# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Shaoming Fang' 'Miao Du' 'Chun-Sen Liu' _publ_contact_author_name 'Du, Miao' _publ_contact_author_email 'dumiao@public.tpt.tj.cn, tjnudumiao@gmail.com' data_1 _database_code_depnum_ccdc_archive 'CCDC 866967' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Cd4 O17' _chemical_formula_weight 1256.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M p_n_m_a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 14.4403(4) _cell_length_b 27.2329(6) _cell_length_c 9.8291(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3865.31(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4159 _cell_measurement_theta_min 3.0577 _cell_measurement_theta_max 72.6730 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 18.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0683 _exptl_absorpt_correction_T_max 0.1089 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_detector_area_resol_mean 16.2542 _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9700 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 72.82 _reflns_number_total 3868 _reflns_number_gt 3419 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and PLATON (Spek, 2009)' _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^)+(0.0641P)^2^+28.9832P] 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 3868 _refine_ls_number_parameters 313 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.113 _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 0.14210(5) -0.2500 0.80836(6) 0.02988(14) Uani 1 2 d S . . Cd2 Cd -0.04886(5) 0.2500 0.53051(7) 0.03207(15) Uani 1 2 d S . . Cd3 Cd 0.20253(14) 0.2500 0.60161(19) 0.0409(4) Uani 0.484(3) 2 d SPD . 1 Cd3' Cd 0.19947(19) 0.26533(10) 0.6242(2) 0.0409(4) Uani 0.2582(15) 1 d PD . 2 Cd4 Cd 0.12225(7) 0.21337(3) 0.26294(10) 0.0358(2) Uani 0.50 1 d PD . . O1 O 0.0936(5) -0.19712(18) 0.9810(6) 0.0624(17) Uani 1 1 d U . . O2 O 0.2235(6) -0.1663(3) 1.0981(8) 0.083(2) Uani 1 1 d . . . O3 O 0.0837(6) 0.1528(2) 0.3971(6) 0.069(2) Uani 1 1 d . . . O4 O 0.0669(4) 0.19553(18) 0.5893(6) 0.0536(15) Uani 1 1 d . . . O5 O 0.3562(5) 0.1860(2) 0.9845(7) 0.074(2) Uani 1 1 d . . . O6 O 0.2897(6) 0.1859(2) 1.1915(6) 0.080(2) Uani 1 1 d . . . O7 O 0.0116(5) -0.2500 0.6925(7) 0.0387(16) Uani 1 2 d S . . H7D H -0.0025 -0.2800 0.6801 0.058 Uiso 0.50 1 d PR . . O8 O 0.2863(6) -0.2500 0.8954(9) 0.061(2) Uani 1 2 d S . . H8D H 0.2856 -0.2802 0.8739 0.092 Uiso 0.50 1 d PR . . O9 O -0.0920(11) 0.2500 0.7626(12) 0.094(4) Uani 1 2 d SU . . H1W H -0.1464 0.2500 0.7934 0.141 Uiso 1 2 d SR . . H2W H -0.0527 0.2500 0.8268 0.141 Uiso 1 2 d SR . . O10 O 0.112(4) 0.2500 0.0613(11) 0.073(4) Uani 0.180(18) 2 d SPDU . 1 H4W H 0.1025 0.2842 0.0401 0.109 Uiso 0.090(9) 1 d PR . 1 H3W H 0.0554 0.2458 0.0451 0.109 Uiso 0.090(9) 1 d PR . 1 O10' O 0.0903(12) 0.1920(7) 0.0496(10) 0.073(4) Uani 0.410(9) 1 d PD . 