#------------------------------------------------------------------------------
#$Date: 2025-06-03 21:28:13 +0200 (Tue, 03 Jun 2025) $
#$Revision: 299943 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023482.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_2023482
loop_
_publ_author_name
'Jiang, Christina Yu'
'Staples, Richard J.'
'Biros, Shannon M.'
_publ_section_title
;
Crystal structure of a
bis-4-aza-tetra-cyclo[5.3.2.02,6.08,10]dodec-11-ene-3,5-dione
compound.
;
_journal_coeditor_code NY2012
_journal_issue 'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 425
_journal_page_last 428
_journal_paper_doi 10.1107/S2056989025003500
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C30 H28 N2 O4'
_chemical_formula_moiety 'C30 H28 N2 O4'
_chemical_formula_sum 'C30 H28 N2 O4'
_chemical_formula_weight 480.54
_chemical_name_systematic
4-({3-[(3,5-Dioxo-4-azatetracyclo[5.3.2.0^2,6^.0^8,10^]dodec-11-en-4-yl)methyl]phenyl}methyl)-4-azatetracyclo[5.3.2.0^2,6^.0^8,10^]dodec-11-ene-3,5-dione
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 11.26039(13)
_cell_length_b 12.26667(15)
_cell_length_c 33.0963(3)
_cell_measurement_reflns_used 15558
_cell_measurement_temperature 99.99(10)
_cell_measurement_theta_max 79.2210
_cell_measurement_theta_min 2.6620
_cell_volume 4571.51(9)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.104a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.104a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.104a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009; Bourhis et al.,
2015)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 99.99(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_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 0.0447
_diffrn_reflns_av_unetI/netI 0.0371
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 32235
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 80.028
_diffrn_reflns_theta_min 2.670
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.749
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.824
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.396
_exptl_crystal_description needle
_exptl_crystal_F_000 2032
_exptl_crystal_size_max 0.219
_exptl_crystal_size_mid 0.103
_exptl_crystal_size_min 0.037
_refine_diff_density_max 0.298
_refine_diff_density_min -0.206
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.070
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 325
_refine_ls_number_reflns 4946
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0467
_refine_ls_R_factor_gt 0.0412
_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^)+(0.0560P)^2^+1.9036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1124
_refine_ls_wR_factor_ref 0.1171
_reflns_number_gt 4324
_reflns_number_total 4946
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ny2012.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023482.cif.'
_cod_database_code 2023482
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 2537.75 141.505 29
0 0 3 46.6985 17.7876 29
0 0 4 484.270 42.8643 29
0 0 4 440.104 33.9157 10
0 0 5 34.9007 27.4317 29
0 0 5 41.6887 17.7110 10
0 0 6 355688. 18843.2 29
0 0 6 351797. 18830.1 10
0 0 6 382847. 18847.2 8
0 0 7 17.9147 45.5043 8
0 0 7 11.0509 21.5613 10
0 0 7 32.8211 38.5943 29
0 0 8 87935.2 4708.32 8
0 0 8 88914.4 4686.67 10
0 0 8 91159.2 4705.36 29
0 0 9 7.90163 51.8871 8
0 0 9 3.56941 25.0381 10
0 0 10 211.858 38.1982 10
0 0 10 276.899 62.7385 8
0 0 11-40.0481 56.6927 8
0 0 11 8.88462 28.4130 10
0 0 12 11193.6 624.510 10
0 0 12 12014.5 662.730 8
0 0 13-36.9502 57.9506 8
0 0 14 8365.89 510.077 8
0 0 15 44.5886 66.3459 8
0 0 16 82261.4 4392.31 8
0 0 17 88.9233 81.6460 8
0 0 18 64644.0 3487.03 8
0 0 19 20.9570 73.0938 8
0 0 20 6358.67 446.088 8
0 0 21-48.7141 81.0300 8
0 0 22 418.096 112.062 8
0 0 23 27.8291 77.4338 8
0 0 24 1633.00 118.614 9
0 0 24 1532.68 203.626 8
0 0 24 1532.72 113.463 18
0 0 24 1553.72 114.676 1
0 0 24 1390.28 116.247 6
0 0 24 1588.66 114.990 13
0 0 24 1478.95 117.951 12
0 0 25-7.09952 38.7909 9
0 0 25-31.0064 89.2875 8
0 0 25 25.1933 38.6175 18
0 0 25-35.8907 35.9654 22
0 0 25 6.46593 37.5492 1
0 0 25 7.01758 38.3433 12
0 0 25-6.97291 42.7534 6
0 0 26 22265.1 1158.46 9
0 0 26 21174.4 1151.33 18
0 0 26 21000.1 1144.68 22
0 0 26 20787.7 1151.38 1
0 0 26 20810.0 1155.54 6
0 0 26 21870.8 1152.27 7
0 0 26 21502.5 1156.97 12
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0 0 27 31.1352 46.3202 9
0 0 27 27.5581 44.6787 18
0 0 27 100.587 56.0903 6
0 0 27-22.9358 43.6850 12
0 0 27 34.1192 44.8310 7
0 0 28 98584.3 5143.92 18
0 0 28 95725.6 5135.02 15
0 0 28 95619.8 5147.94 6
0 0 28 99536.2 5143.62 7
0 0 28 99860.6 5148.72 12
0 0 28 96477.8 5148.48 9
0 0 29 189.800 61.0174 9
0 0 29 131.130 50.3578 18
0 0 29 207.473 67.8398 6
0 0 29 93.9504 55.7058 7
0 0 29 96.8354 56.5982 12
