# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Mark Crimmin' _publ_contact_author_email m.crimmin@imperial.ac.uk _publ_section_title ; Wittig-Olefination via an Yttrium-Coordinated Betaine ; loop_ _publ_author_name M.Crimmin A.White # Attachment '- Compound_1_2.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 843183' #TrackingRef '- Compound_1_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'MRC I 018B1' _chemical_melting_point ? _chemical_formula_moiety 'C31 H53 I N2 P Si4 Y' _chemical_formula_sum 'C31 H53 I N2 P Si4 Y' _chemical_formula_weight 812.89 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8866(18) _cell_length_b 12.252(3) _cell_length_c 36.576(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.160(4) _cell_angle_gamma 90.00 _cell_volume 3979.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 1959 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.23 _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33017 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.1406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9304 _reflns_number_gt 4742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0814P)^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 9304 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _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 C1 C 0.5707(7) 0.2753(5) 0.84205(15) 0.0326(15) Uani 1 1 d . . . H1A H 0.4800 0.2944 0.8546 0.039 Uiso 1 1 calc R . . H1B H 0.5752 0.3272 0.8221 0.039 Uiso 1 1 calc R . . C2 C 0.6759(7) 0.0757(5) 0.80634(15) 0.0290(14) Uani 1 1 d . . . C3 C 0.7919(8) 0.1239(6) 0.78817(17) 0.0404(17) Uani 1 1 d . . . H3 H 0.7893 0.1988 0.7840 0.048 Uiso 1 1 calc R . . C4 C 0.9119(8) 0.0638(7) 0.77595(19) 0.052(2) Uani 1 1 d . . . H4 H 0.9894 0.0982 0.7640 0.062 Uiso 1 1 calc R . . C5 C 0.9159(9) -0.0469(7) 0.7815(2) 0.055(2) Uani 1 1 d . . . H5 H 0.9968 -0.0877 0.7736 0.066 Uiso 1 1 calc R . . C6 C 0.7992(10) -0.0978(7) 0.7990(3) 0.069(3) Uani 1 1 d . . . H6 H 0.8000 -0.1732 0.8020 0.083 Uiso 1 1 calc R . . C7 C 0.6817(8) -0.0366(6) 0.81202(19) 0.0475(19) Uani 1 1 d . . . H7 H 0.6059 -0.0708 0.8247 0.057 Uiso 1 1 calc R . . C8 C 0.4113(7) 0.1827(5) 0.77795(15) 0.0267(14) Uani 1 1 d . . . C9 C 0.4375(8) 0.1278(6) 0.74513(17) 0.0427(18) Uani 1 1 d . . . H9 H 0.5121 0.0747 0.7443 0.051 Uiso 1 1 calc R . . C10 C 0.3515(8) 0.1533(6) 0.71398(17) 0.051(2) Uani 1 1 d . . . H10 H 0.3671 0.1157 0.6924 0.061 Uiso 1 1 calc R . . C11 C 0.2425(7) 0.2338(6) 0.71456(18) 0.0424(17) Uani 1 1 d . . . H11 H 0.1884 0.2521 0.6932 0.051 Uiso 1 1 calc R . . C12 C 0.2145(7) 0.2863(6) 0.74642(18) 0.0449(18) Uani 1 1 d . . . H12 H 0.1392 0.3389 0.7472 0.054 Uiso 1 1 calc R . . C13 C 0.2998(7) 0.2602(6) 0.77778(17) 0.0418(17) Uani 1 1 d . . . H13 H 0.2808 0.2966 0.7994 0.050 Uiso 1 1 calc R . . C14 C 0.4070(7) 0.0707(5) 0.84829(16) 0.0286(14) Uani 1 1 d . . . C15 C 0.2938(7) 0.0041(5) 0.83358(18) 0.0382(16) Uani 1 1 d . . . H15 H 0.2692 0.0068 0.8087 0.046 Uiso 1 1 calc R . . C16 C 0.2176(8) -0.0662(6) 0.8559(2) 0.0450(18) Uani 1 1 d . . . H16 H 0.1428 -0.1114 0.8458 0.054 Uiso 1 1 calc R . . C17 C 0.2511(7) -0.0699(5) 0.89272(18) 0.0383(16) Uani 1 1 d . . . H17 H 0.1988 -0.1172 0.9075 0.046 Uiso 1 1 calc R . . C18 C 0.3615(8) -0.0042(5) 0.90777(18) 0.0405(17) Uani 1 1 d . . . H18 H 0.3833 -0.0069 0.9328 0.049 Uiso 1 1 calc R . . C19 C 0.4409(7) 0.0663(5) 0.88612(16) 0.0328(15) Uani 1 1 d . . . H19 H 0.5162 0.1104 0.8965 0.039 Uiso 1 1 calc R . . C20 C 0.9884(10) 0.1566(6) 0.8896(2) 0.070(3) Uani 1 1 d . . . H20A H 1.0286 0.2293 0.8896 0.105 Uiso 1 1 calc R . . H20B H 0.9214 0.1470 0.8686 0.105 Uiso 1 1 calc R . . H20C H 1.0694 0.1049 