# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1a _database_code_depnum_ccdc_archive 'CCDC 894051' #TrackingRef 'Chem Sci 07-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H23 P Si' _chemical_formula_sum 'C25 H23 P Si' _chemical_formula_weight 382.49 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2823(3) _cell_length_b 16.8988(4) _cell_length_c 22.9869(6) _cell_angle_alpha 81.236(2) _cell_angle_beta 79.739(2) _cell_angle_gamma 81.615(2) _cell_volume 4230.32(19) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13051 _cell_measurement_theta_min 3.0470 _cell_measurement_theta_max 30.7303 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.943 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) 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 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40913 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.80 _reflns_number_total 22303 _reflns_number_gt 16131 _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^)+(0.0565P)^2^+1.5399P] 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 22303 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.043 _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 P1A P 0.79698(4) 0.91779(3) 0.00941(2) 0.02239(10) Uani 1 1 d . . . C2A C 0.77842(18) 0.98627(12) 0.05699(9) 0.0313(4) Uani 1 1 d . . . H2AA H 0.7915 1.0397 0.0397 0.038 Uiso 1 1 calc R . . Si3A Si 0.73679(5) 0.97073(4) 0.13671(2) 0.03249(13) Uani 1 1 d D . . H3AA H 0.8336(14) 0.9666(15) 0.1713(9) 0.056(7) Uiso 1 1 d D . . H3AB H 0.6928(17) 0.8929(6) 0.1552(9) 0.041(6) Uiso 1 1 d D . . C4A C 0.79385(16) 0.96858(10) -0.06554(8) 0.0238(4) Uani 1 1 d . . . C5A C 0.88204(18) 1.01861(12) -0.09165(9) 0.0340(4) Uani 1 1 d . . . H5AA H 0.9477 1.0217 -0.0717 0.041 Uiso 1 1 calc R . . C6A C 0.87408(19) 1.06372(13) -0.14654(9) 0.0385(5) Uani 1 1 d . . . H6AA H 0.9336 1.0984 -0.1640 0.046 Uiso 1 1 calc R . . C7A C 0.77941(19) 1.05850(13) -0.17615(9) 0.0369(5) Uani 1 1 d . . . H7AA H 0.7737 1.0900 -0.2137 0.044 Uiso 1 1 calc R . . C8A C 0.69345(19) 1.00776(13) -0.15135(9) 0.0368(5) Uani 1 1 d . . . H8AA H 0.6295 1.0034 -0.1721 0.044 Uiso 1 1 calc R . . C9A C 0.70032(17) 0.96301(12) -0.09601(9) 0.0299(4) Uani 1 1 d . . . H9AA H 0.6406 0.9283 -0.0788 0.036 Uiso 1 1 calc R . . C10A C 0.93953(15) 0.84992(10) 0.00507(8) 0.0234(4) Uani 1 1 d . . . C11A C 1.00846(17) 0.82979(12) -0.04826(8) 0.0310(4) Uani 1 1 d . . . H11A H 0.9792 0.8485 -0.0848 0.037 Uiso 1 1 calc R . . C12A C 1.11992(18) 0.78239(13) -0.04838(9) 0.0370(5) Uani 1 1 d . . . H12A H 1.1670 0.7694 -0.0850 0.044 Uiso 1 1 calc R . . C13A C 1.16223(19) 0.75428(13) 0.00438(10) 0.0405(5) Uani 1 1 d . . . H13A H 1.2383 0.7216 0.0041 0.049 Uiso 1 1 calc R . . C14A C 1.0946(2) 0.77327(14) 0.05769(10) 0.0432(5) Uani 1 1 d . . . H14A H 1.1239 0.7535 0.0941 0.052 Uiso 1 1 calc R . . C15A C 0.98382(19) 0.82115(12) 0.05810(9) 0.0338(4) Uani 1 1 d . . . H15A H 0.9377 0.8344 0.0949 0.041 Uiso 1 1 calc R . . C16A C 0.68060(16) 0.85062(11) 0.02473(8) 0.0258(4) Uani 1 1 d . . . C17A C 0.70335(18) 0.77288(12) 0.00849(9) 0.0313(4) Uani 1 1 d . . . H17A H 0.7825 0.7533 -0.0096 0.038 Uiso 1 1 calc R . . C18A C 0.6113(2) 0.72399(13) 0.01849(11) 0.0411(5) Uani 1 1 d . . . H18A H 0.6277 0.6712 0.0071 0.049 Uiso 1 1 calc R . . C19A C 0.4966(2) 0.75131(15) 0.04470(11) 0.0457(6) Uani 1 1 d . . . H19A H 0.4342 0.7172 0.0519 0.055 Uiso 1 1 calc R . . C20A C 0.4717(2) 0.82863(16) 0.06062(11) 0.0475(6) Uani 1 1 d . . . H20A H 0.3921 0.8477 0.0784 0.057 Uiso 1 1 calc R . . C21A C 0.56348(18) 0.87818(13) 0.05055(10) 0.0366(5) Uani 1 1 d . . . H21A H 0.5461 0.9312 0.0614 0.044 Uiso 1 1 calc R . . C22A C 0.61664(17) 1.05220(12) 0.16350(9) 0.0303(4) Uani 1 1 d . . . C23A C 0.5772(2) 1.05635(14) 0.22433(10) 0.0420(5) Uani 1 1 d . . . H23A H 0.6137 1.0181 0.2527 0.050 Uiso 1 1 calc R . . C24A C 0.4866(2) 1.11460(16) 0.24399(12) 0.0530(6) Uani 1 1 d . . . H24A H 0.4617 1.1164 0.2855 0.064 Uiso 1 1 calc R . . C25A C 0.4325(2) 1.16983(15) 0.20393(13) 0.0548(7) Uani 1 1 d . . . H25A H 0.3694 1.2095 0.2177 0.066 Uiso 1 1 calc R . . C26A C 0.4692(2) 1.16842(13) 0.14326(12) 0.0451(6) Uani 1 1 d . . . H26A H 0.4317 1.2071 0.1155 0.054 Uiso 1 1 calc R . . C27A C 0.56139(18) 1.11002(12) 0.12327(10) 0.0343(4) Uani 1 1 d . . . H27A H 0.5871 1.1095 0.0817 0.041 Uiso 1 1 calc R . . P1B P 0.29889(4) 0.50350(3) 0.67728(2) 0.02653(11) Uani 1 1 d . . . C2B C 0.26379(19) 0.60368(11) 0.67625(9) 0.0333(4) Uani 1 1 d . . . H2BA H 0.2243 0.6315 0.6445 0.040 Uiso 1 1 calc R . . Si3B Si 0.29322(6) 0.66368(4) 0.72901(3) 0.03684(14) Uani 1 1 d D . . H3BA H 0.3903(13) 0.7138(10) 0.7087(9) 0.047(6) Uiso 1 1 d D . . H3BB H 0.322(2) 0.6146(12) 0.7833(6) 0.053(7) Uiso 1 1 d D . . C4B C 0.20915(16) 0.46506(11) 0.63189(8) 0.0270(4) Uani 1 1 d . . . C5B C 0.20991(19) 0.49957(13) 0.57280(9) 0.0366(5) Uani 1 1 d . . . H5BA H 0.2584 0.5416 0.5566 0.044 Uiso 1 1 calc R . . C6B C 0.1402(2) 0.47286(14) 0.53750(10) 0.0412(5) Uani 1 1 d . . . H6BA H 0.1404 0.4971 0.4974 0.049 Uiso 1 1 calc R . . C7B C 0.07023(19) 0.41098(13) 0.56058(10) 0.0388(5) Uani 1 1 d . . . H7BA H 0.0228 0.3926 0.5363 0.047 Uiso 1 1 calc R . . C8B C 0.0696(2) 0.37624(14) 0.61861(10) 0.0408(5) Uani 1 1 d . . . H8BA H 0.0217 0.3338 0.6344 0.049 Uiso 1 1 calc R . . C9B C 0.13884(19) 0.40303(12) 0.65422(9) 0.0358(5) Uani 1 1 d . . . H9BA H 0.1380 0.3786 0.6943 0.043 Uiso 1 1 calc R . . C10B C 0.45392(17) 0.46602(11) 0.64691(8) 0.0285(4) Uani 1 1 d . . . C11B C 0.48382(19) 0.39016(13) 0.62795(11) 0.0413(5) Uani 1 1 d . . . H11B H 0.4222 0.3564 0.6307 0.050 Uiso 1 1 calc R . . C12B C 0.6021(2) 0.36348(14) 0.60527(11) 0.0466(6) Uani 1 1 d . . . H12B H 0.6219 0.3113 0.5931 0.056 Uiso 1 1 calc R . . C13B C 0.6916(2) 0.41287(14) 0.60032(11) 0.0440(5) Uani 1 1 d . . . H13B H 0.7729 0.3948 0.5844 0.053 Uiso 1 1 calc R . . C14B C 0.6632(2) 0.48790(14) 0.61833(11) 0.0442(5) Uani 1 1 d . . . H14B H 0.7251 0.5218 0.6147 0.053 Uiso 1 1 calc R . . C15B C 0.54476(18) 0.51471(12) 0.64184(10) 0.0347(4) Uani 1 1 d . . . H15B H 0.5259 0.5667 0.6545 0.042 Uiso 1 1 calc R . . C16B C 0.26821(17) 0.44748(11) 0.75130(8) 0.0283(4) Uani 1 1 d . . . C17B C 0.34206(19) 0.37913(12) 0.77142(9) 0.0349(4) Uani 1 1 d . . . H17B H 0.4174 0.3633 0.7478 0.042 Uiso 1 1 calc R . . C18B C 0.3061(2) 0.33406(13) 0.82576(10) 0.0418(5) Uani 1 1 d . . . H18B H 0.3570 0.2875 0.8393 0.050 Uiso 1 1 calc R . . C19B C 0.1964(2) 0.35673(14) 0.86018(10) 0.0415(5) Uani 1 1 d . . . H19B H 0.1709 0.3247 0.8967 0.050 Uiso 1 1 calc R . . C20B C 0.1236(2) 0.42585(14) 0.84173(9) 0.0390(5) Uani 1 1 d . . . H20B H 0.0494 0.4422 0.8661 0.047 Uiso 1 1 calc R . . C21B C 0.15950(18) 0.47117(13) 0.78740(9) 0.0327(4) Uani 1 1 d . . . H21B H 0.1096 0.5187 0.7747 0.039 Uiso 1 1 calc R . . C22B C 0.1599(2) 0.74106(12) 0.74826(9) 0.0357(5) Uani 1 1 d . . . C23B C 0.1711(3) 0.80531(14) 0.77822(10) 0.0491(6) Uani 1 1 d . . . H23B H 0.2467 0.8088 0.7898 0.059 Uiso 1 1 calc R . . C24B C 0.0743(4) 0.86360(16) 0.79122(12) 0.0704(9) Uani 1 1 d . . . H24B H 0.0841 0.9069 0.8112 0.084 Uiso 1 1 calc R . . C25B C -0.0359(3) 0.85900(17) 0.77529(13) 0.0718(10) Uani 1 1 d . . . H25B H -0.1026 0.8986 0.7848 0.086 Uiso 1 1 calc R . . C26B C -0.0499(3) 0.79658(16) 0.74531(12) 0.0584(7) Uani 1 1 d . . . H26B H -0.1260 0.7935 0.7340 0.070 Uiso 1 1 calc R . . C27B C 0.0477(2) 0.73858(13) 0.73197(10) 0.0406(5) Uani 1 1 d . . . H27B H 0.0377 0.6961 0.7112 0.049 Uiso 1 1 calc R . . P1C P 0.27274(4) 0.49488(3) 0.16502(2) 0.02572(11) Uani 1 1 d . . . C2C C 0.23171(19) 0.59458(11) 0.16241(9) 0.0337(4) Uani 1 1 d . . . H2CA H 0.1869 0.6205 0.1321 0.040 Uiso 1 1 calc R . . Si3C Si 0.26661(5) 0.65627(3) 0.21314(3) 0.03466(13) Uani 1 1 d D . . H3CA H 0.3584(15) 0.7096(11) 0.1893(10) 0.058(7) Uiso 1 1 d D . . H3CB H 0.3162(18) 0.6061(10) 0.2623(6) 0.040(6) Uiso 1 1 d D . . C4C C 0.18689(17) 0.45019(11) 0.12100(8) 0.0275(4) Uani 1 1 d . . . C5C C 0.19416(19) 0.47810(13) 0.06044(9) 0.0353(4) Uani 1 1 d . . . H5CA H 0.2443 0.5187 0.0428 0.042 Uiso 1 1 calc R . . C6C C 0.1282(2) 0.44668(14) 0.02579(9) 0.0407(5) Uani 1 1 d . . . H6CA H 0.1325 0.4666 -0.0154 0.049 Uiso 1 1 calc R . . C7C C 0.0563(2) 0.38651(14) 0.05078(10) 0.0405(5) Uani 1 1 d . . . H7CA H 0.0118 0.3649 0.0268 0.049 Uiso 1 1 calc R . . C8C C 0.0496(2) 0.35804(14) 0.11068(10) 0.0430(5) Uani 1 1 d . . . H8CA H 0.0003 0.3168 0.1280 0.052 Uiso 1 1 calc R . . C9C C 0.1150(2) 0.38967(13) 0.14589(9) 0.0369(5) Uani 1 1 d . . . H9CA H 0.1104 0.3697 0.1871 0.044 Uiso 1 1 calc R . . C10C C 0.42902(17) 0.46107(11) 0.13444(8) 0.0276(4) Uani 1 1 d . . . C11C C 0.46416(19) 0.38458(12) 0.11714(10) 0.0379(5) Uani 1 1 d . . . H11C H 0.4054 0.3483 0.1212 0.045 Uiso 1 1 calc R . . C12C C 0.5836(2) 0.36079(14) 0.09408(11) 0.0427(5) Uani 1 1 d . . . H12C H 0.6068 0.3081 0.0830 0.051 Uiso 1 1 calc R . . C13C C 0.66894(19) 0.41338(14) 0.08723(10) 0.0397(5) Uani 1 1 d . . . H13C H 0.7508 0.3974 0.0708 0.048 Uiso 1 1 calc R . . C14C C 0.63555(19) 0.48926(14) 0.10417(10) 0.0402(5) Uani 1 1 d . . . H14C H 0.6948 0.5252 0.0998 0.048 Uiso 1 1 calc R . . C15C C 0.51588(18) 0.51356(12) 0.12759(9) 0.0340(4) Uani 1 1 d . . . H15C H 0.4934 0.5661 0.1389 0.041 Uiso 1 1 calc R . . C16C C 0.24521(16) 0.44126(11) 0.23975(8) 0.0264(4) Uani 1 1 d . . . C17C C 0.32409(18) 0.37613(11) 0.26105(9) 0.0319(4) Uani 1 1 d . . . H17C H 0.4003 0.3617 0.2376 0.038 Uiso 1 1 calc R . . C18C C 0.2914(2) 0.33234(13) 0.31653(10) 0.0390(5) Uani 1 1 d . . . H18C H 0.3456 0.2883 0.3311 0.047 Uiso 1 1 calc R . . C19C C 0.1800(2) 0.35286(13) 0.35059(9) 0.0391(5) Uani 1 1 d . . . H19C H 0.1570 0.3218 0.3879 0.047 Uiso 1 1 calc R . . C20C C 0.10206(19) 0.41827(14) 0.33052(9) 0.0383(5) Uani 1 1 d . . . H20C H 0.0262 0.4326 0.3542 0.046 Uiso 1 1 calc R . . C21C C 0.13512(17) 0.46271(12) 0.27570(9) 0.0317(4) Uani 1 1 d . . . H21C H 0.0823 0.5083 0.2624 0.038 Uiso 1 1 calc R . . C22C C 0.13029(18) 0.72460(11) 0.24427(8) 0.0294(4) Uani 1 1 d . . . C23C C 0.1392(2) 0.77707(12) 0.28440(9) 0.0368(5) Uani 1 1 d . . . H23C H 0.2143 0.7760 0.2979 0.044 Uiso 1 1 calc R . . C24C C 0.0408(2) 0.83065(13) 0.30487(10) 0.0467(6) Uani 1 1 d . . . H24C H 0.0489 0.8654 0.3324 0.056 Uiso 1 1 calc R . . C25C C -0.0683(2) 0.83352(14) 0.28549(11) 0.0492(6) Uani 1 1 d . . . H25C H -0.1353 0.8707 0.2992 0.059 Uiso 1 1 calc R . . C26C C -0.0806(2) 0.78226(14) 0.24602(10) 0.0424(5) Uani 1 1 d . . . H26C H -0.1560 0.7841 0.2326 0.051 Uiso 1 1 calc R . . C27C C 0.01787(19) 0.72809(12) 0.22601(9) 0.0333(4) Uani 1 1 d . . . H27C H 0.0084 0.6926 0.1993 0.040 Uiso 1 1 calc R . . P1D P 0.22766(4) 0.11527(3) 0.46892(2) 0.02835(11) Uani 1 1 d . A . C2D C 0.2667(2) 0.06350(14) 0.41051(10) 0.0454(6) Uani 1 1 d D . . H2DA H 0.3036 0.0903 0.3739 0.054 Uiso 0.789(8) 1 calc PR A 1 H2DB H 0.3225 0.0888 0.3791 0.054 Uiso 0.211(8) 1 d PR A 2 Si3D Si 0.2423(2) -0.04307(18) 0.41312(14) 0.0585(7) Uani 0.789(8) 1 d PDU A 1 H3DA H 0.1319 -0.0455 0.3897 0.070 Uiso 0.789(8) 1 calc PR A 1 H3DB H 0.2259 -0.0802 0.4747 0.070 Uiso 0.789(8) 1 calc PR A 1 Si3E Si 0.2312(5) -0.0202(3) 0.3943(3) 0.0378(12) Uiso 0.211(8) 1 d PDU A 2 H3EA H 0.1547 -0.0006 0.3484 0.045 Uiso 0.211(8) 1 calc PR A 2 H3EB H 0.1614 -0.0602 0.4468 0.045 Uiso 0.211(8) 1 calc PR A 2 C4D C 0.33008(17) 0.19097(12) 0.46450(9) 0.0315(4) Uani 1 1 d . . . C5D C 0.44787(19) 0.17622(15) 0.43406(10) 