# 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
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
C.Redshaw
H.Johnson
M.Elsegood
J.Wright
T.Yamato
S.Giovanni
A.Mueller
_publ_contact_author_name        'Carl Redshaw'
_publ_contact_author_email       carl.redshaw@uea.ac.uk

data_II
_database_code_depnum_ccdc_archive 'CCDC 835504'
#TrackingRef '- Vanadyl-calixarenes.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '(O=)V{Cax[4](O)3(OBu)}, 2MeCN'
_chemical_formula_moiety         'C49 H63 O5 V, 2(C2 H3 N)'
_chemical_formula_sum            'C53 H69 N2 O5 V'
_chemical_formula_weight         865.04

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'
V V 0.3005 0.5294 '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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   12.5308(5)
_cell_length_b                   13.2108(7)
_cell_length_c                   17.1002(7)
_cell_angle_alpha                72.630(4)
_cell_angle_beta                 74.402(3)
_cell_angle_gamma                65.923(4)
_cell_volume                     2431.25(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    8387
_cell_measurement_theta_min      3.1746
_cell_measurement_theta_max      27.4989

_exptl_crystal_description       shard
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5765
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32179
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         27.78
_reflns_number_total             11178
_reflns_number_gt                6521
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_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^)+(0.0556P)^2^] 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         11178
_refine_ls_number_parameters     565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_restrained_S_all      0.941
_refine_ls_shift/su_max          0.007
_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
V1 V 0.34622(3) 0.76871(3) 0.48190(2) 0.02589(11) Uani 1 1 d . . .
O1 O 0.32842(12) 0.64344(12) 0.42006(8) 0.0256(3) Uani 1 1 d . . .
O2 O 0.49649(12) 0.71400(12) 0.42920(9) 0.0300(4) Uani 1 1 d . . .
O3 O 0.36024(12) 0.88344(12) 0.51024(9) 0.0258(3) Uani 1 1 d . . .
O4 O 0.19863(13) 0.84117(12) 0.45953(9) 0.0300(4) Uani 1 1 d . . .
O5 O 0.33880(13) 0.68241(12) 0.56895(9) 0.0311(4) Uani 1 1 d . . .
C1 C 0.33117(19) 0.66771(17) 0.33366(12) 0.0241(5) Uani 1 1 d . . .
C2 C 0.43952(18) 0.63594(17) 0.27984(13) 0.0240(5) Uani 1 1 d . . .
C3 C 0.55863(18) 0.58326(18) 0.30891(13) 0.0273(5) Uani 1 1 d . . .
H3A H 0.5487 0.5438 0.3680 0.033 Uiso 1 1 calc R . .
H3B H 0.6142 0.5263 0.2761 0.033 Uiso 1 1 calc R . .
C4 C 0.61029(17) 0.67290(17) 0.29919(13) 0.0242(5) Uani 1 1 d . . .
C5 C 0.57695(18) 0.73493(18) 0.36075(13) 0.0245(5) Uani 1 1 d . . .
C6 C 0.62741(17) 0.81453(17) 0.35424(13) 0.0238(5) Uani 1 1 d . . .
C7 C 0.59224(17) 0.87959(18) 0.42220(13) 0.0256(5) Uani 1 1 d . . .
H7A H 0.5790 0.8294 0.4770 0.031 Uiso 1 1 calc R . .
H7B H 0.6573 0.9042 0.4216 0.031 Uiso 1 1 calc R . .
C8 C 0.48035(18) 0.98248(18) 0.40994(12) 0.0233(5) Uani 1 1 d . . .
C9 C 0.36813(17) 0.97825(18) 0.45105(12) 0.0222(5) Uani 1 1 d . . .
C10 C 0.26534(18) 1.07156(18) 0.43435(12) 0.0235(5) Uani 1 1 d . . .
C11 C 0.14332(17) 1.06693(18) 0.47262(13) 0.0237(5) Uani 1 1 d . . .
H11A H 0.0893 1.1410 0.4862 0.028 Uiso 1 1 calc R . .
H11B H 0.1477 1.0081 0.5248 0.028 Uiso 1 1 calc R . .
C12 C 0.09559(17) 1.03931(18) 0.41210(12) 0.0230(5) Uani 1 1 d . . .
C13 C 0.12646(17) 0.92690(18) 0.40788(12) 0.0239(5) Uani 1 1 d . . .
C14 C 0.08059(18) 0.89809(18) 0.35517(13) 0.0245(5) Uani 1 1 d . . .
C15 C 0.10797(18) 0.77553(18) 0.35702(13) 0.0272(5) Uani 1 1 d . . .
H15A H 0.0440 0.7690 0.3374 0.033 Uiso 1 1 calc R . .
H15B H 0.1109 0.7311 0.4149 0.033 Uiso 1 1 calc R . .
C16 C 0.22508(19) 0.72716(18) 0.30266(13) 0.0265(5) Uani 1 1 d . . .
C17 C 0.22885(19) 0.74932(19) 0.21702(13) 0.0288(5) Uani 1 1 d . . .
H17 H 0.1566 0.7888 0.1957 0.035 Uiso 1 1 calc R . .
C18 C 0.33426(19) 0.71582(19) 0.16155(13) 0.0284(5) Uani 1 1 d . . .
C19 C 0.43821(19) 0.65916(18) 0.19544(13) 0.0269(5) Uani 1 1 d . . .
H19 H 0.5114 0.6354 0.1590 0.032 Uiso 1 1 calc R . .
C20 C 0.3399(2) 0.7392(2) 0.06744(13) 0.0343(6) Uani 1 1 d . . .
C21 C 0.2181(2) 0.8073(3) 0.04204(16) 0.0615(9) Uani 1 1 d . . .
H21A H 0.1653 0.7642 0.0687 0.092 Uiso 1 1 calc R . .
H21B H 0.2260 0.8216 -0.0185 0.092 Uiso 1 1 calc R . .
H21C H 0.1849 0.8798 0.0596 0.092 Uiso 1 1 calc R . .
C22 C 0.3912(3) 0.6260(2) 0.04025(16) 0.0550(8) Uani 1 1 d . . .
H22A H 0.4713 0.5840 0.0537 0.083 Uiso 1 1 calc R . .
H22B H 0.3947 0.6401 -0.0198 0.083 Uiso 1 1 calc R . .
H22C H 0.3405 0.5814 0.0695 0.083 Uiso 1 1 calc R . .
C23 C 0.4210(2) 0.8072(2) 0.02286(15) 0.0506(7) Uani 1 1 d . . .
H23A H 0.3910 0.8781 0.0423 0.076 Uiso 1 1 calc R . .
H23B H 0.4226 0.8245 -0.0372 0.076 Uiso 1 1 calc R . .
H23C H 0.5014 0.7624 0.0350 0.076 Uiso 1 1 calc R . .
C24 C 0.01140(18) 0.98620(19) 0.30093(13) 0.0271(5) Uani 1 1 d . . .
H24 H -0.0183 0.9678 0.2635 0.033 Uiso 1 1 calc R . .
C25 C -0.01637(18) 1.09992(19) 0.29894(13) 0.0277(5) Uani 1 1 d . . .
C26 C 0.02499(17) 1.12424(19) 0.35670(13) 0.0258(5) Uani 1 1 d . . .
H26 H 0.0043 1.2013 0.3583 0.031 Uiso 1 1 calc R . .
C27 C -0.0895(2) 1.1928(2) 0.23502(14) 0.0347(6) Uani 1 1 d . . .
C28 C -0.0249(2) 1.1769(2) 0.14689(15) 0.0485(7) Uani 1 1 d . . .
H28A H 0.0523 1.1848 0.1370 0.073 Uiso 1 1 calc R . .
H28B H -0.0726 1.2346 0.1061 0.073 Uiso 1 1 calc R . .
H28C H -0.0133 1.1012 0.1415 0.073 Uiso 1 1 calc R . .
C29 C -0.2110(2) 1.1814(2) 0.24953(17) 0.0535(8) Uani 1 1 d . . .
H29A H -0.2000 1.1079 0.2401 0.080 Uiso 1 1 calc R . .
H29B H -0.2599 1.2426 0.2109 0.080 Uiso 1 1 calc R . .
H29C H -0.2505 1.1864 0.3068 0.080 Uiso 1 1 calc R . .
C30 C -0.1098(2) 1.3115(2) 0.24219(17) 0.0525(7) Uani 1 1 d . . .
H30A H -0.1547 1.3236 0.2972 0.079 Uiso 1 1 calc R . .
H30B H -0.1546 1.3677 0.1993 0.079 Uiso 1 1 calc R . .
H30C H -0.0331 1.3197 0.2346 0.079 Uiso 1 1 calc R . .
C31 C 0.27628(18) 1.16963(18) 0.37878(13) 0.0249(5) Uani 1 1 d . . .
H31 H 0.2062 1.2332 0.3681 0.030 Uiso 1 1 calc R . .
C32 C 0.38528(18) 1.17838(18) 0.33830(13) 0.0255(5) Uani 1 1 d . . .
C33 C 0.48566(18) 1.08226(18) 0.35574(13) 0.0253(5) Uani 1 1 d . . .
H33 H 0.5614 1.0857 0.3289 0.030 Uiso 1 1 calc R . .
C34 C 0.39794(19) 1.28793(19) 0.28117(14) 0.0309(5) Uani 1 1 d . . .
C35 C 0.4671(2) 1.3265(2) 0.32061(17) 0.0485(7) Uani 1 1 d . . .
H35A H 0.4253 1.3367 0.3766 0.073 Uiso 1 1 calc R . .
H35B H 0.4736 1.3986 0.2865 0.073 Uiso 1 1 calc R . .
H35C H 0.5466 1.2689 0.3239 0.073 Uiso 1 1 calc R . .
C36 C 0.2787(2) 1.3832(2) 0.27132(18) 0.0566(8) Uani 1 1 d . . .
H36A H 0.2321 1.3600 0.2470 0.085 Uiso 1 1 calc R . .
H36B H 0.2915 1.4516 0.2347 0.085 Uiso 1 1 calc R . .
H36C H 0.2358 1.3992 0.3259 0.085 Uiso 1 1 calc R . .
C37 C 0.4668(2) 1.2666(2) 0.19535(15) 0.0450(6) Uani 1 1 d . . .
H37A H 0.5437 1.2056 0.2014 0.068 Uiso 1 1 calc R . .
H37B H 0.4791 1.3361 0.1606 0.068 Uiso 1 1 calc R . .
H37C H 0.4215 1.2445 0.1691 0.068 Uiso 1 1 calc R . .
C38 C 0.70649(17) 0.83526(18) 0.28225(13) 0.0264(5) Uani 1 1 d . . .
H38 H 0.7400 0.8903 0.2769 0.032 Uiso 1 1 calc R . .
C39 C 0.73892(18) 0.77889(18) 0.21753(13) 0.0276(5) Uani 1 1 d . . .
C40 C 0.68999(18) 0.69654(18) 0.22885(13) 0.0276(5) Uani 1 1 d . . .
H40 H 0.7122 0.6550 0.1867 0.033 Uiso 1 1 calc R . .
C41 C 0.8203(2) 0.8062(2) 0.13617(14) 0.0348(6) Uani 1 1 d . . .
C42 C 0.8701(2) 0.8934(3) 0.13706(17) 0.0543(8) Uani 1 1 d . . .
H42A H 0.8048 0.9650 0.1438 0.081 Uiso 1 1 calc R . .
H42B H 0.9236 0.9061 0.0846 0.081 Uiso 1 1 calc R . .
H42C H 0.9140 0.8653 0.1834 0.081 Uiso 1 1 calc R . .
C43 C 0.9253(2) 0.6969(2) 0.12035(17) 0.0517(7) Uani 1 1 d . . .
H43A H 0.9760 0.7142 0.0675 0.078 Uiso 1 1 calc R . .
H43B H 0.8950 0.6404 0.1179 0.078 Uiso 1 1 calc R . .
H43C H 0.9715 0.6666 0.1656 0.078 Uiso 1 1 calc R . .
C44 C 0.7501(2) 0.8525(2) 0.06482(15) 0.0536(7) Uani 1 1 d . . .
H44A H 0.6823 0.9213 0.0746 0.080 Uiso 1 1 calc R . .
H44B H 0.7215 0.7952 0.0616 0.080 Uiso 1 1 calc R . .
H44C H 0.8014 0.8706 0.0124 0.080 Uiso 1 1 calc R . .
C45 C 0.34990(19) 0.52432(18) 0.46128(13) 0.0298(5) Uani 1 1 d . . .
H45A H 0.3933 0.5042 0.5076 0.036 Uiso 1 1 calc R . .
H45B H 0.4005 0.4758 0.4212 0.036 Uiso 1 1 calc R . .
C46 C 0.2358(2) 0.50095(19) 0.49486(14) 0.0312(5) Uani 1 1 d . . .
H46A H 0.2550 0.4180 0.5145 0.037 Uiso 1 1 calc R . .
H46B H 0.1896 0.5271 0.4493 0.037 Uiso 1 1 calc R . .
C47 C 0.15932(19) 0.55936(19) 0.56638(13) 0.0306(5) Uani 1 1 d . . .
H47A H 0.2031 0.5278 0.6137 0.037 Uiso 1 1 calc R . .
H47B H 0.1473 0.6412 0.5482 0.037 Uiso 1 1 calc R . .
C48 C 0.0387(2) 0.5469(2) 0.59653(15) 0.0357(6) Uani 1 1 d . . .
H48A H -0.0060 0.5914 0.6400 0.043 Uiso 1 1 calc R . .
H48B H -0.0058 0.5796 0.5496 0.043 Uiso 1 1 calc R . .
C49 C 0.0448(2) 0.4260(2) 0.63130(16) 0.0434(6) Uani 1 1 d . . .
H49A H 0.0773 0.3842 0.5865 0.065 Uiso 1 1 calc R . .
H49B H -0.0350 0.4251 0.6564 0.065 Uiso 1 1 calc R . .
H49C H 0.0961 0.3901 0.6737 0.065 Uiso 1 1 calc R . .
N1 N 0.7334(3) 0.5268(3) 0.0722(2) 0.0887(10) Uani 1 1 d . . .
C50 C 0.7860(3) 0.5501(3) 0.0102(2) 0.0635(9) Uani 1 1 d . . .
C51 C 0.8546(4) 0.5824(3) -0.0692(2) 0.1023(14) Uani 1 1 d . . .
H51A H 0.8174 0.6638 -0.0916 0.153 Uiso 1 1 calc R . .
H51B H 0.8576 0.5391 -0.1078 0.153 Uiso 1 1 calc R . .
H51C H 0.9353 0.5663 -0.0618 0.153 Uiso 1 1 calc R . .
N2 N 0.2969(3) 0.1394(3) 0.1285(2) 0.1041(12) Uani 1 1 d . . .
C52 C 0.3318(3) 0.0557(3) 0.17414(19) 0.0542(8) Uani 1 1 d . . .
C53 C 0.3748(2) -0.0485(2) 0.23263(17) 0.0489(7) Uani 1 1 d . . .
H53A H 0.4550 -0.0936 0.2094 0.073 Uiso 1 1 calc R . .
H53B H 0.3221 -0.0912 0.2441 0.073 Uiso 1 1 calc R . .
H53C H 0.3766 -0.0320 0.2843 0.073 Uiso 1 1 calc R . .

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
V1 0.0291(2) 0.0255(2) 0.02195(19) -0.00572(15) -0.00309(15) -0.00895(16)
O1 0.0337(9) 0.0219(8) 0.0194(7) -0.0044(6) -0.0030(6) -0.0091(7)
O2 0.0326(9) 0.0299(9) 0.0282(8) -0.0119(7) 0.0018(7) -0.0123(7)
O3 0.0281(8) 0.0250(8) 0.0246(8) -0.0051(6) -0.0038(6) -0.0102(7)
O4 0.0323(9) 0.0261(9) 0.0331(9) -0.0097(7) -0.0095(7) -0.0071(7)
O5 0.0409(10) 0.0273(9) 0.0243(8) -0.0036(7) -0.0060(7) -0.0125(7)
C1 0.0317(13) 0.0207(11) 0.0221(11) -0.0059(9) -0.0037(9) -0.0109(9)
C2 0.0270(12) 0.0190(11) 0.0270(11) -0.0077(9) -0.0018(9) -0.0092(9)
C3 0.0307(13) 0.0233(12) 0.0258(11) -0.0101(9) -0.0039(9) -0.0047(10)
C4 0.0197(11) 0.0225(12) 0.0272(11) -0.0057(9) -0.0065(9) -0.0025(9)
C5 0.0204(11) 0.0231(12) 0.0256(11) -0.0065(9) -0.0050(9) -0.0019(9)
C6 0.0195(11) 0.0206(12) 0.0285(11) -0.0079(9) -0.0082(9) -0.0001(9)
C7 0.0204(11) 0.0304(13) 0.0293(12) -0.0122(10) -0.0052(9) -0.0075(9)
C8 0.0225(12) 0.0268(12) 0.0226(11) -0.0125(9) -0.0036(9) -0.0057(9)
C9 0.0222(12) 0.0250(12) 0.0232(11) -0.0110(9) -0.0041(9) -0.0080(9)
C10 0.0230(12) 0.0279(12) 0.0233(11) -0.0111(9) -0.0029(9) -0.0094(9)
C11 0.0221(12) 0.0238(12) 0.0261(11) -0.0100(9) -0.0006(9) -0.0080(9)
C12 0.0183(11) 0.0274(12) 0.0235(11) -0.0083(9) 0.0021(9) -0.0098(9)
C13 0.0180(11) 0.0276(13) 0.0233(11) -0.0075(9) 0.0018(9) -0.0073(9)
C14 0.0206(11) 0.0294(13) 0.0264(11) -0.0108(9) 0.0034(9) -0.0131(9)
C15 0.0269(12) 0.0327(13) 0.0271(11) -0.0107(10) -0.0018(9) -0.0144(10)
C16 0.0300(13) 0.0253(12) 0.0302(12) -0.0116(10) -0.0007(10) -0.0146(10)
C17 0.0282(13) 0.0323(13) 0.0279(12) -0.0095(10) -0.0045(10) -0.0107(10)
C18 0.0334(14) 0.0290(13) 0.0254(11) -0.0076(10) -0.0025(10) -0.0139(10)
C19 0.0307(13) 0.0256(12) 0.0242(11) -0.0109(9) 0.0016(9) -0.0099(10)
C20 0.0363(14) 0.0436(15) 0.0225(11) -0.0089(10) -0.0039(10) -0.0132(11)
C21 0.0488(18) 0.096(3) 0.0290(14) -0.0125(15) -0.0109(13) -0.0136(16)
C22 0.081(2) 0.0556(19) 0.0345(15) -0.0147(13) -0.0074(14) -0.0283(16)
C23 0.0636(19) 0.0566(19) 0.0297(14) -0.0032(13) -0.0043(13) -0.0260(15)
C24 0.0231(12) 0.0354(14) 0.0267(11) -0.0127(10) -0.0007(9) -0.0122(10)
C25 0.0214(12) 0.0342(14) 0.0263(11) -0.0085(10) -0.0018(9) -0.0087(10)
C26 0.0222(12) 0.0258(12) 0.0277(11) -0.0095(9) 0.0026(9) -0.0085(9)
C27 0.0317(14) 0.0366(14) 0.0303(12) -0.0067(11) -0.0093(10) -0.0046(11)
C28 0.0526(18) 0.0504(18) 0.0314(14) -0.0052(12) -0.0095(12) -0.0082(13)
C29 0.0349(16) 0.066(2) 0.0537(17) -0.0103(15) -0.0179(13) -0.0070(13)
C30 0.0656(19) 0.0377(16) 0.0475(17) -0.0051(13) -0.0274(14) -0.0035(14)
C31 0.0231(12) 0.0244(12) 0.0270(11) -0.0100(9) -0.0035(9) -0.0057(9)
C32 0.0243(12) 0.0292(13) 0.0261(11) -0.0098(9) -0.0023(9) -0.0112(10)
C33 0.0191(11) 0.0311(13) 0.0293(12) -0.0151(10) 0.0010(9) -0.0096(9)
C34 0.0286(13) 0.0294(13) 0.0335(13) -0.0089(10) 0.0035(10) -0.0130(10)
C35 0.0610(19) 0.0404(16) 0.0515(17) -0.0172(13) 0.0059(14) -0.0299(14)
C36 0.0441(17) 0.0359(16) 0.0640(19) 0.0130(14) -0.0002(14) -0.0111(13)
C37 0.0549(18) 0.0468(17) 0.0334(14) -0.0055(12) 0.0022(12) -0.0263(13)
C38 0.0203(12) 0.0270(13) 0.0329(12) -0.0101(10) -0.0041(9) -0.0071(9)
C39 0.0243(12) 0.0285(13) 0.0280(12) -0.0068(10) -0.0038(9) -0.0074(10)
C40 0.0245(12) 0.0281(13) 0.0268(12) -0.0109(10) -0.0042(9) -0.0028(10)
C41 0.0326(14) 0.0433(15) 0.0298(12) -0.0124(11) 0.0045(10) -0.0176(11)
C42 0.0584(19) 0.068(2) 0.0478(17) -0.0219(15) 0.0122(14) -0.0409(16)
C43 0.0399(16) 0.061(2) 0.0486(17) -0.0235(14) 0.0156(12) -0.0186(14)
C44 0.0617(19) 0.065(2) 0.0319(14) -0.0010(13) -0.0029(13) -0.0307(16)
C45 0.0366(14) 0.0216(12) 0.0277(12) -0.0048(9) -0.0022(10) -0.0094(10)
C46 0.0397(14) 0.0243(13) 0.0321(13) -0.0033(10) -0.0063(11) -0.0156(10)
C47 0.0341(14) 0.0294(13) 0.0285(12) -0.0066(10) -0.0038(10) -0.0121(10)
C48 0.0314(14) 0.0372(15) 0.0369(13) -0.0061(11) -0.0045(11) -0.0127(11)
C49 0.0391(15) 0.0401(16) 0.0504(16) -0.0053(13) -0.0041(12) -0.0188(12)
N1 0.087(2) 0.095(3) 0.072(2) -0.028(2) -0.0154(18) -0.0113(18)
C50 0.070(2) 0.055(2) 0.058(2) -0.0226(18) -0.0224(19) -0.0002(17)
C51 0.120(3) 0.080(3) 0.067(3) -0.009(2) -0.007(2) -0.006(2)
N2 0.137(3) 0.075(2) 0.115(3) 0.016(2) -0.080(2) -0.042(2)
C52 0.061(2) 0.057(2) 0.0548(18) -0.0079(16) -0.0250(15) -0.0243(16)
C53 0.0586(18) 0.0424(17) 0.0473(16) -0.0111(13) -0.0118(14) -0.0166(14)

_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
V1 O5 1.5884(14) . ?
V1 O4 1.7890(14) . ?
V1 O2 1.8016(15) . ?
V1 O3 1.8068(14) . ?
V1 O1 2.3196(14) . ?
O1 C1 1.409(2) . ?
O1 C45 1.463(2) . ?
O2 C5 1.365(2) . ?
O3 C9 1.376(2) . ?
O4 C13 1.370(2) . ?
C1 C16 1.394(3) . ?
C1 C2 1.400(3) . ?
C2 C19 1.386(3) . ?
C2 C3 1.518(3) . ?
C3 C4 1.516(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C40 1.388(3) . ?
C4 C5 1.398(3) . ?
C5 C6 1.397(3) . ?
C6 C38 1.392(3) . ?
C6 C7 1.515(3) . ?
C7 C8 1.513(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C33 1.382(3) . ?
C8 C9 1.408(3) . ?
C9 C10 1.397(3) . ?
C10 C31 1.393(3) . ?
C10 C11 1.511(3) . ?
C11 C12 1.516(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.393(3) . ?
C12 C26 1.395(3) . ?
C13 C14 1.396(3) . ?
C14 C24 1.390(3) . ?
C14 C15 1.504(3) . ?
C15 C16 1.511(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.397(3) . ?
C17 C18 1.393(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(3) . ?
C18 C20 1.533(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.527(3) . ?
C20 C22 1.529(3) . ?
C20 C23 1.529(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.389(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(3) . ?
C25 C27 1.537(3) . ?
C26 H26 0.9500 . ?
C27 C30 1.520(3) . ?
C27 C29 1.537(3) . ?
C27 C28 1.538(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.389(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.399(3) . ?
C32 C34 1.528(3) . ?
C33 H33 0.9500 . ?
C34 C36 1.523(3) . ?
C34 C37 1.531(3) . ?
C34 C35 1.531(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.396(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.397(3) . ?
C39 C41 1.531(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.524(3) . ?
C41 C44 1.526(3) . ?
C41 C43 1.543(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.511(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.530(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.520(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.506(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N1 C50 1.117(4) . ?
C50 C51 1.445(5) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
N2 C52 1.139(4) . ?
C52 C53 1.431(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?

