data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C23 H24 O5' _chemical_formula_sum 'C23 H24 O5' _chemical_formula_weight 380.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting 'Triclinic' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4475(10) _cell_length_b 11.312(2) _cell_length_c 21.111(4) _cell_angle_alpha 93.876(6) _cell_angle_beta 98.152(6) _cell_angle_gamma 107.681(6) _cell_volume 1889.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 105 _cell_measurement_reflns_used 11052 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 32.6 _exptl_crystal_description 'needle fragment' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 105 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 35457 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.073 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 32.6 _reflns_number_total 13250 _reflns_number_gt 8222 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.1773P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13250 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.104 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.138 _refine_ls_wR_factor_gt 0.119 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.86910(12) 0.95802(9) 1.15517(5) 0.0244(2) Uani 1 1 d . . . O2A O 0.35464(11) 0.80460(9) 0.99607(4) 0.0198(2) Uani 1 1 d . . . O3A O 0.92149(12) 0.76283(9) 0.70050(4) 0.0211(2) Uani 1 1 d . . . O4A O 0.74472(12) 0.61820(8) 0.89893(4) 0.0192(2) Uani 1 1 d . . . O5A O 0.42949(12) 0.84680(8) 0.87683(5) 0.0198(2) Uani 1 1 d . . . H50A H 0.364(2) 0.8490(14) 0.9052(8) 0.030 Uiso 1 1 d . . . C1A C 0.52433(16) 0.76495(11) 0.89820(6) 0.0152(2) Uani 1 1 d . . . C2A C 0.61723(16) 0.81610(11) 0.96714(6) 0.0150(2) Uani 1 1 d . . . C3A C 0.79167(16) 0.85300(11) 0.98475(6) 0.0172(3) Uani 1 1 d . . . H3A H 0.8578 0.8448 0.9529 0.021 Uiso 1 1 calc R . . C4A C 0.87262(16) 0.90138(11) 1.04719(7) 0.0185(3) Uani 1 1 d . . . H4A H 0.9921 0.9263 1.0574 0.022 Uiso 1 1 calc R . . C5A C 0.77834(16) 0.91321(11) 1.09466(6) 0.0172(3) Uani 1 1 d . . . C6A C 0.60348(16) 0.88068(11) 1.07906(6) 0.0162(2) Uani 1 1 d . . . H6A H 0.5382 0.8899 1.1111 0.019 Uiso 1 1 calc R . . C7A C 0.52588(16) 0.83432(11) 1.01560(6) 0.0153(2) Uani 1 1 d . . . C8A C 0.64199(16) 0.76709(11) 0.84888(6) 0.0154(2) Uani 1 1 d . . . C9A C 0.64391(16) 0.84264(11) 0.79932(6) 0.0173(3) Uani 1 1 d . . . H9A H 0.5773 0.8969 0.7984 0.021 Uiso 1 1 calc R . . C10A C 0.73997(16) 0.84140(12) 0.75112(6) 0.0178(3) Uani 1 1 d . . . H10A H 0.7392 0.8946 0.7182 0.021 Uiso 1 1 calc R . . C11A C 0.83682(16) 0.76205(11) 0.75144(6) 0.0166(3) Uani 1 1 d . . . C12A C 0.84278(16) 0.68748(11) 0.80101(6) 0.0172(3) Uani 1 1 d . . . H12A H 0.9123 0.6353 0.8021 0.021 Uiso 1 1 calc R . . C13A C 0.74550(16) 0.69003(11) 0.84917(6) 0.0159(2) Uani 1 1 d . . . C14A C 0.39704(15) 0.63179(11) 0.89280(6) 0.0148(2) Uani 1 1 d . . . C15A C 0.28680(16) 