# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1468 data_sep299 _audit_creation_date 1999-09-02T14:03:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H53 N2 P3 Si' _chemical_formula_structural 'C31 H53 N2 P3 SI' _chemical_formula_sum 'C31 H53 N2 P3 Si' _chemical_formula_weight 574.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0632(18) _cell_length_b 11.090(5) _cell_length_c 15.682(7) _cell_angle_alpha 77.81(4) _cell_angle_beta 76.87(3) _cell_angle_gamma 62.15(3) _cell_volume 1644.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.3 _cell_measurement_theta_max 8.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION (NOT APPLIED) # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_T_min 0.9316 _exptl_absorpt_correction_T_max 0.9537 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.33094E-1 _diffrn_orient_matrix_ub_12 0.53927E-1 _diffrn_orient_matrix_ub_13 -0.50896E-1 _diffrn_orient_matrix_ub_21 -0.86805E-1 _diffrn_orient_matrix_ub_22 0.31917E-1 _diffrn_orient_matrix_ub_23 -0.25283E-1 _diffrn_orient_matrix_ub_31 -0.45375E-1 _diffrn_orient_matrix_ub_32 0.81342E-1 _diffrn_orient_matrix_ub_33 0.33494E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_standards_decay_corr_max 1.049 _diffrn_standards_decay_corr_min 0.978 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 4 1 -1 3 -2 _diffrn_reflns_number 5781 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 5781 _reflns_number_gt 4575 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0310P)^2^+3.8836P] 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_number_reflns 5781 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.402 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' P P 0.1023 0.0942 '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' 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 Si Si 0.84864(9) 0.54764(9) 0.26806(6) 0.0177(2) Uani 1 1 d . . . P1 P 0.96340(9) 0.66527(9) 0.17899(6) 0.0192(2) Uani 1 1 d . . . P2 P 0.66043(9) 0.84311(9) 0.24524(6) 0.0230(2) Uani 1 1 d . . . P3 P 0.87001(10) 0.72955(10) 0.37047(6) 0.0228(2) Uani 1 1 d . . . N1 N 0.9427(3) 0.3877(3) 0.32359(19) 0.0220(6) Uani 1 1 d . . . N2 N 0.7533(3) 0.4858(3) 0.23196(19) 0.0205(6) Uani 1 1 d . . . C1 C 0.7372(3) 0.7031(3) 0.3338(2) 0.0187(7) Uani 1 1 d . . . C2 C 0.7948(4) 0.8137(3) 0.1628(2) 0.0214(8) Uani 1 1 d . . . C3 C 0.9895(4) 0.7075(3) 0.2798(2) 0.0218(8) Uani 1 1 d . . . C4 C 0.6226(4) 0.6985(4) 0.4133(2) 