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
O5 V1 O4 107.19(7) . . ?
O5 V1 O2 105.80(7) . . ?
O4 V1 O2 140.01(7) . . ?
O5 V1 O3 101.97(7) . . ?
O4 V1 O3 97.61(6) . . ?
O2 V1 O3 97.03(6) . . ?
O5 V1 O1 89.04(6) . . ?
O4 V1 O1 78.46(6) . . ?
O2 V1 O1 80.14(6) . . ?
O3 V1 O1 168.97(6) . . ?
C1 O1 C45 114.74(15) . . ?
C1 O1 V1 120.91(11) . . ?
C45 O1 V1 121.84(11) . . ?
C5 O2 V1 144.82(14) . . ?
C9 O3 V1 120.57(12) . . ?
C13 O4 V1 146.22(14) . . ?
C16 C1 C2 120.76(19) . . ?
C16 C1 O1 119.00(18) . . ?
C2 C1 O1 120.21(18) . . ?
C19 C2 C1 118.41(19) . . ?
C19 C2 C3 118.37(18) . . ?
C1 C2 C3 123.12(19) . . ?
C4 C3 C2 111.06(17) . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C40 C4 C5 118.49(19) . . ?
C40 C4 C3 121.08(19) . . ?
C5 C4 C3 120.42(19) . . ?
O2 C5 C6 120.11(18) . . ?
O2 C5 C4 118.81(18) . . ?
C6 C5 C4 121.04(19) . . ?
C38 C6 C5 118.00(19) . . ?
C38 C6 C7 121.42(19) . . ?
C5 C6 C7 120.53(19) . . ?
C8 C7 C6 110.72(16) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C33 C8 C9 118.26(18) . . ?
C33 C8 C7 120.54(19) . . ?
C9 C8 C7 121.17(19) . . ?
O3 C9 C10 119.99(18) . . ?
O3 C9 C8 119.70(17) . . ?
C10 C9 C8 120.26(19) . . ?
C31 C10 C9 118.83(19) . . ?
C31 C10 C11 119.51(18) . . ?
C9 C10 C11 121.62(19) . . ?
C10 C11 C12 109.63(16) . . ?
C10 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C26 118.01(19) . . ?
C13 C12 C11 120.15(18) . . ?
C26 C12 C11 121.77(19) . . ?
O4 C13 C12 119.79(18) . . ?
O4 C13 C14 118.43(19) . . ?
C12 C13 C14 121.68(19) . . ?
C24 C14 C13 117.59(19) . . ?
C24 C14 C15 122.06(18) . . ?
C13 C14 C15 120.35(19) . . ?
C14 C15 C16 111.15(17) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C1 C16 C17 118.4(2) . . ?
C1 C16 C15 122.68(19) . . ?
C17 C16 C15 118.75(19) . . ?
C18 C17 C16 122.6(2) . . ?
C18 C17 H17 118.7 . . ?
C16 C17 H17 118.7 . . ?
C17 C18 C19 116.7(2) . . ?
C17 C18 C20 123.30(19) . . ?
C19 C18 C20 120.00(19) . . ?
C2 C19 C18 123.0(2) . . ?
C2 C19 H19 118.5 . . ?
C18 C19 H19 118.5 . . ?
C21 C20 C22 109.3(2) . . ?
C21 C20 C23 108.1(2) . . ?
C22 C20 C23 109.0(2) . . ?
C21 C20 C18 112.16(19) . . ?
C22 C20 C18 108.9(2) . . ?
C23 C20 C18 109.30(19) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C14 123.04(19) . . ?
C25 C24 H24 118.5 . . ?
C14 C24 H24 118.5 . . ?
C24 C25 C26 117.1(2) . . ?
C24 C25 C27 120.16(19) . . ?
C26 C25 C27 122.7(2) . . ?
C12 C26 C25 122.3(2) . . ?
C12 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C30 C27 C25 112.33(19) . . ?
C30 C27 C29 108.3(2) . . ?
C25 C27 C29 108.7(2) . . ?
C30 C27 C28 109.1(2) . . ?
C25 C27 C28 109.30(19) . . ?
C29 C27 C28 109.0(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C10 122.8(2) . . ?
C32 C31 H31 118.6 . . ?
C10 C31 H31 118.6 . . ?
C31 C32 C33 116.4(2) . . ?
C31 C32 C34 122.90(19) . . ?
C33 C32 C34 120.60(19) . . ?
C8 C33 C32 123.40(19) . . ?
C8 C33 H33 118.3 . . ?
C32 C33 H33 118.3 . . ?
C36 C34 C32 112.58(18) . . ?
C36 C34 C37 109.2(2) . . ?
C32 C34 C37 110.33(19) . . ?
C36 C34 C35 107.9(2) . . ?
C32 C34 C35 107.54(19) . . ?
C37 C34 C35 109.2(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C6 C38 C39 123.1(2) . . ?
C6 C38 H38 118.5 . . ?
C39 C38 H38 118.5 . . ?
C38 C39 C40 116.6(2) . . ?
C38 C39 C41 123.2(2) . . ?
C40 C39 C41 120.15(19) . . ?
C4 C40 C39 122.7(2) . . ?
C4 C40 H40 118.7 . . ?
C39 C40 H40 118.7 . . ?
C42 C41 C44 108.7(2) . . ?
C42 C41 C39 112.58(19) . . ?
C44 C41 C39 108.84(18) . . ?
C42 C41 C43 108.3(2) . . ?
C44 C41 C43 108.7(2) . . ?
C39 C41 C43 109.7(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O1 C45 C46 111.94(17) . . ?
O1 C45 H45A 109.2 . . ?
C46 C45 H45A 109.2 . . ?
O1 C45 H45B 109.2 . . ?
C46 C45 H45B 109.2 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 C47 113.10(18) . . ?
C45 C46 H46A 109.0 . . ?
C47 C46 H46A 109.0 . . ?
C45 C46 H46B 109.0 . . ?
C47 C46 H46B 109.0 . . ?
H46A C46 H46B 107.8 . . ?
C48 C47 C46 114.65(18) . . ?
C48 C47 H47A 108.6 . . ?
C46 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
C46 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
C49 C48 C47 113.93(19) . . ?
C49 C48 H48A 108.8 . . ?
C47 C48 H48A 108.8 . . ?
C49 C48 H48B 108.8 . . ?
C47 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N1 C50 C51 178.5(4) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N2 C52 C53 179.1(4) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 V1 O1 C1 -178.49(14) . . . . ?
O4 V1 O1 C1 73.75(14) . . . . ?
O2 V1 O1 C1 -72.27(14) . . . . ?
O3 V1 O1 C1 3.7(4) . . . . ?
O5 V1 O1 C45 -17.40(14) . . . . ?
O4 V1 O1 C45 -125.17(14) . . . . ?
O2 V1 O1 C45 88.81(14) . . . . ?
O3 V1 O1 C45 164.8(3) . . . . ?
O5 V1 O2 C5 -173.6(2) . . . . ?
O4 V1 O2 C5 41.8(3) . . . . ?
O3 V1 O2 C5 -69.0(2) . . . . ?
O1 V1 O2 C5 100.2(2) . . . . ?
O5 V1 O3 C9 -179.32(14) . . . . ?
O4 V1 O3 C9 -69.86(14) . . . . ?
O2 V1 O3 C9 72.83(14) . . . . ?
O1 V1 O3 C9 -1.6(4) . . . . ?
O5 V1 O4 C13 172.3(2) . . . . ?
O2 V1 O4 C13 -43.4(3) . . . . ?
O3 V1 O4 C13 67.2(2) . . . . ?
O1 V1 O4 C13 -102.4(2) . . . . ?
C45 O1 C1 C16 107.6(2) . . . . ?
V1 O1 C1 C16 -90.05(19) . . . . ?
C45 O1 C1 C2 -74.6(2) . . . . ?
V1 O1 C1 C2 87.7(2) . . . . ?
C16 C1 C2 C19 -3.7(3) . . . . ?
O1 C1 C2 C19 178.61(18) . . . . ?
C16 C1 C2 C3 172.80(18) . . . . ?
O1 C1 C2 C3 -4.9(3) . . . . ?
C19 C2 C3 C4 81.7(2) . . . . ?
C1 C2 C3 C4 -94.8(2) . . . . ?
C2 C3 C4 C40 -94.7(2) . . . . ?
C2 C3 C4 C5 84.3(2) . . . . ?
V1 O2 C5 C6 73.9(3) . . . . ?
V1 O2 C5 C4 -108.2(2) . . . . ?
C40 C4 C5 O2 178.48(18) . . . . ?
C3 C4 C5 O2 -0.6(3) . . . . ?
C40 C4 C5 C6 -3.6(3) . . . . ?
C3 C4 C5 C6 177.38(18) . . . . ?
O2 C5 C6 C38 -178.23(17) . . . . ?
C4 C5 C6 C38 3.9(3) . . . . ?
O2 C5 C6 C7 -0.9(3) . . . . ?
C4 C5 C6 C7 -178.82(18) . . . . ?
C38 C6 C7 C8 92.9(2) . . . . ?
C5 C6 C7 C8 -84.3(2) . . . . ?
C6 C7 C8 C33 -82.7(2) . . . . ?
C6 C7 C8 C9 95.1(2) . . . . ?
V1 O3 C9 C10 90.67(19) . . . . ?
V1 O3 C9 C8 -91.91(18) . . . . ?
C33 C8 C9 O3 -174.90(17) . . . . ?
C7 C8 C9 O3 7.2(3) . . . . ?
C33 C8 C9 C10 2.5(3) . . . . ?
C7 C8 C9 C10 -175.40(17) . . . . ?
O3 C9 C10 C31 175.17(17) . . . . ?
C8 C9 C10 C31 -2.2(3) . . . . ?
O3 C9 C10 C11 -7.1(3) . . . . ?
C8 C9 C10 C11 175.52(17) . . . . ?
C31 C10 C11 C12 81.4(2) . . . . ?
C9 C10 C11 C12 -96.4(2) . . . . ?
C10 C11 C12 C13 84.1(2) . . . . ?
C10 C11 C12 C26 -92.8(2) . . . . ?
V1 O4 C13 C12 -73.7(3) . . . . ?
V1 O4 C13 C14 109.7(2) . . . . ?
C26 C12 C13 O4 178.04(18) . . . . ?
C11 C12 C13 O4 1.0(3) . . . . ?
C26 C12 C13 C14 -5.5(3) . . . . ?
C11 C12 C13 C14 177.52(18) . . . . ?
O4 C13 C14 C24 -177.52(18) . . . . ?
C12 C13 C14 C24 5.9(3) . . . . ?
O4 C13 C14 C15 1.4(3) . . . . ?
C12 C13 C14 C15 -175.10(19) . . . . ?
C24 C14 C15 C16 94.3(2) . . . . ?
C13 C14 C15 C16 -84.6(2) . . . . ?
C2 C1 C16 C17 3.1(3) . . . . ?
O1 C1 C16 C17 -179.14(18) . . . . ?
C2 C1 C16 C15 -172.43(19) . . . . ?
O1 C1 C16 C15 5.3(3) . . . . ?
C14 C15 C16 C1 95.0(2) . . . . ?
C14 C15 C16 C17 -80.5(2) . . . . ?
C1 C16 C17 C18 -0.9(3) . . . . ?
C15 C16 C17 C18 174.8(2) . . . . ?
C16 C17 C18 C19 -0.7(3) . . . . ?
C16 C17 C18 C20 179.9(2) . . . . ?
C1 C2 C19 C18 2.1(3) . . . . ?
C3 C2 C19 C18 -174.59(19) . . . . ?
C17 C18 C19 C2 0.1(3) . . . . ?
C20 C18 C19 C2 179.6(2) . . . . ?
C17 C18 C20 C21 2.4(3) . . . . ?
C19 C18 C20 C21 -177.0(2) . . . . ?
C17 C18 C20 C22 -118.7(2) . . . . ?
C19 C18 C20 C22 61.9(3) . . . . ?
C17 C18 C20 C23 122.3(2) . . . . ?
C19 C18 C20 C23 -57.1(3) . . . . ?
C13 C14 C24 C25 -2.0(3) . . . . ?
C15 C14 C24 C25 179.07(19) . . . . ?
C14 C24 C25 C26 -2.2(3) . . . . ?
C14 C24 C25 C27 177.7(2) . . . . ?
C13 C12 C26 C25 1.0(3) . . . . ?
C11 C12 C26 C25 177.95(18) . . . . ?
C24 C25 C26 C12 2.7(3) . . . . ?
C27 C25 C26 C12 -177.2(2) . . . . ?
C24 C25 C27 C30 -179.5(2) . . . . ?
C26 C25 C27 C30 0.4(3) . . . . ?
C24 C25 C27 C29 60.6(3) . . . . ?
C26 C25 C27 C29 -119.5(2) . . . . ?
C24 C25 C27 C28 -58.3(3) . . . . ?
C26 C25 C27 C28 121.6(2) . . . . ?
C9 C10 C31 C32 0.8(3) . . . . ?
C11 C10 C31 C32 -177.03(18) . . . . ?
C10 C31 C32 C33 0.4(3) . . . . ?
C10 C31 C32 C34 -176.40(19) . . . . ?
C9 C8 C33 C32 -1.4(3) . . . . ?
C7 C8 C33 C32 176.56(18) . . . . ?
C31 C32 C33 C8 0.0(3) . . . . ?
C34 C32 C33 C8 176.80(19) . . . . ?
C31 C32 C34 C36 -2.3(3) . . . . ?
C33 C32 C34 C36 -178.9(2) . . . . ?
C31 C32 C34 C37 -124.6(2) . . . . ?
C33 C32 C34 C37 58.8(3) . . . . ?
C31 C32 C34 C35 116.4(2) . . . . ?
C33 C32 C34 C35 -60.3(3) . . . . ?
C5 C6 C38 C39 -1.2(3) . . . . ?
C7 C6 C38 C39 -178.52(18) . . . . ?
C6 C38 C39 C40 -1.6(3) . . . . ?
C6 C38 C39 C41 176.4(2) . . . . ?
C5 C4 C40 C39 0.6(3) . . . . ?
C3 C4 C40 C39 179.66(19) . . . . ?
C38 C39 C40 C4 1.9(3) . . . . ?
C41 C39 C40 C4 -176.17(19) . . . . ?
C38 C39 C41 C42 5.1(3) . . . . ?
C40 C39 C41 C42 -177.0(2) . . . . ?
C38 C39 C41 C44 -115.5(2) . . . . ?
C40 C39 C41 C44 62.4(3) . . . . ?
C38 C39 C41 C43 125.7(2) . . . . ?
C40 C39 C41 C43 -56.4(3) . . . . ?
C1 O1 C45 C46 -92.9(2) . . . . ?
V1 O1 C45 C46 104.93(17) . . . . ?
O1 C45 C46 C47 -67.1(2) . . . . ?
C45 C46 C47 C48 174.60(18) . . . . ?
C46 C47 C48 C49 62.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.78
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.050

data_III
_database_code_depnum_ccdc_archive 'CCDC 835505'
#TrackingRef '- IIInew.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H80 O9 V2, 1.5(C2 H3 N)'
_chemical_formula_sum            'C59 H84.50 N1.50 O9 V2'
_chemical_formula_weight         1060.66

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'
V V 0.3005 0.5294 '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
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   16.663(3)
_cell_length_b                   13.179(2)
_cell_length_c                   26.712(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.201(2)
_cell_angle_gamma                90.00
_cell_volume                     5850.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4529
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      20.20

_exptl_crystal_description       LATH
_exptl_crystal_colour            ORANGE
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2268
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6942
_diffrn_radiation_type           SYNCHROTRON
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        4
_diffrn_reflns_number            36467
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         22.50
_reflns_number_total             8197
_reflns_number_gt                4889
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_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 and local programs'