0 0 29 256.864 51.6857 15
0 0 30 7191.11 431.167 6
0 0 30 7686.59 426.729 7
0 0 30 7216.44 415.823 15
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0 0 30 7278.35 423.775 18
0 0 31 22.0402 44.3772 18
0 0 31-51.0831 63.3022 6
0 0 31 65.7670 54.0600 7
0 0 31 8.34725 53.0270 9
0 0 31-16.8925 37.6798 15
0 0 32 27632.6 1458.25 7
0 0 32 28372.2 1466.44 6
0 0 32 28241.4 1465.92 9
0 0 32 25410.9 1445.43 15
0 0 33 16.5560 57.7626 6
0 0 33-6.97519 49.2299 7
0 0 33 72.1945 53.7050 9
0 0 33 44.7533 31.4182 15
0 0 34 103.617 60.9065 6
0 0 34 73.0117 49.3262 7
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0 0 34 92.1555 54.6705 9
0 0 35-15.0947 57.7751 6
0 0 35 24.7188 45.0192 7
0 0 35-43.4135 48.7164 9
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0 0 36 10254.1 529.178 11
0 0 36 8596.74 519.473 7
0 0 36 8955.44 529.094 6
0 0 36 9959.92 530.487 9
0 0 37-5.83499 41.4033 11
0 0 37-25.5885 48.9845 6
0 0 37-34.6976 37.6037 7
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0 0 38 63.1318 36.6059 7
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0 -1 -3-5.74461 17.3217 26
0 -1 -4-1.90991 16.7467 26
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0 -1 5-5.50367 16.8175 26
0 -1 -5-5.56664 17.6146 26
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0 -1 9-34.7559 28.2837 10
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0 -1 14 22.8995 29.7959 10
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0 -1 15 24.5712 29.2547 10
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0 -2 -2 131113. 6880.83 26
0 -2 -3 446087. 22561.7 26
0 -2 3 416375. 22560.5 26
0 -2 -4 39958.4 2084.60 26
0 -2 4 38916.8 2083.70 26
0 -2 5 16014.2 849.029 26
0 -2 -5 15619.7 849.120 26
0 -2 -6 57826.2 3081.85 26
0 -2 6 59198.5 3082.20 26
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0 -2 -9 11956.7 647.592 26
0 2 9 12480.0 686.273 29
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0 2 11 132587. 7002.38 29
0 -2 12 31482.6 1683.08 10
0 2 12 31728.4 1722.99 29
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0 -2 14 62024.1 3318.95 10
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0 -2 15 11857.7 663.320 10
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0 -2 16 1103.78 97.1800 10
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0 -2 23 5259.24 325.460 12
0 2 23 6435.02 447.522 8
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0 -2 25 2457.29 166.763 1
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-14 0 0 1537.96 112.825 4
14 0 1-12.6911 16.7240 23
14 0 -1 11.2179 14.7463 23
-14 0 1-13.8883 39.3968 2
-14 0 -1-37.1383 42.6949 2
-14 0 1-15.8156 36.5615 4
-14 0 -1 4.95892 36.6863 4
14 0 -2 1096.75 68.7704 23
14 0 2 1228.66 72.2704 23
-14 0 2 1246.15 91.2322 2
-14 0 -2 1134.27 90.5089 2
-14 0 2 1435.87 97.5838 4
-14 0 -2 1141.73 89.3524 4
14 0 -3-22.4268 11.9948 23
14 0 3-26.5766 17.6355 23
-14 0 3-22.3073 35.4373 2
-14 0 -3-67.5691 38.4980 2
-14 0 3 21.2935 37.5676 4
-14 0 -3 8.70411 31.8909 4
14 0 4 48.2188 17.2183 23
-14 0 4 56.1869 36.2776 2
-14 0 -4 13.1456 33.4528 2
-14 0 4 63.1396 36.1311 4
-14 0 -4 19.5070 27.4489 4
14 0 5 21.2638 16.9829 23
-14 0 5-41.4081 31.2462 2
-14 0 -5-4.21314 33.0035 2
-14 0 5-30.8192 35.0028 4
14 0 6 1061.37 63.6939 23
-14 0 -6 945.027 77.0706 2
-14 0 6 1003.02 83.1965 4
14 0 7 19.6248 15.2380 23
-14 0 -7 11.2336 29.2070 2
-14 0 7-14.0092 31.6379 4
14 0 8 274.722 24.4094 23
-14 0 -8 267.697 38.1308 2
-14 0 8 298.278 41.5797 4
14 0 9-10.0807 12.1909 23
-14 0 -9-18.3172 22.1301 2
-14 0 9 3.87207 27.3172 4
14 1 0-15.0344 13.7785 23
14 -1 0-12.8058 17.9900 23
-14 -1 0-56.5809 40.5562 2
-14 -1 0-4.20985 30.9973 4
-14 1 0-5.42996 39.5656 4
14 1 -1 166.025 17.3040 23
14 1 1 163.561 19.7372 23
14 -1 1 147.417 22.1544 23
14 -1 -1 176.044 20.8280 23
-14 -1 1 203.408 42.9278 2
-14 -1 -1 134.529 39.7719 2
-14 -1 1 145.902 38.8515 4
-14 -1 -1 120.702 33.3381 4
-14 1 1 142.800 45.3505 4
-14 1 -1 233.848 45.5075 4
14 1 2-4.31582 14.4005 23
14 -1 2 3.37219 16.8747 23
14 -1 -2-11.2327 14.6627 23
-14 -1 2-25.5741 37.3674 2
-14 -1 -2-72.9778 40.7535 2
-14 -1 -2-13.9169 25.8743 4
-14 1 2 5.49421 37.8870 4
-14 1 -2-35.8698 39.9630 4
-14 -1 2 4.55228 32.4694 4
14 1 3 636.620 42.9635 23
14 -1 3 775.080 46.1656 23
14 -1 -3 570.912 40.9405 23
-14 -1 3 594.514 59.9269 2
-14 -1 -3 596.555 61.0060 2
-14 1 -3 652.521 63.6897 4
-14 1 3 701.034 70.6577 4
-14 -1 3 605.508 61.3543 4
14 1 4 821.628 47.5583 23
14 -1 4 819.113 48.7864 23
14 -1 -4 589.505 42.6886 23
-14 -1 4 690.399 63.9227 2
-14 -1 -4 590.026 62.7136 2
-14 -1 4 771.193 66.6364 4
-14 1 4 876.926 73.9868 4
-14 1 -4 661.941 64.5745 4
14 1 5 834.261 49.5623 23
14 -1 5 736.403 50.0111 23
-14 -1 -5 791.245 66.6559 2
-14 1 -5 578.419 61.5501 4
-14 -1 5 749.239 67.4263 4
-14 1 5 687.351 72.1285 4
