# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Maerz, Andrew' _publ_contact_author_email akmny4@mail.missouri.edu loop_ _publ_author_name A.Maerz D.Fowler A.Mossine M.Mistry H.Kumari C.Barnes ; C.Deakyne ; J.Atwood data_andyciso _database_code_depnum_ccdc_archive 'CCDC 807883' #TrackingRef 'ANDYCISO.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H58 O14.40' _chemical_formula_weight 853.29 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_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.531(7) _cell_length_b 10.5545(18) _cell_length_c 23.913(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.845(2) _cell_angle_gamma 90.00 _cell_volume 9261(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3641 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9563 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48210 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.42 _reflns_number_total 9470 _reflns_number_gt 5027 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1820P)^2^+13.5295P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9470 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.3266 _refine_ls_wR_factor_gt 0.2585 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.005 _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 O1 O 0.03708(8) 1.0172(4) 0.28016(12) 0.0698(9) Uani 1 1 d . . . H1O H 0.0178 0.9747 0.2716 0.084 Uiso 1 1 calc R . . C1 C 0.10760(9) 1.0264(4) 0.43052(15) 0.0428(8) Uani 1 1 d . . . H1 H 0.1334 1.0205 0.4493 0.051 Uiso 1 1 calc R . . O2 O -0.00282(10) 1.0537(5) 0.35020(17) 0.0762(19) Uani 0.760(12) 1 d P . . C2 C 0.09188(9) 1.0159(4) 0.36851(15) 0.0434(8) Uani 1 1 d . . . O3 O 0.02704(7) 1.0705(3) 0.46986(12) 0.0640(8) Uani 1 1 d . . . H3O H 0.0059 1.0460 0.4488 0.077 Uiso 1 1 calc R . . C3 C 0.05414(10) 1.0251(4) 0.34150(16) 0.0512(9) Uani 1 1 d . . . O4 O 0.05376(8) 1.0086(3) 0.59257(13) 0.0712(9) Uani 1 1 d . . . H4O H 0.0327 0.9789 0.5835 0.085 Uiso 1 1 d . . . C4 C 0.03312(10) 1.0431(4) 0.37623(17) 0.0538(10) Uani 1 1 d . . . O5 O 0.04950(17) 0.7837(7) 0.6411(3) 0.121(3) Uani 0.755(13) 1 d P . . C5 C 0.04980(10) 1.0527(4) 0.43826(17) 0.0518(9) Uani 1 1 d . . . O6 O 0.09368(10) 0.5852(3) 0.64207(14) 0.0728(9) Uani 1 1 d . . . H6O H 0.0888 0.5270 0.6163 0.087 Uiso 1 1 calc R . . C6 C 0.08722(9) 1.0453(4) 0.46698(15) 0.0450(8) Uani 1 1 d . . . O7 O 0.09101(10) 0.4318(4) 0.54849(14) 0.0772(9) Uani 1 1 d . . . H7O H 0.0732 0.3835 0.5319 0.093 Uiso 1 1 calc R . . C7 C 0.10486(10) 1.0564(4) 0.53494(16) 0.0502(9) Uani 1 1 d . B . H7 H 0.0898 1.1178 0.5475 0.060 Uiso 1 1 calc R . . O8 O 0.0687(3) 0.3246(9) 0.4367(4) 0.081(4) Uani 0.363(12) 1 d P . . C8 C 0.12471(10) 0.8298(4) 0.56317(15) 0.0494(9) Uani 1 1 d . . . H8 H 0.1417 0.8412 0.5440 0.059 Uiso 1 1 calc R . . O9 O 0.10227(11) 0.3578(3) 0.36029(14) 0.0794(10) Uani 1 1 d . . . H9O H 0.1064 0.4003 0.3338 0.095 Uiso 1 1 calc R . . C9 C 0.10246(10) 0.9304(4) 0.56401(15) 0.0495(9) Uani 1 1 d . . . O10 O 0.11606(10) 0.4738(3) 0.26402(12) 0.0733(9) Uani 1 1 d . . . H10O H 0.1055 0.4647 0.2266 0.088 Uiso 1 1 calc R . . C10 C 0.07762(11) 0.9118(5) 0.59196(17) 0.0580(11) Uani 1 1 d . . . O11 O 0.07271(14) 0.6466(5) 0.18159(19) 0.079(2) Uani 0.663(12) 1 d P . . C11 C 0.07505(12) 0.7964(5) 0.61719(19) 0.0646(12) Uani 1 1 d . . . O12 O 0.06905(8) 0.8930(3) 0.21150(11) 0.0663(9) Uani 1 1 d . . . H12O H 0.0597 0.9442 0.2285 0.080 Uiso 1 1 calc R . . C12 C 0.09793(12) 0.6985(4) 0.61603(17) 0.0590(11) Uani 1 1 d . . . O13 O 0.00861(14) 0.7506(6) 0.1093(3) 0.144(2) Uani 1 1 d . . . C13 C 0.12343(10) 0.7123(4) 0.58910(15) 0.0511(9) Uani 1 1 d . . . C14 C 0.14918(11) 0.6047(4) 0.58784(16) 0.0538(10) Uani 1 1 d . . . H14 H 0.1472 0.5384 0.6164 0.065 Uiso 1 1 calc R . . O15 O 0.0118(7) 0.564(2) 0.6074(10) 0.273(10) Uiso 0.50 1 d P . . C15 C 0.15305(10) 0.5680(4) 0.48467(16) 0.0497(9) Uani 1 1 d . . . H15 H 0.1721 0.6289 0.4952 0.060 Uiso 1 1 calc R . . O16 O 0.0154(9) 0.335(3) 0.2436(18) 0.194(13) Uiso 0.25 1 d P . . C16 C 0.13695(11) 0.5427(4) 0.52617(16) 0.0524(9) Uani 1 1 d . . . O17 O 0.0198(6) 0.350(2) 0.3083(9) 0.230(8) Uiso 0.50 1 d P . . C17 C 0.10842(13) 0.4565(4) 0.50893(19) 0.0613(11) Uani 1 1 d . . . O18 O -0.0318(8) 0.378(3) 0.2789(13) 0.251(11) Uiso 0.40 1 d P . . C18 C 0.09771(13) 0.3956(4) 0.4539(2) 0.0669(12) Uani 1 1 d . . . C19 C 0.11483(12) 0.4226(4) 0.41394(18) 0.0592(11) Uani 1 1 d . . . C20 C 0.14305(11) 0.5097(4) 0.42884(16) 0.0513(9) Uani 1 1 d . . . C21 C 0.16041(10) 0.5445(4) 0.38330(16) 0.0514(9) Uani 1 1 d . . . H21 H 0.1611 0.4652 0.3609 0.062 Uiso 1 1 calc R . . C22 C 0.13398(9) 0.7645(4) 0.35174(15) 0.0457(9) Uani 1 1 d . . . H22 H 0.1477 0.7911 0.3918 0.055 Uiso 1 1 calc R . . C23 C 0.13608(10) 0.6382(4) 0.33690(15) 0.0488(9) Uani 1 1 d . . . C24 C 0.11501(11) 0.6002(4) 0.27888(17) 0.0541(10) Uani 1 1 d . . . C25 C 0.09235(11) 0.6847(4) 0.23756(16) 0.0577(11) Uani 1 1 d . . . C26 C 0.09177(10) 0.8112(4) 0.25363(15) 0.0534(10) Uani 1 1 d . . . C27 C 0.11291(9) 0.8537(4) 0.31131(15) 0.0452(9) Uani 1 1 d . . . C28 C 0.11365(10) 0.9928(4) 0.32886(15) 0.0464(9) Uani 1 1 d . . . H28 H 0.1013 1.0413 0.2907 0.056 Uiso 1 1 calc R . . C29 C 0.14380(10) 1.1119(4) 0.55674(17) 0.0559(10) Uani 1 1 d . . . H29A H 0.1608 1.0409 0.5601 0.067 Uiso 1 1 calc R A 1 H29B H 0.1451 1.1689 0.5247 0.067 Uiso 1 1 calc R A 1 C31 C 0.1655(6) 1.101(2) 0.6694(9) 0.090(8) Uani 0.296(14) 1 d P B 1 H31A H 0.1901 1.1172 0.6986 0.135 Uiso 0.296(14) 1 calc PR B 1 H31B H 0.1634 1.0119 0.6569 0.135 Uiso 0.296(14) 1 calc PR B 1 H31C H 0.1477 1.1189 0.6881 0.135 Uiso 0.296(14) 1 calc PR B 1 C33 C 0.18900(11) 0.6475(4) 0.61162(17) 0.0579(10) Uani 1 1 d . . . H33A H 0.2043 0.5756 0.6086 0.070 Uiso 1 1 calc R . . H33B H 0.1917 0.7161 0.5853 0.070 Uiso 1 1 calc R . . C34 C 0.20351(12) 0.6951(5) 0.67657(18) 0.0686(13) Uani 1 1 d . . . H34 H 0.1860 0.7602 0.6800 0.082 Uiso 1 1 calc R . . C35 C 0.24025(16) 0.7599(6) 0.6916(2) 0.0936(18) Uani 1 1 d . . . H35A H 0.2485 0.7938 0.7327 0.140 Uiso 1 1 calc R . . H35B H 0.2378 0.8293 0.6631 0.140 Uiso 1 1 calc R . . H35C H 0.2581 0.6983 0.6887 0.140 Uiso 1 1 calc R . . C36 C 0.20577(15) 0.5912(6) 0.7213(2) 0.0875(17) Uani 1 1 d . . . H36A H 0.2228 0.5258 0.7191 0.131 Uiso 