# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_email STEPHEN.LIDDLE@NOTTINGHAM.AC.UK _publ_section_title ; Synthesis and Reactivity of the Yttrium-Alkyl-Carbene Complex [Y(BIPM)(CH2C6H5)(THF)] (BIPM = {C(PPh2NSiMe3)2}) ; loop_ _publ_author_name 'Stephen Liddle' 'Oliver J. Cooper' 'William Lewis' 'Jonathan McMaster' 'David P. Mills' #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 710583' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 O3 Y' _chemical_formula_sum 'C33 H45 O3 Y' _chemical_formula_weight 578.60 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' O O 0.0106 0.0060 '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 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 17.3179(14) _cell_length_b 20.8626(17) _cell_length_c 8.4199(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.319(2) _cell_angle_gamma 90.00 _cell_volume 3037.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3978 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.61 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7439 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3574 _reflns_number_gt 3354 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0172P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(4) _refine_ls_number_reflns 3574 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.014 _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 Y1 Y 0.071227(19) 0.218049(11) 0.98127(2) 0.02389(8) Uani 1 1 d . . . C1 C 0.0537(2) 0.13701(18) 1.1870(4) 0.0344(9) Uani 1 1 d . . . H1A H 0.0826 0.0985 1.1556 0.041 Uiso 1 1 calc R . . H1B H 0.0805 0.1534 1.2859 0.041 Uiso 1 1 calc R . . C2 C -0.02202(19) 0.11482(16) 1.2300(3) 0.0347(8) Uani 1 1 d . . . C3 C -0.0701(2) 0.15183(18) 1.3212(4) 0.0432(8) Uani 1 1 d . . . H3A H -0.0523 0.1919 1.3625 0.052 Uiso 1 1 calc R . . C4 C -0.1446(2) 0.1301(2) 1.3524(4) 0.0592(12) Uani 1 1 d . . . H4A H -0.1760 0.1557 1.4162 0.071 Uiso 1 1 calc R . . C5 C -0.1732(2) 0.0731(2) 1.2935(5) 0.0632(12) Uani 1 1 d . . . H5A H -0.2239 0.0595 1.3147 0.076 Uiso 1 1 calc R . . C6 C -0.1273(2) 0.0363(2) 1.2041(5) 0.0611(11) Uani 1 1 d . . . H6A H -0.1465 -0.0032 1.1616 0.073 Uiso 1 1 calc R . . C7 C -0.0526(2) 0.05601(17) 1.1743(5) 0.0445(9) Uani 1 1 d . . . H7A H -0.0213 0.0288 1.1143 0.053 Uiso 1 1 calc R . . C8 C 0.0188(2) 0.30426(17) 1.1426(4) 0.0394(8) Uani 1 1 d . . . H8A H -0.0385 0.3024 1.1353 0.047 Uiso 1 1 calc R . . H8B H 0.0367 0.2986 1.2555 0.047 Uiso 1 1 calc R . . C9 C 0.0444(2) 0.36637(15) 1.0857(4) 0.0359(8) Uani 1 1 d . . . C10 C 0.1202(2) 0.38785(15) 1.1187(4) 0.0376(8) Uani 1 1 d . . . H10A H 0.1534 0.3636 1.1895 0.045 Uiso 1 1 calc R . . C11 C 0.1485(3) 0.44304(18) 1.0520(4) 0.0472(10) Uani 1 1 d . . . H11A H 0.2002 0.4564 1.0781 0.057 Uiso 1 1 calc R . . C12 C 0.1015(3) 0.47875(18) 0.9473(5) 0.0577(12) Uani 1 1 d . . . H12A H 0.1213 0.5157 0.8978 0.069 Uiso 1 1 calc R . . C13 C 0.0262(3) 0.46035(18) 0.9154(5) 0.0561(12) Uani 1 1 d . . . H13A H -0.0068 0.4855 0.8463 0.067 Uiso 1 1 calc R . . C14 C -0.0020(2) 0.40521(17) 0.9837(4) 0.0495(10) Uani 1 1 d . . . H14A H -0.0545 0.3935 0.9605 0.059 Uiso 1 1 calc R . . C15 C 0.2071(2) 0.23409(17) 1.0760(4) 0.0333(7) Uani 1 1 d . . . H15A H 0.2281 0.2696 1.0136 0.040 Uiso 1 1 calc R . . H15B H 0.2075 0.2486 1.1880 0.040 Uiso 1 1 calc R . . C16 C 0.26078(18) 0.17977(15) 1.0692(4) 0.0324(7) Uani 1 1 d . . . C17 C 0.2686(2) 0.13444(16) 1.1927(4) 0.0387(8) Uani 1 1 d . . . H17A H 0.2404 0.1405 1.2850 0.046 Uiso 1 1 calc R . . C18 C 0.3159(2) 0.08146(18) 1.1846(5) 0.0517(10) Uani 1 1 d . . . H18A H 0.3197 0.0519 1.2704 0.062 Uiso 1 1 calc R . . C19 C 0.3579(2) 0.07128(19) 1.0514(6) 0.0598(11) Uani 1 1 d . . . H19A H 0.3901 0.0347 1.0447 0.072 Uiso 1 1 calc R . . C20 C 0.3519(2) 0.11490(19) 0.9300(5) 0.0536(10) Uani 1 1 d . . . H20A H 0.3806 0.1086 0.8385 0.064 Uiso 1 1 calc R . . C21 C 0.30468(18) 0.16806(18) 0.9388(4) 0.0420(8) Uani 1 1 d . . . H21A H 0.3021 0.1976 0.8529 0.050 Uiso 1 1 calc R . . O1 O 0.08208(13) 0.28416(9) 0.7505(3) 0.0271(5) Uani 1 1 d . . . C22 C 0.01931(18) 0.31108(15) 0.6459(4) 0.0313(7) Uani 1 1 d . . . H22A H -0.0234 0.3266 0.7091 0.038 Uiso 1 1 calc R . . H22B H -0.0014 0.2783 0.5697 0.038 Uiso 1 1 calc R . . C23 C 0.05495(18) 0.36599(14) 0.5587(4) 0.0316(7) Uani 1 1 d . . . H23A H 0.0496 0.4069 0.6166 0.038 Uiso 1 1 calc R . . H23B H 0.0309 0.3706 0.4497 0.038 Uiso 1 1 calc R . . C24 C 0.13906(19) 0.34628(16) 0.5550(4) 0.0358(7) Uani 1 1 d . . . H24A H 0.1728 0.3838 0.5403 0.043 Uiso 1 1 calc R . . H24B H 0.1467 0.3148 0.4693 0.043 Uiso 1 1 calc R . . C25 C 0.15458(18) 0.31642(16) 0.7181(4) 0.0342(7) Uani 1 1 d . . . H25A H 0.1977 0.2853 0.7173 0.041 Uiso 1 1 calc R . . H25B H 0.1675 0.3497 0.7991 0.041 Uiso 1 1 calc R . . O2 O 0.10990(13) 0.13722(11) 0.7952(3) 0.0296(6) Uani 1 1 d . . . C26 C 0.1124(2) 0.14350(14) 0.6236(4) 0.0362(8) Uani 1 1 d . . . H26A H 0.1554 0.1719 0.5962 0.043 Uiso 1 1 calc R . . H26B H 0.0632 0.1615 0.5773 0.043 Uiso 1 1 calc R . . C27 C 0.1247(2) 0.07664(16) 0.5623(4) 0.0475(9) Uani 1 1 d . . . H27A H 0.0748 0.0545 0.5383 0.057 Uiso 1 1 calc R . . H27B H 0.1546 0.0771 0.4656 0.057 Uiso 1 1 calc R . . C28 C 0.1697(2) 0.04538(16) 0.6994(4) 0.0426(8) Uani 1 1 d . . . H28A H 0.1632 -0.0018 0.6964 0.051 Uiso 1 1 calc R . . H28B H 0.2255 0.0556 0.6975 0.051 Uiso 1 1 calc R . . C29 C 0.13591(19) 0.07325(14) 0.8429(4) 0.0331(7) Uani 1 1 d . . . H29A H 0.0919 0.0470 0.8755 0.040 Uiso 1 1 calc R . . H29B H 0.1753 0.0756 0.9328 0.040 Uiso 1 1 calc R . . O3 O -0.04857(12) 0.19330(10) 0.8393(3) 0.0317(5) Uani 1 1 d . . . C30 C -0.07639(19) 0.12890(15) 0.7996(4) 0.0368(7) Uani 1 1 d . . . H30A H -0.0485 0.0967 0.8676 0.044 Uiso 1 1 calc R . . H30B H -0.0681 0.1189 0.6869 0.044 Uiso 1 1 calc R . . C31 C -0.1618(2) 0.12810(18) 0.8283(5) 0.0434(9) Uani 1 1 d . . . H31A H -0.1751 0.0905 0.8931 0.052 Uiso 1 1 calc R . . H31B H -0.1934 0.1270 0.7265 0.052 Uiso 1 1 calc R . . C32 C -0.1748(2) 0.19045(19) 0.9179(4) 0.0408(8) Uani 1 1 d . . . H32A H -0.2281 0.2068 0.8969 0.049 Uiso 1 1 calc R . . H32B H -0.1643 0.1850 1.0340 0.049 Uiso 1 1 calc R . . C33 C -0.1162(2) 0.23370(16) 0.8477(5) 0.0388(8) Uani 1 1 d . . . H33A H -0.1346 0.2487 0.7407 0.047 Uiso 1 1 calc R . . H33B H -0.1050 0.2713 0.9169 0.047 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 Y1 0.02294(13) 0.02807(13) 0.02037(12) 0.00020(16) -0.00132(8) -0.00040(16) C1 0.036(2) 0.041(2) 0.0263(18) 0.0085(15) 0.0025(15) 0.0038(16) C2 0.0396(19) 0.0451(19) 0.0194(16) 0.0147(14) 0.0029(14) 0.0118(16) C3 0.044(2) 0.061(2) 0.0241(17) 0.0052(16) 0.0022(15) 0.0138(18) C4 0.049(3) 0.102(3) 0.0284(19) 0.022(2) 0.0131(17) 0.035(2) C5 0.038(2) 0.088(3) 0.064(3) 0.036(3) 0.008(2) 0.000(2) C6 0.052(3) 0.055(2) 0.076(3) 0.025(2) 0.003(2) -0.011(2) C7 0.045(2) 0.038(2) 0.051(2) 0.0144(18) 0.0081(18) 0.0051(17) C8 0.042(2) 0.0415(19) 0.035(2) -0.0073(16) 0.0085(17) -0.0007(17) C9 0.048(2) 0.0328(17) 0.0269(17) -0.0135(13) 0.0027(15) 0.0093(16) C10 0.049(2) 0.0356(18) 0.0282(17) -0.0053(14) 0.0031(14) 0.0076(15) C11 0.064(3) 0.040(2) 0.040(2) -0.0106(18) 0.0174(19) -0.0030(19) C12 0.107(4) 0.0265(19) 0.042(2) -0.0060(17) 0.021(2) 0.004(2) C13 0.092(4) 0.036(2) 0.040(2) -0.0069(18) -0.004(2) 0.026(2) C14 0.056(2) 0.044(2) 0.047(2) -0.0188(18) -0.0082(17) 0.0189(18) C15 0.031(2) 0.0420(19) 0.0263(17) -0.0014(14) -0.0079(14) -0.0020(15) C16 0.0218(17) 0.0384(18) 0.0360(18) -0.0030(14) -0.0082(13) -0.0079(14) C17 0.0266(19) 0.0405(19) 0.048(2) 0.0051(16) -0.0060(16) -0.0083(15) C18 0.035(2) 0.042(2) 0.075(3) 0.010(2) -0.0233(19) -0.0091(17) C19 0.034(2) 0.044(2) 0.100(4) -0.011(2) -0.012(2) 0.0034(17) C20 0.032(2) 0.061(3) 0.068(3) -0.013(2) 0.0025(18) 0.0000(18) C21 0.0266(18) 0.053(2) 0.045(2) 0.0027(17) -0.0049(15) -0.0039(15) O1 0.0283(12) 0.0268(11) 0.0261(11) 0.0024(9) 0.0002(9) -0.0025(9) C22 0.0298(17) 0.0323(16) 0.0310(17) 0.0014(14) -0.0037(13) 0.0011(14) C23 0.0383(18) 0.0282(16) 0.0285(16) 0.0038(13) 0.0045(13) 0.0048(14) C24 0.0336(18) 0.0413(18) 0.0330(18) 0.0088(15) 0.0054(14) 0.0018(15) C25 0.0289(17) 0.0402(18) 0.0333(18) -0.0007(15) -0.0009(14) -0.0070(14) O2 0.0389(15) 0.0265(11) 0.0230(12) 0.0027(9) -0.0007(10) 0.0052(10) C26 0.052(2) 0.0322(17) 0.0245(16) 0.0013(13) 0.0071(14) 0.0055(15) C27 0.073(3) 0.0387(19) 0.0306(18) -0.0022(15) 0.0031(17) 0.0068(18) C28 0.050(2) 0.0327(18) 0.045(2) -0.0039(17) 0.0034(17) 0.0117(16) C29 0.0411(19) 0.0279(16) 0.0296(17) 0.0056(13) -0.0039(14) 0.0014(14) O3 0.0226(12) 0.0330(11) 0.0388(13) 0.0036(10) -0.0044(9) -0.0005(10) C30 0.0338(19) 0.0371(17) 0.0388(18) 0.0017(15) -0.0026(14) -0.0059(15) C31 0.0284(19) 0.052(2) 0.049(2) 0.0119(18) -0.0048(16) -0.0120(17) C32 0.0277(19) 0.064(2) 0.0309(19) 0.0083(17) 0.0003(14) 0.0014(17) C33 0.0263(19) 0.043(2) 0.046(2) -0.0016(16) -0.0024(16) 0.0031(15) _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 Y1 O3 2.390(2) . ? Y1 O1 2.399(2) . ? Y1 O2 2.422(2) . ? Y1 C1 2.452(3) . ? Y1 C8 2.459(3) . ? Y1 C15 2.463(3) . ? C1 C2 1.456(5) . ? C2 C3 1.397(5) . ? C2 C7 1.406(5) . ? C3 C4 1.407(6) . ? C4 C5 1.370(6) . ? C5 C6 1.362(6) . ? C6 C7 1.395(5) . ? C8 C9 1.459(5) . ? C9 C10 1.399(5) . ? C9 C14 1.400(5) . ? C10 C11 1.384(5) . ? C11 C12 1.382(6) . ? C12 C13 1.371(7) . ? C13 C14 1.388(6) . ? C15 C16 1.469(5) . ? C16 C21 1.393(5) . ? C16 C17 1.406(5) . ? C17 C18 1.379(5) . ? C18 C19 1.387(6) . ? C19 C20 1.368(6) . ? C20 C21 1.383(5) . ? O1 C25 1.464(4) . ? O1 C22 1.471(4) . ? C22 C23 1.512(4) . ? C23 C24 1.516(4) . ? C24 C25 1.518(4) . ? O2 C26 1.454(4) . ? O2 C29 1.458(4) . ? C26 C27 1.507(4) . ? C27 C28 1.504(5) . ? C28 C29 1.491(4) . ? O3 C33 1.448(4) . ? O3 C30 1.460(4) . ? C30 C31 1.513(5) . ? C31 C32 1.527(5) . ? C32 C33 1.504(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 O3 Y1 O1 79.96(7) . . ? O3 Y1 O2 77.92(8) . . ? O1 Y1 O2 80.73(7) . . ? O3 Y1 C1 93.72(10) . . ? O1 Y1 C1 170.87(11) . . ? O2 Y1 C1 91.55(9) . . ? O3 Y1 C8 95.53(11) . . ? O1 Y1 C8 94.33(10) . . ? O2 Y1 C8 172.35(12) . . ? C1 Y1 C8 92.83(13) . . ? O3 Y1 C15 167.57(9) . . ? O1 Y1 C15 93.78(10) . . ? O2 Y1 C15 90.53(9) . . ? C1 Y1 C15 91.14(12) . . ? C8 Y1 C15 95.65(12) . . ? C2 C1 Y1 123.0(2) . . ? C3 C2 C7 116.2(3) . . ? C3 C2 C1 122.3(3) . . ? C7 C2 C1 121.4(3) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 121.9(4) . . ? C6 C5 C4 118.7(4) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C2 122.2(4) . . ? C9 C8 Y1 109.8(2) . . ? C10 C9 C14 115.8(3) . . ? C10 C9 C8 121.3(3) . . ? C14 C9 C8 122.7(4) . . ? C11 C10 C9 122.5(3) . . ? C12 C11 C10 119.9(4) . . ? C13 C12 C11 119.5(4) . . ? C12 C13 C14 120.3(4) . . ? C13 C14 C9 122.0(4) . . ? C16 C15 Y1 118.5(2) . . ? C21 C16 C17 115.5(3) . . ? C21 C16 C15 122.8(3) . . ? C17 C16 C15 121.6(3) . . ? C18 C17 C16 122.3(4) . . ? C17 C18 C19 120.2(4) . . ? C20 C19 C18 118.8(4) . . ? C19 C20 C21 120.8(4) . . ? C20 C21 C16 122.3(4) . . ? C25 O1 C22 109.0(2) . . ? C25 O1 Y1 121.57(18) . . ? C22 O1 Y1 127.96(17) . . ? O1 C22 C23 105.8(2) . . ? C22 C23 C24 103.0(2) . . ? C23 C24 C25 102.3(2) . . ? O1 C25 C24 104.4(2) . . ? C26 O2 C29 109.3(2) . . ? C26 O2 Y1 127.25(17) . . ? C29 O2 Y1 123.49(17) . . ? O2 C26 C27 105.7(2) . . ? C28 C27 C26 102.5(3) . . ? C29 C28 C27 104.0(3) . . ? O2 C29 C28 105.3(2) . . ? C33 O3 C30 106.8(2) . . ? C33 O3 Y1 122.1(2) . . ? C30 O3 Y1 125.38(18) . . ? O3 C30 C31 106.6(3) . . ? C30 C31 C32 104.0(3) . . ? C33 C32 C31 101.3(3) . . ? O3 C33 C32 103.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.323 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.047 #===END #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 718808' _refine_special_details ; THF disordered over mirror plane. Resolved using a two-part model. SIMU, DELU, DFIX, EADP, and EXYZ restraints and constraints were applied. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H53 N2 O P2 Si2 Y' _chemical_formula_sum 'C42 H53 N2 O P2 Si2 Y' _chemical_formula_weight 808.89 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.4711(7) _cell_length_b 19.2484(13) _cell_length_c 10.6315(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.894(2) _cell_angle_gamma 90.00 _cell_volume 2137.