# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#TrackingRef '- CB8-6MC_cpx_CCDC_revised1.cif'

_audit_creation_method           'APEX2 v2010.5-0'

_publ_contact_author_name        'J. Sivaguru'
_publ_contact_author_address     
;
;
_publ_contact_author_email       Sivaguru.Jayaraman@ndsu.edu
_publ_contact_author_fax         ?
_publ_contact_author_phone       '701 231-8923'
loop_
_publ_author_name
_publ_author_address
'Barry Pemberton'
;
Dunbar Hall
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;
'Raushan Singh'
;
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;
'Alexander C. Johnson'
;
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;
'Steffen Jockusch'
;
Department of Chemistry
Columbia University
New York, NY 58108-6050
;
'Jose Paulo Da Silva'
;
FCT-Universidade do Algarve
Campus de Gambelas
8005-139 Faro, Portugal
;
;
N.J.Turro
;
;
Department of Chemistry
Columbia University
New York, NY 58108-6050
;
'Angel Ugrinov'
;
Dunbar Hall
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;
'D.K. Srivastava'
;
IACC 312
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;
'Jayaraman Sivaguru'
;
Ladd Hall
Department of Chemistry and Biochemistry
North Dakota State University
Fargo, ND 58108
USA

;

_publ_section_title              
;
;
_publ_section_abstract           
;
;
_publ_section_references         
;
;
_publ_section_comment            
;
;

data_cu_bxp9_0m
_database_code_depnum_ccdc_archive 'CCDC 814052'
#TrackingRef '- CB8-6MC_cpx_CCDC_revised1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C48 H48 N32 O16), 2(C10 H8 O2), 13.5 (H2 O)'
_chemical_formula_sum            'C68 H64 N32 O33.5'
_chemical_formula_weight         1865.51

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   16.4918(3)
_cell_length_b                   22.0793(4)
_cell_length_c                   22.2875(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8115.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9704
_cell_measurement_theta_min      6.25
_cell_measurement_theta_max      66.19

_exptl_crystal_description       chunk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3856
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'Acta Cryst (1995). A51, 33-38'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44959
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.89
_diffrn_reflns_theta_max         66.53
_reflns_number_total             6974
_reflns_number_gt                6587
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^2^+18.2196P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6974
_refine_ls_number_parameters     645
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2084
_refine_ls_wR_factor_gt          0.1966
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.062
_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
C32 C 1.0587(3) 0.4664(3) 0.89748(19) 0.0655(14) Uani 1 1 d . . .
C25 C 0.8497(3) 0.51073(19) 0.8938(2) 0.0575(13) Uani 1 1 d . . .
O1 O 0.98695(13) 0.25291(11) 1.04903(10) 0.0298(5) Uani 1 1 d . . .
O2 O 1.26143(12) 0.36702(9) 0.84860(9) 0.0248(5) Uani 1 1 d . . .
O3 O 0.98541(13) 0.51578(10) 0.73184(11) 0.0318(5) Uani 1 1 d . . .
O4 O 0.93920(12) 0.33568(9) 1.20327(9) 0.0255(5) Uani 1 1 d . . .
O5 O 1.11991(12) 0.26509(9) 0.90043(9) 0.0214(4) Uani 1 1 d . . .
O6 O 0.68662(13) 0.48286(9) 1.06565(9) 0.0254(5) Uani 1 1 d . . .
O7 O 0.69780(15) 0.37400(11) 0.91397(10) 0.0354(6) Uani 1 1 d . . .
O8 O 0.83780(13) 0.39379(10) 0.78899(10) 0.0306(5) Uani 1 1 d . . .
O9 O 0.8070(2) 0.54435(13) 0.86355(17) 0.0634(9) Uani 1 1 d . . .
O10 O 0.9277(2) 0.50549(15) 0.87957(15) 0.0603(9) Uani 1 1 d . . .
N1 N 0.90286(14) 0.24900(11) 0.96644(11) 0.0210(5) Uani 1 1 d . . .
N2 N 0.98368(14) 0.25729(11) 0.87621(10) 0.0189(5) Uani 1 1 d . . .
N3 N 0.95890(14) 0.34603(11) 0.76658(11) 0.0236(5) Uani 1 1 d . . .
N4 N 1.05279(14) 0.42376(11) 0.73435(11) 0.0211(5) Uani 1 1 d . . .
N5 N 0.87476(14) 0.49163(11) 1.26391(11) 0.0206(5) Uani 1 1 d . . .
N6 N 0.82920(14) 0.39961(11) 1.21509(11) 0.0202(5) Uani 1 1 d . . .
