
data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Prof Min Shi'
_publ_contact_author_address     
;
State Key Laboratory of Organometallic Chemistry
Shanghai Institute of Organic Chemistry
354 Fenglin Lu
Shanghai
200032
CHINA
;

_publ_contact_author_email       MSHI@MAIL.SIOC.AC.CN

_publ_section_title              
;
Carbolithiation of gem-Aryl Disubstituted
Methylenecyclopropanes
;
loop_
_publ_author_name
'Min Shi'
'Jin-Wen Huang'

data_cd2493
_database_code_depnum_ccdc_archive 'CCDC 246793'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H36 O2'
_chemical_formula_weight         548.69

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   P2(1)2(1)2(1)

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'

_cell_length_a                   10.113(2)
_cell_length_b                   10.206(2)
_cell_length_c                   29.277(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3021.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    652
_cell_measurement_theta_min      4.866
_cell_measurement_theta_max      25.027

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.81329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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            18167
_diffrn_reflns_av_R_equivalents  0.1626
_diffrn_reflns_av_sigmaI/netI    0.3332
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         28.13
_reflns_number_total             6835
_reflns_number_gt                1918
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² 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/[σ²(Fo²)+(0.0101P)²+0.0000P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_number_reflns         6835
_refine_ls_number_parameters     413
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2113
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   0.635
_refine_ls_restrained_S_all      0.636
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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 0.0823(2) 0.5656(3) 0.04091(10) 0.0544(10) Uani 1 1 d . . .
H1 H 0.1312 0.5812 0.0192 0.082 Uiso 1 1 calc R . .
O2 O 0.6772(3) 0.7495(3) 0.04193(10) 0.0520(9) Uani 1 1 d . . .
C1 C 0.1679(4) 0.3851(4) 0.28262(17) 0.0397(12) Uani 1 1 d . . .
C2 C 0.1134(4) 0.3622(5) 0.24245(16) 0.0423(13) Uani 1 1 d . . .
C3 C -0.0115(5) 0.3525(6) 0.21643(18) 0.0528(15) Uani 1 1 d D . .
C4 C 0.1253(5) 0.3478(5) 0.19265(16) 0.0424(13) Uani 1 1 d . . .
C5 C 0.1696(4) 0.4611(5) 0.16254(15) 0.0372(12) Uani 1 1 d . . .
C6 C 0.1748(6) 0.5943(6) 0.18640(18) 0.0557(15) Uani 1 1 d D . .
C7 C 0.3026(5) 0.5215(5) 0.17701(17) 0.0504(14) Uani 1 1 d D . .
C8 C 0.1270(4) 0.4504(4) 0.11146(15) 0.0348(12) Uani 1 1 d . . .
C9 C 0.1558(5) 0.5783(5) 0.08310(16) 0.0384(12) Uani 1 1 d D . .
C10 C 0.2967(4) 0.6163(4) 0.07298(14) 0.0346(12) Uani 1 1 d . . .
C11 C 0.3770(4) 0.5467(4) 0.04395(14) 0.0394(12) Uani 1 1 d . . .
H11 H 0.3446 0.4698 0.0311 0.047 Uiso 1 1 calc R . .
C12 C 0.5051(4) 0.5863(4) 0.03291(14) 0.0392(13) Uani 1 1 d . . .
H12 H 0.5571 0.5365 0.0133 0.047 Uiso 1 1 calc R . .
C13 C 0.5524(4) 0.6988(5) 0.05141(15) 0.0398(12) Uani 1 1 d . . .
C14 C 0.4766(4) 0.7737(4) 0.08110(14) 0.0441(13) Uani 1 1 d . . .
H14 H 0.5104 0.8494 0.0943 0.053 Uiso 1 1 calc R . .
C15 C 0.3492(4) 0.7323(4) 0.09040(15) 0.0440(13) Uani 1 1 d . . .
H15 H 0.2962 0.7840 0.1091 0.053 Uiso 1 1 calc R . .
