#------------------------------------------------------------------------------
#$Date: 2025-02-22 04:53:29 +0200 (Sat, 22 Feb 2025) $
#$Revision: 297834 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312764.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_2312764
loop_
_publ_author_name
'Vlahakis, Niko'
'Qu, Songrong'
'Richards, Logan S.'
'Moraes, Lygia Silva de'
'Cascio, Duilio'
'Nelson, Hosea M.'
'Rodriguez, Jose A.'
_publ_section_title
;
Fast event-based electron counting for small-molecule structure
determination by MicroED.
;
_journal_coeditor_code YP3239
_journal_issue 3
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624012300
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration rm
_chemical_formula_iupac 'C36 H54 N2 O2'
_chemical_formula_moiety 'C36 H54 N2 O2'
_chemical_formula_sum 'C36 H54 N2 O2'
_chemical_formula_weight 546.81
_chemical_name_common '(S,S)-Jacobsen's Ligand'
_chemical_name_systematic
;
(S,S)-(+)-N,N'-Bis(3,5-di-tert-\
butylsalicylidene)-1,2-cyclohexanediaminomanganese(III) chloride
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.160(2)
_cell_length_b 19.4400(19)
_cell_length_c 29.780(3)
_cell_measurement_reflns_used 13767
_cell_measurement_temperature 293
_cell_measurement_theta_max 0.837
_cell_measurement_theta_min 0.044
_cell_volume 4145.1(13)
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type TEM
_diffrn_measurement_method 'continuous rotation 3D ED'
_diffrn_radiation_type electron
_diffrn_radiation_wavelength 0.0251
_diffrn_reflns_av_R_equivalents 0.0994
_diffrn_reflns_av_unetI/netI 0.1254
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 13767
_diffrn_reflns_theta_full 0.837
_diffrn_reflns_theta_max 0.837
_diffrn_reflns_theta_min 0.044
_diffrn_source FEG
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.000
_exptl_absorpt_correction_type none
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 0.876
_exptl_crystal_description rod
_exptl_crystal_F_000 509
_exptl_crystal_size_max 0.010
_exptl_crystal_size_mid 0.0007
_exptl_crystal_size_min 0.00015
_refine_diff_density_max 0.101
_refine_diff_density_min -0.096
_refine_ls_abs_structure_details
;
All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef 1934(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 382
_refine_ls_number_reflns 5692
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.1707
_refine_ls_R_factor_gt 0.1167
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3180
_refine_ls_wR_factor_ref 0.3641
_reflns_number_gt 2894
_reflns_number_total 5692
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yp3239.cif
_cod_data_source_block a_1
_cod_database_code 2312764
_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 -1 0 44.96 25.728 1
0 1 0 37.44 23.709 1
0 -1 1 29.01 23.220 -1
0 1 -1 -1.99 30.294 -1
0 -1 2 -149.20 87.787 1
0 1 -2 236.44 118.245 1
0 -1 3 48180. 5423.72 1
0 1 -3 39736. 4535.89 1
0 -2 0 542372. 59472. 1
0 2 0 627616. 68794. 1
0 2 1 316899. 34796. 1
0 -2 1 319541. 35065. 1
0 -2 -1 318644. 34960. 1
0 2 -1 323280. 35479. 1
0 -2 2 153739. 16934. 1
0 2 -2 159222. 17547. 1
0 -2 3 156780. 17283. 1
0 2 -3 169641. 18679. 1
0 -2 4 384895. 42283. 1
0 2 -4 396460. 43534. 1
0 -2 5 630608. 69242. 1
0 2 -5 664506. 72881. 1
0 -2 7 157128. 17438. 1
0 2 -7 131505. 14641. 1
0 -3 0 1176.97 1289.63 1
0 3 0 -2203.4 1177.47 1
0 3 1 449003. 49287. 1
0 -3 1 417597. 45857. 1
0 -3 -1 450398. 49447. 1
0 3 -1 421286. 46256. 1
0 3 2 114008. 12672. 1
0 -3 -2 115254. 12831. 1
0 3 -2 138833. 15334. 1
0 -3 3 34521. 4019.44 -1
0 3 -3 33589. 3923.23 -1
0 -3 5 319840. 35189. 1
0 3 -5 344217. 37846. 1
0 -3 6 110468. 12308. 1
0 3 -6 117647. 13091. 1
0 -3 8 3934.19 1305.08 1
0 3 -8 8050.84 1628.11 1
0 -3 9 192472. 21341. 1
0 3 -9 210518. 23315. 1
0 -3 10 25454. 3290.62 1
0 3 -10 28549. 3661.51 1
0 -4 0 920238. 100947. 1
0 4 0 999999. 109671. 1
0 4 1 494715. 54337. 1
0 -4 1 491375. 53988. 1
0 -4 -1 542372. 59571. 1
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0 -4 2 57976. 6565.30 1
0 -4 -2 57577. 6600.19 1
0 4 -2 53888. 6116.64 1
0 -4 3 249302. 27492. 1
0 -4 -3 291924. 32188. 1
0 4 -3 277467. 30568. 1
0 -4 4 30573. 3645.06 1
0 4 -4 28699. 3464.10 1
