#------------------------------------------------------------------------------
#$Date: 2023-03-16 03:28:11 +0000 (Thu, 16 Mar 2023) $
#$Revision: 281912 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244242.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_2244242
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 'C15 H14 N2 O S'
_chemical_formula_moiety 'C15 H14 N2 O S'
_chemical_formula_sum 'C15 H14 N2 O S'
_chemical_formula_weight 270.34
_chemical_name_systematic
;
2-Methoxy-4-(thiophen-2-yl)-5,6,7,8-tetrahydroquinoline-3-carbonitrile
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 98.7757(12)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.85636(13)
_cell_length_b 9.18570(10)
_cell_length_c 13.31001(16)
_cell_measurement_reflns_used 35765
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 77.0990
_cell_measurement_theta_min 4.9090
_cell_volume 1311.78(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.51a (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(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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 0.0321
_diffrn_reflns_av_unetI/netI 0.0107
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 59253
_diffrn_reflns_theta_full 77.000
_diffrn_reflns_theta_max 77.661
_diffrn_reflns_theta_min 4.906
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.128
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82009
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.369
_exptl_crystal_description irregular
_exptl_crystal_F_000 568
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.280
_refine_diff_density_min -0.236
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 173
_refine_ls_number_reflns 2774
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all 0.0272
_refine_ls_R_factor_gt 0.0263
_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^)+(0.0343P)^2^+0.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0708
_refine_ls_wR_factor_ref 0.0714
_reflns_number_gt 2663
_reflns_number_total 2774
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2030sup1.cif
_cod_data_source_block 1a
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2244242
_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 0.815
_shelx_estimated_absorpt_t_max 0.939
_shelx_hkl_file
;
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0 0 -1 13.7927 16.4599 20
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0 0 -2 9134.46 312.585 22
0 0 -2 8888.50 318.436 20
0 0 2 8915.57 319.060 21
0 0 3 60.9326 43.9807 36
0 0 3 10.7300 31.5427 30
0 0 -3 46.9769 36.9633 22
0 0 -3 25.3837 46.5326 20
0 0 3-4.31502 48.1929 21
0 0 -3 53.2564 37.7390 11
0 0 4 117562. 3732.88 36
0 0 4 113266. 3735.70 31
0 0 -4 103647. 3726.79 11
0 0 4 113473. 3730.24 9
0 0 4 112436. 3734.84 21
0 0 -4 110966. 3720.21 22
0 0 -4 111268. 3734.03 20
0 0 4 107783. 3724.16 18
0 0 5-21.3375 51.6170 36
0 0 5-23.2945 57.7705 31
0 0 5-21.2691 47.9174 9
0 0 5 18.8167 51.8179 18
0 0 -5-10.9591 41.1620 22
0 0 -5 30.0802 57.8193 20
0 0 5-7.65053 57.7431 21
0 0 6 924.256 102.743 31
0 0 6 1069.30 98.3900 36
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0 0 6 898.595 97.9149 40
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0 0 -7 27.5744 55.5651 48
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0 0 7 59.6091 77.1877 31
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0 0 -7 58.0775 65.4070 20
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10 -2 -8 29.1339 37.8925 58
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10 2 -8 6.56258 31.5828 110
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-10 -2 8 15.0368 27.8398 112
10 -2 -8 32.5905 39.9839 111
10 2 -8 62.7523 32.5632 111
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-10 -2 8 87.9989 32.7761 97
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-10 -2 7 189.707 94.0986 43
-10 -2 7 206.884 86.2183 52
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-10 2 7 196.871 41.9616 167
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10 2 -7 37.5237 34.4264 60
10 -2 -7 143.751 41.9281 80
10 -2 -7 151.911 42.5364 62
-10 -2 7 132.729 36.6334 57
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10 -2 -7 130.212 44.4119 58
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10 -2 -7 133.260 39.6477 137
10 2 -7 161.768 40.6602 137
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10 2 -7 58.6292 36.2916 110
10 2 -7 96.9712 41.7062 118
-10 -2 7 229.410 43.6912 105
-10 -2 7 103.849 32.4034 112
10 -2 -7 247.357 50.4978 111
10 2 -7 175.142 38.5006 111
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-10 2 7 179.885 42.3014 97
-10 -2 6 557.707 118.828 43
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-10 -2 5 961.689 63.0675 88
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-10 -2 4 307.655 89.5487 43
10 -2 -4 120.411 127.723 54
-10 -2 4 235.491 96.0188 52
10 -2 -4 283.581 111.406 47
10 2 -4 251.785 84.9891 47
10 -2 -4 365.015 110.151 45
