# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email r.bedford@bristol.ac.uk _publ_contact_author_name 'Robin Bedford' loop_ _publ_author_name R.Bedford 'Yu-Ning Chang' M.Haddow C.McMullin data_3b _database_code_depnum_ccdc_archive 'CCDC 815801' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H51 Cl O6 P2 Pd, C4 H10 O' _chemical_formula_sum 'C62 H61 Cl O7 P2 Pd' _chemical_formula_weight 1121.90 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.1839(5) _cell_length_b 15.9875(6) _cell_length_c 22.2064(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5390.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46309 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.61 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.61 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.6509 _exptl_absorpt_correction_T_max 0.9278 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46257 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.61 _reflns_number_total 6267 _reflns_number_gt 5920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+3.1865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(15) _refine_ls_number_reflns 6267 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.298567(12) 0.0000 0.5000 0.01386(5) Uani 1 2 d S . . P1 P 0.27129(3) 0.11492(3) 0.44453(2) 0.01478(10) Uani 1 1 d . . . Cl1 Cl 0.45402(4) 0.0000 0.5000 0.02696(14) Uani 1 2 d S . . O1 O 0.16701(9) 0.11789(9) 0.43361(6) 0.0178(3) Uani 1 1 d . . . O2 O 0.29791(9) 0.20152(8) 0.47485(6) 0.0157(3) Uani 1 1 d . . . O3 O 0.29845(10) 0.12690(8) 0.37555(6) 0.0167(3) Uani 1 1 d . . . C1 C 0.16579(16) 0.0000 0.5000 0.0162(4) Uani 1 2 d S . . C2 C 0.11849(13) 0.05838(12) 0.46690(8) 0.0152(4) Uani 1 1 d . . . C3 C 0.02708(13) 0.05888(13) 0.46351(8) 0.0161(4) Uani 1 1 d . . . C4 C -0.01507(16) 0.0000 0.5000 0.0168(5) Uani 1 2 d S . . H4 H -0.0776 0.0000 0.5000 0.020 Uiso 1 2 calc SR . . C5 C -0.02443(13) 0.11805(13) 0.42143(9) 0.0192(4) Uani 1 1 d . . . C6 C 0.00301(14) 0.10129(15) 0.35580(9) 0.0240(5) Uani 1 1 d . . . H6A H -0.0102 0.0430 0.3454 0.036 Uiso 1 1 calc R . . H6B H 0.0663 0.1114 0.3513 0.036 Uiso 1 1 calc R . . H6C H -0.0297 0.1387 0.3289 0.036 Uiso 1 1 calc R . . C7 C -0.00768(16) 0.21038(14) 0.43801(11) 0.0292(5) Uani 1 1 d . . . H7A H 0.0550 0.2232 0.4331 0.044 Uiso 1 1 calc R . . H7B H -0.0250 0.2200 0.4800 0.044 Uiso 1 1 calc R . . H7C H -0.0425 0.2466 0.4115 0.044 Uiso 1 1 calc R . . C8 C -0.12366(14) 0.10262(15) 0.42567(10) 0.0250(5) Uani 1 1 d . . . H8A H -0.1546 0.1407 0.3983 0.038 Uiso 1 1 calc R . . H8B H -0.1435 0.1127 0.4670 0.038 Uiso 1 1 calc R . . H8C H -0.1365 0.0446 0.4144 0.038 Uiso 1 1 calc R . . C9 C 0.27683(12) 0.27675(12) 0.44437(9) 0.0147(4) Uani 1 1 d . . . C10 C 0.20704(14) 0.32471(12) 0.46920(9) 0.0167(4) Uani 1 1 d . . . C11 C 0.18475(12) 0.39660(13) 0.43942(9) 0.0172(4) Uani 1 1 d . . . H11 H 0.1387 0.4305 0.4549 0.021 Uiso 1 1 calc R . . C12 C 0.22841(13) 0.42186(12) 0.38617(9) 0.0158(4) Uani 1 1 d . . . C13 C 0.20192(12) 0.49508(16) 0.35509(8) 0.0198(3) Uani 1 1 d . . . H13 H 0.1548 0.5278 0.3705 0.024 Uiso 1 1 calc R . . C14 C 0.24325(14) 0.51941(12) 0.30319(9) 0.0198(4) Uani 1 1 d . . . H14 H 0.2253 0.5691 0.2832 0.024 Uiso 1 1 calc R . . C15 C 0.31227(14) 0.47083(13) 0.27948(9) 0.0193(4) Uani 1 1 d . . . H15 H 0.3402 0.4875 0.2431 0.023 Uiso 1 1 calc R . . C16 C 0.33967(13) 0.39970(13) 0.30836(9) 0.0168(4) Uani 1 1 d . . . H16 H 0.3862 0.3675 0.2916 0.020 Uiso 1 1 calc R . . C17 C 0.29964(13) 0.37332(11) 0.36304(8) 0.0145(3) Uani 1 1 d . . . C18 C 0.32512(12) 0.29858(12) 0.39459(8) 0.0145(4) Uani 1 1 d . . . C19 C 0.39799(13) 0.24354(12) 0.37262(8) 0.0141(4) Uani 1 1 d . . . C20 C 0.48492(13) 0.27433(12) 0.36176(8) 0.0142(4) Uani 1 1 d . . . C21 C 0.51300(13) 0.35558(13) 0.37816(8) 0.0165(4) Uani 1 1 d . . . H21 H 0.4725 0.3925 0.3971 0.020 Uiso 1 1 calc R . . C22 C 0.59722(13) 0.38211(13) 0.36730(9) 0.0191(4) Uani 1 1 d . . . H22 H 0.6147 0.4367 0.3793 0.023 Uiso 1 1 calc R . . C23 C 0.65821(14) 0.32898(14) 0.33837(9) 0.0205(4) Uani 1 1 d . . . H23 H 0.7162 0.3481 0.3302 0.025 Uiso 1 1 calc R . . C24 C 0.63369(14) 0.25007(13) 0.32212(9) 0.0192(4) Uani 1 1 d . . . H24 H 0.6749 0.2149 0.3022 0.023 Uiso 1 1 calc R . . C25 C 0.54798(13) 0.21944(13) 0.33428(8) 0.0162(4) Uani 1 1 d . . . C26 C 0.52454(13) 0.13590(13) 0.32225(8) 0.0173(4) Uani 1 1 d . . . H26 H 0.5660 0.1008 0.3026 0.021 Uiso 1 1 calc R . . C27 C 0.44431(14) 0.10334(13) 0.33781(8) 0.0165(4) Uani 1 1 d . . . C28 C 0.38263(13) 0.15976(12) 0.36285(8) 0.0153(4) Uani 1 1 d . . . C29 C 0.16290(15) 0.29910(15) 0.52698(9) 0.0222(4) Uani 1 1 d . . . H29A H 0.1125 0.3359 0.5347 0.033 Uiso 1 1 calc R . . H29B H 0.2050 0.3036 0.5603 0.033 Uiso 1 1 calc R . . H29C H 0.1425 0.2411 0.5236 0.033 Uiso 1 1 calc R . . C30 C 0.42224(14) 0.01198(14) 0.32987(9) 0.0228(5) Uani 1 1 d . . . H30A H 0.4723 -0.0169 0.3114 0.034 Uiso 1 1 calc R . . H30B H 0.3705 0.0065 0.3038 0.034 Uiso 1 1 calc R . . H30C H 0.4096 -0.0130 0.3692 0.034 Uiso 1 1 calc R . . O4 O 1.0000 0.26211(17) 0.2500 0.0379(6) Uani 1 2 d S . . C31 C 0.9181(5) 0.3032(4) 0.2543(3) 0.0388(16) Uani 0.50 1 d P A -1 H31A H 0.9221 0.3585 0.2345 0.047 Uiso 0.50 1 calc PR A -1 H31B H 0.9034 0.3122 0.2972 0.047 Uiso 0.50 1 calc PR A -1 C32 C 0.8484(12) 0.2542(13) 0.2258(6) 0.041(3) Uani 0.50 1 d P A -1 H32A H 0.8612 0.2478 0.1828 0.062 Uiso 0.50 1 calc PR A -1 H32B H 0.7919 0.2831 0.2308 0.062 Uiso 0.50 1 calc PR A -1 H32C H 0.8452 0.1989 0.2447 0.062 Uiso 0.50 1 calc PR A -1 C33 C 1.0738(5) 0.2987(5) 0.2739(3) 0.0402(16) Uani 0.50 1 d P A -1 H33A H 1.0678 0.3030 0.3182 0.048 Uiso 0.50 1 calc PR A -1 H33B H 1.0808 0.3559 0.2574 0.048 Uiso 0.50 1 calc PR A -1 C34 C 1.1557(11) 0.2449(13) 0.2578(5) 0.037(3) Uani 0.50 1 d P A -1 H34A H 1.1482 0.1883 0.2739 0.055 Uiso 0.50 1 calc PR A -1 H34B H 1.2085 0.2704 0.2754 0.055 Uiso 0.50 1 calc PR A -1 H34C H 1.1622 0.2422 0.2139 0.055 Uiso 0.50 1 calc PR A -1 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 Pd1 0.01197(9) 0.01228(9) 0.01733(9) 0.00253(9) 0.000 0.000 P1 0.0149(2) 0.0126(2) 0.0169(2) 0.00163(19) -0.00063(18) -0.00069(18) Cl1 0.0135(3) 0.0392(4) 0.0282(3) 0.0068(5) 0.000 0.000 O1 0.0149(7) 0.0148(7) 0.0238(7) 0.0052(6) -0.0017(5) -0.0023(6) O2 0.0177(6) 0.0144(7) 0.0150(5) 0.0022(5) -0.0006(5) -0.0010(6) O3 0.0189(7) 0.0156(7) 0.0157(6) 0.0008(5) 0.0003(6) -0.0021(6) C1 0.0151(11) 0.0150(11) 0.0185(11) -0.0040(15) 0.000 0.000 C2 0.0161(9) 0.0136(9) 0.0158(9) -0.0004(7) -0.0003(7) -0.0007(7) C3 0.0159(10) 0.0140(9) 0.0185(9) -0.0043(7) -0.0019(7) 0.0020(7) C4 0.0137(11) 0.0163(12) 0.0203(11) -0.0049(15) 0.000 0.000 C5 0.0165(10) 0.0154(10) 0.0259(10) 0.0002(8) -0.0042(8) 0.0021(8) C6 0.0214(11) 0.0279(12) 0.0226(10) 0.0063(9) -0.0046(8) -0.0001(9) C7 0.0265(12) 0.0164(11) 0.0445(14) -0.0001(10) -0.0114(10) 0.0053(9) C8 0.0147(10) 0.0278(12) 0.0326(12) 0.0040(9) -0.0051(9) 0.0026(9) C9 0.0162(10) 0.0118(9) 0.0160(8) 0.0003(7) -0.0007(7) -0.0002(7) C10 0.0132(9) 0.0181(10) 0.0190(9) -0.0030(7) 0.0008(8) -0.0038(8) C11 0.0119(9) 0.0195(10) 0.0204(9) -0.0055(8) 0.0012(7) 0.0009(7) C12 0.0150(9) 0.0140(9) 0.0184(9) -0.0026(7) -0.0021(7) 0.0013(7) C13 0.0188(8) 0.0182(9) 0.0225(8) -0.0024(9) -0.0033(7) 0.0046(12) C14 0.0234(10) 0.0117(11) 0.0242(9) 0.0021(7) -0.0066(8) 0.0030(7) C15 0.0220(11) 0.0179(9) 0.0181(9) 0.0025(7) -0.0017(8) -0.0002(7) C16 0.0184(10) 0.0160(10) 0.0160(9) -0.0007(7) 0.0000(7) 0.0011(8) C17 0.0146(8) 0.0133(9) 0.0156(8) -0.0015(7) -0.0005(8) 0.0010(8) C18 0.0154(9) 0.0121(9) 0.0161(9) -0.0029(7) -0.0003(7) -0.0007(7) C19 0.0175(10) 0.0129(9) 0.0119(8) 0.0014(7) -0.0004(7) 0.0038(7) C20 0.0164(9) 0.0156(10) 0.0107(8) 0.0022(7) 0.0014(7) 0.0034(8) C21 0.0185(10) 0.0165(10) 0.0145(9) 0.0018(7) 0.0021(7) 0.0045(8) C22 0.0207(10) 0.0190(11) 0.0177(9) 0.0015(8) 0.0005(8) -0.0002(8) C23 0.0146(10) 0.0254(11) 0.0214(10) 0.0048(8) 0.0016(8) 0.0009(8) C24 0.0190(10) 0.0228(11) 0.0157(9) 0.0036(8) 0.0055(8) 0.0070(8) C25 0.0194(10) 0.0187(10) 0.0104(8) 0.0033(7) -0.0009(7) 0.0057(8) C26 0.0214(10) 0.0188(10) 0.0118(8) 0.0014(7) 0.0002(7) 0.0088(8) C27 0.0249(11) 0.0125(10) 0.0121(9) -0.0003(7) -0.0038(7) 0.0035(8) C28 0.0184(10) 0.0163(9) 0.0111(8) 0.0018(7) -0.0011(7) 0.0006(8) C29 0.0213(11) 0.0256(12) 0.0197(9) -0.0008(9) 0.0059(8) -0.0036(9) C30 0.0314(11) 0.0138(12) 0.0233(9) -0.0018(8) -0.0005(8) 0.0046(9) O4 0.0308(15) 0.0379(15) 0.0450(15) 0.000 0.0016(11) 0.000 C31 0.056(4) 0.026(3) 0.034(3) -0.001(3) 0.010(4) 0.013(3) C32 0.039(4) 0.051(5) 0.033(7) 0.024(6) 0.014(5) 0.021(3) C33 0.053(4) 0.032(3) 0.036(4) -0.008(3) 0.013(4) -0.018(3) C34 0.021(4) 0.065(7) 0.025(6) -0.017(5) 0.008(4) -0.017(4) _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 Pd1 C1 2.016(2) . ? Pd1 P1 2.2504(5) . ? Pd1 P1 2.2504(5) 4_556 ? Pd1 Cl1 2.3604(6) . ? P1 O2 1.5918(14) . ? P1 O3 1.5979(13) . ? P1 O1 1.6026(15) . ? O1 C2 1.412(2) . ? O2 C9 1.417(2) . ? O3 C28 1.410(2) . ? C1 C2 1.388(2) 4_556 ? C1 C2 1.388(2) . ? C2 C3 1.390(3) . ? C3 C4 1.397(2) . ? C3 C5 1.543(3) . ? C4 C3 1.397(2) 4_556 ? C4 H4 0.9500 . ? C5 C8 1.530(3) . ? C5 C6 1.539(3) . ? C5 C7 1.542(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C18 1.372(3) . ? C9 C10 1.419(3) . ? C10 C11 1.369(3) . ? C10 C29 1.504(3) . ? C11 C12 1.415(3) . ? C11 H11 0.9500 . ? C12 C13 1.417(3) . ? C12 C17 1.427(3) . ? C13 C14 1.369(3) . ? C13 H13 0.9500 . ? C14 C15 1.407(3) . ? C14 H14 0.9500 . ? C15 C16 1.370(3) . ? C15 H15 0.9500 . ? C16 C17 1.422(3) . ? C16 H16 0.9500 . ? C17 C18 1.438(3) . ? C18 C19 1.495(3) . ? C19 C28 1.377(3) . ? C19 C20 1.429(3) . ? C20 C21 1.415(3) . ? C20 C25 1.435(3) . ? C21 C22 1.369(3) . ? C21 H21 0.9500 . ? C22 C23 1.411(3) . ? C22 H22 0.9500 . ? C23 C24 1.364(3) . ? C23 H23 0.9500 . ? C24 C25 1.416(3) . ? C24 H24 0.9500 . ? C25 C26 1.408(3) . ? C26 C27 1.369(3) . ? C26 H26 0.9500 . ? C27 C28 1.414(3) . ? C27 C30 1.509(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O4 C33 1.371(7) 3_755 ? O4 C33 1.371(7) . ? O4 C31 1.409(7) 3_755 ? O4 C31 1.409(7) . ? C31 C32 1.46(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.555(18) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 79.396(14) . . ? C1 Pd1 P1 79.396(14) . 4_556 ? P1 Pd1 P1 158.79(3) . 4_556 ? C1 Pd1 Cl1 180.0 . . ? P1 Pd1 Cl1 100.604(14) . . ? P1 Pd1 Cl1 100.604(14) 4_556 . ? O2 P1 O3 103.63(7) . . ? O2 P1 O1 106.80(8) . . ? O3 P1 O1 96.10(7) . . ? O2 P1 Pd1 115.59(5) . . ? O3 P1 Pd1 125.11(6) . . ? O1 P1 Pd1 106.79(6) . . ? C2 O1 P1 114.60(12) . . ? C9 O2 P1 118.62(12) . . ? C28 O3 P1 118.05(12) . . ? C2 C1 C2 117.7(2) 4_556 . ? C2 C1 Pd1 121.15(12) 4_556 . ? C2 C1 Pd1 121.15(12) . . ? C1 C2 C3 123.30(19) . . ? C1 C2 O1 117.40(18) . . ? C3 C2 O1 119.26(17) . . ? C2 C3 C4 114.97(18) . . ? C2 C3 C5 122.85(18) . . ? C4 C3 C5 122.16(18) . . ? C3 C4 C3 125.5(2) . 4_556 ? C3 C4 H4 117.3 . . ? C3 C4 H4 117.3 4_556 . ? C8 C5 C6 107.26(17) . . ? C8 C5 C7 107.58(18) . . ? C6 C5 C7 110.36(19) . . ? C8 C5 C3 111.30(17) . . ? C6 C5 C3 109.24(16) . . ? C7 C5 C3 111.03(17) . . ? 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 . . ? C18 C9 O2 118.70(17) . . ? C18 C9 C10 125.08(18) . . ? O2 C9 C10 116.22(16) . . ? C11 C10 C9 116.78(18) . . ? C11 C10 C29 122.04(19) . . ? C9 C10 C29 121.12(18) . . ? C10 C11 C12 121.86(18) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 120.65(18) . . ? C11 C12 C17 120.06(18) . . ? C13 C12 C17 119.29(18) . . ? C14 C13 C12 120.97(19) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.99(18) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.61(19) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.07(19) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C12 118.04(17) . . ? C16 C17 C18 123.19(17) . . ? C12 C17 C18 118.72(17) . . ? C9 C18 C17 117.39(17) . . ? C9 C18 C19 120.58(17) . . ? C17 C18 C19 121.94(17) . . ? C28 C19 C20 117.70(18) . . ? C28 C19 C18 119.90(18) . . ? C20 C19 C18 122.40(18) . . ? C21 C20 C19 123.43(18) . . ? C21 C20 C25 118.02(18) . . ? C19 C20 C25 118.52(18) . . ? C22 C21 C20 121.37(19) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 120.4(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.87(19) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.33(19) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 121.61(18) . . ? C26 C25 C20 119.48(18) . . ? C24 C25 C20 118.87(19) . . ? C27 C26 C25 122.53(18) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C28 116.49(19) . . ? C26 C27 C30 122.42(18) . . ? C28 C27 C30 121.08(19) . . ? C19 C28 O3 118.97(17) . . ? C19 C28 C27 124.77(19) . . ? O3 C28 C27 116.19(17) . . ? C10 C29 H29A 109.5 . . ? C10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 O4 C33 129.4(7) 3_755 . ? C33 O4 C31 119.7(4) 3_755 3_755 ? C33 O4 C31 26.7(3) . 3_755 ? C33 O4 C31 26.7(3) 3_755 . ? C33 O4 C31 119.7(4) . . ? C31 O4 C31 124.5(6) 3_755 . ? O4 C31 C32 111.2(9) . . ? O4 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? O4 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? O4 C33 C34 109.2(7) . . ? O4 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O4 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P1 O2 112.09(6) . . . . ? P1 Pd1 P1 O2 112.10(6) 4_556 . . . ? Cl1 Pd1 P1 O2 -67.91(6) . . . . ? C1 Pd1 P1 O3 -116.91(7) . . . . ? P1 Pd1 P1 O3 -116.90(7) 4_556 . . . ? Cl1 Pd1 P1 O3 63.09(7) . . . . ? C1 Pd1 P1 O1 -6.55(6) . . . . ? P1 Pd1 P1 O1 -6.54(6) 4_556 . . . ? Cl1 Pd1 P1 O1 173.45(6) . . . . ? O2 P1 O1 C2 -115.64(13) . . . . ? O3 P1 O1 C2 138.10(13) . . . . ? Pd1 P1 O1 C2 8.57(14) . . . . ? O3 P1 O2 C9 43.93(15) . . . . ? O1 P1 O2 C9 -56.87(15) . . . . ? Pd1 P1 O2 C9 -175.51(11) . . . . ? O2 P1 O3 C28 47.43(14) . . . . ? O1 P1 O3 C28 156.40(13) . . . . ? Pd1 P1 O3 C28 -88.12(13) . . . . ? P1 Pd1 C1 C2 -175.61(9) . . . 4_556 ? P1 Pd1 C1 C2 4.39(9) 4_556 . . 4_556 ? Cl1 Pd1 C1 C2 0(93) . . . 4_556 ? P1 Pd1 C1 C2 4.38(9) . . . . ? P1 Pd1 C1 C2 -175.61(9) 4_556 . . . ? Cl1 Pd1 C1 C2 0(25) . . . . ? C2 C1 C2 C3 -2.68(13) 4_556 . . . ? Pd1 C1 C2 C3 177.33(13) . . . . ? C2 C1 C2 O1 179.63(18) 4_556 . . . ? Pd1 C1 C2 O1 -0.36(18) . . . . ? P1 O1 C2 C1 -6.0(2) . . . . ? P1 O1 C2 C3 176.18(14) . . . . ? C1 C2 C3 C4 5.0(2) . . . . ? O1 C2 C3 C4 -177.39(14) . . . . ? C1 C2 C3 C5 -173.39(15) . . . . ? O1 C2 C3 C5 4.3(3) . . . . ? C2 C3 C4 C3 -2.36(12) . . . 4_556 ? C5 C3 C4 C3 176.01(19) . . . 4_556 ? C2 C3 C5 C8 178.07(19) . . . . ? C4 C3 C5 C8 -0.2(3) . . . . ? C2 C3 C5 C6 59.8(2) . . . . ? C4 C3 C5 C6 -118.42(18) . . . . ? C2 C3 C5 C7 -62.1(3) . . . . ? C4 C3 C5 C7 119.65(19) . . . . ? P1 O2 C9 C18 -73.9(2) . . . . ? P1 O2 C9 C10 107.21(17) . . . . ? C18 C9 C10 C11 2.5(3) . . . . ? O2 C9 C10 C11 -178.61(16) . . . . ? C18 C9 C10 C29 -174.83(19) . . . . ? O2 C9 C10 C29 4.0(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C29 C10 C11 C12 177.87(18) . . . . ? C10 C11 C12 C13 177.78(19) . . . . ? C10 C11 C12 C17 -1.9(3) . . . . ? C11 C12 C13 C14 -179.29(19) . . . . ? C17 C12 C13 C14 0.4(3) . . . . ? C12 C13 C14 C15 0.9(3) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C14 C15 C16 C17 -0.3(3) . . . . ? C15 C16 C17 C12 1.7(3) . . . . ? C15 C16 C17 C18 179.07(18) . . . . ? C11 C12 C17 C16 178.03(18) . . . . ? C13 C12 C17 C16 -1.7(3) . . . . ? C11 C12 C17 C18 0.5(3) . . . . ? C13 C12 C17 C18 -179.22(17) . . . . ? O2 C9 C18 C17 177.28(16) . . . . ? C10 C9 C18 C17 -3.9(3) . . . . ? O2 C9 C18 C19 0.6(3) . . . . ? C10 C9 C18 C19 179.41(18) . . . . ? C16 C17 C18 C9 -175.15(18) . . . . ? C12 C17 C18 C9 2.2(3) . . . . ? C16 C17 C18 C19 1.5(3) . . . . ? C12 C17 C18 C19 178.87(17) . . . . ? C9 C18 C19 C28 51.5(3) . . . . ? C17 C18 C19 C28 -125.0(2) . . . . ? C9 C18 C19 C20 -127.7(2) . . . . ? C17 C18 C19 C20 55.8(3) . . . . ? C28 C19 C20 C21 -170.48(18) . . . . ? C18 C19 C20 C21 8.8(3) . . . . ? C28 C19 C20 C25 7.8(3) . . . . ? C18 C19 C20 C25 -173.01(17) . . . . ? C19 C20 C21 C22 179.44(18) . . . . ? C25 C20 C21 C22 1.2(3) . . . . ? C20 C21 C22 C23 1.0(3) . . . . ? C21 C22 C23 C24 -1.3(3) . . . . ? C22 C23 C24 C25 -0.7(3) . . . . ? C23 C24 C25 C26 -174.57(19) . . . . ? C23 C24 C25 C20 2.9(3) . . . . ? C21 C20 C25 C26 174.45(17) . . . . ? C19 C20 C25 C26 -3.9(3) . . . . ? C21 C20 C25 C24 -3.1(3) . . . . ? C19 C20 C25 C24 178.58(17) . . . . ? C24 C25 C26 C27 174.95(18) . . . . ? C20 C25 C26 C27 -2.5(3) . . . . ? C25 C26 C27 C28 4.6(3) . . . . ? C25 C26 C27 C30 -174.46(18) . . . . ? C20 C19 C28 O3 177.42(15) . . . . ? C18 C19 C28 O3 -1.8(3) . . . . ? C20 C19 C28 C27 -5.9(3) . . . . ? C18 C19 C28 C27 174.87(17) . . . . ? P1 O3 C28 C19 -73.6(2) . . . . ? P1 O3 C28 C27 109.46(16) . . . . ? C26 C27 C28 C19 -0.3(3) . . . . ? C30 C27 C28 C19 178.78(18) . . . . ? C26 C27 C28 O3 176.46(16) . . . . ? C30 C27 C28 O3 -4.4(3) . . . . ? C33 O4 C31 C32 60.1(11) 3_755 . . . ? C33 O4 C31 C32 179.6(7) . . . . ? C31 O4 C31 C32 148.5(7) 3_755 . . . ? C33 O4 C33 C34 -144.3(9) 3_755 . . . ? C31 O4 C33 C34 -66.3(13) 3_755 . . . ? C31 O4 C33 C34 -174.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.835 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.054 data_6dsqueeze _database_code_depnum_ccdc_archive 'CCDC 815802' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H50 O4 Si2' _chemical_formula_sum 'C60 H50 O4 Si2' _chemical_formula_weight 891.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9481(4) _cell_length_b 17.2684(6) _cell_length_c 31.2989(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5376.