data_h _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H38 Cd3 O28' _chemical_formula_weight 1087.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8386(5) _cell_length_b 11.5023(3) _cell_length_c 11.6566(3) _cell_angle_alpha 117.1610(10) _cell_angle_beta 103.249(2) _cell_angle_gamma 94.302(2) _cell_volume 890.40(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10944 _cell_measurement_theta_min 1.03 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.273 _exptl_crystal_size_mid 0.156 _exptl_crystal_size_min 0.112 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 1.879 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.810 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEXII area-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10126 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3451 _reflns_number_gt 3196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,2004)' _computing_cell_refinement 'SAINT (Bruker,2004)' _computing_data_reduction 'SAINT ' _computing_structure_solution 'SHELXS97 (Sheldrick,1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick,1997)' _computing_molecular_graphics 'SHELXTL (Bruker,2002)' _computing_publication_material 'SHELXL97' _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^)+(0.0470P)^2^+0.8523P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3451 _refine_ls_number_parameters 241 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _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 Cd1 Cd 0.0000 0.0000 0.5000 0.02856(10) Uani 1 2 d S . . Cd2 Cd 0.04876(3) 0.249475(18) -0.104516(18) 0.02723(9) Uani 1 1 d . . . O1W O 0.2903(3) 0.1437(2) -0.0941(2) 0.0469(6) Uani 1 1 d D . . H1WA H 0.3826 0.2032 -0.0432 0.056 Uiso 1 1 d RD . . H1WB H 0.2759 0.0925 -0.0637 0.056 Uiso 1 1 d RD . . O2W O -0.2166(3) 0.3273(2) -0.1235(2) 0.0379(5) Uani 1 1 d D . . H2WA H -0.1929 0.4014 -0.1145 0.045 Uiso 1 1 d RD . . H2WB H -0.2614 0.3288 -0.0659 0.045 Uiso 1 1 d RD . . O3W O 0.2427(4) -0.0301(3) 0.6254(3) 0.0611(7) Uani 1 1 d D . . H3WA H 0.3277 -0.0020 0.6068 0.073 Uiso 1 1 d RD . . H3WB H 0.2500 0.0197 0.7058 0.073 Uiso 1 1 d RD . . O4W O 0.2222(4) -0.0648(3) 0.9507(3) 0.0657(8) Uani 1 1 d D . . H4WA H 0.1562 -0.1254 0.8785 0.079 Uiso 1 1 d RD . . H4WB H 0.1750 -0.0491 1.0098 0.079 Uiso 1 1 d RD . . O5W O -0.4685(5) 0.1186(3) 0.6371(4) 0.0878(12) Uani 1 1 d D . . H5WA H -0.4057 0.1850 0.7096 0.105 Uiso 1 1 d RD . . H5WB H -0.5056 0.1353 0.5737 0.105 Uiso 1 1 d RD . . O6W O -0.3682(4) 0.3026(3) 1.0612(3) 0.0591(7) Uani 1 1 d D . . H6WA H -0.3899 0.3775 1.0887 0.071 Uiso 1 1 d RD . . H6WB H -0.2738 0.2997 1.1062 0.071 Uiso 1 1 d RD . . O1 O 0.1853(3) 0.4254(2) 0.10061(19) 