# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Scheschkewitz, David' _publ_contact_author_email d.scheschkewitz@imperial.ac.uk _publ_section_title ; Synthesis, Characterisation and Complexation of Phosphino Disilenes ; loop_ _publ_author_name M.Hartmann A.Haji-Abdi K.Abersfelder A.White P.Haycock ; D.Scheschkewitz ; data_sad _database_code_depnum_ccdc_archive 'CCDC 768711' #TrackingRef '- Compound_2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-Dicyclohexylphosphino-1,2,2-tris(2',4',6'-triisopropylphenyl)disilene ; _chemical_name_common ;1-Dicyclohexylphosphino-1,2,2-tris(2',4',6'- triisopropylphenyl)disilene ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H91 P Si2' _chemical_formula_weight 863.45 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' 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)/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 20.8212(12) _cell_length_b 10.5035(6) _cell_length_c 26.2637(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.6030(10) _cell_angle_gamma 90.00 _cell_volume 5582.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6871 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_max 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828286 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details SADABS _exptl_special_details ; Explanation for PLATON Alerts (for other alerts see REFINE and GEOM SPECIAL DETAILS): ABSTM02 ALERT 3C: Both alerts refer to the Tmin value given by PLAT061 ALERT 3C SADABS. The crystal measured was slightly too big for the beam, which may have resulted in the unrealistic ratio. The weakly diffracting nature of the crystals, however, required a large crystal in order to get diffraction to sufficiently large 2theta angles. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 42316 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9822 _reflns_number_gt 9336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material Pov-Ray _refine_special_details ; Explanation for PLATON Alerts: PLAT220 ALERT 2B: These alerts are due to unaccounted disorder PLAT222 ALERT 3B of the triisopropylphenylgroups, that is PLAT241 ALERT 2C commonly observed for this substituent and PLAT242 ALERT 2C cannot be modeled in a reasonable way. PLAT301 ALERT 3C PLAT340 ALERT 3C ; _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^)+(0.0352P)^2^+8.3621P] 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 9822 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.25758(4) 0.27997(9) 0.46973(3) 0.0283(2) Uani 1 1 d . A . Si2 Si 0.26946(4) 0.26690(8) 0.55329(3) 0.02215(19) Uani 1 1 d . . . P1 P 0.35608(5) 0.29155(11) 0.44976(4) 0.0439(3) Uani 1 1 d . . . C1 C 0.17348(14) 0.3016(3) 0.42328(11) 0.0264(6) Uani 1 1 d . . . C2 C 0.13195(17) 0.4047(3) 0.42710(13) 0.0374(8) Uani 1 1 d . A . C3 C 0.06857(17) 0.4067(3) 0.39525(13) 0.0397(8) Uani 1 1 d . . . H3A H 0.0405 0.4764 0.3981 0.048 Uiso 1 1 calc R A . C4 C 0.04450(16) 0.3118(3) 0.35954(12) 0.0367(8) Uani 1 1 d . A . C5 C 0.08675(16) 0.2128(3) 0.35488(12) 0.0343(7) Uani 1 1 d . . . H5A H 0.0715 0.1473 0.3300 0.041 Uiso 1 1 calc R A . C6 C 0.15053(15) 0.2067(3) 0.38552(11) 0.0302(7) Uani 1 1 d . A . C7 C 0.1537(2) 0.5167(3) 0.46393(15) 0.0504(10) Uani 1 1 d . . . H7A H 0.2008 0.5020 0.4824 0.061 Uiso 1 1 calc R A . C8 C 0.1141(3) 0.5257(5) 0.50539(18) 0.0725(14) Uani 1 1 d . A . H8A H 0.1184 0.4460 0.5253 0.109 Uiso 1 1 calc R . . H8B H 0.0674 0.5404 0.4885 0.109 Uiso 1 1 calc R . . H8C H 0.1307 0.5964 0.5291 0.109 Uiso 1 1 calc R . . C9 C 0.1507(3) 0.6425(4) 0.4337(2) 0.0765(15) Uani 1 1 d . A . H9A H 0.1739 0.6328 0.4055 0.115 Uiso 1 1 calc R . . H9B H 0.1718 0.7100 0.4576 0.115 Uiso 1 1 calc R . . H9C H 0.1044 0.6651 0.4186 0.115 Uiso 1 1 calc R . . C10 C -0.02669(17) 0.3095(4) 0.32741(15) 0.0477(9) Uani 1 1 d . . . H10A H -0.0276 0.2554 0.2959 0.057 Uiso 1 1 calc R A . C11 C -0.07052(19) 0.2439(4) 0.35902(18) 0.0603(11) Uani 1 1 d . A . H11A H -0.0531 0.1587 0.3695 0.091 Uiso 1 1 calc R . . H11B H -0.1157 0.2366 0.3374 0.091 Uiso 1 1 calc R . . H11C H -0.0708 0.2943 0.3903 0.091 Uiso 1 1 calc R . . C12 C -0.05343(19) 0.4381(4) 0.30779(17) 0.0610(12) Uani 1 1 d . A . H12A H -0.0229 0.4795 0.2897 0.092 Uiso 1 1 calc R . . H12B H -0.0582 0.4909 0.3375 0.092 Uiso 1 1 calc R . . H12C H -0.0966 0.4278 0.2834 0.092 Uiso 1 1 calc R . . C13 C 0.19340(16) 0.0949(3) 0.37745(12) 0.0339(7) Uani 1 1 d . . . H13A H 0.2398 0.1167 0.3958 0.041 Uiso 1 1 calc R A . C14 C 0.1760(2) -0.0271(4) 0.40200(16) 0.0509(10) Uani 1 1 d . A . H14A H 0.1824 -0.0151 0.4399 0.076 Uiso 1 1 calc R . . H14B H 0.2047 -0.0961 0.3954 0.076 Uiso 1 1 calc R . . H14C H 0.1298 -0.0491 0.3866 0.076 Uiso 1 1 calc R . . C15 C 0.1934(2) 0.0722(4) 0.32010(14) 0.0547(11) Uani 1 1 d . A . H15A H 0.2032 0.1522 0.3043 0.082 Uiso 1 1 calc R . . H15B H 0.1499 0.0411 0.3014 0.082 Uiso 1 1 calc R . . H15C H 0.2271 0.0088 0.3178 0.082 Uiso 1 1 calc R . . C16 C 0.20175(14) 0.2534(3) 0.59073(11) 0.0252(6) Uani 1 1 d . . . C17 C 0.20928(14) 0.3237(3) 0.63759(11) 0.0282(7) Uani 1 1 d . . . C18 C 0.16721(15) 0.3025(3) 0.67016(12) 0.0325(7) Uani 1 1 d . . . H18A H 0.1736 0.3494 0.7019 0.039 Uiso 1 1 calc R . . C19 C 0.11616(15) 0.2156(3) 0.65849(13) 0.0353(8) Uani 1 1 d . . . C20 C 0.10705(15) 0.1520(3) 0.61122(13) 0.0354(8) Uani 1 1 d . . . H20A H 0.0711 0.0942 0.6018 0.042 Uiso 1 1 calc R . . C21 C 0.14792(15) 0.1688(3) 0.57695(12) 0.0297(7) Uani 1 1 d . . . C22 C 0.26186(15) 0.4259(3) 0.65376(13) 0.0332(7) Uani 1 1 d . . . H22A H 0.2878 0.4292 0.6262 0.040 Uiso 1 1 calc R . . C23 C 0.23127(19) 0.5579(4) 0.65614(16) 0.0495(10) Uani 1 1 d . . . H23A H 0.2018 0.5778 0.6221 0.074 Uiso 1 1 calc R . . H23B H 0.2664 0.6219 0.6645 0.074 Uiso 1 1 calc R . . H23C H 0.2060 0.5584 0.6833 0.074 Uiso 1 1 calc R . . C24 C 0.31032(17) 0.3947(4) 0.70576(13) 0.0441(9) Uani 1 1 d . . . H24A H 0.3301 0.3109 0.7033 0.066 Uiso 1 1 calc R . . H24B H 0.2867 0.3938 0.7339 0.066 Uiso 1 1 calc R . . H24C H 0.3452 0.4593 0.7133 0.066 Uiso 1 1 calc R . . C25 C 0.07442(17) 0.1894(4) 0.69769(14) 0.0441(9) Uani 1 1 d . . . H25A H 0.0769 0.2670 0.7201 0.053 Uiso 1 1 calc R . . C26 C 0.1036(2) 0.0815(5) 0.73327(17) 0.0670(13) Uani 1 1 d . . . H26A H 0.0794 0.0720 0.7608 0.101 Uiso 1 1 calc R . . H26B H 0.1502 0.0997 0.7492 0.101 Uiso 1 1 calc R . . H26C H 0.1003 0.0025 0.7130 0.101 Uiso 1 1 calc R . . C27 C 0.0033(2) 0.1674(6) 0.67292(18) 0.0836(17) Uani 1 1 d . . . H27A H -0.0214 0.1583 0.7002 0.125 Uiso 1 1 calc R . . H27B H -0.0014 0.0895 0.6518 0.125 Uiso 1 1 calc R . . H27C H -0.0142 0.2398 0.6504 0.125 Uiso 1 1 calc R . . C28 C 0.13122(15) 0.0942(3) 0.52610(12) 0.0344(7) Uani 1 1 d . . . H28A H 0.1661 0.1132 0.5067 0.041 Uiso 1 1 calc R . . C29 C 0.13078(19) -0.0498(3) 0.53453(14) 0.0452(9) Uani 1 1 d . . . H29A H 0.1746 -0.0776 0.5540 0.068 Uiso 1 1 calc R . . H29B H 0.1195 -0.0929 0.5005 0.068 Uiso 1 1 calc R . . H29C H 0.0980 -0.0712 0.5545 0.068 Uiso 1 1 calc R . . C30 C 0.06521(18) 0.1377(4) 0.49178(14) 0.0491(10) Uani 1 1 d . . . H30A H 0.0668 0.2295 0.4855 0.074 Uiso 1 1 calc R . . H30B H 0.0298 0.1193 0.5096 0.074 Uiso 1 1 calc R . . H30C H 0.0566 0.0922 0.4583 0.074 Uiso 1 1 calc R . . C31 C 0.35210(13) 0.2344(3) 0.59974(11) 0.0222(6) Uani 1 1 d . . . C32 C 0.40346(14) 0.3251(3) 0.61273(11) 0.0245(6) Uani 1 1 d . . . C33 C 0.45434(14) 0.3055(3) 0.65712(12) 0.0293(7) Uani 1 1 d . . . H33A H 0.4884 0.3675 0.6660 0.035 Uiso 1 1 calc R . . C34 C 0.45722(15) 0.2000(3) 0.68869(12) 0.0292(7) Uani 1 1 d . . . C35 C 0.40972(15) 0.1063(3) 0.67310(12) 0.0284(7) Uani 1 1 d . . . H35A H 0.4128 0.0298 0.6929 0.034 Uiso 1 1 calc R . . C36 C 0.35775(14) 0.1211(3) 0.62943(11) 0.0246(6) Uani 1 1 d . . . C37 C 0.40639(15) 0.4447(3) 0.58067(12) 0.0293(7) Uani 1 1 d . . . H37A H 0.3674 0.4438 0.5500 0.035 Uiso 1 1 calc R . . C38 C 0.46875(17) 0.4461(4) 0.55959(14) 0.0417(8) Uani 1 1 d . . . H38A H 0.4707 0.3680 0.5396 0.063 Uiso 1 1 calc R . . H38B H 0.5077 0.4509 0.5889 0.063 Uiso 1 1 calc R . . H38C H 0.4678 0.5202 0.5368 0.063 Uiso 1 1 calc R . . C39 C 0.4034(2) 0.5671(3) 0.61129(15) 0.0469(9) Uani 1 1 d . . . H39A H 0.3614 0.5706 0.6220 0.070 Uiso 1 1 calc R . . H39B H 0.4067 0.6406 0.5891 0.070 Uiso 1 1 calc R . . H39C H 0.4401 0.5686 0.6424 0.070 Uiso 1 1 calc R . . C40 C 0.50766(16) 0.1888(3) 0.74060(13) 0.0379(8) Uani 1 1 d . . . H40A H 0.5097 0.0976 0.7518 0.045 Uiso 1 1 calc R . . C41 C 0.57706(17) 0.2301(4) 0.73850(16) 0.0573(11) Uani 1 1 d . . . H41A H 0.5915 0.1812 0.7115 0.086 Uiso 1 1 calc R . . H41B H 0.6074 0.2147 0.7726 0.086 Uiso 1 1 calc R . . H41C H 0.5769 0.3211 0.7301 0.086 Uiso 1 1 calc R . . C42 C 0.48416(19) 0.2676(4) 0.78172(13) 0.0495(10) Uani 1 1 d . . . H42A H 0.4407 0.2370 0.7847 0.074 Uiso 1 1 calc R . . H42B H 0.4808 0.3573 0.7712 0.074 Uiso 1 1 calc R . . H42C H 0.5158 0.2591 0.8156 0.074 Uiso 1 1 calc R . . C43 C 0.30906(15) 0.0117(3) 0.61400(12) 0.0285(7) Uani 1 1 d . . . H43A H 0.2741 0.0403 0.5831 0.034 Uiso 1 1 calc R . . C44 C 0.34317(18) -0.1042(3) 0.59694(15) 0.0442(9) Uani 1 1 d . . . H44A H 0.3653 -0.0791 0.5694 0.066 Uiso 1 1 calc R . . H44B H 0.3102 -0.1700 0.5834 0.066 Uiso 1 1 calc R . . H44C H 0.3759 -0.1379 0.6270 0.066 Uiso 1 1 calc R . . C45 C 0.27468(17) -0.0247(3) 0.65727(14) 0.0412(8) Uani 1 1 d . . . H45A H 0.2516 0.0497 0.6668 0.062 Uiso 1 1 calc R . . H45B H 0.3076 -0.0544 0.6880 0.062 Uiso 1 1 calc R . . H45C H 0.2427 -0.0929 0.6447 0.062 Uiso 1 1 calc R . . C46 C 0.37243(17) 0.1341(4) 0.42322(13) 0.0442(9) Uani 1 1 d . A . H46A H 0.3380 0.1181 0.3902 0.053 Uiso 1 1 calc R . . C47 C 0.3697(2) 0.0274(4) 0.46135(17) 0.0582(11) Uani 1 1 d . . . H47A H 0.3252 0.0245 0.4687 0.070 Uiso 1 1 calc R A . H47B H 0.4023 0.0438 0.4948 0.070 Uiso 1 1 calc R . . C48 C 0.3846(3) -0.0996(5) 0.4393(2) 0.0804(15) Uani 1 1 d . A . H48A H 0.3489 -0.1205 0.4082 0.096 Uiso 1 1 calc R . . H48B H 0.3854 -0.1668 0.4658 0.096 Uiso 1 1 calc R . . C49 C 0.4507(3) -0.0985(6) 0.4236(2) 0.0917(19) Uani 1 1 d . . . H49A H 0.4871 -0.0915 0.4554 0.110 Uiso 1 1 calc R A . H49B H 0.4562 -0.1798 0.4060 0.110 Uiso 1 1 calc R . . C50 C 0.4548(2) 0.0114(6) 0.3871(2) 0.0858(17) Uani 1 1 d . A . H50A H 0.4996 0.0141 0.3803 0.103 Uiso 1 1 calc R . . H50B H 0.4227 -0.0023 0.3532 0.103 Uiso 1 1 calc R . . C51 C 0.44042(19) 0.1365(5) 0.41001(17) 0.0648(13) Uani 1 1 d . . . H51A H 0.4415 0.2057 0.3846 0.078 Uiso 1 1 calc R A . H51B H 0.4749 0.1542 0.4422 0.078 Uiso 1 1 calc R . . C52 C 0.3482(3) 0.3953(5) 0.39343(19) 0.0423(13) Uani 0.816(8) 1 d P A 1 H52A H 0.3935 0.4056 0.3872 0.051 Uiso 0.816(8) 1 calc PR A 1 C53 C 0.3259(4) 0.5271(6) 0.4071(2) 0.0542(16) Uani 0.816(8) 1 d P A 1 H53A H 0.2821 0.5204 0.4154 0.065 Uiso 0.816(8) 1 calc PR A 1 H53B H 0.3576 0.5601 0.4385 0.065 Uiso 0.816(8) 1 calc PR A 1 C54 C 0.3218(4) 0.6196(5) 0.3617(2) 0.074(2) Uani 0.816(8) 1 d P A 1 H54A H 0.3033 0.7014 0.3703 0.088 Uiso 0.816(8) 1 calc PR A 1 H54B H 0.3669 0.6362 0.3571 0.088 Uiso 0.816(8) 1 calc PR A 1 C55 C 0.2795(6) 0.5694(11) 0.3110(4) 0.072(3) Uani 0.816(8) 1 d P A 1 H55A H 0.2330 0.5642 0.3140 0.086 Uiso 0.816(8) 1 calc PR A 1 H55B H 0.2812 0.6299 0.2824 0.086 Uiso 0.816(8) 1 calc PR A 1 C56 C 0.3012(7) 0.4404(13) 0.2969(5) 0.058(2) Uani 0.816(8) 1 d P A 1 H56A H 0.3455 0.4469 0.2894 0.070 Uiso 0.816(8) 1 calc PR A 1 H56B H 0.2700 0.4086 0.2650 0.070 Uiso 0.816(8) 1 calc PR A 1 C57 C 0.3037(3) 0.3474(5) 0.34194(17) 0.0459(14) Uani 0.816(8) 1 d P A 1 H57A H 0.3204 0.2642 0.3329 0.055 Uiso 0.816(8) 1 calc PR A 1 H57B H 0.2584 0.3344 0.3468 0.055 Uiso 0.816(8) 1 calc PR A 1 C52A C 0.3066(12) 0.4008(16) 0.3795(7) 0.026(5) Uani 0.184(8) 1 d P A 2 H52B H 0.2639 0.3566 0.3640 0.031 Uiso 0.184(8) 1 calc PR A 2 C57A C 0.3445(13) 0.404(3) 0.3389(10) 0.061(8) Uani 0.184(8) 1 d P A 2 H57C H 0.3892 0.4367 0.3547 0.074 Uiso 0.184(8) 1 calc PR A 2 H57D H 0.3496 0.3150 0.3275 0.074 Uiso 0.184(8) 1 calc PR A 2 C54A C 0.2545(16) 0.609(2) 0.3432(10) 0.065(9) Uani 0.184(8) 1 d P A 2 H54C H 0.2106 0.5694 0.3292 0.078 Uiso 0.184(8) 1 calc PR A 2 H54D H 0.2470 0.6974 0.3531 0.078 Uiso 0.184(8) 1 calc PR A 2 C53A C 0.2894(13) 0.536(3) 0.3927(9) 0.041(6) Uani 0.184(8) 1 d P A 2 H53C H 0.3304 0.5814 0.4099 0.050 Uiso 0.184(8) 1 calc PR A 2 H53D H 0.2603 0.5327 0.4175 0.050 Uiso 0.184(8) 1 calc PR A 2 C55A C 0.291(3) 0.611(5) 0.301(2) 0.073(12) Uani 0.184(8) 1 d P A 2 H55C H 0.3280 0.6716 0.3106 0.088 Uiso 0.184(8) 1 calc PR A 2 H55D H 0.2608 0.6403 0.2682 0.088 Uiso 0.184(8) 1 calc PR A 2 C56A C 0.317(3) 0.478(6) 0.294(2) 0.058(11) Uani 0.184(8) 1 d P A 2 H56D H 0.2798 0.4286 0.2719 0.069 Uiso 0.184(8) 1 calc PR A 2 H56C H 0.3507 0.4871 0.2732 0.069 Uiso 0.184(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0264(4) 0.0381(5) 0.0204(4) 0.0008(4) 0.0051(3) -0.0023(4) Si2 0.0222(4) 0.0243(4) 0.0203(4) 0.0011(3) 0.0057(3) 0.0006(3) P1 0.0388(5) 0.0640(7) 0.0344(5) -0.0171(5) 0.0198(4) -0.0162(5) C1 0.0275(15) 0.0284(16) 0.0215(14) 0.0081(12) 0.0023(12) -0.0003(13) C2 0.0421(19) 0.0332(18) 0.0342(18) 0.0049(15) 0.0033(15) 0.0012(15) C3 0.045(2) 0.0323(18) 0.0401(19) 0.0076(15) 0.0054(16) 0.0119(15) C4 0.0354(18) 0.043(2) 0.0297(17) 0.0124(15) 0.0032(14) -0.0003(15) C5 0.0384(18) 0.0353(18) 0.0268(16) 0.0031(14) 0.0028(13) -0.0042(15) C6 0.0327(16) 0.0347(18) 0.0224(15) 0.0064(13) 0.0051(12) -0.0049(14) C7 0.056(2) 0.034(2) 0.052(2) -0.0028(17) -0.0058(19) 0.0132(17) C8 0.092(4) 0.061(3) 0.056(3) -0.016(2) 0.001(3) 0.022(3) C9 0.092(4) 0.034(2) 0.089(4) 0.002(2) -0.007(3) 0.001(2) C10 0.0368(19) 0.059(2) 0.043(2) 0.0056(18) 0.0008(16) 0.0047(18) C11 0.039(2) 0.068(3) 0.071(3) 0.011(2) 0.0070(19) 0.002(2) C12 0.039(2) 0.082(3) 0.058(3) 0.021(2) 0.0052(19) 0.021(2) C13 0.0319(17) 0.0401(19) 0.0288(16) -0.0050(14) 0.0057(13) -0.0015(14) C14 0.059(2) 0.038(2) 0.058(2) -0.0059(18) 0.019(2) 0.0052(18) C15 0.054(2) 0.073(3) 0.036(2) -0.014(2) 0.0085(17) 0.008(2) C16 0.0240(14) 0.0253(15) 