#------------------------------------------------------------------------------
#$Date: 2024-05-06 07:20:48 +0300 (Mon, 06 May 2024) $
#$Revision: 291722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023070.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_2023070
loop_
_publ_author_name
'Metwally, Nadia H.'
'Elgemeie, Galal H.'
'Abd Al-Latif, El-Shimaa S M'
'Jones, Peter G.'
_publ_section_title
;
Crystal structure of
2,4-di-amino-5-(4-hy-droxy-3-meth-oxy-phen-yl)-8,8-dimethyl-6-oxo-6,7,8,9-tetra-hydro-5H-chromeno[2,3-b]pyridine-3-carbo-nitrile-di-methyl-formamide-water
(1/1/1).
;
_journal_coeditor_code YZ2052
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 396
_journal_page_last 400
_journal_paper_doi 10.1107/S2056989024002615
_journal_volume 80
_journal_year 2024
_chemical_formula_moiety 'C22 H22 N4 O4, C3 H7 N O, H2 O'
_chemical_formula_sum 'C25 H31 N5 O6'
_chemical_formula_weight 497.55
_chemical_name_systematic
'2,4-Diamino-5-(4-hydroxy-3-methoxyphenyl)-8,8-dimethyl-6-oxo-6,7,8,9-tetrahydro-5H-chromeno[2,3-b]pyridine-3-carbonitrile--dimethylformamide--water (1/1/1)'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 106.344(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.9055(2)
_cell_length_b 15.9600(3)
_cell_length_c 16.4794(4)
_cell_measurement_reflns_used 76991
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 39.5630
_cell_measurement_theta_min 2.1720
_cell_volume 2499.98(10)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0(4)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0559
_diffrn_reflns_av_unetI/netI 0.0224
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 210685
_diffrn_reflns_theta_full 37.500
_diffrn_reflns_theta_max 37.784
_diffrn_reflns_theta_min 2.167
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.096
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73482
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.322
_exptl_crystal_description tablet
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.668
_refine_diff_density_min -0.217
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 358
_refine_ls_number_reflns 13416
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.0485
_refine_ls_R_factor_gt 0.0377
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1062
_refine_ls_wR_factor_ref 0.1138
_reflns_number_gt 11108
_reflns_number_total 13416
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2052.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023070.cif.'
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023070
_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 0.981
_shelx_estimated_absorpt_t_max 0.990
_shelx_hkl_file
;
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0 0 2 82.2823 6.29503 24
0 0 -2 98.8815 6.30227 24
0 0 -2 90.2072 6.28678 10
0 0 2 99.3103 6.28442 10
0 0 -3 1.02895 0.73240 24
0 0 3 0.33370 0.76413 24
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0 0 3 0.10176 0.83917 2
0 0 3-0.25307 0.56099 18
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0 0 -4 3499.34 235.033 14
0 0 -4 3454.84 235.209 2
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0 0 5-0.21961 0.92261 6
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0 0 5-0.59147 1.13084 2
0 0 -5-1.23344 1.18685 1
0 0 -5-1.07653 1.16210 2
0 0 -5 1.09529 0.63949 18
0 0 -5-0.27454 0.62570 14
0 0 5 1.01969 0.83385 10
0 0 -6 2137.05 167.371 24
0 0 6 2669.98 167.454 6
0 0 -6 2527.23 167.509 1
0 0 6 2543.93 167.516 2
0 0 -6 2665.30 167.311 18
0 0 -6 2631.03 167.235 14
0 0 6 2488.22 167.188 13
0 0 6 2629.86 167.394 10
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0 0 8 2.71548 1.78020 11
0 0 -8 3.61750 1.34344 10
0 0 -9-1.07161 1.33325 24
0 0 9-0.88493 1.43407 6
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0 0 9-1.50366 1.55195 2
0 0 -9-0.50604 1.64185 1
0 0 -9-0.21390 0.89329 18
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0 0 -9-0.48314 1.19596 10
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0 0 10 1.56510 1.47339 5
0 0 -10 0.49537 0.80281 14
0 0 -10 0.57026 1.78946 1
0 0 -11 0.84577 1.87598 1
0 0 -11-0.15123 1.52953 10
0 0 11 0.49098 2.11854 11
0 0 -11-0.08365 0.98300 18
0 0 -11-0.68037 0.82744 14
0 0 11 0.74124 1.02223 15
0 0 11 1.38939 1.69887 5
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0 0 -12 1414.12 90.0401 6
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0 0 12 1485.25 90.1200 24
0 0 -12 1484.94 89.5125 18
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0 0 -12 1499.44 89.8364 10
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17 -1 -10 9.50826 5.50097 14
