# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2007

data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440

_publ_contact_author_name        'Paula M. Marcos'
_publ_contact_author_address     
;
FCUL, Dep Qu\'imica / CCMM,
Universidade de Lisboa
Edif\'icio C8, 1749-016 Lisboa
Lisbon
1749-016 Lisboa
PORTUGAL
;

_publ_contact_author_email       PMMARCOS@FC.UL.PT

_publ_section_title              
;
X-ray crystal structure, complexation and transport properties
towards transition and heavy metal cations of
p-tert-butyldihomooxacalix[4]arene tetraketone derivatives
;
loop_
_publ_author_name
P.M.Marcos
S.Felix
J.R.Ascenso
M.A.P.Segurado
P.Thuery
;
S.Michel
;
B.Mellah,
V.Hubscher-Bruder
F.Arnaud-Neu

data_fa1
_database_code_depnum_ccdc_archive 'CCDC 656213'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C71 H101 N O9'
_chemical_formula_weight         1112.53

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

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                   19.0372(7)
_cell_length_b                   22.9422(7)
_cell_length_c                   30.2456(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13209.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    142525
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4848
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_special_details           'crystal-to-detector distance 50 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'one \f and three \w scans with 2\% steps'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            142525
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.68
_reflns_number_total             12490
_reflns_number_gt                7422
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms were introduced at calculated
positions and were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the
parent atom.
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^)+(0.0932P)^2^+15.1976P] 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         12490
_refine_ls_number_parameters     755
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.2175
_refine_ls_wR_factor_gt          0.1960
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.71324(12) 0.40865(10) 0.61642(7) 0.0321(6) Uani 1 1 d . . .
O2 O 0.74872(14) 0.46651(12) 0.54132(8) 0.0459(7) Uani 1 1 d . . .
O3 O 0.84480(12) 0.45917(10) 0.64670(7) 0.0329(6) Uani 1 1 d . . .
O4 O 0.91828(13) 0.46395(11) 0.57187(8) 0.0420(6) Uani 1 1 d . . .
O5 O 0.87910(11) 0.31258(10) 0.65713(7) 0.0321(6) Uani 1 1 d . . .
O6 O 0.94711(13) 0.24277(12) 0.59870(9) 0.0461(7) Uani 1 1 d . . .
O7 O 0.76121(12) 0.23355(9) 0.59968(7) 0.0299(6) Uani 1 1 d . . .
O8 O 0.72204(13) 0.20846(11) 0.51555(8) 0.0384(6) Uani 1 1 d . . .
O9 O 0.61194(12) 0.31234(9) 0.61106(7) 0.0308(5) Uani 1 1 d . . .
C1 C 0.59092(18) 0.41080(14) 0.59053(11) 0.0297(8) Uani 1 1 d . . .
C2 C 0.64978(18) 0.43663(15) 0.60861(11) 0.0299(8) Uani 1 1 d . . .
C3 C 0.64799(18) 0.49378(15) 0.62444(11) 0.0301(8) Uani 1 1 d . . .
C4 C 0.58558(18) 0.52537(15) 0.62045(11) 0.0321(8) Uani 1 1 d . . .
H4 H 0.5838 0.5631 0.6316 0.038 Uiso 1 1 calc R . .
C5 C 0.52607(18) 0.50219(15) 0.60042(11) 0.0327(8) Uani 1 1 d . . .
C6 C 0.53033(18) 0.44455(15) 0.58620(11) 0.0335(8) Uani 1 1 d . . .
H6 H 0.4909 0.4278 0.5732 0.040 Uiso 1 1 calc R . .
C7 C 0.45797(19) 0.53774(16) 0.59260(13) 0.0403(9) Uani 1 1 d . . .
C8 C 0.4635(2) 0.59830(17) 0.61192(14) 0.0506(11) Uani 1 1 d . . .
H8A H 0.4207 0.6192 0.6065 0.076 Uiso 1 1 calc R . .
H8B H 0.5020 0.6186 0.5983 0.076 Uiso 1 1 calc R . .
H8C H 0.4715 0.5956 0.6432 0.076 Uiso 1 1 calc R . .
C9 C 0.4464(2) 0.5445(2) 0.54245(14) 0.0570(12) Uani 1 1 d . . .
H9A H 0.4028 0.5644 0.5372 0.085 Uiso 1 1 calc R . .
H9B H 0.4448 0.5067 0.5289 0.085 Uiso 1 1 calc R . .
H9C H 0.4843 0.5667 0.5300 0.085 Uiso 1 1 calc R . .
C10 C 0.3958(2) 0.5059(2) 0.61342(18) 0.0675(14) Uani 1 1 d . . .
H10A H 0.4043 0.5006 0.6444 0.101 Uiso 1 1 calc R . .
H10B H 0.3901 0.4686 0.5995 0.101 Uiso 1 1 calc R . .
H10C H 0.3539 0.5286 0.6094 0.101 Uiso 1 1 calc R . .
C11 C 0.74878(18) 0.37859(15) 0.58195(11) 0.0323(8) Uani 1 1 d . . .
H11A H 0.7212 0.3448 0.5735 0.039 Uiso 1 1 calc R . .
H11B H 0.7935 0.3647 0.5931 0.039 Uiso 1 1 calc R . .
C12 C 0.76159(18) 0.41518(16) 0.54171(12) 0.0349(9) Uani 1 1 d . . .
C13 C 0.79340(19) 0.38508(16) 0.49995(12) 0.0369(9) Uani 1 1 d . . .