0.0441(5) Uani 1 1 d . A . H5DA H 0.4718 0.1283 0.4158 0.053 Uiso 1 1 calc R . . C6D C 0.5306(2) 0.23099(18) 0.43015(12) 0.0553(7) Uani 1 1 d . . . H6DA H 0.6108 0.2201 0.4095 0.066 Uiso 1 1 calc R A . C7D C 0.4971(2) 0.30033(17) 0.45578(13) 0.0602(7) Uani 1 1 d . A . H7DA H 0.5538 0.3378 0.4527 0.072 Uiso 1 1 calc R . . C8D C 0.3817(2) 0.31582(15) 0.48592(14) 0.0580(7) Uani 1 1 d . . . H8DA H 0.3587 0.3639 0.5040 0.070 Uiso 1 1 calc R A . C9D C 0.2980(2) 0.26139(14) 0.49021(11) 0.0437(5) Uani 1 1 d . A . H9DA H 0.2181 0.2728 0.5110 0.052 Uiso 1 1 calc R . . C10D C 0.07569(17) 0.17144(11) 0.47836(8) 0.0282(4) Uani 1 1 d . . . C11D C 0.01953(18) 0.20009(12) 0.53169(9) 0.0333(4) Uani 1 1 d . A . H11D H 0.0613 0.1914 0.5649 0.040 Uiso 1 1 calc R . . C12D C -0.09661(19) 0.24106(13) 0.53638(10) 0.0389(5) Uani 1 1 d . . . H12D H -0.1344 0.2601 0.5729 0.047 Uiso 1 1 calc R A . C13D C -0.1576(2) 0.25437(14) 0.48809(11) 0.0463(6) Uani 1 1 d . A . H13D H -0.2370 0.2830 0.4913 0.056 Uiso 1 1 calc R . . C14D C -0.1036(2) 0.22625(14) 0.43515(11) 0.0441(5) Uani 1 1 d . . . H14D H -0.1459 0.2353 0.4020 0.053 Uiso 1 1 calc R A . C15D C 0.01235(18) 0.18488(13) 0.43045(9) 0.0347(4) Uani 1 1 d . A . H15D H 0.0491 0.1654 0.3940 0.042 Uiso 1 1 calc R . . C16D C 0.23316(17) 0.05237(11) 0.53942(8) 0.0284(4) Uani 1 1 d . . . C17D C 0.13367(19) 0.01554(13) 0.57059(10) 0.0383(5) Uani 1 1 d . A . H17D H 0.0597 0.0241 0.5550 0.046 Uiso 1 1 calc R . . C18D C 0.1419(2) -0.03330(14) 0.62408(10) 0.0470(6) Uani 1 1 d . . . H18D H 0.0740 -0.0589 0.6446 0.056 Uiso 1 1 calc R A . C19D C 0.2482(2) -0.04503(14) 0.64773(11) 0.0486(6) Uani 1 1 d . A . H19D H 0.2529 -0.0779 0.6848 0.058 Uiso 1 1 calc R . . C20D C 0.3474(2) -0.00911(14) 0.61760(11) 0.0461(6) Uani 1 1 d . . . H20D H 0.4206 -0.0171 0.6339 0.055 Uiso 1 1 calc R A . C21D C 0.34023(19) 0.03880(13) 0.56347(10) 0.0372(5) Uani 1 1 d . A . H21D H 0.4094 0.0627 0.5425 0.045 Uiso 1 1 calc R . . C22D C 0.3720(3) -0.1033(2) 0.36922(10) 0.0395(12) Uani 0.789(8) 1 d PGDU A 1 C23D C 0.3772(3) -0.09808(19) 0.30791(11) 0.0423(9) Uani 0.789(8) 1 d PGDU A 1 H23D H 0.3134 -0.0673 0.2893 0.051 Uiso 0.789(8) 1 calc PR A 1 C24D C 0.4755(3) -0.13787(16) 0.27379(10) 0.0485(9) Uani 0.789(8) 1 d PG A 1 H24D H 0.4790 -0.1343 0.2319 0.058 Uiso 0.789(8) 1 calc PR A 1 C25D C 0.56878(18) -0.18287(16) 0.3010(2) 0.0500(11) Uani 0.789(8) 1 d PG A 1 H25D H 0.6360 -0.2101 0.2777 0.060 Uiso 0.789(8) 1 calc PR A 1 C26D C 0.5637(3) -0.18807(14) 0.3623(2) 0.0586(13) Uani 0.789(8) 1 d PG A 1 H26D H 0.6274 -0.2188 0.3809 0.070 Uiso 0.789(8) 1 calc PR A 1 C27D C 0.4653(4) -0.14828(19) 0.39642(12) 0.0496(9) Uani 0.789(8) 1 d PGDU A 1 H27D H 0.4618 -0.1518 0.4383 0.060 Uiso 0.789(8) 1 calc PR A 1 C22E C 0.3675(9) -0.0920(8) 0.3677(4) 0.024(3) Uiso 0.211(8) 1 d PGDU A 2 C23E C 0.4076(9) -0.0938(7) 0.3070(4) 0.029(3) Uiso 0.211(8) 1 d PGDU A 2 H23E H 0.3645 -0.0601 0.2787 0.034 Uiso 0.211(8) 1 calc PR A 2 C24E C 0.5107(9) -0.1448(6) 0.2878(4) 0.043(4) Uiso 0.211(8) 1 d PG A 2 H24E H 0.5381 -0.1460 0.2464 0.052 Uiso 0.211(8) 1 calc PR A 2 C25E C 0.5738(8) -0.1940(6) 0.3292(6) 0.044(4) Uiso 0.211(8) 1 d PG A 2 H25E H 0.6443 -0.2288 0.3161 0.053 Uiso 0.211(8) 1 calc PR A 2 C26E C 0.5338(10) -0.1922(7) 0.3898(5) 0.075(6) Uiso 0.211(8) 1 d PG A 2 H26E H 0.5769 -0.2258 0.4181 0.090 Uiso 0.211(8) 1 calc PR A 2 C27E C 0.4306(11) -0.1412(9) 0.4091(4) 0.065(5) Uiso 0.211(8) 1 d PGDU A 2 H27E H 0.4033 -0.1400 0.4505 0.078 Uiso 0.211(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 P1A 0.0201(2) 0.0227(2) 0.0235(2) -0.00372(17) -0.00169(17) -0.00116(17) C2A 0.0344(10) 0.0266(9) 0.0326(10) -0.0090(8) -0.0012(8) -0.0029(8) Si3A 0.0320(3) 0.0364(3) 0.0294(3) -0.0111(2) -0.0070(2) 0.0045(2) C4A 0.0224(8) 0.0226(8) 0.0246(9) -0.0025(7) -0.0019(7) 0.0003(7) C5A 0.0307(10) 0.0382(11) 0.0342(11) 0.0026(9) -0.0084(8) -0.0115(9) C6A 0.0372(11) 0.0389(11) 0.0381(11) 0.0076(9) -0.0042(9) -0.0157(9) C7A 0.0421(12) 0.0375(11) 0.0296(10) 0.0074(9) -0.0089(9) -0.0086(9) C8A 0.0354(11) 0.0426(12) 0.0345(11) 0.0033(9) -0.0152(9) -0.0082(9) C9A 0.0260(9) 0.0321(10) 0.0319(10) 0.0004(8) -0.0064(8) -0.0071(8) C10A 0.0207(8) 0.0226(8) 0.0266(9) -0.0042(7) -0.0017(7) -0.0030(7) C11A 0.0280(10) 0.0384(11) 0.0249(9) -0.0061(8) -0.0043(8) 0.0034(8) C12A 0.0292(10) 0.0451(12) 0.0338(11) -0.0124(9) 0.0015(8) 0.0049(9) C13A 0.0299(11) 0.0436(12) 0.0470(13) -0.0121(10) -0.0111(9) 0.0112(9) C14A 0.0438(13) 0.0473(13) 0.0357(12) -0.0049(10) -0.0161(10) 0.0152(10) C15A 0.0368(11) 0.0348(10) 0.0262(10) -0.0034(8) -0.0040(8) 0.0060(9) C16A 0.0241(9) 0.0279(9) 0.0243(9) 0.0007(7) -0.0042(7) -0.0040(7) C17A 0.0288(10) 0.0296(10) 0.0349(10) -0.0019(8) -0.0052(8) -0.0032(8) C18A 0.0408(12) 0.0328(11) 0.0522(14) -0.0006(10) -0.0132(10) -0.0113(9) C19A 0.0372(12) 0.0502(14) 0.0525(14) 0.0039(11) -0.0102(10) -0.0222(11) C20A 0.0253(11) 0.0608(15) 0.0547(15) -0.0069(12) 0.0030(10) -0.0116(10) C21A 0.0271(10) 0.0389(11) 0.0419(12) -0.0076(9) 0.0011(9) -0.0042(9) C22A 0.0278(9) 0.0340(10) 0.0321(10) -0.0133(8) -0.0031(8) -0.0059(8) C23A 0.0444(13) 0.0486(13) 0.0347(12) -0.0156(10) -0.0041(10) -0.0037(10) C24A 0.0548(15) 0.0587(16) 0.0449(14) -0.0266(12) 0.0099(12) -0.0058(13) C25A 0.0422(13) 0.0438(14) 0.0770(19) -0.0313(14) 0.0095(13) 0.0001(11) C26A 0.0406(12) 0.0310(11) 0.0645(16) -0.0136(11) -0.0089(11) 0.0013(10) C27A 0.0343(11) 0.0310(10) 0.0391(11) -0.0104(9) -0.0046(9) -0.0046(9) P1B 0.0259(2) 0.0233(2) 0.0285(2) -0.00237(19) -0.00144(19) -0.00116(19) C2B 0.0401(11) 0.0249(9) 0.0330(10) -0.0032(8) -0.0065(9) 0.0027(8) Si3B 0.0428(3) 0.0306(3) 0.0385(3) -0.0039(2) -0.0097(3) -0.0057(3) C4B 0.0257(9) 0.0259(9) 0.0274(9) -0.0035(7) -0.0005(7) -0.0011(7) C5B 0.0377(11) 0.0375(11) 0.0334(11) 0.0012(9) -0.0024(9) -0.0101(9) C6B 0.0447(13) 0.0485(13) 0.0302(11) -0.0004(9) -0.0070(9) -0.0081(10) C7B 0.0355(11) 0.0454(12) 0.0384(12) -0.0098(10) -0.0091(9) -0.0065(10) C8B 0.0427(12) 0.0400(12) 0.0421(12) -0.0036(10) -0.0059(10) -0.0157(10) C9B 0.0434(12) 0.0332(10) 0.0308(10) -0.0002(8) -0.0043(9) -0.0103(9) C10B 0.0284(9) 0.0251(9) 0.0302(10) -0.0023(7) -0.0017(8) -0.0029(8) C11B 0.0314(11) 0.0325(11) 0.0597(15) -0.0150(10) 0.0049(10) -0.0085(9) C12B 0.0375(12) 0.0344(11) 0.0646(16) -0.0175(11) 0.0084(11) -0.0020(10) C13B 0.0284(11) 0.0415(12) 0.0568(15) -0.0085(11) 0.0066(10) -0.0009(9) C14B 0.0293(11) 0.0415(12) 0.0626(15) -0.0092(11) -0.0027(10) -0.0100(10) C15B 0.0314(10) 0.0307(10) 0.0430(12) -0.0084(9) -0.0056(9) -0.0042(8) C16B 0.0292(10) 0.0275(9) 0.0284(9) -0.0024(7) -0.0059(8) -0.0035(8) C17B 0.0351(11) 0.0317(10) 0.0363(11) -0.0026(9) -0.0073(9) 0.0015(9) C18B 0.0530(14) 0.0312(11) 0.0414(12) 0.0025(9) -0.0172(11) -0.0010(10) C19B 0.0505(13) 0.0451(12) 0.0308(11) 0.0032(9) -0.0100(10) -0.0167(11) C20B 0.0333(11) 0.0522(13) 0.0321(11) -0.0034(10) -0.0022(9) -0.0128(10) C21B 0.0292(10) 0.0375(11) 0.0306(10) -0.0003(8) -0.0069(8) -0.0033(8) C22B 0.0525(13) 0.0277(10) 0.0244(9) -0.0031(8) 0.0067(9) -0.0122(9) C23B 0.0772(18) 0.0377(12) 0.0318(11) -0.0084(10) 0.0077(11) -0.0208(12) C24B 0.118(3) 0.0396(14) 0.0466(15) -0.0208(12) 0.0299(17) -0.0223(16) C25B 0.090(2) 0.0421(15) 0.0607(18) -0.0092(13) 0.0360(17) 0.0107(15) C26B 0.0532(16) 0.0553(16) 0.0532(16) -0.0036(13) 0.0148(12) 0.0059(13) C27B 0.0478(13) 0.0364(11) 0.0340(11) -0.0081(9) 0.0060(10) -0.0046(10) P1C 0.0261(2) 0.0221(2) 0.0263(2) -0.00240(18) -0.00045(19) 0.00034(18) C2C 0.0413(11) 0.0238(9) 0.0332(11) -0.0033(8) -0.0060(9) 0.0054(8) Si3C 0.0331(3) 0.0273(3) 0.0424(3) -0.0062(2) -0.0016(2) -0.0034(2) C4C 0.0257(9) 0.0260(9) 0.0292(9) -0.0057(7) -0.0014(7) 0.0002(7) C5C 0.0330(11) 0.0404(11) 0.0299(10) 0.0004(9) -0.0008(8) -0.0066(9) C6C 0.0398(12) 0.0529(14) 0.0278(10) -0.0041(9) -0.0039(9) -0.0030(10) C7C 0.0358(11) 0.0487(13) 0.0398(12) -0.0143(10) -0.0080(9) -0.0034(10) C8C 0.0476(13) 0.0426(12) 0.0406(12) -0.0049(10) -0.0040(10) -0.0160(10) C9C 0.0438(12) 0.0376(11) 0.0292(10) -0.0018(9) -0.0043(9) -0.0092(10) C10C 0.0268(9) 0.0273(9) 0.0258(9) -0.0020(7) 0.0005(7) -0.0011(8) C11C 0.0303(10) 0.0313(10) 0.0500(13) -0.0113(9) 0.0062(9) -0.0058(9) C12C 0.0361(12) 0.0351(11) 0.0521(14) -0.0128(10) 0.0086(10) -0.0003(9) C13C 0.0264(10) 0.0500(13) 0.0385(12) -0.0067(10) 0.0048(9) -0.0017(9) C14C 0.0291(10) 0.0463(13) 0.0467(13) -0.0083(10) 0.0005(9) -0.0148(9) C15C 0.0342(11) 0.0317(10) 0.0364(11) -0.0074(8) -0.0015(9) -0.0071(9) C16C 0.0262(9) 0.0269(9) 0.0263(9) -0.0033(7) -0.0043(7) -0.0037(7) C17C 0.0311(10) 0.0282(10) 0.0349(11) -0.0042(8) -0.0047(8) 0.0009(8) C18C 0.0490(13) 0.0303(10) 0.0376(11) 0.0027(9) -0.0140(10) -0.0029(9) C19C 0.0471(13) 0.0400(12) 0.0308(11) 0.0042(9) -0.0065(9) -0.0164(10) C20C 0.0327(11) 0.0497(13) 0.0313(11) -0.0048(9) 0.0031(8) -0.0119(10) C21C 0.0257(9) 0.0371(11) 0.0311(10) -0.0041(8) -0.0039(8) -0.0014(8) C22C 0.0366(11) 0.0229(9) 0.0264(9) -0.0014(7) 0.0029(8) -0.0078(8) C23C 0.0479(13) 0.0324(10) 0.0300(10) -0.0035(8) 0.0001(9) -0.0130(9) C24C 0.0697(17) 0.0332(11) 0.0347(12) -0.0126(9) 0.0120(11) -0.0148(11) C25C 0.0513(14) 0.0361(12) 0.0494(14) -0.0064(10) 0.0169(11) 0.0006(11) C26C 0.0359(12) 0.0405(12) 0.0449(13) 0.0007(10) 0.0032(10) -0.0041(10) C27C 0.0387(11) 0.0307(10) 0.0290(10) -0.0039(8) 0.0025(8) -0.0089(9) P1D 0.0249(2) 0.0330(3) 0.0262(2) -0.0073(2) 0.00015(19) -0.0020(2) C2D 0.0446(13) 0.0560(14) 0.0339(12) -0.0199(11) 0.0074(10) -0.0027(11) Si3D 0.0520(7) 0.0666(12) 0.0618(11) -0.0413(10) 0.0287(8) -0.0346(8) C4D 0.0262(9) 0.0359(10) 0.0303(10) 0.0020(8) -0.0035(8) -0.0051(8) C5D 0.0311(11) 0.0547(14) 0.0419(13) 0.0011(11) -0.0004(9) -0.0044(10) C6D 0.0330(12) 0.0718(18) 0.0558(15) 0.0132(13) -0.0019(11) -0.0179(12) C7D 0.0475(15) 0.0534(16) 0.081(2) 0.0180(14) -0.0213(14) -0.0236(13) C8D 0.0503(15) 0.0406(13) 0.088(2) -0.0078(13) -0.0181(14) -0.0120(12) C9D 0.0330(11) 0.0400(12) 0.0587(15) -0.0073(11) -0.0066(10) -0.0064(10) C10D 0.0246(9) 0.0288(9) 0.0306(10) -0.0039(8) -0.0020(7) -0.0044(8) C11D 0.0301(10) 0.0369(11) 0.0327(10) -0.0086(9) -0.0038(8) -0.0006(9) C12D 0.0296(10) 0.0377(11) 0.0473(13) -0.0123(10) 0.0008(9) 0.0018(9) C13D 0.0290(11) 0.0441(13) 0.0618(16) -0.0032(11) -0.0079(10) 0.0058(10) C14D 0.0375(12) 0.0496(13) 0.0456(13) 0.0028(11) -0.0182(10) -0.0022(10) C15D 0.0328(11) 0.0405(11) 0.0306(10) -0.0020(9) -0.0038(8) -0.0079(9) C16D 0.0285(9) 0.0260(9) 0.0298(10) -0.0067(8) -0.0005(8) -0.0022(8) C17D 0.0317(11) 0.0438(12) 0.0389(12) -0.0053(10) -0.0013(9) -0.0090(9) C18D 0.0517(14) 0.0461(13) 0.0419(13) 0.0004(10) 0.0022(11) -0.0198(11) C19D 0.0654(16) 0.0387(12) 0.0401(13) 0.0054(10) -0.0113(12) -0.0089(12) C20D 0.0471(14) 0.0427(13) 0.0477(14) 0.0015(10) -0.0165(11) -0.0001(11) C21D 0.0320(11) 0.0372(11) 0.0402(12) -0.0015(9) -0.0036(9) -0.0039(9) C22D 0.048(2) 0.036(2) 0.0381(18) -0.0138(13) 0.0021(13) -0.0190(14) C23D 0.0353(18) 0.0519(19) 0.0402(18) -0.0119(13) -0.0039(14) -0.0035(17) C24D 0.051(2) 0.059(2) 0.0336(16) -0.0136(15) 0.0021(16) -0.0033(17) C25D 0.0378(17) 0.0345(16) 0.075(3) -0.0178(18) 0.0060(16) -0.0018(13) C26D 0.062(2) 0.0329(17) 0.091(4) -0.0074(18) -0.042(3) -0.0045(15) C27D 0.075(3) 0.0431(18) 0.0411(17) -0.0042(15) -0.0236(19) -0.0231(19) _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 P1A C2A 1.6771(19) . ? P1A C4A 1.8079(18) . ? P1A C16A 1.8124(19) . ? P1A C10A 1.8307(17) . ? C2A Si3A 1.797(2) . ? Si3A C22A 1.8786(19) . ? C4A