# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_CCDC944132

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H120 F18 N8 O10'
_chemical_formula_weight         1888.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   13.026(3)
_cell_length_b                   25.015(5)
_cell_length_c                   16.358(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.574(4)
_cell_angle_gamma                90.00
_cell_volume                     5325(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9867
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.74

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1988
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9733
_exptl_absorpt_correction_T_max  0.9903
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61885
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_UnetI/netI     0.0322
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9393
_reflns_number_gt                7928
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 3.2'
_computing_publication_material  'ORTEP 3V.2'

_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. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 377 100 ' '
2 0.500 0.000 1.000 377 100 ' '
_platon_squeeze_details          
;
The unit cell contains one water and one dioxane molecule which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. 
;

_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)+(0.1034P)²+13.3923P] 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         9393
_refine_ls_number_parameters     600
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.2382
_refine_ls_wR_factor_gt          0.2323
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.2137(2) 0.49424(10) 0.01861(17) 0.0387(6) Uani 1 1 d . . .
O2 O 0.26853(17) 0.43493(9) -0.07032(15) 0.0307(5) Uani 1 1 d . . .
C1 C 0.2529(2) 0.45083(13) 0.0011(2) 0.0284(7) Uani 1 1 d . . .
C2 C 0.2838(3) 0.41389(17) 0.0716(3) 0.0461(10) Uani 1 1 d . . .
H2A H 0.3270 0.4329 0.1107 0.069 Uiso 1 1 calc R . .
H2B H 0.3205 0.3838 0.0512 0.069 Uiso 1 1 calc R . .
H2C H 0.2233 0.4016 0.0973 0.069 Uiso 1 1 calc R . .
F6 F 0.09320(18) 0.65783(10) 0.85607(14) 0.0481(6) Uani 1 1 d . . .
F7 F 0.59238(18) 0.71818(11) 1.13005(16) 0.0546(7) Uani 1 1 d . . .
F4 F 0.0638(2) 0.73290(10) 0.91325(18) 0.0599(7) Uani 1 1 d . . .
F5 F -0.06145(19) 0.68261(13) 0.87429(18) 0.0700(9) Uani 1 1 d . . .
F2 F 0.2379(3) 0.50275(12) 0.61362(16) 0.0680(8) Uani 1 1 d . . .
F8 F 0.7339(2) 0.70326(18) 1.07798(17) 0.0921(12) Uani 1 1 d . . .
F1 F 0.1707(3) 0.57784(13) 0.57998(18) 0.0775(9) Uani 1 1 d . . .
F3 F 0.0923(3) 0.50532(17) 0.5494(2) 0.1067(14) Uani 1 1 d . . .
F9 F 0.7139(4) 0.77127(13) 1.1533(3) 0.1083(15) Uani 1 1 d . . .
O3 O 0.4956(2) 0.63586(10) 1.26557(15) 0.0370(6) Uani 1 1 d . . .
O4 O 0.26321(18) 0.68490(9) 0.97114(17) 0.0358(6) Uani 1 1 d . . .
O5 O 0.3036(2) 0.58099(11) 0.72910(17) 0.0454(7) Uani 1 1 d . . .
N2 N 0.28572(19) 0.59554(10) 0.98240(17) 0.0252(6) Uani 1 1 d . . .
H2 H 0.2591 0.5654 0.9951 0.030 Uiso 1 1 calc R . .
N3 N 0.3200(2) 0.51336(12) 0.81963(17) 0.0296(6) Uani 1 1 d . . .
H3 H 0.2888 0.4896 0.8472 0.036 Uiso 1 1 calc R . .
N1 N 0.5621(2) 0.60324(11) 1.15115(18) 0.0300(6) Uani 1 1 d . . .
H1 H 0.6152 0.5995 1.1222 0.036 Uiso 1 1 calc R . .
N4 N 0.2951(2) 0.73521(12) 0.70540(18) 0.0326(7) Uani 1 1 d . . .
C3 C 0.4476(2) 0.54675(12) 0.97734(18) 0.0205(6) Uani 1 1 d . . .
C4 C 0.4805(2) 0.53849(13) 1.05880(19) 0.0221(6) Uani 1 1 d . . .
C40 C 0.3901(2) 0.59731(13) 0.9538(2) 0.0255(7) Uani 1 1 d . . .
H40A H 0.4259 0.6279 0.9777 0.031 Uiso 1 1 calc R . .
H40B H 0.3877 0.6014 0.8948 0.031 Uiso 1 1 calc R . .
C14 C 0.4675(2) 0.50839(13) 0.91833(18) 0.0211(6) Uani 1 1 d . . .
C41 C 0.2310(2) 0.64044(13) 0.9891(2) 0.0257(7) Uani 1 1 d . . .
C5 C 0.4627(2) 0.58108(15) 1.1226(2) 0.0309(8) Uani 1 1 d . . .
H5A H 0.4195 0.6092 1.0990 0.037 Uiso 1 1 calc R . .
H5B H 0.4280 0.5656 1.1682 0.037 Uiso 1 1 calc R . .
C6 C 0.5694(3) 0.62895(13) 1.2218(2) 0.0275(7) Uani 1 1 d . . .
C42 C 0.1284(2) 0.63342(12) 1.0259(2) 0.0263(7) Uani 1 1 d . . .
C15 C 0.4312(3) 0.51773(15) 0.83014(19) 0.0288(7) Uani 1 1 d . . .
H15A H 0.4525 0.5531 0.8132 0.035 Uiso 1 1 calc R . .
H15B H 0.4631 0.4917 0.7954 0.035 Uiso 1 1 calc R . .
C46 C -0.0540(3) 0.64939(16) 1.0314(3) 0.0400(9) Uani 1 1 d . . .
H46 H -0.1147 0.6631 1.0078 0.048 Uiso 1 1 calc R . .
C12 C 0.7298(3) 0.68923(15) 1.2186(2) 0.0362(8) Uani 1 1 d . . .
C7 C 0.6748(3) 0.64742(14) 1.2517(2) 0.0320(8) Uani 1 1 d . . .
C32 C 0.2756(3) 0.79400(14) 0.7235(2) 0.0348(8) Uani 1 1 d . . .
H32A H 0.3416 0.8116 0.7319 0.042 Uiso 1 1 calc R . .
H32B H 0.2416 0.8099 0.6754 0.042 Uiso 1 1 calc R . .
C47 C 0.0370(3) 0.65465(13) 0.9907(2) 0.0313(8) Uani 1 1 d . . .
C43 C 0.1251(3) 0.60705(14) 1.1002(2) 0.0309(7) Uani 1 1 d . . .
H43 H 0.1845 0.5917 1.1233 0.037 Uiso 1 1 calc R . .
C36 C 0.1949(3) 0.70441(16) 0.6989(2) 0.0387(9) Uani 1 1 d . . .
H36A H 0.1600 0.7093 0.7495 0.046 Uiso 1 1 calc R . .
H36B H 0.2111 0.6667 0.6945 0.046 Uiso 1 1 calc R . .
C28 C 0.3586(3) 0.70909(15) 0.7749(2) 0.0353(8) Uani 1 1 d . . .
H28A H 0.3658 0.6714 0.7627 0.042 Uiso 1 1 calc R . .
H28B H 0.3213 0.7120 0.8247 0.042 Uiso 1 1 calc R . .
C24 C 0.3492(3) 0.73382(15) 0.6257(2) 0.0355(8) Uani 1 1 d . . .
H24A H 0.3049 0.7505 0.5838 0.043 Uiso 1 1 calc R . .
H24B H 0.4109 0.7554 0.6319 0.043 Uiso 1 1 calc R . .
C18 C 0.0964(3) 0.53263(15) 0.8351(3) 0.0432(10) Uani 1 1 d . . .
H18 H 0.1321 0.5333 0.8856 0.052 Uiso 1 1 calc R . .
C44 C 0.0332(3) 0.60337(15) 1.1407(2) 0.0376(8) Uani 1 1 d . . .
H44 H 0.0322 0.5867 1.1914 0.045 Uiso 1 1 calc R . .
C16 C 0.2649(3) 0.54485(14) 0.7690(2) 0.0330(8) Uani 1 1 d . . .
C33 C 0.2125(3) 0.80576(17) 0.7958(3) 0.0447(9) Uani 1 1 d . . .
H33A H 0.2362 0.7839 0.8418 0.054 Uiso 1 1 calc R . .
H33B H 0.1411 0.7969 0.7827 0.054 Uiso 1 1 calc R . .
C34 C 0.2212(3) 0.86470(17) 0.8187(3) 0.0475(10) Uani 1 1 d . . .
H34A H 0.2920 0.8727 0.8353 0.057 Uiso 1 1 calc R . .
H34B H 0.2029 0.8863 0.7710 0.057 Uiso 1 1 calc R . .
C29 C 0.4654(3) 0.73284(17) 0.7905(3) 0.0463(10) Uani 1 1 d . . .
H29A H 0.5051 0.7284 0.7422 0.056 Uiso 1 1 calc R . .
H29B H 0.4596 0.7708 0.8013 0.056 Uiso 1 1 calc R . .
C45 C -0.0553(3) 0.62438(15) 1.1057(2) 0.0379(9) Uani 1 1 d . . .
H45 H -0.1165 0.6216 1.1325 0.045 Uiso 1 1 calc R . .
C8 C 0.7161(3) 0.62119(17) 1.3208(3) 0.0499(11) Uani 1 1 d . . .
H8 H 0.6797 0.5934 1.3437 0.060 Uiso 1 1 calc R . .
C17 C 0.1502(3) 0.53528(14) 0.7642(3) 0.0392(9) Uani 1 1 d . . .
C30 C 0.5208(3) 0.70569(15) 0.8631(2) 0.0399(9) Uani 1 1 d . . .
H30A H 0.4798 0.7091 0.9109 0.048 Uiso 1 1 calc R . .
H30B H 0.5286 0.6679 0.8515 0.048 Uiso 1 1 calc R . .
C25 C 0.3788(3) 0.67939(17) 0.5956(2) 0.0454(10) Uani 1 1 d . . .
H25A H 0.3190 0.6563 0.5926 0.054 Uiso 1 1 calc R . .
H25B H 0.4296 0.6636 0.6336 0.054 Uiso 1 1 calc R . .
C22 C 0.0957(3) 0.53060(16) 0.6883(3) 0.0478(11) Uani 1 1 d . . .
C37 C 0.1207(3) 0.71900(16) 0.6285(2) 0.0397(9) Uani 1 1 d . . .
H37A H 0.1505 0.7105 0.5768 0.048 Uiso 1 1 calc R . .
H37B H 0.1061 0.7570 0.6294 0.048 Uiso 1 1 calc R . .
C38 C 0.0214(3) 0.68711(18) 0.6374(3) 0.0488(10) Uani 1 1 d . . .
H38A H 0.0385 0.6498 0.6467 0.059 Uiso 1 1 calc R . .
H38B H -0.0133 0.7000 0.6848 0.059 Uiso 1 1 calc R . .
C48 C 0.0338(3) 0.68149(17) 0.9097(3) 0.0439(10) Uani 1 1 d . . .
C10 C 0.8633(4) 0.6779(2) 1.3234(3) 0.0609(13) Uani 1 1 d . . .
H10 H 0.9261 0.6884 1.3474 0.073 Uiso 1 1 calc R . .
C11 C 0.8238(3) 0.70406(18) 1.2561(3) 0.0500(11) Uani 1 1 d . . .
H11 H 0.8603 0.7324 1.2347 0.060 Uiso 1 1 calc R . .
C21 C -0.0108(4) 0.5260(2) 0.6868(4) 0.0718(18) Uani 1 1 d . . .
H21 H -0.0472 0.5229 0.6369 0.086 Uiso 1 1 calc R . .
C20 C -0.0626(4) 0.5261(2) 0.7575(4) 0.0729(18) Uani 1 1 d . . .
H20 H -0.1339 0.5242 0.7553 0.088 Uiso 1 1 calc R . .
C13 C 0.6927(3) 0.71954(17) 1.1461(3) 0.0427(9) Uani 1 1 d . . .
C31 C 0.6255(4) 0.7301(2) 0.8813(3) 0.0609(14) Uani 1 1 d . . .
H31A H 0.6702 0.7211 0.8383 0.091 Uiso 1 1 calc R . .
H31B H 0.6537 0.7163 0.9323 0.091 Uiso 1 1 calc R . .
H31C H 0.6191 0.7682 0.8849 0.091 Uiso 1 1 calc R . .
C26 C 0.4227(4) 0.6843(2) 0.5120(3) 0.0539(11) Uani 1 1 d . . .
H26A H 0.3724 0.7016 0.4753 0.065 Uiso 1 1 calc R . .
H26B H 0.4831 0.7069 0.5160 0.065 Uiso 1 1 calc R . .
C9 C 0.8103(4) 0.6361(2) 1.3557(3) 0.0653(14) Uani 1 1 d . . .
H9 H 0.8379 0.6178 1.4010 0.078 Uiso 1 1 calc R . .
C19 C -0.0097(3) 0.52894(17) 0.8321(4) 0.0572(13) Uani 1 1 d . . .
H19 H -0.0450 0.5284 0.8802 0.069 Uiso 1 1 calc R . .
C23 C 0.1497(4) 0.5292(2) 0.6093(3) 0.0646(14) Uani 1 1 d . . .
C39 C -0.0508(4) 0.6917(2) 0.5623(3) 0.0646(14) Uani 1 1 d . . .
H39A H -0.0650 0.7287 0.5511 0.097 Uiso 1 1 calc R . .
H39B H -0.1138 0.6733 0.5720 0.097 Uiso 1 1 calc R . .
H39C H -0.0192 0.6759 0.5162 0.097 Uiso 1 1 calc R . .
C35 C 0.1526(4) 0.8798(2) 0.8875(3) 0.0684(14) Uani 1 1 d . . .
H35A H 0.0820 0.8747 0.8698 0.103 Uiso 1 1 calc R . .
H35B H 0.1637 0.9166 0.9019 0.103 Uiso 1 1 calc R . .
H35C H 0.1686 0.8576 0.9342 0.103 Uiso 1 1 calc R . .
C27 C 0.4514(5) 0.6317(2) 0.4761(3) 0.0738(16) Uani 1 1 d . . .
H27A H 0.5087 0.6169 0.5073 0.111 Uiso 1 1 calc R . .
H27B H 0.4698 0.6368 0.4205 0.111 Uiso 1 1 calc R . .
H27C H 0.3940 0.6077 0.4776 0.111 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
O1 C1 1.239(4) . ?
O2 C1 1.260(4) . ?
C1 C2 1.517(5) . ?
F6 C48 1.334(5) . ?
F7 C13 1.322(5) . ?
F4 C48 1.345(5) . ?
F5 C48 1.346(5) . ?
F2 C23 1.325(6) . ?
F8 C13 1.323(5) . ?
F1 C23 1.341(6) . ?
F3 C23 1.345(5) . ?
F9 C13 1.327(5) . ?
O3 C6 1.236(4) . ?
O4 C41 1.229(4) . ?
O5 C16 1.235(5) . ?
N2 C41 1.337(4) . ?
N2 C40 1.458(4) . ?
N3 C16 1.330(4) . ?
N3 C15 1.455(4) . ?
N1 C6 1.322(4) . ?
N1 C5 1.466(4) . ?
N4 C24 1.510(5) . ?
N4 C36 1.514(5) . ?
N4 C28 1.523(4) . ?
N4 C32 1.523(5) . ?
C3 C14 1.393(4) . ?
C3 C4 1.397(4) . ?
C3 C40 1.511(4) . ?
C4 C14 1.397(4) 3_667 ?
C4 C5 1.516(4) . ?
C14 C4 1.397(4) 3_667 ?
C14 C15 1.516(4) . ?
C41 C42 1.501(5) . ?
C6 C7 1.509(5) . ?
C42 C43 1.385(5) . ?
C42 C47 1.404(5) . ?
C46 C45 1.367(6) . ?
C46 C47 1.391(5) . ?
C12 C7 1.391(6) . ?
C12 C11 1.395(6) . ?
C12 C13 1.470(6) . ?
C7 C8 1.395(5) . ?
C32 C33 1.500(6) . ?
C47 C48 1.485(6) . ?
C43 C44 1.396(5) . ?
C36 C37 1.516(5) . ?
C28 C29 1.524(5) . ?
C24 C25 1.504(6) . ?
C18 C17 1.383(6) . ?
C18 C19 1.383(6) . ?
C44 C45 1.369(6) . ?
C16 C17 1.511(5) . ?
C33 C34 1.525(6) . ?
C34 C35 1.515(7) . ?
C29 C30 1.522(5) . ?
C8 C9 1.381(6) . ?
C17 C22 1.408(5) . ?
C30 C31 1.511(6) . ?
C25 C26 1.512(6) . ?
C22 C21 1.390(7) . ?
C22 C23 1.498(8) . ?
C37 C38 1.531(5) . ?
C38 C39 1.518(6) . ?
C10 C11 1.361(7) . ?
C10 C9 1.372(8) . ?
C21 C20 1.365(9) . ?
C20 C19 1.375(8) . ?
C26 C27 1.493(7) . ?