14 -1 6 238.580 24.8115 23
14 1 6 283.685 24.9684 23
-14 -1 -6 194.793 38.1457 2
-14 1 6 287.674 44.6933 4
-14 -1 6 219.586 40.7848 4
-14 1 -6 241.200 35.5340 4
14 1 7 117.698 17.1814 23
14 -1 7 89.1137 17.2683 23
-14 -1 -7 91.9078 29.0498 2
-14 -1 7 133.280 32.6510 4
-14 1 7 109.017 33.5469 4
14 1 8 35.3461 13.7197 23
-14 -1 -8 6.14079 23.2031 2
-14 -1 8 7.70480 26.7464 4
14 1 9 11.7946 11.5510 23
14 -2 0 87.6713 18.1505 23
-14 -2 0 86.0140 32.2138 2
-14 2 0 39.2493 31.9896 2
-14 2 0 82.1273 38.9498 4
14 -2 1 2934.26 158.200 23
14 -2 -1 3030.40 157.502 23
-14 -2 1 2617.66 167.669 2
-14 2 1 2539.50 167.504 2
-14 -2 -1 2746.48 168.275 2
-14 2 -1 2365.55 166.813 2
-14 2 1 3281.97 181.505 4
-14 2 -1 3307.95 181.368 4
14 -2 2 69.9192 17.5018 23
14 -2 -2 79.9955 16.1016 23
-14 -2 2 13.3739 30.9948 2
-14 2 2 27.8016 31.4708 2
-14 -2 -2 20.2008 30.3953 2
-14 2 -2 41.8933 32.4548 2
-14 2 -2 49.4368 35.5737 4
-14 2 2 86.3231 39.3499 4
14 2 3 158.125 16.8509 23
14 -2 3 168.705 20.7501 23
14 -2 -3 172.806 18.4395 23
-14 2 3 94.1795 31.2093 2
-14 -2 -3 133.639 32.1847 2
-14 2 -3 67.8197 29.9997 2
-14 2 -3 142.442 37.0067 4
-14 2 3 148.687 39.6007 4
14 -2 4 539.076 36.2204 23
14 -2 -4 407.720 31.2038 23
14 2 4 477.609 32.3624 23
-14 -2 -4 462.529 44.1808 2
-14 2 -4 453.730 45.6126 2
-14 2 -4 510.281 54.8990 4
14 2 5 111.223 14.6648 23
14 -2 5 98.3822 17.7256 23
-14 -2 -5 28.9799 24.0164 2
-14 2 -5 9.13023 23.2898 2
-14 2 -5 24.6917 28.6386 4
14 2 6 11.5543 11.8074 23
-14 2 -6 22.2709 22.7830 2
-14 2 -6 25.5616 24.7490 4
-14 2 7 736.134 62.1546 4
14 2 7 763.064 46.5941 23
14 -3 0 14.3993 12.4868 23
14 -3 1 103.615 16.0401 23
14 -3 -1 99.5552 15.4953 23
-14 3 -2 957.816 72.6597 4
14 -3 2 929.953 53.7743 23
14 -3 -2 795.417 52.0137 23
-14 3 -3 2288.11 128.418 4
14 -3 3 2119.59 110.857 23
-14 3 4 70.1302 26.4468 4
-14 3 -4 67.0364 28.0595 4
-14 3 -5 295.200 36.0755 4
0 0 0 0.00 0.00 0
TITL CJ_imide_1224A in Pbca
REM Pbca (#61 in standard setting)
CELL 1.54184 11.260386 12.266668 33.096327 90.0000 90.0000 90.0000
ZERR 85.00 0.000130 0.000151 0.000313 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 85.00 85.00 85.00 85.00
REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0
TEMP -173
SIZE 0.04 0.10 0.22
TREF
HKLF 4
END
;
_shelx_hkl_checksum 57454
_shelx_res_file
;
TITL cj_imide_1224a_a.res in Pbca
cj_imide_1224a.res
created by SHELXL-2019/2 at 10:15:12 on 21-Jan-2025
REM Old TITL CJ_imide_1224A in Pbcn #60
REM SHELXT solution in Pbca: R1 0.109, Rweak 0.003, Alpha 0.038
REM 0.304 for 243 systematic absences, Orientation as input
REM Formula found by SHELXT: C31 N O4
CELL 1.54184 11.260386 12.266668 33.096327 90 90 90
ZERR 8 0.00013 0.000151 0.000313 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O
UNIT 240 224 16 32
L.S. 14
PLAN 15
TEMP -173
CONF
BOND
list 4
fmap 2
ACTA
MORE -1
BOND $H
REM
REM
REM
WGHT 0.056000 1.903600
FVAR 2.03317
O1 4 0.655415 0.221607 0.355062 11.00000 0.03002 0.03692 =
0.01706 0.00258 0.00187 -0.00386
O2 4 0.641141 0.241288 0.492489 11.00000 0.03575 0.02847 =
0.01680 -0.00073 -0.00386 -0.00286
N1 3 0.663062 0.251215 0.423582 11.00000 0.02359 0.02373 =
0.01686 0.00191 -0.00132 -0.00094
C1 1 0.628725 0.194527 0.389162 11.00000 0.02075 0.02590 =
0.01742 0.00039 -0.00036 0.00222
C2 1 0.622383 0.204303 0.459079 11.00000 0.02340 0.02270 =
0.01778 0.00227 -0.00135 0.00241
C3 1 0.555546 0.096888 0.401947 11.00000 0.02424 0.02274 =
0.01587 -0.00039 0.00090 0.00112
AFIX 13
H3 2 0.595702 0.028144 0.393166 11.00000 -1.20000
AFIX 0
C4 1 0.552615 0.102840 0.448591 11.00000 0.02516 0.02068 =
0.01508 0.00168 -0.00092 0.00137
AFIX 13
H4 2 0.592615 0.037261 0.460293 11.00000 -1.20000
AFIX 0
C5 1 0.421967 0.108684 0.463640 11.00000 0.02713 0.02244 =
0.01605 0.00062 0.00238 0.00024
AFIX 13
H5 2 0.417830 0.115687 0.493710 11.00000 -1.20000
AFIX 0
C6 1 0.364147 0.204127 0.442901 11.00000 0.02448 0.02167 =
0.02556 -0.00114 0.00287 0.00188
AFIX 43
H6 2 0.328886 0.262805 0.457289 11.00000 -1.20000
AFIX 0
C7 1 0.366528 0.199477 0.402667 11.00000 0.02401 0.02492 =
0.02553 0.00594 -0.00146 0.00184
AFIX 43
H7 2 0.333527 0.254937 0.386074 11.00000 -1.20000
AFIX 0
C8 1 0.425625 0.099426 0.385562 11.00000 0.02577 0.02785 =
0.01485 0.00052 -0.00048 -0.00084
AFIX 13
H8 2 0.423454 0.098893 0.355357 11.00000 -1.20000
AFIX 0
C9 1 0.368138 -0.003438 0.403489 11.00000 0.02701 0.02522 =
0.02081 -0.00281 -0.00031 -0.00257
AFIX 13
H9 2 0.390834 -0.074758 0.391057 11.00000 -1.20000
AFIX 0
C10 1 0.365996 0.001701 0.449093 11.00000 0.02683 0.02414 =
0.01971 0.00237 0.00111 -0.00162
AFIX 13
H10 2 0.387699 -0.066222 0.464081 11.00000 -1.20000
AFIX 0
C11 1 0.251065 0.000563 0.425660 11.00000 0.02652 0.02985 =
0.02570 0.00077 0.00073 -0.00427
AFIX 23
H11A 2 0.204812 0.069108 0.424354 11.00000 -1.20000
H11B 2 0.202722 -0.066814 0.426447 11.00000 -1.20000
