# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         182

_publ_requested_journal          'Chemical Communications'

_publ_contact_author_name        'Jie Wu'
_publ_contact_author_address     
;
Department of Chemistry
Fudan University
220 Handan Road
Shanghai
200433
CHINA
;

_publ_contact_author_email       JIE_WU@FUDAN.EDU.CN

_publ_section_title              
;
Rapid access to 1-methyleneindenes via
palladium-catalyzed tandem reactions of
1-(2,2-dibromovinyl)-2-alkynylbenzenes
with arylboronic acids
;
loop_
_publ_author_name
'Jie Wu'
'Xiaodi Yang'
'Shengqing Ye'

# Attachment '091010wujie_0m.cif'

data_091010wujie_0m
_database_code_depnum_ccdc_archive 'CCDC 759033'
#TrackingRef '091010wujie_0m.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H24'
_chemical_formula_weight         384.49

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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                   14.9337(15)
_cell_length_b                   9.7984(10)
_cell_length_c                   15.5440(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.1110(10)
_cell_angle_gamma                90.00
_cell_volume                     2223.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7329
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.58

_exptl_crystal_description       ?
_exptl_crystal_colour            red-colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9683
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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            16373
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4363
_reflns_number_gt                3419
_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^)+(0.0594P)^2^+0.3340P] 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       0.0181(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4363
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1216
_refine_ls_wR_factor_gt          0.1067
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.022
_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
C17 C 0.17799(8) 0.31087(13) 0.17494(7) 0.0445(3) Uani 1 1 d . . .
C18 C 0.22498(9) 0.21594(13) 0.13438(8) 0.0499(3) Uani 1 1 d . . .
H18 H 0.1932 0.1433 0.1037 0.060 Uiso 1 1 calc R . .
C4 C -0.07587(9) 0.20553(13) 0.08971(8) 0.0494(3) Uani 1 1 d . . .
C10 C 0.07847(8) 0.29955(13) 0.16881(8) 0.0455(3) Uani 1 1 d . . .
C24 C 0.10724(9) 0.32063(14) -0.03114(8) 0.0487(3) Uani 1 1 d . . .
C9 C 0.01767(9) 0.26055(13) 0.09450(8) 0.0464(3) Uani 1 1 d . . .
C5 C -0.11320(9) 0.17388(14) 0.00100(9) 0.0528(3) Uani 1 1 d . . .
C11 C 0.04512(8) 0.33295(15) 0.25018(8) 0.0504(3) Uani 1 1 d . . .
C28 C 0.14003(9) 0.45063(14) -0.00627(8) 0.0517(3) Uani 1 1 d . . .