10 2 -4 145.965 100.768 45
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10 -2 -4 375.099 127.708 2
-10 2 4 330.503 49.7530 167
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-10 2 4 340.575 39.2214 168
10 2 -4 336.377 54.3558 60
10 -2 -4 271.309 45.5577 80
10 2 -4 308.391 50.6173 62
10 -2 -4 358.643 54.6496 58
-10 -2 4 260.048 43.4391 129
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-10 -2 4 325.923 46.4863 131
10 2 -4 330.364 50.8342 118
-10 -2 4 252.073 45.9764 105
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10 2 -4 300.755 38.0744 111
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-10 -2 4 299.421 42.5736 88
-10 2 4 341.977 48.5145 97
-10 -2 4 292.332 46.0414 97
-10 2 4 354.204 40.0571 89
-10 -2 3 5200.02 308.078 43
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10 2 -3 5657.41 341.756 42
10 -2 -3 5329.45 338.130 54
-10 -2 3 4792.36 311.929 52
10 -2 -3 5898.55 340.712 45
10 2 -3 4958.77 316.221 45
10 -2 -3 5329.37 358.855 2
10 2 -3 4604.65 302.835 23
-10 -2 3 5064.13 323.602 4
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-10 2 3 5568.39 217.371 167
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-10 -2 3 4903.47 204.014 148
10 -2 -3 5046.63 205.580 80
10 2 -3 5439.11 217.550 62
10 -2 -3 5330.31 219.080 58
-10 -2 3 5442.61 212.933 129
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-10 2 3 5558.08 214.944 97
-10 -2 3 5508.14 212.533 97
-10 2 3 5420.03 207.309 89
10 2 -2 753.529 138.378 35
10 -2 -2 708.364 129.215 42
10 2 -2 312.774 126.338 42
10 -2 -2 432.463 123.138 54
-10 -2 2 484.820 119.328 52
10 -2 -2 570.192 124.510 45
10 2 -2 544.239 121.117 45
-10 2 2 575.196 119.777 4
10 2 -2 473.778 117.517 27
-10 -2 2 675.034 127.006 4
10 -2 -2 322.818 126.347 2
-10 2 2 652.225 63.2070 7
-10 2 2 565.628 58.5917 167
-10 -2 2 556.563 55.6231 167
-10 2 2 567.017 56.2081 178
-10 2 2 597.140 54.6478 168
-10 -2 2 555.675 51.0210 148
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10 2 -2 708.799 63.3780 60
10 2 -2 555.889 62.1802 62
10 -2 -2 542.943 62.8946 58
-10 -2 2 698.967 60.0347 129
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-10 -2 2 654.754 52.5150 131
10 2 -2 597.076 55.8854 118
-10 -2 2 659.585 51.3536 112
-10 2 2 619.128 57.6846 97
-10 2 2 634.682 53.8571 89
10 2 -1 9154.55 461.133 35
10 -2 -1 8249.11 425.919 42
10 2 -1 8563.43 456.181 42
10 -2 -1 8585.00 443.941 54
10 -2 -1 8258.79 442.141 45
10 2 -1 9401.60 452.813 45
10 -2 -1 7923.30 461.692 2
10 -2 -1 8168.17 442.644 27
10 2 -1 9465.74 459.608 27
-10 2 1 8211.43 315.850 172
-10 2 1 8729.08 324.425 167
-10 -2 1 8455.46 318.956 167
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-10 -2 1 8215.68 317.995 148
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10 2 -1 8752.53 324.592 62
10 2 -1 8687.16 326.108 60
-10 -2 1 8644.42 323.580 129
-10 2 1 8599.80 322.394 138
10 2 -1 8842.71 317.126 118
-10 -2 1 8378.76 313.079 112
-10 -2 1 8266.09 309.035 103
-10 -2 1 8724.18 322.381 89
-10 2 1 8661.67 318.880 89
10 2 0 6879.33 401.593 35
10 -2 0 6909.38 371.110 42
10 2 0 6348.75 385.844 42
10 -2 0 7035.79 374.421 54
10 -2 0 6727.72 380.527 45
10 -2 0 7151.18 416.146 2
10 -2 0 6470.63 378.252 27
10 2 0 6405.12 381.431 27
-10 -2 0 6385.70 382.244 4
-10 2 0 7111.63 268.176 7
-10 -2 0 6769.75 259.975 167
-10 2 0 7092.54 268.489 178
-10 2 0 7278.66 270.576 169
-10 2 0 6854.98 265.481 168
-10 2 0 6958.15 260.390 172
-10 -2 0 6815.40 263.679 148
-10 2 0 6960.02 258.914 145
10 2 0 6855.32 265.085 62
10 2 0 6992.96 269.825 60
10 -2 0 6667.11 264.991 58
-10 -2 0 6876.48 267.230 129
-10 2 0 7057.90 267.102 138
-10 -2 0 6476.59 255.426 138
10 2 0 6822.53 255.538 118
-10 -2 0 6929.30 256.265 112
-10 -2 0 6777.15 254.047 103
-10 -2 0 7113.88 265.533 89
10 2 1 1702.49 197.166 35
10 -2 1 1737.77 171.446 42
10 -2 1 1837.84 176.681 54
10 -2 1 1764.41 185.143 27
10 2 1 1997.02 192.575 27
-10 -2 -1 1945.55 191.576 4
10 -2 1 1926.10 208.591 2
-10 2 -1 1986.71 104.368 7
-10 -2 -1 2060.40 98.1934 167
-10 2 -1 2135.23 106.324 178
-10 2 -1 2246.26 108.123 169
-10 -2 -1 2190.72 99.1017 169
-10 2 -1 2034.87 104.747 168
-10 2 -1 2667.00 121.675 164
-10 -2 -1 2019.60 100.154 164
-10 2 -1 1955.44 98.5278 172
-10 2 -1 1989.21 94.8661 145
-10 -2 -1 2043.32 105.542 148
10 2 1 1939.41 100.258 62
10 2 1 1973.37 104.544 60
10 -2 1 2049.05 101.872 58
-10 -2 -1 2022.27 106.605 129
-10 2 -1 2089.60 106.202 138
-10 -2 -1 2125.47 99.3831 138
-10 -2 -1 2023.04 107.332 134
-10 2 -1 1872.55 91.5197 132
-10 -2 -1 1939.22 93.2387 103
-10 -2 -1 1916.46 102.705 89
10 2 2 3118.55 264.857 35
10 -2 2 3298.22 240.183 42
10 2 2 3604.43 270.984 42
10 -2 2 3869.92 264.081 27
10 2 2 3955.82 268.773 27
-10 2 -2 3881.95 158.754 7
-10 -2 -2 3688.36 153.917 164
-10 -2 -2 3722.33 161.005 178
-10 2 -2 3780.00 159.647 169
-10 -2 -2 3525.44 145.918 169
-10 2 -2 3934.04 162.889 168
-10 2 -2 4026.49 154.711 172
-10 2 -2 3956.52 167.808 164
-10 2 -2 3644.64 146.448 145
-10 -2 -2 3575.89 158.932 148
10 -2 2 3839.36 154.137 58