C14 C 0.7351(2) 0.34850(19) 0.47834(14) 0.0494(11) Uani 1 1 d . . .
H14A H 0.7516 0.3333 0.4507 0.074 Uiso 1 1 calc R . .
H14B H 0.6947 0.3725 0.4733 0.074 Uiso 1 1 calc R . .
H14C H 0.7227 0.3168 0.4976 0.074 Uiso 1 1 calc R . .
C15 C 0.85384(19) 0.34495(17) 0.51348(13) 0.0430(10) Uani 1 1 d . . .
H15A H 0.8730 0.3265 0.4877 0.064 Uiso 1 1 calc R . .
H15B H 0.8367 0.3157 0.5335 0.064 Uiso 1 1 calc R . .
H15C H 0.8898 0.3674 0.5278 0.064 Uiso 1 1 calc R . .
C16 C 0.8188(2) 0.43176(18) 0.46805(13) 0.0480(10) Uani 1 1 d . . .
H16A H 0.8536 0.4554 0.4823 0.072 Uiso 1 1 calc R . .
H16B H 0.7798 0.4557 0.4593 0.072 Uiso 1 1 calc R . .
H16C H 0.8389 0.4136 0.4424 0.072 Uiso 1 1 calc R . .
C17 C 0.71426(18) 0.52180(15) 0.64228(11) 0.0324(8) Uani 1 1 d . . .
H17A H 0.7050 0.5628 0.6476 0.039 Uiso 1 1 calc R . .
H17B H 0.7505 0.5194 0.6198 0.039 Uiso 1 1 calc R . .
C18 C 0.74214(18) 0.49487(14) 0.68459(11) 0.0307(8) Uani 1 1 d . . .
C19 C 0.80567(18) 0.46444(14) 0.68525(11) 0.0303(8) Uani 1 1 d . . .
C20 C 0.83115(18) 0.43909(15) 0.72420(12) 0.0324(8) Uani 1 1 d . . .
C21 C 0.79099(18) 0.44593(14) 0.76223(11) 0.0309(8) Uani 1 1 d . . .
H21 H 0.8072 0.4291 0.7883 0.037 Uiso 1 1 calc R . .
C22 C 0.72831(19) 0.47634(15) 0.76364(11) 0.0334(8) Uani 1 1 d . . .
C23 C 0.70520(19) 0.49990(15) 0.72387(12) 0.0329(8) Uani 1 1 d . . .
H23 H 0.6628 0.5200 0.7236 0.039 Uiso 1 1 calc R . .
C24 C 0.6882(2) 0.48769(17) 0.80737(12) 0.0420(10) Uani 1 1 d . . .
C25 C 0.7116(3) 0.54846(18) 0.82361(14) 0.0663(14) Uani 1 1 d . . .
H25A H 0.7018 0.5769 0.8012 0.099 Uiso 1 1 calc R . .
H25B H 0.7611 0.5480 0.8296 0.099 Uiso 1 1 calc R . .
H25C H 0.6865 0.5583 0.8501 0.099 Uiso 1 1 calc R . .
C26 C 0.7068(2) 0.44371(18) 0.84329(13) 0.0499(11) Uani 1 1 d . . .
H26A H 0.6782 0.4506 0.8689 0.075 Uiso 1 1 calc R . .
H26B H 0.7555 0.4479 0.8511 0.075 Uiso 1 1 calc R . .
H26C H 0.6986 0.4049 0.8325 0.075 Uiso 1 1 calc R . .
C27 C 0.6095(2) 0.4888(2) 0.80077(15) 0.0664(13) Uani 1 1 d . . .
H27A H 0.5869 0.4966 0.8285 0.100 Uiso 1 1 calc R . .
H27B H 0.5941 0.4517 0.7897 0.100 Uiso 1 1 calc R . .
H27C H 0.5976 0.5188 0.7799 0.100 Uiso 1 1 calc R . .
C28 C 0.88954(19) 0.50817(16) 0.63995(11) 0.0350(9) Uani 1 1 d . . .
H28A H 0.9289 0.5063 0.6603 0.042 Uiso 1 1 calc R . .
H28B H 0.8638 0.5438 0.6458 0.042 Uiso 1 1 calc R . .
C29 C 0.91600(17) 0.50860(16) 0.59328(12) 0.0312(8) Uani 1 1 d . . .
C30 C 0.93867(19) 0.56712(15) 0.57457(12) 0.0363(9) Uani 1 1 d . . .
C31 C 0.9767(3) 0.5591(2) 0.53116(15) 0.0640(13) Uani 1 1 d . . .
H31A H 0.9926 0.5962 0.5206 0.096 Uiso 1 1 calc R . .
H31B H 0.9452 0.5421 0.5099 0.096 Uiso 1 1 calc R . .
H31C H 1.0162 0.5338 0.5354 0.096 Uiso 1 1 calc R . .
C32 C 0.9851(2) 0.59939(17) 0.60759(13) 0.0449(10) Uani 1 1 d . . .
H32A H 1.0261 0.5765 0.6138 0.067 Uiso 1 1 calc R . .
H32B H 0.9594 0.6058 0.6345 0.067 Uiso 1 1 calc R . .
H32C H 0.9990 0.6362 0.5953 0.067 Uiso 1 1 calc R . .
C33 C 0.8708(2) 0.60158(17) 0.56545(14) 0.0511(11) Uani 1 1 d . . .