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8612 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.13 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12378 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.56 _reflns_number_total 12378 _reflns_number_gt 9896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.002 0.250 0.000 435 110 ' ' 2 -0.044 0.750 0.500 435 110 ' ' _platon_squeeze_details ; Solvents used in recrystallisation were dichloromethane and diethyl ether. It was not possible to identify the solvent from the residual electron density map. The electron count suggested by SQUEEZE suggests an extra four molecule of dichloromethane or diethylether per unit cell. ; _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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.23(11) _refine_ls_number_reflns 12378 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.62002(7) 0.61770(4) 0.11346(2) 0.02264(15) Uani 1 1 d . . . Si2 Si 0.97072(7) 0.50677(4) 0.36095(2) 0.02530(16) Uani 1 1 d . . . O1 O 0.83570(19) 0.60768(11) 0.17554(5) 0.0284(4) Uani 1 1 d . . . O2 O 0.9882(2) 0.65082(13) 0.22701(7) 0.0454(6) Uani 1 1 d . . . O3 O 0.78596(17) 0.50474(11) 0.28807(6) 0.0275(4) Uani 1 1 d . . . O4 O 0.5708(2) 0.47582(14) 0.30671(8) 0.0467(6) Uani 1 1 d . . . C1 C 0.7875(2) 0.53294(15) 0.17140(8) 0.0231(5) Uani 1 1 d . . . C2 C 0.6911(2) 0.52696(15) 0.13819(8) 0.0227(5) Uani 1 1 d . . . C3 C 0.6431(3) 0.45464(16) 0.12809(8) 0.0266(6) Uani 1 1 d . . . H3 H 0.5782 0.4495 0.1060 0.032 Uiso 1 1 calc R . . C4 C 0.6880(3) 0.38756(16) 0.14976(8) 0.0266(5) Uani 1 1 d . . . C5 C 0.6400(3) 0.31275(16) 0.13906(9) 0.0343(6) Uani 1 1 d . . . H5 H 0.5758 0.3075 0.1168 0.041 Uiso 1 1 calc R . . C6 C 0.6831(3) 0.24887(17) 0.15967(10) 0.0362(7) Uani 1 1 d . . . H6 H 0.6488 0.1994 0.1521 0.043 Uiso 1 1 calc R . . C7 C 0.7795(3) 0.25568(17) 0.19262(10) 0.0376(7) Uani 1 1 d . . . H7 H 0.8112 0.2107 0.2069 0.045 Uiso 1 1 calc R . . C8 C 0.8266(3) 0.32650(17) 0.20385(9) 0.0327(6) Uani 1 1 d . . . H8 H 0.8917 0.3303 0.2260 0.039 Uiso 1 1 calc R . . C9 C 0.7812(3) 0.39529(16) 0.18347(8) 0.0280(6) Uani 1 1 d . . . C10 C 0.8309(3) 0.46980(15) 0.19482(8) 0.0247(5) Uani 1 1 d . . . C11 C 0.9370(3) 0.47498(15) 0.22871(8) 0.0252(5) Uani 1 1 d . . . C12 C 1.0746(3) 0.46376(16) 0.21572(8) 0.0266(6) Uani 1 1 d . . . C13 C 1.1099(3) 0.44996(16) 0.17240(8) 0.0296(6) Uani 1 1 d . . . H13 H 1.0415 0.4483 0.1512 0.036 Uiso 1 1 calc R . . C14 C 1.2409(3) 0.43905(16) 0.16082(9) 0.0319(6) Uani 1 1 d . . . H14 H 1.2624 0.4295 0.1317 0.038 Uiso 1 1 calc R . . C15 C 1.3435(3) 0.44168(17) 0.19105(10) 0.0345(7) Uani 1 1 d . . . H15 H 1.4343 0.4339 0.1827 0.041 Uiso 1 1 calc R . . C16 C 1.3122(3) 0.45564(16) 0.23324(9) 0.0319(6) Uani 1 1 d . . . H16 H 1.3823 0.4576 0.2538 0.038 Uiso 1 1 calc R . . C17 C 1.1787(3) 0.46698(15) 0.24632(8) 0.0266(5) Uani 1 1 d . . . C18 C 1.1455(3) 0.48044(16) 0.28977(8) 0.0268(6) Uani 1 1 d . . . H18 H 1.2158 0.4828 0.3103 0.032 Uiso 1 1 calc R . . C19 C 1.0151(3) 0.49021(15) 0.30310(8) 0.0255(5) Uani 1 1 d . . . C20 C 0.9119(2) 0.48775(15) 0.27137(8) 0.0240(5) Uani 1 1 d . . . C21 C 0.8553(3) 0.64303(19) 0.21632(10) 0.0387(7) Uani 1 1 d . . . H21A H 0.8127 0.6948 0.2162 0.046 Uiso 1 1 calc R . . H21B H 0.8098 0.6114 0.2384 0.046 Uiso 1 1 calc R . . C22 C 1.0607(5) 0.6997(3) 0.19745(13) 0.0809(15) Uani 1 1 d . . . H22A H 1.0525 0.6786 0.1685 0.121 Uiso 1 1 calc R . . H22B H 1.1557 0.7016 0.2056 0.121 Uiso 1 1 calc R . . H22C H 1.0230 0.7521 0.1982 0.121 Uiso 1 1 calc R . . C23 C 0.6633(3) 0.4698(2) 0.27420(10) 0.0412(7) Uani 1 1 d . . . H23A H 0.6295 0.4963 0.2483 0.049 Uiso 1 1 calc R . . H23B H 0.6787 0.4146 0.2671 0.049 Uiso 1 1 calc R . . C24 C 0.5305(4) 0.5514(2) 0.31589(13) 0.0519(9) Uani 1 1 d . . . H24A H 0.6064 0.5803 0.3278 0.078 Uiso 1 1 calc R . . H24B H 0.4568 0.5503 0.3367 0.078 Uiso 1 1 calc R . . H24C H 0.4998 0.5767 0.2896 0.078 Uiso 1 1 calc R . . C25 C 0.7397(3) 0.67143(15) 0.07861(8) 0.0248(5) Uani 1 1 d . . . C26 C 0.8795(3) 0.66017(18) 0.07879(9) 0.0338(6) Uani 1 1 d . . . H26 H 0.9164 0.6192 0.0953 0.041 Uiso 1 1 calc R . . C27 C 0.9649(3) 0.70747(19) 0.05535(10) 0.0412(7) Uani 1 1 d . . . H27 H 1.0593 0.6993 0.0561 0.049 Uiso 1 1 calc R . . C28 C 0.9118(3) 0.76622(18) 0.03103(9) 0.0366(7) Uani 1 1 d . . . H28 H 0.9704 0.7989 0.0153 0.044 Uiso 1 1 calc R . . C29 C 0.7760(3) 0.77839(17) 0.02913(8) 0.0318(6) Uani 1 1 d . . . H29 H 0.7405 0.8188 0.0119 0.038 Uiso 1 1 calc R . . C30 C 0.6903(3) 0.73105(16) 0.05262(8) 0.0283(6) Uani 1 1 d . . . H30 H 0.5960 0.7393 0.0510 0.034 Uiso 1 1 calc R . . C31 C 0.4714(3) 0.58812(15) 0.08062(8) 0.0254(5) Uani 1 1 d . . . C32 C 0.4881(3) 0.55894(19) 0.03928(9) 0.0367(7) Uani 1 1 d . . . H32 H 0.5755 0.5567 0.0271 0.044 Uiso 1 1 calc R . . C33 C 0.3779(4) 0.5330(2) 0.01563(10) 0.0470(8) Uani 1 1 d . . . H33 H 0.3907 0.5142 -0.0126 0.056 Uiso 1 1 calc R . . C34 C 0.2516(3) 0.53451(19) 0.03290(10) 0.0405(7) Uani 1 1 d . . . H34 H 0.1774 0.5155 0.0170 0.049 Uiso 1 1 calc R . . C35 C 0.2320(3) 0.56357(18) 0.07333(10) 0.0374(7) Uani 1 1 d . . . H35 H 0.1440 0.5651 0.0850 0.045 Uiso 1 1 calc R . . C36 C 0.3389(3) 0.59035(16) 0.09693(9) 0.0312(6) Uani 1 1 d . . . H36 H 0.3235 0.6107 0.1247 0.037 Uiso 1 1 calc R . . C37 C 0.5656(3) 0.68269(17) 0.15830(8) 0.0271(6) Uani 1 1 d . . . C38 C 0.6030(3) 0.75982(17) 0.15919(9) 0.0346(6) Uani 1 1 d . . . H38 H 0.6524 0.7807 0.1359 0.041 Uiso 1 1 calc R . . C39 C 0.5698(4) 0.8072(2) 0.19327(10) 0.0468(8) Uani 1 1 d . . . H39 H 0.5963 0.8601 0.1933 0.056 Uiso 1 1 calc R . . C40 C 0.4975(4) 0.7770(2) 0.22749(10) 0.0476(8) Uani 1 1 d . . . H40 H 0.4750 0.8091 0.2511 0.057 Uiso 1 1 calc R . . C41 C 0.4592(3) 0.7018(2) 0.22701(10) 0.0419(7) Uani 1 1 d . . . H41 H 0.4086 0.6813 0.2501 0.050 Uiso 1 1 calc R . . C42 C 0.4939(3) 0.65430(18) 0.19279(9) 0.0332(6) Uani 1 1 d . . . H42 H 0.4678 0.6014 0.1931 0.040 Uiso 1 1 calc R . . C43 C 0.8771(3) 0.60060(16) 0.36608(9) 0.0322(6) Uani 1 1 d . . . C44 C 0.9011(3) 0.65985(18) 0.33716(12) 0.0434(8) Uani 1 1 d . . . H44 H 0.9684 0.6532 0.3160 0.052 Uiso 1 1 calc R . . C45 C 0.8294(4) 0.7283(2) 0.33839(16) 0.0658(12) Uani 1 1 d . . . H45 H 0.8478 0.7681 0.3183 0.079 Uiso 1 1 calc R . . C46 C 0.7309(4) 0.7388(2) 0.36901(17) 0.0710(14) Uani 1 1 d . . . H46 H 0.6820 0.7860 0.3702 0.085 Uiso 1 1 calc R . . C47 C 0.7046(4) 0.6809(2) 0.39746(15) 0.0637(12) Uani 1 1 d . . . H47 H 0.6364 0.6881 0.4183 0.076 Uiso 1 1 calc R . . C48 C 0.7749(4) 0.6122(2) 0.39655(11) 0.0450(8) Uani 1 1 d . . . H48 H 0.7544 0.5725 0.4165 0.054 Uiso 1 1 calc R . . C49 C 0.8709(3) 0.42502(16) 0.38353(8) 0.0283(6) Uani 1 1 d . . . C50 C 0.8167(3) 0.36653(16) 0.35853(9) 0.0324(6) Uani 1 1 d . . . H50 H 0.8342 0.3664 0.3287 0.039 Uiso 1 1 calc R . . C51 C 0.7374(3) 0.30793(17) 0.37587(9) 0.0352(7) Uani 1 1 d . . . H51 H 0.7027 0.2682 0.3580 0.042 Uiso 1 1 calc R . . C52 C 0.7095(3) 0.30795(18) 0.41921(9) 0.0340(6) Uani 1 1 d . . . H52 H 0.6541 0.2687 0.4311 0.041 Uiso 1 1 calc R . . C53 C 0.7623(3) 0.36518(17) 0.44507(9) 0.0328(6) Uani 1 1 d . . . H53 H 0.7446 0.3649 0.4749 0.039 Uiso 1 1 calc R . . C54 C 0.8416(3) 0.42309(17) 0.42731(8) 0.0311(6) Uani 1 1 d . . . H54 H 0.8768 0.4624 0.4453 0.037 Uiso 1 1 calc R . . C55 C 1.1355(3) 0.51291(16) 0.39028(8) 0.0287(6) Uani 1 1 d . . . C56 C 1.2119(3) 0.44648(18) 0.39708(9) 0.0323(6) Uani 1 1 d . . . H56 H 1.1763 0.3974 0.3893 0.039 Uiso 1 1 calc R . . C57 C 1.3404(3) 0.4509(2) 0.41527(9) 0.0392(7) Uani 1 1 d . . . H57 H 1.3913 0.4049 0.4193 0.047 Uiso 1 1 calc R . . C58 C 1.3932(3) 0.5208(2) 0.42727(9) 0.0398(7) Uani 1 1 d . . . H58 H 1.4806 0.5237 0.4394 0.048 Uiso 1 1 calc R . . C59 C 1.3185(3) 0.5865(2) 0.42162(10) 0.0442(8) Uani 1 1 d . . . H59 H 1.3541 0.6351 0.4302 0.053 Uiso 1 1 calc R . . C60 C 1.1915(3) 0.58308(18) 0.40352(9) 0.0358(7) Uani 1 1 d . . . H60 H 1.1414 0.6295 0.4000 0.043 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 Si1 0.0170(3) 0.0317(4) 0.0193(3) 0.0019(3) 0.0000(3) 0.0004(3) Si2 0.0210(3) 0.0329(4) 0.0220(3) 0.0019(3) 0.0007(3) -0.0029(3) O1 0.0245(10) 0.0371(10) 0.0237(8) 0.0000(8) -0.0045(7) -0.0039(8) O2 0.0427(13) 0.0630(14) 0.0305(10) 0.0039(10) -0.0101(10) -0.0231(11) O3 0.0151(9) 0.0420(11) 0.0254(9) -0.0018(8) 0.0020(7) -0.0017(8) O4 0.0341(12) 0.0581(15) 0.0480(13) -0.0001(11) 0.0032(10) -0.0013(10) C1 0.0173(12) 0.0307(13) 0.0213(11) 0.0009(10) 0.0020(10) 0.0007(10) C2 0.0185(12) 0.0308(13) 0.0189(11) -0.0002(10) 0.0029(10) 0.0016(10) C3 0.0192(13) 0.0400(15) 0.0207(12) -0.0040(10) 0.0031(10) 0.0003(11) C4 0.0212(13) 0.0326(13) 0.0260(12) -0.0015(10) 0.0105(10) 0.0008(11) C5 0.0326(16) 0.0344(14) 0.0360(15) -0.0037(12) 0.0059(13) -0.0045(12) C6 0.0369(17) 0.0297(15) 0.0420(16) -0.0048(12) 0.0152(14) -0.0039(13) C7 0.0386(17) 0.0305(15) 0.0437(17) 0.0080(13) 0.0167(14) 0.0068(13) C8 0.0281(15) 0.0415(16) 0.0286(14) 0.0031(12) 0.0071(12) 0.0044(12) C9 0.0220(13) 0.0359(15) 0.0260(12) 0.0014(11) 0.0112(10) 0.0039(11) C10 0.0186(12) 0.0352(14) 0.0203(11) 0.0021(10) 0.0053(10) 0.0050(10) C11 0.0242(13) 0.0273(13) 0.0239(12) 0.0055(10) 0.0024(10) 0.0033(10) C12 0.0223(13) 0.0313(13) 0.0261(13) 0.0084(11) 0.0061(10) 0.0050(11) C13 0.0289(14) 0.0372(15) 0.0227(12) 0.0035(11) 0.0055(11) 0.0038(12) C14 0.0326(16) 0.0326(14) 0.0304(14) 0.0058(12) 0.0098(12) 0.0036(12) C15 0.0265(15) 0.0368(15) 0.0402(15) 0.0086(12) 0.0121(12) 0.0035(12) C16 0.0231(14) 0.0384(15) 0.0341(14) 0.0097(12) 0.0045(11) 0.0009(12) C17 0.0213(13) 0.0332(14) 0.0253(12) 0.0073(10) 0.0044(10) 0.0008(11) C18 0.0170(13) 0.0376(15) 0.0259(12) 0.0056(11) -0.0037(10) -0.0017(10) C19 0.0213(13) 0.0325(13) 0.0228(12) 0.0033(10) 0.0014(10) -0.0023(11) C20 0.0164(12) 0.0295(13) 0.0260(12) 0.0048(11) 0.0024(10) 0.0010(10) C21 0.0380(18) 0.0416(16) 0.0364(15) -0.0032(13) -0.0076(13) -0.0018(14) C22 0.071(3) 0.120(4) 0.051(2) 0.017(2) -0.011(2) -0.053(3) C23 0.0311(16) 0.0532(19) 0.0393(16) -0.0050(14) -0.0017(13) -0.0077(14) C24 0.0297(17) 0.050(2) 0.076(2) -0.0045(18) 0.0119(17) 0.0044(15) C25 0.0223(13) 0.0336(14) 0.0186(11) -0.0022(10) 0.0014(10) -0.0006(11) C26 0.0198(13) 0.0479(17) 0.0337(14) 0.0093(12) 0.0034(12) 0.0026(13) C27 0.0266(16) 0.0508(19) 0.0462(17) 0.0074(15) 0.0069(14) 0.0008(14) C28 0.0401(18) 0.0412(16) 0.0284(14) 0.0018(12) 0.0113(12) -0.0121(13) C29 0.0376(16) 0.0347(15) 0.0230(13) 0.0000(11) -0.0006(12) -0.0031(12) C30 0.0249(14) 0.0363(14) 0.0238(12) 0.0008(11) -0.0031(11) 0.0007(12) C31 0.0193(13) 0.0331(13) 0.0239(12) 0.0070(10) -0.0023(10) 0.0000(11) C32 0.0257(15) 0.0609(19) 0.0235(13) -0.0009(13) -0.0006(11) -0.0085(14) C33 0.0443(19) 0.073(2) 0.0238(14) 0.0000(14) -0.0059(14) -0.0148(18) C34 0.0310(16) 0.0554(19) 0.0350(15) 0.0114(14) -0.0128(13) -0.0113(15) C35 0.0198(14) 0.0480(18) 0.0445(17) 0.0125(14) -0.0055(13) -0.0061(12) C36 0.0224(14) 0.0372(15) 0.0342(14) 0.0077(12) 0.0005(11) 0.0020(11) C37 0.0182(13) 0.0384(15) 0.0246(12) 0.0023(11) -0.0027(10) 0.0050(11) C38 0.0362(17) 0.0383(16) 0.0292(14) -0.0006(12) 0.0027(12) -0.0005(13) C39 0.060(2) 0.0412(18) 0.0394(17) -0.0087(14) 0.0068(16) -0.0016(16) C40 0.056(2) 0.054(2) 0.0326(16) -0.0089(14) 0.0115(15) 0.0077(17) C41 0.0385(18) 0.0533(19) 0.0339(15) -0.0028(14) 0.0107(14) 0.0038(15) C42 0.0278(15) 0.0403(16) 0.0314(14) 0.0018(12) 0.0030(12) 0.0026(12) C43 0.0277(14) 0.0331(14) 0.0360(14) -0.0019(12) 0.0004(12) -0.0032(12) C44 0.0348(18) 0.0353(17) 0.060(2) 0.0065(14) 0.0113(15) -0.0004(13) C45 0.056(2) 0.0363(19) 0.105(3) 0.021(2) 0.024(2) 0.0025(17) C46 0.046(2) 0.0378(18) 0.129(4) 0.010(2) 0.030(3) 0.0077(17) C47 0.044(2) 0.047(2) 0.099(3) -0.007(2) 0.035(2) 0.0040(16) C48 0.0459(19) 0.0407(17) 0.0485(18) -0.0015(15) 0.0181(15) 0.0000(15) C49 0.0260(14) 0.0329(14) 0.0261(12) 0.0027(11) 0.0007(11) 0.0010(11) C50 0.0334(15) 0.0395(16) 0.0243(12) 0.0014(11) 0.0012(12) -0.0014(12) C51 0.0346(16) 0.0379(16) 0.0331(14) 0.0030(12) -0.0053(12) -0.0090(13) C52 0.0246(15) 0.0415(16) 0.0360(15) 0.0076(13) 0.0015(12) -0.0091(12) C53 0.0306(15) 0.0431(16) 0.0248(13) 0.0067(12) 0.0036(11) -0.0048(13) C54 0.0329(16) 0.0369(15) 0.0235(12) 0.0001(11) 0.0003(11) -0.0076(12) C55 0.0245(13) 0.0410(15) 0.0207(11) 0.0023(11) 0.0042(10) -0.0074(11) C56 0.0297(15) 0.0411(16) 0.0261(13) 0.0046(12) -0.0013(11) -0.0030(12) C57 0.0261(15) 0.062(2) 0.0300(14) 0.0073(14) -0.0052(12) -0.0008(14) C58 0.0287(16) 0.063(2) 0.0275(14) 0.0064(14) -0.0072(12) -0.0101(15) C59 0.0440(19) 0.056(2) 0.0322(15) -0.0057(14) -0.0001(14) -0.0190(17) C60 0.0333(17) 0.0440(16) 0.0301(14) -0.0018(12) 0.0019(12) -0.0079(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C25 1.862(3) . ? Si1 C31 1.872(3) . ? Si1 C37 1.877(3) . ? Si1 C2 1.885(3) . ? Si2 C49 1.865(3) . ? Si2 C43 1.876(3) . ? Si2 C55 1.882(3) . ? Si2 C19 1.885(3) . ? O1 C1 1.383(3) . ? O1 C21 1.428(3) . ? O2 C21 1.370(4) . ? O2 C22 1.445(4) . ? O3 C20 1.389(3) . ? O3 C23 1.429(3) . ? O4 C23 1.376(4) . ? O4 C24 1.395(4) . ? C1 C10 1.383(4) . ? C1 C2 1.418(4) . ? C2 C3 1.374(4) . ? C3 C4 1.415(4) . ? C3 H3 0.9500 . ? C4 C9 1.411(4) . ? C4 C5 1.418(4) . ? C5 C6 1.348(4) . ? C5 H5 0.9500 . ? C6 C7 1.413(5) . ? C6 H6 0.9500 . ? C7 C8 1.356(4) . ? C7 H7 0.9500 . ? C8 C9 1.422(4) . ? C8 H8 0.9500 . ? C9 C10 1.423(4) . ? C10 C11 1.500(4) . ? C11 C20 1.376(4) . ? C11 C12 1.441(4) . ? C12 C17 1.412(4) . ? C12 C13 1.420(4) . ? C13 C14 1.367(4) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.378(4) . ? C15 H15 0.9500 . ? C16 C17 1.404(4) . ? C16 H16 0.9500 . ? C17 C18 1.418(4) . ? C18 C19 1.373(4) . ? C18 H18 0.9500 . ? C19 C20 1.429(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.401(4) . ? C25 C26 1.404(4) . ? C26 C27 1.389(4) . ? C26 H26 0.9500 . ? C27 C28 1.374(4) . ? C27 H27 0.9500 . ? C28 C29 1.369(4) . ? C28 H28 0.9500 . ? C29 C30 1.391(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.398(4) . ? C31 C36 1.414(4) . ? C32 C33 1.397(4) . ? C32 H32 0.9500 . ? C33 C34 1.368(5) . ? C33 H33 0.9500 . ? C34 C35 1.375(5) . ? C34 H34 0.9500 . ? C35 C36 1.375(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 C42 1.384(4) . ? C38 C39 1.385(4) . ? C38 H38 0.9500 . ? C39 C40 1.392(5) . ? C39 H39 0.9500 . ? C40 C41 1.354(5) . ? C40 H40 0.9500 . ? C41 C42 1.392(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.387(4) . ? C43 C48 1.408(4) . ? C44 C45 1.381(5) . ? C44 H44 0.9500 . ? C45 C46 1.383(6) . ? C45 H45 0.9500 . ? C46 C47 1.364(6) . ? C46 H46 0.9500 . ? C47 C48 1.378(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.387(4) . ? C49 C54 1.401(4) . ? C50 C51 1.393(4) . ? C50 H50 0.9500 . ? C51 C52 1.385(4) . ? C51 H51 0.9500 . ? C52 C53 1.381(4) . ? C52 H52 0.9500 . ? C53 C54 1.389(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.392(4) . ? C55 C60 1.396(4) . ? C56 C57 1.401(4) . ? C56 H56 0.9500 . ? C57 C58 1.370(5) . ? C57 H57 0.9500 . ? C58 C59 1.367(5) . ? C58 H58 0.9500 . ? C59 C60 1.386(4) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 Si1 C31 108.62(11) . . ? C25 Si1 C37 108.93(12) . . ? C31 Si1 C37 110.26(12) . . ? C25 Si1 C2 114.51(12) . . ? C31 Si1 C2 107.15(12) . . ? C37 Si1 C2 107.34(11) . . ? C49 Si2 C43 110.92(13) . . ? C49 Si2 C55 108.76(12) . . ? C43 Si2 C55 110.00(13) . . ? C49 Si2 C19 111.95(12) . . ? C43 Si2 C19 109.24(12) . . ? C55 Si2 C19 105.84(12) . . ? C1 O1 C21 122.0(2) . . ? C21 O2 C22 112.5(3) . . ? C20 O3 C23 124.5(2) . . ? C23 O4 C24 114.6(3) . . ? C10 C1 O1 125.3(2) . . ? C10 C1 C2 122.8(2) . . ? O1 C1 C2 111.8(2) . . ? C3 C2 C1 118.0(2) . . ? C3 C2 Si1 122.06(19) . . ? C1 C2 Si1 119.61(19) . . ? C2 C3 C4 121.6(2) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C9 C4 C3 119.2(2) . . ? C9 C4 C5 119.0(3) . . ? C3 C4 C5 121.8(3) . . ? C6 C5 C4 121.7(3) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 121.8(3) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C4 C9 C8 117.7(3) . . ? C4 C9 C10 120.0(2) . . ? C8 C9 C10 122.2(3) . . ? C1 C10 C9 118.2(2) . . ? C1 C10 C11 123.2(2) . . ? C9 C10 C11 118.3(2) . . ? C20 C11 C12 117.9(2) . . ? C20 C11 C10 124.6(2) . . ? C12 C11 C10 117.5(2) . . ? C17 C12 C13 118.2(2) . . ? C17 C12 C11 120.0(2) . . ? C13 C12 C11 121.8(2) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.0(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 119.4(2) . . ? C16 C17 C18 121.5(3) . . ? C12 C17 C18 119.1(2) . . ? C19 C18 C17 122.1(2) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 117.6(2) . . ? C18 C19 Si2 122.1(2) . . ? C20 C19 Si2 120.24(19) . . ? C11 C20 O3 124.2(2) . . ? C11 C20 C19 123.3(2) . . ? O3 C20 C19 112.4(2) . . ? O2 C21 O1 113.1(3) . . ? O2 C21 H21A 109.0 . . ? O1 C21 H21A 109.0 . . ? O2 C21 H21B 109.0 . . ? O1 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 O3 108.3(2) . . ? O4 C23 H23A 110.0 . . ? O3 C23 H23A 110.0 . . ? O4 C23 H23B 110.0 . . ? O3 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 116.9(2) . . ? C30 C25 Si1 118.8(2) . . ? C26 C25 Si1 124.2(2) . . ? C27 C26 C25 121.5(3) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 C26 119.4(3) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 121.1(3) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 119.5(3) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C25 121.6(3) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? C32 C31 C36 117.0(2) . . ? C32 C31 Si1 120.9(2) . . ? C36 C31 Si1 122.0(2) . . ? C33 C32 C31 120.9(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 121.2(3) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C38 C37 C42 117.7(3) . . ? C38 C37 Si1 120.9(2) . . ? C42 C37 Si1 121.3(2) . . ? C37 C38 C39 121.4(3) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C40 119.6(3) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 119.7(3) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.3(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 121.3(3) . . ? C37 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C44 C43 C48 117.5(3) . . ? C44 C43 Si2 119.8(2) . . ? C48 C43 Si2 122.6(2) . . ? C45 C44 C43 121.7(3) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 119.8(3) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 119.5(4) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C43 120.2(3) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C50 C49 C54 117.0(3) . . ? C50 C49 Si2 123.0(2) . . ? C54 C49 Si2 120.0(2) . . ? C49 C50 C51 122.0(3) . . ? C49 C50 H50 119.0 . . ? C51 C50 H50 119.0 . . ? C52 C51 C50 119.7(3) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C53 C52 C51 119.9(3) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 119.8(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C49 121.8(3) . . ? C53 C54 H54 119.1 . . ? C49 C54 H54 119.1 . . ? C56 C55 C60 116.9(3) . . ? C56 C55 Si2 120.2(2) . . ? C60 C55 Si2 122.7(2) . . ? C55 C56 C57 121.0(3) . . ? C55 C56 H56 119.5 . . ? C57 C56 H56 119.5 . . ? C58 C57 C56 120.6(3) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C59 C58 C57 119.2(3) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 120.8(3) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C59 C60 C55 121.5(3) . . ? C59 C60 H60 119.3 . . ? C55 C60 H60 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 O1 C1 C10 -45.5(4) . . . . ? C21 O1 C1 C2 137.7(2) . . . . ? C10 C1 C2 C3 -2.4(4) . . . . ? O1 C1 C2 C3 174.5(2) . . . . ? C10 C1 C2 Si1 171.30(19) . . . . ? O1 C1 C2 Si1 -11.7(3) . . . . ? C25 Si1 C2 C3 -114.5(2) . . . . ? C31 Si1 C2 C3 6.0(2) . . . . ? C37 Si1 C2 C3 124.4(2) . . . . ? C25 Si1 C2 C1 72.0(2) . . . . ? C31 Si1 C2 C1 -167.45(19) . . . . ? C37 Si1 C2 C1 -49.0(2) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? Si1 C2 C3 C4 -173.84(19) . . . . ? C2 C3 C4 C9 2.0(4) . . . . ? C2 C3 C4 C5 -179.2(2) . . . . ? C9 C4 C5 C6 -1.3(4) . . . . ? C3 C4 C5 C6 179.8(3) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C5 C6 C7 C8 1.1(4) . . . . ? C6 C7 C8 C9 0.3(4) . . . . ? C3 C4 C9 C8 -178.5(2) . . . . ? C5 C4 C9 C8 2.6(4) . . . . ? C3 C4 C9 C10 -1.2(4) . . . . ? C5 C4 C9 C10 -180.0(2) . . . . ? C7 C8 C9 C4 -2.2(4) . . . . ? C7 C8 C9 C10 -179.5(3) . . . . ? O1 C1 C10 C9 -173.3(2) . . . . ? C2 C1 C10 C9 3.2(4) . . . . ? O1 C1 C10 C11 0.7(4) . . . . ? C2 C1 C10 C11 177.3(2) . . . . ? C4 C9 C10 C1 -1.4(4) . . . . ? C8 C9 C10 C1 175.9(2) . . . . ? C4 C9 C10 C11 -175.7(2) . . . . ? C8 C9 C10 C11 1.5(4) . . . . ? C1 C10 C11 C20 91.7(3) . . . . ? C9 C10 C11 C20 -94.3(3) . . . . ? C1 C10 C11 C12 -90.0(3) . . . . ? C9 C10 C11 C12 84.0(3) . . . . ? C20 C11 C12 C17 -0.8(4) . . . . ? C10 C11 C12 C17 -179.2(2) . . . . ? C20 C11 C12 C13 179.8(2) . . . . ? C10 C11 C12 C13 1.3(4) . . . . ? C17 C12 C13 C14 0.9(4) . . . . ? C11 C12 C13 C14 -179.6(3) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 0.2(4) . . . . ? C15 C16 C17 C12 0.2(4) . . . . ? C15 C16 C17 C18 179.2(3) . . . . ? C13 C12 C17 C16 -0.7(4) . . . . ? C11 C12 C17 C16 179.7(3) . . . . ? C13 C12 C17 C18 -179.8(2) . . . . ? C11 C12 C17 C18 0.7(4) . . . . ? C16 C17 C18 C19 -178.8(3) . . . . ? C12 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C20 -1.1(4) . . . . ? C17 C18 C19 Si2 179.2(2) . . . . ? C49 Si2 C19 C18 -114.6(2) . . . . ? C43 Si2 C19 C18 122.2(2) . . . . ? C55 Si2 C19 C18 3.8(3) . . . . ? C49 Si2 C19 C20 65.7(2) . . . . ? C43 Si2 C19 C20 -57.6(2) . . . . ? C55 Si2 C19 C20 -176.0(2) . . . . ? C12 C11 C20 O3 175.4(2) . . . . ? C10 C11 C20 O3 -6.3(4) . . . . ? C12 C11 C20 C19 -0.1(4) . . . . ? C10 C11 C20 C19 178.2(2) . . . . ? C23 O3 C20 C11 39.4(4) . . . . ? C23 O3 C20 C19 -144.6(3) . . . . ? C18 C19 C20 C11 1.0(4) . . . . ? Si2 C19 C20 C11 -179.2(2) . . . . ? C18 C19 C20 O3 -174.9(2) . . . . ? Si2 C19 C20 O3 4.8(3) . . . . ? C22 O2 C21 O1 61.6(4) . . . . ? C1 O1 C21 O2 108.0(3) . . . . ? C24 O4 C23 O3 66.6(3) . . . . ? C20 O3 C23 O4 156.9(2) . . . . ? C31 Si1 C25 C30 48.6(2) . . . . ? C37 Si1 C25 C30 -71.5(2) . . . . ? C2 Si1 C25 C30 168.3(2) . . . . ? C31 Si1 C25 C26 -136.3(2) . . . . ? C37 Si1 C25 C26 103.5(3) . . . . ? C2 Si1 C25 C26 -16.6(3) . . . . ? C30 C25 C26 C27 2.0(4) . . . . ? Si1 C25 C26 C27 -173.2(2) . . . . ? C25 C26 C27 C28 -0.7(5) . . . . ? C26 C27 C28 C29 -0.7(5) . . . . ? C27 C28 C29 C30 0.8(5) . . . . ? C28 C29 C30 C25 0.6(4) . . . . ? C26 C25 C30 C29 -1.9(4) . . . . ? Si1 C25 C30 C29 173.5(2) . . . . ? C25 Si1 C31 C32 42.3(3) . . . . ? C37 Si1 C31 C32 161.6(2) . . . . ? C2 Si1 C31 C32 -81.9(2) . . . . ? C25 Si1 C31 C36 -141.0(2) . . . . ? C37 Si1 C31 C36 -21.7(3) . . . . ? C2 Si1 C31 C36 94.8(2) . . . . ? C36 C31 C32 C33 -0.3(4) . . . . ? Si1 C31 C32 C33 176.6(2) . . . . ? C31 C32 C33 C34 -1.2(5) . . . . ? C32 C33 C34 C35 1.8(5) . . . . ? C33 C34 C35 C36 -0.9(5) . . . . ? C34 C35 C36 C31 -0.6(4) . . . . ? C32 C31 C36 C35 1.2(4) . . . . ? Si1 C31 C36 C35 -175.6(2) . . . . ? C25 Si1 C37 C38 6.6(3) . . . . ? C31 Si1 C37 C38 -112.5(2) . . . . ? C2 Si1 C37 C38 131.1(2) . . . . ? C25 Si1 C37 C42 -169.5(2) . . . . ? C31 Si1 C37 C42 71.4(2) . . . . ? C2 Si1 C37 C42 -45.0(3) . . . . ? C42 C37 C38 C39 -0.1(4) . . . . ? Si1 C37 C38 C39 -176.3(3) . . . . ? C37 C38 C39 C40 0.0(5) . . . . ? C38 C39 C40 C41 -0.5(6) . . . . ? C39 C40 C41 C42 1.0(5) . . . . ? C38 C37 C42 C41 0.6(4) . . . . ? Si1 C37 C42 C41 176.9(2) . . . . ? C40 C41 C42 C37 -1.1(5) . . . . ? C49 Si2 C43 C44 -152.6(2) . . . . ? C55 Si2 C43 C44 87.0(3) . . . . ? C19 Si2 C43 C44 -28.8(3) . . . . ? C49 Si2 C43 C48 22.7(3) . . . . ? C55 Si2 C43 C48 -97.7(3) . . . . ? C19 Si2 C43 C48 146.5(3) . . . . ? C48 C43 C44 C45 1.0(5) . . . . ? Si2 C43 C44 C45 176.6(3) . . . . ? C43 C44 C45 C46 -0.1(7) . . . . ? C44 C45 C46 C47 -0.7(7) . . . . ? C45 C46 C47 C48 0.5(7) . . . . ? C46 C47 C48 C43 0.5(6) . . . . ? C44 C43 C48 C47 -1.2(5) . . . . ? Si2 C43 C48 C47 -176.6(3) . . . . ? C43 Si2 C49 C50 111.7(3) . . . . ? C55 Si2 C49 C50 -127.2(2) . . . . ? C19 Si2 C49 C50 -10.6(3) . . . . ? C43 Si2 C49 C54 -64.8(3) . . . . ? C55 Si2 C49 C54 56.3(3) . . . . ? C19 Si2 C49 C54 172.9(2) . . . . ? C54 C49 C50 C51 -0.5(4) . . . . ? Si2 C49 C50 C51 -177.1(2) . . . . ? C49 C50 C51 C52 0.9(5) . . . . ? C50 C51 C52 C53 -1.2(5) . . . . ? C51 C52 C53 C54 1.0(5) . . . . ? C52 C53 C54 C49 -0.5(5) . . . . ? C50 C49 C54 C53 0.3(4) . . . . ? Si2 C49 C54 C53 177.0(2) . . . . ? C49 Si2 C55 C56 47.5(2) . . . . ? C43 Si2 C55 C56 169.1(2) . . . . ? C19 Si2 C55 C56 -73.0(2) . . . . ? C49 Si2 C55 C60 -137.0(2) . . . . ? C43 Si2 C55 C60 -15.3(3) . . . . ? C19 Si2 C55 C60 102.5(2) . . . . ? C60 C55 C56 C57 -1.8(4) . . . . ? Si2 C55 C56 C57 174.0(2) . . . . ? C55 C56 C57 C58 0.8(4) . . . . ? C56 C57 C58 C59 0.5(4) . . . . ? C57 C58 C59 C60 -0.8(4) . . . . ? C58 C59 C60 C55 -0.3(4) . . . . ? C56 C55 C60 C59 1.6(4) . . . . ? Si2 C55 C60 C59 -174.