1 1 calc R . . H36B H 0.1816 0.5536 0.7118 0.131 Uiso 1 1 calc R . . H36C H 0.2144 0.6268 0.7621 0.131 Uiso 1 1 calc R . . C37 C 0.19963(11) 0.5930(4) 0.41119(18) 0.0563(10) Uani 1 1 d . . . H37A H 0.1995 0.6729 0.4328 0.068 Uiso 1 1 calc R . . H37B H 0.2080 0.6136 0.3781 0.068 Uiso 1 1 calc R . . C38 C 0.22751(12) 0.5028(5) 0.4550(2) 0.0696(13) Uani 1 1 d . . . H38 H 0.2212 0.4942 0.4917 0.084 Uiso 1 1 calc R . . C39 C 0.26529(13) 0.5606(6) 0.4746(2) 0.0880(17) Uani 1 1 d . . . H39A H 0.2720 0.5713 0.4394 0.132 Uiso 1 1 calc R . . H39B H 0.2829 0.5046 0.5038 0.132 Uiso 1 1 calc R . . H39C H 0.2653 0.6434 0.4932 0.132 Uiso 1 1 calc R . . C40 C 0.22636(16) 0.3714(6) 0.4285(3) 0.0908(17) Uani 1 1 d . . . H40A H 0.2265 0.3787 0.3877 0.136 Uiso 1 1 calc R . . H40B H 0.2041 0.3277 0.4268 0.136 Uiso 1 1 calc R . . H40C H 0.2477 0.3230 0.4538 0.136 Uiso 1 1 calc R . . C41 C 0.15317(10) 1.0425(4) 0.35664(18) 0.0539(10) Uani 1 1 d . . . H41A H 0.1527 1.1321 0.3685 0.065 Uiso 1 1 calc R . . H41B H 0.1665 0.9935 0.3936 0.065 Uiso 1 1 calc R . . C42 C 0.17371(14) 1.0335(5) 0.3146(2) 0.0767(14) Uani 1 1 d . . . H42 H 0.1718 0.9440 0.3000 0.092 Uiso 1 1 calc R . . C43 C 0.21392(15) 1.0630(7) 0.3472(3) 0.101(2) Uani 1 1 d . . . H43A H 0.2167 1.1499 0.3627 0.152 Uiso 1 1 calc R . . H43B H 0.2266 1.0542 0.3192 0.152 Uiso 1 1 calc R . . H43C H 0.2244 1.0038 0.3809 0.152 Uiso 1 1 calc R . . C44 C 0.1563(2) 1.1183(10) 0.2597(3) 0.152(4) Uani 1 1 d . . . H44A H 0.1303 1.0976 0.2403 0.229 Uiso 1 1 calc R . . H44B H 0.1683 1.1045 0.2310 0.229 Uiso 1 1 calc R . . H44C H 0.1589 1.2072 0.2723 0.229 Uiso 1 1 calc R . . C45 C -0.0541(2) 0.7164(8) 0.0647(5) 0.182(5) Uani 1 1 d . . . H45A H -0.0504 0.7121 0.0265 0.272 Uiso 1 1 calc R . . H45B H -0.0689 0.7910 0.0647 0.272 Uiso 1 1 calc R . . H45C H -0.0668 0.6398 0.0694 0.272 Uiso 1 1 calc R . . C46 C -0.02099(17) 0.7249(6) 0.1115(3) 0.0957(18) Uani 1 1 d . . . C47 C -0.0222(3) 0.7053(12) 0.1737(4) 0.179(4) Uani 1 1 d . . . H47A H -0.0294 0.6178 0.1774 0.268 Uiso 1 1 calc R . . H47B H -0.0400 0.7636 0.1793 0.268 Uiso 1 1 calc R . . H47C H 0.0019 0.7217 0.2045 0.268 Uiso 1 1 calc R . . O14 O 0.0212(3) 0.3342(11) 0.5026(6) 0.146(5) Uiso 0.67(2) 1 d P . . O14' O 0.0351(5) 0.2896(18) 0.5379(10) 0.118(8) Uiso 0.33(2) 1 d P . . C30 C 0.1580(6) 1.185(3) 0.6154(11) 0.062(6) Uani 0.296(14) 1 d P B 1 H30 H 0.1385 1.2454 0.6148 0.074 Uiso 0.296(14) 1 calc PR B 1 C30' C 0.1619(3) 1.1221(12) 0.6262(4) 0.067(3) Uani 0.704(14) 1 d P B 2 H30' H 0.1642 1.0356 0.6443 0.080 Uiso 0.704(14) 1 calc PR B 2 C32 C 0.1914(6) 1.261(2) 0.6240(11) 0.077(6) Uani 0.296(14) 1 d P B 1 H32A H 0.2048 1.2221 0.6012 0.116 Uiso 0.296(14) 1 calc PR B 1 H32B H 0.2070 1.2625 0.6669 0.116 Uiso 0.296(14) 1 calc PR B 1 H32C H 0.1844 1.3473 0.6097 0.116 Uiso 0.296(14) 1 calc PR B 1 C32' C 0.2000(3) 1.177(2) 0.6396(6) 0.147(8) Uani 0.704(14) 1 d P B 2 H32D H 0.2132 1.1817 0.6833 0.220 Uiso 0.704(14) 1 calc PR B 2 H32E H 0.1978 1.2627 0.6225 0.220 Uiso 0.704(14) 1 calc PR B 2 H32F H 0.2134 1.1230 0.6218 0.220 Uiso 0.704(14) 1 calc PR B 2 C31' C 0.1417(2) 1.2059(9) 0.6530(3) 0.083(3) Uani 0.704(14) 1 d P B 2 H31D H 0.1541 1.2070 0.6969 0.124 Uiso 0.704(14) 1 calc PR B 2 H31E H 0.1168 1.1739 0.6425 0.124 Uiso 0.704(14) 1 calc PR B 2 H31F H 0.1408 1.2921 0.6372 0.124 Uiso 0.704(14) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0479(16) 0.113(3) 0.0384(14) 0.0021(15) 0.0043(12) 0.0130(16) C1 0.0377(18) 0.056(2) 0.0353(17) 0.0003(15) 0.0141(14) 0.0029(15) O2 0.042(2) 0.124(4) 0.053(3) -0.002(2) 0.0064(17) 0.011(2) C2 0.0366(18) 0.057(2) 0.0359(17) 0.0068(16) 0.0128(14) 0.0050(16) O3 0.0381(14) 0.107(2) 0.0489(15) 0.0007(15) 0.0184(12) 0.0139(15) C3 0.043(2) 0.070(3) 0.0354(18) 0.0034(17) 0.0085(15) 0.0078(18) O4 0.0649(19) 0.096(2) 0.0611(18) 0.0119(16) 0.0338(15) 0.0266(17) C4 0.038(2) 0.075(3) 0.044(2) 0.0002(19) 0.0116(16) 0.0111(18) O5 0.112(5) 0.150(6) 0.133(6) 0.042(4) 0.083(4) 0.027(4) C5 0.046(2) 0.069(3) 0.043(2) 0.0031(18) 0.0196(16) 0.0121(18) O6 0.086(2) 0.083(2) 0.0568(18) 0.0207(16) 0.0357(17) 0.0077(18) C6 0.0400(19) 0.057(2) 0.0366(18) 0.0013(16) 0.0123(15) 0.0034(16) O7 0.081(2) 0.090(3) 0.063(2) 0.0112(17) 0.0300(17) -0.0140(18) C7 0.052(2) 0.064(2) 0.0356(18) -0.0015(17) 0.0171(16) 0.0118(18) O8 0.101(8) 0.081(7) 0.069(6) -0.013(5) 0.041(5) -0.034(6) C8 0.047(2) 0.069(3) 0.0326(17) 0.0005(17) 0.0163(15) 0.0046(18) O9 0.106(3) 0.070(2) 0.0537(18) -0.0115(15) 0.0193(18) -0.0243(19) C9 0.046(2) 0.071(3) 0.0306(17) 0.0004(17) 0.0131(15) 0.0095(18) O10 0.092(2) 0.077(2) 0.0397(15) -0.0196(14) 0.0117(15) 0.0076(17) C10 0.055(2) 0.082(3) 0.041(2) 0.010(2) 0.0223(18) 0.017(2) O11 0.082(4) 0.096(4) 0.038(3) -0.018(2) 0.000(2) 0.015(3) C11 0.060(3) 0.091(3) 0.050(2) 0.014(2) 0.029(2) 0.011(2) O12 0.0641(18) 0.093(2) 0.0341(13) 0.0047(14) 0.0098(12) 0.0264(16) C12 0.062(2) 0.074(3) 0.041(2) 0.0126(19) 0.0199(18) 0.005(2) O13 0.079(3) 0.192(6) 0.146(5) 0.018(4) 0.025(3) 0.013(3) C13 0.051(2) 0.069(3) 0.0307(17) 0.0062(17) 0.0119(15) 0.0085(19) C14 0.059(2) 0.064(3) 0.0341(18) 0.0090(17) 0.0129(17) 0.0103(19) C15 0.052(2) 0.054(2) 0.0376(18) 0.0038(16) 0.0092(16) 0.0100(17) C16 0.052(2) 0.063(2) 0.0386(19) 0.0087(17) 0.0122(16) 0.0092(19) C17 0.068(3) 0.065(3) 0.048(2) 0.011(2) 0.017(2) 0.004(2) C18 0.073(3) 0.062(3) 0.059(3) 0.008(2) 0.016(2) -0.005(2) C19 0.068(3) 0.057(2) 0.044(2) -0.0036(18) 0.0098(19) -0.002(2) C20 0.054(2) 0.053(2) 0.0387(19) 0.0008(16) 0.0089(16) 0.0080(18) C21 0.053(2) 0.059(2) 0.0369(18) -0.0076(17) 0.0111(16) 0.0091(18) C22 0.0406(18) 0.065(2) 0.0280(16) -0.0022(16) 0.0087(14) 0.0022(16) C23 0.047(2) 0.062(2) 0.0336(18) -0.0063(16) 0.0106(15) 0.0018(17) C24 0.057(2) 0.067(3) 0.0370(19) -0.0093(18) 0.0152(17) 0.0057(19) C25 0.052(2) 0.086(3) 0.0274(17) -0.0117(18) 0.0059(15) 0.007(2) C26 0.045(2) 0.083(3) 0.0291(17) 0.0036(18) 0.0102(15) 0.0122(19) C27 0.0376(18) 0.066(2) 0.0316(17) 0.0009(16) 0.0130(14) 0.0019(16) C28 0.0442(19) 0.064(2) 0.0321(17) 0.0072(16) 0.0150(15) 0.0058(17) C29 0.046(2) 0.078(3) 0.041(2) -0.0067(19) 0.0129(16) 0.0061(19) C31 0.109(16) 0.110(17) 0.049(11) -0.019(10) 0.028(10) -0.040(14) C33 0.053(2) 0.076(3) 0.0378(19) 0.0031(19) 0.0087(17) 0.015(2) C34 