# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_k383 _database_code_CSD 183401 _journal_coden_Cambridge 207 loop_ _publ_author_name _publ_author_address 'Kolbe, Adelheid' ; Institut fur Pflanzenbiochemie Weinberg 3 D-06120 Halle (Saale) Germany ; 'Fuchs, Petra' ; Institut fur Pflanzenbiochemie Weinberg 3 D-06120 Halle (Saale) Germany ; 'Porzel, Andrea' ; Institut fur Pflanzenbiochemie Weinberg 3 D-06120 Halle (Saale) Germany ; 'Baumeister, Ute' ; Institut fur Physikalische Chemie Universitat Halle M\"uhlpforte 1 D-06108 Halle (Saale) Germany ; 'Kolbe, Alfred' ; Institut fur Physikalische Chemie Universitat Halle Muhlpforte 1 D-06108 Halle (Saale) Germany ; 'Adam, Gunter' ; Institut fur Pflanzenbiochemie Weinberg 3 D-06120 Halle (Saale) Germany ; _publ_contact_author_name 'Prof. Dr. Alfred Kolbe' _publ_contact_author_address ; Institut fur Physikalische Chemie Universitat Halle Muhlpforte 1 D-06108 Halle (Saale) Germany ; _publ_contact_author_phone '0345 55 25730' _publ_contact_author_fax '0345 55 27028' _publ_contact_author_email 'kolbe@chemie.uni-halle.de' _journal_name_full 'J. Chem. Soc., Perkin Trans. 1' _publ_section_title ; Synthesis and crystal structure of [26,27-2 H6] 24-epicathasterone ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; [26,27-^2^H~6~] (22S,24S)-3\b,22-dihydroxy-5\a-ergostan-6-one ; _chemical_name_common '[26,27 ^2^H~6~] 24-epicathasteron' _chemical_formula_moiety 'C28 H42 D6 O3, H2 O' _chemical_formula_sum 'C28 H44 D6 O4' _chemical_formula_weight 456.72 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' 'D' 'D' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.4742(10) _cell_length_b 14.290(3) _cell_length_c 14.776(3) _cell_angle_alpha 62.376(11) _cell_angle_beta 77.377(19) _cell_angle_gamma 79.801(12) _cell_volume 1359.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 16.05 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_measurement_device 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 1.02 - 1.17, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_collimation '0.5 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 8.2 _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 10882 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_av_sigmaI/netI 0.2657 _diffrn_reflns_av_R_equivalents 0.1791 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_number_total 5359 _reflns_number_gt 1912 _reflns_threshold_expression >2sigma(I) _reflns_limit_h_min -8 _reflns_limit_h_max 9 _reflns_limit_k_min -15 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP/PC' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0138(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -5(3) _refine_ls_number_reflns 5359 _refine_ls_number_parameters 586 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2502 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.6222(12) 0.7589(7) 0.5545(8) 0.063(3) Uani 1 d . . . H1A1 H 0.5606 0.7579 0.6199 0.076 Uiso 1 calc R . . H1A2 H 0.5434 0.7294 0.5319 0.076 Uiso 1 calc R . . C2A C 0.6482(13) 0.8753(7) 0.4736(8) 0.062(3) Uani 1 d . . . H2A1 H 0.6978 0.8776 0.4063 0.074 Uiso 1 calc R . . H2A2 H 0.5297 0.9166 0.4688 0.074 Uiso 1 calc R . . C3A C 0.7755(12) 0.9231(7) 0.5026(7) 0.052(3) Uani 1 d . . . H3A H 0.7223 0.9209 0.5703 0.062 Uiso 1 calc R . . C4A C 0.9593(12) 0.8597(8) 0.5120(8) 0.054(3) Uani 1 d . . . H4A1 H 1.0409 0.8908 0.5312 0.065 Uiso 1 calc R . . H4A2 H 1.0147 0.8598 0.4461 0.065 Uiso 1 calc R . . C5A C 0.9317(12) 0.7456(7) 0.5949(7) 0.050(3) Uani 1 d . . . H5A H 0.8757 0.7486 0.6600 0.060 Uiso 1 calc R . . C6A C 1.1097(15) 0.6756(8) 0.6127(10) 0.098(5) Uani 1 d . . . C7A C 1.0919(13) 0.5682(7) 0.7023(8) 0.087(4) Uani 1 d . . . H7A1 H 1.0525 0.5754 0.7660 0.104 Uiso 1 calc R . . H7A2 H 1.2107 0.5272 0.7064 0.104 Uiso 1 calc R . . C8A C 0.9516(12) 0.5097(7) 0.6901(8) 0.051(3) Uani 1 d . . . H8A H 1.0029 0.4917 0.6326 0.061 Uiso 1 calc R . . C9A C 0.7731(11) 0.5803(7) 0.6664(7) 0.041(3) Uani 1 d . . . H9A H 0.7256 0.5955 0.7260 0.049 Uiso 1 calc R . . C10A C 0.8030(11) 0.6894(6) 0.5710(7) 0.037(2) Uani 1 d . . . C11A C 0.6300(12) 0.5189(7) 0.6622(8) 0.061(3) Uani 1 d . . . H11A H 0.6688 0.5056 0.6018 0.073 Uiso 1 calc R . . H11B H 0.5139 0.5626 0.6538 0.073 Uiso 1 calc R . . C12A C 0.5983(12) 0.4109(7) 0.7600(7) 0.053(3) Uani 1 d . . . H12A H 0.5423 0.4244 0.8190 0.063 Uiso 