# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_bhw319_1_0m
_database_code_depnum_ccdc_archive 'CCDC 2049899'
loop_
_audit_author_name
_audit_author_address
'Wilson B.H.'
;University of Windsor
Canada
;
_audit_update_record             
;
2020-12-12 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_bhw319_1_0m         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals were very small and weakly diffracting and no 
significant reflections were observed beyond 1.0 \%A.
;
_vrf_PLAT341_bhw319_1_0m         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02739 Ang.  
RESPONSE: The low resolution data obtained due to the small, weakly 
diffracting crystals results in a low C-C bond precision.
;
# end Validation Reply Form
_audit_creation_date             2019-11-28
_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
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H28 Br2 N4 O4, C16 H32 O8, C H4 O'
_chemical_formula_sum            'C55 H64 Br2 N4 O13'
_chemical_formula_weight         1148.92
_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'
Br Br -0.6763 1.2805 '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                   9.3936(9)
_cell_length_b                   16.7830(16)
_cell_length_c                   17.8687(17)
_cell_angle_alpha                75.171(4)
_cell_angle_beta                 83.247(4)
_cell_angle_gamma                84.427(4)
_cell_volume                     2697.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      50.33
_cell_measurement_theta_min      2.57
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.791
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1425 before and 0.0860 after correction. The Ratio of minimum to maximum transmission is 0.7485. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_special_detail            
;
Despite screening a number of crystals, all very small needles which resulted in weak diffraction.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1374
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35147
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        50.895
_diffrn_reflns_theta_max         50.894
_diffrn_reflns_theta_min         2.570
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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                   'I\mS Microfocus Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3866
_reflns_number_total             5559
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         0.763
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     408
_refine_ls_R_factor_all          0.2112
_refine_ls_R_factor_gt           0.1520
_refine_ls_restrained_S_all      1.292
_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)+61.5421P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2761
_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. The low resolution data 
resulted the thermal parameters of the rotaxane thread being chemically 
unrealistic while some were NPD. Therefore the RIGU restraint was applied
to this part of the molecule. Most of the atoms of the crown ether macrocycle 
displayed chemically sensible thermal parameters and required no restraints. 
However, several atoms required the SIMU restraint in order for the thermal
parameteres to be modeled in a chemnically sensible manner. The [2]rotaxane
co-crystallied with a methanol solvent molecule that required the SIUM restraint 
inorder for the thermal parameters of the oxygen and carbon atoms to posses 
chemically sensible values.   
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C55 \\sim O13: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O13 \\sim C55: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O10 \\sim C48: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C47 \\sim O9: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
3. Rigid body (RIGU) restrains
 Br1, Br2, O1, O2, O3, O4, N1, H1, N2, N3, H3, N4, C1, C2, C3, C4, H4, C5, H5,
 C6, C7, C8, C9, H9, C10, H10, C11, C12, H12, C13, H13, C14, C15, C16, C17, H17,
  C18, H18, C19, C20, C21, C22, H22, C23, H23, C24, C25, H25, C26, H26, C27,
 C28, H28A, H28B, C29, H29A, H29B, H29C, C30, C31, H31, C32, H32, C33, C34, H34,
  C35, H35, C36, C37, H37A, H37B, C38, H38A, H38B, H38C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C31(H31), C32(H32),
  C34(H34), C35(H35)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C55(H55A,H55B,H55C)
4.d Idealised tetrahedral OH refined as rotating group:
 O13(H13A)
;
_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
Br1 Br 1.1503(2) 0.93397(13) 0.04576(12) 0.0422(7) Uani 1 1 d . U . . .
Br2 Br 0.9507(2) 1.16167(12) 0.29592(13) 0.0421(7) Uani 1 1 d . U . . .
O1 O 0.0975(16) 0.6696(9) 0.9192(8) 0.068(5) Uani 1 1 d . U . . .
O2 O 0.2921(14) 0.7375(9) 0.8643(8) 0.058(4) Uani 1 1 d . U . . .
O3 O 0.2998(14) 0.2709(8) 0.1990(8) 0.056(4) Uani 1 1 d . U . . .
O4 O 0.2599(14) 0.4019(8) 0.1304(8) 0.052(4) Uani 1 1 d . U . . .
N1 N 0.8416(14) 0.9808(8) 0.2845(8) 0.029(3) Uani 1 1 d . U . . .
H1 H 0.794580 0.996839 0.324331 0.035 Uiso 1 1 calc R U . . .
N2 N 0.9082(14) 0.9036(8) 0.1985(8) 0.029(3) Uani 1 1 d . U . . .
N3 N 0.4277(13) 0.5943(8) 0.4058(8) 0.024(3) Uani 1 1 d . U . . .
H3 H 0.455330 0.586094 0.359377 0.028 Uiso 1 1 calc R U . . .
N4 N 0.4150(14) 0.6505(8) 0.5089(8) 0.027(3) Uani 1 1 d . U . . .
C1 C 0.8298(16) 0.9095(10) 0.2641(10) 0.021(4) Uani 1 1 d . U . . .
C2 C 0.9425(17) 1.0235(10) 0.2299(9) 0.022(4) Uani 1 1 d . U . . .
C3 C 1.0015(18) 1.0975(11) 0.2224(10) 0.028(4) Uani 1 1 d . U . . .
C4 C 1.1038(18) 1.1232(12) 0.1607(10) 0.033(4) Uani 1 1 d . U . . .
H4 H 1.147378 1.173471 0.155067 0.040 Uiso 1 1 calc R U . . .
C5 C 1.144(2) 1.0756(11) 0.1064(10) 0.035(5) Uani 1 1 d . U . . .
H5 H 1.211383 1.095255 0.063175 0.043 Uiso 1 1 calc R U . . .
C6 C 1.0871(19) 1.0015(10) 0.1151(10) 0.028(4) Uani 1 1 d . U . . .
C7 C 0.9811(19) 0.9740(11) 0.1761(10) 0.029(4) Uani 1 1 d . U . . .
C8 C 0.7364(16) 0.8465(10) 0.3081(9) 0.021(4) Uani 1 1 d . U . . .
C9 C 0.7455(17) 0.7684(11) 0.2894(10) 0.030(4) Uani 1 1 d . U . . .
H9 H 0.811297 0.758826 0.247469 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6610(16) 0.7071(11) 0.3310(10) 0.026(4) Uani 1 1 d . U . . .
H10 H 0.669351 0.655701 0.317223 0.032 Uiso 1 1 calc R U . . .
C11 C 0.5632(16) 0.7180(10) 0.3928(10) 0.023(4) Uani 1 1 d . U . . .
C12 C 0.5555(17) 0.7932(10) 0.4127(9) 0.023(4) Uani 1 1 d . U . . .
H12 H 0.490734 0.802063 0.455247 0.027 Uiso 1 1 calc R U . . .
C13 C 0.6413(17) 0.8552(11) 0.3710(10) 0.026(4) Uani 1 1 d . U . . .
H13 H 0.634471 0.905755 0.386309 0.031 Uiso 1 1 calc R U . . .
C14 C 0.4693(18) 0.6544(10) 0.4362(10) 0.026(4) Uani 1 1 d . U . . .
C15 C 0.3278(17) 0.5841(10) 0.5269(10) 0.021(3) Uani 1 1 d . U . . .
C16 C 0.2434(17) 0.5507(11) 0.5969(10) 0.028(4) Uani 1 1 d . U . . .
C17 C 0.1652(17) 0.4834(11) 0.5948(10) 0.029(4) Uani 1 1 d . U . . .
H17 H 0.103554 0.459915 0.639498 0.035 Uiso 1 1 calc R U . . .
C18 C 0.1743(17) 0.4506(11) 0.5315(10) 0.030(4) Uani 1 1 d . U . . .
H18 H 0.120274 0.404406 0.535603 0.036 Uiso 1 1 calc R U . . .
C19 C 0.2571(17) 0.4802(10) 0.4613(10) 0.025(4) Uani 1 1 d . U . . .
C20 C 0.3328(17) 0.5488(10) 0.4629(10) 0.023(4) Uani 1 1 d . U . . .
C21 C 0.2327(18) 0.5838(11) 0.6673(10) 0.030(4) Uani 1 1 d . U . . .
C22 C 0.3435(18) 0.6299(10) 0.6799(10) 0.029(4) Uani 1 1 d . U . . .
H22 H 0.425242 0.640073 0.643021 0.035 Uiso 1 1 calc R U . . .
C23 C 0.3322(19) 0.6597(11) 0.7452(11) 0.040(5) Uani 1 1 d . U . . .
H23 H 0.407692 0.689260 0.753567 0.048 Uiso 1 1 calc R U . . .
C24 C 0.2133(19) 0.6475(12) 0.7989(11) 0.037(4) Uani 1 1 d . U . . .
C25 C 0.1053(19) 0.6022(12) 0.7865(11) 0.041(5) Uani 1 1 d . U . . .
H25 H 0.024386 0.591676 0.823900 0.050 Uiso 1 1 calc R U . . .
C26 C 0.1137(19) 0.5726(11) 0.7213(10) 0.034(4) Uani 1 1 d . U . . .
H26 H 0.036747 0.543939 0.713144 0.041 Uiso 1 1 calc R U . . .
C27 C 0.193(2) 0.6828(12) 0.8680(12) 0.046(5) Uani 1 1 d . U . . .
C28 C 0.280(2) 0.7778(17) 0.9289(14) 0.081(8) Uani 1 1 d . U . . .
H28A H 0.302740 0.737435 0.977685 0.097 Uiso 1 1 calc R U . . .
H28B H 0.180864 0.802829 0.936833 0.097 Uiso 1 1 calc R U . . .
C29 C 0.384(3) 0.8424(18) 0.9059(16) 0.101(10) Uani 1 1 d . U . . .
H29A H 0.350897 0.886723 0.862933 0.152 Uiso 1 1 calc GR U . . .
H29B H 0.478125 0.818176 0.889240 0.152 Uiso 1 1 calc GR U . . .
H29C H 0.393477 0.865138 0.950364 0.152 Uiso 1 1 calc GR U . . .
C30 C 0.2591(18) 0.4468(11) 0.3938(10) 0.030(4) Uani 1 1 d . U . . .
C31 C 0.2568(18) 0.4959(11) 0.3201(10) 0.030(4) Uani 1 1 d . U . . .
H31 H 0.251132 0.554241 0.312380 0.036 Uiso 1 1 calc R U . . .
C32 C 0.2625(19) 0.4632(12) 0.2567(11) 0.037(5) Uani 1 1 d . U . . .
H32 H 0.262263 0.499166 0.206090 0.045 Uiso 1 1 calc R U . . .
C33 C 0.2687(19) 0.3785(12) 0.2653(11) 0.037(4) Uani 1 1 d . U . . .
C34 C 0.2681(18) 0.3301(12) 0.3383(11) 0.039(4) Uani 1 1 d . U . . .
H34 H 0.270917 0.271889 0.345539 0.046 Uiso 1 1 calc R U . . .
C35 C 0.2636(17) 0.3611(11) 0.4029(11) 0.030(4) Uani 1 1 d . U . . .
H35 H 0.263620 0.324690 0.453339 0.036 Uiso 1 1 calc R U . . .
C36 C 0.2773(19) 0.3450(13) 0.1961(12) 0.040(5) Uani 1 1 d . U . . .
C37 C 0.262(2) 0.3737(14) 0.0607(12) 0.063(6) Uani 1 1 d . U . . .
H37A H 0.189868 0.332140 0.067962 0.076 Uiso 1 1 calc R U . . .
H37B H 0.357657 0.348011 0.047872 0.076 Uiso 1 1 calc R U . . .
C38 C 0.226(3) 0.4464(16) -0.0020(14) 0.103(10) Uani 1 1 d . U . . .
H38A H 0.210426 0.428450 -0.048275 0.155 Uiso 1 1 calc GR U . . .
H38B H 0.305795 0.482702 -0.014548 0.155 Uiso 1 1 calc GR U . . .
H38C H 0.138732 0.476438 0.014974 0.155 Uiso 1 1 calc GR U . . .
O5 O 0.7040(12) 1.0271(7) 0.4226(7) 0.033(3) Uani 1 1 d . . . . .
O6 O 0.4693(13) 1.0423(7) 0.3428(7) 0.038(3) Uani 1 1 d . . . . .
O7 O 0.4554(13) 0.9572(7) 0.2145(7) 0.038(3) Uani 1 1 d . . . . .
O8 O 0.5636(14) 0.7837(8) 0.1309(9) 0.055(4) Uani 1 1 d . . . . .
O9 O 0.8439(15) 0.6858(10) 0.1319(9) 0.066(4) Uani 1 1 d . U . . .
O10 O 1.0573(15) 0.6761(9) 0.2425(8) 0.060(4) Uani 1 1 d . U . . .
O11 O 1.1334(18) 0.7972(11) 0.3654(12) 0.087(6) Uani 1 1 d . . . . .
O12 O 0.9358(12) 0.9000(8) 0.4616(7) 0.039(3) Uani 1 1 d . . . . .
C39 C 0.607(2) 1.0988(12) 0.4157(11) 0.039(5) Uani 1 1 d . . . . .
H39A H 0.660142 1.147135 0.415747 0.046 Uiso 1 1 calc R . . . .
H39B H 0.532612 1.090716 0.460386 0.046 Uiso 1 1 calc R . . . .
C40 C 0.5386(19) 1.1140(11) 0.3407(12) 0.042(6) Uani 1 1 d . . . . .
H40A H 0.467996 1.162366 0.335631 0.051 Uiso 1 1 calc R . . . .
H40B H 0.612567 1.124941 0.295758 0.051 Uiso 1 1 calc R . . . .
C41 C 0.367(2) 1.0559(11) 0.2861(11) 0.036(5) Uani 1 1 d . . . . .
H41A H 0.403893 1.094360 0.237266 0.043 Uiso 1 1 calc R . . . .
H41B H 0.275018 1.080784 0.305767 0.043 Uiso 1 1 calc R . . . .
C42 C 0.3447(18) 0.9751(12) 0.2711(11) 0.037(5) Uani 1 1 d . . . . .
H42A H 0.347432 0.931076 0.319957 0.045 Uiso 1 1 calc R . . . .
H42B H 0.249441 0.977390 0.251783 0.045 Uiso 1 1 calc R . . . .
C43 C 0.4431(19) 0.8788(11) 0.1993(12) 0.044(6) Uani 1 1 d . . . . .
H43A H 0.346575 0.876220 0.183374 0.053 Uiso 1 1 calc R . . . .
H43B H 0.457063 0.834041 0.246681 0.053 Uiso 1 1 calc R . . . .
C44 C 0.557(2) 0.8690(12) 0.1351(11) 0.039(5) Uani 1 1 d . . . . .
H44A H 0.531982 0.906285 0.085067 0.047 Uiso 1 1 calc R . . . .
H44B H 0.650899 0.882799 0.146335 0.047 Uiso 1 1 calc R . . . .
C45 C 0.654(2) 0.7688(12) 0.0671(13) 0.051(6) Uani 1 1 d . . . . .
H45A H 0.636086 0.814602 0.021000 0.061 Uiso 1 1 calc R . . . .
H45B H 0.627545 0.717435 0.056223 0.061 Uiso 1 1 calc R . . . .
C46 C 0.813(2) 0.7603(13) 0.0771(13) 0.052(6) Uani 1 1 d . . . . .
H46A H 0.869474 0.760424 0.026681 0.063 Uiso 1 1 calc R . . . .
H46B H 0.839070 0.807493 0.095255 0.063 Uiso 1 1 calc R . . . .
C47 C 0.990(2) 0.6496(15) 0.1297(13) 0.069(4) Uani 1 1 d . U . . .
H47A H 0.989314 0.590521 0.157783 0.082 Uiso 1 1 calc R . . . .
H47B H 1.026077 0.652184 0.074866 0.082 Uiso 1 1 calc R . . . .
C48 C 1.085(2) 0.6865(14) 0.1616(12) 0.063(4) Uani 1 1 d . U . . .
H48A H 1.081180 0.746334 0.136129 0.075 Uiso 1 1 calc R . . . .
H48B H 1.183694 0.663173 0.150041 0.075 Uiso 1 1 calc R . . . .
C49 C 1.134(2) 0.7313(14) 0.2668(14) 0.066(7) Uani 1 1 d . . . . .
H49A H 1.110276 0.788521 0.236917 0.079 Uiso 1 1 calc R . . . .
H49B H 1.238193 0.718249 0.257325 0.079 Uiso 1 1 calc R . . . .
C50 C 1.093(2) 0.7240(14) 0.3516(13) 0.053(6) Uani 1 1 d . . . . .
H50A H 0.988660 0.718784 0.364576 0.064 Uiso 1 1 calc R . . . .
H50B H 1.145200 0.675114 0.383236 0.064 Uiso 1 1 calc R . . . .
C51 C 1.128(2) 0.7989(14) 0.4415(18) 0.075(8) Uani 1 1 d . . . . .
H51A H 1.189117 0.842351 0.444907 0.090 Uiso 1 1 calc R . . . .
H51B H 1.171036 0.745377 0.470528 0.090 Uiso 1 1 calc R . . . .
C52 C 0.984(2) 0.8139(13) 0.4818(12) 0.050(6) Uani 1 1 d . . . . .
H52A H 0.914113 0.781223 0.467499 0.060 Uiso 1 1 calc R . . . .
H52B H 0.988725 0.795270 0.538794 0.060 Uiso 1 1 calc R . . . .
C53 C 0.8210(19) 0.9196(14) 0.5147(10) 0.041(6) Uani 1 1 d . . . . .
H53A H 0.852759 0.905458 0.567697 0.049 Uiso 1 1 calc R . . . .
