# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 # SUBMISSION DETAILS _publ_contact_author_name 'Edwin Weber' _publ_contact_author_address ; Institut fur Organische Chemie TU Bergakademie Freiberg Leipziger Strasse 29 D-09596 Freiberg/Sachsen Germany ; _publ_contact_author_email Edwin.Weber@chemie.tu-freiberg.de _publ_contact_author_fax '49(03731) 393170' _publ_contact_author_phone '49(03731) 392386' # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, crystalline inclusion and structural study of bulkily stoppered and rigid framework molecular constructions ; loop_ _publ_author_name _publ_author_address T.Muller ; Institut fur Organische Chemie TU Bergakademie Freiberg Leipziger Strasse 29 D-09596 Freiberg/Sachsen Germany ; W.Seichter ; Institut fur Organische Chemie TU Bergakademie Freiberg Leipziger Strasse 29 D-09596 Freiberg/Sachsen Germany ; E.Weber ; Institut fur Organische Chemie TU Bergakademie Freiberg Leipziger Strasse 29 D-09596 Freiberg/Sachsen Germany ; # TEXT _publ_section_abstract ; A series of compounds 1-5 featuring a structure composed of linear or trigonal ethynyl and aryl containing rigid construction elements with attached terminal adamantyl stoppers were synthesized to comparatively study their crystalline host versus lattice packing properties. While only the linear tetraethynylenic prototype molecule 1 exhibited versatile inclusion behavior, the compounds 2-5 were found to be inefficient. X-ray crystal structures of the inclusion compounds between 1 and THF, cyclohexanol and aniline as well as of the unsolvated compounds 3, 4 and 5 are reported, throwing light on the respective modes of crystalline packing affected by molecular dimension and shape parameters. ; data_tomu13ad _database_code_depnum_ccdc_archive 'CCDC 119507' _publ_contact_authors_phone '03731 392140' _publ_contact_authors_fax '03731 393170' #4. TEXT _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C49 H72 O3.50' _chemical_formula_weight 717.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 10.5400(10) _cell_length_b 11.6160(10) _cell_length_c 18.944(6) _cell_angle_alpha 101.420(10) _cell_angle_beta 104.020(10) _cell_angle_gamma 98.350(10) _cell_volume 2159.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 178(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.891 _cell_measurement_theta_max 38.596 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method ? _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 178(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 9117 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 74.62 _reflns_number_total 8839 _reflns_number_observed 7135 _reflns_observed_criterion >2sigma(I) _computing_data_collection Enraf-Nonius _computing_cell_refinement Enraf-Nonius _computing_data_reduction Helena _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON _computing_publication_material PLATON _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+2.0839P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8834 _refine_ls_number_parameters 778 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_obs 0.0993 _refine_ls_wR_factor_all 0.2778 _refine_ls_wR_factor_obs 0.2639 _refine_ls_goodness_of_fit_all 1.205 _refine_ls_goodness_of_fit_obs 1.303 _refine_ls_restrained_S_all 1.222 _refine_ls_restrained_S_obs 1.303 _refine_ls_shift/esd_max 0.801 _refine_ls_shift/esd_mean 0.052 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1890(3) 0.6707(2) 0.49561(15) 0.0347(6) Uani 1 d . . C2 C 0.0666(3) 0.6968(2) 0.4418(2) 0.0427(7) Uani 1 d . . H2A H 0.0712(34) 0.6928(30) 0.3903(21) 0.054(9) Uiso 1 d . . H2B H -0.0079(33) 0.6332(29) 0.4353(17) 0.044(8) Uiso 1 d . . C3 C 0.0427(3) 0.8211(2) 0.4755(2) 0.0450(7) Uani 1 d . . H3 H -0.0379(32) 0.8361(28) 0.4371(18) 0.047(8) Uiso 1 d . . C4 C 0.0172(3) 0.8227(3) 0.5517(2) 0.0543(8) Uani 1 d . . H4A H -0.0048(33) 0.9029(30) 0.5755(18) 0.051(9) Uiso 1 d . . H4B H -0.0613(45) 0.7575(39) 0.5438(24) 0.082(13) Uiso 1 d . . C5 C 0.1406(4) 0.7995(3) 0.6055(2) 0.0526(8) Uani 1 d . . H5 H 0.1282(32) 0.8024(28) 0.6523(19) 0.046(8) Uiso 1 d . . C6 C 0.1637(4) 0.6745(3) 0.5728(2) 0.0501(7) Uani 1 d . . H6A H 0.0803(34) 0.6131(30) 0.5610(18) 0.048(9) Uiso 1 d . . H6B H 0.2445(41) 0.6623(34) 0.6066(22) 0.071(11) Uiso 1 d . . C7 C 0.3117(3) 0.7689(2) 0.5053(2) 0.0424(6) Uani 1 d . . H7A H 0.3323(34) 0.7692(30) 0.4584(20) 0.055(10) Uiso 1 d . . H7B H 0.3880(33) 0.7545(28) 0.5413(18) 0.048(8) Uiso 1 d . . C8 C 0.2861(3) 0.8920(3) 0.5382(2) 0.0451(7) Uani 1 d . . H8 H 0.3620(35) 0.9497(30) 0.5444(19) 0.051(9) Uiso 1 d . . C9 C 0.1651(3) 0.9160(2) 0.4851(2) 0.0460(7) Uani 1 d . . H9A H 0.1787(35) 0.9123(31) 0.4332(21) 0.058(10) Uiso 1 d . . H9B H 0.1538(35) 1.0049(32) 0.5149(20) 0.062(10) Uiso 1 d . . C10 C 0.2623(3) 0.8945(3) 0.6140(2) 0.0528(8) Uani 1 d . . H10A H 0.3491(38) 0.8794(32) 0.6553(21) 0.066(10) Uiso 1 d . . H10B H 0.2484(36) 0.9714(34) 0.6361(20) 0.062(10) Uiso 1 d . . C11 C 0.2149(3) 0.5533(2) 0.4638(2) 0.0389(6) Uani 1 d . . C12 C 0.2394(3) 0.4589(2) 0.4382(2) 0.0390(6) Uani 1 d . . C13 C 0.2696(3) 0.3503(2) 0.4123(2) 0.0397(6) Uani 1 d . . C14 C 0.2961(3) 0.2534(2) 0.3916(2) 0.0402(6) Uani 1 d . . C15 C 0.3275(3) 0.1450(2) 0.3719(2) 0.0412(6) Uani 1 d . . C16 C 0.3574(3) 0.0476(2) 0.3567(2) 0.0416(6) Uani 1 d . . C17 C 0.3964(3) -0.0596(2) 0.3422(2) 0.0406(6) Uani 1 d . . C18 C 0.4370(3) -0.1509(2) 0.3320(2) 0.0391(6) Uani 1 d . . C19 C 0.4912(3) -0.2605(2) 0.32173(14) 0.0349(6) Uani 1 d . . C20 C 0.5526(3) -0.2703(3) 0.2553(2) 0.0449(7) Uani 1 d . . H20A H 0.6276(30) -0.1910(27) 0.2700(16) 0.039(7) Uiso 1 d . . H20B H 0.4709(37) -0.2748(31) 0.2053(20) 0.062(10) Uiso 1 d . . C21 C 0.6096(3) -0.3858(3) 0.2450(2) 0.0502(7) Uani 1 d . . H21 H 0.6439(30) -0.3999(27) 0.1997(18) 0.043(8) Uiso 1 d . . C22 C 0.4987(4) -0.4931(3) 0.2305(2) 0.0582(9) Uani 1 d . . H22A H 0.4343(37) -0.5014(32) 0.1882(21) 0.057(10) Uiso 1 d . . H22B H 0.5324(33) -0.5677(31) 0.2164(18) 0.051(9) Uiso 1 d . . C23 C 0.4387(3) -0.4855(3) 0.2968(2) 0.0489(7) Uani 1 d . . H23 H 0.3681(39) -0.5603(35) 0.2875(21) 0.069(11) Uiso 1 d . . C24 C 0.3796(3) -0.3717(2) 0.3065(2) 0.0421(6) Uani 1 d . . H24A H 0.3424(33) -0.3613(29) 0.3541(19) 0.053(9) Uiso 1 d . . H24B H 0.3081(35) -0.3731(30) 0.2617(20) 0.055(9) Uiso 1 d . . C25 C 0.6022(3) -0.2556(3) 0.3936(2) 0.0413(6) Uani 1 d . . H25A H 0.5589(32) -0.2568(28) 0.4385(18) 0.047(8) Uiso 1 d . . H25B H 0.6743(35) -0.1842(32) 0.3958(19) 0.056(9) Uiso 1 d . . C26 C 0.6597(3) -0.3706(3) 0.3826(2) 0.0472(7) Uani 1 d . . H26 H 0.7459(39) -0.3683(34) 0.4293(22) 0.070(11) Uiso 1 d . . C27 C 0.5476(3) -0.4777(3) 0.3688(2) 0.0516(8) Uani 1 d . . H27A H 0.5107(34) -0.4772(29) 0.4155(19) 0.052(9) Uiso 1 d . . H27B H 0.5891(42) -0.5597(38) 0.3619(23) 0.083(13) Uiso 1 d . . C28 C 0.7191(3) -0.3784(3) 0.3166(2) 0.0527(8) Uani 1 d . . H28A H 0.7954(33) -0.3099(29) 0.3278(17) 0.044(8) Uiso 1 d . . H28B H 0.7624(37) -0.4547(33) 0.3118(20) 0.063(10) Uiso 1 d . . O110 O 0.2289(5) 0.0507(6) 0.9119(3) 0.077(2) Uani 0.50 d P 1 H110 H 0.2103(5) 0.0374(6) 0.9506(3) 0.115 Uiso 0.50 calc PR 1 C110 C 0.0342(16) 0.1712(18) 0.8841(10) 0.052(3) Uani 0.50 d P 1 C210 C -0.0645(24) 0.1951(23) 0.8322(11) 0.105(8) Uani 0.50 d P 1 C310 C -0.0093(26) 0.2186(27) 0.7616(12) 0.159(12) Uani 0.50 d P 1 C410 C 0.0201(14) 0.1101(17) 0.7264(9) 0.072(5) Uani 0.50 d P 1 C510 C 0.1310(15) 0.0812(15) 0.7844(8) 0.063(3) Uani 0.50 d P 1 C610 C 0.1043(14) 0.0645(10) 0.8571(8) 0.061(3) Uani 0.50 d P 1 O120 O -0.0188(6) 0.1575(5) 0.9460(3) 0.078(2) Uani 0.50 d P 2 H120 H -0.0276(6) 0.2224(5) 0.9713(3) 0.117 Uiso 0.50 calc PR 2 C120 C 0.0670(28) 0.1833(28) 0.8961(15) 0.118(9) Uani 0.50 d P 2 C220 C -0.0776(19) 0.2045(24) 0.8240(14) 0.106(8) Uani 0.50 d P 2 C320 C -0.0367(16) 0.2105(14) 0.7576(11) 0.074(4) Uani 0.50 d P 2 C420 C 0.0244(23) 0.0923(22) 0.7317(11) 0.124(9) Uani 0.50 d P 2 C520 C 0.1467(34) 0.0665(32) 0.7907(17) 0.170(12) Uani 0.50 d P 2 C620 C 0.0759(29) 0.0656(27) 0.8557(13) 0.171(12) Uani 0.50 d P 2 C111 C -0.0442(8) 0.3980(6) 1.0940(3) 0.121(2) Uani 1 d . . O111 O -0.0350(14) 0.3798(9) 1.0247(4) 0.150(6) Uani 0.52 d P 1 H11C H -0.1115(14) 0.3528(9) 0.9946(4) 0.224 Uiso 0.52 calc PR 1 C211 C 0.0675(8) 0.4418(9) 1.1583(5) 0.087(3) Uani 0.52 d P 1 C311 C 0.0323(15) 0.4592(13) 1.2317(7) 0.101(5) Uani 0.52 d P 1 C411 C -0.0390(20) 0.3480(13) 1.2437(7) 0.103(5) Uani 0.52 d P 1 C511 C -0.1557(12) 0.2930(13) 1.1806(7) 0.114(4) Uani 0.52 d P 1 C611 C -0.1226(14) 0.2711(11) 1.1041(6) 0.142(6) Uani 0.52 d P 1 O121 O -0.0755(18) 0.4323(14) 1.0146(10) 0.203(9) Uani 0.48 d P 2 H121 H -0.0211(18) 0.4099(14) 0.9916(10) 0.304 Uiso 0.48 calc PR 2 C221 C -0.1186(17) 0.4228(17) 1.1439(8) 0.149(7) Uani 0.48 d P 2 C321 C -0.0491(36) 0.4083(38) 1.2288(13) 0.221(19) Uani 0.48 d P 2 C421 C -0.0034(26) 0.2893(25) 1.2178(11) 0.185(11) Uani 0.48 d P 2 C521 C 0.0907(15) 0.2939(13) 1.1628(9) 0.130(5) Uani 0.48 d P 2 C621 C 0.0505(20) 0.3094(19) 1.0883(11) 0.177(8) Uani 0.48 d P 2 O113 O 0.3510(7) -0.3469(6) 0.0267(4) 0.091(2) Uani 0.50 d P . H113 H 0.3868(7) -0.2737(6) 0.0399(4) 0.137 Uiso 0.50 calc PR . C113 C 0.4388(7) -0.4074(6) 0.0324(3) 0.112(2) Uani 1 d . . C213 C 0.3590(7) -0.5369(6) 0.0065(3) 0.119(2) Uani 1 d . . C313 C 0.4581(7) -0.6192(6) 0.0116(3) 0.116(2) Uani 1 d . . O114 O -0.1869(8) -0.0395(8) 0.9514(4) 0.076(2) Uani 0.50 d P 1 H114 H -0.1360(8) 0.0262(8) 0.9566(4) 0.113 Uiso 0.50 calc PR 1 C114 C -0.3089(9) -0.0500(8) 0.8944(5) 0.071(2) Uani 0.50 d P 1 C214 C -0.3975(11) -0.1649(8) 0.8867(7) 0.094(3) Uani 0.50 d P 1 C314 C -0.5302(11) -0.1832(7) 0.8263(6) 0.087(3) Uani 0.50 d P 1 C414 C -0.6031(10) -0.0802(8) 0.8449(7) 0.094(3) Uani 0.50 d P 1 C514 C -0.5140(10) 0.0378(8) 0.8537(8) 0.100(3) Uani 0.50 d P 1 C614 C -0.3779(14) 0.0555(9) 0.9114(5) 0.072(2) Uani 0.50 d P 1 O124 O -0.5038(5) 0.1147(4) 0.9235(3) 0.075(2) Uani 0.50 d P 2 H124 H -0.5875(5) 0.1020(4) 0.9079(3) 0.113 Uiso 0.50 calc PR 2 C124 C -0.4605(10) 0.0057(7) 0.9077(5) 0.060(2) Uani 0.50 d P 2 C224 C -0.5072(8) -0.0496(6) 0.8209(4) 0.059(2) Uani 0.50 d P 2 C324 C -0.4517(13) -0.1617(7) 0.8030(6) 0.081(3) Uani 0.50 d P 2 C424 C -0.3072(11) -0.1395(8) 0.8323(5) 0.082(3) Uani 0.50 d P 2 C524 C -0.2475(17) -0.0781(16) 0.9198(8) 0.105(5) Uani 0.50 d P 2 C624 C -0.3097(10) 0.0315(10) 0.9358(5) 0.075(2) Uani 0.50 d P 2 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 0.0355(13) 0.0276(12) 0.0403(14) 0.0050(10) 0.0079(10) 0.0130(10) C2 0.0372(14) 0.0301(13) 0.052(2) 0.0026(12) -0.0005(12) 0.0124(11) C3 0.0407(15) 0.0327(13) 0.056(2) 0.0051(12) 0.0017(13) 0.0190(11) C4 0.047(2) 0.040(2) 0.082(2) 0.009(2) 0.028(2) 0.0200(14) C5 0.077(2) 0.048(2) 0.046(2) 0.0123(13) 0.030(2) 0.031(2) C6 0.066(2) 0.042(2) 0.053(2) 0.0170(14) 0.024(2) 0.026(2) C7 0.0368(14) 0.0359(14) 0.051(2) 0.0025(12) 0.0099(13) 0.0125(11) C8 0.0385(15) 0.0314(13) 0.057(2) 0.0000(12) 0.0063(13) 0.0065(11) C9 0.055(2) 0.0295(13) 0.052(2) 0.0078(12) 0.0109(14) 0.0159(12) C10 0.060(2) 0.044(2) 0.043(2) -0.0048(13) 0.0014(14) 0.0209(15) C11 0.0393(14) 0.0332(13) 0.0442(15) 0.0079(11) 0.0090(11) 0.0138(11) C12 0.0418(14) 0.0319(13) 0.0450(15) 0.0097(11) 0.0112(12) 0.0137(11) C13 0.0444(15) 0.0329(13) 0.0455(15) 0.0110(11) 0.0142(12) 0.0141(11) C14 0.0411(14) 0.0308(13) 0.050(2) 0.0091(11) 0.0135(12) 0.0118(11) C15 0.0404(14) 0.0326(13) 0.050(2) 0.0064(11) 0.0109(12) 0.0118(11) C16 0.0382(14) 0.0314(13) 0.051(2) 0.0042(11) 0.0082(12) 0.0101(11) C17 0.0385(14) 0.0305(13) 0.048(2) 0.0033(11) 0.0071(12) 0.0092(11) C18 0.0369(13) 0.0315(13) 0.0430(14) 0.0022(11) 0.0048(11) 0.0087(11) C19 0.0395(13) 0.0270(12) 0.0349(13) 0.0017(10) 0.0055(10) 0.0126(10) C20 0.054(2) 0.041(2) 0.043(2) 0.0111(12) 0.0140(13) 0.0186(13) C21 0.062(2) 0.052(2) 0.042(2) 0.0097(13) 0.0184(14) 0.0255(15) C22 0.078(2) 0.041(2) 0.048(2) -0.0045(14) 0.008(2) 0.022(2) C23 0.055(2) 0.0322(14) 0.052(2) 0.0072(12) 0.0047(14) 0.0061(13) C24 0.0412(15) 0.0348(14) 0.044(2) 0.0046(11) 0.0029(12) 0.0103(11) C25 0.0388(14) 0.0402(15) 0.0393(14) 0.0022(11) 0.0050(11) 0.0105(12) C26 0.046(2) 0.050(2) 0.044(2) 0.0126(13) 0.0046(13) 0.0184(13) C27 0.055(2) 0.047(2) 0.056(2) 0.0202(14) 0.0104(15) 0.0223(14) C28 0.048(2) 0.058(2) 0.056(2) 0.0120(15) 0.0171(14) 0.026(2) O110 0.062(3) 0.113(5) 0.061(3) 0.030(3) 0.016(2) 0.023(3) C110 0.056(4) 0.059(6) 0.035(6) 0.003(4) 0.017(4) -0.003(4) C210 0.149(17) 0.149(15) 0.069(9) 0.046(8) 0.069(10) 0.099(13) C310 0.182(21) 0.299(29) 0.077(11) 0.097(15) 0.073(12) 0.174(20) C410 0.056(6) 0.083(8) 0.055(8) 0.019(6) -0.009(5) -0.019(6) C510 0.068(6) 0.088(7) 0.043(6) 0.015(5) 0.024(5) 0.036(5) C610 0.069(5) 0.054(5) 0.060(7) 0.004(4) 0.029(4) 0.005(4) O120 0.100(4) 0.082(4) 0.057(3) 0.018(3) 0.028(3) 0.021(3) C120 0.175(24) 0.118(16) 0.056(10) 0.004(9) 0.031(14) 0.043(15) C220 0.060(7) 0.151(17) 0.114(13) 0.073(11) 0.007(7) 0.014(8) C320 0.059(5) 0.080(7) 0.083(10) 0.022(6) 0.027(5) -0.002(6) C420 0.174(18) 0.166(17) 0.056(9) 0.017(9) 0.059(10) 0.084(13) C520 0.177(22) 0.276(29) 0.108(14) 0.099(15) 0.052(14) 0.112(19) C620 0.230(25) 0.281(26) 0.086(12) 0.105(15) 0.080(13) 0.169(21) C111 0.155(6) 0.138(5) 0.081(4) 0.043(4) 0.037(4) 0.032(5) O111 0.261(15) 0.103(7) 0.050(4) -0.013(4) 0.068(6) -0.071(8) C211 0.062(5) 0.099(7) 0.078(6) 0.027(5) -0.009(4) -0.013(4) C311 0.123(10) 0.094(7) 0.059(6) 0.008(5) 0.015(6) -0.034(8) C411 0.143(14) 0.082(7) 0.058(7) 0.017(5) 0.007(7) -0.017(8) C511 0.101(8) 0.141(10) 0.086(7) 0.023(7) 0.034(6) -0.028(7) C611 0.167(11) 0.131(9) 0.074(6) -0.029(6) 0.050(7) -0.093(9) O121 0.158(11) 0.186(15) 0.239(17) 0.134(13) -0.021(10) -0.027(10) C221 0.168(13) 0.243(19) 0.102(9) 0.078(11) 0.066(9) 0.148(14) C321 0.303(38) 0.377(51) 0.099(15) 0.107(26) 0.117(23) 0.266(39) C421 0.254(25) 0.270(27) 0.089(11) 0.077(13) 0.058(13) 0.177(23) C521 0.127(11) 0.132(11) 0.130(11) -0.016(9) 0.060(9) 0.045(9) C621 0.166(16) 0.213(19) 0.144(14) 0.081(14) -0.024(12) 0.077(15) O113 0.081(4) 0.058(3) 0.120(5) -0.002(3) 0.026(4) 0.004(3) C113 0.139(5) 0.117(5) 0.067(3) 0.007(3) 0.026(3) 0.009(4) C213 0.141(6) 0.099(4) 0.099(4) 0.005(3) 0.025(4) 0.008(4) C313 0.151(6) 0.121(5) 0.068(3) 0.021(3) 0.031(3) 0.008(4) O114 0.072(4) 0.096(5) 0.052(4) 