# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_sn_1796_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1472884'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            TCA
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 N4 O24'
_chemical_formula_sum            'C84 H60 N4 O24'
_chemical_formula_weight         1509.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           'monoclinic '
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   7.2350(9)
_cell_length_b                   27.116(4)
_cell_length_c                   50.042(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.752(6)
_cell_angle_gamma                90.00
_cell_volume                     9806(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      61.50

_exptl_crystal_description       'Niddle shaped'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  Micro-focus
_diffrn_measurement_device_type  'D8 Venture APEX-II'
_diffrn_measurement_method       'CMOS-Photon 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            158928
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         61.50
_reflns_number_total             14569
_reflns_number_gt                7813
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS)'
_computing_cell_refinement       'SHELXTL suite'
_computing_data_reduction        'SHELXTL suite'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  'Mercury 3.1'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1485P)²+7.0834P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00039(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14569
_refine_ls_number_parameters     1014
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.0926
_refine_ls_wR_factor_ref         0.3048
_refine_ls_wR_factor_gt          0.2563
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_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
O21 O 0.6130(5) 0.21069(16) -0.08288(7) 0.0765(11) Uani 1 1 d . . .
O7 O 0.6191(5) 0.79801(18) 0.16535(7) 0.0776(11) Uani 1 1 d . . .
O11 O 0.7590(5) 0.71758(17) 0.38227(7) 0.0876(13) Uani 1 1 d . . .
H119 H 0.8461 0.7209 0.3938 0.131 Uiso 1 1 calc R . .
O3 O -0.0053(5) 0.70560(17) 0.42220(7) 0.0895(13) Uani 1 1 d . . .
O15 O -0.0074(5) 0.34181(17) 0.17233(7) 0.0946(14) Uani 1 1 d . . .
H15 H -0.0673 0.3370 0.1578 0.142 Uiso 1 1 calc R . .
O6 O 1.3728(5) 0.52835(15) 0.52189(9) 0.0886(13) Uani 1 1 d . . .
N1 N 0.6376(5) 0.65567(16) 0.50738(8) 0.0578(11) Uani 1 1 d . . .
N3 N 0.6199(5) 0.37043(16) 0.26268(8) 0.0610(12) Uani 1 1 d . . .
O4 O 0.2285(5) 0.72197(17) 0.39649(8) 0.0900(13) Uani 1 1 d . . .
H117 H 0.1399 0.7279 0.3855 0.135 Uiso 1 1 calc R . .
N4 N 0.3572(5) 0.34239(16) 0.01511(8) 0.0609(11) Uani 1 1 d . . .
O12 O 0.9910(5) 0.72491(18) 0.35522(7) 0.0924(14) Uani 1 1 d . . .
O8 O 0.6598(6) 0.71903(17) 0.15456(8) 0.0932(13) Uani 1 1 d . . .
H8 H 0.6997 0.7323 0.1408 0.140 Uiso 1 1 calc R . .
O20 O 1.0005(5) 0.32466(18) 0.10462(7) 0.0944(14) Uani 1 1 d . . .
H121 H 1.0596 0.3245 0.1195 0.142 Uiso 1 1 calc R . .
O18 O 1.2760(5) 0.52096(16) 0.24516(9) 0.0945(13) Uani 1 1 d . . .
H18 H 1.3760 0.5365 0.2474 0.142 Uiso 1 1 calc R . .
N2 N 0.3347(5) 0.68913(16) 0.26911(8) 0.0586(11) Uani 1 1 d . . .
O1 O 0.2689(6) 0.67657(19) 0.62008(9) 0.0901(14) Uani 1 1 d . . .
O13 O 0.2572(6) 0.32501(18) 0.37342(8) 0.0917(13) Uani 1 1 d . . .
H13 H 0.2126 0.3097 0.3862 0.137 Uiso 1 1 calc R . .
O22 O 0.6601(6) 0.28686(16) -0.09810(8) 0.0930(13) Uani 1 1 d . . .
H22 H 0.6955 0.2707 -0.1112 0.140 Uiso 1 1 calc R . .
O19 O 0.7638(5) 0.33410(18) 0.13106(8) 0.0930(14) Uani 1 1 d . . .
O16 O 0.2303(5) 0.32633(18) 0.14676(8) 0.0917(14) Uani 1 1 d . . .
O17 O 1.3517(6) 0.49595(15) 0.28641(9) 0.0899(13) Uani 1 1 d . . .
O9 O -0.4068(6) 0.56717(16) 0.24864(9) 0.0968(14) Uani 1 1 d . . .
O2 O 0.2863(6) 0.75550(19) 0.60844(8) 0.0932(13) Uani 1 1 d . . .
O5 O 1.3009(5) 0.51486(16) 0.47872(9) 0.0924(13) Uani 1 1 d . . .
H5 H 1.4022 0.4997 0.4798 0.139 Uiso 1 1 calc R . .
O14 O 0.2851(6) 0.24833(19) 0.35774(8) 0.0936(13) Uani 1 1 d . . .
O10 O -0.3239(5) 0.54039(17) 0.28924(9) 0.0981(14) Uani 1 1 d . . .
H10 H -0.4242 0.5250 0.2872 0.147 Uiso 1 1 calc R . .
O24 O -0.3832(6) 0.45882(16) -0.01494(10) 0.1034(15) Uani 1 1 d . . .
O23 O -0.2987(6) 0.49630(17) 0.02312(9) 0.1049(15) Uani 1 1 d . . .
H23 H -0.3986 0.5115 0.0199 0.157 Uiso 1 1 calc R . .
C26 C 0.3981(6) 0.7053(2) 0.24363(10) 0.0553(13) Uani 1 1 d . . .
C12 C 0.5255(7) 0.66924(19) 0.48435(9) 0.0552(13) Uani 1 1 d . . .
C68 C 0.4698(7) 0.33740(19) 0.03872(10) 0.0568(13) Uani 1 1 d . . .
C33 C 0.1820(7) 0.6576(2) 0.26935(10) 0.0576(13) Uani 1 1 d . . .
C47 C 0.5460(6) 0.3522(2) 0.28651(10) 0.0563(13) Uani 1 1 d . . .
C40 C 0.4520(6) 0.69888(19) 0.29192(9) 0.0554(13) Uani 1 1 d . . .
C75 C 0.4177(6) 0.3207(2) -0.00890(10) 0.0567(14) Uani 1 1 d . . .
C61 C 0.7675(7) 0.40357(19) 0.26367(10) 0.0560(13) Uani 1 1 d . . .
C5 C 0.5626(6) 0.6683(2) 0.53237(10) 0.0556(13) Uani 1 1 d . . .
C51 C 0.2869(7) 0.3449(2) 0.19326(10) 0.0623(14) Uani 1 1 d . . .
C58 C 1.0750(7) 0.46663(19) 0.26592(11) 0.0618(14) Uani 1 1 d . . .
C19 C 0.7850(7) 0.62280(18) 0.50609(10) 0.0545(13) Uani 1 1 d . . .
C23 C 0.5349(6) 0.7362(2) 0.19567(10) 0.0564(13) Uani 1 1 d . . .
C72 C 0.5409(7) 0.2783(2) -0.05568(11) 0.0577(13) Uani 1 1 d . . .
C54 C 0.5132(7) 0.36234(18) 0.23870(10) 0.0543(13) Uani 1 1 d . . .
C9 C 0.2935(7) 0.6960(2) 0.44074(10) 0.0610(14) Uani 1 1 d . . .
C39 C 0.6397(7) 0.7029(2) 0.28910(10) 0.0648(15) Uani 1 1 d . . .
H39 H 0.6876 0.7002 0.2718 0.078 Uiso 1 1 calc R . .
C82 C 0.2038(7) 0.3734(2) 0.01328(10) 0.0601(14) Uani 1 1 d . . .
C18 C 0.9067(7) 0.61602(19) 0.52821(10) 0.0598(14) Uani 1 1 d . . .
H18A H 0.8848 0.6327 0.5445 0.072 Uiso 1 1 calc R . .
C65 C 0.7046(7) 0.3305(2) 0.08436(10) 0.0619(14) Uani 1 1 d . . .
C62 C 0.8894(7) 0.40444(18) 0.28610(10) 0.0566(13) Uani 1 1 d . . .
H62 H 0.8699 0.3832 0.3008 0.068 Uiso 1 1 calc R . .
C55 C 0.3257(7) 0.3698(2) 0.23925(10) 0.0648(15) Uani 1 1 d . . .
H55 H 0.2729 0.3806 0.2552 0.078 Uiso 1 1 calc R . .
C37 C 0.6913(7) 0.7148(2) 0.33611(10) 0.0614(14) Uani 1 1 d . . .
C43 C 0.3060(7) 0.2941(3) 0.35563(12) 0.0727(17) Uani 1 1 d . . .
C69 C 0.6602(7) 0.3325(2) 0.03635(10) 0.0675(15) Uani 1 1 d . . .
H69 H 0.7111 0.3319 0.0192 0.081 Uiso 1 1 calc R . .
C34 C 0.0479(7) 0.6606(2) 0.24866(10) 0.0615(14) Uani 1 1 d . . .
H34 H 0.0600 0.6844 0.2349 0.074 Uiso 1 1 calc R . .
C28 C 0.4945(7) 0.6868(2) 0.19981(10) 0.0662(15) Uani 1 1 d . . .
H28 H 0.5142 0.6635 0.1861 0.079 Uiso 1 1 calc R . .