17 1 -10 4.76167 5.03400 14
17 1 -10 15.4332 5.91820 15
-17 -1 9 4.40754 4.78539 8
-17 1 9 3.48025 4.74630 8
17 -1 -9-1.33210 6.01522 25
17 1 -9-2.02783 5.53078 25
17 -1 -9-2.06935 5.13558 14
17 1 -9-1.03771 5.50780 14
17 -1 -9 6.25766 5.76469 15
17 1 -9 4.92706 5.72074 15
-17 -1 8 20.1951 5.24728 8
-17 1 8 19.6178 5.32845 8
17 -1 -8 16.1722 5.37490 14
17 1 -8 27.3526 5.37525 14
17 -1 -8 7.53670 5.70009 15
17 1 -8 27.8114 6.46295 15
17 -1 -8 14.1803 6.11007 25
17 1 -8 11.6242 6.35988 25
17 -1 -7 47.1403 7.24755 25
17 1 -7 39.9374 7.39028 25
-17 1 7 26.6662 4.78293 6
-17 -1 7 35.8262 5.68024 8
-17 1 7 38.5185 6.07091 8
17 -1 -7 45.7565 6.63270 21
17 1 -7 43.3531 6.61328 21
17 -1 -7 34.4218 6.07548 14
17 1 -7 34.5631 6.01148 14
17 -1 -7 25.0318 6.56253 15
17 1 -7 31.9776 6.55857 15
-17 -1 7 27.6513 5.77523 10
17 -1 -6-2.76716 5.98893 25
17 -1 -6-4.16845 5.25165 21
17 1 -6 5.63797 5.24991 21
17 -1 -6 0.47705 4.64343 14
17 1 -6-0.47814 4.67719 14
17 -1 -6 4.97876 5.61994 15
17 1 -6-0.61031 5.34960 15
-17 1 6 3.87795 4.68927 10
-17 -1 6 1.64340 4.55993 10
-17 1 6 3.41866 3.60422 6
-17 -1 6-2.45840 4.45284 8
-17 1 6-4.19194 4.74546 8
-17 1 5 3.89295 3.57586 6
-17 -1 5-2.81947 4.34042 8
-17 1 5-2.52345 4.53105 8
17 -1 -5-0.60690 5.03464 21
17 1 -5-1.27582 5.06975 21
17 -1 -5-5.06024 4.74797 14
17 1 -5 14.5819 5.81005 15
-17 1 4 6.38080 3.86971 6
-17 1 4 4.85856 4.29584 8
17 -1 -4 6.79661 5.35149 21
17 1 -4 16.8428 5.73097 21
17 -1 -4 3.97231 4.43542 14
17 -1 -3 1.25872 5.18568 21
-17 1 3 0.40844 3.78389 6
-17 1 3-4.65005 4.41287 8
-17 1 2 2.09189 3.76962 6
-17 -2 14 18.6725 5.11856 17
-17 2 13 67.8700 7.53867 17
-17 2 12 0.52089 4.32337 17
17 -2 -12-4.98221 6.09354 25
-17 -2 12-2.96966 4.94589 8
17 -2 -11-4.83467 5.71353 14
17 2 -11-3.23043 5.51997 14
17 -2 -11 6.34883 5.78262 25
17 2 -11 9.32637 5.96326 25
-17 -2 11-1.72604 4.86997 8
-17 2 11-0.62395 5.28137 8
17 -2 -10 20.0496 5.79859 14
17 2 -10 28.0743 5.97700 14
17 -2 -10 18.8355 6.25427 25
17 2 -10 15.4506 6.18805 25
-17 -2 10 22.7917 5.56522 8
-17 2 10 26.7425 5.84548 8
17 -2 -9 64.5631 8.01975 14
17 2 -9 85.7945 8.48324 14
17 -2 -9 88.2704 9.31336 15
17 2 -9 73.8890 8.80562 15
17 -2 -9 84.9779 9.32544 25
17 2 -9 88.8703 9.24320 25
-17 2 9 57.8960 7.06023 6
-17 2 9 90.3926 8.97264 8
-17 -2 9 93.8469 8.41500 8
17 -2 -8-3.34497 5.91876 25
17 2 -8 9.59047 6.13316 25
-17 2 8 2.66005 3.59797 6
-17 -2 8-3.09625 4.60716 8
-17 2 8 0.57408 4.84454 8
17 -2 -8-5.04176 5.35244 14
17 2 -8 0.50728 4.97566 14
17 -2 -8 0.63253 5.57943 15
17 2 -8-7.96192 5.46745 15
-17 -2 8-7.43522 4.55550 10
17 -2 -7 14.2446 5.89270 25
-17 2 7 12.8247 3.96297 6
-17 -2 7 31.6192 5.20543 8
-17 2 7 17.8108 5.26828 8
17 -2 -7 13.6150 5.37894 21
17 2 -7 29.1690 5.96907 21
17 -2 -7 5.88819 5.00440 14
17 -2 -7 11.3555 5.84413 15
17 2 -7 31.6266 6.34093 15
-17 -2 7 16.6631 4.94740 10
17 -2 -6 6.19360 5.92503 25
17 -2 -6 5.77146 4.67794 21
17 2 -6 8.96783 5.39165 21
17 -2 -6 7.61218 4.92726 14
17 -2 -6 5.65593 5.53067 15
17 2 -6 3.62075 5.32741 15
-17 -2 6 1.62829 4.50913 10
-17 2 6 1.19235 3.61790 6
-17 -2 6 6.62614 4.09169 8
-17 2 6-4.84893 4.81477 8
-17 2 5 2.84599 3.88193 6
-17 2 5 1.56175 4.67181 8
17 -2 -5 10.0153 4.98129 21
17 2 -5 6.47922 5.23609 21
17 -2 -5 6.88425 4.67471 14
-17 2 4 2.49495 3.76237 6
-17 2 4 8.01290 4.48510 8
17 -2 -4 11.4142 5.31087 21
17 -2 -4 3.95983 4.46516 14
17 -2 -3 3.67718 5.17301 21
-17 2 3 8.68246 4.43370 8
-17 2 3-2.12363 3.91560 6
-17 2 2 30.0791 5.18098 8
-17 3 13-1.10120 4.67639 17
-17 3 12 0.52794 4.58641 17
-17 -3 12-0.57799 4.79641 8
17 -3 -12-6.12748 5.73868 25
-17 3 11 140.384 10.6055 17
17 -3 -11 117.199 11.1938 25
-17 -3 11 128.506 10.7921 8
17 -3 -10 17.3816 5.55587 14
17 3 -10 18.5622 5.61542 14
17 -3 -10 34.5499 6.60652 25
-17 3 10 20.2569 4.07852 6
-17 -3 10 22.0919 5.46675 8
-17 3 10 19.7335 5.75825 8
17 -3 -9 40.4573 7.19894 25
17 -3 -9 37.1101 6.40540 14
-17 -3 9 44.0295 6.09770 10
-17 3 9 35.8732 5.22005 6
-17 -3 9 58.6120 6.74551 8
-17 3 9 60.2356 7.29935 8
17 -3 -8-5.30398 5.86576 25
-17 3 8-3.58152 3.76772 6
-17 -3 8 8.46106 4.68663 8
-17 3 8 5.86355 5.02935 8
17 -3 -8 1.50953 5.06672 14
-17 -3 8 6.30599 4.49319 10
17 -3 -7 37.7830 7.01285 25
-17 3 7 30.0855 5.05457 6
-17 -3 7 34.2969 5.61302 8
-17 3 7 38.0650 6.22093 8
17 -3 -7 45.3544 6.30529 21
17 3 -7 39.4842 6.64450 21
17 -3 -7 35.2385 6.05481 14
-17 -3 7 38.7998 5.92720 10
17 -3 -6 15.6063 5.23163 21
17 3 -6 11.0992 5.54676 21
17 -3 -6 9.01618 4.98390 14
17 -3 -6 2.05593 5.70312 25
-17 3 6 10.7892 4.13110 6
-17 3 6 10.4628 5.11418 8
-17 3 5 66.0378 7.16186 6