0.022(3) 0.004(3) 0.013(4) C114 0.066(5) 0.062(5) 0.074(6) 0.010(5) 0.005(4) 0.016(4) C214 0.090(7) 0.063(5) 0.126(9) 0.030(5) 0.011(6) 0.030(5) C314 0.094(7) 0.047(4) 0.091(7) -0.005(4) -0.011(6) 0.017(5) C414 0.074(6) 0.058(5) 0.136(9) 0.012(5) 0.008(6) 0.021(4) C514 0.081(6) 0.060(5) 0.145(10) 0.021(6) 0.001(6) 0.028(5) C614 0.100(8) 0.056(5) 0.060(5) 0.007(4) 0.017(5) 0.034(6) O124 0.065(3) 0.051(3) 0.097(4) -0.014(3) 0.032(3) 0.002(2) C124 0.076(5) 0.047(4) 0.059(4) 0.007(3) 0.034(4) 0.007(4) C224 0.074(5) 0.039(3) 0.056(4) -0.006(3) 0.022(3) 0.006(3) C324 0.130(9) 0.039(4) 0.090(6) 0.006(4) 0.069(7) 0.017(5) C424 0.109(7) 0.071(5) 0.070(5) 0.012(4) 0.026(5) 0.042(5) C524 0.118(12) 0.147(15) 0.081(9) 0.051(9) 0.031(8) 0.089(12) C624 0.076(6) 0.087(7) 0.053(5) -0.002(5) 0.011(4) 0.024(5) _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 C11 1.470(3) . ? C1 C7 1.543(4) . ? C1 C6 1.543(4) . ? C1 C2 1.547(4) . ? C2 C3 1.541(4) . ? C3 C9 1.519(4) . ? C3 C4 1.528(5) . ? C4 C5 1.540(5) . ? C5 C10 1.518(5) . ? C5 C6 1.539(4) . ? C7 C8 1.531(4) . ? C8 C10 1.512(5) . ? C8 C9 1.519(4) . ? C11 C12 1.199(4) . ? C12 C13 1.370(4) . ? C13 C14 1.213(4) . ? C14 C15 1.352(4) . ? C15 C16 1.217(4) . ? C16 C17 1.364(4) . ? C17 C18 1.198(4) . ? C18 C19 1.467(3) . ? C19 C20 1.541(4) . ? C19 C24 1.543(4) . ? C19 C25 1.550(4) . ? C20 C21 1.545(4) . ? C21 C22 1.511(5) . ? C21 C28 1.531(5) . ? C22 C23 1.531(5) . ? C23 C27 1.532(4) . ? C23 C24 1.539(4) . ? C25 C26 1.543(4) . ? C26 C27 1.519(5) . ? C26 C28 1.522(5) . ? O110 C610 1.52(2) . ? C110 C210 1.35(3) . ? C110 C610 1.59(3) . ? C210 C310 1.64(3) . ? C310 C410 1.42(3) . ? C410 C510 1.53(2) . ? C510 C610 1.51(2) . ? O120 C120 1.50(3) . ? C120 C620 1.46(4) . ? C120 C220 1.87(4) . ? C220 C320 1.44(3) . ? C320 C420 1.64(3) . ? C420 C520 1.60(3) . ? C520 C620 1.59(4) . ? C111 O111 1.318(9) . ? C111 C221 1.382(13) . ? C111 C211 1.419(10) . ? C111 C621 1.54(2) . ? C111 O121 1.60(2) . ? C111 C611 1.652(12) . ? C211 C311 1.51(2) . ? C311 C411 1.48(2) . ? C411 C511 1.45(2) . ? C511 C611 1.552(15) . ? C221 C321 1.65(3) . ? C321 C421 1.52(3) . ? C421 C521 1.61(2) . ? C521 C621 1.43(2) . ? O113 C113 1.238(8) . ? C113 C213 1.534(8) . ? C113 C313 1.554(9) 2_645 ? C213 C313 1.514(9) . ? C313 C113 1.554(9) 2_645 ? O114 C114 1.436(10) . ? C114 C214 1.473(13) . ? C114 C614 1.532(13) . ? C214 C314 1.533(14) . ? C314 C414 1.542(13) . ? C414 C514 1.499(14) . ? C514 C614 1.54(2) . ? O124 C124 1.409(9) . ? C124 C624 1.513(13) . ? C124 C224 1.568(10) . ? C224 C324 1.515(11) . ? C324 C424 1.45(2) . ? C424 C524 1.60(2) . ? C524 C624 1.53(2) . ? 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 C11 C1 C7 109.1(2) . . ? C11 C1 C6 110.8(2) . . ? C7 C1 C6 108.8(2) . . ? C11 C1 C2 110.0(2) . . ? C7 C1 C2 108.5(2) . . ? C6 C1 C2 109.6(2) . . ? C3 C2 C1 109.2(2) . . ? C9 C3 C4 109.6(3) . . ? C9 C3 C2 109.2(2) . . ? C4 C3 C2 109.6(3) . . ? C3 C4 C5 109.6(2) . . ? C10 C5 C6 109.9(3) . . ? C10 C5 C4 109.9(3) . . ? C6 C5 C4 108.6(3) . . ? C1 C6 C5 109.5(2) . . ? C8 C7 C1 109.7(2) . . ? C10 C8 C9 110.1(3) . . ? C10 C8 C7 109.6(3) . . ? C9 C8 C7 109.3(2) . . ? C3 C9 C8 110.0(2) . . ? C8 C10 C5 109.7(2) . . ? C12 C11 C1 178.3(3) . . ? C11 C12 C13 177.4(3) . . ? C14 C13 C12 177.9(3) . . ? C13 C14 C15 177.2(3) . . ? C16 C15 C14 177.9(3) . . ? C15 C16 C17 177.4(3) . . ? C18 C17 C16 176.6(3) . . ? C17 C18 C19 177.9(3) . . ? C18 C19 C20 110.0(2) . . ? C18 C19 C24 110.2(2) . . ? C20 C19 C24 109.4(2) . . ? C18 C19 C25 109.4(2) . . ? C20 C19 C25 108.6(2) . . ? C24 C19 C25 109.4(2) . . ? C21 C20 C19 109.6(2) . . ? C22 C21 C28 110.3(3) . . ? C22 C21 C20 109.2(3) . . ? C28 C21 C20 108.6(3) . . ? C21 C22 C23 110.6(3) . . ? C27 C23 C22 110.0(3) . . ? C27 C23 C24 108.9(2) . . ? C22 C23 C24 108.7(3) . . ? C23 C24 C19 109.4(2) . . ? C26 C25 C19 109.4(2) . . ? C27 C26 C28 111.1(3) . . ? C27 C26 C25 108.4(2) . . ? C28 C26 C25 109.1(3) . . ? C26 C27 C23 110.1(3) . . ? C26 C28 C21 109.7(3) . . ? C210 C110 C610 117.4(15) . . ? C110 C210 C310 109.4(16) . . ? C410 C310 C210 108.1(20) . . ? C310 C410 C510 106.6(14) . . ? C610 C510 C410 118.1(13) . . ? O110 C610 C510 111.4(11) . . ? O110 C610 C110 117.3(10) . . ? C510 C610 C110 106.1(12) . . ? C620 C120 O120 104.7(22) . . ? C620 C120 C220 96.9(19) . . ? O120 C120 C220 92.0(17) . . ? C320 C220 C120 108.2(17) . . ? C220 C320 C420 109.7(17) . . ? C520 C420 C320 118.1(17) . . ? C420 C520 C620 96.4(20) . . ? C120 C620 C520 115.1(25) . . ? O111 C111 C211 123.6(9) . . ? C221 C111 C621 130.8(11) . . ? C221 C111 O121 122.5(11) . . ? C621 C111 O121 104.7(11) . . ? O111 C111 C611 107.8(7) . . ? C211 C111 C611 106.1(7) . . ? C111 C211 C311 114.2(8) . . ? C211 C311 C411 113.9(11) . . ? C511 C411 C311 110.4(12) . . ? C411 C511 C611 112.9(11) . . ? C511 C611 C111 109.7(8) . . ? C111 C221 C321 113.9(12) . . ? C421 C321 C221 106.0(17) . . ? C321 C421 C521 106.8(19) . . ? C621 C521 C421 125.2(15) . . ? C521 C621 C111 103.0(15) . . ? O113 C113 C213 103.3(6) . . ? O113 C113 C313 114.7(7) . 2_645 ? C213 C113 C313 113.6(5) . 2_645 ? C113 C213 C313 107.6(6) . . ? C213 C313 C113 112.1(5) . 2_645 ? O114 C114 C214 108.7(8) . . ? O114 C114 C614 112.3(8) . . ? C214 C114 C614 111.0(9) . . ? C114 C214 C314 111.9(8) . . ? C214 C314 C414 110.5(7) . . ? C514 C414 C314 109.8(9) . . ? C414 C514 C614 112.6(9) . . ? C514 C614 C114 111.7(8) . . ? O124 C124 C624 108.2(8) . . ? O124 C124 C224 109.2(7) . . ? C624 C124 C224 110.2(7) . . ? C324 C224 C124 109.5(7) . . ? C424 C324 C224 112.4(7) . . ? C324 C424 C524 116.1(9) . . ? C624 C524 C424 106.9(9) . . ? C124 C624 C524 114.2(11) . . ? _refine_diff_density_max 0.392 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.068 # Attachment 'Tomu3.cif' data_model3 _database_code_depnum_ccdc_archive 'CCDC 288444' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H38' _chemical_formula_weight 470.66 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.401(3) _cell_length_b 9.533(3) _cell_length_c 11.538(3) _cell_angle_alpha 103.85(3) _cell_angle_beta 92.84(3) _cell_angle_gamma 105.71(3) _cell_volume 653.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.160 _cell_measurement_theta_max 49.345 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method ? _exptl_crystal_F_000 254 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 2918 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.98 _diffrn_reflns_theta_max 74.73 _reflns_number_total 2667 _reflns_number_observed 2219 _reflns_observed_criterion >2sigma(I) _computing_data_collection Enraf-Nonius _computing_cell_refinement Enraf-Nonius _computing_data_reduction Helena _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON _computing_publication_material PLATON _refine_special_details ; Refinement on F^2^ for ALL reflections except for 176 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.1522P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2491 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_obs 0.0385 _refine_ls_wR_factor_all 0.1163 _refine_ls_wR_factor_obs 0.1050 _refine_ls_goodness_of_fit_all 0.994 _refine_ls_goodness_of_fit_obs 1.027 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.027 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.7132(2) 0.65500(14) 0.16492(11) 0.0256(3) Uani 1 d . . H1 H 0.5910(27) 0.7009(18) 0.1595(14) 0.039(4) Uiso 1 d . . C2 C 0.7873(2) 0.59550(14) 0.05841(11) 0.0242(3) Uani 1 d . . H2 H 0.7168(27) 0.5985(18) -0.0186(14) 0.038(4) Uiso 1 d . . C3 C 0.9600(2) 0.53165(12) 0.05734(9) 0.0201(3) Uani 1 d . . C4 C 1.0553(2) 0.52981(14) 0.16890(10) 0.0257(3) Uani 1 d . . H4 H 1.1790(26) 0.4854(17) 0.1745(13) 0.034(4) Uiso 1 d . . C5 C 0.9822(2) 0.58917(14) 0.27579(11) 0.0272(3) Uani 1 d . . H5 H 1.0541(26) 0.5855(17) 0.3540(14) 0.036(4) Uiso 1 d . . C6 C 0.8101(2) 0.65327(13) 0.27551(10) 0.0234(3) Uani 1 d . . C7 C 0.7367(2) 0.71413(14) 0.38764(11) 0.0266(3) Uani 1 d . . C8 C 0.6872(2) 0.76235(14) 0.48434(11) 0.0255(3) Uani 1 d . . C9 C 0.6462(2) 0.81853(13) 0.60888(10) 0.0210(3) Uani 1 d . . C10 C 0.4075(2) 0.74749(14) 0.62693(10) 0.0224(3) Uani 1 d . . H10A H 0.3049(24) 0.7776(16) 0.5725(13) 0.029(4) Uiso 1 d . . H10B H 0.3706(24) 0.6334(17) 0.6038(13) 0.029(4) Uiso 1 d . . C11 C 0.3755(2) 0.80480(14) 0.75932(10) 0.0227(3) Uani 1 d . . H11 H 0.2194(24) 0.7559(16) 0.7695(12) 0.027(4) Uiso 1 d . . C12 C 0.5293(2) 0.76058(15) 0.84045(11) 0.0251(3) Uani 1 d . . H12A H 0.5037(23) 0.7950(16) 0.9283(13) 0.027(4) Uiso 1 d . . H12B H 0.4957(24) 0.6485(17) 0.8212(13) 0.029(4) Uiso 1 d . . C13 C 0.7669(2) 0.83230(14) 0.82444(11) 0.0250(3) Uani 1 d . . H13 H 0.8680(25) 0.7997(17) 0.8785(13) 0.033(4) Uiso 1 d . . C14 C 0.7998(2) 0.77505(15) 0.69249(11) 0.0253(3) Uani 1 d . . H14A H 0.9576(27) 0.8208(18) 0.6786(14) 0.037(4) Uiso 1 d . . H14B H 0.7667(25) 0.6602(18) 0.6690(14) 0.036(4) Uiso 1 d . . C15 C 0.8171(2) 1.00475(15) 0.85732(11) 0.0277(3) Uani 1 d . . H15A H 0.9727(28) 1.0538(19) 0.8496(14) 0.041(4) Uiso 1 d . . H15B H 0.7937(25) 1.0429(17) 0.9449(14) 0.034(4) Uiso 1 d . . C16 C 0.4254(2) 0.97699(14) 0.79131(11) 0.0264(3) Uani 1 d . . H16A H 0.3993(25) 1.0163(17) 0.8787(13) 0.033(4) Uiso 1 d . . H16B H 0.3213(26) 1.0081(17) 0.7363(14) 0.036(4) Uiso 1 d . . C17 C 0.6639(2) 1.04885(14) 0.77573(11) 0.0250(3) Uani 1 d . . H17 H 0.6963(23) 1.1604(16) 0.7955(12) 0.027(4) Uiso 1 d . . C18 C 0.6986(2) 0.99275(14) 0.64382(11) 0.0249(3) Uani 1 d . . H18A H 0.8577(26) 1.0400(17) 0.6333(13) 0.033(4) Uiso 1 d . . H18B H 0.5969(25) 1.0251(16) 0.5893(13) 0.032(4) Uiso 1 d . . 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 0.0319(7) 0.0247(6) 0.0231(6) 0.0057(5) 0.0075(5) 0.0125(5) C2 0.0303(7) 0.0260(6) 0.0193(6) 0.0064(5) 0.0059(5) 0.0122(5) C3 0.0262(6) 0.0163(5) 0.0176(6) 0.0038(4) 0.0056(5) 0.0057(4) C4 0.0316(7) 0.0287(6) 0.0195(6) 0.0053(5) 0.0043(5) 0.0140(5) C5 0.0350(7) 0.0296(6) 0.0175(6) 0.0046(5) 0.0038(5) 0.0118(5) C6 0.0304(7) 0.0187(6) 0.0193(6) 0.0027(4) 0.0083(5) 0.0055(5) C7 0.0316(7) 0.0245(6) 0.0231(6) 0.0042(5) 0.0071(5) 0.0083(5) C8 0.0287(6) 0.0257(6) 0.0224(6) 0.0044(5) 0.0055(5) 0.0096(5) C9 0.0230(6) 0.0234(6) 0.0165(5) 0.0031(4) 0.0044(4) 0.0083(5) C10 0.0218(6) 0.0246(6) 0.0198(6) 0.0040(5) 0.0012(4) 0.0070(5) C11 0.0202(6) 0.0265(6) 0.0211(6) 0.0058(5) 0.0042(4) 0.0063(5) C12 0.0291(7) 0.0259(6) 0.0205(6) 0.0076(5) 0.0032(5) 0.0070(5) C13 0.0240(6) 0.0308(7) 0.0210(6) 0.0066(5) -0.0005(5) 0.0099(5) C14 0.0232(6) 0.0307(7) 0.0241(6) 0.0052(5) 0.0034(5) 0.0129(5) C15 0.0269(7) 0.0292(7) 0.0201(6) 0.0011(5) 0.0008(5) 0.0021(5) C16 0.0313(7) 0.0283(7) 0.0225(6) 0.0042(5) 0.0083(5) 0.0148(5) C17 0.0320(7) 0.0203(6) 0.0210(6) 0.0022(4) 0.0062(5) 0.0070(5) C18 0.0304(7) 0.0236(6) 0.0206(6) 0.0060(5) 0.0062(5) 0.0071(5) _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 1.388(2) . ? C1 C6 1.397(2) . ? C2 C3 1.398(2) . ? C3 C4 1.403(2) . ? C3 C3 1.493(2) 2_765 ? C4 C5 1.388(2) . ? C5 C6 1.397(2) . ? C6 C7 1.442(2) . ? C7 C8 1.194(2) . ? C8 C9 1.472(2) . ? C9 C10 1.541(2) . ? C9 C14 1.545(2) . ? C9 C18 1.549(2) . ? C10 C11 1.538(2) . ? C11 C16 1.532(2) . ? C11 C12 1.532(2) . ? C12 C13 1.530(2) . ? C13 C15 1.534(2) . ? C13 C14 1.535(2) . ? C15 C17 1.531(2) . ? C16 C17 1.534(2) . ? C17 C18 1.536(2) . ? 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 120.73(12) . . ? C1 C2 C3 121.71(11) . . ? C2 C3 C4 117.05(11) . . ? C2 C3 C3 121.57(13) . 2_765 ? C4 C3 C3 121.38(14) . 2_765 ? C5 C4 C3 121.59(12) . . ? C4 C5 C6 120.72(12) . . ? C1 C6 C5 118.20(11) . . ? C1 C6 C7 122.03(12) . . ? C5 C6 C7 119.76(11) . . ? C8 C7 C6 175.56(14) . . ? C7 C8 C9 174.04(13) . . ? C8 C9 C10 111.42(10) . . ? C8 C9 C14 107.81(10) . . ? C10 C9 C14 108.93(10) . . ? C8 C9 C18 110.78(10) . . ? C10 C9 C18 109.45(10) . . ? C14 C9 C18 108.36(10) . . ? C11 C10 C9 109.39(10) . . ? C16 C11 C12 109.85(11) . . ? C16 C11 C10 109.08(10) . . ? C12 C11 C10 109.76(10) . . ? C13 C12 C11 109.81(10) . . ? C12 C13 C15 109.68(11) . . ? C12 C13 C14 108.78(11) . . ? C15 C13 C14 109.47(11) . . ? C13 C14 C9 110.42(10) . . ? C17 C15 C13 109.52(10) . . ? C11 C16 C17 109.71(10) . . ? C15 C17 C16 109.82(11) . . ? C15 C17 C18 109.69(11) . . ? C16 C17 C18 109.06(11) . . ? C17 C18 C9 109.68(10) . . ? _refine_diff_density_max 0.239 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.034 # Attachment 'Tomu4.cif' data_tomu_6x_0m _database_code_depnum_ccdc_archive 'CCDC 288445' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38' _chemical_formula_weight 494.68 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6620(2) _cell_length_b 10.1600(3) _cell_length_c 11.1284(3) _cell_angle_alpha 114.744(2) _cell_angle_beta 92.734(2) _cell_angle_gamma 101.360(2) _cell_volume 663.47(3) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 266 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9633 _exptl_absorpt_correction_T_max 0.9899 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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_% none _diffrn_reflns_number 49528 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 45.73 _reflns_number_total 11373 _reflns_number_gt 8033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _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^)+(0.1000P)^2^+0.8048P] 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_number_reflns 11373 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.001 _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 0.87788(8) 0.73030(6) 0.52867(5) 0.01204(7) Uani 1 1 d . . . C2 C 1.08568(9) 0.83586(7) 0.61262(6) 0.01622(9) Uani 1 1 d . . . H2A H 1.1914 0.7776 0.6046 0.019 Uiso 1 1 calc R . . H2B H 1.1342 0.9105 0.5784 0.019 Uiso 1 1 calc R . . C3 C 1.05775(10) 0.91590(7) 0.76016(6) 0.01806(9) Uani 1 1 d . . . H3 H 1.1926 0.9840 0.8137 0.022 Uiso 1 1 calc R . . C4 C 0.98529(10) 0.79999(8) 0.81326(6) 0.01810(9) Uani 1 1 d . . . H4A H 1.0899 0.7411 0.8061 0.022 Uiso 1 1 calc R . . H4B H 0.9693 0.8512 0.9087 0.022 Uiso 1 1 calc R . . C5 C 0.77785(9) 0.69584(6) 0.73182(5) 0.01431(8) Uani 1 1 d . . . H5 H 0.7307 0.6205 0.7667 0.017 Uiso 1 1 calc R . . C6 C 0.80542(9) 0.61547(6) 0.58439(5) 0.01337(8) Uani 1 1 d . . . H6A H 0.6725 0.5468 0.5316 0.016 Uiso 1 1 calc R . . H6B H 0.9090 0.5556 0.5763 0.016 Uiso 1 1 calc R . . C7 C 0.71364(9) 0.82242(7) 0.54276(5) 0.01530(8) Uani 1 1 d . . . H7A H 0.7573 0.8965 0.5073 0.018 Uiso 1 1 calc R . . H7B H 0.5797 0.7554 0.4900 0.018 Uiso 1 1 calc R . . C8 C 0.68740(10) 0.90299(7) 0.69024(6) 0.01687(9) Uani 1 1 d . . . H8 H 0.5818 0.9627 0.6984 0.020 Uiso 1 1 calc R . . C9 C 0.61578(10) 0.78776(7) 0.74423(6) 0.01734(9) Uani 1 1 d . . . H9A H 0.4811 0.7208 0.6928 0.021 Uiso 1 1 calc R . . H9B H 0.5974 0.8394 0.8392 0.021 Uiso 1 1 calc R . . C10 C 0.89549(12) 1.00761(7) 0.77126(6) 0.02070(11) Uani 1 1 d . . . H10A H 0.8789 1.0617 0.8662 0.025 Uiso 1 1 calc R . . H10B H 0.9422 1.0821 0.7366 0.025 Uiso 1 1 calc R . . C11 C 0.90585(9) 0.65644(7) 0.38791(5) 0.01460(8) Uani 1 1 d . . . C12 C 0.93345(9) 0.60275(6) 0.27201(5) 0.01394(8) Uani 1 1 d . . . C13 C 0.96784(8) 0.54784(6) 0.13560(5) 0.01179(7) Uani 1 1 d . . . C14 C 0.80568(8) 0.44732(6) 0.03195(5) 0.01153(7) Uani 1 1 d . . . C15 C 0.60887(9) 0.39140(6) 0.06043(5) 0.01440(8) Uani 1 1 d . . . H15 H 0.5873 0.4196 0.1508 0.017 Uiso 1 1 calc R . . C16 C 0.45090(9) 0.29783(7) -0.04040(6) 0.01606(9) Uani 1 1 d . . . H16 H 0.3212 0.2614 -0.0196 0.019 Uiso 1 1 calc R . . C17 C 0.47999(9) 0.25483(7) -0.17624(6) 0.01581(8) Uani 1 1 d . . . H17 H 0.3685 0.1919 -0.2457 0.019 Uiso 1 1 calc R . . C18 C 0.66783(9) 0.30363(6) -0.20737(5) 0.01436(8) Uani 1 1 d . . . H18 H 0.6860 0.2726 -0.2985 0.017 Uiso 1 1 calc R . . C19 C 0.83707(8) 0.40054(6) -0.10479(5) 0.01165(7) Uani 1 1 d . . . 