# 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              ?
_publ_contact_author_email       henry@unistra.fr
_publ_contact_author_name        'Marc Henry'
loop_
_publ_author_name
'Marc Henry'
'Pierre Mobian'
'Clarisse Huguenard'

data_e926a
_database_code_depnum_ccdc_archive 'CCDC 817017'
#TrackingRef '- cifiles.txt'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18.67 H17.33 O1.33'
_chemical_formula_weight         262.99

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.4449(10)
_cell_length_b                   15.105(2)
_cell_length_c                   23.962(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2694.7(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9881
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10151
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.59
_reflns_number_total             5784
_reflns_number_gt                3488
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1791P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(3)
_refine_ls_number_reflns         5784
_refine_ls_number_parameters     277
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2723
_refine_ls_wR_factor_gt          0.2389
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002

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 0.0931(6) 0.1237(3) 0.52616(18) 0.0330(11) Uani 1 1 d . . .
C2 C -0.0392(7) 0.0603(3) 0.52169(19) 0.0376(11) Uani 1 1 d . . .
H2 H -0.0482 0.0264 0.4884 0.045 Uiso 1 1 calc R . .
C3 C -0.1587(6) 0.0452(4) 0.5645(2) 0.0401(12) Uani 1 1 d . . .
C4 C -0.1431(7) 0.0963(4) 0.6126(2) 0.0472(14) Uani 1 1 d . . .
H4 H -0.2251 0.0864 0.6423 0.057 Uiso 1 1 calc R . .
C5 C -0.0124(7) 0.1614(4) 0.6190(2) 0.0426(12) Uani 1 1 d . . .
C6 C 0.1062(7) 0.1743(3) 0.57469(19) 0.0376(11) Uani 1 1 d . . .
H6 H 0.1972 0.2181 0.5776 0.045 Uiso 1 1 calc R . .
C7 C -0.3022(7) -0.0267(4) 0.5596(2) 0.0526(14) Uani 1 1 d . . .
H7A H -0.3903 -0.0095 0.5312 0.079 Uiso 1 1 calc R . .
H7B H -0.3628 -0.0341 0.5956 0.079 Uiso 1 1 calc R . .
H7C H -0.2456 -0.0827 0.5487 0.079 Uiso 1 1 calc R . .
C8 C -0.0014(9) 0.2127(5) 0.6716(2) 0.0621(18) Uani 1 1 d . . .
H8A H -0.1072 0.2002 0.6946 0.093 Uiso 1 1 calc R . .
H8B H 0.0030 0.2761 0.6630 0.093 Uiso 1 1 calc R . .
H8C H 0.1074 0.1958 0.6920 0.093 Uiso 1 1 calc R . .
C9 C 0.2322(6) 0.1344(3) 0.48037(18) 0.0327(11) Uani 1 1 d . . .
C10 C 0.1847(6) 0.1380(3) 0.42416(18) 0.0310(10) Uani 1 1 d . . .
O1 O 0.0056(4) 0.1305(2) 0.41053(12) 0.0351(8) Uani 1 1 d . . .
H1 H -0.0248 0.1734 0.3903 0.053 Uiso 1 1 calc R . .
C11 C 0.3178(6) 0.1456(3) 0.38253(17) 0.0317(11) Uani 1 1 d . . .
C12 C 0.4960(6) 0.1545(3) 0.3981(2) 0.0373(11) Uani 1 1 d . . .
H12 H 0.5858 0.1614 0.3702 0.045 Uiso 1 1 calc R . .
C13 C 0.5446(7) 0.1533(4) 0.4540(2) 0.0400(12) Uani 1 1 d . . .
H13 H 0.6671 0.1585 0.4646 0.048 Uiso 1 1 calc R . .
C14 C 0.4117(7) 0.1444(3) 0.4945(2) 0.0384(12) Uani 1 1 d . . .
H14 H 0.4448 0.1452 0.5328 0.046 Uiso 1 1 calc R . .
C15 C 0.2645(5) 0.1391(3) 0.32233(17) 0.0296(10) Uani 1 1 d . . .
C16 C 0.2863(5) 0.2101(3) 0.28549(17) 0.0267(9) Uani 1 1 d . . .
O2 O 0.3588(4) 0.2863(2) 0.30641(12) 0.0314(7) Uani 1 1 d . . .
H2A H 0.3393 0.3281 0.2842 0.047 Uiso 1 1 calc R . .
C17 C 0.2313(5) 0.2025(3) 0.22921(17) 0.0279(10) Uani 1 1 d . . .