0.0279(15) 0.0072(12) 0.0098(12) 0.0058(12) C17 0.0270(15) 0.0324(17) 0.0258(15) 0.0004(13) 0.0077(12) 0.0087(13) C18 0.0320(16) 0.0402(19) 0.0272(16) -0.0034(14) 0.0105(13) 0.0044(14) C19 0.0309(17) 0.044(2) 0.0339(17) 0.0044(15) 0.0132(14) 0.0081(15) C20 0.0269(16) 0.0411(19) 0.0400(19) 0.0059(15) 0.0113(14) -0.0017(14) C21 0.0280(16) 0.0332(17) 0.0293(16) 0.0047(13) 0.0096(13) 0.0012(13) C22 0.0327(17) 0.0329(18) 0.0368(18) -0.0083(14) 0.0138(14) 0.0010(14) C23 0.046(2) 0.040(2) 0.065(3) -0.0127(19) 0.0174(19) 0.0030(17) C24 0.0377(19) 0.055(2) 0.040(2) -0.0144(17) 0.0103(16) -0.0021(17) C25 0.0390(19) 0.055(2) 0.044(2) 0.0027(18) 0.0215(16) 0.0010(17) C26 0.072(3) 0.080(3) 0.061(3) 0.025(2) 0.039(2) 0.007(3) C27 0.045(2) 0.152(5) 0.063(3) 0.018(3) 0.031(2) -0.001(3) C28 0.0307(16) 0.044(2) 0.0304(17) -0.0007(15) 0.0106(13) -0.0124(15) C29 0.047(2) 0.044(2) 0.045(2) -0.0077(17) 0.0114(17) -0.0100(17) C30 0.044(2) 0.062(3) 0.038(2) 0.0058(18) 0.0026(16) -0.0173(19) C31 0.0223(14) 0.0230(15) 0.0222(14) -0.0016(12) 0.0068(11) 0.0033(12) C32 0.0260(15) 0.0249(15) 0.0240(14) -0.0028(12) 0.0084(12) 0.0038(12) C33 0.0244(15) 0.0295(17) 0.0331(16) -0.0055(13) 0.0049(13) -0.0027(13) C34 0.0284(15) 0.0276(16) 0.0303(16) -0.0010(13) 0.0039(13) 0.0047(13) C35 0.0320(16) 0.0247(16) 0.0291(16) 0.0037(13) 0.0082(13) 0.0063(13) C36 0.0253(15) 0.0256(15) 0.0244(15) -0.0036(12) 0.0089(12) 0.0027(12) C37 0.0315(16) 0.0271(16) 0.0275(16) 0.0026(13) 0.0037(13) -0.0030(13) C38 0.0375(18) 0.047(2) 0.042(2) 0.0059(17) 0.0125(15) -0.0099(16) C39 0.067(3) 0.0267(18) 0.050(2) 0.0037(16) 0.0202(19) -0.0026(17) C40 0.0356(18) 0.0335(18) 0.0376(19) 0.0061(15) -0.0054(14) -0.0002(15) C41 0.0317(19) 0.075(3) 0.055(2) 0.002(2) -0.0086(17) 0.0017(19) C42 0.048(2) 0.062(3) 0.0314(18) 0.0022(18) -0.0039(16) 0.0002(19) C43 0.0326(16) 0.0233(15) 0.0274(16) 0.0045(12) 0.0029(13) 0.0003(13) C44 0.048(2) 0.0297(18) 0.052(2) -0.0071(16) 0.0052(17) 0.0005(16) C45 0.0419(19) 0.040(2) 0.0405(19) 0.0080(16) 0.0071(16) -0.0091(16) C46 0.0346(18) 0.068(3) 0.0315(18) -0.0152(18) 0.0115(15) 0.0019(18) C47 0.053(2) 0.069(3) 0.056(3) -0.005(2) 0.021(2) 0.009(2) C48 0.088(4) 0.077(4) 0.080(3) -0.008(3) 0.027(3) 0.023(3) C49 0.080(4) 0.114(5) 0.082(4) -0.014(4) 0.019(3) 0.048(3) C50 0.063(3) 0.128(5) 0.076(3) -0.008(3) 0.036(3) 0.038(3) C51 0.040(2) 0.106(4) 0.053(2) -0.007(3) 0.0201(19) 0.008(2) C52 0.039(3) 0.055(3) 0.037(3) -0.002(2) 0.016(2) -0.014(3) C53 0.066(4) 0.048(3) 0.048(3) -0.003(3) 0.011(3) -0.021(4) C54 0.096(5) 0.049(3) 0.078(4) 0.005(3) 0.024(4) -0.019(3) C55 0.094(6) 0.065(7) 0.055(5) 0.024(4) 0.016(5) -0.011(5) C56 0.067(7) 0.068(7) 0.044(4) 0.005(4) 0.023(4) -0.013(4) C57 0.055(3) 0.055(3) 0.032(3) 0.000(2) 0.018(2) -0.012(3) C52A 0.039(13) 0.026(9) 0.018(9) -0.006(7) 0.017(9) -0.021(9) C57A 0.062(16) 0.068(17) 0.065(17) -0.009(13) 0.037(14) -0.004(14) C54A 0.11(2) 0.033(12) 0.058(16) 0.029(11) 0.034(16) 0.020(13) C53A 0.045(14) 0.051(14) 0.031(12) -0.020(10) 0.016(11) -0.035(13) C55A 0.09(3) 0.07(3) 0.07(2) 0.02(2) 0.043(19) 0.01(2) C56A 0.06(2) 0.08(4) 0.040(16) 0.01(2) 0.012(15) -0.019(19) _geom_special_details ; Explanation for geometry related alerts: PLAT601 ALERT 2C: The Solvent Accesible Void of 32 A**3 is insufficiently big for any solvent. PLAT722 ALERT 1C: The deviation of both angles is small and therefore probably due to rounding errors of PLATON. We checked the angles with XP and foudn that our values are correct. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.898(3) . ? Si1 Si2 2.1542(11) . ? Si1 P1 2.2367(12) . ? Si2 C31 1.892(3) . ? Si2 C16 1.904(3) . ? P1 C52 1.814(5) . ? P1 C46 1.857(4) . ? P1 C52A 2.21(2) . ? C1 C2 1.404(4) . ? C1 C6 1.408(4) . ? C2 C3 1.387(5) . ? C2 C7 1.523(5) . ? C3 C4 1.380(5) . ? C3 H3A 0.9500 . ? C4 C5 1.386(5) . ? C4 C10 1.524(5) . ? C5 C6 1.383(4) . ? C5 H5A 0.9500 . ? C6 C13 1.520(4) . ? C7 C8 1.516(6) . ? C7 C9 1.535(6) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.505(6) . ? C10 C11 1.534(5) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.517(5) . ? C13 C15 1.525(4) . ? C13 H13A 1.0000 . ? 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 1.409(4) . ? C16 C17 1.412(4) . ? C17 C18 1.379(4) . ? C17 C22 1.520(4) . ? C18 C19 1.380(5) . ? C18 H18A 0.9500 . ? C19 C20 1.383(5) . ? C19 C25 1.520(4) . ? C20 C21 1.388(4) . ? C20 H20A 0.9500 . ? C21 C28 1.517(4) . ? C22 C24 1.531(5) . ? C22 C23 1.533(5) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.489(6) . ? C25 C26 1.503(6) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.526(5) . ? C28 C29 1.529(5) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.413(4) . ? C31 C36 1.413(4) . ? C32 C33 1.394(4) . ? C32 C37 1.522(4) . ? C33 C34 1.377(4) . ? C33 H33A 0.9500 . ? C34 C35 1.387(4) . ? C34 C40 1.517(4) . ? C35 C36 1.388(4) . ? C35 H35A 0.9500 . ? C36 C43 1.523(4) . ? C37 C39 1.525(5) . ? C37 C38 1.527(4) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.522(5) . ? C40 C42 1.530(5) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C45 1.527(4) . ? C43 C44 1.529(4) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.513(6) . ? C46 C51 1.535(5) . ? C46 H46A 1.0000 . ? C47 C48 1.515(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.527(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.516(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.505(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.529(8) . ? C52 C57 1.533(7) . ? C52 H52A 1.0000 . ? C53 C54 1.524(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.509(14) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.50(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.525(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C52A C57A 1.47(3) . ? C52A C53A 1.52(3) . ? C52A H52B 1.0000 . ? C57A C56A 1.42(7) . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C54A C55A 1.47(5) . ? C54A C53A 1.54(4) . ? C54A H54C 0.9900 . ? C54A H54D 0.9900 . ? C53A H53C 0.9900 . ? C53A H53D 0.9900 . ? C55A C56A 1.53(9) . ? C55A H55C 0.9900 . ? C55A H55D 0.9900 . ? C56A H56D 0.9900 . ? C56A H56C 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 Si1 Si2 122.01(10) . . ? C1 Si1 P1 126.95(10) . . ? Si2 Si1 P1 110.51(5) . . ? C31 Si2 C16 108.97(12) . . ? C31 Si2 Si1 122.52(9) . . ? C16 Si2 Si1 127.53(10) . . ? C52 P1 C46 102.6(2) . . ? C46 P1 C52A 103.9(5) . . ? C52 P1 Si1 108.2(2) . . ? C46 P1 Si1 107.39(12) . . ? C52A P1 Si1 87.2(6) . . ? C2 C1 C6 118.9(3) . . ? C2 C1 Si1 122.5(2) . . ? C6 C1 Si1 118.5(2) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 118.0(3) . . ? C1 C2 C7 123.1(3) . . ? C4 C3 C2 122.8(3) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C10 122.6(3) . . ? C5 C4 C10 119.6(3) . . ? C6 C5 C4 121.7(3) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 119.9(3) . . ? C5 C6 C13 118.0(3) . . ? C1 C6 C13 122.1(3) . . ? C8 C7 C2 112.0(4) . . ? C8 C7 C9 110.8(4) . . ? C2 C7 C9 111.5(3) . . ? C8 C7 H7A 107.4 . . ? C2 C7 H7A 107.4 . . ? C9 C7 H7A 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C4 114.1(3) . . ? C12 C10 C11 111.7(3) . . ? C4 C10 C11 109.4(3) . . ? C12 C10 H10A 107.1 . . ? C4 C10 H10A 107.1 . . ? C11 C10 H10A 107.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C6 112.8(3) . . ? C14 C13 C15 110.1(3) . . ? C6 C13 C15 113.3(3) . . ? C14 C13 H13A 106.8 . . ? C6 C13 H13A 106.8 . . ? C15 C13 H13A 106.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.2(3) . . ? C21 C16 Si2 123.7(2) . . ? C17 C16 Si2 117.9(2) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 C22 117.5(3) . . ? C16 C17 C22 122.5(3) . . ? C17 C18 C19 122.5(3) . . ? C17 C18 H18A 118.7 . . ? C19 C18 H18A 118.7 . . ? C18 C19 C20 117.0(3) . . ? C18 C19 C25 120.2(3) . . ? C20 C19 C25 122.8(3) . . ? C19 C20 C21 123.1(3) . . ? C19 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? C20 C21 C16 119.1(3) . . ? C20 C21 C28 117.2(3) . . ? C16 C21 C28 123.8(3) . . ? C17 C22 C24 112.2(3) . . ? C17 C22 C23 111.8(3) . . ? C24 C22 C23 110.5(3) . . ? C17 C22 H22A 107.4 . . ? C24 C22 H22A 107.4 . . ? C23 C22 H22A 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 111.7(4) . . ? C27 C25 C19 113.6(3) . . ? C26 C25 C19 110.2(3) . . ? C27 C25 H25A 107.0 . . ? C26 C25 H25A 107.0 . . ? C19 C25 H25A 107.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C30 110.7(3) . . ? C21 C28 C29 113.1(3) . . ? C30 C28 C29 110.3(3) . . ? C21 C28 H28A 107.5 . . ? C30 C28 H28A 107.5 . . ? C29 C28 H28A 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 118.4(3) . . ? C32 C31 Si2 123.8(2) . . ? C36 C31 Si2 116.9(2) . . ? C33 C32 C31 119.1(3) . . ? C33 C32 C37 117.6(3) . . ? C31 C32 C37 123.4(3) . . ? C34 C33 C32 122.6(3) . . ? C34 C33 H33A 118.7 . . ? C32 C33 H33A 118.7 . . ? C33 C34 C35 117.8(3) . . ? C33 C34 C40 121.7(3) . . ? C35 C34 C40 120.4(3) . . ? C34 C35 C36 121.8(3) . . ? C34 C35 H35A 119.1 . . ? C36 C35 H35A 119.1 . . ? C35 C36 C31 119.9(3) . . ? C35 C36 C43 118.4(3) . . ? C31 C36 C43 121.7(3) . . ? C32 C37 C39 113.1(2) . . ? C32 C37 C38 110.9(3) . . ? C39 C37 C38 109.1(3) . . ? C32 C37 H37A 107.9 . . ? C39 C37 H37A 107.9 . . ? C38 C37 H37A 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 C41 114.1(3) . . ? C34 C40 C42 108.9(3) . . ? C41 C40 C42 109.6(3) . . ? C34 C40 H40A 108.0 . . ? C41 C40 H40A 108.0 . . ? C42 C40 H40A 108.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C36 C43 C45 113.0(3) . . ? C36 C43 C44 110.7(3) . . ? C45 C43 C44 110.5(3) . . ? C36 C43 H43A 107.5 . . ? C45 C43 H43A 107.5 . . ? C44 C43 H43A 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 110.0(3) . . ? C47 C46 P1 111.9(2) . . ? C51 C46 P1 109.3(3) . . ? C47 C46 H46A 108.5 . . ? C51 C46 H46A 108.5 . . ? P1 C46 H46A 108.5 . . ? C46 C47 C48 110.9(4) . . ? C46 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? C47 C48 C49 112.1(5) . . ? C47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C50 C49 C48 111.4(4) . . ? C50 C49 H49A 109.3 . . ? C48 C49 H49A 109.3 . . ? C50 C49 H49B 109.3 . . ? C48 C49 H49B 109.3 . . ? H49A C49 H49B 108.0 . . ? C51 C50 C49 111.5(4) . . ? C51 C50 H50A 109.3 . . ? C49 C50 H50A 109.3 . . ? C51 C50 H50B 109.3 . . ? C49 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? C50 C51 C46 111.0(4) . . ? C50 C51 H51A 109.4 . . ? C46 C51 H51A 109.4 . . ? C50 C51 H51B 109.4 . . ? C46 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C53 C52 C57 110.5(5) . . ? C53 C52 P1 109.1(3) . . ? C57 C52 P1 116.2(4) . . ? C53 C52 H52A 106.8 . . ? C57 C52 H52A 106.8 . . ? P1 C52 H52A 106.8 . . ? C54 C53 C52 111.0(5) . . ? C54 C53 H53A 109.4 . . ? C52 C53 H53A 109.4 . . ? C54 C53 H53B 109.4 . . ? C52 C53 H53B 109.4 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 112.4(5) . . ? C55 C54 H54A 109.1 . . ? C53 C54 H54A 109.1 . . ? C55 C54 H54B 109.1 . . ? C53 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 112.6(10) . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55B 109.1 . . ? C54 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C55 C56 C57 110.1(9) . . ? C55 C56 H56A 109.6 . . ? C57 C56 H56A 109.6 . . ? C55 C56 H56B 109.6 . . ? C57 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C56 C57 C52 112.1(6) . . ? C56 C57 H57A 109.2 . . ? C52 C57 H57A 109.2 . . ? C56 C57 H57B 109.2 . . ? C52 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C57A C52A C53A 110.0(17) . . ? C57A C52A P1 113.0(18) . . ? C53A C52A P1 112.4(13) . . ? C57A C52A H52B 107.0 . . ? C53A C52A H52B 107.0 . . ? P1 C52A H52B 107.0 . . ? C56A C57A C52A 116(3) . . ? C56A C57A H57C 108.4 . . ? C52A C57A H57C 108.4 . . ? C56A C57A H57D 108.4 . . ? C52A C57A H57D 108.4 . . ? H57C C57A H57D 107.4 . . ? C55A C54A C53A 115(3) . . ? C55A C54A H54C 108.6 . . ? C53A C54A H54C 108.6 . . ? C55A C54A H54D 108.6 . . ? C53A C54A H54D 108.6 . . ? H54C C54A H54D 107.6 . . ? C52A C53A C54A 111.1(18) . . ? C52A C53A H53C 109.4 . . ? C54A C53A H53C 109.4 . . ? C52A C53A H53D 109.4 . . ? C54A C53A H53D 109.4 . . ? H53C C53A H53D 108.0 . . ? C54A C55A C56A 110(3) . . ? C54A C55A H55C 109.7 . . ? C56A C55A H55C 109.7 . . ? C54A C55A H55D 109.7 . . ? C56A C55A H55D 109.7 . . ? H55C C55A H55D 108.2 . . ? C57A C56A C55A 119(5) . . ? C57A C56A H56D 107.6 . . ? C55A C56A H56D 107.6 . . ? C57A C56A H56C 107.6 . . ? C55A C56A H56C 107.6 . . ? H56D C56A H56C 107.1 . . ? 