# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2003 Compound I _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Nd O7' _chemical_formula_weight 522.56 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MonoclinicMonoclinic _symmetry_space_group_name_H-M C2/c 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 20.9868(6) _cell_length_b 21.5521(7) _cell_length_c 8.3162(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.9500(10) _cell_angle_gamma 90.00 _cell_volume 3650.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.888 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.618872 _exptl_absorpt_correction_T_max 1.000000 _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 sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens SMART-CCD _diffrn_measurement_method /w scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7631 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 23.24 _reflns_number_total 2624 _reflns_number_gt 2172 _reflns_threshold_expression >2sigma(I) _computing_data_collection Siemens XSCANS _computing_cell_refinement Siemens XSCANS _computing_data_reduction Siemens SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material Siemens SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^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 0.00034(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2624 _refine_ls_number_parameters 272 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.0000 0.287358(10) 0.2500 0.02168(11) Uani 1 2 d S . . Nd2 Nd 0.0000 0.206239(10) -0.2500 0.02169(11) Uani 1 2 d S . . O1 O 0.07012(12) 0.20786(9) 0.3785(3) 0.0305(6) Uani 1 1 d . . . O2 O 0.03342(13) 0.35609(10) 0.4996(3) 0.0364(6) Uani 1 1 d . . . O3 O 0.06025(11) 0.24603(10) 0.0473(3) 0.0299(6) Uani 1 1 d . . . O4 O 0.09402(15) 0.36151(14) 0.2372(4) 0.0533(8) Uani 1 1 d D . . O5 O 0.05278(13) 0.14727(10) -0.4205(3) 0.0391(7) Uani 1 1 d . . . O6 O 0.09615(13) 0.16248(11) -0.0531(3) 0.0435(7) Uani 1 1 d . . . O7 O 0.06620(12) 0.29054(9) -0.2914(3) 0.0322(6) Uani 1 1 d . . . C1 C 0.10418(18) 0.20446(15) 0.0527(5) 0.0291(9) Uani 1 1 d . . . C2 C 0.16904(19) 0.20875(15) 0.1781(5) 0.0317(9) Uani 1 1 d . . . C3 C 0.2091(2) 0.25926(19) 0.1652(5) 0.0435(10) Uani 1 1 d . . . H1 H 0.1936 0.2904 0.0884 0.052 Uiso 1 1 calc R . . C4 C 0.2727(2) 0.2630(2) 0.2679(6) 0.0529(12) Uani 1 1 d . . . H2 H 0.3000 0.2960 0.2573 0.063 Uiso 1 1 calc R . . C5 C 0.2942(2) 0.2182(2) 0.3831(6) 0.0545(13) Uani 1 1 d . . . H3 H 0.3358 0.2212 0.4537 0.065 Uiso 1 1 calc R . . C6 C 0.25472(19) 0.1685(2) 0.3957(5) 0.0455(11) Uani 1 1 d . . . H4 H 0.2705 0.1382 0.4749 0.055 Uiso 1 1 calc R . . C7 C 0.19165(17) 0.16189(16) 0.2938(4) 0.0311(9) Uani 1 1 d . . . C8 C 0.15439(18) 0.10416(16) 0.3094(4) 0.0324(9) Uani 1 1 d . . . C9 C 0.1786(2) 0.04794(18) 0.2604(5) 0.0487(12) Uani 1 1 d . . . H5 H 0.2151 0.0489 0.2155 0.058 Uiso 1 1 calc R . . C10 C 0.1496(3) -0.00813(19) 0.2771(6) 0.0581(13) Uani 1 1 d . . . H6 H 0.1665 -0.0445 0.2434 0.070 Uiso 1 1 calc R . . C11 C 0.0956(3) -0.01052(18) 0.3439(5) 0.0552(13) Uani 1 1 d . . . H7 H 0.0750 -0.0481 0.3527 0.066 Uiso 1 1 calc R . . C12 C 0.0727(2) 0.04340(16) 0.3973(5) 0.0428(11) Uani 1 1 d . . . H8 H 0.0373 0.0414 0.4462 0.051 Uiso 1 1 calc R . . C13 C 0.10050(18) 0.10107(15) 0.3809(4) 0.0299(9) Uani 1 1 d . . . C14 C 0.07241(16) 0.15617(15) 0.4501(4) 0.0273(8) Uani 1 1 d . . . C21 C 0.05622(16) 0.34434(14) -0.3509(4) 0.0257(8) Uani 1 1 d . . . C22 C 0.07733(18) 0.39722(14) -0.2314(4) 0.0260(8) Uani 1 1 d . . . C23 C 0.03566(17) 0.44564(14) -0.2094(4) 0.0277(8) Uani 1 1 d . . . C24 C 0.0624(2) 0.49465(16) -0.1035(5) 0.0371(10) Uani 1 1 d . . . H9 H 0.0354 0.5273 -0.0883 0.045 Uiso 1 1 calc R . . C25 C 0.1278(2) 0.49542(18) -0.0216(5) 0.0475(11) Uani 1 1 d . . . H10 H 0.1446 0.5288 0.0465 0.057 Uiso 1 1 calc R . . C26 C 0.1686(2) 0.44702(17) -0.0400(5) 0.0434(10) Uani 1 1 d . . . H11 H 0.2126 0.4473 0.0168 0.052 Uiso 1 1 calc R . . C27 C 0.14355(19) 0.39833(17) -0.1430(4) 0.0347(9) Uani 1 1 d . . . H12 H 0.1709 0.3655 -0.1545 0.042 Uiso 1 1 calc R . . H51 H 0.109(3) 0.372(3) 0.143(5) 0.15(3) Uiso 1 1 d D . . H52 H 0.094(4) 0.397(2) 0.304(8) 0.18(3) Uiso 1 1 d D . . 