#------------------------------------------------------------------------------
#$Date: 2019-02-20 05:43:45 +0200 (Wed, 20 Feb 2019) $
#$Revision: 213724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/06/1550628.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_1550628
loop_
_publ_author_name
'El-Hiti, Gamal A.'
'Abdel-Wahab, Bakr F.'
'Alqahtani, Alaa'
'Hegazy, Amany S.'
'Kariuki, Benson M.'
_publ_section_title
;
3-[5-Methyl-1-(4-methylphenyl)-1H-1,2,3-triazol-4-yl]-1-phenyl-1H-pyrazole-4-carbaldehyde
;
_journal_coeditor_code HB4285
_journal_issue 2
_journal_name_full IUCrData
_journal_page_first x190217
_journal_paper_doi 10.1107/S2414314619002177
_journal_volume 4
_journal_year 2019
_chemical_formula_iupac 'C20 H17 N5 O'
_chemical_formula_moiety 'C20 H17 N5 O'
_chemical_formula_sum 'C20 H17 N5 O'
_chemical_formula_weight 343.39
_chemical_name_systematic
3-[5-Methyl-1-(4-methylphenyl)-1H-1,2,3-triazol-4-yl]-1-phenyl-1H-pyrazole-4-carbaldehyde
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 93.490(4)
_cell_angle_beta 95.702(5)
_cell_angle_gamma 107.729(6)
_cell_formula_units_Z 4
_cell_length_a 9.7894(7)
_cell_length_b 10.9830(6)
_cell_length_c 17.2596(8)
_cell_measurement_reflns_used 3321
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 25.9760
_cell_measurement_theta_min 3.9410
_cell_volume 1750.67(19)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows and WinGX (Farrugia, 2012)
;
_computing_publication_material
;
CHEMDRAW Ultra (Cambridge Soft, 2001)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0326
_diffrn_reflns_av_unetI/netI 0.0655
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 16161
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.997
_diffrn_reflns_theta_min 1.191
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.085
_exptl_absorpt_correction_T_max 0.993
_exptl_absorpt_correction_T_min 0.988
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.303
_exptl_crystal_description block
_exptl_crystal_F_000 720
_exptl_crystal_size_max 0.505
_exptl_crystal_size_mid 0.288
_exptl_crystal_size_min 0.208
_refine_diff_density_max 0.209
_refine_diff_density_min -0.181
_refine_ls_extinction_coef 0.0073(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 474
_refine_ls_number_reflns 8348
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.018
_refine_ls_R_factor_all 0.1244
_refine_ls_R_factor_gt 0.0647
_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^)+(0.0654P)^2^+0.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1441
_refine_ls_wR_factor_ref 0.1862
_reflns_number_gt 4289
_reflns_number_total 8348
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb4285sup1.cif
_cod_data_source_block I
_cod_database_code 1550628
_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 0.958
_shelx_estimated_absorpt_t_max 0.983
_shelx_hkl_file
;
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11 -4 -1 330.631 107.516 5
11 -4 0 29.1286 59.3888 5
11 -4 1 26.4145 27.4151 5
11 -4 2-65.4130 52.3409 5
11 -4 3 7.78771 33.8728 5
11 -4 4 39.4892 51.3703 5
11 -4 5 179.480 100.946 5
11 -4 6 107.134 78.0635 5
11 -4 7-28.5022 42.0488 5
11 -4 8 46.9971 88.8247 5
11 -3 -11-9.68721 35.5593 5
11 -3 -10 67.2844 50.7405 5
11 -3 -9 119.716 69.1920 5
11 -3 -8 301.038 94.1411 5
11 -3 -7 173.076 73.5964 5
11 -3 -6 16.4890 37.9719 5
11 -3 -5 978.463 176.998 5
11 -3 -4 34.7714 24.7670 5
11 -3 -3-163.081 75.9427 5
11 -3 -2 91.5151 47.7859 5
11 -3 -1-60.7579 49.8088 5
11 -3 0 167.546 93.9541 5
11 -3 1-19.3342 33.5052 5
11 -3 2 206.107 91.9967 5
11 -3 3 17.9444 45.3612 5
11 -3 4 197.496 89.2171 5
11 -3 5-130.357 76.9755 5
11 -3 6 70.2112 66.5202 5
11 -3 7-59.9411 60.5546 5
11 -2 -11 106.371 58.1016 5
11 -2 -10-86.8934 64.0006 5
11 -2 -9 276.579 95.7186 5
11 -2 -8 475.869 125.255 5
11 -2 -7 22.6116 30.4730 5
11 -2 -6 355.865 107.823 5
11 -2 -5 719.714 155.647 5
