#------------------------------------------------------------------------------
#$Date: 2023-03-16 03:28:11 +0000 (Thu, 16 Mar 2023) $
#$Revision: 281912 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244244.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_2244244
loop_
_publ_author_name
'Hebishy, Ali M. S.'
'Elgemeie, Galal H.'
'Gouda, Lobna M.'
'Jones, Peter G.'
_publ_section_title
;
Crystal structures of three homologues with increasing ring size:
2-methoxy-4-(thiophen-2-yl)-5,6,7,8-tetrahydroquinoline-3-carbonitrile,
2-methoxy-4-(thiophen-2-yl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile
and
2-methoxy-4-(thiophen-2-yl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine-3-carbonitrile
;
_journal_coeditor_code YZ2030
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989023001883
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C17 H18 N2 O S'
_chemical_formula_moiety 'C17 H18 N2 O S'
_chemical_formula_sum 'C17 H18 N2 O S'
_chemical_formula_weight 298.39
_chemical_name_systematic
2-Methoxy-4-(thiophen-2-yl)-5,6,7,8,9,10-hexahydro-cycloocta[b]pyridine-3-carbonitrile
_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'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 102.9861(14)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.87736(14)
_cell_length_b 12.51312(19)
_cell_length_c 12.53915(19)
_cell_measurement_reflns_used 43890
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 77.3640
_cell_measurement_theta_min 4.5820
_cell_volume 1510.16(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy'
_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 0.0286
_diffrn_reflns_av_unetI/netI 0.0095
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 68720
_diffrn_reflns_theta_full 77.000
_diffrn_reflns_theta_max 77.613
_diffrn_reflns_theta_min 4.594
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.897
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.84022
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.312
_exptl_crystal_description block
_exptl_crystal_F_000 632
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.279
_refine_diff_density_min -0.478
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.101
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 200
_refine_ls_number_reflns 3210
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.115
_refine_ls_R_factor_all 0.0345
_refine_ls_R_factor_gt 0.0337
_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^)+(0.0450P)^2^+0.6567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0902
_refine_ls_wR_factor_ref 0.0910
_reflns_number_gt 3087
_reflns_number_total 3210
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2030sup1.cif
_cod_data_source_block 1c
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2244244
_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 0.804
_shelx_estimated_absorpt_t_max 0.911
_shelx_hkl_file
;
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0 0 -3-5.14750 57.9660 35
0 0 -3-20.4042 62.0452 37
