# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chuan-Feng Chen' _publ_contact_author_email CCHEN@ICCAS.AC.CN _publ_section_title ; Triptycene-derived calix[6]arenes: synthesis and their self-assembled nanotubes ; loop_ _publ_author_name 'Chuan-Feng Chen' 'Xiang Hao' 'Tong-Ling Liang' 'Xiao-Hong Tian' # Attachment '1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 737427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H72 O8' _chemical_formula_weight 1041.28 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 C2/c 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' '-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 14.954(3) _cell_length_b 13.561(3) _cell_length_c 29.634(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.15(3) _cell_angle_gamma 90.00 _cell_volume 5827(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7752 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.50 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9564 _exptl_absorpt_correction_T_max 0.9954 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28032 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5418 _reflns_number_gt 5080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0416P)^2^+7.3051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5418 _refine_ls_number_parameters 377 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_restrained_S_all 1.273 _refine_ls_shift/su_max 0.002 _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 O1 O 0.21063(12) 0.21856(14) 0.29263(7) 0.0513(5) Uani 1 1 d . . . H1O1 H 0.1682 0.2037 0.3054 0.062 Uiso 1 1 d R . . O2 O -0.06416(11) 0.18854(12) 0.08708(6) 0.0393(4) Uani 1 1 d . . . O3 O 0.23208(11) 0.18600(13) 0.16049(6) 0.0398(4) Uani 1 1 d . . . C1 C -0.0922(2) 0.1785(2) 0.03758(10) 0.0564(8) Uani 1 1 d . . . H1A H -0.0837 0.1100 0.0289 0.085 Uiso 1 1 calc R . . H1B H -0.0548 0.2221 0.0232 0.085 Uiso 1 1 calc R . . H1C H -0.1574 0.1966 0.0267 0.085 Uiso 1 1 calc R . . C2 C 0.5555(2) 0.3936(3) 0.44975(10) 0.0618(9) Uani 1 1 d . . . H2A H 0.5108 0.4471 0.4484 0.093 Uiso 1 1 calc R . . H2B H 0.6170 0.4166 0.4661 0.093 Uiso 1 1 calc R . . H2C H 0.5379 0.3373 0.4665 0.093 Uiso 1 1 calc R . . C3 C 0.5936(2) 0.4477(2) 0.37651(11) 0.0563(8) Uani 1 1 d . . . H3A H 0.5517 0.5041 0.3739 0.084 Uiso 1 1 calc R . . H3B H 0.5979 0.4272 0.3454 0.084 Uiso 1 1 calc R . . H3C H 0.6548 0.4665 0.3950 0.084 Uiso 1 1 calc R . . C4 C 0.62172(19) 0.2736(2) 0.40356(10) 0.0522(7) Uani 1 1 d . . . H4A H 0.6833 0.2918 0.4219 0.078 Uiso 1 1 calc R . . H4B H 0.6253 0.2540 0.3722 0.078 Uiso 1 1 calc R . . H4C H 0.5982 0.2184 0.4186 0.078 Uiso 1 1 calc R . . C5 C 0.1629(2) 0.1249(2) 0.17224(11) 0.0508(7) Uani 1 1 d . . . H5A H 0.1724 0.0562 0.1642 0.076 Uiso 1 1 calc R . . H5B H 0.1017 0.1468 0.1549 0.076 Uiso 1 1 calc R . . H5C H 0.1672 0.1297 0.2057 0.076 Uiso 1 1 calc R . . C6 C 0.14255(19) 0.5399(2) 0.00258(10) 0.0495(7) Uani 1 1 d . . . H6A H 0.1507 0.5904 -0.0182 0.059 Uiso 1 1 calc R . . C7 C 0.11926(18) 0.5650(2) 0.04381(9) 0.0437(6) Uani 1 1 d . . . H7A H 0.1111 0.6321 0.0511 0.052 Uiso 1 1 calc R . . C8 C -0.23019(18) 0.2450(2) 0.10830(10) 0.0469(7) Uani 1 1 d . . . H8A H -0.2599 0.2361 0.0748 0.056 Uiso 1 1 calc R . . H8B H -0.2040 0.1804 0.1205 0.056 Uiso 1 1 calc R . . C9 C 0.14020(16) 0.3678(2) 0.02131(9) 0.0403(6) Uani 1 1 d . . . H9A H 0.1469 0.3007 0.0136 0.048 Uiso 1 1 calc R . . C10 C 0.21660(18) 0.4825(2) 0.19706(9) 0.0425(6) Uani 1 1 d . . . H10A H 0.2141 0.5499 0.2053 0.051 Uiso 1 1 calc R . . C11 C -0.15587(18) 0.4146(2) 0.12619(9) 0.0427(6) Uani 1 1 d . . . H11A H -0.2104 0.4375 0.1338 0.051 Uiso 1 1 calc R . . C12 C 0.27724(18) 0.4176(2) 0.22591(9) 0.0436(6) Uani 1 1 d . . . H12A H 0.3160 0.4420 0.2540 0.052 Uiso 1 1 calc R . . C13 C 0.29161(16) 0.25593(19) 0.31985(9) 0.0391(6) Uani 1 1 d . . . C14 C 0.30390(17) 0.2721(2) 0.36716(9) 0.0409(6) Uani 1 1 d . . . C15 C 0.11677(16) 0.39241(19) 0.06224(8) 0.0359(6) Uani 1 1 d . . . C16 C 0.55658(18) 0.3621(2) 0.40029(9) 0.0439(6) Uani 1 1 d . . . C17 C 0.10824(16) 0.49078(19) 0.07403(9) 0.0381(6) Uani 1 1 d . . . C18 C 0.46110(17) 0.32929(19) 0.37215(9) 0.0389(6) Uani 1 1 d . . . C19 C 0.08592(17) 0.50390(19) 0.12134(9) 0.0388(6) Uani 1 1 d . . . H19A H 0.0815 0.5746 0.1301 0.047 Uiso 1 1 calc R . . C20 C 0.34951(17) 0.2495(2) 0.24702(9) 0.0420(6) Uani 1 1 d . . . H20A H 0.3261 0.1812 0.2414 0.050 Uiso 1 1 calc R . . H20B H 0.4100 0.2526 0.2390 0.050 Uiso 1 