# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1353 data_cbc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; dihydroxycalix[4]arene-benzocrown-6 ; _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 O6' _chemical_formula_sum 'C42 H42 O6' _chemical_formula_weight 642.76 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.634(3) _cell_length_b 17.432(4) _cell_length_c 19.578(4) _cell_angle_alpha 70.959(17) _cell_angle_beta 89.846(17) _cell_angle_gamma 77.52(2) _cell_volume 3340.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.2 _exptl_crystal_description 'thick plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'Siemens, 1997' _exptl_absorpt_correction_T_min 0.9606 _exptl_absorpt_correction_T_max 0.9768 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4 _diffrn_reflns_number 10291 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 22 _reflns_number_total 8182 _reflns_number_gt 5392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4-PC (Enraf-Nonius, 1993)' _computing_data_reduction 'XCAD4 (Harms, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0552P)^2^+0.4808P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8182 _refine_ls_number_parameters 896 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.090 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.117 _refine_ls_wR_factor_gt 0.100 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.03 _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 O1 O 0.82491(18) 0.20084(12) 0.51048(10) 0.0399(5) Uani 1 1 d . . . O2 O 0.59785(19) 0.17694(12) 0.59810(11) 0.0466(6) Uani 1 1 d . . . O3 O 0.34502(19) 0.20580(12) 0.64855(11) 0.0414(5) Uani 1 1 d . . . O4 O 0.16085(19) 0.19994(12) 0.56091(11) 0.0453(6) Uani 1 1 d . . . O7 O 0.6798(2) 0.80547(13) 0.08692(12) 0.0504(6) Uani 1 1 d . . . O8 O 0.89603(19) 0.82080(12) 0.17498(11) 0.0434(5) Uani 1 1 d . . . O9 O 1.15627(18) 0.79620(12) 0.22907(10) 0.0405(5) Uani 1 1 d . . . O10 O 1.33041(18) 0.80022(12) 0.12969(10) 0.0386(5) Uani 1 1 d . . . O12 O 1.07341(18) 0.79303(12) -0.11781(10) 0.0410(5) Uani 1 1 d . . . C40 C 0.2974(4) 0.1069(2) 0.51373(19) 0.0616(10) Uani 1 1 d DU . . H40C H 0.2355 0.0930 0.4845 0.074 Uiso 0.24 1 calc PR A 2 H40D H 0.2948 0.0725 0.5649 0.074 Uiso 0.24 1 calc PR A 2 H40A H 0.3715 0.0797 0.5504 0.074 Uiso 0.76 1 d PR A 1 H40B H 0.2270 0.0776 0.5293 0.074 Uiso 0.76 1 d PR A 1 O5 O 0.3365(3) 0.10113(17) 0.44387(16) 0.0456(7) Uani 0.76 1 d PDU B 1 C41 C 0.4574(4) 0.1216(3) 0.4342(3) 0.0518(12) Uani 0.76 1 d PDU B 1 H41A H 0.5209 0.0818 0.4734 0.062 Uiso 0.76 1 calc PR B 1 H41B H 0.4509 0.1783 0.4364 0.062 Uiso 0.76 1 calc PR B 1 C42 C 0.5019(4) 0.1185(3) 0.3613(2) 0.0496(12) Uani 0.76 1 d PDU B 1 H42A H 0.5953 0.1176 0.3600 0.060 Uiso 0.76 1 calc PR B 1 H42B H 0.4893 0.0666 0.3549 0.060 Uiso 0.76 1 calc PR B 1 O6 O 0.43114(19) 0.18966(13) 0.30253(11) 0.0454(5) Uani 1 1 d DU . . O5A O 0.4362(10) 0.0809(7) 0.4896(6) 0.081(3) Uani 0.24 1 d PDU B 2 C41A C 0.4170(15) 0.0958(8) 0.4124(6) 0.035(4) Uiso 0.24 1 d PDU B 2 H41C H 0.3241 0.1101 0.3966 0.042 Uiso 0.24 1 calc PR B 2 H41D H 0.4607 0.0465 0.3998 0.042 Uiso 0.24 1 calc PR B 2 C42A C 0.4790(11) 0.1696(8) 0.3786(6) 0.032(3) Uani 0.24 1 d PDU B 2 H42C H 0.4466 0.2160 0.3973 0.038 Uiso 0.24 1 calc PR B 2 H42D H 0.5744 0.1532 0.3853 0.038 Uiso 0.24 1 calc PR B 2 C90 C 1.1910(4) 