10 2 2 3776.85 160.651 75
10 2 2 3599.75 158.081 60
-10 2 -2 3675.23 162.492 138
-10 2 -2 3368.04 146.089 134
-10 -2 -2 3775.02 163.532 134
-10 2 -2 3698.38 148.656 132
-10 -2 -2 3517.11 149.399 103
-10 2 -2 3924.67 160.727 104
-10 -2 -2 3594.97 157.432 89
10 -2 3 1216.67 139.625 42
10 2 3 1776.10 177.826 42
10 2 3 1996.12 167.793 46
-10 2 -3 1938.22 74.4515 7
-10 2 -3 1754.63 83.2590 164
-10 -2 -3 1553.63 71.6746 164
-10 2 -3 1699.72 78.8540 178
-10 -2 -3 1529.67 75.3427 178
-10 2 -3 1530.18 72.0390 169
-10 2 -3 1564.38 76.9799 168
-10 -2 -3 1653.12 79.3325 168
-10 2 -3 1657.30 69.4074 172
-10 2 -3 1510.86 75.7113 148
-10 -2 -3 1792.64 81.0351 148
10 2 3 1661.54 74.9784 75
10 2 3 1531.59 70.8866 60
-10 -2 -3 1777.80 80.2112 129
-10 2 -3 1781.41 81.1722 138
-10 2 -3 1458.89 60.8057 134
-10 -2 -3 1628.00 67.3512 103
-10 2 -3 1642.96 74.0591 104
-10 2 -3 1667.77 74.7800 91
-10 -2 -3 1787.71 75.0434 89
10 2 4 1348.46 163.822 35
10 -2 4 1043.33 130.164 42
10 2 4 1086.30 133.727 46
-10 2 -4 1143.24 61.4852 7
-10 2 -4 1112.88 74.5157 164
-10 -2 -4 1076.42 67.6043 164
-10 2 -4 1003.15 68.1845 178
-10 -2 -4 1097.04 68.4166 178
-10 2 -4 1033.00 64.3171 169
-10 -2 -4 1035.68 67.9395 168
-10 2 -4 1032.03 71.0674 148
-10 -2 -4 1154.22 73.5270 148
10 2 4 1119.70 65.2971 75
10 2 4 1169.01 73.0638 73
-10 -2 -4 1048.73 69.0865 129
-10 2 -4 1181.58 74.2879 138
-10 2 -4 965.182 58.8980 134
-10 -2 -4 1124.48 63.6822 103
-10 2 -4 1006.63 68.7743 104
-10 2 -4 1188.72 71.3947 91
10 -2 5 2632.12 200.837 42
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-10 -2 -5 3156.79 132.810 164
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-10 -2 -5 3252.05 130.976 178
-10 -2 -5 3158.72 132.913 168
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-10 -2 -5 3249.69 134.370 129
10 2 5 3180.77 134.242 73
-10 2 -5 2953.80 134.192 104
-10 -2 -5 3199.56 131.772 91
-10 2 -6 5.64001 30.1999 177
-10 -2 -6 51.9345 30.8973 164
-10 -2 -6 26.0249 27.8097 168
10 2 6 21.8164 26.0223 73
10 2 6 29.9837 31.9641 64
-10 -2 -6 69.7039 29.6078 129
-10 2 -6 62.9265 29.8358 104
-10 -2 -6 60.8007 27.6423 91
-10 -2 -7-19.0099 28.3046 164
-10 -2 -7 19.4974 28.2940 148
10 2 7-5.16291 24.6750 64
-10 2 -7-28.1627 29.4885 138
-10 -2 -7-2.81646 27.6246 134
-10 2 -7 23.4692 28.9293 104
-10 -2 -7-19.3750 25.2496 91
-10 2 -7-5.24957 27.8849 91
-10 -2 -8 399.557 33.8238 138
-10 2 -8 381.082 31.5887 138
-10 -2 -8 391.160 34.5485 134
-10 -2 -8 328.774 31.5126 148
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-10 -2 -8 351.685 30.0861 164
-10 -2 -9 1031.01 47.2834 138
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10 -3 -12 2730.60 99.8003 156
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10 3 -12 2790.11 99.0694 113
10 -3 -12 2589.43 96.9398 111
10 3 -12 2478.87 97.2465 162
10 3 -12 2912.94 101.635 175
10 3 -12 2638.11 100.175 163
10 3 -11 1070.71 55.5624 163
10 -3 -11 1035.41 54.0424 162
10 3 -11 1125.21 57.1836 175
10 3 -11 1100.40 55.1673 162
10 -3 -11 996.879 47.7613 137
10 3 -11 1114.87 52.5409 137
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10 -3 -11 1075.18 56.8616 156
10 -3 -11 1123.43 55.7435 147
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10 -3 -11 1117.90 55.5706 111
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10 3 -10 1170.11 64.6799 175
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10 -3 -10 1360.83 66.8582 147
10 -3 -10 1209.51 58.0118 137
10 3 -10 1105.89 60.6929 137
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10 -3 -10 1271.00 65.5632 111
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10 -3 -10 1071.71 54.7472 92
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-10 3 9 108.517 28.4030 57
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-10 -3 9 75.6784 66.6620 52
-10 3 9 91.8467 24.6872 167
10 -3 -9 122.227 33.4012 162
10 3 -9 146.489 34.3225 175
10 3 -9 147.807 35.3080 163
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10 -3 -9 127.214 37.1686 80
10 -3 -9 84.9185 30.7562 58
10 -3 -9 94.3535 27.1775 137
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10 -3 -9 114.334 32.1159 118
-10 -3 9 137.507 32.9145 105
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10 -3 -9 102.482 27.7692 92
-10 -3 9 45.1838 25.8583 97
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-10 -3 8 4557.16 267.829 52
-10 3 8 4528.14 168.506 167
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10 -3 -8 4495.11 173.045 162
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10 -3 -8 4634.71 176.691 80
10 -3 -8 4363.21 172.078 62
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10 -3 -8 4395.37 177.086 58
-10 -3 8 4425.67 173.286 57
-10 3 8 3893.76 162.254 7
10 -3 -8 4373.62 169.685 137
10 3 -8 4471.92 175.025 137
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10 3 -8 4360.62 175.686 118
-10 -3 8 4192.61 174.556 105
-10 -3 8 4411.77 171.276 112
10 -3 -8 4562.01 179.557 111
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10 -3 -8 4191.42 164.314 92