0.8886 0.105 Uiso 1 1 calc R . . C21 C 1.0267(9) 0.1382(6) 0.9711(2) 0.065(2) Uani 1 1 d . . . H21A H 1.0678 0.2105 0.9732 0.097 Uiso 1 1 calc R . . H21B H 1.1058 0.0874 0.9663 0.097 Uiso 1 1 calc R . . H21C H 0.9810 0.1188 0.9936 0.097 Uiso 1 1 calc R . . C22 C 0.8066(10) -0.0080(6) 0.9305(2) 0.074(3) Uani 1 1 d . . . H22A H 0.7316 -0.0131 0.9110 0.111 Uiso 1 1 calc R . . H22B H 0.7623 -0.0260 0.9532 0.111 Uiso 1 1 calc R . . H22C H 0.8872 -0.0578 0.9260 0.111 Uiso 1 1 calc R . . C23 C 0.4622(10) 0.3333(8) 0.9519(2) 0.082(3) Uani 1 1 d . . . H23A H 0.4130 0.2896 0.9332 0.124 Uiso 1 1 calc R . . H23B H 0.4892 0.4026 0.9418 0.124 Uiso 1 1 calc R . . H23C H 0.3951 0.3444 0.9715 0.124 Uiso 1 1 calc R . . C24 C 0.5775(12) 0.1359(6) 0.9943(2) 0.085(3) Uani 1 1 d . . . H24A H 0.5265 0.0872 0.9774 0.128 Uiso 1 1 calc R . . H24B H 0.5111 0.1553 1.0134 0.128 Uiso 1 1 calc R . . H24C H 0.6653 0.1006 1.0048 0.128 Uiso 1 1 calc R . . C25 C 0.7281(11) 0.3468(7) 1.0055(2) 0.082(3) Uani 1 1 d . . . H25A H 0.7609 0.4141 0.9949 0.123 Uiso 1 1 calc R . . H25B H 0.8134 0.3084 1.0159 0.123 Uiso 1 1 calc R . . H25C H 0.6583 0.3621 1.0242 0.123 Uiso 1 1 calc R . . C26 C 1.0012(7) 0.4607(5) 0.93094(18) 0.0428(18) Uani 1 1 d . . . H26A H 0.9535 0.4045 0.9446 0.064 Uiso 1 1 calc R . . H26B H 1.0834 0.4911 0.9454 0.064 Uiso 1 1 calc R . . H26C H 1.0387 0.4303 0.9089 0.064 Uiso 1 1 calc R . . C27 C 0.9691(8) 0.6736(5) 0.8928(2) 0.0484(19) Uani 1 1 d . . . H27A H 0.9989 0.6414 0.8703 0.073 Uiso 1 1 calc R . . H27B H 1.0571 0.6948 0.9071 0.073 Uiso 1 1 calc R . . H27C H 0.9081 0.7368 0.8876 0.073 Uiso 1 1 calc R . . C28 C 0.8036(9) 0.6411(6) 0.9623(2) 0.058(2) Uani 1 1 d . . . H28A H 0.7469 0.5911 0.9766 0.087 Uiso 1 1 calc R . . H28B H 0.7431 0.7041 0.9564 0.087 Uiso 1 1 calc R . . H28C H 0.8925 0.6631 0.9760 0.087 Uiso 1 1 calc R . . C29 C 0.3860(8) 0.5366(7) 0.8751(2) 0.069(2) Uani 1 1 d . . . H29A H 0.3617 0.5286 0.9003 0.103 Uiso 1 1 calc R . . H29B H 0.3806 0.4667 0.8632 0.103 Uiso 1 1 calc R . . H29C H 0.3157 0.5857 0.8632 0.103 Uiso 1 1 calc R . . C30 C 0.5603(10) 0.7333(6) 0.8900(3) 0.080(3) Uani 1 1 d . . . H30A H 0.6566 0.7687 0.8895 0.120 Uiso 1 1 calc R . . H30B H 0.5274 0.7312 0.9147 0.120 Uiso 1 1 calc R . . H30C H 0.4885 0.7730 0.8749 0.120 Uiso 1 1 calc R . . C31 C 0.6195(11) 0.6056(9) 0.8235(2) 0.095(4) Uani 1 1 d . . . H31A H 0.7190 0.6349 0.8215 0.142 Uiso 1 1 calc R . . H31B H 0.5477 0.6540 0.8118 0.142 Uiso 1 1 calc R . . H31C H 0.6138 0.5353 0.8119 0.142 Uiso 1 1 calc R . . N1 N 0.7103(5) 0.5131(4) 0.89517(13) 0.0261(11) Uani 1 1 d . . . N2 N 0.7476(6) 0.2344(4) 0.93409(13) 0.0313(12) Uani 1 1 d . . . Si1 Si 0.5769(2) 0.59145(15) 0.87230(5) 0.0398(5) Uani 1 1 d . . . Si2 Si 0.8587(2) 0.57254(14) 0.91890(5) 0.0313(4) Uani 1 1 d . . . Si3 Si 0.6349(2) 0.26204(16) 0.96957(5) 0.0432(5) Uani 1 1 d . . . Si4 Si 0.8817(2) 0.13392(15) 0.93280(5) 0.0441(5) Uani 1 1 d . . . P P 0.51883(18) 0.15613(13) 0.81969(4) 0.0285(4) Uani 1 1 d . . . Y Y 0.77071(7) 0.34144(5) 0.884823(15) 0.02467(16) Uani 1 1 d . . . I I 0.96936(6) 0.39499(4) 0.822208(13) 0.05129(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(4) 0.038(4) 0.018(3) -0.004(3) -0.003(3) -0.008(3) C2 0.032(4) 0.032(4) 0.023(3) -0.002(3) -0.006(3) -0.003(3) C3 0.052(5) 0.038(4) 0.032(4) -0.008(3) 0.005(3) 0.000(3) C4 0.040(4) 0.080(6) 0.036(4) -0.005(4) 0.006(3) -0.008(4) C5 0.043(5) 0.064(6) 0.057(5) -0.008(4) 0.000(4) 0.018(4) C6 0.064(6) 0.044(5) 0.100(7) 0.015(5) 0.011(5) 0.017(4) C7 0.039(4) 0.050(5) 0.054(5) 0.003(4) 0.013(4) 0.008(4) C8 0.028(3) 0.030(4) 0.021(3) -0.006(3) 0.000(3) -0.002(3) C9 0.047(4) 0.045(4) 0.035(4) -0.009(3) -0.010(3) 0.012(3) C10 