#------------------------------------------------------------------------------
#$Date: 2025-01-29 05:24:54 +0200 (Wed, 29 Jan 2025) $
#$Revision: 297520 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023365.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_2023365
loop_
_publ_author_name
'Gurbanov, Atash V.'
'Guseinov, Firudin I.'
'Samigullina, Aida I.'
'H\"okelek, Tuncer'
'Hasanov, Khudayar I.'
'Javadzade, Tahir A.'
'Belay, Alebel N.'
_publ_section_title
;
Synthesis and crystal structure analysis of
1-ethyl-1,3-dihydro-2H-benzo[d]imidazole-2-thione
;
_journal_coeditor_code PK2714
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025000519
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration unknown
_chemical_formula_iupac 'C9 H10 N2 S'
_chemical_formula_moiety 'C9 H10 N2 S'
_chemical_formula_sum 'C9 H10 N2 S'
_chemical_formula_weight 178.25
_chemical_name_systematic
;
1-Ethyl-1,3-dihydro-2H-benzo[d]imidazole-2-thione
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 7.4512(5)
_cell_length_b 14.77990(12)
_cell_length_c 15.89120(11)
_cell_measurement_reflns_used 18990
_cell_measurement_temperature 99.9(4)
_cell_measurement_theta_max 79.0060
_cell_measurement_theta_min 4.0570
_cell_volume 1750.07(12)
_computing_cell_refinement
;
CrysAlisPRO (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPRO (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPRO (Rigaku OD, 2023)
;
_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 99.9(4)
_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 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix 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 0.0348
_diffrn_reflns_av_unetI/netI 0.0205
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 23801
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 79.527
_diffrn_reflns_theta_min 4.085
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.803
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.405
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2023)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 752
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.17
_refine_diff_density_max 0.247
_refine_diff_density_min -0.210
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.454(16)
_refine_ls_extinction_coef 0.0010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 229
_refine_ls_number_reflns 3799
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0258
_refine_ls_R_factor_gt 0.0257
_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^)+(0.0359P)^2^+0.5853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0689
_refine_ls_wR_factor_ref 0.0690
_reflns_number_gt 3779
_reflns_number_total 3799
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2714.cif
_cod_data_source_block I
_cod_original_cell_volume 1750.06(12)
_cod_database_code 2023365
_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 0.393
_shelx_estimated_absorpt_t_max 0.647
_shelx_hkl_file
;
0 0 1 0.05 0.09
0 0 2 4806.00 139.06
0 0 3 0.15 0.27
0 0 4 902.71 28.20
0 0 5 0.13 0.29
0 0 6 374.04 14.04
0 0 7 0.37 0.52
0 0 8 1261.89 37.07
0 0 8 1248.73 40.62
0 0 8 1227.11 37.10
0 0 9 0.07 0.26
0 0 9 0.69 0.34
0 0 10 86.54 4.01
0 0 10 98.06 4.19
0 0 11 1.69 0.62
0 0 11 2.36 0.69
0 0 11 -0.09 0.32
0 0 11 0.66 0.49
0 0 11 -0.09 0.39
0 0 11 0.44 0.41
0 0 11 1.12 0.53
0 0 11 -0.11 0.34
0 0 11 0.60 0.50
0 0 12 361.44 12.68
0 0 12 367.85 12.77
0 0 12 347.49 12.37
0 0 12 353.37 12.61
0 0 12 366.25 12.55
0 0 12 373.09 13.01
0 0 12 367.18 12.42
0 0 12 350.05 12.22
0 0 12 379.65 12.71
0 0 12 396.42 13.01
0 0 12 372.70 12.61
0 0 13 0.21 0.58
0 0 13 1.41 0.60
0 0 13 0.62 0.49
0 0 13 0.54 0.53
0 0 13 1.79 0.75
0 0 13 0.11 0.47
0 0 13 0.68 0.50
0 0 13 0.38 0.38
0 0 13 0.42 0.59
0 0 14 315.83 11.05
0 0 14 319.52 11.01
0 0 14 314.65 11.09
0 0 14 321.89 11.76
0 0 14 276.85 10.47
0 0 14 282.90 11.13
0 0 14 300.95 11.04
0 0 15 0.69 0.55
0 0 15 0.74 0.61
0 0 15 1.16 0.55
0 0 15 0.70 0.62
0 0 15 -0.11 0.51
0 0 15 0.33 0.55
0 0 15 -0.10 0.58
0 0 16 133.74 5.41
0 0 16 127.69 5.45
0 0 16 122.04 5.86
0 0 16 121.58 5.57
0 0 16 114.99 5.28
0 0 16 128.94 5.48
0 0 17 -0.09 0.40
0 0 17 0.11 0.46
0 0 17 0.16 0.53
0 0 17 3.30 0.72
