.40
-2 10 0 23.60 3.00
-2 10 0 20.60 3.50
1 -10 0 14.70 3.90
-1 10 0 11.20 1.90
-1 10 0 12.70 2.80
-1 10 0 13.80 3.10
0 -10 0 8.00 2.40
0 10 0 9.30 1.60
0 10 0 6.50 2.20
0 10 0 7.80 2.00
-1 -10 0 3.90 1.80
1 10 0 3.30 0.90
1 10 0 3.20 1.80
1 10 0 3.20 0.70
-2 -10 0 0.30 1.50
2 10 0 1.40 1.30
-3 -10 0 -1.90 1.30
3 10 0 1.40 1.60
-4 -10 0 25.90 4.30
4 10 0 20.60 4.50
-3 11 0 10.20 2.00
-3 11 0 5.20 2.60
-2 11 0 7.60 1.60
-2 11 0 5.30 2.20
-1 11 0 -0.20 0.80
-1 11 0 1.30 1.70
0 -11 0 9.70 2.40
0 11 0 6.10 1.60
0 11 0 4.90 1.20
0 11 0 6.00 2.30
-1 -11 0 10.90 2.80
1 11 0 16.00 3.50
2 11 0 -0.30 1.30
0 12 0 2.60 1.00
0 12 0 3.20 1.20
2 11 -1 6.10 2.60
1 11 -1 8.50 3.00
-1 -11 1 7.20 2.40
0 11 -1 13.50 3.30
0 11 -1 16.20 2.00
0 11 -1 13.80 2.10
0 -11 1 18.70 3.60
-1 11 -1 5.30 1.80
-1 11 -1 5.90 1.30
-2 11 -1 2.70 1.10
-2 11 -1 4.00 1.90
-3 11 -1 7.10 1.70
-3 11 -1 5.00 2.80
4 10 -1 11.10 3.20
-4 -10 1 9.20 2.90
3 10 -1 20.00 5.00
-3 -10 1 25.80 4.00
2 10 -1 23.90 4.60
-2 -10 1 24.70 3.90
1 10 -1 -1.40 1.10
-1 -10 1 -0.40 1.20
0 10 -1 3.70 1.80
0 10 -1 2.10 1.00
0 10 -1 2.80 0.80
0 -10 1 2.20 1.60
-1 10 -1 3.50 1.50
-1 10 -1 2.10 1.40
-1 10 -1 2.10 0.90
1 -10 1 3.00 1.90
-2 10 -1 1.80 1.60
-2 10 -1 -0.10 1.20
-2 10 -1 0.30 0.80
2 -10 1 3.60 1.70
-3 10 -1 8.20 2.50
-3 10 -1 9.70 2.00
-3 10 -1 8.60 3.10
-4 10 -1 11.10 3.90
-4 10 -1 4.00 2.10
5 9 -1 27.60 4.90
-5 -9 1 32.50 4.70
4 9 -1 10.30 2.90
-4 -9 1 9.20 2.50
3 9 -1 2.00 1.40
-3 -9 1 2.00 1.60
2 9 -1 38.10 5.60
-2 -9 1 43.90 5.30
1 9 -1 -0.10 1.00
-1 -9 1 -0.30 1.30
0 9 -1 95.39 10.20
0 9 -1 98.59 9.60
0 9 -1 95.89 10.70
0 -9 1 101.79 10.60
-1 9 -1 5.20 1.20
-1 9 -1 4.00 1.70
-1 9 -1 5.70 1.80
1 -9 1 6.20 2.10
-2 9 -1 47.10 5.20
-2 9 -1 48.70 6.10
-2 9 -1 41.70 5.40
2 -9 1 47.70 6.00
-3 9 -1 3.90 1.30
-3 9 -1 3.20 1.60
-3 9 -1 3.30 1.60
3 -9 1 8.80 3.40
-4 9 -1 -1.10 1.30
-4 9 -1 -0.40 1.20
-4 9 -1 1.80 1.10
4 -9 1 2.90 1.80
-5 9 -1 7.80 2.40
-5 9 -1 3.00 2.60
-6 -8 1 1.40 1.60
5 8 -1 16.80 3.80
-5 -8 1 19.80 3.50
4 8 -1 15.60 3.40
-4 -8 1 18.10 3.00
3 8 -1 125.09 15.00
-3 -8 1 160.38 14.70
2 8 -1 19.00 3.80
-2 -8 1 21.50 3.40
1 8 -1 153.58 14.40
1 8 -1 138.09 14.20
1 8 -1 162.38 15.60
0 8 -1 9.30 2.40
0 8 -1 8.00 1.30
0 8 -1 5.30 1.60
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0 -4 19 26.70 4.10
-1 4 -19 2.50 1.10
1 -4 19 3.50 1.40
-2 4 -19 6.90 1.70
2 -4 19 4.50 1.70
-3 4 -19 8.50 1.70
-3 4 -19 7.50 1.70
3 -4 19 5.10 2.00
-4 4 -19 4.00 1.20
-4 4 -19 3.00 1.30
-4 4 -19 3.80 1.60
4 -4 19 2.10 1.50
-3 -3 19 0.30 1.00
-2 -3 19 3.90 1.40
1 3 -19 3.00 1.20
-1 -3 19 0.60 1.10
0 3 -19 13.80 2.50
0 -3 19 11.70 2.60
-1 3 -19 20.40 2.70
1 -3 19 12.10 2.90
-2 3 -19 19.70 2.80
2 -3 19 15.90 3.40
-3 3 -19 7.00 0.80
-3 3 -19 5.10 0.80
-3 3 -19 4.20 1.40
3 -3 19 7.20 2.20
-4 3 -19 3.50 1.00
-4 3 -19 2.90 1.10
-4 3 -19 8.50 2.20