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 Nd1 0.02649(18) 0.02125(17) 0.01859(17) 0.000 0.00797(12) 0.000 Nd2 0.02670(18) 0.02044(16) 0.01898(18) 0.000 0.00753(12) 0.000 O1 0.0337(16) 0.0283(14) 0.0323(16) 0.0063(10) 0.0135(12) 0.0085(10) O2 0.0586(18) 0.0312(14) 0.0209(14) -0.0048(10) 0.0126(13) -0.0054(11) O3 0.0304(15) 0.0372(14) 0.0239(14) -0.0010(10) 0.0099(11) 0.0069(11) O4 0.058(2) 0.058(2) 0.053(2) -0.0155(15) 0.0300(17) -0.0259(15) O5 0.0587(19) 0.0330(14) 0.0325(16) 0.0044(11) 0.0245(14) 0.0126(12) O6 0.0479(18) 0.0386(15) 0.0362(17) -0.0096(12) -0.0049(13) 0.0139(12) O7 0.0344(16) 0.0237(14) 0.0419(18) 0.0011(10) 0.0160(13) -0.0022(10) C1 0.034(2) 0.033(2) 0.022(2) 0.0018(15) 0.0094(17) -0.0005(16) C2 0.029(2) 0.043(2) 0.026(2) -0.0086(15) 0.0134(18) 0.0036(16) C3 0.046(3) 0.051(3) 0.037(3) -0.0079(19) 0.017(2) -0.003(2) C4 0.035(2) 0.073(3) 0.058(3) -0.027(3) 0.024(2) -0.016(2) C5 0.026(3) 0.083(4) 0.054(3) -0.030(3) 0.009(2) 0.007(2) C6 0.033(2) 0.067(3) 0.034(2) -0.017(2) 0.0037(19) 0.018(2) C7 0.024(2) 0.045(2) 0.025(2) -0.0103(16) 0.0076(16) 0.0111(16) C8 0.034(2) 0.040(2) 0.019(2) -0.0045(15) -0.0007(17) 0.0141(17) C9 0.052(3) 0.056(3) 0.036(3) -0.008(2) 0.007(2) 0.030(2) C10 0.082(4) 0.037(3) 0.047(3) -0.011(2) -0.001(3) 0.025(2) C11 0.088(4) 0.028(2) 0.043(3) -0.0026(19) 0.004(3) 0.006(2) C12 0.059(3) 0.034(2) 0.033(3) 0.0023(17) 0.008(2) 0.0040(19) C13 0.040(2) 0.0287(19) 0.018(2) 0.0010(14) 0.0015(17) 0.0078(16) C14 0.024(2) 0.033(2) 0.025(2) 0.0003(16) 0.0040(16) 0.0059(15) C21 0.025(2) 0.0251(19) 0.033(2) -0.0031(15) 0.0179(17) -0.0025(14) C22 0.040(2) 0.0228(18) 0.020(2) -0.0001(14) 0.0167(17) -0.0031(15) C23 0.042(2) 0.0206(17) 0.026(2) 0.0012(14) 0.0182(17) -0.0031(15) C24 0.053(3) 0.023(2) 0.043(3) -0.0091(17) 0.028(2) -0.0070(17) C25 0.059(3) 0.045(2) 0.045(3) -0.021(2) 0.025(2) -0.024(2) C26 0.040(3) 0.053(3) 0.040(3) -0.0145(19) 0.015(2) -0.0114(19) C27 0.038(2) 0.042(2) 0.028(2) -0.0023(16) 0.0152(19) -0.0001(17) _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 Nd1 O1 2.342(2) . ? Nd1 O1 2.342(2) 2 ? Nd1 O3 2.502(2) . ? Nd1 O3 2.502(2) 2 ? Nd1 O2 2.508(2) . ? Nd1 O2 2.508(2) 2 ? Nd1 O4 2.561(3) . ? Nd1 O4 2.561(3) 2 ? Nd2 O7 2.362(2) 2_554 ? Nd2 O7 2.362(2) . ? Nd2 O5 2.369(2) 2_554 ? Nd2 O5 2.369(2) . ? Nd2 O6 2.459(2) . ? Nd2 O6 2.459(2) 2_554 ? Nd2 O3 2.635(2) . ? Nd2 O3 2.635(2) 2_554 ? Nd2 C1 2.909(4) . ? Nd2 C1 2.909(4) 2_554 ? O1 C14 1.259(4) . ? O2 C21 1.246(4) 1_556 ? O3 C1 1.278(4) . ? O4 H51 0.943(10) . ? O4 H52 0.942(10) . ? O5 C14 1.256(4) 1_554 ? O6 C1 1.245(4) . ? O7 C21 1.258(4) . ? C1 C2 1.505(5) . ? C2 C3 1.395(5) . ? C2 C7 1.396(5) . ? C3 C4 1.403(6) . ? C3 H1 0.9300 . ? C4 C5 1.359(6) . ? C4 H2 0.9300 . ? C5 C6 1.373(6) . ? C5 H3 0.9300 . ? C6 C7 1.396(5) . ? C6 H4 0.9300 . ? C7 C8 1.492(5) . ? C8 C13 1.400(5) . ? C8 C9 1.412(5) . ? C9 C10 1.375(6) . ? C9 H5 0.9300 . ? C10 C11 1.378(7) . ? C10 H6 0.9300 . ? C11 C12 1.372(5) . ? C11 H7 0.9300 . ? C12 C13 1.394(5) . ? C12 H8 0.9300 . ? C13 C14 1.501(5) . ? C14 O5 1.256(4) 1_556 ? C21 O2 1.246(4) 1_554 ? C21 C22 1.507(4) . ? C22 C23 1.402(5) . ? C22 C27 1.407(5) . ? C23 C24 1.403(5) . ? C23 C23 1.486(7) 2_554 ? C24 C25 1.377(5) . ? C24 H9 0.9300 . ? C25 C26 1.381(6) . ? C25 H10 0.9300 . ? C26 C27 1.376(5) . ? C26 H11 0.9300 . ? C27 H12 0.9300 . ? 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 O1 Nd1 O1 85.97(11) . 2 ? O1 Nd1 O3 71.52(8) . . ? O1 Nd1 O3 78.23(8) 2 . ? O1 Nd1 O3 78.24(8) . 2 ? O1 Nd1 O3 71.52(8) 2 2 ? O3 Nd1 O3 138.29(10) . 2 ? O1 Nd1 O2 91.99(8) . . ? O1 Nd1 O2 146.02(8) 2 . ? O3 Nd1 O2 132.97(8) . . ? O3 Nd1 O2 74.86(8) 2 . ? O1 Nd1 O2 146.02(8) . 2 ? O1 Nd1 O2 91.99(8) 2 2 ? O3 Nd1 O2 74.86(8) . 2 ? O3 Nd1 O2 132.97(8) 2 2 ? O2 Nd1 O2 107.61(11) . 2 ? O1 Nd1 O4 94.00(9) . . ? O1 Nd1 O4 147.47(9) 2 . ? O3 Nd1 O4 71.01(9) . . ? O3 Nd1 O4 140.32(9) 2 . ? O2 Nd1 O4 66.50(9) . . ? O2 Nd1 O4 70.23(9) 2 . ? O1 Nd1 O4 147.47(9) . 2 ? O1 Nd1 O4 94.00(9) 2 2 ? O3 Nd1 O4 140.32(9) . 2 ? O3 Nd1 O4 71.01(9) 2 2 ? O2 Nd1 O4 70.23(9) . 2 ? O2 Nd1 O4 66.50(9) 2 2 ? O4 Nd1 O4 102.79(14) . 2 ? O7 Nd2 O7 79.45(11) 2_554 . ? O7 Nd2 O5 87.08(8) 2_554 2_554 ? O7 Nd2 O5 151.19(9) . 2_554 ? O7 Nd2 O5 151.19(9) 2_554 . ? O7 Nd2 O5 87.08(8) . . ? O5 Nd2 O5 115.10(12) 2_554 . ? O7 Nd2 O6 127.95(8) 2_554 . ? O7 Nd2 O6 88.56(9) . . ? O5 Nd2 O6 79.80(9) 2_554 . ? O5 Nd2 O6 76.45(9) . . ? O7 Nd2 O6 88.56(9) 2_554 2_554 ? O7 Nd2 O6 127.95(8) . 2_554 ? O5 Nd2 O6 76.45(9) 2_554 2_554 ? O5 Nd2 O6 79.80(9) . 