# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_P-TA
_database_code_depnum_ccdc_archive 'CCDC 2115290'
loop_
_audit_author_name
_audit_author_address
yanjun.ding
;KAUST
Saudi Arabia
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H2 Cl2, C63 H84 N6 O6'
_chemical_formula_sum            'C64 H86 Cl2 N6 O6'
_chemical_formula_weight         1106.28
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_H-M_alt        'P 31'
_space_group_name_Hall           'P 31'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   20.2894(6)
_cell_length_b                   20.2894(6)
_cell_length_c                   13.6577(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4869.1(3)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    120.01
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1012 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.9064.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63281
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.007
_diffrn_ambient_temperature      120.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11228
_reflns_number_total             14887
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 4366 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         14887
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0699
_refine_ls_restrained_S_all      1.062
_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/[σ²(Fo²)+(0.1295P)²+0.5763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2123
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9658(12)
 0.0342(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 Cl1-C63
 1.78 with sigma of 0.02
 Cl4-C63
 1.77 with sigma of 0.02
 Cl1-C63 = Cl4-C63
 1.771 with sigma of 0.01
 Cl2-Cl3
 2.916 with sigma of 0.03
 Cl1-Cl4
 2.916 with sigma of 0.03
 Cl2-C2
 1.78 with sigma of 0.02
 Cl3-C2
 1.77 with sigma of 0.02
 Cl2-C2 = Cl3-C2
 1.771 with sigma of 0.01
 Cl1-Cl4
 2.92 with sigma of 0.04
 Cl2-Cl3
 2.92 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl4 \\sim C63: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Cl2 \\sim Cl3 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Cl1 \\sim Cl4 \\sim C63 \\sim Cl2 \\sim Cl3 \\sim C2 \\sim C61: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
5. Rigid body (RIGU) restrains
 Cl1, Cl4, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, Cl3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl1(0.75) Cl4(0.75) C63(0.75) H63A(0.75) H63B(0.75) Cl2(0.25)
 Cl3(0.25) C2(0.25) H2A(0.25) H2B(0.25)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8), C18(H18), C26(H26), C28(H28), C54(H54)
7.b Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C27(H27A,H27B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B),
 C52(H52A,H52B), C55(H55A,H55B), C58(H58A,H58B), C60(H60A,H60B), C65(H65A,H65B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C15(H15), C22(H22), C23(H23), C24(H24), C25(H25),
 C29(H29), C42(H42), C45(H45), C48(H48)
7.d X=CH2 refined with riding coordinates:
 C31(H31A,H31B), C51(H51A,H51B), C53(H53A,H53B), C57(H57A,H57B), C59(H59A,
 H59B), C61(H61A,H61B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.7243(3) 0.7372(3) 0.7176(4) 0.1199(14) Uani 0.75 1 d D U P A 1
Cl4 Cl 0.61156(17) 0.61561(17) 0.5945(4) 0.1034(13) Uani 0.75 1 d D U P A 1
C63 C 0.6645(7) 0.7144(5) 0.6111(11) 0.091(4) Uani 0.75 1 d D U P A 1
H63A H 0.629605 0.734800 0.619003 0.109 Uiso 0.75 1 calc R U P A 1
H63B H 0.696464 0.738391 0.552579 0.109 Uiso 0.75 1 calc R U P A 1
Cl2 Cl 0.6943(9) 0.6991(9) 0.5958(13) 0.152(6) Uani 0.25 1 d D U P B 2
Cl3 Cl 0.6540(9) 0.5869(8) 0.7267(13) 0.139(4) Uani 0.25 1 d D U P B 2
C2 C 0.627(2) 0.655(2) 0.694(3) 0.139(8) Uani 0.25 1 d D U P B 2
H2A H 0.634930 0.690894 0.747439 0.167 Uiso 0.25 1 calc R U P B 2
H2B H 0.573533 0.630747 0.670378 0.167 Uiso 0.25 1 calc R U P B 2
O1 O 0.70637(18) 0.9122(2) 0.6920(2) 0.0337(8) Uani 1 1 d . . . . .
O2 O 0.4108(2) 0.4502(2) 0.6829(3) 0.0388(9) Uani 1 1 d . . . . .
O3 O 0.8519(2) 0.62745(19) 0.6710(2) 0.0334(8) Uani 1 1 d . . . . .
O4 O 0.4970(2) 0.4726(2) 0.2950(2) 0.0308(7) Uani 1 1 d . . . . .
O5 O 0.62596(19) 0.8285(2) 0.3053(2) 0.0369(9) Uani 1 1 d . . . . .
O6 O 0.8572(2) 0.69896(19) 0.2797(2) 0.0313(8) Uani 1 1 d . . . . .
N1 N 0.8732(2) 0.9407(2) 0.4940(3) 0.0213(7) Uani 1 1 d . . . . .
N2 N 0.3920(2) 0.6050(2) 0.5064(3) 0.0241(8) Uani 1 1 d . . . . .
N3 N 0.4560(2) 0.7400(2) 0.5070(3) 0.0232(8) Uani 1 1 d . . . . .
N4 N 0.9393(2) 0.8725(2) 0.4832(3) 0.0216(7) Uani 1 1 d . . . . .
N5 N 0.7171(2) 0.4544(2) 0.4770(3) 0.0259(8) Uani 1 1 d . . . . .
N6 N 0.5831(2) 0.3815(2) 0.4765(3) 0.0226(8) Uani 1 1 d . . . . .
C1 C 0.9901(2) 0.9526(2) 0.4595(3) 0.0191(8) Uani 1 1 d . . . . .
H1 H 0.987283 0.960370 0.387699 0.023 Uiso 1 1 calc R U . . .
C3 C 0.6479(3) 0.4600(3) 0.4739(5) 0.0422(14) Uani 1 1 d . . . . .
H3A H 0.646508 0.486027 0.413290 0.051 Uiso 1 1 calc R U . . .
H3B H 0.646032 0.489224 0.530918 0.051 Uiso 1 1 calc R U . . .
C4 C 0.4437(3) 0.5096(3) 0.4303(3) 0.0250(9) Uani 1 1 d . . . . .
H4 H 0.436971 0.543541 0.389057 0.030 Uiso 1 1 calc R U . . .
C5 C 0.4677(3) 0.6739(3) 0.5154(4) 0.0350(12) Uani 1 1 d . . . . .
H5A H 0.501855 0.675214 0.462815 0.042 Uiso 1 1 calc R U . . .
H5B H 0.490807 0.674531 0.579451 0.042 Uiso 1 1 calc R U . . .
C6 C 0.8133(3) 0.6046(3) 0.4112(3) 0.0274(9) Uani 1 1 d . . . . .
H6 H 0.785483 0.564341 0.366261 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6886(4) 0.9311(5) 0.8587(5) 0.060(2) Uani 1 1 d . . . . .
H7 H 0.726234 0.983554 0.858831 0.072 Uiso 1 1 calc R U . . .
C8 C 0.6162(2) 0.3348(2) 0.4479(3) 0.0221(9) Uani 1 1 d . . . . .
H8 H 0.624766 0.338644 0.375527 0.027 Uiso 1 1 calc R U . . .
C9 C 0.2571(3) 0.5826(3) 0.4950(4) 0.0276(10) Uani 1 1 d . . . . .
H9A H 0.233288 0.532030 0.526914 0.033 Uiso 1 1 calc R U . . .
H9B H 0.256475 0.575192 0.423276 0.033 Uiso 1 1 calc R U . . .
C10 C 1.0730(2) 0.9865(3) 0.4891(3) 0.0246(9) Uani 1 1 d . . . . .
H10A H 1.096760 0.961717 0.452154 0.030 Uiso 1 1 calc R U . . .
H10B H 1.076816 0.978399 0.559905 0.030 Uiso 1 1 calc R U . . .
C11 C 0.6209(3) 0.2153(3) 0.4480(4) 0.0344(11) Uani 1 1 d . . . . .
H11A H 0.596445 0.162524 0.473355 0.041 Uiso 1 1 calc R U . . .
H11B H 0.622011 0.212706 0.375715 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4221(3) 0.5025(3) 0.5275(3) 0.0251(9) Uani 1 1 d . . . . .
C13 C 0.6490(3) 0.8963(4) 0.7636(4) 0.0438(14) Uani 1 1 d . . . . .
H13A H 0.615673 0.840618 0.771269 0.053 Uiso 1 1 calc R U . . .
H13B H 0.617275 0.918319 0.743249 0.053 Uiso 1 1 calc R U . . .
C14 C 0.7411(2) 0.9072(3) 0.5295(3) 0.0234(9) Uani 1 1 d . . . . .
C15 C 0.7032(4) 0.7721(5) 0.2565(6) 0.068(2) Uani 1 1 d . . . . .
H15 H 0.743719 0.775876 0.217514 0.082 Uiso 1 1 calc R U . . .
C16 C 0.4755(2) 0.4676(3) 0.3915(3) 0.0246(9) Uani 1 1 d . . . . .
C17 C 0.5212(3) 0.3728(3) 0.4132(4) 0.0293(10) Uani 1 1 d . . . . .
H17A H 0.481591 0.318414 0.409442 0.035 Uiso 1 1 calc R U . . .
H17B H 0.540935 0.390343 0.346237 0.035 Uiso 1 1 calc R U . . .
C18 C 0.9541(2) 0.9913(2) 0.5150(3) 0.0198(8) Uani 1 1 d . . . . .
H18 H 0.963114 0.989703 0.586670 0.024 Uiso 1 1 calc R U . . .
C19 C 0.4823(3) 0.5208(3) 0.2331(4) 0.0354(11) Uani 1 1 d . . . . .
H19A H 0.513135 0.574424 0.254514 0.042 Uiso 1 1 calc R U . . .
H19B H 0.427863 0.505906 0.236801 0.042 Uiso 1 1 calc R U . . .
C20 C 0.6479(3) 0.8504(3) 0.4012(3) 0.0259(9) Uani 1 1 d . . . . .
C21 C 1.1139(3) 1.0723(3) 0.4660(4) 0.0300(10) Uani 1 1 d . . . . .
H21A H 1.166013 1.096457 0.493478 0.036 Uiso 1 1 calc R U . . .
H21B H 1.118645 1.079043 0.394030 0.036 Uiso 1 1 calc R U . . .
C22 C 0.7227(2) 0.8871(3) 0.4328(3) 0.0248(9) Uani 1 1 d . . . . .
H22 H 0.762141 0.898738 0.386814 0.030 Uiso 1 1 calc R U . . .
C23 C 0.8250(4) 0.6716(3) 0.1122(4) 0.0426(13) Uani 1 1 d . . . . .
H23 H 0.875363 0.698527 0.087159 0.051 Uiso 1 1 calc R U . . .
C24 C 0.6071(2) 0.8521(3) 0.5663(3) 0.0264(9) Uani 1 1 d . . . . .
H24 H 0.567588 0.839438 0.612550 0.032 Uiso 1 1 calc R U . . .
C25 C 0.5026(4) 0.5125(4) 0.1309(4) 0.0483(15) Uani 1 1 d . . . . .
H25 H 0.483079 0.462557 0.105430 0.058 Uiso 1 1 calc R U . . .
C26 C 0.6913(3) 0.3748(2) 0.4994(3) 0.0231(9) Uani 1 1 d . . . . .
H26 H 0.683033 0.366369 0.571523 0.028 Uiso 1 1 calc R U . . .
C27 C 0.4094(5) 0.3924(4) 0.7446(4) 0.0571(19) Uani 1 1 d . . . . .
H27A H 0.461828 0.404509 0.761233 0.069 Uiso 1 1 calc R U . . .
