#------------------------------------------------------------------------------
#$Date: 2025-05-10 02:50:16 +0100 (Sat, 10 May 2025) $
#$Revision: 299612 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023494.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_2023494
loop_
_publ_author_name
'N\"ather, Christian'
'Businski, Artjom'
'Herges, Rainer'
_publ_section_title
;
Reversible phase transition in
8,19-dimethyl-2,3,8,19-tetraazapentacyclo[13.7.0.04,12.06,10.017,21]docosa-1(15),2,4(12),5,10,16,21-heptaene-7,9,18,20-tetrone
;
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025003998
_journal_volume 81
_journal_year 2025
_chemical_formula_sum 'C20 H14 N4 O4'
_chemical_formula_weight 374.35
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 106.993(2)
_cell_angle_beta 90.914(3)
_cell_angle_gamma 90.1121(19)
_cell_formula_units_Z 4
_cell_length_a 7.9465(2)
_cell_length_b 13.7201(3)
_cell_length_c 16.2592(6)
_cell_measurement_reflns_used 13461
_cell_measurement_temperature 90(2)
_cell_measurement_theta_max 79.5650
_cell_measurement_theta_min 2.8330
_cell_volume 1695.04(9)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999) and XP in SHELXTL-PC (Sheldrick,
2008)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.945
_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_unetI/netI 0.0067
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 7780
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 81.037
_diffrn_reflns_theta_min 2.842
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.877
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.91445
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.467
_exptl_crystal_description block
_exptl_crystal_F_000 776
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.273
_refine_diff_density_min -0.199
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 514
_refine_ls_number_reflns 7780
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.071
_refine_ls_R_factor_all 0.0419
_refine_ls_R_factor_gt 0.0413
_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^)+(0.0640P)^2^+0.6702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1161
_refine_ls_wR_factor_ref 0.1167
_reflns_number_gt 7595
_reflns_number_total 7780
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8139.cif
_cod_data_source_block 90K
_cod_database_code 2023494
_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 -1 18290.7 65.8201 -2
0 0 1 18290.7 65.8201 1
0 0 -2 6158.39 54.2328 -2
0 0 2 6158.39 54.2328 1
0 0 -3 349513. 351.835 -2
0 0 3 349513. 351.835 1
0 0 -4 144750. 266.418 -2
0 0 4 144750. 266.418 1
0 0 -5 35.0609 11.7310 -2
0 0 5 35.0609 11.7310 1
0 0 -6 88614.1 264.794 -2
0 0 6 88614.1 264.794 1
0 0 -7 17984.5 131.842 -2
0 0 7 17984.5 131.842 1
0 0 -8 1963.67 50.1541 -2
0 0 8 1963.67 50.1541 1
0 0 -9 1340.90 27.3728 -2
0 0 9 1340.90 27.3728 1
0 0 -10 18690.8 94.3277 -2
0 0 10 18690.8 94.3277 1
0 0 -11 808.126 24.1193 -2
0 0 11 808.126 24.1193 1
0 0 -12 4210.69 51.9860 -2
0 0 12 4210.69 51.9860 1
0 0 13 1222.12 22.4687 -2
0 0 -13 1222.12 22.4687 1
0 0 14 12277.4 69.9617 -2
0 0 -14 12277.4 69.9617 1
0 0 -15 19679.3 150.047 -2
0 0 15 19679.3 150.047 1
0 0 -16 3901.79 47.7926 -2
0 0 16 3901.79 47.7926 1
0 0 -17 2112.38 33.0735 -2
0 0 17 2112.38 33.0735 1
0 0 -18 23.4296 9.98783 -2
0 0 18 23.4296 9.98783 1
0 0 -19 10.2238 7.05504 -2
0 0 19 10.2238 7.05504 1
0 1 -20 157.546 9.94568 -2
0 -1 20 157.546 9.94568 1
0 1 -19 60.2650 14.0019 -2
0 -1 19 60.2650 14.0019 1
0 1 -18 24.1934 10.5556 -2
0 -1 18 24.1934 10.5556 1
0 1 -17 4382.19 37.3900 -2
0 -1 17 4382.19 37.3900 1
0 1 -16 76.6019 14.7400 -2
0 -1 16 76.6019 14.7400 1
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0 -1 15 3009.06 44.3761 1
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0 -1 14 1019.85 21.2175 1
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0 -1 13 122.024 11.8506 1
0 1 -12 1016.44 30.0153 -2
0 -1 12 1016.44 30.0153 1
0 1 -11 1865.98 35.8350 -2
0 -1 11 1865.98 35.8350 1
0 1 -10 497.380 19.8755 -2
0 -1 10 497.380 19.8755 1
0 1 -9 2680.25 62.6148 -2
0 -1 9 2680.25 62.6148 1
0 1 -8 247.339 23.5111 -2
0 -1 8 247.339 23.5111 1
0 1 -7 762.038 30.5997 -2
0 -1 7 762.038 30.5997 1
0 1 -6 3351.24 53.3878 -2
0 -1 6 3351.24 53.3878 1
0 1 -5 822.339 25.3706 -2
0 -1 5 822.339 25.3706 1
0 1 -4 823.648 32.7837 -2
0 -1 4 823.648 32.7837 1
0 1 -3 1744.29 39.1516 -2
0 -1 3 1744.29 39.1516 1
0 1 -2 229.439 13.8741 -2
0 -1 2 229.439 13.8741 1
0 1 -1 232.567 6.90497 -2
0 -1 1 232.567 6.90497 1
0 1 1 833.934 13.5418 -2
0 -1 -1 833.934 13.5418 1
0 1 2 3293.36 23.8639 -2
0 -1 -2 3293.36 23.8639 1
0 -1 -3 47.5683 5.30785 -2
0 1 3 47.5683 5.30785 1
0 -1 -4 1667.17 11.5814 -2
0 1 4 1667.17 11.5814 1
0 -1 -5 405.900 19.5192 -2
0 1 5 405.900 19.5192 1
0 -1 -6 7339.34 76.7364 -2
0 1 6 7339.34 76.7364 1
0 -1 -7 7050.58 83.6189 -2
0 1 7 7050.58 83.6189 1
0 -1 -8 52.2247 17.1910 -2
0 1 8 52.2247 17.1910 1
0 -1 -9 136.473 20.9621 -2
0 1 9 136.473 20.9621 1
0 -1 -10 128.876 19.0382 -2
0 1 10 128.876 19.0382 1
0 -1 -11 645.494 33.7594 -2
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0 -1 -12 400.620 14.4256 -2
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0 -1 -13 99.3073 12.0899 -2
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0 -1 -14 427.133 17.7269 -2
0 1 14 427.133 17.7269 1
0 -1 -15 770.291 34.7330 -2
0 1 15 770.291 34.7330 1
0 -1 -16 1658.01 43.8152 -2
0 1 16 1658.01 43.8152 1
0 -1 -17 214.021 14.4648 -2
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0 -1 -18 19.6955 9.89241 -2
0 1 18 19.6955 9.89241 1
0 1 19 6.40775 7.23335 -2
0 -1 -19 6.40775 7.23335 1
0 2 -20 409.932 14.8587 -2
0 -2 20 409.932 14.8587 1
0 2 -19 376.526 20.0760 -2
0 -2 19 376.526 20.0760 1
0 2 -18 3.94407 14.0388 -2
0 -2 18 3.94407 14.0388 1
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0 -2 17 2755.76 38.3629 1
0 2 -16 1807.80 34.2540 -2
0 -2 16 1807.80 34.2540 1
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0 2 -15 12426.6 84.6073 1
0 -2 14 1994.44 42.6287 -2
0 2 -14 1994.44 42.6287 1
0 2 -13 7155.63 53.7768 -2
0 -2 13 7155.63 53.7768 1
0 2 -12 16919.9 98.3138 -2
0 -2 12 16919.9 98.3138 1
0 2 -11 7748.62 63.1543 -2
0 -2 11 7748.62 63.1543 1
0 2 -10 23298.7 100.783 -2
0 -2 10 23298.7 100.783 1
0 2 -9 41747.1 197.468 -2
0 -2 9 41747.1 197.468 1
0 2 -8 1467.26 36.2669 -2
0 -2 8 1467.26 36.2669 1
0 2 -7 88242.5 298.021 -2
0 -2 7 88242.5 298.021 1
0 2 -6 635.603 37.8862 -2
0 -2 6 635.603 37.8862 1
0 2 -5 39720.9 240.394 -2
0 -2 5 39720.9 240.394 1
0 2 -4 144.035 17.1578 -2
0 -2 4 144.035 17.1578 1
0 2 -3 4856.90 43.1030 -2
0 -2 3 4856.90 43.1030 1
0 2 -2 103610. 115.712 -2
0 -2 2 103610. 115.712 1
0 2 -1 62518.2 72.0758 -2
0 -2 1 62518.2 72.0758 1
0 2 0 54099.9 51.2828 -2
0 -2 0 54099.9 51.2828 1
0 2 1 329531. 400.142 -2
0 -2 -1 329531. 400.142 1
0 2 2 415779. 407.543 -2
0 -2 -2 415779. 407.543 1
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0 -2 -3 620031. 384.239 1