C18 C 0.1625(6) 0.1220(3) 0.21137(19) 0.0336(11) Uani 1 1 d . . .
H18 H 0.1312 0.1153 0.1732 0.040 Uiso 1 1 calc R . .
C19 C 0.1378(6) 0.0516(4) 0.24691(19) 0.0370(11) Uani 1 1 d . . .
H19 H 0.0860 -0.0021 0.2339 0.044 Uiso 1 1 calc R . .
C20 C 0.1906(6) 0.0605(3) 0.30288(19) 0.0358(11) Uani 1 1 d . . .
H20 H 0.1756 0.0122 0.3278 0.043 Uiso 1 1 calc R . .
C21 C 0.2463(6) 0.2786(3) 0.18935(18) 0.0313(11) Uani 1 1 d . . .
C22 C 0.1847(6) 0.3622(3) 0.20361(18) 0.0313(11) Uani 1 1 d . . .
H22 H 0.1357 0.3725 0.2396 0.038 Uiso 1 1 calc R . .
C23 C 0.1949(6) 0.4318(4) 0.1648(2) 0.0396(12) Uani 1 1 d . . .
C24 C 0.2677(6) 0.4155(4) 0.1121(2) 0.0407(12) Uani 1 1 d . . .
H24 H 0.2771 0.4625 0.0859 0.049 Uiso 1 1 calc R . .
C25 C 0.3267(7) 0.3313(4) 0.09738(19) 0.0396(12) Uani 1 1 d . . .
C26 C 0.3193(6) 0.2637(4) 0.13659(17) 0.0349(11) Uani 1 1 d . . .
H26 H 0.3644 0.2067 0.1274 0.042 Uiso 1 1 calc R . .
C27 C 0.1349(8) 0.5238(4) 0.1814(3) 0.0541(15) Uani 1 1 d . . .
H27A H 0.2231 0.5497 0.2070 0.081 Uiso 1 1 calc R . .
H27B H 0.0178 0.5203 0.1999 0.081 Uiso 1 1 calc R . .
H27C H 0.1249 0.5609 0.1480 0.081 Uiso 1 1 calc R . .
C28 C 0.4018(9) 0.3118(5) 0.0393(2) 0.0600(17) Uani 1 1 d . . .
H28A H 0.4260 0.3677 0.0199 0.090 Uiso 1 1 calc R . .
H28B H 0.3141 0.2773 0.0180 0.090 Uiso 1 1 calc R . .
H28C H 0.5136 0.2780 0.0428 0.090 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
C1 0.030(2) 0.039(3) 0.030(2) 0.0121(19) -0.0076(18) 0.000(2)
C2 0.036(3) 0.043(3) 0.033(2) 0.010(2) -0.0004(19) 0.003(2)
C3 0.031(2) 0.050(3) 0.039(3) 0.020(2) -0.001(2) 0.000(2)
C4 0.038(3) 0.062(4) 0.041(3) 0.019(3) 0.006(2) 0.003(3)
C5 0.039(3) 0.055(4) 0.034(2) 0.003(2) 0.000(2) 0.006(2)
C6 0.036(3) 0.041(3) 0.036(2) 0.006(2) 0.002(2) 0.002(2)
C7 0.036(3) 0.066(4) 0.055(3) 0.016(3) 0.003(2) -0.010(3)
C8 0.053(4) 0.085(5) 0.048(3) -0.007(3) 0.005(3) 0.015(3)
C9 0.031(3) 0.035(3) 0.031(2) 0.0035(19) -0.0002(19) -0.001(2)
C10 0.022(2) 0.039(3) 0.031(2) 0.0038(19) 0.0004(17) -0.002(2)
O1 0.0237(15) 0.051(2) 0.0303(16) 0.0094(14) -0.0036(12) -0.0005(15)
C11 0.026(2) 0.037(3) 0.031(2) 0.0081(19) -0.0008(18) 0.000(2)
C12 0.029(2) 0.044(3) 0.039(2) 0.008(2) 0.002(2) -0.005(2)
C13 0.026(2) 0.054(3) 0.040(3) 0.009(2) -0.006(2) -0.001(2)
C14 0.039(3) 0.045(3) 0.031(2) 0.010(2) -0.0059(19) -0.001(2)
C15 0.020(2) 0.041(3) 0.0274(19) 0.0022(19) 0.0031(16) 0.0024(18)
C16 0.0153(19) 0.036(3) 0.028(2) 0.0004(18) 0.0040(15) 0.0012(18)
O2 0.0316(16) 0.0362(19) 0.0264(15) 0.0021(13) -0.0008(13) -0.0048(14)
C17 0.020(2) 0.038(3) 0.026(2) -0.0012(18) 0.0013(16) -0.0001(18)
C18 0.030(2) 0.038(3) 0.033(2) -0.002(2) -0.0014(18) 0.000(2)
C19 0.035(3) 0.038(3) 0.038(2) -0.001(2) 0.000(2) 0.000(2)
C20 0.040(3) 0.032(3) 0.036(2) 0.004(2) -0.002(2) -0.007(2)
C21 0.021(2) 0.042(3) 0.031(2) 0.0016(18) -0.0055(17) 0.0020(19)
C22 0.021(2) 0.038(3) 0.035(2) -0.001(2) -0.0054(17) -0.0012(19)
C23 0.027(2) 0.047(3) 0.045(3) 0.004(2) -0.005(2) -0.004(2)
C24 0.032(3) 0.050(4) 0.040(3) 0.013(2) -0.001(2) -0.010(2)
C25 0.034(3) 0.051(4) 0.034(2) 0.006(2) 0.0023(19) -0.007(2)
C26 0.028(2) 0.048(3) 0.029(2) 0.002(2) -0.0008(17) -0.003(2)
C27 0.056(3) 0.037(3) 0.069(4) 0.012(3) -0.006(3) 0.009(3)
C28 0.056(4) 0.091(5) 0.033(3) 0.009(3) 0.007(2) -0.008(3)