C16 C 0.7689(4) 0.6611(4) 0.02020(15) 0.0536(14) Uani 1 1 d . . .
H16A H 0.7733 0.5809 0.0373 0.080 Uiso 1 1 calc R . .
H16B H 0.8550 0.7007 0.0192 0.080 Uiso 1 1 calc R . .
H16C H 0.7395 0.6427 -0.0103 0.080 Uiso 1 1 calc R . .
C17 C 0.0918(4) 0.4135(4) 0.32414(16) 0.0432(13) Uani 1 1 d . . .
C18 C -0.0375(4) 0.4653(4) 0.32091(15) 0.0482(13) Uani 1 1 d . . .
H18 H -0.0744 0.4815 0.2924 0.058 Uiso 1 1 calc R . .
C19 C -0.1097(4) 0.4920(4) 0.36008(16) 0.0499(14) Uani 1 1 d . . .
H19 H -0.1947 0.5261 0.3575 0.060 Uiso 1 1 calc R . .
C20 C -0.0575(5) 0.4689(5) 0.40274(17) 0.0575(15) Uani 1 1 d . . .
H20 H -0.1063 0.4870 0.4289 0.069 Uiso 1 1 calc R . .
C21 C 0.0705(5) 0.4174(5) 0.40597(16) 0.0572(15) Uani 1 1 d . . .
H21 H 0.1072 0.4007 0.4345 0.069 Uiso 1 1 calc R . .
C22 C 0.1417(4) 0.3917(4) 0.36736(16) 0.0503(14) Uani 1 1 d . . .
H22 H 0.2269 0.3584 0.3703 0.060 Uiso 1 1 calc R . .
C23 C 0.3179(5) 0.3869(5) 0.28612(15) 0.0414(13) Uani 1 1 d . . .
C24 C 0.3838(5) 0.4927(5) 0.30488(15) 0.0547(15) Uani 1 1 d . . .
H24 H 0.3357 0.5623 0.3169 0.066 Uiso 1 1 calc R . .
C25 C 0.5201(6) 0.4963(6) 0.30599(17) 0.0735(19) Uani 1 1 d . . .
H25 H 0.5630 0.5679 0.3189 0.088 Uiso 1 1 calc R . .
C26 C 0.5932(6) 0.3943(7) 0.2880(2) 0.085(2) Uani 1 1 d . . .
H26 H 0.6851 0.3976 0.2883 0.102 Uiso 1 1 calc R . .
C27 C 0.5288(5) 0.2878(6) 0.26989(17) 0.0743(19) Uani 1 1 d . . .
H27 H 0.5769 0.2179 0.2581 0.089 Uiso 1 1 calc R . .
C28 C 0.3905(5) 0.2850(5) 0.26928(16) 0.0569(15) Uani 1 1 d . . .
H28 H 0.3472 0.2124 0.2572 0.068 Uiso 1 1 calc R . .
C29 C 0.1985(4) 0.3353(4) 0.08716(15) 0.0365(12) Uani 1 1 d . . .
C30 C 0.3147(4) 0.2814(4) 0.10471(15) 0.0430(13) Uani 1 1 d . . .
H30 H 0.3439 0.3065 0.1335 0.052 Uiso 1 1 calc R . .
C31 C 0.3869(5) 0.1914(5) 0.07983(18) 0.0575(16) Uani 1 1 d . . .
H31 H 0.4641 0.1567 0.0922 0.069 Uiso 1 1 calc R . .
C32 C 0.3466(5) 0.1523(5) 0.0373(2) 0.0634(17) Uani 1 1 d . . .
H32 H 0.3964 0.0927 0.0206 0.076 Uiso 1 1 calc R . .
C33 C 0.2314(5) 0.2027(5) 0.01982(16) 0.0580(16) Uani 1 1 d . . .
H33 H 0.2024 0.1767 -0.0089 0.070 Uiso 1 1 calc R . .
C34 C 0.1579(4) 0.2927(5) 0.04498(16) 0.0477(14) Uani 1 1 d . . .
H34 H 0.0793 0.3248 0.0329 0.057 Uiso 1 1 calc R . .
C35 C -0.0244(4) 0.4295(5) 0.11317(14) 0.0384(12) Uani 1 1 d . . .
C36 C -0.0837(4) 0.3085(5) 0.10801(14) 0.0472(14) Uani 1 1 d . . .
H36 H -0.0324 0.2359 0.1007 0.057 Uiso 1 1 calc R . .
C37 C -0.2214(5) 0.2941(6) 0.11380(18) 0.0695(18) Uani 1 1 d . . .
H37 H -0.2604 0.2129 0.1085 0.083 Uiso 1 1 calc R . .
C38 C -0.2970(5) 0.3951(6) 0.12672(18) 0.0702(19) Uani 1 1 d . . .
H38 H -0.3869 0.3829 0.1318 0.084 Uiso 1 1 calc R . .
C39 C -0.2421(5) 0.5159(6) 0.13247(17) 0.0614(16) Uani 1 1 d . . .
H39 H -0.2954 0.5862 0.1408 0.074 Uiso 1 1 calc R . .
C40 C -0.1075(5) 0.5349(5) 0.12610(15) 0.0528(14) Uani 1 1 d . . .
H40 H -0.0715 0.6179 0.1304 0.063 Uiso 1 1 calc R . .
H1' H -0.043(3) 0.268(3) 0.2167(12) 0.026(12) Uiso 1 1 d . . .
H2 H -0.060(4) 0.434(3) 0.2092(13) 0.066(17) Uiso 1 1 d D . .
H3 H 0.155(3) 0.264(3) 0.1822(11) 0.030(12) Uiso 1 1 d . . .
H4 H 0.146(3) 0.583(3) 0.2166(7) 0.036(12) Uiso 1 1 d D . .
H5 H 0.163(4) 0.671(3) 0.1674(12) 0.060(16) Uiso 1 1 d D . .
H6 H 0.342(4) 0.471(4) 0.2027(11) 0.082(18) Uiso 1 1 d D . .
H7 H 0.346(3) 0.563(3) 0.1504(8) 0.021(11) Uiso 1 1 d D . .
H8 H 0.114(3) 0.645(2) 0.1010(9) 0.001(9) Uiso 1 1 d D . .


