# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Graeme Cooke'
'Stuart T Caldwell'
'Brian Fitzpatrick'
'De-Liang Long.'
'Gouher Rabani'
'Vincent M Rotello'

_publ_contact_author_name        'Graeme Cooke'
_publ_contact_author_email       GRAEMEC@CHEM.GLA.AC.UK

_publ_section_title              
;
A flavin-based [2]catenane
;

# Attachment 'gccatenane.cif'

data_gccatenane
_database_code_depnum_ccdc_archive 'CCDC 697887'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C48 H63 F3 N6 O6), (C32 H28 N4 O4), 2(C2 H6 O), 2(H2 O)'
_chemical_formula_sum            'C84 H107 F3 N10 O14'
_chemical_formula_weight         1537.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.9514(5)
_cell_length_b                   29.1721(10)
_cell_length_c                   20.3132(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.463(3)
_cell_angle_gamma                90.00
_cell_volume                     8072.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8601
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      24.4

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3280
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD Diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            33859
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.1052
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         24.41
_reflns_number_total             10751
_reflns_number_gt                5051
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
A disordered model was applied to the long chain part involving C30. One
ethanol molecule was also refined with the O position disordered over two
positions. All other parts of the structure are well defined. Due to weak
diffraction of the crystal with limited observable reflection, no hydorgen
atoms were added or tried find on some solvent molecules.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       none
_refine_ls_number_reflns         10751
_refine_ls_number_parameters     949
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1683
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5720(2) 0.61200(9) 0.48701(13) 0.0509(8) Uani 1 1 d . A 1
O2 O 0.7442(2) 0.56620(11) 0.33278(15) 0.0603(9) Uani 1 1 d . A 1
O3 O 0.3854(2) 0.38079(10) 0.25730(17) 0.0617(9) Uani 1 1 d . A 1
O4 O 0.3221(2) 0.23833(10) 0.38306(15) 0.0603(8) Uani 1 1 d . A 1
O5 O 0.6805(3) 0.35731(15) 0.7442(2) 0.1072(14) Uani 1 1 d . A 1
O6 O 0.7729(3) 0.41703(16) 0.7314(2) 0.0935(12) Uani 1 1 d . A 1
O7 O 0.7450(3) 0.36465(14) 0.26849(19) 0.0942(13) Uani 1 1 d . B 1
O8 O 0.3888(2) 0.29531(11) 0.62772(16) 0.0672(9) Uani 1 1 d . B 1
O9 O -0.0394(2) 0.31963(12) 0.37372(17) 0.0731(10) Uani 1 1 d . B 1
O10 O 0.3102(3) 0.34210(14) 0.0166(2) 0.1071(14) Uani 1 1 d . B 1
O11 O 0.5483(2) 0.28177(10) 0.72352(14) 0.0639(9) Uani 1 1 d . C 1
O12 O 0.1730(2) 0.17800(11) 0.40709(16) 0.0796(10) Uani 1 1 d . D 1
F1 F 1.3339(2) 0.57692(10) 0.52497(16) 0.0897(10) Uani 1 1 d . A 1
F2 F 1.30205(19) 0.50640(10) 0.52123(15) 0.0797(8) Uani 1 1 d . A 1
F3 F 1.26220(18) 0.54668(11) 0.43324(15) 0.0920(10) Uani 1 1 d . A 1
N1 N 0.9129(3) 0.56403(11) 0.43158(16) 0.0462(9) Uani 1 1 d . A 1
N2 N 0.8995(2) 0.58625(11) 0.56350(17) 0.0452(9) Uani 1 1 d . A 1
N3 N 0.7331(3) 0.59915(11) 0.52607(17) 0.0432(9) Uani 1 1 d . A 1
N4 N 0.6560(2) 0.58859(11) 0.40884(16) 0.0408(9) Uani 1 1 d . A 1
N5 N 0.4219(2) 0.40212(13) 0.36693(18) 0.0513(10) Uani 1 1 d . A 1
H5 H 0.4236 0.3926 0.4072 0.062 Uiso 1 1 calc R A 1
N6 N 0.3765(3) 0.20629(14) 0.2969(2) 0.0780(13) Uani 1 1 d . A 1
H6 H 0.4000 0.2117 0.2619 0.094 Uiso 1 1 calc R A 1
