#------------------------------------------------------------------------------
#$Date: 2019-04-19 05:23:08 +0300 (Fri, 19 Apr 2019) $
#$Revision: 214703 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/29/2242909.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_2242909
loop_
_publ_author_name
'Samb, Issa'
'Gaye, Nango'
'Sylla-Gueye, Rokhaya'
'Thiam, Elhadj Ibrahima'
'Gaye, Mohamed'
'Retailleau, Pascal'
_publ_section_title
;
Crystal structure of
N,N'-[(ethane-1,2-diyl)bis(azanediylcarbonothioyl)]bis(benzamide)
;
_journal_coeditor_code VM2216
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 642
_journal_page_last 645
_journal_paper_doi 10.1107/S205698901900495X
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C18 H18 N4 O2 S2'
_chemical_formula_moiety 'C18 H18 N4 O2 S2'
_chemical_formula_sum 'C18 H18 N4 O2 S2'
_chemical_formula_weight 386.48
_chemical_name_systematic
;
N,N'-[(Ethane-1,2-diyl)bis(azanediylcarbonothioyl)]bis(benzamide)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 100.978(5)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 11.2250(6)
_cell_length_b 7.2547(5)
_cell_length_c 11.1397(6)
_cell_measurement_reflns_used 3377
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 30.2300
_cell_measurement_theta_min 4.7010
_cell_volume 890.55(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'HPAD Dectris PILATUS3R 200M'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator 'Rigaku MaxFlux mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0396
_diffrn_reflns_av_unetI/netI 0.0492
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 7264
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.023
_diffrn_reflns_theta_min 3.726
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.320
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.51253
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Rigaku OD, 2018)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.441
_exptl_crystal_description prism
_exptl_crystal_F_000 404
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.355
_refine_diff_density_min -0.313
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 124
_refine_ls_number_reflns 2325
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0491
_refine_ls_R_factor_gt 0.0416
_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^)+(0.0683P)^2^+0.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1153
_refine_ls_wR_factor_ref 0.1209
_reflns_number_gt 1942
_reflns_number_total 2328
