# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_cu_gb061_0m
_database_code_depnum_ccdc_archive 'CCDC 2079257'
loop_
_audit_author_name
_audit_author_address
'Ben Wilson'
;University of Windsor
Canada
;
_audit_update_record             
;
2021-04-21 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_cu_gb061_0m         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The small crystals were weakly diffracting and no diffraction was observed beyond 0.9 Angstroms
;
_vrf_PLAT097_cu_gb061_0m         
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.74 eA-3  
RESPONSE: The molecule crystallised with a number of DCM solvent molecules which are disordered over
several positions. Despite modeling the disorder of three such molecules, there remains some unresolved disorder
that is unable to be modled in a chemically sensible manner.
;
_vrf_PLAT340_cu_gb061_0m         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01065 Ang.  
RESPONSE: The low resolution data and the unresolved disorder results in lower C-C bond precision
;
# end Validation Reply Form
_audit_creation_date             2020-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
bwilson@uwindsor.ca
loeb@uwindsor.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'5.17(C H2 Cl2), C114 H82 N4, 2(C0.75 H1.5 Cl1.75)'
_chemical_formula_sum            'C120.67 H95.33 Cl13.83 N4'
_chemical_formula_weight         2091.65
_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'
Cl Cl 0.3639 0.7018 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.2864(7)
_cell_length_b                   12.6134(7)
_cell_length_c                   17.4682(10)
_cell_angle_alpha                76.476(3)
_cell_angle_beta                 89.608(4)
_cell_angle_gamma                89.864(3)
_cell_volume                     2632.0(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      59.87
_cell_measurement_theta_min      2.60
_shelx_estimated_absorpt_T_max   0.643
_shelx_estimated_absorpt_T_min   0.318
_exptl_absorpt_coefficient_mu    3.720
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1178 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.7187. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28330
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        58.927
_diffrn_reflns_theta_max         58.927
_diffrn_reflns_theta_min         3.597
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5783
_reflns_number_total             7454
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         7454
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.1323
_refine_ls_restrained_S_all      1.095
_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)+(0.1239P)²+20.3668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3131
_refine_ls_wR_factor_ref         0.3326
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Hydrogen atoms were included
in calculated positions with isotropic displacement parameters 1.2 times
the isotropic equivalent of their carrier atoms except for methyl groups 
where it is 1.5 times. The disorder of the DCM molecules required the C-Cl 
and Cl...Cl to be restrained with the DFIX restraint. The SIMU, ISOR and RIGU restraints
were required in oder for the thermal parameters of the C and Cl atoms of the disorered 
DCM molecules to be modeled in a chemically sensible manner.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 Cl4B-Cl3B
 2.292 with sigma of 0.02
 Cl3B-Cl4B
 3 with sigma of 0.02
 Cl6A-C60
 1.7 with sigma of 0.02
 C60-Cl5A
 1.7 with sigma of 0.02
 Cl8B-C61B
 1.7 with sigma of 0.02
 Cl8B-Cl7B
 2.927 with sigma of 0.02
 C61B-Cl7B
 1.715 with sigma of 0.02
 Cl8A-C61A
 1.715 with sigma of 0.02
 Cl8A-Cl7A
 2.928 with sigma of 0.02
 C60-Cl6B
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3B \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl4B \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl3A \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl4A \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl4B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl3B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl4A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C60 \\sim Cl5A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C61B \\sim Cl8B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl8A \\sim C61A \\sim Cl7A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl7B \\sim C61B \\sim Cl8B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C61A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C61B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl3B, Cl3A, C59, Cl4B, Cl4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl7A, C61A, Cl8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61A, Cl8A, Cl7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl7A(0.33333) Cl8A(0.33333) Cl8B(0.5) C60(0.75) H60C(0.25)
 H60D(0.25) H60A(0.5) H60B(0.5) Cl6B(0.25) C61B(0.5) H61C(0.5) H61D(0.5)
 Cl3A(0.5) C59(0.75) H59B(0.5) H59A(0.5) H59D(0.25) H59C(0.25) Cl3B(0.25)
 Cl4B(0.25) Cl4A(0.5) Cl6A(0.5) Cl5A(0.75) Cl5B(0.25) Cl7B(0.5) C61A(0.33333)
 H61A(0.33333) H61B(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C60(H60C,H60D), C60(H60A,H60B), C61B(H61C,H61D), C59(H59B,
 H59A), C59(H59D,H59C), C61A(H61A,H61B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C20(H20), C45(H45), C35(H35), C41(H41), C22(H22), C47(H47), C12(H12),
 C32(H32), C34(H34), C13(H13), C10(H10), C37(H37), C26(H26), C23(H23), C16(H16),
  C44(H44), C9(H9), C28(H28), C38(H38), C53(H53), C17(H17), C51(H51), C31(H31),
 C5(H5), C4(H4), C57(H57), C19(H19), C18(H18), C48(H48), C30(H30), C24(H24),
 C29(H29), C25(H25), C42(H42), C56(H56), C43(H43), C54(H54), C55(H55), C49(H49),
  C50(H50)
;
_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 0.5632(2) 0.2928(2) 0.7244(2) 0.0978(10) Uani 1 1 d . . . . .
Cl2 Cl 0.4271(3) 0.1007(2) 0.73089(18) 0.0950(9) Uani 1 1 d . . . . .
Cl7A Cl 0.697(3) 0.269(3) 0.4442(14) 0.249(13) Uani 0.3333 1 d D U P A 3
N2 N 0.4314(5) 0.1226(5) 0.5129(3) 0.0531(19) Uani 1 1 d . . . . .
H2 H 0.402600 0.109569 0.560407 0.064 Uiso 1 1 calc R . . . .
N1 N 0.5206(5) 0.1001(5) 0.4049(4) 0.0541(19) Uani 1 1 d . . . . .
Cl8A Cl 0.785(2) 0.2991(17) 0.5852(8) 0.213(11) Uani 0.3333 1 d D U P A 3
C39 C 0.1151(5) 0.3732(5) 0.7263(4) 0.0340(15) Uani 1 1 d . . . . .
C36 C 0.1893(5) 0.3540(6) 0.6589(4) 0.0333(15) Uani 1 1 d . . . . .
C15 C 0.6996(5) 0.1371(5) 0.0129(4) 0.0364(16) Uani 1 1 d . . . . .
C33 C 0.3191(6) 0.3351(6) 0.5306(4) 0.0429(19) Uani 1 1 d . . . . .
C21 C 0.8625(5) 0.2184(5) 0.0608(4) 0.0317(15) Uani 1 1 d . . . . .
C40 C 0.0352(5) 0.2774(5) 0.7575(3) 0.0309(15) Uani 1 1 d . . . . .
C27 C 0.7238(6) 0.3435(5) -0.0220(4) 0.0338(15) Uani 1 1 d . . . . .
C20 C 0.7235(6) 0.0322(5) 0.0591(4) 0.0384(17) Uani 1 1 d . . . . .
H20 H 0.762375 0.025044 0.106896 0.046 Uiso 1 1 calc R . . . .
C11 C 0.6749(6) 0.2493(5) 0.1162(4) 0.0336(16) Uani 1 1 d . . . . .
C14 C 0.7402(5) 0.2366(5) 0.0420(4) 0.0316(15) Uani 1 1 d . . . . .
C45 C 0.0769(6) 0.1742(6) 0.7882(4) 0.0370(16) Uani 1 1 d . . . . .
H45 H 0.153384 0.163076 0.787653 0.044 Uiso 1 1 calc R . . . .
C46 C 0.0546(5) 0.4809(6) 0.6894(4) 0.0373(17) Uani 1 1 d . . . . .
C52 C 0.1819(6) 0.3791(5) 0.7998(4) 0.0359(16) Uani 1 1 d . . . . .
C35 C 0.1745(6) 0.2672(6) 0.6234(4) 0.0389(17) Uani 1 1 d . . . . .
H35 H 0.119345 0.214765 0.642516 0.047 Uiso 1 1 calc R . . . .
C41 C -0.0773(5) 0.2912(6) 0.7609(4) 0.0390(17) Uani 1 1 d . . . . .