0 -2 -4 994376. 467.264 -2
0 2 4 994376. 467.264 1
0 -2 -5 2489.68 41.3437 -2
0 2 5 2489.68 41.3437 1
0 -2 -6 71227.3 236.255 -2
0 2 6 71227.3 236.255 1
0 -2 -7 63166.7 245.514 -2
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0 -2 -8 99.2275 11.9486 -2
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0 -2 -12 1441.55 27.1435 1
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0 -2 -13 1328.22 29.9717 1
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0 2 14 711.438 33.5157 1
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0 2 15 849.429 34.2544 1
0 -2 -16 304.794 23.0746 -2
0 2 16 304.794 23.0746 1
0 -2 -17 36.2354 9.13856 -2
0 2 17 36.2354 9.13856 1
0 2 18 875.126 17.5058 -2
0 -2 -18 875.126 17.5058 1
0 3 -20 585.917 16.1389 -2
0 -3 20 585.917 16.1389 1
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0 -3 18 885.997 22.0980 1
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0 -3 17 8.61375 14.5508 1
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0 -3 16 4153.35 66.5994 1
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0 3 -15 115.611 15.3085 1
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0 -3 13 2426.32 45.3608 1
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0 -3 10 68.8547 11.8395 1
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0 -3 7 2764.81 44.7050 1
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0 -3 4 597.195 14.3471 1
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0 -3 -1 382.087 15.3357 1
0 -3 -2 44.6984 7.53803 -2
0 3 2 44.6984 7.53803 1
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0 -3 -3 9222.47 55.7165 1
0 -3 -4 3486.75 59.6985 -2
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0 -3 -10 1008.07 27.0187 1
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0 -3 -11 40.2851 9.35441 1
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0 -3 -13 6.30426 10.1074 1
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0 -3 -17 88.5947 11.4911 1
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0 -4 20 66.7544 11.9368 1
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0 -4 19 602.179 24.5109 1
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0 -4 17 9190.33 56.7943 1
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0 -4 16 1223.25 27.8388 1
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0 -4 15 22319.2 88.0951 1
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0 -4 14 1011.55 19.4084 1
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0 -4 13 853.249 21.7269 1
0 4 -12 10207.5 57.7868 -2
0 -4 12 10207.5 57.7868 1
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0 -4 11 44059.7 144.472 1
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0 -4 10 7662.98 57.9467 1
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0 -4 9 8009.56 88.6354 1
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0 -4 8 61744.4 268.042 1
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0 -4 7 6835.19 82.7118 1
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0 -4 6 19591.2 92.5230 1
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0 -4 5 210164. 274.537 1
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0 -4 4 14886.0 66.2242 1
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0 -4 3 4214.98 42.8387 1
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0 -4 2 39912.4 123.863 1
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0 -4 1 46000.2 266.494 1
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0 -4 0 45936.9 93.1526 1
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0 -4 -1 56506.1 79.3353 1
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0 -5 4 9966.55 74.8565 1
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0 -5 -1 5384.79 45.8531 1
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0 -5 -3 941.741 50.1774 1
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0 -5 -4 2048.58 75.7189 1
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0 -5 -5 3009.34 98.2863 1
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0 -5 -6 680.466 56.7303 1
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9 3 -6 904.285 20.9541 1
9 -3 4 3639.60 38.1815 -2
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0 0 0 0.00000 0.00000 0
TITL Herges169a_90_d_twin1_hklf4 in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 7.946466 13.720092 16.259244 106.9927 90.9140 90.1121
ZERR 3.00 0.000223 0.000260 0.000590 0.0024 0.0026 0.0019
LATT 1
SFAC C H N O
UNIT 60.00 42.00 12.00 12.00
REM CrysAlisPro recorded range (K): Min=89.8; max=92.1; aver:91.0
TEMP -182
TREF
HKLF 5
BASF 0.40608
END
;
_shelx_hkl_checksum 14375
_shelx_res_file
;
TITL herges169a_auto_a.res in P-1
herges169a_90_d_tri_twin.res
created by SHELXL-2018/3 at 10:18:20 on 03-Apr-2025
REM Old TITL Herges169a_auto in P-1
REM SHELXT solution in P-1
REM R1 0.136, Rweak 0.008, Alpha 0.062, Orientation as input
REM Formula found by SHELXT: C42 N6 O8
CELL 1.54184 7.946466 13.720092 16.259244 106.9927 90.914 90.1121
ZERR 4 0.000223 0.00026 0.00059 0.0024 0.0026 0.0019
LATT 1
SFAC C H N O
UNIT 80 56 16 16
L.S. 10
PLAN 3
TEMP -183
CONF
MPLA C1 C2 C3 C4 N3 C5 C6 C7 C8 O1 O2
MPLA C11 C12 C13 C14 N4 C15 C16 C17 C18 O3 O4
MPLA C21 C22 C23 C24 N23 C25 C26 C27 C28 O21 O22
MPLA C31 C32 C33 C34 N24 C35 C36 C37 C38 O23 O24
BOND $H
HTAB
list 4
fmap 2 53
acta
OMIT 1 -1 -2
OMIT -4 -10 7
OMIT 8 -3 -2
OMIT 7 -6 2
OMIT 1 -1 -3
OMIT 8 3 2
OMIT -4 -10 6
OMIT -4 -10 5
REM
REM
REM
WGHT 0.064000 0.670200
BASF 0.40565
FVAR 4.79275 0.93079 0.84108 0.47772 0.83489
N1 3 0.903208 0.627426 0.840684 11.00000 0.02776 0.02714 =
0.03335 0.00631 -0.00070 -0.00185
N2 3 0.977174 0.617420 0.771741 11.00000 0.02539 0.03026 =
0.03603 0.00819 -0.00139 -0.00356
C1 1 0.897334 0.562234 0.690167 11.00000 0.02300 0.02648 =
0.03043 0.01081 0.00127 -0.00577
C2 1 0.959724 0.466669 0.646845 11.00000 0.02066 0.02836 =
0.03336 0.01520 -0.00040 -0.00184
AFIX 43
H2 2 1.039969 0.433158 0.672823 11.00000 -1.20000
AFIX 0
C3 1 0.898787 0.422820 0.563789 11.00000 0.01827 0.02456 =
0.03153 0.01338 0.00309 -0.00075
C4 1 0.939625 0.324096 0.499711 11.00000 0.01978 0.02357 =
0.03465 0.01351 0.00148 -0.00297
O1 4 1.028624 0.255963 0.508344 11.00000 0.02828 0.02598 =
0.04357 0.01459 0.00072 0.00485
N3 3 0.853016 0.323837 0.424577 11.00000 0.02274 0.02563 =
0.03075 0.01009 0.00157 -0.00180
C5 1 0.753293 0.409661 0.435555 11.00000 0.01806 0.02737 =
0.03195 0.01424 0.00344 -0.00059
O2 4 0.662874 0.426327 0.380134 11.00000 0.02533 0.03888 =
0.03181 0.01590 -0.00043 0.00085
C6 1 0.784433 0.473563 0.525796 11.00000 0.01654 0.02741 =
0.03116 0.01508 0.00232 -0.00244
C7 1 0.721593 0.567909 0.569093 11.00000 0.01952 0.02618 =
0.03438 0.01630 0.00408 0.00090
AFIX 43
H7 2 0.642211 0.601045 0.542300 11.00000 -1.20000
AFIX 0
C8 1 0.778107 0.613454 0.653638 11.00000 0.02288 0.02376 =
0.03521 0.01284 0.00486 -0.00189