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 0.01337(17) 0.01450(18) 0.00798(14) 0.00474(13) 0.00268(12) 0.00287(14) C2 0.01413(19) 0.0189(2) 0.01374(18) 0.00742(16) 0.00142(15) -0.00059(16) C3 0.0199(2) 0.0170(2) 0.01206(18) 0.00427(16) -0.00208(16) -0.00122(17) C4 0.0219(2) 0.0218(2) 0.01046(17) 0.00738(17) 0.00002(16) 0.00459(19) C5 0.0175(2) 0.01659(19) 0.01114(16) 0.00760(15) 0.00532(14) 0.00487(15) C6 0.01551(18) 0.01319(17) 0.01116(16) 0.00502(14) 0.00397(14) 0.00307(14) C7 0.0186(2) 0.0183(2) 0.01078(17) 0.00693(15) 0.00258(15) 0.00680(17) C8 0.0227(2) 0.0172(2) 0.01269(18) 0.00611(16) 0.00539(16) 0.00937(18) C9 0.0197(2) 0.0212(2) 0.01428(19) 0.00863(17) 0.00829(17) 0.00837(18) C10 0.0314(3) 0.0133(2) 0.01322(19) 0.00254(16) 0.00187(19) 0.00415(19) C11 0.01691(19) 0.0181(2) 0.00894(15) 0.00558(15) 0.00399(14) 0.00475(16) C12 0.01639(19) 0.01688(19) 0.00897(15) 0.00555(14) 0.00387(13) 0.00468(15) C13 0.01417(17) 0.01361(17) 0.00825(14) 0.00491(13) 0.00351(12) 0.00402(14) C14 0.01318(17) 0.01285(17) 0.00910(15) 0.00507(13) 0.00328(12) 0.00325(13) C15 0.01527(19) 0.01631(19) 0.01198(17) 0.00676(15) 0.00459(14) 0.00260(15) C16 0.01520(19) 0.0169(2) 0.01503(19) 0.00710(16) 0.00358(15) 0.00108(16) C17 0.01524(19) 0.0162(2) 0.01365(18) 0.00539(16) 0.00112(15) 0.00150(15) C18 0.01547(19) 0.01562(19) 0.01029(16) 0.00435(14) 0.00168(14) 0.00306(15) C19 0.01378(17) 0.01273(17) 0.00868(15) 0.00462(13) 0.00272(12) 0.00357(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 C11 1.4665(7) . ? C1 C6 1.5463(7) . ? C1 C2 1.5467(8) . ? C1 C7 1.5475(8) . ? C2 C3 1.5372(8) . ? C3 C4 1.5346(9) . ? C3 C10 1.5379(10) . ? C4 C5 1.5338(9) . ? C5 C6 1.5358(7) . ? C5 C9 1.5364(8) . ? C7 C8 1.5340(8) . ? C8 C9 1.5347(9) . ? C8 C10 1.5371(10) . ? C11 C12 1.2116(7) . ? C12 C13 1.4292(7) . ? C13 C14 1.4146(7) . ? C13 C19 1.4164(7) 2_765 ? C14 C15 1.4280(7) . ? C14 C19 1.4315(7) . ? C15 C16 1.3677(8) . ? C16 C17 1.4220(8) . ? C17 C18 1.3684(8) . ? C18 C19 1.4292(7) . ? C19 C13 1.4165(7) 2_765 ? 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 C11 C1 C6 111.37(4) . . ? C11 C1 C2 109.39(4) . . ? C6 C1 C2 108.57(4) . . ? C11 C1 C7 109.79(4) . . ? C6 C1 C7 108.50(4) . . ? C2 C1 C7 109.18(5) . . ? C3 C2 C1 109.94(5) . . ? C4 C3 C2 109.51(5) . . ? C4 C3 C10 109.84(5) . . ? C2 C3 C10 109.07(5) . . ? C5 C4 C3 109.60(5) . . ? C4 C5 C6 109.25(5) . . ? C4 C5 C9 109.48(5) . . ? C6 C5 C9 109.62(4) . . ? C5 C6 C1 110.23(4) . . ? C8 C7 C1 110.05(4) . . ? C7 C8 C9 109.57(5) . . ? C7 C8 C10 109.33(5) . . ? C9 C8 C10 109.55(5) . . ? C8 C9 C5 109.56(5) . . ? C8 C10 C3 109.60(5) . . ? C12 C11 C1 176.56(6) . . ? C11 C12 C13 176.69(6) . . ? C14 C13 C19 120.29(4) . 2_765 ? C14 C13 C12 120.20(5) . . ? C19 C13 C12 119.47(5) 2_765 . ? C13 C14 C15 121.37(4) . . ? C13 C14 C19 119.88(4) . . ? C15 C14 C19 118.74(5) . . ? C16 C15 C14 121.00(5) . . ? C15 C16 C17 120.30(5) . . ? C18 C17 C16 120.31(5) . . ? C17 C18 C19 121.00(5) . . ? C13 C19 C18 121.58(4) 2_765 . ? C13 C19 C14 119.81(5) 2_765 . ? C18 C19 C14 118.60(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 C11 C1 C2 C3 179.13(5) . . . . ? C6 C1 C2 C3 -59.15(6) . . . . ? C7 C1 C2 C3 58.97(6) . . . . ? C1 C2 C3 C4 60.08(7) . . . . ? C1 C2 C3 C10 -60.14(6) . . . . ? C2 C3 C4 C5 -60.31(7) . . . . ? C10 C3 C4 C5 59.45(6) . . . . ? C3 C4 C5 C6 60.20(6) . . . . ? C3 C4 C5 C9 -59.85(6) . . . . ? C4 C5 C6 C1 -60.21(6) . . . . ? C9 C5 C6 C1 59.75(6) . . . . ? C11 C1 C6 C5 179.89(5) . . . . ? C2 C1 C6 C5 59.38(6) . . . . ? C7 C1 C6 C5 -59.17(6) . . . . ? C11 C1 C7 C8 -178.65(5) . . . . ? C6 C1 C7 C8 59.43(6) . . . . ? C2 C1 C7 C8 -58.73(6) . . . . ? C1 C7 C8 C9 -60.35(6) . . . . ? C1 C7 C8 C10 59.72(6) . . . . ? C7 C8 C9 C5 59.97(6) . . . . ? C10 C8 C9 C5 -59.96(6) . . . . ? C4 C5 C9 C8 60.20(6) . . . . ? C6 C5 C9 C8 -59.62(6) . . . . ? C7 C8 C10 C3 -60.70(6) . . . . ? C9 C8 C10 C3 59.37(6) . . . . ? C4 C3 C10 C8 -59.18(6) . . . . ? C2 C3 C10 C8 60.84(7) . . . . ? C6 C1 C11 C12 -172.3(10) . . . . ? C2 C1 C11 C12 -52.3(10) . . . . ? C7 C1 C11 C12 67.5(10) . . . . ? C1 C11 C12 C13 -14.9(19) . . . . ? C11 C12 C13 C14 -114.5(10) . . . . ? C11 C12 C13 C19 63.0(10) . . . 2_765 ? C19 C13 C14 C15 178.78(5) 2_765 . . . ? C12 C13 C14 C15 -3.75(8) . . . . ? C19 C13 C14 C19 -1.63(8) 2_765 . . . ? C12 C13 C14 C19 175.84(5) . . . . ? C13 C14 C15 C16 177.98(5) . . . . ? C19 C14 C15 C16 -1.62(8) . . . . ? C14 C15 C16 C17 -0.25(9) . . . . ? C15 C16 C17 C18 1.66(9) . . . . ? C16 C17 C18 C19 -1.16(9) . . . . ? C17 C18 C19 C13 -179.85(5) . . . 2_765 ? C17 C18 C19 C14 -0.72(8) . . . . ? C13 C14 C19 C13 1.62(8) . . . 2_765 ? C15 C14 C19 C13 -178.78(5) . . . 2_765 ? C13 C14 C19 C18 -177.53(5) . . . . ? C15 C14 C19 C18 2.08(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 45.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.867 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.071 # Attachment 'Tomu_5.cif' data_model5 _database_code_depnum_ccdc_archive 'CCDC 288446' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H48' _chemical_formula_weight 552.80 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 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' _cell_length_a 6.853(3) _cell_length_b 25.898(3) _cell_length_c 37.211(3) _cell_angle_alpha 90.00(3) _cell_angle_beta 95.29(3) _cell_angle_gamma 90.00(3) _cell_volume 6576.1(30) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.923 _cell_measurement_theta_max 28.239 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method ? _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 7361 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 74.91 _reflns_number_total 7360 _reflns_number_observed 5907 _reflns_observed_criterion >2sigma(I) _computing_data_collection Enraf-Nonius _computing_cell_refinement Enraf-Nonius _computing_data_reduction Helena _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON _computing_publication_material PLATON _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+10.7955P] 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 ? _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 2.62(218) _refine_ls_number_reflns 7357 _refine_ls_number_parameters 757 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_obs 0.0696 _refine_ls_wR_factor_all 0.2077 _refine_ls_wR_factor_obs 0.1852 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 1.089 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 1.3736(7) -0.1766(2) -0.05000(13) 0.0310(10) Uani 1 d . . C2 C 1.4640(8) -0.2082(2) -0.02292(13) 0.0308(10) Uani 1 d . . H2 H 1.4085(8) -0.2408(2) -0.01818(13) 0.037 Uiso 1 calc R . C3 C 1.6348(8) -0.1922(2) -0.00280(13) 0.0348(11) Uani 1 d . . C4 C 1.7107(8) -0.1436(2) -0.00944(14) 0.0385(12) Uani 1 d . . H4 H 1.8276(8) -0.1324(2) 0.00402(14) 0.046 Uiso 1 calc R . C5 C 1.6187(8) -0.1115(2) -0.03530(14) 0.0366(11) Uani 1 d . . C6 C 1.4504(8) -0.1286(2) -0.05587(13) 0.0324(11) Uani 1 d . . H6 H 1.3883(8) -0.1069(2) -0.07407(13) 0.039 Uiso 1 calc R . C7 C 1.2065(7) -0.1943(2) -0.07304(13) 0.0302(10) Uani 1 d . . C8 C 1.0766(7) -0.2080(2) -0.09461(13) 0.0310(10) Uani 1 d . . C9 C 0.9154(7) -0.2234(2) -0.12105(12) 0.0266(9) Uani 1 d . . C10 C 0.8551(7) -0.1770(2) -0.14649(13) 0.0299(10) Uani 1 d . . H10A H 0.8145(7) -0.1475(2) -0.13204(13) 0.036 Uiso 1 calc R . H10B H 0.9684(7) -0.1661(2) -0.15932(13) 0.036 Uiso 1 calc R . C11 C 0.6869(7) -0.1929(2) -0.17367(13) 0.0303(10) Uani 1 d . . H11 H 0.6493(7) -0.1631(2) -0.18990(13) 0.036 Uiso 1 calc R . C12 C 0.7493(8) -0.2383(2) -0.19633(13) 0.0313(10) Uani 1 d . . H12A H 0.8629(8) -0.2281(2) -0.20937(13) 0.038 Uiso 1 calc R . H12B H 0.6404(8) -0.2480(2) -0.21440(13) 0.038 Uiso 1 calc R . C13 C 0.8052(7) -0.2848(2) -0.17161(12) 0.0287(10) Uani 1 d . . H13 H 0.8455(7) -0.3144(2) -0.18644(12) 0.034 Uiso 1 calc R . C14 C 0.6292(7) -0.3004(2) -0.15141(13) 0.0308(10) Uani 1 d . . H14A H 0.5187(7) -0.3108(2) -0.16894(13) 0.037 Uiso 1 calc R . H14B H 0.6648(7) -0.3303(2) -0.13558(13) 0.037 Uiso 1 calc R . C15 C 0.5672(7) -0.2551(2) -0.12868(13) 0.0292(10) Uani 1 d . . H15 H 0.4519(7) -0.2655(2) -0.11570(13) 0.035 Uiso 1 calc R . C16 C 0.7356(7) -0.2392(2) -0.10133(12) 0.0303(10) Uani 1 d . . H16A H 0.7710(7) -0.2684(2) -0.08479(12) 0.036 Uiso 1 calc R . H16B H 0.6943(7) -0.2098(2) -0.08677(12) 0.036 Uiso 1 calc R . C17 C 0.9760(7) -0.2691(2) -0.14416(13) 0.0291(10) Uani 1 d . . H17A H 1.0904(7) -0.2592(2) -0.15704(13) 0.035 Uiso 1 calc R . H17B H 1.0144(7) -0.2989(2) -0.12833(13) 0.035 Uiso 1 calc R . C18 C 0.5103(7) -0.2089(2) -0.15376(14) 0.0328(10) Uani 1 d . . H18A H 0.3998(7) -0.2188(2) -0.17145(14) 0.039 Uiso 1 calc R . H18B H 0.4680(7) -0.1795(2) -0.13935(14) 0.039 Uiso 1 calc R . C19 C 1.6927(9) -0.0598(2) -0.04008(15) 0.0425(13) Uani 1 d . . C20 C 1.7426(9) -0.0161(2) -0.04296(15) 0.0414(13) Uani 1 d . . C21 C 1.8025(7) 0.0383(2) -0.04406(12) 0.0304(10) Uani 1 d . . C22 C 1.6630(10) 0.0708(3) -0.0234(2) 0.050(2) Uani 1 d . . H22A H 1.6678(10) 0.0587(3) 0.0019(2) 0.060 Uiso 1 calc R . H22B H 1.5271(10) 0.0666(3) -0.0346(2) 0.060 Uiso 1 calc R . C23 C 1.7210(12) 0.1281(3) -0.0241(2) 0.058(2) Uani 1 d . . H23 H 1.6297(12) 0.1490(3) -0.0104(2) 0.070 Uiso 1 calc R . C24 C 1.9298(12) 0.1330(2) -0.0063(2) 0.056(2) Uani 1 d . . H24A H 1.9696(12) 0.1698(2) -0.0057(2) 0.068 Uiso 1 calc R . H24B H 1.9349(12) 0.1205(2) 0.0190(2) 0.068 Uiso 1 calc R . C25 C 2.0706(9) 0.1018(2) -0.0268(2) 0.0429(13) Uani 1 d . . H25 H 2.2072(9) 0.1061(2) -0.0152(2) 0.051 Uiso 1 calc R . C26 C 2.0597(10) 0.1205(3) -0.0665(2) 0.051(2) Uani 1 d . . H26A H 2.1016(10) 0.1570(3) -0.0672(2) 0.061 Uiso 1 calc R . H26B H 2.1491(10) 0.0996(3) -0.0800(2) 0.061 Uiso 1 calc R . C27 C 1.8519(10) 0.1153(2) -0.08369(14) 0.0421(13) Uani 1 d . . H27 H 1.8455(10) 0.1276(2) -0.10924(14) 0.050 Uiso 1 calc R . C28 C 1.7921(8) 0.0582(2) -0.08315(13) 0.0339(11) Uani 1 d . . H28A H 1.6569(8) 0.0542(2) -0.09470(13) 0.041 Uiso 1 calc R . H28B H 1.8808(8) 0.0375(2) -0.09705(13) 0.041 Uiso 1 calc R . C29 C 2.0135(8) 0.0451(2) -0.02681(14) 0.0363(11) Uani 1 d . . H29A H 2.0237(8) 0.0319(2) -0.00172(14) 0.044 Uiso 1 calc R . H29B H 2.1044(8) 0.0249(2) -0.04053(14) 0.044 Uiso 1 calc R . C30 C 1.7114(12) 0.1466(3) -0.0633(2) 0.056(2) Uani 1 d . . H30A H 1.5763(12) 0.1426(3) -0.0748(2) 0.067 Uiso 1 calc R . H30B H 1.7468(12) 0.1836(3) -0.0639(2) 0.067 Uiso 1 calc R . C31 C 1.7328(8) -0.2245(2) 0.02459(14) 0.0383(12) Uani 1 d . . C32 C 1.8280(9) -0.2483(2) 0.04742(15) 0.0404(12) Uani 1 d . . C33 C 1.9560(8) -0.2764(2) 0.07442(14) 0.0364(11) Uani 1 d . . C34 C 2.1546(11) -0.2841(3) 0.0587(2) 0.063(2) Uani 1 d . . H34A H 2.1353(11) -0.3034(3) 0.0356(2) 0.075 Uiso 1 calc R . H34B H 2.2132(11) -0.2502(3) 0.0538(2) 0.075 Uiso 1 calc R . C35 C 2.2916(11) -0.3144(4) 0.0860(2) 0.075(3) Uani 1 d . . H35 H 2.4186(11) -0.3214(4) 0.0757(2) 0.090 Uiso 1 calc R . C36 C 2.1925(20) -0.3667(3) 0.0950(2) 0.103(4) Uani 1 d . . H36A H 2.1615(20) -0.3866(3) 0.0725(2) 0.124 Uiso 1 calc R . H36B H 2.2849(20) -0.3874(3) 0.1112(2) 0.124 Uiso 1 calc R . C37 C 2.0031(12) -0.3574(3) 0.1134(3) 0.079(3) Uani 1 d . . H37 H 1.9419(12) -0.3906(3) 0.1201(3) 0.094 Uiso 1 calc R . C38 C 2.0364(12) -0.3222(3) 0.1450(2) 0.063(2) Uani 1 d . . H38A H 2.1110(12) -0.3410(3) 0.1650(2) 0.075 Uiso 1 calc R . H38B H 1.9079(12) -0.3126(3) 0.1533(2) 0.075 Uiso 1 calc R . C39 C 2.1436(10) -0.2746(3) 0.1374(2) 0.052(2) Uani 1 d . . H39 H 2.1755(10) -0.2541(3) 0.1600(2) 0.063 Uiso 1 calc R . C40 C 1.9982(10) -0.2437(3) 0.1097(2) 0.052(2) Uani 1 d . . H40A H 1.8741(10) -0.2368(3) 0.1205(2) 0.062 Uiso 1 calc R . H40B H 2.0574(10) -0.2102(3) 0.1038(2) 0.062 Uiso 1 calc R . C41 C 1.8684(13) -0.3276(3) 0.0826(3) 0.086(3) Uani 1 d . . H41A H 1.8542(13) -0.3490(3) 0.0605(3) 0.103 Uiso 1 calc R . H41B H 1.7363(13) -0.3223(3) 0.0908(3) 0.103 Uiso 1 calc R . C42 C 2.3261(10) -0.2838(3) 0.1180(2) 0.056(2) Uani 1 d . . H42A H 2.3806(10) -0.2501(3) 0.1115(2) 0.068 Uiso 1 calc R . H42B H 2.4256(10) -0.3013(3) 0.1348(2) 0.068 Uiso 1 calc R . C1A C 0.9764(8) 0.0579(2) 0.18166(13) 0.0351(11) Uani 1 d . . C2A C 1.0590(9) 0.1063(2) 0.18823(14) 0.0393(12) Uani 1 d . . H2A H 1.1619(9) 0.1173(2) 0.17459(14) 0.047 Uiso 1 calc R . C3A C 0.9946(9) 0.1390(2) 0.21427(14) 0.0377(12) Uani 1 d . . C4A C 0.8452(8) 0.1218(2) 0.23479(13) 0.0339(11) Uani 1 d . . H4A H 0.8000(8) 0.1436(2) 0.25282(13) 0.041 Uiso 1 calc R . C5A C 0.7631(7) 0.0732(2) 0.22891(13) 0.0306(10) Uani 1 d . . C6A C 0.8256(8) 0.0417(2) 0.20176(13) 0.0313(10) Uani 1 d . . H6A H 0.7653(8) 0.0091(2) 0.19696(13) 0.038 Uiso 1 calc R . C7A C 1.0476(9) 0.0257(2) 0.15409(14) 0.0391(12) Uani 1 d . . C8A C 1.1206(8) 0.0014(2) 0.13150(14) 0.0398(12) Uani 1 d . . C9A C 1.2211(8) -0.0262(2) 0.10433(13) 0.0370(11) Uani 