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
O1 C1 O2 125.2(3) . . ?
O1 C1 C2 117.2(3) . . ?
O2 C1 C2 117.6(3) . . ?
C41 N2 C40 120.6(3) . . ?
C16 N3 C15 122.4(3) . . ?
C6 N1 C5 119.4(3) . . ?
C24 N4 C36 111.2(3) . . ?
C24 N4 C28 112.0(3) . . ?
C36 N4 C28 105.8(3) . . ?
C24 N4 C32 106.1(3) . . ?
C36 N4 C32 110.8(3) . . ?
C28 N4 C32 111.0(3) . . ?
C14 C3 C4 120.0(3) . . ?
C14 C3 C40 120.4(3) . . ?
C4 C3 C40 119.6(3) . . ?
C3 C4 C14 120.3(3) . 3_667 ?
C3 C4 C5 120.2(3) . . ?
C14 C4 C5 119.5(3) 3_667 . ?
N2 C40 C3 110.6(3) . . ?
C3 C14 C4 119.7(3) . 3_667 ?
C3 C14 C15 119.6(3) . . ?
C4 C14 C15 120.7(3) 3_667 . ?
O4 C41 N2 123.5(3) . . ?
O4 C41 C42 121.4(3) . . ?
N2 C41 C42 115.0(3) . . ?
N1 C5 C4 108.9(2) . . ?
O3 C6 N1 123.2(3) . . ?
O3 C6 C7 119.3(3) . . ?
N1 C6 C7 117.4(3) . . ?
C43 C42 C47 118.7(3) . . ?
C43 C42 C41 118.1(3) . . ?
C47 C42 C41 123.2(3) . . ?
N3 C15 C14 111.5(3) . . ?
C45 C46 C47 120.9(3) . . ?
C7 C12 C11 119.1(4) . . ?
C7 C12 C13 123.0(3) . . ?
C11 C12 C13 117.9(4) . . ?
C12 C7 C8 118.9(3) . . ?
C12 C7 C6 125.5(3) . . ?
C8 C7 C6 115.5(3) . . ?
C33 C32 N4 116.4(3) . . ?
C46 C47 C42 119.6(3) . . ?
C46 C47 C48 118.7(3) . . ?
C42 C47 C48 121.7(3) . . ?
C42 C43 C44 120.6(3) . . ?
N4 C36 C37 116.7(3) . . ?
N4 C28 C29 114.8(3) . . ?
C25 C24 N4 116.1(3) . . ?
C17 C18 C19 121.1(4) . . ?
C45 C44 C43 120.0(4) . . ?
O5 C16 N3 122.7(3) . . ?
O5 C16 C17 121.0(3) . . ?
N3 C16 C17 116.3(3) . . ?
C32 C33 C34 110.3(3) . . ?
C35 C34 C33 112.6(4) . . ?
C30 C29 C28 110.8(3) . . ?
C46 C45 C44 120.2(4) . . ?
C9 C8 C7 120.7(5) . . ?
C18 C17 C22 118.7(4) . . ?
C18 C17 C16 120.1(3) . . ?
C22 C17 C16 121.2(4) . . ?
C31 C30 C29 111.4(3) . . ?
C24 C25 C26 109.6(3) . . ?
C21 C22 C17 119.0(5) . . ?
C21 C22 C23 119.3(4) . . ?
C17 C22 C23 121.6(4) . . ?
C36 C37 C38 108.3(3) . . ?
C39 C38 C37 112.2(4) . . ?
F6 C48 F4 106.1(3) . . ?
F6 C48 F5 106.1(4) . . ?
F4 C48 F5 105.0(3) . . ?
F6 C48 C47 113.1(3) . . ?
F4 C48 C47 113.4(4) . . ?
F5 C48 C47 112.4(3) . . ?
C11 C10 C9 120.0(4) . . ?
C10 C11 C12 121.3(5) . . ?
C20 C21 C22 121.1(5) . . ?
C21 C20 C19 120.3(5) . . ?
F7 C13 F8 105.0(3) . . ?
F7 C13 F9 104.0(4) . . ?
F8 C13 F9 106.5(4) . . ?
F7 C13 C12 115.7(3) . . ?
F8 C13 C12 112.9(3) . . ?
F9 C13 C12 111.8(4) . . ?
C27 C26 C25 113.3(4) . . ?
C10 C9 C8 120.0(4) . . ?
C20 C19 C18 119.6(5) . . ?
F2 C23 F1 106.3(5) . . ?
F2 C23 F3 105.6(5) . . ?
F1 C23 F3 104.9(4) . . ?
F2 C23 C22 113.9(4) . . ?
F1 C23 C22 113.5(4) . . ?
F3 C23 C22 111.8(5) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.093
_database_code_depnum_ccdc_archive 'CCDC 944132'
#######################################################################
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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data_CCDC944135
_vrf_                            
;
PROBLEM: 
PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s)
RESPPONSE: 
This alert arises due to quite substantial disorder or high thermal motion of 
in particular carbon atoms of the tetrabutyl-ammonium fragment.
Amongst them C6, C11 and C78 have shown splitting 
and treated as disordered atoms;  
See _publ_section_exptl_refinement
PROBLEM: 
THETM01_ALERT_3_A  The value of sine(theta_max)/wavelength is less than 0.550
RESPPONSE: 
The 2theta value was found to be low after repetitive attempt;
PROBLEM:
PLAT430_ALERT_2_A Short Inter D...A Contact O7B .. O8 .. 2.30 Ang.
PLAT430_ALERT_2_A Short Inter D...A Contact O8 .. O9A .. 2.01 Ang.
PLAT430_ALERT_2_A Short Inter D...A Contact O8 .. O7A .. 2.06 Ang.
PLAT430_ALERT_2_A Short Inter D...A Contact O8 .. O9B .. 2.13 Ang.
RESPONSE:
These alerts are generating due modeling of the nitrate segment of the crystal. 
These oxygen atoms O7A, O7B, O8, O9A and O9B are the parts of the disordered nitrate.
Actually the nitrate have rotational disorder. 
The nitrate consisting of N7A-O9A-O8-O7A 
flips to the position N7B-O9B-O8-O7B keeping O8 in pivotal position; 
See _publ_section_exptl_refinement
PROBLEM:
DIFMX01_ALERT_2_B The maximum difference density is > 0.1*ZMAX*1.00
 _refine_diff_density_max given = 1.079
 Test value = 0.900
REFNR01_ALERT_3_B Ratio of reflections to parameters is < 8 for a
 centrosymmetric structure
 sine(theta)/lambda 0.4588
 Proportion of unique data used 1.0000
 Ratio reflections to parameters 6.2761
 Crystal system given = monoclinic
RESPONSE: 
The residual density can not be reduced furthur.
The 2theta value was found to be low after repetitive attempt;
PROBLEM:
PLAT097_ALERT_2_B Large Reported Max. (Positive) Residual Density 1.08 eA-3  
RESPONSE:
The residual density is remaining at 1.08 after using all restrains 
and disorder treatments;
PROBLEM:
PLAT221_ALERT_2_B Large Solv./Anion N Ueq(max)/Ueq(min) Range 10.0 Ratio
RESPONSE:
It is due to the difference of thermal mobility. The nitrogen 
atom is disordered in two positions;See _publ_section_exptl_refinement
PROBLEM:
PLAT230_ALERT_2_B Hirshfeld Test Diff for F12 -- C74 .. 7.4 su 
PLAT230_ALERT_2_B Hirshfeld Test Diff for C16 -- C17 .. 9.6 su 
PLAT230_ALERT_2_B Hirshfeld Test Diff for C47 -- C75 .. 8.0 su 
PLAT230_ALERT_2_B Hirshfeld Test Diff for C68 -- C70 .. 8.3 su 
PLAT230_ALERT_2_B Hirshfeld Test Diff for C49 -- C76 .. 7.2 su
RESPONSE:
The chemical composition and geometry of the ring is correct. 
These carbons represent benzene ring carbons 
and can not be split further; 
PROBLEM:
PLAT088_ALERT_3_B Poor Data / Parameter Ratio .................... 6.33 Note
RESPONSE:
The data/ parameter ratio obtained is optimum in this case; 
PROBLEM:
PLAT097_ALERT_2_B Large Reported Max. (Positive) Residual Density 1.13 eA-3	
RESPONSE:
This value is close to 1
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H71 F19 N8 O10'
_chemical_formula_weight         1617.41

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

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

_cell_length_a                   18.729(3)
_cell_length_b                   31.942(3)
_cell_length_c                   26.316(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.030(5)
_cell_angle_gamma                90.00
_cell_volume                     15452(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3349
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      16.75

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6672
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9878
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6182
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         19.03
_reflns_number_total             6182
_reflns_number_gt                4255
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 3.2'
_computing_publication_material  'ORTEP 3v.2'