1 calc R . . C21 C 0.15387(18) 0.4428(2) -0.00845(9) 0.0473(7) Uani 1 1 d . . . H21A H 0.1710 0.4269 -0.0364 0.057 Uiso 1 1 calc R . . C22 C 0.38836(17) 0.3099(2) 0.39226(9) 0.0404(6) Uani 1 1 d . . . H22A H 0.3963 0.3229 0.4245 0.049 Uiso 1 1 calc R . . C23 C 0.36336(16) 0.27288(19) 0.29822(9) 0.0383(6) Uani 1 1 d . . . C24 C 0.16011(17) 0.44658(18) 0.15615(9) 0.0367(6) Uani 1 1 d . . . C25 C 0.22616(16) 0.28392(18) 0.17327(8) 0.0354(5) Uani 1 1 d . . . C26 C 0.16550(16) 0.34751(18) 0.14413(8) 0.0339(5) Uani 1 1 d . . . C27 C 0.28286(16) 0.31888(19) 0.21497(8) 0.0371(6) Uani 1 1 d . . . C28 C 0.44632(17) 0.30924(19) 0.32477(9) 0.0387(6) Uani 1 1 d . . . H28A H 0.4951 0.3210 0.3100 0.046 Uiso 1 1 calc R . . C29 C 0.00406(16) 0.34774(18) 0.10565(8) 0.0341(5) Uani 1 1 d . . . C30 C 0.09835(16) 0.31988(18) 0.09822(8) 0.0344(5) Uani 1 1 d . . . H30A H 0.1028 0.2493 0.0893 0.041 Uiso 1 1 calc R . . C31 C -0.15144(17) 0.31740(19) 0.11259(9) 0.0380(6) Uani 1 1 d . . . C32 C -0.00247(17) 0.44607(18) 0.11896(8) 0.0360(6) Uani 1 1 d . . . C33 C -0.07037(16) 0.28530(18) 0.10150(8) 0.0345(5) Uani 1 1 d . . . C34 C -0.08245(18) 0.48001(19) 0.12910(9) 0.0406(6) Uani 1 1 d . . . H34A H -0.0875 0.5467 0.1379 0.049 Uiso 1 1 calc R . . O4 O 0.0423(3) 0.1637(3) 0.29790(15) 0.0622(11) Uani 0.50 1 d PDU A -1 H1O4 H 0.0139 0.2140 0.2854 0.075 Uiso 0.50 1 d PR A -1 C35 C 0.0109(8) 0.0907(5) 0.2630(2) 0.073(2) Uani 0.50 1 d PDU A -1 H35A H 0.0640 0.0608 0.2543 0.109 Uiso 0.50 1 calc PR A -1 H35B H -0.0295 0.1215 0.2355 0.109 Uiso 0.50 1 calc PR A -1 H35C H -0.0233 0.0397 0.2751 0.109 Uiso 0.50 1 calc PR A -1 O5 O 0.0635(3) 0.3304(4) 0.23714(19) 0.0730(13) Uani 0.50 1 d PDU B -1 H1O5 H 0.1068 0.3198 0.2607 0.088 Uiso 0.50 1 d PR B -1 C36 C -0.0042(17) 0.3875(7) 0.2526(14) 0.108(3) Uani 0.50 1 d PDU B -1 H36A H -0.0144 0.3587 0.2812 0.162 Uiso 0.50 1 calc PR B -1 H36B H -0.0622 0.3873 0.2284 0.162 Uiso 0.50 1 calc PR B -1 H36C H 0.0178 0.4554 0.2586 0.162 Uiso 0.50 1 calc PR B -1 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 0.0319(10) 0.0554(12) 0.0656(13) 0.0086(10) 0.0098(9) -0.0044(9) O2 0.0382(9) 0.0370(10) 0.0452(10) -0.0044(8) 0.0148(8) -0.0051(7) O3 0.0387(10) 0.0373(10) 0.0454(10) -0.0024(8) 0.0142(8) 0.0004(8) C1 0.067(2) 0.0568(18) 0.0470(17) -0.0152(14) 0.0174(15) -0.0024(15) C2 0.0543(18) 0.080(2) 0.0512(18) -0.0168(16) 0.0123(15) -0.0070(16) C3 0.0542(18) 0.0527(18) 0.0629(19) -0.0052(15) 0.0159(15) -0.0094(14) C4 0.0380(15) 0.0610(19) 0.0552(18) 0.0014(14) 0.0068(13) 0.0012(13) C5 0.0523(17) 0.0404(15) 0.0630(19) 0.0009(13) 0.0202(15) -0.0061(13) C6 0.0471(16) 0.0574(18) 0.0417(15) 0.0091(13) 0.0064(13) -0.0106(13) C7 0.0409(15) 0.0409(15) 0.0460(15) 0.0040(12) 0.0038(12) -0.0074(12) C8 0.0372(14) 0.0566(17) 0.0519(16) -0.0142(13) 0.0207(13) -0.0101(12) C9 0.0321(13) 0.0496(15) 0.0386(14) -0.0003(12) 0.0076(11) -0.0032(11) C10 0.0478(15) 0.0389(14) 0.0400(14) -0.0012(11) 0.0090(12) -0.0063(12) C11 0.0370(14) 0.0490(16) 0.0454(15) -0.0053(12) 0.0165(12) -0.0004(12) C12 0.0422(15) 0.0485(16) 0.0380(14) -0.0031(12) 0.0060(12) -0.0087(12) C13 0.0273(12) 0.0437(15) 0.0457(15) 0.0083(11) 0.0080(11) 0.0042(11) C14 0.0355(13) 0.0471(15) 0.0434(15) 0.0094(12) 0.0162(12) 0.0098(11) C15 0.0260(12) 0.0457(15) 0.0347(13) 0.0013(11) 0.0047(10) -0.0031(10) C16 0.0388(14) 0.0508(16) 0.0434(15) -0.0030(12) 0.0125(12) -0.0015(12) C17 0.0294(12) 0.0433(14) 0.0402(14) 0.0018(11) 0.0058(11) -0.0072(11) C18 0.0351(13) 0.0433(14) 0.0401(14) 0.0033(11) 0.0127(11) 0.0052(11) C19 0.0401(14) 0.0352(13) 0.0411(14) 0.0011(11) 0.0096(11) -0.0039(11) C20 0.0343(13) 0.0531(16) 0.0402(14) 0.0004(12) 0.0118(11) 0.0027(12) C21 0.0422(15) 0.0641(19) 0.0371(14) 0.0047(13) 0.0127(12) -0.0067(13) C22 0.0381(14) 0.0481(15) 0.0373(14) 0.0046(11) 0.0134(11) 0.0078(12) C23 0.0331(13) 0.0439(14) 0.0388(14) 0.0056(11) 0.0106(11) 0.0056(11) C24 0.0364(13) 0.0371(13) 0.0381(13) 0.0017(11) 0.0122(11) -0.0049(11) C25 0.0323(12) 0.0385(14) 0.0390(14) -0.0004(11) 0.0153(11) -0.0024(10) C26 0.0307(12) 0.0381(13) 0.0343(13) -0.0007(10) 0.0104(10) -0.0043(10) C27 0.0335(13) 0.0430(14) 0.0360(13) 0.0028(11) 0.0108(11) -0.0022(11) C28 0.0328(13) 0.0467(15) 0.0393(14) 0.0061(11) 0.0140(11) 0.0057(11) C29 0.0322(12) 0.0397(14) 0.0316(12) 0.0018(10) 0.0103(10) -0.0020(10) C30 0.0311(12) 0.0355(13) 0.0377(13) -0.0010(10) 0.0104(10) -0.0023(10) C31 0.0335(13) 0.0461(15) 0.0367(14) -0.0043(11) 0.0126(11) -0.0046(11) C32 