Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global #============================================================================== _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? # 1. SUBMISSION DETAILS _publ_contact_author ; Peter G. Jones Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_phone '049 531 391-5382' _publ_contact_author_fax '049 531 391-5387' _publ_contact_author_email jones@xray36.anchem.nat.tu-bs.de _publ_requested_journal 'Chem. Commun.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of the first 2,3-dihydro-1,2,3-azadiphosphete complex ; loop_ _publ_author_name _publ_author_address 'Ionescu, Emanuel' ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; 'Jones, Peter G.' ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; 'Streubel, Rainer' ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; #============================================================================= # cif data for "loemilo" (compound 4 in manuscript) #============================================================================= data_loemilo _database_code_CSD 188876 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H43 N O5 P2 Si4 W' _chemical_formula_weight 807.76 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' 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 14.7253(8) _cell_length_b 13.0428(8) _cell_length_c 18.8621(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.072(4) _cell_angle_gamma 90.00 _cell_volume 3595.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6240 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 30.4 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 3.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6749 _exptl_absorpt_correction_T_max 0.8017 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 AXS Smart CCD 1000' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73721 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10522 _reflns_number_gt 7214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0176P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy-atom _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10522 _refine_ls_number_parameters 364 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.913 _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 W W 0.474329(6) 0.246679(8) 0.105676(4) 0.01894(3) Uani 1 1 d . . . P1 P 0.48635(4) 0.37887(4) 0.20424(3) 0.01712(12) Uani 1 1 d . . . P2 P 0.50100(4) 0.36662(4) 0.32450(3) 0.01703(12) Uani 1 1 d . . . Si1 Si 0.60339(4) 0.26115(5) 0.45265(3) 0.01985(13) Uani 1 1 d U . . Si2 Si 