# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email fjaekle@rutgers.edu _publ_contact_author_name 'Frieder Jaekle' loop_ _publ_author_name 'Haiyan Li' 'Roger A. Lalancette' 'Frieder Jaekle' data_072909lhy_42_cn_0m _database_code_depnum_ccdc_archive 'CCDC 828004' #TrackingRef '5704_web_deposit_cif_file_0_FriederJaekle_1306950851.072909lhy_42_CN_0mCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _vrf_PLAT029_072909lhy_42_cn_0m ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.90 RESPONSE: Even though we collected data out to 0.81 \%A resolution with copper radiation,the crystal diffracted poorly beyond 0.88\%A resolution (with only 60% of the theoretical data collected between 0.88 and 0.85 \%A, and only 21% of the theoretical data collected between 0.85 and 0.84 \%A). Larger crystals were not obtainable, and since the crystals of this compound are no longer available, we can only rely on the current data set. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 B2 N2 S4, 2(C16 H36 N)' _chemical_formula_sum 'C88 H128 B2 N4 S4' _chemical_formula_weight 1391.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6855(3) _cell_length_b 12.0398(3) _cell_length_c 16.0851(5) _cell_angle_alpha 78.460(2) _cell_angle_beta 74.957(2) _cell_angle_gamma 70.046(2) _cell_volume 2038.73(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9965 _cell_measurement_theta_min 3.94 _cell_measurement_theta_max 66.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5568 _exptl_absorpt_correction_T_max 0.7910 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; 'crystal mounted on a Cryoloop using Paratone-N' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Apex-II area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16583 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 66.95 _reflns_number_total 6548 _reflns_number_gt 5485 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX 2 (Bruker, 2006)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008b)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.6934P] 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 6548 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.053 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.118 _refine_ls_wR_factor_gt 0.111 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 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 S1 S 0.65911(4) 0.50429(4) 0.04477(3) 0.02118(13) Uani 1 1 d . . . C1 C 0.70528(17) 0.10514(15) 0.25011(12) 0.0199(4) Uani 1 1 d . . . B1 B 0.5820(2) 0.22353(18) 0.23396(14) 0.0204(5) Uani 1 1 d . . . N1 N 0.54202(15) 0.35433(14) 0.36908(11) 0.0261(4) Uani 1 1 d . . . S2 S 0.91841(4) 0.42191(4) 0.09479(3) 0.02407(14) Uani 1 1 d . . . C2 C 0.82051(17) 0.06624(15) 0.19189(12) 0.0206(4) Uani 1 1 d . . . N2 N 0.55200(16) 0.71975(13) 0.30543(11) 0.0263(4) Uani 1 1 d . . . C3 C 0.91507(18) -0.03502(16) 0.21573(13) 0.0238(4) Uani 1 1 d . . . H3 H 0.9906 -0.0591 0.1745 0.029 Uiso 1 1 calc R . . C4 C 0.90347(18) -0.10135(16) 0.29639(14) 0.0253(4) Uani 1 1 d . . . C5 C 0.79112(19) -0.06476(16) 0.35374(13) 0.0250(4) Uani 1 1 d . . . H5 H 0.7802 -0.1078 0.4100 0.030 Uiso 1 1 calc R . . C6 C 0.69295(18) 0.03338(16) 0.33179(13) 0.0217(4) Uani 1 1 d . . . C7 C 0.85606(19) 0.12347(17) 0.09974(13) 0.0250(4) Uani 1 1 d . . . H7A H 0.9233 0.1566 0.0960 0.038 Uiso 1 1 calc R . . H7B H 0.7836 0.1873 0.0841 0.038 Uiso 1 1 calc R . . H7C H 0.8842 0.0634 0.0597 0.038 Uiso 1 1 calc R . . C8 C 1.0075(2) -0.20913(18) 0.32130(15) 0.0357(5) Uani 1 1 d . . . H8A H 1.0271 -0.2691 0.2823 0.054 Uiso 1 1 calc R . . H8B H 0.9811 -0.2427 0.3812 0.054 Uiso 1 1 calc R . . H8C H 1.0815 -0.1855 0.3166 0.054 Uiso 1 1 calc R . . C9 C 0.57504(18) 0.05517(17) 0.40098(13) 0.0264(5) Uani 1 1 d . . . H9A H 0.5801 -0.0152 0.4444 0.040 Uiso 1 1 calc R . . H9B H 0.5036 0.0708 0.3745 0.040 Uiso 1 1 calc R . . H9C H 0.5650 0.1241 0.4290 0.040 Uiso 1 1 calc R . . C10 C 0.46327(18) 0.18023(15) 0.22866(12) 0.0210(4) Uani 1 1 d . . . C11 C 0.47947(18) 0.10818(16) 0.16408(13) 0.0230(4) Uani 1 1 d . . . C12 C 0.38435(19) 0.06681(16) 0.15714(14) 0.0260(5) Uani 1 1 d . . . H12 H 0.3993 0.0195 0.1124 0.031 Uiso 1 1 calc R . . C13 C 0.26956(19) 0.09237(17) 0.21302(14) 0.0278(5) Uani 1 1 d . . . C14 C 0.25157(19) 0.16399(17) 0.27546(14) 0.0273(5) Uani 1 1 d . . . H14 H 0.1738 0.1825 0.3153 0.033 Uiso 1 1 calc R . . C15 C 0.34253(18) 0.21034(17) 0.28266(13) 0.0244(4) Uani 1 1 d . . . C16 C 0.59791(19) 0.07616(17) 0.09564(13) 0.0266(5) Uani 1 1 d . . . H16A H 0.6649 0.0193 0.1225 0.040 Uiso 1 1 calc R . . H16B H 0.6211 0.1482 0.0692 0.040 Uiso 1 1 calc R . . H16C H 0.5844 0.0402 0.0509 0.040 Uiso 1 1 calc R . . C17 C 0.1663(2) 0.04962(19) 0.20488(16) 0.0358(5) Uani 1 1 d . . . H17A H 0.1930 0.0076 0.1536 0.054 Uiso 1 1 calc R . . H17B H 0.0923 0.1180 0.1990 0.054 Uiso 1 1 calc R . . H17C H 0.1466 -0.0046 0.2568 0.054 Uiso 1 1 calc R . . C18 C 0.30021(19) 0.2975(2) 0.34885(14) 0.0340(5) Uani 1 1 d . . . H18A H 0.2104 0.3146 0.3714 0.051 Uiso 1 1 calc R . . H18B H 0.3187 0.3714 0.3213 0.051 Uiso 1 1 calc R . . H18C H 0.3442 0.2626 0.3967 0.051 Uiso 1 1 calc R . . C19 C 0.53440(17) 0.46780(15) 0.03346(12) 0.0193(4) Uani 1 1 d . . . C20 C 0.51503(17) 0.37547(15) 0.09544(12) 0.0197(4) Uani 1 1 d . . . H20 H 0.4488 0.3443 0.1000 0.024 Uiso 1 1 calc R . . C21 C 0.60056(17) 0.32937(15) 0.15248(12) 0.0194(4) Uani 1 1 d . . . C22 C 0.68570(17) 0.39237(15) 0.13225(12) 0.0205(4) Uani 1 1 d . . . C23 C 0.79411(18) 0.38133(15) 0.16619(12) 0.0217(4) Uani 1 1 d . . . C24 C 0.81824(18) 0.34947(16) 0.24805(13) 0.0247(4) Uani 1 1 