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0 0 -4 44767.9 1488.38 46
0 0 -4 46785.0 1507.61 37
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0 0 5 31.6986 29.8349 60
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12 -2 -4 621.788 41.8463 164
12 2 -4 641.563 42.6312 115
12 -2 -4 708.150 44.7217 115
-12 -2 4 516.467 37.1606 124
-12 2 4 464.949 36.0004 108
12 2 -4 659.048 43.0579 103
12 -2 -4 491.089 37.8095 96
-12 -2 3 974.736 52.7548 130
12 -2 -3 1249.12 61.8575 165
12 2 -3 1233.88 54.9525 165
-12 -2 3 1050.21 50.7505 150
12 -2 -3 1169.58 54.6099 164
12 2 -3 1308.89 59.2038 115
-12 -2 3 1109.22 51.6359 124
-12 2 3 933.708 47.4160 185
-12 -2 3 1094.67 55.5799 185
-12 -2 2 3778.48 141.842 185
-12 -2 2 3601.26 139.905 170
-12 2 2 4108.32 144.183 130
-12 -2 2 3890.60 142.025 130
-12 -2 2 3823.72 139.497 150
12 -2 -2 4238.11 145.316 165
12 -2 -2 4143.85 141.907 151
12 2 -2 4340.52 145.968 115
12 -2 -2 4073.76 144.388 115
-12 -2 2 3550.33 135.387 124
12 -2 -2 4004.52 143.616 89
-12 -2 1 2.21080 14.1329 170
-12 2 1 4.52785 21.4987 130
12 -2 -1 12.5334 24.6573 151
12 -2 -1 34.9940 24.6729 165
-12 -2 1 7.94504 19.3789 150
-12 2 1 37.8311 20.7932 150
12 2 -1-1.63571 22.8502 115
12 -2 -1 20.3935 20.4137 115
-12 -2 1-9.20232 15.5987 125
-12 2 1-3.49974 16.5308 125
12 -2 -1-6.17765 23.4770 89
-12 -2 0 1744.00 67.7447 130
-12 2 0 1478.30 64.6749 130
-12 -2 0 1623.49 67.3324 126
12 -2 0 1610.19 68.3712 89
-12 -2 0 1663.01 66.2663 150
-12 2 0 1702.45 67.0455 150
12 -2 0 1802.13 69.2572 151
12 2 0 1793.20 70.0257 151
-12 -3 6 219.363 22.1190 185
-12 -3 6 211.443 20.5430 170
12 -3 -6 290.585 26.9838 165
12 3 -6 236.585 27.4050 165
12 -3 -6 187.258 25.8609 164
-12 -3 6 220.162 23.2327 124
-12 3 6 222.564 24.1835 108
12 3 -6 179.272 24.5145 96
-12 3 5 17647.9 578.428 171
-12 -3 5 17118.2 577.005 185
-12 3 5 16834.8 576.467 130
-12 -3 5 18238.3 578.242 124
-12 3 5 16893.4 575.915 108
12 3 -5 18737.5 579.895 96
12 -3 -5 19745.3 580.636 165
12 3 -5 18330.8 576.788 165
12 -3 -5 18488.7 579.249 164
-12 3 4 7770.07 253.733 171
-12 -3 4 7351.58 253.110 185
-12 -3 4 7778.92 255.037 170
12 -3 -4 7657.40 254.059 164
12 3 -4 7415.01 250.777 115
-12 -3 4 7639.66 253.317 124
-12 3 4 6829.81 248.905 108
12 3 -4 8241.20 257.114 96
-12 -3 3 2900.78 109.583 130
12 -3 -3 3413.37 118.893 165
12 -3 -3 3102.88 113.475 164
12 3 -3 3256.79 115.359 115
12 -3 -3 3258.17 116.282 115
-12 -3 3 3103.11 112.669 124
-12 -3 3 3122.03 114.802 170
-12 3 3 2672.27 111.085 171
-12 3 2 64.8724 23.1386 130
-12 -3 2 92.6781 20.2183 130
12 -3 -2 103.851 28.9154 165
12 3 -2 102.446 24.8409 115
12 -3 -2 86.8001 22.6469 115
-12 -3 2 77.2368 18.1952 124
-12 -3 2 106.753 19.5830 170
12 3 -1 5438.79 170.384 115
-12 -3 1 4809.54 166.425 130
12 -3 -1 5222.66 167.920 165
-12 3 1 4946.06 166.748 150
-12 -4 5 243.262 22.4323 124
-12 -4 5 196.198 20.3382 170
-12 4 5 200.492 22.8054 171
12 -4 -5 263.680 25.2000 164
-12 4 4 59.7016 18.7893 171
12 -4 -4-2.53283 25.1030 165
12 -4 -4 44.6449 20.6025 164