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-10 -3 7 236.272 83.2966 43
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10 -3 -7 67.2201 104.191 54
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-10 3 7 320.680 41.1433 167
-10 3 7 259.153 39.6595 169
10 -3 -7 289.713 39.2788 162
10 -3 -7 176.004 35.5740 82
10 -3 -7 276.547 44.3643 80
10 -3 -7 267.135 46.5811 62
10 3 -7 260.649 37.7636 75
10 -3 -7 209.044 48.3344 58
10 3 -7 169.296 35.4046 6
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10 -3 -7 195.860 37.3829 137
10 3 -7 203.982 39.4938 137
-10 3 7 244.226 41.3611 131
-10 -3 7 262.127 40.8390 131
10 3 -7 303.528 44.0549 110
10 3 -7 227.954 43.6585 118
-10 -3 7 236.265 37.4872 112
10 3 -7 245.221 36.7532 111
-10 3 7 222.923 40.8175 101
-10 -3 7 252.161 39.2698 88
-10 -3 7 264.694 37.5197 97
-10 3 7 284.569 39.1403 97
-10 -3 6 2172.54 196.472 43
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10 -3 -6 2705.60 115.597 162
10 -3 -6 2596.29 126.577 58
10 -3 -6 2582.14 121.350 80
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10 -3 -6 2510.22 115.359 137
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10 3 -6 2655.08 122.458 118
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10 3 -6 2433.92 110.842 111
10 3 -6 2785.47 123.925 110
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10 -3 -6 2686.95 114.176 82
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10 -3 -5 47.4613 114.077 54
-10 -3 5-21.5285 89.2775 52
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10 -3 -5-27.4617 38.7993 80
10 -3 -5-22.8314 38.1470 67
10 3 -5 29.8726 38.8233 75
10 3 -5 19.6786 28.8527 73
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10 -3 -5 21.7528 34.1401 137
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-10 -3 5-5.50984 21.1825 103
10 3 -5-4.47367 36.8136 110
10 3 -5 37.1791 38.6641 118
-10 -3 5-29.9873 34.5410 112
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-10 -3 5 23.3729 35.6684 88
-10 3 5-3.93654 32.9039 97
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-10 -3 4 1320.73 151.339 43
10 -3 -4 1844.16 201.281 54
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12 -5 -4 3001.33 112.548 111
12 5 -4 3077.54 112.795 110
-12 -5 4 3390.80 112.420 89
-12 5 4 3140.92 112.901 145
-12 -5 3 984.636 49.0069 178
-12 5 3 1059.02 49.4744 169
-12 5 3 1123.20 47.4164 172
-12 5 3 1050.39 49.9760 104
12 -5 -3 946.461 48.7347 111
12 5 -3 997.681 49.0221 110
12 5 -3 1018.04 48.2589 98
-12 -5 3 1135.63 48.5979 89
-12 5 3 951.240 47.9310 145
12 5 -2 27.4177 20.3561 6
-12 5 2 22.3963 16.0443 172
-12 -5 2 38.8047 19.8894 178
-12 5 2 52.6250 17.1863 177
-12 5 2 8.59098 20.4105 169
12 5 -2 38.5416 17.9663 110
12 -5 -2 42.4321 17.3048 111
-12 5 2 6.65131 19.0652 104
12 5 -2 44.9184 19.3071 98
-12 -5 2 6.75522 16.5710 89
-12 5 2 29.6879 18.4185 145
12 5 -1 401.469 28.7270 6
-12 -5 1 292.095 28.2083 168
-12 -5 1 329.444 27.8921 178
-12 5 1 256.939 26.0423 177
-12 5 1 262.392 26.7795 169
-12 5 1 292.239 22.6939 172
12 5 -1 276.964 24.1602 110
-12 5 1 348.695 26.7554 104
12 5 -1 335.609 24.8656 100
12 5 0 9.64147 15.8740 6
-12 -5 0 30.4522 13.2737 129
-12 5 0 28.6345 18.1529 177
-12 -5 0 37.2125 17.0180 168
12 5 0 29.9106 16.7741 100
12 5 0 55.8091 18.5346 98
-12 5 0 48.0606 17.8983 104
-12 -5 -1-11.0443 13.7024 178
-12 5 -1 6.85930 16.2163 177
-12 5 -1-5.36575 16.1588 169
-12 5 -1-3.66344 14.3513 104
12 5 1 13.1514 14.6216 100
12 5 1 16.0347 14.8028 98
13 0 -7 32.1900 18.1457 118
-13 0 7 39.8028 17.7541 169
13 0 -7 33.5490 17.3147 137
-13 0 6 1.78297 19.7365 169
13 0 -6 7.11199 19.5949 137
-13 0 6-17.5696 16.2246 7
13 0 -6-9.56448 17.8380 110
13 0 -6 17.2279 20.4427 118
13 0 -5 1537.88 72.1955 137
13 0 -5 1729.32 72.3794 118
-13 0 5 1645.61 70.1865 7
13 0 -4-15.1719 23.4061 75
-13 0 4 10.5429 16.5251 178
13 0 -4-10.8617 23.9937 137
13 0 -4 27.9589 24.1745 118
-13 0 4-1.99535 22.3282 7
-13 0 3 1173.79 55.3625 178
-13 0 3 1249.71 59.6837 169
-13 0 3 1081.04 52.9601 168
13 0 -3 1074.26 54.7149 118
-13 0 3 1233.73 59.3710 7
13 0 -3 1180.86 60.7668 75
13 0 -2 24.3042 18.4295 118
-13 0 2-10.3549 22.3182 178
-13 0 2 10.4045 22.0060 169
-13 0 2 29.1023 22.1574 168
-13 0 1 2595.92 104.620 178
-13 0 1 2611.77 101.853 169
-13 0 1 2573.84 102.617 168
-13 0 1 2504.85 105.003 7
-13 0 1 2804.68 104.264 91
13 0 -1 2401.02 105.207 75
-13 0 0 22.4672 21.2288 178
-13 0 0-3.81783 22.0828 168
-13 0 0 7.61604 20.2760 91
-13 0 0-3.72592 20.8474 7
13 0 0 6.23950 23.1238 75
13 0 1 684.668 36.1085 110
-13 0 -1 815.567 41.7553 91
-13 0 -1 731.425 38.2095 7
-13 0 -2 6.11233 17.1005 178
13 -1 -7 2380.69 88.0870 118
13 1 -7 2338.30 87.1654 118
13 -1 -7 2192.58 84.7000 137
-13 -1 7 2439.65 87.9798 169
13 -1 -6 2477.64 98.8299 137
13 1 -6 2753.30 102.061 137
-13 -1 6 2639.41 100.866 167
-13 1 6 2742.66 101.451 169
-13 -1 6 2662.11 101.388 169
13 -1 -6 2678.73 101.819 118
13 1 -6 2740.68 100.130 118
13 -1 -6 2572.17 98.4867 110
13 1 -6 2706.35 99.6929 110
13 1 -6 2456.45 96.4802 6
