# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Temperature Dependent Charge Distribution in Three-Dimensional Homochiral Cadmium Camphorates ; _publ_contact_author_address ; Department of Chemistry and Biochemistry California State University, Long Beach 1250 Bellflower Boulevard, Long Beach, CA 90840 ; _publ_contact_author_email xbu@csulb.edu _publ_contact_author_fax ? # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Xianhui Bu' loop_ _publ_author_name 'Xianhui Bu' 'Jian Zhang' # Attachment '1.cif' data_664303 _database_code_depnum_ccdc_archive 'CCDC 664303' _publ_section_exptl_refinement ; ? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H34 Cd2 O11' _chemical_formula_weight 675.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 13.4066(2) _cell_length_b 13.4066(2) _cell_length_c 32.0618(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5762.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 7599 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 21.07 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .22 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .723 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29016 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.17 _reflns_number_total 4081 _reflns_number_gt 3440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All H atoms bonded to the water molecules were located from different Fourier maps and refined as riding atoms of the parent oxygen atoms. ; _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(7) _chemical_absolute_configuration rm _refine_ls_number_reflns 4081 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _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 -0.06534(6) -0.53045(6) 0.11229(2) 0.0461(2) Uani 1 1 d . . . Cd2 Cd 0.39856(7) -0.08710(6) 0.01411(2) 0.0622(3) Uani 1 1 d . . . O1 O 0.0814(5) -0.4565(6) 0.1363(2) 0.0588(18) Uani 1 1 d . . . O2 O 0.0664(5) -0.4654(6) 0.0688(2) 0.067(2) Uani 1 1 d . . . O2W O 0.4515(11) 0.0698(8) 0.0086(3) 0.151(6) Uani 1 1 d . . . H2WA H 0.4804 0.0783 -0.0147 0.226 Uiso 1 1 d R . . H2WB H 0.4020 0.1081 0.0127 0.226 Uiso 1 1 d R . . O3W O 0.2544(8) -0.0333(9) -0.0173(3) 0.117(4) Uani 1 1 d . . . H3WA H 0.1873 -0.0223 -0.0157 0.176 Uiso 1 1 d R . . H3WB H 0.2602 -0.0525 -0.0440 0.176 Uiso 1 1 d R . . O3 O 0.3526(5) -0.0767(5) 0.0800(2) 0.0583(19) Uani 1 1 d . . . O1W O 0.5570(8) -0.1195(10) 0.0356(3) 0.134(5) Uani 1 1 d . . . H1WA H 0.5964 -0.1020 0.0550 0.201 Uiso 1 1 d R . . H1WB H 0.5907 -0.1412 0.0150 0.201 Uiso 1 1 d R . . O4 O 0.3592(6) -0.1220(6) 0.1466(2) 0.071(2) Uani 1 1 d . . . O5 O -0.0399(6) -0.6581(5) 0.1624(2) 0.0593(19) Uani 1 1 d . . . O6 O 0.0046(6) -0.6883(6) 0.0980(2) 0.063(2) Uani 1 1 d . . . O7 O 0.3452(6) -0.9250(5) 0.19530(19) 0.058(2) Uani 1 1 d . . . O8 O 0.2478(6) -0.8914(7) 0.2461(2) 0.081(3) Uani 1 1 d . . . C1 C 0.2172(8) -0.3935(8) 0.0932(3) 0.050(3) Uani 1 1 d . . . C2 C 0.2129(7) -0.2784(7) 0.0915(3) 0.044(2) Uani 1 1 d . . . C3 C 0.3239(7) -0.2513(7) 0.0971(3) 0.048(3) Uani 1 1 d . . . H3A H 0.3572 -0.2641 0.0704 0.058 Uiso 1 1 calc R . . C4 C 0.3655(8) -0.3276(9) 0.1290(4) 0.071(3) Uani 1 1 d . . . H4A H 0.4291 -0.3541 0.1197 0.085 Uiso 1 1 calc R . . H4B H 0.3747 -0.2966 0.1561 0.085 Uiso 1 1 calc R . . C5 C 0.2880(8) -0.4097(9) 0.1314(4) 0.071(3) Uani 1 1 d . . . H5A H 0.2509 -0.4052 0.1573 0.085 Uiso 1 1 calc R . . H5B H 0.3195 -0.4747 0.1299 0.085 Uiso 1 1 calc R . . C6 C 0.2627(10) -0.4389(9) 0.0549(3) 0.075(4) Uani 1 1 d . . . H6A H 0.2188 -0.4292 0.0316 0.113 Uiso 1 1 calc R . . H6B H 0.2726 -0.5091 0.0593 0.113 Uiso 1 1 calc R . . H6C H 0.3257 -0.4077 0.0493 0.113 Uiso 1 1 calc R . . C7 C 0.1713(10) -0.2402(9) 0.0504(3) 0.074(4) Uani 1 1 d . . . H7A H 0.2096 -0.2671 0.0278 0.111 Uiso 1 1 calc R . . H7B H 0.1749 -0.1687 0.0499 0.111 Uiso 1 1 calc R . . H7C H 0.1030 -0.2607 0.0477 0.111 Uiso 1 1 calc R . . C8 C 0.1506(9) -0.2349(10) 0.1301(4) 0.078(4) Uani 1 1 d . . . H8A H 0.1484 -0.1634 0.1284 0.117 Uiso 1 1 calc R . . H8B H 0.1822 -0.2542 0.1558 0.117 Uiso 1 1 calc R . . H8C H 0.0839 -0.2609 0.1294 0.117 Uiso 1 1 calc R . . C9 C 0.1154(8) -0.4415(8) 0.0997(3) 0.052(3) Uani 1 1 d . . . C10 C 0.3476(8) -0.1430(9) 0.1096(4) 0.063(3) Uani 1 1 d . . . C11 C 0.0378(7) -0.8153(8) 0.1485(3) 0.052(3) Uani 1 1 d . . . C12 C 0.1537(8) -0.8136(8) 0.1559(3) 0.054(3) Uani 1 1 d . . . C13 C 0.1719(7) -0.9152(8) 0.1800(3) 0.051(3) Uani 1 1 d . . . H13A H 0.1842 -0.9678 0.1594 0.061 Uiso 1 1 calc R . . C14 C 0.0709(9) -0.9384(9) 0.2029(4) 0.071(3) Uani 1 1 d . . . H14A H 0.0452 -1.0030 0.1944 0.085 Uiso 1 1 calc R . . H14B H 0.0803 -0.9386 0.2329 0.085 Uiso 1 1 calc R . . C15 C -0.0007(8) -0.8553(9) 0.1900(3) 0.063(3) Uani 1 1 d . . . H15A H -0.0679 -0.8812 0.1869 0.076 Uiso 1 1 calc R . . H15B H -0.0016 -0.8028 0.2108 0.076 Uiso 1 1 calc R . . C16 C 0.0067(11) -0.8928(8) 0.1134(4) 0.087(4) Uani 1 1 d . . . H16A H -0.0644 -0.8916 0.1098 0.131 Uiso 1 1 calc R . . H16B H 0.0274 -0.9586 0.1215 0.131 Uiso 1 1 calc R . . H16C H 0.0384 -0.8751 0.0875 0.131 Uiso 1 1 calc R . . C17 C 0.2146(12) -0.8169(12) 0.1136(4) 0.105(5) Uani 1 1 d . . . H17A H 0.2848 -0.8160 0.1196 0.158 Uiso 1 1 calc R . . H17B H 0.1976 -0.7600 0.0969 0.158 Uiso 1 1 calc R . . H17C H 0.1983 -0.8768 0.0987 0.158 Uiso 1 1 calc R . . C18 C 0.1831(9) -0.7243(8) 0.1811(4) 0.064(3) Uani 1 1 d . . . H18A H 0.2540 -0.7244 0.1852 0.097 Uiso 1 1 calc R . . H18B H 0.1501 -0.7264 0.2077 0.097 Uiso 1 1 calc R . . H18C H 0.1639 -0.6647 0.1665 0.097 Uiso 1 1 calc R . . C19 C -0.0001(8) -0.7153(8) 0.1371(3) 0.055(3) Uani 1 1 d . . . C20 C 0.2590(8) -0.9095(8) 0.2081(3) 0.050(3) 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 0.0513(5) 0.0521(5) 0.0348(4) 0.0011(3) -0.0011(3) -0.0019(3) Cd2 0.0848(6) 0.0638(5) 0.0379(5) -0.0021(4) -0.0042(4) -0.0095(5) O1 0.056(4) 0.077(5) 0.044(4) -0.003(4) 0.014(3) -0.011(4) O2 0.064(5) 0.091(6) 0.045(4) -0.005(4) 0.001(4) -0.020(4) O2W 0.278(17) 0.104(7) 0.071(6) -0.020(6) 0.060(8) -0.101(10) O3W 0.111(8) 0.178(11) 0.064(6) 0.034(7) 0.005(5) 0.040(8) O3 0.074(5) 0.062(5) 