# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Barbara Becker' _publ_contact_author_email BBECKER@CHEM.PG.GDA.PL _publ_section_title ; In search of molecular precursors for cadmium sulfide - new complexes with sulfur-rich kernel: cadmium(II) tri-tert-butoxysilanethiolates with additional diethyldithiocarbamato ligand ; _publ_requested_category FM loop_ _publ_author_name 'Barbara Becker' 'Jaroslaw Chojnacki' 'Amir Fahmi' 'Anna Kropidlowska' # Attachment 'structures.cif' data_comp2 _database_code_depnum_ccdc_archive 'CCDC 684878' _audit_creation_date 2006-11-07T15:28:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H74 Cd2 N2 O6 S6 Si2' _chemical_formula_sum 'C34 H74 Cd2 N2 O6 S6 Si2' _chemical_formula_weight 1080.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6730(14) _cell_length_b 10.7200(16) _cell_length_c 12.452(2) _cell_angle_alpha 65.199(15) _cell_angle_beta 73.677(13) _cell_angle_gamma 78.583(12) _cell_volume 1235.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7312 _cell_measurement_theta_min 3.002 _cell_measurement_theta_max 32.4637 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.093 _exptl_crystal_size_min 0.016 _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.80282 _exptl_absorpt_correction_T_max 0.94469 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans, 0.75\%' _diffrn_measurement_device_type 'KM4CCD, Oxford Diffraction' _diffrn_measurement_device '4-axis, \k-geometry diffractometer' _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.0024361077 _diffrn_orient_matrix_ub_12 -0.0727496369 _diffrn_orient_matrix_ub_13 0.0310960978 _diffrn_orient_matrix_ub_21 0.019564785 _diffrn_orient_matrix_ub_22 -0.0078263463 _diffrn_orient_matrix_ub_23 -0.0563514512 _diffrn_orient_matrix_ub_31 0.0666895456 _diffrn_orient_matrix_ub_32 -0.00206144 _diffrn_orient_matrix_ub_33 0.0004596636 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_unetI/netI 0.0516 _diffrn_reflns_number 12186 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 7054 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0457P)^2^+3.0298P] 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_number_reflns 7054 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.117 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.356 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.144 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.61167(2) 0.86095(2) 0.01735(2) 0.01583(7) Uani 1 1 d . . . Si1 Si 0.31209(8) 0.83192(8) 0.23057(7) 0.01139(15) Uani 1 1 d . . . S1 S 0.36191(7) 0.88673(8) 0.03998(6) 0.01337(14) Uani 1 1 d . . . S2 S 0.73533(8) 0.66147(8) -0.03877(7) 0.01792(15) Uani 1 1 d . . . S3 S 0.74357(8) 0.70821(8) 0.17882(7) 0.01719(15) Uani 1 1 d . . . N1 N 0.8348(3) 0.4747(3) 0.1459(2) 0.0149(5) Uani 1 1 d . . . O1 O 0.3847(2) 0.6833(2) 0.3013(2) 0.0142(4) Uani 1 1 d . . . O2 O 0.1557(2) 0.8217(2) 0.2881(2) 0.0149(4) Uani 1 1 d . . . O3 O 0.3700(2) 0.9528(2) 0.2451(2) 0.0154(4) Uani 1 1 d . . . C1 C 0.3603(3) 0.5444(3) 0.3246(3) 0.0142(5) Uani 1 1 d . . . C2 C 0.4858(4) 0.4540(4) 0.3506(4) 0.0249(7) Uani 1 1 d . . . H2A H 0.557 0.4838 0.2783 0.03 Uiso 1 1 calc R . . H2B H 0.473 0.3577 0.3721 0.03 Uiso 1 1 calc R . . H2C H 0.5083 0.4623 0.4182 0.03 Uiso 1 1 calc R . . C3 C 0.3287(4) 0.5397(4) 0.2146(3) 0.0253(7) Uani 1 1 d . . . H3A H 0.2488 0.5999 0.1974 0.03 Uiso 1 1 calc R . . H3B H 0.3154 0.4448 0.2314 0.03 Uiso 1 1 calc R . . H3C H 0.4017 0.5713 0.1443 0.03 Uiso 1 1 calc R . . C4 C 0.2468(4) 0.4987(4) 0.4351(3) 0.0275(8) Uani 1 1 d . . . H4A H 0.2712 0.4966 0.5062 0.033 Uiso 1 1 calc R . . H4B H 0.2274 0.4063 0.4504 0.033 Uiso 1 1 calc R . . H4C H 0.1691 0.5638 0.4198 0.033 Uiso 1 1 calc R . . C5 C 0.0346(3) 0.9082(3) 0.2716(3) 0.0171(6) Uani 1 1 d . . . C6 C 0.0346(4) 1.0385(4) 0.2919(4) 0.0279(8) Uani 1 1 d . . . H6A H 0.0536 1.0134 0.3714 0.034 Uiso 1 1 calc R . . H6B H -0.0516 1.091 0.2892 0.034 Uiso 1 1 calc R . . H6C H 0.1018 1.0951 0.2282 0.034 Uiso 1 1 calc R . . C7 C -0.0723(3) 0.8203(4) 0.3671(4) 0.0285(8) Uani 1 1 d . . . H7A H -0.0695 0.7358 0.3539 0.034 Uiso 1 1 calc R . . H7B H -0.1582 0.8725 0.3607 0.034 Uiso 1 1 calc R . . H7C H -0.0579 0.7963 0.4481 0.034 Uiso 1 1 calc R . . C8 C 0.0148(4) 0.9441(5) 0.1453(3) 0.0294(8) Uani 1 1 d . . . H8A H 0.0801 1.0058 0.0848 0.035 Uiso 1 1 calc R . . H8B H -0.0734 0.9902 0.1393 0.035 Uiso 1 1 calc R . . H8C H 0.025 0.8595 0.1305 0.035 Uiso 1 1 calc R . . C9 C 0.4034(3) 0.9634(3) 0.3459(3) 0.0163(6) Uani 1 1 d . . . C10 C 0.3189(3) 0.8783(4) 0.4669(3) 0.0213(6) Uani 1 1 d . . . H10A H 0.2263 0.9114 0.4677 0.026 Uiso 1 1 calc R . . H10B H 0.3434 0.8879 0.533 0.026 Uiso 1 1 calc R . . H10C H 0.3326 0.781 0.4776 0.026 Uiso 1 1 calc R . . C11 C 0.5479(3) 0.9126(4) 0.3415(3) 0.0241(7) Uani 1 1 d . . . H11A H 0.5615 0.8155 0.3518 0.029 Uiso 1 1 calc R . . H11B H 0.5743 0.9219 0.4069 0.029 Uiso 1 1 calc R . . H11C H 0.6007 0.9679 0.263 0.029 Uiso 1 1 calc R . . C12 C 0.3795(4) 1.1164(4) 0.3229(3) 0.0272(7) Uani 1 1 d . . . H12A H 0.4351 1.1687 0.2449 0.033 Uiso 1 1 calc R . . H12B H 0.4008 1.1312 0.388 0.033 Uiso 1 1 calc R . . H12C H 0.2872 1.1479 0.3209 0.033 Uiso 1 1 calc R . . C13 C 0.7784(3) 0.6019(3) 0.1004(3) 0.0143(5) Uani 1 1 d . . . C14 C 0.8583(3) 0.4151(3) 0.2701(3) 0.0173(6) Uani 1 1 d . . . H14A H 0.8541 0.314 0.3037 0.021 Uiso 1 1 calc R . . H14B H 0.7875 0.4531 0.322 0.021 Uiso 1 1 calc R . . C15 C 0.9901(3) 0.4443(4) 0.2751(3) 0.0238(7) Uani 1 1 d . . . H15A H 1.0609 0.4034 0.2267 0.029 Uiso 1 1 calc R . . H15B H 0.9992 0.404 0.3595 0.029 Uiso 1 1 calc R . . H15C H 0.9949 0.5442 0.2423 0.029 Uiso 1 1 calc R . . C16 C 0.8670(3) 0.3805(4) 0.0820(3) 0.0200(6) Uani 1 1 d . . . H16A H 0.9471 0.3197 0.102 0.024 Uiso 1 1 calc R . . H16B H 0.8853 0.4347 -0.0067 0.024 Uiso 1 1 calc R . . C17 C 0.7546(4) 0.2919(4) 0.1172(4) 0.0300(8) Uani 1 1 d . . . H17A H 0.7368 0.2376 0.2049 0.036 Uiso 1 1 calc R . . H17B H 0.7792 0.2295 0.0739 0.036 Uiso 1 1 calc R . . H17C H 0.6758 0.3517 0.0954 0.036 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(11) 0.01419(12) 0.01716(12) -0.00595(8) -0.00235(8) 0.00006(7) Si1 0.0119(3) 0.0115(4) 0.0114(3) -0.0049(3) -0.0023(3) -0.0017(3) S1 0.0145(3) 0.0151(3) 0.0112(3) -0.0055(3) -0.0019(2) -0.0031(2) S2 0.0216(4) 0.0185(4) 0.0144(3) -0.0085(3) -0.0065(3) 0.0051(3) S3 0.0204(3) 0.0166(4) 0.0182(3) -0.0099(3) -0.0073(3) 0.0018(3) N1 0.0151(11) 0.0191(13) 0.0122(11) -0.0076(10) -0.0048(9) 0.0006(9) O1 0.0172(10) 0.0112(10) 0.0153(10) -0.0052(8) -0.0048(8) -0.0020(8) O2 0.0110(9) 0.0158(10) 0.0153(10) -0.0045(8) -0.0020(8) -0.0006(8) O3 0.0209(10) 0.0139(10) 0.0128(10) -0.0044(8) -0.0037(8) -0.0061(8) C1 0.0166(13) 0.0109(13) 0.0145(13) -0.0047(10) -0.0019(10) -0.0024(10) C2 0.0254(16) 0.0140(15) 0.0362(19) -0.0086(14) -0.0117(14) 0.0009(12) C3 0.0366(19) 0.0180(16) 0.0261(17) -0.0093(13) -0.0110(15) -0.0056(14) C4 0.0300(18) 0.0216(17) 0.0250(17) -0.0088(14) 0.0074(14) -0.0101(14) C5 0.0107(12) 0.0193(15) 0.0176(14) -0.0043(12) -0.0031(10) 0.0001(11) C6 0.0224(16) 0.0235(18) 0.038(2) -0.0132(16) -0.0095(15) 0.0050(13) C7 0.0132(14) 0.031(2) 0.0290(18) -0.0038(15) 0.0025(13) -0.0048(13) C8 0.0186(15) 0.048(2) 0.0215(17) -0.0135(16) -0.0077(13) 0.0033(15) C9 0.0198(14) 0.0178(14) 0.0147(13) -0.0071(11) -0.0072(11) -0.0024(11) C10 0.0239(15) 0.0254(17) 0.0139(14) -0.0067(12) -0.0030(12) -0.0047(13) C11 0.0192(15) 0.037(2) 0.0217(16) -0.0137(15) -0.0071(12) -0.0046(14) C12 0.046(2) 0.0165(16) 0.0244(17) -0.0096(13) -0.0139(16) -0.0025(14) C13 0.0149(13) 0.0158(14) 0.0127(13) -0.0061(11) -0.0024(10) -0.0019(10) C14 0.0192(14) 0.0174(14) 0.0127(13) -0.0042(11) -0.0058(11) 0.0036(11) C15 0.0187(14) 0.0353(19) 0.0185(15) -0.0107(14) -0.0074(12) 0.0008(13) C16 0.0259(16) 0.0182(15) 0.0184(14) -0.0111(12) -0.0078(12) 0.0057(12) C17 0.035(2) 0.0259(19) 0.039(2) -0.0177(17) -0.0161(17) -0.0018(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S2 2.5339(9) . ? Cd1 S1 2.5445(9) 2_675 ? Cd1 S1 2.5716(8) . ? Cd1 S3 2.5733(9) . ? Cd1 Cd1 3.3825(7) 2_675 ? Si1 O1 1.622(2) . ? Si1 O2 1.627(2) . ? Si1 O3 1.634(2) . ? Si1 S1 2.1225(11) . ? S1 Cd1 2.5445(9) 2_675 ? S2 C13 1.739(3) . ? S3 C13 1.719(3) . ? N1 C13 1.327(4) . ? N1 C16 1.468(4) . ? N1 C14 1.479(4) . ? O1 C1 1.456(4) . ? O2 C5 1.445(4) . ? O3 C9 1.450(4) . ? C1 C2 1.518(5) . ? C1 C3 1.521(5) . ? C1 C4 1.528(5) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C8 1.520(5) . ? C5 C6 1.521(5) . ? C5 C7 1.525(5) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C12 1.524(5) . ? C9 C11 1.524(5) . ? C9 C10 1.525(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C14 C15 1.523(5) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.529(5) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? 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 S2 Cd1 S1 138.09(3) . 2_675 ? S2 Cd1 S1 115.56(3) . . ? S1 Cd1 S1 97.22(3) 2_675 . ? S2 Cd1 S3 71.43(3) . . ? S1 Cd1 S3 109.23(3) 2_675 . ? S1 Cd1 S3 127.77(3) . . ? S2 Cd1 Cd1 152.60(2) . 2_675 ? S1 Cd1 Cd1 48.96(2) 2_675 2_675 ? S1 Cd1 Cd1 48.27(2) . 2_675 ? S3 Cd1 Cd1 135.51(2) . 2_675 ? O1 Si1 O2 106.62(12) . . ? O1 Si1 O3 109.21(12) . . ? O2 Si1 O3 113.64(12) . . ? O1 Si1 S1 111.71(9) . . ? O2 Si1 S1 113.04(9) . . ? O3 Si1 S1 102.67(9) . . ? Si1 S1 Cd1 96.25(4) . 