# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ; Easy one-pot syntheses of new dppm-type linkers for immobilizations ; _publ_contact_author_name 'ProfD Janet Bluemel' _publ_contact_author_address ; Department of Organic Chemistry University of Heidelberg Im Neuenheimer Feld 270 Heidelberg 69120 Heidelberg GERMANY ; _publ_contact_author_email J.BLUEMEL@URZ.UNI-HEIDELBERG.DE loop_ _publ_author_name _publ_author_address F.Piestert ;Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; R.Fetouaki ;Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; M.Bogza ;Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; T.Oeser ;Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; J.Blumel ;Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _ccdc_publ_extra_info 'goes with CCDC 249320 & 249321' data_rf2 _database_code_depnum_ccdc_archive 'CCDC 249320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'chelate phophine' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 O P2 Si' _chemical_formula_weight 486.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.282(3) _cell_length_b 12.582(3) _cell_length_c 18.736(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.513(5) _cell_angle_gamma 90.00 _cell_volume 2659.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5611 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.39 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9452 _exptl_absorpt_correction_T_max 0.9776 _exptl_absorpt_process_details ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26813 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.39 _reflns_number_total 6585 _reflns_number_gt 5419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.0950P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6585 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 0.71461(4) 0.22558(4) 0.26750(3) 0.01538(12) Uani 1 1 d . . . P2 P 0.93034(4) 0.17859(4) 0.18077(2) 0.01463(12) Uani 1 1 d . . . Si1 Si 0.93896(5) 0.17630(4) 0.34693(3) 0.01637(13) Uani 1 1 d . . . O1 O 0.84600(12) 0.18719(11) 0.41388(7) 0.0194(3) Uani 1 1 d . . . C1 C 0.85023(17) 0.14037(15) 0.26336(10) 0.0146(4) Uani 1 1 d . . . C2 C 0.64553(17) 0.21191(16) 0.17883(10) 0.0188(4) Uani 1 1 d . . . C3 C 0.6552(3) 0.2983(2) 0.13313(13) 0.0356(6) Uani 1 1 d . . . C4 C 0.6084(3) 0.2942(2) 0.06484(14) 0.0496(8) Uani 1 1 d . . . C5 C 0.5503(3) 0.2043(2) 0.04152(13) 0.0420(7) Uani 1 1 d . . . C6 C 0.5383(2) 0.1185(2) 0.08623(13) 0.0323(5) Uani 1 1 d . . . C7 C 0.58645(19) 0.12222(19) 0.15450(12) 0.0241(4) Uani 1 1 d . . . C8 C 0.61152(17) 0.14871(16) 0.32229(10) 0.0176(4) Uani 1 1 d . . . C9 C 0.61002(19) 0.03863(17) 0.33005(12) 0.0237(4) Uani 1 1 d . . . C10 C 0.5287(2) -0.01056(19) 0.37446(13) 0.0309(5) Uani 1 1 d . . . C11 C 0.4471(2) 0.0496(2) 0.41101(13) 0.0342(6) Uani 1 1 d . . . C12 C 0.4448(2) 0.1585(2) 0.40259(13) 0.0325(5) Uani 1 1 d . . . C13 C 0.52709(19) 0.20798(18) 0.35924(11) 0.0237(4) Uani 1 1 d . . . C14 C 0.87373(17) 0.09033(15) 0.11029(10) 0.0158(4) Uani 1 1 d . . . C15 C 0.8884(2) 0.12836(19) 0.04114(11) 0.0293(5) Uani 1 1 d . . . C16 C 0.8547(3) 0.0679(2) -0.01720(12) 0.0375(6) Uani 1 1 d . . . C17 C 0.8051(2) -0.03154(19) -0.00788(11) 0.0278(5) Uani 1 1 d . . . C18 C 0.78976(19) -0.07001(17) 0.06022(11) 0.0216(4) Uani 1 1 d . . . C19 C 0.82368(17) -0.00975(16) 0.11923(11) 0.0182(4) Uani 1 1 d . . . C20 C 1.07682(17) 0.11729(16) 0.19541(10) 0.0176(4) Uani 1 1 d . . . C21 C 1.17532(19) 0.18435(18) 0.19863(11) 0.0228(4) Uani 1 1 d . . . C22 C 1.2882(2) 0.1436(2) 0.21176(13) 0.0323(5) Uani 1 1 d . . . C23 C 1.3036(2) 0.0361(2) 0.22065(13) 0.0324(5) Uani 1 1 d . . . C24 C 1.2071(2) -0.0318(2) 0.21584(12) 0.0282(5) Uani 1 1 d . . . C25 C 1.09433(19) 0.00863(17) 0.20352(11) 0.0217(4) Uani 1 1 d . . . C26 C 1.0547(2) 0.0774(2) 0.37117(12) 0.0253(5) Uani 1 1 d . . . C27 C 1.0007(2) 0.31190(18) 0.33554(12) 0.0238(5) Uani 1 1 d . . . C28 C 0.8209(2) 0.11131(17) 0.46849(11) 0.0239(5) Uani 1 1 d . . . C29 C 0.7596(2) 0.1662(2) 0.52891(13) 0.0306(5) Uani 1 1 d . . . H1 H 0.832(2) 0.0658(19) 0.2663(12) 0.022(6) Uiso 1 1 d . . . H3 H 0.695(3) 0.357(2) 0.1463(15) 0.048(8) Uiso 1 1 d . . . H4 H 0.620(3) 0.355(2) 0.0330(16) 0.052(8) Uiso 1 1 d . . . H5 H 0.516(3) 0.200(2) -0.0029(18) 0.060(9) Uiso 1 1 d . . . H6 H 0.499(2) 0.062(2) 0.0704(13) 0.028(7) Uiso 1 1 d . . . H7 H 0.579(2) 0.065(2) 0.1810(13) 0.026(6) Uiso 1 1 d . . . H9 H 0.665(2) -0.0054(18) 0.3030(12) 0.022(6) Uiso 1 1 d . . . H10 H 0.531(2) -0.083(2) 0.3809(14) 0.036(7) Uiso 1 1 d . . . H11 H 0.393(2) 0.020(2) 0.4411(13) 0.031(7) Uiso 1 1 d . . . H12 H 0.387(2) 0.197(2) 0.4278(14) 0.039(7) Uiso 1 1 d . . . H13 H 0.529(2) 0.284(2) 0.3559(13) 0.027(6) Uiso 1 1 d . . . H15 H 0.921(2) 0.195(2) 0.0351(13) 0.029(6) Uiso 1 1 d . . . H16 H 0.862(3) 0.096(2) -0.0630(17) 0.055(9) Uiso 1 1 d . . . H17 H 0.783(2) -0.0730(19) -0.0469(13) 0.028(6) Uiso 1 1 d . . . H18 H 0.760(2) -0.1320(19) 0.0684(12) 0.021(6) Uiso 1 1 d . . . H19 H 0.808(2) -0.0379(19) 0.1666(13) 0.028(6) Uiso 1 1 d . . . H21 H 1.164(2) 0.258(2) 0.1940(12) 0.026(6) Uiso 1 1 d . . . H22 H 1.354(2) 0.194(2) 0.2120(14) 0.039(7) Uiso 1 1 d . . . H23 H 1.377(2) 0.008(2) 0.2301(14) 0.039(7) Uiso 1 1 d . . . H24 H 1.216(2) -0.103(2) 0.2215(13) 0.030(7) Uiso 1 1 d . . . H25 H 1.030(2) -0.037(2) 0.2000(12) 0.026(6) Uiso 1 1 d . . . H26A H 1.122(2) 0.083(2) 0.3420(14) 0.036(7) Uiso 1 1 d . . . H26B H 1.082(2) 0.090(2) 0.4202(15) 0.044(8) Uiso 1 1 d . . . H26C H 1.027(2) 0.008(2) 0.3708(14) 0.034(7) Uiso 1 1 d . . . H27A H 1.027(3) 0.323(2) 0.2892(16) 0.047(8) Uiso 1 1 d . . . H27B H 1.067(3) 0.327(3) 0.3661(18) 0.069(10) Uiso 1 1 d . . . H27C H 0.946(3) 0.359(3) 0.3485(18) 0.066(10) Uiso 1 1 d . . . H28A H 0.773(2) 0.058(2) 0.4497(13) 0.027(6) Uiso 1 1 d . . . H28B H 0.896(2) 0.0790(19) 0.4851(12) 0.025(6) Uiso 1 1 d . . . H29A H 0.748(2) 0.115(2) 0.5683(14) 0.034(7) Uiso 1 1 d . . . H29B H 0.805(2) 0.222(2) 0.5457(14) 0.038(7) Uiso 1 1 d . . . H29C H 0.687(3) 0.192(2) 0.5155(14) 0.035(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0178(2) 0.0134(2) 0.0149(2) -0.00024(18) -0.00138(18) 0.00151(19) P2 0.0181(2) 0.0128(2) 0.0130(2) 0.00003(18) -0.00155(18) -0.00042(19) Si1 0.0196(3) 0.0167(3) 0.0128(2) -0.0011(2) -0.0027(2) 0.0003(2) O1 0.0263(7) 0.0199(7) 0.0120(6) 0.0020(5) 0.0007(5) 0.0009(6) C1 0.0179(9) 0.0130(9) 0.0130(8) -0.0001(7) -0.0011(7) 0.0007(7) C2 0.0183(9) 0.0218(10) 0.0163(9) 0.0000(8) -0.0028(7) 0.0063(8) C3 0.0505(16) 0.0271(13) 0.0291(12) 0.0074(10) -0.0130(11) 0.0044(11) C4 0.078(2) 0.0412(16) 0.0289(14) 0.0140(12) -0.0180(14) 0.0076(15) C5 0.0505(16) 0.0526(17) 0.0226(12) -0.0022(11) -0.0153(11) 0.0203(13) C6 0.0265(12) 0.0421(15) 0.0282(12) -0.0120(11) -0.0084(10) 0.0080(11) C7 0.0228(11) 0.0275(12) 0.0218(10) -0.0007(9) -0.0021(8) 0.0034(9) C8 0.0188(9) 0.0193(10) 0.0147(9) -0.0011(7) -0.0035(7) -0.0020(7) C9 0.0239(10) 0.0215(11) 0.0255(11) 0.0009(9) -0.0009(8) 0.0016(9) C10 0.0359(13) 0.0229(12) 0.0338(13) 0.0060(10) -0.0024(10) -0.0085(10) C11 0.0370(13) 0.0401(14) 0.0256(12) -0.0019(10) 0.0087(10) -0.0171(11) C12 0.0311(12) 0.0363(14) 0.0302(12) -0.0132(10) 0.0093(10) -0.0077(10) C13 0.0265(11) 0.0206(11) 0.0241(11) -0.0056(8) 0.0023(8) -0.0024(8) C14 0.0176(9) 0.0162(9) 0.0135(9) -0.0022(7) -0.0009(7) 0.0010(7) C15 0.0476(14) 0.0225(11) 0.0179(10) 0.0015(9) -0.0024(10) -0.0103(10) C16 0.0649(18) 0.0323(13) 0.0152(10) 0.0015(9) -0.0024(11) -0.0131(12) C17 0.0375(13) 0.0284(12) 0.0174(10) -0.0079(9) -0.0040(9) -0.0037(10) C18 0.0228(10) 0.0171(10) 0.0250(11) -0.0041(8) 0.0003(8) -0.0029(8) C19 0.0186(10) 0.0191(10) 0.0170(9) 0.0000(8) 0.0008(7) -0.0005(8) C20 0.0175(9) 0.0234(10) 0.0118(9) -0.0034(7) -0.0007(7) 0.0014(8) C21 0.0232(11) 0.0243(11) 0.0210(10) -0.0057(9) 0.0015(8) -0.0033(9) C22 0.0196(11) 0.0411(14) 0.0362(13) -0.0122(11) -0.0002(9) -0.0029(10) C23 0.0215(11) 0.0445(15) 0.0310(12) -0.0108(11) -0.0047(9) 0.0114(10) C24 0.0308(12) 