C63 C 1.0384(7) 0.4362(2) 0.28688(11) 0.0631(14) Uani 1 1 d . . .
H63 H 1.1184 0.4370 0.3025 0.076 Uiso 1 1 calc R . .
C81 C 0.0674(7) 0.3652(2) -0.00698(10) 0.0682(15) Uani 1 1 d . . .
H81 H 0.0787 0.3379 -0.0187 0.082 Uiso 1 1 calc R . .
C30 C -0.1279(7) 0.5960(2) 0.26868(12) 0.0668(15) Uani 1 1 d . . .
C56 C 0.2137(7) 0.3613(2) 0.21651(10) 0.0694(16) Uani 1 1 d . . .
H56 H 0.0844 0.3670 0.2170 0.083 Uiso 1 1 calc R . .
C27 C 0.4262(7) 0.6712(2) 0.22366(11) 0.0617(14) Uani 1 1 d . . .
H27 H 0.3988 0.6373 0.2263 0.074 Uiso 1 1 calc R . .
C11 C 0.3384(7) 0.6622(2) 0.48498(10) 0.0624(14) Uani 1 1 d . . .
H118 H 0.2876 0.6481 0.5004 0.075 Uiso 1 1 calc R . .
C25 C 0.4359(7) 0.7546(2) 0.23971(11) 0.0619(14) Uani 1 1 d . . .
H25 H 0.4153 0.7780 0.2534 0.074 Uiso 1 1 calc R . .
C1 C 0.3140(7) 0.7100(3) 0.60410(12) 0.0726(17) Uani 1 1 d . . .
C38 C 0.7570(7) 0.7105(2) 0.31059(11) 0.0690(15) Uani 1 1 d . . .
H38 H 0.8861 0.7129 0.3082 0.083 Uiso 1 1 calc R . .
C2 C 0.3992(7) 0.6957(2) 0.57911(10) 0.0628(15) Uani 1 1 d . . .
C46 C 0.5088(7) 0.3018(2) 0.28852(10) 0.0652(15) Uani 1 1 d . . .
H46 H 0.5372 0.2801 0.2744 0.078 Uiso 1 1 calc R . .
C44 C 0.3883(7) 0.3149(2) 0.33142(11) 0.0641(15) Uani 1 1 d . . .
C13 C 0.5972(7) 0.6901(2) 0.46172(11) 0.0677(15) Uani 1 1 d . . .
H13A H 0.7267 0.6954 0.4611 0.081 Uiso 1 1 calc R . .
C41 C 0.3843(7) 0.7053(2) 0.31686(10) 0.0663(15) Uani 1 1 d . . .
H41 H 0.2544 0.7048 0.3189 0.080 Uiso 1 1 calc R . .
C71 C 0.6088(7) 0.2578(3) -0.08047(12) 0.0673(15) Uani 1 1 d . . .
C24 C 0.5040(7) 0.7694(2) 0.21568(11) 0.0679(15) Uani 1 1 d . . .
H24 H 0.5300 0.8034 0.2129 0.081 Uiso 1 1 calc R . .
C77 C 0.5112(7) 0.2504(2) -0.03357(12) 0.0675(15) Uani 1 1 d . . .
H77 H 0.5323 0.2158 -0.0343 0.081 Uiso 1 1 calc R . .
C4 C 0.5247(7) 0.6333(2) 0.55138(10) 0.0650(15) Uani 1 1 d . . .
H116 H 0.5543 0.5996 0.5484 0.078 Uiso 1 1 calc R . .
C49 C 0.4260(7) 0.3649(2) 0.32982(10) 0.0656(15) Uani 1 1 d . . .
H49 H 0.3985 0.3864 0.3441 0.079 Uiso 1 1 calc R . .
C20 C 0.8173(7) 0.5964(2) 0.48275(10) 0.0638(14) Uani 1 1 d . . .
H120 H 0.7325 0.5988 0.4677 0.077 Uiso 1 1 calc R . .
C74 C 0.4467(7) 0.3500(2) -0.03115(11) 0.0681(15) Uani 1 1 d . . .
H74 H 0.4237 0.3844 -0.0305 0.082 Uiso 1 1 calc R . .
C59 C 0.7985(7) 0.4358(2) 0.24254(11) 0.0682(15) Uani 1 1 d . . .
H59 H 0.7142 0.4367 0.2274 0.082 Uiso 1 1 calc R . .
C42 C 0.5032(7) 0.7125(2) 0.33914(10) 0.0683(16) Uani 1 1 d . . .
H42 H 0.4551 0.7159 0.3564 0.082 Uiso 1 1 calc R . .
C67 C 0.3996(7) 0.3367(2) 0.06380(10) 0.0672(15) Uani 1 1 d . . .
H67 H 0.2695 0.3383 0.0655 0.081 Uiso 1 1 calc R . .
C22 C 0.6088(7) 0.7520(3) 0.17035(12) 0.0704(16) Uani 1 1 d . . .
C16 C 1.0949(7) 0.56122(19) 0.50349(12) 0.0635(14) Uani 1 1 d . . .
C70 C 0.7744(7) 0.3286(2) 0.05933(10) 0.0679(15) Uani 1 1 d . . .
H70 H 0.9038 0.3244 0.0577 0.082 Uiso 1 1 calc R . .
C32 C 0.1607(7) 0.6226(2) 0.28955(10) 0.0657(15) Uani 1 1 d . . .
H32 H 0.2532 0.6194 0.3036 0.079 Uiso 1 1 calc R . .
C76 C 0.4516(7) 0.2708(2) -0.01032(11) 0.0668(15) Uani 1 1 d . . .
H76 H 0.4338 0.2504 0.0048 0.080 Uiso 1 1 calc R . .
C73 C 0.5097(7) 0.3286(2) -0.05441(10) 0.0688(16) Uani 1 1 d . . .
H73 H 0.5313 0.3487 -0.0695 0.083 Uiso 1 1 calc R . .
C66 C 0.5149(7) 0.3337(2) 0.08644(10) 0.0683(15) Uani 1 1 d . . .
H66 H 0.4640 0.3338 0.1036 0.082 Uiso 1 1 calc R . .
C64 C 0.8297(8) 0.3297(2) 0.10823(12) 0.0742(16) Uani 1 1 d . . .
C36 C 0.8220(8) 0.7198(2) 0.35920(11) 0.0692(16) Uani 1 1 d . . .
C50 C 0.1638(8) 0.3372(2) 0.16885(12) 0.0722(16) Uani 1 1 d . . .
C48 C 0.5040(7) 0.3831(2) 0.30718(11) 0.0671(15) Uani 1 1 d . . .
H48 H 0.5291 0.4173 0.3059 0.081 Uiso 1 1 calc R . .
C3 C 0.4443(7) 0.6467(2) 0.57463(10) 0.0672(15) Uani 1 1 d . . .
H3 H 0.4196 0.6224 0.5877 0.081 Uiso 1 1 calc R . .
C17 C 1.0582(7) 0.58558(19) 0.52687(11) 0.0602(14) Uani 1 1 d . . .
H17 H 1.1387 0.5813 0.5423 0.072 Uiso 1 1 calc R . .
C7 C 0.4360(7) 0.7304(2) 0.56030(11) 0.0656(15) Uani 1 1 d . . .
H7 H 0.4048 0.7640 0.5633 0.079 Uiso 1 1 calc R . .
C52 C 0.4744(7) 0.3372(2) 0.19269(11) 0.0723(16) Uani 1 1 d . . .
H52 H 0.5271 0.3261 0.1768 0.087 Uiso 1 1 calc R . .
C60 C 0.9525(8) 0.4666(2) 0.24369(11) 0.0693(15) Uani 1 1 d . . .
H60 H 0.9741 0.4879 0.2291 0.083 Uiso 1 1 calc R . .
C6 C 0.5184(7) 0.7171(2) 0.53691(10) 0.0623(14) Uani 1 1 d . . .
H6 H 0.5445 0.7415 0.5240 0.075 Uiso 1 1 calc R . .
C79 C -0.1053(7) 0.4350(2) 0.00719(12) 0.0705(16) Uani 1 1 d . . .
C80 C -0.0811(7) 0.3957(2) -0.01018(11) 0.0724(16) Uani 1 1 d . . .
H80 H -0.1696 0.3901 -0.0245 0.087 Uiso 1 1 calc R . .
C53 C 0.5861(7) 0.3459(2) 0.21548(11) 0.0730(16) Uani 1 1 d . . .
H53 H 0.7156 0.3404 0.2150 0.088 Uiso 1 1 calc R . .
C84 C 0.0268(8) 0.4433(2) 0.02784(12) 0.0756(17) Uani 1 1 d . . .
H84 H 0.0103 0.4691 0.0403 0.091 Uiso 1 1 calc R . .
C21 C 0.9715(8) 0.5667(2) 0.48146(11) 0.0690(15) Uani 1 1 d . . .
H21A H 0.9939 0.5498 0.4653 0.083 Uiso 1 1 calc R . .
C45 C 0.4312(7) 0.2838(2) 0.31099(11) 0.0686(15) Uani 1 1 d . . .
H45 H 0.4069 0.2495 0.3124 0.082 Uiso 1 1 calc R . .
C35 C -0.1028(7) 0.6293(2) 0.24782(11) 0.0666(15) Uani 1 1 d . . .
H35 H -0.1899 0.6304 0.2330 0.080 Uiso 1 1 calc R . .
