# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c2_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn3 (C28 H17 O8 Si)2' _chemical_formula_sum 'C56 H34 N0 O16 Si2 Zn3' _chemical_formula_weight 1215.12 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.622(2) _cell_length_b 13.8443(13) _cell_length_c 25.612(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.5820(10) _cell_angle_gamma 90.00 _cell_volume 8124.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.1684 _cell_measurement_theta_max 26.7636 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7014 _exptl_absorpt_correction_T_max 0.8321 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42016 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7982 _reflns_number_gt 6847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0400P)^2^+54.0000P] 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_number_reflns 7982 _refine_ls_number_parameters 380 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.019946(17) 0.28973(3) 0.045124(17) 0.02590(11) Uani 1 1 d . . . O1 O 0.06612(11) 0.29245(19) 0.08699(11) 0.0353(6) Uani 1 1 d . . . C1 C 0.09208(15) 0.3453(2) 0.06566(14) 0.0274(7) Uani 1 1 d . . . Zn2 Zn 0.0000 0.5000 0.0000 0.02202(13) Uani 1 2 d S . . O2 O 0.06848(10) 0.40480(17) 0.02512(10) 0.0288(5) Uani 1 1 d . . . O3 O 0.45667(12) 0.23750(17) 0.46194(10) 0.0328(6) Uani 1 1 d . . . Si4 Si 0.35871(4) 0.28831(7) 0.16520(4) 0.0262(2) Uani 1 1 d . A . O4 O 0.44811(10) 0.08298(16) 0.43278(10) 0.0280(5) Uani 1 1 d . . . O5 O 0.37607(12) -0.1340(2) 0.03004(13) 0.0473(7) Uani 1 1 d . . . O6 O 0.46496(10) -0.07499(17) 0.05768(10) 0.0278(5) Uani 1 1 d . . . O7 O 0.4571(2) 0.6706(3) 0.06765(16) 0.0821(9) Uani 1 1 d . . . O8 O 0.4706(2) 0.7345(3) 0.14923(15) 0.0821(9) Uani 1 1 d . . . H8A H 0.4828 0.7798 0.1358 0.123 Uiso 1 1 calc R . . C2 C 0.15699(15) 0.3323(3) 0.09045(15) 0.0294(7) Uani 1 1 d . . . C3 C 0.18976(17) 0.3082(3) 0.14835(16) 0.0414(10) Uani 1 1 d . . . H3A H 0.1712 0.2993 0.1729 0.050 Uiso 1 1 calc R . . C4 C 0.24943(16) 0.2971(3) 0.17073(16) 0.0382(9) Uani 1 1 d . . . H4A H 0.2716 0.2829 0.2111 0.046 Uiso 1 1 calc R . . C5 C 0.27771(15) 0.3059(3) 0.13609(15) 0.0296(7) Uani 1 1 d . . . C6 C 0.2436(2) 0.3267(5) 0.0775(2) 0.0705(17) Uani 1 1 d . . . H6A H 0.2616 0.3319 0.0522 0.085 Uiso 1 1 calc R . . C7 C 0.1832(2) 0.3401(5) 0.0549(2) 0.0667(16) Uani 1 1 d . . . H7A H 0.1607 0.3547 0.0147 0.080 Uiso 1 1 calc R . . C15 C 0.39843(14) 0.0184(2) 0.07879(14) 0.0264(7) Uani 1 1 d . . . C16 C 0.44171(15) 0.0829(3) 0.11112(16) 0.0313(8) Uani 1 1 d . . . H16A H 0.4805 0.0716 0.1170 0.038 Uiso 1 1 calc R . . C18 C 0.37343(15) 0.1823(3) 0.12848(15) 0.0273(7) Uani 1 1 d . . . C19 C 0.32995(16) 0.1138(3) 0.09585(17) 0.0375(9) Uani 1 1 d . . . H19A H 0.2909 0.1240 0.0895 0.045 Uiso 1 1 calc R . . C20 C 0.34330(16) 0.0331(3) 0.07323(18) 0.0413(9) Uani 1 1 d . . . H20A H 0.3138 -0.0136 0.0534 0.050 Uiso 1 1 calc R . . C21 C 0.41206(16) -0.0698(3) 0.05299(15) 0.0325(8) Uani 1 1 d . . . C23 C 0.41060(19) 0.3253(3) 0.28967(16) 0.0389(9) Uani 1 1 d . . . H23A H 0.4135 0.3911 0.2807 0.047 Uiso 1 1 calc R . . C24 C 0.42831(19) 0.2982(3) 0.34731(17) 0.0395(9) Uani 1 1 d . . . H24A H 0.4433 0.3457 0.3772 0.047 Uiso 1 1 calc R . . C25 C 0.42455(14) 0.2038(2) 0.36172(14) 0.0251(7) Uani 1 1 d . . . C26 C 0.40267(15) 0.1346(2) 0.31746(14) 0.0288(7) Uani 1 1 d . . . H26A H 0.3996 0.0691 0.3266 0.035 Uiso 1 1 calc R . . C27 C 0.38544(16) 0.1622(3) 0.25987(15) 0.0316(8) Uani 1 1 d . . . H27A H 0.3711 0.1146 0.2300 0.038 Uiso 1 1 calc R . . C28 C 0.38882(14) 0.2579(3) 0.24519(14) 0.0271(7) Uani 1 1 d . . . C8 C 0.39223(12) 0.4009(2) 0.15299(12) 0.0316(8) Uani 1 1 d D . . C11 C 0.43548(10) 0.5739(2) 0.12950(9) 0.0344(8) Uani 1 1 d D . . C14 C 0.45852(15) 0.6662(3) 0.11687(14) 0.0446(10) Uani 1 1 d D A . C9 C 0.41968(17) 0.4053(4) 0.11690(17) 0.0408(17) Uani 0.568(5) 1 d PD A 1 H9A H 0.4237 0.3466 0.0998 0.049 Uiso 0.568(5) 1 calc PR A 1 C10 C 0.44170(18) 0.4888(2) 0.10400(18) 0.0427(18) Uani 0.568(5) 1 d PD A 1 H10A H 0.4601 0.4878 0.0790 0.051 Uiso 0.568(5) 1 calc PR A 1 C12 C 0.40839(16) 0.5741(3) 0.16596(15) 0.0392(17) Uani 0.568(5) 1 d PD A 1 H12A H 0.4044 0.6327 0.1831 0.047 Uiso 0.568(5) 1 calc PR A 1 C13 C 0.38721(19) 0.4882(2) 0.17723(18) 0.0333(15) Uani 0.568(5) 1 d PD A 1 H13A H 0.3688 0.4891 0.2022 0.040 Uiso 0.568(5) 1 calc PR A 1 C9' C 0.3597(2) 0.4537(4) 0.1026(2) 0.059(3) Uani 0.432(5) 1 d PD A 2 H9'A H 0.3222 0.4309 0.0757 0.071 Uiso 0.432(5) 1 calc PR A 2 C10' C 0.38085(16) 0.5392(5) 0.0908(2) 0.063(4) Uani 0.432(5) 1 d PD A 2 H10B H 0.3578 0.5740 0.0561 0.075 Uiso 0.432(5) 1 calc PR A 2 C12' C 0.4676(3) 0.5203(4) 0.17972(18) 0.043(2) Uani 0.432(5) 1 d PD A 2 H12B H 0.5050 0.5431 0.2066 0.051 Uiso 0.432(5) 1 calc PR A 2 C13' C 0.44693(16) 0.4348(4) 0.1921(2) 0.042(2) Uani 0.432(5) 1 d PD A 2 H13B H 0.4699 0.3998 0.2268 0.050 Uiso 0.432(5) 1 calc PR A 2 C22 C 0.44458(15) 0.1722(2) 0.42373(14) 0.0276(7) Uani 1 1 d . . . C17 C 0.42949(16) 0.1641(3) 0.13528(17) 0.0363(8) Uani 1 1 d . . . H17A H 0.4600 0.2082 0.1569 0.044 Uiso 1 1 calc R . . 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 Zn1 0.0325(2) 0.0201(2) 0.0254(2) 0.00253(15) 0.01322(17) -0.00221(16) O1 0.0326(13) 0.0388(14) 0.0352(14) 0.0135(11) 0.0158(11) 0.0059(11) C1 0.0321(18) 0.0264(17) 0.0262(17) 0.0030(14) 0.0154(15) 0.0068(14) Zn2 0.0235(3) 0.0169(2) 0.0210(3) -0.0016(2) 0.0057(2) 0.0008(2) O2 0.0324(13) 0.0268(12) 0.0265(12) 0.0073(10) 0.0126(10) 0.0103(10) O3 0.0492(15) 0.0228(12) 0.0272(12) 0.0020(10) 0.0177(11) 0.0044(11) Si4 0.0284(5) 0.0264(5) 0.0277(5) 0.0089(4) 0.0161(4) 0.0051(4) O4 0.0340(13) 0.0235(12) 0.0232(11) 0.0051(9) 0.0098(10) 0.0012(10) O5 0.0434(16) 0.0387(16) 0.0628(19) -0.0200(14) 0.0266(15) -0.0168(13) O6 0.0285(12) 0.0248(12) 0.0292(12) 0.0006(10) 0.0120(10) 0.0002(10) O7 0.147(3) 0.0554(15) 0.0556(15) -0.0062(12) 0.0561(17) -0.0496(17) O8 0.147(3) 0.0554(15) 0.0556(15) -0.0062(12) 0.0561(17) -0.0496(17) C2 0.0312(18) 0.0300(18) 0.0291(17) 0.0083(14) 0.0154(15) 0.0089(14) C3 0.036(2) 0.064(3) 0.0296(19) 0.0093(18) 0.0190(17) 0.0028(19) C4 0.0316(19) 0.056(2) 0.0291(19) 0.0108(17) 0.0152(16) 0.0052(17) C5 0.0292(17) 0.0311(18) 0.0342(18) 0.0111(15) 0.0193(15) 0.0079(14) C6 0.048(3) 0.126(5) 0.049(3) 0.046(3) 0.032(2) 0.035(3) C7 0.044(2) 0.119(5) 0.040(2) 0.041(3) 0.020(2) 0.036(3) C15 0.0288(17) 0.0278(17) 0.0227(16) 0.0013(13) 0.0114(14) -0.0032(14) C16 0.0259(17) 0.0339(19) 0.0372(19) -0.0016(15) 0.0168(15) -0.0029(15) C18 0.0272(17) 0.0308(18) 0.0269(17) 0.0046(14) 0.0147(14) 0.0036(14) C19 0.0224(17) 0.043(2) 0.047(2) -0.0054(18) 0.0155(16) -0.0012(16) C20 0.0283(19) 0.046(2) 0.047(2) -0.0101(19) 0.0138(18) -0.0094(17) C21 0.0353(19) 0.0317(19) 0.0302(18) 0.0040(15) 0.0144(16) 0.0009(16) C23 0.063(3) 0.0236(18) 0.0321(19) 0.0054(15) 0.0225(19) 0.0043(17) C24 0.060(3) 0.0302(19) 0.0314(19) -0.0007(15) 0.0237(19) -0.0007(18) C25 0.0247(16) 0.0269(17) 0.0224(16) 0.0043(13) 0.0094(13) 0.0032(13) C26 0.0396(19) 0.0222(16) 0.0226(16) 0.0033(13) 0.0120(15) 0.0001(14) C27 0.039(2) 0.0267(18) 0.0237(17) 0.0032(14) 0.0093(15) -0.0031(15) C28 0.0271(17) 0.0314(18) 0.0236(16) 0.0073(14) 0.0120(14) 0.0042(14) C8 0.0377(19) 0.0281(18) 0.0333(19) 0.0122(15) 0.0196(16) 0.0079(15) C11 0.0357(19) 0.0315(19) 0.037(2) 0.0072(16) 0.0175(17) 0.0000(16) C14 0.056(3) 0.032(2) 0.041(2) 0.0015(18) 0.018(2) -0.0117(19) C9 0.060(5) 0.026(3) 0.050(4) 0.005(3) 0.037(4) 0.005(3) C10 0.050(4) 0.035(4) 0.062(5) 0.009(3) 0.042(4) 0.006(3) C12 0.055(4) 0.026(3) 0.041(4) 0.008(3) 0.026(3) 0.008(3) C13 0.036(3) 0.032(3) 0.037(3) 0.004(3) 0.020(3) 0.004(3) C9' 0.044(6) 0.061(7) 0.056(6) 0.026(5) 0.009(5) -0.026(5) C10' 0.064(7) 0.058(7) 0.042(6) 0.034(5) 0.002(5) -0.024(6) C12' 0.037(5) 0.044(5) 0.042(5) 0.005(4) 0.013(4) -0.002(4) C13' 0.048(5) 0.037(5) 0.039(5) 0.009(4) 0.018(4) 0.003(4) C22 0.0291(17) 0.0274(17) 0.0260(17) 0.0028(14) 0.0122(14) 0.0023(14) C17 0.0282(18) 0.039(2) 0.047(2) -0.0111(17) 0.0210(17) -0.0081(16) _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 Zn1 O7 1.924(3) 3_445 ? Zn1 O6 1.968(2) 3_455 ? Zn1 O3 1.974(2) 8_455 ? Zn1 O1 1.974(3) . ? O1 C1 1.266(4) . ? C1 O2 1.249(4) . ? C1 C2 1.502(5) . ? Zn2 O4 2.001(2) 8_455 ? Zn2 O4 2.001(2) 4 ? Zn2 O2 2.054(2) 5_565 ? Zn2 O2 2.054(2) . ? Zn2 O6 2.292(2) 7 ? Zn2 O6 2.292(2) 3_455 ? O3 C22 1.264(4) . ? O3 Zn1 1.974(2) 8_556 ? Si4 C18 1.871(4) . ? Si4 C8 1.873(3) . ? Si4 C5 1.881(4) . ? Si4 C28 1.885(3) . ? O4 C22 1.253(4) . ? O4 Zn2 2.001(2) 4_545 ? O5 C21 1.225(4) . ? O6 C21 1.308(4) . ? O6 Zn1 1.968(2) 3_545 ? O6 Zn2 2.292(2) 3_545 ? O7 C14 1.246(5) . ? O7 Zn1 1.924(3) 3 ? O8 C14 1.203(5) . ? O8 H8A 0.8400 . ? C2 C7 1.358(5) . ? C2 C3 1.379(5) . ? C3 C4 1.380(5) . ? C3 H3A 0.9500 . ? C4 C5 1.379(5) . ? C4 H4A 0.9500 . ? C5 C6 1.388(6) . ? C6 C7 1.401(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C15 C20 1.370(5) . ? C15 C16 1.375(5) . ? C15 C21 1.502(5) . ? C16 C17 1.385(5) . ? C16 H16A 0.9500 . ? C18 C17 1.390(5) . ? C18 C19 1.415(5) . ? C19 C20 1.371(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C23 C28 1.383(5) . ? C23 C24 1.388(5) . ? C23 H23A 0.9500 . ? C24 C25 1.373(5) . ? C24 H24A 0.9500 . ? C25 C26 1.396(5) . ? C25 C22 1.499(4) . ? C26 C27 1.390(5) . ? C26 H26A 0.9500 . ? C27 C28 1.391(5) . ? C27 H27A 0.9500 . ? C8 C13' 1.3891(10) . ? C8 C13 1.3897(10) . ? C8 C9' 1.3898(10) . ? C8 C9 1.3908(10) . ? C11 C10' 1.3896(10) . ? C11 C10 1.3896(10) . ? C11 C12' 1.3904(10) . ? C11 C12 1.3906(10) . ? C11 C14 1.503(5) . ? C9 C10 1.3901(10) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C12 C13 1.3901(10) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C9' C10' 1.3900(10) . ? C9' H9'A 0.9500 . ? C10' H10B 0.9500 . ? C12' C13' 1.3899(10) . ? C12' H12B 0.9500 . ? C13' H13B 0.9500 . ? C17 H17A 0.9500 . ? 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 Zn1 O6 131.15(15) 3_445 3_455 ? O7 Zn1 O3 100.02(13) 3_445 8_455 ? O6 Zn1 O3 111.79(10) 3_455 8_455 ? O7 Zn1 O1 105.69(16) 3_445 . ? O6 Zn1 O1 98.43(10) 3_455 . ? O3 Zn1 O1 108.39(11) 8_455 . ? C1 O1 Zn1 116.8(2) . . ? O2 C1 O1 126.0(3) . . ? O2 C1 C2 117.6(3) . . ? O1 C1 C2 116.4(3) . . ? O4 Zn2 O4 180.00(15) 8_455 4 ? O4 Zn2 O2 87.32(9) 8_455 5_565 ? O4 Zn2 O2 92.68(9) 4 5_565 ? O4 Zn2 O2 92.68(9) 8_455 . ? O4 Zn2 O2 87.32(9) 4 . ? O2 Zn2 O2 180.0 5_565 . ? O4 Zn2 O6 90.38(9) 8_455 7 ? O4 Zn2 O6 89.62(9) 4 7 ? O2 Zn2 O6 91.92(9) 5_565 7 ? O2 Zn2 O6 88.08(9) . 7 ? O4 Zn2 O6 89.62(9) 8_455 3_455 ? O4 Zn2 O6 90.38(9) 4 3_455 ? O2 Zn2 O6 88.08(9) 5_565 3_455 ? O2 Zn2 O6 91.92(9) . 3_455 ? O6 Zn2 O6 180.00(9) 7 3_455 ? C1 O2 Zn2 135.3(2) . . ? C22 O3 Zn1 123.3(2) . 8_556 ? C18 Si4 C8 111.03(14) . . ? C18 Si4 C5 109.70(16) . . ? C8 Si4 C5 109.46(14) . . ? C18 Si4 C28 107.12(15) . . ? C8 Si4 C28 111.86(14) . . ? C5 Si4 C28 107.58(15) . . ? C22 O4 Zn2 133.7(2) . 4_545 ? C21 O6 Zn1 108.0(2) . 3_545 ? C21 O6 Zn2 127.2(2) . 3_545 ? Zn1 O6 Zn2 99.41(10) 3_545 3_545 ? C14 O7 Zn1 118.1(3) . 3 ? C14 O8 H8A 109.5 . . ? C7 C2 C3 119.7(3) . . ? C7 C2 C1 119.6(3) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 117.2(3) . . ? C4 C5 Si4 122.5(3) . . ? C6 C5 Si4 120.3(3) . . ? C5 C6 C7 121.3(4) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C2 C7 C6 119.9(4) . . ? C2 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C20 C15 C16 118.9(3) . . ? C20 C15 C21 120.4(3) . . ? C16 C15 C21 120.6(3) . . ? C15 C16 C17 120.9(3) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C17 C18 C19 116.7(3) . . ? C17 C18 Si4 120.6(3) . . ? C19 C18 Si4 122.7(3) . . ? C20 C19 C18 121.1(3) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C15 C20 C19 121.1(3) . . ? C15 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? O5 C21 O6 122.0(3) . . ? O5 C21 C15 121.9(3) . . ? O6 C21 C15 116.1(3) . . ? C28 C23 C24 120.9(3) . . ? C28 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 119.1(3) . . ? C24 C25 C22 122.1(3) . . ? C26 C25 C22 118.9(3) . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 121.3(3) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C23 C28 C27 118.1(3) . . ? C23 C28 Si4 124.2(3) . . ? C27 C28 Si4 117.5(3) . . ? C13' C8 C13 69.6(3) . . ? C13' C8 C9' 119.0(5) . . ? C13 C8 C9' 79.7(3) . . ? C13' C8 C9 79.5(3) . . ? C13 C8 C9 115.8(4) . . ? C9' C8 C9 68.4(3) . . ? C13' C8 Si4 123.4(3) . . ? C13 C8 Si4 120.5(3) . . ? C9' C8 Si4 117.6(3) . . ? C9 C8 Si4 123.6(3) . . ? C10' C11 C10 70.3(3) . . ? C10' C11 C12' 117.7(5) . . ? C10 C11 C12' 80.7(3) . . ? C10' C11 C12 80.4(3) . . ? C10 C11 C12 120.9(4) . . ? C12' C11 C12 69.3(3) . . ? C10' C11 C14 120.5(3) . . ? C10 C11 C14 118.7(2) . . ? C12' C11 C14 121.7(3) . . ? C12 C11 C14 120.3(2) . . ? O8 C14 O7 122.7(4) . . ? O8 C14 C11 121.7(3) . . ? O7 C14 C11 115.0(3) . . ? C10 C9 C8 125.0(5) . . ? C10 C9 H9A 117.5 . . ? C8 C9 H9A 117.5 . . ? C11 C10 C9 116.7(4) . . ? C11 C10 H10A 121.7 . . ? C9 C10 H10A 121.7 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C8 C13 C12 121.9(4) . . ? C8 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C8 C9' C10' 121.2(6) . . ? C8 C9' H9'A 119.4 . . ? C10' C9' H9'A 119.4 . . ? C11 C10' C9' 120.4(6) . . ? C11 C10' H10B 119.8 . . ? C9' C10' H10B 119.8 . . ? C13' C12' C11 122.5(6) . . ? C13' C12' H12B 118.7 . . ? C11 C12' H12B 118.7 . . ? C8 C13' C12' 119.1(6) . . ? C8 C13' H13B 120.4 . . ? C12' C13' H13B 120.4 . . ? O4 C22 O3 126.1(3) . . ? O4 C22 C25 116.5(3) . . ? O3 C22 C25 117.4(3) . . ? C16 C17 C18 121.2(3) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? 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 Zn1 O1 C1 157.4(3) 3_445 . . . ? O6 Zn1 O1 C1 -65.5(3) 3_455 . . . ? O3 Zn1 O1 C1 51.0(3) 8_455 . . . ? Zn1 O1 C1 O2 9.5(5) . . . . ? Zn1 O1 C1 C2 -168.4(2) . . . . ? O1 C1 O2 Zn2 37.4(5) . . . . ? C2 C1 O2 Zn2 -144.8(3) . . . . ? O4 Zn2 O2 C1 -105.8(3) 8_455 . . . ? O4 Zn2 O2 C1 74.2(3) 4 . . . ? O2 Zn2 O2 C1 -93(5) 5_565 . . . ? O6 Zn2 O2 C1 163.9(3) 7 . . . ? O6 Zn2 O2 C1 -16.1(3) 3_455 . . . ? O2 C1 C2 C7 -34.0(6) . . . . ? O1 C1 C2 C7 144.0(4) . . . . ? O2 C1 C2 C3 148.9(4) . . . . ? O1 C1 C2 C3 -33.1(5) . . . . ? C7 C2 C3 C4 3.3(7) . . . . ? C1 C2 C3 C4 -179.6(4) . . . . ? C2 C3 C4 C5 -2.4(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C3 C4 C5 Si4 -178.6(3) . . . . ? C18 Si4 C5 C4 116.5(3) . . . . ? C8 Si4 C5 C4 -121.4(3) . . . . ? C28 Si4 C5 C4 0.3(4) . . . . ? C18 Si4 C5 C6 -62.1(4) . . . . ? C8 Si4 C5 C6 59.9(4) . . . . ? C28 Si4 C5 C6 -178.3(4) . . . . ? C4 C5 C6 C7 1.3(8) . . . . ? Si4 C5 C6 C7 -180.0(5) . . . . ? C3 C2 C7 C6 -2.0(8) . . . . ? C1 C2 C7 C6 -179.1(5) . . . . ? C5 C6 C7 C2 -0.4(10) . . . . ? C20 C15 C16 C17 -3.3(5) . . . . ? C21 C15 C16 C17 -179.7(3) . . . . ? C8 Si4 C18 C17 48.2(3) . . . . ? C5 Si4 C18 C17 169.3(3) . . . . ? C28 Si4 C18 C17 -74.2(3) . . . . ? C8 Si4 C18 C19 -135.8(3) . . . . ? C5 Si4 C18 C19 -14.7(3) . . . . ? C28 Si4 C18 C19 101.8(3) . . . . ? C17 C18 C19 C20 1.2(6) . . . . ? Si4 C18 C19 C20 -175.0(3) . . . . ? C16 C15 C20 C19 4.5(6) . . . . ? C21 C15 C20 C19 -179.1(4) . . . . ? C18 C19 C20 C15 -3.5(6) . . . . ? Zn1 O6 C21 O5 -16.7(4) 3_545 . . . ? Zn2 O6 C21 O5 100.8(4) 3_545 . . . ? Zn1 O6 C21 C15 161.7(2) 3_545 . . . ? Zn2 O6 C21 C15 -80.7(3) 3_545 . . . ? C20 C15 C21 O5 -5.2(5) . . . . ? C16 C15 C21 O5 171.2(4) . . . . ? C20 C15 C21 O6 176.4(3) . . . . ? C16 C15 C21 O6 -7.3(5) . . . . ? C28 C23 C24 C25 -0.2(6) . . . . ? C23 C24 C25 C26 0.2(6) . . . . ? C23 C24 C25 C22 178.6(4) . . . . ? C24 C25 C26 C27 0.4(5) . . . . ? C22 C25 C26 C27 -178.2(3) . . . . ? C25 C26 C27 C28 -0.9(6) . . . . ? C24 C23 C28 C27 -0.3(6) . . . . ? C24 C23 C28 Si4 175.5(3) . . . . ? C26 C27 C28 C23 0.8(5) . . . . ? C26 C27 C28 Si4 -175.3(3) . . . . ? C18 Si4 C28 C23 149.5(3) . . . . ? C8 Si4 C28 C23 27.6(4) . . . . ? C5 Si4 C28 C23 -92.6(3) . . . . ? C18 Si4 C28 C27 -34.7(3) . . . . ? C8 Si4 C28 C27 -156.6(3) . . . . ? C5 Si4 C28 C27 83.2(3) . . . . ? C18 Si4 C8 C13' -94.7(3) . . . . ? C5 Si4 C8 C13' 144.0(3) . . . . ? C28 Si4 C8 C13' 24.9(3) . . . . ? C18 Si4 C8 C13 -179.1(2) . . . . ? C5 Si4 C8 C13 59.6(2) . . . . ? C28 Si4 C8 C13 -59.5(2) . . . . ? C18 Si4 C8 C9' 86.7(3) . . . . ? C5 Si4 C8 C9' -34.6(3) . . . . ? C28 Si4 C8 C9' -153.7(3) . . . . ? C18 Si4 C8 C9 5.4(2) . . . . ? C5 Si4 C8 C9 -115.9(2) . . . . ? C28 Si4 C8 C9 125.0(2) . . . . ? Zn1 O7 C14 O8 4.0(7) 3 . . . ? Zn1 O7 C14 C11 175.3(2) 3 . . . ? C10' C11 C14 O8 119.7(4) . . . . ? C10 C11 C14 O8 -157.4(4) . . . . ? C12' C11 C14 O8 -60.4(5) . . . . ? C12 C11 C14 O8 22.7(4) . . . . ? C10' C11 C14 O7 -51.7(4) . . . . ? C10 C11 C14 O7 31.2(4) . . . . ? C12' C11 C14 O7 128.2(4) . . . . ? C12 C11 C14 O7 -148.7(4) . . . . ? C13' C8 C9 C10 -61.0(3) . . . . ? C13 C8 C9 C10 0.00(3) . . . . ? C9' C8 C9 C10 66.1(3) . . . . ? Si4 C8 C9 C10 175.72(16) . . . . ? C10' C11 C10 C9 -65.2(3) . . . . ? C12' C11 C10 C9 58.8(3) . . . . ? C12 C11 C10 C9 -0.07(7) . . . . ? C14 C11 C10 C9 -179.94(4) . . . . ? C8 C9 C10 C11 0.04(3) . . . . ? C10' C11 C12 C13 60.1(3) . . . . ? C10 C11 C12 C13 0.06(9) . . . . ? C12' C11 C12 C13 -64.6(3) . . . . ? C14 C11 C12 C13 179.93(6) . . . . ? C13' C8 C13 C12 66.6(3) . . . . ? C9' C8 C13 C12 -59.8(3) . . . . ? C9 C8 C13 C12 -0.01(7) . . . . ? Si4 C8 C13 C12 -175.87(16) . . . . ? C11 C12 C13 C8 -0.02(9) . . . . ? C13' C8 C9' C10' 0.00(3) . . . . ? C13 C8 C9' C10' 59.5(2) . . . . ? C9 C8 C9' C10' -63.6(3) . . . . ? Si4 C8 C9' C10' 178.70(16) . . . . ? C10 C11 C10' C9' 67.5(3) . . . . ? C12' C11 C10' C9' 0.03(6) . . . . ? C12 C11 C10' C9' -60.4(2) . . . . ? C14 C11 C10' C9' 179.97(4) . . . . ? C8 C9' C10' C11 -0.02(3) . . . . ? C10' C11 C12' C13' -0.02(9) . . . . ? C10 C11 C12' C13' -61.8(3) . . . . ? C12 C11 C12' C13' 66.4(3) . . . . ? C14 C11 C12' C13' -179.97(6) . . . . ? C13 C8 C13' C12' -64.8(3) . . . . ? C9' C8 C13' C12' 0.01(6) . . . . ? C9 C8 C13' C12' 57.9(3) . . . . ? Si4 C8 C13' C12' -178.62(18) . . . . ? C11 C12' C13' C8 0.00(9) . . . . ? Zn2 O4 C22 O3 -31.0(5) 4_545 . . . ? Zn2 O4 C22 C25 148.5(2) 4_545 . . . ? Zn1 O3 C22 O4 -3.5(5) 8_556 . . . ? Zn1 O3 C22 C25 177.0(2) 8_556 . . . ? C24 C25 C22 O4 -168.6(3) . . . . ? C26 C25 C22 O4 9.9(5) . . . . ? C24 C25 C22 O3 10.9(5) . . . . ? C26 C25 C22 O3 -170.6(3) . . . . ? C15 C16 C17 C18 1.1(6) . . . . ? C19 C18 C17 C16 0.0(6) . . . . ? Si4 C18 C17 C16 176.3(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.999 _refine_diff_density_min -2.008 _refine_diff_density_rms 0.084 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.009 -0.004 3708.2 1027.6 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942372' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pcn513_alertkiller_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn5O2H (C28 H16 O8 Si)2 (C5H9NO)4 (C3H7NO)2' _chemical_formula_sum 'C82 H84 N6 O24 Si2 Zn5' _chemical_formula_weight 1920.58 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9350(16) _cell_length_b 14.196(3) _cell_length_c 14.6708(17) _cell_angle_alpha 107.988(2) _cell_angle_beta 113.7350(10) _cell_angle_gamma 100.298(2) _cell_volume 2368.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7012 _cell_measurement_theta_min 2.2655 _cell_measurement_theta_max 26.3067 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6157 _exptl_absorpt_correction_T_max 0.6888 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24912 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9284 _reflns_number_gt 6544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9284 _refine_ls_number_parameters 470 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2693 _refine_ls_wR_factor_gt 0.2562 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 1.0000 0.5000 0.0243(2) Uani 1 2 d S . . Zn2 Zn 0.52875(6) 1.20329(6) 0.44345(6) 0.0358(2) Uani 1 1 d . . . Zn3 Zn 0.30330(7) 0.99584(5) 0.26420(7) 0.0406(3) Uani 1 1 d . . . Si1 Si 0.23617(12) 1.36569(12) 0.88000(12) 0.0244(3) Uani 1 1 d . . . O1 O -0.3143(4) 1.2195(4) 0.5134(4) 0.0441(11) Uani 1 1 d . . . O2 O -0.3362(3) 1.1227(3) 0.6050(4) 0.0371(10) Uani 1 1 d . . . O3 O 0.3123(4) 1.1105(4) 1.2139(4) 0.0510(13) Uani 1 1 d . . . O4 O 0.4751(3) 1.2443(3) 1.3211(4) 0.0371(10) Uani 1 1 d . . . O5 O 0.2704(3) 1.8642(3) 1.1488(3) 0.0354(10) Uani 1 1 d . . . O6 O 0.4477(3) 1.9072(3) 1.1778(4) 0.0384(10) Uani 1 1 d . . . O7 O 0.4651(3) 1.2434(3) 0.5395(3) 0.0323(9) Uani 1 1 d . . . O8 O 0.4270(3) 1.0951(3) 0.5626(3) 0.0334(9) Uani 1 1 d . . . C1 C -0.2775(5) 1.1843(5) 0.5872(5) 0.0348(14) Uani 1 1 d . . . C2 C -0.1540(5) 1.2242(5) 0.6572(5) 0.0374(14) Uani 1 1 d . . . C3 C -0.0832(5) 1.2505(6) 0.6158(5) 0.0452(17) Uani 1 1 d . . . H3A H -0.1143 1.2412 0.5415 0.054 Uiso 1 1 calc R . . C4 C 0.0325(5) 1.2902(6) 0.6830(5) 0.0406(16) Uani 1 1 d . . . H4A H 0.0792 1.3085 0.6540 0.049 Uiso 1 1 calc R . . C5 C 0.0806(4) 1.3036(4) 0.7912(4) 0.0255(11) Uani 1 1 d . . . C6 C 0.0088(5) 1.2796(4) 0.8337(5) 0.0307(13) Uani 1 1 d . . . H6A H 0.0398 1.2923 0.9089 0.037 Uiso 1 1 calc R . . C7 C -0.1051(5) 1.2382(5) 0.7668(5) 0.0317(13) Uani 1 1 d . . . H7A H -0.1517 1.2186 0.7954 0.038 Uiso 1 1 calc R . . C8 C 0.3839(5) 1.1938(5) 1.2355(5) 0.0319(13) Uani 1 1 d . . . C9 C 0.3511(5) 1.2370(5) 1.1497(5) 0.0292(12) Uani 1 1 d . . . C10 C 0.4095(5) 1.3402(5) 1.1743(5) 0.0344(13) Uani 1 1 d . . . H10A H 0.4733 1.3836 1.2443 0.041 Uiso 1 1 calc R . . C11 C 0.3731(5) 1.3782(5) 1.0950(5) 0.0302(13) Uani 1 1 d . . . H11A H 0.4109 1.4493 1.1127 0.036 Uiso 1 1 calc R . . C12 C 0.2821(5) 1.3150(5) 0.9893(5) 0.0314(13) Uani 1 1 d . . . C13 C 0.2272(5) 1.2123(5) 0.9675(5) 0.0346(14) Uani 1 1 d . . . H13A H 0.1662 1.1672 0.8962 0.042 Uiso 1 1 calc R . . C14 C 0.2590(6) 1.1742(5) 1.0469(5) 0.0415(15) Uani 1 1 d . . . H14A H 0.2178 1.1048 1.0310 0.050 Uiso 1 1 calc R . . C15 C 0.3518(5) 1.8424(5) 1.1353(5) 0.0312(13) Uani 1 1 d . . . C16 C 0.3235(5) 1.7295(5) 1.0656(5) 0.0301(12) Uani 1 1 d . . . C17 C 0.4057(5) 1.6933(5) 1.0523(5) 0.0301(13) Uani 1 1 d . . . H17A H 0.4785 1.7419 1.0822 0.036 Uiso 1 1 calc R . . C18 C 0.3809(5) 1.5850(5) 0.9947(5) 0.0304(13) Uani 1 1 d . . . H18A H 0.4383 1.5607 0.9888 0.036 Uiso 1 1 calc R . . C19 C 0.2725(5) 1.5117(4) 0.9455(4) 0.0268(12) Uani 1 1 d . . . C20 C 0.1909(5) 1.5504(5) 0.9554(5) 0.0338(14) Uani 1 1 d . . . H20A H 0.1164 1.5030 0.9207 0.041 Uiso 1 1 calc R . . C21 C 0.2163(5) 1.6579(5) 1.0154(5) 0.0338(14) Uani 1 1 d . . . H21A H 0.1591 1.6822 1.0219 0.041 Uiso 1 1 calc R . . C22 C 0.4293(5) 1.1880(5) 0.5788(5) 0.0303(13) Uani 1 1 d . . . C23 C 0.3828(5) 1.2350(5) 0.6510(5) 0.0291(12) Uani 1 1 d . . . C24 C 0.3934(5) 1.3414(4) 0.6860(5) 0.0296(12) Uani 1 1 d . . . H24A H 0.4291 1.3853 0.6631 0.036 Uiso 1 1 calc R . . C25 C 0.3512(5) 1.3832(5) 0.7550(5) 0.0309(13) Uani 1 1 d . . . H25A H 0.3579 1.4555 0.7779 0.037 Uiso 1 1 calc R . . C26 C 0.2995(4) 1.3207(4) 0.7909(5) 0.0266(12) Uani 1 1 d . . . C27 C 0.2899(5) 1.2135(5) 0.7535(5) 0.0348(14) Uani 1 1 d . . . H27A H 0.2546 1.1689 0.7761 0.042 Uiso 1 1 calc R . . C28 C 0.3305(5) 1.1724(5) 0.6853(5) 0.0344(14) Uani 1 1 d . . . H28A H 0.3226 1.0998 0.6612 0.041 Uiso 1 1 calc R . . O1S O 0.4642(3) 1.0449(3) 0.3744(3) 0.0309(9) Uani 1 1 d . . . O41S O 0.2048(5) 1.0199(6) 0.3236(6) 0.0747(19) Uani 1 1 d . . . O51S O -0.0206(8) 1.3599(8) 0.4723(10) 0.162(2) Uani 1 1 d D . . N41S N 0.1129(6) 1.0977(7) 0.3951(6) 0.076(2) Uani 1 1 d . . . C41S C 0.1856(8) 1.0958(8) 0.3541(7) 0.069(2) Uani 1 1 d . . . H41A H 0.2207 1.1576 0.3508 0.082 Uiso 1 1 calc R . . C42S C 0.1013(10) 1.1982(8) 0.4305(9) 0.087(3) Uani 1 1 d . . . H42A H 0.1454 1.2462 0.4145 0.131 Uiso 1 1 calc R . . H42B H 0.1281 1.2271 0.5097 0.131 Uiso 1 1 calc R . . H42C H 0.0224 1.1905 0.3915 0.131 Uiso 1 1 calc R . . C43S C 0.0523(10) 1.0173(11) 0.4172(17) 0.162(8) Uani 1 1 d . . . H43A H 0.0027 1.0439 0.4418 0.243 Uiso 1 1 calc R . . H43B H 0.1066 1.0035 0.4745 0.243 Uiso 1 1 calc R . . H43C H 0.0080 0.9517 0.3498 0.243 Uiso 1 1 calc R . . N51S N -0.1325(6) 1.3942(6) 0.3407(8) 0.162(2) Uani 1 1 d D . . C53S C -0.2505(8) 1.4543(9) 0.3913(10) 0.162(2) Uani 1 1 d D . . H53A H -0.2424 1.5299 0.4205 0.194 Uiso 1 1 calc R . . H53B H -0.3291 1.4108 0.3618 0.194 Uiso 1 1 calc R . . C51S C -0.0983(7) 1.3909(6) 0.4379(8) 0.162(2) Uani 1 1 d D . . C52S C -0.1726(10) 1.4300(9) 0.4792(8) 0.162(2) Uani 1 1 d D . . H52A H -0.2148 1.3750 0.4908 0.194 Uiso 1 1 calc R . . H52B H -0.1281 1.4941 0.5495 0.194 Uiso 1 1 calc R . . C54S C -0.2171(8) 1.4281(8) 0.3039(8) 0.162(2) Uani 1 1 d D . . H54A H -0.2803 1.3725 0.2336 0.194 Uiso 1 1 calc R . . H54B H -0.1935 1.4915 0.2923 0.194 Uiso 1 1 calc R . . C55S C -0.0825(11) 1.3628(10) 0.2719(10) 0.162(2) Uani 1 1 d D . . H55A H -0.1211 1.3715 0.2042 0.243 Uiso 1 1 calc R . . H55B H -0.0891 1.2886 0.2535 0.243 Uiso 1 1 calc R . . H55C H -0.0033 1.4070 0.3115 0.243 Uiso 1 1 calc R . . C61S C -0.3330(7) 1.1049(5) 0.1693(9) 0.190(3) Uani 1 1 d D . . N61S N -0.2600(7) 1.0863(6) 0.1356(8) 0.190(3) Uani 1 1 d D . . C62S C -0.2942(10) 1.0929(9) 0.2749(9) 0.190(3) Uani 1 1 d D . . H62A H -0.3521 1.0359 0.2689 0.228 Uiso 1 1 calc R . . H62B H -0.2770 1.1595 0.3361 0.228 Uiso 1 1 calc R . . C63S C -0.1909(10) 1.0655(10) 0.2933(10) 0.190(3) Uani 1 1 d D . . H63A H -0.2006 0.9957 0.2959 0.228 Uiso 1 1 calc R . . H63B H -0.1254 1.1193 0.3630 0.228 Uiso 1 1 calc R . . C64S C -0.1758(8) 1.0632(8) 0.1971(10) 0.190(3) Uani 1 1 d D . . H64A H -0.1031 1.1159 0.2221 0.228 Uiso 1 1 calc R . . H64B H -0.1783 0.9924 0.1550 0.228 Uiso 1 1 calc R . . C65S C -0.2671(12) 1.0900(11) 0.0355(10) 0.190(3) Uani 1 1 d D . . H65A H -0.3327 1.1078 -0.0014 0.285 Uiso 1 1 calc R . . H65B H -0.2742 1.0208 -0.0133 0.285 Uiso 1 1 calc R . . H65C H -0.1994 1.1437 0.0535 0.285 Uiso 1 1 calc R . . O61S O -0.4165(11) 1.1276(8) 0.1202(11) 0.190(3) Uani 1 1 d D . . H1S H 0.481(5) 1.013(5) 0.317(6) 0.037(18) Uiso 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 Zn1 0.0269(5) 0.0234(5) 0.0268(5) 0.0107(4) 0.0152(4) 0.0125(4) Zn2 0.0379(4) 0.0542(5) 0.0391(4) 0.0304(4) 0.0260(4) 0.0301(4) Zn3 0.0503(5) 0.0238(4) 0.0535(5) 0.0098(3) 0.0363(4) 0.0108(3) Si1 0.0211(7) 0.0258(8) 0.0221(7) 0.0061(6) 0.0098(6) 0.0085(6) O1 0.027(2) 0.055(3) 0.036(2) 0.011(2) 0.013(2) 0.001(2) O2 0.024(2) 0.030(2) 0.043(2) 0.0084(19) 0.0114(19) 0.0041(17) O3 0.040(3) 0.047(3) 0.057(3) 0.035(3) 0.008(2) 0.013(2) O4 0.032(2) 0.042(3) 0.036(2) 0.020(2) 0.013(2) 0.0109(19) O5 0.033(2) 0.029(2) 0.036(2) 0.0053(18) 0.0178(19) 0.0055(18) O6 0.031(2) 0.031(2) 0.043(3) 0.0041(19) 0.021(2) 0.0038(18) O7 0.044(2) 0.030(2) 0.033(2) 0.0128(18) 0.024(2) 0.0197(19) O8 0.039(2) 0.036(2) 0.034(2) 0.0155(19) 0.0208(19) 0.0227(19) C1 0.029(3) 0.035(3) 0.030(3) 0.001(3) 0.016(3) 0.007(3) C2 0.037(3) 0.034(3) 0.040(4) 0.008(3) 0.024(3) 0.010(3) C3 0.024(3) 0.066(5) 0.032(3) 0.015(3) 0.012(3) 0.003(3) C4 0.029(3) 0.058(4) 0.030(3) 0.014(3) 0.016(3) 0.007(3) C5 0.022(3) 0.021(3) 0.025(3) 0.004(2) 0.010(2) 0.003(2) C6 0.033(3) 0.029(3) 0.025(3) 0.006(2) 0.014(2) 0.009(2) C7 0.033(3) 0.027(3) 0.034(3) 0.007(3) 0.022(3) 0.008(2) C8 0.026(3) 0.031(3) 0.037(3) 0.013(3) 0.014(3) 0.010(2) C9 0.032(3) 0.035(3) 0.024(3) 0.012(2) 0.015(2) 0.016(3) C10 0.033(3) 0.039(3) 0.033(3) 0.017(3) 0.016(3) 0.012(3) C11 0.025(3) 0.037(3) 0.027(3) 0.013(3) 0.011(2) 0.009(2) C12 0.032(3) 0.034(3) 0.034(3) 0.013(3) 0.019(3) 0.017(3) C13 0.034(3) 0.027(3) 0.026(3) 0.005(2) 0.004(3) 0.011(3) C14 0.047(4) 0.027(3) 0.038(4) 0.010(3) 0.013(3) 0.009(3) C15 0.031(3) 0.036(3) 0.032(3) 0.015(3) 0.020(3) 0.011(3) C16 0.028(3) 0.032(3) 0.026(3) 0.007(2) 0.014(2) 0.008(2) C17 0.021(3) 0.029(3) 0.028(3) 0.003(2) 0.010(2) 0.004(2) C18 0.024(3) 0.036(3) 0.025(3) 0.007(2) 0.011(2) 0.010(2) C19 0.027(3) 0.029(3) 0.024(3) 0.009(2) 0.013(2) 0.012(2) C20 0.020(3) 0.034(3) 0.036(3) 0.004(3) 0.013(2) 0.004(2) C21 0.027(3) 0.033(3) 0.041(3) 0.006(3) 0.024(3) 0.009(2) C22 0.028(3) 0.035(3) 0.023(3) 0.009(3) 0.008(2) 0.020(3) C23 0.028(3) 0.032(3) 0.025(3) 0.011(2) 0.009(2) 0.016(2) C24 0.033(3) 0.027(3) 0.033(3) 0.010(2) 0.021(3) 0.014(2) C25 0.030(3) 0.030(3) 0.029(3) 0.010(2) 0.012(3) 0.013(2) C26 0.022(3) 0.031(3) 0.026(3) 0.010(2) 0.012(2) 0.010(2) C27 0.034(3) 0.036(3) 0.034(3) 0.008(3) 0.019(3) 0.015(3) C28 0.043(3) 0.032(3) 0.031(3) 0.007(3) 0.021(3) 0.019(3) O1S 0.037(2) 0.036(2) 0.034(2) 0.0187(19) 0.0234(19) 0.0221(19) O41S 0.079(4) 0.122(6) 0.090(5) 0.069(4) 0.065(4) 0.076(4) O51S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) N41S 0.056(4) 0.083(6) 0.066(5) -0.006(4) 0.037(4) 0.026(4) C41S 0.069(6) 0.058(5) 0.055(5) 0.014(4) 0.020(4) 0.015(5) C42S 0.100(8) 0.065(6) 0.081(7) 0.015(5) 0.046(6) 0.019(6) C43S 0.074(8) 0.097(10) 0.33(3) 0.113(14) 0.097(13) 0.031(7) N51S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C53S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C51S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C52S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C54S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C55S 0.167(6) 0.169(6) 0.191(6) 0.101(5) 0.092(5) 0.090(5) C61S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) N61S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) C62S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) C63S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) C64S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) C65S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) O61S 0.176(7) 0.176(6) 0.188(7) 0.098(6) 0.049(6) 0.053(5) _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 Zn1 O1S 2.037(4) . ? Zn1 O1S 2.037(4) 2_676 ? Zn1 O8 2.044(4) . ? Zn1 O8 2.044(4) 2_676 ? Zn1 O2 2.170(4) 1_655 ? Zn1 O2 2.170(4) 2_576 ? Zn2 O1 1.939(4) 1_655 ? Zn2 O7 1.946(4) . ? Zn2 O4 1.960(4) 1_554 ? Zn2 O1S 2.007(4) . ? Zn3 O5 1.919(4) 1_544 ? Zn3 O41S 1.925(5) . ? Zn3 O1S 1.989(4) . ? Zn3 O3 1.988(5) 1_554 ? Si1 C19 1.865(6) . ? Si1 C5 1.873(5) . ? Si1 C26 1.874(6) . ? Si1 C12 1.884(6) . ? O1 C1 1.289(8) . ? O1 Zn2 1.939(4) 1_455 ? O2 C1 1.248(7) . ? O2 Zn1 2.170(4) 1_455 ? O3 C8 1.260(7) . ? O3 Zn3 1.988(5) 1_556 ? O4 C8 1.241(7) . ? O4 Zn2 1.960(4) 1_556 ? O5 C15 1.300(7) . ? O5 Zn3 1.919(4) 1_566 ? O6 C15 1.247(7) . ? O7 C22 1.254(7) . ? O8 C22 1.258(7) . ? C1 C2 1.486(9) . ? C2 C7 1.400(9) . ? C2 C3 1.406(9) . ? C3 C4 1.393(9) . ? C3 H3A 0.9500 . ? C4 C5 1.385(8) . ? C4 H4A 0.9500 . ? C5 C6 1.420(8) . ? C6 C7 1.373(8) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.511(8) . ? C9 C14 1.385(9) . ? C9 C10 1.397(9) . ? C10 C11 1.383(8) . ? C10 H10A 0.9500 . ? C11 C12 1.403(8) . ? C11 H11A 0.9500 . ? C12 C13 1.389(9) . ? C13 C14 1.381(9) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.485(8) . ? C16 C21 1.384(8) . ? C16 C17 1.394(8) . ? C17 C18 1.403(8) . ? C17 H17A 0.9500 . ? C18 C19 1.407(8) . ? C18 H18A 0.9500 . ? C19 C20 1.388(8) . ? C20 C21 1.399(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.502(8) . ? C23 C28 1.384(9) . ? C23 C24 1.395(8) . ? C24 C25 1.397(8) . ? C24 H24A 0.9500 . ? C25 C26 1.396(8) . ? C25 H25A 0.9500 . ? C26 C27 1.409(8) . ? C27 C28 1.369(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? O1S H1S 0.96(7) . ? O41S C41S 1.156(10) . ? O51S C51S 1.221(12) . ? N41S C41S 1.371(12) . ? N41S C42S 1.422(12) . ? N41S C43S 1.492(14) . ? C41S H41A 0.9500 . ? C42S H42A 0.9800 . ? C42S H42B 0.9800 . ? C42S H42C 0.9800 . ? C43S H43A 0.9800 . ? C43S H43B 0.9800 . ? C43S H43C 0.9800 . ? N51S C54S 1.328(2) . ? N51S C51S 1.329(2) . ? N51S C55S 1.450(2) . ? C53S C52S 1.498(2) . ? C53S C54S 1.499(2) . ? C53S H53A 0.9900 . ? C53S H53B 0.9900 . ? C51S C52S 1.499(2) . ? C52S H52A 0.9900 . ? C52S H52B 0.9900 . ? C54S H54A 0.9900 . ? C54S H54B 0.9900 . ? C55S H55A 0.9800 . ? C55S H55B 0.9800 . ? C55S H55C 0.9800 . ? C61S O61S 1.257(14) . ? C61S N61S 1.329(2) . ? C61S C62S 1.498(2) . ? N61S C64S 1.330(2) . ? N61S C65S 1.450(2) . ? C62S C63S 1.499(2) . ? C62S H62A 0.9900 . ? C62S H62B 0.9900 . ? C63S C64S 1.500(2) . ? C63S H63A 0.9900 . ? C63S H63B 0.9900 . ? C64S H64A 0.9900 . ? C64S H64B 0.9900 . ? C65S H65A 0.9800 . ? C65S H65B 0.9800 . ? C65S H65C 0.9800 . ? 