N7 N 0.6655(3) 0.29796(15) 0.26847(18) 0.0566(10) Uani 1 1 d . B 1
H7 H 0.6174 0.2813 0.2481 0.068 Uiso 1 1 calc R B 1
N8 N 0.3987(2) 0.27412(12) 0.52310(17) 0.0513(10) Uani 1 1 d . B 1
H8 H 0.3689 0.2681 0.4824 0.062 Uiso 1 1 calc R B 1
N9 N 0.0431(3) 0.25391(15) 0.3622(2) 0.0703(12) Uani 1 1 d . B 1
H9 H 0.0839 0.2335 0.3818 0.084 Uiso 1 1 calc R B 1
N10 N 0.2988(3) 0.34592(14) 0.1250(2) 0.0743(12) Uani 1 1 d . B 1
H10 H 0.3290 0.3466 0.1667 0.089 Uiso 1 1 calc R B 1
C1 C 1.2653(3) 0.54687(18) 0.4990(3) 0.0524(12) Uani 1 1 d . A 1
C2 C 1.1693(3) 0.55631(14) 0.5156(2) 0.0475(11) Uani 1 1 d . A 1
C3 C 1.0859(3) 0.55554(14) 0.4666(2) 0.0477(11) Uani 1 1 d . A 1
H3 H 1.0893 0.5488 0.4224 0.057 Uiso 1 1 calc R A 1
C4 C 0.9947(3) 0.56480(14) 0.4820(2) 0.0445(11) Uani 1 1 d . A 1
C5 C 0.9907(3) 0.57510(14) 0.5499(2) 0.0452(11) Uani 1 1 d . A 1
C6 C 1.0759(3) 0.57445(15) 0.6001(2) 0.0556(12) Uani 1 1 d . A 1
H6A H 1.0736 0.5801 0.6447 0.067 Uiso 1 1 calc R A 1
C7 C 1.1640(3) 0.56522(15) 0.5823(2) 0.0573(13) Uani 1 1 d . A 1
H7A H 1.2214 0.5649 0.6156 0.069 Uiso 1 1 calc R A 1
C8 C 0.8178(3) 0.58795(13) 0.5126(2) 0.0397(11) Uani 1 1 d . A 1
C9 C 0.8294(3) 0.57562(14) 0.4453(2) 0.0419(11) Uani 1 1 d . A 1
C10 C 0.7417(3) 0.57599(14) 0.3905(2) 0.0443(11) Uani 1 1 d . A 1
C11 C 0.6521(3) 0.60083(13) 0.4754(2) 0.0412(11) Uani 1 1 d . A 1
C12 C 0.5640(3) 0.58487(14) 0.3575(2) 0.0485(12) Uani 1 1 d . A 1
H12A H 0.5763 0.5924 0.3135 0.058 Uiso 1 1 calc R A 1
H12B H 0.5163 0.6065 0.3675 0.058 Uiso 1 1 calc R A 1
C13 C 0.5234(3) 0.53715(15) 0.3562(2) 0.0413(11) Uani 1 1 d . A 1
C14 C 0.4716(3) 0.52396(15) 0.4042(2) 0.0451(11) Uani 1 1 d . A 1
H14 H 0.4586 0.5453 0.4352 0.054 Uiso 1 1 calc R A 1
C15 C 0.4393(3) 0.47908(16) 0.4062(2) 0.0481(12) Uani 1 1 d . A 1
H15 H 0.4052 0.4706 0.4389 0.058 Uiso 1 1 calc R A 1
C16 C 0.4569(3) 0.44714(16) 0.3609(2) 0.0440(11) Uani 1 1 d . A 1
C17 C 0.5092(3) 0.45952(17) 0.3131(2) 0.0523(12) Uani 1 1 d . A 1
H17 H 0.5222 0.4380 0.2824 0.063 Uiso 1 1 calc R A 1
C18 C 0.5419(3) 0.50429(17) 0.3115(2) 0.0513(12) Uani 1 1 d . A 1
H18 H 0.5773 0.5124 0.2795 0.062 Uiso 1 1 calc R A 1
C19 C 0.3862(3) 0.37243(16) 0.3168(3) 0.0525(13) Uani 1 1 d . A 1
C20 C 0.3468(3) 0.32771(15) 0.3383(2) 0.0578(13) Uani 1 1 d . A 1
H20A H 0.3565 0.3270 0.3871 0.069 Uiso 1 1 calc R A 1
H20B H 0.2769 0.3257 0.3194 0.069 Uiso 1 1 calc R A 1
C21 C 0.3985(3) 0.28721(15) 0.3148(2) 0.0527(12) Uani 1 1 d . A 1
H21A H 0.3890 0.2884 0.2661 0.063 Uiso 1 1 calc R A 1
H21B H 0.4683 0.2897 0.3336 0.063 Uiso 1 1 calc R A 1
C22 C 0.3625(3) 0.24165(17) 0.3345(2) 0.0542(12) Uani 1 1 d . A 1
C23 C 0.3549(4) 0.15855(19) 0.3106(3) 0.0908(18) Uani 1 1 d . A 1
H23A H 0.3193 0.1444 0.2693 0.109 Uiso 1 1 calc R A 1
H23B H 0.3129 0.1579 0.3430 0.109 Uiso 1 1 calc R A 1
C24 C 0.4457(4) 0.13147(18) 0.3376(3) 0.0793(16) Uani 1 1 d . A 1
H24A H 0.4809 0.1455 0.3791 0.095 Uiso 1 1 calc R A 1
H24B H 0.4879 0.1325 0.3054 0.095 Uiso 1 1 calc R A 1
C25 C 0.4242(5) 0.08166(18) 0.3514(2) 0.0885(18) Uani 1 1 d . A 1
H25A H 0.3835 0.0805 0.3846 0.106 Uiso 1 1 calc R A 1
H25B H 0.3878 0.0677 0.3103 0.106 Uiso 1 1 calc R A 1
C26 C 0.5171(5) 0.0549(2) 0.3771(3) 0.109(2) Uiso 1 1 d D A 1
H26A H 0.5573 0.0549 0.3436 0.131 Uiso 1 1 calc R A 1
H26B H 0.5545 0.0688 0.4180 0.131 Uiso 1 1 calc R A 1
C27 C 0.4903(9) 0.0070(4) 0.3910(8) 0.090(5) Uiso 0.517(13) 1 d PD A 1
H27A H 0.4470 -0.0062 0.3517 0.108 Uiso 1 1 calc R A 1
H27B H 0.4577 0.0061 0.4286 0.108 Uiso 1 1 calc R A 1
C28 C 0.5862(9) -0.0187(5) 0.4077(9) 0.121(6) Uiso 0.517(13) 1 d PD A 1
H28A H 0.5723 -0.0480 0.4262 0.145 Uiso 0.517(13) 1 calc PR A 1
