data_cu_rxc189_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H50 O7, C3 H6 O' _chemical_formula_sum 'C41 H56 O8' _chemical_formula_weight 676.86 _chemical_absolute_configuration ad 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4439(3) _cell_length_b 21.1595(6) _cell_length_c 10.6994(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.5300(10) _cell_angle_gamma 90.00 _cell_volume 1822.87(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 4.18 _cell_measurement_theta_max 69.21 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7554 _exptl_absorpt_correction_T_max 0.9055 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16831 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 69.66 _reflns_number_total 5988 _reflns_number_gt 5871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0632P)^2^+0.3520P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(12) _refine_ls_number_reflns 5988 _refine_ls_number_parameters 455 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _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 O10 O 0.97349(16) 0.60179(7) 0.40620(12) 0.0239(3) Uani 1 1 d . . . O4 O 0.42791(14) 0.65670(6) -0.02674(12) 0.0160(3) Uani 1 1 d . . . H4 H 0.3400 0.6778 -0.0546 0.024 Uiso 1 1 calc R . . O20 O 0.51426(14) 0.73411(6) -0.14823(11) 0.0151(3) Uani 1 1 d . . . O19 O 0.42045(14) 0.69862(6) -0.26488(11) 0.0174(3) Uani 1 1 d . . . O34 O 1.13137(14) 0.72069(6) -0.12867(11) 0.0161(3) Uani 1 1 d . . . H34 H 1.1173 0.7600 -0.1299 0.024 Uiso 1 1 calc R . . O2 O 0.77335(15) 0.54976(6) 0.07974(12) 0.0186(3) Uani 1 1 d . . . O9 O 0.62589(15) 0.70311(6) 0.29444(12) 0.0192(3) Uani 1 1 d . . . O40 O 0.06460(19) 0.84999(7) 0.84511(14) 0.0309(3) Uani 1 1 d . . . C14 C 0.4641(3) 0.48426(10) 0.3952(2) 0.0276(4) Uani 1 1 d . . . H14 H 0.3833 0.4573 0.4127 0.033 Uiso 1 1 calc R . . C15 C 0.4244(2) 0.51987(10) 0.28069(19) 0.0227(4) Uani 1 1 d . . . H15 H 0.3163 0.5171 0.2199 0.027 Uiso 1 1 calc R . . C16 C 0.5415(2) 0.55926(9) 0.25494(18) 0.0193(4) Uani 1 1 d . . . H16 H 0.5131 0.5837 0.1768 0.023 Uiso 1 1 calc R . . C11 C 0.7006(2) 0.56333(9) 0.34266(17) 0.0178(4) Uani 1 1 d . . . C10 C 0.8390(2) 0.60366(9) 0.32497(16) 0.0171(4) Uani 1 1 d . . . C1 C 0.8084(2) 0.64639(9) 0.20252(16) 0.0149(4) Uani 1 1 d . . . C9 C 0.67807(19) 0.69666(8) 0.20165(16) 0.0137(3) Uani 1 1 d . . . C5 C 0.6264(2) 0.73859(9) 0.07957(16) 0.0143(4) Uani 1 1 d . . . C22 C 0.4919(2) 0.78576(9) 0.08909(17) 0.0165(4) Uani 1 1 d . . . H22A H 0.4459 0.8070 0.0033 0.020 Uiso 1 1 calc R . . H22B H 0.4004 0.7622 0.1080 0.020 Uiso 1 1 calc R . . C23 C 0.5554(2) 0.83519(9) 0.19317(18) 0.0173(4) Uani 1 1 d . . . H23 H 0.5970 0.8205 