H33A H 0.8820 0.6367 0.5497 0.077 Uiso 1 1 calc R . .
H33B H 0.8487 0.6113 0.5930 0.077 Uiso 1 1 calc R . .
H33C H 0.8395 0.5782 0.5480 0.077 Uiso 1 1 calc R . .
C34 C 0.89978(18) 0.40510(15) 0.72389(12) 0.0344(9) Uani 1 1 d . . .
H34A H 0.9214 0.4087 0.6950 0.041 Uiso 1 1 calc R . .
H34B H 0.9316 0.4220 0.7454 0.041 Uiso 1 1 calc R . .
C35 C 0.88974(17) 0.34166(15) 0.73437(11) 0.0300(8) Uani 1 1 d . . .
C36 C 0.87741(17) 0.29828(15) 0.70203(11) 0.0288(8) Uani 1 1 d . . .
C37 C 0.86060(16) 0.24202(15) 0.71356(11) 0.0282(8) Uani 1 1 d . . .
C38 C 0.85795(17) 0.22722(16) 0.75833(11) 0.0312(8) Uani 1 1 d . . .
H38 H 0.8467 0.1892 0.7662 0.037 Uiso 1 1 calc R . .
C39 C 0.87168(17) 0.26781(16) 0.79163(11) 0.0317(8) Uani 1 1 d . . .
C40 C 0.88752(18) 0.32457(16) 0.77798(11) 0.0346(9) Uani 1 1 d . . .
H40 H 0.8971 0.3523 0.7996 0.042 Uiso 1 1 calc R . .
C41 C 0.86662(18) 0.25381(17) 0.84133(11) 0.0359(9) Uani 1 1 d . . .
C42 C 0.79841(19) 0.2798(2) 0.85895(13) 0.0474(10) Uani 1 1 d . . .
H42A H 0.7594 0.2645 0.8425 0.071 Uiso 1 1 calc R . .
H42B H 0.7997 0.3214 0.8558 0.071 Uiso 1 1 calc R . .
H42C H 0.7932 0.2699 0.8896 0.071 Uiso 1 1 calc R . .
C43 C 0.9281(2) 0.2795(2) 0.86604(13) 0.0558(12) Uani 1 1 d . . .
H43A H 0.9250 0.2691 0.8967 0.084 Uiso 1 1 calc R . .
H43B H 0.9273 0.3212 0.8632 0.084 Uiso 1 1 calc R . .
H43C H 0.9711 0.2646 0.8539 0.084 Uiso 1 1 calc R . .
C44 C 0.8646(3) 0.18872(19) 0.84951(13) 0.0629(14) Uani 1 1 d . . .
H44A H 0.9062 0.1711 0.8375 0.094 Uiso 1 1 calc R . .
H44B H 0.8239 0.1724 0.8355 0.094 Uiso 1 1 calc R . .
H44C H 0.8625 0.1814 0.8807 0.094 Uiso 1 1 calc R . .
C45 C 0.94540(18) 0.33139(15) 0.63946(11) 0.0333(8) Uani 1 1 d . . .
H45A H 0.9784 0.3366 0.6636 0.040 Uiso 1 1 calc R . .
H45B H 0.9392 0.3688 0.6251 0.040 Uiso 1 1 calc R . .
C46 C 0.97579(18) 0.28866(16) 0.60663(11) 0.0310(8) Uani 1 1 d . . .
C47 C 1.04589(17) 0.30384(15) 0.58404(11) 0.0326(8) Uani 1 1 d . . .
C48 C 1.1028(2) 0.27458(19) 0.61200(14) 0.0496(11) Uani 1 1 d . . .
H48A H 1.1032 0.2915 0.6410 0.074 Uiso 1 1 calc R . .
H48B H 1.1478 0.2802 0.5983 0.074 Uiso 1 1 calc R . .
H48C H 1.0932 0.2336 0.6142 0.074 Uiso 1 1 calc R . .
C49 C 1.0458(2) 0.27845(17) 0.53711(12) 0.0433(10) Uani 1 1 d . . .
H49A H 1.0908 0.2850 0.5236 0.065 Uiso 1 1 calc R . .
H49B H 1.0100 0.2971 0.5199 0.065 Uiso 1 1 calc R . .
H49C H 1.0367 0.2373 0.5385 0.065 Uiso 1 1 calc R . .
C50 C 1.0585(2) 0.36944(17) 0.58194(14) 0.0453(10) Uani 1 1 d . . .
H50A H 1.0623 0.3847 0.6114 0.068 Uiso 1 1 calc R . .
H50B H 1.0199 0.3879 0.5670 0.068 Uiso 1 1 calc R . .
H50C H 1.1012 0.3771 0.5661 0.068 Uiso 1 1 calc R . .
C51 C 0.84037(17) 0.19620(15) 0.67890(11) 0.0294(8) Uani 1 1 d . . .
H51A H 0.8615 0.2061 0.6507 0.035 Uiso 1 1 calc R . .
H51B H 0.8580 0.1583 0.6879 0.035 Uiso 1 1 calc R . .
C52 C 0.76039(17) 0.19359(14) 0.67393(11) 0.0275(8) Uani 1 1 d . . .
C53 C 0.72546(16) 0.21576(13) 0.63652(10) 0.0239(7) Uani 1 1 d . . .
C54 C 0.65242(17) 0.22173(14) 0.63700(11) 0.0283(8) Uani 1 1 d . . .
C55 C 0.61454(18) 0.20276(14) 0.67414(11) 0.0303(8) Uani 1 1 d . . .