_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 C2 1.378(7) . ?
C1 C6 1.395(7) . ?
C1 C9 1.518(7) . ?
C2 C3 1.377(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(8) . ?
C3 C7 1.529(8) . ?
C4 C5 1.392(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(7) . ?
C5 C8 1.482(8) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.387(7) . ?
C9 C10 1.394(6) . ?
C10 O1 1.378(5) . ?
C10 C11 1.411(6) . ?
O1 H1 0.8400 . ?
C11 C12 1.385(7) . ?
C11 C15 1.499(6) . ?
C12 C13 1.390(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(7) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.388(7) . ?
C15 C16 1.398(6) . ?
C16 O2 1.366(5) . ?
C16 C17 1.414(6) . ?
O2 H2A 0.8400 . ?
C17 C18 1.387(7) . ?
C17 C21 1.499(7) . ?
C18 C19 1.375(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.404(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.387(7) . ?
C21 C26 1.394(6) . ?
C22 C23 1.407(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(7) . ?
C23 C27 1.513(8) . ?
C24 C25 1.390(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(7) . ?
C25 C28 1.529(7) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
C2 C1 C6 119.7(4) . . ?
C2 C1 C9 120.4(4) . . ?
C6 C1 C9 119.8(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 118.1(5) . . ?
C2 C3 C7 120.7(5) . . ?
C4 C3 C7 121.2(4) . . ?
C3 C4 C5 122.8(5) . . ?
C3 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C4 C5 C6 117.2(5) . . ?
C4 C5 C8 120.1(5) . . ?
C6 C5 C8 122.7(5) . . ?
C5 C6 C1 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 118.5(4) . . ?
C14 C9 C1 119.5(4) . . ?
C10 C9 C1 122.0(4) . . ?
O1 C10 C9 118.1(4) . . ?
O1 C10 C11 121.3(4) . . ?
C9 C10 C11 120.6(4) . . ?
C10 O1 H1 109.5 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 C15 121.2(4) . . ?
C10 C11 C15 119.3(4) . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C9 C14 C13 121.7(4) . . ?
C9 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C20 C15 C16 119.3(4) . . ?
C20 C15 C11 119.0(4) . . ?
C16 C15 C11 121.8(4) . . ?
O2 C16 C15 117.4(4) . . ?
O2 C16 C17 122.2(4) . . ?
C15 C16 C17 120.4(4) . . ?
C16 O2 H2A 109.5 . . ?
C18 C17 C16 118.2(4) . . ?
C18 C17 C21 120.2(4) . . ?
C16 C17 C21 121.6(4) . . ?
C19 C18 C17 122.5(4) . . ?
C19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
C18 C19 C20 118.6(5) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C15 C20 C19 120.9(4) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C26 119.9(4) . . ?
C22 C21 C17 121.1(4) . . ?
C26 C21 C17 118.9(4) . . ?
C21 C22 C23 120.0(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 C27 121.1(5) . . ?
C22 C23 C27 119.8(5) . . ?
C25 C24 C23 120.9(5) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C26 C25 C24 119.2(4) . . ?
C26 C25 C28 119.3(5) . . ?
C24 C25 C28 121.5(5) . . ?
C25 C26 C21 120.7(5) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 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 . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.119


data_e998a
_database_code_depnum_ccdc_archive 'CCDC 817018'
#TrackingRef '- cifiles.txt'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C28 H26 O2'

_chemical_formula_sum            'C28 H26 O2'

_chemical_formula_weight         394.49

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'
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   P2(1)/n

_symmetry_space_group_name_Hall  '-P 2yn'

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                   7.9028(12)

_cell_length_b                   18.958(2)

_cell_length_c                   28.683(5)

_cell_angle_alpha                90.00

_cell_angle_beta                 91.060(3)

_cell_angle_gamma                90.00

_cell_volume                     4296.5(11)

_cell_formula_units_Z            8

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    943

_cell_measurement_theta_min      2.66

_cell_measurement_theta_max      21.49

_exptl_crystal_description       prism

_exptl_crystal_colour            colorless

_exptl_crystal_size_max          0.10

_exptl_crystal_size_mid          0.05

_exptl_crystal_size_min          0.05

_exptl_crystal_density_meas      none

_exptl_crystal_density_diffrn    1.220

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1680

_exptl_absorpt_coefficient_mu    0.075

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9925

_exptl_absorpt_correction_T_max  0.9963

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      173(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            30618

_diffrn_reflns_av_R_equivalents  0.0524

_diffrn_reflns_av_sigmaI/netI    0.0775

_diffrn_reflns_limit_h_min       -10

_diffrn_reflns_limit_h_max       10

_diffrn_reflns_limit_k_min       -24

_diffrn_reflns_limit_k_max       24

_diffrn_reflns_limit_l_min       -37

_diffrn_reflns_limit_l_max       31

_diffrn_reflns_theta_min         2.26

_diffrn_reflns_theta_max         27.49

_reflns_number_total             9829

_reflns_number_gt                5158

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'

_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    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;

_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.3971P] 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       0.0050(6)

