# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Maija Nissinen' _publ_contact_author_address ;University of Jyvaskyla, Department of Chemistry, Nanoscience Center, P.O.Box 35, FIN-40014, University of Jyvaskyla, Finland ; _publ_contact_author_email majoni@cc.jyu.fi _publ_contact_author_phone '+358 14 260 4242' _publ_contact_author_fax '+358 14 260 4756' _publ_section_title ; Pyrogallarenes as alkali metal receptors: The role of cation-pi interactions for complexation ; loop_ _publ_author_name _publ_author_address M.Nissinen ;University of Jyvaskyla, Department of Chemistry, Nanoscience Center, P.O.Box 35, FIN-40014, University of Jyvaskyla, Finland ; A.Ahman ;University of Jyvaskyla, Department of Chemistry, Nanoscience Center, P.O.Box 35, FIN-40014, University of Jyvaskyla, Finland ; data_ocs080pc1z _database_code_depnum_ccdc_archive 'CCDC 288486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C32 H32 O12),Br, K, 5(C H4 O)' _chemical_formula_sum 'C37 H52 Br K O17' _chemical_formula_weight 887.80 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1714(6) _cell_length_b 16.3264(8) _cell_length_c 18.3847(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.276(3) _cell_angle_gamma 90.00 _cell_volume 3947.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7921 _exptl_absorpt_correction_T_max 0.8875 _exptl_absorpt_process_details ; 'Blessin, R. H. Acta Crystallogr., Sect A 1995, 51, 33-38' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _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 ? _diffrn_measurement_method ; 'Nonius Kappa CCD with Apex II detector' ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18719 _diffrn_reflns_av_R_equivalents 0.1044 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.57 _reflns_number_total 7308 _reflns_number_gt 4092 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0001P)^2^+29.2344P] 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 7308 _refine_ls_number_parameters 525 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1728 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0000(5) 0.0033(4) 0.2705(4) 0.0190(16) Uani 1 1 d . . . C2 C -0.0459(5) 0.0778(4) 0.2481(3) 0.0178(14) Uani 1 1 d . . . H2 H -0.1074 0.0763 0.2185 0.021 Uiso 1 1 calc R . . C3 C -0.0048(5) 0.1525(4) 0.2676(4) 0.0179(16) Uani 1 1 d . . . C4 C 0.0841(5) 0.1546(4) 0.3114(4) 0.0184(16) Uani 1 1 d . . . C5 C 0.1321(5) 0.0825(5) 0.3351(3) 0.0221(15) Uani 1 1 d . . . C6 C 0.0906(5) 0.0076(4) 0.3136(4) 0.0191(16) Uani 1 1 d . . . C7 C -0.0514(5) 0.2351(4) 0.2429(4) 0.0223(16) Uani 1 1 d . . . H7 H -0.0555 0.2697 0.2875 0.027 Uiso 1 1 calc R . . C8 C 0.0171(5) 0.2797(4) 0.1923(4) 0.0217(17) Uani 1 1 d . . . C9 C 0.0753(5) 0.2401(4) 0.1424(4) 0.0177(15) Uani 1 1 d . . . H9 H 0.0722 0.1820 0.1401 0.021 Uiso 1 1 calc R . . C10 C 0.1375(5) 0.2803(4) 0.0960(4) 0.0189(16) Uani 1 1 d . . . C11 C 0.1426(5) 0.3659(4) 0.1005(4) 0.0172(15) Uani 1 1 d . . . C12 C 0.0878(5) 0.4069(4) 0.1510(4) 0.0183(16) Uani 1 1 d . . . C13 C 0.0238(5) 0.3663(4) 0.1964(4) 0.0187(16) Uani 1 1 d . . . C14 C 0.1998(5) 0.2352(4) 0.0416(4) 0.0200(16) Uani 1 1 d . . . H14 H 0.2620 0.2686 0.0343 0.024 Uiso 1 1 calc R . . C15 C 0.2351(5) 0.1515(4) 0.0710(4) 0.0188(16) Uani 1 1 d . . . C16 C 0.1977(5) 0.0777(4) 0.0452(3) 0.0182(14) Uani 1 1 d . . . H16 H 0.1453 0.0785 0.0074 0.022 Uiso 1 1 calc R . . C17 C 0.2322(5) 0.0019(4) 0.0712(4) 0.0180(16) Uani 1 1 d . . . C18 C 0.3081(5) 0.0030(4) 0.1281(4) 0.0202(16) Uani 1 1 d . . . C19 C 0.3465(5) 0.0749(4) 0.1555(3) 0.0184(11) Uani 1 1 d . . . C20 C 0.3117(5) 0.1493(4) 0.1265(4) 0.0189(16) Uani 1 1 d . . . C21 C 0.1934(5) -0.0796(5) 0.0418(3) 0.0194(15) Uani 1 1 d . . . H21 H 0.2545 -0.1136 0.0327 0.023 Uiso 1 1 calc R . . C22 C 0.1325(5) -0.1267(4) 0.0968(4) 0.0174(16) Uani 1 1 d . . . C23 C 0.0760(5) -0.0867(4) 0.1474(3) 0.0187(15) Uani 1 1 d . . . H23 H 0.0765 -0.0285 0.1476 0.022 Uiso 1 1 calc R . . C24 C 0.0188(5) -0.1264(4) 0.1976(4) 0.0141(15) Uani 1 1 d . . . C25 C 0.0178(5) -0.2122(4) 0.1956(4) 0.0179(16) Uani 1 1 d . . . C26 C 0.0712(5) -0.2544(4) 0.1451(4) 0.0184(11) Uani 1 1 d . . . C27 C 0.1301(5) -0.2131(4) 0.0957(4) 0.0207(16) Uani 1 1 d . . . C28 C -0.0438(5) -0.0812(4) 0.2512(3) 0.0182(14) Uani 1 1 d . . . H28 H -0.0404 -0.1141 0.2972 0.022 Uiso 1 1 calc R . . C29 C -0.1583(5) 0.2312(5) 0.2064(4) 0.0274(18) Uani 1 1 d . . . H29A H -0.1832 0.2868 0.1964 0.041 Uiso 1 1 calc R . . H29B H -0.2038 0.2033 0.2387 0.041 Uiso 1 1 calc R . . H29C H -0.1565 0.2008 0.1605 0.041 Uiso 1 1 calc R . . C30 C 0.1384(6) 0.2301(5) -0.0326(4) 0.0257(17) Uani 1 1 d . . . H30A H 0.1792 0.2023 -0.0681 0.039 Uiso 1 1 calc R . . H30B H 0.1216 0.2855 -0.0499 0.039 Uiso 1 1 calc R . . H30C H 0.0755 0.1993 -0.0268 0.039 Uiso 1 1 calc R . . C31 C 0.1291(5) -0.0750(5) -0.0308(3) 0.0269(16) Uani 1 1 d . . . H31A H 0.0662 -0.0448 -0.0236 0.040 Uiso 1 1 calc R . . H31B H 0.1125 -0.1306 -0.0479 0.040 Uiso 1 1 calc R . . H31C H 0.1678 -0.0467 -0.0673 0.040 Uiso 1 1 calc R . . C32 C -0.1555(5) -0.0798(5) 0.2232(4) 0.0294(17) Uani 1 1 d . . . H32A H -0.1959 -0.0508 0.2582 0.044 Uiso 1 1 calc R . . H32B H -0.1806 -0.1361 0.2174 0.044 Uiso 1 1 calc R . . H32C H -0.1617 -0.0516 0.1761 0.044 Uiso 1 1 calc R . . O4 O 0.1331(4) 0.2272(3) 0.3333(3) 0.0242(12) Uani 1 1 d D . . H4 H 0.0919 0.2580 0.3533 0.036 Uiso 1 1 calc RD . . O5 O 0.2186(4) 0.0834(3) 0.3806(3) 0.0279(11) Uani 1 1 d . . . H5 H 0.2417 0.1314 0.3836 0.042 Uiso 1 1 calc R . . O6 O 0.1385(4) -0.0650(3) 0.3356(3) 0.0256(12) Uani 1 1 d . . . H6 H 0.1814 -0.0554 0.3700 0.038 Uiso 1 1 calc R . . O11 O 0.2043(4) 0.4150(3) 0.0613(2) 0.0230(11) Uani 1 1 d . . . H11 H 0.2214 0.3896 0.0242 0.035 Uiso 1 1 calc R . . O12 O 0.0967(4) 0.4906(3) 0.1606(3) 0.0328(13) Uani 1 1 d . . . H12 H 0.1286 0.5108 0.1266 0.049 Uiso 1 1 calc R . . O13 O -0.0279(4) 0.4077(3) 0.2479(3) 0.0288(13) Uani 1 1 d . . . H13 H -0.0456 0.4539 0.2315 0.043 Uiso 1 1 calc R . . O18 O 0.3421(3) -0.0717(3) 0.1578(3) 0.0244(11) Uani 1 1 d . . . H18 H 0.4047 -0.0687 0.1690 0.037 Uiso 1 1 calc R . . O19 O 0.4269(3) 0.0770(3) 0.2075(2) 0.0282(11) Uani 1 1 d . . . H19 H 0.4068 0.0614 0.2477 0.042 Uiso 1 1 calc R . . O20 O 0.3535(4) 0.2216(3) 0.1537(3) 0.0230(11) Uani 1 1 d . . . H20 H 0.4014 0.2109 0.1844 0.034 Uiso 1 1 calc R . . O25 O -0.0334(4) -0.2536(3) 0.2474(3) 0.0226(12) Uani 1 1 d . . . H25 H -0.0763 -0.2852 0.2267 0.034 Uiso 1 1 calc R . . O26 O 0.0706(4) -0.3386(3) 0.1425(3) 0.0270(12) Uani 1 1 d . . . H26 H 0.0137 -0.3560 0.1541 0.041 Uiso 1 1 calc R . . O27 O 0.1808(4) -0.2622(3) 0.0497(3) 0.0259(12) Uani 1 1 d . . . H27 H 0.2236 -0.2341 0.0285 0.039 Uiso 1 1 calc R . . Br1 Br -0.15216(6) -0.42223(5) 0.19811(4) 0.0328(2) Uani 1 1 d . . . K2 K 0.25490(13) 0.32236(10) 0.25025(10) 0.0236(3) Uani 1 1 d . . . O50 O 0.3023(5) 0.3836(4) -0.0567(3) 0.0519(17) Uani 1 1 d . . . H50 H 0.2690 0.3888 -0.0968 0.078 Uiso 1 1 calc R . . C50 C 0.3868(7) 0.4390(6) -0.0539(5) 0.057(3) Uani 1 1 d . . . H50A H 0.3620 0.4951 -0.0610 0.085 Uiso 1 1 calc R . . H50B H 0.4323 0.4251 -0.0924 0.085 Uiso 1 1 calc R . . H50C H 0.4239 0.4346 -0.0063 0.085 Uiso 1 1 calc R . . O51 O 0.3374(5) -0.2232(4) -0.0388(3) 0.0499(17) Uani 1 1 d . . . H51 H 0.3510 -0.1830 -0.0650 0.075 Uiso 1 1 calc R . . C51 C 0.3767(8) -0.2967(6) -0.0698(6) 0.064(3) Uani 1 1 d . . . H51A H 0.4489 -0.2893 -0.0781 0.096 Uiso 1 1 calc R . . H51B H 0.3392 -0.3084 -0.1162 0.096 Uiso 1 1 calc R . . H51C H 0.3687 -0.3425 -0.0361 0.096 Uiso 1 1 calc R . . O52 O 0.0639(5) -0.4301(4) 0.0163(4) 0.0631(18) Uani 1 1 d D . . H52 H 0.0374 -0.4769 0.0153 0.095 Uiso 0.50 1 calc PR A 1 H52D H 0.0325 -0.3856 0.0197 0.095 Uiso 0.50 1 calc PRD A 2 C52 C 0.1314(6) -0.4241(6) -0.0381(4) 0.040(2) Uani 1 1 d . . . H52A H 0.1136 -0.3767 -0.0690 0.060 Uiso 1 1 calc R . . H52B H 0.1280 -0.4740 -0.0678 0.060 Uiso 1 1 calc R . . H52C H 0.2005 -0.4173 -0.0163 0.060 Uiso 1 1 calc R . . O53 O 0.3520(6) -0.0947(4) -0.1241(3) 0.070(2) Uani 1 1 d . . . H53 H 0.3566 -0.0931 -0.1694 0.105 Uiso 1 1 calc R . . C53 C 0.3985(9) -0.0255(7) -0.0925(6) 0.067(3) Uani 1 1 d . . . H53A H 0.3623 -0.0091 -0.0497 0.100 Uiso 1 1 calc R . . H53B H 0.3965 0.0194 -0.1280 0.100 Uiso 1 1 calc R . . H53C H 0.4694 -0.0382 -0.0776 0.100 Uiso 1 1 calc R . . O54 O 0.0247(5) 0.3170(5) 0.4232(4) 0.070(2) Uani 1 1 d D . . H54 H 0.0642 0.3068 0.4596 0.105 Uiso 1 1 calc RD . . C54 C -0.0734(8) 0.3074(8) 0.4414(7) 0.087(4) Uani 1 1 d . . . H54A H -0.0841 0.3377 0.4863 0.131 Uiso 1 1 calc RD . . H54B H -0.0872 0.2491 0.4490 0.131 Uiso 1 1 calc R . . H54C H -0.1194 0.3284 0.4020 0.131 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 0.018(4) 0.023(4) 0.016(4) -0.003(3) 0.009(3) -0.006(3) C2 0.015(3) 0.015(3) 0.024(3) -0.002(4) 0.001(3) 0.000(3) C3 0.022(4) 0.016(4) 0.017(4) -0.003(3) 0.005(3) 0.001(3) C4 0.021(4) 0.016(4) 0.018(4) -0.008(3) 0.001(3) -0.006(3) C5 0.017(4) 0.030(4) 0.018(3) -0.002(4) -0.003(3) 0.000(4) C6 0.024(4) 0.012(4) 0.022(4) -0.003(3) 0.006(3) 0.000(3) C7 0.017(4) 0.017(4) 0.033(4) -0.001(3) 0.002(3) -0.003(3) C8 0.021(4) 0.023(4) 0.021(4) 0.002(3) -0.005(3) 0.000(3) C9 0.015(4) 0.018(4) 0.020(4) -0.003(3) -0.002(3) 0.002(3) C10 0.015(4) 0.018(4) 0.023(4) 0.003(3) 0.000(3) 0.003(3) C11 0.018(4) 0.015(4) 0.019(4) 0.001(3) 0.002(3) -0.001(3) C12 0.012(3) 0.016(4) 0.026(4) 0.003(3) -0.002(3) 0.003(3) C13 0.019(4) 0.020(4) 0.017(4) -0.005(3) -0.002(3) 0.005(3) C14 0.020(4) 0.015(4) 0.026(4) 0.001(3) 0.003(3) -0.001(3) C15 0.023(4) 0.016(4) 0.018(4) 0.001(3) 0.007(3) 0.005(3) C16 0.016(3) 0.020(4) 0.018(3) -0.005(4) -0.003(3) -0.001(3) C17 0.020(4) 0.017(4) 0.016(4) -0.002(3) 0.004(3) 0.000(3) C18 0.023(4) 0.014(4) 0.025(4) 0.008(3) 0.010(3) -0.002(3) C19 0.023(3) 0.010(2) 0.022(3) -0.002(2) -0.003(2) 0.000(2) C20 0.021(4) 0.016(4) 0.020(4) -0.002(3) 0.006(3) -0.005(3) C21 0.022(4) 0.017(3) 0.019(3) 0.000(4) 0.006(3) -0.006(4) C22 0.021(4) 0.013(4) 0.017(4) -0.002(3) -0.005(3) 0.003(3) C23 0.027(4) 0.007(3) 0.022(4) -0.001(3) -0.001(3) 0.002(3) C24 0.014(4) 0.013(4) 0.015(3) -0.002(3) -0.002(3) 0.003(3) C25 0.013(4) 0.018(4) 0.023(4) -0.002(3) -0.002(3) -0.005(3) C26 0.023(3) 0.010(2) 0.022(3) -0.002(2) -0.003(2) 0.000(2) C27 0.021(4) 0.023(4) 0.018(4) -0.006(3) -0.001(3) -0.007(3) C28 0.026(4) 0.010(3) 0.018(3) -0.005(3) 0.003(3) -0.001(3) C29 0.010(4) 0.038(5) 0.035(4) -0.004(4) 0.002(3) 0.006(3) C30 0.033(5) 0.020(4) 0.024(4) -0.002(4) -0.001(3) -0.002(4) C31 0.040(4) 0.019(4) 0.022(4) -0.002(4) 0.001(3) -0.007(4) C32 0.024(4) 0.024(4) 0.041(4) -0.009(4) 0.003(3) -0.003(4) O4 0.023(3) 0.018(3) 0.031(3) -0.002(2) 0.001(2) -0.003(2) O5 0.032(3) 0.019(3) 0.031(3) 0.001(3) -0.013(2) -0.003(2) O6 0.030(3) 0.018(3) 0.028(3) -0.001(2) -0.006(2) 0.009(2) O11 0.028(3) 0.019(3) 0.022(3) 0.003(2) 0.009(2) -0.002(2) O12 0.053(4) 0.012(3) 0.034(3) 0.003(2) 0.015(3) 0.000(2) O13 0.041(3) 0.016(3) 0.031(3) 0.001(2) 0.014(2) 0.006(2) O18 0.022(3) 0.019(3) 0.031(3) 0.007(3) -0.004(2) 0.004(2) O19 0.033(3) 0.022(3) 0.028(3) 0.008(3) -0.009(2) -0.004(3) O20 0.025(3) 0.020(3) 0.023(3) -0.002(2) -0.004(2) -0.002(2) O25 0.027(3) 0.017(3) 0.024(3) -0.004(2) 0.004(2) -0.008(2) O26 0.031(3) 0.016(3) 0.035(3) -0.001(2) 0.013(2) -0.002(2) O27 0.037(3) 0.016(3) 0.026(3) -0.004(2) 0.012(2) 0.000(2) Br1 0.0323(4) 0.0316(4) 0.0338(4) -0.0042(4) -0.0035(3) 0.0025(4) K2 0.0232(8) 0.0229(8) 0.0245(8) -0.0006(7) -0.0005(6) 0.0004(7) O50 0.074(5) 0.051(4) 0.030(3) 0.004(3) -0.001(3) -0.012(4) C50 0.045(6) 0.071(8) 0.057(6) -0.009(6) 0.022(5) -0.014(5) O51 0.071(5) 0.037(4) 0.044(4) 0.006(3) 0.024(3) 0.010(3) C51 0.070(8) 0.048(7) 0.076(8) -0.009(6) 0.023(6) 0.010(6) O52 0.078(5) 0.041(4) 0.072(5) -0.001(4) 0.014(4) -0.003(4) C52 0.041(5) 0.046(5) 0.033(4) 0.000(5) -0.007(4) -0.004(5) O53 0.123(6) 0.057(5) 0.032(3) -0.009(3) 0.018(4) -0.036(4) C53 0.080(8) 0.070(8) 0.053(7) -0.004(6) 0.026(6) -0.006(6) O54 0.060(5) 0.100(6) 0.052(4) -0.025(4) 0.013(4) -0.007(4) C54 0.044(7) 0.116(11) 0.105(10) -0.018(9) 0.035(7) -0.005(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 C6 1.395(9) . ? C1 C2 1.409(10) . ? C1 C28 1.531(9) . ? C2 C3 1.373(9) . ? C3 C4 1.383(9) . ? C3 C7 1.540(9) . ? C4 C5 1.394(10) . ? C4 O4 1.399(8) . ? C5 O5 1.375(7) . ? C5 C6 1.388(10) . ? C6 O6 1.391(8) . ? C7 C8 1.517(10) . ? C7 C29 1.527(9) . ? C8 C9 1.388(10) . ? C8 C13 1.418(10) . ? C8 K2 3.323(7) . ? C9 C10 1.383(9) . ? C9 K2 3.285(7) . ? C10 C11 1.401(9) . ? C10 C14 1.520(10) . ? C10 K2 3.225(7) . ? C11 O11 1.374(8) . ? C11 C12 1.379(9) . ? C11 K2 3.132(7) . ? C12 O12 1.383(8) . ? C12 C13 1.389(10) . ? C12 K2 3.101(6) . ? C13 O13 1.375(8) . ? C13 K2 3.227(7) . ? C14 C15 1.531(9) . ? C14 C30 1.549(9) . ? C15 C16 1.375(9) . ? C15 C20 1.394(10) . ? C16 C17 1.395(9) . ? C17 C18 1.405(10) . ? C17 C21 1.514(9) . ? C18 C19 1.364(9) . ? C18 O18 1.399(8) . ? C19 O19 1.386(7) . ? C19 C20 1.393(10) . ? C20 O20 1.384(8) . ? C21 C22 1.533(9) . ? C21 C31 1.541(9) . ? C22 C23 1.387(9) . ? C22 C27 1.411(10) . ? C22 K2 3.214(7) 2_545 ? C23 C24 1.386(9) . ? C23 K2 3.198(7) 2_545 ? C24 C25 1.401(9) . ? C24 C28 1.513(9) . ? C24 K2 3.190(7) 2_545 ? C25 O25 1.374(8) . ? C25 C26 1.382(10) . ? C25 K2 3.152(7) 2_545 ? C26 O26 1.375(8) . ? C26 C27 1.400(10) . ? C26 K2 3.165(7) 2_545 ? C27 O27 1.367(8) . ? C27 K2 3.187(7) 2_545 ? C28 C32 1.531(9) . ? K2 O18 2.780(5) 2 ? K2 O6 2.845(5) 2 ? K2 C25 3.152(7) 2 ? K2 C26 3.165(7) 2 ? K2 C27 3.187(7) 2 ? K2 C24 3.190(7) 2 ? K2 C23 3.198(7) 2 ? K2 C22 3.214(7) 2 ? O50 C50 1.432(10) . ? O51 C51 1.437(10) . ? O52 C52 1.379(9) . ? O53 C53 1.395(11) . ? O54 C54 1.363(11) . ? 