2_675 ? Si1 S1 Cd1 96.21(4) . . ? Cd1 S1 Cd1 82.78(3) 2_675 . ? C13 S2 Cd1 84.61(11) . . ? C13 S3 Cd1 83.78(11) . . ? C13 N1 C16 122.8(3) . . ? C13 N1 C14 121.3(3) . . ? C16 N1 C14 115.7(3) . . ? C1 O1 Si1 130.55(19) . . ? C5 O2 Si1 138.3(2) . . ? C9 O3 Si1 133.4(2) . . ? O1 C1 C2 106.0(2) . . ? O1 C1 C3 110.9(2) . . ? C2 C1 C3 110.0(3) . . ? O1 C1 C4 108.5(3) . . ? C2 C1 C4 110.6(3) . . ? C3 C1 C4 110.7(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C8 110.1(3) . . ? O2 C5 C6 110.6(3) . . ? C8 C5 C6 110.6(3) . . ? O2 C5 C7 104.9(3) . . ? C8 C5 C7 110.0(3) . . ? C6 C5 C7 110.6(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C12 105.2(3) . . ? O3 C9 C11 107.5(3) . . ? C12 C9 C11 111.0(3) . . ? O3 C9 C10 111.4(3) . . ? C12 C9 C10 111.0(3) . . ? C11 C9 C10 110.5(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 S3 120.9(2) . . ? N1 C13 S2 120.0(2) . . ? S3 C13 S2 119.15(18) . . ? N1 C14 C15 113.2(3) . . ? N1 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? N1 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 111.3(3) . . ? N1 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N1 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? #===END data_comp3 _database_code_depnum_ccdc_archive 'CCDC 684879' _audit_creation_date 2006-11-07T16:01:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H64 Cd N O6 S4 Si2 1-, C16 H36 N 1+' _chemical_formula_sum 'C45 H100 Cd N2 O6 S4 Si2' _chemical_formula_weight 1062.09 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 23.8773(9) _cell_length_b 21.9626(9) _cell_length_c 25.4375(10) _cell_angle_alpha 90 _cell_angle_beta 115.641(13) _cell_angle_gamma 90 _cell_volume 12026.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device '4-axis, \k-geometry diffractometer' _diffrn_measurement_device_type 'KM4CCD, Oxford Diffraction' _diffrn_measurement_method '\w scans, 0.75\%' _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_unetI/netI 0.0502 _diffrn_reflns_number 102895 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 29 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 31918 _reflns_number_gt 26111 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0571P)^2^+23.4604P] 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_number_reflns 31918 _refine_ls_number_parameters 1160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.81 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.111 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 0.057703(11) 0.624196(10) 0.757561(10) 0.01961(6) Uani 1 1 d . . . S1 S 0.11141(4) 0.69448(3) 0.71781(3) 0.01921(15) Uani 1 1 d . . . S2 S 0.09518(4) 0.51794(3) 0.79120(3) 0.02247(16) Uani 1 1 d . . . S3 S 0.01857(4) 0.68213(4) 0.82623(4) 0.02344(16) Uani 1 1 d . . . S4 S -0.06531(4) 0.62181(4) 0.71508(3) 0.02024(15) Uani 1 1 d . . . Si1 Si 0.07022(4) 0.66955(4) 0.63015(4) 0.01591(16) Uani 1 1 d . . . Si2 Si 0.17037(4) 0.54538(4) 0.86749(4) 0.02107(18) Uani 1 1 d . . . N1 N -0.10373(12) 0.67506(13) 0.78854(12) 0.0214(5) Uani 1 1 d . . . O1 O 0.03804(10) 0.72649(10) 0.58597(10) 0.0205(4) Uani 1 1 d . . . O2 O 0.11873(10) 0.64114(10) 0.60664(10) 0.0201(4) Uani 1 1 d . . . O3 O 0.01442(10) 0.62140(9) 0.62036(9) 0.0181(4) Uani 1 1 d . . . O4 O 0.16984(10) 0.61999(10) 0.86622(10) 0.0234(5) Uani 1 1 d . . . O5 O 0.23842(12) 0.52551(11) 0.87216(14) 0.0370(6) Uani 1 1 d . . . O6 O 0.17144(13) 0.51842(12) 0.92776(11) 0.0325(6) Uani 1 1 d . A . C1 C 0.06193(16) 0.77380(14) 0.56203(14) 0.0240(7) Uani 1 1 d . . . C2 C 0.0576(2) 0.75200(17) 0.50316(17) 0.0344(8) Uani 1 1 d . . . H2A H 0.0831 0.7154 0.509 0.041 Uiso 1 1 calc R . . H2B H 0.0726 0.7841 0.4858 0.041 Uiso 1 1 calc R . . H2C H 0.0142 0.7425 0.4771 0.041 Uiso 1 1 calc R . . C3 C 0.12904(17) 0.79021(17) 0.60349(17) 0.0333(8) Uani 1 1 d . . . H3A H 0.1312 0.8019 0.6415 0.04 Uiso 1 1 calc R . . H3B H 0.1429 0.8243 0.5872 0.04 Uiso 1 1 calc R . . H3C H 0.1559 0.7549 0.6082 0.04 Uiso 1 1 calc R . . C4 C 0.01976(19) 0.82861(16) 0.55425(17) 0.0322(8) Uani 1 1 d . . . H4A H -0.0236 0.8168 0.5306 0.039 Uiso 1 1 calc R . . H4B H 0.0311 0.8614 0.5346 0.039 Uiso 1 1 calc R . . H4C H 0.0246 0.8428 0.5925 0.039 Uiso 1 1 calc R . . C5 C 0.16397(15) 0.59275(14) 0.62793(14) 0.0207(6) Uani 1 1 d . . . C6 C 0.17348(16) 0.57305(16) 0.57463(16) 0.0266(7) Uani 1 1 d . . . H6A H 0.1344 0.5571 0.5447 0.032 Uiso 1 1 calc R . . H6B H 0.2054 0.5413 0.586 0.032 Uiso 1 1 calc R . . H6C H 0.1868 0.6081 0.5591 0.032 Uiso 1 1 calc R . . C7 C 0.22390(16) 0.61843(17) 0.67560(16) 0.0283(7) Uani 1 1 d . . . H7A H 0.2379 0.6531 0.6601 0.034 Uiso 1 1 calc R . . H7B H 0.256 0.5868 0.6886 0.034 Uiso 1 1 calc R . . H7C H 0.2162 0.6319 0.7086 0.034 Uiso 1 1 calc R . . C8 C 0.14042(18) 0.53969(15) 0.65156(16) 0.0287(7) Uani 1 1 d . . . H8A H 0.134 0.5534 0.6852 0.034 Uiso 1 1 calc R . . H8B H 0.1711 0.5067 0.6636 0.034 Uiso 1 1 calc R . . H8C H 0.101 0.5249 0.6211 0.034 Uiso 1 1 calc R . . C9 C -0.03825(15) 0.60253(14) 0.56727(13) 0.0210(6) Uani 1 1 d . . . C10 C -0.05971(17) 0.54244(16) 0.58237(16) 0.0283(7) Uani 1 1 d . . . H10A H -0.0268 0.5119 0.5919 0.034 Uiso 1 1 calc R . . H10B H -0.0972 0.5284 0.5489 0.034 Uiso 1 1 calc R . . H10C H -0.0689 0.5483 0.616 0.034 Uiso 1 1 calc R . . C11 C -0.02027(18) 0.59299(16) 0.51712(14) 0.0281(7) Uani 1 1 d . . . H11A H -0.0058 0.6316 0.5081 0.034 Uiso 1 1 calc R . . H11B H -0.0565 0.5786 0.4827 0.034 Uiso 1 1 calc R . . H11C H 0.013 0.5627 0.5285 0.034 Uiso 1 1 calc R . . C12 C -0.08919(16) 0.65001(16) 0.55209(16) 0.0292(7) Uani 1 1 d . . . H12A H -0.1019 0.6528 0.5838 0.035 Uiso 1 1 calc R . . H12B H -0.1249 0.6382 0.516 0.035 Uiso 1 1 calc R . . H12C H -0.0736 0.6896 0.5466 0.035 Uiso 1 1 calc R . . C13 C 0.21717(15) 0.66426(15) 0.89734(15) 0.0248(7) Uani 1 1 d . . . C14 C 0.26212(19) 0.66860(19) 0.8698(2) 0.0414(10) Uani 1 1 d . . . H14A H 0.2844 0.63 0.875 0.05 Uiso 1 1 calc R . . H14B H 0.2919 0.7015 0.8884 0.05 Uiso 1 1 calc R . . H14C H 0.239 0.6772 0.828 0.05 Uiso 1 1 calc R . . C15 C 0.2507(2) 0.64776(18) 0.96199(18) 0.0401(10) Uani 1 1 d . . . H15A H 0.2205 0.645 0.9784 0.048 Uiso 1 1 calc R . . H15B H 0.2815 0.6792 0.9827 0.048 Uiso 1 1 calc R . . H15C H 0.2717 0.6085 0.9663 0.048 Uiso 1 1 calc R . . C16 C 0.18230(18) 0.72449(16) 0.89008(19) 0.0359(9) Uani 1 1 d . . . H16A H 0.1588 0.7336 0.8485 0.043 Uiso 1 1 calc R . . H16B H 0.2121 0.7573 0.9089 0.043 Uiso 1 1 calc R . . H16C H 0.1536 0.7212 0.9082 0.043 Uiso 1 1 calc R . . C17 C 0.26853(17) 0.46851(16) 0.87531(18) 0.0310(8) Uani 1 1 d . . . C18 C 0.3298(2) 0.4722(2) 0.9278(2) 0.0575(14) Uani 1 1 d . . . H18A H 0.3524 0.5083 0.9249 0.069 Uiso 1 1 calc R . . H18B H 0.3542 0.4356 0.9299 0.069 Uiso 1 1 calc R . . H18C H 0.323 0.475 0.963 0.069 Uiso 1 1 calc R . . C19 C 0.2304(2) 0.41454(19) 0.8784(3) 0.0541(13) Uani 1 1 d . . . H19A H 0.2216 0.4188 0.9124 0.065 Uiso 1 1 calc R . . H19B H 0.2538 0.3769 0.8818 0.065 Uiso 1 1 calc R . . H19C H 0.1913 0.413 0.8428 0.065 Uiso 1 1 calc R . . C20 C 0.2776(4) 0.4639(3) 0.8199(3) 0.0723(18) Uani 1 1 d . . . H20A H 0.2375 0.469 0.7859 0.087 Uiso 1 1 calc R . . H20B H 0.295 0.4239 0.8182 0.087 Uiso 1 1 calc R . . H20C H 0.3063 0.4959 0.8198 0.087 Uiso 1 1 calc R . . C21 C 0.12766(18) 0.51317(17) 0.95285(15) 0.0306(8) Uani 1 1 d . . . C22 C 0.0867(3) 0.5672(3) 0.9371(3) 0.0436(17) Uani 0.685(7) 1 d P A 1 H22A H 0.1121 0.6041 0.9501 0.052 Uiso 0.685(7) 1 calc PR A 1 H22B H 0.0587 0.5647 0.956 0.052 Uiso 0.685(7) 1 calc PR A 1 H22C H 0.0622 0.5686 0.8946 0.052 Uiso 0.685(7) 1 calc PR A 1 C23 C 0.1698(4) 0.5077(4) 1.0177(3) 0.058(2) Uani 0.685(7) 1 d P A 1 H23A H 0.1984 0.4733 1.0243 0.069 Uiso 0.685(7) 1 calc PR A 1 H23B H 0.1446 0.5008 1.0389 0.069 Uiso 0.685(7) 1 calc PR A 1 H23C H 0.1938 0.5453 1.0316 0.069 Uiso 0.685(7) 1 calc PR A 1 C24 C 0.0937(4) 0.4540(3) 0.9287(3) 0.0467(18) Uani 0.685(7) 1 d P A 1 H24A H 0.0725 0.4563 0.8861 0.056 Uiso 0.685(7) 1 calc PR A 1 H24B H 0.063 0.4471 0.9441 0.056 Uiso 0.685(7) 1 calc PR A 1 H24C H 0.1235 0.4203 0.9404 0.056 Uiso 0.685(7) 1 calc PR A 1 C22A C 0.1254(9) 0.5738(6) 0.9851(8) 0.055(5) Uani 0.315(7) 1 d P A 2 H22D H 0.1657 0.5805 1.0185 0.066 Uiso 0.315(7) 1 calc PR A 2 H22E H 0.0929 0.5705 0.9989 0.066 Uiso 0.315(7) 1 calc PR A 2 H22F H 0.116 0.6082 0.9581 0.066 Uiso 0.315(7) 1 calc PR A 2 C23A C 0.1443(7) 0.4611(7) 0.9971(6) 0.045(4) Uani 0.315(7) 1 d P A 2 H23D H 0.1412 0.4222 0.9772 0.054 Uiso 0.315(7) 1 calc PR A 2 H23E H 0.1155 0.4612 1.0152 0.054 Uiso 0.315(7) 1 calc PR A 2 H23F H 0.1868 0.4666 1.0272 0.054 Uiso 0.315(7) 1 calc PR A 2 C24A C 0.0571(7) 0.5028(7) 0.9065(6) 0.045(4) Uani 0.315(7) 1 d P A 2 H24D H 0.0429 0.538 0.8803 0.054 Uiso 0.315(7) 1 calc PR A 2 H24E H 0.0309 0.4981 0.9271 0.054 Uiso 0.315(7) 1 calc PR A 2 H24F H 0.0544 0.466 0.8837 0.054 Uiso 0.315(7) 1 calc PR A 2 C25 C -0.05518(14) 0.66062(14) 0.77753(14) 0.0204(6) Uani 1 1 d . . . C26 C -0.09610(16) 0.70314(17) 0.84376(16) 0.0291(8) Uani 1 1 d . . . H26A H -0.1337 0.7271 0.8371 0.035 Uiso 1 1 calc R . . H26B H -0.0603 0.7314 0.8575 0.035 Uiso 1 1 calc R . . C27 C -0.08570(18) 0.6557(2) 0.89027(17) 0.0368(9) Uani 1 1 d . . . H27A H -0.1201 0.6265 0.876 0.044 Uiso 1 1 calc R . . H27B H -0.0837 0.6757 0.9255 0.044 Uiso 1 1 calc R . . H27C H -0.0465 0.6343 0.8994 0.044 Uiso 1 1 calc R . . C28 C -0.16836(15) 0.65975(17) 0.74845(17) 0.0292(7) Uani 1 1 d . . . H28A H -0.1906 0.646 0.7713 0.035 Uiso 1 1 calc R . . H28B H -0.1684 0.6258 0.7228 0.035 Uiso 1 1 calc R . . C29 C -0.20223(18) 0.7137(2) 0.71122(19) 0.0411(10) Uani 1 1 d . . . H29A H -0.2025 0.7474 0.7364 0.049 Uiso 1 1 calc R . . H29B H -0.2451 0.7021 0.6855 0.049 Uiso 1 1 calc R . . H29C H -0.181 0.7267 0.6876 0.049 Uiso 1 1 calc R . . Cd2 Cd 0.486085(10) 0.362906(10) 0.704891(9) 0.01803(6) Uani 1 1 d . . . Si3 Si 0.60114(4) 0.42132(4) 0.66535(4) 0.01695(16) Uani 1 1 d . . . Si4 Si 0.34358(4) 0.30109(4) 0.60911(4) 0.01570(16) Uani 1 1 d . . . S5 S 0.51274(4) 0.44719(3) 0.65404(3) 0.01820(14) Uani 1 1 d . . . S6 S 0.43600(4) 0.27439(3) 0.63930(3) 0.01824(14) Uani 1 1 d . . . S7 S 0.45109(3) 0.40437(4) 0.78378(3) 0.01916(15) Uani 1 1 d . . . S8 S 0.56465(4) 0.33088(3) 0.81254(3) 0.01922(15) Uani 1 1 d . . . N2 N 0.53013(12) 0.37406(12) 0.89201(11) 0.0195(5) Uani 1 1 d . . . O7 O 