H28B H 0.6042 -0.0253 0.3651 0.145 Uiso 0.517(13) 1 calc PR A 1
C29 C 0.6759(12) -0.0005(6) 0.4535(8) 0.144(7) Uiso 0.517(13) 1 d PD A 1
H29A H 0.6532 0.0250 0.4769 0.173 Uiso 0.517(13) 1 calc PR A 1
H29B H 0.7143 0.0130 0.4240 0.173 Uiso 0.517(13) 1 calc PR A 1
C30 C 0.7489(17) -0.025(2) 0.507(3) 0.22(3) Uiso 0.20 1 d PD A 1
H30A H 0.7425 -0.0582 0.4989 0.269 Uiso 0.155(4) 1 calc PR A 1
H30B H 0.7356 -0.0190 0.5508 0.269 Uiso 0.155(4) 1 calc PR A 1
C31 C 0.8524(13) -0.0106(5) 0.5054(8) 0.117(7) Uiso 0.517(13) 1 d PD A 1
H31A H 0.8876 -0.0094 0.5521 0.140 Uiso 0.517(13) 1 calc PR A 1
H31B H 0.8811 -0.0356 0.4848 0.140 Uiso 0.517(13) 1 calc PR A 1
C32 C 0.8784(8) 0.0319(4) 0.4735(5) 0.152(4) Uiso 0.80 1 d PD A 1
H32 H 0.9286 0.0280 0.4505 0.182 Uiso 0.80 1 calc PR A 1
C33 C 0.8449(8) 0.0741(4) 0.4711(5) 0.129(3) Uiso 0.70 1 d PD A 1
H33 H 0.8013 0.0797 0.4989 0.154 Uiso 0.70 1 calc PR A 1
C34 C 0.8656(8) 0.1149(3) 0.4307(5) 0.118(3) Uiso 0.70 1 d PD A 1
H34A H 0.9095 0.1054 0.4021 0.141 Uiso 1 1 calc R A 1
H34B H 0.8046 0.1248 0.4016 0.141 Uiso 1 1 calc R A 1
C35 C 0.9085(6) 0.1527(3) 0.4708(4) 0.147(3) Uiso 1 1 d D A 1
H35A H 0.9187 0.1773 0.4411 0.176 Uiso 1 1 calc R A 1
H35B H 0.9723 0.1435 0.4967 0.176 Uiso 1 1 calc R A 1
C36 C 0.8496(5) 0.1704(3) 0.5177(3) 0.120(2) Uiso 1 1 d . A 1
H36A H 0.7807 0.1693 0.4955 0.144 Uiso 1 1 calc R A 1
H36B H 0.8589 0.1504 0.5567 0.144 Uiso 1 1 calc R A 1
C37 C 0.8742(4) 0.2170(2) 0.5406(3) 0.097(2) Uani 1 1 d . A 1
H37A H 0.8642 0.2370 0.5015 0.117 Uiso 1 1 calc R A 1
H37B H 0.9433 0.2181 0.5621 0.117 Uiso 1 1 calc R A 1
C38 C 0.8163(4) 0.2355(3) 0.5889(3) 0.097(2) Uani 1 1 d . A 1
H38A H 0.7471 0.2327 0.5683 0.117 Uiso 1 1 calc R A 1
H38B H 0.8292 0.2164 0.6290 0.117 Uiso 1 1 calc R A 1
C39 C 0.8359(4) 0.2834(2) 0.6101(3) 0.0946(18) Uani 1 1 d . A 1
H39A H 0.8248 0.3025 0.5700 0.114 Uiso 1 1 calc R A 1
H39B H 0.9047 0.2861 0.6319 0.114 Uiso 1 1 calc R A 1
C40 C 0.7764(4) 0.3017(2) 0.6564(3) 0.0900(18) Uani 1 1 d . A 1
H40A H 0.7073 0.2999 0.6348 0.108 Uiso 1 1 calc R A 1
H40B H 0.7870 0.2830 0.6968 0.108 Uiso 1 1 calc R A 1
C41 C 0.8019(6) 0.3497(3) 0.6754(4) 0.124(2) Uiso 1 1 d . A 1
H41A H 0.7945 0.3673 0.6341 0.149 Uiso 1 1 calc R A 1
H41B H 0.8710 0.3505 0.6972 0.149 Uiso 1 1 calc R A 1
C42 C 0.7454(5) 0.3745(3) 0.7211(3) 0.0893(18) Uani 1 1 d . A 1
C43 C 0.7213(4) 0.4466(2) 0.7697(3) 0.0846(17) Uani 1 1 d . A 1
H43A H 0.7458 0.4420 0.8177 0.102 Uiso 1 1 calc R A 1
H43B H 0.6515 0.4400 0.7588 0.102 Uiso 1 1 calc R A 1
C44 C 0.7399(3) 0.49449(19) 0.7504(2) 0.0733(15) Uani 1 1 d . A 1
H44A H 0.7195 0.4974 0.7018 0.088 Uiso 1 1 calc R A 1
H44B H 0.6997 0.5151 0.7705 0.088 Uiso 1 1 calc R A 1
C45 C 0.8442(4) 0.50915(18) 0.7714(2) 0.0709(15) Uani 1 1 d . A 1
H45A H 0.8859 0.4855 0.7589 0.085 Uiso 1 1 calc R A 1
H45B H 0.8611 0.5123 0.8201 0.085 Uiso 1 1 calc R A 1
C46 C 0.8647(3) 0.55473(17) 0.7392(2) 0.0612(13) Uani 1 1 d . A 1
H46A H 0.8129 0.5763 0.7421 0.073 Uiso 1 1 calc R A 1
H46B H 0.9261 0.5673 0.7644 0.073 Uiso 1 1 calc R A 1
C47 C 0.8708(3) 0.54927(16) 0.6659(2) 0.0560(12) Uani 1 1 d . A 1
H47A H 0.9235 0.5281 0.6632 0.067 Uiso 1 1 calc R A 1
H47B H 0.8100 0.5360 0.6410 0.067 Uiso 1 1 calc R A 1
C48 C 0.8887(3) 0.59383(15) 0.63332(19) 0.0488(12) Uani 1 1 d . A 1
H48A H 0.8341 0.6145 0.6332 0.059 Uiso 1 1 calc R A 1
H48B H 0.9478 0.6081 0.6592 0.059 Uiso 1 1 calc R A 1
C49 C 0.6164(4) 0.34821(16) 0.1738(2) 0.0600(13) Uani 1 1 d . B 1
C50 C 0.6590(4) 0.36793(17) 0.1244(3) 0.0705(15) Uani 1 1 d . B 1
H50 H 0.7262 0.3734 0.1339 0.085 Uiso 1 1 calc R B 1
C51 C 0.6049(5) 0.37929(19) 0.0634(3) 0.0818(16) Uani 1 1 d . B 1