C9A 1.388(2) . ? C4A C5A 1.394(3) . ? C5A C6A 1.381(3) . ? C6A C7A 1.385(3) . ? C7A C8A 1.377(3) . ? C8A C9A 1.386(3) . ? C10A C11A 1.390(2) . ? C10A C15A 1.392(3) . ? C11A C12A 1.389(3) . ? C12A C13A 1.374(3) . ? C13A C14A 1.379(3) . ? C14A C15A 1.386(3) . ? C16A C21A 1.393(3) . ? C16A C17A 1.396(3) . ? C17A C18A 1.386(3) . ? C18A C19A 1.372(3) . ? C19A C20A 1.386(3) . ? C20A C21A 1.391(3) . ? C22A C27A 1.397(3) . ? C22A C23A 1.399(3) . ? C23A C24A 1.376(3) . ? C24A C25A 1.365(4) . ? C25A C26A 1.385(4) . ? C26A C27A 1.391(3) . ? P1B C2B 1.6790(19) . ? P1B C16B 1.818(2) . ? P1B C4B 1.8194(19) . ? P1B C10B 1.8233(19) . ? C2B Si3B 1.796(2) . ? Si3B C22B 1.880(2) . ? C4B C9B 1.388(3) . ? C4B C5B 1.393(3) . ? C5B C6B 1.387(3) . ? C6B C7B 1.386(3) . ? C7B C8B 1.372(3) . ? C8B C9B 1.389(3) . ? C10B C15B 1.384(3) . ? C10B C11B 1.392(3) . ? C11B C12B 1.380(3) . ? C12B C13B 1.380(3) . ? C13B C14B 1.370(3) . ? C14B C15B 1.387(3) . ? C16B C17B 1.391(3) . ? C16B C21B 1.396(3) . ? C17B C18B 1.387(3) . ? C18B C19B 1.382(3) . ? C19B C20B 1.383(3) . ? C20B C21B 1.389(3) . ? C22B C27B 1.391(3) . ? C22B C23B 1.403(3) . ? C23B C24B 1.383(4) . ? C24B C25B 1.373(5) . ? C25B C26B 1.386(4) . ? C26B C27B 1.387(3) . ? P1C C2C 1.6757(19) . ? P1C C16C 1.8126(19) . ? P1C C10C 1.8212(19) . ? P1C C4C 1.8242(19) . ? C2C Si3C 1.804(2) . ? Si3C C22C 1.885(2) . ? C4C C9C 1.389(3) . ? C4C C5C 1.392(3) . ? C5C C6C 1.387(3) . ? C6C C7C 1.385(3) . ? C7C C8C 1.380(3) . ? C8C C9C 1.395(3) . ? C10C C15C 1.389(3) . ? C10C C11C 1.392(3) . ? C11C C12C 1.383(3) . ? C12C C13C 1.376(3) . ? C13C C14C 1.377(3) . ? C14C C15C 1.389(3) . ? C16C C17C 1.396(3) . ? C16C C21C 1.397(3) . ? C17C C18C 1.391(3) . ? C18C C19C 1.385(3) . ? C19C C20C 1.383(3) . ? C20C C21C 1.385(3) . ? C22C C27C 1.396(3) . ? C22C C23C 1.398(3) . ? C23C C24C 1.387(3) . ? C24C C25C 1.374(4) . ? C25C C26C 1.383(3) . ? C26C C27C 1.390(3) . ? P1D C2D 1.672(2) . ? P1D C16D 1.803(2) . ? P1D C4D 1.825(2) . ? P1D C10D 1.8285(19) . ? C2D Si3E 1.637(5) . ? C2D Si3D 1.851(3) . ? Si3D C22D 1.8833(19) . ? Si3E C22E 1.887(6) . ? C4D C9D 1.382(3) . ? C4D C5D 1.394(3) . ? C5D C6D 1.390(3) . ? C6D C7D 1.366(4) . ? C7D C8D 1.370(4) . ? C8D C9D 1.393(3) . ? C10D C15D 1.390(3) . ? C10D C11D 1.398(3) . ? C11D C12D 1.384(3) . ? C12D C13D 1.381(3) . ? C13D C14D 1.380(3) . ? C14D C15D 1.385(3) . ? C16D C21D 1.391(3) . ? C16D C17D 1.394(3) . ? C17D C18D 1.382(3) . ? C18D C19D 1.379(3) . ? C19D C20D 1.377(3) . ? C20D C21D 1.386(3) . ? C22D C23D 1.3900 . ? C22D C27D 1.3900 . ? C23D C24D 1.3900 . ? C24D C25D 1.3900 . ? C25D C26D 1.3900 . ? C26D C27D 1.3900 . ? C22E C23E 1.3900 . ? C22E C27E 1.3900 . ? C23E C24E 1.3900 . ? C24E C25E 1.3900 . ? C25E C26E 1.3900 . ? C26E C27E 1.3900 . ? 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 C2A P1A C4A 109.65(9) . . ? C2A P1A C16A 114.00(9) . . ? C4A P1A C16A 106.82(8) . . ? C2A P1A C10A 116.26(9) . . ? C4A P1A C10A 105.18(8) . . ? C16A P1A C10A 104.16(8) . . ? P1A C2A Si3A 127.79(12) . . ? C2A Si3A C22A 111.31(9) . . ? C9A C4A C5A 119.28(17) . . ? C9A C4A P1A 121.02(14) . . ? C5A C4A P1A 119.55(14) . . ? C6A C5A C4A 120.10(18) . . ? C5A C6A C7A 120.09(19) . . ? C8A C7A C6A 120.21(19) . . ? C7A C8A C9A 119.91(18) . . ? C8A C9A C4A 120.37(18) . . ? C11A C10A C15A 118.81(17) . . ? C11A C10A P1A 123.58(14) . . ? C15A C10A P1A 117.50(14) . . ? C12A C11A C10A 120.34(18) . . ? C13A C12A C11A 120.14(19) . . ? C12A C13A C14A 120.24(19) . . ? C13A C14A C15A 119.94(19) . . ? C14A C15A C10A 120.54(18) . . ? C21A C16A C17A 118.65(18) . . ? C21A C16A P1A 119.57(15) . . ? C17A C16A P1A 121.70(14) . . ? C18A C17A C16A 120.48(19) . . ? C19A C18A C17A 120.4(2) . . ? C18A C19A C20A 120.0(2) . . ? C19A C20A C21A 119.9(2) . . ? C20A C21A C16A 120.5(2) . . ? C27A C22A C23A 117.44(19) . . ? C27A C22A Si3A 121.10(15) . . ? C23A C22A Si3A 121.45(16) . . ? C24A C23A C22A 121.5(2) . . ? C25A C24A C23A 120.2(2) . . ? C24A C25A C26A 120.4(2) . . ? C25A C26A C27A 119.6(2) . . ? C26A C27A C22A 120.9(2) . . ? C2B P1B C16B 113.41(9) . . ? C2B P1B C4B 110.61(9) . . ? C16B P1B C4B 105.75(9) . . ? C2B P1B C10B 117.55(10) . . ? C16B P1B C10B 105.64(9) . . ? C4B P1B C10B 102.76(9) . . ? P1B C2B Si3B 126.70(12) . . ? C2B Si3B C22B 111.10(10) . . ? C9B C4B C5B 118.71(18) . . ? C9B C4B P1B 122.31(15) . . ? C5B C4B P1B 118.98(15) . . ? C6B C5B C4B 120.3(2) . . ? C7B C6B C5B 120.2(2) . . ? C8B C7B C6B 119.9(2) . . ? C7B C8B C9B 120.1(2) . . ? C4B C9B C8B 120.8(2) . . ? C15B C10B C11B 118.78(18) . . ? C15B C10B P1B 119.12(14) . . ? C11B C10B P1B 122.09(15) . . ? C12B C11B C10B 120.7(2) . . ? C11B C12B C13B 119.8(2) . . ? C14B C13B C12B 120.1(2) . . ? C13B C14B C15B 120.4(2) . . ? C10B C15B C14B 120.23(19) . . ? C17B C16B C21B 118.98(19) . . ? C17B C16B P1B 123.41(15) . . ? C21B C16B P1B 117.39(14) . . ? C18B C17B C16B 120.3(2) . . ? C19B C18B C17B 120.1(2) . . ? C18B C19B C20B 120.4(2) . . ? C19B C20B C21B 119.6(2) . . ? C20B C21B C16B 120.60(19) . . ? C27B C22B C23B 117.3(2) . . ? C27B C22B Si3B 121.72(15) . . ? C23B C22B Si3B 120.96(19) . . ? C24B C23B C22B 121.3(3) . . ? C25B C24B C23B 120.1(2) . . ? C24B C25B C26B 120.1(3) . . ? C25B C26B C27B 119.6(3) . . ? C26B C27B C22B 121.6(2) . . ? C2C P1C C16C 113.07(9) . . ? C2C P1C C10C 117.33(10) . . ? C16C P1C C10C 106.16(8) . . ? C2C P1C C4C 111.27(10) . . ? C16C P1C C4C 105.60(9) . . ? C10C P1C C4C 102.27(8) . . ? P1C C2C Si3C 124.67(12) . . ? C2C Si3C C22C 112.74(9) . . ? C9C C4C C5C 119.28(18) . . ? C9C C4C P1C 122.25(15) . . ? C5C C4C P1C 118.47(15) . . ? C6C C5C C4C 120.1(2) . . ? C7C C6C C5C 120.5(2) . . ? C8C C7C C6C 119.7(2) . . ? C7C C8C C9C 120.1(2) . . ? C4C C9C C8C 120.3(2) . . ? C15C C10C C11C 118.84(18) . . ? C15C C10C P1C 118.97(14) . . ? C11C C10C P1C 122.19(15) . . ? C12C C11C C10C 120.7(2) . . ? C13C C12C C11C 120.0(2) . . ? C12C C13C C14C 119.95(19) . . ? C13C C14C C15C 120.5(2) . . ? C10C C15C C14C 120.03(19) . . ? C17C C16C C21C 118.89(18) . . ? C17C C16C P1C 123.15(15) . . ? C21C C16C P1C 117.76(14) . . ? C18C C17C C16C 120.14(19) . . ? C19C C18C C17C 120.04(19) . . ? C20C C19C C18C 120.4(2) . . ? C19C C20C C21C 119.7(2) . . ? C20C C21C C16C 120.79(19) . . ? C27C C22C C23C 117.12(18) . . ? C27C C22C Si3C 121.57(14) . . ? C23C C22C Si3C 121.23(16) . . ? C24C C23C C22C 121.4(2) . . ? C25C C24C C23C 120.2(2) . . ? C24C C25C C26C 120.0(2) . . ? C25C C26C C27C 119.7(2) . . ? C26C C27C C22C 121.56(19) . . ? C2D P1D C16D 113.05(11) . . ? C2D P1D C4D 110.54(11) . . ? C16D P1D C4D 106.87(9) . . ? C2D P1D C10D 117.11(10) . . ? C16D P1D C10D 103.74(9) . . ? C4D P1D C10D 104.67(9) . . ? Si3E C2D P1D 134.7(3) . . ? P1D C2D Si3D 123.84(15) . . ? C2D Si3D C22D 112.93(15) . . ? C2D Si3E C22E 113.3(6) . . ? C9D C4D C5D 118.3(2) . . ? C9D C4D P1D 123.76(16) . . ? C5D C4D P1D 117.96(17) . . ? C6D C5D C4D 120.6(2) . . ? C7D C6D C5D 120.3(2) . . ? C6D C7D C8D 119.9(2) . . ? C7D C8D C9D 120.3(2) . . ? C4D C9D C8D 120.6(2) . . ? C15D C10D C11D 118.58(18) . . ? C15D C10D P1D 118.26(15) . . ? C11D C10D P1D 123.15(15) . . ? C12D C11D C10D 120.44(19) . . ? C13D C12D C11D 120.1(2) . . ? C14D C13D C12D 120.2(2) . . ? C13D C14D C15D 119.8(2) . . ? C14D C15D C10D 120.9(2) . . ? C21D C16D C17D 118.43(19) . . ? C21D C16D P1D 119.46(15) . . ? C17D C16D P1D 122.10(15) . . ? C18D C17D C16D 120.4(2) . . ? C19D C18D C17D 120.3(2) . . ? C20D C19D C18D 120.0(2) . . ? C19D C20D C21D 119.9(2) . . ? C20D C21D C16D 120.9(2) . . ? C23D C22D C27D 120.0 . . ? C23D C22D Si3D 118.64(17) . . ? C27D C22D Si3D 121.24(17) . . ? C22D C23D C24D 120.0 . . ? C23D C24D C25D 120.0 . . ? C24D C25D C26D 120.0 . . ? C25D C26D C27D 120.0 . . ? C26D C27D C22D 120.0 . . ? C23E C22E C27E 120.0 . . ? C23E C22E Si3E 120.4(5) . . ? C27E C22E Si3E 119.5(5) . . ? C24E C23E C22E 120.0 . . ? C23E C24E C25E 120.0 . . ? C24E C25E C26E 120.0 . . ? C27E C26E C25E 120.0 . . ? C26E C27E C22E 120.0 . . ? _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.487 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.054 data_2a _database_code_depnum_ccdc_archive 'CCDC 894052' #TrackingRef 'Chem Sci 07-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H70 Li2 N2 P2 Si4' _chemical_formula_sum 'C50 H70 Li2 N2 P2 Si4' _chemical_formula_weight 887.26 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.8666(4) _cell_length_b 22.2888(5) _cell_length_c 25.4992(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.652(2) _cell_angle_gamma 90.00 _cell_volume 10538.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 13346 _cell_measurement_theta_min 2.9590 _cell_measurement_theta_max 28.8484 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) 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 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41245 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.91 _reflns_number_total 19768 _reflns_number_gt 16161 _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0596 _refine_ls_wR_factor_obs+ 0.1549 _refine_ls_abs_structure_Flack+ 0.44(9) _refine_ls_R_factor_obs- 0.0596 _refine_ls_wR_factor_obs- 0.1550 _refine_ls_abs_structure_Flack- 0.56(9) ; _chemical_absolute_configuration . _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^)+(0.0986P)^2^+3.6605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 7777 Friedel pairs' _refine_ls_abs_structure_Flack 0.44(9) _refine_ls_number_reflns 19768 _refine_ls_number_parameters 1116 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1549 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.064 _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 Li1A Li 0.7542(4) 0.6602(3) 0.5850(3) 0.0258(14) Uani 1 1 d . A . Li2A Li 0.6624(4) 0.5925(3) 0.5262(3) 0.0288(15) Uani 1 1 d . A . N1A N 0.75251(17) 0.56767(14) 0.58295(13) 0.0240(7) Uani 1 1 d . . . N2A N 0.66747(18) 0.68510(15) 0.52786(13) 0.0241(7) Uani 1 1 d D . . Si1A Si 0.73905(7) 0.54329(6) 0.64375(5) 0.0338(3) Uani 1 1 d . . . Si2A Si 0.80355(6) 0.52861(5) 0.54711(5) 0.0336(3) Uani 1 1 d . . . Si3A Si 0.59820(6) 0.70801(6) 0.55757(5) 0.0339(3) Uani 1 1 d . A . Si4A Si 0.70031(8) 0.72696(6) 0.48361(6) 0.0361(4) Uani 0.933(3) 1 d PDU A 1 Si4C Si 0.6725(11) 0.7080(9) 0.4592(7) 0.039(3) Uiso 0.067(3) 1 d PDU A 2 P1A P 0.87368(6) 0.75920(5) 0.68066(4) 0.0274(2) Uani 1 1 d . A . P2A P 0.54094(6) 0.49547(5) 0.43357(4) 0.0272(2) Uani 1 1 d . A . C1A C 0.8320(2) 0.7360(2) 0.61922(17) 0.0312(9) Uani 1 1 d . . . H1AA H 0.8726 0.7309 0.5999 0.037 Uiso 1 1 calc R A . H1AB H 0.8065 0.7726 0.6038 0.037 Uiso 1 1 calc R . . C2A C 0.9404(2) 0.7049(2) 0.70984(17) 0.0323(10) Uani 1 1 d . . . C3A C 0.9382(2) 0.6474(2) 0.69049(19) 0.0418(11) Uani 1 1 d . A . H3AA H 0.9003 0.6361 0.6623 0.050 Uiso 1 1 calc R . . C4A C 0.9898(3) 0.6058(3) 0.7111(2) 0.0589(15) Uani 1 1 d . . . H4AA H 0.9853 0.5657 0.6984 0.071 Uiso 1 1 calc R A . C5A C 1.0477(3) 0.6214(3) 0.7495(2) 0.0534(14) Uani 1 1 d . A . H5AA H 1.0852 0.5934 0.7615 0.064 Uiso 1 1 calc R . . C6A C 1.0504(3) 0.6798(3) 0.7708(2) 0.0553(14) Uani 1 1 d . . . H6AA H 1.0886 0.6906 0.7991 0.066 Uiso 1 1 calc R A . C7A C 0.9976(3) 0.7220(2) 0.7508(2) 0.0486(12) Uani 1 1 d . A . H7AA H 1.0002 0.7617 0.7647 0.058 Uiso 1 1 calc R . . C8A C 0.8083(2) 0.7690(2) 0.72335(17) 0.0327(10) Uani 1 1 d . . . C9A C 0.7995(3) 0.7284(2) 0.76279(17) 0.0379(11) Uani 1 1 d . A . H9AA H 0.8317 0.6955 0.7705 0.045 Uiso 1 1 calc R . . C10A C 0.7439(3) 0.7356(3) 0.7912(2) 