-17 3 5 75.7827 8.02866 8
17 -3 -5 76.9039 8.26491 21
17 -3 -5 72.7413 7.73725 14
-17 3 4 8.20650 3.94389 6
-17 3 4 5.67764 4.49106 8
17 -3 -4-0.58186 5.27682 21
17 -3 -4 2.63355 4.44786 14
17 -3 -3 17.8347 5.54400 21
-17 3 3 8.47187 4.69824 8
-17 3 3 6.60355 4.01621 6
-17 -4 12-0.56315 4.74185 8
-17 4 12-3.86780 3.59112 6
17 -4 -12 0.60003 5.39280 25
-17 4 12-8.57814 5.02623 17
-17 -4 11 2.17343 4.89684 8
-17 4 11 5.90928 3.74279 6
17 -4 -11 12.3060 5.63638 25
-17 4 11 7.18790 4.33819 17
17 -4 -10 207.921 16.2422 25
-17 -4 10 233.055 15.6714 8
17 -4 -9 18.0252 5.47590 14
17 -4 -9 13.5106 5.85905 25
-17 4 9 15.5213 4.38264 6
-17 -4 9 20.4923 5.07255 8
-17 4 9 21.3848 5.71647 8
17 -4 -8 62.3021 7.73769 14
17 -4 -8 85.9029 9.14358 25
-17 4 8 65.7101 6.83375 6
-17 -4 8 79.8824 7.52360 8
-17 4 8 55.9817 7.63656 8
-17 4 7 1.27066 3.77010 6
-17 4 7 3.47834 4.77693 8
17 -4 -7 4.19393 4.51062 21
17 -4 -7-3.41860 4.97396 14
-17 4 6 69.9724 7.42048 6
-17 4 6 78.8636 8.46595 8
17 -4 -6 85.0051 8.31386 21
17 -4 -6 76.6487 8.00742 14
-17 4 5-1.75921 3.91889 6
-17 4 5 7.10722 4.85472 8
17 -4 -5 9.32936 5.19735 21
17 -4 -5 2.28129 4.58684 14
-17 4 4 0.44770 3.86387 6
-17 4 4 6.33540 4.82253 8
17 -4 -4-5.61410 4.90605 21
17 -4 -4 2.18837 4.38572 14
17 -4 -3 6.32056 4.96048 21
-17 -5 12 19.6051 5.35524 8
-17 5 12 19.8831 4.32382 6
-17 -5 11 6.29075 4.83642 8
-17 5 11 9.90791 3.85664 6
-17 5 11 9.37526 4.67074 17
-17 -5 10-4.52742 4.55963 8
-17 5 10-2.93736 3.92304 6
17 -5 -10-4.96312 5.68576 25
-17 5 10 0.49714 4.38829 17
17 -5 -9-10.7742 5.85578 25
-17 5 9 2.13032 3.93810 6
-17 5 8 19.9200 4.54784 6
17 -5 -8 31.6225 5.74145 14
-17 5 7-3.52550 3.91030 6
17 -5 -7 2.50231 4.64841 21
17 -5 -7 0.48757 4.85122 14
-17 5 6-2.68783 3.85562 6
17 -5 -6 6.13958 4.52736 21
17 -5 -6 4.24822 4.91630 14
17 -5 -5 5.23253 4.54357 21
17 -5 -5 10.4620 4.88413 14
17 -5 -4 11.3284 4.81040 21
17 -5 -4 7.41429 4.49277 14
-17 6 10 6.57417 4.34419 17
17 -6 -6 54.9408 6.74800 21
17 -6 -5 31.9286 5.63579 21
17 -6 -4 3.59131 4.59864 21
0 0 0 0.00 0.00 0
TITL elg_ns1 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 9.905499 15.959973 16.479412 90.0000 106.3437 90.0000
ZERR 4.00 0.000106 0.000148 0.000186 0.0000 0.0012 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 100.00 120.00 16.00 20.00
REM CrysAlisPro recorded range (K): Min=99.7; max=100.3; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 45293
_shelx_res_file
;
TITL elg_ns1 in P2(1)/n
shelx.res
created by SHELXL-2019/3 at 15:05:55 on 22-Jan-2024
CELL 0.71073 9.905499 15.959973 16.479412 90.0000 106.3437 90.0000
ZERR 4.00 0.0002 0.0003 0.0004 0.0000 0.0024 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 100 124 20 24
TEMP -173
SIZE 0.2 0.2 0.1
SHEL 999 0.58
L.S. 6
FMAP 2
PLAN 10
ACTA 75
CONF
BOND $H
OMIT 2 2 5
OMIT -2 1 6
OMIT 1 4 12
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z
HTAB N2 O1_$1
HTAB N2 O98
EQIV $2 x+1, y, z
HTAB N4 O98_$2
EQIV $3 -x+1, -y+2, -z+1
HTAB N4 N3_$3
HTAB O3 O99
EQIV $4 -x+5/2, y+1/2, -z+3/2
HTAB O99 O1_$4
EQIV $5 -x+3/2, y+1/2, -z+3/2
HTAB O99 N1_$5
HTAB O99 O10_$5
HTAB C22 O98_$2
WGHT 0.062600 0.408200
FVAR 0.69082
N1 3 0.410403 0.668452 0.582865 11.00000 0.01093 0.01421 =
0.02248 0.00266 0.00540 0.00127
C2 1 0.356814 0.744084 0.556755 11.00000 0.01156 0.01457 =
0.01581 0.00067 0.00391 0.00106
N2 3 0.216223 0.752996 0.542442 11.00000 0.01142 0.01775 =
0.02852 0.00442 0.00582 0.00216
H01 2 0.168335 0.709124 0.552236 11.00000 0.02943
H02 2 0.169214 0.798334 0.519678 11.00000 0.03230
C3 1 0.444573 0.810520 0.545497 11.00000 0.01208 0.01273 =
0.01480 0.00130 0.00318 0.00120
C4 1 0.591138 0.796889 0.559894 11.00000 0.01184 0.01280 =
0.01307 0.00058 0.00285 0.00009
N4 3 0.674856 0.858129 0.545117 11.00000 0.01292 0.01354 =
0.02215 0.00403 0.00446 -0.00014
H03 2 0.761199 0.850286 0.553952 11.00000 0.02955
H04 2 0.642453 0.907588 0.529598 11.00000 0.03248
C4A 1 0.646241 0.716876 0.588227 11.00000 0.01060 0.01223 =
0.01442 0.00092 0.00292 0.00021
C5 1 0.800701 0.695513 0.605318 11.00000 0.01039 0.01210 =
0.01403 0.00053 0.00309 -0.00016
AFIX 13
H5 2 0.832899 0.714157 0.555889 11.00000 -1.20000
AFIX 0
C5A 1 0.818255 0.601667 0.614090 11.00000 0.01084 0.01237 =
0.01570 0.00069 0.00333 0.00037
C6 1 0.949690 0.563932 0.609922 11.00000 0.01133 0.01428 =
0.01549 0.00048 0.00311 0.00046
O1 4 1.038519 0.605917 0.588035 11.00000 0.01310 0.01693 =
0.02538 0.00243 0.00763 -0.00010
C7 1 0.975384 0.471807 0.630574 11.00000 0.01393 0.01443 =
0.02129 0.00277 0.00530 0.00266
AFIX 23
H7A 2 1.075931 0.463992 0.661303 11.00000 -1.20000