11 -2 -4 302.788 103.753 5
11 -2 -3 230.940 90.8500 5
11 -2 -2 367.352 110.133 5
11 -2 -1 50.2040 35.6404 5
11 -2 0 122.737 65.1983 5
11 -2 1 352.242 123.692 5
11 -2 2 0.63092 36.1113 5
11 -2 3-167.652 82.7948 5
11 -2 4 3.11625 34.6660 5
11 -2 5 107.749 69.9642 5
11 -2 6 48.2334 49.1349 5
11 -2 7 22.1929 43.9725 5
11 -1 -11 47.3419 54.8136 5
11 -1 -10 217.839 89.8587 5
11 -1 -9 279.375 104.506 5
11 -1 -8 149.308 70.1841 5
11 -1 -7 107.945 55.2713 5
11 -1 -6-21.1801 22.9006 5
11 -1 -5 61.2092 49.8980 5
11 -1 -4 98.3942 42.5542 5
11 -1 -3 51.9158 54.5872 5
11 -1 -2 24.5785 43.6638 5
11 -1 -1 409.737 123.281 5
11 -1 0 67.8549 46.8517 5
11 -1 1 13.4959 30.6762 5
11 -1 2 30.8128 34.1723 5
11 -1 3-25.4760 25.2578 5
11 -1 4 0.35586 41.6542 5
11 -1 5 51.2226 75.0771 5
11 -1 6 2.34254 41.2138 5
11 0 -10 98.0855 48.2891 5
11 0 -9 155.861 80.1077 5
11 0 -8 38.4818 30.9185 5
11 0 -7 75.8497 58.6408 5
11 0 -6 33.2232 45.2345 5
11 0 -5-25.2323 62.5114 5
11 0 -4-58.2110 42.1097 5
11 0 -3 45.3220 79.1057 5
11 0 -2 47.0577 60.2141 5
11 0 -1 4.64163 37.4071 5
11 0 0 366.838 127.629 5
11 0 1-22.0495 50.0448 5
11 0 2 35.3422 46.5293 5
11 0 3 117.673 65.7849 5
11 0 4-48.2192 62.1808 5
11 0 5-21.5051 42.2380 5
11 1 -9 106.405 69.1158 5
11 1 -8 17.3774 36.4212 5
11 1 -7 80.9598 78.5833 5
11 1 -6 221.205 107.159 5
11 1 -5-68.7109 53.9962 5
11 1 -4 52.4825 60.7865 5
11 1 -3 111.163 72.0554 5
11 1 -2 12.0664 22.9094 5
11 1 -1 174.436 96.1267 5
11 1 0 35.5846 44.4612 5
11 1 1 7.10253 57.2243 5
11 1 2-28.1683 42.4965 5
11 1 3 0.36775 57.4435 5
11 1 4-67.0817 62.7077 5
11 2 -8 82.2383 74.8755 5
11 2 -7 28.9862 26.0106 5
11 2 -6 93.9766 80.1822 5
11 2 -5 322.476 120.283 5
11 2 -4 52.4796 80.8474 5
11 2 -3 20.1005 54.5834 5
11 2 -2 19.9738 43.1981 5
11 2 -1-140.158 76.2506 5
11 2 0 28.0478 39.9413 5
11 2 1 25.4064 40.1445 5
11 2 2-60.7675 57.2393 5
11 3 -6 1.02638 40.6457 5
11 3 -5 71.2709 72.4206 5
11 3 -4 71.4714 88.1025 5
11 3 -3 5.19945 51.8205 5
11 3 -2 0.34985 36.2419 5
11 3 -1-105.560 71.0990 5
11 3 0 23.7554 59.2279 5
12 -10 -6 17.3329 40.1231 5
12 -10 -5-11.0342 33.5810 5
12 -10 -4-78.4247 54.8428 5
12 -10 -3 26.2058 36.2551 5
12 -10 -2-7.32540 29.9708 5
12 -10 -1 70.0843 64.4279 5
12 -10 0-127.808 70.2450 5
12 -10 1 19.3118 42.7517 5
12 -10 2 26.2247 24.7293 5
12 -10 3-0.69118 33.1073 5
12 -9 -8 7.50414 41.9139 5
12 -9 -7 20.5580 47.2006 5
12 -9 -6 44.5280 33.0348 5
12 -9 -5-8.96995 22.2603 5
12 -9 -4-34.4684 39.0445 5
12 -9 -3 79.7670 57.6252 5
12 -9 -2 22.7309 33.9829 5
12 -9 -1 0.61865 28.9186 5
12 -9 0 145.162 70.5266 5
12 -9 1 1.98279 59.8388 5
12 -9 2-63.6127 53.6546 5
12 -9 3 16.0291 44.3265 5
12 -9 4 13.7697 28.4729 5
12 -9 5-12.8654 63.6358 5
12 -8 -8-60.1599 68.2572 5
12 -8 -7-21.0809 33.0303 5
12 -8 -6-18.6617 32.5734 5
12 -8 -5 30.3606 47.7776 5
12 -8 -4 244.481 92.9526 5
12 -8 -3 25.6323 32.0114 5
12 -8 -2-60.9002 50.6365 5
12 -8 -1 24.9859 58.0309 5
12 -8 0 5.83014 23.9476 5
12 -8 1-20.1481 35.5139 5
12 -8 2 145.197 98.6463 5
12 -8 3 3.65293 27.9769 5
12 -8 4-33.4114 46.9735 5
12 -8 5 32.5856 51.9597 5
12 -7 -8 26.4432 42.5848 5
12 -7 -7-71.0192 29.4974 5
12 -7 -6 39.8127 28.9320 5
12 -7 -5 51.6610 39.1037 5
12 -7 -4-46.9976 54.3206 5
12 -7 -3 60.2872 40.5549 5
12 -7 -2-32.0943 41.4459 5
12 -7 -1 626.170 151.336 5
12 -7 0 2.96809 25.4358 5
12 -7 1 358.700 124.278 5
12 -7 2 37.6826 30.9504 5
12 -7 3 63.0878 42.7976 5
12 -7 4-75.9239 86.2186 5
12 -7 5 108.108 70.0592 5
12 -6 -8-4.56296 40.7034 5
12 -6 -7 79.5224 36.4185 5
12 -6 -6-39.7318 33.4817 5
12 -6 -5 8.67138 37.4131 5
12 -6 -4 43.0063 44.4166 5
12 -6 -3 11.9627 35.4858 5
12 -6 -2-89.9245 61.8394 5
12 -6 -1 13.2584 25.0836 5
12 -6 0 96.3521 66.9631 5
12 -6 1 182.607 86.3253 5
12 -6 2 144.045 73.6273 5
12 -6 3 283.105 119.579 5
12 -6 4 128.808 94.1321 5
12 -5 -8 45.6369 43.3200 5
12 -5 -7-89.5525 74.2507 5
12 -5 -6 92.8800 55.2755 5
12 -5 -5 0.31127 25.3495 5