0.0555(15) Uani 1 1 d . . . H10A H 0.7375 0.7069 0.8174 0.067 Uiso 1 1 calc R A . C11A C 0.6989(3) 0.7831(3) 0.7816(2) 0.0635(19) Uani 1 1 d . A . H11A H 0.6622 0.7881 0.8021 0.076 Uiso 1 1 calc R . . C12A C 0.7054(3) 0.8248(3) 0.7423(2) 0.0572(16) Uani 1 1 d . . . H12A H 0.6723 0.8572 0.7348 0.069 Uiso 1 1 calc R A . C13A C 0.7616(3) 0.8182(2) 0.7140(2) 0.0428(11) Uani 1 1 d . A . H13A H 0.7682 0.8473 0.6881 0.051 Uiso 1 1 calc R . . C14A C 0.9237(2) 0.8294(2) 0.68844(18) 0.0329(10) Uani 1 1 d . . . C15A C 0.9265(3) 0.8675(2) 0.73224(19) 0.0435(12) Uani 1 1 d . A . H15A H 0.8972 0.8590 0.7579 0.052 Uiso 1 1 calc R . . C16A C 0.9712(3) 0.9176(2) 0.7389(2) 0.0530(14) Uani 1 1 d . . . H16A H 0.9737 0.9426 0.7694 0.064 Uiso 1 1 calc R A . C17A C 1.0124(3) 0.9304(2) 0.7004(2) 0.0477(13) Uani 1 1 d . A . H17A H 1.0430 0.9646 0.7045 0.057 Uiso 1 1 calc R . . C18A C 1.0093(3) 0.8947(2) 0.6570(2) 0.0453(12) Uani 1 1 d . . . H18A H 1.0373 0.9045 0.6309 0.054 Uiso 1 1 calc R A . C19A C 0.9657(3) 0.8440(2) 0.6503(2) 0.0401(11) Uani 1 1 d . A . H19A H 0.9643 0.8193 0.6198 0.048 Uiso 1 1 calc R . . C20A C 0.6632(3) 0.4888(2) 0.6407(2) 0.0546(14) Uani 1 1 d . . . H20A H 0.6198 0.5052 0.6181 0.082 Uiso 1 1 calc R . . H20B H 0.6537 0.4819 0.6767 0.082 Uiso 1 1 calc R . . H20C H 0.6762 0.4508 0.6256 0.082 Uiso 1 1 calc R . . C21A C 0.8183(3) 0.5057(3) 0.6876(2) 0.0685(17) Uani 1 1 d . . . H21A H 0.8330 0.4706 0.6691 0.103 Uiso 1 1 calc R . . H21B H 0.8043 0.4930 0.7210 0.103 Uiso 1 1 calc R . . H21C H 0.8586 0.5340 0.6953 0.103 Uiso 1 1 calc R . . C22A C 0.7175(3) 0.6083(3) 0.6860(2) 0.0603(15) Uani 1 1 d . . . H22A H 0.6769 0.6312 0.6661 0.090 Uiso 1 1 calc R . . H22B H 0.7598 0.6345 0.6947 0.090 Uiso 1 1 calc R . . H22C H 0.7047 0.5930 0.7190 0.090 Uiso 1 1 calc R . . C23A C 0.7788(3) 0.5467(2) 0.4744(2) 0.0536(13) Uani 1 1 d . . . H23A H 0.7276 0.5381 0.4618 0.080 Uiso 1 1 calc R . . H23B H 0.8079 0.5222 0.4545 0.080 Uiso 1 1 calc R . . H23C H 0.7881 0.5893 0.4688 0.080 Uiso 1 1 calc R . . C24A C 0.7925(3) 0.4441(2) 0.5512(2) 0.0581(13) Uani 1 1 d . . . H24A H 0.7414 0.4336 0.5406 0.087 Uiso 1 1 calc R . . H24B H 0.8100 0.4308 0.5880 0.087 Uiso 1 1 calc R . . H24C H 0.8204 0.4244 0.5273 0.087 Uiso 1 1 calc R . . C25A C 0.9027(2) 0.5453(3) 0.5673(2) 0.0579(15) Uani 1 1 d . . . H25A H 0.9106 0.5886 0.5652 0.087 Uiso 1 1 calc R . . H25B H 0.9293 0.5244 0.5432 0.087 Uiso 1 1 calc R . . H25C H 0.9197 0.5316 0.6039 0.087 Uiso 1 1 calc R . . C26A C 0.6280(3) 0.7573(2) 0.61710(19) 0.0478(12) Uani 1 1 d . . . H26A H 0.6520 0.7930 0.6063 0.072 Uiso 1 1 calc R A . H26B H 0.6617 0.7352 0.6442 0.072 Uiso 1 1 calc R . . H26C H 0.5859 0.7696 0.6320 0.072 Uiso 1 1 calc R . . C27A C 0.5240(3) 0.7493(3) 0.5137(2) 0.0740(19) Uani 1 1 d . . . H27A H 0.5437 0.7852 0.4993 0.111 Uiso 1 1 calc R A . H27B H 0.4875 0.7612 0.5345 0.111 Uiso 1 1 calc R . . H27C H 0.5019 0.7232 0.4842 0.111 Uiso 1 1 calc R . . C28A C 0.5513(2) 0.6408(2) 0.5821(2) 0.0556(13) Uani 1 1 d . . . H28A H 0.5345 0.6136 0.5522 0.083 Uiso 1 1 calc R A . H28B H 0.5100 0.6546 0.5972 0.083 Uiso 1 1 calc R . . H28C H 0.5852 0.6196 0.6096 0.083 Uiso 1 1 calc R . . C29A C 0.7005(4) 0.8105(2) 0.4972(3) 0.0715(18) Uani 0.933(3) 1 d PD A 1 H29A H 0.7242 0.8182 0.5341 0.107 Uiso 0.933(3) 1 calc PR A 1 H29B H 0.6508 0.8252 0.4917 0.107 Uiso 0.933(3) 1 calc PR A 1 H29C H 0.7268 0.8312 0.4728 0.107 Uiso 0.933(3) 1 calc PR A 1 C30A C 0.6517(4) 0.7178(3) 0.4127(2) 0.085(2) Uani 0.933(3) 1 d PDU A 1 H30A H 0.6489 0.6752 0.4033 0.127 Uiso 0.933(3) 1 calc PR A 1 H30B H 0.6779 0.7394 0.3887 0.127 Uiso 0.933(3) 1 calc PR A 1 H30C H 0.6028 0.7343 0.4091 0.127 Uiso 0.933(3) 1 calc PR A 1 C31A C 0.7976(3) 0.7081(2) 0.4817(2) 0.0533(14) Uani 0.933(3) 1 d PD A 1 H31A H 0.8021 0.6649 0.4759 0.080 Uiso 0.933(3) 1 calc PR A 1 H31B H 0.8281 0.7194 0.5157 0.080 Uiso 0.933(3) 1 calc PR A 1 H31C H 0.8130 0.7302 0.4525 0.080 Uiso 0.933(3) 1 calc PR A 1 C29C C 0.751(2) 0.7613(19) 0.465(2) 0.043(16) Uiso 0.067(3) 1 d PD A 2 H29G H 0.7377 0.8002 0.4785 0.065 Uiso 0.067(3) 1 calc PR A 2 H29H H 0.7646 0.7667 0.4303 0.065 Uiso 0.067(3) 1 calc PR A 2 H29I H 0.7923 0.7448 0.4904 0.065 Uiso 0.067(3) 1 calc PR A 2 C30C C 0.595(2) 0.748(2) 0.415(2) 0.066(11) Uiso 0.067(3) 1 d PDU A 2 H30G H 0.5548 0.7524 0.4334 0.099 Uiso 0.067(3) 1 calc PR A 2 H30H H 0.5801 0.7249 0.3818 0.099 Uiso 0.067(3) 1 calc PR A 2 H30I H 0.6115 0.7880 0.4055 0.099 Uiso 0.067(3) 1 calc PR A 2 C31C C 0.695(3) 0.6434(17) 0.417(2) 0.037(14) Uiso 0.067(3) 1 d PD A 2 H31G H 0.6662 0.6083 0.4233 0.056 Uiso 0.067(3) 1 calc PR A 2 H31H H 0.7463 0.6338 0.4274 0.056 Uiso 0.067(3) 1 calc PR A 2 H31I H 0.6839 0.6546 0.3795 0.056 Uiso 0.067(3) 1 calc PR A 2 C32A C 0.5841(2) 0.51666(19) 0.49552(17) 0.0321(9) Uani 1 1 d . . . H32A H 0.6101 0.4800 0.5102 0.039 Uiso 1 1 calc R A . H32B H 0.5446 0.5217 0.5158 0.039 Uiso 1 1 calc R . . C33A C 0.4780(2) 0.55322(19) 0.40451(17) 0.0299(9) Uani 1 1 d . . . C34A C 0.4987(2) 0.61311(19) 0.41148(19) 0.0364(10) Uani 1 1 d . A . H34A H 0.5454 0.6229 0.4305 0.044 Uiso 1 1 calc R . . C35A C 0.4510(3) 0.6588(2) 0.3905(2) 0.0479(12) Uani 1 1 d . . . H35A H 0.4654 0.6996 0.3946 0.058 Uiso 1 1 calc R A . C36A C 0.3831(3) 0.6440(2) 0.3640(2) 0.0442(12) Uani 1 1 d . A . H36A H 0.3509 0.6749 0.3492 0.053 Uiso 1 1 calc R . . C37A C 0.3614(3) 0.5865(3) 0.3587(2) 0.0506(13) Uani 1 1 d . . . H37A H 0.3137 0.5774 0.3410 0.061 Uiso 1 1 calc R A . C38A C 0.4080(2) 0.5404(2) 0.37876(19) 0.0414(10) Uani 1 1 d . A . H38A H 0.3920 0.4999 0.3749 0.050 Uiso 1 1 calc R . . C39A C 0.6065(2) 0.4825(2) 0.39064(18) 0.0315(9) Uani 1 1 d . . . C40A C 0.6184(3) 0.5231(2) 0.35266(19) 0.0401(11) Uani 1 1 d . A . H40A H 0.5896 0.5583 0.3466 0.048 Uiso 1 1 calc R . . C41A C 0.6721(3) 0.5132(3) 0.3231(2) 0.0583(16) Uani 1 1 d . . . H41A H 0.6789 0.5408 0.2961 0.070 Uiso 1 1 calc R A . C42A C 0.7157(3) 0.4632(3) 0.3332(2) 0.0533(15) Uani 1 1 d . A . H42A H 0.7535 0.4568 0.3137 0.064 Uiso 1 1 calc R . . C43A C 0.7042(3) 0.4225(2) 0.3716(3) 0.0523(14) Uani 1 1 d . . . H43A H 0.7334 0.3876 0.3780 0.063 Uiso 1 1 calc R A . C44A C 0.6505(3) 0.4323(2) 0.4009(2) 0.0402(11) Uani 1 1 d . A . H44A H 0.6436 0.4047 0.4279 0.048 Uiso 1 1 calc R . . C45A C 0.4857(2) 0.42675(19) 0.42458(18) 0.0311(9) Uani 1 1 d . . . C46A C 0.4701(3) 0.3981(2) 0.3758(2) 0.0498(13) Uani 1 1 d . A . H46A H 0.4899 0.4126 0.3466 0.060 Uiso 1 1 calc R . . C47A C 0.4257(3) 0.3486(2) 0.3697(3) 0.0605(15) Uani 1 1 d . . . H47A H 0.4155 0.3284 0.3363 0.073 Uiso 1 1 calc R A . C48A C 0.3958(3) 0.3280(2) 0.4120(3) 0.0652(18) Uani 1 1 d . A . H48A H 0.3646 0.2942 0.4074 0.078 Uiso 1 1 calc R . . C49A C 0.4111(3) 0.3564(2) 0.4606(3) 0.0587(16) Uani 1 1 d . . . H49A H 0.3906 0.3425 0.4897 0.070 Uiso 1 1 calc R A . C50A C 0.4573(3) 0.4060(2) 0.4668(2) 0.0406(11) Uani 1 1 d . A . H50A H 0.4691 0.4253 0.5005 0.049 Uiso 1 1 calc R . . Li1B Li 0.2483(3) 0.6613(3) 0.5763(3) 0.0256(14) Uani 1 1 d . B . Li2B Li 0.1548(4) 0.5957(3) 0.5179(3) 0.0263(14) Uani 1 1 d . B . N1B N 0.24736(18) 0.56927(15) 0.57259(13) 0.0252(7) Uani 1 1 d D . . N2B N 0.15859(18) 0.68738(14) 0.52150(13) 0.0232(7) Uani 1 1 d . . . Si1B Si 0.21485(17) 0.52703(9) 0.61748(11) 0.0339(6) Uani 0.834(14) 1 d PDU B 1 Si1D Si 0.2317(10) 0.5325(7) 0.6302(7) 0.052(4) Uiso 0.166(14) 1 d PDU B 2 Si2B Si 0.31523(6) 0.54620(5) 0.54221(4) 0.0304(3) Uani 1 1 d . B . Si3B Si 0.10812(6) 0.72693(5) 0.55856(5) 0.0317(3) Uani 1 1 d . B . Si4B Si 0.16989(7) 0.71228(5) 0.46081(5) 0.0314(3) Uani 1 1 d . B . P1B P 0.37260(6) 0.75751(5) 0.66722(4) 0.0258(2) Uani 1 1 d . B . P2B P 0.03727(6) 0.49642(5) 0.42389(4) 0.0274(2) Uani 1 1 d . B . C1B C 0.3287(2) 0.7347(2) 0.60613(17) 0.0320(9) Uani 1 1 d . . . H1BA H 0.3682 0.7275 0.5862 0.038 Uiso 1 1 calc R B . H1BB H 0.3044 0.7716 0.5904 0.038 Uiso 1 1 calc R . . C2B C 0.4345(2) 0.7005(2) 0.69824(16) 0.0294(9) Uani 1 1 d . . . C3B C 0.4189(3) 0.6411(2) 0.6891(2) 0.0469(12) Uani 1 1 d . B . H3BA H 0.3753 0.6304 0.6659 0.056 Uiso 1 1 calc R . . C4B C 0.4644(3) 0.5961(2) 0.7124(2) 0.0524(13) Uani 1 1 d . . . H4BA H 0.4508 0.5553 0.7065 0.063 Uiso 1 1 calc R B . C5B C 0.5288(3) 0.6100(2) 0.7440(2) 0.0515(13) Uani 1 1 d . B . H5BA H 0.5611 0.5791 0.7588 0.062 Uiso 1 1 calc R . . C6B C 0.5467(3) 0.6696(3) 0.7541(3) 0.085(2) Uani 1 1 d . . . H6BA H 0.5909 0.6800 0.7766 0.102 Uiso 1 1 calc R B . C7B C 0.4994(3) 0.7141(2) 0.7311(3) 0.0662(18) Uani 1 1 d . B . H7BA H 0.5120 0.7550 0.7381 0.079 Uiso 1 1 calc R . . C8B C 0.3072(2) 0.77207(19) 0.70938(17) 0.0281(9) Uani 1 1 d . . . C9B C 0.2938(3) 0.7311(2) 0.74762(19) 0.0378(11) Uani 1 1 d . B . H9BA H 0.3219 0.6956 0.7544 0.045 Uiso 1 1 calc R . . C10B C 0.2385(3) 0.7429(2) 0.7760(2) 0.0460(12) Uani 1 1 d . . . H10B H 0.2293 0.7153 0.8023 0.055 Uiso 1 1 calc R B . C11B C 0.1978(3) 0.7933(2) 0.7661(2) 0.0465(13) Uani 1 1 d . B . H11B H 0.1604 0.8003 0.7858 0.056 Uiso 1 1 calc R . . C12B C 0.2092(3) 0.8344(2) 0.7285(2) 0.0425(12) Uani 1 1 d . . . H12B H 0.1798 0.8692 0.7216 0.051 Uiso 1 1 calc R B . C13B C 0.2653(3) 0.8239(2) 0.70041(18) 0.0356(10) Uani 1 1 d . B . H13B H 0.2749 0.8524 0.6749 0.043 Uiso 1 1 calc R . . C14B C 0.4265(2) 0.82535(19) 0.67256(18) 0.0309(9) Uani 1 1 d . . . C15B C 0.4409(3) 0.8591(2) 0.7194(2) 0.0428(12) Uani 1 1 d . B . H15B H 0.4204 0.8477 0.7493 0.051 Uiso 1 1 calc R . . C16B C 0.4854(3) 0.9097(2) 0.7226(3) 0.0564(15) Uani 1 1 d . . . H16B H 0.4950 0.9329 0.7544 0.068 Uiso 1 1 calc R B . C17B C 0.5148(3) 0.9252(2) 0.6795(3) 0.0517(14) Uani 1 1 d . B . H17B H 0.5459 0.9591 0.6820 0.062 Uiso 1 1 calc R . . C18B C 0.5010(3) 0.8937(2) 0.6333(3) 0.0563(15) Uani 1 1 d . . . H18B H 0.5222 0.9057 0.6040 0.068 Uiso 1 1 calc R B . C19B C 0.4557(2) 0.8438(2) 0.62874(19) 0.0390(11) Uani 1 1 d . B . H19B H 0.4448 0.8225 0.5960 0.047 Uiso 1 1 calc R . . C20B C 0.2144(5) 0.4422(3) 0.6068(4) 0.068(2) Uani 0.834(14) 1 d PDU B 1 H20D H 0.2636 0.4283 0.6068 0.102 Uiso 0.834(14) 1 calc PR B 1 H20E H 0.1837 0.4325 0.5725 0.102 Uiso 0.834(14) 1 calc PR B 1 H20F H 0.1955 0.4223 0.6356 0.102 Uiso 0.834(14) 1 calc PR B 1 C21B C 0.2647(5) 0.5380(5) 0.6878(2) 0.092(3) Uani 0.834(14) 1 d PDU B 1 H21D H 0.3158 0.5286 0.6897 0.138 Uiso 0.834(14) 1 calc PR B 1 H21E H 0.2445 0.5113 0.7118 0.138 Uiso 0.834(14) 1 calc PR B 1 H21F H 0.2597 0.5798 0.6985 0.138 Uiso 0.834(14) 1 calc PR B 1 C22B C 0.1175(3) 0.5454(3) 0.6191(3) 0.0510(19) Uani 0.834(14) 1 d PDU B 1 H22D H 0.1122 0.5888 0.6228 0.077 Uiso 0.834(14) 1 calc PR B 1 H22E H 0.1029 0.5250 0.6494 0.077 Uiso 0.834(14) 1 calc PR B 1 H22F H 0.0870 0.5319 0.5858 0.077 Uiso 0.834(14) 1 calc PR B 1 C20D C 0.216(2) 0.4538(14) 0.6016(18) 0.063(9) Uiso 0.166(14) 1 d PDU B 2 H20G H 0.2619 0.4377 0.5942 0.095 Uiso 0.166(14) 1 calc PR B 2 H20H H 0.1806 0.4552 0.5684 0.095 Uiso 0.166(14) 1 calc PR B 2 H20I H 0.1987 0.4278 0.6274 0.095 Uiso 0.166(14) 1 calc PR B 2 C21D C 0.2972(19) 0.523(2) 0.6942(11) 0.076(9) Uiso 0.166(14) 1 d PDU B 2 H21G H 0.3059 0.5619 0.7121 0.115 Uiso 0.166(14) 1 calc PR B 2 H21H H 0.3427 0.5070 0.6867 0.115 Uiso 0.166(14) 1 calc PR B 2 H21I H 0.2773 0.4950 0.7173 0.115 Uiso 0.166(14) 1 calc PR B 2 C22D C 0.1429(15) 0.5539(16) 0.6487(16) 0.068(8) Uiso 0.166(14) 1 d PDU B 2 H22G H 0.1450 0.5956 0.6610 0.102 Uiso 0.166(14) 1 calc PR B 2 H22H H 0.1331 0.5275 0.6773 0.102 Uiso 0.166(14) 1 calc PR B 2 H22I H 0.1042 0.5496 0.6175 0.102 Uiso 