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3496 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.67 _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11198 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3882 _reflns_number_gt 3388 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0465P)^2^+1.0969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3882 _refine_ls_number_parameters 256 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y -0.77675(3) 0.2500 0.09983(3) 0.01973(11) Uani 1 2 d S . . C1 C -0.6857(3) 0.2500 0.3088(3) 0.0223(7) Uani 1 2 d S . . P1 P -0.64370(6) 0.16758(3) 0.29817(6) 0.01916(16) Uani 1 1 d . . . C2 C -0.7114(2) 0.11679(13) 0.4223(2) 0.0217(5) Uani 1 1 d . . . C3 C -0.6507(3) 0.06119(13) 0.4832(3) 0.0300(6) Uani 1 1 d . . . H3 H -0.5668 0.0486 0.4630 0.036 Uiso 1 1 calc R . . C4 C -0.7110(3) 0.02359(15) 0.5738(3) 0.0378(7) Uani 1 1 d . . . H4 H -0.6674 -0.0136 0.6168 0.045 Uiso 1 1 calc R . . C5 C -0.8341(3) 0.04024(15) 0.6014(3) 0.0353(7) Uani 1 1 d . . . H5 H -0.8764 0.0137 0.6614 0.042 Uiso 1 1 calc R . . C6 C -0.8953(3) 0.09553(16) 0.5414(3) 0.0351(7) Uani 1 1 d . . . H6 H -0.9801 0.1072 0.5602 0.042 Uiso 1 1 calc R . . C7 C -0.8340(2) 0.13436(15) 0.4536(3) 0.0302(6) Uani 1 1 d . . . H7 H -0.8761 0.1733 0.4146 0.036 Uiso 1 1 calc R . . C8 C -0.4718(2) 0.15272(12) 0.3169(2) 0.0229(5) Uani 1 1 d . . . C9 C -0.4030(2) 0.13954(15) 0.2125(3) 0.0321(6) Uani 1 1 d . . . H9 H -0.4473 0.1326 0.1325 0.038 Uiso 1 1 calc R . . C10 C -0.2707(3) 0.13639(16) 0.2233(3) 0.0411(7) Uani 1 1 d . . . H10 H -0.2247 0.1285 0.1507 0.049 Uiso 1 1 calc R . . C11 C -0.2055(3) 0.14471(15) 0.3393(3) 0.0421(8) Uani 1 1 d . . . H11 H -0.1147 0.1423 0.3469 0.050 Uiso 1 1 calc R . . C12 C -0.2727(3) 0.15657(15) 0.4441(3) 0.0420(8) Uani 1 1 d . . . H12 H -0.2280 0.1613 0.5244 0.050 Uiso 1 1 calc R . . C13 C -0.4053(3) 0.16164(14) 0.4333(3) 0.0329(6) Uani 1 1 d . . . H13 H -0.4506 0.1712 0.5057 0.039 Uiso 1 1 calc R . . N1 N -0.70043(18) 0.13970(10) 0.16105(18) 0.0216(4) Uani 1 1 d . . . Si1 Si -0.73903(7) 0.05723(4) 0.10973(7) 0.02587(18) Uani 1 1 d . . . C14 C -0.8922(3) 0.02640(16) 0.1709(3) 0.0404(7) Uani 1 1 d . . . H14A H -0.8797 0.0185 0.2619 0.061 Uiso 1 1 calc R . . H14B H -0.9185 -0.0171 0.1287 0.061 Uiso 1 1 calc R . . H14C H -0.9587 0.0616 0.1540 0.061 Uiso 1 1 calc R . . C15 C -0.6150(3) -0.00978(15) 0.1553(3) 0.0439(8) Uani 1 1 d . . . H15A H -0.5334 0.0036 0.1223 0.066 Uiso 1 1 calc R . . H15B H -0.6421 -0.0549 0.1200 0.066 Uiso 1 1 calc R . . H15C H -0.6044 -0.0132 0.2474 0.066 Uiso 1 1 calc R . . C16 C -0.7586(3) 0.06072(16) -0.0660(3) 0.0394(7) Uani 1 1 d . . . H16A H -0.8258 0.0943 -0.0920 0.059 Uiso 1 1 calc R . . H16B H -0.7827 0.0147 -0.0990 0.059 Uiso 1 1 calc R . . H16C H -0.6777 0.0751 -0.0994 0.059 Uiso 1 1 calc R . . C17 C -1.0027(4) 0.2500 0.1285(4) 0.0401(10) Uani 1 2 d S . . H17A H -1.0307 0.2078 0.1723 0.048 Uiso 0.50 1 calc PR . . H17B H -1.0307 0.2922 0.1723 0.048 Uiso 0.50 1 calc PR . . C18 C -1.0426(3) 0.2500 -0.0032(4) 0.0340(9) Uani 1 2 d S . . C19 C -1.0579(3) 0.18824(16) -0.0736(3) 0.0453(8) Uani 1 1 d . . . H19 H -1.0480 0.1449 -0.0312 0.054 Uiso 1 1 calc R . . C20 C -1.0866(4) 0.18853(18) -0.2013(3) 0.0617(10) Uani 1 1 d . . . H20 H -1.0984 0.1457 -0.2451 0.074 Uiso 1 1 calc R . . C21 C -1.0985(6) 0.2500 -0.2668(5) 0.0713(18) Uani 1 2 d S . . H21 H -1.1147 0.2500 -0.3558 0.086 Uiso 1 2 calc SR . . O1 O -0.6863(2) 0.2500 -0.0971(2) 0.0365(7) Uani 1 2 d SDU . . C22 C -0.5503(3) 0.2500 -0.1014(4) 0.0662(13) Uani 0.50 2 d SPDU A 1 H22A H -0.5156 0.2024 -0.0903 0.079 Uiso 0.25 1 calc PR A 1 H22B H -0.5100 0.2802 -0.0346 0.079 Uiso 0.25 1 calc PR A 1 C23 C -0.5261(14) 0.2780(12) -0.2313(7) 0.071(2) Uani 0.25 1 d PDU A 1 H23A H -0.5249 0.3294 -0.2320 0.085 Uiso 0.25 1 calc PR A 1 H23B H -0.4446 0.2602 -0.2607 0.085 Uiso 0.25 1 calc PR A 1 C24 C -0.6391(4) 0.2500 -0.3096(4) 0.0782(14) Uani 0.50 2 d SPDU A 1 H24A H -0.6599 0.2801 -0.3838 0.094 Uiso 0.25 1 calc PR A 1 H24B H -0.6218 0.2024 -0.3392 0.094 Uiso 0.25 1 calc PR A 1 C22A C -0.5503(3) 0.2500 -0.1014(4) 0.0662(13) Uani 0.50 2 d SPDU A 2 H22C H -0.5129 0.2127 -0.0463 0.079 Uiso 0.25 1 calc PR A 2 H22D H -0.5153 0.2950 -0.0698 0.079 Uiso 0.25 1 calc PR A 2 C23A C -0.5137(10) 0.238(2) -0.2356(6) 0.070(2) Uani 0.25 1 d PDU A 2 H23C H -0.4483 0.2723 -0.2592 0.084 Uiso 0.25 1 calc PR A 2 H23D H -0.4813 0.1908 -0.2474 0.084 Uiso 0.25 1 calc PR A 2 C24A C -0.6391(4) 0.2500 -0.3096(4) 0.0782(14) Uani 0.50 2 d SPDU A 2 H24C H -0.6372 0.2950 -0.3545 0.094 Uiso 0.25 1 calc PR A 2 H24D H -0.6532 0.2128 -0.3733 0.094 Uiso 0.25 1 calc PR A 2 C25 C -0.7461(4) 0.2500 -0.2231(3) 0.0505(11) Uani 1 2 d SDU A . H25A H -0.8003 0.2918 -0.2373 0.061 Uiso 0.50 1 calc PR B 1 H25B H -0.8003 0.2082 -0.2373 0.061 Uiso 0.50 1 calc PR B 1 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 Y1 0.01983(18) 0.0220(2) 0.01715(18) 0.000 -0.00015(13) 0.000 C1 0.0236(18) 0.0218(19) 0.0212(18) 0.000 0.0002(14) 0.000 P1 0.0196(3) 0.0178(3) 0.0199(3) 0.0008(2) 0.0000(2) -0.0003(2) C2 0.0249(13) 0.0199(13) 0.0203(12) -0.0032(10) 0.0007(10) -0.0026(10) C3 0.0305(14) 0.0235(14) 0.0367(15) 0.0052(11) 0.0080(12) 0.0049(11) C4 0.0431(17) 0.0300(16) 0.0407(17) 0.0126(13) 0.0054(13) 0.0026(13) C5 0.0419(17) 0.0367(16) 0.0279(15) 0.0081(12) 0.0058(12) -0.0097(13) C6 0.0254(14) 0.0467(19) 0.0340(15) 0.0051(13) 0.0070(12) -0.0013(13) C7 0.0260(14) 0.0338(16) 0.0309(14) 0.0079(12) 0.0019(11) 0.0016(12) C8 0.0214(12) 0.0154(12) 0.0312(14) 0.0032(10) -0.0027(11) -0.0017(10) C9 0.0229(13) 0.0403(17) 0.0329(15) 0.0103(12) 0.0015(11) -0.0005(12) C10 0.0272(15) 0.0475(19) 0.0497(19) 0.0152(15) 0.0101(13) 0.0006(13) C11 0.0191(14) 0.0398(18) 0.066(2) 0.0154(15) -0.0050(14) -0.0052(12) C12 0.0307(16) 0.0380(18) 0.055(2) -0.0029(14) -0.0180(15) -0.0004(13) C13 0.0317(15) 0.0288(16) 0.0370(16) -0.0041(12) -0.0069(12) 0.0028(12) N1 0.0206(10) 0.0227(11) 0.0213(11) -0.0011(8) 0.0015(8) -0.0005(9) Si1 0.0279(4) 0.0216(4) 0.0278(4) -0.0054(3) -0.0002(3) -0.0004(3) C14 0.0389(17) 0.0344(17) 0.0482(18) -0.0060(14) 0.0042(14) -0.0111(13) C15 0.0499(19) 0.0301(17) 0.0508(19) -0.0088(14) -0.0036(15) 0.0090(14) C16 0.0474(18) 0.0385(18) 0.0316(15) -0.0116(13) -0.0031(13) -0.0020(14) C17 0.025(2) 0.060(3) 0.036(2) 0.000 0.0017(17) 0.000 C18 0.0223(19) 0.042(2) 0.038(2) 0.000 0.0031(17) 0.000 C19 0.060(2) 0.0330(18) 0.0429(18) 0.0050(14) 0.0045(15) 0.0027(15) C20 0.104(3) 0.036(2) 0.043(2) -0.0077(15) -0.0037(19) -0.002(2) C21 0.129(5) 0.052(3) 0.030(3) 0.000 -0.013(3) 0.000 O1 0.0331(14) 0.0582(19) 0.0185(13) 0.000 0.0032(11) 0.000 C22 0.042(2) 0.120(4) 0.037(2) 0.000 0.0086(19) 0.000 C23 0.050(4) 0.124(5) 0.041(4) -0.002(4) 0.021(4) -0.001(4) C24 0.066(3) 0.135(4) 0.035(2) 0.000 0.009(2) 0.000 C22A 0.042(2) 0.120(4) 0.037(2) 0.000 0.0086(19) 0.000 C23A 0.054(4) 0.121(6) 0.038(4) 0.004(5) 0.018(3) -0.001(5) C24A 0.066(3) 0.135(4) 0.035(2) 0.000 0.009(2) 0.000 C25 0.053(2) 0.076(3) 0.022(2) 0.000 -0.0029(18) 0.000 _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 Y1 N1 2.345(2) 4_565 ? Y1 N1 2.345(2) . ? Y1 O1 2.356(2) . ? Y1 C1 2.357(3) . ? Y1 C17 2.406(4) . ? Y1 C18 2.921(4) . ? C1 P1 1.6521(12) 4_565 ? C1 P1 1.6521(11) . ? P1 N1 1.627(2) . ? P1 C8 1.820(2) . ? P1 C2 1.824(2) . ? C2 C3 1.383(3) . ? C2 C7 1.390(3) . ? C3 C4 1.390(4) . ? C4 C5 1.379(4) . ? C5 C6 1.377(4) . ? C6 C7 1.387(4) . ? C8 C9 1.388(4) . ? C8 C13 1.388(4) . ? C9 C10 1.384(4) . ? C10 C11 1.377(4) . ? C11 C12 1.377(5) . ? C12 C13 1.389(4) . ? N1 Si1 1.718(2) . ? Si1 C16 1.867(3) . ? Si1 C14 1.868(3) . ? Si1 C15 1.871(3) . ? C17 C18 1.433(6) . ? C18 C19 1.408(4) . ? C18 C19 1.408(4) 4_565 ? C19 C20 1.371(4) . ? C20 C21 1.374(4) . ? C21 C20 1.374(4) 4_565 ? O1 C22 1.429(3) . ? O1 C25 1.439(3) . ? C22 C23 1.519(5) . ? C23 C24 1.500(5) . ? C24 C25 1.498(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N1 129.74(9) 4_565 . ? N1 Y1 O1 95.55(5) 4_565 . ? N1 Y1 O1 95.55(5) . . ? N1 Y1 C1 68.28(5) 4_565 . ? N1 Y1 C1 68.28(5) . . ? O1 Y1 C1 132.56(10) . . ? N1 Y1 C17 106.52(6) 4_565 . ? N1 Y1 C17 106.52(6) . . ? O1 Y1 C17 124.78(11) . . ? C1 Y1 C17 102.66(13) . . ? N1 Y1 C18 113.71(5) 4_565 . ? N1 Y1 C18 113.71(5) . . ? O1 Y1 C18 95.56(10) . . ? C1 Y1 C18 131.88(12) . . ? C17 Y1 C18 29.22(12) . . ? P1 C1 P1 147.6(2) 4_565 . ? P1 C1 Y1 91.62(12) 4_565 . ? P1 C1 Y1 91.62(12) . . ? N1 P1 C1 107.16(14) . . ? N1 P1 C8 110.15(11) . . ? C1 P1 C8 114.15(14) . . ? N1 P1 C2 109.58(10) . . ? C1 P1 C2 110.31(14) . . ? C8 P1 C2 105.45(11) . . ? C3 C2 C7 118.6(2) . . ? C3 C2 P1 124.39(19) . . ? C7 C2 P1 116.97(19) . . ? C2 C3 C4 120.8(2) . . ? C5 C4 C3 120.1(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C7 120.4(3) . . ? C6 C7 C2 120.5(2) . . ? C9 C8 C13 118.6(2) . . ? C9 C8 P1 120.30(19) . . ? C13 C8 P1 120.7(2) . . ? C10 C9 C8 120.9(3) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 119.6(3) . . ? C11 C12 C13 120.5(3) . . ? C8 C13 C12 120.2(3) . . ? P1 N1 Si1 130.77(12) . . ? P1 N1 Y1 92.68(9) . . ? Si1 N1 Y1 132.85(10) . . ? N1 Si1 C16 106.99(12) . . ? N1 Si1 C14 111.85(12) . . ? C16 Si1 C14 108.72(14) . . ? N1 Si1 C15 114.24(12) . . ? C16 Si1 C15 108.12(14) . . ? C14 Si1 C15 106.76(15) . . ? C18 C17 Y1 95.7(2) . . ? C19 C18 C19 115.2(4) . 4_565 ? C19 C18 C17 122.29(19) . . ? C19 C18 C17 122.29(19) 4_565 . ? C19 C18 Y1 105.7(2) . . ? C19 C18 Y1 105.7(2) 4_565 . ? C17 C18 Y1 55.0(2) . . ? C20 C19 C18 122.2(3) . . ? C19 C20 C21 120.8(3) . . ? C20 C21 C20 118.9(5) 4_565 . ? C22 O1 C25 110.0(3) . . ? C22 O1 Y1 119.3(2) . . ? C25 O1 Y1 130.6(2) . . ? O1 C22 C23 104.9(6) . . ? C24 C23 C22 101.8(5) . . ? C25 C24 C23 104.7(6) . . ? O1 C25 C24 106.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.528 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.060 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 718809' _refine_special_details ; Highly disordered lattice solvent moleculess (231 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 2375.7 \%A**3, equating to 5 molecules of toluene per unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H63 N2 O2 P2 Si2 Y, 0.625(C7 H8)' _chemical_formula_sum 'C59.38 H68 N2 O2 P2 Si2 Y' _chemical_formula_weight 1048.69 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 46.514(4) _cell_length_b 10.2277(9) _cell_length_c 26.579(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.543(2) _cell_angle_gamma 90.00 _cell_volume 12121.3(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11075 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.28 _exptl_crystal_description Block _exptl_crystal_colour COlourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4410 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41978 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10641 _reflns_number_gt 8375 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.078P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10641 _refine_ls_number_parameters 583 _refine_ls_number_restraints 397 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.120 _refine_ls_wR_factor_gt 0.114 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.04 _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 Y1 Y 0.148793(5) 0.25565(2) 0.042880(9) 0.02429(9) Uani 1 1 d . . . C1 C 0.12380(5) 0.1377(2) 0.09593(10) 0.0264(5) Uani 1 1 d . . . P1 P 0.146733(14) 0.20429(7) 0.14996(2) 0.02522(15) Uani 1 1 d . . . P2 P 0.090588(14) 0.17040(6) 0.05410(3) 0.02755(16) Uani 1 1 d . . . C2 C 0.16247(5) 0.0776(3) 0.19836(10) 0.0312(6) Uani 1 1 d U . . C3 C 0.16419(6) -0.0486(3) 0.18098(11) 0.0396(7) Uani 1 1 d U . . H3A H 0.1565 -0.0674 0.1446 0.048 Uiso 1 1 calc R . . C4 C 0.17697(7) -0.1492(3) 0.21548(14) 0.0522(8) Uani 1 1 d U . . H4A H 0.1783 -0.2348 0.2025 0.063 Uiso 1 1 calc R . . C5 C 0.18760(7) -0.1242(4) 0.26818(13) 0.0573(9) Uani 1 1 d U . . H5A H 0.1960 -0.1924 0.2921 0.069 Uiso 1 1 calc R . . C6 C 0.18588(8) 0.0005(4) 0.28593(13) 0.0655(10) Uani 1 1 d U . . H6A H 0.1934 0.0184 0.3224 0.079 Uiso 1 1 calc R . . C7 C 0.17338(7) 0.1010(4) 0.25166(11) 0.0528(8) Uani 1 1 d U . . H7A H 0.1723 0.1866 0.2649 0.063 Uiso 1 1 calc R . . C8 C 0.12905(6) 0.3201(3) 0.18391(10) 0.0328(6) Uani 1 1 d U . . C9 C 0.10861(7) 0.2764(3) 0.20993(12) 0.0451(7) Uani 1 1 d U . . H9A H 0.1058 0.1854 0.2138 0.054 Uiso 1 1 calc R . . C10 C 0.09252(7) 0.3666(4) 0.23005(13) 0.0577(9) Uani 1 1 d U . . H10A H 0.0787 0.3368 0.2479 0.069 Uiso 1 1 calc R . . C11 C 0.09628(7) 0.4995(4) 0.22450(14) 0.0607(9) Uani 1 1 d U . . H11A H 0.0849 0.5604 0.2380 0.073 Uiso 1 1 calc R . . C12 C 0.11643(7) 0.5425(3) 0.19950(14) 0.0557(9) Uani 1 1 d U . . H12A H 0.1192 0.6337 0.1959 0.067 Uiso 1 1 calc R . . C13 C 0.13296(6) 0.4533(3) 0.17914(11) 0.0405(7) Uani 1 1 d U . . H13A H 0.1470 0.4842 0.1619 0.049 Uiso 1 1 calc R . . C14 C 0.06402(6) 0.2574(2) 0.08076(11) 0.0316(6) Uani 1 1 d U . . C15 C 0.04811(6) 0.1923(3) 0.10973(12) 0.0411(7) Uani 1 1 d U . . H15A H 0.0504 0.1004 0.1144 0.049 Uiso 1 1 calc R . . C16 C 0.02886(7) 0.2590(3) 0.13207(14) 0.0497(8) Uani 1 1 d U . . H16A H 0.0177 0.2124 0.1512 0.060 Uiso 1 1 calc R . . C17 C 0.02586(7) 0.3928(3) 0.12654(13) 0.0508(8) Uani 1 1 d U . . H17A H 0.0130 0.4388 0.1424 0.061 Uiso 1 1 calc R . . C18 C 0.04165(7) 0.4593(3) 0.09799(13) 0.0519(8) Uani 1 1 d U . . H18A H 0.0394 0.5513 0.0936 0.062 Uiso 1 1 calc R . . C19 C 0.06085(6) 0.3924(3) 0.07574(12) 0.0418(7) Uani 1 1 d U . . H19A H 0.0720 0.4393 0.0568 0.050 Uiso 1 1 calc R . . C20 C 0.07121(6) 0.0163(3) 0.03113(11) 0.0380(6) Uani 1 1 d U . . C21 C 0.04261(8) 0.0118(4) -0.00222(17) 0.0811(13) Uani 1 1 d U . . H21A H 0.0321 0.0911 -0.0135 0.097 Uiso 1 1 calc R . . C22 C 0.02871(10) -0.1069(5) -0.0198(2) 0.0966(15) Uani 1 1 d U . . H22A H 0.0089 -0.1073 -0.0429 0.116 Uiso 1 1 calc R . . C23 C 0.04266(8) -0.2190(4) -0.00479(19) 0.0728(12) Uani 1 1 d U . . H23A H 0.0332 -0.2994 -0.0178 0.087 Uiso 1 1 calc R . . C24 C 0.07072(9) -0.2179(4) 0.0295(2) 0.0890(14) Uani 1 1 d U . . H24A H 0.0806 -0.2982 0.0415 0.107 Uiso 1 1 calc R . . C25 C 0.08507(7) -0.1000(3) 0.04715(17) 0.0675(11) Uani 1 1 d U . . H25A H 0.1048 -0.1007 0.0706 0.081 Uiso 1 1 calc R . . N1 N 0.17323(4) 0.2789(2) 0.13246(8) 0.0268(5) Uani 1 1 d . . . Si1 Si 0.209443(16) 0.32304(7) 0.16540(3) 0.03520(19) Uani 1 1 d . . . C26 C 0.21151(8) 0.4503(4) 0.21660(18) 0.0877(15) Uani 1 1 d . . . H26A H 0.2016 0.5303 0.2000 0.132 Uiso 1 1 calc R . . H26B H 0.2326 0.4691 0.2348 0.132 Uiso 1 1 calc R . . H26C H 0.2014 0.4183 0.2420 0.132 Uiso 1 1 calc R . . C27 C 0.22696(7) 0.3889(4) 0.11594(15) 0.0681(11) Uani 1 1 d . . . H27A H 0.2168 0.4699 0.1011 0.102 Uiso 1 1 calc R . . H27B H 0.2251 0.3245 0.0879 0.102 Uiso 1 1 calc R . . H27C H 0.2482 0.4070 0.1328 0.102 Uiso 1 1 calc R . . C28 C 0.23360(6) 0.1843(3) 0.19873(14) 0.0539(9) Uani 1 1 d . . . H28A H 0.2251 0.1459 0.2252 0.081 Uiso 1 1 calc R . . H28B H 0.2539 0.2165 0.2158 0.081 Uiso 1 1 calc R . . H28C H 0.2345 0.1176 0.1727 0.081 Uiso 1 1 calc R . . N2 N 0.09637(5) 0.25271(19) 0.00528(9) 0.0308(5) Uani 1 1 d . . . Si2 Si 0.074322(18) 0.29611(9) -0.05595(3) 0.0430(2) Uani 1 1 d . . . C29 C 0.09352(9) 0.4329(4) -0.08006(15) 0.0800(12) Uani 1 1 d . . . H29A H 0.1147 0.4105 -0.0747 0.120 Uiso 1 1 calc R . . H29B H 0.0921 0.5128 -0.0606 0.120 Uiso 1 1 calc R . . H29C H 0.0838 0.4471 -0.1175 0.120 Uiso 1 1 calc R . . C30 C 0.03600(7) 0.3581(4) -0.05792(13) 0.0608(10) Uani 1 1 d . . . H30A H 0.0379 0.4365 -0.0360 0.091 Uiso 1 1 calc R . . H30B H 0.0252 0.2904 -0.0446 0.091 Uiso 1 1 calc R . . H30C H 0.0249 0.3798 -0.0942 0.091 Uiso 1 1 calc R . . C31 C 0.07001(8) 0.1600(4) -0.10392(13) 0.0717(12) Uani 1 1 d . . . H31A H 0.0898 0.1342 -0.1067 0.108 Uiso 1 1 calc R . . H31B H 0.0574 0.1889 -0.1383 0.108 Uiso 1 1 calc R . . H31C H 0.0605 0.0852 -0.0920 0.108 Uiso 1 1 calc R . . O1 O 0.17325(4) 0.15149(17) 0.00378(7) 0.0327(4) Uani 1 1 d . . . C32 C 0.18944(6) 0.0669(3) -0.01910(11) 0.0377(6) Uani 1 1 d U . . C33 C 0.21267(7) -0.0140(3) 0.02619(11) 0.0394(6) Uani 1 1 d U . . C34 C 0.23798(7) -0.0728(3) 0.01928(12) 0.0436(7) Uani 1 1 d U . . H34A H 0.2427 -0.0609 -0.0129 0.052 Uiso 1 1 calc R . . C35 C 0.25642(7) -0.1479(3) 0.05772(13) 0.0485(7) Uani 1 1 d U . . H35A H 0.2738 -0.1857 0.0518 0.058 Uiso 1 1 calc R . . C36 C 0.25027(7) -0.1702(3) 0.10523(13) 0.0491(8) Uani 1 1 d U . . H36A H 0.2629 -0.2243 0.1314 0.059 Uiso 1 1 calc R . . C37 C 0.22488(7) -0.1102(3) 0.11311(12) 0.0458(7) Uani 1 1 d U . . H37A H 0.2201 -0.1221 0.1453 0.055 Uiso 1 1 calc R . . C38 C 0.20682(7) -0.0337(3) 0.07418(11) 0.0402(7) Uani 1 1 d U . . H38A H 0.1898 0.0071 0.0803 0.048 Uiso 1 1 calc R . . C39 C 0.16830(6) -0.0354(3) -0.05313(11) 0.0366(6) Uani 1 1 d U . . C40 C 0.14029(7) -0.0590(3) -0.04760(13) 0.0472(7) Uani 1 1 d U . . H40A H 0.1333 -0.0078 -0.0237 0.057 Uiso 1 1 calc R . . C41 C 0.12209(8) -0.1561(3) -0.07634(16) 0.0647(10) Uani 1 1 d U . . H41A H 0.1029 -0.1710 -0.0716 0.078 Uiso 1 1 calc R . . C42 C 0.13141(10) -0.2308(3) -0.11145(16) 0.0709(11) Uani 1 1 d U . . H42A H 0.1187 -0.2965 -0.1313 0.085 Uiso 1 1 calc R . . C43 C 0.15939(10) -0.2099(3) -0.11768(14) 0.0641(10) Uani 1 1 d U . . H43A H 0.1661 -0.2615 -0.1418 0.077 Uiso 1 1 calc R . . C44 C 0.17783(8) -0.1126(3) -0.08859(11) 0.0478(7) Uani 1 1 d U . . H44A H 0.1972 -0.0987 -0.0930 0.057 Uiso 1 1 calc R . . C45 C 0.20718(7) 0.1447(3) -0.04855(12) 0.0447(7) Uani 1 1 d U . . H45A H 0.2229 0.1941 -0.0225 0.054 Uiso 1 1 calc R . . H45B H 0.2175 0.0823 -0.0661 0.054 Uiso 1 1 calc R . . C46 C 0.18976(7) 0.2401(3) -0.08938(12) 0.0410(7) Uani 1 1 d U . . C47 C 0.15915(7) 0.2335(3) -0.11485(13) 0.0469(8) Uani 1 1 d U . . H47A H 0.1472 0.1674 -0.1056 0.056 Uiso 1 1 calc R . . C48 C 0.14609(8) 0.3235(3) -0.15368(13) 0.0521(8) Uani 1 1 d U . . H48A H 0.1252 0.3183 -0.1710 0.062 Uiso 1 1 calc R . . C49 C 0.16275(8) 0.4194(3) -0.16737(13) 0.0548(8) Uani 1 1 d U . . H49A H 0.1535 0.4810 -0.1938 0.066 Uiso 1 1 calc R . . C50 C 0.19245(8) 0.4265(3) -0.14334(13) 0.0563(8) Uani 1 1 d U . . H50A H 0.2041 0.4929 -0.1531 0.068 Uiso 1 1 calc R . . C51 C 0.20595(7) 0.3395(3) -0.10519(12) 0.0480(7) Uani 1 1 d U . . H51A H 0.2269 0.3464 -0.0889 0.058 Uiso 1 1 calc R . . O2 O 0.15420(5) 0.47241(18) 0.02215(8) 0.0450(5) Uani 1 1 d . . . C52 C 0.14061(9) 0.5826(3) 0.04174(16) 0.0656(10) Uani 1 1 d U . . H52A H 0.1234 0.6178 0.0140 0.079 Uiso 1 1 calc R . . H52B H 0.1337 0.5562 0.0721 0.079 Uiso 1 1 calc R . . C53 C 0.16433(9) 0.6780(4) 0.05704(16) 0.0667(10) Uani 1 1 d U . . H53A H 0.1761 0.6649 0.0941 0.080 Uiso 1 1 calc R . . H53B H 0.1559 0.7677 0.0531 0.080 Uiso 1 1 calc R . . C54 C 0.18400(7) 0.6579(3) 0.02088(13) 0.0476(7) Uani 1 1 d U . . H54A H 0.1808 0.7286 -0.0056 0.057 Uiso 1 1 calc R . . H54B H 0.2055 0.6562 0.0411 0.057 Uiso 1 1 calc R . . C55 C 0.17435(7) 0.5272(3) -0.00518(12) 0.0429(7) Uani 1 1 d U . . H55A H 0.1639 0.5389 -0.0429 0.051 Uiso 1 1 calc R . . H55B H 0.1919 0.4695 -0.0016 0.051 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 Y1 0.02687(15) 0.02156(14) 0.02481(14) 0.00101(9) 0.00797(10) 0.00115(9) C1 0.0255(13) 0.0233(13) 0.0300(13) 0.0011(10) 0.0073(10) 0.0020(10) P1 0.0252(3) 0.0265(3) 0.0235(3) -0.0006(3) 0.0063(3) 0.0025(3) P2 0.0241(3) 0.0256(4) 0.0309(4) -0.0008(3) 0.0046(3) -0.0003(3) C2 0.0286(13) 0.0399(15) 0.0268(13) 0.0064(11) 0.0107(11) 0.0046(11) C3 0.0453(16) 0.0358(16) 0.0369(15) 0.0088(12) 0.0100(13) 0.0054(12) C4 0.0511(18) 0.0436(18) 0.063(2) 0.0188(15) 0.0179(16) 0.0138(14) C5 0.0507(18) 0.077(2) 0.0498(19) 0.0338(17) 0.0238(15) 0.0243(17) C6 0.072(2) 0.094(3) 0.0295(16) 0.0150(17) 0.0124(15) 0.035(2) C7 0.0566(19) 0.071(2) 0.0291(15) 0.0035(14) 0.0086(14) 0.0224(16) C8 0.0306(14) 0.0376(15) 0.0278(13) -0.0063(11) 0.0046(11) 0.0065(11) C9 0.0436(16) 0.0545(18) 0.0415(17) -0.0033(14) 0.0190(14) 0.0052(14) C10 0.0473(18) 0.082(2) 0.0494(18) -0.0127(18) 0.0228(15) 0.0111(17) C11 0.0440(18) 0.074(2) 0.062(2) -0.0315(19) 0.0111(16) 0.0156(17) C12 0.0492(19) 0.0481(19) 0.065(2) -0.0229(16) 0.0085(16) 0.0110(15) C13 0.0368(15) 0.0400(16) 0.0422(16) -0.0094(13) 0.0073(12) 0.0053(12) C14 0.0221(13) 0.0314(14) 0.0374(15) 0.0000(11) 0.0022(11) 0.0008(10) C15 0.0313(15) 0.0381(16) 0.0552(18) 0.0031(14) 0.0144(13) 0.0028(12) C16 0.0344(16) 0.061(2) 0.059(2) 0.0066(16) 0.0208(14) 0.0024(14) C17 0.0410(17) 0.058(2) 0.0560(19) -0.0020(16) 0.0180(14) 0.0152(15) C18 0.059(2) 0.0400(18) 0.059(2) 0.0006(15) 0.0210(16) 0.0148(15) C19 0.0428(16) 0.0380(16) 0.0459(17) 0.0008(13) 0.0146(13) 0.0027(13) C20 0.0309(14) 0.0360(15) 0.0468(17) -0.0088(13) 0.0109(12) -0.0071(11) C21 0.057(2) 0.051(2) 0.103(3) 0.003(2) -0.029(2) -0.0182(17) C22 0.068(2) 0.077(3) 0.113(3) -0.012(3) -0.024(2) -0.035(2) C23 0.056(2) 0.053(2) 0.115(3) -0.042(2) 0.032(2) -0.0268(17) C24 0.050(2) 0.0375(19) 0.176(4) -0.031(2) 0.026(2) -0.0052(16) C25 0.0346(17) 0.0325(17) 0.125(3) -0.0180(19) 0.0065(18) -0.0013(13) N1 0.0259(11) 0.0271(11) 0.0275(11) -0.0005(9) 0.0075(9) 0.0009(8) Si1 0.0264(4) 0.0319(4) 0.0426(4) -0.0049(3) 0.0021(3) -0.0023(3) C26 0.052(2) 0.088(3) 0.109(3) -0.064(3) -0.001(2) -0.005(2) C27 0.0321(17) 0.079(3) 0.088(3) 0.035(2) 0.0106(17) -0.0040(17) C28 0.0332(16) 0.057(2) 0.061(2) 0.0133(17) -0.0029(15) -0.0007(15) N2 0.0316(12) 0.0317(12) 0.0273(12) 0.0023(9) 0.0053(9) 0.0021(9) Si2 0.0409(5) 0.0508(5) 0.0306(4) 0.0038(4) -0.0006(3) 0.0127(4) C29 0.086(3) 0.094(3) 0.053(2) 0.036(2) 0.009(2) 0.003(2) C30 0.051(2) 0.069(2) 0.050(2) 0.0007(18) -0.0051(16) 0.0248(17) C31 0.061(2) 0.099(3) 0.0419(19) -0.022(2) -0.0073(16) 0.028(2) O1 0.0381(10) 0.0320(10) 0.0326(10) -0.0018(8) 0.0175(8) 0.0021(8) C32 0.0380(15) 0.0371(15) 0.0429(15) -0.0098(12) 0.0193(12) -0.0032(12) C33 0.0525(17) 0.0293(14) 0.0395(15) -0.0049(12) 0.0183(13) -0.0007(12) C34 0.0478(17) 0.0407(17) 0.0454(17) -0.0084(13) 0.0180(14) -0.0012(13) C35 0.0429(17) 0.0479(18) 0.0566(19) -0.0136(15) 0.0168(14) -0.0009(14) C36 0.0480(18) 0.0393(17) 0.0497(18) -0.0010(14) -0.0025(14) 0.0055(14) C37 0.0587(18) 0.0397(17) 0.0384(16) 0.0039(13) 0.0131(14) 0.0025(14) C38 0.0536(17) 0.0329(15) 0.0395(16) 0.0021(12) 0.0219(13) 0.0087(13) C39 0.0428(15) 0.0310(14) 0.0335(14) -0.0011(11) 0.0070(12) 0.0012(11) C40 0.0398(16) 0.0368(16) 0.0600(19) -0.0032(14) 0.0060(14) -0.0027(13) C41 0.053(2) 0.0421(19) 0.084(3) 0.0064(18) -0.0045(18) -0.0101(15) C42 0.096(3) 0.042(2) 0.054(2) -0.0012(16) -0.014(2) -0.0184(19) C43 0.108(3) 0.0370(17) 0.0386(18) -0.0079(15) 0.0074(19) -0.0015(19) C44 0.068(2) 0.0425(17) 0.0323(15) -0.0027(13) 0.0138(14) 0.0050(15) C45 0.0456(17) 0.0460(17) 0.0463(17) 0.0007(14) 0.0190(13) 0.0032(13) C46 0.0535(17) 0.0358(16) 0.0316(15) -0.0082(11) 0.0088(13) 0.0109(13) C47 0.0518(18) 0.0439(18) 0.0440(18) 0.0064(14) 0.0123(14) -0.0039(14) C48 0.0551(19) 0.0494(19) 0.0469(18) 0.0095(15) 0.0067(15) 0.0026(15) C49 0.075(2) 0.0442(18) 0.0414(17) 0.0026(14) 0.0096(16) -0.0066(16) C50 0.078(2) 0.0458(19) 0.0435(18) 0.0006(15) 0.0141(16) -0.0156(16) C51 0.0495(18) 0.0447(18) 0.0479(18) -0.0133(14) 0.0107(14) -0.0083(14) O2 0.0620(13) 0.0241(10) 0.0601(13) 0.0066(9) 0.0355(11) 0.0029(9) C52 0.092(3) 0.0345(18) 0.090(3) 0.0051(18) 0.058(2) 0.0090(17) C53 0.087(3) 0.047(2) 0.079(2) -0.0179(18) 0.044(2) -0.0087(18) C54 0.0612(19) 0.0317(16) 0.0567(19) -0.0003(14) 0.0278(15) -0.0056(14) C55 0.0578(19) 0.0354(16) 0.0426(17) 0.0022(13) 0.0257(14) -0.0048(13) _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 Y1 O1 2.0450(17) . ? Y1 O2 2.3153(18) . ? Y1 N1 2.340(2) . ? Y1 N2 2.358(2) . ? Y1 C1 2.393(2) . ? C1 P2 1.660(2) . ? C1 P1 1.671(2) . ? P1 N1 1.626(2) . ? P1 C8 1.821(3) . ? P1 C2 1.826(3) . ? P2 N2 1.632(2) . ? P2 C14 1.822(3) . ? P2 C20 1.832(3) . ? C2 C3 1.381(4) . ? C2 C7 1.383(4) . ? C3 C4 1.393(4) . ? C4 C5 1.370(5) . ? C5 C6 1.369(5) . ? C6 C7 1.387(5) . ? C8 C13 1.385(4) . ? C8 C9 1.399(4) . ? C9 C10 1.388(4) . ? C10 C11 1.383(5) . ? C11 C12 1.367(5) . ? C12 C13 1.398(4) . ? C14 C15 1.381(4) . ? C14 C19 1.391(4) . ? C15 C16 1.386(4) . ? C16 C17 1.379(4) . ? C17 C18 1.377(5) . ? C18 C19 1.384(4) . ? C20 C25 1.362(4) . ? C20 C21 1.373(4) . ? C21 C22 1.392(5) . ? C22 C23 1.322(6) . ? C23 C24 1.363(6) . ? C24 C25 1.393(5) . ? N1 Si1 1.723(2) . ? Si1 C27 1.859(4) . ? Si1 C26 1.866(4) . ? Si1 C28 1.870(3) . ? N2 Si2 1.717(2) . ? Si2 C31 1.860(4) . ? Si2 C29 1.868(4) . ? Si2 C30 1.878(3) . ? O1 C32 1.395(3) . ? C32 C45 1.515(4) . ? C32 C39 1.540(4) . ? C32 C33 1.600(4) . ? C33 C34 1.380(4) . ? C33 C38 1.393(4) . ? C34 C35 