_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. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.823 0.389 0.015 18 1 ' '
2 0.323 0.889 0.015 18 1 ' '
3 0.083 0.263 0.079 8 0 ' '
4 0.583 0.763 0.079 8 0 ' '
5 0.000 0.252 0.250 39 5 ' '
6 0.500 0.752 0.250 39 5 ' '
7 1.000 0.394 0.250 11 0 ' '
8 0.500 0.447 0.250 15 0 ' '
9 0.500 0.894 0.250 11 0 ' '
10 1.000 0.947 0.250 15 0 ' '
11 0.500 0.038 0.250 7 0 ' '
12 0.000 0.538 0.250 7 0 ' '
13 0.917 0.263 0.420 8 0 ' '
14 0.417 0.763 0.420 8 0 ' '
15 0.177 0.389 0.485 18 1 ' '
16 0.677 0.889 0.485 18 1 ' '
17 0.323 0.111 0.515 18 1 ' '
18 0.823 0.611 0.515 18 1 ' '
19 0.583 0.237 0.579 8 0 ' '
20 0.083 0.737 0.579 8 0 ' '
21 0.500 0.248 0.750 39 5 ' '
22 0.000 0.748 0.750 39 5 ' '
23 1.000 0.053 0.750 15 0 ' '
24 0.500 0.106 0.750 11 0 ' '
25 0.500 0.553 0.750 15 0 ' '
26 1.000 0.606 0.750 11 0 ' '
27 0.000 0.462 0.750 7 0 ' '
28 0.500 0.962 0.750 7 0 ' '
29 0.417 0.237 0.920 8 0 ' '
30 0.917 0.737 0.920 8 0 ' '
31 0.677 0.111 0.985 18 1 ' '
32 0.177 0.611 0.985 18 1 ' '
_platon_squeeze_details          
;
The unit cell contains water molecule which have been treated  as a diffuse contribution 
to the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
_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)+(0.2000P)²+0.0100P] 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       0.00058(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6182
_refine_ls_number_parameters     986
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0923
_refine_ls_wR_factor_ref         0.3043
_refine_ls_wR_factor_gt          0.2731
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_restrained_S_all      1.207
_refine_ls_shift/su_max          0.005
_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
O9A O 0.2363(7) 0.6077(4) 0.0973(4) 0.075(3) Uani 0.50 1 d P A 1
O9B O 0.1598(6) 0.6915(3) 0.1083(3) 0.048(3) Uani 0.50 1 d PD B 2
F6B F 0.2523(7) 0.7619(4) 0.3543(5) 0.094(4) Uiso 0.44 1 d P C 1
F4A F 0.2678(7) 0.7550(4) 0.4328(5) 0.097(4) Uiso 0.49 1 d P C 1
F19B F 0.2317(8) 0.7044(5) 0.3802(6) 0.100(4) Uiso 0.43 1 d P C 1
F2A F 0.2554(10) 0.8413(6) 0.1161(8) 0.117(6) Uiso 0.42 1 d P D 1
F3B F 0.1898(7) 0.7897(4) 0.0965(5) 0.087(4) Uiso 0.47 1 d P D 1
F11A F -0.1985(5) 0.6358(4) 0.1334(4) 0.069(4) Uiso 0.51 1 d P E 1
F13A F -0.2262(7) 0.5914(4) 0.0753(5) 0.089(4) Uiso 0.48 1 d P E 1
F8A F 0.2453(10) 0.4961(6) 0.0112(6) 0.139(6) Uiso 0.48 1 d P F 1
F21A F 0.2601(9) 0.5336(5) 0.0605(6) 0.146(5) Uiso 0.48 1 d P F 1
C78A C 0.4394(12) 0.9750(6) 0.2117(8) 0.095(6) Uiso 0.51 1 d P G 1
F6A F 0.2674(6) 0.7804(4) 0.4013(5) 0.111(3) Uiso 0.56 1 d P C 2
F4B F 0.2550(6) 0.7230(4) 0.4401(4) 0.087(3) Uiso 0.51 1 d P C 2
F19A F 0.2496(5) 0.7248(3) 0.3596(4) 0.072(2) Uiso 0.57 1 d P C 2
F2B F 0.2553(6) 0.8591(4) 0.0948(5) 0.112(4) Uiso 0.58 1 d P D 2
F3A F 0.2053(6) 0.8066(4) 0.1207(5) 0.091(3) Uiso 0.53 1 d P D 2
F11B F -0.1988(7) 0.6154(5) 0.1348(5) 0.079(4) Uiso 0.49 1 d P E 2
F13B F -0.2071(7) 0.5700(4) 0.0759(4) 0.095(4) Uiso 0.52 1 d P E 2
F8B F 0.2314(6) 0.4738(4) 0.0147(4) 0.086(4) Uiso 0.52 1 d P F 2
F21B F 0.2411(4) 0.4918(2) 0.0932(3) 0.0414(19) Uiso 0.52 1 d P F 2
C78B C 0.4117(15) 0.9674(7) 0.1546(10) 0.107(7) Uiso 0.49 1 d P G 2
C11A C 0.3711(13) 0.9701(7) 0.1952(10) 0.081(8) Uiso 0.51 1 d P . .
C11B C 0.3663(15) 0.9585(8) 0.1743(11) 0.092(9) Uiso 0.49 1 d P G .
O1A O 0.1625(7) 0.7830(3) 0.2787(4) 0.051(3) Uiso 0.51 1 d P . .
O1B O 0.1266(7) 0.7868(3) 0.2643(4) 0.048(3) Uiso 0.49 1 d P . .
C6A C 0.1859(9) 0.8942(5) 0.3978(7) 0.060(4) Uiso 0.55 1 d P . .
C6B C 0.1556(12) 0.9050(6) 0.3727(8) 0.062(6) Uiso 0.45 1 d P . .
F14A F 0.3482(8) 0.5268(5) 0.4387(5) 0.101(5) Uiso 0.44 1 d P . .
F14B F 0.3328(5) 0.5027(3) 0.4364(4) 0.080(3) Uiso 0.56 1 d P . .
C57 C 0.2119(8) 0.4980(4) 0.0521(6) 0.066(4) Uiso 0.63 1 d P . .
F20 F 0.1926(9) 0.4513(5) 0.0617(6) 0.114(5) Uiso 0.37 1 d P F .
N7A N 0.2173(8) 0.6403(7) 0.0948(5) 0.004(4) Uiso 0.31 1 d PD A 1
O7A O 0.1549(8) 0.6540(6) 0.0960(6) 0.071(4) Uiso 0.43 1 d PD A 1
N7B N 0.1968(6) 0.6611(4) 0.0990(4) 0.067(3) Uiso 0.69 1 d PD B 2
O7B O 0.1617(5) 0.6261(3) 0.0913(3) 0.053(3) Uiso 0.57 1 d P B 2
O6 O -0.0539(3) 0.65105(16) 0.1802(2) 0.0547(15) Uani 1 1 d . . .
O4 O 0.5060(3) 0.61789(15) 0.1831(2) 0.0532(15) Uani 1 1 d . . .
N6 N 0.3876(3) 0.55921(19) 0.2673(2) 0.0404(16) Uani 1 1 d . . .
H6 H 0.4163 0.5770 0.2853 0.048 Uiso 1 1 calc R . .
F12 F -0.1201(4) 0.57644(19) 0.1363(3) 0.100(2) Uani 1 1 d . E .
N2 N 0.3999(3) 0.65240(17) 0.1632(2) 0.0376(16) Uani 1 1 d . . .
H2 H 0.3671 0.6626 0.1390 0.045 Uiso 1 1 calc R . .
O2 O 0.3428(3) 0.49322(18) 0.2647(2) 0.0637(17) Uani 1 1 d . . .
C44 C 0.4551(5) 0.6327(2) 0.1501(3) 0.042(2) Uani 1 1 d . . .
N8 N 0.2769(4) 0.8919(2) 0.2728(3) 0.060(2) Uani 1 1 d . G .
N3 N 0.1664(3) 0.54937(19) 0.1537(2) 0.0465(17) Uani 1 1 d . . .
H3 H 0.1805 0.5684 0.1348 0.056 Uiso 1 1 calc R . .
F010 F 0.3004(3) 0.5290(2) 0.3593(2) 0.0953(18) Uani 1 1 d . . .
N4 N 0.0490(4) 0.62597(18) 0.1585(2) 0.0454(17) Uani 1 1 d . . .
H4 H 0.0717 0.6194 0.1342 0.054 Uiso 1 1 calc R . .
C30 C 0.1667(4) 0.6298(3) 0.2202(2) 0.037(2) Uani 1 1 d . . .
C27 C 0.2903(4) 0.6070(2) 0.2212(2) 0.0354(19) Uani 1 1 d . . .
O8 O 0.2615(3) 0.6687(2) 0.09487(19) 0.0742(19) Uani 1 1 d D . .
C35 C 0.1907(4) 0.5527(2) 0.2098(3) 0.045(2) Uani 1 1 d . . .
H35A H 0.2299 0.5331 0.2218 0.054 Uiso 1 1 calc R . .
H35B H 0.1510 0.5468 0.2275 0.054 Uiso 1 1 calc R . .
C25 C 0.2641(4) 0.6810(2) 0.2268(2) 0.0345(19) Uani 1 1 d . . .
C33 C 0.2893(4) 0.7262(2) 0.2277(3) 0.045(2) Uani 1 1 d . . .
H33A H 0.2543 0.7442 0.2398 0.054 Uiso 1 1 calc R . .
H33B H 0.3358 0.7291 0.2511 0.054 Uiso 1 1 calc R . .
C32 C 0.3911(4) 0.6580(2) 0.2170(3) 0.044(2) Uani 1 1 d . . .
H32A H 0.4033 0.6866 0.2276 0.053 Uiso 1 1 calc R . .
H32B H 0.4245 0.6396 0.2392 0.053 Uiso 1 1 calc R . .
C31 C 0.0853(4) 0.6209(2) 0.2123(3) 0.045(2) Uani 1 1 d . . .
H31A H 0.0780 0.5925 0.2233 0.054 Uiso 1 1 calc R . .
H31B H 0.0634 0.6397 0.2338 0.054 Uiso 1 1 calc R . .
N1 N 0.2962(3) 0.73795(19) 0.1756(2) 0.0429(17) Uani 1 1 d . . .
H1 H 0.2734 0.7231 0.1504 0.052 Uiso 1 1 calc R . .
C28 C 0.3137(4) 0.6485(3) 0.2233(3) 0.038(2) Uani 1 1 d . . .
C63 C -0.0520(5) 0.6433(2) 0.0905(3) 0.044(2) Uani 1 1 d . . .
C34 C 0.3456(4) 0.5727(2) 0.2174(3) 0.044(2) Uani 1 1 d . . .
H34A H 0.3202 0.5487 0.2000 0.053 Uiso 1 1 calc R . .
H34B H 0.3790 0.5828 0.1961 0.053 Uiso 1 1 calc R . .
N5 N 0.1188(3) 0.7165(2) 0.2722(2) 0.0453(17) Uani 1 1 d . . .
H5 H 0.1046 0.6967 0.2900 0.054 Uiso 1 1 calc R . .
C29 C 0.2171(4) 0.5977(2) 0.2201(2) 0.0368(19) Uani 1 1 d . . .
C26 C 0.1911(4) 0.6716(2) 0.2244(2) 0.038(2) Uani 1 1 d . . .
C69 C 0.4210(5) 0.5030(2) 0.3821(4) 0.054(2) Uani 1 1 d . . .
O5 O 0.1029(4) 0.4895(2) 0.1523(2) 0.0783(19) Uani 1 1 d . . .
C71 C 0.4377(5) 0.5123(2) 0.3348(3) 0.044(2) Uani 1 1 d . . .
F17 F 0.5631(4) 0.6871(2) 0.1343(3) 0.118(2) Uani 1 1 d . . .
C24 C 0.1342(4) 0.7061(2) 0.2217(3) 0.044(2) Uani 1 1 d . . .
H24A H 0.1513 0.7309 0.2066 0.053 Uiso 1 1 calc R . .
H24B H 0.0896 0.6971 0.1993 0.053 Uiso 1 1 calc R . .
F15 F 0.3119(3) 0.4641(3) 0.3801(3) 0.136(3) Uani 1 1 d . . .
C4 C 0.2162(5) 0.8750(3) 0.3504(4) 0.073(3) Uani 1 1 d . G .
C38 C 0.3454(6) 0.7713(3) 0.1091(4) 0.056(2) Uani 1 1 d . . .
C15 C 0.3376(5) 0.8606(3) 0.2912(4) 0.067(3) Uani 1 1 d . . .
H15A H 0.3547 0.8498 0.2612 0.080 Uiso 1 1 calc R . .
H15B H 0.3175 0.8372 0.3075 0.080 Uiso 1 1 calc R . .
O3 O 0.3639(4) 0.7947(2) 0.1962(3) 0.098(2) Uani 1 1 d . . .
C14 C 0.4033(5) 0.8781(3) 0.3297(4) 0.069(3) Uani 1 1 d . . .
H14A H 0.4252 0.9009 0.3138 0.083 Uiso 1 1 calc R . .
H14B H 0.3875 0.8888 0.3602 0.083 Uiso 1 1 calc R . .
C2 C 0.2213(5) 0.8680(2) 0.2347(3) 0.060(2) Uani 1 1 d . . .
H2A H 0.2118 0.8416 0.2503 0.072 Uiso 1 1 calc R . .
H2B H 0.2418 0.8618 0.2044 0.072 Uiso 1 1 calc R . .
C46 C 0.4552(5) 0.6265(2) 0.0948(3) 0.052(2) Uani 1 1 d . . .
C64 C -0.0192(5) 0.6407(2) 0.1462(3) 0.041(2) Uani 1 1 d . . .
C62 C -0.1228(5) 0.6286(3) 0.0715(4) 0.057(2) Uani 1 1 d . E .
C50 C 0.1245(4) 0.5194(3) 0.1301(3) 0.048(2) Uani 1 1 d . F .
C65 C 0.3838(5) 0.5208(3) 0.2865(3) 0.049(2) Uani 1 1 d . . .
C68 C 0.5428(7) 0.4921(3) 0.4209(4) 0.080(3) Uani 1 1 d . . .
H68 H 0.5781 0.4852 0.4496 0.096 Uiso 1 1 calc R . .
C66 C 0.5114(5) 0.5113(2) 0.3317(3) 0.060(2) Uani 1 1 d . . .
H66 H 0.5253 0.5176 0.3004 0.072 Uiso 1 1 calc R . .
C36 C 0.3342(5) 0.7693(3) 0.1644(3) 0.055(2) Uani 1 1 d . . .
C23 C 0.1250(4) 0.7536(3) 0.2923(3) 0.050(2) Uani 1 1 d . . .
C9 C 0.3055(5) 0.9298(2) 0.2487(4) 0.069(3) Uani 1 1 d . . .
H9A H 0.3406 0.9439 0.2751 0.083 Uiso 1 1 calc R G .
H9B H 0.2654 0.9491 0.2377 0.083 Uiso 1 1 calc R . .
C19 C 0.0019(5) 0.7729(3) 0.3883(4) 0.065(3) Uani 1 1 d . . .
H19 H -0.0470 0.7789 0.3871 0.078 Uiso 1 1 calc R . .
C21 C 0.0283(5) 0.7680(2) 0.3438(4) 0.057(2) Uani 1 1 d . . .
H21 H -0.0034 0.7708 0.3121 0.069 Uiso 1 1 calc R . .
C45 C 0.3971(6) 0.6066(3) 0.0649(4) 0.061(2) Uani 1 1 d . . .
H45 H 0.3579 0.5988 0.0798 0.074 Uiso 1 1 calc R . .
C22 C 0.1017(5) 0.7589(2) 0.3441(3) 0.054(2) Uani 1 1 d . . .
C61 C -0.1541(6) 0.6346(3) 0.0199(5) 0.088(3) Uani 1 1 d . . .
H61 H -0.2004 0.6242 0.0070 0.106 Uiso 1 1 calc R . .
C59 C -0.0483(6) 0.6702(3) 0.0050(4) 0.063(2) Uani 1 1 d . . .
H59 H -0.0233 0.6842 -0.0171 0.075 Uiso 1 1 calc R . .
C3 C 0.2449(5) 0.9090(3) 0.3179(3) 0.068(3) Uani 1 1 d . . .
H3A H 0.2054 0.9279 0.3043 0.082 Uiso 1 1 calc R G .
H3B H 0.2821 0.9251 0.3404 0.082 Uiso 1 1 calc R . .
F16 F 0.6277(4) 0.6333(3) 0.1282(3) 0.149(3) Uani 1 1 d . . .
C58 C -0.0156(5) 0.6637(2) 0.0563(3) 0.053(2) Uani 1 1 d . . .
H58 H 0.0316 0.6733 0.0681 0.064 Uiso 1 1 calc R . .
C52 C 0.0047(7) 0.5558(3) 0.0059(6) 0.094(4) Uani 1 1 d . . .
H52 H -0.0404 0.5686 -0.0044 0.113 Uiso 1 1 calc R . .
C70 C 0.4717(6) 0.4930(3) 0.4249(4) 0.076(3) Uani 1 1 d . . .
H70 H 0.4578 0.4870 0.4562 0.091 Uiso 1 1 calc R . .
C55 C 0.1388(5) 0.5191(3) 0.0354(4) 0.076(3) Uani 1 1 d . F .
C56 C 0.0986(5) 0.5276(2) 0.0738(4) 0.057(2) Uani 1 1 d . . .
C1 C 0.1501(6) 0.8906(3) 0.2177(4) 0.098(3) Uani 1 1 d . . .
H1A H 0.1272 0.8947 0.2474 0.117 Uiso 1 1 calc R . .
H1B H 0.1597 0.9181 0.2046 0.117 Uiso 1 1 calc R . .
C20 C 0.0491(7) 0.7687(3) 0.4349(4) 0.070(3) Uani 1 1 d . . .
H20 H 0.0318 0.7724 0.4654 0.084 Uiso 1 1 calc R . .
C18 C 0.1196(7) 0.7595(3) 0.4373(3) 0.067(3) Uani 1 1 d . . .
H18 H 0.1505 0.7564 0.4692 0.080 Uiso 1 1 calc R . .
C39 C 0.3015(6) 0.7923(3) 0.0695(4) 0.071(3) Uani 1 1 d . D .
F1 F 0.1921(5) 0.8283(2) 0.0386(3) 0.163(3) Uani 1 1 d . D .
C67 C 0.5634(5) 0.5014(3) 0.3737(4) 0.067(3) Uani 1 1 d . . .
H67 H 0.6122 0.5008 0.3710 0.080 Uiso 1 1 calc R . .
C17 C 0.1464(5) 0.7545(3) 0.3912(4) 0.060(2) Uani 1 1 d . C .
C51 C 0.0303(6) 0.5462(3) 0.0571(4) 0.076(3) Uani 1 1 d . F .
H51 H 0.0014 0.5521 0.0813 0.091 Uiso 1 1 calc R . .
C47 C 0.3950(7) 0.5976(3) 0.0136(5) 0.092(3) Uani 1 1 d . . .
H47 H 0.3549 0.5842 -0.0059 0.110 Uiso 1 1 calc R . .
C7 C 0.0995(6) 0.8679(3) 0.1771(4) 0.088(3) Uani 1 1 d . . .
H7A H 0.1203 0.8671 0.1461 0.106 Uiso 1 1 calc R . .
H7B H 0.0957 0.8393 0.1886 0.106 Uiso 1 1 calc R . .
C43 C 0.4019(6) 0.7493(3) 0.0972(4) 0.076(3) Uani 1 1 d . . .
H43 H 0.4326 0.7350 0.1234 0.092 Uiso 1 1 calc R . .
C10 C 0.3411(6) 0.9205(3) 0.2027(5) 0.106(4) Uani 1 1 d . G .
F18 F 0.6151(5) 0.6790(4) 0.0687(4) 0.216(5) Uani 1 1 d . . .
C49 C 0.5139(6) 0.6366(3) 0.0706(5) 0.077(3) Uani 1 1 d . . .
C12 C 0.5249(7) 0.8600(4) 0.3832(5) 0.129(5) Uani 1 1 d . . .
H12A H 0.5425 0.8850 0.3696 0.193 Uiso 1 1 calc R . .
H12B H 0.5626 0.8392 0.3883 0.193 Uiso 1 1 calc R . .
H12C H 0.5111 0.8661 0.4157 0.193 Uiso 1 1 calc R . .
C53 C 0.0467(10) 0.5463(4) -0.0294(5) 0.102(4) Uani 1 1 d . F .
H53 H 0.0294 0.5528 -0.0640 0.122 Uiso 1 1 calc R . .
C42 C 0.4155(7) 0.7475(3) 0.0472(6) 0.091(3) Uani 1 1 d . . .
H42 H 0.4538 0.7314 0.0401 0.109 Uiso 1 1 calc R . .
C13 C 0.4587(7) 0.8434(3) 0.3449(5) 0.110(4) Uani 1 1 d . . .
H13A H 0.4741 0.8327 0.3142 0.132 Uiso 1 1 calc R . .
H13B H 0.4366 0.8206 0.3607 0.132 Uiso 1 1 calc R . .
C60 C -0.1161(7) 0.6562(3) -0.0128(4) 0.076(3) Uani 1 1 d . . .
H60 H -0.1380 0.6610 -0.0471 0.092 Uiso 1 1 calc R . .
C48 C 0.5122(9) 0.6280(4) 0.0195(6) 0.113(5) Uani 1 1 d . . .
H48 H 0.5513 0.6353 0.0043 0.135 Uiso 1 1 calc R . .
C37 C 0.2381(7) 0.8163(4) 0.0803(4) 0.098(4) Uani 1 1 d . . .
C16 C 0.2236(7) 0.7454(3) 0.3948(4) 0.081(3) Uani 1 1 d . . .
C54 C 0.1129(7) 0.5277(4) -0.0161(4) 0.100(4) Uani 1 1 d . . .
H54 H 0.1400 0.5209 -0.0411 0.120 Uiso 1 1 calc R F .
C40 C 0.3151(7) 0.7914(4) 0.0187(4) 0.092(3) Uani 1 1 d . . .
H40 H 0.2850 0.8058 -0.0078 0.110 Uiso 1 1 calc R D .
C5 C 0.1507(7) 0.8680(4) 0.4268(5) 0.130(5) Uani 1 1 d . . .
C8 C 0.0259(7) 0.8856(4) 0.1636(5) 0.121(4) Uani 1 1 d . . .
H8A H 0.0033 0.8849 0.1934 0.181 Uiso 1 1 calc R . .
H8B H -0.0024 0.8693 0.1363 0.181 Uiso 1 1 calc R . .
H8C H 0.0287 0.9140 0.1523 0.181 Uiso 1 1 calc R . .
C41 C 0.3724(8) 0.7693(4) 0.0087(4) 0.095(4) Uani 1 1 d . D .
H41 H 0.3824 0.7690 -0.0246 0.114 Uiso 1 1 calc R . .
C73 C 0.3453(8) 0.5026(4) 0.3888(4) 0.094(4) Uani 1 1 d . . .
C74 C -0.1612(6) 0.6026(5) 0.1055(5) 0.105(4) Uani 1 1 d . . .
C75 C 0.4537(11) 0.6090(5) -0.0087(5) 0.119(6) Uani 1 1 d . . .
H75 H 0.4526 0.6033 -0.0436 0.143 Uiso 1 1 calc R . .
C76 C 0.5786(9) 0.6596(6) 0.1001(7) 0.125(5) Uani 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
O9A N7A 1.099(17) . ?
O9B N7B 1.244(9) . ?
F6B C16 1.385(16) . ?
F4A C16 1.210(14) . ?
F19B C16 1.379(16) . ?
F2A C37 1.231(19) . ?
F3B C37 1.369(15) . ?
F11A C74 1.532(17) . ?
F13A C74 1.369(15) . ?
F8A C57 1.346(19) . ?
F8A F21A 1.75(2) . ?
F21A C57 1.443(19) . ?
C78A C11A 1.28(3) . ?
C78A C11B 1.61(4) . ?
F6A C16 1.380(14) . ?
F4B C16 1.419(14) . ?
F19A C16 1.303(12) . ?
F2B C37 1.440(17) . ?
F3A C37 1.363(15) . ?
F11B C74 1.210(14) . ?
F13B C74 1.475(15) . ?
F8B C57 1.356(17) . ?
F8B F20 1.71(2) . ?
F21B C57 1.133(14) . ?
F21B F20 1.704(18) . ?
C78B C11B 1.11(3) . ?
C78B C11A 1.43(4) . ?
C11A C11B 0.65(3) . ?
C11A C10 1.70(3) . ?
C11B C10 1.55(3) . ?
O1A O1B 0.717(13) . ?
O1A C23 1.263(12) . ?
O1B C23 1.294(12) . ?
C6A C6B 0.86(2) . ?
C6A C5 1.382(19) . ?
C6A C4 1.589(18) . ?
C6B C4 1.68(2) . ?
C6B C5 1.87(2) . ?
F14A F14B 0.822(14) . ?
F14A C73 1.514(17) . ?
F14B C73 1.317(12) . ?
C57 C55 1.514(17) . ?
C57 F20 1.57(2) . ?
N7A O8 1.228(19) . ?
N7A O7A 1.253(10) . ?
N7B O8 1.262(9) . ?
N7B O7B 1.293(13) . ?
O6 C64 1.247(9) . ?
O4 C44 1.252(8) . ?
N6 C65 1.335(9) . ?
N6 C34 1.462(8) . ?
F12 C74 1.307(15) . ?
N2 C44 1.313(9) . ?
N2 C32 1.465(9) . ?
O2 C65 1.235(9) . ?
C44 C46 1.468(11) . ?
N8 C2 1.506(10) . ?
N8 C9 1.512(10) . ?
N8 C15 1.522(10) . ?
N8 C3 1.530(10) . ?
N3 C50 1.314(9) . ?
N3 C35 1.463(9) . ?
F010 C73 1.331(11) . ?
N4 C64 1.340(10) . ?
N4 C31 1.458(9) . ?
C30 C29 1.393(10) . ?
C30 C26 1.408(10) . ?
C30 C31 1.526(10) . ?
C27 C28 1.396(9) . ?
C27 C29 1.397(10) . ?
C27 C34 1.524(10) . ?
C35 C29 1.528(10) . ?
C25 C26 1.390(10) . ?
C25 C28 1.407(10) . ?
C25 C33 1.516(10) . ?
C33 N1 1.452(9) . ?
C32 C28 1.521(10) . ?
N1 C36 1.295(10) . ?
C63 C58 1.390(10) . ?
C63 C62 1.404(11) . ?
C63 C64 1.481(11) . ?
N5 C23 1.293(9) . ?
N5 C24 1.451(9) . ?
C26 C24 1.526(10) . ?
C69 C70 1.366(12) . ?
C69 C71 1.372(11) . ?
C69 C73 1.462(15) . ?
O5 C50 1.228(9) . ?
C71 C66 1.400(11) . ?
C71 C65 1.487(11) . ?
F17 C76 1.330(17) . ?
F15 C73 1.379(13) . ?
C4 C3 1.542(12) . ?
C38 C43 1.356(12) . ?
C38 C39 1.372(12) . ?
C38 C36 1.512(12) . ?
C15 C14 1.542(12) . ?
O3 C36 1.219(9) . ?
C14 C13 1.517(12) . ?
C2 C1 1.507(13) . ?
C46 C45 1.371(11) . ?
C46 C49 1.411(13) . ?
C62 C61 1.385(12) . ?
C62 C74 1.502(15) . ?
C50 C56 1.489(12) . ?
C68 C70 1.356(13) . ?
C68 C67 1.401(13) . ?
C66 C67 1.362(11) . ?
C23 C22 1.518(11) . ?
C9 C10 1.520(13) . ?
C19 C21 1.365(11) . ?
C19 C20 1.373(12) . ?
C21 C22 1.404(12) . ?
C45 C47 1.373(13) . ?
C22 C17 1.364(11) . ?
C61 C60 1.399(13) . ?
C59 C60 1.342(12) . ?
C59 C58 1.388(11) . ?
F16 C76 1.357(15) . ?
C52 C53 1.361(16) . ?
C52 C51 1.375(14) . ?
C55 C54 1.377(13) . ?
C55 C56 1.398(12) . ?
C56 C51 1.403(12) . ?
C1 C7 1.475(13) . ?
C20 C18 1.343(12) . ?
C18 C17 1.407(12) . ?
C39 C40 1.408(13) . ?
C39 C37 1.487(15) . ?
F1 C37 1.317(12) . ?
C17 C16 1.460(14) . ?
C47 C75 1.389(17) . ?
C7 C8 1.469(14) . ?
C43 C42 1.387(13) . ?
F18 C76 1.324(13) . ?
C49 C48 1.365(15) . ?
C49 C76 1.500(19) . ?
C12 C13 1.535(16) . ?
C53 C54 1.360(16) . ?
C42 C41 1.361(15) . ?
C48 C75 1.346(18) . ?
C40 C41 1.351(15) . ?