0.8974(2) 0.0337(2) 0.0828(14) Uani 1 1 d DU . . H90C H 1.2540 0.9282 0.0423 0.099 Uiso 0.46 1 calc PR C 2 H90D H 1.1045 0.9227 0.0451 0.099 Uiso 0.46 1 calc PR C 2 H90A H 1.1856 0.9293 0.0675 0.099 Uiso 0.54 1 d PR C 1 H90B H 1.2585 0.9130 0.0004 0.099 Uiso 0.54 1 d PR C 1 O11 O 1.0647(4) 0.9227(2) -0.0091(2) 0.0440(10) Uani 0.54 1 d PDU D 1 C91 C 1.0758(4) 0.9014(2) -0.06988(18) 0.0576(10) Uani 1 1 d DU . . H91A H 1.1676 0.8913 -0.0808 0.069 Uiso 0.54 1 calc PR D 1 H91B H 1.0265 0.9482 -0.1112 0.069 Uiso 0.54 1 calc PR D 1 H91C H 1.0624 0.9354 -0.1219 0.069 Uiso 0.46 1 d PR D 2 H91D H 1.0187 0.9334 -0.0438 0.069 Uiso 0.46 1 d PR D 2 O11A O 1.1894(5) 0.8967(3) -0.0501(2) 0.0485(12) Uani 0.46 1 d PDU D 2 C1 C 0.8353(3) 0.26445(17) 0.44673(16) 0.0335(7) Uani 1 1 d . . . C2 C 0.7623(3) 0.34425(19) 0.43694(16) 0.0357(7) Uani 1 1 d . . . C3 C 0.7813(3) 0.40863(19) 0.37650(18) 0.0439(8) Uani 1 1 d . . . H3 H 0.7328 0.4638 0.3686 0.053 Uiso 1 1 calc R . . C4 C 0.8693(3) 0.3939(2) 0.32772(18) 0.0484(9) Uani 1 1 d . . . H4 H 0.8820 0.4387 0.2870 0.058 Uiso 1 1 calc R . . C5 C 0.9386(3) 0.3141(2) 0.33819(17) 0.0432(8) Uani 1 1 d . . . H5 H 0.9978 0.3043 0.3039 0.052 Uiso 1 1 calc R . . C6 C 0.9237(3) 0.24765(18) 0.39781(16) 0.0363(8) Uani 1 1 d . . . C7 C 0.6640(3) 0.36167(19) 0.48890(16) 0.0411(8) Uani 1 1 d . . . H7A H 0.6763 0.4108 0.5006 0.049 Uiso 1 1 calc R . . H7B H 0.6804 0.3135 0.5345 0.049 Uiso 1 1 calc R . . C8 C 0.5242(3) 0.37790(16) 0.46033(15) 0.0315(7) Uani 1 1 d . . . C9 C 0.4909(3) 0.36011(17) 0.39972(15) 0.0364(8) Uani 1 1 d . . . H9 H 0.5574 0.3377 0.3745 0.044 Uiso 1 1 calc R . . C10 C 0.3630(3) 0.37409(17) 0.37486(15) 0.0333(7) Uani 1 1 d . . . C11 C 0.2666(3) 0.40691(17) 0.41258(15) 0.0350(7) Uani 1 1 d . . . H11 H 0.1785 0.4175 0.3963 0.042 Uiso 1 1 calc R . . C12 C 0.2983(3) 0.42404(17) 0.47333(15) 0.0369(8) Uani 1 1 d . . . H12 H 0.2320 0.4458 0.4991 0.044 Uiso 1 1 calc R . . C13 C 0.4260(3) 0.40984(17) 0.49697(15) 0.0346(7) Uani 1 1 d . . . H13 H 0.4468 0.4221 0.5388 0.042 Uiso 1 1 calc R . . C14 C 0.3252(3) 0.3511(2) 0.31051(16) 0.0437(8) Uani 1 1 d . B . H14A H 0.2882 0.3013 0.3286 0.052 Uiso 1 1 calc R . . H14B H 0.2567 0.3974 0.2794 0.052 Uiso 1 1 calc R . . C15 C 0.4352(3) 0.3332(2) 0.26475(16) 0.0370(8) Uani 1 1 d . . . C16 C 0.4901(3) 0.25304(19) 0.26483(15) 0.0359(7) Uani 1 1 d . B . C17 C 0.5956(3) 0.23743(19) 0.22520(15) 0.0369(8) Uani 1 1 d . . . C18 C 0.6444(3) 0.3045(2) 0.18422(16) 0.0433(8) Uani 1 1 d . B . H18 H 0.7169 0.2950 0.1572 0.052 Uiso 1 1 calc R . . C19 C 0.5899(3) 0.3844(2) 0.18190(17) 0.0476(9) Uani 1 1 d . . . H19 H 0.6235 0.4297 0.1529 0.057 Uiso 1 1 calc R B . C20 C 0.4858(3) 0.3981(2) 0.22226(17) 0.0445(8) Uani 1 1 d . B . H20 H 0.4483 0.4534 0.2208 0.053 Uiso 1 1 calc R . . C21 C 0.6630(3) 0.15067(19) 0.22720(17) 0.0468(8) Uani 1 1 d . B . H21A H 0.6964 0.1542 0.1793 0.056 Uiso 1 1 calc R . . H21B H 0.5988 0.1157 0.2355 0.056 Uiso 1 1 calc R . . C22 C 0.7742(3) 0.10784(19) 0.28503(16) 0.0406(8) Uani 1 1 d . . . C23 C 0.8322(3) 0.15208(19) 0.31840(16) 0.0403(8) Uani 1 1 d . B . H23 H 0.8020 0.2108 0.3044 0.048 Uiso 1 1 calc R . . C24 C 0.9327(3) 0.11263(18) 0.37146(16) 0.0389(8) Uani 1 1 d . . . C25 C 0.9771(3) 0.0274(2) 0.39023(18) 0.0504(9) Uani 1 1 d . B . H25 H 1.0462 -0.0006 0.4264 0.060 Uiso 1 1 calc R . . C26 C 0.9229(4) -0.0175(2) 