#------------------------------------------------------------------------------
#$Date: 2018-02-24 09:34:40 +0200 (Sat, 24 Feb 2018) $
#$Revision: 206649 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242399.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_2242399
loop_
_publ_author_name
'Purandara, H.'
'Foro, S.'
'Thimme Gowda, B.'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
(E)-4-chloro-N-{2-[2-(4-nitrobenzylidene)hydrazin-1-yl]-2-oxoethyl}benzenesulfonamide
N,N-dimethylformamide monosolvate
;
_journal_coeditor_code RZ5227
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 394
_journal_page_last 399
_journal_paper_doi 10.1107/S205698901800292X
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'C15 H13 Cl N4 O5 S, C3 H7 N O'
_chemical_formula_moiety 'C15 H13 Cl N4 O5 S, C3 H7 N O'
_chemical_formula_sum 'C18 H20 Cl N5 O6 S'
_chemical_formula_weight 469.90
_chemical_name_systematic
;(E)-4-Chloro-N-{2-[2-(4-nitrobenzylidene)hydrazin-1-yl]-2-oxoethyl}benzenesulfonamide N,N-dimethylformamide
monosolvate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2014/6
_cell_angle_alpha 108.150(10)
_cell_angle_beta 98.360(10)
_cell_angle_gamma 105.070(10)
_cell_formula_units_Z 2
_cell_length_a 8.2400(10)
_cell_length_b 10.6310(10)
_cell_length_c 13.720(2)
_cell_measurement_reflns_used 1907
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.96
_cell_measurement_theta_min 2.64
_cell_volume 1068.7(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008) and PLATON (Spek,
2015)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
with Sapphire CCD detector
;
_diffrn_measurement_method
;
Rotation method data acquisition using omega scans.
;
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0269
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 6809
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 2.642
_exptl_absorpt_coefficient_mu 0.322
_exptl_absorpt_correction_T_max 0.975
_exptl_absorpt_correction_T_min 0.866
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.460
_exptl_crystal_description plate
_exptl_crystal_F_000 488
_exptl_crystal_size_max 0.460
_exptl_crystal_size_mid 0.220
_exptl_crystal_size_min 0.080
_refine_diff_density_max 0.610
_refine_diff_density_min -0.432
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.319
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 288
_refine_ls_number_reflns 3847
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.318
_refine_ls_R_factor_all 0.1402
_refine_ls_R_factor_gt 0.0895
_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^)+3.0287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1464
_refine_ls_wR_factor_ref 0.1668
_reflns_number_gt 2623
_reflns_number_total 3847
_reflns_threshold_expression 'I > 2\s(I)'
_iucr_refine_instructions_details
;
Cg1 is the centroid of the C1--C6 ring
;
_cod_data_source_file rz5227sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 1068.7(2)
_cod_database_code 2242399
_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 0.866
_shelx_estimated_absorpt_t_max 0.975
_shelx_hkl_file
;
0 0 2 278.848 11.9928 5
0 0 3 25470.3 73.3601 1
0 0 3 25688.3 94.0241 5
0 0 3 25453.2 78.5482 3
