# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wingard, Leah' _publ_contact_author_email pranger@email.unc.edu loop_ _publ_author_name L.Wingard P.White J.Templeton data_c08370 _database_code_depnum_ccdc_archive 'CCDC 877929' #TrackingRef '- c08370.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 N O3 P2 Si2 W' _chemical_formula_sum 'C33 H36 N O3 P2 Si2 W' _chemical_formula_weight 796.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' N N 0.0311 0.0180 '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' W W -5.4734 5.5774 '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/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.8236(8) _cell_length_b 18.5277(13) _cell_length_c 14.1186(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.327(5) _cell_angle_gamma 90.00 _cell_volume 3327.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3016 _cell_measurement_theta_min 5.91 _cell_measurement_theta_max 68.62 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 8.305 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3689 _exptl_absorpt_correction_T_max 0.6815 _exptl_absorpt_process_details 'Bruker-AXS APEX2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15353 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.91 _diffrn_reflns_theta_max 69.07 _reflns_number_total 5881 _reflns_number_gt 4566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0782P)^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 SHELXL _refine_ls_extinction_coef 0.00015(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5881 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 W1 W 0.95122(2) 0.828473(17) 0.51216(2) 0.01998(14) Uani 1 1 d . . . P1 P 0.78218(13) 0.88063(10) 0.54258(11) 0.0213(4) Uani 1 1 d . . . P2 P 1.13782(13) 0.79410(10) 0.51401(12) 0.0227(4) Uani 1 1 d . . . Si1 Si 0.90866(15) 0.90301(11) 0.73698(12) 0.0235(4) Uani 1 1 d . . . Si2 Si 1.12764(14) 0.83108(11) 0.72221(12) 0.0233(4) Uani 1 1 d . . . N1 N 1.0128(4) 0.8782(3) 0.6697(4) 0.0218(12) Uani 1 1 d . . . C1 C 0.9025(5) 0.7900(4) 0.3859(5) 0.0252(15) Uani 1 1 d . . . O1 O 0.8741(4) 0.7680(3) 0.3095(3) 0.0310(12) Uani 1 1 d . . . C2 C 0.9124(5) 0.7275(4) 0.5543(5) 0.0208(13) Uani 1 1 d . . . O2 O 0.8877(5) 0.6692(3) 0.5671(4) 0.0381(13) Uani 1 1 d . . . C3 C 0.9713(5) 0.9199(4) 0.4401(5) 0.0227(14) Uani 1 1 d . . . O3 O 0.9732(4) 0.9669(3) 0.3876(4) 0.0356(13) Uani 1 1 d . . . C4 C 1.2159(5) 0.8266(4) 0.4220(5) 0.0251(14) Uani 1 1 d . . . C5 C 1.1686(5) 0.8447(4) 0.3306(5) 0.0256(15) Uani 1 1 d . . . H5 H 1.0963 0.8397 0.3154 0.031 Uiso 1 1 calc R . . C6 C 1.2286(6) 0.8704(4) 0.2614(5) 0.0283(16) Uani 1 1 d . . . H6 H 1.1960 0.8819 0.2006 0.034 Uiso 1 1 calc R . . C7 C 1.3366(6) 0.8789(4) 0.2835(5) 0.0324(17) Uani 1 1 d . . . H7 H 1.3764 0.8966 0.2379 0.039 Uiso 1 1 calc R . . C8 C 1.3848(6) 0.8607(4) 0.3738(5) 0.0297(16) Uani 1 1 d . . . H8 H 1.4571 0.8662 0.3887 0.036 Uiso 1 1 calc R . . C9 C 1.3258(6) 0.8342(4) 0.4425(5) 0.0290(16) Uani 1 1 d . . . H9 H 1.3593 0.8213 0.5024 0.035 Uiso 1 1 calc R . . C10 C 1.1682(5) 0.6967(4) 0.5130(5) 0.0259(15) Uani 1 1 d . . . C11 C 1.1081(7) 0.6538(5) 0.4440(6) 0.0379(19) Uani 1 1 d . . . H11 H 1.0541 0.6748 0.4029 0.045 Uiso 1 1 calc R . . C12 C 1.1284(7) 0.5811(5) 0.4365(6) 0.045(2) Uani 1 1 d . . . H12 H 1.0886 0.5536 0.3900 0.054 Uiso 1 1 calc R . . C13 C 1.2091(7) 0.5483(5) 0.4987(7) 0.043(2) Uani 1 1 d . . . H13 H 1.2233 0.4993 0.4939 0.051 Uiso 1 1 calc R . . C14 C 1.2669(7) 0.5908(5) 0.5673(7) 0.042(2) Uani 1 1 d . . . H14 H 1.3205 0.5698 0.6088 0.051 Uiso 1 1 calc R . . C15 C 1.2467(6) 0.6638(5) 0.5756(6) 0.0372(18) Uani 1 1 d . . . H15 H 1.2856 0.6909 0.6230 0.045 Uiso 1 1 calc R . . C16 C 1.2119(5) 0.8304(4) 0.6234(5) 0.0283(15) Uani 1 1 d . . . H16A H 1.2350 0.8791 0.6119 0.034 Uiso 1 1 calc R . . H16B H 1.2738 0.8009 0.6417 0.034 Uiso 1 1 calc R . . C17 C 1.1976(6) 0.8826(4) 0.8247(5) 0.0306(16) Uani 1 1 d . . . H17A H 1.2064 0.9318 0.8058 0.046 Uiso 1 1 calc R . . H17B H 1.2652 0.8613 0.8436 0.046 Uiso 1 1 calc R . . H17C H 1.1570 0.8813 0.8773 0.046 Uiso 1 1 calc R . . C18 C 1.0947(5) 0.7387(4) 0.7595(5) 0.0266(15) Uani 1 1 d . . . H18A H 1.0494 0.7416 0.8085 0.040 Uiso 1 1 calc R . . H18B H 1.1581 0.7137 0.7838 0.040 Uiso 1 1 calc R . . H18C H 1.0596 0.7130 0.7056 0.040 Uiso 1 1 calc R . . C19 C 0.8581(6) 0.8237(5) 0.7982(5) 0.0332(17) Uani 1 1 d . . . H19A H 0.8409 0.7857 0.7528 0.050 Uiso 1 1 calc R . . H19B H 0.7963 0.8374 0.8256 0.050 Uiso 1 1 calc R . . H19C H 0.9110 0.8073 0.8477 0.050 Uiso 1 1 calc R . . C20 C 0.9514(6) 0.9744(4) 0.8278(5) 0.0314(17) Uani 1 1 d . . . H20A H 1.0066 0.9558 0.8736 0.047 Uiso 1 1 calc R . . H20B H 0.8929 0.9884 0.8597 0.047 Uiso 1 1 calc R . . H20C H 0.9767 1.0157 0.7964 0.047 Uiso 1 1 calc R . . C21 C 0.8067(5) 0.9431(4) 0.6443(5) 0.0245(14) Uani 1 1 d . . . H21A H 0.7420 0.9513 0.6716 0.029 Uiso 1 1 calc R . . H21B H 0.8312 0.9891 0.6229 0.029 Uiso 1 1 calc R . . C22 C 0.7060(5) 0.9362(4) 0.4489(5) 0.0243(14) Uani 1 1 d . . . C23 C 0.7120(6) 0.9228(4) 0.3528(5) 0.0286(16) Uani 1 1 d . . . H23 H 0.7571 0.8873 0.3352 0.034 Uiso 1 1 calc R . . C24 C 0.6502(6) 0.9627(5) 0.2828(6) 0.0349(17) Uani 1 1 d . . . H24 H 0.6537 0.9531 0.2186 0.042 Uiso 1 1 calc R . . C25 C 0.5843(6) 1.0159(5) 0.3076(6) 0.0336(17) Uani 1 1 d . . . H25 H 0.5437 1.0424 0.2606 0.040 Uiso 1 1 calc R . . C26 C 0.5788(6) 1.0298(4) 0.4027(6) 0.0351(18) Uani 1 1 d . . . H26 H 0.5345 1.0660 0.4197 0.042 Uiso 1 1 calc R . . C27 C 0.6390(5) 0.9900(4) 0.4741(5) 0.0297(16) Uani 1 1 d . . . H27 H 0.6342 0.9993 0.5381 0.036 Uiso 1 1 calc R . . C28 C 0.6769(5) 0.8195(4) 0.5739(5) 0.0245(14) Uani 1 1 d . . . C29 C 0.6187(5) 0.8330(4) 0.6489(5) 0.0267(15) Uani 1 1 d . . . H29 H 0.6313 0.8744 0.6860 0.032 Uiso 1 1 calc R . . C30 C 0.5413(6) 0.7841(4) 0.6681(5) 0.0312(17) Uani 1 1 d . . . H30 H 0.5023 0.7933 0.7180 0.037 Uiso 1 1 calc R . . C31 C 0.5220(6) 0.7235(5) 0.6154(6) 0.0363(18) Uani 1 1 d . . . H31 H 0.4708 0.6912 0.6298 0.044 Uiso 1 1 calc R . . C32 C 0.5787(6) 0.7093(5) 0.5392(6) 0.0355(18) Uani 1 1 d . . . H32 H 0.5644 0.6682 0.5020 0.043 Uiso 1 1 calc R . . C33 C 0.6575(5) 0.7577(4) 0.5193(5) 0.0294(16) Uani 1 1 d . . . H33 H 0.6965 0.7482 0.4695 0.035 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 W1 0.01736(17) 0.0242(2) 0.01924(17) 0.00148(13) 0.00560(11) 0.00058(13) P1 0.0190(8) 0.0241(9) 0.0219(7) 0.0019(7) 0.0068(6) 0.0019(7) P2 0.0194(8) 0.0285(9) 0.0212(7) 0.0026(7) 0.0060(6) 0.0007(7) Si1 0.0236(9) 0.0276(10) 0.0202(8) -0.0002(7) 0.0058(7) 0.0001(7) Si2 0.0218(8) 0.0273(10) 0.0212(8) 0.0017(8) 0.0046(7) -0.0011(8) N1 0.021(3) 0.025(3) 0.020(2) -0.004(2) 0.005(2) -0.002(2) C1 0.011(3) 0.035(4) 0.030(4) 0.001(3) 0.004(3) 0.000(3) O1 0.025(2) 0.046(3) 0.023(2) -0.007(2) 0.004(2) 0.004(2) C2 0.022(3) 0.017(3) 0.024(3) 0.004(3) 0.005(3) -0.007(3) O2 0.043(3) 0.034(3) 0.038(3) 0.005(2) 0.007(2) -0.006(3) C3 0.028(3) 0.019(4) 0.023(3) 0.008(3) 0.012(3) 