N7 N 0.82060(15) 0.32421(11) 1.14960(11) 0.0221(5) Uani 1 1 d . . .
N8 N 0.85047(14) 0.27691(11) 1.05429(11) 0.0208(5) Uani 1 1 d . . .
N9 N 1.16573(14) 0.36366(10) 0.77339(10) 0.0178(5) Uani 1 1 d . . .
N10 N 0.73879(15) 0.32527(11) 1.00034(10) 0.0218(5) Uani 1 1 d . . .
N11 N 0.78909(15) 0.29443(12) 0.91317(11) 0.0234(5) Uani 1 1 d . . .
N12 N 1.07084(14) 0.28607(11) 0.80586(10) 0.0187(5) Uani 1 1 d . . .
N13 N 1.22619(13) 0.45145(10) 0.79228(10) 0.0175(5) Uani 1 1 d . . .
N14 N 0.72641(13) 0.38541(10) 1.09051(10) 0.0176(5) Uani 1 1 d . . .
N15 N 0.72563(14) 0.45659(10) 1.16153(11) 0.0198(5) Uani 1 1 d . . .
N16 N 0.86739(14) 0.29691(11) 0.82100(11) 0.0227(5) Uani 1 1 d . . .
C1 C 0.92046(18) 0.25870(13) 1.02574(13) 0.0219(6) Uani 1 1 d . . .
C2 C 0.96059(17) 0.22000(13) 0.92688(13) 0.0227(6) Uani 1 1 d . . .
H2A H 0.9368 0.1818 0.9118 0.027 Uiso 1 1 calc R . .
H2B H 1.0098 0.2096 0.9501 0.027 Uiso 1 1 calc R . .
C3 C 0.93619(16) 0.25675(13) 0.82124(12) 0.0194(6) Uani 1 1 d . . .
H3 H 0.9206 0.2147 0.8093 0.023 Uiso 1 1 calc R . .
C4 C 0.99432(16) 0.28605(12) 0.77490(13) 0.0190(6) Uani 1 1 d . . .
H4 H 0.9966 0.2626 0.7366 0.023 Uiso 1 1 calc R . .
C5 C 0.98397(18) 0.38629(14) 0.71886(14) 0.0260(7) Uani 1 1 d . . .
H5A H 0.9978 0.3618 0.6831 0.031 Uiso 1 1 calc R . .
H5B H 0.9378 0.4128 0.7080 0.031 Uiso 1 1 calc R . .
C6 C 1.04731(17) 0.48604(13) 0.73392(13) 0.0222(6) Uani 1 1 d . . .
C7 C 0.85595(18) 0.42799(13) 1.27027(13) 0.0215(6) Uani 1 1 d . . .
H7A H 0.8130 0.4233 1.3009 0.026 Uiso 1 1 calc R . .
H7B H 0.9048 0.4066 1.2850 0.026 Uiso 1 1 calc R . .
C8 C 0.87030(17) 0.35188(12) 1.19018(13) 0.0198(6) Uani 1 1 d . . .
C9 C 0.84249(19) 0.26899(13) 1.11857(13) 0.0227(6) Uani 1 1 d . . .
H9A H 0.8006 0.2379 1.1266 0.027 Uiso 1 1 calc R . .
H9B H 0.8945 0.2539 1.1349 0.027 Uiso 1 1 calc R . .
C10 C 1.22192(16) 0.39156(12) 0.80896(12) 0.0182(6) Uani 1 1 d . . .
C11 C 1.13547(16) 0.40296(12) 0.72644(12) 0.0182(6) Uani 1 1 d . . .
H11 H 1.1440 0.3850 0.6857 0.022 Uiso 1 1 calc R . .
C12 C 0.78040(17) 0.26937(13) 1.01580(13) 0.0199(6) Uani 1 1 d . . .
H12 H 0.7420 0.2385 1.0323 0.024 Uiso 1 1 calc R . .
C13 C 0.73786(18) 0.33531(14) 0.93976(13) 0.0251(6) Uani 1 1 d . . .
C14 C 0.81681(17) 0.24883(13) 0.95515(13) 0.0205(6) Uani 1 1 d . . .
H14 H 0.7972 0.2076 0.9436 0.025 Uiso 1 1 calc R . .
C15 C 1.06383(16) 0.26941(12) 0.86478(12) 0.0176(6) Uani 1 1 d . . .
C16 C 1.14740(16) 0.29969(12) 0.77755(13) 0.0182(6) Uani 1 1 d . . .
H16A H 1.1472 0.2823 0.7366 0.022 Uiso 1 1 calc R . .