0.0356(5) Uani 1 1 d . . . O2 O 0.0617(4) 0.2684(2) 0.1290(2) 0.0525(7) Uani 1 1 d . . . O3 O 0.5432(3) 0.77880(19) 0.55449(19) 0.0315(5) Uani 1 1 d . . . O4 O 0.8295(4) 0.9414(2) 0.6046(2) 0.0505(7) Uani 1 1 d . . . O5 O 0.8640(3) 1.0535(2) 0.8244(2) 0.0399(5) Uani 1 1 d . . . O6 O 0.2154(3) 0.48172(18) 0.64560(18) 0.0275(4) Uani 1 1 d . . . O7 O 0.0447(3) 0.2104(2) 0.6822(2) 0.0344(5) Uani 1 1 d . . . O8 O 0.1687(4) 0.4184(2) 0.8304(2) 0.0472(6) Uani 1 1 d . . . C1 C 0.2247(3) 0.4702(2) 0.3261(2) 0.0217(5) Uani 1 1 d . . . C2 C 0.3468(4) 0.5871(3) 0.3766(3) 0.0234(5) Uani 1 1 d . . . H2 H 0.3804 0.6122 0.3183 0.028 Uiso 1 1 calc R . . C3 C 0.4194(3) 0.6673(2) 0.5158(3) 0.0229(5) Uani 1 1 d . . . C4 C 0.3703(3) 0.6315(2) 0.6034(2) 0.0221(5) Uani 1 1 d . . . H4 H 0.4169 0.6866 0.6963 0.027 Uiso 1 1 calc R . . C5 C 0.2492(3) 0.5110(3) 0.5504(3) 0.0210(5) Uani 1 1 d . . . C6 C 0.1747(3) 0.4303(3) 0.4129(3) 0.0236(5) Uani 1 1 d . . . H6 H 0.0928 0.3510 0.3784 0.028 Uiso 1 1 calc R . . C7 C 0.1505(4) 0.3817(3) 0.1761(3) 0.0278(6) Uani 1 1 d . . . C8 C 0.6360(4) 0.8625(3) 0.6937(3) 0.0254(6) Uani 1 1 d . . . H8B H 0.6822 0.8090 0.7335 0.031 Uiso 1 1 calc R . . H8A H 0.5551 0.9102 0.7409 0.031 Uiso 1 1 calc R . . C9 C 0.7891(4) 0.9608(3) 0.7067(3) 0.0255(6) Uani 1 1 d . . . C10 C 0.1205(4) 0.3495(3) 0.5963(3) 0.0257(6) Uani 1 1 d . . . H10B H 0.1799 0.2852 0.5402 0.031 Uiso 1 1 calc R . . H10A H -0.0004 0.3365 0.5415 0.031 Uiso 1 1 calc R . . C11 C 0.1142(4) 0.3285(3) 0.7131(3) 0.0273(6) Uani 1 1 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 Cd1 0.03415(17) 0.02568(16) 0.02425(17) 0.01111(13) 0.01072(12) -0.00156(12) Cd2 0.03643(14) 0.02296(12) 0.01482(12) 0.00667(9) 0.00386(9) -0.00605(9) O1W 0.0440(13) 0.0484(14) 0.0440(14) 0.0240(12) 0.0046(11) 0.0031(11) O2W 0.0473(12) 0.0321(11) 0.0349(12) 0.0184(10) 0.0106(10) 0.0024(9) O3W 0.0568(16) 0.080(2) 0.0516(16) 0.0334(15) 0.0178(13) 0.0297(14) O4W 0.0729(19) 0.0628(18) 0.0561(17) 0.0320(15) 0.0107(15) -0.0090(15) O5W 0.096(3) 0.069(2) 0.073(2) 0.0425(18) -0.0251(18) -0.0196(18) O6W 0.0581(16) 0.0584(17) 0.0425(15) 0.0142(13) 0.0103(12) -0.0034(13) O1 0.0571(13) 0.0282(10) 0.0136(9) 0.0086(8) 0.0043(9) -0.0039(9) O2 0.0780(18) 0.0313(12) 0.0229(11) 0.0053(9) -0.0004(11) -0.0268(12) O3 0.0408(11) 0.0268(10) 0.0160(9) 0.0084(8) 0.0011(8) -0.0176(8) O4 0.0673(16) 0.0329(12) 0.0406(13) 0.0062(10) 0.0315(12) -0.0165(11) O5 0.0494(13) 0.0290(11) 0.0254(11) 0.0108(9) -0.0033(9) -0.0178(9) O6 0.0390(10) 0.0220(9) 0.0176(9) 0.0091(8) 0.0070(8) -0.0068(8) O7 0.0548(13) 0.0251(10) 0.0265(11) 0.0148(9) 0.0157(10) -0.0008(9) O8 0.0797(17) 0.0325(12) 0.0216(11) 0.0109(10) 0.0131(11) -0.0096(11) C1 