2 H5W H 0.0434 0.2057 0.0856 0.109 Uiso 0.410(9) 1 d PR . 2 H6W H 0.1336 0.2128 0.0396 0.109 Uiso 0.410(9) 1 d PR . 2 C1 C 0.1515(6) -0.1610(3) 1.0208(9) 0.050(2) Uani 1 1 d . . . C2 C 0.0719(6) 0.1552(3) 0.5211(9) 0.051(2) Uani 1 1 d . . . C3 C 0.3130(6) 0.1654(3) 1.0808(8) 0.0481(19) Uani 1 1 d . . . C4 C 0.1305(6) -0.1113(2) 0.9647(9) 0.052(2) Uani 1 1 d . . . C5 C 0.0694(6) -0.1104(3) 0.8591(12) 0.060(3) Uani 1 1 d . . . H5A H 0.0408 -0.1391 0.8297 0.072 Uiso 1 1 calc R . . C6 C 0.0512(6) -0.0671(3) 0.7980(10) 0.052(2) Uani 1 1 d . . . H6A H 0.0099 -0.0667 0.7253 0.063 Uiso 1 1 calc R . . C7 C 0.0912(5) -0.0228(2) 0.8387(7) 0.0324(14) Uani 1 1 d . . . C8 C 0.1533(5) -0.0231(2) 0.9482(6) 0.0300(14) Uani 1 1 d . . . C9 C 0.1725(5) -0.0675(3) 1.0116(7) 0.0391(16) Uani 1 1 d . . . H9A H 0.2131 -0.0685 1.0850 0.047 Uiso 1 1 calc R . . C10 C 0.0651(5) 0.1086(2) 0.6029(8) 0.0389(16) Uani 1 1 d . . . C11 C 0.0431(6) 0.1089(2) 0.7409(9) 0.0455(18) Uani 1 1 d . . . H11A H 0.0255 0.1382 0.7820 0.055 Uiso 1 1 calc R . . C12 C 0.0470(5) 0.0665(2) 0.8178(7) 0.0403(17) Uani 1 1 d . . . H12A H 0.0321 0.0675 0.9098 0.048 Uiso 1 1 calc R . . C13 C 0.0732(5) 0.0223(2) 0.7576(7) 0.0354(15) Uani 1 1 d . . . C14 C 0.0884(5) 0.0212(2) 0.6174(7) 0.0388(16) Uani 1 1 d . . . H14A H 0.1006 -0.0085 0.5742 0.047 Uiso 1 1 calc R . . C15 C 0.0855(5) 0.0643(3) 0.5420(7) 0.0399(16) Uani 1 1 d . . . H15A H 0.0975 0.0633 0.4491 0.048 Uiso 1 1 calc R . . C17 C 0.2221(5) 0.0902(2) 1.1468(7) 0.0361(15) Uani 1 1 d . . . H17A H 0.2106 0.1045 1.2311 0.043 Uiso 1 1 calc R . . C18 C 0.1852(5) 0.0446(2) 1.1160(7) 0.0340(14) Uani 1 1 d . . . H18A H 0.1501 0.0280 1.1805 0.041 Uiso 1 1 calc R . . C19 C 0.2003(5) 0.0236(2) 0.9895(6) 0.0305(14) Uani 1 1 d . . . C20 C 0.2572(5) 0.0476(2) 0.8967(7) 0.0396(16) Uani 1 1 d . . . H20A H 0.2697 0.0331 0.8130 0.048 Uiso 1 1 calc R . . C21 C 0.2952(6) 0.0925(3) 0.9276(7) 0.0422(17) Uani 1 1 d . . . H21A H 0.3336 0.1081 0.8653 0.051 Uiso 1 1 calc R . . O11 O 0.198(2) 0.2500 0.8281(9) 0.098(6) Uani 0.42(2) 2 d SPDU A 1 H7W H 0.2213 0.2778 0.8101 0.147 Uiso 0.209(11) 1 d PR A 1 H8W H 0.1405 0.2500 0.8070 0.147 Uiso 0.42(2) 2 d SPR A 1 O11' O 0.175(2) 0.2911(10) 0.8355(13) 0.098(6) Uani 0.291(11) 1 d PD . 2 H9W H 0.2317 0.2828 0.8282 0.147 Uiso 0.291(11) 1 d PR A 2 H10W H 0.1654 0.3171 0.7898 0.147 Uiso 0.291(11) 1 d PR A 2 C16 C 0.2761(5) 0.1145(2) 1.0521(7) 0.0375(16) Uani 1 1 d U . . 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 0.0344(3) 0.0221(3) 0.0331(3) 0.000 0.0006(3) 0.000 Cd2 0.0395(3) 0.0204(3) 0.0363(3) 0.000 -0.0028(3) 0.000 Cd3 0.0591(6) 0.0284(12) 0.0351(6) 0.000 0.0012(5) 0.000 Cd3' 0.0591(6) 0.0284(12) 0.0351(6) 0.000 0.0012(5) 0.000 Cd4 0.0332(4) 0.0345(4) 0.0396(5) 0.0004(4) -0.0030(4) -0.0031(4) O1 0.098(4) 0.022(2) 0.067(3) -0.006(2) 0.029(3) -0.015(3) O2 0.113(7) 0.057(4) 0.079(5) 0.003(4) -0.026(5) 