AFIX 0
C12 1 0.736407 0.349956 0.422921 11.00000 0.02402 0.02494 =
0.02300 0.00254 -0.00150 -0.00272
AFIX 23
H12A 2 0.785149 0.350056 0.398026 11.00000 -1.20000
H12B 2 0.791177 0.348634 0.446316 11.00000 -1.20000
AFIX 0
C13 1 0.663612 0.453732 0.424393 11.00000 0.02203 0.02275 =
0.02214 0.00186 0.00106 -0.00509
C14 1 0.615286 0.496990 0.389020 11.00000 0.02564 0.02429 =
0.01789 0.00029 0.00211 -0.00347
AFIX 43
H14 2 0.628213 0.460844 0.364018 11.00000 -1.20000
AFIX 0
C15 1 0.548094 0.592834 0.389898 11.00000 0.02284 0.02452 =
0.02088 0.00260 0.00252 -0.00457
C16 1 0.530089 0.645536 0.426673 11.00000 0.02721 0.02421 =
0.02746 -0.00221 0.00347 -0.00229
AFIX 43
H16 2 0.485926 0.711479 0.427569 11.00000 -1.20000
AFIX 0
C17 1 0.576539 0.601923 0.462040 11.00000 0.03503 0.03228 =
0.02082 -0.00628 0.00397 -0.00542
AFIX 43
H17 2 0.562699 0.637477 0.487103 11.00000 -1.20000
AFIX 0
C18 1 0.643006 0.506769 0.460971 11.00000 0.03003 0.02959 =
0.01924 0.00126 -0.00062 -0.00613
AFIX 43
H18 2 0.674638 0.477605 0.485287 11.00000 -1.20000
AFIX 0
C19 1 0.490459 0.635900 0.351694 11.00000 0.02327 0.02629 =
0.02338 0.00418 0.00124 -0.00153
AFIX 23
H19A 2 0.451709 0.574514 0.337436 11.00000 -1.20000
H19B 2 0.427710 0.688583 0.359291 11.00000 -1.20000
AFIX 0
O1A 4 0.543113 0.865023 0.345020 11.00000 0.04076 0.02630 =
0.02338 -0.00447 0.00733 0.00273
O2A 4 0.630972 0.535840 0.289835 11.00000 0.04530 0.02115 =
0.02806 -0.00102 0.00436 0.00234
N1A 3 0.573121 0.689342 0.323885 11.00000 0.02455 0.02132 =
0.01823 0.00065 0.00115 0.00024
C1A 1 0.589956 0.801057 0.322213 11.00000 0.02650 0.02181 =
0.01725 -0.00074 -0.00325 -0.00014
C2A 1 0.635555 0.633859 0.294336 11.00000 0.02649 0.02376 =
0.01851 -0.00048 -0.00236 0.00310
C3A 1 0.671600 0.826687 0.287316 11.00000 0.02555 0.02161 =
0.01719 -0.00151 -0.00059 -0.00127
AFIX 13
H3A 2 0.744287 0.865214 0.297186 11.00000 -1.20000
AFIX 0
C4A 1 0.704975 0.714878 0.269340 11.00000 0.02271 0.02346 =
0.01823 0.00012 -0.00006 0.00206
AFIX 13
H4A 2 0.792121 0.701612 0.272446 11.00000 -1.20000
AFIX 0
C5A 1 0.669558 0.710278 0.223817 11.00000 0.03025 0.02368 =
0.01738 -0.00189 -0.00040 0.00177
AFIX 13
H5A 2 0.689249 0.638089 0.211481 11.00000 -1.20000
AFIX 0
C6A 1 0.538988 0.733664 0.221919 11.00000 0.02847 0.03034 =
0.01856 0.00071 -0.00397 -0.00331
AFIX 43
H6A 2 0.483456 0.684407 0.210359 11.00000 -1.20000
AFIX 0
C7A 1 0.507237 0.828960 0.237733 11.00000 0.02548 0.03253 =
0.02004 0.00373 -0.00156 0.00396
AFIX 43
H7A 2 0.427000 0.852806 0.238485 11.00000 -1.20000
AFIX 0
C8A 1 0.607745 0.896263 0.254353 11.00000 0.03031 0.02152 =
0.01994 0.00122 -0.00014 0.00248
AFIX 13
H8A 2 0.579303 0.967581 0.265335 11.00000 -1.20000
AFIX 0
C9A 1 0.702737 0.911701 0.221649 11.00000 0.03306 0.02711 =
0.01933 0.00244 0.00035 -0.00286
AFIX 13
H9A 2 0.767960 0.964581 0.227680 11.00000 -1.20000
AFIX 0
C10A 1 0.738801 0.803346 0.203763 11.00000 0.02895 0.03103 =
0.01855 0.00038 0.00129 -0.00013
AFIX 13
H10A 2 0.825524 0.791281 0.199034 11.00000 -1.20000
AFIX 0
C11A 1 0.678162 0.888289 0.177847 11.00000 0.03967 0.03123 =
0.01949 0.00350 0.00220 -0.00035
AFIX 23
H11C 2 0.726822 0.926744 0.157413 11.00000 -1.20000
H11D 2 0.594763 0.874818 0.169802 11.00000 -1.20000
AFIX 0
HKLF 4
REM cj_imide_1224a_a.res in Pbca
REM wR2 = 0.1171, GooF = S = 1.070, Restrained GooF = 1.070 for all data
REM R1 = 0.0412 for 4324 Fo > 4sig(Fo) and 0.0467 for all 4946 data
REM 325 parameters refined using 0 restraints
END
WGHT 0.0558 1.9095
REM Highest difference peak 0.298, deepest hole -0.206, 1-sigma level 0.046
Q1 1 0.3958 -0.0118 0.4269 11.00000 0.05 0.30
Q2 1 0.5563 0.0966 0.4236 11.00000 0.05 0.28
Q3 1 0.3803 0.0640 0.4593 11.00000 0.05 0.27
Q4 1 0.6043 0.7263 0.2218 11.00000 0.05 0.27
Q5 1 0.3954 0.1535 0.4561 11.00000 0.05 0.27
Q6 1 0.6465 0.4725 0.4079 11.00000 0.05 0.27
Q7 1 0.6487 0.4754 0.4400 11.00000 0.05 0.26
Q8 1 0.5415 0.6250 0.4063 11.00000 0.05 0.26
Q9 1 0.5271 0.6168 0.3710 11.00000 0.05 0.26
Q10 1 0.7062 0.7652 0.2176 11.00000 0.05 0.25
Q11 1 0.3966 0.1508 0.3919 11.00000 0.05 0.23
Q12 1 0.7055 0.4022 0.4251 11.00000 0.05 0.23
Q13 1 0.5456 0.8002 0.2139 11.00000 0.05 0.22
Q14 1 0.4953 0.1000 0.3921 11.00000 0.05 0.22
Q15 1 0.5506 0.6196 0.4418 11.00000 0.05 0.21
;
_shelx_res_checksum 57160
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.65542(9) 0.22161(9) 0.35506(3) 0.0280(2) Uani d 1 . .
O O2 0.64114(9) 0.24129(8) 0.49249(3) 0.0270(2) Uani d 1 . .
N N1 0.66306(10) 0.25121(9) 0.42358(3) 0.0214(2) Uani d 1 . .
C C1 0.62872(12) 0.19453(11) 0.38916(4) 0.0214(3) Uani d 1 . .
C C2 0.62238(12) 0.20430(11) 0.45908(4) 0.0213(3) Uani d 1 . .
C C3 0.55555(12) 0.09689(11) 0.40195(4) 0.0209(3) Uani d 1 . .
H H3 0.595702 0.028144 0.393166 0.025 Uiso calc 1 . .
C C4 0.55262(12) 0.10284(10) 0.44859(4) 0.0203(3) Uani d 1 . .