_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^

_refine_ls_number_reflns         9829

_refine_ls_number_parameters     554

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.1240

_refine_ls_R_factor_gt           0.0544

_refine_ls_wR_factor_ref         0.1606

_refine_ls_wR_factor_gt          0.1297

_refine_ls_goodness_of_fit_ref   1.006

_refine_ls_restrained_S_all      1.006

_refine_ls_shift/su_max          0.027

_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 1.0981(3) 0.42617(12) 0.32645(8) 0.0331(5) Uani 1 1 d . . .
C2 C 1.2328(3) 0.37866(12) 0.32539(9) 0.0374(6) Uani 1 1 d . . .
H2A H 1.3164 0.3836 0.3022 0.045 Uiso 1 1 calc R . .
C3 C 1.2466(3) 0.32411(12) 0.35776(9) 0.0415(6) Uani 1 1 d . . .
C4 C 1.1227(4) 0.31749(13) 0.39097(9) 0.0463(7) Uani 1 1 d . . .
H4A H 1.1310 0.2801 0.4129 0.056 Uiso 1 1 calc R . .
C5 C 0.9861(3) 0.36378(13) 0.39332(9) 0.0424(6) Uani 1 1 d . . .
C6 C 0.9769(3) 0.41819(13) 0.36086(9) 0.0388(6) Uani 1 1 d . . .
H6 H 0.8857 0.4508 0.3621 0.047 Uiso 1 1 calc R . .
C7 C 1.3929(4) 0.27305(15) 0.35595(11) 0.0616(8) Uani 1 1 d . . .
H7A H 1.3836 0.2448 0.3274 0.092 Uiso 1 1 calc R . .
H7B H 1.3903 0.2418 0.3832 0.092 Uiso 1 1 calc R . .
H7C H 1.4996 0.2994 0.3561 0.092 Uiso 1 1 calc R . .
C8 C 0.8504(4) 0.35561(15) 0.42953(10) 0.0556(8) Uani 1 1 d . . .
H8A H 0.7422 0.3444 0.4140 0.083 Uiso 1 1 calc R . .
H8B H 0.8395 0.3998 0.4470 0.083 Uiso 1 1 calc R . .
H8C H 0.8817 0.3174 0.4510 0.083 Uiso 1 1 calc R . .
C9 C 1.0802(3) 0.48454(12) 0.29188(8) 0.0323(5) Uani 1 1 d . . .
C10 C 1.0914(3) 0.47268(11) 0.24391(8) 0.0307(5) Uani 1 1 d . . .
O1 O 1.1266(2) 0.40617(8) 0.22724(6) 0.0385(4) Uani 1 1 d . . .
H1 H 1.1280 0.3773 0.2494 0.058 Uiso 1 1 calc R . .
C11 C 1.0635(3) 0.52610(12) 0.21101(8) 0.0317(5) Uani 1 1 d . . .
C12 C 1.0245(3) 0.59294(12) 0.22794(9) 0.0403(6) Uani 1 1 d . . .
H12 H 1.0047 0.6303 0.2064 0.048 Uiso 1 1 calc R . .
C13 C 1.0138(3) 0.60637(13) 0.27499(9) 0.0433(6) Uani 1 1 d . . .
H13 H 0.9875 0.6525 0.2856 0.052 Uiso 1 1 calc R . .
C14 C 1.0414(3) 0.55255(12) 0.30668(9) 0.0401(6) Uani 1 1 d . . .
H14 H 1.0339 0.5621 0.3391 0.048 Uiso 1 1 calc R . .
C15 C 1.0803(3) 0.51554(12) 0.15972(8) 0.0319(5) Uani 1 1 d . . .
C16 C 1.0007(3) 0.46151(12) 0.13406(8) 0.0323(5) Uani 1 1 d . . .
O2 O 0.9021(2) 0.41145(9) 0.15529(6) 0.0390(4) Uani 1 1 d . . .
H2 H 0.9368 0.4054 0.1829 0.059 Uiso 1 1 calc R . .
C17 C 1.0135(3) 0.45679(12) 0.08560(8) 0.0342(5) Uani 1 1 d . . .
C18 C 1.1129(3) 0.50545(13) 0.06271(9) 0.0402(6) Uani 1 1 d . . .
H18 H 1.1255 0.5018 0.0299 0.048 Uiso 1 1 calc R . .
C19 C 1.1944(3) 0.55937(13) 0.08691(9) 0.0429(6) Uani 1 1 d . . .
H19 H 1.2613 0.5927 0.0707 0.051 Uiso 1 1 calc R . .
C20 C 1.1776(3) 0.56439(12) 0.13491(9) 0.0368(6) Uani 1 1 d . . .
H20 H 1.2330 0.6016 0.1513 0.044 Uiso 1 1 calc R . .
C21 C 0.9197(3) 0.40019(12) 0.05956(8) 0.0336(5) Uani 1 1 d . . .
C22 C 0.7433(3) 0.40399(14) 0.05486(8) 0.0395(6) Uani 1 1 d . . .
H22 H 0.6852 0.4430 0.0678 0.047 Uiso 1 1 calc R . .
C23 C 0.6511(3) 0.35166(14) 0.03150(8) 0.0412(6) Uani 1 1 d . . .
C24 C 0.7388(3) 0.29551(14) 0.01322(8) 0.0421(6) Uani 1 1 d . . .
H24 H 0.6775 0.2599 -0.0031 0.050 Uiso 1 1 calc R . .
C25 C 0.9135(3) 0.28913(14) 0.01783(9) 0.0431(6) Uani 1 1 d . . .
C26 C 1.0018(3) 0.34277(14) 0.04100(9) 0.0412(6) Uani 1 1 d . . .
H26 H 1.1215 0.3397 0.0441 0.049 Uiso 1 1 calc R . .
C27 C 0.4613(3) 0.35662(17) 0.02729(10) 0.0594(8) Uani 1 1 d . . .
H27A H 0.4303 0.3962 0.0069 0.089 Uiso 1 1 calc R . .
H27B H 0.4139 0.3642 0.0582 0.089 Uiso 1 1 calc R . .
H27C H 0.4161 0.3127 0.0140 0.089 Uiso 1 1 calc R . .