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.817 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.058 data_7 _database_code_depnum_ccdc_archive 'CCDC 815803' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H52 O6 P2' _chemical_formula_sum 'C58 H52 O6 P2' _chemical_formula_weight 906.94 _chemiccal_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.8619(2) _cell_length_b 18.1864(3) _cell_length_c 26.4065(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4736.07(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34625 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.52 _exptl_crystal_description 'cut block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34556 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10860 _reflns_number_gt 8687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.1548P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(7) _refine_ls_number_reflns 10860 _refine_ls_number_parameters 606 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.66927(7) 0.41971(4) 0.15019(2) 0.02834(15) Uani 1 1 d . . . P2 P 0.46861(7) 0.49184(4) 0.33500(2) 0.02954(15) Uani 1 1 d . . . O1 O 0.66789(18) 0.50888(9) 0.14519(6) 0.0314(4) Uani 1 1 d . . . O2 O 0.73375(17) 0.40824(9) 0.09301(6) 0.0294(4) Uani 1 1 d . . . O3 O 0.80402(18) 0.40746(9) 0.18517(5) 0.0291(4) Uani 1 1 d . . . O4 O 0.38334(18) 0.53816(9) 0.29290(6) 0.0305(4) Uani 1 1 d . . . O5 O 0.38801(18) 0.52983(9) 0.38282(6) 0.0305(4) Uani 1 1 d . . . O6 O 0.39316(18) 0.41226(9) 0.33378(5) 0.0296(4) Uani 1 1 d . . . C1 C 0.5270(3) 0.52433(13) 0.21981(8) 0.0269(5) Uani 1 1 d . . . H1 H 0.5407 0.4742 0.2285 0.032 Uiso 1 1 calc R . . C2 C 0.5878(3) 0.55304(13) 0.17664(8) 0.0257(5) Uani 1 1 d . . . C3 C 0.5717(3) 0.62684(13) 0.16343(8) 0.0281(5) Uani 1 1 d . . . C4 C 0.4877(3) 0.66779(13) 0.19523(8) 0.0301(6) Uani 1 1 d . . . H4 H 0.4739 0.7180 0.1866 0.036 Uiso 1 1 calc R . . C5 C 0.4221(3) 0.64198(13) 0.23848(8) 0.0282(5) Uani 1 1 d . . . C6 C 0.4463(2) 0.56858(13) 0.25026(8) 0.0262(5) Uani 1 1 d . . . C7 C 0.6426(3) 0.66467(13) 0.11873(9) 0.0341(6) Uani 1 1 d . . . C8 C 0.7927(3) 0.6714(2) 0.13171(13) 0.0634(10) Uani 1 1 d . . . H8A H 0.8322 0.6222 0.1350 0.095 Uiso 1 1 calc R . . H8B H 0.8029 0.6980 0.1637 0.095 Uiso 1 1 calc R . . H8C H 0.8395 0.6983 0.1047 0.095 Uiso 1 1 calc R . . C9 C 0.6189(4) 0.62434(16) 0.06888(9) 0.0538(9) Uani 1 1 d . . . H9A H 0.6621 0.6516 0.0412 0.081 Uiso 1 1 calc R . . H9B H 0.5212 0.6206 0.0625 0.081 Uiso 1 1 calc R . . H9C H 0.6581 0.5749 0.0709 0.081 Uiso 1 1 calc R . . C10 C 0.5864(3) 0.74285(14) 0.11096(10) 0.0415(7) Uani 1 1 d . . . H10A H 0.6326 0.7661 0.0823 0.062 Uiso 1 1 calc R . . H10B H 0.6018 0.7720 0.1416 0.062 Uiso 1 1 calc R . . H10C H 0.4889 0.7402 0.1040 0.062 Uiso 1 1 calc R . . C11 C 0.3368(3) 0.69379(14) 0.27139(9) 0.0368(7) Uani 1 1 d . . . C12 C 0.3188(4) 0.76880(16) 0.24534(10) 0.0523(9) Uani 1 1 d . . . H12A H 0.2776 0.7617 0.2119 0.079 Uiso 1 1 calc R . . H12B H 0.4075 0.7924 0.2414 0.079 Uiso 1 1 calc R . . H12C H 0.2600 0.8001 0.2661 0.079 Uiso 1 1 calc R . . C13 C 0.1955(3) 0.66356(17) 0.28110(11) 0.0455(7) Uani 1 1 d . . . H13A H 0.1469 0.6589 0.2489 0.068 Uiso 1 1 calc R . . H13B H 0.1460 0.6971 0.3035 0.068 Uiso 1 1 calc R . . H13C H 0.2025 0.6151 0.2972 0.068 Uiso 1 1 calc R . . C14 C 0.4127(4) 0.70679(15) 0.32135(9) 0.0451(8) Uani 1 1 d . . . H14A H 0.3648 0.7441 0.3413 0.068 Uiso 1 1 calc R . . H14B H 0.5050 0.7239 0.3141 0.068 Uiso 1 1 calc R . . H14C H 0.4169 0.6607 0.3406 0.068 Uiso 1 1 calc R . . C15 C 0.7942(3) 0.33852(14) 0.08754(8) 0.0275(5) Uani 1 1 d . . . C16 C 0.7204(3) 0.28234(14) 0.06236(8) 0.0291(6) Uani 1 1 d . . . C17 C 0.7766(3) 0.21391(14) 0.06176(8) 0.0295(6) Uani 1 1 d . . . H17 H 0.7294 0.1754 0.0450 0.035 Uiso 1 1 calc R . . C18 C 0.9021(3) 0.19775(13) 0.08498(8) 0.0281(5) Uani 1 1 d . . . C19 C 0.9524(3) 0.12508(14) 0.08895(9) 0.0306(6) Uani 1 1 d . . . H19 H 0.9019 0.0859 0.0744 0.037 Uiso 1 1 calc R . . C20 C 1.0715(3) 0.10989(15) 0.11313(10) 0.0359(6) Uani 1 1 d . . . H20 H 1.1025 0.0606 0.1158 0.043 Uiso 1 1 calc R . . C21 C 1.1482(3) 0.16775(14) 0.13411(9) 0.0355(6) Uani 1 1 d . . . H21 H 1.2320 0.1573 0.1503 0.043 Uiso 1 1 calc R . . C22 C 1.1034(3) 0.23837(14) 0.13140(9) 0.0301(6) Uani 1 1 d . . . H22 H 1.1564 0.2766 0.1459 0.036 Uiso 1 1 calc R . . C23 C 0.9785(3) 0.25596(13) 0.10724(8) 0.0267(5) Uani 1 1 d . . . C24 C 0.9223(3) 0.32853(13) 0.10715(8) 0.0252(5) Uani 1 1 d . . . C25 C 0.9926(3) 0.39271(13) 0.12980(8) 0.0265(5) Uani 1 1 d . . . C26 C 1.1193(3) 0.41868(13) 0.11074(8) 0.0267(5) Uani 1 1 d . . . C27 C 1.1842(3) 0.38677(14) 0.06800(8) 0.0298(5) Uani 1 1 d . . . H27 H 1.1446 0.3455 0.0516 0.036 Uiso 1 1 calc R . . C28 C 1.3034(3) 0.41526(15) 0.05046(9) 0.0322(6) Uani 1 1 d . . . H28 H 1.3455 0.3936 0.0217 0.039 Uiso 1 1 calc R . . C29 C 1.3644(3) 0.47533(15) 0.07384(9) 0.0343(6) Uani 1 1 d . . . H29 H 1.4482 0.4938 0.0615 0.041 Uiso 1 1 calc R . . C30 C 1.3032(3) 0.50788(15) 0.11480(9) 0.0335(6) Uani 1 1 d . . . H30 H 1.3450 0.5491 0.1304 0.040 Uiso 1 1 calc R . . C31 C 1.1799(3) 0.48114(13) 0.13393(8) 0.0284(5) Uani 1 1 d . . . C32 C 1.1134(3) 0.51563(14) 0.17536(8) 0.0313(6) Uani 1 1 d . . . H32 H 1.1564 0.5561 0.1915 0.038 Uiso 1 1 calc R . . C33 C 0.9900(3) 0.49284(13) 0.19291(8) 0.0305(6) Uani 1 1 d . . . C34 C 0.9314(3) 0.43162(13) 0.16860(8) 0.0268(5) Uani 1 1 d . . . C35 C 0.5835(3) 0.29905(16) 0.04006(10) 0.0380(6) Uani 1 1 d . . . H35A H 0.5507 0.2561 0.0213 0.057 Uiso 1 1 calc R . . H35B H 0.5910 0.3411 0.0170 0.057 Uiso 1 1 calc R . . H35C H 0.5197 0.3108 0.0673 0.057 Uiso 1 1 calc R . . C36 C 0.9178(3) 0.53052(15) 0.23633(9) 0.0355(6) Uani 1 1 d . . . H36A H 0.9829 0.5600 0.2556 0.053 Uiso 1 1 calc R . . H36B H 0.8772 0.4934 0.2585 0.053 Uiso 1 1 calc R . . H36C H 0.8464 0.5626 0.2229 0.053 Uiso 1 1 calc R . . C37 C 0.3853(3) 0.48815(14) 0.42777(8) 0.0292(6) Uani 1 1 d . . . C38 C 0.4799(3) 0.50825(16) 0.46623(9) 0.0363(6) Uani 1 1 d . . . C39 C 0.4784(3) 0.46590(18) 0.50930(9) 0.0442(8) Uani 1 1 d . . . H39 H 0.5390 0.4778 0.5360 0.053 Uiso 1 1 calc R . . C40 C 0.3899(3) 0.40534(16) 0.51540(9) 0.0383(7) Uani 1 1 d . . . C41 C 0.3961(4) 0.3597(2) 0.55940(10) 0.0527(9) Uani 1 1 d . . . H41 H 0.4578 0.3716 0.5858 0.063 Uiso 1 1 calc R . . C42 C 0.3153(4) 0.29960(19) 0.56410(10) 0.0574(10) Uani 1 1 d . . . H42 H 0.3213 0.2697 0.5935 0.069 Uiso 1 1 calc R . . C43 C 0.2233(3) 0.28153(18) 0.52571(10) 0.0497(8) Uani 1 1 d . . . H43 H 0.1680 0.2390 0.5290 0.060 Uiso 1 1 calc R . . C44 C 0.2126(3) 0.32490(15) 0.48333(9) 0.0379(7) Uani 1 1 d . . . H44 H 0.1487 0.3124 0.4578 0.045 Uiso 1 1 calc R . . C45 C 0.2956(3) 0.38816(15) 0.47694(8) 0.0325(6) Uani 1 1 d . . . C46 C 0.2930(3) 0.43283(14) 0.43176(8) 0.0276(5) Uani 1 1 d . . . C47 C 0.1999(3) 0.41701(13) 0.38874(8) 0.0266(5) Uani 1 1 d . . . C48 C 0.0558(3) 0.41367(13) 0.39438(8) 0.0275(5) Uani 1 1 d . . . C49 C -0.0118(3) 0.43222(13) 0.44037(9) 0.0312(6) Uani 1 1 d . . . H49 H 0.0397 0.4468 0.4690 0.037 Uiso 1 1 calc R . . C50 C -0.1500(3) 0.42923(14) 0.44363(9) 0.0358(6) Uani 1 1 d . . . H50 H -0.1932 0.4419 0.4746 0.043 Uiso 1 1 calc R . . C51 C -0.2286(3) 0.40797(15) 0.40231(10) 0.0384(6) Uani 1 1 d . . . H51 H -0.3245 0.4053 0.4055 0.046 Uiso 1 1 calc R . . C52 C -0.1688(3) 0.39104(14) 0.35765(10) 0.0372(6) Uani 1 1 d . . . H52 H -0.2237 0.3775 0.3296 0.045 Uiso 1 1 calc R . . C53 C -0.0256(3) 0.39308(13) 0.35190(9) 0.0323(6) Uani 1 1 d . . . C54 C 0.0388(3) 0.37695(14) 0.30551(9) 0.0348(6) Uani 1 1 d . . . H54 H -0.0151 0.3610 0.2778 0.042 Uiso 1 1 calc R . . C55 C 0.1754(3) 0.38330(13) 0.29891(8) 0.0312(6) Uani 1 1 d . . . C56 C 0.2531(3) 0.40543(13) 0.34109(8) 0.0271(5) Uani 1 1 d . . . C57 C 0.5738(3) 0.57168(17) 0.45943(11) 0.0478(8) Uani 1 1 d . . . H57A H 0.6291 0.5778 0.4900 0.072 Uiso 1 1 calc R . . H57B H 0.5211 0.6165 0.4535 0.072 Uiso 1 1 calc R . . H57C H 0.6332 0.5625 0.4303 0.072 Uiso 1 1 calc R . . C58 C 0.2440(3) 0.36624(16) 0.24946(9) 0.0395(7) Uani 1 1 d . . . H58A H 0.1757 0.3523 0.2243 0.059 Uiso 1 1 calc R . . H58B H 0.3079 0.3255 0.2542 0.059 Uiso 1 1 calc R . . H58C H 0.2932 0.4098 0.2376 0.059 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 P1 0.0321(4) 0.0244(3) 0.0285(3) 0.0002(2) 0.0077(3) 0.0061(3) P2 0.0328(4) 0.0310(3) 0.0248(3) 0.0020(2) 0.0052(3) 0.0084(3) O1 0.0341(10) 0.0270(9) 0.0331(8) 0.0011(7) 0.0109(7) 0.0070(8) O2 0.0327(10) 0.0270(9) 0.0285(7) 0.0006(7) 0.0042(7) 0.0091(8) O3 0.0356(10) 0.0264(9) 0.0253(7) 0.0005(6) 0.0071(7) 0.0052(8) O4 0.0314(10) 0.0323(10) 0.0279(8) 0.0048(7) 0.0073(7) 0.0077(8) O5 0.0363(10) 0.0289(9) 0.0261(7) -0.0015(7) 0.0054(7) 0.0058(8) O6 0.0389(10) 0.0269(9) 0.0231(7) 0.0010(7) 0.0054(7) 0.0103(8) C1 0.0297(13) 0.0223(12) 0.0288(10) 0.0028(9) 0.0026(10) 0.0046(11) C2 0.0262(13) 0.0266(12) 0.0242(10) -0.0021(9) 0.0049(9) 0.0049(10) C3 0.0373(15) 0.0218(12) 0.0252(10) -0.0008(9) 0.0029(10) -0.0009(11) C4 0.0425(16) 0.0203(11) 0.0274(10) 0.0001(9) 0.0000(11) 0.0020(12) C5 0.0361(15) 0.0250(13) 0.0234(10) -0.0034(9) 0.0024(10) 0.0057(11) C6 0.0287(14) 0.0269(13) 0.0231(9) 0.0028(9) 0.0025(10) 0.0022(11) C7 0.0477(18) 0.0237(12) 0.0309(12) 0.0026(10) 0.0066(11) -0.0018(12) C8 0.040(2) 0.076(3) 0.075(2) 0.0386(19) 0.0167(17) -0.0034(19) C9 0.099(3) 0.0322(16) 0.0302(13) 0.0037(11) 0.0175(15) 0.0044(17) C10 0.059(2) 0.0268(14) 0.0385(13) 0.0063(11) 0.0109(14) -0.0032(14) C11 0.057(2) 0.0246(13) 0.0289(11) -0.0026(9) 0.0058(12) 0.0141(14) C12 0.084(3) 0.0330(15) 0.0400(14) -0.0010(12) 0.0079(16) 0.0263(17) C13 0.047(2) 0.0455(17) 0.0435(14) -0.0071(13) 0.0084(14) 0.0203(15) C14 0.072(2) 0.0343(15) 0.0290(12) -0.0087(11) 0.0041(13) 0.0083(15) C15 0.0318(15) 0.0273(13) 0.0233(10) -0.0014(9) 0.0060(10) 0.0062(11) C16 0.0279(14) 0.0355(15) 0.0240(10) -0.0018(10) 0.0041(10) 0.0020(11) C17 0.0304(15) 0.0309(14) 0.0273(11) -0.0079(10) 0.0045(10) -0.0014(11) C18 0.0327(15) 0.0270(13) 0.0247(10) -0.0052(9) 0.0056(10) 0.0028(12) C19 0.0337(15) 0.0247(13) 0.0334(11) -0.0078(10) 0.0014(11) 0.0015(12) C20 0.0373(16) 0.0244(13) 0.0459(14) -0.0046(11) 0.0017(12) 0.0053(12) C21 0.0330(16) 0.0316(14) 0.0419(13) -0.0035(11) -0.0027(12) 0.0084(12) C22 0.0292(15) 0.0279(13) 0.0333(11) -0.0053(10) -0.0006(11) -0.0006(12) C23 0.0291(14) 0.0267(12) 0.0243(10) -0.0016(9) 0.0075(10) 0.0026(11) C24 0.0293(14) 0.0248(12) 0.0216(10) -0.0019(9) 0.0050(10) 0.0023(11) C25 0.0307(14) 0.0248(12) 0.0239(10) 0.0036(9) -0.0005(10) 0.0052(11) C26 0.0295(14) 0.0252(12) 0.0256(10) 0.0015(9) -0.0008(10) 0.0053(11) C27 0.0294(14) 0.0305(13) 0.0294(11) -0.0001(10) -0.0006(11) 0.0053(12) C28 0.0286(14) 0.0402(15) 0.0279(11) 0.0000(10) 0.0002(10) 0.0057(13) C29 0.0272(14) 0.0407(16) 0.0349(12) 0.0042(11) -0.0007(10) 0.0011(12) C30 0.0318(15) 0.0320(14) 0.0365(12) 0.0016(11) -0.0053(11) 0.0000(12) C31 0.0320(14) 0.0265(12) 0.0266(10) 0.0036(9) -0.0029(10) 0.0036(12) C32 0.0372(15) 0.0252(13) 0.0313(11) -0.0022(9) -0.0032(10) 0.0026(12) C33 0.0396(16) 0.0255(12) 0.0263(10) -0.0005(9) -0.0005(10) 0.0066(12) C34 0.0288(14) 0.0262(12) 0.0252(10) 0.0032(9) 0.0032(10) 0.0052(11) C35 0.0369(17) 0.0390(16) 0.0381(13) -0.0069(11) -0.0043(12) 0.0081(13) C36 0.0414(16) 0.0336(15) 0.0316(12) -0.0089(10) 0.0033(11) 0.0044(13) C37 0.0320(14) 0.0349(14) 0.0208(9) -0.0016(9) 0.0025(9) 0.0122(12) C38 0.0322(15) 0.0433(16) 0.0334(11) -0.0113(11) 0.0008(11) 0.0134(13) C39 0.0416(17) 0.060(2) 0.0309(12) -0.0142(12) -0.0103(12) 0.0260(16) C40 0.0406(17) 0.0489(17) 0.0254(11) -0.0025(11) 0.0009(11) 0.0229(15) C41 0.064(2) 0.066(2) 0.0283(13) 0.0015(13) -0.0073(14) 0.0382(19) C42 0.080(3) 0.061(2) 0.0309(13) 0.0220(13) 0.0089(16) 0.030(2) C43 0.062(2) 0.0491(19) 0.0377(14) 0.0184(13) 0.0172(15) 0.0256(16) C44 0.0444(18) 0.0389(16) 0.0303(12) 0.0091(11) 0.0103(12) 0.0173(14) C45 0.0389(16) 0.0361(14) 0.0226(10) -0.0003(10) 0.0049(10) 0.0171(13) C46 0.0299(14) 0.0317(14) 0.0212(10) 0.0018(9) 0.0033(10) 0.0098(11) C47 0.0363(15) 0.0200(11) 0.0234(10) 0.0036(9) 0.0020(10) 0.0056(11) C48 0.0354(15) 0.0194(12) 0.0276(10) 0.0063(9) 0.0009(10) 0.0047(11) C49 0.0370(16) 0.0276(13) 0.0291(11) 0.0065(9) 0.0015(11) 0.0067(12) C50 0.0411(17) 0.0312(14) 0.0351(12) 0.0108(10) 0.0071(12) 0.0105(13) C51 0.0323(15) 0.0348(16) 0.0481(15) 0.0125(12) 0.0021(12) 0.0031(13) C52 0.0391(16) 0.0291(14) 0.0435(13) 0.0047(11) -0.0083(13) -0.0024(13) C53 0.0393(16) 0.0234(12) 0.0342(11) 0.0051(10) -0.0052(12) 0.0005(12) C54 0.0516(19) 0.0254(13) 0.0273(11) 0.0001(9) -0.0075(12) 0.0002(13) C55 0.0484(18) 0.0214(12) 0.0237(10) 0.0022(9) -0.0020(11) 0.0063(13) C56 0.0362(15) 0.0192(12) 0.0258(10) 0.0043(9) 0.0021(10) 0.0059(10) C57 0.0379(17) 0.0504(19) 0.0549(16) -0.0202(14) 0.0000(14) 0.0048(15) C58 0.055(2) 0.0384(16) 0.0253(11) -0.0026(11) -0.0010(12) 0.0105(14) _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 P1 O1 1.6272(18) . ? P1 O3 1.6338(19) . ? P1 O2 1.6516(16) . ? P2 O6 1.6277(19) . ? P2 O4 1.6286(17) . ? P2 O5 1.6442(16) . ? O1 C2 1.399(3) . ? O2 C15 1.408(3) . ? O3 C34 1.401(3) . ? O4 C6 1.400(3) . ? O5 C37 1.409(3) . ? O6 C56 1.400(3) . ? C1 C6 1.388(3) . ? C1 C2 1.390(3) . ? C1 H1 0.9500 . ? C2 C3 1.396(3) . ? C3 C4 1.395(3) . ? C3 C7 1.535(3) . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? C5 C6 1.391(3) . ? C5 C11 1.533(3) . ? C7 C8 1.525(4) . ? C7 C9 1.525(4) . ? C7 C10 1.540(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.520(4) . ? C11 C14 1.535(4) . ? C11 C12 1.538(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.378(4) . ? C15 C16 1.420(3) . ? C16 C17 1.363(3) . ? C16 C35 1.504(4) . ? C17 C18 1.412(4) . ? C17 H17 0.9500 . ? C18 C19 1.415(3) . ? C18 C23 1.426(3) . ? C19 C20 1.365(4) . ? C19 H19 0.9500 . ? C20 C21 1.409(4) . ? C20 H20 0.9500 . ? C21 C22 1.360(4) . ? C21 H21 0.9500 . ? C22 C23 1.424(4) . ? C22 H22 0.9500 . ? C23 C24 1.431(3) . ? C24 C25 1.483(3) . ? C25 C34 1.384(3) . ? C25 C26 1.428(3) . ? C26 C27 1.422(3) . ? C26 C31 1.422(3) . ? C27 C28 1.365(4) . ? C27 H27 0.9500 . ? C28 C29 1.391(4) . ? C28 H28 0.9500 . ? C29 C30 1.373(3) . ? C29 H29 0.9500 . ? C30 C31 1.404(4) . ? C30 H30 0.9500 . ? C31 C32 1.421(3) . ? C32 C33 1.366(4) . ? C32 H32 0.9500 . ? C33 C34 1.410(3) . ? C33 C36 1.514(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C46 1.361(4) . ? C37 C38 1.427(3) . ? C38 C39 1.374(4) . ? C38 C57 1.490(4) . ? C39 C40 1.414(4) . ? C39 H39 0.9500 . ? C40 C45 1.412(4) . ? C40 C41 1.429(4) . ? C41 C42 1.359(5) . ? C41 H41 0.9500 . ? C42 C43 1.400(5) . ? C42 H42 0.9500 . ? C43 C44 1.373(3) . ? C43 H43 0.9500 . ? C44 C45 1.422(4) . ? C44 H44 0.9500 . ? C45 C46 1.443(3) . ? C46 C47 1.489(3) . ? C47 C56 1.380(3) . ? C47 C48 1.431(4) . ? C48 C49 1.426(3) . ? C48 C53 1.429(3) . ? C49 C50 1.367(4) . ? C49 H49 0.9500 . ? C50 C51 1.393(4) . ? C50 H50 0.9500 . ? C51 C52 1.354(4) . ? C51 H51 0.9500 . ? C52 C53 1.422(4) . ? C52 H52 0.9500 . ? C53 C54 1.411(4) . ? C54 C55 1.363(4) . ? C54 H54 0.9500 . ? C55 C56 1.411(3) . ? C55 C58 1.503(3) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 O3 100.87(10) . . ? O1 P1 O2 93.14(9) . . ? O3 P1 O2 100.75(9) . . ? O6 P2 O4 102.14(9) . . ? O6 P2 O5 99.66(9) . . ? O4 P2 O5 93.29(8) . . ? C2 O1 P1 121.91(14) . . ? C15 O2 P1 111.74(14) . . ? C34 O3 P1 120.65(13) . . ? C6 O4 P2 121.62(15) . . ? C37 O5 P2 115.48(14) . . ? C56 O6 P2 121.81(15) . . ? C6 C1 C2 120.3(2) . . ? C6 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C1 C2 C3 121.1(2) . . ? C1 C2 O1 121.0(2) . . ? C3 C2 O1 117.9(2) . . ? C4 C3 C2 115.5(2) . . ? C4 C3 C7 119.6(2) . . ? C2 C3 C7 124.8(2) . . ? C5 C4 C3 126.1(2) . . ? C5 C4 H4 117.0 . . ? C3 C4 H4 117.0 . . ? C6 C5 C4 115.3(2) . . ? C6 C5 C11 123.9(2) . . ? C4 C5 C11 120.8(2) . . ? C1 C6 C5 121.7(2) . . ? C1 C6 O4 119.4(2) . . ? C5 C6 O4 118.9(2) . . ? C8 C7 C9 112.4(3) . . ? C8 C7 C3 107.8(2) . . ? C9 C7 C3 112.3(2) . . ? C8 C7 C10 107.8(2) . . ? C9 C7 C10 105.9(2) . . ? C3 C7 C10 110.6(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C5 112.1(2) . . ? C13 C11 C14 111.0(2) . . ? C5 C11 C14 108.3(2) . . ? C13 C11 C12 106.9(3) . . ? C5 C11 C12 110.8(2) . . ? C14 C11 C12 107.7(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 O2 117.9(2) . . ? C24 C15 C16 123.5(2) . . ? O2 C15 C16 118.6(2) . . ? C17 C16 C15 117.0(2) . . ? C17 C16 C35 123.0(2) . . ? C15 C16 C35 119.9(2) . . ? C16 C17 C18 122.8(2) . . ? C16 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C17 C18 C19 122.2(2) . . ? C17 C18 C23 119.2(2) . . ? C19 C18 C23 118.6(2) . . ? C20 C19 C18 121.7(2) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 119.6(2) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.7(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 121.1(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.3(2) . . ? C22 C23 C24 122.9(2) . . ? C18 C23 C24 118.7(2) . . ? C15 C24 C23 118.5(2) . . ? C15 C24 C25 118.4(2) . . ? C23 C24 C25 123.0(2) . . ? C34 C25 C26 118.3(2) . . ? C34 C25 C24 119.8(2) . . ? C26 C25 C24 121.8(2) . . ? C27 C26 C31 118.6(2) . . ? C27 C26 C25 122.6(2) . . ? C31 C26 C25 118.7(2) . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 121.3(2) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 121.0(2) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C32 121.6(2) . . ? C30 C31 C26 119.1(2) . . ? C32 C31 C26 119.3(2) . . ? C33 C32 C31 122.6(2) . . ? C33 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C32 C33 C34 116.8(2) . . ? C32 C33 C36 122.6(2) . . ? C34 C33 C36 120.6(2) . . ? C25 C34 O3 117.5(2) . . ? C25 C34 C33 124.2(2) . . ? O3 C34 C33 118.3(2) . . ? C16 C35 H35A 109.5 . . ? C16 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C16 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C46 C37 O5 118.4(2) . . ? C46 C37 C38 124.9(2) . . ? O5 C37 C38 116.7(2) . . ? C39 C38 C37 116.0(3) . . ? C39 C38 C57 122.7(3) . . ? C37 C38 C57 121.3(2) . . ? C38 C39 C40 122.5(3) . . ? C38 C39 H39 118.7 . . ? C40 C39 H39 118.7 . . ? C45 C40 C39 119.8(2) . . ? C45 C40 C41 119.0(3) . . ? C39 C40 C41 121.2(3) . . ? C42 C41 C40 121.1(3) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 120.2(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 120.4(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 121.1(3) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C40 C45 C44 118.2(2) . . ? C40 C45 C46 118.8(3) . . ? C44 C45 C46 122.9(2) . . ? C37 C46 C45 117.9(2) . . ? C37 C46 C47 119.8(2) . . ? C45 C46 C47 122.2(2) . . ? C56 C47 C48 117.8(2) . . ? C56 C47 C46 119.4(2) . . ? C48 C47 C46 122.8(2) . . ? C49 C48 C53 117.9(2) . . ? C49 C48 C47 122.9(2) . . ? C53 C48 C47 119.1(2) . . ? C50 C49 C48 120.7(2) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 121.1(2) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C52 C51 C50 120.2(3) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 121.3(3) . . ? C51 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C54 C53 C52 122.3(2) . . ? C54 C53 C48 118.9(2) . . ? C52 C53 C48 118.7(2) . . ? C55 C54 C53 122.6(2) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C54 C55 C56 117.4(2) . . ? C54 C55 C58 122.6(2) . . ? C56 C55 C58 120.0(3) . . ? C47 C56 O6 119.2(2) . . ? C47 C56 C55 123.9(2) . . ? O6 C56 C55 116.9(2) . . ? C38 C57 H57A 109.5 . . ? C38 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C38 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C2 -97.02(18) . . . . ? O2 P1 O1 C2 161.40(18) . . . . ? O1 P1 O2 C15 160.10(16) . . . . ? O3 P1 O2 C15 58.41(17) . . . . ? O1 P1 O3 C34 -59.66(17) . . . . ? O2 P1 O3 C34 35.69(18) . . . . ? O6 P2 O4 C6 -120.94(17) . . . . ? O5 P2 O4 C6 138.44(18) . . . . ? O6 P2 O5 C37 52.45(18) . . . . ? O4 P2 O5 C37 155.36(18) . . . . ? O4 P2 O6 C56 -54.69(17) . . . . ? O5 P2 O6 C56 40.82(17) . . . . ? C6 C1 C2 C3 1.3(4) . . . . ? C6 C1 C2 O1 -179.1(2) . . . . ? P1 O1 C2 C1 12.9(3) . . . . ? P1 O1 C2 C3 -167.43(19) . . . . ? C1 C2 C3 C4 -2.2(4) . . . . ? O1 C2 C3 C4 178.2(2) . . . . ? C1 C2 C3 C7 175.6(2) . . . . ? O1 C2 C3 C7 -4.1(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C7 C3 C4 C5 -176.7(3) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C3 C4 C5 C11 177.5(2) . . . . ? C2 C1 C6 C5 0.9(4) . . . . ? C2 C1 C6 O4 178.5(2) . . . . ? C4 C5 C6 C1 -1.9(4) . . . . ? C11 C5 C6 C1 -178.4(2) . . . . ? C4 C5 C6 O4 -179.5(2) . . . . ? C11 C5 C6 O4 4.0(4) . . . . ? P2 O4 C6 C1 51.9(3) . . . . ? P2 O4 C6 C5 -130.5(2) . . . . ? C4 C3 C7 C8 107.4(3) . . . . ? C2 C3 C7 C8 -70.2(3) . . . . ? C4 C3 C7 C9 -128.3(3) . . . . ? C2 C3 C7 C9 54.1(4) . . . . ? C4 C3 C7 C10 -10.2(3) . . . . ? C2 C3 C7 C10 172.1(3) . . . . ? C6 C5 C11 C13 -55.4(3) . . . . ? C4 C5 C11 C13 128.3(3) . . . . ? C6 C5 C11 C14 67.4(3) . . . . ? C4 C5 C11 C14 -108.9(3) . . . . ? C6 C5 C11 C12 -174.7(3) . . . . ? C4 C5 C11 C12 8.9(4) . . . . ? P1 O2 C15 C24 -79.7(2) . . . . ? P1 O2 C15 C16 100.2(2) . . . . ? C24 C15 C16 C17 5.6(3) . . . . ? O2 C15 C16 C17 -174.2(2) . . . . ? C24 C15 C16 C35 -177.3(2) . . . . ? O2 C15 C16 C35 2.9(3) . . . . ? C15 C16 C17 C18 0.3(3) . . . . ? C35 C16 C17 C18 -176.7(2) . . . . ? C16 C17 C18 C19 172.9(2) . . . . ? C16 C17 C18 C23 -4.3(3) . . . . ? C17 C18 C19 C20 -177.6(2) . . . . ? C23 C18 C19 C20 -0.4(3) . . . . ? C18 C19 C20 C21 -1.0(4) . . . . ? C19 C20 C21 C22 1.3(4) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? C21 C22 C23 C18 -1.2(3) . . . . ? C21 C22 C23 C24 174.8(2) . . . . ? C17 C18 C23 C22 178.7(2) . . . . ? C19 C18 C23 C22 1.5(3) . . . . ? C17 C18 C23 C24 2.6(3) . . . . ? C19 C18 C23 C24 -174.6(2) . . . . ? O2 C15 C24 C23 172.71(19) . . . . ? C16 C15 C24 C23 -7.1(3) . . . . ? O2 C15 C24 C25 -3.9(3) . . . . ? C16 C15 C24 C25 176.2(2) . . . . ? C22 C23 C24 C15 -173.1(2) . . . . ? C18 C23 C24 C15 2.8(3) . . . . ? C22 C23 C24 C25 3.4(3) . . . . ? C18 C23 C24 C25 179.3(2) . . . . ? C15 C24 C25 C34 56.0(3) . . . . ? C23 C24 C25 C34 -120.4(2) . . . . ? C15 C24 C25 C26 -120.2(2) . . . . ? C23 C24 C25 C26 63.4(3) . . . . ? C34 C25 C26 C27 -174.1(2) . . . . ? C24 C25 C26 C27 2.2(3) . . . . ? C34 C25 C26 C31 2.9(3) . . . . ? C24 C25 C26 C31 179.2(2) . . . . ? C31 C26 C27 C28 1.0(3) . . . . ? C25 C26 C27 C28 178.0(2) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? C27 C28 C29 C30 -1.2(4) . . . . ? C28 C29 C30 C31 0.5(4) . . . . ? C29 C30 C31 C32 -178.1(2) . . . . ? C29 C30 C31 C26 1.0(4) . . . . ? C27 C26 C31 C30 -1.7(3) . . . . ? C25 C26 C31 C30 -178.8(2) . . . . ? C27 C26 C31 C32 177.4(2) . . . . ? C25 C26 C31 C32 0.3(3) . . . . ? C30 C31 C32 C33 176.6(2) . . . . ? C26 C31 C32 C33 -2.5(4) . . . . ? C31 C32 C33 C34 1.3(3) . . . . ? C31 C32 C33 C36 -178.7(2) . . . . ? C26 C25 C34 O3 176.97(19) . . . . ? C24 C25 C34 O3 0.6(3) . . . . ? C26 C25 C34 C33 -4.2(3) . . . . ? C24 C25 C34 C33 179.4(2) . . . . ? P1 O3 C34 C25 -72.5(2) . . . . ? P1 O3 C34 C33 108.7(2) . . . . ? C32 C33 C34 C25 2.1(4) . . . . ? C36 C33 C34 C25 -177.8(2) . . . . ? C32 C33 C34 O3 -179.1(2) . . . . ? C36 C33 C34 O3 0.9(3) . . . . ? P2 O5 C37 C46 -80.4(2) . . . . ? P2 O5 C37 C38 100.3(2) . . . . ? C46 C37 C38 C39 2.4(4) . . . . ? O5 C37 C38 C39 -178.4(2) . . . . ? C46 C37 C38 C57 -177.5(2) . . . . ? O5 C37 C38 C57 1.7(3) . . . . ? C37 C38 C39 C40 0.7(4) . . . . ? C57 C38 C39 C40 -179.4(2) . . . . ? C38 C39 C40 C45 -2.2(4) . . . . ? C38 C39 C40 C41 176.3(3) . . . . ? C45 C40 C41 C42 1.5(4) . . . . ? C39 C40 C41 C42 -176.9(3) . . . . ? C40 C41 C42 C43 -0.4(5) . . . . ? C41 C42 C43 C44 -0.9(5) . . . . ? C42 C43 C44 C45 1.1(4) . . . . ? C39 C40 C45 C44 177.2(2) . . . . ? C41 C40 C45 C44 -1.3(4) . . . . ? C39 C40 C45 C46 0.7(4) . . . . ? C41 C40 C45 C46 -177.8(2) . . . . ? C43 C44 C45 C40 0.1(4) . . . . ? C43 C44 C45 C46 176.4(2) . . . . ? O5 C37 C46 C45 177.0(2) . . . . ? C38 C37 C46 C45 -3.8(4) . . . . ? O5 C37 C46 C47 1.0(3) . . . . ? C38 C37 C46 C47 -179.8(2) . . . . ? C40 C45 C46 C37 2.1(3) . . . . ? C44 C45 C46 C37 -174.2(2) . . . . ? C40 C45 C46 C47 178.0(2) . . . . ? C44 C45 C46 C47 1.7(4) . . . . ? C37 C46 C47 C56 52.9(3) . . . . ? C45 C46 C47 C56 -122.8(3) . . . . ? C37 C46 C47 C48 -126.6(3) . . . . ? C45 C46 C47 C48 57.6(3) . . . . ? C56 C47 C48 C49 -173.2(2) . . . . ? C46 C47 C48 C49 6.4(4) . . . . ? C56 C47 C48 C53 4.8(3) . . . . ? C46 C47 C48 C53 -175.6(2) . . . . ? C53 C48 C49 C50 0.9(3) . . . . ? C47 C48 C49 C50 179.0(2) . . . . ? C48 C49 C50 C51 0.1(4) . . . . ? C49 C50 C51 C52 -1.2(4) . . . . ? C50 C51 C52 C53 1.2(4) . . . . ? C51 C52 C53 C54 -178.8(2) . . . . ? C51 C52 C53 C48 -0.2(4) . . . . ? C49 C48 C53 C54 177.8(2) . . . . ? C47 C48 C53 C54 -0.3(3) . . . . ? C49 C48 C53 C52 -0.9(3) . . . . ? C47 C48 C53 C52 -179.0(2) . . . . ? C52 C53 C54 C55 175.8(2) . . . . ? C48 C53 C54 C55 -2.9(4) . . . . ? C53 C54 C55 C56 1.4(4) . . . . ? C53 C54 C55 C58 -179.9(2) . . . . ? C48 C47 C56 O6 176.6(2) . . . . ? C46 C47 C56 O6 -3.0(3) . . . . ? C48 C47 C56 C55 -6.6(4) . . . . ? C46 C47 C56 C55 173.8(2) . . . . ? P2 O6 C56 C47 -71.4(3) . . . . ? P2 O6 C56 C55 111.6(2) . . . . ? C54 C55 C56 C47 3.6(4) . . . . ? C58 C55 C56 C47 -175.1(2) . . . . ? C54 C55 C56 O6 -179.6(2) . . . . ? C58 C55 C56 O6 1.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.291 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.060 data_8a _database_code_depnum_ccdc_archive 'CCDC 815804' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H49 O4 P Si2' _chemical_formula_sum 'C40 H49 O4 P Si2' _chemical_formula_weight 680.94 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9085(4) _cell_length_b 11.2581(4) _cell_length_c 34.2755(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3823.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40935 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.30 _exptl_crystal_description cut-block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.9165 _exptl_absorpt_correction_T_max 0.9766 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40852 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9480 _reflns_number_gt 8686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.9011P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(6) _refine_ls_number_reflns 9480 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.87696(4) 0.86867(4) 0.919223(11) 0.01541(8) Uani 1 1 d . . . Si1 Si 0.70617(4) 1.12529(4) 0.986904(12) 0.01748(9) Uani 1 1 d . . . Si2 Si 0.90102(4) 0.55576(4) 0.850404(13) 0.01762(9) Uani 1 1 d . . . O1 O 0.93916(10) 0.89852(10) 0.87610(3) 0.0169(2) Uani 1 1 d . . . O2 O 1.32933(11) 1.12240(11) 0.91520(3) 0.0203(2) Uani 1 1 d . . . H2 H 1.3293 1.0683 0.9321 0.030 Uiso 1 1 calc R . . O3 O 0.75080(10) 0.96382(10) 0.91605(3) 0.0165(2) Uani 1 1 d . . . O4 O 0.80248(11) 0.74401(10) 0.90908(3) 0.0166(2) Uani 1 1 d . . . C1 C 1.13128(16) 1.01505(14) 0.89614(4) 0.0157(3) Uani 1 1 d . . . H1 H 1.1376 0.9686 0.9192 0.019 Uiso 1 1 calc R . . C2 C 1.02793(15) 0.99291(14) 0.86952(4) 0.0150(3) Uani 1 1 d . . . C3 C 1.01603(15) 1.05938(14) 0.83513(4) 0.0150(3) Uani 1 1 d . . . C4 C 1.11266(16) 1.14856(14) 0.83003(4) 0.0168(3) Uani 1 1 d . . . H4 H 1.1058 1.1954 0.8071 0.020 Uiso 1 1 calc R . . C5 C 1.21837(15) 1.17518(14) 0.85559(4) 0.0164(3) Uani 1 1 d . . . C6 C 1.22471(15) 1.10382(14) 0.88931(4) 0.0162(3) Uani 1 1 d . . . C7 C 0.90687(16) 1.03464(14) 0.80397(4) 0.0178(3) Uani 1 1 d . . . C8 C 0.92390(17) 1.11544(16) 0.76820(5) 0.0224(3) Uani 1 1 d . . . H8A H 0.8559 1.0949 0.7486 0.034 Uiso 1 1 calc R . . H8B H 1.0143 1.1045 0.7572 0.034 Uiso 1 1 calc R . . H8C H 0.9123 1.1985 0.7761 0.034 Uiso 1 1 calc R . . C9 C 0.91580(18) 0.90497(15) 0.78964(5) 0.0231(4) Uani 1 1 d . . . H9A H 0.8472 0.8912 0.7696 0.035 Uiso 1 1 calc R . . H9B H 0.9004 0.8510 0.8116 0.035 Uiso 1 1 calc R . . H9C H 1.0056 0.8904 0.7786 0.035 Uiso 1 1 calc R . . C10 C 0.76522(16) 1.05860(18) 0.82100(5) 0.0255(4) Uani 1 1 d . . . H10A H 0.7595 1.1414 0.8296 0.038 Uiso 1 1 calc R . . H10B H 0.7494 1.0057 0.8432 0.038 Uiso 1 1 calc R . . H10C H 0.6968 1.0438 0.8009 0.038 Uiso 1 1 calc R . . C11 C 1.32445(16) 1.27082(15) 0.84646(5) 0.0194(3) Uani 1 1 d . . . C12 C 1.32874(18) 1.36537(16) 0.87902(5) 0.0261(4) Uani 1 1 d . . . H12A H 1.3970 1.4253 0.8727 0.039 Uiso 1 1 calc R . . H12B H 1.3518 1.3273 0.9039 0.039 Uiso 1 1 calc R . . H12C H 1.2402 1.4035 0.8812 0.039 Uiso 1 1 calc R . . C13 C 1.29391(18) 1.33592(16) 0.80791(5) 0.0247(4) Uani 1 1 d . . . H13A H 1.2907 1.2783 0.7865 0.037 Uiso 1 1 calc R . . H13B H 1.3649 1.3944 0.8028 0.037 Uiso 1 1 calc R . . H13C H 1.2067 1.3765 0.8100 0.037 Uiso 1 1 calc R . . C14 C 1.46423(17) 1.21258(17) 0.84215(5) 0.0263(4) Uani 1 1 d . . . H14A H 1.4618 1.1546 0.8208 0.039 Uiso 1 1 calc R . . H14B H 1.4882 1.1723 0.8665 0.039 Uiso 1 1 calc R . . H14C H 1.5317 1.2738 0.8363 0.039 Uiso 1 1 calc R . . C15 C 0.62848(14) 0.93661(14) 0.93393(4) 0.0149(3) Uani 1 1 d . . . C16 C 0.59481(15) 1.00169(13) 0.96808(4) 0.0145(3) Uani 1 1 d . . . C17 C 0.47342(15) 0.97401(14) 0.98554(4) 0.0158(3) Uani 1 1 d . . . H17 H 0.4467 1.0168 1.0082 0.019 Uiso 1 1 calc R . . C18 C 0.38686(15) 0.88370(14) 0.97087(4) 0.0154(3) Uani 1 1 d . . . C19 C 0.26481(15) 0.85408(15) 0.99065(5) 0.0188(3) Uani 1 1 d . . . H19 H 0.2401 0.8962 1.0136 0.023 Uiso 1 1 calc R . . C20 C 0.18313(16) 0.76590(16) 0.97698(5) 0.0218(3) Uani 1 1 d . . . H20 H 0.1017 0.7473 0.9903 0.026 Uiso 1 1 calc R . . C21 C 0.21928(17) 0.70249(15) 0.94323(5) 0.0223(3) Uani 1 1 d . . . H21 H 0.1625 0.6404 0.9342 0.027 Uiso 1 1 calc R . . C22 C 0.33588(16) 0.72904(15) 0.92306(5) 0.0188(3) Uani 1 1 d . . . H22 H 0.3583 0.6854 0.9002 0.023 Uiso 1 1 calc R . . C23 C 0.42269(15) 0.82124(14) 0.93618(4) 0.0157(3) Uani 1 1 d . . . C24 C 0.54655(14) 0.85230(14) 0.91666(4) 0.0148(3) Uani 1 1 d . . . C25 C 0.58951(15) 0.79255(13) 0.87984(4) 0.0158(3) Uani 1 1 d . . . C26 C 0.50738(15) 0.79417(14) 0.84524(5) 0.0160(3) Uani 1 1 d . . . C27 C 0.39324(16) 0.86875(15) 0.84145(5) 0.0206(3) Uani 1 1 d . . . H27 H 0.3665 0.9171 0.8628 0.025 Uiso 1 1 calc R . . C28 C 0.32069(16) 0.87226(17) 0.80746(5) 0.0240(4) Uani 1 1 d . . . H28 H 0.2452 0.9239 0.8054 0.029 Uiso 1 1 calc R . . C29 C 0.35676(18) 0.80015(17) 0.77561(5) 0.0260(4) Uani 1 1 d . . . H29 H 0.3049 0.8022 0.7523 0.031 Uiso 1 1 calc R . . C30 C 0.46657(17) 0.72721(16) 0.77830(5) 0.0229(4) Uani 1 1 d . . . H30 H 0.4900 0.6783 0.7568 0.027 Uiso 1 1 calc R . . C31 C 0.54600(16) 0.72320(15) 0.81259(5) 0.0179(3) Uani 1 1 d . . . C32 C 0.66358(16) 0.65241(14) 0.81522(4) 0.0182(3) Uani 1 1 d . . . H32 H 0.6840 0.5996 0.7944 0.022 Uiso 1 1 calc R . . C33 C 0.74986(15) 0.65700(13) 0.84685(5) 0.0161(3) Uani 1 1 d . . . C34 C 0.71130(15) 0.73342(14) 0.87764(4) 0.0152(3) Uani 1 1 d . . . C35 C 0.61892(19) 1.19255(17) 1.02959(5) 0.0280(4) Uani 1 1 d . . . H35A H 0.6680 1.2636 1.0380 0.042 Uiso 1 1 calc R . . H35B H 0.6161 1.1350 1.0510 0.042 Uiso 1 1 calc R . . H35C H 0.5267 1.2145 1.0222 0.042 Uiso 1 1 calc R . . C36 C 0.7239(2) 1.23890(17) 0.94774(5) 0.0305(4) Uani 1 1 d . . . H36A H 0.6344 1.2602 0.9378 0.046 Uiso 1 1 calc R . . H36B H 0.7787 1.2065 0.9264 0.046 Uiso 1 1 calc R . . H36C H 0.7680 1.3098 0.9584 0.046 Uiso 1 1 calc R . . C37 C 0.87374(17) 1.06732(17) 1.00324(5) 0.0280(4) Uani 1 1 d . . . H37A H 0.9191 1.1275 1.0192 0.042 Uiso 1 1 calc R . . H37B H 0.9294 1.0491 0.9804 0.042 Uiso 1 1 calc R . . H37C H 0.8605 0.9950 1.0187 0.042 Uiso 1 1 calc R . . C38 C 1.06349(15) 0.63591(15) 0.84205(5) 0.0208(3) Uani 1 1 d . . . H38A H 1.0732 0.6994 0.8614 0.031 Uiso 1 1 calc R . . H38B H 1.0637 0.6703 0.8158 0.031 Uiso 1 1 calc R . . H38C H 1.1389 0.5801 0.8446 0.031 Uiso 1 1 calc R . . C39 C 0.9005(2) 0.48277(17) 0.89910(5) 0.0296(4) Uani 1 1 d . . . H39A H 0.9610 0.4139 0.8986 0.044 Uiso 1 1 calc R . . H39B H 0.8088 0.4566 0.9054 0.044 Uiso 1 1 calc R . . H39C H 0.9316 0.5393 0.9189 0.044 Uiso 1 1 calc R . . C40 C 0.87695(18) 0.43546(15) 0.81335(6) 0.0271(4) Uani 1 1 d . . . H40A H 0.9506 0.3778 0.8155 0.041 Uiso 1 1 calc R . . H40B H 0.8770 0.4702 0.7871 0.041 Uiso 1 1 calc R . . H40C H 0.7906 0.3954 0.8180 0.041 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 P1 0.01284(17) 0.02002(19) 0.01336(18) -0.00053(16) 0.00041(14) -0.00102(15) Si1 0.0187(2) 0.0176(2) 0.0161(2) -0.00080(18) 0.00035(16) -0.00367(18) Si2 0.0164(2) 0.0166(2) 0.0198(2) 0.00020(17) 0.00101(17) 0.00258(17) O1 0.0143(5) 0.0213(6) 0.0153(5) -0.0006(4) 0.0017(4) -0.0014(4) O2 0.0188(5) 0.0222(6) 0.0199(6) 0.0038(5) -0.0057(4) -0.0007(5) O3 0.0132(5) 0.0190(6) 0.0174(5) -0.0004(4) 0.0031(4) -0.0015(4) O4 0.0148(5) 0.0189(5) 0.0159(5) 0.0010(4) -0.0027(4) 0.0000(4) C1 0.0161(7) 0.0183(7) 0.0126(7) 0.0017(6) 0.0019(6) 0.0032(6) C2 0.0128(7) 0.0168(7) 0.0153(7) -0.0006(6) 0.0030(6) 0.0024(6) C3 0.0131(7) 0.0178(7) 0.0141(7) -0.0024(6) 0.0011(5) 0.0039(6) C4 0.0169(7) 0.0189(8) 0.0147(7) 0.0005(6) -0.0002(6) 0.0065(6) C5 0.0151(7) 0.0175(7) 0.0166(7) 0.0000(6) 0.0024(6) 0.0041(6) C6 0.0131(7) 0.0197(8) 0.0158(7) -0.0030(6) -0.0019(6) 0.0041(6) C7 0.0182(7) 0.0214(8) 0.0137(7) -0.0005(6) -0.0031(6) 0.0017(6) C8 0.0261(8) 0.0237(8) 0.0175(8) 0.0017(7) -0.0049(6) 0.0033(7) C9 0.0275(8) 0.0249(8) 0.0168(8) 0.0000(7) -0.0035(6) -0.0006(7) C10 0.0168(8) 0.0375(10) 0.0221(9) 0.0009(8) -0.0030(6) 0.0050(7) C11 0.0178(8) 0.0208(8) 0.0197(8) 0.0018(7) 0.0006(6) -0.0005(6) C12 0.0294(9) 0.0206(8) 0.0282(9) 0.0001(7) -0.0012(7) -0.0032(7) C13 0.0244(8) 0.0247(9) 0.0249(9) 0.0083(7) 0.0021(7) -0.0002(7) C14 0.0166(8) 0.0328(10) 0.0294(10) 0.0055(8) 0.0034(7) 0.0007(7) C15 0.0117(7) 0.0182(7) 0.0149(7) 0.0031(6) 0.0007(5) 0.0016(6) C16 0.0147(7) 0.0161(7) 0.0125(7) 0.0018(6) -0.0014(6) 0.0004(6) C17 0.0169(7) 0.0180(7) 0.0123(7) 0.0010(6) -0.0006(6) 0.0032(6) C18 0.0152(7) 0.0173(7) 0.0138(7) 0.0050(6) -0.0010(6) 0.0027(6) C19 0.0165(7) 0.0244(8) 0.0156(7) 0.0042(6) 0.0028(6) 0.0018(6) C20 0.0166(8) 0.0276(9) 0.0213(8) 0.0094(7) 0.0019(6) -0.0021(7) C21 0.0190(8) 0.0231(8) 0.0249(9) 0.0042(7) -0.0019(7) -0.0048(7) C22 0.0180(7) 0.0199(8) 0.0185(8) -0.0010(6) -0.0020(6) -0.0014(6) C23 0.0140(7) 0.0169(7) 0.0161(7) 0.0036(6) -0.0010(6) 0.0019(6) C24 0.0131(6) 0.0175(7) 0.0139(7) 0.0002(6) 0.0000(5) 0.0019(6) C25 0.0154(7) 0.0160(7) 0.0159(7) -0.0013(6) 0.0002(6) -0.0011(6) C26 0.0143(7) 0.0169(7) 0.0168(8) -0.0002(6) -0.0005(6) -0.0017(6) C27 0.0172(7) 0.0233(8) 0.0213(8) -0.0034(7) -0.0006(6) 0.0009(7) C28 0.0171(8) 0.0289(9) 0.0261(9) 0.0001(8) -0.0032(6) 0.0049(7) C29 0.0233(8) 0.0351(10) 0.0197(8) -0.0015(7) -0.0073(7) 0.0008(7) C30 0.0246(8) 0.0286(9) 0.0155(8) -0.0055(7) -0.0029(6) 0.0000(7) C31 0.0169(7) 0.0194(8) 0.0173(8) -0.0018(6) -0.0012(6) -0.0006(6) C32 0.0216(8) 0.0195(8) 0.0137(7) -0.0046(6) 0.0021(6) -0.0002(6) C33 0.0145(7) 0.0158(7) 0.0180(7) 0.0020(6) 0.0016(6) 0.0002(6) C34 0.0150(7) 0.0171(7) 0.0134(7) 0.0020(6) -0.0016(6) -0.0025(6) C35 0.0285(9) 0.0300(9) 0.0254(9) -0.0104(7) 0.0005(7) -0.0039(8) C36 0.0391(11) 0.0255(9) 0.0269(9) 0.0038(8) -0.0007(8) -0.0082(8) C37 0.0193(8) 0.0327(10) 0.0319(10) -0.0031(8) -0.0040(7) -0.0035(8) C38 0.0176(7) 0.0205(8) 0.0243(8) -0.0024(7) 0.0010(6) 0.0022(7) C39 0.0290(9) 0.0277(9) 0.0322(10) 0.0111(8) 0.0019(8) 0.0049(8) C40 0.0241(8) 0.0204(8) 0.0368(10) -0.0078(7) 0.0034(8) 0.0029(7) _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 P1 O4 1.6232(11) . ? P1 O1 1.6362(11) . ? P1 O3 1.6498(11) . ? Si1 C35 1.8604(18) . ? Si1 C36 1.8623(18) . ? Si1 C37 1.8698(18) . ? Si1 C16 1.8895(16) . ? Si2 C39 1.8605(18) . ? Si2 C38 1.8676(17) . ? Si2 C40 1.8721(18) . ? Si2 C33 1.8860(15) . ? O1 C2 1.3977(18) . ? O2 C6 1.3805(18) . ? O2 H2 0.8400 . ? O3 C15 1.3923(18) . ? O4 C34 1.4113(17) . ? C1 C6 1.382(2) . ? C1 C2 1.394(2) . ? C1 H1 0.9500 . ? C2 C3 1.401(2) . ? C3 C4 1.398(2) . ? C3 C7 1.545(2) . ? C4 C5 1.398(2) . ? C4 H4 0.9500 . ? C5 C6 1.409(2) . ? C5 C11 1.537(2) . ? C7 C8 1.536(2) . ? C7 C9 1.543(2) . ? C7 C10 1.544(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.539(2) . ? C11 C13 1.541(2) . ? C11 C12 1.543(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.382(2) . ? C15 C16 1.420(2) . ? C16 C17 1.379(2) . ? C17 C18 1.422(2) . ? C17 H17 0.9500 . ? C18 C19 1.426(2) . ? C18 C23 1.426(2) . ? C19 C20 1.364(2) . ? C19 H19 0.9500 . ? C20 C21 1.406(2) . ? C20 H20 0.9500 . ? C21 C22 1.379(2) . ? C21 H21 0.9500 . ? C22 C23 1.421(2) . ? C22 H22 0.9500 . ? C23 C24 1.441(2) . ? C24 C25 1.492(2) . ? C25 C34 1.380(2) . ? C25 C26 1.438(2) . ? C26 C27 1.415(2) . ? C26 C31 1.427(2) . ? C27 C28 1.370(2) . ? C27 H27 0.9500 . ? C28 C29 1.407(2) . ? C28 H28 0.9500 . ? C29 C30 1.366(2) . ? C29 H29 0.9500 . ? C30 C31 1.415(2) . ? C30 H30 0.9500 . ? C31 C32 1.414(2) . ? C32 C33 1.382(2) . ? C32 H32 0.9500 . ? C33 C34 1.414(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 P1 O1 98.94(6) . . ? O4 P1 O3 101.70(6) . . ? O1 P1 O3 95.31(6) . . ? C35 Si1 C36 109.34(9) . . ? C35 Si1 C37 108.62(9) . . ? C36 Si1 C37 111.82(9) . . ? C35 Si1 C16 107.27(8) . . ? C36 Si1 C16 108.35(8) . . ? C37 Si1 C16 111.33(8) . . ? C39 Si2 C38 110.68(8) . . ? C39 Si2 C40 106.79(9) . . ? C38 Si2 C40 110.81(8) . . ? C39 Si2 C33 108.83(8) . . ? C38 Si2 C33 112.50(7) . . ? C40 Si2 C33 106.99(8) . . ? C2 O1 P1 122.63(10) . . ? C6 O2 H2 109.5 . . ? C15 O3 P1 119.19(10) . . ? C34 O4 P1 121.84(10) . . ? C6 C1 C2 120.69(14) . . ? C6 C1 H1 119.7 . . ? C2 C1 H1 119.7 . . ? C1 C2 O1 119.50(14) . . ? C1 C2 C3 121.12(14) . . ? O1 C2 C3 119.27(13) . . ? C4 C3 C2 115.54(14) . . ? C4 C3 C7 121.48(14) . . ? C2 C3 C7 122.96(14) . . ? C5 C4 C3 126.05(14) . . ? C5 C4 H4 117.0 . . ? C3 C4 H4 117.0 . . ? C4 C5 C6 115.17(14) . . ? C4 C5 C11 122.33(14) . . ? C6 C5 C11 122.42(14) . . ? O2 C6 C1 120.24(14) . . ? O2 C6 C5 118.32(14) . . ? C1 C6 C5 121.42(14) . . ? C8 C7 C9 107.47(13) . . ? C8 C7 C10 107.35(13) . . ? C9 C7 C10 109.75(14) . . ? C8 C7 C3 111.59(13) . . ? C9 C7 C3 110.51(13) . . ? C10 C7 C3 110.09(13) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 C14 109.66(13) . . ? C5 C11 C13 111.94(13) . . ? C14 C11 C13 107.28(14) . . ? C5 C11 C12 110.78(13) . . ? C14 C11 C12 109.78(14) . . ? C13 C11 C12 107.31(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 O3 118.28(13) . . ? C24 C15 C16 124.69(14) . . ? O3 C15 C16 116.97(13) . . ? C17 C16 C15 116.47(14) . . ? C17 C16 Si1 121.84(12) . . ? C15 C16 Si1 121.61(11) . . ? C16 C17 C18 122.28(14) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C19 120.71(14) . . ? C17 C18 C23 119.82(14) . . ? C19 C18 C23 119.48(14) . . ? C20 C19 C18 120.68(15) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.07(15) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 121.06(16) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.45(15) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 118.25(14) . . ? C22 C23 C24 123.08(14) . . ? C18 C23 C24 118.65(14) . . ? C15 C24 C23 117.90(14) . . ? C15 C24 C25 120.28(13) . . ? C23 C24 C25 121.76(14) . . ? C34 C25 C26 117.11(14) . . ? C34 C25 C24 120.87(13) . . ? C26 C25 C24 122.02(13) . . ? C27 C26 C31 118.33(14) . . ? C27 C26 C25 122.39(14) . . ? C31 C26 C25 119.19(14) . . ? C28 C27 C26 120.99(15) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.68(16) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 119.79(16) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 121.21(16) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 121.93(15) . . ? C32 C31 C26 119.10(14) . . ? C30 C31 C26 118.96(15) . . ? C33 C32 C31 122.59(14) . . ? C33 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C32 C33 C34 116.18(14) . . ? C32 C33 Si2 121.29(12) . . ? C34 C33 Si2 122.28(11) . . ? C25 C34 O4 118.50(13) . . ? C25 C34 C33 124.78(14) . . ? O4 C34 C33 116.63(13) . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 P1 O1 C2 -172.54(11) . . . . ? O3 P1 O1 C2 84.71(11) . . . . ? O4 P1 O3 C15 46.30(11) . . . . ? O1 P1 O3 C15 146.59(11) . . . . ? O1 P1 O4 C34 -52.30(12) . . . . ? O3 P1 O4 C34 45.07(12) . . . . ? C6 C1 C2 O1 176.59(13) . . . . ? C6 C1 C2 C3 0.2(2) . . . . ? P1 O1 C2 C1 42.17(18) . . . . ? P1 O1 C2 C3 -141.41(12) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? O1 C2 C3 C4 -177.16(13) . . . . ? C1 C2 C3 C7 177.36(14) . . . . ? O1 C2 C3 C7 1.0(2) . . . . ? C2 C3 C4 C5 0.8(2) . . . . ? C7 C3 C4 C5 -177.43(14) . . . . ? C3 C4 C5 C6 -0.1(2) . . . . ? C3 C4 C5 C11 176.69(14) . . . . ? C2 C1 C6 O2 -177.81(14) . . . . ? C2 C1 C6 C5 0.5(2) . . . . ? C4 C5 C6 O2 177.79(13) . . . . ? C11 C5 C6 O2 1.0(2) . . . . ? C4 C5 C6 C1 -0.5(2) . . . . ? C11 C5 C6 C1 -177.32(14) . . . . ? C4 C3 C7 C8 2.0(2) . . . . ? C2 C3 C7 C8 -176.07(14) . . . . ? C4 C3 C7 C9 121.50(16) . . . . ? C2 C3 C7 C9 -56.56(19) . . . . ? C4 C3 C7 C10 -117.11(17) . . . . ? C2 C3 C7 C10 64.84(19) . . . . ? C4 C5 C11 C14 -115.51(16) . . . . ? C6 C5 C11 C14 61.1(2) . . . . ? C4 C5 C11 C13 3.4(2) . . . . ? C6 C5 C11 C13 180.00(14) . . . . ? C4 C5 C11 C12 123.16(16) . . . . ? C6 C5 C11 C12 -60.27(19) . . . . ? P1 O3 C15 C24 -74.63(16) . . . . ? P1 O3 C15 C16 107.76(13) . . . . ? C24 C15 C16 C17 2.6(2) . . . . ? O3 C15 C16 C17 179.99(13) . . . . ? C24 C15 C16 Si1 -174.22(12) . . . . ? O3 C15 C16 Si1 3.22(19) . . . . ? C35 Si1 C16 C17 -0.53(15) . . . . ? C36 Si1 C16 C17 -118.46(14) . . . . ? C37 Si1 C16 C17 118.18(13) . . . . ? C35 Si1 C16 C15 176.07(12) . . . . ? C36 Si1 C16 C15 58.14(15) . . . . ? C37 Si1 C16 C15 -65.22(14) . . . . ? C15 C16 C17 C18 1.2(2) . . . . ? Si1 C16 C17 C18 177.95(11) . . . . ? C16 C17 C18 C19 177.32(14) . . . . ? C16 C17 C18 C23 -2.2(2) . . . . ? C17 C18 C19 C20 -178.73(14) . . . . ? C23 C18 C19 C20 0.8(2) . . . . ? C18 C19 C20 C21 0.5(2) . . . . ? C19 C20 C21 C22 -1.0(3) . . . . ? C20 C21 C22 C23 0.3(2) . . . . ? C21 C22 C23 C18 0.9(2) . . . . ? C21 C22 C23 C24 179.28(15) . . . . ? C17 C18 C23 C22 178.06(14) . . . . ? C19 C18 C23 C22 -1.4(2) . . . . ? C17 C18 C23 C24 -0.4(2) . . . . ? C19 C18 C23 C24 -179.87(14) . . . . ? O3 C15 C24 C23 177.57(13) . . . . ? C16 C15 C24 C23 -5.0(2) . . . . ? O3 C15 C24 C25 0.1(2) . . . . ? C16 C15 C24 C25 177.51(14) . . . . ? C22 C23 C24 C15 -174.60(15) . . . . ? C18 C23 C24 C15 3.8(2) . . . . ? C22 C23 C24 C25 2.8(2) . . . . ? C18 C23 C24 C25 -178.82(14) . . . . ? C15 C24 C25 C34 55.7(2) . . . . ? C23 C24 C25 C34 -121.65(16) . . . . ? C15 C24 C25 C26 -124.00(17) . . . . ? C23 C24 C25 C26 58.6(2) . . . . ? C34 C25 C26 C27 -168.35(15) . . . . ? C24 C25 C26 C27 11.4(2) . . . . ? C34 C25 C26 C31 8.0(2) . . . . ? C24 C25 C26 C31 -172.24(14) . . . . ? C31 C26 C27 C28 0.5(2) . . . . ? C25 C26 C27 C28 176.96(16) . . . . ? C26 C27 C28 C29 1.0(3) . . . . ? C27 C28 C29 C30 -1.1(3) . . . . ? C28 C29 C30 C31 -0.5(3) . . . . ? C29 C30 C31 C32 -176.99(16) . . . . ? C29 C30 C31 C26 2.0(3) . . . . ? C27 C26 C31 C32 177.00(15) . . . . ? C25 C26 C31 C32 0.5(2) . . . . ? C27 C26 C31 C30 -2.0(2) . . . . ? C25 C26 C31 C30 -178.55(15) . . . . ? C30 C31 C32 C33 172.99(16) . . . . ? C26 C31 C32 C33 -6.0(2) . . . . ? C31 C32 C33 C34 2.6(2) . . . . ? C31 C32 C33 Si2 176.96(12) . . . . ? C39 Si2 C33 C32 -129.85(14) . . . . ? C38 Si2 C33 C32 107.12(14) . . . . ? C40 Si2 C33 C32 -14.80(15) . . . . ? C39 Si2 C33 C34 44.18(15) . . . . ? C38 Si2 C33 C34 -78.85(14) . . . . ? C40 Si2 C33 C34 159.23(13) . . . . ? C26 C25 C34 O4 171.28(13) . . . . ? C24 C25 C34 O4 -8.4(2) . . . . ? C26 C25 C34 C33 -12.2(2) . . . . ? C24 C25 C34 C33 168.09(14) . . . . ? P1 O4 C34 C25 -67.72(17) . . . . ? P1 O4 C34 C33 115.46(13) . . . . ? C32 C33 C34 C25 6.9(2) . . . . ? Si2 C33 C34 C25 -167.37(12) . . . . ? C32 C33 C34 O4 -176.46(13) . . . . ? Si2 C33 C34 O4 9.22(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.327 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.041 data_8b _database_code_depnum_ccdc_archive 'CCDC 815805' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H57 O4 P Si2, C6' _chemical_formula_sum 'C66 H57 O4 P Si2' _chemical_formula_weight 1001.27 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9513(10) _cell_length_b 19.713(2) _cell_length_c 28.496(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5590.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 57889 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 65.18 _exptl_crystal_description cut-block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5716 _exptl_absorpt_correction_T_max 0.7523 _exptl_absorpt_process_details 'TWINABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Microstar CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57780 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 65.18 _reflns_number_total 57780 _reflns_number_gt 50192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker PROTEUM' _computing_cell_refinement 'Bruker PROTEUM' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(10) _refine_ls_number_reflns 57780 _refine_ls_number_parameters 670 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.87261(4) 0.146663(18) 0.779602(16) 0.02298(11) Uani 1 1 d . . . Si1 Si 0.91809(4) 0.204981(19) 0.922874(18) 0.02514(11) Uani 1 1 d . . . Si2 Si 0.67532(4) 0.08046(2) 0.658746(18) 0.02665(12) Uani 1 1 d . . . O1 O 0.80639(10) 0.19568(4) 0.81886(4) 0.0217(3) Uani 1 1 d . . . O2 O 0.74244(10) 0.10162(4) 0.76157(4) 0.0240(3) Uani 1 1 d . . . O3 O 0.92840(10) 0.08764(4) 0.81457(4) 0.0232(3) Uani 1 1 d . . . O4 O 1.32251(10) 0.02708(5) 0.72785(4) 0.0306(3) Uani 1 1 d . . . H4 H 1.3252 0.0696 0.7261 0.046 Uiso 1 1 calc R . . C1 C 1.12447(14) 0.05553(7) 0.77094(6) 0.0227(4) Uani 1 1 d . . . H1 H 1.1342 0.1013 0.7610 0.027 Uiso 1 1 calc R . . C2 C 1.01842(15) 0.03772(7) 0.79983(6) 0.0230(4) Uani 1 1 d . . . C3 C 1.00312(14) -0.02829(7) 0.81670(6) 0.0217(4) Uani 1 1 d . . . C4 C 1.09867(15) -0.07464(7) 0.79997(6) 0.0241(4) Uani 1 1 d . . . H4A H 1.0900 -0.1203 0.8102 0.029 Uiso 1 1 calc R . . C5 C 1.20549(15) -0.06005(6) 0.76971(6) 0.0238(4) Uani 1 1 d . . . C6 C 1.21593(15) 0.00767(7) 0.75644(6) 0.0244(4) Uani 1 1 d . . . C7 C 0.89147(16) -0.04998(7) 0.85074(6) 0.0255(4) Uani 1 1 d . . . C8 C 0.75300(16) -0.04376(8) 0.82737(7) 0.0340(5) Uani 1 1 d . . . H8A H 0.6831 -0.0572 0.8497 0.051 Uiso 1 1 calc R . . H8B H 0.7493 -0.0734 0.7998 0.051 Uiso 1 1 calc R . . H8C H 0.7382 0.0033 0.8177 0.051 Uiso 1 1 calc R . . C9 C 0.89519(17) -0.00600(7) 0.89506(6) 0.0315(4) Uani 1 1 d . . . H9A H 0.8735 0.0410 0.8869 0.047 Uiso 1 1 calc R . . H9B H 0.9852 -0.0079 0.9089 0.047 Uiso 1 1 calc R . . H9C H 0.8293 -0.0230 0.9177 0.047 Uiso 1 1 calc R . . C10 C 0.90980(18) -0.12350(7) 0.86738(6) 0.0314(4) Uani 1 1 d . . . H10A H 0.9971 -0.1281 0.8830 0.047 Uiso 1 1 calc R . . H10B H 0.9061 -0.1541 0.8403 0.047 Uiso 1 1 calc R . . H10C H 0.8379 -0.1352 0.8895 0.047 Uiso 1 1 calc R . . C11 C 1.30730(16) -0.11516(7) 0.75414(7) 0.0296(4) Uani 1 1 d . . . C12 C 1.30886(19) -0.12075(8) 0.70085(7) 0.0412(5) Uani 1 1 d . . . H12A H 1.3360 -0.0772 0.6873 0.062 Uiso 1 1 calc R . . H12B H 1.2188 -0.1327 0.6896 0.062 Uiso 1 1 calc R . . H12C H 1.3728 -0.1560 0.6913 0.062 Uiso 1 1 calc R . . C13 C 1.44588(16) -0.09767(8) 0.77327(7) 0.0362(5) Uani 1 1 d . . . H13A H 1.5106 -0.1322 0.7632 0.054 Uiso 1 1 calc R . . H13B H 1.4426 -0.0963 0.8076 0.054 Uiso 1 1 calc R . . H13C H 1.4737 -0.0532 0.7613 0.054 Uiso 1 1 calc R . . C14 C 1.26799(17) -0.18503(7) 0.77288(7) 0.0373(5) Uani 1 1 d . . . H14A H 1.3344 -0.2187 0.7627 0.056 Uiso 1 1 calc R . . H14B H 1.1792 -0.1975 0.7607 0.056 Uiso 1 1 calc R . . H14C H 1.2651 -0.1837 0.8072 0.056 Uiso 1 1 calc R . . C15 C 0.71360(15) 0.17051(7) 0.85206(6) 0.0210(4) Uani 1 1 d . . . C16 C 0.75338(15) 0.16974(7) 0.90001(6) 0.0223(4) Uani 1 1 d . . . C17 C 0.66366(15) 0.14272(7) 0.93071(6) 0.0257(4) Uani 1 1 d . . . H17 H 0.6840 0.1442 0.9633 0.031 Uiso 1 1 calc R . . C18 C 0.54119(16) 0.11246(7) 0.91640(6) 0.0234(4) Uani 1 1 d . . . C19 C 0.45470(16) 0.07927(8) 0.94872(7) 0.0324(4) Uani 1 1 d . . . H19 H 0.4756 0.0799 0.9812 0.039 Uiso 1 1 calc R . . C20 C 0.34184(18) 0.04638(8) 0.93367(8) 0.0387(5) Uani 1 1 d . . . H20 H 0.2841 0.0246 0.9555 0.046 Uiso 1 1 calc R . . C21 C 0.31250(18) 0.04527(8) 0.88567(7) 0.0336(5) Uani 1 1 d . . . H21 H 0.2370 0.0202 0.8750 0.040 Uiso 1 1 calc R . . C22 C 0.38904(15) 0.07909(7) 0.85398(7) 0.0284(4) Uani 1 1 d . . . H22 H 0.3646 0.0787 0.8218 0.034 Uiso 1 1 calc R . . C23 C 0.50498(16) 0.11500(7) 0.86848(6) 0.0242(4) Uani 1 1 d . . . C24 C 0.59047(15) 0.14976(7) 0.83601(6) 0.0222(4) Uani 1 1 d . . . C25 C 0.54814(14) 0.16073(7) 0.78686(6) 0.0209(4) Uani 1 1 d . . . C26 C 0.42952(15) 0.19933(7) 0.77496(6) 0.0229(4) Uani 1 1 d . . . C27 C 0.35186(16) 0.23293(7) 0.80893(7) 0.0304(4) Uani 1 1 d . . . H27 H 0.3752 0.2289 0.8411 0.036 Uiso 1 1 calc R . . C28 C 0.24307(17) 0.27136(8) 0.79636(7) 0.0324(4) Uani 1 1 d . . . H28 H 0.1921 0.2936 0.8200 0.039 Uiso 1 1 calc R . . C29 C 0.20619(17) 0.27830(8) 0.74963(7) 0.0310(4) Uani 1 1 d . . . H29 H 0.1303 0.3050 0.7414 0.037 Uiso 1 1 calc R . . C30 C 0.27953(16) 0.24644(7) 0.71537(7) 0.0275(4) Uani 1 1 d . . . H30 H 0.2541 0.2512 0.6834 0.033 Uiso 1 1 calc R . . C31 C 0.39382(14) 0.20615(7) 0.72726(6) 0.0218(4) Uani 1 1 d . . . C32 C 0.46952(15) 0.17184(7) 0.69198(6) 0.0230(4) Uani 1 1 d . . . H32 H 0.4406 0.1745 0.6603 0.028 Uiso 1 1 calc R . . C33 C 0.58291(15) 0.13500(7) 0.70242(6) 0.0211(4) Uani 1 1 d . . . C34 C 0.62232(15) 0.13419(6) 0.75047(6) 0.0227(4) Uani 1 1 d . . . C35 C 1.07138(17) 0.17008(8) 0.89445(7) 0.0342(5) Uani 1 1 d . . . H35A H 1.0765 0.1863 0.8620 0.051 Uiso 1 1 calc R . . H35B H 1.0673 0.1204 0.8946 0.051 Uiso 1 1 calc R . . H35C H 1.1511 0.1851 0.9117 0.051 Uiso 1 1 calc R . . C36 C 0.91876(17) 0.29997(8) 0.91851(6) 0.0283(4) Uani 1 1 d . . . C37 C 1.04045(18) 0.33616(8) 0.91691(7) 0.0367(5) Uani 1 1 d . . . H37 H 1.1229 0.3120 0.9151 0.044 Uiso 1 1 calc R . . C38 C 1.04226(19) 0.40622(8) 0.91796(7) 0.0385(5) Uani 1 1 d . . . H38 H 1.1255 0.4298 0.9168 0.046 Uiso 1 1 calc R . . C39 C 0.9232(2) 0.44211(8) 0.92072(7) 0.0410(5) Uani 1 1 d . . . H39 H 0.9243 0.4903 0.9216 0.049 Uiso 1 1 calc R . . C40 C 0.80280(19) 0.40765(8) 0.92220(8) 0.0463(6) Uani 1 1 d . . . H40 H 0.7208 0.4322 0.9241 0.056 Uiso 1 1 calc R . . C41 C 0.80090(18) 0.33726(8) 0.92095(8) 0.0415(5) Uani 1 1 d . . . H41 H 0.7171 0.3142 0.9218 0.050 Uiso 1 1 calc R . . C42 C 0.92373(15) 0.18258(7) 0.98705(6) 0.0243(4) Uani 1 1 d . . . C43 C 0.92329(18) 0.23209(8) 1.02135(7) 0.0336(4) Uani 1 1 d . . . H43 H 0.9182 0.2784 1.0122 0.040 Uiso 1 1 calc R . . C44 C 0.9300(2) 0.21626(8) 1.06853(7) 0.0452(5) Uani 1 1 d . . . H44 H 0.9331 0.2516 1.0912 0.054 Uiso 1 1 calc R . . C45 C 0.93208(17) 0.14965(8) 1.08295(7) 0.0378(5) Uani 1 1 d . . . H45 H 0.9337 0.1388 1.1154 0.045 Uiso 1 1 calc R . . C46 C 0.93179(18) 0.09877(8) 1.04949(7) 0.0361(5) Uani 1 1 d . . . H46 H 0.9330 0.0525 1.0588 0.043 Uiso 1 1 calc R . . C47 C 0.92971(18) 0.11551(8) 1.00259(7) 0.0349(5) Uani 1 1 d . . . H47 H 0.9325 0.0801 0.9800 0.042 Uiso 1 1 calc R . . C48 C 0.67618(18) -0.00896(7) 0.68081(7) 0.0375(5) Uani 1 1 d . . . H48A H 0.7228 -0.0381 0.6582 0.056 Uiso 1 1 calc R . . H48B H 0.5835 -0.0248 0.6847 0.056 Uiso 1 1 calc R . . H48C H 0.7227 -0.0108 0.7111 0.056 Uiso 1 1 calc R . . C49 C 0.58156(16) 0.08362(7) 0.60146(6) 0.0280(4) Uani 1 1 d . . . C50 C 0.44560(17) 0.06676(7) 0.59918(7) 0.0323(4) Uani 1 1 d . . . H50 H 0.3995 0.0549 0.6272 0.039 Uiso 1 1 calc R . . C51 C 0.3759(2) 0.06686(8) 0.55683(7) 0.0384(5) Uani 1 1 d . . . H51 H 0.2829 0.0561 0.5564 0.046 Uiso 1 1 calc R . . C52 C 0.4394(2) 0.08207(9) 0.51641(8) 0.0463(5) Uani 1 1 d . . . H52 H 0.3914 0.0816 0.4876 0.056 Uiso 1 1 calc R . . C53 C 0.5738(2) 0.09824(9) 0.51695(8) 0.0514(6) Uani 1 1 d . . . H53 H 0.6185 0.1089 0.4884 0.062 Uiso 1 1 calc R . . C54 C 0.64429(19) 0.09914(8) 0.55894(7) 0.0391(5) Uani 1 1 d . . . H54 H 0.7371 0.1105 0.5588 0.047 Uiso 1 1 calc R . . C55 C 0.84966(16) 0.11209(7) 0.64922(6) 0.0300(4) Uani 1 1 d . . . C56 C 0.87291(19) 0.17646(8) 0.62969(7) 0.0421(5) Uani 1 1 d . . . H56 H 0.7992 0.2061 0.6244 0.050 Uiso 1 1 calc R . . C57 C 1.0011(2) 0.19743(9) 0.61810(9) 0.0539(6) Uani 1 1 d . . . H57 H 1.0149 0.2408 0.6043 0.065 Uiso 1 1 calc R . . C58 C 1.11024(18) 0.15476(10) 0.62672(8) 0.0489(6) Uani 1 1 d . . . H58 H 1.1986 0.1689 0.6188 0.059 Uiso 1 1 calc R . . C59 C 1.08953(19) 0.09275(10) 0.64653(8) 0.0467(5) Uani 1 1 d . . . H59 H 1.1641 0.0641 0.6529 0.056 Uiso 1 1 calc R . . C60 C 0.96166(17) 0.07099(9) 0.65745(8) 0.0413(5) Uani 1 1 d . . . H60 H 0.9494 0.0273 0.6708 0.050 Uiso 1 1 calc R . . C61 C 0.4882(8) 0.3072(3) 0.5817(3) 0.315(5) Uani 1 1 d . . . C62 C 0.3911(5) 0.26574(16) 0.56325(17) 0.1425(17) Uani 1 1 d . . . C63 C 0.4526(12) 0.2967(4) 0.51595(19) 0.339(6) Uani 1 1 d . . . C64 C 0.6541(9) 0.3185(5) 0.5520(5) 0.476(10) Uani 1 1 d . . . C65 C 0.4817(6) 0.3897(4) 0.5089(3) 0.259(4) Uani 1 1 d . . . C66 C 0.542(2) 0.3622(3) 0.5656(3) 0.633(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0223(2) 0.02417(18) 0.0224(3) -0.00035(19) 0.0011(2) 0.00289(16) Si1 0.0246(2) 0.0284(2) 0.0224(3) -0.0027(2) -0.0015(2) -0.00214(18) Si2 0.0277(2) 0.0286(2) 0.0237(3) -0.0047(2) 0.0027(2) -0.00020(18) O1 0.0204(6) 0.0240(5) 0.0207(7) -0.0029(5) 0.0011(5) -0.0020(4) O2 0.0248(6) 0.0258(5) 0.0214(7) -0.0033(5) -0.0002(5) 0.0039(4) O3 0.0234(6) 0.0214(5) 0.0247(7) -0.0008(5) -0.0003(5) 0.0027(4) O4 0.0264(6) 0.0293(5) 0.0362(8) 0.0048(6) 0.0077(6) -0.0013(5) C1 0.0210(8) 0.0221(7) 0.0250(11) 0.0027(7) 0.0001(8) 0.0005(6) C2 0.0215(9) 0.0220(7) 0.0256(12) -0.0078(7) -0.0061(8) 0.0007(6) C3 0.0194(8) 0.0241(7) 0.0218(11) 0.0000(7) -0.0041(8) -0.0016(6) C4 0.0210(9) 0.0219(7) 0.0295(11) 0.0012(7) -0.0082(8) -0.0032(6) C5 0.0198(9) 0.0236(7) 0.0280(12) -0.0030(7) -0.0052(8) 0.0011(6) C6 0.0193(9) 0.0308(8) 0.0231(12) 0.0026(8) 0.0016(8) -0.0039(7) C7 0.0251(9) 0.0259(7) 0.0254(12) -0.0017(8) 0.0021(8) -0.0002(6) C8 0.0271(10) 0.0370(9) 0.0380(14) 0.0061(9) 0.0021(9) -0.0026(7) C9 0.0389(11) 0.0331(8) 0.0226(12) 0.0015(8) 0.0021(9) 0.0008(7) C10 0.0323(10) 0.0314(8) 0.0304(12) 0.0008(8) 0.0032(9) -0.0019(7) C11 0.0268(9) 0.0269(8) 0.0351(13) -0.0015(8) 0.0001(9) 0.0019(7) C12 0.0435(11) 0.0413(9) 0.0387(14) -0.0087(9) 0.0104(10) 0.0019(8) C13 0.0297(10) 0.0393(9) 0.0397(14) 0.0036(9) 0.0051(9) 0.0104(7) C14 0.0341(10) 0.0278(8) 0.0501(15) -0.0044(9) 0.0068(10) 0.0089(7) C15 0.0231(9) 0.0204(7) 0.0195(11) -0.0005(7) 0.0027(8) 0.0017(6) C16 0.0247(9) 0.0207(7) 0.0214(12) -0.0037(7) 0.0011(8) 0.0020(6) C17 0.0312(9) 0.0298(8) 0.0160(11) -0.0045(8) -0.0003(8) 0.0022(7) C18 0.0278(9) 0.0288(8) 0.0137(11) -0.0013(8) 0.0006(8) -0.0002(7) C19 0.0348(11) 0.0407(9) 0.0218(12) 0.0011(8) -0.0023(9) -0.0095(8) C20 0.0355(11) 0.0458(10) 0.0347(14) 0.0048(9) 0.0034(10) -0.0083(8) C21 0.0281(10) 0.0341(9) 0.0386(14) -0.0009(9) 0.0023(9) -0.0079(7) C22 0.0249(9) 0.0331(8) 0.0271(12) -0.0004(8) -0.0019(8) -0.0022(7) C23 0.0253(9) 0.0245(8) 0.0228(12) -0.0019(8) -0.0001(8) -0.0003(7) C24 0.0245(9) 0.0233(7) 0.0189(11) -0.0028(7) 0.0025(8) 0.0035(7) C25 0.0205(8) 0.0240(7) 0.0183(11) -0.0022(7) -0.0033(7) -0.0012(6) C26 0.0248(8) 0.0231(7) 0.0209(11) -0.0005(8) 0.0026(8) -0.0026(6) C27 0.0308(10) 0.0375(8) 0.0230(12) -0.0025(8) 0.0005(8) 0.0040(7) C28 0.0315(10) 0.0422(9) 0.0235(12) -0.0009(8) 0.0033(9) 0.0121(8) C29 0.0266(10) 0.0345(9) 0.0319(13) 0.0023(8) -0.0021(9) 0.0093(7) C30 0.0299(9) 0.0306(8) 0.0220(12) 0.0015(8) -0.0030(8) 0.0020(7) C31 0.0204(9) 0.0238(7) 0.0211(11) -0.0003(7) 0.0033(8) -0.0014(6) C32 0.0279(9) 0.0250(7) 0.0163(11) -0.0025(7) 0.0000(8) -0.0039(7) C33 0.0206(8) 0.0255(7) 0.0172(10) -0.0005(7) 0.0011(8) -0.0021(6) C34 0.0215(8) 0.0188(7) 0.0278(12) 0.0004(7) 0.0003(8) -0.0019(6) C35 0.0300(10) 0.0360(9) 0.0367(13) -0.0059(8) -0.0004(9) -0.0007(7) C36 0.0281(9) 0.0382(8) 0.0188(11) 0.0032(8) -0.0040(8) -0.0055(7) C37 0.0356(10) 0.0376(9) 0.0370(14) -0.0035(9) 0.0062(9) -0.0021(7) C38 0.0393(11) 0.0380(9) 0.0383(14) 0.0000(9) 0.0074(10) -0.0131(8) C39 0.0520(12) 0.0317(8) 0.0392(14) 0.0075(9) -0.0027(11) -0.0067(9) C40 0.0391(11) 0.0334(9) 0.0663(17) 0.0120(10) -0.0156(11) 0.0016(8) C41 0.0307(10) 0.0392(10) 0.0547(16) -0.0002(10) -0.0130(10) -0.0033(8) C42 0.0165(8) 0.0315(8) 0.0248(11) -0.0079(8) -0.0054(8) 0.0025(6) C43 0.0443(11) 0.0293(8) 0.0273(13) -0.0021(8) -0.0001(10) -0.0017(8) C44 0.0718(14) 0.0405(10) 0.0232(14) -0.0074(9) 0.0072(11) -0.0087(9) C45 0.0397(10) 0.0510(10) 0.0225(12) 0.0037(9) 0.0000(9) -0.0071(9) C46 0.0380(10) 0.0343(9) 0.0358(14) 0.0061(9) -0.0062(10) 0.0012(8) C47 0.0425(11) 0.0296(8) 0.0326(14) -0.0049(8) 0.0005(10) 0.0025(8) C48 0.0413(11) 0.0350(8) 0.0363(14) -0.0132(9) -0.0017(10) 0.0023(8) C49 0.0279(9) 0.0291(8) 0.0271(12) -0.0022(8) 0.0014(9) -0.0001(7) C50 0.0368(11) 0.0308(8) 0.0293(13) -0.0048(8) 0.0011(9) 0.0005(7) C51 0.0424(11) 0.0364(9) 0.0365(14) -0.0052(9) -0.0092(11) 0.0004(8) C52 0.0560(14) 0.0462(10) 0.0366(15) -0.0016(10) -0.0165(11) -0.0005(10) C53 0.0765(16) 0.0617(12) 0.0161(12) 0.0023(10) 0.0015(11) -0.0163(11) C54 0.0437(12) 0.0488(10) 0.0249(13) -0.0052(9) 0.0028(10) -0.0122(8) C55 0.0305(10) 0.0317(8) 0.0279(12) -0.0105(8) 0.0019(9) -0.0020(7) C56 0.0383(11) 0.0367(9) 0.0512(16) -0.0163(9) 0.0075(10) -0.0052(8) C57 0.0508(14) 0.0391(10) 0.0719(19) -0.0163(11) 0.0090(12) -0.0171(10) C58 0.0257(11) 0.0658(13) 0.0551(16) -0.0313(11) 0.0072(10) -0.0144(10) C59 0.0294(11) 0.0696(13) 0.0411(15) -0.0119(11) -0.0057(10) 0.0036(9) C60 0.0319(11) 0.0530(11) 0.0391(14) -0.0091(10) -0.0033(10) 0.0055(8) C61 0.296(8) 0.090(3) 0.559(17) -0.013(6) 0.046(10) -0.048(4) C62 0.196(4) 0.0726(19) 0.159(4) 0.017(2) 0.085(4) 0.003(2) C63 0.696(18) 0.233(6) 0.087(4) 0.040(4) -0.004(7) 0.284(9) C64 0.303(8) 0.373(10) 0.75(2) 0.412(13) 0.322(12) 0.266(8) C65 0.232(6) 0.304(8) 0.242(7) -0.180(6) -0.134(6) 0.025(5) C66 1.42(4) 0.143(4) 0.334(11) -0.144(6) 0.573(18) -0.337(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.6185(11) . ? P1 O3 1.6294(11) . ? P1 O2 1.6524(10) . ? Si1 C35 1.8592(17) . ? Si1 C36 1.8766(16) . ? Si1 C42 1.8821(18) . ? Si1 C16 1.8958(16) . ? Si2 C55 1.8634(17) . ? Si2 C48 1.8716(16) . ? Si2 C49 1.8814(19) . ? Si2 C33 1.8844(16) . ? O1 C15 1.4120(18) . ? O2 C34 1.3932(17) . ? O3 C2 1.3954(17) . ? O4 C6 1.3911(18) . ? O4 H4 0.8400 . ? C1 C6 1.374(2) . ? C1 C2 1.384(2) . ? C1 H1 0.9500 . ? C2 C3 1.396(2) . ? C3 C4 1.402(2) . ? C3 C7 1.536(2) . ? C4 C5 1.399(2) . ? C4 H4A 0.9500 . ? C5 C6 1.391(2) . ? C5 C11 1.550(2) . ? C7 C9 1.533(2) . ? C7 C8 1.535(2) . ? C7 C10 1.536(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.522(2) . ? C11 C12 1.523(3) . ? C11 C14 1.528(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.370(2) . ? C15 C16 1.423(2) . ? C16 C17 1.359(2) . ? C17 C18 1.417(2) . ? C17 H17 0.9500 . ? C18 C23 1.413(2) . ? C18 C19 1.420(2) . ? C19 C20 1.366(2) . ? C19 H19 0.9500 . ? C20 C21 1.399(3) . ? C20 H20 0.9500 . ? C21 C22 1.357(2) . ? C21 H21 0.9500 . ? C22 C23 1.415(2) . ? C22 H22 0.9500 . ? C23 C24 1.432(2) . ? C24 C25 1.478(2) . ? C25 C34 1.376(2) . ? C25 C26 1.445(2) . ? C26 C27 1.405(2) . ? C26 C31 1.411(2) . ? C27 C28 1.369(2) . ? C27 H27 0.9500 . ? C28 C29 1.388(2) . ? C28 H28 0.9500 . ? C29 C30 1.371(2) . ? C29 H29 0.9500 . ? C30 C31 1.428(2) . ? C30 H30 0.9500 . ? C31 C32 1.427(2) . ? C32 C33 1.374(2) . ? C32 H32 0.9500 . ? C33 C34 1.424(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C41 1.386(2) . ? C36 C37 1.406(2) . ? C37 C38 1.382(2) . ? C37 H37 0.9500 . ? C38 C39 1.382(3) . ? C38 H38 0.9500 . ? C39 C40 1.378(2) . ? C39 H39 0.9500 . ? C40 C41 1.388(2) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.381(2) . ? C42 C47 1.396(2) . ? C43 C44 1.382(3) . ? C43 H43 0.9500 . ? C44 C45 1.376(2) . ? C44 H44 0.9500 . ? C45 C46 1.384(2) . ? C45 H45 0.9500 . ? C46 C47 1.377(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.395(2) . ? C49 C54 1.397(2) . ? C50 C51 1.392(3) . ? C50 H50 0.9500 . ? C51 C52 1.348(3) . ? C51 H51 0.9500 . ? C52 C53 1.374(3) . ? C52 H52 0.9500 . ? C53 C54 1.387(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.398(2) . ? C55 C56 1.405(2) . ? C56 C57 1.381(3) . ? C56 H56 0.9500 . ? C57 C58 1.396(3) . ? C57 H57 0.9500 . ? C58 C59 1.362(3) . ? C58 H58 0.9500 . ? C59 C60 1.378(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.295(8) . ? C61 C62 1.371(8) . ? C61 C64 1.869(10) . ? C61 C63 1.918(10) . ? C62 C63 1.601(8) . ? C63 C65 1.868(11) . ? C64 C66 1.459(15) . ? C65 C66 1.808(15) . ? 