0.65454(10) 0.47272(10) 0.69962(9) 0.0195(4) Uani 1 1 d . . . O8 O 0.62232(10) 0.36065(10) 0.70667(10) 0.0209(4) Uani 1 1 d . . . O9 O 0.60735(11) 0.41065(10) 0.60407(10) 0.0211(4) Uani 1 1 d . . . O10 O 0.34392(10) 0.36472(9) 0.64303(10) 0.0212(5) Uani 1 1 d . . . O11 O 0.30670(10) 0.30838(10) 0.53819(9) 0.0202(4) Uani 1 1 d . . . O12 O 0.30068(10) 0.25298(10) 0.62451(10) 0.0211(4) Uani 1 1 d . . . C30 C 0.67154(15) 0.52763(14) 0.67966(14) 0.0191(6) Uani 1 1 d . . . C31 C 0.72639(17) 0.51327(16) 0.66630(17) 0.0284(7) Uani 1 1 d . . . H31A H 0.7608 0.4975 0.7015 0.034 Uiso 1 1 calc R . . H31B H 0.7396 0.5505 0.6536 0.034 Uiso 1 1 calc R . . H31C H 0.714 0.4827 0.6353 0.034 Uiso 1 1 calc R . . C32 C 0.61764(16) 0.55355(14) 0.62571(14) 0.0232(6) Uani 1 1 d . . . H32A H 0.6075 0.5256 0.5928 0.028 Uiso 1 1 calc R . . H32B H 0.6296 0.5932 0.616 0.028 Uiso 1 1 calc R . . H32C H 0.5812 0.5585 0.6337 0.028 Uiso 1 1 calc R . . C33 C 0.69001(16) 0.57197(15) 0.73042(15) 0.0252(7) Uani 1 1 d . . . H33A H 0.6544 0.5791 0.7392 0.03 Uiso 1 1 calc R . . H33B H 0.7031 0.6106 0.72 0.03 Uiso 1 1 calc R . . H33C H 0.7244 0.5547 0.7648 0.03 Uiso 1 1 calc R . . C34 C 0.68327(16) 0.33459(15) 0.73987(17) 0.0271(7) Uani 1 1 d . . . C35 C 0.72344(18) 0.33823(17) 0.7063(2) 0.0359(9) Uani 1 1 d . . . H35A H 0.7008 0.3202 0.6675 0.043 Uiso 1 1 calc R . . H35B H 0.7623 0.3158 0.7277 0.043 Uiso 1 1 calc R . . H35C H 0.7329 0.3809 0.7023 0.043 Uiso 1 1 calc R . . C36 C 0.71356(18) 0.36705(19) 0.79813(17) 0.0349(8) Uani 1 1 d . . . H36A H 0.719 0.4102 0.7917 0.042 Uiso 1 1 calc R . . H36B H 0.7542 0.3487 0.8218 0.042 Uiso 1 1 calc R . . H36C H 0.6871 0.3633 0.8185 0.042 Uiso 1 1 calc R . . C37 C 0.6707(2) 0.26807(17) 0.7483(2) 0.0437(11) Uani 1 1 d . . . H37A H 0.6464 0.2658 0.7709 0.052 Uiso 1 1 calc R . . H37B H 0.7103 0.2467 0.7692 0.052 Uiso 1 1 calc R . . H37C H 0.6474 0.2489 0.7101 0.052 Uiso 1 1 calc R . . C38 C 0.57041(17) 0.37572(15) 0.55264(15) 0.0244(7) Uani 1 1 d . . . C39 C 0.6133(2) 0.36376(17) 0.52333(18) 0.0351(9) Uani 1 1 d . . . H39A H 0.6288 0.4026 0.5158 0.042 Uiso 1 1 calc R . . H39B H 0.5902 0.3424 0.4864 0.042 Uiso 1 1 calc R . . H39C H 0.6485 0.3387 0.549 0.042 Uiso 1 1 calc R . . C40 C 0.51564(19) 0.41360(19) 0.51228(17) 0.0366(9) Uani 1 1 d . . . H40A H 0.4906 0.4254 0.5326 0.044 Uiso 1 1 calc R . . H40B H 0.4901 0.3897 0.4776 0.044 Uiso 1 1 calc R . . H40C H 0.5308 0.4502 0.5005 0.044 Uiso 1 1 calc R . . C41 C 0.54900(19) 0.31594(16) 0.56878(17) 0.0313(8) Uani 1 1 d . . . H41A H 0.5852 0.2935 0.5966 0.038 Uiso 1 1 calc R . . H41B H 0.5274 0.2913 0.5336 0.038 Uiso 1 1 calc R . . H41C H 0.5207 0.3247 0.5865 0.038 Uiso 1 1 calc R . . C42 C 0.29436(16) 0.39631(17) 0.64965(16) 0.0306(8) Uani 1 1 d . . . C43 C 0.23405(18) 0.39530(19) 0.59256(18) 0.0413(10) Uani 1 1 d . . . H43A H 0.242 0.4127 0.561 0.05 Uiso 1 1 calc R . . H43B H 0.2021 0.4194 0.5975 0.05 Uiso 1 1 calc R . . H43C H 0.2197 0.3532 0.5829 0.05 Uiso 1 1 calc R . . C44 C 0.28432(18) 0.3668(2) 0.69898(18) 0.0426(10) Uani 1 1 d . . . H44A H 0.2697 0.3249 0.6882 0.051 Uiso 1 1 calc R . . H44B H 0.2532 0.39 0.7061 0.051 Uiso 1 1 calc R . . H44C H 0.3236 0.3664 0.7344 0.051 Uiso 1 1 calc R . . C45 C 0.31666(19) 0.46209(18) 0.6640(2) 0.0465(12) Uani 1 1 d . . . H45A H 0.3555 0.463 0.6999 0.056 Uiso 1 1 calc R . . H45B H 0.285 0.4861 0.6695 0.056 Uiso 1 1 calc R . . H45C H 0.3237 0.4793 0.6319 0.056 Uiso 1 1 calc R . . C46 C 0.32162(17) 0.33913(16) 0.49574(14) 0.0264(7) Uani 1 1 d . . . C47 C 0.25931(19) 0.3517(2) 0.44399(17) 0.0399(10) Uani 1 1 d . . . H47A H 0.2359 0.3136 0.4313 0.048 Uiso 1 1 calc R . . H47B H 0.2664 0.3688 0.4118 0.048 Uiso 1 1 calc R . . H47C H 0.2356 0.3808 0.4556 0.048 Uiso 1 1 calc R . . C48 C 0.3607(2) 0.2966(2) 0.47823(18) 0.0409(10) Uani 1 1 d . . . H48A H 0.3997 0.2878 0.5123 0.049 Uiso 1 1 calc R . . H48B H 0.3696 0.316 0.448 0.049 Uiso 1 1 calc R . . H48C H 0.3379 0.2586 0.463 0.049 Uiso 1 1 calc R . . C49 C 0.35569(18) 0.39834(17) 0.52026(16) 0.0319(8) Uani 1 1 d . . . H49A H 0.3297 0.4248 0.5316 0.038 Uiso 1 1 calc R . . H49B H 0.3647 0.4188 0.4905 0.038 Uiso 1 1 calc R . . H49C H 0.3947 0.3897 0.5545 0.038 Uiso 1 1 calc R . . C50 C 0.26475(15) 0.20085(15) 0.59331(14) 0.0233(6) Uani 1 1 d . . . C51 C 0.26011(17) 0.16065(18) 0.64002(17) 0.0326(8) Uani 1 1 d . . . H51A H 0.3018 0.1476 0.6676 0.039 Uiso 1 1 calc R . . H51B H 0.2347 0.1248 0.6217 0.039 Uiso 1 1 calc R . . H51C H 0.2408 0.1837 0.6609 0.039 Uiso 1 1 calc R . . C52 C 0.2966(2) 0.16670(16) 0.56130(17) 0.0328(8) Uani 1 1 d . . . H52A H 0.2977 0.1927 0.5305 0.039 Uiso 1 1 calc R . . H52B H 0.2733 0.1295 0.544 0.039 Uiso 1 1 calc R . . H52C H 0.339 0.1561 0.5889 0.039 Uiso 1 1 calc R . . C53 C 0.20055(17) 0.22213(18) 0.55044(17) 0.0340(8) Uani 1 1 d . . . H53A H 0.1817 0.246 0.5712 0.041 Uiso 1 1 calc R . . H53B H 0.1744 0.1867 0.5322 0.041 Uiso 1 1 calc R . . H53C H 0.2041 0.2474 0.5203 0.041 Uiso 1 1 calc R . . C54 C 0.51680(14) 0.37000(12) 0.83499(13) 0.0156(5) Uani 1 1 d . . . C55 C 0.58756(16) 0.34923(15) 0.93819(14) 0.0241(7) Uani 1 1 d . . . H55A H 0.6011 0.3757 0.973 0.029 Uiso 1 1 calc R . . H55B H 0.6207 0.3495 0.9246 0.029 Uiso 1 1 calc R . . C56 C 0.57908(19) 0.28469(17) 0.95498(17) 0.0344(8) Uani 1 1 d . . . H56A H 0.5461 0.2841 0.9681 0.041 Uiso 1 1 calc R . . H56B H 0.618 0.2705 0.9865 0.041 Uiso 1 1 calc R . . H56C H 0.5677 0.2579 0.9211 0.041 Uiso 1 1 calc R . . C57 C 0.48840(18) 0.40381(18) 0.91325(15) 0.0301(8) Uani 1 1 d . . . H57A H 0.4897 0.3812 0.9474 0.036 Uiso 1 1 calc R . . H57B H 0.4452 0.4024 0.8823 0.036 Uiso 1 1 calc R . . C58 C 0.5068(2) 0.46914(19) 0.93024(18) 0.0436(10) Uani 1 1 d . . . H58A H 0.5483 0.4704 0.963 0.052 Uiso 1 1 calc R . . H58B H 0.4768 0.4883 0.9418 0.052 Uiso 1 1 calc R . . H58C H 0.5074 0.4912 0.897 0.052 Uiso 1 1 calc R . . N3 N -0.05777(12) 0.39132(11) 0.71466(11) 0.0179(5) Uani 1 1 d . . . C59 C -0.03390(16) 0.33422(14) 0.75252(14) 0.0218(6) Uani 1 1 d . . . H59A H -0.0658 0.3208 0.7651 0.026 Uiso 1 1 calc R . . H59B H -0.0288 0.3013 0.7283 0.026 Uiso 1 1 calc R . . C60 C 0.02697(17) 0.34237(15) 0.80609(15) 0.0266(7) Uani 1 1 d . . . H60A H 0.0196 0.3657 0.8358 0.032 Uiso 1 1 calc R . . H60B H 0.0558 0.3662 0.7956 0.032 Uiso 1 1 calc R . . C61 C 0.05672(17) 0.28184(16) 0.83181(17) 0.0311(8) Uani 1 1 d . . . H61A H 0.0279 0.2583 0.8427 0.037 Uiso 1 1 calc R . . H61B H 0.0634 0.2583 0.8018 0.037 Uiso 1 1 calc R . . C62 C 0.11788(18) 0.28900(18) 0.88477(18) 0.0361(9) Uani 1 1 d . . . H62A H 0.1455 0.3149 0.8751 0.043 Uiso 1 1 calc R . . H62B H 0.1371 0.2489 0.8973 0.043 Uiso 1 1 calc R . . H62C H 0.1108 0.3078 0.9163 0.043 Uiso 1 1 calc R . . C63 C -0.01324(15) 0.40995(14) 0.68939(14) 0.0206(6) Uani 1 1 d . . . H63A H 0.0283 0.4164 0.722 0.025 Uiso 1 1 calc R . . H63B H -0.0272 0.4495 0.6692 0.025 Uiso 1 1 calc R . . C64 C -0.00659(16) 0.36496(16) 0.64671(15) 0.0259(7) Uani 1 1 d . . . H64A H -0.0042 0.323 0.6618 0.031 Uiso 1 1 calc R . . H64B H -0.0437 0.3676 0.6087 0.031 Uiso 1 1 calc R . . C65 C 0.05148(18) 0.37839(17) 0.63800(17) 0.0309(8) Uani 1 1 d . . . H65A H 0.0524 0.3507 0.6077 0.037 Uiso 1 1 calc R . . H65B H 0.0489 0.4206 0.6234 0.037 Uiso 1 1 calc R . . C66 C 0.1114(2) 0.3713(2) 0.6927(2) 0.0520(13) Uani 1 1 d . . . H66A H 0.1149 0.4042 0.72 0.062 Uiso 1 1 calc R . . H66B H 0.1466 0.3731 0.6827 0.062 Uiso 1 1 calc R . . H66C H 0.1114 0.3319 0.7109 0.062 Uiso 1 1 calc R . . C67 C -0.12118(15) 0.37591(14) 0.66646(14) 0.0206(6) Uani 1 1 d . . . H67A H -0.1487 0.3631 0.6844 0.025 Uiso 1 1 calc R . . H67B H -0.1167 0.3408 0.6441 0.025 Uiso 1 1 calc R . . C68 C -0.15228(15) 0.42784(14) 0.62426(15) 0.0233(6) Uani 1 1 d . . . H68A H -0.1237 0.4432 0.6084 0.028 Uiso 1 1 calc R . . H68B H -0.1609 0.4617 0.6455 0.028 Uiso 1 1 calc R . . C69 C -0.21275(16) 0.40748(16) 0.57421(15) 0.0276(7) Uani 1 1 d . . . H69A H -0.2414 0.3922 0.59 0.033 Uiso 1 1 calc R . . H69B H -0.2042 0.3737 0.5529 0.033 Uiso 1 1 calc R . . C70 C -0.24365(16) 0.45995(16) 0.53206(15) 0.0275(7) Uani 1 1 d . . . H70A H -0.2525 0.4932 0.553 0.033 Uiso 1 1 calc R . . H70B H -0.2826 0.4457 0.5005 0.033 Uiso 1 1 calc R . . H70C H -0.2157 0.4745 0.5157 0.033 Uiso 1 1 calc R . . C71 C -0.06128(15) 0.44481(14) 0.75124(14) 0.0200(6) Uani 1 1 d . . . H71A H -0.0187 0.4543 0.7807 0.024 Uiso 1 1 calc R . . H71B H -0.0768 0.4808 0.7255 0.024 Uiso 1 1 calc R . . C72 C -0.10233(16) 0.43515(15) 0.78257(15) 0.0245(7) Uani 1 1 d . . . H72A H -0.145 0.4248 0.7538 0.029 Uiso 1 1 calc R . . H72B H -0.0861 0.4007 0.8102 0.029 Uiso 1 1 calc R . . C73 C -0.1040(2) 0.49222(18) 0.81548(19) 0.0375(9) Uani 1 1 d . . . H73A H -0.1218 0.5261 0.7875 0.045 Uiso 1 1 calc R . . H73B H -0.061 0.5036 0.8428 0.045 Uiso 1 1 calc R . . C74 C -0.1423(3) 0.4831(2) 0.8495(2) 0.0486(12) Uani 1 1 d . . . H74A H -0.1857 0.4754 0.8224 0.058 Uiso 1 1 calc R . . H74B H -0.1399 0.5199 0.8723 0.058 Uiso 1 1 calc R . . H74C H -0.126 0.4483 0.8759 0.058 Uiso 1 1 calc R . . N4 N 0.51953(13) 0.12253(11) 0.75868(12) 0.0197(5) Uani 1 1 d . . . C75 C 0.54110(16) 0.13852(15) 0.71209(14) 0.0226(6) Uani 1 1 d . . . H75A H 0.504 0.148 0.6755 0.027 Uiso 1 1 calc R . . H75B H 0.5665 0.176 0.7244 0.027 Uiso 1 1 calc R . . C76 C 0.57866(18) 0.08986(17) 0.69906(17) 0.0305(8) Uani 1 1 d . . . H76A H 0.5523 0.0535 0.6824 0.037 Uiso 1 1 calc R . . H76B H 0.6143 0.0775 0.7357 0.037 Uiso 1 1 calc R . . C77 C 0.6026(2) 0.1139(2) 0.6558(2) 0.0476(12) Uani 1 1 d . . . H77A H 0.6324 0.1474 0.6746 0.057 Uiso 1 1 calc R . . H77B H 0.6256 0.0808 0.6471 0.057 Uiso 1 1 calc R . . C78 C 0.5522(3) 0.1371(2) 0.5987(2) 0.0599(15) Uani 1 1 d . . . H78A H 0.5212 0.1051 0.5807 0.072 Uiso 1 1 calc R . . H78B H 0.5707 0.1483 0.5723 0.072 Uiso 1 1 calc R . . H78C H 