C10 C 0.2231(7) 0.6755(2) 0.46346(10) 0.0662(15) Uani 1 1 d . . .
H10A H 0.0935 0.6704 0.4642 0.079 Uiso 1 1 calc R . .
C14 C 0.4816(7) 0.7033(2) 0.44012(11) 0.0717(16) Uani 1 1 d . . .
H14 H 0.5323 0.7175 0.4247 0.086 Uiso 1 1 calc R . .
C31 C 0.0057(8) 0.5928(2) 0.28916(11) 0.0720(16) Uani 1 1 d . . .
H31 H -0.0090 0.5698 0.3032 0.086 Uiso 1 1 calc R . .
C8 C 0.1660(8) 0.7086(2) 0.41856(11) 0.0707(16) Uani 1 1 d . . .
C83 C 0.1806(7) 0.4140(2) 0.03000(11) 0.0714(16) Uani 1 1 d . . .
H83 H 0.2746 0.4215 0.0433 0.086 Uiso 1 1 calc R . .
C29 C -0.2978(8) 0.5669(2) 0.26802(14) 0.0753(17) Uani 1 1 d . . .
C57 C 1.2454(8) 0.4960(2) 0.26663(14) 0.0744(16) Uani 1 1 d . . .
C15 C 1.2676(8) 0.5333(2) 0.50181(14) 0.0718(16) Uani 1 1 d . . .
C78 C -0.2746(9) 0.4642(2) 0.00419(15) 0.0798(18) Uani 1 1 d . . .
H105 H 0.197(13) 0.684(4) 0.638(2) 0.21(4) Uiso 1 1 d . . .


_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
O21 C71 1.284(7) . ?
O7 C22 1.274(7) . ?
O11 C36 1.263(6) . ?
O11 H119 0.8400 . ?
O3 C8 1.264(6) . ?
O15 C50 1.265(6) . ?
O15 H15 0.8400 . ?
O6 C15 1.238(7) . ?
N1 C19 1.394(6) . ?
N1 C12 1.426(6) . ?
N1 C5 1.428(6) . ?
N3 C61 1.395(6) . ?
N3 C54 1.413(6) . ?
N3 C47 1.419(6) . ?
O4 C8 1.267(6) . ?
O4 H117 0.8400 . ?
N4 C82 1.392(6) . ?
N4 C68 1.409(6) . ?
N4 C75 1.425(6) . ?
O12 C36 1.256(6) . ?
O8 C22 1.261(7) . ?
O8 H8 0.8400 . ?
O20 C64 1.265(6) . ?
O20 H121 0.8400 . ?
O18 C57 1.298(7) . ?
O18 H18 0.8400 . ?
N2 C33 1.397(6) . ?
N2 C40 1.414(6) . ?
N2 C26 1.444(6) . ?
O1 C1 1.263(7) . ?
O1 H105 1.09(10) . ?
O13 C43 1.284(7) . ?
O13 H13 0.8400 . ?
O22 C71 1.253(7) . ?
O22 H22 0.8400 . ?
O19 C64 1.265(6) . ?
O16 C50 1.261(6) . ?
O17 C57 1.224(7) . ?
O9 C29 1.220(7) . ?
O2 C1 1.269(7) . ?
O5 C15 1.292(6) . ?
O5 H5 0.8400 . ?
O14 C43 1.256(7) . ?
O10 C29 1.304(7) . ?
O10 H10 0.8400 . ?
O24 C78 1.218(7) . ?
O23 C78 1.303(7) . ?
O23 H23 0.8400 . ?
C26 C25 1.380(7) . ?
C26 C27 1.384(7) . ?
C12 C11 1.369(6) . ?
C12 C13 1.389(7) . ?
C68 C67 1.376(7) . ?
C68 C69 1.395(7) . ?
C33 C34 1.387(6) . ?
C33 C32 1.400(7) . ?
C47 C48 1.376(7) . ?
C47 C46 1.397(7) . ?
C40 C41 1.374(7) . ?
C40 C39 1.376(7) . ?
C75 C76 1.377(7) . ?
C75 C74 1.392(7) . ?
C61 C62 1.394(6) . ?
C61 C59 1.398(7) . ?
C5 C4 1.382(7) . ?
C5 C6 1.383(7) . ?
C51 C52 1.373(7) . ?
C51 C56 1.376(7) . ?
C51 C50 1.492(7) . ?
C58 C63 1.370(7) . ?
C58 C60 1.389(7) . ?
C58 C57 1.466(7) . ?
C19 C18 1.393(6) . ?
C19 C20 1.400(7) . ?
C23 C24 1.373(7) . ?
C23 C28 1.388(7) . ?
C23 C22 1.463(7) . ?
C72 C77 1.365(7) . ?
C72 C73 1.385(7) . ?
C72 C71 1.465(7) . ?
C54 C55 1.373(7) . ?
C54 C53 1.373(7) . ?
C9 C14 1.377(7) . ?
C9 C10 1.385(7) . ?
C9 C8 1.449(7) . ?
C39 C38 1.354(7) . ?
C39 H39 0.9500 . ?
C82 C81 1.398(7) . ?
C82 C83 1.399(7) . ?
C18 C17 1.376(7) . ?
C18 H18A 0.9500 . ?
C65 C70 1.374(7) . ?
C65 C66 1.383(7) . ?
C65 C64 1.464(7) . ?
C62 C63 1.379(7) . ?
C62 H62 0.9500 . ?
C55 C56 1.384(7) . ?
C55 H55 0.9500 . ?
C37 C42 1.378(7) . ?
C37 C38 1.388(7) . ?
C37 C36 1.464(7) . ?
C43 C44 1.487(8) . ?
C69 C70 1.387(7) . ?
C69 H69 0.9500 . ?
C34 C35 1.381(7) . ?
C34 H34 0.9500 . ?
C28 C27 1.380(7) . ?
C28 H28 0.9500 . ?
C63 H63 0.9500 . ?
C81 C80 1.359(7) . ?
C81 H81 0.9500 . ?
C30 C31 1.377(7) . ?
C30 C35 1.398(7) . ?
C30 C29 1.460(7) . ?
C56 H56 0.9500 . ?
C27 H27 0.9500 . ?
C11 C10 1.378(7) . ?
C11 H118 0.9500 . ?
C25 C24 1.381(7) . ?
C25 H25 0.9500 . ?
C1 C2 1.473(8) . ?
C38 H38 0.9500 . ?
C2 C7 1.367(7) . ?
C2 C3 1.388(7) . ?
C46 C45 1.371(7) . ?
C46 H46 0.9500 . ?
C44 C45 1.373(7) . ?
C44 C49 1.386(7) . ?
C13 C14 1.381(7) . ?
C13 H13A 0.9500 . ?
C41 C42 1.389(7) . ?
C41 H41 0.9500 . ?
C24 H24 0.9500 . ?
C77 C76 1.376(7) . ?
C77 H77 0.9500 . ?
C4 C3 1.375(7) . ?
C4 H116 0.9500 . ?
C49 C48 1.380(7) . ?
C49 H49 0.9500 . ?
C20 C21 1.379(7) . ?
C20 H120 0.9500 . ?
C74 C73 1.396(7) . ?
C74 H74 0.9500 . ?
C59 C60 1.391(7) . ?
C59 H59 0.9500 . ?
C42 H42 0.9500 . ?
C67 C66 1.377(7) . ?
C67 H67 0.9500 . ?
C16 C17 1.380(7) . ?
C16 C21 1.393(7) . ?
C16 C15 1.468(7) . ?
C70 H70 0.9500 . ?
C32 C31 1.382(7) . ?
C32 H32 0.9500 . ?
C76 H76 0.9500 . ?
C73 H73 0.9500 . ?
C66 H66 0.9500 . ?
C48 H48 0.9500 . ?
C3 H3 0.9500 . ?
C17 H17 0.9500 . ?
C7 C6 1.387(7) . ?
C7 H7 0.9500 . ?
C52 C53 1.386(7) . ?
C52 H52 0.9500 . ?
C60 H60 0.9500 . ?
C6 H6 0.9500 . ?
C79 C80 1.392(7) . ?
C79 C84 1.392(7) . ?
C79 C78 1.460(8) . ?
C80 H80 0.9500 . ?
C53 H53 0.9500 . ?
C84 C83 1.367(7) . ?
C84 H84 0.9500 . ?
C21 H21A 0.9500 . ?
C45 H45 0.9500 . ?
C35 H35 0.9500 . ?
C10 H10A 0.9500 . ?
C14 H14 0.9500 . ?
C31 H31 0.9500 . ?
C83 H83 0.9500 . ?

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
C36 O11 H119 109.5 . . ?
C50 O15 H15 109.5 . . ?
C19 N1 C12 122.3(4) . . ?
C19 N1 C5 121.2(4) . . ?
C12 N1 C5 114.9(4) . . ?
C61 N3 C54 121.1(4) . . ?
C61 N3 C47 120.9(4) . . ?
C54 N3 C47 116.6(4) . . ?
C8 O4 H117 109.5 . . ?
C82 N4 C68 122.7(4) . . ?
C82 N4 C75 118.0(4) . . ?
C68 N4 C75 118.6(4) . . ?
C22 O8 H8 109.5 . . ?
C64 O20 H121 109.5 . . ?
C57 O18 H18 109.5 . . ?
C33 N2 C40 123.5(4) . . ?
C33 N2 C26 118.6(4) . . ?
C40 N2 C26 116.9(4) . . ?