0.166(14) 1 calc PR B 2 C23B C 0.2846(2) 0.4951(2) 0.48430(18) 0.0438(11) Uani 1 1 d . . . H23D H 0.3193 0.4622 0.4850 0.066 Uiso 1 1 calc R B . H23E H 0.2814 0.5177 0.4510 0.066 Uiso 1 1 calc R . . H23F H 0.2371 0.4786 0.4866 0.066 Uiso 1 1 calc R . . C24B C 0.3920(3) 0.5066(3) 0.5859(2) 0.0577(14) Uani 1 1 d . . . H24D H 0.4053 0.4710 0.5674 0.087 Uiso 1 1 calc R B . H24E H 0.3773 0.4945 0.6193 0.087 Uiso 1 1 calc R . . H24F H 0.4336 0.5337 0.5939 0.087 Uiso 1 1 calc R . . C25B C 0.3593(2) 0.6122(2) 0.5151(2) 0.0468(11) Uani 1 1 d . . . H25D H 0.3954 0.5979 0.4949 0.070 Uiso 1 1 calc R B . H25E H 0.3828 0.6375 0.5447 0.070 Uiso 1 1 calc R . . H25F H 0.3226 0.6357 0.4915 0.070 Uiso 1 1 calc R . . C26B C 0.1206(3) 0.8110(2) 0.5566(2) 0.0543(13) Uani 1 1 d . . . H26D H 0.0734 0.8306 0.5505 0.081 Uiso 1 1 calc R B . H26E H 0.1460 0.8213 0.5275 0.081 Uiso 1 1 calc R . . H26F H 0.1490 0.8246 0.5906 0.081 Uiso 1 1 calc R . . C27B C 0.0092(2) 0.7124(3) 0.5397(2) 0.0590(15) Uani 1 1 d . . . H27D H -0.0171 0.7505 0.5387 0.089 Uiso 1 1 calc R B . H27E H -0.0060 0.6857 0.5660 0.089 Uiso 1 1 calc R . . H27F H -0.0013 0.6936 0.5044 0.089 Uiso 1 1 calc R . . C28B C 0.1336(3) 0.7087(2) 0.63158(19) 0.0528(13) Uani 1 1 d . . . H28D H 0.0966 0.7241 0.6504 0.079 Uiso 1 1 calc R B . H28E H 0.1801 0.7274 0.6462 0.079 Uiso 1 1 calc R . . H28F H 0.1375 0.6651 0.6362 0.079 Uiso 1 1 calc R . . C29B C 0.2473(3) 0.7665(2) 0.4641(2) 0.0505(12) Uani 1 1 d . . . H29D H 0.2326 0.7999 0.4395 0.076 Uiso 1 1 calc R B . H29E H 0.2886 0.7459 0.4540 0.076 Uiso 1 1 calc R . . H29F H 0.2609 0.7820 0.5006 0.076 Uiso 1 1 calc R . . C30B C 0.0912(3) 0.7528(2) 0.4190(2) 0.0504(12) Uani 1 1 d . . . H30D H 0.1085 0.7895 0.4043 0.076 Uiso 1 1 calc R B . H30E H 0.0559 0.7632 0.4413 0.076 Uiso 1 1 calc R . . H30F H 0.0685 0.7267 0.3897 0.076 Uiso 1 1 calc R . . C31B C 0.1871(3) 0.6473(2) 0.41828(17) 0.0438(11) Uani 1 1 d . . . H31D H 0.1988 0.6623 0.3847 0.066 Uiso 1 1 calc R B . H31E H 0.1440 0.6221 0.4106 0.066 Uiso 1 1 calc R . . H31F H 0.2277 0.6237 0.4373 0.066 Uiso 1 1 calc R . . C32B C 0.0794(2) 0.5206(2) 0.48531(17) 0.0323(9) Uani 1 1 d . . . H32C H 0.1055 0.4844 0.5009 0.039 Uiso 1 1 calc R B . H32D H 0.0390 0.5255 0.5048 0.039 Uiso 1 1 calc R . . C33B C -0.0268(2) 0.55189(19) 0.39284(17) 0.0283(9) Uani 1 1 d . . . C34B C -0.0242(3) 0.6092(2) 0.4137(2) 0.0496(13) Uani 1 1 d . B . H34B H 0.0131 0.6199 0.4426 0.059 Uiso 1 1 calc R . . C35B C -0.0764(3) 0.6519(2) 0.3924(2) 0.0550(14) Uani 1 1 d . . . H35B H -0.0755 0.6911 0.4072 0.066 Uiso 1 1 calc R B . C36B C -0.1280(3) 0.6362(2) 0.3505(2) 0.0447(12) Uani 1 1 d . B . H36B H -0.1628 0.6652 0.3353 0.054 Uiso 1 1 calc R . . C37B C -0.1311(3) 0.5808(3) 0.3299(2) 0.0592(15) Uani 1 1 d . . . H37B H -0.1684 0.5711 0.3008 0.071 Uiso 1 1 calc R B . C38B C -0.0814(3) 0.5376(2) 0.3501(2) 0.0485(12) Uani 1 1 d . B . H38B H -0.0844 0.4986 0.3350 0.058 Uiso 1 1 calc R . . C39B C 0.1032(2) 0.4817(2) 0.38190(17) 0.0283(9) Uani 1 1 d . . . C40B C 0.1148(3) 0.5208(2) 0.34301(18) 0.0350(10) Uani 1 1 d . B . H40B H 0.0859 0.5558 0.3359 0.042 Uiso 1 1 calc R . . C41B C 0.1688(3) 0.5097(2) 0.3138(2) 0.0457(12) Uani 1 1 d . . . H41B H 0.1754 0.5360 0.2858 0.055 Uiso 1 1 calc R B . C42B C 0.2130(3) 0.4595(3) 0.3258(2) 0.0450(12) Uani 1 1 d . B . H42B H 0.2508 0.4522 0.3066 0.054 Uiso 1 1 calc R . . C43B C 0.2020(3) 0.4214(2) 0.3647(2) 0.0449(12) Uani 1 1 d . . . H43B H 0.2319 0.3871 0.3727 0.054 Uiso 1 1 calc R B . C44B C 0.1474(2) 0.4320(2) 0.39316(19) 0.0380(10) Uani 1 1 d . B . H44B H 0.1402 0.4051 0.4205 0.046 Uiso 1 1 calc R . . C45B C -0.0167(2) 0.42725(19) 0.41831(18) 0.0303(9) Uani 1 1 d . . . C46B C -0.0224(3) 0.3893(2) 0.3748(2) 0.0463(13) Uani 1 1 d . B . H46B H 0.0022 0.3986 0.3465 0.056 Uiso 1 1 calc R . . C47B C -0.0637(3) 0.3379(2) 0.3724(2) 0.0464(12) Uani 1 1 d . . . H47B H -0.0654 0.3112 0.3432 0.056 Uiso 1 1 calc R B . C48B C -0.1014(3) 0.3250(2) 0.4108(2) 0.0449(12) Uani 1 1 d . B . H48B H -0.1311 0.2903 0.4079 0.054 Uiso 1 1 calc R . . C49B C -0.0970(3) 0.3624(2) 0.4546(2) 0.0471(12) Uani 1 1 d . . . H49B H -0.1228 0.3533 0.4822 0.057 Uiso 1 1 calc R B . C50B C -0.0539(2) 0.4139(2) 0.45769(19) 0.0366(10) Uani 1 1 d . B . H50B H -0.0506 0.4399 0.4876 0.044 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 Li1A 0.023(3) 0.024(3) 0.032(4) -0.002(3) 0.007(3) -0.001(2) Li2A 0.035(4) 0.020(3) 0.032(4) 0.002(3) 0.008(3) 0.005(3) N1A 0.0232(17) 0.0164(16) 0.0313(19) 0.0012(13) 0.0022(13) -0.0013(12) N2A 0.0216(16) 0.0225(17) 0.0278(18) 0.0020(13) 0.0032(12) 0.0012(12) Si1A 0.0361(6) 0.0306(6) 0.0339(7) 0.0101(5) 0.0047(5) -0.0022(5) Si2A 0.0250(6) 0.0288(6) 0.0473(7) -0.0077(6) 0.0077(5) 0.0014(5) Si3A 0.0281(6) 0.0389(7) 0.0322(6) -0.0110(6) -0.0008(5) 0.0123(5) Si4A 0.0469(8) 0.0311(7) 0.0284(7) 0.0084(6) 0.0022(6) -0.0106(6) P1A 0.0271(5) 0.0262(5) 0.0284(6) 0.0021(4) 0.0036(4) -0.0055(4) P2A 0.0253(5) 0.0239(5) 0.0320(6) 0.0010(4) 0.0046(4) -0.0010(4) C1A 0.027(2) 0.033(2) 0.032(2) -0.0033(18) 0.0032(17) -0.0082(16) C2A 0.027(2) 0.040(2) 0.030(2) 0.0086(18) 0.0059(17) -0.0038(17) C3A 0.032(2) 0.048(3) 0.041(3) -0.006(2) -0.0031(18) 0.0078(19) C4A 0.055(3) 0.055(3) 0.064(4) -0.016(3) 0.001(3) 0.025(3) C5A 0.032(3) 0.072(4) 0.057(3) 0.019(3) 0.011(2) 0.016(2) C6A 0.034(2) 0.064(3) 0.058(3) 0.023(3) -0.016(2) -0.014(2) C7A 0.044(3) 0.043(3) 0.053(3) 0.009(2) -0.007(2) -0.010(2) C8A 0.032(2) 0.038(2) 0.027(2) -0.0045(18) 0.0014(17) -0.0139(18) C9A 0.044(3) 0.038(3) 0.030(2) 0.0045(19) 0.0028(18) -0.014(2) C10A 0.065(4) 0.060(4) 0.045(3) -0.009(3) 0.021(3) -0.025(3) C11A 0.052(3) 0.088(5) 0.058(4) -0.041(3) 0.029(3) -0.029(3) C12A 0.038(3) 0.073(4) 0.063(4) -0.027(3) 0.015(2) 0.001(3) C13A 0.052(3) 0.036(3) 0.041(3) -0.006(2) 0.011(2) 0.002(2) C14A 0.030(2) 0.032(2) 0.036(2) 0.0035(18) 0.0033(17) -0.0058(17) C15A 0.047(3) 0.045(3) 0.038(3) -0.010(2) 0.006(2) -0.018(2) C16A 0.051(3) 0.050(3) 0.057(3) -0.021(2) 0.007(2) -0.025(2) C17A 0.043(3) 0.027(2) 0.074(4) -0.011(2) 0.013(2) -0.014(2) C18A 0.034(2) 0.034(3) 0.072(4) 0.001(2) 0.020(2) -0.0064(19) C19A 0.046(3) 0.029(2) 0.049(3) -0.005(2) 0.018(2) -0.0064(19) C20A 0.059(3) 0.052(3) 0.054(3) 0.013(2) 0.013(2) -0.023(2) C21A 0.061(3) 0.062(4) 0.071(4) 0.028(3) -0.018(3) -0.009(3) C22A 0.077(4) 0.067(4) 0.038(3) -0.005(3) 0.014(2) -0.011(3) C23A 0.062(3) 0.056(3) 0.047(3) -0.016(2) 0.020(2) -0.019(2) C24A 0.056(3) 0.033(3) 0.087(4) -0.008(3) 0.017(3) 0.005(2) C25A 0.029(2) 0.073(4) 0.074(4) -0.031(3) 0.014(2) -0.001(2) C26A 0.047(3) 0.054(3) 0.042(3) -0.018(2) 0.006(2) 0.002(2) C27A 0.055(3) 0.102(5) 0.055(4) -0.022(3) -0.015(3) 0.045(3) C28A 0.034(2) 0.069(4) 0.069(3) -0.016(3) 0.023(2) -0.011(2) C29A 0.101(5) 0.035(3) 0.078(4) 0.021(3) 0.013(4) -0.007(3) C30A 0.089(5) 0.132(6) 0.028(3) 0.022(3) -0.003(3) -0.049(4) C31A 0.058(3) 0.048(3) 0.061(3) -0.002(3) 0.030(3) -0.015(2) C32A 0.034(2) 0.026(2) 0.035(2) -0.0001(18) 0.0034(17) 0.0009(17) C33A 0.028(2) 0.030(2) 0.032(2) 0.0040(17) 0.0079(16) 0.0032(16) C34A 0.031(2) 0.028(2) 0.048(3) -0.0026(19) 0.0001(18) 0.0023(16) C35A 0.060(3) 0.031(2) 0.049(3) 0.006(2) -0.003(2) 0.005(2) C36A 0.038(3) 0.050(3) 0.044(3) 0.011(2) 0.006(2) 0.015(2) C37A 0.035(2) 0.065(4) 0.047(3) 0.005(2) -0.007(2) 0.003(2) C38A 0.031(2) 0.038(3) 0.052(3) 0.003(2) -0.0020(19) -0.0077(17) C39A 0.029(2) 0.034(2) 0.031(2) -0.0074(18) 0.0058(17) -0.0033(17) C40A 0.034(2) 0.047(3) 0.041(3) 0.003(2) 0.012(2) 0.000(2) C41A 0.050(3) 0.083(4) 0.048(3) 0.013(3) 0.024(2) -0.008(3) C42A 0.038(3) 0.076(4) 0.050(3) -0.018(3) 0.016(2) 0.001(3) C43A 0.045(3) 0.039(3) 0.075(4) -0.019(3) 0.018(3) 0.007(2) C44A 0.038(2) 0.036(3) 0.048(3) -0.006(2) 0.011(2) -0.0006(19) C45A 0.029(2) 0.023(2) 0.041(2) 0.0018(18) 0.0053(17) 0.0006(16) C46A 0.050(3) 0.041(3) 0.055(3) -0.006(2) 0.000(2) -0.016(2) C47A 0.062(4) 0.045(3) 0.069(4) -0.020(3) -0.003(3) -0.017(3) C48A 0.038(3) 0.032(3) 0.119(6) 0.000(3) 0.000(3) -0.010(2) C49A 0.050(3) 0.035(3) 0.098(5) 0.016(3) 0.031(3) -0.004(2) C50A 0.036(2) 0.029(2) 0.059(3) 0.005(2) 0.015(2) 0.0005(17) Li1B 0.017(3) 0.029(4) 0.030(4) -0.002(3) 0.002(2) -0.003(2) Li2B 0.025(3) 0.024(3) 0.028(3) -0.001(3) 0.001(3) 0.000(2) N1B 0.0255(17) 0.0242(17) 0.0259(18) -0.0008(13) 0.0050(13) -0.0034(12) N2B 0.0246(17) 0.0203(16) 0.0252(17) -0.0006(13) 0.0057(13) 0.0006(12) Si1B 0.0445(12) 0.0337(9) 0.0229(11) 0.0048(7) 0.0045(9) -0.0136(7) Si2B 0.0244(6) 0.0374(6) 0.0280(6) -0.0062(5) 0.0008(4) 0.0075(5) Si3B 0.0253(6) 0.0293(6) 0.0420(7) -0.0083(5) 0.0100(5) -0.0017(5) Si4B 0.0318(6) 0.0291(6) 0.0335(6) 0.0072(5) 0.0060(5) -0.0027(4) P1B 0.0251(5) 0.0223(5) 0.0302(6) -0.0037(4) 0.0061(4) -0.0048(4) P2B 0.0259(5) 0.0255(5) 0.0310(6) -0.0030(4) 0.0061(4) -0.0032(4) C1B 0.034(2) 0.033(2) 0.029(2) -0.0050(18) 0.0050(17) -0.0064(17) C2B 0.027(2) 0.032(2) 0.030(2) 0.0001(17) 0.0064(16) -0.0049(16) C3B 0.055(3) 0.032(3) 0.046(3) 0.000(2) -0.011(2) 0.001(2) C4B 0.065(4) 0.031(3) 0.056(3) -0.005(2) -0.002(2) 0.010(2) C5B 0.055(3) 0.044(3) 0.054(3) 0.012(2) 0.005(2) 0.010(2) C6B 0.040(3) 0.057(4) 0.140(6) 0.023(4) -0.032(3) -0.008(3) C7B 0.046(3) 0.037(3) 0.102(5) 0.012(3) -0.022(3) -0.007(2) C8B 0.027(2) 0.030(2) 0.027(2) -0.0033(17) 0.0040(15) -0.0120(16) C9B 0.043(3) 0.032(2) 0.041(3) 0.0032(19) 0.011(2) -0.0038(19) C10B 0.049(3) 0.049(3) 0.043(3) 0.005(2) 0.017(2) -0.009(2) C11B 0.045(3) 0.046(3) 0.053(3) -0.010(2) 0.021(2) -0.008(2) C12B 0.039(3) 0.042(3) 0.049(3) -0.006(2) 0.014(2) 0.001(2) C13B 0.044(3) 0.027(2) 0.039(3) -0.0030(18) 0.015(2) -0.0029(18) C14B 0.026(2) 0.025(2) 0.039(2) -0.0011(18) 0.0001(17) -0.0042(16) C15B 0.052(3) 0.036(3) 0.039(3) -0.003(2) 0.005(2) -0.013(2) C16B 0.049(3) 0.043(3) 0.075(4) -0.011(3) 0.005(3) -0.021(2) C17B 0.047(3) 0.025(2) 0.088(4) -0.002(2) 0.022(3) -0.010(2) C18B 0.049(3) 0.041(3) 0.087(4) 0.012(3) 0.034(3) -0.010(2) C19B 0.040(3) 0.039(3) 0.041(3) -0.002(2) 0.014(2) -0.0025(19) C20B 0.085(5) 0.024(3) 0.094(6) 0.020(4) 0.011(4) -0.005(3) C21B 0.081(6) 0.157(8) 0.032(4) 0.028(4) -0.007(3) -0.052(6) C22B 0.058(4) 0.055(4) 0.049(4) -0.011(3) 0.032(3) -0.027(3) C23B 0.040(2) 0.051(3) 0.041(3) -0.019(2) 0.0083(19) 0.004(2) C24B 0.049(3) 0.076(4) 0.043(3) -0.012(3) -0.005(2) 0.032(3) C25B 0.036(2) 0.057(3) 0.051(3) -0.007(2) 0.0166(19) -0.006(2) C26B 0.052(3) 0.031(3) 0.083(4) -0.015(2) 0.018(3) 0.003(2) C27B 0.029(2) 0.075(4) 0.076(4) -0.031(3) 0.015(2) -0.009(2) C28B 0.065(3) 0.058(3) 0.039(3) -0.016(2) 0.019(2) -0.018(3) C29B 0.048(3) 0.054(3) 0.051(3) 0.018(2) 0.013(2) -0.018(2) C30B 0.049(3) 0.052(3) 0.047(3) 0.023(2) 0.001(2) 0.006(2) C31B 0.051(3) 0.051(3) 0.031(2) 0.002(2) 0.0101(19) -0.001(2) C32B 0.031(2) 0.032(2) 0.032(2) -0.0043(18) 0.0014(17) -0.0063(17) C33B 0.023(2) 0.027(2) 0.034(2) -0.0022(17) 0.0045(16) -0.0005(15) C34B 0.044(3) 0.039(3) 0.060(3) -0.016(2) -0.006(2) 0.012(2) C35B 0.049(3) 0.044(3) 0.067(4) -0.012(3) -0.003(3) 0.013(2) C36B 0.031(2) 0.050(3) 0.052(3) 0.008(2) 0.0044(19) 0.012(2) C37B 0.051(3) 0.052(3) 0.065(4) 0.009(3) -0.016(2) -0.001(2) C38B 0.046(3) 0.039(3) 0.051(3) -0.002(2) -0.015(2) -0.013(2) C39B 0.025(2) 0.029(2) 0.031(2) -0.0074(17) 0.0059(16) -0.0027(16) C40B 0.034(2) 0.035(2) 0.037(2) -0.0036(19) 0.0102(18) -0.0059(18) C41B 0.045(3) 0.059(3) 0.037(3) -0.005(2) 0.018(2) -0.014(2) C42B 0.035(3) 0.066(3) 0.037(3) -0.017(2) 0.0111(19) -0.001(2) C43B 0.037(3) 0.051(3) 