# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email nathanh@chem.ubc.ca _publ_contact_author_name 'Nathan Halcovitch' loop_ _publ_author_name N.Halcovitch M.Fryzuk data_mf864 _database_code_depnum_ccdc_archive 'CCDC 837086' #TrackingRef 'CCDC-837086-new.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H65 N2 O P2 Sc Si' _chemical_formula_sum 'C36 H65 N2 O P2 Sc Si' _chemical_formula_weight 676.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5520(8) _cell_length_b 19.4650(15) _cell_length_c 18.3410(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.253(3) _cell_angle_gamma 90.00 _cell_volume 4081.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11862 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9225 _exptl_absorpt_correction_T_max 0.9396 _exptl_absorpt_process_details 'twinabs 2008/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7283 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.16 _reflns_number_total 7283 _reflns_number_gt 6426 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+1.7695P] 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 7283 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.006 _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 Sc1 Sc 0.25706(5) 0.16339(3) 0.26194(3) 0.01581(14) Uani 1 1 d . . . P2 P 0.42169(6) 0.06705(4) 0.30190(4) 0.01708(17) Uani 1 1 d . . . P1 P 0.11605(6) 0.23660(4) 0.33916(4) 0.01788(17) Uani 1 1 d . . . Si1 Si 0.00555(9) 0.09944(5) 0.13079(5) 0.0300(2) Uani 1 1 d . . . O1 O 0.37991(19) 0.22108(10) 0.20421(10) 0.0232(5) Uani 1 1 d . . . C15 C 0.2177(2) 0.01594(14) 0.34516(14) 0.0173(6) Uani 1 1 d . . . C1 C 0.3378(2) 0.29043(14) 0.37728(15) 0.0180(6) Uani 1 1 d . . . C16 C 0.2645(3) -0.04735(15) 0.36935(15) 0.0207(6) Uani 1 1 d . . . H16 H 0.3434 -0.0575 0.3644 0.025 Uiso 1 1 calc R . . C2 C 0.3042(3) 0.34662(14) 0.41664(14) 0.0203(6) Uani 1 1 d . . . H2 H 0.2233 0.3564 0.4150 0.024 Uiso 1 1 calc R . . C17 C 0.1988(3) -0.09591(15) 0.40055(15) 0.0228(6) Uani 1 1 d . . . C20 C 0.1007(3) 0.02960(14) 0.35344(15) 0.0188(6) Uani 1 1 d . . . H20 H 0.0667 0.0722 0.3368 0.023 Uiso 1 1 calc R . . C19 C 0.0347(2) -0.01767(15) 0.38526(14) 0.0206(6) Uani 1 1 d . . . C6 C 0.4584(3) 0.27822(15) 0.38022(16) 0.0227(6) Uani 1 1 d . . . H6 H 0.4839 0.2408 0.3533 0.027 Uiso 1 1 calc R . . C33 C 0.3613(3) 0.29367(15) 0.18610(16) 0.0261(7) Uani 1 1 d . . . H33A H 0.3690 0.3220 0.2314 0.031 Uiso 1 1 calc R . . H33B H 0.2826 0.3011 0.1578 0.031 Uiso 1 1 calc R . . C21 C 0.2500(3) -0.16559(16) 0.4225(2) 0.0330(8) Uani 1 1 d . . . H21A H 0.2484 -0.1943 0.3785 0.050 Uiso 1 1 calc R . . H21B H 0.2038 -0.1875 0.4568 0.050 Uiso 1 1 calc R . . H21C H 0.3310 -0.1601 0.4463 0.050 Uiso 1 1 calc R . . C5 C 0.5404(3) 0.31921(16) 0.42112(17) 0.0275(7) Uani 1 1 d . . . C18 C 0.0837(3) -0.08059(16) 0.40854(15) 0.0226(6) Uani 1 1 d . . . H18 H 0.0381 -0.1134 0.4301 0.027 Uiso 1 1 calc R . . C22 C -0.0905(3) -0.00182(17) 0.39360(18) 0.0302(7) Uani 1 1 d . . . H22A H -0.1391 -0.0425 0.3804 0.045 Uiso 1 1 calc R . . H22B H -0.1187 0.0364 0.3610 0.045 Uiso 1 1 calc R . . H22C H -0.0951 0.0109 0.4448 0.045 Uiso 1 1 calc R . . C4 C 0.5034(3) 0.37418(16) 0.46042(16) 0.0281(7) Uani 1 1 d . . . H4 H 0.5598 0.4022 0.4892 0.034 Uiso 1 1 calc R . . C3 C 0.3856(3) 0.38874(16) 0.45820(16) 0.0268(7) Uani 1 1 d . . . C13 C -0.0881(3) 0.30040(19) 0.2697(2) 0.0390(8) Uani 1 1 d . . . H13A H -0.1301 0.3432 0.2555 0.059 Uiso 1 1 calc R . . H13B H -0.1304 0.2744 0.3033 0.059 Uiso 1 1 calc R . . H13C H -0.0826 0.2729 0.2256 0.059 Uiso 1 1 calc R . . C9 C 0.0941(3) 0.23046(15) 0.43740(15) 0.0215(6) Uani 1 1 d . . . H9 H 0.1139 0.2760 0.4612 0.026 Uiso 1 1 calc R . . C25 C 0.4600(3) 0.08821(17) 0.45430(15) 0.0271(7) Uani 1 1 d . . . H25A H 0.5114 0.0814 0.5011 0.041 Uiso 1 1 calc R . . H25B H 0.3838 0.0670 0.4571 0.041 Uiso 1 1 calc R . . H25C H 0.4495 0.1375 0.4447 0.041 Uiso 1 1 calc R . . C10 C 0.1750(3) 0.17673(16) 0.47772(15) 0.0252(7) Uani 1 1 d . . . H10A H 0.1619 0.1743 0.5293 0.038 Uiso 1 1 calc R . . H10B H 0.2565 0.1895 0.4756 0.038 Uiso 1 1 calc R . . H10C H 0.1587 0.1319 0.4543 0.038 Uiso 1 1 calc R . . C29 C 0.1360(3) 0.15729(16) 0.15497(15) 0.0254(7) Uani 1 1 d . . . H29A H 0.1058 0.2045 0.1455 0.030 Uiso 1 1 calc R . . H29B H 0.1871 0.1481 0.1171 0.030 Uiso 1 1 calc R . . C36 C 0.4557(3) 0.19108(16) 0.15506(17) 0.0307(7) Uani 1 1 d . . . H36A H 0.4205 0.1486 0.1319 0.037 Uiso 1 1 calc R . . H36B H 0.5334 0.1798 0.1827 0.037 Uiso 1 1 calc R . . C34 C 0.4559(4) 0.31143(17) 0.14002(18) 0.0373(9) Uani 1 1 d . . . H34A H 0.5303 0.3232 0.1714 0.045 Uiso 1 1 calc R . . H34B H 0.4320 0.3501 0.1062 0.045 Uiso 1 1 calc R . . C35 C 0.4668(3) 0.24478(16) 0.09769(18) 0.0356(8) Uani 1 1 d . . . H35A H 0.4035 0.2406 0.0554 0.043 Uiso 1 1 calc R . . H35B H 0.5434 0.2418 0.0796 0.043 Uiso 1 1 calc R . . C8 C 0.6689(3) 0.30454(19) 0.4235(2) 0.0420(9) Uani 1 1 d . . . H8A H 0.7017 0.2889 0.4729 0.063 Uiso 1 1 calc R . . H8B H 0.7092 0.3465 0.4116 0.063 Uiso 1 1 calc R . . H8C H 0.6795 0.2687 0.3874 0.063 Uiso 1 1 calc R . . C26 C 0.4591(3) -0.00998(15) 0.24892(16) 0.0261(7) Uani 1 1 d . . . H26 H 0.4753 -0.0493 0.2840 0.031 Uiso 1 1 calc R . . C12 C 0.0353(3) 0.31723(15) 0.30848(16) 0.0243(6) Uani 1 1 d . . . H12 H 0.0282 0.3457 0.3530 0.029 Uiso 1 1 calc R . . C23 C 0.5146(3) 0.05520(16) 0.39231(16) 0.0263(7) Uani 1 1 d . . . H23 H 0.5240 0.0049 0.4024 0.032 Uiso 1 1 calc R . . C11 C -0.0342(3) 0.21498(19) 0.4426(2) 0.0380(8) Uani 1 1 d . . . H11A H -0.0559 0.1708 0.4188 0.057 Uiso 1 1 calc R . . H11B H -0.0836 0.2514 0.4178 0.057 Uiso 1 1 calc R . . H11C H -0.0455 0.2128 0.4945 0.057 Uiso 1 1 calc R . . C28 C 0.3556(3) -0.02871(18) 0.19180(17) 0.0361(8) Uani 1 1 d . . . H28A H 0.3306 0.0118 0.1619 0.054 Uiso 1 1 calc R . . H28B H 0.2909 -0.0447 0.2166 0.054 Uiso 1 1 calc R . . H28C H 0.3784 -0.0653 0.1600 0.054 Uiso 1 1 calc R . . C14 C 0.1002(3) 0.35887(16) 0.25704(17) 0.0294(7) Uani 1 1 d . . . H14A H 0.1096 0.3312 0.2136 0.044 Uiso 1 1 calc R . . H14B H 0.1774 0.3718 0.2828 0.044 Uiso 1 1 calc R . . H14C H 0.0555 0.4004 0.2416 0.044 Uiso 