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 117.5(6) . . ? C6 C1 C28 118.4(6) . . ? C2 C1 C28 124.1(6) . . ? C3 C2 C1 122.3(6) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 C7 123.9(6) . . ? C4 C3 C7 117.4(6) . . ? C3 C4 C5 121.0(6) . . ? C3 C4 O4 123.4(6) . . ? C5 C4 O4 115.6(6) . . ? O5 C5 C6 118.8(7) . . ? O5 C5 C4 121.8(7) . . ? C6 C5 C4 119.4(6) . . ? C5 C6 O6 120.2(6) . . ? C5 C6 C1 121.0(6) . . ? O6 C6 C1 118.8(6) . . ? C8 C7 C29 108.5(6) . . ? C8 C7 C3 111.1(6) . . ? C29 C7 C3 115.8(6) . . ? C9 C8 C13 117.7(7) . . ? C9 C8 C7 123.5(6) . . ? C13 C8 C7 118.9(6) . . ? C9 C8 K2 76.3(4) . . ? C13 C8 K2 73.7(4) . . ? C7 C8 K2 119.1(4) . . ? C10 C9 C8 123.8(7) . . ? C10 C9 K2 75.3(4) . . ? C8 C9 K2 79.4(4) . . ? C9 C10 C11 117.7(6) . . ? C9 C10 C14 122.5(6) . . ? C11 C10 C14 119.8(6) . . ? C9 C10 K2 80.2(4) . . ? C11 C10 K2 73.6(4) . . ? C14 C10 K2 115.6(4) . . ? O11 C11 C12 114.7(6) . . ? O11 C11 C10 125.3(6) . . ? C12 C11 C10 119.9(6) . . ? O11 C11 K2 109.2(4) . . ? C12 C11 K2 76.0(4) . . ? C10 C11 K2 81.0(4) . . ? C11 C12 O12 121.5(6) . . ? C11 C12 C13 122.2(6) . . ? O12 C12 C13 116.3(6) . . ? C11 C12 K2 78.5(4) . . ? O12 C12 K2 108.2(4) . . ? C13 C12 K2 82.4(4) . . ? O13 C13 C12 121.4(6) . . ? O13 C13 C8 119.7(6) . . ? C12 C13 C8 118.8(6) . . ? O13 C13 K2 113.2(4) . . ? C12 C13 K2 72.3(4) . . ? C8 C13 K2 81.3(4) . . ? C10 C14 C15 111.5(6) . . ? C10 C14 C30 109.3(6) . . ? C15 C14 C30 113.3(6) . . ? C16 C15 C20 117.5(6) . . ? C16 C15 C14 124.4(6) . . ? C20 C15 C14 118.2(6) . . ? C15 C16 C17 123.7(6) . . ? C16 C17 C18 116.7(6) . . ? C16 C17 C21 124.1(6) . . ? C18 C17 C21 119.3(6) . . ? C19 C18 O18 120.3(6) . . ? C19 C18 C17 121.2(6) . . ? O18 C18 C17 118.5(6) . . ? C18 C19 O19 121.9(6) . . ? C18 C19 C20 120.2(6) . . ? O19 C19 C20 117.6(6) . . ? O20 C20 C19 119.3(6) . . ? O20 C20 C15 120.0(6) . . ? C19 C20 C15 120.7(6) . . ? C17 C21 C22 112.6(5) . . ? C17 C21 C31 115.1(6) . . ? C22 C21 C31 108.3(5) . . ? C23 C22 C27 117.8(6) . . ? C23 C22 C21 121.9(6) . . ? C27 C22 C21 120.3(6) . . ? C23 C22 K2 76.9(4) . 2_545 ? C27 C22 K2 76.2(4) . 2_545 ? C21 C22 K2 118.3(4) . 2_545 ? C24 C23 C22 124.0(6) . . ? C24 C23 K2 77.1(4) . 2_545 ? C22 C23 K2 78.1(4) . 2_545 ? C23 C24 C25 117.1(6) . . ? C23 C24 C28 122.9(6) . . ? C25 C24 C28 120.0(6) . . ? C23 C24 K2 77.8(4) . 2_545 ? C25 C24 K2 75.7(4) . 2_545 ? C28 C24 K2 117.9(4) . 2_545 ? O25 C25 C26 120.6(6) . . ? O25 C25 C24 118.5(6) . . ? C26 C25 C24 120.8(6) . . ? O25 C25 K2 111.4(4) . 2_545 ? C26 C25 K2 77.9(4) . 2_545 ? C24 C25 K2 78.8(4) . 2_545 ? O26 C26 C25 121.3(6) . . ? O26 C26 C27 117.5(6) . . ? C25 C26 C27 121.2(6) . . ? O26 C26 K2 114.8(4) . 2_545 ? C25 C26 K2 76.8(4) . 2_545 ? C27 C26 K2 78.1(4) . 2_545 ? O27 C27 C26 115.3(6) . . ? O27 C27 C22 125.7(6) . . ? C26 C27 C22 119.1(6) . . ? O27 C27 K2 115.6(4) . 2_545 ? C26 C27 K2 76.4(4) . 2_545 ? C22 C27 K2 78.3(4) . 2_545 ? C24 C28 C32 109.8(5) . . ? C24 C28 C1 112.2(5) . . ? C32 C28 C1 114.0(6) . . ? O18 K2 O6 101.18(15) 2 2 ? O18 K2 C12 75.29(16) 2 . ? O6 K2 C12 75.06(16) 2 . ? O18 K2 C11 100.54(16) 2 . ? O6 K2 C11 65.74(16) 2 . ? C12 K2 C11 25.56(17) . . ? O18 K2 C25 112.38(17) 2 2 ? O6 K2 C25 78.49(16) 2 2 ? C12 K2 C25 153.47(19) . 2 ? C11 K2 C25 135.29(19) . 2 ? O18 K2 C26 102.61(16) 2 2 ? O6 K2 C26 103.29(17) 2 2 ? C12 K2 C26 176.89(19) . 2 ? C11 K2 C26 156.00(19) . 2 ? C25 K2 C26 25.27(17) 2 2 ? O18 K2 C27 77.53(16) 2 2 ? O6 K2 C27 112.66(17) 2 2 ? C12 K2 C27 152.74(19) . 2 ? C11 K2 C27 177.3(2) . 2 ? C25 K2 C27 44.95(18) 2 2 ? C26 K2 C27 25.47(17) 2 2 ? O18 K2 C24 96.22(16) 2 2 ? O6 K2 C24 60.98(15) 2 2 ? C12 K2 C24 132.81(18) . 2 ? C11 K2 C24 126.22(18) . 2 ? C25 K2 C24 25.51(17) 2 2 ? C26 K2 C24 44.74(17) 2 2 ? C27 K2 C24 52.56(18) 2 2 ? O18 K2 C23 71.47(16) 2 2 ? O6 K2 C23 71.17(15) 2 2 ? C12 K2 C23 125.93(18) . 2 ? C11 K2 C23 133.63(18) . 2 ? C25 K2 C23 43.96(18) 2 2 ? C26 K2 C23 50.98(17) 2 2 ? C27 K2 C23 44.08(18) 2 2 ? C24 K2 C23 25.06(17) 2 2 ? O18 K2 C22 60.77(16) 2 2 ? O6 K2 C22 95.75(16) 2 2 ? C12 K2 C22 132.57(18) . 2 ? C11 K2 C22 151.85(17) . 2 ? C25 K2 C22 52.22(18) 2 2 ? C26 K2 C22 44.65(17) 2 2 ? C27 K2 C22 25.47(17) 2 2 ? C24 K2 C22 44.97(18) 2 2 ? C23 K2 C22 24.98(17) 2 2 ? O18 K2 C10 116.95(16) 2 . ? O6 K2 C10 82.93(16) 2 . ? C12 K2 C10 44.66(17) . . ? C11 K2 C10 25.42(17) . . ? C25 K2 C10 129.68(18) 2 . ? C26 K2 C10 138.10(18) 2 . ? C27 K2 C10 157.26(18) 2 . ? C24 K2 C10 135.45(18) 2 . ? C23 K2 C10 154.02(18) 2 . ? C22 K2 C10 177.15(19) 2 . ? O18 K2 C13 65.80(15) 2 . ? O6 K2 C13 99.97(17) 2 . ? C12 K2 C13 25.26(17) . . ? C11 K2 C13 44.77(18) . . ? C25 K2 C13 177.4(2) 2 . ? C26 K2 C13 155.74(19) 2 . ? C27 K2 C13 134.82(19) 2 . ? C24 K2 C13 151.96(17) 2 . ? C23 K2 C13 133.65(18) 2 . ? C22 K2 C13 126.22(18) 2 . ? C10 K2 C13 51.78(17) . . ? 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 -0.4(9) . . . . ? C28 C1 C2 C3 179.0(7) . . . . ? C1 C2 C3 C4 -0.8(10) . . . . ? C1 C2 C3 C7 178.7(7) . . . . ? C2 C3 C4 C5 0.6(10) . . . . ? C7 C3 C4 C5 -178.9(6) . . . . ? C2 C3 C4 O4 178.8(6) . . . . ? C7 C3 C4 O4 -0.7(10) . . . . ? C3 C4 C5 O5 -177.8(6) . . . . ? O4 C4 C5 O5 3.8(9) . . . . ? C3 C4 C5 C6 0.7(10) . . . . ? O4 C4 C5 C6 -177.6(6) . . . . ? O5 C5 C6 O6 -2.7(10) . . . . ? C4 C5 C6 O6 178.8(7) . . . . ? O5 C5 C6 C1 176.6(6) . . . . ? C4 C5 C6 C1 -1.9(10) . . . . ? C2 C1 C6 C5 1.7(10) . . . . ? C28 C1 C6 C5 -177.7(6) . . . . ? C2 C1 C6 O6 -179.0(6) . . . . ? C28 C1 C6 O6 1.6(9) . . . . ? C2 C3 C7 C8 -113.2(7) . . . . ? C4 C3 C7 C8 66.2(8) . . . . ? C2 C3 C7 C29 11.1(10) . . . . ? C4 C3 C7 C29 -169.5(6) . . . . ? C29 C7 C8 C9 -93.3(8) . . . . ? C3 C7 C8 C9 35.1(9) . . . . ? C29 C7 C8 C13 87.6(8) . . . . ? C3 C7 C8 C13 -144.1(6) . . . . ? C29 C7 C8 K2 174.2(4) . . . . ? C3 C7 C8 K2 -57.5(7) . . . . ? C13 C8 C9 C10 -1.1(10) . . . . ? C7 C8 C9 C10 179.7(6) . . . . ? K2 C8 C9 C10 -64.2(6) . . . . ? C13 C8 C9 K2 63.1(6) . . . . ? C7 C8 C9 K2 -116.1(6) . . . . ? C8 C9 C10 C11 0.7(10) . . . . ? K2 C9 C10 C11 -65.5(6) . . . . ? C8 C9 C10 C14 -179.7(6) . . . . ? K2 C9 C10 C14 114.1(6) . . . . ? C8 C9 C10 K2 66.2(6) . . . . ? C9 C10 C11 O11 176.4(6) . . . . ? C14 C10 C11 O11 -3.3(10) . . . . ? K2 C10 C11 O11 107.2(7) . . . . ? C9 C10 C11 C12 1.1(10) . . . . ? C14 C10 C11 C12 -178.5(6) . . . . ? K2 C10 C11 C12 -68.1(6) . . . . ? C9 C10 C11 K2 69.2(6) . . . . ? C14 C10 C11 K2 -110.5(6) . . . . ? O11 C11 C12 O12 -0.5(9) . . . . ? C10 C11 C12 O12 175.2(6) . . . . ? K2 C11 C12 O12 104.4(6) . . . . ? O11 C11 C12 C13 -178.3(6) . . . . ? C10 C11 C12 C13 -2.6(10) . . . . ? K2 C11 C12 C13 -73.3(6) . . . . ? O11 C11 C12 K2 -105.0(5) . . . . ? C10 C11 C12 K2 70.8(6) . . . . ? C11 C12 C13 O13 178.1(6) . . . . ? O12 C12 C13 O13 0.2(10) . . . . ? K2 C12 C13 O13 106.8(6) . . . . ? C11 C12 C13 C8 2.1(10) . . . . ? O12 C12 C13 C8 -175.8(6) . . . . ? K2 C12 C13 C8 -69.1(6) . . . . ? C11 C12 C13 K2 71.2(6) . . . . ? O12 C12 C13 K2 -106.6(6) . . . . ? C9 C8 C13 O13 -176.3(6) . . . . ? C7 C8 C13 O13 2.9(10) . . . . ? K2 C8 C13 O13 -111.8(6) . . . . ? C9 C8 C13 C12 -0.3(10) . . . . ? C7 C8 C13 C12 178.9(6) . . . . ? K2 C8 C13 C12 64.2(6) . . . . ? C9 C8 C13 K2 -64.5(6) . . . . ? C7 C8 C13 K2 114.7(6) . . . . ? C9 C10 C14 C15 -32.9(9) . . . . ? C11 C10 C14 C15 146.7(6) . . . . ? K2 C10 C14 C15 61.7(6) . . . . ? C9 C10 C14 C30 93.1(8) . . . . ? C11 C10 C14 C30 -87.3(8) . . . . ? K2 C10 C14 C30 -172.3(4) . . . . ? C10 C14 C15 C16 108.9(7) . . . . ? C30 C14 C15 C16 -14.9(10) . . . . ? C10 C14 C15 C20 -72.5(8) . . . . ? C30 C14 C15 C20 163.7(6) . . . . ? C20 C15 C16 C17 -0.2(10) . . . . ? C14 C15 C16 C17 178.4(7) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C15 C16 C17 C21 -178.3(7) . . . . ? C16 C17 C18 C19 -0.8(10) . . . . ? C21 C17 C18 C19 178.9(6) . . . . ? C16 C17 C18 O18 177.6(6) . . . . ? C21 C17 C18 O18 -2.7(9) . . . . ? O18 C18 C19 O19 6.9(10) . . . . ? C17 C18 C19 O19 -174.7(6) . . . . ? O18 C18 C19 C20 -179.3(6) . . . . ? C17 C18 C19 C20 -0.9(10) . . . . ? C18 C19 C20 O20 -178.3(6) . . . . ? O19 C19 C20 O20 -4.2(9) . . . . ? C18 C19 C20 C15 2.1(10) . . . . ? O19 C19 C20 C15 176.2(6) . . . . ? C16 C15 C20 O20 178.9(6) . . . . ? C14 C15 C20 O20 0.2(10) . . . . ? C16 C15 C20 C19 -1.6(10) . . . . ? C14 C15 C20 C19 179.7(6) . . . . ? C16 C17 C21 C22 -111.8(7) . . . . ? C18 C17 C21 C22 68.5(8) . . . . ? C16 C17 C21 C31 12.9(9) . . . . ? C18 C17 C21 C31 -166.8(6) . . . . ? C17 C21 C22 C23 31.0(9) . . . . ? C31 C21 C22 C23 -97.4(8) . . . . ? C17 C21 C22 C27 -150.9(6) . . . . ? C31 C21 C22 C27 80.7(8) . . . . ? C17 C21 C22 K2 -60.8(7) . . . 2_545 ? C31 C21 C22 K2 170.8(4) . . . 2_545 ? C27 C22 C23 C24 1.1(10) . . . . ? C21 C22 C23 C24 179.3(6) . . . . ? K2 C22 C23 C24 -65.3(6) 2_545 . . . ? C27 C22 C23 K2 66.5(6) . . . 2_545 ? C21 C22 C23 K2 -115.4(6) . . . 2_545 ? C22 C23 C24 C25 -1.0(10) . . . . ? K2 C23 C24 C25 -66.8(5) 2_545 . . . ? C22 C23 C24 C28 -178.7(6) . . . . ? K2 C23 C24 C28 115.5(6) 2_545 . . . ? C22 C23 C24 K2 65.8(6) . . . 2_545 ? C23 C24 C25 O25 176.4(6) . . . . ? C28 C24 C25 O25 -5.9(9) . . . . ? K2 C24 C25 O25 108.3(6) 2_545 . . . ? C23 C24 C25 C26 -0.5(10) . . . . ? C28 C24 C25 C26 177.3(6) . . . . ? K2 C24 C25 C26 -68.5(6) 2_545 . . . ? C23 C24 C25 K2 68.0(5) . . . 2_545 ? C28 C24 C25 K2 -114.2(6) . . . 2_545 ? O25 C25 C26 O26 3.3(10) . . . . ? C24 C25 C26 O26 -179.9(6) . . . . ? K2 C25 C26 O26 111.2(6) 2_545 . . . ? O25 C25 C26 C27 -175.0(6) . . . . ? C24 C25 C26 C27 1.8(10) . . . . ? K2 C25 C26 C27 -67.1(6) 2_545 . . . ? O25 C25 C26 K2 -107.8(6) . . . 2_545 ? C24 C25 C26 K2 68.9(6) . . . 2_545 ? O26 C26 C27 O27 0.2(9) . . . . ? C25 C26 C27 O27 178.6(6) . . . . ? K2 C26 C27 O27 112.1(6) 2_545 . . . ? O26 C26 C27 C22 180.0(6) . . . . ? C25 C26 C27 C22 -1.6(10) . . . . ? K2 C26 C27 C22 -68.1(6) 2_545 . . . ? O26 C26 C27 K2 -111.9(6) . . . 2_545 ? C25 C26 C27 K2 66.5(6) . . . 2_545 ? C23 C22 C27 O27 179.9(6) . . . . ? C21 C22 C27 O27 1.8(10) . . . . ? K2 C22 C27 O27 -113.2(7) 2_545 . . . ? C23 C22 C27 C26 0.2(10) . . . . ? C21 C22 C27 C26 -178.0(6) . . . . ? K2 C22 C27 C26 67.1(6) 2_545 . . . ? C23 C22 C27 K2 -66.8(6) . . . 2_545 ? C21 C22 C27 K2 115.0(6) . . . 2_545 ? C23 C24 C28 C32 99.7(8) . . . . ? C25 C24 C28 C32 -77.9(8) . . . . ? K2 C24 C28 C32 -167.0(4) 2_545 . . . ? C23 C24 C28 C1 -28.2(9) . . . . ? C25 C24 C28 C1 154.2(6) . . . . ? K2 C24 C28 C1 65.1(6) 2_545 . . . ? C6 C1 C28 C24 -70.9(8) . . . . ? C2 C1 C28 C24 109.8(7) . . . . ? C6 C1 C28 C32 163.5(6) . . . . ? C2 C1 C28 C32 -15.8(9) . . . . ? C11 C12 K2 O18 170.8(4) . . . 2 ? O12 C12 K2 O18 51.2(4) . . . 2 ? C13 C12 K2 O18 -64.1(4) . . . 2 ? C11 C12 K2 O6 64.7(4) . . . 2 ? O12 C12 K2 O6 -54.9(4) . . . 2 ? C13 C12 K2 O6 -170.2(4) . . . 2 ? O12 C12 K2 C11 -119.6(6) . . . . ? C13 C12 K2 C11 125.1(6) . . . . ? C11 C12 K2 C25 60.0(6) . . . 2 ? O12 C12 K2 C25 -59.6(7) . . . 2 ? C13 C12 K2 C25 -174.9(5) . . . 2 ? C11 C12 K2 C27 175.3(5) . . . 2 ? O12 C12 K2 C27 55.7(6) . . . 2 ? C13 C12 K2 C27 -59.6(6) . . . 2 ? C11 C12 K2 C24 86.0(4) . . . 2 ? O12 C12 K2 C24 -33.6(5) . . . 2 ? C13 C12 K2 C24 -148.9(4) . . . 2 ? C11 C12 K2 C23 117.4(4) . . . 2 ? O12 C12 K2 C23 -2.2(5) . . . 2 ? C13 C12 K2 C23 -117.5(4) . . . 2 ? C11 C12 K2 C22 148.7(4) . . . 2 ? O12 C12 K2 C22 29.1(5) . . . 2 ? C13 C12 K2 C22 -86.2(4) . . . 