_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 C9 1.447(5) . ?
O1 H1 0.8200 . ?
O2 C13 1.393(5) . ?
O2 C16 1.442(4) . ?
C1 C2 1.320(6) . ?
C1 C17 1.468(6) . ?
C1 C23 1.521(5) . ?
C2 C4 1.470(6) . ?
C2 C3 1.478(7) . ?
C3 C4 1.549(6) . ?
C3 H1 0.92(3) . ?
C3 H2 0.986(18) . ?
C4 C5 1.521(6) . ?
C4 H3 0.96(3) . ?
C5 C6 1.530(6) . ?
C5 C7 1.539(6) . ?
C5 C8 1.560(5) . ?
C6 C7 1.515(7) . ?
C6 H4 0.939(18) . ?
C6 H5 0.970(18) . ?
C7 H6 0.999(18) . ?
C7 H7 0.988(17) . ?
C8 C35 1.547(5) . ?
C8 C29 1.552(6) . ?
C8 C9 1.574(6) . ?
C9 C10 1.507(6) . ?
C9 H8 0.957(17) . ?
C10 C11 1.373(5) . ?
C10 C15 1.393(5) . ?
C11 C12 1.395(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.357(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(5) . ?
C14 C15 1.383(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C22 1.380(6) . ?
C17 C18 1.414(5) . ?
C18 C19 1.387(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.376(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.400(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.365(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C28 1.365(6) . ?
C23 C24 1.383(6) . ?
C24 C25 1.379(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.381(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.374(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.400(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.372(5) . ?
C29 C30 1.395(6) . ?
C30 C31 1.382(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.369(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.372(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.393(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.381(5) . ?
C35 C40 1.417(6) . ?
C36 C37 1.411(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.338(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.361(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.388(6) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?