0 0 4 182.709 12.8736 3
0 0 4 179.288 12.6042 1
0 0 4 186.932 19.3384 5
0 0 5 11408.7 82.4292 5
0 0 5 11389.3 65.7739 2
0 0 5 11480.2 64.3004 1
0 0 5 11481.1 68.8337 3
0 0 6 878.300 31.0286 5
0 0 6 792.370 22.2649 2
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0 0 6 825.719 22.2808 1
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0 0 8 835.745 35.0491 5
0 0 8 830.265 27.6615 3
0 0 8 878.480 26.8963 2
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0 0 9 794.612 37.8973 5
0 0 9 717.171 29.0022 3
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0 -1 12 28.0233 18.5746 2
0 -1 11 138.283 29.5391 5
0 -1 11 123.564 18.8504 2
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0 -1 10 43.1564 16.2278 2
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0 -1 4 21465.6 77.2606 2
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0 -1 2 9223.59 37.6625 2
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0 -1 -4 7.18064 4.18083 0
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0 1 5 4844.87 39.5635 1
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0 -1 -5 4800.42 24.7005 0
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0 -1 -6 607.637 10.1921 0
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0 1 8 311.978 21.0098 3
0 1 8 363.230 29.7513 5
0 1 9-10.2722 15.8155 3
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0 1 9 0.04567 14.3678 2
0 1 10-8.78018 27.0807 5
0 1 10 62.1410 19.3924 3
0 1 10 60.0818 18.4950 2
0 1 11-23.4934 29.3038 5
0 1 11-20.9096 19.1235 3
0 1 12 200.228 36.7694 5
0 1 13 84.4566 35.9966 5
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0 -3 -5 3.72814 7.82446 6
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0 -7 16 54.5698 25.1428 2
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-9 6 -5 223.385 28.5823 1
-9 6 -6 132.066 29.4360 1
9 -6 7 117.648 32.0404 2
-9 5 10 130.348 40.0747 3
-9 5 8 211.039 32.0882 1
-9 5 7-65.4984 25.1683 1
-9 5 6 1.26449 26.2757 1
-9 5 5-93.8392 23.8922 1
-9 5 4 136.739 27.1577 1
-9 5 3-30.1684 27.9194 1
-9 5 2 369.012 35.7066 1
-9 5 1-17.3690 26.1164 1
-9 5 0-30.8830 23.5936 1
-9 5 -1 425.742 37.0843 1
-9 5 -1 395.407 27.2959 6
-9 5 -2 38.9918 21.8645 1
-9 5 -3 84.7784 21.4750 1
-9 5 -3 119.882 20.4879 6
-9 5 -4 57.9315 25.6876 1
-9 5 -4 178.362 25.2486 6
-9 5 -5 222.665 27.1867 1
-9 5 -5 275.240 26.4027 6
-9 5 -6 13.2539 27.6776 6
9 -5 6 13.8371 26.6836 2
9 -5 7 2.05204 30.0446 2
-9 4 10-106.090 32.5638 3
-9 4 9-92.9810 26.6934 1
-9 4 8 88.6270 24.6600 1
-9 4 7-2.52615 25.2278 1
-9 4 6 47.0743 25.5777 1
-9 4 5 7.13446 22.7066 1
-9 4 4 33.8378 25.9153 1
-9 4 3 146.866 28.0589 1
-9 4 2 180.827 29.4458 1
-9 4 1 141.416 30.7436 1
-9 4 0 45.6204 26.0198 1
-9 4 -1-43.6780 19.2699 1
-9 4 -1-26.5859 19.0629 6
-9 4 -2-5.21661 19.9469 1
-9 4 -2 85.8035 19.9716 6
-9 4 -3 158.396 21.8856 1
-9 4 -3 4.97844 21.7425 6
-9 4 -4-43.4218 24.4273 6
-9 4 -5-105.137 27.8645 6
9 -4 6-9.80704 27.3410 2
-9 3 11 68.8973 32.8069 3
-9 3 9 5.52184 22.8756 1
-9 3 8-6.96012 24.2791 1
-9 3 7 58.0006 24.2428 1
-9 3 6 140.126 27.2459 1
-9 3 5 111.188 29.6511 1
-9 3 4 17.5423 26.7251 1
-9 3 3 39.7917 27.6861 1
-9 3 2 208.214 21.1862 6