H41 H -0.108151 0.361182 0.740718 0.047 Uiso 1 1 calc R . . . .
C22 C 0.9287(6) 0.1771(6) 0.0085(4) 0.0397(17) Uani 1 1 d . . . . .
H22 H 0.896493 0.159301 -0.036102 0.048 Uiso 1 1 calc R . . . .
C7 C 0.4278(6) 0.2194(6) 0.4551(4) 0.046(2) Uani 1 1 d . . . . .
C47 C -0.0103(6) 0.4836(6) 0.6245(4) 0.0443(18) Uani 1 1 d . . . . .
H47 H -0.017507 0.419052 0.605755 0.053 Uiso 1 1 calc R . . . .
C12 C 0.6886(6) 0.3415(5) 0.1447(4) 0.0384(17) Uani 1 1 d . . . . .
H12 H 0.737135 0.396624 0.118118 0.046 Uiso 1 1 calc R . . . .
C8 C 0.5597(7) 0.2788(5) 0.2492(4) 0.045(2) Uani 1 1 d . . . . .
C32 C 0.6202(6) 0.3885(6) -0.0349(4) 0.0391(17) Uani 1 1 d . . . . .
H32 H 0.560893 0.353837 -0.003763 0.047 Uiso 1 1 calc R . . . .
C34 C 0.2399(6) 0.2565(6) 0.5601(4) 0.0429(18) Uani 1 1 d . . . . .
H34 H 0.230694 0.195960 0.537110 0.052 Uiso 1 1 calc R . . . .
C13 C 0.6334(6) 0.3561(5) 0.2110(4) 0.0424(18) Uani 1 1 d . . . . .
H13 H 0.646370 0.419415 0.230224 0.051 Uiso 1 1 calc R . . . .
C10 C 0.5971(6) 0.1723(5) 0.1537(4) 0.0435(19) Uani 1 1 d . . . . .
H10 H 0.582324 0.109751 0.134018 0.052 Uiso 1 1 calc R . . . .
C37 C 0.2668(6) 0.4310(6) 0.6265(4) 0.0430(18) Uani 1 1 d . . . . .
H37 H 0.276000 0.492678 0.648197 0.052 Uiso 1 1 calc R . . . .
C26 C 0.9124(6) 0.2420(6) 0.1252(4) 0.0430(18) Uani 1 1 d . . . . .
H26 H 0.870138 0.269436 0.162046 0.052 Uiso 1 1 calc R . . . .
C2 C 0.4840(7) 0.2072(6) 0.3872(4) 0.051(2) Uani 1 1 d . . . . .
C3 C 0.5015(7) 0.2944(6) 0.3221(4) 0.050(2) Uani 1 1 d . . . . .
C23 C 1.0388(6) 0.1619(6) 0.0202(4) 0.0402(17) Uani 1 1 d . . . . .
H23 H 1.081371 0.133846 -0.016254 0.048 Uiso 1 1 calc R . . . .
C16 C 0.6434(5) 0.1448(6) -0.0556(4) 0.0381(16) Uani 1 1 d . . . . .
H16 H 0.625870 0.214538 -0.087535 0.046 Uiso 1 1 calc R . . . .
C6 C 0.3832(6) 0.3210(6) 0.4599(4) 0.0446(19) Uani 1 1 d . . . . .
C44 C 0.0097(6) 0.0873(6) 0.8196(4) 0.0458(18) Uani 1 1 d . . . . .
H44 H 0.039798 0.016785 0.839150 0.055 Uiso 1 1 calc R . . . .
C9 C 0.5418(7) 0.1890(6) 0.2200(5) 0.056(2) Uani 1 1 d . . . . .
H9 H 0.490112 0.136325 0.245553 0.067 Uiso 1 1 calc R . . . .
C28 C 0.8084(6) 0.3977(6) -0.0677(4) 0.0466(19) Uani 1 1 d . . . . .
H28 H 0.880399 0.370049 -0.059573 0.056 Uiso 1 1 calc R . . . .
C38 C 0.3316(6) 0.4209(6) 0.5631(4) 0.049(2) Uani 1 1 d . . . . .
H38 H 0.384861 0.474787 0.542716 0.059 Uiso 1 1 calc R . . . .
C53 C 0.2910(6) 0.3508(6) 0.8084(5) 0.0473(19) Uani 1 1 d . . . . .
H53 H 0.330231 0.333575 0.765883 0.057 Uiso 1 1 calc R . . . .
C17 C 0.6117(6) 0.0506(6) -0.0787(5) 0.0482(19) Uani 1 1 d . . . . .
H17 H 0.573381 0.056707 -0.126632 0.058 Uiso 1 1 calc R . . . .
C51 C 0.0688(7) 0.5756(6) 0.7133(4) 0.050(2) Uani 1 1 d . . . . .
H51 H 0.115149 0.576433 0.756434 0.060 Uiso 1 1 calc R . . . .
C31 C 0.6016(7) 0.4834(6) -0.0926(4) 0.052(2) Uani 1 1 d . . . . .
H31 H 0.529959 0.512076 -0.100704 0.062 Uiso 1 1 calc R . . . .
C5 C 0.4034(7) 0.4069(6) 0.3954(4) 0.054(2) Uani 1 1 d . . . . .
H5 H 0.377155 0.477399 0.396534 0.065 Uiso 1 1 calc R . . . .
C4 C 0.4603(7) 0.3936(6) 0.3294(4) 0.052(2) Uani 1 1 d . . . . .
H4 H 0.471574 0.455580 0.287252 0.063 Uiso 1 1 calc R . . . .
C57 C 0.1265(7) 0.4019(6) 0.8646(4) 0.0484(19) Uani 1 1 d . . . . .
H57 H 0.051229 0.419713 0.860645 0.058 Uiso 1 1 calc R . . . .
C19 C 0.6913(6) -0.0602(6) 0.0360(5) 0.049(2) Uani 1 1 d . . . . .
H19 H 0.707915 -0.130259 0.067835 0.059 Uiso 1 1 calc R . . . .
C1 C 0.4870(7) 0.0552(6) 0.4809(5) 0.053(2) Uani 1 1 d . . . . .
C18 C 0.6358(6) -0.0511(7) -0.0326(5) 0.053(2) Uani 1 1 d . . . . .
H18 H 0.613635 -0.114794 -0.048473 0.064 Uiso 1 1 calc R . . . .
C48 C -0.0652(6) 0.5770(7) 0.5857(5) 0.054(2) Uani 1 1 d . . . . .
H48 H -0.110236 0.576389 0.541868 0.065 Uiso 1 1 calc R . . . .
C30 C 0.6857(7) 0.5358(6) -0.1376(5) 0.055(2) Uani 1 1 d . . . . .
H30 H 0.673250 0.601065 -0.176522 0.066 Uiso 1 1 calc R . . . .
C24 C 1.0868(6) 0.1867(6) 0.0836(5) 0.050(2) Uani 1 1 d . . . . .
H24 H 1.162974 0.177119 0.091091 0.061 Uiso 1 1 calc R . . . .
C29 C 0.7888(8) 0.4922(7) -0.1255(5) 0.058(2) Uani 1 1 d . . . . .
H29 H 0.847553 0.527322 -0.157043 0.070 Uiso 1 1 calc R . . . .
C25 C 1.0244(6) 0.2262(7) 0.1374(5) 0.052(2) Uani 1 1 d . . . . .
H25 H 1.057538 0.242462 0.182260 0.062 Uiso 1 1 calc R . . . .
C42 C -0.1439(6) 0.2046(7) 0.7933(4) 0.051(2) Uani 1 1 d . . . . .
H42 H -0.220277 0.215469 0.795232 0.061 Uiso 1 1 calc R . . . .
C56 C 0.1817(9) 0.3987(7) 0.9350(4) 0.063(3) Uani 1 1 d . . . . .
H56 H 0.143975 0.415196 0.978413 0.075 Uiso 1 1 calc R . . . .
C43 C -0.1011(6) 0.1028(7) 0.8227(5) 0.0491(19) Uani 1 1 d . . . . .