0 -4 5 289332. 31869. 1
0 4 -5 305832. 33669. 1
0 -4 6 82752. 9267.19 1
0 4 -6 64806. 7303.08 1
0 -4 8 14108. 2005.98 1
0 4 -8 14935. 2112.66 1
0 -4 10 315852. 34845. 1
0 4 -10 311465. 34382. 1
0 -4 12 213410. 23694. 1
0 4 -12 192871. 21446. 1
0 -4 13 141775. 15907. 1
0 4 -13 152841. 17099. 1
0 -4 14 9227.31 1947.66 1
0 4 -14 8763.70 2026.92 1
0 4 -15 6784.64 1701.39 1
0 -5 0 -1709.9 1537.39 1
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0 5 1 124476. 13843. 1
0 -5 1 119940. 13355. 1
0 -5 -1 147707. 16396. 1
0 5 2 72782. 8250.24 1
0 -5 2 83799. 9406.77 1
0 -5 -2 75424. 8544.36 1
0 5 3 120339. 13475. 1
0 -5 3 156780. 17378. 1
0 -5 -3 126919. 14177. 1
0 5 -3 107627. 11979. 1
0 -5 5 117348. 13061. 1
0 5 -5 133649. 14855. 1
0 -5 6 138684. 15394. 1
0 5 -6 123828. 13764. 1
0 -5 7 5997.00 1217.35 1
0 5 -7 6899.29 1262.21 1
0 -5 8 104337. 11640. 1
0 5 -8 134746. 14975. 1
0 -5 10 106680. 11929. 1
0 5 -10 101446. 11386. 1
0 -5 13 50150. 5882.35 1
0 5 -13 41067. 4990.02 1
0 -5 15 43355. 5259.22 1
0 5 -15 29292. 3849.95 1
0 -5 16 2926.72 1483.05 1
0 5 -16 4542.37 1788.63 1
0 -5 17 25743. 3344.46 1
0 5 -17 35703. 4480.55 1
0 5 -19 9242.26 1775.17 1
0 -6 0 575274. 63210. 1
0 6 0 699401. 76819. 1
0 6 1 4096.71 1328.01 1
0 -6 1 4302.59 1310.07 1
0 -6 -1 3536.39 1198.90 1
0 6 -1 5907.27 1296.61 1
0 6 2 209721. 23225. 1
0 -6 2 163260. 18106. 1
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0 6 -2 211715. 23405. 1
0 6 3 15828. 2368.89 1
0 -6 3 15977. 2150.05 1
0 -6 -3 16361. 2451.64 1
0 6 -3 13873. 1948.65 1
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0 -6 -4 30573. 3927.71 1
0 -6 6 6291.12 1263.21 1
0 6 -6 6161.51 1293.62 1
0 -6 7 16615. 2198.40 1
0 6 -7 13245. 1857.92 1
0 -6 8 97757. 10957. 1
0 6 -8 106181. 11874. 1
0 -6 9 95812. 10748. 1
0 6 -9 122084. 13599. 1
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0 6 -10 100997. 11341. 1
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0 6 -15 16256. 2492.02 1
0 -6 16 15758. 2277.66 1
0 6 -16 12697. 2149.55 1
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0 -6 19 425.12 1188.43 -1
0 6 -19 3267.69 1557.33 -1
0 -6 20 2470.59 1229.81 1
0 6 -20 874.87 1415.25 1
0 -6 21 1450.15 1165.50 1
0 6 -21 307.63 1429.71 1
0 6 -22 1054.34 1452.64 1
0 6 -23 934.20 1206.88 1
0 -7 0 -600.20 1388.83 1
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0 -7 1 18400. 2564.30 1
0 -7 -1 15025. 2205.88 1
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0 7 2 260418. 28774. 1
0 -7 2 210917. 23340. 1
0 -7 -2 238783. 26411. 1
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0 -7 -3 35080. 4302.59 1
0 7 -3 36495. 4293.12 1
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0 -7 -4 62911. 7328.01 1
0 7 -4 68395. 7741.77 1
0 -7 5 22134. 2818.04 1
0 -7 -5 13509. 2424.72 1
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0 7 -7 4532.90 1303.09 1
0 -7 8 7806.57 1463.61 1
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0 -7 9 16361. 2283.15 1
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0 -7 23 1195.41 1267.20 -1
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0 -7 24 -777.17 1216.85 1
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0 -7 25 389.78 954.137 1
0 7 -25 -1340.5 1573.78 1
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0 7 -27 88.48 1197.41 1
0 -8 0 224825. 24930. 1
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0 -8 -1 9411.76 1912.26 1
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0 -8 4 1883.85 1143.07 1
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0 8 -4 660.02 1170.49 1
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0 -8 5 8374.87 1644.56 1
0 -8 -5 7647.05 2083.25 1
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0 -8 -6 2610.17 1501.00 1
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0 8 -8 3824.52 1300.10 -1
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0 -8 10 6131.60 1238.78 1
0 8 -10 3230.80 1157.53 1
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0 8 -16 768.69 1137.59 1
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0 8 -17 1690.43 1187.94 1
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0 -8 21 5089.73 1280.16 1
0 8 -21 2465.60 1543.37 1