0.2809 0.021 Uiso 1 1 calc R . . C24 C 0.5594(2) 0.89750(9) 0.17520(18) 0.0188(4) Uani 1 1 d . . . C26 C 0.6271(2) 0.94095(10) 0.2900(2) 0.0238(4) Uani 1 1 d . . . H26A H 0.6619 0.9153 0.3711 0.029 Uiso 1 1 calc R . . H26B H 0.5371 0.9695 0.2966 0.029 Uiso 1 1 calc R . . C27 C 0.7755(2) 0.98132(10) 0.2819(2) 0.0246(4) Uani 1 1 d . . . H27A H 0.7409 1.0074 0.2014 0.030 Uiso 1 1 calc R . . H27B H 0.8078 1.0104 0.3579 0.030 Uiso 1 1 calc R . . C28 C 0.9238(2) 0.94225(10) 0.2805(2) 0.0243(4) Uani 1 1 d . . . H28 H 0.9750 0.9190 0.3581 0.029 Uiso 1 1 calc R . . C29 C 0.9924(2) 0.93620(10) 0.1842(2) 0.0257(4) Uani 1 1 d . . . C30 C 1.1414(3) 0.89458(12) 0.1989(2) 0.0356(5) Uani 1 1 d . . . H30A H 1.1712 0.8737 0.2846 0.053 Uiso 1 1 calc R . . H30B H 1.2350 0.9204 0.1923 0.053 Uiso 1 1 calc R . . H30C H 1.1151 0.8626 0.1295 0.053 Uiso 1 1 calc R . . C13 C 0.6218(3) 0.48819(10) 0.48357(19) 0.0258(4) Uani 1 1 d . . . H13 H 0.6491 0.4642 0.5622 0.031 Uiso 1 1 calc R . . C12 C 0.7392(2) 0.52683(9) 0.45757(18) 0.0213(4) Uani 1 1 d . . . H12 H 0.8476 0.5288 0.5181 0.026 Uiso 1 1 calc R . . C8 C 0.9700(2) 0.68559(9) 0.19735(16) 0.0151(4) Uani 1 1 d . . . C7 C 0.9188(2) 0.72409(9) 0.06716(16) 0.0148(3) Uani 1 1 d . . . H7 H 1.0185 0.7474 0.0595 0.018 Uiso 1 1 calc R . . C6 C 0.7831(2) 0.77200(9) 0.06428(17) 0.0146(3) Uani 1 1 d . . . H6A H 0.7535 0.7954 -0.0197 0.018 Uiso 1 1 calc R . . H6B H 0.8249 0.8029 0.1363 0.018 Uiso 1 1 calc R . . C31 C 0.9333(3) 0.96837(11) 0.0530(2) 0.0340(5) Uani 1 1 d . . . H31A H 0.8390 0.9959 0.0505 0.051 Uiso 1 1 calc R . . H31B H 0.8985 0.9365 -0.0162 0.051 Uiso 1 1 calc R . . H31C H 1.0237 0.9938 0.0393 0.051 Uiso 1 1 calc R . . C25 C 0.4954(3) 0.92859(10) 0.0430(2) 0.0295(5) Uani 1 1 d . . . H25A H 0.5857 0.9321 0.0035 0.044 Uiso 1 1 calc R . . H25B H 0.4534 0.9708 0.0532 0.044 Uiso 1 1 calc R . . H25C H 0.4054 0.9030 -0.0138 0.044 Uiso 1 1 calc R . . C4 C 0.5613(2) 0.69223(8) -0.03851(16) 0.0137(3) Uani 1 1 d . . . C19 C 0.5258(2) 0.69069(9) -0.34891(17) 0.0180(4) Uani 1 1 d . . . C20 C 0.5461(2) 0.75429(10) -0.40906(18) 0.0229(4) Uani 1 1 d . . . H20A H 0.4370 0.7700 -0.4611 0.034 Uiso 1 1 calc R . . H20B H 0.6175 0.7493 -0.4656 0.034 Uiso 1 1 calc R . . H20C H 0.5969 0.7845 -0.3391 0.034 Uiso 1 1 calc R . . C18 C 0.6889(2) 0.65722(9) -0.27379(16) 0.0164(4) Uani 1 1 d . . . H18 H 0.7292 0.6334 -0.3390 0.020 Uiso 1 1 calc R . . C33 C 0.8358(2) 0.69898(9) -0.19019(16) 0.0143(3) Uani 1 1 d . . . H33 H 0.8008 0.7443 -0.1996 0.017 Uiso 1 1 calc R . . C34 C 0.9973(2) 0.69174(9) -0.22935(16) 0.0159(4) Uani 1 1 d . . . C36 C 1.0533(2) 0.62385(9) -0.23457(19) 0.0195(4) Uani 1 1 d . . . H36A H 1.1541 