_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^)+(0.1281P)^2^+10.5321P] 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     SHELXL
_refine_ls_extinction_coef       0.029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         8197
_refine_ls_number_parameters     726
_refine_ls_number_restraints     295
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_ref         0.2686
_refine_ls_wR_factor_gt          0.2310
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.59013(8) 0.52481(10) 0.19261(5) 0.0694(5) Uani 1 1 d . . .
V2 V 0.76791(8) 0.45674(10) 0.15543(6) 0.0752(5) Uani 1 1 d . . .
O5 O 0.6624(3) 0.4694(4) 0.15515(19) 0.0714(14) Uani 1 1 d . . .
O6 O 0.5198(3) 0.4449(4) 0.1971(2) 0.0840(17) Uani 1 1 d . . .
O8 O 0.7895(4) 0.3436(4) 0.1429(3) 0.109(2) Uani 1 1 d . . .
O1 O 0.6881(3) 0.3522(3) 0.25089(18) 0.0595(12) Uani 1 1 d DU . .
C45 C 0.6362(8) 0.2650(8) 0.2376(6) 0.065(4) Uani 0.505(14) 1 d PDU A 1
H45A H 0.6132 0.2722 0.2026 0.079 Uiso 0.505(14) 1 calc PR A 1
H45B H 0.5913 0.2630 0.2598 0.079 Uiso 0.505(14) 1 calc PR A 1
C46 C 0.6832(8) 0.1682(8) 0.2429(7) 0.075(5) Uani 0.505(14) 1 d PDU A 1
H46A H 0.7051 0.1597 0.2781 0.089 Uiso 0.505(14) 1 calc PR A 1
H46B H 0.7289 0.1704 0.2212 0.089 Uiso 0.505(14) 1 calc PR A 1
C47 C 0.6274(4) 0.0775(5) 0.2274(3) 0.071(2) Uani 1 1 d DU . .
H47A H 0.6584 0.0143 0.2300 0.107 Uiso 0.505(14) 1 calc PR A 1
H47B H 0.6052 0.0869 0.1927 0.107 Uiso 0.505(14) 1 calc PR A 1
H47C H 0.5833 0.0742 0.2497 0.107 Uiso 0.505(14) 1 calc PR A 1
H47D H 0.5877 0.0336 0.2418 0.107 Uiso 0.495(14) 1 calc PR A 2
H47E H 0.6813 0.0487 0.2342 0.107 Uiso 0.495(14) 1 calc PR A 2
H47F H 0.6151 0.0827 0.1910 0.107 Uiso 0.495(14) 1 calc PR A 2
C45X C 0.6854(10) 0.2481(9) 0.2283(6) 0.064(5) Uiso 0.495(14) 1 d PDU A 2
H45C H 0.6722 0.2534 0.1917 0.077 Uiso 0.495(14) 1 calc PR A 2
H45D H 0.7391 0.2160 0.2338 0.077 Uiso 0.495(14) 1 calc PR A 2
C46X C 0.6245(9) 0.1836(9) 0.2510(5) 0.065(4) Uiso 0.495(14) 1 d PDU A 2
H46C H 0.5702 0.2134 0.2444 0.078 Uiso 0.495(14) 1 calc PR A 2
H46D H 0.6365 0.1792 0.2878 0.078 Uiso 0.495(14) 1 calc PR A 2
O2 O 0.6255(3) 0.5625(3) 0.25346(18) 0.0600(12) Uani 1 1 d . . .
O3 O 0.7167(2) 0.6869(3) 0.19101(16) 0.0537(12) Uani 1 1 d D . .
C48 C 0.7168(4) 0.7405(5) 0.1434(3) 0.0592(18) Uani 1 1 d D . .
H48A H 0.7010 0.6925 0.1159 0.071 Uiso 1 1 calc R . .
H48B H 0.7723 0.7637 0.1387 0.071 Uiso 1 1 calc R . .
C49 C 0.6615(4) 0.8302(5) 0.1394(3) 0.065(2) Uani 1 1 d D . .
H49A H 0.6786 0.8805 0.1656 0.078 Uiso 1 1 calc R . .
H49B H 0.6060 0.8082 0.1451 0.078 Uiso 1 1 calc R . .
C50 C 0.6624(5) 0.8793(7) 0.0875(3) 0.084(2) Uani 1 1 d D . .
H50A H 0.7178 0.8969 0.0810 0.126 Uiso 1 1 calc R . .
H50B H 0.6294 0.9409 0.0865 0.126 Uiso 1 1 calc R . .
H50C H 0.6407 0.8315 0.0619 0.126 Uiso 1 1 calc R . .
O4 O 0.8158(3) 0.4963(3) 0.21272(19) 0.0632(13) Uani 1 1 d . . .
C1 C 0.7156(4) 0.3548(5) 0.3014(3) 0.0565(18) Uani 1 1 d . A .
C2 C 0.7975(4) 0.3356(5) 0.3150(3) 0.0558(18) Uani 1 1 d . . .
C3 C 0.8212(4) 0.3320(5) 0.3654(3) 0.0587(19) Uani 1 1 d . A .
H3 H 0.8758 0.3157 0.3749 0.070 Uiso 1 1 calc R . .
C4 C 0.7705(4) 0.3507(5) 0.4033(3) 0.0576(18) Uani 1 1 d . . .
C5 C 0.6921(4) 0.3754(5) 0.3879(3) 0.0638(19) Uani 1 1 d . A .
H5 H 0.6561 0.3915 0.4127 0.077 Uiso 1 1 calc R . .
C6 C 0.6633(4) 0.3778(5) 0.3373(3) 0.0555(18) Uani 1 1 d . . .
C7 C 0.8031(5) 0.3460(6) 0.4586(3) 0.069(2) Uani 1 1 d . A .
C8 C 0.8769(5) 0.4169(6) 0.4670(3) 0.080(2) Uani 1 1 d . . .
H8A H 0.9195 0.3941 0.4462 0.119 Uiso 1 1 calc R A .
H8B H 0.8968 0.4150 0.5024 0.119 Uiso 1 1 calc R . .
H8C H 0.8613 0.4864 0.4577 0.119 Uiso 1 1 calc R . .
C9 C 0.8313(6) 0.2371(6) 0.4702(4) 0.095(3) Uani 1 1 d . . .
H9A H 0.7850 0.1911 0.4668 0.142 Uiso 1 1 calc R A .
H9B H 0.8560 0.2338 0.5046 0.142 Uiso 1 1 calc R . .
H9C H 0.8708 0.2170 0.4467 0.142 Uiso 1 1 calc R . .
C10 C 0.7398(5) 0.3798(8) 0.4932(3) 0.094(3) Uani 1 1 d . . .
H10A H 0.7269 0.4515 0.4870 0.141 Uiso 1 1 calc R A .
H10B H 0.7606 0.3710 0.5282 0.141 Uiso 1 1 calc R . .
H10C H 0.6911 0.3388 0.4867 0.141 Uiso 1 1 calc R . .
C11 C 0.5782(4) 0.4136(5) 0.3243(3) 0.0613(19) Uani 1 1 d . A .
H11A H 0.5625 0.3974 0.2887 0.074 Uiso 1 1 calc R . .
H11B H 0.5412 0.3772 0.3454 0.074 Uiso 1 1 calc R . .
C12 C 0.5924(4) 0.5959(5) 0.2964(3) 0.0540(17) Uani 1 1 d . A .
C13 C 0.5703(4) 0.5264(5) 0.3324(3) 0.0581(18) Uani 1 1 d . . .
C14 C 0.5424(4) 0.5653(6) 0.3756(3) 0.0628(19) Uani 1 1 d . A .
H14 H 0.5269 0.5191 0.4004 0.075 Uiso 1 1 calc R . .
C15 C 0.5356(4) 0.6697(5) 0.3850(3) 0.0601(19) Uani 1 1 d . . .
C16 C 0.5573(4) 0.7348(6) 0.3471(3) 0.0605(19) Uani 1 1 d . A .
H16 H 0.5519 0.8059 0.3519 0.073 Uiso 1 1 calc R . .
C17 C 0.5863(3) 0.7007(5) 0.3025(3) 0.0557(18) Uani 1 1 d . . .
C18 C 0.5056(5) 0.7131(6) 0.4329(3) 0.071(2) Uani 1 1 d . A .
C19 C 0.4256(5) 0.7671(8) 0.4202(3) 0.098(3) Uani 1 1 d . . .
H19A H 0.4324 0.8181 0.3942 0.147 Uiso 1 1 calc R A .
H19B H 0.4082 0.8003 0.4504 0.147 Uiso 1 1 calc R . .
H19C H 0.3850 0.7175 0.4080 0.147 Uiso 1 1 calc R . .
C20 C 0.4924(5) 0.6319(6) 0.4724(3) 0.081(2) Uani 1 1 d . . .
H20A H 0.4524 0.5828 0.4587 0.122 Uiso 1 1 calc R A .
H20B H 0.4730 0.6640 0.5023 0.122 Uiso 1 1 calc R . .
H20C H 0.5433 0.5969 0.4814 0.122 Uiso 1 1 calc R . .
C21 C 0.5702(6) 0.7864(7) 0.4562(4) 0.098(3) Uani 1 1 d . . .
H21A H 0.6210 0.7497 0.4629 0.147 Uiso 1 1 calc R A .
H21B H 0.5526 0.8138 0.4877 0.147 Uiso 1 1 calc R . .
H21C H 0.5780 0.8422 0.4328 0.147 Uiso 1 1 calc R . .
C22 C 0.6101(4) 0.7720(5) 0.2619(3) 0.0552(17) Uani 1 1 d . A .
H22A H 0.5824 0.8378 0.2654 0.066 Uiso 1 1 calc R . .
H22B H 0.5922 0.7434 0.2287 0.066 Uiso 1 1 calc R . .
C23 C 0.7505(4) 0.7432(5) 0.2319(2) 0.0486(16) Uani 1 1 d . A .
C24 C 0.7008(4) 0.7898(5) 0.2644(2) 0.0498(16) Uani 1 1 d . . .
C25 C 0.7355(4) 0.8520(5) 0.3015(3) 0.0523(16) Uani 1 1 d . A .
H25 H 0.7012 0.8845 0.3235 0.063 Uiso 1 1 calc R . .
C26 C 0.8171(4) 0.8697(5) 0.3085(3) 0.0527(17) Uani 1 1 d . . .
C27 C 0.8651(4) 0.8163(5) 0.2764(3) 0.0517(17) Uani 1 1 d . A .
H27 H 0.9217 0.8258 0.2802 0.062 Uiso 1 1 calc R . .
C28 C 0.8342(3) 0.7509(4) 0.2397(2) 0.0442(15) Uani 1 1 d . . .
C29 C 0.8553(4) 0.9438(5) 0.3479(3) 0.0621(18) Uani 1 1 d U A .
C30 C 0.9142(8) 0.8864(10) 0.3832(5) 0.087(5) Uani 0.694(15) 1 d PDU A 1
H30A H 0.8861 0.8308 0.3989 0.131 Uiso 0.694(15) 1 calc PR A 1
H30B H 0.9370 0.9326 0.4093 0.131 Uiso 0.694(15) 1 calc PR A 1
H30C H 0.9574 0.8587 0.3644 0.131 Uiso 0.694(15) 1 calc PR A 1
C31 C 0.7909(8) 0.9855(12) 0.3810(6) 0.092(5) Uani 0.694(15) 1 d PDU A 1
H31A H 0.7655 0.9290 0.3978 0.138 Uiso 0.694(15) 1 calc PR A 1
H31B H 0.7500 1.0225 0.3601 0.138 Uiso 0.694(15) 1 calc PR A 1
H31C H 0.8163 1.0315 0.4063 0.138 Uiso 0.694(15) 1 calc PR A 1
C32 C 0.8939(9) 1.0283(10) 0.3227(5) 0.078(4) Uani 0.694(15) 1 d PDU A 1
H32A H 0.9180 1.0752 0.3480 0.117 Uiso 0.694(15) 1 calc PR A 1
H32B H 0.8535 1.0642 0.3009 0.117 Uiso 0.694(15) 1 calc PR A 1
H32C H 0.9359 1.0015 0.3025 0.117 Uiso 0.694(15) 1 calc PR A 1
C30X C 0.9491(17) 0.947(3) 0.3464(13) 0.096(10) Uani 0.306(15) 1 d PDU A 2
H30D H 0.9716 0.9948 0.3718 0.145 Uiso 0.306(15) 1 calc PR A 2
H30E H 0.9630 0.9693 0.3131 0.145 Uiso 0.306(15) 1 calc PR A 2
H30F H 0.9712 0.8793 0.3534 0.145 Uiso 0.306(15) 1 calc PR A 2
C31X C 0.832(3) 0.915(4) 0.4005(13) 0.117(11) Uani 0.306(15) 1 d PDU A 2
H31D H 0.8569 0.9633 0.4251 0.175 Uiso 0.306(15) 1 calc PR A 2
H31E H 0.8511 0.8465 0.4087 0.175 Uiso 0.306(15) 1 calc PR A 2
H31F H 0.7734 0.9180 0.4014 0.175 Uiso 0.306(15) 1 calc PR A 2
C32X C 0.834(3) 1.053(2) 0.3326(16) 0.120(12) Uani 0.306(15) 1 d PDU A 2
H32D H 0.8591 1.0996 0.3575 0.180 Uiso 0.306(15) 1 calc PR A 2
H32E H 0.7755 1.0612 0.3307 0.180 Uiso 0.306(15) 1 calc PR A 2
H32F H 0.8539 1.0668 0.2996 0.180 Uiso 0.306(15) 1 calc PR A 2
C33 C 0.8923(4) 0.6855(5) 0.2131(3) 0.0518(16) Uani 1 1 d . A .
H33A H 0.8648 0.6582 0.1818 0.062 Uiso 1 1 calc R . .
H33B H 0.9381 0.7276 0.2037 0.062 Uiso 1 1 calc R . .
C34 C 0.8832(4) 0.5053(5) 0.2448(3) 0.0548(17) Uani 1 1 d . A .
C35 C 0.9233(3) 0.5992(5) 0.2457(2) 0.0499(16) Uani 1 1 d . . .
C36 C 0.9893(4) 0.6092(5) 0.2803(3) 0.0542(17) Uani 1 1 d . A .
H36 H 1.0172 0.6721 0.2819 0.065 Uiso 1 1 calc R . .
C37 C 1.0168(3) 0.5317(5) 0.3129(3) 0.0545(17) Uani 1 1 d . . .
C38 C 0.9743(4) 0.4401(5) 0.3088(3) 0.0559(18) Uani 1 1 d . A .
H38 H 0.9923 0.3857 0.3301 0.067 Uiso 1 1 calc R . .
C39 C 0.9084(4) 0.4243(5) 0.2760(3) 0.0531(17) Uani 1 1 d . . .
C40 C 1.0876(4) 0.5491(5) 0.3507(3) 0.0610(19) Uani 1 1 d . A .
C41 C 1.0738(6) 0.6453(7) 0.3808(4) 0.095(3) Uani 1 1 d . . .
H41A H 1.0702 0.7038 0.3581 0.142 Uiso 1 1 calc R A .
H41B H 1.1188 0.6550 0.4060 0.142 Uiso 1 1 calc R . .
H41C H 1.0236 0.6388 0.3974 0.142 Uiso 1 1 calc R . .
C42 C 1.1646(4) 0.5591(9) 0.3227(3) 0.100(3) Uani 1 1 d . . .
H42A H 1.1806 0.4920 0.3111 0.150 Uiso 1 1 calc R A .
H42B H 1.2078 0.5874 0.3453 0.150 Uiso 1 1 calc R . .
H42C H 1.1544 0.6042 0.2937 0.150 Uiso 1 1 calc R . .
C43 C 1.0997(5) 0.4620(7) 0.3890(3) 0.087(3) Uani 1 1 d . . .
H43A H 1.0509 0.4540 0.4070 0.131 Uiso 1 1 calc R A .
H43B H 1.1453 0.4778 0.4130 0.131 Uiso 1 1 calc R . .
H43C H 1.1106 0.3988 0.3714 0.131 Uiso 1 1 calc R . .
C44 C 0.8599(4) 0.3272(5) 0.2765(3) 0.0579(18) Uani 1 1 d . A .
H44A H 0.8962 0.2692 0.2850 0.069 Uiso 1 1 calc R . .
H44B H 0.8328 0.3149 0.2428 0.069 Uiso 1 1 calc R . .
O7 O 0.5412(3) 0.6245(4) 0.1599(2) 0.0739(14) Uani 1 1 d DU B .
C51 C 0.4624(6) 0.6257(8) 0.1346(4) 0.111(3) Uani 1 1 d DU . .
H51A H 0.4393 0.6949 0.1353 0.133 Uiso 0.78(2) 1 calc PR B 1
H51B H 0.4263 0.5788 0.1513 0.133 Uiso 0.78(2) 1 calc PR B 1
H51C H 0.4285 0.6704 0.1541 0.133 Uiso 0.22(2) 1 calc PR B 2
H51D H 0.4401 0.5563 0.1366 0.133 Uiso 0.22(2) 1 calc PR B 2
C52 C 0.4715(7) 0.5906(15) 0.0780(4) 0.124(6) Uani 0.78(2) 1 d PDU B 1
H52A H 0.5069 0.6381 0.0611 0.149 Uiso 0.78(2) 1 calc PR B 1
H52B H 0.4952 0.5218 0.0773 0.149 Uiso 0.78(2) 1 calc PR B 1
C53 C 0.3876(8) 0.5909(13) 0.0520(6) 0.181(6) Uani 1 1 d DU . .
H53A H 0.3902 0.5698 0.0170 0.271 Uiso 0.78(2) 1 calc PR B 1
H53B H 0.3650 0.6594 0.0531 0.271 Uiso 0.78(2) 1 calc PR B 1
H53C H 0.3534 0.5436 0.0691 0.271 Uiso 0.78(2) 1 calc PR B 1
H53D H 0.3896 0.5992 0.0156 0.271 Uiso 0.22(2) 1 calc PR B 2
H53E H 0.3341 0.6097 0.0618 0.271 Uiso 0.22(2) 1 calc PR B 2
H53F H 0.3986 0.5199 0.0611 0.271 Uiso 0.22(2) 1 calc PR B 2
C52X C 0.4514(18) 0.660(2) 0.0794(7) 0.090(8) Uani 0.22(2) 1 d PDU B 2
H52C H 0.5031 0.6538 0.0635 0.108 Uiso 0.22(2) 1 calc PR B 2
H52D H 0.4337 0.7312 0.0774 0.108 Uiso 0.22(2) 1 calc PR B 2
O9 O 0.8035(3) 0.5297(4) 0.1076(2) 0.0856(16) Uani 1 1 d DU . .
C54 C 0.8405(8) 0.5011(11) 0.0621(4) 0.150(5) Uani 1 1 d DU . .
H54A H 0.8402 0.4265 0.0580 0.180 Uiso 1 1 calc R . .
H54B H 0.8969 0.5254 0.0632 0.180 Uiso 1 1 calc R . .
C55 C 0.7916(13) 0.5499(17) 0.0208(6) 0.247(9) Uani 1 1 d DU . .
H55A H 0.8152 0.5363 -0.0114 0.297 Uiso 1 1 calc R . .
H55B H 0.7908 0.6243 0.0261 0.297 Uiso 1 1 calc R . .
C56 C 0.7046(14) 0.507(3) 0.0191(13) 0.42(2) Uani 1 1 d DU . .
H56A H 0.6715 0.5407 -0.0079 0.635 Uiso 1 1 calc R . .
H56B H 0.6817 0.5206 0.0513 0.635 Uiso 1 1 calc R . .
H56C H 0.7056 0.4342 0.0130 0.635 Uiso 1 1 calc R . .
N1 N 0.7645(7) 0.6731(9) 0.4413(4) 0.140(4) Uani 1 1 d D . .
C57 C 0.7795(6) 0.6447(7) 0.4019(4) 0.089(3) Uani 1 1 d D . .
C58 C 0.7960(4) 0.6076(5) 0.3553(3) 0.068(2) Uani 1 1 d D . .
H58A H 0.7609 0.5496 0.3467 0.102 Uiso 1 1 calc R . .
H58B H 0.8524 0.5860 0.3562 0.102 Uiso 1 1 calc R . .
H58C H 0.7865 0.6610 0.3300 0.102 Uiso 1 1 calc R . .
N2 N 1.0199(12) 0.2123(15) 0.4072(7) 0.126(6) Uani 0.50 1 d PDU . .
C59 C 1.056(2) 0.229(3) 0.4459(9) 0.117(9) Uani 0.327(15) 1 d PDU C 1
C60 C 1.072(2) 0.266(3) 0.4941(9) 0.123(12) Uani 0.327(15) 1 d PDU C 1
C59X C 1.064(4) 0.168(4) 0.436(2) 0.128(14) Uiso 0.173(15) 1 d PDU C 2
C60X C 1.128(3) 0.157(5) 0.471(2) 0.125(17) Uiso 0.173(15) 1 d PDU . 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0625(8) 0.0662(9) 0.0785(10) -0.0023(7) -0.0013(7) -0.0200(6)
V2 0.0709(9) 0.0539(8) 0.0981(11) -0.0163(7) -0.0109(7) 0.0011(6)
O5 0.064(3) 0.074(3) 0.075(3) -0.008(3) -0.008(3) -0.017(3)
O6 0.074(3) 0.086(4) 0.091(4) -0.002(3) -0.001(3) -0.038(3)
O8 0.119(5) 0.055(3) 0.148(6) -0.029(4) -0.020(4) 0.012(3)
O1 0.054(3) 0.044(2) 0.078(3) -0.006(2) -0.008(2) -0.006(2)
C45 0.060(9) 0.040(6) 0.095(10) 0.000(7) -0.008(8) -0.009(5)
C46 0.061(9) 0.051(6) 0.110(11) -0.013(8) 0.004(8) 0.003(5)
C47 0.063(4) 0.043(4) 0.106(6) -0.011(4) -0.004(4) -0.003(3)
O2 0.051(3) 0.056(3) 0.073(3) -0.002(2) 0.006(2) -0.009(2)
O3 0.050(2) 0.046(3) 0.065(3) -0.002(2) 0.000(2) -0.008(2)
C48 0.058(4) 0.057(4) 0.062(5) -0.002(4) 0.001(3) -0.002(3)
C49 0.059(4) 0.062(5) 0.075(5) 0.005(4) -0.002(4) 0.002(4)
C50 0.067(5) 0.094(6) 0.089(6) 0.020(5) -0.014(4) -0.002(4)
O4 0.050(3) 0.046(3) 0.091(4) -0.004(2) -0.013(2) 0.002(2)
C1 0.051(4) 0.038(4) 0.078(5) -0.007(3) -0.007(4) -0.013(3)
C2 0.050(4) 0.036(4) 0.079(5) -0.003(3) -0.007(4) -0.006(3)
C3 0.042(4) 0.038(4) 0.095(6) 0.003(4) -0.008(4) -0.003(3)
C4 0.057(4) 0.041(4) 0.075(5) 0.005(3) -0.002(4) -0.012(3)
C5 0.059(5) 0.046(4) 0.087(6) -0.004(4) 0.010(4) -0.007(3)
C6 0.048(4) 0.040(4) 0.077(5) 0.001(3) -0.003(4) -0.011(3)
C7 0.069(5) 0.064(5) 0.074(5) 0.003(4) 0.006(4) -0.011(4)
C8 0.072(5) 0.084(6) 0.080(6) -0.004(5) -0.010(4) -0.025(4)
C9 0.114(7) 0.069(6) 0.099(7) 0.007(5) -0.011(5) -0.010(5)
C10 0.076(6) 0.126(8) 0.080(6) 0.003(6) -0.001(5) -0.009(5)
C11 0.053(4) 0.051(4) 0.080(5) 0.005(4) 0.006(4) -0.017(3)
C12 0.035(3) 0.057(4) 0.070(5) 0.002(4) 0.001(3) -0.006(3)
C13 0.037(3) 0.063(5) 0.075(5) -0.002(4) 0.002(3) -0.006(3)
C14 0.042(4) 0.063(5) 0.083(5) 0.009(4) 0.003(4) -0.003(3)
C15 0.041(4) 0.058(5) 0.081(5) 0.005(4) 0.003(3) 0.004(3)
C16 0.043(4) 0.055(4) 0.083(5) 0.004(4) -0.001(4) 0.003(3)
C17 0.032(3) 0.058(5) 0.077(5) 0.007(4) 0.003(3) 0.004(3)
C18 0.072(5) 0.061(5) 0.082(6) 0.002(4) 0.016(4) 0.003(4)
C19 0.100(7) 0.106(7) 0.093(6) 0.017(5) 0.038(5) 0.048(6)
C20 0.087(6) 0.081(6) 0.077(6) 0.007(5) 0.009(4) 0.008(5)
C21 0.103(7) 0.093(7) 0.102(7) -0.022(6) 0.028(6) -0.013(5)
C22 0.042(4) 0.051(4) 0.073(5) -0.004(4) 0.004(3) 0.003(3)
C23 0.043(4) 0.039(3) 0.062(4) 0.004(3) -0.008(3) -0.002(3)
C24 0.044(4) 0.047(4) 0.058(4) 0.006(3) 0.001(3) 0.002(3)
C25 0.049(4) 0.041(4) 0.066(4) -0.003(3) 0.003(3) 0.001(3)
C26 0.055(4) 0.039(4) 0.064(4) 0.002(3) -0.002(3) -0.003(3)
C27 0.039(3) 0.051(4) 0.065(4) 0.009(3) 0.003(3) -0.003(3)
C28 0.041(3) 0.039(3) 0.052(4) 0.000(3) -0.001(3) -0.004(3)
C29 0.069(4) 0.050(4) 0.067(4) -0.014(3) -0.001(3) -0.011(3)
C30 0.098(9) 0.076(8) 0.082(9) -0.015(6) -0.027(7) -0.011(6)
C31 0.092(8) 0.095(11) 0.092(10) -0.051(8) 0.020(7) -0.025(6)
C32 0.091(10) 0.063(8) 0.080(8) -0.019(6) 0.005(7) -0.029(7)
C30X 0.072(9) 0.11(2) 0.11(2) -0.047(19) -0.001(13) -0.041(13)
C31X 0.12(2) 0.14(3) 0.089(15) 0.000(17) 0.020(17) -0.02(2)
C32X 0.17(3) 0.047(11) 0.14(3) -0.017(14) -0.04(3) -0.011(17)
C33 0.040(3) 0.053(4) 0.062(4) -0.001(3) 0.007(3) -0.003(3)
C34 0.042(4) 0.053(4) 0.068(5) -0.014(3) -0.005(3) 0.005(3)
C35 0.037(3) 0.049(4) 0.065(4) -0.008(3) 0.011(3) 0.007(3)
C36 0.038(3) 0.050(4) 0.076(5) -0.004(4) 0.011(3) 0.002(3)
C37 0.034(3) 0.053(4) 0.077(5) 0.003(4) 0.007(3) 0.004(3)
C38 0.045(4) 0.048(4) 0.076(5) 0.004(3) 0.007(3) 0.012(3)
C39 0.043(4) 0.041(4) 0.076(5) -0.011(3) 0.005(3) 0.007(3)
C40 0.047(4) 0.060(4) 0.075(5) 0.009(4) -0.004(3) -0.006(3)
C41 0.094(6) 0.075(6) 0.110(7) -0.009(5) -0.030(5) 0.009(5)
C42 0.041(4) 0.162(10) 0.096(7) 0.010(6) -0.004(4) -0.017(5)
C43 0.071(5) 0.081(6) 0.105(7) 0.017(5) -0.024(5) -0.004(4)
C44 0.048(4) 0.045(4) 0.080(5) -0.008(3) -0.003(4) 0.005(3)
O7 0.061(3) 0.069(3) 0.090(4) 0.004(3) -0.007(3) -0.011(2)
C51 0.089(6) 0.102(7) 0.135(7) 0.025(6) -0.033(6) -0.018(5)
C52 0.101(8) 0.168(14) 0.096(6) 0.071(8) -0.040(7) -0.030(9)
C53 0.155(10) 0.212(14) 0.165(10) 0.025(11) -0.062(9) -0.035(10)
C52X 0.065(16) 0.086(18) 0.116(13) 0.014(15) -0.017(12) 0.049(13)
O9 0.075(3) 0.085(4) 0.098(4) -0.022(3) 0.016(3) -0.006(3)
C54 0.155(10) 0.165(11) 0.134(9) -0.069(9) 0.040(7) 0.009(9)
C55 0.275(19) 0.34(2) 0.123(8) -0.039(14) 0.019(13) 0.053(18)
C56 0.25(2) 0.58(5) 0.41(4) 0.07(4) -0.12(3) 0.03(3)
N1 0.153(9) 0.142(9) 0.128(8) -0.009(7) 0.025(7) 0.039(7)
C57 0.080(6) 0.077(6) 0.111(8) 0.007(6) 0.012(6) 0.007(5)
C58 0.067(5) 0.047(4) 0.090(6) 0.007(4) 0.006(4) 0.001(3)
N2 0.132(14) 0.121(13) 0.124(12) -0.002(11) -0.002(11) 0.014(11)
C59 0.146(18) 0.117(18) 0.093(14) -0.005(15) 0.037(13) -0.054(16)
C60 0.13(3) 0.14(3) 0.097(17) 0.010(18) -0.014(18) 0.02(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
V1 O6 1.587(5) . ?
V1 O7 1.746(5) . ?
V1 O2 1.760(5) . ?
V1 O5 1.778(5) . ?
V2 O8 1.576(6) . ?
V2 O9 1.738(6) . ?
V2 O4 1.753(5) . ?
V2 O5 1.766(5) . ?
O1 C1 1.393(8) . ?
O1 C45 1.466(10) . ?
O1 C45X 1.497(12) . ?
C45 C46 1.498(13) . ?
C46 C47 1.552(12) . ?
C47 C46X 1.536(12) . ?
C45X C46X 1.487(14) . ?
O2 C12 1.381(8) . ?
O3 C23 1.404(7) . ?
O3 C48 1.455(7) . ?
C48 C49 1.499(8) . ?
C49 C50 1.531(9) . ?
O4 C34 1.366(7) . ?
C1 C6 1.375(10) . ?
C1 C2 1.410(9) . ?
C2 C3 1.378(10) . ?
C2 C44 1.518(10) . ?
C3 C4 1.387(10) . ?
C4 C5 1.379(10) . ?
C4 C7 1.537(10) . ?
C5 C6 1.401(10) . ?
C6 C11 1.510(9) . ?
C7 C10 1.519(11) . ?
C7 C9 1.534(11) . ?
C7 C8 1.549(10) . ?
C11 C13 1.510(10) . ?
C12 C17 1.394(9) . ?
C12 C13 1.397(10) . ?
C13 C14 1.374(10) . ?
C14 C15 1.404(10) . ?
C15 C16 1.395(10) . ?
C15 C18 1.520(11) . ?
C16 C17 1.393(10) . ?
C17 C22 1.509(9) . ?
C18 C19 1.526(11) . ?
C18 C20 1.530(11) . ?
C18 C21 1.544(11) . ?
C22 C24 1.527(8) . ?
C23 C24 1.385(9) . ?
C23 C28 1.400(8) . ?
C24 C25 1.381(9) . ?
C25 C26 1.379(9) . ?
C26 C27 1.402(9) . ?
C26 C29 1.539(9) . ?
C27 C28 1.377(9) . ?
C28 C33 1.512(9) . ?
C29 C32 1.472(14) . ?
C29 C30 1.513(14) . ?
C29 C32X 1.53(3) . ?
C29 C31X 1.53(3) . ?
C29 C31 1.542(14) . ?
C29 C30X 1.57(3) . ?
C33 C35 1.501(9) . ?
C34 C39 1.400(9) . ?
C34 C35 1.406(9) . ?
C35 C36 1.390(9) . ?
C36 C37 1.397(9) . ?
C37 C38 1.399(9) . ?
C37 C40 1.514(9) . ?
C38 C39 1.371(9) . ?
C39 C44 1.515(9) . ?
C40 C41 1.527(11) . ?
C40 C42 1.538(10) . ?
C40 C43 1.541(10) . ?
O7 C51 1.433(10) . ?
C51 C52X 1.539(15) . ?
C51 C52 1.601(12) . ?
C52 C53 1.515(12) . ?
C53 C52X 1.540(15) . ?
O9 C54 1.452(10) . ?
C54 C55 1.471(12) . ?
C55 C56 1.552(13) . ?
C55 C60X 1.95(6) 2_755 ?
N1 C57 1.161(12) . ?
C57 C58 1.384(13) . ?
N2 C59 1.175(14) . ?
N2 C59X 1.176(15) . ?
C59 C60 1.386(16) . ?
C59X C60X 1.383(16) . ?
C60X C55 1.95(6) 2_745 ?