0.001(3) O3 0.037(3) 0.036(3) 0.035(3) 0.005(3) 0.011(2) 0.003(2) C4 0.020(3) 0.028(4) 0.027(3) -0.001(3) 0.005(3) 0.003(3) C5 0.020(3) 0.034(4) 0.023(3) -0.003(3) 0.006(3) 0.002(3) C6 0.033(4) 0.029(4) 0.024(3) -0.001(3) 0.011(3) 0.005(3) C7 0.037(4) 0.034(4) 0.029(3) -0.005(3) 0.018(3) -0.003(3) C8 0.023(4) 0.034(4) 0.035(4) -0.002(3) 0.012(3) -0.005(3) C9 0.024(3) 0.034(4) 0.030(3) 0.001(3) 0.011(3) 0.002(3) C10 0.021(3) 0.035(4) 0.024(3) 0.000(3) 0.010(3) 0.000(3) C11 0.040(4) 0.034(5) 0.038(4) -0.002(3) -0.001(4) 0.012(3) C12 0.044(5) 0.048(6) 0.041(4) -0.005(4) -0.005(4) 0.005(4) C13 0.046(5) 0.028(4) 0.059(5) 0.008(4) 0.025(4) 0.014(4) C14 0.036(4) 0.042(5) 0.050(5) 0.007(4) 0.006(4) 0.004(4) C15 0.032(4) 0.035(5) 0.043(4) 0.001(4) -0.002(4) 0.002(3) C16 0.021(3) 0.040(4) 0.025(3) -0.004(3) 0.004(3) -0.003(3) C17 0.028(4) 0.033(4) 0.031(3) -0.003(3) 0.004(3) -0.004(3) C18 0.023(3) 0.032(4) 0.024(3) 0.003(3) 0.001(3) 0.002(3) C19 0.028(4) 0.045(5) 0.029(3) 0.005(3) 0.011(3) 0.000(3) C20 0.037(4) 0.035(4) 0.021(3) -0.009(3) 0.001(3) 0.000(3) C21 0.023(3) 0.030(4) 0.022(3) 0.002(3) 0.006(3) 0.004(3) C22 0.021(3) 0.027(4) 0.025(3) -0.001(3) 0.001(3) -0.005(3) C23 0.028(4) 0.033(4) 0.024(3) 0.006(3) 0.000(3) -0.003(3) C24 0.033(4) 0.039(5) 0.033(4) 0.003(3) 0.004(3) -0.004(3) C25 0.028(4) 0.036(4) 0.035(4) 0.008(3) -0.006(3) -0.002(3) C26 0.024(4) 0.031(4) 0.050(5) 0.002(4) 0.007(3) 0.006(3) C27 0.024(3) 0.035(4) 0.032(3) 0.005(3) 0.009(3) 0.004(3) C28 0.022(3) 0.026(4) 0.025(3) 0.003(3) 0.003(3) 0.003(3) C29 0.022(3) 0.032(4) 0.028(3) 0.005(3) 0.009(3) 0.007(3) C30 0.025(4) 0.038(5) 0.034(4) 0.005(3) 0.016(3) 0.000(3) C31 0.024(4) 0.044(5) 0.042(4) 0.013(4) 0.008(3) -0.001(3) C32 0.037(4) 0.035(5) 0.034(4) -0.004(3) 0.002(3) -0.005(3) C33 0.017(3) 0.041(5) 0.031(3) 0.005(3) 0.003(3) -0.005(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 W1 C1 1.947(7) . ? W1 C3 2.009(6) . ? W1 C2 2.043(6) . ? W1 N1 2.443(5) . ? W1 P1 2.4606(16) . ? W1 P2 2.4731(17) . ? P1 C21 1.841(7) . ? P1 C22 1.854(7) . ? P1 C28 1.858(7) . ? P2 C16 1.835(7) . ? P2 C4 1.840(7) . ? P2 C10 1.847(8) . ? Si1 N1 1.795(5) . ? Si1 C19 1.862(8) . ? Si1 C20 1.875(7) . ? Si1 C21 1.881(7) . ? Si2 N1 1.789(6) . ? Si2 C18 1.856(8) . ? Si2 C17 1.865(8) . ? Si2 C16 1.871(7) . ? C1 O1 1.167(9) . ? C2 O2 1.147(9) . ? C3 O3 1.146(8) . ? C4 C5 1.394(10) . ? C4 C9 1.409(10) . ? C5 C6 1.402(10) . ? C5 H5 0.9300 . ? C6 C7 1.390(11) . ? C6 H6 0.9300 . ? C7 C8 1.386(11) . ? C7 H7 0.9300 . ? C8 C9 1.393(10) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.393(11) . ? C10 C11 1.408(12) . ? C11 C12 1.380(13) . ? C11 H11 0.9300 . ? C12 C13 1.406(13) . ? C12 H12 0.9300 . ? C13 C14 1.388(14) . ? C13 H13 0.9300 . ? C14 C15 1.385(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.391(10) . ? C22 C23 1.391(10) . ? C23 C24 1.398(11) . ? C23 H23 0.9300 . ? C24 C25 1.372(12) . ? C24 H24 0.9300 . ? C25 C26 1.378(12) . ? C25 H25 0.9300 . ? C26 C27 1.399(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.385(11) . ? C28 C29 1.395(10) . ? C29 C30 1.396(11) . ? C29 H29 0.9300 . ? C30 C31 1.351(12) . ? C30 H30 0.9300 . ? C31 C32 1.398(11) . ? C31 H31 0.9300 . ? C32 C33 1.405(11) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? 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 W1 C3 83.8(3) . . ? C1 W1 C2 82.5(3) . . ? C3 W1 C2 166.1(3) . . ? C1 W1 N1 179.2(3) . . ? C3 W1 N1 95.5(2) . . ? C2 W1 N1 98.2(2) . . ? C1 W1 P1 96.69(19) . . ? C3 W1 P1 85.98(19) . . ? C2 W1 P1 93.22(19) . . ? N1 W1 P1 83.28(13) . . ? C1 W1 P2 96.45(19) . . ? C3 W1 P2 92.1(2) . . ? C2 W1 P2 91.85(19) . . ? N1 W1 P2 83.53(13) . . ? P1 W1 P2 166.42(6) . . ? C21 P1 C22 103.3(3) . . ? C21 P1 C28 104.7(3) . . ? C22 P1 C28 100.1(3) . . ? C21 P1 W1 108.5(2) . . ? C22 P1 W1 119.3(2) . . ? C28 P1 W1 119.0(2) . . ? C16 P2 C4 101.8(3) . . ? C16 P2 C10 106.1(4) . . ? C4 P2 C10 100.4(3) . . ? C16 P2 W1 108.1(2) . . ? C4 P2 W1 121.4(2) . . ? C10 P2 W1 117.1(2) . . ? N1 Si1 C19 111.7(3) . . ? N1 Si1 C20 111.7(3) . . ? C19 Si1 C20 109.2(4) . . ? N1 Si1 C21 103.4(3) . . ? C19 Si1 C21 112.5(3) . . ? C20 Si1 C21 108.3(3) . . ? N1 Si2 C18 111.3(3) . . ? N1 Si2 C17 111.1(3) . . ? C18 Si2 C17 110.9(3) . . ? N1 Si2 C16 102.6(3) . . ? C18 Si2 C16 112.3(3) . . ? C17 Si2 C16 108.4(3) . . ? Si2 N1 Si1 122.3(3) . . ? Si2 N1 W1 110.3(3) . . ? Si1 N1 W1 113.7(3) . . ? O1 C1 W1 178.8(7) . . ? O2 C2 W1 172.2(6) . . ? O3 C3 W1 169.4(6) . . ? C5 C4 C9 118.2(6) . . ? C5 C4 P2 121.3(5) . . ? C9 C4 P2 120.5(5) . . ? C4 C5 C6 120.9(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 120.1(7) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 119.5(7) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.6(7) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 120.6(7) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C15 C10 C11 118.7(7) . . ? C15 C10 P2 124.0(6) . . ? C11 C10 P2 117.4(6) . . ? C12 C11 C10 120.8(8) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.3(9) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 118.4(8) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 121.6(8) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C10 120.1(8) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? P2 C16 Si2 110.1(4) . . ? P2 C16 H16A 109.6 . . ? Si2 C16 H16A 109.6 . . ? P2 C16 H16B 109.6 . . ? Si2 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P1 C21 Si1 109.2(4) . . ? P1 C21 H21A 109.8 . . ? Si1 C21 H21A 109.8 . . ? P1 C21 H21B 109.8 . . ? Si1 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? C27 C22 C23 119.4(7) . . ? C27 C22 P1 120.1(5) . . ? C23 C22 P1 120.4(6) . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.8(7) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.5(7) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 120.8(7) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 119.7(7) . . ? C22 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C33 C28 C29 119.7(7) . . ? C33 C28 P1 117.1(5) . . ? C29 C28 P1 123.2(6) . . ? C28 C29 C30 119.5(7) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C31 C30 C29 121.2(7) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 120.2(7) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 119.4(8) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 119.9(7) . . ? C28 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 W1 P1 C21 -165.2(3) . . . . ? C3 W1 P1 C21 -81.9(3) . . . . ? C2 W1 P1 C21 112.0(3) . . . . ? N1 W1 P1 C21 14.1(3) . . . . ? P2 W1 P1 C21 0.2(4) . . . . ? C1 W1 P1 C22 -47.5(3) . . . . ? C3 W1 P1 C22 35.8(3) . . . . ? C2 W1 P1 C22 -130.3(3) . . . . ? N1 W1 P1 C22 131.8(3) . . . . ? P2 W1 P1 C22 117.9(3) . . . . ? C1 W1 P1 C28 75.4(3) . . . . ? C3 W1 P1 C28 158.6(3) . . . . ? C2 W1 P1 C28 -7.5(3) . . . . ? N1 W1 P1 C28 -105.4(3) . . . . ? P2 W1 P1 C28 -119.2(3) . . . . ? C1 W1 P2 C16 175.2(4) . . . . ? C3 W1 P2 C16 91.2(3) . . . . ? C2 W1 P2 C16 -102.1(3) . . . . ? N1 W1 P2 C16 -4.1(3) . . . . ? P1 