1 d . . C10A C 1.4344(11) -0.0335(4) 0.1198(2) 0.066(2) Uani 1 d . . H10C H 1.4390(11) -0.0510(4) 0.1435(2) 0.079 Uiso 1 calc R . H10D H 1.4994(11) 0.0005(4) 0.1233(2) 0.079 Uiso 1 calc R . C11A C 1.5429(11) -0.0671(5) 0.0925(2) 0.085(3) Uani 1 d . . H11A H 1.6798(11) -0.0747(5) 0.1029(2) 0.102 Uiso 1 calc R . C12A C 1.4348(21) -0.1167(3) 0.0836(2) 0.106(4) Uani 1 d . . H12C H 1.4255(21) -0.1369(3) 0.1059(2) 0.127 Uiso 1 calc R . H12D H 1.5089(21) -0.1375(3) 0.0671(2) 0.127 Uiso 1 calc R . C13A C 1.2305(13) -0.1063(3) 0.0658(3) 0.076(3) Uani 1 d . . H13A H 1.1630(13) -0.1396(3) 0.0589(3) 0.091 Uiso 1 calc R . C14A C 1.2324(12) -0.0721(3) 0.0338(2) 0.065(2) Uani 1 d . . H14C H 1.2901(12) -0.0911(3) 0.0143(2) 0.078 Uiso 1 calc R . H14D H 1.0958(12) -0.0631(3) 0.0251(2) 0.078 Uiso 1 calc R . C15A C 1.3448(9) -0.0241(3) 0.0416(2) 0.052(2) Uani 1 d . . H15A H 1.3536(9) -0.0034(3) 0.0192(2) 0.062 Uiso 1 calc R . C16A C 1.2279(10) 0.0062(3) 0.0695(2) 0.052(2) Uani 1 d . . H16C H 1.2925(10) 0.0397(3) 0.0753(2) 0.062 Uiso 1 calc R . H16D H 1.0928(10) 0.0131(3) 0.0587(2) 0.062 Uiso 1 calc R . C17A C 1.1228(13) -0.0781(3) 0.0954(2) 0.072(2) Uani 1 d . . H17C H 0.9835(13) -0.0726(3) 0.0866(2) 0.087 Uiso 1 calc R . H17D H 1.1277(13) -0.0997(3) 0.1174(2) 0.087 Uiso 1 calc R . C18A C 1.5464(11) -0.0336(3) 0.0607(2) 0.059(2) Uani 1 d . . H18C H 1.6303(11) -0.0497(3) 0.0436(2) 0.070 Uiso 1 calc R . H18D H 1.6058(11) 0.0000(3) 0.0683(2) 0.070 Uiso 1 calc R . C19A C 1.0715(9) 0.1902(2) 0.21912(15) 0.0423(13) Uani 1 d . . C20A C 1.1261(9) 0.2342(2) 0.22170(15) 0.0416(13) Uani 1 d . . C21A C 1.1856(7) 0.2882(2) 0.22300(13) 0.0314(10) Uani 1 d . . C22A C 1.3801(8) 0.2952(2) 0.20558(14) 0.0357(11) Uani 1 d . . H22C H 1.4849(8) 0.2749(2) 0.21918(14) 0.043 Uiso 1 calc R . H22D H 1.3649(8) 0.2822(2) 0.18045(14) 0.043 Uiso 1 calc R . C23A C 1.4374(9) 0.3522(2) 0.2057(2) 0.0426(13) Uani 1 d . . H23A H 1.5624(9) 0.3566(2) 0.1942(2) 0.051 Uiso 1 calc R . C24A C 1.2753(12) 0.3833(2) 0.1852(2) 0.056(2) Uani 1 d . . H24C H 1.2562(12) 0.3711(2) 0.1599(2) 0.067 Uiso 1 calc R . H24D H 1.3133(12) 0.4202(2) 0.1850(2) 0.067 Uiso 1 calc R . C25A C 1.0831(12) 0.3775(3) 0.2030(2) 0.060(2) Uani 1 d . . H25A H 0.9778(12) 0.3984(3) 0.1895(2) 0.072 Uiso 1 calc R . C26A C 1.1144(12) 0.3966(3) 0.2423(2) 0.059(2) Uani 1 d . . H26C H 1.1519(12) 0.4335(3) 0.2427(2) 0.071 Uiso 1 calc R . H26D H 0.9911(12) 0.3931(3) 0.2540(2) 0.071 Uiso 1 calc R . C27A C 1.2742(10) 0.3651(2) 0.26265(14) 0.0424(13) Uani 1 d . . H27A H 1.2938(10) 0.3775(2) 0.28819(14) 0.051 Uiso 1 calc R . C28A C 1.2148(9) 0.3083(2) 0.26214(13) 0.0375(12) Uani 1 d . . H28C H 1.0914(9) 0.3043(2) 0.27376(13) 0.045 Uiso 1 calc R . H28D H 1.3177(9) 0.2878(2) 0.27602(13) 0.045 Uiso 1 calc R . C29A C 1.4655(10) 0.3704(2) 0.2452(2) 0.0490(15) Uani 1 d . . H29C H 1.5686(10) 0.3494(2) 0.2587(2) 0.059 Uiso 1 calc R . H29D H 1.5083(10) 0.4069(2) 0.2460(2) 0.059 Uiso 1 calc R . C30A C 1.0258(9) 0.3211(3) 0.2021(2) 0.051(2) Uani 1 d . . H30C H 1.0069(9) 0.3091(3) 0.1767(2) 0.062 Uiso 1 calc R . H30D H 0.9003(9) 0.3167(3) 0.2129(2) 0.062 Uiso 1 calc R . C31A C 0.6194(7) 0.0557(2) 0.25201(13) 0.0300(10) Uani 1 d . . C32A C 0.5114(7) 0.0422(2) 0.27363(13) 0.0311(10) Uani 1 d . . C33A C 0.3764(7) 0.0264(2) 0.29993(12) 0.0250(9) Uani 1 d . . C34A C 0.4600(7) -0.0190(2) 0.32307(12) 0.0273(9) Uani 1 d . . H34C H 0.5869(7) -0.0088(2) 0.33601(12) 0.033 Uiso 1 calc R . H34D H 0.4835(7) -0.0487(2) 0.30732(12) 0.033 Uiso 1 calc R . C35A C 0.3164(7) -0.0347(2) 0.35048(12) 0.0283(10) Uani 1 d . . H35A H 0.3715(7) -0.0644(2) 0.36533(12) 0.034 Uiso 1 calc R . C36A C 0.1202(7) -0.0503(2) 0.33022(13) 0.0315(10) Uani 1 d . . H36C H 0.1397(7) -0.0802(2) 0.31438(13) 0.038 Uiso 1 calc R . H36D H 0.0270(7) -0.0606(2) 0.34773(13) 0.038 Uiso 1 calc R . C37A C 0.0359(7) -0.0050(2) 0.30754(13) 0.0301(10) Uani 1 d . . H37A H -0.0923(7) -0.0154(2) 0.29454(13) 0.036 Uiso 1 calc R . C38A C 0.0038(7) 0.0414(2) 0.33251(14) 0.0341(11) Uani 1 d . . H38C H -0.0522(7) 0.0708(2) 0.31801(14) 0.041 Uiso 1 calc R . H38D H -0.0896(7) 0.0318(2) 0.35016(14) 0.041 Uiso 1 calc R . C39A C 0.2009(7) 0.0571(2) 0.35246(13) 0.0330(11) Uani 1 d . . H39A H 0.1800(7) 0.0870(2) 0.36865(13) 0.040 Uiso 1 calc R . C40A C 0.3419(7) 0.0729(2) 0.32522(13) 0.0310(10) Uani 1 d . . H40C H 0.4681(7) 0.0840(2) 0.33800(13) 0.037 Uiso 1 calc R . H40D H 0.2868(7) 0.1024(2) 0.31069(13) 0.037 Uiso 1 calc R . C41A C 0.1755(7) 0.0109(2) 0.28035(12) 0.0279(10) Uani 1 d . . H41C H 0.1198(7) 0.0405(2) 0.26600(12) 0.033 Uiso 1 calc R . H41D H 0.1932(7) -0.0180(2) 0.26361(12) 0.033 Uiso 1 calc R . C42A C 0.2841(8) 0.0119(2) 0.37520(13) 0.0324(10) Uani 1 d . . H42C H 0.1920(8) 0.0023(2) 0.39307(13) 0.039 Uiso 1 calc R . H42D H 0.4101(8) 0.0221(2) 0.38847(13) 0.039 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.035(3) 0.025(2) -0.005(2) 0.003(2) -0.005(2) C2 0.035(3) 0.026(2) 0.031(2) 0.000(2) 0.003(2) -0.004(2) C3 0.041(3) 0.035(3) 0.027(2) 0.001(2) -0.002(2) -0.003(2) C4 0.039(3) 0.040(3) 0.035(3) 0.001(2) -0.005(2) -0.012(2) C5 0.042(3) 0.033(3) 0.034(3) 0.002(2) 0.002(2) -0.011(2) C6 0.036(3) 0.031(2) 0.029(2) -0.001(2) -0.002(2) -0.007(2) C7 0.031(2) 0.031(2) 0.028(2) 0.000(2) 0.005(2) -0.002(2) C8 0.032(2) 0.033(2) 0.028(2) -0.001(2) 0.005(2) -0.003(2) C9 0.027(2) 0.023(2) 0.029(2) 0.002(2) 0.002(2) -0.004(2) C10 0.033(2) 0.023(2) 0.034(2) 0.004(2) 0.008(2) -0.005(2) C11 0.030(2) 0.031(2) 0.030(2) 0.008(2) 0.004(2) 0.001(2) C12 0.034(2) 0.036(3) 0.025(2) 0.006(2) 0.005(2) -0.001(2) C13 0.031(2) 0.027(2) 0.028(2) 0.000(2) 0.003(2) -0.004(2) C14 0.032(3) 0.032(2) 0.029(2) 0.004(2) 0.002(2) -0.008(2) C15 0.026(2) 0.032(2) 0.030(2) 0.005(2) 0.006(2) -0.004(2) C16 0.035(3) 0.031(2) 0.025(2) 0.002(2) 0.005(2) -0.004(2) C17 0.029(2) 0.026(2) 0.032(2) 0.002(2) 0.003(2) 0.001(2) C18 0.026(2) 0.038(3) 0.035(2) 0.007(2) 0.006(2) 0.001(2) C19 0.047(3) 0.039(3) 0.040(3) 0.006(2) -0.006(2) -0.013(2) C20 0.045(3) 0.040(3) 0.037(3) 0.008(2) -0.008(2) -0.012(2) C21 0.033(2) 0.032(2) 0.027(2) 0.001(2) 0.003(2) -0.005(2) C22 0.045(3) 0.067(4) 0.041(3) 0.011(3) 0.018(3) 0.006(3) C23 0.076(5) 0.055(4) 0.045(3) -0.013(3) 0.016(3) 0.020(4) C24 0.096(6) 0.036(3) 0.035(3) -0.007(2) -0.004(3) -0.002(3) C25 0.045(3) 0.039(3) 0.043(3) 0.002(2) -0.007(2) -0.014(2) C26 0.062(4) 0.046(3) 0.044(3) 0.007(3) 0.003(3) -0.018(3) C27 0.064(4) 0.037(3) 0.025(2) 0.006(2) 0.004(2) -0.006(3) C28 0.041(3) 0.034(3) 0.026(2) 0.002(2) 0.001(2) -0.006(2) C29 0.041(3) 0.030(2) 0.037(3) 0.005(2) -0.002(2) -0.001(2) C30 0.075(5) 0.039(3) 0.053(4) 0.006(3) -0.002(3) 0.016(3) C31 0.042(3) 0.038(3) 0.034(3) 0.001(2) -0.001(2) -0.007(2) C32 0.041(3) 0.045(3) 0.034(3) 0.004(2) -0.003(2) 0.000(2) C33 0.035(3) 0.042(3) 0.031(2) 0.001(2) 0.000(2) 0.004(2) C34 0.056(4) 0.089(5) 0.043(3) -0.008(3) 0.001(3) 0.014(4) C35 0.046(4) 0.117(8) 0.060(4) -0.031(5) -0.003(3) 0.024(4) C36 0.190(12) 0.053(5) 0.062(5) -0.009(4) -0.013(6) 0.067(6) C37 0.061(5) 0.046(4) 0.123(7) -0.009(4) -0.026(5) 0.002(3) C38 0.069(5) 0.073(5) 0.047(4) 0.002(3) 0.010(3) -0.017(4) C39 0.049(4) 0.068(4) 0.041(3) -0.014(3) 0.015(3) -0.013(3) C40 0.054(4) 0.058(4) 0.044(3) 0.000(3) 0.008(3) 0.003(3) C41 0.074(5) 0.059(5) 0.115(7) 0.031(5) -0.044(5) -0.026(4) C42 0.052(4) 0.055(4) 0.063(4) 0.008(3) 0.009(3) 0.009(3) C1A 0.046(3) 0.034(3) 0.026(2) -0.002(2) 0.004(2) -0.003(2) C2A 0.045(3) 0.044(3) 0.031(2) -0.001(2) 0.013(2) -0.015(2) C3A 0.047(3) 0.035(3) 0.031(2) -0.004(2) 0.006(2) -0.013(2) C4A 0.038(3) 0.035(3) 0.029(2) -0.003(2) 0.005(2) -0.007(2) C5A 0.034(3) 0.031(2) 0.026(2) 0.003(2) 0.004(2) -0.007(2) C6A 0.036(3) 0.029(2) 0.028(2) 0.001(2) 0.002(2) -0.005(2) C7A 0.046(3) 0.039(3) 0.034(3) -0.001(2) 0.009(2) -0.007(2) C8A 0.041(3) 0.047(3) 0.032(3) -0.003(2) 0.010(2) -0.005(2) C9A 0.039(3) 0.045(3) 0.027(2) -0.004(2) 0.005(2) 0.002(2) C10A 0.050(4) 0.094(6) 0.053(4) 0.000(4) 0.005(3) 0.010(4) C11A 0.044(4) 0.154(10) 0.059(4) 0.045(6) 0.014(3) 0.032(5) C12A 0.210(13) 0.053(5) 0.055(5) 0.006(4) 0.018(6) 0.069(7) C13A 0.077(5) 0.043(4) 0.114(7) 0.009(4) 0.041(5) -0.001(4) C14A 0.068(5) 0.076(5) 0.049(4) -0.009(3) -0.001(3) -0.017(4) C15A 0.046(3) 0.069(4) 0.038(3) 0.012(3) -0.008(3) -0.009(3) C16A 0.056(4) 0.057(4) 0.041(3) -0.002(3) -0.001(3) 0.003(3) C17A 0.079(6) 0.055(4) 0.089(6) -0.016(4) 0.037(5) -0.019(4) C18A 0.054(4) 0.058(4) 0.062(4) -0.004(3) -0.003(3) 0.010(3) C19A 0.048(3) 0.043(3) 0.037(3) -0.005(2) 0.013(2) -0.015(3) C20A 0.050(3) 0.040(3) 0.037(3) -0.006(2) 0.016(2) -0.013(3) C21A 0.032(2) 0.035(3) 0.028(2) -0.002(2) 0.006(2) -0.007(2) C22A 0.041(3) 0.034(3) 0.033(3) -0.002(2) 0.010(2) -0.005(2) C23A 0.052(3) 0.040(3) 0.038(3) -0.001(2) 0.013(2) -0.015(3) C24A 0.094(5) 0.033(3) 0.040(3) 0.007(2) 0.010(3) 0.000(3) C25A 0.068(5) 0.063(4) 0.048(4) 0.008(3) -0.007(3) 0.020(4) C26A 0.073(5) 0.045(4) 0.061(4) -0.003(3) 0.012(4) 0.015(3) C27A 0.064(4) 0.036(3) 0.027(2) -0.006(2) 0.003(2) -0.006(3) C28A 0.046(3) 0.038(3) 0.029(2) -0.002(2) 0.005(2) -0.005(2) C29A 0.057(4) 0.042(3) 0.047(3) -0.005(3) 0.002(3) -0.017(3) C30A 0.043(3) 0.068(4) 0.041(3) -0.007(3) -0.010(3) 0.002(3) C31A 0.031(2) 0.029(2) 0.030(2) 0.003(2) 0.001(2) -0.001(2) C32A 0.033(2) 0.030(2) 0.030(2) 0.003(2) 0.000(2) -0.003(2) C33A 0.025(2) 0.024(2) 0.026(2) -0.001(2) 0.004(2) -0.005(2) C34A 0.028(2) 0.026(2) 0.028(2) -0.003(2) 0.002(2) 0.000(2) C35A 0.033(3) 0.026(2) 0.026(2) 0.003(2) 0.001(2) -0.002(2) C36A 0.033(3) 0.032(2) 0.030(2) -0.003(2) 0.007(2) -0.012(2) C37A 0.027(2) 0.033(2) 0.030(2) -0.004(2) 0.000(2) -0.004(2) C38A 0.028(2) 0.041(3) 0.034(2) -0.008(2) 0.001(2) 0.003(2) C39A 0.031(3) 0.037(3) 0.032(2) -0.011(2) 0.004(2) -0.003(2) C40A 0.035(3) 0.021(2) 0.036(2) -0.006(2) -0.002(2) -0.004(2) C41A 0.029(2) 0.028(2) 0.026(2) -0.004(2) 0.001(2) -0.002(2) C42A 0.033(2) 0.038(3) 0.026(2) -0.007(2) 0.000(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.376(7) . ? C1 C2 1.397(7) . ? C1 C7 1.440(7) . ? C2 C3 1.393(7) . ? C3 C4 1.392(7) . ? C3 C31 1.436(7) . ? C4 C5 1.379(7) . ? C5 C6 1.396(7) . ? C5 C19 1.449(7) . ? C7 C8 1.196(7) . ? C8 C9 1.465(7) . ? C9 C17 1.543(6) . ? C9 C16 1.546(6) . ? C9 C10 1.561(6) . ? C10 C11 1.518(7) . ? C11 C18 1.533(7) . ? C11 C12 1.530(7) . ? C12 C13 1.541(7) . ? C13 C14 1.533(7) . ? C13 C17 1.535(7) . ? C14 C15 1.530(7) . ? C15 C16 1.523(7) . ? C15 C18 1.544(7) . ? C19 C20 1.191(8) . ? C20 C21 1.467(7) . ? C21 C22 1.533(8) . ? C21 C28 1.539(6) . ? C21 C29 1.537(7) . ? C22 C23 1.538(10) . ? C23 C24 1.526(11) . ? C23 C30 1.531(9) . ? C24 C25 1.518(10) . ? C25 C29 1.521(7) . ? C25 C26 1.548(8) . ? C26 C27 1.513(9) . ? C27 C30 1.516(9) . ? C27 C28 1.535(7) . ? C31 C32 1.194(8) . ? C32 C33 1.466(7) . ? C33 C41 1.499(9) . ? C33 C34 1.544(9) . ? C33 C40 1.566(8) . ? C34 C35 1.536(11) . ? C35 C42 1.432(10) . ? C35 C36 1.565(15) . ? C36 C37 1.540(15) . ? C37 C38 1.490(11) . ? C37 C41 1.599(11) . ? C38 C39 1.475(10) . ? C39 C42 1.520(9) . ? C39 C40 1.584(10) . ? C1A C2A 1.387(7) . ? C1A C6A 1.395(7) . ? C1A C7A 1.442(7) . ? C2A C3A 1.389(8) . ? C3A C4A 1.406(7) . ? C3A C19A 1.431(7) . ? C4A C5A 1.388(7) . ? C5A C6A 1.396(7) . ? C5A C31A 1.438(7) . ? C7A C8A 1.195(8) . ? C8A C9A 1.462(7) . ? C9A C17A 1.527(9) . ? C9A C10A 1.533(9) . ? C9A C16A 1.550(8) . ? C10A C11A 1.574(12) . ? C11A C18A 1.469(10) . ? C11A C12A 1.505(15) . ? C12A C13A 1.517(15) . ? C13A C14A 1.483(11) . ? C13A C17A 1.563(11) . ? C14A C15A 1.477(10) . ? C15A C18A 1.514(9) . ? C15A C16A 1.576(10) . ? C19A C20A 1.201(8) . ? C20A C21A 1.456(7) . ? C21A C30A 1.541(8) . ? C21A C28A 1.543(7) . ? C21A C22A 1.545(7) . ? C22A C23A 1.527(7) . ? C23A C24A 1.520(9) . ? C23A C29A 1.536(8) . ? C24A C25A 1.535(11) . ? C25A C30A 1.513(10) . ? C25A C26A 1.537(10) . ? C26A C27A 1.512(9) . ? C27A C28A 1.526(8) . ? C27A C29A 1.522(9) . ? C31A C32A 1.194(7) . ? C32A C33A 1.466(7) . ? C33A C34A 1.535(6) . ? C33A C41A 1.550(6) . ? C33A C40A 1.561(6) . ? C34A C35A 1.536(7) . ? C35A C36A 1.534(7) . ? C35A C42A 1.547(7) . ? C36A C37A 1.527(7) . ? C37A C41A 1.512(7) . ? C37A C38A 1.547(7) . ? C38A C39A 1.535(7) . ? C39A C42A 1.523(7) . ? C39A C40A 1.520(7) . ? 