# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Kenneth W. Henderson' _publ_contact_author_address ; University of Notre Dame Department of Chemistry Notre Dame, IN 46556-5670 ; _publ_contact_author_email khenders@nd.edu _publ_contact_author_phone 574.631.8025 _publ_contact_author_fax 574.631.6652 loop_ _publ_author_name _publ_author_address J.J.Morris ; University of Notre Dame Department of Chemistry Notre Dame, IN 46556-5670 ; B.C.Noll ; University of Notre Dame Department of Chemistry Notre Dame, IN 46556-5670 ; K.W.Henderson ; University of Notre Dame Department of Chemistry Notre Dame, IN 46556-5670 ; # Attachment 'CHEMCOMMUN 651287-651290.cif' data_jjm40 _database_code_depnum_ccdc_archive 'CCDC 651287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium 4-Cl-2,6-Dimethylphenoxide Dioxane' _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 Cl2 K2 O9' _chemical_formula_sum 'C30 H44 Cl2 K2 O9' _chemical_formula_weight 697.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.9385(3) _cell_length_b 19.5849(5) _cell_length_c 32.2466(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6908.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8183 _cell_measurement_theta_min 2.862 _cell_measurement_theta_max 31.310 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_measurement_device_type 'Bruker SMART Apex2 CCD diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56225 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8172 _reflns_number_gt 7233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker,2006)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2006; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)' _refine_special_details ; The asymmetric unit is composed of a dimeric potassium 4-Cl-2,6-dimethyl- phenoxide aggregate that is coordinated by 7 dioxane molecules. All seven dioxanes bridge to other aggregates to give a 7-connected three-dimensional network. 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^)+(0.0405P)^2^+5.8710P] 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 8172 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _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 K1 K 0.63759(4) 0.07816(2) 0.346095(12) 0.02016(10) Uani 1 1 d . . . K2 K 0.90754(4) -0.01377(2) 0.387246(12) 0.02054(10) Uani 1 1 d . . . Cl1 Cl 0.31084(5) -0.22707(3) 0.31240(2) 0.04290(16) Uani 1 1 d . . . Cl2 Cl 0.75413(9) 0.30036(4) 0.53369(3) 0.0795(3) Uani 1 1 d . . . O1 O 0.73732(12) -0.04826(6) 0.33344(4) 0.0209(3) Uani 1 1 d . . . O2 O 0.75349(13) 0.07137(7) 0.41680(4) 0.0243(3) Uani 1 1 d . . . O3 O 0.48739(16) 0.11038(8) 0.27641(5) 0.0364(4) Uani 1 1 d . . . O4 O 0.35871(16) 0.10381(9) 0.20017(5) 0.0415(4) Uani 1 1 d . . . O5 O 0.57537(14) 0.21295(7) 0.36453(5) 0.0299(3) Uani 1 1 d . . . O6 O 0.52270(13) 0.35277(7) 0.37818(5) 0.0267(3) Uani 1 1 d . . . O7 O 1.02853(16) -0.02663(8) 0.46035(5) 0.0362(4) Uani 1 1 d . . . O8 O 1.14511(13) 0.02922(9) 0.37267(5) 0.0346(4) Uani 1 1 d . . . O9 O 1.40039(13) 0.05144(8) 0.37052(5) 0.0325(3) Uani 1 1 d . . . C1 C 0.64624(16) -0.09033(9) 0.32876(6) 0.0181(3) Uani 1 1 d . . . C2 C 0.60249(17) -0.10837(9) 0.28849(6) 0.0210(4) Uani 1 1 d . . . C3 C 0.50020(18) -0.15035(10) 0.28402(7) 0.0262(4) Uani 1 1 d . . . H3 H 0.4707 -0.1613 0.2571 0.031 Uiso 1 1 calc R . . C4 C 0.44176(18) -0.17595(10) 0.31868(7) 0.0281(4) Uani 1 1 d . . . C5 C 0.48417(19) -0.16187(10) 0.35817(7) 0.0273(4) Uani 1 1 d . . . H5 H 0.4438 -0.1807 0.3816 0.033 Uiso 1 1 calc R . . C6 C 0.58625(17) -0.11996(9) 0.36369(6) 0.0222(4) Uani 1 1 d . . . C7 C 0.6684(2) -0.08017(11) 0.25124(7) 0.0294(4) Uani 1 1 d . . . H7A H 0.6261 -0.0945 0.2259 0.044 Uiso 1 1 calc R . . H7B H 0.7525 -0.0974 0.2509 0.044 Uiso 1 1 calc R . . H7C H 0.6696 -0.0302 0.2527 0.044 Uiso 1 1 calc R . . C8 C 0.6346(2) -0.10409(11) 0.40634(6) 0.0295(4) Uani 1 1 d . . . H8A H 0.5782 -0.1221 0.4273 0.044 Uiso 1 1 calc R . . H8B H 0.6419 -0.0545 0.4097 0.044 Uiso 1 1 calc R . . H8C H 0.7151 -0.1253 0.4098 0.044 Uiso 1 1 calc R . . C9 C 0.75566(17) 0.12151(9) 0.44328(6) 0.0190(3) Uani 1 1 d . . . C10 C 0.66825(18) 0.12556(10) 0.47584(6) 0.0249(4) Uani 1 1 d . . . C11 C 0.6702(2) 0.17989(12) 0.50354(7) 0.0343(5) Uani 1 1 d . . . H11 H 0.6118 0.1821 0.5253 0.041 Uiso 1 1 calc R . . C12 C 0.7568(2) 0.23049(12) 0.49950(8) 0.0393(6) Uani 1 1 d . . . C13 C 0.8446(2) 0.22776(11) 0.46885(8) 0.0364(5) Uani 1 1 d . . . H13 H 0.9044 0.2628 0.4669 0.044 Uiso 1 1 calc R . . C14 C 0.84563(18) 0.17378(10) 0.44090(7) 0.0266(4) Uani 1 1 d . . . C15 C 0.5730(2) 0.07106(13) 0.47871(9) 0.0409(6) Uani 1 1 d . . . H15A H 0.5188 0.0806 0.5022 0.061 Uiso 1 1 calc R . . H15B H 0.6126 0.0267 0.4828 0.061 Uiso 1 1 calc R . . H15C H 0.5252 0.0701 0.4530 0.061 Uiso 1 1 calc R . . C16 C 0.9411(2) 0.16818(13) 0.40771(9) 0.0417(6) Uani 1 1 d . . . H16A H 0.9943 0.2084 0.4086 0.063 Uiso 1 1 calc R . . H16B H 0.9014 0.1655 0.3805 0.063 Uiso 1 1 calc R . . H16C H 0.9901 0.1270 0.4123 0.063 Uiso 1 1 calc R . . C17 C 0.4291(2) 0.04929(11) 0.26256(7) 0.0320(5) Uani 1 1 d . . . H17A H 0.3453 0.0475 0.2741 0.038 Uiso 1 1 calc R . . H17B H 0.4747 0.0094 0.2734 0.038 Uiso 1 1 calc R . . C18 C 0.4223(2) 0.04421(13) 0.21678(7) 0.0360(5) Uani 1 1 d . . . H18A H 0.5058 0.0418 0.2050 0.043 Uiso 1 1 calc R . . H18B H 0.3780 0.0021 0.2089 0.043 Uiso 1 1 calc R . . C19 C 0.4175(3) 0.16461(13) 0.21366(8) 0.0431(6) Uani 1 1 d . . . H19A H 0.3711 0.2047 0.2036 0.052 Uiso 1 1 calc R . . H19B H 0.5006 0.1667 0.2016 0.052 Uiso 1 1 calc R . . C20 C 0.4265(3) 0.16760(13) 0.25946(9) 0.0464(6) Uani 1 1 d . . . H20A H 0.4708 0.2096 0.2675 0.056 Uiso 1 1 calc R . . H20B H 0.3431 0.1703 0.2713 0.056 Uiso 1 1 calc R . . C21 C 0.6366(2) 0.26558(11) 0.34180(7) 0.0307(4) Uani 1 1 d . . . H21A H 0.6578 0.2486 0.3138 0.037 Uiso 1 1 calc R . . H21B H 0.7135 0.2780 0.3562 0.037 Uiso 1 1 calc R . . C22 C 0.5562(2) 0.32778(10) 0.33803(6) 0.0276(4) Uani 1 1 d . . . H22A H 0.6003 0.3639 0.3226 0.033 Uiso 1 1 calc R . . H22B H 0.4816 0.3160 0.3222 0.033 Uiso 1 1 calc R . . C23 C 0.46182(19) 0.30004(10) 0.40114(7) 0.0263(4) Uani 1 1 d . . . H23A H 0.3849 0.2874 0.3869 0.032 Uiso 1 1 calc R . . H23B H 0.4409 0.3171 0.4292 0.032 Uiso 1 1 calc R . . C24 C 0.5430(2) 0.23818(10) 0.40482(7) 0.0291(4) Uani 1 1 d . . . H24A H 0.6181 0.2504 0.4203 0.035 Uiso 1 1 calc R . . H24B H 0.4999 0.2020 0.4205 0.035 Uiso 1 1 calc R . . C25 C 0.9623(2) -0.06581(13) 0.48997(7) 0.0378(5) Uani 1 1 d . . . H25A H 1.0200 -0.0936 0.5066 0.045 Uiso 1 1 calc R . . H25B H 0.9059 -0.0972 0.4754 0.045 Uiso 1 1 calc R . . C26 C 1.1094(2) 0.01969(14) 0.48175(8) 0.0385(5) Uani 1 1 d . . . H26A H 1.1549 0.0475 0.4613 0.046 Uiso 1 1 calc R . . H26B H 1.1695 -0.0067 0.4982 0.046 Uiso 1 1 calc R . . C27 C 1.2300(2) -0.02622(12) 0.37390(10) 0.0441(6) Uani 1 1 d . . . H27A H 1.2457 -0.0427 0.3454 0.053 Uiso 1 1 calc R . . H27B H 1.1948 -0.0644 0.3901 0.053 Uiso 1 1 calc R . . C28 C 1.1970(2) 0.08605(14) 0.35125(8) 0.0374(5) Uani 1 1 d . . . H28A H 1.1393 0.1250 0.3522 0.045 Uiso 1 1 calc R . . H28B H 1.2100 0.0738 0.3218 0.045 Uiso 1 1 calc R . . C29 C 1.3165(2) 0.10697(11) 0.37020(8) 0.0330(5) Uani 1 1 d . . . H29A H 1.3516 0.1453 0.3542 0.040 Uiso 1 1 calc R . . H29B H 1.3025 0.1229 0.3990 0.040 Uiso 1 1 calc R . . C30 C 1.3482(2) -0.00378(13) 0.39340(9) 0.0404(6) Uani 1 1 d . . . H30A H 1.3330 0.0108 0.4223 0.048 Uiso 1 1 calc R . . H30B H 1.4062 -0.0426 0.3940 0.048 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 K1 0.01876(18) 0.01796(18) 0.02376(19) -0.00084(14) -0.00243(15) 0.00115(14) K2 0.01815(18) 0.01983(19) 0.02363(19) -0.00437(14) -0.00196(15) 0.00115(15) Cl1 0.0241(2) 0.0281(3) 0.0765(4) -0.0038(3) 0.0001(3) -0.0100(2) Cl2 0.0893(6) 0.0615(5) 0.0876(6) -0.0577(4) -0.0542(5) 0.0395(4) O1 0.0208(6) 0.0182(6) 0.0239(6) -0.0016(5) -0.0008(5) -0.0024(5) O2 0.0266(7) 0.0226(6) 0.0238(7) -0.0063(5) -0.0012(6) 0.0044(6) O3 0.0478(9) 0.0294(8) 0.0322(8) -0.0058(6) -0.0170(7) 0.0029(7) O4 0.0418(9) 0.0498(10) 0.0330(8) 0.0083(7) -0.0154(7) -0.0190(8) O5 0.0312(8) 0.0165(6) 0.0421(9) -0.0045(6) -0.0034(6) 0.0011(6) O6 0.0317(7) 0.0162(6) 0.0321(7) -0.0019(5) 0.0010(6) -0.0009(6) O7 0.0452(9) 0.0408(9) 0.0225(7) 0.0004(6) -0.0016(7) 0.0030(8) O8 0.0175(7) 0.0419(9) 0.0445(9) 0.0028(7) 0.0043(6) -0.0013(6) O9 0.0196(7) 0.0333(8) 0.0446(9) -0.0034(7) 0.0037(6) -0.0021(6) C1 0.0171(8) 0.0129(7) 0.0243(9) -0.0009(6) 0.0002(7) 0.0030(6) C2 0.0206(8) 0.0174(8) 0.0251(9) -0.0021(7) -0.0012(7) 0.0026(7) C3 0.0227(9) 0.0214(9) 0.0346(11) -0.0067(8) -0.0051(8) 0.0006(8) C4 0.0182(8) 0.0164(8) 0.0499(13) -0.0024(8) -0.0002(9) -0.0029(7) C5 0.0251(9) 0.0181(9) 0.0387(11) 0.0053(8) 0.0068(8) 0.0014(8) C6 0.0219(9) 0.0168(8) 0.0278(10) 0.0013(7) 0.0024(7) 0.0031(7) C7 0.0290(10) 0.0356(11) 0.0236(9) -0.0032(8) -0.0005(8) -0.0031(9) C8 0.0322(10) 0.0314(10) 0.0248(10) 0.0046(8) 0.0039(8) -0.0002(9) C9 0.0206(8) 0.0175(8) 0.0189(8) 0.0011(6) -0.0031(7) 0.0042(7) C10 0.0248(9) 0.0272(10) 0.0226(9) 0.0005(7) -0.0001(8) 0.0048(8) C11 0.0364(11) 0.0440(12) 0.0225(10) -0.0077(9) -0.0028(9) 0.0171(10) C12 0.0453(13) 0.0322(11) 0.0403(12) -0.0209(10) -0.0236(11) 0.0167(10) C13 0.0312(11) 0.0211(10) 0.0569(15) -0.0043(9) -0.0198(10) 0.0005(9) C14 0.0242(9) 0.0213(9) 0.0343(11) 0.0057(8) -0.0043(8) 0.0021(8) C15 0.0309(11) 0.0430(13) 0.0486(14) 0.0034(11) 0.0125(10) -0.0039(10) C16 0.0325(12) 0.0417(13) 0.0511(15) 0.0139(11) 0.0093(11) -0.0053(10) C17 0.0371(12) 0.0286(10) 0.0302(11) -0.0053(8) -0.0039(9) 0.0049(9) C18 0.0358(12) 0.0388(12) 0.0334(12) -0.0064(9) 0.0024(9) -0.0085(10) C19 0.0436(13) 0.0416(13) 0.0442(14) 0.0110(11) -0.0172(11) -0.0143(11) C20 0.0615(17) 0.0307(12) 0.0472(15) -0.0058(10) -0.0130(13) 0.0101(12) C21 0.0269(10) 0.0264(10) 0.0387(12) -0.0091(8) 0.0025(9) -0.0019(8) C22 0.0330(10) 0.0221(9) 0.0277(10) -0.0001(7) 0.0001(8) -0.0045(8) C23 0.0268(10) 0.0232(9) 0.0289(10) 0.0004(7) 0.0007(8) -0.0021(8) C24 0.0327(11) 0.0212(9) 0.0333(11) 0.0032(8) -0.0078(9) -0.0017(8) C25 0.0451(13) 0.0392(12) 0.0291(11) 0.0023(9) -0.0045(10) -0.0001(11) C26 0.0333(11) 0.0504(14) 0.0317(11) 0.0019(10) -0.0003(9) 0.0006(11) C27 0.0290(11) 0.0296(11) 0.0737(18) -0.0082(11) 0.0092(12) -0.0040(10) C28 0.0249(10) 0.0504(14) 0.0370(12) 0.0115(10) 0.0090(9) 0.0046(10) C29 0.0328(11) 0.0261(10) 0.0402(12) -0.0038(9) 0.0082(9) -0.0018(9) C30 0.0234(10) 0.0339(12) 0.0638(16) 0.0074(11) 0.0051(10) 0.0060(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.7364(13) . ? K1 O2 2.6121(14) . ? K1 O9 2.7615(15) 1_455 ? K1 O5 2.7901(14) . ? K1 O3 2.8542(16) . ? K1 O4 2.8859(16) 6_656 ? K2 O2 2.5549(14) . ? K2 O1 2.6332(13) . ? K2 O7 2.7151(16) . ? K2 O6 2.7386(14) 8_755 ? K2 O8 2.7718(15) . ? K2 C22 3.508(2) 8_755 ? Cl1 C4 1.759(2) . ? Cl2 C12 1.758(2) . ? O1 C1 1.302(2) . ? O3 C20 1.414(3) . ? O3 C17 1.427(3) . ? O2 C9 1.302(2) . ? O4 C19 1.422(3) . ? O4 C18 1.461(3) . ? O4 K1 2.8859(16) 6_556 ? O5 C21 1.431(3) . ? O5 C24 1.434(3) . ? O6 C22 1.432(3) . ? O6 C23 1.435(2) . ? O6 K2 2.7386(14) 8_765 ? O7 C25 1.423(3) . ? O7 C26 1.443(3) . ? O8 C28 1.427(3) . ? O8 C27 1.429(3) . ? O9 C29 1.423(3) . ? O9 C30 1.428(3) . ? O9 K1 2.7615(15) 1_655 ? C1 C6 1.427(3) . ? C1 C2 1.429(3) . ? C2 C3 1.396(3) . ? C2 C7 1.506(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C8 1.506(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.422(3) . ? C9 C10 1.422(3) . ? C10 C11 1.389(3) . ? C10 C15 1.494(3) . ? C11 C12 1.377(4) . ? C11 H11 0.9500 . ? C12 C13 1.380(4) . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 C16 1.500(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.481(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.481(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.507(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 K2 3.508(2) 8_765 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.507(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.504(4) 5_756 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C25 1.504(4) 5_756 ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C30 1.503(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.500(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 K1 O1 83.72(4) . . ? O2 K1 O9 101.39(5) . 1_455 ? O1 K1 O9 104.22(4) . 1_455 ? O2 K1 O5 88.89(4) . . ? O1 K1 O5 170.11(4) . . ? O9 K1 O5 83.65(5) 1_455 . ? O2 K1 O3 167.90(5) . . ? O1 K1 O3 108.19(4) . . ? O9 K1 O3 74.07(5) 1_455 . ? O5 K1 O3 79.53(5) . . ? O2 K1 O4 93.05(5) . 6_656 ? O1 K1 O4 75.30(5) . 6_656 ? O9 K1 O4 165.44(5) 1_455 6_656 ? O5 K1 O4 98.62(5) . 6_656 ? O3 K1 O4 92.12(5) . 