12 -5 -4-8.83430 41.9089 5
12 -5 -3-36.9428 41.8279 5
12 -5 -2-39.2940 43.6672 5
12 -5 -1 24.3448 39.4265 5
12 -5 0 32.2935 49.4237 5
12 -5 1-10.2504 30.6515 5
12 -5 2 9.93747 26.7712 5
12 -5 3 158.543 105.683 5
12 -5 4 111.933 75.3075 5
12 -4 -7-50.4359 48.2035 5
12 -4 -6 83.0692 78.1673 5
12 -4 -5 58.9113 54.9214 5
12 -4 -4 292.923 110.406 5
12 -4 -3 203.994 98.9773 5
12 -4 -2 0.64471 41.0784 5
12 -4 -1 78.8313 81.8556 5
12 -4 0 91.1347 62.8969 5
12 -4 1 58.0439 38.5451 5
12 -4 2-0.35640 40.4590 5
12 -4 3 96.8693 64.3628 5
12 -3 -7 98.7846 79.9466 5
12 -3 -6 199.897 89.8540 5
12 -3 -5-71.4352 57.4061 5
12 -3 -4 17.7754 41.9723 5
12 -3 -3 452.243 131.809 5
12 -3 -2-52.7867 57.1946 5
12 -3 -1 21.4671 46.6366 5
12 -3 0-46.9690 35.7339 5
12 -3 1 11.0730 31.2456 5
12 -3 2 0.35877 30.2446 5
12 -2 -6 62.3047 56.2510 5
12 -2 -5 20.6166 47.3254 5
12 -2 -4 92.7334 72.1147 5
12 -2 -3 101.900 81.3621 5
12 -2 -2-0.33260 59.8550 5
12 -2 -1 14.4903 38.1347 5
12 -2 0 190.973 91.8917 5
12 -2 1 0.35060 45.1534 5
12 -1 -3 172.114 99.4300 5
1 0 0 18.6180 6.19220 7
-1 1 0 45227.8 17035.4 7
0 1 0 58552.0 21480.5 7
0 -1 1 17.0265 4.13376 7
1 -1 1 2514.21 1171.19 7
-1 0 1 63352.5 24199.7 7
0 0 1 6406.85 2311.30 7
1 0 1 147.396 456.545 7
-1 1 1294058.1 115624. 7
0 1 1 2143.77 7144.00 7
0 -1 2 18.0444 6.99821 7
0 0 2 1806.96 594.561 7
1 0 2 9574.28 3173.52 7
-1 1 2 91.8251 39.2061 7
0 1 2 43502.8 142.965 7
0 0 3 57103.5 20340.1 7
0 0 0 0.00 0.00 0
TITL bmk1630b in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 9.789435 10.982977 17.259583 93.4901 95.7021 107.7295
ZERR 4.00 0.000739 0.000646 0.000802 0.0043 0.0049 0.0059
LATT 1
SFAC C H N O
UNIT 88.00 48.00 8.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 4149
_shelx_res_file
;
TITL bmk1630b in P-1
shelx.res
created by SHELXL-2018/1 at 16:14:35 on 05-Feb-2019
CELL 0.71073 9.7894 10.9830 17.2596 93.490 95.702 107.729
ZERR 4.00 0.0007 0.0006 0.0008 0.004 0.005 0.006
LATT 1
SFAC C H N O
UNIT 80 68 20 4
MERG 2
MPLA C1 C2 C3 C4 C5 C6 C7
MPLA C8 C9 C10 N1 N2 N3
MPLA C11 C12 C13 C14 N4 N5 O1
MPLA C15 C16 C17 C18 C19 C20
MPLA C21 C22 C23 C24 C25 C26 C27
MPLA C28 C29 C30 N6 N7 N8
MPLA C31 C32 C33 C34 N9 N10 O2
MPLA C35 C36 C37 C38 C39 C40
EQIV $1 -x+1, -y+1, -z+1
HTAB C13 O2_$1
HTAB C16 O2_$1
HTAB C33 O1_$1
HTAB C36 O1_$1
FMAP 2
PLAN 10
SIZE 0.208 0.288 0.505
ACTA
BOND $H
L.S. 4
TEMP 23.00
WGHT 0.065400 0.349100
EXTI 0.007323
FVAR 3.77933
C1 1 0.071223 -0.324874 1.282442 11.00000 0.14430 0.10142 =
0.07356 0.01281 0.03964 0.00786
AFIX 137
H1A 2 0.052641 -0.415552 1.284534 11.00000 -1.50000
H1B 2 -0.016407 -0.304173 1.286566 11.00000 -1.50000
H1C 2 0.142888 -0.279085 1.324964 11.00000 -1.50000
AFIX 0
C2 1 0.125345 -0.286978 1.206086 11.00000 0.09596 0.06054 =
0.06406 0.00262 0.02003 0.00591
C3 1 0.246467 -0.312370 1.184141 11.00000 0.08657 0.07050 =
0.06517 0.01505 0.00035 0.00683
AFIX 43
H3 2 0.292625 -0.356492 1.216383 11.00000 -1.20000
AFIX 0
C4 1 0.301179 -0.274102 1.115596 11.00000 0.06705 0.06429 =
0.06893 0.00977 0.00655 0.01358
AFIX 43
H4 2 0.383419 -0.291762 1.102293 11.00000 -1.20000
AFIX 0
C5 1 0.233322 -0.210085 1.067560 11.00000 0.07203 0.05380 =
0.05629 0.00641 0.01650 0.01731
C6 1 0.108312 -0.188481 1.085901 11.00000 0.09303 0.07846 =
0.07566 0.01735 0.03179 0.03979
AFIX 43
H6 2 0.059060 -0.149184 1.051878 11.00000 -1.20000
AFIX 0
C7 1 0.056669 -0.225758 1.155381 11.00000 0.10074 0.07849 =
0.08455 0.01202 0.04221 0.03243
AFIX 43
H7 2 -0.026400 -0.209094 1.168172 11.00000 -1.20000
AFIX 0
C8 1 0.296566 -0.065714 0.958518 11.00000 0.06716 0.05324 =
0.06218 0.00713 0.01527 0.02293
C9 1 0.357199 -0.083567 0.892401 11.00000 0.05679 0.05091 =
0.06186 0.00685 0.01361 0.02073
C10 1 0.254648 0.045170 0.989589 11.00000 0.14468 0.07036 =
0.08724 0.01682 0.05372 0.05466
AFIX 137
H10A 2 0.263488 0.049410 1.045658 11.00000 -1.50000
H10B 2 0.156385 0.034654 0.969319 11.00000 -1.50000