0.067(5) 0.066(5) 0.019(3) -0.008(3) -0.011(3) 0.013(4) C11 0.035(4) 0.057(5) 0.035(4) 0.006(3) -0.005(3) -0.006(4) C12 0.033(4) 0.061(5) 0.040(4) 0.002(4) 0.001(3) 0.011(4) C13 0.041(4) 0.055(5) 0.029(4) -0.010(3) 0.003(3) 0.005(4) C14 0.026(3) 0.025(3) 0.034(4) -0.003(3) -0.002(3) 0.002(3) C15 0.045(4) 0.036(4) 0.034(4) -0.007(3) -0.002(3) -0.004(3) C16 0.037(4) 0.038(4) 0.060(5) -0.010(4) 0.009(4) -0.006(3) C17 0.039(4) 0.036(4) 0.040(4) 0.002(3) 0.003(3) 0.000(3) C18 0.045(4) 0.043(4) 0.034(4) 0.009(3) 0.001(3) 0.000(3) C19 0.038(4) 0.032(4) 0.027(3) -0.003(3) -0.006(3) -0.003(3) C20 0.091(7) 0.059(5) 0.059(5) 0.005(4) -0.016(5) 0.050(5) C21 0.082(6) 0.041(5) 0.069(6) 0.005(4) -0.038(5) 0.002(4) C22 0.106(7) 0.029(4) 0.082(6) -0.008(4) -0.049(6) 0.008(5) C23 0.081(7) 0.105(8) 0.065(6) 0.012(5) 0.047(5) 0.013(6) C24 0.153(10) 0.053(6) 0.051(5) 0.002(4) 0.030(6) -0.043(6) C25 0.120(8) 0.083(7) 0.044(5) -0.025(5) 0.026(5) -0.045(6) C26 0.039(4) 0.037(4) 0.052(4) -0.008(3) -0.015(3) -0.012(3) C27 0.049(5) 0.032(4) 0.064(5) -0.005(4) 0.008(4) -0.015(3) C28 0.072(6) 0.055(5) 0.048(5) -0.022(4) 0.005(4) -0.014(4) C29 0.049(5) 0.061(6) 0.095(7) 0.008(5) -0.014(5) 0.005(4) C30 0.069(6) 0.040(5) 0.129(8) -0.005(5) -0.022(6) 0.021(4) C31 0.084(7) 0.129(9) 0.071(6) 0.046(6) 0.011(5) 0.050(7) N1 0.024(3) 0.023(3) 0.031(3) 0.000(2) 0.003(2) 0.000(2) N2 0.046(3) 0.022(3) 0.025(3) 0.001(2) -0.006(2) -0.005(2) Si1 0.0414(11) 0.0309(11) 0.0469(12) 0.0043(9) -0.0015(9) 0.0096(9) Si2 0.0383(11) 0.0263(9) 0.0294(10) -0.0051(7) 0.0016(8) -0.0062(8) Si3 0.0700(14) 0.0363(11) 0.0235(10) 0.0019(8) 0.0061(9) -0.0179(10) Si4 0.0627(14) 0.0244(10) 0.0436(12) -0.0002(8) -0.0195(10) 0.0042(9) P 0.0313(9) 0.0311(9) 0.0228(8) -0.0042(7) -0.0016(7) -0.0042(7) Y 0.0310(3) 0.0204(3) 0.0227(3) -0.0012(3) 0.0011(2) -0.0002(3) I 0.0545(3) 0.0520(3) 0.0493(3) -0.0096(2) 0.0266(2) -0.0089(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P 1.728(6) . ? C1 Y 2.460(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.380(9) . ? C2 C7 1.392(9) . ? C2 P 1.792(6) . ? C3 C4 1.384(10) . ? C3 H3 0.9300 . ? C4 C5 1.371(10) . ? C4 H4 0.9300 . ? C5 C6 1.387(11) . ? C5 H5 0.9300 . ? C6 C7 1.385(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.372(8) . ? C8 C9 1.403(8) . ? C8 P 1.800(6) . ? C9 C10 1.384(9) . ? C9 H9 0.9300 . ? C10 C11 1.383(9) . ? C10 H10 0.9300 . ? C11 C12 1.363(9) . ? C11 H11 0.9300 . ? C12 C13 1.388(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.388(8) . ? C14 C19 1.406(8) . ? C14 P 1.804(6) . ? C15 C16 1.382(9) . ? C15 H15 0.9300 . ? C16 C17 1.369(9) . ? C16 H16 0.9300 . ? C17 C18 1.368(9) . ? C17 H17 0.9300 . ? C18 C19 1.383(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 Si4 1.895(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 Si4 1.869(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 Si4 1.863(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 Si3 1.860(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 Si3 1.871(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 Si3 1.846(8) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 Si2 1.906(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 Si2 1.865(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 Si2 1.877(7) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 Si1 1.831(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 Si1 1.862(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 Si1 1.846(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 Si2 1.714(5) . ? N1 Si1 1.718(5) . ? N1 Y 2.207(5) . ? N2 Si3 1.703(5) . ? N2 Si4 1.715(5) . ? N2 Y 2.244(5) . ? Y I 3.0161(8) . ? 