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 O1S Zn1 O1S 179.999(1) . 2_676 ? O1S Zn1 O8 91.00(16) . . ? O1S Zn1 O8 89.00(16) 2_676 . ? O1S Zn1 O8 89.00(16) . 2_676 ? O1S Zn1 O8 91.00(16) 2_676 2_676 ? O8 Zn1 O8 179.999(1) . 2_676 ? O1S Zn1 O2 93.64(17) . 1_655 ? O1S Zn1 O2 86.36(17) 2_676 1_655 ? O8 Zn1 O2 91.79(17) . 1_655 ? O8 Zn1 O2 88.21(17) 2_676 1_655 ? O1S Zn1 O2 86.36(17) . 2_576 ? O1S Zn1 O2 93.64(17) 2_676 2_576 ? O8 Zn1 O2 88.21(17) . 2_576 ? O8 Zn1 O2 91.79(17) 2_676 2_576 ? O2 Zn1 O2 180.000(1) 1_655 2_576 ? O1 Zn2 O7 116.86(18) 1_655 . ? O1 Zn2 O4 116.71(19) 1_655 1_554 ? O7 Zn2 O4 113.50(18) . 1_554 ? O1 Zn2 O1S 98.26(19) 1_655 . ? O7 Zn2 O1S 102.89(17) . . ? O4 Zn2 O1S 105.40(18) 1_554 . ? O5 Zn3 O41S 122.9(3) 1_544 . ? O5 Zn3 O1S 107.33(18) 1_544 . ? O41S Zn3 O1S 115.5(2) . . ? O5 Zn3 O3 109.9(2) 1_544 1_554 ? O41S Zn3 O3 100.2(3) . 1_554 ? O1S Zn3 O3 97.49(18) . 1_554 ? C19 Si1 C5 108.3(2) . . ? C19 Si1 C26 114.5(3) . . ? C5 Si1 C26 107.3(2) . . ? C19 Si1 C12 109.7(3) . . ? C5 Si1 C12 108.8(3) . . ? C26 Si1 C12 108.0(3) . . ? C1 O1 Zn2 118.9(4) . 1_455 ? C1 O2 Zn1 132.6(4) . 1_455 ? C8 O3 Zn3 139.0(4) . 1_556 ? C8 O4 Zn2 123.9(4) . 1_556 ? C15 O5 Zn3 118.9(4) . 1_566 ? C22 O7 Zn2 126.8(4) . . ? C22 O8 Zn1 134.8(4) . . ? O2 C1 O1 125.9(6) . . ? O2 C1 C2 118.8(6) . . ? O1 C1 C2 115.3(6) . . ? C7 C2 C3 118.2(6) . . ? C7 C2 C1 120.9(5) . . ? C3 C2 C1 120.9(6) . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 121.2(6) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 118.2(5) . . ? C4 C5 Si1 119.2(4) . . ? C6 C5 Si1 122.3(4) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 121.4(6) . . ? C6 C7 H7A 119.3 . . ? C2 C7 H7A 119.3 . . ? O4 C8 O3 126.1(6) . . ? O4 C8 C9 118.3(5) . . ? O3 C8 C9 115.6(5) . . ? C14 C9 C10 120.0(6) . . ? C14 C9 C8 119.1(6) . . ? C10 C9 C8 120.9(5) . . ? C11 C10 C9 118.9(6) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 122.1(6) . . ? C10 C11 H11A 119.0 . . ? C12 C11 H11A 119.0 . . ? C13 C12 C11 117.3(6) . . ? C13 C12 Si1 120.8(5) . . ? C11 C12 Si1 121.9(5) . . ? C14 C13 C12 121.6(6) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C9 120.0(6) . . ? C13 C14 H14A 120.0 . . ? C9 C14 H14A 120.0 . . ? O6 C15 O5 125.1(6) . . ? O6 C15 C16 120.6(5) . . ? O5 C15 C16 114.3(5) . . ? C21 C16 C17 118.8(5) . . ? C21 C16 C15 120.8(5) . . ? C17 C16 C15 120.3(5) . . ? C16 C17 C18 120.0(5) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 121.3(5) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C20 C19 C18 117.6(5) . . ? C20 C19 Si1 118.3(4) . . ? C18 C19 Si1 123.8(4) . . ? C19 C20 C21 121.1(5) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C16 C21 C20 121.1(5) . . ? C16 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? O7 C22 O8 126.2(5) . . ? O7 C22 C23 117.8(5) . . ? O8 C22 C23 116.0(5) . . ? C28 C23 C24 119.3(5) . . ? C28 C23 C22 119.5(5) . . ? C24 C23 C22 121.2(5) . . ? C23 C24 C25 119.7(6) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C26 C25 C24 121.3(5) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C27 117.4(5) . . ? C25 C26 Si1 125.6(4) . . ? C27 C26 Si1 117.0(4) . . ? C28 C27 C26 121.3(6) . . ? C28 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? C27 C28 C23 120.9(6) . . ? C27 C28 H28A 119.5 . . ? C23 C28 H28A 119.5 . . ? Zn3 O1S Zn2 110.02(18) . . ? Zn3 O1S Zn1 116.1(2) . . ? Zn2 O1S Zn1 106.57(19) . . ? Zn3 O1S H1S 90(4) . . ? Zn2 O1S H1S 113(4) . . ? Zn1 O1S H1S 120(4) . . ? C41S O41S Zn3 129.3(8) . . ? C41S N41S C42S 112.8(9) . . ? C41S N41S C43S 131.8(9) . . ? C42S N41S C43S 115.2(9) . . ? O41S C41S N41S 120.7(9) . . ? O41S C41S H41A 119.7 . . ? N41S C41S H41A 119.7 . . ? N41S C42S H42A 109.5 . . ? N41S C42S H42B 109.5 . . ? H42A C42S H42B 109.5 . . ? N41S C42S H42C 109.5 . . ? H42A C42S H42C 109.5 . . ? H42B C42S H42C 109.5 . . ? N41S C43S H43A 109.5 . . ? N41S C43S H43B 109.5 . . ? H43A C43S H43B 109.5 . . ? N41S C43S H43C 109.5 . . ? H43A C43S H43C 109.5 . . ? H43B C43S H43C 109.5 . . ? C54S N51S C51S 118.6(5) . . ? C54S N51S C55S 117.8(6) . . ? C51S N51S C55S 123.6(3) . . ? C52S C53S C54S 105.23(18) . . ? C52S C53S H53A 110.7 . . ? C54S C53S H53A 110.7 . . ? C52S C53S H53B 110.7 . . ? C54S C53S H53B 110.7 . . ? H53A C53S H53B 108.8 . . ? O51S C51S N51S 118.9(10) . . ? O51S C51S C52S 135.5(10) . . ? N51S C51S C52S 105.5(4) . . ? C53S C52S C51S 105.19(18) . . ? C53S C52S H52A 110.7 . . ? C51S C52S H52A 110.7 . . ? C53S C52S H52B 110.7 . . ? C51S C52S H52B 110.7 . . ? H52A C52S H52B 108.8 . . ? N51S C54S C53S 105.5(4) . . ? N51S C54S H54A 110.6 . . ? C53S C54S H54A 110.6 . . ? N51S C54S H54B 110.6 . . ? C53S C54S H54B 110.6 . . ? H54A C54S H54B 108.8 . . ? N51S C55S H55A 109.5 . . ? N51S C55S H55B 109.5 . . ? H55A C55S H55B 109.5 . . ? N51S C55S H55C 109.5 . . ? H55A C55S H55C 109.5 . . ? H55B C55S H55C 109.5 . . ? O61S C61S N61S 125.6(11) . . ? O61S C61S C62S 128.6(11) . . ? N61S C61S C62S 105.7(4) . . ? C61S N61S C64S 118.3(5) . . ? C61S N61S C65S 123.6(3) . . ? C64S N61S C65S 118.1(6) . . ? C61S C62S C63S 105.18(19) . . ? C61S C62S H62A 110.7 . . ? C63S C62S H62A 110.7 . . ? C61S C62S H62B 110.7 . . ? C63S C62S H62B 110.7 . . ? H62A C62S H62B 108.8 . . ? C62S C63S C64S 105.12(18) . . ? C62S C63S H63A 110.7 . . ? C64S C63S H63A 110.7 . . ? C62S C63S H63B 110.7 . . ? C64S C63S H63B 110.7 . . ? H63A C63S H63B 108.8 . . ? N61S C64S C63S 105.7(4) . . ? N61S C64S H64A 110.6 . . ? C63S C64S H64A 110.6 . . ? N61S C64S H64B 110.6 . . ? C63S C64S H64B 110.6 . . ? H64A C64S H64B 108.7 . . ? N61S C65S H65A 109.5 . . ? N61S C65S H65B 109.5 . . ? H65A C65S H65B 109.5 . . ? N61S C65S H65C 109.5 . . ? H65A C65S H65C 109.5 . . ? H65B C65S H65C 109.5 . . ? 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 O1 Zn2 O7 C22 -83.0(5) 1_655 . . . ? O4 Zn2 O7 C22 136.7(5) 1_554 . . . ? O1S Zn2 O7 C22 23.3(5) . . . . ? O1S Zn1 O8 C22 -44.0(5) . . . . ? O1S Zn1 O8 C22 136.0(5) 2_676 . . . ? O8 Zn1 O8 C22 -113(67) 2_676 . . . ? O2 Zn1 O8 C22 49.6(5) 1_655 . . . ? O2 Zn1 O8 C22 -130.4(5) 2_576 . . . ? Zn1 O2 C1 O1 28.7(9) 1_455 . . . ? Zn1 O2 C1 C2 -152.6(4) 1_455 . . . ? Zn2 O1 C1 O2 14.4(8) 1_455 . . . ? Zn2 O1 C1 C2 -164.3(4) 1_455 . . . ? O2 C1 C2 C7 -30.6(9) . . . . ? O1 C1 C2 C7 148.2(6) . . . . ? O2 C1 C2 C3 150.4(6) . . . . ? O1 C1 C2 C3 -30.8(9) . . . . ? C7 C2 C3 C4 -0.5(11) . . . . ? C1 C2 C3 C4 178.5(7) . . . . ? C2 C3 C4 C5 0.8(11) . . . . ? C3 C4 C5 C6 -2.4(10) . . . . ? C3 C4 C5 Si1 -175.9(6) . . . . ? C19 Si1 C5 C4 88.4(5) . . . . ? C26 Si1 C5 C4 -35.7(6) . . . . ? C12 Si1 C5 C4 -152.3(5) . . . . ? C19 Si1 C5 C6 -84.8(5) . . . . ? C26 Si1 C5 C6 151.1(5) . . . . ? C12 Si1 C5 C6 34.4(6) . . . . ? C4 C5 C6 C7 3.9(9) . . . . ? Si1 C5 C6 C7 177.2(4) . . . . ? C5 C6 C7 C2 -3.8(9) . . . . ? C3 C2 C7 C6 2.1(10) . . . . ? C1 C2 C7 C6 -176.9(6) . . . . ? Zn2 O4 C8 O3 0.5(9) 1_556 . . . ? Zn2 O4 C8 C9 177.5(4) 1_556 . . . ? Zn3 O3 C8 O4 -18.7(12) 1_556 . . . ? Zn3 O3 C8 C9 164.2(5) 1_556 . . . ? O4 C8 C9 C14 169.6(6) . . . . ? O3 C8 C9 C14 -13.0(8) . . . . ? O4 C8 C9 C10 -12.8(9) . . . . ? O3 C8 C9 C10 164.5(6) . . . . ? C14 C9 C10 C11 0.8(9) . . . . ? C8 C9 C10 C11 -176.8(5) . . . . ? C9 C10 C11 C12 -2.7(9) . . . . ? C10 C11 C12 C13 1.7(9) . . . . ? C10 C11 C12 Si1 -177.7(5) . . . . ? C19 Si1 C12 C13 152.3(5) . . . . ? C5 Si1 C12 C13 34.0(6) . . . . ? C26 Si1 C12 C13 -82.2(5) . . . . ? C19 Si1 C12 C11 -28.3(5) . . . . ? C5 Si1 C12 C11 -146.6(5) . . . . ? C26 Si1 C12 C11 97.2(5) . . . . ? C11 C12 C13 C14 1.2(9) . . . . ? Si1 C12 C13 C14 -179.3(5) . . . . ? C12 C13 C14 C9 -3.1(10) . . . . ? C10 C9 C14 C13 2.1(10) . . . . ? C8 C9 C14 C13 179.7(6) . . . . ? Zn3 O5 C15 O6 -13.7(8) 1_566 . . . ? Zn3 O5 C15 C16 164.5(4) 1_566 . . . ? O6 C15 C16 C21 -177.9(6) . . . . ? O5 C15 C16 C21 3.8(8) . . . . ? O6 C15 C16 C17 4.0(9) . . . . ? O5 C15 C16 C17 -174.3(5) . . . . ? C21 C16 C17 C18 -4.0(9) . . . . ? C15 C16 C17 C18 174.1(5) . . . . ? C16 C17 C18 C19 2.8(9) . . . . ? C17 C18 C19 C20 0.4(8) . . . . ? C17 C18 C19 Si1 -173.6(4) . . . . ? C5 Si1 C19 C20 22.7(5) . . . . ? C26 Si1 C19 C20 142.4(5) . . . . ? C12 Si1 C19 C20 -96.0(5) . . . . ? C5 Si1 C19 C18 -163.4(5) . . . . ? C26 Si1 C19 C18 -43.7(6) . . . . ? C12 Si1 C19 C18 77.9(5) . . . . ? C18 C19 C20 C21 -2.2(9) . . . . ? Si1 C19 C20 C21 172.1(5) . . . . ? C17 C16 C21 C20 2.2(9) . . . . ? C15 C16 C21 C20 -175.9(6) . . . . ? C19 C20 C21 C16 1.0(10) . . . . ? Zn2 O7 C22 O8 -0.6(8) . . . . ? Zn2 O7 C22 C23 -179.6(4) . . . . ? Zn1 O8 C22 O7 14.4(9) . . . . ? Zn1 O8 C22 C23 -166.5(4) . . . . ? O7 C22 C23 C28 172.4(5) . . . . ? O8 C22 C23 C28 -6.8(8) . . . . ? O7 C22 C23 C24 -9.0(8) . . . . ? O8 C22 C23 C24 171.9(5) . . . . ? C28 C23 C24 C25 0.0(9) . . . . ? C22 C23 C24 C25 -178.7(5) . . . . ? C23 C24 C25 C26 0.7(9) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C24 C25 C26 Si1 -178.2(4) . . . . ? C19 Si1 C26 C25 -12.5(6) . . . . ? C5 Si1 C26 C25 107.7(5) . . . . ? C12 Si1 C26 C25 -135.1(5) . . . . ? C19 Si1 C26 C27 170.1(4) . . . . ? C5 Si1 C26 C27 -69.6(5) . . . . ? C12 Si1 C26 C27 47.6(5) . . . . ? C25 C26 C27 C28 0.5(9) . . . . ? Si1 C26 C27 C28 178.0(5) . . . . ? C26 C27 C28 C23 0.2(9) . . . . ? C24 C23 C28 C27 -0.4(9) . . . . ? C22 C23 C28 C27 178.2(5) . . . . ? O5 Zn3 O1S Zn2 146.8(2) 1_544 . . . ? O41S Zn3 O1S Zn2 -72.0(3) . . . . ? O3 Zn3 O1S Zn2 33.2(2) 1_554 . . . ? O5 Zn3 O1S Zn1 -92.1(2) 1_544 . . . ? O41S Zn3 O1S Zn1 49.1(3) . . . . ? O3 Zn3 O1S Zn1 154.3(2) 1_554 . . . ? O1 Zn2 O1S Zn3 -166.4(2) 1_655 . . . ? O7 Zn2 O1S Zn3 73.5(2) . . . . ? O4 Zn2 O1S Zn3 -45.7(2) 1_554 . . . ? O1 Zn2 O1S Zn1 66.9(2) 1_655 . . . ? O7 Zn2 O1S Zn1 -53.2(2) . . . . ? O4 Zn2 O1S Zn1 -172.35(17) 1_554 . . . ? O1S Zn1 O1S Zn3 134(27) 2_676 . . . ? O8 Zn1 O1S Zn3 -68.5(2) . . . . ? O8 Zn1 O1S Zn3 111.5(2) 2_676 . . . ? O2 Zn1 O1S Zn3 -160.3(2) 1_655 . . . ? O2 Zn1 O1S Zn3 19.7(2) 2_576 . . . ? O1S Zn1 O1S Zn2 -103(27) 2_676 . . . ? O8 Zn1 O1S Zn2 54.45(19) . . . . ? O8 Zn1 O1S Zn2 -125.55(19) 2_676 . . . ? O2 Zn1 O1S Zn2 -37.40(19) 1_655 . . . ? O2 Zn1 O1S Zn2 142.60(19) 2_576 . . . ? O5 Zn3 O41S C41S -144.0(8) 1_544 . . . ? O1S Zn3 O41S C41S 81.4(8) . . . . ? O3 Zn3 O41S C41S -22.1(9) 1_554 . . . ? Zn3 O41S C41S N41S -179.4(6) . . . . ? C42S N41S C41S O41S 178.9(9) . . . . ? C43S N41S C41S O41S 4.7(17) . . . . ? C54S N51S C51S O51S 180.00(4) . . . . ? C55S N51S C51S O51S 0.00(4) . . . . ? C54S N51S C51S C52S 0.00(5) . . . . ? C55S N51S C51S C52S 180.00(4) . . . . ? C54S C53S C52S C51S -0.1(13) . . . . ? O51S C51S C52S C53S 180.00(3) . . . . ? N51S C51S C52S C53S 0.00(5) . . . . ? C51S N51S C54S C53S -0.01(6) . . . . ? C55S N51S C54S C53S 180.00(5) . . . . ? C52S C53S C54S N51S 0.1(13) . . . . ? O61S C61S N61S C64S 180.00(4) . . . . ? C62S C61S N61S C64S 0.00(5) . . . . ? O61S C61S N61S C65S 0.1(18) . . . . ? C62S C61S N61S C65S -179.9(11) . . . . ? O61S C61S C62S C63S 180.00(3) . . . . ? N61S C61S C62S C63S -0.01(6) . . . . ? C61S C62S C63S C64S 0.01(7) . . . . ? C61S N61S C64S C63S 0.00(6) . . . . ? C65S N61S C64S C63S 179.9(11) . . . . ? C62S C63S C64S N61S -0.01(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.606 _refine_diff_density_min -1.566 _refine_diff_density_rms 0.141 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.009 -0.004 3708.2 1027.6 _platon_squeeze_details ; ; _vrf_PLAT097_I ; PROBLEM: Large Reported Max. (Positive) Residual Density 2.61 eA-3 RESPONSE: The most significant residual electron density (2.61eA-3) in the structure is located at (0.65, 1.39, 0.54), near Zn2 coordinate (0.53, 1.20, 0.44). It is more possible to be assigned as solvent oxygen instead of carbon, nitrogen, or hydrogen on account of chemical sense. However, there are two reasons we left this high Q-peak there. One is due to its enormous thermal ellipsoids (0.99). It indicates too many electrons are assigned on the position, inferring the occupancy of this atom should be lower. The other reason is due to the distortion of five-membered coordinated form constructed with O1, O4, O7, Zn2 and this Q-peak. Based on the structure deposition in CCDC, five-membered coordinated form of Zn prefers square pyramid rather than trigonal bipyramid. Even compared with trigonal bipyramid form, the plane constructed with O1, O4, O7, Zn2 looks more distorted. Therefore, we decide to propose a structure without partially coordinated oxygen and leave this high Q-peak. ; _database_code_depnum_ccdc_archive 'CCDC 942373' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cd3 (C28 H16 O8 Si)2] [Cd (C5H9NO)2 (C4H9NO)2 (H2O)2] (C4H9NO)2' _chemical_formula_sum 'C82 H90 Cd4 N6 O24 Si2' _chemical_formula_weight 2049.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9817(19) _cell_length_b 14.1817(19) _cell_length_c 14.270(3) _cell_angle_alpha 115.922(2) _cell_angle_beta 113.196(2) _cell_angle_gamma 97.1440(10) _cell_volume 2183.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.6224 _cell_measurement_theta_max 29.1589 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7407 _exptl_absorpt_correction_T_max 0.8153 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22910 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8546 _reflns_number_gt 8180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0300P)^2^+8.8000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8546 _refine_ls_number_parameters 542 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _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 0.504891(17) 0.384270(17) 0.185287(18) 0.01239(6) Uani 1 1 d . . . Cd2 Cd 0.5000 0.5000 0.0000 0.01117(7) Uani 1 2 d S . . Cd3 Cd 1.0000 0.5000 0.5000 0.01789(8) Uani 1 2 d S . . Si1 Si 0.76388(6) 0.14398(7) -0.32130(7) 0.01205(16) Uani 1 1 d . . . O2 O 0.57825(17) 0.39172(17) 0.06922(18) 0.0155(4) Uani 1 1 d . . . O1 O 0.5167(2) 0.21903(19) 0.0284(2) 0.0231(5) Uani 1 1 d . . . O8 O 0.5650(2) -0.43483(19) -0.6786(2) 0.0254(5) Uani 1 1 d . . . O10S O 0.84655(19) 0.3737(2) 0.3196(2) 0.0239(5) Uani 1 1 d D . . O1S O 1.0011(2) 0.6474(2) 0.4720(2) 0.0258(5) Uani 1 1 d . . . O3 O 1.32815(19) 0.4030(2) -0.0464(2) 0.0267(5) Uani 1 1 d . . . C5 C 0.7069(2) 0.1802(2) -0.2163(3) 0.0143(6) Uani 1 1 d . . . C12 C 0.9205(2) 0.2009(3) -0.2312(3) 0.0148(6) Uani 1 1 d . . . O5 O 0.64816(19) 0.3521(2) -0.6918(2) 0.0228(5) Uani 1 1 d . . . C15 C 0.5864(3) 0.3199(3) -0.6583(3) 0.0174(6) Uani 1 1 d . . . O4 O 1.32623(18) 0.3209(2) 0.0571(2) 0.0220(5) Uani 1 1 d . . . O13 O 1.1154(2) 0.4478(2) 0.4265(2) 0.0270(5) Uani 1 1 d . . . C2 C 0.6182(2) 0.2500(3) -0.0625(3) 0.0153(6) Uani 1 1 d . . . C19 C 0.7173(2) 0.2116(2) -0.4098(3) 0.0151(6) Uani 1 1 d . . . O6 O 0.48809(18) 0.3184(2) -0.6958(2) 0.0213(5) Uani 1 1 d . . . C23 C 0.6196(2) -0.2419(3) -0.6116(3) 0.0165(6) Uani 1 1 d . . . C1 C 0.5666(2) 0.2872(3) 0.0156(3) 0.0166(6) Uani 1 1 d . . . C24 C 0.6760(3) -0.2057(3) -0.4900(3) 0.0168(6) Uani 1 1 d . . . H19 H 0.6844 -0.2590 -0.4669 0.020 Uiso 1 1 calc R . . C25 C 0.7202(2) -0.0916(3) -0.4023(3) 0.0163(6) Uani 1 1 d . . . H20 H 0.7592 -0.0678 -0.3197 0.020 Uiso 1 1 calc R . . C7 C 0.5951(3) 0.1362(3) -0.1368(3) 0.0186(6) Uani 1 1 d . . . H21 H 0.5501 0.0821 -0.1347 0.022 Uiso 1 1 calc R . . C26 C 0.7082(2) -0.0111(2) -0.4336(3) 0.0143(6) Uani 1 1 d . . . C10 C 1.0945(3) 0.3570(3) -0.1230(3) 0.0202(6) Uani 1 1 d . . . H23 H 1.1321 0.4313 -0.0983 0.024 Uiso 1 1 calc R . . N2S N 1.1997(3) 0.4255(2) 0.3140(3) 0.0300(7) Uani 1 1 d D . . C20 C 0.6111(3) 0.2191(3) -0.4471(3) 0.0218(7) Uani 1 1 d . . . H25 H 0.5669 0.1998 -0.4174 0.026 Uiso 1 1 calc R . . C14 C 1.0989(3) 0.1850(3) -0.1320(3) 0.0214(7) Uani 1 1 d . . . H26 H 1.1395 0.1421 -0.1102 0.026 Uiso 1 1 calc R . . C6 C 0.6379(3) 0.1017(3) -0.2144(3) 0.0178(6) Uani 1 1 d . . . H27 H 0.6198 0.0238 -0.2667 0.021 Uiso 1 1 calc R . . O7 O 0.5386(2) -0.3862(2) -0.8136(2) 0.0325(6) Uani 1 1 d . . . C17 C 0.7391(3) 0.2779(3) -0.5336(3) 0.0186(6) Uani 1 1 d . . . H29 H 0.7837 0.2987 -0.5622 0.022 Uiso 1 1 calc R . . C8 C 1.2813(2) 0.3440(3) -0.0217(3) 0.0177(6) Uani 1 1 d . . . C28 C 0.6082(3) -0.1634(3) -0.6442(3) 0.0200(6) Uani 1 1 d . . . H31 H 0.5706 -0.1875 -0.7270 0.024 Uiso 1 1 calc R . . C22 C 0.5700(3) -0.3645(3) -0.7094(3) 0.0192(6) Uani 1 1 d . . . C1S C 0.9289(3) 0.6787(3) 0.4210(3) 0.0233(7) Uani 1 1 d . . . C9 C 1.1556(2) 0.2940(3) -0.0938(3) 0.0168(6) Uani 1 1 d . . . C27 C 0.6514(3) -0.0499(3) -0.5567(3) 0.0188(6) Uani 1 1 d . . . H35 H 0.6423 0.0027 -0.5806 0.023 Uiso 1 1 calc R . . C13 C 0.9832(3) 0.1382(3) -0.2022(3) 0.0205(6) Uani 1 1 d . . . H37 H 0.9461 0.0624 -0.2309 0.025 Uiso 1 1 calc R . . C16 C 0.6326(3) 0.2831(3) -0.5713(3) 0.0174(6) Uani 1 1 d . . . C5S C 1.1163(3) 0.4382(2) 0.3358(3) 0.0249(7) Uani 1 1 d D . . C21 C 0.5694(3) 0.2542(3) -0.5267(3) 0.0235(7) Uani 1 1 d . . . H40 H 0.4972 0.2586 -0.5509 0.028 Uiso 1 1 calc R . . C3 C 0.6869(3) 0.3292(3) -0.0627(3) 0.0198(6) Uani 1 1 d . . . H41 H 0.7034 0.4069 -0.0115 0.024 Uiso 1 1 calc R . . N1S N 0.9498(3) 0.7888(3) 0.4659(3) 0.0290(7) Uani 1 1 d . . . C4 C 0.7315(3) 0.2945(3) -0.1381(3) 0.0211(7) Uani 1 1 d . . . H43 H 0.7797 0.3493 -0.1366 0.025 Uiso 1 1 calc R . . C9S C 1.3035(3) 0.4264(3) 0.3942(4) 0.0354(9) Uani 1 1 d . . . H44A H 1.3012 0.4335 0.4647 0.053 Uiso 1 1 calc R . . H44B H 1.3654 0.4902 0.4204 0.053 Uiso 1 1 calc R . . H44C H 1.3143 0.3563 0.3519 0.053 Uiso 1 1 calc R . . C2S C 0.8189(3) 0.5941(3) 0.3121(3) 0.0306(8) Uani 1 1 d . . . H47A H 0.8273 0.5220 0.2716 0.046 Uiso 1 1 calc R . . H47B H 0.7933 0.6204 0.2567 0.046 Uiso 1 1 calc R . . H47C H 0.7640 0.5846 0.3369 0.046 Uiso 1 1 calc R . . C6S C 1.0224(3) 0.4326(3) 0.2314(3) 0.0330(8) Uani 1 1 d D . . H48A H 1.0074 0.5035 0.2579 0.040 Uiso 1 1 calc R . . H48B H 0.9533 0.3696 0.1940 0.040 Uiso 1 1 calc R . . C18 C 0.7801(3) 0.2423(3) -0.4545(3) 0.0183(6) Uani 1 1 d . . . H52 H 0.8526 0.2387 -0.4299 0.022 Uiso 1 1 calc R . . C3S C 1.0510(4) 0.8712(3) 0.5804(4) 0.0417(10) Uani 1 1 d . . . H53A H 1.0841 0.8341 0.6219 0.063 Uiso 1 1 calc R . . H53B H 1.0323 0.9301 0.6309 0.063 Uiso 1 1 calc R . . H53C H 1.1043 0.9049 0.5653 0.063 Uiso 1 1 calc R . . C11 C 0.9791(3) 0.3117(3) -0.1880(3) 0.0187(6) Uani 1 1 d . . . H54 H 0.9386 0.3571 -0.2037 0.022 Uiso 1 1 calc R . . C4S C 0.8797(4) 0.8363(4) 0.4072(4) 0.0374(9) Uani 1 1 d . . . H55A H 0.8130 0.7755 0.3327 0.056 Uiso 1 1 calc R . . H55B H 0.9214 0.8789 0.3882 0.056 Uiso 1 1 calc R . . H55C H 0.8575 0.8863 0.4613 0.056 Uiso 1 1 calc R . . C7S C 1.0647(4) 0.4144(4) 0.1441(4) 0.0580(14) Uani 1 1 d D . . H57A H 1.0143 0.3430 0.0661 0.070 Uiso 1 1 calc R . . H57B H 1.0679 0.4765 0.1296 0.070 Uiso 1 1 calc R . . C8S C 1.1771(4) 0.4104(3) 0.1990(4) 0.0529(12) Uani 1 1 d D . . H58A H 1.1793 0.3373 0.1469 0.064 Uiso 1 1 calc R . . H58B H 1.2330 0.4711 0.2109 0.064 Uiso 1 1 calc R . . H15 H 0.839(4) 0.2980(13) 0.269(4) 0.072(18) Uiso 1 1 d D . . H17 H 0.7732(19) 0.355(3) 0.309(5) 0.081(19) Uiso 1 1 d D . . O11S O 0.8724(7) 0.1920(6) 0.1700(7) 0.0340(12) Uani 0.477(9) 1 d P A 1 N11S N 0.7203(6) 0.0278(5) 0.0513(6) 0.0340(12) Uani 0.477(9) 1 d PD A 1 C11S C 0.8195(7) 0.0955(7) 0.0812(7) 0.0340(12) Uani 0.477(9) 1 d PD A 1 C12S C 0.8398(8) 0.0313(8) -0.0213(7) 0.0340(12) Uani 0.477(9) 1 d PD A 1 H12A H 0.9106 0.0756 -0.0047 0.051 Uiso 0.477(9) 1 calc PR A 1 H12B H 0.7790 0.0171 -0.0963 0.051 Uiso 0.477(9) 1 calc PR A 1 H12C H 0.8431 -0.0403 -0.0295 0.051 Uiso 0.477(9) 1 calc PR A 1 C13S C 0.6660(14) 0.0600(12) 0.1177(15) 0.0340(12) Uani 0.477(9) 1 d PD A 1 H13A H 0.7160 0.1309 0.1947 0.051 Uiso 0.477(9) 1 calc PR A 1 H13B H 0.6453 0.0017 0.1329 0.051 Uiso 0.477(9) 1 calc PR A 1 H13C H 0.5987 0.0700 0.0721 0.051 Uiso 0.477(9) 1 calc PR A 1 C14S C 0.6670(8) -0.0741(6) -0.0610(7) 0.0340(12) Uani 0.477(9) 1 d PD A 1 H14A H 0.7184 -0.0861 -0.0922 0.051 Uiso 0.477(9) 1 calc PR A 1 H14B H 0.6009 -0.0710 -0.1176 0.051 Uiso 0.477(9) 1 calc PR A 1 H14C H 0.6444 -0.1360 -0.0515 0.051 Uiso 0.477(9) 1 calc PR A 1 O21S O 0.8567(7) 0.1768(6) 0.1849(7) 0.0430(13) Uani 0.523(9) 1 d P A 2 N21S N 0.7715(6) 0.0097(6) 0.0095(6) 0.0430(13) Uani 0.523(9) 1 d P A 2 C21S C 0.7709(8) 0.0883(8) 0.1044(8) 0.0430(13) Uani 0.523(9) 1 d P A 2 C23S C 0.8718(8) 0.0378(9) -0.0004(8) 0.0430(13) Uani 0.523(9) 1 d P A 2 H23A H 0.9276 0.1093 0.0724 0.064 Uiso 0.523(9) 1 calc PR A 2 H23B H 0.8508 0.0443 -0.0709 0.064 Uiso 0.523(9) 1 calc PR A 2 H23C H 0.9031 -0.0217 -0.0094 0.064 Uiso 0.523(9) 1 calc PR A 2 C22S C 0.6723(15) 0.0731(12) 0.1271(16) 0.0430(13) Uani 0.523(9) 1 d P A 2 H22A H 0.6890 0.1403 0.2019 0.064 Uiso 0.523(9) 1 calc PR A 2 H22B H 0.6610 0.0075 0.1342 0.064 Uiso 0.523(9) 1 calc PR A 2 H22C H 0.6046 0.0620 0.0597 0.064 Uiso 0.523(9) 1 calc PR A 2 C24S C 0.6799(8) -0.0934(8) -0.0901(9) 0.0430(13) Uani 0.523(9) 1 d P A 2 H24A H 0.6177 -0.1000 -0.0749 0.064 Uiso 0.523(9) 1 calc PR A 2 H24B H 0.7040 -0.1573 -0.0988 0.064 Uiso 0.523(9) 1 calc PR A 2 H24C H 0.6559 -0.0930 -0.1644 0.064 Uiso 0.523(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01268(11) 0.01271(11) 0.01127(11) 0.00658(9) 0.00522(8) 0.00505(8) Cd2 0.01096(14) 0.01121(14) 0.00967(14) 0.00516(11) 0.00439(11) 0.00341(11) Cd3 0.01701(16) 0.01832(16) 0.01791(16) 0.00938(13) 0.00865(13) 0.00656(12) Si1 0.0111(4) 0.0125(4) 0.0121(4) 0.0067(3) 0.0052(3) 0.0045(3) O2 0.0186(10) 0.0150(10) 0.0146(10) 0.0078(9) 0.0089(9) 0.0094(9) O1 0.0319(13) 0.0191(11) 0.0283(12) 0.0135(10) 0.0220(11) 0.0118(10) O8 0.0309(13) 0.0142(11) 0.0221(12) 0.0049(10) 0.0122(10) 0.0045(10) O10S 0.0186(11) 0.0243(12) 0.0248(12) 0.0115(10) 0.0100(10) 0.0058(10) O1S 0.0218(12) 0.0265(12) 0.0318(13) 0.0189(11) 0.0113(11) 0.0107(10) O3 0.0135(11) 0.0312(13) 0.0376(14) 0.0244(12) 0.0087(10) 0.0043(10) C5 0.0128(13) 0.0164(14) 0.0131(13) 0.0076(12) 0.0057(11) 0.0073(11) C12 0.0131(14) 0.0171(14) 0.0137(14) 0.0079(12) 0.0067(12) 0.0051(12) O5 0.0193(11) 0.0340(13) 0.0261(12) 0.0233(11) 0.0116(10) 0.0128(10) C15 0.0175(15) 0.0162(15) 0.0160(14) 0.0084(12) 0.0066(12) 0.0052(12) O4 0.0137(11) 0.0268(12) 0.0224(12) 0.0152(10) 0.0046(9) 0.0057(9) O13 0.0293(13) 0.0314(13) 0.0274(13) 0.0165(11) 0.0184(11) 0.0140(11) C2 0.0150(14) 0.0180(15) 0.0142(14) 0.0089(12) 0.0071(12) 0.0088(12) C19 0.0155(14) 0.0134(14) 0.0147(14) 0.0073(12) 0.0063(12) 0.0055(11) O6 0.0179(11) 0.0298(13) 0.0246(12) 0.0204(11) 0.0104(10) 0.0117(10) C23 0.0136(14) 0.0164(15) 0.0156(14) 0.0055(12) 0.0073(12) 0.0061(12) C1 0.0155(14) 0.0204(15) 0.0145(14) 0.0097(13) 0.0068(12) 0.0094(12) C24 0.0186(15) 0.0159(15) 0.0168(15) 0.0092(13) 0.0089(12) 0.0068(12) C25 0.0165(14) 0.0167(15) 0.0119(14) 0.0065(12) 0.0055(12) 0.0043(12) C7 0.0232(16) 0.0171(15) 0.0235(16) 0.0132(13) 0.0151(14) 0.0091(13) C26 0.0120(13) 0.0149(14) 0.0155(14) 0.0068(12) 0.0077(12) 0.0055(11) C10 0.0181(15) 0.0167(15) 0.0229(16) 0.0108(13) 0.0082(13) 0.0043(12) N2S 0.0359(17) 0.0323(17) 0.0326(17) 0.0172(14) 0.0248(15) 0.0182(14) C20 0.0195(16) 0.0304(18) 0.0302(18) 0.0230(16) 0.0160(14) 0.0127(14) C14 0.0171(15) 0.0214(16) 0.0262(17) 0.0149(14) 0.0082(13) 0.0086(13) C6 0.0218(15) 0.0137(14) 0.0191(15) 0.0082(12) 0.0115(13) 0.0075(12) O7 0.0478(16) 0.0272(13) 0.0128(11) 0.0052(10) 0.0105(11) 0.0228(12) C17 0.0173(15) 0.0220(16) 0.0199(15) 0.0132(13) 0.0101(13) 0.0063(12) C8 0.0137(14) 0.0150(14) 0.0194(15) 0.0068(13) 0.0066(12) 0.0052(12) C28 0.0198(15) 0.0230(16) 0.0127(14) 0.0076(13) 0.0061(12) 0.0093(13) C22 0.0160(15) 0.0191(16) 0.0160(15) 0.0050(13) 0.0070(12) 0.0080(12) C1S 0.0238(17) 0.0306(18) 0.0288(18) 0.0203(16) 0.0180(15) 0.0143(15) C9 0.0140(14) 0.0193(15) 0.0156(14) 0.0090(12) 0.0069(12) 0.0052(12) C27 0.0195(15) 0.0199(16) 0.0174(15) 0.0110(13) 0.0075(13) 0.0095(13) C13 0.0177(15) 0.0173(15) 0.0263(17) 0.0130(14) 0.0094(13) 0.0063(13) C16 0.0179(15) 0.0174(15) 0.0181(15) 0.0112(13) 0.0077(13) 0.0073(12) C5S 0.0299(18) 0.0194(16) 0.0265(18) 0.0109(14) 0.0165(15) 0.0094(14) C21 0.0175(15) 0.0338(19) 0.0322(18) 0.0248(16) 0.0136(14) 0.0146(14) C3 0.0197(15) 0.0134(14) 0.0205(15) 0.0047(13) 0.0106(13) 0.0045(12) N1S 0.0307(16) 0.0285(16) 0.0352(17) 0.0193(14) 0.0185(14) 0.0163(13) C4 0.0213(16) 0.0160(15) 0.0254(17) 0.0088(13) 0.0144(14) 0.0047(13) C9S 0.039(2) 0.036(2) 0.043(2) 0.0216(19) 0.0272(19) 0.0216(18) C2S 0.0243(18) 0.034(2) 0.035(2) 0.0224(17) 0.0112(16) 0.0115(16) C6S 0.038(2) 0.038(2) 0.031(2) 0.0211(18) 0.0201(17) 0.0163(17) C18 0.0138(14) 0.0218(16) 0.0198(15) 0.0120(13) 0.0075(12) 0.0075(12) C3S 0.044(2) 0.027(2) 0.042(2) 0.0127(18) 0.018(2) 0.0143(18) C11 0.0176(15) 0.0191(15) 0.0201(15) 0.0120(13) 0.0080(13) 0.0081(12) C4S 0.039(2) 0.037(2) 0.056(3) 0.033(2) 0.028(2) 0.0241(18) C7S 0.069(3) 0.086(4) 0.042(3) 0.040(3) 0.037(3) 0.043(3) C8S 0.065(3) 0.079(4) 0.050(3) 0.044(3) 0.044(3) 0.040(3) O11S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) N11S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) C11S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) C12S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) C13S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) C14S 0.037(2) 0.027(2) 0.031(2) 0.0129(16) 0.0140(16) 0.0095(16) O21S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) N21S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) C21S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) C23S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) C22S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) C24S 0.048(2) 0.030(2) 0.035(2) 0.0105(16) 0.0160(16) 0.0096(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.191(2) 1_455 ? Cd1 O8 2.210(2) 1_566 ? Cd1 O2 2.296(2) . ? Cd1 O6 2.335(2) 1_556 ? Cd1 O5 2.335(2) 1_556 ? Cd1 O1 2.516(2) . ? Cd1 C15 2.674(3) 1_556 ? Cd1 C1 2.744(3) . ? Cd2 O7 2.207(2) 2_654 ? Cd2 O7 2.207(2) 1_566 ? Cd2 O3 2.288(2) 2_765 ? Cd2 O3 2.288(2) 1_455 ? Cd2 O2 2.329(2) . ? Cd2 O2 2.329(2) 2_665 ? Cd3 O10S 2.259(2) 2_766 ? Cd3 O10S 2.259(2) . ? Cd3 O13 2.282(2) . ? Cd3 O13 2.282(2) 2_766 ? Cd3 O1S 2.292(2) . ? Cd3 O1S 2.292(2) 2_766 ? Si1 C19 1.872(3) . ? Si1 C5 1.873(3) . ? Si1 C26 1.876(3) . ? Si1 C12 1.880(3) . ? O2 C1 1.288(4) . ? O1 C1 1.242(4) . ? O8 C22 1.259(4) . ? O8 Cd1 2.210(2) 1_544 ? O10S H15 0.9599(10) . ? O10S H17 0.9599(10) . ? O1S C1S 1.249(4) . ? O3 C8 1.248(4) . ? O3 Cd2 2.288(2) 1_655 ? C5 C6 1.397(4) . ? C5 C4 1.403(4) . ? C12 C11 1.398(4) . ? C12 C13 1.400(4) . ? O5 C15 1.266(4) . ? O5 Cd1 2.335(2) 1_554 ? C15 O6 1.257(4) . ? C15 C16 1.501(4) . ? C15 Cd1 2.674(3) 1_554 ? O4 C8 1.258(4) . ? O4 Cd1 2.191(2) 1_655 ? O13 C5S 1.245(4) . ? C2 C3 1.385(4) . ? C2 C7 1.392(4) . ? C2 C1 1.502(4) . ? C19 C18 1.398(4) . ? C19 C20 1.403(4) . ? O6 Cd1 2.335(2) 1_554 ? C23 C28 1.385(5) . ? C23 C24 1.392(4) . ? C23 C22 1.506(4) . ? C24 C25 1.393(4) . ? C24 H19 0.9500 . ? C25 C26 1.401(4) . ? C25 H20 0.9500 . ? C7 C6 1.395(4) . ? C7 H21 0.9500 . ? C26 C27 1.402(4) . ? C10 C11 1.386(4) . ? C10 C9 1.391(4) . ? C10 H23 0.9500 . ? N2S C5S 1.334(5) . ? N2S C9S 1.445(5) . ? N2S C8S 1.452(5) . ? C20 C21 1.387(5) . ? C20 H25 0.9500 . ? C14 C9 1.390(4) . ? C14 C13 1.391(4) . ? C14 H26 0.9500 . ? C6 H27 0.9500 . ? O7 C22 1.245(4) . ? O7 Cd2 2.207(2) 1_544 ? C17 C18 1.384(4) . ? C17 C16 1.394(4) . ? C17 H29 0.9500 . ? C8 C9 1.509(4) . ? C28 C27 1.387(4) . ? C28 H31 0.9500 . ? C1S N1S 1.340(5) . ? C1S C2S 1.500(5) . ? C27 H35 0.9500 . ? C13 H37 0.9500 . ? C16 C21 1.391(5) . ? C5S C6S 1.510(5) . ? C21 H40 0.9500 . ? C3 C4 1.390(4) . ? C3 H41 0.9500 . ? N1S C4S 1.459(5) . ? N1S C3S 1.461(5) . ? C4 H43 0.9500 . ? C9S H44A 0.9800 . ? C9S H44B 0.9800 . ? C9S H44C 0.9800 . ? C2S H47A 0.9800 . ? C2S H47B 0.9800 . ? C2S H47C 0.9800 . ? C6S C7S 1.519(6) . ? C6S H48A 0.9900 . ? C6S H48B 0.9900 . ? C18 H52 0.9500 . ? C3S H53A 0.9800 . ? C3S H53B 0.9800 . ? C3S H53C 0.9800 . ? C11 H54 0.9500 . ? C4S H55A 0.9800 . ? C4S H55B 0.9800 . ? C4S H55C 0.9800 . ? C7S C8S 1.476(7) . ? C7S H57A 0.9900 . ? C7S H57B 0.9900 . ? C8S H58A 0.9900 . ? C8S H58B 0.9900 . ? O11S C11S 1.233(11) . ? N11S C11S 1.368(12) . ? N11S C13S 1.399(3) . ? N11S C14S 1.406(3) . ? C11S C12S 1.509(2) . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? C13S H13A 0.9800 . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? O21S C21S 1.270(12) . ? N21S C21S 1.329(12) . ? N21S C24S 1.443(11) . ? N21S C23S 1.488(12) . ? C21S C22S 1.546(16) . ? C23S H23A 0.9800 . ? C23S H23B 0.9800 . ? C23S H23C 0.9800 . ? C22S H22A 0.9800 . ? C22S H22B 0.9800 . ? C22S H22C 0.9800 . ? C24S H24A 0.9800 . ? C24S H24B 0.9800 . ? C24S H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O8 111.03(9) 1_455 1_566 ? O4 Cd1 O2 100.73(8) 1_455 . ? O8 Cd1 O2 100.13(8) 1_566 . ? O4 Cd1 O6 96.44(8) 1_455 1_556 ? O8 Cd1 O6 96.87(9) 1_566 1_556 ? O2 Cd1 O6 149.54(7) . 1_556 ? O4 Cd1 O5 145.70(8) 1_455 1_556 ? O8 Cd1 O5 94.03(9) 1_566 1_556 ? O2 Cd1 O5 97.26(8) . 1_556 ? O6 Cd1 O5 56.28(8) 1_556 1_556 ? O4 Cd1 O1 87.46(8) 1_455 . ? O8 Cd1 O1 152.13(8) 1_566 . ? O2 Cd1 O1 54.61(7) . . ? O6 Cd1 O1 101.69(8) 1_556 . ? O5 Cd1 O1 79.53(8) 1_556 . ? O4 Cd1 C15 121.97(9) 1_455 1_556 ? O8 Cd1 C15 96.37(9) 1_566 1_556 ? O2 Cd1 C15 124.13(9) . 1_556 ? O6 Cd1 C15 28.03(9) 1_556 1_556 ? O5 Cd1 C15 28.25(9) 1_556 1_556 ? O1 Cd1 C15 90.56(9) . 1_556 ? O4 Cd1 C1 96.03(9) 1_455 . ? O8 Cd1 C1 126.62(9) 1_566 . ? O2 Cd1 C1 27.84(8) . . ? O6 Cd1 C1 125.64(9) 1_556 . ? O5 Cd1 C1 86.52(9) 1_556 . ? O1 Cd1 C1 26.86(8) . . ? C15 Cd1 C1 107.17(9) 1_556 . ? O7 Cd2 O7 180.0(2) 2_654 1_566 ? O7 Cd2 O3 89.75(10) 2_654 2_765 ? O7 Cd2 O3 90.25(10) 1_566 2_765 ? O7 Cd2 O3 90.25(10) 2_654 1_455 ? O7 Cd2 O3 89.75(10) 1_566 1_455 ? O3 Cd2 O3 180.00(15) 2_765 1_455 ? O7 Cd2 O2 93.95(8) 2_654 . ? O7 Cd2 O2 86.05(8) 1_566 . ? O3 Cd2 O2 89.23(8) 2_765 . ? O3 Cd2 O2 90.77(8) 1_455 . ? O7 Cd2 O2 86.05(8) 2_654 2_665 ? O7 Cd2 O2 93.95(8) 1_566 2_665 ? O3 Cd2 O2 90.77(8) 2_765 2_665 ? O3 Cd2 O2 89.23(8) 1_455 2_665 ? O2 Cd2 O2 180.0 . 2_665 ? O10S Cd3 O10S 179.999(1) 2_766 . ? O10S Cd3 O13 88.03(9) 2_766 . ? O10S Cd3 O13 91.97(9) . . ? O10S Cd3 O13 91.97(9) 2_766 2_766 ? O10S Cd3 O13 88.03(9) . 2_766 ? O13 Cd3 O13 179.998(1) . 2_766 ? O10S Cd3 O1S 84.81(9) 2_766 . ? O10S Cd3 O1S 95.19(9) . . ? O13 Cd3 O1S 94.77(9) . . ? O13 Cd3 O1S 85.23(9) 2_766 . ? O10S Cd3 O1S 95.19(9) 2_766 2_766 ? O10S Cd3 O1S 84.81(9) . 2_766 ? O13 Cd3 O1S 85.23(9) . 2_766 ? O13 Cd3 O1S 94.77(9) 2_766 2_766 ? O1S Cd3 O1S 179.999(1) . 2_766 ? C19 Si1 C5 108.31(13) . . ? C19 Si1 C26 106.61(13) . . ? C5 Si1 C26 112.08(13) . . ? C19 Si1 C12 108.99(14) . . ? C5 Si1 C12 109.39(13) . . ? C26 Si1 C12 111.34(13) . . ? C1 O2 Cd1 95.82(18) . . ? C1 O2 Cd2 132.63(19) . . ? Cd1 O2 Cd2 104.49(8) . . ? C1 O1 Cd1 86.84(18) . . ? C22 O8 Cd1 119.6(2) . 1_544 ? Cd3 O10S H15 124(3) . . ? Cd3 O10S H17 123(3) . . ? H15 O10S H17 95.4(3) . . ? C1S O1S Cd3 135.8(2) . . ? C8 O3 Cd2 142.4(2) . 1_655 ? C6 C5 C4 117.9(3) . . ? C6 C5 Si1 124.7(2) . . ? C4 C5 Si1 117.3(2) . . ? C11 C12 C13 117.2(3) . . ? C11 C12 Si1 119.6(2) . . ? C13 C12 Si1 123.2(2) . . ? C15 O5 Cd1 90.93(18) . 1_554 ? O6 C15 O5 121.6(3) . . ? O6 C15 C16 119.6(3) . . ? O5 C15 C16 118.8(3) . . ? O6 C15 Cd1 60.81(16) . 1_554 ? O5 C15 Cd1 60.83(16) . 1_554 ? C16 C15 Cd1 179.4(2) . 1_554 ? C8 O4 Cd1 126.1(2) . 1_655 ? C5S O13 Cd3 130.7(2) . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 119.8(3) . . ? C7 C2 C1 120.2(3) . . ? C18 C19 C20 117.5(3) . . ? C18 C19 Si1 121.4(2) . . ? C20 C19 Si1 120.5(2) . . ? C15 O6 Cd1 91.16(18) . 1_554 ? C28 C23 C24 119.4(3) . . ? C28 C23 C22 118.8(3) . . ? C24 C23 C22 121.8(3) . . ? O1 C1 O2 122.3(3) . . ? O1 C1 C2 120.4(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 Cd1 66.30(16) . . ? O2 C1 Cd1 56.35(15) . . ? C2 C1 Cd1 170.6(2) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H19 120.0 . . ? C25 C24 H19 120.0 . . ? C24 C25 C26 121.3(3) . . ? C24 C25 H20 119.3 . . ? C26 C25 H20 119.3 . . ? C2 C7 C6 120.0(3) . . ? C2 C7 H21 120.0 . . ? C6 C7 H21 120.0 . . ? C25 C26 C27 117.4(3) . . ? C25 C26 Si1 124.1(2) . . ? C27 C26 Si1 118.6(2) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H23 119.9 . . ? C9 C10 H23 119.9 . . ? C5S N2S C9S 125.1(3) . . ? C5S N2S C8S 113.2(3) . . ? C9S N2S C8S 121.8(3) . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H25 119.4 . . ? C19 C20 H25 119.4 . . ? C9 C14 C13 120.5(3) . . ? C9 C14 H26 119.7 . . ? C13 C14 H26 119.7 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H27 119.6 . . ? C7 C6 H27 119.6 . . ? C22 O7 Cd2 150.7(2) . 1_544 ? C18 C17 C16 120.1(3) . . ? C18 C17 H29 120.0 . . ? C16 C17 H29 120.0 . . ? O3 C8 O4 127.8(3) . . ? O3 C8 C9 116.9(3) . . ? O4 C8 C9 115.3(3) . . ? C23 C28 C27 120.4(3) . . ? C23 C28 H31 119.8 . . ? C27 C28 H31 119.8 . . ? O7 C22 O8 126.3(3) . . ? O7 C22 C23 116.2(3) . . ? O8 C22 C23 117.5(3) . . ? O1S C1S N1S 119.4(3) . . ? O1S C1S C2S 120.3(3) . . ? N1S C1S C2S 120.2(3) . . ? C14 C9 C10 118.9(3) . . ? C14 C9 C8 120.9(3) . . ? C10 C9 C8 120.2(3) . . ? C28 C27 C26 121.4(3) . . ? C28 C27 H35 119.3 . . ? C26 C27 H35 119.3 . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H37 119.4 . . ? C12 C13 H37 119.4 . . ? C21 C16 C17 119.2(3) . . ? C21 C16 C15 120.1(3) . . ? C17 C16 C15 120.7(3) . . ? O13 C5S N2S 124.3(3) . . ? O13 C5S C6S 126.0(3) . . ? N2S C5S C6S 109.6(3) . . ? C20 C21 C16 120.4(3) . . ? C20 C21 H40 119.8 . . ? C16 C21 H40 119.8 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H41 120.1 . . ? C4 C3 H41 120.1 . . ? C1S N1S C4S 125.0(3) . . ? C1S N1S C3S 120.1(3) . . ? C4S N1S C3S 114.9(3) . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H43 119.3 . . ? C5 C4 H43 119.3 . . ? N2S C9S H44A 109.5 . . ? N2S C9S H44B 109.5 . . ? H44A C9S H44B 109.5 . . ? N2S C9S H44C 109.5 . . ? H44A C9S H44C 109.5 . . ? H44B C9S H44C 109.5 . . ? C1S C2S H47A 109.5 . . ? C1S C2S H47B 109.5 . . ? H47A C2S H47B 109.5 . . ? C1S C2S H47C 109.5 . . ? H47A C2S H47C 109.5 . . ? H47B C2S H47C 109.5 . . ? C5S C6S C7S 104.0(3) . . ? C5S C6S H48A 111.0 . . ? C7S C6S H48A 111.0 . . ? C5S C6S H48B 111.0 . . ? C7S C6S H48B 111.0 . . ? H48A C6S H48B 109.0 . . ? C17 C18 C19 121.6(3) . . ? C17 C18 H52 119.2 . . ? C19 C18 H52 119.2 . . ? N1S C3S H53A 109.5 . . ? N1S C3S H53B 109.5 . . ? H53A C3S H53B 109.5 . . ? N1S C3S H53C 109.5 . . ? H53A C3S H53C 109.5 . . ? H53B C3S H53C 109.5 . . ? C10 C11 C12 121.8(3) . . ? C10 C11 H54 119.1 . . ? C12 C11 H54 119.1 . . ? N1S C4S H55A 109.5 . . ? N1S C4S H55B 109.5 . . ? H55A C4S H55B 109.5 . . ? N1S C4S H55C 109.5 . . ? H55A C4S H55C 109.5 . . ? H55B C4S H55C 109.5 . . ? C8S C7S C6S 107.4(4) . . ? C8S C7S H57A 110.2 . . ? C6S C7S H57A 110.2 . . ? C8S C7S H57B 110.2 . . ? C6S C7S H57B 110.2 . . ? H57A C7S H57B 108.5 . . ? N2S C8S C7S 105.8(4) . . ? N2S C8S H58A 110.6 . . ? C7S C8S H58A 110.6 . . ? N2S C8S H58B 110.6 . . ? C7S C8S H58B 110.6 . . ? H58A C8S H58B 108.7 . . ? C11S N11S C13S 124.0(8) . . ? C11S N11S C14S 115.4(7) . . ? C13S N11S C14S 120.2(9) . . ? O11S C11S N11S 124.4(8) . . ? O11S C11S C12S 129.7(9) . . ? N11S C11S C12S 105.6(7) . . ? C11S C12S H12A 109.5 . . ? C11S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? C11S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? N11S C13S H13A 109.5 . . ? N11S C13S H13B 109.5 . . ? H13A C13S H13B 109.5 . . ? N11S C13S H13C 109.5 . . ? H13A C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? N11S C14S H14A 109.5 . . ? N11S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? N11S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? C21S N21S C24S 126.2(8) . . ? C21S N21S C23S 116.0(8) . . ? C24S N21S C23S 117.4(7) . . ? O21S C21S N21S 119.9(9) . . ? O21S C21S C22S 117.3(9) . . ? N21S C21S C22S 122.6(9) . . ? N21S C23S H23A 109.5 . . ? N21S C23S H23B 109.5 . . ? H23A C23S H23B 109.5 . . ? N21S C23S H23C 109.5 . . ? H23A C23S H23C 109.5 . . ? H23B C23S H23C 109.5 . . ? C21S C22S H22A 109.5 . . ? C21S C22S H22B 109.5 . . ? H22A C22S H22B 109.5 . . ? C21S C22S H22C 109.5 . . ? H22A C22S H22C 109.5 . . ? H22B C22S H22C 109.5 . . ? N21S C24S H24A 109.5 . . ? N21S C24S H24B 109.5 . . ? H24A C24S H24B 109.5 . . ? N21S C24S H24C 109.5 . . ? H24A C24S H24C 109.5 . . ? H24B C24S H24C 109.5 . . ? 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 O4 Cd1 O2 C1 -82.53(18) 1_455 . . . ? O8 Cd1 O2 C1 163.58(17) 1_566 . . . ? O6 Cd1 O2 C1 40.7(2) 1_556 . . . ? O5 Cd1 O2 C1 68.14(18) 1_556 . . . ? O1 Cd1 O2 C1 -3.48(16) . . . . ? C15 Cd1 O2 C1 58.7(2) 1_556 . . . ? O4 Cd1 O2 Cd2 54.31(10) 1_455 . . . ? O8 Cd1 O2 Cd2 -59.58(10) 1_566 . . . ? O6 Cd1 O2 Cd2 177.50(12) 1_556 . . . ? O5 Cd1 O2 Cd2 -155.02(9) 1_556 . . . ? O1 Cd1 O2 Cd2 133.36(12) . . . . ? C15 Cd1 O2 Cd2 -164.48(9) 1_556 . . . ? C1 Cd1 O2 Cd2 136.8(2) . . . . ? O7 Cd2 O2 C1 -23.1(3) 2_654 . . . ? O7 Cd2 O2 C1 156.9(3) 1_566 . . . ? O3 Cd2 O2 C1 -112.8(3) 2_765 . . . ? O3 Cd2 O2 C1 67.2(3) 1_455 . . . ? O2 Cd2 O2 C1 -33(83) 2_665 . . . ? O7 Cd2 O2 Cd1 -135.39(10) 2_654 . . . ? O7 Cd2 O2 Cd1 44.61(10) 1_566 . . . ? O3 Cd2 O2 Cd1 134.91(10) 2_765 . . . ? O3 Cd2 O2 Cd1 -45.09(10) 1_455 . . . ? O2 Cd2 O2 Cd1 -145(83) 2_665 . . . ? O4 Cd1 O1 C1 108.67(19) 1_455 . . . ? O8 Cd1 O1 C1 -24.5(3) 1_566 . . . ? O2 Cd1 O1 C1 3.60(17) . . . . ? O6 Cd1 O1 C1 -155.27(18) 1_556 . . . ? O5 Cd1 O1 C1 -103.21(19) 1_556 . . . ? C15 Cd1 O1 C1 -129.35(19) 1_556 . . . ? O10S Cd3 O1S C1S -145.4(3) 2_766 . . . ? O10S Cd3 O1S C1S 34.6(3) . . . . ? O13 Cd3 O1S C1S 127.0(3) . . . . ? O13 Cd3 O1S C1S -53.0(3) 2_766 . . . ? O1S Cd3 O1S C1S 104(17) 2_766 . . . ? C19 Si1 C5 C6 121.9(3) . . . . ? C26 Si1 C5 C6 4.6(3) . . . . ? C12 Si1 C5 C6 -119.4(3) . . . . ? C19 Si1 C5 C4 -55.0(3) . . . . ? C26 Si1 C5 C4 -172.3(2) . . . . ? C12 Si1 C5 C4 63.7(3) . . . . ? C19 Si1 C12 C11 32.3(3) . . . . ? C5 Si1 C12 C11 -85.9(3) . . . . ? C26 Si1 C12 C11 149.7(2) . . . . ? C19 Si1 C12 C13 -149.0(3) . . . . ? C5 Si1 C12 C13 92.7(3) . . . . ? C26 Si1 C12 C13 -31.7(3) . . . . ? Cd1 O5 C15 O6 -0.7(3) 1_554 . . . ? Cd1 O5 C15 C16 179.5(2) 1_554 . . . ? O10S Cd3 O13 C5S -128.6(3) 2_766 . . . ? O10S Cd3 O13 C5S 51.4(3) . . . . ? O13 Cd3 O13 C5S 144(13) 2_766 . . . ? O1S Cd3 O13 C5S -44.0(3) . . . . ? O1S Cd3 O13 C5S 136.0(3) 2_766 . . . ? C5 Si1 C19 C18 152.0(2) . . . . ? C26 Si1 C19 C18 -87.2(3) . . . . ? C12 Si1 C19 C18 33.1(3) . . . . ? C5 Si1 C19 C20 -36.7(3) . . . . ? C26 Si1 C19 C20 84.1(3) . . . . ? C12 Si1 C19 C20 -155.6(3) . . . . ? O5 C15 O6 Cd1 0.7(3) . . . 1_554 ? C16 C15 O6 Cd1 -179.5(3) . . . 1_554 ? Cd1 O1 C1 O2 -6.2(3) . . . . ? Cd1 O1 C1 C2 172.6(3) . . . . ? Cd1 O2 C1 O1 6.8(3) . . . . ? Cd2 O2 C1 O1 -109.0(3) . . . . ? Cd1 O2 C1 C2 -172.0(2) . . . . ? Cd2 O2 C1 C2 72.2(3) . . . . ? Cd2 O2 C1 Cd1 -115.8(2) . . . . ? C3 C2 C1 O1 -170.8(3) . . . . ? C7 C2 C1 O1 10.7(4) . . . . ? C3 C2 C1 O2 8.0(4) . . . . ? C7 C2 C1 O2 -170.4(3) . . . . ? C3 C2 C1 Cd1 -37.4(14) . . . . ? C7 C2 C1 Cd1 144.2(12) . . . . ? O4 Cd1 C1 O1 -72.12(19) 1_455 . . . ? O8 Cd1 C1 O1 166.00(17) 1_566 . . . ? O2 Cd1 C1 O1 -173.7(3) . . . . ? O6 Cd1 C1 O1 30.3(2) 1_556 . . . ? O5 Cd1 C1 O1 73.56(18) 1_556 . . . ? C15 Cd1 C1 O1 54.0(2) 1_556 . . . ? O4 Cd1 C1 O2 101.60(17) 1_455 . . . ? O8 Cd1 C1 O2 -20.3(2) 1_566 . . . ? O6 Cd1 C1 O2 -156.02(15) 1_556 . . . ? O5 Cd1 C1 O2 -112.73(17) 1_556 . . . ? O1 Cd1 C1 O2 173.7(3) . . . . ? C15 Cd1 C1 O2 -132.26(17) 1_556 . . . ? O4 Cd1 C1 C2 151.0(13) 1_455 . . . ? O8 Cd1 C1 C2 29.2(13) 1_566 . . . ? O2 Cd1 C1 C2 49.4(12) . . . . ? O6 Cd1 C1 C2 -106.6(13) 1_556 . . . ? O5 Cd1 C1 C2 -63.3(13) 1_556 . . . ? O1 Cd1 C1 C2 -136.8(14) . . . . ? C15 Cd1 C1 C2 -82.8(13) 1_556 . . . ? C28 C23 C24 C25 0.2(5) . . . . ? C22 C23 C24 C25 -179.7(3) . . . . ? C23 C24 C25 C26 0.7(5) . . . . ? C3 C2 C7 C6 -2.2(5) . . . . ? C1 C2 C7 C6 176.2(3) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C24 C25 C26 Si1 179.4(2) . . . . ? C19 Si1 C26 C25 -176.4(2) . . . . ? C5 Si1 C26 C25 -58.1(3) . . . . ? C12 Si1 C26 C25 64.8(3) . . . . ? C19 Si1 C26 C27 3.9(3) . . . . ? C5 Si1 C26 C27 122.2(2) . . . . ? C12 Si1 C26 C27 -114.9(2) . . . . ? C18 C19 C20 C21 0.9(5) . . . . ? Si1 C19 C20 C21 -170.8(3) . . . . ? C4 C5 C6 C7 -0.2(5) . . . . ? Si1 C5 C6 C7 -177.0(2) . . . . ? C2 C7 C6 C5 2.0(5) . . . . ? Cd2 O3 C8 O4 4.4(6) 1_655 . . . ? Cd2 O3 C8 C9 -175.8(2) 1_655 . . . ? Cd1 O4 C8 O3 3.2(5) 1_655 . . . ? Cd1 O4 C8 C9 -176.63(19) 1_655 . . . ? C24 C23 C28 C27 -0.8(5) . . . . ? C22 C23 C28 C27 179.1(3) . . . . ? Cd2 O7 C22 O8 -24.0(7) 1_544 . . . ? Cd2 O7 C22 C23 155.5(4) 1_544 . . . ? Cd1 O8 C22 O7 3.9(5) 1_544 . . . ? Cd1 O8 C22 C23 -175.51(19) 1_544 . . . ? C28 C23 C22 O7 12.0(4) . . . . ? C24 C23 C22 O7 -168.1(3) . . . . ? C28 C23 C22 O8 -168.5(3) . . . . ? C24 C23 C22 O8 11.4(4) . . . . ? Cd3 O1S C1S N1S 147.9(3) . . . . ? Cd3 O1S C1S C2S -30.8(5) . . . . ? C13 C14 C9 C10 2.3(5) . . . . ? C13 C14 C9 C8 -177.7(3) . . . . ? C11 C10 C9 C14 0.8(5) . . . . ? C11 C10 C9 C8 -179.3(3) . . . . ? O3 C8 C9 C14 139.9(3) . . . . ? O4 C8 C9 C14 -40.3(4) . . . . ? O3 C8 C9 C10 -40.1(4) . . . . ? O4 C8 C9 C10 139.8(3) . . . . ? C23 C28 C27 C26 0.5(5) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? Si1 C26 C27 C28 -180.0(2) . . . . ? C9 C14 C13 C12 -3.1(5) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? Si1 C12 C13 C14 -177.9(3) . . . . ? C18 C17 C16 C21 1.2(5) . . . . ? C18 C17 C16 C15 -179.1(3) . . . . ? O6 C15 C16 C21 -4.0(5) . . . . ? O5 C15 C16 C21 175.8(3) . . . . ? Cd1 C15 C16 C21 -139(27) 1_554 . . . ? O6 C15 C16 C17 176.3(3) . . . . ? O5 C15 C16 C17 -3.9(5) . . . . ? Cd1 C15 C16 C17 41(28) 1_554 . . . ? Cd3 O13 C5S N2S 167.93(18) . . . . ? Cd3 O13 C5S C6S -15.7(4) . . . . ? C9S N2S C5S O13 -3.2(4) . . . . ? C8S N2S C5S O13 177.0(3) . . . . ? C9S N2S C5S C6S 179.9(3) . . . . ? C8S N2S C5S C6S 0.1(5) . . . . ? C19 C20 C21 C16 -0.1(5) . . . . ? C17 C16 C21 C20 -1.0(5) . . . . ? C15 C16 C21 C20 179.4(3) . . . . ? C7 C2 C3 C4 0.6(5) . . . . ? C1 C2 C3 C4 -177.8(3) . . . . ? O1S C1S N1S C4S 171.7(3) . . . . ? C2S C1S N1S C4S -9.6(5) . . . . ? O1S C1S N1S C3S -6.5(5) . . . . ? C2S C1S N1S C3S 172.2(3) . . . . ? C2 C3 C4 C5 1.2(5) . . . . ? C6 C5 C4 C3 -1.4(5) . . . . ? Si1 C5 C4 C3 175.7(3) . . . . ? O13 C5S C6S C7S -176.8(3) . . . . ? N2S C5S C6S C7S 0.06(2) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C20 C19 C18 C17 -0.6(5) . . . . ? Si1 C19 C18 C17 170.9(2) . . . . ? C9 C10 C11 C12 -3.2(5) . . . . ? C13 C12 C11 C10 2.4(5) . . . . ? Si1 C12 C11 C10 -178.9(2) . . . . ? C5S C6S C7S C8S -0.1(5) . . . . ? C5S N2S C8S C7S -0.1(5) . . . . ? C9S N2S C8S C7S -180.0(3) . . . . ? C6S C7S C8S N2S 0.1(5) . . . . ? C13S N11S C11S O11S 0.4(17) . . . . ? C14S N11S C11S O11S 172.7(9) . . . . ? C13S N11S C11S C12S -174.3(12) . . . . ? C14S N11S C11S C12S -2.0(10) . . . . ? C24S N21S C21S O21S -178.4(9) . . . . ? C23S N21S C21S O21S -5.8(13) . . . . ? C24S N21S C21S C22S 6.5(17) . . . . ? C23S N21S C21S C22S 179.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.133 _refine_diff_density_min -2.367 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 942374' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cd3 (C28 H16 O8 Si)2][Cd (C3H7NO)6](C3H7NO)2' _chemical_formula_sum 'C80 H88 Cd4 N8 O24 Si2' _chemical_formula_weight 2051.36 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.875(7) _cell_length_b 14.072(7) _cell_length_c 14.208(7) _cell_angle_alpha 116.300(5) _cell_angle_beta 109.724(5) _cell_angle_gamma 101.428(5) _cell_volume 2133.1(18) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9839 _cell_measurement_theta_min 2.5214 _cell_measurement_theta_max 28.7678 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6696 _exptl_absorpt_correction_T_max 0.7357 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23787 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9199 _reflns_number_gt 8115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0442P)^2^+13.8000P] 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 9199 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 1.0000 0.0000 0.01785(10) Uani 1 2 d S . . Cd2 Cd 0.29469(2) 1.12624(3) 0.11388(3) 0.01951(9) Uani 1 1 d . . . Cd3 Cd 0.5000 1.5000 0.0000 0.03580(13) Uani 1 2 d S . . Si1 Si 0.01012(9) 1.34604(10) 0.61091(10) 0.0190(2) Uani 1 1 d . . . O2 O 0.2832(3) 1.2871(3) 0.2751(3) 0.0311(7) Uani 1 1 d . . . O1 O 0.1665(2) 1.1031(3) 0.1820(3) 0.0245(6) Uani 1 1 d . . . O7 O -0.5631(3) 1.1547(3) 0.2890(3) 0.0347(8) Uani 1 1 d . . . O8 O -0.5125(3) 1.2204(3) 0.1903(3) 0.0298(7) Uani 1 1 d . . . O6 O 0.2323(3) 1.1706(3) 0.9808(3) 0.0298(7) Uani 1 1 d . . . C13 C 0.1791(4) 1.5779(4) 0.8037(4) 0.0271(9) Uani 1 1 d . . . H8 H 0.2310 1.5431 0.8103 0.033 Uiso 1 1 calc R . . O4 O 0.2837(3) 1.9435(3) 1.0118(3) 0.0345(8) Uani 1 1 d . . . C5 C 0.0802(3) 1.3101(4) 0.5155(4) 0.0212(8) Uani 1 1 d . . . C19 C 0.0386(5) 1.2785(6) 0.6994(5) 0.0417(5) Uani 1 1 d . . . C26 C -0.1431(3) 1.2945(4) 0.5073(4) 0.0224(8) Uani 1 1 d . . . O5 O 0.0625(3) 1.1369(3) 0.9706(3) 0.0337(8) Uani 1 1 d . . . C2 C 0.1661(4) 1.2447(4) 0.3545(4) 0.0234(8) Uani 1 1 d . . . C22 C -0.4896(4) 1.2028(4) 0.2735(4) 0.0258(9) Uani 1 1 d . . . C1 C 0.2090(4) 1.2115(4) 0.2657(4) 0.0245(9) Uani 1 1 d . . . C28 C -0.2865(4) 1.2620(4) 0.3264(4) 0.0308(10) Uani 1 1 d . . . H20 H -0.3057 1.2601 0.2546 0.037 Uiso 1 1 calc R . . O3S O 0.4439(4) 1.3043(3) -0.1056(4) 0.0480(10) Uani 1 1 d . . . C23 C -0.3683(4) 1.2389(4) 0.3569(4) 0.0243(9) Uani 1 1 d . . . C12 C 0.0652(4) 1.5074(4) 0.7188(4) 0.0207(8) Uani 1 1 d . . . N3S N 0.4332(4) 1.1298(4) -0.1358(4) 0.0368(10) Uani 1 1 d . . . C15 C 0.1339(5) 1.1653(6) 0.9413(5) 0.0417(5) Uani 1 1 d . . . C16 C 0.0987(5) 1.1996(6) 0.8530(5) 0.0417(5) Uani 1 1 d . . . C4 C 0.1592(4) 1.3937(4) 0.5210(4) 0.0256(9) Uani 1 1 d . . . H28 H 0.1841 1.4737 0.5798 0.031 Uiso 1 1 calc R . . C14 C 0.2173(4) 1.6978(4) 0.8786(4) 0.0264(9) Uani 1 1 d . . . H29 H 0.2949 1.7441 0.9347 0.032 Uiso 1 1 calc R . . C6 C 0.0465(4) 1.1921(4) 0.4281(4) 0.0254(9) Uani 1 1 d . . . H30 H -0.0059 1.1333 0.4237 0.030 Uiso 1 1 calc R . . C3 C 0.2024(4) 1.3621(4) 0.4420(4) 0.0268(9) Uani 1 1 d . . . H31 H 0.2566 1.4204 0.4474 0.032 Uiso 1 1 calc R . . C7 C 0.0887(4) 1.1607(4) 0.3488(4) 0.0240(9) Uani 1 1 d . . . H32 H 0.0642 1.0808 0.2899 0.029 Uiso 1 1 calc R . . C27 C -0.1756(4) 1.2881(5) 0.4000(5) 0.0324(10) Uani 1 1 d . . . H34 H -0.1208 1.3019 0.3762 0.039 Uiso 1 1 calc R . . C7S C 0.4584(4) 1.2413(4) -0.0672(5) 0.0334(10) Uani 1 1 d . . . H35 H 0.4897 1.2759 0.0168 0.040 Uiso 1 1 calc R . . C11 C -0.0085(4) 1.5617(4) 0.7150(4) 0.0307(10) Uani 1 1 d . . . H36 H -0.0863 1.5160 0.6592 0.037 Uiso 1 1 calc R . . O2S O 0.5886(4) 1.5043(4) 0.1726(4) 0.0558(6) Uani 1 1 d . . . O1S O 0.3502(5) 1.4967(5) 0.0278(5) 0.0821(10) Uani 1 1 d . . . C8S C 0.4490(5) 1.0598(5) -0.0863(5) 0.0424(13) Uani 1 1 d . . . H40A H 0.4810 1.1089 0.0010 0.064 Uiso 1 1 calc R . . H40B H 0.5003 1.0259 -0.1057 0.064 Uiso 1 1 calc R . . H40C H 0.3764 0.9974 -0.1209 0.064 Uiso 1 1 calc R . . C21 C 0.1601(5) 1.2128(6) 0.7985(5) 0.0417(5) Uani 1 1 d . . . H43 H 0.2245 1.1957 0.8128 0.050 Uiso 1 1 calc R . . C20 C 0.1294(5) 1.2508(5) 0.7224(5) 0.0417(5) Uani 1 1 d . . . H48 H 0.1731 1.2579 0.6848 0.050 Uiso 1 1 calc R . . C25 C -0.2269(4) 1.2736(6) 0.5374(5) 0.0416(13) Uani 1 1 d . . . H49 H -0.2075 1.2789 0.6109 0.050 Uiso 1 1 calc R . . C1S C 0.3066(8) 1.4675(7) 0.0661(8) 0.0821(10) Uani 1 1 d . . . H52 H 0.3266 1.4132 0.0816 0.099 Uiso 1 1 calc R . . C18 C -0.0186(5) 1.2711(6) 0.7616(5) 0.0417(5) Uani 1 1 d . . . H53 H -0.0784 1.2955 0.7539 0.050 Uiso 1 1 calc R . . C17 C 0.0091(5) 1.2291(6) 0.8345(5) 0.0417(5) Uani 1 1 d . . . H54 H -0.0345 1.2208 0.8716 0.050 Uiso 1 1 calc R . . N1S N 0.2302(6) 1.4931(6) 0.0956(7) 0.0821(10) Uani 1 1 d . . . C3S C 0.2034(8) 1.4482(7) 0.1611(8) 0.0821(10) Uani 1 1 d . . . H66A H 0.2411 1.3968 0.1643 0.123 Uiso 1 1 calc R . . H66B H 0.1219 1.4042 0.1208 0.123 Uiso 1 1 calc R . . H66C H 0.2289 1.5128 0.2428 0.123 Uiso 1 1 calc R . . C2S C 0.1741(8) 1.5608(7) 0.0718(8) 0.0821(10) Uani 1 1 d . . . H74A H 0.2017 1.6356 0.1468 0.123 Uiso 1 1 calc R . . H74B H 0.0930 1.5190 0.0372 0.123 Uiso 1 1 calc R . . H74C H 0.1888 1.5744 0.0151 0.123 Uiso 1 1 calc R . . C9 C 0.1424(4) 1.7504(4) 0.8716(4) 0.0234(8) Uani 1 1 d . . . C10 C 0.0295(4) 1.6816(4) 0.7913(5) 0.0319(10) Uani 1 1 d . . . H5 H -0.0227 1.7163 0.7880 0.038 Uiso 1 1 calc R . . C24 C -0.3388(4) 1.2452(6) 0.4631(5) 0.0429(13) Uani 1 1 d . . . H1 H -0.3942 1.2304 0.4857 0.052 Uiso 1 1 calc R . . O3 O 0.1070(3) 1.9199(3) 0.9326(3) 0.0314(7) Uani 1 1 d . . . C8 C 0.1805(4) 1.8806(4) 0.9446(4) 0.0260(9) Uani 1 1 d . . . C9S C 0.3862(9) 1.0706(6) -0.2653(6) 0.085(3) Uani 1 1 d . . . H9A H 0.3052 1.0249 -0.3046 0.128 Uiso 1 1 calc R . . H9B H 0.4224 1.0188 -0.2928 0.128 Uiso 1 1 calc R . . H9C H 0.3995 1.1283 -0.2856 0.128 Uiso 1 1 calc R . . N4S N 0.6697(5) 1.0776(5) -0.3258(5) 0.0565(14) Uani 1 1 d . . . C12S C 0.6944(11) 0.9797(8) -0.3836(10) 0.102(4) Uani 1 1 d . . . H6A H 0.6659 0.9515 -0.4685 0.153 Uiso 1 1 calc R . . H6B H 0.6583 0.9174 -0.3769 0.153 Uiso 1 1 calc R . . H6C H 0.7759 1.0034 -0.3448 0.153 Uiso 1 1 calc R . . C11S C 0.6926(8) 1.1220(7) -0.2049(6) 0.071(2) Uani 1 1 d . . . H19A H 0.6733 1.1890 -0.1759 0.107 Uiso 1 1 calc R . . H19B H 0.7726 1.1463 -0.1541 0.107 Uiso 1 1 calc R . . H19C H 0.6476 1.0613 -0.2019 0.107 Uiso 1 1 calc R . . N2S N 0.5485(5) 1.5705(5) 0.3274(5) 0.0558(6) Uani 1 1 d . . . C4S C 0.5566(6) 1.4886(6) 0.2396(6) 0.0558(6) Uani 1 1 d . . . H13 H 0.5370 1.4136 0.2267 0.067 Uiso 1 1 calc R . . O4S O 0.6098(9) 1.2117(9) -0.3388(8) 0.138(4) Uani 1 1 d . . . C5S C 0.5872(6) 1.6889(6) 0.3557(6) 0.0558(6) Uani 1 1 d . . . H14A H 0.6535 1.7403 0.4355 0.084 Uiso 1 1 calc R . . H14B H 0.5273 1.7161 0.3547 0.084 Uiso 1 1 calc R . . H14C H 0.6068 1.6899 0.2959 0.084 Uiso 1 1 calc R . . C6S C 0.5060(6) 1.5491(6) 0.3977(6) 0.0558(6) Uani 1 1 d . . . H15A H 0.4880 1.4680 0.3730 0.084 Uiso 1 1 calc R . . H15B H 0.4380 1.5635 0.3857 0.084 Uiso 1 1 calc R . . H15C H 0.5629 1.6010 0.4827 0.084 Uiso 1 1 calc R . . C10S C 0.6286(7) 1.1260(8) -0.3810(7) 0.071(2) Uani 1 1 d . . . H7 H 0.6119 1.0901 -0.4624 0.086 Uiso 1 1 calc R . . 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 0.01459(19) 0.0200(2) 0.0178(2) 0.01010(16) 0.00723(16) 0.00692(15) Cd2 0.01643(15) 0.02124(15) 0.01793(15) 0.00951(12) 0.00729(12) 0.00762(11) Cd3 0.0469(3) 0.0291(3) 0.0434(3) 0.0193(2) 0.0330(3) 0.0189(2) Si1 0.0185(5) 0.0212(5) 0.0168(5) 0.0099(4) 0.0083(4) 0.0091(4) O2 0.0308(17) 0.0311(17) 0.0265(16) 0.0113(14) 0.0175(14) 0.0086(14) O1 0.0211(15) 0.0280(16) 0.0181(14) 0.0091(13) 0.0079(12) 0.0107(13) O7 0.0212(16) 0.043(2) 0.0313(18) 0.0206(16) 0.0072(14) 0.0070(14) O8 0.0210(15) 0.0361(18) 0.0279(16) 0.0174(15) 0.0085(13) 0.0104(14) O6 0.0270(16) 0.0353(18) 0.0303(17) 0.0229(15) 0.0110(14) 0.0120(14) C13 0.023(2) 0.027(2) 0.026(2) 0.0118(19) 0.0091(18) 0.0143(18) O4 0.0314(18) 0.0241(16) 0.0325(18) 0.0088(14) 0.0106(15) 0.0092(14) C5 0.0198(19) 0.025(2) 0.0177(19) 0.0108(17) 0.0090(16) 0.0106(16) C19 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C26 0.0185(19) 0.021(2) 0.0199(19) 0.0079(17) 0.0068(17) 0.0065(16) O5 0.0360(19) 0.0378(19) 0.044(2) 0.0305(17) 0.0234(17) 0.0176(15) C2 0.023(2) 0.028(2) 0.0186(19) 0.0114(18) 0.0096(17) 0.0128(17) C22 0.019(2) 0.023(2) 0.023(2) 0.0062(17) 0.0069(17) 0.0078(17) C1 0.021(2) 0.031(2) 0.020(2) 0.0126(18) 0.0090(17) 0.0121(18) C28 0.021(2) 0.044(3) 0.028(2) 0.024(2) 0.0073(19) 0.011(2) O3S 0.070(3) 0.0313(19) 0.044(2) 0.0225(18) 0.026(2) 0.0220(19) C23 0.020(2) 0.021(2) 0.021(2) 0.0073(17) 0.0056(17) 0.0068(16) C12 0.024(2) 0.0204(19) 0.0184(19) 0.0106(16) 0.0112(17) 0.0101(16) N3S 0.050(3) 0.029(2) 0.033(2) 0.0154(18) 0.021(2) 0.019(2) C15 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C16 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C4 0.027(2) 0.022(2) 0.021(2) 0.0081(17) 0.0118(18) 0.0076(17) C14 0.022(2) 0.026(2) 0.025(2) 0.0112(18) 0.0080(18) 0.0109(18) C6 0.027(2) 0.025(2) 0.026(2) 0.0139(18) 0.0136(19) 0.0095(18) C3 0.026(2) 0.025(2) 0.024(2) 0.0105(18) 0.0133(18) 0.0068(18) C7 0.026(2) 0.021(2) 0.0190(19) 0.0083(17) 0.0095(17) 0.0104(17) C27 0.022(2) 0.047(3) 0.036(3) 0.029(2) 0.014(2) 0.013(2) C7S 0.038(3) 0.031(2) 0.035(3) 0.018(2) 0.021(2) 0.015(2) C11 0.020(2) 0.028(2) 0.033(2) 0.012(2) 0.0073(19) 0.0106(18) O2S 0.0614(16) 0.0537(15) 0.0429(13) 0.0243(12) 0.0212(12) 0.0199(13) O1S 0.081(2) 0.0609(19) 0.081(2) 0.0169(16) 0.0549(19) 0.0168(16) C8S 0.063(4) 0.033(3) 0.041(3) 0.020(2) 0.031(3) 0.024(3) C21 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C20 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C25 0.024(2) 0.071(4) 0.024(2) 0.026(3) 0.009(2) 0.014(2) C1S 0.081(2) 0.0609(19) 0.081(2) 0.0169(16) 0.0549(19) 0.0168(16) C18 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) C17 0.0380(11) 0.0691(14) 0.0532(13) 0.0486(12) 0.0302(10) 0.0339(11) N1S 0.081(2) 0.0609(19) 0.081(2) 0.0169(16) 0.0549(19) 0.0168(16) C3S 0.081(2) 0.0609(19) 0.081(2) 0.0169(16) 0.0549(19) 0.0168(16) C2S 0.081(2) 0.0609(19) 0.081(2) 0.0169(16) 0.0549(19) 0.0168(16) C9 0.027(2) 0.025(2) 0.021(2) 0.0127(18) 0.0135(18) 0.0131(18) C10 0.026(2) 0.028(2) 0.039(3) 0.016(2) 0.014(2) 0.0161(19) C24 0.023(2) 0.070(4) 0.029(3) 0.024(3) 0.014(2) 0.012(2) O3 0.0396(19) 0.0289(17) 0.0334(18) 0.0156(15) 0.0229(16) 0.0223(15) C8 0.032(2) 0.027(2) 0.022(2) 0.0125(18) 0.0161(19) 0.0143(19) C9S 0.148(9) 0.046(4) 0.039(4) 0.020(3) 0.029(5) 0.040(5) N4S 0.072(4) 0.053(3) 0.048(3) 0.033(3) 0.029(3) 0.018(3) C12S 0.183(12) 0.060(5) 0.110(8) 0.056(5) 0.100(8) 0.059(6) C11S 0.092(6) 0.061(4) 0.049(4) 0.034(4) 0.028(4) 0.014(4) N2S 0.0614(16) 0.0537(15) 0.0429(13) 0.0243(12) 0.0212(12) 0.0199(13) C4S 0.0614(16) 0.0537(15) 0.0429(13) 0.0243(12) 0.0212(12) 0.0199(13) O4S 0.215(10) 0.228(10) 0.157(7) 0.161(8) 0.149(8) 0.186(9) C5S 0.0614(16) 0.0537(15) 0.0429(13) 0.0243(12) 0.0212(12) 0.0199(13) C6S 0.0614(16) 0.0537(15) 0.0429(13) 0.0243(12) 0.0212(12) 0.0199(13) C10S 0.079(5) 0.099(6) 0.060(4) 0.056(5) 0.037(4) 0.041(5) _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 O5 2.220(3) 2_576 ? Cd1 O5 2.220(3) 1_554 ? Cd1 O3 2.249(3) 2_586 ? Cd1 O3 2.249(3) 1_544 ? Cd1 O1 2.333(3) 2_575 ? Cd1 O1 2.333(3) . ? Cd2 O6 2.206(3) 1_554 ? Cd2 O4 2.265(3) 1_544 ? Cd2 O1 2.327(3) . ? Cd2 O8 2.334(3) 1_655 ? Cd2 O7 2.395(4) 1_655 ? Cd2 O2 2.488(3) . ? Cd2 C22 2.690(4) 1_655 ? Cd2 C1 2.741(4) . ? Cd3 O1S 2.239(6) . ? Cd3 O1S 2.239(6) 2_685 ? Cd3 O3S 2.268(4) 2_685 ? Cd3 O3S 2.268(4) . ? Cd3 O2S 2.310(5) 2_685 ? Cd3 O2S 2.310(5) . ? Si1 C5 1.875(4) . ? Si1 C19 1.875(5) . ? Si1 C12 1.878(4) . ? Si1 C26 1.883(4) . ? O2 C1 1.249(6) . ? O1 C1 1.285(5) . ? O7 C22 1.247(6) . ? O7 Cd2 2.395(3) 1_455 ? O8 C22 1.263(6) . ? O8 Cd2 2.334(3) 1_455 ? O6 C15 1.261(6) . ? O6 Cd2 2.206(3) 1_556 ? C13 C14 1.391(6) . ? C13 C12 1.403(6) . ? C13 H8 0.9500 . ? O4 C8 1.253(6) . ? O4 Cd2 2.265(3) 1_566 ? C5 C4 1.394(6) . ? C5 C6 1.411(6) . ? C19 C20 1.369(7) . ? C19 C18 1.395(7) . ? C26 C25 1.390(7) . ? C26 C27 1.390(6) . ? O5 C15 1.258(6) . ? O5 Cd1 2.220(3) 1_556 ? C2 C7 1.383(6) . ? C2 C3 1.399(6) . ? C2 C1 1.502(6) . ? C22 C23 1.510(6) . ? C22 Cd2 2.690(4) 1_455 ? C28 C23 1.375(6) . ? C28 C27 1.395(6) . ? C28 H20 0.9500 . ? O3S C7S 1.243(6) . ? C23 C24 1.379(7) . ? C12 C11 1.393(6) . ? N3S C7S 1.316(6) . ? N3S C8S 1.451(7) . ? N3S C9S 1.457(8) . ? C15 C16 1.504(7) . ? C16 C17 1.367(7) . ? C16 C21 1.368(7) . ? C4 C3 1.391(6) . ? C4 H28 0.9500 . ? C14 C9 1.392(6) . ? C14 H29 0.9500 . ? C6 C7 1.384(6) . ? C6 H30 0.9500 . ? C3 H31 0.9500 . ? C7 H32 0.9500 . ? C27 H34 0.9500 . ? C7S H35 0.9500 . ? C11 C10 1.394(7) . ? C11 H36 0.9500 . ? O2S C4S 1.258(8) . ? O1S C1S 1.073(10) . ? C8S H40A 0.9800 . ? C8S H40B 0.9800 . ? C8S H40C 0.9800 . ? C21 C20 1.389(7) . ? C21 H43 0.9500 . ? C20 H48 0.9500 . ? C25 C24 1.400(7) . ? C25 H49 0.9500 . ? C1S N1S 1.320(10) . ? C1S H52 0.9500 . ? C18 C17 1.391(7) . ? C18 H53 0.9500 . ? C17 H54 0.9500 . ? N1S C2S 1.425(12) . ? N1S C3S 1.438(11) . ? C3S H66A 0.9800 . ? C3S H66B 0.9800 . ? C3S H66C 0.9800 . ? C2S H74A 0.9800 . ? C2S H74B 0.9800 . ? C2S H74C 0.9800 . ? C9 C10 1.381(7) . ? C9 C8 1.507(6) . ? C10 H5 0.9500 . ? C24 H1 0.9500 . ? O3 C8 1.252(6) . ? O3 Cd1 2.249(3) 1_566 ? C9S H9A 0.9800 . ? C9S H9B 0.9800 . ? C9S H9C 0.9800 . ? N4S C10S 1.315(9) . ? N4S C11S 1.429(8) . ? N4S C12S 1.437(10) . ? C12S H6A 0.9800 . ? C12S H6B 0.9800 . ? C12S H6C 0.9800 . ? C11S H19A 0.9800 . ? C11S H19B 0.9800 . ? C11S H19C 0.9800 . ? N2S C4S 1.329(9) . ? N2S C6S 1.426(9) . ? N2S C5S 1.460(9) . ? C4S H13 0.9500 . ? O4S C10S 1.213(11) . ? C5S H14A 0.9800 . ? C5S H14B 0.9800 . ? C5S H14C 0.9800 . ? C6S H15A 0.9800 . ? C6S H15B 0.9800 . ? C6S H15C 0.9800 . ? C10S H7 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 O5 180.0 2_576 1_554 ? O5 Cd1 O3 87.21(13) 2_576 2_586 ? O5 Cd1 O3 92.79(13) 1_554 2_586 ? O5 Cd1 O3 92.79(13) 2_576 1_544 ? O5 Cd1 O3 87.21(13) 1_554 1_544 ? O3 Cd1 O3 180.0(2) 2_586 1_544 ? O5 Cd1 O1 87.58(13) 2_576 2_575 ? O5 Cd1 O1 92.42(13) 1_554 2_575 ? O3 Cd1 O1 81.61(12) 2_586 2_575 ? O3 Cd1 O1 98.39(12) 1_544 2_575 ? O5 Cd1 O1 92.42(13) 2_576 . ? O5 Cd1 O1 87.58(13) 1_554 . ? O3 Cd1 O1 98.39(12) 2_586 . ? O3 Cd1 O1 81.61(12) 1_544 . ? O1 Cd1 O1 179.999(1) 2_575 . ? O6 Cd2 O4 106.58(13) 1_554 1_544 ? O6 Cd2 O1 109.60(12) 1_554 . ? O4 Cd2 O1 102.47(12) 1_544 . ? O6 Cd2 O8 99.06(12) 1_554 1_655 ? O4 Cd2 O8 95.78(12) 1_544 1_655 ? O1 Cd2 O8 139.50(11) . 