#------------------------------------------------------------------------------
#$Date: 2016-06-11 05:09:49 +0300 (Sat, 11 Jun 2016) $
#$Revision: 183351 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/17/2241714.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_2241714
loop_
_publ_author_name
'Gomes, L\'igia R.'
'Low, John Nicolson'
'Fonseca, Andr\'e'
'Matos, Maria Jo\~ao'
'Borges, Fernanda'
_publ_section_title
;
Crystal structures of three 6-substituted coumarin-3-carboxamide
derivatives
;
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 926
_journal_page_last 932
_journal_paper_doi 10.1107/S2056989016008665
_journal_volume 72
_journal_year 2016
_chemical_formula_iupac 'C18 H15 N O5'
_chemical_formula_moiety 'C18 H15 N O5'
_chemical_formula_sum 'C18 H15 N O5'
_chemical_formula_weight 325.31
_chemical_name_systematic
;
6-Methoxy-N-(3-methoxyphenyl)-2-oxo-2H-chromene-3-carboxamide
;
_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
_cell_angle_alpha 91.874(7)
_cell_angle_beta 100.009(7)
_cell_angle_gamma 113.042(7)
_cell_formula_units_Z 2
_cell_length_a 6.7722(5)
_cell_length_b 8.3098(7)
_cell_length_c 14.4202(13)
_cell_measurement_reflns_used 3630
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.4420
_cell_measurement_theta_min 2.6630
_cell_volume 730.84(11)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2006)
;
_computing_publication_material
;
OSCAIL (McArdle et al., 2004),
SHELXL2014 (Sheldrick, 2015b) and
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
OSCAIL (McArdle et al., 2004),
ShelXle (H\"ubschle et al., 2011) and
SHELXL-2014/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
OSCAIL (McArdle et al., 2004) and
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device 'four-circle \k diffractometer'
_diffrn_measurement_device_type 'Rigaku AFC12 (Right)'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_radiation_monochromator 'Confocal mirrors, HF Varimax'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0331
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 8745
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 27.465
_diffrn_reflns_theta_min 2.680
_exptl_absorpt_coefficient_mu 0.109
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.79232
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.483
_exptl_crystal_description plate
_exptl_crystal_F_000 340
_exptl_crystal_size_max 0.170
_exptl_crystal_size_mid 0.110
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.245
_refine_diff_density_min -0.261
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.159
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 223
_refine_ls_number_reflns 3302
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.159
_refine_ls_R_factor_all 0.0935
_refine_ls_R_factor_gt 0.0710
_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^)+(0.0606P)^2^+0.3539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1414
_refine_ls_wR_factor_ref 0.1518
_reflns_number_gt 2666
_reflns_number_total 3302
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7589sup1.cif
_cod_data_source_block 3
_cod_database_code 2241714
_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 0.982
_shelx_estimated_absorpt_t_max 0.998
_shelx_hkl_file
;
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0 0 2 10599.2 97.2739 6
0 0 2 10706.5 101.366 5
0 0 -2 10533.9 117.231 2
0 0 -3 15093.7 180.160 2
0 0 -3 15107.7 151.417 6
0 0 3 14883.2 162.909 1
0 0 3 14702.5 146.631 5
0 0 3 14947.8 141.721 6
0 0 -3 15148.2 160.597 1
0 0 4 7654.05 137.749 1
0 0 -4 7732.66 126.449 6
0 0 4 7424.35 122.845 5
0 0 -4 7341.63 155.740 2
0 0 4 7568.47 119.881 6
0 0 -4 7046.64 133.561 1
0 0 4 7292.18 151.717 2
0 0 -5 1293.56 68.3606 6
0 0 5 1205.04 67.8152 5
0 0 -5 1103.92 87.8563 2
0 0 5 1196.03 71.9184 1
0 0 -5 1013.08 68.6060 1
0 0 5 1117.87 87.1537 2
0 0 5 1314.25 63.9808 6
0 0 -6 347.338 57.6308 6
0 0 6 299.237 76.0807 2
0 0 -6 259.720 60.4919 1
0 0 6 254.210 63.7411 1
