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 _publ_contact_author_name 'Wang, Zhong-Xia' _publ_contact_author_email zxwang@ustc.edu.cn _publ_section_title ; Dimethylaluminium iminophosphoranylenamides and iminophosphoranylanilides: synthesis, characterisation, and their controlled ring-opening polymerisation of e-caprolactone ; _publ_author_name 'Zhong-Xia Wang' # Attachment '- 9.cif' data_100119a _database_code_depnum_ccdc_archive 'CCDC 803993' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H34 Al N2 P' _chemical_formula_weight 540.59 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3833(13) _cell_length_b 13.9861(14) _cell_length_c 18.4732(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.1360(10) _cell_angle_gamma 90.00 _cell_volume 3199.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3167 _cell_measurement_theta_min 2.913 _cell_measurement_theta_max 24.954 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9716 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16587 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5650 _reflns_number_gt 2888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5650 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Al1 Al 0.72580(8) 0.47673(7) 0.31764(5) 0.0532(3) Uani 1 1 d . . . P1 P 0.60219(7) 0.53745(6) 0.18421(4) 0.0517(3) Uani 1 1 d . . . N1 N 0.82555(19) 0.48781(18) 0.24003(13) 0.0548(7) Uani 1 1 d . . . N2 N 0.60015(19) 0.53097(18) 0.27184(12) 0.0507(6) Uani 1 1 d . . . C1 C 0.6946(2) 0.4561(2) 0.14904(16) 0.0536(8) Uani 1 1 d . . . H1 H 0.6722 0.4148 0.1125 0.064 Uiso 1 1 calc R . . C2 C 0.7984(3) 0.4505(2) 0.17316(16) 0.0519(8) Uani 1 1 d . . . C3 C 0.8816(2) 0.3991(2) 0.12997(18) 0.0532(8) Uani 1 1 d . . . C4 C 0.9443(3) 0.3287(3) 0.1625(2) 0.0680(10) Uani 1 1 d . . . H4 H 0.9374 0.3173 0.2119 0.082 Uiso 1 1 calc R . . C5 C 1.0153(3) 0.2765(3) 0.1233(3) 0.0898(13) Uani 1 1 d . . . H5 H 1.0554 0.2288 0.1459 0.108 Uiso 1 1 calc R . . C6 C 1.0291(3) 0.2931(4) 0.0509(3) 0.1003(15) Uani 1 1 d . . . H6 H 1.0782 0.2573 0.0243 0.120 Uiso 1 1 calc R . . C7 C 0.9688(4) 0.3637(4) 0.0181(2) 0.0931(14) Uani 1 1 d . . . H7 H 0.9781 0.3763 -0.0309 0.112 Uiso 1 1 calc R . . C8 C 0.8948(3) 0.4159(3) 0.05743(19) 0.0690(10) Uani 1 1 d . . . H8 H 0.8537 0.4627 0.0346 0.083 Uiso 1 1 calc R . . C9 C 0.9324(3) 0.5256(3) 0.2461(2) 0.0661(10) Uani 1 1 d . . . C10 C 0.9982(3) 0.4963(3) 0.3026(2) 0.0979(14) Uani 1 1 d . . . H10 H 0.9739 0.4513 0.3359 0.118 Uiso 1 1 calc R . . C11 C 1.1037(5) 0.5361(5) 0.3090(4) 0.123(2) Uani 1 1 d . . . H11 H 1.1492 0.5191 0.3470 0.148 Uiso 1 1 