W1 P2 C16 9.8(4) . . . . ? C1 W1 P2 C4 58.3(4) . . . . ? C3 W1 P2 C4 -25.6(3) . . . . ? C2 W1 P2 C4 141.0(3) . . . . ? N1 W1 P2 C4 -120.9(3) . . . . ? P1 W1 P2 C4 -107.1(4) . . . . ? C1 W1 P2 C10 -65.1(3) . . . . ? C3 W1 P2 C10 -149.0(3) . . . . ? C2 W1 P2 C10 17.6(3) . . . . ? N1 W1 P2 C10 115.7(3) . . . . ? P1 W1 P2 C10 129.5(3) . . . . ? C18 Si2 N1 Si1 66.1(5) . . . . ? C17 Si2 N1 Si1 -58.0(5) . . . . ? C16 Si2 N1 Si1 -173.7(4) . . . . ? C18 Si2 N1 W1 -71.7(3) . . . . ? C17 Si2 N1 W1 164.2(3) . . . . ? C16 Si2 N1 W1 48.5(3) . . . . ? C19 Si1 N1 Si2 -54.3(5) . . . . ? C20 Si1 N1 Si2 68.3(5) . . . . ? C21 Si1 N1 Si2 -175.5(4) . . . . ? C19 Si1 N1 W1 82.2(4) . . . . ? C20 Si1 N1 W1 -155.2(3) . . . . ? C21 Si1 N1 W1 -39.0(4) . . . . ? C3 W1 N1 Si2 -117.9(3) . . . . ? C2 W1 N1 Si2 64.5(3) . . . . ? P1 W1 N1 Si2 156.8(3) . . . . ? P2 W1 N1 Si2 -26.4(2) . . . . ? C3 W1 N1 Si1 100.5(3) . . . . ? C2 W1 N1 Si1 -77.1(3) . . . . ? P1 W1 N1 Si1 15.2(3) . . . . ? P2 W1 N1 Si1 -168.0(3) . . . . ? C1 W1 C3 O3 15(3) . . . . ? C2 W1 C3 O3 5(4) . . . . ? N1 W1 C3 O3 -165(3) . . . . ? P1 W1 C3 O3 -82(3) . . . . ? P2 W1 C3 O3 111(3) . . . . ? C16 P2 C4 C5 -147.1(6) . . . . ? C10 P2 C4 C5 103.9(6) . . . . ? W1 P2 C4 C5 -27.1(7) . . . . ? C16 P2 C4 C9 32.7(7) . . . . ? C10 P2 C4 C9 -76.4(7) . . . . ? W1 P2 C4 C9 152.7(5) . . . . ? C9 C4 C5 C6 -0.7(11) . . . . ? P2 C4 C5 C6 179.1(6) . . . . ? C4 C5 C6 C7 -0.6(11) . . . . ? C5 C6 C7 C8 1.0(11) . . . . ? C6 C7 C8 C9 -0.1(12) . . . . ? C7 C8 C9 C4 -1.2(12) . . . . ? C5 C4 C9 C8 1.6(11) . . . . ? P2 C4 C9 C8 -178.2(6) . . . . ? C16 P2 C10 C15 -10.2(7) . . . . ? C4 P2 C10 C15 95.4(7) . . . . ? W1 P2 C10 C15 -131.1(6) . . . . ? C16 P2 C10 C11 170.2(6) . . . . ? C4 P2 C10 C11 -84.2(6) . . . . ? W1 P2 C10 C11 49.3(6) . . . . ? C15 C10 C11 C12 -1.9(12) . . . . ? P2 C10 C11 C12 177.7(7) . . . . ? C10 C11 C12 C13 0.8(14) . . . . ? C11 C12 C13 C14 0.1(13) . . . . ? C12 C13 C14 C15 0.2(13) . . . . ? C13 C14 C15 C10 -1.3(13) . . . . ? C11 C10 C15 C14 2.1(12) . . . . ? P2 C10 C15 C14 -177.5(6) . . . . ? C4 P2 C16 Si2 161.6(4) . . . . ? C10 P2 C16 Si2 -93.8(4) . . . . ? W1 P2 C16 Si2 32.7(4) . . . . ? N1 Si2 C16 P2 -52.7(5) . . . . ? C18 Si2 C16 P2 66.8(5) . . . . ? C17 Si2 C16 P2 -170.3(4) . . . . ? C22 P1 C21 Si1 -167.3(3) . . . . ? C28 P1 C21 Si1 88.2(4) . . . . ? W1 P1 C21 Si1 -39.8(4) . . . . ? N1 Si1 C21 P1 50.4(4) . . . . ? C19 Si1 C21 P1 -70.3(4) . . . . ? C20 Si1 C21 P1 169.0(4) . . . . ? C21 P1 C22 C27 -31.8(7) . . . . ? C28 P1 C22 C27 76.1(6) . . . . ? W1 P1 C22 C27 -152.2(5) . . . . ? C21 P1 C22 C23 150.8(6) . . . . ? C28 P1 C22 C23 -101.3(6) . . . . ? W1 P1 C22 C23 30.5(7) . . . . ? C27 C22 C23 C24 -0.6(11) . . . . ? P1 C22 C23 C24 176.8(6) . . . . ? C22 C23 C24 C25 0.9(12) . . . . ? C23 C24 C25 C26 -0.4(12) . . . . ? C24 C25 C26 C27 -0.4(12) . . . . ? C23 C22 C27 C26 -0.2(11) . . . . ? P1 C22 C27 C26 -177.5(6) . . . . ? C25 C26 C27 C22 0.7(12) . . . . ? C21 P1 C28 C33 -167.1(6) . . . . ? C22 P1 C28 C33 86.1(6) . . . . ? W1 P1 C28 C33 -45.8(6) . . . . ? C21 P1 C28 C29 12.4(7) . . . . ? C22 P1 C28 C29 -94.3(6) . . . . ? W1 P1 C28 C29 133.8(5) . . . . ? C33 C28 C29 C30 -0.1(11) . . . . ? P1 C28 C29 C30 -179.6(6) . . . . ? C28 C29 C30 C31 0.3(12) . . . . ? C29 C30 C31 C32 -1.0(12) . . . . ? C30 C31 C32 C33 1.4(12) . . . . ? C29 C28 C33 C32 0.6(11) . . . . ? P1 C28 C33 C32 -179.9(6) . . . . ? C31 C32 C33 C28 -1.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.382 _refine_diff_density_min -1.630 _refine_diff_density_rms 0.182 # Attachment '- c08393.cif' data_c08393 _database_code_depnum_ccdc_archive 'CCDC 877930' #TrackingRef '- c08393.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H37 N O4 P2 Si2 W, 0.5(C6 H6)' _chemical_formula_sum 'C37 H40 N O4 P2 Si2 W' _chemical_formula_weight 864.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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/n' _symmetry_space_group_name_Hall '-P 2yn' 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 8.9073(3) _cell_length_b 24.0432(10) _cell_length_c 17.5465(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.894(3) _cell_angle_gamma 90.00 _cell_volume 3744.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6149 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.35 _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 3.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4401 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details SADABS _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 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25129 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.71 _reflns_number_total 7072 _reflns_number_gt 5238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0277P)^2^+5.8095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7072 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.11928(2) 0.846966(9) 0.820254(12) 0.01561(7) Uani 1 1 d . . . P1 P 0.04288(13) 0.90670(6) 0.74098(8) 0.0168(3) Uani 1 1 d . . . P2 P 0.06904(13) 0.79712(6) 0.91366(8) 0.0169(3) Uani 1 1 d . . . Si1 Si 0.28341(15) 0.97407(7) 0.85447(9) 0.0207(4) Uani 1 1 d . . . Si2 Si 0.30764(15) 0.88750(7) 0.99011(9) 0.0207(4) Uani 1 1 d . . . C1 C -0.1311(5) 0.9095(2) 0.8967(3) 0.0199(13) Uani 1 1 d . . . O2 O -0.1346(4) 0.94508(17) 0.9411(2) 0.0260(9) Uani 1 1 d . . . C3 C -0.2791(6) 0.8005(2) 0.8596(3) 0.0224(13) Uani 1 1 d . . . O4 O -0.3829(4) 0.77483(18) 0.8755(2) 0.0328(11) Uani 1 1 d . . . C5 C -0.0807(5) 0.7845(2) 0.7458(3) 0.0210(13) Uani 1 1 d . . . O6 O -0.0592(4) 0.74885(17) 0.7050(2) 0.0305(10) Uani 1 1 d . . . C7 C -0.2922(6) 0.8758(2) 0.7541(3) 0.0212(13) Uani 1 1 d . . . O8 O -0.4019(4) 0.88977(16) 0.7175(2) 0.0279(10) Uani 1 1 d . . . C9 C 0.2380(5) 0.9251(2) 0.7717(3) 0.0208(13) Uani 1 1 d . . . H9A H 0.2823 0.9412 0.7268 0.025 Uiso 1 1 calc R . . H9B H 0.2925 0.8899 0.7841 0.025 Uiso 1 1 calc R . . N10 N 0.2420(4) 0.94473(18) 0.9392(3) 0.0206(11) Uani 1 1 d . . . H10 H 0.1719 0.9629 0.9614 0.025 Uiso 1 1 calc R . . C11 C 0.2628(5) 0.8215(2) 0.9345(3) 0.0180(12) Uani 1 1 d . . . H11A H 0.3065 0.8256 0.8848 0.022 Uiso 1 1 calc R . . H11B H 0.3189 0.7911 0.9623 0.022 Uiso 1 1 calc R . . C12 C 0.1812(6) 1.0414(2) 0.8454(3) 0.0296(15) Uani 1 1 d . . . H12A H 0.0758 1.0358 0.8556 0.044 Uiso 1 1 calc R . . H12B H 0.1855 1.0560 0.7934 0.044 Uiso 1 1 calc R . . H12C H 0.2285 1.0681 0.8823 0.044 Uiso 1 1 calc R . . C13 C 0.4910(6) 0.9859(3) 0.8516(4) 0.0315(15) Uani 1 1 d . . . H13A H 0.5306 1.0049 0.8986 0.047 Uiso 1 1 calc R . . H13B H 0.5088 1.0090 0.8073 0.047 Uiso 1 1 calc R . . H13C H 0.5421 0.9501 0.8476 0.047 Uiso 1 1 calc R . . C14 C 0.5185(5) 0.8861(3) 1.0020(4) 0.0322(16) Uani 1 1 d . . . H14A H 0.5578 0.8819 0.9518 0.048 Uiso 1 1 calc R . . H14B H 0.5522 0.8547 1.0348 0.048 Uiso 1 1 calc R . . H14C H 0.5560 0.9209 1.0256 0.048 Uiso 1 1 calc R . . C15 C 0.2310(6) 0.8893(3) 1.0839(3) 0.0327(15) Uani 1 1 d . . . H15A H 0.2659 