d . . . H24 H 0.7639 0.3220 0.2964 0.030 Uiso 1 1 calc R . . C25 C 0.93257(18) 0.36161(17) 0.25324(13) 0.0253(4) Uani 1 1 d . . . H25 H 0.9613 0.3437 0.3059 0.030 Uiso 1 1 calc R . . C26 C 0.99788(19) 0.40112(16) 0.17651(13) 0.0259(4) Uani 1 1 d . . . C27 C 1.11940(19) 0.42644(19) 0.15747(14) 0.0312(5) Uani 1 1 d . . . H27A H 1.1368 0.4364 0.2115 0.047 Uiso 1 1 calc R . . H27B H 1.1151 0.4996 0.1169 0.047 Uiso 1 1 calc R . . H27C H 1.1859 0.3599 0.1315 0.047 Uiso 1 1 calc R . . C28 C 0.55284(17) 0.29779(16) 0.31579(13) 0.0210(4) Uani 1 1 d . . . C29 C 0.6229(2) 0.62658(17) 0.36858(14) 0.0289(5) Uani 1 1 d . . . H29A H 0.5637 0.5905 0.4115 0.035 Uiso 1 1 calc R . . H29B H 0.6855 0.5627 0.3360 0.035 Uiso 1 1 calc R . . C30 C 0.6888(2) 0.67352(18) 0.41714(14) 0.0333(5) Uani 1 1 d . . . H30A H 0.6289 0.7087 0.4681 0.040 Uiso 1 1 calc R . . H30B H 0.7196 0.7371 0.3788 0.040 Uiso 1 1 calc R . . C31 C 0.7980(2) 0.57480(19) 0.44725(15) 0.0362(5) Uani 1 1 d . . . H31A H 0.8606 0.5444 0.3957 0.043 Uiso 1 1 calc R . . H31B H 0.8376 0.6086 0.4792 0.043 Uiso 1 1 calc R . . C32 C 0.7599(2) 0.47200(19) 0.50511(16) 0.0417(6) Uani 1 1 d . . . H32A H 0.6917 0.5025 0.5531 0.063 Uiso 1 1 calc R . . H32B H 0.8312 0.4166 0.5283 0.063 Uiso 1 1 calc R . . H32C H 0.7323 0.4304 0.4713 0.063 Uiso 1 1 calc R . . C33 C 0.6386(2) 0.77698(17) 0.23531(13) 0.0278(5) Uani 1 1 d . . . H33A H 0.5937 0.8216 0.1886 0.033 Uiso 1 1 calc R . . H33B H 0.6575 0.8353 0.2609 0.033 Uiso 1 1 calc R . . C34 C 0.7606(2) 0.69107(18) 0.19511(14) 0.0320(5) Uani 1 1 d . . . H34A H 0.7438 0.6245 0.1781 0.038 Uiso 1 1 calc R . . H34B H 0.8138 0.6575 0.2386 0.038 Uiso 1 1 calc R . . C35 C 0.8301(2) 0.75293(18) 0.11517(14) 0.0317(5) Uani 1 1 d . . . H35A H 0.8290 0.8298 0.1292 0.038 Uiso 1 1 calc R . . H35B H 0.9180 0.7029 0.1019 0.038 Uiso 1 1 calc R . . C36 C 0.7756(2) 0.77613(19) 0.03511(14) 0.0349(5) Uani 1 1 d . . . H36A H 0.7814 0.7001 0.0184 0.052 Uiso 1 1 calc R . . H36B H 0.8220 0.8186 -0.0125 0.052 Uiso 1 1 calc R . . H36C H 0.6880 0.8246 0.0478 0.052 Uiso 1 1 calc R . . C37 C 0.4537(2) 0.82063(17) 0.35187(14) 0.0285(5) Uani 1 1 d . . . H37A H 0.4957 0.8566 0.3804 0.034 Uiso 1 1 calc R . . H37B H 0.4160 0.8827 0.3078 0.034 Uiso 1 1 calc R . . C38 C 0.3498(2) 0.78671(17) 0.41947(14) 0.0303(5) Uani 1 1 d . . . H38A H 0.3840 0.7339 0.4687 0.036 Uiso 1 1 calc R . . H38B H 0.3124 0.7427 0.3939 0.036 Uiso 1 1 calc R . . C39 C 0.2498(2) 0.89834(18) 0.45216(14) 0.0311(5) Uani 1 1 d . . . H39A H 0.2896 0.9468 0.4711 0.037 Uiso 1 1 calc R . . H39B H 0.2099 0.9466 0.4039 0.037 Uiso 1 1 calc R . . C40 C 0.1504(2) 0.8690(2) 0.52722(15) 0.0379(5) Uani 1 1 d . . . H40A H 0.1101 0.8217 0.5087 0.057 Uiso 1 1 calc R . . H40B H 0.0882 0.9430 0.5455 0.057 Uiso 1 1 calc R . . H40C H 0.1890 0.8233 0.5759 0.057 Uiso 1 1 calc R . . C41 C 0.4946(2) 0.65283(17) 0.26515(14) 0.0280(5) Uani 1 1 d . . . H41A H 0.5629 0.5914 0.2336 0.034 Uiso 1 1 calc R . . H41B H 0.4458 0.6109 0.3127 0.034 Uiso 1 1 calc R . . C42 C 0.4108(2) 0.72706(17) 0.20337(14) 0.0306(5) Uani 1 1 d . . . H42A H 0.4620 0.7491 0.1470 0.037 Uiso 1 1 calc R . . H42B H 0.3556 0.8012 0.2275 0.037 Uiso 1 1 calc R . . C43 C 0.3326(2) 0.65579(17) 0.19001(14) 0.0298(5) Uani 1 1 d . . . H43A H 0.3883 0.5774 0.1731 0.036 Uiso 1 1 calc R . . H43B H 0.2755 0.6415 0.2456 0.036 Uiso 1 1 calc R . . C44 C 0.2567(2) 0.71842(19) 0.12102(15) 0.0336(5) Uani 1 1 d . . . H44A H 0.2028 0.7969 0.1367 0.050 Uiso 1 1 calc R . . H44B H 0.2055 0.6709 0.1169 0.050 Uiso 1 1 calc R . . H44C H 0.3129 0.7279 0.0649 0.050 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 S1 0.0242(3) 0.0183(2) 0.0225(3) 0.00236(18) -0.00728(18) -0.00929(19) C1 0.0252(10) 0.0172(9) 0.0217(11) -0.0013(7) -0.0081(8) -0.0102(8) B1 0.0224(11) 0.0194(10) 0.0187(12) 0.0007(8) -0.0046(8) -0.0069(9) N1 0.0269(9) 0.0266(9) 0.0251(10) -0.0038(7) -0.0037(7) -0.0094(7) S2 0.0240(3) 0.0250(2) 0.0241(3) 0.00085(19) -0.00580(19) -0.0101(2) C2 0.0247(10) 0.0182(9) 0.0235(11) -0.0028(7) -0.0067(8) -0.0109(8) N2 0.0348(10) 0.0180(8) 0.0258(10) -0.0014(7) -0.0073(7) -0.0075(7) C3 0.0230(10) 0.0211(9) 0.0287(12) -0.0047(8) -0.0044(8) -0.0083(8) C4 0.0251(10) 0.0192(9) 0.0331(12) 0.0004(8) -0.0104(8) -0.0077(8) C5 0.0321(11) 0.0207(9) 0.0249(11) 0.0041(8) -0.0104(8) -0.0120(8) C6 0.0251(10) 0.0193(9) 0.0241(11) -0.0011(7) -0.0066(8) -0.0107(8) C7 0.0257(11) 0.0218(9) 0.0256(11) -0.0031(8) -0.0021(8) -0.0070(8) C8 0.0298(12) 0.0284(11) 0.0406(14) 0.0063(9) -0.0084(10) -0.0036(9) C9 0.0300(11) 0.0250(10) 0.0217(11) 0.0039(8) -0.0051(8) -0.0095(9) C10 0.0268(10) 0.0158(8) 0.0208(10) 0.0041(7) -0.0091(8) -0.0074(8) C11 0.0286(11) 0.0167(9) 0.0242(11) 0.0046(7) -0.0104(8) -0.0081(8) C12 0.0349(12) 0.0175(9) 0.0300(12) 0.0012(8) -0.0152(9) -0.0094(8) C13 0.0311(11) 0.0202(9) 0.0367(13) 0.0068(8) -0.0173(9) -0.0119(9) C14 0.0238(11) 0.0258(10) 0.0311(12) 0.0049(8) -0.0087(8) -0.0088(8) C15 0.0243(10) 0.0241(10) 0.0239(11) 0.0032(8) -0.0085(8) -0.0072(8) C16 0.0346(12) 0.0215(9) 0.0248(11) -0.0035(8) -0.0079(9) -0.0083(9) C17 0.0336(12) 0.0301(11) 0.0507(15) 0.0014(10) -0.0175(10) -0.0156(10) C18 0.0221(11) 0.0460(13) 0.0344(13) -0.0138(10) -0.0020(9) -0.0089(10) C19 0.0201(9) 0.0170(9) 0.0218(10) -0.0038(7) -0.0038(8) -0.0064(7) C20 0.0207(10) 0.0162(8) 0.0227(10) -0.0032(7) -0.0037(7) -0.0064(7) C21 0.0207(10) 0.0153(8) 0.0215(10) -0.0035(7) -0.0029(7) -0.0049(7) C22 0.0237(10) 0.0166(9) 0.0195(10) 0.0007(7) -0.0052(7) -0.0052(8) C23 0.0241(10) 0.0168(9) 0.0238(11) -0.0006(7) -0.0042(8) -0.0074(8) C24 0.0234(10) 0.0222(9) 0.0285(12) 