0 0 17 2.22 0.71
0 0 18 249.46 8.11
0 0 18 230.96 8.32
0 0 18 227.07 8.52
0 0 19 0.56 0.36
0 0 19 -0.05 0.30
0 1 0 0.03 0.08
0 -1 1 48.80 1.91
0 1 1 49.47 2.06
0 -1 -1 50.07 1.97
0 -1 2 584.36 18.12
0 -1 -2 600.51 17.64
0 -1 2 588.63 17.65
0 1 3 2.38 0.32
0 1 -3 4.27 0.41
0 -1 3 3.49 0.63
0 -1 3 3.61 0.39
0 -1 -3 2.85 0.35
0 1 4 423.86 13.08
0 1 -4 457.39 13.16
0 -1 4 453.35 14.95
0 -1 -4 444.93 13.10
0 -1 4 439.36 13.12
0 -1 5 52.25 3.40
0 -1 6 196.25 8.60
0 -1 7 187.90 8.77
0 1 8 68.87 2.99
0 -1 8 67.13 4.85
0 -1 8 62.16 2.86
0 1 8 65.98 2.96
0 -1 8 62.25 2.97
0 1 9 0.93 0.39
0 -1 9 0.51 0.32
0 1 10 18.47 1.51
0 -1 10 19.13 1.58
0 1 11 25.33 2.00
0 1 11 27.55 2.22
0 -1 11 25.33 1.93
0 1 11 23.63 1.99
0 1 11 27.02 1.95
0 -1 11 26.44 2.05
0 -1 11 26.91 2.05
0 -1 11 27.15 1.98
0 -1 11 23.52 1.87
0 -1 11 24.35 2.07
0 1 12 70.89 3.79
0 1 12 68.53 3.63
0 1 12 69.56 3.66
0 -1 12 66.36 3.76
0 1 12 72.36 3.86
0 -1 12 71.91 3.67
0 1 12 68.55 3.56
0 -1 12 72.06 3.85
0 -1 12 70.94 3.74
0 -1 12 67.75 3.60
0 -1 12 67.12 3.85
0 1 12 61.18 3.72
0 1 12 64.10 3.50
0 1 12 67.32 3.34
0 -1 12 68.10 3.59
0 1 12 66.29 3.65
0 -1 12 67.62 3.47
0 -1 13 23.60 2.06
0 1 13 21.80 1.88
0 -1 13 20.54 1.99
0 -1 13 23.54 2.19
0 1 13 21.04 1.93
0 -1 13 22.79 1.95
0 1 13 20.41 1.80
0 -1 13 18.61 1.78
0 1 13 22.93 2.09
0 1 13 18.27 1.58
0 -1 13 23.67 2.14
0 -1 13 17.97 1.68
0 -1 13 21.85 1.89
0 1 13 22.54 2.05
0 1 13 22.47 1.95
0 -1 13 19.35 1.92
0 1 13 24.10 2.00
0 -1 14 339.23 11.98
0 1 14 361.94 12.48
0 1 14 305.67 11.36
0 1 14 288.43 10.60
0 1 14 311.18 11.60
0 -1 14 315.16 11.25
0 1 14 318.85 11.29
0 -1 14 312.46 11.56
0 -1 14 317.15 11.78
0 1 14 316.44 10.84
0 -1 14 319.39 11.49
0 1 14 326.63 11.16
0 -1 14 321.38 11.31
0 1 14 316.33 11.53
0 1 14 296.08 11.19
0 -1 14 334.89 11.42
0 -1 15 138.93 5.90
0 -1 15 138.44 6.33
0 1 15 134.99 6.52
0 1 15 129.27 5.71
0 1 15 129.82 6.01
0 -1 15 135.41 6.21
0 -1 15 131.14 5.70
0 -1 15 133.08 6.04
0 1 15 140.30 6.10
0 -1 15 146.47 5.97
0 1 15 145.35 5.79
0 -1 16 22.39 1.92
0 -1 16 25.30 2.21
0 1 16 24.88 2.33
0 -1 16 24.56 2.04
0 -1 16 27.61 2.23
0 1 16 22.61 1.97
0 1 16 25.01 2.07
0 -1 16 24.33 2.11
0 1 16 26.73 1.92
0 -1 16 26.23 2.02
0 -1 17 7.26 1.03
0 -1 17 6.38 1.05
0 1 17 6.50 1.12
0 -1 17 7.87 1.10
0 -1 17 6.44 0.94
0 1 17 4.30 0.80
0 -1 17 5.80 0.91
0 -1 17 6.61 1.02
0 1 17 6.30 0.99
0 -1 18 9.72 1.11
0 1 18 9.69 1.12
0 -1 18 10.91 1.12
0 1 18 9.99 1.25
0 1 18 12.98 1.07
0 -1 18 11.53 1.11
0 -1 19 187.87 6.19
0 -1 19 175.97 6.23
0 -1 20 25.55 1.17
0 2 0 1192.59 34.79
0 -2 -1 42.98 2.20
0 2 1 49.69 2.17
0 2 1 41.25 2.04
0 -2 1 43.40 1.74
0 2 1 43.39 1.73
0 -2 2 150.62 5.42
0 -2 -2 144.41 5.36
0 2 2 134.00 5.36
0 -2 2 150.00 5.28
0 2 2 152.99 5.27
0 -2 -3 18.44 1.33
0 -2 3 20.35 1.39
0 2 3 20.85 1.58
0 -2 3 17.45 1.47
0 -2 -4 1640.94 47.90
0 -2 4 1611.99 47.91
0 2 -4 1614.08 47.87
0 2 4 1580.35 47.79
0 2 4 1646.49 48.93
0 -2 4 1701.97 49.07
0 -2 5 97.66 3.80
0 -2 -5 99.24 3.79
0 -2 5 98.11 5.02
0 2 5 99.41 4.98
0 2 -5 101.02 3.86
0 2 5 88.78 3.68
0 2 6 318.54 11.75
0 -2 6 318.76 11.80
0 2 6 275.26 8.98
0 2 -6 312.01 9.15
0 -2 6 296.81 9.03
0 -2 -6 282.46 8.98
0 2 7 24.79 2.59
0 -2 7 23.16 2.55
0 -2 7 21.06 1.47
0 2 8 842.60 28.69
0 -2 8 887.35 29.00
0 2 8 848.67 25.26
0 -2 8 767.25 25.13
0 -2 8 886.45 25.64
0 -2 8 835.69 25.45
0 -2 9 19.92 1.47
0 2 9 21.31 1.54
0 -2 9 18.80 1.56
0 -2 10 114.42 4.88
0 2 10 112.16 4.67
0 -2 10 105.68 4.57
0 -2 11 58.79 3.35
0 -2 11 57.16 3.11
0 2 11 62.22 3.39
0 2 11 63.28 3.17
0 -2 11 63.27 3.41
0 2 11 62.47 3.43
0 2 11 57.70 3.42
0 -2 11 65.73 3.32
0 2 11 61.40 3.23
0 -2 11 55.49 3.36
0 2 11 62.59 3.65
0 -2 11 65.40 3.36
0 2 11 60.90 3.43
0 -2 11 69.90 3.68
0 2 11 62.42 3.70
0 2 11 61.79 3.46
0 -2 12 130.28 5.66
0 2 12 135.97 5.69
0 2 12 137.48 6.03
0 -2 12 142.53 6.22
0 2 12 105.44 5.55
0 2 12 130.83 5.73
0 -2 12 152.15 6.22
0 2 12 130.26 6.14
0 2 12 133.20 5.64
0 2 12 132.65 5.86
0 2 12 132.44 5.64
0 -2 12 136.80 5.64
0 -2 12 140.06 6.10
0 2 12 138.61 5.98
0 2 12 139.51 6.12
0 -2 12 146.10 6.06
0 2 12 129.55 5.36
0 -2 12 133.32 5.88
0 2 12 141.88 6.08
0 2 12 132.30 5.65
0 -2 12 146.25 5.83
0 2 13 0.85 0.63
0 2 13 0.38 0.43
0 -2 13 0.59 0.51
0 2 13 2.61 0.75