0.3573(2) 0.0591(10) Uani 1 1 d . . . H26 H 0.9551 -0.0760 0.3703 0.071 Uiso 1 1 calc R B . C27 C 0.8214(3) 0.0227(2) 0.30532(19) 0.0548(10) Uani 1 1 d . B . H27 H 0.7834 -0.0088 0.2832 0.066 Uiso 1 1 calc R . . C28 C 0.9972(3) 0.16031(19) 0.40778(17) 0.0466(8) Uani 1 1 d . B . H28A H 1.0113 0.1287 0.4603 0.056 Uiso 1 1 calc R . . H28B H 1.0831 0.1628 0.3887 0.056 Uiso 1 1 calc R . . C29 C 0.7315(3) 0.15437(19) 0.50684(16) 0.0458(8) Uani 1 1 d . . . H29A H 0.7688 0.1101 0.4865 0.055 Uiso 1 1 calc R . . H29B H 0.6552 0.1915 0.4749 0.055 Uiso 1 1 calc R . . C30 C 0.6924(3) 0.11644(19) 0.58154(17) 0.0455(8) Uani 1 1 d . . . H30A H 0.6570 0.0676 0.5841 0.055 Uiso 1 1 calc R . . H30B H 0.7684 0.0975 0.6169 0.055 Uiso 1 1 calc R . . C31 C 0.5699(3) 0.15119(19) 0.67179(16) 0.0454(8) Uani 1 1 d . . . H31A H 0.6464 0.1462 0.7030 0.054 Uiso 1 1 calc R . . H31B H 0.5481 0.0960 0.6854 0.054 Uiso 1 1 calc R . . C32 C 0.4585(3) 0.21395(19) 0.68272(17) 0.0450(8) Uani 1 1 d . . . H32A H 0.4487 0.2034 0.7351 0.054 Uiso 1 1 calc R . . H32B H 0.4726 0.2709 0.6606 0.054 Uiso 1 1 calc R . . C33 C 0.2402(3) 0.27175(18) 0.63085(15) 0.0331(7) Uani 1 1 d . . . C34 C 0.1463(3) 0.26868(18) 0.58295(15) 0.0350(7) Uani 1 1 d . . . C35 C 0.0371(3) 0.33156(19) 0.56116(16) 0.0426(8) Uani 1 1 d . . . H35 H -0.0267 0.3295 0.5283 0.051 Uiso 1 1 calc R . . C36 C 0.0195(3) 0.39782(19) 0.58672(17) 0.0438(8) Uani 1 1 d . . . H36 H -0.0559 0.4416 0.5714 0.053 Uiso 1 1 calc R . . C37 C 0.1116(3) 0.4000(2) 0.63441(16) 0.0419(8) Uani 1 1 d . . . H37 H 0.0992 0.4454 0.6524 0.050 Uiso 1 1 calc R . . C38 C 0.2219(3) 0.33738(19) 0.65652(15) 0.0392(8) Uani 1 1 d . . . H38 H 0.2852 0.3396 0.6895 0.047 Uiso 1 1 calc R . . C39 C 0.2508(3) 0.19766(19) 0.50722(17) 0.0522(9) Uani 1 1 d . B . H39A H 0.3242 0.2209 0.5156 0.063 Uiso 1 1 calc R . . H39B H 0.2087 0.2307 0.4583 0.063 Uiso 1 1 calc R . . C51 C 0.6639(3) 0.7437(2) 0.05902(17) 0.0414(8) Uani 1 1 d . . . C52 C 0.7289(3) 0.6619(2) 0.09404(16) 0.0392(8) Uani 1 1 d . . . C53 C 0.6997(3) 0.6007(2) 0.07062(19) 0.0521(9) Uani 1 1 d . . . H53 H 0.7428 0.5442 0.0943 0.063 Uiso 1 1 calc R . . C54 C 0.6099(4) 0.6195(3) 0.0138(2) 0.0666(11) Uani 1 1 d . . . H54 H 0.5911 0.5766 -0.0015 0.080 Uiso 1 1 calc R . . C55 C 0.5479(3) 0.7011(3) -0.0205(2) 0.0640(11) Uani 1 1 d . . . H55 H 0.4848 0.7138 -0.0592 0.077 Uiso 1 1 calc R . . C56 C 0.5745(3) 0.7658(2) -0.00016(18) 0.0497(9) Uani 1 1 d . . . C57 C 0.8268(3) 0.63907(19) 0.15659(16) 0.0430(8) Uani 1 1 d . . . H57A H 0.8115 0.5893 0.1950 0.052 Uiso 1 1 calc R . . H57B H 0.8130 0.6853 0.1767 0.052 Uiso 1 1 calc R . . C58 C 0.9670(3) 0.62091(17) 0.13806(15) 0.0323(7) Uani 1 1 d . . . C59 C 1.0030(3) 0.62903(16) 0.06842(15) 0.0323(7) Uani 1 1 d . . . H59 H 0.9377 0.6457 0.0301 0.039 Uiso 1 1 calc R . . C60 C 1.1319(3) 0.61356(16) 0.05279(14) 0.0295(7) Uani 1 1 d . . . C61 C 1.2257(3) 0.58840(17) 0.10949(16) 0.0357(7) Uani 1 1 d . . . H61 H 1.3144 0.5767 0.1004 0.043 Uiso 1 1 calc R . . C62 C 1.1916(3) 0.58026(17) 0.17887(16) 0.0382(8) Uani 1 1 d . . . H62 H 1.2569 0.5633 0.2172 0.046 Uiso 1 1 calc R . . C63 C 1.0637(3) 0.59638(18) 0.19324(16) 0.0397(8) Uani 1 1 d . . . H63 H 1.0415 0.5907 0.2414 0.048 Uiso 1 1 calc R . . C64 C 1.1729(3) 0.62416(19) -0.02349(15) 0.0412(8) Uani 1 1 d . . . H64A H 1.2246 0.6671 -0.0368 0.049 Uiso 1 1 calc R . . H64B H 1.2298 0.5710 -0.0234 0.049 Uiso 1 1 calc R . . C65 C 1.0648(3) 0.64852(18) -0.08076(14) 0.0321(7) Uani 1 1 d . . . C66 C 1.0154(3) 0.73105(17) -0.12347(15) 0.0320(7) Uani 1 1 d . . . C67 C 0.9103(3) 0.75450(18) -0.17499(15) 0.0353(7) Uani 1 1 d . . . C68 C 0.8559(3) 0.6919(2) -0.18143(16) 0.0428(8) Uani 1 1 d . . . H68 H 0.7836 0.7060 -0.2151 0.051 Uiso 1 1 calc R . . C69 C 0.9035(3) 0.6098(2) -0.14045(17) 0.0457(8) Uani 1 1 d . . . H69 H 0.8648 0.5679 -0.1464 0.055 Uiso 1 1 calc R . . C70 C 1.0065(3) 0.58862(19) -0.09119(16) 0.0404(8) Uani 1 1 d . . . H70 H 1.0392 0.5316 -0.0634 0.048 Uiso 1 1 calc R . . C71 C 0.8557(3) 0.84395(19) -0.21957(17) 0.0503(9) Uani 1 1 d . . . H71A H 0.8091 0.8457 -0.2640 0.060 Uiso 1 1 calc R . . H71B H 0.9280 0.8717 -0.2348 0.060 Uiso 1 1 calc R . . C72 C 0.7651(3) 0.8925(2) -0.18126(17) 0.0467(9) Uani 1 1 d . . . C73 C 0.6817(3) 0.8553(2) -0.13371(17) 0.0484(9) Uani 1 1 d . . . H73 H 0.6816 0.7987 -0.1263 0.058 Uiso 1 1 calc R . . C74 C 0.5978(3) 0.8980(2) -0.09629(18) 0.0558(10) Uani 1 1 d . . . C75 C 0.5989(5) 0.9813(3) -0.1088(2) 0.0826(15) Uani 1 1 d . . . H75 H 0.5433 1.0121 -0.0842 0.099 Uiso 1 1 calc R . . C76 C 0.6793(6) 1.0188(3) -0.1562(2) 0.0931(17) Uani 1 1 d . . . H76 H 0.6774 1.0759 -0.1650 0.112 Uiso 1 1 calc R . . C77 C 0.7636(4) 0.9752(2) -0.19171(19) 0.0671(11) Uani 1 1 d . . . H77 H 0.8206 1.0021 -0.2234 0.081 Uiso 1 1 calc R . . C78 C 0.5127(3) 0.8552(2) -0.0414(2) 0.0665(11) Uani 1 1 d . . . H78A H 0.4917 0.8857 -0.0066 0.080 Uiso 1 1 calc R . . H78B H 0.4308 0.8578 -0.0668 0.080 Uiso 1 1 calc R . . C79 C 0.7850(3) 0.8429(2) 0.06339(17) 0.0526(9) Uani 1 1 d . . . H79A H 0.7621 0.8855 0.0147 0.063 Uiso 1 1 calc R . . H79B H 0.8610 0.8002 0.0602 0.063 Uiso 1 1 calc R . . C80 C 0.8167(3) 0.88285(19) 0.11698(18) 0.0537(9) Uani 1 1 d . . . H80A H 0.8622 0.9275 0.0934 0.064 Uiso 1 1 calc R . . H80B H 0.7364 0.9078 0.1349 0.064 Uiso 1 1 calc R . . C81 C 0.9337(3) 0.85104(18) 0.22895(16) 0.0383(8) Uani 1 1 d . . . H81A H 0.8621 0.8583 0.2603 0.046 Uiso 1 1 calc R . . H81B H 0.9557 0.9057 0.2060 0.046 Uiso 1 1 calc R . . C82 C 1.0484(3) 0.78910(18) 0.27282(16) 0.0389(8) Uani 1 1 d . . . H82A H 1.0648 0.8009 0.3177 0.047 Uiso 1 1 calc R . . H82B H 1.0335 0.7321 0.2863 0.047 Uiso 1 1 calc R . . C83 C 1.3485(3) 0.73203(17) 0.19263(15) 0.0322(7) Uani 1 1 d . . . C84 C 1.2607(3) 0.72993(17) 0.24576(15) 0.0312(7) Uani 1 1 d . . . C85 C 1.2833(3) 0.66342(18) 0.31031(15) 0.0362(8) Uani 1 1 d . . . H85 H 1.2245 0.6618 0.3471 0.043 Uiso 1 1 calc R . . C86 C 1.3922(3) 0.59940(18) 0.32079(16) 0.0370(8) Uani 1 1 d . . . H86 H 1.4074 0.5535 0.3648 0.044 Uiso 1 1 calc R . . C87 C 1.4779(3) 0.60173(19) 0.26825(16) 0.0409(8) Uani 1 1 d . . . H87 H 1.5525 0.5577 0.2760 0.049 Uiso 1 1 calc R . . C88 C 1.4561(3) 0.66829(18) 0.20383(16) 0.0373(8) Uani 1 1 d . . . H88 H 1.5157 0.6698 0.1674 0.045 Uiso 1 1 calc R . . C89 C 1.2312(3) 0.80594(19) 0.07759(17) 0.0526(9) Uani 1 1 d . D . H89A H 1.1573 0.7856 0.1021 0.063 Uiso 1 1 calc R . . H89B H 1.2649 0.7727 0.0463 0.063 Uiso 1 1 calc R . . C92 C 1.0266(3) 0.82505(18) -0.06168(16) 0.0393(8) Uani 1 1 d . D . H92A H 1.0572 0.7827 -0.0136 0.047 Uiso 1 1 calc R . . H92B H 0.9310 0.8390 -0.0654 0.047 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 O1 0.0325(12) 0.0417(13) 