H53B H 0.739217 0.886229 0.515470 0.049 Uiso 1 1 calc R . . . .
C54 C 0.774(2) 1.0087(12) 0.4922(11) 0.035(5) Uani 1 1 d . . . . .
H54A H 0.706581 1.023201 0.534563 0.042 Uiso 1 1 calc R . . . .
H54B H 0.857870 1.042146 0.484230 0.042 Uiso 1 1 calc R . . . .
O13 O 0.4763(16) 0.6270(8) 0.2311(9) 0.068(4) Uani 1 1 d . U . . .
H13A H 0.490265 0.675320 0.204943 0.102 Uiso 1 1 calc GR . . . .
C55 C 0.559(2) 0.5710(12) 0.1961(14) 0.072(5) Uani 1 1 d . U . . .
H55A H 0.522371 0.572269 0.146656 0.107 Uiso 1 1 calc GR . . . .
H55B H 0.553842 0.515314 0.230482 0.107 Uiso 1 1 calc GR . . . .
H55C H 0.659001 0.585803 0.186532 0.107 Uiso 1 1 calc GR . . . .


_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
Br1 C6 1.894(17) . ?
Br2 C3 1.895(17) . ?
O1 C27 1.20(2) . ?
O2 C27 1.35(2) . ?
O2 C28 1.47(2) . ?
O3 C36 1.23(2) . ?
O4 C36 1.32(2) . ?
O4 C37 1.44(2) . ?
N1 C1 1.36(2) . ?
N1 C2 1.39(2) . ?
N2 C1 1.330(19) . ?
N2 C7 1.37(2) . ?
N3 C14 1.37(2) . ?
N3 C20 1.393(19) . ?
N4 C14 1.33(2) . ?
N4 C15 1.40(2) . ?
C1 C8 1.45(2) . ?
C2 C3 1.38(2) . ?
C2 C7 1.42(2) . ?
C3 C4 1.38(2) . ?
C4 C5 1.40(2) . ?
C5 C6 1.37(2) . ?
C6 C7 1.40(2) . ?
C8 C9 1.43(2) . ?
C8 C13 1.38(2) . ?
C9 C10 1.37(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.39(2) . ?
C11 C14 1.45(2) . ?
C12 C13 1.38(2) . ?
C15 C16 1.41(2) . ?
C15 C20 1.41(2) . ?
C16 C17 1.42(2) . ?
C16 C21 1.49(2) . ?
C17 C18 1.37(2) . ?
C18 C19 1.40(2) . ?
C19 C20 1.42(2) . ?
C19 C30 1.45(2) . ?
C21 C22 1.43(2) . ?
C21 C26 1.38(2) . ?
C22 C23 1.37(2) . ?
C23 C24 1.38(2) . ?
C24 C25 1.40(2) . ?
C24 C27 1.49(3) . ?
C25 C26 1.37(2) . ?
C28 C29 1.48(3) . ?
C30 C31 1.37(2) . ?
C30 C35 1.40(2) . ?
C31 C32 1.37(2) . ?
C32 C33 1.39(2) . ?
C33 C34 1.35(2) . ?
C33 C36 1.48(3) . ?
C34 C35 1.38(2) . ?
C37 C38 1.47(3) . ?
O5 C39 1.42(2) . ?
O5 C54 1.42(2) . ?
O6 C40 1.41(2) . ?
O6 C41 1.44(2) . ?
O7 C42 1.429(19) . ?
O7 C43 1.43(2) . ?
O8 C44 1.45(2) . ?
O8 C45 1.40(2) . ?
O9 C46 1.41(2) . ?
O9 C47 1.45(2) . ?
O10 C48 1.41(2) . ?
O10 C49 1.40(2) . ?
O11 C50 1.41(2) . ?
O11 C51 1.36(3) . ?
O12 C52 1.44(2) . ?
O12 C53 1.422(19) . ?
C39 C40 1.51(2) . ?
C41 C42 1.49(2) . ?
C43 C44 1.50(2) . ?
C45 C46 1.51(3) . ?
C47 C48 1.38(3) . ?
C49 C50 1.49(3) . ?
C51 C52 1.48(3) . ?
C53 C54 1.48(2) . ?
O13 C55 1.39(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
C27 O2 C28 116.1(16) . . ?
C36 O4 C37 117.4(16) . . ?
C1 N1 C2 106.1(14) . . ?
C1 N2 C7 104.7(14) . . ?
C14 N3 C20 106.2(13) . . ?
C14 N4 C15 104.0(13) . . ?
N1 C1 C8 123.2(15) . . ?
N2 C1 N1 113.9(15) . . ?
N2 C1 C8 122.9(15) . . ?
N1 C2 C7 105.3(15) . . ?
C3 C2 N1 132.3(16) . . ?
C3 C2 C7 122.4(16) . . ?
C2 C3 Br2 121.6(13) . . ?
C2 C3 C4 118.3(16) . . ?
C4 C3 Br2 120.0(14) . . ?
C3 C4 C5 120.6(17) . . ?
C6 C5 C4 120.8(17) . . ?
C5 C6 Br1 120.8(14) . . ?
C5 C6 C7 120.2(17) . . ?
C7 C6 Br1 118.9(13) . . ?
N2 C7 C2 109.9(15) . . ?
N2 C7 C6 132.4(16) . . ?
C6 C7 C2 117.6(16) . . ?
C9 C8 C1 119.6(15) . . ?
C13 C8 C1 124.1(15) . . ?
C13 C8 C9 116.3(15) . . ?
C10 C9 C8 120.9(16) . . ?
C9 C10 C11 121.8(16) . . ?
C10 C11 C12 117.8(16) . . ?
C10 C11 C14 122.6(15) . . ?
C12 C11 C14 119.6(15) . . ?
C13 C12 C11 120.6(16) . . ?
C8 C13 C12 122.6(16) . . ?
N3 C14 C11 123.4(15) . . ?
N4 C14 N3 114.1(15) . . ?
N4 C14 C11 122.5(15) . . ?
N4 C15 C16 129.4(15) . . ?
N4 C15 C20 110.4(14) . . ?
C20 C15 C16 120.2(16) . . ?
C15 C16 C17 114.7(16) . . ?
C15 C16 C21 123.7(16) . . ?
C17 C16 C21 121.6(16) . . ?
C18 C17 C16 123.1(16) . . ?
C17 C18 C19 124.8(17) . . ?
C18 C19 C20 111.9(15) . . ?
C18 C19 C30 123.6(16) . . ?
C20 C19 C30 124.4(15) . . ?
N3 C20 C15 105.2(14) . . ?
N3 C20 C19 129.5(15) . . ?
C15 C20 C19 125.2(15) . . ?
C22 C21 C16 120.9(15) . . ?
C26 C21 C16 121.1(17) . . ?
C26 C21 C22 118.0(16) . . ?
C23 C22 C21 120.2(16) . . ?
C22 C23 C24 121.2(18) . . ?
C23 C24 C25 118.5(17) . . ?
C23 C24 C27 122.8(19) . . ?
C25 C24 C27 118.6(17) . . ?
C26 C25 C24 121.3(17) . . ?
C25 C26 C21 120.8(18) . . ?
O1 C27 O2 122.6(19) . . ?
O1 C27 C24 126(2) . . ?
O2 C27 C24 111.6(17) . . ?
O2 C28 C29 105.6(18) . . ?
C31 C30 C19 122.5(16) . . ?
C31 C30 C35 117.5(17) . . ?
C35 C30 C19 120.1(16) . . ?
C30 C31 C32 121.7(17) . . ?
C31 C32 C33 121.1(18) . . ?
C32 C33 C36 119.9(19) . . ?
C34 C33 C32 117.2(18) . . ?
C34 C33 C36 122.9(19) . . ?
C33 C34 C35 123.0(19) . . ?
C34 C35 C30 119.5(18) . . ?
O3 C36 O4 123.0(18) . . ?
O3 C36 C33 123(2) . . ?
O4 C36 C33 114.1(18) . . ?
O4 C37 C38 107.2(18) . . ?
C54 O5 C39 112.0(13) . . ?
C40 O6 C41 113.1(14) . . ?
C43 O7 C42 112.0(13) . . ?
C45 O8 C44 112.8(15) . . ?
C46 O9 C47 118.0(17) . . ?
C49 O10 C48 110.0(18) . . ?
C51 O11 C50 115.8(19) . . ?
C53 O12 C52 112.1(15) . . ?
O5 C39 C40 108.7(14) . . ?
O6 C40 C39 107.5(16) . . ?
O6 C41 C42 108.4(14) . . ?
O7 C42 C41 109.0(14) . . ?
O7 C43 C44 107.6(15) . . ?
O8 C44 C43 107.3(15) . . ?
O8 C45 C46 115.1(17) . . ?
O9 C46 C45 108.8(16) . . ?
C48 C47 O9 115.2(18) . . ?
C47 C48 O10 114(2) . . ?
O10 C49 C50 109.0(19) . . ?
O11 C50 C49 105.3(19) . . ?
O11 C51 C52 117(2) . . ?
O12 C52 C51 111.4(17) . . ?
O12 C53 C54 110.8(16) . . ?
O5 C54 C53 110.2(14) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
####################################################################### 
# 
# 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_uwdm_11_ligand
_database_code_depnum_ccdc_archive 'CCDC 2049900'
loop_
_audit_author_name
_audit_author_address
'Wilson B.H.'
;University of Windsor
Canada
;
_audit_update_record             
;
2020-12-12 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_cu_uwdm_11_ligand   
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE:  All crystals trialed exhibited low crystallinity resulting in low qualitiy data 
which contributes to a high Rint value
;
_vrf_THETM01_cu_uwdm_11_ligand   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All crystals trialed exhibited weak diffraction and therefore only 
low resolution data could be obtained
;
_vrf_PLAT020_cu_uwdm_11_ligand   
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.462 Report
RESPONSE: All crystals trialed exhibited low crystallinity resulting in low qualitiy data 
which contributes to a high Rint value.
;
_vrf_PLAT084_cu_uwdm_11_ligand   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.54 Report
RESPONSE: All crystals trialed exhibited low crystallinity resulting in low qualitiy data 
which contributes to a high wR2 value.
;
_vrf_PLAT082_cu_uwdm_11_ligand   
;
PROBLEM: High R1 Value ..................................       0.20 Report
RESPONSE: All crystals trialed exhibited low crystallinity resulting in low qualitiy data 
which contributes to a high R1 value.
;
_vrf_PLAT241_cu_uwdm_11_ligand   
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         N5 Check 
RESPONSE: The poor quality and low resolution data resulted in large thermal elipsoids for an number of atoms.
;
_vrf_PLAT242_cu_uwdm_11_ligand   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C47 Check 
RESPONSE: The poor quality and low resolution data resulted in large thermal elipsoids for an number of atoms.
;
_vrf_PLAT341_cu_uwdm_11_ligand   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02572 Ang.  
RESPONSE: The poor quality and low resolution data resulted in a low C-C bond precision.
;
_vrf_PLAT410_cu_uwdm_11_ligand   
;
PROBLEM: Short Intra H...H Contact  H17      ..H26      .       1.83 Ang.  
RESPONSE: This is a consequence of the packing of adjacent rotaxane axles.
;
_vrf_PLAT420_cu_uwdm_11_ligand   
;
PROBLEM: D-H Without Acceptor       O2       --H2       .     Please Check 
RESPONSE: The solvent mask function of Olex2 was applied as after modeling the 
two crystallograohically unique rotaxanes molecules there remianed diffuse
electron density attributed disordered solvent molecules which was unable
to be modeled due to the poor quality data. One of these solvent molecules 
most likely acted as the hydrogen bond acceptor.
;
# end Validation Reply Form
_audit_creation_date             2020-08-24
_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         'C34 H20 Br2 N4 O4, C16 H32 O8'
_chemical_formula_sum            'C50 H52 Br2 N4 O12'
_chemical_formula_weight         1060.77
_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'
Br Br -0.6763 1.2805 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   19.889(5)
_cell_length_b                   18.209(4)
_cell_length_c                   33.691(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.93(2)
_cell_angle_gamma                90
_cell_volume                     11733(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3221
_cell_measurement_temperature    170
_cell_measurement_theta_max      39.5090
_cell_measurement_theta_min      2.3380
_shelx_estimated_absorpt_T_max   0.809
_shelx_estimated_absorpt_T_min   0.666
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51304
_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    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_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  0.4617
_diffrn_reflns_av_unetI/netI     0.1686
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            111138
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        50.429
_diffrn_reflns_theta_max         50.429
_diffrn_reflns_theta_min         2.338
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.93  97.53   1.80   10.00    --   20.69  59.25 159.92   52
  2  φ   -349.73   8.47   1.80   40.00 -80.41 -89.16 -31.50    --   199
  3  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  10.05   56
  4  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74-149.95   56
  5  ω      3.93  97.53   1.80   10.00    --   20.69  59.25-110.08   52
  6  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74 130.05   56
  7  ω    -26.23  70.97   1.80   15.00    --   50.69 -83.74  29.95   54
  8  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74 -29.95   56
  9  ω    192.04 285.64   1.80   40.00    --  -89.16 -59.25 -99.92   52
 10  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  90.05   56
 11  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74-109.95   56
 12  ω    192.04 285.64   1.80   40.00    --  -89.16 -59.25 140.08   52
 13  ω    192.04 285.64   1.80   40.00    --  -89.16 -59.25-139.92   52
 14  ω   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  50.05   56
;
_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      -0.0167089000
_diffrn_orient_matrix_UB_12      0.0505910000
_diffrn_orient_matrix_UB_13      0.0330198000
_diffrn_orient_matrix_UB_21      -0.0708046000
_diffrn_orient_matrix_UB_22      -0.0379840000
_diffrn_orient_matrix_UB_23      -0.0062480000
_diffrn_orient_matrix_UB_31      0.0345058000
_diffrn_orient_matrix_UB_32      -0.0563311000
_diffrn_orient_matrix_UB_33      0.0336486000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'I\mS Microfocus Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5158
_reflns_number_total             12204
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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         0.750
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         12204
_refine_ls_number_restraints     1052
_refine_ls_R_factor_all          0.2789
_refine_ls_R_factor_gt           0.2005
_refine_ls_restrained_S_all      1.306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4848
_refine_ls_wR_factor_ref         0.5352
_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. The poor quality and low resolution
data was sufficient to obtain the connectivity of the structure. The low resolution data
required a number of C-C anbd C-O bonds to be restrained to chemically sensible values
using the DFIX restraint. The FLAT restraints were required to model the carboxylate moities
while the RIGU restraint was applied inorder for the thermal parameters to be modeled 
in a chemically sensible manner. the AFIX restraint was required to modeled the 6-membered
aromatic rings in a chemically sensible manner. 
The solvent mask function of Olex2 was applied as after modeling the 
two crystallograohically unique rotaxanes molecules there remianed diffuse
electron density attributed disordered solvent molecules which was unable
to be modeled due to the poor quality data.This gave a solvent accessible
void of 3426.8 cubic angestroms, caqlculated to contain 782 electrons.

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C49B-C50B
 1.3 with sigma of 0.02
 C49A-C50A
 1.3 with sigma of 0.02
 O12-C49A
 1.5 with sigma of 0.02
 C6-C7
 1.4 with sigma of 0.002
 C28-C19
 1.4 with sigma of 0.002
 C16-C21
 1.4 with sigma of 0.002
 C1-C8
 1.4 with sigma of 0.002
 C89-C90
 1.4 with sigma of 0.002
 C95-C96
 1.4 with sigma of 0.002
 C99-C100
 1.4 with sigma of 0.002
 C81-C84
 1.4 with sigma of 0.002
 C24-C27
 1.4 with sigma of 0.002
 C31-C34
 1.4 with sigma of 0.002
 C51-C58
 1.4 with sigma of 0.002
 C62-C63
 1.4 with sigma of 0.002
 C66-C71
 1.4 with sigma of 0.002
 C69-C78
 1.4 with sigma of 0.002
 C74-C77
 1.4 with sigma of 0.002
 O12-C49B
 1.5 with sigma of 0.002
 C37-C38
 1.45 with sigma of 0.0002
3. Restrained planarity
 C34, H4, O4, O3, C31
 with sigma of 0.01
 H14, O14, C77, O13, C74
 with sigma of 0.01
 H16, O16, C84, O15, C81
 with sigma of 0.01
4. Rigid body (RIGU) restrains
 C55, Br3B, C53, C54, C52, C57, N5, C56, N6, C51, Br4B, C58, C59, C63, C60,
 C62, C61, C64, N8, N7, C70, C65, C69, C66, C78, C68, C71, C67, C79, C83, C72,
 C76, C80, C82, C73, C75, C81, C74, C84, C77, O16, O15, O14, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, Br2, C6, C7, C5, N1, C2, C1, C4, N2, C3, C8, Br1, C9, C13, C10, C12, C11,
  C14, N3, N4, C20, C15, C19, C16, C28, C18, C21, C17, C33, C29, C26, C22, C32,
 C30, C25, C23, C24, C34, C27, O3, O4, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C89, O17, C100, C85, C99, C86, O24, O18, C97, C87, O23, C88, C96, O19, C95,
 O22, C90, C94, O20, C93, C91, O21, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, O6, C36, C37, C35, C38, O5, O7, C50A, C50B, C39, C49A, C49B, C40, O12,
 O8, C48, C41, C47, C42, O11, O9, C46, C43, C44, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Br3B(0.5) Br4B(0.5) C50A(0.5) H50A(0.5) H50B(0.5) C49A(0.5)
 H49A(0.5) H49B(0.5) C49B(0.5) H49C(0.5) H49D(0.5) C50B(0.5) H50C(0.5)
 H50D(0.5) Br3A(0.5) Br4A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C92(H92A,H92B), C87(H87A,H87B), C38(H38A,
 H38B), C91(H91A,H91B), C93(H93A,H93B), C100(H10A,H10B), C41(H41A,H41B),
 C42(H42A,H42B), C88(H88A,H88B), C44(H44A,H44B), C47(H47A,H47B), C45(H45A,H45B),
  C85(H85A,H85B), C99(H99A,H99B), C35(H35A,H35B), C39(H39A,H39B), C43(H43A,
 H43B), C90(H90A,H90B), C94(H94A,H94B), C97(H97A,H97B), C46(H46A,H46B),
 C48(H48A,H48B), C50A(H50A,H50B), C96(H96A,H96B), C95(H95A,H95B), C89(H89A,
 H89B), C49A(H49A,H49B), C40(H40A,H40B), C86(H86A,H86B), C49B(H49C,H49D),
 C50B(H50C,H50D), C98(H98A,H98B)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), N7(H7), C75(H75), C76(H76), C72(H72), C73(H73), C83(H83),
 C79(H79), C80(H80), C82(H82), C62(H62), C9(H9), C55(H55), C54(H54), C18(H18),
 C17(H17), C29(H29), C30(H30), C32(H32), C33(H33), C23(H23), C22(H22), C26(H26),
  C25(H25), N5(H5), C68(H68), C67(H67), C13(H13), C12(H12), C59(H59), C10(H10),
 C60(H60), C63(H63), C4(H4A), C5(H5A)
6.c Fitted hexagon refined as free rotating group:
 C74(C75,C76,C71,C72,C73), C83(C78,C79,C80,C81,C82), C57(C56,C55,C54,C53,C52),
 C16(C15,C20,C19,C18,C17), C28(C29,C30,C31,C32,C33), C24(C23,C22,C21,C26,C25),
 C66(C65,C70,C69,C68,C67)
6.d Tetrahedral OH refined with riding coordinates:
 O4(H4)
6.e Idealised tetrahedral OH refined as rotating group:
 O14(H14), O16(H16), O2(H2)
;
_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
Br2 Br 0.21674(17) 0.32399(19) 0.11194(8) 0.1206(12) Uani 1 1 d . U . . .