0.43278(4) 0.13717(5) 0.37060(3) 0.01943(13) Uani 1 1 d U . . Si3 Si 0.48285(4) 0.62088(5) 0.18667(3) 0.01990(13) Uani 1 1 d U . . Si4 Si 0.67170(4) 0.49679(5) 0.23054(3) 0.02234(14) Uani 1 1 d U . . N N 0.37788(12) 0.41728(13) 0.22232(10) 0.0197(4) Uani 1 1 d U . . O1 O 0.44057(11) 0.09422(12) -0.02457(9) 0.0293(4) Uani 1 1 d . . . O2 O 0.40289(13) 0.42507(14) -0.00190(9) 0.0403(5) Uani 1 1 d . . . O3 O 0.67536(13) 0.29052(16) 0.06642(10) 0.0461(5) Uani 1 1 d . . . O4 O 0.55930(12) 0.05757(13) 0.19781(9) 0.0353(4) Uani 1 1 d . . . O5 O 0.26675(11) 0.20629(15) 0.12959(9) 0.0354(4) Uani 1 1 d . . . C1 C 0.45408(15) 0.15020(18) 0.02301(13) 0.0226(5) Uani 1 1 d . . . C2 C 0.42795(16) 0.36227(19) 0.03814(12) 0.0265(5) Uani 1 1 d . . . C3 C 0.60347(18) 0.27549(18) 0.08210(13) 0.0289(6) Uani 1 1 d . . . C4 C 0.52716(15) 0.12725(19) 0.16682(12) 0.0238(5) Uani 1 1 d . . . C5 C 0.34208(17) 0.22021(18) 0.12359(12) 0.0248(5) Uani 1 1 d . . . C6 C 0.52617(14) 0.23790(15) 0.36472(11) 0.0173(4) Uani 1 1 d U . . H6 H 0.5677 0.2056 0.3330 0.021 Uiso 1 1 calc R . . C7 C 0.63693(16) 0.13778(18) 0.49869(12) 0.0261(5) Uani 1 1 d U . . H7A H 0.6682 0.0942 0.4670 0.039 Uiso 1 1 calc R . . H7B H 0.5821 0.1026 0.5107 0.039 Uiso 1 1 calc R . . H7C H 0.6781 0.1517 0.5425 0.039 Uiso 1 1 calc R . . C8 C 0.71122(15) 0.32692(18) 0.43625(12) 0.0258(5) Uani 1 1 d U . . H8A H 0.6964 0.3917 0.4111 0.039 Uiso 1 1 calc R . . H8B H 0.7457 0.2828 0.4070 0.039 Uiso 1 1 calc R . . H8C H 0.7483 0.3409 0.4820 0.039 Uiso 1 1 calc R . . C9 C 0.54521(16) 0.34572(18) 0.51291(12) 0.0291(6) Uani 1 1 d U . . H9A H 0.5846 0.3544 0.5583 0.044 Uiso 1 1 calc R . . H9B H 0.4872 0.3144 0.5218 0.044 Uiso 1 1 calc R . . H9C H 0.5332 0.4128 0.4902 0.044 Uiso 1 1 calc R . . C10 C 0.34189(15) 0.14035(17) 0.29308(12) 0.0244(5) Uani 1 1 d U . . H10A H 0.3695 0.1311 0.2488 0.037 Uiso 1 1 calc R . . H10B H 0.3103 0.2066 0.2918 0.037 Uiso 1 1 calc R . . H10C H 0.2979 0.0851 0.2977 0.037 Uiso 1 1 calc R . . C11 C 0.37743(15) 0.14925(18) 0.45425(12) 0.0247(5) Uani 1 1 d U . . H11A H 0.3466 0.2158 0.4547 0.037 Uiso 1 1 calc R . . H11B H 0.4242 0.1441 0.4958 0.037 Uiso 1 1 calc R . . H11C H 0.3325 0.0942 0.4560 0.037 Uiso 1 1 calc R . . C12 C 0.48862(16) 0.00848(17) 0.36686(12) 0.0247(5) Uani 1 1 d U . . H12A H 0.4420 -0.0454 0.3657 0.037 Uiso 1 1 calc R . . H12B H 0.5337 -0.0006 0.4092 0.037 Uiso 1 1 calc R . . H12C H 0.5193 0.0041 0.3237 0.037 Uiso 1 1 calc R . . C13 C 0.38039(14) 0.39086(15) 0.28920(12) 0.0177(4) Uani 1 1 d U . . C14 C 0.30065(15) 0.40144(16) 0.32858(12) 0.0198(5) Uani 1 1 