-9 3 2 96.9869 26.5506 1
-9 3 1-34.0819 24.6163 1
-9 3 1-114.289 22.5698 6
-9 3 0 177.033 29.2815 1
-9 3 0 344.269 29.2515 6
-9 3 -1 83.9625 22.7702 1
-9 3 -1-13.5662 19.8497 6
-9 3 -2-57.6141 25.9670 1
-9 3 -2-16.3250 20.7945 6
-9 3 -3 360.109 34.3594 6
-9 3 -4 120.784 23.1388 6
-9 3 -5 114.348 24.4073 6
9 -3 5 167.996 35.1979 2
9 -3 6 140.422 35.7237 2
-9 2 10-104.462 24.0155 1
-9 2 9 69.4190 25.7225 1
-9 2 8-39.3057 26.4355 1
-9 2 7-4.23011 27.1811 1
-9 2 6 48.2558 28.3966 1
-9 2 5-16.5462 20.7712 1
-9 2 4 169.747 28.2667 1
-9 2 3 234.139 29.8627 1
-9 2 2-30.3174 25.3479 1
-9 2 1 271.857 27.1508 6
-9 2 1 287.653 31.0905 1
-9 2 0 31.2962 22.8105 1
-9 2 0-36.2456 23.6389 6
-9 2 -1 51.6841 23.5889 6
-9 2 -2 168.390 29.6291 6
-9 2 -3-82.1825 24.8836 6
9 -2 4 53.9896 27.8434 2
9 -2 5-19.7185 28.1470 2
-9 1 10 79.0889 27.6384 1
-9 1 8 63.0658 27.5429 1
-9 1 7 149.946 27.9957 1
-9 1 6 115.168 27.3135 1
-9 1 5 521.114 40.4220 1
-9 1 4-7.02050 22.3987 1
-9 1 3-24.2983 21.7646 1
-9 1 2 98.3230 29.1118 7
-9 1 2 208.051 29.8342 1
-9 1 1 93.7742 26.1143 7
-9 1 1-50.3532 21.8616 1
-9 1 0-58.4536 28.2614 7
-9 1 0 210.299 31.0632 6
-9 1 -1 0.72582 26.0380 6
-9 1 -3 155.248 28.6924 6
-9 1 -4 425.383 30.8154 6
9 -1 5 70.9454 30.3893 2
-9 0 10 170.882 24.8660 1
-9 0 9 80.9826 26.9987 1
-9 0 8 40.7045 22.2735 1
-9 0 7 12.9413 24.9807 1
-9 0 6 138.599 28.9247 1
-9 0 5-60.7585 22.6676 1
-9 0 4 120.235 31.9066 7
-9 0 4 1.81667 21.8185 1
-9 0 3-73.6371 26.7351 7
-9 0 3 96.0629 23.5773 1
-9 0 2 266.816 31.5408 7
-9 0 1 82.9648 26.8521 7
-9 0 0 219.702 32.8401 7
-9 0 -1 327.517 35.8098 7
-9 0 -1 502.139 33.8401 6
-9 0 -2 216.194 29.4359 7
-9 0 -2 193.874 30.1731 6
-9 0 -3 143.176 24.0001 6
-9 -1 10-23.5568 24.0766 1
-9 -1 9-34.1476 26.0121 1
-9 -1 8 85.5381 28.1347 1
-9 -1 7 16.7757 25.5291 1
-9 -1 6 43.6651 24.3038 1
-9 -1 5 434.629 42.4860 7
-9 -1 5 404.671 31.1331 1
-9 -1 4-31.2781 24.0229 7
-9 -1 3 429.931 39.9412 7
-9 -1 2 102.956 30.8840 7
-9 -1 1 171.228 30.3747 7
-9 -1 0-18.4349 25.0997 7
-9 -1 -1 201.167 31.5664 7
-9 -1 -2-38.8174 34.0548 7
-9 -2 10 148.126 29.7961 1
-9 -2 9 114.229 28.6827 1
-9 -2 8-25.7166 28.0879 1
-9 -2 7 19.6234 25.1148 1
-9 -2 6 412.112 36.4447 7
-9 -2 6 312.601 29.6924 1
-9 -2 4 146.611 32.1070 7
-9 -2 2 210.002 36.9207 7
-9 -2 0 212.755 34.3040 7
-9 -2 -1 87.6109 32.8444 7
-9 -3 9-73.3004 32.0712 1
-9 -3 8 42.7978 24.3767 1
-9 -3 5 264.926 38.3565 7
-9 -3 3 164.907 39.7464 7
-10 7 -4 400.713 30.0639 6
-10 6 3-42.3986 25.3785 1
-10 6 2 138.063 33.5043 1
-10 6 1 154.275 29.3242 1
-10 6 0 18.4813 28.9626 1
-10 6 -1 278.661 31.5079 1
-10 6 -2 303.673 35.3991 1
-10 6 -3 131.685 30.3779 1
-10 5 4-73.4059 29.4167 1
-10 5 3 45.3056 30.6640 1
-10 5 2 34.4901 27.4357 1
-10 5 1 11.6364 23.4572 1
-10 5 0 225.477 34.1778 1
-10 5 -1-71.2801 28.2554 1
-10 5 -2-88.4492 26.5143 1
-10 5 -2 104.803 27.3104 6
-10 5 -3 64.8311 29.7326 1
-10 5 -3 349.632 30.5797 6
-10 4 5 127.442 26.8689 1
-10 4 4-91.1770 29.3088 1
-10 4 3 22.0016 24.6803 1
-10 4 2 93.6706 27.6439 1
-10 4 1 25.0076 29.2903 1
-10 4 0-70.7585 29.2118 1
-10 4 0-1.86958 26.4745 6
-10 4 -1 124.849 31.6339 1
-10 4 -1 210.766 31.6662 6
-10 4 -2 46.0651 29.1270 1