-13 1 6 2246.84 95.0510 7
-13 -1 6 2573.49 95.8131 7
-13 -1 5 70.7112 20.5368 7
-13 1 5 79.0159 21.9622 7
-13 1 5 75.7476 23.0476 169
13 -1 -5 66.3742 20.7158 137
13 1 -5 79.2194 23.0890 137
13 1 -5 54.1984 22.2581 110
13 -1 -5 88.1349 24.1351 118
13 1 -5 78.0763 20.7072 118
-13 1 5 81.7599 16.4613 104
-13 -1 5 71.6267 18.8167 89
-13 1 4 768.542 44.0732 7
-13 -1 4 679.447 42.5101 7
13 -1 -4 811.345 45.3031 75
13 1 -4 731.707 44.1972 75
-13 -1 4 692.407 38.3243 178
-13 -1 4 782.502 44.6551 169
-13 -1 4 630.761 37.0819 168
13 -1 -4 700.272 42.5397 137
13 1 -4 876.024 46.1630 137
13 -1 -4 739.856 43.8893 118
13 1 -4 783.122 41.4266 118
-13 1 4 733.106 37.7392 104
-13 -1 4 736.208 41.0344 89
13 -1 -3 1495.03 68.4986 75
13 1 -3 1303.23 65.9893 75
13 -1 -3 1417.37 63.8946 137
13 -1 -3 1402.93 62.6688 118
13 1 -3 1379.40 58.9514 118
-13 1 3 1286.17 58.6413 104
13 1 -3 1514.05 67.0486 110
-13 1 3 1433.58 65.5658 7
-13 -1 3 1353.09 64.7935 7
-13 1 3 1240.19 61.0824 178
-13 -1 3 1348.65 62.3321 178
-13 1 3 1364.57 66.0496 169
-13 -1 3 1351.24 63.6279 169
-13 -1 3 1472.54 62.2298 168
-13 1 2 2555.23 98.1747 178
-13 -1 2 2658.88 99.3924 178
-13 1 2 2808.69 101.264 169
-13 -1 2 2690.71 97.8318 169
-13 -1 2 2533.16 97.7120 168
13 -1 -2 2434.37 95.0015 118
-13 1 2 2640.26 93.9951 104
13 1 -2 2951.35 102.101 110
-13 -1 1 293.016 31.6700 7
-13 1 1 258.035 30.8239 7
-13 1 1 315.204 30.0166 178
-13 -1 1 256.972 30.1402 178
-13 1 1 288.021 29.1255 169
-13 -1 1 326.614 31.2678 168
13 1 -1 293.425 30.3118 110
-13 1 1 266.266 25.4040 104
-13 1 1 310.236 26.1740 91
13 1 -1 277.375 31.7669 75
-13 1 0 1544.34 70.0195 7
-13 -1 0 1839.24 72.0268 7
-13 1 0 1531.80 65.1547 104
13 1 0 1625.83 69.7790 110
-13 1 0 1591.18 69.0405 91
-13 1 0 1656.73 72.4632 178
-13 -1 0 1589.91 71.9986 178
-13 1 0 1653.48 68.1486 169
-13 -1 0 1755.40 72.6329 168
-13 -1 -1 264.996 27.8439 168
-13 1 -1 308.403 25.8963 91
-13 -1 -1 276.306 26.3275 91
13 1 1 303.901 25.0257 6
-13 1 -1 274.407 24.3684 7
-13 -1 -1 285.523 24.2137 7
-13 -1 -2 1164.64 53.0418 178
-13 -1 -2 1261.00 53.5302 91
13 1 2 1294.77 52.5661 98
-13 1 -2 1166.38 52.2341 91
-13 -2 7 2052.25 78.1978 169
13 -2 -6 800.163 41.2482 118
13 2 -6 774.602 38.4671 118
13 2 -6 805.562 38.8009 110
13 2 -6 870.526 40.7618 137
-13 -2 6 730.298 38.0886 167
-13 2 6 781.486 39.0973 169
13 2 -5 1869.78 77.8612 6
-13 2 5 1976.59 77.3474 7
-13 -2 5 2006.90 77.2821 7
13 2 -5 1814.90 79.7748 137
-13 2 5 1921.62 79.5293 169
-13 -2 5 2076.45 80.4077 169
13 -2 -5 1965.91 80.5815 118
13 2 -5 1851.57 75.5328 118
-13 2 5 1983.92 77.1933 104
13 2 -5 1992.11 79.7719 110
-13 -2 5 1938.15 77.8030 89
-13 -2 4 92.3160 21.5729 7
13 2 -4 147.134 24.6000 6
-13 2 4 130.284 22.4543 7
-13 -2 4 96.4797 18.9616 178
-13 2 4 120.393 23.9457 169
-13 -2 4 157.871 22.9278 169
-13 -2 4 98.0602 20.3707 168
13 -2 -4 137.298 19.7399 137
13 2 -4 145.898 24.3928 137
13 -2 -4 117.001 24.0181 118
13 2 -4 116.716 17.6599 118
-13 2 4 129.190 22.2294 104
13 2 -4 118.232 20.6729 98
-13 -2 4 117.885 22.1695 89
-13 2 3 1129.26 55.2440 7
-13 -2 3 1191.12 55.1949 7
13 2 -3 1097.73 56.1684 75
13 -2 -3 1032.31 49.3689 137
13 2 -3 1201.67 56.3798 137
-13 -2 3 1017.58 52.5670 178
-13 2 3 1073.62 51.0120 177
-13 -2 3 1222.53 52.8244 169
-13 -2 3 1114.18 52.7260 168
13 -2 -3 1182.47 54.7820 118
-13 2 3 1096.04 52.1632 104
13 2 -3 1232.91 56.5436 110
13 2 -3 1080.39 53.7281 98
-13 -2 3 1220.98 55.0786 89
13 -2 -2 1964.87 84.8301 137
-13 -2 2 2331.71 90.6033 178
-13 2 2 2268.85 91.6581 169
-13 -2 2 2142.08 89.6967 168
13 -2 -2 2262.94 87.7049 118
-13 2 2 2227.17 88.2260 104
13 2 -2 2418.55 91.4081 110
13 2 -2 2265.45 91.9420 6
13 -2 -1 46.2806 17.0947 137
13 2 -1 72.2963 20.4421 110
-13 2 1 63.7644 20.6669 104
-13 -2 1 98.7353 22.5727 7
13 2 -1 86.6553 22.8364 6
-13 2 1 38.3601 21.0287 7
-13 -2 1 48.4306 21.4828 178
-13 2 1 65.6994 22.0893 169
-13 -2 1 87.3309 23.0870 168
-13 -2 0 193.125 22.8426 7
13 2 0 238.618 24.8181 6
-13 2 0 228.825 23.0867 7
-13 -2 0 177.896 24.5310 178
-13 2 0 227.700 26.9331 177
-13 2 0 193.580 21.8634 169
-13 -2 0 194.203 24.8157 168
13 2 0 254.127 26.2746 98
13 2 0 180.791 19.8418 110
-13 2 0 186.476 22.7570 104
-13 2 -1 504.643 33.3923 177
-13 -2 -1 529.758 30.7415 91
13 2 1 567.117 32.3687 98
-13 2 -1 445.853 28.5036 104
-13 3 5 10757.0 383.606 169
13 -3 -5 11997.8 386.335 118
-13 3 5 11547.0 384.167 104
13 3 -5 11430.6 385.002 110
-13 -3 5 10809.9 383.986 89
13 3 -4 969.332 43.7665 137
-13 3 4 1029.18 46.8225 169
-13 -3 4 930.187 43.0728 168
13 -3 -4 1068.73 48.4981 118
-13 3 4 939.799 45.5666 104
13 3 -4 994.689 46.8593 110
13 3 -4 919.775 45.8247 6
-13 -3 4 1037.71 45.4649 7
-13 3 3 1686.46 70.7144 7
-13 -3 3 1786.54 71.2876 7
13 3 -3 1587.40 68.1370 137
-13 -3 3 1624.07 68.6337 178
-13 3 3 1811.24 72.4336 169
-13 -3 3 1638.68 69.7652 168
13 -3 -3 1845.48 71.7990 118
-13 3 3 1787.81 70.7201 104
13 3 -3 1695.45 71.1876 110
13 3 -3 1791.37 69.9249 98
-13 -3 3 1823.08 70.8783 89
13 3 -2 819.641 40.6388 6