0.004(4) O3 0.107(6) 0.047(3) 0.055(3) 0.014(3) -0.002(4) -0.004(4) O4 0.060(3) 0.030(2) 0.070(4) 0.010(2) -0.009(3) 0.010(2) O5 0.096(5) 0.047(3) 0.080(4) -0.007(3) 0.006(4) -0.042(3) O6 0.137(7) 0.046(3) 0.057(3) -0.013(3) -0.006(4) -0.044(4) O7 0.032(3) 0.041(3) 0.044(4) 0.000 0.001(3) 0.000 O8 0.040(4) 0.090(6) 0.054(5) 0.000 -0.002(4) 0.000 O9 0.129(8) 0.082(6) 0.071(5) 0.000 0.009(6) 0.000 O10 0.057(7) 0.094(8) 0.067(7) 0.000 0.004(6) 0.000 O10' 0.057(7) 0.094(8) 0.067(7) 0.000 0.004(6) 0.000 C1 0.057(5) 0.041(4) 0.051(4) 0.004(3) -0.006(4) -0.004(4) C2 0.052(5) 0.040(4) 0.062(5) 0.016(4) -0.008(4) 0.008(3) C3 0.062(5) 0.033(3) 0.049(4) 0.006(3) -0.021(4) -0.018(3) C4 0.063(5) 0.020(3) 0.072(5) 0.007(3) 0.024(4) -0.006(3) C5 0.038(4) 0.027(3) 0.113(8) -0.013(4) 0.000(5) -0.002(3) C6 0.042(4) 0.030(3) 0.085(6) -0.013(4) -0.009(4) -0.003(3) C7 0.034(3) 0.020(2) 0.043(3) -0.003(2) 0.003(3) -0.003(2) C8 0.037(3) 0.019(2) 0.033(3) 0.003(2) 0.009(3) -0.004(2) C9 0.040(4) 0.037(3) 0.041(3) 0.009(3) 0.006(3) 0.000(3) C10 0.035(3) 0.032(3) 0.049(4) 0.008(3) -0.008(3) 0.005(3) C11 0.052(4) 0.027(3) 0.057(4) 0.000(3) 0.008(4) 0.012(3) C12 0.050(4) 0.033(3) 0.038(3) 0.002(3) 0.007(3) 0.012(3) C13 0.035(3) 0.030(3) 0.041(3) -0.001(3) -0.008(3) 0.002(3) C14 0.048(4) 0.027(3) 0.042(3) -0.007(3) -0.005(3) 0.005(3) C15 0.044(4) 0.040(3) 0.036(3) 0.000(3) -0.011(3) 0.006(3) C17 0.044(4) 0.034(3) 0.030(3) -0.004(3) -0.005(3) -0.003(3) C18 0.037(3) 0.030(3) 0.035(3) 0.004(3) 0.003(3) -0.002(3) C19 0.033(3) 0.027(3) 0.031(3) 0.001(2) -0.002(3) 0.000(3) C20 0.049(4) 0.033(3) 0.036(3) -0.007(3) 0.005(3) -0.011(3) C21 0.051(4) 0.040(3) 0.036(3) 0.005(3) 0.004(3) -0.015(3) O11 0.098(9) 0.108(9) 0.089(8) 0.000 -0.003(7) 0.000 O11' 0.098(9) 0.108(9) 0.089(8) 0.000 -0.003(7) 0.000 C16 0.043(3) 0.029(3) 0.040(3) -0.004(3) -0.010(3) -0.009(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 Cd1 O7 2.201(7) . ? Cd1 O8 2.251(8) . ? Cd1 O6 2.310(6) 7_655 ? Cd1 O6 2.310(6) 2_554 ? Cd1 O1 2.333(6) 8 ? Cd1 O1 2.333(6) . ? Cd2 O5 2.222(6) 6_557 ? Cd2 O5 2.222(6) 3_456 ? Cd2 O7 2.257(7) 5_556 ? Cd2 O4 2.308(5) 8_565 ? Cd2 O4 2.308(5) . ? Cd2 O9 2.365(12) . ? Cd3 O8 2.034(9) 2_554 ? Cd3 O11 2.228(9) . ? Cd3 O4 2.460(6) . ? Cd3 O4 2.460(6) 8_565 ? Cd3 O2 2.518(8) 7_665 ? Cd3 O2 2.518(8) 2_554 ? Cd3' Cd3' 0.835(5) 8_565 ? Cd3' O2 2.185(8) 7_665 ? Cd3' O4 2.218(7) 8_565 ? Cd3' O11' 2.221(10) . ? Cd3' O8 2.297(9) 2_554 ? Cd3' O11' 2.608(14) 8_565 ? Cd4 Cd4 1.9951(19) 8_565 ? Cd4 O8 2.106(8) 2_554 ? Cd4 O3 2.184(6) . ? Cd4 O7 2.219(6) 5_556 ? Cd4 O10 2.223(9) . ? Cd4 O10' 2.224(9) . ? Cd4 O6 2.627(9) 1_554 ? O1 C1 1.348(10) . ? O2 C1 1.296(12) . ? O2 Cd3' 2.185(8) 7_656 ? O2 Cd3 2.518(8) 2 ? O3 C2 1.231(11) . ? O4 C2 1.290(10) . ? O4 Cd3' 2.218(7) 8_565 ? O5 C3 1.265(11) . ? O5 Cd2 2.222(6) 6_657 ? O6 C3 1.269(11) . ? O6 Cd1 2.310(6) 2 ? O6 Cd4 2.627(9) 1_556 ? O7 Cd4 2.219(6) 4_546 ? O7 Cd4 2.219(6) 5_556 ? O7 Cd2 2.257(7) 5_556 ? O7 H7D 0.8499 . ? O8 Cd3 2.034(9) 2 ? O8 Cd4 2.106(8) 7_656 ? O8 Cd4 2.106(8) 2 ? O8 Cd3' 2.297(9) 7_656 ? O8 Cd3' 2.297(9) 2 ? O8 H8D 0.8501 . ? O9 H1W 0.8427 . ? O9 H2W 0.8482 . ? O10 Cd4 2.223(9) 8_565 ? O10 H4W 0.9657 . ? O10 H3W 0.8433 . ? O10' H5W 0.8512 . ? O10' H6W 0.8479 . ? C1 C4 1.493(11) . ? C2 C10 1.505(10) . ? C3 C16 1.512(9) . ? C4 C5 1.362(13) . ? C4 C9 1.415(11) . ? C5 C6 1.351(12) . ? C5 H5A 0.9300 . ? C6 C7 1.396(9) . ? C6 H6A 0.9300 . ? C7 C8 1.401(9) . ? C7 C13 1.486(9) . ? C8 C9 1.390(9) . ? C8 C19 1.498(8) . ? C9 H9A 0.9300 . ? C10 C15 1.377(10) . ? C10 C11 1.393(11) . ? C11 C12 1.382(10) . ? C11 H11A 0.9300 . ? C12 C13 1.394(9) . ? C12 H12A 0.9300 . ? C13 C14 1.397(10) . ? C14 C15 1.390(10) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 C16 1.383(10) . ? C17 C18 1.384(9) . ? C17 H17A 0.9300 . ? C18 C19 1.386(9) . ? C18 H18A 0.9300 . ? C19 C20 1.390(10) . ? C20 C21 1.374(10) . ? C20 H20A 0.9300 . ? C21 C16 1.390(10) . ? C21 H21A 0.9300 . ? O11 H7W 0.8498 . ? O11 H8W 0.8591 . ? O11' Cd3' 2.608(14) 8_565 ? O11' H9W 0.8522 . ? O11' H10W 0.8500 . ? 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 O8 171.2(3) . . ? O7 Cd1 O6 96.2(2) . 7_655 ? O8 Cd1 O6 78.2(3) . 7_655 ? O7 Cd1 O6 96.2(2) . 2_554 ? O8 Cd1 O6 78.2(3) . 2_554 ? O6 Cd1 O6 98.2(4) 7_655 2_554 ? O7 Cd1 O1 96.8(2) . 8 ? O8 Cd1 O1 90.1(3) . 8 ? O6 Cd1 O1 91.3(2) 7_655 8 ? O6 Cd1 O1 162.9(2) 2_554 8 ? O7 Cd1 O1 96.8(2) . . ? O8 Cd1 O1 90.1(3) . . ? O6 Cd1 O1 162.9(2) 7_655 . ? O6 Cd1 O1 91.3(2) 2_554 . ? O1 Cd1 O1 76.2(3) 8 . ? O5 Cd2 O5 103.3(4) 6_557 3_456 ? O5 Cd2 O7 94.7(2) 6_557 5_556 ? O5 Cd2 O7 94.7(2) 3_456 5_556 ? O5 Cd2 O4 165.3(2) 6_557 8_565 ? O5 Cd2 O4 87.7(2) 3_456 8_565 ? O7 Cd2 O4 94.1(2) 5_556 8_565 ? O5 Cd2 O4 87.7(2) 6_557 . ? O5 Cd2 O4 165.3(2) 3_456 . ? O7 Cd2 O4 94.1(2) 5_556 . ? O4 Cd2 O4 80.0(3) 8_565 . ? O5 Cd2 O9 84.4(3) 6_557 . ? O5 Cd2 O9 84.4(3) 3_456 . ? O7 Cd2 O9 178.5(4) 5_556 . ? O4 Cd2 O9 87.1(3) 8_565 . ? O4 Cd2 O9 87.1(3) . . ? O8 Cd3 O11 177.3(9) 2_554 . ? O8 Cd3 O4 90.8(2) 2_554 . ? O11 Cd3 O4 91.3(7) . . ? O8 Cd3 O4 90.8(2) 2_554 8_565 ? O11 Cd3 O4 91.3(7) . 8_565 ? O4 Cd3 O4 74.2(2) . 8_565 ? O8 Cd3 O2 87.3(2) 2_554 7_665 ? O11 Cd3 O2 91.6(4) . 7_665 ? O4 Cd3 O2 152.0(2) . 7_665 ? O4 Cd3 O2 77.9(2) 8_565 7_665 ? O8 Cd3 O2 87.3(2) 2_554 2_554 ? O11 Cd3 O2 91.6(4) . 2_554 ? O4 Cd3 O2 77.9(2) . 2_554 ? O4 Cd3 O2 152.0(2) 8_565 2_554 ? O2 Cd3 O2 129.8(4) 7_665 2_554 ? O8 Cd3 H7W 156.7 2_554 . ? O4 Cd3 H7W 110.5 . . ? O4 Cd3 H7W 86.3 8_565 . ? O2 Cd3 H7W 69.5 7_665 . ? O2 Cd3 H7W 105.8 2_554 . ? O8 Cd3 H8W 160.6 2_554 . ? O11 Cd3 H8W 22.1 . . ? O4 Cd3 H8W 73.9 . . ? O4 Cd3 H8W 73.9 8_565 . ? O2 Cd3 H8W 100.6 7_665 . ? O2 Cd3 H8W 100.6 2_554 . ? H7W Cd3 H8W 36.8 . . ? Cd3' Cd3' O2 148.5(2) 8_565 7_665 ? Cd3' Cd3' O4 118.73(15) 8_565 8_565 ? O2 Cd3' O4 90.7(3) 7_665 8_565 ? Cd3' Cd3' O11' 108.4(8) 8_565 . ? O2 Cd3' O11' 85.5(8) 7_665 . ? O4 Cd3' O11' 81.7(8) 8_565 . ? Cd3' Cd3' O8 79.53(8) 8_565 2_554 ? O2 Cd3' O8 89.7(2) 7_665 2_554 ? O4 Cd3' O8 90.8(3) 8_565 2_554 ? O11' Cd3' O8 171.0(8) . 