H55 H 0.5661 0.2079 0.6745 0.036 Uiso 1 1 calc R . .
C56 C 0.64632(18) 0.17672(15) 0.71031(11) 0.0298(8) Uani 1 1 d . . .
C57 C 0.71996(17) 0.17326(15) 0.70849(11) 0.0309(8) Uani 1 1 d . . .
H57 H 0.7430 0.1561 0.7322 0.037 Uiso 1 1 calc R . .
C58 C 0.60646(18) 0.15468(15) 0.75088(11) 0.0332(8) Uani 1 1 d . . .
C59 C 0.6106(2) 0.08741(16) 0.75173(13) 0.0480(10) Uani 1 1 d . . .
H59A H 0.5887 0.0731 0.7782 0.072 Uiso 1 1 calc R . .
H59B H 0.6589 0.0755 0.7512 0.072 Uiso 1 1 calc R . .
H59C H 0.5867 0.0719 0.7264 0.072 Uiso 1 1 calc R . .
C60 C 0.6408(2) 0.17730(18) 0.79309(12) 0.0463(10) Uani 1 1 d . . .
H60A H 0.6416 0.2191 0.7926 0.069 Uiso 1 1 calc R . .
H60B H 0.6880 0.1628 0.7950 0.069 Uiso 1 1 calc R . .
H60C H 0.6144 0.1642 0.8183 0.069 Uiso 1 1 calc R . .
C61 C 0.5296(2) 0.1719(2) 0.75001(14) 0.0553(11) Uani 1 1 d . . .
H61A H 0.5257 0.2136 0.7504 0.083 Uiso 1 1 calc R . .
H61B H 0.5063 0.1560 0.7754 0.083 Uiso 1 1 calc R . .
H61C H 0.5081 0.1570 0.7236 0.083 Uiso 1 1 calc R . .
C62 C 0.79769(18) 0.18777(15) 0.57700(10) 0.0286(8) Uani 1 1 d . . .
H62A H 0.7909 0.1514 0.5928 0.034 Uiso 1 1 calc R . .
H62B H 0.8476 0.1963 0.5768 0.034 Uiso 1 1 calc R . .
C63 C 0.77224(17) 0.18076(14) 0.52987(11) 0.0275(8) Uani 1 1 d . . .
C64 C 0.81377(18) 0.14076(15) 0.50022(11) 0.0322(8) Uani 1 1 d . . .
C65 C 0.7685(2) 0.11803(19) 0.46243(12) 0.0483(10) Uani 1 1 d . . .
H65A H 0.7325 0.0931 0.4741 0.072 Uiso 1 1 calc R . .
H65B H 0.7973 0.0964 0.4422 0.072 Uiso 1 1 calc R . .
H65C H 0.7473 0.1503 0.4473 0.072 Uiso 1 1 calc R . .
C66 C 0.8454(2) 0.08945(17) 0.52569(13) 0.0462(10) Uani 1 1 d . . .
H66A H 0.8789 0.1037 0.5468 0.069 Uiso 1 1 calc R . .
H66B H 0.8684 0.0636 0.5054 0.069 Uiso 1 1 calc R . .
H66C H 0.8087 0.0689 0.5409 0.069 Uiso 1 1 calc R . .
C67 C 0.87429(19) 0.17775(17) 0.48125(12) 0.0418(10) Uani 1 1 d . . .
H67A H 0.8553 0.2090 0.4639 0.063 Uiso 1 1 calc R . .
H67B H 0.9036 0.1537 0.4630 0.063 Uiso 1 1 calc R . .
H67C H 0.9016 0.1935 0.5051 0.063 Uiso 1 1 calc R . .
C68 C 0.61572(18) 0.25240(14) 0.59988(11) 0.0272(8) Uani 1 1 d . . .
H68A H 0.6416 0.2473 0.5725 0.033 Uiso 1 1 calc R . .
H68B H 0.5689 0.2366 0.5959 0.033 Uiso 1 1 calc R . .
C69 C 0.58833(18) 0.34812(14) 0.57574(11) 0.0321(8) Uani 1 1 d . . .
H69A H 0.5407 0.3376 0.5677 0.039 Uiso 1 1 calc R . .
H69B H 0.6182 0.3427 0.5501 0.039 Uiso 1 1 calc R . .
N1 N 0.5820(3) 0.3367(2) 0.77330(16) 0.0858(14) Uani 1 1 d . . .
C70 C 0.6245(3) 0.3374(2) 0.74600(17) 0.0609(12) Uani 1 1 d . . .
C71 C 0.6782(2) 0.33801(18) 0.71257(14) 0.0540(11) Uani 1 1 d . . .
H71A H 0.7070 0.3720 0.7162 0.081 Uiso 1 1 calc R . .
H71B H 0.6567 0.3387 0.6839 0.081 Uiso 1 1 calc R . .