H51 H 0.6346 0.3930 0.0316 0.098 Uiso 1 1 calc R B 1
C52 C 0.5056(5) 0.37051(18) 0.0480(3) 0.0750(16) Uani 1 1 d . B 1
H52 H 0.4690 0.3768 0.0051 0.090 Uiso 1 1 calc R B 1
C53 C 0.4593(4) 0.35206(17) 0.0969(3) 0.0624(13) Uani 1 1 d . B 1
C54 C 0.5160(4) 0.34099(15) 0.1588(3) 0.0603(13) Uani 1 1 d . B 1
H54 H 0.4863 0.3284 0.1915 0.072 Uiso 1 1 calc R B 1
C55 C 0.3502(4) 0.34617(18) 0.0774(3) 0.0749(16) Uani 1 1 d . B 1
C56 C 0.6812(4) 0.3375(2) 0.2408(3) 0.0608(13) Uani 1 1 d . B 1
C57 C 0.7251(3) 0.28111(16) 0.3315(2) 0.0587(13) Uani 1 1 d . B 1
H57A H 0.7803 0.3016 0.3463 0.070 Uiso 1 1 calc R B 1
H57B H 0.7510 0.2512 0.3240 0.070 Uiso 1 1 calc R B 1
C58 C 0.6676(3) 0.27751(17) 0.3860(2) 0.0454(11) Uani 1 1 d . B 1
C59 C 0.6469(3) 0.31661(17) 0.4193(2) 0.0548(12) Uani 1 1 d . B 1
H59 H 0.6705 0.3449 0.4086 0.066 Uiso 1 1 calc R B 1
C60 C 0.5914(3) 0.31414(17) 0.4684(2) 0.0558(12) Uani 1 1 d . B 1
H60 H 0.5771 0.3408 0.4896 0.067 Uiso 1 1 calc R B 1
C61 C 0.5574(3) 0.27253(18) 0.4859(2) 0.0489(12) Uani 1 1 d . B 1
C62 C 0.5778(3) 0.23348(17) 0.4527(2) 0.0562(13) Uani 1 1 d . B 1
H62 H 0.5549 0.2051 0.4635 0.067 Uiso 1 1 calc R B 1
C63 C 0.6322(3) 0.23662(16) 0.4036(2) 0.0515(12) Uani 1 1 d . B 1
H63 H 0.6451 0.2100 0.3817 0.062 Uiso 1 1 calc R B 1
C64 C 0.5053(3) 0.26956(17) 0.5433(2) 0.0579(13) Uani 1 1 d . B 1
H64A H 0.5207 0.2403 0.5658 0.069 Uiso 1 1 calc R B 1
H64B H 0.5303 0.2935 0.5757 0.069 Uiso 1 1 calc R B 1
C65 C 0.3477(3) 0.28776(14) 0.5683(3) 0.0491(12) Uani 1 1 d . B 1
C66 C 0.2394(3) 0.29504(14) 0.5472(2) 0.0483(12) Uani 1 1 d . B 1
C67 C 0.1924(3) 0.31325(15) 0.5953(2) 0.0531(12) Uani 1 1 d . B 1
H67 H 0.2285 0.3191 0.6386 0.064 Uiso 1 1 calc R B 1
C68 C 0.0938(4) 0.32273(15) 0.5797(3) 0.0614(13) Uani 1 1 d . B 1
H68 H 0.0634 0.3348 0.6124 0.074 Uiso 1 1 calc R B 1
C69 C 0.0397(4) 0.31438(16) 0.5155(3) 0.0622(13) Uani 1 1 d . B 1
H69 H -0.0271 0.3209 0.5050 0.075 Uiso 1 1 calc R B 1
C70 C 0.0842(3) 0.29640(15) 0.4668(2) 0.0528(12) Uani 1 1 d . B 1
C71 C 0.1842(3) 0.28645(14) 0.4833(2) 0.0495(12) Uani 1 1 d . B 1
H71 H 0.2143 0.2739 0.4509 0.059 Uiso 1 1 calc R B 1
C72 C 0.0241(4) 0.2908(2) 0.3977(3) 0.0632(14) Uani 1 1 d . B 1
C73 C -0.0041(4) 0.24808(19) 0.2915(3) 0.0819(17) Uani 1 1 d . B 1
H73A H -0.0713 0.2589 0.2842 0.098 Uiso 1 1 calc R B 1
H73B H -0.0058 0.2157 0.2802 0.098 Uiso 1 1 calc R B 1
C74 C 0.0485(4) 0.2738(2) 0.2458(3) 0.0700(15) Uani 1 1 d . B 1
C75 C 0.0152(4) 0.3163(2) 0.2186(3) 0.0811(18) Uani 1 1 d . B 1
H75 H -0.0404 0.3293 0.2292 0.097 Uiso 1 1 calc R B 1
C76 C 0.0634(4) 0.3392(2) 0.1762(3) 0.0824(17) Uani 1 1 d . B 1
H76 H 0.0398 0.3675 0.1590 0.099 Uiso 1 1 calc R B 1
C77 C 0.1462(4) 0.3212(2) 0.1585(3) 0.0694(15) Uani 1 1 d . B 1
C78 C 0.1796(4) 0.2787(2) 0.1868(3) 0.0731(16) Uani 1 1 d . B 1
H78 H 0.2358 0.2659 0.1768 0.088 Uiso 1 1 calc R B 1
C79 C 0.1313(4) 0.25567(19) 0.2289(3) 0.0702(15) Uani 1 1 d . B 1
H79 H 0.1548 0.2274 0.2464 0.084 Uiso 1 1 calc R B 1
C80 C 0.1915(4) 0.3445(2) 0.1080(3) 0.0926(18) Uani 1 1 d . B 1
H80A H 0.1707 0.3289 0.0650 0.111 Uiso 1 1 calc R B 1
H80B H 0.1669 0.3757 0.1023 0.111 Uiso 1 1 calc R B 1
O13 O 0.8848(3) 0.41842(12) 0.23341(18) 0.0881(11) Uiso 1 1 d . E 1
H13 H 0.8447 0.3979 0.2216 0.132 Uiso 1 1 calc R E 1
C81 C 0.8544(6) 0.4565(3) 0.1983(4) 0.159(3) Uiso 1 1 d . E 1
H81A H 0.8371 0.4485 0.1509 0.190 Uiso 1 1 calc R E 1
H81B H 0.9093 0.4777 0.2043 0.190 Uiso 1 1 calc R E 1
C82 C 0.7753(6) 0.4794(3) 0.2145(4) 0.151(3) Uiso 1 1 d . E 1
H82A H 0.7282 0.4574 0.2230 0.227 Uiso 1 1 calc R E 1
H82B H 0.7454 0.4988 0.1776 0.227 Uiso 1 1 calc R E 1