1 calc R . . H12B H 0.5132 0.3743 0.7493 0.063 Uiso 1 calc R . . C13A C 0.7757(12) 0.3398(7) 0.7838(8) 0.044(3) Uani 1 d . . . C14A C 0.9105(12) 0.4080(7) 0.7881(8) 0.050(3) Uani 1 d . . . H14A H 0.8524 0.4292 0.8428 0.060 Uiso 1 calc R . . C15A C 1.0760(11) 0.3270(7) 0.8289(7) 0.067(3) Uani 1 d . . . H15A H 1.1430 0.3495 0.8636 0.081 Uiso 1 calc R . . H15B H 1.1597 0.3172 0.7731 0.081 Uiso 1 calc R . . C16A C 0.9825(12) 0.2233(7) 0.9063(8) 0.064(3) Uani 1 d . . . H16A H 1.0393 0.1648 0.8907 0.077 Uiso 1 calc R . . H16B H 0.9950 0.2052 0.9766 0.077 Uiso 1 calc R . . C17A C 0.7756(11) 0.2454(7) 0.8936(6) 0.045(2) Uani 1 d . . . H17A H 0.7104 0.2720 0.9434 0.054 Uiso 1 calc R . . C18A C 0.8469(13) 0.3018(7) 0.7019(7) 0.070(3) Uani 1 d . . . H18A H 0.8635 0.3618 0.6352 0.104 Uiso 1 calc R . . H18B H 0.7600 0.2590 0.7031 0.104 Uiso 1 calc R . . H18C H 0.9626 0.2604 0.7152 0.104 Uiso 1 calc R . . C19A C 0.8856(14) 0.6757(7) 0.4728(8) 0.079(4) Uani 1 d . . . H19A H 0.9886 0.6231 0.4865 0.118 Uiso 1 calc R . . H19B H 0.9259 0.7420 0.4185 0.118 Uiso 1 calc R . . H19C H 0.7941 0.6536 0.4520 0.118 Uiso 1 calc R . . C20A C 0.6928(12) 0.1426(7) 0.9212(7) 0.044(3) Uani 1 d . . . H20A H 0.7667 0.1111 0.8771 0.053 Uiso 1 calc R . . C21A C 0.4908(11) 0.1613(7) 0.9017(6) 0.055(3) Uani 1 d . . . H21A H 0.4144 0.1902 0.9456 0.083 Uiso 1 calc R . . H21B H 0.4487 0.0951 0.9169 0.083 Uiso 1 calc R . . H21C H 0.4845 0.2100 0.8307 0.083 Uiso 1 calc R . . C22A C 0.7069(12) 0.0629(7) 1.0346(7) 0.047(3) Uani 1 d . . . H22A H 0.8378 0.0463 1.0411 0.056 Uiso 1 calc R . . C23A C 0.6250(13) -0.0407(7) 1.0716(8) 0.062(3) Uani 1 d . . . H23A H 0.6693 -0.0676 1.0206 0.074 Uiso 1 calc R . . H23B H 0.4923 -0.0270 1.0759 0.074 Uiso 1 calc R . . C24A C 0.6707(13) -0.1278(8) 1.1785(8) 0.059(3) Uani 1 d . . . H24A H 0.6755 -0.0918 1.2204 0.071 Uiso 1 calc R . . C25A C 0.5200(17) -0.2062(9) 1.2375(9) 0.086(4) Uani 1 d . . . H25A H 0.5656 -0.2619 1.2998 0.103 Uiso 1 calc R . . C26A C 0.3467(17) -0.1521(11) 1.2731(10) 0.141(6) Uani 1 d . . . D26A D 0.2729(17) -0.1190(11) 1.2188(10) 0.211 Uiso 1 d R . . D26B D 0.2787(17) -0.2033(11) 1.3338(10) 0.211 Uiso 1 d R . . D26C D 0.3776(17) -0.0992(11) 1.2885(10) 0.211 Uiso 1 d R . . C27A C 0.482(2) -0.2596(10) 1.1786(10) 0.155(7) Uani 1 d . . . D27A D 0.549(2) -0.3282(10) 1.1974(10) 0.232 Uiso 1 d R . . D27B D 0.352(2) -0.2672(10) 1.1941(10) 0.232 Uiso 1 d R . . D27C D 0.515(2) -0.2159(10) 1.1059(10) 0.232 Uiso 1 d R . . C28A C 0.8621(16) -0.1833(10) 1.1647(9) 0.131(6) Uani 1 d . . . H28A H 0.9530 -0.1337 1.1405 0.196 Uiso 1 calc R . . H28B H 0.8683 -0.2101 1.1152 0.196 Uiso 1 calc R . . H28C H 0.8853 -0.2410 1.2298 0.196 Uiso 1 calc R . . O1A O 1.2514(10) 0.7042(7) 0.5544(9) 0.200(7) Uani 1 d . . . O2A O 0.7984(8) 1.0326(5) 0.4290(5) 0.060(2) Uani 1 d . . . H2AO H 0.7030 1.0693 0.4346 0.089 Uiso 1 calc R . . O3A O 0.6210(8) 0.1107(5) 1.1024(5) 0.0557(18) Uani 1 d . . . H3AO H 0.6930 0.1040 1.1401 0.084 Uiso 1 calc R . . C1B C 0.1148(13) 0.4686(7) 1.0049(8) 0.059(3) Uani 1 d . . . H1B1 H 0.1642 0.4703 0.9378 0.071 Uiso 1 calc R . . H1B2 H -0.0056 0.5077 1.0000 0.071 Uiso 1 calc R . . C2B C 0.0907(13) 0.3518(7) 1.0851(8) 0.067(3) Uani 1 d . . . H2B1 H 0.0312 0.3487 1.1516 0.080 Uiso 1 calc R . . H2B2 H 0.0140 0.3208 1.0628 0.080 Uiso 1 calc R . . C3B C 0.2781(13) 0.2910(8) 1.0946(8) 0.061(3) Uani 1 d . . . H3B H 0.3348 0.2941 1.0270 0.073 Uiso 1 calc R . . C4B C 0.4023(13) 0.3397(8) 1.1281(8) 0.062(3) Uani 1 d . . . H4B1 H 0.3476 0.3385 1.1945 0.074 Uiso 1 calc R . . H4B2 H 0.5216 0.2994 1.1350 0.074 Uiso 1 calc R . . C5B C 0.4244(12) 0.4528(7) 1.0469(7) 0.049(3) Uani 1 d . . . H5B H 0.4754 0.4491 0.9815 0.058 Uiso 1 calc R . . C6B C 0.5600(13) 0.5068(7) 1.0649(7) 0.058(3) Uani 1 d . . . C7B C 0.6016(12) 0.6159(7) 0.9792(7) 0.062(3) Uani 1 d . . . H7B1 H 0.6726 0.6090 0.9189 0.075 Uiso 1 calc R . . H7B2 H 0.6752 0.6483 1.0017 0.075 Uiso 1 calc R . . C8B C 0.4229(12) 0.6881(7) 0.9496(7) 0.046(3) Uani 1 d . . . H8B H 0.3662 0.7074 1.0057 0.055 Uiso 1 calc R . . C9B C 0.2832(12) 0.6329(7) 0.9320(7) 0.043(3) Uani 1 d . . . H9B H 0.3440 0.6151 0.8754 0.052 Uiso 1 calc R . . C10B C 0.2404(13) 0.5256(7) 1.0287(8) 0.050(3) Uani 1 d . . . C11B C 0.1173(12) 0.7082(7) 0.8950(7) 0.053(3) Uani 1 d . . . H11C H 0.0494 0.7244 0.9507 0.064 Uiso 1 calc R . . H11D H 0.0375 0.6732 