2 ? C11 C12 K2 C10 -30.4(4) . . . . ? O12 C12 K2 C10 -150.0(5) . . . . ? C13 C12 K2 C10 94.7(4) . . . . ? C11 C12 K2 C13 -125.1(6) . . . . ? O12 C12 K2 C13 115.3(6) . . . . ? O11 C11 K2 O18 102.6(4) . . . 2 ? C12 C11 K2 O18 -9.1(4) . . . 2 ? C10 C11 K2 O18 -133.1(4) . . . 2 ? O11 C11 K2 O6 5.0(4) . . . 2 ? C12 C11 K2 O6 -106.7(4) . . . 2 ? C10 C11 K2 O6 129.3(4) . . . 2 ? O11 C11 K2 C12 111.7(6) . . . . ? C10 C11 K2 C12 -124.0(6) . . . . ? O11 C11 K2 C25 -35.0(5) . . . 2 ? C12 C11 K2 C25 -146.6(4) . . . 2 ? C10 C11 K2 C25 89.3(5) . . . 2 ? O11 C11 K2 C26 -61.9(6) . . . 2 ? C12 C11 K2 C26 -173.6(5) . . . 2 ? C10 C11 K2 C26 62.4(6) . . . 2 ? O11 C11 K2 C24 -3.2(5) . . . 2 ? C12 C11 K2 C24 -114.9(4) . . . 2 ? C10 C11 K2 C24 121.1(4) . . . 2 ? O11 C11 K2 C23 28.2(5) . . . 2 ? C12 C11 K2 C23 -83.4(4) . . . 2 ? C10 C11 K2 C23 152.6(4) . . . 2 ? O11 C11 K2 C22 57.5(6) . . . 2 ? C12 C11 K2 C22 -54.2(6) . . . 2 ? C10 C11 K2 C22 -178.2(5) . . . 2 ? O11 C11 K2 C10 -124.3(7) . . . . ? C12 C11 K2 C10 124.0(6) . . . . ? O11 C11 K2 C13 141.4(5) . . . . ? C12 C11 K2 C13 29.7(4) . . . . ? C10 C11 K2 C13 -94.3(5) . . . . ? C9 C10 K2 O18 -69.2(4) . . . 2 ? C11 C10 K2 O18 53.7(4) . . . 2 ? C14 C10 K2 O18 169.4(4) . . . 2 ? C9 C10 K2 O6 -168.2(4) . . . 2 ? C11 C10 K2 O6 -45.3(4) . . . 2 ? C14 C10 K2 O6 70.4(5) . . . 2 ? C9 C10 K2 C12 -92.3(4) . . . . ? C11 C10 K2 C12 30.6(4) . . . . ? C14 C10 K2 C12 146.3(6) . . . . ? C9 C10 K2 C11 -122.9(6) . . . . ? C14 C10 K2 C11 115.7(7) . . . . ? C9 C10 K2 C25 123.2(4) . . . 2 ? C11 C10 K2 C25 -113.9(4) . . . 2 ? C14 C10 K2 C25 1.8(6) . . . 2 ? C9 C10 K2 C26 89.8(5) . . . 2 ? C11 C10 K2 C26 -147.3(4) . . . 2 ? C14 C10 K2 C26 -31.6(6) . . . 2 ? C9 C10 K2 C27 56.7(7) . . . 2 ? C11 C10 K2 C27 179.6(5) . . . 2 ? C14 C10 K2 C27 -64.7(7) . . . 2 ? C9 C10 K2 C24 157.2(4) . . . 2 ? C11 C10 K2 C24 -79.9(5) . . . 2 ? C14 C10 K2 C24 35.8(6) . . . 2 ? C9 C10 K2 C23 -172.4(5) . . . 2 ? C11 C10 K2 C23 -49.6(6) . . . 2 ? C14 C10 K2 C23 66.1(7) . . . 2 ? C9 C10 K2 C13 -59.5(4) . . . . ? C11 C10 K2 C13 63.4(4) . . . . ? C14 C10 K2 C13 179.1(6) . . . . ? O13 C13 K2 O18 -9.9(4) . . . 2 ? C12 C13 K2 O18 107.5(4) . . . 2 ? C8 C13 K2 O18 -128.5(5) . . . 2 ? O13 C13 K2 O6 -107.7(5) . . . 2 ? C12 C13 K2 O6 9.6(4) . . . 2 ? C8 C13 K2 O6 133.6(4) . . . 2 ? O13 C13 K2 C12 -117.3(7) . . . . ? C8 C13 K2 C12 124.0(6) . . . . ? O13 C13 K2 C11 -147.4(6) . . . . ? C12 C13 K2 C11 -30.1(4) . . . . ? C8 C13 K2 C11 94.0(5) . . . . ? O13 C13 K2 C26 55.6(7) . . . 2 ? C8 C13 K2 C26 -63.0(6) . . . 2 ? O13 C13 K2 C27 28.9(6) . . . 2 ? C12 C13 K2 C27 146.2(4) . . . 2 ? C8 C13 K2 C27 -89.8(5) . . . 2 ? O13 C13 K2 C24 -63.6(7) . . . 2 ? C12 C13 K2 C24 53.7(6) . . . 2 ? C8 C13 K2 C24 177.8(5) . . . 2 ? O13 C13 K2 C23 -34.3(6) . . . 2 ? C12 C13 K2 C23 83.0(4) . . . 2 ? C8 C13 K2 C23 -152.9(4) . . . 2 ? O13 C13 K2 C22 -3.0(5) . . . 2 ? C12 C13 K2 C22 114.4(4) . . . 2 ? C8 C13 K2 C22 -121.6(4) . . . 2 ? O13 C13 K2 C10 179.6(6) . . . . ? C12 C13 K2 C10 -63.1(4) . . . . ? C8 C13 K2 C10 61.0(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O54 0.84 1.87 2.681(8) 162.4 . O5 H5 O4 0.84 2.28 2.725(7) 113.4 . O5 H5 O27 0.84 2.33 3.091(7) 151.1 2 O5 H5 O26 0.84 2.59 3.106(7) 120.6 2 O6 H6 O11 0.84 1.97 2.745(6) 153.4 2_545 O6 H6 O5 0.84 2.32 2.752(7) 112.1 . O11 H11 O50 0.84 1.88 2.638(8) 149.2 . O12 H12 O11 0.84 2.24 2.677(7) 112.5 . O12 H12 O5 0.84 2.35 3.001(7) 135.0 2 O12 H12 O52 0.84 2.36 2.962(8) 128.9 1_565 O13 H13 Br1 0.84 2.52 3.325(5) 161.4 1_565 O18 H18 O13 0.84 2.20 2.937(7) 146.8 2_545 O19 H19 O12 0.84 2.04 2.837(7) 157.0 2_545 O19 H19 O26 0.84 2.60 3.081(7) 117.7 2 O20 H20 O25 0.84 2.16 2.931(7) 151.7 2 O20 H20 O19 0.84 2.25 2.715(7) 115.3 . O25 H25 Br1 0.84 2.49 3.269(5) 153.9 . O26 H26 Br1 0.84 2.61 3.444(5) 173.9 . O27 H27 O51 0.84 2.01 2.774(8) 151.7 . O50 H50 Br1 0.84 2.41 3.237(6) 168.4 3 O51 H51 O53 0.84 1.81 2.633(9) 168.1 . O52 H52 O52 0.84 2.08 2.880(13) 158.2 3_545 O52 H52D O26 0.84 2.41 2.757(8) 105.5 . O53 H53 Br1 0.84 2.44 3.278(6) 172.0 4_655 O54 H54 O51 0.84 1.96 2.794(10) 174.9 2 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.674 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.109 #===END data_ocs080pc1y _database_code_depnum_ccdc_archive 'CCDC 288487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C32 H32 O12), Rb, 2.5(C H4 O), Cl, 0.5(O)' _chemical_formula_sum 'C34.50 H42 Cl O15 Rb' _chemical_formula_weight 817.60 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' Cl Cl 0.1484 0.1585 '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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2378(2) _cell_length_b 22.9315(5) _cell_length_c 17.3511(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.206(2) _cell_angle_gamma 90.00 _cell_volume 3665.70(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 1.494 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7544 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details ; 'Blessing, R. H. Acta Crystallogr., Sect A 1995, 51, 33-38' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _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 Kappa CCD with APEX II detector' ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19708 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.58 _reflns_number_total 6734 _reflns_number_gt 4590 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0334P)^2^+17.4102P] 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 6734 _refine_ls_number_parameters 505 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1852(5) 0.1350(2) 0.3758(3) 0.0200(12) Uani 1 1 d . . . C2 C 1.1603(6) 0.1075(2) 0.4458(3) 0.0205(12) Uani 1 1 d . . . H2 H 1.1418 0.0668 0.4455 0.025 Uiso 1 1 calc R . . C3 C 1.1612(5) 0.1373(2) 0.5157(3) 0.0196(11) Uani 1 1 d . . . C4 C 1.1837(6) 0.1975(2) 0.5143(3) 0.0234(12) Uani 1 1 d . . . C5 C 1.2124(6) 0.2252(2) 0.4470(3) 0.0240(12) Uani 1 1 d . . . C6 C 1.2161(6) 0.1944(2) 0.3786(3) 0.0227(12) Uani 1 1 d . . . C7 C 1.1395(6) 0.1075(2) 0.5923(3) 0.0222(12) Uani 1 1 d . . . H7 H 1.2177 0.1217 0.6305 0.027 Uiso 1 1 calc R . . C8 C 0.9953(5) 0.1225(2) 0.6237(3) 0.0183(11) Uani 1 1 d . . . C9 C 0.8658(6) 0.1222(2) 0.5769(3) 0.0221(12) Uani 1 1 d . . . H9 H 0.8706 0.1166 0.5228 0.027 Uiso 1 1 calc R . . C10 C 0.7305(6) 0.1295(2) 0.6052(3) 0.0210(12) Uani 1 1 d . . . C11 C 0.7243(6) 0.1370(2) 0.6840(3) 0.0221(12) Uani 1 1 d . . . C12 C 0.8517(6) 0.1409(2) 0.7323(3) 0.0227(12) Uani 1 1 d . . . C13 C 0.9856(6) 0.1326(2) 0.7026(3) 0.0208(12) Uani 1 1 d . . . C14 C 0.5902(6) 0.1248(2) 0.5534(3) 0.0234(12) Uani 1 1 d . . . H14 H 0.5138 0.1465 0.5796 0.028 Uiso 1 1 calc R . . C15 C 0.6023(6) 0.1532(2) 0.4747(3) 0.0217(12) Uani 1 1 d . . . C16 C 0.6112(5) 0.1227(2) 0.4058(3) 0.0195(11) Uani 1 1 d . . . H16 H 0.6154 0.0813 0.4078 0.023 Uiso 1 1 calc R . . C17 C 0.6141(5) 0.1499(2) 0.3344(3) 0.0204(12) Uani 1 1 d . . . C18 C 0.6039(6) 0.2107(2) 0.3330(3) 0.0248(13) Uani 1 1 d . . . C19 C 0.5962(7) 0.2424(2) 0.4011(3) 0.0298(14) Uani 1 1 d . . . C20 C 0.5992(6) 0.2135(2) 0.4712(3) 0.0262(13) Uani 1 1 d . . . C21 C 0.6270(6) 0.1178(2) 0.2583(3) 0.0227(12) Uani 1 1 d . . . H21 H 0.5559 0.1362 0.2193 0.027 Uiso 1 1 calc R . . C22 C 0.7778(6) 0.1255(2) 0.2288(3) 0.0205(12) Uani 1 1 d . . . C23 C 0.9050(6) 0.1168(2) 0.2754(3) 0.0226(12) Uani 1 1 d . . . H23 H 0.8972 0.1098 0.3289 0.027 Uiso 1 1 calc R . . C24 C 1.0432(6) 0.1178(2) 0.2482(3) 0.0194(11) Uani 1 1 d . . . C25 C 1.0529(6) 0.1289(2) 0.1694(3) 0.0223(12) Uani 1 1 d . . . C26 C 0.9281(6) 0.1398(2) 0.1218(3) 0.0235(12) Uani 1 1 d . . . C27 C 0.7921(6) 0.1373(2) 0.1510(3) 0.0224(12) Uani 1 1 d . . . C28 C 1.1806(6) 0.1026(2) 0.2987(3) 0.0217(12) Uani 1 1 d . . . H28 H 1.2654 0.1162 0.2709 0.026 Uiso 1 1 calc R . . C29 C 1.1505(6) 0.0405(3) 0.5899(3) 0.0310(14) Uani 1 1 d . . . H29A H 1.0714 0.0249 0.5553 0.047 Uiso 1 1 calc R . . H29B H 1.1433 0.0248 0.6420 0.047 Uiso 1 1 calc R . . H29C H 1.2439 0.0293 0.5710 0.047 Uiso 1 1 calc R . . C30 C 0.5429(6) 0.0616(2) 0.5480(3) 0.0299(14) Uani 1 1 d . . . H30A H 0.6200 0.0382 0.5275 0.045 Uiso 1 1 calc R . . H30B H 0.4544 0.0584 0.5135 0.045 Uiso 1 1 calc R . . H30C H 0.5237 0.0473 0.5995 0.045 Uiso 1 1 calc R . . C31 C 0.5904(6) 0.0532(3) 0.2609(3) 0.0305(14) Uani 1 1 d . . . H31A H 0.6613 0.0333 0.2966 0.046 Uiso 1 1 calc R . . H31B H 0.5936 0.0364 0.2091 0.046 Uiso 1 1 calc R . . H31C H 0.4929 0.0482 0.2787 0.046 Uiso 1 1 calc R . . C32 C 1.1933(6) 0.0364(2) 0.3073(3) 0.0301(13) Uani 1 1 d . . . H32A H 1.2017 0.0187 0.2564 0.045 Uiso 1 1 calc R . . H32B H 1.1068 0.0212 0.3299 0.045 Uiso 1 1 calc R . . H32C H 1.2797 0.0269 0.3412 0.045 Uiso 1 1 calc R . . O4 O 1.1766(5) 0.22818(17) 0.5821(2) 0.0316(9) Uani 1 1 d . . . H4 H 1.1879 0.2639 0.5735 0.047 Uiso 1 1 calc R . . O5 O 1.2408(5) 0.28479(16) 0.4490(2) 0.0305(9) Uani 1 1 d . . . H5 H 1.1712 0.3028 0.4260 0.046 Uiso 1 1 calc R . . O6 O 1.2469(4) 0.22265(17) 0.3107(2) 0.0325(10) Uani 1 1 d . . . H6 H 1.2709 0.2573 0.3207 0.049 Uiso 1 1 calc R . . O11 O 0.5906(4) 0.14118(19) 0.7136(2) 0.0323(10) Uani 1 1 d . . . H11 H 0.6016 0.1453 0.7618 0.048 Uiso 1 1 calc R . . O12 O 0.8363(4) 0.15322(18) 0.8091(2) 0.0297(9) Uani 1 1 d . . . H12 H 0.9184 0.1590 0.8319 0.045 Uiso 1 1 calc R . . O13 O 1.1103(4) 0.13717(17) 0.7508(2) 0.0273(9) Uani 1 1 d . . . H13 H 1.1109 0.1110 0.7847 0.041 Uiso 1 1 calc R . . O18 O 0.5982(4) 0.23871(17) 0.2628(2) 0.0306(9) Uani 1 1 d . . . H18 H 0.6105 0.2747 0.2699 0.046 Uiso 1 1 calc R . . O19 O 0.5791(5) 0.30233(17) 0.3978(2) 0.0429(12) Uani 1 1 d . . . H19 H 0.6568 0.3178 0.3859 0.064 Uiso 1 1 calc R . . O20 O 0.5955(5) 0.24468(17) 0.5397(2) 0.0405(11) Uani 1 1 d . . . H20 H 0.5734 0.2795 0.5298 0.061 Uiso 1 1 calc R . . O25 O 1.1887(4) 0.12992(17) 0.1409(2) 0.0292(9) Uani 1 1 d . . . H25 H 1.1802 0.1258 0.0927 0.044 Uiso 1 1 calc R . . O26 O 0.9475(4) 0.15115(19) 0.0446(2) 0.0299(9) Uani 1 1 d . . . H26 H 0.8712 0.1657 0.0234 0.09(3) Uiso 1 1 calc R . . O27 O 0.6709(4) 0.14957(17) 0.1007(2) 0.0276(9) Uani 1 1 d D . . H27 H 0.6546 0.1214 0.0704 0.041 Uiso 1 1 calc RD . . C50 C 0.9270(9) 0.2777(4) 0.3207(5) 0.041(2) Uani 0.75 1 d P A 1 H50C H 0.9531 0.2730 0.2673 0.062 Uiso 0.75 1 calc PR A 1 H50D H 0.8240 0.2880 0.3208 0.062 Uiso 0.75 1 calc PR A 1 H50E H 0.9448 0.2411 0.3489 0.062 Uiso 0.75 1 calc PR A 1 O50 O 1.0158(5) 0.3245(2) 0.3586(2) 0.0211(11) Uani 0.75 1 d P A 1 H50B H 0.9615 0.3484 0.3792 0.032 Uiso 0.75 1 calc PR A 1 O50B O 0.9075(18) 0.2612(7) 0.2274(10) 0.041(3) Uani 0.25 1 d P B 2 C52 C 0.6723(12) 0.0415(5) -0.0629(6) 0.063(3) Uiso 0.75 1 d P . . H52A H 0.6945 0.0033 -0.0398 0.094 Uiso 0.25 1 calc PR C 1 H52B H 0.7218 0.0456 -0.1106 0.094 Uiso 0.25 1 calc PR C 1 H52C H 0.5672 0.0451 -0.0746 0.094 Uiso 0.25 1 calc PR C 1 H52D H 0.6868 0.0014 -0.0447 0.094 Uiso 0.50 1 d PR C 2 H52E H 0.5725 0.0462 -0.0854 0.094 Uiso 0.50 1 d PR C 2 H52F H 0.7403 0.0502 -0.1021 0.094 Uiso 0.50 1 d PR C 2 O52 O 0.709(2) 0.0758(8) -0.0223(12) 0.053(5) Uiso 0.25 1 d P D 1 H52G H 0.7903 0.0666 -0.0006 0.079 Uiso 0.25 1 calc PRD D 1 O52B O 0.6226(11) 0.0577(4) 0.0080(5) 0.045(2) Uiso 0.50 1 d P D 2 H52H H 0.5507 0.0371 0.0172 0.067 Uiso 0.50 1 calc PR D 2 C53 C 1.112(2) 0.0111(8) 0.8670(11) 0.043(5) Uiso 0.40 1 d P E 1 H53A H 1.0854 -0.0106 0.8193 0.064 Uiso 0.25 1 calc PR E 1 H53B H 1.0240 0.0202 0.8930 0.064 Uiso 0.25 1 calc PR E 1 H53C H 1.1773 -0.0126 0.9011 0.064 Uiso 0.25 1 calc PR E 1 H53D H 1.0875 0.0122 0.9210 0.064 Uiso 0.15 1 d PR E 2 H53E H 1.0229 0.0065 0.8332 0.064 Uiso 0.15 1 d PR E 2 H53F H 1.1770 -0.0218 0.8594 0.064 Uiso 0.15 1 d PR E 2 O53A O 1.173(2) 0.0563(8) 0.8512(12) 0.050(5) Uiso 0.25 1 d P E 1 H53G H 1.2395 0.0489 0.8224 0.075 Uiso 0.25 1 calc PR E 1 O53B O 1.254(3) 0.0269(13) 0.8926(18) 0.043(7) Uiso 0.15 1 d P F 2 H53H H 1.2734 0.0602 0.9106 0.065 Uiso 0.15 1 calc PR F 2 C53B C 1.0540(19) 0.0179(8) 0.8788(11) 0.085(6) Uiso 0.60 1 d PD F 2 H53I H 1.0234 0.0203 0.8236 0.128 Uiso 0.40 1 calc PR F 1 H53J H 1.0065 0.0489 0.9066 0.128 Uiso 0.40 1 calc PR F 1 H53K H 1.0265 -0.0201 0.8988 0.128 Uiso 0.40 1 calc PR F 1 H53L H 1.0247 0.0172 0.8233 0.128 Uiso 0.20 1 d PR F 2 H53M H 1.0260 -0.0188 0.9024 0.128 Uiso 0.20 1 d PR F 2 H53N H 1.0058 0.0505 0.9031 0.128 Uiso 0.20 1 d PR F 2 O53C O 1.0884(13) 0.0691(5) 0.8741(6) 0.038(3) Uiso 0.40 1 d P G 1 H53O H 1.1078 0.0808 0.9196 0.057 Uiso 0.40 1 calc PR G 1 O53D O 0.996(3) 0.0715(9) 0.9085(14) 0.057(7) Uiso 0.20 1 d PD H 2 H53P H 0.9268 0.0814 0.8772 0.086 Uiso 0.20 1 calc PR H 2 O54 O 1.3443(18) 