0.0275(12) 0.0263(11) -0.0041(9) -0.0047(9) 0.0099(10) C25 0.0230(10) 0.0226(11) 0.0196(10) -0.0029(8) -0.0017(8) 0.0018(9) C26 0.0266(12) 0.0297(13) 0.0194(10) -0.0003(9) -0.0059(9) 0.0061(9) C27 0.0300(12) 0.0213(11) 0.0201(11) -0.0040(9) 0.0017(9) -0.0060(9) C28 0.0343(12) 0.0196(11) 0.0177(10) 0.0030(8) -0.0026(9) -0.0056(9) C29 0.0394(14) 0.0315(13) 0.0210(11) 0.0034(10) 0.0050(10) -0.0067(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 C8 1.834(2) . ? P1 C2 1.837(2) . ? P1 C1 1.870(2) . ? P2 C14 1.8356(19) . ? P2 C20 1.842(2) . ? P2 C1 1.862(2) . ? Si1 O1 1.6479(15) . ? Si1 C27 1.856(2) . ? Si1 C26 1.856(2) . ? Si1 C1 1.9053(19) . ? O1 C28 1.430(2) . ? C1 H1 0.96(2) . ? C2 C7 1.386(3) . ? C2 C3 1.389(3) . ? C3 C4 1.381(3) . ? C3 H3 0.89(3) . ? C4 C5 1.377(4) . ? C4 H4 0.98(3) . ? C5 C6 1.375(4) . ? C5 H5 0.92(3) . ? C6 C7 1.386(3) . ? C6 H6 0.89(3) . ? C7 H7 0.88(3) . ? C8 C9 1.393(3) . ? C8 C13 1.398(3) . ? C9 C10 1.390(3) . ? C9 H9 0.98(2) . ? C10 C11 1.379(4) . ? C10 H10 0.92(3) . ? C11 C12 1.379(4) . ? C11 H11 0.91(3) . ? C12 C13 1.387(3) . ? C12 H12 0.94(3) . ? C13 H13 0.95(2) . ? C14 C19 1.391(3) . ? C14 C15 1.392(3) . ? C15 C16 1.382(3) . ? C15 H15 0.93(3) . ? C16 C17 1.382(3) . ? C16 H16 0.93(3) . ? C17 C18 1.377(3) . ? C17 H17 0.93(2) . ? C18 C19 1.391(3) . ? C18 H18 0.86(2) . ? C19 H19 0.97(2) . ? C20 C25 1.390(3) . ? C20 C21 1.396(3) . ? C21 C22 1.393(3) . ? C21 H21 0.94(3) . ? C22 C23 1.373(4) . ? C22 H22 0.98(3) . ? C23 C24 1.386(3) . ? C23 H23 0.92(3) . ? C24 C25 1.388(3) . ? C24 H24 0.91(3) . ? C25 H25 0.93(2) . ? C26 H26A 0.94(3) . ? C26 H26B 0.98(3) . ? C26 H26C 0.93(3) . ? C27 H27A 0.93(3) . ? C27 H27B 0.96(4) . ? C27 H27C 0.89(4) . ? C28 C29 1.501(3) . ? C28 H28A 0.93(3) . ? C28 H28B 0.99(2) . ? C29 H29A 0.99(3) . ? C29 H29B 0.92(3) . ? C29 H29C 0.92(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 P1 C2 101.00(9) . . ? C8 P1 C1 104.12(9) . . ? C2 P1 C1 104.45(9) . . ? C14 P2 C20 99.19(9) . . ? C14 P2 C1 105.85(9) . . ? C20 P2 C1 102.10(9) . . ? O1 Si1 C27 104.66(9) . . ? O1 Si1 C26 108.69(9) . . ? C27 Si1 C26 112.36(12) . . ? O1 Si1 C1 108.18(8) . . ? C27 Si1 C1 108.57(10) . . ? C26 Si1 C1 113.90(10) . . ? C28 O1 Si1 128.37(13) . . ? P2 C1 P1 106.84(9) . . ? P2 C1 Si1 111.49(10) . . ? P1 C1 Si1 104.71(9) . . ? P2 C1 H1 113.7(14) . . ? P1 C1 H1 112.7(14) . . ? Si1 C1 H1 107.0(14) . . ? C7 C2 C3 118.4(2) . . ? C7 C2 P1 124.94(16) . . ? C3 C2 P1 116.69(17) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 118.2(19) . . ? C2 C3 H3 121.1(19) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.9(18) . . ? C3 C4 H4 118.9(18) . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 117(2) . . ? C4 C5 H5 123(2) . . ? C5 C6 C7 119.7(2) . . ? C5 C6 H6 118.6(16) . . ? C7 C6 H6 121.7(16) . . ? C2 C7 C6 121.0(2) . . ? C2 C7 H7 121.9(16) . . ? C6 C7 H7 117.0(16) . . ? C9 C8 C13 118.03(19) . . ? C9 C8 P1 126.24(16) . . ? C13 C8 P1 115.74(16) . . ? C10 C9 C8 120.9(2) . . ? C10 C9 H9 118.9(13) . . ? C8 C9 H9 120.1(13) . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H10 119.6(17) . . ? C9 C10 H10 120.4(17) . . ? C12 C11 C10 120.0(2) . . ? C12 C11 H11 117.8(16) . . ? C10 C11 H11 122.2(16) . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 117.6(17) . . ? C13 C12 H12 122.3(17) . . ? C12 C13 C8 120.9(2) . . ? C12 C13 H13 120.2(14) . . ? C8 C13 H13 118.9(15) . . ? C19 C14 C15 118.35(18) . . ? C19 C14 P2 126.89(15) . . ? C15 C14 P2 114.70(15) . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15 120.7(15) . . ? C14 C15 H15 118.5(15) . . ? C15 C16 C17 120.5(2) . . ? C15 C16 H16 119.4(19) . . ? C17 C16 H16 120.0(19) . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17 119.7(15) . . ? C16 C17 H17 121.0(15) . . ? C17 C18 C19 120.6(2) . . ? C17 C18 H18 122.3(15) . . ? C19 C18 H18 117.1(15) . . ? C14 C19 C18 120.45(19) . . ? C14 C19 H19 121.0(14) . . ? C18 C19 H19 118.5(14) . . ? C25 C20 C21 118.53(19) . . ? C25 C20 P2 123.69(16) . . ? C21 C20 P2 117.78(16) . . ? C22 C21 C20 120.8(2) . . ? C22 C21 H21 120.4(15) . . ? C20 C21 H21 118.8(15) . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 122.7(16) . . ? C21 C22 H22 117.4(16) . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 120.7(17) . . ? C24 C23 H23 119.1(17) . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 121.1(16) . . ? C25 C24 H24 118.7(16) . . ? C24 C25 C20 120.5(2) . . ? C24 C25 H25 120.0(15) . . ? C20 C25 H25 119.4(15) . . ? Si1 C26 H26A 111.9(16) . . ? Si1 C26 H26B 109.7(16) . . ? H26A C26 H26B 107(2) . . ? Si1 C26 H26C 113.3(16) . . ? H26A C26 H26C 110(2) . . ? H26B C26 H26C 105(2) . . ? Si1 C27 H27A 111.4(18) . . ? Si1 C27 H27B 114(2) . . ? H27A C27 H27B 106(3) . . ? Si1 C27 H27C 109(2) . . ? H27A C27 H27C 113(3) . . ? H27B C27 H27C 104(3) . . ? O1 C28 C29 109.14(18) . . ? O1 C28 H28A 109.2(15) . . ? C29 C28 H28A 110.1(15) . . ? O1 C28 H28B 109.0(14) . . ? C29 C28 H28B 110.6(13) . . ? H28A C28 H28B 109(2) . . ? C28 C29 H29A 108.9(15) . . ? C28 C29 H29B 110.7(17) . . ? H29A C29 H29B 109(2) . . ? C28 C29 H29C 111.9(17) . . ? H29A C29 H29C 108(2) . . ? H29B C29 H29C 109(2) . . ? 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 C27 Si1 O1 C28 -144.32(17) . . . . ? C26 Si1 O1 C28 -24.08(19) . . . . ? C1 Si1 O1 C28 100.07(17) . . . . ? C14 P2 C1 P1 -91.12(10) . . . . ? C20 P2 C1 P1 165.54(9) . . . . ? C14 P2 C1 Si1 155.04(10) . . . . ? C20 P2 C1 Si1 51.70(12) . . . . ? C8 P1 C1 P2 155.65(9) . . . . ? C2 P1 C1 P2 50.10(12) . . . . ? C8 P1 C1 Si1 -85.98(10) . . . . ? C2 P1 C1 Si1 168.47(9) . . . . ? O1 Si1 C1 P2 156.98(9) . . . . ? C27 Si1 C1 P2 43.95(13) . . . . ? C26 Si1 C1 P2 -82.06(13) . . . . ? O1 Si1 C1 P1 41.82(11) . . . . ? C27 Si1 C1 P1 -71.21(12) . . . . ? C26 Si1 C1 P1 162.78(10) . . . . ? C8 P1 C2 C7 -34.9(2) . . . . ? C1 P1 C2 C7 73.00(19) . . . . ? C8 P1 C2 C3 145.88(18) . . . . ? C1 P1 C2 C3 -106.26(19) . . . . ? C7 C2 C3 C4 -0.8(4) . . . . ? P1 C2 C3 C4 178.5(2) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C3 C2 C7 C6 0.1(3) . . . . ? P1 C2 C7 C6 -179.12(17) . . . . ? C5 C6 C7 C2 0.7(3) . . . . ? C2 P1 C8 C9 81.50(19) . . . . ? C1 P1 C8 C9 -26.6(2) . . . . ? C2 P1 C8 C13 -98.42(16) . . . . ? C1 P1 C8 C13 153.46(15) . . . . ? C13 C8 C9 C10 -1.4(3) . . . . ? P1 C8 C9 C10 178.67(17) . . . . ? C8 C9 C10 C11 0.7(3) . . . . ? C9 C10 C11 C12 1.1(4) . . . . ? C10 C11 C12 C13 -2.2(4) . . . . ? C11 C12 C13 C8 1.4(4) . . . . ? C9 C8 C13 C12 0.3(3) . . . . ? P1 C8 C13 C12 -179.73(18) . . . . ? C20 P2 C14 C19 80.65(19) . . . . ? C1 P2 C14 C19 -24.8(2) . . . . ? C20 P2 C14 C15 -96.52(18) . . . . ? C1 P2 C14 C15 158.01(17) . . . . ? C19 C14 C15 C16 -0.4(4) . . . . ? P2 C14 C15 C16 177.0(2) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C15 C14 C19 C18 0.2(3) . . . . ? P2 C14 C19 C18 -176.85(16) . . . . ? C17 C18 C19 C14 -0.1(3) . . . . ? C14 P2 C20 C25 -47.30(18) . . . . ? C1 P2 C20 C25 61.23(18) . . . . ? C14 P2 C20 C21 132.85(16) . . . . ? C1 P2 C20 C21 -118.63(16) . . . . ? C25 C20 C21 C22 -1.9(3) . . . . ? P2 C20 C21 C22 178.01(17) . . . . ? C20 C21 C22 C23 1.0(3) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C22 C23 C24 C25 -1.3(3) . . . . ? C23 C24 C25 C20 0.4(3) . . . . ? C21 C20 C25 C24 1.2(3) . . . . ? P2 C20 C25 C24 -178.69(16) . . . . ? Si1 O1 C28 C29 163.40(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.535 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.064 ###END data_rf3 _database_code_depnum_ccdc_archive 'CCDC 249321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ylide _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H41 O P3 Si' _chemical_formula_weight 670.74 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.662(1) _cell_length_b 11.165(1) _cell_length_c 31.824(3) _cell_angle_alpha 81.616(2) _cell_angle_beta 81.460(2) _cell_angle_gamma 73.455(2) _cell_volume 3569.