4 -3 19 2.30 1.80
-5 3 -19 0.70 1.20
-5 3 -19 -0.70 0.90
-3 -2 19 12.70 2.60
2 2 -19 2.10 1.00
-2 -2 19 0.40 1.00
1 2 -19 18.40 3.60
-1 -2 19 23.50 3.40
0 2 -19 53.49 6.00
0 -2 19 47.00 6.10
-1 2 -19 48.60 5.30
1 -2 19 39.40 5.60
-2 2 -19 3.80 1.40
2 -2 19 2.50 1.30
-3 2 -19 2.10 1.20
3 -2 19 0.20 1.20
-4 2 -19 44.00 4.20
-4 2 -19 51.09 5.30
-4 2 -19 31.20 4.10
4 -2 19 33.50 5.70
-5 2 -19 4.90 2.10
-3 -1 19 0.50 1.20
2 1 -19 5.30 1.80
-2 -1 19 6.60 2.00
1 1 -19 55.19 6.90
-1 -1 19 64.69 7.00
0 1 -19 0.30 0.90
0 -1 19 1.20 1.10
-1 1 -19 40.30 4.70
1 -1 19 33.70 5.00
-2 1 -19 35.60 4.20
2 -1 19 25.90 4.30
-3 1 -19 66.79 7.20
3 -1 19 57.99 7.70
-4 1 -19 8.10 1.50
-4 1 -19 9.40 2.30
-4 1 -19 12.10 1.60
4 -1 19 5.40 2.80
-5 1 -19 -1.20 0.70
5 -1 19 3.80 2.30
-6 1 -19 0.20 1.10
-3 0 19 25.20 3.90
2 0 -19 4.20 1.40
-2 0 19 2.10 1.40
1 0 -19 35.50 5.00
-1 0 19 41.50 5.10
0 0 -19 48.80 6.00
0 0 19 52.29 6.20
-1 0 -19 75.59 8.10
1 0 19 70.89 8.40
-2 0 -19 5.00 1.60
2 0 19 7.20 2.40
-3 0 -19 17.20 3.00
3 0 19 11.20 3.00
-4 0 -19 54.69 5.30
-4 0 -19 57.19 6.10
-4 0 -19 45.80 5.20
4 0 19 38.60 6.60
-5 0 -19 7.80 1.60
-5 0 -19 5.10 1.40
5 0 19 4.10 2.20
-3 1 19 1.00 1.20
2 -1 -19 -0.30 1.50
-2 1 19 -2.00 0.90
1 -1 -19 72.09 8.80
-1 1 19 85.09 8.70
0 -1 -19 15.90 3.10
0 1 19 9.40 2.20
-1 -1 -19 10.40 2.30
1 1 19 7.60 2.20
-2 -1 -19 4.00 1.50
2 1 19 2.80 1.60
-3 -1 -19 175.88 16.50
-3 -1 -19 139.89 15.30
-3 -1 -19 180.78 15.40
3 1 19 155.18 17.30
-4 -1 -19 18.90 2.90
-4 -1 -19 13.50 2.00
-4 -1 -19 16.10 2.30
4 1 19 16.30 3.80
-5 -1 -19 11.90 2.20
-5 -1 -19 6.50 1.70
5 1 19 6.00 2.50
-6 -1 -19 5.10 1.70
-6 -1 -19 1.00 1.20
2 -2 -19 15.80 3.40
-2 2 19 23.30 3.30
1 -2 -19 10.30 2.40
-1 2 19 8.60 2.10
0 -2 -19 54.79 6.30
0 2 19 46.20 6.00
-1 -2 -19 44.20 5.20
1 2 19 36.20 5.30
-2 -2 -19 26.70 3.80
2 2 19 27.10 4.90
-3 -2 -19 37.00 4.90
-3 -2 -19 37.00 3.50
-3 -2 -19 30.20 3.60
3 2 19 27.30 5.30
-4 -2 -19 0.90 0.80
-4 -2 -19 -0.30 0.80
-4 -2 -19 -1.30 0.60
4 2 19 1.00 1.20
-5 -2 -19 16.70 2.80
-5 -2 -19 26.50 4.00
-6 -2 -19 6.20 2.10
-6 -2 -19 2.10 1.30
2 -3 -19 0.60 1.30
-2 3 19 -0.80 1.00
1 -3 -19 94.29 10.60
-1 3 19 94.59 10.20
0 -3 -19 4.60 1.70
0 3 19 7.10 2.10
-1 -3 -19 -0.10 0.80
1 3 19 0.30 1.00
-2 -3 -19 1.40 1.20
-2 -3 -19 2.30 0.50
-2 -3 -19 2.20 0.50
2 3 19 2.60 1.70
-3 -3 -19 61.89 6.70
-3 -3 -19 48.40 5.90
-3 -3 -19 58.99 5.70
3 3 19 62.29 9.20
-4 -3 -19 57.29 6.50
-4 -3 -19 67.19 7.30
-4 -3 -19 66.09 7.00
4 3 19 63.39 8.30
-5 -3 -19 13.40 2.20
-5 -3 -19 10.30 2.60
-6 -3 -19 4.70 2.00
-6 -3 -19 0.90 1.30
1 -4 -19 2.10 1.50
-1 4 19 -0.40 0.90
0 -4 -19 11.60 2.70
0 4 19 19.70 3.00
-1 -4 -19 12.00 2.70
-1 -4 -19 9.10 1.20
1 4 19 7.40 2.50
-2 -4 -19 59.39 6.20
-2 -4 -19 69.69 7.30
2 4 19 59.49 7.70
-3 -4 -19 23.50 3.50
-3 -4 -19 21.00 2.80
3 4 19 19.60 4.40
-4 -4 -19 23.70 3.40
-4 -4 -19 34.00 4.40