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
O6 V1 O7 102.6(3) . . ?
O6 V1 O2 108.4(3) . . ?
O7 V1 O2 111.3(2) . . ?
O6 V1 O5 107.7(3) . . ?
O7 V1 O5 109.7(3) . . ?
O2 V1 O5 116.2(2) . . ?
O8 V2 O9 105.8(3) . . ?
O8 V2 O4 111.7(3) . . ?
O9 V2 O4 108.6(2) . . ?
O8 V2 O5 109.4(3) . . ?
O9 V2 O5 109.8(3) . . ?
O4 V2 O5 111.4(2) . . ?
V2 O5 V1 138.7(3) . . ?
C1 O1 C45 113.6(8) . . ?
C1 O1 C45X 114.3(8) . . ?
C45 O1 C45X 35.4(7) . . ?
O1 C45 C46 110.5(9) . . ?
C45 C46 C47 109.4(9) . . ?
C46X C47 C46 39.3(7) . . ?
C46X C45X O1 111.2(10) . . ?
C45X C46X C47 108.1(10) . . ?
C12 O2 V1 137.0(4) . . ?
C23 O3 C48 113.5(5) . . ?
O3 C48 C49 113.8(5) . . ?
C48 C49 C50 110.5(6) . . ?
C34 O4 V2 151.0(4) . . ?
C6 C1 O1 120.1(6) . . ?
C6 C1 C2 120.8(7) . . ?
O1 C1 C2 119.1(7) . . ?
C3 C2 C1 117.4(7) . . ?
C3 C2 C44 119.9(6) . . ?
C1 C2 C44 122.6(7) . . ?
C2 C3 C4 124.1(6) . . ?
C5 C4 C3 116.0(7) . . ?
C5 C4 C7 123.8(7) . . ?
C3 C4 C7 120.1(6) . . ?
C4 C5 C6 123.0(7) . . ?
C1 C6 C5 118.5(6) . . ?
C1 C6 C11 122.7(7) . . ?
C5 C6 C11 118.6(7) . . ?
C10 C7 C9 111.6(7) . . ?
C10 C7 C4 111.1(6) . . ?
C9 C7 C4 108.3(6) . . ?
C10 C7 C8 108.3(7) . . ?
C9 C7 C8 107.9(7) . . ?
C4 C7 C8 109.7(6) . . ?
C13 C11 C6 111.4(5) . . ?
O2 C12 C17 116.6(6) . . ?
O2 C12 C13 120.3(6) . . ?
C17 C12 C13 123.0(7) . . ?
C14 C13 C12 117.1(7) . . ?
C14 C13 C11 121.8(7) . . ?
C12 C13 C11 121.1(7) . . ?
C13 C14 C15 123.5(7) . . ?
C16 C15 C14 116.4(7) . . ?
C16 C15 C18 119.9(7) . . ?
C14 C15 C18 123.7(7) . . ?
C17 C16 C15 123.1(7) . . ?
C16 C17 C12 116.8(7) . . ?
C16 C17 C22 122.6(6) . . ?
C12 C17 C22 120.6(6) . . ?
C15 C18 C19 109.0(7) . . ?
C15 C18 C20 113.0(6) . . ?
C19 C18 C20 108.1(7) . . ?
C15 C18 C21 108.2(6) . . ?
C19 C18 C21 111.7(8) . . ?
C20 C18 C21 106.9(7) . . ?
C17 C22 C24 112.1(5) . . ?
C24 C23 C28 120.6(6) . . ?
C24 C23 O3 119.9(5) . . ?
C28 C23 O3 119.5(6) . . ?
C25 C24 C23 118.4(6) . . ?
C25 C24 C22 118.9(6) . . ?
C23 C24 C22 122.7(6) . . ?
C26 C25 C24 123.7(6) . . ?
C25 C26 C27 115.7(6) . . ?
C25 C26 C29 123.6(6) . . ?
C27 C26 C29 120.7(6) . . ?
C28 C27 C26 123.3(6) . . ?
C27 C28 C23 117.9(6) . . ?
C27 C28 C33 118.3(5) . . ?
C23 C28 C33 123.7(5) . . ?
C32 C29 C30 112.2(9) . . ?
C32 C29 C32X 42.9(19) . . ?
C30 C29 C32X 139.9(15) . . ?
C32 C29 C31X 138.8(17) . . ?
C30 C29 C31X 60.0(18) . . ?
C32X C29 C31X 114(3) . . ?
C32 C29 C26 109.9(7) . . ?
C30 C29 C26 109.0(7) . . ?
C32X C29 C26 109.7(14) . . ?
C31X C29 C26 110.6(16) . . ?
C32 C29 C31 109.8(9) . . ?
C30 C29 C31 105.4(10) . . ?
C32X C29 C31 70(2) . . ?
C31X C29 C31 47.7(17) . . ?
C26 C29 C31 110.4(7) . . ?
C32 C29 C30X 59.9(15) . . ?
C30 C29 C30X 55.1(15) . . ?
C32X C29 C30X 100(2) . . ?
C31X C29 C30X 110(2) . . ?
C26 C29 C30X 111.3(11) . . ?
C31 C29 C30X 137.9(12) . . ?
C35 C33 C28 111.4(5) . . ?
O4 C34 C39 120.3(6) . . ?
O4 C34 C35 117.1(6) . . ?
C39 C34 C35 122.6(6) . . ?
C36 C35 C34 116.5(6) . . ?
C36 C35 C33 122.4(6) . . ?
C34 C35 C33 120.9(6) . . ?
C35 C36 C37 123.5(6) . . ?
C36 C37 C38 116.2(6) . . ?
C36 C37 C40 120.6(6) . . ?
C38 C37 C40 123.1(6) . . ?
C39 C38 C37 123.9(6) . . ?
C38 C39 C34 117.2(6) . . ?
C38 C39 C44 121.7(6) . . ?
C34 C39 C44 120.9(6) . . ?
C37 C40 C41 109.7(6) . . ?
C37 C40 C42 108.9(6) . . ?
C41 C40 C42 110.4(7) . . ?
C37 C40 C43 112.9(6) . . ?
C41 C40 C43 106.7(7) . . ?
C42 C40 C43 108.3(7) . . ?
C39 C44 C2 109.7(5) . . ?
C51 O7 V1 128.5(5) . . ?
O7 C51 C52X 119.6(12) . . ?
O7 C51 C52 107.1(8) . . ?
C52X C51 C52 35.9(12) . . ?
C53 C52 C51 106.5(11) . . ?
C52 C53 C52X 37.0(12) . . ?
C51 C52X C53 108.3(13) . . ?
C54 O9 V2 131.3(7) . . ?
O9 C54 C55 105.5(10) . . ?
C54 C55 C56 109.2(16) . . ?
C54 C55 C60X 84(2) . 2_755 ?
C56 C55 C60X 154(3) . 2_755 ?
N1 C57 C58 178.0(12) . . ?
C59 N2 C59X 43(3) . . ?
N2 C59 C60 159(4) . . ?
N2 C59X C60X 156(4) . . ?
C59X C60X C55 129(5) . 2_745 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 V2 O5 V1 134.2(5) . . . . ?
O9 V2 O5 V1 -110.2(5) . . . . ?
O4 V2 O5 V1 10.2(5) . . . . ?
O6 V1 O5 V2 -135.6(5) . . . . ?
O7 V1 O5 V2 113.5(5) . . . . ?
O2 V1 O5 V2 -13.8(6) . . . . ?
C1 O1 C45 C46 -66.5(15) . . . . ?
C45X O1 C45 C46 32.7(13) . . . . ?
O1 C45 C46 C47 -178.6(11) . . . . ?
C45 C46 C47 C46X -31.0(12) . . . . ?
C1 O1 C45X C46X 66.2(14) . . . . ?
C45 O1 C45X C46X -30.8(13) . . . . ?
O1 C45X C46X C47 -178.0(10) . . . . ?
C46 C47 C46X C45X 32.9(13) . . . . ?
O6 V1 O2 C12 -49.0(7) . . . . ?
O7 V1 O2 C12 63.1(6) . . . . ?
O5 V1 O2 C12 -170.5(6) . . . . ?
C23 O3 C48 C49 -68.1(7) . . . . ?
O3 C48 C49 C50 -177.5(6) . . . . ?
O8 V2 O4 C34 48.7(10) . . . . ?
O9 V2 O4 C34 -67.6(10) . . . . ?
O5 V2 O4 C34 171.3(9) . . . . ?
C45 O1 C1 C6 -71.5(9) . . . . ?
C45X O1 C1 C6 -110.3(9) . . . . ?
C45 O1 C1 C2 109.7(8) . . . . ?
C45X O1 C1 C2 70.8(9) . . . . ?
C6 C1 C2 C3 5.5(9) . . . . ?
O1 C1 C2 C3 -175.6(5) . . . . ?
C6 C1 C2 C44 -169.7(6) . . . . ?
O1 C1 C2 C44 9.2(9) . . . . ?
C1 C2 C3 C4 -3.1(9) . . . . ?
C44 C2 C3 C4 172.2(6) . . . . ?
C2 C3 C4 C5 -0.9(9) . . . . ?
C2 C3 C4 C7 -179.3(6) . . . . ?
C3 C4 C5 C6 2.6(9) . . . . ?
C7 C4 C5 C6 -179.0(6) . . . . ?
O1 C1 C6 C5 177.2(5) . . . . ?
C2 C1 C6 C5 -4.0(9) . . . . ?
O1 C1 C6 C11 -7.9(9) . . . . ?
C2 C1 C6 C11 170.9(6) . . . . ?
C4 C5 C6 C1 -0.2(10) . . . . ?
C4 C5 C6 C11 -175.4(6) . . . . ?
C5 C4 C7 C10 -4.4(10) . . . . ?
C3 C4 C7 C10 173.9(7) . . . . ?
C5 C4 C7 C9 118.5(8) . . . . ?
C3 C4 C7 C9 -63.3(8) . . . . ?
C5 C4 C7 C8 -124.1(7) . . . . ?
C3 C4 C7 C8 54.2(9) . . . . ?
C1 C6 C11 C13 -103.7(8) . . . . ?
C5 C6 C11 C13 71.2(8) . . . . ?
V1 O2 C12 C17 -93.4(7) . . . . ?
V1 O2 C12 C13 89.4(8) . . . . ?
O2 C12 C13 C14 176.1(5) . . . . ?
C17 C12 C13 C14 -0.9(9) . . . . ?
O2 C12 C13 C11 -2.8(9) . . . . ?
C17 C12 C13 C11 -179.8(6) . . . . ?
C6 C11 C13 C14 -97.3(8) . . . . ?
C6 C11 C13 C12 81.6(8) . . . . ?
C12 C13 C14 C15 -0.2(10) . . . . ?
C11 C13 C14 C15 178.7(6) . . . . ?
C13 C14 C15 C16 1.4(10) . . . . ?
C13 C14 C15 C18 -179.4(6) . . . . ?
C14 C15 C16 C17 -1.7(10) . . . . ?
C18 C15 C16 C17 179.1(6) . . . . ?
C15 C16 C17 C12 0.7(9) . . . . ?
C15 C16 C17 C22 -179.6(6) . . . . ?
O2 C12 C17 C16 -176.5(5) . . . . ?
C13 C12 C17 C16 0.6(9) . . . . ?
O2 C12 C17 C22 3.8(9) . . . . ?
C13 C12 C17 C22 -179.1(6) . . . . ?
C16 C15 C18 C19 65.4(9) . . . . ?
C14 C15 C18 C19 -113.8(8) . . . . ?
C16 C15 C18 C20 -174.4(6) . . . . ?
C14 C15 C18 C20 6.4(10) . . . . ?
C16 C15 C18 C21 -56.2(9) . . . . ?
C14 C15 C18 C21 124.6(8) . . . . ?
C16 C17 C22 C24 98.6(7) . . . . ?
C12 C17 C22 C24 -81.7(8) . . . . ?
C48 O3 C23 C24 102.6(6) . . . . ?
C48 O3 C23 C28 -77.9(7) . . . . ?
C28 C23 C24 C25 6.3(9) . . . . ?
O3 C23 C24 C25 -174.2(5) . . . . ?
C28 C23 C24 C22 -171.4(6) . . . . ?
O3 C23 C24 C22 8.1(9) . . . . ?
C17 C22 C24 C25 -75.1(8) . . . . ?
C17 C22 C24 C23 102.6(7) . . . . ?
C23 C24 C25 C26 -0.7(10) . . . . ?
C22 C24 C25 C26 177.1(6) . . . . ?
C24 C25 C26 C27 -2.7(10) . . . . ?
C24 C25 C26 C29 176.3(6) . . . . ?
C25 C26 C27 C28 0.7(9) . . . . ?
C29 C26 C27 C28 -178.4(6) . . . . ?
C26 C27 C28 C23 4.6(9) . . . . ?
C26 C27 C28 C33 -170.5(6) . . . . ?
C24 C23 C28 C27 -8.1(9) . . . . ?
O3 C23 C28 C27 172.4(5) . . . . ?
C24 C23 C28 C33 166.7(6) . . . . ?
O3 C23 C28 C33 -12.8(9) . . . . ?
C25 C26 C29 C32 -115.5(10) . . . . ?
C27 C26 C29 C32 63.4(10) . . . . ?
C25 C26 C29 C30 121.1(9) . . . . ?
C27 C26 C29 C30 -59.9(10) . . . . ?
C25 C26 C29 C32X -70(2) . . . . ?
C27 C26 C29 C32X 109(2) . . . . ?
C25 C26 C29 C31X 57(2) . . . . ?
C27 C26 C29 C31X -124(2) . . . . ?
C25 C26 C29 C31 5.8(12) . . . . ?
C27 C26 C29 C31 -175.3(9) . . . . ?
C25 C26 C29 C30X -179.9(17) . . . . ?
C27 C26 C29 C30X -1.0(18) . . . . ?
C27 C28 C33 C35 75.5(7) . . . . ?
C23 C28 C33 C35 -99.4(7) . . . . ?
V2 O4 C34 C39 -83.1(11) . . . . ?
V2 O4 C34 C35 98.5(9) . . . . ?
O4 C34 C35 C36 176.8(6) . . . . ?
C39 C34 C35 C36 -1.5(9) . . . . ?
O4 C34 C35 C33 0.9(9) . . . . ?
C39 C34 C35 C33 -177.5(6) . . . . ?
C28 C33 C35 C36 -85.6(7) . . . . ?
C28 C33 C35 C34 90.1(7) . . . . ?
C34 C35 C36 C37 0.6(9) . . . . ?
C33 C35 C36 C37 176.5(6) . . . . ?
C35 C36 C37 C38 0.6(10) . . . . ?
C35 C36 C37 C40 -178.1(6) . . . . ?
C36 C37 C38 C39 -1.1(10) . . . . ?
C40 C37 C38 C39 177.6(6) . . . . ?
C37 C38 C39 C34 0.3(10) . . . . ?
C37 C38 C39 C44 -174.2(6) . . . . ?
O4 C34 C39 C38 -177.2(6) . . . . ?
C35 C34 C39 C38 1.1(10) . . . . ?
O4 C34 C39 C44 -2.7(10) . . . . ?
C35 C34 C39 C44 175.6(6) . . . . ?
C36 C37 C40 C41 51.3(9) . . . . ?
C38 C37 C40 C41 -127.3(8) . . . . ?
C36 C37 C40 C42 -69.6(9) . . . . ?
C38 C37 C40 C42 111.8(8) . . . . ?
C36 C37 C40 C43 170.1(7) . . . . ?
C38 C37 C40 C43 -8.5(10) . . . . ?
C38 C39 C44 C2 85.4(7) . . . . ?
C34 C39 C44 C2 -88.8(8) . . . . ?
C3 C2 C44 C39 -72.6(8) . . . . ?
C1 C2 C44 C39 102.5(7) . . . . ?
O6 V1 O7 C51 -11.3(8) . . . . ?
O2 V1 O7 C51 -127.0(7) . . . . ?
O5 V1 O7 C51 103.0(7) . . . . ?
V1 O7 C51 C52X -126.9(15) . . . . ?
V1 O7 C51 C52 -90.0(10) . . . . ?
O7 C51 C52 C53 179.2(11) . . . . ?
C52X C51 C52 C53 -63.5(14) . . . . ?
C51 C52 C53 C52X 60.7(13) . . . . ?
O7 C51 C52X C53 140.7(17) . . . . ?
C52 C51 C52X C53 62.8(14) . . . . ?
C52 C53 C52X C51 -66.3(14) . . . . ?
O8 V2 O9 C54 4.4(9) . . . . ?
O4 V2 O9 C54 124.5(8) . . . . ?
O5 V2 O9 C54 -113.5(8) . . . . ?
V2 O9 C54 C55 125.1(13) . . . . ?
O9 C54 C55 C56 -62(2) . . . . ?
O9 C54 C55 C60X 95(2) . . . 2_755 ?
C59X N2 C59 C60 -141(14) . . . . ?
C59 N2 C59X C60X -31(16) . . . . ?
N2 C59X C60X C55 -142(17) . . . 2_745 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        22.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.092


data_VI
_database_code_depnum_ccdc_archive 'CCDC 835506'
#TrackingRef '- Vanadyl-calixarenes.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H60 O15 S4 V, 2.25(C2 H3 N)'
_chemical_formula_sum            'C50.50 H66.75 N2.25 O15 S4 V'
_chemical_formula_weight         1124.49