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5267 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.78 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9443 _exptl_absorpt_correction_T_max 0.9817 _exptl_absorpt_process_details ? _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28088 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.71 _reflns_number_total 12028 _reflns_number_gt 9256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12028 _refine_ls_number_parameters 1146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1186 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 0.82006(8) 0.49536(8) 0.37962(3) 0.01373(19) Uani 1 1 d . . . P2 P 0.85275(8) 0.73622(7) 0.39820(2) 0.01127(18) Uani 1 1 d . . . P3 P 0.86348(8) 0.62319(7) 0.46264(2) 0.01308(19) Uani 1 1 d . . . Si1 Si 0.90713(8) 0.69778(8) 0.30558(3) 0.0144(2) Uani 1 1 d . . . O1 O 0.8571(2) 0.85331(19) 0.30397(6) 0.0188(5) Uani 1 1 d . . . C1 C 0.8442(3) 0.6466(3) 0.36028(9) 0.0133(7) Uani 1 1 d . . . C2 C 0.6881(3) 0.4763(3) 0.35194(9) 0.0134(7) Uani 1 1 d . . . C3 C 0.5934(3) 0.5790(3) 0.33478(10) 0.0168(7) Uani 1 1 d . . . C4 C 0.4890(3) 0.5624(3) 0.31686(10) 0.0196(8) Uani 1 1 d . . . C5 C 0.4771(3) 0.4434(3) 0.31577(11) 0.0218(8) Uani 1 1 d . . . C6 C 0.5687(3) 0.3409(3) 0.33313(11) 0.0227(8) Uani 1 1 d . . . C7 C 0.6714(3) 0.3571(3) 0.35161(10) 0.0183(7) Uani 1 1 d . . . C8 C 0.9660(3) 0.3850(3) 0.35435(10) 0.0148(7) Uani 1 1 d . . . C9 C 0.9743(3) 0.3346(3) 0.31604(11) 0.0177(7) Uani 1 1 d . . . C10 C 1.0933(3) 0.2605(3) 0.29820(11) 0.0225(8) Uani 1 1 d . . . C11 C 1.2059(3) 0.2369(3) 0.31788(12) 0.0263(9) Uani 1 1 d . . . C12 C 1.1993(4) 0.2840(3) 0.35653(12) 0.0268(9) Uani 1 1 d . . . C13 C 1.0799(3) 0.3562(3) 0.37449(11) 0.0183(7) Uani 1 1 d . . . C14 C 0.7248(3) 0.8840(3) 0.40121(9) 0.0125(7) Uani 1 1 d . . . C15 C 0.7282(3) 0.9715(3) 0.42793(10) 0.0170(7) Uani 1 1 d . . . C16 C 0.6233(3) 1.0758(3) 0.43309(11) 0.0227(8) Uani 1 1 d . . . C17 C 0.5145(3) 1.0962(3) 0.41163(11) 0.0217(8) Uani 1 1 d . . . C18 C 0.5112(3) 1.0126(3) 0.38396(11) 0.0202(8) Uani 1 1 d . . . C19 C 0.6162(3) 0.9065(3) 0.37900(10) 0.0161(7) Uani 1 1 d . . . C20 C 1.0089(3) 0.7774(3) 0.39159(9) 0.0137(7) Uani 1 1 d . . . C21 C 1.1216(3) 0.6783(3) 0.39751(10) 0.0165(7) Uani 1 1 d . . . C22 C 1.2434(3) 0.7012(3) 0.39451(10) 0.0207(8) Uani 1 1 d . . . C23 C 1.2554(3) 0.8218(4) 0.38423(10) 0.0242(8) Uani 1 1 d . . . C24 C 1.1459(3) 0.9191(4) 0.37607(11) 0.0221(8) Uani 1 1 d . . . C25 C 1.0221(3) 0.8976(3) 0.38000(10) 0.0167(7) Uani 1 1 d . . . C26 C 0.6925(3) 0.6321(3) 0.48514(10) 0.0135(7) Uani 1 1 d . . . C27 C 0.5829(3) 0.6671(3) 0.46252(10) 0.0145(7) Uani 1 1 d . . . C28 C 0.4585(3) 0.6688(3) 0.48389(11) 0.0170(7) Uani 1 1 d . . . C29 C 0.4416(3) 0.6330(3) 0.52699(11) 0.0180(7) Uani 1 1 d . . . C30 C 0.5507(3) 0.5965(3) 0.54974(11) 0.0179(7) Uani 1 1 d . . . C31 C 0.6745(3) 0.5959(3) 0.52910(10) 0.0167(7) Uani 1 1 d . . . C32 C 0.8997(3) 0.7328(3) 0.49443(9) 0.0129(7) Uani 1 1 d . . . C33 C 1.0310(3) 0.7188(3) 0.49903(10) 0.0158(7) Uani 1 1 d . . . C34 C 1.0669(3) 0.7976(3) 0.52194(11) 0.0229(8) Uani 1 1 d . . . C35 C 0.9708(4) 0.8906(3) 0.54126(11) 0.0251(8) Uani 1 1 d . . . C36 C 0.8397(3) 0.9034(3) 0.53862(11) 0.0211(8) Uani 1 1 d . . . C37 C 0.8033(3) 0.8256(3) 0.51537(10) 0.0157(7) Uani 1 1 d . . . C38 C 1.0900(4) 0.6491(4) 0.29267(12) 0.0231(8) Uani 1 1 d . . . C39 C 0.8387(4) 0.6494(4) 0.26229(11) 0.0210(8) Uani 1 1 d . . . C40 C 0.8927(4) 0.9409(4) 0.27054(13) 0.0302(9) Uani 1 1 d . . . C41 C 0.8337(6) 1.0711(4) 0.28223(16) 0.0454(12) Uani 1 1 d . . . H3 H 0.600(3) 0.658(3) 0.3333(9) 0.005(8) Uiso 1 1 d . . . H4 H 0.423(3) 0.635(3) 0.3058(10) 0.015(8) Uiso 1 1 d . . . H5 H 0.406(3) 0.436(3) 0.3024(10) 0.017(8) Uiso 1 1 d . . . H6 H 0.557(3) 0.264(3) 0.3326(10) 0.022(9) Uiso 1 1 d . . . H7 H 0.732(3) 0.284(3) 0.3640(9) 0.015(8) Uiso 1 1 d . . . H9 H 0.902(3) 0.346(3) 0.3017(10) 0.013(8) Uiso 1 1 d . . . H10 H 1.095(3) 0.227(3) 0.2718(10) 0.019(9) Uiso 1 1 d . . . H11 H 1.284(3) 0.188(3) 0.3052(10) 0.017(8) Uiso 1 1 d . . . H12 H 1.271(4) 0.270(3) 0.3686(12) 0.038(11) Uiso 1 1 d . . . H13 H 1.072(3) 0.383(3) 0.4023(11) 0.021(9) Uiso 1 1 d . . . H14 H 0.732(5) 1.087(5) 0.2877(16) 0.091(19) Uiso 1 1 d . . . H15 H 0.802(3) 0.959(3) 0.4416(9) 0.009(8) Uiso 1 1 d . . . H16 H 0.629(3) 1.133(3) 0.4502(10) 0.021(9) Uiso 1 1 d . . . H17 H 0.442(3) 1.170(3) 0.4158(10) 0.017(8) Uiso 1 1 d . . . H18 H 0.441(3) 1.028(3) 0.3689(9) 0.010(8) Uiso 1 1 d . . . H19 H 0.614(3) 0.845(3) 0.3604(9) 0.008(8) Uiso 1 1 d . . . H21 H 1.110(3) 0.598(3) 0.4030(10) 0.019(9) Uiso 1 1 d . . . H22 H 1.318(3) 0.631(3) 0.3988(10) 0.019(9) Uiso 1 1 d . . . H23 H 1.338(3) 0.835(3) 0.3816(10) 0.017(9) Uiso 1 1 d . . . H24 H 1.148(3) 0.998(3) 0.3689(10) 0.015(9) Uiso 1 1 d . . . H25 H 0.951(3) 0.964(3) 0.3746(10) 0.021(9) Uiso 1 1 d . . . H27 H 0.590(3) 0.694(3) 0.4320(10) 0.015(8) Uiso 1 1 d . . . H28 H 0.386(3) 0.697(3) 0.4683(10) 0.014(8) Uiso 1 1 d . . . H29 H 0.357(3) 0.635(3) 0.5419(9) 0.012(8) Uiso 1 1 d . . . H30 H 0.542(3) 0.568(3) 0.5788(10) 0.006(7) Uiso 1 1 d . . . H31 H 0.742(3) 0.576(3) 0.5443(9) 0.009(8) Uiso 1 1 d . . . H33 H 1.096(3) 0.653(3) 0.4872(9) 0.005(7) Uiso 1 1 d . . . H34 H 1.156(3) 0.782(3) 0.5245(10) 0.016(9) Uiso 1 1 d . . . H35 H 1.001(3) 0.944(3) 0.5556(10) 0.025(9) Uiso 1 1 d . . . H36 H 0.773(3) 0.967(3) 0.5527(10) 0.019(9) Uiso 1 1 d . . . H37 H 0.715(3) 0.836(3) 0.5141(9) 0.005(7) Uiso 1 1 d . . . H38A H 1.114(3) 0.673(3) 0.2634(13) 0.036(11) Uiso 1 1 d . . . H38B H 1.133(3) 0.682(3) 0.3091(11) 0.026(10) Uiso 1 1 d . . . H38C H 1.121(3) 0.561(3) 0.2973(11) 0.025(10) Uiso 1 1 d . . . H39A H 0.743(4) 0.678(4) 0.2645(13) 0.053(13) Uiso 1 1 d . . . H39B H 0.869(3) 0.684(3) 0.2363(12) 0.032(10) Uiso 1 1 d . . . H39C H 0.864(4) 0.558(4) 0.2628(12) 0.044(12) Uiso 1 1 d . . . H40A H 0.989(4) 0.922(4) 0.2637(13) 0.051(12) Uiso 1 1 d . . . H40B H 0.860(4) 0.926(4) 0.2451(13) 0.049(12) Uiso 1 1 d . . . H41A H 0.872(5) 1.083(5) 0.3063(19) 0.10(2) Uiso 1 1 d . . . H41B H 0.855(4) 1.130(4) 0.2608(14) 0.049(12) Uiso 1 1 d . . . P4 P 0.41480(8) 0.12693(8) 0.14624(3) 0.01561(19) Uani 1 1 d . . . P5 P 0.66208(8) 0.07830(8) 0.08927(3) 0.01413(19) Uani 1 1 d . . . P6 P 0.56164(8) -0.05503(8) 0.07121(3) 0.0167(2) Uani 1 1 d . . . Si2 Si 0.62207(9) 0.28694(8) 0.14541(3) 0.0170(2) Uani 1 1 d . . . O2 O 0.7834(2) 0.2486(2) 0.13233(7) 0.0265(6) Uani 1 1 d . . . C42 C 0.5734(3) 0.1535(3) 0.13159(9) 0.0143(7) Uani 1 1 d . . . C43 C 0.4123(3) 0.0519(3) 0.20167(10) 0.0174(7) Uani 1 1 d . . . C44 C 0.2990(3) 0.0201(3) 0.22196(11) 0.0220(8) Uani 1 1 d . . . C45 C 0.2987(4) -0.0490(3) 0.26187(11) 0.0263(9) Uani 1 1 d . . . C46 C 0.4116(4) -0.0878(3) 0.28213(11) 0.0254(8) Uani 1 1 d . . . C47 C 0.5250(4) -0.0575(3) 0.26288(11) 0.0257(8) Uani 1 1 d . . . C48 C 0.5248(3) 0.0111(3) 0.22273(11) 0.0219(8) Uani 1 1 d . . . C49 C 0.3001(3) 0.2832(3) 0.15274(10) 0.0151(7) Uani 1 1 d . . . C50 C 0.2522(3) 0.3553(3) 0.11589(11) 0.0226(8) Uani 1 1 d . . . C51 C 0.1603(3) 0.4713(3) 0.11813(12) 0.0272(9) Uani 1 1 d . . . C52 C 0.1135(4) 0.5173(3) 0.15708(12) 0.0296(9) Uani 1 1 d . . . C53 C 0.1604(4) 0.4480(3) 0.19397(12) 0.0285(9) Uani 1 1 d . . . C54 C 0.2521(3) 0.3318(3) 0.19152(11) 0.0191(8) Uani 1 1 d . . . C55 C 0.8321(3) -0.0067(3) 0.09677(10) 0.0153(7) Uani 1 1 d . . . C56 C 0.8665(3) -0.0443(3) 0.13817(11) 0.0194(7) Uani 1 1 d . . . C57 C 0.9914(3) -0.1195(3) 0.14463(12) 0.0243(8) Uani 1 1 d . . . C58 C 1.0835(3) -0.1571(3) 0.11042(12) 0.0260(8) Uani 1 1 d . . . C59 C 1.0508(3) -0.1171(3) 0.06912(12) 0.0250(8) Uani 1 1 d . . . C60 C 0.9260(3) -0.0435(3) 0.06244(11) 0.0200(8) Uani 1 1 d . . . C61 C 0.6714(3) 0.1870(3) 0.04070(9) 0.0151(7) Uani 1 1 d . . . C62 C 0.7712(3) 0.2478(3) 0.03150(10) 0.0194(8) Uani 1 1 d . . . C63 C 0.7636(4) 0.3460(3) -0.00114(11) 0.0248(8) Uani 1 1 d . . . C64 C 0.6576(4) 0.3836(3) -0.02462(11) 0.0252(8) Uani 1 1 d . . . C65 C 0.5581(4) 0.3236(3) -0.01616(11) 0.0240(8) Uani 1 1 d . . . C66 C 0.5637(3) 0.2269(3) 0.01707(11) 0.0212(8) Uani 