0.045(3) -0.020(2) 0.002(2) 0.009(2) C44B 0.029(2) 0.048(3) 0.037(2) -0.004(2) 0.0051(18) 0.0027(19) C45B 0.024(2) 0.030(2) 0.037(2) -0.0040(18) 0.0050(16) 0.0005(16) C46B 0.058(3) 0.046(3) 0.036(3) -0.012(2) 0.011(2) -0.017(2) C47B 0.059(3) 0.036(3) 0.042(3) -0.014(2) 0.005(2) -0.013(2) C48B 0.033(2) 0.029(2) 0.070(3) -0.008(2) 0.005(2) -0.0045(19) C49B 0.045(3) 0.035(3) 0.068(3) -0.002(2) 0.029(2) -0.006(2) C50B 0.033(2) 0.034(2) 0.046(3) -0.0083(19) 0.0142(19) -0.0043(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 Li1A N2A 2.057(8) . ? Li1A N1A 2.062(8) . ? Li1A C1A 2.302(8) . ? Li2A N2A 2.067(8) . ? Li2A N1A 2.093(8) . ? Li2A C32A 2.285(9) . ? N1A Si2A 1.687(3) . ? N1A Si1A 1.706(4) . ? N2A Si4A 1.669(3) . ? N2A Si3A 1.705(3) . ? N2A Si4C 1.843(15) . ? Si1A C20A 1.867(5) . ? Si1A C21A 1.888(5) . ? Si1A C22A 1.894(5) . ? Si2A C23A 1.870(5) . ? Si2A C25A 1.882(5) . ? Si2A C24A 1.900(5) . ? Si3A C27A 1.865(5) . ? Si3A C26A 1.874(4) . ? Si3A C28A 1.904(5) . ? Si4A C30A 1.881(5) . ? Si4A C31A 1.892(5) . ? Si4A C29A 1.893(5) . ? Si4C C31C 1.886(16) . ? Si4C C29C 1.887(16) . ? Si4C C30C 1.897(16) . ? P1A C1A 1.698(4) . ? P1A C8A 1.803(4) . ? P1A C2A 1.804(5) . ? P1A C14A 1.820(4) . ? P2A C32A 1.705(4) . ? P2A C33A 1.814(4) . ? P2A C39A 1.820(4) . ? P2A C45A 1.843(4) . ? C2A C3A 1.370(7) . ? C2A C7A 1.410(7) . ? C3A C4A 1.377(7) . ? C4A C5A 1.370(8) . ? C5A C6A 1.408(8) . ? C6A C7A 1.397(7) . ? C8A C9A 1.385(6) . ? C8A C13A 1.398(7) . ? C9A C10A 1.389(7) . ? C10A C11A 1.352(9) . ? C11A C12A 1.388(9) . ? C12A C13A 1.398(7) . ? C14A C15A 1.395(6) . ? C14A C19A 1.402(6) . ? C15A C16A 1.391(6) . ? C16A C17A 1.390(7) . ? C17A C18A 1.354(7) . ? C18A C19A 1.389(6) . ? C33A C38A 1.392(6) . ? C33A C34A 1.393(6) . ? C34A C35A 1.398(6) . ? C35A C36A 1.374(7) . ? C36A C37A 1.345(7) . ? C37A C38A 1.387(6) . ? C39A C40A 1.374(7) . ? C39A C44A 1.389(7) . ? C40A C41A 1.388(7) . ? C41A C42A 1.381(8) . ? C42A C43A 1.382(8) . ? C43A C44A 1.382(7) . ? C45A C50A 1.369(6) . ? C45A C46A 1.380(7) . ? C46A C47A 1.378(7) . ? C47A C48A 1.384(9) . ? C48A C49A 1.375(9) . ? C49A C50A 1.398(7) . ? Li1B N1B 2.054(8) . ? Li1B N2B 2.068(8) . ? Li1B C1B 2.264(8) . ? Li2B N2B 2.046(8) . ? Li2B N1B 2.108(8) . ? Li2B C32B 2.254(8) . ? N1B Si1B 1.683(4) . ? N1B Si2B 1.694(3) . ? N1B Si1D 1.754(13) . ? N2B Si4B 1.694(3) . ? N2B Si3B 1.706(3) . ? Si1B C21B 1.880(7) . ? Si1B C22B 1.889(6) . ? Si1B C20B 1.910(6) . ? Si1D C21D 1.868(15) . ? Si1D C22D 1.885(14) . ? Si1D C20D 1.902(15) . ? Si2B C23B 1.870(4) . ? Si2B C24B 1.877(5) . ? Si2B C25B 1.884(5) . ? Si3B C27B 1.867(5) . ? Si3B C28B 1.879(5) . ? Si3B C26B 1.889(5) . ? Si4B C31B 1.873(5) . ? Si4B C29B 1.886(4) . ? Si4B C30B 1.889(5) . ? P1B C1B 1.701(4) . ? P1B C2B 1.807(5) . ? P1B C8B 1.809(4) . ? P1B C14B 1.813(4) . ? P2B C32B 1.707(4) . ? P2B C33B 1.806(4) . ? P2B C39B 1.814(4) . ? P2B C45B 1.839(4) . ? C2B C3B 1.366(6) . ? C2B C7B 1.383(7) . ? C3B C4B 1.382(7) . ? C4B C5B 1.362(8) . ? C5B C6B 1.382(8) . ? C6B C7B 1.390(8) . ? C8B C9B 1.393(6) . ? C8B C13B 1.394(6) . ? C9B C10B 1.400(7) . ? C10B C11B 1.358(7) . ? C11B C12B 1.374(7) . ? C12B C13B 1.403(6) . ? C14B C15B 1.396(6) . ? C14B C19B 1.397(6) . ? C15B C16B 1.399(7) . ? C16B C17B 1.365(8) . ? C17B C18B 1.354(8) . ? C18B C19B 1.394(7) . ? C33B C34B 1.382(6) . ? C33B C38B 1.392(6) . ? C34B C35B 1.405(7) . ? C35B C36B 1.351(7) . ? C36B C37B 1.340(8) . ? C37B C38B 1.374(7) . ? C39B C40B 1.368(6) . ? C39B C44B 1.384(6) . ? C40B C41B 1.391(7) . ? C41B C42B 1.394(8) . ? C42B C43B 1.352(8) . ? C43B C44B 1.385(7) . ? C45B C50B 1.360(6) . ? C45B C46B 1.384(6) . ? C46B C47B 1.379(7) . ? C47B C48B 1.344(7) . ? C48B C49B 1.384(7) . ? C49B C50B 1.400(6) . ? 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 N2A Li1A N1A 104.2(3) . . ? N2A Li1A C1A 116.0(3) . . ? N1A Li1A C1A 138.6(4) . . ? N2A Li2A N1A 102.8(4) . . ? N2A Li2A C32A 140.4(4) . . ? N1A Li2A C32A 115.6(3) . . ? Si2A N1A Si1A 121.6(2) . . ? Si2A N1A Li1A 121.5(3) . . ? Si1A N1A Li1A 107.4(3) . . ? Si2A N1A Li2A 103.5(3) . . ? Si1A N1A Li2A 118.3(3) . . ? Li1A N1A Li2A 76.2(3) . . ? Si4A N2A Si3A 122.9(2) . . ? Si3A N2A Si4C 121.1(6) . . ? Si4A N2A Li1A 106.5(3) . . ? Si3A N2A Li1A 109.9(2) . . ? Si4C N2A Li1A 125.1(7) . . ? Si4A N2A Li2A 124.5(3) . . ? Si3A N2A Li2A 105.8(3) . . ? Si4C N2A Li2A 105.5(7) . . ? Li1A N2A Li2A 76.9(3) . . ? N1A Si1A C20A 114.2(2) . . ? N1A Si1A C21A 116.4(2) . . ? C20A Si1A C21A 104.7(2) . . ? N1A Si1A C22A 110.9(2) . . ? C20A Si1A C22A 106.2(3) . . ? C21A Si1A C22A 103.5(3) . . ? N1A Si2A C23A 111.3(2) . . ? N1A Si2A C25A 112.8(2) . . ? C23A Si2A C25A 106.3(2) . . ? N1A Si2A C24A 113.7(2) . . ? C23A Si2A C24A 105.0(2) . . ? C25A Si2A C24A 107.1(2) . . ? N2A Si3A C27A 115.6(2) . . ? N2A Si3A C26A 113.3(2) . . ? C27A Si3A C26A 106.0(2) . . ? N2A Si3A C28A 110.57(19) . . ? C27A Si3A C28A 104.1(3) . . ? C26A Si3A C28A 106.5(2) . . ? N2A Si4A C30A 114.4(2) . . ? N2A Si4A C31A 112.1(2) . . ? C30A Si4A C31A 104.7(3) . . ? N2A Si4A C29A 114.5(2) . . ? C30A Si4A C29A 105.4(3) . . ? C31A Si4A C29A 104.7(3) . . ? N2A Si4C C31C 113(2) . . ? N2A Si4C C29C 106(2) . . ? C31C Si4C C29C 105.7(12) . . ? N2A Si4C C30C 122(2) . . ? C31C Si4C C30C 104.4(12) . . ? C29C Si4C C30C 104.9(12) . . ? C1A P1A C8A 110.0(2) . . ? C1A P1A C2A 110.2(2) . . ? C8A P1A C2A 109.6(2) . . ? C1A P1A C14A 120.3(2) . . ? C8A P1A C14A 103.2(2) . . ? C2A P1A C14A 103.0(2) . . ? C32A P2A C33A 110.3(2) . . ? C32A P2A C39A 109.9(2) . . ? C33A P2A C39A 109.5(2) . . ? C32A P2A C45A 120.5(2) . . ? C33A P2A C45A 103.1(2) . . ? C39A P2A C45A 103.0(2) . . ? P1A C1A Li1A 136.6(3) . . ? C3A C2A C7A 119.2(4) . . ? C3A C2A P1A 120.4(4) . . ? C7A C2A P1A 120.3(4) . . ? C2A C3A C4A 121.3(5) . . ? C5A C4A C3A 121.1(5) . . ? C4A C5A C6A 118.5(5) . . ? C7A C6A C5A 120.6(5) . . ? C6A C7A C2A 119.0(5) . . ? C9A C8A C13A 118.7(4) . . ? C9A C8A P1A 123.1(4) . . ? C13A C8A P1A 118.1(3) . . ? C8A C9A C10A 120.4(5) . . ? C11A C10A C9A 120.4(5) . . ? C10A C11A C12A 121.3(5) . . ? C11A C12A C13A 118.6(6) . . ? C12A C13A C8A 120.6(5) . . ? C15A C14A C19A 118.2(4) . . ? C15A C14A P1A 123.5(3) . . ? C19A C14A P1A 118.2(3) . . ? C16A C15A C14A 121.2(4) . . ? C17A C16A C15A 119.0(4) . . ? C18A C17A C16A 120.7(4) . . ? C17A C18A C19A 121.0(5) . . ? C18A C19A C14A 120.0(4) . . ? P2A C32A Li2A 133.6(3) . . ? C38A C33A C34A 118.4(4) . . ? C38A C33A P2A 122.6(3) . . ? C34A C33A P2A 118.8(3) . . ? C33A C34A C35A 120.3(4) . . ? C36A C35A C34A 119.3(5) . . ? C37A C36A C35A 121.2(5) . . ? C36A C37A C38A 120.5(5) . . ? C37A C38A C33A 120.2(4) . . ? C40A C39A C44A 119.6(4) . . ? C40A C39A P2A 122.5(4) . . ? C44A C39A P2A 117.6(3) . . ? C39A C40A C41A 120.5(5) . . ? C42A C41A C40A 119.9(5) . . ? C41A C42A C43A 119.6(5) . . ? C42A C43A C44A 120.5(5) . . ? C43A C44A C39A 119.8(5) . . ? C50A C45A C46A 120.3(4) . . ? C50A C45A P2A 118.5(4) . . ? C46A C45A P2A 121.1(4) . . ? C47A C46A C45A 119.7(5) . . ? C46A C47A C48A 120.3(5) . . ? C49A C48A C47A 120.1(5) . . ? C48A C49A C50A 119.3(5) . . ? C45A C50A C49A 120.2(5) . . ? N1B Li1B N2B 104.5(3) . . ? N1B Li1B C1B 137.4(4) . . ? N2B Li1B C1B 116.0(3) . . ? N2B Li2B N1B 103.4(3) . . ? N2B Li2B C32B 140.6(4) . . ? N1B Li2B C32B 115.2(3) . . ? Si1B N1B Si2B 122.8(2) . . ? Si2B N1B Si1D 119.9(5) . . ? Si1B N1B Li1B 121.9(3) . . ? Si2B N1B Li1B 108.9(2) . . ? Si1D N1B Li1B 115.5(7) . . ? Si1B N1B Li2B 104.2(3) . . ? Si2B N1B Li2B 112.7(3) . . ? Si1D N1B Li2B 116.0(7) . . ? Li1B N1B Li2B 75.5(3) . . ? Si4B N2B Si3B 120.9(2) . . ? Si4B N2B Li2B 107.2(3) . . ? Si3B N2B Li2B 121.5(3) . . ? Si4B N2B Li1B 118.9(3) . . ? Si3B N2B Li1B 104.0(2) . . ? Li2B N2B Li1B 76.6(3) . . ? N1B Si1B C21B 113.3(3) . . ? N1B Si1B C22B 111.8(2) . . ? C21B Si1B C22B 105.6(3) . . ? N1B Si1B C20B 116.7(4) . . ? C21B Si1B C20B 104.6(4) . . ? C22B Si1B C20B 103.8(3) . . ? N1B Si1D C21D 126.8(17) . . ? N1B Si1D C22D 112.8(13) . . ? C21D Si1D C22D 106.5(10) . . ? N1B Si1D C20D 98.5(19) . . ? C21D Si1D C20D 105.0(10) . . ? C22D Si1D C20D 104.5(10) . . ? N1B Si2B C23B 113.38(19) . . ? N1B Si2B C24B 115.9(2) . . ? C23B Si2B C24B 105.9(2) . . ? N1B Si2B C25B 110.64(19) . . ? C23B Si2B C25B 106.2(2) . . ? C24B Si2B C25B 103.9(3) . . ? N2B Si3B C27B 113.7(2) . . ? N2B Si3B C28B 111.7(2) . . ? C27B Si3B C28B 106.2(3) . . ? N2B Si3B C26B 114.34(19) . . ? C27B Si3B C26B 106.8(2) . . ? C28B Si3B C26B 103.3(2) . . ? N2B Si4B C31B 109.90(18) . . ? N2B Si4B C29B 113.4(2) . . ? C31B Si4B C29B 107.8(2) . . ? N2B Si4B C30B 117.0(2) . . ? C31B Si4B C30B 104.2(2) . . ? C29B Si4B C30B 103.9(2) . . ? C1B P1B C2B 110.9(2) . . ? C1B P1B C8B 109.1(2) . . ? C2B P1B C8B 108.8(2) . . ? C1B P1B C14B 119.3(2) . . ? C2B P1B C14B 104.2(2) . . ? C8B P1B C14B 103.9(2) . . ? C32B P2B C33B 110.3(2) . . ? C32B P2B C39B 110.2(2) . . ? C33B P2B C39B 109.9(2) . . ? C32B P2B C45B 119.5(2) . . ? C33B P2B C45B 102.9(2) . . ? C39B P2B C45B 103.48(19) . . ? P1B C1B Li1B 135.0(3) . . ? C3B C2B C7B 117.1(5) . . ? C3B C2B P1B 120.3(4) . . ? C7B C2B P1B 122.6(4) . . ? C2B C3B C4B 122.1(5) . . ? C5B C4B C3B 120.4(5) . . ? C4B C5B C6B 119.2(5) . . ? C5B C6B C7B 119.4(5) . . ? C2B C7B C6B 121.8(5) . . ? C9B C8B C13B 119.2(4) . . ? C9B C8B P1B 122.0(4) . . ? C13B C8B P1B 118.6(3) . . ? C8B C9B C10B 119.2(5) . . ? C11B C10B C9B 120.7(5) . . ? C10B C11B C12B 121.6(5) . . ? C11B C12B C13B 118.4(5) . . ? C8B C13B C12B 120.9(4) . . ? C15B C14B C19B 118.9(4) . . ? C15B C14B P1B 122.1(3) . . ? C19B C14B P1B 119.0(3) . . ? C14B C15B C16B 120.2(5) . . ? C17B C16B C15B 119.2(5) . . ? C18B C17B C16B 121.8(5) . . ? C17B C18B C19B 120.2(5) . . ? C18B C19B C14B 119.7(5) . . ? P2B C32B Li2B 136.7(3) . . ? C34B C33B C38B 118.8(4) . . ? C34B C33B P2B 119.4(4) . . ? C38B C33B P2B 121.7(3) . . ? C33B C34B C35B 120.3(5) . . ? C36B C35B C34B 118.9(5) . . ? C37B C36B C35B 121.4(5) . . ? C36B C37B C38B 121.4(5) . . ? C37B C38B C33B 119.2(5) . . ? C40B C39B C44B 119.2(4) . . ? C40B C39B P2B 122.2(3) . . ? C44B C39B P2B 118.3(3) . . ? C39B C40B C41B 120.4(5) . . ? C40B C41B C42B 119.5(5) . . ? C43B C42B C41B 119.9(5) . . ? C42B C43B C44B 120.5(5) . . ? C39B C44B C43B 120.4(5) . . ? C50B C45B C46B 119.0(4) . . ? C50B C45B P2B 118.7(3) . . ? C46B C45B P2B 122.3(3) . . ? C47B C46B C45B 120.2(5) . . ? C48B C47B C46B 121.1(5) . . ? C47B C48B C49B 119.8(5) . . ? C48B C49B C50B 119.2(4) . . ? C45B C50B C49B 120.7(4) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.703 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.078 data_2b _database_code_depnum_ccdc_archive 'CCDC 894053' #TrackingRef 'Chem Sci 07-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H70 Ca N2 P2 Si4, 2(C7 H8)' _chemical_formula_sum 'C64 H86 Ca N2 P2 Si4' _chemical_formula_weight 1097.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.6079(11) _cell_length_b 12.39475(17) _cell_length_c 22.0579(8) _cell_angle_alpha 90.00 _cell_angle_beta 128.948(6) _cell_angle_gamma 90.00 _cell_volume 6508.