H71C H 0.7067 0.3037 0.7153 0.081 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
O1 0.0281(13) 0.0354(14) 0.0329(14) -0.0022(11) -0.0035(11) 0.0031(11)
O2 0.0503(17) 0.0385(17) 0.0489(17) 0.0023(13) 0.0139(14) 0.0108(13)
O3 0.0348(14) 0.0330(14) 0.0309(13) -0.0054(10) 0.0038(11) -0.0082(11)
O4 0.0459(16) 0.0393(16) 0.0410(15) -0.0027(13) 0.0068(12) 0.0010(13)
O5 0.0259(13) 0.0455(15) 0.0250(13) 0.0017(10) 0.0029(10) -0.0026(11)
O6 0.0376(15) 0.0497(17) 0.0508(17) -0.0106(13) 0.0131(13) -0.0125(14)
O7 0.0340(13) 0.0295(13) 0.0261(13) -0.0006(10) 0.0014(11) 0.0025(11)
O8 0.0356(14) 0.0491(16) 0.0305(14) -0.0005(12) -0.0022(11) 0.0102(13)
O9 0.0364(13) 0.0292(13) 0.0267(13) -0.0025(10) -0.0030(11) 0.0004(11)
C1 0.034(2) 0.0268(19) 0.0280(19) 0.0021(15) -0.0018(16) 0.0010(16)
C2 0.029(2) 0.031(2) 0.0299(19) 0.0054(15) 0.0017(16) 0.0059(16)
C3 0.035(2) 0.032(2) 0.0230(18) 0.0022(15) 0.0047(16) -0.0023(17)
C4 0.038(2) 0.031(2) 0.0269(19) -0.0004(15) 0.0067(16) 0.0004(17)
C5 0.030(2) 0.037(2) 0.031(2) -0.0003(16) 0.0072(16) 0.0014(17)
C6 0.0281(19) 0.039(2) 0.033(2) -0.0013(16) 0.0009(16) -0.0019(17)
C7 0.033(2) 0.041(2) 0.048(2) -0.0095(18) 0.0020(18) 0.0095(18)
C8 0.046(2) 0.048(2) 0.058(3) -0.011(2) 0.005(2) 0.020(2)
C9 0.049(3) 0.066(3) 0.056(3) -0.010(2) -0.015(2) 0.027(2)
C10 0.039(3) 0.065(3) 0.098(4) -0.006(3) 0.016(3) 0.006(2)
C11 0.0260(18) 0.032(2) 0.039(2) -0.0040(16) -0.0021(17) 0.0050(16)
C12 0.029(2) 0.031(2) 0.045(2) 0.0070(17) 0.0017(17) 0.0025(17)
C13 0.034(2) 0.035(2) 0.042(2) -0.0050(17) 0.0036(17) 0.0027(17)
C14 0.040(2) 0.057(3) 0.051(3) -0.005(2) -0.006(2) 0.003(2)
C15 0.033(2) 0.047(2) 0.048(2) -0.0100(19) 0.0045(18) 0.0061(19)
C16 0.052(3) 0.051(2) 0.041(2) -0.0023(19) 0.011(2) 0.002(2)
C17 0.031(2) 0.032(2) 0.034(2) 0.0012(16) 0.0016(16) -0.0010(16)
C18 0.034(2) 0.0253(19) 0.033(2) -0.0053(15) 0.0011(17) -0.0069(16)
C19 0.033(2) 0.0299(19) 0.0282(19) -0.0021(15) 0.0025(16) -0.0077(17)
C20 0.031(2) 0.031(2) 0.035(2) -0.0038(16) -0.0011(16) -0.0099(16)
C21 0.034(2) 0.0304(19) 0.0288(19) 0.0004(15) 0.0003(16) -0.0012(16)
C22 0.040(2) 0.030(2) 0.030(2) -0.0004(15) 0.0027(17) -0.0057(17)
C23 0.0302(19) 0.029(2) 0.039(2) -0.0040(16) -0.0012(17) -0.0030(16)
C24 0.043(2) 0.045(2) 0.039(2) 0.0042(18) 0.0097(18) 0.0026(19)
C25 0.108(4) 0.050(3) 0.041(3) -0.009(2) 0.025(3) -0.004(3)
C26 0.054(3) 0.053(3) 0.042(2) 0.003(2) 0.014(2) 0.000(2)
C27 0.051(3) 0.099(4) 0.049(3) -0.006(3) 0.014(2) 0.007(3)
C28 0.035(2) 0.040(2) 0.030(2) -0.0044(16) -0.0026(17) -0.0093(18)
C29 0.0249(19) 0.032(2) 0.037(2) -0.0024(17) -0.0037(16) 0.0002(16)
C30 0.033(2) 0.035(2) 0.041(2) -0.0034(17) 0.0086(17) 0.0003(17)
C31 0.082(3) 0.058(3) 0.053(3) 0.005(2) 0.020(3) -0.017(3)
C32 0.039(2) 0.041(2) 0.054(3) 0.0045(19) 0.000(2) -0.0050(19)
C33 0.060(3) 0.037(2) 0.056(3) 0.0040(19) -0.017(2) 0.002(2)
C34 0.030(2) 0.041(2) 0.032(2) -0.0039(16) -0.0035(16) -0.0045(17)
C35 0.0173(16) 0.041(2) 0.032(2) -0.0007(16) -0.0024(15) -0.0015(16)
C36 0.0210(17) 0.034(2) 0.032(2) -0.0008(16) -0.0074(15) 0.0025(15)
C37 0.0160(16) 0.043(2) 0.0251(19) -0.0027(15) -0.0009(14) 0.0031(15)
C38 0.0276(18) 0.035(2) 0.031(2) 0.0044(16) -0.0003(16) 0.0065(16)
C39 0.0260(19) 0.042(2) 0.0266(19) -0.0011(16) -0.0026(15) 0.0052(16)
C40 0.0286(19) 0.046(2) 0.029(2) -0.0046(17) -0.0015(16) 0.0001(17)