13 3 -2 618.681 36.4624 137
13 -3 -2 847.087 38.2826 118
-13 3 2 686.322 38.2860 104
13 3 -2 750.806 39.1738 110
13 3 -2 801.110 40.8405 98
-13 -3 2 742.903 39.1181 178
-13 3 2 707.726 36.8482 177
-13 -3 2 753.388 39.5977 168
13 3 -1 3305.62 124.457 6
-13 3 1 3406.24 124.153 7
-13 -3 1 3572.76 124.760 7
-13 3 1 3483.69 123.876 104
13 3 -1 3494.83 122.115 110
13 3 -1 3107.46 122.494 100
-13 -3 1 3432.90 124.578 178
-13 3 1 3254.88 123.197 177
-13 3 1 3194.10 124.284 169
-13 -3 1 3355.59 124.246 168
-13 -3 0 20.3885 13.7468 7
-13 3 0-16.3990 16.7652 177
-13 3 0 2.42187 14.0939 169
-13 3 0-4.87083 14.9125 104
13 3 0 10.5685 14.7528 100
-13 -3 0 26.4478 14.5365 91
13 3 0 8.06622 15.5532 98
0 0 0 0.00 0.00 0
TITL elg_m6 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 10.856360 9.185696 13.310010 90.0000 98.7757 90.0000
ZERR 4.00 0.000067 0.000052 0.000081 0.0000 0.0006 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O S
UNIT 60.00 56.00 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 83885
_shelx_res_file
;
TITL elg_m6 in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 09:21:12 on 19-Jan-2023
CELL 1.54184 10.85636 9.185696 13.31001 90 98.7757 90
ZERR 4 0.00013 0.0001 0.00016 0 0.0012 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O S
UNIT 60 56 8 4 4
L.S. 6
PLAN 10
SIZE 0.1 0.08 0.03
TEMP -173
EQIV $1 1-X,1-Y,1-Z
EQIV $2 2-X,1-Y,1-Z
HTAB C12 N1_$1
HTAB C13 N2_$2
FMAP 2
PLAN 10
ACTA 154
BOND $H
CONF
WGHT 0.034300 0.568100
FVAR 3.35619
N1 3 0.419013 0.651824 0.621670 11.00000 0.01438 0.01564 =
0.01615 -0.00204 0.00307 -0.00047
C2 1 0.498809 0.697545 0.563502 11.00000 0.01551 0.01321 =
0.01445 -0.00155 0.00146 -0.00024
C3 1 0.618173 0.636230 0.564961 11.00000 0.01449 0.01467 =
0.01449 -0.00143 0.00298 -0.00059
C4 1 0.652922 0.517303 0.629229 11.00000 0.01443 0.01468 =
0.01370 -0.00217 0.00189 -0.00003
C4A 1 0.566083 0.464442 0.689414 11.00000 0.01724 0.01595 =
0.01395 -0.00013 0.00336 -0.00046
C5 1 0.593049 0.330447 0.756090 11.00000 0.02012 0.02088 =
0.02028 0.00592 0.00617 0.00219
AFIX 23
H5A 2 0.649271 0.357815 0.818958 11.00000 -1.20000
H5B 2 0.636738 0.257414 0.719674 11.00000 -1.20000
AFIX 0
C6 1 0.475031 0.262264 0.784602 11.00000 0.02426 0.02267 =
0.02561 0.00832 0.01029 0.00128
AFIX 23
H6A 2 0.425966 0.217090 0.723760 11.00000 -1.20000
H6B 2 0.497721 0.185108 0.836031 11.00000 -1.20000
AFIX 0
C7 1 0.396819 0.377966 0.827213 11.00000 0.02772 0.02960 =
0.02421 0.00654 0.01401 0.00287
AFIX 23
H7A 2 0.446984 0.425907 0.886394 11.00000 -1.20000
H7B 2 0.323728 0.331799 0.850455 11.00000 -1.20000
AFIX 0
C8 1 0.353037 0.491131 0.745764 11.00000 0.01914 0.02209 =
0.02198 0.00113 0.00952 0.00051
AFIX 23
H8A 2 0.281165 0.451055 0.699260 11.00000 -1.20000
H8B 2 0.323737 0.578340 0.778891 11.00000 -1.20000
AFIX 0
C8A 1 0.452093 0.536874 0.683919 11.00000 0.01635 0.01664 =
0.01414 -0.00207 0.00375 -0.00172
C9 1 0.359653 0.892442 0.508566 11.00000 0.01669 0.01665 =
0.02914 0.00364 0.00587 0.00456
AFIX 137
H9A 2 0.350748 0.972299 0.459164 11.00000 -1.50000
H9B 2 0.365752 0.932339 0.577434 11.00000 -1.50000
H9C 2 0.286883 0.828279 0.495114 11.00000 -1.50000
AFIX 0
O1 4 0.470915 0.810601 0.499712 11.00000 0.01636 0.01658 =
0.02209 0.00460 0.00551 0.00400
C10 1 0.700923 0.705703 0.505397 11.00000 0.01594 0.01446 =
0.01869 0.00065 0.00248 0.00398
N2 3 0.764022 0.766856 0.457690 11.00000 0.02021 0.02180 =
0.02883 0.00701 0.00969 0.00387
S1 5 0.875676 0.410824 0.741413 11.00000 0.01736 0.02812 =
0.01744 0.00578 0.00170 0.00374
C11 1 0.777533 0.452832 0.630093 11.00000 0.01475 0.01408 =
0.01674 0.00192 0.00199 0.00002
C12 1 0.834777 0.421627 0.547471 11.00000 0.01644 0.01646 =
0.01877 0.00067 0.00356 -0.00003
AFIX 43
H12 2 0.796800 0.437646 0.479223 11.00000 -1.20000
AFIX 0
C13 1 0.956196 0.363124 0.574194 11.00000 0.01678 0.01765 =
0.02630 0.00164 0.00687 0.00187
AFIX 43
H13 2 1.007563 0.334334 0.525951 11.00000 -1.20000
AFIX 0
C14 1 0.990993 0.352773 0.676408 11.00000 0.01517 0.02124 =
0.02915 0.00724 0.00414 0.00286
AFIX 43
H14 2 1.069755 0.317592 0.707976 11.00000 -1.20000
AFIX 0
HKLF 4
REM elg_m6 in P2(1)/n
REM wR2 = 0.0714, GooF = S = 1.068, Restrained GooF = 1.068 for all data
REM R1 = 0.0263 for 2663 Fo > 4sig(Fo) and 0.0272 for all 2774 data
REM 173 parameters refined using 0 restraints
END
WGHT 0.0343 0.5681
REM Highest difference peak 0.280, deepest hole -0.236, 1-sigma level 0.039
Q1 1 0.5797 0.4002 0.7224 11.00000 0.05 0.28
Q2 1 0.4019 0.5106 0.7161 11.00000 0.05 0.28
Q3 1 0.5595 0.6584 0.5573 11.00000 0.05 0.28
Q4 1 0.5066 0.4967 0.6804 11.00000 0.05 0.26
Q5 1 0.6360 0.5821 0.5995 11.00000 0.05 0.25
Q6 1 0.6141 0.4932 0.6638 11.00000 0.05 0.25
Q7 1 0.7207 0.4904 0.6352 11.00000 0.05 0.25
Q8 1 0.5390 0.3000 0.7718 11.00000 0.05 0.24
Q9 1 0.8188 0.4435 0.6774 11.00000 0.05 0.24
Q10 1 0.8980 0.3971 0.5597 11.00000 0.05 0.24
;
_shelx_res_checksum 69293
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.41901(8) 0.65182(10) 0.62167(7) 0.01531(18) Uani d 1 . .