0.0267(8) Uani 1 1 d . . . C5 C 0.5136(4) 0.6739(5) 0.3841(3) 0.0354(10) Uani 1 1 d . . . H5A H 0.4705 0.7472 0.3378 0.053 Uiso 1 1 calc R . . H5B H 0.4428 0.6739 0.4346 0.053 Uiso 1 1 calc R . . H5C H 0.5579 0.585 0.3611 0.053 Uiso 1 1 calc R . . C6 C 0.5483(4) 0.8370(4) 0.4512(3) 0.0338(9) Uani 1 1 d . . . H6A H 0.5064 0.911 0.405 0.051 Uiso 1 1 calc R . . H6B H 0.6152 0.8535 0.4727 0.051 Uiso 1 1 calc R . . H6C H 0.476 0.8346 0.5001 0.051 Uiso 1 1 calc R . . C7 C 0.6883(4) 0.5821(4) 0.4858(2) 0.0318(9) Uani 1 1 d . . . H7A H 0.7582 0.5963 0.5055 0.048 Uiso 1 1 calc R . . H7B H 0.732 0.4937 0.4623 0.048 Uiso 1 1 calc R . . H7C H 0.6166 0.5823 0.5358 0.048 Uiso 1 1 calc R . . C8 C 0.7796(4) 0.9150(4) 0.0772(2) 0.0255(8) Uani 1 1 d . . . C9 C 0.7746(6) 1.0460(4) 0.0976(3) 0.0490(12) Uani 1 1 d . . . H9A H 0.765 1.1118 0.0439 0.073 Uiso 1 1 calc R . . H9B H 0.8601 1.0239 0.119 0.073 Uiso 1 1 calc R . . H9C H 0.6954 1.0865 0.1431 0.073 Uiso 1 1 calc R . . C10 C 0.6461(5) 0.9525(5) 0.0426(3) 0.0458(11) Uani 1 1 d . . . H10A H 0.6395 1.0165 -0.0117 0.069 Uiso 1 1 calc R . . H10B H 0.5665 0.9959 0.0871 0.069 Uiso 1 1 calc R . . H10C H 0.6469 0.8691 0.0303 0.069 Uiso 1 1 calc R . . C11 C 0.9005(5) 0.8573(5) 0.0028(3) 0.0425(11) Uani 1 1 d . . . H11A H 0.8858 0.9252 -0.0499 0.064 Uiso 1 1 calc R . . H11B H 0.9055 0.7727 -0.0109 0.064 Uiso 1 1 calc R . . H11C H 0.9871 0.8373 0.0218 0.064 Uiso 1 1 calc R . . C12 C 1.1184(4) 0.7294(4) 0.2747(3) 0.0273(8) Uani 1 1 d . . . C13 C 1.1123(5) 0.8497(5) 0.2055(3) 0.0452(11) Uani 1 1 d . . . H13A H 1.0281 0.9323 0.2211 0.068 Uiso 1 1 calc R . . H13B H 1.1114 0.8294 0.1479 0.068 Uiso 1 1 calc R . . H13C H 1.1934 0.8651 0.2029 0.068 Uiso 1 1 calc R . . C14 C 1.1265(4) 0.7615(4) 0.3634(3) 0.0378(10) Uani 1 1 d . . . H14A H 1.1314 0.6844 0.409 0.057 Uiso 1 1 calc R . . H14B H 1.0441 0.8449 0.3799 0.057 Uiso 1 1 calc R . . H14C H 1.2092 0.7755 0.3579 0.057 Uiso 1 1 calc R . . C15 C 1.2498(4) 0.5997(5) 0.2506(4) 0.0510(13) Uani 1 1 d . . . H15A H 1.2534 0.5223 0.2955 0.076 Uiso 1 1 calc R . . H15B H 1.3312 0.6148 0.2479 0.076 Uiso 1 1 calc R . . H15C H 1.2489 0.5792 0.193 0.076 Uiso 1 1 calc R . . C16 C 0.8706(4) 0.3073(4) 0.3373(2) 0.0239(8) Uani 1 1 d . . . C17 C 0.7652(4) 0.3605(4) 0.2837(2) 0.0238(8) Uani 1 1 d . . . C18 C 0.6845(4) 0.2939(4) 0.2891(3) 0.0326(9) Uani 1 1 d . . . H18 H 0.6137 0.3294 0.2533 0.039 Uiso 1 1 calc R . . C19 C 0.7078(5) 0.1744(4) 0.3473(3) 0.0389(10) Uani 