4 4 19 26.60 5.30
-5 -4 -19 18.10 2.90
-5 -4 -19 21.00 3.80
-2 5 19 -1.10 0.60
-1 5 19 74.89 7.50
0 -5 -19 7.50 2.10
0 -5 -19 6.60 1.20
0 5 19 4.70 1.30
0 5 19 6.70 1.30
-1 -5 -19 10.20 2.50
-1 -5 -19 7.60 1.20
1 5 19 4.30 1.60
-2 -5 -19 1.00 0.70
-2 -5 -19 -0.10 0.90
2 5 19 0.70 1.10
-3 -5 -19 2.20 1.20
-3 -5 -19 6.00 2.00
3 5 19 1.50 1.90
-4 -5 -19 69.49 7.50
-5 -5 -19 14.70 2.70
1 -6 -19 1.10 0.70
-1 6 19 0.70 0.80
0 6 19 5.10 1.30
1 6 19 -0.30 0.70
-2 -6 -19 25.00 2.90
2 6 19 18.40 2.90
2 6 19 18.60 4.30
-3 -6 -19 29.90 3.80
-4 -6 -19 50.59 5.90
0 -7 -19 12.80 2.00
0 7 19 12.80 2.30
-1 -7 -19 16.00 2.20
1 7 19 12.10 2.40
-2 -7 -19 2.30 1.00
2 7 19 -0.40 1.00
-3 -7 -19 26.50 3.70
-4 -7 -19 25.10 3.90
0 5 -20 4.20 1.30
0 -5 20 1.00 1.30
-1 5 -20 2.60 1.10
1 -5 20 -0.70 1.10
-2 5 -20 11.00 2.10
2 -5 20 7.30 2.30
1 4 -20 20.00 3.30
-1 -4 20 27.70 3.70
0 4 -20 22.80 3.20
0 -4 20 18.60 3.20
-1 4 -20 0.20 0.90
1 -4 20 1.50 1.10
-2 4 -20 0.10 0.70
2 -4 20 0.80 1.30
3 -4 20 -0.60 2.10
-2 -3 20 28.90 4.10
1 3 -20 0.20 1.00
-1 -3 20 0.10 1.00
0 3 -20 3.90 1.40
0 -3 20 2.70 1.40
-1 3 -20 11.60 2.30
1 -3 20 12.60 2.90
-2 3 -20 4.00 1.40
2 -3 20 2.00 1.50
3 -3 20 2.70 1.80
-4 3 -20 8.70 2.20
-4 3 -20 7.40 1.40
-4 3 -20 7.10 1.40
4 -3 20 8.60 2.50
-2 -2 20 3.90 1.50
1 2 -20 29.60 4.20
-1 -2 20 31.70 4.50
0 2 -20 20.10 3.10
0 -2 20 15.30 3.30
-1 2 -20 20.30 2.80
1 -2 20 13.10 3.10
-2 2 -20 3.10 1.30
2 -2 20 1.70 1.10
3 -2 20 4.70 2.30
-4 2 -20 0.60 0.60
-4 2 -20 -1.50 0.90
4 -2 20 -0.60 1.40
-5 2 -20 1.80 1.10
-5 2 -20 -0.40 0.90
2 1 -20 35.70 5.40
-2 -1 20 49.80 5.60
1 1 -20 8.40 2.10
-1 -1 20 6.80 1.90
0 1 -20 3.80 1.30
0 -1 20 4.40 1.80
-1 1 -20 23.00 3.30
1 -1 20 20.80 4.00
-2 1 -20 0.70 0.90
2 -1 20 -0.50 1.00
3 -1 20 3.00 2.40
-4 1 -20 0.30 0.60
-4 1 -20 -0.10 0.50
-4 1 -20 0.80 1.30
4 -1 20 0.20 1.30
-5 1 -20 17.70 2.50
-3 0 20 8.70 2.30
2 0 -20 3.10 1.70
1 0 -20 31.60 4.50
-1 0 20 33.20 4.50
0 0 -20 35.00 4.60
0 0 20 34.20 4.90
-1 0 -20 10.20 2.40
1 0 20 10.50 2.80
-2 0 -20 1.10 1.10
2 0 20 -0.60 1.10
-3 0 -20 28.70 3.90
3 0 20 15.90 5.70
-4 0 -20 0.00 1.20
-4 0 -20 2.70 0.80
4 0 20 1.40 1.50
2 -1 -20 30.70 4.80
-2 1 20 34.80 4.50
1 -1 -20 19.30 4.90
-1 1 20 32.30 4.70
0 -1 -20 4.80 1.70
0 1 20 5.40 2.00
-1 -1 -20 8.20 1.90
1 1 20 6.70 2.10
-2 -1 -20 1.40 1.30
2 1 20 2.00 1.30
-3 -1 -20 14.80 3.00
3 1 20 15.60 3.80
-4 -1 -20 3.20 0.90
-4 -1 -20 2.90 1.40
-4 -1 -20 5.30 1.00
4 1 20 2.90 1.90
-5 -1 -20 14.10 2.20
2 -2 -20 1.70 1.70
-2 2 20 -1.10 1.00
1 -2 -20 12.10 2.80
-1 2 20 8.50 2.20
0 -2 -20 65.69 8.00
0 2 20 68.99 9.30
1 2 20 10.20 3.30
-2 -2 -20 -0.30 0.80
2 2 20 -3.60 1.80
-3 -2 -20 16.30 1.60
-3 -2 -20 15.40 1.60
-3 -2 -20 20.10 3.10
3 2 20 7.60 2.70
-4 -2 -20 14.60 4.00
-4 -2 -20 10.30 1.90
-4 -2 -20 16.50 2.20
4 2 20 13.10 3.60
-5 -2 -20 18.50 3.90
1 -3 -20 51.69 6.60