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
C57 F8A F21A 53.7(10) . . ?
C57 F21A F8A 48.7(9) . . ?
C11A C78A C11B 22.6(15) . . ?
C57 F8B F20 60.2(9) . . ?
C57 F21B F20 63.4(9) . . ?
C11B C78B C11A 26.3(18) . . ?
C11B C11A C78A 109(4) . . ?
C11B C11A C78B 49(4) . . ?
C78A C11A C78B 67.7(18) . . ?
C11B C11A C10 65(4) . . ?
C78A C11A C10 113.9(18) . . ?
C78B C11A C10 105.3(19) . . ?
C11A C11B C78B 105(5) . . ?
C11A C11B C10 92(4) . . ?
C78B C11B C10 139(3) . . ?
C11A C11B C78A 49(3) . . ?
C78B C11B C78A 64(2) . . ?
C10 C11B C78A 105.3(18) . . ?
O1B O1A C23 76.1(15) . . ?
O1A O1B C23 71.4(14) . . ?
C6B C6A C5 111(2) . . ?
C6B C6A C4 80(2) . . ?
C5 C6A C4 118.6(12) . . ?
C6A C6B C4 69.3(19) . . ?
C6A C6B C5 43.8(16) . . ?
C4 C6B C5 92.3(12) . . ?
F14B F14A C73 60.3(13) . . ?
F14A F14B C73 86.9(15) . . ?
F21B C57 F8A 122.8(15) . . ?
F21B C57 F8B 116.5(13) . . ?
F8A C57 F8B 33.1(8) . . ?
F21B C57 F21A 79.4(12) . . ?
F8A C57 F21A 77.6(13) . . ?
F8B C57 F21A 108.3(13) . . ?
F21B C57 C55 126.8(13) . . ?
F8A C57 C55 108.8(13) . . ?
F8B C57 C55 113.5(12) . . ?
F21A C57 C55 101.4(11) . . ?
F21B C57 F20 76.4(11) . . ?
F8A C57 F20 104.0(14) . . ?
F8B C57 F20 71.1(10) . . ?
F21A C57 F20 152.0(15) . . ?
C55 C57 F20 104.3(11) . . ?
C57 F20 F21B 40.2(7) . . ?
C57 F20 F8B 48.7(8) . . ?
F21B F20 F8B 76.8(8) . . ?
O9A N7A O8 119.4(14) . . ?
O9A N7A O7A 128(2) . . ?
O8 N7A O7A 112.0(18) . . ?
O9B N7B O8 116.5(11) . . ?
O9B N7B O7B 114.9(10) . . ?
O8 N7B O7B 128.4(12) . . ?
C65 N6 C34 123.6(6) . . ?
C44 N2 C32 123.5(6) . . ?
O4 C44 N2 122.1(7) . . ?
O4 C44 C46 119.4(8) . . ?
N2 C44 C46 118.4(8) . . ?
C2 N8 C9 112.5(7) . . ?
C2 N8 C15 105.0(6) . . ?
C9 N8 C15 111.0(6) . . ?
C2 N8 C3 111.9(6) . . ?
C9 N8 C3 105.1(6) . . ?
C15 N8 C3 111.5(7) . . ?
C50 N3 C35 125.0(6) . . ?
C64 N4 C31 121.2(6) . . ?
C29 C30 C26 119.1(7) . . ?
C29 C30 C31 121.5(7) . . ?
C26 C30 C31 119.2(7) . . ?
C28 C27 C29 120.0(7) . . ?
C28 C27 C34 118.3(7) . . ?
C29 C27 C34 121.6(7) . . ?
N7A O8 N7B 36.7(8) . . ?
N3 C35 C29 106.0(5) . . ?
C26 C25 C28 119.6(6) . . ?
C26 C25 C33 120.4(7) . . ?
C28 C25 C33 119.7(7) . . ?
N1 C33 C25 108.4(6) . . ?
N2 C32 C28 111.5(6) . . ?
N4 C31 C30 112.3(6) . . ?
C36 N1 C33 124.6(6) . . ?
C27 C28 C25 119.8(7) . . ?
C27 C28 C32 118.9(7) . . ?
C25 C28 C32 121.1(7) . . ?
C58 C63 C62 118.3(7) . . ?
C58 C63 C64 120.3(8) . . ?
C62 C63 C64 121.2(8) . . ?
N6 C34 C27 114.0(5) . . ?
C23 N5 C24 124.5(6) . . ?
C30 C29 C27 120.5(6) . . ?
C30 C29 C35 119.7(7) . . ?
C27 C29 C35 119.0(7) . . ?
C25 C26 C30 120.7(7) . . ?
C25 C26 C24 121.3(7) . . ?
C30 C26 C24 117.9(7) . . ?
C70 C69 C71 123.8(8) . . ?
C70 C69 C73 115.8(9) . . ?
C71 C69 C73 120.4(9) . . ?
C69 C71 C66 116.5(7) . . ?
C69 C71 C65 125.4(8) . . ?
C66 C71 C65 118.0(8) . . ?
N5 C24 C26 112.5(6) . . ?
C3 C4 C6A 112.1(9) . . ?
C3 C4 C6B 97.0(9) . . ?
C6A C4 C6B 30.3(7) . . ?
C43 C38 C39 117.2(9) . . ?
C43 C38 C36 117.3(9) . . ?
C39 C38 C36 125.5(9) . . ?
N8 C15 C14 115.1(7) . . ?
C13 C14 C15 109.1(7) . . ?
N8 C2 C1 114.5(7) . . ?
C45 C46 C49 116.6(9) . . ?
C45 C46 C44 118.7(8) . . ?
C49 C46 C44 124.5(9) . . ?
O6 C64 N4 121.7(7) . . ?
O6 C64 C63 121.3(8) . . ?
N4 C64 C63 117.0(8) . . ?
C61 C62 C63 119.8(9) . . ?
C61 C62 C74 119.9(9) . . ?
C63 C62 C74 120.0(8) . . ?
O5 C50 N3 124.2(7) . . ?
O5 C50 C56 122.3(8) . . ?
N3 C50 C56 113.2(8) . . ?
O2 C65 N6 123.5(7) . . ?
O2 C65 C71 121.9(8) . . ?
N6 C65 C71 114.4(8) . . ?
C70 C68 C67 120.3(9) . . ?
C67 C66 C71 121.1(8) . . ?
O3 C36 N1 123.8(8) . . ?
O3 C36 C38 120.2(9) . . ?
N1 C36 C38 115.8(8) . . ?
O1A C23 N5 125.2(8) . . ?
O1A C23 O1B 32.5(6) . . ?
N5 C23 O1B 121.9(8) . . ?
O1A C23 C22 116.2(8) . . ?
N5 C23 C22 116.7(6) . . ?
O1B C23 C22 117.5(8) . . ?
N8 C9 C10 114.9(7) . . ?
C21 C19 C20 118.6(9) . . ?
C19 C21 C22 122.2(8) . . ?
C46 C45 C47 122.1(9) . . ?
C17 C22 C21 117.1(8) . . ?
C17 C22 C23 125.0(9) . . ?
C21 C22 C23 117.9(8) . . ?
C62 C61 C60 120.0(9) . . ?
C60 C59 C58 120.2(9) . . ?
N8 C3 C4 114.2(6) . . ?
C59 C58 C63 121.2(8) . . ?
C53 C52 C51 118.7(10) . . ?
C68 C70 C69 118.6(9) . . ?
C54 C55 C56 122.5(10) . . ?
C54 C55 C57 120.2(12) . . ?
C56 C55 C57 117.3(10) . . ?
C55 C56 C51 116.1(8) . . ?
C55 C56 C50 124.5(8) . . ?
C51 C56 C50 119.4(9) . . ?
C7 C1 C2 112.9(9) . . ?
C18 C20 C19 121.5(8) . . ?
C20 C18 C17 119.6(9) . . ?
C38 C39 C40 121.4(10) . . ?
C38 C39 C37 119.3(10) . . ?
C40 C39 C37 119.3(11) . . ?
C66 C67 C68 119.6(9) . . ?
C22 C17 C18 120.9(8) . . ?
C22 C17 C16 120.4(9) . . ?
C18 C17 C16 118.7(9) . . ?
C52 C51 C56 121.8(10) . . ?
C45 C47 C75 119.1(11) . . ?
C8 C7 C1 115.5(10) . . ?
C38 C43 C42 122.3(10) . . ?
C9 C10 C11B 116.9(14) . . ?
C9 C10 C11A 96.6(11) . . ?
C11B C10 C11A 22.6(11) . . ?
C48 C49 C46 121.6(11) . . ?
C48 C49 C76 118.3(13) . . ?
C46 C49 C76 120.0(11) . . ?
C54 C53 C52 122.7(11) . . ?
C41 C42 C43 119.5(10) . . ?
C14 C13 C12 110.3(8) . . ?
C59 C60 C61 120.5(9) . . ?
C75 C48 C49 120.0(13) . . ?
F2A C37 F1 118.9(15) . . ?
F2A C37 F3A 69.0(12) . . ?
F1 C37 F3A 113.3(12) . . ?
F2A C37 F3B 104.9(14) . . ?
F1 C37 F3B 94.3(10) . . ?
F3A C37 F3B 35.9(6) . . ?
F2A C37 F2B 33.6(10) . . ?
F1 C37 F2B 91.2(10) . . ?
F3A C37 F2B 96.9(12) . . ?
F3B C37 F2B 129.5(14) . . ?
F2A C37 C39 112.3(13) . . ?
F1 C37 C39 114.3(11) . . ?
F3A C37 C39 121.9(10) . . ?
F3B C37 C39 109.8(11) . . ?
F2B C37 C39 113.2(10) . . ?
F4A C16 F19A 115.2(13) . . ?
F4A C16 F19B 112.2(12) . . ?
F19A C16 F19B 41.3(6) . . ?
F4A C16 F6A 52.6(8) . . ?
F19A C16 F6A 101.7(10) . . ?
F19B C16 F6A 135.2(13) . . ?
F4A C16 F6B 103.5(12) . . ?
F19A C16 F6B 52.6(7) . . ?
F19B C16 F6B 93.9(10) . . ?
F6A C16 F6B 58.5(8) . . ?
F4A C16 F4B 47.6(7) . . ?
F19A C16 F4B 101.1(10) . . ?
F19B C16 F4B 72.9(9) . . ?
F6A C16 F4B 99.4(9) . . ?
F6B C16 F4B 132.7(12) . . ?
F4A C16 C17 120.9(11) . . ?
F19A C16 C17 123.8(9) . . ?
F19B C16 C17 109.5(10) . . ?
F6A C16 C17 113.8(9) . . ?
F6B C16 C17 113.5(10) . . ?
F4B C16 C17 113.7(9) . . ?
C53 C54 C55 118.1(11) . . ?
C41 C40 C39 119.3(10) . . ?
C6A C5 C6B 25.4(9) . . ?
C40 C41 C42 120.2(10) . . ?
F14B C73 F010 110.3(10) . . ?
F14B C73 F15 90.0(10) . . ?
F010 C73 F15 104.5(10) . . ?
F14B C73 C69 118.0(11) . . ?
F010 C73 C69 116.3(10) . . ?
F15 C73 C69 114.0(9) . . ?
F14B C73 F14A 32.8(6) . . ?
F010 C73 F14A 95.6(10) . . ?
F15 C73 F14A 122.6(11) . . ?
C69 C73 F14A 103.1(11) . . ?
F11B C74 F12 99.6(12) . . ?
F11B C74 F13A 84.1(11) . . ?
F12 C74 F13A 123.0(14) . . ?
F11B C74 F13B 102.9(11) . . ?
F12 C74 F13B 95.1(12) . . ?
F13A C74 F13B 31.1(6) . . ?
F11B C74 C62 126.7(15) . . ?
F12 C74 C62 115.5(9) . . ?
F13A C74 C62 105.8(11) . . ?
F13B C74 C62 111.9(9) . . ?
F11B C74 F11A 24.2(8) . . ?
F12 C74 F11A 114.6(10) . . ?
F13A C74 F11A 91.4(11) . . ?
F13B C74 F11A 118.0(10) . . ?
C62 C74 F11A 102.6(11) . . ?
C48 C75 C47 120.6(11) . . ?
F18 C76 F17 108.7(15) . . ?
F18 C76 F16 104.6(12) . . ?
F17 C76 F16 104.7(14) . . ?
F18 C76 C49 111.6(14) . . ?
F17 C76 C49 114.5(12) . . ?
F16 C76 C49 112.1(14) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        19.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 944135'
#######################################################################
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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data_CCDC996874
_vrf_                            
;
PROBLEM:
THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.4660
RESPONSE:
The 2theta value was found to be low after repetitive attempt;
PROBLEM:
PLAT223_ALERT_4_A Large Solvent/Anion H Ueq(max)/Ueq(min) ... 7.5 Ratio
RESPONSE:
It is originating due hydrogen assignment of the water molecule O14;
PROBLEMM:
PLAT430_ALERT_2_A Short Inter D...A Contact O15 .. O15 .. 1.84 Ang.
RESPONSE:
It is arisinng due to high thermal parameter on O15 atom; 
See _publ_section_exptl_refinement
PROBLEM:
DIFMX01_ALERT_2_B The maximum difference density is > 0.1*ZMAX*1.00
_refine_diff_density_max given = 1.523
Test value = 0.900
RESPONSE:
It is arising due to high residual density value
which can not be reduced further after SQUEEZE 
and disorder treatment; 
PROBLEM:
PLAT097_ALERT_2_B Large Reported Max. (Positive) Residual Density 1.52 eA-3
RESPONSE:
Even after SQUEEZE treatment the residual density is high;
See _publ_section_exptl_refinement
PROBLEM:
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1 Report
RESPONSE:
The alert is due to presence of disordered O16 and O17 atoms in the struture;
PROBLEM:
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) ....... O11 Check
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) ....... O15 Check
RESPONSE:
We can not locate hydrogen after increasing the Q peak numbers in XShell;
PROBLEM:
PLAT340_ALERT_3_B Low Bond Precision on C-C Bonds ............... 0.0143 Ang.
RESPONSE:
The precision obtained is optimum in this case;
PROBLEM:
PLAT417_ALERT_2_B Short Inter D-H..H-D H2 .. H111 .. 2.07 Ang.
PLAT431_ALERT_2_B Short Inter HL..A Contact F17 .. O15 .. 2.51 Ang.
PLAT431_ALERT_2_B Short Inter HL..A Contact F17 .. O11 .. 2.61 Ang.
PLAT431_ALERT_2_B Short Inter HL..A Contact F17 .. O15 .. 2.68 Ang.
RESPONSE:
It is originating in the water cluster though O11 is well
refined. O15 has high thermal value;
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H135 F20 N8 O17'
_chemical_formula_weight         2149.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   19.984(2)
_cell_length_b                   21.583(2)
_cell_length_c                   31.956(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.776(3)
_cell_angle_gamma                90.00
_cell_volume                     13327(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9893
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      18.57