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2216sup1.cif
_cod_data_source_block I
_cod_database_code 2242909
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
-3 0 0 147.02 7.59
-4 0 0 580.90 29.75
-5 0 0 93.77 4.95
-6 0 0 29.68 1.72
-6 0 0 30.07 1.70
-7 0 0 3.81 0.36
-7 0 0 4.02 0.38
-7 0 0 4.06 0.38
-8 0 0 62.37 3.38
-8 0 0 63.09 3.37
-8 0 0 60.21 3.40
-9 0 0 1.37 0.27
-9 0 0 0.95 0.30
-9 0 0 1.23 0.26
-10 0 0 112.84 6.15
-10 0 0 122.28 6.30
-10 0 0 118.21 6.19
-11 0 0 97.61 5.29
-11 0 0 96.10 5.14
-12 0 0 27.36 1.60
-12 0 0 26.33 1.74
-13 0 0 106.74 5.98
-13 0 0 110.07 5.77
-2 1 0 4.78 0.32
-3 -1 0 284.16 14.71
-3 1 0 289.02 14.66
3 1 0 282.70 14.68
-4 -1 0 31.18 1.75
-4 1 0 30.38 1.69
4 -1 0 32.23 1.66
4 1 0 29.08 1.70
-5 1 0 486.15 25.24
5 -1 0 495.40 25.17
-5 -1 0 482.05 25.27
-5 -1 0 494.66 25.30
-5 1 0 496.41 25.22
-6 -1 0 103.09 5.72
-6 1 0 109.34 5.69
6 -1 0 106.80 5.63
-6 -1 0 110.89 5.78
-6 1 0 110.79 5.71
-7 -1 0 35.92 2.13
-7 1 0 35.88 2.02
-7 -1 0 34.90 2.05
-7 1 0 35.32 2.04
7 1 0 35.90 1.99
8 1 0 70.52 3.84
-8 1 0 73.29 3.91
-8 -1 0 75.68 3.94
-8 -1 0 76.40 4.01
-8 1 0 69.03 3.81
-9 1 0 13.24 0.91
-9 -1 0 13.05 1.02
-9 1 0 13.04 0.81
-9 -1 0 12.51 0.90
-10 1 0 4.89 0.52
-10 1 0 4.80 0.38
-10 -1 0 5.22 0.60
-10 1 0 4.48 0.50
-10 -1 0 5.21 0.51
-11 -1 0 21.90 1.54
-11 1 0 22.42 1.48
-11 -1 0 21.55 1.44
-11 1 0 24.84 1.46
-11 1 0 23.92 1.32
-12 1 0 0.73 0.27
-12 1 0 0.76 0.19
-12 -1 0 0.59 0.32
-12 -1 0 1.48 0.44
-12 1 0 0.89 0.33
-13 -1 0 0.31 0.37
-13 -1 0 0.74 0.49
-13 1 0 -0.05 0.38
0 -2 0 2577.43 129.93
0 2 0 2499.87 129.98
1 -2 0 877.99 44.57
-1 2 0 865.41 44.60
-2 2 0 52.94 2.70
2 -2 0 50.07 2.68
-3 2 0 25.90 1.34
3 -2 0 23.92 1.40
-3 -2 0 23.88 1.46
4 2 0 43.92 2.40
4 -2 0 41.19 2.31
-4 2 0 43.58 2.26
-4 -2 0 45.13 2.44
5 -2 0 217.51 11.05
-5 2 0 221.81 11.12
-5 -2 0 207.91 11.19
5 2 0 200.04 11.14
-5 2 0 216.29 10.99
-6 2 0 232.50 11.34
-6 -2 0 223.41 11.41
6 2 0 205.78 11.35
6 -2 0 215.19 11.25
-7 2 0 13.38 0.85
7 -2 0 12.24 0.76
-7 -2 0 13.81 1.00
-7 2 0 12.02 0.88
-7 -2 0 12.11 0.90
-8 -2 0 0.16 0.24
-8 2 0 0.12 0.24
-8 2 0 0.25 0.20
-8 -2 0 0.32 0.34
-9 2 0 1.25 0.35
-9 -2 0 1.18 0.35
-9 -2 0 1.59 0.44
-9 2 0 1.40 0.13
9 2 0 1.92 0.37
-9 2 0 1.90 0.33
-10 2 0 85.18 4.45
-10 -2 0 76.23 4.47
-10 -2 0 81.74 4.61
10 2 0 83.35 4.42
-11 -2 0 53.74 3.17
-11 2 0 59.36 3.13
11 2 0 55.06 3.06
-11 -2 0 54.65 3.32
-12 -2 0 48.06 2.84
-12 -2 0 48.79 2.99
-12 2 0 50.66 2.76
-12 2 0 47.59 2.83
-13 -2 0 6.61 0.73
-13 -2 0 4.97 0.71
-14 -2 0 6.69 0.87
0 3 0 0.13 0.19