0.58519(12) 0.83448(6) 0.0191(3) Uani 1 1 d . . . H15A H 0.2942 0.6346 0.7997 0.023 Uiso 1 1 calc R . . C16A C 0.16630(17) 0.46749(12) 0.82649(6) 0.0208(3) Uani 1 1 d . . . H16A H 0.0913 0.4376 0.7867 0.025 Uiso 1 1 calc R . . C17A C 0.15561(17) 0.39384(12) 0.87657(7) 0.0197(3) Uani 1 1 d . . . H17A H 0.0737 0.3133 0.8712 0.024 Uiso 1 1 calc R . . C18A C 0.26506(17) 0.43841(12) 0.93445(7) 0.0196(3) Uani 1 1 d . . . H18A H 0.2589 0.3880 0.9688 0.024 Uiso 1 1 calc R . . C19A C 0.38477(16) 0.55744(11) 0.94248(6) 0.0174(3) Uani 1 1 d . . . H19A H 0.4586 0.5876 0.9825 0.021 Uiso 1 1 calc R . . C20A C 0.77985(18) 0.98024(13) 1.20493(6) 0.0228(3) Uani 1 1 d . . . H20A H 0.7221 1.0407 1.1929 0.034 Uiso 1 1 calc R . . H20B H 0.8596 1.0137 1.2453 0.034 Uiso 1 1 calc R . . H20C H 0.6966 0.9016 1.2108 0.034 Uiso 1 1 calc R . . C21A C 0.25312(17) 0.81746(14) 1.04327(7) 0.0240(3) Uani 1 1 d . . . H21A H 0.2671 0.7646 1.0772 0.036 Uiso 1 1 calc R . . H21B H 0.1344 0.7917 1.0228 0.036 Uiso 1 1 calc R . . H21C H 0.2883 0.9049 1.0622 0.036 Uiso 1 1 calc R . . C22A C 1.04551(18) 0.70007(13) 0.70376(7) 0.0248(3) Uani 1 1 d . . . H22A H 1.1314 0.7358 0.7422 0.037 Uiso 1 1 calc R . . H22B H 1.0987 0.7105 0.6653 0.037 Uiso 1 1 calc R . . H22C H 0.9914 0.6109 0.7060 0.037 Uiso 1 1 calc R . . C23A C 0.86563(18) 0.55264(13) 0.90612(7) 0.0228(3) Uani 1 1 d . . . H23A H 0.8436 0.4910 0.8684 0.034 Uiso 1 1 calc R . . H23B H 0.8567 0.5100 0.9450 0.034 Uiso 1 1 calc R . . H23C H 0.9794 0.6121 0.9099 0.034 Uiso 1 1 calc R . . O1B O 0.72271(12) 0.03312(9) 0.35891(5) 0.0238(2) Uani 1 1 d . . . O2B O 1.20533(11) 0.21576(8) 0.52023(5) 0.0208(2) Uani 1 1 d . . . O3B O 0.61849(12) 0.27399(9) 0.80773(4) 0.0214(2) Uani 1 1 d . . . O4B O 0.79666(12) 0.40000(8) 0.60674(4) 0.01885(19) Uani 1 1 d . . . O5B O 1.12825(12) 0.18613(8) 0.64216(5) 0.0201(2) Uani 1 1 d . . . H50B H 1.197(2) 0.1794(14) 0.6163(8) 0.030 Uiso 1 1 d . . . C1B C 1.02710(16) 0.25893(11) 0.61506(6) 0.0153(2) Uani 1 1 d . . . C2B C 0.93747(16) 0.19585(11) 0.54751(6) 0.0150(2) Uani 1 1 d . . . C3B C 0.76399(16) 0.15098(11) 0.52954(6) 0.0164(3) Uani 1 1 d . . . H3B H 0.6961 0.1592 0.5607 0.020 Uiso 1 1 calc R . . C4B C 0.68401(16) 0.09409(11) 0.46753(6) 0.0165(3) Uani 1 1 d . . . H4B H 0.5645 0.0640 0.4569 0.020 Uiso 1 1 calc R . . C5B C 0.78283(16) 0.08256(11) 0.42188(6) 0.0171(3) Uani 1 1 d . . . C6B C 0.95826(16) 0.12260(11) 0.43834(6) 0.0183(3) Uani 1 1 d . . . H6B H 1.0255 0.1125 0.4072 0.022 Uiso 1 1 calc R . . C7B C 1.03356(15) 0.17705(11) 0.50023(6) 0.0160(2) Uani 1 1 d . . . C8B C 0.90632(16) 0.26061(11) 0.66296(6) 0.0149(2) Uani 1 1 d . . . C9B C 0.90582(16) 0.19090(11) 0.71516(6) 0.0163(2) Uani 1 1 d . . . H9B H 0.9748 0.1383 0.7184 0.020 Uiso 1 1 calc R . . C10B C 0.80831(16) 0.19546(11) 0.76252(6) 0.0169(3) Uani 1 1 d . . . H10B H 0.8102 0.1463 0.7972 0.020 Uiso 1 1 calc R . . C11B C 0.70834(16) 0.27270(11) 