-1 3 20 48.60 6.10
0 -3 -20 0.20 0.90
0 3 20 -0.70 0.80
-1 -3 -20 18.10 3.20
1 3 20 15.30 3.40
-2 -3 -20 4.20 1.60
2 3 20 1.10 1.30
-3 -3 -20 1.30 0.70
-3 -3 -20 0.40 1.20
3 3 20 2.60 1.80
-4 -3 -20 -1.90 0.80
-4 -3 -20 2.50 1.10
-5 -3 -20 -0.10 1.00
-5 -3 -20 4.10 1.50
0 4 20 22.20 3.60
-1 -4 -20 5.10 1.90
1 4 20 3.20 1.50
-2 -4 -20 1.80 1.50
2 4 20 1.80 1.50
-3 -4 -20 0.70 0.80
3 4 20 -0.20 1.50
-4 -4 -20 2.90 1.30
-4 -4 -20 3.40 1.30
-5 -4 -20 10.10 2.40
-5 -4 -20 7.60 1.90
-1 5 20 20.00 2.10
-1 -5 -20 8.80 1.30
-2 -5 -20 1.60 0.60
-3 -5 -20 23.50 3.00
-4 -5 -20 -0.70 1.20
0 -6 -20 3.50 0.90
0 6 20 2.20 0.90
-1 -6 -20 2.90 0.80
1 6 20 0.30 0.90
-2 -6 -20 5.80 1.20
-3 -6 -20 -1.30 0.90
-4 -6 -20 -1.60 1.40
-2 -7 -20 3.30 1.00
2 7 20 -1.30 0.90
-1 4 -21 12.10 2.30
1 -4 21 9.10 2.50
-2 4 -21 11.40 2.30
2 -4 21 5.00 2.20
1 3 -21 3.60 1.30
-1 -3 21 0.00 1.30
0 3 -21 10.40 2.40
0 -3 21 11.80 2.70
-1 3 -21 23.90 3.10
1 -3 21 15.90 3.20
-2 3 -21 1.00 1.10
2 -3 21 -0.40 1.30
-3 3 -21 4.40 1.60
3 -3 21 2.30 1.80
1 2 -21 4.40 1.50
-1 -2 21 1.70 1.40
0 2 -21 21.20 3.30
0 -2 21 23.20 4.10
-1 2 -21 36.40 4.40
1 -2 21 27.90 5.20
2 -2 21 21.30 5.30
-3 2 -21 6.50 1.80
3 -2 21 10.70 2.70
2 1 -21 2.80 1.40
-2 -1 21 0.80 1.40
1 1 -21 4.60 2.30
-1 -1 21 4.20 1.90
0 1 -21 36.60 4.70
0 -1 21 31.10 4.90
-1 1 -21 47.70 5.50
1 -1 21 38.90 5.90
-2 1 -21 2.10 1.40
2 -1 21 1.60 2.00
-3 1 -21 1.70 1.30
3 -1 21 2.40 1.70
2 0 -21 3.00 1.40
-2 0 21 3.50 1.70
1 0 -21 1.70 1.30
-1 0 21 0.20 1.10
0 0 -21 62.49 8.30
-1 0 -21 10.80 3.20
-2 0 -21 53.19 6.00
2 0 21 44.90 6.60
-3 0 -21 8.70 2.20
3 0 21 5.70 2.20
-4 0 -21 11.00 1.40
-4 0 -21 11.80 1.30
-5 0 -21 -0.30 0.90
1 -1 -21 3.10 1.50
-1 1 21 -1.30 0.80
0 -1 -21 3.70 1.20
0 1 21 0.80 1.30
-1 -1 -21 92.59 10.00
1 1 21 90.49 10.50
-2 -1 -21 5.50 1.70
2 1 21 3.80 2.00
-3 -1 -21 0.60 1.00
3 1 21 2.20 2.00
-1 2 21 0.60 1.50
0 -2 -21 43.10 6.10
0 2 21 56.19 6.40
-1 -2 -21 0.50 1.00
1 2 21 2.60 1.60
-2 -2 -21 29.10 3.90
2 2 21 20.70 4.40
3 2 21 -1.60 1.20
-4 -2 -21 4.80 1.20
-5 -2 -21 7.50 1.60
-5 -2 -21 1.60 1.20
1 3 21 36.00 5.30
2 3 21 13.80 3.50
-3 -3 -21 4.20 0.60
-3 -3 -21 4.20 0.60
-4 -3 -21 3.70 1.10
-3 -4 -21 2.10 0.90
-3 -4 -21 2.50 0.70
-4 -4 -21 9.40 1.90
-4 -4 -21 5.50 1.70
-2 -5 -21 18.20 2.10
-3 -5 -21 18.10 2.40
-1 -6 -21 24.40 2.90
-2 -6 -21 13.70 1.90
0 2 -22 2.70 1.50
0 -2 22 -0.90 1.80
-1 2 -22 2.30 1.10
1 -2 22 -1.40 1.20
-2 2 -22 3.60 1.40
2 -2 22 1.70 1.60
0 1 -22 22.20 3.30
0 -1 22 12.40 3.10
-1 1 -22 2.30 1.20
1 -1 22 -1.60 1.30
-2 1 -22 3.90 1.50
2 -1 22 4.90 2.00
-1 0 22 5.20 2.50
0 0 -22 4.80 1.80
0 0 22 4.90 2.00
-1 0 -22 2.40 1.10
1 0 22 1.40 1.50
-2 0 -22 -0.60 0.90
0 1 22 10.40 3.30
-1 -1 -22 20.70 4.60
2 1 22 -0.70 1.50
-3 -4 -22 8.00 1.30
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 52889
_shelx_res_file
;
TITL sci3_0m_a.res in P-1