1.367(4) . ? C35 C36 1.391(4) . ? C36 C37 1.398(4) . ? C37 C38 1.376(4) . ? C39 C40 1.374(4) . ? C39 C44 1.395(4) . ? C40 C41 1.385(4) . ? C41 C42 1.369(6) . ? C42 C43 1.374(6) . ? C43 C44 1.395(5) . ? C45 C46 1.512(4) . ? C46 C47 1.393(4) . ? C46 C51 1.399(4) . ? C47 C48 1.387(4) . ? C48 C49 1.362(5) . ? C49 C50 1.349(5) . ? C50 C51 1.360(5) . ? O2 C55 1.452(3) . ? O2 C52 1.459(4) . ? C52 C53 1.442(5) . ? C53 C54 1.518(4) . ? C54 C55 1.513(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 O1 Y1 O2 105.31(7) . . ? O1 Y1 N1 112.99(7) . . ? O2 Y1 N1 95.20(7) . . ? O1 Y1 N2 115.84(7) . . ? O2 Y1 N2 94.63(7) . . ? N1 Y1 N2 125.22(8) . . ? O1 Y1 C1 118.08(8) . . ? O2 Y1 C1 136.61(8) . . ? N1 Y1 C1 68.19(8) . . ? N2 Y1 C1 68.04(8) . . ? P2 C1 P1 137.58(16) . . ? P2 C1 Y1 91.12(11) . . ? P1 C1 Y1 90.16(10) . . ? N1 P1 C1 107.20(12) . . ? N1 P1 C8 108.81(12) . . ? C1 P1 C8 115.03(12) . . ? N1 P1 C2 110.49(11) . . ? C1 P1 C2 110.26(12) . . ? C8 P1 C2 105.04(12) . . ? N2 P2 C1 107.67(12) . . ? N2 P2 C14 109.91(12) . . ? C1 P2 C14 116.29(12) . . ? N2 P2 C20 110.83(12) . . ? C1 P2 C20 109.02(13) . . ? C14 P2 C20 103.06(12) . . ? C3 C2 C7 117.7(3) . . ? C3 C2 P1 118.5(2) . . ? C7 C2 P1 123.7(2) . . ? C2 C3 C4 121.6(3) . . ? C5 C4 C3 119.8(3) . . ? C6 C5 C4 119.1(3) . . ? C5 C6 C7 121.2(3) . . ? C2 C7 C6 120.5(3) . . ? C13 C8 C9 119.0(3) . . ? C13 C8 P1 120.3(2) . . ? C9 C8 P1 120.2(2) . . ? C10 C9 C8 119.7(3) . . ? C11 C10 C9 120.9(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C13 120.4(3) . . ? C8 C13 C12 120.4(3) . . ? C15 C14 C19 118.2(3) . . ? C15 C14 P2 120.8(2) . . ? C19 C14 P2 120.9(2) . . ? C14 C15 C16 121.0(3) . . ? C17 C16 C15 120.0(3) . . ? C18 C17 C16 119.7(3) . . ? C17 C18 C19 120.1(3) . . ? C18 C19 C14 120.9(3) . . ? C25 C20 C21 117.3(3) . . ? C25 C20 P2 120.2(2) . . ? C21 C20 P2 122.6(2) . . ? C20 C21 C22 121.2(4) . . ? C23 C22 C21 120.9(4) . . ? C22 C23 C24 119.3(3) . . ? C23 C24 C25 120.5(4) . . ? C20 C25 C24 120.8(3) . . ? P1 N1 Si1 133.52(13) . . ? P1 N1 Y1 93.16(9) . . ? Si1 N1 Y1 131.70(11) . . ? N1 Si1 C27 107.31(14) . . ? N1 Si1 C26 113.17(14) . . ? C27 Si1 C26 108.7(2) . . ? N1 Si1 C28 114.25(12) . . ? C27 Si1 C28 106.55(16) . . ? C26 Si1 C28 106.54(19) . . ? P2 N2 Si2 134.27(14) . . ? P2 N2 Y1 93.11(10) . . ? Si2 N2 Y1 131.69(12) . . ? N2 Si2 C31 112.03(14) . . ? N2 Si2 C29 107.69(14) . . ? C31 Si2 C29 107.1(2) . . ? N2 Si2 C30 114.81(14) . . ? C31 Si2 C30 108.50(16) . . ? C29 Si2 C30 106.27(19) . . ? C32 O1 Y1 172.73(17) . . ? O1 C32 C45 109.9(2) . . ? O1 C32 C39 110.1(2) . . ? C45 C32 C39 113.8(2) . . ? O1 C32 C33 109.0(2) . . ? C45 C32 C33 108.0(2) . . ? C39 C32 C33 105.8(2) . . ? C34 C33 C38 117.1(3) . . ? C34 C33 C32 123.0(3) . . ? C38 C33 C32 119.8(2) . . ? C35 C34 C33 121.5(3) . . ? C34 C35 C36 121.5(3) . . ? C35 C36 C37 117.7(3) . . ? C38 C37 C36 119.9(3) . . ? C37 C38 C33 122.3(3) . . ? C40 C39 C44 117.8(3) . . ? C40 C39 C32 121.5(3) . . ? C44 C39 C32 120.6(3) . . ? C39 C40 C41 121.1(3) . . ? C42 C41 C40 120.9(4) . . ? C41 C42 C43 119.3(3) . . ? C42 C43 C44 119.9(4) . . ? C43 C44 C39 121.0(3) . . ? C46 C45 C32 116.8(3) . . ? C47 C46 C51 116.9(3) . . ? C47 C46 C45 125.6(3) . . ? C51 C46 C45 117.4(3) . . ? C48 C47 C46 120.0(3) . . ? C49 C48 C47 121.0(3) . . ? C50 C49 C48 119.8(3) . . ? C49 C50 C51 120.7(3) . . ? C50 C51 C46 121.7(3) . . ? C55 O2 C52 106.7(2) . . ? C55 O2 Y1 128.19(16) . . ? C52 O2 Y1 124.57(17) . . ? C53 C52 O2 104.4(3) . . ? C52 C53 C54 106.3(3) . . ? C55 C54 C53 104.8(2) . . ? O2 C55 C54 105.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.04 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.07 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 718810' _refine_special_details ; Highly disordered lattice solvent molecules (113 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 735.00 \%A**3, equating to 2.7 molecules of benzene per unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. Data were weak and absent at high angle as a result of extensive disorder of P-aryl and SiMe3 groups. This was resolved with two part models. Occupancies were resolved by competitive refinement and then fixed to aid refinement. SIMU, DELU, DFIX, SADI, FLAT and AFIX66 commands required. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110.10 H118.10 N4 O2 P4 Si4 Y2' _chemical_formula_sum 'C110.10 H118.10 N4 O2 P4 Si4 Y2' _chemical_formula_weight 1943.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2508(12) _cell_length_b 19.8328(18) _cell_length_c 20.2611(18) _cell_angle_alpha 90.00 _cell_angle_beta 106.039(2) _cell_angle_gamma 90.00 _cell_volume 5117.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5577 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.47 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2033 _exptl_absorpt_coefficient_mu 1.288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23074 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6686 _reflns_number_gt 5270 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.0836P)^2^+13.1926P] 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 6686 _refine_ls_number_parameters 715 _refine_ls_number_restraints 1025 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.177 _refine_ls_wR_factor_gt 0.169 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.14 _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 Y1 Y 0.03973(4) 0.41700(3) 0.04449(3) 0.0298(2) Uani 1 1 d . . . C1 C 0.0018(4) 0.5378(3) 0.0803(3) 0.0365(15) Uani 1 1 d . . . P1 P 0.10911(12) 0.52739(9) 0.15170(7) 0.0381(4) Uani 1 1 d D . . P2 P -0.10360(10) 0.58462(7) 0.08815(7) 0.0218(3) Uani 1 1 d D . . C2 C 0.0879(8) 0.5504(4) 0.2350(3) 0.0424(16) Uani 0.50 1 d PGDU A 1 C3 C 0.0522(7) 0.4949(4) 0.2640(4) 0.0471(16) Uani 0.50 1 d PGDU A 1 H3A H 0.0373 0.4538 0.2391 0.057 Uiso 0.50 1 calc PR A 1 C4 C 0.0383(8) 0.4996(4) 0.3293(4) 0.0526(17) Uani 0.50 1 d PGDU A 1 H4A H 0.0139 0.4617 0.3492 0.063 Uiso 0.50 1 calc PR A 1 C5 C 0.0601(8) 0.5598(5) 0.3657(2) 0.0528(18) Uani 0.50 1 d PGDU A 1 H5A H 0.0506 0.5630 0.4104 0.063 Uiso 0.50 1 calc PR A 1 C6 C 0.0958(7) 0.6152(4) 0.3367(3) 0.0537(17) Uani 0.50 1 d PGDU A 1 H6A H 0.1107 0.6563 0.3616 0.064 Uiso 0.50 1 calc PR A 1 C7 C 0.1097(7) 0.6105(4) 0.2713(3) 0.0514(18) Uani 0.50 1 d PGDU A 1 H7A H 0.1341 0.6484 0.2515 0.062 Uiso 0.50 1 calc PR A 1 C2A C 0.0778(6) 0.5330(4) 0.2340(2) 0.0393(16) Uani 0.50 1 d PGDU A 2 C3A C -0.0124(6) 0.5024(4) 0.2421(3) 0.0373(16) Uani 0.50 1 d PGDU A 2 H3AA H -0.0587 0.4796 0.2046 0.045 Uiso 0.50 1 calc PR A 2 C4A C -0.0348(6) 0.5052(4) 0.3051(3) 0.0422(16) Uani 0.50 1 d PGDU A 2 H4AA H -0.0964 0.4843 0.3107 0.051 Uiso 0.50 1 calc PR A 2 C5A C 0.0330(7) 0.5387(5) 0.3601(2) 0.0491(17) Uani 0.50 1 d PGDU A 2 H5AA H 0.0177 0.5406 0.4031 0.059 Uiso 0.50 1 calc PR A 2 C6A C 0.1232(6) 0.5693(4) 0.3519(3) 0.0474(17) Uani 0.50 1 d PGDU A 2 H6AA H 0.1696 0.5921 0.3895 0.057 Uiso 0.50 1 calc PR A 2 C7A C 0.1456(5) 0.5664(4) 0.2889(3) 0.0428(16) Uani 0.50 1 d PGDU A 2 H7AA H 0.2072 0.5874 0.2833 0.051 Uiso 0.50 1 calc PR A 2 C8 C 0.2170(4) 0.5819(3) 0.1478(3) 0.0401(13) Uani 0.70 1 d PGDU A 1 C9 C 0.2290(4) 0.6471(3) 0.1739(3) 0.0462(14) Uani 0.70 1 d PGDU A 1 H9A H 0.1787 0.6653 0.1944 0.055 Uiso 0.70 1 calc PR A 1 C10 C 0.3146(4) 0.6858(2) 0.1698(3) 0.0526(15) Uani 0.70 1 d PGDU A 1 H10A H 0.3228 0.7304 0.1876 0.063 Uiso 0.70 1 calc PR A 1 C11 C 0.3882(4) 0.6591(3) 0.1397(3) 0.0511(15) Uani 0.70 1 d PGDU A 1 H11A H 0.4467 0.6856 0.1369 0.061 Uiso 0.70 1 calc PR A 1 C12 C 0.3763(4) 0.5939(3) 0.1136(3) 0.0455(14) Uani 0.70 1 d PGDU A 1 H12A H 0.4266 0.5757 0.0930 0.055 Uiso 0.70 1 calc PR A 1 C13 C 0.2907(4) 0.5553(2) 0.1177(3) 0.0415(14) Uani 0.70 1 d PGDU A 1 H13A H 0.2825 0.5107 0.0999 0.050 Uiso 0.70 1 calc PR A 1 C8A C 0.2232(8) 0.5774(6) 0.1453(5) 0.0432(15) Uani 0.30 1 d PGDU A 2 C9A C 0.2719(8) 0.6219(6) 0.1973(6) 0.0477(16) Uani 0.30 1 d PGDU A 2 H9AA H 0.2420 0.6304 0.2340 0.057 Uiso 0.30 1 calc PR A 2 C10A C 0.3645(8) 0.6539(6) 0.1956(7) 0.0512(18) Uani 0.30 1 d PGDU A 2 H10B H 0.3978 0.6843 0.2312 0.061 Uiso 0.30 1 calc PR A 2 C11A C 0.4083(7) 0.6414(7) 0.1419(8) 0.0483(18) Uani 0.30 1 d PGDU A 2 H11B H 0.4716 0.6633 0.1408 0.058 Uiso 0.30 1 calc PR A 2 C12A C 0.3596(8) 0.5969(7) 0.0899(6) 0.0447(16) Uani 0.30 1 d PGDU A 2 H12B H 0.3895 0.5883 0.0532 0.054 Uiso 0.30 1 calc PR A 2 C13A C 0.2670(8) 0.5649(7) 0.0915(5) 0.0425(16) Uani 0.30 1 d PGDU A 2 H13B H 0.2337 0.5344 0.0560 0.051 Uiso 0.30 1 calc PR A 2 C14 C -0.0631(5) 0.6578(2) 0.1446(3) 0.0345(13) Uani 0.70 1 d PGDU A 1 C15 C -0.0696(5) 0.6610(2) 0.2118(3) 0.0404(13) Uani 0.70 1 d PGDU A 1 H15A H -0.0938 0.6231 0.2317 0.048 Uiso 0.70 1 calc PR A 1 C16 C -0.0405(5) 0.7196(3) 0.2499(2) 0.0461(14) Uani 0.70 1 d PGDU A 1 H16A H -0.0449 0.7218 0.2959 0.055 Uiso 0.70 1 calc PR A 1 C17 C -0.0049(5) 0.7750(2) 0.2208(3) 0.0482(14) Uani 0.70 1 d PGDU A 1 H17A H 0.0149 0.8151 0.2468 0.058 Uiso 0.70 1 calc PR A 1 C18 C 0.0015(5) 0.7718(2) 0.1536(3) 0.0446(14) Uani 0.70 1 d PGDU A 1 H18A H 0.0258 0.8097 0.1336 0.053 Uiso 0.70 1 calc PR A 1 C19 C -0.0275(5) 0.7132(3) 0.1154(2) 0.0390(14) Uani 0.70 1 d PGDU A 1 H19A H -0.0231 0.7110 0.0695 0.047 Uiso 0.70 1 calc PR A 1 C14A C -0.0748(11) 0.6596(5) 0.1435(7) 0.0365(15) Uani 0.30 1 d PGDU A 2 C15A C -0.1292(10) 0.6804(5) 0.1896(7) 0.0385(15) Uani 0.30 1 d PGDU A 2 H15B H -0.1834 0.6529 0.1975 0.046 Uiso 0.30 1 calc PR A 2 C16A C -0.1044(11) 0.7415(6) 0.2239(6) 0.0425(16) Uani 0.30 1 d PGDU A 2 H16B H -0.1416 0.7557 0.2554 0.051 Uiso 0.30 1 calc PR A 2 C17A C -0.0251(12) 0.7817(4) 0.2123(7) 0.0446(15) Uani 0.30 1 d PGDU A 2 H17B H -0.0081 0.8234 0.2357 0.054 Uiso 0.30 1 calc PR A 2 C18A C 0.0293(10) 0.7608(6) 0.1662(8) 0.0422(16) Uani 0.30 1 d PGDU A 2 H18B H 0.0835 0.7883 0.1583 0.051 Uiso 0.30 1 calc PR A 2 C19A C 0.0045(11) 0.6998(7) 0.1319(7) 0.0382(15) Uani 0.30 1 d PGDU A 2 H19B H 0.0417 0.6855 0.1004 0.046 Uiso 0.30 1 calc PR A 2 C20 C -0.2079(4) 0.5392(3) 0.1138(4) 0.0422(14) Uani 0.70 1 d PGDU A 1 C21 C -0.2606(5) 0.5650(3) 0.1589(3) 0.0507(14) Uani 0.70 1 d PGDU A 1 H21A H -0.2394 0.6067 0.1814 0.061 Uiso 0.70 1 calc PR A 1 C22 C -0.3443(4) 0.5296(3) 0.1709(3) 0.0561(15) Uani 0.70 1 d PGDU A 1 H22A H -0.3803 0.5471 0.2017 0.067 Uiso 0.70 1 calc PR A 1 C23 C -0.3754(4) 0.4685(3) 0.1379(4) 0.0555(15) Uani 0.70 1 d PGDU A 1 H23A H -0.4326 0.4443 0.1461 0.067 Uiso 0.70 1 calc PR A 1 C24 C -0.3227(5) 0.4428(3) 0.0929(4) 0.0524(15) Uani 0.70 1 d PGDU A 1 H24A H -0.3439 0.4010 0.0703 0.063 Uiso 0.70 1 calc PR A 1 C25 C -0.2390(5) 0.4782(3) 0.0808(3) 0.0472(14) Uani 0.70 1 d PGDU A 1 H25A H -0.2029 0.4606 0.0500 0.057 Uiso 0.70 1 calc PR A 1 C20A C -0.1892(10) 0.5325(7) 0.1245(7) 0.0425(16) Uani 0.30 1 d PGDU A 2 C21A C -0.1870(9) 0.5327(6) 0.1935(7) 0.0440(17) Uani 0.30 1 d PGDU A 2 H21B H -0.1369 0.5596 0.2252 0.053 Uiso 0.30 1 calc PR A 2 C22A C -0.2582(10) 0.4938(7) 0.2160(6) 0.0485(19) Uani 0.30 1 d PGDU A 2 H22B H -0.2567 0.4940 0.2631 0.058 Uiso 0.30 1 calc PR A 2 C23A C -0.3316(10) 0.4546(7) 0.1695(7) 0.0517(17) Uani 0.30 1 d PGDU A 2 H23B H -0.3803 0.4279 0.1849 0.062 Uiso 0.30 1 calc PR A 2 C24A C -0.3338(10) 0.4543(7) 0.1005(7) 0.0488(17) Uani 0.30 1 d PGDU A 2 H24B H -0.3840 0.4275 0.0687 0.059 Uiso 0.30 1 calc PR A 2 C25A C -0.2626(12) 0.4932(8) 0.0780(6) 0.0444(16) Uani 0.30 1 d PGDU A 2 H25B H -0.2641 0.4930 0.0309 0.053 Uiso 0.30 1 calc PR A 2 N1 N 0.1482(4) 0.4503(3) 0.1507(2) 0.0401(13) Uani 1 1 d . A . Si1 Si 0.2238(3) 0.40075(18) 0.21706(16) 0.0407(8) Uani 0.70 1 d PD A 1 C26 C 0.1721(8) 0.3881(6) 0.2928(4) 0.064(3) Uani 0.70 1 d PDU A 1 H26A H 0.1624 0.4320 0.3125 0.096 Uiso 0.70 1 calc PR A 1 H26B H 0.2221 0.3611 0.3275 0.096 Uiso 0.70 1 calc PR A 1 H26C H 0.1045 0.3645 0.2785 0.096 Uiso 0.70 1 calc PR A 1 C27 C 0.2383(8) 0.3133(3) 0.1874(5) 0.054(2) Uani 0.70 1 d PDU A 1 H27A H 0.1687 0.2930 0.1693 0.081 Uiso 0.70 1 calc PR A 1 H27B H 0.2795 0.2864 0.2261 0.081 Uiso 0.70 1 calc PR A 1 H27C H 0.2744 0.3146 0.1512 0.081 Uiso 0.70 1 calc PR A 1 C28 C 0.3537(5) 0.4422(5) 0.2517(5) 0.047(2) Uani 0.70 1 d PDU A 1 H28A H 0.3434 0.4881 0.2665 0.071 Uiso 0.70 1 calc PR A 1 H28B H 0.3903 0.4441 0.2158 0.071 Uiso 0.70 1 calc PR A 1 H28C H 0.3957 0.4164 0.2909 