H7B 2 0.956598 0.440073 0.576928 11.00000 -1.20000
AFIX 0
C8 1 0.885876 0.434398 0.683868 11.00000 0.01443 0.01423 =
0.02238 0.00436 0.00503 0.00181
C9 1 0.732043 0.458168 0.641352 11.00000 0.01330 0.01286 =
0.02656 0.00304 0.00501 0.00028
AFIX 23
H9A 2 0.698047 0.427626 0.587129 11.00000 -1.20000
H9B 2 0.673250 0.441184 0.678188 11.00000 -1.20000
AFIX 0
C9A 1 0.716998 0.550188 0.625219 11.00000 0.01132 0.01308 =
0.01900 0.00187 0.00398 0.00082
O10 4 0.585526 0.577474 0.622457 11.00000 0.01171 0.01288 =
0.02909 0.00510 0.00737 0.00140
C10A 1 0.548673 0.658606 0.597009 11.00000 0.01180 0.01265 =
0.01783 0.00174 0.00446 0.00074
C11 1 0.386200 0.890037 0.517092 11.00000 0.01298 0.01587 =
0.01980 0.00216 0.00297 0.00068
N3 3 0.340378 0.955348 0.494193 11.00000 0.01865 0.01773 =
0.03662 0.00751 0.00382 0.00268
C12 1 0.932119 0.468134 0.774709 11.00000 0.02407 0.02668 =
0.02003 0.00681 0.00464 0.00263
AFIX 137
H12A 2 1.026948 0.447741 0.803183 11.00000 -1.50000
H12B 2 0.866481 0.448682 0.805418 11.00000 -1.50000
H12C 2 0.932458 0.529524 0.773538 11.00000 -1.50000
AFIX 0
C13 1 0.902376 0.338956 0.686448 11.00000 0.02096 0.01502 =
0.03959 0.00759 0.00942 0.00374
AFIX 137
H13A 2 0.867471 0.316360 0.629044 11.00000 -1.50000
H13B 2 0.848265 0.314956 0.722263 11.00000 -1.50000
H13C 2 1.001952 0.324471 0.709689 11.00000 -1.50000
AFIX 0
C21 1 0.891092 0.739092 0.684865 11.00000 0.01090 0.01291 =
0.01364 0.00041 0.00269 -0.00027
C22 1 0.982700 0.804129 0.678800 11.00000 0.01250 0.01415 =
0.01379 0.00045 0.00278 -0.00121
AFIX 43
H22 2 0.991495 0.819834 0.624914 11.00000 -1.20000
AFIX 0
C23 1 1.061204 0.846136 0.750940 11.00000 0.01420 0.01438 =
0.01514 0.00023 0.00256 -0.00214
O2 4 1.151184 0.911167 0.750308 11.00000 0.02159 0.01943 =
0.01761 -0.00127 0.00363 -0.00873
C24 1 1.051859 0.821997 0.831283 11.00000 0.01803 0.01691 =
0.01356 -0.00018 0.00167 -0.00189
O3 4 1.128717 0.858244 0.903937 11.00000 0.03428 0.02433 =
0.01417 -0.00124 0.00005 -0.01154
H05 2 1.164796 0.907177 0.897118 11.00000 0.03407
C25 1 0.962444 0.756538 0.836722 11.00000 0.02014 0.01849 =
0.01373 0.00106 0.00417 -0.00243
AFIX 43
H25 2 0.955884 0.739310 0.890663 11.00000 -1.20000
AFIX 0
C26 1 0.882136 0.715648 0.764463 11.00000 0.01537 0.01582 =
0.01525 0.00110 0.00414 -0.00179
AFIX 43
H26 2 0.820851 0.671449 0.769635 11.00000 -1.20000
AFIX 0
C27 1 1.168715 0.933546 0.670302 11.00000 0.02419 0.01966 =
0.02150 -0.00018 0.00776 -0.00715
AFIX 137
H27A 2 1.077008 0.947598 0.631269 11.00000 -1.50000
H27B 2 1.209836 0.886314 0.647569 11.00000 -1.50000
H27C 2 1.231375 0.982140 0.676969 11.00000 -1.50000
AFIX 0
C97 1 -0.129716 0.839367 0.408947 11.00000 0.01951 0.02568 =
0.01723 0.00379 0.00489 0.00279
AFIX 43
H97 2 -0.220125 0.819639 0.409112 11.00000 -1.20000
AFIX 0
C98 1 0.025213 0.884368 0.325962 11.00000 0.01997 0.02767 =
0.03031 0.00453 0.00999 -0.00085
AFIX 137
H98A 2 0.082462 0.904757 0.380990 11.00000 -1.50000
H98B 2 0.008664 0.930221 0.284779 11.00000 -1.50000
H98C 2 0.074841 0.838697 0.306776 11.00000 -1.50000
AFIX 0
O98 4 -0.042214 0.849261 0.478384 11.00000 0.02583 0.03607 =
0.01626 0.00401 0.00111 0.00689
N99 3 -0.108464 0.853924 0.333865 11.00000 0.01647 0.02361 =
0.01594 0.00215 0.00382 -0.00074
C99 1 -0.219665 0.839143 0.256201 11.00000 0.02520 0.04047 =
0.01687 -0.00125 0.00151 -0.00586
AFIX 137
H99A 2 -0.193276 0.792258 0.225408 11.00000 -1.50000
H99B 2 -0.233445 0.889604 0.220932 11.00000 -1.50000
H99C 2 -0.307232 0.825602 0.269909 11.00000 -1.50000
AFIX 0
O99 4 1.234122 1.011077 0.929356 11.00000 0.01655 0.01737 =
0.02780 -0.00182 0.00723 -0.00084
H06 2 1.307836 1.035618 0.923747 11.00000 0.03276
H07 2 1.176474 1.053774 0.923710 11.00000 0.03854
HKLF 4
REM elg_ns1 in P2(1)/n
REM wR2 = 0.1138, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0377 for 11108 Fo > 4sig(Fo) and 0.0485 for all 13416 data
REM 358 parameters refined using 0 restraints
END
WGHT 0.0626 0.4083
REM Highest difference peak 0.668, deepest hole -0.217, 1-sigma level 0.055
Q1 1 0.7672 0.5774 0.6202 11.00000 0.05 0.67
Q2 1 0.5989 0.6879 0.5957 11.00000 0.05 0.60
Q3 1 0.3977 0.7789 0.5508 11.00000 0.05 0.58
Q4 1 0.8809 0.5828 0.6118 11.00000 0.05 0.58
Q5 1 1.0615 0.8330 0.7932 11.00000 0.05 0.56
Q6 1 0.8836 0.7264 0.7217 11.00000 0.05 0.56
Q7 1 0.9345 0.7710 0.6802 11.00000 0.05 0.55
Q8 1 1.0209 0.8296 0.7159 11.00000 0.05 0.55
Q9 1 1.0094 0.7874 0.8376 11.00000 0.05 0.54
Q10 1 0.9178 0.7369 0.7996 11.00000 0.05 0.54
;
_shelx_res_checksum 84480
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.41040(5) 0.66845(3) 0.58286(3) 0.01573(8) Uani d 1 . .