2_554 ? Cd3' Cd3' O11' 53.9(6) 8_565 8_565 ? O2 Cd3' O11' 131.7(7) 7_665 8_565 ? O4 Cd3' O11' 106.8(7) 8_565 8_565 ? O11' Cd3' O11' 54.5(14) . 8_565 ? O8 Cd3' O11' 133.2(6) 2_554 8_565 ? Cd3' Cd3' H7W 100.4 8_565 . ? O2 Cd3' H7W 82.8 7_665 . ? O4 Cd3' H7W 102.0 8_565 . ? O11' Cd3' H7W 20.4 . . ? O8 Cd3' H7W 165.3 2_554 . ? O11' Cd3' H7W 50.0 8_565 . ? Cd3' Cd3' H8W 78.1 8_565 . ? O2 Cd3' H8W 119.5 7_665 . ? O4 Cd3' H8W 82.7 8_565 . ? O11' Cd3' H8W 34.0 . . ? O8 Cd3' H8W 150.0 2_554 . ? O11' Cd3' H8W 28.1 8_565 . ? H7W Cd3' H8W 41.4 . . ? Cd3' Cd3' H9W 103.0 8_565 . ? O2 Cd3' H9W 78.9 7_665 . ? O4 Cd3' H9W 103.2 8_565 . ? O11' Cd3' H9W 22.5 . . ? O8 Cd3' H9W 161.9 2_554 . ? O11' Cd3' H9W 53.6 8_565 . ? H7W Cd3' H9W 4.2 . . ? H8W Cd3' H9W 45.5 . . ? Cd3' Cd3' H10W 129.7 8_565 . ? O2 Cd3' H10W 69.9 7_665 . ? O4 Cd3' H10W 67.3 8_565 . ? O11' Cd3' H10W 22.1 . . ? O8 Cd3' H10W 149.0 2_554 . ? O11' Cd3' H10W 76.0 8_565 . ? H7W Cd3' H10W 37.6 . . ? H8W Cd3' H10W 52.1 . . ? H9W Cd3' H10W 37.4 . . ? Cd4 Cd4 O8 61.72(11) 8_565 2_554 ? Cd4 Cd4 O3 139.03(18) 8_565 . ? O8 Cd4 O3 98.3(3) 2_554 . ? Cd4 Cd4 O7 63.28(8) 8_565 5_556 ? O8 Cd4 O7 102.2(2) 2_554 5_556 ? O3 Cd4 O7 89.9(2) . 5_556 ? Cd4 Cd4 O10 63.34(12) 8_565 . ? O8 Cd4 O10 112.3(9) 2_554 . ? O3 Cd4 O10 149.4(9) . . ? O7 Cd4 O10 85.2(13) 5_556 . ? Cd4 Cd4 O10' 105.2(5) 8_565 . ? O8 Cd4 O10' 146.8(5) 2_554 . ? O3 Cd4 O10' 108.6(5) . . ? O7 Cd4 O10' 97.1(5) 5_556 . ? O10 Cd4 O10' 42.6(6) . . ? Cd4 Cd4 O6 106.54(13) 8_565 1_554 ? O8 Cd4 O6 73.9(2) 2_554 1_554 ? O3 Cd4 O6 100.4(3) . 1_554 ? O7 Cd4 O6 169.34(17) 5_556 1_554 ? O10 Cd4 O6 87.1(13) . 1_554 ? O10' Cd4 O6 82.2(5) . 1_554 ? Cd4 Cd4 H5W 95.7 8_565 . ? O8 Cd4 H5W 154.6 2_554 . ? O3 Cd4 H5W 106.8 . . ? O7 Cd4 H5W 74.6 5_556 . ? O10 Cd4 H5W 42.9 . . ? O10' Cd4 H5W 22.5 . . ? O6 Cd4 H5W 104.5 1_554 . ? Cd4 Cd4 H6W 90.4 8_565 . ? O8 Cd4 H6W 125.0 2_554 . ? O3 Cd4 H6W 128.0 . . ? O7 Cd4 H6W 105.4 5_556 . ? O10 Cd4 H6W 28.3 . . ? O10' Cd4 H6W 22.1 . . ? O6 Cd4 H6W 70.3 1_554 . ? H5W Cd4 H6W 37.7 . . ? C1 O1 Cd1 118.4(6) . . ? C1 O2 Cd3' 124.8(6) . 7_656 ? C1 O2 Cd3 116.6(6) . 2 ? C2 O3 Cd4 126.4(6) . . ? C2 O4 Cd3' 116.2(6) . 8_565 ? C2 O4 Cd2 117.3(5) . . ? Cd3' O4 Cd2 110.8(2) 8_565 . ? C2 O4 Cd3 119.6(6) . . ? Cd2 O4 Cd3 101.61(19) . . ? C3 O5 Cd2 134.6(6) . 6_657 ? C3 O6 Cd1 130.3(6) . 2 ? C3 O6 Cd4 126.7(6) . 1_556 ? Cd1 O6 Cd4 92.5(2) 2 1_556 ? Cd1 O7 Cd4 130.1(3) . 4_546 ? Cd1 O7 Cd4 130.1(3) . 5_556 ? Cd4 O7 Cd4 53.43(17) 4_546 5_556 ? Cd1 O7 Cd2 107.4(3) . 