H H4 0.592615 0.037261 0.460293 0.024 Uiso calc 1 . .
C C5 0.42197(12) 0.10868(11) 0.46364(4) 0.0219(3) Uani d 1 . .
H H5 0.417830 0.115687 0.493710 0.026 Uiso calc 1 . .
C C6 0.36415(12) 0.20413(11) 0.44290(4) 0.0239(3) Uani d 1 . .
H H6 0.328886 0.262805 0.457289 0.029 Uiso calc 1 . .
C C7 0.36653(12) 0.19948(11) 0.40267(4) 0.0248(3) Uani d 1 . .
H H7 0.333527 0.254937 0.386074 0.030 Uiso calc 1 . .
C C8 0.42562(12) 0.09943(11) 0.38556(4) 0.0228(3) Uani d 1 . .
H H8 0.423454 0.098893 0.355357 0.027 Uiso calc 1 . .
C C9 0.36814(12) -0.00344(11) 0.40349(4) 0.0243(3) Uani d 1 . .
H H9 0.390834 -0.074758 0.391057 0.029 Uiso calc 1 . .
C C10 0.36600(12) 0.00170(11) 0.44909(4) 0.0236(3) Uani d 1 . .
H H10 0.387699 -0.066222 0.464081 0.028 Uiso calc 1 . .
C C11 0.25107(13) 0.00056(12) 0.42566(4) 0.0274(3) Uani d 1 . .
H H11A 0.204812 0.069108 0.424354 0.033 Uiso calc 1 . .
H H11B 0.202722 -0.066814 0.426447 0.033 Uiso calc 1 . .
C C12 0.73641(12) 0.34996(11) 0.42292(4) 0.0240(3) Uani d 1 . .
H H12A 0.785149 0.350056 0.398026 0.029 Uiso calc 1 . .
H H12B 0.791177 0.348634 0.446316 0.029 Uiso calc 1 . .
C C13 0.66361(12) 0.45373(11) 0.42439(4) 0.0223(3) Uani d 1 . .
C C14 0.61529(12) 0.49699(11) 0.38902(4) 0.0226(3) Uani d 1 . .
H H14 0.628213 0.460844 0.364018 0.027 Uiso calc 1 . .
C C15 0.54809(12) 0.59283(11) 0.38990(4) 0.0227(3) Uani d 1 . .
C C16 0.53009(13) 0.64554(12) 0.42667(4) 0.0263(3) Uani d 1 . .
H H16 0.485926 0.711479 0.427569 0.032 Uiso calc 1 . .
C C17 0.57654(14) 0.60192(12) 0.46204(4) 0.0294(3) Uani d 1 . .
H H17 0.562699 0.637477 0.487103 0.035 Uiso calc 1 . .
C C18 0.64301(13) 0.50677(12) 0.46097(4) 0.0263(3) Uani d 1 . .
H H18 0.674638 0.477605 0.485287 0.032 Uiso calc 1 . .
C C19 0.49046(12) 0.63590(11) 0.35169(4) 0.0243(3) Uani d 1 . .
H H19A 0.451709 0.574514 0.337436 0.029 Uiso calc 1 . .
H H19B 0.427710 0.688583 0.359291 0.029 Uiso calc 1 . .
O O1A 0.54311(10) 0.86502(8) 0.34502(3) 0.0302(2) Uani d 1 . .
O O2A 0.63097(10) 0.53584(8) 0.28983(3) 0.0315(2) Uani d 1 . .
N N1A 0.57312(10) 0.68934(9) 0.32389(3) 0.0214(2) Uani d 1 . .
C C1A 0.58996(12) 0.80106(11) 0.32221(4) 0.0219(3) Uani d 1 . .
C C2A 0.63556(12) 0.63386(11) 0.29434(4) 0.0229(3) Uani d 1 . .
C C3A 0.67160(12) 0.82669(11) 0.28732(4) 0.0214(3) Uani d 1 . .
H H3A 0.744287 0.865214 0.297186 0.026 Uiso calc 1 . .
C C4A 0.70497(12) 0.71488(11) 0.26934(4) 0.0215(3) Uani d 1 . .
H H4A 0.792121 0.701612 0.272446 0.026 Uiso calc 1 . .
C C5A 0.66956(13) 0.71028(11) 0.22382(4) 0.0238(3) Uani d 1 . .
H H5A 0.689249 0.638089 0.211481 0.029 Uiso calc 1 . .
C C6A 0.53899(13) 0.73366(12) 0.22192(4) 0.0258(3) Uani d 1 . .
H H6A 0.483456 0.684407 0.210359 0.031 Uiso calc 1 . .
C C7A 0.50724(13) 0.82896(12) 0.23773(4) 0.0260(3) Uani d 1 . .
H H7A 0.427000 0.852806 0.238485 0.031 Uiso calc 1 . .
C C8A 0.60774(13) 0.89626(11) 0.25435(4) 0.0239(3) Uani d 1 . .
H H8A 0.579303 0.967581 0.265335 0.029 Uiso calc 1 . .
C C9A 0.70274(13) 0.91170(12) 0.22165(4) 0.0265(3) Uani d 1 . .
H H9A 0.767960 0.964581 0.227680 0.032 Uiso calc 1 . .
C C10A 0.73880(13) 0.80335(12) 0.20376(4) 0.0262(3) Uani d 1 . .
H H10A 0.825524 0.791281 0.199034 0.031 Uiso calc 1 . .
C C11A 0.67816(15) 0.88829(12) 0.17785(4) 0.0301(3) Uani d 1 . .
H H11C 0.726822 0.926744 0.157413 0.036 Uiso calc 1 . .