0 -3 0 0.19 0.16
-1 3 0 87.55 4.35
-1 -3 0 81.85 4.31
1 3 0 74.26 4.38
1 -3 0 80.10 4.25
-2 3 0 582.02 28.71
2 -3 0 545.21 28.65
-3 3 0 253.46 12.94
3 -3 0 247.47 13.02
4 -3 0 80.57 4.04
-4 -3 0 66.33 4.05
-4 3 0 76.88 3.95
-5 -3 0 184.05 10.29
-5 3 0 195.69 10.13
5 -3 0 200.27 10.22
5 3 0 211.13 10.36
6 3 0 2.85 0.40
6 -3 0 3.11 0.31
-6 -3 0 3.50 0.42
-6 3 0 3.32 0.24
-7 3 0 18.67 1.03
7 -3 0 19.36 1.11
-7 -3 0 20.56 1.30
7 3 0 19.36 1.29
8 -3 0 12.15 0.79
-8 -3 0 15.92 1.18
8 3 0 14.82 1.01
-8 -3 0 12.68 0.99
9 -3 0 96.47 5.28
-9 3 0 106.06 5.56
-9 -3 0 111.28 5.71
-9 -3 0 103.61 5.53
-10 3 0 0.94 0.40
-10 -3 0 1.13 0.51
-10 -3 0 1.23 0.42
-11 3 0 9.11 0.89
-11 -3 0 8.37 0.94
-11 -3 0 10.10 0.85
11 3 0 10.19 0.83
-12 -3 0 9.85 1.01
12 3 0 10.53 0.82
-12 -3 0 9.95 0.91
-13 -3 0 4.34 0.72
-13 -3 0 3.34 0.59
-14 -3 0 26.12 1.91
0 4 0 1660.10 86.36
0 -4 0 1703.61 86.23
1 -4 0 460.35 24.52
-1 -4 0 497.71 24.60
-1 4 0 485.27 24.66
-2 4 0 5.17 0.50
-2 -4 0 5.19 0.48
2 -4 0 4.98 0.40
-3 4 0 20.37 1.25
-4 4 0 3.88 0.38
4 -4 0 3.96 0.45
-5 -4 0 102.77 5.68
-5 4 0 104.84 5.53
5 -4 0 107.61 5.63
-6 4 0 165.18 8.92
6 -4 0 177.87 9.03
-6 -4 0 171.84 9.14
6 4 0 187.67 9.26
-7 4 0 49.50 2.77
7 -4 0 53.54 2.86
7 4 0 57.40 3.15
-7 -4 0 55.42 3.06
8 -4 0 15.91 0.96
8 4 0 16.93 1.26
-8 -4 0 14.51 1.17
-9 -4 0 13.32 1.03
9 -4 0 11.84 0.75
9 4 0 11.49 1.04
-9 -4 0 12.53 1.16
-10 4 0 7.45 0.82
-10 -4 0 7.55 0.77
-10 -4 0 7.17 0.92
-11 -4 0 36.31 2.34
-11 4 0 39.51 2.43
-11 -4 0 36.16 2.48
-12 4 0 14.28 1.24
-12 -4 0 12.31 1.27
-12 -4 0 16.48 1.24
-13 -4 0 11.73 1.24
-13 -4 0 12.59 1.14
-14 -4 0 4.93 0.92
0 -5 0 -0.21 0.24
-1 -5 0 1.12 0.32
1 -5 0 0.99 0.27
2 -5 0 113.13 6.21
-2 -5 0 129.27 6.35
-2 5 0 116.03 6.36
-3 5 0 27.09 1.77
-3 -5 0 31.94 1.84
-4 5 0 21.11 1.37
4 -5 0 22.57 1.48
5 -5 0 18.52 1.27
-5 5 0 17.98 1.17
6 5 0 92.64 5.03
-6 -5 0 87.96 4.89
6 -5 0 85.67 4.83
7 -5 0 70.18 4.11
-7 -5 0 76.80 4.28
8 5 0 129.60 6.65
-8 -5 0 122.85 6.49
8 -5 0 112.46 6.23
9 5 0 44.27 2.53
9 -5 0 35.47 2.06
-9 -5 0 37.79 2.59
-9 -5 0 39.00 2.39
-10 -5 0 0.61 0.48
10 5 0 0.36 0.43
10 -5 0 0.43 0.17
-10 -5 0 1.05 0.61
-11 5 0 5.24 0.78
-11 -5 0 4.83 0.76
-11 -5 0 5.40 0.93
-12 -5 0 7.64 0.88
-12 -5 0 6.59 1.04
-13 -5 0 10.68 1.26
-13 -5 0 13.84 1.19
0 -6 0 35.72 2.09
1 -6 0 8.65 0.70
-1 -6 0 8.59 0.73
2 -6 0 52.10 2.89
-2 -6 0 52.07 2.99
-3 -6 0 1.21 0.43
-4 -6 0 36.10 2.21
4 -6 0 33.40 2.22
5 -6 0 11.70 1.05
-6 -6 0 13.16 1.06
6 6 0 11.48 1.12
6 -6 0 10.93 1.00
7 -6 0 19.28 1.35
7 6 0 16.86 1.54