calc R . . C12 C 1.1359(5) 0.6002(5) 0.2574(4) 0.137(2) Uani 1 1 d . . . H12 H 1.2055 0.6249 0.2606 0.165 Uiso 1 1 calc R . . C13 C 1.0729(4) 0.6296(4) 0.2023(3) 0.1242(19) Uani 1 1 d . . . H13 H 1.0977 0.6740 0.1688 0.149 Uiso 1 1 calc R . . C14 C 0.9701(3) 0.5918(3) 0.1972(2) 0.0862(12) Uani 1 1 d . . . H14 H 0.9251 0.6116 0.1597 0.103 Uiso 1 1 calc R . . C15 C 0.4714(3) 0.5102(3) 0.14706(16) 0.0545(8) Uani 1 1 d . . . C16 C 0.4350(3) 0.4189(3) 0.1525(2) 0.0833(12) Uani 1 1 d . . . H16 H 0.4796 0.3721 0.1722 0.100 Uiso 1 1 calc R . . C17 C 0.3315(3) 0.3945(3) 0.1290(2) 0.0957(14) Uani 1 1 d . . . H17 H 0.3069 0.3319 0.1330 0.115 Uiso 1 1 calc R . . C18 C 0.2676(3) 0.4629(4) 0.1006(2) 0.0936(13) Uani 1 1 d . . . H18 H 0.1986 0.4468 0.0849 0.112 Uiso 1 1 calc R . . C19 C 0.3019(3) 0.5544(4) 0.0944(2) 0.0959(14) Uani 1 1 d . . . H19 H 0.2569 0.6005 0.0742 0.115 Uiso 1 1 calc R . . C20 C 0.4035(3) 0.5788(3) 0.11819(18) 0.0756(11) Uani 1 1 d . . . H20 H 0.4267 0.6419 0.1148 0.091 Uiso 1 1 calc R . . C21 C 0.6437(3) 0.6527(2) 0.15205(19) 0.0586(9) Uani 1 1 d . . . C22 C 0.6879(3) 0.7185(3) 0.1982(2) 0.0826(12) Uani 1 1 d . . . H22 H 0.6893 0.7057 0.2475 0.099 Uiso 1 1 calc R . . C23 C 0.7309(4) 0.8044(3) 0.1730(3) 0.1177(17) Uani 1 1 d . . . H23 H 0.7616 0.8482 0.2049 0.141 Uiso 1 1 calc R . . C24 C 0.7269(4) 0.8224(4) 0.1007(3) 0.1227(19) Uani 1 1 d . . . H24 H 0.7533 0.8802 0.0832 0.147 Uiso 1 1 calc R . . C25 C 0.6854(4) 0.7583(4) 0.0538(3) 0.1163(17) Uani 1 1 d . . . H25 H 0.6850 0.7714 0.0045 0.140 Uiso 1 1 calc R . . C26 C 0.6440(3) 0.6743(3) 0.0786(2) 0.0892(12) Uani 1 1 d . . . H26 H 0.6154 0.6306 0.0458 0.107 Uiso 1 1 calc R . . C27 C 0.5153(2) 0.5700(2) 0.31494(16) 0.0494(8) Uani 1 1 d . . . C28 C 0.4861(3) 0.5235(3) 0.37765(19) 0.0722(10) Uani 1 1 d . . . H28 H 0.5198 0.4662 0.3898 0.087 Uiso 1 1 calc R . . C29 C 0.4081(3) 0.5600(3) 0.42260(18) 0.0773(11) Uani 1 1 d . . . H29 H 0.3913 0.5272 0.4649 0.093 Uiso 1 1 calc R . . C30 C 0.3540(3) 0.6434(3) 0.40720(18) 0.0652(10) Uani 1 1 d . . . C31 C 0.3829(3) 0.6889(3) 0.34433(18) 0.0635(9) Uani 1 1 d . . . H31 H 0.3483 0.7458 0.3322 0.076 Uiso 1 1 calc R . . C32 C 0.4606(3) 0.6541(2) 0.29862(17) 0.0600(9) Uani 1 1 d . . . H32 H 0.4768 0.6870 0.2563 0.072 Uiso 1 1 calc R . . C33 C 0.2682(3) 0.6832(3) 0.4566(2) 0.1017(15) Uani 1 1 d . . . H33A H 0.2356 0.6320 0.4833 0.153 Uiso 1 1 calc R . . H33B H 0.2141 0.7151 0.4282 0.153 Uiso 1 1 calc R . . H33C H 0.3004 0.7279 0.4896 0.153 Uiso 1 1 calc R . . C34 C 0.7033(3) 0.3415(2) 0.33746(19) 0.0796(11) Uani 1 1 d . . . H34A H 0.6902 0.3082 