H H11D 0.594763 0.874818 0.169802 0.036 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 0.0300(5) 0.0369(6) 0.0171(4) -0.0039(4) 0.0019(4) 0.0026(4)
O2 0.0357(5) 0.0285(5) 0.0168(4) -0.0029(4) -0.0039(4) -0.0007(4)
N1 0.0236(5) 0.0237(5) 0.0169(5) -0.0009(4) -0.0013(4) 0.0019(4)
C1 0.0208(6) 0.0259(6) 0.0174(6) 0.0022(5) -0.0004(5) 0.0004(5)
C2 0.0234(6) 0.0227(6) 0.0178(6) 0.0024(5) -0.0014(5) 0.0023(5)
C3 0.0242(6) 0.0227(6) 0.0159(6) 0.0011(5) 0.0009(5) -0.0004(4)
C4 0.0252(6) 0.0207(6) 0.0151(5) 0.0014(5) -0.0009(5) 0.0017(4)
C5 0.0271(6) 0.0224(6) 0.0161(5) 0.0002(5) 0.0024(5) 0.0006(5)
C6 0.0245(6) 0.0217(6) 0.0256(7) 0.0019(5) 0.0029(5) -0.0011(5)
C7 0.0240(6) 0.0249(6) 0.0255(6) 0.0018(5) -0.0015(5) 0.0059(5)
C8 0.0258(6) 0.0278(7) 0.0149(5) -0.0008(5) -0.0005(5) 0.0005(5)
C9 0.0270(7) 0.0252(6) 0.0208(6) -0.0026(5) -0.0003(5) -0.0028(5)
C10 0.0268(7) 0.0241(6) 0.0197(6) -0.0016(5) 0.0011(5) 0.0024(5)
C11 0.0265(7) 0.0298(7) 0.0257(6) -0.0043(5) 0.0007(5) 0.0008(5)
C12 0.0240(6) 0.0249(7) 0.0230(6) -0.0027(5) -0.0015(5) 0.0025(5)
C13 0.0220(6) 0.0227(6) 0.0221(6) -0.0051(5) 0.0011(5) 0.0019(5)
C14 0.0256(6) 0.0243(6) 0.0179(6) -0.0035(5) 0.0021(5) 0.0003(5)
C15 0.0228(6) 0.0245(6) 0.0209(6) -0.0046(5) 0.0025(5) 0.0026(5)
C16 0.0272(7) 0.0242(7) 0.0275(7) -0.0023(5) 0.0035(5) -0.0022(5)
C17 0.0350(7) 0.0323(7) 0.0208(6) -0.0054(6) 0.0040(5) -0.0063(5)
C18 0.0300(7) 0.0296(7) 0.0192(6) -0.0061(6) -0.0006(5) 0.0013(5)
C19 0.0233(6) 0.0263(6) 0.0234(6) -0.0015(5) 0.0012(5) 0.0042(5)
O1A 0.0408(6) 0.0263(5) 0.0234(5) 0.0027(4) 0.0073(4) -0.0045(4)
O2A 0.0453(6) 0.0211(5) 0.0281(5) 0.0023(4) 0.0044(4) -0.0010(4)
N1A 0.0245(5) 0.0213(5) 0.0182(5) 0.0002(4) 0.0012(4) 0.0006(4)
C1A 0.0265(6) 0.0218(6) 0.0173(6) -0.0001(5) -0.0032(5) -0.0007(5)
C2A 0.0265(6) 0.0238(6) 0.0185(6) 0.0031(5) -0.0024(5) -0.0005(5)
C3A 0.0255(6) 0.0216(6) 0.0172(6) -0.0013(5) -0.0006(5) -0.0015(5)
C4A 0.0227(6) 0.0235(6) 0.0182(6) 0.0021(5) -0.0001(5) 0.0001(5)
C5A 0.0302(7) 0.0237(6) 0.0174(6) 0.0018(5) -0.0004(5) -0.0019(5)
C6A 0.0285(7) 0.0303(7) 0.0186(6) -0.0033(5) -0.0040(5) 0.0007(5)
C7A 0.0255(7) 0.0325(7) 0.0200(6) 0.0040(6) -0.0016(5) 0.0037(5)
C8A 0.0303(7) 0.0215(6) 0.0199(6) 0.0025(5) -0.0001(5) 0.0012(5)
C9A 0.0331(7) 0.0271(7) 0.0193(6) -0.0029(6) 0.0003(5) 0.0024(5)
C10A 0.0289(7) 0.0310(7) 0.0185(6) -0.0001(6) 0.0013(5) 0.0004(5)
C11A 0.0397(8) 0.0312(7) 0.0195(6) -0.0004(6) 0.0022(6) 0.0035(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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.1175
1 0 0 0.1001
6 0 -12 0.0890
5 -1 16 0.0675
0 8 0 0.0346
0 -8 0 0.0019
0 0 21 0.0503
0 0 -21 0.0524
-6 0 -12 0.1003
-5 -1 14 0.0934
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
C1 N1 C12 . . 123.91(11) ?
C2 N1 C1 . . 113.28(11) ?
C2 N1 C12 . . 122.80(11) ?
O1 C1 N1 . . 123.80(13) ?
O1 C1 C3 . . 127.65(12) ?
N1 C1 C3 . . 108.55(10) ?
O2 C2 N1 . . 124.02(12) ?
O2 C2 C4 . . 127.39(12) ?
N1 C2 C4 . . 108.59(11) ?
C1 C3 H3 . . 109.9 ?
C1 C3 C4 . . 104.68(10) ?
C1 C3 C8 . . 113.41(10) ?
C4 C3 H3 . . 109.9 ?
C4 C3 C8 . . 109.03(10) ?
C8 C3 H3 . . 109.9 ?
C2 C4 C3 . . 104.89(10) ?
C2 C4 H4 . . 109.8 ?
C2 C4 C5 . . 112.34(10) ?
C3 C4 H4 . . 109.8 ?
C3 C4 C5 . . 110.02(10) ?
C5 C4 H4 . . 109.8 ?
C4 C5 H5 . . 111.5 ?
C6 C5 C4 . . 107.40(10) ?
C6 C5 H5 . . 111.5 ?
C6 C5 C10 . . 110.16(11) ?
C10 C5 C4 . . 104.41(10) ?
C10 C5 H5 . . 111.5 ?
C5 C6 H6 . . 122.8 ?
C7 C6 C5 . . 114.43(12) ?
C7 C6 H6 . . 122.8 ?
C6 C7 H7 . . 122.6 ?
C6 C7 C8 . . 114.78(12) ?
C8 C7 H7 . . 122.6 ?
C3 C8 H8 . . 111.7 ?
C7 C8 C3 . . 107.44(11) ?
C7 C8 H8 . . 111.7 ?
C7 C8 C9 . . 109.73(11) ?
C9 C8 C3 . . 104.14(10) ?
C9 C8 H8 . . 111.7 ?
C8 C9 H9 . . 116.8 ?
C10 C9 C8 . . 110.98(11) ?
C10 C9 H9 . . 116.8 ?
C11 C9 C8 . . 121.91(12) ?
C11 C9 H9 . . 116.8 ?
C11 C9 C10 . . 59.94(9) ?
C5 C10 H10 . . 117.2 ?
C9 C10 C5 . . 110.05(11) ?
C9 C10 H10 . . 117.2 ?
C11 C10 C5 . . 121.46(12) ?
C11 C10 C9 . . 59.99(9) ?
C11 C10 H10 . . 117.2 ?
C9 C11 H11A . . 117.8 ?
C9 C11 H11B . . 117.8 ?
C10 C11 C9 . . 60.07(9) ?
C10 C11 H11A . . 117.8 ?
C10 C11 H11B . . 117.8 ?
H11A C11 H11B . . 114.9 ?
N1 C12 H12A . . 109.0 ?
N1 C12 H12B . . 109.0 ?
N1 C12 C13 . . 112.89(11) ?
H12A C12 H12B . . 107.8 ?
C13 C12 H12A . . 109.0 ?
C13 C12 H12B . . 109.0 ?
C14 C13 C12 . . 120.23(12) ?
C18 C13 C12 . . 120.68(12) ?
C18 C13 C14 . . 119.09(13) ?
C13 C14 H14 . . 119.6 ?