-7 -6 0 21.62 1.52
8 -6 0 2.19 0.42
8 6 0 2.82 0.73
-8 -6 0 2.54 0.66
-9 -6 0 11.46 1.10
9 6 0 11.80 1.19
-9 -6 0 10.81 1.19
9 -6 0 8.58 0.68
-10 -6 0 1.14 0.57
-10 -6 0 0.96 0.63
10 6 0 0.36 0.49
-11 -6 0 3.88 0.73
-11 -6 0 4.09 0.91
0 -7 0 0.20 0.31
1 -7 0 0.08 0.33
-1 -7 0 0.31 0.33
2 -7 0 3.09 0.43
-2 -7 0 3.15 0.53
-3 -7 0 9.47 0.87
4 -7 0 4.00 0.68
-4 -7 0 5.76 0.68
5 -7 0 5.43 0.76
6 7 0 -0.09 0.56
6 -7 0 0.07 0.46
7 -7 0 17.97 1.35
7 7 0 17.56 1.58
-7 -7 0 15.64 1.37
8 7 0 59.08 3.60
-8 -7 0 55.84 3.34
8 -7 0 52.10 3.12
-9 -7 0 0.08 0.54
9 7 0 -0.11 0.66
-9 -7 0 0.76 0.64
10 7 0 8.46 1.12
0 -8 0 8.53 0.78
1 -8 0 3.67 0.54
-1 -8 0 2.25 0.50
-2 -8 0 11.57 0.99
-3 -8 0 0.59 0.43
-4 -8 0 -0.06 0.45
4 -8 0 0.08 0.51
-5 -8 0 2.26 0.58
5 -8 0 2.18 0.65
6 8 0 2.85 0.82
6 -8 0 1.72 0.59
7 8 0 0.22 0.80
8 8 0 0.80 0.66
9 8 0 -0.12 0.80
0 -9 0 0.27 0.42
-1 -9 0 -0.40 0.46
-2 -9 0 0.61 0.53
-3 -9 0 4.65 0.73
4 -9 0 0.72 0.55
-13 0 1 0.34 0.34
-13 0 1 0.15 0.37
-12 0 1 -0.19 0.29
-12 0 1 -0.32 0.31
-12 0 1 0.04 0.26
-11 0 1 -0.04 0.30
-11 0 1 -0.16 0.32
-11 0 1 0.22 0.27
-10 0 1 -0.36 0.33
-10 0 1 0.11 0.22
-10 0 1 -0.04 0.27
-9 0 1 1.03 0.28
-9 0 1 0.13 0.40
-8 0 1 -0.03 0.18
-8 0 1 0.08 0.22
-7 0 1 -0.05 0.14
-7 0 1 0.04 0.18
6 0 -1 -0.02 0.13
-6 0 1 0.02 0.11
5 0 -1 0.13 0.11
-5 0 1 0.05 0.08
4 0 -1 0.33 0.11
3 0 -1 0.25 0.11
2 0 1 0.27 0.08
-2 0 -1 0.02 0.02
-2 0 -1 -0.01 0.04
3 0 1 0.18 0.09
-3 0 -1 0.09 0.09
-4 0 -1 0.65 0.11
-4 0 -1 0.43 0.14
4 0 1 0.68 0.15
-5 0 -1 0.41 0.22
-5 0 -1 0.86 0.15
-5 0 -1 0.26 0.11
5 0 1 0.80 0.24
-6 0 -1 0.12 0.09
-6 0 -1 0.04 0.09
-6 0 -1 0.16 0.16
-7 0 -1 0.11 0.20
-7 0 -1 0.20 0.12
-7 0 -1 0.01 0.10
-8 0 -1 0.33 0.26
-8 0 -1 0.24 0.15
-9 0 -1 0.36 0.18
-9 0 -1 0.05 0.28
-10 0 -1 0.08 0.17
-10 0 -1 0.10 0.35
-11 0 -1 0.13 0.17
-11 0 -1 -0.11 0.37
-12 0 -1 0.24 0.38
-12 0 -1 0.07 0.21
-13 0 -1 -0.20 0.39
-13 1 1 30.06 1.86
-13 -1 1 32.43 1.99
-13 1 1 31.97 1.98
-13 1 1 33.65 1.84
-13 -1 1 32.50 2.08
-12 1 1 0.20 0.32
-12 1 1 -0.11 0.21
-12 -1 1 0.31 0.34
-12 -1 1 0.04 0.29
-12 1 1 -0.23 0.27
-11 1 1 0.10 0.25
-11 -1 1 0.39 0.34
-11 1 1 0.18 0.24
-11 -1 1 0.57 0.38
-11 1 1 0.10 0.29
-10 -1 1 5.81 0.61
-10 1 1 5.20 0.46
-10 -1 1 3.96 0.54
-9 -1 1 762.58 40.44
-9 1 1 788.23 40.33
-9 -1 1 788.35 40.46
-9 -1 1 801.31 40.48
9 1 -1 794.93 40.39
-8 -1 1 3.00 0.41
-8 1 1 2.94 0.30
-8 -1 1 2.88 0.39
8 1 -1 2.54 0.35
-7 -1 1 14.61 1.00
7 1 -1 14.15 0.96
-7 1 1 15.48 1.03
-7 1 1 13.47 0.87
-7 -1 1 16.19 1.01
-6 1 1 53.75 3.09