H43 H -0.147619 0.043355 0.845007 0.059 Uiso 1 1 calc R . . . .
C54 C 0.3428(8) 0.3478(7) 0.8789(6) 0.067(3) Uani 1 1 d . . . . .
H54 H 0.417557 0.328333 0.883906 0.080 Uiso 1 1 calc R . . . .
C55 C 0.2897(11) 0.3719(7) 0.9414(5) 0.072(3) Uani 1 1 d . . . . .
H55 H 0.327375 0.370078 0.989023 0.086 Uiso 1 1 calc R . . . .
C49 C -0.0523(8) 0.6706(7) 0.6128(5) 0.068(3) Uani 1 1 d . . . . .
H49 H -0.090787 0.734908 0.588293 0.082 Uiso 1 1 calc R . . . .
C50 C 0.0157(8) 0.6715(8) 0.6748(5) 0.068(3) Uani 1 1 d . . . . .
H50 H 0.026597 0.737131 0.691588 0.082 Uiso 1 1 calc R . . . .
Cl8B Cl 0.6779(4) 0.2787(4) 0.4797(4) 0.0741(16) Uani 0.5 1 d D U P B 1
C58 C 0.5124(12) 0.2019(9) 0.6737(7) 0.104(4) Uani 1 1 d . . . . .
H58A H 0.574155 0.165706 0.653315 0.125 Uiso 1 1 calc R . . . .
H58B H 0.470863 0.242846 0.627815 0.125 Uiso 1 1 calc R . . . .
C60 C 0.8120(15) 0.0571(18) 0.4047(11) 0.198(14) Uani 0.75 1 d D U P . .
H60C H 0.887985 0.031187 0.404084 0.238 Uiso 0.25 1 calc R . P C 2
H60D H 0.764366 -0.005389 0.428255 0.238 Uiso 0.25 1 calc R . P C 2
H60A H 0.756059 0.010728 0.437398 0.238 Uiso 0.5 1 calc R . P D 1
H60B H 0.814243 0.129594 0.417452 0.238 Uiso 0.5 1 calc R . P D 1
Cl6B Cl 0.8006(12) 0.1645(12) 0.4583(10) 0.119(5) Uani 0.25 1 d D . P E 2
C61B C 0.7618(17) 0.3135(17) 0.5456(15) 0.078(7) Uani 0.5 1 d D U P B 1
H61C H 0.719950 0.313667 0.594210 0.094 Uiso 0.5 1 calc R . P B 1
H61D H 0.788519 0.388595 0.523957 0.094 Uiso 0.5 1 calc R . P B 1
Cl3A Cl 0.2690(8) 0.1291(16) 0.2502(7) 0.215(7) Uani 0.5 1 d . U P F 1
C59 C 0.2084(16) 0.0592(18) 0.3265(11) 0.111(6) Uani 0.75 1 d . U P . .
H59B H 0.133822 0.089487 0.324171 0.133 Uiso 0.5 1 calc R . P F 1
H59A H 0.200955 -0.014721 0.316841 0.133 Uiso 0.5 1 calc R . P F 1
H59D H 0.143210 0.045405 0.297352 0.133 Uiso 0.25 1 calc R . P F 2
H59C H 0.189230 0.040649 0.383236 0.133 Uiso 0.25 1 calc R . P F 2
Cl3B Cl 0.305(2) -0.024(2) 0.312(3) 0.273(15) Uani 0.25 1 d D U P F 2
Cl4B Cl 0.2322(19) 0.173(3) 0.304(2) 0.214(12) Uani 0.25 1 d D U P F 2
Cl4A Cl 0.2407(8) 0.0406(8) 0.4116(5) 0.143(3) Uani 0.5 1 d . U P F 1
Cl6A Cl 0.7962(13) 0.0656(10) 0.3041(8) 0.174(6) Uani 0.5 1 d D . P E 1
Cl5A Cl 0.9403(6) -0.0060(5) 0.4107(6) 0.217(5) Uani 0.75 1 d D U P E 1
Cl5B Cl 0.7731(9) 0.1155(14) 0.3192(9) 0.108(7) Uani 0.25 1 d . . P E 2
Cl7B Cl 0.8748(6) 0.2254(5) 0.5701(4) 0.116(3) Uani 0.5 1 d D U P B 1
C61A C 0.8051(19) 0.305(2) 0.4896(11) 0.055(6) Uani 0.3333 1 d D U P A 3
H61A H 0.866966 0.256876 0.484077 0.066 Uiso 0.3333 1 calc R . P A 3
H61B H 0.825798 0.380547 0.462844 0.066 Uiso 0.3333 1 calc R . P A 3


_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 C58 1.725(13) . ?
Cl2 C58 1.766(12) . ?
Cl7A C61A 1.67(3) . ?
N2 C7 1.391(9) . ?
N2 C1 1.310(9) . ?
N1 C2 1.389(9) . ?
N1 C1 1.376(9) . ?
Cl8A C61A 1.673(16) . ?
C39 C36 1.548(9) . ?
C39 C40 1.553(9) . ?
C39 C46 1.551(9) . ?
C39 C52 1.544(9) . ?
C36 C35 1.391(10) . ?
C36 C37 1.382(10) . ?
C15 C20 1.411(9) . ?
C15 C14 1.545(10) . ?
C15 C16 1.369(10) . ?
C33 C34 1.398(11) . ?
C33 C6 1.506(9) . ?
C33 C38 1.345(11) . ?
C21 C14 1.545(9) . ?
C21 C22 1.405(9) . ?
C21 C26 1.379(10) . ?
C40 C45 1.385(9) . ?
C40 C41 1.395(9) . ?
C27 C14 1.551(9) . ?
C27 C32 1.391(10) . ?
C27 C28 1.386(10) . ?
C20 C19 1.379(11) . ?
C11 C14 1.560(8) . ?
C11 C12 1.379(10) . ?
C11 C10 1.408(9) . ?
C45 C44 1.379(10) . ?
C46 C47 1.384(10) . ?
C46 C51 1.366(11) . ?
C52 C53 1.387(10) . ?
C52 C57 1.402(10) . ?
C35 C34 1.395(9) . ?
C41 C42 1.375(11) . ?
C22 C23 1.376(10) . ?
C7 C2 1.407(9) . ?
C7 C6 1.412(10) . ?
C47 C48 1.390(10) . ?
C12 C13 1.387(9) . ?
C8 C13 1.381(10) . ?
C8 C3 1.509(9) . ?
C8 C9 1.366(11) . ?
C32 C31 1.391(10) . ?
C10 C9 1.397(10) . ?
C37 C38 1.388(10) . ?
C26 C25 1.400(11) . ?
C2 C3 1.400(9) . ?
C3 C4 1.381(10) . ?
C23 C24 1.359(11) . ?
C16 C17 1.400(10) . ?
C6 C5 1.390(10) . ?
C44 C43 1.377(11) . ?
C28 C29 1.391(10) . ?
C53 C54 1.382(12) . ?
C17 C18 1.379(11) . ?
C51 C50 1.401(11) . ?
C31 C30 1.368(11) . ?
C5 C4 1.388(10) . ?
C57 C56 1.401(12) . ?
C19 C18 1.364(12) . ?
C1 C1 1.434(13) 2_656 ?
C48 C49 1.380(13) . ?
C30 C29 1.377(12) . ?
C24 C25 1.387(11) . ?
C42 C43 1.372(11) . ?
C56 C55 1.368(15) . ?
C54 C55 1.361(15) . ?
C49 C50 1.376(13) . ?
Cl8B C61B 1.685(16) . ?
C60 Cl6B 1.822(17) . ?
C60 Cl6A 1.748(17) . ?
C60 Cl5A 1.758(15) . ?
C60 Cl5B 1.58(2) . ?
C61B Cl7B 1.768(15) . ?
Cl3A C59 1.60(2) . ?
C59 Cl3B 1.64(3) . ?
C59 Cl4B 1.43(3) . ?
C59 Cl4A 1.51(2) . ?

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
C1 N2 C7 104.8(5) . . ?
C1 N1 C2 106.2(6) . . ?