-10 3 6 42.5762 25.3636 1
-10 3 4 86.0941 26.2565 1
-10 3 3-66.4719 27.1030 1
-10 3 2-103.949 28.7894 1
-10 3 1 219.929 25.4814 6
-10 3 1 123.005 30.8001 1
-10 3 0 31.1096 28.8787 1
-10 3 0-38.8509 31.5145 6
-10 3 -2 331.148 33.4124 6
-10 2 7-71.3188 23.5869 1
-10 2 6 62.5984 28.6333 1
-10 2 5 178.709 30.4837 1
-10 2 4-14.8129 24.3122 1
-10 2 3 100.897 26.4723 1
-10 2 2 60.5967 24.4594 1
-10 2 1 93.5663 25.9300 1
-10 2 0 178.289 27.0107 6
-10 2 -1 173.717 27.9253 6
-10 1 7 128.940 25.8763 1
-10 1 6-60.2184 30.7043 1
-10 1 5 82.6587 29.1286 1
-10 1 4 162.457 29.2981 1
-10 1 3-8.24127 28.0133 1
-10 1 2 306.844 39.9959 7
-10 0 7-87.2987 28.7786 1
-10 0 6 199.678 30.2375 1
-10 0 5 316.856 34.0979 1
-10 0 3-99.1207 26.2984 7
-10 0 2 120.446 30.7031 7
-10 0 1-41.2723 28.5220 7
-10 -1 7 170.212 27.2585 1
-10 -1 6-30.9546 31.2641 1
;
_shelx_hkl_checksum 63054
_shelx_res_file
;
TITL GSH17 P-1
CELL 0.71073 8.24000 10.63100 13.72000 108.15000 98.36000 105.07000
ZERR 2 0.00100 0.00100 0.00200 0.01000 0.01000 0.01000
LATT 1
SFAC C H CL N O S
UNIT 36 40 2 10 12 2
PLAN 30
FMAP 2
SHEL 14 0.83
SIZE 0.46 0.22 0.08
MPLA 5 S1 N1 C7 C8 O3
MPLA 6 C1 C2 C3 C4 C5 C6
MPLA 6 C10 C11 C12 C13 C14 C15
MPLA 5 C9 N3 N2 C8 O3
L.S. 14
BOND $H
DFIX 0.86 0.02 N1 H1N
DFIX 0.86 0.02 N2 H2N
HTAB N1 O3
HTAB N1 O3_$1
HTAB N2 O6_$1
HTAB C5 O2_$2
HTAB C9 O6_$1
HTAB C14 O4_$3
HTAB C16 O1
HTAB C17 O1
HTAB C18 O2_$4
EQIV $1 -x+1, -y+1, -z
EQIV $2 x+1, y, z
EQIV $3 -x, -y+3, -z
EQIV $4 -x+1, -y+1, -z+1
HTAB
CONF
ACTA
WGHT 0.000000 3.028700
FVAR 1.79848
CL1 3 1.288438 1.081831 0.382322 11.00000 0.05482 0.09309 =
0.11259 0.02494 0.00423 0.00292
S1 6 0.520606 0.692118 0.269231 11.00000 0.04521 0.05140 =
0.04298 0.02319 0.01486 0.02328
O1 5 0.521420 0.570446 0.292450 11.00000 0.06112 0.06128 =
0.06289 0.03831 0.01679 0.02315
O2 5 0.425608 0.778384 0.318256 11.00000 0.05294 0.07205 =
0.05582 0.02345 0.02544 0.03708
O3 5 0.398980 0.583449 -0.067350 11.00000 0.07358 0.04736 =
0.04996 0.01004 0.01287 0.03443
O4 5 0.037571 1.513904 0.117530 11.00000 0.09031 0.05908 =
0.09033 0.03027 0.02111 0.04784
O5 5 0.071809 1.466701 0.258949 11.00000 0.10852 0.07990 =
0.06335 0.00994 0.02646 0.05496
N1 4 0.447489 0.642285 0.143781 11.00000 0.05221 0.03963 =
0.04276 0.01477 0.00884 0.02650
H1N 2 0.482251 0.581177 0.103391 11.00000 -1.20000
N2 4 0.326416 0.774451 -0.063610 11.00000 0.05744 0.03848 =
0.03624 0.01360 0.01122 0.02568
H2N 2 0.320857 0.760050 -0.129824 11.00000 -1.20000
N3 4 0.299712 0.893285 -0.002371 11.00000 0.03958 0.03060 =
0.03866 0.01035 0.00854 0.01401
N4 4 0.077137 1.444443 0.166855 11.00000 0.04792 0.04484 =
0.06068 0.00792 0.01070 0.01950
C1 1 0.739074 0.801376 0.301766 11.00000 0.04433 0.04928 =
0.03631 0.01830 0.01219 0.02390
C2 1 0.777673 0.945535 0.339920 11.00000 0.05957 0.05163 =
0.08540 0.00148 0.01667 0.03074
AFIX 43
H2 2 0.689742 0.984580 0.349588 11.00000 -1.20000
AFIX 0
C3 1 0.947014 1.030772 0.363469 11.00000 0.05419 0.04119 =
0.10538 -0.00489 0.01385 0.00883
AFIX 43
H3 2 0.973799 1.127543 0.388215 11.00000 -1.20000
AFIX 0
C4 1 1.075761 0.971708 0.350109 11.00000 0.04369 0.06177 =
0.04835 0.00901 0.00278 0.00676