Br3B Br 0.7419(4) 0.8991(4) 0.7549(2) 0.134(2) Uani 0.5 1 d . U P A 2
Br4B Br 0.8100(4) 1.2346(4) 0.7378(3) 0.129(2) Uani 0.5 1 d . U P B 2
O1 O -0.0126(7) -0.2632(9) 0.4518(4) 0.095(4) Uani 1 1 d . U . . .
O14 O 0.1423(8) 0.7047(9) 0.4547(5) 0.100(4) Uani 1 1 d . U . . .
H14 H 0.139404 0.659586 0.459181 0.150 Uiso 1 1 calc GR . . . .
O13 O 0.1741(8) 0.6920(8) 0.5223(5) 0.099(4) Uani 1 1 d . U . . .
O16 O 0.1724(8) 1.5504(8) 0.5264(4) 0.094(4) Uani 1 1 d . U . . .
H16 H 0.186268 1.594196 0.527971 0.142 Uiso 1 1 calc GR . . . .
N3 N 0.0240(8) 0.2220(9) 0.3485(4) 0.078(4) Uani 1 1 d . U . . .
H3 H 0.035177 0.266528 0.342359 0.093 Uiso 1 1 calc R . . . .
N1 N 0.1370(8) 0.2103(11) 0.1633(4) 0.085(4) Uani 1 1 d . U . . .
H1 H 0.145402 0.253792 0.175006 0.102 Uiso 1 1 calc R . . . .
O3 O 0.1018(8) 0.5714(8) 0.4349(3) 0.099(4) Uani 1 1 d . U . . .
O2 O -0.0337(11) -0.2719(9) 0.3824(5) 0.118(5) Uani 1 1 d . U . . .
H2 H -0.013811 -0.311172 0.392118 0.176 Uiso 1 1 calc GR . . . .
O4 O 0.0006(8) 0.5912(8) 0.4519(3) 0.090(4) Uani 1 1 d . U . . .
H4 H 0.019470 0.632517 0.452142 0.135 Uiso 1 1 calc R . . . .
N8 N 0.3224(9) 1.1730(10) 0.5572(5) 0.080(4) Uani 1 1 d . U . . .
N7 N 0.3189(9) 1.0560(10) 0.5522(5) 0.080(4) Uani 1 1 d . U . . .
H7 H 0.332253 1.009889 0.556048 0.096 Uiso 1 1 calc R . . . .
O6 O 0.1631(10) 0.3272(10) 0.3464(5) 0.123(5) Uani 1 1 d . U . . .
O15 O 0.2753(9) 1.5523(9) 0.5158(4) 0.108(5) Uani 1 1 d . U . . .
O7 O 0.2275(9) 0.1798(10) 0.3680(5) 0.120(5) Uani 1 1 d . U . . .
N4 N 0.0075(10) 0.1023(10) 0.3434(5) 0.095(5) Uani 1 1 d . U . . .
N2 N 0.0995(9) 0.0982(12) 0.1507(5) 0.094(5) Uani 1 1 d . U . . .
O17 O 0.3892(10) 0.9188(11) 0.5375(5) 0.124(6) Uani 1 1 d . U . . .
N6 N 0.6617(10) 1.1443(14) 0.7006(5) 0.111(6) Uani 1 1 d . U . . .
C74 C 0.1753(8) 0.8182(4) 0.4955(4) 0.091(5) Uani 1 1 d D U . . .
C75 C 0.1548(7) 0.8604(6) 0.4599(3) 0.080(5) Uani 1 1 d G U . . .
H75 H 0.135615 0.837379 0.433921 0.096 Uiso 1 1 calc R . . . .
C76 C 0.1626(7) 0.9363(5) 0.4621(3) 0.095(6) Uani 1 1 d G U . . .
H76 H 0.148591 0.965119 0.437754 0.115 Uiso 1 1 calc R . . . .
C71 C 0.1907(8) 0.9700(4) 0.5001(4) 0.078(5) Uani 1 1 d DG U . . .
C72 C 0.2111(7) 0.9278(6) 0.5358(3) 0.099(6) Uani 1 1 d G U . . .
H72 H 0.230341 0.950829 0.561720 0.119 Uiso 1 1 calc R . . . .
C73 C 0.2034(8) 0.8519(6) 0.5335(3) 0.096(6) Uani 1 1 d G U . . .
H73 H 0.217364 0.823088 0.557889 0.115 Uiso 1 1 calc R . . . .
O19 O 0.2969(14) 1.0480(13) 0.6424(6) 0.153(7) Uani 1 1 d . U . . .
O21 O 0.3500(11) 1.3111(13) 0.6078(6) 0.138(7) Uani 1 1 d . U . . .
C14 C 0.0233(11) 0.1565(13) 0.3257(6) 0.079(5) Uani 1 1 d . U . . .
O9 O 0.0449(14) -0.0911(14) 0.2962(7) 0.171(9) Uani 1 1 d . U . . .
C83 C 0.1546(5) 1.3162(6) 0.5176(4) 0.079(5) Uani 1 1 d . U . . .
H83 H 0.115032 1.291691 0.521891 0.094 Uiso 1 1 calc R . . . .
C78 C 0.2084(7) 1.2759(3) 0.5091(4) 0.079(4) Uani 1 1 d DG U . . .
C79 C 0.2663(6) 1.3118(6) 0.5028(3) 0.080(5) Uani 1 1 d G U . . .
H79 H 0.303070 1.284237 0.497033 0.096 Uiso 1 1 calc R . . . .
C80 C 0.2704(5) 1.3879(6) 0.5050(3) 0.070(4) Uani 1 1 d G U . . .
H80 H 0.310027 1.412446 0.500732 0.084 Uiso 1 1 calc R . . . .
C81 C 0.2167(7) 1.4282(3) 0.5135(4) 0.088(5) Uani 1 1 d DG U . . .
C82 C 0.1587(6) 1.3924(6) 0.5198(4) 0.095(6) Uani 1 1 d G U . . .
H82 H 0.121989 1.419902 0.525590 0.114 Uiso 1 1 calc R . . . .
C2 C 0.1352(11) 0.1191(14) 0.1242(6) 0.083(5) Uani 1 1 d . U . . .
C62 C 0.4756(9) 1.0559(11) 0.5957(5) 0.074(5) Uani 1 1 d D U . . .
H62 H 0.466045 1.023376 0.572777 0.089 Uiso 1 1 calc R . . . .
C27 C -0.0271(12) -0.2187(4) 0.4156(6) 0.098(6) Uani 1 1 d D U . . .
O18 O 0.3606(12) 0.9224(11) 0.6135(7) 0.154(7) Uani 1 1 d . U . . .
C9 C 0.1046(13) 0.2117(16) 0.2445(6) 0.106(7) Uani 1 1 d . U . . .
H9 H 0.133838 0.249834 0.239563 0.127 Uiso 1 1 calc R . . . .
C57 C 0.7224(6) 1.1186(8) 0.7312(3) 0.076(5) Uani 1 1 d . U . . .
C56 C 0.7819(7) 1.1496(7) 0.7576(4) 0.097(6) Uani 1 1 d G U . . .
C55 C 0.8272(5) 1.1064(8) 0.7872(3) 0.080(5) Uani 1 1 d G U . . .
H55 H 0.867811 1.127602 0.805263 0.096 Uiso 1 1 calc R . . . .
C54 C 0.8129(7) 1.0323(8) 0.7904(4) 0.092(6) Uani 1 1 d G U . . .
H54 H 0.843880 1.002761 0.810694 0.110 Uiso 1 1 calc R . . . .
C53 C 0.7535(8) 1.0013(7) 0.7640(5) 0.112(7) Uani 1 1 d G U . . .
C52 C 0.7082(6) 1.0444(9) 0.7344(4) 0.088(5) Uani 1 1 d G U . . .
O20 O 0.2749(12) 1.1996(12) 0.6430(5) 0.137(7) Uani 1 1 d . U . . .
C16 C -0.0311(7) 0.0874(4) 0.4092(4) 0.079(5) Uani 1 1 d D U . . .
C15 C -0.0062(7) 0.1242(5) 0.3800(3) 0.074(5) Uani 1 1 d G U . . .
C20 C 0.0030(7) 0.1999(5) 0.3826(3) 0.073(5) Uani 1 1 d G U . . .
C19 C -0.0125(8) 0.2388(4) 0.4144(4) 0.089(5) Uani 1 1 d DG U . . .
C18 C -0.0373(8) 0.2019(6) 0.4437(3) 0.097(6) Uani 1 1 d G U . . .
H18 H -0.047910 0.228509 0.465499 0.116 Uiso 1 1 calc R . . . .
C17 C -0.0466(7) 0.1263(6) 0.4411(3) 0.087(5) Uani 1 1 d G U . . .
H17 H -0.063556 0.101107 0.461092 0.104 Uiso 1 1 calc R . . . .
C84 C 0.2234(13) 1.5046(4) 0.5180(3) 0.094(5) Uani 1 1 d D U . . .
C7 C 0.1555(12) 0.1900(13) 0.1268(6) 0.098(6) Uani 1 1 d D U . . .
C28 C 0.0016(7) 0.3142(4) 0.4200(4) 0.072(4) Uani 1 1 d D U . . .
C29 C 0.0592(6) 0.3459(6) 0.4109(4) 0.121(9) Uani 1 1 d G U . . .
H29 H 0.088667 0.316917 0.399242 0.145 Uiso 1 1 calc R . . . .
C30 C 0.0738(6) 0.4199(7) 0.4189(4) 0.091(5) Uani 1 1 d G U . . .
H30 H 0.113188 0.441578 0.412730 0.109 Uiso 1 1 calc R . . . .
C31 C 0.0307(8) 0.4623(4) 0.4360(3) 0.105(6) Uani 1 1 d DG U . . .
C32 C -0.0269(6) 0.4307(6) 0.4451(3) 0.085(5) Uani 1 1 d G U . . .
H32 H -0.056323 0.459671 0.456790 0.102 Uiso 1 1 calc R . . . .
C33 C -0.0415(5) 0.3566(6) 0.4371(4) 0.083(5) Uani 1 1 d G U . . .
H33 H -0.080845 0.335010 0.443301 0.099 Uiso 1 1 calc R . . . .
C24 C -0.0331(8) -0.1421(4) 0.4128(5) 0.089(5) Uani 1 1 d D U . . .
C23 C -0.0282(8) -0.1064(6) 0.3772(4) 0.110(7) Uani 1 1 d G U . . .
H23 H -0.023847 -0.134135 0.354174 0.132 Uiso 1 1 calc R . . . .
C22 C -0.0296(8) -0.0301(6) 0.3754(3) 0.106(7) Uani 1 1 d G U . . .
H22 H -0.026257 -0.005751 0.351096 0.128 Uiso 1 1 calc R . . . .
C21 C -0.0360(8) 0.0104(4) 0.4091(4) 0.085(5) Uani 1 1 d DG U . . .
C26 C -0.0409(8) -0.0253(6) 0.4447(3) 0.089(5) Uani 1 1 d G U . . .
H26 H -0.045207 0.002440 0.467758 0.107 Uiso 1 1 calc R . . . .
C25 C -0.0394(8) -0.1015(6) 0.4465(4) 0.109(7) Uani 1 1 d G U . . .
H25 H -0.042796 -0.125944 0.470837 0.131 Uiso 1 1 calc R . . . .
C61 C 0.4256(11) 1.1042(11) 0.5987(6) 0.076(5) Uani 1 1 d . U . . .
C34 C 0.0418(12) 0.5382(4) 0.4411(3) 0.105(6) Uani 1 1 d D U . . .
C64 C 0.3558(11) 1.1112(12) 0.5688(5) 0.070(4) Uani 1 1 d . U . . .
O22 O 0.4353(13) 1.2901(15) 0.5607(6) 0.156(8) Uani 1 1 d . U . . .
C51 C 0.6252(10) 1.0897(18) 0.6865(5) 0.099(6) Uani 1 1 d D U . . .
N5 N 0.6522(13) 1.0312(16) 0.7043(8) 0.156(10) Uani 1 1 d . U . . .
H5 H 0.635303 0.986959 0.697280 0.187 Uiso 1 1 calc R . . . .
O5 O 0.0362(14) 0.3790(15) 0.3060(7) 0.172(9) Uani 1 1 d . U . . .
C1 C 0.1064(11) 0.1574(16) 0.1773(5) 0.098(6) Uani 1 1 d D U . . .
C6 C 0.1917(12) 0.2283(13) 0.1030(6) 0.105(6) Uani 1 1 d D U . . .
C66 C 0.1972(7) 1.0468(3) 0.5016(4) 0.094(6) Uani 1 1 d D U . . .
C65 C 0.2561(6) 1.0789(5) 0.5279(4) 0.068(4) Uani 1 1 d G U . . .
C70 C 0.2611(6) 1.1549(6) 0.5314(3) 0.067(4) Uani 1 1 d G U . . .
C69 C 0.2071(7) 1.1988(3) 0.5085(4) 0.092(5) Uani 1 1 d DG U . . .
C68 C 0.1481(6) 1.1667(6) 0.4822(3) 0.077(5) Uani 1 1 d G U . . .
H68 H 0.111221 1.196663 0.466509 0.092 Uiso 1 1 calc R . . . .
C67 C 0.1432(6) 1.0907(6) 0.4787(4) 0.105(6) Uani 1 1 d G U . . .
H67 H 0.102921 1.068717 0.460726 0.126 Uiso 1 1 calc R . . . .
C13 C 0.0434(13) 0.1022(15) 0.2216(6) 0.101(7) Uani 1 1 d . U . . .
H13 H 0.030517 0.061872 0.203169 0.121 Uiso 1 1 calc R . . . .
O12 O -0.0927(15) 0.2891(16) 0.2729(9) 0.196(9) Uani 1 1 d D U . . .
C12 C 0.0228(13) 0.1034(14) 0.2592(6) 0.100(7) Uani 1 1 d . U . . .
H12 H -0.007362 0.066287 0.264389 0.121 Uiso 1 1 calc R . . . .
C59 C 0.5109(12) 1.1468(15) 0.6608(6) 0.095(6) Uani 1 1 d . U . . .
H59 H 0.523748 1.183328 0.681635 0.114 Uiso 1 1 calc R . . . .
C77 C 0.1651(6) 0.7421(4) 0.4925(8) 0.105(6) Uani 1 1 d D U . . .
C10 C 0.0895(13) 0.2131(13) 0.2800(6) 0.092(6) Uani 1 1 d . U . . .
H10 H 0.106932 0.250118 0.300072 0.110 Uiso 1 1 calc R . . . .
C11 C 0.0453(11) 0.1557(13) 0.2866(6) 0.082(5) Uani 1 1 d . U . . .
O23 O 0.425(2) 1.1671(19) 0.5044(10) 0.215(13) Uani 1 1 d . U . . .
C36 C 0.1604(15) 0.3939(15) 0.3296(6) 0.107(7) Uani 1 1 d . U . . .
H36A H 0.197346 0.397544 0.315135 0.128 Uiso 1 1 calc R . . . .
H36B H 0.170750 0.430880 0.352023 0.128 Uiso 1 1 calc R . . . .
C60 C 0.4430(12) 1.1510(13) 0.6345(6) 0.091(6) Uani 1 1 d . U . . .
H60 H 0.409510 1.183573 0.640170 0.109 Uiso 1 1 calc R . . . .
C8 C 0.0812(12) 0.1581(15) 0.2123(5) 0.097(6) Uani 1 1 d D U . . .