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12505 _cell_measurement_theta_min 3.0421 _cell_measurement_theta_max 32.6416 _exptl_crystal_description 'tabular needles' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) 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 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37332 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 32.72 _reflns_number_total 10982 _reflns_number_gt 8561 _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^)+(0.0805P)^2^+3.1897P] 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 10982 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Ca1 Ca 0.5000 0.29066(3) 0.2500 0.02119(8) Uani 1 2 d S . . N1 N 0.48998(5) 0.19682(9) 0.33371(7) 0.0248(2) Uani 1 1 d . . . Si2 Si 0.550998(17) 0.13187(3) 0.40329(2) 0.02741(9) Uani 1 1 d . . . C3 C 0.60296(7) 0.15272(14) 0.38557(11) 0.0386(3) Uani 1 1 d . . . H3A H 0.6376 0.1130 0.4248 0.058 Uiso 1 1 calc R . . H3B H 0.6115 0.2298 0.3892 0.058 Uiso 1 1 calc R . . H3C H 0.5870 0.1262 0.3335 0.058 Uiso 1 1 calc R . . C4 C 0.58819(8) 0.18412(18) 0.50557(10) 0.0469(4) Uani 1 1 d . . . H4A H 0.5995 0.1232 0.5410 0.070 Uiso 1 1 calc R . . H4B H 0.5628 0.2313 0.5062 0.070 Uiso 1 1 calc R . . H4C H 0.6216 0.2250 0.5225 0.070 Uiso 1 1 calc R . . C5 C 0.54475(9) -0.01874(14) 0.40692(14) 0.0504(5) Uani 1 1 d . . . H5A H 0.5645 -0.0413 0.4610 0.076 Uiso 1 1 calc R . . H5B H 0.5615 -0.0546 0.3863 0.076 Uiso 1 1 calc R . . H5C H 0.5050 -0.0387 0.3753 0.076 Uiso 1 1 calc R . . Si6 Si 0.431900(16) 0.18513(3) 0.32683(2) 0.02593(9) Uani 1 1 d . . . C7 C 0.37560(6) 0.28323(13) 0.25461(10) 0.0328(3) Uani 1 1 d . . . H7A H 0.3909 0.3567 0.2684 0.049 Uiso 1 1 calc R . . H7B H 0.3441 0.2784 0.2555 0.049 Uiso 1 1 calc R . . H7C H 0.3625 0.2658 0.2022 0.049 Uiso 1 1 calc R . . C8 C 0.44522(8) 0.20936(18) 0.42151(10) 0.0446(4) Uani 1 1 d . . . H8A H 0.4640 0.2791 0.4432 0.067 Uiso 1 1 calc R . . H8B H 0.4692 0.1518 0.4585 0.067 Uiso 1 1 calc R . . H8C H 0.4094 0.2098 0.4121 0.067 Uiso 1 1 calc R . . C9 C 0.39607(8) 0.04959(14) 0.29233(13) 0.0457(4) Uani 1 1 d . . . H9A H 0.3878 0.0313 0.2428 0.069 Uiso 1 1 calc R . . H9B H 0.3610 0.0525 0.2849 0.069 Uiso 1 1 calc R . . H9C H 0.4208 -0.0055 0.3313 0.069 Uiso 1 1 calc R . . C10 C 0.57269(6) 0.45087(11) 0.32235(8) 0.0280(3) Uani 1 1 d . . . H10A H 0.6086 0.4181 0.3405 0.034 Uiso 1 1 calc R . . H10B H 0.5617 0.5002 0.2795 0.034 Uiso 1 1 calc R . . P11 P 0.592282(14) 0.53661(3) 0.396854(19) 0.02242(8) Uani 1 1 d . . . C12 C 0.53331(5) 0.57119(11) 0.39331(7) 0.0239(2) Uani 1 1 d . . . C13 C 0.50261(7) 0.48803(12) 0.39380(9) 0.0310(3) Uani 1 1 d . . . H13A H 0.5127 0.4149 0.3958 0.037 Uiso 1 1 calc R . . C14 C 0.45712(7) 0.51311(14) 0.39129(10) 0.0375(3) Uani 1 1 d . . . H14A H 0.4368 0.4568 0.3928 0.045 Uiso 1 1 calc R . . C15 C 0.44143(7) 0.61925(15) 0.38661(10) 0.0376(3) Uani 1 1 d . . . H15A H 0.4099 0.6356 0.3839 0.045 Uiso 1 1 calc R . . C16 C 0.47151(7) 0.70149(13) 0.38582(10) 0.0359(3) Uani 1 1 d . . . H16A H 0.4606 0.7744 0.3825 0.043 Uiso 1 1 calc R . . C17 C 0.51764(6) 0.67805(12) 0.38980(9) 0.0299(3) Uani 1 1 d . . . H17A H 0.5386 0.7350 0.3901 0.036 Uiso 1 1 calc R . . C18 C 0.62148(6) 0.66594(11) 0.39963(8) 0.0266(3) Uani 1 1 d . . . C19 C 0.59516(9) 0.72038(14) 0.32923(11) 0.0441(4) Uani 1 1 d . . . H19A H 0.5637 0.6889 0.2821 0.053 Uiso 1 1 calc R . . C20 C 0.61481(11) 0.82049(16) 0.32766(14) 0.0562(5) Uani 1 1 d . . . H20A H 0.5964 0.8579 0.2797 0.067 Uiso 1 1 calc R . . C21 C 0.66135(9) 0.86567(14) 0.39622(14) 0.0496(5) Uani 1 1 d . . . H21A H 0.6756 0.9330 0.3950 0.060 Uiso 1 1 calc R . . C22 C 0.68686(9) 0.81348(15) 0.46576(14) 0.0505(5) Uani 1 1 d . . . H22A H 0.7181 0.8457 0.5128 0.061 Uiso 1 1 calc R . . C23 C 0.66719(7) 0.71337(14) 0.46790(10) 0.0402(4) Uani 1 1 d . . . H23A H 0.6852 0.6775 0.5163 0.048 Uiso 1 1 calc R . . C24 C 0.64542(6) 0.47557(12) 0.49043(8) 0.0302(3) Uani 1 1 d . . . C25 C 0.64626(8) 0.49115(17) 0.55327(10) 0.0429(4) Uani 1 1 d . . . H25A H 0.6174 0.5320 0.5471 0.051 Uiso 1 1 calc R . . C26 C 0.68960(9) 0.4466(2) 0.62600(11) 0.0585(6) Uani 1 1 d . . . H26A H 0.6902 0.4573 0.6691 0.070 Uiso 1 1 calc R . . C27 C 0.73129(9) 0.3875(2) 0.63498(13) 0.0635(6) Uani 1 1 d . . . H27A H 0.7604 0.3567 0.6843 0.076 Uiso 1 1 calc R . . C28 C 0.73132(9) 0.3725(2) 0.57343(14) 0.0664(6) Uani 1 1 d . . . H28A H 0.7606 0.3325 0.5804 0.080 Uiso 1 1 calc R . . C29 C 0.68820(8) 0.41627(17) 0.50036(12) 0.0492(4) Uani 1 1 d . . . H29A H 0.6881 0.4056 0.4576 0.059 Uiso 1 1 calc R . . C30 C 0.28838(19) 0.8064(3) 0.2328(2) 0.1051(12) Uani 1 1 d . . . H30A H 0.2564 0.8555 0.2094 0.158 Uiso 1 1 calc R . . H30B H 0.3144 0.8351 0.2251 0.158 Uiso 1 1 calc R . . H30C H 0.3078 0.7995 0.2888 0.158 Uiso 1 1 calc R . . C31 C 0.26793(10) 0.69877(19) 0.19532(13) 0.0558(5) Uani 1 1 d . . . C32 C 0.21407(9) 0.6648(2) 0.16122(14) 0.0609(6) Uani 1 1 d . . . H32A H 0.1891 0.7126 0.1596 0.073 Uiso 1 1 calc R . . C33 C 0.19592(11) 0.5644(3) 0.12988(17) 0.0766(8) Uani 1 1 d . . . H33A H 0.1588 0.5427 0.1078 0.092 Uiso 1 1 calc R . . C34 C 0.23104(14) 0.4932(2) 0.12981(19) 0.0766(7) Uani 1 1 d . . . H34A H 0.2183 0.4234 0.1075 0.092 Uiso 1 1 calc R . . C35 C 0.28354(12) 0.5257(2) 0.16219(16) 0.0672(7) Uani 1 1 d . . . H35A H 0.3080 0.4780 0.1626 0.081 Uiso 1 1 calc R . . C36 C 0.30257(8) 0.6273(2) 0.19489(13) 0.0595(6) Uani 1 1 d . . . H36A H 0.3398 0.6483 0.2173 0.071 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 Ca1 0.02403(16) 0.01837(15) 0.02139(16) 0.000 0.01438(14) 0.000 N1 0.0270(5) 0.0238(5) 0.0255(5) 0.0020(4) 0.0174(5) 0.0000(4) Si2 0.0321(2) 0.02388(18) 0.02835(19) 0.00544(14) 0.01997(17) 0.00519(14) C3 0.0347(8) 0.0403(8) 0.0443(9) 0.0094(7) 0.0265(7) 0.0084(7) C4 0.0405(9) 0.0624(12) 0.0284(8) 0.0015(7) 0.0172(7) 0.0117(8) C5 0.0545(11) 0.0290(8) 0.0689(13) 0.0157(8) 0.0395(11) 0.0090(8) Si6 0.02774(18) 0.02506(18) 0.02666(18) -0.00082(13) 0.01791(16) -0.00447(14) C7 0.0298(7) 0.0348(7) 0.0358(7) 0.0012(6) 0.0215(6) -0.0001(6) C8 0.0389(8) 0.0676(12) 0.0335(8) -0.0024(8) 0.0258(7) -0.0065(8) C9 0.0463(10) 0.0316(8) 0.0564(11) -0.0038(7) 0.0309(9) -0.0120(7) C10 0.0304(6) 0.0277(6) 0.0274(6) -0.0055(5) 0.0189(6) -0.0035(5) P11 0.02225(15) 0.02292(16) 0.02041(15) -0.00076(11) 0.01261(13) -0.00206(11) C12 0.0232(5) 0.0268(6) 0.0198(5) -0.0042(4) 0.0127(5) -0.0029(5) C13 0.0350(7) 0.0281(6) 0.0361(7) -0.0055(5) 0.0254(6) -0.0056(6) C14 0.0392(8) 0.0390(8) 0.0451(9) -0.0113(7) 0.0317(8) -0.0111(7) C15 0.0329(7) 0.0467(9) 0.0377(8) -0.0116(7) 0.0243(7) -0.0029(7) C16 0.0371(8) 0.0346(8) 0.0379(8) -0.0058(6) 0.0245(7) 0.0026(6) C17 0.0330(7) 0.0264(6) 0.0311(7) -0.0032(5) 0.0206(6) -0.0020(5) C18 0.0291(6) 0.0246(6) 0.0300(6) -0.0014(5) 0.0204(6) -0.0037(5) C19 0.0559(11) 0.0364(8) 0.0361(8) 0.0023(6) 0.0271(8) -0.0104(8) C20 0.0808(15) 0.0365(9) 0.0609(13) 0.0079(8) 0.0492(12) -0.0072(10) C21 0.0622(12) 0.0284(8) 0.0772(14) -0.0021(8) 0.0529(12) -0.0085(8) C22 0.0448(10) 0.0337(8) 0.0616(12) -0.0090(8) 0.0279(9) -0.0139(7) C23 0.0354(8) 0.0352(8) 0.0354(8) -0.0036(6) 0.0153(7) -0.0108(6) C24 0.0257(6) 0.0301(7) 0.0261(6) 0.0035(5) 0.0120(5) -0.0036(5) C25 0.0362(8) 0.0583(11) 0.0272(7) 0.0051(7) 0.0166(7) -0.0045(8) C26 0.0476(11) 0.0841(16) 0.0267(8) 0.0112(9) 0.0151(8) -0.0123(11) C27 0.0395(10) 0.0743(15) 0.0399(10) 0.0240(10) 0.0072(8) -0.0009(10) C28 0.0430(11) 0.0728(16) 0.0546(13) 0.0204(11) 0.0168(10) 0.0224(11) C29 0.0388(9) 0.0540(11) 0.0407(9) 0.0082(8) 0.0182(8) 0.0136(8) C30 0.143(3) 0.074(2) 0.100(3) -0.0177(18) 0.077(3) -0.026(2) C31 0.0559(12) 0.0622(13) 0.0448(11) 0.0081(9) 0.0295(10) 0.0006(10) C32 0.0421(10) 0.0913(17) 0.0500(11) 0.0043(12) 0.0292(10) 0.0137(11) C33 0.0544(13) 0.111(2) 0.0722(17) -0.0216(16) 0.0434(13) -0.0212(15) C34 0.091(2) 0.0671(16) 0.0827(19) -0.0067(14) 0.0602(17) -0.0134(15) C35 0.0709(16) 0.0689(15) 0.0747(16) 0.0257(13) 0.0520(14) 0.0314(13) C36 0.0342(9) 0.0846(17) 0.0508(11) 0.0173(11) 0.0225(9) 0.0038(10) _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 Ca1 N1 2.3596(11) 2_655 ? Ca1 N1 2.3596(11) . ? Ca1 C10 2.6413(14) . ? Ca1 C10 2.6413(14) 2_655 ? N1 Si6 1.6928(12) . ? N1 Si2 1.6994(12) . ? Si2 C3 1.8789(16) . ? Si2 C5 1.8833(18) . ? Si2 C4 1.8910(18) . ? Si6 C7 1.8800(16) . ? Si6 C8 1.8833(17) . ? Si6 C9 1.8854(17) . ? C10 P11 1.7178(14) . ? P11 C24 1.8049(15) . ? P11 C12 1.8086(13) . ? P11 C18 1.8175(14) . ? C12 C17 1.3940(19) . ? C12 C13 1.3995(19) . ? C13 C14 1.393(2) . ? C14 C15 1.382(2) . ? C15 C16 1.381(2) . ? C16 C17 1.389(2) . ? C18 C23 1.386(2) . ? C18 C19 1.394(2) . ? C19 C20 1.389(2) . ? C20 C21 1.386(3) . ? C21 C22 1.369(3) . ? C22 C23 1.393(2) . ? C24 C25 1.384(2) . ? C24 C29 1.394(2) . ? C25 C26 1.401(3) . ? C26 C27 1.373(4) . ? C27 C28 1.371(4) . ? C28 C29 1.400(3) . ? C30 C31 1.484(4) . ? C31 C32 1.379(3) . ? C31 C36 1.386(3) . ? C32 C33 1.361(4) . ? C33 C34 1.391(4) . ? C34 C35 1.346(4) . ? C35 C36 1.384(4) . ? 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 N1 Ca1 N1 120.94(6) 2_655 . ? N1 Ca1 C10 111.65(4) 2_655 . ? N1 Ca1 C10 111.86(4) . . ? N1 Ca1 C10 111.86(4) 2_655 2_655 ? N1 Ca1 C10 111.65(4) . 2_655 ? C10 Ca1 C10 82.50(7) . 2_655 ? Si6 N1 Si2 122.43(7) . . ? Si6 N1 Ca1 128.16(6) . . ? Si2 N1 Ca1 109.31(6) . . ? N1 Si2 C3 109.89(7) . . ? N1 Si2 C5 115.13(8) . . ? C3 Si2 C5 105.49(9) . . ? N1 Si2 C4 114.27(7) . . ? C3 Si2 C4 104.33(9) . . ? C5 Si2 C4 106.85(10) . . ? N1 Si6 C7 111.84(6) . . ? N1 Si6 C8 113.82(7) . . ? C7 Si6 C8 106.30(8) . . ? N1 Si6 C9 115.09(8) . . ? C7 Si6 C9 104.09(8) . . ? C8 Si6 C9 104.79(9) . . ? P11 C10 Ca1 134.26(7) . . ? C10 P11 C24 110.88(7) . . ? C10 P11 C12 111.51(7) . . ? C24 P11 C12 107.83(7) . . ? C10 P11 C18 116.51(7) . . ? C24 P11 C18 105.11(7) . . ? C12 P11 C18 104.40(6) . . ? C17 C12 C13 119.41(13) . . ? C17 C12 P11 121.78(10) . . ? C13 C12 P11 118.81(11) . . ? C14 C13 C12 119.63(14) . . ? C15 C14 C13 120.48(15) . . ? C16 C15 C14 120.02(14) . . ? C15 C16 C17 120.27(15) . . ? C16 C17 C12 120.17(14) . . ? C23 C18 C19 119.12(14) . . ? C23 C18 P11 123.35(12) . . ? C19 C18 P11 117.51(12) . . ? C20 C19 C18 120.28(18) . . ? C21 C20 C19 119.86(19) . . ? C22 C21 C20 120.17(16) . . ? C21 C22 C23 120.30(19) . . ? C18 C23 C22 120.23(17) . . ? C25 C24 C29 119.49(15) . . ? C25 C24 P11 121.54(13) . . ? C29 C24 P11 118.88(13) . . ? C24 C25 C26 119.99(19) . . ? C27 C26 C25 120.0(2) . . ? C28 C27 C26 120.55(18) . . ? C27 C28 C29 120.1(2) . . ? C24 C29 C28 119.9(2) . . ? C32 C31 C36 117.3(2) . . ? C32 C31 C30 121.3(3) . . ? C36 C31 C30 121.4(3) . . ? C33 C32 C31 121.5(2) . . ? C32 C33 C34 120.8(2) . . ? C35 C34 C33 118.4(3) . . ? C34 C35 C36 121.3(2) . . ? C35 C36 C31 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.626 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.064 data_2c _database_code_depnum_ccdc_archive 'CCDC 894054' #TrackingRef 'Chem Sci 07-12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H52 N2 P Si4 Y' _chemical_formula_sum 'C31 H52 N2 P Si4 Y' _chemical_formula_weight 684.