0.9231 1.1114 0.049 Uiso 1 1 calc R . . H15B H 0.2656 0.8565 1.1136 0.049 Uiso 1 1 calc R . . H15C H 0.1207 0.8894 1.0770 0.049 Uiso 1 1 calc R . . C16 C 0.0547(6) 0.8742(2) 0.6474(3) 0.0205(12) Uani 1 1 d . . . C17 C -0.0760(6) 0.8724(2) 0.5964(3) 0.0244(13) Uani 1 1 d . . . H17 H -0.1661 0.8891 0.6108 0.029 Uiso 1 1 calc R . . C18 C -0.0759(6) 0.8472(3) 0.5265(3) 0.0265(13) Uani 1 1 d . . . H18 H -0.1648 0.8469 0.4925 0.032 Uiso 1 1 calc R . . C19 C 0.0546(7) 0.8221(3) 0.5054(3) 0.0327(15) Uani 1 1 d . . . H19 H 0.0549 0.8039 0.4573 0.039 Uiso 1 1 calc R . . C20 C 0.1848(7) 0.8238(3) 0.5550(3) 0.0319(15) Uani 1 1 d . . . H20 H 0.2746 0.8072 0.5402 0.038 Uiso 1 1 calc R . . C21 C 0.1853(6) 0.8493(2) 0.6253(3) 0.0258(13) Uani 1 1 d . . . H21 H 0.2750 0.8500 0.6587 0.031 Uiso 1 1 calc R . . C22 C -0.0320(5) 0.9750(2) 0.7100(3) 0.0170(12) Uani 1 1 d . . . C23 C 0.0324(6) 1.0020(2) 0.6505(3) 0.0235(13) Uani 1 1 d . . . H23 H 0.1097 0.9839 0.6258 0.028 Uiso 1 1 calc R . . C24 C -0.0136(6) 1.0545(3) 0.6268(3) 0.0262(14) Uani 1 1 d . . . H24 H 0.0313 1.0723 0.5861 0.031 Uiso 1 1 calc R . . C25 C -0.1261(6) 1.0809(2) 0.6631(3) 0.0232(13) Uani 1 1 d . . . H25 H -0.1563 1.1175 0.6483 0.028 Uiso 1 1 calc R . . C26 C -0.1938(6) 1.0544(2) 0.7202(3) 0.0242(14) Uani 1 1 d . . . H26 H -0.2731 1.0723 0.7436 0.029 Uiso 1 1 calc R . . C27 C -0.1474(5) 1.0018(2) 0.7439(3) 0.0194(12) Uani 1 1 d . . . H27 H -0.1948 0.9839 0.7837 0.023 Uiso 1 1 calc R . . C28 C 0.0131(5) 0.7856(2) 1.0102(3) 0.0166(12) Uani 1 1 d . . . C29 C -0.1127(5) 0.8115(2) 1.0379(3) 0.0215(13) Uani 1 1 d . . . H29 H -0.1758 0.8344 1.0047 0.026 Uiso 1 1 calc R . . C30 C -0.1457(6) 0.8043(2) 1.1126(3) 0.0249(14) Uani 1 1 d . . . H30 H -0.2301 0.8229 1.1305 0.030 Uiso 1 1 calc R . . C31 C -0.0587(6) 0.7706(2) 1.1615(3) 0.0226(13) Uani 1 1 d . . . H31 H -0.0828 0.7657 1.2128 0.027 Uiso 1 1 calc R . . C32 C 0.0653(6) 0.7438(2) 1.1353(3) 0.0254(14) Uani 1 1 d . . . H32 H 0.1265 0.7204 1.1688 0.030 Uiso 1 1 calc R . . C33 C 0.0996(5) 0.7510(2) 1.0609(3) 0.0206(13) Uani 1 1 d . . . H33 H 0.1838 0.7320 1.0435 0.025 Uiso 1 1 calc R . . C34 C 0.0990(5) 0.7253(2) 0.8832(3) 0.0164(12) Uani 1 1 d . . . C35 C -0.0030(6) 0.6836(3) 0.8985(3) 0.0266(14) Uani 1 1 d . . . H35 H -0.0883 0.6924 0.9252 0.032 Uiso 1 1 calc R . . C36 C 0.0193(6) 0.6292(3) 0.8747(3) 0.0284(14) Uani 1 1 d . . . H36 H -0.0494 0.6008 0.8865 0.034 Uiso 1 1 calc R . . C37 C 0.1401(6) 0.6163(2) 0.8343(3) 0.0263(14) Uani 1 1 d . . . H37 H 0.1543 0.5792 0.8179 0.032 Uiso 1 1 calc R . . C38 C 0.2405(6) 0.6571(2) 0.8177(3) 0.0246(13) Uani 1 1 d . . . H38 H 0.3241 0.6479 0.7899 0.030 Uiso 1 1 calc R . . C39 C 0.2206(5) 0.7114(2) 0.8413(3) 0.0202(13) Uani 1 1 d . . . H39 H 0.2898 0.7394 0.8290 0.024 Uiso 1 1 calc R . . C40 C 0.6210(7) 0.9871(3) 0.5513(4) 0.0420(18) Uani 1 1 d . . . H40 H 0.7041 0.9782 0.5867 0.050 Uiso 1 1 calc R . . C41 C 0.4834(8) 0.9623(3) 0.5573(4) 0.0469(19) Uani 1 1 d . . . H41 H 0.4719 0.9361 0.5969 0.056 Uiso 1 1 calc R . . C42 C 0.3621(7) 0.9752(3) 0.5063(4) 0.0410(18) Uani 1 1 d . . . H42 H 0.2672 0.9581 0.5109 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01364(10) 0.01464(12) 0.01838(12) 0.00053(11) 0.00039(7) -0.00031(10) P1 0.0155(6) 0.0148(8) 0.0200(8) 0.0000(6) 0.0009(5) 0.0000(5) P2 0.0145(6) 0.0157(8) 0.0204(8) -0.0004(6) 0.0003(5) 0.0005(5) Si1 0.0163(7) 0.0188(9) 0.0268(9) -0.0018(7) 0.0005(6) -0.0023(6) Si2 0.0168(7) 0.0233(10) 0.0215(9) -0.0026(7) -0.0008(6) -0.0019(6) C1 0.012(2) 0.023(4) 0.025(3) 0.008(3) 0.004(2) 0.002(2) O2 0.0247(19) 0.025(3) 0.028(2) -0.007(2) 0.0038(17) 0.0031(17) C3 0.031(3) 0.019(3) 0.016(3) -0.002(3) -0.003(2) 0.013(3) O4 0.0212(19) 0.037(3) 0.041(3) 0.005(2) 0.0069(18) -0.0140(19) C5 0.021(3) 0.019(3) 0.022(3) -0.002(3) -0.004(2) -0.001(2) O6 0.037(2) 0.021(3) 0.033(3) -0.005(2) -0.0018(19) 0.0018(19) C7 0.031(3) 0.017(3) 0.017(3) -0.005(3) 0.012(2) -0.004(2) O8 0.0189(18) 0.028(3) 0.035(2) -0.0063(19) -0.0101(17) 0.0053(16) C9 0.016(2) 0.021(3) 0.025(3) 0.003(3) 0.001(2) 0.003(2) N10 0.019(2) 0.018(3) 0.025(3) -0.006(2) 0.0040(19) 0.0030(19) C11 0.018(2) 0.015(3) 0.021(3) 0.000(2) 0.000(2) -0.001(2) C12 0.036(3) 0.017(3) 0.034(4) -0.009(3) -0.005(3) 0.001(3) C13 0.026(3) 0.030(4) 0.038(4) -0.003(3) 0.002(3) -0.008(3) C14 0.019(3) 0.040(4) 0.037(4) 0.000(3) -0.006(3) -0.001(3) C15 0.034(3) 0.034(4) 0.030(4) -0.012(3) 0.002(3) -0.004(3) C16 0.029(3) 0.011(3) 0.022(3) 0.001(2) 0.006(2) -0.003(2) C17 0.024(3) 0.023(3) 0.026(3) 0.007(3) 0.003(2) -0.004(2) C18 0.042(3) 0.020(3) 0.017(3) 0.000(3) 0.000(2) -0.007(3) C19 0.065(4) 0.015(3) 0.019(3) -0.002(3) 0.012(3) -0.005(3) C20 0.045(3) 0.027(4) 0.026(4) 0.006(3) 0.011(3) 0.006(3) C21 0.034(3) 0.017(3) 0.027(3) -0.001(3) 0.005(2) 0.002(3) C22 0.018(2) 0.012(3) 0.021(3) 0.001(2) 0.003(2) -0.003(2) C23 0.020(3) 0.021(3) 0.029(3) -0.001(3) 0.000(2) -0.001(2) C24 0.027(3) 0.032(4) 0.020(3) 0.005(3) 0.003(2) -0.006(3) C25 0.026(3) 0.013(3) 0.029(3) 0.003(3) -0.007(2) -0.001(2) C26 0.023(3) 0.025(4) 0.024(3) 0.000(3) 0.000(2) 0.004(2) C27 0.022(3) 0.016(3) 0.020(3) 0.001(2) 0.002(2) 0.002(2) C28 0.020(2) 0.011(3) 0.019(3) -0.001(2) 0.002(2) -0.002(2) C29 0.020(3) 0.013(3) 0.030(3) 0.007(3) 0.000(2) 0.002(2) C30 0.023(3) 0.026(4) 0.025(3) -0.002(3) 0.004(2) 0.005(2) C31 0.027(3) 0.023(3) 0.018(3) 0.002(3) 0.005(2) -0.004(2) C32 0.028(3) 0.025(4) 0.023(3) 0.011(3) -0.003(2) -0.001(3) C33 0.018(3) 0.014(3) 0.030(3) 0.001(3) 0.002(2) 0.000(2) C34 0.021(2) 0.015(3) 0.013(3) 0.002(2) 0.002(2) 0.005(2) C35 0.020(3) 0.026(4) 0.034(4) 0.000(3) 0.000(2) 0.002(2) C36 0.027(3) 0.025(4) 0.033(4) -0.009(3) 0.001(3) -0.002(3) C37 0.033(3) 0.015(3) 0.029(4) -0.004(3) -0.002(3) 0.005(3) C38 0.025(3) 0.020(3) 0.030(3) -0.001(3) 0.006(2) 0.005(3) C39 0.022(3) 0.017(3) 0.022(3) 0.002(3) 0.002(2) -0.003(2) C40 0.043(4) 0.036(5) 0.043(4) -0.007(4) -0.017(3) 0.010(3) C41 0.078(5) 0.026(4) 0.035(4) 0.011(3) -0.011(4) -0.011(4) C42 0.036(3) 0.047(5) 0.039(4) -0.015(4) 0.002(3) -0.001(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 W1 C7 1.973(5) . ? W1 C3 1.980(6) . ? W1 C1 2.024(6) . ? W1 C5 2.039(6) . ? W1 P1 2.5351(14) . ? W1 P2 2.5431(13) . ? P1 C9 1.829(5) . ? P1 C16 1.830(6) . ? P1 C22 1.838(5) . ? P2 C28 1.828(6) . ? P2 C11 1.830(5) . ? P2 C34 1.833(6) . ? Si1 N10 1.715(5) . ? Si1 C12 1.858(6) . ? Si1 C13 1.876(5) . ? Si1 C9 1.887(6) . ? Si2 N10 1.716(5) . ? Si2 C15 1.836(6) . ? Si2 C14 1.873(5) . ? Si2 C11 1.887(5) . ? C1 O2 1.159(6) . ? C3 O4 1.165(6) . ? C5 O6 1.143(6) . ? C7 O8 1.173(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? N10 H10 0.8800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? 