-12 -4 4 21.2770 16.9311 124
12 4 -4 15.4030 20.8829 96
-12 -4 3 1516.06 62.9597 170
12 -4 -3 1599.42 63.6864 164
-12 -4 3 1556.31 63.0860 124
12 4 -3 1636.27 66.2303 96
-12 4 2 7636.17 270.034 130
-12 -4 2 8260.11 271.140 126
0 0 0 0.00 0.00 0
TITL quik_m8 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 9.877358 12.513121 12.539155 90.0000 102.9861 90.0000
ZERR 4.00 0.000072 0.000096 0.000097 0.0000 0.0007 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O S
UNIT 68.00 72.00 8.00 4.00 4.00
REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 83200
_shelx_res_file
;
TITL quik_m8 in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 09:41:02 on 19-Jan-2023
CELL 1.54184 9.877358 12.513121 12.539155 90.0000 102.9861 90.0000
ZERR 4.00 0.00014 0.00019 0.00019 0.0000 0.0014 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O S
UNIT 68.00 72.00 8.00 4.00 4.00
L.S. 6
FMAP 2
PLAN 10
TEMP -173
SIZE 0.12 0.06 0.05
ACTA 154
BOND $H
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, -y+2, -z+2
HTAB C11 N2_$1
EQIV $2 -x+1, -y+2, -z+1
HTAB C16 N2_$2
WGHT 0.045000 0.656700
FVAR 5.28963 0.89933
N1 3 0.965458 0.704462 0.868830 11.00000 0.01748 0.01690 =
0.02115 0.00214 0.00208 0.00060
C2 1 0.902438 0.797699 0.863267 11.00000 0.01757 0.01608 =
0.01946 0.00079 0.00337 -0.00152
C3 1 0.786133 0.824885 0.780555 11.00000 0.01644 0.01548 =
0.02191 0.00170 0.00318 0.00048
C4 1 0.737957 0.750556 0.697186 11.00000 0.01567 0.01781 =
0.01921 0.00245 0.00290 -0.00065
C4A 1 0.804327 0.650812 0.701376 11.00000 0.01819 0.01656 =
0.01975 0.00095 0.00403 -0.00019
C5 1 0.756936 0.568480 0.612637 11.00000 0.02281 0.01892 =
0.02045 -0.00098 0.00189 0.00231
AFIX 23
H5A 2 0.838085 0.525190 0.604922 11.00000 -1.20000
H5B 2 0.721646 0.605961 0.542353 11.00000 -1.20000
AFIX 0
SAME C6 C7' C8' C9
SIMU C6 > C8' 0.02 0.04 0.9
C6 1 0.643137 0.493096 0.634043 11.00000 0.02505 0.02185 =
0.02710 -0.00014 -0.00159 -0.00291
PART 1 21
AFIX 23
H6A 2 0.555045 0.533710 0.622776 21.00000 -1.20000
H6B 2 0.629649 0.435362 0.578674 21.00000 -1.20000
AFIX 23
PART 2 -21
H6C 2 0.587821 0.464035 0.564337 -21.00000 -1.20000
H6D 2 0.580013 0.531417 0.672098 -21.00000 -1.20000
AFIX 0
PART 1 21
C7 1 0.670335 0.441928 0.747165 21.00000 0.02078 0.02391 =
0.03415 0.00651 0.00442 0.00109
AFIX 23
H7A 2 0.591782 0.393868 0.750517 21.00000 -1.20000
H7B 2 0.672451 0.498915 0.802283 21.00000 -1.20000
AFIX 0
C8 1 0.805784 0.377831 0.778282 21.00000 0.02306 0.01960 =
0.03714 0.00585 0.00176 0.00115
AFIX 23
H8A 2 0.834831 0.358112 0.710285 21.00000 -1.20000
H8B 2 0.786865 0.310712 0.814129 21.00000 -1.20000
AFIX 0
PART 0
C9 1 0.928782 0.436198 0.855523 11.00000 0.02362 0.02374 =
0.03353 0.00864 0.00147 0.00410
PART 1 21
AFIX 23
H9A 2 0.895112 0.465575 0.918164 21.00000 -1.20000
H9B 2 1.001371 0.382682 0.885016 21.00000 -1.20000
AFIX 23
PART 2 -21
H9C 2 0.963248 0.367771 0.832114 -21.00000 -1.20000
H9D 2 0.962418 0.440989 0.935936 -21.00000 -1.20000
AFIX 0
PART 2 -21
