# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/240 data_ni278bc2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'beta-CD/4,7-dimethylcoumarin heptadecahydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H114 O54' _chemical_formula_weight 1615.44 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 'Monoclinic C' _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.513(4) _cell_length_b 24.024(5) _cell_length_c 16.414(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.49(3) _cell_angle_gamma 90.00 _cell_volume 7450(3) _cell_formula_units_Z 4 _cell_measurement_temperature 13(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .5 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 13(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker AXS rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MARResearch imaging plate' _diffrn_measurement_method 'oscillation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16934 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6956 _reflns_number_gt 6697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARDC' _computing_cell_refinement 'MARXDS' _computing_data_reduction 'MARXDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Insight II (MSI)' _computing_publication_material 'SHELXL-97' _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^)+(0.1619P)^2^+14.3252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.045(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.4(12) _refine_ls_number_reflns 6956 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 413 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.2027 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.125 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1_1 C 0.5612(3) 0.2397(3) 0.7336(3) 0.0164(13) Uani 1 1 d . . . H1_1 H 0.5868 0.2034 0.7367 0.020 Uiso 1 1 calc R . . C2_1 C 0.4887(3) 0.2352(3) 0.6703(3) 0.0177(13) Uani 1 1 d . . . H2_1 H 0.4622 0.2034 0.6871 0.021 Uiso 1 1 calc R . . C3_1 C 0.4467(3) 0.2874(3) 0.6706(3) 0.0152(12) Uani 1 1 d . . . H3_1 H 0.4716 0.3192 0.6510 0.018 Uiso 1 1 calc R . . C4_1 C 0.4405(3) 0.2991(3) 0.7596(3) 0.0168(12) Uani 1 1 d . . . H4_1 H 0.4148 0.2678 0.7793 0.020 Uiso 1 1 calc R . . C5_1 C 0.5151(3) 0.3043(3) 0.8171(4) 0.0225(14) Uani 1 1 d . . . H5_1 H 0.5401 0.3355 0.7962 0.027 Uiso 1 1 calc R . . C6_1 C 0.5172(4) 0.3149(4) 0.9089(4) 0.0313(16) Uani 1 1 d . . . H6A_1 H 0.4844 0.3455 0.9131 0.038 Uiso 1 1 calc R . . H6B_1 H 0.5017 0.2811 0.9338 0.038 Uiso 1 1 calc R . . O2_1 O 0.4995(2) 0.2237(2) 0.5885(2) 0.0206(10) Uani 1 1 d . . . O3_1 O 0.3778(2) 0.28076(19) 0.6143(2) 0.0202(10) Uani 1 1 d . . . O4_1 O 0.4018(2) 0.34958(18) 0.7581(2) 0.0166(9) Uani 1 1 d . . . O5_1 O 0.5531(2) 0.2541(2) 0.8143(2) 0.0200(10) Uani 1 1 d . . . O6_1 O 0.5886(3) 0.3296(3) 0.9553(3) 0.0405(14) Uani 1 1 d . . . C1_2 C 0.3407(3) 0.3487(3) 0.7907(4) 0.0181(13) Uani 1 1 d . . . H1_2 H 0.3297 0.3094 0.8029 0.022 Uiso 1 1 calc R . . C2_2 C 0.2793(3) 0.3726(3) 0.7251(4) 0.0180(13) Uani 1 1 d . . . H2_2 H 0.2362 0.3709 0.7476 0.022 Uiso 1 1 calc R . . C3_2 C 0.2921(3) 0.4324(3) 0.7067(4) 0.0175(13) Uani 1 1 d . . . H3_2 H 0.3338 0.4343 0.6817 0.021 Uiso 1 1 calc R . . C4_2 C 0.3088(3) 0.4658(3) 0.7877(4) 0.0148(12) Uani 1 1 d . . . H4_2 H 0.2652 0.4690 0.8091 0.018 Uiso 1 1 calc R . . C5_2 C 0.3681(3) 0.4377(3) 0.8549(4) 0.0174(13) Uani 1 1 d . . . H5_2 H 0.4134 0.4400 0.8371 0.021 Uiso 1 1 calc R . . C6_2 C 0.3778(3) 0.4654(3) 0.9396(4) 0.0221(14) Uani 1 1 d . . . H6A_2 H 0.3918 0.5047 0.9354 0.027 Uiso 1 1 calc R . . H6B_2 H 0.3323 0.4651 0.9559 0.027 Uiso 1 1 calc R . . O2_2 O 0.2665(2) 0.33939(19) 0.6496(2) 0.0205(9) Uani 1 1 d . . . O3_2 O 0.2325(2) 0.45604(19) 0.6487(3) 0.0211(10) Uani 1 1 d . . . O4_2 O 0.33193(19) 0.51982(18) 0.7715(2) 0.0156(9) Uani 1 1 d . . . O5_2 O 0.3518(2) 0.38060(19) 0.8655(2) 0.0183(9) Uani 1 1 d . . . O6_2 O 0.4315(2) 0.4373(2) 1.0040(3) 0.0273(11) Uani 1 1 d . . . C1_3 C 0.2920(3) 0.5667(3) 0.7851(3) 0.0146(12) Uani 1 1 d . . . H1_3 H 0.2466 0.5537 0.7966 0.018 Uiso 1 1 calc R . . C2_3 C 0.2755(3) 0.6023(3) 0.7050(4) 0.0152(12) Uani 1 1 d . . . H2_3 H 0.2478 0.6358 0.7141 0.018 Uiso 1 1 calc R . . C3_3 C 0.3445(3) 0.6213(3) 0.6876(4) 0.0195(13) Uani 1 1 d . . . H3_3 H 0.3734 0.5882 0.6802 0.023 Uiso 1 1 calc R . . C4_3 C 0.3843(3) 0.6554(3) 0.7618(4) 0.0147(12) Uani 1 1 d . . . H4_3 H 0.3579 0.6905 0.7663 0.018 Uiso 1 1 calc R . . C5_3 C 0.3958(3) 0.6215(3) 0.8440(3) 0.0148(12) Uani 1 1 d . . . H5_3 H 0.4299 0.5906 0.8433 0.018 Uiso 1 1 calc R . . C6_3 C 0.4235(3) 0.6574(3) 0.9202(3) 0.0145(12) Uani 1 1 d . . . H6A_3 H 0.4300 0.6343 0.9715 0.017 Uiso 1 1 calc R . . H6B_3 H 0.4703 0.6725 0.9185 0.017 Uiso 1 1 calc R . . O2_3 O 0.2341(2) 0.5706(2) 0.6370(3) 0.0275(11) Uani 1 1 d . . . O3_3 O 0.3287(2) 0.6541(2) 0.6122(2) 0.0247(10) Uani 1 1 d . . . O4_3 O 0.4528(2) 0.66820(18) 0.7480(2) 0.0167(9) Uani 1 1 d . . . O5_3 O 0.3300(2) 0.59877(18) 0.8541(2) 0.0151(9) Uani 1 1 d . . . O6_3 O 0.3774(2) 0.70178(19) 0.9245(2) 0.0204(9) Uani 1 1 d . . . C1_4 C 0.4774(3) 0.7239(3) 0.7615(3) 0.0161(12) Uani 1 1 d . . . H1_4 H 0.4408 0.7469 0.7789 0.019 Uiso 1 1 calc R . . C2_4 C 0.4886(3) 0.7463(3) 0.6786(3) 0.0145(12) Uani 1 1 d . . . H2_4 H 0.5053 0.7857 0.6870 0.017 Uiso 1 1 calc R . . C3_4 C 0.5438(3) 0.7119(2) 0.6513(3) 0.0103(11) Uani 1 1 d . . . H3_4 H 0.5277 0.6723 0.6425 0.012 Uiso 1 1 calc R . . C4_4 C 0.6125(3) 0.7153(3) 0.7225(3) 0.0159(13) Uani 1 1 d . . . H4_4 H 0.6304 0.7545 0.7295 0.019 Uiso 1 1 calc R . . C5_4 C 0.5984(3) 0.6941(3) 0.8048(4) 0.0210(14) Uani 1 1 d . . . H5_4 H 0.5844 0.6539 0.7988 0.025 Uiso 1 1 calc R . . C6_4 C 0.6647(3) 0.7012(3) 0.8779(3) 0.0203(14) Uani 1 1 d . . . H6A_4 H 0.6509 0.6976 0.9317 0.024 Uiso 1 1 calc R . . H6B_4 H 0.6983 0.6708 0.8754 0.024 Uiso 1 1 calc R . . O2_4 O 0.42264(18) 0.74472(19) 0.6148(2) 0.0167(9) Uani 1 1 d . . . O3_4 O 0.55699(19) 0.73390(18) 0.5753(2) 0.0152(9) Uani 1 1 d . . . O4_4 O 0.66320(19) 0.67963(17) 0.6994(2) 0.0128(9) Uani 1 1 d . . . O5_4 O 0.5414(2) 0.7269(2) 0.8243(2) 