#------------------------------------------------------------------------------
#$Date: 2022-03-03 01:09:34 +0200 (Thu, 03 Mar 2022) $
#$Revision: 273210 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/65/1566521.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1566521
loop_
_publ_author_name
'Ding, Yanjun'
'Alimi, Lukman O.'
'Du, Jing'
'Hua, Bin'
'Dey, Avishek'
'Yu, Pei'
'Khashab, Niveen M.'
_publ_section_title
;
 Pillar[3]trianglamines: deeper cavity triangular macrocycles for
 selective hexene isomer separation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00207H
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C H2 Cl2, C63 H84 N6 O6'
_chemical_formula_sum            'C64 H86 Cl2 N6 O6'
_chemical_formula_weight         1106.28
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.2894(6)
_cell_length_b                   20.2894(6)
_cell_length_c                   13.6577(5)
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    120.01
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.32
_cell_volume                     4869.1(3)
_computing_cell_refinement       '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)'
_diffrn_ambient_temperature      120.01
_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_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_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_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
_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_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_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0699
_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
_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_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc00207h2.cif
_cod_data_source_block           P-TA
_cod_database_code               1566521
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.963
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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 . . .
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'
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_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_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) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9658(12)
2 0.0342(12)