0.0007(8) -0.0066(8) -0.0081(8) C25 0.0270(11) 0.0251(10) 0.0253(11) 0.0001(8) -0.0109(8) -0.0077(8) C26 0.0258(11) 0.0212(9) 0.0296(12) -0.0001(8) -0.0085(8) -0.0055(8) C27 0.0287(11) 0.0355(11) 0.0328(13) 0.0026(9) -0.0106(9) -0.0148(9) C28 0.0187(10) 0.0198(9) 0.0228(11) 0.0026(8) -0.0038(7) -0.0071(8) C29 0.0379(12) 0.0192(9) 0.0280(12) 0.0010(8) -0.0095(9) -0.0072(9) C30 0.0419(13) 0.0285(11) 0.0299(12) 0.0010(9) -0.0097(10) -0.0123(10) C31 0.0389(13) 0.0353(12) 0.0333(13) -0.0050(9) -0.0087(10) -0.0085(10) C32 0.0488(15) 0.0318(12) 0.0424(15) 0.0002(10) -0.0161(11) -0.0075(11) C33 0.0382(12) 0.0205(9) 0.0263(12) -0.0003(8) -0.0084(9) -0.0111(9) C34 0.0371(12) 0.0238(10) 0.0324(13) -0.0005(9) -0.0069(9) -0.0076(9) C35 0.0346(12) 0.0242(10) 0.0368(13) -0.0037(9) -0.0055(9) -0.0111(9) C36 0.0435(13) 0.0281(11) 0.0310(13) -0.0035(9) -0.0020(10) -0.0126(10) C37 0.0368(12) 0.0185(9) 0.0286(12) -0.0041(8) -0.0071(9) -0.0055(9) C38 0.0387(12) 0.0233(10) 0.0282(12) -0.0012(8) -0.0085(9) -0.0087(9) C39 0.0363(12) 0.0259(10) 0.0303(12) -0.0037(9) -0.0107(9) -0.0057(9) C40 0.0399(13) 0.0341(12) 0.0359(14) -0.0037(10) -0.0064(10) -0.0081(10) C41 0.0365(12) 0.0191(9) 0.0302(12) -0.0053(8) -0.0068(9) -0.0097(9) C42 0.0376(12) 0.0219(10) 0.0331(13) -0.0026(8) -0.0092(9) -0.0091(9) C43 0.0317(12) 0.0242(10) 0.0322(12) -0.0083(8) -0.0021(9) -0.0076(9) C44 0.0364(12) 0.0320(11) 0.0341(13) -0.0094(9) -0.0061(10) -0.0103(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C19 1.7194(19) . ? S1 C22 1.7535(18) . ? C1 C2 1.414(3) . ? C1 C6 1.423(3) . ? C1 B1 1.679(3) . ? B1 C28 1.636(3) . ? B1 C21 1.662(3) . ? B1 C10 1.667(3) . ? N1 C28 1.154(3) . ? S2 C26 1.731(2) . ? S2 C23 1.7497(19) . ? C2 C3 1.403(3) . ? C2 C7 1.520(3) . ? N2 C37 1.523(2) . ? N2 C29 1.524(2) . ? N2 C41 1.524(3) . ? N2 C33 1.531(2) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 C8 1.513(3) . ? C5 C6 1.398(3) . ? C5 H5 0.9500 . ? C6 C9 1.510(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 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.419(3) . ? C10 C15 1.420(3) . ? C11 C12 1.400(3) . ? C11 C16 1.513(3) . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C14 1.382(3) . ? C13 C17 1.507(3) . ? C14 C15 1.396(3) . ? C14 H14 0.9500 . ? C15 C18 1.516(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 C20 1.375(2) . ? C19 C19 1.448(4) 2_665 ? C20 C21 1.429(3) . ? C20 H20 0.9500 . ? C21 C22 1.385(3) . ? C22 C23 1.461(3) . ? C23 C24 1.370(3) . ? C24 C25 1.417(3) . ? C24 H24 0.9500 . ? C25 C26 1.362(3) . ? C25 H25 0.9500 . ? C26 C27 1.495(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.519(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.526(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.515(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.518(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.534(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.516(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.530(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.521(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.516(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.526(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.519(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 S1 C22 92.18(9) . . ? C2 C1 C6 115.32(16) . . ? C2 C1 B1 128.01(16) . . ? C6 C1 B1 116.67(16) . . ? C28 B1 C21 99.54(14) . . ? C28 B1 C10 113.49(15) . . ? C21 B1 C10 109.25(15) . . ? C28 B1 C1 104.29(15) . . ? C21 B1 C1 119.15(15) . . ? C10 B1 C1 110.66(14) . . ? C26 S2 C23 92.88(9) . . ? C3 C2 C1 120.97(17) . . ? C3 C2 C7 112.96(17) . . ? C1 C2 C7 126.06(16) . . ? C37 N2 C29 111.10(15) . . ? C37 N2 C41 111.97(16) . . ? C29 N2 C41 105.37(14) . . ? C37 N2 C33 106.39(14) . . ? C29 N2 C33 111.50(16) . . ? C41 N2 C33 110.61(16) . . ? C4 C3 C2 123.08(18) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 116.56(17) . . ? C3 C4 C8 122.23(18) . . ? C5 C4 C8 121.21(18) . . ? C4 C5 C6 122.29(18) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 121.70(18) . . ? C5 C6 C9 114.60(17) . . ? C1 C6 C9 123.70(16) . . ? 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 . . ? C11 C10 C15 114.81(18) . . ? C11 C10 B1 119.04(17) . . ? C15 C10 B1 126.13(18) . . ? C12 C11 C10 121.95(18) . . ? C12 C11 C16 115.63(18) . . ? C10 C11 C16 122.35(18) . . ? C13 C12 C11 122.3(2) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 116.51(19) . . ? C12 C13 C17 122.4(2) . . ? C14 C13 C17 121.0(2) . . ? C13 C14 C15 122.96(19) . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C14 C15 C10 121.34(19) . . ? C14 C15 C18 114.91(18) . . ? C10 C15 C18 123.70(18) . . ? 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 . . ? C20 C19 C19 129.2(2) . 2_665 ? C20 C19 S1 110.03(14) . . ? C19 C19 S1 120.77(18) 2_665 . ? C19 C20 C21 115.92(18) . . ? C19 C20 H20 122.0 . . ? C21 C20 H20 122.0 . . ? C22 C21 C20 109.87(16) . . ? C22 C21 B1 129.32(17) . . ? C20 C21 B1 120.59(16) . . ? C21 C22 C23 133.37(16) . . ? C21 C22 S1 111.99(14) . . ? C23 C22 S1 114.59(13) . . ? C24 C23 C22 132.18(18) . . ? C24 C23 S2 109.60(15) . . ? C22 C23 S2 118.13(14) . . ? C23 C24 C25 113.18(18) . . ? C23 C24 H24 123.4 . . ? C25 C24 H24 123.4 . . ? C26 C25 C24 114.53(19) . . ? C26 C25 H25 122.7 . . ? C24 C25 H25 122.7 . . ? C25 C26 C27 129.54(19) . . ? C25 C26 S2 109.76(16) . . ? C27 C26 S2 120.70(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 B1 173.18(19) . . ? C30 C29 N2 114.84(16) . . ? C30 C29 H29A 108.6 . . ? N2 C29 H29A 108.6 . . ? C30 C29 H29B 108.6 . . ? N2 C29 H29B 108.6 . . ? H29A C29 H29B 107.5 . . ? C29 C30 C31 111.42(18) . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C30 113.1(2) . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N2 115.35(15) . . ? C34 C33 H33A 108.4 . . ? N2 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? N2 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 111.45(16) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 113.82(19) . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35B 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N2 115.99(16) . . ? C38 C37 H37A 108.3 . . ? N2 C37 H37A 108.3 . . ? C38 C37 H37B 108.3 . . ? N2 C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? C37 C38 C39 110.23(16) . . ? C37 C38 H38A 109.6 . . ? C39 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? C39 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 112.44(17) . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39B 109.1 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N2 116.40(15) . . ? C42 C41 H41A 108.2 . . ? N2 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? N2 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? C41 C42 C43 109.48(16) . . ? C41 C42 H42A 109.8 . . ? C43 C42 H42A 109.8 . . ? C41 C42 H42B 109.8 . . ? C43 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 112.77(17) . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 66.95 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.34 _refine_diff_density_min -0.28 _refine_diff_density_rms 0.05 # Attachment '5705_web_deposit_cif_file_1_FriederJaekle_1306950851.120309ral_lhy_132_0mCIF.cif' data_120309ral_lhy_132_0m _database_code_depnum_ccdc_archive 'CCDC 828005' #TrackingRef '5705_web_deposit_cif_file_1_FriederJaekle_1306950851.120309ral_lhy_132_0mCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _vrf_PLAT029_120309ral_lhy_132_0m ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.87 RESPONSE: Even though we collected data out to 0.81 \%A resolution with copper radiation,the crystal diffracted poorly beyond 0.88\%A resolution (with only 48% of the theoretical data collected between 0.87 and 0.84 \%A, and only 7% of the theoretical data collected between 0.84 and 0.82 \%A). Larger crystals were not obtainable, and since the crystals of this compound are no longer available, we can only rely on the current data set. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H56 B2 F2 S4, C20 H40 K O8, C12 H24 K O6, 2(C4 H8 O)' _chemical_formula_sum 'C94 H136 B2 F2 K2 O16 S4' _chemical_formula_weight 1788.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7612(1) _cell_length_b 11.4101(2) _cell_length_c 21.9383(3) _cell_angle_alpha 89.5585(9) _cell_angle_beta 88.1985(8) _cell_angle_gamma 63.2907(7) _cell_volume 2405.04(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 70.71 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 958 _exptl_absorpt_coefficient_mu 2.210 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5256 _exptl_absorpt_correction_T_max 0.7050 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; 'crystal mounted on a Cryoloop using Paratone-N' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Apex-II area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23466 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.031 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 71.03 _reflns_number_total 8064 _reflns_number_gt 6688 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX 2 (Bruker, 2006)' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008b)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+1.8667P] 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 'SHELXTL (Sheldrick, 2008b)' _refine_ls_extinction_coef 0.00018(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8064 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.113 _refine_ls_wR_factor_gt 0.106 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.00 _refine_ls_shift/su_mean 0.00 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 S1 S 0.69608(5) 0.88181(5) 0.44967(2) 0.02057(13) Uani 1 1 d . . . K1 K 0.5000 0.5000 0.5000 0.03064(18) Uani 1 2 d S . . C1B C 0.1267(3) 0.3079(3) 0.13658(11) 0.0397(7) Uani 1 1 d . . . H1B1 H 0.1684 0.3640 0.1509 0.048 Uiso 1 1 calc R . . H1B2 H 0.1673 0.2246 0.1595 0.048 Uiso 1 1 calc R . . C1D C 0.0795(4) 0.7930(3) 0.00199(19) 0.0701(11) Uani 1 1 d . . . H1D1 H 0.0116 0.8295 0.0366 0.084 Uiso 1 1 calc R . . H1D2 H 0.0303 0.8270 -0.0364 0.084 Uiso 1 1 calc R . . C1 C 0.2847(2) 1.0685(2) 0.30431(9) 0.0190(4) Uani 1 1 d . . . B1 B 0.4396(2) 0.9390(2) 0.29871(11) 0.0188(5) Uani 1 1 d . . . O1 O 0.23920(18) 0.53599(16) 0.45731(7) 0.0320(4) Uani 1 1 d . . . C1A C 0.1220(3) 0.6191(3) 0.49454(11) 0.0334(6) Uani 1 1 d . . . H1A1 H 0.1215 0.5753 0.5336 0.040 Uiso 1 1 calc R . . H1A2 H 0.0348 0.6381 0.4736 0.040 Uiso 1 1 calc R . . F1 F 0.52514(12) 0.96520(11) 0.25278(5) 0.0210(3) Uani 1 1 d . . . O1C O 0.8430(3) -0.0254(3) 0.12687(11) 0.0800(8) Uani 1 1 d . . . S2 S 0.94302(6) 0.76714(6) 0.35332(2) 0.02589(15) Uani 1 1 d . . . K2 K 0.0000 0.5000 0.0000 0.0343(2) Uani 1 2 d S . . C2B C -0.0283(3) 0.3763(2) 0.14731(11) 0.0347(6) Uani 1 1 d . . . H2B1 H -0.0711 0.3254 0.1282 0.042 Uiso 1 1 calc R . . H2B2 H -0.0509 0.3831 0.1916 0.042 Uiso 1 1 calc R . . C2D C 0.1946(4) 0.8312(4) 0.00750(18) 0.0685(10) Uani 1 1 d . . . H2D1 H 0.1860 0.8991 -0.0227 0.082 Uiso 1 1 calc R . . H2D2 H 0.1943 0.8651 0.0489 0.082 Uiso 1 1 calc R . . C2 C 0.1677(2) 1.0605(2) 0.33188(9) 0.0210(5) Uani 1 1 d . . . C2A C 0.2371(3) 0.4151(3) 0.44300(13) 0.0387(6) Uani 1 1 d . . . H2A1 H 0.1516 0.4324 0.4210 0.046 Uiso 1 1 calc R . . H2A2 H 0.2373 0.3676 0.4810 0.046 Uiso 