d U . . C15 C 0.21281(15) 0.39899(17) 0.29121(14) 0.0257(5) Uani 1 1 d U . . H15 H 0.2047 0.3880 0.2410 0.031 Uiso 1 1 calc R . . C16 C 0.13741(17) 0.41267(18) 0.32738(15) 0.0334(6) Uani 1 1 d U . . H16 H 0.0776 0.4117 0.3019 0.040 Uiso 1 1 calc R . . C17 C 0.14890(19) 0.42774(18) 0.40036(16) 0.0376(7) Uani 1 1 d U . . H17 H 0.0968 0.4371 0.4248 0.045 Uiso 1 1 calc R . . C18 C 0.23494(19) 0.42936(19) 0.43808(15) 0.0368(7) Uani 1 1 d U . . H18 H 0.2422 0.4393 0.4884 0.044 Uiso 1 1 calc R . . C19 C 0.31143(17) 0.41628(17) 0.40227(13) 0.0281(5) Uani 1 1 d U . . H19 H 0.3710 0.4175 0.4281 0.034 Uiso 1 1 calc R . . C20 C 0.54858(13) 0.49492(16) 0.18487(11) 0.0173(4) Uani 1 1 d U . . H20 H 0.5562 0.4868 0.1332 0.021 Uiso 1 1 calc R . . C21 C 0.38283(15) 0.61927(18) 0.11585(12) 0.0269(5) Uani 1 1 d U . . H21A H 0.3428 0.5615 0.1240 0.040 Uiso 1 1 calc R . . H21B H 0.4043 0.6118 0.0690 0.040 Uiso 1 1 calc R . . H21C H 0.3487 0.6836 0.1173 0.040 Uiso 1 1 calc R . . C22 C 0.44608(16) 0.64986(18) 0.27581(12) 0.0280(5) Uani 1 1 d U . . H22A H 0.4355 0.7237 0.2797 0.042 Uiso 1 1 calc R . . H22B H 0.4940 0.6283 0.3136 0.042 Uiso 1 1 calc R . . H22C H 0.3894 0.6127 0.2809 0.042 Uiso 1 1 calc R . . C23 C 0.56030(16) 0.72544(16) 0.16307(14) 0.0285(6) Uani 1 1 d U . . H23A H 0.5853 0.7076 0.1189 0.043 Uiso 1 1 calc R . . H23B H 0.6106 0.7340 0.2018 0.043 Uiso 1 1 calc R . . H23C H 0.5258 0.7896 0.1562 0.043 Uiso 1 1 calc R . . C24 C 0.71606(15) 0.36365(18) 0.24904(13) 0.0281(5) Uani 1 1 d U . . H24A H 0.7219 0.3288 0.2038 0.042 Uiso 1 1 calc R . . H24B H 0.6734 0.3255 0.2751 0.042 Uiso 1 1 calc R . . H24C H 0.7761 0.3669 0.2779 0.042 Uiso 1 1 calc R . . C25 C 0.68475(16) 0.57292(18) 0.31540(13) 0.0309(6) Uani 1 1 d U . . H25A H 0.7473 0.5654 0.3394 0.046 Uiso 1 1 calc R . . H25B H 0.6413 0.5478 0.3468 0.046 Uiso 1 1 calc R . . H25C H 0.6724 0.6454 0.3044 0.046 Uiso 1 1 calc R . . C26 C 0.74596(16) 0.5531(2) 0.16709(14) 0.0365(7) Uani 1 1 d U . . H26A H 0.7334 0.6266 0.1617 0.055 Uiso 1 1 calc R . . H26B H 0.7331 0.5193 0.1205 0.055 Uiso 1 1 calc R . . H26C H 0.8104 0.5429 0.1858 0.055 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 W 0.01937(4) 0.02200(4) 0.01558(4) 0.00171(5) 0.00266(3) 0.00007(4) P1 0.0161(3) 0.0198(3) 0.0154(3) 0.0031(2) 0.0021(2) 0.0000(2) P2 0.0177(3) 0.0172(3) 0.0162(3) 0.0027(2) 0.0023(2) -0.0008(2) Si1 0.0212(3) 0.0219(3) 0.0161(3) 0.0024(3) 0.0006(2) -0.0004(3) Si2 0.0217(3) 0.0186(3) 0.0181(3) 0.0035(3) 0.0024(3) -0.0019(3) Si3 0.0199(3) 0.0194(3) 0.0207(3) 0.0039(3) 0.0034(3) 0.0014(3) Si4 0.0160(3) 0.0270(3) 