0.5323 0.1729 0.6062 0.072 Uiso 1 1 calc R . . C79 C 0.48185(16) 0.06361(14) 0.74329(15) 0.0239(7) Uani 1 1 d . . . H79A H 0.5097 0.0298 0.7442 0.029 Uiso 1 1 calc R . . H79B H 0.4679 0.0554 0.774 0.029 Uiso 1 1 calc R . . C80 C 0.42539(16) 0.06262(15) 0.68463(17) 0.0282(7) Uani 1 1 d . . . H80A H 0.4384 0.0701 0.6532 0.034 Uiso 1 1 calc R . . H80B H 0.3963 0.0954 0.6832 0.034 Uiso 1 1 calc R . . C81 C 0.39268(17) 0.00093(15) 0.67509(17) 0.0293(7) Uani 1 1 d . . . H81A H 0.4231 -0.0316 0.6793 0.035 Uiso 1 1 calc R . . H81B H 0.3785 -0.0052 0.7059 0.035 Uiso 1 1 calc R . . C82 C 0.3382(2) -0.0055(2) 0.6170(2) 0.0481(11) Uani 1 1 d . . . H82A H 0.3056 0.0231 0.6143 0.058 Uiso 1 1 calc R . . H82B H 0.3223 -0.0472 0.6124 0.058 Uiso 1 1 calc R . . H82C H 0.3512 0.0034 0.5861 0.058 Uiso 1 1 calc R . . C83 C 0.57402(16) 0.11135(15) 0.81722(14) 0.0241(7) Uani 1 1 d . . . H83A H 0.5964 0.0746 0.8141 0.029 Uiso 1 1 calc R . . H83B H 0.5578 0.1026 0.8462 0.029 Uiso 1 1 calc R . . C84 C 0.62004(16) 0.16344(15) 0.83989(15) 0.0239(7) Uani 1 1 d . . . H84A H 0.5973 0.2016 0.8383 0.029 Uiso 1 1 calc R . . H84B H 0.6414 0.1685 0.8144 0.029 Uiso 1 1 calc R . . C85 C 0.66821(17) 0.15252(17) 0.90219(15) 0.0292(7) Uani 1 1 d . . . H85A H 0.6929 0.116 0.9032 0.035 Uiso 1 1 calc R . . H85B H 0.6468 0.1446 0.9272 0.035 Uiso 1 1 calc R . . C86 C 0.71173(19) 0.2068(2) 0.92645(18) 0.0390(9) Uani 1 1 d . . . H86A H 0.7349 0.2133 0.9032 0.047 Uiso 1 1 calc R . . H86B H 0.7409 0.1987 0.967 0.047 Uiso 1 1 calc R . . H86C H 0.6874 0.2433 0.9247 0.047 Uiso 1 1 calc R . . C87 C 0.48059(16) 0.17622(14) 0.76110(15) 0.0224(6) Uani 1 1 d . . . H87A H 0.5051 0.2137 0.7652 0.027 Uiso 1 1 calc R . . H87B H 0.4436 0.1787 0.723 0.027 Uiso 1 1 calc R . . C88 C 0.45834(16) 0.17671(15) 0.80833(15) 0.0246(7) Uani 1 1 d . . . H88A H 0.494 0.1814 0.847 0.03 Uiso 1 1 calc R . . H88B H 0.4371 0.1379 0.808 0.03 Uiso 1 1 calc R . . C89 C 0.41312(18) 0.23040(16) 0.79647(18) 0.0313(8) Uani 1 1 d . . . H89A H 0.4332 0.268 0.7915 0.038 Uiso 1 1 calc R . . H89B H 0.3758 0.2229 0.7595 0.038 Uiso 1 1 calc R . . C90 C 0.3933(2) 0.24004(19) 0.8451(2) 0.0407(10) Uani 1 1 d . . . H90A H 0.373 0.2031 0.85 0.049 Uiso 1 1 calc R . . H90B H 0.3642 0.2743 0.8352 0.049 Uiso 1 1 calc R . . H90C H 0.4299 0.2489 0.8816 0.049 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 0.02006(11) 0.02114(11) 0.02032(11) -0.00117(8) 0.01125(9) -0.00077(8) S1 0.0201(4) 0.0213(4) 0.0168(3) -0.0033(3) 0.0085(3) -0.0030(3) S2 0.0259(4) 0.0178(3) 0.0204(4) -0.0029(3) 0.0069(3) -0.0044(3) S3 0.0166(4) 0.0328(4) 0.0219(4) -0.0101(3) 0.0092(3) -0.0054(3) S4 0.0190(4) 0.0244(4) 0.0180(3) -0.0055(3) 0.0086(3) -0.0042(3) Si1 0.0164(4) 0.0157(4) 0.0164(4) 0.0001(3) 0.0078(3) -0.0003(3) Si2 0.0193(4) 0.0181(4) 0.0229(4) -0.0028(3) 0.0064(3) 0.0003(3) N1 0.0152(12) 0.0269(14) 0.0239(14) -0.0080(11) 0.0102(11) -0.0046(10) O1 0.0208(11) 0.0197(10) 0.0207(11) 0.0044(8) 0.0087(9) -0.0002(8) O2 0.0217(11) 0.0193(10) 0.0206(11) 0.0015(8) 0.0103(9) 0.0029(8) O3 0.0192(10) 0.0192(10) 0.0153(10) -0.0008(8) 0.0068(8) -0.0025(8) O4 0.0168(11) 0.0183(10) 0.0270(12) -0.0037(9) 0.0020(9) -0.0026(8) O5 0.0241(13) 0.0220(12) 0.0645(19) -0.0029(12) 0.0187(13) 0.0042(10) O6 0.0365(15) 0.0313(13) 0.0248(13) 0.0001(10) 0.0087(11) 0.0057(11) C1 0.0314(18) 0.0192(14) 0.0222(16) 0.0032(12) 0.0124(14) -0.0047(13) C2 0.051(2) 0.0288(18) 0.0310(19) 0.0012(15) 0.0245(18) -0.0009(17) C3 0.0301(19) 0.0280(18) 0.037(2) 0.0055(15) 0.0098(16) -0.0075(15) C4 0.044(2) 0.0204(16) 0.0301(19) 0.0037(14) 0.0136(17) 0.0016(15) C5 0.0226(15) 0.0195(14) 0.0233(15) -0.0017(12) 0.0131(13) 0.0006(12) C6 0.0262(17) 0.0277(17) 0.0298(18) -0.0045(14) 0.0158(14) 0.0034(13) C7 0.0216(16) 0.0323(18) 0.0302(18) -0.0058(14) 0.0104(14) 0.0039(14) C8 0.0358(19) 0.0224(16) 0.0337(19) 0.0050(14) 0.0206(16) 0.0041(14) C9 0.0239(16) 0.0201(14) 0.0169(14) -0.0025(11) 0.0070(12) -0.0048(12) C10 0.0329(19) 0.0248(16) 0.0267(17) -0.0031(13) 0.0126(15) -0.0099(14) C11 0.038(2) 0.0304(18) 0.0180(15) -0.0021(13) 0.0141(15) -0.0095(15) C12 0.0215(16) 0.0280(17) 0.0288(18) 0.0002(14) 0.0022(14) -0.0025(13) C13 0.0192(15) 0.0202(15) 0.0274(17) -0.0045(13) 0.0030(13) -0.0011(12) C14 0.034(2) 0.031(2) 0.063(3) -0.0081(19) 0.024(2) -0.0088(16) C15 0.038(2) 0.0286(19) 0.035(2) -0.0051(16) -0.0013(17) -0.0015(16) C16 0.0297(19) 0.0224(17) 0.044(2) -0.0087(15) 0.0046(17) -0.0012(14) C17 0.0265(18) 0.0258(17) 0.041(2) -0.0041(15) 0.0151(16) 0.0063(14) C18 0.044(3) 0.042(3) 0.061(3) -0.003(2) -0.001(2) 0.013(2) C19 0.039(2) 0.027(2) 0.100(4) 0.004(2) 0.033(3) 0.0062(17) C20 0.124(6) 0.051(3) 0.065(4) -0.011(3) 0.063(4) 0.010(3) C21 0.039(2) 0.0290(18) 0.0216(16) 0.0046(13) 0.0109(15) -0.0003(15) C22 0.047(4) 0.040(3) 0.050(4) 0.010(3) 0.027(3) 0.013(3) C23 0.066(5) 0.075(6) 0.027(3) 0.010(3) 0.015(3) 0.009(4) C24 0.061(4) 0.041(4) 0.048(4) -0.004(3) 0.032(3) -0.015(3) C22A 0.096(14) 0.030(7) 0.061(11) -0.011(7) 0.054(11) 0.011(7) C23A 0.059(9) 0.058(9) 0.023(6) 0.018(6) 0.024(6) 0.012(7) C24A 0.046(8) 0.059(9) 0.038(7) 0.006(6) 0.025(6) -0.016(7) C25 0.0181(14) 0.0225(15) 0.0228(15) -0.0001(12) 0.0109(12) -0.0008(12) C26 0.0186(16) 0.0381(19) 0.0321(19) -0.0155(15) 0.0124(14) -0.0039(14) C27 0.0283(19) 0.059(3) 0.0266(18) -0.0067(17) 0.0149(16) -0.0036(18) C28 0.0174(15) 0.0364(19) 0.0357(19) -0.0113(15) 0.0132(14) -0.0077(14) C29 0.0229(18) 0.050(2) 0.041(2) -0.0058(19) 0.0047(17) -0.0008(17) Cd2 0.02126(11) 0.01756(10) 0.01601(10) 0.00003(8) 0.00873(9) -0.00044(8) Si3 0.0204(4) 0.0142(4) 0.0187(4) -0.0007(3) 0.0108(3) -0.0012(3) Si4 0.0187(4) 0.0143(4) 0.0141(4) 0.0012(3) 0.0071(3) -0.0012(3) S5 0.0211(4) 0.0166(3) 0.0194(3) -0.0007(3) 0.0111(3) -0.0008(3) S6 0.0197(4) 0.0166(3) 0.0187(3) 0.0002(3) 0.0085(3) 0.0011(3) S7 0.0167(3) 0.0239(4) 0.0159(3) -0.0001(3) 0.0061(3) 0.0025(3) S8 0.0202(4) 0.0189(3) 0.0188(3) 0.0012(3) 0.0086(3) 0.0026(3) N2 0.0186(13) 0.0226(13) 0.0134(12) 0.0028(10) 0.0032(10) -0.0015(10) O7 0.0216(11) 0.0177(10) 0.0196(11) 0.0018(8) 0.0094(9) -0.0054(8) O8 0.0230(11) 0.0156(10) 0.0279(12) 0.0040(9) 0.0145(10) 0.0015(8) O9 0.0256(12) 0.0199(10) 0.0222(11) -0.0073(9) 0.0146(10) -0.0067(9) O10 0.0203(11) 0.0157(10) 0.0288(12) -0.0034(9) 0.0117(10) 0.0022(8) O11 0.0250(11) 0.0189(10) 0.0157(10) 0.0040(8) 0.0078(9) -0.0033(9) O12 0.0246(11) 0.0210(11) 0.0190(11) 0.0010(8) 0.0107(9) -0.0050(9) C30 0.0209(15) 0.0167(14) 0.0219(15) 0.0003(11) 0.0114(12) -0.0025(11) C31 0.0314(18) 0.0289(17) 0.0342(19) 0.0012(14) 0.0227(16) -0.0026(14) C32 0.0298(17) 0.0172(14) 0.0194(15) 0.0023(12) 0.0075(13) -0.0027(12) C33 0.0293(17) 0.0222(15) 0.0235(16) -0.0051(13) 0.0109(14) -0.0064(13) C34 0.0251(17) 0.0203(15) 0.040(2) 0.0098(14) 0.0176(15) 0.0067(13) C35 0.0318(19) 0.0284(18) 0.056(3) 0.0143(17) 0.0274(19) 0.0116(15) C36 0.0269(18) 0.043(2) 0.033(2) 0.0128(16) 0.0112(16) 0.0074(16) C37 0.051(3) 0.0233(18) 0.069(3) 0.0210(19) 0.038(2) 0.0127(17) C38 0.0321(18) 0.0220(15) 0.0251(16) -0.0120(13) 0.0181(14) -0.0089(13) C39 0.046(2) 0.0321(19) 0.042(2) -0.0175(16) 0.0326(19) -0.0149(16) C40 0.037(2) 0.044(2) 0.0254(18) -0.0092(16) 0.0105(16) -0.0017(17) C41 0.040(2) 0.0260(17) 0.037(2) -0.0110(15) 0.0258(17) -0.0159(15) C42 0.0217(16) 0.0320(18) 0.0275(18) -0.0144(14) 0.0007(14) 0.0078(14) C43 0.0259(19) 0.040(2) 0.038(2) -0.0145(18) -0.0042(16) 0.0101(16) C44 0.0229(18) 0.069(3) 0.038(2) -0.021(2) 0.0146(17) -0.0002(18) C45 0.028(2) 0.033(2) 0.050(3) -0.0156(18) -0.0095(18) 0.0151(16) C46 0.0358(19) 0.0267(16) 0.0144(14) 0.0046(12) 0.0088(14) -0.0087(14) C47 0.037(2) 0.048(2) 0.0229(18) 0.0139(16) 0.0019(16) -0.0133(18) C48 0.056(3) 0.047(2) 0.030(2) -0.0002(17) 0.029(2) -0.004(2) C49 0.0338(19) 0.0298(18) 0.0255(17) 0.0097(14) 0.0067(15) -0.0092(15) C50 0.0209(15) 0.0226(15) 0.0231(16) 0.0037(12) 0.0065(13) -0.0061(12) C51 0.0279(18) 0.0347(19) 0.034(2) 0.0140(16) 0.0129(16) -0.0075(15) C52 0.049(2) 0.0190(16) 0.034(2) -0.0027(14) 0.0207(18) -0.0074(15) C53 0.0270(18) 0.0346(19) 0.0291(19) 0.0046(15) 0.0016(15) -0.0109(15) C54 0.0162(13) 0.0132(13) 0.0151(13) 0.0017(10) 0.0044(11) -0.0047(10) C55 0.0243(16) 0.0262(16) 0.0178(15) 0.0016(12) 0.0054(13) -0.0007(13) C56 0.040(2) 0.0271(18) 0.0301(19) 0.0084(15) 0.0093(17) -0.0023(15) C57 0.0328(19) 0.042(2) 0.0199(16) -0.0010(14) 0.0150(15) 0.0055(16) C58 0.057(3) 0.040(2) 0.031(2) -0.0100(17) 0.017(2) 0.011(2) N3 0.0195(13) 0.0172(12) 0.0179(12) 0.0011(10) 0.0087(10) -0.0021(10) C59 0.0283(17) 0.0154(14) 0.0237(16) 0.0033(12) 0.0132(13) -0.0018(12) C60 0.0326(18) 0.0199(15) 0.0231(16) 0.0018(12) 0.0080(14) 0.0001(13) C61 0.0269(18) 0.0243(17) 0.035(2) 0.0086(14) 0.0074(15) 0.0031(14) C62 0.031(2) 0.0324(19) 0.036(2) 0.0131(16) 0.0065(16) 0.0035(15) C63 0.0197(15) 0.0206(14) 0.0230(15) 0.0023(12) 0.0106(13) -0.0020(11) C64 0.0273(17) 0.0285(17) 0.0234(16) -0.0043(13) 0.0123(14) -0.0049(13) C65 0.037(2) 0.0284(17) 0.036(2) 0.0023(15) 0.0238(17) -0.0010(15) C66 0.030(2) 0.064(3) 0.066(3) -0.024(2) 0.024(2) -0.002(2) C67 0.0196(15) 0.0185(14) 0.0225(15) -0.0011(12) 0.0080(12) -0.0058(11) C68 0.0227(16) 0.0196(15) 0.0272(17) -0.0004(12) 0.0103(13) -0.0026(12) C69 0.0254(17) 0.0259(16) 0.0246(17) 0.0010(13) 0.0044(14) -0.0035(13) C70 0.0259(17) 0.0297(17) 0.0233(16) 0.0011(13) 0.0072(14) 0.0006(14) C71 0.0205(15) 0.0170(14) 0.0202(15) 0.0000(11) 0.0066(12) -0.0007(11) C72 0.0301(17) 0.0212(15) 0.0267(17) 0.0026(13) 0.0165(14) 0.0021(13) C73 0.052(3) 0.0293(19) 0.042(2) -0.0056(16) 0.031(2) -0.0030(17) C74 0.076(3) 0.037(2) 0.059(3) -0.001(2) 0.053(3) 0.005(2) N4 0.0254(13) 0.0140(11) 0.0246(13) 0.0057(10) 0.0153(11) 0.0017(10) C75 0.0266(16) 0.0215(15) 0.0225(15) 0.0048(12) 0.0132(13) 0.0002(12) C76 0.0323(19) 0.0317(18) 0.0338(19) -0.0012(15) 0.0201(16) 