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 C6 C1 C2 119.5(4) . . ? C6 C1 C7 119.1(5) . . ? C2 C1 C7 121.3(4) . . ? C3 C2 C1 120.6(4) . . ? C2 C3 C4 118.9(5) . . ? C2 C3 C31 121.6(5) . . ? C4 C3 C31 119.6(5) . . ? C5 C4 C3 120.9(5) . . ? C4 C5 C6 119.5(5) . . ? C4 C5 C19 120.0(5) . . ? C6 C5 C19 120.4(5) . . ? C1 C6 C5 120.5(5) . . ? C8 C7 C1 174.4(5) . . ? C7 C8 C9 178.4(5) . . ? C8 C9 C17 111.0(4) . . ? C8 C9 C16 109.8(4) . . ? C17 C9 C16 109.2(4) . . ? C8 C9 C10 109.8(4) . . ? C17 C9 C10 108.8(4) . . ? C16 C9 C10 108.2(4) . . ? C11 C10 C9 109.7(4) . . ? C10 C11 C18 109.6(4) . . ? C10 C11 C12 110.0(4) . . ? C18 C11 C12 109.4(4) . . ? C11 C12 C13 109.7(4) . . ? C14 C13 C12 109.6(4) . . ? C14 C13 C17 109.2(4) . . ? C12 C13 C17 108.9(4) . . ? C15 C14 C13 109.8(4) . . ? C16 C15 C14 110.2(4) . . ? C16 C15 C18 109.2(4) . . ? C14 C15 C18 109.1(4) . . ? C15 C16 C9 110.0(4) . . ? C13 C17 C9 110.2(4) . . ? C11 C18 C15 109.6(4) . . ? C20 C19 C5 175.5(7) . . ? C19 C20 C21 176.3(6) . . ? C20 C21 C22 108.9(5) . . ? C20 C21 C28 111.0(4) . . ? C22 C21 C28 108.2(4) . . ? C20 C21 C29 110.7(4) . . ? C22 C21 C29 109.5(4) . . ? C28 C21 C29 108.4(4) . . ? C21 C22 C23 110.4(5) . . ? C24 C23 C30 110.1(6) . . ? C24 C23 C22 107.9(5) . . ? C30 C23 C22 109.2(5) . . ? C25 C24 C23 110.5(5) . . ? C24 C25 C29 109.8(5) . . ? C24 C25 C26 109.7(5) . . ? C29 C25 C26 108.2(5) . . ? C27 C26 C25 109.7(5) . . ? C26 C27 C30 110.9(5) . . ? C26 C27 C28 108.8(5) . . ? C30 C27 C28 109.0(5) . . ? C21 C28 C27 110.3(4) . . ? C25 C29 C21 110.0(4) . . ? C27 C30 C23 109.7(5) . . ? C32 C31 C3 174.2(6) . . ? C31 C32 C33 176.4(6) . . ? C32 C33 C41 110.7(5) . . ? C32 C33 C34 107.3(5) . . ? C41 C33 C34 110.4(6) . . ? C32 C33 C40 111.0(5) . . ? C41 C33 C40 110.7(6) . . ? C34 C33 C40 106.6(5) . . ? C35 C34 C33 108.7(6) . . ? C42 C35 C34 108.2(7) . . ? C42 C35 C36 110.0(7) . . ? C34 C35 C36 109.5(7) . . ? C37 C36 C35 111.0(6) . . ? C38 C37 C36 111.9(7) . . ? C38 C37 C41 107.9(7) . . ? C36 C37 C41 102.3(8) . . ? C37 C38 C39 113.8(6) . . ? C38 C39 C42 113.9(6) . . ? C38 C39 C40 104.6(6) . . ? C42 C39 C40 105.4(5) . . ? C33 C40 C39 109.3(5) . . ? C33 C41 C37 110.9(6) . . ? C35 C42 C39 113.8(6) . . ? C2A C1A C6A 119.2(5) . . ? C2A C1A C7A 119.3(5) . . ? C6A C1A C7A 121.5(5) . . ? C3A C2A C1A 121.6(5) . . ? C2A C3A C4A 118.6(5) . . ? C2A C3A C19A 121.1(5) . . ? C4A C3A C19A 120.2(5) . . ? C5A C4A C3A 120.5(5) . . ? C4A C5A C6A 119.8(4) . . ? C4A C5A C31A 118.7(5) . . ? C6A C5A C31A 121.5(4) . . ? C5A C6A C1A 120.3(4) . . ? C8A C7A C1A 174.5(6) . . ? C7A C8A C9A 176.3(6) . . ? C8A C9A C17A 110.8(5) . . ? C8A C9A C10A 107.1(5) . . ? C17A C9A C10A 111.1(6) . . ? C8A C9A C16A 111.5(5) . . ? C17A C9A C16A 110.0(5) . . ? C10A C9A C16A 106.3(5) . . ? C9A C10A C11A 108.5(6) . . ? C18A C11A C12A 111.6(8) . . ? C18A C11A C10A 103.7(8) . . ? C12A C11A C10A 111.3(7) . . ? C11A C12A C13A 111.2(6) . . ? C14A C13A C12A 112.3(7) . . ? C14A C13A C17A 109.0(7) . . ? C12A C13A C17A 104.6(8) . . ? C15A C14A C13A 112.8(6) . . ? C14A C15A C18A 113.1(6) . . ? C14A C15A C16A 105.1(6) . . ? C18A C15A C16A 105.7(5) . . ? C9A C16A C15A 109.7(5) . . ? C9A C17A C13A 109.7(6) . . ? C11A C18A C15A 113.1(6) . . ? C20A C19A C3A 175.8(7) . . ? C19A C20A C21A 176.8(7) . . ? C20A C21A C30A 109.3(5) . . ? C20A C21A C28A 111.6(4) . . ? C30A C21A C28A 108.3(4) . . ? C20A C21A C22A 110.4(4) . . ? C30A C21A C22A 108.9(4) . . ? C28A C21A C22A 108.4(4) . . ? C23A C22A C21A 110.0(4) . . ? C24A C23A C22A 109.6(5) . . ? C24A C23A C29A 109.8(5) . . ? C22A C23A C29A 108.1(5) . . ? C23A C24A C25A 110.3(5) . . ? C30A C25A C24A 108.4(6) . . ? C30A C25A C26A 110.2(6) . . ? C24A C25A C26A 109.1(6) . . ? C27A C26A C25A 109.6(5) . . ? C26A C27A C28A 109.4(5) . . ? C26A C27A C29A 110.4(5) . . ? C28A C27A C29A 108.7(5) . . ? C27A C28A C21A 110.4(4) . . ? C27A C29A C23A 110.1(5) . . ? C25A C30A C21A 110.6(5) . . ? C32A C31A C5A 174.4(5) . . ? C31A C32A C33A 179.0(5) . . ? C32A C33A C34A 111.3(4) . . ? C32A C33A C41A 110.3(4) . . ? C34A C33A C41A 109.7(4) . . ? C32A C33A C40A 109.0(4) . . ? C34A C33A C40A 108.8(4) . . ? C41A C33A C40A 107.8(4) . . ? C33A C34A C35A 110.3(4) . . ? C36A C35A C34A 109.3(4) . . ? C36A C35A C42A 109.3(4) . . ? C34A C35A C42A 108.8(4) . . ? C37A C36A C35A 109.9(4) . . ? C41A C37A C36A 110.4(4) . . ? C41A C37A C38A 108.9(4) . . ? C36A C37A C38A 109.4(4) . . ? C39A C38A C37A 109.1(4) . . ? C42A C39A C40A 110.5(4) . . ? C42A C39A C38A 109.5(4) . . ? C40A C39A C38A 109.5(4) . . ? C39A C40A C33A 109.5(4) . . ? C37A C41A C33A 110.2(4) . . ? C39A C42A C35A 109.7(4) . . ? 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 C6 C1 C2 C3 -2.4(8) . . . . ? C7 C1 C2 C3 174.8(5) . . . . ? C1 C2 C3 C4 1.8(8) . . . . ? C1 C2 C3 C31 -178.5(5) . . . . ? C2 C3 C4 C5 0.4(8) . . . . ? C31 C3 C4 C5 -179.3(5) . . . . ? C3 C4 C5 C6 -2.0(8) . . . . ? C3 C4 C5 C19 175.8(5) . . . . ? C2 C1 C6 C5 0.8(8) . . . . ? C7 C1 C6 C5 -176.5(5) . . . . ? C4 C5 C6 C1 1.4(8) . . . . ? C19 C5 C6 C1 -176.4(5) . . . . ? C6 C1 C7 C8 53.7(58) . . . . ? C2 C1 C7 C8 -123.6(55) . . . . ? C1 C7 C8 C9 -90.7(195) . . . . ? C7 C8 C9 C17 151.8(186) . . . . ? C7 C8 C9 C16 -87.4(187) . . . . ? C7 C8 C9 C10 31.5(188) . . . . ? C8 C9 C10 C11 -179.5(4) . . . . ? C17 C9 C10 C11 58.8(5) . . . . ? C16 C9 C10 C11 -59.7(5) . . . . ? C9 C10 C11 C18 60.4(5) . . . . ? C9 C10 C11 C12 -59.9(5) . . . . ? C10 C11 C12 C13 60.7(5) . . . . ? C18 C11 C12 C13 -59.7(5) . . . . ? C11 C12 C13 C14 59.3(5) . . . . ? C11 C12 C13 C17 -60.1(5) . . . . ? C12 C13 C14 C15 -59.5(5) . . . . ? C17 C13 C14 C15 59.7(5) . . . . ? C13 C14 C15 C16 -59.9(5) . . . . ? C13 C14 C15 C18 59.9(5) . . . . ? C14 C15 C16 C9 59.2(5) . . . . ? C18 C15 C16 C9 -60.6(5) . . . . ? C8 C9 C16 C15 179.8(4) . . . . ? C17 C9 C16 C15 -58.3(5) . . . . ? C10 C9 C16 C15 60.0(5) . . . . ? C14 C13 C17 C9 -59.6(5) . . . . ? C12 C13 C17 C9 60.1(5) . . . . ? C8 C9 C17 C13 179.9(4) . . . . ? C16 C9 C17 C13 58.8(5) . . . . ? C10 C9 C17 C13 -59.2(5) . . . . ? C10 C11 C18 C15 -60.4(5) . . . . ? C12 C11 C18 C15 60.3(5) . . . . ? C16 C15 C18 C11 60.2(5) . . . . ? C14 C15 C18 C11 -60.3(5) . . . . ? C4 C5 C19 C20 -108.1(77) . . . . ? C6 C5 C19 C20 69.7(79) . . . . ? C5 C19 C20 C21 51.6(148) . . . . ? C19 C20 C21 C22 -44.1(100) . . . . ? C19 C20 C21 C28 -163.1(97) . . . . ? C19 C20 C21 C29 76.4(99) . . . . ? C20 C21 C22 C23 -179.8(5) . . . . ? C28 C21 C22 C23 -59.0(6) . . . . ? C29 C21 C22 C23 59.0(6) . . . . ? C21 C22 C23 C24 -60.0(6) . . . . ? C21 C22 C23 C30 59.7(7) . . . . ? C30 C23 C24 C25 -58.4(7) . . . . ? C22 C23 C24 C25 60.7(7) . . . . ? C23 C24 C25 C29 -60.8(6) . . . . ? C23 C24 C25 C26 58.0(7) . . . . ? C24 C25 C26 C27 -58.1(6) . . . . ? C29 C25 C26 C27 61.7(7) . . . . ? C25 C26 C27 C30 59.0(7) . . . . ? C25 C26 C27 C28 -60.9(6) . . . . ? C20 C21 C28 C27 179.1(5) . . . . ? C22 C21 C28 C27 59.6(6) . . . . ? C29 C21 C28 C27 -59.1(6) . . . . ? C26 C27 C28 C21 60.1(6) . . . . ? C30 C27 C28 C21 -60.9(6) . . . . ? C24 C25 C29 C21 58.5(6) . . . . ? C26 C25 C29 C21 -61.2(6) . . . . ? C20 C21 C29 C25 -177.8(5) . . . . ? C22 C21 C29 C25 -57.7(6) . . . . ? C28 C21 C29 C25 60.2(6) . . . . ? C26 C27 C30 C23 -59.1(7) . . . . ? C28 C27 C30 C23 60.7(7) . . . . ? C24 C23 C30 C27 58.1(7) . . . . ? C22 C23 C30 C27 -60.2(8) . . . . ? C2 C3 C31 C32 168.3(58) . . . . ? C4 C3 C31 C32 -12.0(63) . . . . ? C3 C31 C32 C33 -31.3(141) . . . . ? C31 C32 C33 C41 -141.0(94) . . . . ? C31 C32 C33 C34 -20.5(97) . . . . ? C31 C32 C33 C40 95.6(95) . . . . ? C32 C33 C34 C35 -179.0(6) . . . . ? C41 C33 C34 C35 -58.3(8) . . . . ? C40 C33 C34 C35 62.1(7) . . . . ? C33 C34 C35 C42 -63.4(9) . . . . ? C33 C34 C35 C36 56.6(8) . . . . ? C42 C35 C36 C37 55.5(9) . . . . ? C34 C35 C36 C37 -63.3(8) . . . . ? C35 C36 C37 C38 -52.1(10) . . . . ? C35 C36 C37 C41 63.1(8) . . . . ? C36 C37 C38 C39 48.9(10) . . . . ? C41 C37 C38 C39 -62.8(10) . . . . ? C37 C38 C39 C42 -47.8(9) . . . . ? C37 C38 C39 C40 66.7(8) . . . . ? C32 C33 C40 C39 -177.7(5) . . . . ? C41 C33 C40 C39 58.8(7) . . . . ? C34 C33 C40 C39 -61.3(7) . . . . ? C38 C39 C40 C33 -61.8(6) . . . . ? C42 C39 C40 C33 58.6(7) . . . . ? C32 C33 C41 C37 -177.5(7) . . . . ? C34 C33 C41 C37 63.9(9) . . . . ? C40 C33 C41 C37 -54.0(10) . . . . ? C38 C37 C41 C33 53.9(11) . . . . ? C36 C37 C41 C33 -64.2(10) . . . . ? C34 C35 C42 C39 64.7(9) . . . . ? C36 C35 C42 C39 -54.8(9) . . . . ? C38 C39 C42 C35 52.2(9) . . . . ? C40 C39 C42 C35 -61.9(8) . . . . ? C6A C1A C2A C3A -0.2(8) . . . . ? C7A C1A C2A C3A 179.5(5) . . . . ? C1A C2A C3A C4A 1.4(9) . . . . ? C1A C2A C3A C19A -175.7(5) . . . . ? C2A C3A C4A C5A -0.4(8) . . . . ? C19A C3A C4A C5A 176.7(5) . . . . ? C3A C4A C5A C6A -1.8(8) . . . . ? C3A C4A C5A C31A 176.1(5) . . . . ? C4A C5A C6A C1A 3.0(8) . . . . ? C31A C5A C6A C1A -174.8(5) . . . . ? C2A C1A C6A C5A -2.0(8) . . . . ? C7A C1A C6A C5A 178.3(5) . . . . ? C2A C1A C7A C8A 19.8(66) . . . . ? C6A C1A C7A C8A -160.6(61) . . . . ? C1A C7A C8A C9A 4.2(151) . . . . ? C7A C8A C9A C17A 160.9(96) . . . . ? C7A C8A C9A C10A 39.6(99) . . . . ? C7A C8A C9A C16A -76.3(98) . . . . ? C8A C9A C10A C11A 175.5(6) . . . . ? C17A C9A C10A C11A 54.4(8) . . . . ? C16A C9A C10A C11A -65.3(8) . . . . ? C9A C10A C11A C18A 66.7(9) . . . . ? C9A C10A C11A C12A -53.4(8) . . . . ? C18A C11A C12A C13A -54.2(10) . . . . ? C10A C11A C12A C13A 61.1(9) . . . . ? C11A C12A C13A C14A 53.8(10) . . . . ? C11A C12A C13A C17A -64.3(9) . . . . ? C12A C13A C14A C15A -51.8(10) . . . . ? C17A C13A C14A C15A 63.7(10) . . . . ? C13A C14A C15A C18A 49.5(9) . . . . ? C13A C14A C15A C16A -65.3(8) . . . . ? C8A C9A C16A C15A 177.7(5) . . . . ? C17A C9A C16A C15A -59.0(7) . . . . ? C10A C9A C16A C15A 61.3(7) . . . . ? C14A C15A C16A C9A 61.5(6) . . . . ? C18A C15A C16A C9A -58.4(7) . . . . ? C8A C9A C17A C13A 178.9(6) . . . . ? C10A C9A C17A C13A -62.2(9) . . . . ? C16A C9A C17A C13A 55.1(9) . . . . ? C14A C13A C17A C9A -56.0(10) . . . . ? C12A C13A C17A C9A 64.3(9) . . . . ? C12A C11A C18A C15A 52.6(10) . . . . ? C10A C11A C18A C15A -67.3(9) . . . . ? C14A C15A C18A C11A -50.4(9) . . . . ? C16A C15A C18A C11A 64.0(8) . . . . ? C2A C3A C19A C20A 93.6(80) . . . . ? C4A C3A C19A C20A -83.4(79) . . . . ? C3A C19A C20A C21A -19.1(173) . . . . ? C19A C20A C21A C30A 25.2(109) . . . . ? C19A C20A C21A C28A 144.9(106) . . . . ? C19A C20A C21A C22A -94.6(108) . . . . ? C20A C21A C22A C23A 177.8(5) . . . . ? C30A C21A C22A C23A 57.9(6) . . . . ? C28A C21A C22A C23A -59.7(6) . . . . ? C21A C22A C23A C24A -58.7(6) . . . . ? C21A C22A C23A C29A 60.9(6) . . . . ? C22A C23A C24A C25A 60.1(6) . . . . ? C29A C23A C24A C25A -58.4(7) . . . . ? C23A C24A C25A C30A -60.8(7) . . . . ? C23A C24A C25A C26A 59.3(7) . . . . ? C30A C25A C26A C27A 59.4(8) . . . . ? C24A C25A C26A C27A -59.6(7) . . . . ? C25A C26A C27A C28A -59.8(7) . . . . ? C25A C26A C27A C29A 59.8(7) . . . . ? C26A C27A C28A C21A 60.7(6) . . . . ? C29A C27A C28A C21A -60.0(6) . . . . ? C20A C21A C28A C27A -179.2(5) . . . . ? C30A C21A C28A C27A -58.9(6) . . . . ? C22A C21A C28A C27A 59.1(6) . . . . ? C26A C27A C29A C23A -58.9(7) . . . . ? C28A C27A C29A C23A 61.2(6) . . . . ? C24A C23A C29A C27A 57.8(6) . . . . ? C22A C23A C29A C27A -61.7(7) . . . . ? C24A C25A C30A C21A 60.5(7) . . . . ? C26A C25A C30A C21A -58.8(8) . . . . ? C20A C21A C30A C25A 179.8(5) . . . . ? C28A C21A C30A C25A 58.1(6) . . . . ? C22A C21A C30A C25A -59.6(6) . . . . ? C4A C5A C31A C32A -52.5(57) . . . . ? C6A C5A C31A C32A 125.3(54) . . . . ? C5A C31A C32A C33A 121.7(307) . . . . ? C31A C32A C33A C34A 176.3(1000) . . . . ? C31A C32A C33A C41A 54.3(326) . . . . ? C31A C32A C33A C40A -63.8(326) . . . . ? C32A C33A C34A C35A 179.8(4) . . . . ? C41A C33A C34A C35A -58.0(5) . . . . ? C40A C33A C34A C35A 59.7(5) . . . . ? C33A C34A C35A C36A 59.1(5) . . . . ? C33A C34A C35A C42A -60.1(5) . . . . ? C34A C35A C36A C37A -59.5(5) . . . . ? C42A C35A C36A C37A 59.5(5) . . . . ? C35A C36A C37A C41A 59.9(5) . . . . ? C35A C36A C37A C38A -59.9(5) . . . . ? C41A C37A C38A C39A -60.7(5) . . . . ? C36A C37A C38A C39A 60.1(5) . . . . ? C37A C38A C39A C42A -60.5(5) . . . . ? C37A C38A C39A C40A 60.7(5) . . . . ? C42A C39A C40A C33A 59.7(5) . . . . ? C38A C39A C40A C33A -60.9(5) . . . . ? C32A C33A C40A C39A 179.6(4) . . . . ? C34A C33A C40A C39A -58.9(5) . . . . ? C41A C33A C40A C39A 59.9(5) . . . . ? C36A C37A C41A C33A -58.7(5) . . . . ? C38A C37A C41A C33A 61.4(5) . . . . ? C32A C33A C41A C37A -179.5(4) . . . . ? C34A C33A C41A C37A 57.6(5) . . . . ? C40A C33A C41A C37A -60.7(5) . . . . ? C40A C39A C42A C35A -60.2(5) . . . . ? C38A C39A C42A C35A 60.4(5) . . . . ? C36A C35A C42A C39A -59.7(5) . . . . ? C34A C35A C42A C39A 59.6(5) . . . . ? _refine_diff_density_max 0.704 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.055 # Attachment 'tomu5x1.cif' data_tomu5x1 _database_code_depnum_ccdc_archive 'CCDC 288447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H76 O2' _chemical_formula_weight 877.31 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.7567(7) _cell_length_b 12.5555(4) _cell_length_c 19.2403(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.834(2) _cell_angle_gamma 90.00 _cell_volume 4944.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.9642 _exptl_absorpt_correction_T_max 0.9749 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 86450 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 29.00 _reflns_number_total 13155 _reflns_number_gt 8801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _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^)+(0.0498P)^2^+8.6195P] 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 13155 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.005 _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 C1 C 0.40857(8) 0.84581(14) 0.24842(9) 0.0145(3) Uani 1 1 d . . . C2 C 0.42901(9) 0.84534(14) 0.17879(10) 0.0171(3) Uani 1 1 d . . . H2A H 0.4149 0.7779 0.1513 0.021 Uiso 1 1 calc R . . H2B H 0.4074 0.9050 0.1459 0.021 Uiso 1 1 calc R . . C3 C 0.50320(9) 0.85657(14) 0.20117(10) 0.0182(4) Uani 1 1 d . . . H3 H 0.5160 0.8566 0.1559 0.022 Uiso 1 1 calc R . . C4 C 0.52452(9) 0.96164(15) 0.24313(11) 0.0196(4) Uani 1 1 d . . . H4A H 0.5724 0.9704 0.2568 0.024 Uiso 1 1 calc R . . H4B H 0.5030 1.0221 0.2111 0.024 Uiso 1 1 calc R . . C5 C 0.50573(9) 0.96136(14) 0.31310(10) 0.0182(4) Uani 1 1 d . . . H5 H 0.5203 1.0296 0.3406 0.022 Uiso 1 1 calc R . . C6 C 0.43124(8) 0.95104(14) 0.29123(10) 0.0164(3) Uani 1 1 d . . . H6A H 0.4097 1.0122 0.2599 0.020 Uiso 1 1 calc R . . H6B H 0.4187 0.9516 0.3361 0.020 Uiso 1 1 calc R . . C7 C 0.44249(8) 0.75180(14) 0.29875(10) 0.0178(4) Uani 1 1 d . . . H7A H 0.4301 0.7514 0.3437 0.021 Uiso 1 1 calc R . . H7B H 0.4281 0.6837 0.2723 0.021 Uiso 1 1 calc R . . C8 C 0.51689(9) 0.76278(14) 0.32045(10) 0.0193(4) Uani 1 1 d . . . H8 H 0.5386 0.7017 0.3528 0.023 Uiso 1 1 calc R . . C9 C 0.53602(9) 0.76277(15) 0.25074(11) 0.0207(4) Uani 1 1 d . . . H9A H 0.5841 0.7687 0.2647 0.025 Uiso 1 1 calc R . . H9B H 0.5222 0.6951 0.2236 0.025 Uiso 1 1 calc R . . C10 C 0.53885(9) 0.86759(15) 0.36248(10) 0.0210(4) Uani 1 1 d . . . H10A H 0.5869 0.8747 0.3772 0.025 Uiso 1 1 calc R . . H10B H 0.5270 0.8677 0.4078 0.025 Uiso 1 1 calc R . . C11 C 0.33745(9) 0.83502(14) 0.22535(10) 0.0174(3) Uani 1 1 d . . . C12 C 0.27877(9) 0.82634(15) 0.20270(10) 0.0180(4) Uani 1 1 d . . . C13 C 0.21233(9) 0.81923(15) 0.17299(10) 0.0180(4) Uani 1 1 d . . . C14 C 0.15355(9) 0.81346(15) 0.14307(10) 0.0185(4) Uani 1 1 d . . . C15 C 0.08779(9) 0.80993(15) 0.10878(10) 0.0183(4) Uani 1 1 d . . . C16 C 0.02897(9) 0.81011(15) 0.07962(10) 0.0185(4) Uani 1 1 d . . . C17 C -0.03788(9) 0.81433(15) 0.05016(10) 0.0188(4) Uani 1 1 d . . . C18 C -0.09643(9) 0.82356(15) 0.02662(10) 0.0181(4) Uani 1 1 d . . . C19 C -0.16725(8) 0.84260(14) -0.00036(10) 0.0164(3) Uani 1 1 d . . . C20 C -0.18050(9) 0.95821(14) -0.02935(10) 0.0182(4) Uani 1 1 d . . . H20A H -0.1579 1.0087 0.0107 0.022 Uiso 1 1 calc R . . H20B H -0.1633 0.9687 -0.0703 0.022 Uiso 1 1 calc R . . C21 C -0.25425(9) 0.97984(15) -0.05666(10) 0.0199(4) Uani 1 1 d . . . H21 H -0.2626 1.0547 -0.0752 0.024 Uiso 1 1 calc R . . C22 C -0.28040(9) 0.96461(15) 0.00719(11) 0.0204(4) Uani 1 1 d . . . H22A H -0.3278 0.9800 -0.0099 0.024 Uiso 1 1 calc R . . H22B H -0.2582 1.0147 