C C2 0.49881(9) 0.69755(11) 0.56350(8) 0.0145(2) Uani d 1 . .
C C3 0.61817(9) 0.63623(11) 0.56496(8) 0.0145(2) Uani d 1 . .
C C4 0.65292(9) 0.51730(11) 0.62923(8) 0.0143(2) Uani d 1 . .
C C4A 0.56608(10) 0.46444(11) 0.68941(8) 0.0156(2) Uani d 1 . .
C C5 0.59305(10) 0.33045(13) 0.75609(8) 0.0201(2) Uani d 1 . .
H H5A 0.649271 0.357815 0.818958 0.024 Uiso calc 1 . .
H H5B 0.636738 0.257414 0.719674 0.024 Uiso calc 1 . .
C C6 0.47503(11) 0.26226(13) 0.78460(9) 0.0235(2) Uani d 1 . .
H H6A 0.425966 0.217090 0.723760 0.028 Uiso calc 1 . .
H H6B 0.497721 0.185108 0.836031 0.028 Uiso calc 1 . .
C C7 0.39682(12) 0.37797(14) 0.82721(9) 0.0261(3) Uani d 1 . .
H H7A 0.446984 0.425907 0.886394 0.031 Uiso calc 1 . .
H H7B 0.323728 0.331799 0.850455 0.031 Uiso calc 1 . .
C C8 0.35304(10) 0.49113(13) 0.74576(9) 0.0204(2) Uani d 1 . .
H H8A 0.281165 0.451055 0.699260 0.024 Uiso calc 1 . .
H H8B 0.323737 0.578340 0.778891 0.024 Uiso calc 1 . .
C C8A 0.45209(10) 0.53687(12) 0.68392(8) 0.0156(2) Uani d 1 . .
C C9 0.35965(10) 0.89244(12) 0.50857(9) 0.0206(2) Uani d 1 . .
H H9A 0.350748 0.972299 0.459164 0.031 Uiso calc 1 . .
H H9B 0.365752 0.932339 0.577434 0.031 Uiso calc 1 . .
H H9C 0.286883 0.828279 0.495114 0.031 Uiso calc 1 . .
O O1 0.47092(7) 0.81060(8) 0.49971(6) 0.01807(17) Uani d 1 . .
C C10 0.70092(10) 0.70570(11) 0.50540(8) 0.0164(2) Uani d 1 . .
N N2 0.76402(9) 0.76686(11) 0.45769(8) 0.0230(2) Uani d 1 . .
S S1 0.87568(2) 0.41082(3) 0.74141(2) 0.02107(9) Uani d 1 . .
C C11 0.77753(9) 0.45283(11) 0.63009(8) 0.0152(2) Uani d 1 . .
C C12 0.83478(10) 0.42163(11) 0.54747(8) 0.0171(2) Uani d 1 . .
H H12 0.796800 0.437646 0.479223 0.021 Uiso calc 1 . .
C C13 0.95620(10) 0.36312(12) 0.57419(9) 0.0199(2) Uani d 1 . .
H H13 1.007563 0.334334 0.525951 0.024 Uiso calc 1 . .
C C14 0.99099(10) 0.35277(12) 0.67641(9) 0.0218(2) Uani d 1 . .
H H14 1.069755 0.317592 0.707976 0.026 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 0.0144(4) 0.0156(4) 0.0161(4) -0.0005(3) 0.0031(3) -0.0020(3)
C2 0.0155(5) 0.0132(5) 0.0144(5) -0.0002(4) 0.0015(4) -0.0016(4)
C3 0.0145(5) 0.0147(5) 0.0145(5) -0.0006(4) 0.0030(4) -0.0014(4)
C4 0.0144(5) 0.0147(5) 0.0137(5) 0.0000(4) 0.0019(4) -0.0022(4)
C4A 0.0172(5) 0.0159(5) 0.0140(5) -0.0005(4) 0.0034(4) -0.0001(4)
C5 0.0201(5) 0.0209(5) 0.0203(5) 0.0022(4) 0.0062(4) 0.0059(4)
C6 0.0243(6) 0.0227(6) 0.0256(6) 0.0013(5) 0.0103(5) 0.0083(5)
C7 0.0277(6) 0.0296(6) 0.0242(6) 0.0029(5) 0.0140(5) 0.0065(5)
C8 0.0191(5) 0.0221(5) 0.0220(5) 0.0005(4) 0.0095(4) 0.0011(4)
C8A 0.0164(5) 0.0166(5) 0.0141(5) -0.0017(4) 0.0038(4) -0.0021(4)
C9 0.0167(5) 0.0167(5) 0.0291(6) 0.0046(4) 0.0059(4) 0.0036(4)
O1 0.0164(4) 0.0166(4) 0.0221(4) 0.0040(3) 0.0055(3) 0.0046(3)
C10 0.0159(5) 0.0145(5) 0.0187(5) 0.0040(4) 0.0025(4) 0.0007(4)
N2 0.0202(5) 0.0218(5) 0.0288(5) 0.0039(4) 0.0097(4) 0.0070(4)
S1 0.01736(14) 0.02812(16) 0.01744(14) 0.00374(10) 0.00170(10) 0.00578(10)
C11 0.0148(5) 0.0141(5) 0.0167(5) 0.0000(4) 0.0020(4) 0.0019(4)
C12 0.0164(5) 0.0165(5) 0.0188(5) 0.0000(4) 0.0036(4) 0.0007(4)
C13 0.0168(5) 0.0176(5) 0.0263(6) 0.0019(4) 0.0069(4) 0.0016(4)
C14 0.0152(5) 0.0212(5) 0.0292(6) 0.0029(4) 0.0041(4) 0.0072(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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 C8A . . 118.12(9) ?