C9 1 0.714127 0.714978 0.707472 11.00000 0.03048 0.02465 =
0.03944 0.01063 0.00470 0.00042
AFIX 23
H9A 2 0.660111 0.750500 0.669137 11.00000 -1.20000
H9B 2 0.810885 0.757169 0.736927 11.00000 -1.20000
AFIX 0
C10 1 0.586507 0.706109 0.775515 11.00000 0.02795 0.02858 =
0.03439 0.00842 0.00088 -0.00012
AFIX 23
H10A 2 0.601282 0.766655 0.826239 11.00000 -1.20000
H10B 2 0.472099 0.709803 0.751648 11.00000 -1.20000
AFIX 0
C11 1 0.593027 0.612455 0.806770 11.00000 0.02678 0.02557 =
0.02546 0.00374 0.00204 -0.00073
C12 1 0.441322 0.561233 0.810236 11.00000 0.02391 0.02934 =
0.02539 0.00494 0.00091 -0.00014
AFIX 43
H12 2 0.340053 0.579717 0.786947 11.00000 -1.20000
AFIX 0
C13 1 0.442550 0.483387 0.848245 11.00000 0.02884 0.02747 =
0.02354 0.00352 0.00163 -0.00304
C14 1 0.301763 0.419835 0.864439 11.00000 0.03411 0.02958 =
0.02434 0.00264 0.00414 -0.00565
O3 4 0.154793 0.418872 0.842105 11.00000 0.03050 0.04004 =
0.03906 0.00844 0.00402 -0.00766
N4 3 0.372822 0.359017 0.910859 11.00000 0.03712 0.03266 =
0.02710 0.00672 0.00405 -0.00757
C15 1 0.545074 0.377028 0.926707 11.00000 0.03947 0.02796 =
0.02274 0.00462 0.00085 -0.00164
O4 4 0.635118 0.339153 0.969056 11.00000 0.04666 0.03412 =
0.03497 0.01344 -0.00302 -0.00186
C16 1 0.588088 0.455705 0.883821 11.00000 0.03474 0.02524 =
0.02256 0.00340 0.00119 -0.00004
C17 1 0.740868 0.502020 0.879610 11.00000 0.02969 0.02731 =
0.02711 0.00416 -0.00168 0.00036
AFIX 43
H17 2 0.841233 0.482642 0.903060 11.00000 -1.20000
AFIX 0
C18 1 0.740122 0.578934 0.839025 11.00000 0.02792 0.02539 =
0.02646 0.00289 0.00076 -0.00285
C19 1 0.845132 0.236839 0.347717 11.00000 0.03097 0.03196 =
0.03441 0.00629 0.00335 -0.00254
AFIX 127
H19A 2 0.928068 0.186076 0.352851 21.00000 -1.50000
H19B 2 0.869872 0.259322 0.297236 21.00000 -1.50000
H19C 2 0.732144 0.206504 0.341281 21.00000 -1.50000
H19D 2 0.758655 0.248525 0.308061 -21.00000 -1.50000
H19E 2 0.816850 0.175279 0.363676 -21.00000 -1.50000
H19F 2 0.954579 0.228098 0.319631 -21.00000 -1.50000
AFIX 0
C20 1 0.278809 0.285206 0.940907 11.00000 0.04785 0.03449 =
0.03217 0.00880 0.00781 -0.01017
AFIX 127
H20A 2 0.163081 0.308920 0.953165 31.00000 -1.50000
H20B 2 0.332539 0.277794 0.993401 31.00000 -1.50000
H20C 2 0.277532 0.219228 0.896377 31.00000 -1.50000
H20D 2 0.352353 0.228375 0.942130 -31.00000 -1.50000
H20E 2 0.182896 0.259500 0.901894 -31.00000 -1.50000
H20F 2 0.237903 0.318067 0.998918 -31.00000 -1.50000
AFIX 0
N21 3 0.587225 1.138330 0.822536 11.00000 0.02772 0.02589 =
0.04178 0.00479 0.00329 -0.00026
N22 3 0.515081 1.125740 0.750957 11.00000 0.02916 0.02689 =
0.04400 0.00587 0.00128 0.00191
C21 1 0.592553 1.062456 0.673407 11.00000 0.02218 0.02514 =
0.03764 0.01172 -0.00116 0.00325
C22 1 0.525901 0.965362 0.635971 11.00000 0.01971 0.02658 =
0.03673 0.01437 0.00116 0.00012
AFIX 43
H22 2 0.440615 0.937784 0.663066 11.00000 -1.20000
AFIX 0
C23 1 0.589718 0.911281 0.557727 11.00000 0.02008 0.02378 =
0.03540 0.01526 -0.00187 0.00089
C24 1 0.547779 0.807089 0.500872 11.00000 0.02122 0.02505 =
0.03708 0.01336 -0.00102 0.00221
O21 4 0.453386 0.743946 0.514388 11.00000 0.02935 0.02553 =
0.04668 0.01270 0.00264 -0.00366
N23 3 0.640897 0.793798 0.427347 11.00000 0.02112 0.03132 =
0.03455 0.01016 -0.00043 0.00336
C25 1 0.744721 0.877903 0.432499 11.00000 0.02163 0.03643 =
0.03340 0.01730 -0.00246 0.00236
O22 4 0.838975 0.885259 0.377097 11.00000 0.02478 0.05537 =
0.03542 0.02240 0.00261 0.00099
C26 1 0.710626 0.953012 0.517096 11.00000 0.01885 0.03073 =
0.03291 0.01751 -0.00202 0.00035
C27 1 0.777349 1.049190 0.554695 11.00000 0.02134 0.03240 =
0.03951 0.02227 -0.00338 -0.00285
AFIX 43
H27 2 0.861235 1.076412 0.526518 11.00000 -1.20000
AFIX 0
C28 1 0.718862 1.105247 0.634762 11.00000 0.02562 0.02503 =
0.04178 0.01662 -0.00684 -0.00194
C29 1 0.788783 1.209235 0.680717 11.00000 0.03210 0.02541 =
0.05728 0.01751 -0.00807 -0.00464
AFIX 23
H29A 2 0.694153 1.257677 0.695896 11.00000 -1.20000
H29B 2 0.861377 1.231700 0.640681 11.00000 -1.20000
AFIX 0
C30 1 0.891916 1.214948 0.763280 11.00000 0.03300 0.02419 =
0.04167 0.00965 0.00219 -0.00464
AFIX 23
H30A 2 1.009959 1.231213 0.753442 11.00000 -1.20000
H30B 2 0.849053 1.272850 0.809963 11.00000 -1.20000
AFIX 0
C31 1 0.892880 1.122170 0.795001 11.00000 0.02997 0.02316 =
0.02817 0.00401 -0.00065 -0.00338
C32 1 1.044414 1.071312 0.800006 11.00000 0.02596 0.02818 =
0.02757 0.00596 -0.00049 -0.00392
AFIX 43
H32 2 1.144643 1.089582 0.776876 11.00000 -1.20000
AFIX 0
C33 1 1.045428 0.994574 0.838951 11.00000 0.02863 0.02526 =
0.02423 0.00252 -0.00117 -0.00310
C34 1 1.185519 0.931779 0.857130 11.00000 0.03149 0.02853 =
0.02572 0.00369 -0.00259 -0.00261
O23 4 1.331793 0.929947 0.835751 11.00000 0.02759 0.04014 =
0.04116 0.01338 -0.00070 0.00027
N24 3 1.116720 0.871850 0.904184 11.00000 0.03345 0.02931 =
0.02854 0.00722 -0.00182 0.00029
C35 1 0.945055 0.890208 0.917881 11.00000 0.03596 0.02594 =
0.02595 0.00370 0.00062 -0.00351
O24 4 0.856365 0.851877 0.959719 11.00000 0.04475 0.03598 =
0.03897 0.01580 0.00802 -0.00318
C36 1 0.899573 0.967445 0.873491 11.00000 0.03223 0.02431 =
0.02385 0.00306 0.00111 -0.00469
C37 1 0.747653 1.012410 0.867080 11.00000 0.02799 0.02729 =
0.02880 0.00317 0.00442 -0.00405
AFIX 43
H37 2 0.647957 0.992735 0.889717 11.00000 -1.20000
AFIX 0
C38 1 0.746616 1.088322 0.825771 11.00000 0.02704 0.02402 =
0.02866 0.00074 0.00140 -0.00167
C39 1 0.645765 0.699112 0.357964 11.00000 0.03205 0.04120 =
0.04078 0.00274 -0.00326 0.00718
AFIX 127
H39A 2 0.561599 0.651555 0.367721 41.00000 -1.50000
H39B 2 0.757924 0.669068 0.356180 41.00000 -1.50000
H39C 2 0.621057 0.712784 0.303147 41.00000 -1.50000
H39D 2 0.732122 0.704049 0.316978 -41.00000 -1.50000
H39E 2 0.535796 0.686536 0.328519 -41.00000 -1.50000
H39F 2 0.672663 0.642820 0.381551 -41.00000 -1.50000
AFIX 0
C40 1 1.211889 0.799270 0.936291 11.00000 0.04064 0.03086 =
0.03372 0.01111 -0.00518 0.00245
AFIX 127
H40A 2 1.324331 0.827142 0.955215 51.00000 -1.50000
H40B 2 1.222115 0.734965 0.890324 51.00000 -1.50000
H40C 2 1.153120 0.786971 0.984891 51.00000 -1.50000
H40D 2 1.142047 0.738910 0.931739 -51.00000 -1.50000
H40E 2 1.244262 0.831087 0.996629 -51.00000 -1.50000
H40F 2 1.313258 0.779081 0.902062 -51.00000 -1.50000
AFIX 0
HKLF 5
REM herges169a_auto_a.res in P-1
REM wR2 = 0.1167, GooF = S = 1.071, Restrained GooF = 1.071 for all data
REM R1 = 0.0413 for 7595 Fo > 4sig(Fo) and 0.0419 for all 7780 data
REM 514 parameters refined using 0 restraints
END
WGHT 0.0641 0.6684
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, -y+1, -z+1
HTAB C19 N2_$1
HTAB C40 N1
REM Highest difference peak 0.273, deepest hole -0.199, 1-sigma level 0.049
Q1 1 0.1938 0.4587 0.9542 11.00000 0.05 0.27
Q2 1 0.7364 0.6608 0.6824 11.00000 0.05 0.25
Q3 1 0.8610 0.5924 0.6640 11.00000 0.05 0.24
;
_shelx_res_checksum 76515
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.90321(19) 0.62743(12) 0.84068(10) 0.0300(3) Uani d 1 . .