C C2 0.35681(6) 0.74408(3) 0.55675(4) 0.01397(8) Uani d 1 . .
N N2 0.21622(5) 0.75300(4) 0.54244(4) 0.01919(9) Uani d 1 . .
H H01 0.1683(13) 0.7091(8) 0.5522(8) 0.029(3) Uiso d 1 . .
H H02 0.1692(13) 0.7983(8) 0.5197(8) 0.032(3) Uiso d 1 . .
C C3 0.44457(6) 0.81052(3) 0.54550(3) 0.01332(8) Uani d 1 . .
C C4 0.59114(6) 0.79689(3) 0.55989(3) 0.01270(8) Uani d 1 . .
N N4 0.67486(5) 0.85813(3) 0.54512(4) 0.01630(9) Uani d 1 . .
H H03 0.7612(13) 0.8503(8) 0.5540(8) 0.030(3) Uiso d 1 . .
H H04 0.6425(14) 0.9076(8) 0.5296(8) 0.032(3) Uiso d 1 . .
C C4A 0.64624(5) 0.71688(3) 0.58823(3) 0.01254(8) Uani d 1 . .
C C5 0.80070(5) 0.69551(3) 0.60532(3) 0.01224(8) Uani d 1 . .
H H5 0.832899 0.714157 0.555889 0.015 Uiso calc 1 . .
C C5A 0.81825(6) 0.60167(3) 0.61409(3) 0.01306(8) Uani d 1 . .
C C6 0.94969(6) 0.56393(3) 0.60992(4) 0.01383(8) Uani d 1 . .
O O1 1.03852(5) 0.60592(3) 0.58804(3) 0.01802(8) Uani d 1 . .
C C7 0.97538(6) 0.47181(4) 0.63057(4) 0.01648(9) Uani d 1 . .
H H7A 1.075931 0.463992 0.661303 0.020 Uiso calc 1 . .
H H7B 0.956598 0.440073 0.576928 0.020 Uiso calc 1 . .
C C8 0.88588(6) 0.43440(4) 0.68387(4) 0.01705(9) Uani d 1 . .
C C9 0.73204(6) 0.45817(4) 0.64135(4) 0.01770(10) Uani d 1 . .
H H9A 0.698047 0.427626 0.587129 0.021 Uiso calc 1 . .
H H9B 0.673250 0.441184 0.678188 0.021 Uiso calc 1 . .
C C9A 0.71700(6) 0.55019(3) 0.62522(4) 0.01452(9) Uani d 1 . .
O O10 0.58553(5) 0.57747(3) 0.62246(3) 0.01756(8) Uani d 1 . .
C C10A 0.54867(6) 0.65861(3) 0.59701(4) 0.01403(9) Uani d 1 . .
C C11 0.38620(6) 0.89004(4) 0.51709(4) 0.01655(9) Uani d 1 . .
N N3 0.34038(7) 0.95535(4) 0.49419(5) 0.02514(12) Uani d 1 . .
C C12 0.93212(8) 0.46813(5) 0.77471(4) 0.02391(12) Uani d 1 . .
H H12A 1.026948 0.447741 0.803183 0.036 Uiso calc 1 . .
H H12B 0.866481 0.448682 0.805418 0.036 Uiso calc 1 . .
H H12C 0.932458 0.529524 0.773538 0.036 Uiso calc 1 . .
C C13 0.90238(8) 0.33896(4) 0.68645(6) 0.02501(13) Uani d 1 . .
H H13A 0.867471 0.316360 0.629044 0.038 Uiso calc 1 . .
H H13B 0.848265 0.314956 0.722263 0.038 Uiso calc 1 . .
H H13C 1.001952 0.324471 0.709689 0.038 Uiso calc 1 . .
C C21 0.89109(5) 0.73909(3) 0.68486(3) 0.01264(8) Uani d 1 . .
C C22 0.98270(6) 0.80413(3) 0.67880(3) 0.01367(8) Uani d 1 . .
H H22 0.991495 0.819834 0.624914 0.016 Uiso calc 1 . .
C C23 1.06120(6) 0.84614(4) 0.75094(4) 0.01489(9) Uani d 1 . .
O O2 1.15118(5) 0.91117(3) 0.75031(3) 0.01993(9) Uani d 1 . .
C C24 1.05186(6) 0.82200(4) 0.83128(4) 0.01673(9) Uani d 1 . .
O O3 1.12872(6) 0.85824(4) 0.90394(3) 0.02564(11) Uani d 1 . .
H H05 1.1648(14) 0.9072(8) 0.8971(8) 0.034(3) Uiso d 1 . .
C C25 0.96244(7) 0.75654(4) 0.83672(4) 0.01757(10) Uani d 1 . .
H H25 0.955884 0.739310 0.890663 0.021 Uiso calc 1 . .
C C26 0.88214(6) 0.71565(4) 0.76446(4) 0.01552(9) Uani d 1 . .
H H26 0.820851 0.671449 0.769635 0.019 Uiso calc 1 . .