6_656 ? O2 K2 O1 86.96(4) . . ? O2 K2 O7 93.34(5) . . ? O1 K2 O7 153.25(5) . . ? O2 K2 O6 147.83(5) . 8_755 ? O1 K2 O6 83.21(4) . 8_755 ? O7 K2 O6 82.43(5) . 8_755 ? O2 K2 O8 118.91(5) . . ? O1 K2 O8 128.98(5) . . ? O7 K2 O8 73.65(5) . . ? O6 K2 O8 90.60(5) 8_755 . ? O2 K2 C22 145.14(5) . 8_755 ? O1 K2 C22 63.56(5) . 8_755 ? O7 K2 C22 104.81(5) . 8_755 ? O6 K2 C22 22.46(5) 8_755 8_755 ? O8 K2 C22 94.94(5) . 8_755 ? C1 O1 K2 141.26(12) . . ? C1 O1 K1 106.55(10) . . ? K2 O1 K1 87.22(4) . . ? C20 O3 C17 109.44(18) . . ? C20 O3 K1 138.68(14) . . ? C17 O3 K1 108.55(12) . . ? C9 O2 K2 136.48(12) . . ? C9 O2 K1 122.89(11) . . ? K2 O2 K1 91.59(4) . . ? C19 O4 C18 109.97(17) . . ? C19 O4 K1 133.11(15) . 6_556 ? C18 O4 K1 116.72(13) . 6_556 ? C21 O5 C24 109.35(15) . . ? C21 O5 K1 117.26(12) . . ? C24 O5 K1 125.40(11) . . ? C22 O6 C23 109.85(15) . . ? C22 O6 K2 110.58(11) . 8_765 ? C23 O6 K2 139.57(12) . 8_765 ? C25 O7 C26 109.26(17) . . ? C25 O7 K2 112.62(13) . . ? C26 O7 K2 130.99(14) . . ? C28 O8 C27 110.32(17) . . ? C28 O8 K2 133.76(13) . . ? C27 O8 K2 111.95(13) . . ? C29 O9 C30 108.93(16) . . ? C29 O9 K1 117.33(12) . 1_655 ? C30 O9 K1 131.80(12) . 1_655 ? O1 C1 C6 121.21(17) . . ? O1 C1 C2 121.22(17) . . ? C6 C1 C2 117.57(16) . . ? C3 C2 C1 120.54(18) . . ? C3 C2 C7 121.17(18) . . ? C1 C2 C7 118.29(17) . . ? C4 C3 C2 120.06(19) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.15(18) . . ? C3 C4 Cl1 119.33(17) . . ? C5 C4 Cl1 119.51(17) . . ? C4 C5 C6 120.16(19) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.40(18) . . ? C5 C6 C8 121.21(18) . . ? C1 C6 C8 118.38(17) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C14 121.35(17) . . ? O2 C9 C10 120.94(17) . . ? C14 C9 C10 117.70(17) . . ? C11 C10 C9 120.5(2) . . ? C11 C10 C15 121.2(2) . . ? C9 C10 C15 118.33(18) . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.26(19) . . ? C11 C12 Cl2 119.3(2) . . ? C13 C12 Cl2 119.4(2) . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 120.5(2) . . ? C13 C14 C16 121.6(2) . . ? C9 C14 C16 117.90(19) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 113.00(19) . . ? O3 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? O3 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? O4 C18 C17 109.63(19) . . ? O4 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? O4 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O4 C19 C20 111.6(2) . . ? O4 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? O4 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? O3 C20 C19 112.7(2) . . ? O3 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? O3 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? O5 C21 C22 110.51(17) . . ? O5 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O6 C22 C21 110.67(17) . . ? O6 C22 K2 46.96(8) . 8_765 ? C21 C22 K2 127.78(14) . 8_765 ? O6 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? K2 C22 H22A 62.6 8_765 . ? O6 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? K2 C22 H22B 122.2 8_765 . ? H22A C22 H22B 108.1 . . ? O6 C23 C24 110.24(17) . . ? O6 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? O6 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? O5 C24 C23 110.57(17) . . ? O5 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? O5 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? O7 C25 C26 110.4(2) . 5_756 ? O7 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 5_756 . ? O7 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 5_756 . ? H25A C25 H25B 108.1 . . ? O7 C26 C25 110.33(19) . 5_756 ? O7 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 5_756 . ? O7 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 5_756 . ? H26A C26 H26B 108.1 . . ? O8 C27 C30 110.38(19) . . ? O8 C27 H27A 109.6 . . ? C30 C27 H27A 109.6 . . ? O8 C27 H27B 109.6 . . ? C30 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? O8 C28 C29 111.25(19) . . ? O8 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? O8 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? O9 C29 C28 110.86(18) . . ? O9 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? O9 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? O9 C30 C27 110.4(2) . . ? O9 C30 H30A 109.6 . . ? C27 C30 H30A 109.6 . . ? O9 C30 H30B 109.6 . . ? C27 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.914 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.060 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'crystallized on cooling in dioxane from 100 \%C to 20\%C.' # END data_jjm45 _database_code_depnum_ccdc_archive 'CCDC 651288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium 2,4,6-Trimethylphenoxide Dioxane' _chemical_melting_point ? _chemical_formula_moiety 'C65 H95 K5 O15' _chemical_formula_sum 'C65 H95 K5 O15' _chemical_formula_weight 1311.91 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.380(4) _cell_length_b 21.550(4) _cell_length_c 17.740(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.30(3) _cell_angle_gamma 90.00 _cell_volume 7025(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9098 _cell_measurement_theta_min 2.223 _cell_measurement_theta_max 29.94 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.435 _exptl_crystal_size_mid 0.395 _exptl_crystal_size_min 0.285 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_measurement_device_type 'Bruker SMART Apex CCD diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 105361 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 29.93 _reflns_number_total 20144 _reflns_number_gt 17304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker,2006)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2006; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)' _refine_special_details ; The asymmetric unit is composed of a pentameric 2,4,6-trimethylphenoxide aggregate that is coordinated by nine dioxane molecules. Six of the dioxanes form a single bridge to other aggregates while the final two bridging dioxanes form a double bridge to a single aggregate. 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^)+(0.0403P)^2^+4.7714P] 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 20144 _refine_ls_number_parameters 818 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 K1 K 0.417797(16) 0.543693(13) 0.284396(17) 0.01978(6) Uani 1 1 d . . . K2 K 0.257618(16) 0.441303(16) 0.243711(18) 0.02408(7) Uani 1 1 d . . . K3 K 0.113306(17) 0.549867(15) 0.302301(18) 0.02389(7) Uani 1 1 d . . . K4 K 0.361450(17) 0.360370(14) 0.109753(18) 0.02233(7) Uani 1 1 d . . . K5 K 0.143754(18) 0.352601(15) 0.136529(19) 0.02550(7) Uani 1 1 d . . . O1 O 0.27042(6) 0.55250(5) 0.29633(6) 0.0241(2) Uani 1 1 d . . . O2 O 0.11920(6) 0.43205(5) 0.25354(7) 0.0281(2) Uani 1 1 d . B . O3 O 0.26098(7) 0.28720(5) 0.16859(7) 0.0352(3) Uani 1 1 d . B . O4 O 0.39680(6) 0.42451(5) 0.23846(6) 0.0219(2) Uani 1 1 d . . . O5 O 0.24203(5) 0.43267(5) 0.09138(6) 0.0208(2) Uani 1 1 d . B . O7 O 0.46961(7) 0.51456(5) 0.42774(6) 0.0318(3) Uani 1 1 d . . . O8 O 0.52754(6) 0.15245(5) 0.15456(7) 0.0276(2) Uani 1 1 d . . . O9 O 0.48586(6) 0.39925(5) -0.17488(6) 0.0253(2) Uani 1 1 d . . . O10 O 0.42076(6) 0.37742(6) -0.03305(7) 0.0305(2) Uani 1 1 d . . . O11 O 0.47931(6) 0.27569(5) 0.12666(7) 0.0278(2) Uani 1 1 d . . . O13 O 0.10347(6) 0.60763(5) 0.16298(7) 0.0293(2) Uani 1 1 d . . . O14 O 0.05348(8) 0.64120(6) 0.01623(8) 0.0419(3) Uani 1 1 d . . . O15 O -0.02131(7) 0.14882(6) 0.17393(8) 0.0381(3) Uani 1 1 d . . . O16 O 0.04025(7) 0.51957(6) 0.43649(7) 0.0319(3) Uani 1 1 d . . . C1 C 0.26054(7) 0.60099(7) 0.34032(8) 0.0203(3) Uani 1 1 d . . . C2 C 0.24926(8) 0.59351(7) 0.41893(8) 0.0222(3) Uani 1 1 d . . . C3 C 0.23733(8) 0.64530(7) 0.46446(9) 0.0243(3) Uani 1 1 d . . . H3 H 0.2304 0.6391 0.5168 0.029 Uiso 1 1 calc R . . C4 C 0.23522(8) 0.70580(7) 0.43599(9) 0.0260(3) Uani 1 1 d . . . C5 C 0.24620(8) 0.71286(7) 0.35883(9) 0.0258(3) Uani 1 1 d . . . H5 H 0.2450 0.7535 0.3380 0.031 Uiso 1 1 calc R . . C6 C 0.25892(8) 0.66274(7) 0.31102(8) 0.0220(3) Uani 1 1 d . . . C7 C 0.25201(10) 0.52870(8) 0.45156(10) 0.0311(3) Uani 1 1 d . . . H7A H 0.2481 0.5309 0.5065 0.047 Uiso 1 1 calc R . . H7B H 0.2982 0.5090 0.4389 0.047 Uiso 1 1 calc R . . H7C H 0.2115 0.5042 0.4305 0.047 Uiso 1 1 calc R . . C8 C 0.22103(11) 0.76125(8) 0.48612(11) 0.0371(4) Uani 1 1 d . . . H8A H 0.1689 0.7709 0.4847 0.056 Uiso 1 1 calc R . . H8B H 0.2484 0.7971 0.4681 0.056 Uiso 1 1 calc R . . H8C H 0.2366 0.7516 0.5380 0.056 Uiso 1 1 calc R . . C9 C 0.27357(10) 0.67274(8) 0.22844(9) 0.0297(3) Uani 1 1 d . . . H9A H 0.2644 0.7163 0.2153 0.045 Uiso 1 1 calc R . . H9B H 0.2414 0.6460 0.1979 0.045 Uiso 1 1 calc R . . H9C H 0.3244 0.6624 0.2185 0.045 Uiso 1 1 calc R . . C10 C 0.05514(8) 0.40944(7) 0.27155(9) 0.0231(3) Uani 1 1 d . . . C11 C -0.00860(8) 0.42476(8) 0.22784(9) 0.0260(3) Uani 1 1 d . B . C12 C -0.07610(9) 0.40084(8) 0.24737(9) 0.0277(3) Uani 1 1 d . . . H12 H -0.1178 0.4120 0.2178 0.033 Uiso 1 1 calc R B . C13 C -0.08466(9) 0.36137(7) 0.30832(10) 0.0276(3) Uani 1 1 d . B . C14 C -0.02265(10) 0.34648(7) 0.35092(9) 0.0289(3) Uani 1 1 d . . . H14 H -0.0273 0.3194 0.3928 0.035 Uiso 1 1 calc R B . C15 C 0.04655(9) 0.36982(7) 0.33464(9) 0.0264(3) Uani 1 1 d . B . C16 C -0.00262(10) 0.46754(10) 0.16056(10) 0.0374(4) Uani 1 1 d . . . H16A H -0.0511 0.4745 0.1380 0.056 Uiso 1 1 calc R B . H16B H 0.0289 0.4485 0.1232 0.056 Uiso 1 1 calc R . . H16C H 0.0182 0.5073 0.1770 0.056 Uiso 1 1 calc R . . C17 C -0.15925(10) 0.33609(9) 0.32750(12) 0.0394(4) Uani 1 1 d . . . H17A H -0.1766 0.3085 0.2870 0.059 Uiso 1 1 calc R B . H17B H -0.1935 0.3706 0.3328 0.059 Uiso 1 1 calc R . . H17C H -0.1558 0.3129 0.3750 0.059 Uiso 1 1 calc R . . C18 C 0.11272(11) 0.35566(9) 0.38376(12) 0.0423(4) Uani 1 1 d . . . H18A H 0.0996 0.3259 0.4229 0.063 Uiso 1 1 calc R B . H18B H 0.1305 0.3940 0.4074 0.063 Uiso 1 1 calc R . . H18C H 0.1509 0.3379 0.3528 0.063 Uiso 1 1 calc R . . C19 C 0.25565(8) 0.22627(7) 0.16801(10) 0.0276(3) Uani 1 1 d . . . C20 C 0.24920(11) 0.19180(9) 0.09925(10) 0.0372(4) Uani 1 1 d . B . C21 C 0.24295(12) 0.12747(9) 0.10003(11) 0.0405(4) Uani 1 1 d . . . H21 H 0.2387 0.1060 0.0534 0.049 Uiso 1 1 calc R B . C22 C 0.24266(10) 0.09336(8) 0.16695(10) 0.0314(3) Uani 1 1 d . B . C23 C 0.24842(9) 0.12661(7) 0.23379(9) 0.0278(3) Uani 1 1 d . . . H23 H 0.2472 0.1046 0.2801 0.033 Uiso 1 1 calc R B . C24 C 0.25590(9) 0.19105(7) 0.23580(9) 0.0279(3) Uani 1 1 d . B . C25 C 0.24782(18) 0.22684(11) 0.02531(12) 0.0630(7) Uani 1 1 d . . . H25A H 0.2428 0.1974 -0.0166 0.094 Uiso 1 1 calc R B . H25B H 0.2932 0.2502 0.0205 0.094 Uiso 1 1 calc R . . H25C H 0.2066 0.2557 0.0241 0.094 Uiso 1 1 calc R . . C26 C 0.23581(14) 0.02320(9) 0.16737(12) 0.0485(5) Uani 1 1 d . . . H26A H 0.2818 0.0046 0.1520 0.073 Uiso 1 1 calc R B . H26B H 0.1967 0.0106 0.1321 0.073 Uiso 1 1 calc R . . H26C H 0.2244 0.0091 0.2183 0.073 Uiso 1 1 calc R . . C27 C 0.26664(14) 0.22444(9) 0.30956(11) 0.0451(5) Uani 1 1 d . . . H27A H 0.2679 0.1942 0.3509 0.068 Uiso 1 1 calc R B . H27B H 0.2264 0.2535 0.3167 0.068 Uiso 1 1 calc R . . H27C H 0.3127 0.2474 0.3093 0.068 Uiso 1 1 calc R . . C28 C 0.44925(8) 0.39419(6) 0.27445(8) 0.0187(3) Uani 1 1 d . . . C29 C 0.52112(8) 0.39175(6) 0.24589(8) 0.0208(3) Uani 1 1 d . . . C30 C 0.57612(8) 0.36015(7) 0.28549(9) 0.0231(3) Uani 1 1 d . . . H30 H 0.6238 0.3600 0.2660 0.028 Uiso 1 1 calc R . . C31 C 0.56344(8) 0.32869(7) 0.35288(9) 0.0237(3) Uani 1 1 d . . . C32 C 0.49260(8) 0.33046(7) 0.38038(8) 0.0229(3) Uani 1 1 d . . . H32 H 0.4824 0.3086 0.4254 0.027 Uiso 1 1 calc R . . C33 C 0.43660(8) 0.36313(6) 0.34403(8) 0.0210(3) Uani 1 1 d . . . C34 C 0.53555(9) 0.42280(7) 0.17118(9) 0.0272(3) Uani 1 1 d . . . H34A H 0.5877 0.4315 0.1676 0.041 Uiso 1 1 calc R . . H34B H 0.5081 0.4617 0.1677 0.041 Uiso 1 1 calc R . . H34C H 0.5202 0.3952 0.1299 0.041 Uiso 1 1 calc R . . C35 C 0.62473(9) 0.29614(8) 0.39550(10) 0.0312(3) Uani 1 1 d . . . H35A H 0.6413 0.3221 0.4379 0.047 Uiso 1 1 calc R . . H35B H 0.6653 0.2890 0.3616 0.047 Uiso 1 1 calc R . . H35C H 0.6073 0.2563 0.4146 0.047 Uiso 1 1 calc R . . C36 C 0.36230(9) 0.36810(8) 0.37825(10) 0.0304(3) Uani 1 1 d . . . H36A H 0.3625 0.3464 0.4268 0.046 Uiso 1 1 calc R . . H36B H 0.3259 0.3492 0.3442 0.046 Uiso 1 1 calc R . . H36C H 0.3503 0.4119 0.3860 0.046 Uiso 1 1 calc R . . C37 C 0.24887(7) 0.47108(6) 0.03422(8) 0.0180(2) Uani 1 1 d . . . C38 C 0.29495(7) 0.52442(6) 0.03934(8) 0.0187(2) Uani 1 1 d . B . C39 C 0.29964(8) 0.56571(6) -0.02080(8) 0.0204(3) Uani 1 1 d . . . H39 H 0.3301 0.6011 -0.0154 0.024 Uiso 1 1 calc R B . C40 C 0.26125(8) 0.55692(7) -0.08873(8) 