N N2 0.97717(19) 0.61742(13) 0.77174(11) 0.0309(3) Uani d 1 . .
C C1 0.8973(2) 0.56223(14) 0.69017(11) 0.0261(3) Uani d 1 . .
C C2 0.9597(2) 0.46667(14) 0.64684(11) 0.0262(3) Uani d 1 . .
H H2 1.039969 0.433158 0.672823 0.031 Uiso calc 1 . .
C C3 0.89879(19) 0.42282(13) 0.56379(11) 0.0237(3) Uani d 1 . .
C C4 0.9396(2) 0.32410(13) 0.49971(11) 0.0249(3) Uani d 1 . .
O O1 1.02862(16) 0.25596(10) 0.50834(9) 0.0317(3) Uani d 1 . .
N N3 0.85302(18) 0.32384(12) 0.42458(10) 0.0260(3) Uani d 1 . .
C C5 0.75329(19) 0.40966(13) 0.43556(11) 0.0246(3) Uani d 1 . .
O O2 0.66287(16) 0.42633(11) 0.38013(8) 0.0308(3) Uani d 1 . .
C C6 0.78443(19) 0.47356(13) 0.52580(11) 0.0236(3) Uani d 1 . .
C C7 0.7216(2) 0.56791(14) 0.56909(11) 0.0251(3) Uani d 1 . .
H H7 0.642211 0.601045 0.542300 0.030 Uiso calc 1 . .
C C8 0.7781(2) 0.61345(13) 0.65364(12) 0.0263(3) Uani d 1 . .
C C9 0.7141(2) 0.71498(14) 0.70747(13) 0.0312(4) Uani d 1 . .
H H9A 0.660111 0.750500 0.669137 0.037 Uiso calc 1 . .
H H9B 0.810885 0.757169 0.736927 0.037 Uiso calc 1 . .
C C10 0.5865(2) 0.70611(15) 0.77551(12) 0.0305(4) Uani d 1 . .
H H10A 0.601282 0.766655 0.826239 0.037 Uiso calc 1 . .
H H10B 0.472099 0.709803 0.751648 0.037 Uiso calc 1 . .
C C11 0.5930(2) 0.61246(14) 0.80677(11) 0.0267(4) Uani d 1 . .
C C12 0.4413(2) 0.56123(14) 0.81024(11) 0.0269(3) Uani d 1 . .
H H12 0.340053 0.579717 0.786947 0.032 Uiso calc 1 . .
C C13 0.4425(2) 0.48339(14) 0.84824(11) 0.0274(4) Uani d 1 . .
C C14 0.3018(2) 0.41984(15) 0.86444(11) 0.0304(4) Uani d 1 . .
O O3 0.15479(17) 0.41887(12) 0.84211(9) 0.0372(3) Uani d 1 . .
N N4 0.3728(2) 0.35902(13) 0.91086(10) 0.0327(3) Uani d 1 . .
C C15 0.5451(3) 0.37703(15) 0.92671(11) 0.0307(4) Uani d 1 . .
O O4 0.63512(19) 0.33915(11) 0.96906(9) 0.0379(3) Uani d 1 . .
C C16 0.5881(2) 0.45571(14) 0.88382(11) 0.0283(4) Uani d 1 . .
C C17 0.7409(2) 0.50202(14) 0.87961(11) 0.0289(4) Uani d 1 . .
H H17 0.841233 0.482642 0.903060 0.035 Uiso calc 1 . .
C C18 0.7401(2) 0.57893(14) 0.83902(11) 0.0276(4) Uani d 1 . .
C C19 0.8451(2) 0.23684(15) 0.34772(12) 0.0331(4) Uani d 1 . .
H H19A 0.928068 0.186076 0.352851 0.050 Uiso calc 0.93(3) . .
H H19B 0.869872 0.259322 0.297236 0.050 Uiso calc 0.93(3) . .
H H19C 0.732144 0.206504 0.341281 0.050 Uiso calc 0.93(3) . .
H H19D 0.758655 0.248525 0.308061 0.050 Uiso calc 0.07(3) . .
H H19E 0.816850 0.175279 0.363676 0.050 Uiso calc 0.07(3) . .
H H19F 0.954579 0.228098 0.319631 0.050 Uiso calc 0.07(3) . .
C C20 0.2788(3) 0.28521(16) 0.94091(13) 0.0383(5) Uani d 1 . .
H H20A 0.163081 0.308920 0.953165 0.057 Uiso calc 0.84(3) . .
H H20B 0.332539 0.277794 0.993401 0.057 Uiso calc 0.84(3) . .
H H20C 0.277532 0.219228 0.896377 0.057 Uiso calc 0.84(3) . .
H H20D 0.352353 0.228375 0.942130 0.057 Uiso calc 0.16(3) . .
H H20E 0.182896 0.259500 0.901894 0.057 Uiso calc 0.16(3) . .
H H20F 0.237903 0.318067 0.998918 0.057 Uiso calc 0.16(3) . .
N N21 0.5872(2) 1.13833(13) 0.82254(11) 0.0329(3) Uani d 1 . .
N N22 0.5151(2) 1.12574(13) 0.75096(11) 0.0343(4) Uani d 1 . .
C C21 0.5926(2) 1.06246(14) 0.67341(12) 0.0278(4) Uani d 1 . .
C C22 0.5259(2) 0.96536(14) 0.63597(12) 0.0266(3) Uani d 1 . .
H H22 0.440615 0.937784 0.663066 0.032 Uiso calc 1 . .
C C23 0.5897(2) 0.91128(13) 0.55773(12) 0.0250(3) Uani d 1 . .
C C24 0.5478(2) 0.80709(14) 0.50087(12) 0.0269(4) Uani d 1 . .
O O21 0.45339(16) 0.74395(10) 0.51439(9) 0.0334(3) Uani d 1 . .
N N23 0.64090(18) 0.79380(12) 0.42735(10) 0.0289(3) Uani d 1 . .
C C25 0.7447(2) 0.87790(15) 0.43250(12) 0.0290(4) Uani d 1 . .
O O22 0.83897(16) 0.88526(12) 0.37710(9) 0.0366(3) Uani d 1 . .
C C26 0.7106(2) 0.95301(14) 0.51710(12) 0.0258(3) Uani d 1 . .
C C27 0.7773(2) 1.04919(15) 0.55469(12) 0.0286(4) Uani d 1 . .
H H27 0.861235 1.076412 0.526518 0.034 Uiso calc 1 . .
C C28 0.7189(2) 1.10525(14) 0.63476(13) 0.0294(4) Uani d 1 . .
C C29 0.7888(3) 1.20923(15) 0.68072(15) 0.0372(4) Uani d 1 . .
H H29A 0.694153 1.257677 0.695896 0.045 Uiso calc 1 . .