0 0 -6 316.192 83.5385 2
0 0 6 298.598 64.7895 5
0 0 6 328.006 51.5238 6
0 0 -7 23440.0 286.048 6
0 0 7 22998.7 313.107 1
0 0 -7 22334.5 343.045 2
0 0 -7 22397.9 299.549 1
0 0 7 22566.0 269.768 6
0 0 8 20376.5 315.870 1
0 0 8 20703.1 341.452 2
0 0 -8 20639.5 288.462 6
0 0 -8 20997.1 361.990 2
0 0 -9 352.490 90.4117 2
0 0 9 384.347 72.7536 1
0 0 -9 301.675 62.3958 6
0 0 -10 143.213 61.7653 6
0 0 -10 128.222 93.0735 2
0 0 10 229.902 67.0360 1
0 0 11 28.0872 67.0546 1
0 0 -11 75.6744 96.3287 2
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0 0 12 582.266 101.787 1
0 0 -12 797.011 100.803 6
0 0 -12 1001.49 145.220 2
0 0 13 157.081 82.0274 1
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0 0 -13 232.226 83.0341 6
0 0 14 1423.51 140.482 1
0 0 -14 1068.10 155.669 2
0 0 -14 1000.19 120.009 6
0 0 -15 235.422 135.626 2
0 0 -15 215.008 94.6078 6
0 0 15 348.819 106.033 1
0 0 -16-49.2759 91.0924 6
0 0 16 114.661 96.6967 1
0 0 17 231.588 111.881 1
0 0 -17 89.6595 102.431 6
0 0 -18 248.353 123.502 6
0 0 18 332.807 126.042 1
0 -1 18 177.613 115.376 1
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0 1 -17 98.7214 124.843 6
0 -1 17 306.452 114.825 1
0 -1 16 537.676 112.608 1
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0 1 -14 94.4729 93.5096 6
0 1 -13 235.472 91.7368 6
0 -1 13 188.774 88.4035 1
0 -1 12 86.5103 76.1686 1
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0 -1 9 238.814 62.8504 1
0 1 -9 152.176 61.1125 6
0 1 -8 384.094 70.1769 6
0 1 -8 504.246 73.4729 1
0 -1 8 353.745 83.0283 2
0 -1 8 367.000 73.4556 1
0 -1 7 107372. 654.576 1
0 -1 7 105973. 585.974 6
0 1 -7 107002. 628.556 1
0 1 -7 107957. 626.218 6
0 -1 6 5454.74 144.231 1
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0 1 -5 1320.48 75.3786 1
0 1 -5 1580.88 75.6841 6
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0 -1 5 1409.79 90.6191 2
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0 -3 1 122.937 44.4945 7
0 3 -1 254.827 53.6034 7
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6 1 -4 112.008 105.647 1
6 1 -3 1188.07 147.582 1
6 1 -2 349.466 111.094 1
6 1 -1 632.327 122.987 1
6 1 0 2085.02 171.205 1
-6 -1 -1 57.6492 84.2068 6
6 1 1 27.2112 91.1477 1
6 1 2 2836.24 183.468 1
6 1 2 2526.40 172.178 7
6 1 3 985.804 131.165 1
6 1 3 874.921 121.461 7
-6 -1 -3 1073.59 125.234 6
6 1 4 7314.52 263.745 7
-6 -1 -4 8444.88 262.072 6
6 1 5 909.185 138.218 1
6 1 5 883.097 122.907 7
-6 -1 -5 945.139 119.538 6
6 1 6 487.651 120.648 1
6 1 6 616.006 121.931 7
-6 -1 -6 629.979 124.649 6
6 1 7 181.208 104.828 1
-6 -1 -7 201.298 110.758 6
6 1 7 32.0468 99.3596 7
6 1 8 352.607 128.970 1
-6 -1 -8 360.743 118.390 6
6 2 -13 351.617 136.955 6
-6 -2 13 274.852 151.720 3
6 2 -12 230.041 124.417 6
-6 -2 12 301.939 137.335 3
6 2 -11 786.244 145.439 6
-6 -2 11 601.850 149.410 3
6 2 -11 547.714 148.867 1
6 2 -10 412.696 141.383 1
-6 -2 10 621.877 146.201 3
6 2 -9 183.343 127.365 1
-6 -2 9 88.0477 109.680 3
-6 -2 8 1325.01 152.832 3
6 2 -8 935.682 163.086 1
6 2 -7 936.062 154.514 1
-6 -2 7 948.945 138.204 3
6 2 -6 396.589 129.594 1
-6 -2 6 186.341 111.779 3
6 2 -5 53.7119 109.588 1
-6 -2 5 363.663 119.126 3
6 2 -4 800.735 144.198 1
6 2 -3 1421.02 158.218 1
6 2 -2 1210.58 150.290 1
6 2 -1 824.139 131.087 1
6 2 0 36.6514 95.2423 1
6 2 0 168.300 94.1470 7
6 2 1 1484.13 146.810 1
-6 -2 -1 1204.29 130.589 6
6 2 2 2571.10 182.615 7
-6 -2 -2 2987.64 181.846 6
6 2 3 8418.00 301.228 1
-6 -2 -3 7551.34 260.461 6
-6 -2 -4 604.435 123.394 6
6 2 4 489.934 124.922 1
6 2 4 341.016 104.513 7
6 2 5 797.556 135.536 1
6 2 5 606.380 126.288 7
-6 -2 -5 700.449 127.260 6
6 2 6 2590.30 195.123 1
6 2 6 2154.65 184.391 7
-6 -2 -6 2487.09 177.130 6
6 3 -11 237.037 155.215 1
-6 -3 11 850.271 163.279 3
-6 -3 10 962.383 161.434 3
6 3 -10 702.796 170.455 1
6 3 -9 342.728 145.342 1
-6 -3 9 449.854 140.467 3
6 3 -8 346.471 142.787 1
-6 -3 8 445.009 136.322 3
6 3 -7 414.141 139.069 1
-6 -3 7 441.527 135.744 3