C28 C 1.0050(4) 0.22541(16) -0.00053(12) 0.0661(9) Uani 1 1 d . . .
H28A H 0.9935 0.1861 0.0214 0.099 Uiso 1 1 calc R . .
H28B H 1.1251 0.2367 -0.0041 0.099 Uiso 1 1 calc R . .
H28C H 0.9559 0.2120 -0.0309 0.099 Uiso 1 1 calc R . .
C29 C 0.5675(3) 0.54417(12) 0.20160(8) 0.0327(5) Uani 1 1 d . . .
C30 C 0.5009(3) 0.59310(12) 0.23251(9) 0.0377(6) Uani 1 1 d . . .
H30 H 0.4509 0.5771 0.2605 0.045 Uiso 1 1 calc R . .
C31 C 0.5066(3) 0.66527(13) 0.22296(9) 0.0427(6) Uani 1 1 d . . .
C32 C 0.5786(3) 0.68707(13) 0.18160(10) 0.0465(7) Uani 1 1 d . . .
H32 H 0.5836 0.7361 0.1750 0.056 Uiso 1 1 calc R . .
C33 C 0.6438(3) 0.63972(13) 0.14948(9) 0.0420(6) Uani 1 1 d . . .
C34 C 0.6371(3) 0.56827(12) 0.16028(9) 0.0367(6) Uani 1 1 d . . .
H34 H 0.6811 0.5350 0.1389 0.044 Uiso 1 1 calc R . .
C35 C 0.4346(4) 0.71791(14) 0.25677(11) 0.0592(8) Uani 1 1 d . . .
H35A H 0.4660 0.7658 0.2473 0.089 Uiso 1 1 calc R . .
H35B H 0.4802 0.7085 0.2882 0.089 Uiso 1 1 calc R . .
H35C H 0.3110 0.7137 0.2568 0.089 Uiso 1 1 calc R . .
C36 C 0.7221(4) 0.66363(15) 0.10493(10) 0.0623(8) Uani 1 1 d . . .
H36A H 0.8166 0.6324 0.0974 0.093 Uiso 1 1 calc R . .
H36B H 0.7639 0.7120 0.1087 0.093 Uiso 1 1 calc R . .
H36C H 0.6371 0.6621 0.0796 0.093 Uiso 1 1 calc R . .
C37 C 0.5750(3) 0.46809(12) 0.21312(8) 0.0315(5) Uani 1 1 d . . .
C38 C 0.5165(3) 0.41640(11) 0.18171(8) 0.0299(5) Uani 1 1 d . . .
O3 O 0.4376(2) 0.43305(8) 0.14025(6) 0.0379(4) Uani 1 1 d . . .
H3 H 0.4111 0.4760 0.1402 0.057 Uiso 1 1 calc R . .
C39 C 0.5417(3) 0.34455(12) 0.19041(8) 0.0316(5) Uani 1 1 d . . .
C40 C 0.6242(3) 0.32499(12) 0.23169(8) 0.0373(6) Uani 1 1 d . . .
H40 H 0.6430 0.2764 0.2380 0.045 Uiso 1 1 calc R . .
C41 C 0.6794(3) 0.37485(13) 0.26374(9) 0.0396(6) Uani 1 1 d . . .
H41 H 0.7341 0.3606 0.2920 0.048 Uiso 1 1 calc R . .
C42 C 0.6541(3) 0.44572(12) 0.25430(8) 0.0362(6) Uani 1 1 d . . .
H42 H 0.6916 0.4799 0.2764 0.043 Uiso 1 1 calc R . .
C43 C 0.4816(3) 0.29008(11) 0.15629(8) 0.0316(5) Uani 1 1 d . . .
C44 C 0.5982(3) 0.24674(11) 0.13414(8) 0.0303(5) Uani 1 1 d . . .
O4 O 0.76955(19) 0.25879(8) 0.13887(6) 0.0396(4) Uani 1 1 d . . .
H4 H 0.7864 0.3015 0.1453 0.059 Uiso 1 1 calc R . .
C45 C 0.5435(3) 0.18957(11) 0.10663(8) 0.0329(5) Uani 1 1 d . . .
C46 C 0.3691(3) 0.18062(12) 0.09937(8) 0.0361(6) Uani 1 1 d . . .
H46 H 0.3299 0.1426 0.0805 0.043 Uiso 1 1 calc R . .
C47 C 0.2528(3) 0.22564(12) 0.11885(9) 0.0396(6) Uani 1 1 d . . .
H47 H 0.1352 0.2193 0.1127 0.048 Uiso 1 1 calc R . .
C48 C 0.3088(3) 0.28008(12) 0.14740(8) 0.0366(6) Uani 1 1 d . . .
H48 H 0.2290 0.3109 0.1611 0.044 Uiso 1 1 calc R . .
C49 C 0.6659(3) 0.13669(11) 0.08649(8) 0.0340(5) Uani 1 1 d . . .
C50 C 0.7969(3) 0.10988(12) 0.11430(9) 0.0391(6) Uani 1 1 d . . .
H50 H 0.8169 0.1290 0.1445 0.047 Uiso 1 1 calc R . .
C51 C 0.8984(3) 0.05587(13) 0.09856(9) 0.0401(6) Uani 1 1 d . . .
C52 C 0.8654(3) 0.02888(13) 0.05407(9) 0.0414(6) Uani 1 1 d . . .
H52 H 0.9330 -0.0088 0.0430 0.050 Uiso 1 1 calc R . .
C53 C 0.7359(3) 0.05553(13) 0.02538(9) 0.0405(6) Uani 1 1 d . . .
C54 C 0.6360(3) 0.10951(12) 0.04280(9) 0.0393(6) Uani 1 1 d . . .
H54 H 0.5457 0.1278 0.0241 0.047 Uiso 1 1 calc R . .
C55 C 1.0385(4) 0.02582(16) 0.12909(10) 0.0561(8) Uani 1 1 d . . .
H55A H 1.0839 0.0629 0.1496 0.084 Uiso 1 1 calc R . .
H55B H 1.1288 0.0077 0.1095 0.084 Uiso 1 1 calc R . .
H55C H 0.9936 -0.0126 0.1481 0.084 Uiso 1 1 calc R . .
C56 C 0.7065(3) 0.02727(15) -0.02342(9) 0.0503(7) Uani 1 1 d . . .
H56A H 0.5846 0.0236 -0.0299 0.075 Uiso 1 1 calc R . .
H56B H 0.7584 -0.0195 -0.0260 0.075 Uiso 1 1 calc R . .
H56C H 0.7574 0.0594 -0.0460 0.075 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