0.8789 0.064 Uiso 1 calc R . . C12B C 0.1657(13) 0.8139(7) 0.7979(8) 0.058(3) Uani 1 d . . . H12C H 0.2200 0.7990 0.7395 0.069 Uiso 1 calc R . . H12D H 0.0537 0.8601 0.7810 0.069 Uiso 1 calc R . . C13B C 0.2989(13) 0.8705(7) 0.8156(7) 0.044(3) Uani 1 d . . . C14B C 0.4664(11) 0.7899(7) 0.8502(7) 0.047(3) Uani 1 d . . . H14B H 0.5145 0.7681 0.7950 0.057 Uiso 1 calc R . . C15B C 0.6090(13) 0.8568(7) 0.8473(7) 0.070(3) Uani 1 d . . . H15C H 0.7331 0.8248 0.8379 0.084 Uiso 1 calc R . . H15D H 0.5884 0.8649 0.9105 0.084 Uiso 1 calc R . . C16B C 0.5777(12) 0.9643(7) 0.7537(7) 0.058(3) Uani 1 d . . . H16C H 0.6811 0.9753 0.6982 0.070 Uiso 1 calc R . . H16D H 0.5635 1.0218 0.7730 0.070 Uiso 1 calc R . . C17B C 0.3972(11) 0.9599(7) 0.7184(7) 0.049(3) Uani 1 d . . . H17B H 0.4360 0.9329 0.6664 0.059 Uiso 1 calc R . . C18B C 0.2073(14) 0.9127(7) 0.8971(7) 0.069(3) Uani 1 d . . . H18D H 0.0993 0.9589 0.8748 0.103 Uiso 1 calc R . . H18E H 0.2929 0.9511 0.9038 0.103 Uiso 1 calc R . . H18F H 0.1735 0.8539 0.9627 0.103 Uiso 1 calc R . . C19B C 0.1512(14) 0.5413(8) 1.1255(8) 0.074(4) Uani 1 d . . . H19D H 0.0346 0.5821 1.1142 0.111 Uiso 1 calc R . . H19E H 0.2303 0.5781 1.1388 0.111 Uiso 1 calc R . . H19F H 0.1332 0.4734 1.1838 0.111 Uiso 1 calc R . . C20B C 0.2975(12) 1.0693(7) 0.6647(7) 0.050(3) Uani 1 d . . . H20B H 0.2736 1.1006 0.7133 0.060 Uiso 1 calc R . . C21B C 0.1104(11) 1.0666(7) 0.6403(7) 0.063(3) Uani 1 d . . . H21D H 0.0241 1.0406 0.7032 0.094 Uiso 1 calc R . . H21E H 0.1228 1.0207 0.6078 0.094 Uiso 1 calc R . . H21F H 0.0670 1.1369 0.5945 0.094 Uiso 1 calc R . . C22B C 0.4226(14) 1.1417(8) 0.5686(8) 0.058(3) Uani 1 d . . . H22B H 0.5438 1.1330 0.5881 0.070 Uiso 1 calc R . . C23B C 0.3559(14) 1.2583(7) 0.5286(8) 0.065(3) Uani 1 d . . . H23C H 0.2282 1.2665 0.5199 0.077 Uiso 1 calc R . . H23D H 0.3596 1.2806 0.5809 0.077 Uiso 1 calc R . . C24B C 0.4613(14) 1.3319(8) 0.4283(8) 0.061(3) Uani 1 d . . . H24B H 0.4415 1.3141 0.3749 0.073 Uiso 1 calc R . . C25B C 0.3927(17) 1.4498(8) 0.3947(8) 0.081(3) Uani 1 d . . . H25B H 0.4548 1.4902 0.3241 0.098 Uiso 1 calc R . . C26B C 0.1815(18) 1.4672(8) 0.3920(8) 0.101(4) Uani 1 d . . . D26D D 0.1449(18) 1.5417(8) 0.3668(8) 0.152 Uiso 1 d R . . D26E D 0.1510(18) 1.4420(8) 0.3477(8) 0.152 Uiso 1 d R . . D26F D 0.1182(18) 1.4299(8) 0.4609(8) 0.152 Uiso 1 d R . . C27B C 0.4294(19) 1.4956(9) 0.4603(9) 0.126(5) Uani 1 d . . . D27D D 0.3896(19) 1.4512(9) 0.5321(9) 0.189 Uiso 1 d R . . D27E D 0.5588(19) 1.5026(9) 0.4491(9) 0.189 Uiso 1 d R . . D27F D 0.3629(19) 1.5644(9) 0.4406(9) 0.189 Uiso 1 d R . . C28B C 0.6693(15) 1.3171(9) 0.4283(9) 0.115(5) Uani 1 d . . . H28D H 0.7185 1.2514 0.4259 0.173 Uiso 1 calc R . . H28E H 0.6931 1.3159 0.4901 0.173 Uiso 1 calc R . . H28F H 0.7265 1.3747 0.3689 0.173 Uiso 1 calc R . . O1B O 0.6331(10) 0.4664(5) 1.1421(5) 0.088(2) Uani 1 d . . . O2B O 0.2566(8) 0.1814(5) 1.1676(5) 0.064(2) Uani 1 d . . . H2BO H 0.3523 0.1451 1.1615 0.096 Uiso 1 calc R . . O3B O 0.4465(8) 1.1078(5) 0.4875(5) 0.0582(19) Uani 1 d . . . H3BO H 0.3458 1.1107 0.4723 0.087 Uiso 1 calc R . . O1W O 0.8958(10) 1.0901(6) 0.2119(5) 0.099(3) Uani 1 d . . . H1W1 H 0.8739 1.0561 0.2861 0.149 Uiso 1 d R . . H2W1 H 1.0134 1.1175 0.1941 0.149 Uiso 1 d R . . O2W O 0.1527(10) 1.1411(6) 0.3810(6) 0.095(3) Uani 1 d . . . H1W2 H 0.2052 1.1312 0.3203 0.142 Uiso 1 d R . . H2W2 H 0.0486 1.0996 0.4107 0.142 Uiso 1 d 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 C1A 0.046(6) 0.041(7) 0.089(9) -0.008(6) -0.024(6) -0.015(5) C2A 0.044(6) 0.045(7) 0.086(9) -0.016(7) -0.025(6) -0.001(5) C3A 0.058(7) 0.042(7) 0.050(7) -0.021(6) 0.010(5) -0.010(5) C4A 0.041(7) 0.048(7) 0.067(8) -0.015(6) -0.015(6) -0.006(5) C5A 0.047(7) 0.058(8) 0.043(7) -0.014(6) -0.015(5) -0.012(6) C6A 0.053(8) 0.050(8) 0.160(13) 0.004(8) -0.051(8) -0.029(6) C7A 0.050(7) 0.058(7) 0.127(10) -0.001(7) -0.052(7) -0.013(6) C8A 0.034(6) 0.051(7) 0.057(7) -0.012(6) -0.009(5) -0.008(5) C9A 0.029(6) 0.048(7) 0.040(6) -0.017(6) -0.003(5) -0.002(5) C10A 0.029(6) 0.030(6) 0.052(7) -0.017(6) -0.004(5) -0.009(5) C11A 0.036(6) 0.059(8) 0.078(8) -0.015(7) -0.024(6) -0.006(5) C12A 0.047(7) 0.039(6) 0.062(7) -0.011(6) -0.008(5) -0.012(5) C13A 0.032(6) 0.047(7) 0.053(7) -0.023(6) -0.011(5) 0.000(5) C14A 0.032(6) 0.051(7) 0.067(7) -0.021(6) -0.018(5) -0.001(5) C15A 0.038(6) 0.067(8) 