0.0421(13) -0.0098(11) -0.0046(10) -0.0079(10) O2 0.0368(13) 0.0461(13) 0.0400(13) 0.0013(11) 0.0019(10) 0.0010(11) O3 0.0327(13) 0.0415(13) 0.0501(13) -0.0153(10) -0.0040(10) -0.0085(11) O4 0.0408(13) 0.0475(14) 0.0578(14) -0.0271(12) 0.0049(11) -0.0164(11) O7 0.0419(14) 0.0547(14) 0.0602(15) -0.0241(12) -0.0007(11) -0.0149(12) O8 0.0487(14) 0.0345(12) 0.0455(13) -0.0162(11) -0.0099(11) -0.0020(10) O9 0.0331(12) 0.0401(13) 0.0441(13) -0.0101(10) 0.0059(10) -0.0054(11) O10 0.0393(13) 0.0402(13) 0.0347(12) -0.0067(10) -0.0006(10) -0.0143(10) O12 0.0388(13) 0.0450(13) 0.0456(13) -0.0186(11) 0.0060(10) -0.0178(11) C40 0.074(3) 0.056(2) 0.060(2) -0.0252(19) 0.029(2) -0.016(2) O5 0.0378(18) 0.0552(19) 0.0531(19) -0.0276(16) 0.0080(17) -0.0150(15) C41 0.042(3) 0.055(3) 0.055(3) -0.007(3) 0.004(3) -0.022(3) C42 0.046(3) 0.040(3) 0.059(3) -0.012(3) 0.014(2) -0.008(2) O6 0.0332(13) 0.0513(14) 0.0505(14) -0.0135(11) 0.0012(11) -0.0130(11) O5A 0.060(7) 0.088(9) 0.073(8) -0.005(6) 0.012(7) -0.004(6) C42A 0.019(7) 0.034(8) 0.048(7) -0.022(7) 0.008(6) -0.004(6) C90 0.114(3) 0.049(2) 0.073(3) 0.009(2) -0.063(3) -0.038(2) O11 0.048(3) 0.033(2) 0.046(2) -0.0131(19) -0.014(2) 0.0013(19) C91 0.087(3) 0.045(2) 0.044(2) -0.0105(18) -0.005(2) -0.027(2) O11A 0.054(3) 0.048(3) 0.038(3) -0.003(2) -0.011(3) -0.018(3) C1 0.0281(17) 0.0328(19) 0.0387(19) -0.0112(15) -0.0088(15) -0.0063(15) C2 0.0255(17) 0.041(2) 0.043(2) -0.0179(16) -0.0096(15) -0.0070(15) C3 0.038(2) 0.038(2) 0.056(2) -0.0171(18) -0.0066(17) -0.0061(16) C4 0.047(2) 0.041(2) 0.054(2) -0.0073(17) -0.0046(18) -0.0169(18) C5 0.0339(19) 0.054(2) 0.045(2) -0.0182(18) 0.0078(16) -0.0156(17) C6 0.0252(17) 0.043(2) 0.0427(19) -0.0184(17) -0.0068(15) -0.0061(15) C7 0.0351(19) 0.046(2) 0.046(2) -0.0254(16) -0.0087(16) -0.0006(15) C8 0.0286(18) 0.0282(16) 0.0361(18) -0.0117(14) -0.0042(14) -0.0015(13) C9 0.0304(19) 0.0394(18) 0.0420(19) -0.0227(15) -0.0023(15) 0.0011(14) C10 0.0295(18) 0.0344(17) 0.0346(18) -0.0128(14) -0.0045(15) -0.0018(14) C11 0.0267(17) 0.0403(18) 0.0365(18) -0.0121(15) -0.0002(14) -0.0055(14) C12 0.034(2) 0.0392(19) 0.0360(19) -0.0137(15) 0.0044(15) -0.0032(15) C13 0.042(2) 0.0300(17) 0.0299(17) -0.0090(14) 0.0008(15) -0.0049(15) C14 0.0279(18) 0.066(2) 0.044(2) -0.0320(17) -0.0010(15) -0.0041(16) C15 0.0249(17) 0.054(2) 0.0380(19) -0.0249(17) -0.0051(14) -0.0071(16) C16 0.0266(18) 0.050(2) 0.0371(18) -0.0197(16) -0.0024(15) -0.0121(16) C17 0.0334(19) 0.049(2) 0.0342(18) -0.0213(16) -0.0024(15) -0.0093(16) C18 0.0334(19) 0.059(2) 0.0375(19) -0.0178(17) 0.0054(15) -0.0091(18) C19 0.043(2) 0.048(2) 0.047(2) -0.0080(17) -0.0005(17) -0.0127(17) C20 0.038(2) 0.044(2) 0.050(2) -0.0198(17) -0.0093(17) -0.0001(17) C21 0.043(2) 0.058(2) 0.053(2) -0.0352(18) 0.0072(17) -0.0138(17) C22 0.043(2) 0.037(2) 0.047(2) -0.0209(16) 0.0116(16) -0.0093(16) C23 0.040(2) 0.0311(18) 0.048(2) -0.0164(16) 0.0036(17) 0.0001(16) C24 0.0380(19) 0.0365(19) 0.0371(18) -0.0113(15) 0.0072(16) 0.0003(15) C25 0.057(2) 0.037(2) 0.047(2) -0.0098(17) 0.0071(17) 0.0019(18) C26 0.074(3) 0.032(2) 0.064(3) -0.0144(19) 0.015(2) 0.000(2) C27 0.062(3) 0.045(2) 0.067(3) -0.030(2) 0.014(2) -0.017(2) C28 0.0363(19) 0.050(2) 0.049(2) -0.0191(17) -0.0031(16) 0.0029(16) C29 0.048(2) 0.043(2) 0.047(2) -0.0128(16) -0.0033(17) -0.0143(17) C30 0.042(2) 0.0402(19) 0.049(2) -0.0098(16) 0.0020(17) -0.0072(16) C31 