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 P C1 Y 138.8(3) . . ? P C1 H1A 102.4 . . ? Y C1 H1A 102.4 . . ? P C1 H1B 102.4 . . ? Y C1 H1B 102.4 . . ? H1A C1 H1B 104.9 . . ? C3 C2 C7 118.1(6) . . ? C3 C2 P 120.0(5) . . ? C7 C2 P 121.8(5) . . ? C2 C3 C4 121.7(7) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 119.6(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.9(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.1(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.5(7) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C13 C8 C9 118.1(6) . . ? C13 C8 P 119.3(4) . . ? C9 C8 P 122.6(5) . . ? C10 C9 C8 119.4(6) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.0(6) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.1(7) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C8 C13 C12 122.3(6) . . ? C8 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C19 118.9(6) . . ? C15 C14 P 121.6(5) . . ? C19 C14 P 119.4(5) . . ? C16 C15 C14 120.1(6) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.6(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.7(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C14 119.5(6) . . ? C18 C19 H19 120.2 . . ? C14 C19 H19 120.2 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 H21A 109.5 . . ? Si4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 N1 Si1 120.8(3) . . ? Si2 N1 Y 107.7(2) . . ? Si1 N1 Y 128.1(3) . . ? Si3 N2 Si4 126.4(3) . . ? Si3 N2 Y 124.7(3) . . ? Si4 N2 Y 108.2(2) . . ? N1 Si1 C29 113.0(3) . . ? N1 Si1 C31 111.1(3) . . ? C29 Si1 C31 108.2(4) . . ? N1 Si1 C30 114.5(3) . . ? C29 Si1 C30 103.8(4) . . ? C31 Si1 C30 105.7(5) . . ? N1 Si2 C27 115.7(3) . . ? N1 Si2 C28 113.4(3) . . ? C27 Si2 C28 107.1(3) . . ? N1 Si2 C26 107.7(3) . . ? C27 Si2 C26 103.8(3) . . ? C28 Si2 C26 108.6(3) . . ? N2 Si3 C25 113.1(3) . . ? N2 Si3 C23 109.3(3) . . ? C25 Si3 C23 109.0(5) . . ? N2 Si3 C24 112.5(3) . . ? C25 Si3 C24 104.1(4) . . ? C23 Si3 C24 108.6(5) . . ? N2 Si4 C22 115.0(3) . . ? N2 Si4 C21 114.8(3) . . ? C22 Si4 C21 107.2(3) . . ? N2 Si4 C20 106.7(3) . . ? C22 Si4 C20 106.7(4) . . ? C21 Si4 C20 105.6(4) . . ? C1 P C2 113.4(3) . . ? C1 P C8 111.9(3) . . ? C2 P C8 105.2(3) . . ? C1 P C14 111.0(3) . . ? C2 P C14 106.9(3) . . ? C8 P C14 108.1(3) . . ? N1 Y N2 112.88(17) . . ? N1 Y C1 104.36(19) . . ? N2 Y C1 103.45(19) . . ? N1 Y I 94.37(12) . . ? N2 Y I 144.16(13) . . ? C1 Y I 91.04(14) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.095 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.188 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 843184' #TrackingRef '- Compound_1_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'MRC I 065A1' _chemical_melting_point ? _chemical_formula_moiety 'C44 H63 I N2 O P Si4 Y' _chemical_formula_sum 'C44 H63 I N2 O P Si4 Y' _chemical_formula_weight 995.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5750(4) _cell_length_b 24.9990(7) _cell_length_c 15.7491(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.687(3) _cell_angle_gamma 90.00 _cell_volume 4948.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12477 _cell_measurement_theta_min 2.9270 _cell_measurement_theta_max 32.0020 _exptl_crystal_description needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.902 _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 50239 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 32.07 _reflns_number_total 15749 _reflns_number_gt 11490 _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^)+(0.0329P)^2^+1.2197P] 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 15749 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.498540(14) 0.107051(7) 0.247205(12) 0.02017(4) Uani 1 1 d . . . I I 0.460054(12) 0.160527(6) 