C5 1 1.039245 0.828964 0.311186 11.00000 0.04520 0.06212 =
0.05393 0.02675 0.01761 0.02855
AFIX 43
H5 2 1.127579 0.790390 0.301540 11.00000 -1.20000
AFIX 0
C6 1 0.869469 0.743768 0.286641 11.00000 0.05658 0.04750 =
0.05309 0.02663 0.02095 0.03035
AFIX 43
H6 2 0.842906 0.647022 0.259766 11.00000 -1.20000
AFIX 0
C7 1 0.400083 0.740960 0.100865 11.00000 0.04749 0.04342 =
0.04066 0.01579 0.01196 0.02222
AFIX 23
H7A 2 0.490471 0.831336 0.133200 11.00000 -1.20000
H7B 2 0.293551 0.752684 0.118099 11.00000 -1.20000
AFIX 0
C8 1 0.375446 0.690628 -0.016653 11.00000 0.03420 0.03381 =
0.04040 0.00721 0.00324 0.00995
C9 1 0.253072 0.967928 -0.050391 11.00000 0.04305 0.03782 =
0.03546 0.01486 0.00991 0.01360
AFIX 43
H9 2 0.242541 0.942425 -0.122882 11.00000 -1.20000
AFIX 0
C10 1 0.216083 1.093466 0.008074 11.00000 0.03162 0.03363 =
0.04161 0.01582 0.00831 0.00916
C11 1 0.233950 1.138239 0.116991 11.00000 0.06537 0.04758 =
0.03826 0.01933 0.00678 0.02748
AFIX 43
H11 2 0.275711 1.089508 0.154847 11.00000 -1.20000
AFIX 0
C12 1 0.190996 1.253120 0.169562 11.00000 0.06527 0.04818 =
0.03483 0.01047 0.00504 0.02224
AFIX 43
H12 2 0.201947 1.281944 0.242219 11.00000 -1.20000
AFIX 0
C13 1 0.131201 1.324690 0.111899 11.00000 0.03879 0.03736 =
0.03893 0.00751 0.00444 0.01108
C14 1 0.116691 1.287290 0.005848 11.00000 0.05027 0.03970 =
0.06078 0.02707 0.01518 0.02049
AFIX 43
H14 2 0.079455 1.338974 -0.030864 11.00000 -1.20000
AFIX 0
C15 1 0.158428 1.171364 -0.045467 11.00000 0.05071 0.04921 =
0.04528 0.02495 0.01301 0.02252
AFIX 43
H15 2 0.147862 1.144159 -0.118039 11.00000 -1.20000
AFIX 0
O6 5 0.700085 0.243961 0.277913 11.00000 0.13454 0.07453 =
0.04472 0.01664 0.02790 0.05601
N5 4 0.734512 0.400717 0.440599 11.00000 0.08533 0.05685 =
0.04164 0.01364 0.01442 0.03434
C16 1 0.712317 0.359435 0.336814 11.00000 0.10021 0.07536 =
0.05218 0.03010 0.02203 0.05083
AFIX 43
H16A 2 0.705469 0.425222 0.306228 11.00000 -1.20000
AFIX 0
C17 1 0.755727 0.543637 0.505739 11.00000 0.16477 0.08313 =
0.06388 0.01021 0.00371 0.07216
AFIX 137
H17A 2 0.749295 0.597566 0.461573 11.00000 -1.50000
H17B 2 0.866507 0.583922 0.555977 11.00000 -1.50000
H17C 2 0.665407 0.543915 0.542735 11.00000 -1.50000
AFIX 0
C18 1 0.741912 0.305097 0.493982 11.00000 0.14458 0.07670 =
0.05604 0.03012 0.03387 0.03217
AFIX 137
H18A 2 0.704286 0.211362 0.442874 11.00000 -1.50000
H18B 2 0.667491 0.311738 0.541775 11.00000 -1.50000
H18C 2 0.858914 0.328180 0.533032 11.00000 -1.50000
AFIX 0
HKLF 4
REM GSH17 P-1
REM R1 = 0.0895 for 2623 Fo > 4sig(Fo) and 0.1402 for all 3847 data
REM 288 parameters refined using 2 restraints
END
WGHT 0.0000 2.8276
REM Instructions for potential hydrogen bonds
HTAB N1 O3_$1
HTAB N2 O6_$1
HTAB C5 O2_$2
HTAB C9 O6_$1
HTAB C14 O4_$3
HTAB C16 O1
HTAB C17 O1
HTAB C18 O2_$4
REM Highest difference peak 0.610, deepest hole -0.432, 1-sigma level 0.067
Q1 1 1.3051 1.0398 0.4378 11.00000 0.05 0.61
Q2 1 0.8397 0.9530 0.3032 11.00000 0.05 0.26
Q3 1 0.9406 0.9982 0.4300 11.00000 0.05 0.26
Q4 1 0.7509 0.8725 0.2851 11.00000 0.05 0.26
Q5 1 0.3610 0.6561 0.2819 11.00000 0.05 0.24
Q6 1 0.8414 0.2723 0.2847 11.00000 0.05 0.24
Q7 1 0.8035 0.4758 0.3172 11.00000 0.05 0.24