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 C1 Si1 Si2 C31 175.82(16) . . . . ? P1 Si1 Si2 C31 -11.96(13) . . . . ? C1 Si1 Si2 C16 8.40(18) . . . . ? P1 Si1 Si2 C16 -179.38(12) . . . . ? C1 Si1 P1 C52 27.0(2) . . . . ? Si2 Si1 P1 C52 -144.74(18) . . . . ? C1 Si1 P1 C46 -83.10(18) . . . . ? Si2 Si1 P1 C46 105.16(13) . . . . ? C1 Si1 P1 C52A 20.5(5) . . . . ? Si2 Si1 P1 C52A -151.2(4) . . . . ? Si2 Si1 C1 C2 57.6(3) . . . . ? P1 Si1 C1 C2 -113.3(2) . . . . ? Si2 Si1 C1 C6 -118.7(2) . . . . ? P1 Si1 C1 C6 70.4(3) . . . . ? C6 C1 C2 C3 3.0(5) . . . . ? Si1 C1 C2 C3 -173.3(2) . . . . ? C6 C1 C2 C7 -175.6(3) . . . . ? Si1 C1 C2 C7 8.0(5) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C7 C2 C3 C4 178.3(3) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? C2 C3 C4 C10 175.5(3) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C10 C4 C5 C6 -176.0(3) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? C4 C5 C6 C13 -179.7(3) . . . . ? C2 C1 C6 C5 -3.4(4) . . . . ? Si1 C1 C6 C5 173.1(2) . . . . ? C2 C1 C6 C13 177.5(3) . . . . ? Si1 C1 C6 C13 -6.0(4) . . . . ? C3 C2 C7 C8 65.1(4) . . . . ? C1 C2 C7 C8 -116.2(4) . . . . ? C3 C2 C7 C9 -59.7(5) . . . . ? C1 C2 C7 C9 119.0(4) . . . . ? C3 C4 C10 C12 39.9(5) . . . . ? C5 C4 C10 C12 -142.9(3) . . . . ? C3 C4 C10 C11 -86.1(4) . . . . ? C5 C4 C10 C11 91.2(4) . . . . ? C5 C6 C13 C14 -76.6(4) . . . . ? C1 C6 C13 C14 102.4(4) . . . . ? C5 C6 C13 C15 49.2(4) . . . . ? C1 C6 C13 C15 -131.7(3) . . . . ? C31 Si2 C16 C21 -122.2(3) . . . . ? Si1 Si2 C16 C21 46.6(3) . . . . ? C31 Si2 C16 C17 51.8(3) . . . . ? Si1 Si2 C16 C17 -139.4(2) . . . . ? C21 C16 C17 C18 4.3(4) . . . . ? Si2 C16 C17 C18 -170.1(2) . . . . ? C21 C16 C17 C22 -174.5(3) . . . . ? Si2 C16 C17 C22 11.2(4) . . . . ? C16 C17 C18 C19 -1.3(5) . . . . ? C22 C17 C18 C19 177.5(3) . . . . ? C17 C18 C19 C20 -2.0(5) . . . . ? C17 C18 C19 C25 175.6(3) . . . . ? C18 C19 C20 C21 2.4(5) . . . . ? C25 C19 C20 C21 -175.2(3) . . . . ? C19 C20 C21 C16 0.6(5) . . . . ? C19 C20 C21 C28 -179.1(3) . . . . ? C17 C16 C21 C20 -3.9(4) . . . . ? Si2 C16 C21 C20 170.1(2) . . . . ? C17 C16 C21 C28 175.7(3) . . . . ? Si2 C16 C21 C28 -10.3(4) . . . . ? C18 C17 C22 C24 62.3(4) . . . . ? C16 C17 C22 C24 -118.9(3) . . . . ? C18 C17 C22 C23 -62.5(4) . . . . ? C16 C17 C22 C23 116.3(3) . . . . ? C18 C19 C25 C27 143.1(4) . . . . ? C20 C19 C25 C27 -39.3(5) . . . . ? C18 C19 C25 C26 -90.6(4) . . . . ? C20 C19 C25 C26 86.9(4) . . . . ? C20 C21 C28 C30 65.5(4) . . . . ? C16 C21 C28 C30 -114.1(3) . . . . ? C20 C21 C28 C29 -58.8(4) . . . . ? C16 C21 C28 C29 121.5(3) . . . . ? C16 Si2 C31 C32 -116.8(2) . . . . ? Si1 Si2 C31 C32 73.7(3) . . . . ? C16 Si2 C31 C36 52.0(2) . . . . ? Si1 Si2 C31 C36 -117.52(19) . . . . ? C36 C31 C32 C33 -6.1(4) . . . . ? Si2 C31 C32 C33 162.6(2) . . . . ? C36 C31 C32 C37 174.0(3) . . . . ? Si2 C31 C32 C37 -17.3(4) . . . . ? C31 C32 C33 C34 0.9(4) . . . . ? C37 C32 C33 C34 -179.2(3) . . . . ? C32 C33 C34 C35 4.5(4) . . . . ? C32 C33 C34 C40 -171.7(3) . . . . ? C33 C34 C35 C36 -4.8(4) . . . . ? C40 C34 C35 C36 171.4(3) . . . . ? C34 C35 C36 C31 -0.3(4) . . . . ? C34 C35 C36 C43 178.0(3) . . . . ? C32 C31 C36 C35 5.8(4) . . . . ? Si2 C31 C36 C35 -163.6(2) . . . . ? C32 C31 C36 C43 -172.4(3) . . . . ? Si2 C31 C36 C43 18.1(3) . . . . ? C33 C32 C37 C39 -62.1(4) . . . . ? C31 C32 C37 C39 117.7(3) . . . . ? C33 C32 C37 C38 60.8(4) . . . . ? C31 C32 C37 C38 -119.4(3) . . . . ? C33 C34 C40 C41 -44.0(4) . . . . ? C35 C34 C40 C41 139.9(3) . . . . ? C33 C34 C40 C42 78.8(4) . . . . ? C35 C34 C40 C42 -97.3(4) . . . . ? C35 C36 C43 C45 58.9(4) . . . . ? C31 C36 C43 C45 -122.8(3) . . . . ? C35 C36 C43 C44 -65.5(4) . . . . ? C31 C36 C43 C44 112.7(3) . . . . ? C52 P1 C46 C47 -170.6(3) . . . . ? C52A P1 C46 C47 -148.1(6) . . . . ? Si1 P1 C46 C47 -56.7(3) . . . . ? C52 P1 C46 C51 67.3(3) . . . . ? C52A P1 C46 C51 89.8(6) . . . . ? Si1 P1 C46 C51 -178.8(2) . . . . ? C51 C46 C47 C48 -57.1(5) . . . . ? P1 C46 C47 C48 -178.8(3) . . . . ? C46 C47 C48 C49 55.2(6) . . . . ? C47 C48 C49 C50 -53.1(6) . . . . ? C48 C49 C50 C51 53.8(6) . . . . ? C49 C50 C51 C46 -56.6(5) . . . . ? C47 C46 C51 C50 58.2(5) . . . . ? P1 C46 C51 C50 -178.6(3) . . . . ? C46 P1 C52 C53 173.0(4) . . . . ? C52A P1 C52 C53 77.2(13) . . . . ? Si1 P1 C52 C53 59.7(4) . . . . ? C46 P1 C52 C57 47.3(5) . . . . ? C52A P1 C52 C57 -48.5(13) . . . . ? Si1 P1 C52 C57 -66.0(4) . . . . ? C57 C52 C53 C54 -53.7(6) . . . . ? P1 C52 C53 C54 177.3(5) . . . . ? C52 C53 C54 C55 53.5(9) . . . . ? C53 C54 C55 C56 -54.6(10) . . . . ? C54 C55 C56 C57 54.8(11) . . . . ? C55 C56 C57 C52 -55.9(11) . . . . ? C53 C52 C57 C56 55.9(8) . . . . ? P1 C52 C57 C56 -179.1(7) . . . . ? C52 P1 C52A C57A 35.5(16) . . . . ? C46 P1 C52A C57A -53.9(17) . . . . ? Si1 P1 C52A C57A -161.1(16) . . . . ? C52 P1 C52A C53A -89.8(18) . . . . ? C46 P1 C52A C53A -179.2(12) . . . . ? Si1 P1 C52A C53A 73.6(13) . . . . ? C53A C52A C57A C56A -50(4) . . . . ? P1 C52A C57A C56A -177(3) . . . . ? C57A C52A C53A C54A 54(3) . . . . ? P1 C52A C53A C54A -179.4(16) . . . . ? C55A C54A C53A C52A -54(4) . . . . ? C53A C54A C55A C56A 45(5) . . . . ? C52A C57A C56A C55A 46(4) . . . . ? C54A C55A C56A C57A -42(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.701 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.053 _publ_section_abstract ; The treatment of disilenide Tip2Si=Si(Tip)Li (1) with P-chloro phosphines affords the potentially bidentate ligand systems, phosphanyl disilenes (2a-d; a: R = Ph, b: R = iPr, c: R = Cy, d: R = tBu). The diphenyl derivative 2a was also synthesised by reaction of the corresponding lithium phosphide with the iododisilene Tip2Si=Si(Tip)I (3), in turn accessible by oxidation of 1 with iodine. The thermal rearrangement of 2a to a 1-phospha-2,3-disilaindane via C-H insertion is reported as well as a first complexation reaction of 2a with [Pd(PCy3)2]. ; #===END # Attachment '- Compound_cis-4.cif' data_Phosphadisilaindane _database_code_depnum_ccdc_archive 'CCDC 768712' #TrackingRef '- Compound_cis-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; rac-1-Phenyl-2,2,3-tris(2',4',6'-triisopropylphenyl)- 1-phospha-2,3-disilaindane ; _chemical_name_common ;rac-1-Phenyl-2,2,3-tris(2',4',6'-triisopropylphenyl)-1- phospha-2,3-disilaindane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H79 P Si2' _chemical_formula_weight 851.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 13.5451(9) _cell_length_b 20.3454(13) _cell_length_c 19.0323(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.7800(10) _cell_angle_gamma 90.00 _cell_volume 5196.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9285 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.27 _exptl_crystal_description octahedron _exptl_crystal_colour colorless _exptl_crystal_size_min 0.37 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_max 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79106 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details SADABS _exptl_special_details ; Because of the weak diffraction of the compound with no heavy atoms a large crystal with well-defined shape was chosen that exceeded the beam size of 0.3 mm. The absorption correction by SADABS usually accounts for the undesired scattering effects, but the observed Tmin/Tmax ratio can not reflect the theoretical value anymore (ABSTM02 ALERT 3C, PLAT061 ALERT 3 C). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 40563 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9158 _reflns_number_gt 8432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material Pov-Ray _refine_special_details ; Structure was solved by direct methods. Refinement proceeded smoothly. Pronounced disorder of a para-isopropyl (C40, C41, C42) group was accounted for by refinement on split positions with the appropriate conformational restraints (PLAT860 ALERT 3G). The disorder of other isopropyl was not important enough, albeit still present (PLAT222 ALERT 3 B, PLAT 220 ALERT 3 C, PLAT301 ALERT 3 C), to warrant such measures. The alert concerning hybridization and configuration of Si1 and Si2 is raised because of the high steric strain due the bulkiness of substituents leading to abnormal angles around these atoms (PLAT322 ALERT 2C, PLAT793 ALERT 1G). The presence of an SiH bond without acceptor is totally unsurprising (PLAT420 ALERT 2C). ; _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^)+(0.0496P)^2^+4.4071P] 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 9158 _refine_ls_number_parameters 589 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1446 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.20830(5) 0.05504(3) 0.28506(3) 0.02667(16) Uani 1 1 d . . . Si2 Si 0.29796(5) 0.14147(3) 0.34703(3) 0.02577(16) Uani 1 1 d . . . P1 P 0.38614(5) 0.06700(3) 0.42257(3) 0.03067(16) Uani 1 1 d . . . C1 C 0.07844(18) 0.06421(11) 0.23349(13) 0.0294(5) Uani 1 1 d . . . C2 C 0.06313(19) 0.05834(12) 0.15847(13) 0.0324(5) Uani 1 1 d . . . C3 C -0.0320(2) 0.06477(13) 0.12180(15) 0.0399(6) Uani 1 1 d . . . H3A H -0.0407 0.0613 0.0716 0.048 Uiso 1 1 calc R . . C4 C -0.1143(2) 0.07602(14) 0.15523(15) 0.0408(6) Uani 1 1 d . . . C5 C -0.09961(19) 0.08121(14) 0.22808(15) 0.0396(6) Uani 1 1 d . . . H5A H -0.1558 0.0882 0.2521 0.048 Uiso 1 1 calc R . . C6 C -0.00579(18) 0.07659(12) 0.26795(13) 0.0323(5) Uani 1 1 d . . . C7 C 0.1465(2) 0.04227(14) 0.11538(14) 0.0415(6) Uani 1 1 d . . . H7A H 0.2098 0.0602 0.1416 0.050 Uiso 1 1 calc R . . C8 C 0.1332(2) 0.0723(2) 0.04098(15) 0.0612(9) Uani 1 1 d . . . H8A H 0.1169 0.1190 0.0439 0.092 Uiso 1 1 calc R . . H8B H 0.0789 0.0496 0.0112 0.092 Uiso 1 1 calc R . . H8C H 0.1951 0.0673 0.0202 0.092 Uiso 1 1 calc R . . C9 C 0.1582(3) -0.03208(17) 0.1107(2) 0.0663(10) Uani 1 1 d . . . H9A H 0.1712 -0.0506 0.1586 0.099 Uiso 1 1 calc R . . H9B H 0.2140 -0.0423 0.0848 0.099 Uiso 1 1 calc R . . H9C H 0.0968 -0.0512 0.0857 0.099 Uiso 1 1 calc R . . C10 C -0.2173(2) 0.08190(18) 0.11213(16) 0.0537(8) Uani 1 1 d . . . H10A H -0.2076 0.0909 0.0619 0.064 Uiso 1 1 calc R . . C11 C -0.2765(3) 0.1376(2) 0.1363(2) 0.0841(13) Uani 1 1 d . . . H11A H -0.2380 0.1784 0.1361 0.126 Uiso 1 1 calc R . . H11B H -0.2911 0.1288 0.1844 0.126 Uiso 1 1 calc R . . H11C H -0.3390 0.1421 0.1042 0.126 Uiso 1 1 calc R . . C12 C -0.2732(3) 0.0175(2) 0.1131(2) 0.0735(11) Uani 1 1 d . . . H12A H -0.2336 -0.0178 0.0956 0.110 Uiso 1 1 calc R . . H12B H -0.3372 0.0210 0.0825 0.110 Uiso 1 1 calc R . . H12C H -0.2847 0.0076 0.1617 0.110 Uiso 1 1 calc R . . C13 C -0.00156(19) 0.08612(13) 0.34757(14) 0.0363(6) Uani 1 1 d . . . H13A H 0.0700 0.0854 0.3691 0.044 Uiso 1 1 calc R . . C14 C -0.0460(2) 0.15216(15) 0.36566(16) 0.0464(7) Uani 1 1 d . . . H14A H -0.0136 0.1877 0.3426 0.070 Uiso 1 1 calc R . . H14B H -0.0352 0.1587 0.4172 0.070 Uiso 1 1 calc R . . H14C H -0.1177 0.1524 0.3488 0.070 Uiso 1 1 calc R . . C15 C -0.0556(2) 0.03056(15) 0.38124(16) 0.0457(7) Uani 1 1 d . . . H15A H -0.0283 -0.0119 0.3690 0.069 Uiso 1 1 calc R . . H15B H -0.1269 0.0322 0.3634 0.069 Uiso 1 1 calc R . . H15C H -0.0461 0.0358 0.4329 0.069 Uiso 1 1 calc R . . C16 C 0.21044(18) 0.20108(12) 0.38634(12) 0.0285(5) Uani 1 1 d . . . C17 C 0.16734(18) 0.25108(12) 0.34021(13) 0.0308(5) Uani 1 1 d . . . C18 C 0.10907(19) 0.29954(13) 0.36532(13) 0.0360(6) Uani 1 1 d . . . H18A H 0.0820 0.3331 0.3337 0.043 Uiso 1 1 calc R . . C19 C 0.0890(2) 0.30083(13) 0.43467(14) 0.0377(6) Uani 1 1 d . . . C20 C 0.1290(2) 0.25097(13) 0.47889(13) 0.0374(6) Uani 1 1 d . . . H20A H 0.1152 0.2505 0.5265 0.045 Uiso 1 1 calc R . . C21 C 0.18872(19) 0.20152(12) 0.45694(13) 0.0335(6) Uani 1 1 d . . . C22 C 0.1793(2) 0.25490(13) 0.26175(13) 0.0347(6) Uani 1 1 d . . . H22A H 0.2216 0.2169 0.2511 0.042 Uiso 1 1 calc R . . C23 C 0.2339(2) 0.31775(14) 0.24552(16) 0.0492(7) Uani 1 1 d . . . H23A H 0.3002 0.3183 0.2735 0.074 Uiso 1 1 calc R . . H23B H 0.1960 0.3561 0.2578 0.074 Uiso 1 1 calc R . . H23C H 0.2407 0.3191 0.1949 0.074 Uiso 1 1 calc R . . C24 C 0.0797(2) 0.24855(15) 0.21394(14) 0.0455(7) Uani 1 1 d . . . H24A H 0.0475 0.2072 0.2244 0.068 Uiso 1 1 calc R . . H24B H 0.0911 0.2488 0.1642 0.068 Uiso 1 1 calc R . . H24C H 0.0366 0.2855 0.2226 0.068 Uiso 1 1 calc R . . C25 C 0.0218(2) 0.35309(15) 0.45987(15) 0.0481(7) Uani 1 1 d . . . H25A H 0.0281 0.3502 0.5127 0.058 Uiso 1 1 calc R . . C26 C 0.0515(3) 0.42210(16) 0.4411(2) 0.0705(10) Uani 1 1 d . . . H26A H 0.0109 0.4541 0.4629 0.106 Uiso 1 1 calc R . . H26B H 0.0407 0.4276 0.3894 0.106 Uiso 1 1 calc R . . H26C H 0.1220 0.4292 0.4587 0.106 Uiso 1 1 calc R . . C27 C -0.0863(2) 0.3399(2) 0.4308(2) 0.0698(10) Uani 1 1 d . . . H27A H -0.1045 0.2955 0.4441 0.105 Uiso 1 1 calc R . . H27B H -0.0952 0.3439 0.3791 0.105 Uiso 1 1 calc R . . H27C H -0.1290 0.3720 0.4506 0.105 Uiso 1 1 calc R . . C28 C 0.2263(2) 0.14935(14) 0.51181(14) 0.0429(7) Uani 1 1 d . . . H28A H 0.2698 0.1187 0.4887 0.052 Uiso 1 1 calc R . . C29 C 0.2897(2) 0.17799(18) 0.57672(16) 0.0573(9) Uani 1 1 d . . . H29A H 0.3436 0.2044 0.5617 0.086 Uiso 1 1 calc R . . H29B H 0.3181 0.1422 0.6075 0.086 Uiso 1 1 calc R . . H29C H 0.2481 0.2058 0.6028 0.086 Uiso 1 1 calc R . . C30 C 0.1423(3) 0.10859(18) 0.53476(17) 0.0639(10) Uani 1 1 d . . . H30A H 0.1063 0.0862 0.4934 0.096 Uiso 1 1 calc R . . H30B H 0.0964 0.1374 0.5559 0.096 Uiso 1 1 calc R . . H30C H 0.1700 0.0759 0.5698 0.096 Uiso 1 1 calc R . . C31 C 0.39997(18) 0.19258(12) 0.31282(13) 0.0304(5) Uani 1 1 d . A . C32 C 0.45836(19) 0.23299(13) 0.36255(14) 0.0368(6) Uani 1 1 d . . . C33 C 0.5333(2) 0.27209(15) 0.34044(16) 0.0515(8) Uani 1 1 d D A . H33A H 0.5715 0.2997 0.3741 0.062 Uiso 1 1 calc R . . C34 C 0.5535(2) 0.27185(17) 0.27134(17) 0.0558(8) Uani 1 1 d D . . C35 C 0.4974(2) 0.23200(16) 0.22355(16) 0.0480(7) Uani 1 1 d . A . H35A H 0.5113 0.2310 0.1760 0.058 Uiso 1 1 calc R . . C36 C 0.42091(19) 0.19303(13) 0.24222(14) 0.0355(6) Uani 1 1 d . . . C37 C 0.4446(2) 0.23722(13) 0.44074(14) 0.0400(6) Uani 1 1 d . . . H37A H 0.3925 0.2044 0.4492 0.048 Uiso 1 1 calc R . . C38 C 0.4064(3) 0.30516(15) 0.45893(18) 0.0574(8) Uani 1 1 d . . . H38A H 0.3424 0.3138 0.4297 0.086 Uiso 1 1 calc R . . H38B H 0.4548 0.3387 0.4495 0.086 Uiso 1 1 calc R . . H38C H 0.3976 0.3064 0.5092 0.086 Uiso 1 1 calc R . . C39 C 0.5399(2) 0.21976(17) 0.49001(16) 0.0550(8) Uani 1 1 d . . . H39A H 0.5613 0.1753 0.4792 0.082 Uiso 1 1 calc R . . H39B H 0.5270 0.2216 0.5394 0.082 Uiso 1 1 calc R . . H39C H 0.5925 0.2512 0.4830 0.082 Uiso 1 1 calc R . . C40 C 0.6280(6) 0.3200(4) 0.2480(6) 0.087(2) Uani 0.593(18) 1 d PDU A 1 H40A H 0.6164 0.3229 0.1951 0.105 Uiso 0.593(18) 1 calc PR A 1 C41 C 0.6248(6) 0.3896(4) 0.2782(7) 0.088(2) Uani 0.593(18) 1 d PDU A 1 H41A H 0.5572 0.4074 0.2672 0.132 Uiso 0.593(18) 1 calc PR A 1 H41B H 0.6715 0.4178 0.2570 0.132 Uiso 0.593(18) 1 calc PR A 1 H41C H 0.6436 0.3883 0.3298 0.132 Uiso 0.593(18) 1 calc PR A 1 C42 C 0.7346(6) 0.2977(5) 0.2703(6) 0.087(2) Uani 0.593(18) 1 d PDU A 1 H42A H 0.7438 0.2538 0.2513 0.131 Uiso 0.593(18) 1 calc PR A 1 H42B H 0.7483 0.2965 0.3222 0.131 Uiso 0.593(18) 1 calc PR A 1 H42C H 0.7804 0.3286 0.2519 0.131 Uiso 0.593(18) 1 calc PR A 1 C40A C 0.6412(6) 0.3075(5) 0.2482(7) 0.066(3) Uani 0.407(18) 1 d PDU A 2 H40B H 0.6383 0.2927 0.1978 0.079 Uiso 0.407(18) 1 calc PR A 2 C41A C 0.6127(7) 0.3801(5) 0.2393(8) 0.066(3) Uani 0.407(18) 1 d PDU A 2 H41D H 0.5439 0.3837 0.2157 0.099 Uiso 0.407(18) 1 calc PR A 2 H41E H 0.6576 0.4020 0.2104 0.099 Uiso 0.407(18) 1 calc PR A 2 H41F H 0.6182 0.4011 0.2860 0.099 Uiso 0.407(18) 1 calc PR A 2 C42A C 0.7393(7) 0.2776(7) 