0.413433(9) 0.03547(4) Uani 1 1 d . . . O1 O 0.49698(10) 0.17308(5) 0.16768(8) 0.0218(3) Uani 1 1 d . . . C2 C 0.51934(14) 0.22602(7) 0.14500(11) 0.0181(3) Uani 1 1 d . . . C3 C 0.59471(14) 0.24582(7) 0.21987(11) 0.0194(4) Uani 1 1 d . . . H3A H 0.6571 0.2217 0.2195 0.023 Uiso 1 1 calc R . . H3B H 0.5568 0.2373 0.2724 0.023 Uiso 1 1 calc R . . P4 P 0.64943(4) 0.313021(18) 0.23655(3) 0.01806(9) Uani 1 1 d . . . C5 C 0.41469(14) 0.25718(7) 0.13934(12) 0.0198(4) Uani 1 1 d . . . C6 C 0.35487(16) 0.26024(9) 0.06340(14) 0.0310(5) Uani 1 1 d . . . H6A H 0.3799 0.2432 0.0140 0.037 Uiso 1 1 calc R . . C7 C 0.25921(18) 0.28793(10) 0.05933(16) 0.0407(6) Uani 1 1 d . . . H7A H 0.2194 0.2895 0.0072 0.049 Uiso 1 1 calc R . . C8 C 0.22140(17) 0.31310(10) 0.13015(16) 0.0396(6) Uani 1 1 d . . . H8A H 0.1571 0.3331 0.1265 0.048 Uiso 1 1 calc R . . C9 C 0.27741(16) 0.30911(9) 0.20597(15) 0.0327(5) Uani 1 1 d . . . H9A H 0.2510 0.3257 0.2554 0.039 Uiso 1 1 calc R . . C10 C 0.37263(15) 0.28091(8) 0.21074(13) 0.0249(4) Uani 1 1 d . . . H10A H 0.4098 0.2778 0.2639 0.030 Uiso 1 1 calc R . . C11 C 0.58529(15) 0.22808(8) 0.06458(12) 0.0221(4) Uani 1 1 d . . . C12 C 0.58846(17) 0.27193(8) 0.01064(12) 0.0298(4) Uani 1 1 d . . . H12A H 0.5406 0.3008 0.0182 0.036 Uiso 1 1 calc R . . C13 C 0.6610(2) 0.27411(10) -0.05452(14) 0.0429(6) Uani 1 1 d . . . H13A H 0.6628 0.3046 -0.0904 0.052 Uiso 1 1 calc R . . C14 C 0.7299(2) 0.23243(12) -0.06721(15) 0.0475(7) Uani 1 1 d . . . H14A H 0.7801 0.2343 -0.1111 0.057 Uiso 1 1 calc R . . C15 C 0.72577(19) 0.18812(11) -0.01603(16) 0.0442(6) Uani 1 1 d . . . H15A H 0.7716 0.1587 -0.0258 0.053 Uiso 1 1 calc R . . C16 C 0.65523(16) 0.18602(9) 0.04975(14) 0.0328(5) Uani 1 1 d . . . H16A H 0.6545 0.1554 0.0854 0.039 Uiso 1 1 calc R . . C17 C 0.59501(14) 0.33756(7) 0.33351(12) 0.0220(4) Uani 1 1 d . . . C18 C 0.59133(18) 0.30201(8) 0.40147(13) 0.0320(5) Uani 1 1 d . . . H18A H 0.6195 0.2669 0.3961 0.038 Uiso 1 1 calc R . . C19 C 0.5467(2) 0.31768(10) 0.47677(14) 0.0412(6) Uani 1 1 d . . . H19A H 0.5439 0.2932 0.5228 0.049 Uiso 1 1 calc R . . C20 C 0.50671(18) 0.36813(11) 0.48524(15) 0.0423(6) Uani 1 1 d . . . H20A H 0.4753 0.3785 0.5368 0.051 Uiso 1 1 calc R . . C21 C 0.51179(18) 0.40417(10) 0.41902(16) 0.0413(6) Uani 1 1 d . . . H21A H 0.4851 0.4394 0.4257 0.050 Uiso 1 1 calc R . . C22 C 0.55568(16) 0.38926(8) 0.34272(14) 0.0308(5) Uani 1 1 d . . . H22A H 0.5589 0.4141 0.2972 0.037 Uiso 1 1 calc R . . C23 C 0.62863(14) 0.36140(7) 0.15269(12) 0.0210(4) Uani 1 1 d . . . C24 C 0.52665(15) 0.38190(7) 0.13480(13) 0.0249(4) Uani 1 1 d . . . H24A H 0.4685 0.3715 0.1683 0.030 Uiso 1 1 calc R . . C25 C 0.51114(17) 0.41727(9) 0.06828(14) 0.0326(5) Uani 1 1 d . . . H25A H 0.4421 0.4313 0.0562 0.039 Uiso 1 1 calc R . . C26 C 0.59554(19) 0.43249(9) 0.01905(14) 0.0358(5) Uani 1 1 d . . . H26A H 0.5841 0.4565 -0.0271 0.043 Uiso 1 1 calc R . . C27 C 0.69658(18) 0.41273(9) 0.03707(14) 0.0336(5) Uani 1 1 d . . . H27A H 0.7544 0.4233 0.0034 0.040 Uiso 1 1 calc R . . C28 C 0.71359(16) 0.37765(8) 0.10408(13) 0.0266(4) Uani 1 1 d . . . H28A H 0.7832 0.3646 0.1169 0.032 Uiso 1 1 calc R . . C29 C 0.79037(14) 0.30223(7) 0.25225(12) 0.0218(4) Uani 1 1 d . . . C30 C 0.84406(16) 0.31927(8) 0.32547(13) 0.0268(4) Uani 1 1 d . . . H30A H 0.8076 0.3384 0.3679 0.032 Uiso 1 1 calc R . . C31 C 0.95224(17) 0.30803(10) 0.33614(15) 0.0377(5) Uani 1 1 d . . . H31A H 0.9898 0.3193 0.3862 0.045 Uiso 1 1 calc R . . C32 C 1.00452(17) 0.28066(11) 0.27421(17) 0.0443(6) Uani 1 1 d . . . H32A H 1.0781 0.2730 0.2820 0.053 Uiso 1 1 calc R . . C33 C 0.95145(17) 0.26425(10) 0.20104(16) 0.0413(6) Uani 1 1 d . . . H33A H 0.9888 0.2459 0.1583 