0.75847(6) 0.0163(3) Uani 1 1 d . . . C12B C 0.70160(16) 0.34221(11) 0.70671(6) 0.0163(2) Uani 1 1 d . . . H12B H 0.6311 0.3936 0.7037 0.020 Uiso 1 1 calc R . . C13B C 0.79964(16) 0.33559(11) 0.65925(6) 0.0152(2) Uani 1 1 d . . . C14B C 1.14510(15) 0.39367(11) 0.61488(6) 0.0153(2) Uani 1 1 d . . . C15B C 1.26308(16) 0.44862(12) 0.67000(6) 0.0197(3) Uani 1 1 d . . . H15B H 1.2669 0.4035 0.7062 0.024 Uiso 1 1 calc R . . C16B C 1.37558(17) 0.56838(12) 0.67302(7) 0.0220(3) Uani 1 1 d . . . H16B H 1.4564 0.6042 0.7109 0.026 Uiso 1 1 calc R . . C17B C 1.36943(17) 0.63520(12) 0.62070(7) 0.0217(3) Uani 1 1 d . . . H17B H 1.4464 0.7170 0.6225 0.026 Uiso 1 1 calc R . . C18B C 1.25079(17) 0.58264(12) 0.56561(7) 0.0213(3) Uani 1 1 d . . . H18B H 1.2454 0.6287 0.5298 0.026 Uiso 1 1 calc R . . C19B C 1.13911(17) 0.46158(12) 0.56294(6) 0.0182(3) Uani 1 1 d . . . H19B H 1.0583 0.4256 0.5251 0.022 Uiso 1 1 calc R . . C20B C 0.54598(18) -0.00915(13) 0.33828(7) 0.0261(3) Uani 1 1 d . . . H20D H 0.4946 -0.0798 0.3611 0.039 Uiso 1 1 calc R . . H20E H 0.5206 -0.0357 0.2918 0.039 Uiso 1 1 calc R . . H20F H 0.5003 0.0588 0.3476 0.039 Uiso 1 1 calc R . . C21B C 1.30741(17) 0.20567(13) 0.47300(7) 0.0239(3) Uani 1 1 d . . . H21D H 1.2820 0.1176 0.4567 0.036 Uiso 1 1 calc R . . H21E H 1.4267 0.2404 0.4926 0.036 Uiso 1 1 calc R . . H21F H 1.2836 0.2522 0.4373 0.036 Uiso 1 1 calc R . . C22B C 0.50301(19) 0.34481(13) 0.80331(7) 0.0255(3) Uani 1 1 d . . . H22D H 0.5638 0.4319 0.7991 0.038 Uiso 1 1 calc R . . H22E H 0.4519 0.3413 0.8423 0.038 Uiso 1 1 calc R . . H22F H 0.4145 0.3096 0.7656 0.038 Uiso 1 1 calc R . . C23B C 0.68411(18) 0.47261(12) 0.59998(7) 0.0219(3) Uani 1 1 d . . . H23D H 0.5682 0.4182 0.5985 0.033 Uiso 1 1 calc R . . H23E H 0.6923 0.5118 0.5600 0.033 Uiso 1 1 calc R . . H23F H 0.7147 0.5375 0.6368 0.033 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 O1A 0.0189(5) 0.0323(5) 0.0193(5) -0.0055(4) 0.0006(4) 0.0073(4) O2A 0.0150(5) 0.0282(5) 0.0176(5) -0.0006(4) 0.0035(4) 0.0090(4) O3A 0.0234(5) 0.0270(5) 0.0171(5) 0.0061(4) 0.0093(4) 0.0107(4) O4A 0.0267(5) 0.0194(5) 0.0187(5) 0.0078(4) 0.0097(4) 0.0140(4) O5A 0.0249(5) 0.0211(5) 0.0207(5) 0.0064(4) 0.0082(4) 0.0153(4) C1A 0.0174(6) 0.0168(6) 0.0152(6) 0.0041(5) 0.0053(5) 0.0092(5) C2A 0.0177(6) 0.0118(5) 0.0168(6) 0.0021(5) 0.0053(5) 0.0054(5) C3A 0.0187(6) 0.0136(6) 0.0211(6) 0.0019(5) 0.0088(5) 0.0053(5) C4A 0.0143(6) 0.0167(6) 0.0239(7) 0.0012(5) 0.0038(5) 0.0042(5) C5A 0.0187(6) 0.0139(6) 0.0183(6) -0.0006(5) 0.0025(5) 0.0048(5) C6A 0.0171(6) 0.0159(6) 0.0169(6) 0.0015(5) 0.0054(5) 0.0060(5) C7A 0.0145(6) 0.0145(6) 0.0176(6) 0.0013(5) 0.0034(5) 0.0053(4) C8A 0.0178(6) 0.0145(6) 0.0145(6) 0.0011(5) 0.0050(5) 0.0052(5) C9A 0.0191(6) 0.0154(6) 0.0187(6) 0.0033(5) 0.0043(5) 0.0067(5) C10A 0.0202(7) 0.0169(6) 0.0164(6) 0.0050(5) 0.0043(5) 0.0050(5) C11A 0.0162(6) 0.0176(6) 0.0145(6) -0.0004(5) 0.0041(5) 