O10 O -0.0814(16) -0.0336(17) 0.2563(9) 0.188(10) Uani 1 1 d . U . . .
C37 C 0.2288(14) 0.3063(4) 0.3772(4) 0.141(10) Uani 1 1 d D U . . .
H37A H 0.266829 0.305706 0.363481 0.169 Uiso 1 1 calc R . . . .
H37B H 0.240260 0.344761 0.398819 0.169 Uiso 1 1 calc R . . . .
C92 C 0.2974(17) 1.3253(14) 0.6266(6) 0.114(7) Uani 1 1 d . U . . .
H92A H 0.271366 1.369290 0.613406 0.137 Uiso 1 1 calc R . . . .
H92B H 0.319547 1.337739 0.655904 0.137 Uiso 1 1 calc R . . . .
Br1 Br 0.1246(3) -0.0210(2) 0.08376(13) 0.1804(19) Uani 1 1 d . U . . .
C87 C 0.3809(18) 0.9496(16) 0.6503(9) 0.133(8) Uani 1 1 d . U . . .
H87A H 0.414505 0.990221 0.651472 0.160 Uiso 1 1 calc R . . . .
H87B H 0.403341 0.911546 0.670565 0.160 Uiso 1 1 calc R . . . .
C38 C 0.2279(12) 0.2359(4) 0.3972(4) 0.121(7) Uani 1 1 d D U . . .
H38A H 0.269643 0.230959 0.421075 0.145 Uiso 1 1 calc R . . . .
H38B H 0.185692 0.231932 0.407231 0.145 Uiso 1 1 calc R . . . .
O11 O -0.1544(14) 0.111(2) 0.2500(8) 0.192(9) Uani 1 1 d . U . . .
C91 C 0.246(2) 1.2644(19) 0.6252(10) 0.151(10) Uani 1 1 d . U . . .
H91A H 0.210859 1.281087 0.639455 0.182 Uiso 1 1 calc R . . . .
H91B H 0.220141 1.254702 0.596037 0.182 Uiso 1 1 calc R . . . .
C93 C 0.394(2) 1.354(2) 0.6078(10) 0.160(12) Uani 1 1 d . U . . .
H93A H 0.413046 1.371482 0.636640 0.191 Uiso 1 1 calc R . . . .
H93B H 0.370949 1.397247 0.591647 0.191 Uiso 1 1 calc R . . . .
C58 C 0.5581(10) 1.0983(18) 0.6597(6) 0.118(8) Uani 1 1 d D U . . .
C100 C 0.3703(15) 0.8988(13) 0.4955(7) 0.119(8) Uani 1 1 d D U . . .
H10A H 0.395787 0.854174 0.491239 0.142 Uiso 1 1 calc R . . . .
H10B H 0.319420 0.889215 0.485553 0.142 Uiso 1 1 calc R . . . .
C41 C 0.1410(16) -0.0374(16) 0.3449(7) 0.112(7) Uani 1 1 d . U . . .
H41A H 0.134730 -0.073392 0.365657 0.134 Uiso 1 1 calc R . . . .
H41B H 0.111376 0.005703 0.346319 0.134 Uiso 1 1 calc R . . . .
C63 C 0.5408(10) 1.0519(17) 0.6250(6) 0.120(9) Uani 1 1 d D U . . .
H63 H 0.574170 1.017014 0.621371 0.144 Uiso 1 1 calc R . . . .
C42 C 0.1176(17) -0.0679(16) 0.3072(8) 0.121(8) Uani 1 1 d . U . . .
H42A H 0.147102 -0.111012 0.305756 0.145 Uiso 1 1 calc R . . . .
H42B H 0.123629 -0.031899 0.286421 0.145 Uiso 1 1 calc R . . . .
C88 C 0.3128(18) 0.978(2) 0.6592(11) 0.152(9) Uani 1 1 d . U . . .
H88A H 0.273746 0.944451 0.646964 0.183 Uiso 1 1 calc R . . . .
H88B H 0.319211 0.980229 0.689332 0.183 Uiso 1 1 calc R . . . .
C3 C 0.1424(15) 0.0793(17) 0.0894(8) 0.121(8) Uani 1 1 d . U . . .
C44 C -0.066(2) -0.104(2) 0.2470(12) 0.168(10) Uani 1 1 d . U . . .
H44A H -0.088855 -0.115112 0.217732 0.201 Uiso 1 1 calc R . . . .
H44B H -0.081025 -0.139675 0.264701 0.201 Uiso 1 1 calc R . . . .
C47 C -0.1437(15) 0.184(2) 0.2668(8) 0.137(8) Uani 1 1 d . U . . .
H47A H -0.105907 0.181654 0.292950 0.165 Uiso 1 1 calc R . . . .
H47B H -0.186846 0.198580 0.274078 0.165 Uiso 1 1 calc R . . . .
C45 C -0.147(2) -0.020(3) 0.2528(14) 0.215(16) Uani 1 1 d . U . . .
H45A H -0.166454 -0.062632 0.264266 0.258 Uiso 1 1 calc R . . . .
H45B H -0.171693 -0.018122 0.222922 0.258 Uiso 1 1 calc R . . . .
C85 C 0.3871(15) 0.8545(17) 0.5616(9) 0.128(8) Uani 1 1 d . U . . .
H85A H 0.416725 0.815637 0.554685 0.153 Uiso 1 1 calc R . . . .
H85B H 0.338554 0.835842 0.555359 0.153 Uiso 1 1 calc R . . . .
C99 C 0.389(2) 0.9588(16) 0.4747(9) 0.161(13) Uani 1 1 d D U . . .
H99A H 0.437492 0.946994 0.475066 0.193 Uiso 1 1 calc R . . . .
H99B H 0.360978 0.950252 0.445890 0.193 Uiso 1 1 calc R . . . .
C35 C 0.0931(19) 0.4118(18) 0.3005(10) 0.139(9) Uani 1 1 d . U . . .
H35A H 0.086176 0.465514 0.301371 0.167 Uiso 1 1 calc R . . . .
H35B H 0.096011 0.399546 0.272378 0.167 Uiso 1 1 calc R . . . .
C39 C 0.2130(13) 0.1113(15) 0.3802(7) 0.108(7) Uani 1 1 d . U . . .
H39A H 0.165294 0.110140 0.383821 0.129 Uiso 1 1 calc R . . . .
H39B H 0.246741 0.098109 0.406740 0.129 Uiso 1 1 calc R . . . .
O8 O 0.2088(13) -0.0156(13) 0.3555(7) 0.153(7) Uani 1 1 d . U . . .
C43 C 0.009(2) -0.105(2) 0.2549(10) 0.175(12) Uani 1 1 d . U . . .
H43A H 0.023801 -0.153020 0.246790 0.211 Uiso 1 1 calc R . . . .
H43B H 0.023178 -0.066887 0.237420 0.211 Uiso 1 1 calc R . . . .
C90 C 0.228(2) 1.1522(16) 0.6363(10) 0.160(10) Uani 1 1 d D U . . .
H90A H 0.205715 1.153287 0.606161 0.192 Uiso 1 1 calc R . . . .
H90B H 0.192645 1.170175 0.649582 0.192 Uiso 1 1 calc R . . . .
C94 C 0.453(2) 1.337(2) 0.5931(11) 0.163(11) Uani 1 1 d . U . . .
H94A H 0.471876 1.382584 0.584572 0.195 Uiso 1 1 calc R . . . .
H94B H 0.489557 1.314302 0.615643 0.195 Uiso 1 1 calc R . . . .
C97 C 0.398(4) 1.149(3) 0.4694(17) 0.27(3) Uani 1 1 d . U . . .
H97A H 0.421547 1.177139 0.451825 0.324 Uiso 1 1 calc R . . . .
H97B H 0.349188 1.165170 0.462339 0.324 Uiso 1 1 calc R . . . .
C46 C -0.166(2) 0.042(3) 0.2703(11) 0.184(11) Uani 1 1 d . U . . .
H46A H -0.139666 0.043497 0.299733 0.221 Uiso 1 1 calc R . . . .
H46B H -0.216643 0.038178 0.268960 0.221 Uiso 1 1 calc R . . . .
O24 O 0.3898(19) 1.0213(17) 0.4769(10) 0.210(13) Uani 1 1 d . U . . .
C48 C -0.125(2) 0.250(3) 0.2400(11) 0.188(12) Uani 1 1 d . U . . .
H48A H -0.092938 0.234961 0.223428 0.226 Uiso 1 1 calc R . . . .
H48B H -0.166413 0.275171 0.222335 0.226 Uiso 1 1 calc R . . . .
C50A C -0.023(3) 0.400(3) 0.275(2) 0.150(14) Uani 0.5 1 d D U P C 1
H50A H -0.056089 0.426032 0.286992 0.180 Uiso 0.5 1 calc R . P C 1
H50B H -0.008612 0.435129 0.255853 0.180 Uiso 0.5 1 calc R . P C 1
C96 C 0.471(3) 1.228(3) 0.5133(13) 0.26(2) Uani 1 1 d D U . . .
H96A H 0.515517 1.210339 0.508984 0.318 Uiso 1 1 calc R . . . .
H96B H 0.451765 1.264260 0.491385 0.318 Uiso 1 1 calc R . . . .
C95 C 0.488(3) 1.266(3) 0.5505(12) 0.211(16) Uani 1 1 d D U . . .
H95A H 0.515921 1.234079 0.572702 0.253 Uiso 1 1 calc R . . . .
H95B H 0.518514 1.308636 0.548053 0.253 Uiso 1 1 calc R . . . .
C89 C 0.239(2) 1.0779(17) 0.6470(17) 0.23(2) Uani 1 1 d D U . . .
H89A H 0.238473 1.072425 0.676194 0.271 Uiso 1 1 calc R . . . .
H89B H 0.198377 1.049699 0.630023 0.271 Uiso 1 1 calc R . . . .
C49A C -0.054(3) 0.344(3) 0.2533(13) 0.147(15) Uani 0.5 1 d D U P C 1
H49A H -0.018682 0.316354 0.243806 0.177 Uiso 0.5 1 calc R . P C 1
H49B H -0.088408 0.363336 0.228276 0.177 Uiso 0.5 1 calc R . P C 1
C40 C 0.2182(19) 0.0599(18) 0.3482(11) 0.147(10) Uani 1 1 d . U . . .
H40A H 0.183145 0.073987 0.322345 0.177 Uiso 1 1 calc R . . . .
H40B H 0.264949 0.065858 0.343553 0.177 Uiso 1 1 calc R . . . .
C86 C 0.4126(19) 0.8726(18) 0.6059(9) 0.145(10) Uani 1 1 d . U . . .
H86A H 0.416286 0.827776 0.623017 0.174 Uiso 1 1 calc R . . . .
H86B H 0.458988 0.896546 0.612159 0.174 Uiso 1 1 calc R . . . .
C4 C 0.1801(15) 0.1121(18) 0.0664(9) 0.121(8) Uani 1 1 d . U . . .
H4A H 0.190205 0.082547 0.045524 0.145 Uiso 1 1 calc R . . . .
C5 C 0.2039(15) 0.1782(17) 0.0693(7) 0.116(8) Uani 1 1 d . U . . .
H5A H 0.228676 0.195552 0.050769 0.140 Uiso 1 1 calc R . . . .
C49B C -0.099(4) 0.3697(18) 0.263(3) 0.21(3) Uani 0.5 1 d D U P C 2
H49C H -0.095873 0.381183 0.235169 0.251 Uiso 0.5 1 calc R . P C 2
H49D H -0.141591 0.391874 0.268017 0.251 Uiso 0.5 1 calc R . P C 2
C50B C -0.042(5) 0.387(6) 0.292(3) 0.21(4) Uani 0.5 1 d D U P C 2
H50C H -0.054866 0.369195 0.316803 0.257 Uiso 0.5 1 calc R . P C 2
H50D H -0.047239 0.440650 0.292661 0.257 Uiso 0.5 1 calc R . P C 2
Br3A Br 0.7214(4) 0.9134(4) 0.7913(2) 0.135(2) Uani 0.5 1 d . . P A 1
Br4A Br 0.7921(4) 1.2554(4) 0.7625(2) 0.127(2) Uani 0.5 1 d . . P B 1
C98 C 0.398(2) 1.077(3) 0.4575(14) 0.192(17) Uani 1 1 d . . . . .
H98A H 0.361288 1.073715 0.430839 0.230 Uiso 1 1 calc R . . . .
H98B H 0.442980 1.069203 0.450851 0.230 Uiso 1 1 calc R . . . .


_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
Br2 C6 1.82(3) . ?
Br3B C53 1.889(14) . ?
Br4B C56 1.832(14) . ?
O1 C27 1.43(2) . ?
O14 C77 1.40(2) . ?
O13 C77 1.33(2) . ?
O16 C84 1.40(2) . ?
N3 C14 1.42(3) . ?
N3 C20 1.385(16) . ?
N1 C7 1.43(2) . ?
N1 C1 1.29(3) . ?
O3 C34 1.40(3) . ?
O2 C27 1.46(2) . ?
O4 C34 1.38(2) . ?
N8 C64 1.31(2) . ?
N8 C70 1.330(18) . ?
N7 C64 1.28(2) . ?
N7 C65 1.357(18) . ?
O6 C36 1.33(3) . ?
O6 C37 1.48(3) . ?
O15 C84 1.37(2) . ?
O7 C38 1.42(2) . ?
O7 C39 1.37(3) . ?
N4 C14 1.24(2) . ?
N4 C15 1.392(18) . ?
N2 C2 1.34(3) . ?
N2 C1 1.38(3) . ?
O17 C100 1.41(3) . ?
O17 C85 1.43(3) . ?
N6 C57 1.43(2) . ?
N6 C51 1.25(3) . ?
C74 C75 1.3900 . ?
C74 C73 1.3900 . ?
C74 C77 1.401(2) . ?
C75 C76 1.3900 . ?
C76 C71 1.3900 . ?
C71 C72 1.3900 . ?
C71 C66 1.404(2) . ?
C72 C73 1.3900 . ?
O19 C88 1.39(4) . ?
O19 C89 1.33(4) . ?
O21 C92 1.39(3) . ?
O21 C93 1.18(4) . ?
C14 C11 1.50(3) . ?
O9 C42 1.45(3) . ?
O9 C43 1.40(4) . ?
C83 C78 1.3900 . ?
C83 C82 1.3900 . ?
C78 C79 1.3900 . ?
C78 C69 1.404(2) . ?
C79 C80 1.3900 . ?
C80 C81 1.3900 . ?
C81 C82 1.3900 . ?
C81 C84 1.401(2) . ?
C2 C7 1.35(3) . ?
C2 C3 1.42(3) . ?
C62 C61 1.35(3) . ?
C62 C63 1.401(2) . ?
C27 C24 1.401(2) . ?
O18 C87 1.29(3) . ?
O18 C86 1.45(4) . ?
C9 C10 1.31(3) . ?
C9 C8 1.44(3) . ?
C57 C56 1.3900 . ?
C57 C52 1.3900 . ?
C56 C55 1.3900 . ?
C56 Br4A 1.941(14) . ?
C55 C54 1.3900 . ?
C54 C53 1.3900 . ?
C53 C52 1.3900 . ?
C53 Br3A 2.033(15) . ?
C52 N5 1.30(2) . ?
O20 C91 1.38(4) . ?
O20 C90 1.24(3) . ?
C16 C15 1.3900 . ?
C16 C17 1.3900 . ?
C16 C21 1.405(2) . ?
C15 C20 1.3900 . ?
C20 C19 1.3900 . ?
C19 C18 1.3900 . ?
C19 C28 1.405(2) . ?
C18 C17 1.3900 . ?
C7 C6 1.400(2) . ?
C28 C29 1.3900 . ?
C28 C33 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C31 C34 1.401(2) . ?
C32 C33 1.3900 . ?
C24 C23 1.3900 . ?
C24 C25 1.3900 . ?
C23 C22 1.3900 . ?
C22 C21 1.3900 . ?
C21 C26 1.3900 . ?
C26 C25 1.3900 . ?
C61 C64 1.48(3) . ?
C61 C60 1.44(3) . ?
O22 C94 1.35(4) . ?
O22 C95 1.27(4) . ?
C51 N5 1.27(3) . ?
C51 C58 1.400(2) . ?
O5 C35 1.34(4) . ?
O5 C50A 1.40(7) . ?
O5 C50B 1.51(9) . ?
C1 C8 1.401(2) . ?
C6 C5 1.53(3) . ?
C66 C65 1.3900 . ?
C66 C67 1.3900 . ?
C65 C70 1.3900 . ?
C70 C69 1.3900 . ?
C69 C68 1.3900 . ?
C68 C67 1.3900 . ?
C13 C12 1.44(3) . ?
C13 C8 1.35(3) . ?
O12 C48 1.32(4) . ?
O12 C49A 1.51(2) . ?
O12 C49B 1.500(2) . ?
C12 C11 1.32(3) . ?
C59 C60 1.40(3) . ?
C59 C58 1.30(3) . ?
C10 C11 1.42(3) . ?
O23 C97 1.20(5) . ?
O23 C96 1.41(5) . ?
C36 C35 1.46(4) . ?
O10 C44 1.37(4) . ?
O10 C45 1.31(4) . ?
C37 C38 1.4500(4) . ?
C92 C91 1.51(4) . ?
Br1 C3 1.86(3) . ?
C87 C88 1.55(4) . ?
O11 C47 1.45(4) . ?
O11 C46 1.48(5) . ?
C93 C94 1.42(5) . ?
C58 C63 1.41(3) . ?
C100 C99 1.400(2) . ?