H H29B 0.861377 1.231700 0.640681 0.045 Uiso calc 1 . .
C C30 0.8919(2) 1.21495(14) 0.76328(13) 0.0329(4) Uani d 1 . .
H H30A 1.009959 1.231213 0.753442 0.040 Uiso calc 1 . .
H H30B 0.849053 1.272850 0.809963 0.040 Uiso calc 1 . .
C C31 0.8929(2) 1.12217(14) 0.79500(11) 0.0279(4) Uani d 1 . .
C C32 1.0444(2) 1.07131(14) 0.80001(11) 0.0277(4) Uani d 1 . .
H H32 1.144643 1.089582 0.776876 0.033 Uiso calc 1 . .
C C33 1.0454(2) 0.99457(14) 0.83895(11) 0.0271(4) Uani d 1 . .
C C34 1.1855(2) 0.93178(15) 0.85713(11) 0.0295(4) Uani d 1 . .
O O23 1.33179(16) 0.92995(12) 0.83575(9) 0.0360(3) Uani d 1 . .
N N24 1.1167(2) 0.87185(13) 0.90418(10) 0.0307(3) Uani d 1 . .
C C35 0.9451(2) 0.89021(14) 0.91788(11) 0.0301(4) Uani d 1 . .
O O24 0.85636(19) 0.85188(12) 0.95972(9) 0.0388(3) Uani d 1 . .
C C36 0.8996(2) 0.96745(14) 0.87349(11) 0.0276(4) Uani d 1 . .
C C37 0.7477(2) 1.01241(14) 0.86708(12) 0.0291(4) Uani d 1 . .
H H37 0.647957 0.992735 0.889717 0.035 Uiso calc 1 . .
C C38 0.7466(2) 1.08832(14) 0.82577(12) 0.0280(4) Uani d 1 . .
C C39 0.6458(3) 0.69911(17) 0.35796(14) 0.0400(5) Uani d 1 . .
H H39A 0.561599 0.651555 0.367721 0.060 Uiso calc 0.48(3) . .
H H39B 0.757924 0.669068 0.356180 0.060 Uiso calc 0.48(3) . .
H H39C 0.621057 0.712784 0.303147 0.060 Uiso calc 0.48(3) . .
H H39D 0.732122 0.704049 0.316978 0.060 Uiso calc 0.52(3) . .
H H39E 0.535796 0.686536 0.328519 0.060 Uiso calc 0.52(3) . .
H H39F 0.672663 0.642820 0.381551 0.060 Uiso calc 0.52(3) . .
C C40 1.2119(3) 0.79927(16) 0.93629(13) 0.0348(4) Uani d 1 . .
H H40A 1.324331 0.827142 0.955215 0.052 Uiso calc 0.83(3) . .
H H40B 1.222115 0.734965 0.890324 0.052 Uiso calc 0.83(3) . .
H H40C 1.153120 0.786971 0.984891 0.052 Uiso calc 0.83(3) . .
H H40D 1.142047 0.738910 0.931739 0.052 Uiso calc 0.17(3) . .
H H40E 1.244262 0.831087 0.996629 0.052 Uiso calc 0.17(3) . .
H H40F 1.313258 0.779081 0.902062 0.052 Uiso calc 0.17(3) . .
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 0.0278(7) 0.0271(8) 0.0333(8) -0.0018(6) -0.0007(6) 0.0063(6)
N2 0.0254(7) 0.0303(8) 0.0360(8) -0.0036(6) -0.0014(6) 0.0082(6)
C1 0.0230(8) 0.0265(9) 0.0304(9) -0.0058(6) 0.0013(6) 0.0108(7)
C2 0.0207(7) 0.0284(9) 0.0334(9) -0.0018(6) -0.0004(6) 0.0152(7)
C3 0.0183(7) 0.0246(8) 0.0315(8) -0.0008(6) 0.0031(6) 0.0134(7)
C4 0.0198(7) 0.0236(8) 0.0346(9) -0.0030(6) 0.0015(6) 0.0135(7)
O1 0.0283(6) 0.0260(7) 0.0436(7) 0.0049(5) 0.0007(5) 0.0146(6)
N3 0.0227(7) 0.0256(7) 0.0308(7) -0.0018(5) 0.0016(5) 0.0101(6)
C5 0.0181(7) 0.0274(9) 0.0320(9) -0.0006(6) 0.0034(6) 0.0142(7)
O2 0.0253(6) 0.0389(7) 0.0318(7) 0.0008(5) -0.0004(5) 0.0159(5)
C6 0.0165(7) 0.0274(9) 0.0312(8) -0.0024(6) 0.0023(6) 0.0151(7)
C7 0.0195(7) 0.0262(8) 0.0344(9) 0.0009(6) 0.0041(6) 0.0163(7)
C8 0.0229(8) 0.0238(8) 0.0352(9) -0.0019(6) 0.0049(6) 0.0128(7)
C9 0.0305(9) 0.0247(9) 0.0394(10) 0.0004(7) 0.0047(7) 0.0106(7)
C10 0.0279(8) 0.0286(9) 0.0344(9) -0.0001(7) 0.0009(7) 0.0084(7)
C11 0.0268(8) 0.0256(9) 0.0255(8) -0.0007(6) 0.0020(6) 0.0037(6)
C12 0.0239(8) 0.0293(9) 0.0254(8) -0.0001(6) 0.0009(6) 0.0049(7)
C13 0.0288(8) 0.0275(9) 0.0235(8) -0.0030(7) 0.0016(6) 0.0035(6)
C14 0.0341(9) 0.0296(9) 0.0243(8) -0.0056(7) 0.0041(7) 0.0026(7)
O3 0.0305(7) 0.0400(8) 0.0391(7) -0.0077(6) 0.0040(6) 0.0084(6)
N4 0.0371(8) 0.0327(9) 0.0271(7) -0.0076(7) 0.0040(6) 0.0067(6)
C15 0.0395(10) 0.0280(9) 0.0227(8) -0.0016(7) 0.0009(7) 0.0046(7)
O4 0.0467(8) 0.0341(8) 0.0350(7) -0.0019(6) -0.0030(6) 0.0134(6)
C16 0.0347(9) 0.0252(9) 0.0226(8) 0.0000(7) 0.0012(7) 0.0034(6)
C17 0.0297(9) 0.0273(9) 0.0271(8) 0.0004(7) -0.0017(7) 0.0042(7)
C18 0.0279(8) 0.0254(8) 0.0265(8) -0.0029(7) 0.0008(6) 0.0029(7)
C19 0.0310(9) 0.0320(10) 0.0344(9) -0.0025(7) 0.0034(7) 0.0063(8)
C20 0.0478(11) 0.0345(10) 0.0322(9) -0.0102(9) 0.0078(8) 0.0088(8)
N21 0.0277(7) 0.0259(8) 0.0418(9) -0.0003(6) 0.0033(6) 0.0048(7)
N22 0.0292(8) 0.0269(8) 0.0440(9) 0.0019(6) 0.0013(7) 0.0059(7)
C21 0.0222(8) 0.0251(9) 0.0376(9) 0.0032(6) -0.0012(7) 0.0117(7)
C22 0.0197(7) 0.0266(9) 0.0367(9) 0.0001(6) 0.0012(6) 0.0144(7)
C23 0.0201(7) 0.0238(8) 0.0354(9) 0.0009(6) -0.0019(6) 0.0153(7)
C24 0.0212(8) 0.0250(9) 0.0371(9) 0.0022(6) -0.0010(6) 0.0134(7)
O21 0.0293(6) 0.0255(7) 0.0467(8) -0.0037(5) 0.0026(5) 0.0127(6)
N23 0.0211(7) 0.0313(8) 0.0345(8) 0.0034(6) -0.0004(6) 0.0102(6)
C25 0.0216(8) 0.0364(10) 0.0334(9) 0.0024(7) -0.0025(7) 0.0173(8)
O22 0.0248(6) 0.0554(9) 0.0354(7) 0.0010(6) 0.0026(5) 0.0224(6)
C26 0.0189(7) 0.0307(9) 0.0329(9) 0.0004(6) -0.0020(6) 0.0175(7)
C27 0.0213(8) 0.0324(9) 0.0395(10) -0.0029(7) -0.0034(7) 0.0223(8)
C28 0.0256(8) 0.0250(9) 0.0418(10) -0.0019(7) -0.0068(7) 0.0166(8)
C29 0.0321(9) 0.0254(10) 0.0573(12) -0.0046(7) -0.0081(8) 0.0175(9)
C30 0.0330(9) 0.0242(9) 0.0417(10) -0.0046(7) 0.0022(8) 0.0097(8)
C31 0.0300(9) 0.0232(9) 0.0282(8) -0.0034(7) -0.0006(7) 0.0040(7)
C32 0.0260(8) 0.0282(9) 0.0276(8) -0.0039(7) -0.0005(6) 0.0060(7)
C33 0.0286(8) 0.0253(9) 0.0242(8) -0.0031(7) -0.0012(6) 0.0025(6)
C34 0.0315(9) 0.0285(9) 0.0257(8) -0.0026(7) -0.0026(7) 0.0037(7)
O23 0.0276(7) 0.0401(8) 0.0412(7) 0.0003(5) -0.0007(5) 0.0134(6)
N24 0.0334(8) 0.0293(8) 0.0285(7) 0.0003(6) -0.0018(6) 0.0072(6)
C35 0.0360(9) 0.0259(9) 0.0259(8) -0.0035(7) 0.0006(7) 0.0037(7)
O24 0.0448(8) 0.0360(8) 0.0390(7) -0.0032(6) 0.0080(6) 0.0158(6)
C36 0.0322(9) 0.0243(9) 0.0238(8) -0.0047(7) 0.0011(6) 0.0031(6)
C37 0.0280(8) 0.0273(9) 0.0288(8) -0.0041(7) 0.0044(7) 0.0032(7)
C38 0.0270(8) 0.0240(9) 0.0287(8) -0.0017(7) 0.0014(6) 0.0007(7)
C39 0.0320(10) 0.0412(12) 0.0408(11) 0.0072(8) -0.0033(8) 0.0027(9)
C40 0.0406(10) 0.0309(10) 0.0337(9) 0.0025(8) -0.0052(8) 0.0111(8)
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_
_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
N2 N1 C18 . . 119.17(15) ?