1 1 d . . . H19 H 0.6546 0.1266 0.3498 0.047 Uiso 1 1 calc R . . C20 C 0.8069(5) 0.1250(4) 0.4012(3) 0.0385(11) Uani 1 1 d . . . H20 H 0.8199 0.0448 0.4419 0.046 Uiso 1 1 calc R . . C21 C 0.8889(4) 0.1915(4) 0.3969(3) 0.0327(9) Uani 1 1 d . . . H21 H 0.9568 0.1571 0.4348 0.039 Uiso 1 1 calc R . . C22 C 1.0775(4) 0.3321(4) 0.3520(2) 0.0232(8) Uani 1 1 d . . . H22A H 1.0723 0.2845 0.4127 0.028 Uiso 1 1 calc R . . H22B H 1.0969 0.4099 0.3544 0.028 Uiso 1 1 calc R . . C23 C 1.2013(4) 0.2306(4) 0.2933(2) 0.0266(8) Uani 1 1 d . . . C24 C 1.2023(4) 0.2894(4) 0.1969(3) 0.0411(11) Uani 1 1 d . . . H24A H 1.2013 0.3798 0.1897 0.062 Uiso 1 1 calc R . . H24B H 1.1204 0.2987 0.1767 0.062 Uiso 1 1 calc R . . H24C H 1.2859 0.2276 0.162 0.062 Uiso 1 1 calc R . . C25 C 1.3333(4) 0.2095(4) 0.3235(4) 0.0472(12) Uani 1 1 d . . . H25A H 1.3331 0.1712 0.3858 0.071 Uiso 1 1 calc R . . H25B H 1.3367 0.2979 0.3158 0.071 Uiso 1 1 calc R . . H25C H 1.4144 0.1458 0.288 0.071 Uiso 1 1 calc R . . C26 C 1.2028(4) 0.0896(4) 0.3040(3) 0.0401(11) Uani 1 1 d . . . H26A H 1.2024 0.0509 0.3662 0.06 Uiso 1 1 calc R . . H26B H 1.2863 0.0282 0.2687 0.06 Uiso 1 1 calc R . . H26C H 1.1208 0.0993 0.2838 0.06 Uiso 1 1 calc R . . C27 C 0.6479(3) 0.5581(4) 0.1735(2) 0.0230(8) Uani 1 1 d . . . H27A H 0.616 0.6581 0.1714 0.028 Uiso 1 1 calc R . . H27B H 0.5677 0.5386 0.1998 0.028 Uiso 1 1 calc R . . C28 C 0.6935(4) 0.5217(4) 0.0781(2) 0.0247(8) Uani 1 1 d . . . C29 C 0.8240(4) 0.5394(4) 0.0379(2) 0.0297(9) Uani 1 1 d . . . H29A H 0.8069 0.6337 0.0406 0.045 Uiso 1 1 calc R . . H29B H 0.8497 0.5211 -0.0237 0.045 Uiso 1 1 calc R . . H29C H 0.8994 0.4748 0.071 0.045 Uiso 1 1 calc R . . C30 C 0.5744(4) 0.6208(4) 0.0266(3) 0.0366(10) Uani 1 1 d . . . H30A H 0.4913 0.6082 0.0531 0.055 Uiso 1 1 calc R . . H30B H 0.5998 0.6019 -0.0349 0.055 Uiso 1 1 calc R . . H30C H 0.5561 0.7156 0.0287 0.055 Uiso 1 1 calc R . . C31 C 0.7222(4) 0.3743(4) 0.0734(3) 0.0318(9) Uani 1 1 d . . . H31A H 0.6389 0.3616 0.0991 0.048 Uiso 1 1 calc R . . H31B H 0.7979 0.3103 0.1065 0.048 Uiso 1 1 calc R . . H31C H 0.7482 0.3565 0.0117 0.048 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 Si 0.0162(5) 0.0152(5) 0.0187(5) -0.0031(4) -0.0014(4) -0.0047(4) P1 0.0175(4) 0.0174(4) 0.0201(5) -0.0026(4) -0.0009(4) -0.0062(4) P2 0.0195(5) 0.0165(5) 0.0262(5) -0.0023(4) -0.0020(4) -0.0032(4) P3 0.0237(5) 0.0225(5) 0.0226(5) -0.0066(4) -0.0032(4) -0.0091(4) N1 0.0214(16) 0.0181(15) 