H82C H 0.7978 0.4977 0.2541 0.227 Uiso 1 1 calc R E 1
C83 C 0.0892(9) 0.1027(5) 0.2570(7) 0.231(5) Uiso 1 1 d . F 1
C84 C 0.0353(7) 0.0732(3) 0.2029(5) 0.169(3) Uiso 1 1 d . F 1
O14 O 0.0507(9) 0.0931(5) 0.3168(6) 0.214(5) Uiso 0.60 1 d P F 1
O14' O 0.0479(11) 0.1365(6) 0.3054(7) 0.169(5) Uiso 0.40 1 d P G 2
C27' C 0.5224(14) 0.0060(5) 0.4075(9) 0.112(7) Uiso 0.483(13) 1 d PD A 2
C28' C 0.6080(11) -0.0149(5) 0.4513(8) 0.107(5) Uiso 0.483(13) 1 d PD A 2
H28C H 0.6370 0.0066 0.4864 0.128 Uiso 0.483(13) 1 calc PR A 2
H28D H 0.5877 -0.0419 0.4727 0.128 Uiso 0.483(13) 1 calc PR A 2
C29' C 0.6800(8) -0.0279(5) 0.4132(6) 0.092(5) Uiso 0.483(13) 1 d PD A 2
H29C H 0.6901 -0.0030 0.3838 0.111 Uiso 0.483(13) 1 calc PR A 2
H29D H 0.6576 -0.0545 0.3856 0.111 Uiso 0.483(13) 1 calc PR A 2
C30' C 0.7709(6) -0.0382(3) 0.4607(5) 0.120(3) Uiso 0.80 1 d PD A 2
H30C H 0.8191 -0.0454 0.4342 0.144 Uiso 0.70 1 calc PR A 2
H30D H 0.7598 -0.0663 0.4836 0.144 Uiso 0.70 1 calc PR A 2
C31' C 0.818(2) -0.0057(8) 0.5133(11) 0.188(13) Uiso 0.483(13) 1 d PD A 2
H31C H 0.8201 -0.0225 0.5549 0.226 Uiso 0.483(13) 1 calc PR A 2
H31D H 0.7685 0.0177 0.5122 0.226 Uiso 0.483(13) 1 calc PR A 2
C32' C 0.912(3) 0.0207(12) 0.528(2) 0.152(15) Uiso 0.20 1 d PD A 2
H32' H 0.9683 0.0046 0.5473 0.182 Uiso 0.20 1 calc PR A 2
C33' C 0.922(2) 0.0649(9) 0.5158(13) 0.147(9) Uiso 0.30 1 d PD A 2
H33' H 0.8890 0.0785 0.5458 0.176 Uiso 0.30 1 calc PR A 2
C34' C 0.955(2) 0.1055(8) 0.4830(16) 0.186(12) Uiso 0.30 1 d PD A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0377(18) 0.051(2) 0.070(2) -0.0031(15) 0.0237(15) 0.0020(15)
O2 0.0496(19) 0.085(2) 0.051(2) -0.0088(17) 0.0206(16) 0.0016(17)
O3 0.061(2) 0.059(2) 0.068(2) -0.0128(18) 0.0208(18) -0.0079(16)
O4 0.0516(19) 0.066(2) 0.069(2) -0.0077(17) 0.0244(17) -0.0101(17)
O5 0.097(3) 0.111(3) 0.123(3) -0.001(3) 0.045(3) -0.040(3)
O6 0.074(3) 0.083(3) 0.131(3) 0.008(3) 0.038(2) -0.015(2)
O7 0.077(3) 0.096(3) 0.101(3) 0.018(2) 0.000(2) -0.035(2)
O8 0.057(2) 0.090(3) 0.058(2) -0.0086(19) 0.0192(18) 0.0039(18)
O9 0.042(2) 0.082(3) 0.097(3) -0.005(2) 0.0159(18) 0.005(2)
O10 0.091(3) 0.138(4) 0.081(3) -0.017(3) -0.006(2) 0.022(3)
O11 0.067(2) 0.061(2) 0.068(2) 0.0087(16) 0.0248(16) 0.0008(17)
O12 0.084(2) 0.074(2) 0.087(2) -0.0054(18) 0.0317(19) 0.0132(19)
F1 0.0557(18) 0.067(2) 0.159(3) -0.0317(19) 0.0520(18) -0.0114(16)
F2 0.0582(18) 0.062(2) 0.128(2) 0.0144(18) 0.0415(16) 0.0160(15)
F3 0.0541(17) 0.152(3) 0.080(2) 0.0162(19) 0.0359(15) 0.0301(18)
N1 0.040(2) 0.051(2) 0.051(2) -0.0020(18) 0.018(2) 0.0028(19)
N2 0.036(2) 0.051(2) 0.052(2) -0.0043(18) 0.020(2) -0.0042(18)
N3 0.031(2) 0.044(2) 0.059(2) 0.0000(17) 0.018(2) 0.0026(18)
N4 0.031(2) 0.045(2) 0.048(2) -0.0012(17) 0.0127(19) -0.0029(17)
N5 0.052(2) 0.047(3) 0.059(2) -0.008(2) 0.0229(19) -0.004(2)
N6 0.101(3) 0.049(3) 0.105(3) -0.022(3) 0.067(3) -0.016(2)
N7 0.046(2) 0.067(3) 0.059(3) -0.001(2) 0.016(2) -0.004(2)
N8 0.038(2) 0.063(3) 0.056(2) -0.0031(19) 0.017(2) -0.0075(19)
N9 0.045(2) 0.069(3) 0.096(3) -0.023(3) 0.013(2) -0.004(2)
N10 0.055(3) 0.082(3) 0.080(3) -0.004(3) 0.000(3) 0.004(2)
C1 0.036(3) 0.053(4) 0.070(4) 0.005(3) 0.015(3) 0.003(3)
C2 0.035(3) 0.048(3) 0.064(3) 0.001(2) 0.020(3) 0.006(2)
C3 0.043(3) 0.046(3) 0.058(3) 0.000(2) 0.020(3) 0.004(2)
C4 0.042(3) 0.048(3) 0.047(3) 0.003(2) 0.018(3) 0.002(2)
C5 0.034(3) 0.051(3) 0.053(3) 0.003(2) 0.015(2) 0.000(2)
C6 0.045(3) 0.068(3) 0.056(3) 0.001(2) 0.017(3) 0.008(3)
C7 0.043(3) 0.064(3) 0.066(3) 0.006(3) 0.014(2) 0.002(3)
C8 0.032(3) 0.033(3) 0.055(3) 0.003(2) 0.011(2) -0.002(2)
C9 0.040(3) 0.042(3) 0.047(3) -0.004(2) 0.017(2) 0.001(2)