H27B H 0.383110 0.342260 0.711500 0.069 Uiso 1 1 calc R U . . .
C28 C 0.3383(2) 0.6314(2) 0.5306(3) 0.0234(9) Uani 1 1 d . . . . .
H28 H 0.338167 0.638425 0.603065 0.028 Uiso 1 1 calc R U . . .
C29 C 0.3661(5) 0.3915(4) 0.8370(5) 0.064(2) Uani 1 1 d . . . . .
H29 H 0.319387 0.390807 0.827825 0.077 Uiso 1 1 calc R U . . .
C30 C 0.8540(3) 0.6796(3) 0.3774(3) 0.0251(9) Uani 1 1 d . . . . .
C31 C 0.6744(5) 0.8940(7) 0.9404(5) 0.095(4) Uani 1 1 d . . . . .
H31A H 0.637019 0.841535 0.942627 0.114 Uiso 1 1 calc R U . . .
H31B H 0.701347 0.919305 0.998084 0.114 Uiso 1 1 calc R U . . .
C32 C 0.2133(3) 0.6232(3) 0.5208(4) 0.0322(10) Uani 1 1 d . . . . .
H32A H 0.207348 0.622591 0.592755 0.039 Uiso 1 1 calc R U . . .
H32B H 0.161805 0.594779 0.491656 0.039 Uiso 1 1 calc R U . . .
C33 C 0.7029(3) 0.2592(3) 0.4861(4) 0.0352(11) Uani 1 1 d . . . . .
H33A H 0.732449 0.237727 0.456032 0.042 Uiso 1 1 calc R U . . .
H33B H 0.702507 0.251840 0.557779 0.042 Uiso 1 1 calc R U . . .
C34 C 1.0736(3) 1.1136(3) 0.5063(4) 0.0305(10) Uani 1 1 d . . . . .
H34A H 1.080274 1.118165 0.578259 0.037 Uiso 1 1 calc R U . . .
H34B H 1.098317 1.165655 0.478778 0.037 Uiso 1 1 calc R U . . .
C35 C 0.7723(3) 0.5074(3) 0.5464(4) 0.0329(11) Uani 1 1 d . . . . .
H35A H 0.810171 0.491631 0.560773 0.039 Uiso 1 1 calc R U . . .
H35B H 0.745858 0.505173 0.608323 0.039 Uiso 1 1 calc R U . . .
C36 C 0.8133(3) 0.5885(3) 0.5096(3) 0.0266(9) Uani 1 1 d . . . . .
C37 C 0.8131(3) 0.6381(3) 0.2129(4) 0.0355(11) Uani 1 1 d . . . . .
H37A H 0.758528 0.612830 0.230649 0.043 Uiso 1 1 calc R U . . .
H37B H 0.829705 0.599820 0.215175 0.043 Uiso 1 1 calc R U . . .
C38 C 0.4338(3) 0.4531(3) 0.5875(3) 0.0293(10) Uani 1 1 d . . . . .
C39 C 0.5071(2) 0.7949(3) 0.4355(3) 0.0283(10) Uani 1 1 d . . . . .
H39A H 0.492484 0.834101 0.424678 0.034 Uiso 1 1 calc R U . . .
H39B H 0.501920 0.768651 0.372472 0.034 Uiso 1 1 calc R U . . .
C40 C 0.6828(3) 0.8897(3) 0.5971(3) 0.0255(9) Uani 1 1 d . . . . .
C41 C 0.7432(3) 0.3451(3) 0.4643(4) 0.0291(10) Uani 1 1 d . . . . .
H41A H 0.792597 0.371675 0.498902 0.035 Uiso 1 1 calc R U . . .
H41B H 0.752731 0.354129 0.393106 0.035 Uiso 1 1 calc R U . . .
C42 C 0.4655(3) 0.4121(3) 0.5501(4) 0.0308(10) Uani 1 1 d . . . . .
H42 H 0.473234 0.379111 0.591785 0.037 Uiso 1 1 calc R U . . .
C43 C 0.8637(3) 0.8637(3) 0.4991(4) 0.0308(10) Uani 1 1 d . . . . .
H43A H 0.843570 0.840557 0.563931 0.037 Uiso 1 1 calc R U . . .
H43B H 0.827797 0.830529 0.448007 0.037 Uiso 1 1 calc R U . . .
C44 C 0.8236(2) 0.9499(3) 0.5621(3) 0.0264(9) Uani 1 1 d . . . . .
H44A H 0.840375 1.004652 0.568355 0.032 Uiso 1 1 calc R U . . .
H44B H 0.827826 0.931077 0.627328 0.032 Uiso 1 1 calc R U . . .
C45 C 0.8850(4) 0.6493(3) 0.8371(4) 0.0404(12) Uani 1 1 d . . . . .
H45 H 0.836007 0.628946 0.865918 0.049 Uiso 1 1 calc R U . . .
C46 C 0.3376(3) 0.7530(3) 0.5129(4) 0.0278(10) Uani 1 1 d . . . . .
H46A H 0.361914 0.803128 0.479945 0.033 Uiso 1 1 calc R U . . .
H46B H 0.342713 0.761430 0.584544 0.033 Uiso 1 1 calc R U . . .
C47 C 0.2526(3) 0.7066(3) 0.4844(4) 0.0315(11) Uani 1 1 d . . . . .
H47A H 0.248166 0.706721 0.412264 0.038 Uiso 1 1 calc R U . . .
H47B H 0.225723 0.731688 0.512210 0.038 Uiso 1 1 calc R U . . .
C48 C 0.8938(3) 0.7228(3) 0.5416(3) 0.0279(9) Uani 1 1 d . . . . .
H48 H 0.921061 0.763256 0.586591 0.034 Uiso 1 1 calc R U . . .
C49 C 0.8975(3) 0.6861(3) 0.7396(4) 0.0360(12) Uani 1 1 d . . . . .
H49A H 0.882179 0.725421 0.740703 0.043 Uiso 1 1 calc R U . . .
H49B H 0.951920 0.710712 0.721221 0.043 Uiso 1 1 calc R U . . .
C50 C 0.4862(3) 0.4184(3) 0.4519(3) 0.0256(9) Uani 1 1 d . . . . .
C51 C 0.5456(5) 0.5698(5) 0.0746(6) 0.069(2) Uani 1 1 d . . . . .
H51A H 0.565919 0.620359 0.098181 0.083 Uiso 1 1 calc R U . . .
H51B H 0.556742 0.561171 0.009883 0.083 Uiso 1 1 calc R U . . .
C52 C 0.9378(3) 0.8211(3) 0.4083(3) 0.0308(10) Uani 1 1 d . . . . .
H52A H 0.990627 0.834666 0.391638 0.037 Uiso 1 1 calc R U . . .
H52B H 0.913611 0.826788 0.348421 0.037 Uiso 1 1 calc R U . . .
C53 C 0.9367(4) 0.6432(3) 0.8854(5) 0.0532(17) Uani 1 1 d . . . . .
H53A H 0.986253 0.663011 0.858619 0.064 Uiso 1 1 calc R U . . .
H53B H 0.925024 0.618989 0.947573 0.064 Uiso 1 1 calc R U . . .
C54 C 0.3760(2) 0.7084(2) 0.4814(3) 0.0217(9) Uani 1 1 d . . . . .
H54 H 0.370374 0.700685 0.408856 0.026 Uiso 1 1 calc R U . . .
C55 C 0.6818(4) 0.8336(5) 0.2395(4) 0.0561(18) Uani 1 1 d . . . . .
H55A H 0.727976 0.884287 0.246213 0.067 Uiso 1 1 calc R U . . .
H55B H 0.662690 0.829158 0.171721 0.067 Uiso 1 1 calc R U . . .
C56 C 0.8539(3) 0.6483(3) 0.5758(3) 0.0273(10) Uani 1 1 d . . . . .
C57 C 0.3861(5) 0.3915(4) 0.9209(5) 0.066(2) Uani 1 1 d . . . . .
H57A H 0.432503 0.392198 0.933601 0.079 Uiso 1 1 calc R U . . .
H57B H 0.355428 0.390951 0.973766 0.079 Uiso 1 1 calc R U . . .
C58 C 0.3841(3) 0.5439(3) 0.5690(3) 0.0282(10) Uani 1 1 d . . . . .
H58A H 0.329345 0.507160 0.578763 0.034 Uiso 1 1 calc R U . . .
H58B H 0.406568 0.565076 0.633790 0.034 Uiso 1 1 calc R U . . .
C59 C 0.7692(6) 0.6657(5) 0.0567(5) 0.069(2) Uani 1 1 d . . . . .
H59A H 0.718239 0.639061 0.079975 0.083 Uiso 1 1 calc R U . . .
H59B H 0.779854 0.688018 -0.006652 0.083 Uiso 1 1 calc R U . . .
C60 C 0.5722(3) 0.2510(2) 0.4777(4) 0.0286(10) Uani 1 1 d . . . . .
H60A H 0.522346 0.224735 0.443940 0.034 Uiso 1 1 calc R U . . .
H60B H 0.563115 0.246357 0.549264 0.034 Uiso 1 1 calc R U . . .
C61 C 0.6721(5) 0.7134(5) 0.3196(7) 0.077(2) Uani 1 1 d . . . . .
H61A H 0.631340 0.706387 0.360779 0.092 Uiso 1 1 calc R U . . .
H61B H 0.690861 0.678930 0.323020 0.092 Uiso 1 1 calc R U . . .
C62 C 0.8943(3) 0.7390(2) 0.4425(3) 0.0247(9) Uani 1 1 d . . . . .
C64 C 0.5892(2) 0.8331(3) 0.4684(3) 0.0252(9) Uani 1 1 d . . . . .
C65 C 0.9885(3) 1.0735(2) 0.4829(3) 0.0248(9) Uani 1 1 d . . . . .
H65A H 0.964127 1.098267 0.518249 0.030 Uiso 1 1 calc R U . . .
H65B H 0.980680 1.076113 0.411739 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C63 1.800(11) . ?
Cl4 C63 1.751(10) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
Cl2 C2 1.798(13) . ?
Cl3 C2 1.783(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O1 C13 1.429(6) . ?
O1 C40 1.378(5) . ?
O2 C27 1.434(6) . ?
O2 C38 1.376(6) . ?
O3 C49 1.432(6) . ?
O3 C56 1.362(5) . ?
O4 C16 1.376(5) . ?
O4 C19 1.432(6) . ?
O5 C20 1.384(6) . ?
O5 C55 1.409(7) . ?
O6 C30 1.382(5) . ?
O6 C37 1.433(6) . ?
N1 C18 1.464(5) . ?
N1 C43 1.477(6) . ?
N1 C44 1.449(6) . ?
N2 C5 1.476(6) . ?
N2 C28 1.471(5) . ?
N2 C58 1.448(6) . ?
N3 C5 1.479(6) . ?
N3 C39 1.454(6) . ?
N3 C54 1.458(5) . ?
N4 C1 1.461(5) . ?
N4 C43 1.468(6) . ?
N4 C52 1.451(6) . ?
N5 C3 1.466(6) . ?
N5 C26 1.459(5) . ?
N5 C35 1.451(6) . ?
N6 C3 1.474(6) . ?
N6 C8 1.461(5) . ?
N6 C17 1.462(6) . ?
C1 H1 1.0000 . ?
C1 C10 1.519(6) . ?
C1 C18 1.516(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 0.9500 . ?
C4 C12 1.383(7) . ?
C4 C16 1.405(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 0.9500 . ?
C6 C30 1.398(6) . ?
C6 C36 1.382(7) . ?
C7 H7 0.9500 . ?