0.071 Uiso 0.70 1 calc PR A 1 Si1A Si 0.2670(5) 0.4292(3) 0.2206(3) 0.0189(14) Uani 0.30 1 d PD A 2 C26A C 0.3874(10) 0.4289(11) 0.1906(10) 0.042(3) Uani 0.30 1 d PDU A 2 H26D H 0.4028 0.4750 0.1787 0.062 Uiso 0.30 1 calc PR A 2 H26E H 0.3764 0.3999 0.1501 0.062 Uiso 0.30 1 calc PR A 2 H26F H 0.4466 0.4118 0.2272 0.062 Uiso 0.30 1 calc PR A 2 C27A C 0.3115(16) 0.4778(10) 0.3021(7) 0.045(3) Uani 0.30 1 d PDU A 2 H27D H 0.3346 0.5228 0.2924 0.067 Uiso 0.30 1 calc PR A 2 H27E H 0.3700 0.4541 0.3339 0.067 Uiso 0.30 1 calc PR A 2 H27F H 0.2533 0.4821 0.3229 0.067 Uiso 0.30 1 calc PR A 2 C28A C 0.2244(17) 0.3455(7) 0.2449(13) 0.055(3) Uani 0.30 1 d PDU A 2 H28D H 0.1996 0.3175 0.2037 0.082 Uiso 0.30 1 calc PR A 2 H28E H 0.1673 0.3517 0.2665 0.082 Uiso 0.30 1 calc PR A 2 H28F H 0.2838 0.3232 0.2773 0.082 Uiso 0.30 1 calc PR A 2 N2 N -0.1629(3) 0.6120(2) 0.0124(2) 0.0235(10) Uani 1 1 d . . . Si2 Si -0.27509(12) 0.66276(8) -0.00540(8) 0.0337(4) Uani 1 1 d D . . C29 C -0.2439(8) 0.7501(3) -0.0251(7) 0.074(3) Uani 0.70 1 d PDU A 1 H29A H -0.2100 0.7496 -0.0624 0.111 Uiso 0.70 1 calc PR A 1 H29B H -0.1963 0.7705 0.0159 0.111 Uiso 0.70 1 calc PR A 1 H29C H -0.3088 0.7766 -0.0391 0.111 Uiso 0.70 1 calc PR A 1 C30 C -0.3399(10) 0.6707(9) 0.0654(5) 0.111(6) Uani 0.70 1 d PDU A 1 H30A H -0.3201 0.6322 0.0967 0.166 Uiso 0.70 1 calc PR A 1 H30B H -0.4163 0.6713 0.0459 0.166 Uiso 0.70 1 calc PR A 1 H30C H -0.3172 0.7126 0.0908 0.166 Uiso 0.70 1 calc PR A 1 C31 C -0.3799(5) 0.6235(4) -0.0751(4) 0.041(2) Uani 0.70 1 d PDU A 1 H31A H -0.3537 0.6159 -0.1152 0.062 Uiso 0.70 1 calc PR A 1 H31B H -0.4409 0.6535 -0.0877 0.062 Uiso 0.70 1 calc PR A 1 H31C H -0.4004 0.5803 -0.0591 0.062 Uiso 0.70 1 calc PR A 1 C29A C -0.2728(17) 0.7109(10) -0.0840(7) 0.064(4) Uani 0.30 1 d PDU A 2 H29D H -0.2289 0.6871 -0.1083 0.096 Uiso 0.30 1 calc PR A 2 H29E H -0.2438 0.7560 -0.0709 0.096 Uiso 0.30 1 calc PR A 2 H29F H -0.3444 0.7150 -0.1142 0.096 Uiso 0.30 1 calc PR A 2 C30A C -0.270(2) 0.7327(12) 0.0566(12) 0.106(7) Uani 0.30 1 d PDU A 2 H30D H -0.2232 0.7683 0.0487 0.159 Uiso 0.30 1 calc PR A 2 H30E H -0.2431 0.7156 0.1036 0.159 Uiso 0.30 1 calc PR A 2 H30F H -0.3406 0.7512 0.0503 0.159 Uiso 0.30 1 calc PR A 2 C31A C -0.3989(9) 0.6139(9) -0.0198(11) 0.039(3) Uani 0.30 1 d PDU A 2 H31D H -0.4124 0.5895 -0.0634 0.058 Uiso 0.30 1 calc PR A 2 H31E H -0.4572 0.6448 -0.0214 0.058 Uiso 0.30 1 calc PR A 2 H31F H -0.3923 0.5816 0.0178 0.058 Uiso 0.30 1 calc PR A 2 O1 O -0.0374(3) 0.3332(2) 0.0620(2) 0.0425(11) Uani 1 1 d . . . C32 C -0.1008(5) 0.2777(4) 0.0698(4) 0.0502(12) Uani 1 1 d U . . C33 C -0.0485(5) 0.2135(4) 0.0571(4) 0.0601(13) Uani 1 1 d U . . C34 C 0.0362(6) 0.1874(5) 0.1063(5) 0.0865(19) Uani 1 1 d U . . H34A H 0.0588 0.2087 0.1499 0.104 Uiso 1 1 calc R . . C35 C 0.0896(7) 0.1302(5) 0.0932(6) 0.101(2) Uani 1 1 d U . . H35A H 0.1494 0.1141 0.1272 0.121 Uiso 1 1 calc R . . C36 C 0.0569(7) 0.0983(5) 0.0331(6) 0.094(2) Uani 1 1 d U . . H36A H 0.0925 0.0589 0.0251 0.113 Uiso 1 1 calc R . . C37 C -0.0227(7) 0.1204(5) -0.0142(5) 0.0794(17) Uani 1 1 d U . . H37A H -0.0464 0.0965 -0.0563 0.095 Uiso 1 1 calc R . . C38 C -0.0742(6) 0.1794(4) -0.0038(5) 0.0673(15) Uani 1 1 d U . . H38A H -0.1293 0.1964 -0.0406 0.081 Uiso 1 1 calc R . . C39 C -0.1152(5) 0.2771(4) 0.1427(4) 0.0579(13) Uani 1 1 d U . . C40 C -0.1431(6) 0.2181(5) 0.1702(4) 0.0732(16) Uani 1 1 d U . . H40A H -0.1503 0.1771 0.1451 0.088 Uiso 1 1 calc R . . C41 C -0.1608(7) 0.2198(5) 0.2362(4) 0.0852(18) Uani 1 1 d U . . H41A H -0.1833 0.1801 0.2542 0.102 Uiso 1 1 calc R . . C42 C -0.1460(8) 0.2771(5) 0.2735(5) 0.0880(18) Uani 1 1 d U . . H42A H -0.1538 0.2767 0.3187 0.106 Uiso 1 1 calc R . . C43 C -0.1201(7) 0.3350(5) 0.2468(4) 0.0788(17) Uani 1 1 d U . . H43A H -0.1127 0.3757 0.2725 0.095 Uiso 1 1 calc R . . C44 C -0.1041(6) 0.3351(5) 0.1815(4) 0.0670(15) Uani 1 1 d U . . H44A H -0.0853 0.3759 0.1635 0.080 Uiso 1 1 calc R . . C45 C -0.2109(5) 0.2907(4) 0.0173(3) 0.0508(13) Uani 1 1 d U . . H45A H -0.2323 0.3370 0.0257 0.061 Uiso 1 1 calc R . . H45B H -0.2002 0.2905 -0.0291 0.061 Uiso 1 1 calc R . . C46 C -0.3025(5) 0.2456(4) 0.0147(4) 0.0565(13) Uani 1 1 d U . . C47 C -0.3582(5) 0.2504(4) 0.0626(4) 0.0653(15) Uani 1 1 d U . . H47A H -0.3365 0.2816 0.0993 0.078 Uiso 1 1 calc R . . C48 C -0.4462(6) 0.2099(5) 0.0580(5) 0.0724(16) Uani 1 1 d U . . H48A H -0.4830 0.2135 0.0920 0.087 Uiso 1 1 calc R . . C49 C -0.4796(6) 0.1658(5) 0.0058(5) 0.0801(17) Uani 1 1 d U . . H49A H -0.5373 0.1368 0.0043 0.096 Uiso 1 1 calc R . . C50 C -0.4297(6) 0.1633(5) -0.0444(5) 0.0838(17) Uani 1 1 d U . . H50A H -0.4553 0.1345 -0.0829 0.101 Uiso 1 1 calc R . . C51 C -0.3415(6) 0.2029(5) -0.0396(5) 0.0738(16) Uani 1 1 d U . . H51A H -0.3072 0.2003 -0.0750 0.089 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 Y1 0.0244(3) 0.0433(4) 0.0259(4) 0.0171(3) 0.0138(2) 0.0141(2) C1 0.032(3) 0.059(4) 0.021(3) 0.013(3) 0.012(3) 0.022(3) P1 0.0338(9) 0.0639(12) 0.0187(8) 0.0122(8) 0.0107(7) 0.0242(8) P2 0.0192(7) 0.0258(8) 0.0223(8) 0.0012(6) 0.0088(6) 0.0017(6) C2 0.050(3) 0.055(3) 0.023(3) 0.008(2) 0.012(3) 0.019(3) C3 0.058(3) 0.058(3) 0.027(3) 0.007(3) 0.015(3) 0.016(3) C4 0.067(4) 0.063(4) 0.029(3) 0.006(3) 0.017(3) 0.011(3) C5 0.066(4) 0.064(4) 0.028(3) 0.003(3) 0.013(3) 0.012(3) C6 0.064(4) 0.065(4) 0.030(3) 0.001(3) 0.010(3) 0.010(3) C7 0.060(4) 0.063(4) 0.029(3) 0.003(3) 0.010(3) 0.009(3) C2A 0.048(3) 0.053(4) 0.019(3) 0.010(3) 0.014(3) 0.021(3) C3A 0.044(3) 0.052(4) 0.019(3) 0.010(3) 0.014(3) 0.024(3) C4A 0.052(4) 0.057(4) 0.022(3) 0.008(3) 0.018(3) 0.021(3) C5A 0.064(4) 0.062(4) 0.025(3) 0.004(3) 0.017(3) 0.015(3) C6A 0.060(4) 0.061(4) 0.022(3) 0.003(3) 0.013(3) 0.017(3) C7A 0.053(3) 0.056(4) 0.020(3) 0.005(3) 0.011(3) 0.019(3) C8 0.039(3) 0.053(3) 0.027(3) -0.001(2) 0.007(2) 0.014(2) C9 0.049(3) 0.053(3) 0.032(3) -0.001(3) 0.003(3) 0.014(3) C10 0.052(3) 0.056(3) 0.041(3) -0.004(3) -0.001(3) 0.007(2) C11 0.045(3) 0.056(3) 0.043(3) -0.002(3) -0.003(2) 0.001(2) C12 0.034(3) 0.058(3) 0.040(3) -0.005(3) 0.002(2) 0.004(2) C13 0.035(3) 0.056(3) 0.031(3) -0.006(3) 0.005(2) 0.007(2) C8A 0.041(3) 0.054(3) 0.031(3) 0.000(3) 0.004(3) 0.012(3) C9A 0.049(3) 0.055(3) 0.035(3) -0.002(3) 0.004(3) 0.014(3) C10A 0.051(3) 0.055(4) 0.040(3) -0.004(3) -0.001(3) 0.008(3) C11A 0.042(3) 0.055(4) 0.040(3) -0.003(3) -0.001(3) 0.005(3) C12A 0.036(3) 0.056(3) 0.037(3) -0.004(3) 0.001(3) 0.005(3) C13A 0.035(3) 0.055(3) 0.033(3) -0.003(3) 0.003(3) 0.008(3) C14 0.031(3) 0.046(3) 0.028(2) -0.004(2) 0.011(2) -0.006(2) C15 0.040(3) 0.052(3) 0.030(3) -0.007(2) 0.011(2) -0.009(2) C16 0.047(3) 0.057(3) 0.033(3) -0.011(2) 0.008(2) -0.013(3) C17 0.049(3) 0.055(3) 0.038(3) -0.013(2) 0.006(2) -0.015(2) C18 0.046(3) 0.050(3) 0.038(3) -0.009(2) 0.012(3) -0.015(3) C19 0.039(3) 0.047(3) 0.033(3) -0.006(2) 0.013(2) -0.010(2) C14A 0.034(3) 0.047(3) 0.029(3) -0.005(3) 0.011(3) -0.008(2) C15A 0.037(3) 0.050(3) 0.029(3) -0.007(3) 0.010(3) -0.008(3) C16A 0.042(3) 0.053(3) 0.032(3) -0.010(3) 0.009(3) -0.009(3) C17A 0.045(3) 0.052(3) 0.036(3) -0.011(3) 0.008(3) -0.012(3) C18A 0.042(3) 0.049(3) 0.035(3) -0.007(3) 0.010(3) -0.011(3) C19A 0.037(3) 0.047(3) 0.032(3) -0.005(3) 0.011(3) -0.009(3) C20 0.037(3) 0.043(3) 0.057(3) -0.019(2) 0.030(2) -0.012(2) C21 0.046(3) 0.055(3) 0.063(3) -0.022(3) 0.034(3) -0.016(2) C22 0.048(3) 0.065(3) 0.067(3) -0.018(3) 0.035(3) -0.019(3) C23 0.044(3) 0.059(3) 0.071(4) -0.011(3) 0.028(3) -0.020(3) C24 0.039(3) 0.049(3) 0.074(3) -0.017(3) 0.024(3) -0.015(2) C25 0.036(3) 0.047(3) 0.066(3) -0.022(2) 0.027(2) -0.012(2) C20A 0.037(3) 0.045(3) 0.058(3) -0.020(3) 0.033(3) -0.012(3) C21A 0.039(3) 0.048(3) 0.059(3) -0.019(3) 0.035(3) -0.013(3) C22A 0.042(4) 0.055(4) 0.063(4) -0.016(3) 0.037(3) -0.016(3) C23A 0.041(3) 0.056(3) 0.069(3) -0.014(3) 0.032(3) -0.016(3) C24A 0.037(3) 0.049(3) 0.069(3) -0.019(3) 0.029(3) -0.014(3) C25A 0.035(3) 0.045(3) 0.063(3) -0.021(3) 0.030(3) -0.011(3) N1 0.038(3) 0.064(4) 0.022(3) 0.016(3) 0.015(2) 0.021(3) Si1 0.036(2) 0.060(2) 0.0247(16) 0.0140(17) 0.0063(15) 0.0201(17) C26 0.063(5) 0.076(6) 0.052(5) 0.029(5) 0.015(5) 0.027(5) C27 0.053(5) 0.054(5) 0.051(5) 0.027(4) 0.008(4) 0.012(4) C28 0.039(5) 0.055(5) 0.038(5) -0.001(4) -0.006(4) 0.009(4) Si1A 0.014(4) 0.021(4) 0.018(3) 0.002(3) -0.002(3) 0.003(2) C26A 0.033(6) 0.051(7) 0.034(6) -0.003(6) -0.001(6) 0.006(6) C27A 0.035(7) 0.054(7) 0.035(6) -0.002(6) -0.006(6) 0.011(6) C28A 0.054(5) 0.061(6) 0.049(6) 0.029(5) 0.013(5) 0.019(5) N2 0.020(2) 0.028(2) 0.023(3) -0.001(2) 0.007(2) 0.0061(19) Si2 0.0254(8) 0.0416(10) 0.0301(10) -0.0076(8) 0.0008(7) 0.0134(7) C29 0.040(5) 0.038(6) 0.126(10) -0.016(6) -0.006(6) 0.011(4) C30 0.087(10) 0.193(17) 0.047(7) 0.005(9) 0.011(7) 0.110(11) C31 0.025(4) 0.050(5) 0.043(5) 0.009(4) 0.000(4) 0.002(4) C29A 0.032(7) 0.032(7) 0.117(11) -0.016(7) 0.000(7) 0.009(6) C30A 0.085(11) 0.187(18) 0.043(8) 0.004(10) 0.012(8) 0.110(11) C31A 0.023(6) 0.051(7) 0.037(7) 0.011(6) 0.001(6) 0.003(5) O1 0.034(2) 0.056(3) 0.043(3) 0.026(2) 0.020(2) 0.010(2) C32 0.036(2) 0.065(3) 0.056(3) 0.034(2) 0.024(2) 0.012(2) C33 0.040(3) 0.064(3) 0.082(3) 0.028(2) 0.027(2) 0.014(2) C34 0.054(3) 0.075(4) 0.117(4) 0.017(3) 0.001(3) 0.024(3) C35 0.066(4) 0.084(4) 0.136(5) 0.012(4) -0.002(4) 0.030(3) C36 0.067(4) 0.079(4) 0.130(5) 0.012(3) 0.018(4) 0.026(3) C37 0.066(3) 0.072(4) 0.106(4) 0.018(3) 0.033(3) 0.019(3) C38 0.055(3) 0.068(3) 0.088(3) 0.026(3) 0.035(3) 0.017(3) C39 0.047(3) 0.079(3) 0.053(3) 0.038(2) 0.023(2) 0.007(3) C40 0.074(3) 0.090(3) 0.059(3) 0.044(3) 0.025(3) -0.001(3) C41 0.095(4) 0.102(4) 0.065(3) 0.047(3) 0.033(3) -0.006(4) C42 0.099(4) 0.109(4) 0.067(4) 0.037(3) 0.043(3) 0.002(4) C43 0.086(4) 0.102(4) 0.062(3) 0.030(3) 0.043(3) 0.003(3) C44 0.065(3) 0.089(3) 0.056(3) 0.030(3) 0.033(3) 0.005(3) C45 0.039(2) 0.072(3) 0.048(3) 0.030(3) 0.022(2) 0.017(2) C46 0.039(2) 0.083(3) 0.055(3) 0.032(2) 0.025(2) 0.014(2) C47 0.040(3) 0.098(4) 0.066(3) 0.035(3) 0.028(2) 0.019(3) C48 0.040(3) 0.109(4) 0.077(4) 0.043(3) 0.032(3) 0.016(3) C49 0.048(3) 0.111(4) 0.086(4) 0.038(3) 0.028(3) 0.002(3) C50 0.060(3) 0.112(4) 0.084(4) 0.022(3) 0.029(3) -0.011(3) C51 0.057(3) 0.101(4) 0.071(3) 0.019(3) 0.032(3) -0.005(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 Y1 O1 2.034(4) . ? Y1 N2 2.316(4) 3_565 ? Y1 N1 2.329(5) . ? Y1 C1 2.592(6) . ? Y1 C1 2.595(5) 3_565 ? C1 P2 1.721(5) . ? C1 P1 1.738(6) . ? P1 N1 1.616(6) . ? P1 C8 1.811(3) . ? P1 C2A 1.829(3) . ? P1 C8A 1.842(3) . ? P1 C2 1.842(3) . ? P2 N2 1.612(4) . ? P2 C14 1.833(3) . ? P2 C20A 1.833(3) . ? P2 C14A 1.838(3) . ? P2 C20 1.841(3) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C2A C3A 1.3900 . ? C2A C7A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C6A C7A 1.3900 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C8A C9A 1.3900 . ? C8A C13A 1.3900 . ? C9A C10A 1.3900 . ? C10A C11A 1.3900 . ? C11A C12A 1.3900 . ? C12A C13A 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C14A C15A 1.3900 . ? C14A C19A 1.3900 . ? C15A C16A 1.3900 . ? C16A C17A 1.3900 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C20A C21A 1.3900 . ? C20A C25A 1.3900 . ? C21A C22A 1.3900 . ? C22A C23A 1.3900 . ? C23A C24A 1.3900 . ? C24A C25A 1.3900 . ? N1 Si1 1.742(6) . ? N1 Si1A 1.851(7) . ? Si1 C28 1.861(5) . ? Si1 C27 1.862(5) . ? Si1 C26 1.863(5) . ? Si1A C26A 1.858(5) . ? Si1A C27A 1.861(5) . ? Si1A C28A 1.864(5) . ? N2 Si2 1.749(4) . ? Si2 C29 1.850(5) . ? Si2 C31 1.856(5) . ? Si2 C31A 1.858(5) . ? Si2 C30A 1.861(5) . ? Si2 C29A 1.864(5) . ? Si2 C30 1.871(5) . ? O1 C32 1.419(8) . ? C32 C33 1.506(10) . ? C32 C39 1.540(9) . ? C32 C45 1.571(9) . ? C33 C38 1.366(11) . ? C33 C34 1.379(11) . ? C34 C35 1.402(13) . ? C35 C36 1.333(14) . ? C36 C37 1.290(12) . ? C37 C38 1.399(11) . ? C39 C44 1.377(11) . ? C39 C40 1.390(10) . ? C40 C41 1.420(11) . ? C41 C42 1.349(13) . ? C42 C43 1.355(12) . ? C43 C44 1.396(10) . ? C45 C46 1.496(10) . ? C46 C51 1.372(11) . ? C46 C47 1.374(10) . ? C47 C48 1.398(11) . ? C48 C49 1.349(13) . ? C49 C50 1.359(12) . ? C50 C51 1.389(11) . ? 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 Y1 N2 109.96(16) . 3_565 ? O1 Y1 N1 106.41(18) . . ? N2 Y1 N1 100.99(15) 3_565 . ? O1 Y1 C1 124.10(17) . . ? N2 Y1 C1 125.94(17) 3_565 . ? N1 Y1 C1 66.23(17) . . ? O1 Y1 C1 118.11(19) . 