H16B H 1.1912 0.2795 0.8004 0.022 Uiso 1 1 calc R . .
C17 C 1.18605(17) 0.46144(12) 0.73514(12) 0.0189(6) Uani 1 1 d . . .
H17 H 1.2259 0.4675 0.7018 0.023 Uiso 1 1 calc R . .
C18 C 0.74141(17) 0.35226(12) 1.14589(12) 0.0188(6) Uani 1 1 d . . .
H18 H 0.6971 0.3226 1.1545 0.023 Uiso 1 1 calc R . .
C19 C 0.71042(16) 0.44592(13) 1.10242(13) 0.0189(6) Uani 1 1 d . . .
C20 C 0.70370(16) 0.51273(12) 1.19069(13) 0.0205(6) Uani 1 1 d . . .
H20A H 0.6714 0.5035 1.2270 0.025 Uiso 1 1 calc R . .
H20B H 0.6692 0.5368 1.1632 0.025 Uiso 1 1 calc R . .
C21 C 0.74576(17) 0.40237(12) 1.19449(12) 0.0182(6) Uani 1 1 d . . .
H21 H 0.7066 0.3947 1.2279 0.022 Uiso 1 1 calc R . .
C22 C 0.68429(17) 0.35636(13) 1.04078(13) 0.0219(6) Uani 1 1 d . . .
H22A H 0.6447 0.3269 1.0570 0.026 Uiso 1 1 calc R . .
H22B H 0.6538 0.3874 1.0181 0.026 Uiso 1 1 calc R . .
C23 C 0.88361(17) 0.35073(14) 0.79217(13) 0.0231(6) Uani 1 1 d . . .
C24 C 0.79047(17) 0.28473(15) 0.84921(13) 0.0242(6) Uani 1 1 d . . .
H24A H 0.7753 0.2421 0.8411 0.029 Uiso 1 1 calc R . .
H24B H 0.7488 0.3109 0.8305 0.029 Uiso 1 1 calc R . .
C26 C 0.9805(3) 0.46791(19) 0.91456(17) 0.0453(9) Uani 1 1 d . . .
C27 C 0.9470(2) 0.43906(18) 0.96267(19) 0.0454(10) Uani 1 1 d . . .
C28 C 1.0029(3) 0.40185(18) 0.9982(2) 0.0537(11) Uani 1 1 d . . .
H28 H 0.9836 0.3810 1.0326 0.064 Uiso 1 1 calc R . .
C29 C 1.0811(3) 0.39713(19) 0.98246(19) 0.0493(11) Uani 1 1 d . . .
C30 C 1.1384(3) 0.3567(2) 1.01805(19) 0.0518(11) Uani 1 1 d . . .
H30A H 1.1259 0.3141 1.0097 0.078 Uiso 1 1 calc R . .
H30B H 1.1316 0.3646 1.0610 0.078 Uiso 1 1 calc R . .
H30C H 1.1945 0.3653 1.0063 0.078 Uiso 1 1 calc R . .
C31 C 1.1083(3) 0.4299(3) 0.93200(19) 0.0650(14) Uani 1 1 d . . .
H31 H 1.1638 0.4267 0.9211 0.078 Uiso 1 1 calc R . .
H32 H 1.0779 0.4891 0.8642 0.078 Uiso 1 1 d R . .
C33 C 0.8659(3) 0.4444(2) 0.9791(3) 0.0669(14) Uani 1 1 d . . .
H33 H 0.8450 0.4241 1.0133 0.080 Uiso 1 1 calc R . .
C34 C 0.8196(4) 0.4786(2) 0.9456(3) 0.0731(15) Uani 1 1 d . . .
H34 H 0.7639 0.4824 0.9558 0.088 Uiso 1 1 calc R . .
O1S O 0.55150(16) 0.37677(14) 0.15695(14) 0.0538(8) Uani 1 1 d U . .
O2S O 0.89474(19) 0.74746(15) 0.35977(13) 0.0568(8) Uani 1 1 d U . .
O3S O 0.1056(2) 0.36228(17) 0.20024(15) 0.0651(9) Uani 1 1 d U . .
O4S O 0.6371(3) 0.63439(15) 0.04910(16) 0.0496(10) Uani 0.75 1 d PU . .