C1 O1 H105 122(5) . . ?
C43 O13 H13 109.5 . . ?
C71 O22 H22 109.5 . . ?
C15 O5 H5 109.5 . . ?
C29 O10 H10 109.5 . . ?
C78 O23 H23 109.5 . . ?
C25 C26 C27 120.5(5) . . ?
C25 C26 N2 119.5(5) . . ?
C27 C26 N2 120.0(5) . . ?
C11 C12 C13 119.0(5) . . ?
C11 C12 N1 118.1(4) . . ?
C13 C12 N1 123.0(4) . . ?
C67 C68 C69 119.0(5) . . ?
C67 C68 N4 122.8(4) . . ?
C69 C68 N4 118.1(4) . . ?
C34 C33 N2 118.9(5) . . ?
C34 C33 C32 118.7(5) . . ?
N2 C33 C32 122.3(4) . . ?
C48 C47 C46 119.4(5) . . ?
C48 C47 N3 121.7(5) . . ?
C46 C47 N3 118.9(5) . . ?
C41 C40 C39 118.7(5) . . ?
C41 C40 N2 122.0(4) . . ?
C39 C40 N2 119.2(4) . . ?
C76 C75 C74 119.0(5) . . ?
C76 C75 N4 120.8(5) . . ?
C74 C75 N4 120.2(5) . . ?
C62 C61 N3 119.5(5) . . ?
C62 C61 C59 118.7(5) . . ?
N3 C61 C59 121.7(5) . . ?
C4 C5 C6 119.4(5) . . ?
C4 C5 N1 122.3(5) . . ?
C6 C5 N1 118.3(5) . . ?
C52 C51 C56 119.1(5) . . ?
C52 C51 C50 120.9(5) . . ?
C56 C51 C50 119.9(5) . . ?
C63 C58 C60 118.2(5) . . ?
C63 C58 C57 120.1(5) . . ?
C60 C58 C57 121.6(5) . . ?
C18 C19 N1 120.2(5) . . ?
C18 C19 C20 118.1(5) . . ?
N1 C19 C20 121.7(4) . . ?
C24 C23 C28 118.8(5) . . ?
C24 C23 C22 121.2(6) . . ?
C28 C23 C22 120.0(6) . . ?
C77 C72 C73 118.4(5) . . ?
C77 C72 C71 123.3(6) . . ?
C73 C72 C71 118.3(6) . . ?
C55 C54 C53 119.0(5) . . ?
C55 C54 N3 117.4(5) . . ?
C53 C54 N3 123.6(5) . . ?
C14 C9 C10 118.6(5) . . ?
C14 C9 C8 122.9(5) . . ?
C10 C9 C8 118.5(5) . . ?
C38 C39 C40 121.0(5) . . ?
C38 C39 H39 119.5 . . ?
C40 C39 H39 119.5 . . ?
N4 C82 C81 119.0(5) . . ?
N4 C82 C83 123.7(5) . . ?
C81 C82 C83 117.2(5) . . ?
C17 C18 C19 121.0(5) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C70 C65 C66 118.7(5) . . ?
C70 C65 C64 120.2(5) . . ?
C66 C65 C64 121.1(5) . . ?
C63 C62 C61 119.8(5) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C54 C55 C56 120.0(5) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C42 C37 C38 118.7(5) . . ?
C42 C37 C36 121.4(5) . . ?
C38 C37 C36 119.8(5) . . ?
O14 C43 O13 123.3(6) . . ?
O14 C43 C44 119.9(6) . . ?
O13 C43 C44 116.8(7) . . ?
C70 C69 C68 119.2(5) . . ?
C70 C69 H69 120.4 . . ?
C68 C69 H69 120.4 . . ?
C35 C34 C33 120.7(5) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C27 C28 C23 120.8(5) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
C58 C63 C62 122.3(5) . . ?
C58 C63 H63 118.8 . . ?
C62 C63 H63 118.8 . . ?
C80 C81 C82 121.0(5) . . ?
C80 C81 H81 119.5 . . ?
C82 C81 H81 119.5 . . ?
C31 C30 C35 119.0(5) . . ?
C31 C30 C29 122.9(6) . . ?
C35 C30 C29 118.1(5) . . ?
C51 C56 C55 121.0(5) . . ?
C51 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?
C28 C27 C26 119.4(5) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 H118 119.7 . . ?
C10 C11 H118 119.7 . . ?
C26 C25 C24 119.2(5) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
O1 C1 O2 122.8(6) . . ?
O1 C1 C2 118.6(7) . . ?
O2 C1 C2 118.6(6) . . ?
C39 C38 C37 121.0(5) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C7 C2 C3 119.6(5) . . ?
C7 C2 C1 120.4(6) . . ?
C3 C2 C1 120.1(6) . . ?
C45 C46 C47 119.7(5) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
C45 C44 C49 120.5(5) . . ?
C45 C44 C43 119.1(6) . . ?
C49 C44 C43 120.4(6) . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C40 C41 C42 120.9(5) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
O22 C71 O21 123.4(5) . . ?
O22 C71 C72 118.7(6) . . ?
O21 C71 C72 117.9(6) . . ?
C23 C24 C25 121.4(5) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C72 C77 C76 122.0(5) . . ?
C72 C77 H77 119.0 . . ?
C76 C77 H77 119.0 . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H116 119.8 . . ?
C5 C4 H116 119.8 . . ?
C48 C49 C44 119.0(5) . . ?
C48 C49 H49 120.5 . . ?
C44 C49 H49 120.5 . . ?
C21 C20 C19 120.4(5) . . ?
C21 C20 H120 119.8 . . ?
C19 C20 H120 119.8 . . ?
C75 C74 C73 119.8(5) . . ?
C75 C74 H74 120.1 . . ?
C73 C74 H74 120.1 . . ?
C60 C59 C61 120.0(5) . . ?
C60 C59 H59 120.0 . . ?
C61 C59 H59 120.0 . . ?
C37 C42 C41 119.7(5) . . ?
C37 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C68 C67 C66 121.0(5) . . ?
C68 C67 H67 119.5 . . ?
C66 C67 H67 119.5 . . ?
O8 C22 O7 123.3(6) . . ?
O8 C22 C23 117.7(6) . . ?
O7 C22 C23 119.0(6) . . ?
C17 C16 C21 118.5(5) . . ?
C17 C16 C15 119.6(5) . . ?
C21 C16 C15 121.7(5) . . ?
C65 C70 C69 121.5(5) . . ?
C65 C70 H70 119.3 . . ?
C69 C70 H70 119.3 . . ?
C31 C32 C33 120.2(5) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C77 C76 C75 120.2(5) . . ?
C77 C76 H76 119.9 . . ?
C75 C76 H76 119.9 . . ?
C72 C73 C74 120.5(5) . . ?
C72 C73 H73 119.7 . . ?
C74 C73 H73 119.7 . . ?
C67 C66 C65 120.4(5) . . ?
C67 C66 H66 119.8 . . ?
C65 C66 H66 119.8 . . ?
O19 C64 O20 123.5(5) . . ?
O19 C64 C65 119.4(5) . . ?
O20 C64 C65 117.1(5) . . ?
O12 C36 O11 123.2(5) . . ?
O12 C36 C37 118.8(5) . . ?
O11 C36 C37 118.0(5) . . ?
O16 C50 O15 124.1(5) . . ?
O16 C50 C51 120.8(5) . . ?
O15 C50 C51 115.1(5) . . ?
C47 C48 C49 120.9(6) . . ?
C47 C48 H48 119.5 . . ?
C49 C48 H48 119.5 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C18 C17 C16 120.9(5) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C2 C7 C6 120.5(5) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C51 C52 C53 119.7(5) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
C58 C60 C59 120.9(5) . . ?
C58 C60 H60 119.6 . . ?
C59 C60 H60 119.6 . . ?
C5 C6 C7 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C80 C79 C84 119.0(5) . . ?
C80 C79 C78 118.8(6) . . ?
C84 C79 C78 122.1(6) . . ?
C81 C80 C79 121.0(5) . . ?
C81 C80 H80 119.5 . . ?
C79 C80 H80 119.5 . . ?
C54 C53 C52 121.2(5) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C83 C84 C79 119.5(5) . . ?
C83 C84 H84 120.3 . . ?
C79 C84 H84 120.3 . . ?
C20 C21 C16 121.0(5) . . ?
C20 C21 H21A 119.5 . . ?
C16 C21 H21A 119.5 . . ?
C46 C45 C44 120.5(6) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C34 C35 C30 120.3(5) . . ?
C34 C35 H35 119.8 . . ?
C30 C35 H35 119.8 . . ?
C11 C10 C9 120.9(5) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C9 C14 C13 120.4(5) . . ?
C9 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C30 C31 C32 120.9(5) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
O3 C8 O4 122.5(5) . . ?
O3 C8 C9 117.9(5) . . ?
O4 C8 C9 119.6(5) . . ?
C84 C83 C82 122.1(5) . . ?
C84 C83 H83 119.0 . . ?
C82 C83 H83 119.0 . . ?
O9 C29 O10 122.5(5) . . ?
O9 C29 C30 121.7(6) . . ?
O10 C29 C30 115.7(6) . . ?
O17 C57 O18 123.0(5) . . ?
O17 C57 C58 121.0(6) . . ?
O18 C57 C58 116.1(6) . . ?
O6 C15 O5 123.4(5) . . ?
O6 C15 C16 120.1(6) . . ?