H28 H 0.1126 0.5016 0.0316 0.062 Uiso 1 1 calc R . .
C8 C 0.03048(9) 0.26031(13) 0.00206(8) 0.0488(3) Uani 1 1 d . . .
C22 C 0.22886(9) 0.41534(14) 0.22273(8) 0.0519(3) Uani 1 1 d . . .
H22 H 0.1998 0.4785 0.2522 0.062 Uiso 1 1 calc R . .
C6 C -0.20047(10) 0.11963(15) -0.02375(10) 0.0633(4) Uani 1 1 d . . .
H6 H -0.2255 0.1017 -0.0827 0.076 Uiso 1 1 calc R . .
C30 C 0.21231(10) 0.50493(16) -0.03684(9) 0.0588(4) Uani 1 1 d . . .
H30 H 0.2332 0.5919 -0.0189 0.071 Uiso 1 1 calc R . .
C21 C 0.32167(10) 0.42634(16) 0.22689(9) 0.0593(4) Uani 1 1 d . . .
H21 H 0.3540 0.4973 0.2590 0.071 Uiso 1 1 calc R . .
C20 C 0.36782(10) 0.33464(17) 0.18460(10) 0.0612(4) Uani 1 1 d . . .
C3 C -0.12544(10) 0.17367(16) 0.15279(10) 0.0612(4) Uani 1 1 d . . .
H3 H -0.1007 0.1894 0.2120 0.073 Uiso 1 1 calc R . .
C19 C 0.31759(10) 0.22814(15) 0.13914(9) 0.0586(4) Uani 1 1 d . . .
H19 H 0.3473 0.1636 0.1113 0.070 Uiso 1 1 calc R . .
C25 C 0.14851(10) 0.24896(16) -0.08974(9) 0.0585(4) Uani 1 1 d . . .
H25 H 0.1271 0.1626 -0.1085 0.070 Uiso 1 1 calc R . .
C7 C -0.04631(10) 0.21048(15) -0.05018(9) 0.0560(3) Uani 1 1 d . . .
H7 H -0.0550 0.2010 -0.1109 0.067 Uiso 1 1 calc R . .
C27 C 0.25474(10) 0.43296(18) -0.09373(10) 0.0654(4) Uani 1 1 d . . .
C26 C 0.22078(11) 0.30480(18) -0.12021(10) 0.0691(4) Uani 1 1 d . . .
H26 H 0.2473 0.2552 -0.1594 0.083 Uiso 1 1 calc R . .
C16 C 0.07778(10) 0.26439(17) 0.32870(9) 0.0632(4) Uani 1 1 d . . .
H16 H 0.1246 0.2007 0.3322 0.076 Uiso 1 1 calc R . .
C12 C -0.02055(10) 0.43356(18) 0.24806(10) 0.0669(4) Uani 1 1 d . . .
H12 H -0.0415 0.4830 0.1967 0.080 Uiso 1 1 calc R . .
C1 C -0.24976(11) 0.09253(17) 0.03975(12) 0.0700(4) Uani 1 1 d . . .
H1 H -0.3086 0.0568 0.0237 0.084 Uiso 1 1 calc R . .
C2 C -0.21232(11) 0.11816(18) 0.12715(11) 0.0701(4) Uani 1 1 d . . .
H2 H -0.2459 0.0979 0.1696 0.084 Uiso 1 1 calc R . .
C15 C 0.04127(13) 0.2902(2) 0.40151(11) 0.0836(6) Uani 1 1 d . . .
H15 H 0.0620 0.2414 0.4532 0.100 Uiso 1 1 calc R . .
C13 C -0.05492(12) 0.4605(2) 0.32231(14) 0.0875(6) Uani 1 1 d . . .
H13 H -0.0985 0.5288 0.3208 0.105 Uiso 1 1 calc R . .
C14 C -0.02534(13) 0.3873(3) 0.39823(13) 0.0931(7) Uani 1 1 d . . .
H14 H -0.0504 0.4036 0.4472 0.112 Uiso 1 1 calc R . .
C23 C 0.46885(12) 0.3492(2) 0.18768(15) 0.0968(6) Uani 1 1 d . . .
H23A H 0.4804 0.3362 0.1298 0.145 Uiso 1 1 calc R . .
H23B H 0.5019 0.2819 0.2268 0.145 Uiso 1 1 calc R . .
H23C H 0.4887 0.4387 0.2085 0.145 Uiso 1 1 calc R . .
C29 C 0.33526(14) 0.4933(2) -0.12479(15) 0.1030(7) Uani 1 1 d . . .
H29A H 0.3686 0.4219 -0.1465 0.154 Uiso 1 1 calc R . .
H29B H 0.3748 0.5387 -0.0766 0.154 Uiso 1 1 calc R . .