C C27 1.16872(8) 0.93355(4) 0.67030(4) 0.02151(11) Uani d 1 . .
H H27A 1.077008 0.947598 0.631269 0.032 Uiso calc 1 . .
H H27B 1.209836 0.886314 0.647569 0.032 Uiso calc 1 . .
H H27C 1.231375 0.982140 0.676969 0.032 Uiso calc 1 . .
C C97 -0.12972(7) 0.83937(4) 0.40895(4) 0.02086(11) Uani d 1 . .
H H97 -0.220125 0.819639 0.409112 0.025 Uiso calc 1 . .
C C98 0.02521(8) 0.88437(5) 0.32596(5) 0.02539(13) Uani d 1 . .
H H98A 0.082462 0.904757 0.380990 0.038 Uiso calc 1 . .
H H98B 0.008664 0.930221 0.284779 0.038 Uiso calc 1 . .
H H98C 0.074841 0.838697 0.306776 0.038 Uiso calc 1 . .
O O98 -0.04221(6) 0.84926(4) 0.47838(3) 0.02704(11) Uani d 1 . .
N N99 -0.10846(6) 0.85392(4) 0.33387(3) 0.01883(9) Uani d 1 . .
C C99 -0.21966(8) 0.83914(6) 0.25620(5) 0.02841(14) Uani d 1 . .
H H99A -0.193276 0.792258 0.225408 0.043 Uiso calc 1 . .
H H99B -0.233445 0.889604 0.220932 0.043 Uiso calc 1 . .
H H99C -0.307232 0.825602 0.269909 0.043 Uiso calc 1 . .
O O99 1.23412(5) 1.01108(3) 0.92936(3) 0.02037(9) Uani d 1 . .
H H06 1.3078(14) 1.0356(8) 0.9237(8) 0.033(3) Uiso d 1 . .
H H07 1.1765(15) 1.0538(9) 0.9237(9) 0.039(3) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.01093(17) 0.01421(18) 0.0225(2) 0.00127(14) 0.00540(16) 0.00266(15)
C2 0.01156(19) 0.0146(2) 0.0158(2) 0.00106(15) 0.00391(16) 0.00067(16)
N2 0.01142(19) 0.0177(2) 0.0285(3) 0.00216(16) 0.00582(17) 0.00442(18)
C3 0.01208(19) 0.01273(19) 0.0148(2) 0.00120(15) 0.00318(15) 0.00130(15)
C4 0.01184(19) 0.01280(19) 0.01307(19) 0.00009(15) 0.00285(15) 0.00058(15)
N4 0.01292(18) 0.01354(18) 0.0221(2) -0.00014(15) 0.00446(16) 0.00403(16)
C4A 0.01060(18) 0.01223(18) 0.01442(19) 0.00021(14) 0.00292(15) 0.00092(15)
C5 0.01039(18) 0.01210(18) 0.01403(19) -0.00016(14) 0.00309(15) 0.00053(15)
C5A 0.01084(18) 0.01237(18) 0.0157(2) 0.00037(15) 0.00333(15) 0.00069(15)
C6 0.01133(19) 0.0143(2) 0.0155(2) 0.00046(15) 0.00311(16) 0.00048(16)
O1 0.01310(17) 0.01693(18) 0.0254(2) -0.00010(14) 0.00763(15) 0.00243(15)
C7 0.0139(2) 0.0144(2) 0.0213(2) 0.00266(16) 0.00530(18) 0.00277(17)
C8 0.0144(2) 0.0142(2) 0.0224(2) 0.00181(17) 0.00503(18) 0.00436(18)
C9 0.0133(2) 0.0129(2) 0.0266(3) 0.00028(16) 0.00501(19) 0.00304(18)
C9A 0.01132(19) 0.01308(19) 0.0190(2) 0.00082(15) 0.00398(16) 0.00187(16)
O10 0.01171(16) 0.01288(16) 0.0291(2) 0.00140(13) 0.00737(15) 0.00510(15)
C10A 0.01180(19) 0.01265(19) 0.0178(2) 0.00074(15) 0.00446(16) 0.00174(16)
C11 0.0130(2) 0.0159(2) 0.0198(2) 0.00068(16) 0.00297(17) 0.00216(17)
N3 0.0186(2) 0.0177(2) 0.0366(3) 0.00268(18) 0.0038(2) 0.0075(2)
C12 0.0241(3) 0.0267(3) 0.0200(3) 0.0026(2) 0.0046(2) 0.0068(2)
C13 0.0210(3) 0.0150(2) 0.0396(4) 0.0037(2) 0.0094(3) 0.0076(2)
C21 0.01090(18) 0.01291(19) 0.01364(19) -0.00027(15) 0.00269(15) 0.00041(15)
C22 0.01250(19) 0.0141(2) 0.01379(19) -0.00121(15) 0.00278(15) 0.00045(15)
C23 0.0142(2) 0.0144(2) 0.0151(2) -0.00214(16) 0.00256(16) 0.00023(16)
O2 0.0216(2) 0.01943(19) 0.01761(18) -0.00873(16) 0.00363(15) -0.00127(15)
C24 0.0180(2) 0.0169(2) 0.0136(2) -0.00189(18) 0.00167(17) -0.00018(17)
O3 0.0343(3) 0.0243(2) 0.01417(18) -0.0115(2) 0.00005(18) -0.00124(16)
C25 0.0201(2) 0.0185(2) 0.0137(2) -0.00243(19) 0.00417(18) 0.00106(17)
C26 0.0154(2) 0.0158(2) 0.0153(2) -0.00179(17) 0.00414(17) 0.00110(16)
C27 0.0242(3) 0.0197(2) 0.0215(3) -0.0072(2) 0.0078(2) -0.0002(2)
C97 0.0195(2) 0.0257(3) 0.0172(2) 0.0028(2) 0.0049(2) 0.0038(2)
C98 0.0200(3) 0.0277(3) 0.0303(3) -0.0008(2) 0.0100(2) 0.0045(2)
O98 0.0258(2) 0.0361(3) 0.0163(2) 0.0069(2) 0.00111(17) 0.00401(18)
N99 0.0165(2) 0.0236(2) 0.0159(2) -0.00074(17) 0.00382(16) 0.00215(17)
C99 0.0252(3) 0.0405(4) 0.0169(3) -0.0059(3) 0.0015(2) -0.0013(2)
O99 0.01655(19) 0.01737(19) 0.0278(2) -0.00084(15) 0.00723(17) -0.00182(16)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C10A N1 C2 . . 117.21(5) y
N1 C2 N2 . . 116.49(5) ?