O5 C15 C16 116.5(6) . . ?
O24 C78 O23 123.2(6) . . ?
O24 C78 C79 121.4(6) . . ?
O23 C78 C79 115.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        61.50
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1472885'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            TCA
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 N4 O24'
_chemical_formula_sum            'C84 H60 N4 O24'
_chemical_formula_weight         1509.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   7.2350(9)
_cell_length_b                   27.116(4)
_cell_length_c                   50.042(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.752(6)
_cell_angle_gamma                90.00
_cell_volume                     9806(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      61.5

_exptl_crystal_description       'niddle shaped'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  Micro-focus
_diffrn_measurement_device_type  'D8 Venture APEX-II'
_diffrn_measurement_method       'CMOS-Photon 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            158928
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         61.50
_reflns_number_total             14569
_reflns_number_gt                8271
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS)'
_computing_cell_refinement       'SHELXTL suite'
_computing_data_reduction        'SHELXTL suite'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  'Mercury 3.1'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14569
_refine_ls_number_parameters     1013
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.1218
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.802
_refine_ls_restrained_S_all      1.802
_refine_ls_shift/su_max          0.002
_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
O21 O 0.6122(3) 0.21049(9) -0.08296(4) 0.0723(8) Uani 1 1 d . . .
O7 O 0.6185(3) 0.79793(10) 0.16537(5) 0.0713(8) Uani 1 1 d . . .
O11 O 0.7595(3) 0.71726(9) 0.38214(4) 0.0853(8) Uani 1 1 d . . .
H119 H 0.8464 0.7206 0.3937 0.128 Uiso 1 1 calc R . .
O3 O -0.0068(3) 0.70562(9) 0.42228(4) 0.0844(8) Uani 1 1 d . . .
O15 O -0.0061(4) 0.34219(9) 0.17233(4) 0.0920(9) Uani 1 1 d . . .
H15 H -0.0663 0.3374 0.1578 0.138 Uiso 1 1 calc R . .
O6 O 1.3737(3) 0.52843(9) 0.52189(5) 0.0858(9) Uani 1 1 d . . .
N1 N 0.6376(4) 0.65575(10) 0.50731(5) 0.0530(8) Uani 1 1 d . . .
N3 N 0.6206(4) 0.37051(10) 0.26259(5) 0.0567(8) Uani 1 1 d . . .
O4 O 0.2292(3) 0.72163(9) 0.39670(5) 0.0868(8) Uani 1 1 d . . .
H117 H 0.1413 0.7276 0.3856 0.130 Uiso 1 1 calc R . .
N4 N 0.3572(4) 0.34210(10) 0.01516(5) 0.0560(8) Uani 1 1 d . . .
O12 O 0.9924(3) 0.72486(10) 0.35514(4) 0.0874(8) Uani 1 1 d . . .
O8 O 0.6594(3) 0.71857(10) 0.15442(5) 0.0936(9) Uani 1 1 d . . .
H8 H 0.6994 0.7316 0.1406 0.140 Uiso 1 1 calc R . .
O20 O 1.0005(3) 0.32473(9) 0.10455(4) 0.0933(9) Uani 1 1 d . . .
H121 H 1.0585 0.3246 0.1195 0.140 Uiso 1 1 calc R . .
O18 O 1.2764(3) 0.52079(9) 0.24484(5) 0.0927(9) Uani 1 1 d . . .
H18 H 1.3764 0.5363 0.2471 0.139 Uiso 1 1 calc R . .
N2 N 0.3341(4) 0.68903(10) 0.26904(5) 0.0536(8) Uani 1 1 d . . .
O1 O 0.2685(4) 0.67619(11) 0.62015(6) 0.0870(9) Uani 1 1 d . . .
O13 O 0.2579(3) 0.32535(10) 0.37345(5) 0.0887(9) Uani 1 1 d . . .
H13 H 0.2131 0.3104 0.3863 0.133 Uiso 1 1 calc R . .
O22 O 0.6607(3) 0.28734(9) -0.09809(5) 0.0912(9) Uani 1 1 d . . .
H22 H 0.6967 0.2718 -0.1114 0.137 Uiso 1 1 calc R . .
O19 O 0.7633(3) 0.33425(9) 0.13099(4) 0.0877(8) Uani 1 1 d . . .
O16 O 0.2307(3) 0.32683(9) 0.14669(4) 0.0892(9) Uani 1 1 d . . .
O17 O 1.3515(3) 0.49609(9) 0.28648(5) 0.0887(9) Uani 1 1 d . . .
O9 O -0.4072(4) 0.56716(9) 0.24848(5) 0.0947(9) Uani 1 1 d . . .
O2 O 0.2854(4) 0.75597(11) 0.60845(5) 0.0903(10) Uani 1 1 d . . .
O5 O 1.3006(3) 0.51503(8) 0.47857(5) 0.0900(9) Uani 1 1 d . . .
H5 H 1.4018 0.4998 0.4794 0.135 Uiso 1 1 calc R . .
O14 O 0.2856(4) 0.24810(11) 0.35779(5) 0.0926(10) Uani 1 1 d . . .
O10 O -0.3238(3) 0.54065(9) 0.28948(5) 0.0941(9) Uani 1 1 d . . .
H10 H -0.4239 0.5251 0.2876 0.141 Uiso 1 1 calc R . .
O24 O -0.3845(4) 0.45864(10) -0.01513(6) 0.1028(10) Uani 1 1 d . . .
O23 O -0.3001(3) 0.49574(10) 0.02320(5) 0.1027(9) Uani 1 1 d . . .
H23 H -0.3997 0.5111 0.0201 0.154 Uiso 1 1 calc R . .
C26 C 0.3980(4) 0.70512(16) 0.24350(7) 0.0512(9) Uani 1 1 d . . .
C12 C 0.5248(5) 0.66949(12) 0.48423(6) 0.0503(9) Uani 1 1 d . . .
C68 C 0.4714(5) 0.33696(12) 0.03874(7) 0.0528(9) Uani 1 1 d . . .
C33 C 0.1818(5) 0.65764(13) 0.26930(7) 0.0528(9) Uani 1 1 d . . .
C47 C 0.5453(4) 0.35181(16) 0.28661(7) 0.0509(9) Uani 1 1 d . . .
C40 C 0.4521(5) 0.69908(11) 0.29177(7) 0.0516(9) Uani 1 1 d . . .
C75 C 0.4172(4) 0.32154(15) -0.00889(7) 0.0527(10) Uani 1 1 d . . .
C61 C 0.7674(5) 0.40379(13) 0.26345(7) 0.0526(9) Uani 1 1 d . . .
C5 C 0.5622(4) 0.66827(16) 0.53247(7) 0.0521(9) Uani 1 1 d . . .
C51 C 0.2885(5) 0.34496(12) 0.19300(7) 0.0564(10) Uani 1 1 d . . .
C58 C 1.0738(5) 0.46690(13) 0.26561(7) 0.0573(10) Uani 1 1 d . . .
C19 C 0.7862(5) 0.62270(12) 0.50617(7) 0.0502(9) Uani 1 1 d . . .
C23 C 0.5348(4) 0.73571(16) 0.19575(7) 0.0512(10) Uani 1 1 d . . .
C72 C 0.5411(4) 0.27893(16) -0.05558(7) 0.0527(9) Uani 1 1 d . . .
C54 C 0.5127(5) 0.36195(12) 0.23872(7) 0.0518(9) Uani 1 1 d . . .
C9 C 0.2938(5) 0.69637(12) 0.44074(7) 0.0572(10) Uani 1 1 d . . .
C39 C 0.6395(5) 0.70283(12) 0.28899(6) 0.0612(10) Uani 1 1 d . . .
H39 H 0.6879 0.6998 0.2718 0.073 Uiso 1 1 calc R . .
C82 C 0.2030(5) 0.37306(14) 0.01317(7) 0.0566(10) Uani 1 1 d . . .
C18 C 0.9076(5) 0.61603(12) 0.52841(6) 0.0535(9) Uani 1 1 d . . .
H18A H 0.8856 0.6326 0.5447 0.064 Uiso 1 1 calc R . .
C65 C 0.7041(5) 0.33091(12) 0.08425(7) 0.0581(10) Uani 1 1 d . . .
C62 C 0.8887(5) 0.40458(11) 0.28608(6) 0.0532(9) Uani 1 1 d . . .
H62 H 0.8677 0.3835 0.3008 0.064 Uiso 1 1 calc R . .
C55 C 0.3260(5) 0.36929(12) 0.23913(6) 0.0605(10) Uani 1 1 d . . .
H55 H 0.2726 0.3799 0.2551 0.073 Uiso 1 1 calc R . .
C37 C 0.6907(5) 0.71496(12) 0.33629(7) 0.0590(10) Uani 1 1 d . . .
C43 C 0.3056(5) 0.2939(2) 0.35577(8) 0.0708(13) Uani 1 1 d . . .
C69 C 0.6608(5) 0.33282(12) 0.03648(6) 0.0613(10) Uani 1 1 d . . .
H69 H 0.7116 0.3327 0.0193 0.074 Uiso 1 1 calc R . .
C34 C 0.0478(5) 0.66037(13) 0.24855(6) 0.0597(10) Uani 1 1 d . . .
H34 H 0.0603 0.6839 0.2347 0.072 Uiso 1 1 calc R . .
C28 C 0.4948(4) 0.68661(15) 0.19945(7) 0.0621(10) Uani 1 1 d . . .