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 O1 P1 O3 98.18(6) . . ? O1 P1 O2 102.50(5) . . ? O3 P1 O2 94.22(5) . . ? C35 Si1 C36 109.72(7) . . ? C35 Si1 C42 108.18(8) . . ? C36 Si1 C42 107.36(7) . . ? C35 Si1 C16 115.09(7) . . ? C36 Si1 C16 110.24(7) . . ? C42 Si1 C16 105.89(7) . . ? C55 Si2 C48 111.09(7) . . ? C55 Si2 C49 108.92(8) . . ? C48 Si2 C49 108.97(8) . . ? C55 Si2 C33 111.07(7) . . ? C48 Si2 C33 108.52(8) . . ? C49 Si2 C33 108.19(7) . . ? C15 O1 P1 121.30(8) . . ? C34 O2 P1 119.71(8) . . ? C2 O3 P1 122.57(10) . . ? C6 O4 H4 109.5 . . ? C6 C1 C2 120.65(13) . . ? C6 C1 H1 119.7 . . ? C2 C1 H1 119.7 . . ? C1 C2 O3 119.32(12) . . ? C1 C2 C3 121.65(13) . . ? O3 C2 C3 118.94(14) . . ? C2 C3 C4 114.61(15) . . ? C2 C3 C7 123.79(13) . . ? C4 C3 C7 121.59(13) . . ? C5 C4 C3 126.22(13) . . ? C5 C4 H4A 116.9 . . ? C3 C4 H4A 116.9 . . ? C6 C5 C4 114.93(13) . . ? C6 C5 C11 123.08(14) . . ? C4 C5 C11 121.94(12) . . ? C1 C6 O4 119.49(12) . . ? C1 C6 C5 121.83(14) . . ? O4 C6 C5 118.68(13) . . ? C9 C7 C8 109.51(13) . . ? C9 C7 C3 110.22(13) . . ? C8 C7 C3 110.68(14) . . ? C9 C7 C10 106.04(14) . . ? C8 C7 C10 108.42(12) . . ? C3 C7 C10 111.84(12) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 111.37(16) . . ? C13 C11 C14 108.11(14) . . ? C12 C11 C14 106.62(14) . . ? C13 C11 C5 109.32(13) . . ? C12 C11 C5 110.05(14) . . ? C14 C11 C5 111.36(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 O1 117.77(15) . . ? C24 C15 C16 124.49(15) . . ? O1 C15 C16 117.73(13) . . ? C17 C16 C15 116.09(14) . . ? C17 C16 Si1 119.37(13) . . ? C15 C16 Si1 124.53(12) . . ? C16 C17 C18 123.02(17) . . ? C16 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C23 C18 C17 118.85(15) . . ? C23 C18 C19 119.23(15) . . ? C17 C18 C19 121.92(17) . . ? C20 C19 C18 120.90(18) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.08(17) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 121.74(17) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.62(18) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 118.18(15) . . ? C18 C23 C24 119.34(15) . . ? C22 C23 C24 122.36(16) . . ? C15 C24 C23 117.29(16) . . ? C15 C24 C25 121.83(15) . . ? C23 C24 C25 120.86(14) . . ? C34 C25 C26 117.49(15) . . ? C34 C25 C24 120.35(13) . . ? C26 C25 C24 122.15(14) . . ? C27 C26 C31 118.71(15) . . ? C27 C26 C25 122.42(16) . . ? C31 C26 C25 118.81(14) . . ? C28 C27 C26 121.04(18) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.98(17) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 119.81(15) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.64(17) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C26 C31 C32 120.04(14) . . ? C26 C31 C30 118.82(15) . . ? C32 C31 C30 121.13(16) . . ? C33 C32 C31 122.10(16) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 116.11(15) . . ? C32 C33 Si2 124.00(13) . . ? C34 C33 Si2 119.61(11) . . ? C25 C34 O2 117.66(15) . . ? C25 C34 C33 124.91(14) . . ? O2 C34 C33 117.37(14) . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 117.46(14) . . ? C41 C36 Si1 121.53(12) . . ? C37 C36 Si1 120.76(12) . . ? C38 C37 C36 121.18(16) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.11(15) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.66(14) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.26(16) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C36 C41 C40 121.33(15) . . ? C36 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C43 C42 C47 116.42(17) . . ? C43 C42 Si1 121.44(12) . . ? C47 C42 Si1 122.13(13) . . ? C42 C43 C44 121.92(16) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C45 C44 C43 120.45(18) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 119.08(19) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? C47 C46 C45 119.67(16) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C42 122.39(17) . . ? C46 C47 H47 118.8 . . ? C42 C47 H47 118.8 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C54 116.44(17) . . ? C50 C49 Si2 120.91(14) . . ? C54 C49 Si2 122.56(13) . . ? C51 C50 C49 121.56(19) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C52 C51 C50 120.51(19) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 119.9(2) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C52 C53 C54 120.3(2) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C49 121.28(18) . . ? C53 C54 H54 119.4 . . ? C49 C54 H54 119.4 . . ? C60 C55 C56 117.31(16) . . ? C60 C55 Si2 121.60(12) . . ? C56 C55 Si2 120.88(13) . . ? C57 C56 C55 121.15(17) . . ? C57 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C56 C57 C58 119.76(18) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C59 C58 C57 119.74(17) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C58 C59 C60 120.83(18) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C59 C60 C55 121.18(18) . . ? C59 C60 H60 119.4 . . ? C55 C60 H60 119.4 . . ? C66 C61 C62 131.0(12) . . ? C66 C61 C64 51.1(7) . . ? C62 C61 C64 121.3(9) . . ? C66 C61 C63 79.6(8) . . ? C62 C61 C63 55.3(5) . . ? C64 C61 C63 74.5(7) . . ? C61 C62 C63 80.0(6) . . ? C62 C63 C65 121.6(4) . . ? C62 C63 C61 44.7(3) . . ? C65 C63 C61 88.3(5) . . ? C66 C64 C61 43.7(3) . . ? C66 C65 C63 70.1(5) . . ? C61 C66 C64 85.2(7) . . ? C61 C66 C65 115.5(13) . . ? C64 C66 C65 101.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C15 -52.76(11) . . . . ? O2 P1 O1 C15 43.44(12) . . . . ? O1 P1 O2 C34 47.33(13) . . . . ? O3 P1 O2 C34 146.68(12) . . . . ? O1 P1 O3 C2 -167.31(10) . . . . ? O2 P1 O3 C2 89.40(11) . . . . ? C6 C1 C2 O3 178.99(14) . . . . ? C6 C1 C2 C3 2.5(3) . . . . ? P1 O3 C2 C1 41.69(18) . . . . ? P1 O3 C2 C3 -141.71(13) . . . . ? C1 C2 C3 C4 -3.3(2) . . . . ? O3 C2 C3 C4 -179.80(13) . . . . ? C1 C2 C3 C7 176.87(15) . . . . ? O3 C2 C3 C7 0.4(2) . . . . ? C2 C3 C4 C5 1.4(2) . . . . ? C7 C3 C4 C5 -178.74(15) . . . . ? C3 C4 C5 C6 1.3(2) . . . . ? C3 C4 C5 C11 178.79(16) . . . . ? C2 C1 C6 O4 -179.26(15) . . . . ? C2 C1 C6 C5 0.5(3) . . . . ? C4 C5 C6 C1 -2.2(2) . . . . ? C11 C5 C6 C1 -179.72(16) . . . . ? C4 C5 C6 O4 177.52(14) . . . . ? C11 C5 C6 O4 0.0(2) . . . . ? C2 C3 C7 C9 -55.8(2) . . . . ? C4 C3 C7 C9 124.38(16) . . . . ? C2 C3 C7 C8 65.5(2) . . . . ? C4 C3 C7 C8 -114.33(16) . . . . ? C2 C3 C7 C10 -173.49(15) . . . . ? C4 C3 C7 C10 6.7(2) . . . . ? C6 C5 C11 C13 62.3(2) . . . . ? C4 C5 C11 C13 -115.06(17) . . . . ? C6 C5 C11 C12 -60.4(2) . . . . ? C4 C5 C11 C12 122.33(17) . . . . ? C6 C5 C11 C14 -178.36(16) . . . . ? C4 C5 C11 C14 4.3(2) . . . . ? P1 O1 C15 C24 -67.70(15) . . . . ? P1 O1 C15 C16 113.58(12) . . . . ? C24 C15 C16 C17 3.9(2) . . . . ? O1 C15 C16 C17 -177.49(12) . . . . ? C24 C15 C16 Si1 -174.79(11) . . . . ? O1 C15 C16 Si1 3.84(18) . . . . ? C35 Si1 C16 C17 126.25(13) . . . . ? C36 Si1 C16 C17 -109.02(12) . . . . ? C42 Si1 C16 C17 6.81(13) . . . . ? C35 Si1 C16 C15 -55.13(14) . . . . ? C36 Si1 C16 C15 69.61(13) . . . . ? C42 Si1 C16 C15 -174.57(12) . . . . ? C15 C16 C17 C18 4.3(2) . . . . ? Si1 C16 C17 C18 -176.96(10) . . . . ? C16 C17 C18 C23 -5.1(2) . . . . ? C16 C17 C18 C19 174.32(14) . . . . ? C23 C18 C19 C20 4.0(2) . . . . ? C17 C18 C19 C20 -175.40(14) . . . . ? C18 C19 C20 C21 0.5(2) . . . . ? C19 C20 C21 C22 -3.7(3) . . . . ? C20 C21 C22 C23 2.3(2) . . . . ? C17 C18 C23 C22 174.10(13) . . . . ? C19 C18 C23 C22 -5.4(2) . . . . ? C17 C18 C23 C24 -2.0(2) . . . . ? C19 C18 C23 C24 178.59(13) . . . . ? C21 C22 C23 C18 2.3(2) . . . . ? C21 C22 C23 C24 178.24(14) . . . . ? O1 C15 C24 C23 170.80(12) . . . . ? C16 C15 C24 C23 -10.6(2) . . . . ? O1 C15 C24 C25 -7.42(19) . . . . ? C16 C15 C24 C25 171.21(13) . . . . ? C18 C23 C24 C15 9.3(2) . . . . ? C22 C23 C24 C15 -166.60(13) . . . . ? C18 C23 C24 C25 -172.48(13) . . . . ? C22 C23 C24 C25 11.6(2) . . . . ? C15 C24 C25 C34 58.68(19) . . . . ? C23 C24 C25 C34 -119.48(16) . . . . ? C15 C24 C25 C26 -121.06(15) . . . . ? C23 C24 C25 C26 60.79(18) . . . . ? C34 C25 C26 C27 -175.19(13) . . . . ? C24 C25 C26 C27 4.6(2) . . . . ? C34 C25 C26 C31 1.81(19) . . . . ? C24 C25 C26 C31 -178.45(13) . . . . ? C31 C26 C27 C28 0.3(2) . . . . ? C25 C26 C27 C28 177.34(14) . . . . ? C26 C27 C28 C29 0.0(2) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? C28 C29 C30 C31 -0.1(2) . . . . ? C27 C26 C31 C32 -179.07(13) . . . . ? C25 C26 C31 C32 3.8(2) . . . . ? C27 C26 C31 C30 -0.5(2) . . . . ? C25 C26 C31 C30 -177.64(12) . . . . ? C29 C30 C31 C26 0.4(2) . . . . ? C29 C30 C31 C32 178.93(14) . . . . ? C26 C31 C32 C33 -4.1(2) . . . . ? C30 C31 C32 C33 177.38(13) . . . . ? C31 C32 C33 C34 -1.3(2) . . . . ? C31 C32 C33 Si2 172.58(11) . . . . ? C55 Si2 C33 C32 117.31(13) . . . . ? C48 Si2 C33 C32 -120.29(13) . . . . ? C49 Si2 C33 C32 -2.20(14) . . . . ? C55 Si2 C33 C34 -69.03(13) . . . . ? C48 Si2 C33 C34 53.37(13) . . . . ? C49 Si2 C33 C34 171.46(11) . . . . ? C26 C25 C34 O2 174.97(11) . . . . ? C24 C25 C34 O2 -4.78(19) . . . . ? C26 C25 C34 C33 -7.8(2) . . . . ? C24 C25 C34 C33 172.48(13) . . . . ? P1 O2 C34 C25 -71.18(15) . . . . ? P1 O2 C34 C33 111.35(13) . . . . ? C32 C33 C34 C25 7.5(2) . . . . ? Si2 C33 C34 C25 -166.62(11) . . . . ? C32 C33 C34 O2 -175.21(11) . . . . ? Si2 C33 C34 O2 10.64(17) . . . . ? C35 Si1 C36 C41 156.54(16) . . . . ? C42 Si1 C36 C41 -86.12(17) . . . . ? C16 Si1 C36 C41 28.78(18) . . . . ? C35 Si1 C36 C37 -29.28(18) . . . . ? C42 Si1 C36 C37 88.07(16) . . . . ? C16 Si1 C36 C37 -157.04(15) . . . . ? C41 C36 C37 C38 0.3(3) . . . . ? Si1 C36 C37 C38 -174.11(15) . . . . ? C36 C37 C38 C39 0.1(3) . . . . ? C37 C38 C39 C40 -0.3(3) . . . . ? C38 C39 C40 C41 0.0(3) . . . . ? C37 C36 C41 C40 -0.6(3) . . . . ? Si1 C36 C41 C40 173.81(16) . . . . ? C39 C40 C41 C36 0.4(3) . . . . ? C35 Si1 C42 C43 120.36(14) . . . . ? C36 Si1 C42 C43 2.01(15) . . . . ? C16 Si1 C42 C43 -115.76(14) . . . . ? C35 Si1 C42 C47 -59.09(15) . . . . ? C36 Si1 C42 C47 -177.44(14) . . . . ? C16 Si1 C42 C47 64.80(15) . . . . ? C47 C42 C43 C44 0.7(3) . . . . ? Si1 C42 C43 C44 -178.75(15) . . . . ? C42 C43 C44 C45 -2.5(3) . . . . ? C43 C44 C45 C46 2.1(3) . . . . ? C44 C45 C46 C47 0.1(3) . . . . ? C45 C46 C47 C42 -2.0(3) . . . . ? C43 C42 C47 C46 1.5(3) . . . . ? Si1 C42 C47 C46 -178.98(14) . . . . ? C55 Si2 C49 C50 -175.89(12) . . . . ? C48 Si2 C49 C50 62.77(14) . . . . ? C33 Si2 C49 C50 -55.04(13) . . . . ? C55 Si2 C49 C54 7.61(15) . . . . ? C48 Si2 C49 C54 -113.73(14) . . . . ? C33 Si2 C49 C54 128.46(13) . . . . ? C54 C49 C50 C51 -1.3(2) . . . . ? Si2 C49 C50 C51 -178.01(11) . . . . ? C49 C50 C51 C52 1.4(2) . . . . ? C50 C51 C52 C53 -0.6(3) . . . . ? C51 C52 C53 C54 -0.1(3) . . . . ? C52 C53 C54 C49 0.2(3) . . . . ? C50 C49 C54 C53 0.6(2) . . . . ? Si2 C49 C54 C53 177.20(13) . . . . ? C48 Si2 C55 C60 1.06(19) . . . . ? C49 Si2 C55 C60 -118.97(16) . . . . ? C33 Si2 C55 C60 121.96(16) . . . . ? C48 Si2 C55 C56 175.64(15) . . . . ? C49 Si2 C55 C56 55.61(17) . . . . ? C33 Si2 C55 C56 -63.46(17) . . . . ? C60 C55 C56 C57 1.5(3) . . . . ? Si2 C55 C56 C57 -173.30(16) . . . . ? C55 C56 C57 C58 -1.3(3) . . . . ? C56 C57 C58 C59 0.0(3) . . . . ? C57 C58 C59 C60 1.2(3) . . . . ? C58 C59 C60 C55 -0.9(3) . . . . ? C56 C55 C60 C59 -0.4(3) . . . . ? Si2 C55 C60 C59 174.38(16) . . . . ? C66 C61 C62 C63 26.9(11) . . . . ? C64 C61 C62 C63 -36.7(5) . . . . ? C61 C62 C63 C65 -47.9(7) . . . . ? C66 C61 C63 C62 -159.7(10) . . . . ? C64 C61 C63 C62 148.0(5) . . . . ? C66 C61 C63 C65 -18.9(10) . . . . ? C62 C61 C63 C65 140.8(5) . . . . ? C64 C61 C63 C65 -71.2(5) . . . . ? C62 C61 C64 C66 119.7(14) . . . . ? C63 C61 C64 C66 89.1(12) . . . . ? C62 C63 C65 C66 45.6(9) . . . . ? C61 C63 C65 C66 14.1(7) . . . . ? C62 C61 C66 C64 -100.6(17) . . . . ? C63 C61 C66 C64 -78.4(10) . . . . ? C62 C61 C66 C65 -0.4(16) . . . . ? C64 C61 C66 C65 100.2(7) . . . . ? C63 C61 C66 C65 21.8(8) . . . . ? C61 C64 C66 C65 -115.0(12) . . . . ? C63 C65 C66 C61 -23.5(9) . . . . ? C63 C65 C66 C64 66.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 65.18 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.742 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.066 data_10c _database_code_depnum_ccdc_archive 'CCDC 815806' #TrackingRef '- all DT-ART-03-2011-010356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H69 Cl O4 P2 Pd Si2, 2(C4 H8 O), C6 H12' _chemical_formula_sum 'C96 H99 Cl O6 P2 Pd Si2' _chemical_formula_weight 1608.72 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.5371(3) _cell_length_b 23.2484(5) _cell_length_c 14.3898(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.0080(10) _cell_angle_gamma 90.00 _cell_volume 4136.91(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 147708 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 33.32 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8359 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 147604 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 33.32 _reflns_number_total 31588 _reflns_number_gt 29279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+1.1792P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(9) _refine_ls_number_reflns 31588 _refine_ls_number_parameters 1036 _refine_ls_number_restraints 277 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.260129(9) 0.676734(5) 0.770696(9) 0.01303(3) Uani 1 1 d . . . P1 P 0.28719(4) 0.771353(18) 0.76073(3) 0.01300(7) Uani 1 1 d . . . P2 P 0.18544(4) 0.58830(2) 0.72789(4) 0.01721(9) Uani 1 1 d . . . Si1 Si 0.10411(4) 0.87070(2) 0.88222(4) 0.01534(9) Uani 1 1 d . . . Si2 Si 0.54941(4) 0.71907(2) 0.69522(4) 0.01699(9) Uani 1 1 d . . . Cl1 Cl 0.40418(4) 0.65498(2) 0.92741(4) 0.02515(9) Uani 1 1 d . . . O1 O 0.18424(11) 0.79513(6) 0.66555(11) 0.0171(2) Uani 1 1 d . . . O2 O 0.08081(12) 0.59646(6) 0.62035(12) 0.0220(3) Uani 1 1 d . . . O3 O 0.29682(11) 0.80818(5) 0.85758(10) 0.0145(2) Uani 1 1 d . . . O4 O 0.37674(11) 0.80059(6) 0.72897(10) 0.0153(2) Uani 1 1 d . . . C1 C 0.13352(14) 0.69560(8) 0.64076(13) 0.0146(3) Uani 1 1 d . . . C2 C 0.11366(15) 0.75217(8) 0.60562(13) 0.0155(3) Uani 1 1 d . . . C3 C 0.02980(16) 0.76798(9) 0.51467(14) 0.0196(3) Uani 1 1 d . . . C4 C -0.04083(17) 0.72295(10) 0.46345(15) 0.0239(4) Uani 1 1 d . . . H4 H -0.1005 0.7322 0.4018 0.029 Uiso 1 1 calc R . . C5 C -0.03066(16) 0.66580(9) 0.49555(15) 0.0229(4) Uani 1 1 d . . . C6 C 0.06074(16) 0.65336(9) 0.58464(15) 0.0189(3) Uani 1 1 d . . . C7 C 0.01488(18) 0.83005(10) 0.47389(16) 0.0248(4) Uani 1 1 d . . . C8 C -0.00727(18) 0.87095(9) 0.54679(16) 0.0252(4) Uani 1 1 d . . . H8A H -0.0769 0.8612 0.5486 0.038 Uiso 1 1 calc R . . H8B H -0.0095 0.9107 0.5231 0.038 Uiso 1 1 calc R . . H8C H 0.0504 0.8671 0.6152 0.038 Uiso 1 1 calc R . . C9 C 0.1170(2) 0.85022(12) 0.4604(2) 0.0364(6) Uani 1 1 d . . . H9A H 0.1077 0.8903 0.4373 0.055 Uiso 1 1 calc R . . H9B H 0.1280 0.8259 0.4098 0.055 Uiso 1 1 calc R . . H9C H 0.1800 0.8472 0.5255 0.055 Uiso 1 1 calc R . . C10 C -0.0807(2) 0.83459(13) 0.36930(18) 0.0367(6) Uani 1 1 d . . . H10A H -0.1472 0.8221 0.3750 0.055 Uiso 1 1 calc R . . H10B H -0.0672 0.8100 0.3204 0.055 Uiso 1 1 calc R . . H10C H -0.0888 0.8746 0.3458 0.055 Uiso 1 1 calc R . . C11 C -0.11796(18) 0.62054(11) 0.43989(19) 0.0310(5) Uani 1 1 d . . . C12 C -0.2098(2) 0.64606(14) 0.3465(2) 0.0423(7) Uani 1 1 d . . . H12A H -0.1811 0.6596 0.2979 0.063 Uiso 1 1 calc R . . H12B H -0.2424 0.6784 0.3675 0.063 Uiso 1 1 calc R . . H12C H -0.2649 0.6165 0.3143 0.063 Uiso 1 1 calc R . . C13 C -0.0698(2) 0.56999(12) 0.4026(2) 0.0389(6) Uani 1 1 d . . . H13A H -0.1277 0.5433 0.3630 0.058 Uiso 1 1 calc R . . H13B H -0.0163 0.5498 0.4613 0.058 Uiso 1 1 calc R . . H13C H -0.0347 0.5848 0.3598 0.058 Uiso 1 1 calc R . . C14 C -0.1681(2) 0.59908(14) 0.5132(3) 0.0426(7) Uani 1 1 d . . . H14A H -0.2078 0.6306 0.5277 0.064 Uiso 1 1 calc R . . H14B H -0.1104 0.5859 0.5769 0.064 Uiso 1 1 calc R . . H14C H -0.2177 0.5672 0.4815 0.064 Uiso 1 1 calc R . . C15 C 0.30970(14) 0.86842(7) 0.85977(13) 0.0139(3) Uani 1 1 d . . . C16 C 0.22224(15) 0.90131(7) 0.86098(14) 0.0159(3) Uani 1 1 d . . . C17 C 0.23667(16) 0.96052(8) 0.86471(15) 0.0169(3) Uani 1 1 d . . . H17 H 0.1810 0.9844 0.8674 0.020 Uiso 1 1 calc R . . C18 C 0.33096(15) 0.98673(7) 0.86469(14) 0.0163(3) Uani 1 1 d . . . C19 C 0.34119(17) 1.04777(8) 0.86602(15) 0.0191(3) Uani 1 1 d . . . H19 H 0.2839 1.0710 0.8670 0.023 Uiso 1 1 calc R . . C20 C 0.43201(18) 1.07333(8) 0.86590(16) 0.0221(4) Uani 1 1 d . . . H20 H 0.4380 1.1141 0.8672 0.027 Uiso 1 1 calc R . . C21 C 0.51700(17) 1.03875(9) 0.86389(17) 0.0225(4) Uani 1 1 d . . . H21 H 0.5803 1.0565 0.8642 0.027 Uiso 1 1 calc R . . C22 C 0.50919(16) 0.97971(8) 0.86154(15) 0.0195(3) Uani 1 1 d . . . H22 H 0.5661 0.9573 0.8577 0.023 Uiso 1 1 calc R . . C23 C 0.41742(15) 0.95180(7) 0.86478(13) 0.0153(3) Uani 1 1 d . . . C24 C 0.40734(14) 0.89037(7) 0.86665(14) 0.0146(3) Uani 1 1 d . . . C25 C 0.49830(15) 0.85124(7) 0.87547(14) 0.0153(3) Uani 1 1 d . . . C26 C 0.60397(15) 0.85690(8) 0.95495(14) 0.0171(3) Uani 1 1 d . . . C27 C 0.62861(16) 0.89622(8) 1.03765(15) 0.0197(3) Uani 1 1 d . . . H27 H 0.5728 0.9193 1.0420 0.024 Uiso 1 1 calc R . . C28 C 0.73208(18) 0.90101(9) 1.11091(16) 0.0239(4) Uani 1 1 d . . . H28 H 0.7470 0.9274 1.1654 0.029 Uiso 1 1 calc R . . C29 C 0.81665(17) 0.86716(10) 1.10616(16) 0.0241(4) Uani 1 1 d . . . H29 H 0.8885 0.8719 1.1558 0.029 Uiso 1 1 calc R . . C30 C 0.79483(16) 0.82737(9) 1.02961(16) 0.0231(4) Uani 1 1 d . . . H30 H 0.8516 0.8040 1.0277 0.028 Uiso 1 1 calc R . . C31 C 0.68835(15) 0.82079(8) 0.95335(15) 0.0192(3) Uani 1 1 d . . . C32 C 0.66547(17) 0.77927(9) 0.87584(17) 0.0203(4) Uani 1 1 d . . . H32 H 0.7229 0.7560 0.8752 0.024 Uiso 1 1 calc R . . C33 C 0.56284(15) 0.77099(8) 0.80073(15) 0.0177(3) Uani 1 1 d . . . C34 C 0.48162(14) 0.80756(8) 0.80537(14) 0.0155(3) Uani 1 1 d . . . C35 C 0.14760(16) 0.87049(8) 1.02456(15) 0.0182(3) Uani 1 1 d . . . C36 C 0.23604(18) 0.90255(9) 1.09028(16) 0.0229(4) Uani 1 1 d . . . H36 H 0.2747 0.9262 1.0627 0.027 Uiso 1 1 calc R . . C37 C 0.2686(2) 0.90046(11) 1.19578(17) 0.0294(4) Uani 1 1 d . . . H37 H 0.3288 0.9225 1.2390 0.035 Uiso 1 1 calc R . . C38 C 0.2128(2) 0.86611(12) 1.23739(18) 0.0323(5) Uani 1 1 d . . . H38 H 0.2346 0.8648 1.3090 0.039 Uiso 1 1 calc R . . C39 C 0.1252(2) 0.83380(11) 1.17383(19) 0.0312(5) Uani 1 1 d . . . H39 H 0.0869 0.8103 1.2020 0.037 Uiso 1 1 calc R . . C40 C 0.09316(18) 0.83570(10) 1.06856(17) 0.0244(4) Uani 1 1 d . . . H40 H 0.0335 0.8131 1.0259 0.029 Uiso 1 1 calc R . . C41 C -0.01838(16) 0.91794(8) 0.81665(16) 0.0193(3) Uani 1 1 d . . . C42 C -0.10634(18) 0.91206(10) 0.84380(18) 0.0258(4) Uani 1 1 d . . . H42 H -0.1002 0.8872 0.8982 0.031 Uiso 1 1 calc R . . C43 C -0.20255(19) 0.94201(12) 0.7925(2) 0.0350(5) Uani 1 1 d . . . H43 H -0.2611 0.9374 0.8122 0.042 Uiso 1 1 calc R . . C44 C -0.2129(2) 0.97849(12) 0.7130(2) 0.0377(6) Uani 1 1 d . . . H44 H -0.2783 0.9991 0.6784 0.045 Uiso 1 1 calc R . . C45 C -0.1271(2) 0.98475(10) 0.6840(2) 0.0315(5) Uani 1 1 d . . . H45 H -0.1338 1.0096 0.6294 0.038 Uiso 1 1 calc R . . C46 C -0.03133(17) 0.95448(9) 0.73532(17) 0.0235(4) Uani 1 1 d . . . H46 H 0.0265 0.9588 0.7146 0.028 Uiso 1 1 calc R . . C47 C 0.05954(16) 0.79538(8) 0.83879(15) 0.0179(3) Uani 1 1 d . . . C48 C 0.11585(17) 0.74786(8) 0.89663(17) 0.0215(4) Uani 1 1 d . . . H48 H 0.1815 0.7538 0.9546 0.026 Uiso 1 1 calc R . . C49 C 0.0767(2) 0.69216(9) 0.87013(19) 0.0260(4) Uani 1 1 d . . . H49 H 0.1154 0.6605 0.9102 