0.0200(10) Uani 1 1 d . . . O6_4 O 0.6999(2) 0.7532(2) 0.8773(2) 0.0237(10) Uani 1 1 d . . . C1_5 C 0.7301(3) 0.7040(2) 0.7017(3) 0.0124(12) Uani 1 1 d . . . H1_5 H 0.7268 0.7451 0.7094 0.015 Uiso 1 1 calc R . . C2_5 C 0.7461(3) 0.6931(2) 0.6176(3) 0.0128(12) Uani 1 1 d . . . H2_5 H 0.7915 0.7121 0.6168 0.015 Uiso 1 1 calc R . . C3_5 C 0.7549(3) 0.6311(3) 0.6061(3) 0.0144(12) Uani 1 1 d . . . H3_5 H 0.7093 0.6116 0.6044 0.017 Uiso 1 1 calc R . . C4_5 C 0.8125(3) 0.6091(2) 0.6795(3) 0.0118(12) Uani 1 1 d . . . H4_5 H 0.8595 0.6249 0.6779 0.014 Uiso 1 1 calc R . . C5_5 C 0.7954(3) 0.6231(3) 0.7632(3) 0.0146(12) Uani 1 1 d . . . H5_5 H 0.7517 0.6026 0.7669 0.018 Uiso 1 1 calc R . . C6_5 C 0.8539(3) 0.6106(3) 0.8410(4) 0.0225(14) Uani 1 1 d . . . H6A_5 H 0.8351 0.6138 0.8915 0.027 Uiso 1 1 calc R . . H6B_5 H 0.8705 0.5719 0.8380 0.027 Uiso 1 1 calc R . . O2_5 O 0.6912(2) 0.71457(18) 0.5505(2) 0.0176(9) Uani 1 1 d . . . O3_5 O 0.7757(2) 0.62027(19) 0.5304(2) 0.0221(10) Uani 1 1 d . . . O4_5 O 0.81282(19) 0.54971(17) 0.6712(2) 0.0141(9) Uani 1 1 d . . . O5_5 O 0.7830(2) 0.68256(18) 0.7680(2) 0.0159(9) Uani 1 1 d . . . O6_5 O 0.9122(3) 0.6479(3) 0.8486(3) 0.0409(13) Uani 1 1 d . . . C1_6 C 0.8791(3) 0.5231(2) 0.6745(4) 0.0131(12) Uani 1 1 d . . . H1_6 H 0.9166 0.5519 0.6772 0.016 Uiso 1 1 calc R . . C2_6 C 0.8700(3) 0.4884(3) 0.5935(4) 0.0166(12) Uani 1 1 d . . . H2_6 H 0.9164 0.4701 0.5949 0.020 Uiso 1 1 calc R . . C3_6 C 0.8155(3) 0.4433(3) 0.5895(4) 0.0157(12) Uani 1 1 d . . . H3_6 H 0.7681 0.4604 0.5853 0.019 Uiso 1 1 calc R . . C4_6 C 0.8372(3) 0.4087(3) 0.6696(4) 0.0167(13) Uani 1 1 d . . . H4_6 H 0.8822 0.3883 0.6711 0.020 Uiso 1 1 calc R . . C5_6 C 0.8467(3) 0.4457(3) 0.7476(3) 0.0135(12) Uani 1 1 d . . . H5_6 H 0.8005 0.4637 0.7474 0.016 Uiso 1 1 calc R . . C6_6 C 0.8723(3) 0.4134(3) 0.8282(4) 0.0228(14) Uani 1 1 d . . . H6A_6 H 0.8900 0.4399 0.8750 0.027 Uiso 1 1 calc R . . H6B_6 H 0.8319 0.3929 0.8402 0.027 Uiso 1 1 calc R . . O2_6 O 0.8517(2) 0.52319(19) 0.5202(3) 0.0224(10) Uani 1 1 d . . . O3_6 O 0.8123(2) 0.40809(19) 0.5179(2) 0.0227(10) Uani 1 1 d . . . O4_6 O 0.78054(19) 0.36937(18) 0.6677(2) 0.0157(9) Uani 1 1 d . . . O5_6 O 0.89808(19) 0.48807(19) 0.7454(2) 0.0183(9) Uani 1 1 d . . . O6_6 O 0.9286(2) 0.3739(2) 0.8248(3) 0.0311(11) Uani 1 1 d . . . C1_7 C 0.7998(3) 0.3130(3) 0.6776(4) 0.0157(12) Uani 1 1 d . . . H1_7 H 0.8498 0.3090 0.6733 0.019 Uiso 1 1 calc R . . C2_7 C 0.7509(3) 0.2805(3) 0.6051(3) 0.0145(12) Uani 1 1 d . . . H2_7 H 0.7638 0.2401 0.6108 0.017 Uiso 1 1 calc R . . C3_7 C 0.6748(3) 0.2874(3) 0.6113(3) 0.0159(12) Uani 1 1 d . . . H3_7 H 0.6603 0.3274 0.6028 0.019 Uiso 1 1 calc R . . C4_7 C 0.6702(3) 0.2680(3) 0.6982(4) 0.0159(13) Uani 1 1 d . . . H4_7 H 0.6772 0.2268 0.7030 0.019 Uiso 1 1 calc R . . C5_7 C 0.7239(3) 0.2969(3) 0.7689(3) 0.0163(12) Uani 1 1 d . . . H5_7 H 0.7114 0.3372 0.7697 0.020 Uiso 1 1 calc R . . C6_7 C 0.7277(3) 0.2713(3) 0.8558(3) 0.0178(13) Uani 1 1 d . . . H6A_7 H 0.7677 0.2880 0.8981 0.021 Uiso 1 1 calc R . . H6B_7 H 0.6835 0.2796 0.8727 0.021 Uiso 1 1 calc R . . O2_7 O 0.7587(2) 0.3003(2) 0.5260(2) 0.0211(10) Uani 1 1 d . . . O3_7 O 0.6285(2) 0.2536(2) 0.5503(2) 0.0215(10) Uani 1 1 d . . . O4_7 O 0.5999(2) 0.28180(18) 0.7043(2) 0.0164(9) Uani 1 1 d . . . O5_7 O 0.7946(2) 0.29155(19) 0.7555(2) 0.0176(9) Uani 1 1 d . . . O6_7 O 0.7373(2) 0.2119(2) 0.8529(2) 0.0226(10) Uani 1 1 d . . . O_8 O 0.6595(2) 0.1581(2) 0.9442(3) 0.0289(11) Uani 1 1 d . . . O_9 O 0.4330(2) 0.8028(2) 0.9518(3) 0.0243(10) Uani 1 1 d . . . O_10 O 0.6477(2) 0.2401(3) 1.0599(3) 0.0407(13) Uani 1 1 d . . . O_11 O 1.0586(3) 0.4183(3) 0.8415(4) 0.0467(14) Uani 1 1 d . . . O_12 O 0.6456(2) 0.8431(2) 0.9435(3) 0.0337(12) Uani 1 1 d . . . O_13 O 0.2691(2) 0.5842(3) 0.9964(3) 0.0382(13) Uani 1 1 d . . . O_14 O 1.0532(4) 0.5059(3) 0.9516(5) 0.0677(19) Uani 1 1 d . . . O_15 O 0.1247(4) 0.6355(4) 0.5853(5) 0.070(2) Uani 1 1 d . . . O_16 O 0.4478(4) 0.8479(3) 0.5516(5) 0.0599(18) Uani 1 1 d . . . O_17 O 0.1294(4) 0.3349(3) 0.6237(6) 0.0668(19) Uani 1 1 d . . . O_18 O 1.0426(3) 0.6026(3) 0.8544(6) 0.065(2) Uani 1 1 d . . . O_19 O 0.7638(3) 0.8901(3) 1.0578(5) 0.0623(18) Uani 1 1 d . . . O_20 O 0.8011(4) 0.4943(4) 0.9621(7) 0.095(3) Uani 1 1 d . . . OA_21 O 0.4666(7) 0.1110(5) 0.5777(8) 0.048(3) Uani 0.50 1 d P . . OB_21 O 0.0779(8) 0.6365(7) 0.4724(10) 0.063(4) Uani 0.50 1 d P . . OA_22 O 0.0507(5) 0.4091(6) 0.6719(7) 0.044(3) Uani 0.50 1 d P . . OB_22 O 0.0964(8) 0.4538(14) 0.6877(15) 0.136(12) Uani 0.50 1 d P . . OA_23 O 0.0671(9) 0.5008(9) 0.5929(12) 0.061(5) Uani 0.50 1 d P . . OB_23 O 0.0393(8) 0.5127(7) 0.5538(11) 0.049(4) Uani 0.50 1 d P . . OA_24 O 0.5327(8) 0.0967(8) 0.6695(11) 0.073(4) Uani 0.50 1 d P . . OB_24 O 0.6027(13) 0.0892(15) 0.727(2) 0.152(13) Uani 0.50 1 d P . . O1_25 O 0.5819(4) 0.5738(4) 0.5694(5) 0.074(4) Uani 0.50 1 d PGDU A 1 O2_25 O 0.5568(6) 0.6211(6) 0.4511(7) 0.110(7) Uani 0.50 1 d PGDU A 1 C2_25 C 0.5347(5) 0.5909(4) 0.4974(5) 0.066(6) Uani 0.50 1 d PGDU A 1 C3_25 C 0.4625(4) 0.5713(4) 0.4831(5) 0.052(5) Uani 0.50 1 d PGDU A 1 H3_25 H 0.4284 0.5824 0.4337 0.062 Uiso 0.50 1 calc PR A 1 C4_25 C 0.4429(3) 0.5374(4) 0.5394(5) 0.039(4) Uani 0.50 1 d PGDU A 1 C5_25 C 0.4772(4) 0.4852(4) 0.6749(5) 0.055(6) Uani 0.50 1 d PGDU A 1 H5_25 H 0.4305 0.4713 0.6672 0.066 Uiso 0.50 1 calc PR A 1 C6_25 C 0.5286(4) 0.4708(5) 0.7455(5) 0.075(6) Uani 0.50 1 d PGDU A 1 H6_25 H 0.5174 0.4469 0.7864 0.090 Uiso 0.50 1 calc PR A 1 C7_25 C 0.5967(4) 0.4912(5) 0.7570(4) 0.048(7) Uani 0.50 1 d PGDU A 1 C8_25 C 0.6146(3) 0.5256(4) 0.6984(4) 0.060(5) Uani 0.50 1 d PGDU A 1 H8_25 H 0.6614 0.5395 0.7067 0.073 Uiso 0.50 1 calc PR A 1 C9_25 C 0.5621(3) 0.5395(3) 0.6267(4) 0.051(4) Uani 0.50 1 d PGDU A 1 C10_25 C 0.4933(3) 0.5203(3) 0.6140(4) 0.036(4) Uani 0.50 1 d PGDU A 1 C11_25 C 0.3659(3) 0.5172(6) 0.5228(7) 0.133(15) Uani 0.50 1 d PGDU A 1 H11A_25 H 0.3608 0.4932 0.5693 0.199 Uiso 0.50 1 calc PR A 1 H11B_25 H 0.3536 0.4961 0.4701 0.199 Uiso 0.50 1 calc PR A 1 H11C_25 H 0.3343 0.5494 0.5186 0.199 Uiso 0.50 1 calc