H28 H 0.5147 0.6634 0.1857 0.074 Uiso 1 1 calc R . .
C63 C 1.0382(4) 0.43596(13) 0.28698(7) 0.0596(10) Uani 1 1 d . . .
H63 H 1.1190 0.4365 0.3025 0.072 Uiso 1 1 calc R . .
C81 C 0.0685(5) 0.36468(13) -0.00718(6) 0.0668(11) Uani 1 1 d . . .
H81 H 0.0809 0.3376 -0.0190 0.080 Uiso 1 1 calc R . .
C30 C -0.1276(5) 0.59618(14) 0.26869(8) 0.0611(10) Uani 1 1 d . . .
C56 C 0.2146(5) 0.36131(12) 0.21630(7) 0.0663(11) Uani 1 1 d . . .
H56 H 0.0853 0.3672 0.2167 0.080 Uiso 1 1 calc R . .
C27 C 0.4249(4) 0.67112(12) 0.22352(8) 0.0574(10) Uani 1 1 d . . .
H27 H 0.3959 0.6374 0.2262 0.069 Uiso 1 1 calc R . .
C11 C 0.3377(5) 0.66229(11) 0.48485(6) 0.0589(10) Uani 1 1 d . . .
H118 H 0.2870 0.6480 0.5002 0.071 Uiso 1 1 calc R . .
C25 C 0.4366(4) 0.75396(14) 0.23964(7) 0.0583(10) Uani 1 1 d . . .
H25 H 0.4174 0.7773 0.2534 0.070 Uiso 1 1 calc R . .
C1 C 0.3116(5) 0.7108(2) 0.60442(8) 0.0717(14) Uani 1 1 d . . .
C38 C 0.7568(5) 0.71079(12) 0.31071(7) 0.0666(11) Uani 1 1 d . . .
H38 H 0.8859 0.7135 0.3083 0.080 Uiso 1 1 calc R . .
C2 C 0.3993(5) 0.69529(17) 0.57946(7) 0.0595(10) Uani 1 1 d . . .
C46 C 0.5091(4) 0.30152(15) 0.28851(7) 0.0606(10) Uani 1 1 d . . .
H46 H 0.5380 0.2798 0.2744 0.073 Uiso 1 1 calc R . .
C44 C 0.3889(4) 0.31495(17) 0.33147(7) 0.0572(10) Uani 1 1 d . . .
C13 C 0.5971(5) 0.69036(12) 0.46162(7) 0.0651(11) Uani 1 1 d . . .
H13A H 0.7266 0.6955 0.4610 0.078 Uiso 1 1 calc R . .
C41 C 0.3839(5) 0.70571(11) 0.31704(7) 0.0627(10) Uani 1 1 d . . .
H41 H 0.2541 0.7053 0.3191 0.075 Uiso 1 1 calc R . .
C71 C 0.6090(5) 0.25719(18) -0.08075(8) 0.0630(11) Uani 1 1 d . . .
C24 C 0.5040(4) 0.76914(13) 0.21544(8) 0.0626(10) Uani 1 1 d . . .
H24 H 0.5289 0.8031 0.2126 0.075 Uiso 1 1 calc R . .
C77 C 0.5099(4) 0.25065(13) -0.03350(8) 0.0624(10) Uani 1 1 d . . .
H77 H 0.5302 0.2161 -0.0341 0.075 Uiso 1 1 calc R . .
C4 C 0.5250(4) 0.63282(13) 0.55148(8) 0.0624(10) Uani 1 1 d . . .
H116 H 0.5558 0.5993 0.5485 0.075 Uiso 1 1 calc R . .
C49 C 0.4258(4) 0.36497(15) 0.32995(6) 0.0632(11) Uani 1 1 d . . .
H49 H 0.3976 0.3864 0.3442 0.076 Uiso 1 1 calc R . .
C20 C 0.8174(5) 0.59622(12) 0.48257(6) 0.0604(10) Uani 1 1 d . . .
H120 H 0.7324 0.5987 0.4676 0.073 Uiso 1 1 calc R . .
C74 C 0.4469(4) 0.34992(13) -0.03115(8) 0.0622(10) Uani 1 1 d . . .
H74 H 0.4238 0.3844 -0.0305 0.075 Uiso 1 1 calc R . .
C59 C 0.7996(5) 0.43594(13) 0.24242(6) 0.0650(11) Uani 1 1 d . . .
H59 H 0.7160 0.4367 0.2272 0.078 Uiso 1 1 calc R . .
C42 C 0.5019(5) 0.71290(12) 0.33917(7) 0.0649(11) Uani 1 1 d . . .
H42 H 0.4535 0.7164 0.3564 0.078 Uiso 1 1 calc R . .
C67 C 0.3988(5) 0.33659(12) 0.06380(7) 0.0659(11) Uani 1 1 d . . .
H67 H 0.2686 0.3382 0.0655 0.079 Uiso 1 1 calc R . .
C22 C 0.6089(5) 0.75182(19) 0.17017(8) 0.0677(12) Uani 1 1 d . . .
C16 C 1.0951(5) 0.56103(12) 0.50333(8) 0.0579(10) Uani 1 1 d . . .
C70 C 0.7744(5) 0.32893(12) 0.05898(7) 0.0644(10) Uani 1 1 d . . .
H70 H 0.9037 0.3248 0.0573 0.077 Uiso 1 1 calc R . .
C32 C 0.1606(5) 0.62273(13) 0.28957(6) 0.0609(10) Uani 1 1 d . . .
H32 H 0.2527 0.6195 0.3036 0.073 Uiso 1 1 calc R . .
C76 C 0.4488(4) 0.27202(16) -0.01016(7) 0.0637(11) Uani 1 1 d . . .
H76 H 0.4289 0.2519 0.0050 0.076 Uiso 1 1 calc R . .
C73 C 0.5100(4) 0.32923(16) -0.05448(7) 0.0645(10) Uani 1 1 d . . .
H73 H 0.5314 0.3495 -0.0695 0.077 Uiso 1 1 calc R . .
C66 C 0.5156(5) 0.33388(12) 0.08642(6) 0.0658(11) Uani 1 1 d . . .
H66 H 0.4654 0.3341 0.1036 0.079 Uiso 1 1 calc R . .
C64 C 0.8279(6) 0.32957(14) 0.10793(8) 0.0734(12) Uani 1 1 d . . .
C36 C 0.8228(6) 0.71987(14) 0.35900(7) 0.0670(11) Uani 1 1 d . . .
C50 C 0.1657(5) 0.33720(14) 0.16881(8) 0.0701(12) Uani 1 1 d . . .
C48 C 0.5050(4) 0.38337(13) 0.30716(7) 0.0623(10) Uani 1 1 d . . .
H48 H 0.5313 0.4176 0.3058 0.075 Uiso 1 1 calc R . .
C3 C 0.4432(4) 0.64634(16) 0.57477(7) 0.0644(11) Uani 1 1 d . . .
H3 H 0.4169 0.6219 0.5877 0.077 Uiso 1 1 calc R . .
C17 C 1.0594(4) 0.58547(12) 0.52688(7) 0.0577(10) Uani 1 1 d . . .
H17 H 1.1406 0.5811 0.5422 0.069 Uiso 1 1 calc R . .
C7 C 0.4360(4) 0.73018(14) 0.56027(8) 0.0629(10) Uani 1 1 d . . .
H7 H 0.4046 0.7637 0.5633 0.075 Uiso 1 1 calc R . .
C52 C 0.4756(5) 0.33767(12) 0.19265(7) 0.0695(11) Uani 1 1 d . . .
H52 H 0.5291 0.3270 0.1767 0.083 Uiso 1 1 calc R . .
C60 C 0.9524(5) 0.46683(13) 0.24351(7) 0.0673(11) Uani 1 1 d . . .
H60 H 0.9737 0.4881 0.2289 0.081 Uiso 1 1 calc R . .
C6 C 0.5179(4) 0.71737(15) 0.53662(7) 0.0591(10) Uani 1 1 d . . .
H6 H 0.5429 0.7417 0.5236 0.071 Uiso 1 1 calc R . .
C79 C -0.1055(5) 0.43428(14) 0.00716(7) 0.0615(10) Uani 1 1 d . . .
C80 C -0.0802(5) 0.39508(14) -0.01012(7) 0.0689(11) Uani 1 1 d . . .
H80 H -0.1692 0.3894 -0.0244 0.083 Uiso 1 1 calc R . .
C53 C 0.5868(5) 0.34575(12) 0.21545(7) 0.0691(11) Uani 1 1 d . . .
H53 H 0.7163 0.3401 0.2151 0.083 Uiso 1 1 calc R . .
C84 C 0.0279(5) 0.44308(13) 0.02776(7) 0.0738(11) Uani 1 1 d . . .
H84 H 0.0119 0.4692 0.0401 0.089 Uiso 1 1 calc R . .
C21 C 0.9719(5) 0.56673(12) 0.48143(7) 0.0630(10) Uani 1 1 d . . .
H21A H 0.9947 0.5499 0.4653 0.076 Uiso 1 1 calc R . .
C45 C 0.4309(4) 0.28357(13) 0.31112(8) 0.0645(11) Uani 1 1 d . . .
H45 H 0.4061 0.2493 0.3126 0.077 Uiso 1 1 calc R . .
C35 C -0.1024(5) 0.62945(13) 0.24781(7) 0.0606(10) Uani 1 1 d . . .