6 3 -6 61.8003 118.346 1
-6 -3 6 68.4032 124.229 3
6 3 -5 495.716 135.228 1
6 3 -4 848.191 146.617 1
6 3 -3 12.2330 111.644 1
6 3 -2 128.683 108.225 1
6 3 -2 58.9849 98.6788 7
6 3 -1 951.378 144.947 1
6 3 -1 714.741 138.393 7
6 3 0 152.633 107.004 1
6 3 0 10.4176 97.4897 7
-6 -3 -1 452.396 122.004 6
6 3 1 586.574 118.576 1
6 3 1 502.227 128.187 7
6 3 2 1751.62 165.427 1
-6 -3 -2 1629.00 163.603 6
-6 -3 -3 26.6375 113.057 6
6 3 3 117.339 108.494 7
6 3 3 146.844 112.740 1
6 3 4 1152.25 153.408 1
6 3 4 838.364 148.721 7
-6 -3 -4 1165.94 152.790 6
6 4 -7 183.416 133.413 1
-6 -4 7 35.5151 137.175 3
6 4 -6 331.407 132.867 1
-6 -4 6 662.658 154.806 3
6 4 -5 616.604 143.030 1
6 4 -5 588.115 148.351 7
6 4 -4 194.253 129.733 1
6 4 -4-1.32245 113.987 7
6 4 -3 424.493 146.588 1
6 4 -3 77.9495 114.360 7
6 4 -2 405.752 128.100 1
6 4 -2 313.448 126.887 7
6 4 -1 1014.65 149.227 1
6 4 -1 859.424 151.660 7
6 4 0 678.199 135.981 1
7 -9 -5 274.075 150.490 2
7 -9 -4 285.304 158.122 2
7 -9 -3 369.614 161.811 2
7 -9 -2 297.731 173.242 2
7 -9 -1 3381.54 277.871 2
7 -9 0 256.387 185.327 2
7 -9 1 417.715 181.378 2
7 -9 2 710.831 211.082 2
7 -8 -8 1351.75 184.168 2
7 -8 -7 3523.53 235.285 2
7 -8 -6 331.647 143.054 2
7 -8 -5 242.392 131.189 2
7 -8 -4 238.049 143.748 2
7 -8 -3 2390.79 212.710 2
7 -8 -2 286.326 150.411 2
7 -8 -1 455.716 166.797 2
7 -8 0 569.080 163.225 2
7 -8 1 574.940 171.038 2
7 -8 2 1449.91 214.560 2
7 -8 3 334.834 176.587 2
7 -8 4 325.284 185.168 2
7 -8 5 256.307 189.350 2
-7 7 10 394.341 179.027 4
7 -7 -8 83.7580 106.366 1
7 -7 -8 211.025 126.506 2
7 -7 -7 129.009 109.345 1
7 -7 -7 345.363 132.014 2
7 -7 -6 173.366 112.108 1
7 -7 -6 348.798 126.059 2
7 -7 -5 244.582 103.461 1
7 -7 -5 184.953 114.746 2
7 -7 -4 1280.32 140.771 1
7 -7 -4 1573.90 171.067 2
7 -7 -3 432.309 105.418 1
7 -7 -3 537.458 132.638 2
7 -7 -2 120.410 124.262 2
7 -7 -2 130.204 89.9923 1
7 -7 -1 447.212 139.915 2
7 -7 -1 341.045 89.6350 1
7 -7 0 436.986 146.273 2
7 -7 0 136.464 87.4394 1
7 -7 1 2458.67 154.722 1
7 -7 1 2889.63 240.743 2
7 -7 2 294.131 157.546 2
7 -7 2 87.7406 78.0625 1
7 -7 3 610.694 172.987 2
7 -7 3 253.075 85.1644 1
7 -7 4 810.853 109.050 1
7 -7 4 959.400 181.615 2
7 -7 5 564.546 180.500 2
7 -7 5 242.887 92.1944 1
7 -7 6 186.638 88.8715 1
-7 6 11 278.990 178.066 4
-7 6 10 72.6903 151.517 4
7 -6 -8 154.919 103.487 1
7 -6 -7 157.662 107.322 1
7 -6 -6 970.653 133.371 2
7 -6 -6 986.615 143.581 1
7 -6 -5 2776.46 177.415 2
7 -6 -5 3137.31 197.083 1
7 -6 -4 208.587 101.425 1
7 -6 -4 298.087 118.692 2
7 -6 -3 534.324 107.116 1
7 -6 -3 567.267 139.960 2
7 -6 -2 149.218 108.897 1
7 -6 -2 321.768 126.876 2
7 -6 -1 2790.94 168.569 1
7 -6 -1 2792.23 199.423 2
7 -6 0 406.154 144.675 2
7 -6 0 103.912 87.5617 1
7 -6 1 806.418 121.665 1
7 -6 1 535.368 141.765 2
7 -6 2 299.941 137.405 2
7 -6 2 189.144 82.1778 1
7 -6 3 236.817 132.152 2
7 -6 3 192.071 80.3889 1
7 -6 4 1015.06 114.575 1
7 -6 5 325.351 95.8057 1
7 -6 6 123.006 89.7111 1
7 -6 7 182.551 95.2641 1
-7 5 12 87.0843 165.649 4
-7 5 11 265.903 162.839 4
-7 5 10 134.503 156.812 4
7 -5 -8 370.586 111.957 1
7 -5 -7 209.337 109.474 1
7 -5 -6 411.168 112.661 1
7 -5 -5 398.967 102.233 2
7 -5 -5 41.8911 85.9496 1
7 -5 -4 204.493 101.498 1
7 -5 -4 210.224 102.422 2
7 -5 -3 271.368 116.256 2
7 -5 -3 189.371 100.674 1
7 -5 -2 1986.59 160.946 1
7 -5 -2 2155.35 170.928 2
7 -5 -1 579.663 104.896 1
7 -5 -1 801.805 139.713 2
7 -5 0 361.313 124.913 2
7 -5 0 57.0201 83.9020 1
7 -5 1 565.781 103.123 1
7 -5 1 487.515 134.531 2
7 -5 2 108.778 119.646 2
7 -5 2 161.745 85.1199 1
7 -5 3 1177.07 120.877 1
7 -5 4 152.744 80.6491 1
7 -5 5 126.527 84.2861 1
7 -5 6 430.293 102.891 1
7 -5 7 577.489 108.231 1
7 -5 8 134.716 96.5715 1
-7 4 13 592.792 195.249 4
-7 4 12 229.803 172.983 4
-7 4 11 221.532 160.827 4
-7 4 10 107.280 145.565 4
7 -4 -8 247.010 100.740 1
7 -4 -7 685.842 129.165 1
7 -4 -6 227.438 107.116 1
7 -4 -5 214.134 97.3624 1
7 -4 -4 216.229 101.678 1
7 -4 -3 389.295 107.677 1