PR A 1 C12_25 C 0.6532(5) 0.4752(6) 0.8370(6) 0.061(6) Uani 0.50 1 d PGDU A 1 H12A_25 H 0.6322 0.4507 0.8719 0.092 Uiso 0.50 1 calc PR A 1 H12B_25 H 0.6714 0.5089 0.8687 0.092 Uiso 0.50 1 calc PR A 1 H12C_25 H 0.6922 0.4557 0.8213 0.092 Uiso 0.50 1 calc PR A 1 O1_26 O 0.4179(3) 0.5134(3) 0.6071(4) 0.061(4) Uani 0.50 1 d PGDU B 2 O2_26 O 0.3196(4) 0.5148(5) 0.5060(6) 0.125(9) Uani 0.50 1 d PGDU B 2 C2_26 C 0.3755(3) 0.4921(4) 0.5344(4) 0.063(6) Uani 0.50 1 d PGDU B 2 C3_26 C 0.4013(3) 0.4440(3) 0.4981(4) 0.057(5) Uani 0.50 1 d PGDU B 2 H3_26 H 0.3732 0.4282 0.4478 0.068 Uiso 0.50 1 calc PR B 2 C4_26 C 0.4652(3) 0.4213(3) 0.5352(4) 0.035(3) Uani 0.50 1 d PGDU B 2 C5_26 C 0.5748(3) 0.4239(3) 0.6527(4) 0.056(5) Uani 0.50 1 d PGDU B 2 H5_26 H 0.5938 0.3926 0.6304 0.067 Uiso 0.50 1 calc PR B 2 C6_26 C 0.6130(3) 0.4483(3) 0.7260(4) 0.061(5) Uani 0.50 1 d PGDU B 2 H6_26 H 0.6582 0.4339 0.7538 0.074 Uiso 0.50 1 calc PR B 2 C7_26 C 0.5857(3) 0.4937(3) 0.7591(3) 0.021(4) Uani 0.50 1 d PGDU B 2 C8_26 C 0.5205(3) 0.5155(3) 0.7195(3) 0.038(4) Uani 0.50 1 d PGDU B 2 H8_26 H 0.5019 0.5467 0.7424 0.045 Uiso 0.50 1 calc PR B 2 C9_26 C 0.4826(3) 0.4905(2) 0.6450(3) 0.031(4) Uani 0.50 1 d PGDU B 2 C10_26 C 0.5082(3) 0.4446(2) 0.6109(3) 0.029(3) Uani 0.50 1 d PGDU B 2 C11_26 C 0.4915(5) 0.3704(4) 0.4955(6) 0.060(5) Uani 0.50 1 d PGDU B 2 H11A_26 H 0.5382 0.3593 0.5298 0.090 Uiso 0.50 1 calc PR B 2 H11B_26 H 0.4951 0.3797 0.4385 0.090 Uiso 0.50 1 calc PR B 2 H11C_26 H 0.4581 0.3396 0.4927 0.090 Uiso 0.50 1 calc PR B 2 C12_26 C 0.6288(4) 0.5201(4) 0.8416(4) 0.031(3) Uani 0.50 1 d PGDU B 2 H12A_26 H 0.6735 0.4999 0.8615 0.047 Uiso 0.50 1 calc PR B 2 H12B_26 H 0.6016 0.5181 0.8842 0.047 Uiso 0.50 1 calc PR B 2 H12C_26 H 0.6387 0.5592 0.8315 0.047 Uiso 0.50 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 C1_1 0.023(3) 0.017(3) 0.010(3) 0.006(2) 0.006(2) 0.008(2) C2_1 0.031(3) 0.022(4) 0.003(2) -0.004(2) 0.009(2) -0.002(3) C3_1 0.012(2) 0.022(3) 0.008(3) 0.001(2) -0.0037(19) -0.004(2) C4_1 0.030(3) 0.011(3) 0.010(3) 0.002(2) 0.005(2) 0.008(3) C5_1 0.031(3) 0.027(4) 0.006(3) -0.002(3) -0.002(2) 0.014(3) C6_1 0.036(3) 0.042(4) 0.014(3) -0.001(3) 0.003(2) 0.016(3) O2_1 0.0225(19) 0.028(3) 0.0132(19) -0.0040(19) 0.0083(16) -0.0006(19) O3_1 0.021(2) 0.027(3) 0.0114(19) -0.0037(19) 0.0010(15) 0.0001(19) O4_1 0.023(2) 0.016(2) 0.0125(18) -0.0012(17) 0.0075(16) 0.0044(17) O5_1 0.031(2) 0.022(2) 0.0075(19) 0.0062(18) 0.0056(16) 0.014(2) O6_1 0.040(3) 0.053(4) 0.021(2) -0.012(3) -0.006(2) 0.019(3) C1_2 0.019(3) 0.023(3) 0.013(3) -0.002(3) 0.007(2) 0.001(3) C2_2 0.024(3) 0.019(3) 0.011(3) -0.003(3) 0.005(2) 0.001(3) C3_2 0.022(3) 0.018(3) 0.012(3) -0.003(2) 0.002(2) 0.002(2) C4_2 0.018(3) 0.012(3) 0.015(3) -0.001(2) 0.006(2) 0.002(2) C5_2 0.021(3) 0.020(3) 0.010(3) 0.004(3) 0.004(2) 0.004(3) C6_2 0.032(3) 0.019(3) 0.013(3) 0.001(3) 0.002(2) 0.010(3) O2_2 0.030(2) 0.017(2) 0.013(2) -0.0040(18) 0.0027(16) 0.0032(18) O3_2 0.023(2) 0.020(2) 0.015(2) -0.0004(18) -0.0059(16) 0.0037(18) O4_2 0.0183(19) 0.014(2) 0.0153(19) 0.0011(17) 0.0061(15) 0.0022(17) O5_2 0.029(2) 0.018(2) 0.0072(18) 0.0038(17) 0.0047(15) 0.0060(19) O6_2 0.033(2) 0.030(3) 0.016(2) -0.001(2) 0.0012(17) 0.007(2) C1_3 0.015(2) 0.016(3) 0.011(3) -0.003(3) 0.002(2) 0.003(2) C2_3 0.022(3) 0.010(3) 0.011(3) -0.003(2) -0.002(2) -0.003(2) C3_3 0.028(3) 0.020(3) 0.008(3) 0.001(3) 0.000(2) 0.000(3) C4_3 0.017(3) 0.015(3) 0.013(3) 0.001(2) 0.006(2) 0.000(2) C5_3 0.011(2) 0.023(3) 0.010(3) 0.000(2) 0.002(2) -0.003(2) C6_3 0.014(3) 0.021(3) 0.004(2) 0.005(2) -0.007(2) 0.001(2) O2_3 0.035(2) 0.029(3) 0.012(2) 0.001(2) -0.0041(17) -0.014(2) O3_3 0.040(2) 0.022(3) 0.0082(19) 0.0068(18) -0.0014(17) -0.004(2) O4_3 0.0148(18) 0.018(2) 0.019(2) 0.0005(18) 0.0077(15) 0.0000(17) O5_3 0.0187(19) 0.016(2) 0.0102(19) -0.0027(17) 0.0031(14) -0.0008(17) O6_3 0.024(2) 0.025(2) 0.0099(18) -0.0033(18) 0.0003(15) 0.0015(19) C1_4 0.015(3) 0.022(3) 0.011(3) -0.001(3) 0.003(2) 0.002(2) C2_4 0.013(2) 0.018(3) 0.009(3) 0.001(2) -0.005(2) -0.001(2) C3_4 0.010(2) 0.015(3) 0.005(2) -0.001(2) 0.0015(19) -0.001(2) C4_4 0.014(3) 0.027(4) 0.006(3) -0.003(2) 0.001(2) 0.006(2) C5_4 0.015(3) 0.035(4) 0.011(3) 0.002(3) -0.001(2) 0.007(3) C6_4 0.017(3) 0.037(4) 0.007(3) 0.004(3) 0.001(2) 0.002(3) O2_4 0.0109(17) 0.028(2) 0.0085(18) 0.0010(18) -0.0025(14) 0.0010(17) O3_4 0.0199(19) 0.019(2) 0.0058(18) 0.0031(16) 0.0026(14) 0.0013(17) O4_4 0.0144(17) 0.015(2) 0.0092(18) -0.0021(16) 0.0028(14) 0.0008(17) O5_4 0.0153(19) 0.031(3) 0.0136(19) -0.0054(19) 0.0045(15) 0.0015(19) O6_4 0.023(2) 0.037(3) 0.0088(19) -0.0084(19) -0.0008(15) 0.001(2) C1_5 0.013(3) 0.008(3) 0.013(3) 0.000(2) -0.002(2) 0.004(2) C2_5 0.015(2) 0.011(3) 0.012(3) 0.000(2) 0.003(2) 0.001(2) C3_5 0.014(2) 0.019(3) 0.008(3) -0.002(2) -0.001(2) 0.002(2) C4_5 0.016(3) 0.009(3) 0.008(3) 0.006(2) 0.000(2) 0.004(2) C5_5 0.019(3) 0.016(3) 0.007(3) -0.004(2) -0.001(2) 0.004(2) C6_5 0.026(3) 0.027(4) 0.009(3) 0.004(3) -0.007(2) 0.007(3) O2_5 0.0216(19) 0.020(2) 0.0089(18) 0.0027(18) 0.0002(15) 0.0083(17) O3_5 0.033(2) 0.023(2) 0.0103(19) 0.0005(18) 0.0065(16) 0.010(2) O4_5 0.0110(17) 0.014(2) 0.0167(19) -0.0001(17) 0.0018(14) 0.0063(16) O5_5 0.0188(19) 0.018(2) 0.0080(18) -0.0024(17) -0.0018(15) 0.0040(17) O6_5 0.033(3) 0.036(3) 0.041(3) 0.007(3) -0.014(2) -0.008(2) C1_6 0.010(2) 0.010(3) 0.019(3) 0.005(2) 0.003(2) 0.006(2) C2_6 0.018(3) 0.013(3) 0.019(3) 0.008(3) 0.004(2) 0.009(2) C3_6 0.020(3) 0.013(3) 0.012(3) 0.003(2) 0.000(2) 0.005(2) C4_6 0.019(3) 0.018(3) 0.012(3) 0.000(3) 0.003(2) -0.005(3) C5_6 0.008(2) 0.020(3) 0.011(3) 0.001(2) -0.002(2) 0.002(2) C6_6 0.017(3) 0.025(4) 0.022(3) 0.002(3) -0.002(2) 0.003(3) O2_6 0.032(2) 0.021(2) 0.017(2) 0.0096(19) 0.0106(17) 0.0092(19) O3_6 0.040(2) 0.019(2) 0.0094(19) -0.0032(18) 0.0064(17) 0.002(2) O4_6 0.0162(19) 0.015(2) 0.0144(19) -0.0028(18) 0.0018(15) -0.0018(17) O5_6 0.0149(18) 0.017(2) 0.018(2) 0.0063(19) -0.0052(15) 0.0018(18) O6_6 0.026(2) 0.034(3) 0.027(2) 0.014(2) -0.0034(18) 0.009(2) C1_7 0.019(3) 0.014(3) 0.013(3) -0.002(2) 0.001(2) 