0.0367(13) 0.0375(13) 0.0337(13) 0.0005(10) 0.0084(11) -0.0021(11) C33 0.0342(13) 0.0365(13) 0.0340(13) -0.0021(10) 0.0109(11) -0.0014(10) C34 0.0437(15) 0.0380(14) 0.0411(14) -0.0034(11) 0.0125(12) 0.0028(11) O4 0.048(2) 0.072(3) 0.069(3) 0.000(2) 0.019(2) -0.006(2) C35 0.065(5) 0.078(4) 0.077(6) -0.013(3) 0.020(6) -0.009(4) O5 0.060(3) 0.080(3) 0.080(3) 0.013(3) 0.020(2) 0.010(2) C36 0.120(6) 0.115(5) 0.093(7) -0.027(8) 0.034(4) -0.012(9) _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 C13 1.377(3) . ? O1 H1O1 0.8399 . ? O2 C33 1.390(3) . ? O2 C1 1.430(3) . ? O3 C25 1.390(3) . ? O3 C5 1.434(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C16 1.531(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C16 1.529(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C16 1.534(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C21 1.377(4) . ? C6 C7 1.392(4) . ? C6 H6A 0.9500 . ? C7 C17 1.384(4) . ? C7 H7A 0.9500 . ? C8 C14 1.507(3) 2 ? C8 C31 1.515(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C15 1.383(3) . ? C9 C21 1.393(4) . ? C9 H9A 0.9500 . ? C10 C24 1.386(4) . ? C10 C12 1.396(4) . ? C10 H10A 0.9500 . ? C11 C31 1.384(4) . ? C11 C34 1.398(4) . ? C11 H11A 0.9500 . ? C12 C27 1.385(4) . ? C12 H12A 0.9500 . ? C13 C14 1.386(4) . ? C13 C23 1.397(3) . ? C14 C22 1.397(4) . ? C14 C8 1.507(3) 2 ? C15 C17 1.393(4) . ? C15 C30 1.524(3) . ? C16 C18 1.533(4) . ? C17 C19 1.529(4) . ? C18 C22 1.387(3) . ? C18 C28 1.394(3) . ? C19 C32 1.524(3) . ? C19 C24 1.530(4) . ? C19 H19A 1.0000 . ? C20 C23 1.514(3) . ? C20 C27 1.522(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.387(4) . ? C24 C26 1.397(3) . ? C25 C26 1.389(3) . ? C25 C27 1.399(3) . ? C26 C30 1.527(3) . ? C28 H28A 0.9500 . ? C29 C33 1.380(3) . ? C29 C32 1.401(3) . ? C29 C30 1.527(3) . ? C30 H30A 1.0000 . ? C31 C33 1.401(3) . ? C32 C34 1.381(3) . ? C34 H34A 0.9500 . ? O4 C35 1.426(6) . ? O4 H1O4 0.8400 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O5 C36 1.435(10) . ? O5 H1O5 0.8401 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 C13 O1 H1O1 118.5 . . ? C33 O2 C1 112.3(2) . . ? C25 O3 C5 112.86(19) . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C16 C2 H2A 109.5 . . ? C16 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C16 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C16 C3 H3A 109.5 . . ? C16 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C16 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C16 C4 H4A 109.5 . . ? C16 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C16 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 H5A 109.5 . . ? O3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C21 C6 C7 120.9(3) . . ? C21 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C17 C7 C6 119.0(3) . . ? C17 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C14 C8 C31 116.5(2) 2 . ? C14 C8 H8A 108.2 2 . ? C31 C8 H8A 108.2 . . ? C14 C8 H8B 108.2 2 . ? C31 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C15 C9 C21 119.2(3) . . ? C15 C9 H9A 120.4 . . ? C21 C9 H9A 120.4 . . ? C24 C10 C12 118.7(3) . . ? C24 C10 H10A 120.6 . . ? C12 C10 H10A 120.6 . . ? C31 C11 C34 122.0(2) . . ? C31 C11 H11A 119.0 . . ? C34 C11 H11A 119.0 . . ? C27 C12 C10 122.2(2) . . ? C27 C12 H12A 118.9 . . ? C10 C12 H12A 118.9 . . ? O1 C13 C14 122.1(2) . . ? O1 C13 C23 117.1(2) . . ? C14 C13 C23 120.7(2) . . ? C13 C14 C22 118.4(2) . . ? C13 C14 C8 121.2(2) . 2 ? C22 C14 C8 120.4(2) . 2 ? C9 C15 C17 120.6(2) . . ? C9 C15 C30 125.9(2) . . ? C17 C15 C30 113.5(2) . . ? C3 C16 C2 108.6(2) . . ? C3 C16 C18 111.3(2) . . ? C2 C16 C18 112.0(2) . . ? C3 C16 C4 109.1(2) . . ? C2 C16 C4 108.3(2) . . ? C18 C16 C4 107.4(2) . . ? C7 C17 C15 120.1(2) . . ? C7 C17 C19 126.6(2) . . ? C15 C17 C19 113.3(2) . . ? C22 C18 C28 116.6(2) . . ? C22 C18 C16 123.0(2) . . ? C28 C18 C16 120.1(2) . . ? C32 C19 C17 106.2(2) . . ? C32 C19 C24 104.3(2) . . ? C17 C19 C24 105.9(2) . . ? C32 C19 H19A 113.2 . . ? C17 C19 H19A 113.2 . . ? C24 C19 H19A 113.2 . . ? C23 C20 C27 113.9(2) . . ? C23 C20 H20A 108.8 . . ? C27 C20 H20A 108.8 . . ? C23 C20 H20B 108.8 . . ? C27 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C6 C21 C9 120.1(3) . . ? C6 C21 H21A 119.9 . . ? C9 C21 H21A 119.9 . . ? C18 C22 C14 122.9(2) . . ? C18 C22 H22A 118.6 . . ? C14 C22 H22A 118.6 . . ? C28 C23 C13 118.6(2) . . ? C28 C23 C20 121.8(2) . . ? C13 C23 C20 119.6(2) . . ? C10 C24 C26 120.0(2) . . ? C10 C24 C19 126.8(2) . . ? C26 C24 