5_556 ? Cd4 O7 Cd2 113.5(3) 4_546 5_556 ? Cd4 O7 Cd2 113.5(3) 5_556 5_556 ? Cd1 O7 H7D 106.3 . . ? Cd4 O7 H7D 52.2 4_546 . ? Cd4 O7 H7D 104.5 5_556 . ? Cd2 O7 H7D 85.3 5_556 . ? Cd3 O8 Cd4 124.5(4) 2 7_656 ? Cd3 O8 Cd4 124.5(4) 2 2 ? Cd4 O8 Cd4 56.6(2) 7_656 2 ? Cd3 O8 Cd1 116.9(4) 2 . ? Cd4 O8 Cd1 110.2(3) 7_656 . ? Cd4 O8 Cd1 110.2(3) 2 . ? Cd4 O8 Cd3' 129.4(4) 7_656 7_656 ? Cd4 O8 Cd3' 117.6(3) 2 7_656 ? Cd1 O8 Cd3' 117.1(4) . 7_656 ? Cd4 O8 Cd3' 117.6(3) 7_656 2 ? Cd4 O8 Cd3' 129.4(4) 2 2 ? Cd1 O8 Cd3' 117.1(4) . 2 ? Cd3 O8 H8D 104.4 2 . ? Cd4 O8 H8D 52.8 7_656 . ? Cd4 O8 H8D 108.2 2 . ? Cd1 O8 H8D 84.0 . . ? Cd3' O8 H8D 114.8 7_656 . ? Cd3' O8 H8D 93.9 2 . ? Cd2 O9 H1W 126.3 . . ? Cd2 O9 H2W 122.8 . . ? H1W O9 H2W 110.9 . . ? Cd4 O10 Cd4 53.3(2) 8_565 . ? Cd4 O10 H4W 76.7 8_565 . ? Cd4 O10 H4W 129.5 . . ? Cd4 O10 H3W 107.0 8_565 . ? Cd4 O10 H3W 99.9 . . ? H4W O10 H3W 87.1 . . ? Cd4 O10 H6W 125.3 8_565 . ? Cd4 O10 H6W 74.7 . . ? H4W O10 H6W 154.7 . . ? H3W O10 H6W 96.5 . . ? Cd4 O10' H5W 70.0 . . ? Cd4 O10' H6W 77.4 . . ? H5W O10' H6W 110.1 . . ? O2 C1 O1 126.0(8) . . ? O2 C1 C4 118.7(8) . . ? O1 C1 C4 115.3(8) . . ? O3 C2 O4 124.5(8) . . ? O3 C2 C10 119.6(8) . . ? O4 C2 C10 115.9(7) . . ? O5 C3 O6 125.1(7) . . ? O5 C3 C16 116.2(7) . . ? O6 C3 C16 118.1(7) . . ? C5 C4 C9 120.7(7) . . ? C5 C4 C1 115.4(7) . . ? C9 C4 C1 123.8(8) . . ? C6 C5 C4 118.7(7) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C7 123.2(8) . . ? C5 C6 H6A 118.4 . . ? C7 C6 H6A 118.4 . . ? C6 C7 C8 118.7(6) . . ? C6 C7 C13 119.1(7) . . ? C8 C7 C13 121.9(6) . . ? C9 C8 C7 118.5(6) . . ? C9 C8 C19 121.9(6) . . ? C7 C8 C19 119.5(5) . . ? C8 C9 C4 120.1(7) . . ? C8 C9 H9A 119.9 . . ? C4 C9 H9A 119.9 . . ? C15 C10 C11 118.5(6) . . ? C15 C10 C2 119.4(7) . . ? C11 C10 C2 122.0(7) . . ? C12 C11 C10 121.2(7) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C13 120.1(7) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 118.7(6) . . ? C12 C13 C7 122.2(6) . . ? C14 C13 C7 119.0(6) . . ? C15 C14 C13 120.2(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C10 C15 C14 121.0(7) . . ? C10 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C16 C17 C18 119.9(6) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C19 120.4(6) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C20 119.2(6) . . ? C18 C19 C8 121.5(6) . . ? C20 C19 C8 119.3(6) . . ? C21 C20 C19 120.6(6) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C16 119.9(7) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? Cd3 O11 H7W 77.2 . . ? Cd3 O11 H8W 77.7 . . ? H7W O11 H8W 109.9 . . ? Cd3 O11 H9W 89.1 . . ? H8W O11 H9W 117.9 . . ? Cd3' O11' H7W 55.4 . . ? Cd3' O11' H7W 51.0 8_565 . ? Cd3' O11' H8W 64.7 . . ? Cd3' O11' H8W 49.5 8_565 . ? H7W O11' H8W 81.8 . . ? Cd3' O11' H9W 71.6 . . ? Cd3' O11' H9W 69.3 8_565 . ? H8W O11' H9W 97.2 . . ? Cd3' O11' H10W 78.2 . . ? Cd3' O11' H10W 95.3 8_565 . ? H7W O11' H10W 110.4 . . ? H8W O11' H10W 124.0 . . ? H9W O11' H10W 109.4 . . ? C17 C16 C21 