1_655 ? O6 Cd2 O7 152.90(12) 1_554 1_655 ? O4 Cd2 O7 87.21(13) 1_544 1_655 ? O1 Cd2 O7 89.26(12) . 1_655 ? O8 Cd2 O7 55.60(12) 1_655 1_655 ? O6 Cd2 O2 95.66(13) 1_554 . ? O4 Cd2 O2 153.14(12) 1_544 . ? O1 Cd2 O2 54.82(11) . . ? O8 Cd2 O2 95.34(11) 1_655 . ? O7 Cd2 O2 79.12(13) 1_655 . ? O6 Cd2 C22 126.65(14) 1_554 1_655 ? O4 Cd2 C22 90.97(13) 1_544 1_655 ? O1 Cd2 C22 115.10(13) . 1_655 ? O8 Cd2 C22 28.00(13) 1_655 1_655 ? O7 Cd2 C22 27.62(13) 1_655 1_655 ? O2 Cd2 C22 87.51(12) . 1_655 ? O6 Cd2 C1 106.01(13) 1_554 . ? O4 Cd2 C1 128.26(14) 1_544 . ? O1 Cd2 C1 27.87(12) . . ? O8 Cd2 C1 117.25(13) 1_655 . ? O7 Cd2 C1 81.40(13) 1_655 . ? O2 Cd2 C1 27.08(12) . . ? C22 Cd2 C1 100.43(14) 1_655 . ? O1S Cd3 O1S 179.999(2) . 2_685 ? O1S Cd3 O3S 84.51(18) . 2_685 ? O1S Cd3 O3S 95.49(18) 2_685 2_685 ? O1S Cd3 O3S 95.49(18) . . ? O1S Cd3 O3S 84.51(18) 2_685 . ? O3S Cd3 O3S 179.999(1) 2_685 . ? O1S Cd3 O2S 90.5(2) . 2_685 ? O1S Cd3 O2S 89.5(2) 2_685 2_685 ? O3S Cd3 O2S 88.03(16) 2_685 2_685 ? O3S Cd3 O2S 91.97(16) . 2_685 ? O1S Cd3 O2S 89.5(2) . . ? O1S Cd3 O2S 90.5(2) 2_685 . ? O3S Cd3 O2S 91.97(16) 2_685 . ? O3S Cd3 O2S 88.03(16) . . ? O2S Cd3 O2S 179.999(2) 2_685 . ? C5 Si1 C19 108.9(2) . . ? C5 Si1 C12 111.49(19) . . ? C19 Si1 C12 108.4(2) . . ? C5 Si1 C26 107.00(19) . . ? C19 Si1 C26 114.5(2) . . ? C12 Si1 C26 106.57(19) . . ? C1 O2 Cd2 87.8(3) . . ? C1 O1 Cd2 94.3(3) . . ? C1 O1 Cd1 127.6(3) . . ? Cd2 O1 Cd1 99.22(12) . . ? C22 O7 Cd2 89.5(3) . 1_455 ? C22 O8 Cd2 91.8(3) . 1_455 ? C15 O6 Cd2 120.5(3) . 1_556 ? C14 C13 C12 121.2(4) . . ? C14 C13 H8 119.4 . . ? C12 C13 H8 119.4 . . ? C8 O4 Cd2 104.6(3) . 1_566 ? C4 C5 C6 117.7(4) . . ? C4 C5 Si1 123.7(3) . . ? C6 C5 Si1 118.4(3) . . ? C20 C19 C18 115.7(5) . . ? C20 C19 Si1 121.0(4) . . ? C18 C19 Si1 122.4(4) . . ? C25 C26 C27 116.6(4) . . ? C25 C26 Si1 123.3(3) . . ? C27 C26 Si1 119.7(3) . . ? C15 O5 Cd1 137.2(3) . 1_556 ? C7 C2 C3 119.5(4) . . ? C7 C2 C1 120.8(4) . . ? C3 C2 C1 119.8(4) . . ? O7 C22 O8 123.0(4) . . ? O7 C22 C23 117.9(4) . . ? O8 C22 C23 119.0(4) . . ? O7 C22 Cd2 62.9(2) . 1_455 ? O8 C22 Cd2 60.2(2) . 1_455 ? C23 C22 Cd2 176.2(3) . 1_455 ? O2 C1 O1 122.5(4) . . ? O2 C1 C2 120.5(4) . . ? O1 C1 C2 117.1(4) . . ? O2 C1 Cd2 65.1(2) . . ? O1 C1 Cd2 57.9(2) . . ? C2 C1 Cd2 170.7(3) . . ? C23 C28 C27 120.6(4) . . ? C23 C28 H20 119.7 . . ? C27 C28 H20 119.7 . . ? C7S O3S Cd3 128.6(4) . . ? C28 C23 C24 119.2(4) . . ? C28 C23 C22 120.7(4) . . ? C24 C23 C22 120.1(4) . . ? C11 C12 C13 117.4(4) . . ? C11 C12 Si1 119.6(3) . . ? C13 C12 Si1 122.9(3) . . ? C7S N3S C8S 121.7(4) . . ? C7S N3S C9S 121.3(5) . . ? C8S N3S C9S 117.0(5) . . ? O5 C15 O6 126.4(5) . . ? O5 C15 C16 116.4(5) . . ? O6 C15 C16 117.2(4) . . ? C17 C16 C21 118.4(5) . . ? C17 C16 C15 119.5(5) . . ? C21 C16 C15 121.8(5) . . ? C3 C4 C5 121.2(4) . . ? C3 C4 H28 119.4 . . ? C5 C4 H28 119.4 . . ? C13 C14 C9 120.3(4) . . ? C13 C14 H29 119.8 . . ? C9 C14 H29 119.8 . . ? C7 C6 C5 121.0(4) . . ? C7 C6 H30 119.5 . . ? C5 C6 H30 119.5 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H31 120.0 . . ? C2 C3 H31 120.0 . . ? C2 C7 C6 120.5(4) . . ? C2 C7 H32 119.8 . . ? C6 C7 H32 119.8 . . ? C28 C27 C26 121.7(4) . . ? C28 C27 H34 119.1 . . ? C26 C27 H34 119.1 . . ? O3S C7S N3S 124.1(5) . . ? O3S C7S H35 117.9 . . ? N3S C7S H35 117.9 . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H36 119.3 . . ? C12 C11 H36 119.3 . . ? C4S O2S Cd3 134.1(5) . . ? C1S O1S Cd3 140.8(8) . . ? N3S C8S H40A 109.5 . . ? N3S C8S H40B 109.5 . . ? H40A C8S H40B 109.5 . . ? N3S C8S H40C 109.5 . . ? H40A C8S H40C 109.5 . . ? H40B C8S H40C 109.5 . . ? C16 C21 C20 120.8(5) . . ? C16 C21 H43 119.6 . . ? C20 C21 H43 119.6 . . ? C19 C20 C21 122.5(5) . . ? C19 C20 H48 118.8 . . ? C21 C20 H48 118.8 . . ? C26 C25 C24 122.1(5) . . ? C26 C25 H49 118.9 . . ? C24 C25 H49 118.9 . . ? O1S C1S N1S 131.9(11) . . ? O1S C1S H52 114.0 . . ? N1S C1S H52 114.0 . . ? C19 C18 C17 122.0(5) . . ? C19 C18 H53 119.0 . . ? C17 C18 H53 119.0 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H54 119.7 . . ? C18 C17 H54 119.7 . . ? C1S N1S C2S 127.7(8) . . ? C1S N1S C3S 115.1(9) . . ? C2S N1S C3S 117.3(7) . . ? N1S C3S H66A 109.5 . . ? N1S C3S H66B 109.5 . . ? H66A C3S H66B 109.5 . . ? N1S C3S H66C 109.5 . . ? H66A C3S H66C 109.5 . . ? H66B C3S H66C 109.5 . . ? N1S C2S H74A 109.5 . . ? N1S C2S H74B 109.5 . . ? H74A C2S H74B 109.5 . . ? N1S C2S H74C 109.5 . . ? H74A C2S H74C 109.5 . . ? H74B C2S H74C 109.5 . . ? C10 C9 C14 119.1(4) . . ? C10 C9 C8 118.5(4) . . ? C14 C9 C8 122.4(4) . . ? C9 C10 C11 120.5(4) . . ? C9 C10 H5 119.7 . . ? C11 C10 H5 119.7 . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H1 120.1 . . ? C25 C24 H1 120.1 . . ? C8 O3 Cd1 150.9(3) . 1_566 ? O3 C8 O4 123.6(4) . . ? O3 C8 C9 117.8(4) . . ? O4 C8 C9 118.6(4) . . ? N3S C9S H9A 109.5 . . ? N3S C9S H9B 109.5 . . ? H9A C9S H9B 109.5 . . ? N3S C9S H9C 109.5 . . ? H9A C9S H9C 109.5 . . ? H9B C9S H9C 109.5 . . ? C10S N4S C11S 120.7(7) . . ? C10S N4S C12S 121.6(7) . . ? C11S N4S C12S 117.7(7) . . ? N4S C12S H6A 109.5 . . ? N4S C12S H6B 109.5 . . ? H6A C12S H6B 109.5 . . ? N4S C12S H6C 109.5 . . ? H6A C12S H6C 109.5 . . ? H6B C12S H6C 109.5 . . ? N4S C11S H19A 109.5 . . ? N4S C11S H19B 109.5 . . ? H19A C11S H19B 109.5 . . ? N4S C11S H19C 109.5 . . ? H19A C11S H19C 109.5 . . ? H19B C11S H19C 109.5 . . ? C4S N2S C6S 123.1(6) . . ? C4S N2S C5S 119.0(6) . . ? C6S N2S C5S 117.9(6) . . ? O2S C4S N2S 124.1(7) . . ? O2S C4S H13 118.0 . . ? N2S C4S H13 118.0 . . ? N2S C5S H14A 109.5 . . ? N2S C5S H14B 109.5 . . ? H14A C5S H14B 109.5 . . ? N2S C5S H14C 109.5 . . ? H14A C5S H14C 109.5 . . ? H14B C5S H14C 109.5 . . ? N2S C6S H15A 109.5 . . ? N2S C6S H15B 109.5 . . ? H15A C6S H15B 109.5 . . ? N2S C6S H15C 109.5 . . ? H15A C6S H15C 109.5 . . ? H15B C6S H15C 109.5 . . ? O4S C10S N4S 126.9(8) . . ? O4S C10S H7 116.6 . . ? N4S C10S H7 116.6 . . ? 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 O6 Cd2 O2 C1 114.5(3) 1_554 . . . ? O4 Cd2 O2 C1 -31.7(4) 1_544 . . . ? O1 Cd2 O2 C1 4.5(2) . . . . ? O8 Cd2 O2 C1 -145.8(3) 1_655 . . . ? O7 Cd2 O2 C1 -92.4(3) 1_655 . . . ? C22 Cd2 O2 C1 -118.9(3) 1_655 . . . ? O6 Cd2 O1 C1 -87.3(3) 1_554 . . . ? O4 Cd2 O1 C1 159.8(3) 1_544 . . . ? O8 Cd2 O1 C1 45.1(3) 1_655 . . . ? O7 Cd2 O1 C1 72.8(3) 1_655 . . . ? O2 Cd2 O1 C1 -4.4(2) . . . . ? C22 Cd2 O1 C1 62.7(3) 1_655 . . . ? O6 Cd2 O1 Cd1 41.83(15) 1_554 . . . ? O4 Cd2 O1 Cd1 -71.06(13) 1_544 . . . ? O8 Cd2 O1 Cd1 174.23(13) 1_655 . . . ? O7 Cd2 O1 Cd1 -158.04(13) 1_655 . . . ? O2 Cd2 O1 Cd1 124.78(16) . . . . ? C22 Cd2 O1 Cd1 -168.11(12) 1_655 . . . ? C1 Cd2 O1 Cd1 129.1(3) . . . . ? O5 Cd1 O1 C1 -128.0(4) 2_576 . . . ? O5 Cd1 O1 C1 52.0(4) 1_554 . . . ? O3 Cd1 O1 C1 -40.5(4) 2_586 . . . ? O3 Cd1 O1 C1 139.5(4) 1_544 . . . ? O1 Cd1 O1 C1 175(9) 2_575 . . . ? O5 Cd1 O1 Cd2 129.26(13) 2_576 . . . ? O5 Cd1 O1 Cd2 -50.74(13) 1_554 . . . ? O3 Cd1 O1 Cd2 -143.21(12) 2_586 . . . ? O3 Cd1 O1 Cd2 36.79(12) 1_544 . . . ? O1 Cd1 O1 Cd2 72(9) 2_575 . . . ? C19 Si1 C5 C4 -122.4(4) . . . . ? C12 Si1 C5 C4 -2.8(4) . . . . ? C26 Si1 C5 C4 113.4(4) . . . . ? C19 Si1 C5 C6 61.5(4) . . . . ? C12 Si1 C5 C6 -178.9(3) . . . . ? C26 Si1 C5 C6 -62.7(4) . . . . ? C5 Si1 C19 C20 22.9(6) . . . . ? C12 Si1 C19 C20 -98.5(6) . . . . ? C26 Si1 C19 C20 142.6(5) . . . . ? C5 Si1 C19 C18 -167.8(5) . . . . ? C12 Si1 C19 C18 70.7(6) . . . . ? C26 Si1 C19 C18 -48.1(6) . . . . ? C5 Si1 C26 C25 159.9(4) . . . . ? C19 Si1 C26 C25 39.2(5) . . . . ? C12 Si1 C26 C25 -80.7(5) . . . . ? C5 Si1 C26 C27 -27.3(4) . . . . ? C19 Si1 C26 C27 -148.1(4) . . . . ? C12 Si1 C26 C27 92.1(4) . . . . ? Cd2 O7 C22 O8 2.8(5) 1_455 . . . ? Cd2 O7 C22 C23 -175.8(3) 1_455 . . . ? Cd2 O8 C22 O7 -2.8(5) 1_455 . . . ? Cd2 O8 C22 C23 175.7(3) 1_455 . . . ? Cd2 O2 C1 O1 -7.9(4) . . . . ? Cd2 O2 C1 C2 171.5(4) . . . . ? Cd2 O1 C1 O2 8.5(5) . . . . ? Cd1 O1 C1 O2 -96.6(5) . . . . ? Cd2 O1 C1 C2 -171.0(3) . . . . ? Cd1 O1 C1 C2 83.9(4) . . . . ? Cd1 O1 C1 Cd2 -105.1(3) . . . . ? C7 C2 C1 O2 -176.2(4) . . . . ? C3 C2 C1 O2 5.6(6) . . . . ? C7 C2 C1 O1 3.2(6) . . . . ? C3 C2 C1 O1 -175.0(4) . . . . ? C7 C2 C1 Cd2 -52(2) . . . . ? C3 C2 C1 Cd2 130.1(18) . . . . ? O6 Cd2 C1 O2 -70.4(3) 1_554 . . . ? O4 Cd2 C1 O2 162.4(2) 1_544 . . . ? O1 Cd2 C1 O2 -172.1(4) . . . . ? O8 Cd2 C1 O2 39.0(3) 1_655 . . . ? O7 Cd2 C1 O2 82.9(3) 1_655 . . . ? C22 Cd2 C1 O2 62.8(3) 1_655 . . . ? O6 Cd2 C1 O1 101.8(3) 1_554 . . . ? O4 Cd2 C1 O1 -25.4(3) 1_544 . . . ? O8 Cd2 C1 O1 -148.8(2) 1_655 . . . ? O7 Cd2 C1 O1 -105.0(3) 1_655 . . . ? O2 Cd2 C1 O1 172.1(4) . . . . ? C22 Cd2 C1 O1 -125.1(3) 1_655 . . . ? O6 Cd2 C1 C2 161.2(19) 1_554 . . . ? O4 Cd2 C1 C2 34.0(19) 1_544 . . . ? O1 Cd2 C1 C2 59.4(18) . . . . ? O8 Cd2 C1 C2 -89.5(19) 1_655 . . . ? O7 Cd2 C1 C2 -45.6(19) 1_655 . . . ? O2 Cd2 C1 C2 -128(2) . . . . ? C22 Cd2 C1 C2 -65.7(19) 1_655 . . . ? O1S Cd3 O3S C7S -85.7(5) . . . . ? O1S Cd3 O3S C7S 94.3(5) 2_685 . . . ? O3S Cd3 O3S C7S -15(24) 2_685 . . . ? O2S Cd3 O3S C7S -176.4(5) 2_685 . . . ? O2S Cd3 O3S C7S 3.6(5) . . . . ? C27 C28 C23 C24 1.9(8) . . . . ? C27 C28 C23 C22 -175.9(4) . . . . ? O7 C22 C23 C28 161.9(4) . . . . ? O8 C22 C23 C28 -16.7(6) . . . . ? Cd2 C22 C23 C28 60(5) 1_455 . . . ? O7 C22 C23 C24 -15.9(7) . . . . ? O8 C22 C23 C24 165.5(5) . . . . ? Cd2 C22 C23 C24 -118(5) 1_455 . . . ? C14 C13 C12 C11 -2.0(7) . . . . ? C14 C13 C12 Si1 177.2(4) . . . . ? C5 Si1 C12 C11 120.9(4) . . . . ? C19 Si1 C12 C11 -119.2(4) . . . . ? C26 Si1 C12 C11 4.5(4) . . . . ? C5 Si1 C12 C13 -58.2(4) . . . . ? C19 Si1 C12 C13 61.6(4) . . . . ? C26 Si1 C12 C13 -174.6(4) . . . . ? Cd1 O5 C15 O6 -44.3(10) 1_556 . . . ? Cd1 O5 C15 C16 137.7(5) 1_556 . . . ? Cd2 O6 C15 O5 0.6(9) 1_556 . . . ? Cd2 O6 C15 C16 178.6(4) 1_556 . . . ? O5 C15 C16 C17 17.6(9) . . . . ? O6 C15 C16 C17 -160.6(6) . . . . ? O5 C15 C16 C21 -168.5(6) . . . . ? O6 C15 C16 C21 13.3(9) . . . . ? C6 C5 C4 C3 0.9(7) . . . . ? Si1 C5 C4 C3 -175.2(4) . . . . ? C12 C13 C14 C9 0.9(7) . . . . ? C4 C5 C6 C7 -1.5(6) . . . . ? Si1 C5 C6 C7 174.8(3) . . . . ? C5 C4 C3 C2 0.4(7) . . . . ? C7 C2 C3 C4 -1.1(7) . . . . ? C1 C2 C3 C4 177.1(4) . . . . ? C3 C2 C7 C6 0.5(7) . . . . ? C1 C2 C7 C6 -177.7(4) . . . . ? C5 C6 C7 C2 0.8(7) . . . . ? C23 C28 C27 C26 -1.5(8) . . . . ? C25 C26 C27 C28 -0.1(8) . . . . ? Si1 C26 C27 C28 -173.3(4) . . . . ? Cd3 O3S C7S N3S -172.4(4) . . . . ? C8S N3S C7S O3S -178.2(5) . . . . ? C9S N3S C7S O3S 0.8(10) . . . . ? C13 C12 C11 C10 0.9(7) . . . . ? Si1 C12 C11 C10 -178.3(4) . . . . ? O1S Cd3 O2S C4S 11.7(6) . . . . ? O1S Cd3 O2S C4S -168.3(6) 2_685 . . . ? O3S Cd3 O2S C4S 96.2(6) 2_685 . . . ? O3S Cd3 O2S C4S -83.8(6) . . . . ? O2S Cd3 O2S C4S 91(50) 2_685 . . . ? O1S Cd3 O1S C1S 173(71) 2_685 . . . ? O3S Cd3 O1S C1S -121.5(10) 2_685 . . . ? O3S Cd3 O1S C1S 58.5(10) . . . . ? O2S Cd3 O1S C1S 150.5(10) 2_685 . . . ? O2S Cd3 O1S C1S -29.5(10) . . . . ? C17 C16 C21 C20 -2.5(10) . . . . ? C15 C16 C21 C20 -176.4(6) . . . . ? C18 C19 C20 C21 2.8(10) . . . . ? Si1 C19 C20 C21 172.7(5) . . . . ? C16 C21 C20 C19 1.0(10) . . . . ? C27 C26 C25 C24 1.3(8) . . . . ? Si1 C26 C25 C24 174.3(5) . . . . ? Cd3 O1S C1S N1S 164.4(7) . . . . ? C20 C19 C18 C17 -5.1(10) . . . . ? Si1 C19 C18 C17 -174.9(5) . . . . ? C21 C16 C17 C18 0.1(10) . . . . ? C15 C16 C17 C18 174.2(6) . . . . ? C19 C18 C17 C16 3.8(10) . . . . ? O1S C1S N1S C2S 7.4(17) . . . . ? O1S C1S N1S C3S -171.4(10) . . . . ? C13 C14 C9 C10 1.4(7) . . . . ? C13 C14 C9 C8 -175.7(4) . . . . ? C14 C9 C10 C11 -2.5(7) . . . . ? C8 C9 C10 C11 174.8(4) . . . . ? C12 C11 C10 C9 1.3(8) . . . . ? C28 C23 C24 C25 -0.7(8) . . . . ? C22 C23 C24 C25 177.1(5) . . . . ? C26 C25 C24 C23 -0.9(10) . . . . ? Cd1 O3 C8 O4 -77.2(8) 1_566 . . . ? Cd1 O3 C8 C9 104.4(6) 1_566 . . . ? Cd2 O4 C8 O3 7.4(5) 1_566 . . . ? Cd2 O4 C8 C9 -174.2(3) 1_566 . . . ? C10 C9 C8 O3 3.0(6) . . . . ? C14 C9 C8 O3 -179.8(4) . . . . ? C10 C9 C8 O4 -175.4(4) . . . . ? C14 C9 C8 O4 1.7(6) . . . . ? Cd3 O2S C4S N2S -83.8(8) . . . . ? C6S N2S C4S O2S 176.3(6) . . . . ? C5S N2S C4S O2S -5.2(10) . . . . ? C11S N4S C10S O4S 2.9(15) . . . . ? C12S N4S C10S O4S -176.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.280 _refine_diff_density_min -2.316 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 942375' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p21c_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn4O2 Zn3O4 Zn2O (C28 H16 O8 Si)2 (C28 H17 O8 Si)2' _chemical_formula_sum 'C112 H66 O39 Si4 Zn9' _chemical_formula_weight 2736.34 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 38.22(2) _cell_length_b 29.788(19) _cell_length_c 25.377(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.005(8) _cell_angle_gamma 90.00 _cell_volume 28536(30) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.1948 _cell_measurement_theta_max 16.3619 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5504 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7968 _exptl_absorpt_correction_T_max 0.8575 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 346308 _diffrn_reflns_av_R_equivalents 0.1245 _diffrn_reflns_av_sigmaI/netI 0.2692 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.56 _reflns_number_total 72070 _reflns_number_gt 16081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0380P)^2^+0.5000P] 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 72070 _refine_ls_number_parameters 613 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.2487 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.002 _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 Zn1 Zn 0.450049(15) 0.445127(17) 0.75668(2) 0.06380(18) Uani 1 1 d . . . Zn2 Zn 0.521194(15) 0.392759(18) 0.74051(2) 0.06872(19) Uani 1 1 d . . . Zn3 Zn 0.841248(19) 0.60239(2) 0.91065(3) 0.1062(3) Uani 1 1 d . . . Zn4 Zn 0.840079(18) 0.54059(2) 1.01952(3) 0.0970(2) Uani 1 1 d . . . Zn5 Zn 0.446954(15) 0.393535(18) 0.64905(2) 0.06572(18) Uani 1 1 d . . . Zn6 Zn 0.451211(16) 0.344799(18) 0.75959(2) 0.07070(19) Uani 1 1 d . . . Zn7 Zn 0.140418(19) 0.14935(2) 0.46960(3) 0.1050(3) Uani 1 1 d . . . Zn8 Zn 0.16750(2) 0.63330(3) 0.52557(4) 0.1259(3) Uani 1 1 d . . . Zn9 Zn 0.91676(2) 0.40719(3) 0.47150(4) 0.1513(4) Uani 1 1 d . . . Si1 Si 0.61742(4) 0.61419(4) 0.93473(5) 0.0618(4) Uani 1 1 d . . . Si2 Si 0.21946(4) 0.37708(6) 0.67181(7) 0.0926(5) Uani 1 1 d . . . Si3 Si 0.92190(5) 0.34521(7) 0.80892(8) 0.1257(7) Uani 1 1 d . . . Si4 Si 0.39302(4) 0.67376(5) 0.54746(6) 0.0823(5) Uani 1 1 d . . . O1S O 0.46989(7) 0.39325(8) 0.72514(12) 0.0649(9) Uani 1 1 d . . . O1 O 0.54358(8) 0.44880(10) 0.76794(13) 0.0852(11) Uani 1 1 d . . . O2 O 0.49495(9) 0.47607(10) 0.79489(12) 0.0747(5) Uani 1 1 d . . . O2S O 0.86313(9) 0.59453(11) 0.99111(13) 0.0967(12) Uani 1 1 d . . . O3 O 0.56094(8) 0.56734(10) 1.17310(12) 0.0744(5) Uani 1 1 d . . . O3S O 0.82097(15) 0.61573(17) 0.8232(2) 0.1952(10) Uani 1 1 d . . . O4 O 0.57339(10) 0.64205(11) 1.18124(14) 0.1014(12) Uani 1 1 d . . . O4S O 0.88651(15) 0.64146(17) 0.9044(2) 0.1952(10) Uani 1 1 d . . . O5 O 0.55406(9) 0.82256(10) 0.85736(12) 0.0810(10) Uani 1 1 d . . . O5S O 0.84475(15) 0.48264(17) 1.0650(2) 0.1952(10) Uani 1 1 d . . . O6 O 0.57592(9) 0.79977(10) 0.78536(13) 0.0829(6) Uani 1 1 d . . . O7S O 0.45953(15) 0.39288(17) 0.5753(2) 0.1952(10) Uani 1 1 d . . . O7 O 0.78904(8) 0.54920(12) 0.99709(13) 0.1017(12) Uani 1 1 d D . . O8 O 0.79263(9) 0.58215(15) 0.91735(15) 0.1286(15) Uani 1 1 d D . . O9 O 0.16061(10) 0.42927(13) 0.90357(14) 0.1045(7) Uani 1 1 d . . . O10 O 0.17581(10) 0.35841(14) 0.92046(17) 0.1212(14) Uani 1 1 d . . . O11 O 0.39511(8) 0.39165(10) 0.65034(15) 0.0936(11) Uani 1 1 d . . . O12 O 0.39544(9) 0.42167(14) 0.72820(15) 0.1089(7) Uani 1 1 d . . . O13 O 0.18285(14) 0.16585(14) 0.57392(19) 0.182(2) Uani 1 1 d D . . O14 O 0.15133(11) 0.20561(12) 0.50609(15) 0.1204(14) Uani 1 1 d D . . O15 O 0.11641(15) 0.54404(18) 0.5543(2) 0.160(2) Uani 1 1 d . . . O16 O 0.16660(16) 0.56915(18) 0.5433(2) 0.157(2) Uani 1 1 d . . . O17 O 0.85854(10) 0.54238(14) 0.89007(15) 0.1173(14) Uani 1 1 d . . . O18 O 0.85253(11) 0.49905(13) 0.95957(17) 0.1218(8) Uani 1 1 d . . . O19 O 0.85985(15) 0.35434(17) 0.54508(19) 0.171(2) Uani 1 1 d . . . O20 O 0.90823(14) 0.3900(2) 0.5436(2) 0.174(2) Uani 1 1 d . . . O21 O 0.90642(14) 0.14744(17) 0.9396(2) 0.1703(19) Uani 1 1 d . . . O22 O 0.84950(14) 0.16720(17) 0.9177(2) 0.1722(7) Uani 1 1 d . . . O23 O 1.09500(13) 0.34275(17) 0.9220(2) 0.1722(7) Uani 1 1 d D . . O24 O 1.07512(12) 0.34423(16) 0.99331(18) 0.1722(7) Uani 1 1 d D . . H24B H 1.0930 0.3595 1.0058 0.258 Uiso 1 1 calc R . . O25 O 0.44584(9) 0.46426(11) 0.63936(13) 0.0852(6) Uani 1 1 d . . . O26 O 0.43766(10) 0.49825(10) 0.71438(15) 0.1096(13) Uani 1 1 d . . . O27 O 0.21668(11) 0.64116(15) 0.5324(2) 0.1497(8) Uani 1 1 d . . . O28 O 0.21446(11) 0.71087(15) 0.5056(2) 0.1497(8) Uani 1 1 d . . . O29 O 0.50865(13) 0.80774(15) 0.70133(19) 0.1480(7) Uani 1 1 d . . . O30 O 0.46303(9) 0.85132(13) 0.70109(15) 0.1057(13) Uani 1 1 d . . . O31 O 0.40429(11) 0.63204(14) 0.28288(17) 0.1480(7) Uani 1 1 d D . . H31A H 0.4127 0.6346 0.2544 0.222 Uiso 1 1 calc R . . O32 O 0.46130(12) 0.62733(14) 0.32286(18) 0.1480(7) Uani 1 1 d D . . O6S O 0.96952(15) 0.41695(17) 0.4840(2) 0.1952(10) Uani 1 1 d . . . C1 C 0.52728(15) 0.47527(17) 0.7957(2) 0.0747(5) Uani 1 1 d . . . C2 C 0.55016(8) 0.51030(9) 0.82494(11) 0.0747(5) Uani 1 1 d G . . C3 C 0.58685(8) 0.50644(9) 0.83397(12) 0.0747(5) Uani 1 1 d G . . H3A H 0.5980 0.4825 0.8182 0.090 Uiso 1 1 calc R . . C4 C 0.60724(6) 0.53758(10) 0.86606(12) 0.0747(5) Uani 1 1 d G . . H4A H 0.6323 0.5349 0.8722 0.090 Uiso 1 1 calc R . . C5 C 0.59093(8) 0.57258(9) 0.88912(11) 0.0747(5) Uani 1 1 d G . . C6 C 0.55424(8) 0.57644(9) 0.88009(12) 0.0747(5) Uani 1 1 d G . . H6A H 0.5431 0.6004 0.8959 0.090 Uiso 1 1 calc R . . C7 C 0.53385(6) 0.54530(10) 0.84800(12) 0.0747(5) Uani 1 1 d G . . H7A H 0.5088 0.5479 0.8418 0.090 Uiso 1 1 calc R . . C11 C 0.57178(13) 0.60376(19) 1.1563(2) 0.0744(5) Uani 1 1 d . . . C12 C 0.58613(8) 0.60494(11) 1.10455(10) 0.0744(5) Uani 1 1 d G . . C13 C 0.57511(7) 0.57182(9) 1.06702(13) 0.0744(5) Uani 1 1 d G . . H13A H 0.5609 0.5477 1.0758 0.089 Uiso 1 1 calc R . . C14 C 0.58492(8) 0.57407(9) 1.01661(11) 0.0744(5) Uani 1 1 d G . . H14A H 0.5774 0.5514 0.9910 0.089 Uiso 1 1 calc R . . C15 C 0.60575(8) 0.60943(10) 1.00372(10) 0.0744(5) Uani 1 1 d G . . C16 C 0.61678(8) 0.64255(9) 1.04125(13) 0.0744(5) Uani 1 1 d G . . H16A H 0.6310 0.6667 1.0324 0.089 Uiso 1 1 calc R . . C17 C 0.60696(8) 0.64030(9) 1.09167(11) 0.0744(5) Uani 1 1 d G . . H17A H 0.6145 0.6629 1.1173 0.089 Uiso 1 1 calc R . . C21 C 0.56913(15) 0.79651(17) 0.8323(2) 0.0829(6) Uani 1 1 d . . . C22 C 0.58267(9) 0.75260(8) 0.85785(12) 0.0829(6) Uani 1 1 d G . . C23 C 0.57808(9) 0.74411(9) 0.91019(12) 0.0829(6) Uani 1 1 d G . . H23A H 0.5674 0.7661 0.9297 0.099 Uiso 1 1 calc R . . C24 C 0.58908(9) 0.70343(10) 0.93405(10) 0.0829(6) Uani 1 1 d G . . H24A H 0.5859 0.6976 0.9698 0.099 Uiso 1 1 calc R . . C25 C 0.60468(9) 0.67124(8) 0.90556(12) 0.0829(6) Uani 1 1 d G . . C26 C 0.60927(9) 0.67973(9) 0.85322(12) 0.0829(6) Uani 1 1 d G . . H26A H 0.6199 0.6577 0.8337 0.099 Uiso 1 1 calc R . . C27 C 0.59826(9) 0.72041(10) 0.82936(10) 0.0829(6) Uani 1 1 d G . . H27A H 0.6014 0.7262 0.7936 0.099 Uiso 1 1 calc R . . C31 C 0.77547(7) 0.56791(14) 0.95327(15) 0.0952(7) Uani 1 1 d D . . C32 C 0.73697(6) 0.58120(10) 0.94623(13) 0.0952(7) Uani 1 1 d GD . . C33 C 0.72194(9) 0.61203(11) 0.90817(12) 0.0952(7) Uani 1 1 d GD . . H33A H 0.7361 0.6258 0.8851 0.114 Uiso 1 1 calc R . . C34 C 0.68620(9) 0.62272(10) 0.90389(12) 0.0952(7) Uani 1 1 d GD . . H34A H 0.6759 0.6438 0.8779 0.114 Uiso 1 1 calc R . . C35 C 0.66551(6) 0.60260(11) 0.93767(14) 0.0952(7) Uani 1 1 d GD . . C36 C 0.68054(9) 0.57178(11) 0.97572(13) 0.0952(7) Uani 1 1 d GD . . H36A H 0.6664 0.5580 0.9988 0.114 Uiso 1 1 calc R . . C37 C 0.71627(9) 0.56108(10) 0.98000(12) 0.0952(7) Uani 1 1 d GD . . H37A H 0.7266 0.5400 1.0060 0.114 Uiso 1 1 calc R . . C41 C 0.17326(16) 0.3921(3) 0.8911(3) 0.1045(7) Uani 1 1 d . . . C42 C 0.18448(10) 0.38847(14) 0.84089(12) 0.1045(7) Uani 1 1 d G . . C43 C 0.18057(9) 0.42501(10) 0.80641(16) 0.1045(7) Uani 1 1 d G . . H43A H 0.1707 0.4522 0.8169 0.125 Uiso 1 1 calc R . . C44 C 0.19113(10) 0.42174(11) 0.75656(14) 0.1045(7) Uani 1 1 d G . . H44A H 0.1885 0.4467 0.7330 0.125 Uiso 1 1 calc R . . C45 C 0.20561(10) 0.38192(14) 0.74121(12) 0.1045(7) Uani 1 1 d G . . C46 C 0.20953(9) 0.34538(10) 0.77569(16) 0.1045(7) Uani 1 1 d G . . H46A H 0.2194 0.3182 0.7652 0.125 Uiso 1 1 calc R . . C47 C 0.19896(9) 0.34865(11) 0.82554(14) 0.1045(7) Uani 1 1 d G . . H47A H 0.2016 0.3237 0.8491 0.125 Uiso 1 1 calc R . . C51 C 0.37896(16) 0.4019(2) 0.6896(3) 0.1089(7) Uani 1 1 d . . . C52 C 0.34187(7) 0.39522(13) 0.68545(16) 0.1089(7) Uani 1 1 d G . . C53 C 0.32292(9) 0.37361(13) 0.64146(13) 0.1089(7) Uani 1 1 d G . . H53A H 0.3348 0.3632 0.6136 0.131 Uiso 1 1 calc R . . C54 C 0.28663(9) 0.36715(13) 0.63831(13) 0.1089(7) Uani 1 1 d G . . H54A H 0.2737 0.3524 0.6082 0.131 Uiso 1 1 calc R . . C55 C 0.26929(7) 0.38231(13) 0.67915(16) 0.1089(7) Uani 1 1 d G . . C56 C 0.28824(9) 0.40393(13) 0.72314(13) 0.1089(7) Uani 1 1 d G . . H56A H 0.2764 0.4143 0.7511 0.131 Uiso 1 1 calc R . . C57 C 0.32453(9) 0.41038(12) 0.72629(13) 0.1089(7) Uani 1 1 d G . . H57A H 0.3375 0.4252 0.7564 0.131 Uiso 1 1 calc R . . C61 C 0.17079(17) 0.20216(11) 0.5514(2) 0.1248(9) Uani 1 1 d D . . C62 C 0.18280(11) 0.24461(11) 0.58118(17) 0.1248(9) Uani 1 1 d GD . . C63 C 0.20190(11) 0.24293(10) 0.63248(17) 0.1248(9) Uani 1 1 d G . . H63A H 0.2075 0.2148 0.6492 0.150 Uiso 1 1 calc R . . C64 C 0.21278(10) 0.28246(14) 0.65923(13) 0.1248(9) Uani 1 1 d G . . H64A H 0.2258 0.2813 0.6943 0.150 Uiso 1 1 calc R . . C65 C 0.20456(10) 0.32367(11) 0.63469(16) 0.1248(9) Uani 1 1 d G . . C66 C 0.18547(11) 0.32535(11) 0.58340(16) 0.1248(9) Uani 1 1 d G . . H66A H 0.1799 0.3535 0.5666 0.150 Uiso 1 1 calc R . . C67 C 0.17459(10) 0.28582(15) 0.55664(12) 0.1248(9) Uani 1 1 d G . . H67A H 0.1615 0.2870 0.5216 0.150 Uiso 1 1 calc R . . C71 C 0.1473(3) 0.5378(4) 0.5600(5) 0.170(4) Uani 1 1 d . . . C72 C 0.1647(2) 0.49839(19) 0.57991(17) 0.109(2) Uani 1 1 d G . . C73 C 0.20141(19) 0.49440(18) 0.58838(19) 0.132(3) Uani 1 1 d G . . H73A H 0.2156 0.5173 0.5764 0.158 Uiso 1 1 calc R . . C74 C 0.21740(10) 0.4569(2) 0.6144(2) 0.114(2) Uani 1 1 d G . . H74A H 0.2425 0.4542 0.6202 0.137 Uiso 1 1 calc R . . C75 C 0.1967(2) 0.42339(16) 0.63202(17) 0.099(2) Uani 1 1 d G . . C76 C 0.16001(19) 0.4274(2) 0.6236(2) 0.149(3) Uani 1 1 d G . . H76A H 0.1459 0.4045 0.6356 0.179 Uiso 1 1 calc R . . C77 C 0.14403(10) 0.4649(3) 0.5975(2) 0.137(3) Uani 1 1 d G . . H77A H 0.1190 0.4676 0.5917 0.165 Uiso 1 1 calc R . . C81 C 0.85669(18) 0.5052(3) 0.9141(3) 0.1218(8) Uani 1 1 d . . . C82 C 0.87081(10) 0.46454(13) 0.88675(17) 0.1218(8) Uani 1 1 d G . . C83 C 0.88093(10) 0.46894(11) 0.83673(17) 0.1218(8) Uani 1 1 d G . . H83A H 0.8793 0.4973 0.8194 0.146 Uiso 1 1 calc R . . C84 C 0.89347(10) 0.43188(16) 0.81213(12) 0.1218(8) Uani 1 1 d G . . H84A H 0.9004 0.4349 0.7779 0.146 Uiso 1 1 calc R . . C85 C 0.89589(10) 0.39041(12) 0.83754(17) 0.1218(8) Uani 1 1 d G . . C86 C 0.88576(10) 0.38600(11) 0.88757(17) 0.1218(8) Uani 1 1 d G . . H86A H 0.8874 0.3577 0.9049 0.146 Uiso 1 1 calc R . . C87 C 0.87322(10) 0.42306(16) 0.91217(12) 0.1218(8) Uani 1 1 d G . . H87A H 0.8663 0.4201 0.9464 0.146 Uiso 1 1 calc R . . C91 C 0.8894(3) 0.3688(4) 0.5694(4) 0.1722(7) Uani 1 1 d . . . C92 C 0.89765(16) 0.36058(18) 0.62451(16) 0.1722(7) Uani 1 1 d G . . C93 C 0.92772(13) 0.37992(15) 0.6536(2) 0.1722(7) Uani 1 1 d G . . H93A H 0.9433 0.3971 0.6359 0.207 Uiso 1 1 calc R . . C94 C 0.93497(11) 0.37419(16) 0.7086(2) 0.1722(7) Uani 1 1 d G . . H94A H 0.9555 0.3874 0.7284 0.207 Uiso 1 1 calc R . . C95 C 0.91213(16) 0.34912(18) 0.73449(16) 0.1722(7) Uani 1 1 d G . . C96 C 0.88206(13) 0.32977(15) 0.7054(2) 0.1722(7) Uani 1 1 d G . . H96A H 0.8665 0.3126 0.7231 0.207 Uiso 1 1 calc R . . C97 C 0.87481(11) 0.33550(16) 0.6504(2) 0.1722(7) Uani 1 1 d G . . H97A H 0.8543 0.3223 0.6306 0.207 Uiso 1 1 calc R . . C101 C 0.8822(3) 0.1722(2) 0.9151(3) 0.1722(7) Uani 1 1 d D . . C102 C 0.88942(17) 0.21230(15) 0.88207(19) 0.1722(7) Uani 1 1 d GD . . C103 C 0.86318(10) 0.2429(2) 0.8621(2) 0.1722(7) Uani 1 1 d G . . H10A H 0.8391 0.2368 0.8649 0.207 Uiso 1 1 calc R . . C104 C 0.87212(14) 0.28226(17) 0.83805(19) 0.1722(7) Uani 1 1 d G . . H10B H 0.8542 0.3031 0.8244 0.207 Uiso 1 1 calc R . . C105 C 0.90730(17) 0.29109(15) 0.83394(19) 0.1722(7) Uani 1 1 d G . . C106 C 0.93354(10) 0.2605(2) 0.8539(2) 0.1722(7) Uani 1 1 d G . . H10C H 0.9576 0.2666 0.8511 0.207 Uiso 1 1 calc R . . C107 C 0.92460(14) 0.22114(17) 0.87796(19) 0.1722(7) Uani 1 1 d G . . H10D H 0.9425 0.2003 0.8916 0.207 Uiso 1 1 calc R . . C111 C 1.06740(12) 0.3514(3) 0.94282(18) 0.1722(7) Uani 1 1 d D . . C112 C 1.03576(11) 0.34960(17) 0.8990(2) 0.1722(7) Uani 1 1 d GD . . C113 C 1.00701(17) 0.36608(16) 0.92049(16) 0.1722(7) Uani 1 1 d G . . H11A H 1.0102 0.3768 0.9562 0.207 Uiso 1 1 calc R . . C114 C 0.97356(13) 0.36689(16) 0.8897(2) 0.1722(7) Uani 1 1 d G . . H11B H 0.9539 0.3782 0.9044 0.207 Uiso 1 1 calc R . . C115 C 0.96887(10) 0.35123(17) 0.8375(2) 0.1722(7) Uani 1 1 d G . . C116 C 0.99762(16) 0.33475(16) 0.81604(16) 0.1722(7) Uani 1 1 d G . . H11C H 0.9944 0.3240 0.7803 0.207 Uiso 1 1 calc R . . C117 C 1.03107(12) 0.33394(15) 0.8468(2) 0.1722(7) Uani 1 1 d G . . H11D H 1.0507 0.3227 0.8322 0.207 Uiso 1 1 calc R . . C121 C 0.43887(15) 0.49637(18) 0.6622(2) 0.0852(6) Uani 1 1 d . . . C122 C 0.42742(9) 0.53988(8) 0.63584(13) 0.0852(6) Uani 1 1 d G . . C123 C 0.42419(9) 0.54179(9) 0.58056(13) 0.0852(6) Uani 1 1 d G . . H12A H 0.4286 0.5158 0.5610 0.102 Uiso 1 1 calc R . . C124 C 0.41457(9) 0.58179(11) 0.55397(10) 0.0852(6) Uani 1 1 d G . . H12B H 0.4124 0.5831 0.5162 0.102 Uiso 1 1 calc R . . C125 C 0.40819(9) 0.61987(8) 0.58266(13) 0.0852(6) Uani 1 1 d G . . C126 C 0.41142(9) 0.61796(9) 0.63794(13) 0.0852(6) Uani 1 1 d G . . H12C H 0.4071 0.6440 0.6575 0.102 Uiso 1 1 calc R . . C127 C 0.42103(9) 0.57796(11) 0.66453(10) 0.0852(6) Uani 1 1 d G . . H12D H 0.4232 0.5767 0.7023 0.102 Uiso 1 1 calc R . . C131 C 0.2300(2) 0.6751(3) 0.5205(3) 0.1497(8) Uani 1 1 d . . . C132 C 0.27020(8) 0.67830(17) 0.52834(19) 0.1497(8) Uani 1 1 d G . . C133 C 0.28870(12) 0.64056(13) 0.54947(19) 0.1497(8) Uani 1 1 d G . . H13B H 0.2762 0.6152 0.5595 0.180 Uiso 1 1 calc R . . C134 C 0.32548(12) 0.63997(13) 0.55595(18) 0.1497(8) Uani 1 1 d G . . H13C H 0.3381 0.6142 0.5704 0.180 Uiso 1 1 calc R . . C135 C 0.34378(8) 0.67710(17) 0.54129(19) 0.1497(8) Uani 1 1 d G . . C136 C 0.32528(12) 0.71483(13) 0.52015(19) 0.1497(8) Uani 1 1 d G . . H13D H 0.3378 0.7402 0.5101 0.180 Uiso 1 1 calc R . . C137 C 0.28849(12) 0.71543(13) 0.51367(18) 0.1497(8) Uani 1 1 d G . . H13E H 0.2758 0.7412 0.4992 0.180 Uiso 1 1 calc R . . C141 C 0.4762(2) 0.8171(3) 0.6873(3) 0.1480(7) Uani 1 1 d . . . C142 C 0.45716(13) 0.78373(14) 0.64991(16) 0.1480(7) Uani 1 1 d G . . C143 C 0.42123(13) 0.79064(12) 0.63265(18) 0.1480(7) Uani 1 1 d G . . H14B H 0.4102 0.8175 0.6419 0.178 Uiso 1 1 calc R . . C144 C 0.40137(9) 0.75823(17) 0.60188(18) 0.1480(7) Uani 1 1 d G . . H14C H 0.3768 0.7630 0.5901 0.178 Uiso 1 1 calc R . . C145 C 0.41745(13) 0.71892(14) 0.58837(16) 0.1480(7) Uani 1 1 d G . . C146 C 0.45338(13) 0.71201(12) 0.60564(18) 0.1480(7) Uani 1 1 d G . . H14D H 0.4644 0.6851 0.5964 0.178 Uiso 1 1 calc R . . C147 C 0.47324(9) 0.74442(17) 0.63641(18) 0.1480(7) Uani 1 1 d G . . H14E H 0.4978 0.7397 0.6482 0.178 Uiso 1 1 calc R . . C151 C 0.42910(13) 0.6383(2) 0.32294(14) 0.1480(7) Uani 1 1 d D . . C152 C 0.42412(15) 0.64664(14) 0.37996(15) 0.1480(7) Uani 1 1 d GD . . C153 C 0.45122(10) 0.65188(14) 0.4229(2) 0.1480(7) Uani 1 1 d G . . H15A H 0.4752 0.6476 0.4182 0.178 Uiso 1 1 calc R . . C154 C 0.44328(12) 0.66334(14) 0.47281(17) 0.1480(7) Uani 1 1 d G . . H15B H 0.4618 0.6669 0.5022 0.178 Uiso 1 1 calc R . . C155 C 0.40824(15) 0.66955(14) 0.47975(15) 0.1480(7) Uani 1 1 d G . . C156 C 0.38115(10) 0.66431(13) 0.4368(2) 0.1480(7) Uani 1 1 d G . . H15C H 0.3572 0.6686 0.4415 0.178 Uiso 1 1 calc R . . C157 C 0.38908(12) 0.65286(14) 0.38689(17) 0.1480(7) Uani 1 1 d G . . H15D H 0.3706 0.6493 0.3575 0.178 Uiso 1 1 calc R . . 