0.2822(6) 0.066(3) Uani 0.407(18) 1 d PDU A 2 H42D H 0.7354 0.2296 0.2786 0.099 Uiso 0.407(18) 1 calc PR A 2 H42E H 0.7519 0.2904 0.3322 0.099 Uiso 0.407(18) 1 calc PR A 2 H42F H 0.7937 0.2935 0.2576 0.099 Uiso 0.407(18) 1 calc PR A 2 C43 C 0.3642(2) 0.15228(13) 0.18309(13) 0.0368(6) Uani 1 1 d . A . H43A H 0.3034 0.1347 0.2012 0.044 Uiso 1 1 calc R . . C44 C 0.3287(2) 0.19297(16) 0.11657(15) 0.0508(8) Uani 1 1 d . . . H44A H 0.2886 0.1652 0.0815 0.076 Uiso 1 1 calc R A . H44B H 0.3866 0.2097 0.0964 0.076 Uiso 1 1 calc R . . H44C H 0.2883 0.2300 0.1293 0.076 Uiso 1 1 calc R . . C45 C 0.4251(2) 0.09346(15) 0.16436(16) 0.0499(7) Uani 1 1 d . . . H45A H 0.4420 0.0659 0.2065 0.075 Uiso 1 1 calc R A . H45B H 0.4864 0.1089 0.1477 0.075 Uiso 1 1 calc R . . H45C H 0.3860 0.0678 0.1269 0.075 Uiso 1 1 calc R . . C46 C 0.28987(18) 0.00254(12) 0.41871(13) 0.0315(5) Uani 1 1 d . . . C47 C 0.21398(18) -0.00485(12) 0.36132(13) 0.0313(5) Uani 1 1 d . . . C48 C 0.1504(2) -0.05874(13) 0.36069(16) 0.0399(6) Uani 1 1 d . . . H48A H 0.1005 -0.0654 0.3212 0.048 Uiso 1 1 calc R . . C49 C 0.1588(2) -0.10274(14) 0.41672(18) 0.0494(8) Uani 1 1 d . . . H49A H 0.1147 -0.1391 0.4155 0.059 Uiso 1 1 calc R . . C50 C 0.2307(2) -0.09382(15) 0.47384(17) 0.0514(8) Uani 1 1 d . . . H50A H 0.2353 -0.1235 0.5127 0.062 Uiso 1 1 calc R . . C51 C 0.2964(2) -0.04190(14) 0.47515(15) 0.0432(7) Uani 1 1 d . . . H51A H 0.3465 -0.0363 0.5147 0.052 Uiso 1 1 calc R . . C52 C 0.47071(18) 0.03200(13) 0.36374(13) 0.0329(6) Uani 1 1 d . . . C53 C 0.5543(2) 0.06850(15) 0.35276(14) 0.0409(6) Uani 1 1 d . . . H53A H 0.5620 0.1121 0.3707 0.049 Uiso 1 1 calc R . . C54 C 0.6260(2) 0.04183(18) 0.31599(17) 0.0534(8) Uani 1 1 d . . . H54A H 0.6827 0.0672 0.3088 0.064 Uiso 1 1 calc R . . C55 C 0.6158(3) -0.02105(18) 0.28984(18) 0.0595(9) Uani 1 1 d . . . H55A H 0.6653 -0.0394 0.2648 0.071 Uiso 1 1 calc R . . C56 C 0.5338(2) -0.05710(16) 0.30020(18) 0.0557(8) Uani 1 1 d . . . H56A H 0.5266 -0.1006 0.2820 0.067 Uiso 1 1 calc R . . C57 C 0.4616(2) -0.03132(14) 0.33659(15) 0.0417(6) Uani 1 1 d . . . H57A H 0.4050 -0.0571 0.3432 0.050 Uiso 1 1 calc R . . H1 H 0.2698(18) 0.0287(12) 0.2413(13) 0.032(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 Si1 0.0277(3) 0.0245(3) 0.0275(3) 0.0017(3) 0.0024(3) 0.0011(3) Si2 0.0284(3) 0.0253(3) 0.0235(3) 0.0024(3) 0.0033(3) -0.0003(3) P1 0.0310(3) 0.0317(3) 0.0282(3) 0.0043(3) 0.0001(3) 0.0023(3) C1 0.0291(12) 0.0222(12) 0.0350(13) 0.0018(10) -0.0018(10) -0.0013(10) C2 0.0336(13) 0.0268(13) 0.0345(13) -0.0014(10) -0.0035(10) -0.0026(10) C3 0.0422(15) 0.0389(15) 0.0370(14) 0.0004(12) -0.0004(12) -0.0056(12) C4 0.0364(15) 0.0423(16) 0.0409(15) 0.0063(12) -0.0047(12) -0.0065(12) C5 0.0287(13) 0.0423(15) 0.0480(16) 0.0077(13) 0.0057(12) -0.0016(11) C6 0.0324(13) 0.0269(13) 0.0368(13) 0.0041(10) 0.0016(11) -0.0039(10) C7 0.0406(15) 0.0464(16) 0.0357(14) -0.0099(12) -0.0021(12) 0.0018(13) C8 0.0529(19) 0.095(3) 0.0345(16) -0.0039(17) 0.0024(14) -0.0011(18) C9 0.066(2) 0.056(2) 0.075(2) -0.0274(18) 0.0018(18) 0.0113(17) C10 0.0340(15) 0.080(2) 0.0443(17) 0.0152(16) -0.0048(13) -0.0073(15) C11 0.053(2) 0.094(3) 0.097(3) 0.018(2) -0.022(2) 0.019(2) C12 0.051(2) 0.098(3) 0.066(2) 0.003(2) -0.0113(17) -0.029(2) C13 0.0293(13) 0.0414(15) 0.0384(14) 0.0038(12) 0.0056(11) 0.0005(11) C14 0.0392(15) 0.0500(18) 0.0518(17) -0.0042(14) 0.0122(13) 0.0004(13) C15 0.0420(16) 0.0499(17) 0.0470(16) 0.0108(14) 0.0128(13) 0.0005(13) C16 0.0316(12) 0.0263(12) 0.0274(12) -0.0002(10) 0.0033(10) 0.0003(10) C17 0.0348(13) 0.0285(13) 0.0289(13) -0.0008(10) 0.0035(10) 0.0000(10) C18 0.0410(15) 0.0310(14) 0.0341(14) 0.0007(11) -0.0019(11) 0.0068(11) C19 0.0394(15) 0.0367(14) 0.0361(14) -0.0080(11) 0.0016(11) 0.0052(12) C20 0.0419(15) 0.0427(15) 0.0279(13) -0.0037(11) 0.0058(11) 0.0029(12) C21 0.0382(14) 0.0334(14) 0.0291(13) 0.0015(11) 0.0056(11) 0.0028(11) C22 0.0446(15) 0.0316(13) 0.0279(13) 0.0043(10) 0.0053(11) 0.0084(11) C23 0.066(2) 0.0386(16) 0.0441(16) 0.0107(13) 0.0125(15) 0.0017(14) C24 0.0599(18) 0.0419(16) 0.0328(14) 0.0028(12) -0.0005(13) 0.0105(14) C25 0.0492(17) 0.0561(19) 0.0371(15) -0.0103(13) -0.0003(13) 0.0190(14) C26 0.081(3) 0.0447(19) 0.087(3) -0.0203(18) 0.014(2) 0.0178(18) C27 0.050(2) 0.088(3) 0.071(2) -0.016(2) 0.0090(17) 0.0177(19) C28 0.0577(18) 0.0429(16) 0.0305(14) 0.0061(12) 0.0147(13) 0.0123(13) C29 0.0580(19) 0.074(2) 0.0385(16) 0.0177(16) 0.0019(14) 0.0115(17) C30 0.087(3) 0.063(2) 0.0413(17) 0.0177(16) 0.0083(17) -0.0124(19) C31 0.0290(12) 0.0265(12) 0.0354(13) 0.0040(10) 0.0035(10) -0.0013(10) C32 0.0361(14) 0.0305(13) 0.0425(15) 0.0057(11) 0.0004(11) -0.0023(11) C33 0.0473(17) 0.0469(18) 0.0559(19) 0.0045(14) -0.0094(14) -0.0186(14) C34 0.0457(17) 0.066(2) 0.0549(19) 0.0197(16) 0.0042(14) -0.0182(16) C35 0.0421(16) 0.0606(19) 0.0420(16) 0.0108(14) 0.0081(13) -0.0101(14) C36 0.0334(13) 0.0356(14) 0.0387(14) 0.0075(11) 0.0089(11) 0.0010(11) C37 0.0452(16) 0.0340(14) 0.0387(15) -0.0044(12) -0.0020(12) -0.0048(12) C38 0.067(2) 0.0422(18) 0.060(2) -0.0111(15) -0.0031(16) -0.0017(15) C39 0.0547(19) 0.062(2) 0.0440(17) -0.0043(15) -0.0099(14) -0.0036(16) C40 0.081(4) 0.082(4) 0.097(4) 0.036(3) 0.004(3) -0.042(3) C41 0.082(4) 0.082(4) 0.098(4) 0.036(3) 0.003(3) -0.042(3) C42 0.080(4) 0.082(4) 0.097(4) 0.036(3) 0.005(3) -0.041(3) C40A 0.041(3) 0.092(5) 0.063(5) 0.019(4) 0.005(3) -0.030(3) C41A 0.042(3) 0.092(5) 0.063(5) 0.019(4) 0.004(3) -0.030(3) C42A 0.040(3) 0.093(5) 0.064(5) 0.019(4) 0.006(3) -0.031(3) C43 0.0408(15) 0.0392(15) 0.0317(13) 0.0033(11) 0.0094(11) -0.0043(12) C44 0.063(2) 0.0563(19) 0.0327(15) 0.0050(13) 0.0037(13) -0.0060(15) C45 0.0497(18) 0.0537(19) 0.0484(17) -0.0041(14) 0.0142(14) 0.0046(14) C46 0.0318(13) 0.0305(13) 0.0334(13) 0.0065(10) 0.0086(10) 0.0058(10) C47 0.0312(13) 0.0265(13) 0.0375(14) 0.0064(10) 0.0095(11) 0.0047(10) C48 0.0357(14) 0.0313(14) 0.0535(17) 0.0060(12) 0.0090(12) 0.0001(11) C49 0.0440(17) 0.0346(15) 0.073(2) 0.0145(14) 0.0196(15) -0.0019(13) C50 0.0560(19) 0.0421(17) 0.0595(19) 0.0268(15) 0.0199(16) 0.0064(14) C51 0.0430(16) 0.0447(16) 0.0422(15) 0.0162(13) 0.0069(12) 0.0073(13) C52 0.0292(13) 0.0387(14) 0.0299(13) 0.0084(11) 0.0007(10) 0.0066(11) C53 0.0348(14) 0.0466(16) 0.0405(15) 0.0107(13) 0.0025(12) 0.0031(12) C54 0.0358(16) 0.070(2) 0.0557(19) 0.0246(17) 0.0104(14) 0.0056(15) C55 0.056(2) 0.066(2) 0.062(2) 0.0146(17) 0.0264(16) 0.0273(17) C56 0.060(2) 0.0469(18) 0.062(2) 0.0024(15) 0.0163(16) 0.0168(16) C57 0.0408(15) 0.0381(15) 0.0469(16) 0.0039(12) 0.0088(12) 0.0066(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 Si1 C47 1.889(2) . ? Si1 C1 1.904(2) . ? Si1 Si2 2.3601(9) . ? Si1 H1 1.37(2) . ? Si2 C31 1.913(2) . ? Si2 C16 1.917(2) . ? Si2 P1 2.3075(9) . ? P1 C46 1.844(3) . ? P1 C52 1.849(3) . ? C1 C6 1.413(4) . ? C1 C2 1.420(3) . ? C2 C3 1.386(4) . ? C2 C7 1.519(4) . ? C3 C4 1.375(4) . ? C3 H3A 0.9500 . ? C4 C5 1.378(4) . ? C4 C10 1.524(4) . ? C5 C6 1.392(4) . ? C5 H5A 0.9500 . ? C6 C13 1.521(4) . ? C7 C9 1.525(4) . ? C7 C8 1.530(4) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.496(5) . ? C10 C12 1.515(5) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.531(4) . ? C13 C15 1.533(4) . ? C13 H13A 1.0000 . ? 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 1.414(3) . ? C16 C17 1.417(3) . ? C17 C18 1.388(3) . ? C17 C22 1.526(3) . ? C18 C19 1.384(4) . ? C18 H18A 0.9500 . ? C19 C20 1.381(4) . ? C19 C25 1.519(4) . ? C20 C21 1.390(4) . ? C20 H20A 0.9500 . ? C21 C28 1.527(4) . ? C22 C24 1.527(4) . ? C22 C23 1.530(4) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.517(5) . ? C25 C27 1.517(4) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.519(4) . ? C28 C29 1.522(4) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.410(3) . ? C31 C32 1.412(4) . ? C32 C33 1.399(4) . ? C32 C37 1.527(4) . ? C33 C34 1.379(4) . ? C33 H33A 0.9500 . ? C34 C35 1.369(4) . ? C34 C40A 1.508(4) . ? C34 C40 1.515(4) . ? C35 C36 1.389(4) . ? C35 H35A 0.9500 . ? C36 C43 1.520(4) . ? C37 C38 1.531(4) . ? C37 C39 1.532(4) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.517(5) . ? C40 C41 1.532(5) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40A C42A 1.523(5) . ? C40A C41A 1.531(5) . ? C40A H40B 1.0000 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43 C45 1.523(4) . ? C43 C44 1.534(4) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C51 1.398(3) . ? C46 C47 1.403(4) . ? C47 C48 1.394(4) . ? C48 C49 1.385(4) . ? C48 H48A 0.9500 . ? C49 C50 1.370(5) . ? C49 H49A 0.9500 . ? C50 C51 1.379(4) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C57 1.387(4) . ? C52 C53 1.393(4) . ? C53 C54 1.383(4) . ? C53 H53A 0.9500 . ? C54 C55 1.373(5) . ? C54 H54A 0.9500 . ? C55 C56 1.367(5) . ? C55 H55A 0.9500 . ? C56 C57 1.377(4) . ? C56 H56A 0.9500 . ? C57 H57A 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 C47 Si1 C1 113.46(11) . . ? C47 Si1 Si2 97.59(8) . . ? C1 Si1 Si2 124.17(8) . . ? C47 Si1 H1 104.5(11) . . ? C1 Si1 H1 108.8(10) . . ? Si2 Si1 H1 106.4(10) . . ? C31 Si2 C16 107.59(11) . . ? C31 Si2 P1 103.43(8) . . ? C16 Si2 P1 117.87(8) . . ? C31 Si2 Si1 125.56(8) . . ? C16 Si2 Si1 111.27(8) . . ? P1 Si2 Si1 90.57(3) . . ? C46 P1 C52 101.23(11) . . ? C46 P1 Si2 97.97(8) . . ? C52 P1 Si2 100.74(8) . . ? C6 C1 C2 117.7(2) . . ? C6 C1 Si1 121.72(18) . . ? C2 C1 Si1 120.61(18) . . ? C3 C2 C1 119.9(2) . . ? C3 C2 C7 117.2(2) . . ? C1 C2 C7 122.9(2) . . ? C4 C3 C2 122.6(3) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 117.6(2) . . ? C3 C4 C10 120.3(3) . . ? C5 C4 C10 122.2(3) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C13 116.3(2) . . ? C1 C6 C13 124.1(2) . . ? C2 C7 C9 109.6(3) . . ? C2 C7 C8 114.2(2) . . ? C9 C7 C8 110.0(3) . . ? C2 C7 H7A 107.6 . . ? C9 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.3(3) . . ? C11 C10 C4 112.5(3) . . ? C12 C10 C4 110.4(3) . . ? C11 C10 H10A 107.5 . . ? C12 C10 H10A 107.5 . . ? C4 C10 H10A 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C14 111.9(2) . . ? C6 C13 C15 111.5(2) . . ? C14 C13 C15 109.2(2) . . ? C6 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C15 C13 H13A 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 117.6(2) . . ? C21 C16 Si2 126.44(18) . . ? C17 C16 Si2 115.91(17) . . ? C18 C17 C16 120.2(2) . . ? C18 C17 C22 116.2(2) . . ? C16 C17 C22 123.6(2) . . ? C19 C18 C17 122.4(2) . . ? C19 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? C20 C19 C18 117.1(2) . . ? C20 C19 C25 121.6(2) . . ? C18 C19 C25 121.2(2) . . ? C19 C20 C21 123.0(2) . . ? C19 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? C20 C21 C16 119.6(2) . . ? C20 C21 C28 116.8(2) . . ? C16 C21 C28 123.5(2) . . ? C17 C22 C24 112.1(2) . . ? C17 C22 C23 111.0(2) . . ? C24 C22 C23 111.3(2) . . ? C17 C22 H22A 107.4 . . ? C24 C22 H22A 107.4 . . ? C23 C22 H22A 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 110.5(3) . . ? C26 C25 C19 112.6(3) . . ? C27 C25 C19 110.6(3) . . ? C26 C25 H25A 107.6 . . ? C27 C25 H25A 107.6 . . ? C19 C25 H25A 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 109.7(2) . . ? C30 C28 C21 112.5(2) . . ? C29 C28 C21 112.9(2) . . ? C30 C28 H28A 107.1 . . ? C29 C28 H28A 107.1 . . ? C21 C28 H28A 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.9(2) . . ? C36 C31 Si2 125.13(19) . . ? C32 C31 Si2 116.95(18) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 C37 116.8(2) . . ? C31 C32 C37 123.7(2) . . ? C34 C33 C32 122.0(3) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C35 C34 C33 118.2(2) . . ? C35 C34 C40A 118.6(6) . . ? C33 C34 C40A 122.9(6) . . ? C35 C34 C40 121.3(5) . . ? C33 C34 C40 120.2(5) . . ? C34 C35 C36 122.3(3) . . ? C34 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C35 C36 C31 120.0(2) . . ? C35 C36 C43 116.2(2) . . ? C31 C36 C43 123.7(2) . . ? C32 C37 C38 111.1(2) . . ? C32 C37 C39 112.3(2) . . ? C38 C37 C39 110.7(2) . . ? C32 C37 H37A 107.5 . . ? C38 C37 H37A 107.5 . . ? C39 C37 H37A 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 C42 111.8(6) . . ? C34 C40 C41 115.7(5) . . ? C42 C40 C41 104.2(8) . . ? C34 C40 H40A 108.3 . . ? C42 C40 H40A 108.3 . . ? C41 C40 H40A 108.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C34 C40A C42A 111.1(6) . . ? C34 C40A C41A 107.4(6) . . ? C42A C40A C41A 128.7(10) . . ? C34 C40A H40B 101.9 . . ? C42A C40A H40B 101.9 . . ? C41A C40A H40B 101.9 . . ? C40A C41A H41D 109.5 . . ? C40A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40A C42A H42D 109.5 . . ? C40A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C36 C43 C45 111.5(2) . . ? C36 C43 C44 112.8(2) . . ? C45 C43 C44 110.5(2) . . ? C36 C43 H43A 107.3 . . ? C45 C43 H43A 107.3 . . ? C44 C43 H43A 107.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 C46 C47 119.5(2) . . ? C51 C46 P1 117.3(2) . . ? C47 C46 P1 123.15(18) . . ? C48 C47 C46 118.6(2) . . ? C48 C47 Si1 122.7(2) . . ? C46 C47 Si1 118.59(18) . . ? C49 C48 C47 121.0(3) . . ? C49 C48 H48A 119.5 . . ? C47 C48 H48A 119.5 . . ? C50 C49 C48 120.1(3) . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C51 120.2(3) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C50 C51 C46 120.5(3) . . ? C50 C51 H51A 119.7 . . ? C46 C51 H51A 119.7 . . ? C57 C52 C53 118.2(2) . . ? C57 C52 P1 123.5(2) . . ? C53 C52 P1 117.9(2) . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C55 C54 C53 120.4(3) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C56 C55 C54 119.4(3) . . ? C56 C55 H55A 120.3 . . ? C54 C55 H55A 120.3 . . ? C55 C56 C57 121.0(3) . . ? C55 C56 H56A 119.5 . . ? C57 C56 H56A 119.5 . . ? C56 C57 C52 120.5(3) . . ? C56 C57 H57A 119.8 . . ? C52 C57 H57A 119.8 . . ? 