H10C 2 0.316988 0.123090 0.973863 11.00000 -1.50000
AFIX 0
C11 1 0.391679 -0.002336 0.828560 11.00000 0.05313 0.05160 =
0.06077 0.00682 0.01159 0.01945
C12 1 0.463354 -0.017852 0.763068 11.00000 0.06341 0.05283 =
0.05961 0.00667 0.01759 0.02453
C13 1 0.466545 0.086643 0.723098 11.00000 0.06482 0.05802 =
0.05368 0.00517 0.01731 0.02490
AFIX 43
H13 2 0.506839 0.105062 0.676932 11.00000 -1.20000
AFIX 0
C14 1 0.523398 -0.117552 0.741179 11.00000 0.11100 0.07224 =
0.07753 0.01983 0.04172 0.05115
AFIX 43
H14 2 0.514676 -0.183787 0.773318 11.00000 -1.20000
AFIX 0
C15 1 0.386245 0.279351 0.746147 11.00000 0.05700 0.05261 =
0.06746 0.00935 0.00978 0.02447
C16 1 0.415254 0.326287 0.675881 11.00000 0.07773 0.06731 =
0.07113 0.01551 0.01182 0.03140
AFIX 43
H16 2 0.444824 0.279264 0.638028 11.00000 -1.20000
AFIX 0
C17 1 0.400146 0.444231 0.661787 11.00000 0.08016 0.07346 =
0.09452 0.02796 0.00894 0.02881
AFIX 43
H17 2 0.418989 0.476358 0.613998 11.00000 -1.20000
AFIX 0
C18 1 0.357889 0.513972 0.717247 11.00000 0.08491 0.06270 =
0.12647 0.02141 0.01341 0.03439
AFIX 43
H18 2 0.346166 0.592598 0.707025 11.00000 -1.20000
AFIX 0
C19 1 0.332770 0.467616 0.788148 11.00000 0.12508 0.08352 =
0.12529 0.01888 0.04938 0.06282
AFIX 43
H19 2 0.306254 0.516093 0.826522 11.00000 -1.20000
AFIX 0
C20 1 0.346472 0.349594 0.803125 11.00000 0.10972 0.07319 =
0.08907 0.01987 0.04071 0.05106
AFIX 43
H20 2 0.328967 0.318124 0.851216 11.00000 -1.20000
AFIX 0
C21 1 -0.294053 0.586386 0.986105 11.00000 0.17336 0.08789 =
0.10138 0.02951 0.07796 0.03591
AFIX 137
H21A 2 -0.241402 0.636997 1.033160 11.00000 -1.50000
H21B 2 -0.306369 0.497299 0.991423 11.00000 -1.50000
H21C 2 -0.387077 0.598747 0.977108 11.00000 -1.50000
AFIX 0
C22 1 -0.211437 0.627333 0.918093 11.00000 0.10684 0.05912 =
0.07209 0.01239 0.03520 0.02180
C23 1 -0.075203 0.616227 0.916139 11.00000 0.11122 0.07053 =
0.06432 0.02079 0.01243 0.02508
AFIX 43
H23 2 -0.035778 0.580842 0.956870 11.00000 -1.20000
AFIX 0
C24 1 0.004249 0.656121 0.855474 11.00000 0.07760 0.06933 =
0.07130 0.02069 0.01046 0.02338
AFIX 43
H24 2 0.096526 0.648968 0.855653 11.00000 -1.20000
AFIX 0
C25 1 -0.055058 0.706547 0.794837 11.00000 0.06897 0.05955 =
0.06026 0.01320 0.01414 0.02184
C26 1 -0.191934 0.715967 0.794109 11.00000 0.07668 0.09019 =
0.07524 0.02590 0.02156 0.03745
AFIX 43
H26 2 -0.232868 0.748106 0.752328 11.00000 -1.20000
AFIX 0
C27 1 -0.268225 0.676907 0.856511 11.00000 0.08618 0.08645 =
0.09332 0.02442 0.03963 0.03348
AFIX 43
H27 2 -0.360245 0.684591 0.856511 11.00000 -1.20000
AFIX 0
C28 1 0.048800 0.856600 0.695142 11.00000 0.06131 0.05592 =
0.05800 0.01149 0.01097 0.02276
C29 1 0.134834 0.842289 0.639646 11.00000 0.06170 0.05276 =
0.06166 0.00979 0.01345 0.02323
C30 1 -0.006520 0.963266 0.718388 11.00000 0.09609 0.06457 =
0.07885 0.01524 0.03511 0.03621
AFIX 137
H30A 2 -0.097793 0.952025 0.687926 11.00000 -1.50000
H30B 2 0.061226 1.043504 0.709403 11.00000 -1.50000
H30C 2 -0.018804 0.963322 0.772884 11.00000 -1.50000
AFIX 0
C31 1 0.188821 0.926520 0.579796 11.00000 0.06068 0.05053 =
0.05819 0.00611 0.01196 0.01762
C32 1 0.270995 0.910660 0.519107 11.00000 0.05960 0.05564 =
0.06062 0.00637 0.01435 0.02005
C33 1 0.284000 1.016954 0.478840 11.00000 0.06412 0.05897 =
0.05984 0.00571 0.02067 0.01958
AFIX 43
H33 2 0.331495 1.035272 0.434849 11.00000 -1.20000
AFIX 0
C34 1 0.330420 0.807975 0.500724 11.00000 0.08208 0.06187 =
0.07591 0.01024 0.02791 0.02893
AFIX 43
H34 2 0.321107 0.744151 0.534681 11.00000 -1.20000
AFIX 0
C35 1 0.202539 1.210566 0.495927 11.00000 0.06226 0.05310 =
0.05981 0.00763 0.00991 0.02052
C36 1 0.277818 1.276012 0.440624 11.00000 0.09074 0.06468 =
0.08216 0.02031 0.03309 0.03237
AFIX 43
H36 2 0.337994 1.241736 0.414163 11.00000 -1.20000
AFIX 0
C37 1 0.263581 1.393421 0.424484 11.00000 0.09748 0.07004 =
0.09480 0.02776 0.02853 0.02967
AFIX 43