N1 C2 C3 . . 120.95(5) ?
N2 C2 C3 . . 122.56(5) ?
C2 N2 H01 . . 117.6(8) ?
C2 N2 H02 . . 123.6(8) ?
H01 N2 H02 . . 118.6(11) ?
C2 C3 C11 . . 120.33(5) ?
C2 C3 C4 . . 119.98(5) ?
C11 C3 C4 . . 119.65(5) ?
N4 C4 C4A . . 120.95(5) ?
N4 C4 C3 . . 120.71(5) ?
C4A C4 C3 . . 118.32(5) ?
C4 N4 H03 . . 120.8(9) ?
C4 N4 H04 . . 121.4(9) ?
H03 N4 H04 . . 117.7(12) ?
C10A C4A C4 . . 115.27(5) ?
C10A C4A C5 . . 122.02(5) ?
C4 C4A C5 . . 122.69(5) ?
C5A C5 C4A . . 108.92(4) ?
C5A C5 C21 . . 110.17(4) ?
C4A C5 C21 . . 111.95(4) ?
C5A C5 H5 . . 108.6 ?
C4A C5 H5 . . 108.6 ?
C21 C5 H5 . . 108.6 ?
C9A C5A C6 . . 117.67(5) ?
C9A C5A C5 . . 123.19(5) ?
C6 C5A C5 . . 119.14(5) ?
O1 C6 C5A . . 120.61(5) ?
O1 C6 C7 . . 120.18(5) ?
C5A C6 C7 . . 119.19(5) ?
C6 C7 C8 . . 114.77(5) ?
C6 C7 H7A . . 108.6 ?
C8 C7 H7A . . 108.6 ?
C6 C7 H7B . . 108.6 ?
C8 C7 H7B . . 108.6 ?
H7A C7 H7B . . 107.6 ?
C13 C8 C7 . . 109.19(5) ?
C13 C8 C12 . . 108.77(6) ?
C7 C8 C12 . . 111.11(5) ?
C13 C8 C9 . . 110.06(5) ?
C7 C8 C9 . . 107.58(5) ?
C12 C8 C9 . . 110.12(5) ?
C9A C9 C8 . . 111.17(5) ?
C9A C9 H9A . . 109.4 ?
C8 C9 H9A . . 109.4 ?
C9A C9 H9B . . 109.4 ?
C8 C9 H9B . . 109.4 ?
H9A C9 H9B . . 108.0 ?
C5A C9A O10 . . 122.79(5) ?
C5A C9A C9 . . 125.66(5) ?
O10 C9A C9 . . 111.55(5) ?
C9A O10 C10A . . 118.66(5) ?
N1 C10A C4A . . 128.24(5) ?
N1 C10A O10 . . 109.59(5) ?
C4A C10A O10 . . 122.17(5) y
N3 C11 C3 . . 179.08(6) ?
C8 C12 H12A . . 109.5 ?
C8 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C8 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C8 C13 H13A . . 109.5 ?
C8 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C8 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C26 C21 C22 . . 118.77(5) ?
C26 C21 C5 . . 120.55(5) ?
C22 C21 C5 . . 120.68(5) ?
C23 C22 C21 . . 120.81(5) ?
C23 C22 H22 . . 119.6 ?
C21 C22 H22 . . 119.6 ?
O2 C23 C22 . . 124.42(5) ?
O2 C23 C24 . . 115.46(5) ?
C22 C23 C24 . . 120.12(5) ?
C23 O2 C27 . . 116.52(5) ?
O3 C24 C25 . . 118.31(5) ?
O3 C24 C23 . . 123.06(6) ?
C25 C24 C23 . . 118.61(5) ?
C24 O3 H05 . . 114.5(9) ?
C24 C25 C26 . . 121.20(5) ?
C24 C25 H25 . . 119.4 ?
C26 C25 H25 . . 119.4 ?
C21 C26 C25 . . 120.48(5) ?
C21 C26 H26 . . 119.8 ?
C25 C26 H26 . . 119.8 ?
O2 C27 H27A . . 109.5 ?
O2 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
O2 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
O98 C97 N99 . . 125.77(7) ?
O98 C97 H97 . . 117.1 ?
N99 C97 H97 . . 117.1 ?
N99 C98 H98A . . 109.5 ?
N99 C98 H98B . . 109.5 ?
H98A C98 H98B . . 109.5 ?
N99 C98 H98C . . 109.5 ?
H98A C98 H98C . . 109.5 ?
H98B C98 H98C . . 109.5 ?
C97 N99 C98 . . 121.91(6) ?
C97 N99 C99 . . 120.70(6) ?
C98 N99 C99 . . 117.39(6) ?
N99 C99 H99A . . 109.5 ?
N99 C99 H99B . . 109.5 ?
H99A C99 H99B . . 109.5 ?
N99 C99 H99C . . 109.5 ?
H99A C99 H99C . . 109.5 ?
H99B C99 H99C . . 109.5 ?
H06 O99 H07 . . 100.5(12) ?
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 C10A . 1.3324(7) y
N1 C2 . 1.3399(7) y
C2 N2 . 1.3529(8) ?
C2 C3 . 1.4160(8) ?
N2 H01 . 0.886(13) ?
N2 H02 . 0.885(13) ?
C3 C11 . 1.4183(8) ?
C3 C4 . 1.4204(8) ?
C4 N4 . 1.3476(7) ?
C4 C4A . 1.4154(7) ?
N4 H03 . 0.836(13) ?
N4 H04 . 0.863(13) ?
C4A C10A . 1.3779(8) ?
C4A C5 . 1.5146(7) ?
C5 C5A . 1.5101(7) ?
C5 C21 . 1.5308(8) ?
C5 H5 . 1.0000 ?
C5A C9A . 1.3484(8) y
C5A C6 . 1.4535(8) ?
C6 O1 . 1.2377(7) ?
C6 C7 . 1.5145(8) ?
C7 C8 . 1.5337(9) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C13 . 1.5313(9) ?
C8 C12 . 1.5345(10) ?
C8 C9 . 1.5349(8) ?
C9 C9A . 1.4925(8) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9A O10 . 1.3617(7) y
O10 C10A . 1.3783(7) y
C11 N3 . 1.1570(8) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C21 C26 . 1.3907(8) ?
C21 C22 . 1.4007(8) ?