0.6232 -0.2620 0.029 Uiso 1 1 calc R . . H36B H 0.9653 0.5999 -0.2975 0.029 Uiso 1 1 calc R . . H36C H 1.0768 0.6046 -0.1475 0.029 Uiso 1 1 calc R . . C35 C 0.9795(2) 0.72336(10) -0.36114(17) 0.0209(4) Uani 1 1 d . . . H35A H 0.9463 0.7676 -0.3577 0.031 Uiso 1 1 calc R . . H35B H 0.8948 0.7012 -0.4302 0.031 Uiso 1 1 calc R . . H35C H 1.0860 0.7217 -0.3801 0.031 Uiso 1 1 calc R . . C32 C 0.86183(19) 0.67810(8) -0.04776(16) 0.0136(3) Uani 1 1 d . . . H32 H 0.9480 0.6441 -0.0302 0.016 Uiso 1 1 calc R . . C3 C 0.6983(2) 0.64495(8) -0.04692(16) 0.0139(3) Uani 1 1 d . . . C2 C 0.75356(19) 0.60642(9) 0.07695(16) 0.0139(4) Uani 1 1 d . . . C17 C 0.6549(2) 0.60865(9) -0.17652(16) 0.0164(4) Uani 1 1 d . . . H17A H 0.5370 0.5954 -0.2043 0.020 Uiso 1 1 calc R . . H17B H 0.7260 0.5708 -0.1691 0.020 Uiso 1 1 calc R . . C21 C 0.4199(2) 0.64675(11) -0.45411(18) 0.0244(4) Uani 1 1 d . . . H21A H 0.4182 0.6045 -0.4169 0.037 Uiso 1 1 calc R . . H21B H 0.4671 0.6442 -0.5272 0.037 Uiso 1 1 calc R . . H21C H 0.3064 0.6633 -0.4858 0.037 Uiso 1 1 calc R . . C38 C 1.0270(2) 0.73119(10) 0.31417(17) 0.0187(4) Uani 1 1 d . . . H38A H 1.0623 0.7069 0.3959 0.028 Uiso 1 1 calc R . . H38B H 0.9348 0.7591 0.3154 0.028 Uiso 1 1 calc R . . H38C H 1.1202 0.7566 0.3057 0.028 Uiso 1 1 calc R . . C37 C 1.1160(2) 0.64088(9) 0.20140(18) 0.0191(4) Uani 1 1 d . . . H37A H 1.1952 0.6627 0.1657 0.029 Uiso 1 1 calc R . . H37B H 1.0737 0.6031 0.1488 0.029 Uiso 1 1 calc R . . H37C H 1.1717 0.6284 0.2923 0.029 Uiso 1 1 calc R . . C39 C 0.2374(3) 0.86625(12) 0.7091(2) 0.0347(5) Uani 1 1 d . . . H39A H 0.2940 0.8282 0.7526 0.052 Uiso 1 1 calc R . . H39B H 0.3162 0.9015 0.7252 0.052 Uiso 1 1 calc R . . H39C H 0.1933 0.8586 0.6146 0.052 Uiso 1 1 calc R . . C40 C 0.0976(2) 0.88225(9) 0.76248(19) 0.0234(4) Uani 1 1 d . . . C41 C -0.0006(3) 0.94001(11) 0.7104(2) 0.0310(5) Uani 1 1 d . . . H41A H -0.1038 0.9396 0.7344 0.047 Uiso 1 1 calc R . . H41B H -0.0271 0.9409 0.6147 0.047 Uiso 1 1 calc R . . H41C H 0.0644 0.9776 0.7477 0.047 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 O10 0.0207(6) 0.0299(7) 0.0183(6) 0.0056(6) 0.0015(5) -0.0013(6) O4 0.0118(5) 0.0211(6) 0.0165(6) -0.0006(5) 0.0065(4) 0.0004(5) O20 0.0160(6) 0.0201(6) 0.0088(6) -0.0004(5) 0.0033(4) 0.0009(5) O19 0.0120(5) 0.0291(7) 0.0109(6) -0.0059(5) 0.0032(4) -0.0009(5) O34 0.0143(5) 0.0203(6) 0.0151(6) -0.0013(5) 0.0065(4) 0.0003(5) O2 0.0213(6) 0.0187(6) 0.0182(6) -0.0002(5) 0.0097(5) 0.0013(5) O9 0.0245(6) 0.0229(6) 0.0151(6) -0.0010(5) 0.0135(5) 0.0010(5) O40 0.0444(9) 0.0236(7) 0.0298(8) 0.0022(6) 0.0191(7) 0.0011(7) C14 0.0308(10) 0.0289(11) 0.0291(11) 0.0069(9) 0.0180(9) -0.0007(9) C15 0.0206(9) 