7 -4 -3 583.528 114.757 2
7 -4 -2 187.558 99.8229 1
7 -4 -2 320.278 111.839 2
7 -4 -1 804.186 115.117 1
7 -4 -1 1020.92 137.215 2
7 -4 0 305.943 115.329 2
7 -4 0 166.280 98.6946 1
7 -4 1 1838.43 149.116 1
7 -4 2 183.594 88.5255 1
7 -4 3 631.264 111.203 1
7 -4 4 234.760 92.5178 1
7 -4 5 305.913 93.6854 1
7 -4 6 246.302 99.9185 1
7 -4 7 277.694 104.540 1
7 -4 8 153.043 98.6895 1
-7 3 13 164.819 165.960 4
-7 3 12 156.992 158.827 4
-7 3 11 211.719 155.600 4
-7 3 10 312.690 147.847 4
7 -3 -8 434.820 116.568 1
7 -3 -7 927.529 148.556 1
7 -3 -6 340.776 113.276 1
7 -3 -5 336.071 109.903 1
7 -3 -4 1167.43 144.080 1
7 -3 -3 90.0575 94.0482 1
7 -3 -2 161.293 98.7856 1
7 -3 -1 903.238 123.716 1
7 -3 -1 750.849 111.977 2
7 -3 0 864.378 121.514 1
7 -3 1 832.165 115.836 1
7 -3 2 143.336 88.9284 1
7 -3 3 105.181 83.6546 1
7 -3 4 368.496 102.167 1
7 -3 5 273.032 94.6010 1
7 -3 6 124.246 96.2553 1
7 -3 7 177.459 97.5397 1
7 -3 8 90.8438 95.3810 1
-7 2 13 325.188 160.139 4
-7 2 12 84.5830 137.738 4
-7 2 11 715.933 165.125 4
7 -2 -9 391.479 118.977 1
7 -2 -8 244.238 112.373 1
7 -2 -7 993.810 145.947 1
7 -2 -6 242.770 110.752 1
7 -2 -5 967.265 140.838 1
7 -2 -4 188.405 105.254 1
7 -2 -3 145.037 93.8644 1
7 -2 -2 222.818 95.1516 1
7 -2 -1 314.683 98.1532 1
7 -2 0 128.142 94.5231 1
7 -2 1 1002.65 130.679 1
7 -2 2 431.567 108.070 1
7 -2 3 698.781 111.834 1
7 -2 4 254.721 96.4831 1
7 -2 5 336.012 102.237 1
7 -2 6 75.8379 96.4135 1
7 -2 7 511.795 117.270 1
-7 1 12 166.909 148.762 4
7 -1 -10 185.097 122.477 1
-7 1 10 7.71853 102.153 3
7 -1 -9 95.5992 122.854 1
-7 1 9 137.789 100.811 3
7 -1 -8 385.410 148.284 1
-7 1 8 495.076 106.387 3
7 -1 -7 196.501 127.749 1
-7 1 7 77.9792 97.7942 3
7 -1 -6 597.585 143.906 1
7 -1 -5 1083.89 159.038 1
7 -1 -4 330.118 124.266 1
7 -1 -3 61.8854 110.538 1
7 -1 -2 688.303 128.020 1
-7 1 1 35.7567 79.1873 6
7 -1 -1 293.665 116.118 1
-7 1 0 41.2579 74.7254 6
7 -1 0 315.040 116.841 1
7 -1 1 2362.99 193.756 1
-7 1 -1 1741.08 125.615 6
-7 1 -2 143.331 82.5660 6
7 -1 2 183.872 103.601 1
7 -1 3 213.906 102.234 1
-7 1 -3 375.693 95.1268 6
-7 1 -4 189.666 88.8008 6
7 -1 4 25.9350 86.2505 1
7 -1 4 103.308 98.2233 7
7 -1 5 28.6908 87.3146 7
7 -1 5 37.7579 90.3084 1
7 -1 6 115.530 97.9990 1
-7 0 12 153.581 133.034 3
7 0 -11 141.229 142.095 1
-7 0 11 74.4916 128.370 3
7 0 -10 352.502 148.195 1
-7 0 10 309.889 119.609 3
-7 0 9 417.798 123.516 3
7 0 -9 559.648 165.410 1
-7 0 8 673.911 127.465 3
7 0 -8 951.099 170.291 1
7 0 -7 359.921 137.620 1
-7 0 7 294.230 116.161 3
7 0 -6 46.1374 129.293 1
-7 0 6 229.986 111.070 3
7 0 -5 922.315 154.141 1
7 0 -4 387.681 144.598 1
7 0 -3 1665.82 173.356 1
7 0 -2 472.330 133.197 1
-7 0 1 92.5089 88.8358 6
7 0 -1 340.009 128.479 1
-7 0 0-133.044 98.0937 6
7 0 0-10.8139 104.427 1
7 0 1 2489.46 188.909 1
-7 0 -1 2364.64 153.835 6
-7 0 -2 69.7251 96.5195 6
7 0 2-10.3861 103.953 1
7 0 2 47.7677 96.8520 7
7 0 3 763.759 136.908 1
7 0 3 583.079 117.859 7
-7 0 -3 582.566 108.537 6
-7 0 -4 33.5933 94.6063 6
7 0 4 39.6622 101.820 1
7 0 4 142.751 106.666 7
-7 0 -5 181.577 106.881 6
7 0 5 172.345 104.797 7
7 0 5 188.642 117.954 1
7 1 -11 232.107 153.252 1
-7 -1 11 4.13217 126.685 3
7 1 -10 240.741 158.839 1
-7 -1 10 148.646 130.048 3
7 1 -9 289.572 143.874 1
-7 -1 9 77.5301 117.216 3
7 1 -8 122.828 133.891 1
-7 -1 8 329.363 134.628 3
7 1 -7 43.2491 125.661 1
-7 -1 7 375.185 135.696 3
7 1 -6 1123.70 174.099 1
7 1 -5 365.091 141.988 1
7 1 -4 388.796 135.352 1
7 1 -3 265.288 125.504 1
7 1 -2 67.8587 112.152 1
7 1 -1 126.998 111.296 1
-7 -1 0 125.385 104.786 6
7 1 0 9.57455 106.440 1
-7 -1 -1 114.433 109.957 6
7 1 1 157.136 109.835 1
7 1 1 104.765 112.147 7
-7 -1 -2 68.9017 109.161 6
7 1 2 131.437 108.185 1
7 1 2 73.8332 105.767 7
7 1 3 1424.34 165.864 1
7 1 3 1038.10 142.926 7
-7 -1 -3 1260.02 144.377 6
-7 -1 -4 690.877 128.877 6
7 1 4 409.761 118.038 7
7 1 4 585.503 136.489 1
7 2 -8 117.770 140.430 1
-7 -2 8 285.974 143.551 3
7 2 -7 63.8626 130.645 1