H37 2 0.312940 1.437398 0.386147 11.00000 -1.20000
AFIX 0
C38 1 0.178151 1.445487 0.464040 11.00000 0.09005 0.06254 =
0.10847 0.01972 0.01225 0.03273
AFIX 43
H38 2 0.169949 1.525055 0.453187 11.00000 -1.20000
AFIX 0
C39 1 0.104090 1.380002 0.520067 11.00000 0.08937 0.08353 =
0.10976 0.02323 0.02551 0.05124
AFIX 43
H39 2 0.046390 1.415715 0.547634 11.00000 -1.20000
AFIX 0
C40 1 0.114979 1.261935 0.535508 11.00000 0.07284 0.07390 =
0.08221 0.02045 0.02262 0.03402
AFIX 43
H40 2 0.063151 1.216867 0.572699 11.00000 -1.20000
AFIX 0
N1 3 0.289148 -0.172159 0.995936 11.00000 0.06959 0.05398 =
0.05912 0.00913 0.01666 0.02562
N2 3 0.344731 -0.251962 0.955373 11.00000 0.08600 0.06801 =
0.07205 0.01905 0.02958 0.04031
N3 3 0.386048 -0.197746 0.892702 11.00000 0.08153 0.06594 =
0.07287 0.01849 0.02865 0.03621
N4 3 0.353690 0.104201 0.827718 11.00000 0.05998 0.05867 =
0.05998 0.01096 0.01720 0.02404
N5 3 0.401591 0.157576 0.762055 11.00000 0.05813 0.05405 =
0.05796 0.00950 0.01377 0.02364
N6 3 0.027819 0.748172 0.732131 11.00000 0.06866 0.06320 =
0.06282 0.01668 0.01886 0.03067
N7 3 0.098778 0.671456 0.701718 11.00000 0.08445 0.07070 =
0.08628 0.02601 0.03217 0.04196
N8 3 0.163844 0.729148 0.645191 11.00000 0.08408 0.06656 =
0.08105 0.02387 0.03215 0.03708
N9 3 0.155107 1.034797 0.576603 11.00000 0.06930 0.05817 =
0.05935 0.01224 0.01905 0.02317
N10 3 0.216208 1.089348 0.514171 11.00000 0.06538 0.05359 =
0.05902 0.01008 0.01913 0.01999
O1 4 0.584277 -0.121115 0.683998 11.00000 0.16049 0.10139 =
0.09946 0.03272 0.07646 0.07995
O2 4 0.391703 0.800383 0.443542 11.00000 0.11424 0.08294 =
0.09471 0.01467 0.05097 0.04928
HKLF 4
REM bmk1630b in P-1
REM R1 = 0.0647 for 4289 Fo > 4sig(Fo) and 0.1244 for all 8348 data
REM 474 parameters refined using 0 restraints
END
WGHT 0.0652 0.3512
REM Highest difference peak 0.209, deepest hole -0.181, 1-sigma level 0.043
Q1 1 0.3837 -0.0378 0.8703 11.00000 0.05 0.21
Q2 1 0.1497 -0.2031 1.1938 11.00000 0.05 0.19
Q3 1 0.3021 0.1065 0.8693 11.00000 0.05 0.19
Q4 1 0.0974 1.0529 0.6256 11.00000 0.05 0.18
Q5 1 0.2599 0.0969 0.9403 11.00000 0.05 0.18
Q6 1 0.5491 0.1586 0.6726 11.00000 0.05 0.17
Q7 1 0.0850 1.2230 0.5951 11.00000 0.05 0.16
Q8 1 0.3605 0.0222 0.8252 11.00000 0.05 0.16
Q9 1 0.4287 -0.0247 0.7998 11.00000 0.05 0.16
Q10 1 0.3207 1.0714 0.4250 11.00000 0.05 0.16
;
_shelx_res_checksum 26762
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
C C1 0.0712(4) -0.3249(3) 1.28244(17) 0.1113(12) Uani d 1
H H1A 0.052641 -0.415552 1.284534 0.167 Uiso calc 1
H H1B -0.016407 -0.304173 1.286566 0.167 Uiso calc 1
H H1C 0.142888 -0.279085 1.324964 0.167 Uiso calc 1
C C2 0.1253(3) -0.2870(2) 1.20609(15) 0.0772(8) Uani d 1
C C3 0.2465(3) -0.3124(2) 1.18414(15) 0.0784(8) Uani d 1
H H3 0.292625 -0.356492 1.216383 0.094 Uiso calc 1
C C4 0.3012(3) -0.2741(2) 1.11560(14) 0.0683(7) Uani d 1
H H4 0.383419 -0.291762 1.102293 0.082 Uiso calc 1
C C5 0.2333(3) -0.2101(2) 1.06756(13) 0.0606(6) Uani d 1
C C6 0.1083(3) -0.1885(2) 1.08590(16) 0.0775(8) Uani d 1
H H6 0.059060 -0.149184 1.051878 0.093 Uiso calc 1
C C7 0.0567(3) -0.2258(3) 1.15538(17) 0.0846(8) Uani d 1
H H7 -0.026400 -0.209094 1.168172 0.101 Uiso calc 1
C C8 0.2966(3) -0.0657(2) 0.95852(13) 0.0593(6) Uani d 1
C C9 0.3572(2) -0.08357(19) 0.89240(13) 0.0551(5) Uani d 1
C C10 0.2546(4) 0.0452(2) 0.98959(17) 0.0928(10) Uani d 1
H H10A 0.263488 0.049410 1.045658 0.139 Uiso calc 1
H H10B 0.156385 0.034654 0.969319 0.139 Uiso calc 1
H H10C 0.316988 0.123090 0.973863 0.139 Uiso calc 1
C C11 0.3917(2) -0.00234(19) 0.82856(13) 0.0541(5) Uani d 1
C C12 0.4634(2) -0.01785(19) 0.76307(13) 0.0564(6) Uani d 1
C C13 0.4665(2) 0.0866(2) 0.72310(13) 0.0569(6) Uani d 1
H H13 0.506839 0.105062 0.676932 0.068 Uiso calc 1
C C14 0.5234(3) -0.1176(2) 0.74118(16) 0.0792(8) Uani d 1
H H14 0.514676 -0.183787 0.773318 0.095 Uiso calc 1