119.9(6) . . ? C17 C16 C3 120.8(7) . . ? C21 C16 C3 119.3(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cd1 O1 C1 -135.6(6) . . . . ? O8 Cd1 O1 C1 38.9(6) . . . . ? O6 Cd1 O1 C1 84.9(10) 7_655 . . . ? O6 Cd1 O1 C1 -39.2(6) 2_554 . . . ? O1 Cd1 O1 C1 129.0(5) 8 . . . ? Cd4 Cd4 O3 C2 -18.7(11) 8_565 . . . ? O8 Cd4 O3 C2 37.1(9) 2_554 . . . ? O7 Cd4 O3 C2 -65.2(9) 5_556 . . . ? O10 Cd4 O3 C2 -146(2) . . . . ? O10' Cd4 O3 C2 -162.6(9) . . . . ? O6 Cd4 O3 C2 112.1(9) 1_554 . . . ? O5 Cd2 O4 C2 43.0(6) 6_557 . . . ? O5 Cd2 O4 C2 -178.2(9) 3_456 . . . ? O7 Cd2 O4 C2 -51.6(6) 5_556 . . . ? O4 Cd2 O4 C2 -145.0(5) 8_565 . . . ? O9 Cd2 O4 C2 127.5(6) . . . . ? O5 Cd2 O4 Cd3' 179.6(3) 6_557 . . 8_565 ? O5 Cd2 O4 Cd3' -41.6(11) 3_456 . . 8_565 ? O7 Cd2 O4 Cd3' 85.0(3) 5_556 . . 8_565 ? O4 Cd2 O4 Cd3' -8.4(4) 8_565 . . 8_565 ? O9 Cd2 O4 Cd3' -95.9(3) . . . 8_565 ? O5 Cd2 O4 Cd3 175.4(3) 6_557 . . . ? O5 Cd2 O4 Cd3 -45.9(11) 3_456 . . . ? O7 Cd2 O4 Cd3 80.8(2) 5_556 . . . ? O4 Cd2 O4 Cd3 -12.6(3) 8_565 . . . ? O9 Cd2 O4 Cd3 -100.2(3) . . . . ? O8 Cd3 O4 C2 52.4(6) 2_554 . . . ? O11 Cd3 O4 C2 -126.0(8) . . . . ? O4 Cd3 O4 C2 143.0(5) 8_565 . . . ? O2 Cd3 O4 C2 138.2(6) 7_665 . . . ? O2 Cd3 O4 C2 -34.6(6) 2_554 . . . ? O8 Cd3 O4 Cd3' 124.8(6) 2_554 . . 8_565 ? O11 Cd3 O4 Cd3' -53.5(8) . . . 8_565 ? O4 Cd3 O4 Cd3' -144.5(6) 8_565 . . 8_565 ? O2 Cd3 O4 Cd3' -149.4(8) 7_665 . . 8_565 ? O2 Cd3 O4 Cd3' 37.8(6) 2_554 . . 8_565 ? O8 Cd3 O4 Cd2 -78.5(2) 2_554 . . . ? O11 Cd3 O4 Cd2 103.1(6) . . . . ? O4 Cd3 O4 Cd2 12.1(3) 8_565 . . . ? O2 Cd3 O4 Cd2 7.2(6) 7_665 . . . ? O2 Cd3 O4 Cd2 -165.6(3) 2_554 . . . ? O6 Cd1 O7 Cd4 94.6(3) 7_655 . . 4_546 ? O6 Cd1 O7 Cd4 -166.5(3) 2_554 . . 4_546 ? O1 Cd1 O7 Cd4 2.5(3) 8 . . 4_546 ? O1 Cd1 O7 Cd4 -74.4(3) . . . 4_546 ? O6 Cd1 O7 Cd4 166.5(3) 7_655 . . 5_556 ? O6 Cd1 O7 Cd4 -94.6(3) 2_554 . . 5_556 ? O1 Cd1 O7 Cd4 74.4(3) 8 . . 5_556 ? O1 Cd1 O7 Cd4 -2.5(3) . . . 5_556 ? O6 Cd1 O7 Cd2 -49.48(18) 7_655 . . 5_556 ? O6 Cd1 O7 Cd2 49.48(18) 2_554 . . 5_556 ? O1 Cd1 O7 Cd2 -141.56(13) 8 . . 5_556 ? O1 Cd1 O7 Cd2 141.56(13) . . . 5_556 ? O6 Cd1 O8 Cd3 -129.45(18) 7_655 . . 2 ? O6 Cd1 O8 Cd3 129.45(18) 2_554 . . 2 ? O1 Cd1 O8 Cd3 -38.11(13) 8 . . 2 ? O1 Cd1 O8 Cd3 38.11(13) . . . 2 ? O6 Cd1 O8 Cd4 20.2(2) 7_655 . . 7_656 ? O6 Cd1 O8 Cd4 -80.9(3) 2_554 . . 7_656 ? O1 Cd1 O8 Cd4 111.6(2) 8 . . 7_656 ? O1 Cd1 O8 Cd4 -172.2(2) . . . 7_656 ? O6 Cd1 O8 Cd4 80.9(3) 7_655 . . 2 ? O6 Cd1 O8 Cd4 -20.2(2) 2_554 . . 2 ? O1 Cd1 O8 Cd4 172.2(2) 8 . . 2 ? O1 Cd1 O8 Cd4 -111.6(2) . . . 2 ? O6 Cd1 O8 Cd3' -141.2(2) 7_655 . . 7_656 ? O6 Cd1 O8 Cd3' 117.7(2) 2_554 . . 7_656 ? O1 Cd1 O8 Cd3' -49.89(17) 8 . . 7_656 ? O1 Cd1 O8 Cd3' 26.34(17) . . . 7_656 ? O6 Cd1 O8 Cd3' -117.7(2) 7_655 . . 2 ? O6 Cd1 O8 Cd3' 141.2(2) 2_554 . . 2 ? O1 Cd1 O8 Cd3' -26.34(17) 8 . . 2 ? O1 Cd1 O8 Cd3' 49.89(17) . . . 2 ? O8 Cd4 O10 Cd4 -38.8(12) 2_554 . . 