0.039(4) 0.008(4) 0.000(4) -0.009(4) O1W 0.098(7) 0.241(15) 0.062(6) -0.041(7) -0.012(5) 0.011(9) O4 0.101(6) 0.086(6) 0.026(4) -0.019(4) 0.007(4) -0.037(5) O5 0.072(5) 0.060(5) 0.047(4) 0.007(4) 0.004(4) 0.005(4) O6 0.079(5) 0.069(5) 0.043(4) 0.009(4) -0.007(4) 0.005(4) O7 0.063(5) 0.075(5) 0.035(4) -0.001(4) 0.006(3) 0.014(4) O8 0.069(5) 0.138(9) 0.036(4) -0.012(5) 0.003(4) 0.017(5) C1 0.052(6) 0.055(6) 0.043(5) 0.013(5) 0.003(5) 0.000(5) C2 0.045(6) 0.048(6) 0.040(5) -0.003(5) 0.004(4) 0.004(5) C3 0.054(6) 0.051(6) 0.040(6) -0.007(5) 0.004(5) -0.005(5) C4 0.053(7) 0.087(9) 0.073(8) 0.018(7) -0.006(6) -0.005(6) C5 0.052(7) 0.061(7) 0.100(9) 0.006(7) -0.011(6) -0.002(6) C6 0.072(8) 0.077(9) 0.077(8) -0.024(7) 0.014(7) -0.013(7) C7 0.089(10) 0.072(8) 0.061(7) 0.023(6) -0.033(7) -0.024(7) C8 0.056(7) 0.074(9) 0.104(10) -0.014(8) -0.007(7) -0.008(7) C9 0.054(6) 0.051(6) 0.051(7) 0.002(5) -0.004(5) 0.009(5) C10 0.044(6) 0.066(8) 0.079(9) -0.016(7) 0.018(6) -0.009(6) C11 0.040(6) 0.063(7) 0.053(6) 0.006(5) -0.003(5) -0.001(5) C12 0.049(6) 0.072(8) 0.041(6) -0.002(5) 0.008(5) -0.004(6) C13 0.059(7) 0.049(6) 0.044(6) 0.007(5) -0.003(5) 0.002(5) C14 0.073(8) 0.071(8) 0.068(7) 0.018(6) 0.012(6) -0.003(7) C15 0.059(7) 0.068(7) 0.063(7) 0.018(6) 0.009(6) 0.003(6) C16 0.128(12) 0.061(8) 0.073(8) -0.006(6) -0.038(8) -0.019(8) C17 0.110(11) 0.135(13) 0.071(9) 0.065(9) 0.029(9) 0.037(10) C18 0.064(7) 0.042(6) 0.087(9) -0.002(6) -0.017(7) -0.004(5) C19 0.056(7) 0.057(7) 0.053(7) -0.001(6) -0.013(6) -0.004(5) C20 0.056(7) 0.057(7) 0.038(6) 0.002(5) 0.002(5) 0.001(6) _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 O7 2.281(6) 5_435 ? Cd1 O4 2.298(7) 5_445 ? Cd1 O1 2.333(7) . ? Cd1 O6 2.359(7) . ? Cd1 O5 2.372(7) . ? Cd1 O2 2.414(7) . ? Cd1 O3 2.588(7) 5_445 ? Cd1 C9 2.730(11) . ? Cd1 C19 2.746(11) . ? Cd1 C10 2.754(11) 5_445 ? Cd2 O3 2.205(7) . ? Cd2 O2W 2.227(9) . ? Cd2 O1W 2.274(10) . ? Cd2 O8 2.290(8) 2_444 ? Cd2 O3W 2.296(9) . ? Cd2 O7 2.412(6) 2_444 ? Cd2 C20 2.739(10) 2_444 ? O1 C9 1.272(11) . ? O2 C9 1.233(11) . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.9135 . ? O3W H3WB 0.8969 . ? O3 C10 1.301(13) . ? O3 Cd1 2.588(7) 5_545 ? O1W H1WA 0.8498 . ? O1W H1WB 0.8502 . ? O4 C10 1.229(13) . ? O4 Cd1 2.298(7) 5_545 ? O5 C19 1.237(12) . ? O6 C19 1.306(12) . ? O7 C20 1.245(12) . ? O7 Cd1 2.281(6) 5_535 ? O7 Cd2 2.411(6) 4_545 ? O8 C20 1.250(11) . ? O8 Cd2 2.290(8) 4_545 ? C1 C6 1.501(14) . ? C1 C9 1.524(14) . ? C1 C2 1.545(14) . ? C1 C5 1.564(15) . ? C2 C7 1.520(13) . ? C2 C3 1.542(14) . ? C2 C8 1.603(15) . ? C3 C10 1.540(15) . ? C3 C4 1.552(14) . ? C3 H3A 0.9800 . ? C4 C5 1.515(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 Cd1 2.754(11) 5_545 ? C11 C19 1.479(14) . ? C11 C15 1.525(13) . ? C11 C12 1.572(14) . ? C11 C16 1.588(14) . ? C12 C18 1.497(14) . ? C12 C17 1.584(15) . ? C12 C13 1.585(14) . ? C13 C20 1.477(14) . ? C13 C14 1.571(14) . ? C13 H13A 0.9800 . ? C14 C15 1.529(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 Cd2 2.739(10) 4_545 ? 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 O7 Cd1 O4 84.4(3) 5_435 5_445 ? O7 Cd1 O1 145.2(2) 5_435 . ? O4 Cd1 O1 91.9(3) 5_445 . ? O7 Cd1 O6 79.5(3) 5_435 . ? O4 Cd1 O6 161.6(2) 5_445 . ? O1 Cd1 O6 96.3(3) . . ? O7 Cd1 O5 115.8(2) 5_435 . ? O4 Cd1 O5 142.1(2) 5_445 . ? O1 Cd1 O5 87.8(3) . . ? O6 Cd1 O5 55.0(2) . . ? O7 Cd1 O2 90.6(2) 5_435 . ? O4 Cd1 O2 86.0(3) 5_445 . ? O1 Cd1 O2 54.5(2) . . ? O6 Cd1 O2 85.5(3) . . ? O5 Cd1 O2 123.1(3) . . ? O7 Cd1 O3 120.0(3) 5_435 5_445 ? O4 Cd1 O3 53.7(2) 5_445 5_445 ? O1 Cd1 O3 83.5(2) . 5_445 ? O6 Cd1 O3 143.6(2) . 5_445 ? O5 Cd1 O3 88.7(2) . 5_445 ? O2 Cd1 O3 121.6(2) . 5_445 ? O7 Cd1 C9 117.5(3) 5_435 . ? O4 Cd1 C9 89.1(3) 5_445 . ? O1 Cd1 C9 27.7(2) . . ? O6 Cd1 C9 90.6(3) . . ? O5 Cd1 C9 106.7(3) . . ? O2 Cd1 C9 26.8(2) . . ? O3 Cd1 C9 103.9(3) 5_445 . ? O7 Cd1 C19 99.6(3) 5_435 . ? O4 Cd1 C19 168.1(3) 5_445 . ? O1 Cd1 C19 91.1(3) . . ? O6 Cd1 C19 28.4(3) . . ? O5 Cd1 C19 26.7(3) . . ? O2 Cd1 C19 105.1(3) . . ? O3 Cd1 C19 115.4(3) 5_445 . ? C9 Cd1 C19 98.9(3) . . ? O7 Cd1 C10 105.3(3) 5_435 5_445 ? O4 Cd1 C10 26.2(3) 5_445 5_445 ? O1 Cd1 C10 83.7(3) . 5_445 ? O6 Cd1 C10 171.6(3) . 5_445 ? O5 Cd1 C10 116.6(3) . 5_445 ? O2 Cd1 C10 101.2(3) . 5_445 ? O3 Cd1 C10 28.0(3) 5_445 5_445 ? C9 Cd1 C10 93.2(3) . 5_445 ? C19 Cd1 C10 143.3(4) . 5_445 ? O3 Cd2 O2W 96.0(3) . . ? O3 Cd2 O1W 89.1(3) . . ? O2W Cd2 O1W 84.7(5) . . ? O3 Cd2 O8 106.9(3) . 2_444 ? O2W Cd2 O8 155.0(3) . 2_444 ? O1W Cd2 O8 86.0(4) . 2_444 ? O3 Cd2 O3W 99.5(3) . . ? O2W Cd2 O3W 86.4(5) . . ? O1W Cd2 O3W 168.2(4) . . ? O8 Cd2 O3W 99.1(4) 2_444 . ? O3 Cd2 O7 160.3(2) . 2_444 ? O2W Cd2 O7 103.7(3) . 2_444 ? O1W Cd2 O7 93.9(3) . 2_444 ? O8 Cd2 O7 54.0(2) 2_444 2_444 ? O3W Cd2 O7 80.8(3) . 2_444 ? O3 Cd2 C20 133.7(3) . 2_444 ? O2W Cd2 C20 130.0(3) . 2_444 ? O1W Cd2 C20 90.2(3) . 2_444 ? O8 Cd2 C20 26.9(3) 2_444 2_444 ? O3W Cd2 C20 89.6(4) . 2_444 ? O7 Cd2 C20 27.0(3) 2_444 2_444 ? C9 O1 Cd1 93.8(6) . . ? C9 O2 Cd1 91.0(6) . . ? Cd2 O2W H2WA 109.9 . . ? Cd2 O2W H2WB 108.1 . . ? H2WA O2W H2WB 114.2 . . ? Cd2 O3W H3WA 148.7 . . ? Cd2 O3W H3WB 104.8 . . ? H3WA O3W H3WB 100.8 . . ? C10 O3 Cd2 132.0(7) . . ? C10 O3 Cd1 83.1(6) . 5_545 ? Cd2 O3 Cd1 127.0(3) . 5_545 ? Cd2 O1W H1WA 138.5 . . ? Cd2 O1W H1WB 109.1 . . ? H1WA O1W H1WB 109.4 . . ? C10 O4 Cd1 98.1(7) . 5_545 ? C19 O5 Cd1 93.8(6) . . ? C19 O6 Cd1 92.5(6) . . ? C20 O7 Cd1 143.1(7) . 5_535 ? C20 O7 Cd2 91.3(6) . 4_545 ? Cd1 O7 Cd2 125.5(3) 5_535 4_545 ? C20 O8 Cd2 97.0(7) . 4_545 ? C6 C1 C9 107.7(9) . . ? C6 C1 C2 113.1(8) . . ? C9 C1 C2 113.2(9) . . ? C6 C1 C5 109.8(9) . . ? C9 C1 C5 112.2(8) . . ? C2 C1 C5 100.9(8) . . ? C7 C2 C3 112.1(9) . . ? C7 C2 C1 112.4(9) . . ? C3 C2 C1 101.2(8) . . ? C7 C2 C8 110.9(9) . . ? C3 C2 C8 109.1(8) . . ? C1 C2 C8 110.8(8) . . ? C10 C3 C2 116.8(8) . . ? C10 C3 C4 112.1(9) . . ? C2 C3 C4 105.6(8) . . ? C10 C3 H3A 107.3 . . ? C2 C3 H3A 107.3 . . ? C4 C3 H3A 107.3 . . ? C5 C4 C3 105.3(9) . . ? C5 C4 H4A 110.7 . . ? C3 C4 H4A 110.7 . . ? C5 C4 H4B 110.7 . . ? C3 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C4 C5 C1 106.0(10) . . ? C4 C5 H5A 110.5 . . ? C1 C5 H5A 110.5 . . ? C4 C5 H5B 110.5 . . ? C1 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 120.6(10) . . ? O2 C9 C1 118.5(9) . . ? O1 C9 C1 120.9(9) . . ? O2 C9 Cd1 62.1(5) . . ? O1 C9 Cd1 58.5(5) . . ? C1 C9 Cd1 178.9(7) . . ? O4 C10 O3 122.7(10) . . ? O4 C10 C3 119.5(11) . . ? O3 C10 C3 117.7(10) . . ? O4 C10 Cd1 55.7(6) . 