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 C47 Si1 Si2 C31 135.94(12) . . . . ? C1 Si1 Si2 C31 -98.91(13) . . . . ? C47 Si1 Si2 C16 -91.45(11) . . . . ? C1 Si1 Si2 C16 33.70(13) . . . . ? C47 Si1 Si2 P1 28.92(8) . . . . ? C1 Si1 Si2 P1 154.07(10) . . . . ? C31 Si2 P1 C46 -156.09(11) . . . . ? C16 Si2 P1 C46 85.37(12) . . . . ? Si1 Si2 P1 C46 -29.19(8) . . . . ? C31 Si2 P1 C52 -52.98(12) . . . . ? C16 Si2 P1 C52 -171.52(12) . . . . ? Si1 Si2 P1 C52 73.91(9) . . . . ? C47 Si1 C1 C6 50.2(2) . . . . ? Si2 Si1 C1 C6 -67.7(2) . . . . ? C47 Si1 C1 C2 -129.39(19) . . . . ? Si2 Si1 C1 C2 112.68(18) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? Si1 C1 C2 C3 179.62(19) . . . . ? C6 C1 C2 C7 -177.4(2) . . . . ? Si1 C1 C2 C7 2.2(3) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C7 C2 C3 C4 176.7(3) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C2 C3 C4 C10 -179.3(3) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C10 C4 C5 C6 -179.3(3) . . . . ? C4 C5 C6 C1 -1.9(4) . . . . ? C4 C5 C6 C13 177.6(3) . . . . ? C2 C1 C6 C5 1.3(3) . . . . ? Si1 C1 C6 C5 -178.34(19) . . . . ? C2 C1 C6 C13 -178.2(2) . . . . ? Si1 C1 C6 C13 2.2(3) . . . . ? C3 C2 C7 C9 -90.5(3) . . . . ? C1 C2 C7 C9 86.9(3) . . . . ? C3 C2 C7 C8 33.4(4) . . . . ? C1 C2 C7 C8 -149.1(3) . . . . ? C3 C4 C10 C11 -136.3(3) . . . . ? C5 C4 C10 C11 44.2(4) . . . . ? C3 C4 C10 C12 98.7(3) . . . . ? C5 C4 C10 C12 -80.8(4) . . . . ? C5 C6 C13 C14 -56.4(3) . . . . ? C1 C6 C13 C14 123.0(3) . . . . ? C5 C6 C13 C15 66.2(3) . . . . ? C1 C6 C13 C15 -114.4(3) . . . . ? C31 Si2 C16 C21 -120.9(2) . . . . ? P1 Si2 C16 C21 -4.6(2) . . . . ? Si1 Si2 C16 C21 98.0(2) . . . . ? C31 Si2 C16 C17 56.2(2) . . . . ? P1 Si2 C16 C17 172.50(15) . . . . ? Si1 Si2 C16 C17 -84.91(19) . . . . ? C21 C16 C17 C18 2.2(4) . . . . ? Si2 C16 C17 C18 -175.08(19) . . . . ? C21 C16 C17 C22 -176.6(2) . . . . ? Si2 C16 C17 C22 6.1(3) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C22 C17 C18 C19 177.7(2) . . . . ? C17 C18 C19 C20 -0.5(4) . . . . ? C17 C18 C19 C25 -177.7(3) . . . . ? C18 C19 C20 C21 1.1(4) . . . . ? C25 C19 C20 C21 178.4(3) . . . . ? C19 C20 C21 C16 -0.1(4) . . . . ? C19 C20 C21 C28 -179.2(3) . . . . ? C17 C16 C21 C20 -1.6(4) . . . . ? Si2 C16 C21 C20 175.4(2) . . . . ? C17 C16 C21 C28 177.5(2) . . . . ? Si2 C16 C21 C28 -5.5(4) . . . . ? C18 C17 C22 C24 -61.3(3) . . . . ? C16 C17 C22 C24 117.5(3) . . . . ? C18 C17 C22 C23 63.8(3) . . . . ? C16 C17 C22 C23 -117.3(3) . . . . ? C20 C19 C25 C26 132.1(3) . . . . ? C18 C19 C25 C26 -50.8(4) . . . . ? C20 C19 C25 C27 -103.7(3) . . . . ? C18 C19 C25 C27 73.5(4) . . . . ? C20 C21 C28 C30 64.7(3) . . . . ? C16 C21 C28 C30 -114.4(3) . . . . ? C20 C21 C28 C29 -60.2(3) . . . . ? C16 C21 C28 C29 120.7(3) . . . . ? C16 Si2 C31 C36 -121.6(2) . . . . ? P1 Si2 C31 C36 113.0(2) . . . . ? Si1 Si2 C31 C36 12.4(3) . . . . ? C16 Si2 C31 C32 58.3(2) . . . . ? P1 Si2 C31 C32 -67.2(2) . . . . ? Si1 Si2 C31 C32 -167.75(16) . . . . ? C36 C31 C32 C33 0.6(4) . . . . ? Si2 C31 C32 C33 -179.2(2) . . . . ? C36 C31 C32 C37 -179.7(2) . . . . ? Si2 C31 C32 C37 0.5(3) . . . . ? C31 C32 C33 C34 -1.0(5) . . . . ? C37 C32 C33 C34 179.2(3) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C32 C33 C34 C40A -172.7(5) . . . . ? C32 C33 C34 C40 173.8(5) . . . . ? C33 C34 C35 C36 0.9(5) . . . . ? C40A C34 C35 C36 174.2(5) . . . . ? C40 C34 C35 C36 -172.5(5) . . . . ? C34 C35 C36 C31 -1.3(5) . . . . ? C34 C35 C36 C43 179.0(3) . . . . ? C32 C31 C36 C35 0.5(4) . . . . ? Si2 C31 C36 C35 -179.7(2) . . . . ? C32 C31 C36 C43 -179.8(2) . . . . ? Si2 C31 C36 C43 0.0(4) . . . . ? C33 C32 C37 C38 66.9(3) . . . . ? C31 C32 C37 C38 -112.9(3) . . . . ? C33 C32 C37 C39 -57.7(3) . . . . ? C31 C32 C37 C39 122.6(3) . . . . ? C35 C34 C40 C42 -107.4(8) . . . . ? C33 C34 C40 C42 79.3(8) . . . . ? C40A C34 C40 C42 -27(4) . . . . ? C35 C34 C40 C41 133.5(8) . . . . ? C33 C34 C40 C41 -39.8(12) . . . . ? C40A C34 C40 C41 -146(5) . . . . ? C35 C34 C40A C42A -107.5(9) . . . . ? C33 C34 C40A C42A 65.4(10) . . . . ? C40 C34 C40A C42A 146(5) . . . . ? C35 C34 C40A C41A 107.1(10) . . . . ? C33 C34 C40A C41A -79.9(11) . . . . ? C40 C34 C40A C41A 0(4) . . . . ? C35 C36 C43 C45 74.7(3) . . . . ? C31 C36 C43 C45 -104.9(3) . . . . ? C35 C36 C43 C44 -50.2(3) . . . . ? C31 C36 C43 C44 130.1(3) . . . . ? C52 P1 C46 C51 99.7(2) . . . . ? Si2 P1 C46 C51 -157.60(19) . . . . ? C52 P1 C46 C47 -78.0(2) . . . . ? Si2 P1 C46 C47 24.7(2) . . . . ? C51 C46 C47 C48 -3.4(4) . . . . ? P1 C46 C47 C48 174.24(19) . . . . ? C51 C46 C47 Si1 -179.0(2) . . . . ? P1 C46 C47 Si1 -1.3(3) . . . . ? C1 Si1 C47 C48 29.9(2) . . . . ? Si2 Si1 C47 C48 162.4(2) . . . . ? C1 Si1 C47 C46 -154.79(19) . . . . ? Si2 Si1 C47 C46 -22.3(2) . . . . ? C46 C47 C48 C49 2.7(4) . . . . ? Si1 C47 C48 C49 178.0(2) . . . . ? C47 C48 C49 C50 -0.2(4) . . . . ? C48 C49 C50 C51 -1.4(5) . . . . ? C49 C50 C51 C46 0.6(5) . . . . ? C47 C46 C51 C50 1.8(4) . . . . ? P1 C46 C51 C50 -176.0(2) . . . . ? C46 P1 C52 C57 -8.2(2) . . . . ? Si2 P1 C52 C57 -108.7(2) . . . . ? C46 P1 C52 C53 179.28(19) . . . . ? Si2 P1 C52 C53 78.82(19) . . . . ? C57 C52 C53 C54 -0.3(4) . . . . ? P1 C52 C53 C54 172.6(2) . . . . ? C52 C53 C54 C55 0.0(4) . . . . ? C53 C54 C55 C56 0.2(5) . . . . ? C54 C55 C56 C57 -0.2(5) . . . . ? C55 C56 C57 C52 -0.1(5) . . . . ? C53 C52 C57 C56 0.4(4) . . . . ? P1 C52 C57 C56 -172.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.469 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.049 _publ_section_abstract ; The treatment of disilenide Tip2Si=Si(Tip)Li (1) with P-chloro phosphines affords the potentially bidentate ligand systems, phosphanyl disilenes (2a-d; a: R = Ph, b: R = iPr, c: R = Cy, d: R = tBu). The diphenyl derivative 2a was also synthesised by reaction of the corresponding lithium phosphide with the iododisilene Tip2Si=Si(Tip)I (3), in turn accessible by oxidation of 1 with iodine. The thermal rearrangement of 2a to a 1-phospha-2,3-disilaindane via C-H insertion is reported as well as a first complexation reaction of 2a with [Pd(PCy3)2]. ; # Attachment '- Compound_3.cif' data_sad_p21c _database_code_depnum_ccdc_archive 'CCDC 768713' #TrackingRef '- Compound_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1-Iodo-1,2,2-tris(2',4',6'-triisopropylphenyl)disilene ; _chemical_name_common 1-Iodo-1,2,2-tris(2',4',6'-triisopropylphenyl)disilene _chemical_melting_point ? _chemical_formula_moiety 'C45 H69 I Si2' _chemical_formula_sum 'C45 H69 I Si2' _chemical_formula_weight 793.08 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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)/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 23.6013(19) _cell_length_b 10.7701(9) _cell_length_c 17.9227(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.941(2) _cell_angle_gamma 90.00 _cell_volume 4500.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7404 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.29 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.390 _exptl_crystal_size_min 0.210 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7165262 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 43109 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7936 _reflns_number_gt 7337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction SAINT+ _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _computing_publication_material Pov-Ray _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^)+(0.0336P)^2^+4.8614P] 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 7936 _refine_ls_number_parameters 481 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.32854(3) 0.37916(6) 0.92847(4) 0.03038(14) Uani 1 1 d . . . Si2 Si 0.25161(2) 0.49581(6) 0.91719(3) 0.02828(14) Uani 1 1 d . . . I1 I 0.371103(8) 0.36324(2) 0.812445(10) 0.05436(8) Uani 1 1 d . . . C1 C 0.38540(9) 0.3595(2) 1.01305(12) 0.0278(5) Uani 1 1 d . . . C2 C 0.41287(9) 0.4596(2) 1.05411(12) 0.0292(5) Uani 1 1 d . . . C3 C 0.45087(10) 0.4347(2) 1.12039(13) 0.0349(5) Uani 1 1 d . . . H3A H 0.4689 0.5021 1.1489 0.042 Uiso 1 1 calc R . . C4 C 0.46310(10) 0.3146(2) 1.14579(14) 0.0368(5) Uani 1 1 d . . . C5 C 0.43725(10) 0.2174(2) 1.10306(14) 0.0376(5) Uani 1 1 d . . . H5A H 0.4461 0.1347 1.1193 0.045 Uiso 1 1 calc R . . C6 C 0.39898(9) 0.2366(2) 1.03740(13) 0.0328(5) Uani 1 1 d . . . C7 C 0.40251(10) 0.5936(2) 1.02912(13) 0.0322(5) Uani 1 1 d . . . H7A H 0.3833 0.5924 0.9753 0.039 Uiso 1 1 calc R . . C8 C 0.36155(11) 0.6565(2) 1.07565(17) 0.0451(6) Uani 1 1 d . . . H8A H 0.3246 0.6129 1.0678 0.068 Uiso 1 1 calc R . . H8B H 0.3558 0.7431 1.0596 0.068 Uiso 1 1 calc R . . H8C H 0.3780 0.6536 1.1293 0.068 Uiso 1 1 calc R . . C9 C 0.45787(11) 0.6682(2) 1.03239(17) 0.0452(6) Uani 1 1 d . . . H9A H 0.4836 0.6258 1.0028 0.068 Uiso 1 1 calc R . . H9B H 0.4766 0.6754 1.0850 0.068 Uiso 1 1 calc R . . H9C H 0.4489 0.7512 1.0115 0.068 Uiso 1 1 calc R . . C10 C 0.50628(12) 0.2848(3) 1.21596(15) 0.0471(6) Uani 1 1 d . . . H10A H 0.4915 0.2105 1.2403 0.057 Uiso 1 1 calc R . . C11 C 0.51413(15) 0.3869(3) 1.27413(16) 0.0581(8) Uani 1 1 d . . . H11A H 0.4769 0.4085 1.2883 0.087 Uiso 1 1 calc R . . H11B H 0.5305 0.4601 1.2530 0.087 Uiso 1 1 calc R . . H11C H 0.5401 0.3585 1.3189 0.087 Uiso 1 1 calc R . . C12 C 0.56300(13) 0.2479(4) 1.19191(19) 0.0685(9) Uani 1 1 d . . . H12A H 0.5900 0.2221 1.2364 0.103 Uiso 1 1 calc R . . H12B H 0.5789 0.3189 1.1679 0.103 Uiso 1 1 calc R . . H12C H 0.5566 0.1789 1.1559 0.103 Uiso 1 1 calc R . . C13 C 0.37456(11) 0.1248(2) 0.99103(17) 0.0442(6) Uani 1 1 d . . . H13A H 0.3421 0.1550 0.9527 0.053 Uiso 1 1 calc R . . C14 C 0.35078(16) 0.0259(3) 1.0386(2) 0.0782(11) Uani 1 1 d . . . H14A H 0.3307 -0.0376 1.0053 0.117 Uiso 1 1 calc R . . H14B H 0.3240 0.0643 1.0683 0.117 Uiso 1 1 calc R . . H14C H 0.3824 -0.0127 1.0726 0.117 Uiso 1 1 calc R . . C15 C 0.41907(16) 0.0690(3) 0.9487(2) 0.0777(11) Uani 1 1 d . . . H15A H 0.4015 0.0028 0.9153 0.117 Uiso 1 1 calc R . . H15B H 0.4506 0.0345 0.9848 0.117 Uiso 1 1 calc R . . H15C H 0.4340 0.1335 0.9184 0.117 Uiso 1 1 calc R . . C16 C 0.20550(9) 0.5167(2) 0.99437(12) 0.0309(5) Uani 1 1 d . . . C17 C 0.20067(10) 0.4322(3) 1.05322(13) 0.0382(5) Uani 1 1 d . . . C18 C 0.15537(12) 0.4475(3) 1.09488(14) 0.0481(7) Uani 1 1 d . . . H18A H 0.1520 0.3904 1.1344 0.058 Uiso 1 1 calc R . . C19 C 0.11543(11) 0.5422(3) 1.08079(15) 0.0472(7) Uani 1 1 d . . . C20 C 0.12394(11) 0.6292(3) 1.02789(16) 0.0444(6) Uani 1 1 d . . . H20A H 0.0986 0.6982 1.0199 0.053 Uiso 1 1 calc R . . C21 C 0.16834(10) 0.6200(2) 0.98546(13) 0.0353(5) Uani 1 1 d . . . C22 C 0.24274(12) 0.3274(3) 1.07526(16) 0.0541(8) Uani 1 1 d . . . H22A H 0.2671 0.3197 1.0345 0.065 Uiso 1 1 calc R . . C23 C 0.21334(16) 0.2021(3) 1.0816(2) 0.0806(11) Uani 1 1 d . . . H23A H 0.2425 0.1368 1.0917 0.121 Uiso 1 1 calc R . . H23B H 0.1881 0.1840 1.0341 0.121 Uiso 1 1 calc R . . H23C H 0.1907 0.2051 1.1229 0.121 Uiso 1 1 calc R . . C24 C 0.28242(15) 0.3586(4) 1.1484(2) 0.0832(13) Uani 1 1 d . . . H24A H 0.3016 0.4380 1.1426 0.125 Uiso 1 1 calc R . . H24B H 0.3113 0.2931 1.1597 0.125 Uiso 1 1 calc R . . H24C H 0.2599 0.3648 1.1898 0.125 Uiso 1 1 calc R . . C25 C 0.06381(14) 0.5523(3) 1.12186(19) 0.0642(9) Uani 1 1 d . . . H25A H 0.0387 0.6160 1.0927 0.077 Uiso 1 1 calc R . . C26 C 0.02855(14) 0.4389(3) 1.1162(2) 0.0726(10) Uani 1 1 d . . . H26A H -0.0055 0.4530 1.1402 0.109 Uiso 1 1 calc R . . H26B H 0.0510 0.3703 1.1417 0.109 Uiso 1 1 calc R . . H26C H 0.0166 0.4178 1.0628 0.109 Uiso 1 1 calc R . . C27 C 0.07828(16) 0.6051(4) 1.1965(2) 0.0704(10) Uani 1 1 d . . . H27A H 0.0435 0.6132 1.2196 0.106 Uiso 1 1 calc R . . H27B H 0.0956 0.6872 1.1929 0.106 Uiso 1 1 calc R . . H27C H 0.1056 0.5507 1.2278 0.106 Uiso 1 1 calc R . . C28 C 0.17555(11) 0.7256(2) 0.93204(14) 0.0400(6) Uani 1 1 d . . . H28A H 0.2058 0.6997 0.9018 0.048 Uiso 1 1 calc R . . C29 C 0.12148(14) 0.7528(4) 0.87631(18) 0.0658(9) Uani 1 1 d . . . H29A H 0.1098 0.6780 0.8467 0.099 Uiso 1 1 calc R . . H29B H 0.1291 0.8199 0.8423 0.099 Uiso 1 1 calc R . . H29C H 0.0907 0.7780 0.9040 0.099 Uiso 1 1 calc R . . C30 C 0.19780(17) 0.8418(3) 0.97646(19) 0.0657(9) Uani 1 1 d . . . H30A H 0.2331 0.8215 1.0108 0.098 Uiso 1 1 calc R . . H30B H 0.1687 0.8715 1.0057 0.098 Uiso 1 1 calc R . . H30C H 0.2058 0.9067 0.9412 0.098 Uiso 1 1 calc R . . C31 C 0.20325(9) 0.4892(2) 0.82216(12) 0.0281(5) Uani 1 1 d . A . C32 C 0.20804(9) 0.5749(2) 0.76401(12) 0.0319(5) Uani 1 1 d . . . C33 C 0.16420(10) 0.5820(2) 0.70230(12) 0.0358(5) Uani 1 1 d . A . H33A H 0.1674 0.6409 0.6637 0.043 Uiso 1 1 calc R . . C34 C 0.11642(10) 0.5071(2) 0.69515(12) 0.0361(5) Uani 1 1 d . . . C35 C 0.11390(10) 0.4177(2) 0.75010(13) 0.0370(5) Uani 1 1 d . A . H35A H 0.0823 0.3621 0.7446 0.044 Uiso 1 1 calc R . . C36 C 0.15630(10) 0.4067(2) 0.81327(12) 0.0318(5) Uani 1 1 d . . . C37 C 0.26005(11) 0.6578(3) 0.76340(14) 0.0413(6) Uani 1 1 d . . . H37A H 0.2877 0.6400 0.8103 0.050 Uiso 1 1 calc R . . C38 C 0.24632(15) 0.7966(3) 0.7626(2) 0.0673(9) Uani 1 1 d . . . H38A H 0.2272 0.8169 0.8058 0.101 Uiso 1 1 calc R . . H38B H 0.2210 0.8175 0.7156 0.101 Uiso 1 1 calc R . . H38C H 0.2820 0.8443 0.7658 0.101 Uiso 1 1 calc R . . C39 C 0.28973(12) 0.6248(3) 0.69540(15) 0.0582(8) Uani 1 1 d . . . H39A H 0.2962 0.5350 0.6945 0.087 Uiso 1 1 calc R . . H39B H 0.3266 0.6682 0.6998 0.087 Uiso 1 1 calc R . . H39C H 0.2653 0.6501 0.6486 0.087 Uiso 1 1 calc R . . C40 C 0.0659(5) 0.5251(12) 0.6262(6) 0.0360(19) Uani 0.63(2) 1 d P A 1 H40A H 0.0773 0.5890 0.5908 0.043 Uiso 0.63(2) 1 calc PR A 1 C41 C 0.0139(4) 0.5683(12) 0.6569(6) 0.062(2) Uani 0.63(2) 1 d P A 1 H41A H -0.0174 0.5831 0.6150 0.092 Uiso 0.63(2) 1 calc PR A 1 H41B H 0.0227 0.6456 0.6852 0.092 Uiso 0.63(2) 1 calc PR A 1 H41C H 0.0022 0.5047 0.6905 0.092 Uiso 0.63(2) 1 calc PR A 1 C42 C 0.0542(7) 0.4017(12) 0.5845(8) 0.088(4) Uani 0.63(2) 1 d P A 1 H42A H 0.0884 0.3761 0.5637 0.132 Uiso 0.63(2) 1 calc PR A 1 H42B H 0.0219 0.4117 0.5433 0.132 Uiso 0.63(2) 1 calc PR A 1 H42C H 0.0447 0.3382 0.6197 0.132 Uiso 0.63(2) 1 calc PR A 1 C40A C 0.0730(11) 0.517(3) 0.6356(13) 0.053(3) Uani 0.37(2) 1 d PU A 2 H40B H 0.0778 0.6027 0.6160 0.064 Uiso 0.37(2) 1 calc PR A 2 C41A C 0.0096(7) 0.516(2) 0.6510(9) 0.055(3) Uani 0.37(2) 