0.0030(15) C77 0.069(3) 0.036(2) 0.065(3) -0.010(2) 0.055(3) -0.006(2) C78 0.115(5) 0.038(2) 0.055(3) -0.002(2) 0.064(3) -0.011(3) C79 0.0289(17) 0.0146(14) 0.0319(18) 0.0048(12) 0.0167(15) 0.0006(12) C80 0.0251(17) 0.0208(15) 0.038(2) 0.0041(14) 0.0133(15) 0.0012(13) C81 0.0313(19) 0.0198(15) 0.037(2) 0.0003(14) 0.0149(16) 0.0006(13) C82 0.045(3) 0.032(2) 0.051(3) 0.0027(19) 0.006(2) -0.0104(18) C83 0.0295(17) 0.0211(15) 0.0228(16) 0.0079(12) 0.0123(14) 0.0060(13) C84 0.0248(16) 0.0209(15) 0.0262(16) 0.0061(12) 0.0114(14) 0.0043(12) C85 0.0297(18) 0.0379(19) 0.0215(16) 0.0061(14) 0.0124(14) 0.0073(15) C86 0.037(2) 0.045(2) 0.0288(19) -0.0079(17) 0.0082(17) 0.0033(18) C87 0.0258(16) 0.0164(14) 0.0272(16) 0.0063(12) 0.0135(14) 0.0031(12) C88 0.0295(17) 0.0203(15) 0.0295(17) -0.0009(13) 0.0180(15) -0.0022(13) C89 0.0313(19) 0.0231(16) 0.046(2) 0.0006(15) 0.0233(17) -0.0001(14) C90 0.043(2) 0.039(2) 0.053(3) -0.0097(19) 0.032(2) -0.0031(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.4843(8) . ? Cd1 S2 2.5131(8) . ? Cd1 S3 2.6375(8) . ? Cd1 S4 2.6554(9) . ? S1 Si1 2.0836(11) . ? S2 Si2 2.0826(12) . ? S3 C25 1.724(3) . ? S4 C25 1.725(3) . ? Si1 O3 1.634(2) . ? Si1 O1 1.634(2) . ? Si1 O2 1.640(2) . ? Si2 O6 1.633(3) . ? Si2 O5 1.636(3) . ? Si2 O4 1.639(2) . ? N1 C25 1.343(4) . ? N1 C26 1.471(4) . ? N1 C28 1.474(4) . ? O1 C1 1.441(4) . ? O2 C5 1.443(4) . ? O3 C9 1.452(4) . ? O4 C13 1.441(4) . ? O5 C17 1.429(4) . ? O6 C21 1.446(5) . ? C1 C4 1.526(5) . ? C1 C2 1.532(5) . ? C1 C3 1.532(5) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C8 1.526(5) . ? C5 C7 1.528(5) . ? C5 C6 1.531(4) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C12 1.520(5) . ? C9 C10 1.524(4) . ? C9 C11 1.526(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.518(5) . ? C13 C15 1.529(5) . ? C13 C16 1.531(5) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.497(6) . ? C17 C19 1.516(6) . ? C17 C20 1.521(6) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.479(7) . ? C21 C24 1.514(7) . ? C21 C23 1.520(7) . ? C21 C23A 1.532(13) . ? C21 C22A 1.579(13) . ? C21 C24A 1.600(15) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C22A H22D 0.98 . ? C22A H22E 0.98 . ? C22A H22F 0.98 . ? C23A H23D 0.98 . ? C23A H23E 0.98 . ? C23A H23F 0.98 . ? C24A H24D 0.98 . ? C24A H24E 0.98 . ? C24A H24F 0.98 . ? C26 C27 1.514(6) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.515(6) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? Cd2 S5 2.4935(8) . ? Cd2 S6 2.5033(8) . ? Cd2 S7 2.6468(8) . ? Cd2 S8 2.6584(9) . ? Si3 O8 1.636(2) . ? Si3 O7 1.643(2) . ? Si3 O9 1.645(2) . ? Si3 S5 2.0822(11) . ? Si4 O12 1.633(2) . ? Si4 O11 1.637(2) . ? Si4 O10 1.640(2) . ? Si4 S6 2.0826(11) . ? S7 C54 1.720(3) . ? S8 C54 1.713(3) . ? N2 C54 1.347(4) . ? N2 C55 1.471(4) . ? N2 C57 1.476(4) . ? O7 C30 1.434(4) . ? O8 C34 1.447(4) . ? O9 C38 1.442(4) . ? O10 C42 1.443(4) . ? O11 C46 1.443(4) . ? O12 C50 1.445(4) . ? C30 C31 1.522(4) . ? C30 C33 1.522(4) . ? C30 C32 1.528(4) . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 C36 1.517(6) . ? C34 C37 1.525(5) . ? C34 C35 1.537(5) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C40 1.515(5) . ? C38 C41 1.528(5) . ? C38 C39 1.528(5) . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 C44 1.521(6) . ? C42 C45 1.528(5) . ? C42 C43 1.541(5) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C46 C48 1.516(6) . ? C46 C49 1.518(5) . ? C46 C47 1.526(5) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 C53 1.520(5) . ? C50 C51 1.522(4) . ? C50 C52 1.529(5) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C55 C56 1.519(5) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C57 C58 1.508(6) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 H58A 0.98 . ? C58 H58B 0.98 . ? C58 H58C 0.98 . ? N3 C63 1.518(4) . ? N3 C67 1.518(4) . ? N3 C71 1.523(4) . ? N3 C59 1.533(4) . ? C59 C60 1.512(5) . ? C59 H59A 0.99 . ? C59 H59B 0.99 . ? C60 C61 1.516(5) . ? C60 H60A 0.99 . ? C60 H60B 0.99 . ? C61 C62 1.507(5) . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63 C64 1.526(5) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? C64 C65 1.525(5) . ? C64 H64A 0.99 . ? C64 H64B 0.99 . ? C65 C66 1.511(6) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 H66A 0.98 . ? C66 H66B 0.98 . ? C66 H66C 0.98 . ? C67 C68 1.521(4) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C69 1.521(5) . ? C68 H68A 0.99 . ? C68 H68B 0.99 . ? C69 C70 1.529(5) . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? C70 H70A 0.98 . ? C70 H70B 0.98 . ? C70 H70C 0.98 . ? C71 C72 1.522(4) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 C73 1.517(5) . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? C73 C74 1.522(6) . ? C73 H73A 0.99 . ? C73 H73B 0.99 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? N4 C83 1.515(4) . ? N4 C87 1.519(4) . ? N4 C75 1.524(4) . ? N4 C79 1.527(4) . ? C75 C76 1.521(5) . ? C75 H75A 0.99 . ? C75 H75B 0.99 . ? C76 C77 1.538(5) . ? C76 H76A 0.99 . ? C76 H76B 0.99 . ? C77 C78 1.518(8) . ? C77 H77A 0.99 . ? C77 H77B 0.99 . ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? C79 C80 1.518(5) . ? C79 H79A 0.99 . ? C79 H79B 0.99 . ? C80 C81 1.530(5) . ? C80 H80A 0.99 . ? C80 H80B 0.99 . ? C81 C82 1.494(6) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? C83 C84 1.517(5) . ? C83 H83A 0.99 . ? C83 H83B 0.99 . ? C84 C85 1.521(5) . ? C84 H84A 0.99 . ? C84 H84B 0.99 . ? C85 C86 1.526(6) . ? C85 H85A 0.99 . ? C85 H85B 0.99 . ? C86 H86A 0.98 . ? C86 H86B 0.98 . ? C86 H86C 0.98 . ? C87 C88 1.509(5) . ? C87 H87A 0.99 . ? C87 H87B 0.99 . ? C88 C89 1.538(5) . ? C88 H88A 0.99 . ? C88 H88B 0.99 . ? C89 C90 1.519(5) . ? C89 H89A 0.99 . ? C89 H89B 0.99 . ? C90 H90A 0.98 . ? C90 H90B 0.98 . ? C90 H90C 0.98 . ? 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 S1 Cd1 S2 123.03(3) . . ? S1 Cd1 S3 111.28(3) . . ? S2 Cd1 S3 113.48(3) . . ? S1 Cd1 S4 121.44(3) . . ? S2 Cd1 S4 106.76(3) . . ? S3 Cd1 S4 68.44(3) . . ? Si1 S1 Cd1 100.64(4) . . ? Si2 S2 Cd1 94.87(4) . . ? C25 S3 Cd1 86.34(11) . . ? C25 S4 Cd1 85.75(11) . . ? O3 Si1 O1 106.31(12) . . ? O3 Si1 O2 110.87(12) . . ? O1 Si1 O2 103.69(12) . . ? O3 Si1 S1 108.03(9) . . ? O1 Si1 S1 113.50(9) . . ? O2 Si1 S1 114.18(9) . . ? O6 Si2 O5 102.91(15) . . ? O6 Si2 O4 112.20(14) . . ? O5 Si2 O4 105.50(13) . . ? O6 Si2 S2 115.26(11) . . ? O5 Si2 S2 114.77(12) . . ? O4 Si2 S2 105.94(9) . . ? C25 N1 C26 122.4(3) . . ? C25 N1 C28 122.8(3) . . ? C26 N1 C28 114.6(3) . . ? C1 O1 Si1 133.5(2) . . ? C5 O2 Si1 132.5(2) . . ? C9 O3 Si1 130.38(19) . . ? C13 O4 Si2 131.8(2) . . ? C17 O5 Si2 134.2(2) . . ? C21 O6 Si2 136.3(2) . . ? O1 C1 C4 105.3(3) . . ? O1 C1 C2 108.4(3) . . ? C4 C1 C2 111.0(3) . . ? O1 C1 C3 111.5(3) . . ? C4 C1 C3 109.8(3) . . ? C2 C1 C3 110.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C8 111.5(3) . . ? O2 C5 C7 108.5(3) . . ? C8 C5 C7 110.3(3) . . ? O2 C5 C6 104.4(3) . . ? C8 C5 C6 110.7(3) . . ? C7 C5 C6 111.1(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C12 108.4(3) . . ? O3 C9 C10 105.3(3) . . ? C12 C9 C10 109.8(3) . . ? O3 C9 C11 111.9(3) . . ? C12 C9 C11 111.4(3) . . ? C10 C9 C11 109.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C14 109.4(3) . . ? O4 C13 C15 110.6(3) . . ? C14 C13 C15 111.4(3) . . ? O4 C13 C16 105.1(3) . . ? C14 C13 C16 110.3(3) . . ? C15 C13 C16 109.8(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C18 106.1(3) . . ? O5 C17 C19 112.9(3) . . ? C18 C17 C19 111.9(4) . . ? O5 C17 C20 106.1(4) . . ? C18 C17 C20 110.7(4) . . ? C19 C17 C20 109.0(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 C22 109.6(4) . . ? O6 C21 C24 104.6(4) . . ? C22 C21 C24 113.8(5) . . ? O6 C21 C23 102.6(4) . . ? C22 C21 C23 114.1(5) . . ? C24 C21 C23 111.0(5) . . ? O6 C21 C23A 112.2(6) . . ? C22 C21 C23A 136.8(7) . . ? C24 C21 C23A 65.2(7) . . ? C23 C21 C23A 45.9(7) . . ? O6 C21 C22A 110.9(7) . . ? C22 C21 C22A 45.2(7) . . ? C24 C21 C22A 143.3(8) . . ? C23 C21 C22A 70.1(8) . . ? C23A C21 C22A 107.7(9) . . ? O6 C21 C24A 114.7(5) . . ? C22 C21 C24A 63.4(7) . . ? C24 C21 C24A 51.0(6) . . ? C23 C21 C24A 141.3(6) . . ? C23A C21 C24A 106.9(9) . . ? C22A C21 C24A 103.9(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C22A H22D 109.5 . . ? C21 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21 C23A H23D 109.5 . . ? C21 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21 C24A H24D 109.5 . . ? C21 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C21 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N1 C25 S3 119.4(2) . . ? N1 C25 S4 121.3(2) . . ? S3 C25 S4 119.34(18) . . ? N1 C26 C27 111.6(3) . . ? N1 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? N1 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 C29 111.7(3) . . ? N1 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? N1 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? S5 Cd2 S6 112.73(3) . . ? S5 Cd2 S7 111.90(3) . . ? S6 Cd2 S7 123.78(3) . . ? S5 Cd2 S8 120.41(3) . . ? S6 Cd2 S8 113.68(3) . . ? S7 Cd2 S8 67.89(2) . . ? O8 Si3 O7 105.40(12) . . ? O8 Si3 O9 111.30(12) . . ? O7 Si3 O9 103.49(11) . . ? O8 Si3 S5 108.92(9) . . ? O7 Si3 S5 113.16(9) . . ? O9 Si3 S5 114.17(10) . . ? O12 Si4 O11 103.50(12) . . ? O12 Si4 O10 106.61(12) . . ? O11 Si4 O10 111.98(12) . . ? O12 Si4 S6 113.82(9) . . ? O11 Si4 S6 114.38(9) . . ? O10 Si4 S6 106.42(9) . . ? Si3 S5 Cd2 101.35(4) . . ? Si4 S6 Cd2 98.71(4) . . ? C54 S7 Cd2 86.53(10) . . ? C54 S8 Cd2 86.30(10) . . ? C54 N2 C55 122.7(3) . . ? C54 N2 C57 122.8(3) . . ? C55 N2 C57 114.6(3) . . ? C30 O7 Si3 131.6(2) . . ? C34 O8 Si3 130.6(2) . . ? C38 O9 Si3 131.7(2) . . ? C42 O10 Si4 130.8(2) . . ? C46 O11 Si4 132.9(2) . . ? C50 O12 Si4 131.8(2) . . ? O7 C30 C31 107.9(3) . . ? O7 C30 C33 105.1(2) . . ? C31 C30 C33 111.1(3) . . ? O7 C30 C32 