C7 C13 1.504(8) . ?
C7 C31 1.295(11) . ?
C8 H8 1.0000 . ?
C8 C26 1.496(6) . ?
C8 C60 1.529(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C28 1.517(6) . ?
C9 C32 1.524(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C21 1.541(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C33 1.532(8) . ?
C11 C60 1.545(6) . ?
C12 C38 1.402(6) . ?
C12 C58 1.507(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C22 1.378(6) . ?
C14 C40 1.398(6) . ?
C14 C44 1.516(6) . ?
C15 H15 0.9500 . ?
C15 C55 1.531(12) . ?
C15 C61 1.344(13) . ?
C16 C50 1.394(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C50 1.515(6) . ?
C18 H18 1.0000 . ?
C18 C65 1.515(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C25 1.488(7) . ?
C20 C22 1.383(6) . ?
C20 C64 1.403(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C34 1.537(7) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C37 1.498(7) . ?
C23 C59 1.317(10) . ?
C24 H24 0.9500 . ?
C24 C40 1.396(6) . ?
C24 C64 1.388(6) . ?
C25 H25 0.9500 . ?
C25 C51 1.301(10) . ?
C26 H26 1.0000 . ?
C26 C41 1.528(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C29 1.532(9) . ?
C28 H28 1.0000 . ?
C28 C54 1.510(6) . ?
C29 H29 0.9500 . ?
C29 C57 1.216(10) . ?
C30 C62 1.389(6) . ?
C31 H31A 0.9500 . ?
C31 H31B 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C47 1.548(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C41 1.538(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C65 1.530(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.511(6) . ?
C36 C56 1.403(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C42 1.380(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C64 1.511(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42 0.9500 . ?
C42 C50 1.391(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45 0.9500 . ?
C45 C49 1.486(7) . ?
C45 C53 1.296(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.545(6) . ?
C46 C54 1.521(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48 0.9500 . ?
C48 C56 1.391(6) . ?
C48 C62 1.391(6) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C51 H51A 0.9500 . ?
C51 H51B 0.9500 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C62 1.517(6) . ?
C53 H53A 0.9500 . ?
C53 H53B 0.9500 . ?
C54 H54 1.0000 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C57 H57A 0.9500 . ?
C57 H57B 0.9500 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9500 . ?
C59 H59B 0.9500 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9500 . ?
C61 H61B 0.9500 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 C63 H63A 109.6 . . ?
Cl1 C63 H63B 109.6 . . ?
Cl4 C63 Cl1 110.4(6) . . ?
Cl4 C63 H63A 109.6 . . ?
Cl4 C63 H63B 109.6 . . ?
H63A C63 H63B 108.1 . . ?
Cl2 C2 H2A 112.4 . . ?
Cl2 C2 H2B 112.4 . . ?
Cl3 C2 Cl2 96.9(12) . . ?
Cl3 C2 H2A 112.4 . . ?
Cl3 C2 H2B 112.4 . . ?
H2A C2 H2B 109.9 . . ?
C40 O1 C13 117.5(4) . . ?
C38 O2 C27 117.3(4) . . ?
C56 O3 C49 117.4(4) . . ?
C16 O4 C19 116.6(4) . . ?
C20 O5 C55 117.5(4) . . ?
C30 O6 C37 116.7(4) . . ?
C18 N1 C43 103.9(3) . . ?
C44 N1 C18 113.1(3) . . ?
C44 N1 C43 112.0(4) . . ?
C28 N2 C5 104.2(3) . . ?
C58 N2 C5 112.3(4) . . ?
C58 N2 C28 113.2(4) . . ?
C39 N3 C5 111.7(4) . . ?
C39 N3 C54 112.8(3) . . ?
C54 N3 C5 105.5(3) . . ?
C1 N4 C43 106.4(3) . . ?
C52 N4 C1 113.1(3) . . ?
C52 N4 C43 111.8(4) . . ?
C26 N5 C3 105.3(4) . . ?
C35 N5 C3 112.0(4) . . ?
C35 N5 C26 113.7(4) . . ?
C8 N6 C3 104.1(3) . . ?
C8 N6 C17 114.2(3) . . ?
C17 N6 C3 111.3(4) . . ?
N4 C1 H1 109.1 . . ?
N4 C1 C10 116.7(3) . . ?
N4 C1 C18 102.1(3) . . ?
C10 C1 H1 109.1 . . ?
C18 C1 H1 109.1 . . ?
C18 C1 C10 110.2(3) . . ?
N5 C3 N6 106.6(4) . . ?
N5 C3 H3A 110.4 . . ?
N5 C3 H3B 110.4 . . ?
N6 C3 H3A 110.4 . . ?
N6 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C12 C4 H4 119.5 . . ?
C12 C4 C16 121.0(4) . . ?
C16 C4 H4 119.5 . . ?
N2 C5 N3 106.8(3) . . ?
N2 C5 H5A 110.4 . . ?
N2 C5 H5B 110.4 . . ?
N3 C5 H5A 110.4 . . ?
N3 C5 H5B 110.4 . . ?
H5A C5 H5B 108.6 . . ?
C30 C6 H6 119.7 . . ?
C36 C6 H6 119.7 . . ?
C36 C6 C30 120.6(4) . . ?
C13 C7 H7 118.0 . . ?
C31 C7 H7 118.0 . . ?
C31 C7 C13 124.0(8) . . ?
N6 C8 H8 109.4 . . ?
N6 C8 C26 101.4(3) . . ?
N6 C8 C60 116.6(4) . . ?
C26 C8 H8 109.4 . . ?
C26 C8 C60 110.4(4) . . ?
C60 C8 H8 109.4 . . ?
H9A C9 H9B 108.4 . . ?
C28 C9 H9A 110.1 . . ?
C28 C9 H9B 110.1 . . ?
C28 C9 C32 108.0(4) . . ?
C32 C9 H9A 110.1 . . ?
C32 C9 H9B 110.1 . . ?
C1 C10 H10A 110.2 . . ?
C1 C10 H10B 110.2 . . ?
C1 C10 C21 107.8(3) . . ?
H10A C10 H10B 108.5 . . ?
C21 C10 H10A 110.2 . . ?
C21 C10 H10B 110.2 . . ?
H11A C11 H11B 107.7 . . ?
C33 C11 H11A 108.8 . . ?
C33 C11 H11B 108.8 . . ?
C33 C11 C60 113.7(4) . . ?
C60 C11 H11A 108.8 . . ?
C60 C11 H11B 108.8 . . ?
C4 C12 C38 118.6(4) . . ?
C4 C12 C58 121.7(4) . . ?
C38 C12 C58 119.6(4) . . ?
O1 C13 C7 107.6(4) . . ?
O1 C13 H13A 110.2 . . ?
O1 C13 H13B 110.2 . . ?
C7 C13 H13A 110.2 . . ?
C7 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
C22 C14 C40 119.2(4) . . ?
C22 C14 C44 120.6(4) . . ?
C40 C14 C44 120.2(4) . . ?
C55 C15 H15 115.8 . . ?
C61 C15 H15 115.8 . . ?
C61 C15 C55 128.4(7) . . ?
O4 C16 C4 122.8(4) . . ?
O4 C16 C50 117.5(4) . . ?
C50 C16 C4 119.6(4) . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
N6 C17 C50 110.9(4) . . ?
H17A C17 H17B 108.0 . . ?
C50 C17 H17A 109.5 . . ?
C50 C17 H17B 109.5 . . ?
N1 C18 C1 101.6(3) . . ?
N1 C18 H18 109.2 . . ?
N1 C18 C65 117.0(3) . . ?
C1 C18 H18 109.2 . . ?
C65 C18 C1 110.4(3) . . ?
C65 C18 H18 109.2 . . ?
O4 C19 H19A 110.1 . . ?
O4 C19 H19B 110.1 . . ?
O4 C19 C25 108.1(4) . . ?
H19A C19 H19B 108.4 . . ?
C25 C19 H19A 110.1 . . ?
C25 C19 H19B 110.1 . . ?
O5 C20 C64 116.3(4) . . ?
C22 C20 O5 123.9(4) . . ?
C22 C20 C64 119.8(4) . . ?
C10 C21 H21A 108.7 . . ?
C10 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C34 C21 C10 114.2(4) . . ?
C34 C21 H21A 108.7 . . ?
C34 C21 H21B 108.7 . . ?
C14 C22 C20 121.4(4) . . ?
C14 C22 H22 119.3 . . ?
C20 C22 H22 119.3 . . ?
C37 C23 H23 118.3 . . ?
C59 C23 H23 118.3 . . ?
C59 C23 C37 123.4(7) . . ?
C40 C24 H24 119.8 . . ?
C64 C24 H24 119.8 . . ?
C64 C24 C40 120.4(4) . . ?
C19 C25 H25 118.2 . . ?
C51 C25 C19 123.6(7) . . ?
C51 C25 H25 118.2 . . ?
N5 C26 C8 101.9(3) . . ?
N5 C26 H26 109.4 . . ?
N5 C26 C41 115.7(4) . . ?
C8 C26 H26 109.4 . . ?
C8 C26 C41 110.8(4) . . ?
C41 C26 H26 109.4 . . ?
O2 C27 H27A 110.6 . . ?
O2 C27 H27B 110.6 . . ?
O2 C27 C29 105.6(5) . . ?
H27A C27 H27B 108.7 . . ?
C29 C27 H27A 110.6 . . ?
C29 C27 H27B 110.6 . . ?
N2 C28 C9 116.7(4) . . ?
N2 C28 H28 109.3 . . ?
N2 C28 C54 101.1(3) . . ?
C9 C28 H28 109.3 . . ?
C54 C28 C9 110.8(4) . . ?
C54 C28 H28 109.3 . . ?
C27 C29 H29 117.0 . . ?
C57 C29 C27 125.9(8) . . ?
C57 C29 H29 117.0 . . ?
O6 C30 C6 123.2(4) . . ?
O6 C30 C62 116.6(4) . . ?
C62 C30 C6 120.3(4) . . ?
C7 C31 H31A 120.0 . . ?
C7 C31 H31B 120.0 . . ?
H31A C31 H31B 120.0 . . ?
C9 C32 H32A 108.9 . . ?
C9 C32 H32B 108.9 . . ?
C9 C32 C47 113.3(4) . . ?
H32A C32 H32B 107.7 . . ?
C47 C32 H32A 108.9 . . ?
C47 C32 H32B 108.9 . . ?
C11 C33 H33A 108.8 . . ?
C11 C33 H33B 108.8 . . ?
C11 C33 C41 113.6(4) . . ?
H33A C33 H33B 107.7 . . ?
C41 C33 H33A 108.8 . . ?
C41 C33 H33B 108.8 . . ?
C21 C34 H34A 108.8 . . ?
C21 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C65 C34 C21 113.7(4) . . ?
C65 C34 H34A 108.8 . . ?
C65 C34 H34B 108.8 . . ?
N5 C35 H35A 109.0 . . ?
N5 C35 H35B 109.0 . . ?
N5 C35 C36 113.1(4) . . ?
H35A C35 H35B 107.8 . . ?
C36 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C6 C36 C35 121.0(4) . . ?
C6 C36 C56 119.4(4) . . ?
C56 C36 C35 119.5(4) . . ?
O6 C37 C23 107.7(4) . . ?
O6 C37 H37A 110.2 . . ?
O6 C37 H37B 110.2 . . ?
C23 C37 H37A 110.2 . . ?
C23 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
O2 C38 C12 114.2(4) . . ?
O2 C38 C42 125.1(4) . . ?
C42 C38 C12 120.7(4) . . ?