REM Old TITL sci3_0m in P-1
REM SHELXT solution in P-1
REM R1 0.209, Rweak 0.015, Alpha 0.044, Orientation as input
REM Formula found by SHELXT: C14 N2 O4 S2
CELL 0.71073 6.2286 8.5209 16.2157 84.881 79.671 84.66
ZERR 2 0.0004 0.0004 0.0007 0.002 0.002 0.002
LATT 1
SFAC C H N O S
UNIT 28 42 6 6 4
ISOR 0.005 0.005 O3 O2 O1
L.S. 10
PLAN 20
SIZE 0.04 0.16 0.24
TEMP 21.85
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.010000 2.038400
FVAR 1.01378
S1 5 0.066504 0.211378 0.845068 11.00000 0.04366 0.03263 =
0.03309 -0.00372 -0.00121 -0.00585
O1 4 0.091032 0.340462 0.893012 11.00000 0.12355 0.09718 =
0.06745 -0.04078 0.02215 -0.06266
O2 4 0.132708 0.058772 0.876779 11.00000 0.10255 0.07194 =
0.08826 0.03156 0.03425 0.02580
O3 4 -0.158226 0.214767 0.833376 11.00000 0.05967 0.11049 =
0.06677 0.00176 0.00134 -0.01135
C8 1 0.228383 0.244125 0.744186 11.00000 0.03804 0.03112 =
0.03346 -0.00229 -0.00446 -0.00202
C9 1 0.425477 0.310420 0.734448 11.00000 0.04387 0.05901 =
0.04367 -0.00997 -0.00283 -0.01300
AFIX 43
H9 2 0.472209 0.345019 0.780589 11.00000 -1.20000
AFIX 0
C10 1 0.553360 0.325185 0.655640 11.00000 0.04841 0.07793 =
0.05915 -0.00795 0.00723 -0.02095
AFIX 43
H10 2 0.686867 0.369344 0.649520 11.00000 -1.20000
AFIX 0
C11 1 0.488307 0.276195 0.585838 11.00000 0.06379 0.07219 =
0.03941 -0.00142 0.00758 -0.00365
C12 1 0.290293 0.209938 0.596492 11.00000 0.07095 0.08802 =
0.03504 -0.01154 -0.00808 -0.01217
AFIX 43
H12 2 0.244083 0.175545 0.550191 11.00000 -1.20000
AFIX 0
C13 1 0.159394 0.193754 0.674706 11.00000 0.05390 0.06873 =
0.03785 -0.00597 -0.00946 -0.01663
AFIX 43
H13 2 0.026005 0.149441 0.680801 11.00000 -1.20000
AFIX 0
C14 1 0.632082 0.290557 0.499770 11.00000 0.10364 0.14078 =
0.05324 -0.01068 0.03053 -0.02451
AFIX 137
H14A 2 0.731032 0.371002 0.498479 11.00000 -1.50000
H14B 2 0.541889 0.318378 0.457674 11.00000 -1.50000
H14C 2 0.714206 0.191368 0.488752 11.00000 -1.50000
AFIX 0
S2 5 0.844609 0.772665 0.641253 11.00000 0.07492 0.10049 =
0.03692 -0.00939 0.00911 -0.00095
N1 3 0.690574 0.773357 0.840333 11.00000 0.04537 0.03252 =
0.03367 -0.00470 -0.00022 -0.01112
N2 3 0.541383 0.645656 0.857213 11.00000 0.04470 0.03262 =
0.03507 -0.00599 -0.00155 -0.00986
N3 3 0.260751 0.577768 0.964412 11.00000 0.04587 0.04792 =
0.04192 -0.00376 0.00176 -0.01486
AFIX 93
H3A 2 0.232397 0.500600 0.938381 11.00000 -1.20000
H3B 2 0.185200 0.596758 1.012810 11.00000 -1.20000
AFIX 0
C1 1 0.694334 0.838104 0.923874 11.00000 0.07717 0.06064 =
0.03902 -0.01700 0.00215 -0.03388
AFIX 23
H1A 2 0.713076 0.950534 0.917247 11.00000 -1.20000
H1B 2 0.810318 0.783863 0.950789 11.00000 -1.20000
AFIX 0
C2 1 0.470525 0.804742 0.973385 11.00000 0.06575 0.04155 =
0.03545 -0.00953 0.00217 -0.01229
AFIX 23
H2A 2 0.476133 0.776045 1.032251 11.00000 -1.20000
H2B 2 0.364269 0.894367 0.968630 11.00000 -1.20000