3_565 ? N2 Y1 C1 65.75(16) 3_565 3_565 ? N1 Y1 C1 135.5(2) . 3_565 ? C1 Y1 C1 87.03(19) . 3_565 ? P2 C1 P1 119.1(3) . . ? P2 C1 Y1 138.6(3) . . ? P1 C1 Y1 86.9(2) . . ? P2 C1 Y1 86.8(2) . 3_565 ? P1 C1 Y1 139.1(3) . 3_565 ? Y1 C1 Y1 92.97(19) . 3_565 ? N1 P1 C1 107.0(3) . . ? N1 P1 C8 107.7(3) . . ? C1 P1 C8 111.6(3) . . ? N1 P1 C2A 102.9(3) . . ? C1 P1 C2A 114.3(3) . . ? C8 P1 C2A 112.6(3) . . ? N1 P1 C8A 103.7(5) . . ? C1 P1 C8A 112.1(5) . . ? C2A P1 C8A 115.4(3) . . ? N1 P1 C2 112.1(3) . . ? C1 P1 C2 115.8(4) . . ? C8 P1 C2 102.4(4) . . ? C8A P1 C2 105.5(4) . . ? N2 P2 C1 106.8(2) . . ? N2 P2 C14 108.0(3) . . ? C1 P2 C14 112.3(3) . . ? N2 P2 C20A 112.3(5) . . ? C1 P2 C20A 109.9(5) . . ? C14 P2 C20A 107.6(5) . . ? N2 P2 C14A 105.8(5) . . ? C1 P2 C14A 117.1(5) . . ? C20A P2 C14A 105.0(7) . . ? N2 P2 C20 103.1(3) . . ? C1 P2 C20 117.0(3) . . ? C14 P2 C20 108.9(3) . . ? C14A P2 C20 105.6(5) . . ? C3 C2 C7 120.0 . . ? C3 C2 P1 110.3(5) . . ? C7 C2 P1 129.5(5) . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C7 120.0 . . ? C6 C7 C2 120.0 . . ? C3A C2A C7A 120.0 . . ? C3A C2A P1 120.0(4) . . ? C7A C2A P1 120.0(4) . . ? C4A C3A C2A 120.0 . . ? C3A C4A C5A 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C7A 120.0 . . ? C6A C7A C2A 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 123.2(3) . . ? C13 C8 P1 116.8(3) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C8 120.0 . . ? C9A C8A C13A 120.0 . . ? C9A C8A P1 120.4(2) . . ? C13A C8A P1 119.2(2) . . ? C10A C9A C8A 120.0 . . ? C11A C10A C9A 120.0 . . ? C10A C11A C12A 120.0 . . ? C11A C12A C13A 120.0 . . ? C12A C13A C8A 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 P2 124.1(4) . . ? C19 C14 P2 115.9(4) . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C14 120.0 . . ? C15A C14A C19A 120.0 . . ? C15A C14A P2 126.2(8) . . ? C19A C14A P2 113.5(8) . . ? C16A C15A C14A 120.0 . . ? C15A C16A C17A 120.0 . . ? C18A C17A C16A 120.0 . . ? C19A C18A C17A 120.0 . . ? C18A C19A C14A 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 P2 124.0(3) . . ? C25 C20 P2 115.8(3) . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C21A C20A C25A 120.0 . . ? C21A C20A P2 123.9(8) . . ? C25A C20A P2 116.0(8) . . ? C20A C21A C22A 120.0 . . ? C23A C22A C21A 120.0 . . ? C22A C23A C24A 120.0 . . ? C25A C24A C23A 120.0 . . ? C24A C25A C20A 120.0 . . ? P1 N1 Si1 130.0(3) . . ? P1 N1 Si1A 114.3(4) . . ? P1 N1 Y1 99.3(2) . . ? Si1 N1 Y1 129.0(3) . . ? Si1A N1 Y1 145.1(3) . . ? N1 Si1 C28 108.4(4) . . ? N1 Si1 C27 111.4(4) . . ? C28 Si1 C27 111.5(5) . . ? N1 Si1 C26 116.6(4) . . ? C28 Si1 C26 105.2(5) . . ? C27 Si1 C26 103.6(5) . . ? N1 Si1A C26A 112.1(7) . . ? N1 Si1A C27A 123.8(7) . . ? C26A Si1A C27A 101.6(10) . . ? N1 Si1A C28A 98.5(8) . . ? C26A Si1A C28A 115.7(10) . . ? C27A Si1A C28A 105.8(11) . . ? P2 N2 Si2 123.6(3) . . ? P2 N2 Y1 99.51(19) . 3_565 ? Si2 N2 Y1 135.7(2) . 3_565 ? N2 Si2 C29 110.8(4) . . ? N2 Si2 C31 109.3(3) . . ? C29 Si2 C31 113.2(5) . . ? N2 Si2 C31A 113.3(7) . . ? N2 Si2 C30A 114.8(8) . . ? C31A Si2 C30A 111.2(13) . . ? N2 Si2 C29A 104.9(7) . . ? C31A Si2 C29A 110.8(9) . . ? C30A Si2 C29A 100.9(13) . . ? N2 Si2 C30 115.7(4) . . ? C29 Si2 C30 105.3(7) . . ? C31 Si2 C30 102.3(6) . . ? C32 O1 Y1 174.1(4) . . ? O1 C32 C33 108.7(5) . . ? O1 C32 C39 110.3(6) . . ? C33 C32 C39 110.0(6) . . ? O1 C32 C45 105.4(5) . . ? C33 C32 C45 114.1(6) . . ? C39 C32 C45 108.2(5) . . ? C38 C33 C34 114.6(8) . . ? C38 C33 C32 124.2(7) . . ? C34 C33 C32 121.0(8) . . ? C33 C34 C35 121.4(10) . . ? C36 C35 C34 120.2(9) . . ? C37 C36 C35 120.7(10) . . ? C36 C37 C38 120.3(10) . . ? C33 C38 C37 122.7(8) . . ? C44 C39 C40 118.2(7) . . ? C44 C39 C32 121.3(6) . . ? C40 C39 C32 120.5(8) . . ? C39 C40 C41 119.2(9) . . ? C42 C41 C40 120.8(8) . . ? C41 C42 C43 120.3(8) . . ? C42 C43 C44 120.0(10) . . ? C39 C44 C43 121.4(8) . . ? C46 C45 C32 121.2(5) . . ? C51 C46 C47 116.8(7) . . ? C51 C46 C45 121.3(6) . . ? C47 C46 C45 121.5(8) . . ? C46 C47 C48 121.0(9) . . ? C49 C48 C47 120.8(8) . . ? C48 C49 C50 119.3(9) . . ? C49 C50 C51 120.0(10) . . ? C46 C51 C50 121.9(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.93 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.09 # Attachment '6.cif' data_yccphn _database_code_depnum_ccdc_archive 'CCDC 718811' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H63 N2 O P2 Si2 Y, 0.5(C4 H10 O)' _chemical_formula_sum 'C56 H68 N4 O1.50 P2 Si2 Y' _chemical_formula_weight 1028.17 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.719(2) _cell_length_b 19.171(2) _cell_length_c 25.914(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10790(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3187 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.02 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4328 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 54011 _diffrn_reflns_av_R_equivalents 0.1355 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9557 _reflns_number_gt 5374 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0612P)^2^+4.8784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9557 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Y1 Y 0.15828(2) 0.76556(2) 0.149172(17) 0.02670(13) Uani 1 1 d . . . N1 N 0.20876(16) 0.75148(19) 0.22831(14) 0.0297(9) Uani 1 1 d . . . P1 P 0.26636(6) 0.80117(7) 0.21187(5) 0.0301(3) Uani 1 1 d . . . C1 C 0.2480(2) 0.8389(2) 0.15566(17) 0.0296(11) Uani 1 1 d . . . P2 P 0.26515(6) 0.82466(7) 0.09367(5) 0.0295(3) Uani 1 1 d . . . N2 N 0.21294(16) 0.77273(19) 0.06938(14) 0.0301(9) Uani 1 1 d . . . C2 C 0.3371(2) 0.7503(3) 0.21145(17) 0.0340(12) Uani 1 1 d . . . C3 C 0.3356(2) 0.6783(3) 0.21090(17) 0.0391(13) Uani 1 1 d . . . H3A H 0.2970 0.6550 0.2126 0.047 Uiso 1 1 calc R . . C4 C 0.3894(3) 0.6393(3) 0.20783(19) 0.0484(15) Uani 1 1 d . . . H4A H 0.3873 0.5898 0.2069 0.058 Uiso 1 1 calc R . . C5 C 0.4450(3) 0.6717(4) 0.2061(2) 0.0546(16) Uani 1 1 d . . . H5A H 0.4818 0.6449 0.2045 0.066 Uiso 1 1 calc R . . C6 C 0.4480(2) 0.7433(4) 0.20669(19) 0.0500(16) Uani 1 1 d . . . H6A H 0.4870 0.7658 0.2051 0.060 Uiso 1 1 calc R . . C7 C 0.3944(2) 0.7833(3) 0.20956(18) 0.0399(13) Uani 1 1 d . . . H7A H 0.3969 0.8328 0.2102 0.048 Uiso 1 1 calc R . . C8 C 0.2798(2) 0.8661(3) 0.26232(19) 0.0370(13) Uani 1 1 d . . . C9 C 0.2530(2) 0.9312(3) 0.2575(2) 0.0475(14) Uani 1 1 d . . . H9A H 0.2307 0.9427 0.2271 0.057 Uiso 1 1 calc R . . C10 C 0.2586(3) 0.9799(3) 0.2970(2) 0.0616(17) Uani 1 1 d . . . H10A H 0.2401 1.0246 0.2935 0.074 Uiso 1 1 calc R . . C11 C 0.2908(3) 0.9636(4) 0.3411(3) 0.069(2) Uani 1 1 d . . . H11A H 0.2946 0.9971 0.3679 0.082 Uiso 1 1 calc R . . C12 C 0.3172(3) 0.8995(4) 0.3463(2) 0.0564(17) Uani 1 1 d . . . H12A H 0.3392 0.8885 0.3770 0.068 Uiso 1 1 calc R . . C13 C 0.3124(2) 0.8500(3) 0.3074(2) 0.0469(14) Uani 1 1 d . . . H13A H 0.3311 0.8055 0.3113 0.056 Uiso 1 1 calc R . . C14 C 0.2619(2) 0.9051(3) 0.05666(19) 0.0334(12) Uani 1 1 d . . . C15 C 0.2237(2) 0.9582(3) 0.0726(2) 0.0423(14) Uani 1 1 d . . . H15A H 0.2037 0.9549 0.1051 0.051 Uiso 1 1 calc R . . C16 C 0.2138(3) 1.0170(3) 0.0418(3) 0.0578(17) Uani 1 1 d . . . H16A H 0.1871 1.0531 0.0532 0.069 Uiso 1 1 calc R . . C17 C 0.2431(3) 1.0223(3) -0.0056(3) 0.0582(17) Uani 1 1 d . . . H17A H 0.2365 1.0622 -0.0267 0.070 Uiso 1 1 calc R . . C18 C 0.2814(3) 0.9707(3) -0.0220(2) 0.0591(17) Uani 1 1 d . . . H18A H 0.3014 0.9745 -0.0545 0.071 Uiso 1 1 calc R . . C19 C 0.2911(2) 0.9123(3) 0.0088(2) 0.0473(15) Uani 1 1 d . . . H19A H 0.3182 0.8767 -0.0028 0.057 Uiso 1 1 calc R . . C20 C 0.3426(2) 0.7919(3) 0.08188(18) 0.0337(12) Uani 1 1 d . . . C21 C 0.3931(2) 0.8356(3) 0.0826(2) 0.0481(14) Uani 1 1 d . . . H21A H 0.3875 0.8844 0.0871 0.058 Uiso 1 1 calc R . . C22 C 0.4524(3) 0.8085(4) 0.0767(2) 0.0570(17) Uani 1 1 d . . . H22A H 0.4870 0.8387 0.0767 0.068 Uiso 1 1 calc R . . C23 C 0.4602(3) 0.7375(4) 0.0709(2) 0.0576(17) Uani 1 1 d . . . H23A H 0.5006 0.7190 0.0675 0.069 Uiso 1 1 calc R . . C24 C 0.4110(3) 0.6936(3) 0.0699(2) 0.0512(16) Uani 1 1 d . . . H24A H 0.4167 0.6448 0.0654 0.061 Uiso 1 1 calc R . . C25 C 0.3524(2) 0.7210(3) 0.07558(18) 0.0407(14) Uani 1 1 d . . . H25A H 0.3180 0.6904 0.0751 0.049 Uiso 1 1 calc R . . Si1 Si 0.18257(6) 0.72248(7) 0.28742(5) 0.0341(3) Uani 1 1 d . . . C26 C 0.1492(3) 0.7932(3) 0.3281(2) 0.0506(15) Uani 1 1 d . . . H26A H 0.1804 0.8295 0.3338 0.076 Uiso 1 1 calc R . . H26B H 0.1363 0.7739 0.3613 0.076 Uiso 1 1 calc R . . H26C H 0.1136 0.8136 0.3104 0.076 Uiso 1 1 calc R . . C27 C 0.1200(2) 0.6585(3) 0.2751(2) 0.0508(15) Uani 1 1 d . . . H27A H 0.0877 0.6805 0.2544 0.076 Uiso 1 1 calc R . . H27B H 0.1026 0.6429 0.3081 0.076 Uiso 1 1 calc R . . H27C H 0.1367 0.6183 0.2564 0.076 Uiso 1 1 calc R . . C28 C 0.2426(2) 0.6781(3) 0.32707(18) 0.0429(14) Uani 1 1 d . . . H28A H 0.2668 0.7132 0.3457 0.064 Uiso 1 1 calc R . . H28B H 0.2698 0.6511 0.3045 0.064 Uiso 1 1 calc R . . H28C H 0.2228 0.6468 0.3519 0.064 Uiso 1 1 calc R . . Si2 Si 0.19577(6) 0.75129(7) 0.00654(5) 0.0348(4) Uani 1 1 d . . . C29 C 0.1373(2) 0.6809(3) 0.0085(2) 0.0505(15) Uani 1 1 d . . . H29A H 0.1007 0.6976 0.0268 0.076 Uiso 1 1 calc R . . H29B H 0.1543 0.6403 0.0266 0.076 Uiso 1 1 calc R . . H29C H 0.1261 0.6676 -0.0267 0.076 Uiso 1 1 calc R . . C30 C 0.2626(2) 0.7192(3) -0.03225(19) 0.0428(14) Uani 1 1 d . . . H30A H 0.2832 0.6813 -0.0136 0.064 Uiso 1 1 calc R . . H30B H 0.2918 0.7575 -0.0378 0.064 Uiso 1 1 calc R . . H30C H 0.2480 0.7019 -0.0657 0.064 Uiso 1 1 calc R . . C31 C 0.1616(2) 0.8246(3) -0.03227(19) 0.0486(14) Uani 1 1 d . . . H31A H 0.1267 0.8447 -0.0135 0.073 Uiso 1 1 calc R . . H31B H 0.1475 0.8067 -0.0657 0.073 Uiso 1 1 calc R . . H31C H 0.1929 0.8607 -0.0379 0.073 Uiso 1 1 calc R . . N3 N 0.05310(17) 0.8097(2) 0.11627(14) 0.0308(10) Uani 1 1 d . . . N4 N 0.07690(17) 0.8299(2) 0.16623(14) 0.0317(10) Uani 1 1 d . . . C32 C 0.0630(2) 0.8618(3) 0.07463(18) 0.0358(12) Uani 1 1 d . . . H32A H 0.0571 0.8381 0.0411 0.043 Uiso 1 1 calc R . . H32B H 0.1064 0.8775 0.0762 0.043 Uiso 1 1 calc R . . C33 C 0.0222(2) 0.9260(3) 0.07540(18) 0.0343(12) Uani 1 1 d . . . C34 C -0.0343(2) 0.9270(3) 0.0509(2) 0.0448(14) Uani 1 1 d . . . H34A H -0.0472 0.8874 0.0316 0.054 Uiso 1 1 calc R . . C35 C -0.0725(3) 0.9847(3) 0.0538(2) 0.0559(17) Uani 1 1 d . . . H35A H -0.1112 0.9845 0.0366 0.067 Uiso 1 1 calc R . . C36 C -0.0548(3) 1.0414(3) 0.0810(2) 0.0596(17) Uani 1 1 d . . . H36A H -0.0817 1.0803 0.0839 0.072 Uiso 1 1 calc R . . C37 C 0.0032(3) 1.0431(3) 0.1052(2) 0.0558(17) Uani 1 1 d . . . H37A H 0.0164 1.0831 0.1237 0.067 Uiso 1 1 calc R . . C38 C 0.0403(3) 0.9849(3) 0.1011(2) 0.0450(14) Uani 1 1 d . . . H38A H 0.0799 0.9858 0.1167 0.054 Uiso 1 1 calc R . . C39 C 0.0006(2) 0.7654(3) 0.11408(17) 0.0308(11) Uani 1 1 d . . . C40 C -0.0249(2) 0.7450(3) 0.06680(19) 0.0398(13) Uani 1 1 d . . . H40A H -0.0085 0.7630 0.0356 0.048 Uiso 1 1 calc R . . C41 C -0.0739(2) 0.6987(3) 0.0650(2) 0.0447(14) Uani 1 1 d . . . H41A H -0.0904 0.6851 0.0326 0.054 Uiso 1 1 calc R . . C42 C -0.0988(2) 0.6724(3) 0.1097(2) 0.0487(15) Uani 1 1 d . . . H42A H -0.1330 0.6416 0.1084 0.058 Uiso 1 1 calc R . . C43 C -0.0734(2) 0.6913(3) 0.1563(2) 0.0436(14) Uani 1 1 d . . . H43A H -0.0898 0.6722 0.1872 0.052 Uiso 1 1 calc R . . C44 C -0.0246(2) 0.7375(3) 0.15907(18) 0.0357(12) Uani 1 1 d . . . H44A H -0.0082 0.7503 0.1917 0.043 Uiso 1 1 calc R . . C45 C 0.0453(2) 0.8798(2) 0.19563(18) 0.0318(12) Uani 1 1 d . . . C46 C 0.0811(2) 0.9131(3) 0.2337(2) 0.0434(14) Uani 1 1 d . . . H46A H 0.1230 0.9001 0.2382 0.052 Uiso 1 1 calc R . . C47 C 0.0559(3) 0.9642(3) 0.2644(2) 0.0597(17) Uani 1 1 d . . . H47A H 0.0808 0.9867 0.2895 0.072 Uiso 1 1 calc R . . C48 C -0.0049(3) 0.9832(3) 0.2590(2) 0.0601(17) Uani 1 1 d . . . H48A H -0.0220 1.0186 0.2803 0.072 Uiso 1 1 calc R . . C49 C -0.0404(2) 0.9502(3) 0.2225(2) 0.0458(14) Uani 1 1 d . . . H49A H -0.0823 0.9634 0.2186 0.055 Uiso 1 1 calc R . . C50 C -0.0168(2) 0.8986(3) 0.19136(19) 0.0340(12) Uani 1 1 d . . . H50A H -0.0426 0.8758 0.1670 0.041 Uiso 1 1 calc R . . O1 O 0.13860(15) 0.64424(16) 0.14183(12) 0.0372(8) Uani 1 1 d . . . C51 C 0.0815(2) 0.6059(3) 0.1318(2) 0.0491(15) Uani 1 1 d . . . H51A H 0.0589 0.6272 0.1027 0.059 Uiso 1 1 calc R . . H51B H 0.0547 0.6066 0.1627 0.059 Uiso 1 1 calc R . . C52 C 0.0994(3) 0.5330(3) 0.1191(2) 0.0614(17) Uani 1 1 d . . . H52A H 0.1120 0.5284 0.0825 0.074 Uiso 1 1 calc R . . H52B H 0.0658 0.4997 0.1266 0.074 Uiso 1 1 calc R . . C53 C 0.1551(3) 0.5234(3) 0.1566(2) 0.0623(17) Uani 1 1 d . . . H53A H 0.1411 0.5164 0.1926 0.075 Uiso 1 1 calc R . . H53B H 0.1814 0.4837 0.1461 0.075 Uiso 1 1 calc R . . C54 C 0.1884(3) 0.5926(3) 0.1502(3) 0.0659(19) Uani 1 1 d . . . H54A H 0.2124 0.6041 0.1816 0.079 Uiso 1 1 calc R . . H54B H 0.2166 0.5911 0.1202 0.079 Uiso 1 1 calc R . . C55 C 0.5868(9) 0.9524(10) 0.1034(6) 0.118(7) Uani 0.50 1 d P . . H55A H 0.6201 0.9756 0.1223 0.176 Uiso 0.50 1 calc PR A 1 H55B H 0.6030 0.9108 0.0861 0.176 Uiso 0.50 1 calc PR A 1 H55C H 0.5543 0.9387 0.1276 0.176 Uiso 0.50 1 calc PR A 1 C56 C 0.5622(11) 0.9986(13) 0.0662(11) 0.122(11) Uani 0.50 1 d P B 1 H56A H 0.5491 1.0417 0.0842 0.146 Uiso 0.50 1 calc PR B 1 H56B H 0.5958 1.0117 0.0422 0.146 Uiso 0.50 1 calc PR B 1 O2 O 0.5148(10) 0.9755(8) 0.0382(8) 0.099(5) Uani 0.50 1 d P . 