N3 C39 H39A 109.2 . . ?
N3 C39 H39B 109.2 . . ?
N3 C39 C64 112.0(4) . . ?
H39A C39 H39B 107.9 . . ?
C64 C39 H39A 109.2 . . ?
C64 C39 H39B 109.2 . . ?
O1 C40 C14 115.3(4) . . ?
O1 C40 C24 124.7(4) . . ?
C24 C40 C14 120.0(4) . . ?
C26 C41 C33 107.8(4) . . ?
C26 C41 H41A 110.2 . . ?
C26 C41 H41B 110.2 . . ?
C33 C41 H41A 110.2 . . ?
C33 C41 H41B 110.2 . . ?
H41A C41 H41B 108.5 . . ?
C38 C42 H42 119.6 . . ?
C38 C42 C50 120.8(4) . . ?
C50 C42 H42 119.6 . . ?
N1 C43 H43A 110.4 . . ?
N1 C43 H43B 110.4 . . ?
N4 C43 N1 106.7(3) . . ?
N4 C43 H43A 110.4 . . ?
N4 C43 H43B 110.4 . . ?
H43A C43 H43B 108.6 . . ?
N1 C44 C14 112.2(4) . . ?
N1 C44 H44A 109.2 . . ?
N1 C44 H44B 109.2 . . ?
C14 C44 H44A 109.2 . . ?
C14 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C49 C45 H45 117.9 . . ?
C53 C45 H45 117.9 . . ?
C53 C45 C49 124.1(6) . . ?
H46A C46 H46B 108.4 . . ?
C47 C46 H46A 110.0 . . ?
C47 C46 H46B 110.0 . . ?
C54 C46 H46A 110.0 . . ?
C54 C46 H46B 110.0 . . ?
C54 C46 C47 108.3(4) . . ?
C32 C47 H47A 108.9 . . ?
C32 C47 H47B 108.9 . . ?
C46 C47 C32 113.2(4) . . ?
C46 C47 H47A 108.9 . . ?
C46 C47 H47B 108.9 . . ?
H47A C47 H47B 107.8 . . ?
C56 C48 H48 119.5 . . ?
C56 C48 C62 121.0(4) . . ?
C62 C48 H48 119.5 . . ?
O3 C49 C45 107.0(4) . . ?
O3 C49 H49A 110.3 . . ?
O3 C49 H49B 110.3 . . ?
C45 C49 H49A 110.3 . . ?
C45 C49 H49B 110.3 . . ?
H49A C49 H49B 108.6 . . ?
C16 C50 C17 121.2(4) . . ?
C42 C50 C16 119.3(4) . . ?
C42 C50 C17 119.5(4) . . ?
C25 C51 H51A 120.0 . . ?
C25 C51 H51B 120.0 . . ?
H51A C51 H51B 120.0 . . ?
N4 C52 H52A 109.4 . . ?
N4 C52 H52B 109.4 . . ?
N4 C52 C62 111.3(4) . . ?
H52A C52 H52B 108.0 . . ?
C62 C52 H52A 109.4 . . ?
C62 C52 H52B 109.4 . . ?
C45 C53 H53A 120.0 . . ?
C45 C53 H53B 120.0 . . ?
H53A C53 H53B 120.0 . . ?
N3 C54 C28 103.0(3) . . ?
N3 C54 C46 117.2(4) . . ?
N3 C54 H54 108.7 . . ?
C28 C54 C46 110.1(4) . . ?
C28 C54 H54 108.7 . . ?
C46 C54 H54 108.7 . . ?
O5 C55 C15 112.9(6) . . ?
O5 C55 H55A 109.0 . . ?
O5 C55 H55B 109.0 . . ?
C15 C55 H55A 109.0 . . ?
C15 C55 H55B 109.0 . . ?
H55A C55 H55B 107.8 . . ?
O3 C56 C36 115.6(4) . . ?
O3 C56 C48 124.7(4) . . ?
C48 C56 C36 119.7(4) . . ?
C29 C57 H57A 120.0 . . ?
C29 C57 H57B 120.0 . . ?
H57A C57 H57B 120.0 . . ?
N2 C58 C12 112.8(4) . . ?
N2 C58 H58A 109.0 . . ?
N2 C58 H58B 109.0 . . ?
C12 C58 H58A 109.0 . . ?
C12 C58 H58B 109.0 . . ?
H58A C58 H58B 107.8 . . ?
C23 C59 H59A 120.0 . . ?
C23 C59 H59B 120.0 . . ?
H59A C59 H59B 120.0 . . ?
C8 C60 C11 107.3(4) . . ?
C8 C60 H60A 110.3 . . ?
C8 C60 H60B 110.3 . . ?
C11 C60 H60A 110.3 . . ?
C11 C60 H60B 110.3 . . ?
H60A C60 H60B 108.5 . . ?
C15 C61 H61A 120.0 . . ?
C15 C61 H61B 120.0 . . ?
H61A C61 H61B 120.0 . . ?
C30 C62 C48 119.1(4) . . ?
C30 C62 C52 121.5(4) . . ?
C48 C62 C52 119.4(4) . . ?
C20 C64 C39 120.9(4) . . ?
C24 C64 C20 119.3(4) . . ?
C24 C64 C39 119.8(4) . . ?
C18 C65 C34 107.5(4) . . ?
C18 C65 H65A 110.2 . . ?
C18 C65 H65B 110.2 . . ?
C34 C65 H65A 110.2 . . ?
C34 C65 H65B 110.2 . . ?
H65A C65 H65B 108.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C27 C29 C57 -132.3(8) . . . . ?
O2 C38 C42 C50 179.4(5) . . . . ?
O4 C16 C50 C17 0.7(7) . . . . ?
O4 C16 C50 C42 179.7(4) . . . . ?
O4 C19 C25 C51 -130.3(7) . . . . ?
O5 C20 C22 C14 -179.7(4) . . . . ?
O5 C20 C64 C24 178.8(4) . . . . ?
O5 C20 C64 C39 -1.8(6) . . . . ?
O6 C30 C62 C48 -179.3(4) . . . . ?
O6 C30 C62 C52 1.4(7) . . . . ?
N1 C18 C65 C34 -176.4(4) . . . . ?
N2 C28 C54 N3 -43.7(4) . . . . ?
N2 C28 C54 C46 -169.4(3) . . . . ?
N3 C39 C64 C20 142.4(4) . . . . ?
N3 C39 C64 C24 -38.2(6) . . . . ?
N4 C1 C10 C21 -174.8(4) . . . . ?
N4 C1 C18 N1 -43.1(4) . . . . ?
N4 C1 C18 C65 -167.9(3) . . . . ?
N4 C52 C62 C30 148.7(4) . . . . ?
N4 C52 C62 C48 -30.6(6) . . . . ?
N5 C26 C41 C33 -174.9(4) . . . . ?
N5 C35 C36 C6 -17.6(7) . . . . ?
N5 C35 C36 C56 164.5(4) . . . . ?
N6 C8 C26 N5 -45.3(4) . . . . ?
N6 C8 C26 C41 -169.0(4) . . . . ?
N6 C8 C60 C11 -175.2(4) . . . . ?
N6 C17 C50 C16 129.9(5) . . . . ?
N6 C17 C50 C42 -49.1(6) . . . . ?
C1 N4 C43 N1 -5.5(5) . . . . ?
C1 N4 C52 C62 171.2(4) . . . . ?
C1 C10 C21 C34 50.3(5) . . . . ?
C1 C18 C65 C34 -60.9(4) . . . . ?
C3 N5 C26 C8 34.0(5) . . . . ?
C3 N5 C26 C41 154.3(4) . . . . ?
C3 N5 C35 C36 -75.5(5) . . . . ?
C3 N6 C8 C26 39.0(5) . . . . ?
C3 N6 C8 C60 158.9(4) . . . . ?
C3 N6 C17 C50 -66.6(5) . . . . ?
C4 C12 C38 O2 179.7(4) . . . . ?
C4 C12 C38 C42 -0.6(7) . . . . ?
C4 C12 C58 N2 -15.8(6) . . . . ?
C4 C16 C50 C17 -179.3(4) . . . . ?
C4 C16 C50 C42 -0.2(7) . . . . ?
C5 N2 C28 C9 159.4(4) . . . . ?
C5 N2 C28 C54 39.2(4) . . . . ?
C5 N2 C58 C12 -78.7(5) . . . . ?
C5 N3 C39 C64 -67.4(5) . . . . ?
C5 N3 C54 C28 31.0(5) . . . . ?
C5 N3 C54 C46 152.1(4) . . . . ?
C6 C30 C62 C48 0.4(7) . . . . ?
C6 C30 C62 C52 -178.9(4) . . . . ?
C6 C36 C56 O3 -179.0(4) . . . . ?
C6 C36 C56 C48 0.0(7) . . . . ?
C8 N6 C3 N5 -18.4(5) . . . . ?
C8 N6 C17 C50 175.8(4) . . . . ?
C8 C26 C41 C33 -59.6(5) . . . . ?
C9 C28 C54 N3 -168.1(4) . . . . ?
C9 C28 C54 C46 66.2(5) . . . . ?
C9 C32 C47 C46 -50.0(6) . . . . ?
C10 C1 C18 N1 -167.8(3) . . . . ?
C10 C1 C18 C65 67.4(4) . . . . ?
C10 C21 C34 C65 -48.9(5) . . . . ?
C11 C33 C41 C26 51.2(6) . . . . ?
C12 C4 C16 O4 179.4(4) . . . . ?
C12 C4 C16 C50 -0.7(7) . . . . ?
C12 C38 C42 C50 -0.3(8) . . . . ?
C13 O1 C40 C14 179.4(5) . . . . ?
C13 O1 C40 C24 -0.4(7) . . . . ?
C16 O4 C19 C25 -174.6(5) . . . . ?
C16 C4 C12 C38 1.1(7) . . . . ?
C16 C4 C12 C58 -176.7(4) . . . . ?
C17 N6 C3 N5 -142.0(4) . . . . ?
C17 N6 C8 C26 160.7(4) . . . . ?
C17 N6 C8 C60 -79.5(5) . . . . ?
C18 N1 C43 N4 -22.0(5) . . . . ?
C18 N1 C44 C14 170.3(4) . . . . ?
C18 C1 C10 C21 -58.9(4) . . . . ?
C19 O4 C16 C4 -2.8(6) . . . . ?
C19 O4 C16 C50 177.2(4) . . . . ?
C20 O5 C55 C15 72.9(7) . . . . ?
C21 C34 C65 C18 51.9(5) . . . . ?
C22 C14 C40 O1 -179.7(4) . . . . ?
C22 C14 C40 C24 0.2(7) . . . . ?
C22 C14 C44 N1 -21.3(6) . . . . ?
C22 C20 C64 C24 -1.1(7) . . . . ?
C22 C20 C64 C39 178.3(4) . . . . ?
C26 N5 C3 N6 -10.2(6) . . . . ?
C26 N5 C35 C36 165.3(4) . . . . ?
C26 C8 C60 C11 -60.3(5) . . . . ?
C27 O2 C38 C12 170.2(5) . . . . ?
C27 O2 C38 C42 -9.5(8) . . . . ?
C28 N2 C5 N3 -20.8(5) . . . . ?
C28 N2 C58 C12 163.7(4) . . . . ?
C28 C9 C32 C47 52.5(5) . . . . ?
C30 O6 C37 C23 -179.9(4) . . . . ?
C30 C6 C36 C35 -177.3(4) . . . . ?
C30 C6 C36 C56 0.6(7) . . . . ?
C31 C7 C13 O1 -126.7(8) . . . . ?