AFIX 0
C3 1 0.421247 0.667632 0.929863 11.00000 0.03888 0.03275 =
0.03403 -0.00240 -0.00424 -0.00286
C4 1 0.915138 0.708798 0.803993 11.00000 0.03923 0.05596 =
0.05088 -0.00177 -0.00579 -0.00479
AFIX 23
H4A 2 0.967340 0.629491 0.844054 11.00000 -1.20000
H4B 2 1.012760 0.793339 0.794992 11.00000 -1.20000
AFIX 0
C5 1 0.923660 0.635869 0.721923 11.00000 0.04852 0.05743 =
0.06058 -0.01833 0.00703 0.00276
AFIX 23
H5A 2 0.827912 0.550161 0.731240 11.00000 -1.20000
H5B 2 1.071557 0.591180 0.703186 11.00000 -1.20000
AFIX 0
C6 1 0.583002 0.839372 0.699535 11.00000 0.06279 0.08047 =
0.04139 0.01090 -0.00621 0.00593
AFIX 23
H6A 2 0.514229 0.922445 0.665877 11.00000 -1.20000
H6B 2 0.489338 0.752400 0.710390 11.00000 -1.20000
AFIX 0
C7 1 0.603024 0.900513 0.781308 11.00000 0.05849 0.03321 =
0.04898 0.00266 0.00796 0.00521
AFIX 23
H7A 2 0.460365 0.943570 0.807965 11.00000 -1.20000
H7B 2 0.700014 0.985501 0.770564 11.00000 -1.20000
AFIX 0
HKLF 4
REM sci3_0m_a.res in P-1
REM R1 = 0.0965 for 4011 Fo > 4sig(Fo) and 0.1077 for all 4869 data
REM 200 parameters refined using 18 restraints
END
WGHT 0.1538 0.6784
REM Highest difference peak 1.695, deepest hole -0.568, 1-sigma level 0.134
Q1 1 0.2380 0.2445 0.8971 11.00000 0.05 1.70
Q2 1 -0.0943 0.3096 0.8483 11.00000 0.05 1.54
Q3 1 0.0411 0.0587 0.8404 11.00000 0.05 1.03
Q4 1 0.7158 0.7989 0.6579 11.00000 0.05 0.94
Q5 1 0.2062 0.2013 0.8307 11.00000 0.05 0.84
Q6 1 0.9239 0.7344 0.6718 11.00000 0.05 0.79
Q7 1 -0.0081 0.2241 0.8099 11.00000 0.05 0.71
Q8 1 0.8074 0.7525 0.8161 11.00000 0.05 0.68
Q9 1 0.2248 0.1215 0.8879 11.00000 0.05 0.64
Q10 1 -0.1058 0.1329 0.8420 11.00000 0.05 0.64
Q11 1 0.9959 0.7637 0.6304 11.00000 0.05 0.55
Q12 1 0.2595 0.5451 0.9539 11.00000 0.05 0.40
Q13 1 0.5447 0.3076 0.7073 11.00000 0.05 0.40
Q14 1 0.5827 0.8265 0.9500 11.00000 0.05 0.39
Q15 1 0.2970 0.6324 0.9415 11.00000 0.05 0.35
Q16 1 0.7306 0.8368 0.9418 11.00000 0.05 0.34
Q17 1 0.0967 0.5891 0.9725 11.00000 0.05 0.34
Q18 1 0.1389 0.2403 0.6119 11.00000 0.05 0.34
Q19 1 0.1687 0.5724 0.9276 11.00000 0.05 0.30
Q20 1 0.6698 0.8213 0.8189 11.00000 0.05 0.30
;
_shelx_res_checksum 87149
_shelxl_version_number 2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.06650(13) 0.21138(9) 0.84507(5) 0.0369(2) Uani d 1 . .
O O1 0.0910(7) 0.3405(5) 0.8930(2) 0.0953(13) Uani d 1 . .
O O2 0.1327(7) 0.0588(4) 0.8768(3) 0.0983(13) Uani d 1 . .
O O3 -0.1582(5) 0.2148(5) 0.8334(2) 0.0807(10) Uani d 1 . .
C C8 0.2284(5) 0.2441(3) 0.74419(18) 0.0345(6) Uani d 1 . .
C C9 0.4255(6) 0.3104(5) 0.7344(2) 0.0485(8) Uani d 1 . .
H H9 0.4722 0.3450 0.7806 0.058 Uiso calc 1 . .
C C10 0.5534(7) 0.3252(6) 0.6556(3) 0.0627(11) Uani d 1 . .
H H10 0.6869 0.3693 0.6495 0.075 Uiso calc 1 . .
C C11 0.4883(7) 0.2762(6) 0.5858(2) 0.0608(10) Uani d 1 . .
C C12 0.2903(8) 0.2099(6) 0.5965(2) 0.0640(11) Uani d 1 . .