0 2 13 0.62 0.60
0 -2 13 1.12 0.66
0 2 13 2.39 0.80
0 2 13 1.66 0.60
0 2 13 0.62 0.48
0 -2 13 0.93 0.63
0 2 13 1.01 0.50
0 2 13 1.04 0.63
0 2 13 1.07 0.54
0 -2 13 2.15 0.73
0 2 13 1.17 0.53
0 -2 13 1.22 0.60
0 2 13 0.94 0.61
0 -2 13 1.15 0.66
0 2 13 0.71 0.61
0 -2 13 0.40 0.56
0 -2 13 0.41 0.54
0 2 14 158.88 6.21
0 -2 14 167.88 6.91
0 2 14 159.05 6.67
0 2 14 151.90 6.25
0 -2 14 155.75 6.82
0 2 14 137.44 6.06
0 -2 14 152.06 6.54
0 2 14 149.88 6.60
0 -2 14 154.34 6.79
0 -2 14 147.63 6.29
0 -2 14 157.45 6.39
0 2 14 143.28 6.47
0 2 14 155.84 6.77
0 2 14 165.67 6.51
0 -2 14 162.09 6.51
0 -2 15 42.81 2.92
0 -2 15 41.09 2.70
0 -2 15 35.72 2.76
0 2 15 38.52 2.68
0 2 15 39.31 2.61
0 -2 15 40.44 2.66
0 -2 15 35.79 2.71
0 2 15 41.90 3.20
0 -2 15 37.45 2.73
0 2 15 37.16 2.75
0 2 15 39.54 2.43
0 -2 16 23.67 2.06
0 -2 16 21.77 1.81
0 -2 16 21.86 1.95
0 2 16 21.91 1.84
0 2 16 22.07 1.82
0 -2 16 21.56 1.83
0 -2 16 22.81 1.99
0 2 16 21.50 2.19
0 2 16 22.07 1.99
0 -2 16 20.01 1.86
0 2 16 23.47 1.72
0 -2 17 67.28 3.46
0 -2 17 58.64 3.20
0 -2 17 62.72 3.15
0 2 17 64.88 3.18
0 -2 17 60.32 3.21
0 2 17 58.38 3.24
0 2 17 63.05 2.91
0 2 17 60.32 3.60
0 -2 17 54.25 3.14
0 -2 18 146.65 5.49
0 2 18 134.38 5.84
0 2 18 148.49 5.16
0 2 18 139.01 5.62
0 -2 18 148.23 5.52
0 -2 19 33.20 1.68
0 -2 19 29.41 1.66
0 -2 20 16.28 0.87
0 3 0 1.28 0.33
0 3 1 333.52 10.99
0 3 1 324.24 10.77
0 -3 -1 335.92 11.33
0 -3 2 1154.44 34.43
0 3 2 1136.39 34.34
0 3 2 1176.76 35.27
0 3 2 1143.05 35.09
0 -3 -2 1206.27 35.32
0 -3 2 1176.04 35.34
0 3 3 151.52 5.90
0 -3 3 158.32 6.02
0 3 3 158.25 6.46
0 -3 3 153.29 6.21
0 -3 -3 155.87 6.18
0 -3 4 1.73 0.57
0 3 4 2.28 0.64
0 3 4 2.25 0.58
0 3 -4 2.41 0.59
0 -3 -4 2.19 0.59
0 -3 4 2.05 0.58
0 3 5 117.85 5.72
0 -3 5 124.60 5.85
0 3 -5 124.12 5.19
0 3 5 123.04 5.14
0 -3 5 124.50 5.22
0 -3 -5 119.26 5.13
0 -3 6 564.98 18.95
0 3 6 546.10 18.81
0 3 -6 586.54 17.47
0 3 6 523.95 17.11
0 -3 -6 523.30 17.15
0 -3 6 509.58 17.10
0 -3 7 1.78 0.47
0 3 7 2.03 0.81
0 -3 7 2.47 0.87
0 3 7 1.65 0.37
0 -3 7 2.28 0.44
0 -3 8 254.14 8.73
0 3 8 242.37 8.27
0 -3 8 242.67 8.23
0 -3 9 8.77 1.10
0 3 9 9.91 1.00
0 -3 9 10.29 1.02
0 -3 10 25.77 1.99
0 3 10 26.13 1.81
0 -3 10 25.63 2.02
0 -3 11 168.71 6.81
0 3 11 170.15 7.04
0 3 11 167.34 6.86
0 -3 11 199.84 7.09
0 -3 11 162.62 6.91
0 3 11 165.00 6.82
0 -3 11 170.08 6.51
0 3 11 172.02 6.95
0 3 11 174.40 6.88
0 3 11 170.03 7.12
0 3 11 156.79 6.26
0 -3 11 165.42 6.96
0 -3 11 180.92 6.90
0 3 11 179.65 6.66
0 -3 11 167.98 6.63
0 -3 11 165.68 6.92
0 3 11 174.68 7.11
0 3 11 170.93 7.41
0 -3 12 227.69 8.92
0 3 12 236.43 9.20
0 3 12 250.15 9.19
0 -3 12 223.92 9.08
0 -3 12 266.17 9.26
0 3 12 233.35 9.01
0 3 12 249.74 9.27
0 -3 12 231.07 8.64
0 -3 12 255.80 9.45
0 -3 12 237.43 9.23
0 3 12 240.02 9.40
0 3 12 230.09 8.48
0 -3 12 258.85 9.18
0 3 12 252.27 9.21
0 -3 12 244.61 8.87
0 3 12 250.39 8.87
0 -3 12 225.15 9.12
0 3 12 229.34 9.24
0 3 12 235.78 9.70
0 3 13 0.88 0.62
0 -3 13 0.30 0.51
0 -3 13 0.54 0.61
0 3 13 1.57 0.69
0 3 13 0.56 0.56
0 -3 13 1.26 0.65
0 3 13 0.43 0.45
0 -3 13 1.78 0.72
0 3 13 0.48 0.55
0 3 13 0.40 0.59
0 -3 13 2.21 0.80
0 3 13 0.80 0.52
0 -3 13 0.12 0.48
0 -3 13 1.67 0.67
0 3 13 1.24 0.59
0 3 13 0.26 0.62
0 3 14 23.53 2.18
0 3 14 17.91 1.87
0 -3 14 19.29 1.93
0 3 14 21.33 2.09
0 3 14 25.58 1.80
0 -3 14 18.44 1.94
0 -3 14 18.77 1.94
0 3 14 19.41 1.93
0 3 14 20.57 1.89
0 3 14 20.58 1.82
0 -3 14 20.10 1.82
0 3 14 17.90 1.79
0 -3 14 17.32 1.91
0 -3 14 18.42 1.88
0 -3 14 18.65 1.94
0 -3 14 20.58 1.92
0 -3 14 18.33 1.80
0 -3 15 135.41 6.04
0 3 15 136.65 5.33
0 -3 15 136.46 5.84
0 3 15 136.32 6.54
0 3 15 125.87 5.78
0 -3 15 135.09 6.09
0 -3 15 133.27 6.05
0 3 15 117.98 5.52
0 -3 15 124.12 5.75
0 -3 15 126.33 5.57
0 3 15 131.35 6.10
0 -3 15 135.75 5.84
0 -3 15 139.85 5.74
0 3 15 136.50 5.65
0 3 16 171.01 6.55
0 -3 16 165.25 6.50
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8 -6 -6 76.02 3.30
8 -6 -6 75.32 3.27
-8 -6 6 82.70 3.54
8 6 6 76.49 3.31
8 -6 -7 18.00 1.22
8 -6 -7 17.86 1.16
8 6 7 22.25 1.35
-8 -6 7 19.51 1.38
8 6 7 19.72 1.37
8 6 8 17.75 1.11
8 6 8 18.68 1.15
-8 7 7 141.38 4.84
8 7 -7 151.18 4.82
-8 7 6 27.88 1.74
8 7 -6 31.23 1.54
8 7 -6 31.84 1.73
-8 7 5 26.20 1.78