C41 0.035(2) 0.053(2) 0.0201(18) 0.0015(16) -0.0020(15) 0.0042(18)
C42 0.032(2) 0.079(3) 0.032(2) 0.001(2) 0.0044(17) 0.008(2)
C43 0.039(2) 0.098(4) 0.030(2) 0.003(2) -0.0042(19) 0.002(2)
C44 0.110(4) 0.052(3) 0.027(2) 0.0093(19) 0.002(2) 0.019(3)
C45 0.032(2) 0.039(2) 0.0291(19) 0.0038(16) -0.0015(16) -0.0026(17)
C46 0.031(2) 0.037(2) 0.0249(19) 0.0049(16) 0.0000(15) -0.0036(17)
C47 0.0224(18) 0.044(2) 0.032(2) 0.0058(16) 0.0006(15) -0.0018(16)
C48 0.031(2) 0.065(3) 0.052(3) 0.018(2) -0.0050(19) -0.002(2)
C49 0.040(2) 0.051(2) 0.039(2) -0.0003(18) 0.0126(18) 0.0011(19)
C50 0.036(2) 0.049(2) 0.051(2) 0.0044(19) 0.0044(19) -0.0119(19)
C51 0.0249(18) 0.0310(19) 0.032(2) 0.0035(15) -0.0022(15) 0.0013(15)
C52 0.0275(18) 0.0298(19) 0.0251(18) -0.0053(15) 0.0029(15) -0.0024(15)
C53 0.0259(18) 0.0240(18) 0.0218(17) -0.0007(14) 0.0013(14) -0.0040(15)
C54 0.0310(19) 0.0290(19) 0.0248(18) -0.0063(14) 0.0008(15) -0.0017(16)
C55 0.0258(18) 0.035(2) 0.030(2) -0.0037(15) -0.0008(16) 0.0008(16)
C56 0.0304(19) 0.034(2) 0.0252(19) -0.0017(15) 0.0027(16) -0.0016(16)
C57 0.0283(19) 0.038(2) 0.0270(19) 0.0003(16) -0.0003(15) 0.0011(16)
C58 0.0290(19) 0.043(2) 0.0280(19) 0.0027(16) 0.0050(15) 0.0004(17)
C59 0.058(3) 0.044(2) 0.042(2) -0.0020(19) 0.009(2) -0.004(2)
C60 0.055(3) 0.052(2) 0.032(2) 0.0007(18) 0.0071(19) -0.009(2)
C61 0.043(2) 0.072(3) 0.051(3) 0.016(2) 0.013(2) 0.006(2)
C62 0.0278(18) 0.0328(19) 0.0252(18) -0.0018(15) 0.0040(15) -0.0013(16)
C63 0.0216(18) 0.0300(19) 0.0309(19) 0.0020(15) 0.0027(15) -0.0034(16)
C64 0.037(2) 0.036(2) 0.0236(18) 0.0006(15) -0.0012(16) 0.0039(17)
C65 0.050(3) 0.060(3) 0.035(2) -0.0100(19) 0.0014(19) -0.001(2)
C66 0.058(3) 0.039(2) 0.041(2) -0.0037(18) 0.008(2) 0.012(2)
C67 0.040(2) 0.049(2) 0.036(2) -0.0015(18) 0.0132(18) 0.0038(19)
C68 0.0261(18) 0.0297(19) 0.0259(18) 0.0004(14) -0.0005(15) 0.0051(15)
C69 0.0300(19) 0.034(2) 0.033(2) 0.0017(16) -0.0039(16) 0.0041(16)
N1 0.089(3) 0.079(3) 0.089(3) 0.001(3) 0.028(3) -0.001(3)
C70 0.062(3) 0.055(3) 0.066(3) -0.002(2) 0.013(3) -0.007(2)
C71 0.065(3) 0.046(3) 0.051(3) -0.011(2) 0.014(2) -0.012(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
O1 C2 1.388(4) . ?
O1 C11 1.421(4) . ?
O1 O3 2.908(3) . ?
O1 O7 4.151(3) . ?
O2 C12 1.203(4) . ?
O3 C19 1.389(4) . ?
O3 C28 1.425(4) . ?
O3 O5 3.440(3) . ?
O4 C29 1.213(4) . ?
O5 C36 1.397(4) . ?
O5 C45 1.437(4) . ?
O5 O7 3.368(3) . ?
O6 C46 1.210(4) . ?
O7 C53 1.368(4) . ?
O7 C62 1.434(4) . ?
O8 C63 1.227(4) . ?
O9 C68 1.418(4) . ?
O9 C69 1.420(4) . ?
C1 C2 1.381(5) . ?
C1 C6 1.395(5) . ?
C1 C69 1.507(5) . ?
C2 C3 1.396(5) . ?
C3 C4 1.397(5) . ?
C3 C17 1.515(5) . ?
C4 C5 1.391(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(5) . ?
C5 C7 1.550(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.511(5) . ?
C7 C10 1.526(6) . ?
C7 C9 1.541(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.498(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.562(5) . ?
C13 C16 1.520(5) . ?
C13 C15 1.529(5) . ?
C13 C14 1.537(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.517(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.385(5) . ?
C18 C19 1.397(5) . ?
C19 C20 1.401(5) . ?
C20 C21 1.390(5) . ?
C20 C34 1.522(5) . ?
C21 C22 1.383(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.390(5) . ?
C22 C24 1.549(5) . ?
C23 H23 0.9300 . ?
C24 C27 1.511(6) . ?