0.062(3) 0.093(3) 0.043(2) -0.007(2) 0.0098(19) 0.020(2) C35 0.095(4) 0.108(4) 0.055(3) -0.009(3) 0.000(3) -0.003(3) C36 0.086(4) 0.129(5) 0.040(2) 0.004(3) 0.014(2) 0.009(3) C37 0.053(2) 0.070(3) 0.043(2) -0.0048(19) 0.0153(17) 0.009(2) C38 0.059(3) 0.094(3) 0.049(2) 0.001(2) 0.012(2) 0.018(2) C39 0.055(3) 0.123(5) 0.070(3) -0.008(3) 0.005(2) 0.020(3) C40 0.084(4) 0.092(4) 0.087(4) 0.005(3) 0.021(3) 0.031(3) C41 0.045(2) 0.067(3) 0.053(2) 0.0030(19) 0.0225(18) 0.0016(18) C42 0.078(3) 0.088(3) 0.084(3) -0.006(3) 0.053(3) -0.013(3) C43 0.070(3) 0.115(5) 0.143(6) -0.029(4) 0.068(4) -0.019(3) C44 0.132(6) 0.236(10) 0.120(6) 0.084(6) 0.082(5) 0.012(6) C45 0.101(5) 0.107(6) 0.245(11) -0.027(7) -0.041(6) -0.009(5) C46 0.070(4) 0.100(4) 0.102(5) 0.007(3) 0.015(3) 0.018(3) C47 0.218(11) 0.208(11) 0.128(7) 0.036(7) 0.084(8) 0.063(9) C30 0.039(9) 0.089(17) 0.044(10) 0.006(11) -0.001(7) 0.010(10) C30' 0.061(5) 0.089(7) 0.037(5) -0.006(5) 0.004(4) 0.014(5) C32 0.044(10) 0.101(16) 0.070(12) -0.022(11) 0.001(8) 0.006(9) C32' 0.063(6) 0.27(2) 0.081(8) -0.097(11) -0.001(5) 0.005(9) C31' 0.086(5) 0.115(7) 0.042(4) -0.018(4) 0.018(3) 0.024(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 O1 C3 1.370(4) . ? O1 H1O 0.8400 . ? C1 C2 1.383(5) . ? C1 C6 1.404(5) . ? C1 H1 0.9500 . ? O2 C4 1.327(5) . ? C2 C3 1.391(5) . ? C2 C28 1.519(5) . ? O3 C5 1.386(4) . ? O3 H3O 0.8400 . ? C3 C4 1.389(5) . ? O4 C10 1.394(5) . ? O4 H4O 0.8398 . ? C4 C5 1.385(5) . ? O5 C11 1.340(6) . ? C5 C6 1.382(5) . ? O6 C12 1.387(5) . ? O6 H6O 0.8400 . ? C6 C7 1.516(5) . ? O7 C17 1.386(5) . ? O7 H7O 0.8400 . ? C7 C9 1.520(6) . ? C7 C29 1.545(6) . ? C7 H7 1.0000 . ? O8 C18 1.303(10) . ? C8 C9 1.384(5) . ? C8 C13 1.395(6) . ? C8 H8 0.9500 . ? O9 C19 1.373(5) . ? O9 H9O 0.8400 . ? C9 C10 1.392(5) . ? O10 C24 1.385(5) . ? O10 H10O 0.8400 . ? C10 C11 1.379(7) . ? O11 C25 1.335(5) . ? C11 C12 1.381(6) . ? O12 C26 1.377(5) . ? O12 H12O 0.8400 . ? C12 C13 1.391(5) . ? O13 C46 1.221(8) . ? C13 C14 1.533(6) . ? C14 C16 1.519(5) . ? C14 C33 1.530(6) . ? C14 H14 1.0000 . ? C15 C20 1.387(5) . ? C15 C16 1.390(5) . ? C15 H15 0.9500 . ? O16 O18 1.08(4) 2 ? O16 O16 1.36(6) 2 ? O16 O17 1.49(4) 2 ? O16 O17 1.50(4) . ? C16 C17 1.387(6) . ? O17 O16 1.49(4) 2 ? C17 C18 1.382(6) . ? O18 O16 1.08(4) 2 ? C18 C19 1.390(6) . ? C19 C20 1.386(6) . ? C20 C21 1.532(6) . ? C21 C23 1.530(5) . ? C21 C37 1.530(6) . ? C21 H21 1.0000 . ? C22 C27 1.384(5) . ? C22 C23 1.390(6) . ? C22 H22 0.9500 . ? C23 C24 1.385(5) . ? C24 C25 1.384(6) . ? C25 C26 1.392(6) . ? C26 C27 1.395(5) . ? C27 C28 1.523(6) . ? C28 C41 1.544(5) . ? C28 H28 1.0000 . ? C29 C30 1.51(3) . ? C29 C30' 1.548(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C30 1.50(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.527(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C36 1.512(7) . ? C34 C35 1.522(8) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.536(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.517(7) . ? C38 C40 1.519(8) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.512(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.519(7) . ? C42 C44 1.526(9) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.374(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.520(10) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? O14 O14' 0.943(17) . ? C30 C32 1.49(3) . ? C30 H30 1.0000 . ? C30' C31' 1.488(14) . ? C30' C32' 1.534(17) . ? C30' H30' 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 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 C3 O1 H1O 109.5 . . ? C2 C1 C6 123.0(3) . . ? C2 C1 H1 118.5 . . ? C6 C1 H1 118.5 . . ? C1 C2 C3 117.9(3) . . ? C1 C2 C28 123.3(3) . . ? C3 C2 C28 118.7(3) . . ? C5 O3 H3O 109.5 . . ? O1 C3 C4 118.9(3) . . ? O1 C3 C2 120.5(3) . . ? C4 C3 C2 120.6(3) . . ? C10 O4 H4O 109.5 . . ? O2 C4 C5 119.8(4) . . ? O2 C4 C3 120.3(4) . . ? C5 C4 C3 119.9(3) . . ? C6 C5 C4 121.5(3) . . ? C6 C5 O3 121.9(3) . . ? C4 C5 O3 116.5(3) . . ? C12 O6 H6O 109.5 . . ? C5 C6 C1 117.1(3) . . ? C5 C6 C7 120.6(3) . . ? C1 C6 C7 122.4(3) . . ? C17 O7 H7O 109.5 . . ? C6 C7 C9 109.9(3) . . ? C6 C7 C29 113.2(3) . . ? C9 C7 C29 113.7(3) . . ? C6 C7 H7 106.5 . . ? C9 C7 H7 106.5 . . ? C29 C7 H7 106.5 . . ? C9 C8 C13 123.2(3) . . ? C9 C8 H8 118.4 . . ? C13 C8 H8 118.4 . . ? C19 O9 H9O 109.5 . . ? C8 C9 C10 117.7(4) . . ? C8 C9 C7 121.1(3) . . ? C10 C9 C7 121.2(3) . . ? C24 O10 H10O 109.5 . . ? C11 C10 C9 121.0(4) . . ? C11 C10 O4 118.8(4) . . ? C9 C10 O4 120.1(4) . . ? O5 C11 C10 117.7(5) . . ? O5 C11 C12 122.5(5) . . ? C10 C11 C12 119.8(4) . . ? C26 O12 H12O 109.5 . . ? C11 C12 O6 116.5(4) . . ? C11 C12 C13 121.6(4) . . ? O6 C12 C13 121.9(4) . . ? C12 C13 C8 116.8(4) . . ? C12 C13 C14 122.1(4) . . ? C8 C13 C14 121.0(3) . . ? C16 C14 C33 113.6(3) . . ? C16 C14 C13 111.4(3) . . ? C33 C14 C13 111.9(4) . . ? C16 C14 H14 106.5 . . ? C33 C14 H14 106.5 . . ? C13 C14 H14 106.5 . . ? C20 C15 C16 124.1(4) . . ? C20 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? O18 O16 O16 149(4) 2 2 ? O18 O16 O17 95(4) 2 2 ? O16 O16 O17 63(3) 2 2 ? O18 O16 O17 127(4) 2 . ? O16 O16 O17 62(3) 2 . ? O17 O16 O17 124(3) 2 . ? C17 C16 C15 116.8(4) . . ? C17 C16 C14 120.1(4) . . ? C15 C16 C14 123.1(4) . . ? O16 O17 O16 54(3) 2 . ? C18 C17 O7 120.6(4) . . ? C18 C17 C16 121.0(4) . . ? O7 C17 C16 118.4(4) . . ? O8 C18 C17 119.3(6) . . ? O8 C18 C19 119.9(6) . . ? C17 C18 C19 120.3(4) . . ? O9 C19 C20 123.2(4) . . ? O9 C19 C18 116.1(4) . . ? C20 C19 C18 120.7(4) . . ? C19 C20 C15 117.1(4) . . ? C19 C20 C21 120.5(3) . . ? C15 C20 C21 122.3(4) . . ? C23 C21 C37 111.2(3) . . ? C23 C21 C20 110.1(3) . . ? C37 C21 C20 114.8(3) . . ? C23 C21 H21 106.8 . . ? C37 C21 H21 106.8 . . ? C20 C21 H21 106.8 . . ? C27 C22 C23 123.5(3) . . ? C27 C22 H22 118.3 . . ? C23 C22 H22 118.3 . . ? C24 C23 C22 117.5(3) . . ? C24 C23 C21 121.4(4) . . ? C22 C23 C21 121.0(3) . . ? C25 C24 O10 120.7(3) . . ? C25 C24 C23 121.1(4) . . ? O10 C24 C23 118.1(4) . . ? O11 C25 C24 120.2(4) . . ? O11 C25 C26 120.2(4) . . ? C24 C25 C26 119.6(3) . . ? O12 C26 C25 118.2(3) . . ? O12 C26 C27 120.6(4) . . ? C25 C26 C27 121.1(4) . . ? C22 C27 C26 117.1(4) . . ? C22 C27 C28 121.2(3) . . ? C26 C27 C28 121.7(3) . . ? C2 C28 C27 111.7(3) . . ? C2 C28 C41 113.2(3) . . ? C27 C28 C41 111.0(3) . . ? C2 C28 H28 106.8 . . ? C27 C28 H28 106.8 . . ? C41 C28 H28 106.8 . . ? C30 C29 C7 119.1(10) . . ? C30 C29 C30' 26.5(8) . . ? C7 C29 C30' 113.1(5) . . ? C30 C29 H29A 107.6 . . ? C7 C29 H29A 107.6 . . ? C30' C29 H29A 86.4 . . ? C30 C29 H29B 107.6 . . ? C7 C29 H29B 107.6 . . ? C30' C29 H29B 130.6 . . ? H29A C29 H29B 107.