C7' 1 0.726281 0.395056 0.712541 -21.00000 0.01782
AFIX 23
H7'1 2 0.663372 0.332962 0.709291 -21.00000 -1.20000
H7'2 2 0.807401 0.372112 0.684096 -21.00000 -1.20000
AFIX 0
C8' 1 0.775367 0.431165 0.831175 -21.00000 0.02092
AFIX 23
H8'1 2 0.736369 0.502322 0.841452 -21.00000 -1.20000
H8'2 2 0.744341 0.379823 0.880831 -21.00000 -1.20000
AFIX 0
PART 0
C10 1 0.996282 0.527485 0.803769 11.00000 0.01838 0.01830 =
0.02592 -0.00013 0.00104 0.00299
AFIX 23
H10A 2 1.090157 0.540801 0.849794 11.00000 -1.20000
H10B 2 1.007839 0.503787 0.731011 11.00000 -1.20000
AFIX 0
C10A 1 0.916817 0.631331 0.789953 11.00000 0.01732 0.01678 =
0.02134 0.00136 0.00430 0.00042
O1 4 0.950287 0.874908 0.937118 11.00000 0.02087 0.01692 =
0.02134 -0.00128 -0.00280 0.00138
C11 1 1.065863 0.848617 1.025495 11.00000 0.02394 0.02110 =
0.02212 -0.00017 -0.00452 0.00062
AFIX 137
H11A 2 1.144124 0.824411 0.995574 11.00000 -1.50000
H11B 2 1.038666 0.791551 1.069970 11.00000 -1.50000
H11C 2 1.093504 0.911983 1.071124 11.00000 -1.50000
AFIX 0
C12 1 0.722941 0.927620 0.784550 11.00000 0.01616 0.01999 =
0.02096 0.00038 0.00030 -0.00124
N2 3 0.676781 1.010768 0.792591 11.00000 0.02267 0.02082 =
0.02769 -0.00098 -0.00020 0.00267
S1 5 0.660616 0.860509 0.502131 11.00000 0.02601 0.03626 =
0.02987 0.01445 0.00100 -0.00005
C13 1 0.623290 0.781548 0.604242 11.00000 0.02014 0.01594 =
0.02091 0.00035 0.00137 0.00142
C14 1 0.483409 0.757197 0.583855 11.00000 0.02157 0.02326 =
0.02767 0.00481 0.00030 0.00170
AFIX 43
H14 2 0.441950 0.713919 0.630015 11.00000 -1.20000
AFIX 0
C15 1 0.409168 0.805184 0.484858 11.00000 0.02355 0.02816 =
0.03743 0.00224 -0.00764 0.00018
AFIX 43
H15 2 0.311650 0.798012 0.458326 11.00000 -1.20000
AFIX 0
C16 1 0.490707 0.861801 0.432413 11.00000 0.03397 0.03035 =
0.02860 0.00751 -0.00607 0.00417
AFIX 43
H16 2 0.457697 0.897968 0.364963 11.00000 -1.20000
AFIX 0
HKLF 4
REM quik_m8 in P2(1)/c
REM wR2 = 0.0910, GooF = S = 1.101, Restrained GooF = 1.115 for all data
REM R1 = 0.0337 for 3087 Fo > 4sig(Fo) and 0.0345 for all 3210 data
REM 200 parameters refined using 5 restraints
END
WGHT 0.0450 0.6567
REM Highest difference peak 0.279, deepest hole -0.478, 1-sigma level 0.043
Q1 1 0.6738 0.7629 0.6509 11.00000 0.05 0.28
Q2 1 0.7793 0.6081 0.6598 11.00000 0.05 0.27
Q3 1 0.7571 0.7876 0.7412 11.00000 0.05 0.27
Q4 1 0.7792 0.6998 0.6955 11.00000 0.05 0.25
Q5 1 0.8533 0.6383 0.7435 11.00000 0.05 0.24
Q6 1 0.8358 0.8086 0.8248 11.00000 0.05 0.24
Q7 1 0.5535 0.7770 0.6107 11.00000 0.05 0.23
Q8 1 0.4460 0.7752 0.5381 11.00000 0.05 0.22
Q9 1 0.9555 0.4849 0.8289 11.00000 0.05 0.22
Q10 1 0.6988 0.5358 0.6251 11.00000 0.05 0.21
;
_shelx_res_checksum 88233
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.96546(10) 0.70446(8) 0.86883(8) 0.0189(2) Uani d 1 . .
C C2 0.90244(11) 0.79770(9) 0.86327(9) 0.0178(2) Uani d 1 . .
C C3 0.78613(11) 0.82488(9) 0.78055(9) 0.0181(2) Uani d 1 . .
C C4 0.73796(11) 0.75056(9) 0.69719(9) 0.0177(2) Uani d 1 . .
C C4A 0.80433(12) 0.65081(9) 0.70138(9) 0.0182(2) Uani d 1 . .