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4524
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9821
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70781
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         19.34
_reflns_number_total             11220
_reflns_number_gt                8505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 3.2'
_computing_publication_material  'ORTEP 3v.2'

_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. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.013 0.000 0.000 1504 343 ' '
2 0.129 0.500 0.500 1504 342 ' '
_platon_squeeze_details          
;
The unit cell contains water and dioxane molecules which have been treated  as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_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)+(0.1724P)²+42.6648P] 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         11220
_refine_ls_number_parameters     1350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.2919
_refine_ls_wR_factor_gt          0.2778
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
O16 O 0.5598(6) 0.0575(5) 0.1664(4) 0.080(3) Uiso 0.60 1 d P A 1
O17 O 0.5209(8) 0.9654(8) 0.1956(5) 0.093(5) Uiso 0.44 1 d P B 1
O16A O 0.5639(10) 0.0255(9) 0.1337(6) 0.095(6) Uiso 0.40 1 d P C 2
O17A O 0.5211(6) 0.9347(6) 0.1591(4) 0.087(4) Uiso 0.56 1 d P D 2
C102 C 0.4974(11) 0.4879(9) 0.2857(6) 0.179(7) Uiso 1 1 d . . .
C7 C 1.0793(4) 0.4739(3) 0.1811(2) 0.035(2) Uani 1 1 d . . .
H7A H 1.1158 0.4842 0.2066 0.042 Uiso 1 1 calc R . .
H7B H 1.0629 0.4326 0.1852 0.042 Uiso 1 1 calc R . .
C5 C 1.0201(4) 0.5196(3) 0.1770(2) 0.0268(18) Uani 1 1 d . . .
C3 C 0.9008(3) 0.5420(4) 0.1760(2) 0.0274(19) Uani 1 1 d . . .
C4 C 0.9527(4) 0.4991(3) 0.1759(2) 0.0290(19) Uani 1 1 d . . .
C46 C 1.1991(4) 0.4615(3) 0.1073(2) 0.0304(19) Uani 1 1 d . . .
C30 C 0.7008(4) 0.4406(4) 0.0868(2) 0.036(2) Uani 1 1 d . . .
C1 C 0.9799(3) 0.6268(3) 0.1719(2) 0.0244(18) Uani 1 1 d . . .
C11 C 0.8587(4) 0.6524(4) 0.1752(2) 0.035(2) Uani 1 1 d . . .
H11A H 0.8439 0.6468 0.2016 0.042 Uiso 1 1 calc R . .
H11B H 0.8774 0.6939 0.1755 0.042 Uiso 1 1 calc R . .
C6 C 1.0337(4) 0.5842(4) 0.1746(2) 0.031(2) Uani 1 1 d . . .
C29 C 0.7394(4) 0.4565(4) 0.1326(3) 0.040(2) Uani 1 1 d . . .
C28 C 0.8308(4) 0.5204(4) 0.1780(2) 0.035(2) Uani 1 1 d . . .
H28A H 0.8358 0.4874 0.1991 0.042 Uiso 1 1 calc R . .
H28B H 0.8064 0.5544 0.1875 0.042 Uiso 1 1 calc R . .
C52 C 1.1542(3) 0.6773(4) 0.0776(2) 0.0283(18) Uani 1 1 d . . .
C51 C 1.1604(4) 0.4354(4) 0.0704(3) 0.043(2) Uani 1 1 d . . .
H51 H 1.1173 0.4191 0.0704 0.052 Uiso 1 1 calc R . .
C35 C 0.6921(4) 0.3805(4) 0.0715(3) 0.041(2) Uani 1 1 d . . .
C9 C 1.1051(3) 0.6057(3) 0.1746(2) 0.0296(19) Uani 1 1 d . . .
H9A H 1.1175 0.6408 0.1941 0.035 Uiso 1 1 calc R . .
H9B H 1.1379 0.5727 0.1854 0.035 Uiso 1 1 calc R . .
C8 C 0.9376(4) 0.4303(4) 0.1745(2) 0.040(2) Uani 1 1 d . . .
H8A H 0.9682 0.4110 0.1996 0.048 Uiso 1 1 calc R . .
H8B H 0.8905 0.4243 0.1766 0.048 Uiso 1 1 calc R . .
C2 C 0.9142(4) 0.6062(3) 0.1741(2) 0.0300(19) Uani 1 1 d . . .
C10 C 0.9915(4) 0.6942(3) 0.1667(2) 0.036(2) Uani 1 1 d . . .
H10A H 0.9772 0.7171 0.1890 0.044 Uiso 1 1 calc R . .
H10B H 1.0405 0.7016 0.1703 0.044 Uiso 1 1 calc R . .
C13 C 0.9168(4) 0.7691(4) 0.1189(3) 0.046(2) Uani 1 1 d . . .
C43 C 0.9811(4) 0.2542(4) 0.0874(3) 0.050(2) Uani 1 1 d . . .
C37 C 0.9809(4) 0.3472(4) 0.1371(3) 0.0329(19) Uani 1 1 d . . .
C45 C 1.1745(4) 0.4577(3) 0.1486(3) 0.033(2) Uani 1 1 d . . .
C53 C 1.1681(4) 0.6258(4) 0.0561(3) 0.038(2) Uani 1 1 d . . .
H53 H 1.1701 0.5870 0.0690 0.045 Uiso 1 1 calc R . .
C39 C 1.0001(4) 0.3562(4) 0.0641(3) 0.041(2) Uani 1 1 d . . .
H39 H 1.0003 0.3989 0.0677 0.049 Uiso 1 1 calc R . .
C22 C 0.6837(5) 0.6685(5) 0.0611(4) 0.067(3) Uani 1 1 d . . .
H22 H 0.7266 0.6799 0.0572 0.080 Uiso 1 1 calc R . .
C57 C 1.1492(4) 0.7331(4) 0.0586(3) 0.041(2) Uani 1 1 d . . .
C31 C 0.6701(4) 0.4879(4) 0.0599(3) 0.042(2) Uani 1 1 d . . .
H31 H 0.6767 0.5284 0.0701 0.050 Uiso 1 1 calc R . .
C48 C 1.2851(4) 0.4823(4) 0.0695(3) 0.052(2) Uani 1 1 d . . .
H48 H 1.3276 0.4995 0.0691 0.062 Uiso 1 1 calc R . .
C21 C 0.6776(4) 0.6557(3) 0.1011(3) 0.038(2) Uani 1 1 d . . .
C33 C 0.6225(4) 0.4191(6) 0.0029(3) 0.054(2) Uani 1 1 d . . .
H33 H 0.5970 0.4115 -0.0253 0.065 Uiso 1 1 calc R . .
C14 C 0.8777(4) 0.7849(4) 0.0735(3) 0.049(2) Uani 1 1 d . . .
C49 C 1.2469(5) 0.4555(4) 0.0332(3) 0.048(2) Uani 1 1 d . . .
H49 H 1.2637 0.4527 0.0087 0.058 Uiso 1 1 calc R . .
C44 C 0.9598(7) 0.2099(5) 0.1167(4) 0.078(3) Uani 1 1 d . . .
C32 C 0.6300(4) 0.4779(5) 0.0183(3) 0.047(2) Uani 1 1 d . . .
H32 H 0.6087 0.5108 0.0013 0.057 Uiso 1 1 calc R . .
C47 C 1.2639(4) 0.4853(3) 0.1074(2) 0.0321(19) Uani 1 1 d . . .
C38 C 0.9864(4) 0.3199(4) 0.0954(3) 0.040(2) Uani 1 1 d . . .
C41 C 1.0132(4) 0.2706(6) 0.0205(3) 0.066(3) Uani 1 1 d . . .
H41 H 1.0244 0.2544 -0.0038 0.079 Uiso 1 1 calc R . .
C50 C 1.1821(5) 0.4321(4) 0.0329(3) 0.052(2) Uani 1 1 d . . .
H50 H 1.1541 0.4145 0.0079 0.063 Uiso 1 1 calc R . .
C54 C 1.1790(4) 0.6315(5) 0.0156(3) 0.047(2) Uani 1 1 d . . .
H54 H 1.1889 0.5967 0.0011 0.056 Uiso 1 1 calc R . .
C40 C 1.0137(4) 0.3325(5) 0.0268(3) 0.059(3) Uani 1 1 d . . .
H40 H 1.0231 0.3591 0.0062 0.070 Uiso 1 1 calc R . .
C56 C 1.1591(4) 0.7391(5) 0.0174(3) 0.051(2) Uani 1 1 d . . .
H56 H 1.1547 0.7776 0.0039 0.061 Uiso 1 1 calc R . .
C42 C 0.9959(5) 0.2315(4) 0.0502(4) 0.062(3) Uani 1 1 d . . .
H42 H 0.9941 0.1890 0.0452 0.074 Uiso 1 1 calc R . .
C34 C 0.6528(5) 0.3705(5) 0.0289(3) 0.056(3) Uani 1 1 d . . .
H34 H 0.6471 0.3304 0.0180 0.067 Uiso 1 1 calc R . .
C16 C 0.8009(6) 0.7509(6) 0.0077(4) 0.078(3) Uani 1 1 d . . .
H16 H 0.7760 0.7185 -0.0082 0.094 Uiso 1 1 calc R . .
C15 C 0.8410(5) 0.7398(5) 0.0481(3) 0.056(2) Uani 1 1 d . . .
H15 H 0.8434 0.6996 0.0588 0.068 Uiso 1 1 calc R . .
C12 C 0.7367(4) 0.6672(4) 0.1403(3) 0.039(2) Uani 1 1 d . . .
C18 C 0.8329(7) 0.8566(7) 0.0145(4) 0.106(5) Uani 1 1 d . . .
H18 H 0.8297 0.8965 0.0032 0.127 Uiso 1 1 calc R . .
C26 C 0.6132(5) 0.6348(4) 0.1059(3) 0.059(3) Uani 1 1 d . . .
C27 C 0.6016(5) 0.6167(6) 0.1476(4) 0.077(3) Uani 1 1 d . . .
C58 C 1.1283(5) 0.7911(5) 0.0788(3) 0.064(3) Uani 1 1 d . . .
C36 C 0.7238(5) 0.3261(4) 0.0979(3) 0.053(2) Uani 1 1 d . . .
C19 C 0.8750(6) 0.8450(5) 0.0562(3) 0.070(3) Uani 1 1 d . . .
C25 C 0.5575(5) 0.6291(6) 0.0689(5) 0.086(3) Uani 1 1 d . . .
H25 H 0.5150 0.6145 0.0716 0.103 Uiso 1 1 calc R . .
C55 C 1.1755(4) 0.6875(6) -0.0031(3) 0.058(3) Uani 1 1 d . . .
H55 H 1.1842 0.6913 -0.0302 0.070 Uiso 1 1 calc R . .
C24 C 0.5656(6) 0.6451(6) 0.0294(4) 0.088(4) Uani 1 1 d . . .
H24 H 0.5287 0.6424 0.0049 0.105 Uiso 1 1 calc R . .
C20 C 0.9129(8) 0.8955(7) 0.0789(5) 0.109(4) Uani 1 1 d . . .
C17 C 0.7963(7) 0.8087(8) -0.0098(4) 0.103(4) Uani 1 1 d . . .
H17 H 0.7691 0.8159 -0.0377 0.123 Uiso 1 1 calc R . .
C23 C 0.6286(7) 0.6650(6) 0.0263(4) 0.090(4) Uani 1 1 d . . .
H23 H 0.6341 0.6767 -0.0007 0.108 Uiso 1 1 calc R . .
N1 N 0.7980(3) 0.6458(3) 0.13727(19) 0.0376(16) Uani 1 1 d . . .
H1 H 0.8022 0.6285 0.1138 0.045 Uiso 1 1 calc R . .
N4 N 1.1078(3) 0.4738(3) 0.14332(18) 0.0323(16) Uani 1 1 d . . .
H4 H 1.0824 0.4838 0.1182 0.039 Uiso 1 1 calc R . .
N3 N 0.9460(3) 0.3990(3) 0.13553(18) 0.0343(16) Uani 1 1 d . . .
H3 H 0.9273 0.4152 0.1107 0.041 Uiso 1 1 calc R . .
N2 N 0.7899(3) 0.4980(3) 0.13585(19) 0.0357(16) Uani 1 1 d . . .
H2 H 0.7988 0.5119 0.1126 0.043 Uiso 1 1 calc R . .
N5 N 1.1098(3) 0.6237(3) 0.13144(17) 0.0300(15) Uani 1 1 d . . .
H5 H 1.0849 0.6046 0.1093 0.036 Uiso 1 1 calc R . .
N6 N 0.9537(3) 0.7167(3) 0.12475(19) 0.0374(16) Uani 1 1 d . . .
H6 H 0.9549 0.6952 0.1023 0.045 Uiso 1 1 calc R . .
O4 O 1.0132(3) 0.3225(2) 0.17154(19) 0.0439(14) Uani 1 1 d . . .
O6 O 0.7288(3) 0.6959(3) 0.1713(2) 0.0516(15) Uani 1 1 d . . .
O3 O 1.2118(3) 0.4399(2) 0.18183(18) 0.0408(14) Uani 1 1 d . . .
O5 O 0.7240(3) 0.4321(3) 0.16412(18) 0.0511(15) Uani 1 1 d . . .
O2 O 1.1844(3) 0.7023(3) 0.15409(17) 0.0495(15) Uani 1 1 d . . .
O1 O 0.9115(3) 0.8018(3) 0.15010(19) 0.0528(15) Uani 1 1 d . . .
F4 F 0.6882(3) 0.3089(2) 0.12560(17) 0.0766(16) Uani 1 1 d . . .
F13 F 1.0816(3) 0.7802(2) 0.10053(18) 0.0722(15) Uani 1 1 d . . .
F6 F 0.7890(3) 0.3370(2) 0.12001(17) 0.0690(14) Uani 1 1 d . . .
F7 F 0.9123(3) 0.2337(2) 0.13587(19) 0.0768(16) Uani 1 1 d . . .
F12 F 0.9775(4) 0.8830(3) 0.1053(2) 0.0974(19) Uani 1 1 d . . .
F2 F 0.6539(3) 0.5810(3) 0.17156(17) 0.0748(15) Uani 1 1 d . . .
F15 F 1.1804(3) 0.8204(2) 0.10531(17) 0.0802(17) Uani 1 1 d . . .
F14 F 1.1007(3) 0.8345(2) 0.04847(19) 0.0894(18) Uani 1 1 d . . .
F5 F 0.7273(3) 0.2760(2) 0.07408(17) 0.0744(15) Uani 1 1 d . . .
F8 F 0.9307(3) 0.1595(2) 0.0954(2) 0.099(2) Uani 1 1 d . . .
F3 F 0.5940(3) 0.6626(3) 0.17385(19) 0.0902(19) Uani 1 1 d . . .
F10 F 0.8822(4) 0.9238(3) 0.1085(3) 0.121(3) Uani 1 1 d . . .
F9 F 1.0126(3) 0.1899(2) 0.14915(19) 0.0897(18) Uani 1 1 d . . .
F1 F 0.5449(3) 0.5816(3) 0.1442(2) 0.104(2) Uani 1 1 d . . .
F11 F 0.9242(5) 0.9437(3) 0.0546(3) 0.154(3) Uani 1 1 d . . .
N7 N 0.2070(3) 0.2828(3) 0.2391(2) 0.0440(18) Uani 1 1 d . . .
N8 N 0.7080(3) 0.3575(3) 0.2792(2) 0.0436(18) Uani 1 1 d . . .
C86 C 0.6659(4) 0.2992(4) 0.2636(3) 0.050(2) Uani 1 1 d . . .
H86A H 0.6934 0.2636 0.2762 0.060 Uiso 1 1 calc R . .
H86B H 0.6251 0.2998 0.2748 0.060 Uiso 1 1 calc R . .
C71 C 0.1772(4) 0.3380(4) 0.2575(3) 0.050(2) Uani 1 1 d . . .
H71A H 0.1876 0.3749 0.2431 0.060 Uiso 1 1 calc R . .
H71B H 0.1272 0.3335 0.2500 0.060 Uiso 1 1 calc R . .
C75 C 0.6642(5) 0.4165(4) 0.2669(3) 0.067(3) Uani 1 1 d . . .
H75A H 0.6911 0.4515 0.2811 0.080 Uiso 1 1 calc R . .
H75B H 0.6561 0.4228 0.2359 0.080 Uiso 1 1 calc R . .
C67 C 0.1872(4) 0.2228(4) 0.2572(3) 0.046(2) Uani 1 1 d . . .
H67A H 0.2110 0.2204 0.2877 0.055 Uiso 1 1 calc R . .
H67B H 0.2031 0.1885 0.2427 0.055 Uiso 1 1 calc R . .
C64 C 0.1972(4) 0.2341(4) 0.1650(3) 0.057(2) Uani 1 1 d . . .
H64A H 0.1659 0.2000 0.1656 0.068 Uiso 1 1 calc R . .
H64B H 0.2440 0.2198 0.1776 0.068 Uiso 1 1 calc R . .
C59 C 0.2860(4) 0.2821(4) 0.2533(3) 0.049(2) Uani 1 1 d . . .
H59A H 0.3004 0.2817 0.2847 0.059 Uiso 1 1 calc R . .
H59B H 0.3023 0.2439 0.2432 0.059 Uiso 1 1 calc R . .
C63 C 0.1811(4) 0.2863(4) 0.1910(3) 0.050(2) Uani 1 1 d . . .
H63A H 0.1312 0.2907 0.1841 0.060 Uiso 1 1 calc R . .
H63B H 0.1994 0.3238 0.1814 0.060 Uiso 1 1 calc R . .
C79 C 0.7752(5) 0.4022(4) 0.3507(3) 0.067(3) Uani 1 1 d . . .
H79A H 0.7477 0.4395 0.3489 0.080 Uiso 1 1 calc R . .
H79B H 0.8126 0.4103 0.3372 0.080 Uiso 1 1 calc R . .
C68 C 0.1093(4) 0.2154(4) 0.2524(3) 0.056(2) Uani 1 1 d . . .