0.0813(7) 0.7500(10) 0.041(3) Uani 0.25 1 d P . . Rb1 Rb 0.88099(7) 0.26775(3) 0.63197(3) 0.03412(18) Uani 1 1 d . . . Cl1 Cl 0.82135(19) 0.37012(9) 0.48431(9) 0.0532(5) 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 0.012(3) 0.030(3) 0.018(3) -0.005(2) 0.002(2) 0.000(2) C2 0.017(3) 0.026(3) 0.018(3) 0.000(2) 0.000(2) 0.001(2) C3 0.012(3) 0.029(3) 0.018(3) 0.000(2) 0.003(2) 0.002(2) C4 0.024(3) 0.031(3) 0.015(3) -0.001(2) 0.000(2) -0.007(2) C5 0.022(3) 0.026(3) 0.023(3) 0.001(2) -0.001(2) -0.010(2) C6 0.017(3) 0.033(3) 0.018(3) 0.004(2) 0.001(2) -0.002(2) C7 0.022(3) 0.031(3) 0.014(3) 0.000(2) 0.002(2) 0.001(2) C8 0.016(3) 0.022(3) 0.017(3) -0.001(2) 0.004(2) -0.003(2) C9 0.032(3) 0.024(3) 0.011(2) 0.000(2) 0.003(2) -0.001(2) C10 0.022(3) 0.024(3) 0.017(3) 0.003(2) -0.002(2) -0.002(2) C11 0.021(3) 0.029(3) 0.017(3) 0.002(2) 0.005(2) 0.005(2) C12 0.030(3) 0.026(3) 0.012(3) -0.005(2) 0.006(2) 0.002(2) C13 0.022(3) 0.021(3) 0.019(3) 0.004(2) -0.002(2) -0.001(2) C14 0.020(3) 0.035(3) 0.015(3) 0.002(2) 0.002(2) 0.006(2) C15 0.019(3) 0.025(3) 0.021(3) 0.002(2) -0.001(2) 0.002(2) C16 0.016(3) 0.021(3) 0.021(3) 0.003(2) 0.003(2) 0.003(2) C17 0.011(3) 0.028(3) 0.022(3) -0.003(2) 0.000(2) 0.001(2) C18 0.021(3) 0.036(3) 0.017(3) 0.005(2) -0.001(2) -0.002(2) C19 0.039(4) 0.021(3) 0.027(3) 0.004(2) -0.010(3) 0.002(3) C20 0.031(3) 0.028(3) 0.018(3) -0.004(2) -0.009(2) 0.006(3) C21 0.017(3) 0.031(3) 0.020(3) 0.001(2) 0.002(2) 0.000(2) C22 0.021(3) 0.023(3) 0.018(3) 0.000(2) 0.001(2) 0.006(2) C23 0.025(3) 0.030(3) 0.014(3) -0.001(2) 0.004(2) -0.002(2) C24 0.022(3) 0.021(3) 0.015(3) 0.000(2) -0.001(2) 0.002(2) C25 0.021(3) 0.023(3) 0.023(3) -0.001(2) 0.002(2) 0.001(2) C26 0.028(3) 0.027(3) 0.016(3) 0.001(2) 0.002(2) -0.002(2) C27 0.022(3) 0.022(3) 0.022(3) 0.002(2) -0.005(2) 0.001(2) C28 0.018(3) 0.032(3) 0.015(3) 0.003(2) 0.004(2) 0.002(2) C29 0.029(3) 0.039(3) 0.027(3) 0.007(3) 0.011(3) 0.005(3) C30 0.028(3) 0.033(3) 0.029(3) 0.005(3) 0.001(3) -0.007(3) C31 0.025(3) 0.038(3) 0.029(3) -0.007(3) 0.001(3) -0.003(3) C32 0.031(3) 0.032(3) 0.027(3) 0.001(3) 0.002(3) 0.007(3) O4 0.041(2) 0.033(2) 0.021(2) -0.0055(18) 0.0029(18) -0.008(2) O5 0.040(3) 0.030(2) 0.021(2) 0.0015(17) 0.0003(18) -0.0084(19) O6 0.046(3) 0.033(2) 0.019(2) 0.0035(17) 0.0099(18) -0.010(2) O11 0.026(2) 0.054(3) 0.017(2) -0.0030(19) 0.0033(17) 0.001(2) O12 0.027(2) 0.049(3) 0.0131(18) -0.0040(18) 0.0000(16) 0.002(2) O13 0.026(2) 0.038(2) 0.017(2) 0.0023(17) -0.0043(17) -0.0010(18) O18 0.044(3) 0.027(2) 0.021(2) 0.0049(17) -0.0039(18) -0.0045(19) O19 0.069(3) 0.026(2) 0.032(2) 0.0082(19) -0.008(2) -0.002(2) O20 0.071(3) 0.027(2) 0.022(2) -0.0044(17) -0.005(2) 0.010(2) O25 0.022(2) 0.050(3) 0.0158(19) 0.0002(18) 0.0052(16) -0.0027(18) O26 0.029(2) 0.046(3) 0.0154(19) 0.0037(18) 0.0039(17) -0.001(2) O27 0.026(2) 0.037(2) 0.0190(19) 0.0008(17) -0.0038(17) 0.0036(18) C50 0.024(4) 0.049(6) 0.051(5) 0.009(4) 0.007(4) 0.004(4) O50 0.015(2) 0.038(3) 0.011(2) 0.005(2) 0.003(2) -0.007(2) O50B 0.033(7) 0.027(6) 0.058(8) 0.004(6) -0.019(6) -0.009(5) O54 0.033(7) 0.027(6) 0.058(8) 0.004(6) -0.019(6) -0.009(5) Rb1 0.0339(3) 0.0312(3) 0.0360(3) 0.0020(3) -0.0063(2) 0.0020(3) Cl1 0.0409(10) 0.0919(14) 0.0270(8) 0.0006(9) 0.0042(7) -0.0182(10) _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 1.392(8) . ? C1 C2 1.402(7) . ? C1 C28 1.527(7) . ? C2 C3 1.391(7) . ? C3 C4 1.396(8) . ? C3 C7 1.521(7) . ? C4 O4 1.376(6) . ? C4 C5 1.373(7) . ? C5 C6 1.384(7) . ? C5 O5 1.391(6) . ? C6 O6 1.392(6) . ? C7 C8 1.516(7) . ? C7 C29 1.539(8) . ? C8 C9 1.396(7) . ? C8 C13 1.398(7) . ? C8 Rb1 3.500(5) . ? C9 C10 1.387(7) . ? C9 Rb1 3.473(5) . ? C10 C11 1.382(7) . ? C10 C14 1.526(7) . ? C10 Rb1 3.478(5) . ? C11 O11 1.375(6) . ? C11 C12 1.397(8) . ? C11 Rb1 3.477(5) . ? C12 O12 1.380(6) . ? C12 C13 1.387(7) . ? C12 Rb1 3.411(5) . ? C13 O13 1.376(6) . ? C13 Rb1 3.445(5) . ? C14 C30 1.513(8) . ? C14 C15 1.526(7) . ? C15 C20 1.384(8) . ? C15 C16 1.392(7) . ? C16 C17 1.389(7) . ? C17 C18 1.396(8) . ? C17 C21 1.525(7) . ? C18 O18 1.375(6) . ? C18 C19 1.393(8) . ? C19 C20 1.383(8) . ? C19 O19 1.385(7) . ? C20 O20 1.389(6) . ? C21 C31 1.522(8) . ? C21 C22 1.529(7) . ? C22 C27 1.392(7) . ? C22 C23 1.391(7) . ? C23 C24 1.393(7) . ? C24 C25 1.400(7) . ? C24 C28 1.529(7) . ? C25 O25 1.383(6) . ? C25 C26 1.390(8) . ? C26 O26 1.391(6) . ? C26 C27 1.389(8) . ? C27 O27 1.397(6) . ? C28 C32 1.530(8) . ? O6 Rb1 3.430(4) 4_665 ? O18 Rb1 2.921(4) 4_565 ? O25 Rb1 2.954(4) 4_665 ? O27 Rb1 3.357(4) 4_565 ? C50 O50 1.476(10) . ? C52 O52 1.09(2) . ? C52 O52B 1.394(13) . ? C53 O53A 1.22(2) . ? O53B C53B 1.86(3) . ? Rb1 O18 2.921(4) 4_666 ? Rb1 O25 2.954(4) 4_566 ? Rb1 O27 3.357(4) 4_666 ? Rb1 O6 3.430(4) 4_566 ? Rb1 Cl1 3.4887(19) . ? 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 117.1(5) . . ? C6 C1 C28 119.9(5) . . ? C2 C1 C28 123.0(5) . . ? C3 C2 C1 123.0(5) . . ? C2 C3 C4 117.5(5) . . ? C2 C3 C7 123.2(5) . . ? C4 C3 C7 119.3(5) . . ? O4 C4 C5 121.0(5) . . ? O4 C4 C3 118.3(5) . . ? C5 C4 C3 120.7(5) . . ? C4 C5 C6 120.8(5) . . ? C4 C5 O5 118.7(5) . . ? C6 C5 O5 120.5(5) . . ? C5 C6 C1 120.8(5) . . ? C5 C6 O6 120.4(5) . . ? C1 C6 O6 118.7(5) . . ? C8 C7 C3 112.8(4) . . ? C8 C7 C29 107.3(4) . . ? C3 C7 C29 114.4(4) . . ? C9 C8 C13 117.3(5) . . ? C9 C8 C7 121.8(4) . . ? C13 C8 C7 120.8(5) . . ? C9 C8 Rb1 77.4(3) . . ? C13 C8 Rb1 76.2(3) . . ? C7 C8 Rb1 120.4(3) . . ? C10 C9 C8 123.2(5) . . ? C10 C9 Rb1 78.7(3) . . ? C8 C9 Rb1 79.5(3) . . ? C11 C10 C9 118.0(5) . . ? C11 C10 C14 119.7(5) . . ? C9 C10 C14 122.1(4) . . ? C11 C10 Rb1 78.5(3) . . ? C9 C10 Rb1 78.3(3) . . ? C14 C10 Rb1 117.3(3) . . ? O11 C11 C10 118.8(5) . . ? O11 C11 C12 120.7(4) . . ? C10 C11 C12 120.5(5) . . ? O11 C11 Rb1 116.1(3) . . ? C10 C11 Rb1 78.6(3) . . ? C12 C11 Rb1 75.6(3) . . ? O12 C12 C13 122.9(5) . . ? O12 C12 C11 116.8(5) . . ? C13 C12 C11 120.3(5) . . ? O12 C12 Rb1 109.6(3) . . ? C13 C12 Rb1 79.7(3) . . ? C11 C12 Rb1 81.0(3) . . ? O13 C13 C12 119.6(5) . . ? O13 C13 C8 119.7(5) . . ? C12 C13 C8 120.6(5) . . ? O13 C13 Rb1 110.4(3) . . ? C12 C13 Rb1 77.0(3) . . ? C8 C13 Rb1 80.6(3) . . ? C30 C14 C10 109.5(4) . . ? C30 C14 C15 113.2(4) . . ? C10 C14 C15 112.4(4) . . ? C20 C15 C16 117.9(5) . . ? C20 C15 C14 117.6(5) . . ? C16 C15 C14 124.5(5) . . ? C15 C16 C17 123.1(5) . . ? C16 C17 C18 117.3(5) . . ? C16 C17 C21 124.3(5) . . ? C18 C17 C21 118.4(5) . . ? O18 C18 C17 118.7(5) . . ? O18 C18 C19 120.4(5) . . ? C17 C18 C19 120.9(5) . . ? C20 C19 O19 120.4(5) . . ? C20 C19 C18 119.8(5) . . ? O19 C19 C18 119.7(5) . . ? C19 C20 C15 120.9(5) . . ? C19 C20 O20 120.5(5) . . ? C15 C20 O20 118.6(5) . . ? C17 C21 C31 114.4(4) . . ? C17 C21 C22 111.4(4) . . ? C31 C21 C22 109.4(4) . . ? C27 C22 C23 117.1(5) . . ? C27 C22 C21 120.0(5) . . ? C23 C22 C21 122.7(4) . . ? C22 C23 C24 123.9(5) . . ? C23 C24 C25 117.3(5) . . ? C23 C24 C28 123.1(4) . . ? C25 C24 C28 119.4(5) . . ? O25 C25 C26 121.3(5) . . ? O25 C25 C24 118.5(5) . . ? C26 C25 C24 120.2(5) . . ? O26 C26 C27 122.9(5) . . ? O26 C26 C25 116.5(5) . . ? C27 C26 C25 120.6(5) . . ? C22 C27 C26 120.9(5) . . ? C22 C27 O27 121.0(5) . . ? C26 C27 O27 118.0(4) . . ? C32 C28 C1 113.6(4) . . ? C32 C28 C24 109.7(4) . . ? C1 C28 C24 111.1(4) . . ? C6 O6 Rb1 154.8(3) . 4_665 ? C18 O18 Rb1 130.1(3) . 4_565 ? C25 O25 Rb1 126.7(3) . 4_665 ? C27 O27 Rb1 128.7(3) . 4_565 ? O52 C52 O52B 49.3(12) . . ? O18 Rb1 O25 112.39(10) 4_666 4_566 ? O18 Rb1 O27 69.13(10) 4_666 4_666 ? O25 Rb1 O27 92.84(10) 4_566 4_666 ? O18 Rb1 C12 68.65(12) 4_666 . ? O25 Rb1 C12 125.47(12) 4_566 . ? O27 Rb1 C12 131.16(12) 4_666 . ? O18 Rb1 O6 64.75(10) 4_666 4_566 ? O25 Rb1 O6 69.10(10) 4_566 4_566 ? O27 Rb1 O6 117.07(9) 4_666 4_566 ? C12 Rb1 O6 62.99(11) . 4_566 ? O18 Rb1 C13 61.24(11) 4_666 . ? O25 Rb1 C13 148.22(12) 4_566 . ? O27 Rb1 C13 111.05(11) 4_666 . ? C12 Rb1 C13 23.34(12) . . ? O6 Rb1 C13 81.16(11) 4_566 . ? O18 Rb1 C9 100.19(12) 4_666 . ? O25 Rb1 C9 139.98(12) 4_566 . ? O27 Rb1 C9 121.00(11) 4_666 . ? C12 Rb1 C9 46.96(12) . . ? O6 Rb1 C9 107.50(11) 4_566 . ? C13 Rb1 C9 40.35(12) . . ? O18 Rb1 C10 107.61(12) 4_666 . ? O25 Rb1 C10 119.66(12) 4_566 . ? O27 Rb1 C10 143.97(11) 4_666 . ? C12 Rb1 C10 40.98(12) . . ? O6 Rb1 C10 90.68(11) 4_566 . ? C13 Rb1 C10 47.69(12) . . ? C9 Rb1 C10 23.02(12) . . ? O18 Rb1 C11 91.71(12) 4_666 . ? O25 Rb1 C11 114.08(11) 4_566 . ? O27 Rb1 C11 151.76(11) 4_666 . ? C12 Rb1 C11 23.37(13) . . ? O6 Rb1 C11 68.65(11) 4_566 . ? C13 Rb1 C11 40.82(12) . . ? C9 Rb1 C11 39.95(12) . . ? C10 Rb1 C11 22.93(12) . . ? O18 Rb1 Cl1 131.86(9) 4_666 . ? O25 Rb1 Cl1 56.00(8) 4_566 . ? O27 Rb1 Cl1 65.56(7) 4_666 . ? C12 Rb1 Cl1 159.14(10) . . ? O6 Rb1 Cl1 124.95(7) 4_566 . ? C13 Rb1 Cl1 153.10(9) . . ? C9 Rb1 Cl1 116.33(9) . . ? C10 Rb1 Cl1 118.36(9) . . ? C11 Rb1 Cl1 136.42(9) . . ? O18 Rb1 C8 77.96(11) 4_666 . ? O25 Rb1 C8 160.47(11) 4_566 . ? O27 Rb1 C8 106.51(11) 4_666 . ? C12 Rb1 C8 40.95(12) . . ? O6 Rb1 C8 103.17(10) 4_566 . ? C13 Rb1 C8 23.21(12) . . ? C9 Rb1 C8 23.10(12) . . ? C10 Rb1 C8 41.09(12) . . ? C11 Rb1 C8 47.36(12) . . ? Cl1 Rb1 C8 129.96(9) . . ? 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 1.8(8) . . . . ? C28 C1 C2 C3 -178.5(5) . . . . ? C1 C2 C3 C4 2.1(8) . . . . ? C1 C2 C3 C7 -177.8(5) . . . . ? C2 C3 C4 O4 176.3(5) . . . . ? C7 C3 C4 O4 -3.9(7) . . . . ? C2 C3 C4 C5 -3.8(8) . . . . ? C7 C3 C4 C5 176.0(5) . . . . ? O4 C4 C5 C6 -178.5(5) . . . . ? C3 C4 C5 C6 1.6(8) . . . . ? O4 C4 C5 O5 2.9(8) . . . . ? C3 C4 C5 O5 -177.0(5) . . . . ? C4 C5 C6 C1 2.5(8) . . . . ? O5 C5 C6 C1 -178.9(5) . . . . ? C4 C5 C6 O6 -179.2(5) . . . . ? O5 C5 C6 O6 -0.6(8) . . . . ? C2 C1 C6 C5 -4.1(8) . . . . ? C28 C1 C6 C5 176.2(5) . . . . ? C2 C1 C6 O6 177.6(5) . . . . ? C28 C1 C6 O6 -2.1(7) . . . . ? C2 C3 C7 C8 -110.0(6) . . . . ? C4 C3 C7 C8 70.2(6) . . . . ? C2 C3 C7 C29 13.1(7) . . . . ? C4 C3 C7 C29 -166.8(5) . . . . ? C3 C7 C8 C9 45.6(7) . . . . ? C29 C7 C8 C9 -81.3(6) . . . . ? C3 C7 C8 C13 -139.8(5) . . . . ? C29 C7 C8 C13 93.4(6) . . . . ? C3 C7 C8 Rb1 -48.2(5) . . . . ? C29 C7 C8 Rb1 -175.1(3) . . . . ? C13 C8 C9 C10 -2.0(8) . . . . ? C7 C8 C9 C10 172.9(5) . . . . ? Rb1 C8 C9 C10 -69.0(5) . . . . ? C13 C8 C9 Rb1 67.0(4) . . . . ? C7 C8 C9 Rb1 -118.2(5) . . . . ? C8 C9 C10 C11 -0.6(8) . . . . ? Rb1 C9 C10 C11 -70.0(5) . . . . ? C8 C9 C10 C14 -175.7(5) . . . . ? Rb1 C9 C10 C14 115.0(5) . . . . ? C8 C9 C10 Rb1 69.4(5) . . . . ? C9 C10 C11 O11 -176.5(5) . . . . ? C14 C10 C11 O11 -1.3(8) . . . . ? Rb1 C10 C11 O11 113.6(5) . . . . ? C9 C10 C11 C12 4.2(8) . . . . ? C14 C10 C11 C12 179.4(5) . . . . ? Rb1 C10 C11 C12 -65.7(5) . . . . ? C9 C10 C11 Rb1 69.9(4) . . . . ? C14 C10 C11 Rb1 -115.0(5) . . . . ? O11 C11 C12 O12 -4.6(8) . . . . ? C10 C11 C12 O12 174.7(5) . . . . ? Rb1 C11 C12 O12 107.5(4) . . . . ? O11 C11 C12 C13 175.5(5) . . . . ? C10 C11 C12 C13 -5.2(8) . . . . ? Rb1 C11 C12 C13 -72.4(5) . . . . ? O11 C11 C12 Rb1 -112.1(5) . . . . ? C10 C11 C12 Rb1 67.2(5) . . . . ? O12 C12 C13 O13 -0.6(8) . . . . ? C11 C12 C13 O13 179.4(5) . . . . ? Rb1 C12 C13 O13 106.2(4) . . . . ? O12 C12 C13 C8 -177.5(5) . . . . ? C11 C12 C13 C8 2.4(8) . . . . ? Rb1 C12 C13 C8 -70.7(5) . . . . ? O12 C12 C13 Rb1 -106.8(5) . . . . ? C11 C12 C13 Rb1 73.1(5) . . . . ? C9 C8 C13 O13 -175.8(5) . . . . ? C7 C8 C13 O13 9.2(7) . . . . ? Rb1 C8 C13 O13 -108.2(4) . . . . ? C9 C8 C13 C12 1.1(8) . . . . ? C7 C8 C13 C12 -173.9(5) . . . . ? Rb1 C8 C13 C12 68.7(5) . . . . ? C9 C8 C13 Rb1 -67.6(4) . . . . ? C7 C8 C13 Rb1 117.4(4) . . . . ? C11 C10 C14 C30 -88.7(6) . . . . ? C9 C10 C14 C30 86.2(6) . . . . ? Rb1 C10 C14 C30 179.2(3) . . . . ? C11 C10 C14 C15 144.5(5) . . . . ? C9 C10 C14 C15 -40.5(7) . . . . ? Rb1 C10 C14 C15 52.5(5) . . . . ? C30 C14 C15 C20 160.0(5) . . . . ? C10 C14 C15 C20 -75.2(6) . . . . ? C30 C14 C15 C16 -17.6(7) . . . . ? C10 C14 C15 C16 107.1(6) . . . . ? C20 C15 C16 C17 -1.3(8) . . . . ? C14 C15 C16 C17 176.4(5) . . . . ? C15 C16 C17 C18 -1.7(8) . . . . ? C15 C16 C17 C21 178.7(5) . . . . ? C16 C17 C18 O18 -176.3(5) . . . . ? C21 C17 C18 O18 3.4(7) . . . . ? C16 C17 C18 C19 2.2(8) . . . . ? C21 C17 C18 C19 -178.1(5) . . . . ? O18 C18 C19 C20 178.7(5) . . . . ? C17 C18 C19 C20 0.3(9) . . . . ? O18 C18 C19 O19 1.6(9) . . . . ? C17 C18 C19 O19 -176.9(5) . . . . ? O19 C19 C20 C15 173.8(5) . . . . ? C18 C19 C20 C15 -3.4(9) . . . . ? O19 C19 C20 O20 -4.6(9) . . . . ? C18 C19 C20 O20 178.3(5) . . . . ? C16 C15 C20 C19 3.8(8) . . . . ? C14 C15 C20 C19 -174.0(5) . . . . ? C16 C15 C20 O20 -177.8(5) . . . . ? C14 C15 C20 O20 4.4(8) . . . . ? C16 C17 C21 C31 17.8(7) . . . . ? C18 C17 C21 C31 -161.8(5) . . . . ? C16 C17 C21 C22 -106.8(6) . . . . ? C18 C17 C21 C22 73.5(6) . . . . ? C17 C21 C22 C27 -136.4(5) . . . . ? C31 C21 C22 C27 96.2(6) . . . . ? C17 C21 C22 C23 48.8(7) . . . . ? C31 C21 C22 C23 -78.6(6) . . . . ? C27 C22 C23 C24 -1.6(8) . . . . ? C21 C22 C23 C24 173.3(5) . . . . ? C22 C23 C24 C25 0.7(8) . . . . ? C22 C23 C24 C28 -174.2(5) . . . . ? C23 C24 C25 O25 -179.8(5) . . . . ? C28 C24 C25 O25 -4.6(7) . . . . ? C23 C24 C25 C26 1.5(8) . . . . ? C28 C24 C25 C26 176.6(5) . . . . ? O25 C25 C26 O26 0.5(8) . . . . ? C24 C25 C26 O26 179.2(5) . . . . ? O25 C25 C26 C27 178.5(5) . . . . ? C24 C25 C26 C27 -2.8(8) . . . . ? C23 C22 C27 C26 0.3(8) . . . . ? C21 C22 C27 C26 -174.8(5) . . . . ? C23 C22 C27 O27 -176.7(5) . . . . ? C21 C22 C27 O27 8.3(8) . . . . ? O26 C26 C27 C22 179.8(5) . . . . ? C25 C26 C27 C22 1.9(8) . . . . ? O26 C26 C27 O27 -3.2(8) . . . . ? C25 C26 C27 O27 178.9(5) . . . . ? C6 C1 C28 C32 161.8(5) . . . . ? C2 C1 C28 C32 -17.9(7) . . . . ? C6 C1 C28 C24 -74.0(6) . . . . ? C2 C1 C28 C24 106.3(6) . . . . ? C23 C24 C28 C32 77.8(6) . . . . ? C25 C24 C28 C32 -97.0(6) . . . . ? C23 C24 C28 C1 -48.5(7) . . . . ? C25 C24 C28 C1 136.6(5) . . . . ? C5 C6 O6 Rb1 149.8(6) . . . 