C10 0.040(3) 0.045(3) 0.051(3) -0.001(2) 0.018(3) 0.000(2)
C11 0.036(3) 0.026(3) 0.064(3) 0.005(2) 0.016(3) -0.004(2)
C12 0.041(3) 0.048(3) 0.059(3) 0.005(2) 0.018(2) 0.005(2)
C13 0.035(2) 0.044(3) 0.046(3) 0.002(2) 0.012(2) 0.000(2)
C14 0.037(3) 0.044(3) 0.055(3) -0.011(2) 0.012(2) -0.001(2)
C15 0.036(3) 0.053(3) 0.059(3) -0.002(3) 0.019(2) -0.001(2)
C16 0.040(3) 0.040(3) 0.056(3) -0.005(3) 0.018(2) 0.001(2)
C17 0.046(3) 0.054(3) 0.062(3) -0.012(3) 0.021(2) -0.002(3)
C18 0.046(3) 0.057(3) 0.057(3) -0.004(3) 0.025(2) -0.008(3)
C19 0.035(3) 0.053(4) 0.074(4) -0.014(3) 0.022(3) 0.006(2)
C20 0.047(3) 0.050(3) 0.083(3) -0.017(3) 0.029(3) -0.012(3)
C21 0.042(3) 0.054(3) 0.068(3) -0.012(3) 0.024(2) -0.003(2)
C22 0.044(3) 0.058(4) 0.065(3) -0.010(3) 0.022(3) -0.006(3)
C23 0.101(5) 0.056(4) 0.136(5) -0.016(4) 0.073(4) -0.018(4)
C24 0.102(5) 0.069(4) 0.076(4) -0.014(3) 0.040(3) -0.025(4)
C25 0.139(6) 0.072(4) 0.066(3) -0.012(3) 0.048(3) -0.028(4)
C37 0.062(4) 0.127(6) 0.101(4) 0.026(4) 0.015(4) 0.013(4)
C38 0.052(4) 0.141(6) 0.094(4) 0.028(4) 0.006(3) 0.008(4)
C39 0.068(4) 0.114(6) 0.101(5) 0.012(4) 0.018(3) 0.002(4)
C40 0.064(4) 0.115(5) 0.093(4) 0.005(4) 0.022(3) -0.002(4)
C42 0.067(4) 0.113(6) 0.088(4) 0.000(4) 0.017(3) -0.020(4)
C43 0.064(4) 0.106(5) 0.093(4) 0.002(4) 0.036(3) -0.002(4)
C44 0.053(3) 0.095(5) 0.077(4) 0.017(3) 0.024(3) -0.003(3)
C45 0.061(4) 0.094(4) 0.063(3) 0.016(3) 0.025(3) -0.001(3)
C46 0.054(3) 0.082(4) 0.053(3) -0.003(3) 0.024(2) -0.002(3)
C47 0.055(3) 0.063(3) 0.055(3) 0.001(3) 0.022(2) 0.000(3)
C48 0.045(3) 0.062(3) 0.044(3) -0.003(2) 0.020(2) 0.004(2)
C49 0.060(4) 0.058(3) 0.066(3) 0.003(3) 0.023(3) 0.002(3)
C50 0.066(4) 0.076(4) 0.074(4) 0.000(3) 0.026(3) 0.009(3)
C51 0.085(5) 0.088(4) 0.079(4) 0.012(3) 0.033(4) 0.019(4)
C52 0.082(5) 0.078(4) 0.065(4) 0.002(3) 0.016(3) 0.023(3)
C53 0.061(4) 0.063(3) 0.063(4) -0.005(3) 0.011(3) 0.015(3)
C54 0.058(3) 0.060(3) 0.066(4) -0.006(3) 0.022(3) 0.005(3)
C55 0.077(4) 0.066(4) 0.076(4) -0.013(3) 0.002(4) 0.015(3)
C56 0.048(3) 0.067(4) 0.073(4) 0.004(3) 0.026(3) 0.006(3)
C57 0.041(3) 0.068(3) 0.069(3) -0.001(3) 0.016(3) 0.002(2)
C58 0.031(2) 0.046(3) 0.061(3) -0.005(3) 0.014(2) -0.001(2)
C59 0.049(3) 0.051(3) 0.068(3) 0.005(3) 0.019(3) -0.009(2)
C60 0.048(3) 0.052(3) 0.072(3) -0.006(3) 0.023(3) 0.007(3)
C61 0.034(3) 0.057(3) 0.058(3) -0.003(3) 0.013(2) -0.004(2)
C62 0.052(3) 0.052(3) 0.064(3) 0.002(3) 0.011(3) -0.011(3)
C63 0.052(3) 0.045(3) 0.059(3) -0.005(2) 0.017(2) 0.004(3)
C64 0.042(3) 0.073(4) 0.062(3) 0.003(3) 0.017(2) -0.005(3)
C65 0.054(3) 0.041(3) 0.057(3) 0.002(2) 0.022(3) -0.006(2)
C66 0.042(3) 0.041(3) 0.069(3) 0.006(2) 0.026(3) -0.006(2)
C67 0.052(3) 0.050(3) 0.063(3) 0.006(2) 0.026(3) -0.008(3)
C68 0.061(4) 0.057(3) 0.076(4) 0.009(3) 0.038(3) 0.005(3)
C69 0.051(3) 0.057(3) 0.087(4) 0.013(3) 0.033(3) -0.002(3)
C70 0.041(3) 0.054(3) 0.068(3) -0.006(3) 0.024(3) -0.006(2)
C71 0.041(3) 0.042(3) 0.070(3) -0.003(2) 0.021(3) -0.004(2)
C72 0.030(3) 0.068(4) 0.093(4) 0.000(4) 0.017(3) -0.010(3)
C73 0.047(3) 0.094(4) 0.101(4) -0.045(4) 0.009(3) -0.009(3)
C74 0.040(3) 0.080(4) 0.088(4) -0.028(3) 0.009(3) -0.005(3)
C75 0.046(3) 0.099(5) 0.089(4) -0.033(4) -0.006(3) 0.018(4)
C76 0.063(4) 0.087(5) 0.087(4) -0.020(4) -0.006(3) 0.009(4)
C77 0.044(3) 0.069(4) 0.087(4) -0.024(3) -0.006(3) 0.000(3)
C78 0.042(3) 0.073(4) 0.103(4) -0.031(4) 0.014(3) -0.001(3)
C79 0.046(3) 0.064(4) 0.098(4) -0.025(3) 0.011(3) -0.002(3)
C80 0.060(4) 0.098(5) 0.114(5) 0.002(4) 0.005(4) -0.006(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C11 1.236(5) . ?
O2 C10 1.216(5) . ?
O3 C19 1.230(5) . ?