-6 -1 1 51.66 3.08
-6 1 1 58.61 2.96
-5 -1 1 28.47 1.81
-5 1 1 32.96 1.69
-5 1 1 30.86 1.82
-4 -1 1 176.87 9.10
-4 1 1 172.39 9.08
3 1 -1 1474.48 74.24
-3 -1 1 1429.59 74.24
-2 -1 1 11.83 1.38
2 1 -1 2554.43 6.18
1 1 1 134.14 1.10
1 -1 1 149.44 1.37
2 1 1 728.25 32.00
2 -1 1 710.48 32.02
-3 -1 -1 574.23 28.16
-3 1 -1 543.42 28.19
3 -1 1 547.78 28.16
-3 -1 -1 524.05 28.21
3 1 1 550.82 28.17
4 -1 1 935.31 47.98
-4 1 -1 952.98 48.03
-4 -1 -1 913.40 48.07
-4 -1 -1 946.93 47.99
-5 -1 -1 1480.28 75.52
5 -1 1 1470.91 75.51
-5 -1 -1 1487.14 75.62
-5 1 -1 1476.83 75.57
6 -1 1 189.05 10.21
6 1 1 191.12 10.15
-6 -1 -1 189.87 10.35
-6 1 -1 205.18 10.09
-6 1 -1 197.13 10.19
-6 -1 -1 188.59 10.22
-6 1 -1 197.28 10.29
7 1 1 118.32 6.37
-7 -1 -1 120.32 6.45
-7 1 -1 122.80 6.32
-7 1 -1 127.63 6.55
-7 -1 -1 132.10 6.64
7 -1 1 126.34 6.47
-8 1 -1 186.83 9.73
-8 1 -1 186.39 9.97
-8 -1 -1 190.77 9.87
-8 -1 -1 211.70 10.09
-9 1 -1 95.66 4.97
-9 1 -1 92.90 5.22
-9 -1 -1 97.40 5.30
-9 1 -1 99.19 5.10
-9 -1 -1 96.48 5.12
-10 1 -1 14.41 0.80
-10 -1 -1 15.31 0.99
-10 1 -1 14.26 1.07
-10 -1 -1 14.04 1.12
-10 1 -1 13.61 0.88
-11 -1 -1 8.60 0.83
-11 1 -1 8.09 0.76
-11 -1 -1 8.10 0.66
-12 -1 -1 52.32 3.11
-12 1 -1 50.71 3.01
-12 -1 -1 51.08 2.86
-13 1 -1 11.79 1.06
-13 -1 -1 12.73 0.91
-13 -1 -1 13.59 1.21
-14 -2 1 60.10 3.58
-14 -2 1 60.37 3.48
-13 2 1 28.58 1.86
-13 -2 1 25.55 1.87
-13 -2 1 29.52 1.84
-12 -2 1 3.97 0.57
-12 2 1 4.57 0.35
-11 2 1 8.82 0.59
-11 -2 1 7.75 0.81
11 2 -1 7.76 0.70
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4 2 -9 408.05 22.30
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1 3 9 19.49 1.59
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-2 2 15 1.69 0.71
1 2 -15 8.06 1.16
-1 -2 15 6.92 1.02
-1 2 15 7.24 1.14
0 0 0 0.00 0.00
TITL exp_91 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 11.224997 7.254705 11.139704 90.0000 100.9778 90.0000
ZERR 4.00 0.000584 0.000529 0.000565 0.0000 0.0051 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 44.00 40.00 4.00 4.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 901
_shelx_res_file
;
TITL exp_91_a.res in P2(1)/c
exp_91.res
created by SHELXL-2018/3 at 14:59:45 on 18-Oct-2018
REM Old TITL exp_91 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.260, Rweak 0.007, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: C9 N2 O2
CELL 0.71073 11.225 7.2547 11.1397 90 100.978 90
ZERR 2 0.0006 0.0005 0.0006 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O S
UNIT 36 36 8 4 4
OMIT 0 1 7
OMIT 2 1 0