0.0477 0.024 Uiso 1 1 calc R . . C23 C -0.26818(9) 0.84996(15) 0.03558(11) 0.0223(4) Uani 1 1 d . . . H23 H -0.2857 0.8402 0.0770 0.027 Uiso 1 1 calc R . . C24 C -0.19468(9) 0.82749(15) 0.06344(10) 0.0199(4) Uani 1 1 d . . . H24A H -0.1865 0.7537 0.0824 0.024 Uiso 1 1 calc R . . H24B H -0.1723 0.8767 0.1044 0.024 Uiso 1 1 calc R . . C25 C -0.20255(9) 0.76481(16) -0.06358(11) 0.0234(4) Uani 1 1 d . . . H25A H -0.1853 0.7735 -0.1047 0.028 Uiso 1 1 calc R . . H25B H -0.1944 0.6905 -0.0456 0.028 Uiso 1 1 calc R . . C26 C -0.27637(10) 0.78768(17) -0.09111(12) 0.0279(4) Uani 1 1 d . . . H26 H -0.2992 0.7374 -0.1321 0.033 Uiso 1 1 calc R . . C27 C -0.30287(9) 0.77316(16) -0.02728(12) 0.0281(5) Uani 1 1 d . . . H27A H -0.3505 0.7872 -0.0450 0.034 Uiso 1 1 calc R . . H27B H -0.2956 0.6989 -0.0091 0.034 Uiso 1 1 calc R . . C28 C -0.28844(10) 0.90279(17) -0.11939(11) 0.0271(4) Uani 1 1 d . . . H28A H -0.2714 0.9128 -0.1606 0.033 Uiso 1 1 calc R . . H28B H -0.3359 0.9176 -0.1382 0.033 Uiso 1 1 calc R . . C1A C 0.33832(8) 0.64780(14) -0.01667(9) 0.0150(3) Uani 1 1 d . . . C2A C 0.31854(9) 0.57259(16) 0.03549(10) 0.0214(4) Uani 1 1 d . . . H2A1 H 0.3406 0.5030 0.0382 0.026 Uiso 1 1 calc R . . H2A2 H 0.3324 0.6034 0.0858 0.026 Uiso 1 1 calc R . . C3A C 0.24433(9) 0.55664(17) 0.00690(10) 0.0230(4) Uani 1 1 d . . . H3A H 0.2317 0.5079 0.0409 0.028 Uiso 1 1 calc R . . C4A C 0.22296(9) 0.50827(15) -0.07075(10) 0.0213(4) Uani 1 1 d . . . H4A1 H 0.2443 0.4382 -0.0691 0.026 Uiso 1 1 calc R . . H4A2 H 0.1751 0.4973 -0.0891 0.026 Uiso 1 1 calc R . . C5A C 0.24192(9) 0.58272(15) -0.12292(10) 0.0195(4) Uani 1 1 d . . . H5A H 0.2279 0.5507 -0.1735 0.023 Uiso 1 1 calc R . . C6A C 0.31616(9) 0.59858(15) -0.09476(10) 0.0183(4) Uani 1 1 d . . . H6A1 H 0.3286 0.6462 -0.1288 0.022 Uiso 1 1 calc R . . H6A2 H 0.3382 0.5292 -0.0933 0.022 Uiso 1 1 calc R . . C7A C 0.30383(8) 0.75625(15) -0.02053(11) 0.0211(4) Uani 1 1 d . . . H7A1 H 0.3176 0.7892 0.0291 0.025 Uiso 1 1 calc R . . H7A2 H 0.3162 0.8048 -0.0542 0.025 Uiso 1 1 calc R . . C8A C 0.22966(9) 0.73940(16) -0.04887(12) 0.0260(4) Uani 1 1 d . . . H8A H 0.2074 0.8096 -0.0511 0.031 Uiso 1 1 calc R . . C9A C 0.21087(10) 0.66524(18) 0.00381(12) 0.0295(5) Uani 1 1 d . . . H9A1 H 0.1629 0.6557 -0.0136 0.035 Uiso 1 1 calc R . . H9A2 H 0.2246 0.6971 0.0538 0.035 Uiso 1 1 calc R . . C10A C 0.20835(9) 0.69057(16) -0.12626(11) 0.0253(4) Uani 1 1 d . . . H10C H 0.1603 0.6811 -0.1451 0.030 Uiso 1 1 calc R . . H10D H 0.2204 0.7387 -0.1603 0.030 Uiso 1 1 calc R . . C11A C 0.40951(9) 0.66097(14) 0.01133(10) 0.0172(3) Uani 1 1 d . . . C12A C 0.46813(9) 0.66750(15) 0.03751(10) 0.0180(4) Uani 1 1 d . . . C13A C 0.53419(8) 0.67331(15) 0.07198(10) 0.0177(4) Uani 1 1 d . . . C14A C 0.59219(8) 0.67799(15) 0.10653(10) 0.0175(4) Uani 1 1 d . . . C15A C 0.65701(8) 0.68028(15) 0.14688(10) 0.0179(4) Uani 1 1 d . . . C16A C 0.71499(9) 0.67918(15) 0.18180(10) 0.0182(4) Uani 1 1 d . . . C17A C 0.78107(9) 0.67569(15) 0.21703(10) 0.0188(4) Uani 1 1 d . . . C18A C 0.83963(9) 0.66994(15) 0.24442(10) 0.0181(4) Uani 1 1 d . . . C19A C 0.91072(8) 0.65965(14) 0.27451(10) 0.0156(3) Uani 1 1 d . . . C20A C 0.93152(8) 0.60216(15) 0.35013(10) 0.0176(4) Uani 1 1 d . . . H20C H 0.9165 0.6435 0.3852 0.021 Uiso 1 1 calc R . . H20D H 0.9110 0.5308 0.3442 0.021 Uiso 1 1 calc R . . C21A C 1.00605(9) 0.59073(15) 0.38082(10) 0.0184(4) Uani 1 1 d . . . H21A H 1.0192 0.5536 0.4297 0.022 Uiso 1 1 calc R . . C22A C 1.03727(9) 0.70163(16) 0.39062(10) 0.0206(4) Uani 1 1 d . . . H22C H 1.0854 0.6950 0.4114 0.025 Uiso 1 1 calc R . . H22D H 1.0226 0.7438 0.4255 0.025 Uiso 1 1 calc R . . C23A C 1.01759(9) 0.75837(16) 0.31568(10) 0.0203(4) Uani 1 1 d . . . H23A H 1.0385 0.8303 0.3222 0.024 Uiso 1 1 calc R . . C24A C 0.94310(8) 0.77089(15) 0.28480(10) 0.0186(4) Uani 1 1 d . . . H24C H 0.9302 0.8085 0.2368 0.022 Uiso 1 1 calc R . . H24D H 0.9282 0.8137 0.3193 0.022 Uiso 1 1 calc R . . C25A C 0.93451(8) 0.59357(15) 0.22066(10) 0.0185(4) Uani 1 1 d . . . H25C H 0.9140 0.5222 0.2138 0.022 Uiso 1 1 calc R . . H25D H 0.9215 0.6293 0.1720 0.022 Uiso 1 1 calc R . . C26A C 1.00908(9) 0.58223(16) 0.25184(10) 0.0198(4) Uani 1 1 d . . . H26A H 1.0243 0.5396 0.2168 0.024 Uiso 1 1 calc R . . C27A C 1.04038(9) 0.69282(17) 0.26163(11) 0.0224(4) Uani 1 1 d . . . H27C H 1.0886 0.6859 0.2809 0.027 Uiso 1 1 calc R . . H27D H 1.0278 0.7295 0.2133 0.027 Uiso 1 1 calc R . . C28A C 1.02882(9) 0.52553(16) 0.32663(10) 0.0212(4) Uani 1 1 d . . . H28C H 1.0769 0.5169 0.3466 0.025 Uiso 1 1 calc R . . H28D H 1.0088 0.4538 0.3204 0.025 Uiso 1 1 calc R . . O1G O 0.22686(12) 0.5517(2) 0.30830(11) 0.0666(6) Uani 1 1 d . . . C1G C 0.28917(15) 0.5416(3) 0.30195(17) 0.0642(10) Uani 1 1 d . . . H1GA H 0.3170 0.4949 0.3416 0.077 Uiso 1 1 calc R . . H1GB H 0.3104 0.6123 0.3067 0.077 Uiso 1 1 calc R . . C2G C 0.28118(15) 0.4943(4) 0.2279(2) 0.0828(13) Uani 1 1 d . . . H2GA H 0.2956 0.5451 0.1971 0.099 Uiso 1 1 calc R . . H2GB H 0.3068 0.4278 0.2332 0.099 Uiso 1 1 calc R . . C3G C 0.21164(14) 0.4729(3) 0.19525(18) 0.0690(10) Uani 1 1 d . . . H3GA H 0.1937 0.5072 0.1461 0.083 Uiso 1 1 calc R . . H3GB H 0.2037 0.3953 0.1892 0.083 Uiso 1 1 calc R . . C4G C 0.18128(15) 0.5157(3) 0.24420(19) 0.0646(9) Uani 1 1 d . . . H4GA H 0.1522 0.5751 0.2195 0.078 Uiso 1 1 calc R . . H4GB H 0.1542 0.4600 0.2560 0.078 Uiso 1 1 calc R . . O2H O 0.45774(14) 0.5472(2) 0.4521(2) 0.0404(8) Uani 0.50 1 d P . . C1H C 0.52764(13) 0.5641(3) 0.47585(15) 0.0555(8) Uani 1 1 d . . . H1HA H 0.5447 0.5173 0.4451 0.067 Uiso 1 1 calc R . . H1HB H 0.5345 0.6383 0.4627 0.067 Uiso 1 1 calc R . . C2H C 0.43382(16) 0.4506(3) 0.45349(19) 0.0644(9) Uani 1 1 d . . . H2HA H 0.4432 0.4005 0.4186 0.077 Uiso 1 1 calc R . . H2HB H 0.3866 0.4505 0.4467 0.077 Uiso 1 1 calc R . . O3I O 0.03327(19) 0.4582(3) 0.0745(2) 0.0488(9) Uani 0.50 1 d P . . C1I C -0.02084(17) 0.5068(2) 0.04988(16) 0.0564(8) Uani 1 1 d . . . H1IA H -0.0126 0.5817 0.0665 0.068 Uiso 1 1 calc R . . H1IB H -0.0497 0.4761 0.0749 0.068 Uiso 1 1 calc R . . C2I C 0.05800(17) 0.4909(3) 0.02866(18) 0.0679(9) Uani 1 1 d . . . H2IA H 0.0973 0.4470 0.0350 0.082 Uiso 1 1 calc R . . H2IB H 0.0734 0.5644 0.0433 0.082 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 0.0104(8) 0.0167(8) 0.0147(8) 0.0001(6) 0.0022(6) 0.0002(6) C2 0.0173(9) 0.0179(8) 0.0147(8) -0.0014(7) 0.0035(7) -0.0010(7) C3 0.0179(9) 0.0174(9) 0.0211(9) -0.0011(7) 0.0089(7) -0.0001(7) C4 0.0163(9) 0.0168(9) 0.0260(10) 0.0001(7) 0.0076(7) -0.0021(7) C5 0.0160(9) 0.0157(8) 0.0196(9) -0.0037(7) 0.0019(7) -0.0014(7) C6 0.0155(8) 0.0161(8) 0.0174(8) -0.0021(7) 0.0051(7) 0.0010(6) C7 0.0156(8) 0.0164(8) 0.0196(9) 0.0033(7) 0.0036(7) -0.0004(7) C8 0.0150(8) 0.0159(8) 0.0224(9) 0.0025(7) 0.0004(7) 0.0019(7) C9 0.0149(8) 0.0163(9) 0.0292(10) -0.0021(7) 0.0053(8) 0.0015(7) C10 0.0151(9) 0.0224(9) 0.0195(9) -0.0010(7) -0.0019(7) -0.0015(7) C11 0.0163(9) 0.0186(9) 0.0157(8) 0.0001(7) 0.0035(7) -0.0003(7) C12 0.0164(9) 0.0202(9) 0.0164(9) 0.0005(7) 0.0042(7) 0.0005(7) C13 0.0164(9) 0.0206(9) 0.0164(9) 0.0003(7) 0.0048(7) 0.0002(7) C14 0.0161(9) 0.0226(9) 0.0161(8) -0.0002(7) 0.0046(7) 0.0005(7) C15 0.0170(9) 0.0212(9) 0.0164(9) -0.0001(7) 0.0052(7) 0.0001(7) C16 0.0165(9) 0.0221(9) 0.0155(8) -0.0004(7) 0.0037(7) -0.0004(7) C17 0.0176(9) 0.0199(9) 0.0169(9) -0.0010(7) 0.0033(7) -0.0004(7) C18 0.0164(9) 0.0194(9) 0.0165(8) 0.0007(7) 0.0030(7) -0.0002(7) C19 0.0105(8) 0.0176(8) 0.0172(8) 0.0015(7) -0.0003(7) 0.0000(6) C20 0.0179(9) 0.0168(8) 0.0206(9) 0.0029(7) 0.0073(7) 0.0003(7) C21 0.0200(9) 0.0184(9) 0.0208(9) 0.0046(7) 0.0063(7) 0.0042(7) C22 0.0166(9) 0.0205(9) 0.0241(10) 0.0017(7) 0.0070(7) 0.0013(7) C23 0.0160(9) 0.0233(9) 0.0276(10) 0.0072(8) 0.0074(8) -0.0006(7) C24 0.0163(9) 0.0220(9) 0.0190(9) 0.0057(7) 0.0029(7) -0.0010(7) C25 0.0171(9) 0.0208(9) 0.0259(10) -0.0059(8) -0.0012(8) 0.0022(7) C26 0.0175(9) 0.0256(10) 0.0301(11) -0.0086(8) -0.0054(8) 0.0013(8) C27 0.0128(9) 0.0205(10) 0.0445(13) 0.0037(9) 0.0013(8) -0.0015(7) C28 0.0220(10) 0.0329(11) 0.0203(10) 0.0010(8) -0.0009(8) 0.0091(8) C1A 0.0098(8) 0.0176(8) 0.0158(8) 0.0003(6) 0.0020(6) 0.0006(6) C2A 0.0174(9) 0.0278(10) 0.0164(9) 0.0016(7) 0.0023(7) -0.0042(7) C3A 0.0180(9) 0.0318(11) 0.0188(9) 0.0005(8) 0.0061(7) -0.0062(8) C4A 0.0172(9) 0.0203(9) 0.0229(9) -0.0018(7) 0.0022(7) -0.0032(7) C5A 0.0169(9) 0.0224(9) 0.0152(8) -0.0024(7) 0.0001(7) -0.0009(7) C6A 0.0163(9) 0.0222(9) 0.0156(8) -0.0003(7) 0.0043(7) 0.0003(7) C7A 0.0120(8) 0.0186(9) 0.0290(10) -0.0040(7) 0.0023(7) 0.0011(7) C8A 0.0107(8) 0.0213(10) 0.0416(12) -0.0075(8) 0.0032(8) 0.0029(7) C9A 0.0165(9) 0.0403(12) 0.0340(12) -0.0157(9) 0.0117(9) -0.0059(8) C10A 0.0139(9) 0.0245(10) 0.0291(11) 0.0037(8) -0.0036(8) -0.0005(7) C11A 0.0145(8) 0.0191(9) 0.0163(8) 0.0007(7) 0.0031(7) 0.0014(7) C12A 0.0149(9) 0.0212(9) 0.0169(9) 0.0023(7) 0.0042(7) 0.0017(7) C13A 0.0139(8) 0.0207(9) 0.0181(9) 0.0015(7) 0.0047(7) 0.0008(7) C14A 0.0138(8) 0.0195(9) 0.0185(9) 0.0009(7) 0.0046(7) 0.0010(7) C15A 0.0142(8) 0.0197(9) 0.0191(9) 0.0005(7) 0.0048(7) -0.0001(7) C16A 0.0141(8) 0.0226(9) 0.0171(9) -0.0006(7) 0.0040(7) -0.0004(7) C17A 0.0145(9) 0.0235(9) 0.0171(9) -0.0016(7) 0.0036(7) -0.0007(7) C18A 0.0149(9) 0.0213(9) 0.0169(9) -0.0020(7) 0.0040(7) -0.0007(7) C19A 0.0092(8) 0.0195(8) 0.0161(8) 0.0003(7) 0.0016(6) -0.0009(6) C20A 0.0142(8) 0.0213(9) 0.0172(9) 0.0018(7) 0.0053(7) -0.0008(7) C21A 0.0149(8) 0.0239(9) 0.0146(8) 0.0023(7) 0.0026(7) 0.0017(7) C22A 0.0128(8) 0.0277(10) 0.0179(9) -0.0025(7) 0.0007(7) -0.0013(7) C23A 0.0128(8) 0.0231(9) 0.0224(9) -0.0002(7) 0.0026(7) -0.0040(7) C24A 0.0143(8) 0.0183(9) 0.0210(9) 0.0006(7) 0.0031(7) -0.0006(7) C25A 0.0138(8) 0.0247(9) 0.0152(8) -0.0028(7) 0.0025(7) 0.0001(7) C26A 0.0129(8) 0.0289(10) 0.0170(9) -0.0035(7) 0.0045(7) 0.0010(7) C27A 0.0130(8) 0.0330(11) 0.0206(9) 0.0031(8) 0.0048(7) -0.0018(7) C28A 0.0152(9) 0.0238(9) 0.0220(9) 0.0010(7) 0.0030(7) 0.0046(7) O1G 0.0739(16) 0.0853(17) 0.0413(11) -0.0166(11) 0.0202(11) 0.0002(13) C1G 0.0492(18) 0.073(2) 0.0481(17) 0.0156(16) -0.0131(14) -0.0273(16) C2G 0.0395(17) 0.123(3) 0.098(3) -0.042(3) 0.0387(18) -0.0112(19) C3G 0.0391(16) 0.113(3) 0.0530(18) -0.0371(19) 0.0136(14) -0.0131(17) C4G 0.0440(17) 0.082(2) 0.077(2) -0.0362(19) 0.0333(16) -0.0176(16) O2H 0.0198(15) 0.0177(15) 0.081(3) -0.0051(15) 0.0139(16) -0.0002(12) C1H 0.0403(15) 0.090(2) 0.0373(15) -0.0001(15) 0.0151(12) 0.0004(15) C2H 0.0488(18) 0.081(2) 0.065(2) 0.0038(18) 0.0203(16) 0.0040(17) O3I 0.044(2) 0.058(2) 0.037(2) 0.0123(18) 0.0039(17) 0.0003(19) C1I 0.094(3) 0.0376(15) 0.0433(16) 0.0031(12) 0.0310(17) 0.0026(15) C2I 0.061(2) 0.068(2) 0.058(2) 0.0046(17) -0.0009(17) 0.0107(17) _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 C11 1.464(2) . ? C1 C7 1.546(2) . ? C1 C6 1.546(2) . ? C1 C2 1.548(2) . ? C2 C3 1.529(2) . ? C3 C9 1.531(3) . ? C3 C4 1.534(3) . ? C4 C5 1.534(3) . ? C5 C6 1.535(2) . ? C5 C10 1.531(3) . ? C7 C8 1.535(2) . ? C8 C9 1.533(3) . ? C8 C10 1.534(3) . ? C11 C12 1.206(2) . ? C12 C13 1.365(2) . ? C13 C14 1.214(3) . ? C14 C15 1.358(3) . ? C15 C16 1.210(2) . ? C16 C17 1.371(3) . ? C17 C18 1.204(3) . ? C18 C19 1.469(2) . ? C19 C20 1.547(2) . ? C19 C24 1.548(2) . ? C19 C25 1.546(3) . ? C20 C21 1.534(2) . ? C21 C28 1.529(3) . ? C21 C22 1.531(3) . ? C22 C23 1.531(3) . ? C23 C27 1.531(3) . ? C23 C24 1.530(3) . ? C25 C26 1.538(3) . ? C26 C27 1.534(3) . ? C26 C28 1.535(3) . ? C1A C11A 1.466(2) . ? C1A C6A 1.543(2) . ? C1A C2A 1.542(2) . ? C1A C7A 1.544(2) . ? C2A C3A 1.532(3) . ? C3A C4A 1.532(3) . ? C3A C9A 1.537(3) . ? C4A C5A 1.527(3) . ? C5A C10A 1.529(3) . ? C5A C6A 1.533(2) . ? C7A C8A 1.533(2) . ? C8A C10A 1.530(3) . ? C8A C9A 1.530(3) . ? C11A C12A 1.205(2) . ? C12A C13A 1.365(2) . ? C13A C14A 1.212(2) . ? C14A C15A 1.360(2) . ? C15A C16A 1.211(2) . ? C16A C17A 1.366(2) . ? C17A C18A 1.204(2) . ? C18A C19A 1.462(2) . ? C19A C24A 1.546(2) . ? C19A C20A 1.548(2) . ? C19A C25A 1.547(2) . ? C20A C21A 1.533(2) . ? C21A C22A 1.533(3) . ? C21A C28A 1.534(3) . ? C22A C23A 1.533(3) . ? C23A C27A 1.534(3) . ? C23A C24A 1.533(2) . ? C25A C26A 1.534(2) . ? C26A C27A 1.530(3) . ? C26A C28A 1.531(3) . ? O1G C4G 1.371(4) . ? O1G C1G 1.408(4) . ? C1G C2G 1.498(5) . ? C2G C3G 1.453(4) . ? C3G C4G 1.426(4) . ? O2H C2H 1.323(5) . ? O2H C1H 1.447(4) . ? C1H C2H 1.346(4) 3_666 ? C2H C1H 1.346(4) 3_666 ? O3I C2I 1.248(5) . ? O3I C1I 1.267(5) . ? C1I C2I 1.452(4) 3_565 ? C2I C1I 1.452(4) 3_565 ? 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 C11 C1 C7 110.49(14) . . ? C11 C1 C6 110.72(14) . . ? C7 C1 C6 108.70(14) . . ? C11 C1 C2 108.76(14) . . ? C7 C1 C2 108.83(14) . . ? C6 C1 C2 109.31(14) . . ? C3 C2 C1 109.97(14) . . ? C9 C3 C2 109.21(15) . . ? C9 C3 C4 109.87(15) . . ? C2 C3 C4 109.22(14) . . ? C5 C4 C3 109.69(15) . . ? C4 C5 C6 109.30(15) . . ? C4 C5 C10 109.70(15) . . ? C6 C5 C10 109.63(15) . . ? C5 C6 C1 109.53(14) . . ? C8 C7 C1 109.70(14) . . ? C9 C8 C10 109.45(15) . . ? C9 C8 C7 109.65(15) . . ? C10 C8 C7 109.37(15) . . ? C3 C9 C8 109.71(15) . . ? C8 C10 C5 109.62(15) . . ? C12 C11 C1 176.69(19) . . ? C11 C12 C13 176.4(2) . . ? C14 C13 C12 176.7(2) . . ? C13 C14 C15 178.3(2) . . ? C16 C15 C14 177.6(2) . . ? C15 C16 C17 176.4(2) . . ? C18 C17 C16 176.1(2) . . ? C17 C18 C19 176.0(2) . . ? C18 C19 C20 108.96(15) . . ? C18 C19 C24 109.89(15) . . ? C20 C19 C24 109.03(15) . . ? C18 C19 C25 110.90(15) . . ? C20 C19 C25 109.10(15) . . ? C24 C19 C25 108.92(15) . . ? C21 C20 C19 109.58(14) . . ? C28 C21 C22 109.93(16) . . ? C28 C21 C20 109.31(15) . . ? C22 C21 C20 109.47(15) . . ? C21 C22 C23 109.69(15) . . ? C27 C23 C24 109.70(16) . . ? C27 C23 C22 109.35(16) . . ? C24 C23 C22 109.43(15) . . ? C23 C24 C19 109.74(15) . . ? C26 C25 C19 109.58(15) . . ? C25 C26 C27 109.52(17) . . ? C25 C26 C28 109.32(17) . . ? C27 C26 C28 109.27(17) . . ? C23 C27 C26 109.83(16) . . ? C21 C28 C26 109.70(16) . . ? C11A C1A C6A 110.18(14) . . ? C11A C1A C2A 108.86(14) . . ? C6A C1A C2A 108.94(15) . . ? C11A C1A C7A 110.71(15) . . ? C6A C1A C7A 108.67(14) . . ? C2A C1A C7A 109.45(15) . . ? C3A C2A C1A 109.84(15) . . ? C4A C3A C2A 109.65(15) . . ? C4A C3A C9A 109.32(16) . . ? C2A C3A C9A 109.00(16) . . ? C5A C4A C3A 109.77(15) . . ? C10A C5A C4A 109.75(16) . . ? C10A C5A C6A 109.31(15) . . ? C4A C5A C6A 109.54(15) . . ? C5A C6A C1A 109.87(14) . . ? C8A C7A C1A 109.34(15) . . ? C10A C8A C9A 109.88(16) . . ? C10A C8A C7A 109.66(16) . . ? C9A C8A C7A 109.51(17) . . ? C8A C9A C3A 109.63(15) . . ? C5A C10A C8A 109.35(16) . . ? C12A C11A C1A 176.17(19) . . ? C11A C12A C13A 175.9(2) . . ? C14A C13A C12A 176.1(2) . . ? C13A C14A C15A 177.9(2) . . ? C16A C15A C14A 177.9(2) . . ? C15A C16A C17A 176.2(2) . . ? C18A C17A C16A 176.2(2) . . ? C17A C18A C19A 177.1(2) . . ? C18A C19A C24A 110.23(15) . . ? C18A C19A C20A 110.25(14) . . ? C24A C19A C20A 109.00(14) . . ? C18A C19A C25A 109.37(14) . . ? C24A C19A C25A 109.19(14) . . ? C20A C19A C25A 108.77(14) . . ? C21A C20A C19A 109.85(14) . . ? C22A C21A C20A 109.22(15) . . ? C22A C21A C28A 109.67(15) . . ? C20A C21A C28A 109.36(15) . . ? C21A C22A C23A 109.61(15) . . ? C27A C23A C22A 109.68(16) . . ? C27A C23A C24A 109.54(15) . . ? C22A C23A C24A 109.46(15) . . ? C23A C24A C19A 109.44(15) . . ? C26A C25A C19A 109.74(14) . . ? C27A C26A C25A 109.37(16) . . ? C27A C26A C28A 109.59(15) . . ? C25A C26A C28A 109.46(15) . . ? C23A C27A C26A 109.73(15) . . ? C26A C28A C21A 109.78(15) . . ? C4G O1G C1G 108.4(2) . . ? O1G C1G C2G 108.3(2) . . ? C3G C2G C1G 104.6(2) . . ? C4G C3G C2G 107.0(3) . . ? O1G C4G C3G 111.3(3) . . ? C2H O2H C1H 120.4(3) . . ? C2H C1H O2H 121.8(3) 3_666 . ? O2H C2H C1H 91.8(3) . 