1 1 d . . . C67 C 0.5481(3) -0.1619(3) 0.11991(10) 0.0213(8) Uani 1 1 d . . . C68 C 0.4238(4) -0.1800(3) 0.13249(12) 0.0301(9) Uani 1 1 d . . . C69 C 0.3976(5) -0.2587(4) 0.16781(13) 0.0426(11) Uani 1 1 d . . . C70 C 0.4975(5) -0.3234(4) 0.19191(13) 0.0428(12) Uani 1 1 d . . . C71 C 0.6221(6) -0.3085(4) 0.18062(13) 0.0448(12) Uani 1 1 d . . . C72 C 0.6484(5) -0.2280(3) 0.14472(13) 0.0338(10) Uani 1 1 d . . . C73 C 0.6963(3) -0.1487(3) 0.03613(10) 0.0178(7) Uani 1 1 d . . . C74 C 0.7625(3) -0.2740(3) 0.04665(12) 0.0280(9) Uani 1 1 d . . . C75 C 0.8540(4) -0.3404(4) 0.01687(14) 0.0370(10) Uani 1 1 d . . . C76 C 0.8812(4) -0.2848(4) -0.02354(14) 0.0385(10) Uani 1 1 d . . . C77 C 0.8159(4) -0.1609(4) -0.03474(12) 0.0321(9) Uani 1 1 d . . . C78 C 0.7235(3) -0.0944(4) -0.00539(11) 0.0240(8) Uani 1 1 d . . . C79 C 0.5839(5) 0.3120(4) 0.20323(12) 0.0274(9) Uani 1 1 d . . . C80 C 0.5513(4) 0.4396(3) 0.11402(12) 0.0239(8) Uani 1 1 d . . . C81 C 0.8695(4) 0.3166(4) 0.14084(15) 0.0324(9) Uani 1 1 d . . . C82 C 0.9793(5) 0.2280(5) 0.16259(17) 0.0666(15) Uani 1 1 d . . . H82A H 0.9435 0.1852 0.1887 0.100 Uiso 1 1 calc R . . H82B H 1.0367 0.2748 0.1699 0.100 Uiso 1 1 calc R . . H82C H 1.0303 0.1657 0.1435 0.100 Uiso 1 1 calc R . . H44 H 0.221(3) 0.042(3) 0.2088(10) 0.023(9) Uiso 1 1 d . . . H45 H 0.221(3) -0.067(3) 0.2753(9) 0.006(7) Uiso 1 1 d . . . H46 H 0.409(3) -0.133(3) 0.3101(12) 0.030(10) Uiso 1 1 d . . . H47 H 0.609(4) -0.085(3) 0.2754(12) 0.041(11) Uiso 1 1 d . . . H48 H 0.600(3) 0.028(3) 0.2105(9) 0.011(8) Uiso 1 1 d . . . H50 H 0.288(3) 0.320(3) 0.0886(11) 0.028(10) Uiso 1 1 d . . . H51 H 0.128(3) 0.515(3) 0.0918(11) 0.021(9) Uiso 1 1 d . . . H52 H 0.054(4) 0.598(4) 0.1589(11) 0.036(10) Uiso 1 1 d . . . H53 H 0.126(3) 0.476(3) 0.2217(11) 0.025(9) Uiso 1 1 d . . . H54 H 0.283(3) 0.289(3) 0.2152(9) 0.001(7) Uiso 1 1 d . . . H56 H 0.802(3) -0.019(3) 0.1613(10) 0.019(9) Uiso 1 1 d . . . H57 H 1.011(3) -0.142(3) 0.1730(10) 0.018(9) Uiso 1 1 d . . . H58 H 1.172(4) -0.216(3) 0.1144(11) 0.041(11) Uiso 1 1 d . . . H59 H 1.113(3) -0.143(3) 0.0454(11) 0.033(10) Uiso 1 1 d . . . H60 H 0.904(3) -0.018(3) 0.0347(10) 0.011(8) Uiso 1 1 d . . . H62 H 0.844(3) 0.228(3) 0.0476(10) 0.019(9) Uiso 1 1 d . . . H63 H 0.832(3) 0.387(3) -0.0065(11) 0.029(10) Uiso 1 1 d . . . H64 H 0.653(3) 0.455(3) -0.0455(9) 0.004(7) Uiso 1 1 d . . . H65 H 0.474(3) 0.352(3) -0.0308(11) 0.032(10) Uiso 1 1 d . . . H66 H 0.496(3) 0.187(3) 0.0227(10) 0.018(9) Uiso 1 1 d . . . H68 H 0.355(4) -0.134(4) 0.1168(13) 0.048(13) Uiso 1 1 d . . . H69 H 0.310(4) -0.273(4) 0.1776(13) 0.050(13) Uiso 1 1 d . . . H70 H 0.477(4) -0.379(4) 0.2146(13) 0.049(12) Uiso 1 1 d . . . H71 H 0.700(4) -0.348(4) 0.1922(12) 0.038(12) Uiso 1 1 d . . . H72 H 0.735(3) -0.221(3) 0.1378(10) 0.018(9) Uiso 1 1 d . . . H74 H 0.741(3) -0.317(3) 0.0748(12) 0.034(10) Uiso 1 1 d . . . H75 H 0.894(4) -0.425(4) 0.0256(12) 0.038(11) Uiso 1 1 d . . . H76 H 0.941(4) -0.327(4) -0.0425(13) 0.046(12) Uiso 1 1 d . . . H77 H 0.836(3) -0.123(3) -0.0648(11) 0.028(9) Uiso 1 1 d . . . H78 H 0.677(3) -0.009(3) -0.0127(10) 0.023(9) Uiso 1 1 d . . . H79A H 0.623(3) 0.378(3) 0.2087(11) 0.034(10) Uiso 1 1 d . . . H79B H 0.617(4) 0.246(4) 0.2209(15) 0.064(15) Uiso 1 1 d . . . H79C H 0.494(5) 0.334(5) 0.2100(16) 0.089(19) Uiso 1 1 d . . . H80A H 0.596(3) 0.496(3) 0.1175(11) 0.031(10) Uiso 1 1 d . . . H80B H 0.456(3) 0.472(3) 0.1226(9) 0.014(8) Uiso 1 1 d . . . H80C H 0.568(3) 0.430(3) 0.0827(12) 0.037(11) Uiso 1 1 d . . . H81A H 0.907(4) 0.351(4) 0.1142(14) 0.053(13) Uiso 1 1 d . . . H81B H 0.821(5) 0.384(5) 0.1608(16) 0.088(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0150(4) 0.0131(4) 0.0129(4) -0.0031(3) -0.0008(3) -0.0030(3) P2 0.0124(4) 0.0109(4) 0.0100(4) -0.0016(3) -0.0012(3) -0.0021(3) P3 0.0150(4) 0.0131(4) 0.0109(4) -0.0010(3) -0.0023(3) -0.0031(3) Si1 0.0160(5) 0.0168(5) 0.0105(4) -0.0026(4) -0.0017(4) -0.0037(4) O1 0.0251(13) 0.0181(12) 0.0127(11) 0.0006(10) -0.0014(10) -0.0065(10) C1 0.0151(16) 0.0116(16) 0.0124(16) -0.0034(13) -0.0007(13) -0.0017(13) C2 0.0106(16) 0.0196(17) 0.0111(16) -0.0059(14) 0.0041(13) -0.0064(14) C3 0.0175(18) 0.0153(18) 0.0189(18) -0.0071(15) 0.0011(14) -0.0054(15) C4 0.0118(17) 0.025(2) 0.0199(18) -0.0029(16) -0.0014(14) -0.0010(15) C5 0.0165(18) 0.034(2) 0.0195(18) -0.0069(16) -0.0039(15) -0.0109(16) C6 0.027(2) 0.024(2) 0.0213(19) -0.0075(16) 0.0055(16) -0.0155(17) C7 0.0193(18) 0.0171(18) 0.0173(18) -0.0015(15) 0.0021(15) -0.0054(15) C8 0.0152(17) 0.0109(16) 0.0182(17) -0.0008(14) 0.0012(14) -0.0052(13) C9 0.0187(18) 0.0119(17) 0.0215(18) -0.0025(14) 0.0002(15) -0.0033(14) C10 0.028(2) 0.0149(18) 0.023(2) -0.0046(16) 0.0049(16) -0.0058(16) C11 0.0168(19) 0.0167(19) 0.035(2) -0.0018(17) 0.0094(17) 0.0045(15) C12 0.0175(19) 0.025(2) 0.034(2) 0.0072(17) -0.0066(17) -0.0022(16) C13 0.0198(18) 0.0132(17) 0.0205(19) -0.0001(15) -0.0049(15) -0.0018(14) C14 0.0171(17) 0.0118(16) 0.0079(15) -0.0001(13) 0.0016(13) -0.0047(13) C15 0.0210(18) 0.0129(17) 0.0161(17) -0.0002(14) -0.0060(15) -0.0015(15) C16 0.033(2) 0.0151(18) 0.0192(18) -0.0057(16) -0.0066(16) -0.0019(16) C17 0.0228(19) 0.0150(18) 0.0211(19) -0.0009(15) -0.0007(15) 0.0033(15) C18 0.0147(18) 0.0201(19) 0.0251(19) -0.0008(16) -0.0045(16) -0.0030(15) C19 0.0196(18) 0.0117(17) 0.0185(17) -0.0018(14) -0.0016(14) -0.0069(14) C20 0.0165(17) 0.0177(17) 0.0082(15) -0.0048(13) 0.0001(13) -0.0057(14) C21 0.0166(18) 0.0193(19) 0.0137(17) -0.0026(15) -0.0015(14) -0.0046(15) C22 0.0143(18) 0.032(2) 0.0131(17) -0.0026(16) -0.0025(14) -0.0013(16) C23 0.0160(19) 0.046(2) 0.0148(18) -0.0049(17) 0.0017(15) -0.0157(18) C24 0.028(2) 0.025(2) 0.0171(18) -0.0036(16) -0.0001(15) -0.0146(17) C25 0.0203(18) 0.0201(19) 0.0101(16) -0.0038(14) -0.0007(14) -0.0054(16) C26 0.0156(16) 0.0109(16) 0.0151(16) -0.0050(13) 0.0002(13) -0.0044(13) C27 0.0201(18) 0.0100(16) 0.0141(17) -0.0013(14) -0.0027(14) -0.0047(14) C28 0.0169(18) 0.0092(16) 0.0253(19) -0.0041(14) -0.0065(15) -0.0011(14) C29 0.0149(18) 0.0126(17) 0.0257(19) -0.0073(15) 0.0058(15) -0.0039(14) C30 0.028(2) 0.0110(17) 0.0132(18) -0.0007(14) 0.0016(15) -0.0045(14) C31 0.0204(18) 0.0150(18) 0.0147(17) -0.0031(14) -0.0039(15) -0.0031(15) C32 0.0172(17) 0.0126(16) 0.0072(15) 0.0015(13) -0.0003(13) -0.0032(13) C33 0.0171(17) 0.0173(18) 0.0120(16) 0.0007(14) -0.0039(14) -0.0031(15) C34 0.0174(19) 0.030(2) 0.0227(19) -0.0038(16) -0.0054(16) -0.0066(16) C35 0.031(2) 0.030(2) 0.0207(19) -0.0081(17) -0.0015(16) -0.0163(18) C36 0.0237(19) 0.0198(19) 0.0186(18) -0.0062(15) 0.0010(15) -0.0036(16) C37 0.0175(18) 0.0190(18) 0.0117(16) 0.0011(14) -0.0031(14) -0.0074(15) C38 0.022(2) 0.032(2) 0.016(2) -0.0029(18) -0.0021(16) -0.0089(18) C39 0.024(2) 0.028(2) 0.0117(18) -0.0036(16) -0.0050(15) -0.0051(17) C40 0.029(2) 0.027(2) 0.030(2) 0.0086(18) 0.0004(18) -0.0087(18) C41 0.081(4) 0.018(2) 0.038(3) 0.008(2) -0.013(3) -0.018(2) P4 0.0163(4) 0.0164(4) 0.0125(4) -0.0013(4) -0.0006(3) -0.0025(4) P5 0.0145(4) 0.0156(4) 0.0120(4) -0.0017(3) -0.0022(3) -0.0031(3) P6 0.0181(4) 0.0177(5) 0.0149(4) -0.0008(4) -0.0045(4) -0.0047(4) Si2 0.0186(5) 0.0176(5) 0.0149(5) -0.0027(4) -0.0035(4) -0.0039(4) O2 0.0201(13) 0.0270(14) 0.0355(14) -0.0121(12) -0.0021(11) -0.0075(11) C42 0.0163(17) 0.0126(16) 0.0121(16) -0.0008(13) -0.0020(13) -0.0006(13) C43 0.0208(18) 0.0144(17) 0.0135(16) -0.0012(14) 0.0012(14) -0.0012(14) C44 0.0186(19) 0.0204(19) 0.025(2) -0.0049(16) 0.0027(16) -0.0029(15) C45 0.029(2) 0.024(2) 0.025(2) -0.0014(16) 0.0123(17) -0.0126(17) C46 0.032(2) 0.022(2) 0.0149(18) 0.0014(16) 0.0050(16) -0.0012(17) C47 0.025(2) 0.024(2) 0.0191(19) -0.0004(16) 0.0006(16) 0.0049(16) C48 0.0178(19) 0.025(2) 0.0191(19) 0.0004(16) 0.0029(15) -0.0033(16) C49 0.0110(16) 0.0176(17) 0.0174(17) -0.0016(14) -0.0001(13) -0.0060(13) C50 0.0206(19) 0.028(2) 0.0172(18) -0.0010(16) -0.0001(15) -0.0051(16) C51 0.024(2) 0.028(2) 0.023(2) 0.0059(17) -0.0010(17) -0.0017(17) C52 0.026(2) 