Q8 1 0.3847 0.8271 0.2753 11.00000 0.05 0.24
Q9 1 0.2693 1.5545 0.2612 11.00000 0.05 0.24
Q10 1 0.8035 0.9053 0.3740 11.00000 0.05 0.23
Q11 1 0.8373 0.3708 0.5621 11.00000 0.05 0.23
Q12 1 0.9747 0.6310 0.5794 11.00000 0.05 0.23
Q13 1 -0.0044 1.0144 -0.1178 11.00000 0.05 0.22
Q14 1 0.7290 0.3378 0.5751 11.00000 0.05 0.22
Q15 1 0.6655 0.3189 0.4415 11.00000 0.05 0.22
Q16 1 0.9764 1.1643 0.3219 11.00000 0.05 0.22
Q17 1 0.1208 1.1014 -0.0271 11.00000 0.05 0.22
Q18 1 0.5858 0.3559 0.3901 11.00000 0.05 0.21
Q19 1 0.4789 0.9229 0.2976 11.00000 0.05 0.21
Q20 1 0.1885 0.9970 0.2175 11.00000 0.05 0.21
Q21 1 1.0581 0.3433 0.5627 11.00000 0.05 0.21
Q22 1 0.2312 0.5149 -0.1392 11.00000 0.05 0.21
Q23 1 0.6784 0.5163 0.6024 11.00000 0.05 0.21
Q24 1 1.2876 1.0466 0.3356 11.00000 0.05 0.21
Q25 1 1.0058 0.9029 0.2963 11.00000 0.05 0.21
Q26 1 0.5000 0.8997 0.3002 11.00000 0.05 0.21
Q27 1 0.1887 1.3559 -0.0027 11.00000 0.05 0.21
Q28 1 0.5944 0.2177 0.3819 11.00000 0.05 0.20
Q29 1 0.1775 1.1018 0.0564 11.00000 0.05 0.20
Q30 1 0.1927 0.9203 -0.1599 11.00000 0.05 0.20
;
_shelx_res_checksum 74690
_shelxl_version_number 2014/6
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
Cl Cl1 1.2884(2) 1.0818(2) 0.38232(19) 0.0962(7) Uani d 1
S S1 0.52061(19) 0.69212(16) 0.26923(12) 0.0430(4) Uani d 1
O O1 0.5214(5) 0.5704(4) 0.2924(3) 0.0570(11) Uani d 1
O O2 0.4256(5) 0.7784(4) 0.3183(3) 0.0554(11) Uani d 1
O O3 0.3990(5) 0.5834(4) -0.0674(3) 0.0561(11) Uani d 1
O O4 0.0376(6) 1.5139(5) 0.1175(4) 0.0744(14) Uani d 1
O O5 0.0718(7) 1.4667(5) 0.2589(4) 0.0824(16) Uani d 1
N N1 0.4475(6) 0.6423(5) 0.1438(4) 0.0429(11) Uani d 1
H H1N 0.482(7) 0.581(4) 0.103(4) 0.051 Uiso d 1
N N2 0.3264(6) 0.7745(5) -0.0636(4) 0.0420(11) Uani d 1
H H2N 0.321(7) 0.760(6) -0.1298(19) 0.050 Uiso d 1
N N3 0.2997(5) 0.8933(4) -0.0024(3) 0.0364(10) Uani d 1
N N4 0.0771(6) 1.4444(5) 0.1669(5) 0.0534(13) Uani d 1
C C1 0.7391(7) 0.8014(6) 0.3018(4) 0.0406(13) Uani d 1
C C2 0.7777(9) 0.9455(7) 0.3399(6) 0.069(2) Uani d 1
H H2 0.6897 0.9846 0.3496 0.083 Uiso calc 1
C C3 0.9470(9) 1.0308(7) 0.3635(6) 0.077(2) Uani d 1
H H3 0.9738 1.1275 0.3882 0.092 Uiso calc 1
C C4 1.0758(8) 0.9717(7) 0.3501(5) 0.0572(17) Uani d 1
C C5 1.0392(8) 0.8290(7) 0.3112(5) 0.0495(15) Uani d 1
H H5 1.1276 0.7904 0.3015 0.059 Uiso calc 1
C C6 0.8695(8) 0.7438(6) 0.2866(5) 0.0467(15) Uani d 1
H H6 0.8429 0.6470 0.2598 0.056 Uiso calc 1
C C7 0.4001(7) 0.7410(6) 0.1009(4) 0.0421(13) Uani d 1
H H7A 0.4905 0.8313 0.1332 0.051 Uiso calc 1
H H7B 0.2936 0.7527 0.1181 0.051 Uiso calc 1
C C8 0.3754(7) 0.6906(5) -0.0167(4) 0.0386(13) Uani d 1
C C9 0.2531(7) 0.9679(5) -0.0504(4) 0.0383(13) Uani d 1
H H9 0.2425 0.9424 -0.1229 0.046 Uiso calc 1
C C10 0.2161(6) 1.0935(5) 0.0081(4) 0.0355(12) Uani d 1
C C11 0.2339(8) 1.1382(6) 0.1170(4) 0.0483(15) Uani d 1
H H11 0.2757 1.0895 0.1548 0.058 Uiso calc 1
C C12 0.1910(8) 1.2531(6) 0.1696(5) 0.0506(15) Uani d 1
H H12 0.2019 1.2819 0.2422 0.061 Uiso calc 1
C C13 0.1312(7) 1.3247(6) 0.1119(4) 0.0408(13) Uani d 1
C C14 0.1167(7) 1.2873(6) 0.0058(5) 0.0467(14) Uani d 1
H H14 0.0795 1.3390 -0.0309 0.056 Uiso calc 1
C C15 0.1584(7) 1.1714(6) -0.0455(5) 0.0450(14) Uani d 1