C C15 0.3862(2) 0.2794(2) 0.74615(14) 0.0571(6) Uani d 1
C C16 0.4153(3) 0.3263(2) 0.67588(15) 0.0695(7) Uani d 1
H H16 0.444824 0.279264 0.638028 0.083 Uiso calc 1
C C17 0.4001(3) 0.4442(3) 0.66179(18) 0.0809(8) Uani d 1
H H17 0.418989 0.476358 0.613998 0.097 Uiso calc 1
C C18 0.3579(3) 0.5140(3) 0.7172(2) 0.0882(9) Uani d 1
H H18 0.346166 0.592598 0.707025 0.106 Uiso calc 1
C C19 0.3328(4) 0.4676(3) 0.7881(2) 0.1017(10) Uani d 1
H H19 0.306254 0.516093 0.826522 0.122 Uiso calc 1
C C20 0.3465(3) 0.3496(2) 0.80313(17) 0.0830(8) Uani d 1
H H20 0.328967 0.318124 0.851216 0.100 Uiso calc 1
C C21 -0.2941(4) 0.5864(3) 0.98610(19) 0.1168(13) Uani d 1
H H21A -0.241402 0.636997 1.033160 0.175 Uiso calc 1
H H21B -0.306369 0.497299 0.991423 0.175 Uiso calc 1
H H21C -0.387077 0.598747 0.977108 0.175 Uiso calc 1
C C22 -0.2114(4) 0.6273(2) 0.91809(16) 0.0783(8) Uani d 1
C C23 -0.0752(4) 0.6162(2) 0.91614(16) 0.0821(8) Uani d 1
H H23 -0.035778 0.580842 0.956870 0.098 Uiso calc 1
C C24 0.0042(3) 0.6561(2) 0.85547(15) 0.0720(7) Uani d 1
H H24 0.096526 0.648968 0.855653 0.086 Uiso calc 1
C C25 -0.0551(3) 0.7065(2) 0.79484(14) 0.0618(6) Uani d 1
C C26 -0.1919(3) 0.7160(2) 0.79411(16) 0.0765(7) Uani d 1
H H26 -0.232868 0.748106 0.752328 0.092 Uiso calc 1
C C27 -0.2682(3) 0.6769(3) 0.85651(17) 0.0845(8) Uani d 1
H H27 -0.360245 0.684591 0.856511 0.101 Uiso calc 1
C C28 0.0488(2) 0.8566(2) 0.69514(13) 0.0569(6) Uani d 1
C C29 0.1348(2) 0.8423(2) 0.63965(13) 0.0569(6) Uani d 1
C C30 -0.0065(3) 0.9633(2) 0.71839(16) 0.0752(7) Uani d 1
H H30A -0.097793 0.952025 0.687926 0.113 Uiso calc 1
H H30B 0.061226 1.043504 0.709403 0.113 Uiso calc 1
H H30C -0.018804 0.963322 0.772884 0.113 Uiso calc 1
C C31 0.1888(2) 0.92652(19) 0.57980(13) 0.0561(5) Uani d 1
C C32 0.2710(2) 0.9107(2) 0.51911(13) 0.0576(6) Uani d 1
C C33 0.2840(3) 1.0170(2) 0.47884(13) 0.0600(6) Uani d 1
H H33 0.331495 1.035272 0.434849 0.072 Uiso calc 1
C C34 0.3304(3) 0.8080(2) 0.50072(15) 0.0704(7) Uani d 1
H H34 0.321107 0.744151 0.534681 0.084 Uiso calc 1
C C35 0.2025(3) 1.2106(2) 0.49593(13) 0.0576(6) Uani d 1
C C36 0.2778(3) 1.2760(2) 0.44062(16) 0.0752(7) Uani d 1
H H36 0.337994 1.241736 0.414163 0.090 Uiso calc 1
C C37 0.2636(3) 1.3934(3) 0.42448(18) 0.0846(8) Uani d 1
H H37 0.312940 1.437398 0.386147 0.102 Uiso calc 1
C C38 0.1782(3) 1.4455(3) 0.46404(18) 0.0845(8) Uani d 1
H H38 0.169949 1.525055 0.453187 0.101 Uiso calc 1
C C39 0.1041(3) 1.3800(3) 0.52007(19) 0.0872(8) Uani d 1
H H39 0.046390 1.415715 0.547634 0.105 Uiso calc 1
C C40 0.1150(3) 1.2619(2) 0.53551(16) 0.0723(7) Uani d 1
H H40 0.063151 1.216867 0.572699 0.087 Uiso calc 1
N N1 0.2891(2) -0.17216(16) 0.99594(11) 0.0587(5) Uani d 1
N N2 0.3447(2) -0.25196(18) 0.95537(12) 0.0697(6) Uani d 1
N N3 0.3860(2) -0.19775(18) 0.89270(12) 0.0686(6) Uani d 1
N N4 0.3537(2) 0.10420(16) 0.82772(11) 0.0574(5) Uani d 1
N N5 0.4016(2) 0.15758(16) 0.76206(10) 0.0547(5) Uani d 1
N N6 0.0278(2) 0.74817(17) 0.73213(11) 0.0614(5) Uani d 1
N N7 0.0988(2) 0.67146(19) 0.70172(13) 0.0741(6) Uani d 1
N N8 0.1638(2) 0.72915(18) 0.64519(12) 0.0719(6) Uani d 1
N N9 0.1551(2) 1.03480(17) 0.57660(11) 0.0605(5) Uani d 1
N N10 0.2162(2) 1.08935(16) 0.51417(11) 0.0580(5) Uani d 1
O O1 0.5843(3) -0.12112(19) 0.68400(12) 0.1063(8) Uani d 1
O O2 0.3917(2) 0.80038(17) 0.44354(12) 0.0902(6) Uani 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
C1 0.144(3) 0.101(2) 0.074(2) 0.008(2) 0.040(2) 0.0128(16)
C2 0.096(2) 0.0605(15) 0.0641(16) 0.0059(14) 0.0200(15) 0.0026(12)
C3 0.087(2) 0.0705(16) 0.0652(16) 0.0068(14) 0.0003(15) 0.0151(12)
C4 0.0671(17) 0.0643(14) 0.0689(16) 0.0136(12) 0.0065(13) 0.0098(11)
C5 0.0720(17) 0.0538(12) 0.0563(14) 0.0173(11) 0.0165(12) 0.0064(10)
C6 0.093(2) 0.0785(17) 0.0757(18) 0.0398(15) 0.0318(16) 0.0174(13)
C7 0.101(2) 0.0785(17) 0.085(2) 0.0324(15) 0.0422(17) 0.0120(14)
C8 0.0672(16) 0.0532(12) 0.0622(14) 0.0229(10) 0.0153(12) 0.0071(10)