C41 C42 1.35(3) . ?
C41 O8 1.36(3) . ?
C3 C4 1.36(3) . ?
C44 C43 1.44(5) . ?
C47 C48 1.61(5) . ?
C45 C46 1.37(5) . ?
C85 C86 1.47(4) . ?
C99 O24 1.14(3) . ?
C39 C40 1.45(4) . ?
O8 C40 1.42(4) . ?
C90 C89 1.400(2) . ?
C97 C98 1.37(6) . ?
O24 C98 1.24(4) . ?
C50A C49A 1.31(2) . ?
C96 C95 1.400(2) . ?
C4 C5 1.29(4) . ?
C49B C50B 1.30(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
C20 N3 C14 104.1(14) . . ?
C1 N1 C7 112.4(19) . . ?
C64 N8 C70 106.3(17) . . ?
C64 N7 C65 110.2(17) . . ?
C36 O6 C37 117.2(18) . . ?
C39 O7 C38 114.3(18) . . ?
C14 N4 C15 109.6(17) . . ?
C2 N2 C1 103.5(19) . . ?
C100 O17 C85 109(2) . . ?
C51 N6 C57 108(2) . . ?
C75 C74 C73 120.0 . . ?
C75 C74 C77 118.8(14) . . ?
C73 C74 C77 121.2(14) . . ?
C74 C75 C76 120.0 . . ?
C71 C76 C75 120.0 . . ?
C76 C71 C72 120.0 . . ?
C76 C71 C66 118.9(10) . . ?
C72 C71 C66 121.1(10) . . ?
C71 C72 C73 120.0 . . ?
C72 C73 C74 120.0 . . ?
C89 O19 C88 116(2) . . ?
C93 O21 C92 122(3) . . ?
N3 C14 C11 121.5(19) . . ?
N4 C14 N3 112.1(18) . . ?
N4 C14 C11 126(2) . . ?
C43 O9 C42 120(2) . . ?
C78 C83 C82 120.0 . . ?
C83 C78 C69 121.2(11) . . ?
C79 C78 C83 120.0 . . ?
C79 C78 C69 118.7(11) . . ?
C78 C79 C80 120.0 . . ?
C81 C80 C79 120.0 . . ?
C80 C81 C82 120.0 . . ?
C80 C81 C84 119.3(15) . . ?
C82 C81 C84 120.6(15) . . ?
C81 C82 C83 120.0 . . ?
N2 C2 C7 115.6(19) . . ?
N2 C2 C3 127(2) . . ?
C7 C2 C3 117(2) . . ?
C61 C62 C63 122.6(19) . . ?
O1 C27 O2 103.5(10) . . ?
C24 C27 O1 128.0(17) . . ?
C24 C27 O2 128.5(16) . . ?
C87 O18 C86 111(3) . . ?
C10 C9 C8 126(2) . . ?
C56 C57 N6 136.7(14) . . ?
C56 C57 C52 120.0 . . ?
C52 C57 N6 103.0(14) . . ?
C57 C56 Br4B 113.7(8) . . ?
C57 C56 Br4A 120.6(8) . . ?
C55 C56 Br4B 122.4(8) . . ?
C55 C56 C57 120.0 . . ?
C55 C56 Br4A 117.9(8) . . ?
C54 C55 C56 120.0 . . ?
C55 C54 C53 120.0 . . ?
C54 C53 Br3B 123.2(9) . . ?
C54 C53 Br3A 110.3(8) . . ?
C52 C53 Br3B 114.5(9) . . ?
C52 C53 C54 120.0 . . ?
C52 C53 Br3A 123.2(8) . . ?
C53 C52 C57 120.0 . . ?
N5 C52 C57 105.5(17) . . ?
N5 C52 C53 134.3(17) . . ?
C90 O20 C91 108(3) . . ?
C15 C16 C17 120.0 . . ?
C15 C16 C21 121.2(10) . . ?
C17 C16 C21 118.7(10) . . ?
C16 C15 N4 133.2(11) . . ?
C20 C15 N4 106.6(11) . . ?
C20 C15 C16 120.0 . . ?
N3 C20 C15 107.5(10) . . ?
N3 C20 C19 132.4(10) . . ?
C19 C20 C15 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 C28 121.5(10) . . ?
C18 C19 C28 118.3(10) . . ?
C17 C18 C19 120.0 . . ?
C18 C17 C16 120.0 . . ?
O16 C84 C81 124(2) . . ?
O15 C84 O16 103.4(10) . . ?
O15 C84 C81 133(2) . . ?
C2 C7 N1 99.2(16) . . ?
C2 C7 C6 129(2) . . ?
C6 C7 N1 131(2) . . ?
C29 C28 C19 121.5(11) . . ?
C29 C28 C33 120.0 . . ?
C33 C28 C19 118.4(11) . . ?
C30 C29 C28 120.0 . . ?
C29 C30 C31 120.0 . . ?
C30 C31 C34 120.3(15) . . ?
C32 C31 C30 120.0 . . ?
C32 C31 C34 119.5(15) . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C28 120.0 . . ?
C23 C24 C27 119.9(14) . . ?
C23 C24 C25 120.0 . . ?
C25 C24 C27 120.0(14) . . ?
C22 C23 C24 120.0 . . ?
C23 C22 C21 120.0 . . ?
C22 C21 C16 120.7(10) . . ?
C26 C21 C16 119.1(10) . . ?
C26 C21 C22 120.0 . . ?
C21 C26 C25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C62 C61 C64 125.2(17) . . ?
C62 C61 C60 115.7(19) . . ?
C60 C61 C64 119.0(18) . . ?
O4 C34 O3 109.2(10) . . ?
O4 C34 C31 130(2) . . ?
C31 C34 O3 121.2(19) . . ?
N8 C64 C61 126(2) . . ?
N7 C64 N8 111(2) . . ?
N7 C64 C61 123(2) . . ?
C95 O22 C94 113(3) . . ?
N6 C51 N5 111.3(19) . . ?
N6 C51 C58 121(3) . . ?
N5 C51 C58 127(3) . . ?
C51 N5 C52 112(2) . . ?
C35 O5 C50A 110(3) . . ?
C35 O5 C50B 139(5) . . ?
N1 C1 N2 108.4(14) . . ?
N1 C1 C8 128(2) . . ?
N2 C1 C8 124(2) . . ?
C7 C6 Br2 122.9(17) . . ?
C7 C6 C5 110(2) . . ?
C5 C6 Br2 127.2(15) . . ?
C65 C66 C71 119.7(11) . . ?
C65 C66 C67 120.0 . . ?
C67 C66 C71 120.2(11) . . ?
N7 C65 C66 137.0(12) . . ?
N7 C65 C70 102.9(12) . . ?
C66 C65 C70 120.0 . . ?
N8 C70 C65 109.4(12) . . ?
N8 C70 C69 130.5(12) . . ?
C69 C70 C65 120.0 . . ?
C70 C69 C78 123.9(11) . . ?
C70 C69 C68 120.0 . . ?
C68 C69 C78 116.1(11) . . ?
C67 C68 C69 120.0 . . ?
C68 C67 C66 120.0 . . ?
C8 C13 C12 120(2) . . ?
C48 O12 C49A 100(3) . . ?
C48 O12 C49B 111(4) . . ?
C11 C12 C13 120(2) . . ?
C58 C59 C60 127(2) . . ?
O13 C77 O14 107.1(10) . . ?
O13 C77 C74 129(2) . . ?
C74 C77 O14 123.4(19) . . ?
C9 C10 C11 116(2) . . ?
C12 C11 C14 120(2) . . ?
C12 C11 C10 122(2) . . ?
C10 C11 C14 118.2(19) . . ?
C97 O23 C96 121(5) . . ?
O6 C36 C35 114(2) . . ?
C59 C60 C61 118(2) . . ?
C1 C8 C9 122(2) . . ?
C13 C8 C9 114.8(17) . . ?
C13 C8 C1 123(2) . . ?
C45 O10 C44 116(3) . . ?
C38 C37 O6 115.6(18) . . ?
O21 C92 C91 116(2) . . ?
O18 C87 C88 105(3) . . ?
O7 C38 C37 108.4(12) . . ?
C47 O11 C46 129(3) . . ?
O20 C91 C92 114(3) . . ?
O21 C93 C94 122(4) . . ?
C59 C58 C51 129(2) . . ?
C59 C58 C63 114.8(18) . . ?
C63 C58 C51 116(2) . . ?
C99 C100 O17 105(2) . . ?
C42 C41 O8 115(2) . . ?
C58 C63 C62 121(2) . . ?
C41 C42 O9 115(2) . . ?
O19 C88 C87 110(2) . . ?
C2 C3 Br1 122(2) . . ?
C4 C3 C2 116(3) . . ?
C4 C3 Br1 120(2) . . ?
O10 C44 C43 105(4) . . ?
O11 C47 C48 120(3) . . ?
O10 C45 C46 120(4) . . ?
O17 C85 C86 110(3) . . ?
O24 C99 C100 139(4) . . ?
O5 C35 C36 117(3) . . ?
O7 C39 C40 108(2) . . ?
C41 O8 C40 114(3) . . ?
O9 C43 C44 113(3) . . ?
O20 C90 C89 125(4) . . ?
O22 C94 C93 112(3) . . ?
O23 C97 C98 122(5) . . ?
C45 C46 O11 113(4) . . ?
C99 O24 C98 142(4) . . ?
O12 C48 C47 94(2) . . ?
C49A C50A O5 112(6) . . ?
C95 C96 O23 125(5) . . ?
O22 C95 C96 113(5) . . ?
O19 C89 C90 116(3) . . ?
C50A C49A O12 120(4) . . ?
O8 C40 C39 117(3) . . ?
O18 C86 C85 105(2) . . ?
C5 C4 C3 128(3) . . ?
C4 C5 C6 119(2) . . ?
C50B C49B O12 94(7) . . ?
C49B C50B O5 145(10) . . ?
O24 C98 C97 128(5) . . ?

_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 0.434 -0.744 -0.434 3426.8 782.4 ?

_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.759
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
####################################################################### 
# 
# 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_bhw319_2_0m
_database_code_depnum_ccdc_archive 'CCDC 2049901'
loop_
_audit_author_name
_audit_author_address
'Wilson B.H.'
;University of Windsor
Canada
;
_audit_update_record             
;
2020-12-12 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_bhw319_2_0m         
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range       10.0 Ratio 
RESPONSE: The 24-crown-8 ether moities have residual disorder that was unable to be modeled in a chemically
sensible fashion.This results in the carbon and oxygen atoms having larger thermal parameters than usual.  
;
_vrf_PLAT241_bhw319_2_0m         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C103 Check 
RESPONSE: The 24-crown-8 ether moities have residual disorder that was unable to be modeled in a chemically
sensible fashion.This results in the carbon and oxygen atoms having larger thermal parameters than usual.  
;
_vrf_PLAT242_bhw319_2_0m         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        O22 Check 
RESPONSE: The 24-crown-8 ether moities have residual disorder that was unable to be modeled in a chemically
sensible fashion.This results in the carbon and oxygen atoms having larger thermal parameters than usual.  
;
# end Validation Reply Form

_audit_creation_date             2019-12-12
_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
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C38 H29 Br2 N4 O4, B F4, C16 H32 O8, 0.5(C4 H10 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C57 H67.50 B Br2 F4 N4.50 O12.50'
_chemical_formula_weight         1262.28
_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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   28.49(2)
_cell_length_b                   10.505(4)
_cell_length_c                   43.418(18)
_cell_angle_alpha                90
_cell_angle_beta                 106.34(5)
_cell_angle_gamma                90
_cell_volume                     12468(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    101844
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      65.084
_cell_measurement_theta_min      2.121
_shelx_estimated_absorpt_T_max   0.660
_shelx_estimated_absorpt_T_min   0.464
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1342 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.6596. 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    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            98593
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         2.121
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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                   'I\mS Microfocus Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16902
_reflns_number_total             21024
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ApexIII
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         2.019
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.126
_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     1512
_refine_ls_number_reflns         21024
_refine_ls_number_restraints     474
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.1139
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1390P)²+90.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3088
_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. The 24-crown-8 ether rings 
feature residual disorder that cannot be modeled in a chemically sensible manner.
The DFIX restraints were required to model the C-C and C-O bonds in a chemically
senible manner. The RIGU/SIMU restaints were required for the thermal parameters of the
C and O atoms of the 24-crown-8 ether rings. One of the ethyl ester groups required DFIX 
and RIGU restraints for the bond lengths and thermal eliposids to be modelled in a chemically
sensible manner. One of the tetrafluoroborate anions which was not participating in any
hydrogen bonding interactions is modeled as disordered over two positions, one of which 
required the DFIX and RIGU restraints for the bondlength and thermal parameters to be modelled
in a chemically sinsible manner. The diethyl ether molecule is modelled with one carbon disordered 
over two positions. The inital CHECKCIF report returned a PLAT602 alert for a large solvent
acessible void. Therefore the solvent mask function of OLEX2 (SQUEEZE funtion of PLATON) was applied
and returned four voids of 222.0 cubic angestroms in the unit cell, each containing 46 electrons. 
This corrosponds to 22 electrons per rotaxane which equates to one acetonitrile molecules (23 electrons).
;
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C113-C114
 1.5 with sigma of 0.02
 C1A-C113
 1.5 with sigma of 0.02
 F7B-F5B
 2.29 with sigma of 0.02
 F5B-F6B
 2.29 with sigma of 0.02
 F5B-F8B
 2.29 with sigma of 0.02
 F8B-F6B
 2.29 with sigma of 0.02
 F6B-F7B
 2.29 with sigma of 0.02
 F7B-F8B
 2.29 with sigma of 0.02
 F5B-B2
 1.402 with sigma of 0.02
 C106-O24
 1.448 with sigma of 0.02
 C102-C101
 1.504 with sigma of 0.02
 C95-C96
 1.504 with sigma of 0.02
 O17-C108
 1.448 with sigma of 0.02
 O23-C105
 1.448 with sigma of 0.02
 O24-C106
 1.448 with sigma of 0.001
 O24-C107
 1.448 with sigma of 0.001
 C100-C99
 1.448 with sigma of 0.01
 C96-C95
 1.504 with sigma of 0.01
 C97-C98
 1.504 with sigma of 0.01
 C99-C100
 1.504 with sigma of 0.01
 C101-C102
 1.504 with sigma of 0.01
 C103-C104
 1.504 with sigma of 0.01
 C105-C106
 1.504 with sigma of 0.01
 C107-C108
 1.504 with sigma of 0.01
 O17-C93
 1.448 with sigma of 0.01
 O18-C94
 1.448 with sigma of 0.01
 O18-C95
 1.448 with sigma of 0.01
 O19-C97
 1.448 with sigma of 0.01
 O20-C98
 1.448 with sigma of 0.01
 O21-C101
 1.448 with sigma of 0.01
 O21-C100
 1.448 with sigma of 0.01
 C102-O22
 1.448 with sigma of 0.01
 O22-C103
 1.448 with sigma of 0.01
 O23-C104
 1.448 with sigma of 0.01
 C106-C107
 2.3 with sigma of 0.02
 C104-C105
 2.3 with sigma of 0.001
 O23-C106
 2.3 with sigma of 0.001
 C38-C37
 1.5 with sigma of 0.02
 C52-C51
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C28: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O2 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C113 \\sim C114: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C113 \\sim C1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C28 \\sim C29: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C82 \\sim C83: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C82: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C78 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O13 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C33 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C37: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C37 \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O3 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C91 \\sim C92: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 B2, F5A, F7A, F8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F5B, F6B, F7B, F8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, O7, O8, O9, O10, O11, O12, C39, C40, C41, C42, C43, C44, C45, C46,
 C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, O18, O19, O20, O21, O22, O23, O24, C93, C94, C95, C96, C97, C98, C99,
 C100, C101, C102, C103, C104, C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C28, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H11H(0.4) H11I(0.4) H11F(0.6) H11G(0.6) C1A(0.6) H1AA(0.6)
 H1AB(0.6) H1AC(0.6) C114(0.4) H11J(0.4) H11K(0.4) H11L(0.4) F5A(0.6) F6A(0.6)
 F7A(0.6) F8A(0.6) F5B(0.4) F6B(0.4) F7B(0.4) F8B(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C37(H37A,H37B), C82(H82A,H82B), C91(H91A,H91B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C105(H10K,H10L), C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R), C111(H11A,
 H11B), C113(H11H,H11I), C113(H11F,H11G)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C4(H4A), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
  C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C31(H31),
 C32(H32), C34(H34), C35(H35), N5(H5A), N7(H7), N8(H8), C58(H58), C59(H59),
 C63(H63), C64(H64), C66(H66), C67(H67), C71(H71), C72(H72), C76(H76), C77(H77),
  C79(H79), C80(H80), C85(H85), C86(H86), C88(H88), C89(H89)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C83(H83A,H83B,H83C), C92(H92A,H92B,
 H92C), C112(H11C,H11D,H11E), C1A(H1AA,H1AB,H1AC), C114(H11J,H11K,H11L),
 C110(H11M,H11N,H11O)
;
_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
Br1 Br 0.19286(4) -0.24678(16) 0.27676(4) 0.1190(7) Uani 1 1 d . . . . .
Br2 Br -0.04458(3) -0.32063(8) 0.24898(2) 0.0508(2) Uani 1 1 d . . . . .
O1 O 0.1974(4) 0.0187(10) 0.5790(2) 0.135(4) Uani 1 1 d . . . . .
O2 O 0.2290(3) 0.1900(9) 0.60485(17) 0.096(2) Uani 1 1 d . U . . .