8 7 -5 26.36 1.67
8 7 -5 26.50 1.51
8 7 -4 25.99 1.58
-8 7 3 55.49 2.99
-8 7 3 51.09 2.67
8 7 -3 54.51 2.75
8 7 -3 58.09 2.66
-8 7 2 19.77 1.67
-8 7 2 20.38 1.55
8 -7 2 18.38 1.58
8 7 -2 15.87 1.37
8 7 -2 17.57 1.38
8 -7 1 52.36 2.69
8 7 -1 53.86 2.68
8 -7 1 48.92 2.79
-8 7 1 54.59 2.98
8 -7 1 50.84 2.63
8 7 -1 53.02 2.66
8 7 0 103.11 4.14
-8 7 0 91.93 4.19
8 -7 0 97.47 4.27
8 -7 0 92.17 4.10
8 -7 0 93.19 4.06
-8 7 0 96.18 4.36
8 7 1 55.43 2.73
-8 7 -1 50.14 2.75
8 -7 -1 48.92 2.69
8 -7 -1 49.92 2.57
8 -7 -1 47.92 2.67
8 -7 -1 46.15 2.59
-8 7 -1 57.09 2.93
8 7 2 18.24 1.46
-8 7 -2 15.59 1.37
8 -7 -2 17.75 1.40
8 -7 -2 16.94 1.37
-8 7 -2 20.28 1.58
8 -7 -3 55.43 2.72
8 -7 -3 50.08 2.61
8 -7 -3 54.77 2.78
-8 -7 3 53.38 2.77
8 7 3 60.14 2.82
-8 7 -3 55.29 2.71
8 7 3 50.58 2.36
8 -7 -3 49.70 2.46
-8 7 -3 51.22 2.67
8 -7 -4 22.04 1.57
8 7 4 22.63 1.66
-8 -7 4 22.39 1.60
8 -7 -4 22.88 1.55
-8 7 -4 22.57 1.44
8 7 4 20.49 1.34
8 7 5 24.51 1.66
-8 -7 5 27.13 1.66
8 7 5 23.47 1.38
8 -7 -5 25.43 1.58
8 -7 -5 24.05 1.57
8 7 6 27.83 1.69
8 -7 -6 26.79 1.55
8 -7 -6 29.98 1.58
8 7 6 24.95 1.40
-8 -7 6 27.44 1.57
8 -7 -7 118.57 4.02
8 8 -6 85.22 3.16
8 8 -6 78.02 3.11
-8 8 6 88.81 3.27
8 8 -5 23.85 1.22
-8 8 5 25.47 1.53
8 -8 4 11.67 1.05
8 8 -4 12.36 0.90
8 8 -4 12.08 1.02
8 8 -3 19.20 1.24
8 8 -3 17.59 1.30
8 8 -2 349.35 9.88
-8 8 2 338.54 10.22
8 -8 2 344.58 10.13
8 8 -2 340.51 9.69
8 8 -1 31.16 1.75
8 8 -1 25.29 1.54
-8 8 1 30.64 1.88
8 -8 1 31.68 1.95
-8 8 1 34.35 2.08
8 -8 1 29.94 1.74
8 8 0 3.55 0.65
8 8 0 3.10 0.56
-8 8 0 3.45 0.65
8 -8 0 4.04 0.66
8 -8 0 3.03 0.64
-8 8 0 3.62 0.77
8 -8 0 3.42 0.65
-8 -8 1 30.62 1.85
8 8 1 32.65 1.83
8 8 1 30.33 1.79
-8 8 -1 28.26 1.85
8 -8 -1 31.14 1.86
8 -8 -1 32.21 1.89
-8 8 -1 29.93 1.93
-8 -8 2 303.88 10.51
8 8 2 344.50 10.63
8 8 2 334.18 10.67
-8 8 -2 323.65 10.68
8 -8 -2 324.97 10.53
-8 8 -2 338.56 10.79
8 -8 -2 317.32 10.47
8 -8 -3 15.71 1.20
8 8 3 17.91 1.32
-8 -8 3 19.01 1.30
8 -8 -3 16.16 1.10
8 -8 -3 17.64 1.27
-8 8 -3 16.10 1.26
-8 -8 4 10.36 0.91
-8 8 -4 9.60 0.82
8 -8 -4 12.09 1.03
8 -8 -4 12.33 0.98
8 8 4 11.94 1.04
8 8 5 27.86 1.53
8 -8 -5 25.15 1.43
8 -8 -6 79.37 2.98
8 -8 -6 74.30 2.90
-8 9 5 32.46 1.54
-8 9 4 14.20 1.03
8 9 -4 17.70 1.05
8 9 -3 17.64 1.11
8 9 -2 6.11 0.57
-8 9 2 6.65 0.81
8 -9 2 7.03 0.78
8 9 -1 9.02 0.74
8 -9 1 10.13 0.82
-8 9 1 10.39 0.99
8 -9 1 10.79 0.96
8 -9 0 1.58 0.42
-8 -9 0 0.75 0.27
8 9 0 1.22 0.37
8 -9 0 1.94 0.48
-8 9 0 1.48 0.51
8 -9 -1 9.96 0.85
-8 9 -1 8.99 0.91
8 -9 -1 9.78 0.85
8 -9 -2 6.84 0.72
8 -9 -2 5.96 0.62
-8 9 -2 6.48 0.76
8 -9 -2 6.10 0.69
8 9 2 5.08 0.56
-8 9 -3 14.82 1.03
8 -9 -3 17.63 1.12
8 9 3 17.11 1.04
8 -9 -4 14.69 0.98
8 9 4 13.61 0.89
8 -9 -5 32.90 1.46
8 -10 2 120.90 4.10
-8 10 1 0.95 0.31
8 -10 1 0.66 0.25
8 -10 0 7.91 0.64
8 -10 0 7.17 0.59
-8 10 -1 0.47 0.26
9 0 0 0.22 0.38
-9 0 0 -0.13 0.27
-9 0 -1 0.95 0.37
-9 0 1 0.31 0.36
9 0 2 20.03 1.39
9 0 3 1.36 0.45
9 0 4 24.22 1.47
9 0 5 0.08 0.29
9 0 6 12.02 0.84
9 -1 6 170.79 5.56
9 -1 5 4.83 0.59
9 -1 5 5.19 0.59
9 -1 4 22.01 1.41
9 -1 4 23.16 1.39
9 -1 3 35.67 1.89
-9 1 3 36.07 1.90
9 -1 2 143.85 5.10
-9 1 2 133.63 4.97
9 -1 1 7.47 0.84
-9 -1 -1 7.47 0.88
-9 1 1 5.65 0.78
9 -1 1 7.41 0.81
-9 1 1 6.92 0.73
-9 -1 0 7.71 0.90
-9 1 0 7.67 0.90
9 1 0 9.37 0.94
-9 -1 1 7.21 0.86
-9 1 -1 7.16 0.86
9 1 1 9.00 0.92
9 1 1 9.07 0.92
9 1 2 149.18 5.36
9 1 2 145.46 5.36
9 1 3 41.03 2.08
9 1 3 40.13 2.05
9 1 3 39.88 2.13
9 1 4 24.43 1.44
9 1 4 24.12 1.43
9 1 4 20.52 1.43
9 1 5 6.38 0.68
9 1 5 5.85 0.65
9 1 6 174.72 5.70
9 2 -6 1.08 0.27
9 -2 5 29.90 1.49
9 -2 5 34.24 1.56
9 2 -5 29.93 1.42
9 -2 4 78.57 3.04
-9 2 4 76.35 3.16
9 -2 4 79.26 3.07
9 2 -4 82.96 2.97
9 -2 3 40.57 1.99
-9 2 3 40.11 2.06
9 -2 3 42.66 2.03
9 2 -3 41.61 1.92
9 -2 2 4.27 0.62
-9 2 2 4.32 0.66
9 -2 2 5.21 0.68
9 2 -2 5.10 0.64
9 -2 1 5.16 0.67
-9 2 1 5.03 0.65
9 -2 1 5.58 0.69
9 2 -1 3.89 0.65
9 2 -1 4.76 0.63
9 2 0 133.44 4.46
9 -2 0 128.92 4.40
-9 -2 1 4.91 0.71
9 2 1 4.33 0.65
9 -2 -1 5.20 0.68
9 2 1 5.69 0.73
-9 -2 2 5.12 0.72
9 2 2 5.11 0.68
9 2 2 5.81 0.73
9 2 3 45.24 2.13
-9 -2 3 38.37 2.07
9 2 3 44.01 2.10
9 2 3 45.24 2.21
9 2 4 78.62 3.10
9 2 4 80.75 3.11
-9 -2 4 72.24 3.04
9 2 4 79.76 3.21