H H12 0.2441 0.1755 0.5502 0.077 Uiso calc 1 . .
C C13 0.1594(6) 0.1938(5) 0.6747(2) 0.0524(9) Uani d 1 . .
H H13 0.0260 0.1494 0.6808 0.063 Uiso calc 1 . .
C C14 0.6321(11) 0.2906(9) 0.4998(3) 0.104(2) Uani d 1 . .
H H14A 0.7310 0.3710 0.4985 0.155 Uiso calc 1 . .
H H14B 0.5419 0.3184 0.4577 0.155 Uiso calc 1 . .
H H14C 0.7142 0.1914 0.4888 0.155 Uiso calc 1 . .
S S2 0.8446(2) 0.77266(18) 0.64125(7) 0.0732(4) Uani d 1 . .
N N1 0.6906(4) 0.7734(3) 0.84033(16) 0.0374(5) Uani d 1 . .
N N2 0.5414(4) 0.6457(3) 0.85721(16) 0.0375(5) Uani d 1 . .
N N3 0.2608(5) 0.5778(4) 0.96441(18) 0.0457(7) Uani d 1 . .
H H3A 0.2324 0.5006 0.9384 0.055 Uiso calc 1 . .
H H3B 0.1852 0.5968 1.0128 0.055 Uiso calc 1 . .
C C1 0.6943(7) 0.8381(5) 0.9239(2) 0.0578(10) Uani d 1 . .
H H1A 0.7131 0.9505 0.9172 0.069 Uiso calc 1 . .
H H1B 0.8103 0.7839 0.9508 0.069 Uiso calc 1 . .
C C2 0.4705(6) 0.8047(4) 0.9734(2) 0.0480(8) Uani d 1 . .
H H2A 0.4761 0.7760 1.0323 0.058 Uiso calc 1 . .
H H2B 0.3643 0.8944 0.9686 0.058 Uiso calc 1 . .
C C3 0.4212(5) 0.6676(3) 0.92986(19) 0.0355(6) Uani d 1 . .
C C4 0.9151(6) 0.7088(5) 0.8040(2) 0.0490(8) Uani d 1 . .
H H4A 0.9673 0.6295 0.8441 0.059 Uiso calc 1 . .
H H4B 1.0128 0.7933 0.7950 0.059 Uiso calc 1 . .
C C5 0.9237(7) 0.6359(5) 0.7219(3) 0.0571(10) Uani d 1 . .
H H5A 0.8279 0.5502 0.7312 0.069 Uiso calc 1 . .
H H5B 1.0716 0.5912 0.7032 0.069 Uiso calc 1 . .
C C6 0.5830(7) 0.8394(6) 0.6995(3) 0.0636(11) Uani d 1 . .
H H6A 0.5142 0.9224 0.6659 0.076 Uiso calc 1 . .
H H6B 0.4893 0.7524 0.7104 0.076 Uiso calc 1 . .
C C7 0.6030(6) 0.9005(4) 0.7813(2) 0.0499(8) Uani d 1 . .
H H7A 0.4604 0.9436 0.8080 0.060 Uiso calc 1 . .
H H7B 0.7000 0.9855 0.7706 0.060 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 0.0437(4) 0.0326(4) 0.0331(4) -0.0058(3) -0.0012(3) -0.0037(3)
O1 0.124(3) 0.097(2) 0.0675(19) -0.063(2) 0.0222(18) -0.0408(18)
O2 0.103(2) 0.072(2) 0.088(2) 0.0258(18) 0.0342(19) 0.0316(17)
O3 0.0597(18) 0.110(3) 0.0668(19) -0.0114(17) 0.0013(15) 0.0018(18)
C8 0.0380(15) 0.0311(13) 0.0335(14) -0.0020(11) -0.0045(11) -0.0023(10)
C9 0.0439(18) 0.059(2) 0.0437(18) -0.0130(15) -0.0028(14) -0.0100(15)
C10 0.048(2) 0.078(3) 0.059(2) -0.0210(19) 0.0072(17) -0.008(2)
C11 0.064(2) 0.072(3) 0.0394(18) -0.004(2) 0.0076(17) -0.0014(17)
C12 0.071(3) 0.088(3) 0.0350(18) -0.012(2) -0.0081(17) -0.0115(19)
C13 0.054(2) 0.069(2) 0.0378(17) -0.0166(18) -0.0095(15) -0.0060(16)
C14 0.104(4) 0.141(6) 0.053(3) -0.025(4) 0.031(3) -0.011(3)
S2 0.0749(8) 0.1005(10) 0.0369(5) -0.0010(6) 0.0091(5) -0.0094(5)
N1 0.0454(14) 0.0325(12) 0.0337(12) -0.0111(10) -0.0002(10) -0.0047(9)
N2 0.0447(14) 0.0326(12) 0.0351(12) -0.0099(10) -0.0015(10) -0.0060(9)
N3 0.0459(15) 0.0479(16) 0.0419(14) -0.0149(12) 0.0018(12) -0.0038(12)
C1 0.077(3) 0.061(2) 0.0390(17) -0.034(2) 0.0022(17) -0.0170(16)
C2 0.066(2) 0.0415(17) 0.0354(16) -0.0123(15) 0.0022(14) -0.0095(13)
C3 0.0389(15) 0.0328(13) 0.0340(14) -0.0029(11) -0.0042(11) -0.0024(10)
C4 0.0392(17) 0.056(2) 0.0509(19) -0.0048(15) -0.0058(14) -0.0018(16)
C5 0.049(2) 0.057(2) 0.061(2) 0.0028(17) 0.0070(17) -0.0183(18)
C6 0.063(2) 0.080(3) 0.0414(19) 0.006(2) -0.0062(17) 0.0109(18)
C7 0.058(2) 0.0332(15) 0.0490(19) 0.0052(14) 0.0080(16) 0.0027(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 S1 O3 . . 109.4(3) ?
