# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2010


data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Nair, Vijay'
_publ_contact_author_email       'vijaynair 2001@yahoo.com'

_publ_section_title              
;
NHC Catalysed Annulation of Enals
to Tethered Dienones: Efficient Synthesis of Bicyclic Dienes
;
_publ_author_name                V.Nair

# Attachment 'crystal.cif.txt'

data_vtt110f
_database_code_depnum_ccdc_archive 'CCDC 777238'
#TrackingRef 'crystal.cif.txt'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H32 O5'
_chemical_formula_weight         532.61

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pca21

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

_cell_length_a                   16.977(3)
_cell_length_b                   13.692(3)
_cell_length_c                   11.959(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2779.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_special_details           
;
?
;

_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  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16088
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         28.25
_reflns_number_total             6290
_reflns_number_gt                4839
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SAMRT'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

_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
_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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.6(15)
_refine_ls_number_reflns         6290
_refine_ls_number_parameters     364
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_ref         0.1430
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.04668(15) 0.73223(19) 0.8843(2) 0.0236(6) Uani 1 d . . .
O2 O 0.93748(16) 0.75655(18) 0.9869(2) 0.0233(6) Uani 1 d . . .
O3 O 1.01783(16) 0.53898(18) 1.0018(2) 0.0234(6) Uani 1 d . . .
O4 O 0.91477(14) 0.43708(17) 1.00319(19) 0.0149(6) Uani 1 d . . .
O5 O 1.14486(15) 0.16526(19) 0.8535(2) 0.0235(6) Uani 1 d . . .
C1 C 0.7254(2) 0.2480(3) 0.7158(3) 0.0176(8) Uani 1 d . . .
H1 H 0.7181 0.2832 0.7815 0.021 Uiso 1 calc R . .
C2 C 0.6791(2) 0.1669(3) 0.6959(3) 0.0213(9) Uani 1 d . . .
H2 H 0.6421 0.1473 0.7487 0.026 Uiso 1 calc R . .
C3 C 0.6878(2) 0.1149(3) 0.5975(3) 0.0216(9) Uani 1 d . . .
H3 H 0.6564 0.0606 0.5835 0.026 Uiso 1 calc R . .
C4 C 0.7439(2) 0.1443(3) 0.5201(3) 0.0187(8) Uani 1 d . . .
H4 H 0.7499 0.1100 0.4535 0.022 Uiso 1 calc R . .
C5 C 0.7908(2) 0.2251(3) 0.5419(3) 0.0151(8) Uani 1 d . . .
H5 H 0.8287 0.2440 0.4900 0.018 Uiso 1 calc R . .
C6 C 0.78217(19) 0.2785(2) 0.6408(3) 0.0101(7) Uani 1 d . . .
C7 C 0.8310(2) 0.3694(2) 0.6576(3) 0.0117(7) Uani 1 d . . .
H7 H 0.8758 0.3659 0.6062 0.014 Uiso 1 calc R . .
C8 C 0.7867(2) 0.4650(2) 0.6335(3) 0.0121(7) Uani 1 d . . .
H8 H 0.7337 0.4603 0.6656 0.014 Uiso 1 calc R . .
C9 C 0.8377(2) 0.6370(3) 0.6780(3) 0.0144(8) Uani 1 d . . .
C10 C 0.8332(2) 0.5380(3) 0.7000(3) 0.0138(8) Uani 1 d . . .
C11 C 0.8746(2) 0.4932(3) 0.7859(3) 0.0128(7) Uani 1 d . . .
C12 C 0.8648(2) 0.3827(2) 0.7796(3) 0.0112(7) Uani 1 d . . .
H12 H 0.8245 0.3627 0.8335 0.013 Uiso 1 calc R . .
C13 C 0.9201(2) 0.5498(3) 0.8582(3) 0.0113(7) Uani 1 d . . .