1 d PU A 2 H41D H 0.0056 0.5739 0.6919 0.083 Uiso 0.37(2) 1 calc PR A 2 H41E H -0.0004 0.4318 0.6658 0.083 Uiso 0.37(2) 1 calc PR A 2 H41F H -0.0161 0.5404 0.6052 0.083 Uiso 0.37(2) 1 calc PR A 2 C42A C 0.0759(6) 0.4351(16) 0.5676(7) 0.056(3) Uani 0.37(2) 1 d PU A 2 H42D H 0.0425 0.4514 0.5289 0.084 Uiso 0.37(2) 1 calc PR A 2 H42E H 0.0758 0.3477 0.5828 0.084 Uiso 0.37(2) 1 calc PR A 2 H42F H 0.1111 0.4532 0.5470 0.084 Uiso 0.37(2) 1 calc PR A 2 C43 C 0.15055(10) 0.3030(2) 0.86896(14) 0.0381(5) Uani 1 1 d . A . H43A H 0.1837 0.3100 0.9109 0.046 Uiso 1 1 calc R . . C44 C 0.09555(12) 0.3151(3) 0.90416(17) 0.0552(8) Uani 1 1 d . . . H44A H 0.0951 0.3960 0.9291 0.083 Uiso 1 1 calc R A . H44B H 0.0943 0.2488 0.9413 0.083 Uiso 1 1 calc R . . H44C H 0.0621 0.3083 0.8645 0.083 Uiso 1 1 calc R . . C45 C 0.15446(18) 0.1769(3) 0.8323(2) 0.0717(10) Uani 1 1 d . . . H45A H 0.1920 0.1682 0.8160 0.108 Uiso 1 1 calc R A . H45B H 0.1242 0.1696 0.7885 0.108 Uiso 1 1 calc R . . H45C H 0.1497 0.1115 0.8689 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0250(3) 0.0344(3) 0.0307(3) -0.0009(3) 0.0012(2) 0.0029(2) Si2 0.0217(3) 0.0388(3) 0.0241(3) 0.0046(2) 0.0025(2) 0.0013(2) I1 0.04845(12) 0.07838(15) 0.03854(11) -0.01085(9) 0.01395(8) 0.00474(9) C1 0.0215(10) 0.0303(11) 0.0315(11) 0.0010(9) 0.0041(8) 0.0020(8) C2 0.0269(11) 0.0300(11) 0.0309(11) -0.0006(9) 0.0053(9) 0.0023(9) C3 0.0362(12) 0.0332(12) 0.0332(12) -0.0029(10) -0.0010(10) -0.0014(10) C4 0.0342(12) 0.0387(13) 0.0357(13) 0.0043(10) -0.0001(10) 0.0016(10) C5 0.0360(12) 0.0302(12) 0.0448(14) 0.0081(10) 0.0004(10) 0.0025(10) C6 0.0261(11) 0.0303(12) 0.0413(13) 0.0009(10) 0.0033(9) -0.0001(9) C7 0.0340(12) 0.0280(11) 0.0331(12) -0.0021(9) 0.0008(9) 0.0009(9) C8 0.0421(14) 0.0345(13) 0.0594(17) -0.0082(12) 0.0098(12) 0.0079(11) C9 0.0435(14) 0.0351(13) 0.0573(17) 0.0034(12) 0.0087(12) -0.0043(11) C10 0.0516(16) 0.0436(15) 0.0411(14) 0.0092(12) -0.0084(12) -0.0009(12) C11 0.070(2) 0.0658(19) 0.0339(14) 0.0064(13) -0.0080(13) -0.0006(16) C12 0.0507(18) 0.082(2) 0.063(2) -0.0081(17) -0.0214(15) 0.0176(16) C13 0.0376(13) 0.0275(12) 0.0625(17) 0.0000(11) -0.0080(12) -0.0009(10) C14 0.074(2) 0.0432(18) 0.112(3) 0.0144(19) -0.003(2) -0.0215(16) C15 0.075(2) 0.056(2) 0.102(3) -0.039(2) 0.012(2) 0.0001(17) C16 0.0241(10) 0.0439(13) 0.0242(11) -0.0012(9) 0.0023(8) -0.0044(9) C17 0.0323(12) 0.0525(15) 0.0296(12) 0.0038(11) 0.0039(9) -0.0052(11) C18 0.0496(16) 0.0661(18) 0.0306(13) 0.0028(12) 0.0125(11) -0.0179(14) C19 0.0400(14) 0.0594(17) 0.0456(15) -0.0157(13) 0.0170(12) -0.0069(13) C20 0.0388(14) 0.0485(15) 0.0484(15) -0.0118(12) 0.0143(12) 0.0002(11) C21 0.0312(12) 0.0436(14) 0.0304(12) -0.0079(10) 0.0026(9) -0.0026(10) C22 0.0411(15) 0.076(2) 0.0465(16) 0.0299(15) 0.0111(12) 0.0054(14) C23 0.072(2) 0.067(2) 0.104(3) 0.042(2) 0.019(2) 0.0132(19) C24 0.0508(19) 0.135(4) 0.059(2) 0.043(2) -0.0053(16) 0.002(2) C25 0.0544(18) 0.080(2) 0.066(2) -0.0224(17) 0.0334(16) -0.0145(16) C26 0.0504(18) 0.080(2) 0.095(3) -0.028(2) 0.0341(18) -0.0194(17) C27 0.072(2) 0.081(2) 0.066(2) -0.0222(18) 0.0361(18) -0.0177(18) C28 0.0428(14) 0.0393(13) 0.0373(13) -0.0022(11) 0.0043(11) 0.0051(11) C29 0.0549(18) 0.084(2) 0.0551(18) 0.0089(17) -0.0029(14) 0.0158(17) C30 0.098(3) 0.0432(17) 0.0559(19) -0.0045(14) 0.0130(18) -0.0096(16) C31 0.0242(10) 0.0359(12) 0.0242(10) 0.0009(9) 0.0036(8) 0.0031(9) C32 0.0293(11) 0.0406(13) 0.0264(11) 0.0023(9) 0.0057(9) 0.0011(10) C33 0.0348(12) 0.0475(14) 0.0251(11) 0.0079(10) 0.0049(9) 0.0028(11) C34 0.0298(12) 0.0516(15) 0.0261(11) 0.0007(10) 0.0014(9) 0.0050(10) C35 0.0287(12) 0.0467(14) 0.0343(12) -0.0007(11) 0.0008(9) -0.0048(10) C36 0.0298(11) 0.0380(12) 0.0275(11) 0.0003(9) 0.0042(9) 0.0005(9) C37 0.0361(13) 0.0570(16) 0.0300(12) 0.0110(11) 0.0027(10) -0.0100(11) C38 0.069(2) 0.0564(19) 0.076(2) 0.0155(17) 0.0108(17) -0.0202(16) C39 0.0393(15) 0.100(3) 0.0368(14) 0.0139(15) 0.0098(12) -0.0145(15) C40 0.028(3) 0.051(4) 0.023(3) 0.011(2) -0.016(2) 0.005(3) C41 0.045(4) 0.072(6) 0.062(4) -0.005(4) -0.012(3) 0.022(4) C42 0.078(7) 0.101(7) 0.070(6) -0.038(5) -0.036(5) 0.035(5) C40A 0.037(5) 0.085(7) 0.037(5) 0.010(5) 0.001(4) 0.007(5) C41A 0.034(4) 0.089(7) 0.040(5) 0.009(5) -0.002(3) 0.005(6) C42A 0.043(5) 0.085(6) 0.036(4) 0.005(4) -0.008(4) 0.010(5) C43 0.0379(13) 0.0389(13) 0.0352(12) 0.0046(10) -0.0014(10) -0.0074(10) C44 0.0396(15) 0.076(2) 0.0492(16) 0.0171(15) 0.0047(12) -0.0155(14) C45 0.108(3) 0.0418(17) 0.062(2) 0.0023(15) 0.0018(19) -0.0006(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 Si1 C1 1.874(2) . ? Si1 Si2 2.1914(9) . ? Si1 I1 2.4520(7) . ? Si2 C31 1.898(2) . ? Si2 C16 1.902(2) . ? C1 C2 1.405(3) . ? C1 C6 1.415(3) . ? C2 C3 1.399(3) . ? C2 C7 1.520(3) . ? C3 C4 1.386(3) . ? C3 H3A 0.9500 . ? C4 C5 1.382(3) . ? C4 C10 1.525(3) . ? C5 C6 1.383(3) . ? C5 H5A 0.9500 . ? C6 C13 1.525(3) . ? C7 C9 1.527(3) . ? C7 C8 1.530(3) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.507(4) . ? C10 C12 1.522(4) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.513(4) . ? C13 C14 1.525(4) . ? C13 H13A 1.0000 . ? 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 1.410(3) . ? C16 C17 1.411(3) . ? C17 C18 1.406(4) . ? C17 C22 1.514(4) . ? C18 C19 1.385(4) . ? C18 H18A 0.9500 . ? C19 C20 1.370(4) . ? C19 C25 1.522(4) . ? C20 C21 1.391(3) . ? C20 H20A 0.9500 . ? C21 C28 1.513(4) . ? C22 C24 1.525(5) . ? C22 C23 1.530(5) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.445(4) . ? C25 C26 1.473(5) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.522(4) . ? C28 C30 1.532(4) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.410(3) . ? C31 C36 1.410(3) . ? C32 C33 1.394(3) . ? C32 C37 1.519(3) . ? C33 C34 1.376(3) . ? C33 H33A 0.9500 . ? C34 C40A 1.36(2) . ? C34 C35 1.385(3) . ? C34 C40 1.590(8) . ? C35 C36 1.395(3) . ? C35 H35A 0.9500 . ? C36 C43 1.518(3) . ? C37 C38 1.529(4) . ? C37 C39 1.539(4) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.496(16) . ? C40 C42 1.529(16) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40A C42A 1.51(3) . ? C40A C41A 1.56(3) . ? C40A H40B 1.0000 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43 C45 1.517(4) . ? C43 C44 1.535(4) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 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 Si1 Si2 128.20(7) . . ? C1 Si1 I1 110.00(7) . . ? Si2 Si1 I1 113.86(3) . . ? C31 Si2 C16 108.96(9) . . ? C31 Si2 Si1 115.81(7) . . ? C16 Si2 Si1 124.07(8) . . ? C2 C1 C6 119.5(2) . . ? C2 C1 Si1 123.45(16) . . ? C6 C1 Si1 117.04(16) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C7 119.0(2) . . ? C1 C2 C7 122.27(19) . . ? C4 C3 C2 122.1(2) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C5 C4 C3 118.2(2) . . ? C5 C4 C10 118.6(2) . . ? C3 C4 C10 123.1(2) . . ? C4 C5 C6 122.2(2) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 119.3(2) . . ? C5 C6 C13 119.1(2) . . ? C1 C6 C13 121.5(2) . . ? C2 C7 C9 113.01(19) . . ? C2 C7 C8 110.3(2) . . ? C9 C7 C8 110.8(2) . . ? C2 C7 H7A 107.5 . . ? C9 C7 H7A 107.5 . . ? C8 C7 H7A 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.6(3) . . ? C11 C10 C4 114.3(2) . . ? C12 C10 C4 109.0(2) . . ? C11 C10 H10A 107.2 . . ? C12 C10 H10A 107.2 . . ? C4 C10 H10A 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 110.3(3) . . ? C15 C13 C6 110.8(2) . . ? C14 C13 C6 112.8(3) . . ? C15 C13 H13A 107.6 . . ? C14 C13 H13A 107.6 . . ? C6 C13 H13A 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.2(2) . . ? C21 C16 Si2 115.28(17) . . ? C17 C16 Si2 126.10(18) . . ? C18 C17 C16 118.5(2) . . ? C18 C17 C22 118.1(2) . . ? C16 C17 C22 123.4(2) . . ? C19 C18 C17 122.8(3) . . ? C19 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C20 C19 C18 117.4(2) . . ? C20 C19 C25 120.0(3) . . ? C18 C19 C25 122.5(3) . . ? C19 C20 C21 122.3(3) . . ? C19 C20 H20A 118.9 . . ? C21 C20 H20A 118.9 . . ? C20 C21 C16 120.2(2) . . ? C20 C21 C28 117.4(2) . . ? C16 C21 C28 122.4(2) . . ? C17 C22 C24 110.5(3) . . ? C17 C22 C23 113.0(2) . . ? C24 C22 C23 110.9(3) . . ? C17 C22 H22A 107.4 . . ? C24 C22 H22A 107.4 . . ? C23 C22 H22A 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 116.1(3) . . ? C27 C25 C19 112.6(3) . . ? C26 C25 C19 113.2(3) . . ? C27 C25 H25A 104.5 . . ? C26 C25 H25A 104.5 . . ? C19 C25 H25A 104.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C29 113.3(2) . . ? C21 C28 C30 110.4(2) . . ? C29 C28 C30 111.6(3) . . ? C21 C28 H28A 107.1 . . ? C29 C28 H28A 107.1 . . ? C30 C28 H28A 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 118.76(19) . . ? C32 C31 Si2 122.17(17) . . ? C36 C31 Si2 118.51(16) . . ? C33 C32 C31 119.2(2) . . ? C33 C32 C37 117.6(2) . . ? C31 C32 C37 123.2(2) . . ? C34 C33 C32 122.5(2) . . ? C34 C33 H33A 118.7 . . ? C32 C33 H33A 118.7 . . ? C40A C34 C33 122.1(13) . . ? C40A C34 C35 120.1(13) . . ? C33 C34 C35 117.8(2) . . ? C33 C34 C40 120.4(5) . . ? C35 C34 C40 121.8(5) . . ? C34 C35 C36 122.1(2) . . ? C34 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C35 C36 C31 119.3(2) . . ? C35 C36 C43 118.1(2) . . ? C31 C36 C43 122.6(2) . . ? C32 C37 C38 113.8(2) . . ? C32 C37 C39 109.8(2) . . ? C38 C37 C39 109.9(2) . . ? C32 C37 H37A 107.7 . . ? C38 C37 H37A 107.7 . . ? C39 C37 H37A 107.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 110.7(9) . . ? C41 C40 C34 108.2(8) . . ? C42 C40 C34 109.4(8) . . ? C41 C40 H40A 109.5 . . ? C42 C40 H40A 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40A C42A 117.5(18) . . ? C34 C40A C41A 118.9(18) . . ? C42A C40A C41A 107.5(18) . . ? C34 C40A H40B 103.6 . . ? C42A C40A H40B 103.6 . . ? C41A C40A H40B 103.6 . . ? C40A C41A H41D 109.5 . . ? C40A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40A C42A H42D 109.5 . . ? C40A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C45 C43 C36 110.9(2) . . ? C45 C43 C44 111.5(3) . . ? C36 C43 C44 112.1(2) . . ? C45 C43 H43A 107.4 . . ? C36 C43 H43A 107.4 . . ? C44 C43 H43A 107.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 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 Si1 Si2 C31 -179.13(12) . . . . ? I1 Si1 Si2 C31 35.39(9) . . . . ? C1 Si1 Si2 C16 -39.43(13) . . . . ? I1 Si1 Si2 C16 175.09(9) . . . . ? Si2 Si1 C1 C2 -49.7(2) . . . . ? I1 Si1 C1 C2 96.79(18) . . . . ? Si2 Si1 C1 C6 127.74(16) . . . . ? I1 Si1 C1 C6 -85.74(18) . . . . ? C6 C1 C2 C3 -3.2(3) . . . . ? Si1 C1 C2 C3 174.17(17) . . . . ? C6 C1 C2 C7 177.0(2) . . . . ? Si1 C1 C2 C7 -5.6(3) . . . . ? C1 C2 C3 C4 1.4(3) . . . . ? C7 C2 C3 C4 -178.8(2) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C2 C3 C4 C10 177.3(2) . . . . ? C3 C4 C5 C6 -1.5(4) . . . . ? C10 C4 C5 C6 -178.0(2) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C4 C5 C6 C13 176.8(2) . . . . ? C2 C1 C6 C5 2.8(3) . . . . ? Si1 C1 C6 C5 -174.82(18) . . . . ? C2 C1 C6 C13 -174.3(2) . . . . ? Si1 C1 C6 C13 8.1(3) . . . . ? C3 C2 C7 C9 46.6(3) . . . . ? C1 C2 C7 C9 -133.6(2) . . . . ? C3 C2 C7 C8 -78.0(3) . . . . ? C1 C2 C7 C8 101.7(2) . . . . ? C5 C4 C10 C11 -156.8(3) . . . . ? C3 C4 C10 C11 26.9(4) . . . . ? C5 C4 C10 C12 77.5(3) . . . . ? C3 C4 C10 C12 -98.8(3) . . . . ? C5 C6 C13 C15 -74.5(3) . . . . ? C1 C6 C13 C15 102.5(3) . . . . ? C5 C6 C13 C14 49.7(3) . . . . ? C1 C6 C13 C14 -133.2(3) . . . . ? C31 Si2 C16 C21 -55.25(19) . . . . ? Si1 Si2 C16 C21 162.75(14) . . . . ? C31 Si2 C16 C17 117.1(2) . . . . ? Si1 Si2 C16 C17 -24.9(2) . . . . ? C21 C16 C17 C18 6.6(3) . . . . ? Si2 C16 C17 C18 -165.51(19) . . . . ? C21 C16 C17 C22 -171.8(2) . . . . ? Si2 C16 C17 C22 16.1(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C22 C17 C18 C19 178.2(3) . . . . ? C17 C18 C19 C20 -5.3(4) . . . . ? C17 C18 C19 C25 175.0(3) . . . . ? C18 C19 C20 C21 4.5(4) . . . . ? C25 C19 C20 C21 -175.9(2) . . . . ? C19 C20 C21 C16 1.9(4) . . . . ? C19 C20 C21 C28 -176.5(2) . . . . ? C17 C16 C21 C20 -7.5(3) . . . . ? Si2 C16 C21 C20 165.43(19) . . . . ? C17 C16 C21 C28 170.8(2) . . . . ? Si2 C16 C21 C28 -16.2(3) . . . . ? C18 C17 C22 C24 -73.8(3) . . . . ? C16 C17 C22 C24 104.6(3) . . . . ? C18 C17 C22 C23 51.1(4) . . . . ? C16 C17 C22 C23 -130.6(3) . . . . ? C20 C19 C25 C27 -100.1(4) . . . . ? C18 C19 C25 C27 79.5(4) . . . . ? C20 C19 C25 C26 125.7(3) . . . . ? C18 C19 C25 C26 -54.7(4) . . . . ? C20 C21 C28 C29 -55.4(3) . . . . ? C16 C21 C28 C29 126.2(3) . . . . ? C20 C21 C28 C30 70.6(3) . . . . ? C16 C21 C28 C30 -107.8(3) . . . . ? C16 Si2 C31 C32 120.64(19) . . . . ? Si1 Si2 C31 C32 -93.86(19) . . . . ? C16 Si2 C31 C36 -50.7(2) . . . . ? Si1 Si2 C31 C36 94.82(17) . . . . ? C36 C31 C32 C33 4.8(3) . . . . ? Si2 C31 C32 C33 -166.47(18) . . . . ? C36 C31 C32 C37 -172.8(2) . . . . ? Si2 C31 C32 C37 15.9(3) . . . . ? C31 C32 C33 C34 -1.0(4) . . . . ? C37 C32 C33 C34 176.8(2) . . . . ? C32 C33 C34 C40A 178.2(14) . . . . ? C32 C33 C34 C35 -3.2(4) . . . . ? C32 C33 C34 C40 176.1(6) . . . . ? C40A C34 C35 C36 -177.9(14) . . . . ? C33 C34 C35 C36 3.5(4) . . . . ? C40 C34 C35 C36 -175.8(6) . . . . ? C34 C35 C36 C31 0.4(4) . . . . ? C34 C35 C36 C43 -178.1(2) . . . . ? C32 C31 C36 C35 -4.5(3) . . . . ? Si2 C31 C36 C35 167.08(18) . . . . ? C32 C31 C36 C43 173.8(2) . . . . ? Si2 C31 C36 C43 -14.6(3) . . . . ? C33 C32 C37 C38 62.2(3) . . . . ? C31 C32 C37 C38 -120.2(3) . . . . ? C33 C32 C37 C39 -61.4(3) . . . . ? C31 C32 C37 C39 116.2(3) . . . . ? C33 C34 C40 C41 -114.0(9) . . . . ? C35 C34 C40 C41 65.3(10) . . . . ? C33 C34 C40 C42 125.4(11) . . . . ? C35 C34 C40 C42 -55.3(13) . . . . ? C33 C34 C40A C42A 92(2) . . . . ? C35 C34 C40A C42A -86(2) . . . . ? C33 C34 C40A C41A -135.1(18) . . . . ? C35 C34 C40A C41A 46(3) . . . . ? C35 C36 C43 C45 64.3(3) . . . . ? C31 C36 C43 C45 -114.1(3) . . . . ? C35 C36 C43 C44 -61.0(3) . . . . ? C31 C36 C43 C44 120.