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   25.0873(10)
_cell_length_b                   16.7913(7)
_cell_length_c                   26.7582(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11271.8(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    24353
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.19

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4740
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'

_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 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            112279
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         28.32
_reflns_number_total             14036
_reflns_number_gt                11231
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_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 and local programs'

_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^)+(0.0821P)^2^+9.8582P] 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         14036
_refine_ls_number_parameters     733
_refine_ls_number_restraints     254
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1483
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.668720(15) 0.62466(2) 0.189678(14) 0.02398(10) Uani 1 1 d . B .
O13 O 0.63382(7) 0.57650(10) 0.22853(6) 0.0312(4) Uani 1 1 d . . .
O1 O 0.65171(6) 0.56258(9) 0.13123(5) 0.0237(3) Uani 1 1 d . . .
O2 O 0.73386(6) 0.56171(9) 0.19472(6) 0.0258(3) Uani 1 1 d . . .
O3 O 0.72443(6) 0.32487(10) 0.17843(6) 0.0291(3) Uani 1 1 d . . .
H3 H 0.7129 0.2792 0.1717 0.044 Uiso 1 1 calc R . .
O4 O 0.57285(8) 0.43560(10) 0.18417(6) 0.0330(4) Uani 1 1 d . . .
H4 H 0.5662 0.4839 0.1789 0.049 Uiso 1 1 calc R . .
C1 C 0.64671(8) 0.58530(12) 0.08411(8) 0.0223(4) Uani 1 1 d . . .
C2 C 0.59967(8) 0.57190(12) 0.05667(8) 0.0234(4) Uani 1 1 d . . .
C3 C 0.59649(9) 0.58849(14) 0.00550(8) 0.0277(4) Uani 1 1 d . . .
H3A H 0.5643 0.5772 -0.0119 0.033 Uiso 1 1 calc R . .
C4 C 0.63915(10) 0.62107(15) -0.02057(8) 0.0310(5) Uani 1 1 d . A .
C5 C 0.68578(9) 0.63718(13) 0.00651(8) 0.0279(4) Uani 1 1 d . . .
H5 H 0.7156 0.6600 -0.0100 0.033 Uiso 1 1 calc R . .
C6 C 0.68887(9) 0.62006(12) 0.05729(8) 0.0239(4) Uani 1 1 d . . .
C7 C 0.63574(12) 0.6400(2) -0.07669(9) 0.0449(7) Uani 1 1 d DU . .
C8 C 0.5836(3) 0.6135(5) -0.09964(19) 0.074(3) Uani 0.615(8) 1 d PDU A 1
H8A H 0.5539 0.6345 -0.0798 0.111 Uiso 0.615(8) 1 calc PR A 1
H8B H 0.5820 0.5552 -0.1000 0.111 Uiso 0.615(8) 1 calc PR A 1
H8C H 0.5811 0.6337 -0.1339 0.111 Uiso 0.615(8) 1 calc PR A 1
C9 C 0.6353(3) 0.7348(3) -0.08172(17) 0.0521(15) Uani 0.615(8) 1 d PDU A 1
H9A H 0.6040 0.7564 -0.0645 0.078 Uiso 0.615(8) 1 calc PR A 1
H9B H 0.6340 0.7496 -0.1171 0.078 Uiso 0.615(8) 1 calc PR A 1
H9C H 0.6678 0.7567 -0.0666 0.078 Uiso 0.615(8) 1 calc PR A 1
C10 C 0.6836(3) 0.6094(5) -0.10356(19) 0.066(2) Uani 0.615(8) 1 d PDU A 1
H10A H 0.7159 0.6279 -0.0866 0.099 Uiso 0.615(8) 1 calc PR A 1
H10B H 0.6834 0.6292 -0.1380 0.099 Uiso 0.615(8) 1 calc PR A 1
H10C H 0.6829 0.5511 -0.1038 0.099 Uiso 0.615(8) 1 calc PR A 1
C8X C 0.6262(6) 0.5569(7) -0.1029(3) 0.086(4) Uani 0.385(8) 1 d PDU A 2
H8D H 0.6564 0.5216 -0.0961 0.130 Uiso 0.385(8) 1 calc PR A 2
H8E H 0.6228 0.5647 -0.1391 0.130 Uiso 0.385(8) 1 calc PR A 2
H8F H 0.5934 0.5328 -0.0899 0.130 Uiso 0.385(8) 1 calc PR A 2
C9X C 0.6872(5) 0.6718(10) -0.0986(3) 0.081(4) Uani 0.385(8) 1 d PDU A 2
H9D H 0.7159 0.6331 -0.0930 0.121 Uiso 0.385(8) 1 calc PR A 2
H9E H 0.6964 0.7223 -0.0823 0.121 Uiso 0.385(8) 1 calc PR A 2
H9F H 0.6827 0.6805 -0.1345 0.121 Uiso 0.385(8) 1 calc PR A 2
C10X C 0.5908(5) 0.6953(10) -0.0858(4) 0.103(6) Uani 0.385(8) 1 d PDU A 2
H10D H 0.5886 0.7073 -0.1216 0.155 Uiso 0.385(8) 1 calc PR A 2
H10E H 0.5966 0.7447 -0.0671 0.155 Uiso 0.385(8) 1 calc PR A 2
H10F H 0.5575 0.6705 -0.0748 0.155 Uiso 0.385(8) 1 calc PR A 2
S1 S 0.74643(2) 0.64665(3) 0.09099(2) 0.02354(12) Uani 1 1 d . . .
O5 O 0.72804(6) 0.69142(9) 0.13443(6) 0.0276(3) Uani 1 1 d . . .
O6 O 0.78222(7) 0.68631(10) 0.05724(6) 0.0315(4) Uani 1 1 d . . .
C11 C 0.76772(8) 0.53234(12) 0.16248(8) 0.0228(4) Uani 1 1 d . . .
C12 C 0.77698(8) 0.55964(12) 0.11318(8) 0.0225(4) Uani 1 1 d . . .
C13 C 0.81284(9) 0.52150(12) 0.08090(8) 0.0238(4) Uani 1 1 d . . .
H13 H 0.8179 0.5423 0.0482 0.029 Uiso 1 1 calc R . .
C14 C 0.84126(9) 0.45424(13) 0.09515(8) 0.0249(4) Uani 1 1 d . . .
C15 C 0.83301(8) 0.42702(13) 0.14402(8) 0.0247(4) Uani 1 1 d . . .
H15 H 0.8516 0.3811 0.1552 0.030 Uiso 1 1 calc R . .
C16 C 0.79853(8) 0.46518(12) 0.17648(8) 0.0233(4) Uani 1 1 d . . .
C17 C 0.88077(9) 0.41075(14) 0.06124(9) 0.0288(5) Uani 1 1 d . . .
C18 C 0.88111(11) 0.44430(16) 0.00803(10) 0.0379(6) Uani 1 1 d . . .
H18A H 0.8450 0.4423 -0.0058 0.057 Uiso 1 1 calc R . .
H18B H 0.9050 0.4124 -0.0129 0.057 Uiso 1 1 calc R . .
H18C H 0.8935 0.4996 0.0087 0.057 Uiso 1 1 calc R . .
C19 C 0.93681(10) 0.41993(18) 0.08355(11) 0.0420(6) Uani 1 1 d . . .
H19A H 0.9464 0.4765 0.0847 0.063 Uiso 1 1 calc R . .
H19B H 0.9626 0.3912 0.0627 0.063 Uiso 1 1 calc R . .
H19C H 0.9373 0.3980 0.1175 0.063 Uiso 1 1 calc R . .
C20 C 0.86568(11) 0.32206(14) 0.05843(10) 0.0371(6) Uani 1 1 d . . .
H20A H 0.8648 0.2996 0.0922 0.056 Uiso 1 1 calc R . .
H20B H 0.8922 0.2935 0.0383 0.056 Uiso 1 1 calc R . .
H20C H 0.8305 0.3166 0.0430 0.056 Uiso 1 1 calc R . .
S2 S 0.79337(2) 0.42925(3) 0.238297(19) 0.02370(12) Uani 1 1 d . . .
O7 O 0.80930(7) 0.49061(10) 0.27269(6) 0.0308(3) Uani 1 1 d . . .
O8 O 0.82204(6) 0.35426(10) 0.24068(6) 0.0293(3) Uani 1 1 d . . .
C21 C 0.69857(9) 0.35374(12) 0.21900(8) 0.0237(4) Uani 1 1 d . . .
C22 C 0.72546(9) 0.40842(13) 0.24952(8) 0.0240(4) Uani 1 1 d . . .
C23 C 0.70189(10) 0.44006(14) 0.29178(8) 0.0294(5) Uani 1 1 d . . .
H23 H 0.7212 0.4773 0.3115 0.035 Uiso 1 1 calc R . .
C24 C 0.65029(10) 0.41847(16) 0.30617(9) 0.0334(5) Uani 1 1 d . . .
C25 C 0.62330(10) 0.36580(15) 0.27549(9) 0.0315(5) Uani 1 1 d . . .
H25 H 0.5879 0.3506 0.2840 0.038 Uiso 1 1 calc R . .
C26 C 0.64647(9) 0.33452(13) 0.23269(8) 0.0263(4) Uani 1 1 d . . .
C27 C 0.62718(13) 0.4510(2) 0.35493(10) 0.0470(7) Uani 1 1 d . . .
C28 C 0.6269(3) 0.5418(2) 0.35331(17) 0.106(2) Uani 1 1 d . . .
H28A H 0.6632 0.5612 0.3479 0.160 Uiso 1 1 calc R . .
H28B H 0.6133 0.5625 0.3851 0.160 Uiso 1 1 calc R . .
H28C H 0.6039 0.5598 0.3259 0.160 Uiso 1 1 calc R . .
C29 C 0.66439(14) 0.4259(2) 0.39853(11) 0.0594(9) Uani 1 1 d . . .
H29A H 0.6718 0.3687 0.3963 0.089 Uiso 1 1 calc R . .
H29B H 0.6470 0.4375 0.4305 0.089 Uiso 1 1 calc R . .
H29C H 0.6979 0.4556 0.3964 0.089 Uiso 1 1 calc R . .
C30 C 0.57258(14) 0.4147(3) 0.36590(13) 0.0699(11) Uani 1 1 d . . .
H30A H 0.5474 0.4303 0.3397 0.105 Uiso 1 1 calc R . .
H30B H 0.5597 0.4339 0.3983 0.105 Uiso 1 1 calc R . .
H30C H 0.5756 0.3565 0.3667 0.105 Uiso 1 1 calc R . .
S3 S 0.60992(2) 0.26656(3) 0.19612(2) 0.02903(13) Uani 1 1 d . . .
O9 O 0.64630(7) 0.20416(10) 0.18083(7) 0.0353(4) Uani 1 1 d . . .
O10 O 0.56291(7) 0.24498(12) 0.22334(7) 0.0420(4) Uani 1 1 d . . .
C31 C 0.57448(9) 0.39650(13) 0.14061(8) 0.0253(4) Uani 1 1 d . . .
C32 C 0.59094(9) 0.31667(13) 0.14049(8) 0.0264(4) Uani 1 1 d . . .
C33 C 0.59036(9) 0.27082(14) 0.09693(9) 0.0301(5) Uani 1 1 d . . .
H33 H 0.6020 0.2170 0.0984 0.036 Uiso 1 1 calc R . .
C34 C 0.57321(9) 0.30179(14) 0.05160(9) 0.0295(5) Uani 1 1 d . . .
C35 C 0.55920(9) 0.38213(13) 0.05070(9) 0.0278(4) Uani 1 1 d . . .
H35 H 0.5488 0.4057 0.0199 0.033 Uiso 1 1 calc R . .
C36 C 0.56014(8) 0.42859(13) 0.09382(8) 0.0241(4) Uani 1 1 d . . .
C37 C 0.57062(10) 0.25284(15) 0.00330(10) 0.0366(6) Uani 1 1 d . . .
C38 C 0.58168(16) 0.16545(19) 0.01286(13) 0.0636(10) Uani 1 1 d . . .
H38A H 0.5552 0.1444 0.0363 0.095 Uiso 1 1 calc R . .
H38B H 0.6174 0.1594 0.0272 0.095 Uiso 1 1 calc R . .
H38C H 0.5796 0.1360 -0.0187 0.095 Uiso 1 1 calc R . .
C39 C 0.51577(12) 0.26128(18) -0.02045(12) 0.0506(8) Uani 1 1 d . . .
H39A H 0.5147 0.2312 -0.0518 0.076 Uiso 1 1 calc R . .
H39B H 0.5086 0.3176 -0.0273 0.076 Uiso 1 1 calc R . .
H39C H 0.4887 0.2405 0.0025 0.076 Uiso 1 1 calc R . .
C40 C 0.61214(17) 0.2860(3) -0.03416(14) 0.0715(11) Uani 1 1 d . . .
H40A H 0.6478 0.2829 -0.0194 0.107 Uiso 1 1 calc R . .
H40B H 0.6037 0.3417 -0.0419 0.107 Uiso 1 1 calc R . .
H40C H 0.6112 0.2545 -0.0650 0.107 Uiso 1 1 calc R . .
S4 S 0.54348(2) 0.52996(3) 0.086476(19) 0.02341(12) Uani 1 1 d . . .
O11 O 0.53687(6) 0.56431(9) 0.13571(6) 0.0278(3) Uani 1 1 d . . .
O12 O 0.49946(6) 0.53517(10) 0.05231(6) 0.0303(3) Uani 1 1 d . . .
O14 O 0.62722(7) 0.70672(10) 0.17420(6) 0.0327(4) Uani 1 1 d DU B .
C41 C 0.57405(11) 0.73159(17) 0.18183(11) 0.0421(6) Uani 1 1 d DU . .
H41A H 0.5524 0.7134 0.1531 0.063 Uiso 0.671(7) 1 calc PR B 1
H41B H 0.5733 0.7905 0.1819 0.063 Uiso 0.671(7) 1 calc PR B 1
H41C H 0.5527 0.6825 0.1859 0.063 Uiso 0.329(7) 1 calc PR B 2
H41D H 0.5623 0.7564 0.1501 0.063 Uiso 0.329(7) 1 calc PR B 2
C42 C 0.54911(16) 0.7036(3) 0.22711(15) 0.0411(11) Uani 0.671(7) 1 d PDU B 1
H42A H 0.5535 0.6450 0.2288 0.049 Uiso 0.671(7) 1 calc PR B 1
H42B H 0.5104 0.7147 0.2249 0.049 Uiso 0.671(7) 1 calc PR B 1
C43 C 0.5709(4) 0.7410(8) 0.2784(3) 0.107(5) Uani 0.671(7) 1 d PDU B 1
H43A H 0.5515 0.7178 0.3066 0.160 Uiso 0.671(7) 1 calc PR B 1
H43B H 0.5656 0.7988 0.2780 0.160 Uiso 0.671(7) 1 calc PR B 1
H43C H 0.6090 0.7293 0.2818 0.160 Uiso 0.671(7) 1 calc PR B 1
C42X C 0.5576(3) 0.7851(5) 0.2215(3) 0.040(2) Uani 0.329(7) 1 d PDU B 2
H42C H 0.5191 0.7975 0.2188 0.048 Uiso 0.329(7) 1 calc PR B 2
H42D H 0.5781 0.8355 0.2202 0.048 Uiso 0.329(7) 1 calc PR B 2
C43X C 0.5701(7) 0.7372(7) 0.2724(4) 0.041(3) Uiso 0.329(7) 1 d PDU B 2
H43D H 0.5599 0.7699 0.3012 0.062 Uiso 0.329(7) 1 calc PR B 2
H43E H 0.6083 0.7252 0.2742 0.062 Uiso 0.329(7) 1 calc PR B 2
H43F H 0.5497 0.6874 0.2729 0.062 Uiso 0.329(7) 1 calc PR B 2
O15 O 0.70710(7) 0.69663(10) 0.23998(6) 0.0306(3) Uani 1 1 d DU . .
C44 C 0.7523(2) 0.6730(3) 0.27263(17) 0.0335(12) Uani 0.596(9) 1 d PDU C 1
H44A H 0.7864 0.6862 0.2559 0.040 Uiso 0.596(9) 1 calc PR C 1
H44B H 0.7513 0.6147 0.2782 0.040 Uiso 0.596(9) 1 calc PR C 1
C45 C 0.7496(3) 0.7150(3) 0.32190(19) 0.0484(15) Uani 0.596(9) 1 d PDU C 1
H45A H 0.7143 0.7068 0.3375 0.058 Uiso 0.596(9) 1 calc PR C 1
H45B H 0.7553 0.7729 0.3173 0.058 Uiso 0.596(9) 1 calc PR C 1
C46 C 0.7939(2) 0.6797(4) 0.35540(16) 0.0986(17) Uani 1 1 d DU . .
H46A H 0.7932 0.7060 0.3881 0.148 Uiso 0.596(9) 1 calc PR C 1
H46B H 0.8286 0.6883 0.3396 0.148 Uiso 0.596(9) 1 calc PR C 1
H46C H 0.7878 0.6225 0.3597 0.148 Uiso 0.596(9) 1 calc PR C 1
H46D H 0.8301 0.6993 0.3614 0.148 Uiso 0.404(9) 1 calc PR C 2
H46E H 0.7925 0.6223 0.3619 0.148 Uiso 0.404(9) 1 calc PR C 2
H46F H 0.7689 0.7073 0.3777 0.148 Uiso 0.404(9) 1 calc PR C 2
C44X C 0.7242(4) 0.6697(5) 0.2886(3) 0.048(2) Uani 0.404(9) 1 d PDU C 2
H44C H 0.7227 0.6108 0.2896 0.057 Uiso 0.404(9) 1 calc PR C 2
H44D H 0.6992 0.6902 0.3142 0.057 Uiso 0.404(9) 1 calc PR C 2
C45X C 0.7785(4) 0.6955(8) 0.3016(4) 0.077(4) Uani 0.404(9) 1 d PDU C 2
H45C H 0.7817 0.7533 0.2950 0.092 Uiso 0.404(9) 1 calc PR C 2
H45D H 0.8041 0.6677 0.2795 0.092 Uiso 0.404(9) 1 calc PR C 2
N1 N 0.73417(18) 0.4385(3) -0.02511(14) 0.0951(13) Uani 1 1 d D . .
C47 C 0.72210(14) 0.4164(2) 0.01307(14) 0.0564(8) Uani 1 1 d D . .
C48 C 0.70725(11) 0.38783(16) 0.06235(12) 0.0430(6) Uani 1 1 d D . .
H48A H 0.6928 0.3338 0.0596 0.064 Uiso 1 1 calc R . .
H48B H 0.6802 0.4232 0.0767 0.064 Uiso 1 1 calc R . .
H48C H 0.7388 0.3872 0.0840 0.064 Uiso 1 1 calc R . .
N2 N 0.9598(4) 0.4379(6) 0.2239(4) 0.200(4) Uani 1 1 d DU . .
C49 C 0.9481(4) 0.4942(8) 0.2487(4) 0.171(4) Uani 1 1 d DU . .
C50 C 0.9302(3) 0.5604(4) 0.2815(3) 0.134(2) Uani 1 1 d DU . .
H50A H 0.8913 0.5590 0.2847 0.201 Uiso 1 1 calc R . .
H50B H 0.9411 0.6114 0.2669 0.201 Uiso 1 1 calc R . .
H50C H 0.9464 0.5545 0.3146 0.201 Uiso 1 1 calc R . .
N3 N 0.4850(9) 0.1432(13) 0.0952(8) 0.122(5) Uiso 0.25 1 d PDU . .
C51 C 0.5089(11) 0.1140(17) 0.1274(9) 0.122(5) Uiso 0.25 1 d PDU . .
C52 C 0.5337(11) 0.0764(16) 0.1701(9) 0.122(5) Uiso 0.25 1 d PDU . .