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C33 C14 114.9(4) . . ? C34 C33 H33A 108.6 . . ? C14 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C14 C33 H33B 108.6 . . ? H33A C33 H33B 107.5 . . ? C36 C34 C35 111.0(4) . . ? C36 C34 C33 112.5(4) . . ? C35 C34 C33 110.6(4) . . ? C36 C34 H34 107.5 . . ? C35 C34 H34 107.5 . . ? C33 C34 H34 107.5 . . ? 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 . . ? 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 . . ? C21 C37 C38 116.3(4) . . ? C21 C37 H37A 108.2 . . ? C38 C37 H37A 108.2 . . ? C21 C37 H37B 108.2 . . ? C38 C37 H37B 108.2 . . ? H37A C37 H37B 107.4 . . ? C39 C38 C40 111.6(4) . . ? C39 C38 C37 109.6(4) . . ? C40 C38 C37 112.2(4) . . ? C39 C38 H38 107.7 . . ? C40 C38 H38 107.7 . . ? C37 C38 H38 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C28 113.6(3) . . ? C42 C41 H41A 108.8 . . ? C28 C41 H41A 108.8 . . ? C42 C41 H41B 108.8 . . ? C28 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C41 C42 C43 111.4(4) . . ? C41 C42 C44 110.7(5) . . ? C43 C42 C44 111.9(5) . . ? C41 C42 H42 107.5 . . ? C43 C42 H42 107.5 . . ? C44 C42 H42 107.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O13 C46 C45 128.1(8) . . ? O13 C46 C47 116.9(7) . . ? C45 C46 C47 114.9(9) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C32 C30 C31 108.5(17) . . ? C32 C30 C29 114.0(19) . . ? C31 C30 C29 113(2) . . ? C32 C30 H30 107.1 . . ? C31 C30 H30 107.1 . . ? C29 C30 H30 107.1 . . ? C31' C30' C32' 109.1(9) . . ? C31' C30' C29 113.3(7) . . ? C32' C30' C29 106.1(8) . . ? C31' C30' H30' 109.4 . . ? C32' C30' H30' 109.4 . . ? C29 C30' H30' 109.4 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30' C32' H32D 109.5 . . ? C30' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C30' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 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 C6 C1 C2 C3 0.2(6) . . . . ? C6 C1 C2 C28 -178.7(4) . . . . ? C1 C2 C3 O1 179.1(4) . . . . ? C28 C2 C3 O1 -2.0(6) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C28 C2 C3 C4 178.4(4) . . . . ? O1 C3 C4 O2 -0.7(7) . . . . ? C2 C3 C4 O2 178.9(4) . . . . ? O1 C3 C4 C5 -179.3(4) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? O2 C4 C5 C6 -178.4(4) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? O2 C4 C5 O3 1.5(7) . . . . ? C3 C4 C5 O3 -179.9(4) . . . . ? C4 C5 C6 C1 -0.5(6) . . . . ? O3 C5 C6 C1 179.6(4) . . . . ? C4 C5 C6 C7 179.9(4) . . . . ? O3 C5 C6 C7 0.0(6) . . . . ? C2 C1 C6 C5 0.3(6) . . . . ? C2 C1 C6 C7 179.9(4) . . . . ? C5 C6 C7 C9 80.5(5) . . . . ? C1 C6 C7 C9 -99.1(4) . . . . ? C5 C6 C7 C29 -151.2(4) . . . . ? C1 C6 C7 C29 29.2(5) . . . . ? C13 C8 C9 C10 -0.4(6) . . . . ? C13 C8 C9 C7 -179.8(3) . . . . ? C6 C7 C9 C8 74.9(4) . . . . ? C29 C7 C9 C8 -53.2(5) . . . . ? C6 C7 C9 C10 -104.5(4) . . . . ? C29 C7 C9 C10 127.4(4) . . . . ? C8 C9 C10 C11 -0.8(6) . . . . ? C7 C9 C10 C11 178.7(4) . . . . ? C8 C9 C10 O4 -178.1(4) . . . . ? C7 C9 C10 O4 1.4(6) . . . . ? C9 C10 C11 O5 -177.3(5) . . . . ? O4 C10 C11 O5 0.0(7) . . . . ? C9 C10 C11 C12 1.5(7) . . . . ? O4 C10 C11 C12 178.7(4) . . . . ? O5 C11 C12 O6 -1.1(7) . . . . ? C10 C11 C12 O6 -179.8(4) . . . . ? O5 C11 C12 C13 177.7(5) . . . . ? C10 C11 C12 C13 -0.9(7) . . . . ? C11 C12 C13 C8 -0.2(6) . . . . ? O6 C12 C13 C8 178.6(4) . . . . ? C11 C12 C13 C14 179.6(4) . . . . ? O6 C12 C13 C14 -1.6(6) . . . . ? C9 C8 C13 C12 0.8(6) . . . . ? C9 C8 C13 C14 -178.9(3) . . . . ? C12 C13 C14 C16 103.7(4) . . . . ? C8 C13 C14 C16 -76.5(5) . . . . ? C12 C13 C14 C33 -128.0(4) . . . . ? C8 C13 C14 C33 51.8(4) . . . . ? C20 C15 C16 C17 -2.1(6) . . . . ? C20 C15 C16 C14 178.0(4) . . . . ? C33 C14 C16 C17 154.3(4) . . . . ? C13 C14 C16 C17 -78.4(5) . . . . ? C33 C14 C16 C15 -25.8(5) . . . . ? C13 C14 C16 C15 101.6(4) . . . . ? O18 O16 O17 O16 146(4) 2 . . 2 ? O17 O16 O17 O16 14(4) 2 . . 2 ? C15 C16 C17 C18 2.4(6) . . . . ? C14 C16 C17 C18 -177.7(4) . . . . ? C15 C16 C17 O7 -178.1(4) . . . . ? C14 C16 C17 O7 1.8(6) . . . . ? O7 C17 C18 O8 7.0(8) . . . . ? C16 C17 C18 O8 -173.5(6) . . . . ? O7 C17 C18 C19 178.8(4) . . . . ? C16 C17 C18 C19 -1.7(7) . . . . ? O8 C18 C19 O9 -8.1(8) . . . . ? C17 C18 C19 O9 -179.8(4) . . . . ? O8 C18 C19 C20 172.3(7) . . . . ? C17 C18 C19 C20 0.6(7) . . . . ? O9 C19 C20 C15 -179.8(4) . . . . ? C18 C19 C20 C15 -0.2(6) . . . . ? O9 C19 C20 C21 3.9(6) . . . . ? C18 C19 C20 C21 -176.6(4) . . . . ? C16 C15 C20 C19 1.0(6) . . . . ? C16 C15 C20 C21 177.3(3) . . . . ? C19 C20 C21 C23 78.5(5) . . . . ? C15 C20 C21 C23 -97.6(4) . . . . ? C19 C20 C21 C37 -155.1(4) . . . . ? C15 C20 C21 C37 28.8(5) . . . . ? C27 C22 C23 C24 -1.9(6) . . . . ? C27 C22 C23 C21 178.9(3) . . . . ? C37 C21 C23 C24 127.0(4) . . . . ? C20 C21 C23 C24 -104.6(4) . . . . ? C37 C21 C23 C22 -53.8(5) . . . . ? C20 C21 C23 C22 74.6(5) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C21 C23 C24 C25 178.4(4) . . . . ? C22 C23 C24 O10 -178.2(4) . . . . ? C21 C23 C24 O10 1.0(6) . . . . ? O10 C24 C25 O11 -3.8(7) . . . . ? C23 C24 C25 O11 179.0(4) . . . . ? O10 C24 C25 C26 179.9(4) . . . . ? C23 C24 C25 C26 2.7(6) . . . . ? O11 C25 C26 O12 3.5(6) . . . . ? C24 C25 C26 O12 179.8(4) . . . . ? O11 C25 C26 C27 -178.1(4) . . . . ? C24 C25 C26 C27 -1.8(6) . . . . ? C23 C22 C27 C26 2.7(5) . . . . ? C23 C22 C27 C28 -175.8(3) . . . . ? O12 C26 C27 C22 177.6(3) . . . . ? C25 C26 C27 C22 -0.8(5) . . . . ? O12 C26 C27 C28 -3.9(5) . . . . ? C25 C26 C27 C28 177.7(4) . . . . ? C1 C2 C28 C27 99.2(4) . . . . ? C3 C2 C28 C27 -79.7(4) . . . . ? C1 C2 C28 C41 -27.0(5) . . . . ? C3 C2 C28 C41 154.1(4) . . . . ? C22 C27 C28 C2 -76.6(4) . . . . ? C26 C27 C28 C2 105.0(4) . . . . ? C22 C27 C28 C41 50.8(4) . . . . ? C26 C27 C28 C41 -127.6(4) . . . . ? C6 C7 C29 C30 151.6(11) . . . . ? C9 C7 C29 C30 -82.1(12) . . . . ? C6 C7 C29 C30' -179.5(5) . . . . ? C9 C7 C29 C30' -53.2(6) . . . . ? C16 C14 C33 C34 -172.7(4) . . . . ? C13 C14 C33 C34 60.1(5) . . . . ? C14 C33 C34 C36 66.8(5) . . . . ? C14 C33 C34 C35 -168.4(4) . . . . ? C23 C21 C37 C38 -175.5(3) . . . . ? C20 C21 C37 C38 58.7(5) . . . . ? C21 C37 C38 C39 175.5(4) . . . . ? C21 C37 C38 C40 50.9(5) . . . . ? C2 C28 C41 C42 -173.4(4) . . . . ? C27 C28 C41 C42 60.1(4) . . . . ? C28 C41 C42 C43 -170.6(4) . . . . ? C28 C41 C42 C44 64.2(6) . . . . ? C7 C29 C30 C32 -165.2(13) . . . . ? C30' C29 C30 C32 111(3) . . . . ? C7 C29 C30 C31 70.5(19) . . . . ? C30' C29 C30 C31 -13.4(18) . . . . ? C30 C29 C30' C31' 48(2) . . . . ? C7 C29 C30' C31' -60.8(10) . . . . ? C30 C29 C30' C32' -71(3) . . . . ? C7 C29 C30' C32' 179.