O4 C22 1.242(5) . ?
O5 C42 1.215(7) . ?
O6 C42 1.302(7) . ?
O6 C43 1.453(6) . ?
O7 C56 1.234(5) . ?
O8 C65 1.239(5) . ?
O9 C72 1.242(5) . ?
O10 C55 1.247(6) . ?
F1 C1 1.321(5) . ?
F2 C1 1.327(5) . ?
F3 C1 1.328(5) . ?
N1 C9 1.300(5) . ?
N1 C4 1.360(5) . ?
N2 C8 1.364(5) . ?
N2 C5 1.397(5) . ?
N2 C48 1.475(5) . ?
N3 C8 1.310(5) . ?
N3 C11 1.356(5) . ?
N4 C10 1.376(5) . ?
N4 C11 1.410(5) . ?
N4 C12 1.473(5) . ?
N5 C19 1.348(5) . ?
N5 C16 1.416(5) . ?
N6 C22 1.322(5) . ?
N6 C23 1.464(6) . ?
N7 C56 1.321(6) . ?
N7 C57 1.453(5) . ?
N8 C65 1.338(5) . ?
N8 C64 1.461(5) . ?
N9 C72 1.353(6) . ?
N9 C73 1.456(6) . ?
N10 C55 1.323(7) . ?
N10 C80 1.463(6) . ?
C1 C2 1.475(6) . ?
C2 C3 1.360(5) . ?
C2 C7 1.397(6) . ?
C3 C4 1.400(6) . ?
C4 C5 1.424(5) . ?
C5 C6 1.389(5) . ?
C6 C7 1.381(6) . ?
C8 C9 1.457(5) . ?
C9 C10 1.465(6) . ?
C12 C13 1.501(5) . ?
C13 C18 1.382(6) . ?
C13 C14 1.388(6) . ?
C14 C15 1.388(5) . ?
C15 C16 1.369(6) . ?
C16 C17 1.382(6) . ?
C17 C18 1.386(6) . ?
C19 C20 1.516(6) . ?
C20 C21 1.515(6) . ?
C21 C22 1.505(6) . ?
C23 C24 1.494(7) . ?
C24 C25 1.522(7) . ?
C25 C26 1.508(7) . ?
C26 C27 1.488(11) . ?
C27 C28 1.507(14) . ?
C28 C29 1.487(16) . ?
C29 C30 1.50(2) . ?
C30 C31 1.51(2) . ?
C31 C32 1.480(14) . ?
C32 C33 1.312(12) . ?
C33 C34 1.509(10) . ?
C34 C35 1.424(9) . ?
C35 C36 1.479(9) . ?
C36 C37 1.454(8) . ?
C37 C38 1.499(8) . ?
C38 C39 1.468(8) . ?
C39 C40 1.484(7) . ?
C40 C41 1.474(8) . ?
C41 C42 1.525(9) . ?
C43 C44 1.490(7) . ?
C44 C45 1.487(6) . ?
C45 C46 1.535(6) . ?
C46 C47 1.519(6) . ?
C47 C48 1.503(6) . ?
C49 C54 1.383(6) . ?
C49 C50 1.395(6) . ?
C49 C56 1.495(7) . ?
C50 C51 1.347(6) . ?
C51 C52 1.378(7) . ?
C52 C53 1.403(7) . ?
C53 C54 1.373(6) . ?
C53 C55 1.497(7) . ?
C57 C58 1.504(6) . ?
C58 C63 1.368(6) . ?
C58 C59 1.388(6) . ?
C59 C60 1.390(6) . ?
C60 C61 1.377(6) . ?
C61 C62 1.384(6) . ?
C61 C64 1.505(6) . ?
C62 C63 1.380(6) . ?
C65 C66 1.495(6) . ?
C66 C71 1.382(6) . ?
C66 C67 1.392(6) . ?
C67 C68 1.372(6) . ?
C68 C69 1.381(6) . ?
C69 C70 1.380(6) . ?
C70 C71 1.393(6) . ?
C70 C72 1.481(6) . ?
C73 C74 1.502(7) . ?
C74 C79 1.378(7) . ?
C74 C75 1.396(7) . ?
C75 C76 1.374(7) . ?
C76 C77 1.384(7) . ?
C77 C78 1.403(7) . ?
C77 C80 1.481(7) . ?
C78 C79 1.375(7) . ?
O13 C81 1.338(8) . ?
C81 C82 1.388(10) . ?
C83 O14 1.459(16) . ?
C83 C84 1.469(13) . ?
C27' C28' 1.459(15) . ?
C28' C29' 1.445(14) . ?
C29' C30' 1.450(11) . ?
C30' C31' 1.474(16) . ?
C31' C32' 1.489(19) . ?
C32' C33' 1.33(2) . ?
C33' C34' 1.480(18) . ?

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
C42 O6 C43 119.2(5) . . ?
C9 N1 C4 118.7(4) . . ?
C8 N2 C5 120.4(4) . . ?
C8 N2 C48 118.7(3) . . ?
C5 N2 C48 120.8(3) . . ?
C8 N3 C11 119.5(4) . . ?
C10 N4 C11 122.8(3) . . ?
C10 N4 C12 117.7(3) . . ?
C11 N4 C12 119.3(3) . . ?
C19 N5 C16 127.5(4) . . ?
C22 N6 C23 124.8(4) . . ?
C56 N7 C57 123.7(4) . . ?
C65 N8 C64 119.6(4) . . ?
C72 N9 C73 121.3(4) . . ?
C55 N10 C80 121.0(5) . . ?
F1 C1 F2 105.1(4) . . ?
F1 C1 F3 105.5(4) . . ?
F2 C1 F3 105.3(4) . . ?
F1 C1 C2 113.6(4) . . ?
F2 C1 C2 113.1(4) . . ?
F3 C1 C2 113.4(4) . . ?
C3 C2 C7 119.8(4) . . ?
C3 C2 C1 120.4(4) . . ?
C7 C2 C1 119.8(4) . . ?
C2 C3 C4 120.6(4) . . ?
N1 C4 C3 118.9(4) . . ?
N1 C4 C5 122.1(4) . . ?
C3 C4 C5 119.0(4) . . ?
C6 C5 N2 122.0(4) . . ?
C6 C5 C4 120.1(4) . . ?
N2 C5 C4 117.9(4) . . ?
C7 C6 C5 118.7(4) . . ?