OMIT -4 3 2
DFIX 0.87 N1 HN1 N2 HN2
L.S. 4 0 0
OMIT 7 0 0
PLAN 20
ACTA
CONF
HTAB
BOND $H
list 4
fmap 2 53
REM
REM
REM
WGHT 0.068300 0.122200
FVAR 0.61140
N1 3 0.857362 0.611975 0.419579 11.00000 0.02935 0.05254 =
0.03648 -0.00338 0.00255 0.00510
HN1 2 0.802243 0.635965 0.460581 11.00000 -1.20000
O1 4 0.625650 0.657429 0.432524 11.00000 0.03616 0.06667 =
0.03266 -0.00083 0.00614 0.00381
C1 1 0.983473 0.598928 0.481946 11.00000 0.02879 0.04683 =
0.04052 -0.00518 -0.00134 -0.00304
AFIX 23
H1A 2 0.996007 0.675814 0.554503 11.00000 -1.20000
H1AB 2 1.035920 0.643780 0.428470 11.00000 -1.20000
AFIX 0
S1 5 0.908473 0.530471 0.201898 11.00000 0.03157 0.07975 =
0.04365 -0.00785 0.01212 -0.00179
N2 3 0.695120 0.594941 0.257969 11.00000 0.02742 0.05175 =
0.03164 -0.00139 0.00395 0.00252
HN2 2 0.671075 0.573232 0.182610 11.00000 -1.20000
C2 1 0.820131 0.582341 0.301202 11.00000 0.02822 0.03949 =
0.03706 0.00123 0.00492 -0.00158
C3 1 0.604742 0.627867 0.322615 11.00000 0.02912 0.03731 =
0.03332 0.00363 0.00626 0.00119
C4 1 0.478454 0.619899 0.250547 11.00000 0.02828 0.03382 =
0.03474 0.00274 0.00581 0.00243
C5 1 0.448763 0.651855 0.125431 11.00000 0.03477 0.04275 =
0.03618 0.00528 0.00631 -0.00027
AFIX 43
H5 2 0.508903 0.681492 0.081672 11.00000 -1.20000
AFIX 0
C6 1 0.328488 0.639109 0.066418 11.00000 0.04097 0.04972 =
0.03905 0.00406 -0.00297 0.00264
AFIX 43
H6 2 0.308060 0.662390 -0.017073 11.00000 -1.20000
AFIX 0
C7 1 0.238840 0.592306 0.130134 11.00000 0.02847 0.04897 =
0.05861 0.00055 -0.00092 0.00395
AFIX 43
H7 2 0.158787 0.581443 0.089304 11.00000 -1.20000
AFIX 0
C8 1 0.268088 0.561680 0.254358 11.00000 0.03129 0.05523 =
0.05711 0.00399 0.01553 0.00276
AFIX 43
H8 2 0.207621 0.530909 0.297439 11.00000 -1.20000
REM #####
AFIX 0
C9 1 0.387221 0.576629 0.315072 11.00000 0.03312 0.04859 =
0.03869 0.00484 0.01076 0.00343
AFIX 43
H9 2 0.406519 0.557780 0.399116 11.00000 -1.20000
AFIX 0
HKLF 4
REM exp_91_a.res in P2(1)/c
REM wR2 = 0.1209, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0416 for 1942 Fo > 4sig(Fo) and 0.0491 for all 2325 data
REM 124 parameters refined using 2 restraints
END
WGHT 0.0683 0.1222
REM Instructions for potential hydrogen bonds
HTAB N1 O1
EQIV $2 x, -y+3/2, z+1/2
HTAB C1 S1_$2
REM Highest difference peak 0.355, deepest hole -0.313, 1-sigma level 0.072
Q1 1 0.9004 0.6450 0.2028 11.00000 0.05 0.35
Q2 1 0.6273 0.5802 0.4207 11.00000 0.05 0.29
Q3 1 0.4620 0.6047 0.1820 11.00000 0.05 0.24
Q4 1 0.5404 0.6323 0.2812 11.00000 0.05 0.24