5_545 ? O3 C10 Cd1 68.9(6) . 5_545 ? C3 C10 Cd1 165.7(8) . 5_545 ? C19 C11 C15 114.6(10) . . ? C19 C11 C12 111.3(9) . . ? C15 C11 C12 102.0(8) . . ? C19 C11 C16 109.2(8) . . ? C15 C11 C16 107.5(9) . . ? C12 C11 C16 112.1(9) . . ? C18 C12 C11 110.7(9) . . ? C18 C12 C17 110.4(11) . . ? C11 C12 C17 112.3(10) . . ? C18 C12 C13 112.6(8) . . ? C11 C12 C13 102.3(8) . . ? C17 C12 C13 108.3(9) . . ? C20 C13 C14 114.0(8) . . ? C20 C13 C12 112.0(9) . . ? C14 C13 C12 105.4(8) . . ? C20 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? C12 C13 H13A 108.4 . . ? C15 C14 C13 105.7(8) . . ? C15 C14 H14A 110.6 . . ? C13 C14 H14A 110.6 . . ? C15 C14 H14B 110.6 . . ? C13 C14 H14B 110.6 . . ? H14A C14 H14B 108.7 . . ? C11 C15 C14 106.2(9) . . ? C11 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? C11 C15 H15B 110.5 . . ? C14 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 O6 118.5(10) . . ? O5 C19 C11 123.3(10) . . ? O6 C19 C11 118.1(10) . . ? O5 C19 Cd1 59.5(5) . . ? O6 C19 Cd1 59.1(5) . . ? C11 C19 Cd1 177.1(8) . . ? O7 C20 O8 117.7(9) . . ? O7 C20 C13 121.6(9) . . ? O8 C20 C13 120.6(10) . . ? O7 C20 Cd2 61.7(5) . 4_545 ? O8 C20 Cd2 56.1(5) . 4_545 ? C13 C20 Cd2 176.6(7) . 4_545 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.127 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.161 # Attachment '2.cif' data_664304 _database_code_depnum_ccdc_archive 'CCDC 664304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 Cd4 O18' _chemical_formula_weight 1278.52 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 _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 12.8807(3) _cell_length_b 13.3380(3) _cell_length_c 13.4542(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.9400(10) _cell_angle_gamma 90.00 _cell_volume 2233.33(9) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5202 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.11 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.952 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .897 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18408 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.12 _reflns_number_total 7021 _reflns_number_gt 6518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(18) _chemical_absolute_configuration rm _refine_ls_number_reflns 7021 _refine_ls_number_parameters 559 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _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 Cd1 Cd -0.33943(3) 0.84128(2) -0.32218(3) 0.02451(9) Uani 1 1 d . . . Cd2 Cd -0.14725(3) 1.25309(3) -0.81540(3) 0.03014(9) Uani 1 1 d . . . Cd3 Cd 0.11823(3) 1.19138(2) -0.70908(2) 0.02481(9) Uani 1 1 d . . . Cd4 Cd -0.53208(3) 0.73257(2) -0.24630(2) 0.02726(9) Uani 1 1 d . . . O1W O -0.3232(4) 0.7562(4) -0.1278(4) 0.0832(15) Uani 1 1 d . . . O1 O -0.5148(3) 0.8724(3) -0.1600(3) 0.0517(11) Uani 1 1 d . . . O2 O -0.4146(3) 0.9540(2) -0.2464(2) 0.0338(8) Uani 1 1 d . . . O2W O -0.1802(3) 1.3672(3) -0.7006(3) 0.0543(11) Uani 1 1 d . . . O3 O -0.2790(2) 1.2504(3) 0.0444(2) 0.0415(9) Uani 1 1 d . . . O4 O -0.3440(2) 1.1900(3) 0.1665(2) 0.0298(7) Uani 1 1 d . . . O5 O -0.6593(3) 0.8065(3) -0.3768(3) 0.0425(9) Uani 1 1 d . . . O6 O -0.5081(2) 0.7912(2) -0.4196(2) 0.0344(8) Uani 1 1 d . . . O7 O -0.5533(3) 1.1012(2) -0.7239(2) 0.0313(8) Uani 1 1 d . . . O8 O -0.6947(2) 1.1741(2) -0.6836(2) 0.0265(7) Uani 1 1 d . . . O9 O -0.0527(3) 1.1711(3) 0.0889(3) 0.0555(11) Uani 1 1 d . . . O10 O 0.1242(3) 1.1578(3) 0.1279(2) 0.0421(10) Uani 1 1 d . . . O11 O -0.1736(3) 0.8836(3) -0.2240(3) 0.0555(11) Uani 1 1 d . . . O12 O -0.0162(2) 0.8350(3) -0.2365(2) 0.0342(8) Uani 1 1 d . . . O13 O -0.2898(3) 0.8742(3) -0.4588(3) 0.0484(10) Uani 1 1 d . . . O14 O -0.1590(3) 0.7620(3) -0.4462(2) 0.0404(9) Uani 1 1 d . . . O15 O -0.0691(3) 1.1507(3) -0.6902(3) 0.0372(9) Uani 1 1 d . . . O16 O 0.0520(3) 1.0357(3) -0.6911(3) 0.0387(9) Uani 1 1 d . . . C1 C -0.5060(4) 1.0505(4) -0.1437(3) 0.0297(12) Uani 1 1 d . . . C2 C -0.4519(4) 1.0592(4) -0.0246(3) 0.0306(12) Uani 1 1 d . . . C3 C -0.4534(3) 1.1761(4) -0.0081(3) 0.0271(11) Uani 1 1 d . . . H3A H -0.5160 1.1923 0.0176 0.033 Uiso 1 1 calc R . . C4 C -0.4683(4) 1.2264(4) -0.1132(4) 0.0417(13) Uani 1 1 d . . . H4A H -0.5373 1.2600 -0.1336 0.050 Uiso 1 1 calc R . . H4B H -0.4120 1.2753 -0.1110 0.050 Uiso 1 1 calc R . . C5 C -0.4624(4) 1.1425(4) -0.1875(4) 0.0359(13) Uani 1 1 d . . . H5A H -0.3888 1.1316 -0.1906 0.043 Uiso 1 1 calc R . . H5B H -0.5060 1.1579 -0.2560 0.043 Uiso 1 1 calc R . . C6 C -0.6294(4) 1.0562(5) -0.1688(5) 0.0572(18) Uani 1 1 d . . . H6A H -0.6588 1.0506 -0.2418 0.086 Uiso 1 1 calc R . . H6B H -0.6504 1.1192 -0.1454 0.086 Uiso 1 1 calc R . . H6C H -0.6560 1.0024 -0.1348 0.086 Uiso 1 1 calc R . . C7 C -0.3381(5) 1.0188(4) -0.0011(4) 0.0564(19) Uani 1 1 d . . . H7A H -0.3053 1.0242 0.0714 0.085 Uiso 1 1 calc R . . H7B H -0.2972 1.0569 -0.0383 0.085 Uiso 1 1 calc R . . H7C H -0.3396 0.9497 -0.0214 0.085 Uiso 1 1 calc R . . C8 C -0.5150(6) 1.0067(5) 0.0421(4) 0.064(2) Uani 1 1 d . . . H8A H -0.4780 1.0147 0.1133 0.095 Uiso 1 1 calc R . . H8B H -0.5212 0.9366 0.0253 0.095 Uiso 1 1 calc R . . H8C H -0.5854 1.0357 0.0295 0.095 Uiso 1 1 calc R . . C9 C -0.3532(4) 1.2094(3) 0.0723(3) 0.0265(11) Uani 1 1 d . . . C10 C -0.4756(4) 0.9506(4) -0.1871(4) 0.0321(12) Uani 1 1 d . . . C11 C -0.6593(3) 0.8596(3) -0.5482(3) 0.0248(11) Uani 1 1 d . . . C12 C -0.6476(4) 0.9774(4) -0.5493(3) 0.0257(11) Uani 1 1 d . . . C13 C -0.6773(3) 0.9963(3) -0.6692(3) 0.0229(10) Uani 1 1 d . . . H13A H -0.7558 0.9954 -0.6940 0.027 Uiso 1 1 calc R . . C14 C -0.6337(4) 0.9052(4) -0.7154(4) 0.0334(12) Uani 1 1 d . . . H14A H -0.5709 0.9238 -0.7384 0.040 Uiso 1 1 calc