C14 C 0.9261(2) 0.6508(3) 0.8355(3) 0.0140(8) Uani 1 d . . .
C15 C 0.88602(19) 0.6948(3) 0.7482(3) 0.0125(7) Uani 1 d . . .
C16 C 0.7993(2) 0.6769(3) 0.5732(3) 0.0196(9) Uani 1 d . . .
H16A H 0.8402 0.6984 0.5221 0.023 Uiso 1 calc R . .
H16B H 0.7679 0.7336 0.5930 0.023 Uiso 1 calc R . .
C17 C 0.7463(2) 0.6025(2) 0.5127(3) 0.0202(8) Uani 1 d . . .
H17A H 0.6951 0.6018 0.5486 0.024 Uiso 1 calc R . .
H17B H 0.7388 0.6236 0.4360 0.024 Uiso 1 calc R . .
C18 C 0.7796(2) 0.4988(3) 0.5125(3) 0.0167(8) Uani 1 d . . .
H18A H 0.7448 0.4555 0.4714 0.020 Uiso 1 calc R . .
H18B H 0.8308 0.4980 0.4767 0.020 Uiso 1 calc R . .
C19 C 0.8906(2) 0.8029(2) 0.7314(3) 0.0139(8) Uani 1 d . . .
C20 C 0.9603(2) 0.8488(3) 0.7017(3) 0.0177(8) Uani 1 d . . .
H20 H 1.0049 0.8116 0.6869 0.021 Uiso 1 calc R . .
C21 C 0.9642(2) 0.9494(3) 0.6939(3) 0.0235(9) Uani 1 d . . .
H21 H 1.0115 0.9794 0.6750 0.028 Uiso 1 calc R . .
C22 C 0.8984(2) 1.0055(3) 0.7140(3) 0.0224(9) Uani 1 d . . .
H22 H 0.9008 1.0731 0.7079 0.027 Uiso 1 calc R . .
C23 C 0.8284(2) 0.9600(3) 0.7434(3) 0.0230(9) Uani 1 d . . .
H23 H 0.7836 0.9974 0.7565 0.028 Uiso 1 calc R . .
C24 C 0.8247(2) 0.8607(3) 0.7532(3) 0.0166(8) Uani 1 d . . .
H24 H 0.7777 0.8313 0.7746 0.020 Uiso 1 calc R . .
C25 C 0.9785(2) 0.7157(3) 0.9044(3) 0.0164(8) Uani 1 d . . .
C26 C 0.9799(3) 0.8324(3) 1.0488(3) 0.0350(12) Uani 1 d . . .
H26A H 1.0229 0.8034 1.0890 0.052 Uiso 1 calc R . .
H26B H 0.9447 0.8634 1.1006 0.052 Uiso 1 calc R . .
H26C H 0.9999 0.8802 0.9974 0.052 Uiso 1 calc R . .
C27 C 0.9583(2) 0.5104(3) 0.9599(3) 0.0145(8) Uani 1 d . . .
C28 C 0.9485(3) 0.3867(3) 1.0972(3) 0.0251(10) Uani 1 d . . .
H28A H 1.0010 0.3662 1.0791 0.038 Uiso 1 calc R . .
H28B H 0.9170 0.3305 1.1147 0.038 Uiso 1 calc R . .
H28C H 0.9499 0.4297 1.1606 0.038 Uiso 1 calc R . .
C29 C 0.9389(2) 0.3237(2) 0.8006(3) 0.0110(7) Uani 1 d . . .
C30 C 0.9372(2) 0.2388(2) 0.8649(3) 0.0172(8) Uani 1 d . . .
H30 H 0.8895 0.2186 0.8953 0.021 Uiso 1 calc R . .
C31 C 1.0033(2) 0.1840(3) 0.8847(3) 0.0180(8) Uani 1 d . . .
H31 H 1.0003 0.1275 0.9276 0.022 Uiso 1 calc R . .
C32 C 1.0746(2) 0.2135(3) 0.8400(3) 0.0156(8) Uani 1 d . . .
C33 C 1.0781(2) 0.2977(3) 0.7761(3) 0.0196(8) Uani 1 d . . .
H33 H 1.1261 0.3184 0.7470 0.024 Uiso 1 calc R . .
C34 C 1.0106(2) 0.3513(3) 0.7552(3) 0.0167(8) Uani 1 d . . .
H34 H 1.0134 0.4066 0.7101 0.020 Uiso 1 calc R . .
C35 C 1.1454(3) 0.0832(3) 0.9276(3) 0.0292(10) Uani 1 d . . .
H35A H 1.1266 0.1031 0.9999 0.044 Uiso 1 calc R . .
H35B H 1.1981 0.0586 0.9344 0.044 Uiso 1 calc R . .
H35C H 1.1118 0.0330 0.8984 0.044 Uiso 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 0.0160(14) 0.0268(15) 0.0279(15) 0.0054(13) -0.0089(12) -0.0096(12)
O2 0.0329(17) 0.0169(14) 0.0201(14) -0.0068(12) 0.0010(12) -0.0070(13)
O3 0.0230(15) 0.0243(15) 0.0228(15) 0.0053(13) -0.0112(13) -0.0096(12)
O4 0.0149(13) 0.0163(13) 0.0134(12) 0.0051(11) 0.0010(11) -0.0017(11)
O5 0.0194(15) 0.0283(16) 0.0227(14) 0.0062(13) 0.0027(12) 0.0104(12)
C1 0.0160(19) 0.0196(19) 0.0171(18) -0.0015(16) -0.0079(15) -0.0023(16)
C2 0.0103(19) 0.022(2) 0.032(2) 0.0057(18) 0.0007(17) -0.0033(16)
C3 0.020(2) 0.0101(19) 0.034(2) 0.0032(17) -0.0068(18) -0.0032(17)