-7 -2 7 242.938 141.632 3
7 2 -6 1096.35 173.922 1
7 2 -5 352.675 142.479 1
7 2 -4 329.075 137.742 1
7 2 -3 632.720 148.352 1
7 2 -2 564.779 148.712 1
7 2 -1 1069.52 165.220 1
7 2 -1 592.184 137.006 7
-7 -2 0 48.1369 116.032 6
7 2 0 247.821 125.652 1
7 2 0 138.771 119.305 7
-7 -2 -1-17.8894 113.771 6
7 2 1 253.292 125.736 1
7 2 1 111.003 120.727 7
8 -7 -7 106.963 126.154 1
8 -7 -6 170.829 134.018 1
8 -7 -5 5758.52 278.562 1
8 -7 -4 609.298 150.674 1
8 -7 -3 881.270 139.008 1
8 -7 -2 171.578 105.712 1
8 -7 -1 270.249 157.390 2
8 -7 -1 250.222 107.711 1
8 -7 0 150.553 159.077 2
8 -7 0 111.541 117.791 1
8 -7 1 194.048 179.536 2
8 -7 1 124.725 101.103 1
8 -7 2 173.480 175.275 2
8 -7 2 90.2414 97.2492 1
8 -6 -8 118.191 132.800 1
8 -6 -7 1050.46 167.143 1
8 -6 -6 217.410 122.872 1
8 -6 -5 300.703 123.592 1
8 -6 -4 672.535 139.885 1
8 -6 -3 677.260 129.437 1
8 -6 -2 169.555 100.828 1
8 -6 -1 269.737 115.162 1
8 -6 0 885.122 126.628 1
8 -6 1 301.403 167.467 2
8 -6 1 144.675 106.325 1
8 -6 2 2031.12 163.631 1
8 -6 2 1805.06 215.284 2
8 -6 3 1910.60 157.802 1
8 -6 3 1495.44 211.938 2
8 -5 -10 136.039 133.988 1
8 -5 -9 246.973 138.499 1
8 -5 -8 199.520 131.965 1
8 -5 -7 148.691 124.336 1
8 -5 -6 206.042 126.337 1
8 -5 -5 366.993 122.198 1
8 -5 -4 1218.77 184.976 1
8 -5 -3 8448.07 326.291 1
8 -5 -2 3436.78 225.100 1
8 -5 -1 4003.47 223.815 1
8 -5 0 594.782 121.489 1
8 -5 1 351.640 113.872 1
8 -5 2 131.718 98.1362 1
8 -5 3 256.942 104.601 1
8 -5 4 170.726 105.923 1
8 -4 -10 450.896 151.771 1
8 -4 -9 826.447 175.448 1
8 -4 -8 205.696 133.125 1
8 -4 -7 232.874 120.652 1
8 -4 -6 359.719 130.644 1
8 -4 -5 1637.39 177.488 1
8 -4 -4 188.260 119.777 1
8 -4 -3 625.589 130.696 1
8 -4 -2 698.036 128.439 1
8 -4 -1 1004.01 139.862 1
8 -4 0 192.153 101.514 1
8 -4 1 593.565 132.531 1
8 -4 2 771.834 128.136 1
8 -4 3 85.8774 97.5440 1
8 -4 4 1785.68 162.880 1
8 -3 -10 162.668 137.436 1
8 -3 -9 638.979 167.289 1
8 -3 -8 666.254 158.383 1
8 -3 -7 450.387 135.910 1
8 -3 -6 314.102 130.089 1
8 -3 -5 269.001 122.405 1
8 -3 -4 525.204 140.913 1
8 -3 -3 1124.72 153.229 1
8 -3 -2 1395.64 177.061 1
8 -3 -1 5512.21 272.788 1
8 -3 0 3945.66 231.122 1
8 -3 1 6352.76 295.007 1
8 -3 2 548.427 120.746 1
8 -3 3 143.770 99.5274 1
8 -3 4 199.814 111.523 1
8 -2 -9 211.238 143.113 1
8 -2 -8 665.320 151.842 1
8 -2 -7 1205.65 175.860 1
8 -2 -6 153.776 121.403 1
8 -2 -5 221.484 118.305 1
8 -2 -4 477.959 131.009 1
8 -2 -3 1034.51 155.304 1
8 -2 -2 265.923 112.722 1
8 -2 -1 494.298 126.375 1
8 -2 0 216.372 114.613 1
8 -2 1 1148.51 150.377 1
8 -2 2 235.247 111.610 1
8 -1 -8 335.218 160.612 1
8 -1 -7 1141.50 194.453 1
8 -1 -6 1785.82 208.625 1
8 -1 -5 1360.39 188.257 1
8 -1 -4 462.194 147.666 1
8 -1 -3 698.211 153.560 1
8 -1 -2 208.170 138.340 1
8 -1 -1 1718.82 186.694 1
8 -1 0 882.281 168.663 1
8 -1 1 2136.51 194.106 1
8 0 -5 803.014 168.072 1
8 0 -4 375.657 146.661 1
8 0 -3 238.878 137.278 1
0 0 0 0.00 0.00 0
TITL kat1 in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 6.772228 8.309798 14.420165 91.8738 100.0095 113.0418
ZERR 2.00 0.000463 0.000661 0.001273 0.0068 0.0065 0.0070
LATT 1
SFAC C H N O
UNIT 38.00 36.00 2.00 10.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 35542
_shelx_res_file
;
amf65.res created by SHELXL-2014/7
TITL amf65_a.res in P-1
REM Old TITL kat1 in P-1
REM SHELXT solution in P-1
REM R1 0.152, Rweak 0.012, Alpha 0.046, Orientation as input
REM Formula found by SHELXT: C18 N O5
CELL 0.71073 6.7722 8.3098 14.4202 91.874 100.009 113.042
ZERR 2.000 0.0005 0.0007 0.0013 0.007 0.007 0.007
LATT 1
SFAC C H N O
UNIT 36 30 2 10
Temp -173
size 0.17 0.11 0.02
L.S. 10
BOND $H
HTAB
HTAB N32 O2
EQIV $1 x-1, y, z
HTAB C5 O1_$1
EQIV $2 x+1, y, z
HTAB C8 O6_$2
HTAB C312 O31
conf
LIST 4
acta 50
FMAP 2
PLAN 20
WGHT 0.060600 0.353900
FVAR 4.60591
O1 4 0.775818 0.247646 0.525639 11.00000 0.01695 0.02161 =
0.02805 0.00859 0.00640 0.01117
O2 4 0.949063 0.363074 0.413172 11.00000 0.01894 0.02290 =