R . . H14B H -0.6879 0.8793 -0.7738 0.040 Uiso 1 1 calc R . . C15 C -0.6041(4) 0.8257(4) -0.6297(3) 0.0340(12) Uani 1 1 d . . . H15A H -0.6296 0.7600 -0.6560 0.041 Uiso 1 1 calc R . . H15B H -0.5268 0.8227 -0.6015 0.041 Uiso 1 1 calc R . . C16 C -0.7780(4) 0.8256(4) -0.5780(4) 0.0406(13) Uani 1 1 d . . . H16A H -0.7812 0.7537 -0.5763 0.061 Uiso 1 1 calc R . . H16B H -0.8122 0.8488 -0.6461 0.061 Uiso 1 1 calc R . . H16C H -0.8142 0.8531 -0.5302 0.061 Uiso 1 1 calc R . . C17 C -0.7213(4) 1.0320(4) -0.4953(4) 0.0431(14) Uani 1 1 d . . . H17A H -0.7105 1.1030 -0.4986 0.065 Uiso 1 1 calc R . . H17B H -0.7052 1.0113 -0.4247 0.065 Uiso 1 1 calc R . . H17C H -0.7948 1.0161 -0.5286 0.065 Uiso 1 1 calc R . . C18 C -0.5327(4) 1.0120(4) -0.4994(4) 0.0359(13) Uani 1 1 d . . . H18A H -0.5293 1.0838 -0.5018 0.054 Uiso 1 1 calc R . . H18B H -0.4848 0.9837 -0.5359 0.054 Uiso 1 1 calc R . . H18C H -0.5120 0.9901 -0.4290 0.054 Uiso 1 1 calc R . . C19 C -0.6054(4) 0.8165(3) -0.4417(4) 0.0287(11) Uani 1 1 d . . . C20 C -0.6387(4) 1.0976(4) -0.6957(3) 0.0237(11) Uani 1 1 d . . . C21 C 0.0266(4) 1.1272(3) -0.0479(4) 0.0301(11) Uani 1 1 d . . . C22 C 0.0195(4) 1.0102(4) -0.0615(3) 0.0253(11) Uani 1 1 d . . . C23 C -0.0295(4) 1.0027(4) -0.1812(4) 0.0341(12) Uani 1 1 d . . . H23A H 0.0283 1.0153 -0.2148 0.041 Uiso 1 1 calc R . . C24 C -0.1090(6) 1.0891(5) -0.2075(5) 0.076(2) Uani 1 1 d . . . H24A H -0.1060 1.1197 -0.2721 0.091 Uiso 1 1 calc R . . H24B H -0.1816 1.0651 -0.2140 0.091 Uiso 1 1 calc R . . C25 C -0.0778(5) 1.1645(4) -0.1209(4) 0.0495(16) Uani 1 1 d . . . H25D H -0.1339 1.1697 -0.0849 0.059 Uiso 1 1 calc R . . H25E H -0.0671 1.2301 -0.1478 0.059 Uiso 1 1 calc R . . C26 C 0.1237(5) 1.1710(5) -0.0772(4) 0.0513(16) Uani 1 1 d . . . H26A H 0.1249 1.2424 -0.0678 0.077 Uiso 1 1 calc R . . H26B H 0.1192 1.1559 -0.1480 0.077 Uiso 1 1 calc R . . H26C H 0.1882 1.1424 -0.0344 0.077 Uiso 1 1 calc R . . C27 C 0.1284(4) 0.9573(4) -0.0267(4) 0.0458(15) Uani 1 1 d . . . H27A H 0.1553 0.9636 0.0465 0.069 Uiso 1 1 calc R . . H27B H 0.1782 0.9875 -0.0599 0.069 Uiso 1 1 calc R . . H27C H 0.1199 0.8876 -0.0448 0.069 Uiso 1 1 calc R . . C28 C -0.0545(4) 0.9624(4) -0.0029(4) 0.0404(14) Uani 1 1 d . . . H28A H -0.0227 0.9680 0.0697 0.061 Uiso 1 1 calc R . . H28B H -0.0649 0.8929 -0.0214 0.061 Uiso 1 1 calc R . . H28C H -0.1226 0.9962 -0.0202 0.061 Uiso 1 1 calc R . . C29 C 0.0325(4) 1.1552(4) 0.0649(4) 0.0325(12) Uani 1 1 d . . . C30 C -0.0773(4) 0.9008(4) -0.2157(3) 0.0270(11) Uani 1 1 d . . . C31 C -0.2073(4) 0.8643(3) -0.5973(3) 0.0272(11) Uani 1 1 d . . . C32 C -0.1600(4) 0.9746(4) -0.5908(4) 0.0281(11) Uani 1 1 d . . . C33 C -0.1248(4) 0.9796(4) -0.6927(3) 0.0278(11) Uani 1 1 d . . . H33A H -0.1887 0.9971 -0.7474 0.033 Uiso 1 1 calc R . . C34 C -0.0927(5) 0.8731(4) -0.7147(4) 0.0467(15) Uani 1 1 d . . . H34A H -0.1292 0.8536 -0.7845 0.056 Uiso 1 1 calc R . . H34B H -0.0158 0.8691 -0.7066 0.056 Uiso 1 1 calc R . . C35 C -0.1260(4) 0.8048(4) -0.6374(4) 0.0420(14) Uani 1 1 d . . . H35A H -0.1581 0.7435 -0.6704 0.050 Uiso 1 1 calc R . . H35B H -0.0643 0.7875 -0.5816 0.050 Uiso 1 1 calc R . . C36 C -0.3176(4) 0.8576(5) -0.6732(4) 0.0581(19) Uani 1 1 d . . . H36A H -0.3437 0.7900 -0.6751 0.087 Uiso 1 1 calc R . . H36B H -0.3121 0.8767 -0.7404 0.087 Uiso 1 1 calc R . . H36C H -0.3665 0.9018 -0.6517 0.087 Uiso 1 1 calc R . . C37 C -0.2385(5) 1.0580(5) -0.5837(5) 0.0630(19) Uani 1 1 d . . . H37A H -0.2030 1.1216 -0.5800 0.094 Uiso 1 1 calc R . . H37B H -0.2637 1.0486 -0.5231 0.094 Uiso 1 1 calc R . . H37C H -0.2984 1.0563 -0.6434 0.094 Uiso 1 1 calc R . . C38 C -0.0627(4) 0.9835(5) -0.4981(4) 0.0530(17) Uani 1 1 d . . . H38A H -0.0344 1.0504 -0.4946 0.080 Uiso 1 1 calc R . . H38B H -0.0084 0.9367 -0.5051 0.080 Uiso 1 1 calc R . . H38C H -0.0840 0.9691 -0.4363 0.080 Uiso 1 1 calc R . . C39 C -0.2188(4) 0.8311(4) -0.4913(3) 0.0286(11) Uani 1 1 d . . . C40 C -0.0418(4) 1.0593(4) -0.6920(3) 0.0294(12) 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 0.02200(17) 0.02337(19) 0.02966(19) -0.00208(16) 0.00940(14) 0.00039(14) Cd2 0.02699(19) 0.0318(2) 0.03129(18) -0.00222(17) 0.00691(15) 0.00142(16) Cd3 0.02296(17) 0.02385(19) 0.02711(18) -0.00014(15) 0.00552(14) -0.00298(14) Cd4 0.03299(19) 0.02296(19) 0.02920(18) 0.00169(15) 0.01412(15) 0.00251(15) O1W 0.076(3) 0.090(4) 0.075(3) -0.010(3) 0.005(2) 0.024(3) O1 0.087(3) 0.026(2) 0.049(2) -0.0141(18) 0.030(2) -0.016(2) O2 0.042(2) 0.032(2) 0.0318(19) -0.0080(16) 0.0167(16) 0.0103(16) O2W 0.057(3) 0.050(3) 0.064(3) -0.019(2) 0.031(2) -0.0055(19) O3 0.0320(19) 0.055(2) 0.0383(19) 0.0043(19) 0.0100(15) -0.0103(18) O4 0.0315(18) 0.0343(19) 0.0236(17) -0.0042(16) 0.0073(14) 0.0034(15) O5 0.038(2) 0.056(3) 0.034(2) 0.0159(18) 0.0094(17) 0.0093(17) O6 0.0227(18) 0.033(2) 0.042(2) 0.0023(16) -0.0022(15) 0.0051(14) O7 0.0315(19) 0.0222(19) 0.046(2) 0.0025(16) 0.0204(16) -0.0026(14) O8 0.0244(17) 0.0224(19) 0.0325(17) 0.0001(15) 0.0068(13) 0.0008(14) O9 0.049(2) 0.075(3) 0.050(2) -0.027(2) 0.0267(19) 0.003(2) O10 0.046(2) 0.050(3) 0.0284(19) -0.0081(18) 0.0058(17) -0.0062(18) O11 0.029(2) 0.077(3) 0.055(3) -0.025(2) 0.0007(18) -0.0060(19) O12 0.0346(19) 0.0232(18) 0.041(2) -0.0036(17) 0.0023(15) 0.0060(16) O13 0.047(2) 0.060(3) 0.047(2) 0.016(2) 0.0280(19) 0.015(2) O14 0.049(2) 0.041(2) 0.0304(18) 0.0102(18) 0.0092(16) -0.0005(19) O15 0.050(2) 0.024(2) 0.038(2) 0.0080(16) 0.0113(17) -0.0001(16) O16 0.0251(19) 0.036(2) 0.056(2) 0.0087(18) 0.0104(17) -0.0045(16) C1 0.029(3) 0.036(3) 0.024(3) -0.009(2) 0.006(2) -0.001(2) C2 0.039(3) 0.031(3) 0.022(2) -0.003(2) 0.008(2) 0.001(2) C3 0.023(2) 0.031(3) 0.026(2) -0.004(2) 0.0043(19) 0.003(2) C4 0.051(3) 0.035(3) 0.035(3) -0.001(3) 0.003(2) 0.002(3) C5 0.049(3) 0.028(3) 0.030(3) 0.003(2) 0.009(2) 0.007(2) C6 0.029(3) 0.074(5) 0.065(4) -0.028(4) 0.006(3) 0.002(3) C7 0.069(4) 0.034(3) 0.047(4) -0.017(3) -0.019(3) 0.021(3) C8 0.120(6) 0.045(4) 0.036(3) -0.007(3) 0.039(4) -0.025(4) C9 0.027(3) 0.024(3) 0.027(2) -0.002(2) 0.004(2) 0.006(2) C10 0.035(3) 0.030(3) 0.027(3) -0.007(2) 0.000(2) -0.001(2) C11 