C36 C39 C40 112.8(5) . . ?
C36 C39 C46 104.0(5) . . ?
C46 C39 C40 112.2(5) . . ?
C52 C39 C36 111.4(5) . . ?
C52 C39 C40 103.4(5) . . ?
C52 C39 C46 113.4(6) . . ?
C35 C36 C39 122.6(6) . . ?
C37 C36 C39 119.5(6) . . ?
C37 C36 C35 117.5(6) . . ?
C20 C15 C14 118.0(6) . . ?
C16 C15 C20 118.2(7) . . ?
C16 C15 C14 123.8(6) . . ?
C34 C33 C6 116.9(7) . . ?
C38 C33 C34 119.9(6) . . ?
C38 C33 C6 123.1(7) . . ?
C22 C21 C14 118.7(6) . . ?
C26 C21 C14 124.2(6) . . ?
C26 C21 C22 117.0(6) . . ?
C45 C40 C39 119.1(6) . . ?
C45 C40 C41 117.7(6) . . ?
C41 C40 C39 123.0(6) . . ?
C32 C27 C14 119.4(6) . . ?
C28 C27 C14 123.0(6) . . ?
C28 C27 C32 117.6(6) . . ?
C19 C20 C15 121.0(7) . . ?
C12 C11 C14 119.7(6) . . ?
C12 C11 C10 117.8(6) . . ?
C10 C11 C14 122.5(6) . . ?
C15 C14 C27 110.8(5) . . ?
C15 C14 C11 110.9(5) . . ?
C21 C14 C15 107.2(5) . . ?
C21 C14 C27 110.1(5) . . ?
C21 C14 C11 110.9(5) . . ?
C27 C14 C11 107.0(5) . . ?
C44 C45 C40 121.3(6) . . ?
C47 C46 C39 118.1(6) . . ?
C51 C46 C39 123.5(6) . . ?
C51 C46 C47 118.1(6) . . ?
C53 C52 C39 123.3(6) . . ?
C53 C52 C57 118.1(7) . . ?
C57 C52 C39 118.1(6) . . ?
C36 C35 C34 120.5(7) . . ?
C42 C41 C40 120.7(7) . . ?
C23 C22 C21 122.0(7) . . ?
N2 C7 C2 110.2(6) . . ?
N2 C7 C6 128.6(6) . . ?
C2 C7 C6 121.1(6) . . ?
C46 C47 C48 122.5(7) . . ?
C11 C12 C13 121.9(6) . . ?
C13 C8 C3 119.8(7) . . ?
C9 C8 C13 118.8(6) . . ?
C9 C8 C3 121.4(6) . . ?
C27 C32 C31 121.3(7) . . ?
C35 C34 C33 119.9(7) . . ?
C8 C13 C12 120.2(7) . . ?
C9 C10 C11 119.3(7) . . ?
C36 C37 C38 122.1(7) . . ?
C21 C26 C25 121.2(7) . . ?
N1 C2 C7 105.1(5) . . ?
N1 C2 C3 132.2(6) . . ?
C3 C2 C7 122.5(6) . . ?
C2 C3 C8 121.5(6) . . ?
C4 C3 C8 123.2(6) . . ?
C4 C3 C2 115.3(6) . . ?
C24 C23 C22 120.1(7) . . ?
C15 C16 C17 120.4(7) . . ?
C7 C6 C33 122.1(6) . . ?
C5 C6 C33 122.4(6) . . ?
C5 C6 C7 115.5(6) . . ?
C43 C44 C45 120.0(7) . . ?
C8 C9 C10 121.9(7) . . ?
C27 C28 C29 120.7(7) . . ?
C33 C38 C37 120.1(7) . . ?
C54 C53 C52 120.0(8) . . ?
C18 C17 C16 120.5(8) . . ?
C46 C51 C50 120.7(8) . . ?
C30 C31 C32 120.6(8) . . ?
C6 C5 C4 122.5(6) . . ?
C3 C4 C5 123.1(6) . . ?
C56 C57 C52 120.3(8) . . ?
C18 C19 C20 120.1(7) . . ?
N2 C1 N1 113.7(6) . . ?
N2 C1 C1 125.0(8) . 2_656 ?
N1 C1 C1 121.3(8) . 2_656 ?
C19 C18 C17 119.9(8) . . ?
C49 C48 C47 118.1(8) . . ?
C31 C30 C29 118.8(7) . . ?
C23 C24 C25 120.0(7) . . ?
C30 C29 C28 121.1(7) . . ?
C24 C25 C26 119.7(7) . . ?
C41 C42 C43 120.7(7) . . ?
C55 C56 C57 120.2(9) . . ?
C42 C43 C44 119.5(7) . . ?
C55 C54 C53 122.0(9) . . ?
C54 C55 C56 119.3(8) . . ?
C50 C49 C48 120.5(8) . . ?
C49 C50 C51 119.9(9) . . ?
Cl1 C58 Cl2 113.9(7) . . ?
Cl6A C60 Cl5A 94.9(10) . . ?
Cl5B C60 Cl6B 103.1(15) . . ?
Cl8B C61B Cl7B 113.6(11) . . ?
Cl4B C59 Cl3B 116.7(19) . . ?
Cl4A C59 Cl3A 128.9(15) . . ?
Cl8A C61A Cl7A 113.9(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
####################################################################### 
# 
# 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_cu_gb135
_database_code_depnum_ccdc_archive 'CCDC 2079258'
loop_
_audit_author_name
_audit_author_address
'Ben Wilson'
;University of Windsor
Canada
;
_audit_update_record             
;
2021-04-21 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_cu_gb135            
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The small crystals were weakly diffracting andthe crystalinity was not optimal
this resulted in weak diffraction and relatively poor data at high angle.
;
_vrf_THETM01_cu_gb135            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The crystals were small and weakly diffracting and no significant diffraction
was observed beyond 0.89 Angstroms.
;
_vrf_PLAT020_cu_gb135            
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.198 Report
RESPONSE: The small crystals were weakly diffracting andthe crystalinity was not optimal
this resulted in weak diffraction and relatively poor data at high angle.