C13 C14 C15 . . 120.87(12) ?
C15 C14 H14 . . 119.6 ?
C14 C15 C19 . . 120.48(12) ?
C16 C15 C14 . . 119.15(12) ?
C16 C15 C19 . . 120.31(13) ?
C15 C16 H16 . . 119.9 ?
C17 C16 C15 . . 120.18(14) ?
C17 C16 H16 . . 119.9 ?
C16 C17 H17 . . 119.8 ?
C18 C17 C16 . . 120.38(13) ?
C18 C17 H17 . . 119.8 ?
C13 C18 H18 . . 119.8 ?
C17 C18 C13 . . 120.32(13) ?
C17 C18 H18 . . 119.8 ?
C15 C19 H19A . . 108.7 ?
C15 C19 H19B . . 108.7 ?
H19A C19 H19B . . 107.6 ?
N1A C19 C15 . . 114.09(11) ?
N1A C19 H19A . . 108.7 ?
N1A C19 H19B . . 108.7 ?
C1A N1A C19 . . 123.74(11) ?
C2A N1A C19 . . 123.18(11) ?
C2A N1A C1A . . 112.90(11) ?
O1A C1A N1A . . 123.87(13) ?
O1A C1A C3A . . 127.44(12) ?
N1A C1A C3A . . 108.67(11) ?
O2A C2A N1A . . 123.57(13) ?
O2A C2A C4A . . 127.37(12) ?
N1A C2A C4A . . 109.05(11) ?
C1A C3A H3A . . 110.3 ?
C1A C3A C4A . . 104.98(10) ?
C1A C3A C8A . . 111.61(11) ?
C4A C3A H3A . . 110.3 ?
C4A C3A C8A . . 109.21(10) ?
C8A C3A H3A . . 110.3 ?
C2A C4A C3A . . 104.35(10) ?
C2A C4A H4A . . 110.1 ?
C2A C4A C5A . . 111.89(11) ?
C3A C4A H4A . . 110.1 ?
C3A C4A C5A . . 110.04(10) ?
C5A C4A H4A . . 110.1 ?
C4A C5A H5A . . 111.7 ?
C6A C5A C4A . . 106.52(11) ?
C6A C5A H5A . . 111.7 ?
C6A C5A C10A . . 109.76(11) ?
C10A C5A C4A . . 105.14(11) ?
C10A C5A H5A . . 111.7 ?
C5A C6A H6A . . 122.7 ?
C7A C6A C5A . . 114.54(13) ?
C7A C6A H6A . . 122.7 ?
C6A C7A H7A . . 122.5 ?
C6A C7A C8A . . 115.08(13) ?
C8A C7A H7A . . 122.5 ?
C3A C8A H8A . . 111.8 ?
C7A C8A C3A . . 107.58(11) ?
C7A C8A H8A . . 111.8 ?
C7A C8A C9A . . 109.53(11) ?
C9A C8A C3A . . 103.86(11) ?
C9A C8A H8A . . 111.8 ?
C8A C9A H9A . . 116.8 ?
C10A C9A C8A . . 110.82(11) ?
C10A C9A H9A . . 116.8 ?
C11A C9A C8A . . 121.91(13) ?
C11A C9A H9A . . 116.8 ?
C11A C9A C10A . . 60.24(9) ?
C5A C10A H10A . . 117.0 ?
C9A C10A C5A . . 110.41(11) ?
C9A C10A H10A . . 117.0 ?
C9A C10A C11A . . 59.65(9) ?
C11A C10A C5A . . 121.92(13) ?
C11A C10A H10A . . 117.0 ?
C9A C11A C10A . . 60.11(9) ?
C9A C11A H11C . . 117.8 ?
C9A C11A H11D . . 117.8 ?
C10A C11A H11C . . 117.8 ?
C10A C11A H11D . . 117.8 ?
H11C C11A H11D . . 114.9 ?
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
O1 C1 . 1.2142(16) ?
O2 C2 . 1.2137(16) ?
N1 C1 . 1.3895(17) ?
N1 C2 . 1.3861(16) ?
N1 C12 . 1.4662(17) ?
C1 C3 . 1.5141(18) ?
C2 C4 . 1.5122(18) ?
C3 H3 . 1.0000 ?
C3 C4 . 1.5458(17) ?
C3 C8 . 1.5605(18) ?
C4 H4 . 1.0000 ?
C4 C5 . 1.5548(18) ?
C5 H5 . 1.0000 ?
C5 C6 . 1.5052(18) ?
C5 C10 . 1.5334(18) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.333(2) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.5065(19) ?
C8 H8 . 1.0000 ?
C8 C9 . 1.5373(19) ?
C9 H9 . 1.0000 ?
C9 C10 . 1.5108(18) ?
C9 C11 . 1.5095(19) ?
C10 H10 . 1.0000 ?
C10 C11 . 1.509(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C12 C13 . 1.5149(19) ?
C13 C14 . 1.3958(18) ?
C13 C18 . 1.3938(19) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.3984(19) ?
C15 C16 . 1.3930(19) ?
C15 C19 . 1.5162(18) ?
C16 H16 . 0.9500 ?
C16 C17 . 1.389(2) ?
C17 H17 . 0.9500 ?
C17 C18 . 1.387(2) ?
C18 H18 . 0.9500 ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C19 N1A . 1.4640(17) ?
O1A C1A . 1.2098(17) ?
O2A C2A . 1.2127(17) ?
N1A C1A . 1.3845(17) ?
N1A C2A . 1.3834(17) ?
C1A C3A . 1.5093(18) ?
C2A C4A . 1.5110(19) ?
C3A H3A . 1.0000 ?
C3A C4A . 1.5415(18) ?
C3A C8A . 1.5606(18) ?
C4A H4A . 1.0000 ?
C4A C5A . 1.5596(17) ?
C5A H5A . 1.0000 ?
C5A C6A . 1.499(2) ?
C5A C10A . 1.5336(19) ?
C6A H6A . 0.9500 ?
C6A C7A . 1.330(2) ?
C7A H7A . 0.9500 ?
C7A C8A . 1.505(2) ?
C8A H8A . 1.0000 ?
C8A C9A . 1.5335(19) ?
C9A H9A . 1.0000 ?
C9A C10A . 1.511(2) ?
C9A C11A . 1.5035(18) ?
C10A H10A . 1.0000 ?
C10A C11A . 1.512(2) ?
C11A H11C . 0.9900 ?
C11A H11D . 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
C3A H3A O2A ? ? 8_765 1.00 2.53 3.3958(17) 144 yes
C9A H9A O2A . . 8_765 1.00 2.51 3.3041(17) 136 yes
C9 H9 O1A . . 1_545 1.00 2.41 3.1985(17) 135 yes
C7A H7A O2A . . 3_655 0.95 2.52 3.1135(18) 121 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
O1 C1 C3 C4 . . . . 179.09(13) ?
O1 C1 C3 C8 . . . . -62.18(18) ?