0.0028(5) C12A 0.0202(6) 0.0162(6) 0.0173(6) 0.0017(5) 0.0055(5) 0.0077(5) C13A 0.0202(6) 0.0136(6) 0.0143(6) 0.0019(5) 0.0046(5) 0.0052(5) C14A 0.0148(6) 0.0170(6) 0.0152(6) 0.0021(5) 0.0041(5) 0.0079(5) C15A 0.0207(7) 0.0243(7) 0.0141(6) 0.0043(5) 0.0040(5) 0.0089(5) C16A 0.0180(6) 0.0267(7) 0.0156(6) -0.0021(5) -0.0001(5) 0.0062(5) C17A 0.0170(6) 0.0183(6) 0.0224(7) 0.0001(5) 0.0027(5) 0.0043(5) C18A 0.0219(7) 0.0185(6) 0.0195(6) 0.0043(5) 0.0040(5) 0.0071(5) C19A 0.0183(6) 0.0182(6) 0.0159(6) 0.0021(5) 0.0013(5) 0.0069(5) C20A 0.0260(7) 0.0250(7) 0.0170(6) -0.0017(5) 0.0017(5) 0.0091(6) C21A 0.0172(7) 0.0346(8) 0.0227(7) -0.0004(6) 0.0069(5) 0.0108(6) C22A 0.0273(8) 0.0296(7) 0.0235(7) 0.0049(6) 0.0117(6) 0.0142(6) C23A 0.0297(8) 0.0245(7) 0.0215(7) 0.0082(5) 0.0075(6) 0.0169(6) O1B 0.0194(5) 0.0306(5) 0.0179(5) -0.0060(4) 0.0018(4) 0.0055(4) O2B 0.0144(5) 0.0260(5) 0.0218(5) -0.0016(4) 0.0044(4) 0.0066(4) O3B 0.0244(5) 0.0271(5) 0.0167(5) 0.0062(4) 0.0089(4) 0.0109(4) O4B 0.0261(5) 0.0200(5) 0.0168(5) 0.0071(4) 0.0082(4) 0.0135(4) O5B 0.0221(5) 0.0228(5) 0.0208(5) 0.0057(4) 0.0050(4) 0.0138(4) C1B 0.0166(6) 0.0148(6) 0.0159(6) 0.0022(5) 0.0028(5) 0.0068(5) C2B 0.0179(6) 0.0120(5) 0.0163(6) 0.0022(4) 0.0039(5) 0.0062(5) C3B 0.0175(6) 0.0147(6) 0.0180(6) 0.0021(5) 0.0061(5) 0.0052(5) C4B 0.0156(6) 0.0145(6) 0.0193(6) 0.0016(5) 0.0038(5) 0.0041(5) C5B 0.0198(6) 0.0142(6) 0.0170(6) 0.0001(5) 0.0037(5) 0.0050(5) C6B 0.0193(7) 0.0195(6) 0.0181(6) 0.0011(5) 0.0067(5) 0.0078(5) C7B 0.0143(6) 0.0154(6) 0.0196(6) 0.0022(5) 0.0050(5) 0.0057(5) C8B 0.0167(6) 0.0134(6) 0.0143(6) 0.0008(4) 0.0027(5) 0.0046(5) C9B 0.0171(6) 0.0136(6) 0.0176(6) 0.0024(5) 0.0014(5) 0.0047(5) C10B 0.0174(6) 0.0151(6) 0.0157(6) 0.0032(5) 0.0014(5) 0.0018(5) C11B 0.0170(6) 0.0156(6) 0.0139(6) 0.0004(5) 0.0033(5) 0.0018(5) C12B 0.0187(6) 0.0151(6) 0.0163(6) 0.0010(5) 0.0035(5) 0.0072(5) C13B 0.0194(6) 0.0128(6) 0.0126(6) 0.0016(4) 0.0025(5) 0.0041(5) C14B 0.0150(6) 0.0155(6) 0.0169(6) 0.0011(5) 0.0047(5) 0.0062(5) C15B 0.0185(6) 0.0233(7) 0.0166(6) 0.0019(5) 0.0025(5) 0.0059(5) C16B 0.0172(6) 0.0251(7) 0.0203(7) -0.0041(5) 0.0012(5) 0.0042(5) C17B 0.0199(7) 0.0168(6) 0.0268(7) -0.0007(5) 0.0076(6) 0.0026(5) C18B 0.0253(7) 0.0173(6) 0.0223(7) 0.0044(5) 0.0073(6) 0.0063(5) C19B 0.0201(6) 0.0175(6) 0.0164(6) 0.0006(5) 0.0013(5) 0.0063(5) C20B 0.0214(7) 0.0277(7) 0.0232(7) -0.0048(6) -0.0006(6) 0.0025(6) C21B 0.0179(7) 0.0278(7) 0.0280(8) 0.0016(6) 0.0103(6) 0.0076(5) C22B 0.0311(8) 0.0285(7) 0.0243(7) 0.0066(6) 0.0132(6) 0.0158(6) C23B 0.0302(8) 0.0232(7) 0.0193(7) 0.0070(5) 0.0062(6) 0.0169(6) _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 O1A C5A 1.3693(16) . ? O1A C20A 1.4281(16) . ? O2A C7A 1.3756(15) . ? O2A C21A 1.4310(15) . ? O3A C11A 1.3725(15) . ? O3A C22A 1.4298(16) . ? O4A C13A 1.3703(15) . ? O4A C23A 1.4310(15) . ? O5A C1A 1.4516(15) . ? O5A H50A 0.876(17) . ? C1A C8A 