0.0211(3) Uani 1 1 d . B . C41 C 0.21778(8) 0.50389(7) -0.09475(8) 0.0217(3) Uani 1 1 d . . . H41 H 0.1919 0.4963 -0.1408 0.026 Uiso 1 1 calc R B . C42 C 0.21080(7) 0.46153(7) -0.03573(8) 0.0208(3) Uani 1 1 d . B . C43 C 0.33649(8) 0.53641(7) 0.11189(9) 0.0235(3) Uani 1 1 d . . . H43A H 0.3683 0.5725 0.1057 0.035 Uiso 1 1 calc R B . H43B H 0.3660 0.4999 0.1250 0.035 Uiso 1 1 calc R . . H43C H 0.3022 0.5446 0.1522 0.035 Uiso 1 1 calc R . . C44 C 0.26379(9) 0.60458(7) -0.15136(9) 0.0263(3) Uani 1 1 d . . . H44A H 0.2687 0.5834 -0.1999 0.039 Uiso 1 1 calc R B . H44B H 0.3055 0.6322 -0.1427 0.039 Uiso 1 1 calc R . . H44C H 0.2188 0.6290 -0.1521 0.039 Uiso 1 1 calc R . . C45 C 0.16180(9) 0.40562(8) -0.04423(10) 0.0303(3) Uani 1 1 d . . . H45A H 0.1194 0.4108 -0.0124 0.046 Uiso 1 1 calc R B . H45B H 0.1886 0.3682 -0.0288 0.046 Uiso 1 1 calc R . . H45C H 0.1456 0.4016 -0.0970 0.046 Uiso 1 1 calc R . . C46 C 0.45673(10) 0.55254(7) 0.49254(9) 0.0313(4) Uani 1 1 d . . . H46A H 0.4081 0.5721 0.4873 0.038 Uiso 1 1 calc R . . H46B H 0.4936 0.5860 0.4955 0.038 Uiso 1 1 calc R . . C47 C 0.53952(10) 0.48558(7) 0.43595(9) 0.0310(3) Uani 1 1 d . . . H47A H 0.5780 0.5178 0.4377 0.037 Uiso 1 1 calc R . . H47B H 0.5481 0.4585 0.3920 0.037 Uiso 1 1 calc R . . C48 C 0.56329(8) 0.19214(7) 0.10161(9) 0.0241(3) Uani 1 1 d . . . H48A H 0.5419 0.1856 0.0505 0.029 Uiso 1 1 calc R . . H48B H 0.6156 0.1814 0.1003 0.029 Uiso 1 1 calc R . . C49 C 0.45198(9) 0.16938(8) 0.15854(11) 0.0310(3) Uani 1 1 d . . . H49A H 0.4276 0.1426 0.1957 0.037 Uiso 1 1 calc R . . H49B H 0.4277 0.1630 0.1087 0.037 Uiso 1 1 calc R . . C50 C 0.41240(9) 0.41755(8) -0.16025(10) 0.0296(3) Uani 1 1 d . . . H50A H 0.3786 0.3838 -0.1756 0.035 Uiso 1 1 calc R . . H50B H 0.3998 0.4548 -0.1904 0.035 Uiso 1 1 calc R . . C51 C 0.50220(10) 0.34473(8) -0.13149(10) 0.0314(3) Uani 1 1 d . . . H51A H 0.5530 0.3317 -0.1404 0.038 Uiso 1 1 calc R . . H51B H 0.4695 0.3106 -0.1479 0.038 Uiso 1 1 calc R . . C52 C 0.49279(9) 0.35677(9) -0.04839(10) 0.0319(3) Uani 1 1 d . . . H52A H 0.5031 0.3182 -0.0198 0.038 Uiso 1 1 calc R . . H52B H 0.5282 0.3886 -0.0312 0.038 Uiso 1 1 calc R . . C53 C 0.40377(10) 0.43153(8) -0.07767(10) 0.0330(4) Uani 1 1 d . . . H53A H 0.4366 0.4660 -0.0626 0.040 Uiso 1 1 calc R . . H53B H 0.3531 0.4447 -0.0686 0.040 Uiso 1 1 calc R . . C54 C 0.44512(9) 0.23664(8) 0.18166(10) 0.0328(4) Uani 1 1 d . . . H54A H 0.3931 0.2478 0.1853 0.039 Uiso 1 1 calc R . . H54B H 0.4687 0.2430 0.2318 0.039 Uiso 1 1 calc R . . C55 C 0.55486(8) 0.25938(7) 0.12392(9) 0.0247(3) Uani 1 1 d . . . H55A H 0.5783 0.2663 0.1740 0.030 Uiso 1 1 calc R . . H55B H 0.5794 0.2862 0.0869 0.030 Uiso 1 1 calc R . . C58 C 0.13354(10) 0.58000(9) 0.09690(10) 0.0349(4) Uani 1 1 d . . . H58A H 0.1483 0.5368 0.1083 0.042 Uiso 1 1 calc R . . H58B H 0.1775 0.6033 0.0824 0.042 Uiso 1 1 calc R . . C59 C 0.07917(12) 0.58026(9) 0.03235(10) 0.0393(4) Uani 1 1 d . . . H59A H 0.1021 0.5629 -0.0130 0.047 Uiso 1 1 calc R . . H59B H 0.0375 0.5534 0.0449 0.047 Uiso 1 1 calc R . . C60 C 0.02446(11) 0.66849(9) 0.08255(12) 0.0404(4) Uani 1 1 d . . . H60A H -0.0183 0.6443 0.0986 0.048 Uiso 1 1 calc R . . H60B H 0.0082 0.7113 0.0713 0.048 Uiso 1 1 calc R . . C61 C 0.08117(10) 0.66969(8) 0.14557(11) 0.0342(4) Uani 1 1 d . . . H61A H 0.1237 0.6944 0.1300 0.041 Uiso 1 1 calc R . . H61B H 0.0607 0.6894 0.1908 0.041 Uiso 1 1 calc R . . C63 C 0.05398(10) 0.15827(9) 0.19077(14) 0.0447(5) Uani 1 1 d . B . H63A H 0.0829 0.1479 0.1461 0.054 Uiso 1 1 calc R A 1 H63B H 0.0697 0.1306 0.2326 0.054 Uiso 1 1 calc R A 1 C64 C 0.05127(10) 0.54655(8) 0.50997(10) 0.0336(4) Uani 1 1 d . . . H64A H 0.0199 0.5836 0.5147 0.040 Uiso 1 1 calc R . . H64B H 0.1026 0.5600 0.5161 0.040 Uiso 1 1 calc R . . C65 C -0.03363(9) 0.49938(8) 0.42881(9) 0.0298(3) Uani 1 1 d . . . H65A H -0.0415 0.4798 0.3788 0.036 Uiso 1 1 calc R . . H65B H -0.0665 0.5356 0.4320 0.036 Uiso 1 1 calc R . . O12 O 0.04617(8) 0.26381(7) 0.15073(11) 0.0308(4) Uani 0.804(3) 1 d P B 1 C56 C -0.02950(19) 0.25405(16) 0.13351(18) 0.0298(6) Uani 0.804(3) 1 d P B 1 H56A H -0.0452 0.2814 0.0913 0.036 Uiso 0.804(3) 1 calc PR B 1 H56B H -0.0587 0.2645 0.1780 0.036 Uiso 0.804(3) 1 calc PR B 1 C57 C 0.06731(11) 0.22494(11) 0.21283(14) 0.0357(5) Uani 0.804(3) 1 d P B 1 H57A H 0.0386 0.2356 0.2576 0.043 Uiso 0.804(3) 1 calc PR B 1 H57B H 0.1195 0.2313 0.2257 0.043 Uiso 0.804(3) 1 calc PR B 1 C62 C -0.04183(13) 0.18702(11) 0.11194(13) 0.0353(5) Uani 0.804(3) 1 d P B 1 H62A H -0.0938 0.1803 0.0984 0.042 Uiso 0.804(3) 1 calc PR B 1 H62B H -0.0124 0.1764 0.0677 0.042 Uiso 0.804(3) 1 calc PR B 1 O12' O 0.0491(4) 0.2517(3) 0.0981(5) 0.044(2) Uani 0.196(3) 1 d P B 2 C56' C 0.0734(6) 0.1887(5) 0.1037(7) 0.051(3) Uani 0.196(3) 1 d P B 2 H56C H 0.1266 0.1869 0.0960 0.061 Uiso 0.196(3) 1 calc PR B 2 H56D H 0.0491 0.1636 0.0637 0.061 Uiso 0.196(3) 1 calc PR B 2 C57' C -0.0266(9) 0.2537(8) 0.1015(9) 0.041(4) Uani 0.196(3) 1 d P B 2 H57C H -0.0481 0.2308 0.0582 0.050 Uiso 0.196(3) 1 calc PR B 2 H57D H -0.0431 0.2973 0.0981 0.050 Uiso 0.196(3) 1 calc PR B 2 C62' C -0.0519(6) 0.2262(5) 0.1723(8) 0.050(3) Uani 0.196(3) 1 d P B 2 H62C H -0.1056 0.2276 0.1740 0.061 Uiso 0.196(3) 1 calc PR B 2 H62D H -0.0316 0.2492 0.2162 0.061 Uiso 0.196(3) 1 calc PR B 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 K1 0.02284(14) 0.01957(13) 0.01683(14) -0.00093(10) -0.00171(10) -0.00244(10) K2 0.01700(13) 0.03421(16) 0.02107(15) -0.00416(12) 0.00094(11) -0.00111(11) K3 0.02156(14) 0.02884(15) 0.02140(16) -0.00147(12) 0.00306(11) 0.00275(11) K4 0.02563(15) 0.02186(14) 0.01961(15) -0.00068(11) 0.00326(11) 0.00480(11) K5 0.02633(15) 0.02389(14) 0.02647(17) -0.00329(12) 0.00467(12) -0.00667(11) O1 0.0275(5) 0.0235(5) 0.0215(5) -0.0035(4) 0.0023(4) 0.0019(4) O2 0.0193(5) 0.0348(6) 0.0304(6) -0.0061(5) 0.0049(4) -0.0022(4) O3 0.0395(7) 0.0269(6) 0.0398(7) 0.0101(5) 0.0106(5) 0.0047(5) O4 0.0220(5) 0.0212(5) 0.0223(5) -0.0010(4) -0.0010(4) 0.0019(4) O5 0.0216(5) 0.0210(5) 0.0199(5) 0.0031(4) 0.0008(4) -0.0014(4) O7 0.0525(7) 0.0222(5) 0.0202(6) -0.0028(4) -0.0132(5) 0.0052(5) O8 0.0286(6) 0.0222(5) 0.0321(6) 0.0076(4) 0.0014(5) 0.0046(4) O9 0.0273(5) 0.0281(5) 0.0206(5) 0.0006(4) 0.0044(4) -0.0004(4) O10 0.0304(6) 0.0354(6) 0.0262(6) 0.0058(5) 0.0112(5) 0.0041(5) O11 0.0280(6) 0.0239(5) 0.0318(6) 0.0062(4) 0.0037(4) 0.0065(4) O13 0.0329(6) 0.0318(6) 0.0236(6) -0.0012(4) 0.0075(5) 0.0014(5) O14 0.0601(9) 0.0338(7) 0.0315(7) 0.0057(5) -0.0068(6) -0.0024(6) O15 0.0339(7) 0.0382(7) 0.0423(8) 0.0074(6) 0.0021(5) -0.0143(5) O16 0.0411(7) 0.0340(6) 0.0212(6) -0.0047(5) 0.0106(5) -0.0090(5) C1 0.0169(6) 0.0232(6) 0.0207(7) -0.0010(5) 0.0012(5) 0.0006(5) C2 0.0215(6) 0.0239(6) 0.0212(7) 0.0000(5) 0.0016(5) 0.0004(5) C3 0.0247(7) 0.0293(7) 0.0190(7) -0.0017(5) 0.0016(5) 0.0014(5) C4 0.0256(7) 0.0269(7) 0.0255(8) -0.0040(6) 0.0006(6) 0.0041(6) C5 0.0265(7) 0.0229(7) 0.0280(8) 0.0013(6) 0.0012(6) 0.0040(5) C6 0.0202(6) 0.0247(7) 0.0210(7) 0.0010(5) 0.0009(5) 0.0024(5) C7 0.0417(9) 0.0273(7) 0.0245(8) 0.0034(6) 0.0037(7) 0.0001(6) C8 0.0512(11) 0.0300(8) 0.0302(9) -0.0066(7) 0.0014(8) 0.0095(7) C9 0.0365(8) 0.0297(8) 0.0230(8) 0.0045(6) 0.0044(6) 0.0044(6) C10 0.0212(6) 0.0261(7) 0.0222(7) -0.0067(5) 0.0040(5) -0.0005(5) C11 0.0246(7) 0.0324(8) 0.0211(7) -0.0012(6) 0.0023(6) -0.0038(6) C12 0.0234(7) 0.0332(8) 0.0264(8) -0.0011(6) 0.0006(6) -0.0040(6) C13 0.0286(8) 0.0252(7) 0.0293(8) -0.0041(6) 0.0065(6) -0.0051(6) C14 0.0433(9) 0.0202(6) 0.0234(8) -0.0011(5) 0.0067(6) -0.0010(6) C15 0.0316(8) 0.0226(7) 0.0251(8) -0.0038(6) 0.0012(6) 0.0034(6) C16 0.0327(9) 0.0504(11) 0.0289(9) 0.0106(8) -0.0029(7) -0.0091(8) C17 0.0374(9) 0.0404(9) 0.0409(11) 0.0027(8) 0.0099(8) -0.0130(8) C18 0.0446(11) 0.0397(10) 0.0422(11) 0.0064(8) -0.0082(8) 0.0081(8) C19 0.0242(7) 0.0289(7) 0.0301(8) 0.0065(6) 0.0057(6) 0.0042(6) C20 0.0490(11) 0.0376(9) 0.0254(9) 0.0071(7) 0.0088(7) 0.0065(8) C21 0.0586(12) 0.0375(9) 0.0256(9) -0.0014(7) 0.0032(8) 0.0022(8) C22 0.0345(8) 0.0297(8) 0.0299(9) -0.0001(6) -0.0001(7) -0.0004(6) C23 0.0308(8) 0.0283(7) 0.0242(8) 0.0045(6) -0.0011(6) -0.0004(6) C24 0.0324(8) 0.0265(7) 0.0248(8) 0.0024(6) 0.0003(6) 0.0014(6) C25 0.114(2) 0.0465(12) 0.0294(11) 0.0110(9) 0.0136(12) 0.0129(13) C26 0.0760(15) 0.0328(9) 0.0366(11) -0.0025(8) -0.0003(10) -0.0068(9) C27 0.0723(15) 0.0306(9) 0.0324(10) -0.0001(7) 0.0006(9) 0.0031(9) C28 0.0212(6) 0.0160(6) 0.0189(7) -0.0039(5) -0.0002(5) -0.0010(5) C29 0.0235(7) 0.0187(6) 0.0204(7) -0.0020(5) 0.0022(5) -0.0005(5) C30 0.0228(7) 0.0234(6) 0.0231(7) -0.0048(5) 0.0012(5) 0.0017(5) C31 0.0290(7) 0.0211(6) 0.0207(7) -0.0049(5) -0.0043(6) 0.0040(5) C32 0.0318(7) 0.0200(6) 0.0168(7) -0.0019(5) -0.0018(5) -0.0011(5) C33 0.0252(7) 0.0191(6) 0.0186(7) -0.0041(5) 0.0009(5) -0.0023(5) C34 0.0280(7) 0.0262(7) 0.0275(8) 0.0055(6) 0.0064(6) 0.0016(6) C35 0.0328(8) 0.0342(8) 0.0263(8) -0.0022(6) -0.0060(6) 0.0091(6) C36 0.0276(8) 0.0352(8) 0.0287(8) 0.0038(6) 0.0069(6) -0.0012(6) C37 0.0164(6) 0.0200(6) 0.0175(6) -0.0003(5) 0.0018(5) 0.0021(5) C38 0.0177(6) 0.0205(6) 0.0179(7) -0.0005(5) 0.0020(5) 0.0021(5) C39 0.0188(6) 0.0201(6) 0.0223(7) 0.0007(5) 0.0025(5) 0.0001(5) C40 0.0198(6) 0.0234(6) 0.0201(7) 0.0026(5) 0.0022(5) 0.0024(5) C41 0.0200(6) 0.0271(7) 0.0179(7) 0.0001(5) -0.0015(5) 0.0016(5) C42 0.0177(6) 0.0232(6) 0.0216(7) -0.0008(5) 0.0000(5) -0.0012(5) C43 0.0257(7) 0.0244(7) 0.0204(7) 0.0005(5) -0.0010(5) -0.0048(5) C44 0.0272(7) 0.0278(7) 0.0238(8) 0.0055(6) -0.0008(6) -0.0013(6) C45 0.0325(8) 0.0312(8) 0.0271(8) 0.0014(6) -0.0041(6) -0.0104(6) C46 0.0480(10) 0.0204(7) 0.0249(8) -0.0035(6) -0.0105(7) 0.0060(6) C47 0.0460(10) 0.0232(7) 0.0235(8) -0.0035(6) -0.0038(7) -0.0006(6) C48 0.0268(7) 0.0242(7) 0.0213(7) -0.0005(5) 0.0017(5) 0.0024(5) C49 0.0256(7) 0.0293(8) 0.0380(9) 0.0123(7) 0.0011(6) 0.0004(6) C50 0.0247(7) 0.0334(8) 0.0305(9) 0.0048(6) -0.0012(6) 0.0007(6) C51 0.0364(9) 0.0288(8) 0.0294(9) 0.0013(6) 0.0097(7) 0.0082(6) C52 0.0285(8) 0.0426(9) 0.0248(8) 0.0076(7) 0.0041(6) 0.0071(7) C53 0.0339(9) 0.0320(8) 0.0336(9) 0.0031(7) 0.0120(7) 0.0086(7) C54 0.0300(8) 0.0359(8) 0.0329(9) 0.0098(7) 0.0086(7) 0.0102(6) C55 0.0248(7) 0.0229(7) 0.0263(8) -0.0004(6) -0.0006(6) 0.0009(5) C58 0.0363(9) 0.0405(9) 0.0282(9) -0.0026(7) 0.0103(7) 0.0082(7) C59 0.0590(12) 0.0341(9) 0.0248(9) -0.0028(7) 0.0029(8) 0.0030(8) C60 0.0392(10) 0.0294(8) 0.0523(12) 0.0000(8) -0.0037(8) 0.0051(7) C61 0.0383(9) 0.0272(8) 0.0373(10) -0.0046(7) 0.0061(7) -0.0024(7) C63 0.0288(9) 0.0364(9) 0.0692(15) 0.0092(9) 0.0102(9) 0.0017(7) C64 0.0404(9) 0.0352(8) 0.0255(8) -0.0084(7) 0.0091(7) -0.0131(7) C65 0.0342(8) 0.0339(8) 0.0213(8) -0.0041(6) 0.0011(6) 0.0030(6) O12 0.0279(7) 0.0280(7) 0.0365(10) 0.0047(6) 0.0002(6) -0.0120(6) C56 0.0275(11) 0.0281(11) 0.0336(16) 0.0085(14) -0.0005(14) -0.0027(8) C57 0.0225(9) 0.0424(12) 0.0418(13) 0.0083(10) -0.0056(8) -0.0118(8) C62 0.0370(11) 0.0386(11) 0.0301(11) 0.0000(9) -0.0032(9) -0.0162(9) O12' 0.044(4) 0.038(4) 0.051(5) 0.000(3) 0.007(3) -0.021(3) C56' 0.033(5) 0.046(6) 0.075(8) -0.025(5) 0.026(5) -0.009(4) C57' 0.038(6) 0.037(6) 0.049(9) 0.021(8) -0.012(8) -0.008(4) C62' 0.029(5) 0.043(6) 0.080(9) -0.015(6) 0.008(5) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O4 2.7194(12) . ? K1 O1 2.7284(12) . ? K1 O8 2.7614(12) 2_655 ? K1 O7 2.7673(13) . ? K1 O9 2.9288(13) 3_665 ? K2 O2 2.5619(12) . ? K2 O1 2.5804(12) . ? K2 O4 2.5875(12) . ? K2 O5 2.7174(12) . ? K3 O2 2.6852(13) . ? K3 O15 2.7597(13) 2 ? K3 O13 2.7696(13) . ? K3 O16 2.8358(14) . ? K3 O1 2.8926(13) . ? K4 O3 2.6596(13) . ? K4 O5 2.7055(11) . ? K4 O4 2.7348(12) . ? K4 O10 2.8046(13) . ? K4 O11 2.8432(12) . ? K5 O3 2.6261(14) . ? K5 O5 2.6358(11) . ? K5 O12 2.6386(14) . ? K5 O2 2.7362(12) . ? K5 O12' 2.858(7) . ? O1 C1 1.3193(17) . ? O2 C10 1.3201(18) . ? O3 C19 1.317(2) . ? O4 C28 1.3176(17) . ? O5 C37 1.3171(17) . ? O7 C47 1.433(2) . ? O7 C46 1.4351(19) . ? O8 C49 1.4392(19) . ? O8 C48 1.4400(18) . ? O8 K1 2.7614(12) 2_645 ? O9 C51 1.433(2) . ? O9 C50 1.4359(19) . ? O9 K1 2.9288(13) 3_665 ? O10 C52 1.429(2) . ? O10 C53 1.440(2) . ? O11 C55 1.4343(18) . ? O11 C54 1.443(2) . ? O13 C61 1.431(2) . ? O13 C58 1.437(2) . ? O14 C59 1.422(2) . ? O14 C60 1.429(3) . ? O15 C62 1.418(3) . ? O15 C63 1.424(2) . ? O15 C62' 1.759(11) . ? O15 K3 2.7597(13) 2_545 ? O16 C65 1.430(2) . ? O16 C64 1.437(2) . ? C1 C2 1.424(2) . ? C1 C6 1.429(2) . ? C2 C3 1.398(2) . ? C2 C7 1.512(2) . ? C3 C4 1.398(2) . ? C3 H3 0.9500 . ? C4 C5 1.396(2) . ? C4 C8 1.516(2) . ? C5 C6 1.396(2) . ? C5 H5 0.9500 . ? C6 C9 