0 -8 22 7597.20 1515.45 -1
0 8 -22 4867.89 1654.04 -1
0 -8 23 2433.70 1184.94 1
0 8 -23 2860.91 1580.76 1
0 -8 24 1797.11 1380.86 1
0 8 -24 689.43 1580.76 1
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0 -8 26 1204.39 1300.10 -1
0 8 -26 196.36 1520.44 -1
0 -8 27 772.68 1180.46 -1
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0 8 -29 417.65 1322.03 1
0 8 -30 267.55 1413.26 1
0 8 -31 -362.81 1114.16 1
0 -9 0 -992.52 1601.69 1
0 9 0 653.04 1656.03 1
0 -9 1 89481. 10264. 1
0 -9 -1 92772. 10598. 1
0 9 -1 101745. 11496. 1
0 9 2 281705. 31201. 1
0 -9 2 263360. 29128. 1
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0 -9 3 26231. 3321.03 1
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0 -9 4 19626. 2725.32 1
0 -9 -4 20897. 3006.48 1
0 9 -4 18116. 2619.14 1
0 9 5 4681.95 2259.72 1
0 -9 -5 10444. 2095.21 1
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0 -9 -6 75523. 8808.57 1
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0 -9 7 7093.71 1345.46 1
0 9 -7 3399.80 1195.91 1
0 -9 8 3234.29 979.062 1
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0 -9 9 19801. 2574.27 1
0 9 -9 24716. 3118.14 1
0 -9 10 17856. 2394.31 1
0 9 -10 20130. 2662.51 1
0 -9 11 7696.90 1399.80 1
0 9 -11 5189.43 1288.13 1
0 -9 14 1042.37 966.599 1
0 9 -14 4867.89 1392.82 1
0 -9 17 4578.26 1184.94 1
0 9 -17 8140.57 1687.93 1
0 -9 18 1312.06 1098.20 1
0 9 -18 3455.13 1342.47 1
0 -9 19 10449. 1741.77 1
0 9 -19 12707. 2115.65 1
0 -9 20 621.14 989.530 1
0 9 -20 1603.69 1420.24 1
0 -9 21 3778.16 1171.48 1
0 9 -21 5822.53 1637.59 1
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0 9 -22 2366.90 1520.44 1
0 -9 23 1453.64 1016.95 1
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0 -9 24 573.28 957.128 -1
0 9 -24 2185.44 1456.63 -1
0 -9 25 3022.93 1197.91 1
0 9 -25 345.66 1439.68 1
0 -9 26 740.28 1086.74 1
0 9 -26 -471.24 1374.87 1
0 -9 27 826.52 1100.70 1
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0 -9 28 602.19 1297.61 1
0 9 -28 1087.74 1428.71 1
0 -9 29 2893.32 1318.54 1
0 9 -29 643.57 1335.99 1
0 -9 30 335.39 1174.48 1
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0 -9 31 -816.55 1194.42 1
0 -10 0 98554. 11206. 1
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0 -11 3 1931.20 1134.10 -1
0 -11 -3 -307.88 1384.35 -1
0 11 -3 1428.71 1184.45 -1
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0 0 0 0. 0.00 0
;
_shelx_hkl_checksum 5280
_shelx_res_file
;
REM Best SHELXD solution FINAL CC 75.03
REM Fragments: 35
REM
TITL GGYMLG in space group P 1 21 1 .
a.res
created by SHELXL-2019/3 at 17:09:16 on 11-Jul-2024
REM The peptide contains 6 residues with formula C26 H38 N6 O8 S1.
REM The molecular weight of the peptide is 594.7 Da.
REM The asymmetric unit contains 1 peptides.
REM Vm= 1.3 A^3/Da, solvent content= 3.2%.
CELL 0.0251 7.16 19.44 29.78 90.000 90.000 90.000
ZERR 1.00 0.0020 0.0019 0.0033 0.000 0.0 0.000
LATT -1
SYMM X+1/2,-Y+1/2,-Z
SYMM -X,Y+1/2,-Z+1/2
SYMM -X+1/2,-Y,Z+1/2
SFAC C 0.600 40.938 0.136 0.374 0.547 3.278 1.225 13.013 0 0 0 0 0.76 12.011
SFAC N 0.482 31.526 0.135 0.324 0.519 2.607 1.075 10.017 0 0 0 0 0.71 14.007
SFAC O 0.392 25.675 0.144 0.306 0.511 2.272 0.937 8.270 0 0 0 0 0.66 15.999
SFAC H 0.129 37.737 0.036 0.553 0.127 3.772 0.236 13.518 0 0 0 0 0.31 1.008
UNIT 144 8 8 216
L.S. 1
ACTA
LIST 4
WGHT 0.200000
EXTI 1934.495728
FVAR 27.79534
N1 2 0.561307 0.101364 0.076489 11.00000 0.05579 0.07237 =
0.08687 0.01188 0.00837 -0.00153
C30 1 0.116445 -0.206181 -0.043813 11.00000 0.19560 0.13111 =
0.40518 0.12826 -0.01659 -0.04914
AFIX 137
H22A 4 0.044779 -0.247895 -0.042927 11.00000 -1.50000
H22B 4 0.114682 -0.184834 -0.014747 11.00000 -1.50000
H22C 4 0.242977 -0.216593 -0.052029 11.00000 -1.50000
AFIX 0
C27 1 0.283537 0.100388 -0.201154 11.00000 0.27059 0.14296 =
0.05679 0.01862 0.01592 -0.00689
AFIX 137
H20A 4 0.339915 0.057323 -0.209225 11.00000 -1.50000
H20B 4 0.373071 0.128296 -0.185537 11.00000 -1.50000
H20C 4 0.243208 0.123828 -0.227819 11.00000 -1.50000
AFIX 0
C31 1 0.044487 -0.193847 -0.129069 11.00000 0.20078 0.16206 =
0.16421 -0.04590 0.06810 -0.08536
AFIX 137
H23A 4 -0.074293 -0.213499 -0.136753 11.00000 -1.50000