1 1 calc R . . O2 O 0.48493(18) 0.30190(17) 0.43798(8) 0.0338(4) Uani 1 1 d . . . C3B C -0.2289(2) 0.5755(2) 0.13229(10) 0.0297(5) Uani 1 1 d . . . H3B1 H -0.2506 0.5845 0.1767 0.036 Uiso 1 1 calc R . . H3B2 H -0.2764 0.5280 0.1141 0.036 Uiso 1 1 calc R . . C3D C 0.3232(4) 0.7073(4) -0.00483(17) 0.0717(11) Uani 1 1 d . . . H3D1 H 0.3489 0.6968 -0.0489 0.086 Uiso 1 1 calc R . . H3D2 H 0.4021 0.7050 0.0181 0.086 Uiso 1 1 calc R . . C3 C 0.0392(2) 1.1718(2) 0.33893(10) 0.0232(5) Uani 1 1 d . . . H3 H -0.0372 1.1622 0.3568 0.028 Uiso 1 1 calc R . . O3 O 0.74922(18) 0.28688(17) 0.45836(7) 0.0317(4) Uani 1 1 d . . . C3A C 0.3631(3) 0.3335(3) 0.40389(12) 0.0381(6) Uani 1 1 d . . . H3A1 H 0.3598 0.2520 0.3910 0.046 Uiso 1 1 calc R . . H3A2 H 0.3652 0.3828 0.3668 0.046 Uiso 1 1 calc R . . O4 O 0.15554(18) 0.28215(17) 0.07277(7) 0.0378(4) Uani 1 1 d . . . C4B C -0.2788(3) 0.7081(2) 0.10430(11) 0.0324(6) Uani 1 1 d . . . H4B1 H -0.3765 0.7646 0.1176 0.039 Uiso 1 1 calc R . . H4B2 H -0.2209 0.7501 0.1173 0.039 Uiso 1 1 calc R . . C4D C 0.2846(4) 0.6041(4) 0.01663(19) 0.0799(13) Uani 1 1 d . . . H4D1 H 0.3426 0.5198 -0.0046 0.096 Uiso 1 1 calc R . . H4D2 H 0.2969 0.5909 0.0611 0.096 Uiso 1 1 calc R . . C4 C 0.0193(2) 1.2947(2) 0.32089(10) 0.0239(5) Uani 1 1 d . . . C4A C 0.6081(3) 0.2140(2) 0.40507(11) 0.0332(6) Uani 1 1 d . . . H4A1 H 0.6228 0.2577 0.3683 0.040 Uiso 1 1 calc R . . H4A2 H 0.5989 0.1356 0.3919 0.040 Uiso 1 1 calc R . . O5 O -0.08186(17) 0.50380(16) 0.12150(7) 0.0288(4) Uani 1 1 d . . . C5B C -0.3196(3) 0.8137(3) 0.00877(13) 0.0452(7) Uani 1 1 d . . . H5B1 H -0.2674 0.8622 0.0207 0.054 Uiso 1 1 calc R . . H5B2 H -0.4192 0.8681 0.0196 0.054 Uiso 1 1 calc R . . C5 C 0.1336(2) 1.3047(2) 0.29480(10) 0.0238(5) Uani 1 1 d . . . H5 H 0.1235 1.3884 0.2824 0.029 Uiso 1 1 calc R . . C5A C 0.7283(3) 0.1746(2) 0.44598(11) 0.0326(6) Uani 1 1 d . . . H5A1 H 0.7090 0.1393 0.4846 0.039 Uiso 1 1 calc R . . H5A2 H 0.8130 0.1053 0.4261 0.039 Uiso 1 1 calc R . . O6 O -0.26890(18) 0.69241(16) 0.03956(7) 0.0346(4) Uani 1 1 d . . . C6B C 0.3009(3) 0.2142(3) 0.05862(13) 0.0469(8) Uani 1 1 d . . . H6B1 H 0.3432 0.1311 0.0816 0.056 Uiso 1 1 calc R . . H6B2 H 0.3470 0.2686 0.0700 0.056 Uiso 1 1 calc R . . C6 C 0.2632(2) 1.1952(2) 0.28615(9) 0.0204(5) Uani 1 1 d . . . C6A C 0.8687(3) 0.2564(3) 0.49382(11) 0.0330(6) Uani 1 1 d . . . H6A1 H 0.9536 0.1932 0.4715 0.040 Uiso 1 1 calc R . . H6A2 H 0.8600 0.2165 0.5329 0.040 Uiso 1 1 calc R . . O7 O 0.1422(3) 0.6512(2) 0.00234(13) 0.0736(7) Uani 1 1 d . . . C7 C 0.1753(2) 0.9335(2) 0.35613(11) 0.0278(5) Uani 1 1 d . . . H7A H 0.0875 0.9506 0.3777 0.042 Uiso 1 1 calc R . . H7B H 0.2520 0.8946 0.3843 0.042 Uiso 1 1 calc R . . H7C H 0.1913 0.8726 0.3221 0.042 Uiso 1 1 calc R . . C8 C -0.1202(2) 1.4140(2) 0.32939(11) 0.0319(6) Uani 1 1 d . . . H8A H -0.1663 1.4375 0.2902 0.048 Uiso 1 1 calc R . . H8B H -0.1061 1.4876 0.3446 0.048 Uiso 1 1 calc R . . H8C H -0.1784 1.3943 0.3588 0.048 Uiso 1 1 calc R . . C9 C 0.3773(2) 1.2230(2) 0.25704(11) 0.0276(5) Uani 1 1 d . . . H9A H 0.4609 1.1825 0.2813 0.041 Uiso 1 1 calc R . . H9B H 0.3455 1.3181 0.2554 0.041 Uiso 1 1 calc R . . H9C H 0.3988 1.1865 0.2156 0.041 Uiso 1 1 calc R . . C10 C 0.4402(2) 0.8020(2) 0.27192(9) 0.0192(4) Uani 1 1 d . . . C11 C 0.4022(2) 0.8044(2) 0.21029(10) 0.0220(5) Uani 1 1 d . . . C12 C 0.4229(2) 0.6899(2) 0.17973(10) 0.0260(5) Uani 1 1 d . . . H12 H 0.3961 0.6957 0.1385 0.031 Uiso 1 1 calc R . . C13 C 0.4811(2) 0.5681(2) 0.20732(11) 0.0266(5) Uani 1 1 d . . . C14 C 0.5120(2) 0.5651(2) 0.26804(11) 0.0242(5) Uani 1 1 d . . . H14 H 0.5489 0.4835 0.2887 0.029 Uiso 1 1 calc R . . C15 C 0.4910(2) 0.6784(2) 0.30043(10) 0.0210(5) Uani 1 1 d . . . C16 C 0.3369(2) 0.9306(2) 0.17444(10) 0.0276(5) Uani 1 1 d . . . H16A H 0.3153 0.9120 0.1336 0.041 Uiso 1 1 calc R . . H16B H 0.4021 0.9689 0.1708 0.041 Uiso 1 1 calc R . . H16C H 0.2510 0.9926 0.1956 0.041 Uiso 1 1 calc R . . C17 C 0.5073(3) 0.4444(3) 0.17287(12) 0.0393(6) Uani 1 1 d . . . H17A H 0.5511 0.3686 0.1997 0.059 Uiso 1 1 calc R . . H17B H 0.5691 0.4340 0.1374 0.059 Uiso 1 1 calc R . . H17C H 0.4187 0.4506 0.1592 0.059 Uiso 1 1 calc R . . C18 C 0.5266(3) 0.6570(2) 0.36727(11) 0.0282(5) Uani 1 1 d . . . H18A H 0.6152 0.6595 0.3732 0.042 Uiso 1 1 d . . . H18B H 0.5347 0.5713 0.3799 0.042 Uiso 1 1 d . . . H18C H 0.4530 0.7262 0.3919 0.042 Uiso 1 1 d . . . C19 C 0.5215(2) 0.9736(2) 0.46945(10) 0.0205(4) Uani 1 1 d . . . C20 C 0.4430(2) 0.9862(2) 0.41968(9) 0.0196(4) Uani 1 1 d . . . H20 H 0.3443 1.0324 0.4220 0.023 Uiso 1 1 calc R . . C21 C 0.5165(2) 0.9267(2) 0.36417(10) 0.0191(4) Uani 1 1 d . . . C22 C 0.6584(2) 0.8680(2) 0.37366(9) 0.0193(4) Uani 1 1 d . . . C23 C 0.7770(2) 0.7956(2) 0.33228(10) 0.0199(4) Uani 1 1 d . . . C24 C 0.7847(2) 0.7425(2) 0.27581(10) 0.0221(5) Uani 1 1 d . . . H24 H 0.7058 0.7469 0.2557 0.027 Uiso 1 1 calc R . . C25 C 0.9218(2) 0.6801(2) 0.25006(10) 0.0247(5) Uani 1 1 d . . . H25 H 0.9430 0.6388 0.2111 0.030 Uiso 1 1 calc R . . C26 C 1.0202(2) 0.6845(2) 0.28613(10) 0.0243(5) Uani 1 1 d . . . C27 C 1.1730(2) 0.6326(2) 0.27366(12) 0.0320(6) Uani 1 1 d . . . H27A H 1.2012 0.5716 0.2390 0.048 Uiso 1 1 calc R . . H27B H 1.2234 0.5866 0.3097 0.048 Uiso 1 1 calc R . . H27C H 1.1947 0.7056 0.2641 0.048 Uiso 1 1 calc R . . C1C C 0.7261(3) 0.0413(3) 0.16701(15) 0.0535(8) Uani 1 1 d . B . H1C1 H 0.6753 -0.0118 0.1737 0.064 Uiso 1 1 calc R A 1 H1C2 H 0.6617 0.1266 0.1495 0.064 Uiso 1 1 calc R A 1 C2C C 0.7815(15) 0.0630(11) 0.2277(5) 0.046(3) Uani 0.500(18) 1 d P B 1 H2C1 H 0.7146 0.1449 0.2485 0.055 Uiso 0.500(18) 1 calc PR