0.03018 0.00747 0.00785 0.01091
O6 4 0.049986 0.013240 0.688264 11.00000 0.01926 0.02712 =
0.03126 0.01162 0.01012 0.01145
O31 4 0.404812 0.455226 0.276445 11.00000 0.01692 0.02808 =
0.03154 0.01058 0.00583 0.01013
O313 4 0.533874 0.765585 0.011690 11.00000 0.02622 0.03055 =
0.03182 0.01303 0.00907 0.01684
N32 3 0.759355 0.498548 0.274884 11.00000 0.01760 0.02381 =
0.02667 0.00813 0.00679 0.01157
H32 2 0.871810 0.475539 0.307962 11.00000 0.03165
C2 1 0.782311 0.327034 0.444074 11.00000 0.01864 0.01306 =
0.02544 0.00137 0.00437 0.00510
C3 1 0.589030 0.356681 0.401905 11.00000 0.01719 0.01327 =
0.02520 0.00253 0.00469 0.00688
C4 1 0.412129 0.303784 0.442885 11.00000 0.01820 0.01326 =
0.02678 0.00265 0.00221 0.00758
AFIX 43
H4 2 0.287159 0.323627 0.414726 11.00000 -1.20000
AFIX 0
C4A 1 0.408532 0.218353 0.527921 11.00000 0.01993 0.01265 =
0.02502 0.00096 0.00483 0.00783
C5 1 0.227721 0.157251 0.571419 11.00000 0.01525 0.01720 =
0.02883 0.00164 0.00226 0.00877
AFIX 43
H5 2 0.098678 0.173301 0.545446 11.00000 -1.20000
AFIX 0
C6 1 0.236798 0.073244 0.652454 11.00000 0.01846 0.01621 =
0.02675 0.00207 0.00627 0.00680
C7 1 0.428939 0.054833 0.692508 11.00000 0.02297 0.01866 =
0.02426 0.00522 0.00677 0.00910
AFIX 43
H7 2 0.436155 0.001183 0.749453 11.00000 -1.20000
AFIX 0
C8 1 0.609771 0.114389 0.649715 11.00000 0.01845 0.01751 =
0.02935 0.00405 0.00257 0.00949
AFIX 43
H8 2 0.739878 0.100392 0.676289 11.00000 -1.20000
AFIX 0
C8A 1 0.596270 0.194072 0.568019 11.00000 0.01570 0.01435 =
0.02738 0.00198 0.00691 0.00543
C31 1 0.575938 0.443066 0.311909 11.00000 0.01810 0.01597 =
0.02670 0.00224 0.00353 0.00717
C61 1 0.046506 -0.085169 0.768132 11.00000 0.02577 0.02256 =
0.02899 0.00832 0.01057 0.00919
AFIX 137
H61A 2 -0.097741 -0.123847 0.785141 11.00000 -1.50000
H61B 2 0.159343 -0.010801 0.821920 11.00000 -1.50000
H61C 2 0.075536 -0.188190 0.751980 11.00000 -1.50000
AFIX 0
C311 1 0.791123 0.576644 0.190193 11.00000 0.02063 0.01349 =
0.02539 0.00144 0.00548 0.00514
C312 1 0.643556 0.633716 0.138213 11.00000 0.01899 0.01666 =
0.02926 0.00488 0.00845 0.00766
AFIX 43
H312 2 0.512982 0.621233 0.158816 11.00000 -1.20000
AFIX 0
C313 1 0.688395 0.709315 0.055733 11.00000 0.01895 0.01705 =
0.02832 0.00183 0.00359 0.00725
C314 1 0.876071 0.726345 0.023252 11.00000 0.02564 0.02103 =
0.02617 0.00695 0.00880 0.00879
AFIX 43
H314 2 0.904009 0.776207 -0.033926 11.00000 -1.20000
AFIX 0
C315 1 1.022871 0.668238 0.076842 11.00000 0.01818 0.02525 =
0.03465 0.00602 0.01096 0.00763
AFIX 43
H315 2 1.152950 0.680171 0.055945 11.00000 -1.20000
AFIX 0
C316 1 0.983137 0.594205 0.159118 11.00000 0.02014 0.02159 =
0.03076 0.00444 0.00364 0.00991
AFIX 43
H316 2 1.084647 0.555256 0.194655 11.00000 -1.20000
AFIX 0
C317 1 0.567164 0.843008 -0.074311 11.00000 0.03082 0.02960 =
0.03009 0.01294 0.00693 0.01292
AFIX 137
H31A 2 0.442555 0.871544 -0.100164 11.00000 -1.50000
H31B 2 0.579791 0.759834 -0.120278 11.00000 -1.50000
H31C 2 0.701994 0.950790 -0.061521 11.00000 -1.50000
REM #####
AFIX 0
HKLF 4
REM amf65_a.res in P-1
REM R1 = 0.0710 for 2666 Fo > 4sig(Fo) and 0.0935 for all 3302 data
REM 223 parameters refined using 0 restraints
END
WGHT 0.0606 0.3539
REM Instructions for potential hydrogen bonds
HTAB N32 O2
HTAB C5 O1_$1
HTAB C8 O6_$2
HTAB C312 O31
REM Highest difference peak 0.245, deepest hole -0.261, 1-sigma level 0.056
Q1 1 0.6905 0.3710 0.4321 11.00000 0.05 0.25
Q2 1 0.6104 0.4025 0.3802 11.00000 0.05 0.24
Q3 1 0.4275 0.2777 0.5028 11.00000 0.05 0.23
Q4 1 0.2147 0.0617 0.5910 11.00000 0.05 0.22
Q5 1 -0.1174 0.1311 0.5656 11.00000 0.05 0.21
Q6 1 0.5144 0.2437 0.5582 11.00000 0.05 0.20
Q7 1 0.3765 0.5227 0.2017 11.00000 0.05 0.20
Q8 1 0.5176 0.0844 0.6592 11.00000 0.05 0.19
Q9 1 0.9361 0.2849 0.4788 11.00000 0.05 0.19
Q10 1 0.5624 0.1045 0.5878 11.00000 0.05 0.19
Q11 1 0.4526 -0.0167 0.7947 11.00000 0.05 0.19
Q12 1 0.1879 0.3003 0.3921 11.00000 0.05 0.18
Q13 1 0.5434 0.3660 0.4305 11.00000 0.05 0.18