1.511(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.419(2) . ? C10 C11 1.429(2) . ? C11 C12 1.394(2) . ? C11 C16 1.514(2) . ? C12 C13 1.387(2) . ? C12 H12 0.9500 . ? C13 C14 1.391(3) . ? C13 C17 1.521(2) . ? C14 C15 1.404(2) . ? C14 H14 0.9500 . ? C15 C18 1.511(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.422(2) . ? C19 C20 1.431(3) . ? C20 C21 1.391(3) . ? C20 C25 1.513(3) . ? C21 C22 1.396(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 C26 1.517(3) . ? C23 C24 1.396(2) . ? C23 H23 0.9500 . ? C24 C27 1.502(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.426(2) . ? C28 C33 1.428(2) . ? C29 C30 1.395(2) . ? C29 C34 1.513(2) . ? C30 C31 1.399(2) . ? C30 H30 0.9500 . ? C31 C32 1.401(2) . ? C31 C35 1.515(2) . ? C32 C33 1.393(2) . ? C32 H32 0.9500 . ? C33 C36 1.511(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.426(2) . ? C37 C38 1.4294(19) . ? C38 C39 1.393(2) . ? C38 C43 1.504(2) . ? C39 C40 1.395(2) . ? C39 H39 0.9500 . ? C40 C41 1.397(2) . ? C40 C44 1.515(2) . ? C41 C42 1.397(2) . ? C41 H41 0.9500 . ? C42 C45 1.510(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.512(2) 3_666 ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C46 1.512(2) 3_666 ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C55 1.511(2) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.512(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C53 1.508(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.511(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C58 C59 1.503(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.511(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C63 C57 1.508(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.510(2) 3_566 ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C64 1.510(2) 3_566 ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O12 C57 1.431(3) . ? O12 C56 1.433(4) . ? C56 C62 1.510(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? O12' C57' 1.394(19) . ? O12' C56' 1.431(13) . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? C57' C62' 1.473(18) . ? C57' H57C 0.9900 . ? C57' H57D 0.9900 . ? C62' H62C 0.9900 . ? C62' H62D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 K1 O1 87.39(3) . . ? O4 K1 O8 165.23(4) . 2_655 ? O1 K1 O8 105.28(4) . 2_655 ? O4 K1 O7 96.01(3) . . ? O1 K1 O7 105.43(5) . . ? O8 K1 O7 73.60(4) 2_655 . ? O4 K1 O9 106.35(3) . 3_665 ? O1 K1 O9 129.68(4) . 3_665 ? O8 K1 O9 71.57(3) 2_655 3_665 ? O7 K1 O9 120.27(4) . 3_665 ? O2 K2 O1 97.48(4) . . ? O2 K2 O4 167.37(4) . . ? O1 K2 O4 93.48(4) . . ? O2 K2 O5 88.85(5) . . ? O1 K2 O5 115.46(3) . . ? O4 K2 O5 92.10(4) . . ? O2 K3 O15 144.01(4) . 2 ? O2 K3 O13 98.04(4) . . ? O15 K3 O13 76.19(4) 2 . ? O2 K3 O16 94.36(4) . . ? O15 K3 O16 75.30(4) 2 . ? O13 K3 O16 146.10(4) . . ? O2 K3 O1 87.66(3) . . ? O15 K3 O1 127.31(4) 2 . ? O13 K3 O1 90.20(4) . . ? O16 K3 O1 121.83(4) . . ? O3 K4 O5 79.63(4) . . ? O3 K4 O4 97.24(4) . . ? O5 K4 O4 89.21(4) . . ? O3 K4 O10 136.03(4) . . ? O5 K4 O10 98.43(4) . . ? O4 K4 O10 126.73(4) . . ? O3 K4 O11 96.44(4) . . ? O5 K4 O11 175.21(3) . . ? O4 K4 O11 94.03(4) . . ? O10 K4 O11 82.45(4) . . ? O3 K5 O5 81.53(4) . . ? O3 K5 O12 98.41(5) . . ? O5 K5 O12 167.36(5) . . ? O3 K5 O2 108.67(5) . . ? O5 K5 O2 86.95(4) . . ? O12 K5 O2 104.90(5) . . ? O3 K5 O12' 97.77(17) . . ? O5 K5 O12' 147.51(18) . . ? O12 K5 O12' 19.86(17) . . ? O2 K5 O12' 123.17(18) . . ? C1 O1 K2 159.53(9) . . ? C1 O1 K1 104.55(8) . . ? K2 O1 K1 89.42(3) . . ? C1 O1 K3 80.96(8) . . ? K2 O1 K3 84.96(3) . . ? K1 O1 K3 174.37(4) . . ? C10 O2 K2 159.66(11) . . ? C10 O2 K3 103.20(9) . . ? K2 O2 K3 89.75(4) . . ? C10 O2 K5 96.66(9) . . ? K2 O2 K5 79.39(4) . . ? K3 O2 K5 147.63(5) . . ? C19 O3 K5 118.23(10) . . ? C19 O3 K4 129.82(10) . . ? K5 O3 K4 99.81(4) . . ? C28 O4 K2 139.91(9) . . ? C28 O4 K1 103.05(8) . . ? K2 O4 K1 89.47(3) . . ? C28 O4 K4 108.14(8) . . ? K2 O4 K4 83.36(4) . . ? K1 O4 K4 139.20(4) . . ? C37 O5 K5 136.33(9) . . ? C37 O5 K4 111.30(8) . . ? K5 O5 K4 98.40(4) . . ? C37 O5 K2 135.47(9) . . ? K5 O5 K2 78.47(4) . . ? K4 O5 K2 81.53(4) . . ? C47 O7 C46 109.32(12) . . ? C47 O7 K1 118.77(10) . . ? C46 O7 K1 123.16(9) . . ? C49 O8 C48 109.67(11) . . ? C49 O8 K1 122.60(9) . 2_645 ? C48 O8 K1 126.34(9) . 2_645 ? C51 O9 C50 108.34(12) . . ? C51 O9 K1 125.32(9) . 3_665 ? C50 O9 K1 126.14(9) . 3_665 ? C52 O10 C53 109.75(12) . . ? C52 O10 K4 120.80(10) . . ? C53 O10 K4 121.25(9) . . ? C55 O11 C54 108.48(12) . . ? C55 O11 K4 152.82(9) . . ? C54 O11 K4 95.92(8) . . ? C61 O13 C58 108.97(13) . . ? C61 O13 K3 128.72(10) . . ? C58 O13 K3 121.56(10) . . ? C59 O14 C60 110.04(14) . . ? C62 O15 C63 108.66(15) . . ? C62 O15 C62' 50.0(5) . . ? C63 O15 C62' 100.2(4) . . ? C62 O15 K3 114.45(11) . 2_545 ? C63 O15 K3 132.41(11) . 2_545 ? C62' O15 K3 122.6(4) . 2_545 ? C65 O16 C64 108.88(12) . . ? C65 O16 K3 117.19(9) . . ? C64 O16 K3 127.48(9) . . ? O1 C1 C2 120.99(13) . . ? O1 C1 C6 121.63(13) . . ? C2 C1 C6 117.36(13) . . ? C3 C2 C1 120.25(13) . . ? C3 C2 C7 121.37(14) . . ? C1 C2 C7 118.37(13) . . ? C2 C3 C4 122.63(14) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 116.88(14) . . ? C5 C4 C8 121.32(15) . . ? C3 C4 C8 121.80(15) . . ? C6 C5 C4 122.75(14) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 120.13(14) . . ? C5 C6 C9 120.97(14) . . ? C1 C6 C9 118.88(13) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C15 121.93(14) . . ? O2 C10 C11 120.53(14) . . ? C15 C10 C11 117.54(14) . . ? C12 C11 C10 120.19(15) . . ? C12 C11 C16 120.12(15) . . ? C10 C11 C16 119.68(14) . . ? C13 C12 C11 122.51(16) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 117.32(15) . . ? C12 C13 C17 120.84(16) . . ? C14 C13 C17 121.84(16) . . ? C13 C14 C15 122.73(15) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C10 119.69(15) . . ? C14 C15 C18 122.01(16) . . ? C10 C15 C18 118.27(15) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 C24 121.79(16) . . ? O3 C19 C20 121.95(15) . . ? C24 C19 C20 116.26(15) . . ? C21 C20 C19 120.95(16) . . ? C21 C20 C25 120.41(19) . . ? C19 C20 C25 118.64(17) . . ? C20 C21 C22 122.33(18) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 116.94(16) . . ? C23 C22 C26 121.01(16) . . ? C21 C22 C26 122.04(17) . . ? C22 C23 C24 122.77(16) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C19 120.72(15) . . ? C23 C24 C27 120.65(15) . . ? C19 C24 C27 118.60(15) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 C29 121.29(13) . . ? O4 C28 C33 121.31(13) . . ? C29 C28 C33 117.39(13) . . ? C30 C29 C28 120.36(13) . . ? C30 C29 C34 121.15(13) . . ? C28 C29 C34 118.48(13) . . ? C29 C30 C31 122.28(14) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C30 C31 C32 117.30(14) . . ? C30 C31 C35 120.98(14) . . ? C32 C31 C35 121.68(14) . . ? C33 C32 C31 122.36(14) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C32 C33 C28 120.26(13) . . ? C32 C33 C36 121.00(14) . . ? C28 C33 C36 118.72(13) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C42 121.73(12) . . ? O5 C37 C38 121.55(13) . . ? C42 C37 C38 116.72(12) . . ? C39 C38 C37 120.78(13) . . ? C39 C38 C43 120.44(13) . . ? C37 C38 C43 118.75(12) . . ? C38 C39 C40 122.39(13) . . ? C38 C39 H39 118.8 . . ? C40 C39 H39 118.8 . . ? C39 C40 C41 117.01(13) . . ? C39 C40 C44 121.20(13) . . ? C41 C40 C44 121.71(14) . . ? C40 C41 C42 122.62(14) . . ? C40 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C41 C42 C37 120.43(13) . . ? C41 C42 C45 120.74(14) . . ? C37 C42 C45 118.82(13) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O7 C46 C47 110.91(12) . 3_666 ? O7 C46 H46A 109.5 . . ? C47 C46 H46A 109.5 3_666 . ? O7 C46 H46B 109.5 . . ? C47 C46 H46B 109.5 3_666 . ? H46A C46 H46B 108.0 . . ? O7 C47 C46 110.23(15) . 3_666 ? O7 C47 H47A 109.6 . . ? C46 C47 H47A 109.6 3_666 . ? O7 C47 H47B 109.6 . . ? C46 C47 H47B 109.6 3_666 . ? H47A C47 H47B 108.1 . . ? O8 C48 C55 110.35(12) . . ? O8 C48 H48A 109.6 . . ? C55 C48 H48A 109.6 . . ? O8 C48 H48B 109.6 . . ? C55 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? O8 C49 C54 110.04(14) . . ? O8 C49 H49A 109.7 . . ? C54 C49 H49A 109.7 . . ? O8 C49 H49B 109.7 . . ? C54 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? O9 C50 C53 110.53(14) . . ? O9 C50 H50A 109.5 . . ? C53 C50 H50A 109.5 . . ? O9 C50 H50B 109.5 . . ? C53 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? O9 C51 C52 110.87(13) . . ? O9 C51 H51A 109.5 . . ? C52 C51 H51A 109.5 . . ? O9 C51 H51B 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? O10 C52 C51 111.50(14) . . ? O10 C52 H52A 109.3 . . ? C51 C52 H52A 109.3 . . ? O10 C52 H52B 109.3 . . ? C51 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? O10 C53 C50 110.25(13) . . ? O10 C53 H53A 109.6 . . ? C50 C53 H53A 109.6 . . ? O10 C53 H53B 109.6 . . ? C50 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? O11 C54 C49 109.59(14) . . ? O11 C54 H54A 109.8 . . ? C49 C54 H54A 109.8 . . ? O11 C54 H54B 109.8 . . ? C49 C54 H54B 109.8 . . ? H54A C54 H54B 108.2 . . ? O11 C55 C48 110.42(12) . . ? O11 C55 H55A 109.6 . . ? C48 C55 H55A 109.6 . . ? O11 C55 H55B 109.6 . . ? C48 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? O13 C58 C59 111.03(14) . . ? O13 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? O13 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? O14 C59 C58 111.64(15) . . ? O14 C59 H59A 109.3 . . ? C58 C59 H59A 109.3 . . ? O14 C59 H59B 109.3 . . ? C58 C59 H59B 109.3 . . ? H59A C59 H59B 108.0 . . ? O14 C60 C61 110.61(15) . . ? O14 C60 H60A 109.5 . . ? C61 C60 H60A 109.5 . . ? O14 C60 H60B 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? O13 C61 C60 109.46(14) . . ? O13 C61 H61A 109.8 . . ? C60 C61 H61A 109.8 . . ? O13 C61 H61B 109.8 . . ? C60 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? O15 C63 C57 110.01(16) . . ? O15 C63 C56' 95.0(4) . . ? C57 C63 C56' 80.5(4) . . ? O15 C63 H63A 109.7 . . ? C57 C63 H63A 109.7 . . ? O15 C63 H63B 109.7 . . ? C57 C63 H63B 109.7 . . ? C56' C63 H63B 147.0 . . ? H63A C63 H63B 108.2 . . ? O16 C64 C65 111.04(13) . 3_566 ? O16 C64 H64A 109.4 . . ? C65 C64 H64A 109.4 3_566 . ? O16 C64 H64B 109.4 . . ? C65 C64 H64B 109.4 3_566 . ? H64A C64 H64B 108.0 . . ? O16 C65 C64 110.48(14) . 3_566 ? O16 C65 H65A 109.6 . . ? C64 C65 H65A 109.6 3_566 . ? O16 C65 H65B 109.6 . . ? C64 C65 H65B 109.6 3_566 . ? H65A C65 H65B 108.1 . . ? C57 O12 C56 108.88(17) . . ? C57 O12 K5 108.96(11) . . ? C56 O12 K5 138.14(16) . . ? O12 C56 C62 109.5(3) . . ? O12 C56 H56A 109.8 . . ? C62 C56 H56A 109.8 . . ? O12 C56 H56B 109.8 . . ? C62 C56 H56B 109.8 . . ? H56A C56 H56B 108.2 . . ? O12 C57 C63 108.57(19) . . ? O12 C57 H57A 110.0 . . ? C63 C57 H57A 110.0 . . ? O12 C57 H57B 110.0 . . ? C63 C57 H57B 110.0 . . ? H57A C57 H57B 108.4 . . ? O15 C62 C56 108.8(2) . . ? O15 C62 H62A 109.9 . . ? C56 C62 H62A 109.9 . . ? O15 C62 H62B 109.9 . . ? C56 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C57' O12' C56' 109.7(9) . . ? C57' O12' K5 124.6(9) . . ? C56' O12' K5 121.2(6) . . ? O12' C56' C63 110.6(7) . . ? O12' C56' H56C 109.5 . . ? C63 C56' H56C 109.5 . . ? O12' C56' H56D 109.5 . . ? C63 C56' H56D 109.5 . . ? H56C C56' H56D 108.1 . . ? O12' C57' C62' 111.0(11) . . ? O12' C57' H57C 109.4 . . ? C62' C57' H57C 109.4 . . ? O12' C57' H57D 109.4 . . ? C62' C57' H57D 109.4 . . ? H57C C57' H57D 108.0 . . ? C57' C62' O15 106.8(10) . . ? C57' C62' H62C 110.4 . . ? O15 C62' H62C 110.4 . . ? C57' C62' H62D 110.4 . . ? O15 C62' H62D 110.4 . . ? H62C C62' H62D 108.6 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.93 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.829 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.057 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'crystallized on cooling in dioxane from 100 \%C to 20\%C.' # END data_jjm72 _database_code_depnum_ccdc_archive 'CCDC 651289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rubidium 4-Cl-2,6-Dimethylphenoxide Dioxane' _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 Cl2 O9 Rb2' _chemical_formula_sum 'C30 H44 Cl2 O9 Rb2' _chemical_formula_weight 790.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.324(2) _cell_length_b 19.659(4) _cell_length_c 32.308(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7192(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7525 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 26.178 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.441 _exptl_crystal_size_mid 0.371 _exptl_crystal_size_min 0.147 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 2.