O1 S1 C8 . . 107.08(18) ?
O2 S1 O1 . . 116.8(3) ?
O2 S1 O3 . . 109.0(3) ?
O2 S1 C8 . . 106.86(18) ?
O3 S1 C8 . . 107.25(18) ?
C9 C8 S1 . . 121.1(2) ?
C9 C8 C13 . . 119.8(3) ?
C13 C8 S1 . . 119.0(3) ?
C8 C9 H9 . . 120.2 ?
C8 C9 C10 . . 119.5(3) ?
C10 C9 H9 . . 120.2 ?
C9 C10 H10 . . 119.1 ?
C11 C10 C9 . . 121.7(4) ?
C11 C10 H10 . . 119.1 ?
C10 C11 C12 . . 118.1(4) ?
C10 C11 C14 . . 121.2(5) ?
C12 C11 C14 . . 120.6(5) ?
C11 C12 H12 . . 119.4 ?
C11 C12 C13 . . 121.2(4) ?
C13 C12 H12 . . 119.4 ?
C8 C13 H13 . . 120.2 ?
C12 C13 C8 . . 119.6(4) ?
C12 C13 H13 . . 120.2 ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14B . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C5 S2 C6 . . 96.39(18) ?
N2 N1 C1 . . 106.8(2) ?
N2 N1 C4 . . 109.9(2) ?
N2 N1 C7 . . 108.9(3) ?
C4 N1 C1 . . 109.6(3) ?
C4 N1 C7 . . 111.3(3) ?
C7 N1 C1 . . 110.2(3) ?
C3 N2 N1 . . 106.2(2) ?
H3A N3 H3B . . 120.0 ?
C3 N3 H3A . . 120.0 ?
C3 N3 H3B . . 120.0 ?
N1 C1 H1A . . 111.3 ?
N1 C1 H1B . . 111.3 ?
N1 C1 C2 . . 102.5(3) ?
H1A C1 H1B . . 109.2 ?
C2 C1 H1A . . 111.3 ?
C2 C1 H1B . . 111.3 ?
C1 C2 H2A . . 111.6 ?
C1 C2 H2B . . 111.6 ?
H2A C2 H2B . . 109.4 ?
C3 C2 C1 . . 100.6(3) ?
C3 C2 H2A . . 111.6 ?
C3 C2 H2B . . 111.6 ?
N2 C3 N3 . . 123.2(3) ?
N2 C3 C2 . . 115.9(3) ?
N3 C3 C2 . . 120.9(3) ?
N1 C4 H4A . . 109.0 ?
N1 C4 H4B . . 109.0 ?
N1 C4 C5 . . 112.9(3) ?
H4A C4 H4B . . 107.8 ?
C5 C4 H4A . . 109.0 ?
C5 C4 H4B . . 109.0 ?
S2 C5 H5A . . 108.9 ?
S2 C5 H5B . . 108.9 ?
C4 C5 S2 . . 113.4(3) ?
C4 C5 H5A . . 108.9 ?
C4 C5 H5B . . 108.9 ?
H5A C5 H5B . . 107.7 ?
S2 C6 H6A . . 109.2 ?
S2 C6 H6B . . 109.2 ?
H6A C6 H6B . . 107.9 ?
C7 C6 S2 . . 112.2(3) ?
C7 C6 H6A . . 109.2 ?
C7 C6 H6B . . 109.2 ?
N1 C7 H7A . . 109.2 ?
N1 C7 H7B . . 109.2 ?
C6 C7 N1 . . 112.2(3) ?
C6 C7 H7A . . 109.2 ?
C6 C7 H7B . . 109.2 ?
H7A C7 H7B . . 107.9 ?
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
S1 O1 . 1.437(3) ?
S1 O2 . 1.408(3) ?
S1 O3 . 1.443(3) ?
S1 C8 . 1.775(3) ?
C8 C9 . 1.376(4) ?
C8 C13 . 1.390(4) ?
C9 H9 . 0.9300 ?
C9 C10 . 1.381(5) ?
C10 H10 . 0.9300 ?
C10 C11 . 1.378(6) ?
C11 C12 . 1.380(6) ?
C11 C14 . 1.519(6) ?
C12 H12 . 0.9300 ?
C12 C13 . 1.382(5) ?
C13 H13 . 0.9300 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
S2 C5 . 1.779(5) ?
S2 C6 . 1.801(4) ?
N1 N2 . 1.472(3) ?
N1 C1 . 1.512(4) ?
N1 C4 . 1.492(4) ?
N1 C7 . 1.510(4) ?
N2 C3 . 1.296(4) ?
N3 H3A . 0.8600 ?
N3 H3B . 0.8600 ?
N3 C3 . 1.328(4) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 C2 . 1.517(5) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C3 . 1.500(4) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C5 . 1.509(5) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C6 C7 . 1.497(6) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
_cod_database_fobs_code 2022664