H H15 0.1479 1.1442 -0.1180 0.054 Uiso calc 1
O O6 0.7001(7) 0.2440(5) 0.2779(4) 0.0807(16) Uani d 1
N N5 0.7345(7) 0.4007(5) 0.4406(4) 0.0602(14) Uani d 1
C C16 0.7123(10) 0.3594(8) 0.3368(6) 0.069(2) Uani d 1
H H16A 0.7055 0.4252 0.3062 0.083 Uiso calc 1
C C17 0.7557(13) 0.5436(8) 0.5057(6) 0.104(3) Uani d 1
H H17A 0.7493 0.5976 0.4616 0.156 Uiso calc 1
H H17B 0.8665 0.5839 0.5560 0.156 Uiso calc 1
H H17C 0.6654 0.5439 0.5427 0.156 Uiso calc 1
C C18 0.7419(12) 0.3051(8) 0.4940(6) 0.091(3) Uani d 1
H H18A 0.7043 0.2114 0.4429 0.136 Uiso calc 1
H H18B 0.6675 0.3117 0.5418 0.136 Uiso calc 1
H H18C 0.8589 0.3282 0.5330 0.136 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
Cl1 0.0548(12) 0.0931(16) 0.1126(18) 0.0029(11) 0.0042(11) 0.0249(13)
S1 0.0452(8) 0.0514(9) 0.0430(8) 0.0233(7) 0.0149(7) 0.0232(7)
O1 0.061(3) 0.061(3) 0.063(3) 0.023(2) 0.017(2) 0.038(2)
O2 0.053(3) 0.072(3) 0.056(3) 0.037(2) 0.025(2) 0.023(2)
O3 0.074(3) 0.047(3) 0.050(3) 0.034(2) 0.013(2) 0.010(2)
O4 0.090(4) 0.059(3) 0.090(4) 0.048(3) 0.021(3) 0.030(3)
O5 0.109(4) 0.080(4) 0.063(3) 0.055(3) 0.026(3) 0.010(3)
N1 0.052(3) 0.040(3) 0.043(3) 0.027(2) 0.009(2) 0.015(2)
N2 0.057(3) 0.038(3) 0.036(3) 0.026(2) 0.011(2) 0.014(2)
N3 0.040(3) 0.031(2) 0.039(3) 0.014(2) 0.009(2) 0.010(2)
N4 0.048(3) 0.045(3) 0.061(4) 0.020(3) 0.011(3) 0.008(3)
C1 0.044(3) 0.049(3) 0.036(3) 0.024(3) 0.012(3) 0.018(3)
C2 0.060(4) 0.052(4) 0.085(5) 0.031(4) 0.017(4) 0.001(4)
C3 0.054(4) 0.041(4) 0.105(6) 0.009(3) 0.014(4) -0.005(4)
C4 0.044(4) 0.062(4) 0.048(4) 0.007(3) 0.003(3) 0.009(3)
C5 0.045(4) 0.062(4) 0.054(4) 0.029(3) 0.018(3) 0.027(3)
C6 0.057(4) 0.048(4) 0.053(4) 0.030(3) 0.021(3) 0.027(3)
C7 0.047(3) 0.043(3) 0.041(3) 0.022(3) 0.012(3) 0.016(3)
C8 0.034(3) 0.034(3) 0.040(3) 0.010(2) 0.003(2) 0.007(3)
C9 0.043(3) 0.038(3) 0.035(3) 0.014(3) 0.010(2) 0.015(3)
C10 0.032(3) 0.034(3) 0.042(3) 0.009(2) 0.008(2) 0.016(2)
C11 0.065(4) 0.048(4) 0.038(3) 0.027(3) 0.007(3) 0.019(3)
C12 0.065(4) 0.048(4) 0.035(3) 0.022(3) 0.005(3) 0.010(3)
C13 0.039(3) 0.037(3) 0.039(3) 0.011(3) 0.004(3) 0.008(3)
C14 0.050(4) 0.040(3) 0.061(4) 0.020(3) 0.015(3) 0.027(3)
C15 0.051(4) 0.049(4) 0.045(3) 0.023(3) 0.013(3) 0.025(3)
O6 0.135(5) 0.075(3) 0.045(3) 0.056(3) 0.028(3) 0.017(3)
N5 0.085(4) 0.057(3) 0.042(3) 0.034(3) 0.014(3) 0.014(3)
C16 0.100(6) 0.075(5) 0.052(5) 0.051(5) 0.022(4) 0.030(4)
C17 0.165(9) 0.083(6) 0.064(5) 0.072(6) 0.004(5) 0.010(5)
C18 0.145(8) 0.077(5) 0.056(5) 0.032(5) 0.034(5) 0.030(4)
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'
Cl Cl 0.1484 0.1585 '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
O1 S1 O2 120.2(3)
O1 S1 N1 107.3(2)
O2 S1 N1 107.0(2)
O1 S1 C1 107.6(3)
O2 S1 C1 106.8(3)
N1 S1 C1 107.4(3)
C7 N1 S1 118.6(4)
C7 N1 H1N 116(4)
S1 N1 H1N 118(4)
C8 N2 N3 119.1(4)
C8 N2 H2N 122(4)
N3 N2 H2N 118(4)
C9 N3 N2 116.6(4)
O4 N4 O5 123.6(5)
O4 N4 C13 118.4(6)
O5 N4 C13 118.0(5)
C6 C1 C2 120.0(6)
C6 C1 S1 120.4(4)
C2 C1 S1 119.6(4)
C3 C2 C1 119.7(6)
C3 C2 H2 120.1
C1 C2 H2 120.1
C4 C3 C2 119.5(6)
C4 C3 H3 120.2
C2 C3 H3 120.2
C3 C4 C5 121.4(6)
C3 C4 Cl1 118.5(5)
C5 C4 Cl1 120.1(5)
C4 C5 C6 119.0(5)
C4 C5 H5 120.5
C6 C5 H5 120.5
C1 C6 C5 120.3(6)