2_554 ? O6 Nd2 O6 134.90(11) . 2_554 ? O7 Nd2 O3 77.23(8) 2_554 . ? O7 Nd2 O3 73.76(8) . . ? O5 Nd2 O3 78.50(8) 2_554 . ? O5 Nd2 O3 123.27(8) . . ? O6 Nd2 O3 50.87(7) . . ? O6 Nd2 O3 151.73(8) 2_554 . ? O7 Nd2 O3 73.76(8) 2_554 2_554 ? O7 Nd2 O3 77.23(8) . 2_554 ? O5 Nd2 O3 123.27(8) 2_554 2_554 ? O5 Nd2 O3 78.50(8) . 2_554 ? O6 Nd2 O3 151.73(8) . 2_554 ? O6 Nd2 O3 50.87(7) 2_554 2_554 ? O3 Nd2 O3 142.01(10) . 2_554 ? O7 Nd2 C1 103.29(9) 2_554 . ? O7 Nd2 C1 77.91(9) . . ? O5 Nd2 C1 80.64(9) 2_554 . ? O5 Nd2 C1 98.54(10) . . ? O6 Nd2 C1 25.07(8) . . ? O6 Nd2 C1 153.60(9) 2_554 . ? O3 Nd2 C1 26.06(8) . . ? O3 Nd2 C1 155.08(8) 2_554 . ? O7 Nd2 C1 77.91(9) 2_554 2_554 ? O7 Nd2 C1 103.29(9) . 2_554 ? O5 Nd2 C1 98.54(10) 2_554 2_554 ? O5 Nd2 C1 80.64(9) . 2_554 ? O6 Nd2 C1 153.60(9) . 2_554 ? O6 Nd2 C1 25.06(8) 2_554 2_554 ? O3 Nd2 C1 155.08(8) . 2_554 ? O3 Nd2 C1 26.07(8) 2_554 2_554 ? C1 Nd2 C1 178.49(13) . 2_554 ? C14 O1 Nd1 144.3(2) . . ? C21 O2 Nd1 132.0(2) 1_556 . ? C1 O3 Nd1 134.7(2) . . ? C1 O3 Nd2 89.1(2) . . ? Nd1 O3 Nd2 122.81(9) . . ? Nd1 O4 H51 127(4) . . ? Nd1 O4 H52 111(5) . . ? H51 O4 H52 110(5) . . ? C14 O5 Nd2 136.7(2) 1_554 . ? C1 O6 Nd2 98.1(2) . . ? C21 O7 Nd2 135.9(2) . . ? O6 C1 O3 120.7(3) . . ? O6 C1 C2 118.7(3) . . ? O3 C1 C2 120.3(3) . . ? O6 C1 Nd2 56.81(18) . . ? O3 C1 Nd2 64.88(18) . . ? C2 C1 Nd2 164.7(3) . . ? C3 C2 C7 120.4(4) . . ? C3 C2 C1 117.1(3) . . ? C7 C2 C1 122.2(3) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H1 120.0 . . ? C4 C3 H1 120.0 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H2 120.2 . . ? C3 C4 H2 120.2 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H3 119.9 . . ? C6 C5 H3 119.9 . . ? C5 C6 C7 122.3(4) . . ? C5 C6 H4 118.8 . . ? C7 C6 H4 118.8 . . ? C6 C7 C2 117.3(4) . . ? C6 C7 C8 118.2(3) . . ? C2 C7 C8 124.4(3) . . ? C13 C8 C9 117.7(4) . . ? C13 C8 C7 124.8(3) . . ? C9 C8 C7 117.3(4) . . ? C10 C9 C8 121.8(4) . . ? C10 C9 H5 119.1 . . ? C8 C9 H5 119.1 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H6 120.0 . . ? C11 C10 H6 120.0 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 H7 120.5 . . ? C10 C11 H7 120.5 . . ? C11 C12 C13 122.4(5) . . ? C11 C12 H8 118.8 . . ? C13 C12 H8 118.8 . . ? C12 C13 C8 119.0(3) . . ? C12 C13 C14 117.1(4) . . ? C8 C13 C14 123.9(3) . . ? O5 C14 O1 123.9(3) 1_556 . ? O5 C14 C13 116.6(3) 1_556 . ? O1 C14 C13 119.5(3) . . ? O2 C21 O7 124.6(3) 1_554 . ? O2 C21 C22 119.1(3) 1_554 . ? O7 C21 C22 116.3(3) . . ? C23 C22 C27 119.2(3) . . ? C23 C22 C21 123.8(3) . . ? C27 C22 C21 117.0(3) . . ? C22 C23 C24 118.3(3) . . ? C22 C23 C23 122.2(3) . 2_554 ? C24 C23 C23 119.5(3) . 2_554 ? C25 C24 C23 121.3(3) . . ? C25 C24 H9 119.3 . . ? C23 C24 H9 119.3 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H10 119.8 . . ? C26 C25 H10 119.8 . . ? C27 C26 C25 119.4(4) . . ? C27 C26 H11 120.3 . . ? C25 C26 H11 120.3 . . ? C26 C27 C22 121.2(4) . . ? C26 C27 H12 119.4 . . ? C22 C27 H12 119.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.539 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.090 ### EOF ### Compound II data_sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Dy O7' _chemical_formula_weight 540.82 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' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 20.9794(7) _cell_length_b 21.3829(7) _cell_length_c 8.2116(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.0890(10) _cell_angle_gamma 90.00 _cell_volume 3572.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 4.227 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.611640 _exptl_absorpt_correction_T_max 1.000000 _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 sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens SMART-CCD _diffrn_measurement_method /w scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7408 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 23.23 _reflns_number_total 2560 _reflns_number_gt 2115 _reflns_threshold_expression >2sigma(I) _computing_data_collection Siemens XSCANS _computing_cell_refinement Siemens XSCANS _computing_data_reduction Siemens SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material Siemens SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+5.7019P] 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 0.00067(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2560 _refine_ls_number_parameters 272 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.0000 0.286558(11) 0.2500 0.02018(13) Uani 1 2 d S . . Dy2 Dy 0.0000 0.207499(11) -0.2500 0.01937(13) Uani 1 2 d S . . O1 O 0.06868(16) 0.20988(12) 0.3786(4) 0.0292(8) Uani 1 1 d . . . O2 O 0.03348(16) 0.35292(13) 0.4970(4) 0.0316(8) Uani 1 1 d . . . O3 O 0.05748(14) 0.24654(13) 0.0470(4) 0.0265(7) Uani 1 1 d . . . O4 O 0.09071(19) 0.35810(17) 0.2371(5) 0.0455(10) Uani 1 1 d D . . O5 O 0.04820(17) 0.14895(13) -0.4205(4) 0.0328(8) Uani 1 1 d . . . O6 O 0.09576(16) 0.16541(14) -0.0632(4) 0.0365(8) Uani 1 1 d . . . O7 O 0.06609(16) 0.28806(12) -0.2863(4) 0.0279(8) Uani 1 1 d . . . C1 C 0.1023(2) 0.20566(18) 0.0491(6) 0.0255(11) Uani 1 1 d . . . C2 C 0.1676(2) 0.2095(2) 0.1768(6) 0.0297(12) Uani 1 1 d . . . C3 C 0.2081(3) 0.2597(2) 0.1631(7) 0.0389(13) Uani 1 1 d . . . H1 H 0.1928 0.2912 0.0854 0.047 Uiso 1 1 calc R . . C4 C 0.2725(3) 0.2629(3) 0.2671(7) 0.0472(15) Uani 1 1 d . . . H2 H 0.3002 0.2957 0.2559 0.057 Uiso 1 1 calc R . . C5 C 0.2935(3) 0.2176(3) 0.3834(8) 0.0472(16) Uani 1 1 d . . . H3 H 0.3353 0.2202 0.4546 0.057 Uiso 1 1 calc R . . C6 C 0.2537(2) 0.1679(2) 0.3972(6) 0.0394(13) Uani 1 1 d . . . H4 H 0.2694 0.1371 0.4769 0.047 Uiso 1 1 calc R . . C7 C 0.1903(2) 0.1623(2) 0.2946(6) 0.0299(11) Uani 1 1 d . . . C8 C 0.1520(2) 0.1041(2) 0.3122(6) 0.0298(11) Uani 1 1 d . . . C9 C 0.1767(3) 0.0469(2) 0.2659(7) 0.0425(14) Uani 1 1 d . . . H5 H 0.2135 0.0472 0.2219 0.051 Uiso 1 1 calc R . . C10 C 0.1469(3) -0.0092(2) 0.2850(7) 0.0522(16) Uani 1 1 d . . . H6 H 0.1638 -0.0463 0.2533 0.063 Uiso 1 1 calc R . . C11 C 0.0929(3) -0.0110(2) 0.3498(7) 0.0469(15) Uani 1 1 d . . . H7 H 0.0722 -0.0488 0.3588 0.056 Uiso 1 1 calc R . . C12 C 0.0693(3) 0.04357(19) 0.4019(7) 0.0355(13) Uani 1 1 d . . . H8 H 0.0336 0.0419 0.4503 0.043 Uiso 1 1 calc R . . C13 C 0.0978(2) 0.1016(2) 0.3837(6) 0.0284(11) Uani 1 1 d . . . C14 C 0.0698(2) 0.15753(19) 0.4516(6) 0.0252(10) Uani 1 1 d . . . C21 C 0.0564(2) 0.34208(18) -0.3501(6) 0.0247(10) Uani 1 1 d . . . C22 C 0.0775(2) 0.39628(19) -0.2305(5) 0.0255(11) Uani 1 1 d . . . C23 C 0.0358(2) 0.44500(19) -0.2088(6) 0.0276(11) Uani 1 1 d . . . C24 C 0.0630(3) 0.4950(2) -0.1034(6) 0.0373(13) Uani 1 1 d . . . H9 H 0.0360 0.5279 -0.0883 0.045 Uiso 1 1 calc R . . C25 C 0.1285(3) 0.4964(2) -0.0220(7) 0.0431(14) Uani 1 1 d . . . H10 H 0.1454 0.5305 0.0450 0.052 Uiso 1 1 calc R . . C26 C 0.1695(3) 0.4476(2) -0.0390(7) 0.0413(13) Uani 1 1 d . . . H11 H 0.2136 0.4482 0.0180 0.050 Uiso 1 1 calc R . . C27 C 0.1440(2) 0.3978(2) -0.1420(6) 0.0334(12) Uani 1 1 d . . . H12 H 0.1714 0.3646 -0.1531 0.040 Uiso 1 1 calc R . . H51 H 0.115(4) 0.361(4) 0.154(9) 0.15(4) Uiso 1 1 d D . . H52 H 0.096(4) 0.395(2) 0.302(8) 0.13(3) Uiso 1 1 d D . . 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 Dy1 0.0223(2) 0.02131(19) 0.0170(2) 0.000 0.00492(14) 0.000 Dy2 0.0215(2) 0.02005(18) 0.0170(2) 0.000 0.00555(14) 0.000 O1 0.029(2) 0.0302(18) 0.030(2) 0.0043(13) 0.0094(16) 0.0061(13) O2 0.047(2) 0.0276(16) 0.0191(19) -0.0018(13) 0.0054(16) -0.0042(15) O3 0.0246(18) 0.0335(17) 0.0220(18) -0.0024(13) 0.0066(14) 0.0054(14) O4 0.048(2) 0.050(2) 0.044(2) -0.0167(18) 0.022(2) -0.0239(18) O5 0.048(2) 0.0284(16) 0.027(2) 0.0047(14) 0.0175(17) 0.0083(15) O6 0.036(2) 0.0345(18) 0.033(2) -0.0070(16) -0.0026(16) 0.0111(15) O7 0.028(2) 0.0223(17) 0.035(2) 0.0002(13) 0.0108(16) -0.0025(12) C1 0.028(3) 0.027(2) 0.022(3) 0.0028(19) 0.006(2) -0.001(2) C2 0.023(3) 0.043(3) 0.023(3) -0.0074(19) 0.006(2) 0.004(2) C3 0.039(3) 0.045(3) 0.036(3) -0.007(2) 0.015(3) -0.007(3) C4 0.032(3) 0.061(4) 0.054(4) -0.026(3) 0.021(3) -0.020(3) C5 0.026(3) 0.072(4) 0.044(4) -0.025(3) 0.008(3) 0.008(3) C6 0.031(3) 0.053(3) 0.032(3) -0.008(2) 0.003(2) 0.014(3) C7 0.024(3) 0.044(3) 0.024(3) -0.009(2) 0.008(2) 0.009(2) C8 0.029(3) 0.036(3) 0.019(3) -0.002(2) -0.006(2) 0.012(2) C9 0.043(3) 0.051(3) 0.033(3) -0.005(2) 0.008(3) 0.021(3) C10 0.078(5) 0.033(3) 0.038(3) -0.008(2) -0.002(3) 0.023(3) C11 0.070(4) 0.026(3) 0.039(3) -0.004(2) 0.003(3) 0.007(3) C12 0.045(3) 0.029(3) 0.030(3) 0.000(2) 0.005(3) -0.001(2) C13 0.030(3) 0.030(2) 0.020(3) -0.0011(19) -0.001(2) 0.008(2) C14 0.021(3) 0.027(2) 0.025(3) 0.0013(19) 0.000(2) 0.0004(19) C21 0.025(3) 0.021(2) 0.033(3) -0.0014(19) 0.015(2) -0.0053(19) C22 