112.0(2) . . ? C31 C30 C32 110.4(3) . . ? C33 C30 C32 110.2(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O8 C34 C36 108.6(3) . . ? O8 C34 C37 104.6(3) . . ? C36 C34 C37 110.7(3) . . ? O8 C34 C35 111.5(3) . . ? C36 C34 C35 111.7(3) . . ? C37 C34 C35 109.6(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O9 C38 C40 109.4(3) . . ? O9 C38 C41 111.0(3) . . ? C40 C38 C41 111.3(3) . . ? O9 C38 C39 104.9(3) . . ? C40 C38 C39 109.2(3) . . ? C41 C38 C39 110.9(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O10 C42 C44 108.7(3) . . ? O10 C42 C45 105.3(3) . . ? C44 C42 C45 111.6(3) . . ? O10 C42 C43 111.2(3) . . ? C44 C42 C43 110.8(3) . . ? C45 C42 C43 109.0(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O11 C46 C48 108.3(3) . . ? O11 C46 C49 110.8(3) . . ? C48 C46 C49 111.1(3) . . ? O11 C46 C47 105.4(3) . . ? C48 C46 C47 110.6(3) . . ? C49 C46 C47 110.4(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O12 C50 C53 109.0(3) . . ? O12 C50 C51 104.9(3) . . ? C53 C50 C51 110.3(3) . . ? O12 C50 C52 111.6(3) . . ? C53 C50 C52 110.3(3) . . ? C51 C50 C52 110.6(3) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54 S8 120.7(2) . . ? N2 C54 S7 120.0(2) . . ? S8 C54 S7 119.27(17) . . ? N2 C55 C56 112.3(3) . . ? N2 C55 H55A 109.2 . . ? C56 C55 H55A 109.2 . . ? N2 C55 H55B 109.2 . . ? C56 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2 C57 C58 111.5(3) . . ? N2 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? N2 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C63 N3 C67 110.8(2) . . ? C63 N3 C71 106.5(2) . . ? C67 N3 C71 111.5(2) . . ? C63 N3 C59 110.4(2) . . ? C67 N3 C59 107.1(2) . . ? C71 N3 C59 110.5(2) . . ? C60 C59 N3 114.8(3) . . ? C60 C59 H59A 108.6 . . ? N3 C59 H59A 108.6 . . ? C60 C59 H59B 108.6 . . ? N3 C59 H59B 108.6 . . ? H59A C59 H59B 107.5 . . ? C59 C60 C61 111.9(3) . . ? C59 C60 H60A 109.2 . . ? C61 C60 H60A 109.2 . . ? C59 C60 H60B 109.2 . . ? C61 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C62 C61 C60 112.7(3) . . ? C62 C61 H61A 109 . . ? C60 C61 H61A 109 . . ? C62 C61 H61B 109 . . ? C60 C61 H61B 109 . . ? H61A C61 H61B 107.8 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N3 C63 C64 115.7(3) . . ? N3 C63 H63A 108.3 . . ? C64 C63 H63A 108.3 . . ? N3 C63 H63B 108.3 . . ? C64 C63 H63B 108.3 . . ? H63A C63 H63B 107.4 . . ? C65 C64 C63 111.0(3) . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64B 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 108 . . ? C66 C65 C64 113.8(3) . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65B 108.8 . . ? C64 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N3 C67 C68 114.5(2) . . ? N3 C67 H67A 108.6 . . ? C68 C67 H67A 108.6 . . ? N3 C67 H67B 108.6 . . ? C68 C67 H67B 108.6 . . ? H67A C67 H67B 107.6 . . ? C67 C68 C69 111.5(3) . . ? C67 C68 H68A 109.3 . . ? C69 C68 H68A 109.3 . . ? C67 C68 H68B 109.3 . . ? C69 C68 H68B 109.3 . . ? H68A C68 H68B 108 . . ? C68 C69 C70 111.1(3) . . ? C68 C69 H69A 109.4 . . ? C70 C69 H69A 109.4 . . ? C68 C69 H69B 109.4 . . ? C70 C69 H69B 109.4 . . ? H69A C69 H69B 108 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 N3 115.5(3) . . ? C72 C71 H71A 108.4 . . ? N3 C71 H71A 108.4 . . ? C72 C71 H71B 108.4 . . ? N3 C71 H71B 108.4 . . ? H71A C71 H71B 107.5 . . ? C73 C72 C71 110.5(3) . . ? C73 C72 H72A 109.6 . . ? C71 C72 H72A 109.6 . . ? C73 C72 H72B 109.6 . . ? C71 C72 H72B 109.6 . . ? H72A C72 H72B 108.1 . . ? C72 C73 C74 111.8(3) . . ? C72 C73 H73A 109.3 . . ? C74 C73 H73A 109.3 . . ? C72 C73 H73B 109.3 . . ? C74 C73 H73B 109.3 . . ? H73A C73 H73B 107.9 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C83 N4 C87 111.5(3) . . ? C83 N4 C75 111.5(3) . . ? C87 N4 C75 105.8(2) . . ? C83 N4 C79 105.9(2) . . ? C87 N4 C79 111.4(2) . . ? C75 N4 C79 110.8(2) . . ? C76 C75 N4 115.9(3) . . ? C76 C75 H75A 108.3 . . ? N4 C75 H75A 108.3 . . ? C76 C75 H75B 108.3 . . ? N4 C75 H75B 108.3 . . ? H75A C75 H75B 107.4 . . ? C75 C76 C77 110.6(3) . . ? C75 C76 H76A 109.5 . . ? C77 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 108.1 . . ? C78 C77 C76 114.4(4) . . ? C78 C77 H77A 108.7 . . ? C76 C77 H77A 108.7 . . ? C78 C77 H77B 108.7 . . ? C76 C77 H77B 108.7 . . ? H77A C77 H77B 107.6 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 N4 116.0(3) . . ? C80 C79 H79A 108.3 . . ? N4 C79 H79A 108.3 . . ? C80 C79 H79B 108.3 . . ? N4 C79 H79B 108.3 . . ? H79A C79 H79B 107.4 . . ? C79 C80 C81 110.1(3) . . ? C79 C80 H80A 109.6 . . ? C81 C80 H80A 109.6 . . ? C79 C80 H80B 109.6 . . ? C81 C80 H80B 109.6 . . ? H80A C80 H80B 108.2 . . ? C82 C81 C80 114.0(3) . . ? C82 C81 H81A 108.8 . . ? C80 C81 H81A 108.8 . . ? C82 C81 H81B 108.8 . . ? C80 C81 H81B 108.8 . . ? H81A C81 H81B 107.6 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N4 C83 C84 115.1(3) . . ? N4 C83 H83A 108.5 . . ? C84 C83 H83A 108.5 . . ? N4 C83 H83B 108.5 . . ? C84 C83 H83B 108.5 . . ? H83A C83 H83B 107.5 . . ? C83 C84 C85 112.0(3) . . ? C83 C84 H84A 109.2 . . ? C85 C84 H84A 109.2 . . ? C83 C84 H84B 109.2 . . ? C85 C84 H84B 109.2 . . ? H84A C84 H84B 107.9 . . ? C84 C85 C86 111.9(3) . . ? C84 C85 H85A 109.2 . . ? C86 C85 H85A 109.2 . . ? C84 C85 H85B 109.2 . . ? C86 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 N4 118.0(3) . . ? C88 C87 H87A 107.8 . . ? N4 C87 H87A 107.8 . . ? C88 C87 H87B 107.8 . . ? N4 C87 H87B 107.8 . . ? H87A C87 H87B 107.1 . . ? C87 C88 C89 108.0(3) . . ? C87 C88 H88A 110.1 . . ? C89 C88 H88A 110.1 . . ? C87 C88 H88B 110.1 . . ? C89 C88 H88B 110.1 . . ? H88A C88 H88B 108.4 . . ? C90 C89 C88 112.8(3) . . ? C90 C89 H89A 109 . . ? C88 C89 H89A 109 . . ? C90 C89 H89B 109 . . ? C88 C89 H89B 109 . . ? H89A C89 H89B 107.8 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? #===END data_comp4 _database_code_depnum_ccdc_archive 'CCDC 684880' _audit_creation_date 2006-11-07T16:40:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H64 Cd N O6 S4 Si2 1-, C20 H44 N 1+' _chemical_formula_sum 'C49 H108 Cd N2 O6 S4 Si2' _chemical_formula_weight 1118.19 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.5826(5) _cell_length_b 23.0701(6) _cell_length_c 22.6833(8) _cell_angle_alpha 90 _cell_angle_beta 105.532(3) _cell_angle_gamma 90 _cell_volume 6344.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17884 _cell_measurement_theta_min 2.1238 _cell_measurement_theta_max 32.7025 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.004102552 _diffrn_orient_matrix_ub_12 -0.0062751985 _diffrn_orient_matrix_ub_13 -0.0299234979 _diffrn_orient_matrix_ub_21 0.0058402448 _diffrn_orient_matrix_ub_22 0.0299910687 _diffrn_orient_matrix_ub_23 -0.0052831153 _diffrn_orient_matrix_ub_31 0.0580714225 _diffrn_orient_matrix_ub_32 -0.0025371713 _diffrn_orient_matrix_ub_33 0.0114016205 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_number 54694 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.3 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 18478 _reflns_number_gt 16484 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0339P)^2^+11.5986P] 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_number_reflns 18478 _refine_ls_number_parameters 601 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.477 _refine_diff_density_min -0.97 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 0.006 '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' S S 0.1246 0.1234 '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' 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 0.031668(13) 0.113605(7) 0.191365(7) 0.01703(4) Uani 1 1 d . . . Si1 Si 0.09931(5) 0.20621(3) 0.09062(3) 0.01609(11) Uani 1 1 d . . . Si2 Si -0.23809(5) 0.07765(3) 0.15979(3) 0.01449(11) Uani 1 1 d . . . S1 S 0.03574(5) 0.21917(2) 0.16522(2) 0.01797(10) Uani 1 1 d . . . S2 S -0.10456(4) 0.03849(2) 0.13766(2) 0.01691(10) Uani 1 1 d . . . S3 S 0.09381(5) 0.11114(3) 0.31297(2) 0.02067(11) Uani 1 1 d . . . S4 S 0.22754(5) 0.06176(3) 0.23534(3) 0.01968(11) Uani 1 1 d . . . O1 O 0.21327(14) 0.24189(8) 0.09389(8) 0.0244(3) Uani 1 1 d . . . O2 O 0.11519(14) 0.13600(7) 0.08716(7) 0.0189(3) Uani 1 1 d . . . O3 O 0.01762(15) 0.22571(7) 0.02465(7) 0.0221(3) Uani 1 1 d . . . O4 O -0.18442(13) 0.13074(7) 0.20633(7) 0.0171(3) Uani 1 1 d . . . O5 O -0.33579(13) 0.10077(7) 0.10162(7) 0.0201(3) Uani 1 1 d . . . O6 O -0.30032(13) 0.03603(7) 0.19856(7) 0.0197(3) Uani 1 1 d . . . C1 C 0.3114(2) 0.25388(11) 0.14185(14) 0.0282(5) Uani 1 1 d . . . C2 C 0.2920(2) 0.30779(13) 0.17621(14) 0.0354(6) Uani 1 1 d . . . H2A H 0.2747 0.3406 0.1478 0.042 Uiso 1 1 calc R . . H2B H 0.3586 0.3165 0.2089 0.042 Uiso 1 1 calc R . . H2C H 0.2302 0.301 0.194 0.042 Uiso 1 1 calc R . . C3 C 0.4006(3) 0.26594(18) 0.1095(2) 0.0553(10) Uani 1 1 d . . . H3A H 0.4107 0.2317 0.0861 0.066 Uiso 1 1 calc R . . H3B H 0.4701 0.2749 0.14 0.066 Uiso 1 1 calc R . . H3C H 0.3786 0.299 0.0818 0.066 Uiso 1 1 calc R . . C4 C 0.3429(3) 0.20259(14) 0.18533(18) 0.0476(9) Uani 1 1 d . . . H4A H 0.2846 0.1957 0.2057 0.057 Uiso 1 1 calc R . . H4B H 0.4123 0.2111 0.2161 0.057 Uiso 1 1 calc R . . H4C H 0.3522 0.168 0.1622 0.057 Uiso 1 1 calc R . . C5 C 0.1342(2) 0.09824(10) 0.04013(11) 0.0232(5) Uani 1 1 d . . . C6 C 0.0256(3) 0.08843(13) -0.00755(13) 0.0348(6) Uani 1 1 d . . . H6A H -0.0279 0.0716 0.012 0.042 Uiso 1 1 calc R . . H6B H 0.037 0.0618 -0.039 0.042 Uiso 1 1 calc R . . H6C H -0.0024 0.1255 -0.0265 0.042 Uiso 1 1 calc R . . C7 C 0.2198(3) 0.12389(15) 0.01173(17) 0.0458(8) Uani 1 1 d . . . H7A H 0.1928 0.1609 -0.0078 0.055 Uiso 1 1 calc R . . H7B H 0.2333 0.0971 -0.019 0.055 Uiso 1 1 calc R . . H7C H 0.2887 0.1303 0.0436 0.055 Uiso 1 1 calc R . . C8 C 0.1743(3) 0.04149(12) 0.07281(13) 0.0333(6) Uani 1 1 d . . . H8A H 0.2436 0.0482 0.1043 0.04 Uiso 1 1 calc R . . H8B H 0.1867 0.0131 0.0432 0.04 Uiso 1 1 calc R . . H8C H 0.1186 0.0266 0.0919 