O3 O -0.0961(2) 0.9413(6) 0.30996(14) 0.0656(17) Uani 1 1 d . U . . .
O4 O -0.1557(2) 0.9316(7) 0.33386(17) 0.089(2) Uani 1 1 d . U . . .
N1 N 0.11144(19) -0.0955(5) 0.30608(12) 0.0353(12) Uani 1 1 d . . . . .
H1 H 0.140827 -0.063343 0.314336 0.042 Uiso 1 1 calc R . . . .
N2 N 0.03065(18) -0.1251(4) 0.29651(11) 0.0275(11) Uani 1 1 d . . . . .
N3 N 0.02246(16) 0.4098(4) 0.39854(10) 0.0227(10) Uani 1 1 d . . . . .
H3 H 0.004069 0.432202 0.379416 0.027 Uiso 1 1 calc R . . . .
N4 N 0.07359(17) 0.3025(4) 0.43608(10) 0.0224(10) Uani 1 1 d . . . . .
H4 H 0.094627 0.243662 0.445695 0.027 Uiso 1 1 calc R . . . .
C1 C 0.0694(2) -0.0608(5) 0.31282(13) 0.0291(13) Uani 1 1 d . . . . .
C2 C 0.0984(3) -0.1919(6) 0.28349(14) 0.0385(15) Uani 1 1 d . . . . .
C3 C 0.1242(3) -0.2695(9) 0.26812(19) 0.056(2) Uani 1 1 d . . . . .
C4 C 0.1000(3) -0.3633(8) 0.24830(18) 0.058(2) Uani 1 1 d . . . . .
H4A H 0.117828 -0.418119 0.238280 0.070 Uiso 1 1 calc R . . . .
C5 C 0.0497(3) -0.3807(7) 0.24236(15) 0.0422(16) Uani 1 1 d . . . . .
H5 H 0.033536 -0.446468 0.228349 0.051 Uiso 1 1 calc R . . . .
C6 C 0.0238(2) -0.3024(6) 0.25684(14) 0.0341(14) Uani 1 1 d . . . . .
C7 C 0.0481(2) -0.2085(6) 0.27768(13) 0.0312(13) Uani 1 1 d . . . . .
C8 C 0.0665(2) 0.0369(5) 0.33616(12) 0.0249(12) Uani 1 1 d . . . . .
C9 C 0.0213(2) 0.0610(5) 0.34103(13) 0.0275(12) Uani 1 1 d . . . . .
H9 H -0.006559 0.015524 0.328858 0.033 Uiso 1 1 calc R . . . .
C10 C 0.0161(2) 0.1502(5) 0.36333(13) 0.0246(12) Uani 1 1 d . . . . .
H10 H -0.015075 0.166319 0.366420 0.029 Uiso 1 1 calc R . . . .
C11 C 0.0572(2) 0.2158(5) 0.38113(12) 0.0239(12) Uani 1 1 d . . . . .
C12 C 0.1031(2) 0.1948(6) 0.37638(13) 0.0289(13) Uani 1 1 d . . . . .
H12 H 0.130845 0.241286 0.388303 0.035 Uiso 1 1 calc R . . . .
C13 C 0.1073(2) 0.1049(5) 0.35395(13) 0.0270(12) Uani 1 1 d . . . . .
H13 H 0.138358 0.089380 0.350618 0.032 Uiso 1 1 calc R . . . .
C14 C 0.0515(2) 0.3088(5) 0.40498(13) 0.0235(11) Uani 1 1 d . . . . .
C15 C 0.0580(2) 0.4043(5) 0.45103(13) 0.0216(11) Uani 1 1 d . . . . .
C16 C 0.0701(2) 0.4395(5) 0.48361(13) 0.0256(12) Uani 1 1 d . . . . .
C17 C 0.0481(2) 0.5524(6) 0.48939(14) 0.0301(13) Uani 1 1 d . . . . .
H17 H 0.055075 0.582616 0.510831 0.036 Uiso 1 1 calc R . . . .
C18 C 0.0161(2) 0.6230(5) 0.46493(14) 0.0299(13) Uani 1 1 d . . . . .
H18 H 0.001744 0.697863 0.470567 0.036 Uiso 1 1 calc R . . . .
C19 C 0.0046(2) 0.5883(5) 0.43285(14) 0.0263(12) Uani 1 1 d . . . . .
C20 C 0.0259(2) 0.4738(5) 0.42680(12) 0.0223(11) Uani 1 1 d . . . . .
C21 C 0.1039(2) 0.3630(6) 0.50909(13) 0.0282(13) Uani 1 1 d . . . . .
C22 C 0.1006(2) 0.2314(6) 0.50850(14) 0.0327(14) Uani 1 1 d . . . . .
H22 H 0.076215 0.190456 0.491964 0.039 Uiso 1 1 calc R . . . .
C23 C 0.1329(3) 0.1587(7) 0.53204(16) 0.0461(18) Uani 1 1 d . . . . .
H23 H 0.130893 0.068446 0.531100 0.055 Uiso 1 1 calc R . . . .
C24 C 0.1673(3) 0.2159(9) 0.55635(17) 0.051(2) Uani 1 1 d . . . . .
C25 C 0.1708(3) 0.3469(9) 0.55745(16) 0.050(2) Uani 1 1 d . . . . .
H25 H 0.195009 0.386827 0.574264 0.061 Uiso 1 1 calc R . . . .
C26 C 0.1389(3) 0.4209(7) 0.53410(15) 0.0409(16) Uani 1 1 d . . . . .
H26 H 0.141148 0.511099 0.535242 0.049 Uiso 1 1 calc R . . . .
C27 C 0.2000(4) 0.1337(13) 0.5823(2) 0.080(3) Uani 1 1 d . U . . .
C28 C 0.2568(5) 0.0857(17) 0.6269(3) 0.127(4) Uani 1 1 d . U . . .
H28A H 0.271354 0.022765 0.615303 0.153 Uiso 1 1 calc R . . . .
H28B H 0.236193 0.041625 0.638521 0.153 Uiso 1 1 calc R . . . .
C29 C 0.3008(8) 0.183(3) 0.6520(6) 0.228(12) Uani 1 1 d . U . . .
H29A H 0.323153 0.214660 0.640322 0.342 Uiso 1 1 calc GR . . . .
H29B H 0.319234 0.133476 0.670690 0.342 Uiso 1 1 calc GR . . . .
H29C H 0.284682 0.254667 0.659265 0.342 Uiso 1 1 calc GR . . . .
C30 C -0.0265(2) 0.6654(5) 0.40664(14) 0.0273(12) Uani 1 1 d . . . . .
C31 C -0.0121(2) 0.6908(5) 0.37879(15) 0.0306(13) Uani 1 1 d . . . . .
H31 H 0.017253 0.654381 0.376536 0.037 Uiso 1 1 calc R . . . .
C32 C -0.0397(2) 0.7671(6) 0.35482(15) 0.0345(14) Uani 1 1 d . . . . .
H32 H -0.029110 0.783835 0.336309 0.041 Uiso 1 1 calc R . . . .
C33 C -0.0829(2) 0.8198(6) 0.35763(17) 0.0406(15) Uani 1 1 d . U . . .
C34 C -0.0981(3) 0.7935(7) 0.38469(17) 0.0438(17) Uani 1 1 d . . . . .
H34 H -0.128113 0.827724 0.386517 0.053 Uiso 1 1 calc R . . . .
C35 C -0.0701(2) 0.7181(6) 0.40882(15) 0.0349(14) Uani 1 1 d . . . . .
H35 H -0.080816 0.701857 0.427294 0.042 Uiso 1 1 calc R . . . .
C36 C -0.1115(3) 0.9035(9) 0.3309(2) 0.0592(19) Uani 1 1 d . U . . .
C37 C -0.1897(4) 0.9984(13) 0.3046(3) 0.108(3) Uani 1 1 d D U . . .
H37A H -0.180591 0.981146 0.284590 0.129 Uiso 1 1 calc R . . . .
H37B H -0.224538 0.977414 0.301585 0.129 Uiso 1 1 calc R . . . .
C38 C -0.1778(6) 1.1249(17) 0.3161(5) 0.157(6) Uani 1 1 d D U . . .
H38A H -0.191669 1.185602 0.298805 0.235 Uiso 1 1 calc GR . . . .
H38B H -0.142173 1.134837 0.323322 0.235 Uiso 1 1 calc GR . . . .
H38C H -0.191427 1.141068 0.334098 0.235 Uiso 1 1 calc GR . . . .
Br3 Br 0.54795(3) 0.84824(8) 0.75568(2) 0.0535(2) Uani 1 1 d . . . . .
Br4 Br 0.30823(4) 0.80676(15) 0.70963(3) 0.1061(5) Uani 1 1 d . . . . .
O13 O 0.6094(2) -0.3983(7) 0.69777(16) 0.082(2) Uani 1 1 d . U . . .
O14 O 0.6699(2) -0.3934(8) 0.67441(17) 0.087(2) Uani 1 1 d . U . . .
O15 O 0.2486(3) 0.2009(7) 0.40008(16) 0.083(2) Uani 1 1 d . . . . .
O16 O 0.2908(2) 0.3828(6) 0.40816(13) 0.0653(16) Uani 1 1 d . . . . .
N5 N 0.3942(2) 0.6427(5) 0.68801(12) 0.0389(13) Uani 1 1 d . . . . .
H5A H 0.364925 0.614941 0.677590 0.047 Uiso 1 1 calc R . . . .
N6 N 0.4756(2) 0.6596(5) 0.70355(11) 0.0336(12) Uani 1 1 d . . . . .
N7 N 0.49021(18) 0.1217(4) 0.60347(11) 0.0276(10) Uani 1 1 d . . . . .
H7 H 0.510751 0.106643 0.622439 0.033 Uiso 1 1 calc R . . . .
N8 N 0.43388(17) 0.2126(4) 0.56555(11) 0.0252(10) Uani 1 1 d . . . . .
H8 H 0.410741 0.265896 0.555606 0.030 Uiso 1 1 calc R . . . .
C55 C 0.4375(2) 0.6013(6) 0.68452(14) 0.0314(13) Uani 1 1 d . . . . .
C56 C 0.4565(3) 0.7449(6) 0.72076(15) 0.0362(15) Uani 1 1 d . . . . .
C57 C 0.4792(2) 0.8362(6) 0.74320(14) 0.0363(14) Uani 1 1 d . . . . .
C58 C 0.4509(3) 0.9165(7) 0.75588(16) 0.0470(18) Uani 1 1 d . . . . .
H58 H 0.466342 0.978514 0.771348 0.056 Uiso 1 1 calc R . . . .
C59 C 0.4005(3) 0.9077(8) 0.74636(18) 0.057(2) Uani 1 1 d . . . . .
H59 H 0.381622 0.964028 0.755167 0.068 Uiso 1 1 calc R . . . .
C60 C 0.3774(3) 0.8171(8) 0.72399(18) 0.052(2) Uani 1 1 d . . . . .
C61 C 0.4052(3) 0.7373(7) 0.71117(15) 0.0426(16) Uani 1 1 d . . . . .
C62 C 0.4418(2) 0.5018(5) 0.66165(13) 0.0313(13) Uani 1 1 d . . . . .
C63 C 0.4013(2) 0.4344(6) 0.64338(14) 0.0351(14) Uani 1 1 d . . . . .
H63 H 0.369744 0.452385 0.645611 0.042 Uiso 1 1 calc R . . . .
C64 C 0.4068(2) 0.3413(6) 0.62194(14) 0.0342(14) Uani 1 1 d . . . . .
H64 H 0.379185 0.295935 0.609367 0.041 Uiso 1 1 calc R . . . .
C65 C 0.4529(2) 0.3156(5) 0.61915(13) 0.0275(12) Uani 1 1 d . . . . .
C66 C 0.4941(2) 0.3799(5) 0.63746(13) 0.0291(13) Uani 1 1 d . . . . .
H66 H 0.525683 0.359792 0.635623 0.035 Uiso 1 1 calc R . . . .
C67 C 0.4879(2) 0.4749(6) 0.65867(14) 0.0328(14) Uani 1 1 d . . . . .
H67 H 0.515451 0.520975 0.671044 0.039 Uiso 1 1 calc R . . . .
C68 C 0.4593(2) 0.2181(5) 0.59637(13) 0.0265(12) Uani 1 1 d . . . . .
C69 C 0.4851(2) 0.0482(5) 0.57636(14) 0.0257(12) Uani 1 1 d . . . . .
C70 C 0.5073(2) -0.0667(6) 0.57205(15) 0.0319(13) Uani 1 1 d . . . . .
C71 C 0.4938(2) -0.1124(6) 0.54067(15) 0.0347(14) Uani 1 1 d . . . . .
H71 H 0.508840 -0.187711 0.535925 0.042 Uiso 1 1 calc R . . . .
C72 C 0.4586(2) -0.0512(6) 0.51578(15) 0.0341(14) Uani 1 1 d . . . . .
H72 H 0.450463 -0.088117 0.494965 0.041 Uiso 1 1 calc R . . . .
C73 C 0.4353(2) 0.0603(5) 0.52011(14) 0.0280(12) Uani 1 1 d . . . . .
C74 C 0.4502(2) 0.1079(5) 0.55172(13) 0.0250(12) Uani 1 1 d . . . . .
C75 C 0.5397(2) -0.1383(6) 0.59886(15) 0.0317(13) Uani 1 1 d . . . . .
C76 C 0.5255(2) -0.1587(6) 0.62677(15) 0.0357(14) Uani 1 1 d . . . . .
H76 H 0.495973 -0.121826 0.628607 0.043 Uiso 1 1 calc R . . . .
C77 C 0.5535(3) -0.2313(7) 0.65177(17) 0.0414(16) Uani 1 1 d . . . . .
H77 H 0.543226 -0.244444 0.670519 0.050 Uiso 1 1 calc R . . . .
C78 C 0.5969(3) -0.2849(7) 0.64930(19) 0.0488(17) Uani 1 1 d . U . . .
C79 C 0.6118(3) -0.2634(8) 0.62165(18) 0.0509(19) Uani 1 1 d . . . . .
H79 H 0.641690 -0.298757 0.619957 0.061 Uiso 1 1 calc R . . . .
C80 C 0.5835(3) -0.1913(7) 0.59695(18) 0.0459(17) Uani 1 1 d . . . . .
H80 H 0.593952 -0.177578 0.578286 0.055 Uiso 1 1 calc R . . . .
C81 C 0.6245(3) -0.3657(9) 0.6758(2) 0.063(2) Uani 1 1 d . U . . .
C82 C 0.7003(5) -0.4705(14) 0.7010(3) 0.107(3) Uani 1 1 d . U . . .
H82A H 0.735190 -0.464157 0.701399 0.128 Uiso 1 1 calc R . . . .
H82B H 0.696963 -0.438897 0.721748 0.128 Uiso 1 1 calc R . . . .
C83 C 0.6848(6) -0.5965(19) 0.6963(4) 0.146(6) Uani 1 1 d . U . . .
H83A H 0.692612 -0.630814 0.677372 0.219 Uiso 1 1 calc GR . . . .
H83B H 0.649394 -0.600509 0.693153 0.219 Uiso 1 1 calc GR . . . .
H83C H 0.701514 -0.646993 0.715234 0.219 Uiso 1 1 calc GR . . . .
C84 C 0.3967(2) 0.1189(6) 0.49376(13) 0.0303(13) Uani 1 1 d . . . . .
C85 C 0.3931(3) 0.2491(6) 0.48899(15) 0.0366(15) Uani 1 1 d . . . . .
H85 H 0.415567 0.304490 0.503063 0.044 Uiso 1 1 calc R . . . .
C86 C 0.3561(3) 0.2991(7) 0.46334(15) 0.0403(16) Uani 1 1 d . . . . .
H86 H 0.353668 0.388352 0.459694 0.048 Uiso 1 1 calc R . . . .
C87 C 0.3230(3) 0.2168(7) 0.44331(15) 0.0416(16) Uani 1 1 d . . . . .
C88 C 0.3263(3) 0.0888(7) 0.44812(16) 0.0464(17) Uani 1 1 d . . . . .
H88 H 0.303507 0.033692 0.434158 0.056 Uiso 1 1 calc R . . . .
C89 C 0.3625(3) 0.0392(7) 0.47315(15) 0.0405(16) Uani 1 1 d . . . . .
H89 H 0.364375 -0.050215 0.476518 0.049 Uiso 1 1 calc R . . . .
C90 C 0.2827(3) 0.2656(9) 0.4149(2) 0.055(2) Uani 1 1 d . . . . .
C91 C 0.2531(4) 0.4345(10) 0.3806(2) 0.074(3) Uani 1 1 d . U . . .
H91A H 0.220642 0.432610 0.384668 0.089 Uiso 1 1 calc R . . . .
H91B H 0.251489 0.384800 0.360968 0.089 Uiso 1 1 calc R . . . .
C92 C 0.2683(5) 0.5661(13) 0.3772(3) 0.113(4) Uani 1 1 d . U . . .
H92A H 0.243743 0.607741 0.359653 0.170 Uiso 1 1 calc GR . . . .
H92B H 0.299906 0.565859 0.372378 0.170 Uiso 1 1 calc GR . . . .
H92C H 0.271335 0.612488 0.397233 0.170 Uiso 1 1 calc GR . . . .
F1 F -0.3000(4) 0.3031(12) 0.3860(3) 0.198(6) Uani 1 1 d . . . . .
F2 F -0.29937(18) 0.4384(6) 0.34816(13) 0.0839(17) Uani 1 1 d . . . . .
F3 F -0.2281(3) 0.3874(11) 0.3852(3) 0.174(5) Uani 1 1 d . . . . .