Q5 1 0.3880 0.6297 0.0922 11.00000 0.05 0.23
Q6 1 0.8618 0.5754 0.2547 11.00000 0.05 0.23
Q7 1 0.8402 0.5622 0.3642 11.00000 0.05 0.22
Q8 1 1.0000 0.5000 0.5000 10.50000 0.05 0.22
Q9 1 0.9206 0.6027 0.4509 11.00000 0.05 0.22
Q10 1 0.8478 0.5445 0.2305 11.00000 0.05 0.22
Q11 1 0.3206 0.6381 0.0351 11.00000 0.05 0.21
Q12 1 0.2947 0.5829 0.1007 11.00000 0.05 0.20
Q13 1 0.4388 0.5987 0.2811 11.00000 0.05 0.18
Q14 1 0.6478 0.5938 0.2907 11.00000 0.05 0.18
Q15 1 0.4942 0.7519 0.0655 11.00000 0.05 0.18
Q16 1 0.8836 0.5492 0.1254 11.00000 0.05 0.17
Q17 1 0.3066 0.5867 -0.0324 11.00000 0.05 0.17
Q18 1 0.5629 0.6147 0.4912 11.00000 0.05 0.16
Q19 1 0.9994 0.6143 0.4630 11.00000 0.05 0.16
Q20 1 0.5410 0.6693 0.0203 11.00000 0.05 0.16
;
_shelx_res_checksum 24456
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
N N1 0.85736(10) 0.61198(19) 0.41958(11) 0.0399(3) Uani d 1
H HN1 0.8022(15) 0.636(3) 0.4606(15) 0.048 Uiso d 1
O O1 0.62565(9) 0.65743(17) 0.43252(9) 0.0452(3) Uani d 1
C C1 0.98347(12) 0.5989(2) 0.48195(13) 0.0398(3) Uani d 1
H H1A 0.996007 0.675814 0.554503 0.048 Uiso calc 1
H H1AB 1.035920 0.643780 0.428470 0.048 Uiso calc 1
S S1 0.90847(3) 0.53047(7) 0.20190(4) 0.05100(17) Uani d 1
N N2 0.69512(10) 0.59494(18) 0.25797(10) 0.0372(3) Uani d 1
H HN2 0.6711(17) 0.573(2) 0.1826(14) 0.045 Uiso d 1
C C2 0.82013(12) 0.58234(19) 0.30120(12) 0.0351(3) Uani d 1
C C3 0.60474(11) 0.62787(19) 0.32261(12) 0.0332(3) Uani d 1
C C4 0.47845(11) 0.61990(18) 0.25055(12) 0.0323(3) Uani d 1
C C5 0.44876(13) 0.6519(2) 0.12543(12) 0.0380(3) Uani d 1
H H5 0.508903 0.681492 0.081672 0.046 Uiso calc 1
C C6 0.32849(14) 0.6391(2) 0.06642(14) 0.0446(3) Uani d 1
H H6 0.308060 0.662390 -0.017073 0.054 Uiso calc 1
C C7 0.23884(13) 0.5923(2) 0.13013(16) 0.0466(4) Uani d 1
H H7 0.158787 0.581443 0.089304 0.056 Uiso calc 1
C C8 0.26809(14) 0.5617(2) 0.25436(16) 0.0469(4) Uani d 1
H H8 0.207621 0.530909 0.297439 0.056 Uiso calc 1
C C9 0.38722(13) 0.5766(2) 0.31507(13) 0.0396(3) Uani d 1
H H9 0.406519 0.557780 0.399116 0.048 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
N1 0.0294(6) 0.0525(7) 0.0365(6) 0.0051(5) 0.0025(4) -0.0034(5)
O1 0.0362(5) 0.0667(7) 0.0327(5) 0.0038(5) 0.0061(4) -0.0008(5)
C1 0.0288(6) 0.0468(8) 0.0405(7) -0.0030(5) -0.0013(5) -0.0052(6)
S1 0.0316(2) 0.0798(3) 0.0436(2) -0.00179(16) 0.01212(16) -0.00785(18)
N2 0.0274(5) 0.0518(7) 0.0316(5) 0.0025(5) 0.0039(4) -0.0014(5)
C2 0.0282(6) 0.0395(7) 0.0371(6) -0.0016(5) 0.0049(5) 0.0012(5)
C3 0.0291(6) 0.0373(7) 0.0333(6) 0.0012(5) 0.0063(5) 0.0036(5)