N1 C2 O1 . . 120.82(9) ?
N1 C2 C3 . . 123.40(10) ?
O1 C2 C3 . . 115.75(9) ?
C4 C3 C2 . . 118.70(9) ?
C4 C3 C10 . . 123.38(9) ?
C2 C3 C10 . . 117.78(9) ?
C3 C4 C4A . . 118.20(9) ?
C3 C4 C11 . . 118.57(9) ?
C4A C4 C11 . . 123.23(9) ?
C8A C4A C4 . . 117.96(9) ?
C8A C4A C5 . . 120.43(9) ?
C4 C4A C5 . . 121.58(9) ?
C4A C5 C6 . . 112.56(9) ?
C4A C5 H5A . . 109.1 ?
C6 C5 H5A . . 109.1 ?
C4A C5 H5B . . 109.1 ?
C6 C5 H5B . . 109.1 ?
H5A C5 H5B . . 107.8 ?
C7 C6 C5 . . 110.08(10) y
C7 C6 H6A . . 109.6 ?
C5 C6 H6A . . 109.6 ?
C7 C6 H6B . . 109.6 ?
C5 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.2 ?
C6 C7 C8 . . 110.00(9) y
C6 C7 H7A . . 109.7 ?
C8 C7 H7A . . 109.7 ?
C6 C7 H7B . . 109.7 ?
C8 C7 H7B . . 109.7 ?
H7A C7 H7B . . 108.2 ?
C8A C8 C7 . . 113.99(9) ?
C8A C8 H8A . . 108.8 ?
C7 C8 H8A . . 108.8 ?
C8A C8 H8B . . 108.8 ?
C7 C8 H8B . . 108.8 ?
H8A C8 H8B . . 107.6 ?
N1 C8A C4A . . 123.55(9) ?
N1 C8A C8 . . 113.91(9) y
C4A C8A C8 . . 122.53(10) ?
O1 C9 H9A . . 109.5 ?
O1 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
O1 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C2 O1 C9 . . 117.45(8) ?
N2 C10 C3 . . 176.95(11) ?
C14 S1 C11 . . 92.23(5) ?
C12 C11 C4 . . 127.16(10) ?
C12 C11 S1 . . 110.13(8) ?
C4 C11 S1 . . 122.68(8) ?
C11 C12 C13 . . 113.28(10) ?
C11 C12 H12 . . 123.4 ?
C13 C12 H12 . . 123.4 ?
C14 C13 C12 . . 112.56(10) ?
C14 C13 H13 . . 123.7 ?
C12 C13 H13 . . 123.7 ?
C13 C14 S1 . . 111.79(8) ?
C13 C14 H14 . . 124.1 ?
S1 C14 H14 . . 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 . 1.3156(14) ?
N1 C8A . 1.3563(14) ?
C2 O1 . 1.3463(13) ?
C2 C3 . 1.4104(14) ?
C3 C4 . 1.4032(14) ?
C3 C10 . 1.4353(14) ?
C4 C4A . 1.4130(14) ?
C4 C11 . 1.4752(14) ?
C4A C8A . 1.3971(15) ?
C4A C5 . 1.5195(14) ?
C5 C6 . 1.5252(15) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.5229(16) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.5246(16) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C8A . 1.5102(14) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 O1 . 1.4427(12) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 N2 . 1.1492(15) ?
S1 C14 . 1.7120(12) ?
S1 C11 . 1.7314(11) ?
C11 C12 . 1.3734(15) ?
C12 C13 . 1.4177(15) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.3586(17) ?
C13 H13 . 0.9500 ?
C14 H14 . 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
C12 H12 N1 3_666 0.95 2.65 3.3499(14) 131.2 yes
C13 H13 N2 3_766 0.95 2.63 3.3503(14) 133.4 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
C8A N1 C2 O1 . . . . 179.60(9) ?
C8A N1 C2 C3 . . . . -2.09(15) ?
N1 C2 C3 C4 . . . . 2.08(16) ?
O1 C2 C3 C4 . . . . -179.53(9) ?
N1 C2 C3 C10 . . . . -173.74(9) ?
O1 C2 C3 C10 . . . . 4.65(14) ?
C2 C3 C4 C4A . . . . 0.13(15) ?
C10 C3 C4 C4A . . . . 175.70(9) ?
C2 C3 C4 C11 . . . . 179.62(9) ?
C10 C3 C4 C11 . . . . -4.81(15) ?
C3 C4 C4A C8A . . . . -2.10(15) ?
C11 C4 C4A C8A . . . . 178.44(9) ?
C3 C4 C4A C5 . . . . 176.16(10) ?
C11 C4 C4A C5 . . . . -3.30(16) ?
C8A C4A C5 C6 . . . . 18.12(15) y
C4 C4A C5 C6 . . . . -160.09(10) ?
C4A C5 C6 C7 . . . . -50.80(13) y
C5 C6 C7 C8 . . . . 63.65(13) y
C6 C7 C8 C8A . . . . -42.62(14) y
C2 N1 C8A C4A . . . . -0.11(15) ?
C2 N1 C8A C8 . . . . -178.79(9) ?
C4 C4A C8A N1 . . . . 2.20(16) ?
C5 C4A C8A N1 . . . . -176.07(10) ?
C4 C4A C8A C8 . . . . -179.22(9) ?
C5 C4A C8A C8 . . . . 2.50(16) y
C7 C8 C8A N1 . . . . -171.09(10) ?
C7 C8 C8A C4A . . . . 10.21(15) y
N1 C2 O1 C9 . . . . 9.04(14) ?
C3 C2 O1 C9 . . . . -169.39(9) ?
C3 C4 C11 C12 . . . . -44.17(16) ?
C4A C4 C11 C12 . . . . 135.29(12) ?
C3 C4 C11 S1 . . . . 133.63(9) ?
C4A C4 C11 S1 . . . . -46.91(14) ?
C14 S1 C11 C12 . . . . 0.06(9) ?
C14 S1 C11 C4 . . . . -178.08(9) ?
C4 C11 C12 C13 . . . . 178.59(10) ?
S1 C11 C12 C13 . . . . 0.56(12) ?
C11 C12 C13 C14 . . . . -1.09(14) ?
C12 C13 C14 S1 . . . . 1.11(13) ?
C11 S1 C14 C13 . . . . -0.68(9) ?
_cod_database_fobs_code 2244242