H29C H 0.3137 0.5578 -0.1710 0.154 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
C17 0.0460(7) 0.0482(7) 0.0387(6) 0.0029(5) 0.0077(5) 0.0015(5)
C18 0.0520(7) 0.0465(7) 0.0503(7) 0.0020(5) 0.0084(6) 0.0041(6)
C4 0.0475(7) 0.0485(7) 0.0504(7) -0.0023(6) 0.0057(6) -0.0004(6)
C10 0.0469(7) 0.0457(7) 0.0437(6) -0.0011(5) 0.0088(5) 0.0013(5)
C24 0.0505(7) 0.0545(8) 0.0406(6) 0.0019(5) 0.0087(5) 0.0090(6)
C9 0.0462(7) 0.0477(7) 0.0454(6) -0.0019(5) 0.0094(5) 0.0015(5)
C5 0.0537(8) 0.0481(7) 0.0533(7) -0.0071(6) 0.0033(6) 0.0014(6)
C11 0.0430(7) 0.0616(8) 0.0466(7) -0.0098(6) 0.0091(5) -0.0059(6)
C28 0.0593(8) 0.0504(8) 0.0479(7) 0.0017(6) 0.0169(6) 0.0102(6)
C8 0.0535(7) 0.0482(7) 0.0442(6) -0.0025(5) 0.0093(6) 0.0062(6)
C22 0.0540(8) 0.0558(8) 0.0466(7) -0.0041(6) 0.0119(6) -0.0030(6)
C6 0.0597(9) 0.0586(9) 0.0648(9) -0.0120(7) -0.0022(7) -0.0046(7)
C30 0.0631(9) 0.0571(8) 0.0580(8) 0.0031(6) 0.0169(7) 0.0024(7)
C21 0.0553(8) 0.0659(9) 0.0559(8) -0.0003(7) 0.0097(6) -0.0136(7)
C20 0.0487(8) 0.0744(10) 0.0617(8) 0.0124(7) 0.0140(6) -0.0011(7)
C3 0.0554(8) 0.0719(10) 0.0553(8) 0.0014(7) 0.0098(6) -0.0100(7)
C19 0.0557(8) 0.0618(9) 0.0609(8) 0.0054(7) 0.0182(7) 0.0132(7)
C25 0.0632(9) 0.0620(9) 0.0508(7) -0.0093(6) 0.0128(6) 0.0056(7)
C7 0.0609(8) 0.0599(8) 0.0451(7) -0.0095(6) 0.0066(6) 0.0027(7)
C27 0.0598(9) 0.0816(11) 0.0589(8) -0.0003(8) 0.0215(7) 0.0028(8)
C26 0.0690(10) 0.0847(11) 0.0598(9) -0.0133(8) 0.0273(7) 0.0087(8)
C16 0.0589(9) 0.0825(11) 0.0470(7) -0.0035(7) 0.0087(6) -0.0021(8)
C12 0.0544(8) 0.0784(10) 0.0686(9) -0.0126(8) 0.0147(7) 0.0052(8)
C1 0.0530(8) 0.0659(10) 0.0860(11) -0.0035(8) 0.0026(8) -0.0127(7)
C2 0.0573(9) 0.0778(11) 0.0752(10) 0.0039(8) 0.0139(7) -0.0151(8)
C15 0.0824(12) 0.1221(16) 0.0487(8) -0.0070(9) 0.0190(8) -0.0155(11)
C13 0.0658(10) 0.1083(15) 0.0952(14) -0.0328(12) 0.0324(10) 0.0041(10)
C14 0.0803(12) 0.1382(19) 0.0701(11) -0.0361(12) 0.0366(10) -0.0174(12)
C23 0.0557(10) 0.1235(17) 0.1155(16) 0.0050(13) 0.0276(10) -0.0073(11)
C29 0.0883(13) 0.1274(18) 0.1082(15) -0.0180(13) 0.0546(12) -0.0193(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
C17 C18 1.3930(18) . ?
C17 C22 1.3929(18) . ?
C17 C10 1.4734(17) . ?
C18 C19 1.3745(19) . ?
C18 H18 0.9300 . ?
C4 C3 1.3825(19) . ?
C4 C5 1.4092(18) . ?
C4 C9 1.4845(18) . ?
C10 C9 1.3655(18) . ?
C10 C11 1.4897(17) . ?
C24 C28 1.3901(19) . ?
C24 C25 1.3922(18) . ?
C24 C8 1.4758(18) . ?
C9 C8 1.4887(17) . ?
C5 C6 1.385(2) . ?
C5 C7 1.447(2) . ?
C11 C12 1.386(2) . ?
C11 C16 1.389(2) . ?
C28 C30 1.3745(19) . ?
C28 H28 0.9300 . ?
C8 C7 1.3499(19) . ?
C22 C21 1.3780(19) . ?
C22 H22 0.9300 . ?
C6 C1 1.375(2) . ?
C6 H6 0.9300 . ?
C30 C27 1.384(2) . ?
C30 H30 0.9300 . ?
C21 C20 1.380(2) . ?
C21 H21 0.9300 . ?