0.020(2) 0.024(3) 0.029(2) 0.001(2) 0.0049(19) 0.0015(19) C12 0.028(3) 0.024(3) 0.023(2) 0.003(2) 0.0035(19) 0.004(2) C13 0.021(2) 0.024(3) 0.022(2) 0.002(2) 0.0039(19) -0.001(2) C14 0.044(3) 0.024(3) 0.033(3) -0.004(2) 0.012(2) -0.004(2) C15 0.041(3) 0.025(3) 0.036(3) -0.002(2) 0.010(2) 0.002(2) C16 0.035(3) 0.040(3) 0.045(3) 0.006(3) 0.005(2) -0.007(2) C17 0.058(4) 0.042(3) 0.030(3) 0.002(3) 0.013(3) 0.014(3) C18 0.040(3) 0.026(3) 0.036(3) 0.004(2) 0.001(2) -0.008(2) C19 0.033(3) 0.020(3) 0.032(3) 0.001(2) 0.006(2) -0.005(2) C20 0.026(3) 0.025(3) 0.017(2) -0.002(2) -0.0009(19) -0.004(2) C21 0.040(3) 0.022(3) 0.030(3) -0.005(2) 0.012(2) -0.002(2) C22 0.029(3) 0.023(3) 0.024(2) -0.003(2) 0.005(2) 0.002(2) C23 0.045(3) 0.024(3) 0.031(3) -0.005(2) 0.005(2) 0.001(2) C24 0.117(6) 0.037(4) 0.049(4) -0.008(3) -0.023(4) 0.031(4) C25 0.067(4) 0.035(3) 0.037(3) -0.007(3) -0.006(3) 0.018(3) C26 0.074(4) 0.041(4) 0.046(3) -0.015(3) 0.028(3) -0.021(3) C27 0.039(3) 0.041(3) 0.050(4) -0.010(3) -0.001(3) 0.009(3) C28 0.051(3) 0.036(3) 0.036(3) -0.002(3) 0.013(3) -0.011(3) C29 0.046(3) 0.022(3) 0.029(3) -0.003(2) 0.009(3) -0.003(2) C30 0.022(3) 0.031(3) 0.026(3) -0.001(2) 0.003(2) 0.002(2) C31 0.035(3) 0.026(3) 0.023(2) 0.002(2) 0.011(2) -0.007(2) C32 0.032(3) 0.025(3) 0.030(3) 0.002(2) 0.013(2) -0.001(2) C33 0.027(3) 0.032(3) 0.025(3) 0.003(2) 0.008(2) -0.007(2) C34 0.070(4) 0.034(3) 0.047(3) -0.011(3) 0.037(3) -0.016(3) C35 0.065(4) 0.028(3) 0.041(3) 0.002(3) 0.028(3) 0.000(3) C36 0.045(3) 0.092(5) 0.032(3) 0.011(3) 0.000(2) -0.031(3) C37 0.087(5) 0.039(4) 0.085(5) 0.012(3) 0.061(4) 0.012(3) C38 0.062(4) 0.068(4) 0.026(3) -0.006(3) 0.006(3) -0.039(3) C39 0.027(3) 0.030(3) 0.028(3) 0.003(2) 0.006(2) -0.009(2) C40 0.035(3) 0.036(3) 0.016(2) 0.006(2) 0.004(2) -0.009(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 Cd1 O13 2.141(3) . ? Cd1 O2 2.179(3) . ? Cd1 O8 2.270(3) 2_444 ? Cd1 O11 2.274(3) . ? Cd1 O6 2.328(3) . ? Cd1 O1W 2.809(5) . ? Cd1 Cd4 3.2571(5) . ? Cd1 Cd3 3.4168(5) 2_544 ? Cd2 O3 2.188(3) 1_554 ? Cd2 O15 2.200(3) . ? Cd2 O9 2.268(4) 1_554 ? Cd2 O2W 2.285(4) . ? Cd2 O12 2.314(3) 2_554 ? Cd2 O4 2.621(3) 1_554 ? Cd2 C9 2.756(4) 1_554 ? Cd2 Cd3 3.4488(5) . ? Cd3 O14 2.228(3) 2_554 ? Cd3 O10 2.260(3) 1_554 ? Cd3 O16 2.282(3) . ? Cd3 O12 2.331(3) 2_554 ? Cd3 O8 2.356(3) 1_655 ? Cd3 O15 2.549(4) . ? Cd3 C40 2.766(5) . ? Cd3 O11 2.868(4) 2_554 ? Cd3 Cd1 3.4168(5) 2_554 ? Cd4 O7 2.161(3) 2_444 ? Cd4 O1 2.178(3) . ? Cd4 O4 2.216(3) 2_445 ? Cd4 O5 2.293(3) . ? Cd4 O6 2.552(3) . ? Cd4 O1W 2.769(4) . ? Cd4 C19 2.789(5) . ? O1 C10 1.253(6) . ? O2 C10 1.256(6) . ? O3 C9 1.241(5) . ? O3 Cd2 2.188(3) 1_556 ? O4 C9 1.267(5) . ? O4 Cd4 2.216(3) 2_455 ? O4 Cd2 2.621(3) 1_556 ? O5 C19 1.254(6) . ? O6 C19 1.258(5) . ? O7 C20 1.253(5) . ? O7 Cd4 2.161(3) 2_454 ? O8 C20 1.284(6) . ? O8 Cd1 2.270(3) 2_454 ? O8 Cd3 2.356(3) 1_455 ? O9 C29 1.240(6) . ? O9 Cd2 2.268(4) 1_556 ? O10 C29 1.264(6) . ? O10 Cd3 2.260(3) 1_556 ? O11 C30 1.238(5) . ? O11 Cd3 2.868(4) 2_544 ? O12 C30 1.258(6) . ? O12 Cd2 2.314(3) 2_544 ? O12 Cd3 2.331(3) 2_544 ? O13 C39 1.251(6) . ? O14 C39 1.253(6) . ? O14 Cd3 2.228(3) 2_544 ? O15 C40 1.271(6) . ? O16 C40 1.246(6) . ? C1 C5 1.530(7) . ? C1 C6 1.540(7) . ? C1 C10 1.545(7) . ? C1 C2 1.578(6) . ? C2 C7 1.517(7) . ? C2 C8 1.527(7) . ? C2 C3 1.575(7) . ? C3 C9 1.521(6) . ? C3 C4 1.532(6) . ? C3 H3A 0.9800 . ? C4 C5 1.516(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 Cd2 2.756(4) 1_556 ? C11 C15 1.522(6) . ? C11 C19 1.533(6) . ? C11 C16 1.545(6) . ? C11 C12 1.579(6) . ? C12 C17 1.522(7) . ? C12 C18 1.530(6) . ? C12 C13 1.579(6) . ? C13 C20 1.513(6) . ? C13 C14 1.536(7) . ? C13 H13A 0.9800 . ? C14 C15 1.540(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C26 1.522(7) . ? C21 C25 1.529(7) . ? C21 C29 1.546(6) . ? C21 C22 1.572(6) . ? C22 C28 1.524(7) . ? C22 C27 1.531(7) . ? C22 C23 1.575(6) . ? C23 C30 1.514(7) . ? C23 C24 1.521(7) . ? C23 H23A 0.9800 . ? C24 C25 1.514(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25D 0.9700 . ? C25 H25E 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C31 C35 1.519(7) . ? C31 C36 1.523(6) . ? C31 C39 1.536(6) . ? C31 C32 1.586(6) . ? C32 C37 1.523(7) . ? C32 C38 1.528(7) . ? C32 C33 1.553(6) . ? C33 C40 1.506(7) . ? C33 C34 1.529(7) . ? C33 H33A 0.9800 . ? C34 C35 1.526(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? 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 O13 Cd1 O2 121.81(13) . . ? O13 Cd1 O8 97.64(13) . 2_444 ? O2 Cd1 O8 140.10(12) . 2_444 ? O13 Cd1 O11 90.23(15) . . ? O2 Cd1 O11 91.21(14) . . ? O8 Cd1 O11 94.55(14) 2_444 . ? O13 Cd1 O6 90.99(13) . . ? O2 Cd1 O6 89.92(12) . . ? O8 Cd1 O6 83.22(11) 2_444 . ? O11 Cd1 O6 177.58(15) . . ? O13 Cd1 O1W 156.22(13) . . ? O2 Cd1 O1W 77.19(13) . . ? O8 Cd1 O1W 66.67(13) 2_444 . ? O11 Cd1 O1W 74.13(15) . . ? O6 Cd1 O1W 104.06(13) . . ? O13 Cd1 Cd4 141.30(11) . . ? O2 Cd1 Cd4 72.18(9) . . ? O8 Cd1 Cd4 73.05(8) 2_444 . ? O11 Cd1 Cd4 127.30(11) . . ? O6 Cd1 Cd4 51.15(9) . . ? O1W Cd1 Cd4 53.70(10) . . ? O13 Cd1 Cd3 78.56(10) . 2_544 ? O2 Cd1 Cd3 143.45(9) . 2_544 ? O8 Cd1 Cd3 43.37(7) 2_444 2_544 ? O11 Cd1 Cd3 56.31(11) . 2_544 ? O6 Cd1 Cd3 121.94(8) . 2_544 ? O1W Cd1 Cd3 77.85(9) . 2_544 ? Cd4 Cd1 Cd3 112.301(12) . 2_544 ? O3 Cd2 O15 138.57(14) 1_554 . ? O3 Cd2 O9 85.03(13) 1_554 1_554 ? O15 Cd2 O9 85.91(15) . 1_554 ? O3 Cd2 O2W 110.84(14) 1_554 . ? O15 Cd2 O2W 91.38(14) . . ? O9 Cd2 O2W 157.71(14) 1_554 . ? O3 Cd2 O12 135.31(12) 1_554 2_554 ? O15 Cd2 O12 82.01(12) . 2_554 ? O9 Cd2 O12 79.56(13) 1_554 2_554 ? O2W Cd2 O12 78.15(13) . 2_554 ? O3 Cd2 O4 53.00(11) 1_554 1_554 ? O15 Cd2 O4 96.47(11) . 1_554 ? O9 Cd2 O4 116.11(12) 1_554 1_554 ? O2W Cd2 O4 86.18(12) . 1_554 ? O12 Cd2 O4 164.19(11) 2_554 1_554 ? O3 Cd2 C9 25.97(12) 1_554 1_554 ? O15 Cd2 C9 118.31(13) . 1_554 ? O9 Cd2 C9 99.73(13) 1_554 1_554 ? O2W Cd2 C9 101.02(13) . 