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 Zn1 0.0799(4) 0.0515(4) 0.0620(4) -0.0119(3) 0.0174(3) -0.0083(3) Zn2 0.0851(5) 0.0540(4) 0.0682(4) -0.0182(3) 0.0158(3) -0.0079(4) Zn3 0.1059(6) 0.1124(6) 0.0994(6) 0.0245(5) 0.0136(4) 0.0032(5) Zn4 0.0914(5) 0.1070(6) 0.0906(5) 0.0144(4) 0.0081(4) 0.0195(4) Zn5 0.0798(4) 0.0532(4) 0.0663(4) -0.0153(3) 0.0184(3) -0.0091(3) Zn6 0.0871(5) 0.0515(4) 0.0749(5) -0.0185(3) 0.0171(4) -0.0055(3) Zn7 0.1017(6) 0.1081(6) 0.1027(6) -0.0217(5) 0.0081(5) -0.0111(5) Zn8 0.1010(6) 0.1244(7) 0.1471(8) 0.0016(6) 0.0040(6) -0.0011(5) Zn9 0.1104(7) 0.1529(9) 0.1882(11) 0.0073(7) 0.0157(7) -0.0061(6) Si1 0.0840(11) 0.0367(8) 0.0621(10) 0.0041(7) 0.0032(8) -0.0007(7) Si2 0.0796(12) 0.0923(13) 0.1043(14) -0.0144(11) 0.0092(11) -0.0169(10) Si3 0.1153(16) 0.1211(16) 0.1294(18) 0.0011(13) -0.0158(13) 0.0006(13) Si4 0.1085(13) 0.0620(10) 0.0812(12) -0.0016(9) 0.0297(10) -0.0082(9) O1S 0.079(2) 0.0255(16) 0.098(3) -0.0138(17) 0.0372(19) -0.0037(16) O1 0.096(3) 0.067(2) 0.096(3) -0.032(2) 0.023(2) -0.014(2) O2 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) O2S 0.096(3) 0.108(3) 0.082(3) -0.002(2) 0.002(2) 0.019(2) O3 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) O3S 0.251(3) 0.176(2) 0.172(2) 0.0424(17) 0.077(2) 0.0060(19) O4 0.148(3) 0.067(2) 0.098(3) -0.008(2) 0.047(3) -0.022(2) O4S 0.251(3) 0.176(2) 0.172(2) 0.0424(17) 0.077(2) 0.0060(19) O5 0.116(3) 0.065(2) 0.072(2) 0.0203(19) 0.045(2) 0.027(2) O5S 0.251(3) 0.176(2) 0.172(2) 0.0424(17) 0.077(2) 0.0060(19) O6 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) O7S 0.251(3) 0.176(2) 0.172(2) 0.0424(17) 0.077(2) 0.0060(19) O7 0.073(3) 0.132(3) 0.097(3) 0.012(2) 0.003(2) 0.024(2) O8 0.074(3) 0.190(4) 0.123(4) 0.035(3) 0.019(2) 0.007(3) O9 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) O10 0.110(3) 0.139(4) 0.132(4) 0.031(3) 0.075(3) 0.034(3) O11 0.074(3) 0.070(2) 0.139(3) -0.035(2) 0.026(2) -0.021(2) O12 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) O13 0.241(6) 0.093(3) 0.182(5) -0.019(3) -0.063(4) -0.001(4) O14 0.144(4) 0.105(3) 0.113(3) -0.038(3) 0.024(3) -0.041(3) O15 0.132(4) 0.162(5) 0.164(5) 0.008(3) -0.046(4) 0.022(4) O16 0.163(6) 0.116(5) 0.200(5) 0.037(4) 0.056(4) 0.054(4) O17 0.146(4) 0.102(3) 0.101(3) 0.000(3) 0.011(3) 0.038(3) O18 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) O19 0.187(5) 0.183(5) 0.126(4) 0.040(4) -0.029(4) -0.043(4) O20 0.164(5) 0.202(6) 0.144(5) -0.039(4) -0.011(4) 0.018(4) O21 0.177(5) 0.125(4) 0.208(5) 0.012(4) 0.026(4) -0.005(4) O22 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) O23 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) O24 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) O25 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) O26 0.182(4) 0.051(2) 0.095(3) 0.001(2) 0.019(3) 0.028(2) O27 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) O28 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) O29 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) O30 0.096(3) 0.108(3) 0.104(3) -0.020(3) -0.012(2) -0.003(2) O31 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) O32 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) O6S 0.251(3) 0.176(2) 0.172(2) 0.0424(17) 0.077(2) 0.0060(19) C1 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C2 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C3 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C4 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C5 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C6 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C7 0.0799(14) 0.0666(12) 0.0751(13) -0.0191(9) 0.0040(12) -0.0017(12) C11 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C12 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C13 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C14 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C15 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C16 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C17 0.0954(14) 0.0545(12) 0.0732(13) -0.0009(10) 0.0130(11) -0.0091(10) C21 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C22 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C23 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C24 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C25 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C26 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C27 0.1222(15) 0.0536(11) 0.0765(15) 0.0184(11) 0.0272(13) 0.0314(10) C31 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C32 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C33 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C34 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C35 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C36 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C37 0.0880(18) 0.1044(19) 0.0928(19) 0.0254(13) 0.0127(15) 0.0157(15) C41 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C42 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C43 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C44 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C45 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C46 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C47 0.1132(17) 0.0987(17) 0.1032(18) 0.0033(14) 0.0220(14) 0.0060(14) C51 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C52 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C53 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C54 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C55 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C56 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C57 0.0747(15) 0.160(2) 0.0931(18) -0.0234(14) 0.0161(13) -0.0204(14) C61 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C62 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C63 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C64 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C65 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C66 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C67 0.142(2) 0.0923(19) 0.132(2) -0.0212(18) -0.0022(18) -0.0198(19) C71 0.086(8) 0.190(12) 0.219(12) -0.011(9) -0.021(8) 0.007(8) C72 0.127(8) 0.116(7) 0.078(5) -0.011(5) -0.001(5) 0.019(6) C73 0.089(6) 0.133(7) 0.177(8) 0.029(6) 0.036(5) -0.013(5) C74 0.079(5) 0.091(5) 0.161(7) -0.018(5) -0.021(5) 0.012(5) C75 0.091(6) 0.089(5) 0.117(5) -0.036(4) 0.020(5) -0.031(5) C76 0.087(7) 0.167(9) 0.183(8) -0.021(7) -0.018(5) 0.004(6) C77 0.121(7) 0.141(7) 0.135(7) 0.015(6) -0.027(5) -0.022(7) C81 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C82 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C83 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C84 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C85 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C86 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C87 0.1378(18) 0.130(2) 0.097(2) 0.0022(17) 0.0138(17) 0.0139(16) C91 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C92 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C93 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C94 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C95 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C96 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C97 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C101 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C102 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C103 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C104 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C105 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C106 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C107 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C111 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C112 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C113 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C114 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C115 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C116 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C117 0.1448(15) 0.1769(15) 0.1811(17) 0.0052(13) -0.0172(13) -0.0043(12) C121 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C122 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C123 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C124 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C125 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C126 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C127 0.1217(14) 0.0566(13) 0.0785(14) -0.0078(11) 0.0197(13) 0.0088(12) C131 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C132 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C133 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C134 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C135 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C136 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C137 0.1045(18) 0.116(2) 0.221(2) 0.0071(18) 0.0014(17) 0.0002(15) C141 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C142 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C143 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C144 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C145 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C146 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C147 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C151 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C152 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C153 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C154 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C155 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C156 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) C157 0.1603(17) 0.1299(12) 0.1602(16) -0.0466(11) 0.0455(14) -0.0182(13) _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 Zn1 O26 1.929(3) . ? Zn1 O3 1.930(3) 3_667 ? Zn1 O1S 1.948(3) . ? Zn1 O2 2.053(3) . ? Zn1 O12 2.212(4) . ? Zn1 Zn6 2.990(2) . ? Zn1 Zn5 3.1201(17) . ? Zn2 O32 1.931(4) 3_666 ? Zn2 O1S 1.938(3) . ? Zn2 O30 1.950(4) 2_646 ? Zn2 O1 1.954(3) . ? Zn2 Zn6 3.1361(15) . ? Zn3 O8 1.986(4) . ? Zn3 O17 2.003(4) . ? Zn3 O2S 2.095(4) . ? Zn3 O4S 2.111(5) . ? Zn3 O13 2.165(5) 2_656 ? Zn3 O3S 2.268(5) . ? Zn4 O7 1.961(3) . ? Zn4 O2S 2.019(4) . ? Zn4 O5S 2.069(5) . ? Zn4 O18 2.073(4) . ? Zn4 O9 2.152(4) 3_667 ? Zn5 O11 1.988(3) . ? Zn5 O1S 1.992(3) . ? Zn5 O7S 2.003(5) . ? Zn5 O5 2.120(3) 2_646 ? Zn5 O25 2.121(3) . ? Zn5 Zn6 3.1402(18) . ? Zn6 O1S 1.885(3) . ? Zn6 O4 1.933(4) 3_667 ? Zn6 O6 1.951(3) 2_646 ? Zn6 O29 2.020(5) 2_646 ? Zn7 O14 1.929(4) . ? Zn7 O2S 1.929(3) 2_646 ? Zn7 O23 1.967(5) 4_465 ? Zn7 O10 1.992(4) 4_565 ? Zn8 O27 1.875(4) . ? Zn8 O22 1.951(6) 2_656 ? Zn8 O19 1.964(5) 3_666 ? Zn8 O16 1.965(5) . ? Zn9 O21 1.833(5) 4_565 ? Zn9 O15 1.971(5) 3_666 ? Zn9 O20 1.976(6) . ? Zn9 O6S 2.013(6) . ? Si1 C35 1.860(3) . ? Si1 C15 1.879(3) . ? Si1 C5 1.880(3) . ? Si1 C25 1.887(3) . ? Si2 C75 1.845(5) . ? Si2 C55 1.891(3) . ? Si2 C65 1.891(3) . ? Si2 C45 1.922(3) . ? Si3 C115 1.837(4) . ? Si3 C105 1.850(4) . ? Si3 C95 1.871(4) . ? Si3 C85 1.885(4) . ? Si4 C145 1.859(3) . ? Si4 C135 1.866(3) . ? Si4 C125 1.884(3) . ? Si4 C155 1.903(4) . ? O1 C1 1.282(5) . ? O2 C1 1.233(5) . ? O2S Zn7 1.929(3) 2_656 ? O3 C11 1.260(5) . ? O3 Zn1 1.930(3) 3_667 ? O4 C11 1.302(5) . ? O4 Zn6 1.933(4) 3_667 ? O5 C21 1.205(5) . ? O5 Zn5 2.120(3) 2_656 ? O6 C21 1.263(6) . ? O6 Zn6 1.951(3) 2_656 ? O7 C31 1.2789(19) . ? O8 C31 1.2760(19) . ? O9 C41 1.267(6) . ? O9 Zn4 2.152(4) 3_667 ? O10 C41 1.245(6) . ? O10 Zn7 1.992(4) 4_566 ? O11 C51 1.287(6) . ? O12 C51 1.230(6) . ? O13 C61 1.275(2) . ? O13 Zn3 2.165(5) 2_646 ? O14 C61 1.273(2) . ? O15 C71 1.181(8) . ? O15 Zn9 1.971(5) 3_666 ? O16 C71 1.302(10) . ? O17 C81 1.271(7) . ? O18 C81 1.203(7) . ? O19 C91 1.274(9) . ? O19 Zn8 1.964(5) 3_666 ? O20 C91 1.222(9) . ? O21 C101 1.267(8) . ? O21 Zn9 1.833(5) 4_566 ? O22 C101 1.271(8) . ? O22 Zn8 1.951(6) 2_646 ? O23 C111 1.277(2) . ? O23 Zn7 1.967(5) 4_666 ? O24 C111 1.287(2) . ? O24 H24B 0.8400 . ? O25 C121 1.170(5) . ? O26 C121 1.334(6) . ? O27 C131 1.192(7) . ? O28 C131 1.248(7) . ? O29 C141 1.267(8) . ? O29 Zn6 2.020(5) 2_656 ? O30 C141 1.212(7) . ? O30 Zn2 1.951(4) 2_656 ? O31 C151 1.290(2) . ? O31 H31A 0.8400 . ? O32 C151 1.273(2) . ? O32 Zn2 1.931(4) 3_666 ? C1 C2 1.484(5) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C11 C12 1.500(5) . ? C12 C13 1.3900 . ? C12 C17 1.3900 . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C21 C22 1.514(5) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C31 C32 1.5072 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C41 C42 1.411(7) . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C51 C52 1.419(6) . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 C55 1.3900 . ? C54 H54A 0.9500 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C61 C62 1.5069 . ? C62 C63 1.3900 . ? C62 C67 1.3900 . ? C63 C64 1.3900 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 H64A 0.9500 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C66 H66A 0.9500 . ? C67 H67A 0.9500 . ? C71 C72 1.403(12) . ? C72 C73 1.3900 . ? C72 C77 1.3900 . ? C73 C74 1.3900 . ? C73 H73A 0.9500 . ? C74 C75 1.3900 . ? C74 H74A 0.9500 . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? C81 C82 1.536(8) . ? C82 C83 1.3900 . ? C82 C87 1.3900 . ? C83 C84 1.3900 . ? C83 H83A 0.9500 . ? C84 C85 1.3900 . ? C84 H84A 0.9500 . ? C85 C86 1.3900 . ? C86 C87 1.3900 . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? C91 C92 1.405(11) . ? C92 C93 1.3900 . ? C92 C97 1.3900 . ? C93 C94 1.3900 . ? C93 H93A 0.9500 . ? C94 C95 1.3900 . ? C94 H94A 0.9500 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C96 H96A 0.9500 . ? C97 H97A 0.9500 . ? C101 C102 1.5094(12) . ? C102 C103 1.3900 . ? C102 C107 1.3900 . ? C103 C104 1.3900 . ? C103 H10A 0.9500 . ? C104 C105 1.3900 . ? C104 H10B 0.9500 . ? C105 C106 1.3900 . ? C106 C107 1.3900 . ? C106 H10C 0.9500 . ? C107 H10D 0.9500 . ? C111 C112 1.5096 . ? C112 C113 1.3900 . ? C112 C117 1.3900 . ? C113 C114 1.3900 . ? C113 H11A 0.9500 . ? C114 C115 1.3900 . ? C114 H11B 0.9500 . ? C115 C116 1.3900 . ? C116 C117 1.3900 . ? C116 H11C 0.9500 . ? C117 H11D 0.9500 . ? C121 C122 1.492(6) . ? C122 C123 1.3900 . ? C122 C127 1.3900 . ? C123 C124 1.3900 . ? C123 H12A 0.9500 . ? C124 C125 1.3900 . ? C124 H12B 0.9500 . ? C125 C126 1.3900 . ? C126 C127 1.3900 . ? C126 H12C 0.9500 . ? C127 H12D 0.9500 . ? C131 C132 1.522(8) . ? C132 C133 1.3900 . ? C132 C137 1.3900 . ? C133 C134 1.3900 . ? C133 H13B 0.9500 . ? C134 C135 1.3900 . ? C134 H13C 0.9500 . ? C135 C136 1.3900 . ? C136 C137 1.3900 . ? C136 H13D 0.9500 . ? C137 H13E 0.9500 . ? C141 C142 1.484(8) . ? C142 C143 1.3900 . ? C142 C147 1.3900 . ? C143 C144 1.3900 . ? C143 H14B 0.9500 . ? C144 C145 1.3900 . ? C144 H14C 0.9500 . ? C145 C146 1.3900 . ? C146 C147 1.3900 . ? C146 H14D 0.9500 . ? C147 H14E 0.9500 . ? C151 C152 1.5095 . ? C152 C153 1.3900 . ? C152 C157 1.3900 . ? C153 C154 1.3900 . ? C153 H15A 0.9500 . ? C154 C155 1.3900 . ? C154 H15B 0.9500 . ? C155 C156 1.3900 . ? C156 C157 1.3900 . ? C156 H15C 0.9500 . ? C157 H15D 0.9500 . ? 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 O26 Zn1 O3 126.99(15) . 3_667 ? O26 Zn1 O1S 119.98(15) . . ? O3 Zn1 O1S 112.45(13) 3_667 . ? O26 Zn1 O2 90.51(15) . . ? O3 Zn1 O2 86.37(13) 3_667 . ? O1S Zn1 O2 101.53(13) . . ? O26 Zn1 O12 86.59(16) . . ? O3 Zn1 O12 84.86(14) 3_667 . ? O1S Zn1 O12 91.33(14) . . ? O2 Zn1 O12 166.48(13) . . ? O26 Zn1 Zn6 146.63(11) . . ? O3 Zn1 Zn6 77.85(9) 3_667 . ? O1S Zn1 Zn6 37.98(8) . . ? O2 Zn1 Zn6 115.41(9) . . ? O12 Zn1 Zn6 72.66(11) . . ? O26 Zn1 Zn5 86.82(12) . . ? O3 Zn1 Zn5 136.87(10) 3_667 . ? O1S Zn1 Zn5 38.13(9) . . ? O2 Zn1 Zn5 123.30(9) . . ? O12 Zn1 Zn5 69.75(10) . . ? Zn6 Zn1 Zn5 61.81(3) . . ? O32 Zn2 O1S 107.84(16) 3_666 . ? O32 Zn2 O30 109.30(19) 3_666 2_646 ? O1S Zn2 O30 109.89(14) . 2_646 ? O32 Zn2 O1 111.84(16) 3_666 . ? O1S Zn2 O1 115.98(12) . . ? O30 Zn2 O1 101.77(16) 2_646 . ? O32 Zn2 Zn6 113.74(13) 3_666 . ? O1S Zn2 Zn6 34.33(8) . . ? O30 Zn2 Zn6 76.35(11) 2_646 . ? O1 Zn2 Zn6 132.13(10) . . ? O8 Zn3 O17 95.89(18) . . ? O8 Zn3 O2S 96.82(15) . . ? O17 Zn3 O2S 93.25(15) . . ? O8 Zn3 O4S 164.23(19) . . ? O17 Zn3 O4S 99.5(2) . . ? O2S Zn3 O4S 85.88(18) . . ? O8 Zn3 O13 79.59(19) . 2_656 ? O17 Zn3 O13 173.34(16) . 2_656 ? O2S Zn3 O13 92.15(15) . 2_656 ? O4S Zn3 O13 84.8(2) . 2_656 ? O8 Zn3 O3S 87.48(18) . . ? O17 Zn3 O3S 88.71(18) . . ? O2S Zn3 O3S 175.07(17) . . ? O4S Zn3 O3S 89.3(2) . . ? O13 Zn3 O3S 86.22(18) 2_656 . ? O7 Zn4 O2S 105.19(14) . . ? O7 Zn4 O5S 105.43(19) . . ? O2S Zn4 O5S 149.20(19) . . ? O7 Zn4 O18 101.37(16) . . ? O2S Zn4 O18 92.86(16) . . ? O5S Zn4 O18 84.36(19) . . ? O7 Zn4 O9 93.20(14) . 3_667 ? O2S Zn4 O9 93.42(14) . 3_667 ? O5S Zn4 O9 81.63(19) . 3_667 ? O18 Zn4 O9 162.02(15) . 3_667 ? O11 Zn5 O1S 105.81(14) . . ? O11 Zn5 O7S 113.6(2) . . ? O1S Zn5 O7S 140.52(19) . . ? O11 Zn5 O5 88.10(13) . 2_646 ? O1S Zn5 O5 94.01(11) . 2_646 ? O7S Zn5 O5 85.58(17) . 2_646 ? O11 Zn5 O25 91.60(13) . . ? O1S Zn5 O25 96.57(11) . . ? O7S Zn5 O25 84.54(17) . . ? O5 Zn5 O25 169.07(12) 2_646 . ? O11 Zn5 Zn1 84.30(10) . . ? O1S Zn5 Zn1 37.14(8) . . ? O7S Zn5 Zn1 147.20(16) . . ? O5 Zn5 Zn1 123.78(9) 2_646 . ? O25 Zn5 Zn1 67.01(9) . . ? O11 Zn5 Zn6 83.37(11) . . ? O1S Zn5 Zn6 34.77(8) . . ? O7S Zn5 Zn6 147.50(15) . . ? O5 Zn5 Zn6 66.75(9) 2_646 . ? O25 Zn5 Zn6 124.06(9) . . ? Zn1 Zn5 Zn6 57.05(5) . . ? O1S Zn6 O4 118.10(13) . 3_667 ? O1S Zn6 O6 117.42(14) . 2_646 ? O4 Zn6 O6 108.35(15) 3_667 2_646 ? O1S Zn6 O29 109.42(17) . 2_646 ? O4 Zn6 O29 98.85(18) 3_667 2_646 ? O6 Zn6 O29 101.82(18) 2_646 2_646 ? O1S Zn6 Zn1 39.49(8) . . ? O4 Zn6 Zn1 79.02(10) 3_667 . ? O6 Zn6 Zn1 131.94(10) 2_646 . ? O29 Zn6 Zn1 124.45(15) 2_646 . ? O1S Zn6 Zn2 35.45(9) . . ? O4 Zn6 Zn2 123.93(11) 3_667 . ? O6 Zn6 Zn2 127.67(10) 2_646 . ? O29 Zn6 Zn2 73.98(14) 2_646 . ? Zn1 Zn6 Zn2 63.29(3) . . ? O1S Zn6 Zn5 37.07(9) . . ? O4 Zn6 Zn5 129.57(11) 3_667 . ? O6 Zn6 Zn5 81.20(11) 2_646 . ? O29 Zn6 Zn5 128.35(13) 2_646 . ? Zn1 Zn6 Zn5 61.14(3) . . ? Zn2 Zn6 Zn5 65.02(2) . . ? O14 Zn7 O2S 120.99(16) . 2_646 ? O14 Zn7 O23 107.13(19) . 4_465 ? O2S Zn7 O23 106.97(18) 2_646 4_465 ? O14 Zn7 O10 106.53(17) . 4_565 ? O2S Zn7 O10 109.57(17) 2_646 4_565 ? O23 Zn7 O10 104.5(2) 4_465 4_565 ? O27 Zn8 O22 108.2(2) . 2_656 ? O27 Zn8 O19 116.3(2) . 3_666 ? O22 Zn8 O19 112.7(2) 2_656 3_666 ? O27 Zn8 O16 98.8(2) . . ? O22 Zn8 O16 108.3(2) 2_656 . ? O19 Zn8 O16 111.5(2) 3_666 . ? O21 Zn9 O15 115.1(2) 4_565 3_666 ? O21 Zn9 O20 97.1(2) 4_565 . ? O15 Zn9 O20 107.9(2) 3_666 . ? O21 Zn9 O6S 109.9(2) 4_565 . ? O15 Zn9 O6S 121.5(2) 3_666 . ? O20 Zn9 O6S 101.4(2) . . ? C35 Si1 C15 109.02(16) . . ? C35 Si1 C5 109.62(16) . . ? C15 Si1 C5 109.90(16) . . ? C35 Si1 C25 112.07(17) . . ? C15 Si1 C25 110.44(15) . . ? C5 Si1 C25 105.74(16) . . ? C75 Si2 C55 111.9(3) . . ? C75 Si2 C65 106.1(2) . . ? C55 Si2 C65 109.79(19) . . ? C75 Si2 C45 105.7(2) . . ? C55 Si2 C45 108.73(18) . . ? C65 Si2 C45 114.52(19) . . ? C115 Si3 C105 106.2(3) . . ? C115 Si3 C95 114.9(3) . . ? C105 Si3 C95 112.2(3) . . ? C115 Si3 C85 108.7(3) . . ? C105 Si3 C85 106.5(3) . . ? C95 Si3 C85 108.1(2) . . ? C145 Si4 C135 114.8(2) . . ? C145 Si4 C125 105.1(2) . . ? C135 Si4 C125 108.5(2) . . ? C145 Si4 C155 110.7(2) . . ? C135 Si4 C155 112.0(2) . . ? C125 Si4 C155 104.90(19) . . ? Zn6 O1S Zn2 110.22(14) . . ? Zn6 O1S Zn1 102.53(13) . . ? Zn2 O1S Zn1 111.71(13) . . ? Zn6 O1S Zn5 108.16(13) . . ? Zn2 O1S Zn5 118.22(14) . . ? Zn1 O1S Zn5 104.73(13) . . ? C1 O1 Zn2 119.9(3) . . ? C1 O2 Zn1 139.5(3) . . ? Zn7 O2S Zn4 114.79(18) 2_656 . ? Zn7 O2S Zn3 111.07(16) 2_656 . ? Zn4 O2S Zn3 107.88(16) . . ? C11 O3 Zn1 127.6(3) . 3_667 ? C11 O4 Zn6 124.3(3) . 3_667 ? C21 O5 Zn5 127.3(3) . 2_656 ? C21 O6 Zn6 115.8(3) . 2_656 ? C31 O7 Zn4 124.0(2) . . ? C31 O8 Zn3 139.0(3) . . ? C41 O9 Zn4 130.5(4) . 3_667 ? C41 O10 Zn7 118.1(4) . 4_566 ? C51 O11 Zn5 127.3(4) . . ? C51 O12 Zn1 138.7(4) . . ? C61 O13 Zn3 133.4(5) . 2_646 ? C61 O14 Zn7 114.6(3) . . ? C71 O15 Zn9 137.4(8) . 3_666 ? C71 O16 Zn8 143.5(7) . . ? C81 O17 Zn3 127.3(5) . . ? C81 O18 Zn4 133.8(5) . . ? C91 O19 Zn8 133.2(6) . 3_666 ? C91 O20 Zn9 145.8(7) . . ? C101 O21 Zn9 145.5(5) . 4_566 ? C101 O22 Zn8 122.9(4) . 2_646 ? C111 O23 Zn7 115.4(4) . 4_666 ? C111 O24 H24B 109.5 . . ? C121 O25 Zn5 139.2(4) . . ? C121 O26 Zn1 118.3(3) . . ? C131 O27 Zn8 122.9(5) . . ? C141 O29 Zn6 130.7(5) . 2_656 ? C141 O30 Zn2 131.2(5) . 2_656 ? C151 O31 H31A 109.5 . . ? C151 O32 Zn2 122.8(3) . 3_666 ? O2 C1 O1 125.1(5) . . ? O2 C1 C2 120.4(5) . . ? O1 C1 C2 114.1(5) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 118.0(3) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 Si1 121.33(19) . . ? C6 C5 Si1 118.63(19) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? O3 C11 O4 125.6(5) . . ? O3 C11 C12 120.1(5) . . ? O4 C11 C12 114.2(4) . . ? C13 C12 C17 120.0 . . ? C13 C12 C11 118.0(3) . . ? C17 C12 C11 121.7(3) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 Si1 119.62(19) . . ? C14 C15 Si1 120.32(19) . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C12 120.0 . . ? C16 C17 H17A 120.0 . . ? C12 C17 H17A 120.0 . . ? O5 C21 O6 129.3(5) . . ? O5 C21 C22 119.4(5) . . ? O6 C21 C22 111.3(5) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 118.7(3) . . ? C27 C22 C21 121.3(3) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 Si1 118.38(18) . . ? C24 C25 Si1 121.51(19) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? O8 C31 O7 125.6(3) . . ? O8 C31 C32 115.4(3) . . ? O7 C31 C32 118.2(3) . . ? C33 C32 C37 120.0 . . ? C33 C32 C31 123.1(3) . . ? C37 C32 C31 116.9(3) . . ? C32 C33 C34 120.0 . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 Si1 116.7(2) . . ? C34 C35 Si1 123.3(2) . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37A 120.0 . . ? C32 C37 H37A 120.0 . . ? O10 C41 O9 123.5(7) . . ? O10 C41 C42 118.1(6) . . ? O9 C41 C42 118.4(6) . . ? C43 C42 C47 120.0 . . ? C43 C42 C41 119.3(4) . . ? C47 C42 C41 120.7(4) . . ? C44 C43 C42 120.0 . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 Si2 120.0(2) . . ? C44 C45 Si2 120.0(2) . . ? C47 C46 C45 120.0 . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 H47A 120.0 . . ? C42 C47 H47A 120.0 . . ? O12 C51 O11 118.8(6) . . ? O12 C51 C52 120.4(6) . . ? O11 C51 C52 120.3(6) . . ? C53 C52 C57 120.0 . . ? C53 C52 C51 120.8(4) . . ? C57 C52 C51 119.2(4) . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 Si2 119.3(2) . . ? C56 C55 Si2 120.5(2) . . ? C55 C56 C57 120.0 . . ? C55 C56 H56A 120.0 . . ? C57 C56 H56A 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57A 120.0 . . ? C52 C57 H57A 120.0 . . ? O14 C61 O13 126.3(3) . . ? O14 C61 C62 118.3(4) . . ? O13 C61 C62 115.3(4) . . ? C63 C62 C67 120.0 . . ? C63 C62 C61 120.9(3) . . ? C67 C62 C61 119.1(3) . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 Si2 119.4(3) . . ? C66 C65 Si2 120.6(3) . . ? C65 C66 C67 120.0 . . ? C65 C66 H66A 120.0 . . ? C67 C66 H66A 120.0 . . ? C66 C67 C62 120.0 . . ? C66 C67 H67A 120.0 . . ? C62 C67 H67A 120.0 . . ? O15 C71 O16 116.9(12) . . ? O15 C71 C72 125.9(11) . . ? O16 C71 C72 117.1(8) . . ? C73 C72 C77 120.0 . . ? C73 C72 C71 122.5(7) . . ? C77 C72 C71 117.0(7) . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 Si2 121.8(5) . . ? C74 C75 Si2 118.0(5) . . ? C75 C76 C77 120.0 . . ? C75 C76 H76A 120.0 . . ? C77 C76 H76A 120.0 . . ? C76 C77 C72 120.0 . . ? C76 C77 H77A 120.0 . . ? C72 C77 H77A 120.0 . . ? O18 C81 O17 128.2(7) . . ? O18 C81 C82 114.9(7) . . ? O17 C81 C82 114.8(6) . . ? C83 C82 C87 120.0 . . ? C83 C82 C81 120.4(5) . . ? C87 C82 C81 119.6(5) . . ? C84 C83 C82 120.0 . . ? C84 C83 H83A 120.0 . . ? C82 C83 H83A 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 Si3 117.2(3) . . ? C86 C85 Si3 121.6(3) . . ? C87 C86 C85 120.0 . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C86 C87 C82 120.0 . . ? C86 C87 H87A 120.0 . . ? C82 C87 H87A 120.0 . . ? O20 C91 O19 117.8(10) . . ? O20 C91 C92 124.3(10) . . ? O19 C91 C92 117.9(10) . . ? C93 C92 C97 120.0 . . ? C93 C92 C91 119.6(7) . . ? C97 C92 C91 120.3(7) . . ? C92 C93 C94 120.0 . . ? C92 C93 H93A 120.0 . . ? C94 C93 H93A 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 H94A 120.0 . . ? C93 C94 H94A 120.0 . . ? C94 C95 C96 120.0 . . ? C94 C95 Si3 118.1(4) . . ? C96 C95 Si3 121.8(4) . . ? C97 C96 C95 120.0 . . ? C97 C96 H96A 120.0 . . ? C95 C96 H96A 120.0 . . ? C96 C97 C92 120.0 . . ? C96 C97 H97A 120.0 . . ? C92 C97 H97A 120.0 . . ? O21 C101 O22 123.7(5) . . ? O21 C101 C102 123.4(8) . . ? O22 C101 C102 112.8(7) . . ? C103 C102 C107 120.0 . . ? C103 C102 C101 122.5(6) . . ? C107 C102 C101 117.0(6) . . ? C104 C103 C102 120.0 . . ? C104 C103 H10A 120.0 . . ? C102 C103 H10A 120.0 . . ? C103 C104 C105 120.0 . . ? C103 C104 H10B 120.0 . . ? C105 C104 H10B 120.0 . . ? C104 C105 C106 120.0 . . ? C104 C105 Si3 122.5(4) . . ? C106 C105 Si3 117.2(4) . . ? C107 C106 C105 120.0 . . ? C107 C106 H10C 120.0 . . ? C105 C106 H10C 120.0 . . ? C106 C107 C102 120.0 . . ? C106 C107 H10D 120.0 . . ? C102 C107 H10D 120.0 . . ? O23 C111 O24 107.6(4) . . ? O23 C111 C112 107.9(4) . . ? O24 C111 C112 139.4(6) . . ? C113 C112 C117 120.0 . . ? C113 C112 C111 106.9(5) . . ? C117 C112 C111 133.0(5) . . ? C112 C113 C114 120.0 . . ? C112 C113 H11A 120.0 . . ? C114 C113 H11A 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H11B 120.0 . . ? C113 C114 H11B 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 Si3 126.5(4) . . ? C114 C115 Si3 112.4(4) . . ? C115 C116 C117 120.0 . . ? C115 C116 H11C 120.0 . . ? C117 C116 H11C 120.0 . . ? C116 C117 C112 120.0 . . ? C116 C117 H11D 120.0 . . ? C112 C117 H11D 120.0 . . ? O25 C121 O26 124.9(5) . . ? O25 C121 C122 124.2(5) . . ? O26 C121 C122 110.8(4) . . ? C123 C122 C127 120.0 . . ? C123 C122 C121 117.5(3) . . ? C127 C122 C121 122.5(3) . . ? C124 C123 C122 120.0 . . ? C124 C123 H12A 120.0 . . ? C122 C123 H12A 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H12B 120.0 . . ? C125 C124 H12B 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 Si4 119.1(2) . . ? C124 C125 Si4 120.9(2) . . ? C125 C126 C127 120.0 . . ? C125 C126 H12C 120.0 . . ? C127 C126 H12C 120.0 . . ? C126 C127 C122 120.0 . . ? C126 C127 H12D 120.0 . . ? C122 C127 H12D 120.0 . . ? O27 C131 O28 126.9(8) . . ? O27 C131 C132 118.8(7) . . ? O28 C131 C132 114.1(7) . . ? C133 C132 C137 120.0 . . ? C133 C132 C131 116.3(5) . . ? C137 C132 C131 123.7(5) . . ? C132 C133 C134 120.0 . . ? C132 C133 H13B 120.0 . . ? C134 C133 H13B 120.0 . . ? C135 C134 C133 120.0 . . ? C135 C134 H13C 120.0 . . ? C133 C134 H13C 120.0 . . ? C134 C135 C136 120.0 . . ? C134 C135 Si4 118.5(3) . . ? C136 C135 Si4 121.4(3) . . ? C135 C136 C137 120.0 . . ? C135 C136 H13D 120.0 . . ? C137 C136 H13D 120.0 . . ? C136 C137 C132 120.0 . . ? C136 C137 H13E 120.0 . . ? C132 C137 H13E 120.0 . . ? O30 C141 O29 122.5(7) . . ? O30 C141 C142 124.3(8) . . ? O29 C141 C142 113.1(7) . . ? C143 C142 C147 120.0 . . ? C143 C142 C141 117.6(5) . . ? C147 C142 C141 122.1(5) . . ? C144 C143 C142 120.0 . . ? C144 C143 H14B 120.0 . . ? C142 C143 H14B 120.0 . . ? C143 C144 C145 120.0 . . ? C143 C144 H14C 120.0 . . ? C145 C144 H14C 120.0 . . ? C144 C145 C146 120.0 . . ? C144 C145 Si4 123.0(3) . . ? C146 C145 Si4 117.0(3) . . ? C147 C146 C145 120.0 . . ? C147 C146 H14D 120.0 . . ? C145 C146 H14D 120.0 . . ? C146 C147 C142 120.0 . . ? C146 C147 H14E 120.0 . . ? C142 C147 H14E 120.0 . . ? O32 C151 O31 123.6(4) . . ? O32 C151 C152 108.1(4) . . ? O31 C151 C152 126.3(5) . . ? C153 C152 C157 120.0 . . ? C153 C152 C151 125.5(4) . . ? C157 C152 C151 114.3(4) . . ? C154 C153 C152 120.0 . . ? C154 C153 H15A 120.0 . . ? C152 C153 H15A 120.0 . . ? C153 C154 C155 120.0 . . ? C153 C154 H15B 120.0 . . ? C155 C154 H15B 120.0 . . ? C156 C155 C154 120.0 . . ? C156 C155 Si4 114.8(3) . . ? C154 C155 Si4 124.1(3) . . ? C157 C156 C155 120.0 . . ? C157 C156 H15C 120.0 . . ? C155 C156 H15C 120.0 . . ? C156 C157 C152 120.0 . . ? C156 C157 H15D 120.0 . . ? C152 C157 H15D 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O26 Zn1 Zn5 O11 -82.38(16) . . . . ? O3 Zn1 Zn5 O11 62.91(17) 3_667 . . . ? O1S Zn1 Zn5 O11 125.82(16) . . . . ? O2 Zn1 Zn5 O11 -170.90(15) . . . . ? O12 Zn1 Zn5 O11 5.15(15) . . . . ? Zn6 Zn1 Zn5 O11 85.78(10) . . . . ? O26 Zn1 Zn5 O1S 151.80(17) . . . . ? O3 Zn1 Zn5 O1S -62.91(19) 3_667 . . . ? O2 Zn1 Zn5 O1S 63.28(17) . . . . ? O12 Zn1 Zn5 O1S -120.67(17) . . . . ? Zn6 Zn1 Zn5 O1S -40.04(13) . . . . ? O26 Zn1 Zn5 O7S 43.7(3) . . . . ? O3 Zn1 Zn5 O7S -171.0(3) 3_667 . . . ? O1S Zn1 Zn5 O7S -108.1(3) . . . . ? O2 Zn1 Zn5 O7S -44.8(3) . . . . ? O12 Zn1 Zn5 O7S 131.2(3) . . . . ? Zn6 Zn1 Zn5 O7S -148.2(3) . . . . ? O26 Zn1 Zn5 O5 -166.25(16) . . . 2_646 ? O3 Zn1 Zn5 O5 -20.96(18) 3_667 . . 2_646 ? O1S Zn1 Zn5 O5 41.95(17) . . . 2_646 ? O2 Zn1 Zn5 O5 105.23(15) . . . 2_646 ? O12 Zn1 Zn5 O5 -78.72(16) . . . 2_646 ? Zn6 Zn1 Zn5 O5 1.91(11) . . . 2_646 ? O26 Zn1 Zn5 O25 11.80(15) . . . . ? O3 Zn1 Zn5 O25 157.09(17) 3_667 . . . ? O1S Zn1 Zn5 O25 -140.00(16) . . . . ? O2 Zn1 Zn5 O25 -76.72(14) . . . . ? O12 Zn1 Zn5 O25 99.33(15) . . . . ? Zn6 Zn1 Zn5 O25 179.96(10) . . . . ? O26 Zn1 Zn5 Zn6 -168.16(12) . . . . ? O3 Zn1 Zn5 Zn6 -22.87(14) 3_667 . . . ? O1S Zn1 Zn5 Zn6 40.04(13) . . . . ? O2 Zn1 Zn5 Zn6 103.32(11) . . . . ? O12 Zn1 Zn5 Zn6 -80.63(11) . . . . ? O26 Zn1 Zn6 O1S 62.1(3) . . . . ? O3 Zn1 Zn6 O1S -155.57(17) 3_667 . . . ? O2 Zn1 Zn6 O1S -75.59(18) . . . . ? O12 Zn1 Zn6 O1S 116.08(18) . . . . ? Zn5 Zn1 Zn6 O1S 40.20(14) . . . . ? O26 Zn1 Zn6 O4 -126.1(3) . . . 3_667 ? O3 Zn1 Zn6 O4 16.24(14) 3_667 . . 3_667 ? O1S Zn1 Zn6 O4 171.82(18) . . . 3_667 ? O2 Zn1 Zn6 O4 96.23(16) . . . 3_667 ? O12 Zn1 Zn6 O4 -72.11(16) . . . 3_667 ? Zn5 Zn1 Zn6 O4 -147.98(12) . . . 3_667 ? O26 Zn1 Zn6 O6 -21.2(3) . . . 2_646 ? O3 Zn1 Zn6 O6 121.13(17) 3_667 . . 2_646 ? O1S Zn1 Zn6 O6 -83.3(2) . . . 2_646 ? O2 Zn1 Zn6 O6 -158.89(17) . . . 2_646 ? O12 Zn1 Zn6 O6 32.78(17) . . . 2_646 ? Zn5 Zn1 Zn6 O6 -43.10(14) . . . 2_646 ? O26 Zn1 Zn6 O29 140.6(3) . . . 2_646 ? O3 Zn1 Zn6 O29 -77.02(19) 3_667 . . 2_646 ? O1S Zn1 Zn6 O29 78.6(2) . . . 2_646 ? O2 Zn1 Zn6 O29 2.96(19) . . . 2_646 ? O12 Zn1 Zn6 O29 -165.37(19) . . . 2_646 ? Zn5 Zn1 Zn6 O29 118.75(16) . . . 2_646 ? O26 Zn1 Zn6 Zn2 96.6(2) . . . . ? O3 Zn1 Zn6 Zn2 -120.99(9) 3_667 . . . ? O1S Zn1 Zn6 Zn2 34.58(14) . . . . ? O2 Zn1 Zn6 Zn2 -41.01(11) . . . . ? O12 Zn1 Zn6 Zn2 150.66(10) . . . . ? Zn5 Zn1 Zn6 Zn2 74.78(2) . . . . ? O26 Zn1 Zn6 Zn5 21.9(2) . . . . ? O3 Zn1 Zn6 Zn5 164.23(10) 3_667 . . . ? O1S Zn1 Zn6 Zn5 -40.20(14) . . . . ? O2 Zn1 Zn6 Zn5 -115.79(11) . . . . ? O12 Zn1 Zn6 Zn5 75.88(10) . . . . ? O32 Zn2 Zn6 O1S -87.1(2) 3_666 . . . ? O30 Zn2 Zn6 O1S 167.54(18) 2_646 . . . ? O1 Zn2 Zn6 O1S 73.9(2) . . . . ? O32 Zn2 Zn6 O4 -179.0(2) 3_666 . . 3_667 ? O1S Zn2 Zn6 O4 -91.9(2) . . . 3_667 ? O30 Zn2 Zn6 O4 75.61(18) 2_646 . . 3_667 ? O1 Zn2 Zn6 O4 -18.02(19) . . . 3_667 ? O32 Zn2 Zn6 O6 -1.8(2) 3_666 . . 2_646 ? O1S Zn2 Zn6 O6 85.35(19) . . . 2_646 ? O30 Zn2 Zn6 O6 -107.11(18) 2_646 . . 2_646 ? O1 Zn2 Zn6 O6 159.26(18) . . . 2_646 ? O32 Zn2 Zn6 O29 91.0(2) 3_666 . . 2_646 ? O1S Zn2 Zn6 O29 178.1(2) . . . 2_646 ? O30 Zn2 Zn6 O29 -14.38(18) 2_646 . . 2_646 ? O1 Zn2 Zn6 O29 -108.0(2) . . . 2_646 ? O32 Zn2 Zn6 Zn1 -125.59(16) 3_666 . . . ? O1S Zn2 Zn6 Zn1 -38.49(14) . . . . ? O30 Zn2 Zn6 Zn1 129.06(12) 2_646 . . . ? O1 Zn2 Zn6 Zn1 35.43(14) . . . . ? O32 Zn2 Zn6 Zn5 -56.79(16) 3_666 . . . ? O1S Zn2 Zn6 Zn5 30.31(14) . . . . ? O30 Zn2 Zn6 Zn5 -162.15(12) 2_646 . . . ? O1 Zn2 Zn6 Zn5 104.22(14) . . . . ? O11 Zn5 Zn6 O1S -130.41(16) . . . . ? O7S Zn5 Zn6 O1S 105.0(3) . . . . ? O5 Zn5 Zn6 O1S 138.80(17) 2_646 . . . ? O25 Zn5 Zn6 O1S -42.97(17) . . . . ? Zn1 Zn5 Zn6 O1S -42.93(13) . . . . ? O11 Zn5 Zn6 O4 -45.02(17) . . . 3_667 ? O1S Zn5 Zn6 O4 85.39(19) . . . 3_667 ? O7S Zn5 Zn6 O4 -169.7(3) . . . 3_667 ? O5 Zn5 Zn6 O4 -135.80(17) 2_646 . . 3_667 ? O25 Zn5 Zn6 O4 42.43(18) . . . 3_667 ? Zn1 Zn5 Zn6 O4 42.47(14) . . . 3_667 ? O11 Zn5 Zn6 O6 61.56(14) . . . 2_646 ? O1S Zn5 Zn6 O6 -168.02(17) . . . 2_646 ? O7S Zn5 Zn6 O6 -63.1(3) . . . 2_646 ? O5 Zn5 Zn6 O6 -29.22(13) 2_646 . . 2_646 ? O25 Zn5 Zn6 O6 149.01(15) . . . 2_646 ? Zn1 Zn5 Zn6 O6 149.05(11) . . . 2_646 ? O11 Zn5 Zn6 O29 159.7(2) . . . 2_646 ? O1S Zn5 Zn6 O29 -69.9(2) . . . 2_646 ? O7S Zn5 Zn6 O29 35.1(4) . . . 2_646 ? O5 Zn5 Zn6 O29 68.9(2) 2_646 . . 2_646 ? O25 Zn5 Zn6 O29 -112.8(2) . . . 2_646 ? Zn1 Zn5 Zn6 O29 -112.80(19) . . . 2_646 ? O11 Zn5 Zn6 Zn1 -87.49(9) . . . . ? O1S Zn5 Zn6 Zn1 42.93(13) . . . . ? O7S Zn5 Zn6 Zn1 147.9(3) . . . . ? O5 Zn5 Zn6 Zn1 -178.27(10) 2_646 . . . ? O25 Zn5 Zn6 Zn1 -0.04(11) . . . . ? O11 Zn5 Zn6 Zn2 -159.47(9) . . . . ? O1S Zn5 Zn6 Zn2 -29.05(13) . . . . ? O7S Zn5 Zn6 Zn2 75.9(3) . . . . ? O5 Zn5 Zn6 Zn2 109.75(10) 2_646 . . . ? O25 Zn5 Zn6 Zn2 -72.02(11) . . . . ? Zn1 Zn5 Zn6 Zn2 -71.98(2) . . . . ? O4 Zn6 O1S Zn2 109.95(17) 3_667 . . . ? O6 Zn6 O1S Zn2 -117.27(16) 2_646 . . . ? O29 Zn6 O1S Zn2 -2.0(2) 2_646 . . . ? Zn1 Zn6 O1S Zn2 119.1(2) . . . . ? Zn5 Zn6 O1S Zn2 -130.63(19) . . . . ? O4 Zn6 O1S Zn1 -9.1(2) 3_667 . . . ? O6 Zn6 O1S Zn1 123.67(15) 2_646 . . . ? O29 Zn6 O1S Zn1 -121.02(18) 2_646 . . . ? Zn2 Zn6 O1S Zn1 -119.1(2) . . . . ? Zn5 Zn6 O1S Zn1 110.31(18) . . . . ? O4 Zn6 O1S Zn5 -119.42(16) 3_667 . . . ? O6 Zn6 O1S Zn5 13.36(18) 2_646 . . . ? O29 Zn6 O1S Zn5 128.67(18) 2_646 . . . ? Zn1 Zn6 O1S Zn5 -110.31(18) . . . . ? Zn2 Zn6 O1S Zn5 130.63(19) . . . . ? O32 Zn2 O1S Zn6 106.18(19) 3_666 . . . ? O30 Zn2 O1S Zn6 -12.88(19) 2_646 . . . ? O1 Zn2 O1S Zn6 -127.56(15) . . . . ? O32 Zn2 O1S Zn1 -140.53(18) 3_666 . . . ? O30 Zn2 O1S Zn1 100.42(18) 2_646 . . . ? O1 Zn2 O1S Zn1 -14.3(2) . . . . ? Zn6 Zn2 O1S Zn1 113.3(2) . . . . ? O32 Zn2 O1S Zn5 -18.9(2) 3_666 . . . ? O30 Zn2 O1S Zn5 -137.96(16) 2_646 . . . ? O1 Zn2 O1S Zn5 107.36(16) . . . . ? Zn6 Zn2 O1S Zn5 -125.1(2) . . . . ? O26 Zn1 O1S Zn6 -145.88(16) . . . . ? O3 Zn1 O1S Zn6 25.94(18) 3_667 . . . ? O2 Zn1 O1S Zn6 116.76(14) . . . . ? O12 Zn1 O1S Zn6 -59.05(16) . . . . ? Zn5 Zn1 O1S Zn6 -112.87(18) . . . . ? O26 Zn1 O1S Zn2 96.11(19) . . . . ? O3 Zn1 O1S Zn2 -92.07(16) 3_667 . . . ? O2 Zn1 O1S Zn2 -1.25(17) . . . . ? O12 Zn1 O1S Zn2 -177.06(16) . . . . ? Zn6 Zn1 O1S Zn2 -118.0(2) . . . . ? Zn5 Zn1 O1S Zn2 129.1(2) . . . . ? O26 Zn1 O1S Zn5 -33.0(2) . . . . ? O3 Zn1 O1S Zn5 138.81(13) 3_667 . . . ? O2 Zn1 O1S Zn5 -130.37(13) . . . . ? O12 Zn1 O1S Zn5 53.82(14) . . . . ? Zn6 Zn1 O1S Zn5 112.87(18) . . . . ? O11 Zn5 O1S Zn6 51.81(15) . . . . ? O7S Zn5 O1S Zn6 -125.3(2) . . . . ? O5 Zn5 O1S Zn6 -37.35(14) 2_646 . . . ? O25 Zn5 O1S Zn6 145.36(14) . . . . ? Zn1 Zn5 O1S Zn6 108.80(18) . . . . ? O11 Zn5 O1S Zn2 177.90(14) . . . . ? O7S Zn5 O1S Zn2 0.8(3) . . . . ? O5 Zn5 O1S Zn2 88.73(15) 2_646 . . . ? O25 Zn5 O1S Zn2 -88.56(15) . . . . ? Zn1 Zn5 O1S Zn2 -125.1(2) . . . . ? Zn6 Zn5 O1S Zn2 126.1(2) . . . . ? O11 Zn5 O1S Zn1 -56.99(15) . . . . ? O7S Zn5 O1S Zn1 125.9(2) . . . . ? O5 Zn5 O1S Zn1 -146.15(13) 2_646 . . . ? O25 Zn5 O1S Zn1 36.56(14) . . . . ? Zn6 Zn5 O1S Zn1 -108.80(18) . . . . ? O32 Zn2 O1 C1 154.2(4) 3_666 . . . ? O1S Zn2 O1 C1 30.0(4) . . . . ? O30 Zn2 O1 C1 -89.3(4) 2_646 . . . ? Zn6 Zn2 O1 C1 -7.1(4) . . . . ? O26 Zn1 O2 C1 -105.8(5) . . . . ? O3 Zn1 O2 C1 127.2(5) 3_667 . . . ? O1S Zn1 O2 C1 15.0(6) . . . . ? O12 Zn1 O2 C1 176.8(6) . . . . ? Zn6 Zn1 O2 C1 52.5(6) . . . . ? Zn5 Zn1 O2 C1 -19.3(6) . . . . ? O7 Zn4 O2S Zn7 75.61(19) . . . 2_656 ? O5S Zn4 O2S Zn7 -98.0(4) . . . 2_656 ? O18 Zn4 O2S Zn7 178.21(18) . . . 2_656 ? O9 Zn4 O2S Zn7 -18.65(18) 3_667 . . 2_656 ? O7 Zn4 O2S Zn3 -48.80(18) . . . . ? O5S Zn4 O2S Zn3 137.6(3) . . . . ? O18 Zn4 O2S Zn3 53.80(17) . . . . ? O9 Zn4 O2S Zn3 -143.05(16) 3_667 . . . ? O8 Zn3 O2S Zn7 -91.7(2) . . . 2_656 ? O17 Zn3 O2S Zn7 171.96(19) . . . 2_656 ? O4S Zn3 O2S Zn7 72.7(2) . . . 2_656 ? O13 Zn3 O2S Zn7 -11.9(2) 2_656 . . 2_656 ? O3S Zn3 O2S Zn7 59(2) . . . 2_656 ? O8 Zn3 O2S Zn4 34.90(19) . . . . ? O17 Zn3 O2S Zn4 -61.43(19) . . . . ? O4S Zn3 O2S Zn4 -160.7(2) . . . . ? O13 Zn3 O2S Zn4 114.7(2) 2_656 . . . ? O3S Zn3 O2S Zn4 -174.7(19) . . . . ? O2S Zn4 O7 C31 34.0(4) . . . . ? O5S Zn4 O7 C31 -149.4(4) . . . . ? O18 Zn4 O7 C31 -62.2(4) . . . . ? O9 Zn4 O7 C31 128.4(4) 3_667 . . . ? O17 Zn3 O8 C31 93.5(6) . . . . ? O2S Zn3 O8 C31 -0.5(6) . . . . ? O4S Zn3 O8 C31 -99.5(8) . . . . ? O13 Zn3 O8 C31 -91.5(6) 2_656 . . . ? O3S Zn3 O8 C31 -178.1(6) . . . . ? O1S Zn5 O11 C51 19.3(5) . . . . ? O7S Zn5 O11 C51 -162.7(5) . . . . ? O5 Zn5 O11 C51 112.9(5) 2_646 . . . ? O25 Zn5 O11 C51 -78.0(5) . . . . ? Zn1 Zn5 O11 C51 -11.3(5) . . . . ? Zn6 Zn5 O11 C51 46.1(5) . . . . ? O26 Zn1 O12 C51 85.1(7) . . . . ? O3 Zn1 O12 C51 -147.2(7) 3_667 . . . ? O1S Zn1 O12 C51 -34.8(7) . . . . ? O2 Zn1 O12 C51 163.0(6) . . . . ? Zn6 Zn1 O12 C51 -68.4(7) . . . . ? Zn5 Zn1 O12 C51 -2.7(6) . . . . ? O2S Zn7 O14 C61 30.6(6) 2_646 . . . ? O23 Zn7 O14 C61 153.3(5) 4_465 . . . ? O10 Zn7 O14 C61 -95.3(5) 4_565 . . . ? O27 Zn8 O16 C71 158.7(12) . . . . ? O22 Zn8 O16 C71 46.1(12) 2_656 . . . ? O19 Zn8 O16 C71 -78.4(12) 3_666 . . . ? O8 Zn3 O17 C81 -51.7(6) . . . . ? O2S Zn3 O17 C81 45.5(6) . . . . ? O4S Zn3 O17 C81 131.9(6) . . . . ? O13 Zn3 O17 C81 -98.6(17) 2_656 . . . ? O3S Zn3 O17 C81 -139.0(6) . . . . ? O7 Zn4 O18 C81 76.9(7) . . . . ? O2S Zn4 O18 C81 -29.2(7) . . . . ? O5S Zn4 O18 C81 -178.4(7) . . . . ? O9 Zn4 O18 C81 -139.5(6) 3_667 . . . ? O21 Zn9 O20 C91 -40.0(13) 4_565 . . . ? O15 Zn9 O20 C91 79.4(13) 3_666 . . . ? O6S Zn9 O20 C91 -151.9(13) . . . . ? O11 Zn5 O25 C121 61.6(6) . . . . ? O1S Zn5 O25 C121 -44.5(6) . . . . ? O7S Zn5 O25 C121 175.2(6) . . . . ? O5 Zn5 O25 C121 149.9(7) 2_646 . . . ? Zn1 Zn5 O25 C121 -21.5(6) . . . . ? Zn6 Zn5 O25 C121 -21.5(6) . . . . ? O3 Zn1 O26 C121 -162.3(4) 3_667 . . . ? O1S Zn1 O26 C121 8.2(5) . . . . ? O2 Zn1 O26 C121 111.8(4) . . . . ? O12 Zn1 O26 C121 -81.4(4) . . . . ? Zn6 Zn1 O26 C121 -30.7(5) . . . . ? Zn5 Zn1 O26 C121 -11.5(4) . . . . ? O22 Zn8 O27 C131 -74.1(7) 2_656 . . . ? O19 Zn8 O27 C131 53.9(7) 3_666 . . . ? O16 Zn8 O27 C131 173.2(7) . . . . ? Zn1 O2 C1 O1 -1.9(9) . . . . ? Zn1 O2 C1 C2 169.9(3) . . . . ? Zn2 O1 C1 O2 -22.1(7) . . . . ? Zn2 O1 C1 C2 165.6(3) . . . . ? O2 C1 C2 C3 169.4(4) . . . . ? O1 C1 C2 C3 -18.0(6) . . . . ? O2 C1 C2 C7 -4.3(6) . . . . ? O1 C1 C2 C7 168.4(3) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 -173.5(4) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 Si1 177.8(2) . . . . ? C35 Si1 C5 C4 4.3(2) . . . . ? C15 Si1 C5 C4 -115.54(19) . . . . ? C25 Si1 C5 C4 125.26(19) . . . . ? C35 Si1 C5 C6 -177.92(18) . . . . ? C15 Si1 C5 C6 62.3(2) . . . . ? C25 Si1 C5 C6 -56.9(2) . . . . ? C4 C5 C6 C7 0.0 . . . . ? Si1 C5 C6 C7 -177.8(2) . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 173.8(3) . . . . ? Zn1 O3 C11 O4 -9.4(8) 3_667 . . . ? Zn1 O3 C11 C12 167.3(3) 3_667 . . . ? Zn6 O4 C11 O3 -16.4(7) 3_667 . . . ? Zn6 O4 C11 C12 166.7(3) 3_667 . . . ? O3 C11 C12 C13 24.5(5) . . . . ? O4 C11 C12 C13 -158.5(3) . . . . ? O3 C11 C12 C17 -162.0(3) . . . . ? O4 C11 C12 C17 15.0(5) . . . . ? C17 C12 C13 C14 0.0 . . . . ? C11 C12 C13 C14 173.7(3) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C13 C14 C15 Si1 -177.2(2) . . . . ? C35 Si1 C15 C16 72.4(2) . . . . ? C5 Si1 C15 C16 -167.42(17) . . . . ? C25 Si1 C15 C16 -51.1(2) . . . . ? C35 Si1 C15 C14 -110.38(19) . . . . ? C5 Si1 C15 C14 9.8(2) . . . . ? C25 Si1 C15 C14 126.07(19) . . . . ? C14 C15 C16 C17 0.0 . . . . ? Si1 C15 C16 C17 177.2(2) . . . . ? C15 C16 C17 C12 0.0 . . . . ? C13 C12 C17 C16 0.0 . . . . ? C11 C12 C17 C16 -173.4(3) . . . . ? Zn5 O5 C21 O6 -30.6(9) 2_656 . . . ? Zn5 O5 C21 C22 149.6(3) 2_656 . . . ? Zn6 O6 C21 O5 -17.1(8) 2_656 . . . ? Zn6 O6 C21 C22 162.7(3) 2_656 . . . ? O5 C21 C22 C23 -1.6(7) . . . . ? O6 C21 C22 C23 178.5(3) . . . . ? O5 C21 C22 C27 176.0(4) . . . . ? O6 C21 C22 C27 -3.8(6) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 177.7(4) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C23 C24 C25 Si1 -176.1(3) . . . . ? C35 Si1 C25 C26 62.4(2) . . . . ? C15 Si1 C25 C26 -175.87(17) . . . . ? C5 Si1 C25 C26 -57.0(2) . . . . ? C35 Si1 C25 C24 -121.5(2) . . . . ? C15 Si1 C25 C24 0.3(2) . . . . ? C5 Si1 C25 C24 119.2(2) . . . . ? C24 C25 C26 C27 0.0 . . . . ? Si1 C25 C26 C27 176.2(2) . . . . ? C25 C26 C27 C22 0.0 . . . . ? C23 C22 C27 C26 0.0 . . . . ? C21 C22 C27 C26 -177.6(4) . . . . ? Zn3 O8 C31 O7 -23.3(9) . . . . ? Zn3 O8 C31 C32 146.7(4) . . . . ? Zn4 O7 C31 O8 2.5(7) . . . . ? Zn4 O7 C31 C32 -167.23(19) . . . . ? O8 C31 C32 C33 -9.0(4) . . . . ? O7 C31 C32 C33 161.7(4) . . . . ? O8 C31 C32 C37 171.0(4) . . . . ? O7 C31 C32 C37 -18.3(4) . . . . ? C37 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C34 180.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C33 C34 C35 Si1 -179.4(2) . . . . ? C15 Si1 C35 C36 32.7(2) . . . . ? C5 Si1 C35 C36 -87.7(2) . . . . ? C25 Si1 C35 C36 155.25(17) . . . . ? C15 Si1 C35 C34 -147.92(19) . . . . ? C5 Si1 C35 C34 91.7(2) . . . . ? C25 Si1 C35 C34 -25.3(2) . . . . ? C34 C35 C36 C37 0.0 . . . . ? Si1 C35 C36 C37 179.4(2) . . . . ? C35 C36 C37 C32 0.0 . . . . ? C33 C32 C37 C36 0.0 . . . . ? C31 C32 C37 C36 180.0 . . . . ? Zn7 O10 C41 O9 29.8(9) 4_566 . . . ? Zn7 O10 C41 C42 -149.0(4) 4_566 . . . ? Zn4 O9 C41 O10 29.1(9) 3_667 . . . ? Zn4 O9 C41 C42 -152.1(4) 3_667 . . . ? O10 C41 C42 C43 177.3(4) . . . . ? O9 C41 C42 C43 -1.5(7) . . . . ? O10 C41 C42 C47 -1.9(7) . . . . ? O9 C41 C42 C47 179.2(4) . . . . ? C47 C42 C43 C44 0.0 . . . . ? C41 C42 C43 C44 -179.3(4) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C43 C44 C45 Si2 178.9(3) . . . . ? C75 Si2 C45 C46 161.3(3) . . . . ? C55 Si2 C45 C46 -78.3(2) . . . . ? C65 Si2 C45 C46 44.9(3) . . . . ? C75 Si2 C45 C44 -17.6(3) . . . . ? C55 Si2 C45 C44 102.7(2) . . . . ? C65 Si2 C45 C44 -134.1(2) . . . . ? C44 C45 C46 C47 0.0 . . . . ? Si2 C45 C46 C47 -178.9(3) . . . . ? C45 C46 C47 C42 0.0 . . . . ? C43 C42 C47 C46 0.0 . . . . ? C41 C42 C47 C46 179.3(4) . . . . ? Zn1 O12 C51 O11 -4.0(11) . . . . ? Zn1 O12 C51 C52 -176.5(3) . . . . ? Zn5 O11 C51 O12 12.6(9) . . . . ? Zn5 O11 C51 C52 -174.8(3) . . . . ? O12 C51 C52 C53 178.8(5) . . . . ? O11 C51 C52 C53 6.4(8) . . . . ? O12 C51 C52 C57 -1.6(8) . . . . ? O11 C51 C52 C57 -174.0(4) . . . . ? C57 C52 C53 C54 0.0 . . . . ? C51 C52 C53 C54 179.6(5) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C53 C54 C55 Si2 175.5(3) . . . . ? C75 Si2 C55 C54 -82.2(3) . . . . ? C65 Si2 C55 C54 35.3(3) . . . . ? C45 Si2 C55 C54 161.3(2) . . . . ? C75 Si2 C55 C56 93.2(3) . . . . ? C65 Si2 C55 C56 -149.2(2) . . . . ? C45 Si2 C55 C56 -23.2(3) . . . . ? C54 C55 C56 C57 0.0 . . . . ? Si2 C55 C56 C57 -175.4(3) . . . . ? C55 C56 C57 C52 0.0 . . . . ? C53 C52 C57 C56 0.0 . . . . ? C51 C52 C57 C56 -179.6(5) . . . . ? Zn7 O14 C61 O13 -0.7(11) . . . . ? Zn7 O14 C61 C62 175.8(4) . . . . ? Zn3 O13 C61 O14 -49.8(12) 2_646 . . . ? Zn3 O13 C61 C62 133.6(4) 2_646 . . . ? O14 C61 C62 C63 175.3(5) . . . . ? O13 C61 C62 C63 -7.9(9) . . . . ? O14 C61 C62 C67 -4.8(8) . . . . ? O13 C61 C62 C67 172.1(5) . . . . ? C67 C62 C63 C64 0.0 . . . . ? C61 C62 C63 C64 179.9(5) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C63 C64 C65 Si2 179.8(3) . . . . ? C75 Si2 C65 C64 -169.6(3) . . . . ? C55 Si2 C65 C64 69.2(3) . . . . ? C45 Si2 C65 C64 -53.4(3) . . . . ? C75 Si2 C65 C66 10.2(3) . . . . ? C55 Si2 C65 C66 -111.0(2) . . . . ? C45 Si2 C65 C66 126.4(2) . . . . ? C64 C65 C66 C67 0.0 . . . . ? Si2 C65 C66 C67 -179.8(3) . . . . ? C65 C66 C67 C62 0.0 . . . . ? C63 C62 C67 C66 0.0 . . . . ? C61 C62 C67 C66 -179.9(5) . . . . ? Zn9 O15 C71 O16 -4.4(17) 3_666 . . . ? Zn9 O15 C71 C72 -180.0(5) 3_666 . . . ? Zn8 O16 C71 O15 21.6(19) . . . . ? Zn8 O16 C71 C72 -162.4(6) . . . . ? O15 C71 C72 C73 -176.3(8) . . . . ? O16 C71 C72 C73 8.2(12) . . . . ? O15 C71 C72 C77 -4.2(13) . . . . ? O16 C71 C72 C77 -179.8(7) . . . . ? C77 C72 C73 C74 0.0 . . . . ? C71 C72 C73 C74 171.8(6) . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C73 C74 C75 Si2 -174.4(3) . . . . ? C55 Si2 C75 C76 -177.1(2) . . . . ? C65 Si2 C75 C76 63.2(3) . . . . ? C45 Si2 C75 C76 -58.8(3) . . . . ? C55 Si2 C75 C74 -2.8(3) . . . . ? C65 Si2 C75 C74 -122.5(2) . . . . ? C45 Si2 C75 C74 115.4(3) . . . . ? C74 C75 C76 C77 0.0 . . . . ? Si2 C75 C76 C77 174.2(3) . . . . ? C75 C76 C77 C72 0.0 . . . . ? C73 C72 C77 C76 0.0 . . . . ? C71 C72 C77 C76 -172.2(6) . . . . ? Zn4 O18 C81 O17 9.0(12) . . . . ? Zn4 O18 C81 C82 172.0(3) . . . . ? Zn3 O17 C81 O18 -19.8(11) . . . . ? Zn3 O17 C81 C82 177.2(3) . . . . ? O18 C81 C82 C83 -171.9(5) . . . . ? O17 C81 C82 C83 -6.6(7) . . . . ? O18 C81 C82 C87 8.5(8) . . . . ? O17 C81 C82 C87 173.8(4) . . . . ? C87 C82 C83 C84 0.0 . . . . ? C81 C82 C83 C84 -179.6(4) . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C86 0.0 . . . . ? C83 C84 C85 Si3 -167.3(3) . . . . ? C115 Si3 C85 C84 85.9(3) . . . . ? C105 Si3 C85 C84 -160.1(2) . . . . ? C95 Si3 C85 C84 -39.3(3) . . . . ? C115 Si3 C85 C86 -81.2(3) . . . . ? C105 Si3 C85 C86 32.8(3) . . . . ? C95 Si3 C85 C86 153.6(3) . . . . ? C84 C85 C86 C87 0.0 . . . . ? Si3 C85 C86 C87 166.7(3) . . . . ? C85 C86 C87 C82 0.0 . . . . ? C83 C82 C87 C86 0.0 . . . . ? C81 C82 C87 C86 179.6(4) . . . . ? Zn9 O20 C91 O19 -13(2) . . . . ? Zn9 O20 C91 C92 169.1(5) . . . . ? Zn8 O19 C91 O20 -12.2(16) 3_666 . . . ? Zn8 O19 C91 C92 166.0(5) 3_666 . . . ? O20 C91 C92 C93 4.9(14) . . . . ? O19 C91 C92 C93 -173.1(7) . . . . ? O20 C91 C92 C97 -179.0(8) . . . . ? O19 C91 C92 C97 3.0(12) . . . . ? C97 C92 C93 C94 0.0 . . . . ? C91 C92 C93 C94 176.1(7) . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C93 C94 C95 Si3 -176.7(4) . . . . ? C115 Si3 C95 C94 -27.4(4) . . . . ? C105 Si3 C95 C94 -148.7(3) . . . . ? C85 Si3 C95 C94 94.1(3) . . . . ? C115 Si3 C95 C96 156.0(3) . . . . ? C105 Si3 C95 C96 34.7(4) . . . . ? C85 Si3 C95 C96 -82.5(3) . . . . ? C94 C95 C96 C97 0.0 . . . . ? Si3 C95 C96 C97 176.5(4) . . . . ? C95 C96 C97 C92 0.0 . . . . ? C93 C92 C97 C96 0.0 . . . . ? C91 C92 C97 C96 -176.1(7) . . . . ? Zn9 O21 C101 O22 22.0(18) 4_566 . . . ? Zn9 O21 C101 C102 -161.5(6) 4_566 . . . ? Zn8 O22 C101 O21 18.4(13) 2_646 . . . ? Zn8 O22 C101 C102 -158.3(4) 2_646 . . . ? O21 C101 C102 C103 -170.1(7) . . . . ? O22 C101 C102 C103 6.7(10) . . . . ? O21 C101 C102 C107 1.7(11) . . . . ? O22 C101 C102 C107 178.5(5) . . . . ? C107 C102 C103 C104 0.0 . . . . ? C101 C102 C103 C104 171.5(6) . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C106 0.0 . . . . ? C103 C104 C105 Si3 -173.5(4) . . . . ? C115 Si3 C105 C104 155.5(3) . . . . ? C95 Si3 C105 C104 -78.3(3) . . . . ? C85 Si3 C105 C104 39.8(3) . . . . ? C115 Si3 C105 C106 -18.2(4) . . . . ? C95 Si3 C105 C106 108.0(3) . . . . ? C85 Si3 C105 C106 -133.9(3) . . . . ? C104 C105 C106 C107 0.0 . . . . ? Si3 C105 C106 C107 173.8(4) . . . . ? C105 C106 C107 C102 0.0 . . . . ? C103 C102 C107 C106 0.0 . . . . ? C101 C102 C107 C106 -172.0(6) . . . . ? Zn7 O23 C111 O24 -27.5(8) 4_666 . . . ? Zn7 O23 C111 C112 172.5(4) 4_666 . . . ? O23 C111 C112 C113 -170.5(5) . . . . ? O24 C111 C112 C113 39.5(11) . . . . ? O23 C111 C112 C117 12.4(9) . . . . ? O24 C111 C112 C117 -137.5(8) . . . . ? C117 C112 C113 C114 0.0 . . . . ? C111 C112 C113 C114 -177.5(5) . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C113 C114 C115 Si3 168.9(3) . . . . ? C105 Si3 C115 C116 87.1(4) . . . . ? C95 Si3 C115 C116 -37.5(4) . . . . ? C85 Si3 C115 C116 -158.7(3) . . . . ? C105 Si3 C115 C114 -80.9(3) . . . . ? C95 Si3 C115 C114 154.5(3) . . . . ? C85 Si3 C115 C114 33.3(3) . . . . ? C114 C115 C116 C117 0.0 . . . . ? Si3 C115 C116 C117 -167.2(4) . . . . ? C115 C116 C117 C112 0.0 . . . . ? C113 C112 C117 C116 0.0 . . . . ? C111 C112 C117 C116 176.8(6) . . . . ? Zn5 O25 C121 O26 20.4(10) . . . . ? Zn5 O25 C121 C122 -154.6(4) . . . . ? Zn1 O26 C121 O25 2.6(8) . . . . ? Zn1 O26 C121 C122 178.2(3) . . . . ? O25 C121 C122 C123 1.4(7) . . . . ? O26 C121 C122 C123 -174.3(3) . . . . ? O25 C121 C122 C127 -176.8(4) . . . . ? O26 C121 C122 C127 7.6(6) . . . . ? C127 C122 C123 C124 0.0 . . . . ? C121 C122 C123 C124 -178.2(4) . . . . ? C122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 C126 0.0 . . . . ? C123 C124 C125 Si4 -177.1(2) . . . . ? C145 Si4 C125 C126 42.9(2) . . . . ? C135 Si4 C125 C126 -80.4(2) . . . . ? C155 Si4 C125 C126 159.7(2) . . . . ? C145 Si4 C125 C124 -140.0(2) . . . . ? C135 Si4 C125 C124 96.7(2) . . . . ? C155 Si4 C125 C124 -23.2(3) . . . . ? C124 C125 C126 C127 0.0 . . . . ? Si4 C125 C126 C127 177.1(2) . . . . ? C125 C126 C127 C122 0.0 . . . . ? C123 C122 C127 C126 0.0 . . . . ? C121 C122 C127 C126 178.1(4) . . . . ? Zn8 O27 C131 O28 5.0(13) . . . . ? Zn8 O27 C131 C132 179.1(4) . . . . ? O27 C131 C132 C133 -0.4(9) . . . . ? O28 C131 C132 C133 174.5(5) . . . . ? O27 C131 C132 C137 177.0(6) . . . . ? O28 C131 C132 C137 -8.2(9) . . . . ? C137 C132 C133 C134 0.0 . . . . ? C131 C132 C133 C134 177.4(5) . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C136 0.0 . . . . ? C133 C134 C135 Si4 -177.0(3) . . . . ? C145 Si4 C135 C134 -124.8(3) . . . . ? C125 Si4 C135 C134 -7.6(3) . . . . ? C155 Si4 C135 C134 107.7(3) . . . . ? C145 Si4 C135 C136 58.3(3) . . . . ? C125 Si4 C135 C136 175.5(2) . . . . ? C155 Si4 C135 C136 -69.2(3) . . . . ? C134 C135 C136 C137 0.0 . . . . ? Si4 C135 C136 C137 176.9(3) . . . . ? C135 C136 C137 C132 0.0 . . . . ? C133 C132 C137 C136 0.0 . . . . ? C131 C132 C137 C136 -177.3(5) . . . . ? Zn2 O30 C141 O29 -19.2(13) 2_656 . . . ? Zn2 O30 C141 C142 165.2(4) 2_656 . . . ? Zn6 O29 C141 O30 -7.6(13) 2_656 . . . ? Zn6 O29 C141 C142 168.4(4) 2_656 . . . ? O30 C141 C142 C143 -4.9(10) . . . . ? O29 C141 C142 C143 179.2(5) . . . . ? O30 C141 C142 C147 -178.4(6) . . . . ? O29 C141 C142 C147 5.7(9) . . . . ? C147 C142 C143 C144 0.0 . . . . ? C141 C142 C143 C144 -173.6(5) . . . . ? C142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 C146 0.0 . . . . ? C143 C144 C145 Si4 180.0(3) . . . . ? C135 Si4 C145 C144 -16.0(3) . . . . ? C125 Si4 C145 C144 -135.1(2) . . . . ? C155 Si4 C145 C144 112.1(3) . . . . ? C135 Si4 C145 C146 164.0(2) . . . . ? C125 Si4 C145 C146 44.8(3) . . . . ? C155 Si4 C145 C146 -68.0(3) . . . . ? C144 C145 C146 C147 0.0 . . . . ? Si4 C145 C146 C147 -180.0(3) . . . . ? C145 C146 C147 C142 0.0 . . . . ? C143 C142 C147 C146 0.0 . . . . ? C141 C142 C147 C146 173.3(5) . . . . ? Zn2 O32 C151 O31 8.6(10) 3_666 . . . ? Zn2 O32 C151 C152 173.2(3) 3_666 . . . ? O32 C151 C152 C153 13.8(7) . . . . ? O31 C151 C152 C153 177.8(5) . . . . ? O32 C151 C152 C157 -171.5(4) . . . . ? O31 C151 C152 C157 -7.5(8) . . . . ? C157 C152 C153 C154 0.0 . . . . ? C151 C152 C153 C154 174.4(5) . . . . ? C152 C153 C154 C155 0.0 . . . . ? C153 C154 C155 C156 0.0 . . . . ? C153 C154 C155 Si4 167.4(3) . . . . ? C145 Si4 C155 C156 -136.7(3) . . . . ? C135 Si4 C155 C156 -7.1(3) . . . . ? C125 Si4 C155 C156 110.3(2) . . . . ? C145 Si4 C155 C154 55.3(3) . . . . ? C135 Si4 C155 C154 -175.1(3) . . . . ? C125 Si4 C155 C154 -57.6(3) . . . . ? C154 C155 C156 C157 0.0 . . . . ? Si4 C155 C156 C157 -168.5(3) . . . . ? C155 C156 C157 C152 0.0 . . . . ? C153 C152 C157 C156 0.0 . . . . ? C151 C152 C157 C156 -175.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.125 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.065 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 -0.008 -0.003 20067 7384 ' ' _platon_squeeze_details ; ; _vrf_PLAT026_p21c_sq ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 22 % RESPONSE: Experiments were performed on Bruker SMART APEXII Diffractometer with Mo X-ray tube and low-temperature system (110K). Due to the ultraporous nature of this compound, the diffraction from the crystal was very weak and there were no reflections after 2Theta=30deg, even after we used data collection time 80s/frame. This crystal appears to be more than 0.3mm. However, it's a 50%-50% twinned crystal with twin law 0 0 1 0 1 0 -1 0 0. The presence of twinning might result in destructive interference, which further impairs the diffraction intensity. ; _database_code_depnum_ccdc_archive 'CCDC 942376' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p42mmc_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn2 O2 (C28 H16 O8 Si)' _chemical_formula_sum 'C28 H16 O10 Si Zn2' _chemical_formula_weight 671.24 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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(2)/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x, -y, -z' '-x, y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x, y, z' 'x, -y, z' '-y, -x, z-1/2' 'y, x, z-1/2' _cell_length_a 12.706(4) _cell_length_b 12.706(4) _cell_length_c 23.817(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3845(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5837 _cell_measurement_theta_min 2.2668 _cell_measurement_theta_max 19.8041 _exptl_crystal_description Columnar _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8266 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43156 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.26 _reflns_number_total 2645 _reflns_number_gt 1556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0300P)^2^+3.0000P] 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_number_reflns 2645 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.38242(3) 0.0000 0.0000 0.06659(10) Uani 1 4 d S . . Si1 Si 0.5000 0.5000 0.2500 0.0623(3) Uani 1 8 d S . . C1 C 0.5000 0.38257(15) 0.20289(6) 0.0651(6) Uani 1 2 d S . . C4 C 0.5000 0.22450(15) 0.12061(7) 0.0729(7) Uani 1 2 d S . . O1 O 0.41151(9) 0.11044(8) 0.05860(4) 0.1000(4) Uani 1 1 d . . . C2 C 0.40631(12) 0.34073(13) 0.18193(5) 0.0887(5) Uani 1 1 d . . . H2 H 0.3409 0.3664 0.1956 0.106 Uiso 1 1 calc R . . C5 C 0.5000 0.14120(16) 0.07636(8) 0.0841(8) Uani 1 2 d S . . C3 C 0.40723(13) 0.26308(12) 0.14188(6) 0.0880(5) Uani 1 1 d . . . H3 H 0.3424 0.2355 0.1286 0.106 Uiso 1 1 calc R . . O2 O 0.22767(19) 0.0000 0.0000 0.1305(11) Uani 1 4 d S . . 