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_measurement_device_type 'Bruker SMART Apex2 CCD diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36628 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.67 _reflns_number_total 6412 _reflns_number_gt 5011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker,2006)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2006; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)' _refine_special_details ; Some regions of space were inaccessible to the detector, resulting in holes in the data collection and low coverage, particularly at higher resolution. The asymmetric unit is composed of a dimeric rubidium 4-Cl-2,6-dimethyl- phenoxide aggregate that is coordinated by 7 dioxane molecules. All seven dioxanes bridge to other aggregates to give a 7-connected three-dimensional network. 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^)+(0.0608P)^2^+17.5932P] 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 6412 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Rb1 Rb 0.63581(4) 0.07585(2) 0.345608(15) 0.02031(14) Uani 1 1 d . . . Rb2 Rb 0.90946(4) -0.01035(2) 0.387224(15) 0.02155(15) Uani 1 1 d . . . Cl1 Cl 0.31479(13) -0.22434(7) 0.30837(5) 0.0445(4) Uani 1 1 d . . . Cl2 Cl 0.73527(19) 0.30143(9) 0.53896(6) 0.0739(7) Uani 1 1 d . . . O1 O 0.7392(3) -0.05521(15) 0.33220(10) 0.0227(8) Uani 1 1 d . . . O2 O 0.7507(3) 0.07389(16) 0.42068(10) 0.0267(8) Uani 1 1 d . . . O3 O 0.4814(4) 0.11198(17) 0.27474(12) 0.0368(10) Uani 1 1 d . . . O4 O 0.3665(3) 0.09922(18) 0.19680(11) 0.0325(9) Uani 1 1 d . . . O5 O 0.5697(3) 0.21300(16) 0.36878(12) 0.0339(9) Uani 1 1 d . . . O6 O 0.5124(3) 0.35228(16) 0.37907(11) 0.0295(9) Uani 1 1 d . . . O7 O 1.0388(3) -0.03081(18) 0.46268(11) 0.0333(9) Uani 1 1 d . . . O8 O 1.1495(3) 0.03530(19) 0.37614(12) 0.0368(10) Uani 1 1 d . . . O9 O 1.3977(3) 0.04697(19) 0.36923(13) 0.0345(9) Uani 1 1 d . . . C1 C 0.6473(4) -0.0937(2) 0.32685(16) 0.0194(11) Uani 1 1 d . . . C2 C 0.6026(4) -0.1082(2) 0.28631(16) 0.0218(11) Uani 1 1 d . . . C3 C 0.5009(5) -0.1480(2) 0.28129(17) 0.0261(12) Uani 1 1 d . . . H3 H 0.4712 -0.1569 0.2543 0.031 Uiso 1 1 calc R . . C4 C 0.4438(4) -0.1745(2) 0.31566(18) 0.0274(13) Uani 1 1 d . . . C5 C 0.4845(5) -0.1625(2) 0.35505(18) 0.0293(13) Uani 1 1 d . . . H5 H 0.4440 -0.1814 0.3781 0.035 Uiso 1 1 calc R . . C6 C 0.5855(4) -0.1228(2) 0.36141(16) 0.0220(11) Uani 1 1 d . . . C7 C 0.6657(5) -0.0786(2) 0.24968(17) 0.0299(12) Uani 1 1 d . . . H7A H 0.6237 -0.0910 0.2243 0.045 Uiso 1 1 calc R . . H7B H 0.7464 -0.0965 0.2486 0.045 Uiso 1 1 calc R . . H7C H 0.6682 -0.0289 0.2522 0.045 Uiso 1 1 calc R . . C8 C 0.6309(5) -0.1087(3) 0.40456(17) 0.0317(13) Uani 1 1 d . . . H8A H 0.5777 -0.1293 0.4249 0.048 Uiso 1 1 calc R . . H8B H 0.6345 -0.0594 0.4091 0.048 Uiso 1 1 calc R . . H8C H 0.7101 -0.1282 0.4076 0.048 Uiso 1 1 calc R . . C9 C 0.7478(4) 0.1242(2) 0.44736(15) 0.0205(11) Uani 1 1 d . . . C10 C 0.6624(5) 0.1268(2) 0.47929(16) 0.0252(12) Uani 1 1 d . . . C11 C 0.6609(5) 0.1813(3) 0.50709(17) 0.0334(13) Uani 1 1 d . . . H11 H 0.6030 0.1827 0.5284 0.040 Uiso 1 1 calc R . . C12 C 0.7422(6) 0.2325(3) 0.50392(19) 0.0382(15) Uani 1 1 d . . . C13 C 0.8269(5) 0.2317(3) 0.4734(2) 0.0378(15) Uani 1 1 d . . . H13 H 0.8818 0.2681 0.4715 0.045 Uiso 1 1 calc R . . C14 C 0.8329(5) 0.1784(2) 0.44519(17) 0.0272(12) Uani 1 1 d . . . C15 C 0.5721(5) 0.0708(3) 0.4817(2) 0.0414(15) Uani 1 1 d . . . H15A H 0.5180 0.0797 0.5047 0.062 Uiso 1 1 calc R . . H15B H 0.6121 0.0272 0.4861 0.062 Uiso 1 1 calc R . . H15C H 0.5275 0.0690 0.4557 0.062 Uiso 1 1 calc R . . C16 C 0.9244(5) 0.1767(3) 0.4117(2) 0.0463(16) Uani 1 1 d . . . H16A H 0.9718 0.2183 0.4128 0.069 Uiso 1 1 calc R . . H16B H 0.8854 0.1734 0.3847 0.069 Uiso 1 1 calc R . . H16C H 0.9758 0.1371 0.4157 0.069 Uiso 1 1 calc R . . C17 C 0.4222(5) 0.0504(2) 0.26245(16) 0.0291(13) Uani 1 1 d . . . H17A H 0.3396 0.0515 0.2725 0.035 Uiso 1 1 calc R . . H17B H 0.4620 0.0109 0.2754 0.035 Uiso 1 1 calc R . . C18 C 0.4228(5) 0.0421(3) 0.21665(16) 0.0278(12) Uani 1 1 d . . . H18A H 0.5052 0.0381 0.2067 0.033 Uiso 1 1 calc R . . H18B H 0.3806 -0.0003 0.2092 0.033 Uiso 1 1 calc R . . C19 C 0.4244(5) 0.1619(3) 0.20880(18) 0.0351(14) Uani 1 1 d . . . H19A H 0.3825 0.2010 0.1963 0.042 Uiso 1 1 calc R . . H19B H 0.5066 0.1619 0.1984 0.042 Uiso 1 1 calc R . . C20 C 0.4251(6) 0.1693(3) 0.25515(18) 0.0398(15) Uani 1 1 d . . . H20A H 0.4674 0.2115 0.2628 0.048 Uiso 1 1 calc R . . H20B H 0.3428 0.1732 0.2653 0.048 Uiso 1 1 calc R . . C21 C 0.6293(5) 0.2654(3) 0.34560(19) 0.0350(14) Uani 1 1 d . . . H21A H 0.6534 0.2474 0.3183 0.042 Uiso 1 1 calc R . . H21B H 0.7013 0.2799 0.3606 0.042 Uiso 1 1 calc R . . C22 C 0.5487(5) 0.3256(3) 0.33970(17) 0.0314(13) Uani 1 1 d . . . H22A H 0.5904 0.3613 0.3238 0.038 Uiso 1 1 calc R . . H22B H 0.4783 0.3115 0.3237 0.038 Uiso 1 1 calc R . . C23 C 0.4531(5) 0.3001(2) 0.40265(18) 0.0296(12) Uani 1 1 d . . . H23A H 0.3808 0.2855 0.3879 0.035 Uiso 1 1 calc R . . H23B H 0.4298 0.3183 0.4300 0.035 Uiso 1 1 calc R . . C24 C 0.5350(5) 0.2397(2) 0.40839(17) 0.0303(13) Uani 1 1 d . . . H24A H 0.6060 0.2541 0.4240 0.036 Uiso 1 1 calc R . . H24B H 0.4944 0.2039 0.4245 0.036 Uiso 1 1 calc R . . C25 C 0.9656(5) -0.0666(3) 0.49161(17) 0.0338(13) Uani 1 1 d . . . H25A H 1.0159 -0.0923 0.5112 0.041 Uiso 1 1 calc R . . H25B H 0.9153 -0.0996 0.4766 0.041 Uiso 1 1 calc R . . C26 C 1.1118(5) 0.0176(3) 0.48459(18) 0.0339(13) Uani 1 1 d . . . H26A H 1.1614 0.0430 0.4646 0.041 Uiso 1 1 calc R . . H26B H 1.1647 -0.0068 0.5040 0.041 Uiso 1 1 calc R . . C27 C 1.2245(5) -0.0233(3) 0.3747(2) 0.0479(17) Uani 1 1 d . . . H27A H 1.2328 -0.0387 0.3457 0.057 Uiso 1 1 calc R . . H27B H 1.1882 -0.0607 0.3908 0.057 Uiso 1 1 calc R . . C28 C 1.2023(5) 0.0902(3) 0.3544(2) 0.0403(15) Uani 1 1 d . . . H28A H 1.1517 0.1311 0.3569 0.048 Uiso 1 1 calc R . . H28B H 1.2085 0.0785 0.3247 0.048 Uiso 1 1 calc R . . C29 C 1.3231(5) 0.1056(3) 0.3713(2) 0.0371(14) Uani 1 1 d . . . H29A H 1.3591 0.1431 0.3551 0.045 Uiso 1 1 calc R . . H29B H 1.3162 0.1207 0.4004 0.045 Uiso 1 1 calc R . . C30 C 1.3443(5) -0.0073(3) 0.3921(2) 0.0428(16) Uani 1 1 d . . . H30A H 1.3366 0.0060 0.4215 0.051 Uiso 1 1 calc R . . H30B H 1.3950 -0.0482 0.3906 0.051 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 Rb1 0.0173(3) 0.0135(2) 0.0301(3) -0.00151(19) -0.00116(19) 0.00199(18) Rb2 0.0184(3) 0.0153(2) 0.0310(3) -0.00353(19) -0.00203(19) 0.00110(18) Cl1 0.0253(8) 0.0214(7) 0.0869(12) 0.0035(7) -0.0058(8) -0.0094(6) Cl2 0.0819(14) 0.0494(10) 0.0905(15) -0.0490(10) -0.0458(11) 0.0335(10) O1 0.0197(19) 0.0125(16) 0.036(2) -0.0025(15) -0.0025(15) -0.0023(14) O2 0.031(2) 0.0208(18) 0.028(2) -0.0078(15) -0.0002(16) 0.0044(15) O3 0.052(3) 0.0209(19) 0.038(2) -0.0035(16) -0.0189(19) 0.0013(18) O4 0.033(2) 0.029(2) 0.036(2) 0.0037(17) -0.0130(17) -0.0105(17) O5 0.039(2) 0.0119(17) 0.051(3) -0.0029(17) -0.0039(18) 0.0008(16) O6 0.036(2) 0.0108(16) 0.042(2) 0.0001(15) 0.0060(17) 0.0003(15) O7 0.037(2) 0.035(2) 0.028(2) -0.0016(17) -0.0006(17) 0.0033(18) O8 0.019(2) 0.036(2) 0.055(3) 0.0065(19) 0.0054(18) -0.0028(17) O9 0.0184(19) 0.030(2) 0.056(3) -0.0061(18) 0.0043(17) -0.0027(16) C1 0.022(3) 0.005(2) 0.032(3) -0.0015(19) 0.002(2) 0.0060(19) C2 0.022(3) 0.009(2) 0.034(3) -0.001(2) 0.001(2) 0.003(2) C3 0.027(3) 0.014(2) 0.038(3) -0.005(2) -0.007(2) 0.004(2) C4 0.019(3) 0.007(2) 0.056(4) -0.002(2) -0.004(2) -0.004(2) C5 0.028(3) 0.014(2) 0.046(4) 0.010(2) 0.008(2) 0.004(2) C6 0.017(3) 0.014(2) 0.035(3) 0.002(2) 0.002(2) 0.004(2) C7 0.033(3) 0.023(3) 0.034(3) -0.004(2) -0.003(2) -0.008(2) C8 0.031(3) 0.029(3) 0.035(3) 0.007(3) 0.005(2) 0.004(2) C9 0.021(3) 0.012(2) 0.029(3) 0.003(2) -0.003(2) 0.0048(19) C10 0.023(3) 0.019(3) 0.033(3) 0.000(2) 0.002(2) 0.002(2) C11 0.033(3) 0.035(3) 0.032(3) -0.007(3) 0.000(2) 0.016(3) C12 0.042(4) 0.025(3) 0.049(4) -0.019(3) -0.020(3) 0.015(3) C13 0.030(3) 0.015(3) 0.068(4) 0.001(3) -0.020(3) 0.000(2) C14 0.023(3) 0.020(3) 0.039(3) 0.007(2) -0.003(2) 0.000(2) C15 0.035(4) 0.034(3) 0.055(4) 0.003(3) 0.014(3) -0.004(3) C16 0.035(4) 0.047(4) 0.057(4) 0.017(3) 0.005(3) -0.015(3) C17 0.035(3) 0.016(2) 0.037(3) -0.002(2) -0.004(2) -0.001(2) C18 0.027(3) 0.023(3) 0.033(3) -0.001(2) 0.003(2) -0.002(2) C19 0.037(4) 0.023(3) 0.045(4) 0.007(2) -0.009(3) -0.006(2) C20 0.056(4) 0.018(3) 0.045(4) -0.002(2) -0.012(3) 0.009(3) C21 0.032(3) 0.028(3) 0.045(4) -0.012(3) 0.005(3) 0.000(2) C22 0.038(3) 0.018(3) 0.038(3) 0.000(2) 0.001(3) -0.007(2) C23 0.031(3) 0.019(3) 0.039(3) 0.002(2) 0.000(2) 0.001(2) C24 0.031(3) 0.018(3) 0.042(4) 0.005(2) -0.008(3) 0.000(2) C25 0.038(4) 0.030(3) 0.033(3) 0.003(2) 0.002(3) -0.003(3) C26 0.028(3) 0.037(3) 0.037(4) 0.001(3) -0.007(2) 0.000(3) C27 0.028(3) 0.029(3) 0.086(5) -0.005(3) 0.016(3) -0.008(3) C28 0.028(3) 0.043(3) 0.050(4) 0.017(3) 0.011(3) 0.006(3) C29 0.032(3) 0.024(3) 0.055(4) -0.005(3) 0.013(3) -0.001(2) C30 0.026(3) 0.031(3) 0.071(5) 0.013(3) 0.007(3) 0.011(3) _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 Rb1 O2 2.753(3) . ? Rb1 O9 2.860(4) 1_455 ? Rb1 O1 2.863(3) . ? Rb1 O5 2.896(3) . ? Rb1 O3 2.967(4) . ? Rb1 O4 2.986(4) 6_656 ? Rb1 C29 3.683(6) 1_455 ? Rb2 O2 2.673(3) . ? Rb2 O1 2.767(3) . ? Rb2 O6 2.854(3) 8_755 ? Rb2 O7 2.872(4) . ? Rb2 O8 2.884(4) . ? Rb2 O4 3.499(4) 6_656 ? Rb2 C18 3.514(5) 6_656 ? Rb2 C22 3.604(5) 8_755 ? Cl1 C4 1.775(5) . ? Cl2 C12 1.768(5) . ? O1 C1 1.298(6) . ? O3 C17 1.440(6) . ? O3 C20 1.441(6) . ? O2 C9 1.312(6) . ? O4 C18 1.442(6) . ? O4 C19 1.448(6) . ? O4 Rb1 2.986(4) 6_556 ? O4 Rb2 3.499(4) 6_556 ? O5 C24 1.438(7) . ? O5 C21 1.441(7) . ? O6 C22 1.436(6) . ? O6 C23 1.444(6) . ? O6 Rb2 2.854(3) 8_765 ? O7 C25 1.434(6) . ? O7 C26 1.445(6) . ? O8 C28 1.420(6) . ? O8 C27 1.432(7) . ? O9 C29 1.430(6) . ? O9 C30 1.431(7) . ? O9 Rb1 2.860(4) 1_655 ? C1 C2 1.433(7) . ? C1 C6 1.436(7) . ? C2 C3 1.402(7) . ? C2 C7 1.500(7) . ? C3 C4 1.386(7) . ? C3 H3 0.9500 . ? C4 C5 1.374(8) . ? C5 C6 1.400(7) . ? C5 H5 0.9500 . ? C6 C8 1.512(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.415(7) . ? C9 C14 1.438(7) . ? C10 C11 1.398(7) . ? C10 C15 1.504(7) . ? C11 C12 1.368(8) . ? C11 H11 0.9500 . ? C12 C13 1.376(9) . ? C13 C14 1.391(8) . ? C13 H13 0.9500 . ? C14 C16 1.498(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.489(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.505(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.505(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.517(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.513(8) 5_756 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C25 1.513(8) 5_756 ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C30 1.501(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.504(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 Rb1 3.683(6) 1_655 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rb1 O9 102.00(11) . 1_455 ? O2 Rb1 O1 85.84(10) . . ? O9 Rb1 O1 104.31(10) 1_455 . ? O2 Rb1 O5 84.69(10) . . ? O9 Rb1 O5 82.65(11) 1_455 . ? O1 Rb1 O5 169.25(10) . . ? O2 Rb1 O3 164.12(10) . . ? O9 Rb1 O3 72.41(12) 1_455 . ? O1 Rb1 O3 109.85(10) . . ? O5 Rb1 O3 79.88(10) . . ? O2 Rb1 O4 89.59(11) . 6_656 ? O9 Rb1 O4 168.03(11) 1_455 6_656 ? O1 Rb1 O4 73.22(10) . 6_656 ? O5 Rb1 O4 101.63(10) . 6_656 ? O3 Rb1 O4 97.16(11) . 6_656 ? O2 Rb1 C29 104.97(12) . 1_455 ? O9 Rb1 C29 20.75(11) 1_455 1_455 ? O1 Rb1 C29 124.74(11) . 1_455 ? O5 Rb1 C29 62.98(11) . 1_455 ? O3 Rb1 C29 64.48(13) . 1_455 ? O4 Rb1 C29 156.94(12) 6_656 1_455 ? O2 Rb2 O1 89.35(10) . . ? O2 Rb2 O6 146.33(11) . 8_755 ? O1 Rb2 O6 81.68(10) . 8_755 ? O2 Rb2 O7 94.96(10) . . ? O1 Rb2 O7 148.87(10) . . ? O6 Rb2 O7 77.74(10) 8_755 . ? O2 Rb2 O8 119.42(11) . . ? O1 Rb2 O8 132.53(11) . . ? O6 Rb2 O8 89.47(11) 8_755 . ? O7 Rb2 O8 70.64(11) . . ? O2 Rb2 O4 80.73(9) . 6_656 ? O1 Rb2 O4 66.48(9) . 6_656 ? O6 Rb2 O4 123.63(9) 8_755 6_656 ? O7 Rb2 O4 144.63(10) . 6_656 ? O8 Rb2 O4 80.97(10) . 6_656 ? O2 Rb2 C18 103.50(11) . 6_656 ? O1 Rb2 C18 60.64(11) . 6_656 ? O6 Rb2 C18 100.14(11) 8_755 6_656 ? O7 Rb2 C18 146.08(12) . 6_656 ? O8 Rb2 C18 75.51(12) . 6_656 ? O4 Rb2 C18 23.73(10) 6_656 6_656 ? O2 Rb2 C22 144.63(12) . 8_755 ? O1 Rb2 C22 62.13(11) . 8_755 ? O6 Rb2 C22 22.02(11) 8_755 8_755 ? O7 Rb2 C22 99.74(11) . 8_755 ? O8 Rb2 C22 95.84(12) . 8_755 ? O4 Rb2 C22 103.81(11) 6_656 8_755 ? C18 Rb2 C22 81.37(12) 6_656 8_755 ? C1 O1 Rb2 146.1(3) . . ? C1 O1 Rb1 102.6(3) . . ? Rb2 O1 Rb1 84.31(9) . . ? C17 O3 C20 109.3(4) . . ? C17 O3 Rb1 106.6(3) . . ? C20 O3 Rb1 141.9(3) . . ? C9 O2 Rb2 138.6(3) . . ? C9 O2 Rb1 123.8(3) . . ? Rb2 O2 Rb1 88.29(9) . . ? C18 O4 C19 110.1(4) . . ? C18 O4 Rb1 118.1(3) . 6_556 ? C19 O4 Rb1 130.5(3) . 6_556 ? C18 O4 Rb2 78.7(3) . 