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 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.392(8) . ? C16 C17 1.407(7) . ? C17 C18 1.369(8) . ? C17 H17 0.9500 . ? C18 C19 1.387(8) . ? C18 H18 0.9500 . ? C19 C20 1.390(8) . ? C19 H19 0.9500 . ? C20 C21 1.377(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.389(7) . ? C22 C23 1.393(7) . ? C23 C24 1.380(8) . ? C23 H23 0.9500 . ? C24 C25 1.386(8) . ? C24 H24 0.9500 . ? C25 C26 1.369(8) . ? C25 H25 0.9500 . ? C26 C27 1.384(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.400(7) . ? C28 C29 1.404(7) . ? C29 C30 1.379(8) . ? C29 H29 0.9500 . ? C30 C31 1.371(7) . ? C30 H30 0.9500 . ? C31 C32 1.391(8) . ? C31 H31 0.9500 . ? C32 C33 1.378(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.395(8) . ? C34 C39 1.400(7) . ? C35 C36 1.393(8) . ? C35 H35 0.9500 . ? C36 C37 1.373(8) . ? C36 H36 0.9500 . ? C37 C38 1.374(8) . ? C37 H37 0.9500 . ? C38 C39 1.387(8) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.375(9) . ? C40 C42 1.375(9) 3_676 ? C40 H40 0.9500 . ? C41 C42 1.378(8) . ? C41 H41 0.9500 . ? C42 C40 1.375(9) 3_676 ? C42 H42 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 C7 W1 C3 81.7(2) . . ? C7 W1 C1 92.7(2) . . ? C3 W1 C1 96.2(2) . . ? C7 W1 C5 92.7(2) . . ? C3 W1 C5 88.5(2) . . ? C1 W1 C5 173.31(19) . . ? C7 W1 P1 86.04(16) . . ? C3 W1 P1 166.26(15) . . ? C1 W1 P1 90.43(16) . . ? C5 W1 P1 86.03(16) . . ? C7 W1 P2 169.52(16) . . ? C3 W1 P2 87.92(14) . . ? C1 W1 P2 89.52(14) . . ? C5 W1 P2 85.86(14) . . ? P1 W1 P2 104.20(4) . . ? C9 P1 C16 104.0(2) . . ? C9 P1 C22 100.5(2) . . ? C16 P1 C22 99.4(2) . . ? C9 P1 W1 123.15(19) . . ? C16 P1 W1 109.23(18) . . ? C22 P1 W1 117.34(17) . . ? C28 P2 C11 101.0(2) . . ? C28 P2 C34 100.7(2) . . ? C11 P2 C34 101.6(2) . . ? C28 P2 W1 116.85(16) . . ? C11 P2 W1 122.47(18) . . ? C34 P2 W1 111.13(16) . . ? N10 Si1 C12 107.0(3) . . ? N10 Si1 C13 111.8(2) . . ? C12 Si1 C13 110.0(3) . . ? N10 Si1 C9 111.3(2) . . ? C12 Si1 C9 114.0(2) . . ? C13 Si1 C9 102.8(3) . . ? N10 Si2 C15 108.1(3) . . ? N10 Si2 C14 111.5(3) . . ? C15 Si2 C14 110.3(3) . . ? N10 Si2 C11 111.0(2) . . ? C15 Si2 C11 113.9(3) . . ? C14 Si2 C11 102.0(3) . . ? O2 C1 W1 178.5(4) . . ? O4 C3 W1 172.4(4) . . ? O6 C5 W1 178.9(5) . . ? O8 C7 W1 174.6(5) . . ? P1 C9 Si1 120.9(3) . . ? P1 C9 H9A 107.1 . . ? Si1 C9 H9A 107.1 . . ? P1 C9 H9B 107.1 . . ? Si1 C9 H9B 107.1 . . ? H9A C9 H9B 106.8 . . ? Si1 N10 Si2 133.8(3) . . ? Si1 N10 H10 113.1 . . ? Si2 N10 H10 113.1 . . ? P2 C11 Si2 121.8(3) . . ? P2 C11 H11A 106.9 . . ? Si2 C11 H11A 106.9 . . ? P2 C11 H11B 106.9 . . ? Si2 C11 H11B 106.9 . . ? H11A C11 H11B 106.7 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.4(5) . . ? C21 C16 P1 123.2(4) . . ? C17 C16 P1 118.4(4) . . ? C18 C17 C16 121.3(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.8(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 119.5(6) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C16 120.2(5) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C27 C22 C23 118.2(5) . . ? C27 C22 P1 123.4(4) . . ? C23 C22 P1 118.4(4) . . ? C24 C23 C22 121.3(5) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.3(6) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.2(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.4(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 120.5(5) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C33 C28 C29 117.1(5) . . ? C33 C28 P2 120.0(4) . . ? C29 C28 P2 122.9(4) . . ? C30 C29 C28 121.0(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 120.9(5) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.4(5) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 121.5(5) . . ? C32 C33 H33 119.2 . . ? C28 C33 H33 119.2 . . ? C35 C34 C39 118.3(5) . . ? C35 C34 P2 120.5(4) . . ? C39 C34 P2 121.1(4) . . ? C36 C35 C34 120.4(5) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.3(6) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.1(6) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C39 120.4(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.4(5) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? C41 C40 C42 119.8(6) . 3_676 ? C41 C40 H40 120.1 . . ? C42 C40 H40 120.1 3_676 . ? C40 C41 C42 120.4(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C40 C42 C41 119.8(6) 3_676 . ? C40 C42 H42 120.1 3_676 . ? C41 C42 H42 120.1 . . ? 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 C7 W1 P1 C9 163.3(3) . . . . ? C3 W1 P1 C9 -170.2(7) . . . . ? C1 W1 P1 C9 70.7(3) . . . . ? C5 W1 P1 C9 -103.6(3) . . . . ? P2 W1 P1 C9 -18.9(2) . . . . ? C7 W1 P1 C16 -74.4(2) . . . . ? C3 W1 P1 C16 -48.0(7) . . . . ? C1 W1 P1 C16 -167.1(2) . . . . ? C5 W1 P1 C16 18.6(2) . . . . ? P2 W1 P1 C16 103.31(18) . . . . ? C7 W1 P1 C22 37.6(2) . . . . ? C3 W1 P1 C22 64.1(7) . . . . ? C1 W1 P1 C22 -55.0(2) . . . . ? C5 W1 P1 C22 130.7(2) . . . . ? P2 W1 P1 C22 -144.63(19) . . . . ? C7 W1 P2 C28 -48.8(9) . . . . ? C3 W1 P2 C28 -42.9(2) . . . . ? C1 W1 P2 C28 53.4(2) . . . . ? C5 W1 P2 C28 -131.5(2) . . . . ? P1 W1 P2 C28 143.68(19) . . . . ? C7 W1 P2 C11 -173.9(9) . . . . ? C3 W1 P2 C11 -168.0(3) . . . . ? C1 W1 P2 C11 -71.7(3) . . . . ? C5 W1 P2 C11 103.4(3) . . . . ? P1 W1 P2 C11 18.6(2) . . . . ? C7 W1 P2 C34 66.0(9) . . . . ? C3 W1 P2 C34 71.9(2) . . . . ? C1 W1 P2 C34 168.1(2) . . . . ? C5 W1 P2 C34 -16.7(2) . . . . ? P1 W1 P2 C34 -101.55(19) . . . . ? C16 P1 C9 Si1 166.2(3) . . . . ? C22 P1 C9 Si1 63.6(4) . . . . ? W1 P1 C9 Si1 -69.2(4) . . . . ? N10 Si1 C9 P1 68.0(4) . . . . ? C12 Si1 C9 P1 -53.2(4) . . . . ? C13 Si1 C9 P1 -172.2(3) . . . . ? C12 Si1 N10 Si2 -172.3(3) . . . . ? C13 Si1 N10 Si2 -51.8(4) . . . . ? C9 Si1 N10 Si2 62.5(4) . . . . ? C15 Si2 N10 Si1 170.7(3) . . . . ? C14 Si2 N10 Si1 49.3(4) . . . . ? C11 Si2 N10 Si1 -63.8(4) . . . . ? C28 P2 C11 Si2 -62.2(4) . . . . ? C34 P2 C11 Si2 -165.6(3) . . . . ? W1 P2 C11 Si2 69.8(4) . . . . ? N10 Si2 C11 P2 -67.0(4) . . . . ? C15 Si2 C11 P2 55.3(4) . . . . ? C14 Si2 C11 P2 174.1(3) . . . . ? C9 P1 C16 C21 24.0(6) . . . . ? C22 P1 C16 C21 127.5(5) . . . . ? W1 P1 C16 C21 -109.1(5) . . . . ? C9 P1 C16 C17 -158.3(4) . . . . ? C22 P1 C16 C17 -54.9(5) . . . . ? W1 P1 C16 C17 68.5(5) . . . . ? C21 C16 C17 C18 -0.2(9) . . . . ? P1 C16 C17 C18 -178.0(5) . . . . ? C16 C17 C18 C19 0.9(9) . . . . ? C17 C18 C19 C20 -1.3(9) . . . . ? C18 C19 C20 C21 1.0(9) . . . . ? C19 C20 C21 C16 -0.4(9) . . . . ? C17 C16 C21 C20 0.0(9) . . . . ? P1 C16 C21 C20 177.6(5) . . . . ? C9 P1 C22 C27 -117.6(4) . . . . ? C16 P1 C22 C27 136.2(4) . . . . ? W1 P1 C22 C27 18.7(5) . . . . ? C9 P1 C22 C23 60.9(4) . . . . ? C16 P1 C22 C23 -45.4(4) . . . . ? W1 P1 C22 C23 -162.9(3) . . . . ? C27 C22 C23 C24 1.6(7) . . . . ? P1 C22 C23 C24 -176.9(4) . . . . ? C22 C23 C24 C25 0.1(8) . . . . ? C23 C24 C25 C26 -2.0(8) . . . . ? C24 C25 C26 C27 2.1(8) . . . . ? C25 C26 C27 C22 -0.3(8) . . . . ? C23 C22 C27 C26 -1.5(7) . . . . ? P1 C22 C27 C26 176.9(4) . . . . ? C11 P2 C28 C33 -54.8(5) . . . . ? C34 P2 C28 C33 49.4(5) . . . . ? W1 P2 C28 C33 169.9(4) . . . . ? C11 P2 C28 C29 123.2(4) . . . . ? C34 P2 C28 C29 -132.6(4) . . . . ? W1 P2 C28 C29 -12.1(5) . . . . ? C33 C28 C29 C30 2.0(8) . . . . ? P2 C28 C29 C30 -176.1(4) . . . . ? C28 C29 C30 C31 -1.4(8) . . . . ? C29 C30 C31 C32 0.4(8) . . . . ? C30 C31 C32 C33 -0.1(8) . . . . ? C31 C32 C33 C28 0.8(8) . . . . ? C29 C28 C33 C32 -1.7(8) . . . . ? P2 C28 C33 C32 176.4(4) . . . . ? C28 P2 C34 C35 43.4(5) . . . . ? C11 P2 C34 C35 147.1(4) . . . . ? W1 P2 C34 C35 -81.0(4) . . . . ? C28 P2 C34 C39 -139.4(4) . . . . ? C11 P2 C34 C39 -35.7(5) . . . . ? W1 P2 C34 C39 96.1(4) . . . . ? C39 C34 C35 C36 2.2(8) . . . . ? P2 C34 C35 C36 179.4(4) . . . . ? C34 C35 C36 C37 -1.6(8) . . . . ? C35 C36 C37 C38 0.6(8) . . . . ? C36 C37 C38 C39 -0.2(8) . . . . ? C37 C38 C39 C34 0.9(8) . . . . ? C35 C34 C39 C38 -1.8(7) . . . . ? P2 C34 C39 C38 -179.0(4) . . . . ? C42 C40 C41 C42 -0.4(12) 3_676 . . . ? C40 C41 C42 C40 0.4(12) . . . 