H23B 4 0.137123 -0.229503 -0.127907 11.00000 -1.50000
H23C 4 0.079207 -0.160516 -0.151342 11.00000 -1.50000
AFIX 0
C5 1 0.708915 0.144643 0.051076 11.00000 0.04954 0.08900 =
0.08122 0.00104 -0.00587 0.00313
AFIX 13
H5 4 0.648056 0.186745 0.040423 11.00000 -1.20000
AFIX 0
C9 1 0.255180 0.024004 0.129590 11.00000 0.07129 0.07691 =
0.05863 0.00080 0.01621 -0.00074
C13 1 0.235225 0.130721 0.178173 11.00000 0.07477 0.06506 =
0.07413 -0.03617 0.02741 -0.01084
AFIX 43
H8 4 0.283511 0.173576 0.185779 11.00000 -1.20000
AFIX 0
O1 3 0.332893 -0.012241 0.092891 11.00000 0.11042 0.07674 =
0.06784 0.00010 0.02104 0.00062
H25 4 0.410983 0.008752 0.082909 11.00000 0.13172
C32 1 -0.182368 -0.139338 -0.070585 11.00000 0.14227 0.16804 =
0.33938 0.01461 0.08841 -0.01042
AFIX 137
H5A 4 -0.229687 -0.111318 -0.094568 11.00000 -1.50000
H5B 4 -0.194821 -0.115105 -0.042657 11.00000 -1.50000
H5C 4 -0.251953 -0.181496 -0.069194 11.00000 -1.50000
AFIX 0
C18 1 0.531051 0.025185 -0.027338 11.00000 0.08982 0.07171 =
0.04888 0.00358 0.01317 0.00816
AFIX 43
H16 4 0.569550 -0.008962 -0.007521 11.00000 -1.20000
AFIX 0
C19 1 0.372163 0.007889 -0.058981 11.00000 0.09555 0.06302 =
0.04618 0.01216 -0.02677 -0.00290
C11 1 0.020390 0.034809 0.192040 11.00000 0.08157 0.07209 =
0.05965 0.00351 0.02575 -0.01439
AFIX 43
H9 4 -0.075810 0.015357 0.208745 11.00000 -1.20000
AFIX 0
C6 1 0.883001 0.166698 0.082415 11.00000 0.04372 0.08414 =
0.07344 0.00157 0.00205 0.00952
AFIX 23
H6B 4 0.839438 0.198303 0.105340 11.00000 -1.20000
H6A 4 0.931551 0.126161 0.097397 11.00000 -1.20000
AFIX 0
C28 1 -0.080070 0.047810 -0.195295 11.00000 0.34510 0.13545 =
0.17772 -0.01353 -0.17649 0.05378
AFIX 137
H24A 4 -0.115288 0.074544 -0.221043 11.00000 -1.50000
H24B 4 -0.183730 0.044888 -0.174938 11.00000 -1.50000
H24C 4 -0.044837 0.002402 -0.204718 11.00000 -1.50000
AFIX 0
C78 1 0.470056 0.132201 0.111739 11.00000 0.06166 0.07669 =
0.05884 -0.01580 0.00852 -0.01379
AFIX 43
H7 4 0.498828 0.177523 0.118956 11.00000 -1.20000
AFIX 0
C8 1 0.321383 0.093973 0.139706 11.00000 0.06140 0.07495 =
0.08357 0.00426 -0.00134 -0.00795
N12 2 0.619811 0.085048 -0.025571 11.00000 0.05502 0.08745 =
0.06452 0.00013 0.00904 0.00233
C10 1 0.098790 -0.005964 0.155504 11.00000 0.08596 0.04092 =
0.11216 0.00911 0.01482 -0.00881
C24 1 0.279978 -0.061197 -0.056469 11.00000 0.11229 0.06980 =
0.08292 -0.00073 -0.01060 0.00108
AFIX 43
H17 4 0.324177 -0.092411 -0.035323 11.00000 -1.20000
AFIX 0
C2 1 1.114071 0.154230 0.013350 11.00000 0.03825 0.10121 =
0.16030 0.01800 0.00984 -0.01361
AFIX 23
H2A 4 1.212487 0.177408 -0.003146 11.00000 -1.20000
H2B 4 1.163762 0.111257 0.024808 11.00000 -1.20000
AFIX 0
C016 1 0.321057 0.054063 -0.095698 11.00000 0.09248 0.07645 =
0.07532 -0.03677 -0.01724 -0.00722
C12 1 0.082566 0.104780 0.204478 11.00000 0.07315 0.09260 =
0.07543 -0.01931 0.00722 -0.00403
C4 1 0.777757 0.100002 0.006392 11.00000 0.04947 0.09048 =
0.09090 -0.00134 0.00064 0.01837
AFIX 13
H4 4 0.826317 0.055809 0.017087 11.00000 -1.20000
AFIX 0
O2 3 0.404781 0.117567 -0.101665 11.00000 0.10960 0.09455 =
0.06068 0.02499 -0.00879 -0.02256
H26 4 0.496487 0.114515 -0.075378 11.00000 0.12042
C22 1 0.079554 -0.031595 -0.121393 11.00000 0.11206 0.13192 =
0.03327 -0.00597 -0.02156 -0.02698
AFIX 43
H18 4 -0.013445 -0.045457 -0.141228 11.00000 -1.20000
AFIX 0
C25 1 0.105055 0.086386 -0.168835 11.00000 0.14108 0.08462 =
0.08747 -0.02148 -0.01032 0.01307
C33 1 0.016164 -0.081382 0.139470 11.00000 0.11023 0.05703 =
0.10454 -0.00778 0.03655 -0.01465
C1 1 1.046340 0.202120 0.054817 11.00000 0.05739 0.08639 =
0.13897 0.01474 0.00420 -0.00025
AFIX 23
H1A 4 1.151287 0.210756 0.074629 11.00000 -1.20000
H1B 4 1.003340 0.246026 0.043302 11.00000 -1.20000
AFIX 0
C14 1 -0.019105 0.144652 0.244531 11.00000 0.11187 0.07900 =
0.05917 0.00496 0.01403 0.00972
C23 1 0.135910 -0.081083 -0.083142 11.00000 0.09280 0.08316 =
0.05932 -0.00463 -0.02238 0.00839
C3 1 0.945248 0.139155 -0.018862 11.00000 0.06600 0.12203 =
0.05389 0.00304 0.01356 0.00627
AFIX 23
H3B 4 0.988097 0.111178 -0.043788 11.00000 -1.20000
H3A 4 0.899057 0.182231 -0.030982 11.00000 -1.20000
AFIX 0
C21 1 0.162555 0.033947 -0.127785 11.00000 0.08202 0.07515 =