0.036(3) 0.025(2) 0.019(3) -0.0030(18) 0.013(2) -0.001(2) C23 0.035(3) 0.026(2) 0.026(3) 0.002(2) 0.013(2) -0.004(2) C24 0.051(4) 0.024(2) 0.042(3) -0.007(2) 0.021(3) -0.007(2) C25 0.049(4) 0.040(3) 0.044(3) -0.020(2) 0.018(3) -0.020(3) C26 0.036(3) 0.048(3) 0.040(3) -0.012(3) 0.009(3) -0.011(3) C27 0.035(3) 0.034(3) 0.032(3) -0.004(2) 0.008(2) -0.003(2) _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 Dy1 O1 2.267(3) 2 ? Dy1 O1 2.267(3) . ? Dy1 O2 2.435(3) . ? Dy1 O2 2.435(3) 2 ? Dy1 O3 2.438(3) 2 ? Dy1 O3 2.438(3) . ? Dy1 O4 2.464(3) . ? Dy1 O4 2.464(3) 2 ? Dy2 O7 2.276(3) . ? Dy2 O7 2.276(3) 2_554 ? Dy2 O5 2.289(3) 2_554 ? Dy2 O5 2.289(3) . ? Dy2 O6 2.387(3) . ? Dy2 O6 2.387(3) 2_554 ? Dy2 O3 2.582(3) . ? Dy2 O3 2.582(3) 2_554 ? Dy2 C1 2.841(5) . ? Dy2 C1 2.841(5) 2_554 ? O1 C14 1.268(5) . ? O2 C21 1.252(5) 1_556 ? O3 C1 1.281(5) . ? O4 H51 0.946(11) . ? O4 H52 0.945(10) . ? O5 C14 1.255(5) 1_554 ? O6 C1 1.244(5) . ? O7 C21 1.264(5) . ? C1 C2 1.511(7) . ? C2 C3 1.391(7) . ? C2 C7 1.398(6) . ? C3 C4 1.414(8) . ? C3 H1 0.9300 . ? C4 C5 1.357(8) . ? C4 H2 0.9300 . ? C5 C6 1.373(7) . ? C5 H3 0.9300 . ? C6 C7 1.396(7) . ? C6 H4 0.9300 . ? C7 C8 1.508(7) . ? C8 C13 1.402(7) . ? C8 C9 1.415(6) . ? C9 C10 1.380(8) . ? C9 H5 0.9300 . ? C10 C11 1.364(8) . ? C10 H6 0.9300 . ? C11 C12 1.375(7) . ? C11 H7 0.9300 . ? C12 C13 1.401(6) . ? C12 H8 0.9300 . ? C13 C14 1.499(6) . ? C14 O5 1.255(5) 1_556 ? C21 O2 1.252(5) 1_554 ? C21 C22 1.514(6) . ? C22 C23 1.400(6) . ? C22 C27 1.408(7) . ? C23 C24 1.406(7) . ? C23 C23 1.489(10) 2_554 ? C24 C25 1.375(8) . ? C24 H9 0.9300 . ? C25 C26 1.381(7) . ? C25 H10 0.9300 . ? C26 C27 1.384(6) . ? C26 H11 0.9300 . ? C27 H12 0.9300 . ? 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 O1 Dy1 O1 87.34(16) 2 . ? O1 Dy1 O2 146.23(11) 2 . ? O1 Dy1 O2 90.68(11) . . ? O1 Dy1 O2 90.68(11) 2 2 ? O1 Dy1 O2 146.23(11) . 2 ? O2 Dy1 O2 108.70(14) . 2 ? O1 Dy1 O3 72.56(10) 2 2 ? O1 Dy1 O3 77.99(10) . 2 ? O2 Dy1 O3 74.06(10) . 2 ? O2 Dy1 O3 133.14(10) 2 2 ? O1 Dy1 O3 77.99(10) 2 . ? O1 Dy1 O3 72.56(10) . . ? O2 Dy1 O3 133.14(10) . . ? O2 Dy1 O3 74.06(10) 2 . ? O3 Dy1 O3 138.90(13) 2 . ? O1 Dy1 O4 147.05(12) 2 . ? O1 Dy1 O4 93.38(12) . . ? O2 Dy1 O4 66.72(11) . . ? O2 Dy1 O4 70.82(12) 2 . ? O3 Dy1 O4 139.74(11) 2 . ? O3 Dy1 O4 70.90(11) . . ? O1 Dy1 O4 93.38(12) 2 2 ? O1 Dy1 O4 147.05(12) . 2 ? O2 Dy1 O4 70.83(12) . 2 ? O2 Dy1 O4 66.72(11) 2 2 ? O3 Dy1 O4 70.90(11) 2 2 ? O3 Dy1 O4 139.74(11) . 2 ? O4 Dy1 O4 103.24(18) . 2 ? O7 Dy2 O7 81.62(15) . 2_554 ? O7 Dy2 O5 150.23(12) . 2_554 ? O7 Dy2 O5 87.71(11) 2_554 2_554 ? O7 Dy2 O5 87.71(11) . . ? O7 Dy2 O5 150.23(12) 2_554 . ? O5 Dy2 O5 113.68(15) 2_554 . ? O7 Dy2 O6 85.71(12) . . ? O7 Dy2 O6 130.20(11) 2_554 . ? O5 Dy2 O6 80.14(12) 2_554 . ? O5 Dy2 O6 76.04(11) . . ? O7 Dy2 O6 130.20(11) . 2_554 ? O7 Dy2 O6 85.71(12) 2_554 2_554 ? O5 Dy2 O6 76.04(11) 2_554 2_554 ? O5 Dy2 O6 80.14(12) . 2_554 ? O6 Dy2 O6 135.71(15) . 2_554 ? O7 Dy2 O3 73.72(11) . . ? O7 Dy2 O3 77.94(11) 2_554 . ? O5 Dy2 O3 76.91(10) 2_554 . ? O5 Dy2 O3 125.47(11) . . ? O6 Dy2 O3 52.30(10) . . ? O6 Dy2 O3 148.79(10) 2_554 . ? O7 Dy2 O3 77.93(11) . 2_554 ? O7 Dy2 O3 73.72(11) 2_554 2_554 ? O5 Dy2 O3 125.47(11) 2_554 2_554 ? O5 Dy2 O3 76.91(10) . 2_554 ? O6 Dy2 O3 148.79(10) . 2_554 ? O6 Dy2 O3 52.30(10) 2_554 2_554 ? O3 Dy2 O3 142.28(12) . 2_554 ? O7 Dy2 C1 76.56(12) . . ? O7 Dy2 C1 104.68(12) 2_554 . ? O5 Dy2 C1 79.46(12) 2_554 . ? O5 Dy2 C1 99.66(13) . . ? O6 Dy2 C1 25.70(11) . . ? O6 Dy2 C1 152.96(11) 2_554 . ? O3 Dy2 C1 26.78(11) . . ? O3 Dy2 C1 154.38(11) 2_554 . ? O7 Dy2 C1 104.68(12) . 2_554 ? O7 Dy2 C1 76.56(12) 2_554 2_554 ? O5 Dy2 C1 99.66(13) 2_554 2_554 ? O5 Dy2 C1 79.46(12) . 2_554 ? O6 Dy2 C1 152.96(11) . 2_554 ? O6 Dy2 C1 25.70(11) 2_554 2_554 ? O3 Dy2 C1 154.38(11) . 2_554 ? O3 Dy2 C1 26.78(10) 2_554 2_554 ? C1 Dy2 C1 178.41(16) . 2_554 ? C14 O1 Dy1 142.7(3) . . ? C21 O2 Dy1 133.6(3) 1_556 . ? C1 O3 Dy1 135.6(3) . . ? C1 O3 Dy2 88.0(3) . . ? Dy1 O3 Dy2 124.35(12) . . ? Dy1 O4 H51 129(6) . . ? Dy1 O4 H52 118(5) . . ? H51 O4 H52 111(7) . . ? C14 O5 Dy2 137.3(3) 1_554 . ? C1 O6 Dy2 98.0(3) . . ? C21 O7 Dy2 134.8(3) . . ? O6 C1 O3 121.0(4) . . ? O6 C1 C2 118.0(4) . . ? O3 C1 C2 120.7(4) . . ? O6 C1 Dy2 56.3(2) . . ? O3 C1 Dy2 65.3(2) . . ? C2 C1 Dy2 164.9(3) . . ? C3 C2 C7 120.0(5) . . ? C3 C2 C1 117.0(4) . . ? C7 C2 C1 122.7(4) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H1 120.0 . . ? C4 C3 H1 120.0 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H2 120.3 . . ? C3 C4 H2 120.3 . . ? C4 C5 C6 120.7(5) . . ? C4 C5 H3 119.6 . . ? C6 C5 H3 119.6 . . ? C5 C6 C7 121.7(5) . . ? C5 C6 H4 119.1 . . ? C7 C6 H4 119.1 . . ? C6 C7 C2 118.1(5) . . ? C6 C7 C8 117.7(4) . . ? C2 C7 C8 124.1(4) . . ? C13 C8 C9 117.8(5) . . ? C13 C8 C7 125.3(4) . . ? C9 C8 C7 116.7(4) . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H5 119.4 . . ? C8 C9 H5 119.4 . . ? C11 C10 C9 120.6(5) . . ? C11 C10 H6 119.7 . . ? C9 C10 H6 119.7 . . ? C10 C11 C12 119.6(5) . . ? C10 C11 H7 120.2 . . ? C12 C11 H7 120.2 . . ? C11 C12 C13 121.6(5) . . ? C11 C12 H8 119.2 . . ? C13 C12 H8 119.2 . . ? C12 C13 C8 119.3(4) . . ? C12 C13 C14 116.8(4) . . ? C8 C13 C14 123.8(4) . . ? O5 C14 O1 123.8(4) 1_556 . ? O5 C14 C13 116.7(4) 1_556 . ? O1 C14 C13 119.5(4) . . ? O2 C21 O7 124.6(4) 1_554 . ? O2 C21 C22 119.3(4) 1_554 . ? O7 C21 C22 116.0(4) . . ? C23 C22 C27 119.3(4) . . ? C23 C22 C21 124.0(4) . . ? C27 C22 C21 116.7(4) . . ? C22 C23 C24 118.2(4) . . ? C22 C23 C23 122.3(4) . 2_554 ? C24 C23 C23 119.5(3) . 2_554 ? C25 C24 C23 121.6(5) . . ? C25 C24 H9 119.2 . . ? C23 C24 H9 119.2 . . ? C24 C25 C26 120.5(5) . . ? C24 C25 H10 119.7 . . ? C26 C25 H10 119.7 . . ? C25 C26 C27 119.1(5) . . ? C25 C26 H11 120.4 . . ? C27 C26 H11 120.4 . . ? C26 C27 C22 121.3(5) . . ? C26 C27 H12 119.4 . . ? C22 C27 H12 119.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.886 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.122 ### EOF ### Compound III data_sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 O7 Y' _chemical_formula_weight 467.23 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' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 20.9371(5) _cell_length_b 21.3218(4) _cell_length_c 8.1858(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.1790(10) _cell_angle_gamma 90.00 _cell_volume 3542.95(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 3.337 _exptl_absorpt_correction_type Empirical SADABS _exptl_absorpt_correction_T_min 0.777419 _exptl_absorpt_correction_T_max 1.000000 _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 sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens SMART-CCD _diffrn_measurement_method /w scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7296 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2551 _reflns_number_gt 1807 _reflns_threshold_expression >2sigma(I) _computing_data_collection Siemens XSCANS _computing_cell_refinement Siemens XSCANS _computing_data_reduction Siemens SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material SIEMENS SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+3.3433P] 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 0.00058(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2551 _refine_ls_number_parameters 272 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.0000 0.28632(3) 0.2500 0.0200(2) Uani 1 2 d S . . Y2 Y 0.0000 0.20768(3) -0.2500 0.0194(2) Uani 1 2 d S . . O1 O 0.06835(15) 0.21044(13) 0.3783(4) 0.0253(8) Uani 1 1 d . . . O2 O 0.03376(16) 0.35253(13) 0.4959(4) 0.0289(8) Uani 1 1 d . . . O3 O 0.05682(15) 0.24664(14) 0.0475(4) 0.0246(8) Uani 1 1 d . . . O4 O 0.08969(19) 0.35731(18) 0.2372(5) 0.0435(10) Uani 1 1 d D . . O5 O 0.04746(16) 0.14915(14) -0.4195(4) 0.0304(9) Uani 1 1 d . . . O6 O 0.09524(16) 0.16588(14) -0.0651(4) 0.0308(9) Uani 1 1 d . . . O7 O 0.06571(15) 0.28770(13) -0.2854(4) 0.0245(8) Uani 1 1 d . . . C1 C 0.1024(2) 0.2062(2) 0.0490(6) 0.0248(12) Uani 1 1 d . . . C2 C 0.1671(2) 0.2091(2) 0.1788(6) 0.0238(11) Uani 1 1 d . . . C3 C 0.2082(3) 0.2594(2) 0.1641(7) 0.0381(14) Uani 1 1 d . . . H1 H 0.1927 0.2909 0.0858 0.046 Uiso 1 1 calc R . . C4 C 0.2719(3) 0.2629(3) 0.2650(7) 0.0428(16) Uani 1 1 d . . . H2 H 0.2993 0.2959 0.2521 0.051 Uiso 1 1 calc R . . C5 C 0.2941(3) 0.2173(3) 0.3841(7) 0.0451(16) Uani 1 1 d . . . H3 H 0.3361 0.2199 0.4552 0.054 Uiso 1 1 calc R . . C6 C 0.2536(3) 0.1679(3) 0.3968(6) 0.0370(14) Uani 1 1 d . . . H4 H 0.2694 0.1370 0.4767 0.044 Uiso 1 1 calc R . . C7 C 0.1896(2) 0.1619(2) 0.2946(6) 0.0258(12) Uani 1 1 d . . . C8 C 0.1517(2) 0.1043(2) 0.3123(5) 0.0247(12) Uani 1 1 d . . . C9 C 0.1763(3) 0.0477(2) 0.2665(6) 0.0383(14) Uani 1 1 d . . . H5 H 0.2131 0.0484 0.2220 0.046 Uiso 1 1 calc R . . C10 C 0.1472(3) -0.0093(3) 0.2854(7) 0.0474(17) Uani 1 1 d . . . H6 H 0.1645 -0.0462 0.2537 0.057 Uiso 1 1 calc R . . C11 C 0.0925(3) -0.0112(3) 0.3516(7) 0.0450(16) Uani 1 1 d . . . H7 H 0.0719 -0.0492 0.3618 0.054 Uiso 1 1 calc R . . C12 C 0.0689(3) 0.0444(2) 0.4024(6) 0.0335(13) Uani 1 1 d . . . H8 H 0.0329 0.0432 0.4501 0.040 Uiso 1 1 calc R . . C13 C 0.0975(2) 0.1019(2) 0.3841(6) 0.0224(12) Uani 1 1 d . . . C14 C 0.0691(2) 0.1577(2) 0.4509(6) 0.0216(11) Uani 1 1 d . . . C21 C 0.0568(2) 0.3415(2) -0.3491(6) 0.0235(12) Uani 1 1 d . . . C22 C 0.0784(2) 0.3962(2) -0.2290(6) 0.0226(12) Uani 1 1 d . . . C23 C 0.0358(2) 0.44484(19) -0.2078(6) 0.0231(12) Uani 1 1 d . . . C24 C 0.0625(3) 0.4954(2) -0.1046(6) 0.0323(13) Uani 1 1 d . . . H9 H 0.0355 0.5286 -0.0916 0.039 Uiso 1 1 calc R . . C25 C 0.1278(3) 0.4967(2) -0.0224(7) 0.0432(15) Uani 1 1 d . . . H10 H 0.1445 0.5308 0.0453 0.052 Uiso 1 1 calc R . . C26 C 0.1697(3) 0.4475(2) -0.0389(6) 0.0387(14) Uani 1 1 d . . . H11 H 0.2139 0.4482 0.0188 0.046 Uiso 1 1 calc R . . C27 C 0.1440(2) 0.3978(2) -0.1431(6) 0.0295(13) Uani 1 1 d . . . H12 H 0.1715 0.3647 -0.1554 0.035 Uiso 1 1 calc R . . H51 H 0.101(3) 0.361(3) 0.133(4) 0.12(3) Uiso 1 1 d D . . H52 H 0.098(4) 0.3940(19) 0.303(7) 0.13(3) Uiso 1 1 d D . . 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 Y1 0.0224(4) 0.0218(4) 0.0161(4) 0.000 0.0052(3) 0.000 Y2 0.0229(4) 0.0205(4) 0.0153(4) 0.000 0.0057(3) 0.000 O1 0.0270(19) 0.0257(18) 0.0234(19) 0.0050(16) 0.0062(15) 0.0050(16) O2 0.039(2) 0.0271(19) 0.021(2) -0.0009(15) 0.0081(17) -0.0013(16) O3 0.0242(19) 0.0337(19) 0.0169(19) -0.0006(14) 0.0072(15) 0.0052(17) O4 0.050(3) 0.052(3) 0.036(3) -0.014(2) 0.026(2) -0.024(2) O5 0.044(2) 0.0303(19) 0.020(2) 0.0044(15) 0.0143(18) 0.0113(17) O6 0.033(2) 0.0307(19) 0.023(2) -0.0095(16) -0.0031(17) 0.0058(17) O7 0.0254(19) 0.0214(18) 0.029(2) 0.0021(16) 0.0109(16) -0.0008(16) C1 0.030(3) 0.028(3) 0.018(3) 0.004(2) 0.009(2) -0.002(3) C2 0.014(3) 0.037(3) 0.025(3) -0.008(2) 0.014(2) 0.000(2) C3 0.039(4) 0.048(3) 0.031(4) -0.007(3) 0.017(3) -0.003(3) C4 0.028(3) 0.060(4) 0.047(4) -0.023(3) 0.021(3) -0.017(3) C5 0.021(3) 0.075(5) 0.034(4) -0.023(3) -0.002(3) 0.009(3) C6 0.028(3) 0.051(4) 0.027(3) -0.014(3) -0.002(3) 0.016(3) C7 0.025(3) 0.035(3) 0.018(3) -0.003(2) 0.007(2) 0.010(3) C8 0.025(3) 0.035(3) 0.010(3) -0.002(2) -0.005(2) 0.006(2) C9 0.042(4) 0.046(4) 0.027(3) -0.007(3) 0.008(3) 0.020(3) C10 0.065(5) 0.033(3) 0.037(4) -0.009(3) 0.000(3) 0.024(3) C11 0.069(5) 0.030(3) 0.030(3) -0.001(3) 0.000(3) 0.006(3) C12 0.048(4) 0.030(3) 0.022(3) 0.003(2) 0.007(3) 0.004(3) C13 0.024(3) 0.025(3) 0.016(3) 0.002(2) 0.002(2) 0.008(2) C14 0.015(3) 0.029(3) 0.017(3) 0.000(2) -0.004(2) -0.001(2) C21 0.015(3) 0.030(3) 0.031(3) -0.001(2) 0.014(2) -0.007(2) C22 0.032(3) 0.022(3) 0.018(3) 0.000(2) 0.012(2) -0.004(2) C23 0.032(3) 0.021(3) 0.020(3) 0.004(2) 0.013(2) -0.006(2) C24 0.040(4) 0.027(3) 0.037(3) -0.008(3) 0.024(3) -0.008(3) C25 0.057(4) 0.041(4) 0.037(4) -0.021(3) 0.023(3) -0.018(3) C26 0.038(4) 0.051(4) 0.025(3) -0.007(3) 0.005(3) -0.011(3) C27 0.031(3) 0.035(3) 0.025(3) -0.001(2) 0.011(3) -0.002(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 Y1 O1 2.243(3) 2 ? Y1 O1 2.243(3) . ? Y1 O3 2.418(3) . ? Y1 O3 2.418(3) 2 ? Y1 O2 2.418(3) . ? Y1 O2 2.418(3) 2 ? Y1 O4 2.434(4) 2 ? Y1 O4 2.434(4) . ? Y2 O7 2.254(3) . ? Y2 O7 2.254(3) 2_554 ? Y2 O5 2.269(3) . ? Y2 O5 2.269(3) 2_554 ? Y2 O6 2.363(3) 2_554 ? Y2 O6 2.363(3) . ? Y2 O3 2.572(3) . ? Y2 O3 2.572(3) 2_554 ? Y2 C1 2.831(5) . ? Y2 C1 2.831(5) 2_554 ? O1 C14 1.270(5) . ? O2 C21 1.265(5) 1_556 ? O3 C1 1.284(5) . ? O4 H51 0.943(10) . ? O4 H52 0.943(10) . ? O5 C14 1.265(5) 1_554 ? O6 C1 1.250(5) . ? O7 C21 1.255(5) . ? C1 C2 1.505(6) . ? C2 C7 1.384(6) . ? C2 C3 1.398(6) . ? C3 C4 1.387(7) . ? C3 H1 0.9300 . ? C4 C5 1.375(7) . ? C4 H2 0.9300 . ? C5 C6 1.372(7) . ? C5 H3 0.9300 . ? C6 C7 1.402(7) . ? C6 H4 0.9300 . ? C7 C8 1.489(6) . ? C8 C9 1.398(6) . ? C8 C13 1.402(6) . ? C9 C10 1.384(7) . ? C9 H5 0.9300 . ? C10 C11 1.382(8) . ? C10 H6 0.9300 . ? C11 C12 1.388(7) . ? C11 H7 0.9300 . ? C12 C13 1.387(6) . ? C12 H8 0.9300 . ? C13 C14 1.493(6) . ? C14 O5 1.265(5) 1_556 ? C21 O2 1.265(5) 1_554 ? C21 C22 1.521(6) . ? C22 C27 1.382(6) . ? C22 C23 1.407(6) . ? C23 C24 1.399(6) . ? C23 C23 1.489(9) 2_554 ? C24 C25 1.368(7) . ? C24 H9 0.9300 . ? C25 C26 1.393(7) . ? C25 H10 0.9300 . ? C26 C27 1.385(6) . ? C26 H11 0.9300 . ? C27 H12 0.9300 . ? 