4_665 ? C1 C6 O6 Rb1 -31.9(10) . . . 4_665 ? C17 C18 O18 Rb1 63.0(6) . . . 4_565 ? C19 C18 O18 Rb1 -115.5(5) . . . 4_565 ? C26 C25 O25 Rb1 89.3(5) . . . 4_665 ? C24 C25 O25 Rb1 -89.4(5) . . . 4_665 ? C22 C27 O27 Rb1 41.1(6) . . . 4_565 ? C26 C27 O27 Rb1 -135.9(4) . . . 4_565 ? O12 C12 Rb1 O18 54.9(3) . . . 4_666 ? C13 C12 Rb1 O18 -66.6(3) . . . 4_666 ? C11 C12 Rb1 O18 170.2(3) . . . 4_666 ? O12 C12 Rb1 O25 -48.0(4) . . . 4_566 ? C13 C12 Rb1 O25 -169.5(3) . . . 4_566 ? C11 C12 Rb1 O25 67.3(3) . . . 4_566 ? O12 C12 Rb1 O27 86.7(4) . . . 4_666 ? C13 C12 Rb1 O27 -34.8(3) . . . 4_666 ? C11 C12 Rb1 O27 -158.0(3) . . . 4_666 ? O12 C12 Rb1 O6 -16.8(3) . . . 4_566 ? C13 C12 Rb1 O6 -138.2(3) . . . 4_566 ? C11 C12 Rb1 O6 98.6(3) . . . 4_566 ? O12 C12 Rb1 C13 121.5(5) . . . . ? C11 C12 Rb1 C13 -123.2(5) . . . . ? O12 C12 Rb1 C9 -176.4(4) . . . . ? C13 C12 Rb1 C9 62.1(3) . . . . ? C11 C12 Rb1 C9 -61.1(3) . . . . ? O12 C12 Rb1 C10 -144.1(4) . . . . ? C13 C12 Rb1 C10 94.4(3) . . . . ? C11 C12 Rb1 C10 -28.8(3) . . . . ? O12 C12 Rb1 C11 -115.3(5) . . . . ? C13 C12 Rb1 C11 123.2(5) . . . . ? O12 C12 Rb1 Cl1 -134.6(3) . . . . ? C13 C12 Rb1 Cl1 103.9(4) . . . . ? C11 C12 Rb1 Cl1 -19.3(5) . . . . ? O12 C12 Rb1 C8 151.1(4) . . . . ? C13 C12 Rb1 C8 29.7(3) . . . . ? C11 C12 Rb1 C8 -93.5(3) . . . . ? O13 C13 Rb1 O18 -14.2(3) . . . 4_666 ? C12 C13 Rb1 O18 102.9(3) . . . 4_666 ? C8 C13 Rb1 O18 -132.5(3) . . . 4_666 ? O13 C13 Rb1 O25 -100.7(4) . . . 4_566 ? C12 C13 Rb1 O25 16.4(4) . . . 4_566 ? C8 C13 Rb1 O25 140.9(3) . . . 4_566 ? O13 C13 Rb1 O27 35.5(3) . . . 4_666 ? C12 C13 Rb1 O27 152.6(3) . . . 4_666 ? C8 C13 Rb1 O27 -82.8(3) . . . 4_666 ? O13 C13 Rb1 C12 -117.1(5) . . . . ? C8 C13 Rb1 C12 124.6(5) . . . . ? O13 C13 Rb1 O6 -80.2(3) . . . 4_566 ? C12 C13 Rb1 O6 36.9(3) . . . 4_566 ? C8 C13 Rb1 O6 161.5(3) . . . 4_566 ? O13 C13 Rb1 C9 149.1(4) . . . . ? C12 C13 Rb1 C9 -93.9(3) . . . . ? C8 C13 Rb1 C9 30.7(3) . . . . ? O13 C13 Rb1 C10 -179.2(4) . . . . ? C12 C13 Rb1 C10 -62.2(3) . . . . ? C8 C13 Rb1 C10 62.4(3) . . . . ? O13 C13 Rb1 C11 -147.6(4) . . . . ? C12 C13 Rb1 C11 -30.5(3) . . . . ? C8 C13 Rb1 C11 94.0(3) . . . . ? O13 C13 Rb1 Cl1 112.8(3) . . . . ? C12 C13 Rb1 Cl1 -130.2(3) . . . . ? C8 C13 Rb1 Cl1 -5.6(4) . . . . ? O13 C13 Rb1 C8 118.4(5) . . . . ? C12 C13 Rb1 C8 -124.6(5) . . . . ? C10 C9 Rb1 O18 111.3(3) . . . 4_666 ? C8 C9 Rb1 O18 -16.0(3) . . . 4_666 ? C10 C9 Rb1 O25 -33.4(4) . . . 4_566 ? C8 C9 Rb1 O25 -160.6(3) . . . 4_566 ? C10 C9 Rb1 O27 -177.0(3) . . . 4_666 ? C8 C9 Rb1 O27 55.7(3) . . . 4_666 ? C10 C9 Rb1 C12 63.7(3) . . . . ? C8 C9 Rb1 C12 -63.6(3) . . . . ? C10 C9 Rb1 O6 44.7(3) . . . 4_566 ? C8 C9 Rb1 O6 -82.5(3) . . . 4_566 ? C10 C9 Rb1 C13 96.4(3) . . . . ? C8 C9 Rb1 C13 -30.8(3) . . . . ? C8 C9 Rb1 C10 -127.3(4) . . . . ? C10 C9 Rb1 C11 30.9(3) . . . . ? C8 C9 Rb1 C11 -96.3(3) . . . . ? C10 C9 Rb1 Cl1 -101.0(3) . . . . ? C8 C9 Rb1 Cl1 131.8(3) . . . . ? C10 C9 Rb1 C8 127.3(5) . . . . ? C11 C10 Rb1 O18 48.0(3) . . . 4_666 ? C9 C10 Rb1 O18 -74.2(3) . . . 4_666 ? C14 C10 Rb1 O18 165.6(3) . . . 4_666 ? C11 C10 Rb1 O25 -81.9(3) . . . 4_566 ? C9 C10 Rb1 O25 156.0(3) . . . 4_566 ? C14 C10 Rb1 O25 35.8(4) . . . 4_566 ? C11 C10 Rb1 O27 126.5(3) . . . 4_666 ? C9 C10 Rb1 O27 4.3(4) . . . 4_666 ? C14 C10 Rb1 O27 -115.9(3) . . . 4_666 ? C11 C10 Rb1 C12 29.4(3) . . . . ? C9 C10 Rb1 C12 -92.8(3) . . . . ? C14 C10 Rb1 C12 147.0(4) . . . . ? C11 C10 Rb1 O6 -15.7(3) . . . 4_566 ? C9 C10 Rb1 O6 -137.8(3) . . . 4_566 ? C14 C10 Rb1 O6 102.0(4) . . . 4_566 ? C11 C10 Rb1 C13 61.7(3) . . . . ? C9 C10 Rb1 C13 -60.5(3) . . . . ? C14 C10 Rb1 C13 179.3(4) . . . . ? C11 C10 Rb1 C9 122.1(5) . . . . ? C14 C10 Rb1 C9 -120.2(5) . . . . ? C9 C10 Rb1 C11 -122.1(5) . . . . ? C14 C10 Rb1 C11 117.7(5) . . . . ? C11 C10 Rb1 Cl1 -146.8(3) . . . . ? C9 C10 Rb1 Cl1 91.1(3) . . . . ? C14 C10 Rb1 Cl1 -29.1(4) . . . . ? C11 C10 Rb1 C8 93.8(3) . . . . ? C9 C10 Rb1 C8 -28.4(3) . . . . ? C14 C10 Rb1 C8 -148.6(4) . . . . ? O11 C11 Rb1 O18 108.4(3) . . . 4_666 ? C10 C11 Rb1 O18 -134.9(3) . . . 4_666 ? C12 C11 Rb1 O18 -9.1(3) . . . 4_666 ? O11 C11 Rb1 O25 -7.1(4) . . . 4_566 ? C10 C11 Rb1 O25 109.6(3) . . . 4_566 ? C12 C11 Rb1 O25 -124.6(3) . . . 4_566 ? O11 C11 Rb1 O27 154.2(3) . . . 4_666 ? C10 C11 Rb1 O27 -89.2(4) . . . 4_666 ? C12 C11 Rb1 O27 36.7(4) . . . 4_666 ? O11 C11 Rb1 C12 117.5(5) . . . . ? C10 C11 Rb1 C12 -125.8(5) . . . . ? O11 C11 Rb1 O6 46.5(3) . . . 4_566 ? C10 C11 Rb1 O6 163.1(3) . . . 4_566 ? C12 C11 Rb1 O6 -71.1(3) . . . 4_566 ? O11 C11 Rb1 C13 148.0(4) . . . . ? C10 C11 Rb1 C13 -95.4(4) . . . . ? C12 C11 Rb1 C13 30.5(3) . . . . ? O11 C11 Rb1 C9 -147.7(4) . . . . ? C10 C11 Rb1 C9 -31.0(3) . . . . ? C12 C11 Rb1 C9 94.8(3) . . . . ? O11 C11 Rb1 C10 -116.6(5) . . . . ? C12 C11 Rb1 C10 125.8(5) . . . . ? O11 C11 Rb1 Cl1 -72.3(4) . . . . ? C10 C11 Rb1 Cl1 44.3(4) . . . . ? C12 C11 Rb1 Cl1 170.2(2) . . . . ? O11 C11 Rb1 C8 -179.7(4) . . . . ? C10 C11 Rb1 C8 -63.1(3) . . . . ? C12 C11 Rb1 C8 62.8(3) . . . . ? C9 C8 Rb1 O18 163.9(3) . . . 4_666 ? C13 C8 Rb1 O18 41.3(3) . . . 4_666 ? C7 C8 Rb1 O18 -76.5(4) . . . 4_666 ? C9 C8 Rb1 O25 39.6(5) . . . 4_566 ? C13 C8 Rb1 O25 -83.0(4) . . . 4_566 ? C7 C8 Rb1 O25 159.2(3) . . . 4_566 ? C9 C8 Rb1 O27 -132.4(3) . . . 4_666 ? C13 C8 Rb1 O27 105.0(3) . . . 4_666 ? C7 C8 Rb1 O27 -12.8(4) . . . 4_666 ? C9 C8 Rb1 C12 92.7(3) . . . . ? C13 C8 Rb1 C12 -29.9(3) . . . . ? C7 C8 Rb1 C12 -147.7(4) . . . . ? C9 C8 Rb1 O6 103.8(3) . . . 4_566 ? C13 C8 Rb1 O6 -18.8(3) . . . 4_566 ? C7 C8 Rb1 O6 -136.6(3) . . . 4_566 ? C9 C8 Rb1 C13 122.6(5) . . . . ? C7 C8 Rb1 C13 -117.8(5) . . . . ? C13 C8 Rb1 C9 -122.6(5) . . . . ? C7 C8 Rb1 C9 119.6(5) . . . . ? C9 C8 Rb1 C10 28.3(3) . . . . ? C13 C8 Rb1 C10 -94.3(3) . . . . ? C7 C8 Rb1 C10 147.9(4) . . . . ? C9 C8 Rb1 C11 60.2(3) . . . . ? C13 C8 Rb1 C11 -62.4(3) . . . . ? C7 C8 Rb1 C11 179.8(4) . . . . ? C9 C8 Rb1 Cl1 -60.7(3) . . . . ? C13 C8 Rb1 Cl1 176.7(3) . . . . ? C7 C8 Rb1 Cl1 58.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O27 0.84 2.05 2.823(6) 153.0 4_666 O4 H4 O5 0.84 2.30 2.751(5) 114.0 . O5 H5 O50 0.84 1.85 2.671(6) 164.4 . O6 H6 O12 0.84 2.15 2.964(6) 162.6 4_665 O6 H6 O5 0.84 2.35 2.795(5) 113.7 . O11 H11 O50 0.84 2.03 2.772(6) 146.6 4_566 O11 H11 O12 0.84 2.27 2.724(5) 114.3 . O12 H12 O19 0.84 2.01 2.816(6) 160.2 4_666 O12 H12 O13 0.84 2.40 2.818(5) 111.9 . O13 H13 O53A 0.84 1.77 2.58(2) 161.5 . O13 H13 O53C 0.84 1.85 2.668(11) 164.3 . O13 H13 O53D 0.84 2.63 3.36(3) 146.8 . O18 H18 O13 0.84 2.05 2.857(5) 161.1 4_565 O18 H18 O19 0.84 2.35 2.776(6) 112.3 . O19 H19 Cl1 0.84 2.51 3.031(5) 121.5 . O20 H20 O26 0.84 2.00 2.757(6) 150.0 4_566 O20 H20 O19 0.84 2.35 2.790(6) 112.9 . O25 H25 O26 0.84 2.32 2.729(5) 110.3 . O25 H25 Cl1 0.84 2.37 3.061(4) 140.4 4_665 O26 H26 O5 0.84 2.04 2.844(6) 159.0 4_565 O26 H26 O27 0.84 2.39 2.801(5) 110.6 . O27 H27 O52B 0.84 1.83 2.668(10) 177.4 . O27 H27 O52 0.84 2.01 2.77(2) 148.9 . O50 H50B Cl1 0.84 2.37 3.107(5) 147.4 . O52 H52G O26 0.84 2.51 2.97(2) 114.8 . O53A H53G O54 0.84 1.80 2.52(3) 142.1 . O53B H53H Cl1 0.84 2.07 2.89(3) 163.8 4_666 O53C H53O Cl1 0.84 2.47 3.102(11) 132.9 4_666 O53D H53P O12 0.84 2.16 2.88(2) 143.7 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.58 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.847 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.098 #===END data_ocs080 _database_code_depnum_ccdc_archive 'CCDC 288488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C32 H32 O12), Cs, Br, 2.5(C H4 O), 0.75(O)' _chemical_formula_sum 'C34.50 H42 Br Cs O15.25' _chemical_formula_weight 913.50 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.34140(10) _cell_length_b 23.2823(4) _cell_length_c 17.4432(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.7670(12) _cell_angle_gamma 90.00 _cell_volume 3785.51(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6785 _exptl_absorpt_correction_T_max 0.8173 _exptl_absorpt_process_details ; Blessin, R. H. Acta Crystallogr., Sect A 1995, 51, 33-38' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _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 Kappa CCD with Apex II detector' ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21695 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.57 _reflns_number_total 7011 _reflns_number_gt 6003 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0002P)^2^+51.8680P] 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 7011 _refine_ls_number_parameters 528 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.249 _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 1.1843(8) 0.1327(4) 0.3802(4) 0.0218(17) Uani 1 1 d . . . C2 C 1.1567(8) 0.1058(4) 0.4499(5) 0.0245(18) Uani 1 1 d . . . H2 H 1.1363 0.0659 0.4492 0.029 Uiso 1 1 calc R . . C3 C 1.1576(8) 0.1350(4) 0.5202(4) 0.0230(17) Uani 1 1 d . . . C4 C 1.1857(8) 0.1939(4) 0.5196(5) 0.0270(19) Uani 1 1 d . . . C5 C 1.2160(8) 0.2217(4) 0.4514(5) 0.0282(19) Uani 1 1 d . . . C6 C 1.2167(8) 0.1910(4) 0.3833(4) 0.0248(18) Uani 1 1 d . . . C7 C 1.1358(8) 0.1052(4) 0.5954(4) 0.0236(17) Uani 1 1 d . . . H7 H 1.2130 0.1193 0.6332 0.028 Uiso 1 1 calc R . . C8 C 0.9934(8) 0.1210(3) 0.6269(4) 0.0192(16) Uani 1 1 d . . . C9 C 0.8640(8) 0.1203(3) 0.5815(4) 0.0223(17) Uani 1 1 d . . . H9 H 0.8687 0.1138 0.5279 0.027 Uiso 1 1 calc R . . C10 C 0.7318(8) 0.1283(3) 0.6087(4) 0.0211(16) Uani 1 1 d . . . C11 C 0.7246(8) 0.1372(3) 0.6880(5) 0.0234(17) Uani 1 1 d . . . C12 C 0.8483(8) 0.1421(3) 0.7355(5) 0.0247(18) Uani 1 1 d . . . C13 C 0.9798(8) 0.1324(3) 0.7071(4) 0.0194(16) Uani 1 1 d . . . C14 C 0.5916(8) 0.1248(4) 0.5584(4) 0.0226(17) Uani 1 1 d . . . H14 H 0.5172 0.1456 0.5863 0.027 Uiso 1 1 calc R . . C15 C 0.6021(8) 0.1546(4) 0.4826(4) 0.0232(17) Uani 1 1 d . . . C16 C 0.6187(8) 0.1259(3) 0.4123(4) 0.0219(16) Uani 1 1 d . . . H16 H 0.6292 0.0853 0.4131 0.026 Uiso 1 1 calc R . . C17 C 0.6203(8) 0.1539(3) 0.3425(4) 0.0214(17) Uani 1 1 d . . . C18 C 0.6049(8) 0.2137(4) 0.3415(5) 0.0232(17) Uani 1 1 d . . . C19 C 0.5893(8) 0.2433(3) 0.4090(4) 0.0221(17) Uani 1 1 d . . . C20 C 0.5883(8) 0.2144(3) 0.4795(4) 0.0206(16) Uani 1 1 d . . . C21 C 0.6342(8) 0.1227(3) 0.2666(4) 0.0207(16) Uani 1 1 d . . . H21 H 0.5650 0.1415 0.2283 0.025 Uiso 1 1 calc R . . C22 C 0.7821(8) 0.1282(3) 0.2351(4) 0.0202(16) Uani 1 1 d . . . C23 C 0.9081(8) 0.1183(3) 0.2824(5) 0.0239(17) Uani 1 1 d . . . H23 H 0.9000 0.1126 0.3359 0.029 Uiso 1 1 calc R . . C24 C 1.0441(8) 0.1167(3) 0.2540(5) 0.0237(17) Uani 1 1 d . . . C25 C 1.0526(8) 0.1250(4) 0.1757(5) 0.0256(18) Uani 1 1 d . . . C26 C 0.9309(9) 0.1369(4) 0.1286(4) 0.0236(18) Uani 1 1 d . . . C27 C 0.7976(9) 0.1386(3) 0.1584(5) 0.0234(17) Uani 1 1 d . . . C28 C 1.1788(8) 0.1016(4) 0.3042(5) 0.0269(18) Uani 1 1 d . . . H28 H 1.2626 0.1154 0.2764 0.032 Uiso 1 1 calc R . . C29 C 1.1472(9) 0.0399(4) 0.5934(5) 0.030(2) Uani 1 1 d . . . H29A H 1.0721 0.0244 0.5573 0.046 Uiso 1 1 calc R . . H29B H 1.1352 0.0244 0.6448 0.046 Uiso 1 1 calc R . . H29C H 1.2415 0.0288 0.5767 0.046 Uiso 1 1 calc R . . C30 C 0.5432(9) 0.0622(4) 0.5514(5) 0.0288(19) Uani 1 1 d . . . H30A H 0.4536 0.0600 0.5190 0.043 Uiso 