C32 C9 C28 N2 -175.6(4) . . . . ?
C32 C9 C28 C54 -60.7(5) . . . . ?
C33 C11 C60 C8 52.1(6) . . . . ?
C35 N5 C3 N6 -134.2(4) . . . . ?
C35 N5 C26 C8 157.0(4) . . . . ?
C35 N5 C26 C41 -82.8(5) . . . . ?
C35 C36 C56 O3 -1.0(7) . . . . ?
C35 C36 C56 C48 177.9(5) . . . . ?
C36 C6 C30 O6 178.9(4) . . . . ?
C36 C6 C30 C62 -0.7(7) . . . . ?
C37 O6 C30 C6 3.0(7) . . . . ?
C37 O6 C30 C62 -177.4(4) . . . . ?
C38 O2 C27 C29 -168.0(6) . . . . ?
C38 C12 C58 N2 166.5(4) . . . . ?
C38 C42 C50 C16 0.7(7) . . . . ?
C38 C42 C50 C17 179.8(5) . . . . ?
C39 N3 C5 N2 -129.7(4) . . . . ?
C39 N3 C54 C28 153.2(4) . . . . ?
C39 N3 C54 C46 -85.8(5) . . . . ?
C40 O1 C13 C7 -175.8(5) . . . . ?
C40 C14 C22 C20 0.3(7) . . . . ?
C40 C14 C44 N1 160.5(4) . . . . ?
C40 C24 C64 C20 1.6(7) . . . . ?
C40 C24 C64 C39 -177.8(4) . . . . ?
C43 N1 C18 C1 39.8(4) . . . . ?
C43 N1 C18 C65 160.0(4) . . . . ?
C43 N1 C44 C14 -72.8(5) . . . . ?
C43 N4 C1 C10 150.0(4) . . . . ?
C43 N4 C1 C18 29.7(4) . . . . ?
C43 N4 C52 C62 -68.7(5) . . . . ?
C44 N1 C18 C1 161.4(3) . . . . ?
C44 N1 C18 C65 -78.4(5) . . . . ?
C44 N1 C43 N4 -144.3(4) . . . . ?
C44 C14 C22 C20 -177.9(4) . . . . ?
C44 C14 C40 O1 -1.4(6) . . . . ?
C44 C14 C40 C24 178.4(4) . . . . ?
C47 C46 C54 N3 -176.3(4) . . . . ?
C47 C46 C54 C28 -59.0(5) . . . . ?
C49 O3 C56 C36 175.2(4) . . . . ?
C49 O3 C56 C48 -3.6(7) . . . . ?
C52 N4 C1 C10 -86.9(5) . . . . ?
C52 N4 C1 C18 152.8(4) . . . . ?
C52 N4 C43 N1 -129.5(4) . . . . ?
C53 C45 C49 O3 112.8(6) . . . . ?
C54 N3 C5 N2 -6.8(5) . . . . ?
C54 N3 C39 C64 174.0(4) . . . . ?
C54 C46 C47 C32 51.3(5) . . . . ?
C55 O5 C20 C22 10.0(8) . . . . ?
C55 O5 C20 C64 -169.8(5) . . . . ?
C56 O3 C49 C45 179.5(5) . . . . ?
C56 C48 C62 C30 0.2(7) . . . . ?
C56 C48 C62 C52 179.5(4) . . . . ?
C58 N2 C5 N3 -143.7(4) . . . . ?
C58 N2 C28 C9 -78.3(5) . . . . ?
C58 N2 C28 C54 161.4(4) . . . . ?
C58 C12 C38 O2 -2.5(7) . . . . ?
C58 C12 C38 C42 177.2(5) . . . . ?
C59 C23 C37 O6 -121.5(7) . . . . ?
C60 C8 C26 N5 -169.4(3) . . . . ?
C60 C8 C26 C41 66.9(5) . . . . ?
C60 C11 C33 C41 -50.0(6) . . . . ?
C61 C15 C55 O5 5.1(10) . . . . ?
C62 C48 C56 O3 178.5(4) . . . . ?
C62 C48 C56 C36 -0.3(7) . . . . ?
C64 C20 C22 C14 0.1(7) . . . . ?
C64 C24 C40 O1 178.7(4) . . . . ?
C64 C24 C40 C14 -1.2(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9658(12)
2 0.0342(12)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-He@P-TA
_database_code_depnum_ccdc_archive 'CCDC 2120030'
loop_
_audit_author_name
_audit_author_address
yanjun.ding
;KAUST
Saudi Arabia
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_audit_creation_date             2021-10-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C63 H84 N6 O6, 1(C6 H12)'
_chemical_formula_sum            'C69 H96 N6 O6'
_chemical_formula_weight         1105.51
_chemical_absolute_configuration rm
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   20.366
_cell_length_b                   20.366
_cell_length_c                   13.791
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4953.9
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      65.024
_cell_measurement_theta_min      4.344
_shelx_estimated_absorpt_T_max   0.947
_shelx_estimated_absorpt_T_min   0.937
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0939 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.9041.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16121
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        64.963
_diffrn_reflns_theta_max         64.963
_diffrn_reflns_theta_min         4.342
_diffrn_ambient_temperature      120.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3721
_reflns_number_total             3722
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3722
_refine_ls_number_restraints     1049
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.163
_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/[σ²(Fo²)+(0.0731P)²+2.0170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1073
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.880(2)
 0.120(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C13-C25 = C25-C3
 1.54 with sigma of 0.005
 C11-C23 = C23-C3
 1.54 with sigma of 0.005
 C23-C3 = C3-C25
 1.54 with sigma of 0.005
 C11-C21
 1.32 with sigma of 0.005
 C13-C3
 2.515 with sigma of 0.005
 C11-C3
 2.515 with sigma of 0.005
 C23-C25
 2.515 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10
\\sim C12 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20
\\sim C22 \\sim C24 \\sim C26 \\sim C27 \\sim C3 \\sim C11 \\sim C13 \\sim C21
\\sim C23 \\sim C25 \\sim N1 \\sim N2: within 5A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 5A
5. Others
 Fixed Sof: C3(0.33333) H3A(0.33333) H3B(0.33333) C11(0.33333) H11(0.33333)
 C13(0.33333) H13A(0.33333) H13B(0.33333) H13C(0.33333) C21(0.33333)
 H21A(0.33333) H21B(0.33333) C23(0.33333) H23A(0.33333) H23B(0.33333)
 C25(0.33333) H25A(0.33333) H25B(0.33333)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C8(H8)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C3(H3A,H3B),
 C23(H23A,H23B), C25(H25A,H25B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C19(H19), C24(H24), C11(H11)
6.d X=CH2 refined with riding coordinates:
 C5(H5A,H5B), C17(H17A,H17B), C21(H21A,H21B)
6.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.56148(14) 0.70151(12) 0.30652(15) 0.0389(5) Uani 1 1 d . . . . .
O2 O 0.50556(13) 0.63506(12) 0.69752(15) 0.0383(5) Uani 1 1 d . . . . .
N1 N 0.54019(14) 0.94491(14) 0.50348(17) 0.0285(5) Uani 1 1 d . U . . .
N2 N 0.60466(13) 0.87528(13) 0.49831(18) 0.0293(5) Uani 1 1 d . U . . .
C1 C 0.48866(17) 0.95067(18) 0.5717(2) 0.0352(7) Uani 1 1 d . U . . .
H1A H 0.503576 1.004643 0.580118 0.042 Uiso 1 1 calc R U . . .
H1B H 0.492569 0.930676 0.635534 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5660(2) 0.6776(2) 0.1403(3) 0.0493(8) Uani 1 1 d . U . . .
H2 H 0.535487 0.696757 0.115059 0.059 Uiso 1 1 calc R U . . .
C4 C 0.52917(18) 0.86775(17) 0.5002(3) 0.0410(7) Uani 1 1 d . U . . .
H4A H 0.500692 0.838599 0.558044 0.049 Uiso 1 1 calc R U . . .
H4B H 0.500193 0.840823 0.441565 0.049 Uiso 1 1 calc R U . . .
C5 C 0.4518(3) 0.6780(3) 0.9134(3) 0.0737(13) Uani 1 1 d . U . . .
H5A H 0.432056 0.707993 0.887956 0.088 Uiso 1 1 calc R U . . .
H5B H 0.437627 0.656836 0.976492 0.088 Uiso 1 1 calc R U . . .
C6 C 0.62040(15) 0.99408(16) 0.5276(2) 0.0278(6) Uani 1 1 d . U . . .
H6 H 0.627191 0.991569 0.599052 0.033 Uiso 1 1 calc R U . . .
C7 C 0.55515(17) 0.72689(17) 0.5651(2) 0.0312(6) Uani 1 1 d . U . . .
H7 H 0.569937 0.767728 0.609252 0.037 Uiso 1 1 calc R U . . .
C8 C 0.65666(16) 0.95480(16) 0.4755(2) 0.0286(6) Uani 1 1 d . U . . .
H8 H 0.655350 0.962541 0.404052 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5237(2) 0.6967(2) 0.7624(2) 0.0440(7) Uani 1 1 d . U . . .
H9A H 0.497632 0.724326 0.741689 0.053 Uiso 1 1 calc R U . . .
H9B H 0.579061 0.732539 0.761777 0.053 Uiso 1 1 calc R U . . .
C10 C 0.73873(16) 0.98747(18) 0.5074(2) 0.0344(6) Uani 1 1 d . U . . .
H10A H 0.762237 0.961855 0.472684 0.041 Uiso 1 1 calc R U . . .
H10B H 0.741091 0.979752 0.577897 0.041 Uiso 1 1 calc R U . . .
C12 C 0.78109(18) 1.07257(19) 0.4836(2) 0.0396(7) Uani 1 1 d . U . . .
H12A H 0.832757 1.095917 0.511396 0.047 Uiso 1 1 calc R U . . .
H12B H 0.786281 1.078864 0.412328 0.047 Uiso 1 1 calc R U . . .
C14 C 0.74226(19) 1.11493(17) 0.5218(2) 0.0394(7) Uani 1 1 d . U . . .
H14A H 0.768156 1.166814 0.494393 0.047 Uiso 1 1 calc R U . . .
H14B H 0.748335 1.119565 0.593120 0.047 Uiso 1 1 calc R U . . .
C15 C 0.5470(2) 0.64231(19) 0.2390(2) 0.0453(8) Uani 1 1 d . U . . .
H15A H 0.492999 0.602079 0.241834 0.054 Uiso 1 1 calc R U . . .
H15B H 0.578718 0.619490 0.254375 0.054 Uiso 1 1 calc R U . . .
C16 C 0.65707(18) 1.07654(17) 0.4973(2) 0.0338(6) Uani 1 1 d . U . . .
H16A H 0.633500 1.101897 0.532434 0.041 Uiso 1 1 calc R U . . .
H16B H 0.650106 1.080184 0.426838 0.041 Uiso 1 1 calc R U . . .
C17 C 0.6205(3) 0.6837(2) 0.0877(3) 0.0618(11) Uani 1 1 d . U . . .
H17A H 0.652082 0.665073 0.110763 0.074 Uiso 1 1 calc R U . . .
H17B H 0.629304 0.706749 0.025641 0.074 Uiso 1 1 calc R U . . .
C18 C 0.60879(18) 0.82269(18) 0.4304(2) 0.0345(6) Uani 1 1 d . U . . .
H18A H 0.662675 0.838663 0.418451 0.041 Uiso 1 1 calc R U . . .
H18B H 0.586119 0.824920 0.367813 0.041 Uiso 1 1 calc R U . . .