C19 113.2(2) . . ? C26 C25 O3 119.9(2) . . ? C26 C25 C27 120.1(2) . . ? O3 C25 C27 119.9(2) . . ? C25 C26 C24 120.5(2) . . ? C25 C26 C30 126.1(2) . . ? C24 C26 C30 113.4(2) . . ? C12 C27 C25 118.4(2) . . ? C12 C27 C20 121.3(2) . . ? C25 C27 C20 120.3(2) . . ? C23 C28 C18 122.7(2) . . ? C23 C28 H28A 118.6 . . ? C18 C28 H28A 118.6 . . ? C33 C29 C32 119.9(2) . . ? C33 C29 C30 126.1(2) . . ? C32 C29 C30 114.0(2) . . ? C15 C30 C29 105.80(19) . . ? C15 C30 C26 105.84(19) . . ? C29 C30 C26 103.89(19) . . ? C15 C30 H30A 113.5 . . ? C29 C30 H30A 113.5 . . ? C26 C30 H30A 113.5 . . ? C11 C31 C33 118.0(2) . . ? C11 C31 C8 123.4(2) . . ? C33 C31 C8 118.6(2) . . ? C34 C32 C29 120.1(2) . . ? C34 C32 C19 127.3(2) . . ? C29 C32 C19 112.6(2) . . ? C29 C33 O2 119.6(2) . . ? C29 C33 C31 120.9(2) . . ? O2 C33 C31 119.5(2) . . ? C32 C34 C11 118.9(2) . . ? C32 C34 H34A 120.5 . . ? C11 C34 H34A 120.5 . . ? C35 O4 H1O4 101.7 . . ? C36 O5 H1O5 106.8 . . ? 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 C21 C6 C7 C17 0.5(4) . . . . ? C24 C10 C12 C27 0.1(4) . . . . ? O1 C13 C14 C22 179.8(2) . . . . ? C23 C13 C14 C22 2.8(4) . . . . ? O1 C13 C14 C8 2.8(4) . . . 2 ? C23 C13 C14 C8 -174.1(2) . . . 2 ? C21 C9 C15 C17 -1.0(4) . . . . ? C21 C9 C15 C30 179.2(2) . . . . ? C6 C7 C17 C15 -2.6(4) . . . . ? C6 C7 C17 C19 177.9(2) . . . . ? C9 C15 C17 C7 2.8(4) . . . . ? C30 C15 C17 C7 -177.4(2) . . . . ? C9 C15 C17 C19 -177.6(2) . . . . ? C30 C15 C17 C19 2.2(3) . . . . ? C3 C16 C18 C22 -135.1(3) . . . . ? C2 C16 C18 C22 -13.3(4) . . . . ? C4 C16 C18 C22 105.5(3) . . . . ? C3 C16 C18 C28 50.5(3) . . . . ? C2 C16 C18 C28 172.4(3) . . . . ? C4 C16 C18 C28 -68.9(3) . . . . ? C7 C17 C19 C32 122.8(3) . . . . ? C15 C17 C19 C32 -56.8(3) . . . . ? C7 C17 C19 C24 -126.7(3) . . . . ? C15 C17 C19 C24 53.8(3) . . . . ? C7 C6 C21 C9 1.3(4) . . . . ? C15 C9 C21 C6 -1.1(4) . . . . ? C28 C18 C22 C14 0.1(4) . . . . ? C16 C18 C22 C14 -174.4(2) . . . . ? C13 C14 C22 C18 -1.9(4) . . . . ? C8 C14 C22 C18 175.1(2) 2 . . . ? O1 C13 C23 C28 -179.1(2) . . . . ? C14 C13 C23 C28 -2.0(4) . . . . ? O1 C13 C23 C20 -0.3(4) . . . . ? C14 C13 C23 C20 176.8(2) . . . . ? C27 C20 C23 C28 -111.1(3) . . . . ? C27 C20 C23 C13 70.1(3) . . . . ? C12 C10 C24 C26 -0.9(4) . . . . ? C12 C10 C24 C19 176.5(2) . . . . ? C32 C19 C24 C10 -121.8(3) . . . . ? C17 C19 C24 C10 126.3(3) . . . . ? C32 C19 C24 C26 55.8(3) . . . . ? C17 C19 C24 C26 -56.1(3) . . . . ? C5 O3 C25 C26 -83.9(3) . . . . ? C5 O3 C25 C27 97.6(3) . . . . ? O3 C25 C26 C24 -178.8(2) . . . . ? C27 C25 C26 C24 -0.3(3) . . . . ? O3 C25 C26 C30 2.7(4) . . . . ? C27 C25 C26 C30 -178.8(2) . . . . ? C10 C24 C26 C25 1.0(4) . . . . ? C19 C24 C26 C25 -176.8(2) . . . . ? C10 C24 C26 C30 179.7(2) . . . . ? C19 C24 C26 C30 1.9(3) . . . . ? C10 C12 C27 C25 0.6(4) . . . . ? C10 C12 C27 C20 -179.9(2) . . . . ? C26 C25 C27 C12 -0.5(4) . . . . ? O3 C25 C27 C12 178.0(2) . . . . ? C26 C25 C27 C20 -180.0(2) . . . . ? O3 C25 C27 C20 -1.5(3) . . . . ? C23 C20 C27 C12 34.3(3) . . . . ? C23 C20 C27 C25 -146.3(2) . . . . ? C13 C23 C28 C18 0.2(4) . . . . ? C20 C23 C28 C18 -178.6(2) . . . . ? C22 C18 C28 C23 0.8(4) . . . . ? C16 C18 C28 C23 175.5(2) . . . . ? C9 C15 C30 C29 -126.8(2) . . . . ? C17 C15 C30 C29 53.4(3) . . . . ? C9 C15 C30 C26 123.3(3) . . . . ? C17 C15 C30 C26 -56.5(3) . . . . ? C33 C29 C30 C15 125.6(3) . . . . ? C32 C29 C30 C15 -56.0(3) . . . . ? C33 C29 C30 C26 -123.1(3) . . . . ? C32 C29 C30 C26 55.2(3) . . . . ? C25 C26 C30 C15 -127.4(2) . . . . ? C24 C26 C30 C15 54.0(3) . . . . ? C25 C26 C30 C29 121.4(2) . . . . ? C24 C26 C30 C29 -57.2(3) . . . . ? C34 C11 C31 C33 -0.1(4) . . . . ? C34 C11 C31 C8 -179.0(3) . . . . ? C14 C8 C31 C11 -17.9(4) 2 . . . ? C14 C8 C31 C33 163.3(2) 2 . . . ? C33 C29 C32 C34 1.7(4) . . . . ? C30 C29 C32 C34 -176.8(2) . . . . ? C33 C29 C32 C19 -179.6(2) . . . . ? C30 C29 C32 C19 2.0(3) . . . . ? C17 C19 C32 C34 -127.4(3) . . . . ? C24 C19 C32 C34 121.0(3) . . . . ? C17 C19 C32 C29 53.9(3) . . . . ? C24 C19 C32 C29 -57.7(3) . . . . ? C32 C29 C33 O2 178.3(2) . . . . ? C30 C29 C33 O2 -3.4(4) . . . . ? C32 C29 C33 C31 -3.1(4) . . . . ? C30 C29 C33 C31 175.1(2) . . . . ? C1 O2 C33 C29 -89.3(3) . . . . ? C1 O2 C33 C31 92.1(3) . . . . ? C11 C31 C33 C29 2.3(4) . . . . ? C8 C31 C33 C29 -178.8(2) . . . . ? C11 C31 C33 O2 -179.1(2) . . . . ? C8 C31 C33 O2 -0.2(4) . . . . ? C29 C32 C34 C11 0.5(4) . . . . ? C19 C32 C34 C11 -178.1(2) . . . . ? C31 C11 C34 C32 -1.3(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O1 O4 0.84 1.92 2.666(4) 147.5 . O4 H1O4 O5 0.84 1.97 2.808(7) 171.7 2 O4 H1O4 O5 0.84 2.37 2.954(7) 127.5 . O5 H1O5 O1 0.84 2.12 2.842(5) 144.6 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.279 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.039 # Attachment '2.cif' data_sa123 _database_code_depnum_ccdc_archive 'CCDC 737428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H64 O6, 2(C H4 O), 4(C H2 Cl2)' _chemical_formula_sum 'C74 H80 Cl8 O8' _chemical_formula_weight 1380.