0.086(8) -0.015(6) -0.032(6) -0.006(5) C16A 0.052(7) 0.053(7) 0.072(7) -0.005(6) -0.034(6) -0.005(5) C17A 0.041(6) 0.050(6) 0.043(6) -0.019(5) 0.000(5) -0.013(5) C18A 0.076(8) 0.055(7) 0.060(8) -0.006(6) -0.008(6) -0.022(6) C19A 0.100(9) 0.055(8) 0.070(9) -0.026(7) 0.004(7) -0.009(7) C20A 0.050(6) 0.046(6) 0.037(6) -0.017(5) -0.007(5) -0.008(5) C21A 0.059(6) 0.051(6) 0.049(6) -0.010(5) -0.015(5) -0.015(5) C22A 0.050(6) 0.057(7) 0.043(6) -0.032(5) -0.009(5) 0.003(5) C23A 0.070(7) 0.049(7) 0.055(7) -0.007(6) -0.010(6) -0.025(6) C24A 0.060(7) 0.059(7) 0.048(7) -0.018(6) -0.001(5) -0.007(6) C25A 0.109(10) 0.071(8) 0.059(7) -0.011(7) 0.002(7) -0.034(8) C26A 0.094(11) 0.178(15) 0.123(12) -0.047(11) 0.028(9) -0.060(10) C27A 0.28(2) 0.105(11) 0.103(11) -0.029(9) -0.032(12) -0.119(13) C28A 0.100(11) 0.124(12) 0.089(10) -0.012(9) 0.001(8) 0.055(9) O1A 0.043(5) 0.093(7) 0.316(15) 0.052(8) -0.057(7) -0.024(5) O2A 0.061(5) 0.043(5) 0.066(5) -0.023(4) 0.005(4) -0.004(3) O3A 0.069(4) 0.056(4) 0.050(4) -0.025(4) -0.017(4) -0.009(3) C1B 0.051(7) 0.037(7) 0.078(8) -0.013(6) -0.022(6) -0.002(5) C2B 0.057(8) 0.052(8) 0.080(9) -0.018(7) -0.011(6) -0.010(6) C3B 0.070(8) 0.050(8) 0.052(7) -0.010(6) -0.007(6) -0.019(6) C4B 0.050(7) 0.061(8) 0.063(8) -0.021(7) -0.004(6) -0.002(6) C5B 0.054(7) 0.049(7) 0.046(7) -0.019(6) -0.017(5) -0.006(6) C6B 0.054(7) 0.050(7) 0.047(7) -0.004(6) -0.011(6) 0.004(5) C7B 0.045(6) 0.066(7) 0.068(7) -0.018(6) -0.014(5) -0.014(6) C8B 0.044(6) 0.044(7) 0.043(6) -0.015(5) -0.001(5) -0.008(5) C9B 0.045(6) 0.039(7) 0.038(7) -0.012(5) -0.002(5) -0.010(5) C10B 0.051(7) 0.050(7) 0.052(7) -0.023(6) -0.011(6) -0.006(6) C11B 0.038(6) 0.049(7) 0.066(8) -0.018(6) -0.010(5) -0.005(5) C12B 0.051(6) 0.043(7) 0.065(7) -0.008(6) -0.014(6) -0.009(5) C13B 0.050(7) 0.036(6) 0.042(7) -0.015(5) -0.002(5) -0.010(5) C14B 0.042(7) 0.049(7) 0.051(7) -0.021(6) -0.004(5) -0.011(5) C15B 0.074(8) 0.059(7) 0.065(7) -0.011(6) -0.010(6) -0.029(6) C16B 0.053(7) 0.057(7) 0.062(7) -0.021(6) -0.004(5) -0.018(5) C17B 0.042(6) 0.047(6) 0.055(6) -0.020(5) 0.004(5) -0.018(5) C18B 0.089(8) 0.062(8) 0.049(7) -0.029(6) 0.008(6) 0.000(6) C19B 0.076(8) 0.067(8) 0.054(8) -0.019(7) 0.021(6) -0.007(6) C20B 0.058(7) 0.041(6) 0.052(7) -0.022(5) -0.003(5) -0.009(5) C21B 0.048(6) 0.058(7) 0.072(7) -0.019(6) -0.011(5) -0.006(5) C22B 0.056(7) 0.047(7) 0.059(7) -0.015(6) -0.003(5) -0.009(5) C23B 0.081(8) 0.037(7) 0.062(7) -0.018(6) 0.006(6) -0.005(6) C24B 0.083(8) 0.047(7) 0.055(7) -0.025(6) -0.004(6) -0.014(6) C25B 0.118(11) 0.057(8) 0.054(7) -0.019(6) 0.007(7) -0.015(7) C26B 0.142(12) 0.070(9) 0.068(8) -0.016(7) -0.025(8) 0.017(8) C27B 0.226(17) 0.081(9) 0.090(10) -0.050(8) -0.016(10) -0.036(10) C28B 0.093(10) 0.089(10) 0.119(11) -0.007(8) 0.002(9) -0.036(8) O1B 0.096(6) 0.073(5) 0.077(5) -0.002(4) -0.042(5) -0.023(4) O2B 0.055(4) 0.048(5) 0.070(5) -0.011(4) -0.006(4) -0.006(4) O3B 0.049(4) 0.057(5) 0.070(5) -0.033(4) -0.003(4) -0.002(3) O1W 0.099(6) 0.133(7) 0.069(5) -0.026(5) -0.025(5) -0.056(5) O2W 0.084(6) 0.134(7) 0.071(6) -0.045(5) -0.003(4) -0.037(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C10A 1.521(11) . ? C1A C2A 1.550(11) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.494(11) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A O2A 1.447(9) . ? C3A C4A 1.501(11) . ? C3A H3A 0.9800 . ? C4A C5A 1.536(11) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A C6A 1.509(13) . ? C5A C10A 1.542(11) . ? C5A H5A 0.9800 . ? C6A O1A 1.208(13) . ? C6A C7A 1.496(13) . ? C7A C8A 1.538(12) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A C14A 1.521(12) . ? C8A C9A 1.523(11) . ? C8A H8A 0.9800 . ? C9A C11A 1.527(11) . ? C9A C10A 1.555(11) . ? C9A H9A 0.9800 . ? C10A C19A 1.534(12) . ? C11A C12A 1.562(10) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A C13A 1.520(11) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C13A C18A 1.506(13) . ? C13A C14A 1.550(12) . ? C13A C17A 1.557(12) . ? C14A C15A 1.551(11) . ? C14A H14A 0.9800 . ? C15A C16A 1.561(11) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A C17A 1.557(10) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C17A C20A 1.536(11) . ? C17A H17A 0.9800 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C22A 1.543(10) . ? C20A C21A 1.552(10) . ? C20A H20A 0.9800 . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A O3A 1.443(9) . ? C22A C23A 1.513(11) . ? C22A H22A 0.9800 . ? C23A C24A 1.557(12) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A C28A 1.529(13) . ? C24A C25A 1.547(13) . ? C24A H24A 0.9800 . ? C25A C27A 1.490(15) . ? C25A C26A 1.509(14) . ? C25A H25A 0.9800 . ? C26A D26A 0.9600 . ? C26A D26B 0.9600 . ? C26A D26C 0.9600 . ? C27A D27A 0.9600 . ? C27A D27C 0.9600 . ? C27A D27B 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? O2A H2AO 0.8200 . ? O3A H3AO 0.8200 . ? C1B C10B 1.533(11) . ? C1B C2B 1.549(11) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.510(12) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B O2B 1.445(10) . ? C3B C4B 1.530(12) . ? C3B H3B 0.9800 . ? C4B C5B 1.513(12) . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C5B C6B 1.510(12) . ? C5B C10B 1.562(12) . ? C5B H5B 0.9800 . ? C6B O1B 1.217(10) . ? C6B C7B 1.516(12) . ? C7B C8B 1.545(11) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B C14B 1.534(11) . ? C8B C9B 1.543(11) . ? C8B H8B 0.9800 . ? C9B C11B 1.507(11) . ? C9B C10B 1.561(12) . ? C9B H9B 0.9800 . ? C10B C19B 1.539(13) . ? C11B C12B 1.559(11) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B C13B 1.518(11) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? C13B C14B 1.542(11) . ? C13B C17B 1.551(11) . ? C13B C18B 1.566(12) . ? C14B C15B 1.536(11) . ? C14B H14B 0.9800 . ? C15B C16B 1.540(11) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B C17B 1.569(11) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C20B 1.524(11) . ? C17B H17B 0.9800 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C21B 1.530(11) . ? C20B C22B 1.537(12) . ? C20B H20B 0.9800 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B O3B 1.454(11) . ? C22B C23B 1.515(12) . ? C22B H22B 0.9800 . ? C23B C24B 1.504(11) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B C28B 1.531(12) . ? C24B C25B 1.541(13) . ? C24B H24B 0.9800 . ? C25B C27B 1.488(13) . ? C25B C26B 1.560(15) . ? C25B H25B 0.9800 . ? C26B D26E 0.9600 . ? C26B D26F 0.9600 . ? C26B D26D 0.9601 . ? C27B D27D 0.9599 . ? C27B D27F 0.9599 . ? C27B D27E 0.9599 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? O2B H2BO 0.8200 . ? O3B H3BO 0.8200 . ? O1W H1W1 0.9600 . ? O1W H2W1 0.9600 . ? O2W H1W2 0.9599 . ? O2W H2W2 0.9600 . ? 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 C10A C1A C2A 113.0(7) . . ? C10A C1A H1A1 109.0 . . ? C2A C1A H1A1 109.0 . . ? C10A C1A H1A2 109.0 . . ? C2A C1A H1A2 109.0 . . ? H1A1 C1A H1A2 107.8 . . ? C3A C2A C1A 111.1(8) . . ? C3A C2A H2A1 109.4 . . ? C1A C2A H2A1 109.4 . . ? C3A C2A H2A2 109.4 . . ? C1A C2A H2A2 109.4 . . ? H2A1 C2A H2A2 108.0 . . ? O2A C3A C2A 111.8(8) . . ? O2A C3A C4A 110.0(7) . . ? C2A C3A C4A 110.4(8) . . ? O2A C3A H3A 108.1 . . ? C2A C3A H3A 108.1 . . ? C4A C3A H3A 108.1 . . ? C3A C4A C5A 108.8(7) . . ? C3A C4A H4A1 109.9 . . ? C5A C4A H4A1 109.9 . . ? C3A C4A H4A2 109.9 . . ? C5A C4A H4A2 109.9 . . ? H4A1 C4A H4A2 108.3 . . ? C6A C5A C4A 113.0(8) . . ? C6A C5A C10A 107.1(8) . . ? C4A C5A C10A 113.7(7) . . ? C6A C5A H5A 107.6 . . ? C4A C5A H5A 107.6 . . ? C10A C5A H5A 107.6 . . ? O1A C6A C7A 124.0(11) . . ? O1A C6A C5A 121.1(10) . . ? C7A C6A C5A 114.7(10) . . ? C6A C7A C8A 110.5(8) . . ? C6A C7A H7A1 109.6 . . ? C8A C7A H7A1 109.6 . . ? C6A C7A H7A2 109.6 . . ? C8A C7A H7A2 109.6 . . ? H7A1 C7A H7A2 108.1 . . ? C14A C8A C9A 109.2(8) . . ? C14A C8A C7A 110.8(8) . . ? C9A C8A C7A 110.3(8) . . ? C14A C8A H8A 108.8 . . ? C9A C8A H8A 108.8 . . ? C7A C8A H8A 108.8 . . ? C8A C9A C11A 109.9(8) . . ? C8A C9A C10A 112.9(7) . . ? C11A C9A C10A 114.7(7) . . ? C8A C9A H9A 106.2 . . ? C11A C9A H9A 106.2 . . ? C10A C9A H9A 106.2 . . ? C1A C10A C19A 109.3(8) . . ? C1A C10A C5A 107.3(7) . . ? C19A C10A C5A 111.0(8) . . ? C1A C10A C9A 110.7(7) . . ? C19A C10A C9A 111.1(7) . . ? C5A C10A C9A 107.4(7) . . ? C9A C11A C12A 114.0(8) . . ? C9A C11A H11A 108.8 . . ? C12A C11A H11A 108.8 . . ? C9A C11A H11B 108.8 . . ? C12A C11A H11B 108.8 . . ? H11A C11A H11B 107.7 . . ? C13A C12A C11A 112.6(7) . . ? C13A C12A H12A 109.1 . . ? C11A C12A H12A 109.1 . . ? C13A C12A H12B 109.1 . . ? C11A C12A H12B 109.1 . . ? H12A C12A H12B 107.8 . . ? C18A C13A C12A 109.9(8) . . ? C18A C13A C14A 112.6(8) . . ? C12A C13A C14A 105.8(7) . . ? C18A C13A C17A 110.5(8) . . ? C12A C13A C17A 118.0(8) . . ? C14A C13A C17A 99.6(7) . . ? C8A C14A C13A 115.6(8) . . ? C8A C14A C15A 