Q14 1 1.1491 0.5477 0.2776 11.00000 0.05 0.18
Q15 1 0.9332 0.3767 0.3519 11.00000 0.05 0.18
Q16 1 1.1534 0.7865 -0.0732 11.00000 0.05 0.17
Q17 1 0.6814 0.5453 0.1486 11.00000 0.05 0.17
Q18 1 0.8473 0.3775 0.5596 11.00000 0.05 0.17
Q19 1 0.6353 0.1926 0.6243 11.00000 0.05 0.17
Q20 1 0.8511 0.7040 -0.0447 11.00000 0.05 0.17
;
_shelx_res_checksum 99725
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
O O1 0.7758(2) 0.24765(19) 0.52564(10) 0.0207(3) Uani d 1
O O2 0.9491(2) 0.3631(2) 0.41317(11) 0.0227(4) Uani d 1
O O6 0.0500(2) 0.0132(2) 0.68826(11) 0.0244(4) Uani d 1
O O31 0.4048(2) 0.4552(2) 0.27644(11) 0.0249(4) Uani d 1
O O313 0.5339(3) 0.7656(2) 0.01169(11) 0.0272(4) Uani d 1
N N32 0.7594(3) 0.4985(2) 0.27488(13) 0.0212(4) Uani d 1
H H32 0.872(4) 0.476(3) 0.3080(18) 0.032(7) Uiso d 1
C C2 0.7823(3) 0.3270(3) 0.44407(15) 0.0195(5) Uani d 1
C C3 0.5890(3) 0.3567(3) 0.40191(15) 0.0183(4) Uani d 1
C C4 0.4121(3) 0.3038(3) 0.44288(15) 0.0193(5) Uani d 1
H H4 0.2872 0.3236 0.4147 0.023 Uiso calc 1
C C4A 0.4085(3) 0.2184(3) 0.52792(15) 0.0188(5) Uani d 1
C C5 0.2277(3) 0.1573(3) 0.57142(16) 0.0200(5) Uani d 1
H H5 0.0987 0.1733 0.5454 0.024 Uiso calc 1
C C6 0.2368(3) 0.0732(3) 0.65245(15) 0.0203(5) Uani d 1
C C7 0.4289(4) 0.0548(3) 0.69251(16) 0.0214(5) Uani d 1
H H7 0.4362 0.0012 0.7495 0.026 Uiso calc 1
C C8 0.6098(4) 0.1144(3) 0.64972(15) 0.0213(5) Uani d 1
H H8 0.7399 0.1004 0.6763 0.026 Uiso calc 1
C C8A 0.5963(3) 0.1941(3) 0.56802(15) 0.0190(5) Uani d 1
C C31 0.5759(3) 0.4431(3) 0.31191(15) 0.0203(5) Uani d 1
C C61 0.0465(4) -0.0852(3) 0.76813(16) 0.0252(5) Uani d 1
H H61A -0.0977 -0.1238 0.7851 0.038 Uiso calc 1
H H61B 0.1593 -0.0108 0.8219 0.038 Uiso calc 1
H H61C 0.0755 -0.1882 0.7520 0.038 Uiso calc 1
C C311 0.7911(3) 0.5766(3) 0.19019(15) 0.0203(5) Uani d 1
C C312 0.6436(3) 0.6337(3) 0.13821(15) 0.0210(5) Uani d 1
H H312 0.5130 0.6212 0.1588 0.025 Uiso calc 1
C C313 0.6884(3) 0.7093(3) 0.05573(16) 0.0216(5) Uani d 1
C C314 0.8761(4) 0.7263(3) 0.02325(16) 0.0239(5) Uani d 1
H H314 0.9040 0.7762 -0.0339 0.029 Uiso calc 1
C C315 1.0229(4) 0.6682(3) 0.07684(17) 0.0256(5) Uani d 1
H H315 1.1530 0.6802 0.0559 0.031 Uiso calc 1
C C316 0.9831(4) 0.5942(3) 0.15912(16) 0.0239(5) Uani d 1
H H316 1.0846 0.5553 0.1947 0.029 Uiso calc 1
C C317 0.5672(4) 0.8430(3) -0.07431(17) 0.0296(5) Uani d 1
H H31A 0.4426 0.8715 -0.1002 0.044 Uiso calc 1
H H31B 0.5798 0.7598 -0.1203 0.044 Uiso calc 1
H H31C 0.7020 0.9508 -0.0615 0.044 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
O1 0.0169(8) 0.0216(8) 0.0281(8) 0.0112(6) 0.0064(6) 0.0086(6)
O2 0.0189(8) 0.0229(8) 0.0302(9) 0.0109(7) 0.0078(6) 0.0075(6)
O6 0.0193(8) 0.0271(9) 0.0313(9) 0.0115(7) 0.0101(6) 0.0116(7)
O31 0.0169(8) 0.0281(9) 0.0315(9) 0.0101(7) 0.0058(6) 0.0106(7)
O313 0.0262(9) 0.0306(9) 0.0318(9) 0.0168(7) 0.0091(7) 0.0130(7)
N32 0.0176(10) 0.0238(10) 0.0267(10) 0.0116(8) 0.0068(8) 0.0081(8)
C2 0.0186(11) 0.0131(10) 0.0254(11) 0.0051(8) 0.0044(8) 0.0014(8)
C3 0.0172(10) 0.0133(10) 0.0252(11) 0.0069(8) 0.0047(8) 0.0025(8)
C4 0.0182(11) 0.0133(10) 0.0268(12) 0.0076(8) 0.0022(8) 0.0027(8)
C4A 0.0199(11) 0.0126(10) 0.0250(11) 0.0078(8) 0.0048(8) 0.0010(8)
C5 0.0153(10) 0.0172(11) 0.0288(12) 0.0088(8) 0.0023(8) 0.0016(9)
C6 0.0185(11) 0.0162(11) 0.0267(12) 0.0068(9) 0.0063(9) 0.0021(8)
C7 0.0230(12) 0.0187(11) 0.0243(11) 0.0091(9) 0.0068(9) 0.0052(9)
C8 0.0185(11) 0.0175(11) 0.0294(12) 0.0095(9) 0.0026(9) 0.0041(9)
C8A 0.0157(10) 0.0143(10) 0.0274(12) 0.0054(8) 0.0069(8) 0.0020(8)
C31 0.0181(11) 0.0160(11) 0.0267(12) 0.0072(9) 0.0035(9) 0.0022(9)
C61 0.0258(12) 0.0226(12) 0.0290(12) 0.0092(10) 0.0106(9) 0.0083(9)
C311 0.0206(11) 0.0135(10) 0.0254(11) 0.0051(9) 0.0055(8) 0.0014(8)
C312 0.0190(11) 0.0167(11) 0.0293(12) 0.0077(9) 0.0084(9) 0.0049(9)
C313 0.0190(11) 0.0171(11) 0.0283(12) 0.0073(9) 0.0036(9) 0.0018(9)
C314 0.0256(12) 0.0210(12) 0.0262(12) 0.0088(9) 0.0088(9) 0.0070(9)