C1 0.0391(13) 0.0301(13) 0.0298(13) -0.0051(10) -0.0067(10) -0.0050(10)
C2 0.0425(14) 0.0320(13) 0.0375(14) -0.0040(11) -0.0045(11) -0.0035(11)
C3 0.0498(15) 0.0333(14) 0.0410(15) -0.0022(11) -0.0093(13) -0.0016(11)
C4 0.0641(18) 0.0359(15) 0.0386(15) 0.0040(12) -0.0092(14) -0.0059(13)
C5 0.0544(16) 0.0368(14) 0.0358(15) -0.0018(12) -0.0032(12) -0.0105(12)
C6 0.0432(14) 0.0369(14) 0.0363(14) -0.0042(11) -0.0037(11) -0.0034(11)
C7 0.069(2) 0.0470(17) 0.068(2) 0.0063(15) -0.0117(17) 0.0134(15)
C8 0.071(2) 0.0539(18) 0.0422(17) 0.0004(13) 0.0078(15) -0.0100(15)
C9 0.0317(12) 0.0304(13) 0.0349(14) -0.0037(10) -0.0020(10) -0.0011(10)
C10 0.0312(12) 0.0244(12) 0.0363(13) -0.0042(10) -0.0015(10) 0.0000(9)
O1 0.0531(10) 0.0275(9) 0.0347(10) -0.0019(7) -0.0007(8) 0.0052(8)
C11 0.0314(12) 0.0287(12) 0.0349(13) -0.0002(10) -0.0008(10) -0.0009(10)
C12 0.0475(15) 0.0307(13) 0.0425(16) 0.0004(11) -0.0015(12) 0.0019(11)
C13 0.0531(16) 0.0306(14) 0.0461(16) -0.0080(12) -0.0034(13) 0.0056(11)
C14 0.0478(15) 0.0346(14) 0.0379(15) -0.0069(11) -0.0009(12) 0.0011(11)
C15 0.0301(11) 0.0309(13) 0.0347(13) 0.0026(10) -0.0006(10) 0.0046(10)
C16 0.0295(11) 0.0341(13) 0.0332(13) 0.0016(11) 0.0010(10) -0.0035(10)
O2 0.0387(9) 0.0464(10) 0.0321(9) -0.0002(8) 0.0025(8) -0.0116(8)
C17 0.0287(11) 0.0410(14) 0.0328(14) 0.0022(11) -0.0020(10) 0.0011(10)
C18 0.0358(13) 0.0517(16) 0.0329(14) 0.0094(12) -0.0029(11) -0.0036(12)
C19 0.0408(14) 0.0456(15) 0.0422(16) 0.0139(12) 0.0002(12) -0.0071(12)
C20 0.0345(13) 0.0333(13) 0.0426(15) 0.0061(11) -0.0044(11) 0.0002(10)
C21 0.0318(12) 0.0435(14) 0.0256(12) 0.0032(10) -0.0013(10) -0.0042(11)
C22 0.0329(12) 0.0550(16) 0.0305(14) -0.0041(12) -0.0007(10) -0.0003(11)
C23 0.0323(13) 0.0593(17) 0.0318(14) -0.0011(12) -0.0016(11) -0.0055(12)
C24 0.0411(14) 0.0570(17) 0.0280(13) -0.0042(12) -0.0020(11) -0.0128(13)
C25 0.0407(14) 0.0515(16) 0.0371(15) -0.0053(13) 0.0041(12) -0.0024(12)
C26 0.0311(12) 0.0525(16) 0.0401(15) 0.0000(12) 0.0022(11) -0.0016(12)
C27 0.0324(14) 0.094(2) 0.0513(18) -0.0139(16) -0.0066(13) -0.0091(14)
C28 0.0575(18) 0.066(2) 0.075(2) -0.0257(17) 0.0018(17) -0.0006(15)
C29 0.0320(12) 0.0291(13) 0.0367(14) -0.0027(10) -0.0054(10) -0.0013(10)
C30 0.0406(13) 0.0363(14) 0.0360(14) -0.0034(11) -0.0025(11) 0.0040(11)
C31 0.0490(15) 0.0329(14) 0.0458(16) -0.0078(12) -0.0092(13) 0.0042(12)
C32 0.0523(16) 0.0303(14) 0.0563(18) 0.0026(13) -0.0145(14) -0.0024(12)
C33 0.0424(14) 0.0370(15) 0.0464(16) 0.0065(12) -0.0064(12) -0.0038(11)
C34 0.0341(13) 0.0347(14) 0.0411(15) -0.0013(11) -0.0022(11) -0.0009(10)
C35 0.075(2) 0.0384(16) 0.064(2) -0.0145(14) -0.0064(16) 0.0089(14)
C36 0.070(2) 0.0544(18) 0.062(2) 0.0163(16) 0.0019(17) -0.0105(15)
C37 0.0294(11) 0.0304(12) 0.0346(13) -0.0036(10) 0.0024(10) 0.0005(10)
C38 0.0268(11) 0.0315(12) 0.0315(13) 0.0014(10) 0.0001(10) 0.0018(9)
O3 0.0434(9) 0.0315(9) 0.0385(10) -0.0009(8) -0.0088(8) 0.0052(8)
C39 0.0314(12) 0.0301(13) 0.0335(13) 0.0000(10) 0.0027(10) -0.0003(10)
C40 0.0437(14) 0.0313(13) 0.0369(14) 0.0010(11) -0.0010(11) -0.0017(11)
C41 0.0460(15) 0.0379(14) 0.0347(14) 0.0011(11) -0.0052(11) -0.0009(11)
C42 0.0400(13) 0.0354(14) 0.0331(14) -0.0054(11) 0.0003(11) -0.0016(11)
C43 0.0355(12) 0.0275(12) 0.0317(13) 0.0039(10) -0.0013(10) -0.0008(10)
C44 0.0305(12) 0.0294(12) 0.0311(13) 0.0029(10) -0.0032(10) -0.0012(9)
O4 0.0343(9) 0.0364(10) 0.0481(11) -0.0063(8) -0.0015(8) -0.0031(7)
C45 0.0368(13) 0.0274(12) 0.0345(13) 0.0008(10) -0.0010(10) -0.0005(10)
C46 0.0417(14) 0.0287(13) 0.0377(14) 0.0001(10) -0.0041(11) -0.0030(10)
C47 0.0331(13) 0.0380(14) 0.0476(16) -0.0016(12) -0.0027(11) -0.0032(11)
C48 0.0354(13) 0.0335(13) 0.0409(14) -0.0014(11) 0.0023(11) -0.0001(10)
C49 0.0443(14) 0.0224(12) 0.0348(14) 0.0018(10) -0.0089(11) -0.0043(10)
C50 0.0401(14) 0.0417(15) 0.0354(14) -0.0034(11) -0.0020(11) 0.0011(11)
C51 0.0432(14) 0.0423(15) 0.0346(14) 0.0034(12) -0.0005(11) 0.0075(12)
C52 0.0423(14) 0.0420(14) 0.0399(15) -0.0025(12) 0.0029(12) 0.0064(12)
C53 0.0426(14) 0.0423(15) 0.0366(14) -0.0049(12) -0.0007(12) 0.0010(12)
C54 0.0420(14) 0.0367(14) 0.0392(15) 0.0011(11) -0.0025(11) 0.0036(11)
C55 0.0535(17) 0.072(2) 0.0426(17) 0.0024(15) -0.0013(13) 0.0269(15)
C56 0.0505(16) 0.0571(17) 0.0433(16) -0.0134(14) -0.0011(13) 0.0060(13)