1 1 calc R . . H30B H 0.5275 0.0470 0.6026 0.043 Uiso 1 1 calc R . . H30C H 0.6174 0.0395 0.5282 0.043 Uiso 1 1 calc R . . C31 C 0.5926(9) 0.0588(4) 0.2681(5) 0.0295(19) Uani 1 1 d . . . H31A H 0.6579 0.0384 0.3050 0.044 Uiso 1 1 calc R . . H31B H 0.5995 0.0422 0.2168 0.044 Uiso 1 1 calc R . . H31C H 0.4940 0.0551 0.2834 0.044 Uiso 1 1 calc R . . C32 C 1.1927(10) 0.0358(4) 0.3111(5) 0.034(2) Uani 1 1 d . . . H32A H 1.2838 0.0262 0.3392 0.051 Uiso 1 1 calc R . . H32B H 1.1901 0.0188 0.2597 0.051 Uiso 1 1 calc R . . H32C H 1.1130 0.0207 0.3389 0.051 Uiso 1 1 calc R . . O4 O 1.1828(7) 0.2237(3) 0.5876(3) 0.0322(14) Uani 1 1 d . . . H4 H 1.1871 0.2591 0.5788 0.048 Uiso 1 1 calc R . . O5 O 1.2469(7) 0.2799(3) 0.4546(3) 0.0324(14) Uani 1 1 d . . . H5 H 1.1900 0.2976 0.4238 0.049 Uiso 1 1 calc R . . O6 O 1.2504(6) 0.2188(3) 0.3168(3) 0.0318(14) Uani 1 1 d . . . H6 H 1.2781 0.2523 0.3274 0.048 Uiso 1 1 calc R . . O11 O 0.5931(6) 0.1431(3) 0.7188(3) 0.0321(14) Uani 1 1 d . . . H11 H 0.6053 0.1493 0.7662 0.048 Uiso 1 1 calc R . . O12 O 0.8374(6) 0.1562(3) 0.8119(3) 0.0291(13) Uani 1 1 d . . . H12 H 0.9195 0.1630 0.8324 0.044 Uiso 1 1 calc R . . O13 O 1.1026(6) 0.1396(3) 0.7558(3) 0.0271(13) Uani 1 1 d . . . H13 H 1.1274 0.1077 0.7750 0.041 Uiso 1 1 calc RD . . O18 O 0.6010(6) 0.2412(2) 0.2717(3) 0.0249(12) Uani 1 1 d . . . H18 H 0.6015 0.2769 0.2787 0.037 Uiso 1 1 calc R . . O19 O 0.5660(6) 0.3024(2) 0.4053(3) 0.0279(13) Uani 1 1 d . . . H19 H 0.6400 0.3196 0.4229 0.042 Uiso 1 1 calc R . . O20 O 0.5752(7) 0.2441(3) 0.5456(3) 0.0307(14) Uani 1 1 d . . . H20 H 0.5602 0.2789 0.5352 0.046 Uiso 1 1 calc R . . O25 O 1.1851(6) 0.1210(3) 0.1462(3) 0.0329(14) Uani 1 1 d . . . H25 H 1.1751 0.1201 0.0980 0.049 Uiso 1 1 calc R . . O26 O 0.9512(6) 0.1468(3) 0.0519(3) 0.0333(14) Uani 1 1 d . . . H26 H 0.8730 0.1566 0.0291 0.050 Uiso 1 1 calc R . . O27 O 0.6779(6) 0.1523(3) 0.1094(3) 0.0296(13) Uani 1 1 d . . . H27 H 0.6673 0.1274 0.0748 0.044 Uiso 1 1 calc R . . Br1 Br 0.82997(10) 0.37483(5) 0.48215(6) 0.0412(3) Uani 1 1 d . . . Cs1 Cs 0.87649(6) 0.26926(2) 0.63461(3) 0.03304(17) Uani 1 1 d . . . C50 C 0.9316(11) 0.2737(5) 0.3257(7) 0.032(3) Uani 0.75 1 d P A 1 H50C H 0.9327 0.2749 0.2696 0.048 Uiso 0.75 1 calc PR A 1 H50D H 0.8339 0.2808 0.3407 0.048 Uiso 0.75 1 calc PR A 1 H50E H 0.9635 0.2357 0.3442 0.048 Uiso 0.75 1 calc PR A 1 O50 O 1.0269(6) 0.3172(3) 0.3589(4) 0.0179(15) Uani 0.75 1 d P A 1 H50 H 0.9820 0.3381 0.3883 0.027 Uiso 0.75 1 calc PR A 1 O50B O 0.9130(18) 0.2657(8) 0.2296(10) 0.011(4) Uani 0.25 1 d P B 2 O51 O 1.3433(12) 0.0816(5) 0.7565(7) 0.032(3) Uani 0.50 1 d PD . . C52 C 1.080(2) 0.0146(6) 0.8665(10) 0.068(5) Uani 0.75 1 d P . . H52C H 1.0774 0.0015 0.8130 0.102 Uiso 0.35 1 calc PR C 1 H52D H 0.9908 0.0034 0.8892 0.102 Uiso 0.35 1 calc PR C 1 H52E H 1.1618 -0.0030 0.8957 0.102 Uiso 0.35 1 calc PR C 1 H52F H 1.0665 0.0039 0.8121 0.102 Uiso 0.40 1 calc PR C 2 H52G H 1.0379 0.0526 0.8740 0.102 Uiso 0.40 1 calc PR C 2 H52H H 1.0325 -0.0137 0.8977 0.102 Uiso 0.40 1 calc PR C 2 O52 O 1.091(4) 0.0626(14) 0.8683(19) 0.120(15) Uani 0.35 1 d P D 1 H52A H 1.0092 0.0777 0.8659 0.179 Uiso 0.35 1 calc PR D 1 O52B O 1.234(3) 0.0162(9) 0.8897(14) 0.076(7) Uani 0.40 1 d P D 2 H52B H 1.2757 0.0383 0.8604 0.115 Uiso 0.40 1 calc PR D 2 C53 C 0.685(2) 0.0455(8) -0.0625(11) 0.113(7) Uani 1 1 d . . . H53C H 0.6647 0.0083 -0.0394 0.170 Uiso 0.50 1 calc PR E 1 H53D H 0.7514 0.0399 -0.1033 0.170 Uiso 0.50 1 calc PR E 1 H53E H 0.5960 0.0626 -0.0842 0.170 Uiso 0.50 1 calc PR E 1 H53F H 0.7764 0.0244 -0.0608 0.170 Uiso 0.50 1 calc PR E 2 H53G H 0.6942 0.0807 -0.0926 0.170 Uiso 0.50 1 calc PR E 2 H53H H 0.6089 0.0214 -0.0865 0.170 Uiso 0.50 1 calc PR E 2 O53 O 0.741(2) 0.0777(15) -0.013(2) 0.161(19) Uani 0.50 1 d P F 1 H53 H 0.8204 0.0639 0.0041 0.242 Uiso 0.50 1 calc PRD F 1 O53B O 0.648(3) 0.0614(11) 0.0214(16) 0.110(10) Uani 0.50 1 d PD F 2 H53B H 0.621(18) 0.043(15) 0.057(18) 0.165 Uiso 0.50 1 d PD G 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 0.012(3) 0.036(5) 0.018(4) 0.001(3) 0.004(3) 0.000(3) C2 0.012(4) 0.034(5) 0.027(4) 0.001(4) -0.001(3) 0.001(3) C3 0.014(4) 0.039(5) 0.016(4) 0.004(3) -0.004(3) 0.001(3) C4 0.016(4) 0.039(5) 0.025(4) 0.002(4) -0.006(3) -0.005(3) C5 0.020(4) 0.040(5) 0.025(4) 0.006(4) 0.002(3) -0.005(4) C6 0.015(4) 0.041(5) 0.019(4) 0.005(4) 0.002(3) -0.004(3) C7 0.013(4) 0.038(5) 0.020(4) 0.002(3) 0.002(3) 0.002(3) C8 0.015(4) 0.023(4) 0.020(4) 0.002(3) 0.005(3) 0.000(3) C9 0.024(4) 0.028(4) 0.014(4) 0.004(3) 0.000(3) 0.003(3) C10 0.021(4) 0.019(4) 0.023(4) 0.001(3) 0.000(3) 0.000(3) C11 0.018(4) 0.024(4) 0.029(4) 0.000(3) 0.007(3) 0.003(3) C12 0.016(4) 0.026(4) 0.032(5) -0.001(4) -0.003(3) 0.004(3) C13 0.017(4) 0.022(4) 0.018(4) -0.001(3) -0.005(3) 0.005(3) C14 0.024(4) 0.034(5) 0.011(4) 0.004(3) 0.001(3) 0.001(3) C15 0.014(4) 0.033(5) 0.021(4) -0.005(3) -0.004(3) 0.001(3) C16 0.018(4) 0.024(4) 0.024(4) 0.003(3) -0.001(3) 0.001(3) C17 0.012(3) 0.028(4) 0.024(4) -0.002(3) -0.001(3) 0.001(3) C18 0.013(4) 0.033(5) 0.024(4) 0.004(3) 0.003(3) 0.001(3) C19 0.023(4) 0.022(4) 0.021(4) -0.005(3) -0.001(3) 0.000(3) C20 0.012(3) 0.034(5) 0.016(4) 0.000(3) 0.002(3) -0.001(3) C21 0.014(4) 0.029(4) 0.019(4) 0.004(3) -0.001(3) -0.001(3) C22 0.021(4) 0.020(4) 0.021(4) -0.001(3) 0.006(3) 0.000(3) C23 0.025(4) 0.028(4) 0.019(4) 0.005(3) 0.003(3) 0.000(3) C24 0.023(4) 0.023(4) 0.024(4) 0.000(3) -0.001(3) 0.000(3) C25 0.022(4) 0.029(5) 0.025(4) -0.001(4) -0.001(3) -0.006(3) C26 0.033(4) 0.035(5) 0.004(3) 0.000(3) 0.007(3) -0.004(4) C27 0.027(4) 0.020(4) 0.022(4) 0.001(3) 0.000(3) -0.003(3) C28 0.017(4) 0.039(5) 0.025(4) 0.005(4) 0.001(3) 0.000(4) C29 0.025(4) 0.042(5) 0.025(4) 0.006(4) 0.008(3) 0.005(4) C30 0.025(4) 0.033(5) 0.027(4) 0.002(4) -0.004(3) -0.008(4) C31 0.027(4) 0.033(5) 0.028(5) -0.006(4) 0.002(4) -0.003(4) C32 0.032(5) 0.038(5) 0.030(5) 0.003(4) -0.004(4) 0.001(4) O4 0.039(3) 0.035(3) 0.023(3) -0.003(3) -0.001(3) -0.009(3) O5 0.037(3) 0.034(4) 0.025(3) 0.007(3) -0.008(3) -0.012(3) O6 0.032(3) 0.040(4) 0.024(3) 0.008(3) 0.000(3) -0.008(3) O11 0.022(3) 0.054(4) 0.020(3) -0.004(3) 0.003(2) 0.002(3) O12 0.021(3) 0.046(4) 0.021(3) -0.005(3) -0.001(2) -0.001(3) O13 0.020(3) 0.034(3) 0.027(3) 0.003(3) -0.006(2) -0.003(2) O18 0.024(3) 0.031(3) 0.020(3) 0.006(2) 0.004(2) -0.003(3) O19 0.030(3) 0.024(3) 0.028(3) -0.001(2) -0.006(3) 0.000(2) O20 0.038(3) 0.030(3) 0.023(3) -0.005(2) -0.003(3) 0.000(3) O25 0.024(3) 0.060(4) 0.016(3) 0.001(3) 0.008(2) -0.006(3) O26 0.029(3) 0.053(4) 0.018(3) 0.005(3) 0.001(2) -0.005(3) O27 0.025(3) 0.039(4) 0.023(3) 0.001(3) -0.006(2) 0.002(3) Br1 0.0356(5) 0.0567(6) 0.0313(5) 0.0002(4) 0.0024(4) -0.0060(5) Cs1 0.0326(3) 0.0313(3) 0.0335(3) 0.0038(2) -0.0111(2) -0.0029(2) C50 0.015(5) 0.043(7) 0.040(7) 0.009(6) 0.003(5) -0.007(5) O50 0.007(3) 0.030(4) 0.017(4) 0.007(3) 0.004(3) 0.000(3) O50B 0.005(8) 0.012(9) 0.017(10) 0.001(8) 0.000(7) -0.006(7) O51 0.019(6) 0.031(7) 0.044(7) -0.003(6) -0.005(5) 0.007(5) C52 0.104(15) 0.026(8) 0.068(11) 0.010(7) -0.033(10) -0.012(8) O52 0.18(3) 0.09(2) 0.08(2) 0.045(18) -0.09(2) -0.07(2) O52B 0.105(19) 0.035(12) 0.086(17) -0.008(11) -0.020(15) -0.006(12) C53 0.147(18) 0.084(12) 0.117(15) 0.025(11) 0.068(14) 0.029(12) O53 0.037(12) 0.18(3) 0.26(4) -0.17(3) -0.037(17) 0.018(15) O53B 0.12(2) 0.085(18) 0.12(2) -0.061(15) -0.055(18) 0.043(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 C6 1.391(12) . ? C1 C2 1.405(11) . ? C1 C28 1.508(11) . ? C2 C3 1.401(11) . ? C3 C4 1.397(12) . ? C3 C7 1.509(11) . ? C4 O4 1.376(10) . ? C4 C5 1.398(11) . ? C5 C6 1.387(12) . ? C5 O5 1.386(10) . ? C6 O6 1.383(9) . ? C7 C8 1.518(10) . ? C7 C29 1.526(12) . ? C8 C9 1.402(10) . ? C8 C13 1.436(10) . ? C8 Cs1 3.625(8) . ? C9 C10 1.365(11) . ? C9 Cs1 3.589(8) . ? C10 C11 1.405(11) . ? C10 C14 1.530(10) . ? C10 Cs1 3.567(8) . ? C11 O11 1.380(9) . ? C11 C12 1.382(11) . ? C11 Cs1 3.537(8) . ? C12 C13 1.373(11) . ? C12 O12 1.381(10) . ? C12 Cs1 3.464(8) . ? C13 O13 1.392(9) . ? C13 Cs1 3.538(7) . ? C14 C15 1.502(11) . ? C14 C30 1.527(11) . ? C15 C20 1.398(11) . ? C15 C16 1.414(11) . ? C16 C17 1.383(11) . ? C17 C18 1.398(11) . ? C17 C21 1.525(11) . ? C18 O18 1.374(9) . ? C18 C19 1.382(11) . ? C19 O19 1.393(9) . ? C19 C20 1.403(11) . ? C20 O20 1.357(9) . ? C20 Cs1 3.905(7) . ? C21 C22 1.525(10) . ? C21 C31 1.537(11) . ? C22 C27 1.377(11) . ? C22 C23 1.412(11) . ? C23 C24 1.394(11) . ? C24 C25 1.386(11) . ? C24 C28 1.526(11) . ? C25 O25 1.374(10) . ? C25 C26 1.387(11) . ? C26 C27 1.381(11) . ? C26 O26 1.384(9) . ? C27 O27 1.399(9) . ? C28 C32 1.542(12) . ? Br1 Cs1 3.6264(12) . ? Cs1 O18 3.085(5) 4_666 ? Cs1 O25 3.132(6) 4_566 ? Cs1 O27 3.408(6) 4_666 ? Cs1 O6 3.472(6) 4_566 ? C50 O50 1.444(13) . ? C52 O52 1.12(3) . ? C52 O52B 1.47(3) . ? C53 O53 1.24(3) . ? C53 O53B 1.57(3) . ? 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 116.9(7) . . ? C6 C1 C28 119.8(7) . . ? C2 C1 C28 123.3(8) . . ? C3 C2 C1 123.4(8) . . ? C4 C3 C2 117.3(7) . . ? C4 C3 C7 119.5(7) . . ? C2 C3 C7 123.1(8) . . ? O4 C4 C3 118.3(7) . . ? O4 C4 C5 121.1(8) . . ? C3 C4 C5 120.6(8) . . ? C6 C5 O5 121.7(7) . . ? C6 C5 C4 120.2(8) . . ? O5 C5 C4 118.1(8) . . ? O6 C6 C5 119.5(8) . . ? O6 C6 C1 119.0(7) . . ? C5 C6 C1 121.5(7) . . ? C3 C7 C8 112.1(6) . . ? C3 C7 C29 115.1(7) . . ? C8 C7 C29 108.3(6) . . ? C9 C8 C13 115.1(7) . . ? C9 C8 C7 122.4(7) . . ? C13 C8 C7 122.2(7) . . ? C9 C8 Cs1 77.4(5) . . ? C13 C8 Cs1 75.1(4) . . ? C7 C8 Cs1 121.2(5) . . ? C10 C9 C8 124.6(7) . . ? C10 C9 Cs1 78.1(5) . . ? C8 C9 Cs1 80.2(5) . . ? C9 C10 C11 117.7(7) . . ? C9 C10 C14 123.6(7) . . ? C11 C10 C14 118.6(7) . . ? C9 C10 Cs1 79.9(5) . . ? C11 C10 Cs1 77.4(5) . . ? C14 C10 Cs1 115.2(5) . . ? O11 C11 C12 119.3(7) . . ? O11 C11 C10 119.9(7) . . ? C12 C11 C10 120.7(7) . . ? O11 C11 Cs1 113.5(5) . . ? C12 C11 Cs1 75.6(5) . . ? C10 C11 Cs1 79.8(5) . . ? C13 C12 O12 120.8(7) . . ? C13 C12 C11 120.1(8) . . ? O12 C12 C11 119.1(7) . . ? C13 C12 Cs1 81.7(5) . . ? O12 C12 Cs1 107.4(5) . . ? C11 C12 Cs1 81.6(5) . . ? C12 C13 O13 118.7(7) . . ? C12 C13 C8 121.4(7) . . ? O13 C13 C8 119.6(7) . . ? C12 C13 Cs1 75.7(5) . . ? O13 C13 Cs1 107.8(4) . . ? C8 C13 Cs1 81.9(4) . . ? C15 C14 C30 114.0(7) . . ? C15 C14 C10 112.1(6) . . ? C30 C14 C10 109.5(6) . . ? C20 C15 C16 116.9(7) . . ? C20 C15 C14 118.9(7) . . ? C16 C15 C14 124.1(7) . . ? C17 C16 C15 123.2(7) . . ? C16 C17 C18 118.3(7) . . ? C16 C17 C21 123.1(7) . . ? C18 C17 C21 118.5(7) . . ? O18 C18 C19 121.6(7) . . ? O18 C18 C17 118.2(7) . . ? C19 C18 C17 120.1(7) . . ? C18 C19 O19 118.6(7) . . ? C18 C19 C20 121.0(7) . . ? O19 C19 C20 120.4(7) . . ? O20 C20 C15 119.2(7) . . ? O20 C20 C19 120.3(7) . . ? C15 C20 C19 120.4(7) . . ? O20 C20 Cs1 48.8(4) . . ? C15 C20 Cs1 104.0(5) . . ? C19 C20 Cs1 113.9(5) . . ? C17 C21 C22 113.8(6) . . ? C17 C21 C31 114.3(6) . . ? C22 C21 C31 108.9(6) . . ? C27 C22 C23 117.4(7) . . ? C27 C22 C21 121.4(7) . . ? C23 C22 C21 121.1(7) . . ? C24 C23 C22 122.8(7) . . ? C25 C24 C23 117.3(7) . . ? C25 C24 C28 119.9(7) . . ? C23 C24 C28 122.6(7) . . ? O25 C25 C24 118.1(7) . . ? O25 C25 C26 121.0(7) . . ? C24 C25 C26 120.9(7) . . ? C27 C26 O26 122.9(7) . . ? C27 C26 C25 120.5(7) . . ? O26 C26 C25 116.6(7) . . ? C22 C27 C26 121.1(7) . . ? C22 C27 O27 120.2(7) . . ? C26 C27 O27 118.8(7) . . ? C1 C28 C24 112.0(7) . . ? C1 C28 C32 114.2(7) . . ? C24 C28 C32 109.6(7) . . ? O18 Cs1 O25 112.10(15) 4_666 4_566 ? O18 Cs1 O27 67.46(14) 4_666 4_666 ? O25 Cs1 O27 92.96(15) 4_566 4_666 ? O18 Cs1 C12 66.99(17) 4_666 . ? O25 Cs1 C12 126.98(17) 4_566 . ? O27 Cs1 C12 127.91(16) 4_666 . ? O18 Cs1 O6 63.34(14) 4_666 4_566 ? O25 Cs1 O6 69.26(14) 4_566 4_566 ? O27 Cs1 O6 114.07(14) 4_666 4_566 ? C12 Cs1 O6 64.01(17) . 