3_676 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.252 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.141 # Attachment '- x0911002.cif' data_x0911002 _database_code_depnum_ccdc_archive 'CCDC 893806' #TrackingRef '- x0911002.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H38 N O3 P2 Si2 W, B F4, C H2 Cl2' _chemical_formula_sum 'C34 H40 B Cl2 F4 N O3 P2 Si2 W' _chemical_formula_weight 970.35 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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' F F 0.0727 0.0534 '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' W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1944(5) _cell_length_b 18.9951(8) _cell_length_c 15.4344(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.665(2) _cell_angle_gamma 90.00 _cell_volume 3868.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8257 _cell_measurement_theta_min 3.69 _cell_measurement_theta_max 67.07 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 8.654 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2018 _exptl_absorpt_correction_T_max 0.7345 _exptl_absorpt_process_details Apex2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31454 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 67.96 _reflns_number_total 6614 _reflns_number_gt 4823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0661P)^2^+38.6559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6614 _refine_ls_number_parameters 461 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 W1 W 0.74193(3) 0.60404(2) 0.74242(3) 0.02794(16) Uani 0.50 1 d PDU A 1 C1 C 0.7130(14) 0.6058(11) 0.8670(8) 0.035(3) Uani 0.50 1 d PDU A 1 O2 O 0.6899(11) 0.6054(9) 0.9378(7) 0.050(3) Uani 0.50 1 d PDU A 1 W1A W 0.74193(3) 0.60404(2) 0.74242(3) 0.02794(16) Uani 0.50 1 d PD A 2 C3 C 0.7836(14) 0.6087(11) 0.8649(9) 0.035(3) Uani 0.50 1 d PD A 2 O4 O 0.8012(11) 0.6120(9) 0.9371(7) 0.050(3) Uani 0.50 1 d PD A 2 P1 P 0.93115(18) 0.58845(12) 0.72632(16) 0.0280(5) Uani 1 1 d . . . P2 P 0.55430(19) 0.60875(14) 0.71640(18) 0.0354(6) Uani 1 1 d . . . Si1 Si 0.8681(2) 0.62346(14) 0.54559(17) 0.0310(6) Uani 1 1 d . . . Si2 Si 0.6349(2) 0.63457(15) 0.53417(19) 0.0362(7) Uani 1 1 d . . . C5 C 0.7442(7) 0.7106(5) 0.7440(6) 0.029(2) Uani 1 1 d . . . O6 O 0.7459(6) 0.7712(4) 0.7509(5) 0.0464(19) Uani 1 1 d . A . C7 C 0.7378(8) 0.4966(5) 0.7480(7) 0.033(2) Uani 1 1 d . . . O8 O 0.7372(5) 0.4375(4) 0.7591(5) 0.0439(19) Uani 1 1 d . A . C9 C 0.9875(7) 0.5181(5) 0.7922(6) 0.030(2) Uani 1 1 d . A . C10 C 1.0378(7) 0.5326(5) 0.8682(7) 0.038(2) Uani 1 1 d . . . H10 H 1.0433 0.5801 0.8870 0.045 Uiso 1 1 calc R A . C11 C 1.0810(8) 0.4797(5) 0.9185(7) 0.039(2) Uani 1 1 d . A . H11 H 1.1130 0.4907 0.9723 0.047 Uiso 1 1 calc R . . C12 C 1.0770(8) 0.4112(6) 0.8897(8) 0.043(3) Uani 1 1 d . . . H12 H 1.1077 0.3749 0.9232 0.052 Uiso 1 1 calc R A . C13 C 1.0291(8) 0.3949(6) 0.8134(7) 0.040(2) Uani 1 1 d . A . H13 H 1.0271 0.3474 0.7944 0.047 Uiso 1 1 calc R . . C14 C 0.9833(7) 0.4472(5) 0.7630(7) 0.034(2) Uani 1 1 d . . . H14 H 0.9498 0.4355 0.7101 0.041 Uiso 1 1 calc R A . C15 C 1.0147(7) 0.6620(5) 0.7517(7) 0.031(2) Uani 1 1 d . A . C16 C 0.9904(7) 0.7100(5) 0.8179(6) 0.033(2) Uani 1 1 d . . . H16 H 0.9276 0.7062 0.8471 0.039 Uiso 1 1 calc R A . C17 C 1.0586(7) 0.7629(5) 0.8403(7) 0.037(2) Uani 1 1 d . A . H17 H 1.0414 0.7958 0.8841 0.044 Uiso 1 1 calc R . . C18 C 1.1499(8) 0.7683(5) 0.8002(7) 0.039(3) Uani 1 1 d . . . H18 H 1.1957 0.8046 0.8168 0.047 Uiso 1 1 calc R A . C19 C 1.1772(8) 0.7205(6) 0.7344(7) 0.042(3) Uani 1 1 d . A . H19 H 1.2403 0.7249 0.7058 0.051 Uiso 1 1 calc R . . C20 C 1.1091(8) 0.6662(6) 0.7120(7) 0.041(3) Uani 1 1 d . . . H20 H 1.1275 0.6323 0.6697 0.049 Uiso 1 1 calc R A . C21 C 0.9527(7) 0.5663(5) 0.6136(6) 0.033(2) Uani 1 1 d . A . H21A H 0.9369 0.5160 0.6032 0.039 Uiso 1 1 calc R . . H21B H 1.0246 0.5745 0.5989 0.039 Uiso 1 1 calc R . . C22 C 0.8787(8) 0.5988(5) 0.4297(6) 0.037(2) Uani 1 1 d . A . H22A H 0.8543 0.5505 0.4214 0.055 Uiso 1 1 calc R . . H22B H 0.9497 0.6019 0.4122 0.055 Uiso 1 1 calc R . . H22C H 0.8376 0.6310 0.3942 0.055 Uiso 1 1 calc R . . C23 C 0.8999(8) 0.7179(5) 0.5597(7) 0.041(3) Uani 1 1 d . A . H23A H 0.8640 0.7457 0.5156 0.061 Uiso 1 1 calc R . . H23B H 0.9732 0.7244 0.5534 0.061 Uiso 1 1 calc R . . H23C H 0.8795 0.7334 0.6174 0.061 Uiso 1 1 calc R . . N24 N 0.7488(6) 0.6017(4) 0.5881(5) 0.0323(18) Uani 1 1 d . A . H24 H 0.7449 0.5537 0.5766 0.039 Uiso 1 1 calc R B 1 C25 C 0.6210(8) 0.5957(6) 0.4250(7) 0.049(3) Uani 1 1 d . A . H25A H 0.6537 0.6262 0.3825 0.073 Uiso 1 1 calc R . . H25B H 0.5488 0.5910 0.4103 0.073 Uiso 1 1 calc R . . H25C H 0.6530 0.5491 0.4243 0.073 Uiso 1 1 calc R . . C26 C 0.6412(8) 0.7334(5) 0.5298(7) 0.043(3) Uani 1 1 d . A . H26A H 0.6652 0.7515 0.5859 0.065 Uiso 1 1 calc R . . H26B H 0.5736 0.7523 0.5170 0.065 Uiso 1 1 calc R . . H26C H 0.6881 0.7478 0.4844 0.065 Uiso 1 1 calc R . . C27 C 0.5289(8) 0.5997(6) 0.6015(7) 0.043(3) Uani 1 1 d . A . H27A H 0.4658 0.6254 0.5865 0.052 Uiso 1 1 calc R . . H27B H 0.5180 0.5494 0.5876 0.052 Uiso 1 1 calc R . . C28 C 0.4951(8) 0.6920(6) 0.7491(8) 0.045(3) Uani 1 1 d . A . C29 C 0.4632(9) 0.7432(7) 0.6892(10) 0.061(4) Uani 1 1 d . . . H29 H 0.4703 0.7351 0.6288 0.073 Uiso 1 1 calc R A . C30 C 0.4214(10) 0.8059(7) 0.7183(11) 0.065(4) Uani 1 1 d . A . H30 H 0.3990 0.8406 0.6781 0.078 Uiso 1 1 calc R . . C31 C 0.4129(9) 0.8171(7) 0.8054(11) 0.063(4) Uani 1 1 d . . . H31 H 0.3880 0.8609 0.8259 0.075 Uiso 1 1 calc R A . C32 C 0.4401(9) 0.7655(7) 0.8633(9) 0.057(3) Uani 1 1 d . A . H32 H 0.4287 0.7714 0.9235 0.068 Uiso 1 1 calc R . . C33 C 0.4847(9) 0.7043(6) 0.8320(9) 0.053(3) Uani 1 1 d . . . H33 H 0.5085 0.6702 0.8723 0.064 Uiso 1 1 calc R A . C34 C 0.4721(7) 0.5439(6) 0.7678(7) 0.038(3) Uani 1 1 d . A . C35 C 0.3713(8) 0.5410(6) 0.7431(7) 0.040(3) Uani 1 1 d . . . H35 H 0.3469 0.5719 0.6992 0.048 Uiso 1 1 calc R A . C36 C 0.3052(9) 0.4940(7) 0.7808(8) 0.055(3) Uani 1 1 d . A . H36 H 0.2364 0.4918 0.7622 0.065 Uiso 1 1 calc R . . C37 C 0.3414(9) 0.4495(6) 0.8475(9) 0.056(3) Uani 1 1 d . . . H37 H 0.2972 0.4165 0.8737 0.068 Uiso 1 1 calc R A . C38 C 0.4392(9) 0.4539(7) 0.8740(9) 0.064(4) Uani 1 1 d . A . H38 H 0.4632 0.4246 0.9198 0.077 Uiso 1 