H35 H -0.1899 0.6306 0.2330 0.073 Uiso 1 1 calc R . .
C10 C 0.2230(5) 0.67554(12) 0.46343(7) 0.0624(10) Uani 1 1 d . . .
H10A H 0.0934 0.6704 0.4641 0.075 Uiso 1 1 calc R . .
C14 C 0.4813(5) 0.70357(12) 0.44019(6) 0.0655(11) Uani 1 1 d . . .
H14 H 0.5319 0.7179 0.4248 0.079 Uiso 1 1 calc R . .
C31 C 0.0054(5) 0.59311(13) 0.28903(7) 0.0684(11) Uani 1 1 d . . .
H31 H -0.0096 0.5701 0.3031 0.082 Uiso 1 1 calc R . .
C8 C 0.1656(6) 0.70871(14) 0.41868(7) 0.0693(12) Uani 1 1 d . . .
C83 C 0.1817(5) 0.41367(13) 0.02995(6) 0.0672(11) Uani 1 1 d . . .
H83 H 0.2762 0.4210 0.0432 0.081 Uiso 1 1 calc R . .
C29 C -0.2991(6) 0.56708(14) 0.26794(9) 0.0700(12) Uani 1 1 d . . .
C57 C 1.2448(6) 0.49606(14) 0.26638(9) 0.0701(12) Uani 1 1 d . . .
C15 C 1.2688(6) 0.53326(14) 0.50208(9) 0.0677(11) Uani 1 1 d . . .
C78 C -0.2766(6) 0.46378(15) 0.00399(9) 0.0744(12) Uani 1 1 d . . .
H105 H 0.189(7) 0.6881(16) 0.6385(10) 0.21(2) Uiso 1 1 d . . .


_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
O21 C71 1.271(4) . ?
O7 C22 1.276(4) . ?
O11 C36 1.268(3) . ?
O11 H119 0.8400 . ?
O3 C8 1.271(4) . ?
O15 C50 1.271(4) . ?
O15 H15 0.8400 . ?
O6 C15 1.226(4) . ?
N1 C19 1.403(3) . ?
N1 C12 1.431(3) . ?
N1 C5 1.437(3) . ?
N3 C61 1.393(3) . ?
N3 C54 1.415(3) . ?
N3 C47 1.436(3) . ?
O4 C8 1.262(3) . ?
O4 H117 0.8400 . ?
N4 C82 1.396(4) . ?
N4 C68 1.414(3) . ?
N4 C75 1.413(4) . ?
O12 C36 1.259(4) . ?
O8 C22 1.263(4) . ?
O8 H8 0.8400 . ?
O20 C64 1.275(4) . ?
O20 H121 0.8400 . ?
O18 C57 1.299(4) . ?
O18 H18 0.8400 . ?
N2 C33 1.393(4) . ?
N2 C40 1.415(3) . ?
N2 C26 1.447(3) . ?
O1 C1 1.273(4) . ?
O1 H105 1.15(5) . ?
O13 C43 1.288(4) . ?
O13 H13 0.8400 . ?
O22 C71 1.262(4) . ?
O22 H22 0.8400 . ?
O19 C64 1.272(4) . ?
O16 C50 1.255(4) . ?
O17 C57 1.238(4) . ?
O9 C29 1.219(4) . ?
O2 C1 1.258(4) . ?
O5 C15 1.307(4) . ?
O5 H5 0.8400 . ?
O14 C43 1.255(4) . ?
O10 C29 1.314(4) . ?
O10 H10 0.8400 . ?
O24 C78 1.214(4) . ?
O23 C78 1.311(4) . ?
O23 H23 0.8400 . ?
C26 C25 1.369(4) . ?
C26 C27 1.381(4) . ?
C12 C11 1.370(4) . ?
C12 C13 1.389(4) . ?
C68 C67 1.383(4) . ?
C68 C69 1.385(4) . ?
C33 C34 1.388(4) . ?
C33 C32 1.401(4) . ?
C47 C48 1.380(4) . ?
C47 C46 1.393(4) . ?
C40 C39 1.373(4) . ?
C40 C41 1.391(4) . ?
C75 C76 1.364(4) . ?
C75 C74 1.379(4) . ?
C61 C59 1.394(4) . ?
C61 C62 1.399(4) . ?
C5 C4 1.388(4) . ?
C5 C6 1.387(4) . ?
C51 C52 1.369(4) . ?
C51 C56 1.379(4) . ?
C51 C50 1.482(4) . ?
C58 C63 1.393(4) . ?
C58 C60 1.379(4) . ?
C58 C57 1.467(4) . ?
C19 C18 1.396(4) . ?
C19 C20 1.409(4) . ?
C23 C24 1.365(4) . ?
C23 C28 1.377(4) . ?
C23 C22 1.477(5) . ?
C72 C77 1.372(4) . ?
C72 C73 1.384(4) . ?
C72 C71 1.495(4) . ?
C54 C55 1.366(4) . ?
C54 C53 1.377(4) . ?
C9 C14 1.372(4) . ?
C9 C10 1.388(4) . ?
C9 C8 1.446(4) . ?
C39 C38 1.364(4) . ?
C39 H39 0.9500 . ?
C82 C83 1.398(4) . ?
C82 C81 1.393(4) . ?
C18 C17 1.381(4) . ?
C18 H18A 0.9500 . ?
C65 C66 1.375(4) . ?
C65 C70 1.387(4) . ?
C65 C64 1.451(4) . ?
C62 C63 1.376(4) . ?
C62 H62 0.9500 . ?
C55 C56 1.383(4) . ?
C55 H55 0.9500 . ?
C37 C42 1.382(4) . ?
C37 C38 1.392(4) . ?
C37 C36 1.456(4) . ?
C43 C44 1.496(5) . ?
C69 C70 1.366(4) . ?
C69 H69 0.9500 . ?
C34 C35 1.372(4) . ?
C34 H34 0.9500 . ?
C28 C27 1.393(4) . ?
C28 H28 0.9500 . ?
C63 H63 0.9500 . ?
C81 C80 1.358(4) . ?
C81 H81 0.9500 . ?
C30 C31 1.369(4) . ?
C30 C35 1.399(4) . ?
C30 C29 1.470(5) . ?
C56 H56 0.9500 . ?
C27 H27 0.9500 . ?
C11 C10 1.372(4) . ?
C11 H118 0.9500 . ?
C25 C24 1.389(4) . ?
C25 H25 0.9500 . ?
C1 C2 1.489(5) . ?
C38 H38 0.9500 . ?
C2 C7 1.383(4) . ?
C2 C3 1.387(4) . ?
C46 C45 1.378(4) . ?
C46 H46 0.9500 . ?
C44 C45 1.372(4) . ?
C44 C49 1.385(4) . ?
C13 C14 1.376(4) . ?
C13 H13A 0.9500 . ?
C41 C42 1.380(4) . ?
C41 H41 0.9500 . ?
C24 H24 0.9500 . ?
C77 C76 1.395(4) . ?
C77 H77 0.9500 . ?
C4 C3 1.382(4) . ?
C4 H116 0.9500 . ?
C49 C48 1.393(4) . ?
C49 H49 0.9500 . ?
C20 C21 1.378(4) . ?
C20 H120 0.9500 . ?
C74 C73 1.392(4) . ?
C74 H74 0.9500 . ?
C59 C60 1.386(4) . ?
C59 H59 0.9500 . ?
C42 H42 0.9500 . ?
C67 C66 1.382(4) . ?
C67 H67 0.9500 . ?
C16 C17 1.387(4) . ?
C16 C21 1.388(4) . ?
C16 C15 1.469(4) . ?
C70 H70 0.9500 . ?
C32 C31 1.380(4) . ?
C32 H32 0.9500 . ?
C76 H76 0.9500 . ?
C73 H73 0.9500 . ?
C66 H66 0.9500 . ?
C48 H48 0.9500 . ?
C3 H3 0.9500 . ?
C17 H17 0.9500 . ?
C7 C6 1.393(4) . ?
C7 H7 0.9500 . ?
C52 C53 1.382(4) . ?
C52 H52 0.9500 . ?
C60 H60 0.9500 . ?
C6 H6 0.9500 . ?
C79 C84 1.398(4) . ?
C79 C80 1.388(4) . ?
C79 C78 1.476(5) . ?
C80 H80 0.9500 . ?
C53 H53 0.9500 . ?
C84 C83 1.369(4) . ?
C84 H84 0.9500 . ?
C21 H21A 0.9500 . ?
C45 H45 0.9500 . ?
C35 H35 0.9500 . ?
C10 H10A 0.9500 . ?
C14 H14 0.9500 . ?
C31 H31 0.9500 . ?
C83 H83 0.9500 . ?

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
C36 O11 H119 109.5 . . ?
C50 O15 H15 109.5 . . ?
C19 N1 C12 122.8(3) . . ?
C19 N1 C5 120.7(3) . . ?
C12 N1 C5 114.8(3) . . ?
C61 N3 C54 121.4(3) . . ?
C61 N3 C47 121.5(3) . . ?
C54 N3 C47 115.6(3) . . ?
C8 O4 H117 109.5 . . ?
C82 N4 C68 123.5(3) . . ?
C82 N4 C75 116.9(3) . . ?
C68 N4 C75 118.7(3) . . ?
C22 O8 H8 109.5 . . ?
C64 O20 H121 109.5 . . ?
C57 O18 H18 109.5 . . ?
C33 N2 C40 123.9(3) . . ?