4_566 ? O18 Cs1 C11 89.50(17) 4_666 . ? O25 Cs1 C11 116.84(17) 4_566 . ? O27 Cs1 C11 148.06(16) 4_666 . ? C12 Cs1 C11 22.73(18) . . ? O6 Cs1 C11 70.28(17) 4_566 . ? O18 Cs1 C13 59.76(16) 4_666 . ? O25 Cs1 C13 148.73(16) 4_566 . ? O27 Cs1 C13 108.66(16) 4_666 . ? C12 Cs1 C13 22.59(18) . . ? O6 Cs1 C13 81.16(16) 4_566 . ? C11 Cs1 C13 39.45(17) . . ? O18 Cs1 C10 104.98(16) 4_666 . ? O25 Cs1 C10 123.04(17) 4_566 . ? O27 Cs1 C10 141.80(16) 4_666 . ? C12 Cs1 C10 40.28(18) . . ? O6 Cs1 C10 92.37(16) 4_566 . ? C11 Cs1 C10 22.81(18) . . ? C13 Cs1 C10 46.30(17) . . ? O18 Cs1 C9 97.64(16) 4_666 . ? O25 Cs1 C9 142.70(17) 4_566 . ? O27 Cs1 C9 119.82(16) 4_666 . ? C12 Cs1 C9 45.83(18) . . ? O6 Cs1 C9 107.86(16) 4_566 . ? C11 Cs1 C9 38.86(18) . . ? C13 Cs1 C9 39.28(17) . . ? C10 Cs1 C9 21.98(17) . . ? O18 Cs1 C8 76.25(16) 4_666 . ? O25 Cs1 C8 162.45(16) 4_566 . ? O27 Cs1 C8 104.58(15) 4_666 . ? C12 Cs1 C8 40.36(18) . . ? O6 Cs1 C8 103.38(16) 4_566 . ? C11 Cs1 C8 46.29(17) . . ? C13 Cs1 C8 23.10(17) . . ? C10 Cs1 C8 39.82(17) . . ? C9 Cs1 C8 22.41(17) . . ? O18 Cs1 Br1 131.64(11) 4_666 . ? O25 Cs1 Br1 56.86(10) 4_566 . ? O27 Cs1 Br1 66.59(10) 4_666 . ? C12 Cs1 Br1 160.51(13) . . ? O6 Cs1 Br1 125.82(10) 4_566 . ? C11 Cs1 Br1 138.73(13) . . ? C13 Cs1 Br1 152.75(13) . . ? C10 Cs1 Br1 120.29(12) . . ? C9 Cs1 Br1 117.71(12) . . ? C8 Cs1 Br1 129.80(12) . . ? O18 Cs1 C20 156.07(16) 4_666 . ? O25 Cs1 C20 86.62(16) 4_566 . ? O27 Cs1 C20 128.60(14) 4_666 . ? C12 Cs1 C20 90.02(18) . . ? O6 Cs1 C20 113.61(15) 4_566 . ? C11 Cs1 C20 68.14(18) . . ? C13 Cs1 C20 96.45(17) . . ? C10 Cs1 C20 51.14(17) . . ? C9 Cs1 C20 59.70(17) . . ? C8 Cs1 C20 81.87(17) . . ? Br1 Cs1 C20 70.71(12) . . ? O52 C52 O52B 83(2) . . ? O53 C53 O53B 46.5(19) . . ? 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 1.3(11) . . . . ? C28 C1 C2 C3 -178.1(7) . . . . ? C1 C2 C3 C4 0.9(11) . . . . ? C1 C2 C3 C7 -176.6(7) . . . . ? C2 C3 C4 O4 178.0(7) . . . . ? C7 C3 C4 O4 -4.4(11) . . . . ? C2 C3 C4 C5 -1.9(11) . . . . ? C7 C3 C4 C5 175.6(7) . . . . ? O4 C4 C5 C6 -179.2(7) . . . . ? C3 C4 C5 C6 0.7(12) . . . . ? O4 C4 C5 O5 1.8(11) . . . . ? C3 C4 C5 O5 -178.3(7) . . . . ? O5 C5 C6 O6 0.6(12) . . . . ? C4 C5 C6 O6 -178.4(7) . . . . ? O5 C5 C6 C1 -179.4(7) . . . . ? C4 C5 C6 C1 1.7(12) . . . . ? C2 C1 C6 O6 177.4(7) . . . . ? C28 C1 C6 O6 -3.2(11) . . . . ? C2 C1 C6 C5 -2.6(11) . . . . ? C28 C1 C6 C5 176.8(7) . . . . ? C4 C3 C7 C8 71.9(9) . . . . ? C2 C3 C7 C8 -110.7(8) . . . . ? C4 C3 C7 C29 -163.8(7) . . . . ? C2 C3 C7 C29 13.6(10) . . . . ? C3 C7 C8 C9 47.7(10) . . . . ? C29 C7 C8 C9 -80.4(9) . . . . ? C3 C7 C8 C13 -138.4(8) . . . . ? C29 C7 C8 C13 93.6(9) . . . . ? C3 C7 C8 Cs1 -47.0(8) . . . . ? C29 C7 C8 Cs1 -175.0(5) . . . . ? C13 C8 C9 C10 -1.5(12) . . . . ? C7 C8 C9 C10 172.8(8) . . . . ? Cs1 C8 C9 C10 -68.1(8) . . . . ? C13 C8 C9 Cs1 66.6(6) . . . . ? C7 C8 C9 Cs1 -119.1(7) . . . . ? C8 C9 C10 C11 -0.8(12) . . . . ? Cs1 C9 C10 C11 -69.9(7) . . . . ? C8 C9 C10 C14 -177.3(7) . . . . ? Cs1 C9 C10 C14 113.6(7) . . . . ? C8 C9 C10 Cs1 69.1(8) . . . . ? C9 C10 C11 O11 -177.4(7) . . . . ? C14 C10 C11 O11 -0.7(11) . . . . ? Cs1 C10 C11 O11 111.3(7) . . . . ? C9 C10 C11 C12 4.9(12) . . . . ? C14 C10 C11 C12 -178.4(7) . . . . ? Cs1 C10 C11 C12 -66.4(7) . . . . ? C9 C10 C11 Cs1 71.3(7) . . . . ? C14 C10 C11 Cs1 -112.0(7) . . . . ? O11 C11 C12 C13 175.6(7) . . . . ? C10 C11 C12 C13 -6.7(12) . . . . ? Cs1 C11 C12 C13 -75.3(7) . . . . ? O11 C11 C12 O12 -3.8(12) . . . . ? C10 C11 C12 O12 173.9(7) . . . . ? Cs1 C11 C12 O12 105.3(7) . . . . ? O11 C11 C12 Cs1 -109.1(7) . . . . ? C10 C11 C12 Cs1 68.6(7) . . . . ? O12 C12 C13 O13 -2.7(12) . . . . ? C11 C12 C13 O13 177.9(7) . . . . ? Cs1 C12 C13 O13 102.7(6) . . . . ? O12 C12 C13 C8 -176.3(7) . . . . ? C11 C12 C13 C8 4.3(12) . . . . ? Cs1 C12 C13 C8 -70.9(7) . . . . ? O12 C12 C13 Cs1 -105.4(7) . . . . ? C11 C12 C13 Cs1 75.3(7) . . . . ? C9 C8 C13 C12 -0.3(11) . . . . ? C7 C8 C13 C12 -174.6(7) . . . . ? Cs1 C8 C13 C12 67.7(7) . . . . ? C9 C8 C13 O13 -173.8(7) . . . . ? C7 C8 C13 O13 11.8(11) . . . . ? Cs1 C8 C13 O13 -105.9(7) . . . . ? C9 C8 C13 Cs1 -68.0(6) . . . . ? C7 C8 C13 Cs1 117.7(7) . . . . ? C9 C10 C14 C15 -43.0(11) . . . . ? C11 C10 C14 C15 140.6(7) . . . . ? Cs1 C10 C14 C15 51.6(8) . . . . ? C9 C10 C14 C30 84.7(9) . . . . ? C11 C10 C14 C30 -91.8(9) . . . . ? Cs1 C10 C14 C30 179.3(5) . . . . ? C30 C14 C15 C20 154.7(7) . . . . ? C10 C14 C15 C20 -80.0(9) . . . . ? C30 C14 C15 C16 -22.2(11) . . . . ? C10 C14 C15 C16 103.0(9) . . . . ? C20 C15 C16 C17 -0.6(11) . . . . ? C14 C15 C16 C17 176.4(7) . . . . ? C15 C16 C17 C18 0.0(11) . . . . ? C15 C16 C17 C21 -178.3(7) . . . . ? C16 C17 C18 O18 -177.5(6) . . . . ? C21 C17 C18 O18 0.9(10) . . . . ? C16 C17 C18 C19 0.4(11) . . . . ? C21 C17 C18 C19 178.8(7) . . . . ? O18 C18 C19 O19 1.4(11) . . . . ? C17 C18 C19 O19 -176.4(7) . . . . ? O18 C18 C19 C20 177.7(7) . . . . ? C17 C18 C19 C20 -0.2(12) . . . . ? C16 C15 C20 O20 -178.6(7) . . . . ? C14 C15 C20 O20 4.3(11) . . . . ? C16 C15 C20 C19 0.8(11) . . . . ? C14 C15 C20 C19 -176.4(7) . . . . ? C16 C15 C20 Cs1 -128.3(6) . . . . ? C14 C15 C20 Cs1 54.5(7) . . . . ? C18 C19 C20 O20 179.0(7) . . . . ? O19 C19 C20 O20 -4.9(11) . . . . ? C18 C19 C20 C15 -0.4(11) . . . . ? O19 C19 C20 C15 175.7(7) . . . . ? C18 C19 C20 Cs1 124.1(7) . . . . ? O19 C19 C20 Cs1 -59.8(8) . . . . ? C16 C17 C21 C22 -105.1(8) . . . . ? C18 C17 C21 C22 76.6(9) . . . . ? C16 C17 C21 C31 20.8(10) . . . . ? C18 C17 C21 C31 -157.5(7) . . . . ? C17 C21 C22 C27 -136.9(8) . . . . ? C31 C21 C22 C27 94.4(9) . . . . ? C17 C21 C22 C23 48.1(10) . . . . ? C31 C21 C22 C23 -80.6(9) . . . . ? C27 C22 C23 C24 -2.5(12) . . . . ? C21 C22 C23 C24 172.7(7) . . . . ? C22 C23 C24 C25 -0.3(12) . . . . ? C22 C23 C24 C28 -175.4(8) . . . . ? C23 C24 C25 O25 -177.3(7) . . . . ? C28 C24 C25 O25 -2.0(12) . . . . ? C23 C24 C25 C26 2.8(12) . . . . ? C28 C24 C25 C26 178.0(8) . . . . ? O25 C25 C26 C27 177.5(8) . . . . ? C24 C25 C26 C27 -2.5(13) . . . . ? O25 C25 C26 O26 -2.5(12) . . . . ? C24 C25 C26 O26 177.4(7) . . . . ? C23 C22 C27 C26 2.8(12) . . . . ? C21 C22 C27 C26 -172.3(7) . . . . ? C23 C22 C27 O27 -175.9(7) . . . . ? C21 C22 C27 O27 8.9(11) . . . . ? O26 C26 C27 C22 179.7(7) . . . . ? C25 C26 C27 C22 -0.4(13) . . . . ? O26 C26 C27 O27 -1.6(12) . . . . ? C25 C26 C27 O27 178.3(7) . . . . ? C6 C1 C28 C24 -74.3(9) . . . . ? C2 C1 C28 C24 105.1(9) . . . . ? C6 C1 C28 C32 160.5(7) . . . . ? C2 C1 C28 C32 -20.2(11) . . . . ? C25 C24 C28 C1 139.6(8) . . . . ? C23 C24 C28 C1 -45.5(11) . . . . ? C25 C24 C28 C32 -92.7(9) . . . . ? C23 C24 C28 C32 82.3(10) . . . . ? C13 C12 Cs1 O18 -66.2(4) . . . 4_666 ? O12 C12 Cs1 O18 53.6(4) . . . 4_666 ? C11 C12 Cs1 O18 171.5(5) . . . 4_666 ? C13 C12 Cs1 O25 -167.3(4) . . . 4_566 ? O12 C12 Cs1 O25 -47.5(5) . . . 4_566 ? C11 C12 Cs1 O25 70.4(5) . . . 4_566 ? C13 C12 Cs1 O27 -35.3(5) . . . 4_666 ? O12 C12 Cs1 O27 84.4(5) . . . 4_666 ? C11 C12 Cs1 O27 -157.6(4) . . . 4_666 ? C13 C12 Cs1 O6 -136.6(5) . . . 4_566 ? O12 C12 Cs1 O6 -16.9(4) . . . 4_566 ? C11 C12 Cs1 O6 101.1(5) . . . 4_566 ? C13 C12 Cs1 C11 122.3(7) . . . . ? O12 C12 Cs1 C11 -118.0(7) . . . . ? O12 C12 Cs1 C13 119.8(7) . . . . ? C11 C12 Cs1 C13 -122.3(7) . . . . ? C13 C12 Cs1 C10 93.1(5) . . . . ? O12 C12 Cs1 C10 -147.1(6) . . . . ? C11 C12 Cs1 C10 -29.2(4) . . . . ? C13 C12 Cs1 C9 61.7(5) . . . . ? O12 C12 Cs1 C9 -178.6(6) . . . . ? C11 C12 Cs1 C9 -60.6(5) . . . . ? C13 C12 Cs1 C8 29.6(4) . . . . ? O12 C12 Cs1 C8 149.3(6) . . . . ? C11 C12 Cs1 C8 -92.7(5) . . . . ? C13 C12 Cs1 Br1 98.4(5) . . . . ? O12 C12 Cs1 Br1 -141.9(4) . . . . ? C11 C12 Cs1 Br1 -23.9(8) . . . . ? C13 C12 Cs1 C20 107.0(5) . . . . ? O12 C12 Cs1 C20 -133.3(4) . . . . ? C11 C12 Cs1 C20 -15.3(5) . . . . ? O11 C11 Cs1 O18 108.3(5) . . . 4_666 ? C12 C11 Cs1 O18 -7.8(5) . . . 4_666 ? C10 C11 Cs1 O18 -133.4(4) . . . 4_666 ? O11 C11 Cs1 O25 -6.4(6) . . . 4_566 ? C12 C11 Cs1 O25 -122.5(5) . . . 4_566 ? C10 C11 Cs1 O25 111.9(4) . . . 4_566 ? O11 C11 Cs1 O27 150.7(4) . . . 4_666 ? C12 C11 Cs1 O27 34.6(6) . . . 4_666 ? C10 C11 Cs1 O27 -91.0(5) . . . 4_666 ? O11 C11 Cs1 C12 116.1(8) . . . . ? C10 C11 Cs1 C12 -125.6(7) . . . . ? O11 C11 Cs1 O6 46.5(5) . . . 4_566 ? C12 C11 Cs1 O6 -69.5(5) . . . 4_566 ? C10 C11 Cs1 O6 164.8(5) . . . 4_566 ? O11 C11 Cs1 C13 146.8(7) . . . . ? C12 C11 Cs1 C13 30.7(4) . . . . ? C10 C11 Cs1 C13 -94.9(5) . . . . ? O11 C11 Cs1 C10 -118.3(8) . . . . ? C12 C11 Cs1 C10 125.6(7) . . . . ? O11 C11 Cs1 C9 -148.9(7) . . . . ? C12 C11 Cs1 C9 95.1(5) . . . . ? C10 C11 Cs1 C9 -30.5(4) . . . . ? O11 C11 Cs1 C8 179.6(6) . . . . ? C12 C11 Cs1 C8 63.5(5) . . . . ? C10 C11 Cs1 C8 -62.1(4) . . . . ? O11 C11 Cs1 Br1 -75.8(6) . . . . ? C12 C11 Cs1 Br1 168.2(4) . . . . ? C10 C11 Cs1 Br1 42.5(5) . . . . ? O11 C11 Cs1 C20 -80.5(5) . . . . ? C12 C11 Cs1 C20 163.4(5) . . . . ? C10 C11 Cs1 C20 37.8(4) . . . . ? C12 C13 Cs1 O18 102.9(5) . . . 4_666 ? O13 C13 Cs1 O18 -13.1(4) . . . 4_666 ? C8 C13 Cs1 O18 -131.7(5) . . . 4_666 ? C12 C13 Cs1 O25 19.8(6) . . . 4_566 ? O13 C13 Cs1 O25 -96.2(5) . . . 4_566 ? C8 C13 Cs1 O25 145.2(4) . . . 4_566 ? C12 C13 Cs1 O27 151.2(4) . . . 4_666 ? O13 C13 Cs1 O27 35.2(5) . . . 4_666 ? C8 C13 Cs1 O27 -83.4(4) . . . 4_666 ? O13 C13 Cs1 C12 -116.0(7) . . . . ? C8 C13 Cs1 C12 125.4(7) . . . . ? C12 C13 Cs1 O6 38.7(5) . . . 4_566 ? O13 C13 Cs1 O6 -77.3(5) . . . 4_566 ? C8 C13 Cs1 O6 164.1(4) . . . 4_566 ? C12 C13 Cs1 C11 -30.9(4) . . . . ? O13 C13 Cs1 C11 -147.0(6) . . . . ? C8 C13 Cs1 C11 94.4(5) . . . . ? C12 C13 Cs1 C10 -63.2(5) . . . . ? O13 C13 Cs1 C10 -179.3(6) . . . . ? C8 C13 Cs1 C10 62.1(4) . . . . ? C12 C13 Cs1 C9 -94.2(5) . . . . ? O13 C13 Cs1 C9 149.8(6) . . . . ? C8 C13 Cs1 C9 31.2(4) . . . . ? C12 C13 Cs1 C8 -125.4(7) . . . . ? O13 C13 Cs1 C8 118.6(7) . . . . ? C12 C13 Cs1 Br1 -133.9(4) . . . . ? O13 C13 Cs1 Br1 110.1(4) . . . . ? C8 C13 Cs1 Br1 -8.5(6) . . . . ? C12 C13 Cs1 C20 -74.3(5) . . . . ? O13 C13 Cs1 C20 169.7(5) . . . . ? C8 C13 Cs1 C20 51.1(4) . . . . ? C9 C10 Cs1 O18 -72.8(5) . . . 4_666 ? C11 C10 Cs1 O18 48.8(5) . . . 4_666 ? C14 C10 Cs1 O18 164.6(5) . . . 4_666 ? C9 C10 Cs1 O25 157.5(4) . . . 4_566 ? C11 C10 Cs1 O25 -80.9(5) . . . 4_566 ? C14 C10 Cs1 O25 35.0(6) . . . 4_566 ? C9 C10 Cs1 O27 -0.4(6) . . . 4_666 ? C11 C10 Cs1 O27 121.2(4) . . . 4_666 ? C14 C10 Cs1 O27 -122.9(5) . . . 4_666 ? C9 C10 Cs1 C12 -92.5(5) . . . . ? C11 C10 Cs1 C12 29.1(4) . . . . ? C14 C10 Cs1 C12 145.0(6) . . . . ? C9 C10 Cs1 O6 -135.8(4) . . . 4_566 ? C11 C10 Cs1 O6 -14.3(4) . . . 4_566 ? C14 C10 Cs1 O6 101.6(5) . . . 4_566 ? C9 C10 Cs1 C11 -121.6(7) . . . . ? C14 C10 Cs1 C11 115.9(7) . . . . ? C9 C10 Cs1 C13 -60.5(4) . . . . ? C11 C10 Cs1 C13 61.1(4) . . . . ? C14 C10 Cs1 C13 177.0(6) . . . . ? C11 C10 Cs1 C9 121.6(7) . . . . ? C14 C10 Cs1 C9 -122.5(8) . . . . ? C9 C10 Cs1 C8 -27.7(4) . . . . ? C11 C10 Cs1 C8 93.9(5) . . . . ? C14 C10 Cs1 C8 -150.2(6) . . . . ? C9 C10 Cs1 Br1 89.5(4) . . . . ? C11 C10 Cs1 Br1 -148.9(4) . . . . ? C14 C10 Cs1 Br1 -33.0(5) . . . . ? C9 C10 Cs1 C20 105.4(5) . . . . ? C11 C10 Cs1 C20 -133.0(5) . . . . ? C14 C10 Cs1 C20 -17.1(4) . . . . ? C10 C9 Cs1 O18 111.4(5) . . . 4_666 ? C8 C9 Cs1 O18 -17.3(5) . . . 4_666 ? C10 C9 Cs1 O25 -32.0(6) . . . 4_566 ? C8 C9 Cs1 O25 -160.7(4) . . . 4_566 ? C10 C9 Cs1 O27 179.7(4) . . . 4_666 ? C8 C9 Cs1 O27 51.0(5) . . . 4_666 ? C10 C9 Cs1 C12 64.2(5) . . . . ? C8 C9 Cs1 C12 -64.5(4) . . . . ? C10 C9 Cs1 O6 47.0(5) . . . 4_566 ? C8 C9 Cs1 O6 -81.7(4) . . . 4_566 ? C10 C9 Cs1 C11 31.8(4) . . . . ? C8 C9 Cs1 C11 -96.9(5) . . . . ? C10 C9 Cs1 C13 96.5(5) . . . . ? C8 C9 Cs1 C13 -32.2(4) . . . . ? C8 C9 Cs1 C10 -128.7(7) . . . . ? C10 C9 Cs1 C8 128.7(7) . . . . ? C10 C9 Cs1 Br1 -102.8(4) . . . . ? C8 C9 Cs1 Br1 128.5(4) . . . . ? C10 C9 Cs1 C20 -60.4(4) . . . . ? C8 C9 Cs1 C20 170.9(5) . . . . ? C9 C8 Cs1 O18 162.3(5) . . . 4_666 ? C13 C8 Cs1 O18 41.6(4) . . . 4_666 ? C7 C8 Cs1 O18 -77.3(5) . . . 4_666 ? C9 C8 Cs1 O25 41.6(8) . . . 4_566 ? C13 C8 Cs1 O25 -79.1(7) . . . 4_566 ? C7 C8 Cs1 O25 162.0(5) . . . 4_566 ? C9 C8 Cs1 O27 -135.8(4) . . . 4_666 ? C13 C8 Cs1 O27 103.5(4) . . . 4_666 ? C7 C8 Cs1 O27 -15.4(6) . . . 4_666 ? C9 C8 Cs1 C12 91.8(5) . . . . ? C13 C8 Cs1 C12 -28.9(4) . . . . ? C7 C8 Cs1 C12 -147.8(7) . . . . ? C9 C8 Cs1 O6 104.5(4) . . . 4_566 ? C13 C8 Cs1 O6 -16.2(4) . . . 4_566 ? C7 C8 Cs1 O6 -135.1(5) . . . 4_566 ? C9 C8 Cs1 C11 59.5(4) . . . . ? C13 C8 Cs1 C11 -61.2(4) . . . . ? C7 C8 Cs1 C11 179.9(7) . . . . ? C9 C8 Cs1 C13 120.7(7) . . . . ? C7 C8 Cs1 C13 -118.9(8) . . . . ? C9 C8 Cs1 C10 27.1(4) . . . . ? C13 C8 Cs1 C10 -93.6(5) . . . . ? C7 C8 Cs1 C10 147.5(7) . . . . ? C13 C8 Cs1 C9 -120.7(7) . . . . ? C7 C8 Cs1 C9 120.4(8) . . . . ? C9 C8 Cs1 Br1 -64.4(5) . . . . ? C13 C8 Cs1 Br1 174.9(4) . . . . ? C7 C8 Cs1 Br1 56.0(6) . . . . ? C9 C8 Cs1 C20 -7.9(4) . . . . ? C13 C8 Cs1 C20 -128.6(4) . . . . ? C7 C8 Cs1 C20 112.4(5) . . . . ? O20 C20 Cs1 O18 105.0(6) . . . 4_666 ? C15 C20 Cs1 O18 -11.8(7) . . . 4_666 ? C19 C20 Cs1 O18 -144.7(5) . . . 4_666 ? O20 C20 Cs1 O25 -37.7(5) . . . 4_566 ? C15 C20 Cs1 O25 -154.6(5) . . . 4_566 ? C19 C20 Cs1 O25 72.5(5) . . . 4_566 ? O20 C20 Cs1 O27 -128.8(5) . . . 4_666 ? C15 C20 Cs1 O27 114.3(5) . . . 