0.000(2) C2_7 0.022(3) 0.014(3) 0.006(3) 0.003(2) 0.002(2) 0.002(2) C3_7 0.020(3) 0.015(3) 0.011(3) -0.002(2) 0.002(2) 0.002(2) C4_7 0.016(3) 0.017(3) 0.013(3) -0.002(2) 0.001(2) 0.002(2) C5_7 0.021(3) 0.019(3) 0.009(3) 0.000(2) 0.004(2) 0.001(2) C6_7 0.021(3) 0.024(3) 0.006(3) 0.004(2) -0.002(2) -0.001(3) O2_7 0.026(2) 0.028(3) 0.0082(18) -0.0001(18) 0.0015(15) -0.0019(19) O3_7 0.0203(19) 0.032(3) 0.0105(19) -0.0036(19) 0.0005(15) -0.0077(19) O4_7 0.0189(19) 0.017(2) 0.0115(19) -0.0027(18) 0.0011(15) 0.0013(17) O5_7 0.020(2) 0.019(2) 0.0104(19) 0.0003(17) -0.0025(15) 0.0027(17) O6_7 0.030(2) 0.025(3) 0.0088(19) 0.0057(18) -0.0029(15) -0.0001(19) O_8 0.025(2) 0.031(3) 0.032(2) 0.005(2) 0.0098(17) 0.006(2) O_9 0.023(2) 0.025(3) 0.020(2) 0.0043(19) -0.0047(17) -0.0001(19) O_10 0.032(3) 0.046(4) 0.039(3) -0.012(3) 0.000(2) 0.008(2) O_11 0.038(3) 0.044(4) 0.057(3) 0.010(3) 0.011(2) 0.012(3) O_12 0.027(2) 0.037(3) 0.040(3) 0.000(2) 0.014(2) 0.002(2) O_13 0.030(2) 0.062(4) 0.023(2) 0.008(3) 0.0078(19) 0.019(3) O_14 0.065(4) 0.037(4) 0.093(5) 0.004(4) 0.006(4) 0.010(3) O_15 0.068(4) 0.072(5) 0.066(4) 0.001(4) 0.010(3) 0.012(4) O_16 0.068(4) 0.048(4) 0.072(4) 0.015(3) 0.034(3) 0.017(3) O_17 0.055(4) 0.049(4) 0.097(5) -0.004(4) 0.020(4) -0.014(3) O_18 0.036(3) 0.033(3) 0.116(6) -0.009(4) 0.003(3) -0.003(3) O_19 0.044(3) 0.042(4) 0.102(5) 0.004(4) 0.020(3) 0.000(3) O_20 0.068(5) 0.065(6) 0.137(8) -0.045(6) -0.005(5) 0.003(4) OA_21 0.067(7) 0.034(7) 0.041(6) 0.003(6) 0.010(6) -0.013(6) OB_21 0.065(8) 0.054(9) 0.075(10) 0.015(8) 0.025(8) 0.004(7) OA_22 0.030(5) 0.057(8) 0.046(6) -0.002(6) 0.012(5) -0.001(5) OB_22 0.042(8) 0.23(3) 0.144(17) 0.13(2) 0.047(9) 0.035(13) OA_23 0.051(10) 0.078(12) 0.058(11) 0.019(9) 0.022(7) 0.001(8) OB_23 0.051(9) 0.052(9) 0.049(9) -0.021(8) 0.023(7) -0.010(7) OA_24 0.068(9) 0.076(11) 0.087(10) -0.034(9) 0.041(8) -0.024(8) OB_24 0.107(16) 0.17(3) 0.19(3) -0.10(3) 0.055(17) -0.010(17) O1_25 0.065(8) 0.083(10) 0.078(9) 0.013(9) 0.024(7) -0.015(8) O2_25 0.086(11) 0.116(16) 0.135(16) 0.034(14) 0.040(11) -0.012(12) C2_25 0.073(11) 0.072(14) 0.069(12) 0.059(10) 0.045(9) 0.009(10) C3_25 0.038(8) 0.071(14) 0.043(9) -0.020(11) 0.001(7) 0.006(9) C4_25 0.039(7) 0.031(8) 0.044(8) -0.022(7) 0.005(6) 0.003(7) C5_25 0.026(8) 0.041(10) 0.084(13) 0.032(10) -0.013(9) -0.027(8) C6_25 0.040(9) 0.099(15) 0.080(12) 0.036(12) 0.003(8) -0.038(10) C7_25 0.018(7) 0.096(16) 0.028(11) 0.031(11) 0.000(7) -0.022(9) C8_25 0.035(7) 0.108(14) 0.037(8) 0.022(9) 0.006(6) -0.046(9) C9_25 0.041(7) 0.080(11) 0.038(8) 0.014(8) 0.022(6) 0.003(8) C10_25 0.027(7) 0.039(9) 0.041(8) -0.015(7) 0.004(6) 0.019(7) C11_25 0.16(3) 0.067(18) 0.12(2) 0.004(17) -0.07(2) -0.053(19) C12_25 0.050(10) 0.098(18) 0.029(8) 0.016(10) -0.003(7) -0.015(11) O1_26 0.031(5) 0.080(9) 0.067(8) -0.025(7) 0.000(5) 0.010(6) O2_26 0.062(10) 0.129(17) 0.152(17) -0.107(15) -0.032(10) 0.033(11) C2_26 0.019(7) 0.132(16) 0.033(8) -0.039(10) -0.003(6) -0.008(9) C3_26 0.061(10) 0.048(10) 0.041(8) -0.009(8) -0.025(8) 0.003(9) C4_26 0.047(8) 0.030(7) 0.035(7) 0.011(6) 0.025(6) -0.006(6) C5_26 0.040(8) 0.068(11) 0.059(9) -0.047(9) 0.013(7) -0.008(8) C6_26 0.075(11) 0.055(11) 0.045(9) -0.030(9) -0.003(8) 0.016(10) C7_26 0.040(9) 0.017(8) 0.009(8) -0.011(7) 0.008(7) 0.011(8) C8_26 0.044(8) 0.029(8) 0.037(8) -0.015(7) 0.006(6) 0.011(7) C9_26 0.037(8) 0.017(8) 0.033(8) 0.019(7) -0.002(6) -0.008(7) C10_26 0.043(7) 0.012(6) 0.029(7) -0.002(6) 0.006(5) -0.011(6) C11_26 0.051(10) 0.099(13) 0.038(7) 0.003(16) 0.027(7) 0.042(12) C12_26 0.044(8) 0.031(8) 0.015(6) -0.004(6) 0.000(6) -0.006(7) _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 C1_1 O5_1 1.415(7) . ? C1_1 O4_7 1.417(8) . ? C1_1 C2_1 1.535(8) . ? C2_1 O2_1 1.437(7) . ? C2_1 C3_1 1.498(9) . ? C3_1 O3_1 1.437(7) . ? C3_1 C4_1 1.524(8) . ? C4_1 O4_1 1.426(8) . ? C4_1 C5_1 1.530(8) . ? C5_1 O5_1 1.424(8) . ? C5_1 C6_1 1.519(9) . ? C6_1 O6_1 1.453(9) . ? O4_1 C1_2 1.425(7) . ? C1_2 O5_2 1.417(7) . ? C1_2 C2_2 1.509(9) . ? C2_2 O2_2 1.443(7) . ? C2_2 C3_2 1.503(9) . ? C3_2 O3_2 1.424(8) . ? C3_2 C4_2 1.516(8) . ? C4_2 O4_2 1.421(8) . ? C4_2 C5_2 1.540(8) . ? C5_2 O5_2 1.429(8) . ? C5_2 C6_2 1.509(8) . ? C6_2 O6_2 1.456(8) . ? O4_2 C1_3 1.419(7) . ? C1_3 O5_3 1.417(7) . ? C1_3 C2_3 1.534(8) . ? C2_3 O2_3 1.425(7) . ? C2_3 C3_3 1.515(9) . ? C3_3 O3_3 1.434(8) . ? C3_3 C4_3 1.511(9) . ? C4_3 O4_3 1.444(7) . ? C4_3 C5_3 1.544(8) . ? C5_3 O5_3 1.442(7) . ? C5_3 C6_3 1.503(8) . ? C6_3 O6_3 1.408(8) . ? O4_3 C1_4 1.420(8) . ? C1_4 O5_4 1.408(7) . ? C1_4 C2_4 1.529(8) . ? C2_4 O2_4 1.443(6) . ? C2_4 C3_4 1.512(8) . ? C3_4 O3_4 1.437(7) . ? C3_4 C4_4 1.545(7) . ? C4_4 O4_4 1.431(7) . ? C4_4 C5_4 1.532(8) . ? C5_4 O5_4 1.461(7) . ? C5_4 C6_4 1.539(8) . ? C6_4 O6_4 1.427(9) . ? O4_4 C1_5 1.422(7) . ? C1_5 O5_5 1.399(7) . ? C1_5 C2_5 1.511(8) . ? C2_5 O2_5 1.428(7) . ? C2_5 C3_5 1.516(9) . ? C3_5 O3_5 1.424(7) . ? C3_5 C4_5 1.522(8) . ? C4_5 O4_5 1.433(7) . ? C4_5 C5_5 1.530(8) . ? C5_5 O5_5 1.453(8) . ? C5_5 C6_5 1.514(8) . ? C6_5 O6_5 1.430(9) . ? O4_5 C1_6 1.431(7) . ? C1_6 O5_6 1.409(7) . ? C1_6 C2_6 1.542(9) . ? C2_6 O2_6 1.434(7) . ? C2_6 C3_6 1.509(9) . ? C3_6 O3_6 1.436(7) . ? C3_6 C4_6 1.523(8) . ? C4_6 O4_6 1.448(7) . ? C4_6 C5_6 1.532(8) . ? C5_6 O5_6 1.436(7) . ? C5_6 C6_6 1.506(9) . ? C6_6 O6_6 1.465(8) . ? O4_6 C1_7 1.404(8) . ? C1_7 O5_7 1.406(7) . ? C1_7 C2_7 1.539(8) . ? C2_7 O2_7 1.425(7) . ? C2_7 C3_7 1.523(8) . ? C3_7 O3_7 1.425(7) . ? C3_7 C4_7 1.525(8) . ? C4_7 O4_7 1.439(7) . ? C4_7 C5_7 1.521(8) . ? C5_7 O5_7 1.456(7) . ? C5_7 C6_7 1.538(8) . ? C6_7 O6_7 1.443(9) . ? OA_21 OB_21 1.20(2) 4_546 ? OA_21 OA_24 1.76(2) . ? OB_21 OA_21 1.20(2) 4_556 ? OA_22 OB_22 1.38(3) . ? OA_23 OB_23 0.783(16) . ? OA_24 OB_24 1.46(3) . ? O1_25 C2_25 1.3676 . ? O1_25 C9_25 1.3744 . ? O2_25 C2_25 1.2059 . ? C2_25 C3_25 1.4465 . ? C3_25 C4_25 1.3563 . ? C4_25 C10_25 1.4251 . ? C4_25 C11_25 1.5371 . ? C5_25 C6_25 1.3733 . ? C5_25 C10_25 1.4010 . ? C6_25 C7_25 1.3845 . ? C7_25 C8_25 1.3771 . ? C7_25 C12_25 1.5368 . ? C8_25 C9_25 1.3944 . ? C9_25 C10_25 1.3854 . ? O1_26 C2_26 1.3708 . ? O1_26 C9_26 1.3749 . ? O2_26 C2_26 1.2056 . ? C2_26 C3_26 1.4451 . ? C3_26 C4_26 1.3567 . ? C4_26 C10_26 1.4285 . ? C4_26 C11_26 1.5347 . ? C5_26 C6_26 1.3772 . ? C5_26 C10_26 1.3990 . ? C6_26 C7_26 1.3846 . ? C7_26 C8_26 1.3784 . ? C7_26 C12_26 1.5405 . ? C8_26 C9_26 1.3970 . ? C9_26 C10_26 1.3869 . ? 