0.07236 -0.01734 -0.00331 -0.00137
C29 1 0.029673 -0.155886 -0.079332 11.00000 0.11275 0.07897 =
0.13138 -0.02792 0.01329 -0.01834
C36 1 0.169820 -0.138442 0.142718 11.00000 0.20421 0.06882 =
0.13943 -0.01920 0.03859 -0.00683
AFIX 137
H14A 4 0.280629 -0.123222 0.127530 11.00000 -1.50000
H14B 4 0.124977 -0.179896 0.128910 11.00000 -1.50000
H14C 4 0.198090 -0.147204 0.173707 11.00000 -1.50000
AFIX 0
C35 1 -0.156400 -0.103398 0.174781 11.00000 0.14759 0.07072 =
0.21245 -0.03435 0.07505 -0.02270
AFIX 137
H13A 4 -0.202894 -0.148120 0.166911 11.00000 -1.50000
H13B 4 -0.255648 -0.070353 0.172670 11.00000 -1.50000
H13C 4 -0.109386 -0.104317 0.204965 11.00000 -1.50000
AFIX 0
C34 1 -0.072485 -0.078615 0.090674 11.00000 0.14074 0.09885 =
0.11110 -0.02683 0.01196 -0.04087
AFIX 137
H15A 4 0.021516 -0.089474 0.068807 11.00000 -1.50000
H15B 4 -0.120250 -0.033283 0.085053 11.00000 -1.50000
H15C 4 -0.172358 -0.111415 0.088638 11.00000 -1.50000
AFIX 0
C26 1 0.022668 0.157781 -0.149336 11.00000 0.16671 0.10923 =
0.09589 -0.01716 -0.00576 0.03712
AFIX 137
H19A 4 -0.014689 0.186796 -0.173826 11.00000 -1.50000
H19B 4 0.117152 0.180621 -0.131992 11.00000 -1.50000
H19C 4 -0.083403 0.148338 -0.130606 11.00000 -1.50000
AFIX 0
C15 1 0.075321 0.220382 0.253812 11.00000 0.33303 0.14084 =
0.27125 -0.11935 0.17193 -0.02846
AFIX 137
H10A 4 0.208919 0.216395 0.252995 11.00000 -1.50000
H10B 4 0.037160 0.236882 0.282777 11.00000 -1.50000
H10C 4 0.035044 0.252106 0.231085 11.00000 -1.50000
AFIX 0
C17 1 -0.235821 0.148464 0.232181 11.00000 0.11897 0.17938 =
0.15941 -0.05394 0.01765 0.04408
AFIX 137
H12A 4 -0.267128 0.194540 0.223357 11.00000 -1.50000
H12B 4 -0.308813 0.135651 0.257895 11.00000 -1.50000
H12C 4 -0.261845 0.117495 0.207864 11.00000 -1.50000
AFIX 0
C16 1 0.000824 0.101430 0.291588 11.00000 0.23101 0.14093 =
0.09387 -0.02838 0.02210 0.07176
AFIX 137
H11A 4 -0.047346 0.055777 0.287475 11.00000 -1.50000
H11B 4 -0.068564 0.124260 0.314799 11.00000 -1.50000
H11C 4 0.130046 0.098955 0.300032 11.00000 -1.50000
REM #####
AFIX 0
HKLF 4
REM GGYMLG in space group P 1 21 1 .
REM wR2 = 0.3641, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.1167 for 2894 Fo > 4sig(Fo) and 0.1707 for all 5692 data
REM 382 parameters refined using 0 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 0.101, deepest hole -0.096, 1-sigma level 0.027
Q1 1 0.0165 -0.2694 -0.0580 11.00000 0.05 0.10
Q2 1 -0.0754 -0.1688 -0.0202 11.00000 0.05 0.10
Q3 1 0.0797 -0.1726 0.0067 11.00000 0.05 0.08
Q4 1 -0.2433 -0.1974 -0.0580 11.00000 0.05 0.08
Q5 1 -0.0711 -0.1438 0.0708 11.00000 0.05 0.08
Q6 1 -0.1575 -0.1420 0.0084 11.00000 0.05 0.08
Q7 1 0.1461 0.0579 -0.1906 11.00000 0.05 0.07
Q8 1 -0.0218 -0.1571 -0.1845 11.00000 0.05 0.07
Q9 1 -0.2157 -0.1579 -0.1224 11.00000 0.05 0.07
Q10 1 -0.1251 -0.1751 -0.0933 11.00000 0.05 0.07
Q11 1 0.1488 0.0957 0.1603 11.00000 0.05 0.07
Q12 1 0.2269 0.1229 0.3098 11.00000 0.05 0.07
Q13 1 -0.0157 -0.0113 0.2352 11.00000 0.05 0.07
Q14 1 0.3005 -0.2211 -0.0601 11.00000 0.05 0.07
Q15 1 0.1835 0.0158 -0.1733 11.00000 0.05 0.07
Q16 1 -0.1273 0.1137 0.3334 11.00000 0.05 0.06
Q17 1 0.2822 0.0084 -0.1064 11.00000 0.05 0.06
Q18 1 0.0650 -0.1996 -0.0783 11.00000 0.05 0.06
Q19 1 -0.0806 -0.1197 0.1326 11.00000 0.05 0.06
Q20 1 0.1487 0.0185 0.1273 11.00000 0.05 0.06
;
_shelx_res_checksum 90961
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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 0.5613(11) 0.1014(5) 0.0765(4) 0.072(3) Uani d 1 . .
C C30 0.116(3) -0.2062(11) -0.0438(13) 0.244(19) Uani d 1 . .
H H22A 0.044779 -0.247895 -0.042927 0.366 Uiso calc 1 . .
H H22B 0.114682 -0.184834 -0.014747 0.366 Uiso calc 1 . .
H H22C 0.242977 -0.216593 -0.052029 0.366 Uiso calc 1 . .
C C27 0.284(4) 0.1004(9) -0.2012(7) 0.157(8) Uani d 1 . .
H H20A 0.339915 0.057323 -0.209225 0.235 Uiso calc 1 . .
H H20B 0.373071 0.128296 -0.185537 0.235 Uiso calc 1 . .
H H20C 0.243208 0.123828 -0.227819 0.235 Uiso calc 1 . .
C C31 0.044(3) -0.1938(10) -0.1291(9) 0.176(10) Uani d 1 . .
H H23A -0.074293 -0.213499 -0.136753 0.264 Uiso calc 1 . .
H H23B 0.137123 -0.229503 -0.127907 0.264 Uiso calc 1 . .
H H23C 0.079207 -0.160516 -0.151342 0.264 Uiso calc 1 . .