0.0223(15) -0.0014(12) -0.0029(12) -0.0058(13) N2 0.0206(15) 0.0184(15) 0.0233(16) -0.0036(12) -0.0039(12) -0.0085(12) C1 0.0172(17) 0.0151(17) 0.0201(17) -0.0052(14) -0.0005(14) -0.0038(14) C2 0.0252(19) 0.0165(17) 0.0231(19) -0.0030(14) -0.0054(15) -0.0087(15) C3 0.0210(18) 0.0130(16) 0.030(2) -0.0030(14) -0.0054(15) -0.0052(14) C4 0.0230(19) 0.028(2) 0.0227(19) -0.0078(16) 0.0049(15) -0.0075(16) C5 0.025(2) 0.047(3) 0.034(2) -0.0134(19) 0.0087(17) -0.0178(19) C6 0.034(2) 0.031(2) 0.027(2) -0.0133(17) 0.0084(17) -0.0081(18) C7 0.033(2) 0.029(2) 0.025(2) -0.0038(16) 0.0044(17) -0.0101(18) C8 0.029(2) 0.0195(18) 0.0252(19) 0.0031(15) -0.0057(16) -0.0096(16) C9 0.079(4) 0.027(2) 0.045(3) 0.003(2) -0.013(3) -0.028(2) C10 0.046(3) 0.038(3) 0.047(3) 0.009(2) -0.017(2) -0.016(2) C11 0.048(3) 0.038(2) 0.033(2) 0.0034(19) -0.002(2) -0.017(2) C12 0.0215(19) 0.025(2) 0.039(2) -0.0098(17) -0.0035(16) -0.0111(16) C13 0.056(3) 0.048(3) 0.049(3) 0.004(2) -0.011(2) -0.039(2) C14 0.034(2) 0.038(2) 0.049(3) -0.008(2) -0.017(2) -0.016(2) C15 0.022(2) 0.048(3) 0.089(4) -0.028(3) -0.002(2) -0.015(2) C16 0.0241(19) 0.0176(18) 0.0249(19) -0.0071(15) 0.0043(15) -0.0068(15) C17 0.0262(19) 0.0234(19) 0.0200(18) -0.0052(15) 0.0049(15) -0.0120(16) C18 0.034(2) 0.038(2) 0.030(2) -0.0065(18) 0.0057(17) -0.0229(19) C19 0.049(3) 0.036(2) 0.037(2) -0.0089(19) 0.012(2) -0.029(2) C20 0.047(3) 0.027(2) 0.035(2) -0.0014(18) 0.012(2) -0.020(2) C21 0.034(2) 0.025(2) 0.030(2) -0.0004(16) 0.0024(17) -0.0097(18) C22 0.0264(19) 0.0164(17) 0.0223(18) -0.0039(14) -0.0078(15) -0.0032(15) C23 0.0240(19) 0.0194(18) 0.031(2) -0.0031(15) -0.0079(16) -0.0032(16) C24 0.031(2) 0.036(2) 0.036(2) -0.0074(19) 0.0008(18) 0.0001(19) C25 0.029(2) 0.030(2) 0.077(4) -0.015(2) -0.021(2) 0.0006(19) C26 0.035(2) 0.022(2) 0.057(3) -0.016(2) 0.001(2) -0.0063(18) C27 0.0164(17) 0.0233(19) 0.029(2) -0.0062(15) -0.0031(15) -0.0073(15) C28 0.027(2) 0.0233(19) 0.0257(19) -0.0041(15) -0.0072(16) -0.0112(16) C29 0.033(2) 0.036(2) 0.025(2) -0.0087(17) -0.0011(16) -0.0183(18) C30 0.039(2) 0.036(2) 0.038(2) 0.0011(19) -0.0165(19) -0.017(2) C31 0.042(2) 0.028(2) 0.031(2) -0.0074(17) -0.0055(18) -0.0188(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si N2 1.736(3) . ? Si N1 1.738(3) . ? Si C1 1.935(3) . ? Si P1 2.2886(16) . ? P1 C2 1.850(4) . ? P1 C3 1.857(4) . ? P2 C2 1.685(4) . ? P2 C1 1.858(4) . ? P3 C3 1.680(4) . ? P3 C1 1.853(4) . ? N1 C16 1.408(5) . ? N1 C22 1.460(4) . ? N2 