1 C57 C 0.4989(10) 1.0277(8) 0.0000(12) 0.089(6) Uani 0.50 1 d P C 1 H57A H 0.5357 1.0410 -0.0203 0.107 Uiso 0.50 1 calc PR C 1 H57B H 0.4823 1.0699 0.0170 0.107 Uiso 0.50 1 calc PR C 1 C58 C 0.4512(17) 0.995(3) -0.0342(15) 0.156(17) Uani 0.50 1 d P C 1 H58A H 0.4329 1.0314 -0.0562 0.234 Uiso 0.50 1 calc PR C 1 H58B H 0.4191 0.9738 -0.0130 0.234 Uiso 0.50 1 calc PR C 1 H58C H 0.4705 0.9596 -0.0559 0.234 Uiso 0.50 1 calc PR C 1 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 Y1 0.0238(2) 0.0314(2) 0.0250(2) -0.0025(2) 0.0012(2) -0.0014(2) N1 0.023(2) 0.039(3) 0.027(2) -0.0026(18) -0.0003(17) -0.0012(18) P1 0.0246(7) 0.0371(8) 0.0286(7) -0.0073(6) 0.0002(6) 0.0001(6) C1 0.027(3) 0.030(3) 0.032(3) -0.004(2) 0.004(2) 0.003(2) P2 0.0263(7) 0.0297(7) 0.0325(7) -0.0001(6) 0.0049(6) 0.0005(6) N2 0.030(2) 0.030(2) 0.030(2) -0.0023(18) 0.0051(18) -0.0025(18) C2 0.028(3) 0.045(3) 0.029(3) -0.005(2) -0.007(2) 0.002(2) C3 0.031(3) 0.057(4) 0.029(3) -0.013(2) -0.009(2) 0.006(3) C4 0.045(4) 0.063(4) 0.037(3) -0.013(3) -0.003(3) 0.016(3) C5 0.034(4) 0.093(5) 0.037(3) -0.007(3) 0.000(3) 0.020(3) C6 0.025(3) 0.091(5) 0.033(3) -0.005(3) 0.000(2) 0.003(3) C7 0.029(3) 0.057(4) 0.034(3) -0.002(3) 0.002(2) -0.002(3) C8 0.027(3) 0.047(4) 0.037(3) -0.010(3) 0.007(2) -0.009(2) C9 0.049(4) 0.048(4) 0.046(3) -0.013(3) 0.000(3) -0.007(3) C10 0.072(4) 0.049(4) 0.064(4) -0.023(3) 0.012(4) -0.006(3) C11 0.076(5) 0.074(5) 0.056(5) -0.037(4) 0.014(4) -0.023(4) C12 0.049(4) 0.081(5) 0.039(3) -0.019(3) 0.000(3) -0.015(3) C13 0.035(3) 0.066(4) 0.040(3) -0.016(3) -0.005(3) -0.006(3) C14 0.024(3) 0.036(3) 0.041(3) -0.002(2) -0.002(2) -0.005(2) C15 0.045(3) 0.038(3) 0.044(3) -0.004(3) -0.007(3) -0.003(3) C16 0.058(4) 0.035(3) 0.080(5) -0.003(3) -0.022(4) 0.009(3) C17 0.063(4) 0.042(4) 0.070(5) 0.021(3) -0.023(4) -0.013(3) C18 0.057(4) 0.058(4) 0.061(4) 0.023(3) 0.007(3) 0.002(3) C19 0.042(3) 0.046(3) 0.054(4) 0.014(3) 0.012(3) 0.000(3) C20 0.033(3) 0.038(3) 0.030(3) 0.003(2) 0.007(2) 0.005(3) C21 0.040(3) 0.054(4) 0.050(4) 0.007(3) 0.006(3) 0.005(3) C22 0.032(3) 0.077(5) 0.062(4) 0.012(4) 0.010(3) 0.002(3) C23 0.041(4) 0.091(5) 0.041(3) 0.011(4) 0.008(3) 0.028(4) C24 0.054(4) 0.063(4) 0.036(3) 0.000(3) 0.000(3) 0.025(3) C25 0.040(3) 0.053(4) 0.029(3) 0.000(2) -0.001(2) 0.006(3) Si1 0.0290(7) 0.0440(9) 0.0294(8) 0.0010(7) 0.0006(6) 0.0031(6) C26 0.055(4) 0.058(4) 0.039(3) 0.011(3) 0.016(3) 0.020(3) C27 0.043(3) 0.073(4) 0.036(3) 0.009(3) 0.004(3) -0.016(3) C28 0.043(3) 0.054(4) 0.032(3) 0.000(3) -0.002(3) 0.003(3) Si2 0.0381(8) 0.0399(9) 0.0262(7) -0.0032(6) 0.0035(6) -0.0006(6) C29 0.056(4) 0.060(4) 0.036(3) -0.003(3) -0.002(3) -0.013(3) C30 0.053(4) 0.039(3) 0.036(3) -0.006(2) 0.004(3) 0.000(3) C31 0.053(4) 0.057(4) 0.035(3) 0.001(3) 0.003(3) 0.010(3) N3 0.024(2) 0.043(3) 0.025(2) -0.0018(19) -0.0034(18) -0.0022(19) N4 0.024(2) 0.044(3) 0.027(2) -0.0031(19) -0.0028(17) -0.0004(19) C32 0.029(3) 0.051(3) 0.028(3) 0.004(2) 0.007(2) -0.005(2) C33 0.032(3) 0.042(3) 0.029(3) 0.011(2) 0.002(2) -0.001(2) C34 0.044(4) 0.055(4) 0.036(3) 0.004(3) -0.005(3) -0.001(3) C35 0.045(4) 0.071(5) 0.052(4) 0.019(3) -0.007(3) 0.011(3) C36 0.070(5) 0.047(4) 0.062(4) 0.018(3) 0.015(4) 0.016(3) C37 0.080(5) 0.041(4) 0.046(4) 0.003(3) 0.009(3) -0.004(4) C38 0.051(4) 0.042(4) 0.041(3) 0.013(3) -0.003(3) -0.006(3) C39 0.024(3) 0.038(3) 0.031(3) -0.004(2) 0.000(2) 0.006(2) C40 0.033(3) 0.050(4) 0.036(3) 0.000(3) -0.003(2) -0.003(3) C41 0.035(3) 0.057(4) 0.041(3) -0.013(3) -0.007(3) -0.001(3) C42 0.040(3) 0.056(4) 0.051(4) -0.009(3) 0.002(3) -0.012(3) C43 0.038(3) 0.046(4) 0.046(3) -0.001(3) 0.013(3) -0.010(3) C44 0.034(3) 0.041(3) 0.032(3) -0.005(2) 0.002(2) -0.002(2) C45 0.032(3) 0.033(3) 0.030(3) -0.002(2) 0.007(2) 0.004(2) C46 0.036(3) 0.048(4) 0.046(3) -0.009(3) -0.009(3) 0.000(3) C47 0.062(4) 0.058(4) 0.059(4) -0.023(3) -0.008(3) 0.009(3) C48 0.067(4) 0.050(4) 0.064(4) -0.023(3) 0.009(4) 0.017(3) C49 0.043(3) 0.046(4) 0.049(4) -0.004(3) 0.008(3) 0.010(3) C50 0.031(3) 0.038(3) 0.033(3) 0.001(2) 0.004(2) 0.002(2) O1 0.037(2) 0.032(2) 0.042(2) -0.0021(16) 0.0004(16) -0.0067(16) C51 0.041(3) 0.042(4) 0.064(4) 0.003(3) 0.005(3) -0.007(3) C52 0.062(4) 0.055(4) 0.068(4) -0.009(3) 0.000(4) -0.015(3) C53 0.065(4) 0.051(4) 0.071(4) -0.005(3) 0.005(4) 0.007(3) C54 0.038(3) 0.051(4) 0.109(6) -0.037(4) -0.006(4) -0.001(3) C55 0.18(2) 0.109(16) 0.068(12) -0.001(10) -0.006(12) -0.021(14) C56 0.056(14) 0.076(14) 0.23(4) 0.03(2) 0.03(2) 0.001(10) O2 0.109(14) 0.098(12) 0.089(11) -0.015(9) -0.019(12) -0.010(9) C57 0.082(15) 0.062(11) 0.124(17) 0.002(15) 0.026(14) -0.019(12) C58 0.12(3) 0.24(5) 0.12(3) -0.01(3) -0.02(3) -0.02(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 Y1 N4 2.200(4) . ? Y1 N1 2.341(4) . ? Y1 O1 2.373(3) . ? Y1 N2 2.388(4) . ? Y1 C1 2.408(5) . ? Y1 N3 2.581(4) . ? Y1 P1 2.9353(13) . ? Y1 P2 2.9563(13) . ? N1 P1 1.629(4) . ? N1 Si1 1.726(4) . ? P1 C1 1.674(5) . ? P1 C2 1.820(5) . ? P1 C8 1.829(5) . ? C1 P2 1.671(4) . ? P2 N2 1.635(4) . ? P2 C14 1.817(5) . ? P2 C20 1.821(5) . ? N2 Si2 1.721(4) . ? C2 C3 1.381(7) . ? C2 C7 1.396(6) . ? C3 C4 1.390(6) . ? C3 H3A 0.9500 . ? C4 C5 1.360(7) . ? C4 H4A 0.9500 . ? C5 C6 1.375(8) . ? C5 H5A 0.9500 . ? C6 C7 1.397(7) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.383(7) . ? C8 C13 1.401(7) . ? C9 C10 1.389(7) . ? C9 H9A 0.9500 . ? C10 C11 1.377(8) . ? C10 H10A 0.9500 . ? C11 C12 1.364(9) . ? C11 H11A 0.9500 . ? C12 C13 1.389(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.378(7) . ? C14 C19 1.400(7) . ? C15 C16 1.397(7) . ? C15 H15A 0.9500 . ? C16 C17 1.387(8) . ? C16 H16A 0.9500 . ? C17 C18 1.360(8) . ? C17 H17A 0.9500 . ? C18 C19 1.392(7) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.379(7) . ? C20 C25 1.386(7) . ? C21 C22 1.397(7) . ? C21 H21A 0.9500 . ? C22 C23 1.379(8) . ? C22 H22A 0.9500 . ? C23 C24 1.362(8) . ? C23 H23A 0.9500 . ? C24 C25 1.385(7) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? Si1 C27 1.859(5) . ? Si1 C26 1.864(5) . ? Si1 C28 1.866(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Si2 C29 1.853(5) . ? Si2 C30 1.870(5) . ? Si2 C31 1.881(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N3 C39 1.423(6) . ? N3 N4 1.447(5) . ? N3 C32 1.486(6) . ? N4 C45 1.402(6) . ? C32 C33 1.514(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.370(7) . ? C33 C34 1.383(7) . ? C34 C35 1.385(7) . ? C34 H34A 0.9500 . ? C35 C36 1.352(8) . ? C35 H35A 0.9500 . ? C36 C37 1.407(8) . ? C36 H36A 0.9500 . ? C37 C38 1.381(7) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.395(6) . ? C39 C40 1.401(6) . ? C40 C41 1.385(7) . ? C40 H40A 0.9500 . ? C41 C42 1.373(7) . ? C41 H41A 0.9500 . ? C42 C43 1.378(7) . ? C42 H42A 0.9500 . ? C43 C44 1.382(6) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.401(6) . ? C45 C46 1.408(6) . ? C46 C47 1.375(7) . ? C46 H46A 0.9500 . ? C47 C48 1.377(8) . ? C47 H47A 0.9500 . ? C48 C49 1.376(7) . ? C48 H48A 0.9500 . ? C49 C50 1.375(7) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? O1 C51 1.465(6) . ? O1 C54 1.482(6) . ? C51 C52 1.486(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.563(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.521(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.41(3) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O2 1.34(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O2 C58 0.93(4) 5_675 ? O2 C57 1.04(3) 5_675 ? O2 C57 1.45(4) . ? C57 C58 1.50(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Y1 N1 105.35(13) . . ? N4 Y1 O1 114.90(13) . . ? N1 Y1 O1 92.38(12) . . ? N4 Y1 N2 122.75(13) . . ? N1 Y1 N2 122.16(12) . . ? O1 Y1 N2 94.39(12) . . ? N4 Y1 C1 107.98(14) . . ? N1 Y1 C1 68.11(14) . . ? O1 Y1 C1 136.33(13) . . ? N2 Y1 C1 67.96(14) . . ? N4 Y1 N3 34.06(12) . . ? N1 Y1 N3 137.87(12) . . ? O1 Y1 N3 97.80(12) . . ? N2 Y1 N3 97.77(12) . . ? C1 Y1 N3 123.22(14) . . ? N4 Y1 P1 113.62(10) . . ? N1 Y1 P1 33.63(9) . . ? O1 Y1 P1 114.61(8) . . ? N2 Y1 P1 93.92(9) . . ? C1 Y1 P1 34.78(11) . . ? N3 Y1 P1 144.52(9) . . ? N4 Y1 P2 120.90(11) . . ? N1 Y1 P2 95.89(9) . . ? O1 Y1 P2 118.57(8) . . ? N2 Y1 P2 33.53(9) . . ? C1 Y1 P2 34.42(11) . . ? N3 Y1 P2 114.11(9) . . ? P1 Y1 P2 63.41(4) . . ? P1 N1 Si1 132.3(2) . . ? P1 N1 Y1 93.62(17) . . ? Si1 N1 Y1 131.32(19) . . ? N1 P1 C1 107.3(2) . . ? N1 P1 C2 109.7(2) . . ? C1 P1 C2 115.3(2) . . ? N1 P1 C8 109.5(2) . . ? C1 P1 C8 111.5(2) . . ? C2 P1 C8 103.5(2) . . ? N1 P1 Y1 52.75(13) . . ? C1 P1 Y1 55.13(16) . . ? C2 P1 Y1 123.20(15) . . ? C8 P1 Y1 132.97(17) . . ? P2 C1 P1 135.5(3) . . ? P2 C1 Y1 91.0(2) . . ? P1 C1 Y1 90.1(2) . . ? N2 P2 C1 108.3(2) . . ? N2 P2 C14 106.6(2) . . ? C1 P2 C14 111.1(2) . . ? N2 P2 C20 111.5(2) . . ? C1 P2 C20 115.0(2) . . ? C14 P2 C20 103.9(2) . . ? N2 P2 Y1 53.80(13) . . ? C1 P2 Y1 54.54(16) . . ? C14 P2 Y1 123.46(16) . . ? C20 P2 Y1 132.44(16) . . ? P2 N2 Si2 131.3(2) . . ? P2 N2 Y1 92.66(16) . . ? Si2 N2 Y1 134.3(2) . . ? C3 C2 C7 118.3(5) . . ? C3 C2 P1 121.0(4) . . ? C7 C2 P1 120.6(4) . . ? C2 C3 C4 121.3(5) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 120.6(5) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C2 C7 C6 119.7(5) . . ? C2 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C9 C8 C13 119.2(5) . . ? C9 C8 P1 118.9(4) . . ? C13 C8 P1 121.8(4) . . ? C8 C9 C10 120.2(6) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.2(6) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C12 C13 C8 119.5(6) . . ? C12 C13 H13A 120.2 . . ? C8 C13 H13A 120.2 . . ? C15 C14 C19 117.7(5) . . ? C15 C14 P2 119.6(4) . . ? C19 C14 P2 122.3(4) . . ? C14 C15 C16 121.2(6) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C17 C16 C15 119.6(6) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C18 C17 C16 120.3(5) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C14 121.2(5) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? C21 C20 C25 118.4(5) . . ? C21 C20 P2 121.5(4) . . ? C25 C20 P2 119.9(4) . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C24 C23 C22 121.0(5) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 119.0(6) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C24 C25 C20 121.7(5) . . ? C24 C25 H25A 119.2 . . ? C20 C25 H25A 119.2 . . ? N1 Si1 C27 107.5(2) . . ? N1 Si1 C26 113.3(2) . . ? C27 Si1 C26 107.1(3) . . ? N1 Si1 C28 113.9(2) . . ? C27 Si1 C28 107.7(3) . . ? C26 Si1 C28 107.0(2) . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 Si2 C29 107.2(2) . . ? N2 Si2 C30 114.8(2) . . ? C29 Si2 C30 107.9(2) . . ? N2 Si2 C31 114.4(2) . . ? C29 Si2 C31 106.8(3) . . ? C30 Si2 C31 105.3(2) . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C39 N3 N4 118.8(3) . . ? C39 N3 C32 119.2(4) . . ? N4 N3 C32 114.7(4) . . ? C39 N3 Y1 121.8(3) . . ? N4 N3 Y1 58.40(19) . . ? C32 N3 Y1 109.4(3) . . ? C45 N4 N3 119.6(4) . . ? C45 N4 Y1 152.2(3) . . ? N3 N4 Y1 87.5(2) . . ? N3 C32 C33 116.9(4) . . ? N3 C32 H32A 108.1 . . ? C33 C32 H32A 108.1 . . ? N3 C32 H32B 108.1 . . ? C33 C32 H32B 108.1 . . ? H32A C32 H32B 107.3 . . ? C38 C33 C34 117.8(5) . . ? C38 C33 C32 120.5(5) . . ? C34 C33 C32 121.6(5) . . ? C33 C34 C35 121.3(5) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C36 C35 C34 120.0(6) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.4(6) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 118.1(6) . . ? C38 C37 H37A 121.0 . . ? C36 C37 H37A 121.0 . . ? C33 C38 C37 122.4(5) . . ? C33 C38 H38A 118.8 . . ? C37 C38 H38A 118.8 . . ? C44 C39 C40 117.9(5) . . ? C44 C39 N3 120.7(4) . . ? C40 C39 N3 121.3(4) . . ? C41 C40 C39 120.8(5) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C42 C41 C40 120.7(5) . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C41 C42 C43 119.0(5) . . ? C41 C42 H42A 120.5 . . ? C43 C42 H42A 120.5 . . ? C42 C43 C44 121.4(5) . . ? C42 C43 H43A 119.3 . . ? C44 C43 H43A 119.3 . . ? C43 C44 C39 120.2(5) . . ? C43 C44 H44A 119.9 . . ? C39 C44 H44A 119.9 . . ? C50 C45 N4 127.2(4) . . ? C50 C45 C46 118.0(4) . . ? N4 C45 C46 114.8(4) . . ? C47 C46 C45 120.6(5) . . ? C47 C46 H46A 119.7 . . ? C45 C46 H46A 119.7 . . ? C46 C47 C48 120.7(6) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C49 C48 C47 119.1(5) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C48 121.7(5) . . ? C50 C49 H49A 119.2 . . ? C48 C49 H49A 119.2 . . ? C49 C50 C45 119.9(5) . . ? C49 C50 H50A 120.1 . . ? C45 C50 H50A 120.1 . . ? C51 O1 C54 107.9(4) . . ? C51 O1 Y1 131.2(3) . . ? C54 O1 Y1 120.8(3) . . ? O1 C51 C52 106.8(4) . . ? O1 C51 H51A 110.4 . . ? C52 C51 H51A 110.4 . . ? O1 C51 H51B 110.4 . . ? C52 C51 H51B 110.4 . . ? H51A C51 H51B 108.6 . . ? C51 C52 C53 100.1(5) . . ? C51 C52 H52A 111.8 . . ? C53 C52 H52A 111.8 . . ? C51 C52 H52B 111.8 . . ? C53 C52 H52B 111.8 . . ? H52A C52 H52B 109.5 . . ? C54 C53 C52 101.3(5) . . ? C54 C53 H53A 111.5 . . ? C52 C53 H53A 111.5 . . ? C54 C53 H53B 111.5 . . ? C52 C53 H53B 111.5 . . ? H53A C53 H53B 109.3 . . ? O1 C54 C53 104.6(4) . . ? O1 C54 H54A 110.8 . . ? C53 C54 H54A 110.8 . . ? O1 C54 H54B 110.8 . . ? C53 C54 H54B 110.8 . . ? H54A C54 H54B 108.9 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O2 C56 C55 117.0(19) . . ? O2 C56 H56A 108.1 . . ? C55 C56 H56A 108.1 . . ? O2 C56 H56B 108.1 . . ? C55 C56 H56B 108.1 . . ? H56A C56 H56B 107.3 . . ? C58 O2 C57 99(4) 5_675 5_675 ? C58 O2 C56 41(3) 5_675 . ? C57 O2 C56 139(2) 5_675 . ? C58 O2 C57 72(3) 5_675 . ? C57 O2 C57 47(2) 5_675 . ? C56 O2 C57 109.0(18) . . ? O2 C57 C58 106.5(19) . . ? O2 C57 H57A 110.4 . . ? C58 C57 H57A 110.4 . . ? O2 C57 H57B 110.4 . . ? C58 C57 H57B 110.4 . . ? H57A C57 H57B 108.6 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Y1 N1 P1 -109.73(17) . . . . ? O1 Y1 N1 P1 133.62(16) . . . . ? N2 Y1 N1 P1 36.9(2) . . . . ? C1 Y1 N1 P1 -6.15(16) . . . . ? N3 Y1 N1 P1 -121.99(18) . . . . ? P2 Y1 N1 P1 14.58(15) . . . . ? N4 Y1 N1 Si1 52.9(3) . . . . ? O1 Y1 N1 Si1 -63.8(3) . . . . ? N2 Y1 N1 Si1 -160.5(2) . . . . ? C1 Y1 N1 Si1 156.4(3) . . . . ? N3 Y1 N1 Si1 40.6(4) . . . . ? P1 Y1 N1 Si1 162.6(4) . . . . ? P2 Y1 N1 Si1 177.2(2) . . . . ? Si1 N1 P1 C1 -153.7(3) . . . . ? Y1 N1 P1 C1 8.6(2) . . . . ? Si1 N1 P1 C2 80.4(3) . . . . ? Y1 N1 P1 C2 -117.29(18) . . . . ? Si1 N1 P1 C8 -32.6(4) . . . . ? Y1 N1 P1 C8 129.7(2) . . . . ? Si1 N1 P1 Y1 -162.3(4) . . . . ? N4 Y1 P1 N1 82.2(2) . . . . ? O1 Y1 P1 N1 -52.70(19) . . . . ? N2 Y1 P1 N1 -149.35(19) . . . . ? C1 Y1 P1 N1 170.0(3) . . . . ? N3 Y1 P1 N1 101.4(2) . . . . ? P2 Y1 P1 N1 -163.73(17) . . . . ? N4 Y1 P1 C1 -87.8(2) . . . . ? N1 Y1 P1 C1 -170.0(3) . . . . ? O1 Y1 P1 C1 137.3(2) . . . . ? N2 Y1 P1 C1 40.7(2) . . . . ? N3 Y1 P1 C1 -68.5(2) . . . . ? P2 Y1 P1 C1 26.31(18) . . . . ? N4 Y1 P1 C2 172.7(2) . . . . ? N1 Y1 P1 C2 90.5(3) . . . . ? O1 Y1 P1 C2 37.8(2) . . . . ? N2 Y1 P1 C2 -58.9(2) . . . . ? C1 Y1 P1 C2 -99.6(3) . . . . ? N3 Y1 P1 C2 -168.1(2) . . . . ? P2 Y1 P1 C2 -73.25(19) . . . . ? N4 Y1 P1 C8 0.0(3) . . . . ? N1 Y1 P1 C8 -82.2(3) . . . . ? O1 Y1 P1 C8 -134.9(2) . . . . ? N2 Y1 P1 C8 128.4(2) . . . . ? C1 Y1 P1 C8 87.8(3) . . . . ? N3 Y1 P1 C8 19.2(3) . . . . ? P2 Y1 P1 C8 114.1(2) . . . . ? N1 P1 C1 P2 -99.9(4) . . . . ? C2 P1 C1 P2 22.6(5) . . . . ? C8 P1 C1 P2 140.2(4) . . . . ? Y1 P1 C1 P2 -91.6(4) . . . . ? N1 P1 C1 Y1 -8.4(2) . . . . ? C2 P1 C1 Y1 114.1(2) . . . . ? C8 P1 C1 Y1 -128.22(18) . . . . ? N4 Y1 C1 P2 -118.78(18) . . . . ? N1 Y1 C1 P2 141.5(2) . . . . ? O1 Y1 C1 P2 72.3(3) . . . . ? N2 Y1 C1 P2 0.06(16) . . . . ? N3 Y1 C1 P2 -84.7(2) . . . . ? P1 Y1 C1 P2 135.5(3) . . . . ? N4 Y1 C1 P1 105.74(18) . . . . ? N1 Y1 C1 P1 5.97(15) . . . . ? O1 Y1 C1 P1 -63.2(3) . . . . ? N2 Y1 C1 P1 -135.4(2) . . . . ? N3 Y1 C1 P1 139.78(15) . . . . ? P2 Y1 C1 P1 -135.5(3) . . . . ? P1 C1 P2 N2 91.1(4) . . . . ? Y1 C1 P2 N2 -0.1(2) . . . . ? P1 C1 P2 C14 -152.0(4) . . . . ? Y1 C1 P2 C14 116.77(19) . . . . ? P1 C1 P2 C20 -34.4(5) . . . . ? Y1 C1 P2 C20 -125.6(2) . . . . ? P1 C1 P2 Y1 91.2(4) . . . . ? N4 Y1 P2 N2 -103.8(2) . . . . ? N1 Y1 P2 N2 144.37(19) . . . . ? O1 Y1 P2 N2 48.41(19) . . . . ? C1 Y1 P2 N2 179.9(3) . . . . ? N3 Y1 P2 N2 -65.97(19) . . . . ? P1 Y1 P2 N2 153.34(17) . . . . ? N4 Y1 P2 C1 76.3(2) . . . . ? N1 Y1 P2 C1 -35.5(2) . . . . ? O1 Y1 P2 C1 -131.5(2) . . . . ? N2 Y1 P2 C1 -179.9(3) . . . . ? N3 Y1 P2 C1 114.1(2) . . . . ? P1 Y1 P2 C1 -26.56(19) . . . . ? N4 Y1 P2 C14 -17.1(2) . . . . ? N1 Y1 P2 C14 -129.0(2) . . . . ? O1 Y1 P2 C14 135.1(2) . . . . ? N2 Y1 P2 C14 86.7(3) . . . . ? C1 Y1 P2 C14 -93.4(3) . . . . ? N3 Y1 P2 C14 20.7(2) . . . . ? P1 Y1 P2 C14 -120.0(2) . . . . ? N4 Y1 P2 C20 169.3(2) . . . . ? N1 Y1 P2 C20 57.5(2) . . . . ? O1 Y1 P2 C20 -38.5(2) . . . . ? N2 Y1 P2 C20 -86.9(3) . . . . ? C1 Y1 P2 C20 93.0(3) . . . . ? N3 Y1 P2 C20 -152.9(2) . . . . ? P1 Y1 P2 C20 66.5(2) . . . . ? C1 P2 N2 Si2 166.3(3) . . . . ? C14 P2 N2 Si2 46.6(4) . . . . ? C20 P2 N2 Si2 -66.1(4) . . . . ? Y1 P2 N2 Si2 166.2(4) . . . . ? C1 P2 N2 Y1 0.1(2) . . . . ? C14 P2 N2 Y1 -119.62(19) . . . . ? C20 P2 N2 Y1 127.63(18) . . . . ? N4 Y1 N2 P2 97.73(19) . . . . ? N1 Y1 N2 P2 -43.2(2) . . . . ? O1 Y1 N2 P2 -138.79(16) . . . . ? C1 Y1 N2 P2 -0.06(16) . . . . ? N3 Y1 N2 P2 122.71(16) . . . . ? P1 Y1 N2 P2 -23.71(15) . . . . ? N4 Y1 N2 Si2 -67.8(3) . . . . ? N1 Y1 N2 Si2 151.3(2) . . . . ? O1 Y1 N2 Si2 55.7(3) . . . . ? C1 Y1 N2 Si2 -165.6(3) . . . . ? N3 Y1 N2 Si2 -42.8(3) . . . . ? P1 Y1 N2 Si2 170.8(3) . . . . ? P2 Y1 N2 Si2 -165.5(4) . . . . ? N1 P1 C2 C3 16.5(4) . . . . ? C1 P1 C2 C3 -104.7(4) . . . . ? C8 P1 C2 C3 133.3(4) . . . . ? Y1 P1 C2 C3 -41.2(4) . . . . ? N1 P1 C2 C7 -166.1(4) . . . . ? C1 P1 C2 C7 72.7(4) . . . . ? C8 P1 C2 C7 -49.4(4) . . . . ? Y1 P1 C2 C7 136.1(3) . . . . ? C7 C2 C3 C4 -0.9(7) . . . . ? P1 C2 C3 C4 176.6(4) . . . . ? C2 C3 C4 C5 1.0(8) . . . . ? C3 C4 C5 C6 -0.9(8) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C3 C2 C7 C6 0.6(7) . . . . ? P1 C2 C7 C6 -176.8(4) . . . . ? C5 C6 C7 C2 -0.5(7) . . . . ? N1 P1 C8 C9 -94.7(4) . . . . ? C1 P1 C8 C9 23.9(5) . . . . ? C2 P1 C8 C9 148.4(4) . . . . ? Y1 P1 C8 C9 -37.9(5) . . . . ? N1 P1 C8 C13 80.3(4) . . . . ? C1 P1 C8 C13 -161.1(4) . . . . ? C2 P1 C8 C13 -36.6(5) . . . . ? Y1 P1 C8 C13 137.1(3) . . . . ? C13 C8 C9 C10 0.1(8) . . . . ? P1 C8 C9 C10 175.2(4) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C9 C10 C11 C12 -0.2(10) . . . . ? C10 C11 C12 C13 0.3(9) . . . . ? C11 C12 C13 C8 -0.2(8) . . . . ? C9 C8 C13 C12 0.0(8) . . . . ? P1 C8 C13 C12 -175.0(4) . . . . ? N2 P2 C14 C15 90.5(4) . . . . ? C1 P2 C14 C15 -27.4(5) . . . . ? C20 P2 C14 C15 -151.6(4) . . . . ? Y1 P2 C14 C15 33.3(5) . . . . ? N2 P2 C14 C19 -81.6(4) . . . . ? C1 P2 C14 C19 160.5(4) . . . . ? C20 P2 C14 C19 36.3(5) . . . . ? Y1 P2 C14 C19 -138.8(4) . . . . ? C19 C14 C15 C16 0.8(7) . . . . ? P2 C14 C15 C16 -171.6(4) . . . . ? C14 C15 C16 C17 -0.4(8) . . . . ? C15 C16 C17 C18 0.0(9) . . . . ? C16 C17 C18 C19 0.0(9) . . . . ? C17 C18 C19 C14 0.5(9) . . . . ? C15 C14 C19 C18 -0.9(8) . . . . ? P2 C14 C19 C18 171.3(4) . . . . ? N2 P2 C20 C21 157.8(4) . . . . ? C1 P2 C20 C21 -78.4(5) . . . . ? C14 P2 C20 C21 43.3(5) . . . . ? Y1 P2 C20 C21 -142.3(4) . . . . ? N2 P2 C20 C25 -26.8(4) . . . . ? C1 P2 C20 C25 97.0(4) . . . . ? C14 P2 C20 C25 -141.3(4) . . . . ? Y1 P2 C20 C25 33.2(5) . . . . ? C25 C20 C21 C22 0.4(8) . . . . ? P2 C20 C21 C22 175.9(4) . . . . ? C20 C21 C22 C23 -0.8(8) . . . . ? C21 C22 C23 C24 1.1(9) . . . . ? C22 C23 C24 C25 -0.9(8) . . . . ? C23 C24 C25 C20 0.4(8) . . . . ? C21 C20 C25 C24 -0.2(7) . . . . ? P2 C20 C25 C24 -175.7(4) . . . . ? P1 N1 Si1 C27 -173.1(3) . . . . ? Y1 N1 Si1 C27 30.7(3) . . . . ? P1 N1 Si1 C26 68.8(4) . . . . ? Y1 N1 Si1 C26 -87.4(3) . . . . ? P1 N1 Si1 C28 -53.8(4) . . . . ? Y1 N1 Si1 C28 150.0(3) . . . . ? P2 N2 Si2 C29 173.1(3) . . . . ? Y1 N2 Si2 C29 -26.3(4) . . . . ? P2 N2 Si2 C30 53.3(4) . . . . ? Y1 N2 Si2 C30 -146.1(3) . . . . ? P2 N2 Si2 C31 -68.7(4) . . . . ? Y1 N2 Si2 C31 91.9(3) . . . . ? N4 Y1 N3 C39 -106.5(4) . . . . ? N1 Y1 N3 C39 -85.1(4) . . . . ? O1 Y1 N3 C39 17.3(3) . . . . ? N2 Y1 N3 C39 112.8(3) . . . . ? C1 Y1 N3 C39 -178.5(3) . . . . ? P1 Y1 N3 C39 -139.1(3) . . . . ? P2 Y1 N3 C39 143.4(3) . . . . ? N1 Y1 N3 N4 21.5(3) . . . . ? O1 Y1 N3 N4 123.8(2) . . . . ? N2 Y1 N3 N4 -140.6(2) . . . . ? C1 Y1 N3 N4 -72.0(3) . . . . ? P1 Y1 N3 N4 -32.6(3) . . . . ? P2 Y1 N3 N4 -110.0(2) . . . . ? N4 Y1 N3 C32 107.7(4) . . . . ? N1 Y1 N3 C32 129.1(3) . . . . ? O1 Y1 N3 C32 -128.5(3) . . . . ? N2 Y1 N3 C32 -33.0(3) . . . . ? C1 Y1 N3 C32 35.7(3) . . . . ? P1 Y1 N3 C32 75.1(3) . . . . ? P2 Y1 N3 C32 -2.4(3) . . . . ? C39 N3 N4 C45 -74.7(5) . . . . ? C32 N3 N4 C45 75.3(5) . . . . ? Y1 N3 N4 C45 173.7(4) . . . . ? C39 N3 N4 Y1 111.5(4) . . . . ? C32 N3 N4 Y1 -98.5(3) . . . . ? N1 Y1 N4 C45 26.5(7) . . . . ? O1 Y1 N4 C45 126.5(7) . . . . ? N2 Y1 N4 C45 -119.9(7) . . . . ? C1 Y1 N4 C45 -45.0(7) . . . . ? N3 Y1 N4 C45 -168.3(8) . . . . ? P1 Y1 N4 C45 -8.2(7) . . . . ? P2 Y1 N4 C45 -80.3(7) . . . . ? N1 Y1 N4 N3 -165.3(2) . . . . ? O1 Y1 N4 N3 -65.2(2) . . . . ? N2 Y1 N4 N3 48.3(3) . . . . ? C1 Y1 N4 N3 123.2(2) . . . . ? P1 Y1 N4 N3 160.06(19) . . . . ? P2 Y1 N4 N3 88.0(2) . . . . ? C39 N3 C32 C33 74.9(5) . . . . ? N4 N3 C32 C33 -75.0(5) . . . . ? Y1 N3 C32 C33 -138.3(4) . . . . ? N3 C32 C33 C38 91.0(6) . . . . ? N3 C32 C33 C34 -88.4(6) . . . . ? C38 C33 C34 C35 -2.4(8) . . . . ? C32 C33 C34 C35 177.0(5) . . . . ? C33 C34 C35 C36 0.0(9) . . . . ? C34 C35 C36 C37 2.0(9) . . . . ? C35 C36 C37 C38 -1.5(9) . . . . ? C34 C33 C38 C37 3.0(8) . . . . ? C32 C33 C38 C37 -176.4(5) . . . . ? C36 C37 C38 C33 -1.1(8) . . . . ? N4 N3 C39 C44 -4.9(6) . . . . ? C32 N3 C39 C44 -153.6(4) . . . . ? Y1 N3 C39 C44 63.8(5) . . . . ? N4 N3 C39 C40 179.1(4) . . . . ? C32 N3 C39 C40 30.4(6) . . . . ? Y1 N3 C39 C40 -112.2(4) . . . . ? C44 C39 C40 C41 0.3(7) . . . . ? N3 C39 C40 C41 176.4(4) . . . . ? C39 C40 C41 C42 0.6(8) . . . . ? C40 C41 C42 C43 -1.5(8) . . . . ? C41 C42 C43 C44 1.7(8) . . . . ? C42 C43 C44 C39 -0.9(8) . . . . ? C40 C39 C44 C43 -0.1(7) . . . . ? N3 C39 C44 C43 -176.3(4) . . . . ? N3 N4 C45 C50 21.6(7) . . . . ? Y1 N4 C45 C50 -171.9(5) . . . . ? N3 N4 C45 C46 -159.2(4) . . . . ? Y1 N4 C45 C46 7.3(9) . . . . ? C50 C45 C46 C47 -2.2(8) . . . . ? N4 C45 C46 C47 178.5(5) . . . . ? C45 C46 C47 C48 0.9(9) . . . . ? C46 C47 C48 C49 0.1(10) . . . . ? C47 C48 C49 C50 0.3(9) . . . . ? C48 C49 C50 C45 -1.6(8) . . . . ? N4 C45 C50 C49 -178.3(5) . . . . ? C46 C45 C50 C49 2.5(7) . . . . ? N4 Y1 O1 C51 20.2(4) . . . . ? N1 Y1 O1 C51 128.3(4) . . . . ? N2 Y1 O1 C51 -109.2(4) . . . . ? C1 Y1 O1 C51 -171.5(4) . . . . ? N3 Y1 O1 C51 -10.7(4) . . . . ? P1 Y1 O1 C51 154.5(4) . . . . ? P2 Y1 O1 C51 -133.6(4) . . . . ? N4 Y1 O1 C54 -156.7(4) . . . . ? N1 Y1 O1 C54 -48.5(4) . . . . ? N2 Y1 O1 C54 74.0(4) . . . . ? C1 Y1 O1 C54 11.7(4) . . . . ? N3 Y1 O1 C54 172.4(4) . . . . ? P1 Y1 O1 C54 -22.4(4) . . . . ? P2 Y1 O1 C54 49.5(4) . . . . ? C54 O1 C51 C52 -16.1(6) . . . . ? Y1 O1 C51 C52 166.7(3) . . . . ? O1 C51 C52 C53 36.7(6) . . . . ? C51 C52 C53 C54 -43.1(6) . . . . ? C51 O1 C54 C53 -12.4(6) . . . . ? Y1 O1 C54 C53 165.1(3) . . . . ? C52 C53 C54 O1 34.3(6) . . . . ? C55 C56 O2 C58 -147(7) . . . 5_675 ? C55 C56 O2 C57 -131(3) . . . 5_675 ? C55 C56 O2 C57 -176(2) . . . . ? C58 O2 C57 C58 153(2) 5_675 . . . ? C57 O2 C57 C58 32(3) 5_675 . . . ? C56 O2 C57 C58 173(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.078