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Y Y -2.7962 3.5667 '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 11.1459(3) _cell_length_b 20.7732(4) _cell_length_c 16.6276(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.7824(19) _cell_angle_gamma 90.00 _cell_volume 3781.92(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.9786 _cell_measurement_theta_max 32.5938 _exptl_crystal_description tablets _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.732 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.732 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) 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 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39613 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 32.67 _reflns_number_total 12694 _reflns_number_gt 8602 _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^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12694 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Y Y 0.273826(16) 0.236686(8) 0.404571(9) 0.02283(5) Uani 1 1 d . . . C1 C 0.40053(17) 0.20917(9) 0.53948(10) 0.0289(4) Uani 1 1 d . . . H1A H 0.4046 0.2462 0.5774 0.035 Uiso 1 1 calc R . . H1B H 0.3648 0.1720 0.5640 0.035 Uiso 1 1 calc R . . P2 P 0.54553(4) 0.19011(2) 0.52255(3) 0.02542(10) Uani 1 1 d . . . C3 C 0.53393(17) 0.15199(8) 0.42399(10) 0.0267(4) Uani 1 1 d . . . C4 C 0.43552(17) 0.17327(8) 0.36301(10) 0.0267(4) Uani 1 1 d . . . C5 C 0.43539(19) 0.14613(9) 0.28512(11) 0.0346(4) Uani 1 1 d . . . H5A H 0.3725 0.1584 0.2410 0.042 Uiso 1 1 calc R . . C6 C 0.5223(2) 0.10247(10) 0.26983(12) 0.0396(5) Uani 1 1 d . . . H6A H 0.5175 0.0856 0.2162 0.048 Uiso 1 1 calc R . . C7 C 0.6155(2) 0.08340(10) 0.33155(13) 0.0432(5) Uani 1 1 d . . . H7A H 0.6752 0.0536 0.3207 0.052 Uiso 1 1 calc R . . C8 C 0.62169(19) 0.10797(9) 0.40986(12) 0.0371(5) Uani 1 1 d . . . H8A H 0.6851 0.0949 0.4532 0.045 Uiso 1 1 calc R . . C9 C 0.63070(17) 0.26413(8) 0.52058(11) 0.0290(4) Uani 1 1 d . . . C10 C 0.6934(2) 0.27692(10) 0.45864(13) 0.0418(5) Uani 1 1 d . . . H10A H 0.6934 0.2463 0.4162 0.050 Uiso 1 1 calc R . . C11 C 0.7569(2) 0.33443(12) 0.45790(15) 0.0535(6) Uani 1 1 d . . . H11A H 0.7992 0.3432 0.4145 0.064 Uiso 1 1 calc R . . C12 C 0.7588(2) 0.37846(11) 0.51912(15) 0.0519(6) Uani 1 1 d . . . H12A H 0.8026 0.4176 0.5184 0.062 Uiso 1 1 calc R . . C13 C 0.6972(2) 0.36598(11) 0.58172(14) 0.0490(6) Uani 1 1 d . . . H13A H 0.6989 0.3965 0.6244 0.059 Uiso 1 1 calc R . . C14 C 0.6329(2) 0.30939(9) 0.58292(12) 0.0393(5) Uani 1 1 d . . . H14A H 0.5901 0.3012 0.6262 0.047 Uiso 1 1 calc R . . C15 C 0.63708(17) 0.13868(9) 0.59890(10) 0.0292(4) Uani 1 1 d . . . C16 C 0.7551(2) 0.15431(10) 0.63606(12) 0.0425(5) Uani 1 1 d . . . H16A H 0.7914 0.1929 0.6214 0.051 Uiso 1 1 calc R . . C17 C 0.8206(2) 0.11374(12) 0.69468(13) 0.0545(6) Uani 1 1 d . . . H17A H 0.9020 0.1243 0.7196 0.065 Uiso 1 1 calc R . . C18 C 0.7678(2) 0.05852(11) 0.71667(13) 0.0526(6) Uani 1 1 d . . . H18A H 0.8121 0.0314 0.7578 0.063 Uiso 1 1 calc R . . C19 C 0.6516(2) 0.04215(11) 0.67970(14) 0.0516(6) Uani 1 1 d . . . H19A H 0.6159 0.0034 0.6944 0.062 Uiso 1 1 calc R . . C20 C 0.5861(2) 0.08218(10) 0.62077(13) 0.0427(5) Uani 1 1 d . . . H20A H 0.5055 0.0707 0.5952 0.051 Uiso 1 1 calc R . . N21 N 0.11623(13) 0.16822(7) 0.37921(8) 0.0232(3) Uani 1 1 d . . . Si22 Si 0.08879(5) 0.10730(2) 0.44310(3) 0.02591(11) Uani 1 1 d . . . C23 C 0.2290(2) 0.05759(10) 0.47798(13) 0.0460(5) Uani 1 1 d . . . H23A H 0.2957 0.0854 0.5047 0.069 Uiso 1 1 calc R . . H23B H 0.2527 0.0365 0.4306 0.069 Uiso 1 1 calc R . . H23C H 0.2120 0.0249 0.5168 0.069 Uiso 1 1 calc R . . C24 C 0.0383(3) 0.13997(11) 0.53564(14) 0.0713(9) Uani 1 1 d . . . H24A H -0.0356 0.1660 0.5189 0.107 Uiso 1 1 calc R . . H24B H 0.1032 0.1669 0.5666 0.107 Uiso 1 1 calc R . . H24C H 0.0206 0.1043 0.5702 0.107 Uiso 1 1 calc R . . C25 C -0.0317(2) 0.04951(12) 0.39441(14) 0.0628(8) Uani 1 1 d . . . H25A H -0.1080 0.0729 0.3751 0.094 Uiso 1 1 calc R . . H25B H -0.0449 0.0171 0.4347 0.094 Uiso 1 1 calc R . . H25C H -0.0054 0.0283 0.3480 0.094 Uiso 1 1 calc R . . Si26 Si 0.02972(5) 0.18152(2) 0.28498(3) 0.02743(12) Uani 1 1 d . . . C27 C -0.1285(2) 0.20906(11) 0.28823(14) 0.0492(6) Uani 1 1 d . . . H27A H -0.1252 0.2455 0.3261 0.074 Uiso 1 1 calc R . . H27B H -0.1745 0.1737 0.3070 0.074 Uiso 1 1 calc R . . H27C H -0.1690 0.2225 0.2333 0.074 Uiso 1 1 calc R . . C28 C 0.1057(2) 0.24846(9) 0.23629(11) 0.0417(5) Uani 1 1 d . . . H28A H 0.1122 0.2868 0.2713 0.063 Uiso 1 1 calc R . . H28B H 0.0567 0.2587 0.1825 0.063 Uiso 1 1 calc R . . H28C H 0.1874 0.2347 0.2299 0.063 Uiso 1 1 calc R . . C29 C 0.0222(2) 0.11191(10) 0.21239(12) 0.0489(6) Uani 1 1 d . . . H29A H -0.0172 0.0752 0.2340 0.073 Uiso 1 1 calc R . . H29B H 0.1051 0.0998 0.2064 0.073 Uiso 1 1 calc R . . H29C H -0.0252 0.1243 0.1589 0.073 Uiso 1 1 calc R . . N31 N 0.27053(14) 0.34459(7) 0.39646(8) 0.0280(3) Uani 1 1 d . . . Si32 Si 0.18966(5) 0.37786(2) 0.46316(3) 0.03230(13) Uani 1 1 d . . . C33 C 0.2853(3) 0.42185(13) 0.55069(13) 0.0622(7) Uani 1 1 d . . . H33A H 0.3268 0.4579 0.5296 0.093 Uiso 1 1 calc R . . H33B H 0.3462 0.3924 0.5810 0.093 Uiso 1 1 calc R . . H33C H 0.2329 0.4382 0.5873 0.093 Uiso 1 1 calc R . . C34 C 0.1137(2) 0.31001(10) 0.50943(12) 0.0412(5) Uani 1 1 d . . . H34A H 0.0621 0.2855 0.4658 0.062 Uiso 1 1 calc R . . H34B H 0.0633 0.3276 0.5465 0.062 Uiso 1 1 calc R . . H34C H 0.1763 0.2816 0.5400 0.062 Uiso 1 1 calc R . . C35 C 0.0637(3) 0.43306(12) 0.41521(15) 0.0645(7) Uani 1 1 d . . . H35A H 0.0983 0.4697 0.3902 0.097 Uiso 1 1 calc R . . H35B H 0.0199 0.4487 0.4572 0.097 Uiso 1 1 calc R . . H35C H 0.0071 0.4097 0.3730 0.097 Uiso 1 1 calc R . . Si36 Si 0.34615(6) 0.38621(3) 0.33235(3) 0.03681(14) Uani 1 1 d . . . C37 C 0.2389(3) 0.42968(13) 0.24918(14) 0.0730(9) Uani 1 1 d . . . H37A H 0.1802 0.3990 0.2193 0.110 Uiso 1 1 calc R . . H37B H 0.2857 0.4496 0.2113 0.110 Uiso 1 1 calc R . . H37D H 0.1951 0.4631 0.2736 0.110 Uiso 1 1 calc R . . C38 C 0.4559(2) 0.44725(11) 0.38590(14) 0.0549(6) Uani 1 1 d . . . H38A H 0.5132 0.4263 0.4300 0.082 Uiso 1 1 calc R . . H38D H 0.4108 0.4809 0.4090 0.082 Uiso 1 1 calc R . . H38B H 0.5011 0.4665 0.3468 0.082 Uiso 1 1 calc R . . C39 C 0.4364(3) 0.32906(11) 0.27988(14) 0.0605(7) Uani 1 1 d . . . H39D H 0.4942 0.3054 0.3210 0.091 Uiso 1 1 calc R . . H39A H 0.4814 0.3533 0.2445 0.091 Uiso 1 1 calc R . . H39B H 0.3808 0.2986 0.2467 0.091 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 Y 0.02404(9) 0.01849(8) 0.02550(8) 0.00093(6) 0.00343(6) -0.00092(7) C1 0.0242(10) 0.0341(10) 0.0289(9) -0.0010(8) 0.0061(7) 0.0026(8) P2 0.0230(2) 0.0255(2) 0.0272(2) -0.00231(18) 0.00289(18) 0.00171(19) C3 0.0254(10) 0.0238(8) 0.0325(9) -0.0047(7) 0.0092(7) -0.0031(7) C4 0.0302(10) 0.0225(8) 0.0293(9) -0.0022(7) 0.0101(7) -0.0046(7) C5 0.0394(12) 0.0324(10) 0.0320(9) -0.0050(8) 0.0067(8) -0.0041(9) C6 0.0453(13) 0.0371(11) 0.0399(11) -0.0171(9) 0.0166(9) -0.0088(10) C7 0.0371(13) 0.0351(11) 0.0610(13) -0.0191(10) 0.0185(10) 0.0024(10) C8 0.0287(11) 0.0352(11) 0.0467(11) -0.0085(9) 0.0050(9) 0.0026(9) C9 0.0244(10) 0.0260(9) 0.0338(9) -0.0008(8) -0.0016(7) 0.0026(8) C10 0.0397(13) 0.0387(11) 0.0484(12) -0.0096(10) 0.0119(10) -0.0100(10) C11 0.0474(15) 0.0498(14) 0.0657(15) -0.0004(12) 0.0171(12) -0.0163(12) C12 0.0392(14) 0.0339(12) 0.0769(16) -0.0010(12) -0.0041(12) -0.0096(10) C13 0.0481(15) 0.0349(12) 0.0584(14) -0.0140(10) -0.0047(11) -0.0001(10) C14 0.0417(13) 0.0345(11) 0.0395(11) -0.0051(9) 0.0015(9) 0.0002(9) C15 0.0274(10) 0.0293(9) 0.0308(9) 0.0009(8) 0.0052(7) 0.0053(8) C16 0.0389(13) 0.0361(11) 0.0474(12) 0.0050(10) -0.0050(9) 0.0005(10) C17 0.0463(15) 0.0495(14) 0.0582(14) 0.0071(11) -0.0149(11) 0.0055(12) C18 0.0601(17) 0.0467(14) 0.0475(13) 0.0123(11) 0.0011(11) 0.0182(12) C19 0.0557(16) 0.0373(12) 0.0643(14) 0.0161(11) 0.0170(12) 0.0057(11) C20 0.0321(12) 0.0402(12) 0.0548(12) 0.0068(10) 0.0051(10) 0.0009(10) N21 0.0254(8) 0.0225(7) 0.0213(6) 0.0022(6) 0.0032(6) -0.0032(6) Si22 0.0293(3) 0.0226(2) 0.0258(2) 0.00541(19) 0.0051(2) -0.0024(2) C23 0.0433(14) 0.0368(11) 0.0552(12) 0.0150(10) 0.0021(10) 0.0035(10) C24 0.130(3) 0.0408(13) 0.0610(15) 0.0152(12) 0.0644(17) 0.0138(15) C25 0.0557(16) 0.0605(15) 0.0608(14) 0.0357(12) -0.0187(12) -0.0334(13) Si26 0.0336(3) 0.0256(2) 0.0211(2) 0.00294(19) 0.0000(2) -0.0059(2) C27 0.0386(13) 0.0492(13) 0.0544(13) 0.0108(11) -0.0052(10) 0.0031(11) C28 0.0604(16) 0.0371(11) 0.0250(9) 0.0080(8) 0.0013(9) -0.0138(10) C29 0.0693(18) 0.0429(12) 0.0338(10) -0.0068(9) 0.0076(10) -0.0171(12) N31 0.0368(9) 0.0203(7) 0.0248(7) 0.0026(6) 0.0006(6) -0.0031(7) Si32 0.0416(3) 0.0223(2) 0.0306(3) -0.0041(2) 0.0005(2) -0.0002(2) C33 0.077(2) 0.0658(17) 0.0429(12) -0.0230(12) 0.0085(12) -0.0242(15) C34 0.0484(14) 0.0365(11) 0.0432(11) -0.0039(9) 0.0199(10) 0.0005(10) C35 0.070(2) 0.0460(14) 0.0752(16) 0.0017(13) 0.0085(14) 0.0241(13) Si36 0.0500(4) 0.0259(3) 0.0325(3) 0.0079(2) 0.0027(2) -0.0126(3) C37 0.089(2) 0.0636(17) 0.0572(14) 0.0373(13) -0.0106(14) -0.0223(16) C38 0.0606(17) 0.0429(13) 0.0601(14) 0.0011(11) 0.0080(12) -0.0217(12) C39 0.089(2) 0.0484(14) 0.0545(14) 0.0004(12) 0.0393(14) -0.0200(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y N21 2.2381(14) . ? Y N31 2.2454(15) . ? Y C4 2.4346(18) . ? Y C1 2.4835(17) . ? C1 P2 1.7373(19) . ? P2 C3 1.8028(17) . ? P2 C9 1.8106(19) . ? P2 C15 1.8194(18) . ? C3 C8 1.391(3) . ? C3 C4 1.418(2) . ? C4 C5 1.412(2) . ? C5 C6 1.385(3) . ? C6 C7 1.375(3) . ? C7 C8 1.388(3) . ? C9 C10 1.375(3) . ? C9 C14 1.396(3) . ? C10 C11 1.389(3) . ? C11 C12 1.366(3) . ? C12 C13 1.374(3) . ? C13 C14 1.379(3) . ? C15 C20 1.382(3) . ? C15 C16 1.383(3) . ? C16 C17 1.388(3) . ? C17 C18 1.370(3) . ? C18 C19 1.368(3) . ? C19 C20 1.384(3) . ? N21 Si26 1.7017(13) . ? N21 Si22 1.7161(14) . ? Si22 C24 1.863(2) . ? Si22 C25 1.869(2) . ? Si22 C23 1.873(2) . ? Si26 C27 1.865(2) . ? Si26 C29 1.875(2) . ? Si26 C28 1.887(2) . ? N31 Si32 1.7013(16) . ? N31 Si36 1.7119(15) . ? Si32 C35 1.871(2) . ? Si32 C33 1.873(2) . ? Si32 C34 1.881(2) . ? Si36 C38 1.868(2) . ? Si36 C39 1.874(3) . ? Si36 C37 1.881(2) . ? 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 N21 Y N31 128.29(5) . . ? N21 Y C4 101.49(6) . . ? N31 Y C4 121.86(6) . . ? N21 Y C1 108.52(6) . . ? N31 Y C1 106.51(6) . . ? C4 Y C1 78.80(6) . . ? P2 C1 Y 107.17(8) . . ? C1 P2 C3 109.67(9) . . ? C1 P2 C9 108.43(9) . . ? C3 P2 C9 107.78(9) . . ? C1 P2 C15 115.98(9) . . ? C3 P2 C15 108.17(8) . . ? C9 P2 C15 106.49(8) . . ? C8 C3 C4 123.96(16) . . ? C8 C3 P2 120.61(14) . . ? C4 C3 P2 115.31(13) . . ? C5 C4 C3 113.54(17) . . ? C5 C4 Y 127.05(14) . . ? C3 C4 Y 118.71(12) . . ? C6 C5 C4 123.30(19) . . ? C7 C6 C5 120.57(18) . . ? C6 C7 C8 119.48(19) . . ? C7 C8 C3 119.15(19) . . ? C10 C9 C14 119.03(18) . . ? C10 C9 P2 121.30(15) . . ? C14 C9 P2 119.67(16) . . ? C9 C10 C11 120.3(2) . . ? C12 C11 C10 120.4(2) . . ? C11 C12 C13 119.9(2) . . ? C12 C13 C14 120.4(2) . . ? C13 C14 C9 120.0(2) . . ? C20 C15 C16 119.03(18) . . ? C20 C15 P2 118.55(15) . . ? C16 C15 P2 122.42(15) . . ? C15 C16 C17 120.1(2) . . ? C18 C17 C16 120.0(2) . . ? C19 C18 C17 120.4(2) . . ? C18 C19 C20 119.9(2) . . ? C15 C20 C19 120.5(2) . . ? Si26 N21 Si22 123.63(8) . . ? Si26 N21 Y 111.09(7) . . ? Si22 N21 Y 125.20(7) . . ? N21 Si22 C24 111.05(9) . . ? N21 Si22 C25 113.72(8) . . ? C24 Si22 C25 106.73(13) . . ? N21 Si22 C23 111.30(9) . . ? C24 Si22 C23 107.99(11) . . ? C25 Si22 C23 105.69(11) . . ? N21 Si26 C27 113.53(9) . . ? N21 Si26 C29 114.63(9) . . ? C27 Si26 C29 109.07(11) . . ? N21 Si26 C28 106.99(8) . . ? C27 Si26 C28 106.79(11) . . ? C29 Si26 C28 105.17(10) . . ? Si32 N31 Si36 125.69(9) . . ? Si32 N31 Y 111.78(7) . . ? Si36 N31 Y 122.49(8) . . ? N31 Si32 C35 114.70(10) . . ? N31 Si32 C33 114.26(10) . . ? C35 Si32 C33 107.72(12) . . ? N31 Si32 C34 107.22(8) . . ? C35 Si32 C34 105.94(12) . . ? C33 Si32 C34 106.37(11) . . ? N31 Si36 C38 113.62(9) . . ? N31 Si36 C39 109.86(9) . . ? C38 Si36 C39 106.94(12) . . ? N31 Si36 C37 112.41(11) . . ? C38 Si36 C37 107.09(12) . . ? C39 Si36 C37 106.53(13) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.524 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.071 #===END