0.050 Uiso 1 1 calc R . . C34 C 0.84394(16) 0.27439(9) 0.18967(14) 0.0304(4) Uani 1 1 d . . . H34A H 0.8068 0.2625 0.1397 0.036 Uiso 1 1 calc R . . N35 N 0.66553(12) 0.07334(6) 0.24939(10) 0.0238(3) Uani 1 1 d . . . Si36 Si 0.76001(5) 0.08410(2) 0.32871(4) 0.02995(13) Uani 1 1 d . . . C37 C 0.7926(2) 0.15680(10) 0.33847(18) 0.0507(7) Uani 1 1 d . . . H37A H 0.7272 0.1772 0.3471 0.076 Uiso 1 1 calc R . . H37B H 0.8258 0.1691 0.2864 0.076 Uiso 1 1 calc R . . H37C H 0.8419 0.1623 0.3870 0.076 Uiso 1 1 calc R . . C38 C 0.8906(2) 0.04953(14) 0.31326(19) 0.0645(9) Uani 1 1 d . . . H38A H 0.8788 0.0109 0.3082 0.097 Uiso 1 1 calc R . . H38B H 0.9385 0.0567 0.3621 0.097 Uiso 1 1 calc R . . H38C H 0.9226 0.0629 0.2614 0.097 Uiso 1 1 calc R . . C39 C 0.7145(2) 0.06121(11) 0.43441(15) 0.0468(6) Uani 1 1 d . . . H39A H 0.6461 0.0780 0.4463 0.070 Uiso 1 1 calc R . . H39B H 0.7672 0.0714 0.4785 0.070 Uiso 1 1 calc R . . H39C H 0.7063 0.0222 0.4339 0.070 Uiso 1 1 calc R . . Si40 Si 0.68769(4) 0.03359(2) 0.16370(4) 0.02653(12) Uani 1 1 d . . . C41 C 0.57213(17) 0.03995(9) 0.08533(13) 0.0337(5) Uani 1 1 d . . . H41A H 0.5060 0.0307 0.1133 0.051 Uiso 1 1 calc R . . H41B H 0.5825 0.0156 0.0375 0.051 Uiso 1 1 calc R . . H41C H 0.5679 0.0768 0.0644 0.051 Uiso 1 1 calc R . . C42 C 0.80839(19) 0.05197(11) 0.10257(16) 0.0460(6) Uani 1 1 d . . . H42A H 0.8719 0.0495 0.1400 0.069 Uiso 1 1 calc R . . H42B H 0.8009 0.0886 0.0812 0.069 Uiso 1 1 calc R . . H42C H 0.8154 0.0273 0.0547 0.069 Uiso 1 1 calc R . . C43 C 0.6979(2) -0.03928(9) 0.19170(18) 0.0481(6) Uani 1 1 d . . . H43A H 0.7573 -0.0447 0.2324 0.072 Uiso 1 1 calc R . . H43B H 0.7101 -0.0601 0.1402 0.072 Uiso 1 1 calc R . . H43C H 0.6316 -0.0510 0.2170 0.072 Uiso 1 1 calc R . . N44 N 0.35439(12) 0.05699(6) 0.21781(10) 0.0238(3) Uani 1 1 d . . . Si45 Si 0.34993(5) -0.00311(2) 0.26942(4) 0.02991(13) Uani 1 1 d . . . C46 C 0.4622(2) -0.00563(11) 0.35103(16) 0.0459(6) Uani 1 1 d . . . H46A H 0.5299 0.0002 0.3232 0.069 Uiso 1 1 calc R . . H46B H 0.4631 -0.0407 0.3788 0.069 Uiso 1 1 calc R . . H46C H 0.4521 0.0223 0.3936 0.069 Uiso 1 1 calc R . . C47 C 0.3655(2) -0.06215(10) 0.19739(19) 0.0521(7) Uani 1 1 d . . . H47A H 0.3079 -0.0622 0.1541 0.078 Uiso 1 1 calc R . . H47B H 0.3626 -0.0952 0.2307 0.078 Uiso 1 1 calc R . . H47C H 0.4342 -0.0599 0.1697 0.078 Uiso 1 1 calc R . . C48 C 0.2260(2) -0.01457(12) 0.32976(17) 0.0534(7) Uani 1 1 d . . . H48A H 0.1642 -0.0139 0.2904 0.080 Uiso 1 1 calc R . . H48B H 0.2187 0.0136 0.3724 0.080 Uiso 1 1 calc R . . H48C H 0.2301 -0.0495 0.3581 0.080 Uiso 1 1 calc R . . Si49 Si 0.25375(4) 0.08207(2) 0.15347(4) 0.02586(12) Uani 1 1 d . . . C50 C 0.14562(19) 0.03208(10) 0.12840(17) 0.0456(6) Uani 1 1 d . . . H50A H 0.1158 0.0191 0.1814 0.068 Uiso 1 1 calc R . . H50B H 0.1753 0.0019 0.0972 0.068 Uiso 1 1 calc R . . H50C H 0.0894 0.0492 0.0936 0.068 Uiso 1 1 calc R . . C51 C 0.1913(2) 0.14154(11) 0.20388(17) 0.0488(6) Uani 1 1 d . . . H51A H 0.2462 0.1683 0.2175 0.073 Uiso 1 1 calc R . . H51B H 0.1570 0.1305 0.2561 0.073 Uiso 1 1 calc R . . H51C H 0.1380 0.1570 0.1645 0.073 Uiso 1 1 calc R . . C52 C 0.30424(18) 0.10427(10) 0.04844(14) 0.0368(5) Uani 1 1 d . . . H52A H 0.3615 0.1304 0.0577 0.055 Uiso 1 1 calc R . . H52B H 0.2461 0.1207 0.0149 0.055 Uiso 1 1 calc R . . H52C H 0.3316 0.0733 0.0178 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.01780(8) 0.01712(8) 0.02564(9) 0.00117(7) 0.00156(7) -0.00060(6) I 0.04038(9) 0.03390(8) 0.03269(8) -0.00433(6) 0.01045(6) -0.00011(6) O1 0.0229(7) 0.0159(6) 0.0267(7) 0.0001(5) 0.0009(5) -0.0029(5) C2 0.0180(8) 0.0170(8) 0.0194(8) -0.0012(7) 0.0009(7) -0.0027(6) C3 0.0201(9) 0.0177(8) 0.0202(9) 