O7S O 0.8960(6) 0.5274(5) 0.3998(5) 0.037(3) Uani 0.238(6) 1 d PU A 1
O8S O 0.0418(7) 0.5491(5) 0.4513(6) 0.049(3) Uani 0.238(6) 1 d PU A 1
O6S O 0.9839(3) 0.4561(2) 0.4317(2) 0.0782(16) Uani 0.762(6) 1 d PU A 2
O9S O -0.0273(3) 0.5832(2) 0.4293(4) 0.106(3) Uani 0.762(6) 1 d PU A 2
O5S O 0.3309(5) 0.4030(2) 0.0725(2) 0.0411(18) Uani 0.64(2) 1 d PU B 1
O10S O 0.3299(16) 0.4511(10) 0.0391(8) 0.108(10) Uani 0.224(11) 1 d PU C 2
O11S O 0.382(5) 0.4132(14) 0.0723(10) 0.072(18) Uani 0.14(2) 1 d PU D 3

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C32 0.060(3) 0.103(4) 0.034(2) 0.000(2) 0.006(2) 0.022(3)
C25 0.047(2) 0.039(2) 0.086(3) -0.032(2) -0.030(2) 0.0106(18)
O1 0.0223(11) 0.0415(13) 0.0257(11) 0.0050(9) -0.0033(9) 0.0042(9)
O2 0.0264(11) 0.0204(10) 0.0276(11) 0.0015(8) -0.0091(9) 0.0000(8)
O3 0.0197(11) 0.0254(11) 0.0503(14) 0.0071(10) -0.0076(9) 0.0029(9)
O4 0.0233(11) 0.0247(11) 0.0285(11) 0.0029(8) -0.0034(8) 0.0068(8)
O5 0.0196(10) 0.0235(10) 0.0212(10) 0.0005(8) -0.0017(8) 0.0033(8)
O6 0.0279(11) 0.0217(11) 0.0265(11) 0.0034(8) -0.0038(9) 0.0040(8)
O7 0.0445(14) 0.0398(13) 0.0220(11) -0.0018(10) -0.0088(10) 0.0170(11)
O8 0.0238(11) 0.0292(12) 0.0387(13) 0.0019(9) -0.0087(9) 0.0068(9)
O9 0.0571(19) 0.0448(17) 0.088(2) -0.0185(16) -0.0391(17) 0.0152(14)
O10 0.0550(19) 0.065(2) 0.0606(19) -0.0178(16) -0.0208(15) 0.0154(15)
N1 0.0175(12) 0.0259(13) 0.0197(12) 0.0032(9) 0.0028(9) 0.0026(10)
N2 0.0172(12) 0.0209(12) 0.0187(11) 0.0026(9) 0.0010(9) 0.0011(9)
N3 0.0187(12) 0.0212(12) 0.0309(13) 0.0056(10) -0.0037(10) -0.0012(9)
N4 0.0168(12) 0.0190(12) 0.0275(13) 0.0032(9) -0.0048(9) -0.0014(9)
N5 0.0172(12) 0.0155(12) 0.0289(13) 0.0008(9) -0.0023(9) 0.0009(9)
N6 0.0192(12) 0.0182(12) 0.0231(12) -0.0011(9) -0.0031(9) 0.0025(9)
N7 0.0242(12) 0.0177(12) 0.0243(12) -0.0015(9) -0.0021(10) 0.0054(9)
N8 0.0216(12) 0.0208(12) 0.0199(12) 0.0024(9) 0.0006(9) 0.0028(9)
N9 0.0173(11) 0.0164(12) 0.0196(11) 0.0012(9) -0.0016(9) -0.0006(9)
N10 0.0243(12) 0.0213(12) 0.0199(12) -0.0016(9) -0.0018(10) 0.0059(10)
N11 0.0219(12) 0.0299(13) 0.0184(12) -0.0028(10) -0.0032(9) 0.0038(10)
N12 0.0145(11) 0.0229(12) 0.0187(11) 0.0024(9) -0.0001(9) -0.0018(9)
N13 0.0164(11) 0.0160(11) 0.0202(11) -0.0011(9) -0.0017(9) -0.0008(9)
N14 0.0172(11) 0.0158(11) 0.0197(11) -0.0003(9) -0.0010(9) 0.0010(9)
N15 0.0199(12) 0.0155(12) 0.0240(12) -0.0021(9) -0.0027(9) 0.0012(9)
N16 0.0162(11) 0.0269(13) 0.0249(12) 0.0021(10) -0.0010(10) 0.0013(10)
C1 0.0227(15) 0.0202(14) 0.0229(14) 0.0065(11) 0.0010(12) -0.0002(11)
C2 0.0206(14) 0.0210(14) 0.0264(15) 0.0058(12) 0.0062(11) 0.0045(11)
C3 0.0168(13) 0.0208(14) 0.0206(14) -0.0021(11) -0.0005(11) -0.0013(10)
C4 0.0162(13) 0.0190(14) 0.0218(13) 0.0004(11) -0.0013(11) -0.0018(10)