O2 C2 C4 C3 . . . . 178.79(13) ?
O2 C2 C4 C5 . . . . 59.30(17) ?
N1 C1 C3 C4 . . . . -0.66(14) ?
N1 C1 C3 C8 . . . . 118.07(11) ?
N1 C2 C4 C3 . . . . -0.93(14) ?
N1 C2 C4 C5 . . . . -120.42(11) ?
N1 C12 C13 C14 . . . . -83.59(15) ?
N1 C12 C13 C18 . . . . 95.83(15) ?
C1 N1 C2 O2 . . . . -179.17(13) ?
C1 N1 C2 C4 . . . . 0.56(15) ?
C1 N1 C12 C13 . . . . 95.96(15) ?
C1 C3 C4 C2 . . . . 0.94(13) ?
C1 C3 C4 C5 . . . . 121.97(11) ?
C1 C3 C8 C7 . . . . -61.47(13) ?
C1 C3 C8 C9 . . . . -177.84(10) ?
C2 N1 C1 O1 . . . . -179.68(13) ?
C2 N1 C1 C3 . . . . 0.08(15) ?
C2 N1 C12 C13 . . . . -84.97(15) ?
C2 C4 C5 C6 . . . . 61.26(13) ?
C2 C4 C5 C10 . . . . 178.23(10) ?
C3 C4 C5 C6 . . . . -55.19(13) ?
C3 C4 C5 C10 . . . . 61.77(12) ?
C3 C8 C9 C10 . . . . 62.45(13) ?
C3 C8 C9 C11 . . . . 129.29(12) ?
C4 C3 C8 C7 . . . . 54.72(13) ?
C4 C3 C8 C9 . . . . -61.65(12) ?
C4 C5 C6 C7 . . . . 57.67(15) ?
C4 C5 C10 C9 . . . . -62.34(13) ?
C4 C5 C10 C11 . . . . -128.70(12) ?
C5 C6 C7 C8 . . . . 0.46(18) ?
C5 C10 C11 C9 . . . . 96.36(13) ?
C6 C5 C10 C9 . . . . 52.70(14) ?
C6 C5 C10 C11 . . . . -13.66(16) ?
C6 C7 C8 C3 . . . . -58.46(15) ?
C6 C7 C8 C9 . . . . 54.16(16) ?
C7 C8 C9 C10 . . . . -52.31(14) ?
C7 C8 C9 C11 . . . . 14.54(17) ?
C8 C3 C4 C2 . . . . -120.71(11) ?
C8 C3 C4 C5 . . . . 0.32(14) ?
C8 C9 C10 C5 . . . . 0.10(15) ?
C8 C9 C10 C11 . . . . 115.61(13) ?
C8 C9 C11 C10 . . . . -97.29(13) ?
C10 C5 C6 C7 . . . . -55.47(16) ?
C11 C9 C10 C5 . . . . -115.51(13) ?
C12 N1 C1 O1 . . . . -0.5(2) ?
C12 N1 C1 C3 . . . . 179.24(12) ?
C12 N1 C2 O2 . . . . 1.7(2) ?
C12 N1 C2 C4 . . . . -178.61(11) ?
C12 C13 C14 C15 . . . . -179.88(12) ?
C12 C13 C18 C17 . . . . 179.82(13) ?
C13 C14 C15 C16 . . . . 0.3(2) ?
C13 C14 C15 C19 . . . . -176.71(12) ?
C14 C13 C18 C17 . . . . -0.8(2) ?
C14 C15 C16 C17 . . . . -1.2(2) ?
C14 C15 C19 N1A . . . . -76.21(16) ?
C15 C16 C17 C18 . . . . 1.2(2) ?
C15 C19 N1A C1A . . . . -97.03(15) ?
C15 C19 N1A C2A . . . . 88.29(15) ?
C16 C15 C19 N1A . . . . 106.82(14) ?
C16 C17 C18 C13 . . . . -0.2(2) ?
C18 C13 C14 C15 . . . . 0.7(2) ?
C19 C15 C16 C17 . . . . 175.77(13) ?
C19 N1A C1A O1A . . . . 4.3(2) ?
C19 N1A C1A C3A . . . . -174.23(11) ?
C19 N1A C2A O2A . . . . -2.9(2) ?
C19 N1A C2A C4A . . . . 175.83(11) ?
O1A C1A C3A C4A . . . . 179.52(13) ?
O1A C1A C3A C8A . . . . -62.29(18) ?
O2A C2A C4A C3A . . . . 176.86(14) ?
O2A C2A C4A C5A . . . . 57.92(19) ?
N1A C1A C3A C4A . . . . -2.04(14) ?
N1A C1A C3A C8A . . . . 116.15(12) ?
N1A C2A C4A C3A . . . . -1.85(14) ?
N1A C2A C4A C5A . . . . -120.80(12) ?
C1A N1A C2A O2A . . . . -178.14(13) ?
C1A N1A C2A C4A . . . . 0.63(15) ?
C1A C3A C4A C2A . . . . 2.29(13) ?
C1A C3A C4A C5A . . . . 122.48(11) ?
C1A C3A C8A C7A . . . . -62.90(14) ?
C1A C3A C8A C9A . . . . -178.96(11) ?
C2A N1A C1A O1A . . . . 179.45(13) ?
C2A N1A C1A C3A . . . . 0.93(15) ?
C2A C4A C5A C6A . . . . 58.52(14) ?
C2A C4A C5A C10A . . . . 174.98(11) ?
C3A C4A C5A C6A . . . . -57.00(14) ?
C3A C4A C5A C10A . . . . 59.46(14) ?
C3A C8A C9A C10A . . . . 62.70(14) ?
C3A C8A C9A C11A . . . . 129.81(13) ?
C4A C3A C8A C7A . . . . 52.73(14) ?
C4A C3A C8A C9A . . . . -63.33(13) ?
C4A C5A C6A C7A . . . . 58.06(15) ?
C4A C5A C10A C9A . . . . -61.42(14) ?
C4A C5A C10A C11A . . . . -127.63(13) ?
C5A C6A C7A C8A . . . . 0.41(17) ?
C5A C10A C11A C9A . . . . 96.39(14) ?
C6A C5A C10A C9A . . . . 52.79(14) ?
C6A C5A C10A C11A . . . . -13.42(17) ?
C6A C7A C8A C3A . . . . -58.00(15) ?
C6A C7A C8A C9A . . . . 54.27(15) ?
C7A C8A C9A C10A . . . . -51.98(15) ?
C7A C8A C9A C11A . . . . 15.13(18) ?
C8A C3A C4A C2A . . . . -117.51(11) ?
C8A C3A C4A C5A . . . . 2.69(15) ?
C8A C9A C10A C5A . . . . -0.12(16) ?
C8A C9A C10A C11A . . . . 115.72(14) ?
C8A C9A C11A C10A . . . . -97.25(15) ?
C10A C5A C6A C7A . . . . -55.27(15) ?
C11A C9A C10A C5A . . . . -115.84(13) ?