C20 C19 1.389(2) . ?
C20 C23 1.506(2) . ?
C3 C2 1.386(2) . ?
C3 H3 0.9300 . ?
C19 H19 0.9300 . ?
C25 C26 1.379(2) . ?
C25 H25 0.9300 . ?
C7 H7 0.9300 . ?
C27 C26 1.384(2) . ?
C27 C29 1.507(2) . ?
C26 H26 0.9300 . ?
C16 C15 1.379(2) . ?
C16 H16 0.9300 . ?
C12 C13 1.383(2) . ?
C12 H12 0.9300 . ?
C1 C2 1.379(2) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C15 C14 1.370(3) . ?
C15 H15 0.9300 . ?
C13 C14 1.372(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 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
C18 C17 C22 117.51(12) . . ?
C18 C17 C10 121.17(11) . . ?
C22 C17 C10 121.31(11) . . ?
C19 C18 C17 120.95(13) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C3 C4 C5 118.91(13) . . ?
C3 C4 C9 133.21(12) . . ?
C5 C4 C9 107.69(11) . . ?
C9 C10 C17 123.94(11) . . ?
C9 C10 C11 119.89(11) . . ?
C17 C10 C11 116.16(10) . . ?
C28 C24 C25 117.75(13) . . ?
C28 C24 C8 121.59(11) . . ?
C25 C24 C8 120.65(13) . . ?
C10 C9 C4 126.56(11) . . ?
C10 C9 C8 128.29(12) . . ?
C4 C9 C8 105.14(10) . . ?
C6 C5 C4 120.82(13) . . ?
C6 C5 C7 131.32(13) . . ?
C4 C5 C7 107.85(12) . . ?
C12 C11 C16 118.76(13) . . ?
C12 C11 C10 119.79(13) . . ?
C16 C11 C10 121.44(13) . . ?
C30 C28 C24 120.99(12) . . ?
C30 C28 H28 119.5 . . ?
C24 C28 H28 119.5 . . ?
C7 C8 C24 123.96(12) . . ?
C7 C8 C9 108.43(12) . . ?
C24 C8 C9 127.11(11) . . ?
C21 C22 C17 120.87(13) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
C1 C6 C5 119.26(14) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C28 C30 C27 121.44(14) . . ?
C28 C30 H30 119.3 . . ?
C27 C30 H30 119.3 . . ?
C22 C21 C20 121.64(14) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C20 C19 117.47(13) . . ?
C21 C20 C23 121.35(16) . . ?
C19 C20 C23 121.18(15) . . ?
C4 C3 C2 119.53(14) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C18 C19 C20 121.51(13) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C26 C25 C24 120.68(14) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C8 C7 C5 110.87(12) . . ?
C8 C7 H7 124.6 . . ?
C5 C7 H7 124.6 . . ?
C30 C27 C26 117.64(14) . . ?
C30 C27 C29 120.50(16) . . ?
C26 C27 C29 121.86(15) . . ?
C25 C26 C27 121.46(13) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C15 C16 C11 120.41(16) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C13 C12 C11 120.02(17) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C6 C1 C2 120.29(14) . . ?
C6 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
C1 C2 C3 121.08(15) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C14 C15 C16 120.40(18) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C14 C13 C12 120.60(18) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 119.68(16) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