C9 0.0568(14) 0.0509(12) 0.0619(14) 0.0207(10) 0.0136(11) 0.0068(9)
C10 0.145(3) 0.0704(17) 0.087(2) 0.0547(17) 0.054(2) 0.0168(14)
C11 0.0531(14) 0.0516(12) 0.0608(13) 0.0194(10) 0.0116(11) 0.0068(9)
C12 0.0634(15) 0.0528(12) 0.0596(13) 0.0245(10) 0.0176(11) 0.0067(10)
C13 0.0648(15) 0.0580(13) 0.0537(13) 0.0249(10) 0.0173(11) 0.0052(10)
C14 0.111(2) 0.0722(16) 0.0775(18) 0.0512(15) 0.0417(17) 0.0198(13)
C15 0.0570(14) 0.0526(12) 0.0675(15) 0.0245(10) 0.0098(11) 0.0094(10)
C16 0.0777(18) 0.0673(15) 0.0711(16) 0.0314(12) 0.0118(13) 0.0155(12)
C17 0.080(2) 0.0735(17) 0.095(2) 0.0288(14) 0.0089(16) 0.0280(14)
C18 0.085(2) 0.0627(16) 0.126(3) 0.0344(14) 0.0134(19) 0.0214(16)
C19 0.125(3) 0.084(2) 0.125(3) 0.0628(19) 0.049(2) 0.0189(18)
C20 0.110(2) 0.0732(17) 0.0891(19) 0.0511(15) 0.0407(17) 0.0199(14)
C21 0.173(4) 0.088(2) 0.101(2) 0.036(2) 0.078(3) 0.0295(17)
C22 0.107(2) 0.0591(15) 0.0721(17) 0.0218(14) 0.0352(16) 0.0124(12)
C23 0.111(3) 0.0705(16) 0.0643(16) 0.0251(15) 0.0124(16) 0.0208(12)
C24 0.0776(18) 0.0693(15) 0.0713(16) 0.0234(13) 0.0105(14) 0.0207(12)
C25 0.0690(17) 0.0595(13) 0.0603(14) 0.0218(11) 0.0141(12) 0.0132(10)
C26 0.0767(19) 0.0902(18) 0.0752(17) 0.0375(14) 0.0216(15) 0.0259(14)
C27 0.086(2) 0.0864(18) 0.093(2) 0.0335(15) 0.0396(17) 0.0244(15)
C28 0.0613(15) 0.0559(13) 0.0580(13) 0.0228(10) 0.0110(11) 0.0115(10)
C29 0.0617(15) 0.0528(12) 0.0617(14) 0.0232(10) 0.0134(11) 0.0098(10)
C30 0.096(2) 0.0646(15) 0.0789(17) 0.0362(13) 0.0351(15) 0.0152(12)
C31 0.0607(14) 0.0505(12) 0.0582(13) 0.0176(10) 0.0120(11) 0.0061(9)
C32 0.0596(15) 0.0556(12) 0.0606(14) 0.0200(10) 0.0143(11) 0.0064(10)
C33 0.0641(15) 0.0590(13) 0.0598(14) 0.0196(11) 0.0207(12) 0.0057(10)
C34 0.0821(19) 0.0619(14) 0.0759(17) 0.0289(12) 0.0279(15) 0.0102(12)
C35 0.0623(15) 0.0531(12) 0.0598(14) 0.0205(10) 0.0099(11) 0.0076(10)
C36 0.091(2) 0.0647(15) 0.0822(18) 0.0324(13) 0.0331(15) 0.0203(12)
C37 0.097(2) 0.0700(17) 0.095(2) 0.0297(15) 0.0285(17) 0.0278(14)
C38 0.090(2) 0.0625(16) 0.108(2) 0.0327(14) 0.0123(18) 0.0197(15)
C39 0.089(2) 0.0835(19) 0.110(2) 0.0512(16) 0.0255(18) 0.0232(16)
C40 0.0728(18) 0.0739(16) 0.0822(18) 0.0340(13) 0.0226(14) 0.0204(13)
N1 0.0696(13) 0.0540(10) 0.0591(11) 0.0256(9) 0.0167(10) 0.0091(8)
N2 0.0860(15) 0.0680(12) 0.0720(13) 0.0403(11) 0.0296(12) 0.0191(10)
N3 0.0815(15) 0.0659(12) 0.0729(13) 0.0362(10) 0.0286(11) 0.0185(10)
N4 0.0600(12) 0.0587(11) 0.0600(11) 0.0240(9) 0.0172(9) 0.0110(8)
N5 0.0581(12) 0.0540(10) 0.0580(11) 0.0236(8) 0.0138(9) 0.0095(8)
N6 0.0687(13) 0.0632(11) 0.0628(12) 0.0307(9) 0.0189(10) 0.0167(9)
N7 0.0845(16) 0.0707(13) 0.0863(15) 0.0420(11) 0.0322(13) 0.0260(11)
N8 0.0841(16) 0.0666(12) 0.0811(14) 0.0371(11) 0.0322(12) 0.0239(10)
N9 0.0693(13) 0.0582(11) 0.0593(12) 0.0232(9) 0.0190(10) 0.0122(8)
N10 0.0654(13) 0.0536(10) 0.0590(11) 0.0200(9) 0.0191(10) 0.0101(8)
O1 0.160(2) 0.1014(14) 0.0995(15) 0.0799(14) 0.0765(15) 0.0327(11)
O2 0.1142(16) 0.0829(12) 0.0947(14) 0.0493(11) 0.0510(13) 0.0147(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 C1 H1A 109.5
C2 C1 H1B 109.5
H1A C1 H1B 109.5
C2 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
C7 C2 C3 117.4(2)
C7 C2 C1 121.7(3)
C3 C2 C1 121.0(3)
C2 C3 C4 121.9(3)
C2 C3 H3 119.0
C4 C3 H3 119.0
C5 C4 C3 119.4(3)
C5 C4 H4 120.3
C3 C4 H4 120.3
C4 C5 C6 120.1(2)
C4 C5 N1 119.3(2)
C6 C5 N1 120.5(2)
C5 C6 C7 119.4(3)
C5 C6 H6 120.3
C7 C6 H6 120.3
C2 C7 C6 121.6(3)
C2 C7 H7 119.2
C6 C7 H7 119.2
N1 C8 C9 104.48(18)
N1 C8 C10 124.7(2)
C9 C8 C10 130.7(2)
N3 C9 C8 108.58(19)
N3 C9 C11 121.1(2)
C8 C9 C11 130.3(2)
C8 C10 H10A 109.5
C8 C10 H10B 109.5
H10A C10 H10B 109.5
C8 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
N4 C11 C12 110.92(18)
N4 C11 C9 119.4(2)
C12 C11 C9 129.7(2)
C13 C12 C11 104.52(18)
C13 C12 C14 125.7(2)
C11 C12 C14 129.7(2)
N5 C13 C12 108.00(19)
N5 C13 H13 126.0