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.801 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.076 # Attachment 'mm48.cif' data_MM48 _database_code_depnum_ccdc_archive 'CCDC 807884' #TrackingRef 'mm48.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 O16' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour colourless _diffrn_ambient_temperature 173(2) _chemical_formula_weight 776.72 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' 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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.940(5) _cell_length_b 12.189(5) _cell_length_c 17.454(10) _cell_angle_alpha 78.497(6) _cell_angle_beta 87.202(7) _cell_angle_gamma 84.105(4) _cell_volume 2268(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3242 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.1 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of G\"ottingen, Germany). ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 24603 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.33 _reflns_number_total 9178 _reflns_number_gt 4562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (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. The disordered hydrogen bonding pattern which results from the mixed macrocycle was modeled to a reasonalbe level. Some close contacts remain. ; _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^)+(0.1469P)^2^+0.2353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9178 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2773 _refine_ls_wR_factor_gt 0.2308 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 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 O1 O -0.0812(2) -0.0207(2) 0.30793(17) 0.0646(8) Uani 1 1 d . . . C1 C -0.0315(3) 0.2672(3) 0.2142(2) 0.0470(9) Uani 1 1 d . . . H1 H 0.0210 0.3060 0.1754 0.056 Uiso 1 1 calc R . . O2 O -0.2445(3) 0.0990(3) 0.3901(2) 0.0658(16) Uani 0.779(10) 1 d P . . C2 C -0.0157(3) 0.1503(3) 0.2313(2) 0.0459(8) Uani 1 1 d . . . O3 O -0.2817(2) 0.3213(2) 0.35429(17) 0.0636(7) Uani 1 1 d . . . C3 C -0.0927(3) 0.0963(3) 0.2891(2) 0.0505(9) Uani 1 1 d . . . O4 O -0.2628(2) 0.5423(2) 0.35716(16) 0.0628(7) Uani 1 1 d . . . H4O H -0.2909 0.5684 0.3962 0.075 Uiso 1 1 calc R . . C4 C -0.1789(3) 0.1559(3) 0.3290(2) 0.0530(9) Uani 1 1 d . . . O5 O -0.1378(13) 0.6385(12) 0.4492(9) 0.092(7) Uani 0.246(11) 1 d P . . C5 C -0.1928(3) 0.2722(3) 0.3104(2) 0.0503(9) Uani 1 1 d . . . O6 O 0.1105(2) 0.6519(2) 0.44380(15) 0.0566(7) Uani 1 1 d . . . C6 C -0.1215(3) 0.3306(3) 0.2516(2) 0.0459(8) Uani 1 1 d . . . O7 O 0.3275(3) 0.5261(3) 0.48172(17) 0.0746(9) Uani 1 1 d . . . C7 C -0.1410(4) 0.4600(3) 0.2293(2) 0.0555(10) Uani 1 1 d . . . H7 H -0.2306 0.4795 0.2393 0.067 Uiso 1 1 calc R . . O8 O 0.4512(4) 0.3337(4) 0.5403(2) 0.0637(19) Uani 0.622(10) 1 d P . . C8 C 0.0503(4) 0.5258(3) 0.2785(2) 0.0523(9) Uani 1 1 d . . . H8 H 0.0949 0.5008 0.2362 0.063 Uiso 1 1 calc R . . O9 O 0.5267(2) 0.1710(2) 0.45316(14) 0.0565(7) Uani 1 1 d . . . C9 C -0.0747(3) 0.5136(3) 0.2861(2) 0.0490(9) Uani 1 1 d . . . O10 O 0.4897(2) -0.0203(2) 0.40277(15) 0.0574(7) Uani 1 1 d . . . C10 C -0.1369(3) 0.5522(3) 0.3487(2) 0.0525(9) Uani 1 1 d . . . O11 O 0.3218(3) -0.1677(2) 0.40724(17) 0.0666(13) Uani 0.931(9) 1 d P . . C11 C -0.0774(4) 0.5997(3) 0.4011(2) 0.0547(10) Uani 1 1 d . . . O12 O 0.1399(2) -0.1346(2) 0.30723(15) 0.0585(7) Uani 1 1 d . . . C12 C 0.0482(4) 0.6075(3) 0.3913(2) 0.0514(9) Uani 1 1 d . . . O13 O -0.0313(3) 0.6878(2) 0.56584(16) 0.0767(9) Uani 1 1 d . . . H13 H -0.0527 0.6717 0.5242 0.092 Uiso 1 1 calc R . . C13 C 0.1146(3) 0.5727(3) 0.3297(2) 0.0483(9) Uani 1 1 d . . . O14 O -0.2829(3) -0.1196(3) 0.3453(2) 0.0858(10) Uani 1 1 d . . . H140 H -0.3401 -0.1107 0.3780 0.103 Uiso 1 1 calc R . . C14 C 0.2531(4) 0.5832(3) 0.3187(2) 0.0556(10) Uani 1 1 d . . . H14 H 0.2716 0.6391 0.3504 0.067 Uiso 1 1 calc R . . C15 C 0.3637(3) 0.3892(3) 0.3107(2) 0.0464(8) Uani 1 1 d . . . H15 H 0.3419 0.4024 0.2574 0.056 Uiso 1 1 calc R . . C16 C 0.3264(3) 0.4728(3) 0.3541(2) 0.0501(9) Uani 1 1 d . . . C17 C 0.3572(3) 0.4505(3) 0.4324(2) 0.0534(9) Uani 1 1 d . . . C18 C 0.4249(3) 0.3507(3) 0.4654(2) 0.0511(9) Uani 1 1 d . . . C19 C 0.4592(3) 0.2718(3) 0.4203(2) 0.0461(8) Uani 1 1 d . . . C20 C 0.4307(3) 0.2884(3) 0.3413(2) 0.0442(8) Uani 1 1 d . . . C21 C 0.4743(3) 0.1989(3) 0.2930(2) 0.0474(9) Uani 1 1 d . . . H21 H 0.5495 0.1569 0.3189 0.057 Uiso 1 1 calc R . . C22 C 0.2818(3) 0.1317(3) 0.2491(2) 0.0441(8) Uani 1 1 d . . . H22 H 0.2707 0.2021 0.2140 0.053 Uiso 1 1 calc R . . C23 C 0.3820(3) 0.1124(3) 0.2975(2) 0.0447(8) Uani 1 1 d . . . C24 C 0.3951(3) 0.0091(3) 0.3498(2) 0.0476(9) Uani 1 1 d . . . C25 C 0.3117(3) -0.0697(3) 0.3522(2) 0.0466(8) Uani 1 1 d . . . C26 C 0.2142(3) -0.0484(3) 0.3009(2) 0.0470(9) Uani 1 1 d . . . C27 C 0.1964(3) 0.0540(3) 0.24857(19) 0.0427(8) Uani 1 1 d . . . C28 C 0.0882(3) 0.0813(3) 0.1938(2) 0.0463(8) Uani 1 1 d . . . H28 H 0.0563 0.0079 0.1922 0.056 Uiso 1 1 calc R . . C29 C -0.1179(5) 0.5095(4) 0.1463(3) 0.0736(13) Uani 1 1 d . . . H29A H -0.0332 0.4836 0.1309 0.088 Uiso 1 1 calc R . . H29B H -0.1232 0.5924 0.1402 0.088 Uiso 1 1 calc R . . C30 C -0.2092(5) 0.4791(4) 0.0900(2) 0.0786(14) Uani 1 1 d . . . H30A H -0.1984 0.3968 0.0926 0.094 Uiso 1 1 calc R . . H30B H -0.2942 0.4986 0.1084 0.094 Uiso 1 1 calc R . . C31 C -0.1936(7) 0.5362(6) 0.0082(3) 0.126(2) Uani 1 1 d . . . H31A H -0.1108 0.5121 -0.0114 0.152 Uiso 1 1 calc R . . H31B H -0.1979 0.6183 0.0061 0.152 Uiso 1 1 calc R . . C32 C -0.2889(8) 0.5131(6) -0.0453(4) 