0.04 Uiso 1 1 calc R . . C9 C -0.0063(2) 0.28149(10) -0.00416(11) 0.0241(5) Uani 1 1 d . . . C10 C -0.1250(3) 0.27842(12) -0.04286(13) 0.0339(6) Uani 1 1 d . . . H10A H -0.1335 0.2457 -0.0713 0.041 Uiso 1 1 calc R . . H10B H -0.1442 0.3145 -0.066 0.041 Uiso 1 1 calc R . . H10C H -0.174 0.273 -0.0162 0.041 Uiso 1 1 calc R . . C11 C 0.0712(3) 0.29101(16) -0.04413(16) 0.0468(8) Uani 1 1 d . . . H11A H 0.1474 0.2921 -0.0185 0.056 Uiso 1 1 calc R . . H11B H 0.0533 0.3278 -0.0661 0.056 Uiso 1 1 calc R . . H11C H 0.0629 0.2592 -0.0737 0.056 Uiso 1 1 calc R . . C12 C 0.0056(3) 0.32979(11) 0.04323(13) 0.0345(6) Uani 1 1 d . . . H12A H -0.0408 0.3211 0.0706 0.041 Uiso 1 1 calc R . . H12B H -0.0174 0.3667 0.0224 0.041 Uiso 1 1 calc R . . H12C H 0.0829 0.3325 0.0672 0.041 Uiso 1 1 calc R . . C13 C -0.2333(2) 0.17612(10) 0.23419(11) 0.0206(4) Uani 1 1 d . . . C14 C -0.1418(2) 0.19738(12) 0.28776(13) 0.0312(6) Uani 1 1 d . . . H14A H -0.1205 0.1663 0.3181 0.037 Uiso 1 1 calc R . . H14B H -0.1677 0.2309 0.3065 0.037 Uiso 1 1 calc R . . H14C H -0.0779 0.2086 0.2733 0.037 Uiso 1 1 calc R . . C15 C -0.2694(2) 0.22477(12) 0.18707(13) 0.0309(6) Uani 1 1 d . . . H15A H -0.2063 0.2373 0.1726 0.037 Uiso 1 1 calc R . . H15B H -0.297 0.2576 0.2061 0.037 Uiso 1 1 calc R . . H15C H -0.328 0.2105 0.1524 0.037 Uiso 1 1 calc R . . C16 C -0.3304(2) 0.15444(13) 0.25547(15) 0.0362(6) Uani 1 1 d . . . H16A H -0.3906 0.1436 0.2199 0.043 Uiso 1 1 calc R . . H16B H -0.3556 0.1851 0.2784 0.043 Uiso 1 1 calc R . . H16C H -0.3079 0.1206 0.2819 0.043 Uiso 1 1 calc R . . C17 C -0.3392(2) 0.11848(11) 0.04010(10) 0.0220(4) Uani 1 1 d . . . C18 C -0.2451(2) 0.15963(13) 0.03998(12) 0.0322(6) Uani 1 1 d . . . H18A H -0.2478 0.1929 0.0664 0.039 Uiso 1 1 calc R . . H18B H -0.2521 0.1732 -0.0018 0.039 Uiso 1 1 calc R . . H18C H -0.1746 0.1394 0.0553 0.039 Uiso 1 1 calc R . . C19 C -0.4503(2) 0.14853(16) 0.01591(13) 0.0393(7) Uani 1 1 d . . . H19A H -0.5096 0.1217 0.0179 0.047 Uiso 1 1 calc R . . H19B H -0.4592 0.1604 -0.0266 0.047 Uiso 1 1 calc R . . H19C H -0.4534 0.1828 0.0409 0.047 Uiso 1 1 calc R . . C20 C -0.3333(2) 0.06497(13) 0.00214(12) 0.0319(6) Uani 1 1 d . . . H20A H -0.2658 0.0433 0.0211 0.038 Uiso 1 1 calc R . . H20B H -0.3326 0.0767 -0.0393 0.038 Uiso 1 1 calc R . . H20C H -0.3976 0.0403 0.0001 0.038 Uiso 1 1 calc R . . C21 C -0.39404(19) -0.00214(10) 0.18053(12) 0.0244(5) Uani 1 1 d . . . C22 C -0.3869(2) -0.03862(11) 0.12586(13) 0.0315(6) Uani 1 1 d . . . H22A H -0.3962 -0.0136 0.0899 0.038 Uiso 1 1 calc R . . H22B H -0.4452 -0.068 0.1177 0.038 Uiso 1 1 calc R . . H22C H -0.3147 -0.0577 0.1348 0.038 Uiso 1 1 calc R . . C23 C -0.5003(2) 0.03338(13) 0.16537(16) 0.0366(7) Uani 1 1 d . . . H23A H -0.5051 0.0552 0.2016 0.044 Uiso 1 1 calc R . . H23B H -0.5639 0.0073 0.1527 0.044 Uiso 1 1 calc R . . H23C H -0.5003 0.0604 0.132 0.044 Uiso 1 1 calc R . . C24 C -0.3876(2) -0.04033(13) 0.23636(14) 0.0351(6) Uani 1 1 d . . . H24A H -0.3199 -0.0635 0.2451 0.042 Uiso 1 1 calc R . . H24B H -0.4517 -0.0662 0.2281 0.042 Uiso 1 1 calc R . . H24C H -0.387 -0.0158 0.2717 0.042 Uiso 1 1 calc R . . N1 N 0.30020(16) 0.07389(9) 0.35638(9) 0.0214(4) Uani 1 1 d . . . C25 C 0.21546(18) 0.08158(10) 0.30656(10) 0.0183(4) Uani 1 1 d . . . C26 C 0.4066(2) 0.05029(12) 0.35273(12) 0.0275(5) Uani 1 1 d . . . H26A H 0.3936 0.0211 0.3196 0.033 Uiso 1 1 calc R . . H26B H 0.4426 0.0305 0.3917 0.033 Uiso 1 1 calc R . . C27 C 0.4834(2) 0.09685(14) 0.34050(14) 0.0340(6) Uani 1 1 d . . . H27A H 0.4503 0.1149 0.3007 0.041 Uiso 1 1 calc R . . H27B H 0.5542 0.0793 0.3402 0.041 Uiso 1 1 calc R . . H27C H 0.4954 0.1264 0.3727 0.041 Uiso 1 1 calc R . . C28 C 0.2955(2) 0.09405(12) 0.41715(11) 0.0271(5) Uani 1 1 d . . . H28A H 0.2446 0.1275 0.4121 0.033 Uiso 1 1 calc R . . H28B H 0.3697 0.1075 0.4402 0.033 Uiso 1 1 calc R . . C29 C 0.2571(3) 0.04719(15) 0.45380(13) 0.0430(7) Uani 1 1 d . . . H29A H 0.1806 0.0368 0.4335 0.052 Uiso 1 1 calc R . . H29B H 0.2618 0.0616 0.495 0.052 Uiso 1 1 calc R . . H29C H 0.3042 0.0129 0.4565 0.052 Uiso 1 1 calc R . . N2 N 0.04473(16) 0.89397(8) 0.25540(9) 0.0189(4) Uani 1 1 d . . . C30 C -0.0113(2) 0.94668(10) 0.27416(11) 0.0207(4) Uani 1 1 d . . . H30A H -0.0729 0.9586 0.239 0.025 Uiso 1 1 calc R . . H30B H 0.0423 0.979 0.2833 0.025 Uiso 1 1 calc R . . C31 C -0.0565(2) 0.93715(11) 0.32947(12) 0.0258(5) Uani 1 1 d . . . H31A H 0.0031 0.923 0.3645 0.031 Uiso 1 1 calc R . . H31B H -0.1156 0.9075 0.3197 0.031 Uiso 1 1 calc R . . C32 C -0.1024(2) 0.99421(10) 0.34635(11) 0.0242(5) Uani 1 1 d . . . H32A H -0.0429 1.0236 0.3554 0.029 Uiso 1 1 calc R . . H32B H -0.1612 1.0081 0.3109 0.029 Uiso 1 1 calc R . . C33 C -0.1491(3) 0.98848(14) 0.40146(15) 0.0414(7) Uani 1 1 d . . . H33A H -0.2127 0.9616 0.3913 0.05 Uiso 1 1 calc R . . H33B H -0.0921 0.9716 0.4361 0.05 Uiso 1 1 calc R . . C34 C -0.1860(3) 1.04621(15) 0.42091(17) 0.0481(8) Uani 1 1 d . . . H34A H -0.1236 1.0732 0.4303 0.058 Uiso 1 1 calc R . . H34B H -0.2127 1.0407 0.4573 0.058 Uiso 1 1 calc R . . H34C H -0.2454 1.062 0.3876 0.058 Uiso 1 1 calc R . . C35 C 0.1395(2) 0.87304(10) 0.30767(11) 0.0221(4) Uani 1 1 d . . . H35A H 0.1083 0.8562 0.3396 0.026 Uiso 1 1 calc R . . H35B H 0.178 0.8415 0.2922 0.026 Uiso 1 1 calc R . . C36 C 0.2242(2) 0.91832(12) 0.33744(13) 0.0314(6) Uani 1 1 d . . . H36A H 0.1898 0.9471 0.359 0.038 Uiso 1 1 calc R . . H36B H 0.2501 0.9389 0.3056 0.038 Uiso 1 1 calc R . . C37 C 0.3221(2) 0.88975(13) 0.38294(13) 0.0333(6) Uani 1 1 d . . . H37A H 0.3566 0.8618 0.3606 0.04 Uiso 1 1 calc R . . H37B H 0.3776 0.92 0.4002 0.04 Uiso 1 1 calc R . . C38 C 0.2929(2) 0.85817(15) 0.43540(13) 0.0368(6) Uani 1 1 d . . . H38A H 0.2491 0.8843 0.4544 0.044 Uiso 1 1 calc R . . H38B H 0.2465 0.8242 0.4189 0.044 Uiso 1 1 calc R . . C39 C 0.3943(3) 0.8379(2) 0.48426(17) 0.0601(11) Uani 1 1 d . . . H39A H 0.4365 0.8108 0.4661 0.072 Uiso 1 1 calc R . . H39B H 0.3711 0.8185 0.5172 0.072 Uiso 1 1 calc R . . H39C H 0.4404 0.8714 0.5009 0.072 Uiso 1 1 calc R . . C40 C -0.03345(19) 0.84296(10) 0.23810(10) 0.0198(4) Uani 1 1 d . . . H40A H -0.0523 0.8293 0.2755 0.024 Uiso 1 1 calc R . . H40B H 0.0063 0.811 0.224 0.024 Uiso 1 1 calc R . . C41 C -0.1401(2) 0.85403(11) 0.18915(11) 0.0240(5) Uani 1 1 d . . . H41A H -0.124 0.8728 0.1533 0.029 Uiso 1 1 calc R . . H41B H -0.1881 0.8802 0.2052 0.029 Uiso 1 1 calc R . . C42 C -0.1983(2) 0.79614(11) 0.17029(12) 0.0264(5) Uani 1 1 d . . . H42A H -0.156 0.7735 0.1472 0.032 Uiso 1 1 calc R . . H42B H -0.1985 0.7739 0.2076 0.032 Uiso 1 1 calc R . . C43 C -0.3163(2) 0.80248(12) 0.13131(14) 0.0340(6) Uani 1 1 d . . . H43A H -0.3594 0.8242 0.1546 0.041 Uiso 1 1 calc R . . H43B H -0.3167 0.8252 0.0942 0.041 Uiso 1 1 calc R . . C44 C -0.3711(3) 0.74443(15) 0.1122(2) 0.0609(12) Uani 1 1 d . . . H44A H -0.3338 0.7246 0.0851 0.073 Uiso 1 1 calc R . . H44B H -0.4488 0.7505 0.0906 0.073 Uiso 1 1 calc R . . H44C H -0.366 0.7206 0.1486 0.073 Uiso 1 1 calc R . . C45 C 0.0867(2) 0.91333(10) 0.20123(11) 0.0221(4) Uani 1 1 d U . . H45A H 0.1474 0.9415 0.2161 0.026 Uiso 1 1 calc R . . H45B H 0.0263 0.9337 0.1715 0.026 Uiso 1 1 calc R . . C46 C 0.1283(3) 0.86406(13) 0.16807(15) 0.0391(7) Uani 1 1 d U . . H46A H 0.1677 0.8352 0.1984 0.047 Uiso 1 1 calc R . . H46B H 0.0647 0.8445 0.1399 0.047 Uiso 1 1 calc R . . C47 C 0.2043(3) 0.88631(14) 0.13246(16) 0.0434(7) Uani 1 1 d U . . H47A H 0.2013 0.8601 0.0975 0.052 Uiso 1 1 calc R . . H47B H 0.1793 0.9251 0.1159 0.052 Uiso 1 1 calc R . . C48 C 0.3176(4) 0.89016(18) 0.17015(18) 0.0573(10) Uani 1 1 d U . . H48A H 0.3175 0.909 0.2093 0.069 Uiso 1 1 calc R . . H48B H 0.3595 0.9155 0.1492 0.069 Uiso 1 1 calc R . . C49 C 0.3814(4) 0.8289(2) 0.1850(3) 0.0747(14) Uani 1 1 d U . . H49A H 0.3409 0.8034 0.2059 0.09 Uiso 1 1 calc R . . H49B H 0.4559 0.8355 0.2113 0.09 Uiso 1 1 calc R . . H49C H 0.3859 0.8108 0.1467 0.09 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 0.01737(7) 0.01550(7) 0.01703(7) 0.00068(5) 0.00254(5) -0.00141(6) Si1 0.0195(3) 0.0133(3) 0.0169(3) -0.0008(2) 0.0073(2) -0.0008(2) Si2 0.0146(3) 0.0126(2) 0.0161(3) -0.0009(2) 0.0040(2) -0.0003(2) S1 0.0241(3) 0.0144(2) 0.0180(2) -0.00152(18) 0.0100(2) -0.00052(19) S2 0.0156(2) 0.0137(2) 0.0209(2) -0.00278(18) 0.00403(19) 0.00150(18) S3 0.0170(2) 0.0289(3) 0.0166(2) -0.0002(2) 0.00523(19) 0.0009(2) S4 0.0197(2) 0.0220(3) 0.0178(2) 0.00059(19) 0.00574(19) 0.0019(2) O1 0.0244(8) 0.0231(8) 0.0288(9) -0.0025(7) 0.0124(7) -0.0060(7) O2 0.0253(8) 0.0148(7) 0.0185(7) -0.0024(6) 0.0089(6) 0.0016(6) O3 0.0332(9) 0.0150(7) 0.0177(7) 0.0007(6) 0.0059(7) -0.0003(7) O4 0.0181(7) 0.0151(7) 0.0188(7) -0.0034(6) 0.0062(6) 0.0003(6) O5 0.0183(7) 0.0248(8) 0.0161(7) 0.0005(6) 0.0030(6) 0.0025(6) O6 0.0187(7) 0.0184(7) 0.0218(8) -0.0005(6) 0.0048(6) -0.0063(6) C1 0.0185(11) 0.0222(11) 0.0449(15) -0.0024(10) 0.0104(10) -0.0035(9) C2 0.0306(14) 0.0300(14) 0.0424(16) -0.0094(12) 0.0046(12) -0.0056(11) C3 0.0313(16) 0.058(2) 0.086(3) -0.015(2) 0.0319(18) -0.0142(15) C4 0.0305(15) 0.0325(16) 0.068(2) 0.0100(15) -0.0072(15) 0.0008(12) C5 0.0319(12) 0.0175(10) 0.0236(11) -0.0041(8) 0.0132(9) 0.0016(9) C6 0.0458(16) 0.0289(14) 0.0261(13) -0.0073(10) 0.0034(11) 0.0041(12) C7 0.060(2) 0.0386(17) 0.056(2) -0.0129(14) 0.0444(18) -0.0080(15) C8 0.0470(16) 0.0231(12) 0.0318(13) -0.0030(10) 0.0140(12) 0.0132(11) C9 0.0372(13) 0.0175(10) 0.0180(10) 0.0039(8) 0.0081(9) -0.0005(9) C10 0.0438(16) 0.0254(13) 0.0260(13) 0.0062(10) -0.0017(11) -0.0003(11) C11 0.061(2) 0.0466(19) 0.0415(17) 0.0186(14) 0.0279(16) -0.0020(16) C12 0.0509(17) 0.0168(11) 0.0289(13) -0.0007(9) -0.0011(12) 0.0049(11) C13 0.0237(11) 0.0177(10) 0.0217(10) -0.0044(8) 0.0086(9) 0.0003(8) C14 0.0346(14) 0.0283(13) 0.0296(13) -0.0121(10) 0.0067(11) 0.0013(11) C15 0.0391(15) 0.0223(12) 