F4 F -0.2797(4) 0.5023(13) 0.3992(2) 0.180(5) Uani 1 1 d . . . . .
B1 B -0.2754(4) 0.3995(17) 0.3791(4) 0.093(5) Uani 1 1 d . . . . .
O5 O 0.1153(3) 0.0463(5) 0.45198(12) 0.0674(16) Uani 1 1 d . U . . .
O6 O 0.1750(2) 0.2529(8) 0.45328(13) 0.0726(17) Uani 1 1 d . U . . .
O7 O 0.1614(2) 0.4931(7) 0.41947(16) 0.0740(16) Uani 1 1 d . U . . .
O8 O 0.0850(2) 0.5221(6) 0.36135(15) 0.0673(15) Uani 1 1 d . U . . .
O9 O -0.0128(3) 0.4528(6) 0.33028(14) 0.0741(17) Uani 1 1 d . U . . .
O10 O -0.0803(3) 0.3466(10) 0.3592(2) 0.115(3) Uani 1 1 d . U . . .
O11 O -0.0581(4) 0.2562(10) 0.4266(3) 0.117(3) Uani 1 1 d . U . . .
O12 O 0.0142(3) 0.0731(6) 0.44064(16) 0.083(2) Uani 1 1 d . U . . .
C39 C 0.1646(5) 0.0346(11) 0.4493(2) 0.093(3) Uani 1 1 d . U . . .
H39A H 0.178488 -0.048248 0.458270 0.111 Uiso 1 1 calc R . . . .
H39B H 0.163829 0.036768 0.426355 0.111 Uiso 1 1 calc R . . . .
C40 C 0.1953(4) 0.1362(14) 0.4661(2) 0.096(3) Uani 1 1 d . U . . .
H40A H 0.197452 0.132353 0.489289 0.115 Uiso 1 1 calc R . . . .
H40B H 0.228701 0.127272 0.463779 0.115 Uiso 1 1 calc R . . . .
C41 C 0.2056(3) 0.3686(13) 0.4638(2) 0.086(3) Uani 1 1 d . U . . .
H41A H 0.233394 0.368709 0.454353 0.104 Uiso 1 1 calc R . . . .
H41B H 0.218825 0.368847 0.487474 0.104 Uiso 1 1 calc R . . . .
C42 C 0.1741(4) 0.4859(11) 0.4529(2) 0.081(3) Uani 1 1 d . U . . .
H42A H 0.144185 0.480590 0.460164 0.097 Uiso 1 1 calc R . . . .
H42B H 0.192419 0.563193 0.462382 0.097 Uiso 1 1 calc R . . . .
C43 C 0.1409(4) 0.6160(9) 0.4076(3) 0.074(2) Uani 1 1 d . U . . .
H43A H 0.115120 0.640512 0.417681 0.089 Uiso 1 1 calc R . . . .
H43B H 0.166718 0.682227 0.412549 0.089 Uiso 1 1 calc R . . . .
C44 C 0.1209(3) 0.6029(11) 0.3737(3) 0.093(3) Uani 1 1 d . U . . .
H44A H 0.109281 0.688213 0.365163 0.112 Uiso 1 1 calc R . . . .
H44B H 0.148233 0.580326 0.364832 0.112 Uiso 1 1 calc R . . . .
C45 C 0.0648(5) 0.5248(10) 0.3275(2) 0.087(3) Uani 1 1 d . U . . .
H45A H 0.090952 0.505585 0.317299 0.104 Uiso 1 1 calc R . . . .
H45B H 0.052748 0.611901 0.321000 0.104 Uiso 1 1 calc R . . . .
C46 C 0.0230(4) 0.4312(9) 0.3152(2) 0.078(2) Uani 1 1 d . U . . .
H46A H 0.009201 0.441486 0.291735 0.094 Uiso 1 1 calc R . . . .
H46B H 0.035410 0.343025 0.319480 0.094 Uiso 1 1 calc R . . . .
C47 C -0.0566(4) 0.4053(10) 0.3127(2) 0.087(3) Uani 1 1 d . U . . .
H47A H -0.052593 0.315580 0.306922 0.104 Uiso 1 1 calc R . . . .
H47B H -0.068686 0.454752 0.292620 0.104 Uiso 1 1 calc R . . . .
C48 C -0.0954(4) 0.4134(12) 0.3332(4) 0.105(3) Uani 1 1 d . U . . .
H48A H -0.099623 0.503231 0.338806 0.126 Uiso 1 1 calc R . . . .
H48B H -0.127512 0.380887 0.320266 0.126 Uiso 1 1 calc R . . . .
C49 C -0.1102(4) 0.3594(11) 0.3812(4) 0.111(4) Uani 1 1 d . U . . .
H49A H -0.145526 0.346782 0.370636 0.133 Uiso 1 1 calc R . . . .
H49B H -0.104772 0.440794 0.393193 0.133 Uiso 1 1 calc R . . . .
C50 C -0.0863(7) 0.2448(13) 0.4019(4) 0.145(6) Uani 1 1 d . U . . .
H50A H -0.113335 0.192572 0.405374 0.173 Uiso 1 1 calc R . . . .
H50B H -0.070511 0.193066 0.388585 0.173 Uiso 1 1 calc R . . . .
C51 C -0.0472(6) 0.1820(14) 0.4504(5) 0.135(5) Uani 1 1 d D U . . .
H51A H -0.077032 0.170249 0.457568 0.161 Uiso 1 1 calc R . . . .
H51B H -0.022907 0.226044 0.468016 0.161 Uiso 1 1 calc R . . . .
C52 C -0.0284(5) 0.0593(11) 0.4471(3) 0.105(4) Uani 1 1 d D U . . .
H52A H -0.023896 0.010226 0.467149 0.126 Uiso 1 1 calc R . . . .
H52B H -0.051592 0.012462 0.429431 0.126 Uiso 1 1 calc R . . . .
C53 C 0.0410(5) -0.0485(8) 0.4464(2) 0.093(3) Uani 1 1 d . U . . .
H53A H 0.049850 -0.068553 0.469585 0.111 Uiso 1 1 calc R . . . .
H53B H 0.019395 -0.117274 0.434777 0.111 Uiso 1 1 calc R . . . .
C54 C 0.0847(5) -0.0455(8) 0.4361(2) 0.090(3) Uani 1 1 d . U . . .
H54A H 0.101266 -0.129161 0.440169 0.108 Uiso 1 1 calc R . . . .
H54B H 0.076041 -0.028670 0.412713 0.108 Uiso 1 1 calc R . . . .
O17 O 0.5178(3) 0.0741(7) 0.67267(16) 0.096(2) Uani 1 1 d D U . . .
O18 O 0.4211(2) 0.0100(6) 0.63812(17) 0.0817(18) Uani 1 1 d D U . . .
O19 O 0.3431(3) 0.0562(8) 0.58241(17) 0.091(2) Uani 1 1 d D U . . .
O20 O 0.3383(2) 0.3038(7) 0.54866(14) 0.0773(18) Uani 1 1 d D U . . .
O21 O 0.4057(3) 0.4845(6) 0.54683(15) 0.091(2) Uani 1 1 d D U . . .
O22 O 0.5094(4) 0.4214(9) 0.5614(2) 0.131(3) Uani 1 1 d D U . . .
O23 O 0.5954(4) 0.2935(11) 0.5980(3) 0.202(6) Uani 1 1 d D U . . .
O24 O 0.5857(3) 0.1618(11) 0.6480(2) 0.164(5) Uani 1 1 d D U . . .
C93 C 0.4791(5) 0.0995(11) 0.6860(3) 0.106(3) Uani 1 1 d D U . . .
H93A H 0.466373 0.186723 0.680411 0.128 Uiso 1 1 calc R . . . .
H93B H 0.490319 0.091715 0.709677 0.128 Uiso 1 1 calc R . . . .
C94 C 0.4409(5) 0.0041(13) 0.6722(2) 0.105(3) Uani 1 1 d D U . . .
H94A H 0.454883 -0.081813 0.678014 0.125 Uiso 1 1 calc R . . . .
H94B H 0.413889 0.015131 0.682136 0.125 Uiso 1 1 calc R . . . .
C95 C 0.3848(4) -0.0819(10) 0.6253(3) 0.101(3) Uani 1 1 d D U . . .
H95A H 0.357870 -0.072729 0.635428 0.121 Uiso 1 1 calc R . . . .
H95B H 0.398930 -0.168147 0.630338 0.121 Uiso 1 1 calc R . . . .
C96 C 0.3650(4) -0.0672(11) 0.5897(3) 0.097(3) Uani 1 1 d D U . . .
H96A H 0.391713 -0.077125 0.579424 0.116 Uiso 1 1 calc R . . . .
H96B H 0.340208 -0.134001 0.581063 0.116 Uiso 1 1 calc R . . . .
C97 C 0.3204(4) 0.0770(12) 0.5495(2) 0.105(4) Uani 1 1 d D U . . .
H97A H 0.293139 0.015663 0.542275 0.126 Uiso 1 1 calc R . . . .
H97B H 0.344410 0.058513 0.537498 0.126 Uiso 1 1 calc R . . . .
C98 C 0.3008(3) 0.2079(11) 0.5410(3) 0.103(3) Uani 1 1 d D U . . .
H98A H 0.283950 0.211240 0.517766 0.124 Uiso 1 1 calc R . . . .
H98B H 0.276360 0.226724 0.552708 0.124 Uiso 1 1 calc R . . . .
C99 C 0.3226(4) 0.4222(11) 0.5368(2) 0.103(3) Uani 1 1 d D U . . .
H99A H 0.291356 0.442455 0.541392 0.124 Uiso 1 1 calc R . . . .
H99B H 0.316767 0.422400 0.513170 0.124 Uiso 1 1 calc R . . . .
C100 C 0.3594(4) 0.5198(9) 0.5513(2) 0.103(3) Uani 1 1 d D U . . .
H10A H 0.349039 0.603426 0.541141 0.124 Uiso 1 1 calc R . . . .
H10B H 0.362408 0.527306 0.574520 0.124 Uiso 1 1 calc R . . . .
C101 C 0.4459(5) 0.5688(9) 0.5618(3) 0.120(4) Uani 1 1 d D U . . .
H10C H 0.454540 0.557671 0.585387 0.143 Uiso 1 1 calc R . . . .
H10D H 0.435248 0.658102 0.556911 0.143 Uiso 1 1 calc R . . . .
C102 C 0.4904(6) 0.5442(11) 0.5505(5) 0.167(7) Uani 1 1 d D U . . .
H10E H 0.481516 0.547707 0.526818 0.200 Uiso 1 1 calc R . . . .
H10F H 0.515462 0.610061 0.559202 0.200 Uiso 1 1 calc R . . . .
C103 C 0.5554(7) 0.4281(17) 0.5541(6) 0.225(10) Uani 1 1 d D U . . .
H10G H 0.578887 0.488809 0.567655 0.270 Uiso 1 1 calc R . . . .
H10H H 0.552438 0.440896 0.531064 0.270 Uiso 1 1 calc R . . . .
C104 C 0.5633(6) 0.2937(14) 0.5648(4) 0.188(7) Uani 1 1 d D U . . .
H10I H 0.531684 0.252701 0.563989 0.226 Uiso 1 1 calc R . . . .
H10J H 0.578840 0.245745 0.550675 0.226 Uiso 1 1 calc R . . . .
C105 C 0.6130(5) 0.1688(15) 0.6043(4) 0.201(7) Uani 1 1 d D U . . .
H10K H 0.639824 0.153608 0.594368 0.242 Uiso 1 1 calc R . . . .
H10L H 0.586440 0.107133 0.595133 0.242 Uiso 1 1 calc R . . . .
C106 C 0.6306(4) 0.1532(15) 0.6386(3) 0.216(7) Uani 1 1 d D U . . .
H10M H 0.653792 0.221666 0.648627 0.259 Uiso 1 1 calc R . . . .
H10N H 0.646651 0.069556 0.644448 0.259 Uiso 1 1 calc R . . . .
C107 C 0.6010(5) 0.1031(15) 0.6794(3) 0.178(6) Uani 1 1 d D U . . .
H10O H 0.631941 0.140560 0.692669 0.214 Uiso 1 1 calc R . . . .
H10P H 0.605257 0.010079 0.677685 0.214 Uiso 1 1 calc R . . . .
C108 C 0.5597(5) 0.1323(12) 0.6929(3) 0.133(4) Uani 1 1 d D U . . .
H10Q H 0.566532 0.098178 0.715016 0.160 Uiso 1 1 calc R . . . .
H10R H 0.554939 0.225457 0.693649 0.160 Uiso 1 1 calc R . . . .
O25 O 0.2056(2) 0.0241(7) 0.32981(15) 0.0686(17) Uani 1 1 d . . . . .
C111 C 0.2430(3) -0.0430(12) 0.3520(3) 0.097(4) Uani 1 1 d . . . . .
H11A H 0.269275 0.016551 0.363088 0.116 Uiso 1 1 calc R . . . .
H11B H 0.257232 -0.107578 0.340704 0.116 Uiso 1 1 calc R . . . .
C112 C 0.2220(5) -0.1067(13) 0.3761(3) 0.110(4) Uani 1 1 d . . . . .
H11C H 0.195338 -0.163492 0.364945 0.164 Uiso 1 1 calc GR . . . .
H11D H 0.209336 -0.041948 0.387926 0.164 Uiso 1 1 calc GR . . . .
H11E H 0.247584 -0.156168 0.391124 0.164 Uiso 1 1 calc GR . . . .
C113 C 0.2242(5) 0.1115(18) 0.3092(4) 0.135(6) Uani 1 1 d D U . . .
H11H H 0.228364 0.067116 0.290071 0.162 Uiso 0.4 1 calc R . P A 2
H11I H 0.255710 0.150211 0.321220 0.162 Uiso 0.4 1 calc R . P A 2
H11F H 0.245128 0.065120 0.298276 0.162 Uiso 0.6 1 calc R . P B 1
H11G H 0.243561 0.180998 0.322206 0.162 Uiso 0.6 1 calc R . P B 1
C1A C 0.1789(9) 0.165(3) 0.2848(7) 0.146(9) Uani 0.6 1 d D U P C 1
H1AA H 0.160800 0.095163 0.271697 0.219 Uiso 0.6 1 calc GR . P C 1
H1AB H 0.189012 0.226325 0.270911 0.219 Uiso 0.6 1 calc GR . P C 1
H1AC H 0.157950 0.207214 0.296077 0.219 Uiso 0.6 1 calc GR . P C 1
C114 C 0.1838(14) 0.211(4) 0.3000(11) 0.146(11) Uani 0.4 1 d D U P C 2
H11J H 0.152713 0.169232 0.289239 0.219 Uiso 0.4 1 calc GR . P C 2
H11K H 0.191749 0.273414 0.285529 0.219 Uiso 0.4 1 calc GR . P C 2
H11L H 0.180807 0.254055 0.319415 0.219 Uiso 0.4 1 calc GR . P C 2
N9 N 0.1382(4) 0.7962(10) 0.5090(3) 0.107(3) Uani 1 1 d . . . . .
C109 C 0.1772(4) 0.7694(9) 0.5214(2) 0.063(2) Uani 1 1 d . . . . .
C110 C 0.2242(4) 0.7374(17) 0.5382(4) 0.128(6) Uani 1 1 d . . . . .
H11M H 0.234620 0.662775 0.528326 0.192 Uiso 1 1 calc GR . . . .
H11N H 0.225385 0.717724 0.560504 0.192 Uiso 1 1 calc GR . . . .
H11O H 0.246097 0.808984 0.537851 0.192 Uiso 1 1 calc GR . . . .
B2 B 0.3000(5) 0.7290(13) 0.4718(3) 0.088(3) Uani 1 1 d D U . . .
F5A F 0.3201(7) 0.7809(13) 0.4995(3) 0.108(4) Uani 0.6 1 d . U P D 1
F6A F 0.3133(6) 0.7763(18) 0.4472(3) 0.084(4) Uani 0.6 1 d . . P D 1
F7A F 0.2474(6) 0.7830(15) 0.4603(5) 0.140(5) Uani 0.6 1 d . U P D 1
F8A F 0.2946(8) 0.6024(16) 0.4687(6) 0.119(7) Uani 0.6 1 d . U P D 1
F5B F 0.3528(5) 0.7277(19) 0.4874(5) 0.121(7) Uani 0.4 1 d D U P D 2
F6B F 0.2939(10) 0.765(3) 0.4420(5) 0.135(12) Uani 0.4 1 d D U P D 2
F7B F 0.2829(12) 0.833(2) 0.4889(8) 0.188(12) Uani 0.4 1 d D U P D 2
F8B F 0.2813(9) 0.620(2) 0.4786(9) 0.127(12) Uani 0.4 1 d D U P D 2


_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
Br1 C3 1.899(8) . ?
Br2 C6 1.889(7) . ?
O1 C27 1.215(16) . ?
O2 C27 1.240(14) . ?
O2 C28 1.522(15) . ?
O3 C36 1.183(9) . ?
O4 C36 1.335(9) . ?
O4 C37 1.534(13) . ?
N1 C1 1.360(8) . ?
N1 C2 1.386(8) . ?
N2 C1 1.318(8) . ?
N2 C7 1.382(8) . ?
N3 C14 1.326(7) . ?
N3 C20 1.378(7) . ?
N4 C14 1.321(7) . ?
N4 C15 1.388(7) . ?
C1 C8 1.461(8) . ?
C2 C3 1.390(9) . ?
C2 C7 1.394(10) . ?
C3 C4 1.361(11) . ?
C4 C5 1.395(11) . ?
C5 C6 1.371(9) . ?