C17 1.417(5) . ? N2 C27 1.465(4) . ? C1 C4 1.575(5) . ? C2 C8 1.543(5) . ? C3 C12 1.537(5) . ? C4 C5 1.532(5) . ? C4 C7 1.538(5) . ? C4 C6 1.540(5) . ? C8 C9 1.527(5) . ? C8 C10 1.530(6) . ? C8 C11 1.538(6) . ? C12 C13 1.516(6) . ? C12 C15 1.533(5) . ? C12 C14 1.538(5) . ? C16 C21 1.379(5) . ? C16 C17 1.417(5) . ? C17 C18 1.380(5) . ? C18 C19 1.391(6) . ? C19 C20 1.372(6) . ? C20 C21 1.394(6) . ? C22 C23 1.554(5) . ? C23 C24 1.515(5) . ? C23 C26 1.530(5) . ? C23 C25 1.536(5) . ? C27 C28 1.542(5) . ? C28 C29 1.523(5) . ? C28 C31 1.527(5) . ? C28 C30 1.533(5) . ? 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 N2 Si N1 91.71(14) . . ? N2 Si C1 113.96(15) . . ? N1 Si C1 119.43(15) . . ? N2 Si P1 124.93(11) . . ? N1 Si P1 119.23(11) . . ? C1 Si P1 90.27(11) . . ? C2 P1 C3 98.67(16) . . ? C2 P1 Si 89.14(12) . . ? C3 P1 Si 88.45(12) . . ? C2 P2 C1 102.67(16) . . ? C3 P3 C1 102.00(17) . . ? C16 N1 C22 120.9(3) . . ? C16 N1 Si 109.5(2) . . ? C22 N1 Si 129.6(2) . . ? C17 N2 C27 120.1(3) . . ? C17 N2 Si 109.8(2) . . ? C27 N2 Si 128.5(2) . . ? C4 C1 P3 111.1(2) . . ? C4 C1 P2 111.1(2) . . ? P3 C1 P2 108.87(18) . . ? C4 C1 Si 120.9(2) . . ? P3 C1 Si 102.19(16) . . ? P2 C1 Si 101.80(17) . . ? C8 C2 P2 120.1(3) . . ? C8 C2 P1 120.5(3) . . ? P2 C2 P1 119.3(2) . . ? C12 C3 P3 122.1(3) . . ? C12 C3 P1 117.6(3) . . ? P3 C3 P1 120.1(2) . . ? C5 C4 C7 108.3(3) . . ? C5 C4 C6 107.8(3) . . ? C7 C4 C6 109.6(3) . . ? C5 C4 C1 111.5(3) . . ? C7 C4 C1 110.2(3) . . ? C6 C4 C1 109.5(3) . . ? C9 C8 C10 108.5(3) . . ? C9 C8 C11 108.4(3) . . ? C10 C8 C11 107.5(3) . . ? C9 C8 C2 108.2(3) . . ? C10 C8 C2 111.4(3) . . ? C11 C8 C2 112.7(3) . . ? C13 C12 C15 109.7(4) . . ? C13 C12 C3 109.2(3) . . ? C15 C12 C3 110.3(3) . . ? C13 C12 C14 108.2(3) . . ? C15 C12 C14 107.9(3) . . ? C3 C12 C14 111.4(3) . . ? C21 C16 N1 127.7(4) . . ? C21 C16 C17 119.6(4) . . ? N1 C16 C17 112.7(3) . . ? C18 C17 C16 120.1(3) . . ? C18 C17 N2 127.7(4) . . ? C16 C17 N2 112.1(3) . . ? C17 C18 C19 119.4(4) . . ? C20 C19 C18 120.6(4) . . ? C19 C20 C21 120.7(4) . . ? C16 C21 C20 119.6(4) . . ? N1 C22 C23 115.8(3) . . ? C24 C23 C26 109.1(3) . . ? C24 C23 C25 109.3(4) . . ? C26 C23 C25 107.5(3) . . ? C24 C23 C22 111.0(3) . . ? C26 C23 C22 113.1(3) . . ? C25 C23 C22 106.7(3) . . ? N2 C27 C28 115.9(3) . . ? C29 C28 C31 108.7(3) . . ? C29 C28 C30 110.4(3) . . ? C31 C28 C30 109.0(3) . . ? C29 C28 C27 109.8(3) . . ? C31 C28 C27 112.2(3) . . ? C30 C28 C27 106.8(3) . . ?