C C5 0.7089(12) 0.1446(6) 0.0511(5) 0.073(3) Uani d 1 . .
H H5 0.648056 0.186745 0.040423 0.088 Uiso calc 1 . .
C C9 0.2552(13) 0.0240(5) 0.1296(5) 0.069(3) Uani d 1 . .
C C13 0.2352(13) 0.1307(5) 0.1782(4) 0.071(3) Uani d 1 . .
H H8 0.283511 0.173576 0.185779 0.086 Uiso calc 1 . .
O O1 0.3329(18) -0.0122(5) 0.0929(4) 0.085(3) Uani d 1 . .
H H25 0.411(13) 0.009(5) 0.083(4) 0.13(4) Uiso d 1 . .
C C32 -0.182(3) -0.1393(11) -0.0706(14) 0.217(15) Uani d 1 . .
H H5A -0.229687 -0.111318 -0.094568 0.325 Uiso calc 1 . .
H H5B -0.194821 -0.115105 -0.042657 0.325 Uiso calc 1 . .
H H5C -0.251953 -0.181496 -0.069194 0.325 Uiso calc 1 . .
C C18 0.5311(14) 0.0252(5) -0.0273(4) 0.070(3) Uani d 1 . .
H H16 0.569550 -0.008962 -0.007521 0.084 Uiso calc 1 . .
C C19 0.3722(15) 0.0079(5) -0.0590(4) 0.068(3) Uani d 1 . .
C C11 0.0204(15) 0.0348(5) 0.1920(5) 0.071(3) Uani d 1 . .
H H9 -0.075810 0.015357 0.208745 0.085 Uiso calc 1 . .
C C6 0.8830(10) 0.1667(5) 0.0824(4) 0.067(3) Uani d 1 . .
H H6B 0.839438 0.198303 0.105340 0.081 Uiso calc 1 . .
H H6A 0.931551 0.126161 0.097397 0.081 Uiso calc 1 . .
C C28 -0.080(4) 0.0478(10) -0.1953(9) 0.219(16) Uani d 1 . .
H H24A -0.115288 0.074544 -0.221043 0.329 Uiso calc 1 . .
H H24B -0.183730 0.044888 -0.174938 0.329 Uiso calc 1 . .
H H24C -0.044837 0.002402 -0.204718 0.329 Uiso calc 1 . .
C C78 0.4701(12) 0.1322(5) 0.1117(4) 0.066(3) Uani d 1 . .
H H7 0.498828 0.177523 0.118956 0.079 Uiso calc 1 . .
C C8 0.3214(13) 0.0940(5) 0.1397(5) 0.073(4) Uani d 1 . .
N N12 0.6198(11) 0.0850(5) -0.0256(4) 0.069(3) Uani d 1 . .
C C10 0.0988(14) -0.0060(4) 0.1555(5) 0.080(4) Uani d 1 . .
C C24 0.2800(18) -0.0612(5) -0.0565(5) 0.088(4) Uani d 1 . .
H H17 0.324177 -0.092411 -0.035323 0.106 Uiso calc 1 . .
C C2 1.1141(12) 0.1542(6) 0.0133(6) 0.100(5) Uani d 1 . .
H H2A 1.212487 0.177408 -0.003146 0.120 Uiso calc 1 . .
H H2B 1.163762 0.111257 0.024808 0.120 Uiso calc 1 . .
C C016 0.3211(16) 0.0541(5) -0.0957(5) 0.081(4) Uani d 1 . .
C C12 0.0826(14) 0.1048(6) 0.2045(5) 0.080(4) Uani d 1 . .
C C4 0.7778(11) 0.1000(6) 0.0064(5) 0.077(3) Uani d 1 . .
H H4 0.826317 0.055809 0.017087 0.092 Uiso calc 1 . .
O O2 0.4048(17) 0.1176(5) -0.1017(5) 0.088(3) Uani d 1 . .
H H26 0.496(12) 0.115(4) -0.075(4) 0.12(2) Uiso d 1 . .
C C22 0.0796(18) -0.0316(7) -0.1214(5) 0.092(4) Uani d 1 . .
H H18 -0.013445 -0.045457 -0.141228 0.111 Uiso calc 1 . .
C C25 0.105(2) 0.0864(6) -0.1688(6) 0.104(5) Uani d 1 . .
C C33 0.0162(18) -0.0814(5) 0.1395(6) 0.091(5) Uani d 1 . .
C C1 1.0463(14) 0.2021(6) 0.0548(6) 0.094(5) Uani d 1 . .
H H1A 1.151287 0.210756 0.074629 0.113 Uiso calc 1 . .
H H1B 1.003340 0.246026 0.043302 0.113 Uiso calc 1 . .
C C14 -0.0191(18) 0.1447(5) 0.2445(5) 0.083(4) Uani d 1 . .
C C23 0.1359(16) -0.0811(5) -0.0831(5) 0.078(3) Uani d 1 . .
C C3 0.9452(13) 0.1392(7) -0.0189(5) 0.081(3) Uani d 1 . .
H H3B 0.988097 0.111178 -0.043788 0.097 Uiso calc 1 . .
H H3A 0.899057 0.182231 -0.030982 0.097 Uiso calc 1 . .
C C21 0.1626(15) 0.0339(5) -0.1278(5) 0.077(4) Uani d 1 . .
C C29 0.0297(19) -0.1559(6) -0.0793(6) 0.108(5) Uani d 1 . .
C C36 0.170(3) -0.1384(6) 0.1427(7) 0.137(7) Uani d 1 . .
H H14A 0.280629 -0.123222 0.127530 0.206 Uiso calc 1 . .
H H14B 0.124977 -0.179896 0.128910 0.206 Uiso calc 1 . .
H H14C 0.198090 -0.147204 0.173707 0.206 Uiso calc 1 . .
C C35 -0.156(2) -0.1034(6) 0.1748(8) 0.144(8) Uani d 1 . .