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 O5_1 C1_1 O4_7 109.6(5) . . ? O5_1 C1_1 C2_1 110.6(4) . . ? O4_7 C1_1 C2_1 107.4(4) . . ? O2_1 C2_1 C3_1 111.8(5) . . ? O2_1 C2_1 C1_1 108.7(4) . . ? C3_1 C2_1 C1_1 110.6(5) . . ? O3_1 C3_1 C2_1 109.2(5) . . ? O3_1 C3_1 C4_1 110.5(4) . . ? C2_1 C3_1 C4_1 109.4(5) . . ? O4_1 C4_1 C3_1 108.0(5) . . ? O4_1 C4_1 C5_1 111.0(5) . . ? C3_1 C4_1 C5_1 108.3(5) . . ? O5_1 C5_1 C6_1 106.8(5) . . ? O5_1 C5_1 C4_1 109.4(5) . . ? C6_1 C5_1 C4_1 114.3(5) . . ? O6_1 C6_1 C5_1 110.2(6) . . ? C1_2 O4_1 C4_1 118.1(5) . . ? C1_1 O5_1 C5_1 114.7(4) . . ? O5_2 C1_2 O4_1 110.9(5) . . ? O5_2 C1_2 C2_2 109.6(5) . . ? O4_1 C1_2 C2_2 108.4(5) . . ? O2_2 C2_2 C3_2 111.0(5) . . ? O2_2 C2_2 C1_2 109.8(5) . . ? C3_2 C2_2 C1_2 111.4(5) . . ? O3_2 C3_2 C2_2 111.5(5) . . ? O3_2 C3_2 C4_2 109.6(5) . . ? C2_2 C3_2 C4_2 109.8(5) . . ? O4_2 C4_2 C3_2 109.1(5) . . ? O4_2 C4_2 C5_2 108.5(5) . . ? C3_2 C4_2 C5_2 110.7(5) . . ? O5_2 C5_2 C6_2 107.0(5) . . ? O5_2 C5_2 C4_2 111.0(5) . . ? C6_2 C5_2 C4_2 111.4(5) . . ? O6_2 C6_2 C5_2 111.5(5) . . ? C1_3 O4_2 C4_2 118.8(4) . . ? C1_2 O5_2 C5_2 113.8(4) . . ? O5_3 C1_3 O4_2 111.0(4) . . ? O5_3 C1_3 C2_3 109.7(5) . . ? O4_2 C1_3 C2_3 108.3(4) . . ? O2_3 C2_3 C3_3 111.7(5) . . ? O2_3 C2_3 C1_3 109.2(5) . . ? C3_3 C2_3 C1_3 108.9(5) . . ? O3_3 C3_3 C4_3 110.7(5) . . ? O3_3 C3_3 C2_3 108.6(5) . . ? C4_3 C3_3 C2_3 108.3(5) . . ? O4_3 C4_3 C3_3 107.3(4) . . ? O4_3 C4_3 C5_3 108.2(4) . . ? C3_3 C4_3 C5_3 110.6(5) . . ? O5_3 C5_3 C6_3 105.5(4) . . ? O5_3 C5_3 C4_3 111.2(4) . . ? C6_3 C5_3 C4_3 111.6(5) . . ? O6_3 C6_3 C5_3 111.9(4) . . ? C1_4 O4_3 C4_3 117.8(4) . . ? C1_3 O5_3 C5_3 114.7(4) . . ? O5_4 C1_4 O4_3 111.5(5) . . ? O5_4 C1_4 C2_4 109.6(4) . . ? O4_3 C1_4 C2_4 108.1(5) . . ? O2_4 C2_4 C3_4 110.0(5) . . ? O2_4 C2_4 C1_4 109.8(4) . . ? C3_4 C2_4 C1_4 110.0(5) . . ? O3_4 C3_4 C2_4 110.7(4) . . ? O3_4 C3_4 C4_4 109.1(4) . . ? C2_4 C3_4 C4_4 107.1(4) . . ? O4_4 C4_4 C5_4 108.8(5) . . ? O4_4 C4_4 C3_4 107.1(4) . . ? C5_4 C4_4 C3_4 109.6(4) . . ? O5_4 C5_4 C4_4 109.1(5) . . ? O5_4 C5_4 C6_4 107.8(5) . . ? C4_4 C5_4 C6_4 110.4(5) . . ? O6_4 C6_4 C5_4 113.9(5) . . ? C1_5 O4_4 C4_4 115.9(4) . . ? C1_4 O5_4 C5_4 113.3(4) . . ? O5_5 C1_5 O4_4 111.3(4) . . ? O5_5 C1_5 C2_5 111.4(4) . . ? O4_4 C1_5 C2_5 107.6(4) . . ? O2_5 C2_5 C1_5 110.8(4) . . ? O2_5 C2_5 C3_5 110.2(5) . . ? C1_5 C2_5 C3_5 109.9(5) . . ? O3_5 C3_5 C2_5 110.7(5) . . ? O3_5 C3_5 C4_5 108.2(4) . . ? C2_5 C3_5 C4_5 109.0(5) . . ? O4_5 C4_5 C3_5 106.9(5) . . ? O4_5 C4_5 C5_5 108.2(4) . . ? C3_5 C4_5 C5_5 110.6(4) . . ? O5_5 C5_5 C6_5 104.5(5) . . ? O5_5 C5_5 C4_5 110.0(5) . . ? C6_5 C5_5 C4_5 115.2(5) . . ? O6_5 C6_5 C5_5 111.3(5) . . ? C1_6 O4_5 C4_5 117.8(4) . . ? C1_5 O5_5 C5_5 114.8(4) . . ? O5_6 C1_6 O4_5 110.3(4) . . ? O5_6 C1_6 C2_6 109.9(5) . . ? O4_5 C1_6 C2_6 107.5(4) . . ? O2_6 C2_6 C3_6 111.0(5) . . ? O2_6 C2_6 C1_6 111.0(5) . . ? C3_6 C2_6 C1_6 110.7(5) . . ? O3_6 C3_6 C2_6 110.1(5) . . ? O3_6 C3_6 C4_6 109.3(5) . . ? C2_6 C3_6 C4_6 108.3(5) . . ? O4_6 C4_6 C3_6 106.9(5) . . ? O4_6 C4_6 C5_6 109.2(4) . . ? C3_6 C4_6 C5_6 110.8(5) . . ? O5_6 C5_6 C6_6 107.9(4) . . ? O5_6 C5_6 C4_6 109.3(4) . . ? C6_6 C5_6 C4_6 112.3(5) . . ? O6_6 C6_6 C5_6 112.7(5) . . ? C1_7 O4_6 C4_6 116.4(4) . . ? C1_6 O5_6 C5_6 113.8(4) . . ? O4_6 C1_7 O5_7 112.3(5) . . ? O4_6 C1_7 C2_7 107.7(5) . . ? O5_7 C1_7 C2_7 110.1(5) . . ? O2_7 C2_7 C3_7 110.6(4) . . ? O2_7 C2_7 C1_7 110.3(5) . . ? C3_7 C2_7 C1_7 108.6(5) . . ? O3_7 C3_7 C2_7 110.3(4) . . ? O3_7 C3_7 C4_7 107.9(5) . . ? C2_7 C3_7 C4_7 108.4(4) . . ? O4_7 C4_7 C5_7 109.2(4) . . ? O4_7 C4_7 C3_7 106.0(4) . . ? C5_7 C4_7 C3_7 112.5(5) . . ? O5_7 C5_7 C4_7 110.0(4) . . ? O5_7 C5_7 C6_7 106.1(4) . . ? C4_7 C5_7 C6_7 112.9(5) . . ? O6_7 C6_7 C5_7 110.0(5) . . ? C1_1 O4_7 C4_7 117.3(5) . . ? C1_7 O5_7 C5_7 113.1(4) . . ? OB_21 OA_21 OA_24 159.5(13) 4_546 . ? OB_24 OA_24 OA_21 160.7(17) . . ? C2_25 O1_25 C9_25 121.9 . . ? O2_25 C2_25 O1_25 117.1 . . ? O2_25 C2_25 C3_25 125.5 . . ? O1_25 C2_25 C3_25 117.3 . . ? C4_25 C3_25 C2_25 120.9 . . ? C3_25 C4_25 C10_25 120.4 . . ? C3_25 C4_25 C11_25 119.9 . . ? C10_25 C4_25 C11_25 119.7 . . ? C6_25 C5_25 C10_25 120.5 . . ? C5_25 C6_25 C7_25 120.0 . . ? C8_25 C7_25 C6_25 121.2 . . ? C8_25 C7_25 C12_25 119.6 . . ? C6_25 C7_25 C12_25 119.2 . . ? C7_25 C8_25 C9_25 118.2 . . ? O1_25 C9_25 C10_25 121.6 . . ? O1_25 C9_25 C8_25 116.7 . . ? C10_25 C9_25 C8_25 121.7 . . ? C9_25 C10_25 C5_25 118.3 . . ? C9_25 C10_25 C4_25 117.9 . . ? C5_25 C10_25 C4_25 123.8 . . ? C2_26 O1_26 C9_26 121.9 . . ? O2_26 C2_26 O1_26 117.2 . . ? O2_26 C2_26 C3_26 125.3 . . ? O1_26 C2_26 C3_26 117.5 . . ? C4_26 C3_26 C2_26 120.8 . . ? C3_26 C4_26 C10_26 120.5 . . ? C3_26 C4_26 C11_26 119.9 . . ? C10_26 C4_26 C11_26 119.7 . . ? C6_26 C5_26 C10_26 120.7 . . ? C5_26 C6_26 C7_26 120.1 . . ? C8_26 C7_26 C6_26 121.0 . . ? C8_26 C7_26 C12_26 119.6 . . ? C6_26 C7_26 C12_26 119.4 . . ? C7_26 C8_26 C9_26 118.3 . . ? O1_26 C9_26 C10_26 121.4 . . ? O1_26 C9_26 C8_26 116.7 . . ? C10_26 C9_26 C8_26 121.9 . . ? C9_26 C10_26 C5_26 118.0 . . ? C9_26 C10_26 C4_26 118.0 . . ? C5_26 C10_26 C4_26 124.0 . . ? 