C1 C6 H6 119.8
C5 C6 H6 119.8
N1 C7 C8 111.2(4)
N1 C7 H7A 109.4
C8 C7 H7A 109.4
N1 C7 H7B 109.4
C8 C7 H7B 109.4
H7A C7 H7B 108.0
O3 C8 N2 121.7(5)
O3 C8 C7 123.2(5)
N2 C8 C7 115.1(5)
N3 C9 C10 120.2(5)
N3 C9 H9 119.9
C10 C9 H9 119.9
C15 C10 C11 117.8(5)
C15 C10 C9 119.9(5)
C11 C10 C9 122.2(5)
C12 C11 C10 121.2(5)
C12 C11 H11 119.4
C10 C11 H11 119.4
C11 C12 C13 118.4(5)
C11 C12 H12 120.8
C13 C12 H12 120.8
C14 C13 C12 122.5(5)
C14 C13 N4 118.7(5)
C12 C13 N4 118.8(5)
C13 C14 C15 118.3(5)
C13 C14 H14 120.9
C15 C14 H14 120.9
C14 C15 C10 121.8(5)
C14 C15 H15 119.1
C10 C15 H15 119.1
C16 N5 C18 120.7(6)
C16 N5 C17 122.2(6)
C18 N5 C17 117.1(6)
O6 C16 N5 126.0(7)
O6 C16 H16A 117.0
N5 C16 H16A 117.0
N5 C17 H17A 109.5
N5 C17 H17B 109.5
H17A C17 H17B 109.5
N5 C17 H17C 109.5
H17A C17 H17C 109.5
H17B C17 H17C 109.5
N5 C18 H18A 109.5
N5 C18 H18B 109.5
H18A C18 H18B 109.5
N5 C18 H18C 109.5
H18A C18 H18C 109.5
H18B C18 H18C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 C4 1.739(6)
S1 O1 1.427(4)
S1 O2 1.431(4)
S1 N1 1.603(5)
S1 C1 1.773(6)
O3 C8 1.217(6)
O4 N4 1.217(6)
O5 N4 1.221(6)
N1 C7 1.460(6)
N1 H1N 0.854(19)
N2 C8 1.357(7)
N2 N3 1.374(6)
N2 H2N 0.865(19)
N3 C9 1.274(6)
N4 C13 1.477(7)
C1 C6 1.379(7)
C1 C2 1.386(8)
C2 C3 1.379(9)
C2 H2 0.9300
C3 C4 1.373(9)
C3 H3 0.9300
C4 C5 1.375(8)
C5 C6 1.380(8)
C5 H5 0.9300
C6 H6 0.9300
C7 C8 1.496(7)
C7 H7A 0.9700
C7 H7B 0.9700
C9 C10 1.461(7)
C9 H9 0.9300
C10 C15 1.390(7)
C10 C11 1.392(7)
C11 C12 1.374(8)
C11 H11 0.9300
C12 C13 1.380(7)
C12 H12 0.9300
C13 C14 1.362(8)
C14 C15 1.372(7)
C14 H14 0.9300
C15 H15 0.9300
O6 C16 1.210(8)
N5 C16 1.322(8)
N5 C18 1.434(8)
N5 C17 1.452(8)
C16 H16A 0.9300
C17 H17A 0.9600
C17 H17B 0.9600
C17 H17C 0.9600
C18 H18A 0.9600
C18 H18B 0.9600
C18 H18C 0.9600
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 H1N O3 2_665 0.854(19) 2.18(3) 2.976(6) 155(5)
N2 H2N O6 2_665 0.865(19) 2.00(2) 2.857(6) 171(5)
C5 H5 O2 1_655 0.93 2.47 3.357(7) 158.7
C14 H14 O4 2_585 0.93 2.53 3.457(7) 174.5
C16 H16A O1 . 0.93 2.46 3.207(8) 137.8
C18 H18B O2 2_666 0.96 2.53 3.339(8) 142.4
C15 H15 Cg1 2_675 0.93 2.72 3.629(7) 167
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
O1 S1 N1 C7 167.8(4)
O2 S1 N1 C7 37.6(5)
C1 S1 N1 C7 -76.7(5)
C8 N2 N3 C9 -179.7(5)
O1 S1 C1 C6 35.0(5)
O2 S1 C1 C6 165.3(4)
N1 S1 C1 C6 -80.2(5)
O1 S1 C1 C2 -146.7(5)
O2 S1 C1 C2 -16.4(6)
N1 S1 C1 C2 98.1(5)
C6 C1 C2 C3 -0.6(10)
S1 C1 C2 C3 -178.8(6)
C1 C2 C3 C4 -0.8(12)
C2 C3 C4 C5 1.6(12)
C2 C3 C4 Cl1 -179.1(6)
C3 C4 C5 C6 -1.0(10)
Cl1 C4 C5 C6 179.7(5)
C2 C1 C6 C5 1.2(9)
S1 C1 C6 C5 179.5(4)
C4 C5 C6 C1 -0.5(9)
S1 N1 C7 C8 166.5(4)
N3 N2 C8 O3 179.2(5)
N3 N2 C8 C7 -1.6(7)
N1 C7 C8 O3 -2.5(8)
N1 C7 C8 N2 178.3(5)
N2 N3 C9 C10 177.9(4)
N3 C9 C10 C15 -177.4(5)
N3 C9 C10 C11 1.6(8)
C15 C10 C11 C12 2.0(9)
C9 C10 C11 C12 -177.1(5)
C10 C11 C12 C13 -0.7(9)
C11 C12 C13 C14 -1.3(9)
C11 C12 C13 N4 177.2(5)
O4 N4 C13 C14 -7.1(8)
O5 N4 C13 C14 171.7(6)
O4 N4 C13 C12 174.3(6)
O5 N4 C13 C12 -7.0(8)
C12 C13 C14 C15 2.0(9)
N4 C13 C14 C15 -176.6(5)
C13 C14 C15 C10 -0.7(8)
C11 C10 C15 C14 -1.3(8)
C9 C10 C15 C14 177.8(5)
C18 N5 C16 O6 -1.6(12)
C17 N5 C16 O6 177.1(8)
_cod_database_fobs_code 2242399