H68A H 0.0838 0.2245 0.2229 0.067 Uiso 1 1 calc R . .
H68B H 0.0941 0.2439 0.2716 0.067 Uiso 1 1 calc R . .
C78 C 0.7315(4) 0.3508(4) 0.3277(3) 0.055(2) Uani 1 1 d . . .
H78A H 0.6909 0.3474 0.3389 0.066 Uiso 1 1 calc R . .
H78B H 0.7573 0.3125 0.3344 0.066 Uiso 1 1 calc R . .
C61 C 0.4017(5) 0.3320(5) 0.2561(3) 0.087(3) Uani 1 1 d . . .
H61A H 0.4175 0.2903 0.2525 0.105 Uiso 1 1 calc R . .
H61B H 0.4245 0.3603 0.2406 0.105 Uiso 1 1 calc R . .
C83 C 0.8197(4) 0.3121(4) 0.2683(3) 0.058(3) Uani 1 1 d . . .
H83A H 0.7959 0.2728 0.2615 0.069 Uiso 1 1 calc R . .
H83B H 0.8438 0.3120 0.2988 0.069 Uiso 1 1 calc R . .
C65 C 0.1904(5) 0.2535(5) 0.1187(3) 0.067(3) Uani 1 1 d . . .
H65A H 0.1476 0.2764 0.1085 0.080 Uiso 1 1 calc R . .
H65B H 0.1874 0.2166 0.1010 0.080 Uiso 1 1 calc R . .
C82 C 0.7686(5) 0.3634(4) 0.2595(3) 0.061(3) Uani 1 1 d . . .
H82A H 0.7508 0.3671 0.2283 0.073 Uiso 1 1 calc R . .
H82B H 0.7927 0.4017 0.2697 0.073 Uiso 1 1 calc R . .
C76 C 0.5945(5) 0.4170(5) 0.2781(4) 0.091(4) Uani 1 1 d . . .
H76A H 0.5630 0.3887 0.2591 0.109 Uiso 1 1 calc R . .
H76B H 0.6005 0.4029 0.3076 0.109 Uiso 1 1 calc R . .
C66 C 0.2502(6) 0.2932(5) 0.1130(3) 0.085(3) Uani 1 1 d . . .
H66A H 0.2586 0.3259 0.1341 0.128 Uiso 1 1 calc R . .
H66B H 0.2387 0.3107 0.0844 0.128 Uiso 1 1 calc R . .
H66C H 0.2909 0.2681 0.1169 0.128 Uiso 1 1 calc R . .
C72 C 0.2016(5) 0.3484(4) 0.3057(3) 0.066(3) Uani 1 1 d . . .
H72A H 0.2494 0.3621 0.3134 0.079 Uiso 1 1 calc R . .
H72B H 0.1987 0.3101 0.3210 0.079 Uiso 1 1 calc R . .
C69 C 0.0957(5) 0.1478(5) 0.2640(4) 0.075(3) Uani 1 1 d . . .
H69A H 0.1025 0.1206 0.2413 0.091 Uiso 1 1 calc R . .
H69B H 0.1294 0.1364 0.2906 0.091 Uiso 1 1 calc R . .
C73 C 0.1560(5) 0.3974(4) 0.3184(3) 0.070(3) Uani 1 1 d . . .
H73A H 0.1086 0.3825 0.3115 0.084 Uiso 1 1 calc R . .
H73B H 0.1571 0.4345 0.3016 0.084 Uiso 1 1 calc R . .
C87 C 0.6428(5) 0.2902(4) 0.2151(3) 0.061(3) Uani 1 1 d . . .
H87A H 0.6195 0.3273 0.2015 0.073 Uiso 1 1 calc R . .
H87B H 0.6828 0.2831 0.2038 0.073 Uiso 1 1 calc R . .
C60 C 0.3209(4) 0.3360(5) 0.2372(3) 0.073(3) Uani 1 1 d . . .
H60A H 0.3039 0.3747 0.2461 0.087 Uiso 1 1 calc R . .
H60B H 0.3098 0.3353 0.2058 0.087 Uiso 1 1 calc R . .
C84 C 0.8723(6) 0.3202(6) 0.2409(3) 0.092(4) Uani 1 1 d . . .
H84A H 0.8481 0.3163 0.2106 0.110 Uiso 1 1 calc R . .
H84B H 0.8914 0.3617 0.2453 0.110 Uiso 1 1 calc R . .
C89 C 0.5702(6) 0.2203(5) 0.1575(4) 0.096(4) Uani 1 1 d . . .
H89A H 0.5509 0.2566 0.1417 0.143 Uiso 1 1 calc R . .
H89B H 0.5356 0.1884 0.1534 0.143 Uiso 1 1 calc R . .
H89C H 0.6087 0.2059 0.1473 0.143 Uiso 1 1 calc R . .
C77 C 0.5636(6) 0.4816(5) 0.2732(5) 0.112(4) Uani 1 1 d . . .
H77A H 0.5970 0.5098 0.2908 0.135 Uiso 1 1 calc R . .
H77B H 0.5562 0.4944 0.2433 0.135 Uiso 1 1 calc R . .
C88 C 0.5943(6) 0.2356(4) 0.2046(3) 0.080(3) Uani 1 1 d . . .
H88A H 0.6174 0.1996 0.2199 0.096 Uiso 1 1 calc R . .
H88B H 0.5541 0.2440 0.2155 0.096 Uiso 1 1 calc R . .
C85 C 0.9292(6) 0.2758(7) 0.2506(4) 0.105(4) Uani 1 1 d . . .
H85A H 0.9523 0.2778 0.2809 0.158 Uiso 1 1 calc R . .
H85B H 0.9614 0.2856 0.2339 0.158 Uiso 1 1 calc R . .
H85C H 0.9114 0.2348 0.2435 0.158 Uiso 1 1 calc R . .
C80 C 0.8064(6) 0.3836(5) 0.4006(3) 0.091(4) Uani 1 1 d . . .
H80A H 0.8258 0.4200 0.4170 0.109 Uiso 1 1 calc R . .
H80B H 0.7698 0.3677 0.4125 0.109 Uiso 1 1 calc R . .
C74 C 0.1786(7) 0.4134(5) 0.3663(4) 0.106(4) Uani 1 1 d . . .
H74A H 0.1752 0.3773 0.3832 0.158 Uiso 1 1 calc R . .
H74B H 0.1492 0.4454 0.3726 0.158 Uiso 1 1 calc R . .
H74C H 0.2256 0.4278 0.3735 0.158 Uiso 1 1 calc R . .
C70 C 0.0242(8) 0.1378(7) 0.2698(5) 0.142(6) Uani 1 1 d . . .
H70A H 0.0178 0.1631 0.2932 0.213 Uiso 1 1 calc R . .
H70B H 0.0186 0.0950 0.2764 0.213 Uiso 1 1 calc R . .
H70C H -0.0094 0.1488 0.2437 0.213 Uiso 1 1 calc R . .
C81 C 0.8633(7) 0.3337(7) 0.4041(4) 0.145(6) Uani 1 1 d . . .
H81A H 0.8475 0.3026 0.3824 0.217 Uiso 1 1 calc R . .
H81B H 0.8731 0.3149 0.4323 0.217 Uiso 1 1 calc R . .
H81C H 0.9045 0.3527 0.4000 0.217 Uiso 1 1 calc R . .
C62 C 0.4193(7) 0.3481(6) 0.3019(4) 0.114(4) Uani 1 1 d . . .
H62A H 0.4010 0.3884 0.3054 0.171 Uiso 1 1 calc R . .
H62B H 0.4687 0.3486 0.3129 0.171 Uiso 1 1 calc R . .
H62C H 0.3998 0.3180 0.3175 0.171 Uiso 1 1 calc R . .
O8 O 0.4428(3) 0.4167(4) 0.0751(2) 0.093(2) Uani 1 1 d . . .
O10 O 0.4069(3) 0.7163(4) 0.0599(2) 0.086(2) Uani 1 1 d . . .
O9 O 0.3964(4) 0.7649(3) 0.1389(2) 0.091(2) Uani 1 1 d . . .
O7 O 0.5105(4) 0.3757(4) 0.1577(2) 0.101(3) Uani 1 1 d . . .
C91 C 0.4217(6) 0.3665(6) 0.0931(4) 0.092(3) Uani 1 1 d . . .
H91A H 0.4417 0.3301 0.0832 0.110 Uiso 1 1 calc R . .
H91B H 0.3718 0.3632 0.0825 0.110 Uiso 1 1 calc R . .
C97 C 0.4547(7) 0.7735(7) 0.1233(4) 0.117(5) Uani 1 1 d . . .
H97A H 0.4710 0.8155 0.1301 0.141 Uiso 1 1 calc R . .
H97B H 0.4906 0.7459 0.1392 0.141 Uiso 1 1 calc R . .
C92 C 0.5148(6) 0.4241(9) 0.0938(4) 0.146(7) Uani 1 1 d . . .
H92A H 0.5304 0.4612 0.0820 0.175 Uiso 1 1 calc R . .
H92B H 0.5391 0.3892 0.0854 0.175 Uiso 1 1 calc R . .
C96 C 0.4481(7) 0.7643(7) 0.0805(5) 0.122(5) Uani 1 1 d . . .
H96A H 0.4942 0.7579 0.0766 0.146 Uiso 1 1 calc R . .
H96B H 0.4305 0.8023 0.0656 0.146 Uiso 1 1 calc R . .
C95 C 0.3476(7) 0.7077(7) 0.0762(5) 0.125(5) Uani 1 1 d . . .
H95A H 0.3122 0.7365 0.0613 0.150 Uiso 1 1 calc R . .
H95B H 0.3301 0.6662 0.0685 0.150 Uiso 1 1 calc R . .
C94 C 0.3561(8) 0.7151(7) 0.1189(4) 0.139(7) Uani 1 1 d . . .
H94A H 0.3766 0.6774 0.1331 0.167 Uiso 1 1 calc R . .
H94B H 0.3106 0.7192 0.1242 0.167 Uiso 1 1 calc R . .
C93 C 0.5334(7) 0.4286(7) 0.1397(5) 0.121(5) Uani 1 1 d . . .
H93A H 0.5833 0.4322 0.1502 0.145 Uiso 1 1 calc R . .
H93B H 0.5127 0.4653 0.1486 0.145 Uiso 1 1 calc R . .
C90 C 0.4393(6) 0.3656(7) 0.1402(4) 0.106(4) Uani 1 1 d . . .
H90A H 0.4132 0.3976 0.1505 0.127 Uiso 1 1 calc R . .
H90B H 0.4265 0.3259 0.1501 0.127 Uiso 1 1 calc R . .
F16 F 0.8185(2) 0.57408(18) 0.07454(12) 0.0389(11) Uani 1 1 d . . .
F17 F 0.0356(2) 0.5363(2) 0.07428(12) 0.0485(12) Uani 1 1 d . . .
O11 O 0.9384(2) 0.6202(2) 0.06360(15) 0.0434(14) Uani 1 1 d . . .
O13 O 0.7707(4) 0.1812(3) 0.1965(3) 0.095(2) Uani 1 1 d . . .
O12 O 0.7501(5) 0.0506(3) 0.1859(3) 0.110(3) Uani 1 1 d . . .
C99 C 0.7299(10) 0.0926(7) 0.1502(4) 0.146(6) Uani 1 1 d . . .
H99A H 0.6813 0.1028 0.1461 0.175 Uiso 1 1 calc R . .
H99B H 0.7346 0.0718 0.1242 0.175 Uiso 1 1 calc R . .
C101 C 0.7479(9) 0.0819(6) 0.2260(4) 0.123(5) Uani 1 1 d . . .
H15F H 0.7001 0.0902 0.2258 0.148 Uiso 1 1 calc R . .
H13F H 0.7675 0.0550 0.2503 0.148 Uiso 1 1 calc R . .
C98 C 0.7698(8) 0.1500(6) 0.1555(4) 0.109(4) Uani 1 1 d . . .
H98A H 0.7500 0.1776 0.1316 0.131 Uiso 1 1 calc R . .
H98B H 0.8170 0.1408 0.1546 0.131 Uiso 1 1 calc R . .
C100 C 0.7856(8) 0.1388(7) 0.2309(4) 0.121(5) Uani 1 1 d . . .
H11F H 0.7784 0.1596 0.2562 0.145 Uiso 1 1 calc R . .
H12H H 0.8344 0.1286 0.2369 0.145 Uiso 1 1 calc R . .
F18 F 1.3433(2) 0.4820(3) 0.17625(17) 0.0708(15) Uani 1 1 d . . .
F20 F 1.2711(2) 0.5557(2) 0.16410(16) 0.0625(14) Uani 1 1 d . . .
F19 F 1.3551(3) 0.5550(3) 0.13430(18) 0.0833(17) Uani 1 1 d . . .
C103 C 1.3061(4) 0.5189(4) 0.1442(3) 0.047(2) Uani 1 1 d . . .
O14 O 0.8812(7) 0.4685(4) 0.0610(2) 0.073(2) Uani 1 1 d . . .
O15 O 0.9628(5) 0.4838(5) 0.0082(3) 0.154(4) Uani 1 1 d . . .
C104 C 1.1518(4) 0.6692(4) 0.1254(3) 0.0336(19) Uani 1 1 d . . .
H111 H 0.850(7) 0.495(7) 0.065(4) 0.15(7) Uiso 1 1 d . . .
H110 H 0.911(4) 0.483(4) 0.057(3) 0.02(3) 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
C102 C77 1.48(2) . ?
C7 N4 1.460(9) . ?
C7 C5 1.519(10) . ?
C5 C4 1.411(10) . ?
C5 C6 1.426(10) . ?
C3 C4 1.392(10) . ?
C3 C2 1.414(10) . ?
C3 C28 1.491(10) . ?
C4 C8 1.512(10) . ?
C46 C51 1.358(10) . ?
C46 C47 1.391(10) . ?
C46 C45 1.521(11) . ?
C30 C31 1.375(11) . ?
C30 C35 1.382(11) . ?
C30 C29 1.509(11) . ?
C1 C6 1.401(10) . ?
C1 C2 1.403(10) . ?
C1 C10 1.490(10) . ?
C11 N1 1.488(9) . ?
C11 C2 1.499(10) . ?
C6 C9 1.500(10) . ?
C29 O5 1.243(9) . ?
C29 N2 1.333(10) . ?
C28 N2 1.469(9) . ?
C52 C57 1.341(10) . ?
C52 C53 1.372(10) . ?
C52 C104 1.549(11) . ?
C51 C50 1.377(11) . ?
C35 C34 1.402(12) . ?
C35 C36 1.491(12) . ?
C9 N5 1.460(9) . ?
C8 N3 1.465(9) . ?
C10 N6 1.444(9) . ?
C13 O1 1.248(9) . ?
C13 N6 1.337(10) . ?
C13 C14 1.499(12) . ?
C43 C42 1.385(12) . ?
C43 C38 1.439(11) . ?
C43 C44 1.476(14) . ?
C37 O4 1.245(9) . ?
C37 N3 1.312(9) . ?
C37 C38 1.488(11) . ?
C45 O3 1.196(8) . ?
C45 N4 1.347(9) . ?
C53 C54 1.372(11) . ?
C39 C38 1.351(11) . ?
C39 C40 1.385(11) . ?
C22 C21 1.345(12) . ?
C22 C23 1.352(13) . ?
C57 C56 1.387(11) . ?
C57 C58 1.515(13) . ?
C31 C32 1.383(11) . ?
C48 C49 1.346(11) . ?
C48 C47 1.384(11) . ?
C21 C26 1.408(12) . ?
C21 C12 1.507(11) . ?
C33 C32 1.356(12) . ?
C33 C34 1.378(12) . ?
C14 C15 1.358(12) . ?
C14 C19 1.406(13) . ?
C49 C50 1.387(11) . ?
C44 F8 1.334(11) . ?
C44 F9 1.348(12) . ?
C44 F7 1.356(12) . ?
C47 C103 1.454(11) . ?
C41 C40 1.351(13) . ?
C41 C42 1.378(13) . ?
C54 C55 1.341(12) . ?
C56 C55 1.376(12) . ?
C16 C15 1.355(12) . ?
C16 C17 1.362(16) . ?
C12 O6 1.212(9) . ?
C12 N1 1.335(10) . ?
C18 C17 1.385(17) . ?
C18 C19 1.405(15) . ?
C26 C25 1.407(13) . ?
C26 C27 1.464(15) . ?
C27 F3 1.332(11) . ?
C27 F1 1.342(11) . ?
C27 F2 1.365(12) . ?
C58 F13 1.320(10) . ?
C58 F15 1.324(10) . ?
C58 F14 1.358(10) . ?
C36 F4 1.321(9) . ?
C36 F6 1.335(10) . ?
C36 F5 1.336(9) . ?
C19 C20 1.417(18) . ?
C25 C24 1.359(15) . ?
C24 C23 1.359(15) . ?
C20 F11 1.351(14) . ?
C20 F12 1.376(14) . ?
C20 F10 1.395(15) . ?
N5 C104 1.338(9) . ?
O2 C104 1.213(8) . ?
N7 C63 1.495(10) . ?
N7 C67 1.511(10) . ?
N7 C71 1.516(10) . ?
N7 C59 1.528(9) . ?
N8 C78 1.507(10) . ?
N8 C82 1.507(10) . ?
N8 C86 1.525(10) . ?
N8 C75 1.538(11) . ?
C86 C87 1.515(11) . ?
C71 C72 1.512(11) . ?
C75 C76 1.525(13) . ?
C67 C68 1.533(11) . ?
C64 C63 1.483(11) . ?
C64 C65 1.507(12) . ?
C59 C60 1.513(12) . ?
C79 C78 1.484(12) . ?
C79 C80 1.606(13) . ?
C68 C69 1.547(12) . ?
C61 C62 1.456(15) . ?
C61 C60 1.576(13) . ?
C83 C82 1.483(12) . ?
C83 C84 1.541(13) . ?
C65 C66 1.520(13) . ?
C76 C77 1.517(14) . ?
C72 C73 1.516(12) . ?
C69 C70 1.503(15) . ?
C73 C74 1.522(14) . ?
C87 C88 1.508(12) . ?
C84 C85 1.459(15) . ?
C89 C88 1.496(13) . ?
C80 C81 1.550(17) . ?
O8 C91 1.344(13) . ?
O8 C92 1.421(13) . ?
O10 C96 1.381(14) . ?
O10 C95 1.422(12) . ?
O9 C97 1.391(13) . ?
O9 C94 1.397(13) . ?
O7 C93 1.404(14) . ?
O7 C90 1.407(13) . ?
C91 C90 1.458(15) . ?
C97 C96 1.354(15) . ?
C92 C93 1.423(17) . ?
C95 C94 1.341(15) . ?
O13 C100 1.403(14) . ?
O13 C98 1.469(14) . ?
O12 C99 1.431(15) . ?
O12 C101 1.458(13) . ?
C99 C98 1.461(18) . ?
C101 C100 1.428(17) . ?
F18 C103 1.360(9) . ?
F20 C103 1.323(9) . ?
F19 C103 1.350(9) . ?