1_554 ? O12 Cd2 C9 159.66(13) 2_554 1_554 ? O4 Cd2 C9 27.12(11) 1_554 1_554 ? O3 Cd2 Cd3 145.01(9) 1_554 . ? O15 Cd2 Cd3 47.57(9) . . ? O9 Cd2 Cd3 60.03(10) 1_554 . ? O2W Cd2 Cd3 102.45(10) . . ? O12 Cd2 Cd3 42.25(8) 2_554 . ? O4 Cd2 Cd3 142.51(7) 1_554 . ? C9 Cd2 Cd3 152.68(9) 1_554 . ? O14 Cd3 O10 159.31(13) 2_554 1_554 ? O14 Cd3 O16 106.85(13) 2_554 . ? O10 Cd3 O16 91.68(13) 1_554 . ? O14 Cd3 O12 85.68(12) 2_554 2_554 ? O10 Cd3 O12 90.90(13) 1_554 2_554 ? O16 Cd3 O12 125.82(11) . 2_554 ? O14 Cd3 O8 85.42(11) 2_554 1_655 ? O10 Cd3 O8 80.33(11) 1_554 1_655 ? O16 Cd3 O8 106.95(12) . 1_655 ? O12 Cd3 O8 126.78(11) 2_554 1_655 ? O14 Cd3 O15 89.84(12) 2_554 . ? O10 Cd3 O15 108.93(12) 1_554 . ? O16 Cd3 O15 53.59(11) . . ? O12 Cd3 O15 74.61(11) 2_554 . ? O8 Cd3 O15 157.47(11) 1_655 . ? O14 Cd3 C40 101.08(13) 2_554 . ? O10 Cd3 C40 99.60(13) 1_554 . ? O16 Cd3 C40 26.42(14) . . ? O12 Cd3 C40 100.22(14) 2_554 . ? O8 Cd3 C40 132.98(14) 1_655 . ? O15 Cd3 C40 27.28(13) . . ? O14 Cd3 O11 84.18(13) 2_554 2_554 ? O10 Cd3 O11 78.42(13) 1_554 2_554 ? O16 Cd3 O11 167.73(11) . 2_554 ? O12 Cd3 O11 48.14(11) 2_554 2_554 ? O8 Cd3 O11 78.78(11) 1_655 2_554 ? O15 Cd3 O11 122.68(11) . 2_554 ? C40 Cd3 O11 147.83(13) . 2_554 ? O14 Cd3 Cd1 69.48(9) 2_554 2_554 ? O10 Cd3 Cd1 89.97(9) 1_554 2_554 ? O16 Cd3 Cd1 147.37(9) . 2_554 ? O12 Cd3 Cd1 86.72(8) 2_554 2_554 ? O8 Cd3 Cd1 41.43(8) 1_655 2_554 ? O15 Cd3 Cd1 153.27(8) . 2_554 ? C40 Cd3 Cd1 168.02(9) . 2_554 ? O11 Cd3 Cd1 41.28(7) 2_554 2_554 ? O14 Cd3 Cd2 104.89(9) 2_554 . ? O10 Cd3 Cd2 85.59(9) 1_554 . ? O16 Cd3 Cd2 84.46(8) . . ? O12 Cd3 Cd2 41.86(8) 2_554 . ? O8 Cd3 Cd2 162.02(8) 1_655 . ? O15 Cd3 Cd2 39.57(7) . . ? C40 Cd3 Cd2 60.39(11) . . ? O11 Cd3 Cd2 87.52(7) 2_554 . ? Cd1 Cd3 Cd2 128.141(13) 2_554 . ? O7 Cd4 O1 143.77(14) 2_444 . ? O7 Cd4 O4 110.31(12) 2_444 2_445 ? O1 Cd4 O4 87.04(14) . 2_445 ? O7 Cd4 O5 120.28(13) 2_444 . ? O1 Cd4 O5 89.68(15) . . ? O4 Cd4 O5 91.12(12) 2_445 . ? O7 Cd4 O6 83.79(11) 2_444 . ? O1 Cd4 O6 101.81(13) . . ? O4 Cd4 O6 142.49(10) 2_445 . ? O5 Cd4 O6 53.08(11) . . ? O7 Cd4 O1W 74.55(13) 2_444 . ? O1 Cd4 O1W 69.22(15) . . ? O4 Cd4 O1W 117.67(13) 2_445 . ? O5 Cd4 O1W 142.05(15) . . ? O6 Cd4 O1W 99.38(13) . . ? O7 Cd4 C19 102.45(13) 2_444 . ? O1 Cd4 C19 97.00(14) . . ? O4 Cd4 C19 116.64(12) 2_445 . ? O5 Cd4 C19 26.33(12) . . ? O6 Cd4 C19 26.77(12) . . ? O1W Cd4 C19 122.69(15) . . ? O7 Cd4 Cd1 80.65(8) 2_444 . ? O1 Cd4 Cd1 78.72(11) . . ? O4 Cd4 Cd1 165.57(9) 2_445 . ? O5 Cd4 Cd1 91.16(9) . . ? O6 Cd4 Cd1 45.25(7) . . ? O1W Cd4 Cd1 54.85(11) . . ? C19 Cd4 Cd1 68.05(10) . . ? Cd4 O1W Cd1 71.44(11) . . ? C10 O1 Cd4 123.5(3) . . ? C10 O2 Cd1 134.3(3) . . ? C9 O3 Cd2 103.5(3) . 1_556 ? C9 O4 Cd4 122.5(3) . 2_455 ? C9 O4 Cd2 82.4(3) . 1_556 ? Cd4 O4 Cd2 132.29(13) 2_455 1_556 ? C19 O5 Cd4 99.5(3) . . ? C19 O6 Cd1 141.7(3) . . ? C19 O6 Cd4 87.2(3) . . ? Cd1 O6 Cd4 83.60(10) . . ? C20 O7 Cd4 128.0(3) . 2_454 ? C20 O8 Cd1 132.4(3) . 2_454 ? C20 O8 Cd3 130.3(3) . 1_455 ? Cd1 O8 Cd3 95.20(11) 2_454 1_455 ? C29 O9 Cd2 150.6(3) . 1_556 ? C29 O10 Cd3 113.3(3) . 1_556 ? C30 O11 Cd1 150.2(3) . . ? C30 O11 Cd3 82.5(3) . 2_544 ? Cd1 O11 Cd3 82.42(12) . 2_544 ? C30 O12 Cd2 146.6(3) . 2_544 ? C30 O12 Cd3 108.0(3) . 2_544 ? Cd2 O12 Cd3 95.88(12) 2_544 2_544 ? C39 O13 Cd1 127.8(3) . . ? C39 O14 Cd3 137.1(3) . 2_544 ? C40 O15 Cd2 130.9(3) . . ? C40 O15 Cd3 85.9(3) . . ? Cd2 O15 Cd3 92.86(12) . . ? C40 O16 Cd3 99.0(3) . . ? C5 C1 C6 109.7(4) . . ? C5 C1 C10 113.1(4) . . ? C6 C1 C10 107.9(4) . . ? C5 C1 C2 102.8(4) . . ? C6 C1 C2 112.3(4) . . ? C10 C1 C2 111.0(4) . . ? C7 C2 C8 110.3(5) . . ? C7 C2 C3 111.6(4) . . ? C8 C2 C3 110.1(4) . . ? C7 C2 C1 109.6(4) . . ? C8 C2 C1 113.6(4) . . ? C3 C2 C1 101.4(4) . . ? C9 C3 C4 114.2(4) . . ? C9 C3 C2 110.5(4) . . ? C4 C3 C2 107.8(4) . . ? C9 C3 H3A 108.0 . . ? C4 C3 H3A 108.0 . . ? C2 C3 H3A 108.0 . . ? C5 C4 C3 105.6(4) . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? C4 C5 C1 104.6(4) . . ? C4 C5 H5A 110.8 . . ? C1 C5 H5A 110.8 . . ? C4 C5 H5B 110.8 . . ? C1 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O4 120.7(4) . . ? O3 C9 C3 119.5(4) . . ? O4 C9 C3 119.7(4) . . ? O3 C9 Cd2 50.5(2) . 1_556 ? O4 C9 Cd2 70.5(2) . 1_556 ? C3 C9 Cd2 166.4(3) . 1_556 ? O1 C10 O2 125.4(5) . . ? O1 C10 C1 116.6(5) . . ? O2 C10 C1 118.0(5) . . ? C15 C11 C19 112.3(4) . . ? C15 C11 C16 109.9(4) . . ? C19 C11 C16 108.2(4) . . ? C15 C11 C12 103.0(4) . . ? C19 C11 C12 111.2(4) . . ? C16 C11 C12 112.3(4) . . ? C17 C12 C18 107.3(4) . . ? C17 C12 C13 113.2(4) . . ? C18 C12 C13 110.7(4) . . ? C17 C12 C11 113.5(4) . . ? C18 C12 C11 112.3(4) . . ? C13 C12 C11 99.8(4) . . ? C20 C13 C14 115.7(4) . . ? C20 C13 C12 112.1(4) . . ? C14 C13 C12 105.6(4) . . ? C20 C13 H13A 107.7 . . ? C14 C13 H13A 107.7 . . ? C12 C13 H13A 107.7 . . ? C13 C14 C15 106.7(4) . . ? C13 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? C13 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C11 C15 C14 105.3(4) . . ? C11 C15 H15A 110.7 . . ? C14 C15 H15A 110.7 . . ? C11 C15 H15B 110.7 . . ? C14 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 O6 120.2(4) . . ? O5 C19 C11 119.5(4) . . ? O6 C19 C11 120.3(4) . . ? O5 C19 Cd4 54.2(2) . . ? O6 C19 Cd4 66.1(3) . . ? C11 C19 Cd4 173.2(3) . . ? O7 C20 O8 125.0(4) . . ? O7 C20 C13 118.2(4) . . ? O8 C20 C13 116.7(4) . . ? C26 C21 C25 110.7(5) . . ? C26 C21 C29 109.0(4) . . ? C25 C21 C29 111.4(4) . . ? C26 C21 C22 112.2(4) . . ? C25 C21 C22 103.5(4) . . ? C29 C21 C22 109.9(4) . . ? C28 C22 C27 107.2(4) . . ? C28 C22 C21 112.3(4) . . ? C27 C22 C21 113.6(4) . . ? C28 C22 C23 111.3(4) . . ? C27 C22 C23 112.2(4) . . ? C21 C22 C23 100.2(4) . . ? C30 C23 C24 114.4(4) . . ? C30 C23 C22 113.2(4) . . ? C24 C23 C22 105.0(4) . . ? C30 C23 H23A 108.0 . . ? C24 C23 H23A 108.0 . . ? C22 C23 H23A 108.0 . . ? C25 C24 C23 107.2(4) . . ? C25 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? C25 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C24 C25 C21 107.0(4) . . ? C24 C25 H25D 110.3 . . ? C21 C25 H25D 110.3 . . ? C24 C25 H25E 110.3 . . ? C21 C25 H25E 110.3 . . ? H25D C25 H25E 108.6 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 C29 O10 123.9(5) . . ? O9 C29 C21 118.3(4) . . ? O10 C29 C21 117.7(5) . . ? O11 C30 O12 121.3(5) . . ? O11 C30 C23 120.9(5) . . ? O12 C30 C23 