6_556 ? C19 O4 Rb2 131.9(3) . 6_556 ? Rb1 O4 Rb2 70.78(7) 6_556 6_556 ? C24 O5 C21 109.2(4) . . ? C24 O5 Rb1 129.8(3) . . ? C21 O5 Rb1 114.2(3) . . ? C22 O6 C23 109.9(4) . . ? C22 O6 Rb2 109.8(3) . 8_765 ? C23 O6 Rb2 140.2(3) . 8_765 ? C25 O7 C26 109.5(4) . . ? C25 O7 Rb2 109.1(3) . . ? C26 O7 Rb2 128.0(3) . . ? C28 O8 C27 110.2(4) . . ? C28 O8 Rb2 134.0(3) . . ? C27 O8 Rb2 108.3(3) . . ? C29 O9 C30 109.1(4) . . ? C29 O9 Rb1 114.1(3) . 1_655 ? C30 O9 Rb1 133.2(3) . 1_655 ? O1 C1 C2 121.4(4) . . ? O1 C1 C6 121.3(5) . . ? C2 C1 C6 117.4(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C7 121.1(5) . . ? C1 C2 C7 118.4(4) . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 121.4(5) . . ? C5 C4 Cl1 119.6(4) . . ? C3 C4 Cl1 119.0(4) . . ? C4 C5 C6 120.4(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 C8 121.1(5) . . ? C1 C6 C8 118.6(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 121.6(4) . . ? O2 C9 C14 120.6(5) . . ? C10 C9 C14 117.8(4) . . ? C11 C10 C9 120.3(5) . . ? C11 C10 C15 121.3(5) . . ? C9 C10 C15 118.3(5) . . ? C12 C11 C10 120.5(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 121.0(5) . . ? C11 C12 Cl2 119.1(5) . . ? C13 C12 Cl2 119.9(5) . . ? C12 C13 C14 120.8(5) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C9 119.6(5) . . ? C13 C14 C16 121.6(5) . . ? C9 C14 C16 118.8(5) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 111.4(4) . . ? O3 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O3 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O4 C18 C17 110.8(4) . . ? O4 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? O4 C19 C20 110.6(4) . . ? O4 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O3 C20 C19 111.3(4) . . ? O3 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? O3 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? O5 C21 C22 110.1(4) . . ? O5 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? O5 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.2 . . ? O6 C22 C21 110.4(4) . . ? O6 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? O6 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? O6 C23 C24 109.6(4) . . ? O6 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? O6 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O5 C24 C23 110.1(4) . . ? O5 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O5 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.2 . . ? O7 C25 C26 110.7(4) . 5_756 ? O7 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 5_756 . ? O7 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 5_756 . ? H25A C25 H25B 108.1 . . ? O7 C26 C25 109.7(4) . 5_756 ? O7 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 5_756 . ? O7 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 5_756 . ? H26A C26 H26B 108.2 . . ? O8 C27 C30 110.8(5) . . ? O8 C27 H27A 109.5 . . ? C30 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? C30 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O8 C28 C29 110.9(5) . . ? O8 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? O9 C29 C28 111.0(5) . . ? O9 C29 Rb1 45.1(2) . 1_655 ? C28 C29 Rb1 139.6(4) . 1_655 ? O9 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? Rb1 C29 H29A 66.7 1_655 . ? O9 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? Rb1 C29 H29B 109.8 1_655 . ? H29A C29 H29B 108.0 . . ? O9 C30 C27 110.1(5) . . ? O9 C30 H30A 109.6 . . ? C27 C30 H30A 109.6 . . ? O9 C30 H30B 109.6 . . ? C27 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.433 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.122 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'crystallized on cooling in dioxane from 100 \%C to 20\%C.' # END data_jjm93 _database_code_depnum_ccdc_archive 'CCDC 651290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rubidium 2-iPropylphenoxide Dioxane' _chemical_melting_point ? _chemical_formula_moiety 'C72 H102 O15 Rb6' _chemical_formula_sum 'C72 H102 O15 Rb6' _chemical_formula_weight 1720.36 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 19.0470(4) _cell_length_b 20.6118(5) _cell_length_c 20.0105(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.7130(10) _cell_angle_gamma 90.00 _cell_volume 7852.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8787 _cell_measurement_theta_min 2.223 _cell_measurement_theta_max 27.408 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.358 _exptl_crystal_size_mid 0.325 _exptl_crystal_size_min 0.257 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 3.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.26 _exptl_absorpt_correction_T_max 0.38 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS. University of G\"ottingen, Germany. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_measurement_device_type 'Bruker SMART Apex2 CCD diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133299 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14914 _reflns_number_gt 11405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker,2006)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2006; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)' _refine_special_details ; The asymmetric unit is composed of a hexameric rubidium 2-iPr-phenoxide aggregate that is coordinated by 9 dioxane molecules. All 9 dioxanes bridge to other aggregates to give a 9-connected three-dimensional network. 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^)+(0.0203P)^2^+6.0071P] 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 14914 _refine_ls_number_parameters 850 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.009 _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 Rb1 Rb 0.661631(13) 0.138358(12) 0.322711(12) 0.02057(6) Uani 1 1 d . . . Rb2 Rb 0.412736(13) 0.311666(12) 0.381409(13) 0.02307(7) Uani 1 1 d . . . Rb3 Rb 0.444043(13) 0.151281(12) 0.264956(12) 0.02026(6) Uani 1 1 d . . . Rb4 Rb 0.591728(13) 0.141159(12) 0.124764(12) 0.02212(6) Uani 1 1 d . . . Rb5 Rb 0.573573(13) 0.305033(12) 0.234049(12) 0.01949(6) Uani 1 1 d . . . Rb6 Rb 0.345699(14) 0.320009(13) 0.191261(13) 0.02591(7) Uani 1 1 d . . . O1 O 0.54381(9) 0.23018(8) 0.34926(8) 0.0207(4) Uani 1 1 d . . . O2 O 0.33019(9) 0.23799(8) 0.29521(9) 0.0238(4) Uani 1 1 d . . . O3 O 0.56323(9) 0.07652(8) 0.24235(8) 0.0220(4) Uani 1 1 d . . . O4 O 0.68271(9) 0.21133(8) 0.21063(8) 0.0207(4) Uani 1 1 d . . . O5 O 0.45217(9) 0.37564(8) 0.27153(9) 0.0237(4) Uani 1 1 d . . . O6 O 0.47420(9) 0.23364(9) 0.14913(8) 0.0242(4) Uani 1 1 d . . . O7 O 0.73332(12) 0.13911(12) 0.45345(10) 0.0473(6) Uani 1 1 d . . . O8 O 0.75102(10) 0.01936(9) 0.31244(11) 0.0391(5) Uani 1 1 d . . . O9 O 0.31906(11) 0.36547(11) 0.47063(10) 0.0406(6) Uani 1 1 d . . . O10 O 0.35297(10) 0.03532(8) 0.23512(9) 0.0274(4) Uani 1 1 d . . . O11 O 0.20571(11) 0.40773(11) 0.54581(10) 0.0426(6) Uani 1 1 d . . . O12 O 0.54958(10) 0.04624(9) 0.02411(9) 0.0295(5) Uani 1 1 d . . . O13 O 0.82797(10) -0.08500(9) 0.25853(10) 0.0339(5) Uani 1 1 d . . . O14 O 0.76952(12) 0.10962(11) 0.58687(10) 0.0455(6) Uani 1 1 d . . . O15 O 0.26347(10) -0.07516(9) 0.24117(10) 0.0357(5) Uani 1 1 d . . . C1 C 0.54258(13) 0.23265(12) 0.41484(13) 0.0181(6) Uani 1 1 d . . . C2 C 0.56715(13) 0.28838(12) 0.45174(13) 0.0204(6) Uani 1 1 d . . . C3 C 0.56131(14) 0.28968(14) 0.52051(13) 0.0282(7) Uani 1 1 d . . . H3 H 0.5774 0.3269 0.5444 0.034 Uiso 1 1 calc R . . C4 C 0.53282(15) 0.23869(15) 0.55593(14) 0.0336(7) Uani 1 1 d . . . H4 H 0.5297 0.2407 0.6032 0.040 Uiso 1 1 calc R . . C5 C 0.50914(15) 0.18516(15) 0.52112(14) 0.0310(7) Uani 1 1 d . . . H5 H 0.4892 0.1499 0.5445 0.037 Uiso 1 1 calc R . . C6 C 0.51404(14) 0.18206(13) 0.45232(13) 0.0238(6) Uani 1 1 d . . . H6 H 0.4975 0.1443 0.4296 0.029 Uiso 1 1 calc R . . C7 C 0.60037(14) 0.34354(12) 0.41352(13) 0.0244(6) Uani 1 1 d . . . H7 H 0.5701 0.3519 0.3728 0.029 Uiso 1 1 calc R . . C8 C 0.60689(18) 0.40724(14) 0.45216(16) 0.0425(8) Uani 1 1 d . . . H8A H 0.5607 0.4199 0.4680 0.064 Uiso 1 1 calc R . . H8B H 0.6247 0.4411 0.4228 0.064 Uiso 1 1 calc R . . H8C H 0.6395 0.4015 0.4905 0.064 Uiso 1 1 calc R . . C9 C 0.67270(15) 0.32288(14) 0.39006(15) 0.0347(7) Uani 1 1 d . . . H9A H 0.7037 0.3143 0.4290 0.052 Uiso 1 1 calc R . . H9B H 0.6927 0.3577 0.3632 0.052 Uiso 1 1 calc R . . H9C H 0.6680 0.2834 0.3629 0.052 Uiso 1 1 calc R . . C10 C 0.28980(14) 0.19868(12) 0.32871(13) 0.0210(6) Uani 1 1 d . . . C11 C 0.21613(14) 0.19323(12) 0.31336(13) 0.0224(6) Uani 1 1 d . . . C12 C 0.17673(15) 0.14877(13) 0.34827(14) 0.0284(7) Uani 1 1 d . . . H12 H 0.1279 0.1453 0.3379 0.034 Uiso 1 1 calc R . . C13 C 0.20576(16) 0.10906(14) 0.39783(14) 0.0312(7) Uani 1 1 d . . . H13 H 0.1775 0.0784 0.4201 0.037 Uiso 1 1 calc R . . C14 C 0.27624(16) 0.11475(13) 0.41418(14) 0.0287(7) Uani 1 1 d . . . H14 H 0.2968 0.0882 0.4483 0.034 Uiso 1 1 calc R . . C15 C 0.31731(14) 0.15923(13) 0.38077(13) 0.0236(6) Uani 1 1 d . . . H15 H 0.3656 0.1632 0.3934 0.028 Uiso 1 1 calc R . . C16 C 0.18485(14) 0.23381(13) 0.25676(14) 0.0258(6) Uani 1 1 d . . . H16 H 0.2100 0.2764 0.2572 0.031 Uiso 1 1 calc R . . C17 C 0.10643(14) 0.24790(15) 0.26353(17) 0.0372(8) Uani 1 1 d . . . H17A H 0.0798 0.2073 0.2592 0.056 Uiso 1 1 calc R . . H17B H 0.0908 0.2781 0.2283 0.056 Uiso 1 1 calc R . . H17C H 0.0985 0.2672 0.3074 0.056 Uiso 1 1 calc R . . C18 C 0.19713(16) 0.20181(15) 0.18910(14) 0.0363(8) Uani 1 1 d . . . H18A H 0.2475 0.1940 0.1843 0.054 Uiso 1 1 calc R . . H18B H 0.1799 0.2305 0.1531 0.054 Uiso 1 1 calc R . . H18C H 0.1718 0.1604 0.1865 0.054 Uiso 1 1 calc R . . C19 C 0.55688(13) 0.01322(12) 0.24511(13) 0.0198(6) Uani 1 1 d . . . C20 C 0.53365(13) -0.01987(13) 0.30301(13) 0.0216(6) Uani 1 1 d . . . C21 C 0.52594(14) -0.08696(13) 0.30188(14) 0.0264(7) Uani 1 1 d . . . H21 H 0.5100 -0.1083 0.3407 0.032 Uiso 1 1 calc R . . C22 C 0.54069(15) -0.12358(14) 0.24613(14) 0.0305(7) Uani 1 1 d . . . H22 H 0.5339 -0.1692 0.2463 0.037 Uiso 1 1 calc R . . C23 C 0.56547(15) -0.09278(13) 0.19025(14) 0.0297(7) Uani 1 1 d . . . H23 H 0.5773 -0.1174 0.1521 0.036 Uiso 1 1 calc R . . C24 C 0.57293(14) -0.02649(13) 0.19006(13) 0.0251(6) Uani 1 1 d . . . H24 H 0.5897 -0.0063 0.1510 0.030 Uiso 1 1 calc R . . C25 C 0.51977(14) 0.01843(13) 0.36566(13) 0.0238(6) Uani 1 1 d . . . H25 H 0.5232 0.0654 0.3537 0.029 Uiso 1 1 calc R . . C26 C 0.57498(15) 0.00562(14) 0.42127(14) 0.0322(7) Uani 1 1 d . . . H26A H 0.5723 -0.0398 0.4354 0.048 Uiso 1 1 calc R . . H26B H 0.5661 0.0339 0.4594 0.048 Uiso 1 1 calc R . . H26C H 0.6219 0.0145 0.4046 0.048 Uiso 1 1 calc R . . C27 C 0.44606(15) 0.00733(14) 0.39151(14) 0.0329(7) Uani 1 1 d . . . H27A H 0.4112 0.0172 0.3560 0.049 Uiso 1 1 calc R . . H27B H 0.4386 0.0357 0.4299 0.049 Uiso 1 1 calc R . . H27C H 0.4412 -0.0381 0.4052 0.049 Uiso 1 1 calc R . . C28 C 0.72596(14) 0.24220(12) 0.17191(12) 0.0198(6) Uani 1 1 d . . . C29 C 0.80048(13) 0.24069(12) 0.18322(12) 0.0192(6) Uani 1 1 d . . . C30 C 0.84333(15) 0.27542(13) 0.14144(13) 0.0256(6) Uani 1 1 d . . . H30 H 0.8926 0.2750 0.1502 0.031 Uiso 1 1 calc R . . C31 C 0.81705(15) 0.31083(14) 0.08732(14) 0.0309(7) Uani 1 1 d . . . H31 H 0.8477 0.3342 0.0596 0.037 Uiso 1 1 calc R . . C32 C 0.74575(15) 0.31135(14) 0.07465(14) 0.0292(7) Uani 1 1 d . . . H32 H 0.7269 0.3347 0.0373 0.035 Uiso 1 1 calc R . . C33 C 0.70121(14) 0.27808(13) 0.11589(13) 0.0231(6) Uani 1 1 d . . . H33 H 0.6521 0.2794 0.1062 0.028 Uiso 1 1 calc R . . C34 C 0.82873(14) 0.20067(13) 0.24163(13) 0.0229(6) Uani 1 1 d . . . H34 H 0.7993 0.1606 0.2437 0.027 Uiso 1 1 calc R . . C35 C 0.90466(15) 0.17873(15) 0.23467(16) 0.0361(8) Uani 1 1 d . . . H35A H 0.9092 0.1554 0.1923 0.054 Uiso 1 1 calc R . . H35B H 0.9179 0.1500 0.2719 0.054 Uiso 1 1 calc R . . H35C H 0.9356 0.2167 0.2353 0.054 Uiso 1 1 calc R . . C36 C 0.82060(15) 0.23665(14) 0.30769(13) 0.0293(7) Uani 1 1 d . . . H36A H 0.8521 0.2743 0.3092 0.044 Uiso 1 1 calc R . . H36B H 0.8326 0.2075 0.3450 0.044 Uiso 1 1 calc R . . H36C H 0.7719 0.2513 0.3113 0.044 Uiso 1 1 calc R . . C37 C 0.46106(13) 0.43012(13) 0.23950(14) 0.0220(6) Uani 1 1 d . . . C38 C 0.46293(13) 0.49121(12) 0.27354(14) 0.0220(6) Uani 1 1 d . . . C39 C 0.47028(14) 0.54769(13) 0.23683(15) 0.0273(7) Uani 1 1 d . . . H39 H 0.4698 0.5881 0.2596 0.033 Uiso 1 1 calc R . . C40 C 0.47823(14) 0.54762(14) 0.16829(15) 0.0319(7) Uani 1 1 d . . . H40 H 0.4829 0.5872 0.1445 0.038 Uiso 1 1 calc R . . C41 C 0.47922(14) 0.48922(14) 0.13527(15) 0.0302(7) Uani 1 1 d . . . H41 H 0.4858 0.4883 0.0884 0.036 Uiso 1 1 calc R . . C42 C 0.47074(14) 0.43142(14) 0.16984(14) 0.0273(7) Uani 1 1 d . . . H42 H 0.4715 0.3916 0.1459 0.033 Uiso 1 1 calc R . . C43 C 0.45829(14) 