117.5(8) . . ? C13A C14A C15A 103.2(7) . . ? C8A C14A H14A 106.6 . . ? C13A C14A H14A 106.6 . . ? C15A C14A H14A 106.6 . . ? C14A C15A C16A 103.1(6) . . ? C14A C15A H15A 111.1 . . ? C16A C15A H15A 111.1 . . ? C14A C15A H15B 111.1 . . ? C16A C15A H15B 111.1 . . ? H15A C15A H15B 109.1 . . ? C17A C16A C15A 106.9(7) . . ? C17A C16A H16A 110.4 . . ? C15A C16A H16A 110.4 . . ? C17A C16A H16B 110.4 . . ? C15A C16A H16B 110.4 . . ? H16A C16A H16B 108.6 . . ? C20A C17A C13A 120.4(7) . . ? C20A C17A C16A 111.1(7) . . ? C13A C17A C16A 103.2(7) . . ? C20A C17A H17A 107.2 . . ? C13A C17A H17A 107.2 . . ? C16A C17A H17A 107.2 . . ? C13A C18A H18A 109.5 . . ? C13A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C13A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C10A C19A H19A 109.5 . . ? C10A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C10A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C17A C20A C22A 110.1(7) . . ? C17A C20A C21A 113.2(7) . . ? C22A C20A C21A 110.4(7) . . ? C17A C20A H20A 107.7 . . ? C22A C20A H20A 107.7 . . ? C21A C20A H20A 107.7 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? O3A C22A C23A 108.7(8) . . ? O3A C22A C20A 110.1(7) . . ? C23A C22A C20A 114.9(7) . . ? O3A C22A H22A 107.6 . . ? C23A C22A H22A 107.6 . . ? C20A C22A H22A 107.6 . . ? C22A C23A C24A 114.4(8) . . ? C22A C23A H23A 108.7 . . ? C24A C23A H23A 108.7 . . ? C22A C23A H23B 108.7 . . ? C24A C23A H23B 108.7 . . ? H23A C23A H23B 107.6 . . ? C28A C24A C25A 112.9(10) . . ? C28A C24A C23A 109.8(9) . . ? C25A C24A C23A 112.4(8) . . ? C28A C24A H24A 107.1 . . ? C25A C24A H24A 107.1 . . ? C23A C24A H24A 107.1 . . ? C27A C25A C26A 111.6(12) . . ? C27A C25A C24A 113.7(10) . . ? C26A C25A C24A 110.5(10) . . ? C27A C25A H25A 106.8 . . ? C26A C25A H25A 106.8 . . ? C24A C25A H25A 106.8 . . ? D26A C26A D26B 109.5 . . ? D26A C26A D26C 109.5 . . ? D26B C26A D26C 109.5 . . ? D26A C26A C25A 108.7 . . ? D26B C26A C25A 109.9 . . ? D26C C26A C25A 109.8 . . ? D27A C27A D27C 109.5 . . ? D27A C27A D27B 109.5 . . ? D27C C27A D27B 109.5 . . ? D27A C27A C25A 111.8 . . ? D27C C27A C25A 109.2 . . ? D27B C27A C25A 107.4 . . ? C24A C28A H28A 109.5 . . ? C24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C3A O2A H2AO 109.5 . . ? C22A O3A H3AO 109.5 . . ? C10B C1B C2B 115.2(8) . . ? C10B C1B H1B1 108.5 . . ? C2B C1B H1B1 108.5 . . ? C10B C1B H1B2 108.5 . . ? C2B C1B H1B2 108.5 . . ? H1B1 C1B H1B2 107.5 . . ? C3B C2B C1B 108.7(8) . . ? C3B C2B H2B1 110.0 . . ? C1B C2B H2B1 110.0 . . ? C3B C2B H2B2 110.0 . . ? C1B C2B H2B2 110.0 . . ? H2B1 C2B H2B2 108.3 . . ? O2B C3B C2B 109.1(8) . . ? O2B C3B C4B 111.0(8) . . ? C2B C3B C4B 110.8(9) . . ? O2B C3B H3B 108.6 . . ? C2B C3B H3B 108.6 . . ? C4B C3B H3B 108.6 . . ? C5B C4B C3B 108.4(8) . . ? C5B C4B H4B1 110.0 . . ? C3B C4B H4B1 110.0 . . ? C5B C4B H4B2 110.0 . . ? C3B C4B H4B2 110.0 . . ? H4B1 C4B H4B2 108.4 . . ? C6B C5B C4B 113.8(8) . . ? C6B C5B C10B 109.1(8) . . ? C4B C5B C10B 114.6(8) . . ? C6B C5B H5B 106.2 . . ? C4B C5B H5B 106.2 . . ? C10B C5B H5B 106.2 . . ? O1B C6B C5B 123.1(8) . . ? O1B C6B C7B 121.5(9) . . ? C5B C6B C7B 115.3(8) . . ? C6B C7B C8B 111.4(7) . . ? C6B C7B H7B1 109.4 . . ? C8B C7B H7B1 109.4 . . ? C6B C7B H7B2 109.4 . . ? C8B C7B H7B2 109.4 . . ? H7B1 C7B H7B2 108.0 . . ? C14B C8B C9B 108.2(7) . . ? C14B C8B C7B 110.4(7) . . ? C9B C8B C7B 112.2(7) . . ? C14B C8B H8B 108.7 . . ? C9B C8B H8B 108.7 . . ? C7B C8B H8B 108.7 . . ? C11B C9B C8B 110.9(7) . . ? C11B C9B C10B 115.3(8) . . ? C8B C9B C10B 110.7(7) . . ? C11B C9B H9B 106.5 . . ? C8B C9B H9B 106.5 . . ? C10B C9B H9B 106.5 . . ? C1B C10B C19B 110.3(9) . . ? C1B C10B C9B 109.3(8) . . ? C19B C10B C9B 112.1(8) . . ? C1B C10B C5B 105.9(7) . . ? C19B C10B C5B 110.9(8) . . ? C9B C10B C5B 108.1(8) . . ? C9B C11B C12B 113.7(8) . . ? C9B C11B H11C 108.8 . . ? C12B C11B H11C 108.8 . . ? C9B C11B H11D 108.8 . . ? C12B C11B H11D 108.8 . . ? H11C C11B H11D 107.7 . . ? C13B C12B C11B 111.8(8) . . ? C13B C12B H12C 109.3 . . ? C11B C12B H12C 109.3 . . ? C13B C12B H12D 109.3 . . ? C11B C12B H12D 109.3 . . ? H12C C12B H12D 107.9 . . ? C12B C13B C14B 106.4(7) . . ? C12B C13B C17B 116.9(8) . . ? C14B C13B C17B 99.5(7) . . ? C12B C13B C18B 111.6(8) . . ? C14B C13B C18B 112.1(8) . . ? C17B C13B C18B 109.7(8) . . ? C8B C14B C15B 117.9(8) . . ? C8B C14B C13B 115.0(7) . . ? C15B C14B C13B 103.8(7) . . ? C8B