H H13A -0.202894 -0.148120 0.166911 0.215 Uiso calc 1 . .
H H13B -0.255648 -0.070353 0.172670 0.215 Uiso calc 1 . .
H H13C -0.109386 -0.104317 0.204965 0.215 Uiso calc 1 . .
C C34 -0.072(2) -0.0786(7) 0.0907(7) 0.117(5) Uani d 1 . .
H H15A 0.021516 -0.089474 0.068807 0.175 Uiso calc 1 . .
H H15B -0.120250 -0.033283 0.085053 0.175 Uiso calc 1 . .
H H15C -0.172358 -0.111415 0.088638 0.175 Uiso calc 1 . .
C C26 0.023(3) 0.1578(7) -0.1493(6) 0.124(6) Uani d 1 . .
H H19A -0.014689 0.186796 -0.173826 0.186 Uiso calc 1 . .
H H19B 0.117152 0.180621 -0.131992 0.186 Uiso calc 1 . .
H H19C -0.083403 0.148338 -0.130606 0.186 Uiso calc 1 . .
C C15 0.075(4) 0.2204(10) 0.2538(11) 0.248(18) Uani d 1 . .
H H10A 0.208919 0.216395 0.252995 0.373 Uiso calc 1 . .
H H10B 0.037160 0.236882 0.282777 0.373 Uiso calc 1 . .
H H10C 0.035044 0.252106 0.231085 0.373 Uiso calc 1 . .
C C17 -0.236(2) 0.1485(9) 0.2322(8) 0.153(8) Uani d 1 . .
H H12A -0.267128 0.194540 0.223357 0.229 Uiso calc 1 . .
H H12B -0.308813 0.135651 0.257895 0.229 Uiso calc 1 . .
H H12C -0.261845 0.117495 0.207864 0.229 Uiso calc 1 . .
C C16 0.001(4) 0.1014(9) 0.2916(7) 0.155(8) Uani d 1 . .
H H11A -0.047346 0.055777 0.287475 0.233 Uiso calc 1 . .
H H11B -0.068564 0.124260 0.314799 0.233 Uiso calc 1 . .
H H11C 0.130046 0.098955 0.300032 0.233 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.056(4) 0.072(5) 0.087(10) -0.002(4) 0.008(5) 0.012(5)
C30 0.20(2) 0.131(14) 0.41(5) -0.049(14) -0.02(2) 0.13(2)
C27 0.27(3) 0.143(13) 0.057(15) -0.007(14) 0.016(16) 0.019(9)
C31 0.201(17) 0.162(15) 0.16(3) -0.085(14) 0.068(18) -0.046(15)
C5 0.050(5) 0.089(7) 0.081(11) 0.003(5) -0.006(6) 0.001(6)
C9 0.071(5) 0.077(6) 0.059(11) -0.001(5) 0.016(6) 0.001(5)
C13 0.075(6) 0.065(5) 0.074(10) -0.011(5) 0.027(6) -0.036(5)
O1 0.110(7) 0.077(6) 0.068(10) 0.001(6) 0.021(7) 0.000(5)
C32 0.142(13) 0.168(17) 0.34(5) -0.010(13) 0.09(2) 0.01(2)
C18 0.090(6) 0.072(6) 0.049(9) 0.008(6) 0.013(7) 0.004(5)
C19 0.096(6) 0.063(6) 0.046(9) -0.003(5) -0.027(7) 0.012(5)
C11 0.082(6) 0.072(6) 0.060(10) -0.014(5) 0.026(6) 0.004(5)
C6 0.044(4) 0.084(6) 0.073(10) 0.010(4) 0.002(5) 0.002(5)
C28 0.35(4) 0.135(14) 0.18(3) 0.054(17) -0.18(3) -0.014(13)
C78 0.062(5) 0.077(6) 0.059(9) -0.014(5) 0.009(6) -0.016(5)
C8 0.061(5) 0.075(6) 0.084(12) -0.008(5) -0.001(6) 0.004(6)
N12 0.055(4) 0.087(6) 0.065(9) 0.002(4) 0.009(5) 0.000(5)
C10 0.086(6) 0.041(5) 0.112(13) -0.009(5) 0.015(7) 0.009(5)
C24 0.112(8) 0.070(6) 0.083(12) 0.001(6) -0.011(9) -0.001(6)
C2 0.038(4) 0.101(8) 0.160(18) -0.014(5) 0.010(7) 0.018(8)
C016 0.092(7) 0.076(6) 0.075(13) -0.007(6) -0.017(7) -0.037(6)
C12 0.073(6) 0.093(7) 0.075(12) -0.004(5) 0.007(7) -0.019(6)
C4 0.049(4) 0.090(7) 0.091(12) 0.018(5) 0.001(6) -0.001(6)
O2 0.110(7) 0.095(7) 0.061(10) -0.023(5) -0.009(7) 0.025(5)
C22 0.112(8) 0.132(10) 0.033(11) -0.027(7) -0.022(7) -0.006(7)
C25 0.141(11) 0.085(8) 0.087(15) 0.013(7) -0.010(10) -0.021(7)
C33 0.110(8) 0.057(6) 0.105(15) -0.015(6) 0.037(9) -0.008(6)
C1 0.057(5) 0.086(7) 0.139(15) 0.000(5) 0.004(7) 0.015(8)
C14 0.112(8) 0.079(7) 0.059(11) 0.010(6) 0.014(7) 0.005(6)
C23 0.093(7) 0.083(7) 0.059(11) 0.008(6) -0.022(8) -0.005(6)
C3 0.066(5) 0.122(9) 0.054(10) 0.006(6) 0.014(6) 0.003(6)
C21 0.082(6) 0.075(6) 0.072(12) -0.001(5) -0.003(7) -0.017(6)
C29 0.113(8) 0.079(7) 0.131(17) -0.018(7) 0.013(10) -0.028(8)
C36 0.204(15) 0.069(8) 0.139(19) -0.007(9) 0.039(15) -0.019(8)
C35 0.148(11) 0.071(7) 0.21(2) -0.023(8) 0.075(14) -0.034(10)
C34 0.141(11) 0.099(9) 0.111(17) -0.041(8) 0.012(11) -0.027(8)
C26 0.167(12) 0.109(9) 0.096(17) 0.037(10) -0.006(12) -0.017(8)
C15 0.33(3) 0.141(14) 0.27(4) -0.028(18) 0.17(3) -0.12(2)
C17 0.119(11) 0.179(15) 0.16(2) 0.044(11) 0.018(12) -0.054(14)
C16 0.23(2) 0.141(12) 0.094(18) 0.072(14) 0.022(15) -0.028(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 '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'
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
C78 N1 C5 . . 117.4(9) ?