0.49141(13) 0.34901(14) 0.0253(6) Uani 1 1 d . . . H43 H 0.4783 0.4493 0.3654 0.030 Uiso 1 1 calc R . . C44 C 0.38198(15) 0.49393(15) 0.37096(15) 0.0375(8) Uani 1 1 d . . . H44A H 0.3806 0.4884 0.4195 0.056 Uiso 1 1 calc R . . H44B H 0.3551 0.4591 0.3489 0.056 Uiso 1 1 calc R . . H44C H 0.3614 0.5359 0.3585 0.056 Uiso 1 1 calc R . . C45 C 0.50098(16) 0.54512(14) 0.38310(15) 0.0349(7) Uani 1 1 d . . . H45A H 0.5493 0.5438 0.3677 0.052 Uiso 1 1 calc R . . H45B H 0.5011 0.5388 0.4317 0.052 Uiso 1 1 calc R . . H45C H 0.4800 0.5873 0.3719 0.052 Uiso 1 1 calc R . . C46 C 0.43766(14) 0.21971(13) 0.09463(13) 0.0228(6) Uani 1 1 d . . . C47 C 0.45491(14) 0.24212(13) 0.03005(13) 0.0248(6) Uani 1 1 d . . . C48 C 0.41350(15) 0.22546(14) -0.02524(14) 0.0293(7) Uani 1 1 d . . . H48 H 0.4264 0.2410 -0.0679 0.035 Uiso 1 1 calc R . . C49 C 0.35437(16) 0.18726(15) -0.02125(14) 0.0342(7) Uani 1 1 d . . . H49 H 0.3268 0.1769 -0.0602 0.041 Uiso 1 1 calc R . . C50 C 0.33607(16) 0.16432(15) 0.04082(15) 0.0344(7) Uani 1 1 d . . . H50 H 0.2955 0.1379 0.0447 0.041 Uiso 1 1 calc R . . C51 C 0.37628(15) 0.17946(14) 0.09701(14) 0.0292(7) Uani 1 1 d . . . H51 H 0.3629 0.1626 0.1389 0.035 Uiso 1 1 calc R . . C52 C 0.51883(15) 0.28475(14) 0.02078(14) 0.0313(7) Uani 1 1 d . . . H52 H 0.5425 0.2902 0.0657 0.038 Uiso 1 1 calc R . . C53 C 0.49985(19) 0.35209(16) -0.00480(17) 0.0475(9) Uani 1 1 d . . . H53A H 0.4781 0.3487 -0.0497 0.071 Uiso 1 1 calc R . . H53B H 0.5424 0.3786 -0.0067 0.071 Uiso 1 1 calc R . . H53C H 0.4668 0.3724 0.0254 0.071 Uiso 1 1 calc R . . C54 C 0.57219(16) 0.25297(17) -0.02528(15) 0.0417(8) Uani 1 1 d . . . H54A H 0.5866 0.2108 -0.0068 0.063 Uiso 1 1 calc R . . H54B H 0.6135 0.2811 -0.0285 0.063 Uiso 1 1 calc R . . H54C H 0.5506 0.2468 -0.0699 0.063 Uiso 1 1 calc R . . C55 C 0.70487(17) 0.17418(16) 0.50743(15) 0.0382(8) Uani 1 1 d . . . H55A H 0.6574 0.1901 0.4944 0.046 Uiso 1 1 calc R . . H55B H 0.7349 0.2123 0.5180 0.046 Uiso 1 1 calc R . . C56 C 0.80183(19) 0.11690(19) 0.47312(17) 0.0535(10) Uani 1 1 d . . . H56A H 0.8325 0.1545 0.4836 0.064 Uiso 1 1 calc R . . H56B H 0.8225 0.0926 0.4358 0.064 Uiso 1 1 calc R . . C57 C 0.82589(16) 0.01968(15) 0.31109(18) 0.0432(9) Uani 1 1 d . . . H57A H 0.8455 0.0015 0.3535 0.052 Uiso 1 1 calc R . . H57B H 0.8428 0.0649 0.3071 0.052 Uiso 1 1 calc R . . C58 C 0.72743(16) -0.04629(14) 0.31707(17) 0.0384(8) Uani 1 1 d . . . H58A H 0.6754 -0.0471 0.3164 0.046 Uiso 1 1 calc R . . H58B H 0.7446 -0.0651 0.3601 0.046 Uiso 1 1 calc R . . C59 C 0.24929(18) 0.3607(2) 0.44551(16) 0.0534(10) Uani 1 1 d . . . H59A H 0.2300 0.3176 0.4565 0.064 Uiso 1 1 calc R . . H59B H 0.2485 0.3653 0.3962 0.064 Uiso 1 1 calc R . . C60 C 0.31993(17) 0.35879(16) 0.54139(15) 0.0403(8) Uani 1 1 d . . . H60A H 0.3688 0.3621 0.5593 0.048 Uiso 1 1 calc R . . H60B H 0.3014 0.3156 0.5535 0.048 Uiso 1 1 calc R . . C61 C 0.27816(15) 0.04126(13) 0.23998(14) 0.0289(7) Uani 1 1 d . . . H61A H 0.2564 0.0448 0.1946 0.035 Uiso 1 1 calc R . . H61B H 0.2670 0.0813 0.2648 0.035 Uiso 1 1 calc R . . C62 C 0.36890(16) -0.02390(13) 0.20103(15) 0.0324(7) Uani 1 1 d . . . H62A H 0.4205 -0.0292 0.1994 0.039 Uiso 1 1 calc R . . H62B H 0.3498 -0.0219 0.1545 0.039 Uiso 1 1 calc R . . C63 C 0.27624(18) 0.41038(18) 0.57143(17) 0.0505(9) Uani 1 1 d . . . H63A H 0.2766 0.4049 0.6206 0.061 Uiso 1 1 calc R . . H63B H 0.2966 0.4534 0.5615 0.061 Uiso 1 1 calc R . . C64 C 0.20469(18) 0.41257(19) 0.47521(16) 0.0536(10) Uani 1 1 d . . . H64A H 0.2224 0.4557 0.4621 0.064 Uiso 1 1 calc R . . H64B H 0.1558 0.4083 0.4576 0.064 Uiso 1 1 calc R . . C65 C 0.57038(15) -0.01787(14) 0.00505(15) 0.0324(7) Uani 1 1 d . . . H65A H 0.6120 -0.0313 0.0324 0.039 Uiso 1 1 calc R . . H65B H 0.5835 -0.0178 -0.0425 0.039 Uiso 1 1 calc R . . C66 C 0.48841(16) 0.06524(14) -0.01474(15) 0.0343(7) Uani 1 1 d . . . H66A H 0.4999 0.0670 -0.0626 0.041 Uiso 1 1 calc R . . H66B H 0.4734 0.1091 -0.0010 0.041 Uiso 1 1 calc R . . C67 C 0.75300(15) -0.08653(14) 0.26094(17) 0.0371(8) Uani 1 1 d . . . H67A H 0.7372 -0.1319 0.2666 0.045 Uiso 1 1 calc R . . H67B H 0.7325 -0.0701 0.2182 0.045 Uiso 1 1 calc R . . C68 C 0.85088(16) -0.01900(15) 0.25431(17) 0.0422(8) Uani 1 1 d . . . H68A H 0.8328 0.0002 0.2118 0.051 Uiso 1 1 calc R . . H68B H 0.9028 -0.0177 0.2542 0.051 Uiso 1 1 calc R . . C69 C 0.70062(18) 0.13248(17) 0.56719(16) 0.0472(9) Uani 1 1 d . . . H69A H 0.6804 0.1574 0.6043 0.057 Uiso 1 1 calc R . . H69B H 0.6695 0.0951 0.5572 0.057 Uiso 1 1 calc R . . C70 C 0.79798(19) 0.07394(16) 0.53315(16) 0.0470(9) Uani 1 1 d . . . H70A H 0.7679 0.0359 0.5226 0.056 Uiso 1 1 calc R . . H70B H 0.8455 0.0581 0.5461 0.056 Uiso 1 1 calc R . . C71 C 0.33792(16) -0.08109(14) 0.23604(16) 0.0366(8) Uani 1 1 d . . . H71A H 0.3488 -0.1212 0.2112 0.044 Uiso 1 1 calc R . . H71B H 0.3597 -0.0849 0.2814 0.044 Uiso 1 1 calc R . . C72 C 0.24794(16) -0.01610(13) 0.27503(15) 0.0331(7) Uani 1 1 d . . . H72A H 0.2675 -0.0181 0.3214 0.040 Uiso 1 1 calc R . . H72B H 0.1964 -0.0110 0.2772 0.040 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 Rb1 0.02092(15) 0.02077(13) 0.01990(13) 0.00119(11) -0.00153(11) 0.00118(11) Rb2 0.01916(15) 0.02406(14) 0.02601(14) -0.00154(11) 0.00114(11) 0.00238(11) Rb3 0.01971(14) 0.02054(13) 0.02053(13) 0.00084(11) 0.00068(10) -0.00029(11) Rb4 0.02376(15) 0.02567(14) 0.01703(13) -0.00265(11) 0.00241(11) -0.00389(11) Rb5 0.01843(14) 0.02004(13) 0.02000(13) 0.00089(10) 0.00066(10) -0.00112(10) Rb6 0.02451(16) 0.02512(15) 0.02770(15) 0.00478(12) -0.00568(12) -0.00368(12) O1 0.0241(11) 0.0216(10) 0.0163(10) -0.0017(8) -0.0022(8) 0.0003(8) O2 0.0183(10) 0.0229(10) 0.0303(11) 0.0038(8) 0.0009(8) -0.0032(8) O3 0.0256(11) 0.0174(10) 0.0234(10) -0.0016(8) 0.0049(8) -0.0030(8) O4 0.0161(10) 0.0250(10) 0.0212(10) 0.0022(8) 0.0027(8) -0.0036(8) O5 0.0239(11) 0.0178(10) 0.0295(11) 0.0010(8) 0.0007(8) -0.0003(8) O6 0.0263(11) 0.0292(11) 0.0166(10) 0.0010(8) -0.0055(8) -0.0050(8) O7 0.0438(15) 0.0720(17) 0.0254(12) 0.0053(11) -0.0099(10) 0.0167(12) O8 0.0292(13) 0.0247(11) 0.0636(15) -0.0036(10) 0.0023(11) 0.0078(9) O9 0.0304(13) 0.0610(15) 0.0311(12) 0.0092(11) 0.0103(10) 0.0132(11) O10 0.0272(12) 0.0217(10) 0.0331(11) -0.0048(9) -0.0034(9) -0.0037(8) O11 0.0380(14) 0.0550(14) 0.0357(13) 0.0062(11) 0.0155(11) 0.0118(11) O12 0.0268(12) 0.0285(11) 0.0327(11) -0.0072(9) -0.0067(9) -0.0028(9) O13 0.0161(11) 0.0290(11) 0.0567(14) -0.0064(10) 0.0040(10) 0.0046(9) O14 0.0564(16) 0.0466(14) 0.0323(12) 0.0018(11) -0.0175(11) 0.0059(12) O15 0.0302(13) 0.0220(11) 0.0549(14) -0.0055(10) -0.0005(10) -0.0035(9) C1 0.0119(14) 0.0200(14) 0.0224(14) -0.0013(11) -0.0002(11) 0.0038(11) C2 0.0179(15) 0.0225(14) 0.0206(14) -0.0014(11) -0.0025(11) 0.0042(11) C3 0.0261(17) 0.0349(17) 0.0235(15) -0.0070(13) -0.0026(13) 0.0011(13) C4 0.0346(19) 0.050(2) 0.0166(15) -0.0011(14) 0.0044(13) -0.0008(15) C5 0.0264(17) 0.0384(18) 0.0284(16) 0.0106(14) 0.0047(13) -0.0043(14) C6 0.0191(16) 0.0241(15) 0.0282(16) -0.0007(12) 0.0004(12) -0.0020(12) C7 0.0271(17) 0.0212(14) 0.0247(15) -0.0037(12) -0.0045(12) -0.0011(12) C8 0.063(2) 0.0246(17) 0.0394(19) -0.0031(14) -0.0038(17) -0.0084(16) C9 0.0259(18) 0.0345(17) 0.0437(19) 0.0088(15) 0.0018(14) -0.0039(14) C10 0.0214(16) 0.0187(14) 0.0231(15) -0.0042(12) 0.0035(12) 0.0006(12) C11 0.0174(15) 0.0192(14) 0.0307(16) -0.0058(12) 0.0027(12) -0.0005(12) C12 0.0199(16) 0.0265(16) 0.0394(17) -0.0059(14) 0.0095(13) -0.0035(13) C13 0.0322(19) 0.0299(16) 0.0322(17) 0.0018(14) 0.0124(14) -0.0050(14) C14 0.0364(19) 0.0267(16) 0.0234(15) 0.0001(12) 0.0064(13) 0.0013(13) C15 0.0196(16) 0.0271(15) 0.0240(15) -0.0051(12) 0.0004(12) 0.0004(12) C16 0.0153(15) 0.0219(15) 0.0401(17) 0.0000(13) -0.0013(13) 0.0005(12) C17 0.0200(17) 0.0320(18) 0.059(2) 0.0021(16) -0.0037(15) 0.0010(13) C18 0.037(2) 0.0371(18) 0.0338(18) 0.0049(14) -0.0059(15) 0.0076(15) C19 0.0143(14) 0.0239(15) 0.0210(14) 0.0021(12) -0.0021(11) -0.0002(11) C20 0.0160(15) 0.0258(15) 0.0228(15) 0.0018(12) -0.0008(12) 0.0008(12) C21 0.0267(17) 0.0239(16) 0.0286(16) 0.0070(13) 0.0010(13) 0.0012(12) C22 0.0350(19) 0.0239(15) 0.0324(17) -0.0009(13) -0.0011(14) 0.0012(13) C23 0.0355(19) 0.0268(16) 0.0266(16) -0.0039(13) -0.0036(13) 0.0090(13) C24 0.0288(17) 0.0261(16) 0.0202(15) 0.0022(12) 0.0006(12) 0.0027(13) C25 0.0262(17) 0.0241(15) 0.0211(14) 0.0036(12) 0.0012(12) 0.0013(12) C26 0.0368(19) 0.0327(17) 0.0268(16) 0.0026(13) -0.0020(14) 0.0024(14) C27 0.0322(18) 0.0381(18) 0.0288(17) 0.0000(14) 0.0071(14) 0.0014(14) C28 0.0210(16) 0.0186(14) 0.0198(14) -0.0049(11) 0.0007(12) -0.0005(11) C29 0.0170(15) 0.0195(14) 0.0210(14) -0.0067(11) 0.0007(11) -0.0007(11) C30 0.0185(16) 0.0297(16) 0.0289(16) -0.0057(13) 0.0041(13) -0.0029(12) C31 0.0290(18) 0.0358(17) 0.0281(16) 0.0050(14) 0.0060(13) -0.0123(14) C32 0.0320(18) 0.0313(17) 0.0244(15) 0.0047(13) -0.0001(13) -0.0040(14) C33 0.0191(16) 0.0292(16) 0.0210(14) -0.0013(12) -0.0010(12) -0.0016(12) C34 0.0162(15) 0.0250(15) 0.0273(15) -0.0015(12) -0.0021(12) -0.0013(12) C35 0.0245(18) 0.0355(18) 0.048(2) 0.0002(15) -0.0001(15) 0.0049(14) C36 0.0280(17) 0.0330(17) 0.0267(16) 0.0021(13) -0.0042(13) -0.0007(13) C37 0.0106(14) 0.0223(15) 0.0331(16) 0.0033(13) -0.0014(12) 0.0008(11) C38 0.0105(14) 0.0230(15) 0.0326(16) 0.0025(12) -0.0001(12) 0.0014(11) C39 0.0191(16) 0.0215(15) 0.0411(18) 0.0027(13) -0.0003(13) 0.0010(12) C40 0.0229(17) 0.0294(17) 0.0435(19) 0.0152(15) 0.0024(14) 0.0028(13) C41 0.0220(17) 0.0398(18) 0.0288(16) 0.0066(14) -0.0018(13) 0.0003(14) C42 0.0223(17) 0.0288(16) 0.0309(16) 0.0001(13) -0.0009(13) 0.0005(13) C43 0.0239(16) 0.0184(14) 0.0335(16) -0.0037(12) 0.0004(13) 0.0006(12) C44 0.0299(19) 0.0441(19) 0.0390(19) 0.0042(15) 0.0084(14) -0.0003(15) C45 0.0374(19) 0.0291(17) 0.0384(18) -0.0097(14) 0.0061(15) -0.0040(14) C46 0.0199(16) 0.0258(15) 0.0229(15) -0.0005(12) 0.0015(12) 0.0091(12) C47 0.0220(16) 0.0309(16) 0.0214(15) -0.0009(12) 0.0001(12) 0.0047(13) C48 0.0234(17) 0.0449(19) 0.0194(15) 0.0003(13) -0.0026(13) 0.0077(14) C49 0.0286(18) 0.048(2) 0.0260(16) -0.0097(15) -0.0075(13) 0.0052(15) C50 0.0265(18) 0.0389(18) 0.0377(18) -0.0084(15) -0.0009(14) -0.0032(14) C51 0.0248(17) 0.0394(18) 0.0235(15) 0.0034(13) 0.0016(13) -0.0009(14) C52 0.0283(18) 0.0393(18) 0.0261(16) 0.0072(14) -0.0005(13) -0.0066(14) C53 0.053(2) 0.049(2) 0.040(2) 0.0085(17) -0.0049(17) -0.0100(18) C54 0.0302(19) 0.062(2) 0.0331(18) 0.0069(16) 0.0038(15) -0.0037(16) C55 0.0310(19) 0.046(2) 0.0375(18) 0.0022(16) -0.0047(15) 0.0073(15) C56 0.051(2) 0.068(3) 0.041(2) 0.0002(19) 0.0042(18) 0.019(2) C57 0.030(2) 0.0240(17) 0.075(3) -0.0011(17) -0.0077(17) -0.0008(14) C58 0.0267(18) 0.0326(18) 0.056(2) 0.0068(16) 0.0086(16) 0.0019(14) C59 0.038(2) 0.094(3) 0.0282(18) -0.0013(19) 0.0049(16) 0.021(2) C60 0.0308(19) 0.058(2) 0.0318(18) 0.0094(16) 0.0021(14) 0.0022(16) C61 0.0310(18) 0.0227(15) 0.0328(17) -0.0024(13) -0.0051(14) 0.0030(13) C62 0.0297(18) 0.0314(17) 0.0360(18) -0.0074(14) -0.0021(14) -0.0002(14) C63 0.043(2) 0.063(2) 0.046(2) -0.0088(18) 0.0077(18) -0.0018(19) C64 0.037(2) 0.081(3) 0.043(2) 0.0271(19) 0.0123(17) 0.0223(19) C65 0.0284(18) 0.0342(17) 0.0345(17) -0.0081(14) -0.0015(14) 0.0011(14) C66 0.037(2) 0.0307(17) 0.0350(18) -0.0018(14) -0.0068(15) -0.0022(14) C67 0.0208(17) 0.0259(16) 0.064(2) -0.0056(15) -0.0007(15) -0.0026(13) C68 0.0258(19) 0.0388(19) 0.062(2) 0.0136(17) 0.0083(16) 0.0008(15) C69 0.044(2) 0.059(2) 0.039(2) 0.0001(18) 0.0012(17) -0.0070(18) C70 0.057(2) 0.0343(19) 0.049(2) -0.0019(16) -0.0167(18) 0.0105(17) C71 0.033(2) 0.0252(16) 0.052(2) -0.0054(15) -0.0023(16) 0.0015(14) C72 0.0322(19) 0.0272(16) 0.0398(18) -0.0035(14) 0.0011(14) -0.0009(14) _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 Rb1 O4 2.7399(17) . ? Rb1 O3 2.7464(17) . ? Rb1 O7 2.915(2) . ? Rb1 O1 2.9952(17) . ? Rb1 O8 2.9963(19) . ? Rb2 O5 2.6901(17) . ? Rb2 O2 2.7552(18) . ? Rb2 O9 2.7913(19) . ? Rb2 O1 3.0926(17) . ? Rb3 O3 2.7918(17) . ? Rb3 O2 2.8882(17) . ? Rb3 O6 2.9433(17) . ? Rb3 O1 2.9849(17) . ? Rb3 O10 3.0028(18) . ? Rb4 O3 2.7718(17) . ? Rb4 O4 2.8053(17) . ? Rb4 O11 2.903(2) 4_665 ? Rb4 O12 2.9039(18) . ? Rb4 O6 2.9912(18) . ? Rb5 O1 2.8451(17) . ? Rb5 O5 2.8515(17) . ? Rb5 O4 2.8861(17) . ? Rb5 O6 2.9057(17) . ? Rb5 O13 2.9428(18) 2_655 ? Rb6 O2 2.7034(17) . ? Rb6 O5 2.7951(18) . ? Rb6 O14 2.897(2) 4_565 ? Rb6 O6 3.1614(18) . ? Rb6 O15 3.3149(19) 2 ? O1 C1 1.314(3) . ? O2 C10 1.315(3) . ? O3 C19 1.312(3) . ? O4 C28 1.312(3) . ? O5 C37 1.307(3) . ? O6 C46 1.308(3) . ? O7 C55 1.421(4) . ? O7 C56 1.427(4) . ? O8 C57 1.427(3) . ? O8 C58 1.430(3) . ? O9 C59 1.410(4) . ? O9 C60 1.422(3) . ? O10 C62 1.435(3) . ? O10 C61 1.436(3) . ? O11 C64 1.416(4) . ? O11 C63 1.425(4) . ? O11 Rb4 2.903(2) 4_566 ? O12 C65 1.434(3) . ? O12 C66 1.436(3) . ? O13 C67 1.431(3) . ? O13 C68 1.432(3) . ? O13 Rb5 2.9428(18) 2_645 ? O14 C70 1.423(4) . ? O14 C69 1.438(4) . ? O14 Rb6 2.897(2) 4_666 ? O15 C72 1.428(3) . ? O15 C71 1.430(3) . ? O15 Rb6 3.3149(19) 2_545 ? C1 C6 1.404(3) . ? C1 C2 1.436(3) . ? C2 C3 1.384(4) . ? C2 C7 1.519(4) . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.527(4) . ? C7 C9 1.529(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.410(4) . ? C10 C11 1.432(4) . ? C11 C12 1.387(4) . ? C11 C16 1.516(4) . ? C12 C13 1.388(4) . ? C12 H12 0.9500 . ? C13 C14 1.377(4) . ? C13 H13 0.9500 . ? C14 C15 1.390(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C18 1.530(4) . ? C16 C17 1.532(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.413(4) . ? C19 C20 1.426(3) . ? C20 C21 1.391(4) . ? C20 C25 1.511(4) . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.374(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C27 1.528(4) . ? C25 C26 1.531(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.412(4) . ? C28 C29 1.431(4) . ? C29 C30 1.385(4) . ? C29 C34 1.516(4) . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.374(4) . ? C31 H31 0.9500 . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.526(4) . ? C34 C36 1.527(4) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.412(4) . ? C37 C38 1.431(4) . ? C38 C39 1.386(4) . ? C38 C43 1.516(4) . ? C39 C40 1.385(4) . ? C39 H39 0.9500 . ? C40 C41 1.374(4) . ? C40 H40 0.9500 . ? C41 C42 1.389(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C45 1.523(4) . ? C43 C44 1.532(4) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.420(4) . ? C46 C51 1.436(4) . ? C47 C48 1.383(4) . ? C47 C52 1.517(4) . ? C48 C49 1.379(4) . ? C48 H48 0.9500 . ? C49 C50 1.383(4) . ? C49 H49 0.9500 . ? C50 C51 1.377(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.519(4) . ? C52 C54 1.539(4) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C69 1.477(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C70 1.496(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C68 1.478(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C67 1.490(4) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C64 1.499(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C63 1.488(4) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C72 1.498(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C71 1.501(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.503(4) 3_655 ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C65 1.503(4) 3_655 ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Rb1 O3 83.67(5) . . ? O4 Rb1 O7 130.97(6) . . ? O3 Rb1 O7 145.20(6) . . ? O4 Rb1 O1 85.83(5) . . ? O3 Rb1 O1 83.99(5) . . ? O7 Rb1 O1 99.84(5) . . ? O4 Rb1 O8 107.20(5) . . ? O3 Rb1 O8 87.66(5) . . ? O7 Rb1 O8 79.28(6) . . ? O1 Rb1 O8 163.68(5) . . ? O5 Rb2 O2 85.79(5) . . ? O5 Rb2 O9 121.83(6) . . ? O2 Rb2 O9 104.82(6) . . ? O5 Rb2 O1 81.33(5) . . ? O2 Rb2 O1 91.12(5) . . ? O9 Rb2 O1 152.16(5) . . ? O3 Rb3 O2 174.14(5) . . ? O3 Rb3 O6 90.69(5) . . ? O2 Rb3 O6 88.49(5) . . ? O3 Rb3 O1 83.41(5) . . ? O2 Rb3 O1 90.79(5) . . ? O6 Rb3 O1 89.71(5) . . ? O3 Rb3 O10 89.78(5) . . ? O2 Rb3 O10 95.81(5) . . ? O6 Rb3 O10 115.32(5) . . ? O1 Rb3 O10 154.20(5) . . ? O3 Rb4 O4 82.00(5) . . ? O3 Rb4 O11 117.63(6) . 4_665 ? O4 Rb4 O11 93.09(5) . 4_665 ? O3 Rb4 O12 102.00(5) . . ? O4 Rb4 O12 157.69(5) . . ? O11 Rb4 O12 65.44(6) 4_665 . ? O3 Rb4 O6 90.08(5) . . ? O4 Rb4 O6 91.33(5) . . ? O11 Rb4 O6 152.28(6) 4_665 . ? O12 Rb4 O6 110.47(5) . . ? O1 Rb5 O5 83.16(5) . . ? O1 Rb5 O4 86.02(5) . . ? O5 Rb5 O4 167.94(5) . . ? O1 Rb5 O6 93.27(5) . . ? O5 Rb5 O6 83.86(5) . . ? O4 Rb5 O6 91.48(5) . . ? O1 Rb5 O13 121.26(5) . 2_655 ? O5 Rb5 O13 96.55(5) . 2_655 ? O4 Rb5 O13 93.59(5) . 2_655 ? O6 Rb5 O13 145.34(5) . 2_655 ? O2 Rb6 O5 84.75(5) . . ? O2 Rb6 O14 143.52(6) . 4_565 ? O5 Rb6 O14 123.24(6) . 4_565 ? O2 Rb6 O6 87.50(5) . . ? O5 Rb6 O6 80.21(5) . . ? O14 Rb6 O6 117.70(5) 4_565 . ? O2 Rb6 O15 90.54(5) . 2 ? O5 Rb6 O15 87.22(5) . 2 ? O14 Rb6 O15 70.18(6) 4_565 2 ? O6 Rb6 O15 167.40(5) . 2 ? C1 O1 Rb5 142.94(15) . . ? C1 O1 Rb3 123.74(15) . . ? Rb5 O1 Rb3 88.65(5) . . ? C1 O1 Rb1 103.74(14) . . ? Rb5 O1 Rb1 91.75(5) . . ? Rb3 O1 Rb1 91.33(5) . . ? C1 O1 Rb2 74.49(13) . . ? Rb5 O1 Rb2 93.19(5) . . ? Rb3 O1 Rb2 84.79(4) . . ? Rb1 O1 Rb2 173.64(6) . . ? C10 O2 Rb6 148.95(16) . . ? C10 O2 Rb2 110.62(15) . . ? Rb6 O2 Rb2 93.65(5) . . ? C10 O2 Rb3 100.37(14) . . ? Rb6 O2 Rb3 97.22(5) . . ? Rb2 O2 Rb3 93.11(5) . . ? C19 O3 Rb1 119.95(15) . . ? C19 O3 Rb4 122.31(15) . . ? Rb1 O3 Rb4 97.26(5) . . ? C19 O3 Rb3 117.76(15) . . ? Rb1 O3 Rb3 101.13(5) . . ? Rb4 O3 Rb3 93.04(5) . . ? C28 O4 Rb1 149.26(16) . . ? C28 O4 Rb4 106.00(14) . . ? Rb1 O4 Rb4 96.63(5) . . ? C28 O4 Rb5 103.84(14) . . ? Rb1 O4 Rb5 96.35(5) . . ? Rb4 O4 Rb5 90.56(5) . . ? C37 O5 Rb2 149.96(16) . . ? C37 O5 Rb6 99.97(15) . . ? Rb2 O5 Rb6 93.04(5) . . ? C37 O5 Rb5 101.05(14) . . ? Rb2 O5 Rb5 102.31(6) . . ? Rb6 O5 Rb5 102.69(5) . . ? C46 O6 Rb5 156.90(16) . . ? C46 O6 Rb3 114.74(15) . . ? Rb5 O6 Rb3 88.32(5) . . ? C46 O6 Rb4 96.11(14) . . ? Rb5 O6 Rb4 86.59(5) . . ? Rb3 O6 Rb4 85.73(5) . . ? C46 O6 Rb6 87.08(14) . . ? Rb5 O6 Rb6 93.14(5) . . ? Rb3 O6 Rb6 86.78(4) . . ? Rb4 O6 Rb6 172.51(6) . . ? C55 O7 C56 108.7(2) . . ? C55 O7 Rb1 120.41(17) . . ? C56 O7 Rb1 130.22(18) . . ? C57 O8 C58 108.8(2) . . ? C57 O8 Rb1 124.59(16) . . ? C58 O8 Rb1 126.15(16) . . ? C59 O9 C60 109.3(2) . . ? C59 O9 Rb2 110.99(17) . . ? C60 O9 Rb2 127.57(17) . . ? C62 O10 C61 109.2(2) . . ? C62 O10 Rb3 129.97(15) . . ? C61 O10 Rb3 119.15(14) . . ? C64 O11 C63 109.9(2) . . ? C64 O11 Rb4 125.4(2) . 4_566 ? C63 O11 Rb4 122.00(18) . 4_566 ? C65 O12 C66 109.5(2) . . ? C65 O12 Rb4 137.08(16) . . ? C66 O12 Rb4 113.25(15) . . ? C67 O13 C68 109.2(2) . . ? C67 O13 Rb5 128.06(16) . 2_645 ? C68 O13 Rb5 122.68(16) . 2_645 ? C70 O14 C69 109.1(2) . . ? C70 O14 Rb6 127.56(19) . 4_666 ? C69 O14 Rb6 117.82(18) . 4_666 ? C72 O15 C71 109.1(2) . . ? C72 O15 Rb6 102.75(15) . 2_545 ? C71 O15 Rb6 127.52(16) . 2_545 ? O1 C1 C6 121.6(2) . . ? O1 C1 C2 121.9(2) . . ? C6 C1 C2 116.4(2) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 C7 122.2(2) . . ? C1 C2 C7 118.3(2) . . ? C2 C3 C4 122.5(3) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 118.5(3) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 122.4(3) . . ? C5 C6 H6 118.8 . . ? C1 C6 H6 118.8 . . ? C2 C7 C8 114.7(2) . . ? C2 C7 C9 109.8(2) . . ? C8 C7 C9 109.5(2) . . ? C2 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C15 121.5(2) . . ? O2 C10 C11 121.6(2) . . ? C15 C10 C11 117.0(2) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 C16 122.3(2) . . ? C10 C11 C16 118.5(2) . . ? C11 C12 C13 122.7(3) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 119.0(3) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 122.3(3) . . ? C14 C15 H15 118.9 . . ? C10 C15 H15 118.9 . . ? C11 C16 C18 110.9(2) . . ? C11 C16 C17 113.7(2) . . ? C18 C16 C17 109.6(2) . . ? C11 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 C24 121.4(2) . . ? O3 C19 C20 122.8(2) . . ? C24 C19 C20 115.8(2) . . ? C21 C20 C19 119.8(2) . . ? C21 C20 C25 120.8(2) . . ? C19 C20 C25 119.4(2) . . ? C22 C21 C20 122.1(3) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 123.3(3) . . ? C23 C24 H24 118.3 . . ? C19 C24 H24 118.3 . . ? C20 C25 C27 112.8(2) . . ? C20 C25 C26 112.3(2) . . ? C27 C25 C26 110.3(2) . . ? C20 C25 H25 107.0 . . ? C27 C25 H25 107.0 . . ? C26 C25 H25 107.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 C33 121.5(2) . . ? O4 C28 C29 122.2(2) . . ? C33 C28 C29 116.3(2) . . ? C30 C29 C28 119.5(2) . . ? C30 C29 C34 123.0(2) . . ? C28 C29 C34 117.5(2) . . ? C29 C30 C31 122.5(3) . . ? C29 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C32 C31 C30 118.7(3) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C28 122.5(3) . . ? C32 C33 H33 118.8 . . ? C28 C33 H33 118.8 . . ? C29 C34 C35 114.0(2) . . ? C29 C34 C36 111.1(2) . . ? C35 C34 C36 110.1(2) . . ? C29 C34 H34 107.1 . . ? C35 C34 H34 107.1 . . ? C36 C34 H34 107.1 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C42 121.6(2) . . ? O5 C37 C38 121.6(2) . . ? C42 C37 C38 116.8(2) . . ? C39 C38 C37 119.2(2) . . ? C39 C38 C43 122.4(2) . . ? C37 C38 C43 118.4(2) . . ? C40 C39 C38 122.7(3) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C41 C40 C39 118.7(3) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 120.6(3) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 121.9(3) . . ? C41 C42 H42 119.1 . . ? C37 C42 H42 119.1 . . ? C38 C43 C45 113.7(2) . . ? C38 C43 C44 111.7(2) . . ? C45 C43 C44 110.2(2) . . ? C38 C43 H43 106.9 . . ? C45 C43 H43 106.9 . . ? C44 C43 H43 106.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O6 C46 C47 123.7(2) . . ? O6 C46 C51 120.8(2) . . ? C47 C46 C51 115.4(2) . . ? C48 C47 C46 120.4(3) . . ? C48 C47 C52 119.1(2) . . ? C46 C47 C52 120.5(2) . . ? C49 C48 C47 122.9(3) . . ? C49 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? C48 C49 C50 118.4(3) . . ? C48 C49 H49 120.8 . . ? C50 C49 H49 120.8 . . ? C51 C50 C49 120.4(3) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C46 122.5(3) . . ? C50 C51 H51 118.7 . . ? C46 C51 H51 118.7 . . ? C47 C52 C53 112.7(2) . . ? C47 C52 C54 111.9(2) . . ? C53 C52 C54 110.0(2) . . ? C47 C52 H52 107.3 . . ? C53 C52 H52 107.3 . . ? C54 C52 H52 107.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O7 C55 C69 110.5(3) . . ? O7 C55 H55A 109.5 . . ? C69 C55 H55A 109.5 . . ? O7 C55 H55B 109.5 . . ? C69 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? O7 C56 C70 110.2(3) . . ? O7 C56 H56A 109.6 . . ? C70 C56 H56A 109.6 . . ? O7 C56 H56B 109.6 . . ? C70 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? O8 C57 C68 110.9(3) . . ? O8 C57 H57A 109.5 . . ? C68 C57 H57A 109.5 . . ? O8 C57 H57B 109.5 . . ? C68 C57 H57B 109.5 . . ? H57A C57 H57B 108.0 . . ? O8 C58 C67 111.6(2) . . ? O8 C58 H58A 109.3 . . ? C67 C58 H58A 109.3 . . ? O8 C58 H58B 109.3 . . ? C67 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? O9 C59 C64 110.4(3) . . ? O9 C59 H59A 109.6 . . ? C64 C59 H59A 109.6 . . ? O9 C59 H59B 109.6 . . ? C64 C59 H59B 109.6 . . ? H59A C59 H59B 108.1 . . ? O9 C60 C63 110.1(3) . . ? O9 C60 H60A 109.6 . . ? C63 C60 H60A 109.6 . . ? O9 C60 H60B 109.6 . . ? C63 C60 H60B 109.6 . . ? H60A C60 H60B 108.2 . . ? O10 C61 C72 111.1(2) . . ? O10 C61 H61A 109.4 . . ? C72 C61 H61A 109.4 . . ? O10 C61 H61B 109.4 . . ? C72 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? O10 C62 C71 110.8(2) . . ? O10 C62 H62A 109.5 . . ? C71 C62 H62A 109.5 . . ? O10 C62 H62B 109.5 . . ? C71 C62 H62B 109.5 . . ? H62A C62 H62B 108.1 . . ? O11 C63 C60 111.1(3) . . ? O11 C63 H63A 109.4 . . ? C60 C63 H63A 109.4 . . ? O11 C63 H63B 109.4 . . ? C60 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? O11 C64 C59 110.8(3) . . ? O11 C64 H64A 109.5 . . ? C59 C64 H64A 109.5 . . ? O11 C64 H64B 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? O12 C65 C66 110.6(2) . 3_655 ? O12 C65 H65A 109.5 . . ? C66 C65 H65A 109.5 3_655 . ? O12 C65 H65B 109.5 . . ? C66 C65 H65B 109.5 3_655 . ? H65A C65 H65B 108.1 . . ? O12 C66 C65 110.4(2) . 3_655 ? O12 C66 H66A 109.6 . . ? C65 C66 H66A 109.6 3_655 . ? O12 C66 H66B 109.6 . . ? C65 C66 H66B 109.6 3_655 . ? H66A C66 H66B 108.1 . . ? O13 C67 C58 111.2(2) . . ? O13 C67 H67A 109.4 . . ? C58 C67 H67A 109.4 . . ? O13 C67 H67B 109.4 . . ? C58 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? O13 C68 C57 111.2(2) . . ? O13 C68 H68A 109.4 . . ? C57 C68 H68A 109.4 . . ? O13 C68 H68B 109.4 . . ? C57 C68 H68B 109.4 . . ? H68A C68 H68B 108.0 . . ? O14 C69 C55 109.9(3) . . ? O14 C69 H69A 109.7 . . ? C55 C69 H69A 109.7 . . ? O14 C69 H69B 109.7 . . ? C55 C69 H69B 109.7 . . ? H69A C69 H69B 108.2 . . ? O14 C70 C56 109.3(3) . . ? O14 C70 H70A 109.8 . . ? C56 C70 H70A 109.8 . . ? O14 C70 H70B 109.8 . . ? C56 C70 H70B 109.8 . . ? H70A C70 H70B 108.3 . . ? O15 C71 C62 111.8(2) . . ? O15 C71 H71A 109.3 . . ? C62 C71 H71A 109.3 . . ? O15 C71 H71B 109.3 . . ? C62 C71 H71B 109.3 . . ? H71A C71 H71B 107.9 . . ? O15 C72 C61 111.3(2) . . ? O15 C72 H72A 109.4 . . ? C61 C72 H72A 109.4 . . ? O15 C72 H72B 109.4 . . ? C61 C72 H72B 109.4 . . ? H72A C72 H72B 108.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.823 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.072 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'crystallized on cooling in dioxane and hexane from 100 \%C to 20\%C.' # END