C6 C7 C2 121.7(4) . . ?
N3 C8 N2 119.7(4) . . ?
N3 C8 C9 123.0(4) . . ?
N2 C8 C9 117.3(4) . . ?
N1 C9 C8 123.5(4) . . ?
N1 C9 C10 118.7(4) . . ?
C8 C9 C10 117.8(4) . . ?
O2 C10 N4 122.1(4) . . ?
O2 C10 C9 122.5(4) . . ?
N4 C10 C9 115.4(4) . . ?
O1 C11 N3 120.3(4) . . ?
O1 C11 N4 118.3(4) . . ?
N3 C11 N4 121.4(4) . . ?
N4 C12 C13 110.4(3) . . ?
C18 C13 C14 117.9(4) . . ?
C18 C13 C12 122.1(4) . . ?
C14 C13 C12 119.7(4) . . ?
C13 C14 C15 120.2(4) . . ?
C16 C15 C14 121.0(4) . . ?
C15 C16 C17 119.5(4) . . ?
C15 C16 N5 117.2(4) . . ?
C17 C16 N5 123.2(4) . . ?
C16 C17 C18 119.3(4) . . ?
C13 C18 C17 122.0(4) . . ?
O3 C19 N5 122.6(5) . . ?
O3 C19 C20 121.8(4) . . ?
N5 C19 C20 115.6(5) . . ?
C21 C20 C19 110.6(4) . . ?
C22 C21 C20 113.3(4) . . ?
O4 C22 N6 123.1(5) . . ?
O4 C22 C21 121.0(4) . . ?
N6 C22 C21 115.9(4) . . ?
N6 C23 C24 112.3(5) . . ?
C23 C24 C25 112.8(5) . . ?
C26 C25 C24 111.7(5) . . ?
C27 C26 C25 108.6(7) . . ?
C26 C27 C28 105.2(10) . . ?
C29 C28 C27 123.3(14) . . ?
C28 C29 C30 129(2) . . ?
C29 C30 C31 111(2) . . ?
C32 C31 C30 124.9(19) . . ?
C33 C32 C31 133.0(13) . . ?
C32 C33 C34 130.6(11) . . ?
C35 C34 C33 114.0(8) . . ?
C34 C35 C36 114.6(8) . . ?
C37 C36 C35 114.1(7) . . ?
C36 C37 C38 115.1(6) . . ?
C39 C38 C37 116.2(6) . . ?
C38 C39 C40 115.7(6) . . ?
C41 C40 C39 111.7(6) . . ?
C40 C41 C42 118.8(7) . . ?
O5 C42 O6 123.4(6) . . ?
O5 C42 C41 124.5(7) . . ?
O6 C42 C41 112.1(6) . . ?
O6 C43 C44 106.3(5) . . ?
C45 C44 C43 114.2(4) . . ?
C44 C45 C46 112.8(4) . . ?
C47 C46 C45 112.4(4) . . ?
C48 C47 C46 113.0(4) . . ?
N2 C48 C47 110.8(3) . . ?
C54 C49 C50 118.2(5) . . ?
C54 C49 C56 123.5(5) . . ?
C50 C49 C56 118.2(5) . . ?
C51 C50 C49 121.5(5) . . ?
C50 C51 C52 119.9(5) . . ?
C51 C52 C53 120.4(5) . . ?
C54 C53 C52 118.5(5) . . ?
C54 C53 C55 124.6(5) . . ?
C52 C53 C55 117.0(5) . . ?
C53 C54 C49 121.4(5) . . ?
O10 C55 N10 121.8(5) . . ?
O10 C55 C53 119.0(6) . . ?
N10 C55 C53 119.2(5) . . ?
O7 C56 N7 122.4(5) . . ?
O7 C56 C49 121.0(5) . . ?
N7 C56 C49 116.6(5) . . ?
N7 C57 C58 112.2(4) . . ?
C63 C58 C59 117.6(4) . . ?
C63 C58 C57 122.2(4) . . ?
C59 C58 C57 120.1(4) . . ?
C58 C59 C60 120.9(4) . . ?
C61 C60 C59 120.4(4) . . ?
C60 C61 C62 118.8(4) . . ?
C60 C61 C64 120.1(4) . . ?
C62 C61 C64 121.0(4) . . ?
C63 C62 C61 120.0(4) . . ?
C58 C63 C62 122.2(4) . . ?
N8 C64 C61 114.2(3) . . ?
O8 C65 N8 121.2(4) . . ?
O8 C65 C66 118.7(4) . . ?
N8 C65 C66 120.0(4) . . ?
C71 C66 C67 118.5(4) . . ?
C71 C66 C65 124.5(4) . . ?
C67 C66 C65 116.9(4) . . ?
C68 C67 C66 121.0(4) . . ?
C67 C68 C69 119.9(5) . . ?
C70 C69 C68 120.3(5) . . ?
C69 C70 C71 119.3(4) . . ?
C69 C70 C72 118.1(5) . . ?
C71 C70 C72 122.5(4) . . ?
C66 C71 C70 120.9(4) . . ?
O9 C72 N9 122.3(5) . . ?
O9 C72 C70 120.5(5) . . ?
N9 C72 C70 117.2(5) . . ?
N9 C73 C74 112.0(4) . . ?
C79 C74 C75 117.9(6) . . ?
C79 C74 C73 120.7(6) . . ?
C75 C74 C73 121.5(6) . . ?
C76 C75 C74 120.9(6) . . ?
C75 C76 C77 121.9(6) . . ?
C76 C77 C78 116.7(6) . . ?
C76 C77 C80 120.8(6) . . ?
C78 C77 C80 122.3(6) . . ?
C79 C78 C77 121.6(5) . . ?
C78 C79 C74 121.1(5) . . ?
N10 C80 C77 114.6(5) . . ?
O13 C81 C82 116.7(8) . . ?
O14 C83 C84 106.8(11) . . ?
C29' C28' C27' 110.8(14) . . ?
C28' C29' C30' 107.9(11) . . ?
C29' C30' C31' 122.6(14) . . ?
C30' C31' C32' 135(3) . . ?
C33' C32' C31' 126(3) . . ?
C32' C33' C34' 157(3) . . ?

_diffrn_measured_fraction_theta_max 0.809
_diffrn_reflns_theta_full        24.41
_diffrn_measured_fraction_theta_full 0.809
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.05