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
C9 O1 H1 109.5 . . ?
C13 O2 C16 116.0(3) . . ?
C2 C1 C17 123.7(4) . . ?
C2 C1 C23 118.6(4) . . ?
C17 C1 C23 117.7(4) . . ?
C1 C2 C4 150.1(5) . . ?
C1 C2 C3 145.9(5) . . ?
C4 C2 C3 63.4(3) . . ?
C2 C3 C4 58.1(3) . . ?
C2 C3 H1 111(2) . . ?
C4 C3 H1 107(2) . . ?
C2 C3 H2 119(3) . . ?
C4 C3 H2 112(2) . . ?
H1 C3 H2 128(3) . . ?
C2 C4 C5 121.5(4) . . ?
C2 C4 C3 58.6(3) . . ?
C5 C4 C3 120.0(5) . . ?
C2 C4 H3 116(2) . . ?
C5 C4 H3 113(2) . . ?
C3 C4 H3 117(2) . . ?
C4 C5 C6 114.9(4) . . ?
C4 C5 C7 113.7(4) . . ?
C6 C5 C7 59.2(3) . . ?
C4 C5 C8 114.9(4) . . ?
C6 C5 C8 120.6(4) . . ?
C7 C5 C8 122.2(4) . . ?
C7 C6 C5 60.7(3) . . ?
C7 C6 H4 112(2) . . ?
C5 C6 H4 108(2) . . ?
C7 C6 H5 114(3) . . ?
C5 C6 H5 117(3) . . ?
H4 C6 H5 127(4) . . ?
C6 C7 C5 60.1(3) . . ?
C6 C7 H6 118(3) . . ?
C5 C7 H6 111(3) . . ?
C6 C7 H7 108.0(19) . . ?
C5 C7 H7 110.0(19) . . ?
H6 C7 H7 130(3) . . ?
C35 C8 C29 111.8(4) . . ?
C35 C8 C5 104.6(3) . . ?
C29 C8 C5 111.3(4) . . ?
C35 C8 C9 108.3(4) . . ?
C29 C8 C9 107.5(3) . . ?
C5 C8 C9 113.3(4) . . ?
O1 C9 C10 109.9(4) . . ?
O1 C9 C8 106.3(4) . . ?
C10 C9 C8 119.5(4) . . ?
O1 C9 H8 107.6(18) . . ?
C10 C9 H8 110.2(18) . . ?
C8 C9 H8 102.5(18) . . ?
C11 C10 C15 116.2(4) . . ?
C11 C10 C9 123.2(4) . . ?
C15 C10 C9 120.4(4) . . ?
C10 C11 C12 122.8(4) . . ?
C10 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C13 C12 C11 118.7(4) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 O2 123.7(4) . . ?
C12 C13 C14 121.4(4) . . ?
O2 C13 C14 114.9(4) . . ?
C15 C14 C13 118.0(5) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
C14 C15 C10 122.8(5) . . ?
C14 C15 H15 118.6 . . ?
C10 C15 H15 118.6 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 117.4(4) . . ?
C22 C17 C1 122.4(4) . . ?
C18 C17 C1 120.2(4) . . ?
C19 C18 C17 120.4(4) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 121.0(5) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 118.7(5) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C22 C21 C20 120.2(5) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C17 122.4(5) . . ?
C21 C22 H22 118.8 . . ?
C17 C22 H22 118.8 . . ?
C28 C23 C24 118.7(5) . . ?
C28 C23 C1 120.2(5) . . ?
C24 C23 C1 121.1(5) . . ?
C25 C24 C23 120.8(5) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.4(6) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 119.3(6) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 119.7(6) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C23 C28 C27 121.1(5) . . ?
C23 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C34 C29 C30 117.3(4) . . ?
C34 C29 C8 120.8(4) . . ?
C30 C29 C8 121.4(4) . . ?
C31 C30 C29 120.9(5) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C32 C31 C30 121.0(5) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C33 118.9(5) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C32 C33 C34 120.2(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C29 C34 C33 121.7(5) . . ?
C29 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C36 C35 C40 116.7(4) . . ?
C36 C35 C8 123.3(4) . . ?
C40 C35 C8 119.5(4) . . ?
C35 C36 C37 120.6(5) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C38 C37 C36 121.1(6) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C37 C38 C39 120.0(5) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C38 C39 C40 120.7(5) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C39 C40 C35 120.8(5) . . ?
C39 C40 H40 119.6 . . ?
C35 C40 H40 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C17 C1 C2 C4 166.7(8) . . . . ?