1.5346(17) . ? C1A C2A 1.5347(18) . ? C1A C14A 1.5480(17) . ? C2A C3A 1.3907(18) . ? C2A C7A 1.4059(17) . ? C3A C4A 1.3871(18) . ? C3A H3A 0.9500 . ? C4A C5A 1.3891(18) . ? C4A H4A 0.9500 . ? C5A C6A 1.3933(18) . ? C6A C7A 1.3951(18) . ? C6A H6A 0.9500 . ? C8A C9A 1.3939(17) . ? C8A C13A 1.4095(17) . ? C9A C10A 1.3904(17) . ? C9A H9A 0.9500 . ? C10A C11A 1.3858(18) . ? C10A H10A 0.9500 . ? C11A C12A 1.3928(18) . ? C12A C13A 1.3989(17) . ? C12A H12A 0.9500 . ? C14A C19A 1.3838(17) . ? C14A C15A 1.3965(18) . ? C15A C16A 1.3911(18) . ? C15A H15A 0.9500 . ? C16A C17A 1.3858(19) . ? C16A H16A 0.9500 . ? C17A C18A 1.3838(19) . ? C17A H17A 0.9500 . ? C18A C19A 1.3992(18) . ? C18A H18A 0.9500 . ? C19A H19A 0.9500 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? O1B C5B 1.3688(15) . ? O1B C20B 1.4145(17) . ? O2B C7B 1.3751(15) . ? O2B C21B 1.4279(15) . ? O3B C11B 1.3734(15) . ? O3B C22B 1.4357(16) . ? O4B C13B 1.3684(15) . ? O4B C23B 1.4320(15) . ? O5B C1B 1.4450(15) . ? O5B H50B 0.866(17) . ? C1B C2B 1.5311(17) . ? C1B C8B 1.5381(17) . ? C1B C14B 1.5478(17) . ? C2B C3B 1.3834(18) . ? C2B C7B 1.4165(17) . ? C3B C4B 1.3984(18) . ? C3B H3B 0.9500 . ? C4B C5B 1.3857(17) . ? C4B H4B 0.9500 . ? C5B C6B 1.3953(18) . ? C6B C7B 1.3814(18) . ? C6B H6B 0.9500 . ? C8B C9B 1.3974(17) . ? C8B C13B 1.4109(17) . ? C9B C10B 1.3905(17) . ? C9B H9B 0.9500 . ? C10B C11B 1.3862(18) . ? C10B H10B 0.9500 . ? C11B C12B 1.3934(18) . ? C12B C13B 1.3993(17) . ? C12B H12B 0.9500 . ? C14B C19B 1.3846(18) . ? C14B C15B 1.3894(18) . ? C15B C16B 1.3898(18) . ? C15B H15B 0.9500 . ? C16B C17B 1.384(2) . ? C16B H16B 0.9500 . ? C17B C18B 1.387(2) . ? C17B H17B 0.9500 . ? C18B C19B 1.3994(18) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 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 C5A O1A C20A 117.85(10) . . ? C7A O2A C21A 118.46(10) . . ? C11A O3A C22A 118.01(10) . . ? C13A O4A C23A 117.81(10) . . ? C1A O5A H50A 106.2(11) . . ? O5A C1A C8A 104.73(10) . . ? O5A C1A C2A 107.97(9) . . ? C8A C1A C2A 113.86(10) . . ? O5A C1A C14A 107.25(10) . . ? C8A C1A C14A 108.98(10) . . ? C2A C1A C14A 113.47(10) . . ? C3A C2A C7A 116.49(12) . . ? C3A C2A C1A 123.55(11) . . ? C7A C2A C1A 119.86(11) . . ? C4A C3A C2A 122.35(11) . . ? C4A C3A H3A 118.8 . . ? C2A C3A H3A 118.8 . . ? C3A C4A C5A 119.78(12) . . ? C3A C4A H4A 120.1 . . ? C5A C4A H4A 120.1 . . ? O1A C5A C4A 115.48(12) . . ? O1A C5A C6A 124.49(11) . . ? C4A C5A C6A 120.03(12) . . ? C5A C6A C7A 118.85(11) . . ? C5A C6A H6A 120.6 . . ? C7A C6A H6A 120.6 . . ? O2A C7A C6A 122.15(11) . . ? O2A C7A C2A 115.44(11) . . ? C6A C7A C2A 122.41(12) . . ? C9A C8A C13A 117.01(11) . . ? C9A C8A C1A 120.32(11) . . ? C13A C8A C1A 122.59(11) . . ? C10A C9A C8A 122.31(12) . . ? C10A C9A H9A 118.8 . . ? C8A C9A H9A 118.8 . . ? C11A C10A C9A 119.54(12) . . ? C11A C10A H10A 120.2 . . ? C9A C10A H10A 120.2 . . ? O3A C11A C10A 115.60(11) . . ? O3A