1 1 calc R . . C7 C 0.3447(4) 0.44960(18) 0.49755(19) 0.0390(9) Uani 1 1 d . . . H7A H 0.3204 0.4862 0.4619 0.059 Uiso 1 1 calc R . . H7B H 0.4085 0.4662 0.5343 0.059 Uiso 1 1 calc R . . H7C H 0.2782 0.4362 0.5222 0.059 Uiso 1 1 calc R . . C27 C 0.5687(3) 0.0031(2) 0.21270(18) 0.0395(9) Uani 1 1 d . . . H27A H 0.5899 -0.0390 0.1884 0.059 Uiso 1 1 calc R . . H27B H 0.6335 0.0168 0.2504 0.059 Uiso 1 1 calc R . . H27C H 0.5529 0.0399 0.1761 0.059 Uiso 1 1 calc R . . C30 C 0.0419(4) 0.00691(17) 0.14880(19) 0.0398(9) Uani 1 1 d . . . H30A H 0.1033 -0.0070 0.1201 0.060 Uiso 1 1 calc R . . H30B H -0.0281 -0.0211 0.1344 0.060 Uiso 1 1 calc R . . H30C H 0.0696 0.0003 0.2014 0.060 Uiso 1 1 calc R . . C24 C 0.6361(3) 0.0868(3) 0.3897(2) 0.0531(12) Uani 1 1 d . . . H24A H 0.6286 0.1366 0.3834 0.080 Uiso 1 1 calc R . . H24B H 0.6698 0.0671 0.3483 0.080 Uiso 1 1 calc R . . H24C H 0.6873 0.0767 0.4358 0.080 Uiso 1 1 calc R . . C31 C -0.0544(4) 0.1047(2) 0.0300(2) 0.0519(11) Uani 1 1 d . . . H31A H 0.0074 0.0933 0.0006 0.078 Uiso 1 1 calc R . . H31B H -0.0826 0.1515 0.0181 0.078 Uiso 1 1 calc R . . H31C H -0.1193 0.0722 0.0188 0.078 Uiso 1 1 calc R . . C32 C -0.1197(4) 0.1212(2) 0.1820(2) 0.0541(11) Uani 1 1 d . . . H32A H -0.1788 0.0848 0.1743 0.081 Uiso 1 1 calc R . . H32B H -0.1547 0.1649 0.1637 0.081 Uiso 1 1 calc R . . H32C H -0.0908 0.1253 0.2347 0.081 Uiso 1 1 calc R . . N2 N 0.2804(2) 0.06661(11) 0.31254(12) 0.0175(5) Uani 1 1 d . . . N1 N 0.2595(2) 0.24567(11) 0.33611(11) 0.0167(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0218(3) 0.0136(3) 0.0122(2) 0.0008(2) 0.0030(2) 0.0031(2) P2 0.0199(4) 0.0163(4) 0.0157(3) 0.0012(3) 0.0048(3) 0.0040(3) P1 0.0198(4) 0.0149(3) 0.0192(4) -0.0004(3) 0.0037(3) 0.0024(3) Si1 0.0352(5) 0.0245(5) 0.0276(4) 0.0012(4) -0.0043(4) -0.0051(4) O1 0.0348(12) 0.0179(10) 0.0200(10) 0.0028(8) 0.0141(9) 0.0040(9) C15 0.0227(14) 0.0166(14) 0.0128(12) -0.0011(11) 0.0032(11) 0.0015(12) C1 0.0232(15) 0.0159(14) 0.0152(13) 0.0058(11) 0.0040(11) 0.0003(12) C16 0.0198(14) 0.0225(15) 0.0198(13) 0.0034(12) 0.0030(12) 0.0034(12) C2 0.0262(15) 0.0180(14) 0.0176(13) 0.0024(11) 0.0066(12) -0.0021(12) C17 0.0246(16) 0.0206(15) 0.0222(14) 0.0048(12) 0.0000(12) 0.0018(13) C20 0.0233(15) 0.0139(13) 0.0182(13) -0.0019(11) -0.0004(12) 0.0020(12) C19 0.0208(15) 0.0240(15) 0.0162(13) -0.0041(12) 0.0002(11) 0.0001(13) C6 0.0249(16) 0.0175(15) 0.0252(15) 0.0051(12) 0.0021(12) 0.0002(12) C33 0.0353(18) 0.0187(15) 0.0250(15) 0.0045(12) 0.0065(14) 0.0020(14) C21 0.0278(17) 0.0251(17) 0.047(2) 0.0135(15) 0.0086(15) 0.0035(14) C5 0.0267(16) 0.0256(16) 0.0289(16) 0.0147(13) -0.0009(13) -0.0045(13) C18 0.0248(15) 0.0229(15) 0.0202(14) 0.0027(12) 0.0036(12) -0.0038(12) C22 0.0248(16) 0.0277(17) 0.0392(18) 0.0002(14) 0.0084(14) -0.0010(14) C4 0.0351(18) 0.0259(17) 0.0207(15) 0.0080(13) -0.0051(13) -0.0158(14) C3 0.0422(19) 0.0205(15) 0.0176(14) 0.0020(12) 0.0040(13) -0.0095(14) C13 0.0312(18) 0.040(2) 0.042(2) 0.0050(16) -0.0066(16) 0.0101(16) C9 0.0270(16) 0.0192(14) 0.0209(14) -0.0001(12) 0.0122(12) 0.0013(12) C25 0.0275(16) 0.0357(17) 0.0162(14) -0.0001(13) -0.0033(12) 0.0018(14) C10 0.0312(17) 0.0254(16) 0.0191(14) 0.0009(12) 0.0043(13) -0.0007(13) C29 0.0348(17) 0.0260(16) 0.0112(13) -0.0060(12) -0.0106(12) 0.0084(14) C36 0.0434(19) 0.0238(16) 0.0296(16) -0.0020(13) 0.0211(15) 0.0008(15) C34 0.061(2) 0.0232(16) 0.0335(18) -0.0066(14) 0.0268(18) -0.0107(17) C35 0.059(2) 0.0233(16) 0.0298(17) -0.0051(14) 0.0238(16) -0.0120(16) C8 0.0242(17) 0.0352(19) 0.063(2) 0.0162(18) -0.0054(17) -0.0057(15) C26 0.0381(18) 0.0202(15) 0.0225(15) 0.0014(12) 0.0131(14) 0.0086(13) C12 0.0248(15) 0.0209(15) 0.0274(15) 0.0012(12) 0.0048(13) 0.0088(13) C23 0.0278(16) 0.0259(16) 0.0227(14) -0.0013(12) -0.0052(13) 0.0113(14) C11 0.0299(18) 0.039(2) 0.049(2) 0.0136(17) 0.0186(16) 0.0056(16) C28 0.049(2) 0.0356(19) 0.0257(16) -0.0147(14) 0.0112(16) -0.0032(17) C14 0.0386(18) 0.0243(16) 0.0255(16) 0.0062(13) 0.0050(14) 0.0097(14) C7 0.056(2) 0.0271(17) 0.0339(18) -0.0091(15) 0.0071(17) -0.0140(17) C27 0.042(2) 0.048(2) 0.0314(18) -0.0131(16) 0.0173(16) 0.0086(18) C30 0.058(2) 0.0233(17) 0.0354(18) 0.0041(14) -0.0027(17) -0.0074(17) C24 0.0208(17) 0.094(3) 0.043(2) -0.024(2) -0.0014(16) 0.011(2) C31 0.062(3) 0.047(2) 0.039(2) 0.0092(18) -0.0210(19) -0.018(2) C32 0.040(2) 0.049(2) 0.075(3) -0.014(2) 0.013(2) -0.0079(19) N2 0.0207(12) 0.0163(12) 0.0159(11) 0.0025(9) 0.0039(10) 0.0036(10) N1 0.0207(12) 0.0152(11) 0.0147(11) -0.0005(9) 0.0042(10) 0.0034(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sc1 N1 2.099(2) . ? Sc1 N2 2.100(2) . ? Sc1 O1 2.197(2) . ? Sc1 C29 2.243(3) . ? Sc1 P2 2.6965(9) . ? Sc1 P1 2.7115(9) . ? P2 N2 1.672(2) . ? P2 C23 1.856(3) . ? P2 C26 1.871(3) . ? P1 N1 1.676(2) . ? P1 C9 1.859(3) . ? P1 C12 1.871(3) . ? Si1 C30 1.868(3) . ? Si1 C31 1.882(3) . ? Si1 C29 1.883(3) . ? Si1 C32 1.883(4) . ? O1 C33 1.460(3) . ? O1 C36 1.465(4) . ? C15 C16 1.392(4) . ? C15 C20 1.407(4) . ? C15 N2 1.407(4) . ? C1 C2 1.396(4) . ? C1 N1 1.396(4) . ? C1 C6 1.408(4) . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C2 C3 1.390(4) . ? C2 H2 0.9500 . ? C17 C18 1.391(4) . ? C17 C21 1.511(4) . ? C20 C19 1.377(4) . ? C20 H20 0.9500 . ? C19 C18 1.390(4) . ? C19 C22 1.508(4) . ? C6 C5 1.375(4) . ? C6 H6 0.9500 . ? C33 C34 1.515(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C5 C4 1.391(5) . ? C5 C8 1.507(5) . ? C18 H18 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C4 C3 1.384(5) . ? C4 H4 0.9500 . ? C3 C7 1.499(5) . ? C13 C12 1.535(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 C10 1.522(4) . ? C9 C11 1.529(4) . ? C9 H9 1.0000 . ? C25 C23 1.520(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C36 C35 1.502(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C34 C35 1.526(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C26 C28 1.517(5) . ? C26 C27 1.534(4) . ? C26 H26 1.0000 . ? C12 C14 1.521(4) . ? C12 H12 1.0000 . ? C23 C24 1.540(5) . ? C23 H23 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 N1 Sc1 N2 114.15(9) . . ? N1 Sc1 O1 88.44(8) . . ? N2 Sc1 O1 128.36(9) . . ? N1 