9 2 5 31.84 1.57
9 2 5 34.22 1.59
9 2 5 34.53 1.68
9 2 6 1.14 0.26
9 3 -5 5.24 0.54
9 3 -5 4.82 0.49
9 3 -4 17.71 1.07
-9 3 4 17.63 1.20
9 3 -3 0.47 0.31
-9 3 3 0.39 0.36
9 3 -2 24.12 1.33
9 3 -2 23.15 1.35
-9 3 2 21.06 1.40
9 -3 1 9.65 0.83
9 3 -1 10.78 0.88
9 3 -1 9.22 0.86
-9 3 1 8.64 0.84
9 3 0 9.36 0.83
9 3 0 9.16 0.85
9 -3 0 9.00 0.80
9 3 0 9.05 0.85
-9 3 0 7.14 0.71
9 3 0 8.37 0.79
9 3 1 10.54 0.91
9 3 1 10.19 0.89
9 3 1 10.52 0.88
-9 -3 1 9.09 0.95
9 -3 -1 10.81 0.87
9 3 1 9.41 0.87
9 3 2 20.20 1.27
9 3 2 20.07 1.33
-9 -3 2 19.53 1.37
9 3 2 20.74 1.28
9 3 2 24.02 1.35
9 3 3 0.48 0.29
9 3 3 0.36 0.28
-9 -3 3 0.67 0.34
9 3 3 0.23 0.30
9 3 4 14.88 1.05
9 3 4 17.59 1.11
9 3 4 15.58 0.98
-9 -3 4 15.13 1.07
9 3 4 14.86 0.99
-9 -3 5 4.35 0.50
9 3 5 4.62 0.51
-9 4 4 92.16 3.44
-9 4 3 67.85 2.74
9 4 -3 61.16 2.58
9 4 -2 5.58 0.54
9 4 -2 5.08 0.50
-9 4 2 6.24 0.69
9 4 -1 12.65 0.88
9 4 -1 13.31 0.86
9 4 -1 14.96 1.03
-9 4 1 12.30 0.99
9 4 0 77.14 2.82
9 4 0 73.58 2.74
9 4 0 81.77 3.03
9 4 1 12.16 0.86
9 4 1 12.77 0.85
9 4 1 14.48 1.02
9 4 2 5.75 0.56
9 4 2 4.57 0.52
9 4 2 5.37 0.53
9 4 2 6.37 0.67
9 4 3 57.14 2.30
9 4 4 78.51 3.00
-9 5 3 8.26 0.70
9 5 -3 9.69 0.69
9 5 -3 7.42 0.61
-9 5 2 1.85 0.37
9 5 -2 1.32 0.34
-9 5 1 18.31 1.10
-9 -5 0 13.29 1.00
-9 -5 1 20.76 1.28
9 5 2 1.17 0.34
-9 -5 2 1.41 0.36
9 5 3 7.74 0.68
-9 -5 3 8.35 0.70
9 6 0 5.09 0.50
0 0 0 0.00 0.00
TITL 23SAI_R067_g in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 7.451189 14.779900 15.891199 90.0000 90.0000 90.0000
ZERR 8.00 0.000054 0.000119 0.000111 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 88.00 80.00 8.00 8.00
REM CrysAlisPro recorded range (K): Min=99.7; max=100.2; aver:99.9
TEMP -173
SIZE 0.17 0.24 0.41
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 41604
_shelx_res_file
;
TITL 23sai_r067_g_a.res in P2(1)2(1)2(1)
23sai_r067_g.res
created by SHELXL-2018/3 at 17:29:42 on 25-Sep-2023
REM Old TITL 23SAI_R067_g in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.068, Rweak 0.021, Alpha 0.001, Orientation as input
REM Flack x = 0.462 ( 0.004 ) from Parsons' quotients
REM Formula found by SHELXT: C18 N4 Cl2
CELL 1.54184 7.45119 14.7799 15.8912 90 90 90
ZERR 8 0.0005 0.00012 0.00011 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N S
UNIT 72 80 16 8
EQIV $1 1+X,+Y,+Z
EQIV $2 -1+X,+Y,+Z
L.S. 11
PLAN 6
SIZE 0.17 0.24 0.41
TEMP -173
CONF
HTAB N1B S2A_$1
HTAB N1A S2B_$2
BOND $H
list 4
MORE -1
fmap 2 53
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.035900 0.585300
EXTI 0.000978
BASF 0.45417
FVAR 0.52870
S2A 4 -0.222036 0.213634 0.892505 11.00000 0.02179 0.02432 =
0.01827 0.00069 0.00212 0.00626
N1A 3 -0.047923 0.197218 0.742475 11.00000 0.01827 0.02051 =
0.01728 0.00065 -0.00011 0.00425
N3A 3 0.112308 0.154277 0.850656 11.00000 0.01845 0.01532 =
0.01815 -0.00044 -0.00098 0.00050
C2A 1 -0.050587 0.188415 0.827393 11.00000 0.02014 0.01452 =
0.01984 -0.00110 -0.00139 0.00090
C4A 1 0.218118 0.141324 0.779411 11.00000 0.01848 0.01279 =
0.02172 -0.00085 -0.00055 -0.00102
C5A 1 0.390901 0.107299 0.769779 11.00000 0.01839 0.01873 =
0.02815 0.00152 -0.00209 0.00072
AFIX 43
H5A 2 0.459639 0.087262 0.816552 11.00000 -1.20000
AFIX 0
C6A 1 0.457862 0.104117 0.688180 11.00000 0.01933 0.02019 =
0.03541 -0.00046 0.00509 0.00219
AFIX 43
H6A 2 0.575684 0.081670 0.678910 11.00000 -1.20000
AFIX 0
C7A 1 0.355605 0.133260 0.619214 11.00000 0.02537 0.01954 =
0.02531 -0.00024 0.00660 -0.00118
AFIX 43
H7A 2 0.405983 0.130237 0.564370 11.00000 -1.20000
AFIX 0
C8A 1 0.182607 0.166408 0.629134 11.00000 0.02393 0.01926 =
0.02217 0.00116 0.00143 0.00036
AFIX 43
H8A 2 0.112969 0.185807 0.582421 11.00000 -1.20000
AFIX 0
C9A 1 0.116435 0.169796 0.710739 11.00000 0.01791 0.01427 =
0.02190 -0.00123 0.00032 0.00054
C10A 1 0.173491 0.145563 0.937912 11.00000 0.02324 0.02105 =
0.01935 -0.00044 -0.00583 -0.00033
AFIX 23
H10A 2 0.117518 0.193980 0.972037 11.00000 -1.20000
H10B 2 0.305098 0.154553 0.939713 11.00000 -1.20000
AFIX 0
C11A 1 0.128978 0.054715 0.976974 11.00000 0.02754 0.02255 =
0.02412 0.00221 -0.00208 0.00196
AFIX 137
H11A 2 0.182860 0.006293 0.943261 11.00000 -1.50000
H11B 2 -0.001560 0.046798 0.978545 11.00000 -1.50000