C24 C26 1.525(5) . ?
C24 C25 1.544(6) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.499(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.519(5) . ?
C30 C31 1.510(5) . ?
C30 C32 1.525(5) . ?
C30 C33 1.539(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.502(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C40 1.377(5) . ?
C35 C36 1.415(5) . ?
C36 C37 1.375(5) . ?
C37 C38 1.397(5) . ?
C37 C51 1.534(5) . ?
C38 C39 1.396(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.399(5) . ?
C39 C41 1.540(5) . ?
C40 H40 0.9300 . ?
C41 C43 1.509(5) . ?
C41 C44 1.514(6) . ?
C41 C42 1.525(5) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.511(5) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.539(5) . ?
C47 C50 1.525(5) . ?
C47 C48 1.530(5) . ?
C47 C49 1.534(5) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C52 1.531(5) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C57 1.379(5) . ?
C52 C53 1.408(5) . ?
C53 C54 1.397(5) . ?
C54 C55 1.404(5) . ?
C54 C68 1.498(5) . ?
C55 C56 1.386(5) . ?
C55 H55 0.9300 . ?
C56 C57 1.405(5) . ?
C56 C58 1.529(5) . ?
C57 H57 0.9300 . ?
C58 C61 1.516(5) . ?
C58 C60 1.525(5) . ?
C58 C59 1.545(5) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 C63 1.514(5) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.507(5) . ?
C64 C65 1.523(5) . ?
C64 C66 1.530(5) . ?
C64 C67 1.542(5) . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
N1 C70 1.157(6) . ?
C70 C71 1.437(6) . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?

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
C2 O1 C11 120.9(3) . . ?
C2 O1 O3 128.23(19) . . ?
C11 O1 O3 90.83(18) . . ?
C2 O1 O7 128.19(19) . . ?
C11 O1 O7 48.41(16) . . ?
O3 O1 O7 103.57(8) . . ?
C19 O3 C28 111.8(2) . . ?
C19 O3 O1 80.63(17) . . ?
C28 O3 O1 141.6(2) . . ?
C19 O3 O5 96.32(18) . . ?
C28 O3 O5 132.1(2) . . ?
O1 O3 O5 78.62(8) . . ?
C36 O5 C45 116.9(2) . . ?
C36 O5 O7 111.08(18) . . ?
C45 O5 O7 123.72(18) . . ?
C36 O5 O3 108.32(18) . . ?
C45 O5 O3 80.73(17) . . ?
O7 O5 O3 110.64(8) . . ?
C53 O7 C62 114.3(2) . . ?
C53 O7 O5 94.12(17) . . ?
C62 O7 O5 108.57(17) . . ?
C53 O7 O1 94.59(17) . . ?
C62 O7 O1 150.90(18) . . ?
O5 O7 O1 64.06(6) . . ?
C68 O9 C69 113.4(2) . . ?
C2 C1 C6 118.0(3) . . ?
C2 C1 C69 123.6(3) . . ?
C6 C1 C69 118.3(3) . . ?
C1 C2 O1 125.1(3) . . ?
C1 C2 C3 121.3(3) . . ?
O1 C2 C3 113.4(3) . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 C17 120.0(3) . . ?
C4 C3 C17 121.2(3) . . ?
C5 C4 C3 122.1(3) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C6 116.8(3) . . ?
C4 C5 C7 123.1(3) . . ?
C6 C5 C7 120.1(3) . . ?
C5 C6 C1 123.1(3) . . ?
C5 C6 H6 118.4 . . ?
C1 C6 H6 118.4 . . ?
C8 C7 C10 109.5(3) . . ?
C8 C7 C9 107.3(3) . . ?
C10 C7 C9 110.1(4) . . ?
C8 C7 C5 111.5(3) . . ?
C10 C7 C5 109.5(3) . . ?
C9 C7 C5 108.9(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C12 113.7(3) . . ?
O1 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
O1 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
O2 C12 C11 121.6(3) . . ?
O2 C12 C13 120.3(3) . . ?
C11 C12 C13 118.2(3) . . ?
C16 C13 C15 110.8(3) . . ?
C16 C13 C14 110.1(3) . . ?
C15 C13 C14 109.1(3) . . ?
C16 C13 C12 109.0(3) . . ?
C15 C13 C12 110.0(3) . . ?
C14 C13 C12 107.8(3) . . ?
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 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C3 C17 C18 114.8(3) . . ?
C3 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
C3 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C23 C18 C19 118.0(3) . . ?
C23 C18 C17 120.8(3) . . ?
C19 C18 C17 121.2(3) . . ?
O3 C19 C18 119.7(3) . . ?
O3 C19 C20 119.0(3) . . ?
C18 C19 C20 121.3(3) . . ?
C21 C20 C19 117.3(3) . . ?
C21 C20 C34 122.4(3) . . ?
C19 C20 C34 120.3(3) . . ?
C22 C21 C20 123.8(3) . . ?
C22 C21 H21 118.1 . . ?
C20 C21 H21 118.1 . . ?
C21 C22 C23 116.3(3) . . ?
C21 C22 C24 122.4(3) . . ?
C23 C22 C24 121.1(3) . . ?
C18 C23 C22 123.3(3) . . ?
C18 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C27 C24 C26 109.6(3) . . ?
C27 C24 C25 108.3(4) . . ?
C26 C24 C25 107.7(3) . . ?
C27 C24 C22 112.3(3) . . ?
C26 C24 C22 112.5(3) . . ?