0.157(3) Uani 1 1 d . . . H32A H -0.2723 0.4359 -0.0539 0.236 Uiso 1 1 calc R . . H32B H -0.2848 0.5658 -0.0956 0.236 Uiso 1 1 calc R . . H32C H -0.3710 0.5228 -0.0211 0.236 Uiso 1 1 calc R . . C33 C 0.2917(4) 0.6314(3) 0.2346(3) 0.0666(11) Uani 1 1 d . . . H33A H 0.2372 0.7003 0.2151 0.080 Uiso 1 1 calc R . . H33B H 0.2809 0.5761 0.2015 0.080 Uiso 1 1 calc R . . C34 C 0.4261(4) 0.6600(4) 0.2267(3) 0.0849(14) Uani 1 1 d . . . H34A H 0.4407 0.7040 0.2668 0.102 Uiso 1 1 calc R . . H34B H 0.4811 0.5893 0.2370 0.102 Uiso 1 1 calc R . . C35 C 0.4582(6) 0.7254(6) 0.1481(4) 0.126(2) Uani 1 1 d . . . H35A H 0.4212 0.6945 0.1073 0.152 Uiso 1 1 calc R . . H35B H 0.5485 0.7185 0.1396 0.152 Uiso 1 1 calc R . . C36 C 0.4090(10) 0.8543(9) 0.1414(6) 0.213(5) Uani 1 1 d . . . H36A H 0.3191 0.8613 0.1467 0.319 Uiso 1 1 calc R . . H36B H 0.4342 0.8970 0.0904 0.319 Uiso 1 1 calc R . . H36C H 0.4434 0.8840 0.1831 0.319 Uiso 1 1 calc R . . C37 C 0.5148(4) 0.2468(3) 0.2093(2) 0.0569(10) Uani 1 1 d . . . H37A H 0.5716 0.3049 0.2097 0.068 Uiso 1 1 calc R . . H37B H 0.4420 0.2832 0.1793 0.068 Uiso 1 1 calc R . . C38 C 0.5802(5) 0.1532(4) 0.1686(3) 0.0811(14) Uani 1 1 d . . . H38A H 0.6538 0.1193 0.1986 0.097 Uiso 1 1 calc R . . H38B H 0.5241 0.0935 0.1719 0.097 Uiso 1 1 calc R . . C39 C 0.6183(7) 0.1872(5) 0.0877(3) 0.119(2) Uani 1 1 d . . . H39A H 0.6755 0.2463 0.0829 0.143 Uiso 1 1 calc R . . H39B H 0.5456 0.2190 0.0561 0.143 Uiso 1 1 calc R . . C40 C 0.6829(7) 0.0849(6) 0.0563(5) 0.160(3) Uani 1 1 d . . . H40A H 0.7447 0.0449 0.0932 0.239 Uiso 1 1 calc R . . H40B H 0.7230 0.1112 0.0054 0.239 Uiso 1 1 calc R . . H40C H 0.6218 0.0339 0.0503 0.239 Uiso 1 1 calc R . . C41 C 0.1242(4) 0.1322(3) 0.1098(2) 0.0560(10) Uani 1 1 d . . . H41A H 0.1529 0.2070 0.1086 0.067 Uiso 1 1 calc R . . H41B H 0.1939 0.0839 0.0922 0.067 Uiso 1 1 calc R . . C42 C 0.0208(4) 0.1454(4) 0.0527(2) 0.0630(11) Uani 1 1 d . . . H42A H -0.0144 0.0724 0.0585 0.076 Uiso 1 1 calc R . . H42B H -0.0449 0.2006 0.0668 0.076 Uiso 1 1 calc R . . C43 C 0.0585(5) 0.1828(5) -0.0309(3) 0.0863(15) Uani 1 1 d . . . H43A H 0.1195 0.1246 -0.0461 0.104 Uiso 1 1 calc R . . H43B H 0.0999 0.2525 -0.0358 0.104 Uiso 1 1 calc R . . C44 C -0.0455(5) 0.2050(5) -0.0879(3) 0.0929(16) Uani 1 1 d . . . H44A H -0.0829 0.1351 -0.0869 0.139 Uiso 1 1 calc R . . H44B H -0.0131 0.2330 -0.1408 0.139 Uiso 1 1 calc R . . H44C H -0.1075 0.2614 -0.0729 0.139 Uiso 1 1 calc R . . C45 C -0.0998(10) 0.8743(5) 0.5220(4) 0.174(4) Uani 1 1 d . . . H45A H -0.0143 0.8924 0.5137 0.261 Uiso 1 1 calc R . . H45B H -0.1508 0.9384 0.5364 0.261 Uiso 1 1 calc R . . H45C H -0.1295 0.8583 0.4737 0.261 Uiso 1 1 calc R . . C46 C -0.1063(4) 0.7806(4) 0.5816(3) 0.0824(14) Uani 1 1 d . . . H46A H -0.1925 0.7615 0.5888 0.099 Uiso 1 1 calc R . . H46B H -0.0814 0.7988 0.6310 0.099 Uiso 1 1 calc R . . C47 C -0.2243(7) -0.1873(6) 0.2298(4) 0.132(2) Uani 1 1 d . . . H47A H -0.2042 -0.1142 0.1997 0.198 Uiso 1 1 calc R . . H47B H -0.2515 -0.2324 0.1944 0.198 Uiso 1 1 calc R . . H47C H -0.1513 -0.2266 0.2570 0.198 Uiso 1 1 calc R . . C48 C -0.3247(5) -0.1698(4) 0.2884(4) 0.1013(18) Uani 1 1 d . . . H48A H -0.3946 -0.1216 0.2618 0.122 Uiso 1 1 calc R . . H48B H -0.3540 -0.2432 0.3131 0.122 Uiso 1 1 calc R . . H3O H -0.2775 0.4072 0.3501 0.090 Uiso 1 1 d R . . H1O H -0.1599 -0.0455 0.3278 0.090 Uiso 1 1 d R . . H12O H 0.0495 -0.1098 0.3071 0.090 Uiso 1 1 d R . . H10O H 0.5090 0.0543 0.4203 0.090 Uiso 1 1 d R . . H9O H 0.5394 0.1592 0.5110 0.090 Uiso 1 1 d R . . H7O H 0.2427 0.5760 0.4686 0.090 Uiso 1 1 d R . . H6O H 0.0519 0.6720 0.4917 0.090 Uiso 1 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 O1 0.0548(16) 0.0398(14) 0.093(2) -0.0006(13) 0.0092(14) -0.0067(12) C1 0.051(2) 0.049(2) 0.0431(19) -0.0074(16) -0.0123(16) -0.0100(17) O2 0.054(2) 0.056(2) 0.084(3) -0.0047(19) 0.0050(18) -0.0084(16) C2 0.046(2) 0.043(2) 0.050(2) -0.0083(16) -0.0128(16) -0.0074(16) O3 0.0542(16) 0.0544(16) 0.0818(19) -0.0156(14) 0.0042(14) -0.0020(13) C3 0.043(2) 0.043(2) 0.064(2) -0.0034(18) -0.0111(18) -0.0056(16) O4 0.0579(17) 0.0705(18) 0.0674(17) -0.0300(14) -0.0083(13) -0.0046(13) C4 0.045(2) 0.054(2) 0.058(2) -0.0049(19) -0.0061(18) -0.0081(18) O5 0.082(11) 0.090(11) 0.118(13) -0.057(9) -0.046(9) 0.011(7) C5 0.042(2) 0.050(2) 0.059(2) -0.0092(18) -0.0098(18) 0.0007(16) O6 0.0620(16) 0.0507(15) 0.0626(16) -0.0219(12) -0.0198(13) -0.0020(12) C6 0.049(2) 0.0415(19) 0.049(2) -0.0090(16) -0.0161(17) -0.0034(16) O7 0.0701(18) 0.086(2) 0.080(2) -0.0519(17) -0.0283(15) 0.0159(15) C7 0.070(2) 0.043(2) 0.055(2) -0.0083(17) -0.0234(19) -0.0042(18) O8 0.057(3) 0.086(4) 0.050(3) -0.018(2) -0.014(2) 0.001(2) C8 0.069(3) 0.0359(19) 0.052(2) -0.0087(16) -0.0093(19) 0.0001(17) O9 0.0580(16) 0.0618(16) 0.0481(14) -0.0077(12) -0.0133(12) 0.0019(13) C9 0.056(2) 0.0390(19) 0.052(2) -0.0061(16) -0.0153(17) -0.0031(16) O10 0.0513(15) 0.0567(16) 0.0625(16) -0.0043(13) -0.0204(12) -0.0029(12) C10 0.053(2) 0.050(2) 0.056(2) -0.0126(18) -0.0153(18) -0.0016(17) O11 0.080(2) 0.0471(19) 0.069(2) -0.0035(14) -0.0206(16) 0.0020(14) C11 0.062(3) 0.047(2) 0.058(2) -0.0176(19) -0.016(2) 0.0021(19) O12 0.0574(15) 0.0410(14) 0.0757(18) -0.0016(12) -0.0150(13) -0.0117(12) C12 0.064(2) 0.040(2) 0.054(2) -0.0141(17) -0.0181(19) -0.0037(17) O13 0.099(2) 0.071(2) 0.0609(18) -0.0218(15) -0.0153(16) 0.0077(17) C13 0.056(2) 0.0340(18) 0.056(2) -0.0087(16) -0.0151(18) -0.0026(16) O14 0.070(2) 0.085(2) 0.111(3) -0.034(2) 0.0136(18) -0.0284(17) C14 0.068(3) 0.039(2) 0.062(2) -0.0134(18) -0.011(2) -0.0089(18) C15 0.047(2) 0.050(2) 0.044(2) -0.0096(16) -0.0076(16) -0.0126(17) C16 0.048(2) 0.048(2) 0.056(2) -0.0131(17) -0.0081(17) -0.0089(16) C17 0.050(2) 0.060(2) 0.057(2) -0.0242(19) -0.0118(18) -0.0041(18) C18 0.043(2) 0.067(2) 0.048(2) -0.0174(19) -0.0087(16) -0.0087(18) C19 0.0366(18) 0.052(2) 0.049(2) -0.0069(17) -0.0069(15) -0.0030(16) C20 0.0399(19) 0.047(2) 0.047(2) -0.0103(16) -0.0038(15) -0.0114(15) C21 0.0409(19) 0.052(2) 0.051(2) -0.0125(17) -0.0058(16) -0.0065(16) C22 0.049(2) 0.0388(18) 0.0440(19) -0.0061(15) -0.0049(16) -0.0031(15) C23 0.0397(19) 0.048(2) 0.048(2) -0.0134(16) -0.0019(16) -0.0044(15) C24 0.044(2) 0.048(2) 0.049(2) -0.0085(17) -0.0088(16) 