H11C 2 0.176860 0.052327 1.034369 11.00000 -1.50000
AFIX 0
S2B 4 0.712478 0.327084 0.619942 11.00000 0.01998 0.02526 =
0.02224 0.00493 0.00136 0.00355
N1B 3 0.520631 0.336992 0.765709 11.00000 0.01962 0.02053 =
0.02026 0.00333 -0.00149 0.00351
N3B 3 0.394138 0.406864 0.659961 11.00000 0.01902 0.01643 =
0.02101 0.00151 -0.00314 0.00116
C2B 1 0.541081 0.357615 0.683202 11.00000 0.01849 0.01522 =
0.02287 0.00174 -0.00457 0.00001
C4B 1 0.276828 0.414203 0.727782 11.00000 0.02017 0.01444 =
0.02211 0.00066 -0.00164 -0.00139
C5B 1 0.107914 0.453424 0.735435 11.00000 0.02195 0.01744 =
0.02939 0.00101 -0.00336 0.00269
AFIX 43
H5B 2 0.051416 0.482733 0.689295 11.00000 -1.20000
AFIX 0
C6B 1 0.025774 0.447724 0.813671 11.00000 0.02351 0.01920 =
0.03513 -0.00189 0.00341 0.00303
AFIX 43
H6B 2 -0.089939 0.473475 0.821187 11.00000 -1.20000
AFIX 0
C7B 1 0.109408 0.404961 0.881663 11.00000 0.02876 0.01913 =
0.02635 -0.00245 0.00458 -0.00144
AFIX 43
H7B 2 0.049496 0.402837 0.934396 11.00000 -1.20000
AFIX 0
C8B 1 0.277741 0.365527 0.874093 11.00000 0.02609 0.01741 =
0.02187 0.00088 -0.00058 -0.00171
AFIX 43
H8B 2 0.334784 0.336867 0.920438 11.00000 -1.20000
AFIX 0
C9B 1 0.358706 0.370007 0.795481 11.00000 0.01968 0.01436 =
0.02314 -0.00028 -0.00170 -0.00076
C10B 1 0.365440 0.444312 0.576016 11.00000 0.02204 0.01878 =
0.02057 0.00437 -0.00371 -0.00046
AFIX 23
H10C 2 0.483111 0.454711 0.548751 11.00000 -1.20000
H10D 2 0.304031 0.503466 0.581024 11.00000 -1.20000
AFIX 0
C11B 1 0.253806 0.382011 0.521244 11.00000 0.02859 0.02588 =
0.02413 0.00006 -0.00660 -0.00328
AFIX 137
H11D 2 0.238632 0.409231 0.465462 11.00000 -1.50000
H11E 2 0.135862 0.372960 0.547203 11.00000 -1.50000
H11F 2 0.314744 0.323560 0.515652 11.00000 -1.50000
AFIX 0
H1B 2 0.595855 0.308172 0.794555 11.00000 0.03443
H1A 2 -0.129702 0.225299 0.712527 11.00000 0.03175
HKLF 4
REM 23sai_r067_g_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0690, GooF = S = 1.063, Restrained GooF = 1.063 for all data
REM R1 = 0.0257 for 3779 Fo > 4sig(Fo) and 0.0258 for all 3799 data
REM 229 parameters refined using 0 restraints
END
WGHT 0.0359 0.5853
REM Highest difference peak 0.247, deepest hole -0.210, 1-sigma level 0.041
Q1 1 0.1748 0.1612 0.7423 11.00000 0.05 0.25
Q2 1 -0.1568 0.1980 0.8426 11.00000 0.05 0.22
Q3 1 0.6347 0.3421 0.6618 11.00000 0.05 0.22
Q4 1 0.3986 0.1183 0.6596 11.00000 0.05 0.21
Q5 1 0.3037 0.3846 0.7577 11.00000 0.05 0.21
Q6 1 0.0318 0.1780 0.8456 11.00000 0.05 0.21
;
_shelx_res_checksum 12165
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -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 S2A -0.22204(7) 0.21363(3) 0.89250(3) 0.02146(13) Uani d 1 . .
N N1A -0.0479(2) 0.19722(11) 0.74247(10) 0.0187(3) Uani d 1 . .
N N3A 0.1123(2) 0.15428(11) 0.85066(10) 0.0173(3) Uani d 1 . .
C C2A -0.0506(3) 0.18841(13) 0.82739(12) 0.0182(4) Uani d 1 . .
C C4A 0.2181(3) 0.14132(12) 0.77941(12) 0.0177(4) Uani d 1 . .
C C5A 0.3909(3) 0.10730(14) 0.76978(14) 0.0218(4) Uani d 1 . .
H H5A 0.459639 0.087262 0.816552 0.026 Uiso calc 1 . .
C C6A 0.4579(3) 0.10412(14) 0.68818(15) 0.0250(4) Uani d 1 . .
H H6A 0.575684 0.081670 0.678910 0.030 Uiso calc 1 . .
C C7A 0.3556(3) 0.13326(14) 0.61921(14) 0.0234(4) Uani d 1 . .
H H7A 0.405983 0.130237 0.564370 0.028 Uiso calc 1 . .
C C8A 0.1826(3) 0.16641(14) 0.62913(13) 0.0218(4) Uani d 1 . .
H H8A 0.112969 0.185807 0.582421 0.026 Uiso calc 1 . .
C C9A 0.1164(3) 0.16980(13) 0.71074(13) 0.0180(4) Uani d 1 . .
C C10A 0.1735(3) 0.14556(14) 0.93791(13) 0.0212(4) Uani d 1 . .
H H10A 0.117518 0.193980 0.972037 0.025 Uiso calc 1 . .
H H10B 0.305098 0.154553 0.939713 0.025 Uiso calc 1 . .
C C11A 0.1290(3) 0.05472(14) 0.97697(14) 0.0247(4) Uani d 1 . .
H H11A 0.182860 0.006293 0.943261 0.037 Uiso calc 1 . .
H H11B -0.001560 0.046798 0.978545 0.037 Uiso calc 1 . .
H H11C 0.176860 0.052327 1.034369 0.037 Uiso calc 1 . .
S S2B 0.71248(7) 0.32708(3) 0.61994(3) 0.02249(13) Uani d 1 . .
N N1B 0.5206(2) 0.33699(12) 0.76571(11) 0.0201(3) Uani d 1 . .
N N3B 0.3941(2) 0.40686(11) 0.65996(11) 0.0188(3) Uani d 1 . .
C C2B 0.5411(3) 0.35762(13) 0.68320(13) 0.0189(4) Uani d 1 . .
C C4B 0.2768(3) 0.41420(13) 0.72778(12) 0.0189(4) Uani d 1 . .