C11A C12A 124.19(12) . . ? C10A C11A C12A 120.21(11) . . ? C11A C12A C13A 119.45(12) . . ? C11A C12A H12A 120.3 . . ? C13A C12A H12A 120.3 . . ? O4A C13A C12A 122.30(11) . . ? O4A C13A C8A 116.27(10) . . ? C12A C13A C8A 121.43(12) . . ? C19A C14A C15A 118.37(12) . . ? C19A C14A C1A 123.91(11) . . ? C15A C14A C1A 117.71(11) . . ? C16A C15A C14A 121.02(12) . . ? C16A C15A H15A 119.5 . . ? C14A C15A H15A 119.5 . . ? C17A C16A C15A 120.03(12) . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C18A C17A C16A 119.55(12) . . ? C18A C17A H17A 120.2 . . ? C16A C17A H17A 120.2 . . ? C17A C18A C19A 120.19(12) . . ? C17A C18A H18A 119.9 . . ? C19A C18A H18A 119.9 . . ? C14A C19A C18A 120.83(12) . . ? C14A C19A H19A 119.6 . . ? C18A C19A H19A 119.6 . . ? O1A C20A H20A 109.5 . . ? O1A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? O1A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? O2A C21A H21A 109.5 . . ? O2A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? O2A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? O3A C22A H22A 109.5 . . ? O3A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? O3A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? O4A C23A H23A 109.5 . . ? O4A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? O4A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C5B O1B C20B 117.87(10) . . ? C7B O2B C21B 117.35(10) . . ? C11B O3B C22B 117.87(10) . . ? C13B O4B C23B 117.87(10) . . ? C1B O5B H50B 108.7(11) . . ? O5B C1B C2B 108.36(9) . . ? O5B C1B C8B 104.41(10) . . ? C2B C1B C8B 113.71(10) . . ? O5B C1B C14B 108.01(10) . . ? C2B C1B C14B 112.91(10) . . ? C8B C1B C14B 108.94(9) . . ? C3B C2B C7B 116.56(11) . . ? C3B C2B C1B 123.67(11) . . ? C7B C2B C1B 119.74(11) . . ? C2B C3B C4B 122.98(11) . . ? C2B C3B H3B 118.5 . . ? C4B C3B H3B 118.5 . . ? C5B C4B C3B 118.58(12) . . ? C5B C4B H4B 120.7 . . ? C3B C4B H4B 120.7 . . ? O1B C5B C4B 125.14(12) . . ? O1B C5B C6B 114.37(11) . . ? C4B C5B C6B 120.49(12) . . ? C7B C6B C5B 119.55(11) . . ? C7B C6B H6B 120.2 . . ? C5B C6B H6B 120.2 . . ? O2B C7B C6B 122.66(11) . . ? O2B C7B C2B 115.59(11) . . ? C6B C7B C2B 121.74(12) . . ? C9B C8B C13B 116.92(11) . . ? C9B C8B C1B 119.91(11) . . ? C13B C8B C1B 123.07(11) . . ? C10B C9B C8B 122.58(12) . . ? C10B C9B H9B 118.7 . . ? C8B C9B H9B 118.7 . . ? C11B C10B C9B 119.12(12) . . ? C11B C10B H10B 120.4 . . ? C9B C10B H10B 120.4 . . ? O3B C11B C10B 115.64(11) . . ? O3B C11B C12B 123.77(12) . . ? C10B C11B C12B 120.58(11) . . ? C11B C12B C13B 119.42(12) . . ? C11B C12B H12B 120.3 . . ? C13B C12B H12B 120.3 . . ? O4B C13B C12B 122.24(11) . . ? O4B C13B C8B 116.42(11) . . ? C12B C13B C8B 121.34(11) . . ? C19B C14B C15B 118.66(11) . . ? C19B C14B C1B 123.53(11) . . ? C15B C14B C1B 117.81(11) . . ? C14B C15B C16B 121.16(13) . . ? C14B C15B H15B 119.4 . . ? C16B C15B H15B 119.4 . . ? C17B C16B C15B 119.76(13) . . ? C17B C16B H16B 120.1 . . ? C15B C16B H16B 120.1 . . ? C16B C17B C18B 119.93(12) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C19B 119.79(13) . . ? C17B C18B H18B 120.1 . . ? C19B C18B H18B 120.1 . . ? C14B C19B C18B 120.70(12) . . ? C14B C19B H19B 119.7 . . ? C18B C19B H19B 119.7 . . ? O1B C20B H20D 109.5 . . ? O1B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? O1B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O2B C21B H21D 109.5 . . ? O2B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? O2B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? O3B C22B H22D 109.5 . . ? O3B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? O3B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? O4B C23B H23D 109.5 . . ? O4B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? O4B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? 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 O5A C1A C2A C3A -120.18(12) . . . . ? C8A C1A C2A C3A -4.34(16) . . . . ? C14A C1A C2A C3A 121.09(13) . . . . ? O5A C1A C2A C7A 56.17(14) . . . . ? C8A C1A C2A C7A 172.01(11) . . . . ? C14A C1A C2A C7A -62.56(14) . . . . ? C7A C2A C3A C4A 2.16(18) . . . . ? C1A C2A C3A C4A 178.62(11) . . . . ? C2A C3A C4A C5A 0.55(19) . . . . ? C20A O1A C5A C4A 175.76(11) . . . . ? C20A O1A C5A C6A -4.03(18) . . . . ? C3A C4A C5A O1A 177.94(11) . . . . ? C3A C4A C5A C6A -2.26(18) . . . . ? O1A C5A C6A C7A -179.07(12) . . . . ? C4A C5A C6A C7A 1.15(18) . . . . ? C21A O2A C7A C6A -2.44(17) . . . . ? C21A O2A C7A C2A 178.25(11) . . . . ? C5A C6A C7A O2A -177.55(11) . . . . ? C5A C6A C7A C2A 1.71(18) . . . . ? C3A C2A C7A O2A 176.01(11) . . . . ? C1A C2A C7A O2A -0.59(16) . . . . ? C3A C2A C7A C6A -3.31(18) . . . . ? C1A C2A C7A C6A -179.91(11) . . . . ? O5A C1A C8A C9A 2.66(15) . . . . ? C2A C1A C8A C9A -115.06(13) . . . . ? C14A C1A C8A C9A 117.16(12) . . . . ? O5A C1A C8A C13A -174.14(11) . . . . ? C2A C1A C8A C13A 68.14(15) . . . . ? C14A C1A C8A C13A -59.64(16) . . . . ? C13A C8A C9A C10A 1.35(19) . . . . ? C1A C8A C9A C10A -175.62(12) . . . . ? C8A C9A C10A C11A 0.52(19) . . . . ? C22A O3A C11A C10A 169.34(11) . . . . ? C22A O3A C11A C12A -11.16(18) . . . . ? C9A C10A C11A O3A 177.15(11) . . . . ? C9A C10A C11A C12A -2.38(19) . . . . ? O3A C11A C12A C13A -177.19(11) . . . . ? C10A C11A C12A C13A 2.30(19) . . . . ? C23A O4A C13A C12A 8.95(18) . . . . ? C23A O4A C13A C8A -171.21(11) . . . . ? C11A C12A C13A O4A 179.47(11) . . . . ? C11A C12A C13A C8A -0.36(19) . . . . ? C9A C8A C13A O4A 178.74(11) . . . . ? C1A C8A C13A O4A -4.36(18) . . . . ? C9A C8A C13A C12A -1.42(18) . . . . ? C1A C8A C13A C12A 175.47(11) . . . . ? O5A C1A C14A C19A -128.48(12) . . . . ? C8A C1A C14A C19A 118.66(13) . . . . ? C2A C1A C14A C19A -9.34(17) . . . . ? O5A C1A C14A C15A 50.58(14) . . . . ? C8A C1A C14A C15A -62.27(14) . . . . ? C2A C1A C14A C15A 169.73(11) . . . . ? C19A C14A C15A C16A 0.64(19) . . . . ? C1A