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.756 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.051 _publ_section_abstract ; The treatment of disilenide Tip2Si=Si(Tip)Li (1) with P-chloro phosphines affords the potentially bidentate ligand systems, phosphanyl disilenes (2a-d; a: R = Ph, b: R = iPr, c: R = Cy, d: R = tBu). The diphenyl derivative 2a was also synthesised by reaction of the corresponding lithium phosphide with the iododisilene Tip2Si=Si(Tip)I (3), in turn accessible by oxidation of 1 with iodine. The thermal rearrangement of 2a to a 1-phospha-2,3-disilaindane via C-H insertion is reported as well as a first complexation reaction of 2a with [Pd(PCy3)2]. ; # Attachment '- Compound_5a.cif' data_5a _database_code_depnum_ccdc_archive 'CCDC 769675' #TrackingRef '- Compound_5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H112 P2 Pd Si2, 1/2(C6 H14)' _chemical_formula_sum 'C78 H119 P2 Pd Si2' _chemical_formula_weight 1281.25 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' 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' Pd Pd 0.1215 3.9337 '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)/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 19.87013(7) _cell_length_b 14.06651(4) _cell_length_c 27.06129(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.9683(3) _cell_angle_gamma 90.00 _cell_volume 7425.55(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 59354 _cell_measurement_theta_min 2.2630 _cell_measurement_theta_max 72.4273 _exptl_crystal_description blocks _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_absorpt_coefficient_mu 3.016 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90750 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 72.58 _reflns_number_total 14685 _reflns_number_gt 13722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0412P)^2^+2.1811P] 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 0.000234(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14685 _refine_ls_number_parameters 771 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.063 _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 Pd Pd 0.258382(5) 0.359771(7) 0.341560(4) 0.02378(4) Uani 1 1 d . . . Si1 Si 0.208567(18) 0.50904(3) 0.354635(13) 0.02192(8) Uani 1 1 d . . . Si2 Si 0.292177(18) 0.50234(2) 0.308774(13) 0.02092(8) Uani 1 1 d . . . P1 P 0.097730(18) 0.52108(3) 0.314422(13) 0.02627(8) Uani 1 1 d . . . P2 P 0.259876(19) 0.18726(2) 0.326788(14) 0.02686(8) Uani 1 1 d . . . C1 C 0.22431(7) 0.54465(10) 0.42417(5) 0.0243(3) Uani 1 1 d . . . C2 C 0.24775(9) 0.63571(10) 0.44212(6) 0.0300(3) Uani 1 1 d . . . C3 C 0.25933(10) 0.65524(11) 0.49351(6) 0.0361(4) Uani 1 1 d . . . H3A H 0.2745 0.7170 0.5047 0.043 Uiso 1 1 calc R . . C4 C 0.24954(9) 0.58778(11) 0.52896(6) 0.0348(3) Uani 1 1 d . . . C5 C 0.22552(8) 0.49981(11) 0.51124(6) 0.0303(3) Uani 1 1 d . . . H5A H 0.2176 0.4530 0.5348 0.036 Uiso 1 1 calc R . . C6 C 0.21236(7) 0.47658(10) 0.46020(5) 0.0246(3) Uani 1 1 d . . . C7 C 0.26102(10) 0.71674(11) 0.40797(6) 0.0397(4) Uani 1 1 d . . . H7A H 0.2565 0.6909 0.3731 0.048 Uiso 1 1 calc R . . C8 C 0.20702(14) 0.79487(13) 0.40696(8) 0.0582(6) Uani 1 1 d . . . H8A H 0.1611 0.7674 0.3967 0.087 Uiso 1 1 calc R . . H8B H 0.2140 0.8443 0.3829 0.087 Uiso 1 1 calc R . . H8C H 0.2114 0.8229 0.4406 0.087 Uiso 1 1 calc R . . C9 C 0.33341(13) 0.75681(14) 0.42372(7) 0.0552(5) Uani 1 1 d . . . H9A H 0.3669 0.7056 0.4241 0.083 Uiso 1 1 calc R . . H9B H 0.3386 0.7846 0.4574 0.083 Uiso 1 1 calc R . . H9C H 0.3411 0.8059 0.3997 0.083 Uiso 1 1 calc R . . C10 C 0.26620(11) 0.60741(13) 0.58506(6) 0.0459(4) Uani 1 1 d . . . H10A H 0.2522 0.5501 0.6025 0.055 Uiso 1 1 calc R . . C11 C 0.22646(11) 0.69138(15) 0.59976(7) 0.0524(5) Uani 1 1 d . . . H11A H 0.1773 0.6812 0.5876 0.079 Uiso 1 1 calc R . . H11B H 0.2409 0.7495 0.5847 0.079 Uiso 1 1 calc R . . H11C H 0.2355 0.6977 0.6365 0.079 Uiso 1 1 calc R . . C12 C 0.34261(13) 0.62102(18) 0.60340(8) 0.0647(6) Uani 1 1 d . . . H12A H 0.3517 0.6336 0.6397 0.097 Uiso 1 1 calc R . . H12B H 0.3585 0.6750 0.5858 0.097 Uiso 1 1 calc R . . H12C H 0.3670 0.5633 0.5966 0.097 Uiso 1 1 calc R . . C13 C 0.18883(8) 0.37462(10) 0.44788(5) 0.0286(3) Uani 1 1 d . . . H13A H 0.1748 0.3690 0.4105 0.034 Uiso 1 1 calc R . . C14 C 0.12742(9) 0.34648(13) 0.47144(7) 0.0404(4) Uani 1 1 d . . . H14A H 0.1144 0.2806 0.4624 0.061 Uiso 1 1 calc R . . H14B H 0.0887 0.3887 0.4588 0.061 Uiso 1 1 calc R . . H14C H 0.1399 0.3521 0.5081 0.061 Uiso 1 1 calc R . . C15 C 0.24836(9) 0.30649(11) 0.46506(6) 0.0380(4) Uani 1 1 d . . . H15A H 0.2873 0.3251 0.4498 0.057 Uiso 1 1 calc R . . H15B H 0.2342 0.2417 0.4546 0.057 Uiso 1 1 calc R . . H15C H 0.2618 0.3089 0.5018 0.057 Uiso 1 1 calc R . . C16 C 0.37212(7) 0.57077(10) 0.33884(5) 0.0251(3) Uani 1 1 d . . . C17 C 0.42024(8) 0.53808(11) 0.38083(5) 0.0295(3) Uani 1 1 d . . . C18 C 0.47893(8) 0.59158(12) 0.39876(6) 0.0354(3) Uani 1 1 d . . . H18A H 0.5111 0.5684 0.4267 0.042 Uiso 1 1 calc R . . C19 C 0.49204(8) 0.67772(13) 0.37709(6) 0.0360(4) Uani 1 1 d . . . C20 C 0.44416(8) 0.71006(11) 0.33655(6) 0.0331(3) Uani 1 1 d . . . H20A H 0.4522 0.7688 0.3213 0.040 Uiso 1 1 calc R . . C21 C 0.38466(8) 0.65953(11) 0.31728(5) 0.0276(3) Uani 1 1 d . . . C22 C 0.41040(8) 0.44757(12) 0.40952(6) 0.0353(3) Uani 1 1 d . . . H22A H 0.3678 0.4157 0.3914 0.042 Uiso 1 1 calc R . . C23 C 0.39982(9) 0.47133(14) 0.46266(6) 0.0416(4) Uani 1 1 d . . . H23A H 0.3617 0.5163 0.4607 0.062 Uiso 1 1 calc R . . H23B H 0.4417 0.4999 0.4819 0.062 Uiso 1 1 calc R . . H23C H 0.3892 0.4130 0.4795 0.062 Uiso 1 1 calc R . . C24 C 0.46973(11) 0.37736(13) 0.41176(7) 0.0460(4) Uani 1 1 d . . . H24A H 0.4760 0.3627 0.3775 0.069 Uiso 1 1 calc R . . H24B H 0.4594 0.3187 0.4284 0.069 Uiso 1 1 calc R . . H24C H 0.5119 0.4057 0.4308 0.069 Uiso 1 1 calc R . . C25 C 0.55603(10) 0.73450(14) 0.39793(6) 0.0462(5) Uani 1 1 d . . . H25A H 0.5568 0.7911 0.3757 0.055 Uiso 1 1 calc R . . C26 C 0.55423(11) 0.77072(14) 0.45057(7) 0.0511(5) Uani 1 1 d . . . H26A H 0.5120 0.8071 0.4500 0.077 Uiso 1 1 calc R . . H26B H 0.5940 0.8118 0.4621 0.077 Uiso 1 1 calc R . . H26C H 0.5555 0.7167 0.4736 0.077 Uiso 1 1 calc R . . C27 C 0.62098(11) 0.6777(2) 0.39741(9) 0.0701(7) Uani 1 1 d . . . H27A H 0.6210 0.6551 0.3632 0.105 Uiso 1 1 calc R . . H27B H 0.6226 0.6231 0.4201 0.105 Uiso 1 1 calc R . . H27C H 0.6611 0.7182 0.4086 0.105 Uiso 1 1 calc R . . C28 C 0.33620(8) 0.70325(10) 0.27241(6) 0.0299(3) Uani 1 1 d . . . H28A H 0.2943 0.6624 0.2652 0.036 Uiso 1 1 calc R . . C29 C 0.31298(10) 0.80409(12) 0.28287(7) 0.0416(4) Uani 1 1 d . . . H29A H 0.2925 0.8035 0.3131 0.062 Uiso 1 1 calc R . . H29B H 0.2790 0.8263 0.2541 0.062 Uiso 1 1 calc R . . H29C H 0.3526 0.8469 0.2881 0.062 Uiso 1 1 calc R . . C30 C 0.36837(9) 0.70324(12) 0.22521(6) 0.0369(3) Uani 1 1 d . . . H30A H 0.3831 0.6386 0.2188 0.055 Uiso 1 1 calc R . . H30B H 0.4081 0.7459 0.2304 0.055 Uiso 1 1 calc R . . H30C H 0.3345 0.7252 0.1963 0.055 Uiso 1 1 calc R . . C31 C 0.29674(7) 0.48480(9) 0.23915(5) 0.0228(3) Uani 1 1 d . . . C32 C 0.35807(7) 0.44753(10) 0.22759(5) 0.0257(3) Uani 1 1 d . . . C33 C 0.36719(8) 0.44593(11) 0.17754(5) 0.0295(3) Uani 1 1 d . . . H33A H 0.4090 0.4220 0.1704 0.035 Uiso 1 1 calc R . . C34 C 0.31759(8) 0.47786(11) 0.13814(5) 0.0301(3) Uani 1 1 d . . . C35 C 0.25630(8) 0.50999(11) 0.14947(5) 0.0295(3) Uani 1 1 d . . . H35A H 0.2209 0.5303 0.1228 0.035 Uiso 1 1 calc R . . C36 C 0.24484(7) 0.51356(10) 0.19866(5) 0.0248(3) Uani 1 1 d . . . C37 C 0.41583(8) 0.40575(11) 0.26678(6) 0.0311(3) Uani 1 1 d . . . H37A H 0.4009 0.4074 0.3000 0.037 Uiso 1 1 calc R . . C38 C 0.48244(8) 0.46290(15) 0.27200(7) 0.0438(4) Uani 1 1 d . . . H38A H 0.4736 0.5293 0.2798 0.066 Uiso 1 1 calc R . . H38B H 0.4995 0.4600 0.2403 0.066 Uiso 1 1 calc R . . H38C H 0.5168 0.4360 0.2992 0.066 Uiso 1 1 calc R . . C39 C 0.42828(10) 0.30159(13) 0.25460(7) 0.0421(4) Uani 1 1 d . . . H39A H 0.3852 0.2660 0.2514 0.063 Uiso 1 1 calc R . . H39B H 0.4624 0.2741 0.2818 0.063 Uiso 1 1 calc R . . H39C H 0.4451 0.2980 0.2229 0.063 Uiso 1 1 calc R . . C40 C 0.33017(10) 0.47855(13) 0.08443(6) 0.0398(4) Uani 1 1 d . . . H40A H 0.3733 0.4421 0.0842 0.048 Uiso 1 1 calc R . . C41 C 0.34160(15) 0.57940(16) 0.06760(9) 0.0658(7) Uani 1 1 d . . . H41A H 0.3496 0.5784 0.0330 0.099 Uiso 1 1 calc R . . H41B H 0.3816 0.6068 0.0899 0.099 Uiso 1 1 calc R . . H41C H 0.3010 0.6180 0.0691 0.099 Uiso 1 1 calc R . . C42 C 0.27311(13) 0.4295(2) 0.04815(7) 0.0667(6) Uani 1 1 d . . . H42A H 0.2832 0.4315 0.0141 0.100 Uiso 1 1 calc R . . H42B H 0.2296 0.4621 0.0485 0.100 Uiso 1 1 calc R . . H42C H 0.2696 0.3632 0.0585 0.100 Uiso 1 1 calc R . . C43 C 0.17438(7) 0.54459(11) 0.20582(5) 0.0286(3) Uani 1 1 d . . . H43A H 0.1765 0.5540 0.2427 0.034 Uiso 1 1 calc R . . C44 C 0.15080(9) 0.63832(12) 0.17954(7) 0.0386(4) Uani 1 1 d . . . H44A H 0.1847 0.6879 0.1912 0.058 Uiso 1 1 calc R . . H44B H 0.1065 0.6567 0.1875 0.058 Uiso 1 1 calc R . . H44C H 0.1460 0.6304 0.1431 0.058 Uiso 1 1 calc R . . C45 C 0.12255(8) 0.46541(14) 0.18852(7) 0.0421(4) Uani 1 1 d . . . H45A H 0.1387 0.4061 0.2058 0.063 Uiso 1 1 calc R . . H45B H 0.1176 0.4566 0.1521 0.063 Uiso 1 1 calc R . . H45C H 0.0781 0.4828 0.1966 0.063 Uiso 1 1 calc R . . C46 C 0.08275(8) 0.65017(11) 0.30404(6) 0.0302(3) Uani 1 1 d . . . C47 C 0.13192(9) 0.71181(11) 0.29249(6) 0.0359(3) Uani 1 1 d . . . H47A H 0.1773 0.6894 0.2938 0.043 Uiso 1 1 calc R . . C48 C 0.11625(10) 0.80590(12) 0.27902(7) 0.0422(4) Uani 1 1 d . . . H48A H 0.1508 0.8466 0.2711 0.051 Uiso 1 1 calc R . . C49 C 0.05098(11) 0.84025(13) 0.27718(7) 0.0455(4) Uani 1 1 d . . . H49A H 0.0403 0.9046 0.2684 0.055 Uiso 1 1 calc R . . C50 C 0.00143(10) 0.78005(15) 0.28825(8) 0.0537(5) Uani 1 1 d . . . H50A H -0.0438 0.8032 0.2869 0.064 Uiso 1 1 calc R . . C51 C 0.01650(9) 0.68600(14) 0.30131(7) 0.0439(4) Uani 1 1 d . . . H51A H -0.0186 0.6454 0.3085 0.053 Uiso 1 1 calc R . . C52 C 0.04524(8) 0.49831(11) 0.36235(6) 0.0305(3) Uani 1 1 d . . . C53 C 0.04160(9) 0.55881(13) 0.40278(6) 0.0370(3) Uani 1 1 d . . . H53A H 0.0712 0.6123 0.4090 0.044 Uiso 1 1 calc R . . C54 C -0.00510(10) 0.54110(15) 0.43389(7) 0.0461(4) Uani 1 1 d . . . H54A H -0.0078 0.5833 0.4609 0.055 Uiso 1 1 calc R . . C55 C -0.04781(9) 0.46247(16) 0.42596(7) 0.0485(4) Uani 1 1 d . . . H55A H -0.0799 0.4510 0.4472 0.058 Uiso 1 1 calc R . . C56 C -0.04346(9) 0.40104(15) 0.38708(7) 0.0476(4) Uani 1 1 d . . . H56A H -0.0719 0.3462 0.3820 0.057 Uiso 1 1 calc R . . C57 C 0.00249(9) 0.41912(13) 0.35521(6) 0.0384(4) Uani 1 1 d . . . H57A H 0.0047 0.3768 0.3282 0.046 Uiso 1 1 calc R . . C58 C 0.18344(8) 0.14856(11) 0.35166(6) 0.0326(3) Uani 1 1 d . . . H58A H 0.1898 0.1772 0.3861 0.039 Uiso 1 1 calc R . . C59 C 0.11727(8) 0.19430(12) 0.32248(7) 0.0388(4) Uani 1 1 d . . . H59A H 0.1246 0.2634 0.3191 0.047 Uiso 1 1 calc R . . H59B H 0.1062 0.1667 0.2882 0.047 Uiso 1 1 calc R . . C60 C 0.05760(9) 0.17835(14) 0.34902(8) 0.0482(4) Uani 1 1 d . . . H60A H 0.0152 0.2032 0.3277 0.058 Uiso 1 1 calc R . . H60B H 0.0657 0.2143 0.3811 0.058 Uiso 1 1 calc R . . C61 C 0.04779(10) 0.07406(15) 0.35997(9) 0.0535(5) Uani 1 1 d . . . H61A H 0.0115 0.0678 0.3803 0.064 Uiso 1 1 calc R . . H61B H 0.0323 0.0399 0.3278 0.064 Uiso 1 1 calc R . . C62 C 0.11279(11) 0.02851(14) 0.38799(9) 0.0526(5) Uani 1 1 d . . . H62A H 0.1050 -0.0404 0.3919 0.063 Uiso 1 1 calc R . . H62B H 0.1250 0.0567 0.4220 0.063 Uiso 1 1 calc R . . C63 C 0.17239(10) 0.04282(12) 0.35989(8) 0.0445(4) Uani 1 1 d . . . H63A H 0.2148 0.0148 0.3797 0.053 Uiso 1 1 calc R . . H63B H 0.1620 0.0099 0.3270 0.053 Uiso 1 1 calc R . . C64 C 0.32791(8) 0.10324(10) 0.35738(6) 0.0304(3) Uani 1 1 d . . . H64A H 0.3110 0.0370 0.3492 0.036 Uiso 1 1 calc R . . C65 C 0.34167(9) 0.11455(12) 0.41468(6) 0.0351(3) Uani 1 1 d . . . H65A H 0.2985 0.1043 0.4271 0.042 Uiso 1 1 calc R . . H65B H 0.3575 0.1802 0.4236 0.042 Uiso 1 1 calc R . . C66 C 0.39585(9) 0.04393(13) 0.44036(7) 0.0415(4) Uani 1 1 d . . . H66A H 0.4045 0.0545 0.4772 0.050 Uiso 1 1 calc R . . H66B H 0.3784 -0.0217 0.4338 0.050 Uiso 1 1 calc R . . C67 C 0.46233(10) 0.05494(15) 0.42126(8) 0.0492(4) Uani 1 1 d . . . H67A H 0.4953 0.0058 0.4368 0.059 Uiso 1 1 calc R . . H67B H 0.4825 0.1181 0.4311 0.059 Uiso 1 1 calc R . . C68 C 0.45013(10) 0.04521(17) 0.36447(8) 0.0546(5) Uani 1 1 d . . . H68A H 0.4352 -0.0205 0.3549 0.065 Uiso 1 1 calc R . . H68B H 0.4936 0.0570 0.3527 0.065 Uiso 1 1 calc R . . C69 C 0.39555(10) 0.11522(15) 0.33863(7) 0.0442(4) Uani 1 1 d . . . H69A H 0.3874 0.1048 0.3018 0.053 Uiso 1 1 calc R . . H69B H 0.4125 0.1810 0.3454 0.053 Uiso 1 1 calc R . . C70 C 0.24931(9) 0.15459(12) 0.25924(6) 0.0364(3) Uani 1 1 d . . . H70A H 0.2969 0.1532 0.2523 0.044 Uiso 1 1 calc R . . C71 C 0.22000(11) 0.05640(12) 0.24376(7) 0.0440(4) Uani 1 1 d . . . H71A H 0.2473 0.0075 0.2650 0.053 Uiso 1 1 calc R . . H71B H 0.1723 0.0527 0.2494 0.053 Uiso 1 1 calc R . . C72 C 0.22090(15) 0.03611(17) 0.18854(8) 0.0641(6) Uani 1 1 d . . . H72A H 0.2690 0.0304 0.1840 0.077 Uiso 1 1 calc R . . H72B H 0.1978 -0.0254 0.1790 0.077 Uiso 1 1 calc R . . C73 C 0.18573(15) 0.11290(19) 0.15426(8) 0.0670(6) Uani 1 1 d . . . H73A H 0.1360 0.1114 0.1545 0.080 Uiso 1 1 calc R . . H73B H 0.1918 0.0999 0.1194 0.080 Uiso 1 1 calc R . . C74 C 0.21333(12) 0.21144(16) 0.16966(7) 0.0541(5) Uani 1 1 d . . . H74A H 0.1851 0.2596 0.1485 0.065 Uiso 1 1 calc R . . H74B H 0.2608 0.2168 0.1638 0.065 Uiso 1 1 calc R . . C75 C 0.21272(11) 0.23170(13) 0.22473(6) 0.0434(4) Uani 1 1 d . . . H75A H 0.1647 0.2365 0.2295 0.052 Uiso 1 1 calc R . . H75B H 0.2353 0.2936 0.2341 0.052 Uiso 1 1 calc R . . C81 C -0.0360(8) 0.2896(8) 0.0195(6) 0.116(5) Uiso 0.364(5) 1 d PDU A -1 H81A H -0.0783 0.2536 0.0077 0.174 Uiso 0.364(5) 1 calc PR A -1 H81B H -0.0272 0.2931 0.0563 0.174 Uiso 0.364(5) 1 calc PR A -1 H81C H 0.0024 0.2576 0.0085 0.174 Uiso 0.364(5) 1 calc PR A -1 C82 C -0.0437(7) 0.3878(8) -0.0020(6) 0.117(5) Uiso 0.364(5) 1 d PDU A -1 H82A H -0.0538 0.3826 -0.0392 0.140 Uiso 0.364(5) 1 calc PR A -1 H82B H -0.0840 0.4178 0.0083 0.140 Uiso 0.364(5) 1 calc PR A -1 C83 C 0.0150(6) 0.4513(7) 0.0123(5) 0.088(3) Uiso 