C4 0.0283(6) 0.0338(6) 0.0347(6) 0.0024(5) 0.0058(5) 0.0027(5)
C5 0.0348(6) 0.0427(7) 0.0362(6) -0.0003(5) 0.0063(5) 0.0053(5)
C6 0.0410(7) 0.0497(8) 0.0390(7) 0.0026(6) -0.0030(6) 0.0041(6)
C7 0.0285(6) 0.0490(9) 0.0586(9) 0.0040(6) -0.0009(6) 0.0005(7)
C8 0.0313(7) 0.0552(9) 0.0571(9) 0.0028(6) 0.0155(6) 0.0040(7)
C9 0.0331(7) 0.0486(8) 0.0387(7) 0.0034(6) 0.0108(5) 0.0048(6)
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
C2 N1 C1 . . 123.98(12)
C2 N1 HN1 . . 116.3(12)
C1 N1 HN1 . . 119.7(12)
N1 C1 C1 . 3_766 110.75(14)
N1 C1 H1A . . 109.5
C1 C1 H1A 3_766 . 109.5
N1 C1 H1AB . . 109.5
C1 C1 H1AB 3_766 . 109.5
H1A C1 H1AB . . 108.1
C3 N2 C2 . . 128.67(11)
C3 N2 HN2 . . 115.1(13)
C2 N2 HN2 . . 116.1(13)
N1 C2 N2 . . 116.03(12)
N1 C2 S1 . . 125.77(10)
N2 C2 S1 . . 118.19(10)
O1 C3 N2 . . 122.46(12)
O1 C3 C4 . . 121.88(12)
N2 C3 C4 . . 115.64(11)
C5 C4 C9 . . 119.69(12)
C5 C4 C3 . . 123.74(12)
C9 C4 C3 . . 116.58(12)
C6 C5 C4 . . 119.34(13)
C6 C5 H5 . . 120.3
C4 C5 H5 . . 120.3
C7 C6 C5 . . 120.78(14)
C7 C6 H6 . . 119.6
C5 C6 H6 . . 119.6
C8 C7 C6 . . 119.91(13)
C8 C7 H7 . . 120.0
C6 C7 H7 . . 120.0
C7 C8 C9 . . 120.11(14)
C7 C8 H8 . . 119.9
C9 C8 H8 . . 119.9
C8 C9 C4 . . 120.15(14)
C8 C9 H9 . . 119.9
C4 C9 H9 . . 119.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
N1 C2 . 1.3228(17)
N1 C1 . 1.4564(17)
N1 HN1 . 0.854(14)
O1 C3 . 1.2209(16)
C1 C1 3_766 1.518(3)
C1 H1A . 0.9700
C1 H1AB . 0.9700
S1 C2 . 1.6633(14)
N2 C3 . 1.3723(17)
N2 C2 . 1.3971(16)
N2 HN2 . 0.846(14)
C3 C4 . 1.4913(17)
C4 C5 . 1.3894(17)
C4 C9 . 1.3944(18)
C5 C6 . 1.388(2)
C5 H5 . 0.9300
C6 C7 . 1.380(2)
C6 H6 . 0.9300
C7 C8 . 1.378(2)
C7 H7 . 0.9300
C8 C9 . 1.383(2)
C8 H8 . 0.9300
C9 H9 . 0.9300
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
N1 HN1 O1 . 0.855(17) 1.953(17) 2.6528(16) 138.3(15)
C5 H5 O1 4_575 0.93 2.583 3.478(16) 161.7
C9 H9 O1 3_666 0.93 2.519 3.311(16) 143.3
C1 H1A S1 4_576 0.97 2.97 3.8375(16) 149.6
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_4
_geom_torsion
C2 N1 C1 C1 3_766 -84.6(2)
C1 N1 C2 N2 . 177.90(13)
C1 N1 C2 S1 . -1.5(2)
C3 N2 C2 N1 . -2.5(2)
C3 N2 C2 S1 . 177.01(12)
C2 N2 C3 O1 . 2.4(2)
C2 N2 C3 C4 . -175.85(13)
O1 C3 C4 C5 . 156.36(14)
N2 C3 C4 C5 . -25.33(19)
O1 C3 C4 C9 . -23.98(19)
N2 C3 C4 C9 . 154.33(13)
C9 C4 C5 C6 . -0.4(2)
C3 C4 C5 C6 . 179.28(13)
C4 C5 C6 C7 . -1.1(2)
C5 C6 C7 C8 . 1.5(3)
C6 C7 C8 C9 . -0.4(3)
C7 C8 C9 C4 . -1.0(2)
C5 C4 C9 C8 . 1.4(2)
C3 C4 C9 C8 . -178.28(14)
_cod_database_fobs_code 2242909