C6 C7 1.385(9) . ?
C8 C9 1.385(8) . ?
C8 C13 1.397(8) . ?
C9 C10 1.385(8) . ?
C10 C11 1.391(8) . ?
C11 C12 1.395(8) . ?
C11 C14 1.465(7) . ?
C12 C13 1.386(8) . ?
C15 C16 1.408(8) . ?
C15 C20 1.390(8) . ?
C16 C17 1.397(8) . ?
C16 C21 1.482(8) . ?
C17 C18 1.401(9) . ?
C18 C19 1.387(8) . ?
C19 C20 1.406(8) . ?
C19 C30 1.472(8) . ?
C21 C22 1.386(9) . ?
C21 C26 1.391(9) . ?
C22 C23 1.395(9) . ?
C23 C24 1.362(11) . ?
C24 C25 1.379(12) . ?
C24 C27 1.514(11) . ?
C25 C26 1.392(10) . ?
C28 C29 1.74(3) . ?
C30 C31 1.407(8) . ?
C30 C35 1.388(9) . ?
C31 C32 1.372(9) . ?
C32 C33 1.386(9) . ?
C33 C34 1.391(9) . ?
C33 C36 1.500(9) . ?
C34 C35 1.375(9) . ?
C37 C38 1.426(15) . ?
Br3 C57 1.884(7) . ?
Br4 C60 1.895(8) . ?
O13 C81 1.201(9) . ?
O14 C81 1.344(10) . ?
O14 C82 1.475(12) . ?
O15 C90 1.211(11) . ?
O16 C90 1.302(11) . ?
O16 C91 1.468(10) . ?
N5 C55 1.355(8) . ?
N5 C61 1.385(8) . ?
N6 C55 1.316(8) . ?
N6 C56 1.373(8) . ?
N7 C68 1.321(7) . ?
N7 C69 1.381(7) . ?
N8 C68 1.332(7) . ?
N8 C74 1.394(7) . ?
C55 C62 1.470(8) . ?
C56 C57 1.390(9) . ?
C56 C61 1.407(10) . ?
C57 C58 1.383(10) . ?
C58 C59 1.379(12) . ?
C59 C60 1.387(11) . ?
C60 C61 1.373(10) . ?
C62 C63 1.395(9) . ?
C62 C67 1.384(9) . ?
C63 C64 1.390(8) . ?
C64 C65 1.379(9) . ?
C65 C66 1.392(9) . ?
C65 C68 1.470(8) . ?
C66 C67 1.402(8) . ?
C69 C70 1.399(8) . ?
C69 C74 1.388(8) . ?
C70 C71 1.393(9) . ?
C70 C75 1.472(9) . ?
C71 C72 1.405(9) . ?
C72 C73 1.385(8) . ?
C73 C74 1.409(8) . ?
C73 C84 1.481(8) . ?
C75 C76 1.397(9) . ?
C75 C80 1.391(9) . ?
C76 C77 1.382(9) . ?
C77 C78 1.389(10) . ?
C78 C79 1.400(10) . ?
C78 C81 1.468(10) . ?
C79 C80 1.374(10) . ?
C82 C83 1.39(2) . ?
C84 C85 1.383(9) . ?
C84 C89 1.399(9) . ?
C85 C86 1.402(10) . ?
C86 C87 1.389(10) . ?
C87 C88 1.360(11) . ?
C87 C90 1.520(11) . ?
C88 C89 1.373(10) . ?
C91 C92 1.468(17) . ?
F1 B1 1.315(16) . ?
F2 B1 1.385(14) . ?
F3 B1 1.303(14) . ?
F4 B1 1.42(2) . ?
O5 C39 1.447(13) . ?
O5 C54 1.352(13) . ?
O6 C40 1.403(13) . ?
O6 C41 1.490(13) . ?
O7 C42 1.396(11) . ?
O7 C43 1.451(11) . ?
O8 C44 1.320(12) . ?
O8 C45 1.418(11) . ?
O9 C46 1.377(12) . ?
O9 C47 1.361(12) . ?
O10 C48 1.296(16) . ?
O10 C49 1.454(15) . ?
O11 C50 1.151(16) . ?
O11 C51 1.263(17) . ?
O12 C52 1.327(13) . ?
O12 C53 1.474(14) . ?
C39 C40 1.442(18) . ?
C41 C42 1.519(16) . ?
C43 C44 1.429(15) . ?
C45 C46 1.520(16) . ?
C47 C48 1.605(18) . ?
C49 C50 1.54(2) . ?
C51 C52 1.419(14) . ?
C53 C54 1.436(17) . ?
O17 C93 1.407(9) . ?
O17 C108 1.409(12) . ?
O18 C94 1.428(8) . ?
O18 C95 1.410(8) . ?
O19 C96 1.435(14) . ?
O19 C97 1.408(8) . ?
O20 C98 1.437(8) . ?
O20 C99 1.372(12) . ?
O21 C100 1.435(8) . ?
O21 C101 1.448(9) . ?
O22 C102 1.427(9) . ?
O22 C103 1.434(9) . ?
O23 C104 1.474(9) . ?
O23 C105 1.401(15) . ?
O24 C106 1.4477(14) . ?
O24 C107 1.4476(12) . ?
C93 C94 1.477(18) . ?
C95 C96 1.500(8) . ?
C97 C98 1.490(9) . ?
C99 C100 1.476(7) . ?
C101 C102 1.504(9) . ?
C103 C104 1.484(10) . ?
C105 C106 1.444(9) . ?
C107 C108 1.486(9) . ?
O25 C111 1.408(13) . ?
O25 C113 1.479(15) . ?
C111 C112 1.499(17) . ?
C113 C1A 1.527(18) . ?
C113 C114 1.52(2) . ?
N9 C109 1.126(13) . ?
C109 C110 1.374(16) . ?
B2 F5A 1.298(17) . ?
B2 F6A 1.327(19) . ?
B2 F7A 1.55(2) . ?
B2 F8A 1.34(2) . ?
B2 F5B 1.467(15) . ?
B2 F6B 1.31(2) . ?
B2 F7B 1.48(2) . ?
B2 F8B 1.33(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
C27 O2 C28 105.5(11) . . ?
C36 O4 C37 114.5(7) . . ?
C1 N1 C2 105.7(5) . . ?
C1 N2 C7 104.9(5) . . ?
C14 N3 C20 108.6(4) . . ?
C14 N4 C15 108.5(5) . . ?
N1 C1 C8 124.2(5) . . ?
N2 C1 N1 113.7(5) . . ?
N2 C1 C8 122.1(5) . . ?
N1 C2 C3 134.1(7) . . ?
N1 C2 C7 106.1(5) . . ?
C3 C2 C7 119.8(6) . . ?
C2 C3 Br1 119.1(6) . . ?
C4 C3 Br1 121.7(6) . . ?
C4 C3 C2 119.1(7) . . ?
C3 C4 C5 121.6(7) . . ?
C6 C5 C4 119.7(6) . . ?
C5 C6 Br2 121.2(5) . . ?
C5 C6 C7 119.5(6) . . ?
C7 C6 Br2 119.3(5) . . ?
N2 C7 C2 109.5(5) . . ?
N2 C7 C6 129.9(6) . . ?
C6 C7 C2 120.5(6) . . ?
C9 C8 C1 118.0(5) . . ?
C9 C8 C13 119.1(5) . . ?
C13 C8 C1 122.9(5) . . ?
C8 C9 C10 121.2(5) . . ?
C9 C10 C11 118.9(5) . . ?
C10 C11 C12 121.1(5) . . ?
C10 C11 C14 118.6(5) . . ?
C12 C11 C14 120.3(5) . . ?
C13 C12 C11 118.8(5) . . ?
C12 C13 C8 120.9(5) . . ?
N3 C14 C11 124.8(5) . . ?
N4 C14 N3 110.2(5) . . ?
N4 C14 C11 125.0(5) . . ?
N4 C15 C16 130.7(5) . . ?
N4 C15 C20 106.2(5) . . ?
C20 C15 C16 123.1(5) . . ?
C15 C16 C21 122.1(5) . . ?
C17 C16 C15 114.0(5) . . ?
C17 C16 C21 123.8(5) . . ?
C16 C17 C18 122.8(5) . . ?
C19 C18 C17 122.8(5) . . ?
C18 C19 C20 114.8(5) . . ?
C18 C19 C30 123.6(5) . . ?
C20 C19 C30 121.6(5) . . ?
N3 C20 C15 106.5(5) . . ?
N3 C20 C19 131.1(5) . . ?
C15 C20 C19 122.3(5) . . ?
C22 C21 C16 120.1(5) . . ?
C22 C21 C26 118.7(6) . . ?
C26 C21 C16 121.2(6) . . ?
C21 C22 C23 120.4(6) . . ?
C24 C23 C22 120.6(7) . . ?
C23 C24 C25 119.7(7) . . ?
C23 C24 C27 118.9(9) . . ?
C25 C24 C27 121.4(9) . . ?
C24 C25 C26 120.4(7) . . ?
C21 C26 C25 120.1(7) . . ?
O1 C27 O2 124.8(10) . . ?
O1 C27 C24 118.5(11) . . ?
O2 C27 C24 116.7(11) . . ?
O2 C28 C29 97.4(13) . . ?
C31 C30 C19 120.8(5) . . ?
C35 C30 C19 121.5(5) . . ?
C35 C30 C31 117.7(5) . . ?
C32 C31 C30 121.4(6) . . ?
C31 C32 C33 119.9(6) . . ?
C32 C33 C34 119.5(6) . . ?
C32 C33 C36 117.9(6) . . ?
C34 C33 C36 122.6(6) . . ?
C35 C34 C33 120.4(6) . . ?
C34 C35 C30 121.1(6) . . ?
O3 C36 O4 124.3(7) . . ?
O3 C36 C33 123.6(7) . . ?
O4 C36 C33 112.1(6) . . ?
C38 C37 O4 96.0(13) . . ?
C81 O14 C82 116.3(7) . . ?
C90 O16 C91 113.4(8) . . ?
C55 N5 C61 106.6(6) . . ?
C55 N6 C56 105.2(5) . . ?
C68 N7 C69 109.1(5) . . ?
C68 N8 C74 108.3(5) . . ?
N5 C55 C62 123.7(6) . . ?
N6 C55 N5 113.3(5) . . ?
N6 C55 C62 123.0(6) . . ?
N6 C56 C57 130.9(6) . . ?
N6 C56 C61 109.9(6) . . ?
C57 C56 C61 119.1(6) . . ?
C56 C57 Br3 119.2(5) . . ?
C58 C57 Br3 121.3(5) . . ?
C58 C57 C56 119.5(6) . . ?
C59 C58 C57 120.8(7) . . ?
C58 C59 C60 120.3(7) . . ?
C59 C60 Br4 121.0(6) . . ?
C61 C60 Br4 119.7(6) . . ?
C61 C60 C59 119.2(7) . . ?
N5 C61 C56 105.0(6) . . ?
C60 C61 N5 134.0(7) . . ?
C60 C61 C56 121.0(6) . . ?
C63 C62 C55 122.1(6) . . ?
C67 C62 C55 118.0(6) . . ?
C67 C62 C63 119.8(5) . . ?
C64 C63 C62 120.5(6) . . ?
C65 C64 C63 119.1(6) . . ?
C64 C65 C66 121.6(5) . . ?
C64 C65 C68 119.8(5) . . ?
C66 C65 C68 118.6(5) . . ?
C65 C66 C67 118.6(6) . . ?
C62 C67 C66 120.3(6) . . ?
N7 C68 N8 109.8(5) . . ?
N7 C68 C65 125.3(5) . . ?
N8 C68 C65 124.9(5) . . ?
N7 C69 C70 130.8(6) . . ?
N7 C69 C74 106.6(5) . . ?
C74 C69 C70 122.6(5) . . ?
C69 C70 C75 122.7(5) . . ?
C71 C70 C69 114.7(6) . . ?
C71 C70 C75 122.5(5) . . ?
C70 C71 C72 122.4(6) . . ?
C73 C72 C71 123.2(6) . . ?
C72 C73 C74 114.1(5) . . ?
C72 C73 C84 121.8(5) . . ?
C74 C73 C84 124.0(5) . . ?
N8 C74 C73 130.8(5) . . ?
C69 C74 N8 106.1(5) . . ?
C69 C74 C73 123.0(5) . . ?
C76 C75 C70 119.7(5) . . ?
C80 C75 C70 122.1(6) . . ?
C80 C75 C76 118.2(6) . . ?
C77 C76 C75 121.5(6) . . ?
C76 C77 C78 119.5(6) . . ?
C77 C78 C79 119.4(7) . . ?
C77 C78 C81 117.7(6) . . ?
C79 C78 C81 122.8(7) . . ?
C80 C79 C78 120.3(7) . . ?
C79 C80 C75 121.0(6) . . ?
O13 C81 O14 122.7(7) . . ?
O13 C81 C78 123.7(7) . . ?
O14 C81 C78 113.5(7) . . ?
C83 C82 O14 108.4(14) . . ?
C85 C84 C73 122.3(6) . . ?
C85 C84 C89 119.1(6) . . ?
C89 C84 C73 118.5(6) . . ?
C84 C85 C86 119.8(6) . . ?
C87 C86 C85 119.3(6) . . ?
C86 C87 C90 121.6(7) . . ?
C88 C87 C86 121.0(7) . . ?
C88 C87 C90 117.5(7) . . ?
C87 C88 C89 120.0(7) . . ?
C88 C89 C84 120.8(7) . . ?
O15 C90 O16 125.4(8) . . ?
O15 C90 C87 123.6(8) . . ?
O16 C90 C87 111.0(8) . . ?
O16 C91 C92 105.2(9) . . ?
F1 B1 F2 107.5(11) . . ?
F1 B1 F4 107.5(14) . . ?
F2 B1 F4 105.6(12) . . ?
F3 B1 F1 117.7(14) . . ?
F3 B1 F2 115.2(12) . . ?
F3 B1 F4 102.3(12) . . ?
C54 O5 C39 113.5(8) . . ?
C40 O6 C41 116.8(8) . . ?
C42 O7 C43 112.2(8) . . ?
C44 O8 C45 116.7(9) . . ?
C47 O9 C46 111.0(8) . . ?
C48 O10 C49 114.1(10) . . ?
C50 O11 C51 130.1(16) . . ?
C52 O12 C53 109.4(8) . . ?
C40 C39 O5 111.1(7) . . ?
O6 C40 C39 108.8(8) . . ?
O6 C41 C42 108.9(7) . . ?
O7 C42 C41 109.0(8) . . ?
C44 C43 O7 106.5(8) . . ?
O8 C44 C43 121.3(12) . . ?
O8 C45 C46 113.6(8) . . ?
O9 C46 C45 109.7(8) . . ?
O9 C47 C48 109.6(8) . . ?
O10 C48 C47 110.0(9) . . ?
O10 C49 C50 93.8(10) . . ?
O11 C50 C49 122.6(13) . . ?
O11 C51 C52 119.3(15) . . ?
O12 C52 C51 108.5(10) . . ?
C54 C53 O12 112.4(7) . . ?
O5 C54 C53 110.3(8) . . ?
C93 O17 C108 106.6(10) . . ?
C95 O18 C94 114.2(9) . . ?
C97 O19 C96 114.2(9) . . ?
C99 O20 C98 114.0(8) . . ?
C100 O21 C101 114.9(8) . . ?
C102 O22 C103 99.6(10) . . ?
C105 O23 C104 106.2(8) . . ?
C106 O24 C107 100.5(8) . . ?
O17 C93 C94 106.1(9) . . ?
O18 C94 C93 115.0(10) . . ?
O18 C95 C96 111.0(8) . . ?
O19 C96 C95 109.5(9) . . ?
O19 C97 C98 115.3(10) . . ?
O20 C98 C97 112.8(8) . . ?
O20 C99 C100 110.6(8) . . ?
O21 C100 C99 109.3(8) . . ?
O21 C101 C102 112.3(10) . . ?
O22 C102 C101 108.9(11) . . ?
O22 C103 C104 87.3(11) . . ?
O23 C104 C103 107.8(14) . . ?
O23 C105 C106 107.9(10) . . ?
C105 C106 O24 101.8(11) . . ?
O24 C107 C108 103.0(10) . . ?
O17 C108 C107 106.8(10) . . ?
C111 O25 C113 113.2(9) . . ?
O25 C111 C112 109.1(8) . . ?
O25 C113 C1A 105.8(15) . . ?
O25 C113 C114 102(2) . . ?
N9 C109 C110 176.8(13) . . ?
F5A B2 F6A 115.8(12) . . ?
F5A B2 F7A 106.3(15) . . ?
F5A B2 F8A 121.1(17) . . ?
F6A B2 F7A 94.3(13) . . ?
F6A B2 F8A 110.0(17) . . ?
F8A B2 F7A 105.0(14) . . ?
F5B B2 F7B 102.3(15) . . ?
F6B B2 F5B 107.1(15) . . ?
F6B B2 F7B 108.0(17) . . ?
F6B B2 F8B 121.3(19) . . ?
F8B B2 F5B 108.2(15) . . ?
F8B B2 F7B 108.4(16) . . ?

_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 0.257 0.106 0.220 222.0 45.7 ?
2 0.257 0.394 0.720 222.0 45.8 ?
3 0.174 -0.001 0.811 12.7 0.0 ?
4 0.174 0.501 0.311 12.7 0.0 ?
5 0.743 0.606 0.280 222.0 45.8 ?
6 0.743 0.894 0.780 222.0 45.9 ?
7 0.826 0.001 0.189 12.7 0.4 ?
8 0.826 0.499 0.689 12.7 0.4 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