0.364(5) 1 d PDU A -1 H83A H 0.0542 0.4237 -0.0004 0.106 Uiso 0.364(5) 1 calc PR A -1 H83B H 0.0274 0.4522 0.0495 0.106 Uiso 0.364(5) 1 calc PR A -1 C84 C 0.0063(5) 0.5512(6) -0.0055(4) 0.066(2) Uiso 0.364(5) 1 d PDU A -1 H84A H -0.0057 0.5512 -0.0428 0.079 Uiso 0.364(5) 1 calc PR A -1 H84B H -0.0327 0.5798 0.0072 0.079 Uiso 0.364(5) 1 calc PR A -1 C85 C 0.0672(6) 0.6114(6) 0.0102(5) 0.077(3) Uiso 0.364(5) 1 d PDU A -1 H85A H 0.1061 0.5813 -0.0019 0.092 Uiso 0.364(5) 1 calc PR A -1 H85B H 0.0785 0.6114 0.0475 0.092 Uiso 0.364(5) 1 calc PR A -1 C86 C 0.0623(6) 0.7117(6) -0.0071(5) 0.086(3) Uiso 0.364(5) 1 d PDU A -1 H86A H 0.1056 0.7445 0.0058 0.129 Uiso 0.364(5) 1 calc PR A -1 H86B H 0.0249 0.7435 0.0053 0.129 Uiso 0.364(5) 1 calc PR A -1 H86C H 0.0531 0.7133 -0.0440 0.129 Uiso 0.364(5) 1 calc PR A -1 C81' C 0.009(2) 0.301(2) 0.0617(13) 0.143(10) Uiso 0.136(5) 1 d PDU A -2 H81D H -0.0251 0.2507 0.0520 0.215 Uiso 0.136(5) 1 calc PR A -2 H81E H -0.0017 0.3366 0.0901 0.215 Uiso 0.136(5) 1 calc PR A -2 H81F H 0.0547 0.2717 0.0714 0.215 Uiso 0.136(5) 1 calc PR A -2 C82' C 0.009(2) 0.3641(17) 0.0194(12) 0.141(8) Uiso 0.136(5) 1 d PDU A -2 H82C H -0.0371 0.3931 0.0102 0.170 Uiso 0.136(5) 1 calc PR A -2 H82D H 0.0168 0.3260 -0.0097 0.170 Uiso 0.136(5) 1 calc PR A -2 C83' C 0.0599(15) 0.4407(15) 0.0279(12) 0.120(7) Uiso 0.136(5) 1 d PDU A -2 H83C H 0.0988 0.4229 0.0118 0.144 Uiso 0.136(5) 1 calc PR A -2 H83D H 0.0776 0.4464 0.0645 0.144 Uiso 0.136(5) 1 calc PR A -2 C84' C 0.0337(14) 0.5342(14) 0.0084(12) 0.103(7) Uiso 0.136(5) 1 d PDU A -2 H84C H -0.0025 0.5546 0.0267 0.123 Uiso 0.136(5) 1 calc PR A -2 H84D H 0.0123 0.5272 -0.0276 0.123 Uiso 0.136(5) 1 calc PR A -2 C85' C 0.0866(14) 0.6099(15) 0.0130(17) 0.107(8) Uiso 0.136(5) 1 d PDU A -2 H85C H 0.1202 0.6004 0.0446 0.128 Uiso 0.136(5) 1 calc PR A -2 H85D H 0.1114 0.6043 -0.0153 0.128 Uiso 0.136(5) 1 calc PR A -2 C86' C 0.0574(18) 0.7065(15) 0.0129(15) 0.118(8) Uiso 0.136(5) 1 d PDU A -2 H86D H 0.0944 0.7536 0.0163 0.177 Uiso 0.136(5) 1 calc PR A -2 H86E H 0.0333 0.7129 0.0412 0.177 Uiso 0.136(5) 1 calc PR A -2 H86F H 0.0251 0.7172 -0.0188 0.177 Uiso 0.136(5) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02923(6) 0.01776(6) 0.02490(6) -0.00036(3) 0.00659(4) 0.00018(3) Si1 0.02398(17) 0.02072(17) 0.02245(17) -0.00027(13) 0.00793(13) 0.00099(13) Si2 0.02166(17) 0.02196(17) 0.01971(16) 0.00089(13) 0.00534(13) -0.00092(13) P1 0.02523(17) 0.02968(18) 0.02477(17) -0.00090(13) 0.00700(13) 0.00140(13) P2 0.03269(18) 0.01988(16) 0.02791(17) -0.00199(13) 0.00553(14) 0.00035(13) C1 0.0269(7) 0.0225(6) 0.0252(6) -0.0001(5) 0.0090(5) 0.0011(5) C2 0.0407(8) 0.0224(7) 0.0297(7) -0.0021(5) 0.0142(6) -0.0010(6) C3 0.0539(10) 0.0245(7) 0.0329(8) -0.0069(6) 0.0158(7) -0.0077(7) C4 0.0499(9) 0.0300(8) 0.0274(7) -0.0047(6) 0.0145(7) -0.0050(7) C5 0.0409(8) 0.0263(7) 0.0255(7) 0.0003(6) 0.0111(6) -0.0044(6) C6 0.0271(7) 0.0234(7) 0.0247(6) -0.0016(5) 0.0081(5) -0.0004(5) C7 0.0688(12) 0.0221(7) 0.0327(8) -0.0022(6) 0.0206(8) -0.0062(7) C8 0.1049(18) 0.0280(9) 0.0456(10) 0.0036(8) 0.0242(11) 0.0122(10) C9 0.0867(15) 0.0427(10) 0.0432(10) -0.0110(8) 0.0301(10) -0.0300(10) C10 0.0774(13) 0.0352(9) 0.0276(8) -0.0076(7) 0.0165(8) -0.0139(9) C11 0.0594(12) 0.0602(12) 0.0440(10) -0.0236(9) 0.0262(9) -0.0167(10) C12 0.0746(15) 0.0716(14) 0.0428(11) -0.0182(10) -0.0023(10) 0.0143(12) C13 0.0368(8) 0.0251(7) 0.0240(7) 0.0010(5) 0.0061(6) -0.0064(6) C14 0.0416(9) 0.0429(9) 0.0378(9) 0.0026(7) 0.0103(7) -0.0151(7) C15 0.0496(10) 0.0264(7) 0.0378(8) -0.0032(6) 0.0074(7) 0.0023(7) C16 0.0268(7) 0.0262(7) 0.0226(6) 0.0005(5) 0.0053(5) -0.0036(5) C17 0.0309(7) 0.0309(7) 0.0254(7) 0.0042(6) 0.0021(6) -0.0078(6) C18 0.0340(8) 0.0423(9) 0.0264(7) 0.0077(6) -0.0031(6) -0.0128(7) C19 0.0357(8) 0.0428(9) 0.0280(7) 0.0034(7) 0.0022(6) -0.0175(7) C20 0.0382(8) 0.0331(8) 0.0281(7) 0.0055(6) 0.0064(6) -0.0112(6) C21 0.0304(7) 0.0292(7) 0.0237(7) 0.0022(6) 0.0061(6) -0.0039(6) C22 0.0342(8) 0.0358(8) 0.0311(7) 0.0110(6) -0.0061(6) -0.0111(6) C23 0.0344(8) 0.0533(10) 0.0358(8) 0.0186(8) 0.0033(7) -0.0063(7) C24 0.0548(11) 0.0388(9) 0.0405(9) 0.0071(7) -0.0011(8) -0.0008(8) C25 0.0472(10) 0.0541(11) 0.0331(8) 0.0102(8) -0.0031(7) -0.0282(9) C26 0.0631(12) 0.0430(10) 0.0420(9) 0.0014(8) -0.0027(8) -0.0221(9) C27 0.0424(11) 0.105(2) 0.0636(13) -0.0183(13) 0.0116(10) -0.0330(12) C28 0.0325(7) 0.0257(7) 0.0308(7) 0.0065(6) 0.0043(6) -0.0036(6) C29 0.0489(10) 0.0296(8) 0.0460(9) 0.0055(7) 0.0087(8) 0.0018(7) C30 0.0422(9) 0.0391(8) 0.0287(7) 0.0099(6) 0.0047(6) -0.0029(7) C31 0.0245(6) 0.0228(6) 0.0220(6) 0.0000(5) 0.0066(5) -0.0007(5) C32 0.0256(7) 0.0264(7) 0.0258(7) 0.0015(5) 0.0066(5) 0.0008(5) C33 0.0317(7) 0.0300(7) 0.0293(7) 0.0008(6) 0.0123(6) 0.0060(6) C34 0.0384(8) 0.0296(7) 0.0243(7) -0.0005(6) 0.0106(6) 0.0037(6) C35 0.0324(7) 0.0340(8) 0.0218(6) 0.0012(6) 0.0043(6) 0.0034(6) C36 0.0247(7) 0.0258(7) 0.0244(6) 0.0005(5) 0.0060(5) 0.0002(5) C37 0.0270(7) 0.0401(8) 0.0279(7) 0.0061(6) 0.0095(6) 0.0078(6) C38 0.0272(8) 0.0604(11) 0.0430(9) 0.0069(8) 0.0049(7) 0.0022(7) C39 0.0438(9) 0.0429(9) 0.0421(9) 0.0110(7) 0.0143(7) 0.0162(8) C40 0.0521(10) 0.0449(9) 0.0255(7) 0.0025(7) 0.0156(7) 0.0165(8) C41 0.0998(18) 0.0556(12) 0.0557(12) 0.0188(10) 0.0498(13) 0.0226(12) C42 0.0732(15) 0.0964(18) 0.0301(9) -0.0184(10) 0.0091(9) 0.0093(13) C43 0.0249(7) 0.0364(8) 0.0250(7) 0.0045(6) 0.0060(5) 0.0033(6) C44 0.0377(9) 0.0440(9) 0.0361(8) 0.0110(7) 0.0117(7) 0.0132(7) C45 0.0277(8) 0.0507(10) 0.0474(10) 0.0028(8) 0.0058(7) -0.0049(7) C46 0.0327(8) 0.0330(8) 0.0244(7) -0.0013(6) 0.0043(6) 0.0062(6) C47 0.0384(8) 0.0313(8) 0.0393(8) 0.0027(6) 0.0102(7) 0.0076(6) C48 0.0535(10) 0.0305(8) 0.0418(9) 0.0011(7) 0.0071(8) 0.0057(7) C49 0.0591(11) 0.0312(8) 0.0410(9) -0.0031(7) -0.0038(8) 0.0159(8) C50 0.0421(10) 0.0493(11) 0.0658(12) -0.0023(9) 0.0007(9) 0.0206(9) C51 0.0325(8) 0.0459(10) 0.0527(10) 0.0025(8) 0.0062(7) 0.0097(7) C52 0.0257(7) 0.0374(8) 0.0291(7) 0.0022(6) 0.0073(6) 0.0028(6) C53 0.0361(8) 0.0445(9) 0.0326(8) -0.0023(7) 0.0122(6) 0.0000(7) C54 0.0473(10) 0.0598(11) 0.0352(8) -0.0009(8) 0.0180(7) 0.0073(9) C55 0.0346(9) 0.0712(13) 0.0443(10) 0.0119(9) 0.0188(7) 0.0017(9) C56 0.0358(9) 0.0583(12) 0.0508(10) 0.0072(9) 0.0137(8) -0.0098(8) C57 0.0347(8) 0.0429(9) 0.0386(8) 0.0002(7) 0.0093(7) -0.0037(7) C58 0.0334(8) 0.0270(7) 0.0381(8) -0.0010(6) 0.0087(6) 0.0001(6) C59 0.0334(8) 0.0337(8) 0.0478(9) -0.0013(7) 0.0041(7) -0.0013(7) C60 0.0344(9) 0.0470(10) 0.0630(12) -0.0088(9) 0.0085(8) -0.0004(8) C61 0.0399(10) 0.0505(11) 0.0734(13) -0.0075(10) 0.0190(9) -0.0105(8) C62 0.0504(11) 0.0426(10) 0.0700(13) 0.0111(9) 0.0242(10) -0.0054(8) C63 0.0440(10) 0.0281(8) 0.0651(12) 0.0030(8) 0.0196(9) -0.0030(7) C64 0.0353(8) 0.0232(7) 0.0338(7) -0.0008(6) 0.0093(6) 0.0035(6) C65 0.0384(8) 0.0336(8) 0.0343(8) 0.0017(6) 0.0094(6) 0.0060(7) C66 0.0439(9) 0.0378(9) 0.0413(9) 0.0055(7) 0.0041(7) 0.0077(7) C67 0.0392(9) 0.0530(11) 0.0533(11) 0.0033(9) 0.0038(8) 0.0125(8) C68 0.0428(10) 0.0686(13) 0.0549(11) -0.0021(10) 0.0161(9) 0.0174(9) C69 0.0410(9) 0.0547(10) 0.0397(9) 0.0034(8) 0.0150(7) 0.0056(8) C70 0.0439(9) 0.0346(8) 0.0313(8) -0.0033(6) 0.0087(7) 0.0023(7) C71 0.0598(11) 0.0334(8) 0.0385(9) -0.0116(7) 0.0085(8) 0.0009(8) C72 0.0929(18) 0.0557(12) 0.0428(11) -0.0212(9) 0.0107(11) 0.0078(12) C73 0.0863(17) 0.0769(15) 0.0340(10) -0.0196(10) 0.0016(10) 0.0123(13) C74 0.0655(13) 0.0640(13) 0.0322(9) 0.0022(9) 0.0080(8) 0.0122(10) C75 0.0560(11) 0.0392(9) 0.0331(8) 0.0000(7) 0.0039(7) 0.0047(8) _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 Pd Si2 2.3424(4) . ? Pd Si1 2.3764(4) . ? Pd P2 2.4604(4) . ? Si1 C1 1.9145(14) . ? Si1 Si2 2.2569(5) . ? Si1 P1 2.2696(5) . ? Si2 C16 1.9027(14) . ? Si2 C31 1.9194(14) . ? P1 C52 1.8404(15) . ? P1 C46 1.8528(16) . ? P2 C58 1.8561(17) . ? P2 C70 1.8577(16) . ? P2 C64 1.8665(15) . ? C1 C2 1.417(2) . ? C1 C6 1.4186(19) . ? C2 C3 1.393(2) . ? C2 C7 1.522(2) . ? C3 C4 1.389(2) . ? C4 C5 1.379(2) . ? C4 C10 1.516(2) . ? C5 C6 1.395(2) . ? C6 C13 1.5257(19) . ? C7 C9 1.528(3) . ? C7 C8 1.533(3) . ? C10 C11 1.515(3) . ? C10 C12 1.517(3) . ? C13 C15 1.525(2) . ? C13 C14 1.533(2) . ? C16 C17 1.415(2) . ? C16 C21 1.420(2) . ? C17 C18 1.395(2) . ? C17 C22 1.523(2) . ? C18 C19 1.392(2) . ? C19 C20 1.385(2) . ? C19 C25 1.517(2) . ? C20 C21 1.393(2) . ? C21 C28 1.528(2) . ? C22 C23 1.529(2) . ? C22 C24 1.530(3) . ? C25 C26 1.520(3) . ? C25 C27 1.520(3) . ? C28 C30 1.533(2) . ? C28 C29 1.534(2) . ? C31 C36 1.4135(19) . ? C31 C32 1.4152(19) . ? C32 C33 1.400(2) . ? C32 C37 1.525(2) . ? C33 C34 1.382(2) . ? C34 C35 1.387(2) . ? C34 C40 1.521(2) . ? C35 C36 1.393(2) . ? C36 C43 1.5137(19) . ? C37 C38 1.532(2) . ? C37 C39 1.532(2) . ? C40 C42 1.517(3) . ? C40 C41 1.520(3) . ? C43 C44 1.529(2) . ? C43 C45 1.529(2) . ? C46 C47 1.386(2) . ? C46 C51 1.398(2) . ? C47 C48 1.392(2) . ? C48 C49 1.376(3) . ? C49 C50 1.374(3) . ? C50 C51 1.387(3) . ? C52 C57 1.392(2) . ? C52 C53 1.399(2) . ? C53 C54 1.389(2) . ? C54 C55 1.386(3) . ? C55 C56 1.377(3) . ? C56 C57 1.394(2) . ? C58 C63 1.526(2) . ? C58 C59 1.540(2) . ? C59 C60 1.515(3) . ? C60 C61 1.517(3) . ? C61 C62 1.510(3) . ? C62 C63 1.538(3) . ? C64 C65 1.531(2) . ? C64 C69 1.533(2) . ? C65 C66 1.531(2) . ? C66 C67 1.515(3) . ? C67 C68 1.516(3) . ? C68 C69 1.532(3) . ? C70 C75 1.523(2) . ? C70 C71 1.526(2) . ? C71 C72 1.525(3) . ? C72 C73 1.506(3) . ? C73 C74 1.520(3) . ? C74 C75 1.520(2) . ? C81 C82 1.496(11) . ? C82 C83 1.460(12) . ? C83 C84 1.486(8) . ? C84 C85 1.472(11) . ? C85 C86 1.485(10) . ? C81' C82' 1.450(16) . ? C82' C83' 1.465(16) . ? C83' C84' 1.474(16) . ? C84' C85' 1.484(15) . ? C85' C86' 1.478(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 Pd Si1 57.142(12) . . ? Si2 Pd P2 140.325(13) . . ? Si1 Pd P2 156.049(13) . . ? C1 Si1 Si2 123.48(5) . . ? C1 Si1 P1 114.45(4) . . ? Si2 Si1 P1 119.22(2) . . ? C1 Si1 Pd 112.50(4) . . ? Si2 Si1 Pd 60.671(13) . . ? P1 Si1 Pd 112.843(17) . . ? C16 Si2 C31 107.06(6) . . ? C16 Si2 Si1 112.69(4) . . ? C31 Si2 Si1 136.25(5) . . ? C16 Si2 Pd 123.18(4) . . ? C31 Si2 Pd 109.40(4) . . ? Si1 Si2 Pd 62.187(13) . . ? C52 P1 C46 100.44(7) . . ? C52 P1 Si1 106.11(5) . . ? C46 P1 Si1 105.01(5) . . ? C58 P2 C70 109.70(8) . . ? C58 P2 C64 103.12(7) . . ? C70 P2 C64 102.50(7) . . ? C58 P2 Pd 101.21(5) . . ? C70 P2 Pd 113.66(5) . . ? C64 P2 Pd 125.63(5) . . ? C2 C1 C6 117.48(12) . . ? C2 C1 Si1 123.72(11) . . ? C6 C1 Si1 118.79(10) . . ? C3 C2 C1 120.12(13) . . ? C3 C2 C7 116.35(13) . . ? C1 C2 C7 123.53(13) . . ? C4 C3 C2 122.44(14) . . ? C5 C4 C3 117.22(14) . . ? C5 C4 C10 120.45(14) . . ? C3 C4 C10 122.30(14) . . ? C4 C5 C6 122.82(14) . . ? C5 C6 C1 119.88(13) . . ? C5 C6 C13 115.39(12) . . ? C1 C6 C13 124.66(12) . . ? C2 C7 C9 111.69(16) . . ? C2 C7 C8 110.26(15) . . ? C9 C7 C8 111.04(17) . . ? C11 C10 C4 112.29(17) . . ? C11 C10 C12 110.79(16) . . ? C4 C10 C12 111.39(16) . . ? C15 C13 C6 109.66(13) . . ? C15 C13 C14 110.10(13) . . ? C6 C13 C14 112.77(13) . . ? C17 C16 C21 118.10(13) . . ? C17 C16 Si2 124.09(11) . . ? C21 C16 Si2 117.81(10) . . ? C18 C17 C16 119.75(13) . . ? C18 C17 C22 116.97(13) . . ? C16 C17 C22 123.24(13) . . ? C19 C18 C17 122.28(14) . . ? C20 C19 C18 117.65(14) . . ? C20 C19 C25 121.50(15) . . ? C18 C19 C25 120.84(14) . . ? C19 C20 C21 122.35(14) . . ? C20 C21 C16 119.84(13) . . ? C20 C21 C28 116.98(13) . . ? C16 C21 C28 123.17(13) . . ? C17 C22 C23 110.52(14) . . ? C17 C22 C24 112.76(14) . . ? C23 C22 C24 110.28(13) . . ? C19 C25 C26 110.95(15) . . ? C19 C25 C27 111.89(17) . . ? C26 C25 C27 110.89(17) . . ? C21 C28 C30 111.24(13) . . ? C21 C28 C29 113.06(13) . . ? C30 C28 C29 109.96(13) . . ? C36 C31 C32 117.81(12) . . ? C36 C31 Si2 124.09(10) . . ? C32 C31 Si2 117.91(10) . . ? C33 C32 C31 119.68(13) . . ? C33 C32 C37 116.60(13) . . ? C31 C32 C37 123.71(12) . . ? C34 C33 C32 122.45(14) . . ? C33 C34 C35 117.55(13) . . ? C33 C34 C40 121.11(14) . . ? C35 C34 C40 121.34(14) . . ? C34 C35 C36 122.21(14) . . ? C35 C36 C31 120.17(13) . . ? C35 C36 C43 117.12(12) . . ? C31 C36 C43 122.64(12) . . ? C32 C37 C38 112.63(13) . . ? C32 C37 C39 110.49(13) . . ? C38 C37 C39 110.47(14) . . ? C42 C40 C41 111.50(18) . . ? C42 C40 C34 112.15(16) . . ? C41 C40 C34 110.69(14) . . ? C36 C43 C44 113.47(12) . . ? C36 C43 C45 109.65(13) . . ? C44 C43 C45 110.91(13) . . ? C47 C46 C51 117.36(15) . . ? C47 C46 P1 123.20(12) . . ? C51 C46 P1 118.93(13) . . ? C46 C47 C48 121.44(16) . . ? C49 C48 C47 120.38(18) . . ? C50 C49 C48 119.03(17) . . ? C49 C50 C51 120.94(18) . . ? C50 C51 C46 120.84(18) . . ? C57 C52 C53 118.33(15) . . ? C57 C52 P1 117.02(12) . . ? C53 C52 P1 124.46(12) . . ? C54 C53 C52 120.33(17) . . ? C55 C54 C53 120.61(17) . . ? C56 C55 C54 119.59(16) . . ? C55 C56 C57 120.15(18) . . ? C52 C57 C56 120.97(17) . . ? C63 C58 C59 110.46(14) . . ? C63 C58 P2 119.29(12) . . ? C59 C58 P2 111.67(11) . . ? C60 C59 C58 111.34(15) . . ? C59 C60 C61 112.15(16) . . ? C62 C61 C60 112.27(16) . . ? C61 C62 C63 111.21(17) . . ? C58 C63 C62 110.22(15) . . ? C65 C64 C69 108.96(14) . . ? C65 C64 P2 110.98(10) . . ? C69 C64 P2 112.96(11) . . ? C64 C65 C66 111.53(13) . . ? C67 C66 C65 111.23(15) . . ? C66 C67 C68 110.80(16) . . ? C67 C68 C69 111.56(16) . . ? C68 C69 C64 111.55(15) . . ? C75 C70 C71 111.32(15) . . ? C75 C70 P2 112.24(11) . . ? C71 C70 P2 117.37(12) . . ? C72 C71 C70 111.30(17) . . ? C73 C72 C71 112.25(17) . . ? C72 C73 C74 112.60(19) . . ? C73 C74 C75 111.73(18) . . ? C74 C75 C70 112.07(15) . . ? C83 C82 C81 116.4(11) . . ? C82 C83 C84 117.1(10) . . ? C85 C84 C83 114.3(9) . . ? C84 C85 C86 116.9(10) . . ? C81' C82' C83' 115.5(18) . . ? C82' C83' C84' 114.5(18) . . ? C83' C84' C85' 114.5(17) . . ? C86' C85' C84' 112.8(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.58 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.340 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.045