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
V1 0.02604(19) 0.02387(18) 0.02204(18) -0.00203(13) 0.00091(13) -0.00057(14)
O13 0.0349(9) 0.0334(9) 0.0254(8) 0.0003(7) 0.0035(6) -0.0019(7)
O1 0.0284(7) 0.0233(7) 0.0194(7) 0.0014(6) -0.0036(6) -0.0011(6)
O2 0.0278(8) 0.0260(8) 0.0236(7) -0.0005(6) -0.0002(6) 0.0011(6)
O3 0.0285(8) 0.0258(8) 0.0331(8) -0.0075(7) 0.0029(6) -0.0019(6)
O4 0.0456(10) 0.0282(8) 0.0251(8) -0.0009(6) -0.0030(7) 0.0047(7)
C1 0.0268(10) 0.0197(9) 0.0204(9) -0.0022(7) -0.0016(8) 0.0044(8)
C2 0.0243(10) 0.0226(9) 0.0232(10) -0.0020(8) -0.0013(8) 0.0040(8)
C3 0.0305(11) 0.0287(11) 0.0238(10) -0.0025(8) -0.0046(8) 0.0039(9)
C4 0.0370(12) 0.0350(12) 0.0209(10) 0.0003(9) -0.0002(9) 0.0033(10)
C5 0.0313(11) 0.0270(11) 0.0253(11) 0.0005(8) 0.0032(9) 0.0027(9)
C6 0.0253(10) 0.0214(10) 0.0250(10) -0.0008(8) -0.0019(8) 0.0032(8)
C7 0.0459(15) 0.0685(19) 0.0203(11) 0.0032(12) -0.0026(10) -0.0052(14)
C8 0.079(4) 0.119(6) 0.025(2) 0.019(3) -0.020(3) -0.045(4)
C9 0.067(4) 0.059(3) 0.030(2) 0.016(2) -0.004(2) 0.000(3)
C10 0.083(4) 0.090(5) 0.025(2) 0.001(3) 0.013(2) 0.015(4)
C8X 0.116(10) 0.117(8) 0.026(4) -0.025(5) 0.007(5) -0.037(7)
C9X 0.093(6) 0.125(11) 0.024(4) 0.021(5) 0.003(4) -0.038(7)
C10X 0.110(9) 0.159(13) 0.041(5) 0.039(7) -0.009(6) 0.055(10)
S1 0.0253(2) 0.0193(2) 0.0261(3) 0.00219(19) -0.0013(2) -0.00021(19)
O5 0.0326(8) 0.0206(7) 0.0295(8) -0.0020(6) -0.0040(6) -0.0002(6)
O6 0.0319(8) 0.0264(8) 0.0362(9) 0.0084(7) 0.0013(7) -0.0028(7)
C11 0.0225(10) 0.0212(9) 0.0245(10) -0.0013(8) -0.0023(8) -0.0030(8)
C12 0.0217(9) 0.0189(9) 0.0269(10) 0.0018(8) -0.0031(8) -0.0015(8)
C13 0.0250(10) 0.0221(10) 0.0243(10) 0.0015(8) -0.0007(8) -0.0034(8)
C14 0.0229(10) 0.0231(10) 0.0286(11) 0.0001(8) 0.0007(8) -0.0012(8)
C15 0.0233(10) 0.0223(10) 0.0285(11) 0.0030(8) -0.0032(8) 0.0000(8)
C16 0.0244(10) 0.0215(10) 0.0239(10) 0.0025(8) -0.0037(8) -0.0033(8)
C17 0.0302(11) 0.0253(10) 0.0311(11) 0.0000(9) 0.0057(9) 0.0025(9)
C18 0.0458(14) 0.0342(13) 0.0336(13) 0.0042(10) 0.0130(11) 0.0055(11)
C19 0.0273(12) 0.0485(16) 0.0502(16) -0.0017(13) 0.0053(11) 0.0045(11)
C20 0.0474(15) 0.0255(11) 0.0386(13) -0.0015(10) 0.0070(11) 0.0026(10)
S2 0.0254(2) 0.0229(2) 0.0227(2) 0.00229(19) -0.00429(19) -0.00201(19)
O7 0.0350(9) 0.0310(8) 0.0265(8) -0.0007(6) -0.0068(7) -0.0073(7)
O8 0.0298(8) 0.0273(8) 0.0309(8) 0.0065(6) -0.0049(6) 0.0015(6)
C21 0.0268(10) 0.0208(9) 0.0235(10) 0.0030(8) -0.0022(8) 0.0012(8)
C22 0.0256(10) 0.0226(10) 0.0237(10) 0.0026(8) -0.0004(8) -0.0012(8)
C23 0.0366(12) 0.0288(11) 0.0229(10) -0.0002(9) -0.0017(9) -0.0012(9)
C24 0.0374(13) 0.0392(13) 0.0237(11) 0.0016(9) 0.0051(9) 0.0021(10)
C25 0.0288(11) 0.0388(13) 0.0268(11) 0.0086(9) 0.0025(9) -0.0018(10)
C26 0.0271(10) 0.0261(10) 0.0256(10) 0.0045(8) -0.0037(8) -0.0026(8)
C27 0.0526(17) 0.0576(18) 0.0309(13) -0.0046(12) 0.0141(12) -0.0002(14)
C28 0.196(6) 0.055(2) 0.068(3) 0.0094(19) 0.074(3) 0.043(3)
C29 0.059(2) 0.088(3) 0.0314(14) -0.0112(15) 0.0046(13) -0.0014(18)
C30 0.0494(19) 0.119(3) 0.0412(17) -0.0026(19) 0.0132(14) 0.005(2)
S3 0.0283(3) 0.0258(3) 0.0330(3) 0.0058(2) -0.0058(2) -0.0061(2)
O9 0.0371(9) 0.0241(8) 0.0448(10) 0.0036(7) -0.0126(8) -0.0014(7)
O10 0.0352(9) 0.0460(11) 0.0449(11) 0.0119(9) -0.0021(8) -0.0146(8)
C31 0.0238(10) 0.0253(10) 0.0267(10) -0.0015(8) -0.0025(8) -0.0015(8)
C32 0.0252(10) 0.0229(10) 0.0310(11) 0.0019(8) -0.0061(8) -0.0016(8)
C33 0.0275(11) 0.0233(10) 0.0395(13) -0.0027(9) -0.0085(9) 0.0002(9)
C34 0.0273(11) 0.0275(11) 0.0339(12) -0.0085(9) -0.0095(9) 0.0036(9)
C35 0.0271(11) 0.0286(11) 0.0275(11) -0.0030(9) -0.0077(8) 0.0029(9)
C36 0.0215(9) 0.0225(10) 0.0284(11) -0.0012(8) -0.0043(8) 0.0012(8)
C37 0.0383(13) 0.0322(12) 0.0393(13) -0.0140(10) -0.0140(11) 0.0062(10)
C38 0.089(3) 0.0402(16) 0.062(2) -0.0223(15) -0.0349(19) 0.0243(17)
C39 0.0529(17) 0.0409(15) 0.0579(18) -0.0207(13) -0.0289(14) 0.0110(13)
C40 0.077(2) 0.080(3) 0.057(2) -0.0376(19) 0.0170(18) -0.024(2)
S4 0.0225(2) 0.0236(2) 0.0241(2) -0.00199(19) -0.00324(19) 0.00373(19)
O11 0.0296(8) 0.0278(8) 0.0259(8) -0.0033(6) 0.0013(6) 0.0049(6)
O12 0.0253(8) 0.0326(8) 0.0332(8) -0.0002(7) -0.0092(6) 0.0050(6)
O14 0.0408(9) 0.0279(8) 0.0293(8) -0.0011(7) -0.0017(7) 0.0038(7)
C41 0.0435(14) 0.0411(14) 0.0416(14) -0.0017(11) 0.0012(11) 0.0198(12)
C42 0.0321(19) 0.044(2) 0.048(2) -0.0069(18) 0.0083(16) -0.0006(16)
C43 0.052(4) 0.227(12) 0.041(3) -0.055(5) 0.010(3) -0.020(5)
C42X 0.029(4) 0.045(5) 0.047(5) -0.007(3) 0.007(3) -0.003(3)
O15 0.0376(9) 0.0263(8) 0.0281(8) -0.0035(6) -0.0062(7) 0.0010(7)
C44 0.034(3) 0.039(2) 0.027(2) -0.0007(17) -0.0013(18) -0.0023(19)
C45 0.069(4) 0.044(3) 0.032(2) -0.001(2) -0.009(2) -0.007(3)
C46 0.115(4) 0.129(4) 0.052(2) 0.013(2) -0.032(2) 0.016(3)
C44X 0.064(6) 0.045(4) 0.034(4) 0.005(3) -0.007(4) -0.002(4)
C45X 0.059(6) 0.106(8) 0.066(6) 0.053(6) -0.024(5) -0.031(6)
N1 0.098(3) 0.126(4) 0.061(2) 0.010(2) -0.008(2) -0.024(3)
C47 0.0516(18) 0.061(2) 0.057(2) -0.0008(16) -0.0106(15) -0.0101(15)
C48 0.0362(13) 0.0319(13) 0.0607(18) -0.0042(12) -0.0042(12) -0.0037(11)
N2 0.182(8) 0.241(11) 0.178(9) -0.006(6) 0.027(6) -0.033(8)
C49 0.099(6) 0.243(13) 0.170(9) -0.031(7) 0.002(6) -0.037(7)
C50 0.100(4) 0.119(5) 0.184(7) 0.040(4) -0.060(4) -0.050(4)

_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
V1 O13 1.5817(16) . ?
V1 O14 1.7759(17) . ?
V1 O1 1.9273(15) . ?
V1 O2 1.9508(16) . ?
V1 O15 2.0491(16) . ?
V1 O5 2.3782(17) . ?
O1 C1 1.323(2) . ?
O2 C11 1.307(3) . ?
O3 C21 1.354(3) . ?
O4 C31 1.338(3) . ?
C1 C6 1.405(3) . ?
C1 C2 1.408(3) . ?
C2 C3 1.399(3) . ?
C2 S4 1.766(2) . ?
C3 C4 1.390(3) . ?
C4 C5 1.403(3) . ?
C4 C7 1.537(3) . ?
C5 C6 1.391(3) . ?
C6 S1 1.760(2) . ?
C7 C10X 1.481(9) . ?
C7 C10 1.491(6) . ?
C7 C8 1.512(6) . ?
C7 C9X 1.516(9) . ?
C7 C8X 1.581(9) . ?
C7 C9 1.598(6) . ?
S1 O6 1.4373(17) . ?
S1 O5 1.4591(16) . ?
S1 C12 1.753(2) . ?
C11 C12 1.416(3) . ?
C11 C16 1.418(3) . ?
C12 C13 1.402(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.401(3) . ?
C14 C17 1.529(3) . ?
C15 C16 1.383(3) . ?
C16 S2 1.765(2) . ?
C17 C18 1.531(3) . ?
C17 C19 1.535(4) . ?
C17 C20 1.538(3) . ?
S2 O7 1.4381(16) . ?
S2 O8 1.4514(17) . ?
S2 C22 1.765(2) . ?
C21 C26 1.395(3) . ?
C21 C22 1.402(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.398(3) . ?
C24 C25 1.384(4) . ?
C24 C27 1.529(3) . ?
C25 C26 1.388(3) . ?
C26 S3 1.761(2) . ?
C27 C28 1.525(5) . ?
C27 C30 1.528(5) . ?
C27 C29 1.553(5) . ?
S3 O10 1.4327(19) . ?
S3 O9 1.4485(19) . ?
S3 C32 1.775(2) . ?
C31 C32 1.403(3) . ?
C31 C36 1.410(3) . ?
C32 C33 1.397(3) . ?
C33 C34 1.388(3) . ?
C34 C35 1.394(3) . ?
C34 C37 1.533(3) . ?
C35 C36 1.393(3) . ?
C36 S4 1.764(2) . ?
C37 C38 1.515(4) . ?
C37 C39 1.522(4) . ?
C37 C40 1.549(5) . ?
S4 O12 1.4363(16) . ?
S4 O11 1.4477(16) . ?
O14 C41 1.412(3) . ?
C41 C42 1.443(5) . ?
C41 C42X 1.451(8) . ?
C42 C43 1.605(6) . ?
C42X C43X 1.613(8) . ?
O15 C44X 1.444(7) . ?
O15 C44 1.486(5) . ?
C44 C45 1.497(7) . ?
C45 C46 1.544(7) . ?
C46 C45X 1.514(9) . ?
C44X C45X 1.471(11) . ?
N1 C47 1.129(5) . ?
C47 C48 1.452(5) . ?
N2 C49 1.192(10) . ?
C49 C50 1.486(10) . ?
N3 C51 1.159(15) . ?
C51 C52 1.446(16) . ?

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
O13 V1 O14 103.03(9) . . ?
O13 V1 O1 97.71(8) . . ?
O14 V1 O1 95.78(7) . . ?
O13 V1 O2 98.12(8) . . ?
O14 V1 O2 158.06(8) . . ?
O1 V1 O2 87.05(6) . . ?
O13 V1 O15 97.47(8) . . ?
O14 V1 O15 88.34(7) . . ?
O1 V1 O15 162.94(7) . . ?
O2 V1 O15 83.14(7) . . ?
O13 V1 O5 174.85(8) . . ?
O14 V1 O5 81.74(7) . . ?
O1 V1 O5 83.63(6) . . ?
O2 V1 O5 76.95(6) . . ?
O15 V1 O5 80.58(6) . . ?
C1 O1 V1 129.66(13) . . ?
C11 O2 V1 134.67(14) . . ?
O1 C1 C6 122.36(19) . . ?
O1 C1 C2 122.03(19) . . ?
C6 C1 C2 115.51(19) . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 S4 118.41(17) . . ?
C1 C2 S4 119.81(16) . . ?
C4 C3 C2 121.7(2) . . ?
C3 C4 C5 117.3(2) . . ?
C3 C4 C7 121.9(2) . . ?
C5 C4 C7 120.7(2) . . ?
C6 C5 C4 120.8(2) . . ?
C5 C6 C1 122.9(2) . . ?
C5 C6 S1 119.59(17) . . ?
C1 C6 S1 117.46(16) . . ?
C10 C7 C8 113.6(5) . . ?
C10X C7 C9X 111.4(8) . . ?
C10X C7 C4 109.5(4) . . ?
C10 C7 C4 110.8(3) . . ?
C8 C7 C4 112.6(3) . . ?
C9X C7 C4 113.7(4) . . ?
C10X C7 C8X 111.4(9) . . ?
C9X C7 C8X 105.6(7) . . ?
C4 C7 C8X 105.1(4) . . ?
C10 C7 C9 107.9(4) . . ?
C8 C7 C9 104.7(4) . . ?
C4 C7 C9 106.8(3) . . ?
O6 S1 O5 117.35(10) . . ?
O6 S1 C12 109.01(10) . . ?
O5 S1 C12 107.33(10) . . ?
O6 S1 C6 107.94(10) . . ?
O5 S1 C6 106.23(10) . . ?
C12 S1 C6 108.71(10) . . ?
S1 O5 V1 116.75(9) . . ?
O2 C11 C12 126.83(19) . . ?
O2 C11 C16 118.68(19) . . ?
C12 C11 C16 114.48(19) . . ?
C13 C12 C11 122.11(19) . . ?
C13 C12 S1 116.91(16) . . ?
C11 C12 S1 120.89(16) . . ?
C14 C13 C12 122.1(2) . . ?
C13 C14 C15 116.5(2) . . ?
C13 C14 C17 123.9(2) . . ?
C15 C14 C17 119.6(2) . . ?
C16 C15 C14 121.8(2) . . ?
C15 C16 C11 122.9(2) . . ?
C15 C16 S2 118.41(16) . . ?
C11 C16 S2 118.66(16) . . ?
C14 C17 C18 112.31(19) . . ?
C14 C17 C19 108.4(2) . . ?
C18 C17 C19 108.6(2) . . ?
C14 C17 C20 109.38(19) . . ?
C18 C17 C20 108.2(2) . . ?
C19 C17 C20 110.0(2) . . ?
O7 S2 O8 117.11(10) . . ?
O7 S2 C22 107.53(10) . . ?
O8 S2 C22 107.39(10) . . ?
O7 S2 C16 109.53(10) . . ?
O8 S2 C16 107.54(10) . . ?
C22 S2 C16 107.33(10) . . ?
O3 C21 C26 125.2(2) . . ?
O3 C21 C22 118.09(19) . . ?
C26 C21 C22 116.7(2) . . ?
C23 C22 C21 121.5(2) . . ?
C23 C22 S2 118.43(17) . . ?
C21 C22 S2 119.68(17) . . ?
C22 C23 C24 121.4(2) . . ?
C25 C24 C23 117.1(2) . . ?
C25 C24 C27 123.3(2) . . ?
C23 C24 C27 119.6(2) . . ?
C24 C25 C26 121.8(2) . . ?
C25 C26 C21 121.4(2) . . ?
C25 C26 S3 119.07(18) . . ?
C21 C26 S3 119.45(17) . . ?
C28 C27 C30 113.6(4) . . ?
C28 C27 C24 109.6(2) . . ?
C30 C27 C24 111.2(3) . . ?
C28 C27 C29 107.2(4) . . ?
C30 C27 C29 106.6(3) . . ?
C24 C27 C29 108.4(2) . . ?
O10 S3 O9 118.64(12) . . ?
O10 S3 C26 108.05(11) . . ?
O9 S3 C26 107.32(11) . . ?
O10 S3 C32 109.00(11) . . ?
O9 S3 C32 105.97(11) . . ?
C26 S3 C32 107.37(10) . . ?
O4 C31 C32 118.7(2) . . ?
O4 C31 C36 125.3(2) . . ?
C32 C31 C36 116.0(2) . . ?
C33 C32 C31 121.7(2) . . ?
C33 C32 S3 116.18(17) . . ?
C31 C32 S3 122.02(17) . . ?
C34 C33 C32 121.7(2) . . ?
C33 C34 C35 117.1(2) . . ?
C33 C34 C37 123.3(2) . . ?
C35 C34 C37 119.6(2) . . ?
C36 C35 C34 121.5(2) . . ?
C35 C36 C31 121.7(2) . . ?
C35 C36 S4 116.37(17) . . ?
C31 C36 S4 121.89(16) . . ?
C38 C37 C39 109.0(2) . . ?
C38 C37 C34 111.7(2) . . ?
C39 C37 C34 109.9(2) . . ?
C38 C37 C40 109.5(3) . . ?
C39 C37 C40 107.7(3) . . ?
C34 C37 C40 108.9(2) . . ?
O12 S4 O11 117.84(10) . . ?
O12 S4 C36 108.18(10) . . ?
O11 S4 C36 108.08(10) . . ?
O12 S4 C2 107.57(10) . . ?
O11 S4 C2 110.09(10) . . ?
C36 S4 C2 104.24(10) . . ?
C41 O14 V1 138.53(17) . . ?
O14 C41 C42 115.8(3) . . ?
O14 C41 C42X 123.9(4) . . ?
C41 C42 C43 116.2(5) . . ?
C41 C42X C43X 104.7(7) . . ?
C44X O15 V1 123.2(3) . . ?
C44 O15 V1 126.0(2) . . ?
O15 C44 C45 111.0(4) . . ?
C44 C45 C46 107.4(5) . . ?
O15 C44X C45X 113.3(7) . . ?
C44X C45X C46 114.1(8) . . ?
N1 C47 C48 179.3(4) . . ?
N2 C49 C50 175.6(12) . . ?
N3 C51 C52 174(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O13 V1 O1 C1 146.43(18) . . . . ?
O14 V1 O1 C1 42.40(19) . . . . ?
O2 V1 O1 C1 -115.77(18) . . . . ?
O15 V1 O1 C1 -60.9(3) . . . . ?
O5 V1 O1 C1 -38.58(17) . . . . ?
O13 V1 O2 C11 135.4(2) . . . . ?
O14 V1 O2 C11 -60.1(3) . . . . ?
O1 V1 O2 C11 38.03(19) . . . . ?
O15 V1 O2 C11 -128.0(2) . . . . ?
O5 V1 O2 C11 -46.11(19) . . . . ?
V1 O1 C1 C6 60.7(3) . . . . ?
V1 O1 C1 C2 -123.13(19) . . . . ?
O1 C1 C2 C3 -173.24(19) . . . . ?
C6 C1 C2 C3 3.2(3) . . . . ?
O1 C1 C2 S4 4.6(3) . . . . ?
C6 C1 C2 S4 -178.99(15) . . . . ?
C1 C2 C3 C4 -1.8(3) . . . . ?
S4 C2 C3 C4 -179.63(18) . . . . ?
C2 C3 C4 C5 -0.3(3) . . . . ?
C2 C3 C4 C7 -179.5(2) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C7 C4 C5 C6 180.0(2) . . . . ?
C4 C5 C6 C1 0.9(3) . . . . ?
C4 C5 C6 S1 -176.08(18) . . . . ?
O1 C1 C6 C5 173.7(2) . . . . ?
C2 C1 C6 C5 -2.8(3) . . . . ?
O1 C1 C6 S1 -9.3(3) . . . . ?
C2 C1 C6 S1 174.25(15) . . . . ?
C3 C4 C7 C10X 57.3(9) . . . . ?
C5 C4 C7 C10X -122.0(8) . . . . ?
C3 C4 C7 C10 -132.8(4) . . . . ?
C5 C4 C7 C10 48.0(5) . . . . ?
C3 C4 C7 C8 -4.4(5) . . . . ?
C5 C4 C7 C8 176.4(4) . . . . ?
C3 C4 C7 C9X -177.4(7) . . . . ?
C5 C4 C7 C9X 3.3(8) . . . . ?
C3 C4 C7 C8X -62.5(6) . . . . ?
C5 C4 C7 C8X 118.3(6) . . . . ?
C3 C4 C7 C9 109.9(3) . . . . ?
C5 C4 C7 C9 -69.3(4) . . . . ?
C5 C6 S1 O6 1.5(2) . . . . ?
C1 C6 S1 O6 -175.60(16) . . . . ?
C5 C6 S1 O5 128.18(18) . . . . ?
C1 C6 S1 O5 -48.93(18) . . . . ?
C5 C6 S1 C12 -116.60(18) . . . . ?
C1 C6 S1 C12 66.29(19) . . . . ?
O6 S1 O5 V1 179.89(9) . . . . ?
C12 S1 O5 V1 -57.05(12) . . . . ?
C6 S1 O5 V1 59.11(11) . . . . ?
O14 V1 O5 S1 -121.68(11) . . . . ?
O1 V1 O5 S1 -24.87(10) . . . . ?
O2 V1 O5 S1 63.57(10) . . . . ?
O15 V1 O5 S1 148.64(11) . . . . ?
V1 O2 C11 C12 23.0(3) . . . . ?
V1 O2 C11 C16 -155.70(16) . . . . ?
O2 C11 C12 C13 -177.3(2) . . . . ?
C16 C11 C12 C13 1.5(3) . . . . ?
O2 C11 C12 S1 6.3(3) . . . . ?
C16 C11 C12 S1 -174.94(15) . . . . ?
O6 S1 C12 C13 -30.8(2) . . . . ?
O5 S1 C12 C13 -158.91(16) . . . . ?
C6 S1 C12 C13 86.59(18) . . . . ?
O6 S1 C12 C11 145.78(17) . . . . ?
O5 S1 C12 C11 17.7(2) . . . . ?
C6 S1 C12 C11 -96.79(18) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
S1 C12 C13 C14 177.02(17) . . . . ?
C12 C13 C14 C15 -1.1(3) . . . . ?
C12 C13 C14 C17 -180.0(2) . . . . ?
C13 C14 C15 C16 -0.2(3) . . . . ?
C17 C14 C15 C16 178.7(2) . . . . ?
C14 C15 C16 C11 2.3(3) . . . . ?
C14 C15 C16 S2 -176.87(17) . . . . ?
O2 C11 C16 C15 176.02(19) . . . . ?
C12 C11 C16 C15 -2.9(3) . . . . ?
O2 C11 C16 S2 -4.8(3) . . . . ?
C12 C11 C16 S2 176.33(15) . . . . ?
C13 C14 C17 C18 -6.1(3) . . . . ?
C15 C14 C17 C18 175.1(2) . . . . ?
C13 C14 C17 C19 113.9(2) . . . . ?
C15 C14 C17 C19 -64.9(3) . . . . ?
C13 C14 C17 C20 -126.2(2) . . . . ?
C15 C14 C17 C20 55.0(3) . . . . ?
C15 C16 S2 O7 118.93(18) . . . . ?
C11 C16 S2 O7 -60.31(19) . . . . ?
C15 C16 S2 O8 -9.3(2) . . . . ?
C11 C16 S2 O8 171.43(16) . . . . ?
C15 C16 S2 C22 -124.61(18) . . . . ?
C11 C16 S2 C22 56.15(19) . . . . ?
O3 C21 C22 C23 -179.5(2) . . . . ?
C26 C21 C22 C23 1.6(3) . . . . ?
O3 C21 C22 S2 -6.8(3) . . . . ?
C26 C21 C22 S2 174.27(16) . . . . ?
O7 S2 C22 C23 -10.9(2) . . . . ?
O8 S2 C22 C23 115.93(18) . . . . ?
C16 S2 C22 C23 -128.69(18) . . . . ?
O7 S2 C22 C21 176.19(17) . . . . ?
O8 S2 C22 C21 -56.9(2) . . . . ?
C16 S2 C22 C21 58.4(2) . . . . ?
C21 C22 C23 C24 0.5(3) . . . . ?
S2 C22 C23 C24 -172.28(19) . . . . ?
C22 C23 C24 C25 -1.8(4) . . . . ?
C22 C23 C24 C27 176.2(2) . . . . ?
C23 C24 C25 C26 1.0(4) . . . . ?
C27 C24 C25 C26 -176.9(2) . . . . ?
C24 C25 C26 C21 1.1(4) . . . . ?
C24 C25 C26 S3 178.98(19) . . . . ?
O3 C21 C26 C25 178.8(2) . . . . ?
C22 C21 C26 C25 -2.4(3) . . . . ?
O3 C21 C26 S3 0.9(3) . . . . ?
C22 C21 C26 S3 179.76(16) . . . . ?
C25 C24 C27 C28 -123.6(4) . . . . ?
C23 C24 C27 C28 58.6(4) . . . . ?
C25 C24 C27 C30 2.8(4) . . . . ?
C23 C24 C27 C30 -175.1(3) . . . . ?
C25 C24 C27 C29 119.7(3) . . . . ?
C23 C24 C27 C29 -58.1(3) . . . . ?
C25 C26 S3 O10 -9.6(2) . . . . ?
C21 C26 S3 O10 168.30(18) . . . . ?
C25 C26 S3 O9 -138.63(19) . . . . ?
C21 C26 S3 O9 39.3(2) . . . . ?
C25 C26 S3 C32 107.83(19) . . . . ?
C21 C26 S3 C32 -74.3(2) . . . . ?
O4 C31 C32 C33 175.9(2) . . . . ?
C36 C31 C32 C33 -3.3(3) . . . . ?
O4 C31 C32 S3 -0.4(3) . . . . ?
C36 C31 C32 S3 -179.51(16) . . . . ?
O10 S3 C32 C33 -99.0(2) . . . . ?
O9 S3 C32 C33 29.7(2) . . . . ?
C26 S3 C32 C33 144.19(18) . . . . ?
O10 S3 C32 C31 77.4(2) . . . . ?
O9 S3 C32 C31 -153.82(18) . . . . ?
C26 S3 C32 C31 -39.4(2) . . . . ?
C31 C32 C33 C34 -0.3(4) . . . . ?
S3 C32 C33 C34 176.10(19) . . . . ?
C32 C33 C34 C35 3.4(4) . . . . ?
C32 C33 C34 C37 -178.4(2) . . . . ?
C33 C34 C35 C36 -2.7(3) . . . . ?
C37 C34 C35 C36 179.0(2) . . . . ?
C34 C35 C36 C31 -1.0(3) . . . . ?
C34 C35 C36 S4 178.01(18) . . . . ?
O4 C31 C36 C35 -175.2(2) . . . . ?
C32 C31 C36 C35 3.9(3) . . . . ?
O4 C31 C36 S4 5.9(3) . . . . ?
C32 C31 C36 S4 -175.02(16) . . . . ?
C33 C34 C37 C38 7.7(4) . . . . ?
C35 C34 C37 C38 -174.1(3) . . . . ?
C33 C34 C37 C39 128.9(3) . . . . ?
C35 C34 C37 C39 -52.9(3) . . . . ?
C33 C34 C37 C40 -113.4(3) . . . . ?
C35 C34 C37 C40 64.8(3) . . . . ?
C35 C36 S4 O12 40.8(2) . . . . ?
C31 C36 S4 O12 -140.24(18) . . . . ?
C35 C36 S4 O11 169.39(17) . . . . ?
C31 C36 S4 O11 -11.6(2) . . . . ?
C35 C36 S4 C2 -73.50(19) . . . . ?
C31 C36 S4 C2 105.49(19) . . . . ?
C3 C2 S4 O12 -11.3(2) . . . . ?
C1 C2 S4 O12 170.81(16) . . . . ?
C3 C2 S4 O11 -140.90(17) . . . . ?
C1 C2 S4 O11 41.2(2) . . . . ?
C3 C2 S4 C36 103.40(18) . . . . ?
C1 C2 S4 C36 -74.49(19) . . . . ?
O13 V1 O14 C41 -10.0(3) . . . . ?
O1 V1 O14 C41 89.4(2) . . . . ?
O2 V1 O14 C41 -174.2(2) . . . . ?
O15 V1 O14 C41 -107.2(2) . . . . ?
O5 V1 O14 C41 172.0(3) . . . . ?
V1 O14 C41 C42 29.3(4) . . . . ?
V1 O14 C41 C42X 96.2(5) . . . . ?
O14 C41 C42 C43 70.1(6) . . . . ?
C42X C41 C42 C43 -45.2(7) . . . . ?
O14 C41 C42X C43X -64.1(9) . . . . ?
C42 C41 C42X C43X 37.0(7) . . . . ?
O13 V1 O15 C44X 37.4(5) . . . . ?
O14 V1 O15 C44X 140.3(5) . . . . ?
O1 V1 O15 C44X -115.3(6) . . . . ?
O2 V1 O15 C44X -59.9(5) . . . . ?
O5 V1 O15 C44X -137.8(5) . . . . ?
O13 V1 O15 C44 77.3(3) . . . . ?
O14 V1 O15 C44 -179.8(3) . . . . ?
O1 V1 O15 C44 -75.4(4) . . . . ?
O2 V1 O15 C44 -20.1(3) . . . . ?
O5 V1 O15 C44 -97.9(3) . . . . ?
C44X O15 C44 C45 -48.8(7) . . . . ?
V1 O15 C44 C45 -145.8(4) . . . . ?
O15 C44 C45 C46 173.4(4) . . . . ?
C44 C45 C46 C45X 27.8(7) . . . . ?
C44 O15 C44X C45X 29.1(9) . . . . ?
V1 O15 C44X C45X 135.4(9) . . . . ?
O15 C44X C45X C46 170.5(8) . . . . ?
C45 C46 C45X C44X -48.4(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O9 0.84 2.11 2.820(2) 143 .
O3 H3 O5 0.84 2.32 2.798(2) 117 8_755
O4 H4 O11 0.84 1.92 2.677(2) 148 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076