0.0002(7) -0.0017(7) -0.0003(6) P4 0.0171(2) 0.0173(2) 0.0198(2) -0.00026(18) -0.00021(18) -0.00035(16) C5 0.0164(8) 0.0186(8) 0.0245(9) 0.0018(7) 0.0006(7) -0.0024(6) C6 0.0300(11) 0.0345(11) 0.0281(10) -0.0020(9) -0.0042(9) 0.0021(9) C7 0.0311(12) 0.0505(15) 0.0397(13) 0.0057(11) -0.0109(10) 0.0063(10) C8 0.0226(10) 0.0400(13) 0.0564(15) 0.0110(12) 0.0032(10) 0.0084(9) C9 0.0247(10) 0.0342(12) 0.0400(12) 0.0002(10) 0.0125(9) 0.0034(8) C10 0.0197(9) 0.0295(10) 0.0255(10) 0.0012(8) 0.0027(8) -0.0012(7) C11 0.0213(9) 0.0257(9) 0.0192(9) -0.0044(7) 0.0008(7) -0.0060(7) C12 0.0384(12) 0.0298(11) 0.0215(9) -0.0040(8) 0.0045(9) -0.0120(9) C13 0.0579(16) 0.0453(14) 0.0262(11) -0.0042(10) 0.0111(11) -0.0256(12) C14 0.0419(14) 0.0667(18) 0.0349(13) -0.0173(12) 0.0192(11) -0.0229(12) C15 0.0323(12) 0.0584(16) 0.0427(14) -0.0157(12) 0.0136(11) -0.0001(11) C16 0.0267(10) 0.0377(12) 0.0342(11) -0.0057(10) 0.0051(9) 0.0002(9) C17 0.0189(9) 0.0237(9) 0.0234(9) -0.0034(8) 0.0017(7) -0.0024(7) C18 0.0449(13) 0.0252(10) 0.0263(10) -0.0037(8) 0.0048(9) -0.0042(9) C19 0.0518(15) 0.0458(14) 0.0265(11) -0.0057(10) 0.0111(10) -0.0149(11) C20 0.0275(11) 0.0641(17) 0.0357(12) -0.0208(12) 0.0096(10) -0.0017(11) C21 0.0341(12) 0.0446(14) 0.0449(14) -0.0200(11) -0.0030(11) 0.0156(10) C22 0.0301(11) 0.0270(10) 0.0352(11) -0.0044(9) -0.0023(9) 0.0044(8) C23 0.0231(9) 0.0164(8) 0.0235(9) 0.0007(7) -0.0001(7) -0.0036(7) C24 0.0243(9) 0.0205(9) 0.0297(10) 0.0021(8) 0.0011(8) -0.0013(7) C25 0.0302(11) 0.0300(11) 0.0372(12) 0.0079(9) -0.0045(9) 0.0032(8) C26 0.0445(13) 0.0294(11) 0.0335(12) 0.0124(9) -0.0004(10) 0.0001(9) C27 0.0344(12) 0.0355(12) 0.0310(11) 0.0080(9) 0.0054(9) -0.0066(9) C28 0.0237(10) 0.0258(10) 0.0304(10) 0.0039(8) 0.0014(8) -0.0025(8) C29 0.0171(8) 0.0214(9) 0.0268(10) 0.0026(8) -0.0013(7) -0.0013(7) C30 0.0258(10) 0.0272(10) 0.0273(10) 0.0027(8) -0.0036(8) -0.0043(8) C31 0.0269(11) 0.0505(14) 0.0351(12) 0.0110(11) -0.0109(10) -0.0107(10) C32 0.0178(10) 0.0659(17) 0.0491(14) 0.0155(13) 0.0007(10) 0.0024(10) C33 0.0256(11) 0.0555(15) 0.0433(13) 0.0027(12) 0.0118(10) 0.0078(10) C34 0.0226(10) 0.0374(12) 0.0312(11) -0.0022(9) 0.0019(8) 0.0012(8) N35 0.0205(8) 0.0256(8) 0.0251(8) -0.0002(7) -0.0008(7) 0.0032(6) Si36 0.0254(3) 0.0361(3) 0.0278(3) 0.0027(3) -0.0065(2) 0.0047(2) C37 0.0542(16) 0.0485(15) 0.0480(15) 0.0041(12) -0.0218(13) -0.0131(12) C38 0.0360(14) 0.104(3) 0.0526(17) -0.0085(17) -0.0140(13) 0.0284(15) C39 0.0453(15) 0.0626(17) 0.0318(12) 0.0140(12) -0.0091(11) 0.0026(12) Si40 0.0245(3) 0.0267(3) 0.0286(3) -0.0025(2) 0.0037(2) 0.0047(2) C41 0.0337(11) 0.0379(12) 0.0296(11) -0.0094(9) 0.0011(9) -0.0037(9) C42 0.0325(12) 0.0671(18) 0.0390(13) 0.0010(13) 0.0116(11) 0.0063(11) C43 0.0554(16) 0.0294(12) 0.0598(17) -0.0038(12) 0.0063(13) 0.0126(11) N44 0.0225(8) 0.0216(8) 0.0273(8) 0.0015(7) 0.0032(7) -0.0030(6) Si45 0.0305(3) 0.0271(3) 0.0323(3) 0.0074(2) 0.0044(2) -0.0074(2) C46 0.0447(14) 0.0470(15) 0.0455(14) 0.0185(12) -0.0051(12) -0.0064(11) C47 0.0617(17) 0.0273(12) 0.0674(18) -0.0007(12) 0.0052(15) -0.0065(11) C48 0.0429(14) 0.075(2) 0.0427(14) 0.0194(14) 0.0100(12) -0.0165(13) Si49 0.0221(3) 0.0265(3) 0.0290(3) -0.0015(2) -0.0002(2) -0.0022(2) C50 0.0349(13) 0.0460(14) 0.0551(16) 0.0085(12) -0.0134(12) -0.0146(10) C51 0.0473(15) 0.0495(15) 0.0497(15) -0.0080(13) 0.0001(12) 0.0179(12) C52 0.0313(12) 0.0482(14) 0.0306(11) 0.0047(10) -0.0034(9) 0.0006(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 Y O1 2.0717(13) . ? Y N44 2.2399(15) . ? Y N35 2.2620(15) . ? Y I 2.9916(2) . ? O1 C2 1.401(2) . ? C2 C5 1.529(2) . ? C2 C11 1.535(3) . ? C2 C3 1.571(2) . ? C3 P4 1.8315(17) . ? P4 C17 1.7993(19) . ? P4 C29 