0.031 Uiso 1 1 calc R . . C50 C -0.01920(19) 0.68277(10) 0.7848(2) 0.0306(5) Uani 1 1 d . . . H50 H -0.0461 0.6448 0.7670 0.037 Uiso 1 1 calc R . . C51 C -0.07501(19) 0.72862(10) 0.7261(2) 0.0277(4) Uani 1 1 d . . . H51 H -0.1398 0.7222 0.6674 0.033 Uiso 1 1 calc R . . C52 C -0.03606(17) 0.78474(9) 0.75324(17) 0.0222(4) Uani 1 1 d . . . H52 H -0.0753 0.8161 0.7127 0.027 Uiso 1 1 calc R . . C53 C 0.41249(17) 0.69264(9) 0.60472(16) 0.0206(4) Uani 1 1 d . . . C54 C 0.3910(2) 0.63395(11) 0.59563(18) 0.0303(5) Uani 1 1 d . . . H54 H 0.4406 0.6084 0.6434 0.036 Uiso 1 1 calc R . . C55 C 0.2982(3) 0.61167(13) 0.5180(2) 0.0405(6) Uani 1 1 d . . . H55 H 0.2859 0.5713 0.5126 0.049 Uiso 1 1 calc R . . C56 C 0.2250(2) 0.64828(15) 0.4494(2) 0.0383(6) Uani 1 1 d . . . H56 H 0.1612 0.6333 0.3972 0.046 Uiso 1 1 calc R . . C57 C 0.2439(2) 0.70767(14) 0.4560(2) 0.0359(6) Uani 1 1 d . . . H57 H 0.1937 0.7331 0.4083 0.043 Uiso 1 1 calc R . . C58 C 0.33740(19) 0.72893(11) 0.53350(18) 0.0279(4) Uani 1 1 d . . . H58 H 0.3504 0.7692 0.5380 0.034 Uiso 1 1 calc R . . C59 C 0.63329(16) 0.65477(8) 0.75731(16) 0.0196(3) Uani 1 1 d . . . C60 C 0.62360(19) 0.62840(10) 0.84127(18) 0.0262(4) Uani 1 1 d . . . H60 H 0.5769 0.6446 0.8688 0.031 Uiso 1 1 calc R . . C61 C 0.6818(2) 0.57878(11) 0.8843(2) 0.0321(5) Uani 1 1 d . . . H61 H 0.6747 0.5614 0.9411 0.039 Uiso 1 1 calc R . . C62 C 0.7502(2) 0.55454(10) 0.8447(2) 0.0338(5) Uani 1 1 d . . . H62 H 0.7902 0.5208 0.8747 0.041 Uiso 1 1 calc R . . C63 C 0.7603(2) 0.57939(10) 0.7617(2) 0.0317(5) Uani 1 1 d . . . H63 H 0.8064 0.5626 0.7340 0.038 Uiso 1 1 calc R . . C64 C 0.70249(19) 0.62924(9) 0.71865(19) 0.0259(4) Uani 1 1 d . . . H64 H 0.7102 0.6463 0.6619 0.031 Uiso 1 1 calc R . . C65 C 0.60646(16) 0.75627(8) 0.61204(16) 0.0197(3) Uani 1 1 d . . . C66 C 0.58873(19) 0.73194(9) 0.51726(18) 0.0260(4) Uani 1 1 d . . . H66 H 0.5480 0.6974 0.4971 0.031 Uiso 1 1 calc R . . C67 C 0.6290(2) 0.75692(11) 0.45198(19) 0.0290(4) Uani 1 1 d . . . H67 H 0.6166 0.7393 0.3886 0.035 Uiso 1 1 calc R . . C68 C 0.6875(2) 0.80776(11) 0.4800(2) 0.0313(5) Uani 1 1 d . . . H68 H 0.7144 0.8254 0.4355 0.038 Uiso 1 1 calc R . . C69 C 0.7067(2) 0.83309(10) 0.5744(2) 0.0298(5) Uani 1 1 d . . . H69 H 0.7470 0.8678 0.5940 0.036 Uiso 1 1 calc R . . C70 C 0.66651(18) 0.80722(9) 0.63959(18) 0.0244(4) Uani 1 1 d . . . H70 H 0.6801 0.8245 0.7035 0.029 Uiso 1 1 calc R . . C71 C 0.12979(18) 0.55012(8) 0.80561(19) 0.0240(4) Uani 1 1 d . . . C72 C 0.0362(2) 0.51669(10) 0.7602(3) 0.0349(6) Uani 1 1 d . . . H72 H -0.0004 0.5142 0.6883 0.042 Uiso 1 1 calc R . . C73 C -0.0022(2) 0.48690(11) 0.8237(3) 0.0470(8) Uani 1 1 d . . . H73 H -0.0658 0.4642 0.7940 0.056 Uiso 1 1 calc R . . C74 C 0.0489(3) 0.48968(12) 0.9258(3) 0.0513(9) Uani 1 1 d . . . H74 H 0.0202 0.4698 0.9670 0.062 Uiso 1 1 calc R . . C75 C 0.1438(3) 0.52164(12) 0.9715(3) 0.0429(7) Uani 1 1 d . . . H75 H 0.1808 0.5227 1.0435 0.051 Uiso 1 1 calc R . . C76 C 0.1839(2) 0.55204(10) 0.9110(2) 0.0302(5) Uani 1 1 d . . . H76 H 0.2482 0.5741 0.9417 0.036 Uiso 1 1 calc R . . C77 C 0.26353(17) 0.53266(8) 0.70180(17) 0.0220(4) Uani 1 1 d . . . C78 C 0.2156(2) 0.49332(10) 0.6229(2) 0.0291(4) Uani 1 1 d . . . H78 H 0.1403 0.4954 0.5813 0.035 Uiso 1 1 calc R . . C79 C 0.2787(2) 0.45089(11) 0.6054(2) 0.0391(6) Uani 1 1 d . . . H79 H 0.2468 0.4247 0.5505 0.047 Uiso 1 1 calc R . . C80 C 0.3870(3) 0.44679(14) 0.6670(3) 0.0537(9) Uani 1 1 d . . . H80 H 0.4295 0.4177 0.6547 0.064 Uiso 1 1 calc R . . C81 C 0.4343(2) 0.48473(13) 0.7469(3) 0.0505(9) Uani 1 1 d . . . H81 H 0.5089 0.4812 0.7899 0.061 Uiso 1 1 calc R . . C82 C 0.37326(19) 0.52817(10) 0.7650(2) 0.0337(5) Uani 1 1 d . . . H82 H 0.4060 0.5544 0.8196 0.040 Uiso 1 1 calc R . . O5 O 0.9241(6) 0.6820(3) 0.0344(8) 0.226(5) Uani 1 1 d . . . C84 C 0.8841(4) 0.6187(2) 0.1384(4) 0.0698(12) Uani 1 1 d . . . H84A H 0.8981 0.6184 0.2115 0.084 Uiso 1 1 calc R . . H84B H 0.8182 0.5957 0.1010 0.084 Uiso 1 1 calc R . . C83 C 0.8688(6) 0.6766(3) 0.1009(6) 0.108(2) Uani 1 1 d . . . H83A H 0.8989 0.7041 0.1582 0.129 Uiso 1 1 calc R . . H83B H 0.7907 0.6848 0.0632 0.129 Uiso 1 1 calc R . . C86 C 0.9938(4) 0.6293(2) 0.0523(5) 0.0768(14) Uani 1 1 d . . . H86A H 0.9758 0.6077 -0.0118 0.092 Uiso 1 1 calc R . . H86B H 1.0714 0.6399 0.0803 0.092 Uiso 1 1 calc R . . C85 C 0.9694(5) 0.5957(3) 0.1249(6) 0.108(2) Uani 1 1 d . . . H85A H 0.9524 0.5557 0.1001 0.129 Uiso 1 1 calc R . . H85B H 1.0333 0.5949 0.1908 0.129 Uiso 1 1 calc R . . O6 O 0.4114(4) 0.93896(18) 0.4325(3) 0.1011(13) Uani 1 1 d . . . C87 C 0.4322(6) 0.9000(3) 0.5057(4) 0.103(2) Uani 1 1 d . B . H87A H 0.4907 0.8745 0.5055 0.124 Uiso 1 1 calc R A 1 H87B H 0.3669 0.8760 0.4895 0.124 Uiso 1 1 calc R A 1 C88A C 0.4636(5) 0.9229(2) 0.6065(3) 0.0753(13) Uani 0.694(13) 1 d PU B 1 H88A H 0.5403 0.9144 0.6500 0.090 Uiso 0.694(13) 1 calc PR B 1 H88B H 0.4173 0.9079 0.6394 0.090 Uiso 0.694(13) 1 calc PR B 1 C89A C 0.4451(10) 0.9877(4) 0.5834(5) 0.087(3) Uani 0.694(13) 1 d PU B 1 H89A H 0.3776 1.0005 0.5882 0.104 Uiso 0.694(13) 1 calc PR B 1 H89B H 0.5063 1.0104 0.6317 0.104 Uiso 0.694(13) 1 calc PR B 1 C90A C 0.4373(13) 0.9941(4) 0.4809(6) 0.107(4) Uani 0.694(13) 1 d PU B 1 H90A H 0.5068 1.0081 0.4820 0.128 Uiso 0.694(13) 1 calc PR B 1 H90B H 0.3802 1.0223 0.4433 0.128 Uiso 0.694(13) 1 calc PR B 1 C88B C 0.4636(5) 0.9229(2) 0.6065(3) 0.0753(13) Uani 0.306(13) 1 d PU B 2 H88C H 0.5357 0.9414 0.6321 0.090 Uiso 0.306(13) 1 calc PR B 2 H88D H 0.4621 0.8933 0.6554 0.090 Uiso 0.306(13) 1 calc PR B 2 C89B C 0.373(2) 0.9667(10) 0.5822(14) 0.090(6) Uani 0.306(13) 1 d PU B 2 H89C H 0.3119 0.9505 0.5956 0.108 Uiso 0.306(13) 1 calc PR B 2 H89D H 0.3987 1.0021 0.6231 0.108 Uiso 0.306(13) 1 calc PR B 2 C90B C 0.339(3) 0.9786(8) 0.4732(13) 0.111(9) Uani 0.306(13) 1 d PU B 2 H90C H 0.3500 1.0198 0.4627 0.134 Uiso 0.306(13) 1 calc PR B 2 H90D H 0.2612 0.9695 0.4354 0.134 Uiso 0.306(13) 1 calc PR B 2 C91A C 0.3109(7) 0.6237(4) 0.2419(6) 0.123(3) Uani 0.526(5) 1 d PU C 1 H91A H 0.2419 0.6033 0.2215 0.184 Uiso 0.526(5) 1 calc PR C 1 H91B H 0.3314 0.6399 0.3101 0.184 Uiso 0.526(5) 1 calc PR C 1 H91C H 0.3669 0.5968 0.2425 0.184 Uiso 0.526(5) 1 calc PR C 1 C92A C 0.2982(6) 0.6761(4) 0.1601(6) 0.0556(15) Uani 0.526(5) 1 d PU C 1 H92A H 0.2777 0.6600 0.0912 0.067 Uiso 0.526(5) 1 calc PR C 1 H92B H 0.2404 0.7029 0.1580 0.067 Uiso 0.526(5) 1 calc PR C 1 C93A C 0.4124(4) 0.71067(18) 0.1949(4) 0.0716(11) Uani 0.526(5) 1 d PU C 1 H93A H 0.4457 0.7132 0.2701 0.086 Uiso 0.526(5) 1 calc PR C 1 H93B H 0.4617 0.6880 0.1739 0.086 Uiso 0.526(5) 1 calc PR C 1 C94A C 0.4038(5) 0.7686(3) 0.1534(9) 0.078(3) Uani 0.526(5) 1 d PU C 1 H94A H 0.3337 0.7696 0.0935 0.094 Uiso 0.526(5) 1 calc PR C 1 H94B H 0.3957 0.7943 0.2047 0.094 Uiso 0.526(5) 1 calc PR C 1 C95A C 0.4742(5) 0.7949(2) 0.1242(5) 0.0475(16) Uani 0.526(5) 1 d PDU C 1 H95A H 0.4368 0.8136 0.0571 0.057 Uiso 0.526(5) 1 calc PR C 1 H95B H 0.5284 0.7674 0.1205 0.057 Uiso 0.526(5) 1 calc PR C 1 C96A C 0.5240(14) 0.8368(7) 0.2028(11) 0.135(5) Uani 0.526(5) 1 d PDU C 1 H96A H 0.5782 0.8585 0.1884 0.203 Uiso 0.526(5) 1 calc PR C 1 H96B H 0.5590 0.8173 0.2686 0.203 Uiso 0.526(5) 1 calc PR C 1 H96C H 0.4687 0.8632 0.2052 0.203 Uiso 0.526(5) 1 calc PR C 1 C91B C 0.3109(7) 0.6237(4) 0.2419(6) 0.123(3) Uani 0.474(5) 1 d PU C 2 H91D H 0.2654 0.6165 0.2789 0.184 Uiso 0.474(5) 1 calc PR C 2 H91E H 0.3776 0.6012 0.2725 0.184 Uiso 0.474(5) 1 calc PR C 2 H91F H 0.2718 0.6124 0.1705 0.184 Uiso 0.474(5) 1 calc PR C 2 C92B C 0.3430(13) 0.6974(5) 0.2484(11) 0.097(3) Uani 0.474(5) 1 d PU C 2 H92C H 0.2753 0.7200 0.2179 0.117 Uiso 0.474(5) 1 calc PR C 2 H92D H 0.3804 0.7089 0.3206 0.117 Uiso 0.474(5) 1 calc PR C 2 C93B C 0.4124(4) 0.71067(18) 0.1949(4) 0.0716(11) Uani 0.474(5) 1 d PU C 2 H93C H 0.3897 0.7506 0.1728 0.086 Uiso 0.474(5) 1 calc PR C 2 H93D H 0.3769 0.6874 0.1324 0.086 Uiso 0.474(5) 1 calc PR C 2 C94B C 0.5436(7) 0.7120(3) 0.2042(6) 0.0559(18) Uani 0.474(5) 1 d PU C 2 H94C H 0.5909 0.7080 0.2774 0.067 Uiso 0.474(5) 1 calc PR C 2 H94D H 0.5531 0.6764 0.1709 0.067 Uiso 0.474(5) 1 calc PR C 2 C95B C 0.5941(7) 0.7639(2) 0.1617(4) 0.0530(19) Uani 0.474(5) 1 d PDU C 2 H95C H 0.6553 0.7496 0.1472 0.064 Uiso 0.474(5) 1 calc PR C 2 H95D H 0.5385 0.7798 0.0982 0.064 Uiso 0.474(5) 1 calc PR C 2 C96B C 0.6330(10) 0.8100(6) 0.2438(8) 0.109(4) Uani 0.474(5) 1 d PDU C 2 H96D H 0.6631 0.8423 0.2202 0.163 Uiso 0.474(5) 1 calc PR C 2 H96E H 0.6888 0.7939 0.3059 0.163 Uiso 0.474(5) 1 calc PR C 2 H96F H 0.5719 0.8234 0.2581 0.163 Uiso 0.474(5) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01371(5) 0.01086(4) 0.01344(5) -0.00051(5) 0.00440(4) -0.00065(5) P1 0.01111(18) 0.01113(17) 0.01583(18) -0.00040(14) 0.00451(15) -0.00041(14) P2 0.0179(2) 0.01216(18) 0.0227(2) -0.00274(16) 0.00940(18) -0.00250(16) Si1 0.0148(2) 0.01247(19) 0.0203(2) -0.00001(16) 0.00867(18) 0.00061(16) Si2 0.0158(2) 0.0154(2) 0.0223(2) -0.00293(18) 0.01030(19) -0.00123(17) Cl1 0.0267(2) 0.0256(2) 0.01704(19) 0.00235(16) 0.00264(17) 0.00669(18) O1 0.0127(6) 0.0149(5) 0.0207(6) 0.0035(5) 0.0037(5) 0.0001(4) O2 0.0202(7) 0.0160(6) 0.0263(7) -0.0061(5) 0.0058(6) -0.0048(5) O3 0.0160(6) 0.0101(5) 0.0180(6) -0.0008(4) 0.0076(5) -0.0016(4) O4 0.0121(5) 0.0152(5) 0.0176(6) -0.0012(4) 0.0050(5) -0.0019(4) C1 0.0130(7) 0.0161(6) 0.0153(7) -0.0015(5) 0.0064(6) -0.0007(6) C2 0.0135(7) 0.0190(8) 0.0139(7) 0.0003(6) 0.0056(6) 0.0003(6) C3 0.0170(8) 0.0272(9) 0.0136(7) 0.0012(6) 0.0052(6) 0.0050(7) C4 0.0172(9) 0.0330(10) 0.0160(8) -0.0037(7) 0.0012(7) 0.0047(7) C5 0.0153(8) 0.0291(11) 0.0197(8) -0.0096(7) 0.0025(6) 0.0002(6) C6 0.0160(8) 0.0202(8) 0.0200(8) -0.0053(6) 0.0067(7) -0.0004(6) C7 0.0258(10) 0.0303(10) 0.0183(8) 0.0077(7) 0.0091(7) 0.0092(8) C8 0.0263(10) 0.0243(9) 0.0231(9) 0.0060(7) 0.0080(8) 0.0072(8) C9 0.0383(13) 0.0384(13) 0.0428(13) 0.0221(11) 0.0271(11) 0.0118(10) C10 0.0419(14) 0.0424(14) 0.0197(9) 0.0085(9) 0.0063(9) 0.0170(11) C11 0.0175(9) 0.0353(11) 0.0326(11) -0.0174(9) 0.0025(8) -0.0022(8) C12 0.0240(11) 0.0465(15) 0.0377(13) -0.0210(12) -0.0067(10) 0.0023(10) C13 0.0296(12) 0.0381(13) 0.0368(13) -0.0212(11) 0.0010(10) 0.0012(10) C14 0.0241(11) 0.0493(16) 0.0531(17) -0.0201(13) 0.0142(11) -0.0173(11) C15 0.0155(7) 0.0105(6) 0.0152(7) 0.0000(5) 0.0058(6) -0.0002(5) C16 0.0156(7) 0.0129(7) 0.0193(8) -0.0001(6) 0.0073(6) 0.0000(6) C17 0.0178(8) 0.0125(7) 0.0212(8) 0.0006(6) 0.0089(7) 0.0006(6) C18 0.0175(8) 0.0119(7) 0.0175(7) 0.0012(6) 0.0049(6) -0.0003(6) C19 0.0212(9) 0.0117(7) 0.0206(8) 0.0010(6) 0.0046(7) -0.0002(6) C20 0.0259(9) 0.0131(7) 0.0210(8) 0.0018(6) 0.0030(7) -0.0033(7) C21 0.0202(9) 0.0166(8) 0.0274(9) -0.0001(7) 0.0061(7) -0.0074(7) C22 0.0165(8) 0.0166(7) 0.0234(8) 0.0003(6) 0.0061(7) -0.0028(6) C23 0.0172(8) 0.0113(6) 0.0168(7) -0.0003(5) 0.0062(6) -0.0015(6) C24 0.0148(7) 0.0116(6) 0.0172(7) -0.0011(5) 0.0064(6) -0.0005(5) C25 0.0136(7) 0.0138(7) 0.0185(7) -0.0003(6) 0.0065(6) -0.0002(6) C26 0.0144(7) 0.0159(7) 0.0186(7) -0.0003(6) 0.0045(6) -0.0007(6) C27 0.0182(8) 0.0170(8) 0.0207(8) -0.0026(6) 0.0046(7) -0.0006(6) C28 0.0227(10) 0.0231(9) 0.0196(9) -0.0038(7) 0.0020(7) -0.0033(7) C29 0.0173(8) 0.0270(9) 0.0222(9) -0.0010(7) 0.0022(7) -0.0035(7) C30 0.0138(8) 0.0266(9) 0.0252(9) 0.0004(7) 0.0040(7) 0.0004(7) C31 0.0145(8) 0.0197(8) 0.0220(8) -0.0013(6) 0.0061(7) -0.0011(6) C32 0.0147(8) 0.0211(8) 0.0253(9) -0.0026(7) 0.0083(7) 0.0009(7) C33 0.0140(7) 0.0169(7) 0.0233(8) -0.0029(6) 0.0088(6) -0.0011(6) C34 0.0118(7) 0.0161(7) 0.0183(7) -0.0004(6) 0.0058(6) -0.0014(6) C35 0.0187(8) 0.0171(7) 0.0209(8) 0.0010(6) 0.0102(7) 0.0034(6) C36 0.0238(9) 0.0230(9) 0.0230(9) -0.0014(7) 0.0108(8) -0.0018(7) C37 0.0287(11) 0.0365(12) 0.0218(9) -0.0030(8) 0.0092(8) -0.0007(9) C38 0.0361(12) 0.0422(13) 0.0216(9) 0.0019(9) 0.0149(9) 0.0031(10) C39 0.0327(12) 0.0375(12) 0.0305(11) 0.0066(9) 0.0202(10) -0.0003(9) C40 0.0229(9) 0.0279(9) 0.0268(9) -0.0002(7) 0.0147(8) -0.0027(7) C41 0.0167(8) 0.0152(7) 0.0255(9) -0.0018(6) 0.0081(7) 0.0020(6) C42 0.0201(9) 0.0279(10) 0.0312(10) -0.0022(8) 0.0121(8) 0.0021(8) C43 0.0180(10) 0.0412(13) 0.0465(14) -0.0098(11) 0.0138(10) 0.0022(9) C44 0.0195(10) 0.0336(12) 0.0491(15) -0.0032(11) 0.0028(10) 0.0084(9) C45 0.0253(10) 0.0237(10) 0.0364(12) 0.0046(9) 0.0031(9) 0.0037(8) C46 0.0214(9) 0.0185(8) 0.0285(9) 0.0007(7) 0.0081(8) 0.0015(7) C47 0.0179(8) 0.0143(7) 0.0247(9) -0.0002(6) 0.0121(7) -0.0005(6) C48 0.0232(9) 0.0158(8) 0.0286(9) 0.0008(7) 0.0139(8) 0.0000(7) C49 0.0345(11) 0.0136(7) 0.0395(11) 0.0023(7) 0.0248(10) 0.0026(7) C50 0.0326(10) 0.0187(10) 0.0502(13) -0.0102(9) 0.0268(10) -0.0093(8) C51 0.0234(10) 0.0228(9) 0.0380(11) -0.0084(8) 0.0135(9) -0.0049(8) C52 0.0211(9) 0.0195(8) 0.0270(9) -0.0029(7) 0.0108(8) -0.0021(7) C53 0.0196(9) 0.0219(8) 0.0238(9) -0.0062(6) 0.0123(7) -0.0045(6) C54 0.0364(12) 0.0275(11) 0.0256(10) -0.0047(8) 0.0112(9) -0.0134(9) C55 0.0488(16) 0.0411(14) 0.0312(12) -0.0118(10) 0.0157(12) -0.0259(12) C56 0.0277(12) 0.0605(18) 0.0272(11) -0.0179(12) 0.0116(10) -0.0142(12) C57 0.0243(11) 0.0505(16) 0.0297(12) -0.0120(11) 0.0077(9) 0.0026(10) C58 0.0211(10) 0.0325(11) 0.0293(10) -0.0065(9) 0.0093(8) 0.0021(8) C59 0.0191(8) 0.0159(7) 0.0270(9) -0.0022(7) 0.0126(7) -0.0015(6) C60 0.0288(10) 0.0259(10) 0.0287(10) 0.0018(8) 0.0164(9) 0.0019(8) C61 0.0398(14) 0.0253(10) 0.0305(11) 0.0062(9) 0.0136(10) 0.0009(9) C62 0.0336(12) 0.0201(9) 0.0433(13) 0.0048(9) 0.0111(10) 0.0008(8) C63 0.0324(12) 0.0207(9) 0.0477(14) 0.0016(9) 0.0221(11) 0.0052(8) C64 0.0278(10) 0.0179(8) 0.0396(12) 0.0021(8) 0.0214(9) 0.0030(7) C65 0.0200(8) 0.0156(7) 0.0265(9) 0.0011(6) 0.0126(7) 0.0000(6) C66 0.0296(11) 0.0244(10) 0.0296(10) -0.0024(7) 0.0179(9) -0.0040(8) C67 0.0327(11) 0.0303(10) 0.0300(10) 0.0030(8) 0.0190(9) 0.0003(9) C68 0.0320(12) 0.0313(11) 0.0365(12) 0.0108(9) 0.0197(10) -0.0014(9) C69 0.0278(11) 0.0231(9) 0.0386(12) 0.0059(8) 0.0137(9) -0.0047(8) C70 0.0222(9) 0.0206(8) 0.0312(10) -0.0010(7) 0.0116(8) -0.0028(7) C71 0.0264(10) 0.0132(7) 0.0401(11) 0.0021(7) 0.0213(9) 0.0024(7) C72 0.0280(11) 0.0186(9) 0.0646(17) 0.0057(10) 0.0255(12) -0.0003(8) C73 0.0346(13) 0.0215(10) 0.098(3) 0.0170(13) 0.0409(16) 0.0047(9) C74 0.063(2) 0.0301(12) 0.091(3) 0.0286(15) 0.063(2) 0.0184(13) C75 0.0626(19) 0.0312(12) 0.0527(16) 0.0177(12) 0.0417(16) 0.0157(12) C76 0.0423(13) 0.0195(9) 0.0391(12) 0.0072(8) 0.0272(11) 0.0053(9) C77 0.0239(9) 0.0140(7) 0.0313(10) -0.0059(7) 0.0145(8) -0.0033(7) C78 0.0292(11) 0.0217(9) 0.0369(12) -0.0122(8) 0.0140(9) -0.0034(8) C79 0.0399(14) 0.0267(11) 0.0552(16) -0.0211(11) 0.0240(13) -0.0038(10) C80 0.0366(14) 0.0396(15) 0.092(3) -0.0338(16) 0.0331(16) -0.0021(12) C81 0.0214(11) 0.0377(14) 0.089(2) -0.0309(16) 0.0192(14) -0.0022(10) C82 0.0212(10) 0.0238(10) 0.0552(15) -0.0176(10) 0.0145(10) -0.0039(8) O5 0.259(7) 0.157(5) 0.409(11) 0.183(7) 0.287(9) 0.143(5) C84 0.070(3) 0.078(3) 0.075(3) 0.023(2) 0.044(2) -0.011(2) C83 0.122(5) 0.089(4) 0.144(5) 0.054(4) 0.087(4) 0.012(4) C86 0.073(3) 0.057(2) 0.107(4) 0.028(2) 0.043(3) 0.018(2) C85 0.076(3) 0.119(5) 0.138(5) 0.075(4) 0.053(4) 0.017(3) O6 0.152(4) 0.085(3) 0.0552(19) -0.0026(17) 0.031(2) -0.002(3) C87 0.119(5) 0.119(5) 0.047(2) 0.006(3) 0.008(3) 0.043(4) C88A 0.104(4) 0.071(3) 0.0454(19) 0.0104(18) 0.025(2) 0.025(3) C89A 0.116(7) 0.080(4) 0.047(3) -0.007(3) 0.015(4) 0.043(5) C90A 0.170(10) 0.073(5) 0.060(4) 0.021(4) 0.029(5) 0.015(6) C88B 0.104(4) 0.071(3) 0.0454(19) 0.0104(18) 0.025(2) 0.025(3) C89B 0.082(10) 0.095(11) 0.063(8) -0.019(8) -0.001(8) 0.016(8) C90B 0.155(17) 0.047(7) 0.066(9) -0.005(6) -0.022(9) 0.039(9) C91A 0.153(6) 0.136(5) 0.128(5) -0.014(4) 0.108(5) -0.044(5) C92A 0.060(3) 0.043(3) 0.073(4) -0.010(3) 0.037(3) -0.009(3) C93A 0.094(3) 0.048(2) 0.064(2) 0.0001(17) 0.023(2) -0.005(2) C94A 0.036(3) 0.043(3) 0.156(8) 0.061(4) 0.039(4) 0.021(2) C95A 0.042(3) 0.034(3) 0.070(4) 0.026(3) 0.027(3) 0.000(2) C96A 0.144(11) 0.139(11) 0.147(11) -0.005(8) 0.085(9) -0.035(8) C91B 0.153(6) 0.136(5) 0.128(5) -0.014(4) 0.108(5) -0.044(5) C92B 0.165(9) 0.065(5) 0.113(7) 0.022(5) 0.109(7) 0.022(6) C93B 0.094(3) 0.048(2) 0.064(2) 0.0001(17) 0.023(2) -0.005(2) C94B 0.065(4) 0.049(4) 0.045(3) -0.001(3) 0.014(3) 0.028(3) C95B 0.106(5) 0.033(3) 0.034(3) 0.032(2) 0.043(3) 0.038(3) C96B 0.062(6) 0.197(10) 0.060(6) -0.015(7) 0.017(5) -0.036(7) _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 Pd1 C1 2.0045(18) . ? Pd1 P1 2.2442(4) . ? Pd1 P2 2.2631(5) . ? Pd1 Cl1 2.3591(5) . ? P1 O3 1.5951(14) . ? P1 O1 1.6034(14) . ? P1 O4 1.6097(14) . ? P2 O2 1.6289(16) . ? P2 C77 1.804(2) . ? P2 C71 1.814(2) . ? Si1 C47 1.8745(19) . ? Si1 C16 1.8853(19) . ? Si1 C35 1.887(2) . ? Si1 C41 1.890(2) . ? Si2 C59 1.870(2) . ? Si2 C65 1.879(2) . ? Si2 C53 1.883(2) . ? Si2 C33 1.8896(19) . ? O1 C2 1.408(2) . ? O2 C6 1.405(3) . ? O3 C15 1.410(2) . ? O4 C34 1.407(2) . ? C1 C6 1.393(3) . ? C1 C2 1.395(3) . ? C2 C3 1.388(3) . ? C3 C4 1.407(3) . ? C3 C7 1.540(3) . ? C4 C5 1.395(3) . ? C4 H4 0.9500 . ? C5 C6 1.403(3) . ? C5 C11 1.541(3) . ? C7 C8 1.533(3) . ? C7 C10 1.538(3) . ? C7 C9 1.544(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.531(4) . ? C11 C13 1.543(3) . ? C11 C14 1.551(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.382(2) . ? C15 C16 1.415(2) . ? C16 C17 1.388(2) . ? C17 C18 1.414(3) . ? C17 H17 0.9500 . ? C18 C23 1.424(3) . ? C18 C19 1.425(2) . ? C19 C20 1.366(3) . ? C19 H19 0.9500 . ? C20 C21 1.413(3) . ? C20 H20 0.9500 . ? C21 C22 1.376(3) . ? C21 H21 0.9500 . ? C22 C23 1.419(3) . ? C22 H22 0.9500 . ? C23 C24 1.436(2) . ? C24 C25 1.494(2) . ? C25 C34 1.384(2) . ? C25 C26 1.428(3) . ? C26 C31 1.425(3) . ? C26 C27 1.428(3) . ? C27 C28 1.373(3) . ? C27 H27 0.9500 . ? C28 C29 1.414(3) . ? C28 H28 0.9500 . ? C29 C30 1.375(3) . ? C29 H29 0.9500 . ? C30 C31 1.421(3) . ? C30 H30 0.9500 . ? C31 C32 1.411(3) . ? C32 C33 1.383(3) . ? C32 H32 0.9500 . ? C33 C34 1.413(3) . ? C35 C36 1.401(3) . ? C35 C40 1.406(3) . ? C36 C37 1.399(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(4) . ? C37 H37 0.9500 . ? C38 C39 1.387(4) . ? C38 H38 0.9500 . ? C39 C40 1.397(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.398(3) . ? C41 C42 1.403(3) . ? C42 C43 1.394(3) . ? C42 H42 0.9500 . ? C43 C44 1.385(4) . ? C43 H43 0.9500 . ? C44 C45 1.393(4) . ? C44 H44 0.9500 . ? C45 C46 1.393(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.398(3) . ? C47 C48 1.407(3) . ? C48 C49 1.392(3) . ? C48 H48 0.9500 . ? C49 C50 1.394(4) . ? C49 H49 0.9500 . ? C50 C51 1.378(4) . ? C50 H50 0.9500 . ? C51 C52 1.402(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.390(3) . ? C53 C58 1.396(3) . ? C54 C55 1.397(4) . ? C54 H54 0.9500 . ? C55 C56 1.373(5) . ? C55 H55 0.9500 . ? C56 C57 1.400(4) . ? C56 H56 0.9500 . ? C57 C58 1.394(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.401(3) . ? C59 C60 1.408(3) . ? C60 C61 1.392(3) . ? C60 H60 0.9500 . ? C61 C62 1.390(4) . ? C61 H61 0.9500 . ? C62 C63 1.383(4) . ? C62 H62 0.9500 . ? C63 C64 1.394(3) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.400(3) . ? C65 C66 1.404(3) . ? C66 C67 1.391(3) . ? C66 H66 0.9500 . ? C67 C68 1.388(4) . ? C67 H67 0.9500 . ? C68 C69 1.404(4) . ? C68 H68 0.9500 . ? C69 C70 1.397(3) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C76 1.392(4) . ? C71 C72 1.401(3) . ? C72 C73 1.404(4) . ? C72 H72 0.9500 . ? C73 C74 1.347(6) . ? C73 H73 0.9500 . ? C74 C75 1.395(5) . ? C74 H74 0.9500 . ? C75 C76 1.391(3) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.395(3) . ? C77 C78 1.396(3) . ? C78 C79 1.394(3) . ? C78 H78 0.9500 . ? C79 C80 1.373(5) . ? C79 H79 0.9500 . ? C80 C81 1.382(4) . ? C80 H80 0.9500 . ? C81 C82 1.394(3) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? O5 C83 1.441(7) . ? O5 C86 1.504(6) . ? C84 C85 1.356(8) . ? C84 C83 1.434(8) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C86 C85 1.447(7) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? O6 C87 1.330(7) . ? O6 C90A 1.433(11) . ? O6 C90B 1.62(3) . ? C87 C88A 1.437(7) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88A C89A 1.541(9) . ? C88A H88A 0.9900 . ? C88A H88B 0.9900 . ? C89A C90A 1.443(11) . ? C89A H89A 0.9900 . ? C89A H89B 0.9900 . ? C90A H90A 0.9900 . ? C90A H90B 0.9900 . ? C89B C90B 1.47(3) . ? C89B H89C 0.9900 . ? C89B H89D 0.9900 . ? C90B H90C 0.9900 . ? C90B H90D 0.9900 . ? C91A C92A 1.654(11) . ? C91A H91A 0.9800 . ? C91A H91B 0.9800 . ? C91A H91C 0.9800 . ? C92A C93A 1.630(8) . ? C92A H92A 0.9900 . ? C92A H92B 0.9900 . ? C93A C94A 1.458(7) . ? C93A H93A 0.9900 . ? C93A H93B 0.9900 . ? C94A C95A 1.337(8) . ? C94A H94A 0.9900 . ? C94A H94B 0.9900 . ? C95A C96A 1.437(9) . ? C95A H95A 0.9900 . ? C95A H95B 0.9900 . ? C96A H96A 0.9800 . ? C96A H96B 0.9800 . ? C96A H96C 0.9800 . ? C92B H92C 0.9900 . ? C92B H92D 0.9900 . ? C94B C95B 1.624(11) . ? C94B H94C 0.9900 . ? C94B H94D 0.9900 . ? C95B C96B 1.521(9) . ? C95B H95C 0.9900 . ? C95B H95D 0.9900 . ? C96B H96D 0.9800 . ? C96B H96E 0.9800 . ? C96B H96F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 79.97(5) . . ? C1 Pd1 P2 80.05(5) . . ? P1 Pd1 P2 159.973(19) . . ? C1 Pd1 Cl1 177.50(5) . . ? P1 Pd1 Cl1 100.266(18) . . ? P2 Pd1 Cl1 99.757(19) . . ? O3 P1 O1 107.15(7) . . ? O3 P1 O4 102.61(7) . . ? O1 P1 O4 96.03(7) . . ? O3 P1 Pd1 115.32(5) . . ? O1 P1 Pd1 106.54(5) . . ? O4 P1 Pd1 126.40(5) . . ? O2 P2 C77 104.03(9) . . ? O2 P2 C71 102.94(10) . . ? C77 P2 C71 101.70(9) . . ? O2 P2 Pd1 105.80(6) . . ? C77 P2 Pd1 118.25(7) . . ? C71 P2 Pd1 121.89(7) . . ? C47 Si1 C16 118.54(8) . . ? C47 Si1 C35 105.99(9) . . ? C16 Si1 C35 105.44(9) . . ? C47 Si1 C41 106.16(9) . . ? C16 Si1 C41 109.23(9) . . ? C35 Si1 C41 111.48(9) . . ? C59 Si2 C65 110.20(9) . . ? C59 Si2 C53 107.76(9) . . ? C65 Si2 C53 104.70(9) . . ? C59 Si2 C33 106.59(9) . . ? C65 Si2 C33 106.73(9) . . ? C53 Si2 C33 120.66(9) . . ? C2 O1 P1 114.58(12) . . ? C6 O2 P2 114.90(12) . . ? C15 O3 P1 121.19(11) . . ? C34 O4 P1 117.62(12) . . ? C6 C1 C2 117.90(17) . . ? C6 C1 Pd1 121.41(14) . . ? C2 C1 Pd1 120.65(13) . . ? C3 C2 C1 123.65(18) . . ? C3 C2 O1 118.71(17) . . ? C1 C2 O1 117.63(16) . . ? C2 C3 C4 114.69(19) . . ? C2 C3 C7 122.51(18) . . ? C4 C3 C7 122.80(18) . . ? C5 C4 C3 125.49(18) . . ? C5 C4 H4 117.3 . . ? C3 C4 H4 117.3 . . ? C4 C5 C6 115.50(18) . . ? C4 C5 C11 121.78(19) . . ? C6 C5 C11 122.6(2) . . ? C1 C6 C5 122.51(19) . . ? C1 C6 O2 117.77(17) . . ? C5 C6 O2 119.72(17) . . ? C8 C7 C10 107.80(18) . . ? C8 C7 C3 110.63(16) . . ? C10 C7 C3 111.4(2) . . ? C8 C7 C9 109.4(2) . . ? C10 C7 C9 107.2(2) . . ? C3 C7 C9 110.31(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C5 111.7(2) . . ? C12 C11 C13 107.3(2) . . ? C5 C11 C13 110.95(19) . . ? C12 C11 C14 107.3(2) . . ? C5 C11 C14 108.74(19) . . ? C13 C11 C14 110.8(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 O3 118.31(15) . . ? C24 C15 C16 125.44(16) . . ? O3 C15 C16 116.13(15) . . ? C17 C16 C15 115.52(17) . . ? C17 C16 Si1 118.91(14) . . ? C15 C16 Si1 124.54(13) . . ? C16 C17 C18 122.68(17) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C17 C18 C23 119.72(16) . . ? C17 C18 C19 120.77(17) . . ? C23 C18 C19 119.50(17) . . ? C20 C19 C18 121.04(19) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.54(18) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.85(19) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.99(19) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.00(16) . . ? C22 C23 C24 123.13(17) . . ? C18 C23 C24 118.87(16) . . ? C15 C24 C23 117.47(16) . . ? C15 C24 C25 120.81(15) . . ? C23 C24 C25 121.72(16) . . ? C34 C25 C26 117.69(16) . . ? C34 C25 C24 120.03(16) . . ? C26 C25 C24 122.28(16) . . ? C31 C26 C27 118.26(17) . . ? C31 C26 C25 118.74(17) . . ? C27 C26 C25 122.98(17) . . ? C28 C27 C26 120.74(18) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.74(19) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 119.93(19) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.72(19) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 120.77(19) . . ? C32 C31 C26 119.75(18) . . ? C30 C31 C26 119.48(18) . . ? C33 C32 C31 122.71(18) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C32 C33 C34 115.65(17) . . ? C32 C33 Si2 117.02(14) . . ? C34 C33 Si2 126.88(14) . . ? C25 C34 O4 117.88(16) . . ? C25 C34 C33 125.23(17) . . ? O4 C34 C33 116.80(16) . . ? C36 C35 C40 117.55(18) . . ? C36 C35 Si1 122.35(15) . . ? C40 C35 Si1 120.06(16) . . ? C37 C36 C35 121.3(2) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 120.0(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 119.7(2) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.2(2) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C35 121.2(2) . . ? C39 C40 H40 119.4 . . ? C35 C40 H40 119.4 . . ? C46 C41 C42 117.43(19) . . ? C46 C41 Si1 123.82(16) . . ? C42 C41 Si1 118.43(16) . . ? C43 C42 C41 121.3(2) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.7(2) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 119.9(2) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 121.5(2) . . ? C45 C46 H46 119.2 . . ? C41 C46 H46 119.2 . . ? C52 C47 C48 117.81(18) . . ? C52 C47 Si1 121.06(15) . . ? C48 C47 Si1 120.87(16) . . ? C49 C48 C47 120.9(2) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 C50 120.1(2) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 120.0(2) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 119.9(2) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C47 C52 C51 121.2(2) . . ? C47 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C54 C53 C58 117.5(2) . . ? C54 C53 Si2 119.66(18) . . ? C58 C53 Si2 121.90(16) . . ? C53 C54 C55 121.7(3) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 119.8(3) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C57 120.2(3) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C58 C57 C56 119.0(3) . . ? C58 C57 H57 120.5 . . ? C56 C57 H57 120.5 . . ? C57 C58 C53 121.8(2) . . ? C57 C58 H58 119.1 . . ? C53 C58 H58 119.1 . . ? C64 C59 C60 117.84(19) . . ? C64 C59 Si2 121.54(16) . . ? C60 C59 Si2 120.52(15) . . ? C61 C60 C59 120.6(2) . . ? C61 C60 H60 119.7 . . ? C59 C60 H60 119.7 . . ? C62 C61 C60 120.3(2) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C63 C62 C61 120.1(2) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C62 C63 C64 119.7(2) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C63 C64 C59 121.4(2) . . ? C63 C64 H64 119.3 . . ? C59 C64 H64 119.3 . . ? C70 C65 C66 117.79(19) . . ? C70 C65 Si2 123.44(16) . . ? C66 C65 Si2 118.77(15) . . ? C67 C66 C65 121.9(2) . . ? C67 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? C68 C67 C66 119.5(2) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C67 C68 C69 119.9(2) . . ? C67 C68 H68 120.1 . . ? C69 C68 H68 120.1 . . ? C70 C69 C68 119.9(2) . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C70 C65 120.9(2) . . ? C69 C70 H70 119.5 . . ? C65 C70 H70 119.5 . . ? C76 C71 C72 120.1(2) . . ? C76 C71 P2 119.33(18) . . ? C72 C71 P2 120.5(2) . . ? C71 C72 C73 118.3(3) . . ? C71 C72 H72 120.9 . . ? C73 C72 H72 120.9 . . ? C74 C73 C72 121.6(3) . . ? C74 C73 H73 119.2 . . ? C72 C73 H73 119.2 . . ? C73 C74 C75 120.3(2) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C76 C75 C74 119.7(3) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? C75 C76 C71 119.9(3) . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? C82 C77 C78 120.0(2) . . ? C82 C77 P2 118.48(16) . . ? C78 C77 P2 121.43(17) . . ? C79 C78 C77 119.7(2) . . ? C79 C78 H78 120.2 . . ? C77 C78 H78 120.2 . . ? C80 C79 C78 120.3(2) . . ? C80 C79 H79 119.9 . . ? C78 C79 H79 119.9 . . ? C79 C80 C81 120.3(2) . . ? C79 C80 H80 119.8 . . ? C81 C80 H80 119.8 . . ? C80 C81 C82 120.5(3) . . ? C80 C81 H81 119.7 . . ? C82 C81 H81 119.7 . . ? C81 C82 C77 119.2(2) . . ? C81 C82 H82 120.4 . . ? C77 C82 H82 120.4 . . ? C83 O5 C86 106.0(4) . . ? C85 C84 C83 108.5(4) . . ? C85 C84 H84A 110.0 . . ? C83 C84 H84A 110.0 . . ? C85 C84 H84B 110.0 . . ? C83 C84 H84B 110.0 . . ? H84A C84 H84B 108.4 . . ? C84 C83 O5 107.3(5) . . ? C84 C83 H83A 110.3 . . ? O5 C83 H83A 110.3 . . ? C84 C83 H83B 110.3 . . ? O5 C83 H83B 110.3 . . ? H83A C83 H83B 108.5 . . ? C85 C86 O5 104.5(5) . . ? C85 C86 H86A 110.8 . . ? O5 C86 H86A 110.8 . . ? C85 C86 H86B 110.8 . . ? O5 C86 H86B 110.8 . . ? H86A C86 H86B 108.9 . . ? C84 C85 C86 110.4(5) . . ? C84 C85 H85A 109.6 . . ? C86 C85 H85A 109.6 . . ? C84 C85 H85B 109.6 . . ? C86 C85 H85B 109.6 . . ? H85A C85 H85B 108.1 . . ? C87 O6 C90A 107.0(5) . . ? C87 O6 C90B 93.7(9) . . ? C90A O6 C90B 51.6(9) . . ? O6 C87 C88A 115.3(6) . . ? O6 C87 H87A 108.4 . . ? C88A C87 H87A 108.4 . . ? O6 C87 H87B 108.4 . . ? C88A C87 H87B 108.4 . . ? H87A C87 H87B 107.5 . . ? C87 C88A C89A 100.9(4) . . ? C87 C88A H88A 111.6 . . ? C89A C88A H88A 111.6 . . ? C87 C88A H88B 111.6 . . ? C89A C88A H88B 111.6 . . ? H88A C88A H88B 109.4 . . ? C90A C89A C88A 105.0(6) . . ? C90A C89A H89A 110.7 . . ? C88A C89A H89A 110.7 . . ? C90A C89A H89B 110.7 . . ? C88A C89A H89B 110.7 . . ? H89A C89A H89B 108.8 . . ? C89A C90A O6 107.9(7) . . ? C89A C90A H90A 110.1 . . ? O6 C90A H90A 110.1 . . ? C89A C90A H90B 110.1 . . ? O6 C90A H90B 110.1 . . ? H90A C90A H90B 108.4 . . ? C90B C89B H89C 111.0 . . ? C90B C89B H89D 111.0 . . ? H89C C89B H89D 109.0 . . ? C89B C90B O6 108.0(13) . . ? C89B C90B H90C 110.1 . . ? O6 C90B H90C 110.1 . . ? C89B C90B H90D 110.1 . . ? O6 C90B H90D 110.1 . . ? H90C C90B H90D 108.4 . . ? C92A C91A H91A 109.5 . . ? C92A C91A H91B 109.5 . . ? H91A C91A H91B 109.5 . . ? C92A C91A H91C 109.5 . . ? H91A C91A H91C 109.5 . . ? H91B C91A H91C 109.5 . . ? C93A C92A C91A 109.5(6) . . ? C93A C92A H92A 109.8 . . ? C91A C92A H92A 109.8 . . ? C93A C92A H92B 109.8 . . ? C91A C92A H92B 109.8 . . ? H92A C92A H92B 108.2 . . ? C94A C93A C92A 114.9(5) . . ? C94A C93A H93A 108.5 . . ? C92A C93A H93A 108.5 . . ? C94A C93A H93B 108.5 . . ? C92A C93A H93B 108.5 . . ? H93A C93A H93B 107.5 . . ? C95A C94A C93A 127.1(6) . . ? C95A C94A H94A 105.5 . . ? C93A C94A H94A 105.5 . . ? C95A C94A H94B 105.5 . . ? C93A C94A H94B 105.5 . . ? H94A C94A H94B 106.1 . . ? C94A C95A C96A 103.2(9) . . ? C94A C95A H95A 111.1 . . ? C96A C95A H95A 111.1 . . ? C94A C95A H95B 111.1 . . ? C96A C95A H95B 111.1 . . ? H95A C95A H95B 109.1 . . ? C95A C96A H96A 109.5 . . ? C95A C96A H96B 109.5 . . ? H96A C96A H96B 109.5 . . ? C95A C96A H96C 109.5 . . ? H96A C96A H96C 109.5 . . ? H96B C96A H96C 109.5 . . ? H92C C92B H92D 107.9 . . ? C95B C94B H94C 106.3 . . ? C95B C94B H94D 106.3 . . ? H94C C94B H94D 106.4 . . ? C96B C95B C94B 107.3(7) . . ? C96B C95B H95C 110.3 . . ? C94B C95B H95C 110.3 . . ? C96B C95B H95D 110.3 . . ? C94B C95B H95D 110.3 . . ? H95C C95B H95D 108.5 . . ? C95B C96B H96D 109.5 . . ? C95B C96B H96E 109.5 . . ? H96D C96B H96E 109.5 . . ? C95B C96B H96F 109.5 . . ? H96D C96B H96F 109.5 . . ? H96E C96B H96F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P1 O3 124.71(8) . . . . ? P2 Pd1 P1 O3 128.37(7) . . . . ? Cl1 Pd1 P1 O3 -52.76(6) . . . . ? C1 Pd1 P1 O1 5.97(8) . . . . ? P2 Pd1 P1 O1 9.63(8) . . . . ? Cl1 Pd1 P1 O1 -171.51(6) . . . . ? C1 Pd1 P1 O4 -104.84(8) . . . . ? P2 Pd1 P1 O4 -101.18(8) . . . . ? Cl1 Pd1 P1 O4 77.69(7) . . . . ? C1 Pd1 P2 O2 1.15(8) . . . . ? P1 Pd1 P2 O2 -2.51(9) . . . . ? Cl1 Pd1 P2 O2 178.62(6) . . . . ? C1 Pd1 P2 C77 117.13(10) . . . . ? P1 Pd1 P2 C77 113.47(10) . . . . ? Cl1 Pd1 P2 C77 -65.40(9) . . . . ? C1 Pd1 P2 C71 -115.61(10) . . . . ? P1 Pd1 P2 C71 -119.27(10) . . . . ? Cl1 Pd1 P2 C71 61.86(9) . . . . ? O3 P1 O1 C2 -132.48(12) . . . . ? O4 P1 O1 C2 122.31(13) . . . . ? Pd1 P1 O1 C2 -8.52(13) . . . . ? C77 P2 O2 C6 -127.80(14) . . . . ? C71 P2 O2 C6 126.42(15) . . . . ? Pd1 P2 O2 C6 -2.51(15) . . . . ? O1 P1 O3 C15 -59.12(15) . . . . ? O4 P1 O3 C15 41.35(15) . . . . ? Pd1 P1 O3 C15 -177.53(11) . . . . ? O3 P1 O4 C34 51.06(14) . . . . ? O1 P1 O4 C34 160.18(13) . . . . ? Pd1 P1 O4 C34 -84.12(13) . . . . ? P1 Pd1 C1 C6 179.02(15) . . . . ? P2 Pd1 C1 C6 0.29(14) . . . . ? Cl1 Pd1 C1 C6 -85.4(13) . . . . ? P1 Pd1 C1 C2 -3.19(14) . . . . ? P2 Pd1 C1 C2 178.08(15) . . . . ? Cl1 Pd1 C1 C2 92.4(13) . . . . ? C6 C1 C2 C3 -4.4(3) . . . . ? Pd1 C1 C2 C3 177.71(14) . . . . ? C6 C1 C2 O1 176.66(16) . . . . ? Pd1 C1 C2 O1 -1.2(2) . . . . ? P1 O1 C2 C3 -172.04(14) . . . . ? P1 O1 C2 C1 6.9(2) . . . . ? C1 C2 C3 C4 5.3(3) . . . . ? O1 C2 C3 C4 -175.84(17) . . . . ? C1 C2 C3 C7 -175.32(18) . . . . ? O1 C2 C3 C7 3.6(3) . . . . ? C2 C3 C4 C5 -1.7(3) . . . . ? C7 C3 C4 C5 178.9(2) . . . . ? C3 C4 C5 C6 -2.5(3) . . . . ? C3 C4 C5 C11 174.0(2) . . . . ? C2 C1 C6 C5 -0.3(3) . . . . ? Pd1 C1 C6 C5 177.57(15) . . . . ? C2 C1 C6 O2 -179.86(17) . . . . ? Pd1 C1 C6 O2 -2.0(2) . . . . ? C4 C5 C6 C1 3.5(3) . . . . ? C11 C5 C6 C1 -173.01(19) . . . . ? C4 C5 C6 O2 -176.97(18) . . . . ? C11 C5 C6 O2 6.6(3) . . . . ? P2 O2 C6 C1 3.0(2) . . . . ? P2 O2 C6 C5 -176.58(15) . . . . ? C2 C3 C7 C8 -63.1(3) . . . . ? C4 C3 C7 C8 116.3(2) . . . . ? C2 C3 C7 C10 177.04(19) . . . . ? C4 C3 C7 C10 -3.6(3) . . . . ? C2 C3 C7 C9 58.1(3) . . . . ? C4 C3 C7 C9 -122.5(2) . . . . ? C4 C5 C11 C12 2.4(3) . . . . ? C6 C5 C11 C12 178.6(2) . . . . ? C4 C5 C11 C13 122.0(2) . . . . ? C6 C5 C11 C13 -61.7(3) . . . . ? C4 C5 C11 C14 -115.8(3) . . . . ? C6 C5 C11 C14 60.4(3) . . . . ? P1 O3 C15 C24 -70.68(19) . . . . ? P1 O3 C15 C16 113.09(16) . . . . ? C24 C15 C16 C17 3.1(3) . . . . ? O3 C15 C16 C17 179.05(16) . . . . ? C24 C15 C16 Si1 -165.03(15) . . . . ? O3 C15 C16 Si1 10.9(2) . . . . ? C47 Si1 C16 C17 161.50(15) . . . . ? C35 Si1 C16 C17 -80.11(17) . . . . ? C41 Si1 C16 C17 39.81(18) . . . . ? C47 Si1 C16 C15 -30.7(2) . . . . ? C35 Si1 C16 C15 87.69(17) . . . . ? C41 Si1 C16 C15 -152.40(16) . . . . ? C15 C16 C17 C18 1.6(3) . . . . ? Si1 C16 C17 C18 170.43(15) . . . . ? C16 C17 C18 C23 -2.5(3) . . . . ? C16 C17 C18 C19 178.41(18) . . . . ? C17 C18 C19 C20 -179.93(19) . . . . ? C23 C18 C19 C20 1.0(3) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C22 0.3(3) . . . . ? C20 C21 C22 C23 -2.3(3) . . . . ? C21 C22 C23 C18 3.5(3) . . . . ? C21 C22 C23 C24 -177.42(19) . . . . ? C17 C18 C23 C22 178.06(18) . . . . ? C19 C18 C23 C22 -2.8(3) . . . . ? C17 C18 C23 C24 -1.1(3) . . . . ? C19 C18 C23 C24 178.08(17) . . . . ? O3 C15 C24 C23 177.64(15) . . . . ? C16 C15 C24 C23 -6.5(3) . . . . ? O3 C15 C24 C25 -2.3(2) . . . . ? C16 C15 C24 C25 173.58(17) . . . . ? C22 C23 C24 C15 -173.84(18) . . . . ? C18 C23 C24 C15 5.2(3) . . . . ? C22 C23 C24 C25 6.1(3) . . . . ? C18 C23 C24 C25 -174.89(16) . . . . ? C15 C24 C25 C34 53.0(2) . . . . ? C23 C24 C25 C34 -126.86(19) . . . . ? C15 C24 C25 C26 -126.78(19) . . . . ? C23 C24 C25 C26 53.3(3) . . . . ? C34 C25 C26 C31 5.1(3) . . . . ? C24 C25 C26 C31 -175.09(17) . . . . ? C34 C25 C26 C27 -173.31(18) . . . . ? C24 C25 C26 C27 6.5(3) . . . . ? C31 C26 C27 C28 3.1(3) . . . . ? C25 C26 C27 C28 -178.45(19) . . . . ? C26 C27 C28 C29 0.0(3) . . . . ? C27 C28 C29 C30 -2.5(3) . . . . ? C28 C29 C30 C31 1.6(3) . . . . ? C29 C30 C31 C32 -178.8(2) . . . . ? C29 C30 C31 C26 1.6(3) . . . . ? C27 C26 C31 C32 176.54(19) . . . . ? C25 C26 C31 C32 -1.9(3) . . . . ? C27 C26 C31 C30 -3.9(3) . . . . ? C25 C26 C31 C30 177.59(18) . . . . ? C30 C31 C32 C33 179.3(2) . . . . ? C26 C31 C32 C33 -1.2(3) . . . . ? C31 C32 C33 C34 0.9(3) . . . . ? C31 C32 C33 Si2 173.77(17) . . . . ? C59 Si2 C33 C32 44.08(18) . . . . ? C65 Si2 C33 C32 -73.68(18) . . . . ? C53 Si2 C33 C32 167.22(16) . . . . ? C59 Si2 C33 C34 -143.99(17) . . . . ? C65 Si2 C33 C34 98.25(18) . . . . ? C53 Si2 C33 C34 -20.9(2) . . . . ? C26 C25 C34 O4 177.88(16) . . . . ? C24 C25 C34 O4 -1.9(2) . . . . ? C26 C25 C34 C33 -5.7(3) . . . . ? C24 C25 C34 C33 174.51(17) . . . . ? P1 O4 C34 C25 -75.54(19) . . . . ? P1 O4 C34 C33 107.72(16) . . . . ? C32 C33 C34 C25 2.6(3) . . . . ? Si2 C33 C34 C25 -169.39(15) . . . . ? C32 C33 C34 O4 179.11(17) . . . . ? Si2 C33 C34 O4 7.1(3) . . . . ? C47 Si1 C35 C36 142.64(16) . . . . ? C16 Si1 C35 C36 16.14(18) . . . . ? C41 Si1 C35 C36 -102.28(17) . . . . ? C47 Si1 C35 C40 -34.98(18) . . . . ? C16 Si1 C35 C40 -161.48(16) . . . . ? C41 Si1 C35 C40 80.10(18) . . . . ? C40 C35 C36 C37 -0.5(3) . . . . ? Si1 C35 C36 C37 -178.20(17) . . . . ? C35 C36 C37 C38 -0.1(4) . . . . ? C36 C37 C38 C39 0.3(4) . . . . ? C37 C38 C39 C40 0.0(4) . . . . ? C38 C39 C40 C35 -0.6(4) . . . . ? C36 C35 C40 C39 0.9(3) . . . . ? Si1 C35 C40 C39 178.59(18) . . . . ? C47 Si1 C41 C46 -106.00(18) . . . . ? C16 Si1 C41 C46 22.9(2) . . . . ? C35 Si1 C41 C46 139.02(17) . . . . ? C47 Si1 C41 C42 67.36(18) . . . . ? C16 Si1 C41 C42 -163.74(16) . . . . ? C35 Si1 C41 C42 -47.62(19) . . . . ? C46 C41 C42 C43 -0.7(3) . . . . ? Si1 C41 C42 C43 -174.53(19) . . . . ? C41 C42 C43 C44 0.0(4) . . . . ? C42 C43 C44 C45 0.5(4) . . . . ? C43 C44 C45 C46 -0.2(4) . . . . ? C44 C45 C46 C41 -0.6(4) . . . . ? C42 C41 C46 C45 1.0(3) . . . . ? Si1 C41 C46 C45 174.47(18) . . . . ? C16 Si1 C47 C52 -106.99(17) . . . . ? C35 Si1 C47 C52 134.90(16) . . . . ? C41 Si1 C47 C52 16.24(19) . . . . ? C16 Si1 C47 C48 79.00(18) . . . . ? C35 Si1 C47 C48 -39.11(18) . . . . ? C41 Si1 C47 C48 -157.77(16) . . . . ? C52 C47 C48 C49 -0.8(3) . . . . ? Si1 C47 C48 C49 173.37(16) . . . . ? C47 C48 C49 C50 0.5(3) . . . . ? C48 C49 C50 C51 0.4(3) . . . . ? C49 C50 C51 C52 -0.9(3) . . . . ? C48 C47 C52 C51 0.3(3) . . . . ? Si1 C47 C52 C51 -173.86(17) . . . . ? C50 C51 C52 C47 0.6(3) . . . . ? C59 Si2 C53 C54 0.4(2) . . . . ? C65 Si2 C53 C54 117.70(18) . . . . ? C33 Si2 C53 C54 -122.19(18) . . . . ? C59 Si2 C53 C58 -168.49(17) . . . . ? C65 Si2 C53 C58 -51.17(19) . . . . ? C33 Si2 C53 C58 68.9(2) . . . . ? C58 C53 C54 C55 0.4(3) . . . . ? Si2 C53 C54 C55 -169.0(2) . . . . ? C53 C54 C55 C56 -1.0(4) . . . . ? C54 C55 C56 C57 1.1(4) . . . . ? C55 C56 C57 C58 -0.5(4) . . . . ? C56 C57 C58 C53 -0.1(4) . . . . ? C54 C53 C58 C57 0.2(3) . . . . ? Si2 C53 C58 C57 169.29(19) . . . . ? C65 Si2 C59 C64 -19.7(2) . . . . ? C53 Si2 C59 C64 94.00(19) . . . . ? C33 Si2 C59 C64 -135.14(18) . . . . ? C65 Si2 C59 C60 164.20(17) . . . . ? C53 Si2 C59 C60 -82.10(19) . . . . ? C33 Si2 C59 C60 48.76(19) . . . . ? C64 C59 C60 C61 0.4(3) . . . . ? Si2 C59 C60 C61 176.65(19) . . . . ? C59 C60 C61 C62 -0.1(4) . . . . ? C60 C61 C62 C63 -0.5(4) . . . . ? C61 C62 C63 C64 0.8(4) . . . . ? C62 C63 C64 C59 -0.5(4) . . . . ? C60 C59 C64 C63 -0.1(3) . . . . ? Si2 C59 C64 C63 -176.31(19) . . . . ? C59 Si2 C65 C70 -103.38(19) . . . . ? C53 Si2 C65 C70 140.99(18) . . . . ? C33 Si2 C65 C70 12.0(2) . . . . ? C59 Si2 C65 C66 76.39(19) . . . . ? C53 Si2 C65 C66 -39.24(19) . . . . ? C33 Si2 C65 C66 -168.25(17) . . . . ? C70 C65 C66 C67 0.1(3) . . . . ? Si2 C65 C66 C67 -179.66(19) . . . . ? C65 C66 C67 C68 -0.8(4) . . . . ? C66 C67 C68 C69 0.8(4) . . . . ? C67 C68 C69 C70 -0.3(4) . . . . ? C68 C69 C70 C65 -0.3(4) . . . . ? C66 C65 C70 C69 0.4(3) . . . . ? Si2 C65 C70 C69 -179.80(18) . . . . ? O2 P2 C71 C76 -158.59(17) . . . . ? C77 P2 C71 C76 93.86(18) . . . . ? Pd1 P2 C71 C76 -40.4(2) . . . . ? O2 P2 C71 C72 24.51(19) . . . . ? C77 P2 C71 C72 -83.04(19) . . . . ? Pd1 P2 C71 C72 142.68(15) . . . . ? C76 C71 C72 C73 1.7(3) . . . . ? P2 C71 C72 C73 178.53(18) . . . . ? C71 C72 C73 C74 -0.3(4) . . . . ? C72 C73 C74 C75 -1.4(4) . . . . ? C73 C74 C75 C76 1.8(4) . . . . ? C74 C75 C76 C71 -0.4(4) . . . . ? C72 C71 C76 C75 -1.3(3) . . . . ? P2 C71 C76 C75 -178.20(18) . . . . ? O2 P2 C77 C82 159.0(2) . . . . ? C71 P2 C77 C82 -94.3(2) . . . . ? Pd1 P2 C77 C82 42.1(2) . . . . ? O2 P2 C77 C78 -23.4(2) . . . . ? C71 P2 C77 C78 83.3(2) . . . . ? Pd1 P2 C77 C78 -140.30(17) . . . . ? C82 C77 C78 C79 -2.3(4) . . . . ? P2 C77 C78 C79 -179.9(2) . . . . ? C77 C78 C79 C80 1.7(5) . . . . ? C78 C79 C80 C81 -0.1(6) . . . . ? C79 C80 C81 C82 -1.0(6) . . . . ? C80 C81 C82 C77 0.4(5) . . . . ? C78 C77 C82 C81 1.2(4) . . . . ? P2 C77 C82 C81 178.8(3) . . . . ? C85 C84 C83 O5 18.7(9) . . . . ? C86 O5 C83 C84 -12.6(10) . . . . ? C83 O5 C86 C85 2.7(10) . . . . ? C83 C84 C85 C86 -17.3(9) . . . . ? O5 C86 C85 C84 9.0(9) . . . . ? C90A O6 C87 C88A 5.1(10) . . . . ? C90B O6 C87 C88A -45.8(12) . . . . ? O6 C87 C88A C89A 7.1(9) . . . . ? C87 C88A C89A C90A -16.2(10) . . . . ? C88A C89A C90A O6 20.2(12) . . . . ? C87 O6 C90A C89A -16.2(12) . . . . ? C90B O6 C90A C89A 64.8(11) . . . . ? C87 O6 C90B C89B 24.0(19) . . . . ? C90A O6 C90B C89B -84.8(17) . . . . ? C91A C92A C93A C94A -159.2(7) . . . . ? C92A C93A C94A C95A -143.8(10) . . . . ? C93A C94A C95A C96A -107.4(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.531 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.083