4_666 ? C19 C20 Cs1 O27 -18.6(6) . . . 4_666 ? O20 C20 Cs1 C12 89.3(5) . . . . ? C15 C20 Cs1 C12 -27.5(5) . . . . ? C19 C20 Cs1 C12 -160.4(5) . . . . ? O20 C20 Cs1 O6 27.9(5) . . . 4_566 ? C15 C20 Cs1 O6 -89.0(5) . . . 4_566 ? C19 C20 Cs1 O6 138.1(5) . . . 4_566 ? O20 C20 Cs1 C11 83.0(5) . . . . ? C15 C20 Cs1 C11 -33.8(5) . . . . ? C19 C20 Cs1 C11 -166.8(6) . . . . ? O20 C20 Cs1 C13 111.0(5) . . . . ? C15 C20 Cs1 C13 -5.8(5) . . . . ? C19 C20 Cs1 C13 -138.7(5) . . . . ? O20 C20 Cs1 C10 100.8(5) . . . . ? C15 C20 Cs1 C10 -16.1(5) . . . . ? C19 C20 Cs1 C10 -149.0(6) . . . . ? O20 C20 Cs1 C9 125.5(5) . . . . ? C15 C20 Cs1 C9 8.7(5) . . . . ? C19 C20 Cs1 C9 -124.3(6) . . . . ? O20 C20 Cs1 C8 129.0(5) . . . . ? C15 C20 Cs1 C8 12.2(5) . . . . ? C19 C20 Cs1 C8 -120.8(5) . . . . ? O20 C20 Cs1 Br1 -93.7(5) . . . . ? C15 C20 Cs1 Br1 149.5(5) . . . . ? C19 C20 Cs1 Br1 16.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O27 0.84 2.13 2.912(9) 154.1 4_666 O4 H4 O5 0.84 2.32 2.762(8) 113.1 . O5 H5 O50 0.84 1.89 2.705(9) 162.2 . O6 H6 O12 0.84 2.22 3.026(9) 160.1 4_665 O6 H6 O5 0.84 2.35 2.796(9) 114.1 . O11 H11 O50 0.84 1.98 2.722(9) 147.0 4_566 O11 H11 O12 0.84 2.27 2.729(8) 115.0 . O12 H12 O19 0.84 1.98 2.773(8) 157.8 4_666 O12 H12 O13 0.84 2.30 2.750(8) 113.5 . O13 H13 O52 0.84 1.98 2.66(3) 137.5 . O13 H13 O51 0.84 2.15 2.621(12) 115.2 . O18 H18 O13 0.84 1.99 2.790(8) 160.1 4_565 O18 H18 O19 0.84 2.33 2.769(8) 112.9 . O19 H19 Br1 0.84 2.37 3.208(6) 173.0 . O20 H20 O26 0.84 2.04 2.795(9) 150.0 4_566 O20 H20 O19 0.84 2.34 2.794(8) 114.8 . O25 H25 O26 0.84 2.28 2.715(8) 112.7 . O25 H25 Br1 0.84 2.56 3.247(5) 139.2 4_665 O26 H26 O53 0.84 2.30 2.72(2) 111.3 . O26 H26 O5 0.84 2.25 3.000(8) 149.1 4_565 O26 H26 O27 0.84 2.37 2.807(8) 112.7 . O27 H27 O53B 0.84 1.80 2.62(2) 165.2 . O27 H27 O53 0.84 2.07 2.84(3) 152.6 . O50 H50 Br1 0.84 2.39 3.214(7) 165.3 . O52B H52B O51 0.84 2.20 3.01(3) 162.1 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.416 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.142 #===END data_ocs080z _database_code_depnum_ccdc_archive 'CCDC 288489' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 O8, 3(C H4 O), 5(O)' _chemical_formula_sum 'C35 H44 O16' _chemical_formula_weight 720.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 10.4761(3) _cell_length_b 16.4356(4) _cell_length_c 20.9672(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3610.15(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9793 _exptl_absorpt_correction_T_max 0.9948 _exptl_absorpt_process_details ; 'Blessing, R. H. Acta Crystallogr., Sect A 1995, 51, 33-38' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _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 Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15091 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 24.56 _reflns_number_total 3064 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0557P)^2^+7.9071P] 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 3064 _refine_ls_number_parameters 257 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0857(3) 0.4014(2) 0.40734(16) 0.0184(8) Uani 1 1 d . . . C2 C -0.1074(3) 0.4752(2) 0.37640(16) 0.0175(8) Uani 1 1 d . . . H2 H -0.0941 0.4774 0.3316 0.021 Uiso 1 1 calc R . . C3 C -0.1472(3) 0.5460(2) 0.40691(16) 0.0180(8) Uani 1 1 d . . . C4 C -0.1679(3) 0.5417(2) 0.47266(17) 0.0193(8) Uani 1 1 d . . . C5 C -0.1509(3) 0.4687(2) 0.50538(17) 0.0216(8) Uani 1 1 d . . . H5 H -0.1676 0.4659 0.5499 0.026 Uiso 1 1 calc R . . C6 C -0.1097(3) 0.4005(2) 0.47284(17) 0.0196(8) Uani 1 1 d . . . C7 C -0.1672(3) 0.6260(2) 0.37227(16) 0.0198(8) Uani 1 1 d . . . H7 H -0.1297 0.6696 0.3998 0.024 Uiso 1 1 calc R . . C8 C -0.0974(3) 0.6294(2) 0.30884(16) 0.0178(8) Uani 1 1 d . . . C9 C -0.1594(5) 0.6263(3) 0.2500 0.0197(12) Uani 1 2 d S . . H9 H -0.2498 0.6219 0.2500 0.024 Uiso 1 2 calc SR . . C12 C 0.1016(5) 0.6398(3) 0.2500 0.0195(11) Uani 1 2 d S . . H12 H 0.1919 0.6452 0.2500 0.023 Uiso 1 2 calc SR . . C13 C 0.0354(3) 0.6359(2) 0.30719(16) 0.0194(8) Uani 1 1 d . . . C23 C -0.0286(5) 0.3272(3) 0.2500 0.0195(11) Uani 1 2 d S . . H23 H -0.1078 0.2991 0.2500 0.023 Uiso 1 2 calc SR . . C24 C 0.0254(3) 0.3463(2) 0.30859(16) 0.0192(8) Uani 1 1 d . . . C25 C 0.1422(3) 0.3880(2) 0.30732(16) 0.0184(8) Uani 1 1 d . . . C26 C 0.1996(5) 0.4077(3) 0.2500 0.0199(12) Uani 1 2 d S . . H26 H 0.2795 0.4351 0.2500 0.024 Uiso 1 2 calc SR . . C28 C -0.0360(4) 0.3258(2) 0.37259(16) 0.0203(8) Uani 1 1 d . . . H28 H 0.0330 0.3024 0.4000 0.024 Uiso 1 1 calc R . . C29 C -0.3102(4) 0.6442(2) 0.36630(18) 0.0280(9) Uani 1 1 d . . . H29A H -0.3513 0.6013 0.3412 0.042 Uiso 1 1 calc R . . H29B H -0.3220 0.6967 0.3450 0.042 Uiso 1 1 calc R . . H29C H -0.3486 0.6462 0.4089 0.042 Uiso 1 1 calc R . . C32 C -0.1405(4) 0.2602(2) 0.36723(18) 0.0291(10) Uani 1 1 d . . . H32A H -0.2152 0.2831 0.3456 0.044 Uiso 1 1 calc R . . H32B H -0.1649 0.2420 0.4100 0.044 Uiso 1 1 calc R . . H32C H -0.1078 0.2139 0.3427 0.044 Uiso 1 1 calc R . . O4 O -0.2033(3) 0.61154(15) 0.50404(11) 0.0248(6) Uani 1 1 d . . . H4 H -0.1861 0.6070 0.5430 0.037 Uiso 1 1 calc R . . O6 O -0.0885(3) 0.32760(15) 0.50558(11) 0.0262(6) Uani 1 1 d . . . H6 H -0.0816 0.3372 0.5448 0.039 Uiso 1 1 calc R . . O13 O 0.0997(2) 0.63976(17) 0.36464(11) 0.0243(6) Uani 1 1 d . . . H13 H 0.1787 0.6410 0.3578 0.036 Uiso 1 1 calc R . . O25 O 0.1974(2) 0.40875(17) 0.36467(11) 0.0255(6) Uani 1 1 d . . . H25 H 0.2694 0.4296 0.3580 0.038 Uiso 1 1 calc R . . O50 O 0.4341(3) 0.47377(18) 0.36282(14) 0.0357(7) Uani 1 1 d D . . H50 H 0.4158 0.5229 0.3691 0.054 Uiso 1 1 calc RD . . C50 C 0.5095(5) 0.4433(4) 0.4161(2) 0.0579(15) Uani 1 1 d . . . H50A H 0.5837 0.4787 0.4226 0.087 Uiso 1 1 calc R . . H50B H 0.5385 0.3879 0.4067 0.087 Uiso 1 1 calc R . . H50C H 0.4571 0.4429 0.4548 0.087 Uiso 1 1 calc R . . C51 C 0.6490(8) 0.4025(5) 0.2500 0.063(2) Uani 1 2 d S . . H51A H 0.6832 0.3995 0.2934 0.095 Uiso 0.20 1 calc PR A 1 H51B H 0.7124 0.4277 0.2219 0.095 Uiso 0.20 1 calc PR A 1 H51C H 0.6295 0.3476 0.2347 0.095 Uiso 0.20 1 calc PR A 1 H51D H 0.6752 0.3907 0.2939 0.095 Uiso 0.30 1 calc PR A 2 H51E H 0.7241 0.4177 0.2248 0.095 Uiso 0.30 1 calc PR A 2 H51F H 0.6090 0.3542 0.2313 0.095 Uiso 0.30 1 calc PR A 2 O51 O 0.534(5) 0.451(3) 0.2500 0.090(16) Uani 0.40 2 d SP B 1 H51G H 0.4997 0.4481 0.2861 0.134 Uiso 0.20 1 calc PRD B 1 O51B O 0.563(3) 0.4661(12) 0.2500 0.034(4) Uani 0.60 2 d SP B 2 H51H H 0.5151 0.4624 0.2821 0.051 Uiso 0.30 1 calc PR B 2 O52 O 0.3560(3) 0.63312(17) 0.36634(13) 0.0350(7) Uani 1 1 d . . . O53 O -0.0455(4) 0.8216(3) 0.2500 0.0460(11) Uani 1 2 d S . . O54 O 0.3834(3) 0.7053(2) 0.48323(16) 0.0556(10) 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 0.0181(18) 0.022(2) 0.0149(18) 0.0025(16) 0.0008(15) 0.0001(16) C2 0.0185(18) 0.024(2) 0.0104(17) 0.0011(15) -0.0006(14) -0.0025(16) C3 0.0153(18) 0.024(2) 0.0145(18) 0.0022(16) -0.0001(15) 0.0007(16) C4 0.0187(19) 0.023(2) 0.0167(18) -0.0034(16) 0.0013(15) 0.0005(17) C5 0.0228(19) 0.027(2) 0.0152(18) 0.0020(17) 0.0049(16) -0.0014(17) C6 0.0225(19) 0.020(2) 0.0159(18) 0.0023(16) -0.0015(16) -0.0033(16) C7 0.026(2) 0.020(2) 0.0128(18) -0.0012(15) -0.0007(15) 0.0020(17) C8 0.0217(19) 0.0164(18) 0.0154(18) 0.0010(15) 0.0010(15) -0.0007(16) C9 0.020(3) 0.018(3) 0.021(3) 0.000 0.000 -0.005(2) C12 0.019(3) 0.018(3) 0.022(3) 0.000 0.000 -0.001(2) C13 0.027(2) 0.0158(18) 0.0153(19) -0.0003(15) 0.0005(16) 0.0017(17) C23 0.025(3) 0.016(3) 0.018(3) 0.000 0.000 0.003(2) C24 0.026(2) 0.0145(19) 0.0174(19) 0.0032(15) 0.0019(16) 0.0045(16) C25 0.0207(19) 0.0184(18) 0.0162(19) -0.0012(16) -0.0032(15) 0.0029(16) C26 0.019(3) 0.023(3) 0.018(3) 0.000 0.000 -0.002(2) C28 0.025(2) 0.0199(19) 0.0164(19) 0.0010(15) 0.0016(16) 0.0019(17) C29 0.028(2) 0.034(2) 0.021(2) 0.0029(18) 0.0052(17) 0.0074(19) C32 0.042(2) 0.024(2) 0.021(2) -0.0026(17) 0.0035(19) -0.0065(19) O4 0.0346(15) 0.0258(14) 0.0141(13) -0.0024(11) 0.0022(12) 0.0048(12) O6 0.0398(16) 0.0253(14) 0.0133(13) 0.0036(11) 0.0003(12) 0.0025(13) O13 0.0204(13) 0.0385(16) 0.0139(12) 0.0001(12) -0.0021(11) -0.0025(14) O25 0.0243(14) 0.0383(17) 0.0140(13) -0.0020(12) -0.0028(11) -0.0040(13) O50 0.0345(17) 0.0377(17) 0.0348(17) -0.0039(14) -0.0029(13) -0.0048(14) C50 0.048(3) 0.079(4) 0.047(3) 0.006(3) -0.016(2) -0.016(3) C51 0.055(5) 0.074(6) 0.060(5) 0.000 0.000 0.021(5) O51 0.04(2) 0.16(4) 0.065(16) 0.000 0.000 0.03(2) O51B 0.030(11) 0.041(5) 0.030(6) 0.000 0.000 0.006(6) O52 0.0252(15) 0.0414(18) 0.0383(17) -0.0030(14) 0.0000(13) 0.0006(14) O53 0.054(3) 0.042(3) 0.042(3) 0.000 0.000 0.004(2) O54 0.066(2) 0.056(2) 0.045(2) 0.0041(17) -0.0033(18) -0.0087(18) _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 1.394(5) . ? C1 C6 1.396(5) . ? C1 C28 1.532(5) . ? C2 C3 1.391(5) . ? C3 C4 1.397(5) . ? C3 C7 1.517(5) . ? C4 O4 1.375(4) . ? C4 C5 1.392(5) . ? C5 C6 1.382(5) . ? C6 O6 1.399(4) . ? C7 C8 1.519(5) . ? C7 C29 1.533(5) . ? C8 C9 1.395(4) . ? C8 C13 1.395(5) . ? C9 C8 1.395(4) 6_556 ? C12 C13 1.387(4) 6_556 ? C12 C13 1.387(4) . ? C13 O13 1.382(4) . ? C23 C24 1.388(4) . ? C23 C24 1.388(4) 6_556 ? C24 C25 1.403(5) . ? C24 C28 1.525(5) . ? C25 O25 1.377(4) . ? C25 C26 1.382(4) . ? C26 C25 1.382(4) 6_556 ? C28 C32 1.541(5) . ? O50 C50 1.457(5) . ? C51 O51B 1.38(3) . ? C51 O51 1.44(6) . ? 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 116.0(3) . . ? C2 C1 C28 122.7(3) . . ? C6 C1 C28 121.4(3) . . ? C3 C2 C1 124.2(3) . . ? C2 C3 C4 117.3(3) . . ? C2 C3 C7 123.1(3) . . ? C4 C3 C7 119.7(3) . . ? O4 C4 C5 121.2(3) . . ? O4 C4 C3 118.1(3) . . ? C5 C4 C3 120.7(3) . . ? C6 C5 C4 119.7(3) . . ? C5 C6 C1 122.2(3) . . ? C5 C6 O6 120.2(3) . . ? C1 C6 O6 117.6(3) . . ? C3 C7 C8 112.6(3) . . ? C3 C7 C29 110.1(3) . . ? C8 C7 C29 113.1(3) . . ? C9 C8 C13 116.4(3) . . ? C9 C8 C7 123.3(3) . . ? C13 C8 C7 120.3(3) . . ? C8 C9 C8 124.3(5) . 6_556 ? C13 C12 C13 119.7(5) 6_556 . ? O13 C13 C12 120.5(3) . . ? O13 C13 C8 117.9(3) . . ? C12 C13 C8 121.6(3) . . ? C24 C23 C24 124.5(5) . 6_556 ? C23 C24 C25 116.7(3) . . ? C23 C24 C28 123.9(3) . . ? C25 C24 C28 119.5(3) . . ? O25 C25 C26 121.2(3) . . ? O25 C25 C24 118.1(3) . . ? C26 C25 C24 120.7(3) . . ? C25 C26 C25 120.8(5) 6_556 . ? C24 C28 C1 112.5(3) . . ? C24 C28 C32 112.9(3) . . ? C1 C28 C32 111.1(3) . . ? O51B C51 O51 16(3) . . ? 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 1.7(5) . . . . ? C28 C1 C2 C3 -177.2(3) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C7 178.6(3) . . . . ? C2 C3 C4 O4 177.9(3) . . . . ? C7 C3 C4 O4 -1.4(5) . . . . ? C2 C3 C4 C5 -1.1(5) . . . . ? C7 C3 C4 C5 179.6(3) . . . . ? O4 C4 C5 C6 -177.1(3) . . . . ? C3 C4 C5 C6 1.9(5) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C4 C5 C6 O6 178.0(3) . . . . ? C2 C1 C6 C5 -0.8(5) . . . . ? C28 C1 C6 C5 178.0(3) . . . . ? C2 C1 C6 O6 -179.7(3) . . . . ? C28 C1 C6 O6 -0.9(5) . . . . ? C2 C3 C7 C8 -20.0(5) . . . . ? C4 C3 C7 C8 159.2(3) . . . . ? C2 C3 C7 C29 107.1(4) . . . . ? C4 C3 C7 C29 -73.6(4) . . . . ? C3 C7 C8 C9 108.5(4) . . . . ? C29 C7 C8 C9 -17.0(5) . . . . ? C3 C7 C8 C13 -71.5(4) . . . . ? C29 C7 C8 C13 163.0(3) . . . . ? C13 C8 C9 C8 0.0(7) . . . 6_556 ? C7 C8 C9 C8 180.0(3) . . . 6_556 ? C13 C12 C13 O13 -180.0(3) 6_556 . . . ? C13 C12 C13 C8 -1.1(7) 6_556 . . . ? C9 C8 C13 O13 179.5(3) . . . . ? C7 C8 C13 O13 -0.5(5) . . . . ? C9 C8 C13 C12 0.6(6) . . . . ? C7 C8 C13 C12 -179.4(4) . . . . ? C24 C23 C24 C25 0.1(7) 6_556 . . . ? C24 C23 C24 C28 179.2(3) 6_556 . . . ? C23 C24 C25 O25 179.3(3) . . . . ? C28 C24 C25 O25 0.2(5) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C28 C24 C25 C26 -179.7(4) . . . . ? O25 C25 C26 C25 -178.8(3) . . . 6_556 ? C24 C25 C26 C25 1.1(7) . . . 6_556 ? C23 C24 C28 C1 -109.3(4) . . . . ? C25 C24 C28 C1 69.7(4) . . . . ? C23 C24 C28 C32 17.5(5) . . . . ? C25 C24 C28 C32 -163.5(3) . . . . ? C2 C1 C28 C24 18.1(5) . . . . ? C6 C1 C28 C24 -160.7(3) . . . . ? C2 C1 C28 C32 -109.7(4) . . . . ? C6 C1 C28 C32 71.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O25 0.84 1.96 2.774(3) 163.9 5_566 O6 H6 O13 0.84 1.95 2.776(3) 169.5 5_566 O13 H13 O52 0.84 1.87 2.687(4) 163.8 . O25 H25 O50 0.84 1.87 2.700(4) 167.3 . O50 H50 O52 0.84 1.92 2.745(4) 167.8 . O51 H51G O50 0.84 1.80 2.62(2) 163.4 . O51B H51H O50 0.84 1.90 2.725(14) 166.0 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.56 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.696 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.064 #===END