C315 0.0182(11) 0.0252(12) 0.0346(13) 0.0076(9) 0.0110(9) 0.0060(10)
C316 0.0201(11) 0.0216(12) 0.0308(13) 0.0099(9) 0.0036(9) 0.0044(9)
C317 0.0308(13) 0.0296(13) 0.0301(13) 0.0129(11) 0.0069(10) 0.0129(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 O1 C8A 123.06(16)
C6 O6 C61 117.74(17)
C313 O313 C317 117.52(18)
C31 N32 C311 127.96(19)
C31 N32 H32 114.6(16)
C311 N32 H32 117.4(16)
O2 C2 O1 116.03(18)
O2 C2 C3 126.7(2)
O1 C2 C3 117.27(18)
C4 C3 C2 119.95(19)
C4 C3 C31 117.69(18)
C2 C3 C31 122.35(18)
C3 C4 C4A 121.62(19)
C3 C4 H4 119.2
C4A C4 H4 119.2
C8A C4A C5 118.77(19)
C8A C4A C4 117.53(19)
C5 C4A C4 123.69(19)
C6 C5 C4A 119.93(19)
C6 C5 H5 120.0
C4A C5 H5 120.0
O6 C6 C5 115.76(19)
O6 C6 C7 124.16(19)
C5 C6 C7 120.1(2)
C8 C7 C6 120.5(2)
C8 C7 H7 119.7
C6 C7 H7 119.7
C8A C8 C7 118.6(2)
C8A C8 H8 120.7
C7 C8 H8 120.7
C8 C8A O1 117.40(18)
C8 C8A C4A 122.04(19)
O1 C8A C4A 120.55(19)
O31 C31 N32 124.7(2)
O31 C31 C3 119.63(19)
N32 C31 C3 115.61(18)
O6 C61 H61A 109.5
O6 C61 H61B 109.5
H61A C61 H61B 109.5
O6 C61 H61C 109.5
H61A C61 H61C 109.5
H61B C61 H61C 109.5
C312 C311 C316 120.1(2)
C312 C311 N32 123.3(2)
C316 C311 N32 116.59(19)
C311 C312 C313 119.3(2)
C311 C312 H312 120.3
C313 C312 H312 120.3
O313 C313 C314 124.3(2)
O313 C313 C312 114.19(19)
C314 C313 C312 121.5(2)
C313 C314 C315 118.3(2)
C313 C314 H314 120.9
C315 C314 H314 120.9
C316 C315 C314 121.4(2)
C316 C315 H315 119.3
C314 C315 H315 119.3
C315 C316 C311 119.4(2)
C315 C316 H316 120.3
C311 C316 H316 120.3
O313 C317 H31A 109.5
O313 C317 H31B 109.5
H31A C317 H31B 109.5
O313 C317 H31C 109.5
H31A C317 H31C 109.5
H31B C317 H31C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C2 1.366(2)
O1 C8A 1.379(2)
O2 C2 1.218(2)
O6 C6 1.366(3)
O6 C61 1.432(3)
O31 C31 1.226(3)
O313 C313 1.374(3)
O313 C317 1.428(3)
N32 C31 1.356(3)
N32 C311 1.412(3)
N32 H32 0.92(3)
C2 C3 1.459(3)
C3 C4 1.352(3)
C3 C31 1.509(3)
C4 C4A 1.436(3)
C4 H4 0.9500
C4A C8A 1.394(3)
C4A C5 1.397(3)
C5 C6 1.385(3)
C5 H5 0.9500
C6 C7 1.397(3)
C7 C8 1.391(3)
C7 H7 0.9500
C8 C8A 1.377(3)
C8 H8 0.9500
C61 H61A 0.9800
C61 H61B 0.9800
C61 H61C 0.9800
C311 C312 1.385(3)
C311 C316 1.404(3)
C312 C313 1.388(3)
C312 H312 0.9500
C313 C314 1.388(3)
C314 C315 1.397(3)
C314 H314 0.9500
C315 C316 1.374(3)
C315 H315 0.9500
C316 H316 0.9500
C317 H31A 0.9800
C317 H31B 0.9800
C317 H31C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N32 H32 O2 . 0.92(3) 1.91(3) 2.699(2) 143(2)
C4 H4 O2 1_455 0.95 2.43 3.319(3) 155
C5 H5 O1 1_455 0.95 2.47 3.391(3) 164
C8 H8 O6 1_655 0.95 2.46 3.364(3) 160
C312 H312 O31 . 0.95 2.26 2.868(3) 121
C315 H315 O313 1_655 0.95 2.59 3.536(4) 171
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
_geom_torsion_publ_flag
C8A O1 C2 O2 -178.07(17) ?
C8A O1 C2 C3 0.7(3) ?
O2 C2 C3 C4 177.7(2) ?
O1 C2 C3 C4 -1.0(3) ?
O2 C2 C3 C31 -1.4(3) ?
O1 C2 C3 C31 -179.99(18) ?
C2 C3 C4 C4A 0.1(3) ?
C31 C3 C4 C4A 179.18(18) ?
C3 C4 C4A C8A 1.0(3) ?
C3 C4 C4A C5 -178.2(2) ?
C8A C4A C5 C6 -0.5(3) ?
C4 C4A C5 C6 178.8(2) ?
C61 O6 C6 C5 175.76(18) ?
C61 O6 C6 C7 -4.4(3) ?
C4A C5 C6 O6 -178.04(18) ?
C4A C5 C6 C7 2.2(3) ?
O6 C6 C7 C8 177.8(2) ?
C5 C6 C7 C8 -2.4(3) ?
C6 C7 C8 C8A 1.0(3) ?
C7 C8 C8A O1 -178.30(18) ?
C7 C8 C8A C4A 0.8(3) ?
C2 O1 C8A C8 179.51(19) ?
C2 O1 C8A C4A 0.4(3) ?
C5 C4A C8A C8 -1.0(3) ?
C4 C4A C8A C8 179.69(19) ?
C5 C4A C8A O1 178.01(18) ?
C4 C4A C8A O1 -1.3(3) ?
C311 N32 C31 O31 -1.1(4) ?
C311 N32 C31 C3 177.28(19) ?
C4 C3 C31 O31 -3.4(3) ?
C2 C3 C31 O31 175.63(19) ?
C4 C3 C31 N32 178.15(18) y
C2 C3 C31 N32 -2.8(3) y
C31 N32 C311 C312 10.4(3) y
C31 N32 C311 C316 -169.2(2) y
C316 C311 C312 C313 -0.5(3) ?
N32 C311 C312 C313 179.91(19) ?
C317 O313 C313 C314 1.5(3) ?
C317 O313 C313 C312 -179.27(19) ?
C311 C312 C313 O313 -178.17(19) ?
C311 C312 C313 C314 1.1(3) ?
O313 C313 C314 C315 178.0(2) ?
C312 C313 C314 C315 -1.2(3) ?
C313 C314 C315 C316 0.7(3) ?
C314 C315 C316 C311 -0.1(3) ?
C312 C311 C316 C315 0.0(3) ?
N32 C311 C316 C315 179.6(2) ?
_cod_database_fobs_code 2241714