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4028(15) _cell_length_b 15.554(3) _cell_length_c 16.174(3) _cell_angle_alpha 78.87(3) _cell_angle_beta 81.79(3) _cell_angle_gamma 82.09(3) _cell_volume 1797.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 417 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9140 _exptl_absorpt_correction_T_max 0.9370 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24372 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6323 _reflns_number_gt 5809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6323 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.3979 _refine_ls_wR_factor_gt 0.3905 _refine_ls_goodness_of_fit_ref 1.809 _refine_ls_restrained_S_all 1.809 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.4141(3) 0.8543(3) 0.06472(14) 0.1549(16) Uani 1 1 d . . . Cl2 Cl 0.7990(4) 0.8460(4) 0.05719(19) 0.190(2) Uani 1 1 d . . . Cl3 Cl 0.59445(19) 0.79461(10) 0.36665(10) 0.0647(5) Uani 1 1 d . . . Cl4 Cl 0.6490(2) 0.59926(11) 0.40209(14) 0.0818(7) Uani 1 1 d . . . O1 O 1.0713(4) 0.85871(19) 0.40507(18) 0.0394(8) Uani 1 1 d . . . H1 H 1.0875 0.8397 0.4560 0.059 Uiso 1 1 calc R . . O2 O 0.8445(4) 1.08827(17) 0.20470(17) 0.0294(7) Uani 1 1 d . . . O3 O 0.7461(3) 1.28983(17) 0.34035(17) 0.0287(7) Uani 1 1 d . . . O4 O 1.0186(10) 0.9550(2) 0.5543(2) 0.105(2) Uani 1 1 d . . . H4 H 1.0469 0.9570 0.5018 0.126 Uiso 1 1 d R . . C1 C 1.1908(7) 0.5832(3) 0.2237(3) 0.0434(11) Uani 1 1 d . . . C2 C 1.0995(12) 0.6098(5) 0.1403(5) 0.098(3) Uani 1 1 d . . . H2A H 1.1248 0.5611 0.1083 0.147 Uiso 1 1 calc R . . H2B H 1.1498 0.6622 0.1059 0.147 Uiso 1 1 calc R . . H2C H 0.9665 0.6230 0.1540 0.147 Uiso 1 1 calc R . . C3 C 1.3986(8) 0.5671(3) 0.1989(3) 0.0527(13) Uani 1 1 d . . . H3A H 1.4416 0.6202 0.1625 0.079 Uiso 1 1 calc R . . H3B H 1.4263 0.5175 0.1682 0.079 Uiso 1 1 calc R . . H3C H 1.4608 0.5534 0.2502 0.079 Uiso 1 1 calc R . . C4 C 1.1323(11) 0.4934(4) 0.2828(5) 0.091(3) Uani 1 1 d . . . H4A H 1.1580 0.4454 0.2500 0.136 Uiso 1 1 calc R . . H4B H 1.0007 0.5012 0.3028 0.136 Uiso 1 1 calc R . . H4C H 1.2024 0.4790 0.3316 0.136 Uiso 1 1 calc R . . C5 C 1.1537(5) 0.6564(3) 0.2722(3) 0.0325(9) Uani 1 1 d . . . C6 C 1.1054(5) 0.7450(3) 0.2319(2) 0.0284(9) Uani 1 1 d . . . H6A H 1.0931 0.7561 0.1730 0.034 Uiso 1 1 calc R . . C7 C 1.0760(5) 0.8141(2) 0.2741(2) 0.0277(8) Uani 1 1 d . . . C8 C 1.0998(5) 0.7915(2) 0.3624(2) 0.0269(8) Uani 1 1 d . . . C9 C 1.1504(5) 0.7041(3) 0.4060(2) 0.0278(9) Uani 1 1 d . . . C10 C 1.1746(5) 0.6376(2) 0.3597(2) 0.0291(9) Uani 1 1 d . . . H10A H 1.2055 0.5784 0.3865 0.035 Uiso 1 1 calc R . . C11 C 1.1901(6) 0.6806(3) 0.4987(2) 0.0354(10) Uani 1 1 d . . . H11A H 1.2246 0.6161 0.5125 0.042 Uiso 1 1 calc R . . H11B H 1.2974 0.7097 0.5044 0.042 Uiso 1 1 calc R . . C12 C 1.0043(6) 0.9077(3) 0.2287(3) 0.0355(10) Uani 1 1 d . . . H12A H 0.9964 0.9046 0.1687 0.043 Uiso 1 1 calc R . . H12B H 0.8780 0.9232 0.2552 0.043 Uiso 1 1 calc R . . C13 C 1.1179(5) 0.9831(2) 0.2297(2) 0.0269(8) Uani 1 1 d . . . C14 C 1.2996(5) 0.9682(2) 0.2441(3) 0.0298(9) Uani 1 1 d . . . H14A H 1.3605 0.9099 0.2495 0.036 Uiso 1 1 calc R . . C15 C 1.3966(5) 1.0376(3) 0.2511(2) 0.0290(9) Uani 1 1 d . . . H15A H 1.5210 1.0266 0.2623 0.035 Uiso 1 1 calc R . . C16 C 1.3057(5) 1.1229(2) 0.2413(2) 0.0255(8) Uani 1 1 d . . . C17 C 1.1230(5) 1.1392(2) 0.2228(2) 0.0251(8) Uani 1 1 d . . . C18 C 1.0287(5) 1.0706(3) 0.2173(2) 0.0254(8) Uani 1 1 d . . . C19 C 0.8116(6) 1.1074(3) 0.1174(3) 0.0443(11) Uani 1 1 d . . . H19A H 0.6791 1.1189 0.1141 0.066 Uiso 1 1 calc R . . H19B H 0.8626 1.0569 0.0900 0.066 Uiso 1 1 calc R . . H19C H 0.8706 1.1595 0.0884 0.066 Uiso 1 1 calc R . . C20 C 1.3808(5) 1.2058(2) 0.2514(2) 0.0260(8) Uani 1 1 d . . . H20A H 1.5105 1.1947 0.2651 0.031 Uiso 1 1 calc R . . C21 C 1.2473(5) 1.2388(2) 0.3210(2) 0.0250(8) Uani 1 1 d . . . C22 C 1.0656(5) 1.2545(2) 0.3016(2) 0.0242(8) Uani 1 