C C5 0.75694(12) 0.56848(9) 0.61264(10) 0.0212(2) Uani d 1 . .
H H5A 0.838085 0.525190 0.604922 0.025 Uiso calc 1 . .
H H5B 0.721646 0.605961 0.542353 0.025 Uiso calc 1 . .
C C6 0.64314(13) 0.49310(10) 0.63404(10) 0.0258(3) Uani d 1 . .
H H6A 0.555045 0.533710 0.622776 0.031 Uiso calc 0.899(3) A 1
H H6B 0.629649 0.435362 0.578674 0.031 Uiso calc 0.899(3) A 1
H H6C 0.587821 0.464035 0.564337 0.031 Uiso calc 0.101(3) A 2
H H6D 0.580013 0.531417 0.672098 0.031 Uiso calc 0.101(3) A 2
C C7 0.67033(14) 0.44193(12) 0.74716(12) 0.0266(4) Uani d 0.899(3) A 1
H H7A 0.591782 0.393868 0.750517 0.032 Uiso calc 0.899(3) A 1
H H7B 0.672451 0.498915 0.802283 0.032 Uiso calc 0.899(3) A 1
C C8 0.80578(15) 0.37783(11) 0.77828(13) 0.0274(4) Uani d 0.899(3) A 1
H H8A 0.834831 0.358112 0.710285 0.033 Uiso calc 0.899(3) A 1
H H8B 0.786865 0.310712 0.814129 0.033 Uiso calc 0.899(3) A 1
C C9 0.92878(13) 0.43620(10) 0.85552(11) 0.0277(3) Uani d 1 . .
H H9A 0.895112 0.465575 0.918164 0.033 Uiso calc 0.899(3) A 1
H H9B 1.001371 0.382682 0.885016 0.033 Uiso calc 0.899(3) A 1
H H9C 0.963248 0.367771 0.832114 0.033 Uiso calc 0.101(3) A 2
H H9D 0.962418 0.440989 0.935936 0.033 Uiso calc 0.101(3) A 2
C C7' 0.7263(11) 0.3951(8) 0.7125(8) 0.018(3) Uiso d 0.101(3) A 2
H H7'1 0.663372 0.332962 0.709291 0.021 Uiso calc 0.101(3) A 2
H H7'2 0.807401 0.372112 0.684096 0.021 Uiso calc 0.101(3) A 2
C C8' 0.7754(10) 0.4312(9) 0.8312(8) 0.021(3) Uiso d 0.101(3) A 2
H H8'1 0.736369 0.502322 0.841452 0.025 Uiso calc 0.101(3) A 2
H H8'2 0.744341 0.379823 0.880831 0.025 Uiso calc 0.101(3) A 2
C C10 0.99628(12) 0.52748(9) 0.80377(10) 0.0215(2) Uani d 1 . .
H H10A 1.090157 0.540801 0.849794 0.026 Uiso calc 1 . .
H H10B 1.007839 0.503787 0.731011 0.026 Uiso calc 1 . .
C C10A 0.91682(12) 0.63133(9) 0.78995(10) 0.0185(2) Uani d 1 . .
O O1 0.95029(9) 0.87491(6) 0.93712(7) 0.02090(19) Uani d 1 . .
C C11 1.06586(13) 0.84862(10) 1.02549(10) 0.0239(3) Uani d 1 . .
H H11A 1.144124 0.824411 0.995574 0.036 Uiso calc 1 . .
H H11B 1.038666 0.791551 1.069970 0.036 Uiso calc 1 . .
H H11C 1.093504 0.911983 1.071124 0.036 Uiso calc 1 . .
C C12 0.72294(12) 0.92762(9) 0.78455(9) 0.0196(2) Uani d 1 . .
N N2 0.67678(11) 1.01077(8) 0.79259(9) 0.0247(2) Uani d 1 . .
S S1 0.66062(3) 0.86051(3) 0.50213(3) 0.03155(12) Uani d 1 . .
C C13 0.62329(12) 0.78155(9) 0.60424(9) 0.0195(2) Uani d 1 . .
C C14 0.48341(13) 0.75720(10) 0.58386(10) 0.0250(3) Uani d 1 . .