C33 N2 C26 118.6(3) . . ?
C40 N2 C26 116.4(3) . . ?
C1 O1 H105 116(2) . . ?
C43 O13 H13 109.5 . . ?
C71 O22 H22 109.5 . . ?
C15 O5 H5 109.5 . . ?
C29 O10 H10 109.5 . . ?
C78 O23 H23 109.5 . . ?
C25 C26 C27 120.4(3) . . ?
C25 C26 N2 119.5(4) . . ?
C27 C26 N2 120.0(4) . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 N1 118.1(3) . . ?
C13 C12 N1 122.7(3) . . ?
C67 C68 C69 119.6(3) . . ?
C67 C68 N4 121.7(3) . . ?
C69 C68 N4 118.7(3) . . ?
C34 C33 N2 119.0(3) . . ?
C34 C33 C32 118.7(3) . . ?
N2 C33 C32 122.3(3) . . ?
C48 C47 C46 120.6(3) . . ?
C48 C47 N3 120.5(4) . . ?
C46 C47 N3 118.9(3) . . ?
C39 C40 C41 118.5(3) . . ?
C39 C40 N2 119.6(3) . . ?
C41 C40 N2 121.9(3) . . ?
C76 C75 C74 118.6(3) . . ?
C76 C75 N4 119.1(4) . . ?
C74 C75 N4 122.3(4) . . ?
C59 C61 C62 118.7(3) . . ?
C59 C61 N3 122.4(3) . . ?
C62 C61 N3 118.8(3) . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 N1 122.1(4) . . ?
C6 C5 N1 117.3(4) . . ?
C52 C51 C56 118.8(3) . . ?
C52 C51 C50 121.6(4) . . ?
C56 C51 C50 119.6(4) . . ?
C63 C58 C60 118.8(3) . . ?
C63 C58 C57 119.4(4) . . ?
C60 C58 C57 121.7(4) . . ?
C18 C19 N1 120.3(3) . . ?
C18 C19 C20 118.8(3) . . ?
N1 C19 C20 120.9(3) . . ?
C24 C23 C28 120.1(3) . . ?
C24 C23 C22 120.5(4) . . ?
C28 C23 C22 119.3(4) . . ?
C77 C72 C73 119.0(3) . . ?
C77 C72 C71 122.1(4) . . ?
C73 C72 C71 118.9(4) . . ?
C55 C54 C53 119.0(3) . . ?
C55 C54 N3 118.0(3) . . ?
C53 C54 N3 123.0(3) . . ?
C14 C9 C10 118.6(3) . . ?
C14 C9 C8 123.4(4) . . ?
C10 C9 C8 118.0(4) . . ?
C38 C39 C40 120.7(3) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
N4 C82 C83 122.8(3) . . ?
N4 C82 C81 118.8(3) . . ?
C83 C82 C81 118.3(3) . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C66 C65 C70 118.9(3) . . ?
C66 C65 C64 120.8(4) . . ?
C70 C65 C64 120.3(4) . . ?
C63 C62 C61 119.8(3) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C54 C55 C56 120.1(3) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C42 C37 C38 118.5(3) . . ?
C42 C37 C36 122.5(3) . . ?
C38 C37 C36 118.9(3) . . ?
O14 C43 O13 124.3(4) . . ?
O14 C43 C44 119.7(4) . . ?
O13 C43 C44 115.9(4) . . ?
C70 C69 C68 119.8(3) . . ?
C70 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
C35 C34 C33 120.8(3) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C23 C28 C27 119.7(3) . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C58 C63 C62 121.4(3) . . ?
C58 C63 H63 119.3 . . ?
C62 C63 H63 119.3 . . ?
C80 C81 C82 120.1(3) . . ?
C80 C81 H81 119.9 . . ?
C82 C81 H81 119.9 . . ?
C31 C30 C35 118.8(4) . . ?
C31 C30 C29 123.3(4) . . ?
C35 C30 C29 117.9(4) . . ?
C55 C56 C51 120.9(3) . . ?
C55 C56 H56 119.5 . . ?
C51 C56 H56 119.5 . . ?
C26 C27 C28 119.6(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H118 119.8 . . ?
C12 C11 H118 119.8 . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
O1 C1 O2 125.1(4) . . ?
O1 C1 C2 116.0(5) . . ?
O2 C1 C2 118.9(4) . . ?
C39 C38 C37 121.2(3) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C7 C2 C3 119.0(3) . . ?
C7 C2 C1 119.6(4) . . ?
C3 C2 C1 121.5(4) . . ?
C45 C46 C47 119.2(3) . . ?
C45 C46 H46 120.4 . . ?
C47 C46 H46 120.4 . . ?
C45 C44 C49 121.1(3) . . ?
C45 C44 C43 118.6(4) . . ?
C49 C44 C43 120.3(4) . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C42 C41 C40 121.0(3) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
O22 C71 O21 125.3(4) . . ?
O22 C71 C72 116.4(4) . . ?
O21 C71 C72 118.3(4) . . ?
C23 C24 C25 120.6(3) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C72 C77 C76 120.9(3) . . ?
C72 C77 H77 119.6 . . ?
C76 C77 H77 119.6 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H116 120.0 . . ?
C3 C4 H116 120.0 . . ?
C48 C49 C44 118.9(3) . . ?
C48 C49 H49 120.5 . . ?
C44 C49 H49 120.5 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H120 120.2 . . ?
C19 C20 H120 120.2 . . ?
C75 C74 C73 121.5(3) . . ?
C75 C74 H74 119.2 . . ?
C73 C74 H74 119.2 . . ?
C60 C59 C61 120.7(3) . . ?
C60 C59 H59 119.7 . . ?
C61 C59 H59 119.7 . . ?
C41 C42 C37 119.9(3) . . ?
C41 C42 H42 120.0 . . ?
C37 C42 H42 120.0 . . ?
C66 C67 C68 119.9(3) . . ?
C66 C67 H67 120.0 . . ?
C68 C67 H67 120.0 . . ?
O8 C22 O7 124.2(4) . . ?
O8 C22 C23 117.2(4) . . ?
O7 C22 C23 118.6(4) . . ?
C17 C16 C21 118.6(3) . . ?
C17 C16 C15 118.4(4) . . ?
C21 C16 C15 122.8(4) . . ?
C69 C70 C65 121.1(3) . . ?
C69 C70 H70 119.5 . . ?
C65 C70 H70 119.5 . . ?
C31 C32 C33 119.8(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C75 C76 C77 120.6(3) . . ?
C75 C76 H76 119.7 . . ?
C77 C76 H76 119.7 . . ?
C74 C73 C72 119.4(3) . . ?
C74 C73 H73 120.3 . . ?
C72 C73 H73 120.3 . . ?
C67 C66 C65 120.6(3) . . ?
C67 C66 H66 119.7 . . ?
C65 C66 H66 119.7 . . ?
O20 C64 O19 122.4(4) . . ?
O20 C64 C65 117.7(4) . . ?
O19 C64 C65 119.9(4) . . ?
O12 C36 O11 123.0(3) . . ?
O12 C36 C37 119.9(3) . . ?
O11 C36 C37 117.1(4) . . ?
O16 C50 O15 123.8(4) . . ?
O16 C50 C51 121.1(4) . . ?
O15 C50 C51 115.1(4) . . ?
C47 C48 C49 119.9(3) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C18 C17 C16 121.0(3) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C2 C7 C6 121.5(3) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C51 C52 C53 120.2(3) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 H52 119.9 . . ?
C58 C60 C59 120.6(3) . . ?
C58 C60 H60 119.7 . . ?
C59 C60 H60 119.7 . . ?
C5 C6 C7 118.5(3) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C84 C79 C80 118.9(4) . . ?
C84 C79 C78 122.2(4) . . ?
C80 C79 C78 118.9(4) . . ?
C81 C80 C79 121.7(4) . . ?
C81 C80 H80 119.2 . . ?
C79 C80 H80 119.2 . . ?
C52 C53 C54 120.9(3) . . ?
C52 C53 H53 119.6 . . ?
C54 C53 H53 119.6 . . ?
C83 C84 C79 119.3(3) . . ?
C83 C84 H84 120.4 . . ?
C79 C84 H84 120.4 . . ?
C20 C21 C16 121.6(3) . . ?
C20 C21 H21A 119.2 . . ?
C16 C21 H21A 119.2 . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C34 C35 C30 120.4(3) . . ?
C34 C35 H35 119.8 . . ?
C30 C35 H35 119.8 . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C13 C14 C9 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C30 C31 C32 121.4(4) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
O4 C8 O3 122.9(4) . . ?
O4 C8 C9 118.8(4) . . ?
O3 C8 C9 118.3(3) . . ?
C84 C83 C82 121.5(3) . . ?
C84 C83 H83 119.2 . . ?
C82 C83 H83 119.2 . . ?
O9 C29 O10 123.3(4) . . ?
O9 C29 C30 121.9(4) . . ?
O10 C29 C30 114.8(4) . . ?
O17 C57 O18 123.1(4) . . ?
O17 C57 C58 120.9(4) . . ?
O18 C57 C58 116.0(4) . . ?
O6 C15 O5 123.9(4) . . ?
O6 C15 C16 121.2(4) . . ?
O5 C15 C16 114.9(4) . . ?
O24 C78 O23 123.6(4) . . ?
O24 C78 C79 121.8(4) . . ?
O23 C78 C79 114.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        61.50
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.047