Sc1 C29 123.79(10) . . ? N2 Sc1 C29 111.30(10) . . ? O1 Sc1 C29 88.29(10) . . ? N1 Sc1 P2 114.27(6) . . ? N2 Sc1 P2 38.31(7) . . ? O1 Sc1 P2 90.42(6) . . ? C29 Sc1 P2 121.85(8) . . ? N1 Sc1 P1 38.17(7) . . ? N2 Sc1 P1 106.81(7) . . ? O1 Sc1 P1 117.46(6) . . ? C29 Sc1 P1 97.99(8) . . ? P2 Sc1 P1 132.58(3) . . ? N2 P2 C23 110.13(13) . . ? N2 P2 C26 111.02(13) . . ? C23 P2 C26 102.57(14) . . ? N2 P2 Sc1 51.15(8) . . ? C23 P2 Sc1 128.61(10) . . ? C26 P2 Sc1 128.51(10) . . ? N1 P1 C9 108.19(12) . . ? N1 P1 C12 110.76(13) . . ? C9 P1 C12 102.36(13) . . ? N1 P1 Sc1 50.70(8) . . ? C9 P1 Sc1 130.40(10) . . ? C12 P1 Sc1 126.49(10) . . ? C30 Si1 C31 105.57(18) . . ? C30 Si1 C29 112.52(16) . . ? C31 Si1 C29 111.60(16) . . ? C30 Si1 C32 107.4(2) . . ? C31 Si1 C32 106.1(2) . . ? C29 Si1 C32 113.21(16) . . ? C33 O1 C36 109.1(2) . . ? C33 O1 Sc1 121.31(18) . . ? C36 O1 Sc1 125.26(17) . . ? C16 C15 C20 117.9(3) . . ? C16 C15 N2 123.8(3) . . ? C20 C15 N2 118.3(2) . . ? C2 C1 N1 124.2(3) . . ? C2 C1 C6 117.4(3) . . ? N1 C1 C6 118.4(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C3 C2 C1 121.9(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 C21 120.3(3) . . ? C18 C17 C21 120.6(3) . . ? C19 C20 C15 121.2(3) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C20 C19 C18 119.5(3) . . ? C20 C19 C22 120.3(3) . . ? C18 C19 C22 120.2(3) . . ? C5 C6 C1 121.5(3) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O1 C33 C34 104.7(3) . . ? O1 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O1 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 C8 120.3(3) . . ? C4 C5 C8 120.4(3) . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 C7 121.6(3) . . ? C2 C3 C7 119.6(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C9 C11 111.6(3) . . ? C10 C9 P1 110.82(19) . . ? C11 C9 P1 109.9(2) . . ? C10 C9 H9 108.1 . . ? C11 C9 H9 108.1 . . ? P1 C9 H9 108.1 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C29 Sc1 127.97(16) . . ? Si1 C29 H29A 105.3 . . ? Sc1 C29 H29A 105.3 . . ? Si1 C29 H29B 105.3 . . ? Sc1 C29 H29B 105.3 . . ? H29A C29 H29B 106.0 . . ? O1 C36 C35 105.8(3) . . ? O1 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? O1 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? C33 C34 C35 102.0(3) . . ? C33 C34 H34A 111.4 . . ? C35 C34 H34A 111.4 . . ? C33 C34 H34B 111.4 . . ? C35 C34 H34B 111.4 . . ? H34A C34 H34B 109.2 . . ? C36 C35 C34 102.3(2) . . ? C36 C35 H35A 111.3 . . ? C34 C35 H35A 111.3 . . ? C36 C35 H35B 111.3 . . ? C34 C35 H35B 111.3 . . ? H35A C35 H35B 109.2 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C28 C26 C27 111.0(3) . . ? C28 C26 P2 109.5(2) . . ? C27 C26 P2 111.0(2) . . ? C28 C26 H26 108.4 . . ? C27 C26 H26 108.4 . . ? P2 C26 H26 108.4 . . ? C14 C12 C13 109.5(3) . . ? C14 C12 P1 111.4(2) . . ? C13 C12 P1 110.5(2) . . ? C14 C12 H12 108.4 . . ? C13 C12 H12 108.4 . . ? P1 C12 H12 108.4 . . ? C25 C23 C24 109.4(3) . . ? C25 C23 P2 111.5(2) . . ? C24 C23 P2 109.6(2) . . ? C25 C23 H23 108.7 . . ? C24 C23 H23 108.7 . . ? P2 C23 H23 108.7 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C15 N2 P2 128.60(19) . . ? C15 N2 Sc1 140.85(19) . . ? P2 N2 Sc1 90.54(10) . . ? C1 N1 P1 127.88(19) . . ? C1 N1 Sc1 140.73(19) . . ? P1 N1 Sc1 91.13(10) . . ? 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 N1 Sc1 P2 N2 98.81(12) . . . . ? O1 Sc1 P2 N2 -172.71(11) . . . . ? C29 Sc1 P2 N2 -84.47(14) . . . . ? P1 Sc1 P2 N2 58.01(11) . . . . ? N1 Sc1 P2 C23 13.27(16) . . . . ? N2 Sc1 P2 C23 -85.54(17) . . . . ? O1 Sc1 P2 C23 101.75(15) . . . . ? C29 Sc1 P2 C23 -170.00(17) . . . . ? P1 Sc1 P2 C23 -27.53(15) . . . . ? N1 Sc1 P2 C26 -174.18(14) . . . . ? N2 Sc1 P2 C26 87.01(16) . . . . ? O1 Sc1 P2 C26 -85.71(14) . . . . ? C29 Sc1 P2 C26 2.54(17) . . . . ? P1 Sc1 P2 C26 145.02(13) . . . . ? N2 Sc1 P1 N1 107.89(12) . . . . ? O1 Sc1 P1 N1 -44.69(12) . . . . ? C29 Sc1 P1 N1 -136.92(13) . . . . ? P2 Sc1 P1 N1 74.58(10) . . . . ? N1 Sc1 P1 C9 -80.40(16) . . . . ? N2 Sc1 P1 C9 27.49(15) . . . . ? O1 Sc1 P1 C9 -125.08(14) . . . . ? C29 Sc1 P1 C9 142.68(16) . . . . ? P2 Sc1 P1 C9 -5.82(14) . . . . ? N1 Sc1 P1 C12 87.95(16) . . . . ? N2 Sc1 P1 C12 -164.16(14) . . . . ? O1 Sc1 P1 C12 43.26(14) . . . . ? C29 Sc1 P1 C12 -48.97(15) . . . . ? P2 Sc1 P1 C12 162.53(13) . . . . ? N1 Sc1 O1 C33 -46.4(2) . . . . ? N2 Sc1 O1 C33 -166.44(19) . . . . ? C29 Sc1 O1 C33 77.5(2) . . . . ? P2 Sc1 O1 C33 -160.68(19) . . . . ? P1 Sc1 O1 C33 -20.6(2) . . . . ? N1 Sc1 O1 C36 159.5(2) . . . . ? N2 Sc1 O1 C36 39.5(3) . . . . ? C29 Sc1 O1 C36 -76.6(2) . . . . ? P2 Sc1 O1 C36 45.3(2) . . . . ? P1 Sc1 O1 C36 -174.7(2) . . . . ? C20 C15 C16 C17 0.2(4) . . . . ? N2 C15 C16 C17 -179.4(3) . . . . ? N1 C1 C2 C3 178.5(2) . . . . ? C6 C1 C2 C3 -0.9(4) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C15 C16 C17 C21 176.7(3) . . . . ? C16 C15 C20 C19 0.8(4) . . . . ? N2 C15 C20 C19 -179.7(2) . . . . ? C15 C20 C19 C18 -1.1(4) . . . . ? C15 C20 C19 C22 179.9(3) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? N1 C1 C6 C5 -178.4(2) . . . . ? C36 O1 C33 C34 -16.2(3) . . . . ? Sc1 O1 C33 C34 -173.94(19) . . . . ? C1 C6 C5 C4 -0.2(4) . . . . ? C1 C6 C5 C8 179.7(3) . . . . ? C20 C19 C18 C17 0.5(4) . . . . ? C22 C19 C18 C17 179.5(3) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C21 C17 C18 C19 -177.0(3) . . . . ? C6 C5 C4 C3 -0.8(4) . . . . ? C8 C5 C4 C3 179.3(3) . . . . ? C5 C4 C3 C2 1.0(4) . . . . ? C5 C4 C3 C7 -177.3(3) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C7 178.2(3) . . . . ? N1 P1 C9 C10 -50.6(2) . . . . ? C12 P1 C9 C10 -167.6(2) . . . . ? Sc1 P1 C9 C10 2.8(3) . . . . ? N1 P1 C9 C11 -174.4(2) . . . . ? C12 P1 C9 C11 68.6(2) . . . . ? Sc1 P1 C9 C11 -121.0(2) . . . . ? C30 Si1 C29 Sc1 -53.3(2) . . . . ? C31 Si1 C29 Sc1 -171.8(2) . . . . ? C32 Si1 C29 Sc1 68.7(3) . . . . ? N1 Sc1 C29 Si1 -108.04(19) . . . . ? N2 Sc1 C29 Si1 34.1(2) . . . . ? O1 Sc1 C29 Si1 164.98(19) . . . . ? P2 Sc1 C29 Si1 75.6(2) . . . . ? P1 Sc1 C29 Si1 -77.52(19) . . . . ? C33 O1 C36 C35 -9.3(3) . . . . ? Sc1 O1 C36 C35 147.4(2) . . . . ? O1 C33 C34 C35 34.5(3) . . . . ? O1 C36 C35 C34 30.5(4) . . . . ? C33 C34 C35 C36 -39.7(4) . . . . ? N2 P2 C26 C28 34.4(2) . . . . ? C23 P2 C26 C28 152.0(2) . . . . ? Sc1 P2 C26 C28 -22.1(3) . . . . ? N2 P2 C26 C27 157.3(2) . . . . ? C23 P2 C26 C27 -85.1(2) . . . . ? Sc1 P2 C26 C27 100.9(2) . . . . ? N1 P1 C12 C14 25.7(3) . . . . ? C9 P1 C12 C14 140.9(2) . . . . ? Sc1 P1 C12 C14 -30.1(3) . . . . ? N1 P1 C12 C13 147.7(2) . . . . ? C9 P1 C12 C13 -97.1(2) . . . . ? Sc1 P1 C12 C13 91.9(2) . . . . ? N2 P2 C23 C25 -33.4(3) . . . . ? C26 P2 C23 C25 -151.7(2) . . . . ? Sc1 P2 C23 C25 22.3(3) . . . . ? N2 P2 C23 C24 -154.8(2) . . . . ? C26 P2 C23 C24 87.0(3) . . . . ? Sc1 P2 C23 C24 -99.0(2) . . . . ? C16 C15 N2 P2 -5.8(4) . . . . ? C20 C15 N2 P2 174.7(2) . . . . ? C16 C15 N2 Sc1 175.0(2) . . . . ? C20 C15 N2 Sc1 -4.5(4) . . . . ? C23 P2 N2 C15 -55.5(3) . . . . ? C26 P2 N2 C15 57.4(3) . . . . ? Sc1 P2 N2 C15 -179.5(3) . . . . ? C23 P2 N2 Sc1 123.94(12) . . . . ? C26 P2 N2 Sc1 -123.16(11) . . . . ? N1 Sc1 N2 C15 80.2(3) . . . . ? O1 Sc1 N2 C15 -171.3(2) . . . . ? C29 Sc1 N2 C15 -65.8(3) . . . . ? P2 Sc1 N2 C15 179.4(3) . . . . ? P1 Sc1 N2 C15 40.1(3) . . . . ? N1 Sc1 N2 P2 -99.16(11) . . . . ? O1 Sc1 N2 P2 9.31(14) . . . . ? C29 Sc1 N2 P2 114.84(12) . . . . ? P1 Sc1 N2 P2 -139.28(7) . . . . ? C2 C1 N1 P1 -15.3(4) . . . . ? C6 C1 N1 P1 164.1(2) . . . . ? C2 C1 N1 Sc1 172.4(2) . . . . ? C6 C1 N1 Sc1 -8.2(4) . . . . ? C9 P1 N1 C1 -47.3(3) . . . . ? C12 P1 N1 C1 64.1(3) . . . . ? Sc1 P1 N1 C1 -175.1(3) . . . . ? C9 P1 N1 Sc1 127.78(11) . . . . ? C12 P1 N1 Sc1 -120.78(12) . . . . ? N2 Sc1 N1 C1 87.2(3) . . . . ? O1 Sc1 N1 C1 -44.7(3) . . . . ? C29 Sc1 N1 C1 -131.6(3) . . . . ? P2 Sc1 N1 C1 45.1(3) . . . . ? P1 Sc1 N1 C1 173.9(3) . . . . ? N2 Sc1 N1 P1 -86.70(11) . . . . ? O1 Sc1 N1 P1 141.38(10) . . . . ? C29 Sc1 N1 P1 54.48(15) . . . . ? P2 Sc1 N1 P1 -128.87(7) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.628 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.062 # Attachment 'CCDC-837087-new.txt' data_mo_mf848_0m _database_code_depnum_ccdc_archive 'CCDC 837087' #TrackingRef 'CCDC-837087-new.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H77 N3 O P3 Y' _chemical_formula_sum 'C46 H77 N3 O P3 Y' _chemical_formula_weight 869.93 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' 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 17.0260(9) _cell_length_b 13.4302(6) _cell_length_c 23.0701(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.7330(10) _cell_angle_gamma 90.00 _cell_volume 5101.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9355 _cell_measurement_theta_min 2.453 _cell_measurement_theta_max 25.058 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'SADABS 2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35458 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.06 _reflns_number_total 9023 _reflns_number_gt 7153 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 279 64 ' ' 2 0.500 0.500 0.500 279 66 ' ' _platon_squeeze_details ; Squeeze removed 130 electrons from the unit cell, this agrees well with three pentane or ether molecules which would account for 126 electrons. ; _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^)+(0.0509P)^2^+1.0221P] 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 9023 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.92633(14) 0.49706(17) 0.65751(10) 0.0165(5) Uani 1 1 d . . . C2 C 0.93429(15) 0.59945(17) 0.66882(11) 0.0225(6) Uani 1 1 d . . . H2 H 0.9718 0.6222 0.7042 0.027 Uiso 1 1 calc R . . C3 C 0.88840(15) 0.66875(18) 0.62941(12) 0.0262(6) Uani 1 1 d . . . C4 C 0.83280(15) 0.63556(18) 0.57827(11) 0.0242(6) Uani 1 1 d . . . H4 H 0.8003 0.6824 0.5519 0.029 Uiso 1 1 calc R . . C5 C 0.82398(15) 0.53469(19) 0.56505(11) 0.0219(5) Uani 1 1 d . . . C6 C 0.87120(15) 0.46692(17) 0.60470(10) 0.0194(5) Uani 1 1 d . . . H6 H 0.8657 0.3979 0.5955 0.023 Uiso 1 1 calc R . . C7 C 0.9006(2) 0.7787(2) 0.64292(17) 0.0545(10) Uani 1 1 d . . . H7A H 0.9377 0.8062 0.6208 0.082 Uiso 1 1 calc R . . H7B H 0.9238 0.7881 0.6860 0.082 Uiso 1 1 calc R . . H7C H 0.8482 0.8131 0.6307 0.082 Uiso 1 1 calc R . . C8 C 0.76312(17) 0.4984(2) 0.50959(12) 0.0344(7) Uani 1 1 d . . . H8A H 0.7760 0.4297 0.5011 0.052 Uiso 1 1 calc R . . H8B H 0.7654 0.5410 0.4755 0.052 Uiso 1 1 calc R . . H8C H 0.7085 0.5010 0.5161 0.052 Uiso 1 1 calc R . . C9 C 1.11427(15) 0.52744(17) 0.76501(11) 0.0199(5) Uani 1 1 d . . . H9 H 1.0939 0.5957 0.7706 0.024 Uiso 1 1 calc R . . C10 C 1.18849(16) 0.50577(19) 0.81688(12) 0.0286(6) Uani 1 1 d . . . H10A H 1.2085 0.4385 0.8124 0.043 Uiso 1 1 calc R . . H10B H 1.1732 0.5105 0.8550 0.043 Uiso 1 1 calc R . . H10C H 1.2313 0.5544 0.8164 0.043 Uiso 1 1 calc R . . C11 C 1.13842(15) 0.52508(18) 0.70585(11) 0.0229(6) Uani 1 1 d . . . H11A H 1.1828 0.5724 0.7075 0.034 Uiso 1 1 calc R . . H11B H 1.0916 0.5435 0.6731 0.034 Uiso 1 1 calc R . . H11C H 1.1564 0.4579 0.6989 0.034 Uiso 1 1 calc R . . C12 C 0.97441(16) 0.49883(19) 0.81326(11) 0.0258(6) Uani 1 1 d . . . H12 H 0.9691 0.5710 0.8022 0.031 Uiso 1 1 calc R . . C13 C 1.0188(2) 0.4916(3) 0.87901(15) 0.0697(12) Uani 1 1 d . . . H13A H 0.9857 0.5220 0.9033 0.105 Uiso 1 1 calc R . . H13B H 1.0708 0.5267 0.8860 0.105 Uiso 1 1 calc R . . H13C H 1.0286 0.4214 0.8902 0.105 Uiso 1 1 calc R . . C14 C 0.88978(19) 0.4556(3) 0.80200(15) 0.0535(10) Uani 1 1 d . . . H14A H 0.8934 0.3831 0.8073 0.080 Uiso 1 1 calc R . . H14B H 0.8591 0.4712 0.7610 0.080 Uiso 1 1 calc R . . H14C H 0.8621 0.4843 0.8304 0.080 Uiso 1 1 calc R . . C15 C 1.18968(14) 0.25653(15) 0.66858(10) 0.0152(5) Uani 1 1 d . . . C16 C 1.23192(14) 0.26985(16) 0.72901(10) 0.0169(5) Uani 1 1 d . . . H16 H 1.2024 0.2681 0.7589 0.020 Uiso 1 1 calc R . . C17 C 1.31543(15) 0.28549(17) 0.74645(11) 0.0190(5) Uani 1 1 d . . . C18 C 1.35838(15) 0.28904(17) 0.70242(11) 0.0217(5) Uani 1 1 d . . . H18 H 1.4153 0.3002 0.7137 0.026 Uiso 1 1 calc R . . C19 C 1.31910(15) 0.27648(17) 0.64251(11) 0.0198(5) Uani 1 1 d . . . C20 C 1.23558(14) 0.26062(16) 0.62598(11) 0.0176(5) Uani 1 1 d . . . H20 H 1.2089 0.2523 0.5848 0.021 Uiso 1 1 calc R . . C21 C 1.35907(16) 0.2979(2) 0.81151(11) 0.0277(6) Uani 1 1 d . . . H21A H 