C4 0.020(2) 0.0190(19) 0.0173(19) -0.0033(17) -0.0035(16) -0.0029(17)
C5 0.0102(18) 0.022(2) 0.0129(18) 0.0019(15) 0.0002(14) 0.0016(16)
C6 0.0083(17) 0.0108(18) 0.0112(17) 0.0049(14) -0.0026(14) 0.0009(14)
C7 0.0125(18) 0.0133(19) 0.0093(17) 0.0025(15) -0.0005(14) -0.0015(15)
C8 0.0110(18) 0.0086(17) 0.0165(18) -0.0004(15) 0.0014(15) 0.0031(15)
C9 0.0093(18) 0.019(2) 0.0154(19) 0.0004(15) -0.0001(14) 0.0016(15)
C10 0.0159(19) 0.0193(19) 0.0063(17) -0.0028(15) 0.0005(14) -0.0008(15)
C11 0.0101(17) 0.0169(18) 0.0112(17) 0.0049(15) 0.0046(13) -0.0009(14)
C12 0.0108(17) 0.0127(18) 0.0101(17) -0.0014(15) -0.0004(14) -0.0022(14)
C13 0.0091(17) 0.0171(18) 0.0076(17) -0.0015(15) 0.0043(13) 0.0046(15)
C14 0.0111(18) 0.0170(19) 0.0139(18) -0.0045(15) 0.0027(14) 0.0017(15)
C15 0.0056(16) 0.0186(18) 0.0133(18) -0.0020(15) 0.0035(14) 0.0019(14)
C16 0.018(2) 0.015(2) 0.025(2) 0.0046(17) -0.0096(17) -0.0022(17)
C17 0.021(2) 0.0179(18) 0.022(2) 0.0025(18) -0.0049(17) -0.0034(17)
C18 0.0170(19) 0.0175(18) 0.0156(18) -0.0006(17) -0.0061(15) -0.0038(15)
C19 0.0185(19) 0.0143(18) 0.0089(17) -0.0021(14) -0.0048(15) 0.0019(15)
C20 0.019(2) 0.0161(19) 0.0180(19) 0.0011(17) 0.0001(16) -0.0001(15)
C21 0.022(2) 0.024(2) 0.025(2) 0.0083(18) 0.0006(17) -0.0092(17)
C22 0.036(3) 0.0114(19) 0.020(2) 0.0014(17) -0.0073(18) -0.0056(17)
C23 0.029(2) 0.023(2) 0.017(2) 0.0029(17) -0.0029(18) 0.0093(18)
C24 0.0175(19) 0.020(2) 0.0126(18) -0.0019(16) 0.0004(15) -0.0003(16)
C25 0.025(2) 0.0160(19) 0.0084(18) 0.0008(15) -0.0045(15) -0.0018(16)
C26 0.055(3) 0.025(2) 0.025(2) -0.0138(19) -0.009(2) -0.013(2)
C27 0.019(2) 0.0129(19) 0.0111(18) -0.0055(15) 0.0017(15) 0.0032(16)
C28 0.033(2) 0.023(2) 0.019(2) 0.0063(17) -0.0099(18) -0.0013(19)
C29 0.0121(18) 0.0109(17) 0.0100(17) -0.0029(14) -0.0017(14) 0.0018(14)
C30 0.016(2) 0.0144(19) 0.021(2) 0.0026(17) 0.0019(16) -0.0044(15)
C31 0.020(2) 0.0135(19) 0.021(2) 0.0022(16) 0.0020(17) -0.0008(15)
C32 0.0181(19) 0.0211(19) 0.0076(17) -0.0012(15) 0.0023(15) 0.0078(17)
C33 0.0089(19) 0.025(2) 0.025(2) 0.0063(18) 0.0049(16) -0.0025(16)
C34 0.0188(19) 0.0160(18) 0.0152(19) 0.0061(16) 0.0037(16) 0.0020(16)
C35 0.026(2) 0.030(3) 0.031(2) 0.008(2) 0.0025(19) 0.013(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 C25 1.203(4) . ?
O2 C25 1.331(4) . ?
O2 C26 1.465(4) . ?
O3 C27 1.194(4) . ?
O4 C27 1.350(4) . ?
O4 C28 1.438(4) . ?
O5 C32 1.373(4) . ?
O5 C35 1.431(4) . ?
C1 C2 1.381(5) . ?
C1 C6 1.381(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.509(5) . ?
C7 C8 1.537(5) . ?
C7 C12 1.578(5) . ?
C7 H7 0.9800 . ?
C8 C10 1.501(5) . ?
C8 C18 1.524(5) . ?
C8 H8 0.9800 . ?
C9 C10 1.383(5) . ?
C9 C15 1.415(5) . ?
C9 C16 1.515(5) . ?
C10 C11 1.388(5) . ?
C11 C13 1.394(5) . ?
C11 C12 1.524(5) . ?
C12 C29 1.516(5) . ?
C12 H12 0.9800 . ?
C13 C14 1.412(5) . ?
C13 C27 1.481(5) . ?
C14 C15 1.384(5) . ?
C14 C25 1.504(5) . ?
C15 C19 1.496(5) . ?
C16 C17 1.540(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.528(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.386(5) . ?
C19 C24 1.395(5) . ?
C20 C21 1.382(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.376(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.387(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.366(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C34 1.386(5) . ?