N1 N2 C1 . . 120.42(14) ?
C2 C1 C8 . . 123.02(16) ?
C2 C1 N2 . . 118.01(16) ?
C8 C1 N2 . . 118.36(16) ?
C3 C2 C1 . . 116.58(16) ?
C3 C2 H2 . . 121.7 ?
C1 C2 H2 . . 121.7 ?
C2 C3 C6 . . 121.18(17) ?
C2 C3 C4 . . 130.69(16) ?
C6 C3 C4 . . 108.10(15) ?
O1 C4 N3 . . 125.28(17) ?
O1 C4 C3 . . 128.95(17) ?
N3 C4 C3 . . 105.77(14) ?
C5 N3 C4 . . 112.23(15) ?
C5 N3 C19 . . 123.10(16) ?
C4 N3 C19 . . 123.93(16) ?
O2 C5 N3 . . 124.94(17) ?
O2 C5 C6 . . 129.18(17) ?
N3 C5 C6 . . 105.87(14) ?
C7 C6 C3 . . 122.15(16) ?
C7 C6 C5 . . 129.92(16) ?
C3 C6 C5 . . 107.92(15) ?
C6 C7 C8 . . 118.10(16) ?
C6 C7 H7 . . 120.9 ?
C8 C7 H7 . . 120.9 ?
C7 C8 C1 . . 118.93(17) ?
C7 C8 C9 . . 122.41(17) ?
C1 C8 C9 . . 118.65(17) ?
C8 C9 C10 . . 113.34(15) ?
C8 C9 H9A . . 108.9 ?
C10 C9 H9A . . 108.9 ?
C8 C9 H9B . . 108.9 ?
C10 C9 H9B . . 108.9 ?
H9A C9 H9B . . 107.7 ?
C11 C10 C9 . . 118.20(16) ?
C11 C10 H10A . . 107.8 ?
C9 C10 H10A . . 107.8 ?
C11 C10 H10B . . 107.8 ?
C9 C10 H10B . . 107.8 ?
H10A C10 H10B . . 107.1 ?
C12 C11 C18 . . 118.15(16) ?
C12 C11 C10 . . 118.09(16) ?
C18 C11 C10 . . 123.54(15) ?
C13 C12 C11 . . 118.56(17) ?
C13 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
C12 C13 C16 . . 121.96(16) ?
C12 C13 C14 . . 130.29(17) ?
C16 C13 C14 . . 107.66(16) ?
O3 C14 N4 . . 125.86(18) ?
O3 C14 C13 . . 128.46(19) ?
N4 C14 C13 . . 105.69(16) ?
C14 N4 C15 . . 112.75(16) ?
C14 N4 C20 . . 124.15(17) ?
C15 N4 C20 . . 123.09(18) ?
O4 C15 N4 . . 126.50(18) ?
O4 C15 C16 . . 128.53(18) ?
N4 C15 C16 . . 104.91(17) ?
C17 C16 C13 . . 121.37(17) ?
C17 C16 C15 . . 129.62(18) ?
C13 C16 C15 . . 108.95(16) ?
C16 C17 C18 . . 116.52(17) ?
C16 C17 H17 . . 121.7 ?
C18 C17 H17 . . 121.7 ?
C17 C18 C11 . . 123.28(16) ?
C17 C18 N1 . . 113.43(16) ?
C11 C18 N1 . . 123.04(16) ?
N3 C19 H19A . . 109.5 ?
N3 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
N3 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
N3 C19 H19D . . 109.5 ?
H19A C19 H19D . . 141.1 ?
H19B C19 H19D . . 56.3 ?
H19C C19 H19D . . 56.3 ?
N3 C19 H19E . . 109.5 ?
H19A C19 H19E . . 56.3 ?
H19B C19 H19E . . 141.1 ?
H19C C19 H19E . . 56.3 ?
H19D C19 H19E . . 109.5 ?
N3 C19 H19F . . 109.5 ?
H19A C19 H19F . . 56.3 ?
H19B C19 H19F . . 56.3 ?
H19C C19 H19F . . 141.1 ?
H19D C19 H19F . . 109.5 ?
H19E C19 H19F . . 109.5 ?
N4 C20 H20A . . 109.5 ?
N4 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
N4 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
N4 C20 H20D . . 109.5 ?
H20A C20 H20D . . 141.1 ?
H20B C20 H20D . . 56.3 ?
H20C C20 H20D . . 56.3 ?
N4 C20 H20E . . 109.5 ?
H20A C20 H20E . . 56.3 ?
H20B C20 H20E . . 141.1 ?
H20C C20 H20E . . 56.3 ?
H20D C20 H20E . . 109.5 ?
N4 C20 H20F . . 109.5 ?
H20A C20 H20F . . 56.3 ?
H20B C20 H20F . . 56.3 ?
H20C C20 H20F . . 141.1 ?
H20D C20 H20F . . 109.5 ?
H20E C20 H20F . . 109.5 ?
N22 N21 C38 . . 118.80(16) ?
N21 N22 C21 . . 119.77(16) ?
C22 C21 C28 . . 122.88(17) ?
C22 C21 N22 . . 117.98(16) ?
C28 C21 N22 . . 118.80(17) ?
C23 C22 C21 . . 116.70(16) ?
C23 C22 H22 . . 121.6 ?
C21 C22 H22 . . 121.6 ?
C22 C23 C26 . . 121.48(17) ?
C22 C23 C24 . . 130.62(15) ?
C26 C23 C24 . . 107.88(16) ?
O21 C24 N23 . . 125.14(17) ?
O21 C24 C23 . . 128.60(17) ?
N23 C24 C23 . . 106.25(14) ?
C24 N23 C25 . . 111.89(15) ?
C24 N23 C39 . . 123.79(16) ?
C25 N23 C39 . . 123.91(16) ?
O22 C25 N23 . . 125.03(19) ?
O22 C25 C26 . . 128.97(18) ?
N23 C25 C26 . . 105.99(15) ?
C27 C26 C23 . . 121.64(17) ?
C27 C26 C25 . . 130.42(16) ?
C23 C26 C25 . . 107.94(16) ?
C26 C27 C28 . . 118.51(16) ?
C26 C27 H27 . . 120.7 ?
C28 C27 H27 . . 120.7 ?
C27 C28 C21 . . 118.73(17) ?
C27 C28 C29 . . 121.54(17) ?
C21 C28 C29 . . 119.73(18) ?
C28 C29 C30 . . 114.67(16) ?
C28 C29 H29A . . 108.6 ?
C30 C29 H29A . . 108.6 ?
C28 C29 H29B . . 108.6 ?
C30 C29 H29B . . 108.6 ?
H29A C29 H29B . . 107.6 ?
C31 C30 C29 . . 117.71(15) ?