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 Zn1 0.0865(2) 0.06033(18) 0.05295(15) 0.000 0.000 0.000 Si1 0.0753(4) 0.0753(4) 0.0362(4) 0.000 0.000 0.000 C1 0.0881(12) 0.0717(12) 0.0356(8) 0.0029(9) 0.000 0.000 C4 0.1120(15) 0.0598(11) 0.0469(9) 0.0002(9) 0.000 0.000 O1 0.1316(9) 0.0866(7) 0.0818(6) -0.0260(6) 0.0030(7) -0.0071(7) C2 0.0866(10) 0.1088(11) 0.0705(8) -0.0267(8) 0.0009(8) 0.0006(9) C5 0.1322(18) 0.0676(13) 0.0526(10) 0.0000(10) 0.000 0.000 C3 0.0948(10) 0.0918(10) 0.0774(8) -0.0246(8) -0.0029(8) -0.0105(9) O2 0.0813(16) 0.146(2) 0.164(2) 0.000 0.000 0.000 _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 Zn1 O2 1.966(3) . ? Zn1 O1 2.0134(11) 5 ? Zn1 O1 2.0134(11) 14 ? Zn1 O1 2.0134(11) 11 ? Zn1 O1 2.0134(11) . ? Zn1 Zn1 2.9881(12) 9_655 ? Si1 C1 1.8669(19) 12_656 ? Si1 C1 1.8669(19) 10_566 ? Si1 C1 1.8669(19) 3_665 ? Si1 C1 1.8669(18) . ? C1 C2 1.3960(18) 13_655 ? C1 C2 1.3960(18) . ? C4 C3 1.3734(18) . ? C4 C3 1.3734(18) 13_655 ? C4 C5 1.494(3) . ? O1 C5 1.2633(15) . ? C2 C3 1.373(2) . ? C2 H2 0.9500 . ? C5 O1 1.2633(15) 13_655 ? C3 H3 0.9500 . ? 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 Zn1 O1 100.58(4) . 5 ? O2 Zn1 O1 100.58(4) . 14 ? O1 Zn1 O1 87.77(6) 5 14 ? O2 Zn1 O1 100.58(4) . 11 ? O1 Zn1 O1 88.37(6) 5 11 ? O1 Zn1 O1 158.84(7) 14 11 ? O2 Zn1 O1 100.58(4) . . ? O1 Zn1 O1 158.84(7) 5 . ? O1 Zn1 O1 88.37(6) 14 . ? O1 Zn1 O1 87.77(6) 11 . ? O2 Zn1 Zn1 180.0 . 9_655 ? O1 Zn1 Zn1 79.42(4) 5 9_655 ? O1 Zn1 Zn1 79.42(4) 14 9_655 ? O1 Zn1 Zn1 79.42(4) 11 9_655 ? O1 Zn1 Zn1 79.42(4) . 9_655 ? C1 Si1 C1 106.12(11) 12_656 10_566 ? C1 Si1 C1 111.17(5) 12_656 3_665 ? C1 Si1 C1 111.17(5) 10_566 3_665 ? C1 Si1 C1 111.17(5) 12_656 . ? C1 Si1 C1 111.17(5) 10_566 . ? C1 Si1 C1 106.12(11) 3_665 . ? C2 C1 C2 117.02(18) 13_655 . ? C2 C1 Si1 121.28(9) 13_655 . ? C2 C1 Si1 121.28(9) . . ? C3 C4 C3 118.24(18) . 13_655 ? C3 C4 C5 120.87(9) . . ? C3 C4 C5 120.87(9) 13_655 . ? C5 O1 Zn1 127.67(11) . . ? C1 C2 C3 121.00(15) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? O1 C5 O1 125.76(19) 13_655 . ? O1 C5 C4 117.10(9) 13_655 . ? O1 C5 C4 117.10(9) . . ? C4 C3 C2 121.35(15) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? 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 C1 Si1 C1 C2 -34.82(11) 12_656 . . 13_655 ? C1 Si1 C1 C2 -152.81(16) 10_566 . . 13_655 ? C1 Si1 C1 C2 86.19(13) 3_665 . . 13_655 ? C1 Si1 C1 C2 152.81(16) 12_656 . . . ? C1 Si1 C1 C2 34.82(11) 10_566 . . . ? C1 Si1 C1 C2 -86.19(13) 3_665 . . . ? O2 Zn1 O1 C5 178.61(14) . . . . ? O1 Zn1 O1 C5 -1.38(14) 5 . . . ? O1 Zn1 O1 C5 78.15(15) 14 . . . ? O1 Zn1 O1 C5 -81.04(15) 11 . . . ? Zn1 Zn1 O1 C5 -1.39(14) 9_655 . . . ? C2 C1 C2 C3 -1.0(3) 13_655 . . . ? Si1 C1 C2 C3 171.70(12) . . . . ? Zn1 O1 C5 O1 3.0(3) . . . 13_655 ? Zn1 O1 C5 C4 -179.67(11) . . . . ? C3 C4 C5 O1 179.42(16) . . . 13_655 ? C3 C4 C5 O1 -1.9(3) 13_655 . . 13_655 ? C3 C4 C5 O1 1.8(3) . . . . ? C3 C4 C5 O1 -179.42(16) 13_655 . . . ? C3 C4 C3 C2 2.2(3) 13_655 . . . ? C5 C4 C3 C2 -179.00(16) . . . . ? C1 C2 C3 C4 -0.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.410 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.047 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.018 -0.013 -0.005 2812 1017 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942377' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_aaa_sq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cd3 (C28 H16 O8 Si)2][Cd O4]' _chemical_formula_sum 'C56 H32 Cd4 O20 Si2' _chemical_formula_weight 1530.60 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.775(4) _cell_length_b 14.507(4) _cell_length_c 24.244(7) _cell_angle_alpha 83.217(3) _cell_angle_beta 81.797(3) _cell_angle_gamma 65.572(3) _cell_volume 4357(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8348 _cell_measurement_theta_min 2.2218 _cell_measurement_theta_max 25.6414 _exptl_crystal_description Blocky _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7455 _exptl_absorpt_correction_T_max 0.8190 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45816 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17024 _reflns_number_gt 11389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0389P)^2^+174.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00195(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17024 _refine_ls_number_parameters 480 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.1520 _refine_ls_R_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.2893 _refine_ls_wR_factor_gt 0.2771 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.003 _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 -0.25255(5) 0.77374(5) -0.39938(3) 0.0163(2) Uani 1 1 d . . . Cd2 Cd -0.24926(7) 0.74967(6) -0.25021(4) 0.0272(2) Uani 1 1 d . . . Cd3 Cd 0.2716(3) 0.2598(4) 0.1036(2) 0.0629(12) Uani 0.50 1 d P . 1 O4 O 0.3610(9) 0.3003(12) 0.0271(5) 0.0548(12) Uani 0.50 1 d PD . 1 Cd3' Cd 0.2262(3) 0.2859(3) 0.09812(18) 0.0469(9) Uani 0.50 1 d P . 2 O4' O 0.3106(14) 0.3691(14) 0.0202(6) 0.0548(12) Uani 0.50 1 d PD . 2 Si1 Si 0.36915(19) 0.39464(19) -0.26376(11) 0.0161(5) Uani 1 1 d . . . Si2 Si 0.1289(7) 1.1054(6) -0.2353(2) 0.104(3) Uani 1 1 d D . . O1 O -0.1316(6) 0.7265(6) -0.3301(3) 0.0296(7) Uani 1 1 d . B . O2 O -0.0862(6) 0.6285(6) -0.4004(3) 0.0296(7) Uani 1 1 d . B . O3 O 0.2172(8) 0.2802(8) 0.0096(4) 0.0548(12) Uani 1 1 d D . . O5 O 0.6290(7) -0.1183(6) -0.3073(4) 0.0379(9) Uani 1 1 d . . . O6 O 0.6519(7) -0.0656(6) -0.3819(4) 0.0379(9) Uani 1 1 d . . . O7 O 0.6502(10) 0.6837(10) -0.3708(4) 0.068(4) Uani 1 1 d . . . O8 O 0.6792(10) 0.6628(11) -0.2840(4) 0.068(4) Uani 1 1 d . . . O11 O 0.2844(6) 1.2093(7) -0.5096(3) 0.037(2) Uani 1 1 d . . . O12 O 0.1578(7) 1.1625(8) -0.5225(4) 0.042(2) Uani 1 1 d . . . O14 O -0.1485(15) 1.5961(11) -0.2104(5) 0.094(2) Uani 1 1 d . . . O15 O 0.6310(14) 0.7686(11) -0.1689(6) 0.104(3) Uani 1 1 d . . . O16 O 0.5894(14) 0.8717(11) -0.1001(6) 0.104(3) Uani 1 1 d . . . O13 O -0.1021(15) 1.5662(11) -0.1222(5) 0.094(2) Uani 1 1 d . . . C1 C -0.0663(5) 0.6519(8) -0.3553(5) 0.0296(7) Uani 1 1 d D . . C2 C 0.0405(4) 0.5868(5) -0.3341(3) 0.0296(7) Uani 1 1 d D B . C3 C 0.1104(5) 0.4998(5) -0.3603(3) 0.0296(7) Uani 1 1 d D . . H3A H 0.0913 0.4813 -0.3922 0.036 Uiso 1 1 calc R B . C4 C 0.2082(4) 0.4400(4) -0.3400(3) 0.0296(7) Uani 1 1 d D B . H4A H 0.2559 0.3806 -0.3579 0.036 Uiso 1 1 calc R . . C5 C 0.2361(4) 0.4672(5) -0.2934(3) 0.0296(7) Uani 1 1 d D . . C6 C 0.1662(5) 0.5541(5) -0.2672(3) 0.0296(7) Uani 1 1 d D B . H6A H 0.1853 0.5727 -0.2354 0.036 Uiso 1 1 calc R . . C7 C 0.0684(5) 0.6139(4) -0.2875(3) 0.0296(7) Uani 1 1 d D . . H7A H 0.0206 0.6733 -0.2696 0.036 Uiso 1 1 calc R B . C8 C 0.3014(9) 0.3080(5) -0.0096(2) 0.0548(12) Uani 1 1 d D . . C9 C 0.3061(7) 0.3423(5) -0.0708(2) 0.0548(12) Uani 1 1 d D . . C10 C 0.3888(7) 0.3716(7) -0.0923(3) 0.0548(12) Uani 1 1 d D . . H10A H 0.4325 0.3796 -0.0678 0.066 Uiso 1 1 calc R . . C11 C 0.4077(7) 0.3894(8) -0.1496(3) 0.0548(12) Uani 1 1 d D . . H11A H 0.4643 0.4095 -0.1643 0.066 Uiso 1 1 calc R . . C12 C 0.3438(8) 0.3778(8) -0.1854(2) 0.0548(12) Uani 1 1 d D . . C13 C 0.2610(8) 0.3484(9) -0.1639(3) 0.0548(12) Uani 1 1 d D . . H13A H 0.2174 0.3405 -0.1884 0.066 Uiso 1 1 calc R . . C14 C 0.2422(7) 0.3307(7) -0.1066(3) 0.0548(12) Uani 1 1 d D . . H14A H 0.1856 0.3106 -0.0919 0.066 Uiso 1 1 calc R . . C15 C 0.6267(9) -0.0448(5) -0.3348(6) 0.0379(9) Uani 1 1 d D . . C16 C 0.5635(4) 0.0628(4) -0.3186(3) 0.0379(9) Uani 1 1 d D B . C17 C 0.5378(5) 0.1425(5) -0.3594(2) 0.0379(9) Uani 1 1 d D . . H17A H 0.5611 0.1293 -0.3975 0.046 Uiso 1 1 calc R . . C18 C 0.4781(6) 0.2415(4) -0.3444(3) 0.0379(9) Uani 1 1 d D B . H18A H 0.4606 0.2959 -0.3723 0.046 Uiso 1 1 calc R . . C19 C 0.4439(6) 0.2610(4) -0.2885(3) 0.0379(9) Uani 1 1 d D . . C20 C 0.4695(7) 0.1813(5) -0.2477(2) 0.0379(9) Uani 1 1 d D B . H20A H 0.4462 0.1945 -0.2095 0.046 Uiso 1 1 calc R . . C21 C 0.5293(6) 0.0823(4) -0.2627(3) 0.0379(9) Uani 1 1 d D . . H21A H 0.5468 0.0279 -0.2348 0.046 Uiso 1 1 calc R B . C22 C 0.6402(7) 0.6504(7) -0.3224(5) 0.0259(10) Uani 1 1 d D A . C23 C 0.5752(4) 0.5870(4) -0.3113(3) 0.0259(10) Uani 1 1 d D . . C26 C 0.4548(5) 0.4712(5) -0.2844(3) 0.0259(10) Uani 1 1 d D . . C24 C 0.4786(6) 0.6159(5) -0.3336(4) 0.0259(10) Uani 0.50 1 d PD A 1 H24A H 0.4536 0.6752 -0.3580 0.031 Uiso 0.50 1 calc PR A 1 C25 C 0.4183(5) 0.5581(6) -0.3202(4) 0.0259(10) Uani 0.50 1 d PD A 1 H25A H 0.3523 0.5778 -0.3355 0.031 Uiso 0.50 1 calc PR A 1 C27 C 0.5514(6) 0.4423(5) -0.2621(4) 0.0259(10) Uani 0.50 1 d PD A 1 H27A H 0.5764 0.3830 -0.2377 0.031 Uiso 0.50 1 calc PR A 1 C28 C 0.6116(5) 0.5002(6) -0.2755(4) 0.0259(10) Uani 0.50 1 d PD A 1 H28A H 0.6776 0.4805 -0.2602 0.031 Uiso 0.50 1 calc PR A 1 C25' C 0.4371(10) 0.5513(7) -0.2525(5) 0.0259(10) Uani 0.50 1 d PD A 2 H25B H 0.3838 0.5664 -0.2214 0.031 Uiso 0.50 1 calc PR A 2 C24' C 0.4972(7) 0.6092(10) -0.2658(4) 0.0259(10) Uani 0.50 1 d PD A 2 H24B H 0.4850 0.6639 -0.2439 0.031 Uiso 0.50 1 calc PR A 2 C28' C 0.5927(10) 0.5070(7) -0.3431(5) 0.0259(10) Uani 0.50 1 d PD A 2 H28B H 0.6460 0.4919 -0.3742 0.031 Uiso 0.50 1 calc PR A 2 C27' C 0.5327(7) 0.4489(11) -0.3299(4) 0.0259(10) Uani 0.50 1 d PD A 2 H27B H 0.5449 0.3942 -0.3518 0.031 Uiso 0.50 1 calc PR A 2 O10 O -0.1556(8) 0.8192(7) -0.1289(4) 0.0460(13) Uani 1 1 d . . . O9 O -0.1171(15) 0.7847(14) -0.2131(8) 0.0460(13) Uani 0.50 1 d P B 1 C31 C -0.1024(7) 0.8231(9) -0.1700(10) 0.0460(13) Uani 0.50 1 d PD B 1 C32 C -0.0392(7) 0.8876(8) -0.1854(5) 0.0460(13) Uani 0.50 1 d PD B 1 C33 C 0.0379(10) 0.8674(9) -0.2313(5) 0.0460(13) Uani 0.50 1 d PD B 1 H33A H 0.0511 0.8126 -0.2533 0.055 Uiso 0.50 1 calc PR B 1 C34 C 0.0957(10) 0.9275(10) -0.2450(6) 0.0460(13) Uani 0.50 1 d PD B 1 H34A H 0.1483 0.9137 -0.2764 0.055 Uiso 0.50 1 calc PR B 1 C35 C 0.0764(10) 1.0077(9) -0.2129(7) 0.0460(13) Uani 0.50 1 d PD B 1 C36 C -0.0007(12) 1.0279(10) -0.1670(7) 0.0460(13) Uani 0.50 1 d PD B 1 H36A H -0.0139 1.0827 -0.1450 0.055 Uiso 0.50 1 calc PR B 1 C37 C -0.0584(10) 0.9678(11) -0.1533(5) 0.0460(13) Uani 0.50 1 d PD B 1 H37A H -0.1111 0.9816 -0.1219 0.055 Uiso 0.50 1 calc PR B 1 O9' O -0.2312(15) 0.8778(14) -0.2178(8) 0.0460(13) Uani 0.50 1 d P B 2 C31' C -0.1657(17) 0.8771(15) -0.1789(13) 0.0460(13) Uani 0.50 1 d PD B 2 C32' C -0.1048(8) 0.9442(7) -0.1905(6) 0.0460(13) Uani 0.50 1 d PD B 2 C33' C -0.0108(9) 0.9142(8) -0.1654(6) 0.0460(13) Uani 0.50 1 d PD B 2 H33B H 0.0099 0.8562 -0.1398 0.055 Uiso 0.50 1 calc PR B 2 C34' C 0.0529(8) 0.9688(10) -0.1777(7) 0.0460(13) Uani 0.50 1 d PD B 2 H34B H 0.1171 0.9482 -0.1605 0.055 Uiso 0.50 1 calc PR B 2 C35' C 0.0227(9) 1.0536(10) -0.2152(7) 0.0460(13) Uani 0.50 1 d PD B 2 C36' C -0.0713(10) 1.0837(9) -0.2404(7) 0.0460(13) Uani 0.50 1 d PD B 2 H36B H -0.0920 1.1417 -0.2660 0.055 Uiso 0.50 1 calc PR B 2 C37' C -0.1349(8) 1.0290(9) -0.2280(6) 0.0460(13) Uani 0.50 1 d PD B 2 H37B H -0.1991 1.0496 -0.2452 0.055 Uiso 0.50 1 calc PR B 2 C38 C 0.2154(12) 1.1791(13) -0.4923(4) 0.0498(13) Uani 1 1 d D . . C39 C 0.1983(7) 1.1544(5) -0.4304(4) 0.0498(13) Uani 1 1 d D . . C40 C 0.1137(7) 1.1295(7) -0.4063(3) 0.0498(13) Uani 1 1 d D B . H40A H 0.0645 1.1282 -0.4296 0.060 Uiso 1 1 calc R . . C41 C 0.0988(7) 1.1065(8) -0.3493(3) 0.0498(13) Uani 1 1 d D . . H41A H 0.0402 1.0898 -0.3343 0.060 Uiso 1 1 calc R B . C42 C 0.1697(8) 1.1079(8) -0.3143(4) 0.0498(13) Uani 1 1 d D B . C43 C 0.2545(9) 1.1327(9) -0.3381(4) 0.0498(13) Uani 1 1 d D . . H43A H 0.3038 1.1341 -0.3148 0.060 Uiso 1 1 calc R B . C44 C 0.2689(8) 1.1557(8) -0.3952(4) 0.0498(13) Uani 1 1 d D B . H44A H 0.3275 1.1724 -0.4102 0.060 Uiso 1 1 calc R . . C45 C -0.1224(16) 1.5424(8) -0.1704(8) 0.094(2) Uani 1 1 d D . . C46 C -0.0497(5) 1.4344(7) -0.1828(4) 0.094(2) Uani 1 1 d D . . C47 C -0.0162(8) 1.4133(7) -0.2385(4) 0.094(2) Uani 1 1 d D B . H47A H -0.0326 1.4670 -0.2668 0.113 Uiso 1 1 calc R . . C48 C 0.0412(11) 1.3135(8) -0.2527(3) 0.094(2) Uani 1 1 d D . . H48A H 0.0640 1.2992 -0.2908 0.113 Uiso 1 1 calc R B . C49 C 0.0652(12) 1.2348(6) -0.2113(5) 0.094(2) Uani 1 1 d D B . C50 C 0.0319(13) 1.2557(8) -0.1556(4) 0.094(2) Uani 1 1 d D . . H50A H 0.0482 1.2020 -0.1273 0.113 Uiso 1 1 calc R B . C51 C -0.0256(10) 1.3555(9) -0.1415(4) 0.094(2) Uani 1 1 d D B . H51A H -0.0484 1.3699 -0.1034 0.113 Uiso 1 1 calc R . . C52 C 0.5666(9) 0.8534(14) -0.1414(7) 0.104(3) Uani 1 1 d D . . C53 C 0.4612(6) 0.9138(9) -0.1651(4) 0.104(3) Uani 1 1 d D . . C54 C 0.4348(8) 0.8857(7) -0.2118(4) 0.104(3) Uani 1 1 d D B . H54A H 0.4834 0.8265 -0.2296 0.124 Uiso 1 1 calc R . . C55 C 0.3371(9) 0.9444(9) -0.2326(4) 0.104(3) Uani 1 1 d D . . H55A H 0.3190 0.9251 -0.2645 0.124 Uiso 1 1 calc R B . C56 C 0.2658(7) 1.0311(8) -0.2066(5) 0.104(3) Uani 1 1 d D B . C57 C 0.2923(8) 1.0592(7) -0.1599(5) 0.104(3) Uani 1 1 d D . . H57A H 0.2436 1.1185 -0.1421 0.124 Uiso 1 1 calc R B . C58 C 0.3900(9) 1.0006(9) -0.1391(4) 0.104(3) Uani 1 1 d D B . H58A H 0.4081 1.0198 -0.1072 0.124 Uiso 1 1 calc R . . Cd4 Cd 0.3538(4) 0.4804(4) 0.0559(2) 0.0564(12) Uani 0.25 1 d PD . . Cd5 Cd 0.2351(3) 0.7367(3) 0.0139(2) 0.0480(10) Uani 0.25 1 d PD . . O41S O 0.233(3) 0.6388(19) 0.087(2) 0.092(8) Uani 0.25 1 d PD . . O42S O 0.510(2) 0.373(4) 0.097(2) 0.092(8) Uani 0.25 1 d PD . . O52S O 0.410(2) 0.728(5) 0.011(2) 0.092(8) Uani 0.25 1 d PD . . O51S O 0.0478(6) 0.826(4) 0.023(2) 0.092(8) Uani 0.25 1 d PD . . O53S O 0.191(5) 0.734(5) -0.0757(10) 0.092(8) Uani 0.25 1 d PD . . O54S O 0.224(5) 0.584(2) -0.001(2) 0.092(8) Uani 0.25 1 d PD . . Cd6 Cd 0.1783(3) 1.0042(4) -0.55162(19) 0.0510(11) Uani 0.25 1 d PD C 1 O62S O 0.098(2) 1.042(3) -0.6355(7) 0.041(3) Uani 0.25 1 d PD C 1 O61S O 0.3132(19) 0.920(2) -0.4918(11) 0.041(3) Uani 0.25 1 d PD C 1 O63S O 0.304(2) 1.051(3) -0.6100(14) 0.041(3) Uani 0.25 1 d PD . 1 O64S O 0.072(3) 0.950(3) -0.4823(11) 0.041(3) Uani 0.25 1 d PD C 1 Cd7 Cd 0.2301(3) 0.7816(3) -0.51810(19) 0.0470(10) Uani 0.25 1 d PD D 2 O71S O 0.212(3) 0.6393(16) -0.4685(13) 0.041(3) Uani 0.25 1 d PD D 2 O72S O 0.195(3) 0.714(3) -0.5928(9) 0.041(3) Uani 0.25 1 d PD D 2 O73S O 0.208(3) 0.9191(17) -0.5841(11) 0.041(3) Uani 0.25 1 d PD D 2 O74S O 0.288(3) 0.861(3) -0.4587(11) 0.041(3) Uani 0.25 1 d PD D 2 O76S O 0.4141(7) 0.679(2) -0.5337(15) 0.041(3) Uani 0.25 1 d PD D 2 O75S O 0.0489(9) 0.876(2) -0.4884(15) 0.041(3) Uani 0.25 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0109(3) 0.0165(3) 0.0161(3) 0.0011(2) -0.0023(2) -0.0003(3) Cd2 0.0311(4) 0.0257(4) 0.0249(4) -0.0016(3) -0.0013(3) -0.0121(3) Cd3 0.082(3) 0.060(2) 0.0395(16) 0.0022(15) 0.002(2) -0.026(2) O4 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) Cd3' 0.073(2) 0.0429(19) 0.0367(16) -0.0119(14) 0.0096(17) -0.0375(18) O4' 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) Si1 0.0073(11) 0.0143(12) 0.0221(13) -0.0027(10) 0.0007(9) -0.0001(9) Si2 0.228(9) 0.121(5) 0.030(2) -0.001(3) -0.002(4) -0.140(6) O1 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) O2 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) O3 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) O5 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) O6 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) O7 0.086(8) 0.115(10) 0.047(6) 0.028(6) -0.032(6) -0.084(8) O8 0.094(9) 0.129(11) 0.033(5) -0.006(6) -0.005(5) -0.097(9) O11 0.028(4) 0.055(6) 0.024(4) 0.009(4) -0.007(3) -0.014(4) O12 0.035(5) 0.068(6) 0.025(4) 0.006(4) -0.007(4) -0.022(4) O14 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) O15 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) O16 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) O13 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C1 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C2 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C3 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C4 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C5 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C6 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C7 0.0197(16) 0.0272(17) 0.0337(18) 0.0045(14) -0.0141(13) 0.0005(13) C8 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C9 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C10 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C11 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C12 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C13 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C14 0.068(3) 0.069(3) 0.040(3) -0.005(2) 0.000(2) -0.042(3) C15 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C16 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C17 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C18 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C19 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C20 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C21 0.035(2) 0.0237(18) 0.049(2) -0.0067(16) -0.0042(17) -0.0044(16) C22 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C23 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C26 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C24 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C25 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C27 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C28 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C25' 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C24' 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C28' 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) C27' 0.021(2) 0.024(2) 0.033(3) -0.003(2) -0.001(2) -0.0091(19) O10 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) O9 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C31 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C32 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C33 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C34 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C35 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C36 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C37 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) O9' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C31' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C32' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C33' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C34' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C35' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C36' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C37' 0.044(3) 0.035(3) 0.052(3) -0.006(2) 0.005(3) -0.011(2) C38 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C39 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C40 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C41 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C42 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C43 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C44 0.055(3) 0.069(4) 0.034(3) 0.003(3) -0.006(2) -0.035(3) C45 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C46 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C47 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C48 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C49 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C50 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C51 0.168(7) 0.093(4) 0.051(3) 0.025(3) -0.029(4) -0.083(5) C52 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C53 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C54 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C55 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C56 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C57 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) C58 0.141(6) 0.091(5) 0.090(5) -0.061(4) 0.077(5) -0.072(5) Cd4 0.044(2) 0.066(3) 0.053(3) 0.011(2) -0.019(2) -0.014(2) Cd5 0.036(2) 0.044(2) 0.067(3) 0.000(2) -0.0030(19) -0.0204(18) O41S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) O42S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) O52S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) O51S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) O53S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) O54S 0.112(19) 0.14(2) 0.063(13) 0.021(14) -0.030(13) -0.085(18) Cd6 0.045(2) 0.056(3) 0.049(2) 0.009(2) -0.0166(19) -0.017(2) O62S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O61S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O63S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O64S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) Cd7 0.039(2) 0.048(2) 0.058(3) 0.0024(19) -0.0022(18) -0.0235(18) O71S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O72S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O73S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O74S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O76S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) O75S 0.048(7) 0.037(6) 0.045(7) -0.014(5) 0.015(5) -0.027(5) _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 O6 2.210(8) 1_465 ? Cd1 O7 2.225(10) 1_455 ? Cd1 O11 2.277(8) 2_574 ? Cd1 O63S 2.37(3) 2_574 ? Cd1 O1 2.377(7) . ? Cd1 O2 2.386(7) . ? Cd1 O12 2.454(9) 2_574 ? Cd1 C38 2.667(9) 2_574 ? Cd1 C1 2.726(4) . ? Cd2 O8 2.176(9) 1_455 ? Cd2 O9' 2.22(2) . ? Cd2 O14 2.267(15) 1_545 ? Cd2 O1 2.303(8) . ? Cd2 O15 2.346(12) 1_455 ? Cd2 O9 2.39(2) . ? Cd2 O5 2.403(9) 1_465 ? Cd3 O16 2.070(17) 2_665 ? Cd3 O15 2.12(2) 2_665 ? Cd3 O4 2.235(14) . ? Cd3 O10 2.305(11) 2_565 ? Cd3 C52 2.389(10) 2_665 ? Cd3 O3 2.447(11) . ? O4 C8 1.260(2) . ? Cd3' O10 2.139(11) 2_565 ? Cd3' O3 2.181(11) . ? Cd3' O13 2.202(18) 2_575 ? Cd3' O4' 2.524(15) . ? Cd3' O15 2.61(2) 2_665 ? Cd3' O16 2.624(18) 2_665 ? Cd3' C8 2.703(8) . ? O4' C8 1.261(2) . ? O4' Cd4 2.233(9) . ? Si1 C12 1.886(6) . ? Si1 C5 1.893(5) . ? Si1 C19 1.905(5) . ? Si1 C26 1.913(6) . ? Si2 C49 1.839(11) . ? Si2 C35 1.839(11) . ? Si2 C35' 1.887(3) . ? Si2 C42 1.918(10) . ? Si2 C56 1.929(12) . ? O1 C1 1.244(13) . ? O2 C1 1.278(13) . ? O3 C8 1.384(11) . ? O5 C15 1.180(14) . ? O5 Cd2 2.403(8) 1_645 ? O6 O63S 0.714(16) 2_664 ? O6 C15 1.181(15) . ? O6 Cd1 2.210(8) 1_645 ? O7 C22 1.226(14) . ? O7 Cd1 2.225(10) 1_655 ? O8 C22 1.204(14) . ? O8 Cd2 2.176(9) 1_655 ? O11 C38 1.207(16) . ? O11 Cd1 2.277(8) 2_574 ? O12 C38 1.261(16) . ? O12 Cd6 2.376(12) . ? O12 Cd1 2.454(9) 2_574 ? O14 C45 1.17(2) . ? O14 Cd2 2.267(15) 1_565 ? O15 C52 1.37(2) . ? O15 Cd3 2.12(2) 2_665 ? O15 Cd2 2.346(12) 1_655 ? O15 Cd3' 2.61(2) 2_665 ? O16 C52 1.18(2) . ? O16 Cd3 2.070(17) 2_665 ? O16 Cd3' 2.624(18) 2_665 ? O13 C45 1.35(2) . ? O13 Cd3' 2.202(18) 2_575 ? C1 C2 1.5080(11) . ? C2 C7 1.3899(10) . ? C2 C3 1.3900(10) . ? C3 C4 1.3903(10) . ? C3 H3A 0.9500 . ? C4 C5 1.3903(9) . ? C4 H4A 0.9500 . ? C5 C6 1.3902(10) . ? C6 C7 1.3901(10) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.5080(11) . ? C9 C14 1.3900(10) . ? C9 C10 1.3901(10) . ? C10 C11 1.3901(10) . ? C10 H10A 0.9500 . ? C11 C12 1.3903(9) . ? C11 H11A 0.9500 . ? C12 C13 1.3903(10) . ? C13 C14 1.3901(11) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.5082(11) . ? C15 O63S 1.52(2) 2_664 ? C16 C17 1.3898(10) . ? C16 C21 1.3900(11) . ? C17 C18 1.3899(10) . ? C17 H17A 0.9500 . ? C18 C19 1.3903(9) . ? C18 H18A 0.9500 . ? C19 C20 1.3905(10) . ? C20 C21 1.3903(11) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.5082(11) . ? C23 C24 1.3900(11) . ? C23 C24' 1.3900(11) . ? C23 C28' 1.3900(11) . ? C23 C28 1.3901(11) . ? C26 C27' 1.3900(11) . ? C26 C25' 1.3900(11) . ? C26 C27 1.3903(10) . ? C26 C25 1.3904(9) . ? C24 C25 1.3900(10) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C27 C28 1.3902(10) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C25' C24' 1.3900(11) . ? C25' H25B 0.9500 . ? C24' H24B 0.9500 . ? C28' C27' 1.3900(11) . ? C28' H28B 0.9500 . ? C27' H27B 0.9500 . ? O10 C31 1.16(2) . ? O10 C31' 1.38(3) . ? O10 Cd3' 2.139(11) 2_565 ? O10 Cd3 2.305(11) 2_565 ? O9 C31 1.32(3) . ? C31 C32 1.5080(11) . ? C32 C37 1.3900(11) . ? C32 C33 1.3900(10) . ? C33 C34 1.3902(10) . ? C33 H33A 0.9500 . ? C34 C35 1.3903(9) . ? C34 H34A 0.9500 . ? C35 C36 1.3902(10) . ? C36 C37 1.3901(10) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? O9' C31' 1.39(3) . ? C31' C32' 1.5081(11) . ? C32' C33' 1.3898(10) . ? C32' C37' 1.3901(11) . ? C33' C34' 1.3898(10) . ? C33' H33B 0.9500 . ? C34' C35' 1.3904(9) . ? C34' H34B 0.9500 . ? C35' C36' 1.3907(10) . ? C36' C37' 1.3902(10) . ? C36' H36B 0.9500 . ? C37' H37B 0.9500 . ? C38 C39 1.5080(11) . ? C38 Cd1 2.667(9) 2_574 ? C39 C40 1.3900(11) . ? C39 C44 1.3899(11) . ? C40 C41 1.3899(11) . ? C40 H40A 0.9500 . ? C41 C42 1.3900(11) . ? C41 H41A 0.9500 . ? C42 C43 1.3901(11) . ? C43 C44 1.3900(11) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.5080(11) . ? C46 C47 1.3899(11) . ? C46 C51 1.3899(11) . ? C47 C48 1.3899(11) . ? C47 H47A 0.9500 . ? C48 C49 1.3899(10) . ? C48 H48A 0.9500 . ? C49 C50 1.3900(11) . ? C50 C51 1.3900(11) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.5080(11) . ? C52 Cd3 2.389(10) 2_665 ? C53 C58 1.3900(10) . ? C53 C54 1.3901(10) . ? C54 C55 1.3901(10) . ? C54 H54A 0.9500 . ? C55 C56 1.3903(9) . ? C55 H55A 0.9500 . ? C56 C57 1.3902(10) . ? C57 C58 1.3901(10) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? Cd4 O54S 2.31(5) . ? Cd4 O42S 2.349(3) . ? Cd4 O41S 2.349(3) . ? Cd4 Cd5 3.478(7) . ? Cd5 O41S 2.15(5) . ? Cd5 O52S 2.350(3) . ? Cd5 O51S 2.350(3) . ? Cd5 O54S 2.350(3) . ? Cd5 O53S 2.350(3) . ? Cd6 O64S 2.349(3) . ? Cd6 O62S 2.350(3) . ? Cd6 O63S 2.350(3) . ? Cd6 O61S 2.351(3) . ? O63S O6 0.714(16) 2_664 ? O63S C15 1.52(2) 2_664 ? O63S Cd1 2.37(3) 2_574 ? Cd7 O71S 2.349(3) . ? Cd7 O75S 2.350(3) . ? Cd7 O76S 2.350(3) . ? Cd7 O74S 2.350(3) . ? Cd7 O73S 2.350(3) . ? Cd7 O72S 2.351(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cd1 O7 109.7(5) 1_465 1_455 ? O6 Cd1 O11 96.3(3) 1_465 2_574 ? O7 Cd1 O11 94.8(3) 1_455 2_574 ? O6 Cd1 O63S 17.5(5) 1_465 2_574 ? O7 Cd1 O63S 127.0(5) 1_455 2_574 ? O11 Cd1 O63S 95.8(10) 2_574 2_574 ? O6 Cd1 O1 99.7(3) 1_465 . ? O7 Cd1 O1 102.7(3) 1_455 . ? O11 Cd1 O1 150.6(3) 2_574 . ? O63S Cd1 O1 92.3(10) 2_574 . ? O6 Cd1 O2 149.7(3) 1_465 . ? O7 Cd1 O2 93.7(4) 1_455 . ? O11 Cd1 O2 100.9(3) 2_574 . ? O63S Cd1 O2 134.3(8) 2_574 . ? O1 Cd1 O2 55.1(3) . . ? O6 Cd1 O12 86.3(3) 1_465 2_574 ? O7 Cd1 O12 147.9(4) 1_455 2_574 ? O11 Cd1 O12 54.9(3) 2_574 2_574 ? O63S Cd1 O12 72.2(4) 2_574 2_574 ? O1 Cd1 O12 101.6(3) . 2_574 ? O2 Cd1 O12 83.4(3) . 2_574 ? O6 Cd1 C38 92.3(4) 1_465 2_574 ? O7 Cd1 C38 120.8(4) 1_455 2_574 ? O11 Cd1 C38 26.8(4) 2_574 2_574 ? O63S Cd1 C38 84.3(8) 2_574 2_574 ? O1 Cd1 C38 127.5(4) . 2_574 ? O2 Cd1 C38 91.9(4) . 2_574 ? O12 Cd1 C38 28.1(4) 2_574 2_574 ? O6 Cd1 C1 124.9(3) 1_465 . ? O7 Cd1 C1 100.0(4) 1_455 . ? O11 Cd1 C1 126.8(3) 2_574 . ? O63S Cd1 C1 113.8(10) 2_574 . ? O1 Cd1 C1 27.1(3) . . ? O2 Cd1 C1 28.0(3) . . ? O12 Cd1 C1 92.3(3) 2_574 . ? C38 Cd1 C1 110.9(4) 2_574 . ? O8 Cd2 O9' 160.8(6) 1_455 . ? O8 Cd2 O14 82.9(5) 1_455 1_545 ? O9' Cd2 O14 113.5(6) . 1_545 ? O8 Cd2 O1 88.7(4) 1_455 . ? O9' Cd2 O1 99.9(5) . . ? O14 Cd2 O1 92.7(4) 1_545 . ? O8 Cd2 O15 89.9(5) 1_455 1_455 ? O9' Cd2 O15 81.7(6) . 1_455 ? O14 Cd2 O15 86.2(6) 1_545 1_455 ? O1 Cd2 O15 178.3(4) . 1_455 ? O8 Cd2 O9 158.7(6) 1_455 . ? O9' Cd2 O9 40.4(6) . . ? O14 Cd2 O9 78.0(6) 1_545 . ? O1 Cd2 O9 82.9(5) . . ? O15 Cd2 O9 98.0(6) 1_455 . ? O8 Cd2 O5 80.4(4) 1_455 1_465 ? O9' Cd2 O5 83.5(6) . 1_465 ? O14 Cd2 O5 162.9(4) 1_545 1_465 ? O1 Cd2 O5 83.8(3) . 1_465 ? O15 Cd2 O5 96.9(5) 1_455 1_465 ? O9 Cd2 O5 117.9(5) . 1_465 ? O16 Cd3 O15 64.3(6) 2_665 2_665 ? O16 Cd3 O4 80.3(6) 2_665 . ? O15 Cd3 O4 105.8(5) 2_665 . ? O16 Cd3 O10 96.2(5) 2_665 2_565 ? O15 Cd3 O10 108.6(5) 2_665 2_565 ? O4 Cd3 O10 139.7(4) . 2_565 ? O16 Cd3 C52 29.6(6) 2_665 2_665 ? O15 Cd3 C52 34.7(5) 2_665 2_665 ? O4 Cd3 C52 92.4(6) . 2_665 ? O10 Cd3 C52 104.1(6) 2_565 2_665 ? O16 Cd3 O3 102.3(6) 2_665 . ? O15 Cd3 O3 160.7(5) 2_665 . ? O4 Cd3 O3 56.4(2) . . ? O10 Cd3 O3 85.9(4) 2_565 . ? C52 Cd3 O3 130.7(5) 2_665 . ? C8 O4 Cd3 101.0(7) . . ? O10 Cd3' O3 97.2(4) 2_565 . ? O10 Cd3' O13 104.0(5) 2_565 2_575 ? O3 Cd3' O13 105.8(5) . 2_575 ? O10 Cd3' O4' 151.9(4) 2_565 . ? O3 Cd3' O4' 55.7(3) . . ? O13 Cd3' O4' 91.6(6) 2_575 . ? O10 Cd3' O15 97.8(4) 2_565 2_665 ? O3 Cd3' O15 139.7(4) . 