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 O5_1 C1_1 C2_1 O2_1 176.7(5) . . . . ? O4_7 C1_1 C2_1 O2_1 57.1(6) . . . . ? O5_1 C1_1 C2_1 C3_1 53.6(6) . . . . ? O4_7 C1_1 C2_1 C3_1 -66.0(5) . . . . ? O2_1 C2_1 C3_1 O3_1 62.1(6) . . . . ? C1_1 C2_1 C3_1 O3_1 -176.7(4) . . . . ? O2_1 C2_1 C3_1 C4_1 -176.9(5) . . . . ? C1_1 C2_1 C3_1 C4_1 -55.7(6) . . . . ? O3_1 C3_1 C4_1 O4_1 -61.1(6) . . . . ? C2_1 C3_1 C4_1 O4_1 178.6(5) . . . . ? O3_1 C3_1 C4_1 C5_1 178.6(5) . . . . ? C2_1 C3_1 C4_1 C5_1 58.4(6) . . . . ? O4_1 C4_1 C5_1 O5_1 -177.5(4) . . . . ? C3_1 C4_1 C5_1 O5_1 -59.1(6) . . . . ? O4_1 C4_1 C5_1 C6_1 62.8(7) . . . . ? C3_1 C4_1 C5_1 C6_1 -178.8(6) . . . . ? O5_1 C5_1 C6_1 O6_1 69.5(8) . . . . ? C4_1 C5_1 C6_1 O6_1 -169.3(6) . . . . ? C3_1 C4_1 O4_1 C1_2 125.6(5) . . . . ? C5_1 C4_1 O4_1 C1_2 -115.8(5) . . . . ? O4_7 C1_1 O5_1 C5_1 61.4(6) . . . . ? C2_1 C1_1 O5_1 C5_1 -56.8(7) . . . . ? C6_1 C5_1 O5_1 C1_1 -175.6(5) . . . . ? C4_1 C5_1 O5_1 C1_1 60.2(6) . . . . ? C4_1 O4_1 C1_2 O5_2 112.2(5) . . . . ? C4_1 O4_1 C1_2 C2_2 -127.5(5) . . . . ? O5_2 C1_2 C2_2 O2_2 -178.4(5) . . . . ? O4_1 C1_2 C2_2 O2_2 60.4(6) . . . . ? O5_2 C1_2 C2_2 C3_2 58.3(6) . . . . ? O4_1 C1_2 C2_2 C3_2 -62.9(6) . . . . ? O2_2 C2_2 C3_2 O3_2 60.9(6) . . . . ? C1_2 C2_2 C3_2 O3_2 -176.5(4) . . . . ? O2_2 C2_2 C3_2 C4_2 -177.4(4) . . . . ? C1_2 C2_2 C3_2 C4_2 -54.7(6) . . . . ? O3_2 C3_2 C4_2 O4_2 -66.5(6) . . . . ? C2_2 C3_2 C4_2 O4_2 170.6(4) . . . . ? O3_2 C3_2 C4_2 C5_2 174.1(5) . . . . ? C2_2 C3_2 C4_2 C5_2 51.3(6) . . . . ? O4_2 C4_2 C5_2 O5_2 -172.1(4) . . . . ? C3_2 C4_2 C5_2 O5_2 -52.4(6) . . . . ? O4_2 C4_2 C5_2 C6_2 68.9(6) . . . . ? C3_2 C4_2 C5_2 C6_2 -171.4(5) . . . . ? O5_2 C5_2 C6_2 O6_2 55.9(6) . . . . ? C4_2 C5_2 C6_2 O6_2 177.4(5) . . . . ? C3_2 C4_2 O4_2 C1_3 118.4(5) . . . . ? C5_2 C4_2 O4_2 C1_3 -120.8(5) . . . . ? O4_1 C1_2 O5_2 C5_2 59.3(6) . . . . ? C2_2 C1_2 O5_2 C5_2 -60.4(6) . . . . ? C6_2 C5_2 O5_2 C1_2 179.7(4) . . . . ? C4_2 C5_2 O5_2 C1_2 58.0(6) . . . . ? C4_2 O4_2 C1_3 O5_3 111.6(5) . . . . ? C4_2 O4_2 C1_3 C2_3 -127.9(5) . . . . ? O5_3 C1_3 C2_3 O2_3 -177.0(4) . . . . ? O4_2 C1_3 C2_3 O2_3 61.7(6) . . . . ? O5_3 C1_3 C2_3 C3_3 60.8(6) . . . . ? O4_2 C1_3 C2_3 C3_3 -60.5(6) . . . . ? O2_3 C2_3 C3_3 O3_3 58.7(7) . . . . ? C1_3 C2_3 C3_3 O3_3 179.4(5) . . . . ? O2_3 C2_3 C3_3 C4_3 178.9(5) . . . . ? C1_3 C2_3 C3_3 C4_3 -60.4(6) . . . . ? O3_3 C3_3 C4_3 O4_3 -66.9(6) . . . . ? C2_3 C3_3 C4_3 O4_3 174.2(5) . . . . ? O3_3 C3_3 C4_3 C5_3 175.4(4) . . . . ? C2_3 C3_3 C4_3 C5_3 56.4(6) . . . . ? O4_3 C4_3 C5_3 O5_3 -169.6(5) . . . . ? C3_3 C4_3 C5_3 O5_3 -52.4(6) . . . . ? O4_3 C4_3 C5_3 C6_3 72.8(6) . . . . ? C3_3 C4_3 C5_3 C6_3 -169.9(5) . . . . ? O5_3 C5_3 C6_3 O6_3 -62.2(6) . . . . ? C4_3 C5_3 C6_3 O6_3 58.7(6) . . . . ? C3_3 C4_3 O4_3 C1_4 133.7(5) . . . . ? C5_3 C4_3 O4_3 C1_4 -107.0(5) . . . . ? O4_2 C1_3 O5_3 C5_3 61.3(6) . . . . ? C2_3 C1_3 O5_3 C5_3 -58.4(6) . . . . ? C6_3 C5_3 O5_3 C1_3 175.4(5) . . . . ? C4_3 C5_3 O5_3 C1_3 54.2(7) . . . . ? C4_3 O4_3 C1_4 O5_4 120.0(5) . . . . ? C4_3 O4_3 C1_4 C2_4 -119.4(5) . . . . ? O5_4 C1_4 C2_4 O2_4 -178.4(5) . . . . ? O4_3 C1_4 C2_4 O2_4 59.8(6) . . . . ? O5_4 C1_4 C2_4 C3_4 60.4(6) . . . . ? O4_3 C1_4 C2_4 C3_4 -61.3(5) . . . . ? O2_4 C2_4 C3_4 O3_4 61.4(6) . . . . ? C1_4 C2_4 C3_4 O3_4 -177.6(4) . . . . ? O2_4 C2_4 C3_4 C4_4 -179.8(5) . . . . ? C1_4 C2_4 C3_4 C4_4 -58.8(6) . . . . ? O3_4 C3_4 C4_4 O4_4 -64.2(6) . . . . ? C2_4 C3_4 C4_4 O4_4 176.0(4) . . . . ? O3_4 C3_4 C4_4 C5_4 177.9(5) . . . . ? C2_4 C3_4 C4_4 C5_4 58.1(7) . . . . ? O4_4 C4_4 C5_4 O5_4 -174.3(5) . . . . ? C3_4 C4_4 C5_4 O5_4 -57.5(7) . . . . ? O4_4 C4_4 C5_4 C6_4 67.4(7) . . . . ? C3_4 C4_4 C5_4 C6_4 -175.8(5) . . . . ? O5_4 C5_4 C6_4 O6_4 -76.6(6) . . . . ? C4_4 C5_4 C6_4 O6_4 42.5(7) . . . . ? C5_4 C4_4 O4_4 C1_5 -113.5(5) . . . . ? C3_4 C4_4 O4_4 C1_5 128.0(5) . . . . ? O4_3 C1_4 O5_4 C5_4 58.9(6) . . . . ? C2_4 C1_4 O5_4 C5_4 -60.7(7) . . . . ? C4_4 C5_4 O5_4 C1_4 59.9(7) . . . . ? C6_4 C5_4 O5_4 C1_4 179.8(5) . . . . ? C4_4 O4_4 C1_5 O5_5 109.6(5) . . . . ? C4_4 O4_4 C1_5 C2_5 -128.0(5) . . . . ? O5_5 C1_5 C2_5 O2_5 179.3(4) . . . . ? O4_4 C1_5 C2_5 O2_5 57.0(6) . . . . ? O5_5 C1_5 C2_5 C3_5 57.3(6) . . . . ? O4_4 C1_5 C2_5 C3_5 -65.0(5) . . . . ? O2_5 C2_5 C3_5 O3_5 62.4(5) . . . . ? C1_5 C2_5 C3_5 O3_5 -175.3(4) . . . . ? O2_5 C2_5 C3_5 C4_5 -178.7(4) . . . . ? C1_5 C2_5 C3_5 C4_5 -56.4(6) . . . . ? O3_5 C3_5 C4_5 O4_5 -66.3(6) . . . . ? C2_5 C3_5 C4_5 O4_5 173.2(4) . . . . ? O3_5 C3_5 C4_5 C5_5 176.1(5) . . . . ? C2_5 C3_5 C4_5 C5_5 55.6(6) . . . . ? O4_5 C4_5 C5_5 O5_5 -170.6(4) . . . . ? C3_5 C4_5 C5_5 O5_5 -53.9(6) . . . . ? O4_5 C4_5 C5_5 C6_5 71.6(6) . . . . ? C3_5 C4_5 C5_5 C6_5 -171.7(5) . . . . ? O5_5 C5_5 C6_5 O6_5 -50.6(6) . . . . ? C4_5 C5_5 C6_5 O6_5 70.2(7) . . . . ? C3_5 C4_5 O4_5 C1_6 128.9(5) . . . . ? C5_5 C4_5 O4_5 C1_6 -112.1(5) . . . . ? O4_4 C1_5 O5_5 C5_5 62.2(6) . . . . ? C2_5 C1_5 O5_5 C5_5 -57.9(6) . . . . ? C6_5 C5_5 O5_5 C1_5 -179.8(4) . . . . ? C4_5 C5_5 O5_5 C1_5 55.9(6) . . . . ? C4_5 O4_5 C1_6 O5_6 115.7(5) . . . . ? C4_5 O4_5 C1_6 C2_6 -124.5(5) . . . . ? O5_6 C1_6 C2_6 O2_6 -179.1(4) . . . . ? O4_5 C1_6 C2_6 O2_6 60.8(6) . . . . ? O5_6 C1_6 C2_6 C3_6 57.2(5) . . . . ? O4_5 C1_6 C2_6 C3_6 -62.8(6) . . . . ? O2_6 C2_6 C3_6 O3_6 61.7(6) . . . . ? C1_6 C2_6 C3_6 O3_6 -174.7(4) . . . . ? O2_6 C2_6 C3_6 C4_6 -178.8(5) . . . . ? C1_6 C2_6 C3_6 C4_6 -55.2(6) . . . . ? O3_6 C3_6 C4_6 O4_6 -65.5(6) . . . . ? C2_6 C3_6 C4_6 O4_6 174.5(4) . . . . ? O3_6 C3_6 C4_6 C5_6 175.6(4) . . . . ? C2_6 C3_6 C4_6 C5_6 55.7(6) . . . . ? O4_6 C4_6 C5_6 O5_6 -174.5(4) . . . . ? C3_6 C4_6 C5_6 O5_6 -57.0(6) . . . . ? O4_6 C4_6 C5_6 C6_6 65.8(6) . . . . ? C3_6 C4_6 C5_6 C6_6 -176.7(5) . . . . ? O5_6 C5_6 C6_6 O6_6 -77.2(6) . . . . ? C4_6 C5_6 C6_6 O6_6 43.3(7) . . . . ? C3_6 C4_6 O4_6 C1_7 126.1(5) . . . . ? C5_6 C4_6 O4_6 C1_7 -114.0(5) . . . . ? O4_5 C1_6 O5_6 C5_6 58.3(6) . . . . ? C2_6 C1_6 O5_6 C5_6 -60.1(5) . . . . ? C6_6 C5_6 O5_6 C1_6 -177.4(5) . . . . ? C4_6 C5_6 O5_6 C1_6 60.2(6) . . . . ? C4_6 O4_6 C1_7 O5_7 109.7(5) . . . . ? C4_6 O4_6 C1_7 C2_7 -128.8(5) . . . . ? O4_6 C1_7 C2_7 O2_7 60.1(6) . . . . ? O5_7 C1_7 C2_7 O2_7 -177.1(4) . . . . ? O4_6 C1_7 C2_7 C3_7 -61.4(6) . . . . ? O5_7 C1_7 C2_7 C3_7 61.5(6) . . . . ? O2_7 C2_7 C3_7 O3_7 64.5(6) . . . . ? C1_7 C2_7 C3_7 O3_7 -174.3(5) . . . . ? O2_7 C2_7 C3_7 C4_7 -177.6(5) . . . . ? C1_7 C2_7 C3_7 C4_7 -56.4(6) . . . . ? O3_7 C3_7 C4_7 O4_7 -67.4(6) . . . . ? C2_7 C3_7 C4_7 O4_7 173.1(5) . . . . ? O3_7 C3_7 C4_7 C5_7 173.4(5) . . . . ? C2_7 C3_7 C4_7 C5_7 53.9(7) . . . . ? O4_7 