0.038(2) 0.047(2) 0.042(2) -0.0050(16) -0.0097(16) -0.0059(16) C32 0.0336(19) 0.053(2) 0.047(2) -0.0134(17) -0.0067(16) -0.0126(17) C33 0.0259(18) 0.0391(19) 0.0356(18) -0.0137(15) 0.0063(15) -0.0081(15) C34 0.0343(19) 0.0369(19) 0.0394(18) -0.0164(15) 0.0055(15) -0.0139(16) C35 0.0318(19) 0.051(2) 0.046(2) -0.0157(17) -0.0025(16) -0.0127(17) C36 0.035(2) 0.042(2) 0.051(2) -0.0121(17) 0.0069(17) -0.0074(16) C37 0.041(2) 0.048(2) 0.046(2) -0.0249(17) 0.0163(17) -0.0156(18) C38 0.036(2) 0.051(2) 0.0367(19) -0.0203(16) 0.0040(15) -0.0142(17) C39 0.069(3) 0.048(2) 0.044(2) -0.0202(17) 0.0118(19) -0.0168(19) C51 0.0290(18) 0.060(2) 0.048(2) -0.0302(19) 0.0082(16) -0.0168(17) C52 0.0295(18) 0.047(2) 0.044(2) -0.0173(17) 0.0113(15) -0.0113(16) C53 0.039(2) 0.057(2) 0.070(3) -0.031(2) 0.017(2) -0.0167(18) C54 0.044(2) 0.087(3) 0.098(3) -0.063(3) 0.016(2) -0.026(2) C55 0.033(2) 0.103(3) 0.073(3) -0.055(3) -0.0007(19) -0.011(2) C56 0.033(2) 0.073(3) 0.050(2) -0.035(2) 0.0025(17) -0.0033(19) C57 0.044(2) 0.0433(19) 0.0364(19) -0.0076(15) 0.0073(16) -0.0089(16) C58 0.0346(18) 0.0298(17) 0.0340(18) -0.0108(14) 0.0011(15) -0.0100(14) C59 0.0309(19) 0.0302(17) 0.0317(18) -0.0062(14) 0.0006(14) -0.0051(14) C60 0.0314(18) 0.0239(16) 0.0304(17) -0.0077(13) -0.0007(15) -0.0026(13) C61 0.0292(18) 0.0356(18) 0.042(2) -0.0140(15) -0.0014(16) -0.0059(14) C62 0.041(2) 0.0383(18) 0.0369(19) -0.0155(15) -0.0053(16) -0.0088(15) C63 0.049(2) 0.0421(19) 0.0315(18) -0.0167(15) 0.0043(17) -0.0104(16) C64 0.0330(18) 0.048(2) 0.0355(19) -0.0085(15) 0.0026(15) -0.0031(15) C65 0.0287(17) 0.0376(19) 0.0285(17) -0.0107(15) 0.0046(14) -0.0054(15) C66 0.0349(18) 0.0343(18) 0.0318(17) -0.0141(15) 0.0071(15) -0.0135(15) C67 0.0335(18) 0.042(2) 0.0296(17) -0.0103(15) 0.0004(15) -0.0102(15) C68 0.043(2) 0.055(2) 0.0349(19) -0.0187(17) -0.0039(15) -0.0144(18) C69 0.057(2) 0.049(2) 0.044(2) -0.0262(18) 0.0068(18) -0.0243(18) C70 0.051(2) 0.0332(18) 0.0373(19) -0.0128(15) 0.0111(17) -0.0092(16) C71 0.045(2) 0.050(2) 0.046(2) -0.0008(17) -0.0078(17) -0.0108(17) C72 0.052(2) 0.037(2) 0.041(2) -0.0040(16) -0.0235(18) -0.0026(17) C73 0.049(2) 0.041(2) 0.051(2) -0.0222(18) -0.0191(18) 0.0070(18) C74 0.059(2) 0.051(2) 0.047(2) -0.0218(19) -0.0279(19) 0.0183(19) C75 0.125(4) 0.054(3) 0.045(3) -0.021(2) -0.038(3) 0.034(3) C76 0.178(5) 0.039(2) 0.047(3) -0.012(2) -0.044(3) 0.004(3) C77 0.099(3) 0.044(2) 0.046(2) -0.001(2) -0.031(2) -0.016(2) C78 0.046(2) 0.091(3) 0.059(2) -0.043(2) -0.013(2) 0.018(2) C79 0.048(2) 0.058(2) 0.045(2) -0.0118(18) -0.0035(17) -0.0074(19) C80 0.055(2) 0.037(2) 0.063(2) -0.0134(18) -0.0155(19) -0.0046(17) C81 0.040(2) 0.0345(18) 0.0447(19) -0.0186(16) 0.0050(16) -0.0096(15) C82 0.0348(19) 0.044(2) 0.0432(19) -0.0196(16) 0.0074(16) -0.0123(16) C83 0.0351(19) 0.0331(18) 0.0296(18) -0.0079(15) -0.0005(15) -0.0145(15) C84 0.0274(18) 0.0318(18) 0.0354(18) -0.0126(15) -0.0031(15) -0.0068(15) C85 0.039(2) 0.0425(19) 0.0293(18) -0.0131(16) -0.0024(15) -0.0128(16) C86 0.042(2) 0.0344(18) 0.0322(18) -0.0061(14) -0.0100(16) -0.0111(16) C87 0.0351(19) 0.041(2) 0.044(2) -0.0137(17) -0.0086(16) -0.0021(15) C88 0.0313(19) 0.045(2) 0.0365(19) -0.0145(16) 0.0015(15) -0.0088(16) C89 0.069(2) 0.044(2) 0.042(2) -0.0027(16) -0.0181(18) -0.0257(18) C92 0.0414(19) 0.0401(19) 