C14B H14B 106.5 . . ? C15B C14B H14B 106.5 . . ? C13B C14B H14B 106.5 . . ? C14B C15B C16B 103.8(7) . . ? C14B C15B H15C 111.0 . . ? C16B C15B H15C 111.0 . . ? C14B C15B H15D 111.0 . . ? C16B C15B H15D 111.0 . . ? H15C C15B H15D 109.0 . . ? C15B C16B C17B 106.4(7) . . ? C15B C16B H16C 110.5 . . ? C17B C16B H16C 110.5 . . ? C15B C16B H16D 110.5 . . ? C17B C16B H16D 110.5 . . ? H16C C16B H16D 108.6 . . ? C20B C17B C13B 121.0(8) . . ? C20B C17B C16B 112.6(7) . . ? C13B C17B C16B 103.4(7) . . ? C20B C17B H17B 106.3 . . ? C13B C17B H17B 106.3 . . ? C16B C17B H17B 106.3 . . ? C13B C18B H18D 109.5 . . ? C13B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C13B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C10B C19B H19D 109.5 . . ? C10B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C10B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17B C20B C21B 113.8(7) . . ? C17B C20B C22B 110.7(8) . . ? C21B C20B C22B 112.1(8) . . ? C17B C20B H20B 106.6 . . ? C21B C20B H20B 106.6 . . ? C22B C20B H20B 106.6 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? O3B C22B C23B 110.7(8) . . ? O3B C22B C20B 110.0(8) . . ? C23B C22B C20B 113.7(8) . . ? O3B C22B H22B 107.4 . . ? C23B C22B H22B 107.4 . . ? C20B C22B H22B 107.4 . . ? C24B C23B C22B 116.1(8) . . ? C24B C23B H23C 108.3 . . ? C22B C23B H23C 108.3 . . ? C24B C23B H23D 108.3 . . ? C22B C23B H23D 108.3 . . ? H23C C23B H23D 107.4 . . ? C23B C24B C28B 113.1(9) . . ? C23B C24B C25B 113.5(8) . . ? C28B C24B C25B 109.6(9) . . ? C23B C24B H24B 106.7 . . ? C28B C24B H24B 106.7 . . ? C25B C24B H24B 106.7 . . ? C27B C25B C24B 115.0(10) . . ? C27B C25B C26B 108.0(10) . . ? C24B C25B C26B 110.5(9) . . ? C27B C25B H25B 107.7 . . ? C24B C25B H25B 107.7 . . ? C26B C25B H25B 107.7 . . ? D26E C26B D26F 109.5 . . ? D26E C26B D26D 109.5 . . ? D26F C26B D26D 109.5 . . ? D26E C26B C25B 111.4 . . ? D26F C26B C25B 108.8 . . ? D26D C26B C25B 108.3 . . ? D27D C27B D27F 109.5 . . ? D27D C27B D27E 109.5 . . ? D27F C27B D27E 109.5 . . ? D27D C27B C25B 110.7 . . ? D27F C27B C25B 108.2 . . ? D27E C27B C25B 109.5 . . ? C24B C28B H28D 109.5 . . ? C24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C3B O2B H2BO 109.5 . . ? C22B O3B H3BO 109.5 . . ? H1W1 O1W H2W1 104.5 . . ? H1W2 O2W H2W2 104.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10A C1A C2A C3A -56.2(12) . . . . ? C1A C2A C3A O2A -178.8(8) . . . . ? C1A C2A C3A C4A 58.3(11) . . . . ? O2A C3A C4A C5A 176.9(8) . . . . ? C2A C3A C4A C5A -59.2(11) . . . . ? C3A C4A C5A C6A -178.2(9) . . . . ? C3A C4A C5A C10A 59.4(11) . . . . ? C4A C5A C6A O1A -11.7(17) . . . . ? C10A C5A C6A O1A 114.2(13) . . . . ? C4A C5A C6A C7A 172.2(10) . . . . ? C10A C5A C6A C7A -61.8(13) . . . . ? O1A C6A C7A C8A -119.5(14) . . . . ? C5A C6A C7A C8A 56.4(14) . . . . ? C6A C7A C8A C14A -171.2(10) . . . . ? C6A C7A C8A C9A -50.2(13) . . . . ? C14A C8A C9A C11A -53.9(11) . . . . ? C7A C8A C9A C11A -175.9(8) . . . . ? C14A C8A C9A C10A 176.5(8) . . . . ? C7A C8A C9A C10A 54.5(12) . . . . ? C2A C1A C10A C19A -68.0(10) . . . . ? C2A C1A C10A C5A 52.5(11) . . . . ? C2A C1A C10A C9A 169.3(8) . . . . ? C6A C5A C10A C1A 179.2(9) . . . . ? C4A C5A C10A C1A -55.2(11) . . . . ? C6A C5A C10A C19A -61.5(10) . . . . ? C4A C5A C10A C19A 64.1(10) . . . . ? C6A C5A C10A C9A 60.2(11) . . . . ? C4A C5A C10A C9A -174.2(8) . . . . ? C8A C9A C10A C1A -176.9(8) . . . . ? C11A C9A C10A C1A 56.1(11) . . . . ? C8A C9A C10A C19A 61.5(11) . . . . ? C11A C9A C10A C19A -65.5(10) . . . . ? C8A C9A C10A C5A -60.1(11) . . . . ? C11A C9A C10A C5A 172.9(8) . . . . ? C8A C9A C11A C12A 52.9(11) . . . . ? C10A C9A C11A C12A -178.5(8) . . . . ? C9A C11A C12A C13A -54.4(12) . . . . ? C11A C12A C13A C18A -69.0(10) . . . . ? C11A C12A C13A C14A 52.9(11) . . . . ? C11A C12A C13A C17A 163.2(8) . . . . ? C9A C8A C14A C13A 60.4(12) . . . . ? C7A C8A C14A C13A -177.9(8) . . . . ? C9A C8A C14A C15A -177.2(8) . . . . ? C7A C8A C14A C15A -55.5(12) . . . . ? C18A C13A C14A C8A 61.4(11) . . . . ? C12A C13A C14A C8A -58.7(11) . . . . ? C17A C13A C14A C8A 178.4(8) . . . . ? C18A C13A C14A C15A -68.3(10) . . . . ? C12A C13A C14A C15A 171.6(8) . . . . ? C17A C13A C14A C15A 48.8(9) . . . . ? C8A C14A C15A C16A -163.9(9) . . . . ? C13A C14A C15A C16A -35.4(10) . . . . ? C14A C15A C16A C17A 8.2(10) . . . . ? C18A C13A C17A C20A -48.5(11) . . . . ? C12A C13A