C25 C24 C22 106.3(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C29 109.9(3) . . ?
O3 C28 H28A 109.7 . . ?
C29 C28 H28A 109.7 . . ?
O3 C28 H28B 109.7 . . ?
C29 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
O4 C29 C28 120.6(3) . . ?
O4 C29 C30 122.5(3) . . ?
C28 C29 C30 116.9(3) . . ?
C31 C30 C29 110.6(3) . . ?
C31 C30 C32 110.6(3) . . ?
C29 C30 C32 110.5(3) . . ?
C31 C30 C33 108.0(3) . . ?
C29 C30 C33 106.4(3) . . ?
C32 C30 C33 110.7(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C20 112.7(3) . . ?
C35 C34 H34A 109.0 . . ?
C20 C34 H34A 109.0 . . ?
C35 C34 H34B 109.0 . . ?
C20 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
C40 C35 C36 117.2(3) . . ?
C40 C35 C34 118.8(3) . . ?
C36 C35 C34 123.8(3) . . ?
C37 C36 O5 118.2(3) . . ?
C37 C36 C35 121.6(3) . . ?
O5 C36 C35 120.2(3) . . ?
C36 C37 C38 118.9(3) . . ?
C36 C37 C51 121.9(3) . . ?
C38 C37 C51 119.1(3) . . ?
C39 C38 C37 122.0(3) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C38 C39 C40 116.6(3) . . ?
C38 C39 C41 123.6(3) . . ?
C40 C39 C41 119.7(3) . . ?
C35 C40 C39 123.7(3) . . ?
C35 C40 H40 118.2 . . ?
C39 C40 H40 118.2 . . ?
C43 C41 C44 108.9(3) . . ?
C43 C41 C42 109.5(3) . . ?
C44 C41 C42 107.9(3) . . ?
C43 C41 C39 110.7(3) . . ?
C44 C41 C39 111.5(3) . . ?
C42 C41 C39 108.2(3) . . ?
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 . . ?
O5 C45 C46 112.7(3) . . ?
O5 C45 H45A 109.1 . . ?
C46 C45 H45A 109.1 . . ?
O5 C45 H45B 109.1 . . ?
C46 C45 H45B 109.1 . . ?
H45A C45 H45B 107.8 . . ?
O6 C46 C45 121.5(3) . . ?
O6 C46 C47 120.0(3) . . ?
C45 C46 C47 118.5(3) . . ?
C50 C47 C48 110.2(3) . . ?
C50 C47 C49 109.7(3) . . ?
C48 C47 C49 110.2(3) . . ?
C50 C47 C46 112.2(3) . . ?
C48 C47 C46 105.6(3) . . ?
C49 C47 C46 108.9(3) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C37 110.1(3) . . ?
C52 C51 H51A 109.6 . . ?
C37 C51 H51A 109.6 . . ?
C52 C51 H51B 109.6 . . ?
C37 C51 H51B 109.6 . . ?
H51A C51 H51B 108.2 . . ?
C57 C52 C53 117.9(3) . . ?
C57 C52 C51 119.6(3) . . ?
C53 C52 C51 122.3(3) . . ?
O7 C53 C54 118.3(3) . . ?
O7 C53 C52 121.8(3) . . ?
C54 C53 C52 119.8(3) . . ?
C53 C54 C55 119.3(3) . . ?
C53 C54 C68 120.2(3) . . ?
C55 C54 C68 120.4(3) . . ?
C56 C55 C54 122.8(3) . . ?
C56 C55 H55 118.6 . . ?
C54 C55 H55 118.6 . . ?
C55 C56 C57 115.4(3) . . ?
C55 C56 C58 124.0(3) . . ?
C57 C56 C58 120.5(3) . . ?
C52 C57 C56 124.5(3) . . ?
C52 C57 H57 117.7 . . ?
C56 C57 H57 117.7 . . ?
C61 C58 C60 109.8(3) . . ?
C61 C58 C56 112.3(3) . . ?
C60 C58 C56 110.3(3) . . ?
C61 C58 C59 108.0(3) . . ?
C60 C58 C59 107.7(3) . . ?
C56 C58 C59 108.6(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O7 C62 C63 111.9(3) . . ?
O7 C62 H62A 109.2 . . ?
C63 C62 H62A 109.2 . . ?
O7 C62 H62B 109.2 . . ?
C63 C62 H62B 109.2 . . ?
H62A C62 H62B 107.9 . . ?
O8 C63 C64 120.9(3) . . ?
O8 C63 C62 121.8(3) . . ?
C64 C63 C62 117.2(3) . . ?
C63 C64 C65 111.0(3) . . ?
C63 C64 C66 112.0(3) . . ?
C65 C64 C66 109.7(3) . . ?
C63 C64 C67 106.2(3) . . ?
C65 C64 C67 109.4(3) . . ?
C66 C64 C67 108.5(3) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O9 C68 C54 107.5(3) . . ?
O9 C68 H68A 110.2 . . ?
C54 C68 H68A 110.2 . . ?
O9 C68 H68B 110.2 . . ?
C54 C68 H68B 110.2 . . ?
H68A C68 H68B 108.5 . . ?
O9 C69 C1 108.5(3) . . ?
O9 C69 H69A 110.0 . . ?
C1 C69 H69A 110.0 . . ?
O9 C69 H69B 110.0 . . ?
C1 C69 H69B 110.0 . . ?
H69A C69 H69B 108.4 . . ?
N1 C70 C71 179.1(6) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?