C19 C 0.4990(3) 0.6658(2) 0.8609(3) 0.0546(9) Uani 1 1 d . U . . .
H19 H 0.517950 0.635631 0.887982 0.066 Uiso 1 1 calc R U . . .
C20 C 0.56818(16) 0.74200(17) 0.4670(2) 0.0297(6) Uani 1 1 d . U . . .
C22 C 0.54629(17) 0.68177(17) 0.4026(2) 0.0319(6) Uani 1 1 d . U . . .
C24 C 0.51241(17) 0.60806(17) 0.4375(2) 0.0334(6) Uani 1 1 d . U . . .
H24 H 0.497840 0.567359 0.393213 0.040 Uiso 1 1 calc R U . . .
C26 C 0.49933(16) 0.59259(17) 0.5364(2) 0.0321(6) Uani 1 1 d . U . . .
C27 C 0.52091(17) 0.65326(17) 0.6002(2) 0.0309(6) Uani 1 1 d . U . . .
C3 C 0.3578(4) 0.6739(11) 0.4623(6) 0.059(3) Uani 0.3333 1 d D U P A -1
H3A H 0.391837 0.652300 0.464671 0.071 Uiso 0.3333 1 calc R U P A -1
H3B H 0.389596 0.729818 0.463796 0.071 Uiso 0.3333 1 calc R U P A -1
C11 C 0.3631(8) 0.6956(9) 0.2826(7) 0.080(3) Uani 0.3333 1 d D U P A -1
H11 H 0.411302 0.729862 0.309443 0.096 Uiso 0.3333 1 calc R U P A -1
C13 C 0.3518(11) 0.6845(13) 0.6427(7) 0.080(4) Uani 0.3333 1 d D U P A -1
H13A H 0.400447 0.728614 0.624653 0.120 Uiso 0.3333 1 calc R U P A -1
H13B H 0.360968 0.647914 0.677681 0.120 Uiso 0.3333 1 calc R U P A -1
H13C H 0.323595 0.700689 0.684358 0.120 Uiso 0.3333 1 calc R U P A -1
C21 C 0.3686(16) 0.7080(14) 0.1887(8) 0.120(6) Uani 0.3333 1 d D U P A -1
H21A H 0.325985 0.679174 0.148000 0.144 Uiso 0.3333 1 calc R U P A -1
H21B H 0.415182 0.745640 0.161406 0.144 Uiso 0.3333 1 calc R U P A -1
C23 C 0.3121(6) 0.6496(11) 0.3678(6) 0.067(3) Uani 0.3333 1 d D U P A -1
H23A H 0.268421 0.658131 0.372762 0.080 Uiso 0.3333 1 calc R U P A -1
H23B H 0.292204 0.594808 0.356471 0.080 Uiso 0.3333 1 calc R U P A -1
C25 C 0.3055(6) 0.6471(9) 0.5506(6) 0.070(3) Uani 0.3333 1 d D U P A -1
H25A H 0.280692 0.591229 0.556274 0.083 Uiso 0.3333 1 calc R U P A -1
H25B H 0.265476 0.660735 0.542813 0.083 Uiso 0.3333 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.433(4) . ?
O1 C22 1.375(3) . ?
O2 C9 1.431(4) . ?
O2 C27 1.385(3) . ?
N1 C1 1.457(4) . ?
N1 C4 1.473(4) . ?
N1 C6 1.465(4) . ?
N2 C4 1.467(4) . ?
N2 C8 1.459(4) . ?
N2 C18 1.457(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C26 1.515(4) 2_665 ?
C2 H2 0.9500 . ?
C2 C15 1.496(5) . ?
C2 C17 1.279(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9500 . ?
C5 H5B 0.9500 . ?
C5 C19 1.323(7) . ?
C6 H6 1.0000 . ?
C6 C8 1.514(4) . ?
C6 C16 1.516(4) . ?
C7 H7 0.9500 . ?
C7 C20 1.384(4) . ?
C7 C27 1.387(4) . ?
C8 H8 1.0000 . ?
C8 C10 1.523(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C19 1.476(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C12 1.536(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C14 1.526(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C16 1.542(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9500 . ?
C17 H17B 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C20 1.510(4) . ?
C19 H19 0.9500 . ?
C20 C22 1.394(4) . ?
C22 C24 1.388(4) . ?
C24 H24 0.9500 . ?
C24 C26 1.395(4) . ?
C26 C27 1.398(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C23 1.533(5) . ?
C3 C25 1.528(5) . ?
C11 H11 0.9500 . ?
C11 C21 1.314(7) . ?
C11 C23 1.538(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C25 1.538(7) . ?
C21 H21A 0.9500 . ?
C21 H21B 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 O1 C15 117.3(2) . . ?
C27 O2 C9 116.5(2) . . ?
C1 N1 C4 112.0(3) . . ?
C1 N1 C6 113.6(2) . . ?
C6 N1 C4 105.0(2) . . ?
C8 N2 C4 105.1(2) . . ?
C18 N2 C4 112.2(2) . . ?
C18 N2 C8 113.6(2) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C26 111.3(2) . 2_665 ?
H1A C1 H1B 108.0 . . ?
C26 C1 H1A 109.4 2_665 . ?
C26 C1 H1B 109.4 2_665 . ?
C15 C2 H2 117.8 . . ?
C17 C2 H2 117.8 . . ?
C17 C2 C15 124.5(4) . . ?
N1 C4 H4A 110.3 . . ?
N1 C4 H4B 110.3 . . ?
N2 C4 N1 107.2(2) . . ?
N2 C4 H4A 110.3 . . ?
N2 C4 H4B 110.3 . . ?
H4A C4 H4B 108.5 . . ?
H5A C5 H5B 120.0 . . ?
C19 C5 H5A 120.0 . . ?
C19 C5 H5B 120.0 . . ?
N1 C6 H6 108.9 . . ?
N1 C6 C8 101.7(2) . . ?
N1 C6 C16 117.3(2) . . ?
C8 C6 H6 108.9 . . ?
C8 C6 C16 110.7(2) . . ?
C16 C6 H6 108.9 . . ?
C20 C7 H7 119.4 . . ?
C20 C7 C27 121.2(3) . . ?
C27 C7 H7 119.4 . . ?
N2 C8 C6 102.1(2) . . ?
N2 C8 H8 109.0 . . ?
N2 C8 C10 116.8(2) . . ?
C6 C8 H8 109.0 . . ?
C6 C8 C10 110.5(2) . . ?
C10 C8 H8 109.0 . . ?
O2 C9 H9A 110.0 . . ?
O2 C9 H9B 110.0 . . ?
O2 C9 C19 108.5(3) . . ?
H9A C9 H9B 108.4 . . ?
C19 C9 H9A 110.0 . . ?
C19 C9 H9B 110.0 . . ?
C8 C10 H10A 110.1 . . ?
C8 C10 H10B 110.1 . . ?
C8 C10 C12 107.8(2) . . ?
H10A C10 H10B 108.5 . . ?
C12 C10 H10A 110.1 . . ?
C12 C10 H10B 110.1 . . ?
C10 C12 H12A 108.8 . . ?
C10 C12 H12B 108.8 . . ?
H12A C12 H12B 107.6 . . ?
C14 C12 C10 114.0(3) . . ?
C14 C12 H12A 108.8 . . ?
C14 C12 H12B 108.8 . . ?
C12 C14 H14A 108.7 . . ?
C12 C14 H14B 108.7 . . ?
C12 C14 C16 114.0(3) . . ?
H14A C14 H14B 107.6 . . ?
C16 C14 H14A 108.7 . . ?
C16 C14 H14B 108.7 . . ?
O1 C15 C2 107.0(3) . . ?
O1 C15 H15A 110.3 . . ?
O1 C15 H15B 110.3 . . ?
C2 C15 H15A 110.3 . . ?
C2 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C6 C16 C14 107.9(2) . . ?
C6 C16 H16A 110.1 . . ?
C6 C16 H16B 110.1 . . ?
C14 C16 H16A 110.1 . . ?
C14 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
C2 C17 H17A 120.0 . . ?
C2 C17 H17B 120.0 . . ?
H17A C17 H17B 120.0 . . ?
N2 C18 H18A 109.1 . . ?
N2 C18 H18B 109.1 . . ?
N2 C18 C20 112.5(2) . . ?
H18A C18 H18B 107.8 . . ?
C20 C18 H18A 109.1 . . ?
C20 C18 H18B 109.1 . . ?
C5 C19 C9 123.3(5) . . ?
C5 C19 H19 118.4 . . ?
C9 C19 H19 118.4 . . ?
C7 C20 C18 120.6(3) . . ?
C7 C20 C22 119.0(3) . . ?
C22 C20 C18 120.3(2) . . ?
O1 C22 C20 115.5(2) . . ?
O1 C22 C24 124.6(3) . . ?
C24 C22 C20 119.9(3) . . ?
C22 C24 H24 119.4 . . ?
C22 C24 C26 121.3(3) . . ?
C26 C24 H24 119.4 . . ?
C24 C26 C1 119.7(3) . 3_565 ?
C24 C26 C27 118.4(3) . . ?
C27 C26 C1 121.8(3) . 3_565 ?
O2 C27 C7 123.5(3) . . ?
O2 C27 C26 116.4(2) . . ?
C7 C27 C26 120.1(3) . . ?
H3A C3 H3B 108.0 . . ?
C23 C3 H3A 109.4 . . ?
C23 C3 H3B 109.4 . . ?
C25 C3 H3A 109.4 . . ?
C25 C3 H3B 109.4 . . ?
C25 C3 C23 111.1(5) . . ?
C21 C11 H11 106.6 . . ?
C21 C11 C23 146.8(15) . . ?
C23 C11 H11 106.6 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C25 C13 H13A 109.5 . . ?
C25 C13 H13B 109.5 . . ?
C25 C13 H13C 109.5 . . ?
C11 C21 H21A 120.0 . . ?
C11 C21 H21B 120.0 . . ?
H21A C21 H21B 120.0 . . ?
C3 C23 C11 109.6(6) . . ?
C3 C23 H23A 109.7 . . ?
C3 C23 H23B 109.7 . . ?
C11 C23 H23A 109.7 . . ?
C11 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C3 C25 C13 109.6(6) . . ?
C3 C25 H25A 109.7 . . ?
C3 C25 H25B 109.7 . . ?
C13 C25 H25A 109.7 . . ?
C13 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C22 C24 C26 179.5(3) . . . . ?
O2 C9 C19 C5 -123.6(4) . . . . ?
N1 C6 C8 N2 -43.5(2) . . . . ?
N1 C6 C8 C10 -168.5(2) . . . . ?
N1 C6 C16 C14 -175.0(3) . . . . ?
N2 C8 C10 C12 -175.4(3) . . . . ?
N2 C18 C20 C7 -22.3(4) . . . . ?
N2 C18 C20 C22 160.6(3) . . . . ?
C1 N1 C4 N2 -137.4(3) . . . . ?
C1 N1 C6 C8 157.5(2) . . . . ?
C1 N1 C6 C16 -81.6(3) . . . . ?
C1 C26 C27 O2 -0.7(4) 3_565 . . . ?
C1 C26 C27 C7 179.8(3) 3_565 . . . ?
C4 N1 C1 C26 -68.7(3) . . . 2_665 ?
C4 N1 C6 C8 34.8(3) . . . . ?
C4 N1 C6 C16 155.7(3) . . . . ?
C4 N2 C8 C6 35.3(3) . . . . ?
C4 N2 C8 C10 156.0(3) . . . . ?
C4 N2 C18 C20 -73.7(3) . . . . ?
C6 N1 C1 C26 172.6(2) . . . 2_665 ?