0.0237(3) 0.0076(3) 0.0013(3) -0.0010(3) N 0.0173(9) 0.0197(10) 0.0225(10) 0.0028(8) 0.0039(8) -0.0011(7) O1 0.0348(10) 0.0292(10) 0.0240(9) -0.0025(8) 0.0038(8) 0.0047(8) O2 0.0603(13) 0.0349(11) 0.0246(10) 0.0073(8) 0.0004(9) 0.0091(9) O3 0.0303(10) 0.0741(14) 0.0365(11) 0.0066(10) 0.0147(9) -0.0063(10) O4 0.0331(10) 0.0356(10) 0.0363(11) 0.0124(9) 0.0013(8) 0.0032(8) O5 0.0230(10) 0.0564(12) 0.0258(10) 0.0051(8) -0.0004(8) -0.0038(8) C1 0.0223(12) 0.0231(12) 0.0231(13) 0.0073(10) 0.0053(10) 0.0050(10) C2 0.0303(14) 0.0301(14) 0.0192(12) -0.0017(11) 0.0026(10) 0.0001(11) C3 0.0336(14) 0.0326(15) 0.0203(12) 0.0013(10) 0.0032(10) 0.0008(11) C4 0.0197(12) 0.0313(13) 0.0207(12) -0.0007(10) 0.0042(9) -0.0034(10) C5 0.0290(13) 0.0291(13) 0.0156(11) 0.0031(9) -0.0006(10) 0.0012(10) C6 0.0191(10) 0.0174(11) 0.0155(9) 0.0014(9) 0.0024(8) 0.0000(9) C7 0.0277(13) 0.0301(13) 0.0198(12) 0.0051(10) -0.0007(10) 0.0007(10) C8 0.0235(12) 0.0318(14) 0.0210(12) 0.0027(10) -0.0021(10) -0.0039(10) C9 0.0308(14) 0.0320(14) 0.0239(13) -0.0028(11) 0.0012(11) -0.0018(11) C10 0.0241(12) 0.0216(12) 0.0269(13) 0.0003(10) 0.0015(10) -0.0028(10) C11 0.0260(12) 0.0265(13) 0.0225(12) 0.0030(10) 0.0061(10) -0.0014(10) C12 0.0299(13) 0.0228(12) 0.0217(12) 0.0037(10) 0.0044(10) -0.0032(10) C13 0.0181(11) 0.0120(10) 0.0235(12) 0.0029(9) 0.0039(9) -0.0009(8) C14 0.0205(11) 0.0117(10) 0.0287(13) 0.0042(9) 0.0087(10) 0.0013(9) C15 0.0217(12) 0.0201(12) 0.0362(14) 0.0067(10) 0.0068(10) 0.0001(9) C16 0.0219(13) 0.0242(13) 0.0560(18) 0.0088(12) 0.0122(12) 0.0029(10) C17 0.0361(15) 0.0209(13) 0.062(2) 0.0003(13) 0.0313(14) 0.0013(11) C18 0.0481(17) 0.0294(14) 0.0373(16) -0.0074(12) 0.0237(13) -0.0036(12) C19 0.0301(14) 0.0254(13) 0.0305(14) -0.0017(11) 0.0110(11) -0.0008(10) C20 0.0177(11) 0.0202(11) 0.0144(11) 0.0044(9) 0.0036(8) -0.0007(9) C21 0.0262(13) 0.0251(13) 0.0287(13) 0.0068(11) 0.0010(10) 0.0043(10) C22 0.0317(14) 0.0250(13) 0.0281(13) 0.0000(10) 0.0073(11) 0.0036(10) C23 0.0279(13) 0.0220(13) 0.0357(14) 0.0052(10) 0.0042(11) -0.0003(9) C24 0.0221(12) 0.0350(14) 0.0267(13) 0.0064(11) 0.0015(10) 0.0074(11) C25 0.0275(13) 0.0293(13) 0.0336(14) 0.0030(11) -0.0058(11) -0.0051(11) C26 0.0208(13) 0.0500(17) 0.0387(16) 0.0180(13) 0.0038(11) -0.0021(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 W C1 1.997(2) . ? W C4 2.035(2) . ? W C2 2.037(2) . ? W C3 2.041(3) . ? W C5 2.046(3) . ? W P1 2.5257(6) . ? P1 N 1.7473(18) . ? P1 C20 1.829(2) . ? P1 P2 2.2577(8) . ? P2 C13 1.846(2) . ? P2 C6 1.861(2) . ? Si1 C8 1.864(2) . ? Si1 C7 1.866(2) . ? Si1 C9 