C5 0.0215(15) 0.0263(16) 0.0303(16) 0.0081(12) -0.0098(12) -0.0059(12)
C6 0.0204(14) 0.0223(15) 0.0239(14) 0.0025(11) -0.0034(11) -0.0002(11)
C7 0.0236(14) 0.0187(14) 0.0222(14) 0.0020(11) -0.0040(11) -0.0002(11)
C8 0.0220(14) 0.0170(13) 0.0204(13) 0.0048(11) 0.0002(11) 0.0009(11)
C9 0.0306(16) 0.0172(14) 0.0205(14) 0.0020(11) 0.0014(12) 0.0049(11)
C10 0.0169(13) 0.0177(13) 0.0200(13) -0.0013(11) 0.0010(10) 0.0012(10)
C11 0.0191(13) 0.0175(13) 0.0179(13) -0.0002(10) -0.0001(10) -0.0008(11)
C12 0.0202(13) 0.0168(13) 0.0228(14) -0.0006(11) 0.0010(11) 0.0000(10)
C13 0.0263(15) 0.0275(15) 0.0215(14) -0.0034(12) -0.0064(12) 0.0029(12)
C14 0.0171(13) 0.0210(14) 0.0234(14) -0.0008(11) 0.0026(11) -0.0020(11)
C15 0.0178(13) 0.0132(12) 0.0219(13) -0.0012(10) 0.0013(11) 0.0017(10)
C16 0.0159(13) 0.0171(13) 0.0215(13) 0.0005(11) 0.0026(10) 0.0006(10)
C17 0.0178(13) 0.0177(14) 0.0212(14) 0.0006(10) -0.0002(10) -0.0001(10)
C18 0.0206(14) 0.0158(13) 0.0200(13) 0.0015(11) 0.0005(11) -0.0011(10)
C19 0.0127(12) 0.0186(14) 0.0252(14) 0.0007(11) 0.0000(11) -0.0003(10)
C20 0.0149(13) 0.0166(14) 0.0300(15) -0.0039(11) -0.0026(11) 0.0008(10)
C21 0.0168(13) 0.0159(13) 0.0218(13) 0.0004(10) 0.0007(11) -0.0001(10)
C22 0.0185(13) 0.0225(14) 0.0245(14) -0.0044(11) -0.0035(11) 0.0024(11)
C23 0.0175(14) 0.0263(15) 0.0255(15) -0.0015(12) -0.0090(11) -0.0004(12)
C24 0.0166(13) 0.0362(17) 0.0199(14) -0.0038(12) -0.0019(11) -0.0020(12)
C26 0.050(2) 0.053(2) 0.0333(19) -0.0163(17) -0.0009(16) -0.0018(18)
C27 0.044(2) 0.0335(19) 0.059(2) -0.0215(18) 0.0074(18) -0.0139(16)
C28 0.059(3) 0.032(2) 0.070(3) -0.0162(19) -0.011(2) 0.0019(19)
C29 0.056(2) 0.044(2) 0.048(2) -0.0265(18) -0.0188(19) 0.0182(19)
C30 0.063(3) 0.047(2) 0.046(2) -0.0170(18) -0.017(2) 0.018(2)
C31 0.066(3) 0.093(4) 0.035(2) -0.013(2) -0.010(2) 0.033(3)
C33 0.048(2) 0.043(2) 0.110(4) 0.002(3) 0.006(3) -0.013(2)
C34 0.075(3) 0.041(3) 0.103(4) 0.001(3) -0.017(3) -0.010(2)
O1S 0.0350(14) 0.0569(18) 0.0694(19) -0.0300(15) 0.0097(13) -0.0058(12)
O2S 0.0528(17) 0.073(2) 0.0446(16) -0.0116(14) -0.0138(13) -0.0165(15)
O3S 0.0522(18) 0.082(2) 0.061(2) -0.0081(17) -0.0169(15) 0.0040(16)
O4S 0.078(3) 0.0272(17) 0.0442(19) -0.0015(14) -0.0424(19) 0.0087(16)
O7S 0.042(6) 0.035(6) 0.035(6) 0.003(4) -0.005(4) 0.012(4)
O8S 0.030(6) 0.046(7) 0.070(8) -0.006(6) -0.001(5) 0.003(5)
O6S 0.087(4) 0.062(3) 0.086(4) -0.006(2) 0.027(3) 0.005(2)
O9S 0.046(3) 0.058(3) 0.215(8) 0.028(4) 0.041(4) 0.015(2)
O5S 0.044(4) 0.033(3) 0.046(3) -0.0025(18) -0.017(2) 0.005(2)
O10S 0.17(2) 0.087(15) 0.065(12) 0.021(10) -0.044(13) -0.031(13)
O11S 0.13(5) 0.055(16) 0.027(12) -0.007(10) -0.027(16) 0.01(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C32 C26 1.345(6) . ?