;
# end Validation Reply Form
_audit_creation_date             2020-10-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
bwilson@uwindsor.ca
loeb@uwindsor.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C114 H82 N4, C18 H36 O6'
_chemical_formula_sum            'C132 H118 N4 O6'
_chemical_formula_weight         1856.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0214(9)
_cell_length_b                   13.7471(13)
_cell_length_c                   22.9679(19)
_cell_angle_alpha                94.140(7)
_cell_angle_beta                 93.355(8)
_cell_angle_gamma                100.854(8)
_cell_volume                     2782.6(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6552
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      50.4140
_cell_measurement_theta_min      1.9380
_shelx_estimated_absorpt_T_max   0.950
_shelx_estimated_absorpt_T_min   0.903
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1984
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66583
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        60.015
_diffrn_reflns_theta_max         60.015
_diffrn_reflns_theta_min         1.934
_diffrn_ambient_temperature      170.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -10.27 349.73   2.00   60.00  -9.60 -89.16  31.50    --   180
  2  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 -29.95   52
  3  φ   -339.92  20.08   2.00   38.50 -56.84 -74.16 -59.25    --   180
  4  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 130.05   52
  5  ω      3.93  99.93   2.00   10.00    --   20.69  59.25 159.92   48
  6  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74-109.95   52
  7  ω      3.93  99.93   2.00   10.00    --   20.69  59.25 -20.08   48
  8  ω    -26.23  71.77   2.00   18.40    --   50.69 -83.74-126.05   49
  9  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25  60.08   48
 10  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74  50.05   52
 11  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -19.92   48
 12  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25 140.08   48
 13  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -99.92   48
 14  ω     33.93 129.93   2.00   18.40    --   50.69  59.25-125.08   48
 15  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25-179.92   48
 16  ω     33.93 129.93   2.00   18.40    --   50.69  59.25  30.92   48
 17  ω    -26.23  71.77   2.00   18.40    --   50.69 -83.74  80.95   49
 18  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 170.05   52
 19  ω     33.93 129.93   2.00   18.40    --   50.69  59.25 132.92   48
 20  ω     27.40 123.40   2.00   15.50    --   44.16  59.25 -20.08   48
 21  ω     33.93 129.93   2.00   18.40    --   50.69  59.25-176.08   48
 22  ω     33.93 129.93   2.00   18.40    --   50.69  59.25  81.92   48
 23  φ   -339.92  20.08   2.00   60.00 -71.84 -89.16 -59.25    --   180
 24  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -59.92   48
 25  ω     33.93 129.93   2.00   18.40    --   50.69  59.25 -74.08   48
 26  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74  10.05   52
 27  ω      3.93  99.93   2.00   10.00    --   20.69  59.25  69.92   48
 28  ω     42.40 138.40   2.00   24.20    --   59.16  59.25-110.08   48
 29  ω   -120.80 -16.80   2.00   60.00    --  -89.16  83.74-149.95   52
 30  ω    192.04 288.04   2.00   60.00    --  -89.16 -59.25 100.08   48
 31  ω     42.40 138.40   2.00   24.20    --   59.16  59.25 -20.08   48
 32  ω     42.40 138.40   2.00   24.20    --   59.16  59.25 159.92   48
 33  ω      3.93  99.93   2.00   10.00    --   20.69  59.25-110.08   48
 34  ω     27.40 123.40   2.00   15.50    --   44.16  59.25  69.92   48
 35  ω     27.40 123.40   2.00   15.50    --   44.16  59.25 159.92   48
 36  ω     33.93 129.93   2.00   18.40    --   50.69  59.25 -20.08   48
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1350997000
_diffrn_orient_matrix_UB_12      -0.0415535000
_diffrn_orient_matrix_UB_13      -0.0447205000
_diffrn_orient_matrix_UB_21      -0.1068779000
_diffrn_orient_matrix_UB_22      -0.0103255000
_diffrn_orient_matrix_UB_23      0.0500557000
_diffrn_orient_matrix_UB_31      -0.0268946000
_diffrn_orient_matrix_UB_32      0.1062133000
_diffrn_orient_matrix_UB_33      -0.0064592000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3367
_reflns_number_total             8161
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         8161
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0817
_refine_ls_restrained_S_all      0.906
_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)+(0.1205P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2472
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Hydrogen atoms were included
in calculated positions with isotropic displacement parameters 1.2 times
the isotropic equivalent of their carrier atoms except for methyl groups 
where it is 1.5 times.The crown ether is modeled as disordered over two
positions and required some of the 1,2 and 1,3 distances to be restrained
with the DFIX restraint. In order for the thermal elipsoids to be modeled
in a chemically sensible manner, the RIGU restraint was applied to the crown
ether moiety. In several cases, the ISOR restraint was required due to
unresolved disorder that was unable to be modeled. After modeling the
rotaxane axle and crown ether, there remained a significant amount of 
residual electron density that could not be atomically modeled and was
attributed to disordered solvent molecules. Therefore the solvent mask
function of OLEX2 was applied (1.2 Angstrom probe) which found two crystallographically unique
solvent acessible voids of 209.9 and 274.3 cubic Angstroms calculated to contain
approximately 48 and 50 electrons respectively. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 C66A-C65A
 1.35 with sigma of 0.02
 C67A-C66A
 1.35 with sigma of 0.02
 C65B-C64B
 1.35 with sigma of 0.02
 C64A-C63A
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C64B) \\sim Ueq, Uanis(C65B) \\sim Ueq, Uanis(C62B) \\sim Ueq,
Uanis(C63B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C67A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C65A, O2, C60, C59, C61, C58, C62A, O3B, O1, C63A, C62B, C64A, C63B, O4B,
 C66A, C64B, C67A, C65B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C62A(0.5) H62A(0.5) H62B(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
 H61D(0.5) C66A(0.5) H66A(0.5) H66B(0.5) C64A(0.5) H64A(0.5) H64B(0.5)
 C65B(0.5) H65A(0.5) H65B(0.5) C67A(0.5) H67A(0.5) H67B(0.5) C64B(0.5)
 H64C(0.5) H64D(0.5) C65A(0.5) H65C(0.5) H65D(0.5) O4B(0.5) C63B(0.5) H63A(0.5)
 H63B(0.5) C62B(0.5) H62C(0.5) H62D(0.5) O3B(0.5) C63A(0.5) H63C(0.5) H63D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C62A(H62A,H62B), C60(H60A,H60B), C61(H61A,H61B), C61(H61C,H61D), C59(H59A,
 H59B), C58(H58A,H58B), C66A(H66A,H66B), C64A(H64A,H64B), C65B(H65A,H65B),
 C67A(H67A,H67B), C64B(H64C,H64D), C65A(H65C,H65D), C63B(H63A,H63B), C62B(H62C,
 H62D), C63A(H63C,H63D)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C37(H37), C35(H35), C34(H34), C53(H53), C57(H57), C4(H4), C38(H38),
 C47(H47), C48(H48), C28(H28), C41(H41), C56(H56), C5(H5), C45(H45), C54(H54),
 C16(H16), C20(H20), C55(H55), C32(H32), C49(H49), C24(H24), C51(H51), C23(H23),
  C50(H50), C29(H29), C44(H44), C22(H22), C13(H13), C17(H17), C12(H12),
 C42(H42), C26(H26), C18(H18), C19(H19), C25(H25), C43(H43), C31(H31), C10(H10),
  C9(H9), C30(H30)
;
_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
N1 N 0.9380(4) 0.9439(2) 0.56711(14) 0.0512(10) Uani 1 1 d . . . . .
H1 H 0.983570 0.983824 0.597184 0.061 Uiso 1 1 calc R . . . .
N2 N 0.8695(4) 0.8828(2) 0.47409(14) 0.0530(10) Uani 1 1 d . . . . .
C1 C 0.9522(5) 0.9567(3) 0.51072(19) 0.0519(12) Uani 1 1 d . . . . .
C2 C 0.7957(5) 0.8168(3) 0.51078(19) 0.0551(12) Uani 1 1 d . . . . .
C7 C 0.8375(5) 0.8556(3) 0.56886(18) 0.0534(12) Uani 1 1 d . . . . .
C14 C 0.5154(5) 0.5253(3) 0.26166(17) 0.0483(11) Uani 1 1 d . . . . .
C21 C 0.5810(5) 0.5887(3) 0.21305(18) 0.0500(12) Uani 1 1 d . . . . .
C3 C 0.6919(5) 0.7255(3) 0.49701(19) 0.0598(13) Uani 1 1 d . . . . .
C33 C 0.8197(6) 0.8447(3) 0.67902(19) 0.0550(12) Uani 1 1 d . . . . .
C15 C 0.5741(5) 0.4273(3) 0.2555(2) 0.0556(12) Uani 1 1 d . . . . .
C37 C 0.7472(5) 0.8750(3) 0.7775(2) 0.0600(13) Uani 1 1 d . . . . .
H37 H 0.669148 0.874295 0.803607 0.072 Uiso 1 1 calc R . . . .
C27 C 0.3407(5) 0.5032(4) 0.2552(2) 0.0567(12) Uani 1 1 d . . . . .
C39 C 0.9332(5) 0.9443(3) 0.86400(18) 0.0530(12) Uani 1 1 d . . . . .
C52 C 0.8924(5) 1.0478(3) 0.8757(2) 0.0566(13) Uani 1 1 d . . . . .
C35 C 1.0065(5) 0.9015(3) 0.7594(2) 0.0595(13) Uani 1 1 d . . . . .
H35 H 1.110040 0.919997 0.773228 0.071 Uiso 1 1 calc R . . . .
C8 C 0.6487(5) 0.6778(3) 0.4373(2) 0.0617(13) Uani 1 1 d . . . . .
C34 C 0.9700(6) 0.8718(3) 0.7004(2) 0.0608(13) Uani 1 1 d . . . . .
H34 H 1.048265 0.869898 0.674635 0.073 Uiso 1 1 calc R . . . .
C36 C 0.8962(6) 0.9051(3) 0.79873(19) 0.0551(12) Uani 1 1 d . . . . .