1 calc R . . C39 C 0.5054(8) 0.5014(6) 0.8346(9) 0.050(3) Uani 1 1 d . . . H39 H 0.5738 0.5043 0.8540 0.060 Uiso 1 1 calc R A . B1 B 0.7581(9) 0.0923(6) 0.0098(8) 0.035(3) Uani 1 1 d . . . F1 F 0.6943(5) 0.0469(3) 0.0574(4) 0.0523(17) Uani 1 1 d . . . F2 F 0.8491(5) 0.0983(4) 0.0551(5) 0.066(2) Uani 1 1 d . . . F3 F 0.7733(5) 0.0640(3) -0.0698(4) 0.0531(17) Uani 1 1 d . . . F4 F 0.7110(5) 0.1568(3) 0.0027(5) 0.062(2) Uani 1 1 d . . . C40 C 0.2492(12) 0.6657(9) 0.9721(12) 0.093(5) Uani 1 1 d . . . H40A H 0.2286 0.6578 0.9110 0.111 Uiso 1 1 calc R . . H40B H 0.2733 0.7148 0.9775 0.111 Uiso 1 1 calc R . . Cl2 Cl 0.3456(4) 0.6094(4) 0.9990(4) 0.145(3) Uani 1 1 d . . . Cl4 Cl 0.1452(3) 0.6536(2) 1.0382(3) 0.0758(10) 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 W1 0.0285(2) 0.0208(2) 0.0346(3) -0.0019(2) 0.00312(18) -0.00084(19) C1 0.040(8) 0.029(7) 0.035(3) 0.002(6) 0.006(7) 0.004(9) O2 0.043(6) 0.069(8) 0.039(3) 0.000(6) 0.013(5) 0.002(6) W1A 0.0285(2) 0.0208(2) 0.0346(3) -0.0019(2) 0.00312(18) -0.00084(19) C3 0.040(8) 0.029(7) 0.035(3) 0.002(6) 0.006(7) 0.004(9) O4 0.043(6) 0.069(8) 0.039(3) 0.000(6) 0.013(5) 0.002(6) P1 0.0280(12) 0.0219(13) 0.0339(12) -0.0030(10) 0.0022(11) 0.0014(9) P2 0.0290(12) 0.0270(13) 0.0504(15) -0.0042(13) 0.0035(12) 0.0003(11) Si1 0.0355(14) 0.0247(14) 0.0329(13) -0.0030(11) 0.0040(13) -0.0007(11) Si2 0.0369(15) 0.0288(15) 0.0427(15) -0.0013(13) -0.0054(14) 0.0030(12) C5 0.032(5) 0.023(5) 0.032(5) -0.003(4) 0.005(4) 0.003(4) O6 0.056(5) 0.027(4) 0.057(5) -0.007(4) -0.002(4) 0.008(3) C7 0.040(6) 0.019(5) 0.040(6) -0.002(5) 0.006(5) -0.001(4) O8 0.046(4) 0.033(5) 0.053(5) -0.002(4) 0.017(4) -0.001(3) C9 0.025(5) 0.026(5) 0.039(5) -0.003(4) 0.015(5) -0.004(4) C10 0.040(6) 0.024(5) 0.049(6) -0.007(5) -0.005(5) 0.001(4) C11 0.041(6) 0.034(6) 0.042(6) 0.001(5) 0.005(5) 0.001(5) C12 0.041(6) 0.033(6) 0.055(7) 0.006(5) 0.002(6) 0.002(5) C13 0.043(6) 0.028(6) 0.047(6) -0.007(5) 0.008(5) 0.001(5) C14 0.034(5) 0.024(5) 0.045(6) 0.005(5) -0.002(5) -0.008(4) C15 0.031(5) 0.020(5) 0.042(5) 0.004(4) 0.001(5) -0.002(4) C16 0.029(5) 0.031(6) 0.037(5) -0.009(5) 0.006(5) -0.001(4) C17 0.036(6) 0.034(6) 0.040(6) -0.009(5) -0.008(5) 0.005(4) C18 0.035(6) 0.023(5) 0.058(7) 0.006(5) -0.007(6) -0.005(4) C19 0.027(5) 0.044(7) 0.056(7) 0.004(6) 0.010(5) -0.009(5) C20 0.040(6) 0.040(7) 0.042(6) -0.010(5) 0.006(5) -0.001(5) C21 0.029(5) 0.025(5) 0.045(6) -0.010(5) 0.012(5) 0.002(4) C22 0.049(6) 0.022(5) 0.039(5) -0.004(5) 0.005(5) -0.005(5) C23 0.046(6) 0.033(6) 0.044(6) -0.004(5) -0.001(5) -0.009(5) N24 0.044(5) 0.020(4) 0.033(4) -0.003(4) 0.000(4) 0.004(4) C25 0.041(6) 0.057(8) 0.049(6) -0.003(6) -0.008(6) 0.016(5) C26 0.047(6) 0.028(6) 0.055(7) 0.000(5) 0.002(6) 0.001(5) C27 0.035(5) 0.043(7) 0.052(6) -0.012(6) -0.002(5) 0.007(5) C28 0.033(6) 0.034(6) 0.067(8) -0.002(6) -0.002(6) -0.004(5) C29 0.048(7) 0.041(8) 0.094(10) 0.000(7) 0.018(7) 0.007(6) C30 0.052(8) 0.039(7) 0.103(12) 0.010(8) 0.008(8) 0.004(6) C31 0.037(6) 0.041(7) 0.109(12) -0.019(8) -0.020(8) 0.003(5) C32 0.046(7) 0.055(8) 0.069(8) -0.022(7) -0.011(7) 0.011(6) C33 0.049(7) 0.040(7) 0.069(8) -0.013(6) -0.018(7) 0.014(5) C34 0.028(5) 0.034(6) 0.053(6) -0.017(5) 0.006(5) 0.001(4) C35 0.038(6) 0.036(6) 0.045(6) -0.007(5) 0.002(5) -0.009(5) C36 0.031(6) 0.072(9) 0.061(8) -0.007(7) 0.006(6) -0.015(6) C37 0.049(7) 0.038(7) 0.083(9) 0.004(7) 0.019(7) -0.011(5) C38 0.044(7) 0.070(10) 0.078(9) 0.023(8) 0.013(7) 0.014(6) C39 0.026(5) 0.039(7) 0.086(9) 0.002(7) 0.014(6) -0.002(5) B1 0.035(6) 0.024(6) 0.045(7) 0.002(5) 0.004(6) -0.004(5) F1 0.067(4) 0.042(4) 0.049(4) 0.003(3) 0.016(3) 0.001(3) F2 0.050(4) 0.070(5) 0.076(5) -0.015(4) -0.025(4) 0.003(4) F3 0.073(5) 0.050(4) 0.037(3) -0.005(3) 0.005(3) -0.013(3) F4 0.055(4) 0.036(4) 0.095(5) 0.020(4) 0.020(4) 0.015(3) C40 0.080(11) 0.094(14) 0.104(13) 0.041(11) 0.015(10) -0.005(9) Cl2 0.129(4) 0.197(6) 0.108(4) 0.042(4) 0.023(3) 0.099(4) Cl4 0.060(2) 0.083(3) 0.084(2) -0.022(2) 0.0021(19) -0.0069(18) _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 W1 C1 1.965(13) . ? W1 C5 2.025(9) . ? W1 C7 2.044(9) . ? W1 N24 2.386(8) . ? W1 P2 2.505(2) . ? W1 P1 2.529(2) . ? C1 O2 1.137(16) . ? C3 O4 1.137(16) . ? P1 C21 1.815(10) . ? P1 C15 1.820(9) . ? P1 C9 1.832(10) . ? P2 C27 1.809(11) . ? P2 C34 1.828(11) . ? P2 C28 1.836(12) . ? Si1 N24 1.761(9) . ? Si1 C23 1.854(10) . ? Si1 C22 1.856(10) . ? Si1 C21 1.872(10) . ? Si2 N24 1.819(8) . ? Si2 C25 1.847(11) . ? Si2 C27 1.873(11) . ? Si2 C26 1.880(10) . ? C5 O6 1.155(11) . ? C7 O8 1.135(11) . ? C9 C10 1.370(14) . ? C9 C14 1.421(13) . ? C10 C11 1.389(14) . ? C10 H10 0.9500 . ? C11 C12 1.377(14) . ? C11 H11 0.9500 . ? C12 C13 1.364(15) . ? C12 H12 0.9500 . ? C13 C14 1.394(14) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.398(14) . ? C15 C16 1.408(13) . ? C16 C17 1.390(13) . ? C16 H16 0.9500 . ? C17 C18 1.365(14) . ? C17 H17 0.9500 . ? C18 C19 1.412(15) . ? C18 H18 0.9500 . ? C19 C20 1.408(14) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N24 H24 0.9300 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.309(17) . ? C28 C29 1.404(17) . ? C29 C30 1.389(17) . ? C29 H29 0.9500 . ? C30 C31 1.368(19) . ? C30 H30 0.9500 . ? C31 C32 1.371(18) . ? C31 H31 0.9500 . ? C32 C33 1.392(15) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.377(16) . ? C34 C35 1.381(14) . ? C35 C36 1.381(15) . ? C35 H35 0.9500 . ? C36 C37 1.412(18) . ? C36 H36 0.9500 . ? C37 C38 1.352(17) . ? C37 H37 0.9500 . ? C38 C39 1.399(16) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? B1 F3 1.358(13) . ? B1 F4 1.377(13) . ? B1 F2 1.387(13) . ? B1 F1 1.416(13) . ? C40 Cl2 1.709(16) . ? C40 Cl4 1.735(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 W1 C5 88.5(7) . . ? C1 W1 C7 88.3(7) . . ? C5 W1 C7 176.8(4) . . ? C1 W1 N24 171.0(6) . . ? C5 W1 N24 91.7(3) . . ? C7 W1 N24 91.4(3) . . ? C1 W1 P2 87.3(6) . . ? C5 W1 P2 88.9(3) . . ? C7 W1 P2 90.9(3) . . ? N24 W1 P2 83.7(2) . . ? C1 W1 P1 107.5(6) . . ? C5 W1 P1 96.0(3) . . ? C7 W1 P1 85.1(3) . . ? N24 W1 P1 81.4(2) . . ? P2 W1 P1 164.42(9) . . ? O2 C1 W1 175.4(17) . . ? C21 P1 C15 106.5(5) . . ? C21 P1 C9 107.1(4) . . ? C15 P1 C9 101.6(4) . . ? C21 P1 W1 106.7(3) . . ? C15 P1 W1 119.0(3) . . ? C9 P1 W1 115.2(3) . . ? C27 P2 C34 104.9(5) . . ? C27 P2 C28 106.0(5) . . ? C34 P2 C28 101.8(5) . . ? C27 P2 W1 109.0(3) . . ? C34 P2 W1 119.8(4) . . ? C28 P2 W1 114.2(3) . . ? N24 Si1 C23 112.7(5) . . ? N24 Si1 C22 112.1(4) . . ? C23 Si1 C22 109.7(5) . . ? N24 Si1 C21 100.7(4) . . ? C23 Si1 C21 111.3(5) . . ? C22 Si1 C21 110.1(5) . . ? N24 Si2 C25 110.6(4) . . ? N24 Si2 C27 104.1(4) . . ? C25 Si2 C27 107.3(5) . . ? N24 Si2 C26 108.8(4) . . ? C25 Si2 C26 111.8(5) . . ? C27 Si2 C26 114.0(5) . . ? O6 C5 W1 175.4(8) . . ? O8 C7 W1 173.6(9) . . ? C10 C9 C14 118.6(9) . . ? C10 C9 P1 121.2(7) . . ? C14 C9 P1 120.2(7) . . ? C9 C10 C11 121.7(10) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 119.3(10) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 