0.0150(19) 0.040(2) 0.0019(18) 0.0039(18) 0.0007(16) C53 0.032(2) 0.026(2) 0.024(2) -0.0072(17) 0.0039(17) -0.0026(17) C54 0.0180(18) 0.0233(19) 0.0148(18) -0.0020(16) -0.0010(15) -0.0043(15) C55 0.0170(17) 0.0102(16) 0.0185(17) -0.0012(14) -0.0002(14) -0.0046(14) C56 0.0183(18) 0.0184(18) 0.0185(18) -0.0033(15) -0.0005(15) -0.0002(15) C57 0.029(2) 0.023(2) 0.021(2) 0.0010(16) -0.0075(17) -0.0053(16) C58 0.0170(19) 0.024(2) 0.035(2) -0.0019(17) -0.0044(17) -0.0025(16) C59 0.0202(19) 0.027(2) 0.026(2) -0.0071(17) 0.0026(17) -0.0035(16) C60 0.0172(18) 0.0242(19) 0.0192(19) -0.0038(16) -0.0029(15) -0.0053(15) C61 0.0205(17) 0.0134(16) 0.0106(16) -0.0030(13) -0.0020(14) -0.0024(14) C62 0.0185(18) 0.0226(19) 0.0172(18) -0.0042(15) -0.0008(15) -0.0052(15) C63 0.028(2) 0.024(2) 0.0222(19) -0.0007(16) 0.0021(16) -0.0109(17) C64 0.033(2) 0.0190(19) 0.0182(19) 0.0062(16) 0.0007(16) -0.0041(17) C65 0.025(2) 0.0220(19) 0.0214(19) 0.0042(16) -0.0055(16) -0.0013(16) C66 0.0218(19) 0.0208(19) 0.0204(18) -0.0022(15) -0.0011(15) -0.0056(16) C67 0.031(2) 0.0149(18) 0.0185(18) -0.0047(15) -0.0049(15) -0.0045(15) C68 0.030(2) 0.022(2) 0.032(2) 0.0005(18) 0.0067(19) -0.0045(17) C69 0.055(3) 0.031(2) 0.035(2) 0.001(2) 0.014(2) -0.011(2) C70 0.088(4) 0.026(2) 0.019(2) -0.0040(19) 0.004(2) -0.027(3) C71 0.091(4) 0.028(2) 0.027(2) 0.0057(19) -0.038(3) -0.023(3) C72 0.051(3) 0.022(2) 0.037(2) 0.0011(18) -0.024(2) -0.017(2) C73 0.0171(17) 0.0197(18) 0.0211(18) -0.0065(15) -0.0065(14) -0.0080(14) C74 0.027(2) 0.026(2) 0.030(2) -0.0070(18) 0.0039(17) -0.0064(17) C75 0.031(2) 0.020(2) 0.056(3) -0.011(2) 0.005(2) -0.0019(18) C76 0.033(2) 0.044(3) 0.042(3) -0.025(2) 0.007(2) -0.010(2) C77 0.031(2) 0.048(3) 0.020(2) -0.0140(19) 0.0007(17) -0.013(2) C78 0.0233(19) 0.030(2) 0.0202(19) -0.0074(17) -0.0055(16) -0.0055(17) C79 0.041(3) 0.026(2) 0.019(2) -0.0052(18) -0.0077(19) -0.013(2) C80 0.029(2) 0.023(2) 0.022(2) -0.0016(16) -0.0081(17) -0.0081(18) C81 0.029(2) 0.034(2) 0.041(2) -0.007(2) -0.003(2) -0.0174(19) C82 0.054(3) 0.080(4) 0.082(4) 0.026(3) -0.038(3) -0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.787(3) . ? P1 C2 1.843(3) . ? P1 C8 1.847(3) . ? P2 C1 1.704(3) . ? P2 C14 1.822(3) . ? P2 C20 1.825(3) . ? P2 P3 2.2458(11) . ? P3 C26 1.837(3) . ? P3 C32 1.848(3) . ? Si1 O1 1.660(2) . ? Si1 C1 1.841(3) . ? Si1 C39 1.860(3) . ? Si1 C38 1.868(4) . ? O1 C40 1.421(4) . ? C2 C7 1.394(4) . ? C2 C3 1.398(4) . ? C3 C4 1.391(4) . ? C3 H3 0.89(3) . ? C4 C5 1.376(5) . ? C4 H4 0.97(3) . ? C5 C6 1.381(5) . ? C5 H5 0.95(3) . ? C6 C7 1.382(5) . ? C6 H6 0.91(3) . ? C7 H7 0.96(3) . ? C8 C13 1.392(4) . ? C8 C9 1.397(4) . ? C9 C10 1.394(4) . ? C9 H9 0.92(3) . ? C10 C11 1.377(5) . ? C10 H10 0.96(3) . ? C11 C12 1.392(5) . ? C11 H11 0.93(3) . ? C12 C13 1.390(5) . ? C12 H12 0.87(4) . ? C13 H13 0.96(3) . ? C14 C19 1.389(4) . ? C14 C15 1.396(4) . ? C15 C16 1.376(5) . ? C15 H15 0.92(3) . ? C16 C17 1.380(5) . ? C16 H16 0.91(3) . ? C17 C18 1.384(5) . ? C17 H17 0.97(3) . ? C18 C19 1.388(4) . ? C18 H18 0.91(3) . ? C19 H19 0.98(3) . ? C20 C25 1.380(4) . ? C20 C21 1.397(4) . ? C21 C22 1.381(5) . ? C21 H21 0.93(3) . ? C22 C23 1.376(5) . ? C22 H22 0.95(3) . ? C23 C24 1.377(5) . ? C23 H23 0.92(3) . ? C24 C25 1.392(5) . ? C24 H24 0.88(3) . ? C25 H25 0.91(3) . ? C26 C27 1.395(4) . ? C26 C31 1.399(4) . ? C27 C28 1.393(4) . ? C27 H27 0.97(3) . ? C28 C29 1.372(5) . ? C28 H28 0.94(3) . ? C29 C30 1.392(5) . ? C29 H29 0.95(3) . ? C30 C31 1.383(4) . ? C30 H30 0.93(3) . ? C31 H31 0.89(3) . ? C32 C33 1.391(4) . ? C32 C37 1.402(4) . ? C33 C34 1.384(5) . ? C33 H33 0.94(3) . ? C34 C35 1.378(5) . ? C34 H34 0.92(3) . ? C35 C36 1.378(5) . ? C35 H35 0.95(3) . ? C36 C37 1.385(5) . ? C36 H36 0.96(3) . ? C37 H37 0.92(3) . ? C38 H38A 0.95(4) . ? C38 H38B 0.92(4) . ? C38 H38C 0.94(4) . ? C39 H39A 0.97(4) . ? C39 H39B 0.92(4) . ? C39 H39C 0.97(4) . ? C40 C41 1.488(6) . ? C40 H40A 0.98(4) . ? C40 H40B 0.98(4) . ? C41 H14 1.03(5) . ? C41 H41A 0.96(6) . ? C41 H41B 0.92(4) . ? P4 C42 1.782(3) . ? P4 C43 1.839(3) . ? P4 C49 1.843(3) . ? P5 C42 1.706(3) . ? P5 C55 1.823(3) . ? P5 C61 1.830(3) . ? P5 P6 2.2436(12) . ? P6 C67 1.827(3) . ? P6 C73 1.847(3) . ? Si2 O2 1.654(2) . ? Si2 C42 1.840(3) . ? Si2 C80 1.862(4) . ? Si2 C79 1.869(4) . ? O2 C81 1.421(4) . ? C43 C48 1.390(5) . ? C43 C44 1.396(4) . ? C44 C45 1.387(5) . ? C44 H44 0.94(3) . ? C45 C46 1.380(5) . ? C45 H45 0.93(3) . ? C46 C47 1.379(5) . ? C46 H46 0.96(4) . ? C47 C48 1.391(5) . ? C47 H47 0.98(4) . ? C48 H48 0.89(3) . ? C49 C54 1.389(4) . ? C49 C50 1.397(4) . ? C50 C51 1.387(5) . ? C50 H50 0.99(3) . ? C51 C52 1.381(5) . ? C51 H51 0.96(3) . ? C52 C53 1.384(5) . ? C52 H52 0.95(4) . ? C53 C54 1.389(5) . ? C53 H53 0.96(3) . ? C54 H54 0.88(3) . ? C55 C60 1.392(4) . ? C55 C56 1.393(4) . ? C56 C57 1.384(5) . ? C56 H56 0.95(3) . ? C57 C58 1.381(5) . ? C57 H57 0.94(3) . ? C58 C59 1.387(5) . ? C58 H58 1.00(4) . ? C59 C60 1.379(5) . ? C59 H59 0.95(4) . ? C60 H60 0.93(3) . ? C61 C62 1.393(4) . ? C61 C66 1.396(4) . ? C62 C63 1.390(5) . ? C62 H62 0.95(3) . ? C63 C64 1.379(5) . ? C63 H63 0.95(4) . ? C64 C65 1.383(5) . ? C64 H64 0.96(3) . ? C65 C66 1.392(5) . ? C65 H65 1.02(3) . ? C66 H66 0.94(3) . ? C67 C68 1.390(5) . ? C67 C72 1.393(5) . ? C68 C69 1.368(5) . ? C68 H68 0.93(4) . ? C69 C70 1.374(6) . ? C69 H69 0.99(4) . ? C70 C71 1.375(6) . ? C70 H70 0.92(4) . ? C71 C72 1.393(6) . ? C71 H71 0.93(4) . ? C72 H72 0.94(3) . ? C73 C74 1.393(5) . ? C73 C78 1.396(5) . ? C74 C75 1.385(5) . ? C74 H74 0.98(4) . ? C75 C76 1.372(6) . ? C75 H75 0.94(4) . ? C76 C77 1.381(6) . ? C76 H76 0.89(4) . ? C77 C78 1.381(5) . ? C77 H77 1.01(3) . ? C78 H78 0.96(3) . ? C79 H79A 0.99(4) . ? C79 H79B 0.88(5) . ? C79 H79C 0.92(5) . ? C80 H80A 0.92(4) . ? C80 H80B 0.99(3) . ? C80 H80C 1.00(4) . ? C81 C82 1.487(6) . ? C81 H81A 0.96(4) . ? C81 H81B 1.03(5) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 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 P1 C2 107.19(14) . . ? C1 P1 C8 103.81(14) . . ? C2 P1 C8 101.38(14) . . ? C1 P2 C14 115.92(14) . . ? C1 P2 C20 112.51(14) . . ? C14 P2 C20 105.83(14) . . ? C1 P2 P3 110.63(11) . . ? C14 P2 P3 110.55(10) . . ? C20 P2 P3 100.19(10) . . ? C26 P3 C32 99.72(13) . . ? C26 P3 P2 106.16(10) . . ? C32 P3 P2 100.97(10) . . ? O1 Si1 C1 102.39(12) . . ? O1 Si1 C39 108.62(15) . . ? C1 Si1 C39 115.08(16) . . ? O1 Si1 C38 108.76(16) . . ? C1 Si1 C38 115.60(16) . . ? C39 Si1 C38 106.10(17) . . ? C40 O1 Si1 126.2(2) . . ? P2 C1 P1 115.95(17) . . ? P2 C1 Si1 114.85(17) . . ? P1 C1 Si1 126.70(17) . . ? C7 C2 C3 117.4(3) . . ? C7 C2 P1 120.0(2) . . ? C3 C2 P1 122.3(2) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 116.8(18) . . ? C2 C3 H3 121.9(18) . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9(18) . . ? C3 C4 H4 119.8(18) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H5 117.3(19) . . ? C6 C5 H5 123.3(19) . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 117(2) . . ? C7 C6 H6 122(2) . . ? C6 C7 C2 121.2(3) . . ? C6 C7 H7 118.1(18) . . ? C2 C7 H7 120.7(18) . . ? C13 C8 C9 117.6(3) . . ? C13 C8 P1 116.0(2) . . ? C9 C8 P1 126.2(2) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H9 116.6(19) . . ? C8 C9 H9 122.4(19) . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 121.3(19) . . ? C9 C10 H10 118.4(19) . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 119(2) . . ? C12 C11 H11 121.6(19) . . ? C13 C12 C11 119.7(3) . . ? C13 C12 H12 121(2) . . ? C11 C12 H12 119(2) . . ? C12 C13 C8 121.6(3) . . ? C12 C13 H13 120.7(19) . . ? C8 C13 H13 117.6(19) . . ? C19 C14 C15 118.9(3) . . ? C19 C14 P2 119.5(2) . . ? C15 C14 P2 121.5(2) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 121.0(18) . . ? C14 C15 H15 118.8(18) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119(2) . . ? C17 C16 H16 121(2) . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 118.9(19) . . ? C18 C17 H17 121.2(19) . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18 120.1(18) . . ? C19 C18 H18 120.4(19) . . ? C18 C19 C14 120.7(3) . . ? C18 C19 H19 120.4(17) . . ? C14 C19 H19 118.9(17) . . ? C25 C20 C21 119.0(3) . . ? C25 C20 P2 124.4(2) . . ? C21 C20 P2 116.6(2) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 123(2) . . ? C20 C21 H21 117(2) . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 121.7(19) . . ? C21 C22 H22 118.2(19) . . ? C22 C23 C24 119.7(3) . . ? C22 C23 H23 118.8(19) . . ? C24 C23 H23 121(2) . . ? C23 C24 C25 120.7(3) . . ? C23 C24 H24 124(2) . . ? C25 C24 H24 115(2) . . ? C20 C25 C24 119.8(3) . . ? C20 C25 H25 121(2) . . ? C24 C25 H25 119(2) . . ? C27 C26 C31 118.4(3) . . ? C27 C26 P3 126.4(2) . . ? C31 C26 P3 115.2(2) . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27 118.6(18) . . ? C26 C27 H27 121.3(18) . . ? C29 C28 C27 121.2(3) . . ? C29 C28 H28 120.3(19) . . ? C27 C28 H28 118.5(19) . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 121.9(18) . . ? C30 C29 H29 119.0(18) . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.1(18) . . ? C29 C30 H30 120.4(18) . . ? C30 C31 C26 120.8(3) . . ? C30 C31 H31 119.2(19) . . ? C26 C31 H31 119.9(19) . . ? C33 C32 C37 118.2(3) . . ? C33 C32 P3 117.6(2) . . ? C37 C32 P3 124.2(2) . . ? C34 C33 C32 121.3(3) . . ? C34 C33 H33 119.5(17) . . ? C32 C33 H33 119.1(17) . . ? C35 C34 C33 119.5(3) . . ? C35 C34 H34 123.1(19) . . ? C33 C34 H34 117.3(19) . . ? C36 C35 C34 120.3(3) . . ? C36 C35 H35 124(2) . . ? C34 C35 H35 116(2) . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36 120.3(19) . . ? C37 C36 H36 119.4(19) . . ? C36 C37 C32 120.2(3) . . ? C36 C37 H37 118.8(17) . . ? C32 C37 H37 121.1(17) . . ? Si1 C38 H38A 111(2) . . ? Si1 C38 H38B 113(2) . . ? H38A C38 H38B 109(3) . . ? Si1 C38 H38C 110(2) . . ? H38A C38 H38C 107(3) . . ? H38B C38 H38C 107(3) . . ? Si1 C39 H39A 113(2) . . ? Si1 C39 H39B 109(2) . . ? H39A C39 H39B 107(3) . . ? Si1 C39 H39C 111(2) . . ? H39A C39 H39C 108(3) . . ? H39B C39 H39C 109(3) . . ? O1 C40 C41 109.8(3) . . ? O1 C40 H40A 111(2) . . ? C41 C40 H40A 112(2) . . ? O1 C40 H40B 106(2) . . ? C41 C40 H40B 112(2) . . ? H40A C40 H40B 105(3) . . ? C40 C41 H14 109(3) . . ? C40 C41 H41A 110(3) . . ? H14 C41 H41A 113(4) . . ? C40 C41 H41B 111(3) . . ? H14 C41 H41B 110(4) . . ? H41A C41 H41B 104(4) . . ? C42 P4 C43 106.72(14) . . ? C42 P4 C49 105.60(14) . . ? C43 P4 C49 101.65(14) . . ? C42 P5 C55 115.29(15) . . ? C42 P5 C61 112.08(14) . . ? C55 P5 C61 105.62(14) . . ? C42 P5 P6 110.83(11) . . ? C55 P5 P6 108.65(10) . . ? C61 P5 P6 103.60(10) . . ? C67 P6 C73 104.09(15) . . ? C67 P6 P5 104.03(11) . . ? C73 P6 P5 100.53(10) . . ? O2 Si2 C42 103.33(13) . . ? O2 Si2 C80 107.65(16) . . ? C42 Si2 C80 114.26(16) . . ? O2 Si2 C79 109.58(17) . . ? C42 Si2 C79 114.34(17) . . ? C80 Si2 C79 107.41(19) . . ? C81 O2 Si2 125.0(2) . . ? P5 C42 P4 114.27(17) . . ? P5 C42 Si2 117.78(17) . . ? P4 C42 Si2 124.74(17) . . ? C48 C43 C44 117.7(3) . . ? C48 C43 P4 122.2(2) . . ? C44 C43 P4 119.6(3) . . ? C45 C44 C43 121.0(3) . . ? C45 C44 H44 117(2) . . ? C43 C44 H44 121(2) . . ? C46 C45 C44 120.1(3) . . ? C46 C45 H45 120.2(17) . . ? C44 C45 H45 119.7(18) . . ? C47 C46 C45 120.2(3) . . ? C47 C46 H46 121(2) . . ? C45 C46 H46 119(2) . . ? C46 C47 C48 119.4(4) . . ? C46 C47 H47 123(2) . . ? C48 C47 H47 117(2) . . ? C43 C48 C47 121.6(3) . . ? C43 C48 H48 120.3(19) . . ? C47 C48 H48 118.0(19) . . ? C54 C49 C50 117.6(3) . . ? C54 C49 P4 125.2(2) . . ? C50 C49 P4 117.2(2) . . ? C51 C50 C49 121.0(3) . . ? C51 C50 H50 122(2) . . ? C49 C50 H50 117(2) . . ? C52 C51 C50 120.4(3) . . ? C52 C51 H51 122.2(19) . . ? C50 C51 H51 117.3(19) . . ? C51 C52 C53 119.6(3) . . ? C51 C52 H52 121(2) . . ? C53 C52 H52 119(2) . . ? C52 C53 C54 119.7(3) . . ? C52 C53 H53 121(2) . . ? C54 C53 H53 119(2) . . ? C49 C54 C53 121.7(3) . . ? C49 C54 H54 119.2(18) . . ? C53 C54 H54 119.0(18) . . ? C60 C55 C56 118.9(3) . . ? C60 C55 P5 121.9(2) . . ? C56 C55 P5 119.0(2) . . ? C57 C56 C55 120.0(3) . . ? C57 C56 H56 121.9(19) . . ? C55 C56 H56 118.1(19) . . ? C58 C57 C56 120.8(3) . . ? C58 C57 H57 121.7(19) . . ? C56 C57 H57 117.5(19) . . ? C57 C58 C59 119.5(3) . . ? C57 C58 H58 122(2) . . ? C59 C58 H58 118(2) . . ? C60 C59 C58 120.1(3) . . ? C60 C59 H59 120(2) . . ? C58 C59 H59 120(2) . . ? C59 C60 C55 120.8(3) . . ? C59 C60 H60 119.8(18) . . ? C55 C60 H60 119.4(18) . . ? C62 C61 C66 119.2(3) . . ? C62 C61 P5 121.1(2) . . ? C66 C61 P5 118.6(2) . . ? C63 C62 C61 120.0(3) . . ? C63 C62 H62 117.3(19) . . ? C61 C62 H62 122.6(19) . . ? C64 C63 C62 120.3(3) . . ? C64 C63 H63 121(2) . . ? C62 C63 H63 118(2) . . ? C63 C64 C65 120.5(3) . . ? C63 C64 H64 117.5(17) . . ? C65 C64 H64 121.9(17) . . ? C64 C65 C66 119.6(3) . . ? C64 C65 H65 124.0(19) . . ? C66 C65 H65 116.1(19) . . ? C65 C66 C61 120.4(3) . . ? C65 C66 H66 119.3(19) . . ? C61 C66 H66 120.2(19) . . ? C68 C67 C72 117.5(3) . . ? C68 C67 P6 115.2(3) . . ? C72 C67 P6 127.3(3) . . ? C69 C68 C67 122.6(4) . . ? C69 C68 H68 119(2) . . ? C67 C68 H68 118(2) . . ? C68 C69 C70 119.3(4) . . ? C68 C69 H69 124(2) . . ? C70 C69 H69 117(2) . . ? C69 C70 C71 120.1(4) . . ? C69 C70 H70 117(3) . . ? C71 C70 H70 123(3) . . ? C70 C71 C72 120.5(4) . . ? C70 C71 H71 131(2) . . ? C72 C71 H71 109(2) . . ? C71 C72 C67 120.1(4) . . ? C71 C72 H72 118(2) . . ? C67 C72 H72 122(2) . . ? C74 C73 C78 117.7(3) . . ? C74 C73 P6 124.4(3) . . ? C78 C73 P6 117.5(2) . . ? C75 C74 C73 120.4(4) . . ? C75 C74 H74 119(2) . . ? C73 C74 H74 120(2) . . ? C76 C75 C74 121.0(4) . . ? C76 C75 H75 122(2) . . ? C74 C75 H75 116(2) . . ? C75 C76 C77 119.5(4) . . ? C75 C76 H76 121(3) . . ? C77 C76 H76 119(3) . . ? C78 C77 C76 119.9(4) . . ? C78 C77 H77 122.0(19) . . ? C76 C77 H77 118.1(19) . . ? C77 C78 C73 121.5(4) . . ? C77 C78 H78 121(2) . . ? C73 C78 H78 118(2) . . ? Si2 C79 H79A 109(2) . . ? Si2 C79 H79B 115(3) . . ? H79A C79 H79B 105(3) . . ? Si2 C79 H79C 109(3) . . ? H79A C79 H79C 112(4) . . ? H79B C79 H79C 108(4) . . ? Si2 C80 H80A 109(2) . . ? Si2 C80 H80B 111.6(17) . . ? H80A C80 H80B 111(3) . . ? Si2 C80 H80C 110(2) . . ? H80A C80 H80C 105(3) . . ? H80B C80 H80C 110(3) . . ? O2 C81 C82 108.9(3) . . ? O2 C81 H81A 109(3) . . ? C82 C81 H81A 108(2) . . ? O2 C81 H81B 111(3) . . ? C82 C81 H81B 108(3) . . ? H81A C81 H81B 112(4) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? 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 P2 P3 C26 -85.48(15) . . . . ? C14 P2 P3 C26 44.32(15) . . . . ? C20 P2 P3 C26 155.63(14) . . . . ? C1 P2 P3 C32 170.92(15) . . . . ? C14 P2 P3 C32 -59.29(15) . . . . ? C20 P2 P3 C32 52.02(14) . . . . ? C1 Si1 O1 C40 171.9(3) . . . . ? C39 Si1 O1 C40 -66.0(3) . . . . ? C38 Si1 O1 C40 49.1(3) . . . . ? C14 P2 C1 P1 -117.68(17) . . . . ? C20 P2 C1 P1 120.33(18) . . . . ? P3 P2 C1 P1 9.2(2) . . . . ? C14 P2 C1 Si1 79.0(2) . . . . ? C20 P2 C1 Si1 -43.0(2) . . . . ? P3 P2 C1 Si1 -154.11(12) . . . . ? C2 P1 C1 P2 132.89(17) . . . . ? C8 P1 C1 P2 -120.32(18) . . . . ? C2 P1 C1 Si1 -66.1(2) . . . . ? C8 P1 C1 Si1 40.7(2) . . . . ? O1 Si1 C1 P2 -37.95(19) . . . . ? C39 Si1 C1 P2 -155.58(18) . . . . ? C38 Si1 C1 P2 80.1(2) . . . . ? O1 Si1 C1 P1 160.84(19) . . . . ? C39 Si1 C1 P1 43.2(3) . . . . ? C38 Si1 C1 P1 -81.1(3) . . . . ? C1 P1 C2 C7 162.8(2) . . . . ? C8 P1 C2 C7 54.3(3) . . . . ? C1 P1 C2 C3 -24.2(3) . . . . ? C8 P1 C2 C3 -132.7(3) . . . . ? C7 C2 C3 C4 -2.0(5) . . . . ? P1 C2 C3 C4 -175.2(2) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 0.9(5) . . . . ? C4 C5 C6 C7 0.2(5) . . . . ? C5 C6 C7 C2 -2.2(5) . . . . ? C3 C2 C7 C6 3.1(4) . . . . ? P1 C2 C7 C6 176.4(2) . . . . ? C1 P1 C8 C13 82.2(3) . . . . ? C2 P1 C8 C13 -166.7(2) . . . . ? C1 P1 C8 C9 -93.7(3) . . . . ? C2 P1 C8 C9 17.4(3) . . . . ? C13 C8 C9 C10 -1.4(5) . . . . ? P1 C8 C9 C10 174.5(2) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C9 C10 C11 C12 2.2(5) . . . . ? C10 C11 C12 C13 -1.2(5) . . . . ? C11 C12 C13 C8 -1.2(5) . . . . ? C9 C8 C13 C12 2.5(5) . . . . ? P1 C8 C13 C12 -173.8(3) . . . . ? C1 P2 C14 C19 11.4(3) . . . . ? C20 