_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 C2 1.395(3) . ?
C1 C6 1.397(3) . ?
C1 C9 1.491(3) . ?
C2 C3 1.393(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.384(4) . ?
C3 C7 1.509(4) . ?
C4 C5 1.394(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.390(3) . ?
C5 C8 1.515(4) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.393(3) . ?
C9 C10 1.399(3) . ?
C10 O1 1.379(2) . ?
C10 C11 1.399(3) . ?
O1 H1 0.8400 . ?
C11 C12 1.394(3) . ?
C11 C15 1.493(3) . ?
C12 C13 1.377(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.403(3) . ?
C15 C20 1.406(3) . ?
C16 O2 1.377(3) . ?
C16 C17 1.398(3) . ?
O2 H2 0.8400 . ?
C17 C18 1.385(3) . ?
C17 C21 1.496(3) . ?
C18 C19 1.387(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.379(3) . ?
C21 C22 1.400(3) . ?
C22 C23 1.395(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(3) . ?
C23 C27 1.506(3) . ?
C24 C25 1.390(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(3) . ?
C25 C28 1.508(4) . ?
C26 H26 0.9500 . ?
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 C34 1.393(3) . ?
C29 C30 1.393(3) . ?
C29 C37 1.481(3) . ?
C30 C31 1.396(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(4) . ?
C31 C35 1.510(4) . ?
C32 C33 1.392(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(3) . ?
C33 C36 1.500(4) . ?
C34 H34 0.9500 . ?
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 C42 1.392(3) . ?
C37 C38 1.404(3) . ?
C38 O3 1.370(3) . ?
C38 C39 1.398(3) . ?
O3 H3 0.8400 . ?
C39 C40 1.391(3) . ?
C39 C43 1.494(3) . ?
C40 C41 1.383(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.396(3) . ?
C43 C48 1.397(3) . ?
C44 O4 1.377(3) . ?
C44 C45 1.404(3) . ?
O4 H4 0.8400 . ?
C45 C46 1.400(3) . ?
C45 C49 1.515(3) . ?
C46 C47 1.380(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(3) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.371(3) . ?
C49 C50 1.392(3) . ?
C50 C51 1.381(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.395(3) . ?
C51 C55 1.510(3) . ?
C52 C53 1.396(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.391(3) . ?
C53 C56 1.513(3) . ?
C54 H54 0.9500 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 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