data_L(OH)2(OPent)2
_database_code_depnum_ccdc_archive 'CCDC 835507'
#TrackingRef '- Vanadyl-calixarenes.cif'

_chemical_name_systematic        
;
1,3-Dipentoxy-p-tert-butylcalix[4]areneH2
;
_chemical_name_common            1,3-Dipentoxy-p-tert-butylcalix(4)areneH2
_chemical_melting_point          ?
_chemical_formula_structural     'Cax[4](OH)2(OPent)2, MeCN'
_chemical_formula_moiety         'C54 H76 O4, C2 H3 N'
_chemical_formula_sum            'C56 H79 N O4'
_chemical_formula_weight         830.20

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   19.6800(7)
_cell_length_b                   11.5784(4)
_cell_length_c                   23.5588(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.527(4)
_cell_angle_gamma                90.00
_cell_volume                     5059.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    6760
_cell_measurement_theta_min      3.1585
_cell_measurement_theta_max      27.4996

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1816
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40390
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         22.50
_reflns_number_total             6590
_reflns_number_gt                4119
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_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.

The hydrogen atoms on O(2) and O(4) were located in the Fourier difference
map. The O---H distance was restrained to 0.84 \%A, and the thermal motion
of the hydrogen atoms was set to 1.2 times that of the parent oyxgen.
;

_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^)+(0.0882P)^2^+11.2386P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6590
_refine_ls_number_parameters     571
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.1007
_refine_ls_wR_factor_ref         0.2470
_refine_ls_wR_factor_gt          0.2140
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0001(3) 0.3124(5) 0.1319(2) 0.0315(13) Uani 1 1 d . . .
C2 C 0.0077(3) 0.2450(5) 0.1830(2) 0.0302(13) Uani 1 1 d . . .
C3 C 0.0802(3) 0.2203(5) 0.2300(2) 0.0348(14) Uani 1 1 d . . .
H3A H 0.1178 0.2215 0.2107 0.042 Uiso 1 1 calc R . .
H3B H 0.0795 0.1422 0.2468 0.042 Uiso 1 1 calc R . .
C4 C 0.0988(3) 0.3080(5) 0.2805(2) 0.0312(13) Uani 1 1 d . . .
C5 C 0.1298(3) 0.4145(5) 0.2761(2) 0.0334(14) Uani 1 1 d . . .
C6 C 0.1437(3) 0.4960(5) 0.3221(2) 0.0318(13) Uani 1 1 d . . .
C7 C 0.1719(3) 0.6144(5) 0.3151(2) 0.0383(15) Uani 1 1 d . . .
H7A H 0.1992 0.6103 0.2867 0.046 Uiso 1 1 calc R . .
H7B H 0.2053 0.6410 0.3545 0.046 Uiso 1 1 calc R . .
C8 C 0.1103(3) 0.7005(5) 0.2918(2) 0.0324(13) Uani 1 1 d . . .
C9 C 0.0859(3) 0.7377(5) 0.2316(3) 0.0347(14) Uani 1 1 d . . .
C10 C 0.1790(3) 0.7794(6) 0.1901(3) 0.0478(16) Uani 1 1 d . . .
H10A H 0.2177 0.7818 0.2299 0.057 Uiso 1 1 calc R . .
H10B H 0.1605 0.8588 0.1795 0.057 Uiso 1 1 calc R . .
C11 C 0.2081(3) 0.7336(6) 0.1436(3) 0.0483(16) Uani 1 1 d . . .
H11A H 0.2457 0.7867 0.1396 0.058 Uiso 1 1 calc R . .
H11B H 0.1688 0.7306 0.1042 0.058 Uiso 1 1 calc R . .
C12 C 0.2403(3) 0.6130(6) 0.1597(3) 0.0543(18) Uani 1 1 d . . .
H12A H 0.2860 0.6199 0.1939 0.065 Uiso 1 1 calc R . .
H12B H 0.2068 0.5660 0.1735 0.065 Uiso 1 1 calc R . .
C13 C 0.2548(5) 0.5511(7) 0.1104(3) 0.090(3) Uani 1 1 d . . .
H13A H 0.2897 0.5962 0.0974 0.109 Uiso 1 1 calc R . .
H13B H 0.2096 0.5453 0.0757 0.109 Uiso 1 1 calc R . .
C14 C 0.2849(5) 0.4303(8) 0.1284(4) 0.100(3) Uani 1 1 d . . .
H14A H 0.3338 0.4359 0.1577 0.150 Uiso 1 1 calc R . .
H14B H 0.2864 0.3886 0.0926 0.150 Uiso 1 1 calc R . .
H14C H 0.2540 0.3886 0.1465 0.150 Uiso 1 1 calc R . .
C15 C 0.0241(3) 0.8055(5) 0.2089(2) 0.0343(14) Uani 1 1 d . . .
C16 C -0.0089(3) 0.8303(5) 0.1418(2) 0.0381(14) Uani 1 1 d . . .
H16A H 0.0296 0.8318 0.1235 0.046 Uiso 1 1 calc R . .
H16B H -0.0322 0.9073 0.1360 0.046 Uiso 1 1 calc R . .
C17 C -0.0648(3) 0.7389(5) 0.1103(2) 0.0356(14) Uani 1 1 d . . .
C18 C -0.0460(3) 0.6349(5) 0.0893(2) 0.0364(15) Uani 1 1 d . . .
C19 C -0.0985(3) 0.5526(5) 0.0625(2) 0.0353(14) Uani 1 1 d . . .
C20 C -0.0769(3) 0.4369(5) 0.0444(2) 0.0410(15) Uani 1 1 d . . .
H20A H -0.0313 0.4450 0.0356 0.049 Uiso 1 1 calc R . .
H20B H -0.1146 0.4096 0.0073 0.049 Uiso 1 1 calc R . .
C21 C -0.0670(3) 0.3486(5) 0.0946(2) 0.0339(14) Uani 1 1 d . . .
C22 C -0.1273(3) 0.3075(5) 0.1070(2) 0.0355(14) Uani 1 1 d . . .
H22 H -0.1736 0.3298 0.0809 0.043 Uiso 1 1 calc R . .
C23 C -0.1232(3) 0.2361(5) 0.1551(2) 0.0320(13) Uani 1 1 d . . .
C24 C -0.0541(3) 0.2076(5) 0.1928(2) 0.0356(14) Uani 1 1 d . . .
H24 H -0.0493 0.1602 0.2268 0.043 Uiso 1 1 calc R . .
C25 C -0.1900(3) 0.1904(5) 0.1675(3) 0.0439(16) Uani 1 1 d . . .
C26 C -0.1890(4) 0.0583(7) 0.1674(5) 0.118(4) Uani 1 1 d . . .
H26A H -0.1496 0.0306 0.2026 0.178 Uiso 1 1 calc R . .
H26B H -0.1817 0.0306 0.1306 0.178 Uiso 1 1 calc R . .
H26C H -0.2350 0.0289 0.1691 0.178 Uiso 1 1 calc R . .
C27 C -0.1914(5) 0.2352(12) 0.2258(4) 0.160(6) Uani 1 1 d . . .
H27A H -0.1991 0.3189 0.2230 0.241 Uiso 1 1 calc R . .
H27B H -0.1454 0.2182 0.2573 0.241 Uiso 1 1 calc R . .
H27C H -0.2307 0.1981 0.2359 0.241 Uiso 1 1 calc R . .
C28 C -0.2592(3) 0.2207(8) 0.1186(3) 0.080(3) Uani 1 1 d . . .
H28A H -0.2997 0.1844 0.1271 0.121 Uiso 1 1 calc R . .
H28B H -0.2574 0.1929 0.0798 0.121 Uiso 1 1 calc R . .
H28C H -0.2655 0.3048 0.1170 0.121 Uiso 1 1 calc R . .
C29 C -0.1696(3) 0.5765(5) 0.0564(2) 0.0373(15) Uani 1 1 d . . .
H29 H -0.2053 0.5212 0.0365 0.045 Uiso 1 1 calc R . .
C30 C -0.1913(3) 0.6751(5) 0.0774(2) 0.0399(15) Uani 1 1 d . . .
C31 C -0.1370(3) 0.7562(5) 0.1045(2) 0.0424(16) Uani 1 1 d . . .
H31 H -0.1500 0.8258 0.1195 0.051 Uiso 1 1 calc R . .
C32 C -0.2697(3) 0.7004(6) 0.0723(3) 0.0470(16) Uani 1 1 d . . .
C33 C -0.2990(4) 0.7948(7) 0.0272(4) 0.078(2) Uani 1 1 d . . .
H33A H -0.3508 0.8039 0.0199 0.117 Uiso 1 1 calc R . .
H33B H -0.2913 0.7748 -0.0106 0.117 Uiso 1 1 calc R . .
H33C H -0.2741 0.8673 0.0428 0.117 Uiso 1 1 calc R . .
C34 C -0.3183(4) 0.5929(7) 0.0485(4) 0.085(3) Uani 1 1 d . . .
H34A H -0.3006 0.5280 0.0763 0.127 Uiso 1 1 calc R . .
H34B H -0.3170 0.5719 0.0086 0.127 Uiso 1 1 calc R . .
H34C H -0.3680 0.6109 0.0457 0.127 Uiso 1 1 calc R . .
C35 C -0.2739(4) 0.7260(11) 0.1335(4) 0.118(4) Uani 1 1 d . . .
H35A H -0.2551 0.8037 0.1459 0.177 Uiso 1 1 calc R . .
H35B H -0.2451 0.6693 0.1625 0.177 Uiso 1 1 calc R . .
H35C H -0.3242 0.7217 0.1319 0.177 Uiso 1 1 calc R . .
C36 C -0.0105(3) 0.8396(5) 0.2480(3) 0.0384(15) Uani 1 1 d . . .
H36 H -0.0524 0.8863 0.2328 0.046 Uiso 1 1 calc R . .
C37 C 0.0122(3) 0.8094(5) 0.3085(3) 0.0369(14) Uani 1 1 d . . .
C38 C 0.0727(3) 0.7381(5) 0.3282(2) 0.0379(14) Uani 1 1 d . . .
H38 H 0.0888 0.7141 0.3691 0.045 Uiso 1 1 calc R . .
C39 C -0.0249(3) 0.8555(5) 0.3520(3) 0.0441(16) Uani 1 1 d . . .
C40 C -0.0144(6) 0.7772(9) 0.4056(4) 0.121(4) Uani 1 1 d . . .
H40A H 0.0364 0.7781 0.4312 0.182 Uiso 1 1 calc R . .
H40B H -0.0285 0.6982 0.3916 0.182 Uiso 1 1 calc R . .
H40C H -0.0443 0.8044 0.4288 0.182 Uiso 1 1 calc R . .
C41 C -0.1054(4) 0.8664(9) 0.3207(4) 0.098(3) Uani 1 1 d . . .
H41A H -0.1288 0.8837 0.3505 0.147 Uiso 1 1 calc R . .
H41B H -0.1244 0.7936 0.3003 0.147 Uiso 1 1 calc R . .
H41C H -0.1152 0.9289 0.2910 0.147 Uiso 1 1 calc R . .
C42 C 0.0040(6) 0.9738(8) 0.3718(5) 0.138(5) Uani 1 1 d . . .
H42A H 0.0514 0.9675 0.4032 0.206 Uiso 1 1 calc R . .
H42B H -0.0291 1.0152 0.3877 0.206 Uiso 1 1 calc R . .
H42C H 0.0088 1.0162 0.3373 0.206 Uiso 1 1 calc R . .
C43 C 0.1281(3) 0.4671(5) 0.3741(2) 0.0367(14) Uani 1 1 d . . .
H43 H 0.1398 0.5206 0.4066 0.044 Uiso 1 1 calc R . .
C44 C 0.0962(3) 0.3629(5) 0.3800(2) 0.0366(14) Uani 1 1 d . . .
C45 C 0.0823(3) 0.2852(5) 0.3326(2) 0.0346(14) Uani 1 1 d . . .
H45 H 0.0605 0.2133 0.3357 0.041 Uiso 1 1 calc R . .
C46 C 0.0758(3) 0.3320(5) 0.4355(2) 0.0442(16) Uani 1 1 d . . .
C47 C 0.1195(3) 0.2240(5) 0.4657(3) 0.0515(17) Uani 1 1 d . . .
H47A H 0.1044 0.1576 0.4385 0.077 Uiso 1 1 calc R . .
H47B H 0.1107 0.2076 0.5034 0.077 Uiso 1 1 calc R . .
H47C H 0.1710 0.2384 0.4741 0.077 Uiso 1 1 calc R . .
C48 C 0.0934(4) 0.4286(6) 0.4829(3) 0.0570(18) Uani 1 1 d . . .
H48A H 0.1451 0.4460 0.4957 0.085 Uiso 1 1 calc R . .
H48B H 0.0806 0.4035 0.5177 0.085 Uiso 1 1 calc R . .
H48C H 0.0658 0.4980 0.4654 0.085 Uiso 1 1 calc R . .
C49 C -0.0043(3) 0.3060(6) 0.4174(3) 0.0587(19) Uani 1 1 d . . .
H49A H -0.0320 0.3755 0.4003 0.088 Uiso 1 1 calc R . .
H49B H -0.0159 0.2816 0.4530 0.088 Uiso 1 1 calc R . .
H49C H -0.0168 0.2441 0.3873 0.088 Uiso 1 1 calc R . .
C50 C 0.0771(3) 0.2888(5) 0.0727(3) 0.0430(16) Uani 1 1 d . . .
H50A H 0.1119 0.3347 0.0599 0.052 Uiso 1 1 calc R . .
H50B H 0.0319 0.2831 0.0380 0.052 Uiso 1 1 calc R . .
C51 C 0.1069(3) 0.1703(5) 0.0896(3) 0.0495(16) Uani 1 1 d . . .
H51A H 0.0730 0.1248 0.1036 0.059 Uiso 1 1 calc R . .
H51B H 0.1531 0.1758 0.1234 0.059 Uiso 1 1 calc R . .
C52 C 0.1195(4) 0.1080(6) 0.0369(3) 0.067(2) Uani 1 1 d . . .
H52A H 0.0739 0.1077 0.0023 0.081 Uiso 1 1 calc R . .
H52B H 0.1555 0.1519 0.0246 0.081 Uiso 1 1 calc R . .
C53 C 0.1451(5) -0.0129(6) 0.0503(3) 0.075(2) Uani 1 1 d . . .
H53A H 0.1097 -0.0569 0.0632 0.090 Uiso 1 1 calc R . .
H53B H 0.1914 -0.0130 0.0841 0.090 Uiso 1 1 calc R . .
C54 C 0.1555(6) -0.0731(7) -0.0036(4) 0.115(4) Uani 1 1 d . . .
H54A H 0.1096 -0.0743 -0.0370 0.173 Uiso 1 1 calc R . .
H54B H 0.1720 -0.1524 0.0074 0.173 Uiso 1 1 calc R . .
H54C H 0.1915 -0.0312 -0.0159 0.173 Uiso 1 1 calc R . .
C55 C 0.6015(4) 0.0289(6) 0.2293(4) 0.081(2) Uani 1 1 d . . .
C56 C 0.5598(3) 0.0219(6) 0.2668(3) 0.0520(17) Uani 1 1 d . . .
H56A H 0.5223 0.0815 0.2554 0.078 Uiso 1 1 calc R . .
H56B H 0.5906 0.0339 0.3087 0.078 Uiso 1 1 calc R . .
H56C H 0.5373 -0.0545 0.2628 0.078 Uiso 1 1 calc R . .
N1 N 0.6327(6) 0.0337(8) 0.1955(6) 0.161(4) Uani 1 1 d . . .
O1 O 0.06242(18) 0.3489(3) 0.12139(16) 0.0393(10) Uani 1 1 d . . .
O2 O 0.1486(2) 0.4447(4) 0.22707(17) 0.0454(11) Uani 1 1 d D . .
O3 O 0.12125(18) 0.7036(3) 0.19253(16) 0.0373(10) Uani 1 1 d . . .
O4 O 0.0232(2) 0.6124(4) 0.09178(17) 0.0444(11) Uani 1 1 d D . .
H2 H 0.124(3) 0.404(4) 0.1966(18) 0.053 Uiso 1 1 d D . .
H4 H 0.056(2) 0.645(5) 0.1207(19) 0.053 Uiso 1 1 d D . .