C12 C13 H13 126.0
O1 C14 C12 124.5(2)
O1 C14 H14 117.7
C12 C14 H14 117.7
C16 C15 C20 120.8(2)
C16 C15 N5 120.2(2)
C20 C15 N5 119.0(2)
C15 C16 C17 119.3(3)
C15 C16 H16 120.4
C17 C16 H16 120.4
C18 C17 C16 120.6(3)
C18 C17 H17 119.7
C16 C17 H17 119.7
C17 C18 C19 119.6(3)
C17 C18 H18 120.2
C19 C18 H18 120.2
C18 C19 C20 120.6(3)
C18 C19 H19 119.7
C20 C19 H19 119.7
C15 C20 C19 119.1(3)
C15 C20 H20 120.4
C19 C20 H20 120.4
C22 C21 H21A 109.5
C22 C21 H21B 109.5
H21A C21 H21B 109.5
C22 C21 H21C 109.5
H21A C21 H21C 109.5
H21B C21 H21C 109.5
C27 C22 C23 117.8(2)
C27 C22 C21 121.4(3)
C23 C22 C21 120.7(3)
C22 C23 C24 121.9(3)
C22 C23 H23 119.1
C24 C23 H23 119.1
C25 C24 C23 119.0(3)
C25 C24 H24 120.5
C23 C24 H24 120.5
C24 C25 C26 120.6(2)
C24 C25 N6 118.8(2)
C26 C25 N6 120.6(2)
C25 C26 C27 119.1(3)
C25 C26 H26 120.4
C27 C26 H26 120.4
C22 C27 C26 121.6(3)
C22 C27 H27 119.2
C26 C27 H27 119.2
N6 C28 C29 103.65(18)
N6 C28 C30 124.0(2)
C29 C28 C30 132.2(2)
N8 C29 C28 109.49(18)
N8 C29 C31 121.5(2)
C28 C29 C31 129.0(2)
C28 C30 H30A 109.5
C28 C30 H30B 109.5
H30A C30 H30B 109.5
C28 C30 H30C 109.5
H30A C30 H30C 109.5
H30B C30 H30C 109.5
N9 C31 C32 111.11(18)
N9 C31 C29 118.7(2)
C32 C31 C29 130.2(2)
C33 C32 C31 104.39(19)
C33 C32 C34 125.8(2)
C31 C32 C34 129.8(2)
N10 C33 C32 107.81(19)
N10 C33 H33 126.1
C32 C33 H33 126.1
O2 C34 C32 123.9(2)
O2 C34 H34 118.1
C32 C34 H34 118.1
C36 C35 C40 120.2(2)
C36 C35 N10 120.5(2)
C40 C35 N10 119.3(2)
C35 C36 C37 119.3(2)
C35 C36 H36 120.3
C37 C36 H36 120.3
C38 C37 C36 120.7(3)
C38 C37 H37 119.6
C36 C37 H37 119.6
C37 C38 C39 119.7(3)
C37 C38 H38 120.2
C39 C38 H38 120.2
C38 C39 C40 120.2(3)
C38 C39 H39 119.9
C40 C39 H39 119.9
C35 C40 C39 119.8(2)
C35 C40 H40 120.1
C39 C40 H40 120.1
C8 N1 N2 110.73(17)
C8 N1 C5 130.73(19)
N2 N1 C5 118.54(17)
N3 N2 N1 107.00(17)
N2 N3 C9 109.21(18)
C11 N4 N5 104.88(17)
C13 N5 N4 111.67(17)
C13 N5 C15 128.83(18)
N4 N5 C15 119.37(17)
C28 N6 N7 111.17(18)
C28 N6 C25 130.08(19)
N7 N6 C25 118.74(18)
N8 N7 N6 107.05(18)
N7 N8 C29 108.63(19)
C31 N9 N10 104.86(18)
C33 N10 N9 111.82(18)
C33 N10 C35 129.31(19)
N9 N10 C35 118.86(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.504(3)
C1 H1A 0.9600
C1 H1B 0.9600
C1 H1C 0.9600
C2 C7 1.378(4)
C2 C3 1.380(4)
C3 C4 1.383(3)
C3 H3 0.9300
C4 C5 1.367(3)
C4 H4 0.9300
C5 C6 1.378(3)
C5 N1 1.435(3)
C6 C7 1.384(3)
C6 H6 0.9300
C7 H7 0.9300
C8 N1 1.356(3)
C8 C9 1.368(3)
C8 C10 1.486(3)
C9 N3 1.367(3)
C9 C11 1.461(3)
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
C11 N4 1.332(3)
C11 C12 1.416(3)
C12 C13 1.369(3)
C12 C14 1.440(3)
C13 N5 1.336(3)
C13 H13 0.9300
C14 O1 1.207(3)
C14 H14 0.9300
C15 C16 1.368(3)
C15 C20 1.371(3)
C15 N5 1.430(3)
C16 C17 1.381(3)
C16 H16 0.9300
C17 C18 1.363(4)
C17 H17 0.9300
C18 C19 1.370(4)
C18 H18 0.9300
C19 C20 1.380(4)
C19 H19 0.9300
C20 H20 0.9300
C21 C22 1.505(3)
C21 H21A 0.9600
C21 H21B 0.9600
C21 H21C 0.9600
C22 C27 1.368(4)
C22 C23 1.379(4)
C23 C24 1.380(3)
C23 H23 0.9300
C24 C25 1.373(3)
C24 H24 0.9300
C25 C26 1.374(3)
C25 N6 1.431(3)
C26 C27 1.387(3)
C26 H26 0.9300
C27 H27 0.9300
C28 N6 1.356(3)
C28 C29 1.369(3)
C28 C30 1.483(3)
C29 N8 1.363(3)
C29 C31 1.459(3)
C30 H30A 0.9600
C30 H30B 0.9600
C30 H30C 0.9600
C31 N9 1.330(3)
C31 C32 1.416(3)
C32 C33 1.374(3)
C32 C34 1.450(3)
C33 N10 1.337(3)
C33 H33 0.9300
C34 O2 1.216(3)
C34 H34 0.9300
C35 C36 1.368(3)
C35 C40 1.372(3)
C35 N10 1.429(3)
C36 C37 1.380(3)
C36 H36 0.9300
C37 C38 1.360(4)
C37 H37 0.9300
C38 C39 1.373(4)
C38 H38 0.9300
C39 C40 1.373(3)
C39 H39 0.9300
C40 H40 0.9300
N1 N2 1.359(3)
N2 N3 1.306(2)
N4 N5 1.366(2)
N6 N7 1.358(3)
N7 N8 1.308(3)
N9 N10 1.366(2)
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
C13 H13 O2 2_666 0.93 2.54 3.452(3) 168 yes
C16 H16 O2 2_666 0.93 2.54 3.432(3) 161 yes
C33 H33 O1 2_666 0.93 2.42 3.329(3) 165 yes
C36 H36 O1 2_666 0.93 2.41 3.297(3) 160 yes
_cod_database_fobs_code 1550628