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
N4 C7 C5 112.8(6) . . ?
C4 C5 C6 119.9(6) . . ?
C4 C5 C7 121.1(7) . . ?
C6 C5 C7 119.0(6) . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 C28 120.0(7) . . ?
C2 C3 C28 119.9(7) . . ?
C3 C4 C5 119.9(7) . . ?
C3 C4 C8 120.7(6) . . ?
C5 C4 C8 119.4(7) . . ?
C51 C46 C47 118.6(7) . . ?
C51 C46 C45 119.5(7) . . ?
C47 C46 C45 121.6(7) . . ?
C31 C30 C35 118.6(7) . . ?
C31 C30 C29 118.2(8) . . ?
C35 C30 C29 123.1(8) . . ?
C6 C1 C2 120.2(6) . . ?
C6 C1 C10 120.5(6) . . ?
C2 C1 C10 119.3(6) . . ?
N1 C11 C2 111.8(6) . . ?
C1 C6 C5 119.4(6) . . ?
C1 C6 C9 120.8(7) . . ?
C5 C6 C9 119.8(7) . . ?
O5 C29 N2 124.1(7) . . ?
O5 C29 C30 121.2(7) . . ?
N2 C29 C30 114.7(8) . . ?
N2 C28 C3 111.8(6) . . ?
C57 C52 C53 120.1(7) . . ?
C57 C52 C104 121.9(7) . . ?
C53 C52 C104 117.7(7) . . ?
C46 C51 C50 122.8(8) . . ?
C30 C35 C34 118.5(8) . . ?
C30 C35 C36 122.7(8) . . ?
C34 C35 C36 118.8(8) . . ?
N5 C9 C6 111.8(5) . . ?
N3 C8 C4 114.4(6) . . ?
C1 C2 C3 120.2(6) . . ?
C1 C2 C11 119.8(7) . . ?
C3 C2 C11 120.0(7) . . ?
N6 C10 C1 112.0(6) . . ?
O1 C13 N6 121.4(8) . . ?
O1 C13 C14 121.0(8) . . ?
N6 C13 C14 117.4(8) . . ?
C42 C43 C38 118.6(9) . . ?
C42 C43 C44 118.2(9) . . ?
C38 C43 C44 123.1(9) . . ?
O4 C37 N3 123.4(7) . . ?
O4 C37 C38 118.8(7) . . ?
N3 C37 C38 117.6(7) . . ?
O3 C45 N4 124.5(7) . . ?
O3 C45 C46 121.4(7) . . ?
N4 C45 C46 114.0(7) . . ?
C54 C53 C52 120.1(8) . . ?
C38 C39 C40 122.9(8) . . ?
C21 C22 C23 121.3(10) . . ?
C52 C57 C56 120.1(8) . . ?
C52 C57 C58 123.2(8) . . ?
C56 C57 C58 116.6(9) . . ?
C30 C31 C32 122.8(8) . . ?
C49 C48 C47 122.8(8) . . ?
C22 C21 C26 118.4(8) . . ?
C22 C21 C12 121.0(8) . . ?
C26 C21 C12 120.5(8) . . ?
C32 C33 C34 120.1(8) . . ?
C15 C14 C19 117.6(8) . . ?
C15 C14 C13 119.0(8) . . ?
C19 C14 C13 123.3(9) . . ?
C48 C49 C50 119.1(8) . . ?
F8 C44 F9 106.6(8) . . ?
F8 C44 F7 106.0(9) . . ?
F9 C44 F7 105.9(10) . . ?
F8 C44 C43 111.4(10) . . ?
F9 C44 C43 113.5(9) . . ?
F7 C44 C43 112.9(8) . . ?
C33 C32 C31 118.6(8) . . ?
C48 C47 C46 118.3(7) . . ?
C48 C47 C103 119.1(7) . . ?
C46 C47 C103 122.3(7) . . ?
C39 C38 C43 117.3(8) . . ?
C39 C38 C37 120.6(8) . . ?
C43 C38 C37 122.0(8) . . ?
C40 C41 C42 119.7(9) . . ?
C51 C50 C49 118.4(8) . . ?
C55 C54 C53 119.9(8) . . ?
C41 C40 C39 120.0(9) . . ?
C55 C56 C57 119.1(8) . . ?
C41 C42 C43 121.3(9) . . ?
C33 C34 C35 121.3(8) . . ?
C15 C16 C17 121.0(11) . . ?
C16 C15 C14 122.8(10) . . ?
O6 C12 N1 123.3(7) . . ?
O6 C12 C21 121.6(7) . . ?
N1 C12 C21 115.0(8) . . ?
C17 C18 C19 120.1(12) . . ?
C25 C26 C21 119.0(10) . . ?
C25 C26 C27 117.8(10) . . ?
C21 C26 C27 123.1(8) . . ?
F3 C27 F1 104.0(8) . . ?
F3 C27 F2 105.1(9) . . ?
F1 C27 F2 103.8(10) . . ?
F3 C27 C26 116.4(10) . . ?
F1 C27 C26 113.7(9) . . ?
F2 C27 C26 112.6(8) . . ?
F13 C58 F15 107.2(8) . . ?
F13 C58 F14 106.7(8) . . ?
F15 C58 F14 103.8(8) . . ?
F13 C58 C57 112.6(8) . . ?
F15 C58 C57 114.2(8) . . ?
F14 C58 C57 111.9(8) . . ?
F4 C36 F6 108.4(7) . . ?
F4 C36 F5 105.7(7) . . ?
F6 C36 F5 105.0(8) . . ?
F4 C36 C35 112.1(8) . . ?
F6 C36 C35 112.2(7) . . ?
F5 C36 C35 113.0(8) . . ?
C18 C19 C14 119.5(11) . . ?
C18 C19 C20 117.4(12) . . ?
C14 C19 C20 123.1(10) . . ?
C24 C25 C26 120.2(10) . . ?
C54 C55 C56 120.6(8) . . ?
C25 C24 C23 118.8(9) . . ?
F11 C20 F12 103.6(12) . . ?
F11 C20 F10 102.7(11) . . ?
F12 C20 F10 100.1(12) . . ?
F11 C20 C19 116.4(13) . . ?
F12 C20 C19 117.3(11) . . ?
F10 C20 C19 114.5(12) . . ?
C16 C17 C18 118.9(12) . . ?
C22 C23 C24 122.1(11) . . ?
C12 N1 C11 118.7(6) . . ?
C45 N4 C7 118.7(6) . . ?
C37 N3 C8 122.4(6) . . ?
C29 N2 C28 121.8(6) . . ?
C104 N5 C9 121.7(6) . . ?
C13 N6 C10 123.7(6) . . ?
C63 N7 C67 112.4(6) . . ?
C63 N7 C71 106.9(6) . . ?
C67 N7 C71 110.9(6) . . ?
C63 N7 C59 111.6(6) . . ?
C67 N7 C59 103.3(5) . . ?
C71 N7 C59 111.8(6) . . ?
C78 N8 C82 111.5(6) . . ?
C78 N8 C86 105.0(6) . . ?
C82 N8 C86 111.6(6) . . ?
C78 N8 C75 110.5(7) . . ?
C82 N8 C75 106.7(6) . . ?
C86 N8 C75 111.7(6) . . ?
C87 C86 N8 116.0(6) . . ?
C72 C71 N7 117.1(7) . . ?
C76 C75 N8 116.1(7) . . ?
N7 C67 C68 114.2(6) . . ?
C63 C64 C65 111.1(7) . . ?
C60 C59 N7 114.9(6) . . ?
C64 C63 N7 118.1(7) . . ?
C78 C79 C80 109.6(7) . . ?
C67 C68 C69 108.0(7) . . ?
C79 C78 N8 115.3(7) . . ?
C62 C61 C60 109.5(10) . . ?
C82 C83 C84 110.1(8) . . ?
C64 C65 C66 113.4(8) . . ?
C83 C82 N8 116.4(7) . . ?
C77 C76 C75 110.8(9) . . ?
C71 C72 C73 108.5(7) . . ?
C70 C69 C68 113.3(9) . . ?
C72 C73 C74 112.6(8) . . ?
C88 C87 C86 109.7(7) . . ?
C59 C60 C61 110.0(7) . . ?
C85 C84 C83 114.4(9) . . ?
C102 C77 C76 115.2(12) . . ?
C89 C88 C87 114.8(9) . . ?
C81 C80 C79 109.8(9) . . ?
C91 O8 C92 107.8(9) . . ?
C96 O10 C95 112.0(8) . . ?
C97 O9 C94 112.1(9) . . ?
C93 O7 C90 111.5(9) . . ?
O8 C91 C90 115.7(11) . . ?
C96 C97 O9 117.9(11) . . ?
O8 C92 C93 114.3(10) . . ?
C97 C96 O10 119.0(11) . . ?
C94 C95 O10 117.1(11) . . ?
C95 C94 O9 117.8(11) . . ?
O7 C93 C92 109.9(12) . . ?
O7 C90 C91 111.1(9) . . ?
C100 O13 C98 110.5(9) . . ?
C99 O12 C101 109.9(9) . . ?
O12 C99 C98 114.2(12) . . ?
C100 C101 O12 111.1(11) . . ?
C99 C98 O13 112.0(10) . . ?
O13 C100 C101 118.4(12) . . ?
F20 C103 F19 105.6(7) . . ?
F20 C103 F18 104.1(7) . . ?
F19 C103 F18 103.0(7) . . ?
F20 C103 C47 114.8(7) . . ?
F19 C103 C47 113.9(7) . . ?
F18 C103 C47 114.2(7) . . ?
O2 C104 N5 124.0(7) . . ?
O2 C104 C52 122.2(7) . . ?
N5 C104 C52 113.8(7) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        19.34
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.084
#end
_database_code_depnum_ccdc_archive 'CCDC 996874'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CCDC996875