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
C1 0.028(3) 0.042(4) 0.027(3) -0.002(3) 0.012(3) 0.001(3)
C2 0.029(3) 0.035(3) 0.025(3) -0.001(3) 0.007(3) 0.002(3)
C3 0.026(3) 0.035(3) 0.038(3) 0.006(3) 0.003(3) 0.005(3)
C4 0.027(3) 0.031(3) 0.031(3) 0.007(3) 0.003(3) 0.007(3)
C5 0.028(3) 0.041(4) 0.031(3) 0.008(3) 0.010(3) 0.007(3)
C6 0.023(3) 0.034(3) 0.033(3) 0.007(3) 0.002(2) 0.002(2)
C7 0.030(3) 0.045(4) 0.035(3) 0.001(3) 0.004(3) -0.002(3)
C8 0.030(3) 0.033(3) 0.032(3) 0.004(3) 0.006(3) -0.008(3)
C9 0.033(3) 0.030(3) 0.044(4) 0.002(3) 0.016(3) -0.006(3)
C10 0.042(4) 0.049(4) 0.055(4) 0.006(3) 0.021(3) -0.006(3)
C11 0.040(4) 0.058(4) 0.049(4) 0.010(3) 0.018(3) -0.004(3)
C12 0.054(4) 0.059(5) 0.056(4) -0.004(4) 0.025(3) -0.003(3)
C13 0.118(7) 0.100(7) 0.057(5) 0.008(5) 0.033(5) 0.050(6)
C14 0.118(7) 0.098(7) 0.095(6) 0.019(6) 0.050(6) 0.065(6)
C15 0.032(3) 0.033(3) 0.040(3) 0.005(3) 0.015(3) 0.001(3)
C16 0.041(3) 0.039(4) 0.037(3) 0.017(3) 0.017(3) 0.011(3)
C17 0.041(4) 0.040(4) 0.027(3) 0.017(3) 0.012(3) 0.006(3)
C18 0.032(3) 0.051(4) 0.030(3) 0.018(3) 0.014(3) 0.016(3)
C19 0.032(4) 0.044(4) 0.026(3) 0.010(3) 0.006(3) 0.008(3)
C20 0.042(4) 0.052(4) 0.027(3) 0.005(3) 0.009(3) 0.008(3)
C21 0.033(3) 0.042(4) 0.025(3) -0.003(3) 0.006(3) 0.001(3)
C22 0.035(3) 0.038(4) 0.030(3) 0.000(3) 0.006(3) 0.003(3)
C23 0.025(3) 0.034(3) 0.034(3) -0.005(3) 0.007(3) 0.002(3)
C24 0.043(4) 0.039(4) 0.024(3) 0.002(3) 0.009(3) -0.001(3)
C25 0.040(4) 0.045(4) 0.050(4) 0.004(3) 0.018(3) 0.002(3)
C26 0.075(6) 0.066(6) 0.232(12) 0.042(7) 0.074(7) 0.001(5)
C27 0.103(7) 0.314(17) 0.102(7) -0.105(9) 0.084(6) -0.110(9)
C28 0.041(4) 0.113(7) 0.085(6) 0.032(5) 0.018(4) -0.005(4)
C29 0.030(3) 0.048(4) 0.030(3) 0.010(3) 0.005(3) 0.006(3)
C30 0.041(4) 0.045(4) 0.034(3) 0.016(3) 0.012(3) 0.007(3)
C31 0.053(4) 0.043(4) 0.035(3) 0.019(3) 0.020(3) 0.019(3)
C32 0.035(4) 0.054(4) 0.055(4) 0.003(3) 0.020(3) 0.011(3)
C33 0.050(4) 0.070(6) 0.107(6) 0.033(5) 0.016(4) 0.021(4)
C34 0.056(5) 0.070(6) 0.133(7) 0.013(5) 0.039(5) 0.004(4)
C35 0.057(5) 0.214(12) 0.092(7) -0.025(7) 0.036(5) 0.019(6)
C36 0.036(3) 0.031(3) 0.046(4) 0.011(3) 0.011(3) 0.002(3)
C37 0.037(3) 0.034(3) 0.042(4) 0.010(3) 0.015(3) 0.000(3)
C38 0.047(4) 0.035(4) 0.031(3) 0.002(3) 0.012(3) -0.008(3)
C39 0.042(4) 0.041(4) 0.050(4) -0.002(3) 0.018(3) -0.005(3)
C40 0.165(9) 0.144(9) 0.098(7) 0.060(7) 0.102(7) 0.082(8)
C41 0.076(6) 0.150(9) 0.081(6) -0.003(6) 0.044(5) 0.037(6)
C42 0.156(9) 0.118(8) 0.194(11) -0.112(8) 0.132(9) -0.077(7)
C43 0.037(3) 0.036(4) 0.034(3) 0.001(3) 0.007(3) 0.002(3)
C44 0.035(3) 0.037(4) 0.035(3) 0.010(3) 0.009(3) 0.001(3)
C45 0.037(3) 0.030(3) 0.034(3) -0.001(3) 0.010(3) 0.000(3)
C46 0.058(4) 0.043(4) 0.029(3) 0.000(3) 0.011(3) -0.009(3)
C47 0.072(5) 0.050(4) 0.036(3) 0.001(3) 0.022(3) -0.005(3)
C48 0.087(5) 0.049(4) 0.040(4) 0.001(3) 0.028(4) -0.009(4)
C49 0.061(5) 0.077(5) 0.046(4) -0.001(4) 0.028(3) -0.007(4)
C50 0.041(4) 0.056(4) 0.038(3) 0.002(3) 0.020(3) 0.013(3)
C51 0.058(4) 0.049(4) 0.048(4) -0.003(3) 0.027(3) 0.003(3)
C52 0.093(6) 0.070(5) 0.055(4) 0.003(4) 0.046(4) 0.015(4)
C53 0.118(7) 0.049(5) 0.072(5) 0.004(4) 0.049(5) 0.015(4)
C54 0.225(11) 0.067(6) 0.099(7) -0.021(5) 0.113(8) -0.003(7)
C55 0.092(6) 0.050(5) 0.128(7) 0.015(5) 0.071(6) 0.000(4)
C56 0.054(4) 0.048(4) 0.053(4) 0.001(3) 0.016(3) 0.005(3)
N1 0.214(10) 0.095(7) 0.254(12) 0.019(7) 0.184(10) 0.001(7)
O1 0.038(2) 0.044(2) 0.039(2) 0.001(2) 0.0172(19) 0.0026(18)
O2 0.049(3) 0.051(3) 0.041(3) 0.000(2) 0.021(2) -0.010(2)
O3 0.031(2) 0.042(2) 0.042(2) 0.0052(19) 0.0169(18) -0.0003(18)
O4 0.034(3) 0.058(3) 0.042(3) 0.000(2) 0.0134(19) 0.006(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
C1 C21 1.381(7) . ?
C1 O1 1.399(6) . ?
C1 C2 1.400(7) . ?
C2 C24 1.380(7) . ?
C2 C3 1.512(7) . ?
C3 C4 1.514(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C45 1.394(7) . ?
C4 C5 1.394(7) . ?
C5 O2 1.371(6) . ?
C5 C6 1.395(8) . ?
C6 C43 1.399(7) . ?
C6 C7 1.509(8) . ?
C7 C8 1.523(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C38 1.378(7) . ?
C8 C9 1.405(7) . ?
C9 O3 1.383(6) . ?
C9 C15 1.395(7) . ?
C10 O3 1.453(6) . ?
C10 C11 1.493(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.527(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.471(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.523(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C36 1.374(7) . ?
C15 C16 1.522(7) . ?
C16 C17 1.528(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C31 1.395(8) . ?
C17 C18 1.398(8) . ?
C18 O4 1.367(6) . ?
C18 C19 1.392(8) . ?
C19 C29 1.386(7) . ?
C19 C20 1.510(8) . ?
C20 C21 1.525(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.397(7) . ?
C22 C23 1.383(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(7) . ?
C23 C25 1.535(8) . ?
C24 H24 0.9500 . ?
C25 C27 1.477(9) . ?
C25 C28 1.501(8) . ?
C25 C26 1.530(10) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.368(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.406(8) . ?
C30 C32 1.535(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.499(9) . ?
C32 C35 1.500(10) . ?
C32 C34 1.555(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.387(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(8) . ?
C37 C39 1.541(8) . ?
C38 H38 0.9500 . ?
C39 C42 1.497(10) . ?
C39 C40 1.512(9) . ?
C39 C41 1.513(9) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.388(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.389(7) . ?
C44 C46 1.534(8) . ?
C45 H45 0.9500 . ?
C46 C49 1.520(8) . ?
C46 C48 1.535(8) . ?
C46 C47 1.549(8) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 O1 1.450(6) . ?
C50 C51 1.492(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.527(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.486(9) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.520(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 N1 1.158(10) . ?
C55 C56 1.395(10) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
O2 H2 0.86(2) . ?
O4 H4 0.85(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 C1 O1 120.2(5) . . ?
C21 C1 C2 121.6(5) . . ?
O1 C1 C2 118.1(4) . . ?
C24 C2 C1 118.0(5) . . ?
C24 C2 C3 119.2(5) . . ?
C1 C2 C3 122.7(5) . . ?
C2 C3 C4 111.7(4) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C45 C4 C5 118.1(5) . . ?
C45 C4 C3 119.9(5) . . ?
C5 C4 C3 122.0(5) . . ?
O2 C5 C4 122.5(5) . . ?
O2 C5 C6 116.4(5) . . ?
C4 C5 C6 121.1(5) . . ?
C5 C6 C43 118.4(5) . . ?
C5 C6 C7 120.9(5) . . ?
C43 C6 C7 120.7(5) . . ?
C6 C7 C8 110.9(4) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C38 C8 C9 117.3(5) . . ?
C38 C8 C7 120.7(5) . . ?
C9 C8 C7 121.8(5) . . ?
O3 C9 C15 118.3(5) . . ?
O3 C9 C8 120.4(5) . . ?
C15 C9 C8 121.2(5) . . ?
O3 C10 C11 108.1(5) . . ?
O3 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
O3 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C10 C11 C12 111.8(5) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C11 115.0(6) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 C14 112.8(6) . . ?
C12 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
C12 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C36 C15 C9 118.0(5) . . ?
C36 C15 C16 120.5(5) . . ?
C9 C15 C16 121.2(5) . . ?
C15 C16 C17 111.2(4) . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C31 C17 C18 118.0(5) . . ?
C31 C17 C16 119.5(5) . . ?
C18 C17 C16 122.4(5) . . ?
O4 C18 C19 117.8(5) . . ?
O4 C18 C17 121.8(5) . . ?
C19 C18 C17 120.4(5) . . ?
C29 C19 C18 118.8(5) . . ?
C29 C19 C20 121.1(5) . . ?
C18 C19 C20 120.0(5) . . ?
C19 C20 C21 110.5(4) . . ?
C19 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C1 C21 C22 117.3(5) . . ?
C1 C21 C20 123.0(5) . . ?
C22 C21 C20 119.5(5) . . ?
C23 C22 C21 123.7(5) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C22 C23 C24 116.2(5) . . ?
C22 C23 C25 122.9(5) . . ?
C24 C23 C25 120.9(5) . . ?
C2 C24 C23 123.1(5) . . ?
C2 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C27 C25 C28 109.8(7) . . ?
C27 C25 C26 110.9(8) . . ?
C28 C25 C26 104.0(6) . . ?
C27 C25 C23 109.9(5) . . ?
C28 C25 C23 112.8(5) . . ?
C26 C25 C23 109.4(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C19 123.7(6) . . ?
C30 C29 H29 118.1 . . ?
C19 C29 H29 118.1 . . ?
C29 C30 C31 116.0(5) . . ?
C29 C30 C32 123.9(6) . . ?
C31 C30 C32 120.0(6) . . ?
C17 C31 C30 123.0(6) . . ?
C17 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
C33 C32 C35 113.9(7) . . ?
C33 C32 C30 109.4(5) . . ?
C35 C32 C30 109.8(5) . . ?
C33 C32 C34 106.5(6) . . ?
C35 C32 C34 106.3(6) . . ?
C30 C32 C34 110.9(5) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C15 C36 C37 123.6(5) . . ?
C15 C36 H36 118.2 . . ?
C37 C36 H36 118.2 . . ?
C36 C37 C38 116.0(5) . . ?
C36 C37 C39 122.3(5) . . ?
C38 C37 C39 121.7(5) . . ?
C8 C38 C37 123.8(5) . . ?
C8 C38 H38 118.1 . . ?
C37 C38 H38 118.1 . . ?
C42 C39 C40 111.0(8) . . ?
C42 C39 C41 107.6(7) . . ?
C40 C39 C41 106.6(6) . . ?
C42 C39 C37 107.9(5) . . ?
C40 C39 C37 112.7(5) . . ?
C41 C39 C37 110.9(5) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C6 122.3(5) . . ?
C44 C43 H43 118.9 . . ?
C6 C43 H43 118.9 . . ?
C43 C44 C45 117.2(5) . . ?
C43 C44 C46 123.0(5) . . ?
C45 C44 C46 119.8(5) . . ?
C44 C45 C4 122.9(5) . . ?
C44 C45 H45 118.6 . . ?
C4 C45 H45 118.6 . . ?
C49 C46 C44 110.5(5) . . ?
C49 C46 C48 108.0(5) . . ?
C44 C46 C48 112.9(5) . . ?
C49 C46 C47 109.5(5) . . ?
C44 C46 C47 108.4(5) . . ?
C48 C46 C47 107.4(5) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O1 C50 C51 113.3(5) . . ?
O1 C50 H50A 108.9 . . ?
C51 C50 H50A 108.9 . . ?
O1 C50 H50B 108.9 . . ?
C51 C50 H50B 108.9 . . ?
H50A C50 H50B 107.7 . . ?
C50 C51 C52 111.9(5) . . ?
C50 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
C50 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C53 C52 C51 114.0(6) . . ?
C53 C52 H52A 108.7 . . ?
C51 C52 H52A 108.7 . . ?
C53 C52 H52B 108.7 . . ?
C51 C52 H52B 108.7 . . ?
H52A C52 H52B 107.6 . . ?
C52 C53 C54 112.6(6) . . ?
C52 C53 H53A 109.1 . . ?
C54 C53 H53A 109.1 . . ?
C52 C53 H53B 109.1 . . ?
C54 C53 H53B 109.1 . . ?
H53A C53 H53B 107.8 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1 C55 C56 176.2(11) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C1 O1 C50 114.4(4) . . ?
C5 O2 H2 109(4) . . ?
C9 O3 C10 115.3(4) . . ?
C18 O4 H4 115(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 C1 C2 C24 5.1(8) . . . . ?
O1 C1 C2 C24 -179.0(5) . . . . ?
C21 C1 C2 C3 -169.8(5) . . . . ?
O1 C1 C2 C3 6.0(8) . . . . ?
C24 C2 C3 C4 -82.5(6) . . . . ?
C1 C2 C3 C4 92.4(6) . . . . ?
C2 C3 C4 C45 93.8(6) . . . . ?
C2 C3 C4 C5 -83.5(6) . . . . ?
C45 C4 C5 O2 179.4(5) . . . . ?
C3 C4 C5 O2 -3.2(8) . . . . ?
C45 C4 C5 C6 -0.2(7) . . . . ?
C3 C4 C5 C6 177.2(5) . . . . ?
O2 C5 C6 C43 -177.4(4) . . . . ?
C4 C5 C6 C43 2.2(7) . . . . ?
O2 C5 C6 C7 5.1(7) . . . . ?
C4 C5 C6 C7 -175.3(5) . . . . ?
C5 C6 C7 C8 93.8(6) . . . . ?
C43 C6 C7 C8 -83.6(6) . . . . ?
C6 C7 C8 C38 71.3(6) . . . . ?
C6 C7 C8 C9 -103.6(6) . . . . ?
C38 C8 C9 O3 179.8(5) . . . . ?
C7 C8 C9 O3 -5.1(7) . . . . ?
C38 C8 C9 C15 -3.0(8) . . . . ?
C7 C8 C9 C15 172.2(5) . . . . ?
O3 C10 C11 C12 -62.2(6) . . . . ?
C10 C11 C12 C13 166.6(6) . . . . ?
C11 C12 C13 C14 -178.4(7) . . . . ?
O3 C9 C15 C36 -179.7(5) . . . . ?
C8 C9 C15 C36 3.0(8) . . . . ?
O3 C9 C15 C16 6.9(7) . . . . ?
C8 C9 C15 C16 -170.4(5) . . . . ?
C36 C15 C16 C17 -83.1(6) . . . . ?
C9 C15 C16 C17 90.1(6) . . . . ?
C15 C16 C17 C31 91.3(6) . . . . ?
C15 C16 C17 C18 -85.6(6) . . . . ?
C31 C17 C18 O4 178.2(5) . . . . ?
C16 C17 C18 O4 -4.9(8) . . . . ?
C31 C17 C18 C19 1.1(7) . . . . ?
C16 C17 C18 C19 178.0(5) . . . . ?
O4 C18 C19 C29 -176.3(5) . . . . ?
C17 C18 C19 C29 0.9(8) . . . . ?
O4 C18 C19 C20 7.5(7) . . . . ?
C17 C18 C19 C20 -175.3(5) . . . . ?
C29 C19 C20 C21 -82.6(6) . . . . ?
C18 C19 C20 C21 93.4(6) . . . . ?
O1 C1 C21 C22 179.0(5) . . . . ?
C2 C1 C21 C22 -5.2(8) . . . . ?
O1 C1 C21 C20 -5.6(8) . . . . ?
C2 C1 C21 C20 170.2(5) . . . . ?
C19 C20 C21 C1 -104.5(6) . . . . ?
C19 C20 C21 C22 70.8(6) . . . . ?
C1 C21 C22 C23 1.9(8) . . . . ?
C20 C21 C22 C23 -173.6(5) . . . . ?
C21 C22 C23 C24 1.3(8) . . . . ?
C21 C22 C23 C25 -179.1(5) . . . . ?
C1 C2 C24 C23 -1.6(8) . . . . ?
C3 C2 C24 C23 173.5(5) . . . . ?
C22 C23 C24 C2 -1.4(8) . . . . ?
C25 C23 C24 C2 179.0(5) . . . . ?
C22 C23 C25 C27 -116.6(8) . . . . ?
C24 C23 C25 C27 62.9(9) . . . . ?
C22 C23 C25 C28 6.2(8) . . . . ?
C24 C23 C25 C28 -174.2(6) . . . . ?
C22 C23 C25 C26 121.5(7) . . . . ?
C24 C23 C25 C26 -59.0(8) . . . . ?
C18 C19 C29 C30 -2.7(8) . . . . ?
C20 C19 C29 C30 173.4(5) . . . . ?
C19 C29 C30 C31 2.3(8) . . . . ?
C19 C29 C30 C32 -178.2(5) . . . . ?
C18 C17 C31 C30 -1.4(8) . . . . ?
C16 C17 C31 C30 -178.4(5) . . . . ?
C29 C30 C31 C17 -0.2(8) . . . . ?
C32 C30 C31 C17 -179.7(5) . . . . ?
C29 C30 C32 C33 -109.4(7) . . . . ?
C31 C30 C32 C33 70.1(7) . . . . ?
C29 C30 C32 C35 124.9(7) . . . . ?
C31 C30 C32 C35 -55.6(8) . . . . ?
C29 C30 C32 C34 7.8(8) . . . . ?
C31 C30 C32 C34 -172.7(6) . . . . ?
C9 C15 C36 C37 -0.5(8) . . . . ?
C16 C15 C36 C37 172.9(5) . . . . ?
C15 C36 C37 C38 -1.8(8) . . . . ?
C15 C36 C37 C39 175.9(5) . . . . ?
C9 C8 C38 C37 0.5(8) . . . . ?
C7 C8 C38 C37 -174.7(5) . . . . ?
C36 C37 C38 C8 1.8(8) . . . . ?
C39 C37 C38 C8 -175.9(5) . . . . ?
C36 C37 C39 C42 -81.7(8) . . . . ?
C38 C37 C39 C42 95.9(8) . . . . ?
C36 C37 C39 C40 155.5(7) . . . . ?
C38 C37 C39 C40 -27.0(9) . . . . ?
C36 C37 C39 C41 36.0(8) . . . . ?
C38 C37 C39 C41 -146.4(6) . . . . ?
C5 C6 C43 C44 -3.3(8) . . . . ?
C7 C6 C43 C44 174.2(5) . . . . ?
C6 C43 C44 C45 2.3(8) . . . . ?
C6 C43 C44 C46 -177.3(5) . . . . ?
C43 C44 C45 C4 -0.1(8) . . . . ?
C46 C44 C45 C4 179.4(5) . . . . ?
C5 C4 C45 C44 -0.9(8) . . . . ?
C3 C4 C45 C44 -178.3(5) . . . . ?
C43 C44 C46 C49 122.0(6) . . . . ?
C45 C44 C46 C49 -57.6(7) . . . . ?
C43 C44 C46 C48 0.8(8) . . . . ?
C45 C44 C46 C48 -178.7(5) . . . . ?
C43 C44 C46 C47 -118.1(6) . . . . ?
C45 C44 C46 C47 62.4(6) . . . . ?
O1 C50 C51 C52 178.2(5) . . . . ?
C50 C51 C52 C53 -176.5(6) . . . . ?
C51 C52 C53 C54 178.8(7) . . . . ?
C21 C1 O1 C50 -77.8(6) . . . . ?
C2 C1 O1 C50 106.2(5) . . . . ?
C51 C50 O1 C1 -76.3(6) . . . . ?
C15 C9 O3 C10 92.6(6) . . . . ?
C8 C9 O3 C10 -90.1(6) . . . . ?
C11 C10 O3 C9 -176.8(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O1 0.86(2) 1.89(2) 2.735(5) 166(6) .
O4 H4 O3 0.85(2) 1.88(2) 2.723(5) 171(6) .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        22.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.056