1.3198 0.2942 0.8360 0.042 Uiso 1 1 calc R . . H21B H 1.3864 0.3627 0.8174 0.042 Uiso 1 1 calc R . . H21C H 1.3994 0.2448 0.8235 0.042 Uiso 1 1 calc R . . C22 C 1.36674(17) 0.2789(2) 0.59530(13) 0.0317(6) Uani 1 1 d . . . H22A H 1.4214 0.2523 0.6122 0.047 Uiso 1 1 calc R . . H22B H 1.3707 0.3478 0.5822 0.047 Uiso 1 1 calc R . . H22C H 1.3389 0.2383 0.5609 0.047 Uiso 1 1 calc R . . C23 C 1.04480(15) 0.10232(17) 0.55749(10) 0.0198(5) Uani 1 1 d . . . H23 H 0.9962 0.0952 0.5227 0.024 Uiso 1 1 calc R . . C24 C 1.03546(18) 0.02395(18) 0.60339(11) 0.0288(6) Uani 1 1 d . . . H24A H 1.0332 -0.0425 0.5854 0.043 Uiso 1 1 calc R . . H24B H 0.9852 0.0364 0.6156 0.043 Uiso 1 1 calc R . . H24C H 1.0819 0.0277 0.6386 0.043 Uiso 1 1 calc R . . C25 C 1.11874(17) 0.08044(19) 0.53351(13) 0.0310(6) Uani 1 1 d . . . H25A H 1.1678 0.0806 0.5668 0.046 Uiso 1 1 calc R . . H25B H 1.1235 0.1317 0.5043 0.046 Uiso 1 1 calc R . . H25C H 1.1124 0.0150 0.5140 0.046 Uiso 1 1 calc R . . C26 C 1.05247(15) 0.31292(17) 0.53012(10) 0.0193(5) Uani 1 1 d . . . H26 H 1.1003 0.2897 0.5161 0.023 Uiso 1 1 calc R . . C27 C 1.06920(15) 0.41816(17) 0.55517(11) 0.0219(5) Uani 1 1 d . . . H27A H 1.0741 0.4636 0.5230 0.033 Uiso 1 1 calc R . . H27B H 1.1199 0.4187 0.5869 0.033 Uiso 1 1 calc R . . H27C H 1.0244 0.4398 0.5717 0.033 Uiso 1 1 calc R . . C28 C 0.97671(16) 0.31033(19) 0.47697(11) 0.0264(6) Uani 1 1 d . . . H28A H 0.9297 0.3348 0.4900 0.040 Uiso 1 1 calc R . . H28B H 0.9666 0.2418 0.4624 0.040 Uiso 1 1 calc R . . H28C H 0.9856 0.3527 0.4446 0.040 Uiso 1 1 calc R . . C29 C 0.82945(14) 0.11665(17) 0.61727(10) 0.0187(5) Uani 1 1 d . . . C30 C 0.81975(15) 0.16271(18) 0.56120(11) 0.0235(6) Uani 1 1 d . . . H30 H 0.8484 0.2226 0.5587 0.028 Uiso 1 1 calc R . . C31 C 0.76965(16) 0.12334(19) 0.50955(11) 0.0271(6) Uani 1 1 d . . . C32 C 0.72804(15) 0.03558(19) 0.51273(11) 0.0254(6) Uani 1 1 d . . . H32 H 0.6933 0.0085 0.4774 0.030 Uiso 1 1 calc R . . C33 C 0.73665(14) -0.01323(17) 0.56718(11) 0.0214(5) Uani 1 1 d . . . C34 C 0.78732(14) 0.02779(17) 0.61887(11) 0.0186(5) Uani 1 1 d . . . H34 H 0.7933 -0.0055 0.6561 0.022 Uiso 1 1 calc R . . C35 C 0.7620(2) 0.1747(2) 0.44993(12) 0.0433(8) Uani 1 1 d . . . H35A H 0.7770 0.2450 0.4568 0.065 Uiso 1 1 calc R . . H35B H 0.7058 0.1698 0.4257 0.065 Uiso 1 1 calc R . . H35C H 0.7983 0.1426 0.4287 0.065 Uiso 1 1 calc R . . C36 C 0.69247(17) -0.11047(19) 0.56914(13) 0.0312(6) Uani 1 1 d . . . H36A H 0.6338 -0.0993 0.5557 0.047 Uiso 1 1 calc R . . H36B H 0.7062 -0.1361 0.6103 0.047 Uiso 1 1 calc R . . H36C H 0.7088 -0.1590 0.5427 0.047 Uiso 1 1 calc R . . C37 C 0.84415(17) 0.0649(2) 0.77300(12) 0.0313(7) Uani 1 1 d . A . H37 H 0.7913 0.0332 0.7524 0.038 Uiso 1 1 calc R . . C38 C 0.91294(18) -0.0070(2) 0.77186(13) 0.0390(8) Uani 1 1 d . . . H38A H 0.9649 0.0231 0.7926 0.058 Uiso 1 1 calc R . . H38B H 0.9130 -0.0213 0.7302 0.058 Uiso 1 1 calc R . . H38C H 0.9051 -0.0691 0.7921 0.058 Uiso 1 1 calc R . . C39 C 0.8431(3) 0.0902(3) 0.83758(14) 0.0724(13) Uani 1 1 d . . . H39A H 0.8414 0.0286 0.8600 0.109 Uiso 1 1 calc R . . H39B H 0.7949 0.1305 0.8373 0.109 Uiso 1 1 calc R . . H39C H 0.8921 0.1279 0.8567 0.109 Uiso 1 1 calc R . . C43 C 1.07718(17) 0.18426(19) 0.84070(10) 0.0263(6) Uani 1 1 d . . . H43A H 1.0217 0.1924 0.8462 0.032 Uiso 1 1 calc R . . H43B H 1.1082 0.2463 0.8535 0.032 Uiso 1 1 calc R . . C44 C 1.11937(17) 0.0961(2) 0.87639(12) 0.0332(7) Uani 1 1 d . . . H44A H 1.1486 0.1159 0.9176 0.040 Uiso 1 1 calc R . . H44B H 1.0803 0.0424 0.8785 0.040 Uiso 1 1 calc R . . C45 C 1.17763(17) 0.0643(2) 0.84042(12) 0.0323(7) Uani 1 1 d . . . H45A H 1.1948 -0.0057 0.8489 0.039 Uiso 1 1 calc R . . H45B H 1.2263 0.1076 0.8487 0.039 Uiso 1 1 calc R . . C46 C 1.12679(15) 0.07678(18) 0.77593(11) 0.0230(6) Uani 1 1 d . . . H46A H 1.1619 0.0905 0.7486 0.028 Uiso 1 1 calc R . . H46B H 1.0944 0.0162 0.7620 0.028 Uiso 1 1 calc R . . N1 N 0.97071(11) 0.42308(14) 0.69502(8) 0.0153(4) Uani 1 1 d . . . N2 N 1.10569(12) 0.24290(13) 0.65526(8) 0.0146(4) Uani 1 1 d . . . N3 N 0.88091(12) 0.16209(14) 0.66835(8) 0.0178(4) Uani 1 1 d . A . O1 O 1.07404(10) 0.16155(11) 0.77842(7) 0.0184(4) Uani 1 1 d . . . P1 P 1.03155(4) 0.43639(4) 0.76428(3) 0.01663(14) Uani 1 1 d . . . P2 P 1.03758(4) 0.22775(4) 0.58937(3) 0.01481(14) Uani 1 1 d . . . P3 P 0.85619(4) 0.18262(5) 0.73326(3) 0.01917(15) Uani 1 1 d . . . Y1 Y 0.995771(13) 0.256684(15) 0.696843(9) 0.01273(7) Uani 1 1 d . A . C42A C 0.7097(4) 0.2373(4) 0.7597(3) 0.0405(17) Uani 0.545(6) 1 d P A 1 H42A H 0.7420 0.2872 0.7864 0.061 Uiso 0.545(6) 1 calc PR A 1 H42B H 0.7075 0.1759 0.7823 0.061 Uiso 0.545(6) 1 calc PR A 1 H42C H 0.6545 0.2626 0.7435 0.061 Uiso 0.545(6) 1 calc PR A 1 C41A C 0.7393(8) 0.3051(7) 0.6662(6) 0.0237(17) Uani 0.545(6) 1 d P A 1 H41A H 0.6821 0.3252 0.6543 0.036 Uiso 0.545(6) 1 calc PR A 1 H41B H 0.7573 0.2871 0.6305 0.036 Uiso 0.545(6) 1 calc PR A 1 H41C H 0.7723 0.3604 0.6869 0.036 Uiso 0.545(6) 1 calc PR A 1 C40A C 0.7488(5) 0.2154(5) 0.7081(3) 0.0200(16) Uani 0.545(6) 1 d P A 1 H40A H 0.7194 0.1579 0.6848 0.024 Uiso 0.545(6) 1 calc PR A 1 C42B C 0.6791(3) 0.1900(4) 0.7033(3) 0.0267(17) Uani 0.455(6) 1 d P A 2 H42D H 0.6305 0.2317 0.6978 0.040 Uiso 0.455(6) 1 calc PR A 2 H42E H 0.6803 0.1415 0.7353 0.040 Uiso 0.455(6) 1 calc PR A 2 H42F H 0.6779 0.1547 0.6659 0.040 Uiso 0.455(6) 1 calc PR A 2 C41B C 0.7532(9) 0.3358(9) 0.6733(8) 0.0237(17) Uani 0.455(6) 1 d P A 2 H41D H 0.7518 0.3045 0.6347 0.036 Uiso 0.455(6) 1 calc PR A 2 H41E H 0.8022 0.3768 0.6859 0.036 Uiso 0.455(6) 1 calc PR A 2 H41F H 0.7050 0.3777 0.6693 0.036 Uiso 0.455(6) 1 calc PR A 2 C40B C 0.7543(5) 0.2550(6) 0.7203(4) 0.0189(18) Uani 0.455(6) 1 d P A 2 H40B H 0.7539 0.2893 0.7587 0.023 Uiso 0.455(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0156(12) 0.0190(12) 0.0162(12) 0.0017(9) 0.0065(10) 0.0033(10) C2 0.0182(13) 0.0205(13) 0.0262(14) -0.0038(11) 0.0010(11) 0.0021(10) C3 0.0201(14) 0.0193(13) 0.0387(16) 0.0017(11) 0.0064(12) 0.0047(11) C4 0.0207(14) 0.0241(14) 0.0280(15) 0.0098(11) 0.0066(11) 0.0089(11) C5 0.0184(13) 0.0310(14) 0.0160(13) 0.0018(10) 0.0041(10) 0.0049(11) C6 