1 d . . . C23 C 0.9263(5) 1.2807(2) 0.3592(2) 0.0248(8) Uani 1 1 d . . . C24 C 0.9668(5) 1.2938(3) 0.4366(2) 0.0278(8) Uani 1 1 d . . . C25 C 1.1479(5) 1.2809(3) 0.4530(2) 0.0309(9) Uani 1 1 d . . . H25A H 1.1750 1.2919 0.5055 0.037 Uiso 1 1 calc R . . C26 C 1.2906(6) 1.2526(3) 0.3963(2) 0.0321(9) Uani 1 1 d . . . H26A H 1.4139 1.2431 0.4091 0.038 Uiso 1 1 calc R . . C27 C 0.6766(6) 1.3788(3) 0.3004(3) 0.0383(10) Uani 1 1 d . . . H27A H 0.5496 1.3792 0.2895 0.057 Uiso 1 1 calc R . . H27B H 0.7532 1.3962 0.2467 0.057 Uiso 1 1 calc R . . H27C H 0.6805 1.4204 0.3384 0.057 Uiso 1 1 calc R . . C28 C 1.0424(5) 1.2364(2) 0.2154(2) 0.0265(8) Uani 1 1 d . . . H28A H 0.9115 1.2465 0.2036 0.032 Uiso 1 1 calc R . . C29 C 1.1703(5) 1.2931(2) 0.1477(2) 0.0276(9) Uani 1 1 d . . . C30 C 1.3550(5) 1.2768(2) 0.1670(2) 0.0270(8) Uani 1 1 d . . . C31 C 1.4887(6) 1.3225(3) 0.1117(3) 0.0345(10) Uani 1 1 d . . . H31A H 1.6121 1.3130 0.1243 0.041 Uiso 1 1 calc R . . C32 C 1.4434(7) 1.3836(3) 0.0358(3) 0.0426(11) Uani 1 1 d . . . H32A H 1.5372 1.4122 -0.0012 0.051 Uiso 1 1 calc R . . C33 C 1.2614(8) 1.4006(3) 0.0168(3) 0.0440(12) Uani 1 1 d . . . H33A H 1.2293 1.4416 -0.0320 0.053 Uiso 1 1 calc R . . C34 C 1.1263(7) 1.3544(3) 0.0732(3) 0.0367(10) Uani 1 1 d . . . H34A H 1.0027 1.3646 0.0609 0.044 Uiso 1 1 calc R . . C35 C 0.6179(8) 0.8562(5) -0.0011(4) 0.0694(17) Uani 1 1 d . . . H35A H 0.6161 0.9123 -0.0422 0.083 Uiso 1 1 calc R . . H35B H 0.6332 0.8071 -0.0334 0.083 Uiso 1 1 calc R . . C37 C 1.2232(11) 0.9359(4) 0.5728(3) 0.0678(18) Uani 1 1 d . . . H37A H 1.2899 0.9857 0.5442 0.102 Uiso 1 1 calc R . . H37B H 1.2803 0.8823 0.5517 0.102 Uiso 1 1 calc R . . H37C H 1.2279 0.9275 0.6341 0.102 Uiso 1 1 calc R . . C46 C 0.6318(10) 0.7032(6) 0.3232(5) 0.084(2) Uani 1 1 d . . . H46A H 0.7471 0.7052 0.2837 0.101 Uiso 1 1 calc R . . H46B H 0.5304 0.7028 0.2894 0.101 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 Cl1 0.0678(13) 0.341(5) 0.0754(14) -0.089(2) 0.0133(10) -0.039(2) Cl2 0.0721(15) 0.409(7) 0.123(2) -0.123(3) -0.0341(14) -0.017(2) Cl3 0.0453(8) 0.0663(9) 0.0807(11) 0.0012(8) -0.0259(7) -0.0015(6) Cl4 0.0528(9) 0.0735(11) 0.1345(17) -0.0538(11) -0.0266(9) 0.0054(7) O1 0.0542(19) 0.0330(16) 0.0331(15) -0.0183(13) 0.0038(13) -0.0034(14) O2 0.0221(14) 0.0311(14) 0.0376(15) -0.0112(12) -0.0058(11) -0.0020(11) O3 0.0219(13) 0.0264(14) 0.0383(15) -0.0093(11) -0.0014(11) -0.0018(10) O4 0.247(8) 0.0279(19) 0.0319(19) -0.0155(15) 0.036(3) -0.032(3) C1 0.056(3) 0.029(2) 0.051(3) -0.020(2) -0.011(2) 0.0002(19) C2 0.105(6) 0.097(5) 0.119(6) -0.084(5) -0.069(5) 0.039(4) C3 0.066(3) 0.042(3) 0.049(3) -0.024(2) 0.001(2) 0.010(2) C4 0.104(6) 0.056(4) 0.122(6) -0.056(4) 0.043(5) -0.044(4) C5 0.028(2) 0.034(2) 0.040(2) -0.0175(18) 0.0001(16) -0.0058(16) C6 0.028(2) 0.030(2) 0.0295(19) -0.0097(16) -0.0032(15) -0.0042(15) C7 0.0225(18) 0.0264(19) 0.037(2) -0.0094(16) -0.0059(15) -0.0033(14) C8 0.0269(19) 0.0230(18) 0.033(2) -0.0116(16) 0.0020(15) -0.0065(15) C9 0.0212(18) 0.031(2) 0.031(2) -0.0089(16) 0.0012(15) -0.0026(15) C10 0.0252(19) 0.0223(18) 0.038(2) -0.0072(16) 0.0028(16) 0.0002(15) C11 0.035(2) 0.041(2) 0.028(2) -0.0116(17) 0.0021(17) 0.0049(18) C12 0.034(2) 0.026(2) 0.051(2) -0.0099(18) -0.0157(19) -0.0055(17) C13 0.0281(19) 0.0254(19) 0.0274(18) -0.0043(15) -0.0033(15) -0.0050(15) C14 0.028(2) 0.0233(18) 0.039(2) -0.0112(16) 0.0001(16) -0.0022(15) C15 0.0237(19) 0.030(2) 0.034(2) -0.0086(16) -0.0039(15) 0.0004(15) C16 0.0228(18) 0.0297(19) 0.0256(18) -0.0100(15) 0.0009(14) -0.0051(15) C17 0.0274(19) 0.0246(18) 0.0235(18) -0.0064(14) -0.0033(14) -0.0006(15) C18 0.0195(18) 0.0307(19) 0.0266(18) -0.0081(15) 0.0000(14) -0.0033(14) C19 0.038(2) 0.057(3) 0.041(2) -0.015(2) -0.019(2) 0.006(2) C20 0.0200(18) 0.0280(19) 0.0314(19) -0.0086(16) -0.0030(14) -0.0032(14) C21 0.0227(18) 0.0274(18) 0.0260(18) -0.0061(15) -0.0013(14) -0.0057(14) C22 0.0234(18) 0.0217(17) 0.0278(19) -0.0051(14) -0.0015(14) -0.0042(14) C23 0.0230(18) 0.0211(17) 0.0306(19) -0.0058(15) -0.0030(15) -0.0024(14) C24 0.0279(19) 0.0307(19) 0.0261(18) -0.0089(15) -0.0009(15) -0.0043(15) C25 0.034(2) 0.037(2) 0.0249(19) -0.0111(16) -0.0003(16) -0.0085(17) C26 0.028(2) 0.039(2) 0.032(2) -0.0080(17) -0.0038(16) -0.0084(17) C27 0.036(2) 0.028(2) 0.052(3) -0.0075(18) -0.0132(19) 0.0014(17) C28 0.0254(19) 0.0233(18) 0.0324(19) -0.0088(15) -0.0032(15) -0.0039(14) C29 0.032(2) 0.0218(18) 0.0315(19) -0.0130(15) -0.0027(16) -0.0021(15) C30 