C C5B 0.1079(3) 0.45342(14) 0.73544(14) 0.0229(4) Uani d 1 . .
H H5B 0.051416 0.482733 0.689295 0.028 Uiso calc 1 . .
C C6B 0.0258(3) 0.44772(14) 0.81367(15) 0.0259(4) Uani d 1 . .
H H6B -0.089939 0.473475 0.821187 0.031 Uiso calc 1 . .
C C7B 0.1094(3) 0.40496(14) 0.88166(14) 0.0247(4) Uani d 1 . .
H H7B 0.049496 0.402837 0.934396 0.030 Uiso calc 1 . .
C C8B 0.2777(3) 0.36553(13) 0.87409(13) 0.0218(4) Uani d 1 . .
H H8B 0.334784 0.336867 0.920438 0.026 Uiso calc 1 . .
C C9B 0.3587(3) 0.37001(13) 0.79548(13) 0.0191(4) Uani d 1 . .
C C10B 0.3654(3) 0.44431(14) 0.57602(13) 0.0205(4) Uani d 1 . .
H H10C 0.483111 0.454711 0.548751 0.025 Uiso calc 1 . .
H H10D 0.304031 0.503466 0.581024 0.025 Uiso calc 1 . .
C C11B 0.2538(3) 0.38201(15) 0.52124(13) 0.0262(5) Uani d 1 . .
H H11D 0.238632 0.409231 0.465462 0.039 Uiso calc 1 . .
H H11E 0.135862 0.372960 0.547203 0.039 Uiso calc 1 . .
H H11F 0.314744 0.323560 0.515652 0.039 Uiso calc 1 . .
H H1B 0.596(4) 0.308(2) 0.7946(19) 0.034(8) Uiso d 1 . .
H H1A -0.130(4) 0.225(2) 0.7125(19) 0.032(7) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S2A 0.0218(2) 0.0243(2) 0.0183(2) 0.00626(19) 0.00212(18) 0.00069(17)
N1A 0.0183(8) 0.0205(8) 0.0173(8) 0.0042(7) -0.0001(6) 0.0007(6)
N3A 0.0185(8) 0.0153(7) 0.0181(8) 0.0005(6) -0.0010(6) -0.0004(6)
C2A 0.0201(9) 0.0145(8) 0.0198(9) 0.0009(7) -0.0014(8) -0.0011(7)
C4A 0.0185(9) 0.0128(8) 0.0217(9) -0.0010(7) -0.0005(8) -0.0008(7)
C5A 0.0184(9) 0.0187(9) 0.0282(10) 0.0007(8) -0.0021(8) 0.0015(8)
C6A 0.0193(9) 0.0202(10) 0.0354(12) 0.0022(8) 0.0051(9) -0.0005(8)
C7A 0.0254(10) 0.0195(9) 0.0253(10) -0.0012(8) 0.0066(9) -0.0002(8)
C8A 0.0239(10) 0.0193(9) 0.0222(9) 0.0004(8) 0.0014(8) 0.0012(7)
C9A 0.0179(9) 0.0143(8) 0.0219(9) 0.0005(7) 0.0003(7) -0.0012(7)
C10A 0.0232(10) 0.0211(9) 0.0193(9) -0.0003(8) -0.0058(8) -0.0004(7)
C11A 0.0275(11) 0.0226(10) 0.0241(10) 0.0020(9) -0.0021(9) 0.0022(8)
S2B 0.0200(2) 0.0253(2) 0.0222(2) 0.00355(19) 0.00136(18) 0.00493(18)
N1B 0.0196(8) 0.0205(8) 0.0203(8) 0.0035(7) -0.0015(7) 0.0033(6)
N3B 0.0190(7) 0.0164(7) 0.0210(8) 0.0012(6) -0.0031(7) 0.0015(6)
C2B 0.0185(9) 0.0152(8) 0.0229(9) 0.0000(7) -0.0046(8) 0.0017(7)
C4B 0.0202(9) 0.0144(8) 0.0221(9) -0.0014(8) -0.0016(8) 0.0007(7)
C5B 0.0220(10) 0.0174(9) 0.0294(11) 0.0027(8) -0.0034(9) 0.0010(8)
C6B 0.0235(10) 0.0192(9) 0.0351(12) 0.0030(8) 0.0034(9) -0.0019(8)
C7B 0.0288(10) 0.0191(9) 0.0263(10) -0.0014(8) 0.0046(9) -0.0025(8)
C8B 0.0261(10) 0.0174(9) 0.0219(9) -0.0017(8) -0.0006(8) 0.0009(7)
C9B 0.0197(9) 0.0144(8) 0.0231(9) -0.0008(7) -0.0017(8) -0.0003(7)
C10B 0.0220(9) 0.0188(9) 0.0206(9) -0.0005(8) -0.0037(8) 0.0044(7)
C11B 0.0286(11) 0.0259(10) 0.0241(10) -0.0033(9) -0.0066(9) 0.0001(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'
N N 0.0311 0.0180 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.1103
-1 -1 0 0.1140
-1 1 0 0.1006
1 -1 0 0.1103
0 0 1 0.2486
0 0 -1 0.1614
0 1 0 0.0812
0 -1 0 0.0896
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
C2A N1A C9A . . 110.32(17) ?
C2A N1A H1A . . 125.1(19) ?
C9A N1A H1A . . 123.7(19) ?
C2A N3A C4A . . 109.50(16) ?
C2A N3A C10A . . 124.42(16) ?
C4A N3A C10A . . 125.52(17) ?
N1A C2A S2A . . 126.93(16) ?
N1A C2A N3A . . 106.97(17) ?
N3A C2A S2A . . 126.10(15) ?
N3A C4A C9A . . 106.69(17) ?
C5A C4A N3A . . 131.55(19) ?
C5A C4A C9A . . 121.76(19) ?
C4A C5A H5A . . 121.7 ?
C6A C5A C4A . . 116.6(2) ?
C6A C5A H5A . . 121.7 ?
C5A C6A H6A . . 119.2 ?
C5A C6A C7A . . 121.6(2) ?
C7A C6A H6A . . 119.2 ?
C6A C7A H7A . . 119.2 ?
C8A C7A C6A . . 121.6(2) ?
C8A C7A H7A . . 119.2 ?
C7A C8A H8A . . 121.7 ?
C7A C8A C9A . . 116.66(19) ?
C9A C8A H8A . . 121.7 ?
N1A C9A C4A . . 106.50(17) ?
N1A C9A C8A . . 131.66(19) ?
C8A C9A C4A . . 121.84(18) ?
N3A C10A H10A . . 108.9 ?
N3A C10A H10B . . 108.9 ?
N3A C10A C11A . . 113.41(17) ?
H10A C10A H10B . . 107.7 ?
C11A C10A H10A . . 108.9 ?
C11A C10A H10B . . 108.9 ?
C10A C11A H11A . . 109.5 ?
C10A C11A H11B . . 109.5 ?
C10A C11A H11C . . 109.5 ?
H11A C11A H11B . . 109.5 ?
H11A C11A H11C . . 109.5 ?
H11B C11A H11C . . 109.5 ?
C2B N1B C9B . . 110.45(17) ?
C2B N1B H1B . . 125(2) ?
C9B N1B H1B . . 125(2) ?
C2B N3B C4B . . 109.61(16) ?