C31 C30 H30A . . 107.9 ?
C29 C30 H30A . . 107.9 ?
C31 C30 H30B . . 107.9 ?
C29 C30 H30B . . 107.9 ?
H30A C30 H30B . . 107.2 ?
C38 C31 C32 . . 118.13(17) ?
C38 C31 C30 . . 121.45(17) ?
C32 C31 C30 . . 120.27(16) ?
C33 C32 C31 . . 119.03(16) ?
C33 C32 H32 . . 120.5 ?
C31 C32 H32 . . 120.5 ?
C32 C33 C36 . . 121.03(18) ?
C32 C33 C34 . . 131.01(16) ?
C36 C33 C34 . . 107.88(16) ?
O23 C34 N24 . . 125.09(19) ?
O23 C34 C33 . . 128.66(19) ?
N24 C34 C33 . . 106.25(15) ?
C34 N24 C35 . . 111.81(16) ?
C34 N24 C40 . . 124.40(16) ?
C35 N24 C40 . . 123.79(17) ?
O24 C35 N24 . . 125.53(19) ?
O24 C35 C36 . . 128.47(18) ?
N24 C35 C36 . . 105.97(15) ?
C37 C36 C33 . . 121.82(17) ?
C37 C36 C35 . . 130.10(16) ?
C33 C36 C35 . . 108.03(16) ?
C36 C37 C38 . . 116.85(16) ?
C36 C37 H37 . . 121.6 ?
C38 C37 H37 . . 121.6 ?
C37 C38 C31 . . 122.92(17) ?
C37 C38 N21 . . 116.45(16) ?
C31 C38 N21 . . 120.41(17) ?
N23 C39 H39A . . 109.5 ?
N23 C39 H39B . . 109.5 ?
H39A C39 H39B . . 109.5 ?
N23 C39 H39C . . 109.5 ?
H39A C39 H39C . . 109.5 ?
H39B C39 H39C . . 109.5 ?
N23 C39 H39D . . 109.5 ?
H39A C39 H39D . . 141.1 ?
H39B C39 H39D . . 56.3 ?
H39C C39 H39D . . 56.3 ?
N23 C39 H39E . . 109.5 ?
H39A C39 H39E . . 56.3 ?
H39B C39 H39E . . 141.1 ?
H39C C39 H39E . . 56.3 ?
H39D C39 H39E . . 109.5 ?
N23 C39 H39F . . 109.5 ?
H39A C39 H39F . . 56.3 ?
H39B C39 H39F . . 56.3 ?
H39C C39 H39F . . 141.1 ?
H39D C39 H39F . . 109.5 ?
H39E C39 H39F . . 109.5 ?
N24 C40 H40A . . 109.5 ?
N24 C40 H40B . . 109.5 ?
H40A C40 H40B . . 109.5 ?
N24 C40 H40C . . 109.5 ?
H40A C40 H40C . . 109.5 ?
H40B C40 H40C . . 109.5 ?
N24 C40 H40D . . 109.5 ?
H40A C40 H40D . . 141.1 ?
H40B C40 H40D . . 56.3 ?
H40C C40 H40D . . 56.3 ?
N24 C40 H40E . . 109.5 ?
H40A C40 H40E . . 56.3 ?
H40B C40 H40E . . 141.1 ?
H40C C40 H40E . . 56.3 ?
H40D C40 H40E . . 109.5 ?
N24 C40 H40F . . 109.5 ?
H40A C40 H40F . . 56.3 ?
H40B C40 H40F . . 56.3 ?
H40C C40 H40F . . 141.1 ?
H40D C40 H40F . . 109.5 ?
H40E C40 H40F . . 109.5 ?
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 N2 . 1.246(2) ?
N1 C18 . 1.452(2) ?
N2 C1 . 1.456(2) ?
C1 C2 . 1.391(3) ?
C1 C8 . 1.405(3) ?
C2 C3 . 1.387(2) ?
C2 H2 . 0.9500 ?
C3 C6 . 1.389(2) ?
C3 C4 . 1.488(2) ?
C4 O1 . 1.212(2) ?
C4 N3 . 1.392(2) ?
N3 C5 . 1.390(2) ?
N3 C19 . 1.455(2) ?
C5 O2 . 1.217(2) ?
C5 C6 . 1.489(2) ?
C6 C7 . 1.379(3) ?
C7 C8 . 1.400(3) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.506(3) ?
C9 C10 . 1.543(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C11 . 1.514(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.404(2) ?
C11 C18 . 1.406(3) ?
C12 C13 . 1.381(3) ?
C12 H12 . 0.9500 ?
C13 C16 . 1.387(3) ?
C13 C14 . 1.490(2) ?
C14 O3 . 1.216(2) ?
C14 N4 . 1.393(3) ?
N4 C15 . 1.397(3) ?
N4 C20 . 1.456(2) ?
C15 O4 . 1.205(2) ?
C15 C16 . 1.488(3) ?
C16 C17 . 1.381(3) ?
C17 C18 . 1.399(3) ?
C17 H17 . 0.9500 ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
C19 H19D . 0.9800 ?
C19 H19E . 0.9800 ?
C19 H19F . 0.9800 ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
C20 H20D . 0.9800 ?
C20 H20E . 0.9800 ?
C20 H20F . 0.9800 ?
N21 N22 . 1.255(3) ?
N21 C38 . 1.449(2) ?
N22 C21 . 1.452(2) ?
C21 C22 . 1.392(3) ?
C21 C28 . 1.407(2) ?
C22 C23 . 1.377(3) ?
C22 H22 . 0.9500 ?
C23 C26 . 1.388(2) ?
C23 C24 . 1.492(2) ?
C24 O21 . 1.215(2) ?
C24 N23 . 1.382(2) ?
N23 C25 . 1.399(2) ?
N23 C39 . 1.451(3) ?
C25 O22 . 1.207(2) ?
C25 C26 . 1.487(3) ?
C26 C27 . 1.383(3) ?
C27 C28 . 1.392(3) ?
C27 H27 . 0.9500 ?
C28 C29 . 1.504(3) ?
C29 C30 . 1.544(3) ?
C29 H29A . 0.9900 ?
C29 H29B . 0.9900 ?
C30 C31 . 1.507(3) ?
C30 H30A . 0.9900 ?
C30 H30B . 0.9900 ?
C31 C38 . 1.403(2) ?
C31 C32 . 1.406(3) ?
C32 C33 . 1.378(3) ?
C32 H32 . 0.9500 ?
C33 C36 . 1.392(2) ?
C33 C34 . 1.487(3) ?
C34 O23 . 1.217(2) ?
C34 N24 . 1.393(2) ?
N24 C35 . 1.397(3) ?
N24 C40 . 1.460(3) ?
C35 O24 . 1.208(2) ?
C35 C36 . 1.488(3) ?
C36 C37 . 1.373(3) ?
C37 C38 . 1.395(3) ?
C37 H37 . 0.9500 ?
C39 H39A . 0.9800 ?
C39 H39B . 0.9800 ?
C39 H39C . 0.9800 ?
C39 H39D . 0.9800 ?
C39 H39E . 0.9800 ?
C39 H39F . 0.9800 ?
C40 H40A . 0.9800 ?
C40 H40B . 0.9800 ?
C40 H40C . 0.9800 ?
C40 H40D . 0.9800 ?
C40 H40E . 0.9800 ?
C40 H40F . 0.9800 ?
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
C18 N1 N2 C1 . . . . 3.1(3) ?
N1 N2 C1 C2 . . . . -108.0(2) ?
N1 N2 C1 C8 . . . . 80.7(2) ?
C8 C1 C2 C3 . . . . 0.3(2) ?
N2 C1 C2 C3 . . . . -170.52(14) ?
C1 C2 C3 C6 . . . . 1.5(2) ?
C1 C2 C3 C4 . . . . 178.86(15) ?
C2 C3 C4 O1 . . . . 5.6(3) ?
C6 C3 C4 O1 . . . . -176.78(16) ?
C2 C3 C4 N3 . . . . -174.53(16) ?
C6 C3 C4 N3 . . . . 3.10(17) ?
O1 C4 N3 C5 . . . . 176.38(15) ?
C3 C4 N3 C5 . . . . -3.50(17) ?
O1 C4 N3 C19 . . . . 6.0(3) ?
C3 C4 N3 C19 . . . . -173.93(14) ?
C4 N3 C5 O2 . . . . -178.44(15) ?
C19 N3 C5 O2 . . . . -7.9(2) ?
C4 N3 C5 C6 . . . . 2.54(17) ?