0.028(2) 0.0247(18) 0.0302(19) -0.0119(15) -0.0007(15) -0.0038(15) C31 0.037(2) 0.032(2) 0.038(2) -0.0169(17) 0.0069(17) -0.0115(17) C32 0.056(3) 0.037(2) 0.037(2) -0.0124(19) 0.008(2) -0.018(2) C33 0.073(3) 0.028(2) 0.032(2) -0.0065(18) 0.000(2) -0.009(2) C34 0.048(3) 0.031(2) 0.033(2) -0.0106(17) -0.0042(18) -0.0031(18) C35 0.059(4) 0.094(5) 0.069(4) -0.044(3) -0.008(3) -0.015(3) C37 0.111(5) 0.047(3) 0.035(3) 0.006(2) -0.011(3) 0.013(3) C46 0.062(4) 0.123(6) 0.077(4) -0.037(4) 0.018(3) -0.043(4) _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 Cl1 C35 1.718(6) . ? Cl2 C35 1.720(6) . ? Cl3 C46 1.678(8) . ? Cl4 C46 1.858(9) . ? O1 C8 1.338(4) . ? O1 H1 0.8400 . ? O2 C18 1.390(4) . ? O2 C19 1.435(5) . ? O3 C23 1.393(4) . ? O3 C27 1.467(5) . ? O4 C37 1.563(9) . ? O4 H4 0.8400 . ? C1 C5 1.478(5) . ? C1 C3 1.532(7) . ? C1 C2 1.554(8) . ? C1 C4 1.606(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.416(6) . ? C5 C6 1.427(6) . ? C6 C7 1.359(5) . ? C6 H6A 0.9500 . ? C7 C8 1.433(6) . ? C7 C12 1.559(5) . ? C8 C9 1.433(5) . ? C9 C10 1.368(5) . ? C9 C11 1.534(6) . ? C10 H10A 0.9500 . ? C11 C24 1.513(5) 2_776 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.538(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.379(5) . ? C13 C18 1.418(5) . ? C14 C15 1.406(5) . ? C14 H14A 0.9500 . ? C15 C16 1.394(5) . ? C15 H15A 0.9500 . ? C16 C17 1.405(5) . ? C16 C20 1.518(5) . ? C17 C18 1.377(5) . ? C17 C28 1.535(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.507(5) . ? C20 C30 1.598(5) . ? C20 H20A 1.0000 . ? C21 C26 1.365(5) . ? C21 C22 1.403(5) . ? C22 C23 1.362(5) . ? C22 C28 1.512(5) . ? C23 C24 1.386(5) . ? C24 C25 1.384(5) . ? C24 C11 1.513(5) 2_776 ? C25 C26 1.379(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.560(5) . ? C28 H28A 1.0000 . ? C29 C30 1.425(5) . ? C29 C34 1.431(6) . ? C30 C31 1.408(6) . ? C31 C32 1.450(7) . ? C31 H31A 0.9500 . ? C32 C33 1.403(7) . ? C32 H32A 0.9500 . ? C33 C34 1.426(7) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? 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 C8 O1 H1 109.5 . . ? C18 O2 C19 114.7(3) . . ? C23 O3 C27 115.0(3) . . ? C37 O4 H4 93.2 . . ? C5 C1 C3 108.2(4) . . ? C5 C1 C2 109.8(4) . . ? C3 C1 C2 107.5(5) . . ? C5 C1 C4 110.3(4) . . ? C3 C1 C4 106.1(5) . . ? C2 C1 C4 114.6(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 120.0(3) . . ? C10 C5 C1 118.5(4) . . ? C6 C5 C1 121.4(4) . . ? C7 C6 C5 122.8(3) . . ? C7 C6 H6A 118.6 . . ? C5 C6 H6A 118.6 . . ? C6 C7 C8 114.9(3) . . ? C6 C7 C12 120.2(3) . . ? C8 C7 C12 124.6(3) . . ? O1 C8 C9 119.5(3) . . ? O1 C8 C7 115.7(3) . . ? C9 C8 C7 124.8(3) . . ? C10 C9 C8 117.1(3) . . ? C10 C9 C11 117.9(3) . . ? C8 C9 C11 124.9(3) . . ? C9 C10 C5 120.4(4) . . ? C9 C10 H10A 119.8 . . ? C5 C10 H10A 119.8 . . ? C24 C11 C9 115.3(3) 2_776 . ? C24 C11 H11A 108.4 2_776 . ? C9 C11 H11A 108.4 . . ? C24 C11 H11B 108.4 2_776 . ? C9 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? C13 C12 C7 116.8(3) . . ? C13 C12 H12A 108.1 . . ? C7 C12 H12A 108.1 . . ? C13 C12 H12B 108.1 . . ? C7 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C14 C13 C18 119.6(3) . . ? C14 C13 C12 122.4(3) . . ? C18 C13 C12 117.9(3) . . ? C13 C14 C15 121.3(3) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 118.4(3) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 C20 126.8(3) . . ? C17 C16 C20 112.5(3) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 C28 125.5(3) . . ? C16 C17 C28 114.1(3) . . ? C17 C18 O2 118.9(3) . . ? C17 C18 C13 119.5(3) . . ? O2 C18 C13 121.5(3) . . ? O2 C19 H19A 109.5 . . ? O2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C16 103.2(3) . . ? C21 C20 C30 106.3(3) . . ? C16 C20 C30 107.4(3) . . ? C21 C20 H20A 113.0 . . ? C16 C20 H20A 113.0 . . ? C30 C20 H20A 113.0 . . ? C26 C21 C22 121.3(3) . . ? C26 C21 C20 125.8(3) . . ? C22 C21 C20 112.9(3) . . ? C23 C22 C21 120.6(3) . . ? C23 C22 C28 125.1(3) . . ? C21 C22 C28 114.3(3) . . ? C22 C23 C24 119.1(3) . . ? C22 C23 O3 119.2(3) . . ? C24 C23 O3 121.7(3) . . ? C25 C24 C23 119.2(3) . . ? C25 C24 C11 122.3(3) . 2_776 ? C23 C24 C11 118.5(3) . 2_776 ? C26 C25 C24 122.6(3) . . ? C26 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? C21 C26 C25 117.2(4) . . ? C21 C26 H26A 121.4 . . ? C25 C26 H26A 121.4 . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C28 C17 101.1(3) . . ? C22 C28 C29 107.7(3) . . ? C17 C28 C29 108.5(3) . . ? C22 C28 H28A 112.9 . . ? C17 C28 H28A 112.9 . . ? C29 C28 H28A 112.9 . . ? C30 C29 C34 119.6(4) . . ? C30 C29 C28 111.0(3) . . ? C34 C29 C28 129.4(4) . . ? C31 C30 C29 118.2(4) . . ? C31 C30 C20 128.6(4) . . ? C29 C30 C20 113.2(3) . . ? C30 C31 C32 121.8(4) . . ? C30 C31 H31A 119.1 . . ? C32 C31 H31A 119.1 . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 117.7(4) . . ? C32 C33 H33A 121.1 . . ? C34 C33 H33A 121.1 . . ? C33 C34 C29 122.4(4) . . ? C33 C34 H34A 118.8 . . ? C29 C34 H34A 118.8 . . ? Cl1 C35 Cl2 110.3(4) . . ? Cl1 C35 H35A 109.6 . . ? Cl2 C35 H35A 109.6 . . ? Cl1 C35 H35B 109.6 . . ? Cl2 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? O4 C37 H37A 109.5 . . ? O4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Cl3 C46 Cl4 113.8(4) . . ? Cl3 C46 H46A 108.8 . . ? Cl4 C46 H46A 108.8 . . ? Cl3 C46 H46B 108.8 . . ? Cl4 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? 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 C3 C1 C5 C10 -81.9(5) . . . . ? C2 C1 C5 C10 161.1(5) . . . . ? C4 C1 C5 C10 33.9(6) . . . . ? C3 C1 C5 C6 95.5(5) . . . . ? C2 C1 C5 C6 -21.5(7) . . . . ? C4 C1 C5 C6 -148.7(5) . . . . ? C10 C5 C6 C7 -0.5(6) . . . . ? C1 C5 C6 C7 -177.9(4) . . . . ? C5 C6 C7 C8 0.8(5) . . . . ? C5 C6 C7 C12 -173.8(3) . . . . ? C6 C7 C8 O1 -179.9(3) . . . . ? C12 C7 C8 O1 -5.7(5) . . . . ? C6 C7 C8 C9 0.0(6) . . . . ? C12 C7 C8 C9 174.3(3) . . . . ? O1 C8 C9 C10 178.8(3) . . . . ? C7 C8 C9 C10 -1.1(6) . . . . ? O1 C8 C9 C11 -4.9(6) . . . . ? C7 C8 C9 C11 175.1(4) . . . . ? C8 C9 C10 C5 1.4(5) . . . . ? C11 C9 C10 C5 -175.2(3) . . . . ? C6 C5 C10 C9 -0.6(6) . . . . ? C1 C5 C10 C9 176.8(4) . . . . ? C10 C9 C11 C24 -124.2(4) . . . 2_776 ? C8 C9 C11 C24 59.6(5) . . . 2_776 ? C6 C7 C12 C13 -125.8(4) . . . . ? C8 C7 C12 C13 60.1(5) . . . . ? C7 C12 C13 C14 20.4(6) . . . . ? C7 C12 C13 C18 -157.9(4) . . . . ? C18 C13 C14 C15 3.2(6) . . . . ? C12 C13 C14 C15 -175.1(4) . . . . ? C13 C14 C15 C16 -1.3(6) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C14 C15 C16 C20 176.1(3) . . . . ? C15 C16 C17 C18 2.5(5) . . . . ? C20 C16 C17 C18 -175.5(3) . . . . ? C15 C16 C17 C28 179.1(3) . . . . ? C20 C16 C17 C28 1.1(4) . . . . ? C16 C17 C18 O2 175.6(3) . . . . ? C28 C17 C18 O2 -0.5(5) . . . . ? C16 C17 C18 C13 -0.6(5) . . . . ? C28 C17 C18 C13 -176.8(3) . . . . ? C19 O2 C18 C17 90.6(4) . . . . ? C19 O2 C18 C13 -93.3(4) . . . . ? C14 C13 C18 C17 -2.2(5) . . . . ? C12 C13 C18 C17 176.2(3) . . . . ? C14 C13 C18 O2 -178.3(3) . . . . ? C12 C13 C18 O2 0.1(5) . . . . ? C15 C16 C20 C21 -120.8(4) . . . . ? C17 C16 C20 C21 57.1(4) . . . . ? C15 C16 C20 C30 127.1(4) . . . . ? C17 C16 C20 C30 -55.1(4) . . . . ? C16 C20 C21 C26 121.9(4) . . . . ? C30 C20 C21 C26 -125.1(4) . . . . ? C16 C20 C21 C22 -57.7(4) . . . . ? C30 C20 C21 C22 55.3(4) . . . . ? C26 C21 C22 C23 -2.6(5) . . . . ? C20 C21 C22 C23 177.0(3) . . . . ? C26 C21 C22 C28 179.6(3) . . . . ? C20 C21 C22 C28 -0.8(4) . . . . ? C21 C22 C23 C24 1.6(5) . . . . ? C28 C22 C23 C24 179.1(3) . . . . ? C21 C22 C23 O3 -175.6(3) . . . . ? C28 C22 C23 O3 2.0(5) . . . . ? C27 O3 C23 C22 -93.0(4) . . . . ? C27 O3 C23 C24 89.9(4) . . . . ? C22 C23 C24 C25 0.7(5) . . . . ? O3 C23 C24 C25 177.7(3) . . . . ? C22 C23 C24 C11 -177.6(3) . . . 2_776 ? O3 C23 C24 C11 -0.5(5) . . . 2_776 ? C23 C24 C25 C26 -2.1(6) . . . . ? C11 C24 C25 C26 176.2(4) 2_776 . . . ? C22 C21 C26 C25 1.3(6) . . . . ? C20 C21 C26 C25 -178.3(4) . . . . ? C24 C25 C26 C21 1.1(6) . . . . ? C23 C22 C28 C17 -120.1(4) . . . . ? C21 C22 C28 C17 57.6(4) . . . . ? C23 C22 C28 C29 126.2(4) . . . . ? C21 C22 C28 C29 -56.2(4) . . . . ? C18 C17 C28 C22 118.6(4) . . . . ? C16 C17 C28 C22 -57.7(4) . . . . ? C18 C17 C28 C29 -128.2(4) . . . . ? C16 C17 C28 C29 55.4(4) . . . . ? C22 C28 C29 C30 54.5(4) . . . . ? C17 C28 C29 C30 -54.1(4) . . . . ? C22 C28 C29 C34 -126.3(4) . . . . ? C17 C28 C29 C34 125.0(4) . . . . ? C34 C29 C30 C31 0.3(5) . . . . ? C28 C29 C30 C31 179.6(3) . . . . ? C34 C29 C30 C20 -179.1(3) . . . . ? C28 C29 C30 C20 0.1(4) . . . . ? C21 C20 C30 C31 125.5(4) . . . . ? C16 C20 C30 C31 -124.5(4) . . . . ? C21 C20 C30 C29 -55.1(4) . . . . ? C16 C20 C30 C29 54.9(4) . . . . ? C29 C30 C31 C32 -1.1(5) . . . . ? C20 C30 C31 C32 178.3(4) . . . . ? C30 C31 C32 C33 1.7(6) . . . . ? C31 C32 C33 C34 -1.5(6) . . . . ? C32 C33 C34 C29 0.7(6) . . . . ? C30 C29 C34 C33 -0.2(6) . . . . ? C28 C29 C34 C33 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.104 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.150