0.0278(10) 0.0211(10) 0.0002(9) 0.0085(8) 0.0005(8) C16 0.0228(9) 0.0222(10) 0.0157(9) 0.0027(8) 0.0100(7) 0.0044(8) C11 0.0235(9) 0.0191(9) 0.0140(8) 0.0003(7) 0.0103(7) 0.0048(7) C10 0.0201(9) 0.0190(9) 0.0138(8) -0.0029(8) 0.0074(7) 0.0008(7) C1 0.0145(8) 0.0205(9) 0.0111(8) -0.0007(7) 0.0058(6) 0.0001(7) C9 0.0129(7) 0.0172(8) 0.0116(8) -0.0042(7) 0.0046(6) -0.0040(7) C5 0.0148(8) 0.0188(9) 0.0108(8) -0.0008(7) 0.0061(7) -0.0011(7) C22 0.0145(8) 0.0216(9) 0.0146(8) 0.0006(7) 0.0063(7) 0.0042(7) C23 0.0171(8) 0.0223(9) 0.0156(9) -0.0018(8) 0.0098(7) 0.0024(7) C24 0.0140(8) 0.0228(9) 0.0233(9) -0.0023(8) 0.0115(7) 0.0008(7) C26 0.0284(10) 0.0212(9) 0.0286(10) -0.0065(9) 0.0190(8) -0.0008(8) C27 0.0304(10) 0.0228(10) 0.0256(10) -0.0071(9) 0.0158(9) -0.0057(9) C28 0.0247(9) 0.0245(10) 0.0254(10) -0.0047(9) 0.0103(8) -0.0074(8) C29 0.0252(10) 0.0248(10) 0.0301(10) -0.0109(9) 0.0131(8) -0.0121(8) C30 0.0243(10) 0.0395(12) 0.0489(14) -0.0141(12) 0.0199(10) -0.0098(10) C13 0.0315(10) 0.0305(11) 0.0194(10) 0.0075(9) 0.0138(8) 0.0056(9) C12 0.0255(9) 0.0257(10) 0.0150(9) 0.0019(8) 0.0095(7) 0.0057(8) C8 0.0154(8) 0.0207(9) 0.0097(8) -0.0012(7) 0.0045(6) -0.0016(7) C7 0.0145(8) 0.0196(9) 0.0119(8) -0.0015(7) 0.0063(6) -0.0027(7) C6 0.0159(8) 0.0184(9) 0.0104(8) 0.0009(7) 0.0050(6) -0.0003(7) C31 0.0410(12) 0.0387(13) 0.0296(12) -0.0060(10) 0.0217(10) -0.0085(10) C25 0.0316(10) 0.0242(11) 0.0295(11) 0.0044(9) 0.0045(8) -0.0010(9) C4 0.0136(7) 0.0193(9) 0.0097(8) 0.0010(7) 0.0060(6) 0.0006(7) C19 0.0154(8) 0.0302(10) 0.0095(8) -0.0005(7) 0.0054(6) 0.0018(7) C20 0.0196(9) 0.0355(11) 0.0153(9) 0.0067(9) 0.0076(7) 0.0087(8) C18 0.0157(8) 0.0236(9) 0.0123(8) -0.0034(8) 0.0078(7) -0.0004(7) C33 0.0136(7) 0.0211(8) 0.0095(8) -0.0010(7) 0.0054(6) 0.0018(7) C34 0.0139(7) 0.0246(10) 0.0106(8) 0.0001(7) 0.0056(6) 0.0000(7) C36 0.0162(8) 0.0232(10) 0.0215(9) -0.0043(8) 0.0095(7) 0.0018(7) C35 0.0191(8) 0.0322(10) 0.0146(9) 0.0001(8) 0.0100(7) 0.0000(8) C32 0.0114(7) 0.0196(9) 0.0115(8) -0.0015(7) 0.0059(6) 0.0002(7) C3 0.0135(8) 0.0182(9) 0.0106(8) -0.0016(7) 0.0045(6) 0.0008(7) C2 0.0079(7) 0.0213(9) 0.0146(8) -0.0015(7) 0.0064(6) -0.0007(7) C17 0.0158(8) 0.0208(9) 0.0137(8) -0.0040(8) 0.0063(7) 0.0005(7) C21 0.0181(9) 0.0400(12) 0.0146(9) -0.0060(9) 0.0042(7) 0.0033(8) C38 0.0188(8) 0.0250(9) 0.0127(8) -0.0024(8) 0.0055(7) -0.0007(8) C37 0.0160(8) 0.0274(10) 0.0142(8) 0.0003(8) 0.0048(7) 0.0009(8) C39 0.0320(11) 0.0399(12) 0.0346(11) 0.0101(11) 0.0136(9) 0.0050(10) C40 0.0255(9) 0.0219(10) 0.0211(9) -0.0027(8) 0.0044(8) -0.0038(8) C41 0.0339(11) 0.0297(11) 0.0295(11) 0.0028(10) 0.0095(9) 0.0044(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O10 C10 1.205(2) . ? O4 C4 1.391(2) . ? O4 H4 0.8400 . ? O20 C4 1.428(2) . ? O20 O19 1.4675(16) . ? O19 C19 1.453(2) . ? O34 C34 1.443(2) . ? O34 H34 0.8400 . ? O2 C2 1.210(2) . ? O9 C9 1.209(2) . ? O40 C40 1.214(2) . ? C14 C13 1.384(3) . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C11 1.391(3) . ? C16 H16 0.9500 . ? C11 C12 1.405(3) . ? C11 C10 1.504(2) . ? C10 C1 1.548(2) . ? C1 C9 1.528(2) . ? C1 C2 1.536(2) . ? C1 C8 1.612(2) . ? C9 C5 1.530(2) . ? C5 C22 1.538(2) . ? C5 C6 1.552(2) . ? C5 C4 1.563(2) . ? C22 C23 1.504(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.334(3) . ? C23 H23 0.9500 . ? C24 C26 1.502(3) . ? C24 C25 1.505(3) . ? C26 C27 1.540(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.504(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.332(3) . ? C28 H28 0.9500 . ? C29 C31 1.503(3) . ? C29 C30 1.504(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C13 C12 1.376(3) . ? C13 H13 0.9500 . ? C12 H12 0.9500 . ? C8 C38 1.537(2) . ? C8 C37 1.544(2) . ? C8 C7 1.558(2) . ? C7 C6 1.523(2) . ? C7 C32 1.528(2) . ? C7 H7 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C4 C3 1.553(2) . ? C19 C20 1.523(3) . ? C19 C21 1.525(3) . ? C19 C18 1.542(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18 C17 1.550(2) . ? C18 C33 1.566(2) . ? C18 H18 1.0000 . ? C33 C32 1.537(2) . ? C33 C34 1.551(2) . ? C33 H33 1.0000 . ? C34 C36 1.519(3) . ? C34 C35 1.527(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C32 C3 1.551(2) . ? C32 H32 1.0000 . ? C3 C2 1.505(2) . ? C3 C17 1.530(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 C40 1.496(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.488(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 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 C4 O4 H4 109.5 . . ? C4 O20 O19 109.07(12) . . ? C19 O19 O20 108.13(11) . . ? C34 O34 H34 109.5 . . ? C13 C14 C15 119.77(18) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.32(18) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.42(17) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C16 C11 C12 118.62(17) . . ? C16 C11 C10 125.42(16) . . ? C12 C11 C10 115.96(16) . . ? O10 C10 C11 119.33(16) . . ? O10 C10 C1 120.69(16) . . ? C11 C10 C1 119.98(15) . . ? C9 C1 C2 110.55(13) . . ? C9 C1 C10 110.36(13) . . ? C2 C1 C10 110.38(14) . . ? C9 C1 C8 104.89(14) . . ? C2 C1 C8 106.77(12) . . ? C10 C1 C8 113.73(13) . . ? O9 C9 C1 120.88(16) . . ? O9 C9 C5 123.70(15) . . ? C1 C9 C5 115.37(13) . . ? C9 C5 C22 110.26(13) . . ? C9 C5 C6 108.74(13) . . ? C22 C5 C6 112.41(14) . . ? C9 C5 C4 105.46(13) . . ? C22 C5 C4 111.95(14) . . ? C6 C5 C4 107.72(13) . . ? C23 C22 C5 