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
C22 C17 C18 C19 -2.14(18) . . . . ?
C10 C17 C18 C19 178.98(12) . . . . ?
C18 C17 C10 C9 -39.21(19) . . . . ?
C22 C17 C10 C9 141.95(13) . . . . ?
C18 C17 C10 C11 140.49(12) . . . . ?
C22 C17 C10 C11 -38.35(17) . . . . ?
C17 C10 C9 C4 159.40(12) . . . . ?
C11 C10 C9 C4 -20.3(2) . . . . ?
C17 C10 C9 C8 -19.0(2) . . . . ?
C11 C10 C9 C8 161.29(13) . . . . ?
C3 C4 C9 C10 -2.9(2) . . . . ?
C5 C4 C9 C10 -177.77(13) . . . . ?
C3 C4 C9 C8 175.78(15) . . . . ?
C5 C4 C9 C8 0.94(14) . . . . ?
C3 C4 C5 C6 4.0(2) . . . . ?
C9 C4 C5 C6 179.72(13) . . . . ?
C3 C4 C5 C7 -176.96(13) . . . . ?
C9 C4 C5 C7 -1.26(15) . . . . ?
C9 C10 C11 C12 -56.95(18) . . . . ?
C17 C10 C11 C12 123.34(14) . . . . ?
C9 C10 C11 C16 122.42(15) . . . . ?
C17 C10 C11 C16 -57.29(17) . . . . ?
C25 C24 C28 C30 -1.6(2) . . . . ?
C8 C24 C28 C30 179.19(12) . . . . ?
C28 C24 C8 C7 125.60(15) . . . . ?
C25 C24 C8 C7 -53.54(19) . . . . ?
C28 C24 C8 C9 -45.41(19) . . . . ?
C25 C24 C8 C9 135.45(14) . . . . ?
C10 C9 C8 C7 178.43(13) . . . . ?
C4 C9 C8 C7 -0.25(14) . . . . ?
C10 C9 C8 C24 -9.4(2) . . . . ?
C4 C9 C8 C24 171.90(12) . . . . ?
C18 C17 C22 C21 2.18(19) . . . . ?
C10 C17 C22 C21 -178.94(12) . . . . ?
C4 C5 C6 C1 -2.1(2) . . . . ?
C7 C5 C6 C1 179.15(15) . . . . ?
C24 C28 C30 C27 0.4(2) . . . . ?
C17 C22 C21 C20 -0.3(2) . . . . ?
C22 C21 C20 C19 -1.6(2) . . . . ?
C22 C21 C20 C23 178.55(15) . . . . ?
C5 C4 C3 C2 -3.3(2) . . . . ?
C9 C4 C3 C2 -177.71(15) . . . . ?
C17 C18 C19 C20 0.3(2) . . . . ?
C21 C20 C19 C18 1.6(2) . . . . ?
C23 C20 C19 C18 -178.52(15) . . . . ?
C28 C24 C25 C26 1.4(2) . . . . ?
C8 C24 C25 C26 -179.44(13) . . . . ?
C24 C8 C7 C5 -172.98(12) . . . . ?
C9 C8 C7 C5 -0.53(16) . . . . ?
C6 C5 C7 C8 -179.97(15) . . . . ?
C4 C5 C7 C8 1.15(16) . . . . ?
C28 C30 C27 C26 1.1(2) . . . . ?
C28 C30 C27 C29 -178.62(16) . . . . ?
C24 C25 C26 C27 0.1(2) . . . . ?
C30 C27 C26 C25 -1.4(2) . . . . ?
C29 C27 C26 C25 178.36(17) . . . . ?
C12 C11 C16 C15 4.0(2) . . . . ?
C10 C11 C16 C15 -175.37(14) . . . . ?
C16 C11 C12 C13 -2.5(2) . . . . ?
C10 C11 C12 C13 176.92(14) . . . . ?
C5 C6 C1 C2 -0.5(2) . . . . ?
C6 C1 C2 C3 1.1(3) . . . . ?
C4 C3 C2 C1 0.8(3) . . . . ?
C11 C16 C15 C14 -2.4(3) . . . . ?
C11 C12 C13 C14 -0.7(3) . . . . ?
C16 C15 C14 C13 -0.9(3) . . . . ?
C12 C13 C14 C15 2.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.045