C6 C 0.7768(5) 0.8085(3) 0.61697(19) 0.0598(13) Uani 1 1 d . . . . .
C40 C 1.1055(6) 0.9555(4) 0.8802(2) 0.0621(13) Uani 1 1 d . . . . .
C53 C 0.9486(5) 1.1052(4) 0.9276(2) 0.0660(14) Uani 1 1 d . . . . .
H53 H 1.010081 1.079336 0.955218 0.079 Uiso 1 1 calc R . . . .
C11 C 0.5652(5) 0.5809(3) 0.32300(19) 0.0565(13) Uani 1 1 d . . . . .
C57 C 0.8040(5) 1.0879(4) 0.8369(2) 0.0659(14) Uani 1 1 d . . . . .
H57 H 0.764650 1.050835 0.801013 0.079 Uiso 1 1 calc R . . . .
C4 C 0.6325(6) 0.6815(4) 0.5450(2) 0.0718(15) Uani 1 1 d . . . . .
H4 H 0.559874 0.621366 0.538379 0.086 Uiso 1 1 calc R . . . .
C46 C 0.8405(5) 0.8676(4) 0.9004(2) 0.0608(13) Uani 1 1 d . . . . .
C38 C 0.7093(5) 0.8457(3) 0.7184(2) 0.0596(13) Uani 1 1 d . . . . .
H38 H 0.605713 0.825956 0.704808 0.071 Uiso 1 1 calc R . . . .
O2 O 1.1130(7) 1.0984(3) 0.66719(19) 0.1207(15) Uani 1 1 d . U . . .
C47 C 0.7629(5) 0.8929(4) 0.9478(2) 0.0661(14) Uani 1 1 d . . . . .
H47 H 0.764469 0.961003 0.959087 0.079 Uiso 1 1 calc R . . . .
C48 C 0.6822(6) 0.8195(5) 0.9795(2) 0.0774(16) Uani 1 1 d . . . . .
H48 H 0.630094 0.838169 1.011950 0.093 Uiso 1 1 calc R . . . .
C28 C 0.2529(6) 0.4098(4) 0.2496(2) 0.0686(14) Uani 1 1 d . . . . .
H28 H 0.301124 0.354101 0.246285 0.082 Uiso 1 1 calc R . . . .
C41 C 1.1661(6) 0.8922(4) 0.9147(2) 0.0701(14) Uani 1 1 d . . . . .
H41 H 1.101473 0.838943 0.930213 0.084 Uiso 1 1 calc R . . . .
C56 C 0.7710(6) 1.1819(4) 0.8492(2) 0.0738(15) Uani 1 1 d . . . . .
H56 H 0.709266 1.208085 0.821843 0.089 Uiso 1 1 calc R . . . .
C5 C 0.6734(6) 0.7208(3) 0.6026(2) 0.0711(15) Uani 1 1 d . . . . .
H5 H 0.628425 0.685788 0.633316 0.085 Uiso 1 1 calc R . . . .
C45 C 1.2056(6) 1.0335(4) 0.8600(2) 0.0720(15) Uani 1 1 d . . . . .
H45 H 1.166390 1.079797 0.837728 0.086 Uiso 1 1 calc R . . . .
C54 C 0.9175(6) 1.1985(4) 0.9398(2) 0.0731(15) Uani 1 1 d . . . . .
H54 H 0.958318 1.236368 0.975338 0.088 Uiso 1 1 calc R . . . .
C16 C 0.6417(5) 0.3877(4) 0.3013(2) 0.0709(15) Uani 1 1 d . . . . .
H16 H 0.653458 0.421151 0.339459 0.085 Uiso 1 1 calc R . . . .
C20 C 0.5610(6) 0.3749(4) 0.2014(2) 0.0694(14) Uani 1 1 d . . . . .
H20 H 0.515678 0.400763 0.169015 0.083 Uiso 1 1 calc R . . . .
C55 C 0.8275(6) 1.2369(4) 0.9009(3) 0.0744(15) Uani 1 1 d . . . . .
H55 H 0.804445 1.300847 0.909475 0.089 Uiso 1 1 calc R . . . .
C32 C 0.2658(6) 0.5817(4) 0.2644(2) 0.0829(17) Uani 1 1 d . . . . .
H32 H 0.323090 0.647349 0.271601 0.099 Uiso 1 1 calc R . . . .
C49 C 0.6783(7) 0.7211(5) 0.9637(2) 0.0865(18) Uani 1 1 d . . . . .
H49 H 0.623013 0.671677 0.985165 0.104 Uiso 1 1 calc R . . . .
C24 C 0.7126(7) 0.6979(4) 0.1244(2) 0.0785(16) Uani 1 1 d . . . . .
H24 H 0.757072 0.738036 0.095651 0.094 Uiso 1 1 calc R . . . .
C51 C 0.8357(6) 0.7654(4) 0.8857(2) 0.0765(16) Uani 1 1 d . . . . .
H51 H 0.889035 0.745538 0.853837 0.092 Uiso 1 1 calc R . . . .
C23 C 0.8003(6) 0.6585(4) 0.1623(2) 0.0770(16) Uani 1 1 d . . . . .
H23 H 0.906740 0.668861 0.159688 0.092 Uiso 1 1 calc R . . . .
C50 C 0.7541(7) 0.6937(4) 0.9171(2) 0.0865(18) Uani 1 1 d . . . . .
H50 H 0.750660 0.625307 0.906191 0.104 Uiso 1 1 calc R . . . .
C29 C 0.0980(6) 0.3935(4) 0.2486(2) 0.0802(17) Uani 1 1 d . . . . .
H29 H 0.041282 0.327462 0.244862 0.096 Uiso 1 1 calc R . . . .
C44 C 1.3600(7) 1.0454(5) 0.8713(3) 0.0848(17) Uani 1 1 d . . . . .
H44 H 1.425540 1.097595 0.855306 0.102 Uiso 1 1 calc R . . . .
C22 C 0.7332(6) 0.6025(4) 0.2053(2) 0.0738(15) Uani 1 1 d . . . . .
H22 H 0.795477 0.572495 0.230397 0.089 Uiso 1 1 calc R . . . .
C13 C 0.5179(6) 0.6074(4) 0.4253(2) 0.0848(18) Uani 1 1 d . . . . .
H13 H 0.453108 0.591016 0.455733 0.102 Uiso 1 1 calc R . . . .
O1 O 1.3023(8) 0.9608(6) 0.6321(3) 0.163(2) Uani 1 1 d . U . . .
C17 C 0.6931(6) 0.2977(5) 0.2915(4) 0.0939(19) Uani 1 1 d . . . . .
H17 H 0.740541 0.271132 0.323033 0.113 Uiso 1 1 calc R . . . .
C12 C 0.4790(6) 0.5601(4) 0.3699(2) 0.0802(17) Uani 1 1 d . . . . .
H12 H 0.388865 0.511059 0.363836 0.096 Uiso 1 1 calc R . . . .
C42 C 1.3229(8) 0.9069(5) 0.9268(2) 0.0855(17) Uani 1 1 d . . . . .
H42 H 1.363609 0.863161 0.950631 0.103 Uiso 1 1 calc R . . . .
C26 C 0.4918(6) 0.6259(4) 0.1718(2) 0.0765(15) Uani 1 1 d . . . . .
H26 H 0.385109 0.614789 0.173681 0.092 Uiso 1 1 calc R . . . .
C18 C 0.6758(7) 0.2492(5) 0.2380(4) 0.099(2) Uani 1 1 d . . . . .
H18 H 0.709319 0.188002 0.231977 0.119 Uiso 1 1 calc R . . . .
C19 C 0.6104(7) 0.2876(5) 0.1924(3) 0.0880(18) Uani 1 1 d . . . . .
H19 H 0.599211 0.253692 0.154351 0.106 Uiso 1 1 calc R . . . .
C25 C 0.5590(7) 0.6793(4) 0.1279(2) 0.0884(18) Uani 1 1 d . . . . .
H25 H 0.496940 0.703530 0.099744 0.106 Uiso 1 1 calc R . . . .
C43 C 1.4192(7) 0.9828(6) 0.9052(3) 0.0906(18) Uani 1 1 d . . . . .