113.26(14) . . ? C23 C22 H22A 108.9 . . ? C5 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C5 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 126.82(17) . . ? C24 C23 H23 116.6 . . ? C22 C23 H23 116.6 . . ? C23 C24 C26 120.46(17) . . ? C23 C24 C25 123.36(18) . . ? C26 C24 C25 116.17(17) . . ? C24 C26 C27 114.17(15) . . ? C24 C26 H26A 108.7 . . ? C27 C26 H26A 108.7 . . ? C24 C26 H26B 108.7 . . ? C27 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 112.93(16) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C27 128.2(2) . . ? C29 C28 H28 115.9 . . ? C27 C28 H28 115.9 . . ? C28 C29 C31 125.4(2) . . ? C28 C29 C30 121.3(2) . . ? C31 C29 C30 113.30(18) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C12 C13 C14 120.04(18) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C12 C11 120.81(18) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C38 C8 C37 108.05(14) . . ? C38 C8 C7 109.48(14) . . ? C37 C8 C7 110.44(13) . . ? C38 C8 C1 110.86(13) . . ? C37 C8 C1 111.14(14) . . ? C7 C8 C1 106.87(13) . . ? C6 C7 C32 110.79(13) . . ? C6 C7 C8 111.73(13) . . ? C32 C7 C8 108.78(14) . . ? C6 C7 H7 108.5 . . ? C32 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? C7 C6 C5 110.78(14) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 C4 O20 112.19(13) . . ? O4 C4 C3 107.15(13) . . ? O20 C4 C3 112.30(13) . . ? O4 C4 C5 111.32(13) . . ? O20 C4 C5 102.59(13) . . ? C3 C4 C5 111.36(13) . . ? O19 C19 C20 109.09(14) . . ? O19 C19 C21 101.25(13) . . ? C20 C19 C21 110.02(15) . . ? O19 C19 C18 110.35(13) . . ? C20 C19 C18 115.45(15) . . ? C21 C19 C18 109.75(15) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C18 C17 109.74(13) . . ? C19 C18 C33 117.90(15) . . ? C17 C18 C33 105.41(13) . . ? C19 C18 H18 107.8 . . ? C17 C18 H18 107.8 . . ? C33 C18 H18 107.8 . . ? C32 C33 C34 111.38(13) . . ? C32 C33 C18 104.85(13) . . ? C34 C33 C18 113.57(13) . . ? C32 C33 H33 109.0 . . ? C34 C33 H33 109.0 . . ? C18 C33 H33 109.0 . . ? O34 C34 C36 104.24(13) . . ? O34 C34 C35 109.90(14) . . ? C36 C34 C35 109.01(15) . . ? O34 C34 C33 108.21(13) . . ? C36 C34 C33 114.36(15) . . ? C35 C34 C33 110.88(14) . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C7 C32 C33 122.08(15) . . ? C7 C32 C3 110.40(13) . . ? C33 C32 C3 105.89(13) . . ? C7 C32 H32 105.8 . . ? C33 C32 H32 105.8 . . ? C3 C32 H32 105.8 . . ? C2 C3 C17 116.88(15) . . ? C2 C3 C32 102.12(13) . . ? C17 C3 C32 101.12(13) . . ? C2 C3 C4 109.66(13) . . ? C17 C3 C4 113.35(13) . . ? C32 C3 C4 112.90(14) . . ? O2 C2 C3 124.22(15) . . ? O2 C2 C1 121.40(15) . . ? C3 C2 C1 113.81(14) . . ? C3 C17 C18 103.49(14) . . ? C3 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? C3 