C4_7 C5_7 O5_7 -170.1(5) . . . . ? C3_7 C4_7 C5_7 O5_7 -52.8(7) . . . . ? O4_7 C4_7 C5_7 C6_7 71.6(6) . . . . ? C3_7 C4_7 C5_7 C6_7 -171.0(5) . . . . ? O5_7 C5_7 C6_7 O6_7 -69.1(6) . . . . ? C4_7 C5_7 C6_7 O6_7 51.5(6) . . . . ? O5_1 C1_1 O4_7 C4_7 110.9(5) . . . . ? C2_1 C1_1 O4_7 C4_7 -128.9(5) . . . . ? C5_7 C4_7 O4_7 C1_1 -106.6(6) . . . . ? C3_7 C4_7 O4_7 C1_1 131.9(5) . . . . ? O4_6 C1_7 O5_7 C5_7 57.7(6) . . . . ? C2_7 C1_7 O5_7 C5_7 -62.3(6) . . . . ? C4_7 C5_7 O5_7 C1_7 57.3(6) . . . . ? C6_7 C5_7 O5_7 C1_7 179.7(5) . . . . ? OB_21 OA_21 OA_24 OB_24 -98(6) 4_546 . . . ? C9_25 O1_25 C2_25 O2_25 179.6 . . . . ? C9_25 O1_25 C2_25 C3_25 -0.3 . . . . ? O2_25 C2_25 C3_25 C4_25 -179.8 . . . . ? O1_25 C2_25 C3_25 C4_25 0.0 . . . . ? C2_25 C3_25 C4_25 C10_25 0.0 . . . . ? C2_25 C3_25 C4_25 C11_25 180.0 . . . . ? C10_25 C5_25 C6_25 C7_25 0.3 . . . . ? C5_25 C6_25 C7_25 C8_25 -0.5 . . . . ? C5_25 C6_25 C7_25 C12_25 179.3 . . . . ? C6_25 C7_25 C8_25 C9_25 0.0 . . . . ? C12_25 C7_25 C8_25 C9_25 -179.8 . . . . ? C2_25 O1_25 C9_25 C10_25 0.5 . . . . ? C2_25 O1_25 C9_25 C8_25 -179.0 . . . . ? C7_25 C8_25 C9_25 O1_25 -179.8 . . . . ? C7_25 C8_25 C9_25 C10_25 0.8 . . . . ? O1_25 C9_25 C10_25 C5_25 179.6 . . . . ? C8_25 C9_25 C10_25 C5_25 -1.0 . . . . ? O1_25 C9_25 C10_25 C4_25 -0.4 . . . . ? C8_25 C9_25 C10_25 C4_25 179.0 . . . . ? C6_25 C5_25 C10_25 C9_25 0.4 . . . . ? C6_25 C5_25 C10_25 C4_25 -179.6 . . . . ? C3_25 C4_25 C10_25 C9_25 0.2 . . . . ? C11_25 C4_25 C10_25 C9_25 -179.8 . . . . ? C3_25 C4_25 C10_25 C5_25 -179.8 . . . . ? C11_25 C4_25 C10_25 C5_25 0.2 . . . . ? C9_26 O1_26 C2_26 O2_26 179.7 . . . . ? C9_26 O1_26 C2_26 C3_26 0.0 . . . . ? O2_26 C2_26 C3_26 C4_26 -179.8 . . . . ? O1_26 C2_26 C3_26 C4_26 -0.1 . . . . ? C2_26 C3_26 C4_26 C10_26 0.1 . . . . ? C2_26 C3_26 C4_26 C11_26 -179.9 . . . . ? C10_26 C5_26 C6_26 C7_26 0.1 . . . . ? C5_26 C6_26 C7_26 C8_26 -0.5 . . . . ? C5_26 C6_26 C7_26 C12_26 179.4 . . . . ? C6_26 C7_26 C8_26 C9_26 0.0 . . . . ? C12_26 C7_26 C8_26 C9_26 -179.8 . . . . ? C2_26 O1_26 C9_26 C10_26 0.2 . . . . ? C2_26 O1_26 C9_26 C8_26 -179.1 . . . . ? C7_26 C8_26 C9_26 O1_26 -179.9 . . . . ? C7_26 C8_26 C9_26 C10_26 0.8 . . . . ? O1_26 C9_26 C10_26 C5_26 179.6 . . . . ? C8_26 C9_26 C10_26 C5_26 -1.2 . . . . ? O1_26 C9_26 C10_26 C4_26 -0.2 . . . . ? C8_26 C9_26 C10_26 C4_26 179.0 . . . . ? C6_26 C5_26 C10_26 C9_26 0.7 . . . . ? C6_26 C5_26 C10_26 C4_26 -179.5 . . . . ? C3_26 C4_26 C10_26 C9_26 0.1 . . . . ? C11_26 C4_26 C10_26 C9_26 -179.9 . . . . ? C3_26 C4_26 C10_26 C5_26 -179.7 . . . . ? C11_26 C4_26 C10_26 C5_26 0.3 . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.929 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.154 #===END data_dimehv2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4,7-dimethylcoumarin anti-HT photodimer' _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 O4' _chemical_formula_sum 'C22 H20 O4' _chemical_formula_weight 348.38 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 'Monoclinic P' _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.733 _cell_length_b 15.587 _cell_length_c 5.722 _cell_angle_alpha 90.00 _cell_angle_beta 99.184(2) _cell_angle_gamma 90.00 _cell_volume 856.9 _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2817 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max .6 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 0.092 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MARResearch imaging plate' _diffrn_measurement_method 'oscillation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3409 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 21.97 _reflns_number_total 995 _reflns_number_gt 693 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARDC _computing_cell_refinement MARXDS _computing_data_reduction MARXDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.08(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -2(10) _refine_ls_number_reflns 995 _refine_ls_number_parameters 106 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1746 _refine_ls_R_factor_gt 0.1190 _refine_ls_wR_factor_ref 0.3015 _refine_ls_wR_factor_gt 0.2829 _refine_ls_goodness_of_fit_ref 2.218 _refine_ls_restrained_S_all 2.217 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.004 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O11 O 0.1937(15) 0.4884(7) 0.2842(19) 0.026(3) Uiso 1 1 d . . . O12 O 0.2723(13) 0.4058(7) 0.5789(18) 0.040(4) Uiso 1 1 d . . . C12 C 0.3014(19) 0.4583(10) 0.439(3) 0.017(4) Uiso 1 1 d . . . C13 C 0.4477(19) 0.4785(10) 0.405(3) 0.014(4) Uiso 1 1 d . . . H13 H 0.5020 0.4955 0.5573 0.017 Uiso 1 1 calc R . . C14 C 0.473(2) 0.5426(10) 0.214(3) 0.017(4) Uiso 1 1 d . . . C15 C 0.342(2) 0.6195(10) -0.146(3) 0.021(5) Uiso 1 1 d . . . H15 H 0.4274 0.6389 -0.1801 0.025 Uiso 1 1 calc R . . C16 C 0.2215(19) 0.6420(11) -0.291(3) 0.024(5) Uiso 1 1 d . . . H16 H 0.2262 0.6776 -0.4202 0.029 Uiso 1 1 calc R . . C17 C 0.094(2) 0.6134(12) -0.252(3) 0.028(5) Uiso 1 1 d . . . C18 C 0.091(2) 0.5623(12) -0.057(3) 0.022(4) Uiso 1 1 d . . . H18 H 0.0063 0.5420 -0.0248 0.027 Uiso 1 1 calc R . . C19 C 0.2141(19) 0.5404(10) 0.093(3) 0.016(4) Uiso 1 1 d . . . C110 C 0.3390(17) 0.5679(9) 0.053(2) 0.011(4) Uiso 1 1 d . . . C111 C 0.563(2) 0.6178(10) 0.309(3) 0.026(5) Uiso 1 1 d . . . H11A H 0.5756 0.6551 0.1801 0.038 Uiso 1 1 calc R . . H11B H 0.6520 0.5974 0.3848 0.038 Uiso 1 1 calc R . . H11C H 0.5186 0.6488 0.4207 0.038 Uiso 1 1 calc R . . C112 C -0.036(3) 0.6362(14) -0.409(4) 0.043(6) Uiso 1 1 d . . . H11D H -0.0145 0.6713 -0.5360 0.064 Uiso 1 1 calc R . . H11E H -0.0952 0.6674 -0.3201 0.064 Uiso 1 1 calc R . . H11F H -0.0819 0.5849 -0.4717 0.064 Uiso 1 1 calc R . . O21 O 0.8062(15) 0.4598(6) 0.2211(19) 0.027(3) Uiso 1 1 d . . . O22 O 0.7188(13) 0.5314(6) -0.1031(18) 0.032(3) Uiso 1 1 d . . . C22 C 0.695(2) 0.4920(11) 0.068(3) 0.022(5) Uiso 1 1 d . . . C23 C 0.555(2) 0.4689(11) 0.096(3) 0.016(4) Uiso 1 1 d . . . H23 H 0.5020 0.4518 -0.0571 0.019 Uiso 1 1 calc R . . C24 C 0.5270(19) 0.4051(9) 0.292(3) 0.015(4) Uiso 1 1 d . . . C25 