C2B N3B C10B . . 124.51(18) ?
C4B N3B C10B . . 125.87(17) ?
N1B C2B S2B . . 127.00(15) ?
N1B C2B N3B . . 106.95(18) ?
N3B C2B S2B . . 126.05(16) ?
N3B C4B C9B . . 106.57(17) ?
C5B C4B N3B . . 131.94(19) ?
C5B C4B C9B . . 121.5(2) ?
C4B C5B H5B . . 121.6 ?
C6B C5B C4B . . 116.9(2) ?
C6B C5B H5B . . 121.6 ?
C5B C6B H6B . . 119.2 ?
C5B C6B C7B . . 121.5(2) ?
C7B C6B H6B . . 119.2 ?
C6B C7B H7B . . 119.2 ?
C8B C7B C6B . . 121.7(2) ?
C8B C7B H7B . . 119.2 ?
C7B C8B H8B . . 121.6 ?
C7B C8B C9B . . 116.77(19) ?
C9B C8B H8B . . 121.6 ?
N1B C9B C4B . . 106.37(18) ?
N1B C9B C8B . . 131.99(19) ?
C8B C9B C4B . . 121.64(19) ?
N3B C10B H10C . . 109.2 ?
N3B C10B H10D . . 109.2 ?
N3B C10B C11B . . 112.01(17) ?
H10C C10B H10D . . 107.9 ?
C11B C10B H10C . . 109.2 ?
C11B C10B H10D . . 109.2 ?
C10B C11B H11D . . 109.5 ?
C10B C11B H11E . . 109.5 ?
C10B C11B H11F . . 109.5 ?
H11D C11B H11E . . 109.5 ?
H11D C11B H11F . . 109.5 ?
H11E C11B H11F . . 109.5 ?
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
S2A C2A . 1.686(2) ?
N1A C2A . 1.356(3) ?
N1A C9A . 1.385(3) ?
N1A H1A . 0.88(3) ?
N3A C2A . 1.365(3) ?
N3A C4A . 1.393(3) ?
N3A C10A . 1.465(2) ?
C4A C5A . 1.391(3) ?
C4A C9A . 1.394(3) ?
C5A H5A . 0.9500 ?
C5A C6A . 1.390(3) ?
C6A H6A . 0.9500 ?
C6A C7A . 1.403(3) ?
C7A H7A . 0.9500 ?
C7A C8A . 1.388(3) ?
C8A H8A . 0.9500 ?
C8A C9A . 1.388(3) ?
C10A H10A . 0.9900 ?
C10A H10B . 0.9900 ?
C10A C11A . 1.516(3) ?
C11A H11A . 0.9800 ?
C11A H11B . 0.9800 ?
C11A H11C . 0.9800 ?
S2B C2B . 1.687(2) ?
N1B C2B . 1.355(3) ?
N1B C9B . 1.385(3) ?
N1B H1B . 0.84(3) ?
N3B C2B . 1.366(3) ?
N3B C4B . 1.392(3) ?
N3B C10B . 1.460(2) ?
C4B C5B . 1.391(3) ?
C4B C9B . 1.399(3) ?
C5B H5B . 0.9500 ?
C5B C6B . 1.388(3) ?
C6B H6B . 0.9500 ?
C6B C7B . 1.398(3) ?
C7B H7B . 0.9500 ?
C7B C8B . 1.388(3) ?
C8B H8B . 0.9500 ?
C8B C9B . 1.389(3) ?
C10B H10C . 0.9900 ?
C10B H10D . 0.9900 ?
C10B C11B . 1.516(3) ?
C11B H11D . 0.9800 ?
C11B H11E . 0.9800 ?
C11B H11F . 0.9800 ?
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
N1B H1B S2A 1_655 0.84(3) 2.49(3) 3.3258(18) 171(3) yes
N1A H1A S2B 1_455 0.88(3) 2.41(3) 3.2654(18) 165(3) yes
C6B H6B Cg3 4_645 0.95 2.85 3.6470(17) 143 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
N3A C4A C5A C6A . . . . -179.6(2) ?
N3A C4A C9A N1A . . . . -1.1(2) ?
N3A C4A C9A C8A . . . . 179.75(18) ?
C2A N1A C9A C4A . . . . 1.1(2) ?
C2A N1A C9A C8A . . . . -179.9(2) ?
C2A N3A C4A C5A . . . . -178.9(2) ?
C2A N3A C4A C9A . . . . 0.8(2) ?
C2A N3A C10A C11A . . . . 91.4(2) ?
C4A N3A C2A S2A . . . . 179.34(14) ?
C4A N3A C2A N1A . . . . -0.2(2) ?
C4A N3A C10A C11A . . . . -98.0(2) ?
C4A C5A C6A C7A . . . . -0.4(3) ?
C5A C4A C9A N1A . . . . 178.60(17) ?
C5A C4A C9A C8A . . . . -0.5(3) ?
C5A C6A C7A C8A . . . . -0.2(3) ?
C6A C7A C8A C9A . . . . 0.4(3) ?
C7A C8A C9A N1A . . . . -178.9(2) ?
C7A C8A C9A C4A . . . . -0.1(3) ?
C9A N1A C2A S2A . . . . 179.93(14) ?
C9A N1A C2A N3A . . . . -0.6(2) ?
C9A C4A C5A C6A . . . . 0.7(3) ?
C10A N3A C2A S2A . . . . -8.8(3) ?
C10A N3A C2A N1A . . . . 171.69(17) ?
C10A N3A C4A C5A . . . . 9.4(3) ?
C10A N3A C4A C9A . . . . -170.92(17) ?
N3B C4B C5B C6B . . . . 179.4(2) ?
N3B C4B C9B N1B . . . . -0.7(2) ?
N3B C4B C9B C8B . . . . 179.23(18) ?
C2B N1B C9B C4B . . . . -0.8(2) ?
C2B N1B C9B C8B . . . . 179.3(2) ?
C2B N3B C4B C5B . . . . -176.8(2) ?
C2B N3B C4B C9B . . . . 1.9(2) ?
C2B N3B C10B C11B . . . . 94.4(2) ?
C4B N3B C2B S2B . . . . 176.59(15) ?
C4B N3B C2B N1B . . . . -2.3(2) ?
C4B N3B C10B C11B . . . . -84.5(2) ?
C4B C5B C6B C7B . . . . 0.3(3) ?
C5B C4B C9B N1B . . . . 178.17(18) ?
C5B C4B C9B C8B . . . . -1.9(3) ?
C5B C6B C7B C8B . . . . -0.5(3) ?
C6B C7B C8B C9B . . . . -0.5(3) ?
C7B C8B C9B N1B . . . . -178.5(2) ?
C7B C8B C9B C4B . . . . 1.7(3) ?
C9B N1B C2B S2B . . . . -176.99(15) ?
C9B N1B C2B N3B . . . . 1.9(2) ?
C9B C4B C5B C6B . . . . 0.9(3) ?
C10B N3B C2B S2B . . . . -2.5(3) ?
C10B N3B C2B N1B . . . . 178.59(18) ?
C10B N3B C4B C5B . . . . 2.3(3) ?
C10B N3B C4B C9B . . . . -179.08(18) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.546(16)
2 0.454(16)