C32 C31 1.382(7) . ?
C32 H32 0.9500 . ?
C25 O9 1.225(5) . ?
C25 O10 1.330(6) . ?
C25 C34 1.442(8) . ?
O1 C1 1.220(4) . ?
O2 C10 1.224(3) . ?
O3 C6 1.215(4) . ?
O4 C8 1.227(4) . ?
O5 C15 1.223(3) . ?
O6 C19 1.221(3) . ?
O7 C13 1.223(4) . ?
O8 C23 1.216(4) . ?
O10 C26 1.434(5) . ?
N1 C1 1.370(4) . ?
N1 C14 1.441(4) . ?
N1 C2 1.447(4) . ?
N2 C15 1.373(4) . ?
N2 C2 1.449(4) . ?
N2 C3 1.454(4) . ?
N3 C23 1.370(4) . ?
N3 C5 1.446(4) . ?
N3 C4 1.459(4) . ?
N4 C6 1.378(4) . ?
N4 C5 1.446(4) . ?
N4 C11 1.449(4) . ?
N5 C6 1.377(4) 5_767 ?
N5 C17 1.442(4) 5_767 ?
N5 C7 1.446(4) . ?
N6 C8 1.370(4) . ?
N6 C7 1.449(4) . ?
N6 C21 1.452(4) . ?
N7 C8 1.365(4) . ?
N7 C9 1.447(4) . ?
N7 C18 1.448(4) . ?
N8 C1 1.378(4) . ?
N8 C12 1.449(4) . ?
N8 C9 1.449(4) . ?
N9 C10 1.366(4) . ?
N9 C16 1.447(4) . ?
N9 C11 1.448(4) . ?
N10 C13 1.368(4) . ?
N10 C22 1.446(4) . ?
N10 C12 1.454(4) . ?
N11 C13 1.371(4) . ?
N11 C24 1.442(4) . ?
N11 C14 1.449(4) . ?
N12 C15 1.368(4) . ?
N12 C4 1.438(4) . ?
N12 C16 1.443(3) . ?
N13 C10 1.375(4) . ?
N13 C20 1.451(3) 5_767 ?
N13 C17 1.452(4) . ?
N14 C19 1.387(4) . ?
N14 C18 1.456(3) . ?
N14 C22 1.457(4) . ?
N15 C19 1.362(4) . ?
N15 C21 1.443(4) . ?
N15 C20 1.445(4) . ?
N16 C23 1.377(4) . ?
N16 C3 1.440(4) . ?
N16 C24 1.441(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.551(4) . ?
C3 H3 1.0000 . ?
C4 H4 1.0000 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.377(4) 5_767 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C17 1.549(4) . ?
C11 H11 1.0000 . ?
C12 C14 1.547(4) . ?
C12 H12 1.0000 . ?
C14 H14 1.0000 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N5 1.442(4) 5_767 ?
C17 H17 1.0000 . ?
C18 C21 1.550(4) . ?
C18 H18 1.0000 . ?
C20 N13 1.451(3) 5_767 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21 1.0000 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.364(6) . ?
C27 C33 1.391(6) . ?
C27 C28 1.468(6) . ?
C28 C29 1.340(7) . ?
C28 H28 0.9500 . ?
C29 C31 1.410(7) . ?
C29 C30 1.523(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 0.9500 . ?
C33 C34 1.308(8) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 C32 C31 115.1(5) . . ?
C26 C32 H32 121.8 . . ?
C31 C32 H32 123.1 . . ?
O9 C25 O10 118.4(5) . . ?
O9 C25 C34 122.8(5) . . ?
O10 C25 C34 118.8(4) . . ?
C25 O10 C26 120.5(4) . . ?
C1 N1 C14 112.2(2) . . ?
C1 N1 C2 121.2(2) . . ?
C14 N1 C2 122.7(2) . . ?
C15 N2 C2 120.6(2) . . ?
C15 N2 C3 111.3(2) . . ?
C2 N2 C3 120.7(2) . . ?
C23 N3 C5 121.2(2) . . ?
C23 N3 C4 112.2(2) . . ?
C5 N3 C4 122.5(2) . . ?
C6 N4 C5 121.2(2) . . ?
C6 N4 C11 112.1(2) . . ?
C5 N4 C11 121.9(2) . . ?
C6 N5 C17 113.0(2) 5_767 5_767 ?