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 O1 Y1 O1 87.68(15) 2 . ? O1 Y1 O3 77.96(11) 2 . ? O1 Y1 O3 72.78(10) . . ? O1 Y1 O3 72.77(10) 2 2 ? O1 Y1 O3 77.96(11) . 2 ? O3 Y1 O3 139.04(14) . 2 ? O1 Y1 O2 146.47(11) 2 . ? O1 Y1 O2 90.50(10) . . ? O3 Y1 O2 133.03(11) . . ? O3 Y1 O2 74.11(10) 2 . ? O1 Y1 O2 90.50(10) 2 2 ? O1 Y1 O2 146.47(11) . 2 ? O3 Y1 O2 74.11(10) . 2 ? O3 Y1 O2 133.03(11) 2 2 ? O2 Y1 O2 108.55(15) . 2 ? O1 Y1 O4 93.34(12) 2 2 ? O1 Y1 O4 147.02(12) . 2 ? O3 Y1 O4 139.59(12) . 2 ? O3 Y1 O4 70.96(12) 2 2 ? O2 Y1 O4 70.88(12) . 2 ? O2 Y1 O4 66.50(12) 2 2 ? O1 Y1 O4 147.02(12) 2 . ? O1 Y1 O4 93.34(12) . . ? O3 Y1 O4 70.96(12) . . ? O3 Y1 O4 139.59(12) 2 . ? O2 Y1 O4 66.50(12) . . ? O2 Y1 O4 70.88(12) 2 . ? O4 Y1 O4 103.09(19) 2 . ? O7 Y2 O7 81.63(15) . 2_554 ? O7 Y2 O5 88.01(11) . . ? O7 Y2 O5 150.16(11) 2_554 . ? O7 Y2 O5 150.16(11) . 2_554 ? O7 Y2 O5 88.01(11) 2_554 2_554 ? O5 Y2 O5 113.24(16) . 2_554 ? O7 Y2 O6 130.46(11) . 2_554 ? O7 Y2 O6 85.53(11) 2_554 2_554 ? O5 Y2 O6 80.09(12) . 2_554 ? O5 Y2 O6 75.93(11) 2_554 2_554 ? O7 Y2 O6 85.53(11) . . ? O7 Y2 O6 130.46(11) 2_554 . ? O5 Y2 O6 75.93(11) . . ? O5 Y2 O6 80.09(12) 2_554 . ? O6 Y2 O6 135.67(15) 2_554 . ? O7 Y2 O3 73.85(10) . . ? O7 Y2 O3 77.83(10) 2_554 . ? O5 Y2 O3 125.91(10) . . ? O5 Y2 O3 76.64(10) 2_554 . ? O6 Y2 O3 148.25(11) 2_554 . ? O6 Y2 O3 52.65(10) . . ? O7 Y2 O3 77.84(10) . 2_554 ? O7 Y2 O3 73.85(10) 2_554 2_554 ? O5 Y2 O3 76.64(10) . 2_554 ? O5 Y2 O3 125.91(10) 2_554 2_554 ? O6 Y2 O3 52.65(10) 2_554 2_554 ? O6 Y2 O3 148.25(11) . 2_554 ? O3 Y2 O3 142.32(14) . 2_554 ? O7 Y2 C1 76.29(12) . . ? O7 Y2 C1 104.73(13) 2_554 . ? O5 Y2 C1 99.80(13) . . ? O5 Y2 C1 79.47(12) 2_554 . ? O6 Y2 C1 152.99(13) 2_554 . ? O6 Y2 C1 25.90(11) . . ? O3 Y2 C1 26.95(11) . . ? O3 Y2 C1 153.99(12) 2_554 . ? O7 Y2 C1 104.73(13) . 2_554 ? O7 Y2 C1 76.29(12) 2_554 2_554 ? O5 Y2 C1 79.47(12) . 2_554 ? O5 Y2 C1 99.79(13) 2_554 2_554 ? O6 Y2 C1 25.90(11) 2_554 2_554 ? O6 Y2 C1 152.99(13) . 2_554 ? O3 Y2 C1 153.99(12) . 2_554 ? O3 Y2 C1 26.95(11) 2_554 2_554 ? C1 Y2 C1 178.69(19) . 2_554 ? C14 O1 Y1 142.3(3) . . ? C21 O2 Y1 133.5(3) 1_556 . ? C1 O3 Y1 135.9(3) . . ? C1 O3 Y2 87.8(3) . . ? Y1 O3 Y2 124.82(12) . . ? Y1 O4 H51 117(4) . . ? Y1 O4 H52 122(5) . . ? H51 O4 H52 113(6) . . ? C14 O5 Y2 137.3(3) 1_554 . ? C1 O6 Y2 98.5(3) . . ? C21 O7 Y2 135.3(3) . . ? O6 C1 O3 120.1(4) . . ? O6 C1 C2 118.6(4) . . ? O3 C1 C2 121.1(4) . . ? O6 C1 Y2 55.6(2) . . ? O3 C1 Y2 65.2(2) . . ? C2 C1 Y2 166.0(3) . . ? C7 C2 C3 120.2(4) . . ? C7 C2 C1 123.3(4) . . ? C3 C2 C1 116.0(4) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H1 119.6 . . ? C2 C3 H1 119.6 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 H2 120.2 . . ? C3 C4 H2 120.2 . . ? C6 C5 C4 119.2(5) . . ? C6 C5 H3 120.4 . . ? C4 C5 H3 120.4 . . ? C5 C6 C7 122.9(5) . . ? C5 C6 H4 118.6 . . ? C7 C6 H4 118.6 . . ? C2 C7 C6 117.3(5) . . ? C2 C7 C8 124.6(4) . . ? C6 C7 C8 118.1(5) . . ? C9 C8 C13 118.0(5) . . ? C9 C8 C7 116.6(5) . . ? C13 C8 C7 125.2(4) . . ? C10 C9 C8 121.8(5) . . ? C10 C9 H5 119.1 . . ? C8 C9 H5 119.1 . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H6 120.0 . . ? C9 C10 H6 120.0 . . ? C10 C11 C12 118.8(6) . . ? C10 C11 H7 120.6 . . ? C12 C11 H7 120.6 . . ? C13 C12 C11 121.9(5) . . ? C13 C12 H8 119.1 . . ? C11 C12 H8 119.1 . . ? C12 C13 C8 119.5(4) . . ? C12 C13 C14 116.3(4) . . ? C8 C13 C14 124.1(4) . . ? O5 C14 O1 123.7(4) 1_556 . ? O5 C14 C13 116.7(4) 1_556 . ? O1 C14 C13 119.7(4) . . ? O7 C21 O2 124.7(4) . 1_554 ? O7 C21 C22 116.2(4) . . ? O2 C21 C22 119.1(4) 1_554 . ? C27 C22 C23 120.0(4) . . ? C27 C22 C21 116.7(4) . . ? C23 C22 C21 123.2(4) . . ? C24 C23 C22 118.1(4) . . ? C24 C23 C23 119.3(4) . 2_554 ? C22 C23 C23 122.6(3) . 2_554 ? C25 C24 C23 121.1(5) . . ? C25 C24 H9 119.5 . . ? C23 C24 H9 119.5 . . ? C24 C25 C26 121.0(5) . . ? C24 C25 H10 119.5 . . ? C26 C25 H10 119.5 . . ? C27 C26 C25 118.5(5) . . ? C27 C26 H11 120.7 . . ? C25 C26 H11 120.7 . . ? C22 C27 C26 121.3(5) . . ? C22 C27 H12 119.4 . . ? C26 C27 H12 119.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.346 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.095 ### EOF ###