2_665 ? O13 Cd3' O15 106.4(5) 2_575 2_665 ? O4' Cd3' O15 99.9(5) . 2_665 ? O10 Cd3' O16 85.7(4) 2_565 2_665 ? O3 Cd3' O16 94.0(5) . 2_665 ? O13 Cd3' O16 156.4(5) 2_575 2_665 ? O4' Cd3' O16 89.0(6) . 2_665 ? O15 Cd3' O16 50.4(4) 2_665 2_665 ? O10 Cd3' C8 124.3(4) 2_565 . ? O3 Cd3' C8 30.6(2) . . ? O13 Cd3' C8 107.9(4) 2_575 . ? O4' Cd3' C8 27.66(9) . . ? O15 Cd3' C8 114.7(4) 2_665 . ? O16 Cd3' C8 82.7(4) 2_665 . ? C8 O4' Cd4 166.4(11) . . ? C8 O4' Cd3' 84.1(7) . . ? Cd4 O4' Cd3' 108.9(5) . . ? C12 Si1 C5 108.8(4) . . ? C12 Si1 C19 105.5(4) . . ? C5 Si1 C19 113.5(4) . . ? C12 Si1 C26 111.2(4) . . ? C5 Si1 C26 107.8(3) . . ? C19 Si1 C26 110.1(4) . . ? C49 Si2 C35 123.4(7) . . ? C49 Si2 C35' 103.9(8) . . ? C35 Si2 C35' 23.7(6) . . ? C49 Si2 C42 110.8(6) . . ? C35 Si2 C42 111.2(7) . . ? C35' Si2 C42 112.2(7) . . ? C49 Si2 C56 111.0(6) . . ? C35 Si2 C56 95.7(7) . . ? C35' Si2 C56 117.5(7) . . ? C42 Si2 C56 101.6(6) . . ? C1 O1 Cd2 135.4(8) . . ? C1 O1 Cd1 92.3(5) . . ? Cd2 O1 Cd1 100.5(3) . . ? C1 O2 Cd1 91.0(5) . . ? C8 O3 Cd3' 96.1(4) . . ? C8 O3 Cd3 87.9(4) . . ? Cd3' O3 Cd3 13.54(15) . . ? C15 O5 Cd2 137.6(9) . 1_645 ? O63S O6 C15 103(3) 2_664 . ? O63S O6 Cd1 94(3) 2_664 1_645 ? C15 O6 Cd1 118.3(7) . 1_645 ? C22 O7 Cd1 123.6(7) . 1_655 ? C22 O8 Cd2 148.0(9) . 1_655 ? C38 O11 Cd1 94.9(7) . 2_574 ? C38 O12 Cd6 127.9(10) . . ? C38 O12 Cd1 85.3(6) . 2_574 ? Cd6 O12 Cd1 103.1(4) . 2_574 ? C45 O14 Cd2 149.7(13) . 1_565 ? C52 O15 Cd3 83.7(9) . 2_665 ? C52 O15 Cd2 130.4(12) . 1_655 ? Cd3 O15 Cd2 103.9(7) 2_665 1_655 ? C52 O15 Cd3' 92.0(9) . 2_665 ? Cd3 O15 Cd3' 8.6(2) 2_665 2_665 ? Cd2 O15 Cd3' 96.6(6) 1_655 2_665 ? C52 O16 Cd3 90.3(9) . 2_665 ? C52 O16 Cd3' 95.9(9) . 2_665 ? Cd3 O16 Cd3' 6.1(2) 2_665 2_665 ? C45 O13 Cd3' 109.8(11) . 2_575 ? O1 C1 O2 121.6(6) . . ? O1 C1 C2 120.8(9) . . ? O2 C1 C2 117.6(8) . . ? O1 C1 Cd1 60.6(4) . . ? O2 C1 Cd1 61.1(4) . . ? C2 C1 Cd1 176.4(8) . . ? C7 C2 C3 120.00(17) . . ? C7 C2 C1 119.3(6) . . ? C3 C2 C1 120.7(6) . . ? C2 C3 C4 120.01(12) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 119.99(9) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C6 C5 C4 119.98(9) . . ? C6 C5 Si1 116.3(4) . . ? C4 C5 Si1 123.7(4) . . ? C7 C6 C5 120.02(12) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C2 C7 C6 119.99(17) . . ? C2 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? O4 C8 O4' 44.9(11) . . ? O4 C8 O3 114.3(8) . . ? O4' C8 O3 114.0(8) . . ? O4 C8 C9 131.2(12) . . ? O4' C8 C9 111.8(11) . . ? O3 C8 C9 114.5(7) . . ? O4 C8 Cd3' 62.8(6) . . ? O4' C8 Cd3' 68.3(7) . . ? O3 C8 Cd3' 53.3(4) . . ? C9 C8 Cd3' 161.6(6) . . ? C14 C9 C10 119.97(18) . . ? C14 C9 C8 122.3(7) . . ? C10 C9 C8 117.0(7) . . ? C9 C10 C11 120.03(12) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 120.00(9) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 119.98(9) . . ? C11 C12 Si1 122.1(5) . . ? C13 C12 Si1 117.8(5) . . ? C14 C13 C12 120.00(12) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C9 C14 C13 120.03(18) . . ? C9 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? O5 C15 O6 108.3(8) . . ? O5 C15 C16 125.4(11) . . ? O6 C15 C16 122.3(10) . . ? O5 C15 O63S 121.7(15) . 2_664 ? O6 C15 O63S 27.2(13) . 2_664 ? C16 C15 O63S 112.7(15) . 2_664 ? C17 C16 C21 119.87(17) . . ? C17 C16 C15 120.2(7) . . ? C21 C16 C15 120.0(7) . . ? C16 C17 C18 120.07(12) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 120.03(9) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 119.94(9) . . ? C18 C19 Si1 122.9(4) . . ? C20 C19 Si1 117.1(4) . . ? C21 C20 C19 119.96(12) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C16 C21 C20 120.12(17) . . ? C16 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? O8 C22 O7 125.6(8) . . ? O8 C22 C23 118.2(9) . . ? O7 C22 C23 116.2(9) . . ? C24 C23 C24' 74.6(6) . . ? C24 C23 C28' 76.3(6) . . ? C24' C23 C28' 119.8(9) . . ? C24 C23 C28 119.91(17) . . ? C24' C23 C28 76.5(6) . . ? C28' C23 C28 74.5(6) . . ? C24 C23 C22 121.7(6) . . ? C24' C23 C22 117.3(8) . . ? C28' C23 C22 122.9(8) . . ? C28 C23 C22 118.3(6) . . ? C27' C26 C25' 120.0(9) . . ? C27' C26 C27 74.7(6) . . ? C25' C26 C27 76.4(6) . . ? C27' C26 C25 76.5(6) . . ? C25' C26 C25 74.5(6) . . ? C27 C26 C25 119.95(9) . . ? C27' C26 Si1 121.9(7) . . ? C25' C26 Si1 118.1(7) . . ? C27 C26 Si1 120.0(4) . . ? C25 C26 Si1 120.0(4) . . ? C25 C24 C23 120.06(12) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.02(9) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C28 C27 C26 119.99(12) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C23 C28 C27 120.08(17) . . ? C23 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C26 C25' C24' 120.3(13) . . ? C26 C25' H25B 119.9 . . ? C24' C25' H25B 119.9 . . ? C23 C24' C25' 119.8(13) . . ? C23 C24' H24B 120.1 . . ? C25' C24' H24B 120.1 . . ? C27' C28' C23 120.5(13) . . ? C27' C28' H28B 119.7 . . ? C23 C28' H28B 119.7 . . ? C26 C27' C28' 119.6(13) . . ? C26 C27' H27B 120.2 . . ? C28' C27' H27B 120.2 . . ? C31 O10 C31' 41.9(11) . . ? C31 O10 Cd3' 131.0(11) . 2_565 ? C31' O10 Cd3' 128.9(9) . 2_565 ? C31 O10 Cd3 132.3(11) . 2_565 ? C31' O10 Cd3 117.8(9) . 2_565 ? Cd3' O10 Cd3 15.09(14) 2_565 2_565 ? C31 O9 Cd2 141.7(13) . . ? O10 C31 O9 115.8(13) . . ? O10 C31 C32 128.6(18) . . ? O9 C31 C32 113.7(16) . . ? C37 C32 C33 119.99(18) . . ? C37 C32 C31 119.4(11) . . ? C33 C32 C31 120.6(11) . . ? C32 C33 C34 120.02(12) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 119.99(9) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 119.98(9) . . ? C36 C35 Si2 116.2(8) . . ? C34 C35 Si2 122.7(9) . . ? C37 C36 C35 120.01(12) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C32 C37 C36 120.01(18) . . ? C32 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C31' O9' Cd2 129.9(14) . . ? O10 C31' O9' 122.9(10) . . ? O10 C31' C32' 117.8(19) . . ? O9' C31' C32' 119(2) . . ? C33' C32' C37' 119.85(18) . . ? C33' C32' C31' 117.4(13) . . ? C37' C32' C31' 122.5(13) . . ? C32' C33' C34' 120.09(12) . . ? C32' C33' H33B 120.0 . . ? C34' C33' H33B 120.0 . . ? C33' C34' C35' 120.04(9) . . ? C33' C34' H34B 120.0 . . ? C35' C34' H34B 120.0 . . ? C34' C35' C36' 119.91(9) . . ? C34' C35' Si2 113.9(8) . . ? C36' C35' Si2 125.5(9) . . ? C37' C36' C35' 119.97(12) . . ? C37' C36' H36B 120.0 . . ? C35' C36' H36B 120.0 . . ? C32' C37' C36' 120.13(18) . . ? C32' C37' H37B 119.9 . . ? C36' C37' H37B 119.9 . . ? O11 C38 O12 124.8(9) . . ? O11 C38 C39 119.0(11) . . ? O12 C38 C39 116.2(11) . . ? O11 C38 Cd1 58.3(5) . 2_574 ? O12 C38 Cd1 66.5(5) . 2_574 ? C39 C38 Cd1 177.2(9) . 2_574 ? C40 C39 C44 117.4(9) . . ? C40 C39 C38 122.7(9) . . ? C44 C39 C38 119.9(9) . . ? C41 C40 C39 122.2(6) . . ? C41 C40 H40A 118.9 . . ? C39 C40 H40A 118.9 . . ? C40 C41 C42 120.05(13) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C43 118.1(7) . . ? C41 C42 Si2 118.1(6) . . ? C43 C42 Si2 122.3(7) . . ? C44 C43 C42 121.5(11) . . ? C44 C43 H43A 119.2 . . ? C42 C43 H43A 119.2 . . ? C39 C44 C43 120.7(11) . . ? C39 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? O14 C45 O13 127.3(15) . . ? O14 C45 C46 113.5(15) . . ? O13 C45 C46 110.8(14) . . ? C47 C46 C51 119.7(4) . . ? C47 C46 C45 117.6(10) . . ? C51 C46 C45 122.3(10) . . ? C48 C47 C46 120.06(13) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C49 120.05(13) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C48 C49 C50 120.03(13) . . ? C48 C49 Si2 116.3(7) . . ? C50 C49 Si2 123.3(7) . . ? C51 C50 C49 119.8(4) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C46 C51 C50 120.3(5) . . ? C46 C51 H51A 119.8 . . ? C50 C51 H51A 119.8 . . ? O16 C52 O15 121.7(14) . . ? O16 C52 C53 123.9(15) . . ? O15 C52 C53 114.1(14) . . ? O16 C52 Cd3 60.1(9) . 2_665 ? O15 C52 Cd3 61.7(9) . 2_665 ? C53 C52 Cd3 173.0(14) . 2_665 ? C58 C53 C54 119.98(18) . . ? C58 C53 C52 118.0(10) . . ? C54 C53 C52 122.0(10) . . ? C53 C54 C55 120.02(12) . . ? C53 C54 H54A 120.0 . . ? C55 C54 H54A 120.0 . . ? C54 C55 C56 120.00(9) . . ? C54 C55 H55A 120.0 . . ? C56 C55 H55A 120.0 . . ? C57 C56 C55 119.98(9) . . ? C57 C56 Si2 122.0(7) . . ? C55 C56 Si2 117.9(7) . . ? C58 C57 C56 120.00(12) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C53 C58 C57 120.02(18) . . ? C53 C58 H58A 120.0 . . ? C57 C58 H58A 120.0 . . ? O4' Cd4 O54S 77.8(6) . . ? O4' Cd4 O42S 101.5(16) . . ? O54S Cd4 O42S 168(2) . . ? O4' Cd4 O41S 125.9(14) . . ? O54S Cd4 O41S 62.2(16) . . ? O42S Cd4 O41S 125(2) . . ? O4' Cd4 Cd5 119.9(6) . . ? O54S Cd4 Cd5 42.2(2) . . ? O42S Cd4 Cd5 136.3(14) . . ? O41S Cd4 Cd5 37.3(13) . . ? O41S Cd5 O52S 99.4(19) . . ? O41S Cd5 O51S 93.4(17) . . ? O52S Cd5 O51S 152(2) . . ? O41S Cd5 O54S 64.5(16) . . ? O52S Cd5 O54S 115(2) . . ? O51S Cd5 O54S 93(2) . . ? O41S Cd5 O53S 129.7(19) . . ? O52S Cd5 O53S 111.7(19) . . ? O51S Cd5 O53S 77(2) . . ? O54S Cd5 O53S 67(2) . . ? O41S Cd5 Cd4 41.5(3) . . ? O52S Cd5 Cd4 83.8(16) . . ? O51S Cd5 Cd4 121.1(14) . . ? O54S Cd5 Cd4 41.4(13) . . ? O53S Cd5 Cd4 102.6(16) . . ? Cd5 O41S Cd4 101.2(16) . . ? Cd4 O54S Cd5 96.4(15) . . ? O64S Cd6 O62S 108.5(13) . . ? O64S Cd6 O63S 170.8(14) . . ? O62S Cd6 O63S 80.7(13) . . ? O64S Cd6 O61S 83.9(13) . . ? O62S Cd6 O61S 156.5(12) . . ? O63S Cd6 O61S 87.1(13) . . ? O64S Cd6 O12 103.8(9) . . ? O62S Cd6 O12 105.6(9) . . ? O63S Cd6 O12 73.9(9) . . ? O61S Cd6 O12 89.9(9) . . ? O6 O63S C15 49(2) 2_664 2_664 ? O6 O63S Cd6 159(4) 2_664 . ? C15 O63S Cd6 150(2) 2_664 . ? O6 O63S Cd1 69(3) 2_664 2_574 ? C15 O63S Cd1 96.8(12) 2_664 2_574 ? Cd6 O63S Cd1 106.6(11) . 2_574 ? O71S Cd7 O75S 88.0(12) . . ? O71S Cd7 O76S 86.8(12) . . ? O75S Cd7 O76S 171.5(13) . . ? O71S Cd7 O74S 108.4(13) . . ? O75S Cd7 O74S 92.1(12) . . ? O76S Cd7 O74S 83.1(12) . . ? O71S Cd7 O73S 161.7(13) . . ? O75S Cd7 O73S 84.2(12) . . ? O76S Cd7 O73S 102.7(12) . . ? O74S Cd7 O73S 88.4(13) . . ? O71S Cd7 O72S 82.2(12) . . ? O75S Cd7 O72S 95.1(12) . . ? O76S Cd7 O72S 90.9(12) . . ? O74S Cd7 O72S 167.4(12) . . ? O73S Cd7 O72S 82.1(12) . . ? 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 O16 Cd3 O4 C8 115.6(8) 2_665 . . . ? O15 Cd3 O4 C8 175.2(6) 2_665 . . . ? O10 Cd3 O4 C8 27.5(11) 2_565 . . . ? C52 Cd3 O4 C8 142.7(7) 2_665 . . . ? O3 Cd3 O4 C8 3.7(3) . . . . ? O10 Cd3' O4' C8 -3(2) 2_565 . . . ? O3 Cd3' O4' C8 -19.4(7) . . . . ? O13 Cd3' O4' C8 -127.5(11) 2_575 . . . ? O15 Cd3' O4' C8 125.5(10) 2_665 . . . ? O16 Cd3' O4' C8 76.1(10) 2_665 . . . ? O10 Cd3' O4' Cd4 -178.8(7) 2_565 . . . ? O3 Cd3' O4' Cd4 164.7(11) . . . . ? O13 Cd3' O4' Cd4 56.6(9) 2_575 . . . ? O15 Cd3' O4' Cd4 -50.4(9) 2_665 . . . ? O16 Cd3' O4' Cd4 -99.8(8) 2_665 . . . ? C8 Cd3' O4' Cd4 -175.9(17) . . . . ? O8 Cd2 O1 C1 -55.2(9) 1_455 . . . ? O9' Cd2 O1 C1 142.0(10) . . . . ? O14 Cd2 O1 C1 27.6(9) 1_545 . . . ? O15 Cd2 O1 C1 -20(19) 1_455 . . . ? O9 Cd2 O1 C1 105.2(9) . . . . ? O5 Cd2 O1 C1 -135.6(9) 1_465 . . . ? O8 Cd2 O1 Cd1 49.0(4) 1_455 . . . ? O9' Cd2 O1 Cd1 -113.8(6) . . . . ? O14 Cd2 O1 Cd1 131.8(4) 1_545 . . . ? O15 Cd2 O1 Cd1 84(19) 1_455 . . . ? O9 Cd2 O1 Cd1 -150.7(5) . . . . ? O5 Cd2 O1 Cd1 -31.5(3) 1_465 . . . ? O6 Cd1 O1 C1 -160.0(7) 1_465 . . . ? O7 Cd1 O1 C1 87.1(8) 1_455 . . . ? O11 Cd1 O1 C1 -38.0(10) 2_574 . . . ? O63S Cd1 O1 C1 -144.0(7) 2_574 . . . ? O2 Cd1 O1 C1 1.6(7) . . . . ? O12 Cd1 O1 C1 -71.8(7) 2_574 . . . ? C38 Cd1 O1 C1 -59.4(9) 2_574 . . . ? O6 Cd1 O1 Cd2 63.0(4) 1_465 . . . ? O7 Cd1 O1 Cd2 -49.9(5) 1_455 . . . ? O11 Cd1 O1 Cd2 -175.0(5) 2_574 . . . ? O63S Cd1 O1 Cd2 78.9(4) 2_574 . . . ? O2 Cd1 O1 Cd2 -135.4(4) . . . . ? O12 Cd1 O1 Cd2 151.2(3) 2_574 . . . ? C38 Cd1 O1 Cd2 163.5(5) 2_574 . . . ? C1 Cd1 O1 Cd2 -137.0(8) . . . . ? O6 Cd1 O2 C1 36.6(10) 1_465 . . . ? O7 Cd1 O2 C1 -104.5(7) 1_455 . . . ? O11 Cd1 O2 C1 159.9(7) 2_574 . . . ? O63S Cd1 O2 C1 50.5(13) 2_574 . . . ? O1 Cd1 O2 C1 -1.6(6) . . . . ? O12 Cd1 O2 C1 107.6(7) 2_574 . . . ? C38 Cd1 O2 C1 134.4(7) 2_574 . . . ? O10 Cd3' O3 C8 -154.6(5) 2_565 . . . ? O13 Cd3' O3 C8 98.6(6) 2_575 . . . ? O4' Cd3' O3 C8 17.7(6) . . . . ? O15 Cd3' O3 C8 -43.5(9) 2_665 . . . ? O16 Cd3' O3 C8 -68.4(6) 2_665 . . . ? O10 Cd3' O3 Cd3 -101.3(10) 2_565 . . . ? O13 Cd3' O3 Cd3 151.9(11) 2_575 . . . ? O4' Cd3' O3 Cd3 71.0(11) . . . . ? O15 Cd3' O3 Cd3 9.9(9) 2_665 . . . ? O16 Cd3' O3 Cd3 -15.1(9) 2_665 . . . ? C8 Cd3' O3 Cd3 53.3(11) . . . . ? O16 Cd3 O3 C8 -72.7(6) 2_665 . . . ? O15 Cd3 O3 C8 -28.6(17) 2_665 . . . ? O4 Cd3 O3 C8 -3.3(3) . . . . ? O10 Cd3 O3 C8 -168.1(5) 2_565 . . . ? C52 Cd3 O3 C8 -62.9(9) 2_665 . . . ? O16 Cd3 O3 Cd3' 160.3(12) 2_665 . . . ? O15 Cd3 O3 Cd3' -156(2) 2_665 . . . ? O4 Cd3 O3 Cd3' -130.3(11) . . . . ? O10 Cd3 O3 Cd3' 64.9(9) 2_565 . . . ? C52 Cd3 O3 Cd3' 170.0(14) 2_665 . . . ? Cd2 O1 C1 O2 104.5(12) . . . . ? Cd1 O1 C1 O2 -2.9(12) . . . . ? Cd2 O1 C1 C2 -76.5(13) . . . . ? Cd1 O1 C1 C2 176.1(9) . . . . ? Cd2 O1 C1 Cd1 107.4(8) . . . . ? Cd1 O2 C1 O1 2.9(12) . . . . ? Cd1 O2 C1 C2 -176.2(9) . . . . ? O6 Cd1 C1 O1 24.3(9) 1_465 . . . ? O7 Cd1 C1 O1 -98.4(7) 1_455 . . . ? O11 Cd1 C1 O1 157.8(6) 2_574 . . . ? O63S Cd1 C1 O1 39.9(9) 2_574 . . . ? O2 Cd1 C1 O1 -177.2(12) . . . . ? O12 Cd1 C1 O1 111.4(7) 2_574 . . . ? C38 Cd1 C1 O1 133.0(7) 2_574 . . . ? O6 Cd1 C1 O2 -158.5(6) 1_465 . . . ? O7 Cd1 C1 O2 78.8(7) 1_455 . . . ? O11 Cd1 C1 O2 -25.0(8) 2_574 . . . ? O63S Cd1 C1 O2 -142.9(8) 2_574 . . . ? O1 Cd1 C1 O2 177.2(12) . . . . ? O12 Cd1 C1 O2 -71.4(7) 2_574 . . . ? C38 Cd1 C1 O2 -49.8(8) 2_574 . . . ? O6 Cd1 C1 C2 -90(12) 1_465 . . . ? O7 Cd1 C1 C2 148(12) 1_455 . . . ? O11 Cd1 C1 C2 44(13) 2_574 . . . ? O63S Cd1 C1 C2 -74(12) 2_574 . . . ? O1 Cd1 C1 C2 -114(13) . . . . ? O2 Cd1 C1 C2 69(12) . . . . ? O12 Cd1 C1 C2 -3(12) 2_574 . . . ? C38 Cd1 C1 C2 19(12) 2_574 . . . ? O1 C1 C2 C7 -3.6(14) . . . . ? O2 C1 C2 C7 175.4(8) . . . . ? Cd1 C1 C2 C7 108(12) . . . . ? O1 C1 C2 C3 175.9(9) . . . . ? O2 C1 C2 C3 -5.1(13) . . . . ? Cd1 C1 C2 C3 -72(13) . . . . ? C7 C2 C3 C4 -0.1(10) . . . . ? C1 C2 C3 C4 -179.4(8) . . . . ? C2 C3 C4 C5 0.1(10) . . . . ? C3 C4 C5 C6 0.00(6) . . . . ? C3 C4 C5 Si1 -177.5(6) . . . . ? C12 Si1 C5 C6 47.8(6) . . . . ? C19 Si1 C5 C6 164.8(4) . . . . ? C26 Si1 C5 C6 -73.0(5) . . . . ? C12 Si1 C5 C4 -134.7(5) . . . . ? C19 Si1 C5 C4 -17.6(6) . . . . ? C26 Si1 C5 C4 104.6(5) . . . . ? C4 C5 C6 C7 0.00(9) . . . . ? Si1 C5 C6 C7 177.7(6) . . . . ? C3 C2 C7 C6 0.1(10) . . . . ? C1 C2 C7 C6 179.5(8) . . . . ? C5 C6 C7 C2 -0.1(10) . . . . ? Cd3 O4 C8 O4' 94.3(7) . . . . ? Cd3 O4 C8 O3 -5.9(5) . . . . ? Cd3 O4 C8 C9 174.1(5) . . . . ? Cd3 O4 C8 Cd3' 8.6(2) . . . . ? Cd4 O4' C8 O4 90(7) . . . . ? Cd3' O4' C8 O4 -72.8(8) . . . . ? Cd4 O4' C8 O3 -169(6) . . . . ? Cd3' O4' C8 O3 28.3(9) . . . . ? Cd4 O4' C8 C9 -37(7) . . . . ? Cd3' O4' C8 C9 160.2(7) . . . . ? Cd4 O4' C8 Cd3' 163(7) . . . . ? Cd3' O3 C8 O4 16.2(5) . . . . ? Cd3 O3 C8 O4 5.3(5) . . . . ? Cd3' O3 C8 O4' -33.3(12) . . . . ? Cd3 O3 C8 O4' -44.1(12) . . . . ? Cd3' O3 C8 C9 -163.8(5) . . . . ? Cd3 O3 C8 C9 -174.7(5) . . . . ? Cd3 O3 C8 Cd3' -10.83(19) . . . . ? O10 Cd3' C8 O4 -132.4(8) 2_565 . . . ? O3 Cd3' C8 O4 -163.4(5) . . . . ? O13 Cd3' C8 O4 105.7(8) 2_575 . . . ? O4' Cd3' C8 O4 49.2(12) . . . . ? O15 Cd3' C8 O4 -12.7(7) 2_665 . . . ? O16 Cd3' C8 O4 -52.7(7) 2_665 . . . ? O10 Cd3' C8 O4' 178.4(11) 2_565 . . . ? O3 Cd3' C8 O4' 147.3(11) . . . . ? O13 Cd3' C8 O4' 56.5(12) 2_575 . . . ? O15 Cd3' C8 O4' -62.0(11) 2_665 . . . ? O16 Cd3' C8 O4' -101.9(11) 2_665 . . . ? O10 Cd3' C8 O3 31.0(6) 2_565 . . . ? O13 Cd3' C8 O3 -90.9(7) 2_575 . . . ? O4' Cd3' C8 O3 -147.3(11) . . . . ? O15 Cd3' C8 O3 150.7(6) 2_665 . . . ? O16 Cd3' C8 O3 110.7(6) 2_665 . . . ? O10 Cd3' C8 C9 84.3(19) 2_565 . . . ? O3 Cd3' C8 C9 53(2) . . . . ? O13 Cd3' C8 C9 -38(2) 2_575 . . . ? O4' Cd3' C8 C9 -94.1(19) . . . . ? O15 Cd3' C8 C9 -156.0(19) 2_665 . . . ? O16 Cd3' C8 C9 164.0(19) 2_665 . . . ? O4 C8 C9 C14 169.8(7) . . . . ? O4' C8 C9 C14 -141.8(12) . . . . ? O3 C8 C9 C14 -10.2(7) . . . . ? Cd3' C8 C9 C14 -55(2) . . . . ? O4 C8 C9 C10 -0.3(6) . . . . ? O4' C8 C9 C10 48.1(12) . . . . ? O3 C8 C9 C10 179.7(6) . . . . ? Cd3' C8 C9 C10 134.7(18) . . . . ? C14 C9 C10 C11 0.00(3) . . . . ? C8 C9 C10 C11 170.4(6) . . . . ? C9 C10 C11 C12 0.00(3) . . . . ? C10 C11 C12 C13 0.00(6) . . . . ? C10 C11 C12 Si1 -177.0(7) . . . . ? C5 Si1 C12 C11 -138.4(6) . . . . ? C19 Si1 C12 C11 99.6(6) . . . . ? C26 Si1 C12 C11 -19.8(7) . . . . ? C5 Si1 C12 C13 44.5(6) . . . . ? C19 Si1 C12 C13 -77.5(6) . . . . ? C26 Si1 C12 C13 163.1(5) . . . . ? C11 C12 C13 C14 0.00(9) . . . . ? Si1 C12 C13 C14 177.2(7) . . . . ? C10 C9 C14 C13 0.00(6) . . . . ? C8 C9 C14 C13 -169.8(6) . . . . ? C12 C13 C14 C9 0.00(9) . . . . ? Cd2 O5 C15 O6 97.6(14) 1_645 . . . ? Cd2 O5 C15 C16 -104.3(13) 1_645 . . . ? Cd2 O5 C15 O63S 71(2) 1_645 . . 2_664 ? O63S O6 C15 O5 -124(4) 2_664 . . . ? Cd1 O6 C15 O5 -22.3(15) 1_645 . . . ? O63S O6 C15 C16 77(4) 2_664 . . . ? Cd1 O6 C15 C16 178.7(7) 1_645 . . . ? Cd1 O6 C15 O63S 102(4) 1_645 . . 2_664 ? O5 C15 C16 C17 -158.8(11) . . . . ? O6 C15 C16 C17 -3.6(16) . . . . ? O63S C15 C16 C17 25(2) 2_664 . . . ? O5 C15 C16 C21 20.1(16) . . . . ? O6 C15 C16 C21 175.4(10) . . . . ? O63S C15 C16 C21 -155.7(17) 2_664 . . . ? C21 C16 C17 C18 0.00(3) . . . . ? C15 C16 C17 C18 179.0(8) . . . . ? C16 C17 C18 C19 0.00(3) . . . . ? C17 C18 C19 C20 0.00(6) . . . . ? C17 C18 C19 Si1 176.2(6) . . . . ? C12 Si1 C19 C18 -179.3(5) . . . . ? C5 Si1 C19 C18 61.6(6) . . . . ? C26 Si1 C19 C18 -59.2(5) . . . . ? C12 Si1 C19 C20 -3.1(5) . . . . ? C5 Si1 C19 C20 -122.1(5) . . . . ? C26 Si1 C19 C20 117.0(5) . . . . ? C18 C19 C20 C21 0.1(14) . . . . ? Si1 C19 C20 C21 -176.4(6) . . . . ? C17 C16 C21 C20 0.00(6) . . . . ? C15 C16 C21 C20 -179.0(8) . . . . ? C19 C20 C21 C16 -0.1(14) . . . . ? Cd2 O8 C22 O7 19(3) 1_655 . . . ? Cd2 O8 C22 C23 -162.5(14) 1_655 . . . ? Cd1 O7 C22 O8 1(2) 1_655 . . . ? Cd1 O7 C22 C23 -177.4(7) 1_655 . . . ? O8 C22 C23 C24 137.1(11) . . . . ? O7 C22 C23 C24 -44.3(13) . . . . ? O8 C22 C23 C24' 48.9(13) . . . . ? O7 C22 C23 C24' -132.4(11) . . . . ? O8 C22 C23 C28' -129.1(12) . . . . ? O7 C22 C23 C28' 49.6(13) . . . . ? O8 C22 C23 C28 -39.9(14) . . . . ? O7 C22 C23 C28 138.8(11) . . . . ? C12 Si1 C26 C27' 142.4(6) . . . . ? C5 Si1 C26 C27' -98.4(6) . . . . ? C19 Si1 C26 C27' 25.9(6) . . . . ? C12 Si1 C26 C25' -37.6(7) . . . . ? C5 Si1 C26 C25' 81.6(6) . . . . ? C19 Si1 C26 C25' -154.1(6) . . . . ? C12 Si1 C26 C27 52.4(7) . . . . ? C5 Si1 C26 C27 171.6(5) . . . . ? C19 Si1 C26 C27 -64.2(6) . . . . ? C12 Si1 C26 C25 -125.2(6) . . . . ? C5 Si1 C26 C25 -6.0(6) . . . . ? C19 Si1 C26 C25 118.3(6) . . . . ? C24' C23 C24 C25 -64.0(7) . . . . ? C28' C23 C24 C25 62.7(7) . . . . ? C28 C23 C24 C25 0.00(3) . . . . ? C22 C23 C24 C25 -176.9(7) . . . . ? C23 C24 C25 C26 0.00(3) . . . . ? C27' C26 C25 C24 -63.1(6) . . . . ? C25' C26 C25 C24 63.8(6) . . . . ? C27 C26 C25 C24 0.00(6) . . . . ? Si1 C26 C25 C24 177.6(5) . . . . ? C27' C26 C27 C28 64.1(7) . . . . ? C25' C26 C27 C28 -62.8(7) . . . . ? C25 C26 C27 C28 0.00(9) . . . . ? Si1 C26 C27 C28 -177.6(5) . . . . ? C24 C23 C28 C27 0.00(6) . . . . ? C24' C23 C28 C27 63.0(6) . . . . ? C28' C23 C28 C27 -63.7(7) . . . . ? C22 C23 C28 C27 177.0(7) . . . . ? C26 C27 C28 C23 0.00(9) . . . . ? C27' C26 C25' C24' 0.00(6) . . . . ? C27 C26 C25' C24' 63.0(3) . . . . ? C25 C26 C25' C24' -63.9(3) . . . . ? Si1 C26 C25' C24' -180.0(5) . . . . ? C24 C23 C24' C25' 63.9(3) . . . . ? C28' C23 C24' C25' 0.00(3) . . . . ? C28 C23 C24' C25' -62.9(3) . . . . ? C22 C23 C24' C25' -178.0(6) . . . . ? C26 C25' C24' C23 0.00(3) . . . . ? C24 C23 C28' C27' -63.0(3) . . . . ? C24' C23 C28' C27' 0.00(6) . . . . ? C28 C23 C28' C27' 63.9(3) . . . . ? C22 C23 C28' C27' 177.9(7) . . . . ? C25' C26 C27' C28' 0.00(9) . . . . ? C27 C26 C27' C28' -63.9(3) . . . . ? C25 C26 C27' C28' 62.9(3) . . . . ? Si1 C26 C27' C28' 180.0(5) . . . . ? C23 C28' C27' C26 0.00(9) . . . . ? O8 Cd2 O9 C31 -125.7(19) 1_455 . . . ? O9' Cd2 O9 C31 52(2) . . . . ? O14 Cd2 O9 C31 -99(2) 1_545 . . . ? O1 Cd2 O9 C31 167(2) . . . . ? O15 Cd2 O9 C31 -15(2) 1_455 . . . ? O5 Cd2 O9 C31 87(2) 1_465 . . . ? C31' O10 C31 O9 -77.9(19) . . . . ? Cd3' O10 C31 O9 28.2(19) 2_565 . . . ? Cd3 O10 C31 O9 8.1(19) 2_565 . . . ? C31' O10 C31 C32 85.5(16) . . . . ? Cd3' O10 C31 C32 -168.4(6) 2_565 . . . ? Cd3 O10 C31 C32 171.5(5) 2_565 . . . ? Cd2 O9 C31 O10 26(3) . . . . ? Cd2 O9 C31 C32 -140.0(17) . . . . ? O10 C31 C32 C37 -13.9(13) . . . . ? O9 C31 C32 C37 149.8(12) . . . . ? O10 C31 C32 C33 166.1(13) . . . . ? O9 C31 C32 C33 -30.2(12) . . . . ? C37 C32 C33 C34 0.00(4) . . . . ? C31 C32 C33 C34 180.00(3) . . . . ? C32 C33 C34 C35 0.00(6) . . . . ? C33 C34 C35 C36 0.01(8) . . . . ? C33 C34 C35 Si2 -167.7(10) . . . . ? C49 Si2 C35 C36 -14.0(12) . . . . ? C35' Si2 C35 C36 -52.2(18) . . . . ? C42 Si2 C35 C36 -149.4(8) . . . . ? C56 Si2 C35 C36 105.7(8) . . . . ? C49 Si2 C35 C34 154.1(9) . . . . ? C35' Si2 C35 C34 116(2) . . . . ? C42 Si2 C35 C34 18.7(11) . . . . ? C56 Si2 C35 C34 -86.1(9) . . . . ? C34 C35 C36 C37 0.00(8) . . . . ? Si2 C35 C36 C37 168.5(10) . . . . ? C33 C32 C37 C36 0.00(6) . . . . ? C31 C32 C37 C36 180.00(4) . . . . ? C35 C36 C37 C32 0.00(8) . . . . ? O8 Cd2 O9' C31' 149.5(17) 1_455 . . . ? O14 Cd2 O9' C31' 2(2) 1_545 . . . ? O1 Cd2 O9' C31' -94.9(19) . . . . ? O15 Cd2 O9' C31' 84.6(19) 1_455 . . . ? O9 Cd2 O9' C31' -28.2(17) . . . . ? O5 Cd2 O9' C31' -177.4(19) 1_465 . . . ? C31 O10 C31' O9' 114(3) . . . . ? Cd3' O10 C31' O9' 3(3) 2_565 . . . ? Cd3 O10 C31' O9' -10(3) 2_565 . . . ? C31 O10 C31' C32' -67.7(19) . . . . ? Cd3' O10 C31' C32' -178.9(10) 2_565 . . . ? Cd3 O10 C31' C32' 168.8(12) 2_565 . . . ? Cd2 O9' C31' O10 -46(3) . . . . ? Cd2 O9' C31' C32' 135.8(16) . . . . ? O10 C31' C32' C33' 28(2) . . . . ? O9' C31' C32' C33' -154.0(16) . . . . ? O10 C31' C32' C37' -157.3(14) . . . . ? O9' C31' C32' C37' 21(3) . . . . ? C37' C32' C33' C34' 0.00(3) . . . . ? C31' C32' C33' C34' 175.3(16) . . . . ? C32' C33' C34' C35' 0.00(3) . . . . ? C33' C34' C35' C36' 0.01(6) . . . . ? C33' C34' C35' Si2 -170.8(11) . . . . ? C49 Si2 C35' C34' -118.7(8) . . . . ? C35 Si2 C35' C34' 29.1(16) . . . . ? C42 Si2 C35' C34' 121.5(9) . . . . ? C56 Si2 C35' C34' 4.3(11) . . . . ? C49 Si2 C35' C36' 71.0(10) . . . . ? C35 Si2 C35' C36' -141(2) . . . . ? C42 Si2 C35' C36' -48.7(11) . . . . ? C56 Si2 C35' C36' -166.0(8) . . . . ? C34' C35' C36' C37' -0.01(9) . . . . ? Si2 C35' C36' C37' 169.7(12) . . . . ? C33' C32' C37' C36' 0.00(6) . . . . ? C31' C32' C37' C36' -175.1(16) . . . . ? C35' C36' C37' C32' 0.01(9) . . . . ? Cd1 O11 C38 O12 3.1(18) 2_574 . . . ? Cd1 O11 C38 C39 -179.6(12) 2_574 . . . ? Cd6 O12 C38 O11 100.0(17) . . . . ? Cd1 O12 C38 O11 -2.9(16) 2_574 . . . ? Cd6 O12 C38 C39 -77.2(15) . . . . ? Cd1 O12 C38 C39 179.8(12) 2_574 . . . ? Cd6 O12 C38 Cd1 103.0(7) . . . 2_574 ? O11 C38 C39 C40 173.1(11) . . . . ? O12 C38 C39 C40 -9.5(18) . . . . ? Cd1 C38 C39 C40 167(22) 2_574 . . . ? O11 C38 C39 C44 -7.2(18) . . . . ? O12 C38 C39 C44 170.3(10) . . . . ? Cd1 C38 C39 C44 -13(23) 2_574 . . . ? C44 C39 C40 C41 0.00(3) . . . . ? C38 C39 C40 C41 179.8(10) . . . . ? C39 C40 C41 C42 0.00(3) . . . . ? C40 C41 C42 C43 -0.01(6) . . . . ? C40 C41 C42 Si2 166.4(7) . . . . ? C49 Si2 C42 C41 -94.4(8) . . . . ? C35 Si2 C42 C41 46.7(9) . . . . ? C35' Si2 C42 C41 21.2(9) . . . . ? C56 Si2 C42 C41 147.6(6) . . . . ? C49 Si2 C42 C43 71.4(9) . . . . ? C35 Si2 C42 C43 -147.4(7) . . . . ? C35' Si2 C42 C43 -173.0(7) . . . . ? C56 Si2 C42 C43 -46.6(8) . . . . ? C41 C42 C43 C44 0.1(17) . . . . ? Si2 C42 C43 C44 -165.8(8) . . . . ? C40 C39 C44 C43 0.1(14) . . . . ? C38 C39 C44 C43 -179.8(10) . . . . ? C42 C43 C44 C39 -0.1(17) . . . . ? Cd2 O14 C45 O13 -42(5) 1_565 . . . ? Cd2 O14 C45 C46 173.4(19) 1_565 . . . ? Cd3' O13 C45 O14 44(3) 2_575 . . . ? Cd3' O13 C45 C46 -170.7(11) 2_575 . . . ? O14 C45 C46 C47 5(2) . . . . ? O13 C45 C46 C47 -145.8(13) . . . . ? O14 C45 C46 C51 -168.1(15) . . . . ? O13 C45 C46 C51 41(2) . . . . ? C51 C46 C47 C48 0.00(3) . . . . ? C45 C46 C47 C48 -173.1(13) . . . . ? C46 C47 C48 C49 0.00(3) . . . . ? C47 C48 C49 C50 0.00(6) . . . . ? C47 C48 C49 Si2 173.8(10) . . . . ? C35 Si2 C49 C48 -126.2(9) . . . . ? C35' Si2 C49 C48 -111.4(9) . . . . ? C42 Si2 C49 C48 9.3(10) . . . . ? C56 Si2 C49 C48 121.5(8) . . . . ? C35 Si2 C49 C50 47.4(12) . . . . ? C35' Si2 C49 C50 62.2(10) . . . . ? C42 Si2 C49 C50 -177.1(7) . . . . ? C56 Si2 C49 C50 -65.0(9) . . . . ? C48 C49 C50 C51 0.00(9) . . . . ? Si2 C49 C50 C51 -173.3(11) . . . . ? C47 C46 C51 C50 0.1(19) . . . . ? C45 C46 C51 C50 172.7(14) . . . . ? C49 C50 C51 C46 0.00(9) . . . . ? Cd3 O16 C52 O15 0(2) 2_665 . . . ? Cd3' O16 C52 O15 2(2) 2_665 . . . ? Cd3 O16 C52 C53 173.2(17) 2_665 . . . ? Cd3' O16 C52 C53 175.6(16) 2_665 . . . ? Cd3' O16 C52 Cd3 2.4(2) 2_665 . . 2_665 ? Cd3 O15 C52 O16 0.4(19) 2_665 . . . ? Cd2 O15 C52 O16 -102(2) 1_655 . . . ? Cd3' O15 C52 O16 -2(2) 2_665 . . . ? Cd3 O15 C52 C53 -173.8(14) 2_665 . . . ? Cd2 O15 C52 C53 83(2) 1_655 . . . ? Cd3' O15 C52 C53 -176.2(13) 2_665 . . . ? Cd2 O15 C52 Cd3 -102.8(15) 1_655 . . 2_665 ? Cd3' O15 C52 Cd3 -2.4(3) 2_665 . . 2_665 ? O16 C52 C53 C58 5(3) . . . . ? O15 C52 C53 C58 179.0(12) . . . . ? Cd3 C52 C53 C58 128(9) 2_665 . . . ? O16 C52 C53 C54 -175.6(16) . . . . ? O15 C52 C53 C54 -2(2) . . . . ? Cd3 C52 C53 C54 -53(10) 2_665 . . . ? C58 C53 C54 C55 0.00(3) . . . . ? C52 C53 C54 C55 -179.3(14) . . . . ? C53 C54 C55 C56 -0.1(17) . . . . ? C54 C55 C56 C57 0.1(17) . . . . ? C54 C55 C56 Si2 -177.1(9) . . . . ? C49 Si2 C56 C57 20.8(9) . . . . ? C35 Si2 C56 C57 -108.3(8) . . . . ? C35' Si2 C56 C57 -98.5(10) . . . . ? C42 Si2 C56 C57 138.6(7) . . . . ? C49 Si2 C56 C55 -162.2(7) . . . . ? C35 Si2 C56 C55 68.7(8) . . . . ? C35' Si2 C56 C55 78.5(9) . . . . ? C42 Si2 C56 C55 -44.4(8) . . . . ? C55 C56 C57 C58 -0.1(17) . . . . ? Si2 C56 C57 C58 177.0(9) . . . . ? C54 C53 C58 C57 0.00(6) . . . . ? C52 C53 C58 C57 179.4(13) . . . . ? C56 C57 C58 C53 0.00(9) . . . . ? C8 O4' Cd4 O54S 82(7) . . . . ? Cd3' O4' Cd4 O54S -115.3(17) . . . . ? C8 O4' Cd4 O42S -85(7) . . . . ? Cd3' O4' Cd4 O42S 76.8(16) . . . . ? C8 O4' Cd4 O41S 124(7) . . . . ? Cd3' O4' Cd4 O41S -73.7(19) . . . . ? C8 O4' Cd4 Cd5 80(7) . . . . ? Cd3' O4' Cd4 Cd5 -117.9(7) . . . . ? O4' Cd4 Cd5 O41S 111(2) . . . . ? O54S Cd4 Cd5 O41S 108(3) . . . . ? O42S Cd4 Cd5 O41S -90(3) . . . . ? O4' Cd4 Cd5 O52S -137.0(15) . . . . ? O54S Cd4 Cd5 O52S -141(3) . . . . ? O42S Cd4 Cd5 O52S 22(3) . . . . ? O41S Cd4 Cd5 O52S 112(3) . . . . ? O4' Cd4 Cd5 O51S 56.5(16) . . . . ? O54S Cd4 Cd5 O51S 53(3) . . . . ? O42S Cd4 Cd5 O51S -144(3) . . . . ? O41S Cd4 Cd5 O51S -55(3) . . . . ? O4' Cd4 Cd5 O54S 4(2) . . . . ? O42S Cd4 Cd5 O54S 163(3) . . . . ? O41S Cd4 Cd5 O54S -108(3) . . . . ? O4' Cd4 Cd5 O53S -26.1(15) . . . . ? O54S Cd4 Cd5 O53S -30(3) . . . . ? O42S Cd4 Cd5 O53S 133(3) . . . . ? O41S Cd4 Cd5 O53S -137(3) . . . . ? O52S Cd5 O41S Cd4 -69(2) . . . . ? O51S Cd5 O41S Cd4 136(2) . . . . ? O54S Cd5 O41S Cd4 44(2) . . . . ? O53S Cd5 O41S Cd4 59(3) . . . . ? O4' Cd4 O41S Cd5 -94(2) . . . . ? O54S Cd4 O41S Cd5 -46.4(18) . . . . ? O42S Cd4 O41S Cd5 123(2) . . . . ? O4' Cd4 O54S Cd5 -177(2) . . . . ? O42S Cd4 O54S Cd5 -89(7) . . . . ? O41S Cd4 O54S Cd5 40.8(18) . . . . ? O41S Cd5 O54S Cd4 -44.4(16) . . . . ? O52S Cd5 O54S Cd4 44(3) . . . . ? O51S Cd5 O54S Cd4 -137(2) . . . . ? O53S Cd5 O54S Cd4 148(3) . . . . ? C38 O12 Cd6 O64S 91.9(14) . . . . ? Cd1 O12 Cd6 O64S -173.8(10) 2_574 . . . ? C38 O12 Cd6 O62S -154.0(12) . . . . ? Cd1 O12 Cd6 O62S -59.7(9) 2_574 . . . ? C38 O12 Cd6 O63S -78.9(14) . . . . ? Cd1 O12 Cd6 O63S 15.4(11) 2_574 . . . ? C38 O12 Cd6 O61S 8.2(12) . . . . ? Cd1 O12 Cd6 O61S 102.5(9) 2_574 . . . ? O64S Cd6 O63S O6 -20(17) . . . 2_664 ? O62S Cd6 O63S O6 166(12) . . . 2_664 ? O61S Cd6 O63S O6 -34(11) . . . 2_664 ? O12 Cd6 O63S O6 57(11) . . . 2_664 ? O64S Cd6 O63S C15 128(7) . . . 2_664 ? O62S Cd6 O63S C15 -45(5) . . . 2_664 ? O61S Cd6 O63S C15 114(5) . . . 2_664 ? O12 Cd6 O63S C15 -155(5) . . . 2_664 ? O64S Cd6 O63S Cd1 -93(8) . . . 2_574 ? O62S Cd6 O63S Cd1 93.1(16) . . . 2_574 ? O61S Cd6 O63S Cd1 -107.1(16) . . . 2_574 ? O12 Cd6 O63S Cd1 -16.3(11) . . . 2_574 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.433 _refine_diff_density_min -3.848 _refine_diff_density_rms 0.252 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 138 69 ' ' 2 -0.034 0.519 0.500 436 217 ' ' 3 0.165 0.783 0.640 37 15 ' ' 4 0.500 1.000 1.000 405 200 ' ' 5 0.291 0.749 0.810 16 7 ' ' 6 0.296 0.787 0.305 20 11 ' ' 7 0.703 0.213 0.695 17 4 ' ' 8 0.709 0.251 0.190 16 5 ' ' 9 0.834 0.217 0.360 38 33 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942378'