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.0 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 C38 H38A 109.5 . . ? C8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C8 C37 H37A 109.5 . . ? C8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O40 C40 C41 120.71(19) . . ? O40 C40 C39 122.07(19) . . ? C41 C40 C39 117.23(18) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 C4 O20 O19 C19 -107.16(14) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C11 0.5(3) . . . . ? C15 C16 C11 C12 -0.2(3) . . . . ? C15 C16 C11 C10 179.20(17) . . . . ? C16 C11 C10 O10 -177.78(18) . . . . ? C12 C11 C10 O10 1.6(2) . . . . ? C16 C11 C10 C1 1.5(3) . . . . ? C12 C11 C10 C1 -179.12(15) . . . . ? O10 C10 C1 C9 -117.33(18) . . . . ? C11 C10 C1 C9 63.4(2) . . . . ? O10 C10 C1 C2 120.18(18) . . . . ? C11 C10 C1 C2 -59.08(19) . . . . ? O10 C10 C1 C8 0.2(2) . . . . ? C11 C10 C1 C8 -179.05(14) . . . . ? C2 C1 C9 O9 129.55(16) . . . . ? C10 C1 C9 O9 7.2(2) . . . . ? C8 C1 C9 O9 -115.71(17) . . . . ? C2 C1 C9 C5 -52.83(18) . . . . ? C10 C1 C9 C5 -175.22(13) . . . . ? C8 C1 C9 C5 61.91(17) . . . . ? O9 C9 C5 C22 -4.0(2) . . . . ? C1 C9 C5 C22 178.47(14) . . . . ? O9 C9 C5 C6 119.68(18) . . . . ? C1 C9 C5 C6 -57.86(18) . . . . ? O9 C9 C5 C4 -125.02(17) . . . . ? C1 C9 C5 C4 57.43(17) . . . . ? C9 C5 C22 C23 68.77(18) . . . . ? C6 C5 C22 C23 -52.74(19) . . . . ? C4 C5 C22 C23 -174.15(14) . . . . ? C5 C22 C23 C24 117.87(19) . . . . ? C22 C23 C24 C26 -179.96(15) . . . . ? C22 C23 C24 C25 1.2(3) . . . . ? C23 C24 C26 C27 120.98(19) . . . . ? C25 C24 C26 C27 -60.1(2) . . . . ? C24 C26 C27 C28 -62.3(2) . . . . ? C26 C27 C28 C29 114.5(2) . . . . ? C27 C28 C29 C31 0.0(3) . . . . ? C27 C28 C29 C30 -179.74(19) . . . . ? C15 C14 C13 C12 -0.5(3) . . . . ? C14 C13 C12 C11 0.9(3) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? C10 C11 C12 C13 -179.96(17) . . . . ? C9 C1 C8 C38 58.28(17) . . . . ? C2 C1 C8 C38 175.63(14) . . . . ? C10 C1 C8 C38 -62.38(18) . . . . ? C9 C1 C8 C37 178.47(13) . . . . ? C2 C1 C8 C37 -64.18(17) . . . . ? C10 C1 C8 C37 57.81(18) . . . . ? C9 C1 C8 C7 -60.96(16) . . . . ? C2 C1 C8 C7 56.39(16) . . . . ? C10 C1 C8 C7 178.38(13) . . . . ? C38 C8 C7 C6 -57.12(17) . . . . ? C37 C8 C7 C6 -175.98(14) . . . . ? C1 C8 C7 C6 63.00(17) . . . . ? C38 C8 C7 C32 -179.75(13) . . . . ? C37 C8 C7 C32 61.40(17) . . . . ? C1 C8 C7 C32 -59.62(16) . . . . ? C32 C7 C6 C5 62.53(18) . . . . ? C8 C7 C6 C5 -58.93(18) . . . . ? C9 C5 C6 C7 52.69(18) . . . . ? C22 C5 C6 C7 175.07(14) . . . . ? C4 C5 C6 C7 -61.13(17) . . . . ? O19 O20 C4 O4 -49.59(16) . . . . ? O19 O20 C4 C3 71.18(15) . . . . ? O19 O20 C4 C5 -169.15(11) . . . . ? C9 