C6 N5 C7 123.0(2) 5_767 . ?
C17 N5 C7 123.2(2) 5_767 . ?
C8 N6 C7 121.7(2) . . ?
C8 N6 C21 111.9(2) . . ?
C7 N6 C21 122.6(2) . . ?
C8 N7 C9 122.9(2) . . ?
C8 N7 C18 112.8(2) . . ?
C9 N7 C18 123.9(2) . . ?
C1 N8 C12 111.2(2) . . ?
C1 N8 C9 119.8(2) . . ?
C12 N8 C9 119.9(2) . . ?
C10 N9 C16 123.0(2) . . ?
C10 N9 C11 112.5(2) . . ?
C16 N9 C11 124.0(2) . . ?
C13 N10 C22 122.1(2) . . ?
C13 N10 C12 112.1(2) . . ?
C22 N10 C12 123.3(2) . . ?
C13 N11 C24 122.3(2) . . ?
C13 N11 C14 111.9(2) . . ?
C24 N11 C14 122.0(2) . . ?
C15 N12 C4 112.7(2) . . ?
C15 N12 C16 123.3(2) . . ?
C4 N12 C16 123.9(2) . . ?
C10 N13 C20 119.6(2) . 5_767 ?
C10 N13 C17 111.1(2) . . ?
C20 N13 C17 120.6(2) 5_767 . ?
C19 N14 C18 110.7(2) . . ?
C19 N14 C22 118.6(2) . . ?
C18 N14 C22 120.3(2) . . ?
C19 N15 C21 113.0(2) . . ?
C19 N15 C20 122.5(2) . . ?
C21 N15 C20 122.7(2) . . ?
C23 N16 C3 112.3(2) . . ?
C23 N16 C24 122.4(2) . . ?
C3 N16 C24 125.2(2) . . ?
O1 C1 N1 125.8(3) . . ?
O1 C1 N8 126.0(3) . . ?
N1 C1 N8 108.3(2) . . ?
N1 C2 N2 113.4(2) . . ?
N1 C2 H2A 108.9 . . ?
N2 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
N2 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N16 C3 N2 115.0(2) . . ?
N16 C3 C4 103.2(2) . . ?
N2 C3 C4 103.0(2) . . ?
N16 C3 H3 111.7 . . ?
N2 C3 H3 111.7 . . ?
C4 C3 H3 111.7 . . ?
N12 C4 N3 114.3(2) . . ?
N12 C4 C3 102.9(2) . . ?
N3 C4 C3 102.5(2) . . ?
N12 C4 H4 112.1 . . ?
N3 C4 H4 112.1 . . ?
C3 C4 H4 112.1 . . ?
N4 C5 N3 113.6(2) . . ?
N4 C5 H5A 108.8 . . ?
N3 C5 H5A 108.8 . . ?
N4 C5 H5B 108.8 . . ?
N3 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
O3 C6 N5 126.3(3) . 5_767 ?
O3 C6 N4 126.5(3) . . ?
N5 C6 N4 107.2(2) 5_767 . ?
N5 C7 N6 113.7(2) . . ?
N5 C7 H7A 108.8 . . ?
N6 C7 H7A 108.8 . . ?
N5 C7 H7B 108.8 . . ?
N6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
O4 C8 N7 125.7(3) . . ?
O4 C8 N6 125.9(3) . . ?
N7 C8 N6 108.4(2) . . ?
N7 C9 N8 113.2(2) . . ?
N7 C9 H9A 108.9 . . ?
N8 C9 H9A 108.9 . . ?
N7 C9 H9B 108.9 . . ?
N8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
O2 C10 N9 125.5(3) . . ?
O2 C10 N13 126.4(3) . . ?
N9 C10 N13 108.2(2) . . ?
N9 C11 N4 115.2(2) . . ?
N9 C11 C17 102.9(2) . . ?
N4 C11 C17 103.1(2) . . ?
N9 C11 H11 111.6 . . ?
N4 C11 H11 111.6 . . ?
C17 C11 H11 111.6 . . ?
N8 C12 N10 114.8(2) . . ?
N8 C12 C14 104.0(2) . . ?
N10 C12 C14 103.0(2) . . ?
N8 C12 H12 111.5 . . ?
N10 C12 H12 111.5 . . ?
C14 C12 H12 111.5 . . ?
O7 C13 N10 125.7(3) . . ?
O7 C13 N11 126.1(3) . . ?
N10 C13 N11 108.2(2) . . ?
N1 C14 N11 114.9(2) . . ?
N1 C14 C12 103.2(2) . . ?
N11 C14 C12 103.8(2) . . ?