0.0312(13) -0.0008(10) 0.0095(11) 0.0074(11) C16 0.0377(15) 0.0288(14) 0.0519(18) -0.0101(12) 0.0289(14) -0.0050(11) C17 0.0217(10) 0.0273(12) 0.0162(10) 0.0010(8) 0.0035(8) 0.0057(9) C18 0.0417(15) 0.0314(14) 0.0246(12) 0.0039(10) 0.0107(11) -0.0053(12) C19 0.0348(15) 0.0555(19) 0.0246(13) 0.0066(12) 0.0026(11) 0.0203(14) C20 0.0372(14) 0.0363(15) 0.0204(11) -0.0079(10) 0.0045(10) 0.0038(12) C21 0.0161(10) 0.0187(11) 0.0361(13) 0.0019(9) 0.0033(9) -0.0048(8) C22 0.0294(13) 0.0185(11) 0.0401(15) -0.0040(10) -0.0019(11) -0.0052(10) C23 0.0190(11) 0.0285(14) 0.062(2) 0.0072(13) 0.0103(12) 0.0005(10) C24 0.0299(13) 0.0292(14) 0.0466(17) 0.0093(12) 0.0110(12) -0.0092(11) N1 0.0172(9) 0.0277(10) 0.0184(9) 0.0021(7) 0.0031(7) -0.0009(8) C25 0.0180(10) 0.0176(10) 0.0194(10) 0.0016(8) 0.0051(8) -0.0037(8) C26 0.0192(11) 0.0338(13) 0.0263(12) 0.0054(10) 0.0006(9) 0.0039(10) C27 0.0205(12) 0.0431(16) 0.0384(15) 0.0003(12) 0.0081(11) -0.0047(11) C28 0.0264(12) 0.0337(13) 0.0178(10) -0.0014(9) -0.0001(9) -0.0038(10) C29 0.062(2) 0.0472(18) 0.0225(13) 0.0040(12) 0.0166(13) -0.0071(16) N2 0.0222(9) 0.0152(8) 0.0197(9) 0.0040(7) 0.0061(7) 0.0020(7) C30 0.0266(11) 0.0152(10) 0.0214(10) 0.0015(8) 0.0085(9) 0.0025(8) C31 0.0358(13) 0.0192(11) 0.0264(12) 0.0031(9) 0.0154(10) 0.0010(10) C32 0.0298(12) 0.0190(11) 0.0261(12) -0.0015(9) 0.0116(10) -0.0025(9) C33 0.066(2) 0.0313(15) 0.0376(16) -0.0012(12) 0.0320(16) 0.0012(14) C34 0.071(2) 0.0367(17) 0.0477(19) -0.0050(14) 0.0358(18) 0.0079(16) C35 0.0224(11) 0.0178(10) 0.0234(11) 0.0052(8) 0.0016(9) 0.0028(8) C36 0.0335(13) 0.0257(13) 0.0284(13) 0.0045(10) -0.0029(10) -0.0066(11) C37 0.0259(12) 0.0389(15) 0.0314(13) 0.0005(11) 0.0012(10) -0.0037(11) C38 0.0303(14) 0.0476(18) 0.0279(13) 0.0041(12) -0.0002(11) 0.0013(13) C39 0.0412(18) 0.086(3) 0.0407(19) 0.0216(19) -0.0106(15) -0.0031(19) C40 0.0231(10) 0.0145(9) 0.0212(10) 0.0008(8) 0.0045(8) -0.0002(8) C41 0.0242(11) 0.0195(11) 0.0260(11) 0.0030(9) 0.0024(9) 0.0024(9) C42 0.0306(12) 0.0219(11) 0.0249(12) -0.0028(9) 0.0044(10) 0.0005(10) C43 0.0341(14) 0.0234(13) 0.0389(15) -0.0002(11) -0.0001(12) -0.0024(11) C44 0.052(2) 0.0272(16) 0.080(3) -0.0061(16) -0.0226(19) -0.0066(15) C45 0.0286(12) 0.0168(10) 0.0237(11) 0.0048(8) 0.0120(9) 0.0023(9) C46 0.060(2) 0.0268(13) 0.0404(16) 0.0084(11) 0.0309(15) 0.0148(13) C47 0.056(2) 0.0340(16) 0.0475(18) 0.0079(13) 0.0259(16) 0.0069(14) C48 0.072(3) 0.056(2) 0.0440(19) 0.0083(16) 0.0162(18) -0.029(2) C49 0.050(2) 0.069(3) 0.119(4) -0.006(3) 0.046(3) -0.020(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 2.5103(6) . ? Cd1 S2 2.5113(6) . ? Cd1 S3 2.6586(6) . ? Cd1 S4 2.6801(6) . ? Si1 O3 1.6353(18) . ? Si1 O2 1.6365(17) . ? Si1 O1 1.6377(18) . ? Si1 S1 2.0778(8) . ? Si2 O5 1.6335(17) . ? Si2 O6 1.6362(17) . ? Si2 O4 1.6397(16) . ? Si2 S2 2.0839(8) . ? S3 C25 1.717(2) . ? S4 C25 1.724(2) . ? O1 C1 1.437(3) . ? O2 C5 1.446(3) . ? O3 C9 1.438(3) . ? O4 C13 1.443(3) . ? O5 C17 1.444(3) . ? O6 C21 1.441(3) . ? C1 C2 1.522(4) . ? C1 C3 1.522(4) . ? C1 C4 1.523(4) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C7 1.515(4) . ? C5 C6 1.516(4) . ? C5 C8 1.523(4) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C11 1.515(4) . ? C9 C10 1.518(4) . ? C9 C12 1.528(4) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C16 1.514(3) . ? C13 C14 1.515(3) . ? C13 C15 1.532(4) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.518(4) . ? C17 C20 1.519(3) . ? C17 C19 1.525(3) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.521(4) . ? C21 C24 1.527(4) . ? C21 C23 1.527(4) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? N1 C25 1.342(3) . ? N1 C26 1.468(3) . ? N1 C28 1.471(3) . ? C26 C27 1.520(4) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.519(4) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? N2 C40 1.516(3) . ? N2 C35 1.518(3) . ? N2 C30 1.523(3) . ? N2 C45 1.528(3) . ? C30 C31 1.525(3) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.527(3) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.523(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.514(4) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.516(3) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.529(4) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 C38 1.522(4) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.522(4) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C41 1.517(3) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 C42 1.529(3) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 C43 1.517(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.515(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 C46 1.531(4) . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 C47 1.498(4) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C47 C48 1.455(5) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C48 C49 1.615(6) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? 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 S1 Cd1 S2 127.538(19) . . ? S1 Cd1 S3 104.293(19) . . ? S2 Cd1 S3 117.481(19) . . ? S1 Cd1 S4 116.482(19) . . ? S2 Cd1 S4 108.231(18) . . ? S3 Cd1 S4 67.585(17) . . ? O3 Si1 O2 106.45(9) . . ? O3 Si1 O1 103.38(9) . . ? O2 Si1 O1 112.52(9) . . ? O3 Si1 S1 114.89(7) . . ? O2 Si1 S1 105.07(6) . . ? O1 Si1 S1 114.47(7) . . ? O5 Si2 O6 105.12(9) . . ? O5 Si2 O4 111.55(9) . . ? O6 Si2 O4 105.43(8) . . ? O5 Si2 S2 115.33(7) . . ? O6 Si2 S2 114.07(7) . . ? O4 Si2 S2 105.03(6) . . ? Si1 S1 Cd1 95.13(3) . . ? Si2 S2 Cd1 94.22(3) . . ? C25 S3 Cd1 86.67(8) . . ? C25 S4 Cd1 85.83(8) . . ? C1 O1 Si1 134.05(16) . . ? C5 O2 Si1 132.69(15) . . ? C9 O3 Si1 131.74(15) . . ? C13 O4 Si2 132.34(14) . . ? C17 O5 Si2 133.97(15) . . ? C21 O6 Si2 132.79(16) . . ? O1 C1 C2 108.8(2) . . ? O1 C1 C3 105.4(3) . . ? C2 C1 C3 109.7(2) . . ? O1 C1 C4 111.3(2) . . ? C2 C1 C4 110.7(3) . . ? C3 C1 C4 110.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C7 110.8(2) . . ? O2 C5 C6 108.7(2) . . ? C7 C5 C6 111.2(2) . . ? O2 C5 C8 104.93(19) . . ? C7 C5 C8 111.2(2) . . ? C6 C5 C8 109.7(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C11 108.2(2) . . ? O3 C9 C10 106.0(2) . . ? C11 C9 C10 110.6(2) . . ? O3 C9 C12 111.33(19) . . ? C11 C9 C12 110.9(3) . . ? C10 C9 C12 109.7(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C16 112.02(19) . . ? O4 C13 C14 105.34(19) . . ? C16 C13 C14 110.9(2) . . ? O4 C13 C15 107.90(19) . . ? C16 C13 C15 110.5(2) . . ? C14 C13 C15 110.0(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C18 110.95(19) . . ? O5 C17 C20 109.0(2) . . ? C18 C17 C20 110.5(2) . . ? O5 C17 C19 105.29(19) . . ? C18 C17 C19 110.8(2) . . ? C20 C17 C19 110.2(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 C22 110.3(2) . . ? O6 C21 C24 105.0(2) . . ? C22 C21 C24 110.8(2) . . ? O6 C21 C23 109.7(2) . . ? C22 C21 C23 110.7(2) . . ? C24 C21 C23 110.2(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 N1 C26 122.2(2) . . ? C25 N1 C28 121.7(2) . . ? C26 N1 C28 115.9(2) . . ? N1 C25 S3 120.44(17) . . ? N1 C25 S4 120.29(17) . . ? S3 C25 S4 119.26(13) . . ? N1 C26 C27 112.5(2) . . ? N1 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? N1 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 C29 112.7(2) . . ? N1 C28 H28A 109 . . ? C29 C28 H28A 109 . . ? N1 C28 H28B 109 . . ? C29 C28 H28B 109 . . ? H28A C28 H28B 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C40 N2 C35 105.95(17) . . ? C40 N2 C30 112.02(18) . . ? C35 N2 C30 111.19(18) . . ? C40 N2 C45 111.02(18) . . ? C35 N2 C45 110.66(18) . . ? C30 N2 C45 106.09(16) . . ? N2 C30 C31 114.67(18) . . ? N2 C30 H30A 108.6 . . ? C31 C30 H30A 108.6 . . ? N2 C30 H30B 108.6 . . ? C31 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 C32 109.33(19) . . ? C30 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? C30 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? C33 C32 C31 112.7(2) . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 112.2(3) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N2 116.13(19) . . ? C36 C35 H35A 108.3 . . ? N2 C35 H35A 108.3 . . ? C36 C35 H35B 108.3 . . ? N2 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? C35 C36 C37 110.3(2) . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? C35 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 114.5(2) . . ? C38 C37 H37A 108.6 . . ? C36 C37 H37A 108.6 . . ? C38 C37 H37B 108.6 . . ? C36 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? C39 C38 C37 112.7(3) . . ? C39 C38 H38A 109 . . ? C37 C38 H38A 109 . . ? C39 C38 H38B 109 . . ? C37 C38 H38B 109 . . ? H38A C38 H38B 107.8 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C40 C41 116.36(18) . . ? N2 C40 H40A 108.2 . . ? C41 C40 H40A 108.2 . . ? N2 C40 H40B 108.2 . . ? C41 C40 H40B 108.2 . . ? H40A C40 H40B 107.3 . . ? C40 C41 C42 108.77(19) . . ? C40 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? C40 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? C43 C42 C41 113.6(2) . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42B 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 112.4(2) . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? C42 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N2 C45 C46 114.55(19) . . ? N2 C45 H45A 108.6 . . ? C46 C45 H45A 108.6 . . ? N2 C45 H45B 108.6 . . ? C46 C45 H45B 108.6 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 111.3(3) . . ? C47 C46 H46A 109.4 . . ? C45 C46 H46A 109.4 . . ? C47 C46 H46B 109.4 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 108 . . ? C48 C47 C46 111.7(3) . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? C47 C48 C49 115.0(3) . . ? C47 C48 H48A 108.5 . . ? C49 C48 H48A 108.5 . . ? C47 C48 H48B 108.5 . . ? C49 C48 H48B 108.5 . . ? H48A C48 H48B 107.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? #===END