N1 C5 C6 . . 112.9(10) ?
N1 C5 C4 . . 108.0(8) ?
C6 C5 C4 . . 111.8(7) ?
O1 C9 C8 . . 119.5(9) ?
O1 C9 C10 . . 120.3(10) ?
C8 C9 C10 . . 120.1(10) ?
C12 C13 C8 . . 124.6(9) ?
N12 C18 C19 . . 125.4(10) ?
C016 C19 C24 . . 118.5(9) ?
C016 C19 C18 . . 121.1(8) ?
C24 C19 C18 . . 119.9(9) ?
C10 C11 C12 . . 124.8(9) ?
C1 C6 C5 . . 112.6(11) ?
N1 C78 C8 . . 122.0(9) ?
C9 C8 C13 . . 118.0(9) ?
C9 C8 C78 . . 123.9(10) ?
C13 C8 C78 . . 118.1(8) ?
C18 N12 C4 . . 123.6(10) ?
C11 C10 C9 . . 117.8(8) ?
C11 C10 C33 . . 124.1(9) ?
C9 C10 C33 . . 118.0(11) ?
C23 C24 C19 . . 124.1(11) ?
C3 C2 C1 . . 110.0(8) ?
O2 C016 C19 . . 122.4(10) ?
O2 C016 C21 . . 117.9(12) ?
C19 C016 C21 . . 119.7(9) ?
C13 C12 C11 . . 114.6(10) ?
C13 C12 C14 . . 125.7(9) ?
C11 C12 C14 . . 119.7(9) ?
N12 C4 C3 . . 110.8(11) ?
N12 C4 C5 . . 112.6(7) ?
C3 C4 C5 . . 110.4(9) ?
C21 C22 C23 . . 123.3(10) ?
C26 C25 C27 . . 110.9(13) ?
C26 C25 C21 . . 110.9(14) ?
C27 C25 C21 . . 110.4(11) ?
C26 C25 C28 . . 105.0(12) ?
C27 C25 C28 . . 114.2(18) ?
C21 C25 C28 . . 105.3(12) ?
C36 C33 C34 . . 111.2(12) ?
C36 C33 C10 . . 111.1(11) ?
C34 C33 C10 . . 112.2(10) ?
C36 C33 C35 . . 107.3(10) ?
C34 C33 C35 . . 106.7(13) ?
C10 C33 C35 . . 108.0(11) ?
C6 C1 C2 . . 111.5(9) ?
C17 C14 C12 . . 107.1(12) ?
C17 C14 C16 . . 107.8(15) ?
C12 C14 C16 . . 110.5(10) ?
C17 C14 C15 . . 113.4(14) ?
C12 C14 C15 . . 111.9(11) ?
C16 C14 C15 . . 106.2(16) ?
C24 C23 C22 . . 116.9(10) ?
C24 C23 C29 . . 124.2(11) ?
C22 C23 C29 . . 118.7(10) ?
C2 C3 C4 . . 112.1(11) ?
C22 C21 C016 . . 117.1(11) ?
C22 C21 C25 . . 123.5(10) ?
C016 C21 C25 . . 119.4(10) ?
C30 C29 C32 . . 113(2) ?
C30 C29 C23 . . 114.5(13) ?
C32 C29 C23 . . 106.1(11) ?
C30 C29 C31 . . 107.4(18) ?
C32 C29 C31 . . 107(2) ?
C23 C29 C31 . . 107.6(13) ?
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 C78 . 1.374(16) ?
N1 C5 . 1.548(15) ?
C30 C29 . 1.57(3) ?
C27 C25 . 1.62(3) ?
C31 C29 . 1.66(3) ?
C5 C6 . 1.615(14) ?
C5 C4 . 1.663(19) ?
C9 O1 . 1.414(16) ?
C9 C8 . 1.472(14) ?
C9 C10 . 1.479(15) ?
C13 C12 . 1.436(16) ?
C13 C8 . 1.484(17) ?
C32 C29 . 1.57(2) ?
C18 N12 . 1.327(13) ?
C18 C19 . 1.515(16) ?
C19 C016 . 1.461(18) ?
C19 C24 . 1.498(14) ?
C11 C10 . 1.458(17) ?
C11 C12 . 1.478(15) ?
C6 C1 . 1.587(15) ?
C28 C25 . 1.71(3) ?
C78 C8 . 1.542(16) ?
N12 C4 . 1.506(16) ?
C10 C33 . 1.652(15) ?
C24 C23 . 1.358(17) ?
C2 C3 . 1.571(17) ?
C2 C1 . 1.62(2) ?
C016 O2 . 1.384(15) ?
C016 C21 . 1.534(17) ?
C12 C14 . 1.598(18) ?
C4 C3 . 1.607(16) ?
C22 C21 . 1.419(16) ?
C22 C23 . 1.545(19) ?
C25 C26 . 1.616(18) ?
C25 C21 . 1.64(2) ?
C33 C36 . 1.57(2) ?
C33 C34 . 1.59(3) ?
C33 C35 . 1.68(2) ?
C14 C17 . 1.60(2) ?
C14 C16 . 1.64(2) ?
C14 C15 . 1.64(2) ?
C23 C29 . 1.645(16) ?