1.866(2) . ? Si1 C6 1.916(2) . ? Si2 C10 1.857(2) . ? Si2 C11 1.870(2) . ? Si2 C12 1.874(2) . ? Si2 C6 1.915(2) . ? Si3 C21 1.863(2) . ? Si3 C23 1.866(2) . ? Si3 C22 1.867(2) . ? Si3 C20 1.909(2) . ? Si4 C26 1.868(2) . ? Si4 C24 1.873(2) . ? Si4 C25 1.873(2) . ? Si4 C20 1.909(2) . ? N C13 1.304(3) . ? O1 C1 1.155(3) . ? O2 C2 1.144(3) . ? O3 C3 1.150(3) . ? O4 C4 1.150(3) . ? O5 C5 1.143(3) . ? C13 C14 1.471(3) . ? C14 C19 1.393(3) . ? C14 C15 1.395(3) . ? C15 C16 1.384(3) . ? C16 C17 1.380(4) . ? C17 C18 1.375(4) . ? C18 C19 1.393(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 W C4 88.28(9) . . ? C1 W C2 88.38(9) . . ? C4 W C2 175.21(9) . . ? C1 W C3 89.97(9) . . ? C4 W C3 87.88(9) . . ? C2 W C3 88.69(10) . . ? C1 W C5 88.22(9) . . ? C4 W C5 94.73(9) . . ? C2 W C5 88.60(9) . . ? C3 W C5 176.78(9) . . ? C1 W P1 174.22(6) . . ? C4 W P1 96.79(7) . . ? C2 W P1 86.72(7) . . ? C3 W P1 92.98(7) . . ? C5 W P1 88.60(7) . . ? N P1 C20 107.11(9) . . ? N P1 P2 78.51(6) . . ? C20 P1 P2 105.72(7) . . ? N P1 W 110.89(6) . . ? C20 P1 W 114.16(7) . . ? P2 P1 W 132.89(3) . . ? C13 P2 C6 115.86(9) . . ? C13 P2 P1 69.92(7) . . ? C6 P2 P1 117.58(7) . . ? C8 Si1 C7 106.98(10) . . ? C8 Si1 C9 107.07(11) . . ? C7 Si1 C9 109.96(11) . . ? C8 Si1 C6 110.86(10) . . ? C7 Si1 C6 111.18(10) . . ? C9 Si1 C6 110.65(10) . . ? C10 Si2 C11 108.41(11) . . ? C10 Si2 C12 105.51(11) . . ? C11 Si2 C12 110.25(10) . . ? C10 Si2 C6 113.09(10) . . ? C11 Si2 C6 112.45(10) . . ? C12 Si2 C6 106.91(10) . . ? C21 Si3 C23 106.83(11) . . ? C21 Si3 C22 110.90(11) . . ? C23 Si3 C22 108.68(11) . . ? C21 Si3 C20 109.59(10) . . ? C23 Si3 C20 107.37(10) . . ? C22 Si3 C20 113.20(10) . . ? C26 Si4 C24 105.39(11) . . ? C26 Si4 C25 109.42(12) . . ? C24 Si4 C25 109.61(11) . . ? C26 Si4 C20 108.31(10) . . ? C24 Si4 C20 111.24(10) . . ? C25 Si4 C20 112.59(10) . . ? C13 N P1 101.26(14) . . ? O1 C1 W 178.6(2) . . ? O2 C2 W 177.4(2) . . ? O3 C3 W 177.6(2) . . ? O4 C4 W 175.8(2) . . ? O5 C5 W 176.2(2) . . ? P2 C6 Si2 122.29(11) . . ? P2 C6 Si1 106.10(10) . . ? Si2 C6 Si1 114.35(11) . . ? N C13 C14 122.30(19) . . ? N C13 P2 107.80(15) . . ? C14 C13 P2 128.77(17) . . ? C19 C14 C15 119.5(2) . . ? C19 C14 C13 121.1(2) . . ? C15 C14 C13 119.4(2) . . ? C16 C15 C14 119.9(2) . . ? C17 C16 C15 120.2(2) . . ? C18 C17 C16 120.7(2) . . ? C17 C18 C19 119.7(3) . . ? C14 C19 C18 120.1(2) . . ? P1 C20 Si3 116.17(11) . . ? P1 C20 Si4 113.05(11) . . ? Si3 C20 Si4 115.86(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.769 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.088 # end of cif file