117.8(4) . . ? C35 C31 C36 109.9(4) . . ? C35 C31 C39 114.8(4) . . ? C36 C31 C39 108.0(4) . . ? C35 C31 C32 102.4(4) . . ? C36 C31 C32 111.7(4) . . ? C39 C31 C32 110.1(4) . . ? C37 C32 C38 108.1(5) . . ? C37 C32 C33 112.0(4) . . ? C38 C32 C33 110.6(4) . . ? C37 C32 C31 115.4(4) . . ? C38 C32 C31 109.9(4) . . ? C33 C32 C31 100.7(4) . . ? C40 C33 C34 115.5(4) . . ? C40 C33 C32 113.1(4) . . ? C34 C33 C32 106.6(4) . . ? C40 C33 H33A 107.0 . . ? C34 C33 H33A 107.0 . . ? C32 C33 H33A 107.0 . . ? C35 C34 C33 106.5(4) . . ? C35 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? C35 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C31 C35 C34 105.7(4) . . ? C31 C35 H35A 110.6 . . ? C34 C35 H35A 110.6 . . ? C31 C35 H35B 110.6 . . ? C34 C35 H35B 110.6 . . ? H35A C35 H35B 108.7 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O13 C39 O14 125.5(4) . . ? O13 C39 C31 116.5(4) . . ? O14 C39 C31 117.9(4) . . ? O16 C40 O15 121.0(4) . . ? O16 C40 C33 120.4(5) . . ? O15 C40 C33 118.6(5) . . ? O16 C40 Cd3 54.6(2) . . ? O15 C40 Cd3 66.8(3) . . ? C33 C40 Cd3 172.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.484 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.073 # Attachment '3.cif' data_664305 _database_code_depnum_ccdc_archive 'CCDC 664305' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H28 Cd2 O8' _chemical_formula_weight 621.22 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 Monoclinic _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 7.2911(4) _cell_length_b 11.3103(7) _cell_length_c 13.0172(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.332(4) _cell_angle_gamma 90.00 _cell_volume 1059.25(11) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1925 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.70 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .30 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.050 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11562 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.1167 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.22 _reflns_number_total 4314 _reflns_number_gt 2524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.4991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(9) _chemical_absolute_configuration rm _refine_ls_number_reflns 4314 _refine_ls_number_parameters 271 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 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 1.25275(15) -0.20864(8) 0.76095(8) 0.0480(4) Uani 1 1 d . . . Cd2 Cd 1.74793(15) -0.29130(5) 0.73212(8) 0.0475(4) Uani 1 1 d . . . O1 O 1.6460(19) -0.2376(17) 0.8723(10) 0.123(7) Uani 1 1 d . . . O2 O 1.395(2) -0.1709(17) 0.9116(10) 0.109(6) Uani 1 1 d . . . O3 O 2.1609(18) 0.0215(12) 1.2205(11) 0.076(4) Uani 1 1 d . . . O4 O 1.9388(17) 0.1464(13) 1.2178(11) 0.073(4) Uani 1 1 d . . . O5 O 0.5731(11) 0.2160(13) 0.3451(6) 0.057(3) Uani 1 1 d . . . O6 O 0.3678(15) 0.1805(13) 0.4418(7) 0.068(4) Uani 1 1 d . . . O7 O 1.148(2) -0.0464(16) 0.6855(12) 0.103(5) Uani 1 1 d . . . O8 O 0.901(2) -0.1201(13) 0.7199(10) 0.086(5) Uani 1 1 d . . . C1 C 1.655(3) -0.1768(18) 1.0505(13) 0.068(6) Uani 1 1 d . . . C2 C 1.8294(17) -0.0940(11) 1.0540(10) 0.045(3) Uani 1 1 d . . . C3 C 1.855(2) -0.0590(17) 1.1696(12) 0.059(5) Uani 1 1 d . . . H3A H 1.9102 -0.1288 1.2071 0.071 Uiso 1 1 calc R . . C4 C 1.661(3) -0.050(3) 1.1979(13) 0.134(10) Uani 1 1 d . . . H4B H 1.6576 -0.0864 1.2652 0.161 Uiso 1 1 calc R . . H4C H 1.6231 0.0317 1.2006 0.161 Uiso 1 1 calc R . . C5 C 1.533(2) -0.116(2) 1.1128(12) 0.108(8) Uani 1 1 d . . . H5A H 1.4570 -0.1728 1.1430 0.130 Uiso 1 1 calc R . . H5B H 1.4515 -0.0612 1.0700 0.130 Uiso 1 1 calc R . . C6 C 1.702(4) -0.304(2) 1.0882(17) 0.158(13) Uani 1 1 d . . . H6A H 1.7716 -0.3014 1.1576 0.236 Uiso 1 1 calc R . . H6B H 1.7759 -0.3411 1.0426 0.236 Uiso 1 1 calc R . . H6C H 1.5899 -0.3477 1.0881 0.236 Uiso 1 1 calc R . . C7 C 2.002(2) -0.141(2) 1.0229(19) 0.146(11) Uani 1 1 d . . . H7A H 2.0402 -0.2109 1.0629 0.219 Uiso 1 1 calc R . . H7B H 2.0981 -0.0827 1.0354 0.219 Uiso 1 1 calc R . . H7C H 1.9789 -0.1610 0.9502 0.219 Uiso 1 1 calc R . . C8 C 1.776(4) 0.020(2) 0.9886(15) 0.110(9) Uani 1 1 d . . . H8A H 1.7600 0.0014 0.9158 0.165 Uiso 1 1 calc R . . H8B H 1.8731 0.0780 1.0046 0.165 Uiso 1 1 calc R . . H8C H 1.6621 0.0519 1.0051 0.165 Uiso 1 1 calc R . . C9 C 1.553(3) -0.198(2) 0.9329(12) 0.058(5) Uani 1 1 d . . . C10 C 1.988(3) 0.041(2) 1.2053(14) 0.056(5) Uani 1 1 d . . . C11 C 0.6789(19) 0.1903(15) 0.5321(9) 0.035(3) Uani 1 1 d . . . C12 C 0.722(3) 0.0663(13) 0.5724(13) 0.081(6) Uani 1 1 d . . . C13 C 0.890(2) 0.0785(16) 0.6537(13) 0.059(5) Uani 1 1 d . . . H13A H 0.8526 0.1164 0.7146 0.071 Uiso 1 1 calc R . . C14 C 1.020(2) 0.1682(16) 0.6053(16) 0.097(6) Uani 1 1 d . . . H14A H 1.0677 0.2291 0.6551 0.116 Uiso 1 1 calc R . . H14B H 1.1243 0.1275 0.5831 0.116 Uiso 1 1 calc R . . C15 C 0.890(3) 0.221(2) 0.5112(15) 0.124(8) Uani 1 1 d . . . H15A H 0.9130 0.1859 0.4467 0.149 Uiso 1 1 calc R . . H15B H 0.9074 0.3062 0.5076 0.149 Uiso 1 1 calc R . . C16 C 0.626(3) 0.271(3) 0.6148(15) 0.138(14) Uani 1 1 d . . . H16A H 0.4980 0.2578 0.6214 0.207 Uiso 1 1 calc R . . H16B H 0.6414 0.3520 0.5954 0.207 Uiso 1 1 calc R . . H16C H 0.7035 0.2552 0.6801 0.207 Uiso 1 1 calc R . . C17 C 0.564(3) 0.027(2) 0.6400(15) 0.128(9) Uani 1 1 d . . . H17A H 0.5899 -0.0521 0.6662 0.193 Uiso 1 1 calc R . . H17B H 0.4442 0.0281 0.5967 0.193 Uiso 1 1 calc R . . H17C H 0.5644 0.0801 0.6973 0.193 Uiso 1 1 calc R . . C18 C 0.731(4) -0.0155(19) 0.4910(14) 0.109(9) Uani 1 1 d . . . H18A H 0.8233 0.0101 0.4509 0.164 Uiso 1 1 calc R . . H18B H 0.6125 -0.0201 0.4470 0.164 Uiso 1 1 calc R . . H18C H 0.7647 -0.0920 0.5202 0.164 Uiso 1 1 calc R . . C19 C 0.539(2) 0.197(2) 0.4377(11) 0.049(4) Uani 1 1 d . . . C20 C 0.983(3) -0.039(2) 0.6890(12) 0.052(5) 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 0.0359(7) 0.0548(10) 0.0538(7) -0.0007(7) 0.0090(5) 0.0019(7) Cd2 0.0350(7) 0.0534(10) 0.0540(6) 0.0010(8) 0.0072(5) 0.0037(8) O1 0.116(11) 0.166(18) 0.093(9) -0.080(10) 0.035(8) -0.031(11) O2 