8_565 ? O3 Cd4 O10 Cd4 144.1(13) . . . 8_565 ? O7 Cd4 O10 Cd4 62.4(7) 5_556 . . 8_565 ? O10' Cd4 O10 Cd4 168(2) . . . 8_565 ? O6 Cd4 O10 Cd4 -110.1(7) 1_554 . . 8_565 ? Cd3' O2 C1 O1 23.9(13) 7_656 . . . ? Cd3 O2 C1 O1 24.9(12) 2 . . . ? Cd3' O2 C1 C4 -153.7(7) 7_656 . . . ? Cd3 O2 C1 C4 -152.7(6) 2 . . . ? Cd1 O1 C1 O2 -76.9(10) . . . . ? Cd1 O1 C1 C4 100.8(8) . . . . ? Cd4 O3 C2 O4 11.0(14) . . . . ? Cd4 O3 C2 C10 -167.3(6) . . . . ? Cd3' O4 C2 O3 -75.0(11) 8_565 . . . ? Cd2 O4 C2 O3 59.3(12) . . . . ? Cd3 O4 C2 O3 -64.4(11) . . . . ? Cd3' O4 C2 C10 103.4(7) 8_565 . . . ? Cd2 O4 C2 C10 -122.3(6) . . . . ? Cd3 O4 C2 C10 114.0(7) . . . . ? Cd2 O5 C3 O6 24.4(15) 6_657 . . . ? Cd2 O5 C3 C16 -164.0(6) 6_657 . . . ? Cd1 O6 C3 O5 -28.7(14) 2 . . . ? Cd4 O6 C3 O5 106.2(10) 1_556 . . . ? Cd1 O6 C3 C16 159.8(6) 2 . . . ? Cd4 O6 C3 C16 -65.3(9) 1_556 . . . ? O2 C1 C4 C5 164.2(9) . . . . ? O1 C1 C4 C5 -13.6(12) . . . . ? O2 C1 C4 C9 -13.4(13) . . . . ? O1 C1 C4 C9 168.7(8) . . . . ? C9 C4 C5 C6 1.4(14) . . . . ? C1 C4 C5 C6 -176.3(8) . . . . ? C4 C5 C6 C7 -0.7(14) . . . . ? C5 C6 C7 C8 0.0(13) . . . . ? C5 C6 C7 C13 174.7(8) . . . . ? C6 C7 C8 C9 0.1(10) . . . . ? C13 C7 C8 C9 -174.5(6) . . . . ? C6 C7 C8 C19 177.2(7) . . . . ? C13 C7 C8 C19 2.7(10) . . . . ? C7 C8 C9 C4 0.6(10) . . . . ? C19 C8 C9 C4 -176.5(7) . . . . ? C5 C4 C9 C8 -1.4(12) . . . . ? C1 C4 C9 C8 176.1(8) . . . . ? O3 C2 C10 C15 9.5(13) . . . . ? O4 C2 C10 C15 -169.0(7) . . . . ? O3 C2 C10 C11 -173.8(9) . . . . ? O4 C2 C10 C11 7.7(12) . . . . ? C15 C10 C11 C12 3.9(12) . . . . ? C2 C10 C11 C12 -172.8(8) . . . . ? C10 C11 C12 C13 0.0(12) . . . . ? C11 C12 C13 C14 -4.7(12) . . . . ? C11 C12 C13 C7 171.3(7) . . . . ? C6 C7 C13 C12 132.1(8) . . . . ? C8 C7 C13 C12 -53.3(10) . . . . ? C6 C7 C13 C14 -51.8(10) . . . . ? C8 C7 C13 C14 122.7(8) . . . . ? C12 C13 C14 C15 5.7(11) . . . . ? C7 C13 C14 C15 -170.5(7) . . . . ? C11 C10 C15 C14 -2.9(12) . . . . ? C2 C10 C15 C14 173.9(7) . . . . ? C13 C14 C15 C10 -1.9(12) . . . . ? C16 C17 C18 C19 -1.4(11) . . . . ? C17 C18 C19 C20 3.6(10) . . . . ? C17 C18 C19 C8 -173.6(6) . . . . ? C9 C8 C19 C18 -66.7(9) . . . . ? C7 C8 C19 C18 116.3(7) . . . . ? C9 C8 C19 C20 116.2(8) . . . . ? C7 C8 C19 C20 -60.9(9) . . . . ? C18 C19 C20 C21 -2.6(11) . . . . ? C8 C19 C20 C21 174.6(7) . . . . ? C19 C20 C21 C16 -0.5(12) . . . . ? O2 Cd3' O11' Cd3' -151.1(3) 7_665 . . 8_565 ? O4 Cd3' O11' Cd3' 117.6(3) 8_565 . . 8_565 ? C18 C17 C16 C21 -1.7(11) . . . . ? C18 C17 C16 C3 176.8(7) . . . . ? C20 C21 C16 C17 2.7(12) . . . . ? C20 C21 C16 C3 -175.8(7) . . . . ? O5 C3 C16 C17 -175.2(8) . . . . ? O6 C3 C16 C17 -3.0(12) . . . . ? O5 C3 C16 C21 3.3(12) . . . . ? O6 C3 C16 C21 175.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 72.82 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.737 _refine_diff_density_min -2.024 _refine_diff_density_rms 0.171