C2 C1 C6 118.6(2) . . ?
C2 C1 C9 121.9(2) . . ?
C6 C1 C9 119.5(2) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C4 C3 C2 118.6(2) . . ?
C4 C3 C7 121.2(2) . . ?
C2 C3 C7 120.2(3) . . ?
C3 C4 C5 122.3(2) . . ?
C3 C4 H4A 118.8 . . ?
C5 C4 H4A 118.8 . . ?
C6 C5 C4 117.8(2) . . ?
C6 C5 C8 120.4(2) . . ?
C4 C5 C8 121.8(2) . . ?
C5 C6 C1 121.7(2) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 117.8(2) . . ?
C14 C9 C1 120.2(2) . . ?
C10 C9 C1 121.9(2) . . ?
O1 C10 C9 120.3(2) . . ?
O1 C10 C11 117.3(2) . . ?
C9 C10 C11 122.4(2) . . ?
C10 O1 H1 109.5 . . ?
C12 C11 C10 117.2(2) . . ?
C12 C11 C15 119.3(2) . . ?
C10 C11 C15 123.5(2) . . ?
C13 C12 C11 121.8(2) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C9 121.1(2) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
C16 C15 C20 117.3(2) . . ?
C16 C15 C11 124.6(2) . . ?
C20 C15 C11 118.0(2) . . ?
O2 C16 C17 116.6(2) . . ?
O2 C16 C15 121.5(2) . . ?
C17 C16 C15 121.9(2) . . ?
C16 O2 H2 109.5 . . ?
C18 C17 C16 118.7(2) . . ?
C18 C17 C21 121.4(2) . . ?
C16 C17 C21 119.9(2) . . ?
C17 C18 C19 121.0(2) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C20 119.6(2) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C15 121.3(2) . . ?
C19 C20 H20 119.3 . . ?
C15 C20 H20 119.3 . . ?
C26 C21 C22 118.6(2) . . ?
C26 C21 C17 121.8(2) . . ?
C22 C21 C17 119.6(2) . . ?
C23 C22 C21 121.3(2) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C24 C23 C22 118.0(2) . . ?
C24 C23 C27 121.6(2) . . ?
C22 C23 C27 120.3(2) . . ?
C23 C24 C25 122.4(2) . . ?
C23 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C24 C25 C26 118.0(2) . . ?
C24 C25 C28 121.2(2) . . ?
C26 C25 C28 120.8(2) . . ?
C21 C26 C25 121.6(2) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 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 . . ?
C34 C29 C30 118.9(2) . . ?
C34 C29 C37 119.6(2) . . ?
C30 C29 C37 121.4(2) . . ?
C29 C30 C31 120.9(2) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C32 C31 C30 118.3(2) . . ?
C32 C31 C35 121.2(2) . . ?
C30 C31 C35 120.5(3) . . ?
C31 C32 C33 122.4(2) . . ?
C31 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C34 C33 C32 117.7(2) . . ?
C34 C33 C36 120.1(2) . . ?
C32 C33 C36 122.2(2) . . ?
C33 C34 C29 121.8(2) . . ?
C33 C34 H34 119.1 . . ?
C29 C34 H34 119.1 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 118.0(2) . . ?
C42 C37 C29 120.1(2) . . ?
C38 C37 C29 121.7(2) . . ?
O3 C38 C39 116.14(19) . . ?
O3 C38 C37 122.40(19) . . ?
C39 C38 C37 121.4(2) . . ?
C38 O3 H3 109.5 . . ?
C40 C39 C38 118.3(2) . . ?
C40 C39 C43 120.8(2) . . ?
C38 C39 C43 120.9(2) . . ?
C41 C40 C39 121.4(2) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C40 C41 C42 119.4(2) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C41 C42 C37 121.5(2) . . ?
C41 C42 H42 119.3 . . ?
C37 C42 H42 119.3 . . ?
C44 C43 C48 119.2(2) . . ?
C44 C43 C39 120.01(19) . . ?
C48 C43 C39 120.7(2) . . ?
O4 C44 C43 120.90(19) . . ?
O4 C44 C45 118.4(2) . . ?
C43 C44 C45 120.7(2) . . ?
C44 O4 H4 109.5 . . ?
C46 C45 C44 118.0(2) . . ?
C46 C45 C49 119.8(2) . . ?
C44 C45 C49 122.2(2) . . ?
C47 C46 C45 121.7(2) . . ?
C47 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?
C46 C47 C48 119.5(2) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C47 C48 C43 120.7(2) . . ?
C47 C48 H48 119.7 . . ?
C43 C48 H48 119.7 . . ?
C54 C49 C50 120.0(2) . . ?
C54 C49 C45 119.8(2) . . ?
C50 C49 C45 119.8(2) . . ?
C51 C50 C49 120.9(2) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C52 118.1(2) . . ?
C50 C51 C55 120.9(2) . . ?
C52 C51 C55 121.0(2) . . ?
C51 C52 C53 122.0(2) . . ?
C51 C52 H52 119.0 . . ?
C53 C52 H52 119.0 . . ?
C54 C53 C52 118.0(2) . . ?
C54 C53 C56 121.0(2) . . ?
C52 C53 C56 121.1(2) . . ?
C49 C54 C53 121.0(2) . . ?
C49 C54 H54 119.5 . . ?
C53 C54 H54 119.5 . . ?
C51 C55 H55A 109.5 . . ?
C51 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C51 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        27.49

_diffrn_measured_fraction_theta_full 0.996

_refine_diff_density_max         0.459

_refine_diff_density_min         -0.242

_refine_diff_density_rms         0.054