C29 C30 1.394(5) . ?
C30 C31 1.371(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.383(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.384(5) . ?
C33 C34 1.383(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 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
C25 O2 C26 114.5(3) . . ?
C27 O4 C28 116.0(3) . . ?
C32 O5 C35 117.1(3) . . ?
C2 C1 C6 121.9(4) . . ?
C2 C1 H1 119.0 . . ?
C6 C1 H1 119.0 . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 117.7(3) . . ?
C1 C6 C7 123.1(3) . . ?
C5 C6 C7 119.1(3) . . ?
C6 C7 C8 114.1(3) . . ?
C6 C7 C12 114.7(3) . . ?
C8 C7 C12 104.7(3) . . ?
C6 C7 H7 107.7 . . ?
C8 C7 H7 107.7 . . ?
C12 C7 H7 107.7 . . ?
C10 C8 C18 110.1(3) . . ?
C10 C8 C7 102.1(3) . . ?
C18 C8 C7 118.4(3) . . ?
C10 C8 H8 108.6 . . ?
C18 C8 H8 108.6 . . ?
C7 C8 H8 108.6 . . ?
C10 C9 C15 117.9(3) . . ?
C10 C9 C16 119.2(3) . . ?
C15 C9 C16 122.5(3) . . ?
C9 C10 C11 123.1(3) . . ?
C9 C10 C8 125.5(3) . . ?
C11 C10 C8 111.4(3) . . ?
C10 C11 C13 119.6(3) . . ?
C10 C11 C12 110.3(3) . . ?
C13 C11 C12 130.0(3) . . ?
C29 C12 C11 115.5(3) . . ?
C29 C12 C7 113.2(3) . . ?
C11 C12 C7 101.5(3) . . ?
C29 C12 H12 108.8 . . ?
C11 C12 H12 108.8 . . ?
C7 C12 H12 108.8 . . ?
C11 C13 C14 117.7(3) . . ?
C11 C13 C27 123.3(3) . . ?
C14 C13 C27 118.9(3) . . ?
C15 C14 C13 122.4(3) . . ?
C15 C14 C25 116.5(3) . . ?
C13 C14 C25 121.1(3) . . ?
C14 C15 C9 119.2(3) . . ?
C14 C15 C19 120.4(3) . . ?
C9 C15 C19 120.3(3) . . ?
C9 C16 C17 113.6(3) . . ?
C9 C16 H16A 108.8 . . ?
C17 C16 H16A 108.8 . . ?
C9 C16 H16B 108.8 . . ?
C17 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C18 C17 C16 113.6(3) . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C16 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C8 C18 C17 108.0(3) . . ?
C8 C18 H18A 110.1 . . ?
C17 C18 H18A 110.1 . . ?
C8 C18 H18B 110.1 . . ?
C17 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
C20 C19 C24 118.3(3) . . ?
C20 C19 C15 121.9(3) . . ?
C24 C19 C15 119.7(3) . . ?
C21 C20 C19 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 120.3(4) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 119.3(4) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.5(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 120.8(4) . . ?
C23 C24 H24 119.6 . . ?
C19 C24 H24 119.6 . . ?
O1 C25 O2 124.9(3) . . ?
O1 C25 C14 124.8(3) . . ?
O2 C25 C14 110.2(3) . . ?
O2 C26 H26A 109.5 . . ?
O2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 C27 O4 123.1(3) . . ?
O3 C27 C13 126.6(3) . . ?
O4 C27 C13 110.3(3) . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C29 C30 117.6(3) . . ?
C34 C29 C12 121.2(3) . . ?
C30 C29 C12 121.2(3) . . ?
C31 C30 C29 122.3(3) . . ?
C31 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
C30 C31 C32 119.3(3) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 H31 120.3 . . ?
O5 C32 C31 125.0(3) . . ?
O5 C32 C33 115.3(3) . . ?
C31 C32 C33 119.6(3) . . ?
C34 C33 C32 120.4(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C29 120.8(3) . . ?
C33 C34 H34 119.6 . . ?
C29 C34 H34 119.6 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        28.25
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.065