0.0228(13) 0.0170(12) 0.0189(13) -0.0024(10) 0.0061(11) 0.0005(10) C7 0.041(2) 0.0183(15) 0.087(3) -0.0004(16) -0.0163(18) 0.0062(13) C8 0.0355(17) 0.0407(17) 0.0205(14) -0.0013(12) -0.0050(13) 0.0076(13) C9 0.0219(13) 0.0129(12) 0.0224(13) -0.0045(10) 0.0010(11) -0.0019(10) C10 0.0258(15) 0.0274(14) 0.0274(15) -0.0023(11) -0.0029(12) -0.0067(12) C11 0.0221(14) 0.0178(13) 0.0279(14) -0.0001(10) 0.0047(11) -0.0040(10) C12 0.0303(15) 0.0287(14) 0.0195(13) -0.0100(11) 0.0084(12) -0.0007(12) C13 0.056(2) 0.122(4) 0.0303(19) -0.015(2) 0.0100(17) 0.012(2) C14 0.0328(18) 0.087(3) 0.047(2) -0.0352(19) 0.0233(16) -0.0058(17) C15 0.0185(12) 0.0076(11) 0.0188(12) 0.0015(9) 0.0030(10) 0.0028(9) C16 0.0220(13) 0.0132(12) 0.0154(12) -0.0008(9) 0.0049(10) 0.0015(9) C17 0.0224(13) 0.0124(11) 0.0201(13) -0.0021(10) 0.0016(11) 0.0015(10) C18 0.0167(13) 0.0152(12) 0.0313(15) -0.0013(10) 0.0026(11) -0.0002(10) C19 0.0230(13) 0.0140(12) 0.0240(13) 0.0010(10) 0.0088(11) 0.0017(10) C20 0.0217(13) 0.0153(12) 0.0165(12) 0.0015(9) 0.0062(10) 0.0030(10) C21 0.0251(15) 0.0275(14) 0.0252(14) -0.0053(11) -0.0032(12) 0.0012(11) C22 0.0264(15) 0.0379(16) 0.0342(16) 0.0021(13) 0.0143(13) -0.0001(12) C23 0.0251(14) 0.0192(13) 0.0130(12) -0.0034(10) 0.0008(10) 0.0010(10) C24 0.0483(18) 0.0160(13) 0.0192(14) -0.0011(10) 0.0034(12) 0.0039(12) C25 0.0323(16) 0.0246(14) 0.0364(16) -0.0154(12) 0.0094(13) -0.0009(12) C26 0.0250(14) 0.0206(13) 0.0126(12) 0.0035(9) 0.0052(10) 0.0044(10) C27 0.0260(14) 0.0208(13) 0.0198(13) 0.0066(10) 0.0074(11) 0.0002(11) C28 0.0333(16) 0.0245(14) 0.0176(13) 0.0033(10) -0.0004(12) 0.0031(11) C29 0.0167(12) 0.0209(12) 0.0176(12) -0.0044(10) 0.0030(10) -0.0017(10) C30 0.0255(14) 0.0256(14) 0.0175(13) -0.0012(10) 0.0022(11) -0.0079(11) C31 0.0298(15) 0.0327(15) 0.0170(13) -0.0017(11) 0.0027(11) -0.0026(12) C32 0.0203(14) 0.0317(15) 0.0206(14) -0.0117(11) -0.0015(11) -0.0026(11) C33 0.0162(13) 0.0196(13) 0.0284(14) -0.0080(10) 0.0054(11) -0.0011(10) C34 0.0182(13) 0.0200(13) 0.0175(12) -0.0006(10) 0.0046(10) 0.0001(10) C35 0.055(2) 0.0502(19) 0.0159(15) 0.0021(13) -0.0076(14) -0.0136(16) C36 0.0299(15) 0.0247(14) 0.0362(16) -0.0106(12) 0.0032(13) -0.0088(12) C37 0.0362(16) 0.0371(16) 0.0206(14) 0.0019(12) 0.0071(12) -0.0196(13) C38 0.0372(17) 0.0327(16) 0.0377(17) 0.0204(13) -0.0074(14) -0.0162(13) C39 0.135(4) 0.061(2) 0.0299(19) -0.0031(16) 0.036(2) -0.051(2) C43 0.0332(16) 0.0316(15) 0.0117(13) 0.0026(11) 0.0012(11) 0.0035(12) C44 0.0358(16) 0.0405(17) 0.0204(14) 0.0071(12) 0.0018(12) 0.0019(13) C45 0.0298(15) 0.0410(17) 0.0254(15) 0.0125(12) 0.0060(12) 0.0102(13) C46 0.0258(14) 0.0197(13) 0.0243(14) 0.0036(10) 0.0075(11) 0.0069(11) N1 0.0166(10) 0.0151(10) 0.0136(10) -0.0015(8) 0.0025(8) -0.0007(8) N2 0.0183(10) 0.0132(10) 0.0116(10) -0.0003(7) 0.0024(8) 0.0007(8) N3 0.0209(11) 0.0209(10) 0.0110(10) 0.0004(8) 0.0027(8) -0.0060(8) O1 0.0222(9) 0.0201(8) 0.0121(8) 0.0016(7) 0.0028(7) 0.0027(7) P1 0.0186(3) 0.0159(3) 0.0142(3) -0.0028(2) 0.0020(3) -0.0004(2) P2 0.0173(3) 0.0155(3) 0.0108(3) 0.0004(2) 0.0020(2) 0.0009(2) P3 0.0180(3) 0.0245(4) 0.0153(3) 0.0010(3) 0.0049(3) -0.0045(3) Y1 0.01445(12) 0.01284(12) 0.01031(11) -0.00003(8) 0.00206(8) -0.00119(9) C42A 0.038(3) 0.048(4) 0.044(4) 0.002(3) 0.026(3) 0.010(3) C41A 0.021(4) 0.019(6) 0.030(3) -0.002(4) 0.006(3) 0.000(3) C40A 0.026(3) 0.015(4) 0.023(3) -0.007(3) 0.014(3) 0.003(3) C42B 0.018(3) 0.029(3) 0.036(4) -0.005(3) 0.011(3) -0.002(3) C41B 0.021(4) 0.019(6) 0.030(3) -0.002(4) 0.006(3) 0.000(3) C40B 0.018(3) 0.010(5) 0.032(5) -0.009(3) 0.012(3) 0.002(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.396(3) . ? C1 C2 1.400(3) . ? C1 N1 1.405(3) . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(4) . ? C3 C7 1.513(4) . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 C8 1.508(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.523(3) . ? C9 C10 1.531(3) . ? C9 P1 1.862(2) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.514(4) . ? C12 C13 1.516(4) . ? C12 P1 1.867(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N2 1.396(3) . ? C15 C20 1.404(3) . ? C15 C16 1.408(3) . ? C16 C17 1.392(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(3) . ? C17 C21 1.505(3) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.392(3) . ? C19 C22 1.515(3) . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.527(3) . ? C23 C24 1.530(3) . ? C23 P2 1.855(2) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.526(3) . ? C26 C28 1.538(3) . ? C26 P2 1.849(2) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.398(3) . ? C29 C30 1.405(3) . ? C29 N3 1.415(3) . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 C32 1.387(4) . ? C31 C35 1.514(4) . ? C32 C33 1.391(4) . ? C32 H32 0.9500 . ? C33 C34 1.395(3) . ? C33 C36 1.513(3) . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.523(4) . ? C37 C39 1.533(4) . ? C37 P3 1.865(3) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C43 O1 1.456(3) . ? C43 C44 1.515(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.508(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.528(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 O1 1.460(3) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? N1 P1 1.6782(19) . ? N1 Y1 2.2735(18) . ? N2 P2 1.6733(19) . ? N2 Y1 2.3173(19) . ? N3 P3 1.6783(19) . ? N3 Y1 2.2840(19) . ? O1 Y1 2.3821(15) . ? P1 Y1 2.8521(6) . ? P2 Y1 2.7754(6) . ? P3 C40A 1.825(8) . ? P3 C40B 1.945(8) . ? P3 Y1 2.8912(7) . ? C42A C40A 1.534(9) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C41A C40A 1.527(15) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C40A H40A 1.0000 . ? C42B C40B 1.517(10) . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C41B C40B 1.53(2) . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C40B H40B 1.0000 . ? 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 C6 C1 C2 117.3(2) . . ? C6 C1 N1 118.0(2) . . ? C2 C1 N1 124.6(2) . . ? C3 C2 C1 121.5(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 119.3(2) . . ? C4 C3 C7 121.2(2) . . ? C2 C3 C7 119.5(2) . . ? C3 C4 C5 120.9(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 118.8(2) . . ? C4 C5 C8 120.9(2) . . ? C6 C5 C8 120.2(2) . . ? C5 C6 C1 122.1(2) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 109.8(2) . . ? C11 C9 P1 110.75(16) . . ? C10 C9 P1 110.75(17) . . ? C11 C9 H9 108.5 . . ? C10 C9 H9 108.5 . . ? P1 C9 H9 108.