C22 C23 . 1.3954(8) ?
C22 H22 . 0.9500 ?
C23 O2 . 1.3700(7) ?
C23 C24 . 1.4068(8) ?
O2 C27 . 1.4230(8) ?
C24 O3 . 1.3545(8) ?
C24 C25 . 1.3888(9) ?
O3 H05 . 0.879(14) ?
C25 C26 . 1.3941(8) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
C97 O98 . 1.2359(8) ?
C97 N99 . 1.3326(9) ?
C97 H97 . 0.9500 ?
C98 N99 . 1.4503(9) ?
C98 H98A . 0.9800 ?
C98 H98B . 0.9800 ?
C98 H98C . 0.9800 ?
N99 C99 . 1.4538(9) ?
C99 H99A . 0.9800 ?
C99 H99B . 0.9800 ?
C99 H99C . 0.9800 ?
O99 H06 . 0.856(14) ?
O99 H07 . 0.877(14) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H01 O1 1_455 0.886(13) 2.268(13) 3.1492(7) 173.6(11) yes
N2 H02 O98 . 0.885(13) 2.170(13) 2.9167(8) 141.8(11) yes
N4 H03 O98 1_655 0.836(13) 2.590(12) 3.2891(8) 142.0(11) yes
N4 H04 N3 3_676 0.863(13) 2.237(13) 3.0413(8) 154.9(12) yes
O3 H05 O99 . 0.879(14) 1.816(14) 2.6399(7) 155.2(12) yes
O99 H06 O1 2_756 0.856(14) 1.944(14) 2.7944(7) 172.0(13) yes
O99 H07 N1 2_656 0.877(14) 2.012(14) 2.8699(7) 165.5(13) yes
O99 H07 O10 2_656 0.877(14) 2.519(14) 3.2180(7) 137.2(11) yes
C22 H22 O98 1_655 0.95 2.39 3.3210(8) 166.7 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C10A N1 C2 N2 . . . . 179.82(6) ?
C10A N1 C2 C3 . . . . -0.47(9) ?
N1 C2 C3 C11 . . . . 179.43(6) ?
N2 C2 C3 C11 . . . . -0.88(9) ?
N1 C2 C3 C4 . . . . 1.58(8) ?
N2 C2 C3 C4 . . . . -178.73(6) ?
C2 C3 C4 N4 . . . . 176.42(5) ?
C11 C3 C4 N4 . . . . -1.44(8) ?
C2 C3 C4 C4A . . . . -2.14(8) ?
C11 C3 C4 C4A . . . . 180.00(5) ?
N4 C4 C4A C10A . . . . -176.96(5) ?
C3 C4 C4A C10A . . . . 1.60(8) ?
N4 C4 C4A C5 . . . . 1.29(8) ?
C3 C4 C4A C5 . . . . 179.84(5) ?
C10A C4A C5 C5A . . . . 11.45(7) y
C4 C4A C5 C5A . . . . -166.67(5) ?
C10A C4A C5 C21 . . . . -110.63(6) ?
C4 C4A C5 C21 . . . . 71.24(6) ?
C4A C5 C5A C9A . . . . -14.61(7) y
C21 C5 C5A C9A . . . . 108.55(6) ?
C4A C5 C5A C6 . . . . 164.97(5) ?
C21 C5 C5A C6 . . . . -71.88(6) ?
C9A C5A C6 O1 . . . . 169.75(6) ?
C5 C5A C6 O1 . . . . -9.86(8) ?
C9A C5A C6 C7 . . . . -8.71(8) y
C5 C5A C6 C7 . . . . 171.68(5) ?
O1 C6 C7 C8 . . . . 160.51(6) ?
C5A C6 C7 C8 . . . . -21.02(8) y
C6 C7 C8 C13 . . . . 169.85(5) ?
C6 C7 C8 C12 . . . . -70.19(7) ?
C6 C7 C8 C9 . . . . 50.42(7) y
C13 C8 C9 C9A . . . . -170.71(6) ?
C7 C8 C9 C9A . . . . -51.84(7) y
C12 C8 C9 C9A . . . . 69.39(7) ?
C6 C5A C9A O10 . . . . -173.91(5) ?
C5 C5A C9A O10 . . . . 5.67(9) y
C6 C5A C9A C9 . . . . 5.77(9) y
C5 C5A C9A C9 . . . . -174.65(6) ?
C8 C9 C9A C5A . . . . 26.39(9) y
C8 C9 C9A O10 . . . . -153.90(5) ?
C5A C9A O10 C10A . . . . 8.25(9) y
C9 C9A O10 C10A . . . . -171.47(5) ?
C2 N1 C10A C4A . . . . -0.02(9) ?
C2 N1 C10A O10 . . . . -179.40(5) ?
C4 C4A C10A N1 . . . . -0.56(9) ?
C5 C4A C10A N1 . . . . -178.82(6) ?
C4 C4A C10A O10 . . . . 178.74(5) ?
C5 C4A C10A O10 . . . . 0.48(9) y
C9A O10 C10A N1 . . . . 168.16(5) ?
C9A O10 C10A C4A . . . . -11.26(9) y
C5A C5 C21 C26 . . . . -52.13(7) ?
C4A C5 C21 C26 . . . . 69.23(6) ?
C5A C5 C21 C22 . . . . 128.86(5) ?
C4A C5 C21 C22 . . . . -109.79(6) ?
C26 C21 C22 C23 . . . . -1.52(8) ?
C5 C21 C22 C23 . . . . 177.51(5) ?
C21 C22 C23 O2 . . . . -178.88(5) ?
C21 C22 C23 C24 . . . . 1.67(9) ?
C22 C23 O2 C27 . . . . -3.02(9) ?
C24 C23 O2 C27 . . . . 176.45(6) ?
O2 C23 C24 O3 . . . . -1.81(9) ?
C22 C23 C24 O3 . . . . 177.69(6) ?
O2 C23 C24 C25 . . . . 179.90(6) ?
C22 C23 C24 C25 . . . . -0.60(9) ?
O3 C24 C25 C26 . . . . -178.96(6) ?
C23 C24 C25 C26 . . . . -0.59(9) ?
C22 C21 C26 C25 . . . . 0.33(9) ?
C5 C21 C26 C25 . . . . -178.70(5) ?
C24 C25 C26 C21 . . . . 0.73(9) ?
O98 C97 N99 C98 . . . . -0.18(11) ?
O98 C97 N99 C99 . . . . 179.44(7) ?