C19 N3 C5 C6 . . . . 173.06(14) ?
C2 C3 C6 C7 . . . . -2.2(2) ?
C4 C3 C6 C7 . . . . 179.94(14) ?
C2 C3 C6 C5 . . . . 176.28(14) ?
C4 C3 C6 C5 . . . . -1.62(17) ?
O2 C5 C6 C7 . . . . -1.1(3) ?
N3 C5 C6 C7 . . . . 177.83(15) ?
O2 C5 C6 C3 . . . . -179.41(16) ?
N3 C5 C6 C3 . . . . -0.45(17) ?
C3 C6 C7 C8 . . . . 0.9(2) ?
C5 C6 C7 C8 . . . . -177.17(15) ?
C6 C7 C8 C1 . . . . 0.9(2) ?
C6 C7 C8 C9 . . . . -178.32(15) ?
C2 C1 C8 C7 . . . . -1.5(2) ?
N2 C1 C8 C7 . . . . 169.28(15) ?
C2 C1 C8 C9 . . . . 177.72(15) ?
N2 C1 C8 C9 . . . . -11.5(2) ?
C7 C8 C9 C10 . . . . 103.58(19) ?
C1 C8 C9 C10 . . . . -75.6(2) ?
C8 C9 C10 C11 . . . . 24.9(2) ?
C9 C10 C11 C12 . . . . -132.48(17) ?
C9 C10 C11 C18 . . . . 52.9(2) ?
C18 C11 C12 C13 . . . . 2.6(2) ?
C10 C11 C12 C13 . . . . -172.29(16) ?
C11 C12 C13 C16 . . . . 0.9(3) ?
C11 C12 C13 C14 . . . . 176.91(17) ?
C12 C13 C14 O3 . . . . 5.3(3) ?
C16 C13 C14 O3 . . . . -178.23(19) ?
C12 C13 C14 N4 . . . . -175.21(18) ?
C16 C13 C14 N4 . . . . 1.23(19) ?
O3 C14 N4 C15 . . . . 179.75(18) ?
C13 C14 N4 C15 . . . . 0.3(2) ?
O3 C14 N4 C20 . . . . -0.9(3) ?
C13 C14 N4 C20 . . . . 179.58(16) ?
C14 N4 C15 O4 . . . . 175.77(18) ?
C20 N4 C15 O4 . . . . -3.5(3) ?
C14 N4 C15 C16 . . . . -1.5(2) ?
C20 N4 C15 C16 . . . . 179.14(16) ?
C12 C13 C16 C17 . . . . -2.8(3) ?
C14 C13 C16 C17 . . . . -179.63(16) ?
C12 C13 C16 C15 . . . . 174.62(16) ?
C14 C13 C16 C15 . . . . -2.2(2) ?
O4 C15 C16 C17 . . . . 2.2(3) ?
N4 C15 C16 C17 . . . . 179.48(18) ?
O4 C15 C16 C13 . . . . -174.94(19) ?
N4 C15 C16 C13 . . . . 2.31(19) ?
C13 C16 C17 C18 . . . . 1.0(3) ?
C15 C16 C17 C18 . . . . -175.87(17) ?
C16 C17 C18 C11 . . . . 2.7(3) ?
C16 C17 C18 N1 . . . . 177.19(15) ?
C12 C11 C18 C17 . . . . -4.6(3) ?
C10 C11 C18 C17 . . . . 170.06(17) ?
C12 C11 C18 N1 . . . . -178.51(16) ?
C10 C11 C18 N1 . . . . -3.9(3) ?
N2 N1 C18 C17 . . . . 114.4(2) ?
N2 N1 C18 C11 . . . . -71.1(2) ?
C38 N21 N22 C21 . . . . -0.4(3) ?
N21 N22 C21 C22 . . . . 104.5(2) ?
N21 N22 C21 C28 . . . . -82.0(2) ?
C28 C21 C22 C23 . . . . 0.0(3) ?
N22 C21 C22 C23 . . . . 173.23(16) ?
C21 C22 C23 C26 . . . . -2.0(3) ?
C21 C22 C23 C24 . . . . 179.93(17) ?
C22 C23 C24 O21 . . . . -5.1(3) ?
C26 C23 C24 O21 . . . . 176.64(18) ?
C22 C23 C24 N23 . . . . 175.73(17) ?
C26 C23 C24 N23 . . . . -2.54(19) ?
O21 C24 N23 C25 . . . . -176.75(17) ?
C23 C24 N23 C25 . . . . 2.46(19) ?
O21 C24 N23 C39 . . . . -3.9(3) ?
C23 C24 N23 C39 . . . . 175.32(16) ?
C24 N23 C25 O22 . . . . 179.65(17) ?
C39 N23 C25 O22 . . . . 6.8(3) ?
C24 N23 C25 C26 . . . . -1.46(19) ?
C39 N23 C25 C26 . . . . -174.31(17) ?
C22 C23 C26 C27 . . . . 2.5(3) ?
C24 C23 C26 C27 . . . . -179.01(15) ?
C22 C23 C26 C25 . . . . -176.78(16) ?
C24 C23 C26 C25 . . . . 1.68(19) ?
O22 C25 C26 C27 . . . . -0.6(3) ?
N23 C25 C26 C27 . . . . -179.46(17) ?
O22 C25 C26 C23 . . . . 178.60(18) ?
N23 C25 C26 C23 . . . . -0.23(19) ?
C23 C26 C27 C28 . . . . -0.9(3) ?
C25 C26 C27 C28 . . . . 178.22(17) ?
C26 C27 C28 C21 . . . . -1.0(3) ?
C26 C27 C28 C29 . . . . 178.33(16) ?
C22 C21 C28 C27 . . . . 1.5(3) ?
N22 C21 C28 C27 . . . . -171.66(16) ?
C22 C21 C28 C29 . . . . -177.86(17) ?
N22 C21 C28 C29 . . . . 9.0(3) ?
C27 C28 C29 C30 . . . . -111.8(2) ?
C21 C28 C29 C30 . . . . 67.5(2) ?
C28 C29 C30 C31 . . . . -7.7(3) ?
C29 C30 C31 C38 . . . . -66.5(2) ?
C29 C30 C31 C32 . . . . 118.0(2) ?
C38 C31 C32 C33 . . . . -3.6(3) ?
C30 C31 C32 C33 . . . . 172.12(16) ?
C31 C32 C33 C36 . . . . -0.3(3) ?
C31 C32 C33 C34 . . . . -176.74(17) ?
C32 C33 C34 O23 . . . . -5.6(3) ?
C36 C33 C34 O23 . . . . 177.63(19) ?
C32 C33 C34 N24 . . . . 175.08(18) ?
C36 C33 C34 N24 . . . . -1.68(19) ?
O23 C34 N24 C35 . . . . -179.27(18) ?
C33 C34 N24 C35 . . . . 0.1(2) ?
O23 C34 N24 C40 . . . . 1.3(3) ?
C33 C34 N24 C40 . . . . -179.33(16) ?
C34 N24 C35 O24 . . . . -176.70(18) ?
C40 N24 C35 O24 . . . . 2.7(3) ?
C34 N24 C35 C36 . . . . 1.4(2) ?
C40 N24 C35 C36 . . . . -179.15(16) ?
C32 C33 C36 C37 . . . . 2.9(3) ?
C34 C33 C36 C37 . . . . -179.96(16) ?
C32 C33 C36 C35 . . . . -174.60(15) ?
C34 C33 C36 C35 . . . . 2.54(19) ?
O24 C35 C36 C37 . . . . -1.6(3) ?
N24 C35 C36 C37 . . . . -179.70(18) ?
O24 C35 C36 C33 . . . . 175.58(19) ?
N24 C35 C36 C33 . . . . -2.48(19) ?
C33 C36 C37 C38 . . . . -1.3(3) ?
C35 C36 C37 C38 . . . . 175.60(17) ?
C36 C37 C38 C31 . . . . -2.9(3) ?
C36 C37 C38 N21 . . . . -177.46(15) ?
C32 C31 C38 C37 . . . . 5.3(3) ?
C30 C31 C38 C37 . . . . -170.33(17) ?
C32 C31 C38 N21 . . . . 179.70(16) ?
C30 C31 C38 N21 . . . . 4.1(3) ?
N22 N21 C38 C37 . . . . -113.5(2) ?
N22 N21 C38 C31 . . . . 71.8(2) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5939 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.4061 0.9995 0.0013 0.0030 -0.0046 -1.0005 -0.0008 -0.0599 0.0021 -1.0009