B 1 H2C2 H 0.8049 -0.0121 0.2557 0.055 Uiso 0.500(18) 1 calc PR B 1 C3C C 0.9083(9) 0.0724(13) 0.2045(4) 0.055(3) Uiso 0.500(18) 1 d P B 1 H3C1 H 0.9757 0.0565 0.2370 0.066 Uiso 0.500(18) 1 calc PR B 1 H3C2 H 0.8851 0.1583 0.1853 0.066 Uiso 0.500(18) 1 calc PR B 1 C4C C 0.9642(12) -0.0443(11) 0.1554(4) 0.037(2) Uani 0.500(18) 1 d P B 1 H4C1 H 1.0321 -0.0369 0.1260 0.044 Uiso 0.500(18) 1 calc PR B 1 H4C2 H 1.0081 -0.1310 0.1754 0.044 Uiso 0.500(18) 1 calc PR B 1 C2CA C 0.7771(14) 0.086(2) 0.2206(8) 0.104(7) Uani 0.500(18) 1 d P B 2 H2C3 H 0.7411 0.0657 0.2592 0.125 Uiso 0.500(18) 1 calc PR B 2 H2C4 H 0.7458 0.1820 0.2188 0.125 Uiso 0.500(18) 1 calc PR B 2 C3CA C 0.9343(8) 0.0129(12) 0.2167(4) 0.053(2) Uiso 0.500(18) 1 d P B 2 H3C3 H 0.9768 0.0694 0.2295 0.063 Uiso 0.500(18) 1 calc PR B 2 H3C4 H 0.9693 -0.0666 0.2424 0.063 Uiso 0.500(18) 1 calc PR B 2 C4CA C 0.962(2) -0.020(3) 0.1550(9) 0.140(9) Uani 0.500(18) 1 d P B 2 H4C3 H 1.0447 -0.1059 0.1504 0.168 Uiso 0.500(18) 1 calc PR B 2 H4C4 H 0.9829 0.0466 0.1338 0.168 Uiso 0.500(18) 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 S1 0.0180(3) 0.0225(3) 0.0176(3) -0.0016(2) -0.00141(19) -0.0058(2) K1 0.0380(4) 0.0361(4) 0.0241(3) -0.0015(3) -0.0027(3) -0.0221(3) C1B 0.0437(16) 0.0397(16) 0.0234(12) 0.0066(11) -0.0006(11) -0.0081(12) C1D 0.069(2) 0.051(2) 0.079(3) -0.0213(19) -0.010(2) -0.0162(18) C1 0.0199(11) 0.0221(11) 0.0139(9) -0.0014(8) -0.0019(8) -0.0083(9) B1 0.0191(12) 0.0189(12) 0.0173(11) 0.0005(10) 0.0001(9) -0.0075(10) O1 0.0398(10) 0.0311(9) 0.0321(9) 0.0024(7) -0.0044(7) -0.0221(8) C1A 0.0373(14) 0.0449(16) 0.0253(12) 0.0055(11) -0.0058(10) -0.0248(12) F1 0.0201(6) 0.0215(6) 0.0195(6) 0.0002(5) 0.0016(5) -0.0078(5) O1C 0.0567(15) 0.140(3) 0.0461(13) -0.0223(15) 0.0115(11) -0.0473(16) S2 0.0184(3) 0.0323(3) 0.0252(3) -0.0046(2) 0.0002(2) -0.0098(2) K2 0.0347(4) 0.0322(4) 0.0219(3) 0.0035(3) 0.0047(3) -0.0029(3) C2B 0.0452(16) 0.0325(14) 0.0217(12) 0.0056(10) 0.0019(11) -0.0135(12) C2D 0.077(3) 0.064(2) 0.059(2) -0.0082(18) -0.0008(19) -0.028(2) C2 0.0224(11) 0.0221(11) 0.0177(10) -0.0017(9) -0.0015(8) -0.0091(9) C2A 0.0427(16) 0.0328(14) 0.0488(16) 0.0069(13) -0.0167(13) -0.0234(12) O2 0.0402(10) 0.0330(10) 0.0318(9) 0.0009(8) -0.0102(8) -0.0191(8) C3B 0.0304(13) 0.0372(14) 0.0213(11) -0.0038(10) 0.0046(9) -0.0153(11) C3D 0.078(3) 0.076(3) 0.052(2) -0.0222(19) 0.0037(18) -0.027(2) C3 0.0205(11) 0.0290(13) 0.0194(10) -0.0005(9) 0.0011(9) -0.0107(9) O3 0.0393(10) 0.0347(10) 0.0287(9) 0.0034(7) -0.0059(7) -0.0232(8) C3A 0.0470(16) 0.0311(14) 0.0408(15) 0.0017(12) -0.0183(12) -0.0206(12) O4 0.0371(10) 0.0368(10) 0.0251(9) 0.0050(8) 0.0016(7) -0.0041(8) C4B 0.0307(13) 0.0330(14) 0.0276(12) -0.0043(11) 0.0077(10) -0.0096(11) C4D 0.090(3) 0.056(2) 0.083(3) -0.005(2) -0.050(2) -0.020(2) C4 0.0212(12) 0.0257(12) 0.0181(10) 0.0000(9) -0.0014(9) -0.0044(9) C4A 0.0468(16) 0.0288(13) 0.0289(12) 0.0014(11) -0.0039(11) -0.0212(12) O5 0.0308(9) 0.0288(9) 0.0227(8) 0.0009(7) 0.0034(7) -0.0100(7) C5B 0.0414(16) 0.0314(15) 0.0418(15) 0.0072(12) 0.0088(12) 0.0016(12) C5 0.0251(12) 0.0202(11) 0.0221(11) 0.0023(9) -0.0005(9) -0.0066(9) C5A 0.0430(15) 0.0311(14) 0.0290(12) 0.0004(11) 0.0010(11) -0.0215(12) O6 0.0378(10) 0.0278(9) 0.0272(9) 0.0013(7) 0.0046(7) -0.0052(7) C6B 0.0372(16) 0.0412(17) 0.0391(15) 0.0152(13) 0.0017(12) 0.0025(12) C6 0.0215(11) 0.0218(11) 0.0160(10) 0.0003(9) -0.0007(8) -0.0080(9) C6A 0.0359(14) 0.0377(15) 0.0273(12) 0.0026(11) -0.0031(10) -0.0180(11) O7 0.0738(17) 0.0558(15) 0.0871(18) -0.0055(13) -0.0257(14) -0.0239(13) C7 0.0234(12) 0.0261(12) 0.0324(12) -0.0014(10) 0.0066(10) -0.0103(10) C8 0.0238(12) 0.0296(13) 0.0309(13) 0.0059(11) 0.0035(10) -0.0023(10) C9 0.0258(12) 0.0205(12) 0.0341(13) 0.0020(10) 0.0032(10) -0.0087(10) C10 0.0146(10) 0.0214(11) 0.0188(10) -0.0018(9) 0.0022(8) -0.0057(8) C11 0.0194(11) 0.0240(12) 0.0222(11) -0.0024(9) 0.0023(9) -0.0095(9) C12 0.0280(12) 0.0338(13) 0.0188(11) -0.0042(10) 0.0030(9) -0.0164(10) C13 0.0253(12) 0.0246(12) 0.0307(12) -0.0097(10) 0.0109(10) -0.0126(10) C14 0.0192(11) 0.0193(11) 0.0321(12) 0.0004(10) 0.0048(9) -0.0072(9) C15 0.0155(10) 0.0220(11) 0.0242(11) -0.0004(9) 0.0013(8) -0.0074(9) C16 0.0326(13) 0.0292(13) 0.0187(11) 0.0007(10) -0.0048(9) -0.0115(10) C17 0.0540(17) 0.0321(15) 0.0362(14) -0.0116(12) 0.0135(12) -0.0240(13) C18 0.0349(13) 0.0231(12) 0.0267(12) 0.0051(10) -0.0053(10) -0.0130(10) C19 0.0207(11) 0.0188(11) 0.0211(11) -0.0011(9) 0.0005(8) -0.0080(9) C20 0.0185(11) 0.0175(11) 0.0217(10) 0.0003(9) -0.0006(8) -0.0073(8) C21 0.0197(11) 0.0169(11) 0.0210(10) 0.0002(9) 0.0003(8) -0.0085(9) C22 0.0222(11) 0.0171(11) 0.0181(10) -0.0004(9) -0.0021(8) -0.0083(9) C23 0.0182(11) 0.0178(11) 0.0232(11) 0.0022(9) -0.0021(8) -0.0077(8) C24 0.0200(11) 0.0208(11) 0.0229(11) -0.0018(9) -0.0006(9) -0.0067(9) C25 0.0255(12) 0.0210(11) 0.0233(11) -0.0017(9) 0.0028(9) -0.0068(9) C26 0.0245(12) 0.0187(11) 0.0287(12) -0.0004(9) 0.0039(9) -0.0091(9) C27 0.0237(13) 0.0305(13) 0.0397(14) -0.0049(11) 0.0063(10) -0.0109(10) C1C 0.0460(18) 0.057(2) 0.0522(18) -0.0073(15) 0.0109(15) -0.0194(15) C2C 0.083(8) 0.033(4) 0.029(4) -0.003(3) 0.021(4) -0.034(5) C4C 0.022(4) 0.059(5) 0.022(4) -0.006(3) 0.002(3) -0.012(3) C2CA 0.030(7) 0.139(13) 0.098(11) -0.034(9) -0.012(6) 0.004(7) C4CA 0.086(12) 0.27(3) 0.103(13) -0.053(14) 0.028(9) -0.119(15) _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 S1 C19 1.732(2) . ? S1 C22 1.753(2) . ? K1 O2 2.7161(17) . ? K1 O2 2.7161(17) 2_666 ? K1 O3 2.8211(17) . ? K1 O3 2.8211(17) 2_666 ? K1 O1 2.8365(17) . ? K1 O1 2.8365(17) 2_666 ? K1 C18 3.478(2) 2_666 ? K1 H18B 2.8141 . ? C1B O4 1.428(3) . ? C1B C2B 1.501(4) . ? C1B H1B1 0.9900 . ? C1B H1B2 0.9900 . ? C1D O7 1.446(4) . ? C1D C2D 1.495(5) . ? C1D H1D1 0.9900 . ? C1D H1D2 0.9900 . ? C1 C6 1.414(3) . ? C1 C2 1.419(3) . ? C1 B1 1.659(3) . ? B1 F1 1.462(3) . ? B1 C21 1.653(3) . ? B1 C10 1.672(3) . ? O1 C1A 1.424(3) . ? O1 C2A 1.427(3) . ? C1A C6A 1.493(4) 2_666 ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? O1C C4C 1.391(12) . ? O1C C1C 1.421(4) . ? O1C C4CA 1.47(2) . ? S2 C26 1.730(2) . ? S2 C23 1.743(2) . ? K2 O7 2.775(3) 2_565 ? K2 O7 2.775(3) . ? K2 O5 2.7755(15) . ? K2 O5 2.7755(15) 2_565 ? K2 O4 2.8099(16) 2_565 ? K2 O4 2.8099(16) . ? K2 O6 2.8473(16) . ? K2 O6 2.8473(16) 2_565 ? C2B O5 1.422(3) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C2D C3D 1.487(5) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C2 C3 1.400(3) . ? C2 C7 1.509(3) . ? C2A C3A 1.499(4) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? O2 C4A 1.428(3) . ? O2 C3A 1.428(3) . ? C3B O5 1.430(3) . ? C3B C4B 1.493(4) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? C3D C4D 1.483(6) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? O3 C5A 1.426(3) . ? O3 C6A 1.427(3) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? O4 C6B 1.424(3) . ? C4B O6 1.428(3) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C4D O7 1.423(4) . ? C4D H4D1 0.9900 . ? C4D H4D2 0.9900 . ? C4 C5 1.391(3) . ? C4 C8 1.513(3) . ? C4A C5A 1.492(4) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5B O6 1.414(3) . ? C5B C6B 1.503(4) 2_565 ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C5 C6 1.401(3) . ? C5 H5 0.9500 . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6B C5B 1.503(4) 2_565 ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C6 C9 1.521(3) . ? C6A C1A 1.493(4) 2_666 ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? 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 1.411(3) . ? C10 C11 1.421(3) . ? C11 C12 1.396(3) . ? C11 C16 1.515(3) . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 C17 1.512(3) . ? C14 C15 1.403(3) . ? C14 H14 0.9500 . ? C15 C18 1.517(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 0.9805 . ? C18 H18B 0.9800 . ? C18 H18C 0.9802 . ? C19 C20 1.368(3) . ? C19 C19 1.448(4) 2_676 ? C20 C21 1.428(3) . ? C20 H20 0.9500 . ? C21 C22 1.386(3) . ? C22 C23 1.458(3) . ? C23 C24 1.367(3) . ? C24 C25 1.419(3) . ? C24 H24 0.9500 . ? C25 C26 1.360(3) . ? C25 H25 0.9500 . ? C26 C27 1.493(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C1C C2CA 1.498(17) . ? C1C C2C 1.542(13) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? C2C C3C 1.491(14) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C C4C 1.600(14) . ? C3C H3C1 0.9900 . ? C3C H3C2 0.9900 . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C2CA C3CA 1.513(16) . ? C2CA H2C3 0.9900 . ? C2CA H2C4 0.9900 . ? C3CA C4CA 1.39(2) . ? C3CA H3C3 0.9900 . ? C3CA H3C4 0.9900 . ? C4CA H4C3 0.9900 . ? C4CA H4C4 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 C19 S1 C22 92.00(10) . . ? O2 K1 O2 180.00(6) . 2_666 ? O2 K1 O3 61.23(5) . . ? O2 K1 O3 118.77(5) 2_666 . ? O2 K1 O3 118.78(5) . 2_666 ? O2 K1 O3 61.22(5) 2_666 2_666 ? O3 K1 O3 180.0 . 2_666 ? O2 K1 O1 60.79(5) . . ? O2 K1 O1 119.21(5) 2_666 . ? O3 K1 O1 120.75(5) . . ? O3 K1 O1 59.25(5) 2_666 . ? O2 K1 O1 119.21(5) . 2_666 ? O2 K1 O1 60.79(5) 2_666 2_666 ? O3 K1 O1 59.25(5) . 2_666 ? O3 K1 O1 120.75(5) 2_666 2_666 ? O1 K1 O1 180.0 . 2_666 ? O2 K1 C18 86.85(5) . 2_666 ? O2 K1 C18 93.15(5) 2_666 2_666 ? O3 K1 C18 94.13(5) . 2_666 ? O3 K1 C18 85.87(5) 2_666 2_666 ? O1 K1 C18 93.95(5) . 2_666 ? O1 K1 C18 86.05(5) 2_666 2_666 ? O2 K1 H18B 80.4 . . ? O2 K1 H18B 99.6 2_666 . ? O3 K1 H18B 76.8 . . ? O3 K1 H18B 103.2 2_666 . ? O1 K1 H18B 82.8 . . ? O1 K1 H18B 97.2 2_666 . ? C18 K1 H18B 166.8 2_666 . ? O4 C1B C2B 108.5(2) . . ? O4 C1B H1B1 110.0 . . ? C2B C1B H1B1 110.0 . . ? O4 C1B H1B2 110.0 . . ? C2B C1B H1B2 110.0 . . ? H1B1 C1B H1B2 108.4 . . ? O7 C1D C2D 107.1(3) . . ? O7 C1D H1D1 110.3 . . ? C2D C1D H1D1 110.3 . . ? O7 C1D H1D2 110.3 . . ? C2D C1D H1D2 110.3 . . ? H1D1 C1D H1D2 108.5 . . ? C6 C1 C2 115.72(19) . . ? C6 C1 B1 122.28(19) . . ? C2 C1 B1 121.84(19) . . ? F1 B1 C21 105.72(17) . . ? F1 B1 C1 108.87(17) . . ? C21 B1 C1 107.22(17) . . ? F1 B1 C10 102.33(16) . . ? C21 B1 C10 116.49(17) . . ? C1 B1 C10 115.48(17) . . ? C1A O1 C2A 112.00(19) . . ? C1A O1 K1 114.85(13) . . ? C2A O1 K1 112.74(14) . . ? O1 C1A C6A 108.3(2) . 2_666 ? O1 C1A H1A1 110.0 . . ? C6A C1A H1A1 110.0 2_666 . ? O1 C1A H1A2 110.0 . . ? C6A C1A H1A2 110.0 2_666 . ? H1A1 C1A H1A2 108.4 . . ? C4C O1C C1C 109.9(5) . . ? C4C O1C C4CA 10.5(13) . . ? C1C O1C C4CA 106.8(9) . . ? C26 S2 C23 93.05(11) . . ? O7 K2 O7 180.0 2_565 . ? O7 K2 O5 77.80(7) 2_565 . ? O7 K2 O5 102.20(7) . . ? O7 K2 O5 102.20(7) 2_565 2_565 ? O7 K2 O5 77.80(7) . 2_565 ? O5 K2 O5 180.0 . 2_565 ? O7 K2 O4 104.55(6) 2_565 2_565 ? O7 K2 O4 75.45(6) . 2_565 ? O5 K2 O4 118.62(5) . 2_565 ? O5 K2 O4 61.38(5) 2_565 2_565 ? O7 K2 O4 75.45(6) 2_565 . ? O7 K2 O4 104.54(6) . . ? O5 K2 O4 61.38(5) . . ? O5 K2 O4 118.62(5) 2_565 . ? O4 K2 O4 180.0 2_565 . ? O7 K2 O6 80.68(7) 2_565 . ? O7 K2 O6 99.32(7) . . ? O5 K2 O6 61.17(5) . . ? O5 K2 O6 118.83(5) 2_565 . ? O4 K2 O6 59.00(5) 2_565 . ? O4 K2 O6 121.00(5) . . ? O7 K2 O6 99.32(7) 2_565 2_565 ? O7 K2 O6 80.68(7) . 2_565 ? O5 K2 O6 118.83(5) . 2_565 ? O5 K2 O6 61.17(5) 2_565 2_565 ? O4 K2 O6 120.99(5) 2_565 2_565 ? O4 K2 O6 59.01(5) . 2_565 ? O6 K2 O6 180.0 . 