C6 N1 C4 N2 -13.7(3) . . . . ?
C6 C8 C10 C12 -59.3(3) . . . . ?
C7 C20 C22 O1 -179.7(3) . . . . ?
C7 C20 C22 C24 -0.4(4) . . . . ?
C8 N2 C4 N1 -14.1(3) . . . . ?
C8 N2 C18 C20 167.2(2) . . . . ?
C8 C6 C16 C14 -59.0(3) . . . . ?
C8 C10 C12 C14 51.3(3) . . . . ?
C9 O2 C27 C7 2.8(4) . . . . ?
C9 O2 C27 C26 -176.6(3) . . . . ?
C10 C12 C14 C16 -49.2(3) . . . . ?
C12 C14 C16 C6 50.9(3) . . . . ?
C15 O1 C22 C20 173.9(3) . . . . ?
C15 O1 C22 C24 -5.4(4) . . . . ?
C16 C6 C8 N2 -168.8(2) . . . . ?
C16 C6 C8 C10 66.2(2) . . . . ?
C17 C2 C15 O1 113.8(4) . . . . ?
C18 N2 C4 N1 -138.1(3) . . . . ?
C18 N2 C8 C6 158.3(2) . . . . ?
C18 N2 C8 C10 -81.0(3) . . . . ?
C18 C20 C22 O1 -2.6(4) . . . . ?
C18 C20 C22 C24 176.8(3) . . . . ?
C20 C7 C27 O2 -179.0(3) . . . . ?
C20 C7 C27 C26 0.5(4) . . . . ?
C20 C22 C24 C26 0.2(4) . . . . ?
C22 O1 C15 C2 178.6(3) . . . . ?
C22 C24 C26 C1 179.9(3) . . . 3_565 ?
C22 C24 C26 C27 0.3(4) . . . . ?
C24 C26 C27 O2 178.9(3) . . . . ?
C24 C26 C27 C7 -0.6(4) . . . . ?
C27 O2 C9 C19 176.4(3) . . . . ?
C27 C7 C20 C18 -177.1(3) . . . . ?
C27 C7 C20 C22 0.0(4) . . . . ?
C21 C11 C23 C3 178(4) . . . . ?
C23 C3 C25 C13 -170(2) . . . . ?
C25 C3 C23 C11 163.8(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.880(2)
2 0.120(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_trans-3He@P-TA
_database_code_depnum_ccdc_archive 'CCDC 2113573'
loop_
_audit_author_name
_audit_author_address
yanjun.ding
;KAUST
Saudi Arabia
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_audit_creation_date             2021-09-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C63 H84 N6 O6, 0.5(C6 H12)'
_chemical_formula_sum            'C66 H90 N6 O6'
_chemical_formula_weight         1063.43
_chemical_absolute_configuration syn
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   20.3338(3)
_cell_length_b                   20.3338(3)
_cell_length_c                   13.7372(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4918.9(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      65.10
_cell_measurement_theta_min      5.97
_shelx_estimated_absorpt_T_max   0.974
_shelx_estimated_absorpt_T_min   0.958
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9053.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21516
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        65.098
_diffrn_reflns_theta_max         65.098
_diffrn_reflns_theta_min         5.969
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3648
_reflns_number_total             3650
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3650
_refine_ls_number_restraints     908
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0708
_refine_ls_restrained_S_all      1.061
_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/[σ²(Fo²)+(0.1472P)²+7.5772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2056
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.8(6)
 0.2(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3-C23
 1.32 with sigma of 0.01
 C13-C25 = C25-C3
 1.54 with sigma of 0.01
 C21-C11 = C11-C23
 1.54 with sigma of 0.01
 C21-C23
 2.515 with sigma of 0.01
 C13-C3
 2.515 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10
\\sim C12 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20
\\sim C22 \\sim C24 \\sim C26 \\sim C27 \\sim C3 \\sim C11 \\sim C13 \\sim C21
\\sim C23 \\sim C25: within 5A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 5A
Uanis(C13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: C3(0.16667) H3(0.16667) C11(0.16667) H11A(0.16667) H11B(0.16667)
 C13(0.16667) H13A(0.16667) H13B(0.16667) H13C(0.16667) C21(0.16667)
 H21A(0.16667) H21B(0.16667) H21C(0.16667) C23(0.16667) H23(0.16667)
 C25(0.16667) H25A(0.16667) H25B(0.16667)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C11(H11A,H11B),
  C25(H25A,H25B)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C16(H16), C17(H17), C3(H3), C23(H23)
6.d X=CH2 refined with riding coordinates:
 C5(H5A,H5B), C19(H19A,H19B)
6.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1378(2) 0.4359(3) 0.3131(2) 0.0454(10) Uani 1 1 d . . . . .
O2 O 0.1311(2) 0.4972(2) 0.7040(2) 0.0402(9) Uani 1 1 d . . . . .
N1 N 0.2705(2) 0.39584(19) 0.5058(3) 0.0280(8) Uani 1 1 d . . . . .
N2 N 0.4042(2) 0.4589(2) 0.5102(3) 0.0280(8) Uani 1 1 d . . . . .
C1 C 0.3730(2) 0.3790(2) 0.5342(3) 0.0275(9) Uani 1 1 d . U . . .
H1 H 0.363895 0.372318 0.606008 0.033 Uiso 1 1 calc R U . . .
C2 C 0.1749(3) 0.4798(4) 0.7694(4) 0.0484(12) Uani 1 1 d . U . . .
H2A H 0.228943 0.507497 0.749705 0.058 Uiso 1 1 calc R U . . .
H2B H 0.156862 0.424684 0.767460 0.058 Uiso 1 1 calc R U . . .
C4 C 0.1328(3) 0.4807(3) 0.6069(3) 0.0331(9) Uani 1 1 d . U . . .
C5 C 0.2271(6) 0.5492(5) 0.9235(6) 0.076(2) Uani 1 1 d . U . . .
H5A H 0.276916 0.569036 0.898023 0.092 Uiso 1 1 calc R U . . .
H5B H 0.220117 0.562664 0.987370 0.092 Uiso 1 1 calc R U . . .
C6 C 0.1733(3) 0.4318(3) 0.4741(3) 0.0315(9) Uani 1 1 d . U . . .
C7 C 0.4182(3) 0.3415(3) 0.5034(3) 0.0329(9) Uani 1 1 d . U . . .
H7A H 0.467314 0.364977 0.538350 0.039 Uiso 1 1 calc R U . . .
H7B H 0.428602 0.348538 0.432625 0.039 Uiso 1 1 calc R U . . .
C8 C 0.1726(3) 0.4465(3) 0.5721(3) 0.0334(9) Uani 1 1 d . U . . .
H8 H 0.199788 0.433027 0.616420 0.040 Uiso 1 1 calc R U . . .
C9 C 0.1668(4) 0.5024(4) 0.8695(5) 0.0588(14) Uani 1 1 d . U . . .
H9 H 0.117386 0.483101 0.896077 0.071 Uiso 1 1 calc R U . . .
C10 C 0.2480(3) 0.2609(2) 0.5147(4) 0.0333(10) Uani 1 1 d . U . . .
H10A H 0.198460 0.237486 0.480746 0.040 Uiso 1 1 calc R U . . .
H10B H 0.238728 0.258650 0.585634 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4632(3) 0.5106(3) 0.5775(3) 0.0357(10) Uani 1 1 d . U . . .
H12A H 0.502529 0.495723 0.583622 0.043 Uiso 1 1 calc R U . . .
H12B H 0.440669 0.506602 0.642616 0.043 Uiso 1 1 calc R U . . .
C14 C 0.2139(3) 0.3922(3) 0.4367(3) 0.0348(9) Uani 1 1 d . U . . .
H14A H 0.176318 0.338378 0.423461 0.042 Uiso 1 1 calc R U . . .
H14B H 0.239412 0.415960 0.374588 0.042 Uiso 1 1 calc R U . . .
C15 C 0.0923(3) 0.4495(4) 0.2450(4) 0.0492(12) Uani 1 1 d . U . . .
H15A H 0.104913 0.503161 0.248107 0.059 Uiso 1 1 calc R U . . .
H15B H 0.037731 0.416654 0.260014 0.059 Uiso 1 1 calc R U . . .
C16 C 0.0938(3) 0.4862(3) 0.4442(4) 0.0366(10) Uani 1 1 d . U . . .
H16 H 0.066690 0.499683 0.399779 0.044 Uiso 1 1 calc R U . . .
C17 C 0.1096(4) 0.4315(4) 0.1462(4) 0.0533(13) Uani 1 1 d . U . . .
H17 H 0.159631 0.462860 0.121990 0.064 Uiso 1 1 calc R U . . .
C18 C 0.1339(3) 0.4528(3) 0.4093(3) 0.0341(9) Uani 1 1 d . U . . .
C19 C 0.0643(5) 0.3793(5) 0.0931(6) 0.0693(19) Uani 1 1 d . U . . .
H19A H 0.013748 0.346540 0.114478 0.083 Uiso 1 1 calc R U . . .
H19B H 0.080150 0.371819 0.031025 0.083 Uiso 1 1 calc R U . . .
C20 C 0.2971(3) 0.3428(2) 0.4825(3) 0.0293(9) Uani 1 1 d . U . . .
H20 H 0.305903 0.344018 0.410689 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3718(3) 0.2568(3) 0.5276(4) 0.0374(10) Uani 1 1 d . U . . .
H22A H 0.370689 0.250485 0.599115 0.045 Uiso 1 1 calc R U . . .
H22B H 0.397625 0.230868 0.499361 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3385(3) 0.4707(3) 0.5101(4) 0.0400(10) Uani 1 1 d . U . . .
H24A H 0.338185 0.497688 0.569981 0.048 Uiso 1 1 calc R U . . .
H24B H 0.340638 0.501500 0.453070 0.048 Uiso 1 1 calc R U . . .
C26 C 0.2899(3) 0.2181(3) 0.4896(4) 0.0390(11) Uani 1 1 d . U . . .
H26A H 0.290630 0.213075 0.417982 0.047 Uiso 1 1 calc R U . . .
H26B H 0.261429 0.166273 0.517333 0.047 Uiso 1 1 calc R U . . .
C27 C 0.0921(3) 0.5004(3) 0.5425(3) 0.0322(9) Uani 1 1 d . U . . .
C3 C 0.3306(19) 0.6843(17) 0.4324(14) 0.031(3) Uani 0.1667 1 d D U P A -1
H3 H 0.351338 0.734572 0.408219 0.037 Uiso 0.1667 1 calc R U P A -1
C11 C 0.3129(14) 0.6549(16) 0.6178(16) 0.045(3) Uani 0.1667 1 d D U P A -1
H11A H 0.331277 0.621630 0.644026 0.054 Uiso 0.1667 1 calc R U P A -1
H11B H 0.257867 0.623245 0.604475 0.054 Uiso 0.1667 1 calc R U P A -1
C13 C 0.2663(14) 0.6794(15) 0.2730(14) 0.029(4) Uani 0.1667 1 d D U P A -1
H13A H 0.258354 0.656201 0.208309 0.043 Uiso 0.1667 1 calc R U P A -1
H13B H 0.308703 0.731707 0.270401 0.043 Uiso 0.1667 1 calc R U P A -1
H13C H 0.220118 0.679339 0.293496 0.043 Uiso 0.1667 1 calc R U P A -1
C21 C 0.326(2) 0.717(2) 0.6930(19) 0.060(6) Uani 0.1667 1 d D U P A -1
H21A H 0.325573 0.758943 0.660211 0.090 Uiso 0.1667 1 calc R U P A -1
H21B H 0.376002 0.734907 0.724071 0.090 Uiso 0.1667 1 calc R U P A -1
H21C H 0.286463 0.695191 0.742540 0.090 Uiso 0.1667 1 calc R U P A -1
C23 C 0.3553(15) 0.6925(16) 0.5235(12) 0.046(3) Uani 0.1667 1 d D U P A -1
H23 H 0.407894 0.727513 0.531552 0.055 Uiso 0.1667 1 calc R U P A -1
C25 C 0.2849(18) 0.6328(13) 0.3474(18) 0.047(3) Uani 0.1667 1 d D U P A -1
H25A H 0.237141 0.589313 0.371995 0.057 Uiso 0.1667 1 calc R U P A -1
H25B H 0.314589 0.612641 0.314876 0.057 Uiso 0.1667 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.435(6) . ?