C14A C15A C16A -178.48(11) . . . . ? C14A C15A C16A C17A -0.8(2) . . . . ? C15A C16A C17A C18A 0.2(2) . . . . ? C16A C17A C18A C19A 0.5(2) . . . . ? C15A C14A C19A C18A 0.10(19) . . . . ? C1A C14A C19A C18A 179.16(11) . . . . ? C17A C18A C19A C14A -0.68(19) . . . . ? O5B C1B C2B C3B 119.33(13) . . . . ? C8B C1B C2B C3B 3.72(17) . . . . ? C14B C1B C2B C3B -121.07(13) . . . . ? O5B C1B C2B C7B -58.41(14) . . . . ? C8B C1B C2B C7B -174.03(11) . . . . ? C14B C1B C2B C7B 61.19(15) . . . . ? C7B C2B C3B C4B -2.50(18) . . . . ? C1B C2B C3B C4B 179.69(11) . . . . ? C2B C3B C4B C5B -0.28(19) . . . . ? C20B O1B C5B C4B 0.36(18) . . . . ? C20B O1B C5B C6B -179.71(11) . . . . ? C3B C4B C5B O1B -177.63(12) . . . . ? C3B C4B C5B C6B 2.45(18) . . . . ? O1B C5B C6B C7B 178.38(11) . . . . ? C4B C5B C6B C7B -1.69(19) . . . . ? C21B O2B C7B C6B 4.21(17) . . . . ? C21B O2B C7B C2B -176.19(11) . . . . ? C5B C6B C7B O2B 178.31(11) . . . . ? C5B C6B C7B C2B -1.27(19) . . . . ? C3B C2B C7B O2B -176.33(11) . . . . ? C1B C2B C7B O2B 1.57(16) . . . . ? C3B C2B C7B C6B 3.28(18) . . . . ? C1B C2B C7B C6B -178.82(11) . . . . ? O5B C1B C8B C9B -4.89(14) . . . . ? C2B C1B C8B C9B 113.02(13) . . . . ? C14B C1B C8B C9B -120.09(12) . . . . ? O5B C1B C8B C13B 171.47(11) . . . . ? C2B C1B C8B C13B -70.61(14) . . . . ? C14B C1B C8B C13B 56.28(15) . . . . ? C13B C8B C9B C10B -1.22(18) . . . . ? C1B C8B C9B C10B 175.37(11) . . . . ? C8B C9B C10B C11B -0.54(19) . . . . ? C22B O3B C11B C10B -175.25(11) . . . . ? C22B O3B C11B C12B 4.17(18) . . . . ? C9B C10B C11B O3B -178.72(11) . . . . ? C9B C10B C11B C12B 1.85(18) . . . . ? O3B C11B C12B C13B 179.26(11) . . . . ? C10B C11B C12B C13B -1.35(18) . . . . ? C23B O4B C13B C12B -2.20(17) . . . . ? C23B O4B C13B C8B 177.27(11) . . . . ? C11B C12B C13B O4B 178.96(11) . . . . ? C11B C12B C13B C8B -0.48(18) . . . . ? C9B C8B C13B O4B -177.76(11) . . . . ? C1B C8B C13B O4B 5.78(17) . . . . ? C9B C8B C13B C12B 1.72(18) . . . . ? C1B C8B C13B C12B -174.75(11) . . . . ? O5B C1B C14B C19B 135.30(12) . . . . ? C2B C1B C14B C19B 15.50(17) . . . . ? C8B C1B C14B C19B -111.85(13) . . . . ? O5B C1B C14B C15B -44.64(14) . . . . ? C2B C1B C14B C15B -164.44(11) . . . . ? C8B C1B C14B C15B 68.21(14) . . . . ? C19B C14B C15B C16B -1.22(19) . . . . ? C1B C14B C15B C16B 178.72(11) . . . . ? C14B C15B C16B C17B 0.8(2) . . . . ? C15B C16B C17B C18B 0.2(2) . . . . ? C16B C17B C18B C19B -0.8(2) . . . . ? C15B C14B C19B C18B 0.67(19) . . . . ? C1B C14B C19B C18B -179.26(11) . . . . ? C17B C18B C19B C14B 0.3(2) . . . . ? 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 O5A H50A O2A 0.876(17) 2.022(17) 2.7194(14) 135.8(15) . O5B H50B O2B 0.866(17) 2.103(17) 2.7608(14) 132.3(15) . _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 32.6 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.37 _refine_diff_density_min -0.33 _refine_diff_density_rms 0.059 # END OF CIF