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H66 F18 N6 O12'
_chemical_formula_weight         1549.31

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.968(4)
_cell_length_b                   13.856(5)
_cell_length_c                   14.250(5)
_cell_angle_alpha                76.125(11)
_cell_angle_beta                 73.854(11)
_cell_angle_gamma                81.532(12)
_cell_volume                     2011.9(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6916
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.87

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             798
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9686
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7041
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_UnetI/netI     0.0528
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7041
_reflns_number_gt                5033
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 3.2'
_computing_publication_material  'ORTEP 3v.2'

_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. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 362 129 ' '
_platon_squeeze_details          
;
The unit cell contains one dioxane molecule which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;

_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)+(0.2000P)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     SHELXL
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7041
_refine_ls_number_parameters     488
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.2209
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_restrained_S_all      0.854
_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
C27 C 1.1042(2) 0.79027(19) 0.5295(2) 0.0173(6) Uani 1 1 d . . .
H27A H 1.1877 0.7852 0.5419 0.021 Uiso 1 1 calc R . .
H27B H 1.0499 0.7501 0.5868 0.021 Uiso 1 1 calc R . .
C29 C 0.7524(2) 0.80630(19) 0.6966(2) 0.0219(6) Uani 1 1 d . . .
C24 C 0.9261(2) 0.92383(19) 0.5020(2) 0.0173(6) Uani 1 1 d . . .
C1 C 0.6443(2) 0.8320(2) 0.7822(2) 0.0227(6) Uani 1 1 d . . .
C13 C 0.4449(2) 1.1765(2) 0.5685(2) 0.0212(6) Uani 1 1 d . . .
C26 C 0.8397(2) 0.84146(19) 0.5164(2) 0.0190(6) Uani 1 1 d . . .
H26A H 0.8066 0.8507 0.4581 0.023 Uiso 1 1 calc R . .
H26B H 0.8882 0.7769 0.5242 0.023 Uiso 1 1 calc R . .
C25 C 0.8798(2) 1.02480(19) 0.4808(2) 0.0169(6) Uani 1 1 d . . .
C23 C 1.0486(2) 0.89936(18) 0.51789(19) 0.0166(6) Uani 1 1 d . . .
C14 C 0.5402(2) 1.12119(19) 0.4970(2) 0.0185(6) Uani 1 1 d . . .
C28 C 0.7568(2) 1.0526(2) 0.4479(2) 0.0216(6) Uani 1 1 d . . .
H28A H 0.7725 1.1022 0.3859 0.026 Uiso 1 1 calc R . .
H28B H 0.7322 0.9940 0.4343 0.026 Uiso 1 1 calc R . .
C30 C 1.1946(2) 0.78278(19) 0.3520(2) 0.0199(6) Uani 1 1 d . . .
C21 C 1.2768(3) 0.6762(2) 0.2203(2) 0.0236(6) Uani 1 1 d . . .
C8 C 0.3807(3) 1.1229(2) 0.6602(2) 0.0257(6) Uani 1 1 d . . .
H8 H 0.3989 1.0542 0.6777 0.031 Uiso 1 1 calc R . .
C16 C 1.1819(2) 0.74051(19) 0.2671(2) 0.0202(6) Uani 1 1 d . . .
C6 C 0.6030(3) 0.9319(2) 0.7786(2) 0.0288(7) Uani 1 1 d . . .
H6 H 0.6356 0.9793 0.7220 0.035 Uiso 1 1 calc R . .
C12 C 0.4168(3) 1.2808(2) 0.5434(2) 0.0262(7) Uani 1 1 d . . .
C22 C 1.3978(3) 0.6462(2) 0.2525(2) 0.0285(7) Uani 1 1 d . . .
C17 C 1.0721(3) 0.7710(2) 0.2317(2) 0.0250(6) Uani 1 1 d . . .
H17 H 1.0074 0.8129 0.2628 0.030 Uiso 1 1 calc R . .
C2 C 0.5958(3) 0.7603(2) 0.8676(2) 0.0281(7) Uani 1 1 d . . .
C20 C 1.2617(3) 0.6417(2) 0.1403(2) 0.0289(7) Uani 1 1 d . . .
H20 H 1.3242 0.5973 0.1107 0.035 Uiso 1 1 calc R . .
C19 C 1.1539(3) 0.6733(2) 0.1048(2) 0.0317(7) Uani 1 1 d . . .
H19 H 1.1444 0.6511 0.0508 0.038 Uiso 1 1 calc R . .
C10 C 0.2625(3) 1.2751(2) 0.6998(3) 0.0369(8) Uani 1 1 d . . .
H10 H 0.2012 1.3077 0.7440 0.044 Uiso 1 1 calc R . .
C18 C 1.0602(3) 0.7384(2) 0.1502(2) 0.0310(7) Uani 1 1 d . . .
H18 H 0.9885 0.7605 0.1257 0.037 Uiso 1 1 calc R . .
C11 C 0.3259(3) 1.3291(2) 0.6095(3) 0.0346(8) Uani 1 1 d . . .
H11 H 0.3078 1.3979 0.5930 0.042 Uiso 1 1 calc R . .
C5 C 0.5125(3) 0.9621(3) 0.8596(3) 0.0404(8) Uani 1 1 d . . .
H5 H 0.4852 1.0293 0.8569 0.048 Uiso 1 1 calc R . .
C15 C 0.4856(3) 1.3421(2) 0.4458(3) 0.0362(8) Uani 1 1 d . . .
C7 C 0.6376(3) 0.6506(2) 0.8778(2) 0.0322(7) Uani 1 1 d . . .
C9 C 0.2889(3) 1.1727(2) 0.7256(3) 0.0331(7) Uani 1 1 d . . .
H9 H 0.2451 1.1372 0.7868 0.040 Uiso 1 1 calc R . .
C4 C 0.4643(3) 0.8919(3) 0.9429(3) 0.0429(9) Uani 1 1 d . . .
H4 H 0.4042 0.9116 0.9969 0.051 Uiso 1 1 calc R . .
C3 C 0.5053(3) 0.7905(3) 0.9470(3) 0.0402(8) Uani 1 1 d . . .
H3 H 0.4716 0.7433 1.0034 0.048 Uiso 1 1 calc R . .
F3 F 1.38101(16) 0.63123(13) 0.35076(14) 0.0356(5) Uani 1 1 d . . .
F4 F 0.66507(18) 0.61835(13) 0.79219(14) 0.0392(5) Uani 1 1 d . . .
F1 F 1.48133(16) 0.71585(15) 0.21083(15) 0.0421(5) Uani 1 1 d . . .
F5 F 0.73950(18) 0.62402(15) 0.91489(15) 0.0445(5) Uani 1 1 d . . .
F2 F 1.45719(17) 0.56084(15) 0.22469(16) 0.0481(6) Uani 1 1 d . . .
F7 F 0.61006(18) 1.31645(16) 0.42324(18) 0.0585(7) Uani 1 1 d . . .
F8 F 0.4434(2) 1.33286(17) 0.36922(17) 0.0597(6) Uani 1 1 d . . .
F6 F 0.5462(2) 0.59339(15) 0.94185(17) 0.0559(6) Uani 1 1 d . . .
F9 F 0.4706(2) 1.43956(14) 0.44409(18) 0.0600(6) Uani 1 1 d . . .
O3 O 0.51664(17) 1.10457(14) 0.42276(15) 0.0243(5) Uani 1 1 d . . .
O2 O 0.85158(17) 0.75846(15) 0.71230(15) 0.0270(5) Uani 1 1 d . . .
O1 O 1.27193(17) 0.84504(14) 0.33562(15) 0.0257(5) Uani 1 1 d . . .
N2 N 1.1155(2) 0.75080(16) 0.43984(17) 0.0194(5) Uani 1 1 d . . .
H2 H 1.0682 0.7046 0.4448 0.023 Uiso 1 1 calc R . .
N1 N 0.7342(2) 0.84475(16) 0.60509(17) 0.0198(5) Uani 1 1 d . . .
H1 H 0.6603 0.8714 0.5987 0.024 Uiso 1 1 calc R . .
N3 N 0.65126(19) 1.09177(16) 0.52005(17) 0.0193(5) Uani 1 1 d . . .
H3A H 0.6605 1.0959 0.5769 0.023 Uiso 1 1 calc R . .
O1A O -0.0791(2) 0.01173(16) 0.24874(16) 0.0352(5) Uani 1 1 d . . .
O2A O 0.0314(2) 0.11877(19) 0.05491(18) 0.0452(6) Uani 1 1 d . . .
C7A C -0.0921(3) 0.0853(3) 0.0817(3) 0.0418(8) Uani 1 1 d . . .
H7A1 H -0.0860 0.0201 0.0661 0.050 Uiso 1 1 calc R . .
H7A2 H -0.1442 0.1308 0.0423 0.050 Uiso 1 1 calc R . .
C6A C 0.0445(3) 0.0467(3) 0.2260(3) 0.0383(8) Uani 1 1 d . . .
H6A1 H 0.0965 0.0009 0.2652 0.046 Uiso 1 1 calc R . .
H6A2 H 0.0367 0.1116 0.2426 0.046 Uiso 1 1 calc R . .
C36 C -0.1544(3) 0.0790(3) 0.1893(3) 0.0389(8) Uani 1 1 d . . .
H36A H -0.1644 0.1447 0.2047 0.047 Uiso 1 1 calc R . .
H36B H -0.2384 0.0558 0.2049 0.047 Uiso 1 1 calc R . .
C35 C 0.1061(3) 0.0541(3) 0.1176(3) 0.0449(9) Uani 1 1 d . . .
H35A H 0.1890 0.0792 0.1022 0.054 Uiso 1 1 calc R . .
H35B H 0.1191 -0.0120 0.1029 0.054 Uiso 1 1 calc R . .
O10 O 0.94518(18) 0.59737(14) 0.46751(15) 0.0264(5) Uani 1 1 d . . .
C42A C 0.9053(3) 0.5437(2) 0.5700(2) 0.0307(7) Uani 1 1 d . . .
H42A H 0.8325 0.5075 0.5778 0.037 Uiso 1 1 calc R . .
H42B H 0.8795 0.5907 0.6141 0.037 Uiso 1 1 calc R . .
C43A C 0.9887(3) 0.5278(2) 0.4019(2) 0.0289(7) Uani 1 1 d . . .
H43A H 1.0176 0.5642 0.3336 0.035 Uiso 1 1 calc R . .
H43B H 0.9184 0.4910 0.4051 0.035 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
C27 N2 1.474(3) . ?
C27 C23 1.532(3) . ?
C29 O2 1.234(3) . ?
C29 N1 1.343(4) . ?
C29 C1 1.517(4) . ?
C24 C23 1.404(3) . ?
C24 C25 1.407(4) . ?
C24 C26 1.530(3) . ?
C1 C6 1.385(4) . ?
C1 C2 1.402(4) . ?
C13 C8 1.390(4) . ?
C13 C12 1.411(4) . ?
C13 C14 1.505(4) . ?
C26 N1 1.462(3) . ?
C25 C23 1.408(4) 2_776 ?
C25 C28 1.517(3) . ?
C23 C25 1.408(4) 2_776 ?
C14 O3 1.235(3) . ?
C14 N3 1.331(3) . ?
C28 N3 1.454(3) . ?
C30 O1 1.236(3) . ?
C30 N2 1.326(4) . ?
C30 C16 1.511(4) . ?
C21 C20 1.394(4) . ?
C21 C16 1.396(4) . ?
C21 C22 1.494(4) . ?
C8 C9 1.394(4) . ?
C16 C17 1.403(4) . ?
C6 C5 1.402(5) . ?
C12 C11 1.383(4) . ?
C12 C15 1.505(5) . ?
C22 F3 1.328(4) . ?
C22 F1 1.344(4) . ?
C22 F2 1.355(3) . ?
C17 C18 1.386(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.505(4) . ?
C20 C19 1.386(4) . ?
C19 C18 1.388(4) . ?
C10 C11 1.376(5) . ?
C10 C9 1.385(5) . ?
C5 C4 1.373(5) . ?
C15 F7 1.327(4) . ?
C15 F9 1.331(3) . ?
C15 F8 1.337(4) . ?
C7 F5 1.333(4) . ?
C7 F4 1.341(4) . ?
C7 F6 1.358(4) . ?
C4 C3 1.404(5) . ?
O1A C6A 1.432(4) . ?
O1A C36 1.432(4) . ?
O2A C7A 1.417(4) . ?
O2A C35 1.442(4) . ?
C7A C36 1.483(5) . ?
C6A C35 1.488(5) . ?
O10 C43A 1.442(3) . ?
O10 C42A 1.448(4) . ?
C42A C43A 1.491(4) 2_766 ?
C43A C42A 1.491(4) 2_766 ?

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
N2 C27 C23 112.0(2) . . ?
O2 C29 N1 124.0(3) . . ?
O2 C29 C1 120.8(2) . . ?
N1 C29 C1 115.0(2) . . ?
C23 C24 C25 119.3(2) . . ?
C23 C24 C26 120.2(2) . . ?
C25 C24 C26 120.3(2) . . ?
C6 C1 C2 119.9(3) . . ?
C6 C1 C29 117.4(3) . . ?
C2 C1 C29 122.4(3) . . ?
C8 C13 C12 119.5(3) . . ?
C8 C13 C14 118.9(2) . . ?
C12 C13 C14 121.6(3) . . ?
N1 C26 C24 109.6(2) . . ?
C24 C25 C23 120.7(2) . 2_776 ?
C24 C25 C28 119.6(2) . . ?
C23 C25 C28 119.5(2) 2_776 . ?
C24 C23 C25 119.9(2) . 2_776 ?
C24 C23 C27 119.0(2) . . ?
C25 C23 C27 121.1(2) 2_776 . ?
O3 C14 N3 122.8(2) . . ?
O3 C14 C13 122.3(2) . . ?
N3 C14 C13 114.8(2) . . ?
N3 C28 C25 114.5(2) . . ?
O1 C30 N2 125.0(2) . . ?
O1 C30 C16 119.7(2) . . ?
N2 C30 C16 115.2(2) . . ?
C20 C21 C16 120.4(2) . . ?
C20 C21 C22 119.0(3) . . ?
C16 C21 C22 120.6(2) . . ?
C13 C8 C9 119.5(3) . . ?
C21 C16 C17 119.1(2) . . ?
C21 C16 C30 122.8(2) . . ?
C17 C16 C30 118.1(2) . . ?
C1 C6 C5 120.5(3) . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 C15 118.5(3) . . ?
C13 C12 C15 121.3(3) . . ?
F3 C22 F1 106.8(2) . . ?
F3 C22 F2 106.9(2) . . ?
F1 C22 F2 106.2(2) . . ?
F3 C22 C21 113.4(2) . . ?
F1 C22 C21 111.6(2) . . ?
F2 C22 C21 111.7(2) . . ?
C18 C17 C16 119.9(3) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 C7 117.7(3) . . ?
C1 C2 C7 123.0(3) . . ?
C19 C20 C21 120.2(3) . . ?
C20 C19 C18 119.6(3) . . ?
C11 C10 C9 120.8(3) . . ?
C17 C18 C19 120.9(3) . . ?
C10 C11 C12 119.7(3) . . ?
C4 C5 C6 119.6(3) . . ?
F7 C15 F9 106.9(3) . . ?
F7 C15 F8 106.6(3) . . ?
F9 C15 F8 104.9(2) . . ?
F7 C15 C12 112.5(2) . . ?
F9 C15 C12 113.2(3) . . ?
F8 C15 C12 112.1(3) . . ?
F5 C7 F4 106.8(2) . . ?
F5 C7 F6 104.9(2) . . ?
F4 C7 F6 105.3(3) . . ?
F5 C7 C2 112.9(3) . . ?
F4 C7 C2 114.2(2) . . ?
F6 C7 C2 112.0(2) . . ?
C10 C9 C8 120.3(3) . . ?
C5 C4 C3 120.2(3) . . ?
C2 C3 C4 120.5(3) . . ?
C30 N2 C27 123.5(2) . . ?
C29 N1 C26 120.2(2) . . ?
C14 N3 C28 119.1(2) . . ?
C6A O1A C36 109.4(2) . . ?
C7A O2A C35 108.9(3) . . ?
O2A C7A C36 112.0(3) . . ?
O1A C6A C35 109.3(3) . . ?
O1A C36 C7A 110.1(3) . . ?
O2A C35 C6A 112.6(3) . . ?
C43A O10 C42A 109.9(2) . . ?
O10 C42A C43A 110.4(2) . 2_766 ?
O10 C43A C42A 111.3(2) . 2_766 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.095
_database_code_depnum_ccdc_archive 'CCDC 996875'