N1 C14 H14 111.4 . . ?
N11 C14 H14 111.4 . . ?
C12 C14 H14 111.4 . . ?
O5 C15 N12 125.5(3) . . ?
O5 C15 N2 126.3(3) . . ?
N12 C15 N2 108.2(2) . . ?
N12 C16 N9 114.5(2) . . ?
N12 C16 H16A 108.6 . . ?
N9 C16 H16A 108.6 . . ?
N12 C16 H16B 108.6 . . ?
N9 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
N5 C17 N13 114.4(2) 5_767 . ?
N5 C17 C11 103.1(2) 5_767 . ?
N13 C17 C11 103.2(2) . . ?
N5 C17 H17 111.8 5_767 . ?
N13 C17 H17 111.8 . . ?
C11 C17 H17 111.8 . . ?
N7 C18 N14 114.6(2) . . ?
N7 C18 C21 102.9(2) . . ?
N14 C18 C21 104.0(2) . . ?
N7 C18 H18 111.6 . . ?
N14 C18 H18 111.6 . . ?
C21 C18 H18 111.6 . . ?
O6 C19 N15 126.4(3) . . ?
O6 C19 N14 125.2(3) . . ?
N15 C19 N14 108.5(2) . . ?
N15 C20 N13 112.7(2) . 5_767 ?
N15 C20 H20A 109.1 . . ?
N13 C20 H20A 109.1 5_767 . ?
N15 C20 H20B 109.1 . . ?
N13 C20 H20B 109.1 5_767 . ?
H20A C20 H20B 107.8 . . ?
N15 C21 N6 114.4(2) . . ?
N15 C21 C18 103.0(2) . . ?
N6 C21 C18 103.6(2) . . ?
N15 C21 H21 111.7 . . ?
N6 C21 H21 111.7 . . ?
C18 C21 H21 111.7 . . ?
N10 C22 N14 112.8(2) . . ?
N10 C22 H22A 109.0 . . ?
N14 C22 H22A 109.0 . . ?
N10 C22 H22B 109.0 . . ?
N14 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
O8 C23 N3 126.7(3) . . ?
O8 C23 N16 125.5(3) . . ?
N3 C23 N16 107.8(2) . . ?
N16 C24 N11 114.7(2) . . ?
N16 C24 H24A 108.6 . . ?
N11 C24 H24A 108.6 . . ?
N16 C24 H24B 108.6 . . ?
N11 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C32 C26 C27 126.8(4) . . ?
C32 C26 O10 116.3(4) . . ?
C27 C26 O10 116.8(4) . . ?
C26 C27 C33 123.8(5) . . ?
C26 C27 C28 115.5(4) . . ?
C33 C27 C28 120.7(5) . . ?
C29 C28 C27 120.5(5) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C31 118.3(4) . . ?
C28 C29 C30 120.4(5) . . ?
C31 C29 C30 121.3(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C29 123.7(5) . . ?
C32 C31 H31 118.1 . . ?
C29 C31 H31 118.1 . . ?
C34 C33 C27 117.4(6) . . ?
C34 C33 H33 121.3 . . ?
C27 C33 H33 121.3 . . ?
C33 C34 C25 122.6(6) . . ?
C33 C34 H34 118.7 . . ?
C25 C34 H34 118.7 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        66.53
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.164
# start Validation Reply Form
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: It is a sophisticated work with many analytical methods and
calculations. Based on that many experts from different research areas
participated in this work.
;
_vrf_PLAT306_I                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3S
RESPONSE:
All non-hydrogen atoms of the main molecules, which are subject of interest
of this paper, are refined anisotropically. All H-atoms to these molecules are
generated by HFIX. Parallel with the main molecules, the host and the two
guests, we observed many molecules of disordered water. We did not attach
H-atoms to disordered water molecules. We localized 54 water molecules per cell
and do not have any evidences for H2O inside of the cavity.
Because of the observed solvent disorder the final
refinement error, R1 = 7.07%. The observed A, B and C alerts, after CIF file
PLATON check, are due to disordered solvent molecules too.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact O4S .. O8S .. 2.45 Ang.
Short Inter D...A Contact O5S .. O11S .. 0.87 Ang.
Short Inter D...A Contact O5S .. O10S .. 1.30 Ang.
Short Inter D...A Contact O6S .. O11S .. 0.87 Ang.
RESPONSE:
O4S is refined with 75% probability and O8S with 23.8%, more likely
they do not exist together.
O5s, O10s and O11s are solved as 3 components of one disorder position.
O6S is refined with 76.2% probability and O8S with 14%, more likely
they do not exist together.
;
# end Validation Reply Form