H43 H 1.525417 0.991683 0.913640 0.109 Uiso 1 1 calc R . . . .
C31 C 0.1111(7) 0.5668(5) 0.2634(3) 0.108(2) Uani 1 1 d . . . . .
H31 H 0.061813 0.621473 0.269769 0.130 Uiso 1 1 calc R . . . .
C10 C 0.6964(6) 0.6486(5) 0.3360(2) 0.101(2) Uani 1 1 d . . . . .
H10 H 0.761358 0.664919 0.305621 0.122 Uiso 1 1 calc R . . . .
C9 C 0.7387(7) 0.6944(5) 0.3915(2) 0.109(2) Uani 1 1 d . . . . .
H9 H 0.833443 0.738873 0.398218 0.131 Uiso 1 1 calc R . . . .
C62A C 0.902(3) 1.1877(16) 0.6272(11) 0.097(6) Uani 0.5 1 d . U P A 1
H62A H 0.961972 1.254512 0.640145 0.117 Uiso 0.5 1 calc R . P A 1
H62B H 0.961846 1.152970 0.600893 0.117 Uiso 0.5 1 calc R . P A 1
C30 C 0.0268(7) 0.4703(5) 0.2530(3) 0.119(3) Uani 1 1 d . . . . .
H30 H -0.080601 0.459283 0.249008 0.143 Uiso 1 1 calc R . . . .
C60 C 1.0160(9) 1.1332(5) 0.7054(3) 0.114(2) Uani 1 1 d . U . . .
H60A H 1.063110 1.200724 0.722897 0.136 Uiso 1 1 calc R . . . .
H60B H 0.998539 1.088997 0.737506 0.136 Uiso 1 1 calc R . . . .
C61 C 0.8694(10) 1.1363(5) 0.6734(3) 0.125(2) Uani 1 1 d . U . . .
H61A H 0.814403 1.068056 0.660512 0.150 Uiso 0.5 1 calc R . P A 1
H61B H 0.805299 1.169073 0.698851 0.150 Uiso 0.5 1 calc R . P A 1
H61C H 0.790367 1.136900 0.701463 0.150 Uiso 0.5 1 calc R . P A 2
H61D H 0.838530 1.076091 0.645781 0.150 Uiso 0.5 1 calc R . P A 2
C59 C 1.2557(11) 1.0958(7) 0.6946(4) 0.149(3) Uani 1 1 d . U . . .
H59A H 1.243815 1.047543 0.724760 0.178 Uiso 1 1 calc R . . . .
H59B H 1.300557 1.162147 0.714238 0.178 Uiso 1 1 calc R . . . .
C58 C 1.3573(10) 1.0671(8) 0.6516(4) 0.158(3) Uani 1 1 d . U . . .
H58A H 1.462108 1.077437 0.669600 0.189 Uiso 1 1 calc R . . . .
H58B H 1.356824 1.107921 0.617825 0.189 Uiso 1 1 calc R . . . .
C66A C 0.6946(19) 1.1711(12) 0.4431(6) 0.122(5) Uani 0.5 1 d D U P A 1
H66A H 0.655218 1.214328 0.415856 0.147 Uiso 0.5 1 calc R . P A 1
H66B H 0.805019 1.179992 0.439311 0.147 Uiso 0.5 1 calc R . P A 1
C64A C 0.731(3) 1.1553(18) 0.5474(11) 0.172(7) Uani 0.5 1 d D U P A 1
H64A H 0.650531 1.096979 0.552023 0.207 Uiso 0.5 1 calc R . P A 1
H64B H 0.815719 1.129077 0.530837 0.207 Uiso 0.5 1 calc R . P A 1
C65B C 0.583(4) 1.066(3) 0.3870(13) 0.252(11) Uani 0.5 1 d D U P A 2
H65A H 0.491447 1.017758 0.371170 0.302 Uiso 0.5 1 calc R . P A 2
H65B H 0.575669 1.131698 0.373643 0.302 Uiso 0.5 1 calc R . P A 2
C67A C 0.634(3) 1.0771(18) 0.4242(9) 0.157(8) Uani 0.5 1 d D U P A 1
H67A H 0.522999 1.071275 0.416908 0.188 Uiso 0.5 1 calc R . P A 1
H67B H 0.650788 1.033687 0.455544 0.188 Uiso 0.5 1 calc R . P A 1
C64B C 0.591(4) 1.071(3) 0.4449(12) 0.239(11) Uani 0.5 1 d D U P A 2
H64C H 0.600547 1.003269 0.454298 0.287 Uiso 0.5 1 calc R . P A 2
H64D H 0.487805 1.077966 0.454767 0.287 Uiso 0.5 1 calc R . P A 2
C65A C 0.6726(18) 1.2098(14) 0.5038(5) 0.107(4) Uani 0.5 1 d D U P A 1
H65C H 0.723621 1.280407 0.510236 0.128 Uiso 0.5 1 calc R . P A 1
H65D H 0.563148 1.206474 0.507859 0.128 Uiso 0.5 1 calc R . P A 1
O4B O 0.694(2) 1.1386(16) 0.4921(10) 0.228(7) Uani 0.5 1 d . U P A 2
C63B C 0.781(2) 1.2194(16) 0.5406(9) 0.149(6) Uani 0.5 1 d . U P A 2
H63A H 0.887924 1.211349 0.541178 0.179 Uiso 0.5 1 calc R . P A 2
H63B H 0.778593 1.284024 0.524608 0.179 Uiso 0.5 1 calc R . P A 2
C62B C 0.751(3) 1.234(2) 0.6012(11) 0.141(6) Uani 0.5 1 d . U P A 2
H62C H 0.663332 1.182932 0.609552 0.169 Uiso 0.5 1 calc R . P A 2
H62D H 0.724912 1.299955 0.608886 0.169 Uiso 0.5 1 calc R . P A 2
O3B O 0.884(2) 1.2262(11) 0.6406(7) 0.109(4) Uani 0.5 1 d . U P A 2
C63A C 0.779(4) 1.196(3) 0.6005(13) 0.215(16) Uani 0.5 1 d D U P A 1
H63C H 0.782123 1.267704 0.599563 0.258 Uiso 0.5 1 calc R . P A 1
H63D H 0.698775 1.170817 0.626252 0.258 Uiso 0.5 1 calc R . 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
N1 C1 1.330(5) . ?
N1 C7 1.376(5) . ?
N2 C1 1.347(5) . ?
N2 C2 1.387(5) . ?
C1 C1 1.467(8) 2_776 ?
C2 C7 1.403(6) . ?
C2 C3 1.421(6) . ?
C7 C6 1.407(5) . ?
C14 C21 1.542(5) . ?
C14 C15 1.538(6) . ?
C14 C27 1.544(6) . ?
C14 C11 1.553(6) . ?
C21 C22 1.374(6) . ?
C21 C26 1.394(6) . ?
C3 C8 1.474(6) . ?
C3 C4 1.383(6) . ?
C33 C34 1.387(6) . ?
C33 C6 1.479(6) . ?
C33 C38 1.385(6) . ?
C15 C16 1.380(6) . ?
C15 C20 1.379(6) . ?
C37 C36 1.379(6) . ?
C37 C38 1.391(6) . ?
C27 C28 1.369(6) . ?
C27 C32 1.387(7) . ?
C39 C52 1.544(6) . ?
C39 C36 1.551(6) . ?
C39 C40 1.553(6) . ?
C39 C46 1.545(6) . ?
C52 C53 1.394(6) . ?
C52 C57 1.374(6) . ?
C35 C34 1.388(6) . ?
C35 C36 1.388(6) . ?
C8 C13 1.378(6) . ?
C8 C9 1.373(6) . ?
C6 C5 1.385(6) . ?
C40 C41 1.384(7) . ?
C40 C45 1.392(6) . ?
C53 C54 1.377(7) . ?
C11 C12 1.381(6) . ?
C11 C10 1.364(6) . ?
C57 C56 1.392(7) . ?
C4 C5 1.393(6) . ?
C46 C47 1.389(6) . ?