C5 C4 O4 59.39(17) . . . . ? C22 C5 C4 O4 -60.53(18) . . . . ? C6 C5 C4 O4 175.39(13) . . . . ? C9 C5 C4 O20 179.56(12) . . . . ? C22 C5 C4 O20 59.63(16) . . . . ? C6 C5 C4 O20 -64.45(15) . . . . ? C9 C5 C4 C3 -60.12(16) . . . . ? C22 C5 C4 C3 179.96(13) . . . . ? C6 C5 C4 C3 55.88(17) . . . . ? O20 O19 C19 C20 -70.81(16) . . . . ? O20 O19 C19 C21 173.20(13) . . . . ? O20 O19 C19 C18 57.02(17) . . . . ? O19 C19 C18 C17 34.37(19) . . . . ? C20 C19 C18 C17 158.63(15) . . . . ? C21 C19 C18 C17 -76.37(17) . . . . ? O19 C19 C18 C33 -86.26(18) . . . . ? C20 C19 C18 C33 38.0(2) . . . . ? C21 C19 C18 C33 163.00(14) . . . . ? C19 C18 C33 C32 115.49(15) . . . . ? C17 C18 C33 C32 -7.36(17) . . . . ? C19 C18 C33 C34 -122.70(16) . . . . ? C17 C18 C33 C34 114.45(15) . . . . ? C32 C33 C34 O34 -49.22(19) . . . . ? C18 C33 C34 O34 -167.33(13) . . . . ? C32 C33 C34 C36 66.45(19) . . . . ? C18 C33 C34 C36 -51.7(2) . . . . ? C32 C33 C34 C35 -169.82(15) . . . . ? C18 C33 C34 C35 72.1(2) . . . . ? C6 C7 C32 C33 69.14(18) . . . . ? C8 C7 C32 C33 -167.67(14) . . . . ? C6 C7 C32 C3 -56.16(18) . . . . ? C8 C7 C32 C3 67.03(16) . . . . ? C34 C33 C32 C7 89.81(18) . . . . ? C18 C33 C32 C7 -146.96(14) . . . . ? C34 C33 C32 C3 -142.88(15) . . . . ? C18 C33 C32 C3 -19.64(17) . . . . ? C7 C32 C3 C2 -65.79(17) . . . . ? C33 C32 C3 C2 160.18(13) . . . . ? C7 C32 C3 C17 173.31(14) . . . . ? C33 C32 C3 C17 39.28(16) . . . . ? C7 C32 C3 C4 51.88(18) . . . . ? C33 C32 C3 C4 -82.15(16) . . . . ? O4 C4 C3 C2 -61.66(17) . . . . ? O20 C4 C3 C2 174.71(13) . . . . ? C5 C4 C3 C2 60.29(17) . . . . ? O4 C4 C3 C17 70.97(17) . . . . ? O20 C4 C3 C17 -52.66(18) . . . . ? C5 C4 C3 C17 -167.08(13) . . . . ? O4 C4 C3 C32 -174.80(13) . . . . ? O20 C4 C3 C32 61.58(17) . . . . ? C5 C4 C3 C32 -52.84(18) . . . . ? C17 C3 C2 O2 3.9(2) . . . . ? C32 C3 C2 O2 -105.34(17) . . . . ? C4 C3 C2 O2 134.70(16) . . . . ? C17 C3 C2 C1 175.33(13) . . . . ? C32 C3 C2 C1 66.06(16) . . . . ? C4 C3 C2 C1 -53.90(17) . . . . ? C9 C1 C2 O2 -138.75(15) . . . . ? C10 C1 C2 O2 -16.4(2) . . . . ? C8 C1 C2 O2 107.71(17) . . . . ? C9 C1 C2 C3 49.58(18) . . . . ? C10 C1 C2 C3 171.96(13) . . . . ? C8 C1 C2 C3 -63.96(16) . . . . ? C2 C3 C17 C18 -153.17(14) . . . . ? C32 C3 C17 C18 -43.32(15) . . . . ? C4 C3 C17 C18 77.80(16) . . . . ? C19 C18 C17 C3 -96.01(15) . . . . ? C33 C18 C17 C3 31.92(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O34 0.84 1.93 2.7654(17) 175.3 1_455 O34 H34 O40 0.84 1.96 2.7905(19) 172.7 1_654 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 69.66 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.217 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.055