120.6(10) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.9(10) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C9 118.9(9) . . ? C13 C14 H14 120.5 . . ? C9 C14 H14 120.5 . . ? C20 C15 C16 119.5(9) . . ? C20 C15 P1 119.4(8) . . ? C16 C15 P1 120.7(7) . . ? C17 C16 C15 119.7(9) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.9(10) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.8(9) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 118.7(10) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C15 C20 C19 120.2(10) . . ? C15 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? P1 C21 Si1 107.7(5) . . ? P1 C21 H21A 110.2 . . ? Si1 C21 H21A 110.2 . . ? P1 C21 H21B 110.2 . . ? Si1 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 N24 Si2 119.1(4) . . ? Si1 N24 W1 114.3(4) . . ? Si2 N24 W1 114.2(4) . . ? Si1 N24 H24 101.9 . . ? Si2 N24 H24 101.9 . . ? W1 N24 H24 101.9 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P2 C27 Si2 112.3(5) . . ? P2 C27 H27A 109.1 . . ? Si2 C27 H27A 109.1 . . ? P2 C27 H27B 109.1 . . ? Si2 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C33 C28 C29 119.0(12) . . ? C33 C28 P2 118.2(9) . . ? C29 C28 P2 122.8(10) . . ? C30 C29 C28 119.9(14) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 119.3(14) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 120.3(13) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 118.7(13) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C28 C33 C32 122.6(12) . . ? C28 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C39 C34 C35 118.7(10) . . ? C39 C34 P2 122.3(8) . . ? C35 C34 P2 118.8(9) . . ? C36 C35 C34 121.4(11) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 119.0(11) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 119.8(12) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 120.4(12) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C34 C39 C38 120.6(11) . . ? C34 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? F3 B1 F4 110.6(10) . . ? F3 B1 F2 110.6(9) . . ? F4 B1 F2 110.7(9) . . ? F3 B1 F1 108.9(9) . . ? F4 B1 F1 108.2(9) . . ? F2 B1 F1 107.7(9) . . ? Cl2 C40 Cl4 111.5(9) . . ? Cl2 C40 H40A 109.3 . . ? Cl4 C40 H40A 109.3 . . ? Cl2 C40 H40B 109.3 . . ? Cl4 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 W1 C1 O2 109(25) . . . . ? C7 W1 C1 O2 -71(25) . . . . ? N24 W1 C1 O2 18(28) . . . . ? P2 W1 C1 O2 20(25) . . . . ? P1 W1 C1 O2 -155(24) . . . . ? C1 W1 P1 C21 166.9(7) . . . . ? C5 W1 P1 C21 -102.8(4) . . . . ? C7 W1 P1 C21 80.2(4) . . . . ? N24 W1 P1 C21 -12.0(4) . . . . ? P2 W1 P1 C21 4.8(5) . . . . ? C1 W1 P1 C15 -72.8(7) . . . . ? C5 W1 P1 C15 17.5(5) . . . . ? C7 W1 P1 C15 -159.5(5) . . . . ? N24 W1 P1 C15 108.3(4) . . . . ? P2 W1 P1 C15 125.1(5) . . . . ? C1 W1 P1 C9 48.1(7) . . . . ? C5 W1 P1 C9 138.4(4) . . . . ? C7 W1 P1 C9 -38.6(4) . . . . ? N24 W1 P1 C9 -130.8(4) . . . . ? P2 W1 P1 C9 -114.0(4) . . . . ? C1 W1 P2 C27 -174.4(7) . . . . ? C5 W1 P2 C27 97.0(5) . . . . ? C7 W1 P2 C27 -86.2(5) . . . . ? N24 W1 P2 C27 5.2(4) . . . . ? P1 W1 P2 C27 -11.5(6) . . . . ? C1 W1 P2 C34 -53.7(7) . . . . ? C5 W1 P2 C34 -142.3(5) . . . . ? C7 W1 P2 C34 34.5(5) . . . . ? N24 W1 P2 C34 125.9(4) . . . . ? P1 W1 P2 C34 109.2(5) . . . . ? C1 W1 P2 C28 67.2(8) . . . . ? C5 W1 P2 C28 -21.3(5) . . . . ? C7 W1 P2 C28 155.5(5) . . . . ? N24 W1 P2 C28 -113.2(5) . . . . ? P1 W1 P2 C28 -129.8(5) . . . . ? C1 W1 C5 O6 14(10) . . . . ? C7 W1 C5 O6 15(15) . . . . ? N24 W1 C5 O6 -175(10) . . . . ? P2 W1 C5 O6 102(10) . . . . ? P1 W1 C5 O6 -93(10) . . . . ? C1 W1 C7 O8 -21(8) . . . . ? C5 W1 C7 O8 -22(13) . . . . ? N24 W1 C7 O8 168(8) . . . . ? P2 W1 C7 O8 -109(8) . . . . ? P1 W1 C7 O8 87(8) . . . . ? C21 P1 C9 C10 141.0(8) . . . . ? C15 P1 C9 C10 29.6(9) . . . . ? W1 P1 C9 C10 -100.5(8) . . . . ? C21 P1 C9 C14 -36.4(9) . . . . ? C15 P1 C9 C14 -147.8(8) . . . . ? W1 P1 C9 C14 82.2(8) . . . . ? C14 C9 C10 C11 -2.4(15) . . . . ? P1 C9 C10 C11 -179.9(8) . . . . ? C9 C10 C11 C12 2.7(17) . . . . ? C10 C11 C12 C13 -1.4(17) . . . . ? C11 C12 C13 C14 0.0(17) . . . . ? C12 C13 C14 C9 0.3(16) . . . . ? C10 C9 C14 C13 0.9(14) . . . . ? P1 C9 C14 C13 178.4(8) . . . . ? C21 P1 C15 C20 -33.6(9) . . . . ? C9 P1 C15 C20 78.4(9) . . . . ? W1 P1 C15 C20 -154.0(7) . . . . ? C21 P1 C15 C16 153.8(8) . . . . ? C9 P1 C15 C16 -94.2(8) . . . . ? W1 P1 C15 C16 33.4(9) . . . . ? C20 C15 C16 C17 2.9(15) . . . . ? P1 C15 C16 C17 175.5(8) . . . . ? C15 C16 C17 C18 -1.3(15) . . . . ? C16 C17 C18 C19 0.5(16) . . . . ? C17 C18 C19 C20 -1.2(16) . . . . ? C16 C15 C20 C19 -3.7(16) . . . . ? P1 C15 C20 C19 -176.4(8) . . . . ? C18 C19 C20 C15 2.8(16) . . . . ? C15 P1 C21 Si1 -86.5(5) . . . . ? C9 P1 C21 Si1 165.4(5) . . . . ? W1 P1 C21 Si1 41.5(5) . . . . ? N24 Si1 C21 P1 -57.1(5) . . . . ? C23 Si1 C21 P1 62.5(6) . . . . ? C22 Si1 C21 P1 -175.6(5) . . . . ? C23 Si1 N24 Si2 69.6(6) . . . . ? C22 Si1 N24 Si2 -54.8(6) . . . . ? C21 Si1 N24 Si2 -171.8(5) . . . . ? C23 Si1 N24 W1 -70.4(5) . . . . ? C22 Si1 N24 W1 165.2(4) . . . . ? C21 Si1 N24 W1 48.2(5) . . . . ? C25 Si2 N24 Si1 65.6(7) . . . . ? C27 Si2 N24 Si1 -179.4(5) . . . . ? C26 Si2 N24 Si1 -57.5(6) . . . . ? C25 Si2 N24 W1 -154.3(5) . . . . ? C27 Si2 N24 W1 -39.3(5) . . . . ? C26 Si2 N24 W1 82.5(5) . . . . ? C1 W1 N24 Si1 165(4) . . . . ? C5 W1 N24 Si1 73.7(5) . . . . ? C7 W1 N24 Si1 -106.8(5) . . . . ? P2 W1 N24 Si1 162.4(4) . . . . ? P1 W1 N24 Si1 -22.0(4) . . . . ? C1 W1 N24 Si2 23(4) . . . . ? C5 W1 N24 Si2 -68.3(5) . . . . ? C7 W1 N24 Si2 111.2(5) . . . . ? P2 W1 N24 Si2 20.4(4) . . . . ? P1 W1 N24 Si2 -164.1(4) . . . . ? C34 P2 C27 Si2 -158.5(5) . . . . ? C28 P2 C27 Si2 94.3(6) . . . . ? W1 P2 C27 Si2 -29.0(6) . . . . ? N24 Si2 C27 P2 43.5(7) . . . . ? C25 Si2 C27 P2 160.8(6) . . . . ? C26 Si2 C27 P2 -74.8(7) . . . . ? C27 P2 C28 C33 166.5(10) . . . . ? C34 P2 C28 C33 57.0(11) . . . . ? W1 P2 C28 C33 -73.5(10) . . . . ? C27 P2 C28 C29 -15.1(11) . . . . ? C34 P2 C28 C29 -124.6(10) . . . . ? W1 P2 C28 C29 104.9(9) . . . . ? C33 C28 C29 C30 0.0(18) . . . . ? P2 C28 C29 C30 -178.3(9) . . . . ? C28 C29 C30 C31 0.7(19) . . . . ? C29 C30 C31 C32 -3.6(19) . . . . ? C30 C31 C32 C33 5.6(19) . . . . ? C29 C28 C33 C32 2.1(18) . . . . ? P2 C28 C33 C32 -179.5(9) . . . . ? C31 C32 C33 C28 -5.0(19) . . . . ? C27 P2 C34 C39 136.7(10) . . . . ? C28 P2 C34 C39 -113.0(10) . . . . ? W1 P2 C34 C39 14.0(11) . . . . ? C27 P2 C34 C35 -48.1(9) . . . . ? C28 P2 C34 C35 62.3(9) . . . . ? W1 P2 C34 C35 -170.8(7) . . . . ? C39 C34 C35 C36 -3.3(16) . . . . ? P2 C34 C35 C36 -178.7(9) . . . . ? C34 C35 C36 C37 1.6(18) . . . . ? C35 C36 C37 C38 0.8(19) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C35 C34 C39 C38 2.7(18) . . . . ? P2 C34 C39 C38 178.0(10) . . . . ? C37 C38 C39 C34 0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 67.96 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.416 _refine_diff_density_min -2.251 _refine_diff_density_rms 0.164