0.0391(19) -0.0129(15) -0.0017(15) -0.0154(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.396(3) . ? O1 C29 1.426(3) . ? O2 C30 1.411(3) . ? O2 C31 1.416(3) . ? O3 C33 1.369(3) . ? O3 C32 1.437(3) . ? O4 C34 1.379(3) . ? O4 C39 1.424(3) . ? O7 C51 1.396(3) . ? O7 C79 1.416(4) . ? O8 C80 1.407(3) . ? O8 C81 1.418(3) . ? O9 C84 1.370(3) . ? O9 C82 1.432(3) . ? O10 C83 1.384(3) . ? O10 C89 1.434(3) . ? O12 C66 1.388(3) . ? O12 C92 1.430(3) . ? C40 O5 1.457(4) . ? C40 C39 1.515(4) . ? C40 O5A 1.566(10) . ? O5 C41 1.403(5) . ? C41 C42 1.516(6) . ? C42 O6 1.449(4) . ? O6 C16 1.387(3) . ? O6 C42A 1.479(11) . ? O5A C41A 1.454(13) . ? C41A C42A 1.528(14) . ? C90 O11 1.487(5) . ? C90 C89 1.509(4) . ? C90 O11A 1.644(6) . ? O11 C91 1.355(4) . ? C91 O11A 1.247(5) . ? C91 C92 1.493(4) . ? C1 C2 1.391(4) . ? C1 C6 1.395(4) . ? C2 C3 1.389(4) . ? C2 C7 1.509(4) . ? C3 C4 1.381(4) . ? C4 C5 1.375(4) . ? C5 C6 1.388(4) . ? C6 C28 1.503(4) . ? C7 C8 1.525(4) . ? C8 C9 1.385(4) . ? C8 C13 1.386(4) . ? C9 C10 1.389(4) . ? C10 C11 1.394(4) . ? C10 C14 1.520(4) . ? C11 C12 1.377(4) . ? C12 C13 1.379(4) . ? C14 C15 1.513(4) . ? C15 C20 1.382(4) . ? C15 C16 1.392(4) . ? C16 C17 1.392(4) . ? C17 C18 1.388(4) . ? C17 C21 1.515(4) . ? C18 C19 1.373(4) . ? C19 C20 1.383(4) . ? C21 C22 1.520(4) . ? C22 C27 1.382(4) . ? C22 C23 1.392(4) . ? C23 C24 1.385(4) . ? C24 C25 1.381(4) . ? C24 C28 1.517(4) . ? C25 C26 1.373(5) . ? C26 C27 1.380(5) . ? C29 C30 1.494(4) . ? C31 C32 1.496(4) . ? C33 C38 1.370(4) . ? C33 C34 1.393(4) . ? C34 C35 1.371(4) . ? C35 C36 1.379(4) . ? C36 C37 1.370(4) . ? C37 C38 1.377(4) . ? C51 C52 1.386(4) . ? C51 C56 1.397(4) . ? C52 C53 1.382(4) . ? C52 C57 1.501(4) . ? C53 C54 1.374(5) . ? C54 C55 1.372(5) . ? C55 C56 1.393(5) . ? C56 C78 1.500(5) . ? C57 C58 1.525(4) . ? C58 C59 1.386(4) . ? C58 C63 1.386(4) . ? C59 C60 1.392(4) . ? C60 C61 1.385(4) . ? C60 C64 1.518(4) . ? C61 C62 1.375(4) . ? C62 C63 1.375(4) . ? C64 C65 1.498(4) . ? C65 C70 1.391(4) . ? C65 C66 1.391(4) . ? C66 C67 1.405(4) . ? C67 C68 1.379(4) . ? C67 C71 1.501(4) . ? C68 C69 1.375(4) . ? C69 C70 1.366(4) . ? C71 C72 1.505(4) . ? C72 C77 1.385(5) . ? C72 C73 1.387(4) . ? C73 C74 1.398(4) . ? C74 C75 1.393(5) . ? C74 C78 1.516(5) . ? C75 C76 1.364(6) . ? C76 C77 1.381(6) . ? C79 C80 1.510(4) . ? C81 C82 1.491(4) . ? C83 C88 1.373(4) . ? C83 C84 1.392(4) . ? C84 C85 1.387(4) . ? C85 C86 1.386(4) . ? C86 C87 1.369(4) . ? C87 C88 1.386(4) . ? 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 C1 O1 C29 115.9(2) . . ? C30 O2 C31 112.6(2) . . ? C33 O3 C32 117.8(2) . . ? C34 O4 C39 114.5(2) . . ? C51 O7 C79 116.4(2) . . ? C80 O8 C81 113.5(2) . . ? C84 O9 C82 118.3(2) . . ? C83 O10 C89 116.0(2) . . ? C66 O12 C92 113.3(2) . . ? O5 C40 C39 109.5(3) . . ? O5 C40 O5A 50.7(4) . . ? C39 C40 O5A 116.5(5) . . ? C41 O5 C40 107.2(3) . . ? O5 C41 C42 109.6(4) . . ? O6 C42 C41 111.3(4) . . ? C16 O6 C42 120.6(3) . . ? C16 O6 C42A 103.2(5) . . ? C42 O6 C42A 41.4(5) . . ? C41A O5A C40 104.7(10) . . ? O5A C41A C42A 102.7(11) . . ? O6 C42A C41A 97.8(8) . . ? O11 C90 C89 114.7(3) . . ? O11 C90 O11A 61.5(3) . . ? C89 C90 O11A 102.7(3) . . ? C91 O11 C90 111.2(4) . . ? O11A C91 O11 76.1(3) . . ? O11A C91 C92 121.4(4) . . ? O11 C91 C92 111.7(3) . . ? C91 O11A C90 107.7(4) . . ? C2 C1 C6 122.3(3) . . ? C2 C1 O1 118.0(3) . . ? C6 C1 O1 119.6(2) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C7 