P2 C14 C19 136.9(2) . . . . ? P3 P2 C14 C19 -115.5(2) . . . . ? C1 P2 C14 C15 -173.6(2) . . . . ? C20 P2 C14 C15 -48.1(3) . . . . ? P3 P2 C14 C15 59.5(3) . . . . ? C19 C14 C15 C16 2.1(5) . . . . ? P2 C14 C15 C16 -172.9(2) . . . . ? C14 C15 C16 C17 -0.8(5) . . . . ? C15 C16 C17 C18 -1.3(5) . . . . ? C16 C17 C18 C19 1.9(5) . . . . ? C17 C18 C19 C14 -0.6(5) . . . . ? C15 C14 C19 C18 -1.5(4) . . . . ? P2 C14 C19 C18 173.7(2) . . . . ? C1 P2 C20 C25 112.3(3) . . . . ? C14 P2 C20 C25 -15.3(3) . . . . ? P3 P2 C20 C25 -130.2(3) . . . . ? C1 P2 C20 C21 -65.6(3) . . . . ? C14 P2 C20 C21 166.8(2) . . . . ? P3 P2 C20 C21 51.9(2) . . . . ? C25 C20 C21 C22 4.1(5) . . . . ? P2 C20 C21 C22 -177.9(2) . . . . ? C20 C21 C22 C23 -2.1(5) . . . . ? C21 C22 C23 C24 -1.4(5) . . . . ? C22 C23 C24 C25 2.9(5) . . . . ? C21 C20 C25 C24 -2.5(4) . . . . ? P2 C20 C25 C24 179.6(2) . . . . ? C23 C24 C25 C20 -0.9(5) . . . . ? C32 P3 C26 C27 122.4(3) . . . . ? P2 P3 C26 C27 17.9(3) . . . . ? C32 P3 C26 C31 -59.7(2) . . . . ? P2 P3 C26 C31 -164.2(2) . . . . ? C31 C26 C27 C28 1.7(4) . . . . ? P3 C26 C27 C28 179.6(2) . . . . ? C26 C27 C28 C29 -1.9(5) . . . . ? C27 C28 C29 C30 1.1(5) . . . . ? C28 C29 C30 C31 -0.2(5) . . . . ? C29 C30 C31 C26 0.1(5) . . . . ? C27 C26 C31 C30 -0.9(4) . . . . ? P3 C26 C31 C30 -178.9(2) . . . . ? C26 P3 C32 C33 156.5(2) . . . . ? P2 P3 C32 C33 -94.8(2) . . . . ? C26 P3 C32 C37 -21.1(3) . . . . ? P2 P3 C32 C37 87.6(3) . . . . ? C37 C32 C33 C34 -2.9(5) . . . . ? P3 C32 C33 C34 179.3(2) . . . . ? C32 C33 C34 C35 1.1(5) . . . . ? C33 C34 C35 C36 1.4(5) . . . . ? C34 C35 C36 C37 -2.1(5) . . . . ? C35 C36 C37 C32 0.2(5) . . . . ? C33 C32 C37 C36 2.2(4) . . . . ? P3 C32 C37 C36 179.8(2) . . . . ? Si1 O1 C40 C41 -176.7(3) . . . . ? C42 P5 P6 C67 -58.27(16) . . . . ? C55 P5 P6 C67 69.37(16) . . . . ? C61 P5 P6 C67 -178.67(15) . . . . ? C42 P5 P6 C73 -165.83(15) . . . . ? C55 P5 P6 C73 -38.19(15) . . . . ? C61 P5 P6 C73 73.78(15) . . . . ? C42 Si2 O2 C81 -173.5(3) . . . . ? C80 Si2 O2 C81 65.3(3) . . . . ? C79 Si2 O2 C81 -51.3(3) . . . . ? C55 P5 C42 P4 -132.41(16) . . . . ? C61 P5 C42 P4 106.72(18) . . . . ? P6 P5 C42 P4 -8.49(19) . . . . ? C55 P5 C42 Si2 66.8(2) . . . . ? C61 P5 C42 Si2 -54.0(2) . . . . ? P6 P5 C42 Si2 -169.23(12) . . . . ? C43 P4 C42 P5 119.38(18) . . . . ? C49 P4 C42 P5 -133.01(17) . . . . ? C43 P4 C42 Si2 -81.4(2) . . . . ? C49 P4 C42 Si2 26.2(2) . . . . ? O2 Si2 C42 P5 -32.2(2) . . . . ? C80 Si2 C42 P5 84.5(2) . . . . ? C79 Si2 C42 P5 -151.2(2) . . . . ? O2 Si2 C42 P4 169.27(18) . . . . ? C80 Si2 C42 P4 -74.1(2) . . . . ? C79 Si2 C42 P4 50.3(3) . . . . ? C42 P4 C43 C48 -8.3(3) . . . . ? C49 P4 C43 C48 -118.7(3) . . . . ? C42 P4 C43 C44 179.8(3) . . . . ? C49 P4 C43 C44 69.4(3) . . . . ? C48 C43 C44 C45 0.5(5) . . . . ? P4 C43 C44 C45 172.7(3) . . . . ? C43 C44 C45 C46 -0.2(5) . . . . ? C44 C45 C46 C47 0.3(5) . . . . ? C45 C46 C47 C48 -0.7(5) . . . . ? C44 C43 C48 C47 -0.9(5) . . . . ? P4 C43 C48 C47 -173.0(3) . . . . ? C46 C47 C48 C43 1.1(5) . . . . ? C42 P4 C49 C54 -99.4(3) . . . . ? C43 P4 C49 C54 11.9(3) . . . . ? C42 P4 C49 C50 84.5(3) . . . . ? C43 P4 C49 C50 -164.3(3) . . . . ? C54 C49 C50 C51 0.2(5) . . . . ? P4 C49 C50 C51 176.7(3) . . . . ? C49 C50 C51 C52 -0.6(5) . . . . ? C50 C51 C52 C53 1.2(6) . . . . ? C51 C52 C53 C54 -1.3(6) . . . . ? C50 C49 C54 C53 -0.4(5) . . . . ? P4 C49 C54 C53 -176.6(3) . . . . ? C52 C53 C54 C49 1.0(5) . . . . ? C42 P5 C55 C60 -162.4(3) . . . . ? C61 P5 C55 C60 -38.1(3) . . . . ? P6 P5 C55 C60 72.5(3) . . . . ? C42 P5 C55 C56 22.6(3) . . . . ? C61 P5 C55 C56 146.9(3) . . . . ? P6 P5 C55 C56 -102.5(2) . . . . ? C60 C55 C56 C57 -1.5(5) . . . . ? P5 C55 C56 C57 173.7(3) . . . . ? C55 C56 C57 C58 0.5(5) . . . . ? C56 C57 C58 C59 1.2(5) . . . . ? C57 C58 C59 C60 -2.0(5) . . . . ? C58 C59 C60 C55 1.1(5) . . . . ? C56 C55 C60 C59 0.7(5) . . . . ? P5 C55 C60 C59 -174.3(3) . . . . ? C42 P5 C61 C62 88.4(3) . . . . ? C55 P5 C61 C62 -37.9(3) . . . . ? P6 P5 C61 C62 -152.0(2) . . . . ? C42 P5 C61 C66 -79.5(3) . . . . ? C55 P5 C61 C66 154.2(2) . . . . ? P6 P5 C61 C66 40.0(3) . . . . ? C66 C61 C62 C63 -0.6(5) . . . . ? P5 C61 C62 C63 -168.5(2) . . . . ? C61 C62 C63 C64 -0.2(5) . . . . ? C62 C63 C64 C65 -0.3(5) . . . . ? C63 C64 C65 C66 1.7(5) . . . . ? C64 C65 C66 C61 -2.5(5) . . . . ? C62 C61 C66 C65 2.0(5) . . . . ? P5 C61 C66 C65 170.1(3) . . . . ? C73 P6 C67 C68 -124.8(3) . . . . ? P5 P6 C67 C68 130.4(2) . . . . ? C73 P6 C67 C72 53.8(3) . . . . ? P5 P6 C67 C72 -51.1(3) . . . . ? C72 C67 C68 C69 0.2(5) . . . . ? P6 C67 C68 C69 178.9(3) . . . . ? C67 C68 C69 C70 -0.3(6) . . . . ? C68 C69 C70 C71 0.3(6) . . . . ? C69 C70 C71 C72 -0.1(6) . . . . ? C70 C71 C72 C67 0.0(6) . . . . ? C68 C67 C72 C71 0.0(5) . . . . ? P6 C67 C72 C71 -178.5(3) . . . . ? C67 P6 C73 C74 2.6(3) . . . . ? P5 P6 C73 C74 110.1(3) . . . . ? C67 P6 C73 C78 175.3(3) . . . . ? P5 P6 C73 C78 -77.2(3) . . . . ? C78 C73 C74 C75 1.3(5) . . . . ? P6 C73 C74 C75 174.1(3) . . . . ? C73 C74 C75 C76 -0.2(6) . . . . ? C74 C75 C76 C77 -0.3(6) . . . . ? C75 C76 C77 C78 -0.3(6) . . . . ? C76 C77 C78 C73 1.5(6) . . . . ? C74 C73 C78 C77 -2.0(5) . . . . ? P6 C73 C78 C77 -175.2(3) . . . . ? Si2 O2 C81 C82 128.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.477 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.063 ###END data_fp3 _database_code_depnum_ccdc_archive 'CCDC 256229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 Ni O3 P2 Si' _chemical_formula_weight 601.31 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.9502(3) _cell_length_b 10.9104(2) _cell_length_c 14.8819(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3076.90(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7948 _exptl_absorpt_correction_T_max 0.8823 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30254 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7017 _reflns_number_gt 5547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^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 calculated _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 0.016(9) _refine_ls_number_reflns 7017 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Ni1 Ni 0.065969(15) 0.64824(3) 0.44640(2) 0.02742(8) Uani 1 1 d . . . P1 P 0.08845(3) 0.64679(6) 0.29903(4) 0.02354(13) Uani 1 1 d . . . P2 P -0.04011(3) 0.64601(5) 0.38038(4) 0.02375(13) Uani 1 1 d . . . Si1 Si -0.02123(3) 0.84866(6) 0.22091(5) 0.03107(16) Uani 1 1 d . . . C1 C 0.08591(14) 0.7874(3) 0.5009(2) 0.0429(7) Uani 1 1 d . . . O1 O 0.09907(13) 0.8776(2) 0.5365(2) 0.0791(8) Uani 1 1 d . . . C2 C 0.08998(15) 0.5114(3) 0.5032(2) 0.0451(7) Uani 1 1 d . . . O2 O 0.10446(15) 0.4236(3) 0.54087(18) 0.0828(8) Uani 1 1 d . . . C3 C 0.02212(16) 0.8672(3) 0.10953(18) 0.0472(7) Uani 1 1 d . . . H3A H 0.0733 0.8579 0.1163 0.071 Uiso 1 1 calc R . . H3B H 0.0116 0.9488 0.0856 0.071 Uiso 1 1 calc R . . H3C H 0.0043 0.8047 0.0681 0.071 Uiso 1 1 calc R . . O3 O 0.00913(9) 0.94682(15) 0.29468(12) 0.0389(4) Uani 1 1 d . . . C4 C -0.11757(14) 0.8666(3) 0.2009(2) 0.0465(8) Uani 1 1 d . . . H4A H -0.1430 0.8579 0.2579 0.070 Uiso 1 1 calc R . . H4B H -0.1336 0.8035 0.1588 0.070 Uiso 1 1 calc R . . H4C H -0.1269 0.9479 0.1755 0.070 Uiso 1 1 calc R . . C5 C 0.0137(2) 1.0763(3) 0.2777(3) 0.0728(11) Uani 1 1 d . . . H5A H -0.0344 1.1110 0.2720 0.087 Uiso 1 1 calc R . . H5B H 0.0390 1.0906 0.2205 0.087 Uiso 1 1 calc R . . C6 C 0.0517(2) 1.1383(3) 0.3523(2) 0.0708(11) Uani 1 1 d . . . H6A H 0.0549 1.2263 0.3397 0.106 Uiso 1 1 calc R . . H6B H 0.0993 1.1039 0.3578 0.106 Uiso 1 1 calc R . . H6C H 0.0259 1.1256 0.4087 0.106 Uiso 1 1 calc R . . C10 C -0.00381(12) 0.6909(2) 0.26848(15) 0.0244(5) Uani 1 1 d . . . H10 H -0.0212 0.6297 0.2236 0.029 Uiso 1 1 calc R . . C11 C 0.15060(11) 0.7467(2) 0.23837(17) 0.0291(6) Uani 1 1 d . . . C12 C 0.16826(13) 0.8575(2) 0.2787(2) 0.0389(6) Uani 1 1 d . . . H12 H 0.1495 0.8777 0.3360 0.047 Uiso 1 1 calc R . . C13 C 0.21343(15) 