0.0028(16) C25 0.051(2) 0.0386(19) 0.049(2) -0.0044(16) -0.0106(17) 0.0014(16) C26 0.049(2) 0.0396(19) 0.053(2) -0.0108(16) -0.0051(17) -0.0043(16) C27 0.0440(19) 0.0401(19) 0.0450(19) -0.0121(15) -0.0046(15) 0.0001(15) C28 0.050(2) 0.0420(19) 0.049(2) -0.0089(16) -0.0083(16) -0.0087(16) C29 0.101(3) 0.052(2) 0.069(3) -0.009(2) -0.022(2) -0.007(2) C30 0.119(4) 0.063(3) 0.057(3) -0.011(2) -0.036(3) -0.006(3) C31 0.177(7) 0.115(5) 0.087(4) -0.005(4) -0.044(4) -0.025(4) C32 0.260(10) 0.117(5) 0.101(5) -0.023(4) -0.107(6) 0.005(6) C33 0.074(3) 0.051(2) 0.074(3) -0.007(2) -0.008(2) -0.012(2) C34 0.077(3) 0.081(3) 0.096(4) -0.006(3) 0.002(3) -0.027(3) C35 0.120(5) 0.136(6) 0.122(5) -0.008(5) 0.022(4) -0.049(5) C36 0.264(12) 0.177(10) 0.181(9) 0.043(7) -0.017(8) -0.087(9) C37 0.060(2) 0.065(2) 0.049(2) -0.0126(19) -0.0008(18) -0.021(2) C38 0.098(4) 0.092(4) 0.061(3) -0.025(3) 0.014(2) -0.032(3) C39 0.165(6) 0.104(5) 0.098(4) -0.038(4) 0.036(4) -0.038(4) C40 0.171(7) 0.137(6) 0.183(8) -0.078(6) 0.078(6) -0.019(5) C41 0.062(2) 0.052(2) 0.054(2) -0.0079(18) -0.0110(19) -0.0076(18) C42 0.073(3) 0.061(2) 0.057(2) -0.015(2) -0.017(2) -0.005(2) C43 0.088(3) 0.105(4) 0.066(3) -0.015(3) -0.022(3) -0.005(3) C44 0.104(4) 0.105(4) 0.067(3) -0.010(3) -0.034(3) 0.003(3) C45 0.312(12) 0.072(4) 0.109(5) 0.006(4) 0.013(6) 0.059(5) C46 0.070(3) 0.094(4) 0.086(3) -0.031(3) -0.002(3) 0.005(3) C47 0.138(6) 0.132(6) 0.137(6) -0.055(5) 0.000(5) -0.002(5) C48 0.097(4) 0.081(4) 0.134(5) -0.034(4) -0.008(4) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.392(4) . ? O1 H1O 0.9674 . ? C1 C2 1.391(5) . ? C1 C6 1.406(5) . ? C1 H1 0.9500 . ? O2 C4 1.366(5) . ? C2 C3 1.387(5) . ? C2 C28 1.542(5) . ? O3 C5 1.371(4) . ? O3 H3O 1.0410 . ? C3 C4 1.378(5) . ? O4 C10 1.393(5) . ? O4 H4O 0.8400 . ? C4 C5 1.384(5) . ? O5 C11 1.185(15) . ? C5 C6 1.383(5) . ? O6 C12 1.389(4) . ? O6 H6O 1.0798 . ? C6 C7 1.543(5) . ? O7 C17 1.386(4) . ? O7 H7O 1.0639 . ? C7 C29 1.475(6) . ? C7 C9 1.537(5) . ? C7 H7 1.0000 . ? O8 C18 1.323(5) . ? C8 C9 1.387(5) . ? C8 C13 1.402(5) . ? C8 H8 0.9500 . ? O9 C19 1.400(4) . ? O9 H9O 1.0052 . ? C9 C10 1.394(5) . ? O10 C24 1.392(4) . ? O10 H10O 1.0592 . ? C10 C11 1.394(5) . ? O11 C25 1.374(4) . ? C11 C12 1.387(5) . ? O12 C26 1.377(4) . ? O12 H12O 1.0040 . ? C12 C13 1.382(5) . ? O13 C46 1.393(5) . ? O13 H13 0.8400 . ? C13 C14 1.534(5) . ? O14 C48 1.383(6) . ? O14 H140 0.8400 . ? C14 C33 1.525(6) . ? C14 C16 1.526(5) . ? C14 H14 1.0000 . ? C15 C20 1.386(5) . ? C15 C16 1.404(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(5) . ? C17 C18 1.392(5) . ? C18 C19 1.372(5) . ? C19 C20 1.400(5) . ? C20 C21 1.532(5) . ? C21 C23 1.521(5) . ? C21 C37 1.524(5) . ? C21 H21 1.0000 . ? C22 C23 1.389(5) . ? C22 C27 1.398(5) . ? C22 H22 0.9500 . ? C23 C24 1.399(5) . ? C24 C25 1.385(5) . ? C25 C26 1.397(5) . ? C26 C27 1.394(5) . ? C27 C28 1.526(5) . ? C28 C41 1.524(5) . ? C28 H28 1.0000 . ? C29 C30 1.554(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.469(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.517(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.539(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.487(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.591(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.558(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.443(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.553(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.519(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.490(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.516(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.389(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.491(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 O1 H1O 108.6 . . ? C2 C1 C6 123.0(3) . . ? C2 C1 H1 118.5 . . ? C6 C1 H1 118.5 . . ? C3 C2 C1 117.0(3) . . ? C3 C2 C28 120.0(3) . . ? C1 C2 C28 122.9(3) . . ? C5 O3 H3O 114.0 . . ? C4 C3 C2 121.5(3) . . ? C4 C3 O1 119.3(3) . . ? C2 C3 O1 119.2(3) . . ? C10 O4 H4O 109.5 . . ? O2 C4 C3 119.1(3) . . ? O2 C4 C5 120.6(4) . . ? C3 C4 C5 120.1(4) . . ? O3 C5 C6 124.6(3) . . ? O3 C5 C4 114.4(3) . . ? C6 C5 C4 121.0(4) . . ? C12 O6 H6O 112.6 . . ? C5 C6 C1 117.2(3) . . ? C5 C6 C7 120.6(3) . . ? C1 C6 C7 122.2(3) . . ? C17 O7 H7O 113.3 . . ? C29 C7 C9 113.5(3) . . ? C29 C7 C6 116.0(3) . . ? C9 C7 C6 110.5(3) . . ? C29 C7 H7 105.2 . . ? C9 C7 H7 105.2 . . ? C6 C7 H7 105.2 . . ? C9 C8 C13 124.0(4) . . ? C9 C8 H8 118.0 . . ? C13 C8 H8 118.0 . . ? C19 O9 H9O 115.6 . . ? C8 C9 C10 116.2(3) . . ? C8 C9 C7 122.2(4) . . ? C10 C9 C7 121.7(3) . . ? C24 O10 H10O 107.2 . . ? O4 C10 C11 120.4(4) . . ? O4 C10 C9 117.4(3) . . ? C11 C10 C9 122.2(4) . . ? O5 C11 C12 122.5(7) . . ? O5 C11 C10 118.4(7) . . ? C12 C11 C10 119.0(4) . . ? C26 O12 H12O 114.4 . . ? C13 C12 C11 121.6(3) . . ? C13 C12 O6 118.2(3) . . ? C11 C12 O6 120.3(3) . . ? C46 O13 H13 109.5 . . ? C12 C13 C8 117.2(3) . . ? C12 C13 C14 121.2(3) . . ? C8 C13 C14 121.7(3) . . ? C48 O14 H140 109.5 . . ? C33 C14 C16 114.0(3) . . ? C33 C14 C13 113.1(3) . . ? C16 C14 C13 110.8(3) . . ? C33 C14 H14 106.1 . . ? C16 C14 H14 106.1 . . ? C13 C14 H14 106.1 . . ? C20 C15 C16 123.7(3) . . ? C20 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C17 C16 C15 117.1(3) . . ? C17 C16 C14 120.3(3) . . ? C15 C16 C14 122.6(3) . . ? O7 C17 C18 115.7(3) . . ? O7 C17 C16 123.2(3) . . ? C18 C17 C16 121.1(3) . . ? O8 C18 C19 122.0(4) . . ? O8 C18 C17 118.6(4) . . ? C19 C18 C17 119.4(3) . . ? C18 C19 O9 119.7(3) . . ? C18 C19 C20 122.5(3) . . ? O9 C19 C20 117.7(3) . . ? C15 C20 C19 116.1(3) . . ? C15 C20 C21 123.5(3) . . ? C19 C20 C21 120.4(3) . . ? C23 C21 C37 112.7(3) . . ? C23 C21 C20 111.9(3) . . ? C37 C21 C20 114.0(3) . . ? C23 C21 H21 105.8 . . ? C37 C21 H21 105.8 . . ? C20 C21 H21 105.8 . . ? C23 C22 C27 124.2(3) . . ? C23 C22 H22 117.9 . . ? C27 C22 H22 117.9 . . ? C22 C23 C24 117.0(3) . . ? C22 C23 C21 121.5(3) . . ? C24 C23 C21 121.5(3) . . ? C25 C24 O10 116.2(3) . . ? C25 C24 C23 120.8(3) . . ? O10 C24 C23 123.0(3) . . ? O11 C25 C24 120.0(3) . . ? O11 C25 C26 119.5(3) . . ? C24 C25 C26 120.5(3) . . ? O12 C26 C27 124.4(3) . . ? O12 C26 C25 114.9(3) . . ? C27 C26 C25 120.7(3) . . ? C26 C27 C22 116.9(3) . . ? C26 C27 C28 121.9(3) . . ? C22 C27 C28 121.3(3) . . ? C41 C28 C27 113.6(3) . . ? C41 C28 C2 115.1(3) . . ? C27 C28 C2 108.8(3) . . ? C41 C28 H28 106.2 . . ? C27 C28 H28 106.2 . . ? C2 C28 H28 106.2 . . ? C7 C29 C30 113.7(4) . . ? C7 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C7 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C29 113.9(5) . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C30 C31 C32 113.7(6) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C14 C33 C34 112.7(4) . . ? C14 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C14 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 113.1(5) . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C34 C35 C36 110.3(6) . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C21 C37 C38 111.3(3) . . ? C21 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? C21 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C37 116.7(4) . . ? C39 C38 H38A 108.1 . . ? C37 C38 H38A 108.1 . . ? C39 C38 H38B 108.1 . . ? C37 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? C38 C39 C40 110.2(6) . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C28 114.0(3) . . ? C42 C41 H41A 108.7 . . ? C28 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C28 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C41 114.5(4) . . ? C43 C42 H42A 108.6 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 115.0(4) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C45 C46 O13 112.1(5) . . ? C45 C46 H46A 109.2 . . ? O13 C46 H46A 109.2 . . ? C45 C46 H46B 109.2 . . ? O13 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O14 C48 C47 110.4(5) . . ? O14 C48 H48A 109.6 . . ? C47 C48 H48A 109.6 . . ? O14 C48 H48B 109.6 . . ? C47 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? 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 C6 C1 C2 C3 -1.0(5) . . . . ? C6 C1 C2 C28 -176.1(3) . . . . ? C1 C2 C3 C4 -1.4(5) . . . . ? C28 C2 C3 C4 173.8(3) . . . . ? C1 C2 C3 O1 179.5(3) . . . . ? C28 C2 C3 O1 -5.3(5) . . . . ? C2 C3 C4 O2 -174.1(3) . . . . ? O1 C3 C4 O2 5.0(5) . . . . ? C2 C3 C4 C5 1.8(5) . . . . ? O1 C3 C4 C5 -179.1(3) . . . . ? O2 C4 C5 O3 -4.2(5) . . . . ? C3 C4 C5 O3 179.9(3) . . . . ? O2 C4 C5 C6 176.2(3) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? O3 C5 C6 C1 177.8(3) . . . . ? C4 C5 C6 C1 -2.6(5) . . . . ? O3 C5 C6 C7 -1.8(5) . . . . ? C4 C5 C6 C7 177.8(3) . . . . ? C2 C1 C6 C5 3.0(5) . . . . ? C2 C1 C6 C7 -177.4(3) . . . . ? C5 C6 C7 C29 -147.3(4) . . . . ? C1 C6 C7 C29 33.0(5) . . . . ? C5 C6 C7 C9 81.6(4) . . . . ? C1 C6 C7 C9 -98.0(4) . . . . ? C13 C8 C9 C10 0.5(5) . . . . ? C13 C8 C9 C7 -179.0(3) . . . . ? C29 C7 C9 C8 -51.4(5) . . . . ? C6 C7 C9 C8 81.0(4) . . . . ? C29 C7 C9 C10 129.2(4) . . . . ? C6 C7 C9 C10 -98.5(4) . . . . ? C8 C9 C10 O4 179.2(3) . . . . ? C7 C9 C10 O4 -1.3(5) . . . . ? C8 C9 C10 C11 -0.3(5) . . . . ? C7 C9 C10 C11 179.2(3) . . . . ? O4 C10 C11 O5 -5.3(10) . . . . ? C9 C10 C11 O5 174.2(9) . . . . ? O4 C10 C11 C12 179.5(3) . . . . ? C9 C10 C11 C12 -1.0(6) . . . . ? O5 C11 C12 C13 -172.9(9) . . . . ? C10 C11 C12 C13 2.1(5) . . . . ? O5 C11 C12 O6 6.7(10) . . . . ? C10 C11 C12 O6 -178.4(3) . . . . ? C11 C12 C13 C8 -1.9(5) . . . . ? O6 C12 C13 C8 178.6(3) . . . . ? C11 C12 C13 C14 179.1(3) . . . . ? O6 C12 C13 C14 -0.4(5) . . . . ? C9 C8 C13 C12 0.6(5) . . . . ? C9 C8 C13 C14 179.6(3) . . . . ? C12 C13 C14 C33 -134.3(4) . . . . ? C8 C13 C14 C33 46.7(4) . . . . ? C12 C13 C14 C16 96.3(4) . . . . ? C8 C13 C14 C16 -82.7(4) . . . . ? C20 C15 C16 C17 -1.3(5) . . . . ? C20 C15 C16 C14 179.7(3) . . . . ? C33 C14 C16 C17 143.1(4) . . . . ? C13 C14 C16 C17 -88.0(4) . . . . ? C33 C14 C16 C15 -38.0(5) . . . . ? C13 C14 C16 C15 90.9(4) . . . . ? C15 C16 C17 O7 179.2(3) . . . . ? C14 C16 C17 O7 -1.9(6) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? C14 C16 C17 C18 -179.5(3) . . . . ? O7 C17 C18 O8 2.5(5) . . . . ? C16 C17 C18 O8 -179.7(4) . . . . ? O7 C17 C18 C19 -179.3(3) . . . . ? C16 C17 C18 C19 -1.6(6) . . . . ? O8 C18 C19 O9 -1.6(6) . . . . ? C17 C18 C19 O9 -179.7(3) . . . . ? O8 C18 C19 C20 179.3(4) . . . . ? C17 C18 C19 C20 1.2(5) . . . . ? C16 C15 C20 C19 1.0(5) . . . . ? C16 C15 C20 C21 -178.2(3) . . . . ? C18 C19 C20 C15 -0.9(5) . . . . ? O9 C19 C20 C15 180.0(3) . . . . ? C18 C19 C20 C21 178.4(3) . . . . ? O9 C19 C20 C21 -0.8(5) . . . . ? C15 C20 C21 C23 -92.0(4) . . . . ? C19 C20 C21 C23 88.8(4) . . . . ? C15 C20 C21 C37 37.4(4) . . . . ? C19 C20 C21 C37 -141.8(3) . . . . ? C27 C22 C23 C24 -1.4(5) . . . . ? C27 C22 C23 C21 177.7(3) . . . . ? C37 C21 C23 C22 -46.2(5) . . . . ? C20 C21 C23 C22 83.9(4) . . . . ? C37 C21 C23 C24 132.9(4) . . . . ? C20 C21 C23 C24 -97.0(4) . . . . ? C22 C23 C24 C25 0.4(5) . . . . ? C21 C23 C24 C25 -178.8(3) . . . . ? C22 C23 C24 O10 -178.6(3) . . . . ? C21 C23 C24 O10 2.2(5) . . . . ? O10 C24 C25 O11 3.1(5) . . . . ? C23 C24 C25 O11 -176.0(3) . . . . ? O10 C24 C25 C26 -179.4(3) . . . . ? C23 C24 C25 C26 1.5(5) . . . . ? O11 C25 C26 O12 -4.5(5) . . . . ? C24 C25 C26 O12 178.0(3) . . . . ? O11 C25 C26 C27 175.0(3) . . . . ? C24 C25 C26 C27 -2.5(5) . . . . ? O12 C26 C27 C22 -179.1(3) . . . . ? C25 C26 C27 C22 1.5(5) . . . . ? O12 C26 C27 C28 1.6(5) . . . . ? C25 C26 C27 C28 -177.8(3) . . . . ? C23 C22 C27 C26 0.4(5) . . . . ? C23 C22 C27 C28 179.8(3) . . . . ? C26 C27 C28 C41 -133.8(3) . . . . ? C22 C27 C28 C41 46.9(4) . . . . ? C26 C27 C28 C2 96.7(4) . . . . ? C22 C27 C28 C2 -82.6(4) . . . . ? C3 C2 C28 C41 151.3(3) . . . . ? C1 C2 C28 C41 -33.8(4) . . . . ? C3 C2 C28 C27 -79.9(4) . . . . ? C1 C2 C28 C27 95.0(4) . . . . ? C9 C7 C29 C30 -164.9(4) . . . . ? C6 C7 C29 C30 65.5(5) . . . . ? C7 C29 C30 C31 174.8(5) . . . . ? C29 C30 C31 C32 -175.6(5) . . . . ? C16 C14 C33 C34 -61.8(5) . . . . ? C13 C14 C33 C34 170.4(3) . . . . ? C14 C33 C34 C35 -169.8(5) . . . . ? C33 C34 C35 C36 79.1(7) . . . . ? C23 C21 C37 C38 -61.6(4) . . . . ? C20 C21 C37 C38 169.4(3) . . . . ? C21 C37 C38 C39 177.4(5) . . . . ? C37 C38 C39 C40 179.4(5) . . . . ? C27 C28 C41 C42 172.3(3) . . . . ? C2 C28 C41 C42 -61.3(4) . . . . ? C28 C41 C42 C43 -173.4(4) . . . . ? C41 C42 C43 C44 -175.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.694 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.060