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 111.0(3) . . ? C14 C12 P1 110.09(18) . . ? C13 C12 P1 111.9(2) . . ? C14 C12 H12 107.9 . . ? C13 C12 H12 107.9 . . ? P1 C12 H12 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C20 124.9(2) . . ? N2 C15 C16 118.1(2) . . ? C20 C15 C16 116.9(2) . . ? C17 C16 C15 122.2(2) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C18 118.7(2) . . ? C16 C17 C21 120.9(2) . . ? C18 C17 C21 120.3(2) . . ? C19 C18 C17 120.9(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.5(2) . . ? C18 C19 C22 120.3(2) . . ? C20 C19 C22 120.2(2) . . ? C19 C20 C15 121.7(2) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 111.0(2) . . ? C25 C23 P2 117.54(17) . . ? C24 C23 P2 108.76(16) . . ? C25 C23 H23 106.3 . . ? C24 C23 H23 106.3 . . ? P2 C23 H23 106.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 111.15(19) . . ? C27 C26 P2 109.91(16) . . ? C28 C26 P2 109.31(17) . . ? C27 C26 H26 108.8 . . ? C28 C26 H26 108.8 . . ? P2 C26 H26 108.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 117.3(2) . . ? C34 C29 N3 124.0(2) . . ? C30 C29 N3 118.7(2) . . ? C31 C30 C29 121.8(2) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 119.4(2) . . ? C30 C31 C35 120.0(2) . . ? C32 C31 C35 120.5(2) . . ? C31 C32 C33 120.7(2) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 119.1(2) . . ? C32 C33 C36 119.6(2) . . ? C34 C33 C36 121.3(2) . . ? C33 C34 C29 121.6(2) . . ? C33 C34 H34 119.2 . . ? C29 C34 H34 119.2 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 110.9(3) . . ? C38 C37 P3 110.37(18) . . ? C39 C37 P3 108.6(2) . . ? C38 C37 H37 109.0 . . ? C39 C37 H37 109.0 . . ? P3 C37 H37 109.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O1 C43 C44 105.4(2) . . ? O1 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? O1 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.8 . . ? C45 C44 C43 102.1(2) . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44B 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.2 . . ? C44 C45 C46 102.5(2) . . ? C44 C45 H45A 111.3 . . ? C46 C45 H45A 111.3 . . ? C44 C45 H45B 111.3 . . ? C46 C45 H45B 111.3 . . ? H45A C45 H45B 109.2 . . ? O1 C46 C45 104.40(19) . . ? O1 C46 H46A 110.9 . . ? C45 C46 H46A 110.9 . . ? O1 C46 H46B 110.9 . . ? C45 C46 H46B 110.9 . . ? H46A C46 H46B 108.9 . . ? C1 N1 P1 128.04(16) . . ? C1 N1 Y1 140.84(15) . . ? P1 N1 Y1 91.12(8) . . ? C15 N2 P2 130.56(16) . . ? C15 N2 Y1 142.02(15) . . ? P2 N2 Y1 86.55(8) . . ? C29 N3 P3 124.83(16) . . ? C29 N3 Y1 141.52(15) . . ? P3 N3 Y1 92.44(8) . . ? C43 O1 C46 109.48(17) . . ? C43 O1 Y1 122.68(13) . . ? C46 O1 Y1 127.81(13) . . ? N1 P1 C9 111.16(10) . . ? N1 P1 C12 109.49(11) . . ? C9 P1 C12 102.06(11) . . ? N1 P1 Y1 52.84(6) . . ? C9 P1 Y1 128.09(8) . . ? C12 P1 Y1 129.67(9) . . ? N2 P2 C26 113.76(10) . . ? N2 P2 C23 111.72(10) . . ? C26 P2 C23 103.50(10) . . ? N2 P2 Y1 56.45(7) . . ? C26 P2 Y1 133.51(8) . . ? C23 P2 Y1 122.64(8) . . ? N3 P3 C40A 102.4(2) . . ? N3 P3 C37 112.52(11) . . ? C40A P3 C37 97.7(3) . . ? N3 P3 C40B 111.2(3) . . ? C40A P3 C40B 17.9(2) . . ? C37 P3 C40B 107.1(3) . . ? N3 P3 Y1 52.12(7) . . ? C40A P3 Y1 130.9(2) . . ? C37 P3 Y1 129.47(10) . . ? C40B P3 Y1 123.4(3) . . ? N1 Y1 N3 113.49(7) . . ? N1 Y1 N2 103.79(6) . . ? N3 Y1 N2 123.98(7) . . ? N1 Y1 O1 127.33(6) . . ? N3 Y1 O1 101.25(6) . . ? N2 Y1 O1 86.32(6) . . ? N1 Y1 P2 102.16(5) . . ? N3 Y1 P2 93.46(5) . . ? N2 Y1 P2 37.00(5) . . ? O1 Y1 P2 114.31(4) . . ? N1 Y1 P1 36.03(5) . . ? N3 Y1 P1 132.55(5) . . ? N2 Y1 P1 102.15(5) . . ? O1 Y1 P1 91.37(4) . . ? P2 Y1 P1 122.549(19) . . ? N1 Y1 P3 100.33(5) . . ? N3 Y1 P3 35.45(5) . . ? N2 Y1 P3 154.54(5) . . ? O1 Y1 P3 85.52(4) . . ? P2 Y1 P3 128.904(19) . . ? P1 Y1 P3 102.119(19) . . ? C41A C40A C42A 110.1(7) . . ? C41A C40A P3 109.2(6) . . ? C42A C40A P3 113.4(5) . . ? C41A C40A H40A 108.0 . . ? C42A C40A H40A 108.0 . . ? P3 C40A H40A 108.0 . . ? C40B C42B H42D 109.5 . . ? C40B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C40B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C40B C41B H41D 109.5 . . ? C40B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C40B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C42B C40B C41B 111.6(8) . . ? C42B C40B P3 114.4(5) . . ? C41B C40B P3 108.2(8) . . ? C42B C40B H40B 107.4 . . ? C41B C40B H40B 107.4 . . ? P3 C40B H40B 107.4 . . ? 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 C6 C1 C2 C3 0.8(4) . . . . ? N1 C1 C2 C3 179.7(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C1 C2 C3 C7 -178.6(3) . . . . ? C2 C3 C4 C5 -1.8(4) . . . . ? C7 C3 C4 C5 177.7(3) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C3 C4 C5 C8 179.6(2) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? C8 C5 C6 C1 -177.9(2) . . . . ? C2 C1 C6 C5 -1.6(3) . . . . ? N1 C1 C6 C5 179.4(2) . . . . ? N2 C15 C16 C17 -179.0(2) . . . . ? C20 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C18 0.7(3) . . . . ? C15 C16 C17 C21 -179.0(2) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C21 C17 C18 C19 179.2(2) . . . . ? C17 C18 C19 C20 0.3(3) . . . . ? C17 C18 C19 C22 -179.1(2) . . . . ? C18 C19 C20 C15 -0.3(3) . . . . ? C22 C19 C20 C15 179.1(2) . . . . ? N2 C15 C20 C19 178.7(2) . . . . ? C16 C15 C20 C19 0.4(3) . . . . ? C34 C29 C30 C31 1.1(4) . . . . ? N3 C29 C30 C31 -179.1(2) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C29 C30 C31 C35 -179.1(3) . . . . ? C30 C31 C32 C33 -0.4(4) . . . . ? C35 C31 C32 C33 178.2(3) . . . . ? C31 C32 C33 C34 0.5(4) . . . . ? C31 C32 C33 C36 -178.2(2) . . . . ? C32 C33 C34 C29 0.1(4) . . . . ? C36 C33 C34 C29 178.9(2) . . . . ? C30 C29 C34 C33 -0.9(3) . . . . ? N3 C29 C34 C33 179.3(2) . . . . ? O1 C43 C44 C45 32.7(3) . . . . ? C43 C44 C45 C46 -39.9(3) . . . . ? C44 C45 C46 O1 33.0(3) . . . . ? C6 C1 N1 P1 -171.67(17) . . . . ? C2 C1 N1 P1 9.4(3) . . . . ? C6 C1 N1 Y1 8.3(4) . . . . ? C2 