3_666 ? C2I O3I C1I 98.4(3) . . ? O3I C1I C2I 121.2(3) . 3_565 ? O3I C2I C1I 121.4(3) . 3_565 ? 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 C11 C1 C2 C3 179.98(14) . . . . ? C7 C1 C2 C3 -59.60(18) . . . . ? C6 C1 C2 C3 58.98(18) . . . . ? C1 C2 C3 C9 60.40(19) . . . . ? C1 C2 C3 C4 -59.77(19) . . . . ? C9 C3 C4 C5 -58.99(19) . . . . ? C2 C3 C4 C5 60.77(19) . . . . ? C3 C4 C5 C6 -61.02(19) . . . . ? C3 C4 C5 C10 59.22(19) . . . . ? C4 C5 C6 C1 60.05(18) . . . . ? C10 C5 C6 C1 -60.22(19) . . . . ? C11 C1 C6 C5 -178.70(14) . . . . ? C7 C1 C6 C5 59.76(18) . . . . ? C2 C1 C6 C5 -58.90(18) . . . . ? C11 C1 C7 C8 178.33(15) . . . . ? C6 C1 C7 C8 -59.98(18) . . . . ? C2 C1 C7 C8 58.98(18) . . . . ? C1 C7 C8 C9 -59.68(19) . . . . ? C1 C7 C8 C10 60.34(19) . . . . ? C2 C3 C9 C8 -60.46(19) . . . . ? C4 C3 C9 C8 59.31(19) . . . . ? C10 C8 C9 C3 -59.69(19) . . . . ? C7 C8 C9 C3 60.27(19) . . . . ? C9 C8 C10 C5 59.97(19) . . . . ? C7 C8 C10 C5 -60.17(19) . . . . ? C4 C5 C10 C8 -59.81(19) . . . . ? C6 C5 C10 C8 60.22(19) . . . . ? C7 C1 C11 C12 -123(3) . . . . ? C6 C1 C11 C12 116(3) . . . . ? C2 C1 C11 C12 -4(3) . . . . ? C1 C11 C12 C13 -21(6) . . . . ? C11 C12 C13 C14 18(6) . . . . ? C12 C13 C14 C15 -61(9) . . . . ? C13 C14 C15 C16 -58(10) . . . . ? C14 C15 C16 C17 -20(8) . . . . ? C15 C16 C17 C18 22(6) . . . . ? C16 C17 C18 C19 16(5) . . . . ? C17 C18 C19 C20 35(3) . . . . ? C17 C18 C19 C24 -85(3) . . . . ? C17 C18 C19 C25 155(3) . . . . ? C18 C19 C20 C21 -179.15(15) . . . . ? C24 C19 C20 C21 -59.21(18) . . . . ? C25 C19 C20 C21 59.64(19) . . . . ? C19 C20 C21 C28 -60.43(19) . . . . ? C19 C20 C21 C22 60.03(19) . . . . ? C28 C21 C22 C23 59.5(2) . . . . ? C20 C21 C22 C23 -60.6(2) . . . . ? C21 C22 C23 C27 -59.6(2) . . . . ? C21 C22 C23 C24 60.5(2) . . . . ? C27 C23 C24 C19 59.9(2) . . . . ? C22 C23 C24 C19 -60.0(2) . . . . ? C18 C19 C24 C23 178.67(15) . . . . ? C20 C19 C24 C23 59.30(19) . . . . ? C25 C19 C24 C23 -59.65(19) . . . . ? C18 C19 C25 C26 -179.35(16) . . . . ? C20 C19 C25 C26 -59.3(2) . . . . ? C24 C19 C25 C26 59.6(2) . . . . ? C19 C25 C26 C27 -59.9(2) . . . . ? C19 C25 C26 C28 59.8(2) . . . . ? C24 C23 C27 C26 -59.9(2) . . . . ? C22 C23 C27 C26 60.1(2) . . . . ? C25 C26 C27 C23 59.9(2) . . . . ? C28 C26 C27 C23 -59.9(2) . . . . ? C22 C21 C28 C26 -59.3(2) . . . . ? C20 C21 C28 C26 60.8(2) . . . . ? C25 C26 C28 C21 -60.5(2) . . . . ? C27 C26 C28 C21 59.3(2) . . . . ? C11A C1A C2A C3A -179.41(15) . . . . ? C6A C1A C2A C3A -59.23(19) . . . . ? C7A C1A C2A C3A 59.46(19) . . . . ? C1A C2A C3A C4A 59.7(2) . . . . ? C1A C2A C3A C9A -59.9(2) . . . . ? C2A C3A C4A C5A -59.9(2) . . . . ? C9A C3A C4A C5A 59.5(2) . . . . ? C3A C4A C5A C10A -60.08(19) . . . . ? C3A C4A C5A C6A 59.9(2) . . . . ? C10A C5A C6A C1A 60.34(19) . . . . ? C4A C5A C6A C1A -59.95(19) . . . . ? C11A C1A C6A C5A 178.71(15) . . . . ? C2A C1A C6A C5A 59.36(19) . . . . ? C7A C1A C6A C5A -59.82(19) . . . . ? C11A C1A C7A C8A -179.17(16) . . . . ? C6A C1A C7A C8A 59.7(2) . . . . ? C2A C1A C7A C8A -59.2(2) . . . . ? C1A C7A C8A C10A -60.6(2) . . . . ? C1A C7A C8A C9A 60.0(2) . . . . ? C10A C8A C9A C3A 59.6(2) . . . . ? C7A C8A C9A C3A -61.0(2) . . . . ? C4A C3A C9A C8A -59.2(2) . . . . ? C2A C3A C9A C8A 60.6(2) . . . . ? C4A C5A C10A C8A 59.8(2) . . . . ? C6A C5A C10A C8A -60.3(2) . . . . ? C9A C8A C10A C5A -59.7(2) . . . . ? C7A C8A C10A C5A 60.7(2) . . . . ? C6A C1A C11A C12A -115(3) . . . . ? C2A C1A C11A C12A 4(3) . . . . ? C7A C1A C11A C12A 125(3) . . . . ? C1A C11A C12A C13A -31(5) . . . . ? C11A C12A C13A C14A -8(5) . . . . ? C12A C13A C14A C15A 44(8) . . . . ? C13A C14A C15A C16A 71(9) . . . . ? C14A C15A C16A C17A 43(8) . . . . ? C15A C16A C17A C18A -7(6) . . . . ? C16A C17A C18A C19A -10(7) . . . . ? C17A C18A C19A C24A 122(4) . . . . ? C17A C18A C19A C20A -118(4) . . . . ? C17A C18A C19A C25A 2(4) . . . . ? C18A C19A C20A C21A 179.41(15) . . . . ? C24A C19A C20A C21A -59.47(18) . . . . ? C25A C19A C20A C21A 59.49(18) . . . . ? C19A C20A C21A C22A 60.03(19) . . . . ? C19A C20A C21A C28A -60.00(19) . . . . ? C20A C21A C22A C23A -60.52(19) . . . . ? C28A C21A C22A C23A 59.32(19) . . . . ? C21A C22A C23A C27A -59.36(19) . . . . ? C21A C22A C23A C24A 60.86(19) . . . . ? C27A C23A C24A C19A 59.98(19) . . . . ? C22A C23A C24A C19A -60.32(19) . . . . ? C18A C19A C24A C23A -179.46(15) . . . . ? C20A C19A C24A C23A 59.41(18) . . . . ? C25A C19A C24A C23A -59.29(19) . . . . ? C18A C19A C25A C26A -179.93(15) . . . . ? C24A C19A C25A C26A 59.38(19) . . . . ? C20A C19A C25A C26A -59.46(19) . . . . ? C19A C25A C26A C27A -59.92(19) . . . . ? C19A C25A C26A C28A 60.2(2) . . . . ? C22A C23A C27A C26A 59.56(19) . . . . ? C24A C23A C27A C26A -60.6(2) . . . . ? C25A C26A C27A C23A 60.39(19) . . . . ? C28A C26A C27A C23A -59.60(19) . . . . ? C27A C26A C28A C21A 59.60(19) . . . . ? C25A C26A C28A C21A -60.3(2) . . . . ? C22A C21A C28A C26A -59.52(19) . . . . ? C20A C21A C28A C26A 60.23(19) . . . . ? C4G O1G C1G C2G -0.5(4) . . . . ? O1G C1G C2G C3G -3.3(4) . . . . ? C1G C2G C3G C4G 5.7(5) . . . . ? C1G O1G C4G C3G 4.4(4) . . . . ? C2G C3G C4G O1G -6.5(5) . . . . ? C2H O2H C1H C2H -66.0(6) . . . 3_666 ? C1H O2H C2H C1H 51.0(4) . . . 3_666 ? C2I O3I C1I C2I 45.2(5) . . . 3_565 ? C1I O3I C2I C1I -45.3(5) . . . 3_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.656 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.064 # Attachment 'tomu_7x_0m.cif' data_tomu_7x_0m _database_code_depnum_ccdc_archive 'CCDC 288448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H62.50 N2.50' _chemical_formula_weight 782.60 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' N N 0.0061 0.0033 '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 10.7534(6) _cell_length_b 11.5581(6) _cell_length_c 19.0689(11) _cell_angle_alpha 98.037(3) _cell_angle_beta 105.183(3) _cell_angle_gamma 99.764(3) _cell_volume 2211.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description splitter _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9544 _exptl_absorpt_correction_T_max 0.9953 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 52178 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.20 _reflns_number_total 10895 _reflns_number_gt 7383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _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^)+(0.0000P)^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_number_reflns 10895 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.47258(11) -0.25046(9) 0.31990(6) 0.0181(3) Uani 1 1 d . . . C2 C 0.36018(11) -0.36270(9) 0.30395(7) 0.0231(3) Uani 1 1 d . . . H2A H 0.3274 -0.3658 0.3477 0.028 Uiso 1 1 calc R . . H2B H 0.2859 -0.3587 0.2615 0.028 Uiso 1 1 calc R . . C3 C 0.41293(11) -0.47552(9) 0.28614(7) 0.0260(3) Uani 1 1 d . . . H3 H 0.3407 -0.5481 0.2760 0.031 Uiso 1 1 calc R . . C4 C 0.52693(12) -0.48126(10) 0.35241(7) 0.0283(3) Uani 1 1 d . . . H4A H 0.4956 -0.4837 0.3967 0.034 Uiso 1 1 calc R . . H4B H 0.5595 -0.5550 0.3419 0.034 Uiso 1 1 calc R . . C5 C 0.63889(11) -0.37173(9) 0.36747(7) 0.0226(3) Uani 1 1 d . . . H5 H 0.7135 -0.3765 0.4104 0.027 Uiso 1 1 calc R . . C6 C 0.58755(11) -0.25887(10) 0.38611(6) 0.0223(3) Uani 1 1 d . . . H6A H 0.6597 -0.1872 0.3972 0.027 Uiso 1 1 calc R . . H6B H 0.5567 -0.2617 0.4305 0.027 Uiso 1 1 calc R . . C7 C 0.46201(12) -0.47074(10) 0.21786(7) 0.0271(3) Uani 1 1 d . . . H7A H 0.4943 -0.5440 0.2056 0.033 Uiso 1 1 calc R . . H7B H 0.3885 -0.4670 0.1749 0.033 Uiso 1 1 calc R . . C8 C 0.57358(11) -0.36048(9) 0.23344(7) 0.0217(3) Uani 1 1 d . . . H8 H 0.6056 -0.3578 0.1888 0.026 Uiso 1 1 calc R . . C9 C 0.52179(11) -0.24720(9) 0.25113(6) 0.0222(3) Uani 1 1 d . . . H9A H 0.4486 -0.2424 0.2083 0.027 Uiso 1 1 calc R . . H9B H 0.5932 -0.1754 0.2605 0.027 Uiso 1 1 calc R . . C10 C 0.68701(11) -0.36721(10) 0.29929(6) 0.0230(3) Uani 1 1 d . . . H10A H 0.7213 -0.4396 0.2877 0.028 Uiso 1 1 calc R . . H10B H 0.7597 -0.2963 0.3093 0.028 Uiso 1 1 calc R . . C11 C 0.42488(11) -0.14132(9) 0.33812(6) 0.0196(3) Uani 1 1 d . . . C12 C 0.39142(11) -0.04961(9) 0.35467(6) 0.0198(3) Uani 1 1 d . . . C13 C 0.35812(11) 0.05687(9) 0.37492(6) 0.0196(3) Uani 1 1 d . . . C14 C 0.33429(11) 0.15320(9) 0.39315(6) 0.0193(3) Uani 1 1 d . . . C15 C 0.31074(11) 0.26296(10) 0.41530(6) 0.0196(3) Uani 1 1 d . . . C16 C 0.29006(11) 0.35971(9) 0.43544(6) 0.0197(3) Uani 1 1 d . . . C17 C 0.26081(11) 0.46701(9) 0.45898(6) 0.0212(3) Uani 1 1 d . . . C18 C 0.23157(11) 0.55893(9) 0.47932(6) 0.0212(3) Uani 1 1 d . . . C19 C 0.19854(11) 0.67253(9) 0.50542(6) 0.0196(3) Uani 1 1 d . . . C20 C 0.31084(11) 0.77727(9) 0.50815(7) 0.0224(3) Uani 1 1 d . . . H20A H 0.3948 0.7686 0.5417 0.027 Uiso 1 1 calc R . . H20B H 0.3217 0.7760 0.4581 0.027 Uiso 1 1 calc R . . C21 C 0.27855(11) 0.89647(9) 0.53589(6) 0.0230(3) Uani 1 1 d . . . H21 H 0.3518 0.9639 0.5376 0.028 Uiso 1 1 calc R . . C22 C 0.26341(12) 0.89865(10) 0.61324(7) 0.0300(3) Uani 1 1 d . . . H22A H 0.2438 0.9760 0.6316 0.036 Uiso 1 1 calc R . . H22B H 0.3468 0.8905 0.6476 0.036 Uiso 1 1 calc R . . C23 C 0.15162(13) 0.79613(10) 0.61098(8) 0.0349(4) Uani 1 1 d . . . H23 H 0.1411 0.7981 0.6617 0.042 Uiso 1 1 calc R . . C24 C 0.18312(13) 0.67614(10) 0.58357(7) 0.0320(3) Uani 1 1 d . . . H24A H 0.2658 0.6664 0.6178 0.038 Uiso 1 1 calc R . . H24B H 0.1110 0.6095 0.5826 0.038 Uiso 1 1 calc R . . C25 C 0.02344(13) 0.80880(11) 0.55774(9) 0.0451(4) Uani 1 1 d . . . H25A H -0.0491 0.7421 0.5561 0.054 Uiso 1 1 calc R . . H25B H 0.0008 0.8848 0.5756 0.054 Uiso 1 1 calc R . . C26 C 0.03826(12) 0.80737(10) 0.48038(8) 0.0368(4) Uani 1 1 d . . . H26 H -0.0458 0.8170 0.4462 0.044 Uiso 1 1 calc R . . C27 C 0.06943(11) 0.68744(10) 0.45227(7) 0.0323(3) Uani 1 1 d . . . H27A H 0.0790 0.6856 0.4019 0.039 Uiso 1 1 calc R . . H27B H -0.0038 0.6208 0.4497 0.039 Uiso 1 1 calc R . . C28 C 0.15083(12) 0.91001(10) 0.48323(7) 0.0311(3) Uani 1 1 d . . . H28A H 0.1610 0.9093 0.4331 0.037 Uiso 1 1 calc R . . H28B H 0.1302 0.9874 0.5004 0.037 Uiso 1 1 calc R . . C1A C 0.34619(11) -0.04334(9) 0.08545(6) 0.0196(3) Uani 1 1 d . . . C2A C 0.26763(12) -0.05807(9) 0.14200(7) 0.0241(3) Uani 1 1 d . . . H2A1 H 0.1876 -0.1227 0.1198 0.029 Uiso 1 1 calc R . . H2A2 H 0.3224 -0.0805 0.1863 0.029 Uiso 1 1 calc R . . C3A C 0.22794(12) 0.06017(10) 0.16458(7) 0.0268(3) Uani 1 1 d . . . H3A H 0.1773 0.0506 0.2013 0.032 Uiso 1 1 calc R . . C4A C 0.14148(12) 0.09268(10) 0.09568(7) 0.0283(3) Uani 1 1 d . . . H4A1 H 0.1141 0.1680 0.1099 0.034 Uiso 1 1 calc R . . H4A2 H 0.0610 0.0286 0.0733 0.034 Uiso 1 1 calc R . . C5A C 0.21842(12) 0.10812(9) 0.03940(7) 0.0252(3) Uani 1 1 d . . . H5A H 0.1618 0.1300 -0.0052 0.030 Uiso 1 1 calc R . . C6A C 0.25897(11) -0.00935(9) 0.01648(6) 0.0231(3) Uani 1 1 d . . . H6A1 H 0.3085 0.0004 -0.0202 0.028 Uiso 1 1 calc R . . H6A2 H 0.1792 -0.0739 -0.0068 0.028 Uiso 1 1 calc R . . C7A C 0.35182(12) 0.15944(10) 0.19930(7) 0.0305(3) Uani 1 1 d . . . H7A1 H 0.4078 0.1386 0.2438 0.037 Uiso 1 1 calc R . . H7A2 H 0.3266 0.2353 0.2147 0.037 Uiso 1 1 calc R . . C8A C 0.42906(12) 0.17528(10) 0.14317(7) 0.0278(3) Uani 1 1 d . . . H8A H 0.5096 0.2408 0.1659 0.033 Uiso 1 1 calc R . . C9A C 0.47017(11) 0.05798(9) 0.12064(7) 0.0263(3) Uani 1 1 d . . . H9A1 H 0.5272 0.0371 0.1648 0.032 Uiso 1 1 calc R . . H9A2 H 0.5211 0.0681 0.0847 0.032 Uiso 1 1 calc R . . C10A C 0.34221(12) 0.20744(10) 0.07447(7) 0.0292(3) Uani 1 1 d . . . H10C H 0.3166 0.2838 0.0885 0.035 Uiso 1 1 calc R . . H10D H 0.3923 0.2182 0.0382 0.035 Uiso 1 1 calc R . . C11A C 0.38527(11) -0.15582(9) 0.06441(6) 0.0204(3) Uani 1 1 d . . . C12A C 0.41726(11) -0.24883(9) 0.04894(6) 0.0194(3) Uani 1 1 d . . . C13A C 0.45250(11) -0.35489(9) 0.03013(6) 0.0190(3) Uani 1 1 d . . . C14A C 0.48271(11) -0.44769(9) 0.01120(6) 0.0192(3) Uani 1 1 d . . . N1G1 N 0.72257(13) 0.42274(13) 0.15187(7) 0.0377(3) Uani 1 1 d . . . H1GA H 0.6689(17) 0.3693(16) 0.1035(10) 0.118(8) Uiso 1 1 d . . . H2GA H 0.7518(15) 0.4984(13) 0.1522(8) 0.074(6) Uiso 1 1 d . . . C1G1 C 0.82846(12) 0.37330(10) 0.18491(7) 0.0229(3) Uani 1 1 d . . . C2G1 C 0.93359(12) 0.44066(10) 0.24297(7) 0.0283(3) Uani 1 1 d . . . H2G1 H 0.9352 0.5221 0.2605 0.034 Uiso 1 1 calc R . . C3G1 C 1.03619(13) 0.39018(12) 0.27563(7) 0.0371(4) Uani 1 1 d . . . H3G1 H 1.1078 0.4374 0.3154 0.045 Uiso 1 1 calc R . . C4G1 C 1.03598(14) 0.27148(13) 0.25106(7) 0.0382(4) Uani 1 1 d . . . H4G1 H 1.1071 0.2372 0.2733 0.046 Uiso 1 1 calc R . . C5G1 C 0.93119(13) 0.20445(11) 0.19398(8) 0.0326(3) Uani 1 1 d . . . H5G1 H 0.9298 0.1229 0.1769 0.039 Uiso 1 1 calc R . . C6G1 C 0.82789(12) 0.25351(10) 0.16107(7) 0.0273(3) Uani 1 1 d . . . H6G1 H 0.7558 0.2054 0.1219 0.033 Uiso 1 1 calc R . . N1G2 N 0.81426(13) 0.65231(10) 0.08167(7) 0.0381(3) Uani 1 1 d . . . H1GB H 0.7531(15) 0.6674(13) 0.0441(8) 0.076(6) Uiso 1 1 d . . . H2GB H 0.8839(16) 0.6121(14) 