C23 C1 C2 C4 -11.3(12) . . . . ?
C17 C1 C2 C3 1.5(12) . . . . ?
C23 C1 C2 C3 -176.5(7) . . . . ?
C1 C2 C3 C4 171.8(9) . . . . ?
C1 C2 C4 C5 -62.6(11) . . . . ?
C3 C2 C4 C5 108.2(6) . . . . ?
C1 C2 C4 C3 -170.8(10) . . . . ?
C2 C3 C4 C5 -110.8(5) . . . . ?
C2 C4 C5 C6 -11.0(7) . . . . ?
C3 C4 C5 C6 58.3(6) . . . . ?
C2 C4 C5 C7 54.6(6) . . . . ?
C3 C4 C5 C7 123.9(5) . . . . ?
C2 C4 C5 C8 -157.6(4) . . . . ?
C3 C4 C5 C8 -88.3(5) . . . . ?
C4 C5 C6 C7 103.9(5) . . . . ?
C8 C5 C6 C7 -111.6(5) . . . . ?
C4 C5 C7 C6 -105.9(5) . . . . ?
C8 C5 C7 C6 109.0(5) . . . . ?
C4 C5 C8 C35 53.6(5) . . . . ?
C6 C5 C8 C35 -90.9(5) . . . . ?
C7 C5 C8 C35 -161.6(4) . . . . ?
C4 C5 C8 C29 -67.4(5) . . . . ?
C6 C5 C8 C29 148.1(4) . . . . ?
C7 C5 C8 C29 77.4(5) . . . . ?
C4 C5 C8 C9 171.4(4) . . . . ?
C6 C5 C8 C9 26.8(6) . . . . ?
C7 C5 C8 C9 -43.9(6) . . . . ?
C35 C8 C9 O1 -50.4(4) . . . . ?
C29 C8 C9 O1 70.6(4) . . . . ?
C5 C8 C9 O1 -165.9(3) . . . . ?
C35 C8 C9 C10 -175.4(4) . . . . ?
C29 C8 C9 C10 -54.4(5) . . . . ?
C5 C8 C9 C10 69.1(5) . . . . ?
O1 C9 C10 C11 -54.4(6) . . . . ?
C8 C9 C10 C11 68.8(6) . . . . ?
O1 C9 C10 C15 120.5(4) . . . . ?
C8 C9 C10 C15 -116.3(5) . . . . ?
C15 C10 C11 C12 1.5(7) . . . . ?
C9 C10 C11 C12 176.6(4) . . . . ?
C10 C11 C12 C13 -0.4(7) . . . . ?
C11 C12 C13 O2 -178.3(4) . . . . ?
C11 C12 C13 C14 0.5(7) . . . . ?
C16 O2 C13 C12 -15.0(6) . . . . ?
C16 O2 C13 C14 166.1(4) . . . . ?
C12 C13 C14 C15 -1.8(7) . . . . ?
O2 C13 C14 C15 177.1(4) . . . . ?
C13 C14 C15 C10 3.0(7) . . . . ?
C11 C10 C15 C14 -2.8(7) . . . . ?
C9 C10 C15 C14 -178.1(4) . . . . ?
C2 C1 C17 C22 156.4(5) . . . . ?
C23 C1 C17 C22 -25.6(7) . . . . ?
C2 C1 C17 C18 -23.7(7) . . . . ?
C23 C1 C17 C18 154.3(4) . . . . ?
C22 C17 C18 C19 -0.2(7) . . . . ?
C1 C17 C18 C19 179.9(4) . . . . ?
C17 C18 C19 C20 0.0(7) . . . . ?
C18 C19 C20 C21 -0.1(7) . . . . ?
C19 C20 C21 C22 0.4(8) . . . . ?
C20 C21 C22 C17 -0.6(8) . . . . ?
C18 C17 C22 C21 0.5(7) . . . . ?
C1 C17 C22 C21 -179.6(4) . . . . ?
C2 C1 C23 C28 -51.4(7) . . . . ?
C17 C1 C23 C28 130.6(5) . . . . ?
C2 C1 C23 C24 126.4(5) . . . . ?
C17 C1 C23 C24 -51.6(7) . . . . ?
C28 C23 C24 C25 0.9(8) . . . . ?
C1 C23 C24 C25 -176.9(4) . . . . ?
C23 C24 C25 C26 0.4(9) . . . . ?
C24 C25 C26 C27 -1.3(9) . . . . ?
C25 C26 C27 C28 0.8(9) . . . . ?
C24 C23 C28 C27 -1.4(8) . . . . ?
C1 C23 C28 C27 176.5(4) . . . . ?
C26 C27 C28 C23 0.5(9) . . . . ?
C35 C8 C29 C34 51.0(5) . . . . ?
C5 C8 C29 C34 167.6(4) . . . . ?
C9 C8 C29 C34 -67.7(5) . . . . ?
C35 C8 C29 C30 -136.4(4) . . . . ?
C5 C8 C29 C30 -19.8(5) . . . . ?
C9 C8 C29 C30 104.9(4) . . . . ?
C34 C29 C30 C31 1.6(6) . . . . ?
C8 C29 C30 C31 -171.3(4) . . . . ?
C29 C30 C31 C32 -0.1(7) . . . . ?
C30 C31 C32 C33 -1.0(8) . . . . ?
C31 C32 C33 C34 0.5(7) . . . . ?
C30 C29 C34 C33 -2.1(7) . . . . ?
C8 C29 C34 C33 170.8(4) . . . . ?
C32 C33 C34 C29 1.1(7) . . . . ?
C29 C8 C35 C36 20.0(6) . . . . ?
C5 C8 C35 C36 -100.6(5) . . . . ?
C9 C8 C35 C36 138.2(4) . . . . ?
C29 C8 C35 C40 -168.0(4) . . . . ?
C5 C8 C35 C40 71.4(5) . . . . ?
C9 C8 C35 C40 -49.8(5) . . . . ?
C40 C35 C36 C37 2.4(7) . . . . ?
C8 C35 C36 C37 174.5(5) . . . . ?
C35 C36 C37 C38 -3.5(8) . . . . ?
C36 C37 C38 C39 3.0(9) . . . . ?
C37 C38 C39 C40 -1.5(9) . . . . ?
C38 C39 C40 C35 0.4(8) . . . . ?
C36 C35 C40 C39 -0.9(7) . . . . ?
C8 C35 C40 C39 -173.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        28.13
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.037