120.2(3) . . ? C1 C2 C7 122.1(3) . . ? C4 C3 C2 121.2(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C28 121.0(3) . . ? C1 C6 C28 121.3(3) . . ? C2 C7 C8 114.3(2) . . ? C9 C8 C13 118.4(3) . . ? C9 C8 C7 122.4(3) . . ? C13 C8 C7 119.2(3) . . ? C8 C9 C10 121.9(3) . . ? C9 C10 C11 118.3(3) . . ? C9 C10 C14 122.3(3) . . ? C11 C10 C14 119.3(3) . . ? C12 C11 C10 120.4(3) . . ? C11 C12 C13 120.3(3) . . ? C12 C13 C8 120.7(3) . . ? C15 C14 C10 114.4(2) . . ? C20 C15 C16 118.2(3) . . ? C20 C15 C14 119.2(3) . . ? C16 C15 C14 122.5(3) . . ? O6 C16 C17 120.8(3) . . ? O6 C16 C15 117.5(3) . . ? C17 C16 C15 121.5(3) . . ? C18 C17 C16 118.1(3) . . ? C18 C17 C21 118.6(3) . . ? C16 C17 C21 123.2(3) . . ? C19 C18 C17 121.4(3) . . ? C18 C19 C20 119.3(3) . . ? C19 C20 C15 121.3(3) . . ? C17 C21 C22 114.4(2) . . ? C27 C22 C23 118.1(3) . . ? C27 C22 C21 120.0(3) . . ? C23 C22 C21 122.0(3) . . ? C24 C23 C22 121.7(3) . . ? C25 C24 C23 118.5(3) . . ? C25 C24 C28 119.4(3) . . ? C23 C24 C28 122.1(3) . . ? C26 C25 C24 121.0(3) . . ? C25 C26 C27 119.8(3) . . ? C26 C27 C22 121.0(3) . . ? C6 C28 C24 115.3(3) . . ? O1 C29 C30 108.7(2) . . ? O2 C30 C29 108.6(2) . . ? O2 C31 C32 109.1(2) . . ? O3 C32 C31 107.2(2) . . ? O3 C33 C38 125.6(3) . . ? O3 C33 C34 114.8(3) . . ? C38 C33 C34 119.6(3) . . ? C35 C34 O4 120.4(3) . . ? C35 C34 C33 120.0(3) . . ? O4 C34 C33 119.5(3) . . ? C34 C35 C36 120.3(3) . . ? C37 C36 C35 119.5(3) . . ? C36 C37 C38 120.8(3) . . ? C33 C38 C37 119.9(3) . . ? O4 C39 C40 106.5(3) . . ? C52 C51 O7 119.3(3) . . ? C52 C51 C56 122.1(3) . . ? O7 C51 C56 118.4(3) . . ? C53 C52 C51 118.2(3) . . ? C53 C52 C57 120.2(3) . . ? C51 C52 C57 121.7(3) . . ? C54 C53 C52 121.5(3) . . ? C55 C54 C53 119.2(3) . . ? C54 C55 C56 121.9(3) . . ? C55 C56 C51 117.0(3) . . ? C55 C56 C78 121.4(3) . . ? C51 C56 C78 121.5(3) . . ? C52 C57 C58 114.8(2) . . ? C59 C58 C63 118.2(3) . . ? C59 C58 C57 123.3(3) . . ? C63 C58 C57 118.6(3) . . ? C58 C59 C60 122.1(3) . . ? C61 C60 C59 118.1(3) . . ? C61 C60 C64 119.2(3) . . ? C59 C60 C64 122.7(3) . . ? C62 C61 C60 120.6(3) . . ? C63 C62 C61 120.6(3) . . ? C62 C63 C58 120.6(3) . . ? C65 C64 C60 115.4(2) . . ? C70 C65 C66 117.4(3) . . ? C70 C65 C64 120.5(3) . . ? C66 C65 C64 122.1(3) . . ? O12 C66 C65 119.9(3) . . ? O12 C66 C67 117.8(2) . . ? C65 C66 C67 122.3(3) . . ? C68 C67 C66 117.1(3) . . ? C68 C67 C71 121.0(3) . . ? C66 C67 C71 121.9(3) . . ? C69 C68 C67 121.8(3) . . ? C70 C69 C68 119.8(3) . . ? C69 C70 C65 121.6(3) . . ? C67 C71 C72 114.4(3) . . ? C77 C72 C73 118.1(3) . . ? C77 C72 C71 121.1(3) . . ? C73 C72 C71 120.9(3) . . ? C72 C73 C74 122.4(3) . . ? C75 C74 C73 117.6(4) . . ? C75 C74 C78 120.6(4) . . ? C73 C74 C78 121.8(3) . . ? C76 C75 C74 120.5(4) . . ? C75 C76 C77 121.3(4) . . ? C76 C77 C72 120.2(4) . . ? C56 C78 C74 113.1(3) . . ? O7 C79 C80 108.7(3) . . ? O8 C80 C79 108.1(3) . . ? O8 C81 C82 108.0(2) . . ? O9 C82 C81 107.2(2) . . ? C88 C83 O10 119.7(3) . . ? C88 C83 C84 120.2(3) . . ? O10 C83 C84 120.0(3) . . ? O9 C84 C85 124.8(3) . . ? O9 C84 C83 115.6(2) . . ? C85 C84 C83 119.6(3) . . ? C86 C85 C84 119.6(3) . . ? C87 C86 C85 120.5(3) . . ? C86 C87 C88 120.1(3) . . ? C83 C88 C87 120.0(3) . . ? O10 C89 C90 105.0(2) . . ? O12 C92 C91 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.26 _refine_diff_density_min -0.22 _refine_diff_density_rms 0.04