0.0642(9) 0.103(6) Uiso 1 1 d . . . C1G2 C 0.86762(12) 0.74424(10) 0.14415(7) 0.0245(3) Uani 1 1 d . . . C2G2 C 0.84648(13) 0.91512(10) 0.22456(7) 0.0315(3) Uani 1 1 d . . . H2G2 H 0.7974 0.9729 0.2350 0.038 Uiso 1 1 calc R . . C3G2 C 0.79654(12) 0.83001(10) 0.16015(7) 0.0267(3) Uani 1 1 d . . . H3G2 H 0.7137 0.8297 0.1266 0.032 Uiso 1 1 calc R . . C4G2 C 0.96679(14) 0.91748(12) 0.27402(8) 0.0396(4) Uani 1 1 d . . . H4G2 H 1.0005 0.9763 0.3183 0.048 Uiso 1 1 calc R . . C5G2 C 1.03745(13) 0.83302(12) 0.25814(8) 0.0389(4) Uani 1 1 d . . . H5G2 H 1.1207 0.8343 0.2916 0.047 Uiso 1 1 calc R . . C6G2 C 0.98826(12) 0.74669(11) 0.19402(7) 0.0296(3) Uani 1 1 d . . . H6G2 H 1.0374 0.6887 0.1841 0.036 Uiso 1 1 calc R . . N1G3 N 0.1044(3) 0.4195(2) 0.11465(17) 0.0247(6) Uani 0.50 1 d P . . H1GC H 0.048(2) 0.3692(19) 0.1333(13) 0.058(8) Uiso 0.50 1 d P . . H2GC H 0.168(2) 0.4806(19) 0.1528(12) 0.076(8) Uiso 0.50 1 d P . . C1G3 C 0.05432(15) 0.45852(13) 0.06411(10) 0.0453(4) Uani 1 1 d . . . C2G3 C -0.06284(15) 0.39441(12) 0.01282(10) 0.0495(5) Uani 1 1 d . . . H2G3 H -0.1064 0.3215 0.0215 0.059 Uiso 1 1 calc R . . C3G3 C 0.11676(15) 0.56519(13) 0.05037(10) 0.0488(4) Uani 1 1 d . . . H3G3 H 0.1970 0.6102 0.0848 0.059 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 0.0194(7) 0.0151(6) 0.0206(7) 0.0018(5) 0.0063(6) 0.0070(5) C2 0.0212(7) 0.0176(6) 0.0318(8) 0.0020(5) 0.0103(6) 0.0062(5) C3 0.0223(8) 0.0136(6) 0.0422(9) -0.0002(5) 0.0130(7) 0.0028(5) C4 0.0340(8) 0.0207(6) 0.0405(9) 0.0125(6) 0.0197(7) 0.0142(6) C5 0.0233(8) 0.0241(6) 0.0233(8) 0.0082(5) 0.0062(6) 0.0113(5) C6 0.0249(8) 0.0220(6) 0.0206(8) 0.0027(5) 0.0067(6) 0.0075(5) C7 0.0265(8) 0.0213(6) 0.0308(9) -0.0050(6) 0.0056(7) 0.0105(6) C8 0.0245(8) 0.0236(6) 0.0214(8) 0.0038(5) 0.0110(6) 0.0105(5) C9 0.0270(8) 0.0204(6) 0.0219(8) 0.0052(5) 0.0082(6) 0.0098(5) C10 0.0230(8) 0.0208(6) 0.0285(8) 0.0045(5) 0.0106(6) 0.0092(5) C11 0.0190(7) 0.0187(6) 0.0193(7) 0.0028(5) 0.0038(6) 0.0027(5) C12 0.0188(7) 0.0185(6) 0.0210(8) 0.0024(5) 0.0050(6) 0.0035(5) C13 0.0182(7) 0.0198(6) 0.0201(7) 0.0025(5) 0.0051(6) 0.0039(5) C14 0.0175(7) 0.0196(6) 0.0207(8) 0.0034(5) 0.0050(6) 0.0046(5) C15 0.0185(7) 0.0203(6) 0.0210(8) 0.0047(5) 0.0065(6) 0.0044(5) C16 0.0187(7) 0.0198(6) 0.0217(8) 0.0049(5) 0.0069(6) 0.0049(5) C17 0.0227(7) 0.0187(6) 0.0234(8) 0.0046(5) 0.0075(6) 0.0059(5) C18 0.0214(7) 0.0197(6) 0.0230(8) 0.0050(5) 0.0065(6) 0.0049(5) C19 0.0215(7) 0.0143(6) 0.0246(8) 0.0014(5) 0.0091(6) 0.0066(5) C20 0.0213(7) 0.0203(6) 0.0262(8) 0.0014(5) 0.0094(6) 0.0046(5) C21 0.0237(8) 0.0156(6) 0.0280(8) 0.0002(5) 0.0091(6) 0.0003(5) C22 0.0387(9) 0.0208(6) 0.0301(9) -0.0023(6) 0.0123(7) 0.0078(6) C23 0.0530(10) 0.0230(7) 0.0411(10) 0.0039(6) 0.0343(8) 0.0110(6) C24 0.0466(9) 0.0203(6) 0.0385(9) 0.0078(6) 0.0260(8) 0.0094(6) C25 0.0325(9) 0.0222(7) 0.0878(13) -0.0017(7) 0.0363(9) 0.0061(6) C26 0.0218(8) 0.0225(7) 0.0588(11) -0.0043(6) 0.0013(8) 0.0114(6) C27 0.0228(8) 0.0185(6) 0.0469(10) -0.0043(6) 0.0010(7) 0.0046(5) C28 0.0385(9) 0.0167(6) 0.0370(9) 0.0024(6) 0.0072(7) 0.0114(6) C1A 0.0224(7) 0.0153(6) 0.0238(8) 0.0016(5) 0.0104(6) 0.0075(5) C2A 0.0299(8) 0.0188(6) 0.0291(8) 0.0072(5) 0.0145(7) 0.0087(5) C3A 0.0380(9) 0.0222(6) 0.0309(9) 0.0075(6) 0.0226(7) 0.0135(6) C4A 0.0311(8) 0.0211(6) 0.0400(9) 0.0064(6) 0.0182(7) 0.0127(6) C5A 0.0332(8) 0.0205(6) 0.0284(8) 0.0081(5) 0.0136(7) 0.0132(6) C6A 0.0283(8) 0.0195(6) 0.0252(8) 0.0040(5) 0.0121(6) 0.0085(5) C7A 0.0439(9) 0.0206(6) 0.0298(9) 0.0006(6) 0.0140(7) 0.0130(6) C8A 0.0294(8) 0.0171(6) 0.0351(9) -0.0024(6) 0.0120(7) 0.0027(5) C9A 0.0250(8) 0.0188(6) 0.0343(9) -0.0011(6) 0.0109(7) 0.0042(5) C10A 0.0416(9) 0.0161(6) 0.0385(9) 0.0063(6) 0.0241(7) 0.0094(6) C11A 0.0193(7) 0.0196(6) 0.0228(8) 0.0033(5) 0.0078(6) 0.0035(5) C12A 0.0202(7) 0.0183(6) 0.0203(7) 0.0033(5) 0.0069(6) 0.0048(5) C13A 0.0198(7) 0.0183(6) 0.0193(8) 0.0037(5) 0.0065(6) 0.0038(5) C14A 0.0195(7) 0.0184(6) 0.0193(7) 0.0042(5) 0.0046(6) 0.0039(5) N1G1 0.0353(8) 0.0481(8) 0.0358(9) 0.0119(7) 0.0111(7) 0.0213(7) C1G1 0.0227(8) 0.0295(7) 0.0222(8) 0.0084(6) 0.0119(6) 0.0099(6) C2G1 0.0291(8) 0.0257(7) 0.0290(9) -0.0022(6) 0.0116(7) 0.0046(6) C3G1 0.0274(9) 0.0550(10) 0.0250(9) -0.0018(7) 0.0050(7) 0.0105(7) C4G1 0.0406(10) 0.0576(10) 0.0299(9) 0.0186(7) 0.0166(8) 0.0291(8) C5G1 0.0457(10) 0.0246(7) 0.0427(10) 0.0137(6) 0.0305(8) 0.0152(7) C6G1 0.0263(8) 0.0274(7) 0.0257(8) -0.0033(6) 0.0122(7) -0.0012(6) N1G2 0.0310(8) 0.0320(7) 0.0431(9) -0.0065(6) 0.0036(7) 0.0077(6) C1G2 0.0234(8) 0.0222(6) 0.0285(8) 0.0058(6) 0.0102(7) 0.0016(5) C2G2 0.0391(9) 0.0230(7) 0.0391(10) 0.0067(6) 0.0228(8) 0.0061(6) C3G2 0.0243(8) 0.0243(7) 0.0348(9) 0.0104(6) 0.0106(7) 0.0068(6) C4G2 0.0433(10) 0.0399(8) 0.0303(9) -0.0019(7) 0.0137(8) -0.0033(7) C5G2 0.0272(9) 0.0533(9) 0.0329(10) 0.0125(7) 0.0051(7) 0.0021(7) C6G2 0.0242(8) 0.0330(7) 0.0354(9) 0.0108(6) 0.0115(7) 0.0080(6) N1G3 0.0192(17) 0.0241(14) 0.0290(19) 0.0057(13) 0.0065(15) -0.0003(12) C1G3 0.0385(11) 0.0320(9) 0.0698(14) -0.0066(9) 0.0338(10) 0.0045(8) C2G3 0.0416(11) 0.0265(8) 0.0822(14) -0.0107(9) 0.0397(10) -0.0041(7) C3G3 0.0360(10) 0.0349(9) 0.0733(13) -0.0139(8) 0.0321(10) -0.0038(7) _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 C11 1.4715(14) . ? C1 C9 1.5399(15) . ? C1 C6 1.5457(15) . ? C1 C2 1.5497(15) . ? C2 C3 1.5380(14) . ? C3 C4 1.5309(16) . ? C3 C7 1.5321(16) . ? C4 C5 1.5281(15) . ? C5 C10 1.5242(15) . ? C5 C6 1.5331(14) . ? C7 C8 1.5300(15) . ? C8 C10 1.5256(15) . ? C8 C9 1.5364(14) . ? C11 C12 1.2034(14) . ? C12 C13 1.3715(14) . ? C13 C14 1.2089(13) . ? C14 C15 1.3664(14) . ? C15 C16 1.2068(14) . ? C16 C17 1.3743(14) . ? C17 C18 1.2001(14) . ? C18 C19 1.4716(14) . ? C19 C24 1.5377(16) . ? C19 C27 1.5420(15) . ? C19 C20 1.5428(15) . ? C20 C21 1.5341(14) . ? C21 C28 1.5210(16) . ? C21 C22 1.5231(16) . ? C22 C23 1.5251(16) . ? C23 C25 1.5260(18) . ? C23 C24 1.5365(15) . ? C25 C26 1.5229(19) . ? C26 C28 1.5284(17) . ? C26 C27 1.5378(14) . ? C1A C11A 1.4682(14) . ? C1A C9A 1.5432(15) . ? C1A C2A 1.5443(15) . ? C1A C6A 1.5451(15) . ? C2A C3A 1.5378(14) . ? C3A C7A 1.5285(16) . ? C3A C4A 1.5323(16) . ? C4A C5A 1.5287(15) . ? C5A C10A 1.5289(16) . ? C5A C6A 1.5360(14) . ? C7A C8A 1.5289(16) . ? C8A C10A 1.5296(16) . ? C8A C9A 1.5357(14) . ? C11A C12A 1.2045(14) . ? C12A C13A 1.3714(14) . ? C13A C14A 1.2074(13) . ? C14A C14A 1.369(2) 2_645 ? N1G1 C1G1 1.4020(15) . ? C1G1 C2G1 1.3838(16) . ? C1G1 C6G1 1.3940(15) . ? C2G1 C3G1 1.3804(16) . ? C3G1 C4G1 1.3858(17) . ? C4G1 C5G1 1.3713(17) . ? C5G1 C6G1 1.3774(16) . ? N1G2 C1G2 1.3996(16) . ? C1G2 C6G2 1.3864(16) . ? C1G2 C3G2 1.3981(15) . ? C2G2 C3G2 1.3792(15) . ? C2G2 C4G2 1.3805(17) . ? C4G2 C5G2 1.3826(17) . ? C5G2 C6G2 1.3825(17) . ? N1G3 C1G3 1.164(3) . ? C1G3 C2G3 1.389(2) . ? C1G3 C3G3 1.393(2) . ? C2G3 C3G3 1.374(2) 2_565 ? C3G3 C2G3 1.375(2) 2_565 ? 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 C11 C1 C9 110.24(9) . . ? C11 C1 C6 109.30(9) . . ? C9 C1 C6 109.11(9) . . ? C11 C1 C2 110.28(9) . . ? C9 C1 C2 108.95(9) . . ? C6 C1 C2 108.93(9) . . ? C3 C2 C1 109.29(9) . . ? C4 C3 C7 109.58(9) . . ? C4 C3 C2 109.31(10) . . ? C7 C3 C2 109.51(10) . . ? C5 C4 C3 109.83(10) . . ? C10 C5 C4 109.91(10) . . ? C10 C5 C6 109.78(9) . . ? C4 C5 C6 108.81(9) . . ? C5 C6 C1 109.76(9) . . ? C8 C7 C3 109.67(9) . . ? C10 C8 C7 109.51(10) . . ? C10 C8 C9 109.61(9) . . ? C7 C8 C9 109.32(9) . . ? C8 C9 C1 109.79(9) . . ? C5 C10 C8 109.80(9) . . ? C12 C11 C1 177.17(13) . . ? C11 C12 C13 177.86(13) . . ? C14 C13 C12 177.18(12) . . ? C13 C14 C15 178.37(14) . . ? C16 C15 C14 179.45(13) . . ? C15 C16 C17 177.12(13) . . ? C18 C17 C16 178.07(13) . . ? C17 C18 C19 178.77(14) . . ? C18 C19 C24 110.13(9) . . ? C18 C19 C27 110.52(9) . . ? C24 C19 C27 109.47(10) . . ? C18 C19 C20 109.13(9) . . ? C24 C19 C20 108.90(9) . . ? C27 C19 C20 108.66(10) . . ? C21 C20 C19 109.84(9) . . ? C28 C21 C22 109.79(10) . . ? C28 C21 C20 109.33(10) . . ? C22 C21 C20 109.55(10) . . ? C21 C22 C23 109.66(10) . . ? C25 C23 C22 109.52(11) . . ? C25 C23 C24 108.83(11) . . ? C22 C23 C24 109.66(10) . . ? C19 C24 C23 109.72(10) . . ? C26 C25 C23 110.27(10) . . ? C25 C26 C28 109.44(11) . . ? C25 C26 C27 109.20(11) . . ? C28 C26 C27 109.54(10) . . ? C26 C27 C19 109.37(10) . . ? C21 C28 C26 109.71(10) . . ? C11A C1A C9A 109.79(9) . . ? C11A C1A C2A 109.62(9) . . ? C9A C1A C2A 109.22(9) . . ? C11A C1A C6A 110.19(9) . . ? C9A C1A C6A 108.91(10) . . ? C2A C1A C6A 109.09(9) . . ? C3A C2A C1A 109.57(9) . . ? C7A C3A C4A 109.60(10) . . ? C7A C3A C2A 109.56(10) . . ? C4A C3A C2A 109.17(10) . . ? C3A C4A C5A 109.86(10) . . ? C10A C5A C4A 109.28(10) . . ? C10A C5A C6A 109.29(10) . . ? C4A C5A C6A 109.64(9) . . ? C5A C6A C1A 109.58(9) . . ? C3A C7A C8A 109.73(10) . . ? C10A C8A C7A 109.57(10) . . ? C10A C8A C9A 109.29(10) . . ? C7A C8A C9A 109.45(10) . . ? C8A C9A C1A 109.68(9) . . ? C5A C10A C8A 109.97(10) . . ? C12A C11A C1A 178.27(13) . . ? C11A C12A C13A 179.05(14) . . ? C14A C13A C12A 177.85(13) . . ? C13A C14A C14A 179.12(17) . 2_645 ? C2G1 C1G1 C6G1 118.54(11) . . ? C2G1 C1G1 N1G1 121.11(12) . . ? C6G1 C1G1 N1G1 120.33(12) . . ? C3G1 C2G1 C1G1 120.42(12) . . ? C2G1 C3G1 C4G1 120.80(13) . . ? C5G1 C4G1 C3G1 118.77(12) . . ? C4G1 C5G1 C6G1 121.05(12) . . ? C5G1 C6G1 C1G1 120.42(12) . . ? C6G2 C1G2 C3G2 118.81(11) . . ? C6G2 C1G2 N1G2 120.24(12) . . ? C3G2 C1G2 N1G2 120.79(12) . . ? C3G2 C2G2 C4G2 120.92(12) . . ? C2G2 C3G2 C1G2 120.12(12) . . ? C2G2 C4G2 C5G2 119.03(13) . . ? C4G2 C5G2 C6G2 120.69(13) . . ? C5G2 C6G2 C1G2 120.42(12) . . ? N1G3 C1G3 C2G3 120.6(2) . . ? N1G3 C1G3 C3G3 120.5(2) . . ? C2G3 C1G3 C3G3 118.68(17) . . ? C3G3 C2G3 C1G3 120.99(15) 2_565 . ? C2G3 C3G3 C1G3 120.33(16) 2_565 . ? 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 C11 C1 C2 C3 -179.22(10) . . . . ? C9 C1 C2 C3 59.65(12) . . . . ? C6 C1 C2 C3 -59.28(12) . . . . ? C1 C2 C3 C4 59.93(13) . . . . ? C1 C2 C3 C7 -60.13(13) . . . . ? C7 C3 C4 C5 58.89(12) . . . . ? C2 C3 C4 C5 -61.12(12) . . . . ? C3 C4 C5 C10 -59.04(12) . . . . ? C3 C4 C5 C6 61.19(12) . . . . ? C10 C5 C6 C1 59.60(12) . . . . ? C4 C5 C6 C1 -60.71(13) . . . . ? C11 C1 C6 C5 -179.49(9) . . . . ? C9 C1 C6 C5 -58.88(12) . . . . ? C2 C1 C6 C5 59.95(12) . . . . ? C4 C3 C7 C8 -59.34(11) . . . . ? C2 C3 C7 C8 60.55(12) . . . . ? C3 C7 C8 C10 59.79(11) . . . . ? C3 C7 C8 C9 -60.32(12) . . . . ? C10 C8 C9 C1 -59.79(12) . . . . ? C7 C8 C9 C1 60.26(12) . . . . ? C11 C1 C9 C8 179.01(9) . . . . ? C6 C1 C9 C8 58.97(12) . . . . ? C2 C1 C9 C8 -59.84(12) . . . . ? C4 C5 C10 C8 59.50(11) . . . . ? C6 C5 C10 C8 -60.14(12) . . . . ? C7 C8 C10 C5 -59.81(11) . . . . ? C9 C8 C10 C5 60.12(12) . . . . ? C9 C1 C11 C12 -84(3) . . . . ? C6 C1 C11 C12 36(3) . . . . ? C2 C1 C11 C12 156(3) . . . . ? C1 C11 C12 C13 0(6) . . . . ? C11 C12 C13 C14 23(6) . . . . ? C12 C13 C14 C15 -41(7) . . . . ? C13 C14 C15 C16 -58(15) . . . . ? C14 C15 C16 C17 -65(14) . . . . ? C15 C16 C17 C18 -14(6) . . . . ? C16 C17 C18 C19 142(5) . . . . ? C17 C18 C19 C24 -71(6) . . . . ? C17 C18 C19 C27 168(92) . . . . ? C17 C18 C19 C20 49(6) . . . . ? C18 C19 C20 C21 -179.53(10) . . . . ? C24 C19 C20 C21 -59.28(12) . . . . ? C27 C19 C20 C21 59.89(12) . . . . ? C19 C20 C21 C28 -60.37(13) . . . . ? C19 C20 C21 C22 59.98(13) . . . . ? C28 C21 C22 C23 59.86(12) . . . . ? C20 C21 C22 C23 -60.21(13) . . . . ? C21 C22 C23 C25 -59.14(12) . . . . ? C21 C22 C23 C24 60.22(14) . . . . ? C18 C19 C24 C23 178.78(10) . . . . ? C27 C19 C24 C23 -59.52(13) . . . . ? C20 C19 C24 C23 59.15(13) . . . . ? C25 C23 C24 C19 59.85(13) . . . . ? C22 C23 C24 C19 -59.94(14) . . . . ? C22 C23 C25 C26 59.07(13) . . . . ? C24 C23 C25 C26 -60.81(13) . . . . ? C23 C25 C26 C28 -58.98(13) . . . . ? C23 C25 C26 C27 60.91(13) . . . . ? C25 C26 C27 C19 -59.63(14) . . . . ? C28 C26 C27 C19 60.21(15) . . . . ? C18 C19 C27 C26 -179.35(10) . . . . ? C24 C19 C27 C26 59.19(13) . . . . ? C20 C19 C27 C26 -59.63(13) . . . . ? C22 C21 C28 C26 -59.86(12) . . . . ? C20 C21 C28 C26 60.34(13) . . . . ? C25 C26 C28 C21 59.20(12) . . . . ? C27 C26 C28 C21 -60.49(14) . . . . ? C11A C1A C2A C3A 179.44(10) . . . . ? C9A C1A C2A C3A 59.12(12) . . . . ? C6A C1A C2A C3A -59.82(12) . . . . ? C1A C2A C3A C7A -59.76(13) . . . . ? C1A C2A C3A C4A 60.27(12) . . . . ? C7A C3A C4A C5A 59.59(12) . . . . ? C2A C3A C4A C5A -60.41(12) . . . . ? C3A C4A C5A C10A -59.52(12) . . . . ? C3A C4A C5A C6A 60.25(13) . . . . ? C10A C5A C6A C1A 60.09(12) . . . . ? C4A C5A C6A C1A -59.67(13) . . . . ? C11A C1A C6A C5A 179.76(9) . . . . ? C9A C1A C6A C5A -59.76(12) . . . . ? C2A C1A C6A C5A 59.37(12) . . . . ? C4A C3A C7A C8A -59.36(12) . . . . ? C2A C3A C7A C8A 60.41(13) . . . . ? C3A C7A C8A C10A 59.36(12) . . . . ? C3A C7A C8A C9A -60.47(13) . . . . ? C10A C8A C9A C1A -60.00(13) . . . . ? C7A C8A C9A C1A 59.99(13) . . . . ? C11A C1A C9A C8A -179.54(10) . . . . ? C2A C1A C9A C8A -59.31(13) . . . . ? C6A C1A C9A C8A 59.73(12) . . . . ? C4A C5A C10A C8A 59.61(12) . . . . ? C6A C5A C10A C8A -60.38(12) . . . . ? C7A C8A C10A C5A -59.62(12) . . . . ? C9A C8A C10A C5A 60.30(12) . . . . ? C9A C1A C11A C12A 93(4) . . . . ? C2A C1A C11A C12A -27(4) . . . . ? C6A C1A C11A C12A -147(4) . . . . ? C1A C11A C12A C13A 145(7) . . . . ? C11A C12A C13A C14A 23(11) . . . . ? C12A C13A C14A C14A 20(14) . . . 2_645 ? C6G1 C1G1 C2G1 C3G1 0.89(18) . . . . ? N1G1 C1G1 C2G1 C3G1 179.05(12) . . . . ? C1G1 C2G1 C3G1 C4G1 0.0(2) . . . . ? C2G1 C3G1 C4G1 C5G1 -0.6(2) . . . . ? C3G1 C4G1 C5G1 C6G1 0.3(2) . . . . ? C4G1 C5G1 C6G1 C1G1 0.55(19) . . . . ? C2G1 C1G1 C6G1 C5G1 -1.14(18) . . . . ? N1G1 C1G1 C6G1 C5G1 -179.32(11) . . . . ? C4G2 C2G2 C3G2 C1G2 0.16(19) . . . . ? C6G2 C1G2 C3G2 C2G2 0.00(18) . . . . ? N1G2 C1G2 C3G2 C2G2 175.51(12) . . . . ? C3G2 C2G2 C4G2 C5G2 0.1(2) . . . . ? C2G2 C4G2 C5G2 C6G2 -0.5(2) . . . . ? C4G2 C5G2 C6G2 C1G2 0.7(2) . . . . ? C3G2 C1G2 C6G2 C5G2 -0.41(19) . . . . ? N1G2 C1G2 C6G2 C5G2 -175.95(12) . . . . ? N1G3 C1G3 C2G3 C3G3 -174.3(2) . . . 2_565 ? C3G3 C1G3 C2G3 C3G3 0.0(2) . . . 2_565 ? N1G3 C1G3 C3G3 C2G3 174.3(2) . . . 2_565 ? C2G3 C1G3 C3G3 C2G3 0.0(2) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.267 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.042