C 0.653(2) 0.3286(10) 0.646(3) 0.019(5) Uiso 1 1 d . . . H25 H 0.5675 0.3094 0.6773 0.023 Uiso 1 1 calc R . . C26 C 0.7689(19) 0.3063(11) 0.800(3) 0.023(5) Uiso 1 1 d . . . H26 H 0.7617 0.2733 0.9333 0.027 Uiso 1 1 calc R . . C27 C 0.903(2) 0.3349(11) 0.754(3) 0.022(5) Uiso 1 1 d . . . C28 C 0.908(2) 0.3849(11) 0.550(3) 0.023(5) Uiso 1 1 d . . . H28 H 0.9932 0.4026 0.5118 0.027 Uiso 1 1 calc R . . C29 C 0.7860(19) 0.4071(10) 0.411(3) 0.017(4) Uiso 1 1 d . . . C210 C 0.654(2) 0.3778(10) 0.445(3) 0.019(5) Uiso 1 1 d . . . C211 C 0.440(2) 0.3284(10) 0.189(4) 0.030(5) Uiso 1 1 d . . . H21A H 0.3578 0.3485 0.0880 0.044 Uiso 1 1 calc R . . H21B H 0.4128 0.2952 0.3160 0.044 Uiso 1 1 calc R . . H21C H 0.4933 0.2933 0.0997 0.044 Uiso 1 1 calc R . . C212 C 1.034(2) 0.3127(12) 0.916(3) 0.036(5) Uiso 1 1 d . . . H21D H 1.1117 0.3381 0.8593 0.054 Uiso 1 1 calc R . . H21E H 1.0446 0.2515 0.9227 0.054 Uiso 1 1 calc R . . H21F H 1.0285 0.3341 1.0721 0.054 Uiso 1 1 calc R . . _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 O11 C12 1.34(2) . ? O11 C19 1.399(18) . ? O12 C12 1.211(18) . ? C12 C13 1.50(2) . ? C13 C14 1.53(2) . ? C13 C24 1.58(2) . ? C14 C111 1.51(2) . ? C14 C110 1.53(2) . ? C14 C23 1.61(2) . ? C15 C16 1.37(3) . ? C15 C110 1.40(2) . ? C16 C17 1.37(3) . ? C17 C18 1.37(2) . ? C17 C112 1.47(3) . ? C18 C19 1.40(3) . ? C19 C110 1.34(2) . ? O21 C22 1.37(2) . ? O21 C29 1.400(18) . ? O22 C22 1.207(18) . ? C22 C23 1.45(3) . ? C23 C24 1.56(2) . ? C24 C210 1.46(3) . ? C24 C211 1.53(3) . ? C25 C26 1.36(3) . ? C25 C210 1.38(2) . ? C26 C27 1.45(3) . ? C27 C28 1.41(2) . ? C27 C212 1.49(3) . ? C28 C29 1.37(3) . ? C29 C210 1.41(3) . ? 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 C12 O11 C19 121.5(15) . . ? O12 C12 O11 115.5(16) . . ? O12 C12 C13 123.6(16) . . ? O11 C12 C13 120.0(13) . . ? C12 C13 C14 119.5(15) . . ? C12 C13 C24 116.0(14) . . ? C14 C13 C24 92.0(12) . . ? C111 C14 C110 114.0(14) . . ? C111 C14 C13 113.7(15) . . ? C110 C14 C13 112.4(15) . . ? C111 C14 C23 114.0(17) . . ? C110 C14 C23 111.4(12) . . ? C13 C14 C23 89.0(11) . . ? C16 C15 C110 120.6(17) . . ? C17 C16 C15 121.8(17) . . ? C16 C17 C18 117.4(18) . . ? C16 C17 C112 122.1(16) . . ? C18 C17 C112 120.5(18) . . ? C17 C18 C19 120.9(18) . . ? C110 C19 O11 124.4(16) . . ? C110 C19 C18 121.5(14) . . ? O11 C19 C18 114.0(16) . . ? C19 C110 C15 117.7(15) . . ? C19 C110 C14 121.5(13) . . ? C15 C110 C14 120.8(15) . . ? C22 O21 C29 121.2(14) . . ? O22 C22 O21 118.3(16) . . ? O22 C22 C23 121.3(17) . . ? O21 C22 C23 119.8(15) . . ? C22 C23 C24 121.2(16) . . ? C22 C23 C14 114.2(15) . . ? C24 C23 C14 89.8(12) . . ? C210 C24 C211 111.6(15) . . ? C210 C24 C23 113.0(15) . . ? C211 C24 C23 112.0(15) . . ? C210 C24 C13 112.8(13) . . ? C211 C24 C13 116.5(17) . . ? C23 C24 C13 89.3(11) . . ? C26 C25 C210 124.6(18) . . ? C25 C26 C27 118.6(16) . . ? C28 C27 C26 118.4(17) . . ? C28 C27 C212 120.4(17) . . ? C26 C27 C212 121.2(15) . . ? C29 C28 C27 118.7(18) . . ? C28 C29 O21 112.6(16) . . ? C28 C29 C210 124.4(15) . . ? O21 C29 C210 122.9(16) . . ? C25 C210 C29 115.0(17) . . ? C25 C210 C24 123.0(16) . . ? C29 C210 C24 121.7(14) . . ? 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 C19 O11 C12 O12 -171.3(12) . . . . ? C19 O11 C12 C13 -2(2) . . . . ? O12 C12 C13 C14 176.8(13) . . . . ? O11 C12 C13 C14 8(2) . . . . ? O12 C12 C13 C24 68.1(19) . . . . ? O11 C12 C13 C24 -100.7(18) . . . . ? C12 C13 C14 C111 122.3(18) . . . . ? C24 C13 C14 C111 -116.2(13) . . . . ? C12 C13 C14 C110 -9.1(19) . . . . ? C24 C13 C14 C110 112.5(14) . . . . ? C12 C13 C14 C23 -121.8(14) . . . . ? C24 C13 C14 C23 -0.2(18) . . . . ? C110 C15 C16 C17 -2(3) . . . . ? C15 C16 C17 C18 1(3) . . . . ? C15 C16 C17 C112 -179.2(18) . . . . ? C16 C17 C18 C19 0(3) . . . . ? C112 C17 C18 C19 -179.9(18) . . . . ? C12 O11 C19 C110 -3(2) . . . . ? C12 O11 C19 C18 176.8(15) . . . . ? C17 C18 C19 C110 0(3) . . . . ? C17 C18 C19 O11 179.7(14) . . . . ? O11 C19 C110 C15 180.0(13) . . . . ? C18 C19 C110 C15 0(2) . . . . ? O11 C19 C110 C14 1(2) . . . . ? C18 C19 C110 C14 -178.8(15) . . . . ? C16 C15 C110 C19 1(2) . . . . ? C16 C15 C110 C14 179.8(14) . . . . ? C111 C14 C110 C19 -126.3(18) . . . . ? C13 C14 C110 C19 5(2) . . . . ? C23 C14 C110 C19 102.9(17) . . . . ? C111 C14 C110 C15 55(2) . . . . ? C13 C14 C110 C15 -173.9(14) . . . . ? C23 C14 C110 C15 -75.9(18) . . . . ? C29 O21 C22 O22 -174.2(13) . . . . ? C29 O21 C22 C23 -2(2) . . . . ? O22 C22 C23 C24 169.3(13) . . . . ? O21 C22 C23 C24 -2(2) . . . . ? O22 C22 C23 C14 -85.2(18) . . . . ? O21 C22 C23 C14 103.2(17) . . . . ? C111 C14 C23 C22 -9(2) . . . . ? C110 C14 C23 C22 122.1(16) . . . . ? C13 C14 C23 C22 -124.2(13) . . . . ? C111 C14 C23 C24 115.9(14) . . . . ? C110 C14 C23 C24 -113.4(12) . . . . ? C13 C14 C23 C24 0.3(18) . . . . ? C22 C23 C24 C210 4(2) . . . . ? C14 C23 C24 C210 -114.8(14) . . . . ? C22 C23 C24 C211 -123.4(19) . . . . ? C14 C23 C24 C211 118.2(13) . . . . ? C22 C23 C24 C13 118.2(16) . . . . ? C14 C23 C24 C13 -0.2(18) . . . . ? C12 C13 C24 C210 -120.6(16) . . . . ? C14 C13 C24 C210 114.9(13) . . . . ? C12 C13 C24 C211 10(2) . . . . ? C14 C13 C24 C211 -114.1(14) . . . . ? C12 C13 C24 C23 124.7(12) . . . . ? C14 C13 C24 C23 0.3(18) . . . . ? C210 C25 C26 C27 0(3) . . . . ? C25 C26 C27 C28 0(2) . . . . ? C25 C26 C27 C212 179.9(17) . . . . ? C26 C27 C28 C29 3(3) . . . . ? C212 C27 C28 C29 -177.2(18) . . . . ? C27 C28 C29 O21 177.4(13) . . . . ? C27 C28 C29 C210 -5(3) . . . . ? C22 O21 C29 C28 -176.9(14) . . . . ? C22 O21 C29 C210 6(2) . . . . ? C26 C25 C210 C29 -2(3) . . . . ? C26 C25 C210 C24 -175.9(15) . . . . ? C28 C29 C210 C25 5(3) . . . . ? O21 C29 C210 C25 -178.1(14) . . . . ? C28 C29 C210 C24 179.0(17) . . . . ? O21 C29 C210 C24 -4(2) . . . . ? C211 C24 C210 C25 -60(2) . . . . ? C23 C24 C210 C25 173.0(14) . . . . ? C13 C24 C210 C25 74(2) . . . . ? C211 C24 C210 C29 126.6(19) . . . . ? C23 C24 C210 C29 -1(2) . . . . ? C13 C24 C210 C29 -100.1(18) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.812 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.130