2_565 ? O5 C2B C1B 109.0(2) . . ? O5 C2B H2B1 109.9 . . ? C1B C2B H2B1 109.9 . . ? O5 C2B H2B2 109.9 . . ? C1B C2B H2B2 109.9 . . ? H2B1 C2B H2B2 108.3 . . ? C3D C2D C1D 104.1(3) . . ? C3D C2D H2D1 110.9 . . ? C1D C2D H2D1 110.9 . . ? C3D C2D H2D2 110.9 . . ? C1D C2D H2D2 110.9 . . ? H2D1 C2D H2D2 108.9 . . ? C3 C2 C1 121.2(2) . . ? C3 C2 C7 116.6(2) . . ? C1 C2 C7 122.18(19) . . ? O1 C2A C3A 108.8(2) . . ? O1 C2A H2A1 109.9 . . ? C3A C2A H2A1 109.9 . . ? O1 C2A H2A2 109.9 . . ? C3A C2A H2A2 109.9 . . ? H2A1 C2A H2A2 108.3 . . ? C4A O2 C3A 111.60(19) . . ? C4A O2 K1 116.50(14) . . ? C3A O2 K1 117.46(14) . . ? O5 C3B C4B 108.99(19) . . ? O5 C3B H3B1 109.9 . . ? C4B C3B H3B1 109.9 . . ? O5 C3B H3B2 109.9 . . ? C4B C3B H3B2 109.9 . . ? H3B1 C3B H3B2 108.3 . . ? C4D C3D C2D 103.5(3) . . ? C4D C3D H3D1 111.1 . . ? C2D C3D H3D1 111.1 . . ? C4D C3D H3D2 111.1 . . ? C2D C3D H3D2 111.1 . . ? H3D1 C3D H3D2 109.0 . . ? C4 C3 C2 122.5(2) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C5A O3 C6A 112.69(19) . . ? C5A O3 K1 111.24(14) . . ? C6A O3 K1 116.15(14) . . ? O2 C3A C2A 109.0(2) . . ? O2 C3A H3A1 109.9 . . ? C2A C3A H3A1 109.9 . . ? O2 C3A H3A2 109.9 . . ? C2A C3A H3A2 109.9 . . ? H3A1 C3A H3A2 108.3 . . ? C6B O4 C1B 112.3(2) . . ? C6B O4 K2 116.39(14) . . ? C1B O4 K2 113.29(14) . . ? O6 C4B C3B 108.22(19) . . ? O6 C4B H4B1 110.1 . . ? C3B C4B H4B1 110.1 . . ? O6 C4B H4B2 110.1 . . ? C3B C4B H4B2 110.1 . . ? H4B1 C4B H4B2 108.4 . . ? O7 C4D C3D 105.2(3) . . ? O7 C4D H4D1 110.7 . . ? C3D C4D H4D1 110.7 . . ? O7 C4D H4D2 110.7 . . ? C3D C4D H4D2 110.7 . . ? H4D1 C4D H4D2 108.8 . . ? C3 C4 C5 117.0(2) . . ? C3 C4 C8 121.7(2) . . ? C5 C4 C8 121.3(2) . . ? O2 C4A C5A 108.3(2) . . ? O2 C4A H4A1 110.0 . . ? C5A C4A H4A1 110.0 . . ? O2 C4A H4A2 110.0 . . ? C5A C4A H4A2 110.0 . . ? H4A1 C4A H4A2 108.4 . . ? C2B O5 C3B 111.49(18) . . ? C2B O5 K2 112.78(13) . . ? C3B O5 K2 113.51(12) . . ? O6 C5B C6B 108.0(2) . 2_565 ? O6 C5B H5B1 110.1 . . ? C6B C5B H5B1 110.1 2_565 . ? O6 C5B H5B2 110.1 . . ? C6B C5B H5B2 110.1 2_565 . ? H5B1 C5B H5B2 108.4 . . ? C4 C5 C6 122.1(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? O3 C5A C4A 108.8(2) . . ? O3 C5A H5A1 109.9 . . ? C4A C5A H5A1 109.9 . . ? O3 C5A H5A2 109.9 . . ? C4A C5A H5A2 109.9 . . ? H5A1 C5A H5A2 108.3 . . ? C5B O6 C4B 112.48(19) . . ? C5B O6 K2 115.55(14) . . ? C4B O6 K2 111.48(13) . . ? O4 C6B C5B 108.0(2) . 2_565 ? O4 C6B H6B1 110.1 . . ? C5B C6B H6B1 110.1 2_565 . ? O4 C6B H6B2 110.1 . . ? C5B C6B H6B2 110.1 2_565 . ? H6B1 C6B H6B2 108.4 . . ? C5 C6 C1 121.4(2) . . ? C5 C6 C9 115.4(2) . . ? C1 C6 C9 123.13(19) . . ? O3 C6A C1A 108.1(2) . 2_666 ? O3 C6A H6A1 110.1 . . ? C1A C6A H6A1 110.1 2_666 . ? O3 C6A H6A2 110.1 . . ? C1A C6A H6A2 110.1 2_666 . ? H6A1 C6A H6A2 108.4 . . ? C4D O7 C1D 107.9(3) . . ? C4D O7 K2 125.2(2) . . ? C1D O7 K2 125.8(2) . . ? 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 . . ? C15 C10 C11 115.35(19) . . ? C15 C10 B1 127.61(18) . . ? C11 C10 B1 116.48(18) . . ? C12 C11 C10 121.4(2) . . ? C12 C11 C16 116.5(2) . . ? C10 C11 C16 122.0(2) . . ? C13 C12 C11 122.4(2) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C14 C13 C12 116.8(2) . . ? C14 C13 C17 121.6(2) . . ? C12 C13 C17 121.6(2) . . ? C13 C14 C15 122.4(2) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C14 C15 C10 121.5(2) . . ? C14 C15 C18 114.9(2) . . ? C10 C15 C18 123.60(19) . . ? 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 109.6 . . ? H18A C18 H18B 109.4 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.4 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C19 129.7(3) . 2_676 ? C20 C19 S1 109.45(16) . . ? C19 C19 S1 120.8(2) 2_676 . ? C19 C20 C21 116.84(19) . . ? C19 C20 H20 121.6 . . ? C21 C20 H20 121.6 . . ? C22 C21 C20 109.38(19) . . ? C22 C21 B1 126.94(19) . . ? C20 C21 B1 123.52(18) . . ? C21 C22 C23 131.14(19) . . ? C21 C22 S1 112.26(16) . . ? C23 C22 S1 116.57(15) . . ? C24 C23 C22 131.2(2) . . ? C24 C23 S2 109.43(16) . . ? C22 C23 S2 119.37(16) . . ? C23 C24 C25 113.6(2) . . ? C23 C24 H24 123.2 . . ? C25 C24 H24 123.2 . . ? C26 C25 C24 114.1(2) . . ? C26 C25 H25 123.0 . . ? C24 C25 H25 123.0 . . ? C25 C26 C27 129.0(2) . . ? C25 C26 S2 109.87(17) . . ? C27 C26 S2 121.11(18) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1C C1C C2CA 106.7(6) . . ? O1C C1C C2C 107.2(5) . . ? C2CA C1C C2C 10.9(10) . . ? O1C C1C H1C1 110.3 . . ? C2CA C1C H1C1 119.7 . . ? C2C C1C H1C1 110.3 . . ? O1C C1C H1C2 110.3 . . ? C2CA C1C H1C2 100.9 . . ? C2C C1C H1C2 110.3 . . ? H1C1 C1C H1C2 108.5 . . ? C3C C2C C1C 99.7(7) . . ? C3C C2C H2C1 111.8 . . ? C1C C2C H2C1 111.8 . . ? C3C C2C H2C2 111.8 . . ? C1C C2C H2C2 111.8 . . ? H2C1 C2C H2C2 109.6 . . ? C2C C3C C4C 99.4(9) . . ? C2C C3C H3C1 111.9 . . ? C4C C3C H3C1 111.9 . . ? C2C C3C H3C2 111.9 . . ? C4C C3C H3C2 111.9 . . ? H3C1 C3C H3C2 109.6 . . ? O1C C4C C3C 102.4(7) . . ? O1C C4C H4C1 111.3 . . ? C3C C4C H4C1 111.3 . . ? O1C C4C H4C2 111.3 . . ? C3C C4C H4C2 111.3 . . ? H4C1 C4C H4C2 109.2 . . ? C1C C2CA C3CA 106.4(11) . . ? C1C C2CA H2C3 110.5 . . ? C3CA C2CA H2C3 110.5 . . ? C1C C2CA H2C4 110.5 . . ? C3CA C2CA H2C4 110.5 . . ? H2C3 C2CA H2C4 108.6 . . ? C4CA C3CA C2CA 102.8(13) . . ? C4CA C3CA H3C3 111.2 . . ? C2CA C3CA H3C3 111.2 . . ? C4CA C3CA H3C4 111.2 . . ? C2CA C3CA H3C4 111.2 . . ? H3C3 C3CA H3C4 109.1 . . ? C3CA C4CA O1C 111.1(14) . . ? C3CA C4CA H4C3 109.4 . . ? O1C C4CA H4C3 109.4 . . ? C3CA C4CA H4C4 109.4 . . ? O1C C4CA H4C4 109.4 . . ? H4C3 C4CA H4C4 108.0 . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 71.03 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.69 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.05