0.9389(3) 0.2352(2) 0.0505(8) Uani 1 1 d . . . H13 H 0.2246 1.0155 0.2619 0.061 Uiso 1 1 calc R . . C14 C 0.24169(15) 0.9073(3) 0.1533(2) 0.0527(8) Uani 1 1 d . . . H14 H 0.2730 0.9623 0.1239 0.063 Uiso 1 1 calc R . . C15 C 0.22519(13) 0.7968(3) 0.1132(2) 0.0468(7) Uani 1 1 d . . . H15 H 0.2452 0.7759 0.0568 0.056 Uiso 1 1 calc R . . C16 C 0.17933(12) 0.7167(2) 0.15572(18) 0.0354(6) Uani 1 1 d . . . H16 H 0.1676 0.6409 0.1281 0.042 Uiso 1 1 calc R . . C21 C 0.10607(12) 0.5002(2) 0.24408(15) 0.0263(5) Uani 1 1 d . . . C22 C 0.17070(13) 0.4454(2) 0.26366(18) 0.0383(6) Uani 1 1 d . . . H22 H 0.2008 0.4819 0.3071 0.046 Uiso 1 1 calc R . . C23 C 0.19171(15) 0.3392(3) 0.2212(2) 0.0477(7) Uani 1 1 d . . . H23 H 0.2364 0.3042 0.2346 0.057 Uiso 1 1 calc R . . C24 C 0.14794(15) 0.2840(2) 0.15936(18) 0.0421(7) Uani 1 1 d . . . H24 H 0.1625 0.2113 0.1296 0.051 Uiso 1 1 calc R . . C25 C 0.08345(14) 0.3342(2) 0.14089(19) 0.0396(7) Uani 1 1 d . . . H25 H 0.0527 0.2949 0.0996 0.048 Uiso 1 1 calc R . . C26 C 0.06279(13) 0.4425(2) 0.18230(16) 0.0326(6) Uani 1 1 d . . . H26 H 0.0183 0.4776 0.1680 0.039 Uiso 1 1 calc R . . C31 C -0.11574(12) 0.7438(2) 0.41025(15) 0.0256(5) Uani 1 1 d . . . C32 C -0.10277(13) 0.8630(2) 0.43928(19) 0.0324(5) Uani 1 1 d . . . H32 H -0.0555 0.8913 0.4441 0.039 Uiso 1 1 calc R . . C33 C -0.15780(14) 0.9406(2) 0.46121(16) 0.0394(6) Uani 1 1 d . . . H33 H -0.1482 1.0223 0.4795 0.047 Uiso 1 1 calc R . . C34 C -0.22620(14) 0.9001(3) 0.45660(19) 0.0448(7) Uani 1 1 d . . . H34 H -0.2639 0.9541 0.4708 0.054 Uiso 1 1 calc R . . C35 C -0.24022(13) 0.7809(3) 0.4314(2) 0.0460(7) Uani 1 1 d . . . H35 H -0.2875 0.7519 0.4299 0.055 Uiso 1 1 calc R . . C36 C -0.18514(12) 0.7034(2) 0.40815(17) 0.0353(6) Uani 1 1 d . . . H36 H -0.1951 0.6215 0.3906 0.042 Uiso 1 1 calc R . . C41 C -0.08351(12) 0.4996(2) 0.35880(16) 0.0279(6) Uani 1 1 d . . . C42 C -0.08295(13) 0.4123(2) 0.42661(19) 0.0398(7) Uani 1 1 d . . . H42 H -0.0591 0.4287 0.4814 0.048 Uiso 1 1 calc R . . C43 C -0.11744(15) 0.3001(3) 0.4145(2) 0.0558(9) Uani 1 1 d . . . H43 H -0.1180 0.2413 0.4616 0.067 Uiso 1 1 calc R . . C44 C -0.15017(17) 0.2754(3) 0.3351(2) 0.0577(9) Uani 1 1 d . . . H44 H -0.1728 0.1985 0.3268 0.069 Uiso 1 1 calc R . . C45 C -0.15091(15) 0.3598(3) 0.2668(2) 0.0511(8) Uani 1 1 d . . . H45 H -0.1738 0.3413 0.2117 0.061 Uiso 1 1 calc R . . C46 C -0.11812(13) 0.4726(2) 0.27851(19) 0.0386(6) Uani 1 1 d . . . H46 H -0.1193 0.5315 0.2316 0.046 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 Ni1 0.02782(15) 0.02914(16) 0.02529(14) -0.00137(18) -0.00466(14) 0.00084(13) P1 0.0215(3) 0.0228(3) 0.0264(3) 0.0015(3) -0.0020(2) -0.0003(2) P2 0.0237(3) 0.0219(3) 0.0256(3) 0.0003(3) -0.0013(2) -0.0012(3) Si1 0.0291(4) 0.0303(4) 0.0338(4) 0.0102(3) 0.0018(3) 0.0063(3) C1 0.0351(15) 0.0475(19) 0.0462(17) -0.0146(15) -0.0103(13) 0.0034(13) O1 0.0766(17) 0.0651(17) 0.096(2) -0.0456(15) -0.0280(15) 0.0017(13) C2 0.0436(16) 0.054(2) 0.0380(16) 0.0077(14) -0.0016(13) 0.0114(14) O2 0.102(2) 0.0706(17) 0.0755(17) 0.0330(15) -0.0085(15) 0.0275(16) C3 0.0470(17) 0.056(2) 0.0381(16) 0.0171(14) 0.0025(13) 0.0155(14) O3 0.0451(10) 0.0267(9) 0.0448(10) 0.0070(9) 0.0080(9) -0.0013(8) C4 0.0353(15) 0.054(2) 0.0499(18) 0.0174(14) 0.0008(13) 0.0115(13) C5 0.099(3) 0.0280(17) 0.091(3) 0.0024(18) -0.009(2) -0.0066(17) C6 0.107(3) 0.0396(19) 0.066(2) -0.0119(16) 0.020(2) -0.0156(18) C10 0.0242(12) 0.0217(11) 0.0274(12) 0.0007(10) -0.0024(10) 0.0003(9) C11 0.0209(12) 0.0298(14) 0.0367(14) 0.0095(11) -0.0060(11) -0.0003(10) C12 0.0329(14) 0.0376(15) 0.0463(16) 0.0072(13) -0.0067(12) -0.0054(12) C13 0.0438(16) 0.0425(17) 0.065(2) 0.0164(16) -0.0173(16) -0.0193(14) C14 0.0388(16) 0.066(2) 0.0532(19) 0.0276(17) -0.0145(15) -0.0213(15) C15 0.0305(15) 0.066(2) 0.0445(17) 0.0232(16) 0.0011(13) -0.0033(14) C16 0.0290(14) 0.0390(17) 0.0380(15) 0.0084(13) -0.0025(12) -0.0007(11) C21 0.0276(12) 0.0269(13) 0.0244(13) 0.0042(10) 0.0003(10) -0.0008(10) C22 0.0377(14) 0.0358(15) 0.0413(15) -0.0092(13) -0.0096(12) 0.0099(12) C23 0.0444(16) 0.0466(18) 0.0522(18) -0.0055(14) -0.0109(15) 0.0183(14) C24 0.0562(18) 0.0333(16) 0.0369(15) -0.0091(13) 0.0019(14) 0.0084(13) C25 0.0466(16) 0.0369(17) 0.0354(15) -0.0075(12) -0.0002(12) -0.0024(12) C26 0.0332(13) 0.0331(14) 0.0315(13) -0.0029(11) -0.0029(11) 0.0025(11) C31 0.0274(12) 0.0256(13) 0.0239(11) 0.0014(10) 0.0014(10) 0.0018(10) C32 0.0383(13) 0.0294(13) 0.0295(12) 0.0019(12) 0.0024(12) -0.0013(10) C33 0.0565(17) 0.0307(14) 0.0310(16) -0.0017(12) 0.0023(13) 0.0061(12) C34 0.0471(16) 0.0497(16) 0.0377(17) -0.0041(14) -0.0003(14) 0.0208(13) C35 0.0290(13) 0.0587(19) 0.0502(19) -0.0119(15) -0.0019(13) 0.0065(12) C36 0.0298(13) 0.0327(14) 0.0432(14) -0.0067(12) -0.0034(12) -0.0004(11) C41 0.0235(13) 0.0247(12) 0.0355(15) -0.0043(11) 0.0007(10) 0.0012(10) C42 0.0446(15) 0.0310(14) 0.0438(19) 0.0028(12) -0.0051(12) -0.0081(12) C43 0.0564(19) 0.0300(16) 0.081(2) 0.0146(15) -0.0070(17) -0.0125(14) C44 0.0515(19) 0.0334(18) 0.088(2) -0.0063(17) -0.0093(17) -0.0162(15) C45 0.0441(17) 0.0486(18) 0.0606(19) -0.0159(16) -0.0125(15) -0.0113(14) C46 0.0346(14) 0.0397(15) 0.0414(16) -0.0008(13) -0.0068(12) -0.0080(12) _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 Ni1 C1 1.763(3) . ? Ni1 C2 1.775(3) . ? Ni1 P1 2.2342(6) . ? Ni1 P2 2.2376(7) . ? P1 C21 1.827(2) . ? P1 C11 1.841(2) . ? P1 C10 1.869(2) . ? P2 C41 1.825(2) . ? P2 C31 1.841(2) . ? P2 C10 1.867(2) . ? Si1 O3 1.6381(19) . ? Si1 C4 1.860(3) . ? Si1 C3 1.861(3) . ? Si1 C10 1.890(2) . ? C1 O1 1.145(3) . ? C2 O2 1.143(3) . ? O3 C5 1.437(3) . ? C5 C6 1.486(5) . ? C11 C16 1.384(4) . ? C11 C12 1.391(3) . ? C12 C13 1.393(4) . ? C13 C14 1.376(5) . ? C14 C15 1.381(4) . ? C15 C16 1.386(3) . ? C21 C26 1.383(3) . ? C21 C22 1.393(3) . ? C22 C23 1.378(4) . ? C23 C24 1.378(4) . ? C24 C25 1.367(4) . ? C25 C26 1.389(4) . ? C31 C36 1.387(3) . ? C31 C32 1.392(3) . ? C32 C33 1.383(3) . ? C33 C34 1.371(4) . ? C34 C35 1.380(4) . ? C35 C36 1.387(3) . ? C41 C42 1.388(3) . ? C41 C46 1.395(3) . ? C42 C43 1.399(4) . ? C43 C44 1.362(4) . ? C44 C45 1.371(4) . ? C45 C46 1.389(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 C2 116.81(14) . . ? C1 Ni1 P1 114.62(10) . . ? C2 Ni1 P1 114.37(10) . . ? C1 Ni1 P2 113.82(9) . . ? C2 Ni1 P2 115.48(10) . . ? P1 Ni1 P2 74.94(2) . . ? C21 P1 C11 100.48(11) . . ? C21 P1 C10 106.70(10) . . ? C11 P1 C10 109.06(10) . . ? C21 P1 Ni1 118.71(8) . . ? C11 P1 Ni1 126.80(8) . . ? C10 P1 Ni1 93.36(7) . . ? C41 P2 C31 101.47(11) . . ? C41 P2 C10 103.80(11) . . ? C31 P2 C10 110.50(10) . . ? C41 P2 Ni1 119.44(8) . . ? C31 P2 Ni1 125.94(8) . . ? C10 P2 Ni1 93.31(7) . . ? O3 Si1 C4 112.53(12) . . ? O3 Si1 C3 111.77(12) . . ? C4 Si1 C3 106.22(13) . . ? O3 Si1 C10 106.44(9) . . ? C4 Si1 C10 109.10(11) . . ? C3 Si1 C10 110.82(11) . . ? O1 C1 Ni1 179.7(3) . . ? O2 C2 Ni1 178.8(3) . . ? C5 O3 Si1 123.09(19) . . ? O3 C5 C6 110.2(3) . . ? P2 C10 P1 93.45(10) . . ? P2 C10 Si1 120.55(12) . . ? P1 C10 Si1 119.26(12) . . ? C16 C11 C12 119.7(2) . . ? C16 C11 P1 123.17(19) . . ? C12 C11 P1 117.2(2) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 120.9(3) . . ? C14 C15 C16 119.8(3) . . ? C11 C16 C15 120.2(3) . . ? C26 C21 C22 117.7(2) . . ? C26 C21 P1 125.95(18) . . ? C22 C21 P1 116.26(18) . . ? C23 C22 C21 121.2(2) . . ? C24 C23 C22 120.0(2) . . ? C25 C24 C23 119.8(2) . . ? C24 C25 C26 120.2(2) . . ? C21 C26 C25 121.0(2) . . ? C36 C31 C32 118.1(2) . . ? C36 C31 P2 123.25(18) . . ? C32 C31 P2 118.60(17) . . ? C33 C32 C31 120.8(2) . . ? C34 C33 C32 120.2(2) . . ? C33 C34 C35 120.0(2) . . ? C34 C35 C36 119.8(2) . . ? C35 C36 C31 120.9(2) . . ? C42 C41 C46 118.8(2) . . ? C42 C41 P2 118.00(18) . . ? C46 C41 P2 123.21(19) . . ? C41 C42 C43 120.2(3) . . ? C44 C43 C42 119.9(3) . . ? C43 C44 C45 120.9(3) . . ? C44 C45 C46 119.9(3) . . ? C45 C46 C41 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.376 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.048