C1 N1 Y1 -170.65(18) . . . . ? C20 C15 N2 P2 0.2(3) . . . . ? C16 C15 N2 P2 178.48(15) . . . . ? C20 C15 N2 Y1 -165.06(17) . . . . ? C16 C15 N2 Y1 13.2(3) . . . . ? C34 C29 N3 P3 -48.7(3) . . . . ? C30 C29 N3 P3 131.5(2) . . . . ? C34 C29 N3 Y1 147.9(2) . . . . ? C30 C29 N3 Y1 -31.9(4) . . . . ? C44 C43 O1 C46 -12.3(3) . . . . ? C44 C43 O1 Y1 169.45(15) . . . . ? C45 C46 O1 C43 -12.9(3) . . . . ? C45 C46 O1 Y1 165.22(15) . . . . ? C1 N1 P1 C9 -57.6(2) . . . . ? Y1 N1 P1 C9 122.45(9) . . . . ? C1 N1 P1 C12 54.4(2) . . . . ? Y1 N1 P1 C12 -125.55(10) . . . . ? C1 N1 P1 Y1 180.0(2) . . . . ? C11 C9 P1 N1 -31.76(19) . . . . ? C10 C9 P1 N1 -153.86(16) . . . . ? C11 C9 P1 C12 -148.40(17) . . . . ? C10 C9 P1 C12 89.50(19) . . . . ? C11 C9 P1 Y1 26.9(2) . . . . ? C10 C9 P1 Y1 -95.16(17) . . . . ? C14 C12 P1 N1 42.8(2) . . . . ? C13 C12 P1 N1 166.7(2) . . . . ? C14 C12 P1 C9 160.7(2) . . . . ? C13 C12 P1 C9 -75.4(2) . . . . ? C14 C12 P1 Y1 -14.5(3) . . . . ? C13 C12 P1 Y1 109.3(2) . . . . ? C15 N2 P2 C26 -43.3(2) . . . . ? Y1 N2 P2 C26 127.65(9) . . . . ? C15 N2 P2 C23 73.4(2) . . . . ? Y1 N2 P2 C23 -115.62(9) . . . . ? C15 N2 P2 Y1 -171.0(2) . . . . ? C27 C26 P2 N2 -44.6(2) . . . . ? C28 C26 P2 N2 -166.80(15) . . . . ? C27 C26 P2 C23 -165.99(17) . . . . ? C28 C26 P2 C23 71.76(18) . . . . ? C27 C26 P2 Y1 20.9(2) . . . . ? C28 C26 P2 Y1 -101.30(17) . . . . ? C25 C23 P2 N2 -71.4(2) . . . . ? C24 C23 P2 N2 55.8(2) . . . . ? C25 C23 P2 C26 51.4(2) . . . . ? C24 C23 P2 C26 178.62(18) . . . . ? C25 C23 P2 Y1 -134.53(17) . . . . ? C24 C23 P2 Y1 -7.4(2) . . . . ? C29 N3 P3 C40A -37.0(3) . . . . ? Y1 N3 P3 C40A 132.8(2) . . . . ? C29 N3 P3 C37 66.9(2) . . . . ? Y1 N3 P3 C37 -123.32(11) . . . . ? C29 N3 P3 C40B -53.2(3) . . . . ? Y1 N3 P3 C40B 116.5(3) . . . . ? C29 N3 P3 Y1 -169.8(2) . . . . ? C38 C37 P3 N3 44.2(2) . . . . ? C39 C37 P3 N3 166.0(2) . . . . ? C38 C37 P3 C40A 151.0(3) . . . . ? C39 C37 P3 C40A -87.2(3) . . . . ? C38 C37 P3 C40B 166.6(3) . . . . ? C39 C37 P3 C40B -71.5(4) . . . . ? C38 C37 P3 Y1 -14.5(2) . . . . ? C39 C37 P3 Y1 107.3(2) . . . . ? C1 N1 Y1 N3 -49.0(2) . . . . ? P1 N1 Y1 N3 130.99(8) . . . . ? C1 N1 Y1 N2 88.2(2) . . . . ? P1 N1 Y1 N2 -91.77(8) . . . . ? C1 N1 Y1 O1 -175.8(2) . . . . ? P1 N1 Y1 O1 4.20(11) . . . . ? C1 N1 Y1 P2 50.3(2) . . . . ? P1 N1 Y1 P2 -129.75(6) . . . . ? C1 N1 Y1 P1 -180.0(3) . . . . ? C1 N1 Y1 P3 -83.5(2) . . . . ? P1 N1 Y1 P3 96.44(7) . . . . ? C29 N3 Y1 N1 92.3(3) . . . . ? P3 N3 Y1 N1 -74.14(9) . . . . ? C29 N3 Y1 N2 -35.0(3) . . . . ? P3 N3 Y1 N2 158.54(7) . . . . ? C29 N3 Y1 O1 -128.2(2) . . . . ? P3 N3 Y1 O1 65.38(9) . . . . ? C29 N3 Y1 P2 -12.6(2) . . . . ? P3 N3 Y1 P2 -178.99(7) . . . . ? C29 N3 Y1 P1 129.4(2) . . . . ? P3 N3 Y1 P1 -37.07(11) . . . . ? C29 N3 Y1 P3 166.4(3) . . . . ? C15 N2 Y1 N1 76.9(2) . . . . ? P2 N2 Y1 N1 -91.99(8) . . . . ? C15 N2 Y1 N3 -151.8(2) . . . . ? P2 N2 Y1 N3 39.34(10) . . . . ? C15 N2 Y1 O1 -50.7(2) . . . . ? P2 N2 Y1 O1 140.43(7) . . . . ? C15 N2 Y1 P2 168.9(3) . . . . ? C15 N2 Y1 P1 39.9(2) . . . . ? P2 N2 Y1 P1 -128.96(6) . . . . ? C15 N2 Y1 P3 -122.2(2) . . . . ? P2 N2 Y1 P3 68.92(13) . . . . ? C43 O1 Y1 N1 33.91(19) . . . . ? C46 O1 Y1 N1 -144.00(17) . . . . ? C43 O1 Y1 N3 -97.59(17) . . . . ? C46 O1 Y1 N3 84.49(18) . . . . ? C43 O1 Y1 N2 138.47(17) . . . . ? C46 O1 Y1 N2 -39.44(17) . . . . ? C43 O1 Y1 P2 163.35(15) . . . . ? C46 O1 Y1 P2 -14.56(18) . . . . ? C43 O1 Y1 P1 36.38(16) . . . . ? C46 O1 Y1 P1 -141.53(17) . . . . ? C43 O1 Y1 P3 -65.67(16) . . . . ? C46 O1 Y1 P3 116.42(17) . . . . ? N2 P2 Y1 N1 96.85(9) . . . . ? C26 P2 Y1 N1 4.73(12) . . . . ? C23 P2 Y1 N1 -167.25(11) . . . . ? N2 P2 Y1 N3 -148.23(9) . . . . ? C26 P2 Y1 N3 119.66(12) . . . . ? C23 P2 Y1 N3 -52.33(11) . . . . ? C26 P2 Y1 N2 -92.12(13) . . . . ? C23 P2 Y1 N2 95.90(12) . . . . ? N2 P2 Y1 O1 -44.24(8) . . . . ? C26 P2 Y1 O1 -136.36(12) . . . . ? C23 P2 Y1 O1 51.66(11) . . . . ? N2 P2 Y1 P1 64.39(7) . . . . ? C26 P2 Y1 P1 -27.72(12) . . . . ? C23 P2 Y1 P1 160.29(9) . . . . ? N2 P2 Y1 P3 -148.98(7) . . . . ? C26 P2 Y1 P3 118.91(11) . . . . ? C23 P2 Y1 P3 -53.08(10) . . . . ? C9 P1 Y1 N1 -88.93(13) . . . . ? C12 P1 Y1 N1 85.14(14) . . . . ? N1 P1 Y1 N3 -70.00(11) . . . . ? C9 P1 Y1 N3 -158.93(12) . . . . ? C12 P1 Y1 N3 15.15(13) . . . . ? N1 P1 Y1 N2 96.81(9) . . . . ? C9 P1 Y1 N2 7.88(11) . . . . ? C12 P1 Y1 N2 -178.05(12) . . . . ? N1 P1 Y1 O1 -176.66(9) . . . . ? C9 P1 Y1 O1 94.41(11) . . . . ? C12 P1 Y1 O1 -91.51(12) . . . . ? N1 P1 Y1 P2 63.09(8) . . . . ? C9 P1 Y1 P2 -25.85(10) . . . . ? C12 P1 Y1 P2 148.23(11) . . . . ? N1 P1 Y1 P3 -90.95(8) . . . . ? C9 P1 Y1 P3 -179.88(10) . . . . ? C12 P1 Y1 P3 -5.80(12) . . . . ? N3 P3 Y1 N1 116.26(10) . . . . ? C40A P3 Y1 N1 44.7(3) . . . . ? C37 P3 Y1 N1 -154.42(12) . . . . ? C40B P3 Y1 N1 24.2(3) . . . . ? C40A P3 Y1 N3 -71.6(3) . . . . ? C37 P3 Y1 N3 89.32(14) . . . . ? C40B P3 Y1 N3 -92.0(3) . . . . ? N3 P3 Y1 N2 -44.89(14) . . . . ? C40A P3 Y1 N2 -116.5(3) . . . . ? C37 P3 Y1 N2 44.42(16) . . . . ? C40B P3 Y1 N2 -136.9(3) . . . . ? N3 P3 Y1 O1 -116.58(9) . . . . ? C40A P3 Y1 O1 171.8(3) . . . . ? C37 P3 Y1 O1 -27.26(12) . . . . ? C40B P3 Y1 O1 151.4(3) . . . . ? N3 P3 Y1 P2 1.29(9) . . . . ? C40A P3 Y1 P2 -70.3(3) . . . . ? C37 P3 Y1 P2 90.61(11) . . . . ? C40B P3 Y1 P2 -90.7(3) . . . . ? N3 P3 Y1 P1 152.98(9) . . . . ? C40A P3 Y1 P1 81.4(3) . . . . ? C37 P3 Y1 P1 -117.70(11) . . . . ? C40B P3 Y1 P1 60.9(3) . . . . ? N3 P3 C40A C41A -57.5(5) . . . . ? C37 P3 C40A C41A -172.7(5) . . . . ? C40B P3 C40A C41A 64.2(15) . . . . ? Y1 P3 C40A C41A -7.4(6) . . . . ? N3 P3 C40A C42A 179.3(4) . . . . ? C37 P3 C40A C42A 64.1(5) . . . . ? C40B P3 C40A C42A -59.0(14) . . . . ? Y1 P3 C40A C42A -130.6(4) . . . . ? N3 P3 C40B C42B 84.1(6) . . . . ? C40A P3 C40B C42B 21.0(11) . . . . ? C37 P3 C40B C42B -39.3(6) . . . . ? Y1 P3 C40B C42B 141.8(5) . . . . ? N3 P3 C40B C41B -41.0(6) . . . . ? C40A P3 C40B C41B -104.1(17) . . . . ? C37 P3 C40B C41B -164.4(5) . . . . ? Y1 P3 C40B C41B 16.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.556 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.069