O1 C18 1.378(6) . ?
O2 C2 1.428(7) . ?
O2 C4 1.380(6) . ?
N1 C14 1.464(6) . ?
N1 C20 1.464(5) . ?
N1 C24 1.459(6) . ?
N2 C1 1.455(5) . ?
N2 C12 1.462(6) . ?
N2 C24 1.471(6) . ?
C1 H1 1.0000 . ?
C1 C7 1.518(6) . ?
C1 C20 1.514(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C9 1.486(9) . ?
C4 C8 1.388(6) . ?
C4 C27 1.401(7) . ?
C5 H5A 0.9500 . ?
C5 H5B 0.9500 . ?
C5 C9 1.339(11) . ?
C6 C8 1.380(7) . ?
C6 C14 1.502(6) . ?
C6 C18 1.400(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C22 1.531(6) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C20 1.518(6) . ?
C10 C26 1.531(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C27 1.509(6) 2_665 ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C17 1.492(8) . ?
C16 H16 0.9500 . ?
C16 C18 1.383(7) . ?
C16 C27 1.384(7) . ?
C17 H17 0.9500 . ?
C17 C19 1.237(10) . ?
C19 H19A 0.9500 . ?
C19 H19B 0.9500 . ?
C20 H20 1.0000 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C26 1.534(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C3 H3 0.9500 . ?
C3 C23 1.326(14) . ?
C3 C25 1.534(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C21 1.539(15) . ?
C11 C23 1.532(14) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C25 1.563(14) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 O1 C15 117.1(4) . . ?
C4 O2 C2 116.9(4) . . ?
C20 N1 C14 113.1(3) . . ?
C24 N1 C14 112.9(4) . . ?
C24 N1 C20 105.7(3) . . ?
C1 N2 C12 113.7(3) . . ?
C1 N2 C24 104.9(3) . . ?
C12 N2 C24 111.7(4) . . ?
N2 C1 H1 108.9 . . ?
N2 C1 C7 117.5(3) . . ?
N2 C1 C20 101.9(3) . . ?
C7 C1 H1 108.9 . . ?
C20 C1 H1 108.9 . . ?
C20 C1 C7 110.5(3) . . ?
O2 C2 H2A 109.9 . . ?
O2 C2 H2B 109.9 . . ?
O2 C2 C9 109.1(5) . . ?
H2A C2 H2B 108.3 . . ?
C9 C2 H2A 109.9 . . ?
C9 C2 H2B 109.9 . . ?
O2 C4 C8 123.1(4) . . ?
O2 C4 C27 116.7(4) . . ?
C8 C4 C27 120.1(4) . . ?
H5A C5 H5B 120.0 . . ?
C9 C5 H5A 120.0 . . ?
C9 C5 H5B 120.0 . . ?
C8 C6 C14 121.2(4) . . ?
C8 C6 C18 119.0(4) . . ?
C18 C6 C14 119.9(4) . . ?
C1 C7 H7A 110.0 . . ?
C1 C7 H7B 110.0 . . ?
C1 C7 C22 108.5(3) . . ?
H7A C7 H7B 108.4 . . ?
C22 C7 H7A 110.0 . . ?
C22 C7 H7B 110.0 . . ?
C4 C8 H8 119.5 . . ?
C6 C8 C4 121.1(4) . . ?
C6 C8 H8 119.5 . . ?
C2 C9 H9 119.0 . . ?
C5 C9 C2 122.0(7) . . ?
C5 C9 H9 119.0 . . ?
H10A C10 H10B 108.4 . . ?
C20 C10 H10A 110.1 . . ?
C20 C10 H10B 110.1 . . ?
C20 C10 C26 108.1(4) . . ?
C26 C10 H10A 110.1 . . ?
C26 C10 H10B 110.1 . . ?
N2 C12 H12A 109.4 . . ?
N2 C12 H12B 109.4 . . ?
N2 C12 C27 111.2(4) . 2_665 ?
H12A C12 H12B 108.0 . . ?
C27 C12 H12A 109.4 2_665 . ?
C27 C12 H12B 109.4 2_665 . ?
N1 C14 C6 112.3(4) . . ?
N1 C14 H14A 109.1 . . ?
N1 C14 H14B 109.1 . . ?
C6 C14 H14A 109.1 . . ?
C6 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
O1 C15 H15A 110.3 . . ?
O1 C15 H15B 110.3 . . ?
O1 C15 C17 107.0(4) . . ?
H15A C15 H15B 108.6 . . ?
C17 C15 H15A 110.3 . . ?
C17 C15 H15B 110.3 . . ?
C18 C16 H16 119.2 . . ?
C18 C16 C27 121.5(5) . . ?
C27 C16 H16 119.2 . . ?
C15 C17 H17 117.2 . . ?
C19 C17 C15 125.5(7) . . ?
C19 C17 H17 117.2 . . ?
O1 C18 C6 114.9(4) . . ?
O1 C18 C16 125.2(4) . . ?
C16 C18 C6 119.8(4) . . ?
C17 C19 H19A 120.0 . . ?
C17 C19 H19B 120.0 . . ?
H19A C19 H19B 120.0 . . ?
N1 C20 C1 101.6(3) . . ?
N1 C20 C10 117.5(4) . . ?
N1 C20 H20 109.0 . . ?
C1 C20 C10 110.4(4) . . ?
C1 C20 H20 109.0 . . ?
C10 C20 H20 109.0 . . ?
C7 C22 H22A 108.8 . . ?
C7 C22 H22B 108.8 . . ?
C7 C22 C26 113.8(4) . . ?
H22A C22 H22B 107.7 . . ?
C26 C22 H22A 108.8 . . ?
C26 C22 H22B 108.8 . . ?
N1 C24 N2 107.1(4) . . ?
N1 C24 H24A 110.3 . . ?
N1 C24 H24B 110.3 . . ?
N2 C24 H24A 110.3 . . ?
N2 C24 H24B 110.3 . . ?
H24A C24 H24B 108.6 . . ?
C10 C26 C22 113.7(4) . . ?
C10 C26 H26A 108.8 . . ?
C10 C26 H26B 108.8 . . ?
C22 C26 H26A 108.8 . . ?
C22 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C4 C27 C12 121.8(4) . 3_565 ?
C16 C27 C4 118.5(4) . . ?
C16 C27 C12 119.8(4) . 3_565 ?
C23 C3 H3 105.0 . . ?
C23 C3 C25 150(3) . . ?
C25 C3 H3 105.0 . . ?
H11A C11 H11B 108.2 . . ?
C21 C11 H11A 109.8 . . ?
C21 C11 H11B 109.8 . . ?
C23 C11 H11A 109.8 . . ?
C23 C11 H11B 109.8 . . ?
C23 C11 C21 109.5(14) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C25 C13 H13A 109.5 . . ?
C25 C13 H13B 109.5 . . ?
C25 C13 H13C 109.5 . . ?
C11 C21 H21A 109.5 . . ?
C11 C21 H21B 109.5 . . ?
C11 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C23 C11 131(3) . . ?
C3 C23 H23 114.6 . . ?
C11 C23 H23 114.6 . . ?
C3 C25 C13 109.4(13) . . ?
C3 C25 H25A 109.8 . . ?
C3 C25 H25B 109.8 . . ?
C13 C25 H25A 109.8 . . ?
C13 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C15 C17 C19 114.5(7) . . . . ?
O2 C2 C9 C5 -125.2(7) . . . . ?
O2 C4 C8 C6 -179.3(4) . . . . ?
O2 C4 C27 C12 -1.0(7) . . . 3_565 ?
O2 C4 C27 C16 178.7(4) . . . . ?
N2 C1 C7 C22 -175.0(4) . . . . ?
N2 C1 C20 N1 -43.2(4) . . . . ?
N2 C1 C20 C10 -168.6(3) . . . . ?
C1 N2 C12 C27 173.4(4) . . . 2_665 ?
C1 N2 C24 N1 -16.0(5) . . . . ?
C1 C7 C22 C26 50.7(5) . . . . ?
C2 O2 C4 C8 2.1(7) . . . . ?
C2 O2 C4 C27 -177.7(4) . . . . ?
C4 O2 C2 C9 179.2(5) . . . . ?
C7 C1 C20 N1 -168.8(3) . . . . ?
C7 C1 C20 C10 65.8(4) . . . . ?
C7 C22 C26 C10 -49.1(5) . . . . ?
C8 C4 C27 C12 179.3(4) . . . 3_565 ?
C8 C4 C27 C16 -1.0(7) . . . . ?
C8 C6 C14 N1 -19.5(6) . . . . ?
C8 C6 C18 O1 180.0(4) . . . . ?
C8 C6 C18 C16 -1.4(7) . . . . ?
C12 N2 C1 C7 -80.5(5) . . . . ?
C12 N2 C1 C20 158.6(4) . . . . ?
C12 N2 C24 N1 -139.6(4) . . . . ?
C14 N1 C20 C1 157.7(3) . . . . ?
C14 N1 C20 C10 -81.8(5) . . . . ?
C14 N1 C24 N2 -136.0(4) . . . . ?
C14 C6 C8 C4 -177.7(4) . . . . ?
C14 C6 C18 O1 -1.5(7) . . . . ?
C14 C6 C18 C16 177.2(5) . . . . ?
C15 O1 C18 C6 174.1(5) . . . . ?
C15 O1 C18 C16 -4.5(8) . . . . ?
C18 O1 C15 C17 176.7(5) . . . . ?
C18 C6 C8 C4 0.8(7) . . . . ?
C18 C6 C14 N1 162.0(4) . . . . ?
C18 C16 C27 C4 0.5(7) . . . . ?
C18 C16 C27 C12 -179.8(5) . . . 3_565 ?
C20 N1 C14 C6 165.9(4) . . . . ?
C20 N1 C24 N2 -11.8(5) . . . . ?
C20 C1 C7 C22 -58.7(4) . . . . ?
C20 C10 C26 C22 51.8(5) . . . . ?
C24 N1 C14 C6 -74.1(5) . . . . ?
C24 N1 C20 C1 33.7(4) . . . . ?
C24 N1 C20 C10 154.2(4) . . . . ?
C24 N2 C1 C7 157.2(4) . . . . ?
C24 N2 C1 C20 36.3(4) . . . . ?
C24 N2 C12 C27 -68.1(5) . . . 2_665 ?
C26 C10 C20 N1 -175.7(4) . . . . ?
C26 C10 C20 C1 -59.9(4) . . . . ?
C27 C4 C8 C6 0.4(7) . . . . ?
C27 C16 C18 O1 179.2(5) . . . . ?
C27 C16 C18 C6 0.7(8) . . . . ?
C21 C11 C23 C3 -126(4) . . . . ?
C23 C3 C25 C13 160(5) . . . . ?
C25 C3 C23 C11 -47(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.8(6)
2 0.2(6)