0.0244(12) 0.0208(12) 0.0155(12) 0.0074(10) 0.0026(10) -0.0003(10) C2 0.0290(13) 0.0234(13) 0.0169(12) 0.0110(10) 0.0050(10) -0.0026(10) C3 0.0243(12) 0.0202(12) 0.0200(13) 0.0091(10) 0.0036(10) -0.0044(10) C4 0.0275(12) 0.0198(12) 0.0118(11) 0.0050(10) 0.0018(10) -0.0043(10) C5 0.0247(12) 0.0228(13) 0.0182(12) 0.0125(10) 0.0069(10) 0.0018(10) C6 0.0251(12) 0.0194(12) 0.0223(13) 0.0095(10) 0.0043(10) -0.0035(10) C7 0.0338(14) 0.0234(13) 0.0187(13) 0.0078(11) 0.0023(11) -0.0017(11) C8 0.0299(13) 0.0226(13) 0.0145(12) 0.0056(10) 0.0018(10) -0.0075(10) C9 0.0280(13) 0.0185(12) 0.0263(14) 0.0100(11) 0.0052(11) -0.0004(10) C10 0.0355(14) 0.0194(12) 0.0213(13) 0.0101(11) 0.0091(11) -0.0026(11) C11 0.0346(14) 0.0259(14) 0.0247(14) 0.0139(12) 0.0122(12) 0.0021(11) _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 Cd1 O4 2.255(2) 1_445 ? Cd1 O4 2.255(2) 2_666 ? Cd1 O3W 2.272(3) 2_556 ? Cd1 O3W 2.272(3) . ? Cd1 O7 2.308(2) 2_556 ? Cd1 O7 2.308(2) . ? Cd2 O1 2.2454(19) . ? Cd2 O5 2.2630(19) 1_444 ? Cd2 O7 2.308(2) 1_554 ? Cd2 O2W 2.330(2) . ? Cd2 O1W 2.335(2) . ? Cd2 O8 2.575(2) 1_554 ? Cd2 O2 2.607(2) . ? O1W H1WA 0.8378 . ? O1W H1WB 0.8269 . ? O2W H2WA 0.8105 . ? O2W H2WB 0.8209 . ? O3W H3WA 0.8333 . ? O3W H3WB 0.8309 . ? O4W H4WA 0.8200 . ? O4W H4WB 0.8101 . ? O5W H5WA 0.8388 . ? O5W H5WB 0.8414 . ? O6W H6WA 0.8175 . ? O6W H6WB 0.8160 . ? O1 C7 1.262(3) . ? O2 C7 1.234(4) . ? O3 C3 1.369(3) . ? O3 C8 1.420(3) . ? O4 C9 1.228(4) . ? O4 Cd1 2.255(2) 1_665 ? O5 C9 1.251(3) . ? O5 Cd2 2.2630(19) 1_666 ? O6 C5 1.371(3) . ? O6 C10 1.425(3) . ? O7 C11 1.274(3) . ? O7 Cd2 2.308(2) 1_556 ? O8 C11 1.224(4) . ? O8 Cd2 2.575(2) 1_556 ? C1 C2 1.378(4) . ? C1 C6 1.402(4) . ? C1 C7 1.501(3) . ? C2 C3 1.393(4) . ? C2 H2 0.9300 . ? C3 C4 1.379(4) . ? C4 C5 1.398(4) . ? C4 H4 0.9300 . ? C5 C6 1.379(4) . ? C6 H6 0.9300 . ? C8 C9 1.518(4) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C10 C11 1.498(4) . ? C10 H10B 0.9700 . ? C10 H10A 0.9700 . ? 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 O4 Cd1 O4 180.0 1_445 2_666 ? O4 Cd1 O3W 91.03(11) 1_445 2_556 ? O4 Cd1 O3W 88.97(11) 2_666 2_556 ? O4 Cd1 O3W 88.97(11) 1_445 . ? O4 Cd1 O3W 91.03(11) 2_666 . ? O3W Cd1 O3W 180.000(1) 2_556 . ? O4 Cd1 O7 96.70(8) 1_445 2_556 ? O4 Cd1 O7 83.30(7) 2_666 2_556 ? O3W Cd1 O7 87.01(10) 2_556 2_556 ? O3W Cd1 O7 92.99(10) . 2_556 ? O4 Cd1 O7 83.30(8) 1_445 . ? O4 Cd1 O7 96.70(8) 2_666 . ? O3W Cd1 O7 92.99(10) 2_556 . ? O3W Cd1 O7 87.01(10) . . ? O7 Cd1 O7 180.0 2_556 . ? O1 Cd2 O5 133.05(8) . 1_444 ? O1 Cd2 O7 131.49(7) . 1_554 ? O5 Cd2 O7 95.44(7) 1_444 1_554 ? O1 Cd2 O2W 93.06(8) . . ? O5 Cd2 O2W 83.84(8) 1_444 . ? O7 Cd2 O2W 90.75(8) 1_554 . ? O1 Cd2 O1W 92.02(9) . . ? O5 Cd2 O1W 88.35(9) 1_444 . ? O7 Cd2 O1W 90.32(9) 1_554 . ? O2W Cd2 O1W 172.19(8) . . ? O1 Cd2 O8 79.28(7) . 