0.071(9) 0.157(16) 0.096(10) -0.033(9) 0.003(7) 0.025(9) O3 0.048(7) 0.059(7) 0.117(10) -0.018(6) -0.003(6) 0.005(6) O4 0.043(6) 0.059(8) 0.117(10) -0.028(7) 0.009(6) -0.002(6) O5 0.042(5) 0.084(7) 0.047(5) 0.001(6) 0.005(4) -0.013(6) O6 0.046(6) 0.109(11) 0.048(5) 0.025(6) 0.006(4) 0.018(6) O7 0.074(10) 0.109(11) 0.133(12) 0.040(10) 0.035(8) 0.038(9) O8 0.119(12) 0.047(8) 0.089(9) 0.021(6) 0.006(8) -0.008(8) C1 0.059(10) 0.081(16) 0.067(10) -0.004(9) 0.017(8) -0.031(10) C2 0.048(7) 0.039(8) 0.054(7) -0.015(6) 0.031(6) 0.002(6) C3 0.075(11) 0.051(10) 0.048(9) 0.013(8) 0.002(8) -0.014(9) C4 0.130(17) 0.23(3) 0.053(10) -0.069(14) 0.058(10) -0.117(18) C5 0.081(11) 0.18(2) 0.072(11) -0.062(12) 0.042(8) -0.078(14) C6 0.23(3) 0.048(11) 0.141(19) 0.036(13) -0.120(19) -0.046(18) C7 0.052(10) 0.19(2) 0.20(2) -0.14(2) 0.033(13) -0.002(13) C8 0.17(2) 0.095(17) 0.055(11) 0.033(11) -0.014(12) -0.070(15) C9 0.056(11) 0.063(14) 0.056(10) -0.010(12) 0.014(8) -0.010(12) C10 0.066(14) 0.049(12) 0.054(10) -0.007(8) 0.012(9) -0.014(11) C11 0.042(7) 0.037(8) 0.026(6) 0.004(6) 0.001(5) 0.000(7) C12 0.103(14) 0.040(9) 0.082(11) 0.007(8) -0.038(10) -0.002(9) C13 0.069(11) 0.044(10) 0.059(10) 0.008(7) -0.008(8) 0.003(8) C14 0.051(10) 0.080(13) 0.158(18) 0.030(12) 0.009(11) 0.001(9) C15 0.117(15) 0.109(17) 0.128(16) 0.039(14) -0.037(12) -0.038(15) C16 0.138(19) 0.18(3) 0.082(12) -0.040(15) -0.016(12) 0.10(2) C17 0.14(2) 0.15(2) 0.108(17) 0.036(16) 0.055(15) -0.053(18) C18 0.20(3) 0.046(12) 0.061(12) -0.008(9) -0.032(13) 0.039(14) C19 0.069(12) 0.034(10) 0.046(8) -0.007(9) 0.018(7) -0.006(11) C20 0.068(13) 0.054(13) 0.035(8) -0.001(8) 0.006(8) 0.006(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 O2 2.109(13) . ? Cd1 O7 2.161(16) . ? Cd1 O5 2.194(10) 2_746 ? Cd1 O4 2.200(14) 2_847 ? Cd2 O1 2.166(12) . ? Cd2 O8 2.255(16) 1_655 ? Cd2 O3 2.274(14) 2_947 ? Cd2 O6 2.307(9) 2_746 ? Cd2 O4 2.378(13) 2_947 ? Cd2 O5 2.394(8) 2_746 ? Cd2 C10 2.73(2) 2_947 ? O1 C9 1.21(2) . ? O2 C9 1.18(2) . ? O3 C10 1.26(2) . ? O3 Cd2 2.274(14) 2_957 ? O4 C10 1.27(2) . ? O4 Cd1 2.200(14) 2_857 ? O4 Cd2 2.378(13) 2_957 ? O5 C19 1.288(15) . ? O5 Cd1 2.194(10) 2_756 ? O5 Cd2 2.394(8) 2_756 ? O6 C19 1.272(17) . ? O6 Cd2 2.307(9) 2_756 ? O7 C20 1.21(2) . ? O8 C20 1.20(2) . ? O8 Cd2 2.255(16) 1_455 ? C1 C5 1.47(2) . ? C1 C6 1.54(3) . ? C1 C2 1.58(2) . ? C1 C9 1.61(2) . ? C2 C7 1.482(19) . ? C2 C3 1.538(19) . ? C2 C8 1.56(3) . ? C3 C10 1.51(3) . ? C3 C4 1.52(2) . ? C3 H3A 0.9800 . ? C4 C5 1.52(2) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 Cd2 2.73(2) 2_957 ? C11 C19 1.466(18) . ? C11 C16 1.51(2) . ? C11 C12 1.51(2) . ? C11 C15 1.64(2) . ? C12 C18 1.42(2) . ? C12 C13 1.49(2) . ? C12 C17 1.62(3) . ? C13 C20 1.53(3) . ? C13 C14 1.59(2) . ? C13 H13A 0.9800 . ? C14 C15 1.55(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 O2 Cd1 O7 109.6(7) . . ? O2 Cd1 O5 114.5(4) . 2_746 ? O7 Cd1 O5 104.0(5) . 2_746 ? O2 Cd1 O4 105.2(6) . 2_847 ? O7 Cd1 O4 120.3(5) . 2_847 ? O5 Cd1 O4 103.5(5) 2_746 2_847 ? O1 Cd2 O8 93.5(6) . 1_655 ? O1 Cd2 O3 99.0(6) . 2_947 ? O8 Cd2 O3 133.8(5) 1_655 2_947 ? O1 Cd2 O6 138.2(5) . 2_746 ? O8 Cd2 O6 99.0(5) 1_655 2_746 ? O3 Cd2 O6 100.5(5) 2_947 2_746 ? O1 Cd2 O4 107.3(5) . 2_947 ? O8 Cd2 O4 79.0(5) 1_655 2_947 ? O3 Cd2 O4 54.9(5) 2_947 2_947 ? O6 Cd2 O4 114.2(5) 2_746 2_947 ? O1 Cd2 O5 84.2(4) . 2_746 ? O8 Cd2 O5 113.8(5) 1_655 2_746 ? O3 Cd2 O5 111.6(5) 2_947 2_746 ? O6 Cd2 O5 54.2(3) 2_746 2_746 ? O4 Cd2 O5 162.8(5) 2_947 2_746 ? O1 Cd2 C10 105.4(6) . 2_947 ? O8 Cd2 C10 106.6(6) 1_655 2_947 ? O3 Cd2 C10 27.2(5) 2_947 2_947 ? O6 Cd2 C10 108.9(5) 2_746 2_947 ? O4 Cd2 C10 27.6(5) 2_947 2_947 ? O5 Cd2 C10 137.9(6) 2_746 2_947 ? C9 O1 Cd2 163.9(14) . . ? C9 O2 Cd1 118.8(14) . . ? C10 O3 Cd2 97.1(13) . 2_957 ? C10 O4 Cd1 156.8(14) . 2_857 ? C10 O4 Cd2 92.0(12) . 2_957 ? Cd1 O4 Cd2 110.2(6) 2_857 2_957 ? C19 O5 Cd1 150.8(10) . 2_756 ? C19 O5 Cd2 93.6(9) . 2_756 ? Cd1 O5 Cd2 112.0(4) 2_756 2_756 ? C19 O6 Cd2 98.3(9) . 2_756 ? C20 O7 Cd1 108.8(15) . . ? C20 O8 Cd2 163.9(13) . 1_455 ? C5 C1 C6 112.7(19) . . ? C5 C1 C2 105.3(13) . . ? C6 C1 C2 113.8(17) . . ? C5 C1 C9 111.7(16) . . ? C6 C1 C9 102.2(16) . . ? C2 C1 C9 111.2(14) . . ? C7 C2 C3 112.8(14) . . ? C7 C2 C8 107.3(17) . . ? C3 C2 C8 107.5(14) . . ? C7 C2 C1 119.7(14) . . ? C3 C2 C1 98.6(11) . . ? C8 C2 C1 110.3(14) . . ? C10 C3 C4 117.1(17) . . ? C10 C3 C2 117.5(13) . . ? C4 C3 C2 106.5(13) . . ? C10 C3 H3A 104.8 . . ? C4 C3 H3A 104.8 . . ? C2 C3 H3A 104.8 . . ? C5 C4 C3 106.1(14) . . ? C5 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? C5 C4 H4C 110.5 . . ? C3 C4 H4C 110.5 . . ? H4B C4 H4C 108.7 . . ? C1 C5 C4 106.1(15) . . ? C1 C5 H5A 110.5 . . ? C4 C5 H5A 110.5 . . ? C1 C5 H5B 110.5 . . ? C4 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 124.9(17) . . ? O2 C9 C1 117.8(17) . . ? O1 C9 C1 117.2(17) . . ? O3 C10 O4 116.0(19) . . ? O3 C10 C3 119.9(19) . . ? O4 C10 C3 124.1(19) . . ? O3 C10 Cd2 55.6(10) . 2_957 ? O4 C10 Cd2 60.4(10) . 2_957 ? C3 C10 Cd2 175.5(15) . 2_957 ? C19 C11 C16 110.0(14) . . ? C19 C11 C12 114.5(14) . . ? C16 C11 C12 112.2(16) . . ? C19 C11 C15 113.2(12) . . ? C16 C11 C15 110.1(16) . . ? C12 C11 C15 96.3(14) . . ? C18 C12 C13 117.1(18) . . ? C18 C12 C11 112.3(14) . . ? C13 C12 C11 105.1(12) . . ? C18 C12 C17 110.5(17) . . ? C13 C12 C17 102.5(15) . . ? C11 C12 C17 108.7(17) . . ? C12 C13 C20 114.0(14) . . ? C12 C13 C14 104.7(14) . . ? C20 C13 C14 114.4(16) . . ? C12 C13 H13A 107.8 . . ? C20 C13 H13A 107.8 . . ? C14 C13 H13A 107.8 . . ? C15 C14 C13 103.4(14) . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14B 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.0 . . ? C14 C15 C11 105.0(14) . . ? C14 C15 H15A 110.7 . . ? C11 C15 H15A 110.7 . . ? C14 C15 H15B 110.7 . . ? C11 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C19 O5 113.8(13) . . ? O6 C19 C11 120.8(13) . . ? O5 C19 C11 125.4(14) . . ? O8 C20 O7 120(2) . . ? O8 C20 C13 123(2) . . ? O7 C20 C13 116(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.668 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.138