C46 C51 1.412(7) . ?
O2 C60 1.398(7) . ?
O2 C59 1.407(9) . ?
C47 C48 1.403(7) . ?
C48 C49 1.368(7) . ?
C28 C29 1.371(6) . ?
C41 C42 1.399(7) . ?
C56 C55 1.377(7) . ?
C45 C44 1.379(7) . ?
C54 C55 1.372(7) . ?
C16 C17 1.409(8) . ?
C20 C19 1.364(7) . ?
C32 C31 1.370(7) . ?
C49 C50 1.372(7) . ?
C24 C23 1.352(7) . ?
C24 C25 1.369(7) . ?
C51 C50 1.388(7) . ?
C23 C22 1.391(6) . ?
C29 C30 1.336(8) . ?
C44 C43 1.360(8) . ?
C13 C12 1.380(6) . ?
O1 C58 1.479(10) . ?
O1 C65B 1.25(3) 2_776 ?
O1 C67A 1.54(2) 2_776 ?
C17 C18 1.341(8) . ?
C42 C43 1.370(8) . ?
C26 C25 1.390(7) . ?
C18 C19 1.360(8) . ?
C31 C30 1.395(8) . ?
C10 C9 1.379(7) . ?
C62A C61 1.33(3) . ?
C62A C63A 1.26(4) . ?
C60 C61 1.484(9) . ?
C61 O3B 1.483(18) . ?
C59 C58 1.469(11) . ?
C66A C67A 1.336(17) . ?
C66A C65A 1.493(14) . ?
C64A C65A 1.43(3) . ?
C64A C63A 1.318(18) . ?
C65B C64B 1.324(18) . ?
C64B O4B 1.52(3) . ?
O4B C63B 1.58(3) . ?
C63B C62B 1.44(3) . ?
C62B O3B 1.48(3) . ?

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
C1 N1 C7 106.0(3) . . ?
C1 N2 C2 104.4(3) . . ?
N1 C1 N2 114.1(3) . . ?
N1 C1 C1 123.8(5) . 2_776 ?
N2 C1 C1 122.1(5) . 2_776 ?
N2 C2 C7 108.2(4) . . ?
N2 C2 C3 130.0(4) . . ?
C7 C2 C3 121.7(4) . . ?
N1 C7 C2 107.3(3) . . ?
N1 C7 C6 130.2(4) . . ?
C2 C7 C6 122.5(4) . . ?
C21 C14 C27 110.9(4) . . ?
C21 C14 C11 110.7(3) . . ?
C15 C14 C21 107.2(3) . . ?
C15 C14 C27 109.7(3) . . ?
C15 C14 C11 110.8(4) . . ?
C27 C14 C11 107.6(4) . . ?
C22 C21 C14 119.8(4) . . ?
C22 C21 C26 116.5(4) . . ?
C26 C21 C14 123.4(4) . . ?
C2 C3 C8 124.7(4) . . ?
C4 C3 C2 114.5(4) . . ?
C4 C3 C8 120.7(4) . . ?
C34 C33 C6 121.6(4) . . ?
C38 C33 C34 118.0(4) . . ?
C38 C33 C6 120.2(4) . . ?
C16 C15 C14 124.0(4) . . ?
C20 C15 C14 119.1(5) . . ?
C20 C15 C16 116.9(5) . . ?
C36 C37 C38 121.0(4) . . ?
C28 C27 C14 124.5(5) . . ?
C28 C27 C32 116.4(5) . . ?
C32 C27 C14 118.4(4) . . ?
C52 C39 C36 111.0(4) . . ?
C52 C39 C40 107.4(4) . . ?
C52 C39 C46 110.9(4) . . ?
C36 C39 C40 109.8(4) . . ?
C46 C39 C36 106.8(3) . . ?
C46 C39 C40 110.9(4) . . ?
C53 C52 C39 119.4(4) . . ?
C57 C52 C39 123.3(4) . . ?
C57 C52 C53 117.4(5) . . ?
C34 C35 C36 122.0(4) . . ?
C13 C8 C3 121.1(4) . . ?
C9 C8 C3 123.2(4) . . ?
C9 C8 C13 115.6(4) . . ?
C33 C34 C35 120.2(4) . . ?
C37 C36 C39 119.4(4) . . ?
C37 C36 C35 117.5(4) . . ?
C35 C36 C39 123.1(4) . . ?
C7 C6 C33 124.7(4) . . ?
C5 C6 C7 114.9(4) . . ?
C5 C6 C33 120.4(4) . . ?
C41 C40 C39 123.3(5) . . ?
C41 C40 C45 117.5(5) . . ?
C45 C40 C39 119.2(5) . . ?
C54 C53 C52 121.7(5) . . ?
C12 C11 C14 120.7(4) . . ?
C10 C11 C14 124.5(4) . . ?
C10 C11 C12 114.8(4) . . ?
C52 C57 C56 121.2(5) . . ?
C3 C4 C5 123.5(4) . . ?
C47 C46 C39 123.8(4) . . ?
C47 C46 C51 117.4(5) . . ?
C51 C46 C39 118.8(4) . . ?
C33 C38 C37 121.3(4) . . ?
C60 O2 C59 113.0(6) . . ?
C46 C47 C48 121.0(5) . . ?
C49 C48 C47 120.3(5) . . ?
C27 C28 C29 122.6(5) . . ?
C40 C41 C42 119.7(5) . . ?
C55 C56 C57 120.3(5) . . ?
C6 C5 C4 122.8(4) . . ?
C44 C45 C40 121.9(6) . . ?
C55 C54 C53 120.1(5) . . ?
C15 C16 C17 120.0(5) . . ?
C19 C20 C15 122.7(6) . . ?
C54 C55 C56 119.3(5) . . ?
C31 C32 C27 121.6(5) . . ?
C48 C49 C50 120.1(5) . . ?
C23 C24 C25 119.3(5) . . ?
C50 C51 C46 120.9(5) . . ?
C24 C23 C22 119.4(5) . . ?
C49 C50 C51 120.4(5) . . ?
C30 C29 C28 120.2(5) . . ?
C43 C44 C45 120.4(6) . . ?
C21 C22 C23 123.0(5) . . ?
C8 C13 C12 121.4(4) . . ?
C58 O1 C67A 115.7(11) . 2_776 ?
C65B O1 C58 103.3(18) 2_776 . ?
C65B O1 C67A 37.2(17) 2_776 2_776 ?
C18 C17 C16 120.6(6) . . ?
C13 C12 C11 123.0(4) . . ?
C43 C42 C41 121.6(6) . . ?
C25 C26 C21 120.0(5) . . ?
C17 C18 C19 120.1(7) . . ?
C18 C19 C20 119.7(6) . . ?
C24 C25 C26 121.5(6) . . ?
C44 C43 C42 118.9(6) . . ?
C32 C31 C30 119.3(6) . . ?
C11 C10 C9 122.8(5) . . ?
C8 C9 C10 122.3(5) . . ?
C63A C62A C61 108(3) . . ?
C29 C30 C31 119.6(6) . . ?
O2 C60 C61 110.0(6) . . ?
C62A C61 C60 106.7(15) . . ?
C60 C61 O3B 110.2(10) . . ?
O2 C59 C58 110.7(7) . . ?
C59 C58 O1 107.6(8) . . ?
C67A C66A C65A 119.8(16) . . ?
C63A C64A C65A 122(2) . . ?
O1 C65B C64B 111(3) 2_776 . ?
C66A C67A O1 114.0(17) . 2_776 ?
C65B C64B O4B 133(3) . . ?
C64A C65A C66A 112.6(15) . . ?
C64B O4B C63B 171(3) . . ?
C62B C63B O4B 129(2) . . ?
C63B C62B O3B 112(2) . . ?
C62B O3B C61 116.3(17) . . ?
C62A C63A C64A 125(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 209.9 48.0 ?
2 0.175 0.500 0.000 274.3 51.2 ?
3 0.497 0.992 0.754 12.7 0.0 ?
4 0.503 0.008 0.246 12.7 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.201
_oxdiff_exptl_absorpt_empirical_full_min 0.843
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