H H14 0.441950 0.713919 0.630015 0.030 Uiso calc 1 . .
C C15 0.40917(14) 0.80518(11) 0.48486(12) 0.0320(3) Uani d 1 . .
H H15 0.311650 0.798012 0.458326 0.038 Uiso calc 1 . .
C C16 0.49071(15) 0.86180(11) 0.43241(12) 0.0330(3) Uani d 1 . .
H H16 0.457697 0.897968 0.364963 0.040 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 0.0175(4) 0.0169(5) 0.0212(5) 0.0006(4) 0.0021(4) 0.0021(4)
C2 0.0176(5) 0.0161(5) 0.0195(5) -0.0015(4) 0.0034(4) 0.0008(4)
C3 0.0164(5) 0.0155(5) 0.0219(5) 0.0005(4) 0.0032(4) 0.0017(4)
C4 0.0157(5) 0.0178(5) 0.0192(5) -0.0007(4) 0.0029(4) 0.0024(4)
C4A 0.0182(5) 0.0166(5) 0.0197(5) -0.0002(4) 0.0040(4) 0.0010(4)
C5 0.0228(6) 0.0189(5) 0.0205(5) 0.0023(4) 0.0019(4) -0.0010(4)
C6 0.0250(6) 0.0219(6) 0.0271(6) -0.0029(5) -0.0016(5) -0.0001(5)
C7 0.0208(7) 0.0239(7) 0.0341(8) 0.0011(5) 0.0044(6) 0.0065(6)
C8 0.0231(7) 0.0196(7) 0.0371(8) 0.0012(5) 0.0018(6) 0.0058(6)
C9 0.0236(6) 0.0237(6) 0.0335(7) 0.0041(5) 0.0015(5) 0.0086(5)
C10 0.0184(5) 0.0183(6) 0.0259(6) 0.0030(4) 0.0010(4) -0.0001(4)
C10A 0.0173(5) 0.0168(5) 0.0213(5) 0.0004(4) 0.0043(4) 0.0014(4)
O1 0.0209(4) 0.0169(4) 0.0213(4) 0.0014(3) -0.0028(3) -0.0013(3)
C11 0.0239(6) 0.0211(6) 0.0221(6) 0.0006(5) -0.0045(5) -0.0002(4)
C12 0.0162(5) 0.0200(6) 0.0210(5) -0.0012(4) 0.0003(4) 0.0004(4)
N2 0.0227(5) 0.0208(5) 0.0277(5) 0.0027(4) -0.0002(4) -0.0010(4)
S1 0.02601(18) 0.0363(2) 0.02987(19) -0.00005(13) 0.00100(13) 0.01445(13)
C13 0.0201(5) 0.0159(5) 0.0209(6) 0.0014(4) 0.0014(4) 0.0003(4)
C14 0.0216(6) 0.0233(6) 0.0277(6) 0.0017(5) 0.0003(5) 0.0048(5)
C15 0.0235(6) 0.0282(7) 0.0374(7) 0.0002(5) -0.0076(5) 0.0022(6)
C16 0.0340(7) 0.0303(7) 0.0286(7) 0.0042(5) -0.0061(5) 0.0075(5)
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 N1 C10A . . 118.31(10) ?
N1 C2 O1 . . 120.66(10) ?
N1 C2 C3 . . 123.49(11) ?
O1 C2 C3 . . 115.83(10) ?
C4 C3 C2 . . 118.32(10) ?
C4 C3 C12 . . 122.93(10) ?
C2 C3 C12 . . 118.74(10) ?
C3 C4 C4A . . 118.99(10) ?
C3 C4 C13 . . 118.98(10) ?
C4A C4 C13 . . 121.95(10) ?
C10A C4A C4 . . 117.59(10) ?
C10A C4A C5 . . 121.53(10) ?
C4 C4A C5 . . 120.87(10) ?
C4A C5 C6 . . 114.05(10) ?
C4A C5 H5A . . 108.7 ?
C6 C5 H5A . . 108.7 ?
C4A C5 H5B . . 108.7 ?
C6 C5 H5B . . 108.7 ?
H5A C5 H5B . . 107.6 ?