1_554 ? O5 Cd2 O8 146.54(7) 1_444 1_554 ? O7 Cd2 O8 52.73(7) 1_554 1_554 ? O2W Cd2 O8 86.33(8) . 1_554 ? O1W Cd2 O8 100.45(9) . 1_554 ? O1 Cd2 O2 52.68(7) . . ? O5 Cd2 O2 80.68(7) 1_444 . ? O7 Cd2 O2 173.83(8) 1_554 . ? O2W Cd2 O2 93.59(9) . . ? O1W Cd2 O2 84.80(9) . . ? O8 Cd2 O2 131.92(7) 1_554 . ? Cd2 O1W H1WA 107.6 . . ? Cd2 O1W H1WB 111.2 . . ? H1WA O1W H1WB 109.5 . . ? Cd2 O2W H2WA 107.7 . . ? Cd2 O2W H2WB 109.9 . . ? H2WA O2W H2WB 111.2 . . ? Cd1 O3W H3WA 103.2 . . ? Cd1 O3W H3WB 106.6 . . ? H3WA O3W H3WB 109.6 . . ? H4WA O4W H4WB 110.1 . . ? H5WA O5W H5WB 114.1 . . ? H6WA O6W H6WB 113.9 . . ? C7 O1 Cd2 101.13(16) . . ? C7 O2 Cd2 84.73(18) . . ? C3 O3 C8 119.1(2) . . ? C9 O4 Cd1 151.11(19) . 1_665 ? C9 O5 Cd2 129.26(19) . 1_666 ? C5 O6 C10 116.05(19) . . ? C11 O7 Cd1 135.58(18) . . ? C11 O7 Cd2 98.33(17) . 1_556 ? Cd1 O7 Cd2 123.79(9) . 1_556 ? C11 O8 Cd2 87.03(17) . 1_556 ? C2 C1 C6 120.9(2) . . ? C2 C1 C7 119.3(2) . . ? C6 C1 C7 119.7(2) . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? O3 C3 C4 124.7(2) . . ? O3 C3 C2 114.3(2) . . ? C4 C3 C2 120.9(2) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? O6 C5 C6 124.5(2) . . ? O6 C5 C4 114.4(2) . . ? C6 C5 C4 121.1(2) . . ? C5 C6 C1 118.7(2) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? O2 C7 O1 121.5(3) . . ? O2 C7 C1 120.2(3) . . ? O1 C7 C1 118.3(2) . . ? O3 C8 C9 108.4(2) . . ? O3 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? O3 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? H8B C8 H8A 108.4 . . ? O4 C9 O5 126.9(3) . . ? O4 C9 C8 118.5(2) . . ? O5 C9 C8 114.6(2) . . ? O6 C10 C11 109.4(2) . . ? O6 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? O6 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? H10B C10 H10A 108.2 . . ? O8 C11 O7 121.8(3) . . ? O8 C11 C10 122.8(3) . . ? O7 C11 C10 115.4(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O6W 0.84 1.98 2.794(3) 164.8 1_654 O1W H1WB O4W 0.83 1.92 2.719(4) 162.9 1_554 O2W H2WA O1 0.81 1.92 2.719(3) 169.0 2_565 O2W H2WB O6W 0.82 1.98 2.795(4) 171.1 1_554 O3W H3WA O5W 0.83 1.89 2.671(5) 156.3 1_655 O3W H3WB O1W 0.83 2.03 2.862(4) 175.2 1_556 O4W H4WA O2 0.82 2.24 2.753(4) 121.1 2_556 O4W H4WB O5 0.81 2.05 2.803(4) 155.2 2_667 O5W H5WA O2W 0.84 2.02 2.845(4) 169.2 1_556 O5W H5WB O3 0.84 2.12 2.939(4) 165.0 2_566 O6W H6WA O8 0.82 2.45 2.996(3) 124.7 2_567 O6W H6WB O4W 0.82 2.56 3.001(4) 115.3 2_557 O6W H6WB O2 0.82 2.65 3.376(4) 149.0 1_556 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.516 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.082