1.8026(18) . ? P4 C23 1.8042(19) . ? C5 C10 1.390(3) . ? C5 C6 1.396(3) . ? C6 C7 1.388(3) . ? C7 C8 1.377(3) . ? C8 C9 1.372(3) . ? C9 C10 1.390(3) . ? C11 C12 1.388(3) . ? C11 C16 1.395(3) . ? C12 C13 1.394(3) . ? C13 C14 1.374(4) . ? C14 C15 1.372(4) . ? C15 C16 1.385(3) . ? C17 C22 1.393(3) . ? C17 C18 1.393(3) . ? C18 C19 1.383(3) . ? C19 C20 1.366(4) . ? C20 C21 1.381(4) . ? C21 C22 1.388(3) . ? C23 C28 1.393(3) . ? C23 C24 1.402(3) . ? C24 C25 1.380(3) . ? C25 C26 1.386(3) . ? C26 C27 1.385(3) . ? C27 C28 1.384(3) . ? C29 C30 1.386(3) . ? C29 C34 1.396(3) . ? C30 C31 1.394(3) . ? C31 C32 1.375(4) . ? C32 C33 1.377(3) . ? C33 C34 1.382(3) . ? N35 Si40 1.7056(17) . ? N35 Si36 1.7195(16) . ? Si36 C39 1.866(2) . ? Si36 C37 1.869(3) . ? Si36 C38 1.878(3) . ? Si40 C43 1.878(2) . ? Si40 C42 1.878(2) . ? Si40 C41 1.885(2) . ? N44 Si45 1.7099(17) . ? N44 Si49 1.7164(17) . ? Si45 C48 1.871(3) . ? Si45 C47 1.875(3) . ? Si45 C46 1.882(2) . ? Si49 C51 1.869(2) . ? Si49 C52 1.873(2) . ? Si49 C50 1.880(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 O1 Y N44 109.09(5) . . ? O1 Y N35 107.35(6) . . ? N44 Y N35 122.70(6) . . ? O1 Y I 100.03(4) . . ? N44 Y I 106.25(4) . . ? N35 Y I 109.10(4) . . ? C2 O1 Y 155.24(11) . . ? O1 C2 C5 108.49(14) . . ? O1 C2 C11 111.05(14) . . ? C5 C2 C11 114.81(15) . . ? O1 C2 C3 103.14(13) . . ? C5 C2 C3 112.48(14) . . ? C11 C2 C3 106.26(14) . . ? C2 C3 P4 127.77(12) . . ? C17 P4 C29 109.37(9) . . ? C17 P4 C23 110.00(9) . . ? C29 P4 C23 108.75(9) . . ? C17 P4 C3 106.49(9) . . ? C29 P4 C3 104.25(8) . . ? C23 P4 C3 117.65(8) . . ? C10 C5 C6 117.48(18) . . ? C10 C5 C2 121.17(16) . . ? C6 C5 C2 121.25(17) . . ? C7 C6 C5 120.8(2) . . ? C8 C7 C6 120.7(2) . . ? C9 C8 C7 119.4(2) . . ? C8 C9 C10 120.2(2) . . ? C5 C10 C9 121.38(19) . . ? C12 C11 C16 117.59(19) . . ? C12 C11 C2 123.88(17) . . ? C16 C11 C2 118.13(17) . . ? C11 C12 C13 120.8(2) . . ? C14 C13 C12 120.4(2) . . ? C15 C14 C13 119.5(2) . . ? C14 C15 C16 120.4(2) . . ? C15 C16 C11 121.2(2) . . ? C22 C17 C18 119.47(19) . . ? C22 C17 P4 123.35(16) . . ? C18 C17 P4 117.17(15) . . ? C19 C18 C17 120.1(2) . . ? C20 C19 C18 120.3(2) . . ? C19 C20 C21 120.2(2) . . ? C20 C21 C22 120.5(2) . . ? C21 C22 C17 119.4(2) . . ? C28 C23 C24 119.65(17) . . ? C28 C23 P4 120.05(14) . . ? C24 C23 P4 120.28(15) . . ? C25 C24 C23 119.65(19) . . ? C24 C25 C26 120.5(2) . . ? C27 C26 C25 120.0(2) . . ? C28 C27 C26 120.2(2) . . ? C27 C28 C23 120.00(19) . . ? C30 C29 C34 120.48(18) . . ? C30 C29 P4 121.40(15) . . ? C34 C29 P4 118.08(14) . . ? C29 C30 C31 119.2(2) . . ? C32 C31 C30 120.0(2) . . ? C31 C32 C33 120.8(2) . . ? C32 C33 C34 120.1(2) . . ? C33 C34 C29 119.4(2) . . ? Si40 N35 Si36 122.72(9) . . ? Si40 N35 Y 112.22(8) . . ? Si36 N35 Y 125.03(9) . . ? N35 Si36 C39 112.12(10) . . ? N35 Si36 C37 110.92(10) . . ? C39 Si36 C37 107.29(13) . . ? N35 Si36 C38 114.97(11) . . ? C39 Si36 C38 105.48(13) . . ? C37 Si36 C38 105.52(15) . . ? N35 Si40 C43 113.02(11) . . ? N35 Si40 C42 114.60(11) . . ? C43 Si40 C42 107.87(12) . . ? N35 Si40 C41 109.16(9) . . ? C43 Si40 C41 106.36(11) . . ? C42 Si40 C41 105.23(11) . . ? Si45 N44 Si49 124.59(9) . . ? Si45 N44 Y 115.49(8) . . ? Si49 N44 Y 119.74(8) . . ? N44 Si45 C48 114.55(11) . . ? N44 Si45 C47 113.49(11) . . ? C48 Si45 C47 106.86(13) . . ? N44 Si45 C46 108.64(10) . . ? C48 Si45 C46 105.50(12) . . ? C47 Si45 C46 107.28(13) . . ? N44 Si49 C51 110.58(10) . . ? N44 Si49 C52 111.49(9) . . ? C51 Si49 C52 107.27(12) . . ? N44 Si49 C50 113.40(10) . . ? C51 Si49 C50 107.92(13) . . ? C52 Si49 C50 105.86(11) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.709 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.078