C7 C6 C5 . . 115.95(10) y
C5 C6 C7' . . 105.8(4) ?
C7 C6 H6A . . 108.3 ?
C5 C6 H6A . . 108.3 ?
C7 C6 H6B . . 108.3 ?
C5 C6 H6B . . 108.3 ?
H6A C6 H6B . . 107.4 ?
C5 C6 H6C . . 110.6 ?
C7' C6 H6C . . 110.6 ?
C5 C6 H6D . . 110.6 ?
C7' C6 H6D . . 110.6 ?
H6C C6 H6D . . 108.7 ?
C6 C7 C8 . . 114.70(12) y
C6 C7 H7A . . 108.6 ?
C8 C7 H7A . . 108.6 ?
C6 C7 H7B . . 108.6 ?
C8 C7 H7B . . 108.6 ?
H7A C7 H7B . . 107.6 ?
C7 C8 C9 . . 115.32(12) y
C7 C8 H8A . . 108.4 ?
C9 C8 H8A . . 108.4 ?
C7 C8 H8B . . 108.4 ?
C9 C8 H8B . . 108.4 ?
H8A C8 H8B . . 107.5 ?
C8' C9 C10 . . 117.8(5) ?
C10 C9 C8 . . 115.98(11) y
C10 C9 H9A . . 108.3 ?
C8 C9 H9A . . 108.3 ?
C10 C9 H9B . . 108.3 ?
C8 C9 H9B . . 108.3 ?
H9A C9 H9B . . 107.4 ?
C8' C9 H9C . . 107.9 ?
C10 C9 H9C . . 107.9 ?
C8' C9 H9D . . 107.9 ?
C10 C9 H9D . . 107.9 ?
H9C C9 H9D . . 107.2 ?
C8' C7' C6 . . 111.3(8) ?
C8' C7' H7'1 . . 109.4 ?
C6 C7' H7'1 . . 109.4 ?
C8' C7' H7'2 . . 109.4 ?
C6 C7' H7'2 . . 109.4 ?
H7'1 C7' H7'2 . . 108.0 ?
C9 C8' C7' . . 107.5(8) ?
C9 C8' H8'1 . . 110.2 ?
C7' C8' H8'1 . . 110.2 ?
C9 C8' H8'2 . . 110.2 ?
C7' C8' H8'2 . . 110.2 ?
H8'1 C8' H8'2 . . 108.5 ?
C10A C10 C9 . . 115.14(10) ?
C10A C10 H10A . . 108.5 ?
C9 C10 H10A . . 108.5 ?
C10A C10 H10B . . 108.5 ?
C9 C10 H10B . . 108.5 ?
H10A C10 H10B . . 107.5 ?
N1 C10A C4A . . 123.24(10) ?
N1 C10A C10 . . 114.11(10) y
C4A C10A C10 . . 122.63(10) ?
C2 O1 C11 . . 117.39(9) ?
O1 C11 H11A . . 109.5 ?
O1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
O1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
N2 C12 C3 . . 176.64(12) ?
C16 S1 C13 . . 92.07(6) ?
C14 C13 C4 . . 130.04(11) ?
C14 C13 S1 . . 111.19(9) ?
C4 C13 S1 . . 118.77(9) ?
C13 C14 C15 . . 111.46(12) ?
C13 C14 H14 . . 124.3 ?
C15 C14 H14 . . 124.3 ?
C16 C15 C14 . . 113.52(12) ?
C16 C15 H15 . . 123.2 ?
C14 C15 H15 . . 123.2 ?
C15 C16 S1 . . 111.76(10) ?
C15 C16 H16 . . 124.1 ?
S1 C16 H16 . . 124.1 ?
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
N1 C2 . 1.3168(15) ?
N1 C10A . 1.3538(15) ?
C2 O1 . 1.3482(14) ?
C2 C3 . 1.4056(15) ?
C3 C4 . 1.4003(16) ?
C3 C12 . 1.4348(16) ?
C4 C4A . 1.4053(16) ?
C4 C13 . 1.4826(15) ?
C4A C10A . 1.4046(16) ?
C4A C5 . 1.5115(16) ?
C5 C6 . 1.5365(17) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.5241(19) ?