C17A C20A 79.1(11) . . . . ? C14A C13A C17A C20A -167.1(8) . . . . ? C18A C13A C17A C16A 76.0(9) . . . . ? C12A C13A C17A C16A -156.5(8) . . . . ? C14A C13A C17A C16A -42.7(9) . . . . ? C15A C16A C17A C20A 152.0(7) . . . . ? C15A C16A C17A C13A 21.6(10) . . . . ? C13A C17A C20A C22A -179.0(8) . . . . ? C16A C17A C20A C22A 60.4(10) . . . . ? C13A C17A C20A C21A -54.9(11) . . . . ? C16A C17A C20A C21A -175.5(8) . . . . ? C17A C20A C22A O3A 55.3(9) . . . . ? C21A C20A C22A O3A -70.4(9) . . . . ? C17A C20A C22A C23A 178.5(8) . . . . ? C21A C20A C22A C23A 52.8(10) . . . . ? O3A C22A C23A C24A -66.6(10) . . . . ? C20A C22A C23A C24A 169.5(8) . . . . ? C22A C23A C24A C28A -81.6(12) . . . . ? C22A C23A C24A C25A 151.9(9) . . . . ? C28A C24A C25A C27A -68.2(14) . . . . ? C23A C24A C25A C27A 56.6(14) . . . . ? C28A C24A C25A C26A 165.3(10) . . . . ? C23A C24A C25A C26A -69.9(13) . . . . ? C10B C1B C2B C3B -57.1(12) . . . . ? C1B C2B C3B O2B -178.7(8) . . . . ? C1B C2B C3B C4B 58.7(11) . . . . ? O2B C3B C4B C5B 178.1(8) . . . . ? C2B C3B C4B C5B -60.5(11) . . . . ? C3B C4B C5B C6B -174.0(8) . . . . ? C3B C4B C5B C10B 59.4(11) . . . . ? C4B C5B C6B O1B -5.9(14) . . . . ? C10B C5B C6B O1B 123.4(10) . . . . ? C4B C5B C6B C7B 173.6(9) . . . . ? C10B C5B C6B C7B -57.0(11) . . . . ? O1B C6B C7B C8B -129.6(10) . . . . ? C5B C6B C7B C8B 50.9(11) . . . . ? C6B C7B C8B C14B -169.5(8) . . . . ? C6B C7B C8B C9B -48.7(11) . . . . ? C14B C8B C9B C11B -53.5(10) . . . . ? C7B C8B C9B C11B -175.5(7) . . . . ? C14B C8B C9B C10B 177.2(8) . . . . ? C7B C8B C9B C10B 55.2(11) . . . . ? C2B C1B C10B C19B -67.6(11) . . . . ? C2B C1B C10B C9B 168.7(9) . . . . ? C2B C1B C10B C5B 52.5(11) . . . . ? C11B C9B C10B C1B 58.0(11) . . . . ? C8B C9B C10B C1B -175.1(8) . . . . ? C11B C9B C10B C19B -64.6(11) . . . . ? C8B C9B C10B C19B 62.3(11) . . . . ? C11B C9B C10B C5B 172.8(8) . . . . ? C8B C9B C10B C5B -60.3(10) . . . . ? C6B C5B C10B C1B 176.8(7) . . . . ? C4B C5B C10B C1B -54.3(11) . . . . ? C6B C5B C10B C19B -63.5(10) . . . . ? C4B C5B C10B C19B 65.5(11) . . . . ? C6B C5B C10B C9B 59.8(10) . . . . ? C4B C5B C10B C9B -171.2(8) . . . . ? C8B C9B C11B C12B 53.6(11) . . . . ? C10B C9B C11B C12B -179.6(8) . . . . ? C9B C11B C12B C13B -55.5(12) . . . . ? C11B C12B C13B C14B 54.6(11) . . . . ? C11B C12B C13B C17B 164.6(8) . . . . ? C11B C12B C13B C18B -68.0(10) . . . . ? C9B C8B C14B C15B -177.7(8) . . . . ? C7B C8B C14B C15B -54.5(11) . . . . ? C9B C8B C14B C13B 59.4(10) . . . . ? C7B C8B C14B C13B -177.5(7) . . . . ? C12B C13B C14B C8B -59.8(11) . . . . ? C17B C13B C14B C8B 178.4(8) . . . . ? C18B C13B C14B C8B 62.5(10) . . . . ? C12B C13B C14B C15B 170.0(7) . . . . ? C17B C13B C14B C15B 48.1(9) . . . . ? C18B C13B C14B C15B -67.8(9) . . . . ? C8B C14B C15B C16B -164.2(8) . . . . ? C13B C14B C15B C16B -35.7(10) . . . . ? C14B C15B C16B C17B 9.1(10) . . . . ? C12B C13B C17B C20B 77.6(11) . . . . ? C14B C13B C17B C20B -168.5(8) . . . . ? C18B C13B C17B C20B -50.7(11) . . . . ? C12B C13B C17B C16B -155.3(8) . . . . ? C14B C13B C17B C16B -41.3(9) . . . . ? C18B C13B C17B C16B 76.4(9) . . . . ? C15B C16B C17B C20B 152.8(8) . . . . ? C15B C16B C17B C13B 20.5(10) . . . . ? C13B C17B C20B C21B -50.7(12) . . . . ? C16B C17B C20B C21B -173.5(8) . . . . ? C13B C17B C20B C22B -177.9(9) . . . . ? C16B C17B C20B C22B 59.2(10) . . . . ? C17B C20B C22B O3B 71.4(10) . . . . ? C21B C20B C22B O3B -56.8(10) . . . . ? C17B C20B C22B C23B -163.9(8) . . . . ? C21B C20B C22B C23B 67.9(11) . . . . ? O3B C22B C23B C24B -49.4(12) . . . . ? C20B C22B C23B C24B -173.8(9) . . . . ? C22B C23B C24B C28B -51.4(13) . . . . ? C22B C23B C24B C25B -177.1(9) . . . . ? C23B C24B C25B C27B 69.0(13) . . . . ? C28B C24B C25B C27B -58.5(13) . . . . ? C23B C24B C25B C26B -53.6(12) . . . . ? C28B C24B C25B C26B 178.9(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A #_geom_hbond_publ_flag O2A H2AO O3B 0.820 1.990 2.773(8) 159.4 . O3A H3AO O1W 0.820 1.965 2.778(9) 171.0 1.546 O2B H2BO O3A 0.820 2.079 2.854(9) 157.7 . O3B H3BO O2W 0.820 2.045 2.824(9) 158.6 . O1W H1W1 O2A 0.960 1.943 2.871(9) 161.9 . O1W H2W1 O2B 0.960 2.058 3.015(8) 174.1 1.664 O2W H1W2 O2B 0.960 1.993 2.877(10) 152.2 1.564 O2W H2W2 O2A 0.960 2.160 3.08(9) 162.2 1.455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.201 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.039