C6 C7' . 1.669(10) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C6 H6C . 0.9900 ?
C6 H6D . 0.9900 ?
C7 C8 . 1.5333(19) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.5552(19) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C8' . 1.478(10) ?
C9 C10 . 1.5378(17) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 H9C . 0.9900 ?
C9 H9D . 0.9900 ?
C7' C8' . 1.526(12) ?
C7' H7'1 . 0.9900 ?
C7' H7'2 . 0.9900 ?
C8' H8'1 . 0.9900 ?
C8' H8'2 . 0.9900 ?
C10 C10A . 1.5078(15) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
O1 C11 . 1.4391(13) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 N2 . 1.1494(16) ?
S1 C16 . 1.7093(14) ?
S1 C13 . 1.7216(12) ?
C13 C14 . 1.3815(17) ?
C14 C15 . 1.4248(18) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.349(2) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C11 H11C N2 3_777 0.98 2.69 3.4864(16) 138.2 yes
C16 H16 N2 3_676 0.95 2.41 3.3379(17) 166.5 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
C10A N1 C2 O1 . . . . -177.20(10) ?
C10A N1 C2 C3 . . . . 0.87(17) ?
N1 C2 C3 C4 . . . . -2.62(17) ?
O1 C2 C3 C4 . . . . 175.53(10) ?
N1 C2 C3 C12 . . . . 177.99(10) ?
O1 C2 C3 C12 . . . . -3.86(16) ?
C2 C3 C4 C4A . . . . 2.15(16) ?
C12 C3 C4 C4A . . . . -178.48(11) ?
C2 C3 C4 C13 . . . . -174.70(10) ?
C12 C3 C4 C13 . . . . 4.66(17) ?
C3 C4 C4A C10A . . . . -0.16(16) ?
C13 C4 C4A C10A . . . . 176.60(10) ?
C3 C4 C4A C5 . . . . -179.36(10) ?
C13 C4 C4A C5 . . . . -2.61(17) ?
C10A C4A C5 C6 . . . . 91.62(13) y
C4 C4A C5 C6 . . . . -89.21(13) ?
C4A C5 C6 C7 . . . . -49.08(15) y
C4A C5 C6 C7' . . . . -85.2(4) ?
C5 C6 C7 C8 . . . . -56.74(16) y
C6 C7 C8 C9 . . . . 100.76(15) y
C7 C8 C9 C10 . . . . -72.30(16) y
C5 C6 C7' C8' . . . . 77.4(8) ?
C10 C9 C8' C7' . . . . 72.2(8) ?
C6 C7' C8' C9 . . . . -111.6(8) ?
C8' C9 C10 C10A . . . . 33.5(5) ?
C8 C9 C10 C10A . . . . 78.19(15) y
C2 N1 C10A C4A . . . . 1.34(17) ?
C2 N1 C10A C10 . . . . 179.91(10) ?
C4 C4A C10A N1 . . . . -1.67(17) ?
C5 C4A C10A N1 . . . . 177.53(10) ?
C4 C4A C10A C10 . . . . 179.88(10) ?
C5 C4A C10A C10 . . . . -0.92(17) y
C9 C10 C10A N1 . . . . 99.52(12) ?
C9 C10 C10A C4A . . . . -81.90(15) y
N1 C2 O1 C11 . . . . -4.18(16) ?
C3 C2 O1 C11 . . . . 177.61(10) ?
C3 C4 C13 C14 . . . . -101.27(15) ?
C4A C4 C13 C14 . . . . 81.97(17) ?
C3 C4 C13 S1 . . . . 78.50(13) ?
C4A C4 C13 S1 . . . . -98.25(12) ?
C16 S1 C13 C14 . . . . 0.20(10) ?
C16 S1 C13 C4 . . . . -179.62(10) ?
C4 C13 C14 C15 . . . . 179.12(12) ?
S1 C13 C14 C15 . . . . -0.66(14) ?
C13 C14 C15 C16 . . . . 0.95(18) ?
C14 C15 C16 S1 . . . . -0.79(17) ?
C13 S1 C16 C15 . . . . 0.34(12) ?
_cod_database_fobs_code 2244244