0.2928 0.119 Uiso 1 1 calc R . . H34B H 0.6422 0.3339 0.3688 0.119 Uiso 1 1 calc R . . H34C H 0.7664 0.3156 0.3605 0.119 Uiso 1 1 calc R . . C35 C 0.7656(3) 0.5613(3) 0.39801(18) 0.0792(11) Uani 1 1 d . . . H35A H 0.8270 0.5353 0.4231 0.119 Uiso 1 1 calc R . . H35B H 0.7060 0.5667 0.4309 0.119 Uiso 1 1 calc R . . H35C H 0.7835 0.6234 0.3795 0.119 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 Al1 0.0576(6) 0.0519(6) 0.0501(5) -0.0010(5) -0.0051(4) 0.0003(5) P1 0.0539(5) 0.0501(6) 0.0509(5) 0.0032(4) -0.0002(4) 0.0018(4) N1 0.0498(16) 0.0570(18) 0.0575(16) -0.0090(14) -0.0034(12) -0.0015(13) N2 0.0529(15) 0.0546(17) 0.0445(14) 0.0063(13) 0.0033(11) 0.0074(13) C1 0.052(2) 0.055(2) 0.0541(19) -0.0072(16) -0.0055(15) -0.0018(16) C2 0.060(2) 0.0400(19) 0.056(2) -0.0005(16) 0.0020(16) -0.0042(16) C3 0.050(2) 0.048(2) 0.061(2) -0.0037(17) 0.0059(16) -0.0056(16) C4 0.071(2) 0.060(3) 0.073(2) 0.001(2) 0.0018(19) 0.007(2) C5 0.070(3) 0.076(3) 0.123(4) -0.015(3) 0.005(3) 0.016(2) C6 0.072(3) 0.099(4) 0.129(4) -0.043(3) 0.030(3) -0.001(3) C7 0.090(3) 0.117(4) 0.073(3) -0.019(3) 0.023(2) -0.022(3) C8 0.067(2) 0.080(3) 0.059(2) -0.003(2) 0.0112(18) -0.003(2) C9 0.052(2) 0.070(3) 0.075(2) -0.024(2) -0.0022(19) 0.002(2) C10 0.074(3) 0.102(4) 0.118(3) -0.028(3) -0.028(3) 0.015(3) C11 0.093(4) 0.126(5) 0.151(5) -0.057(4) -0.048(4) 0.025(4) C12 0.070(4) 0.159(7) 0.183(7) -0.069(5) -0.016(4) 0.003(4) C13 0.095(4) 0.130(5) 0.147(5) -0.048(4) 0.029(3) -0.044(4) C14 0.067(3) 0.092(3) 0.099(3) -0.026(3) 0.015(2) -0.025(2) C15 0.056(2) 0.059(2) 0.0487(18) 0.0065(17) -0.0019(15) 0.0016(18) C16 0.074(3) 0.075(3) 0.101(3) 0.027(2) -0.021(2) -0.005(2) C17 0.086(3) 0.095(4) 0.106(3) 0.014(3) -0.019(3) -0.029(3) C18 0.066(3) 0.122(4) 0.092(3) 0.009(3) -0.019(2) -0.009(3) C19 0.068(3) 0.111(4) 0.108(3) 0.001(3) -0.031(2) 0.018(3) C20 0.076(3) 0.072(3) 0.080(2) -0.003(2) -0.017(2) 0.011(2) C21 0.066(2) 0.050(2) 0.060(2) 0.0064(18) 0.0091(17) 0.0039(17) C22 0.106(3) 0.063(3) 0.079(3) 0.007(2) 0.010(2) -0.014(2) C23 0.165(5) 0.072(3) 0.116(4) -0.001(3) 0.025(3) -0.044(3) C24 0.181(5) 0.063(3) 0.124(5) 0.017(3) 0.056(4) -0.020(3) C25 0.189(5) 0.080(4) 0.081(3) 0.024(3) 0.026(3) -0.013(4) C26 0.131(4) 0.072(3) 0.064(3) 0.013(2) 0.013(2) -0.004(3) C27 0.0512(19) 0.049(2) 0.0482(18) 0.0029(16) 0.0019(15) 0.0000(15) C28 0.070(2) 0.071(3) 0.075(2) 0.024(2) 0.0157(19) 0.020(2) C29 0.080(3) 0.091(3) 0.060(2) 0.025(2) 0.0177(19) 0.021(2) C30 0.065(2) 0.078(3) 0.052(2) 0.0016(19) -0.0004(17) 0.017(2) C31 0.069(2) 0.064(2) 0.057(2) 0.0009(18) -0.0008(18) 0.0191(18) C32 0.071(2) 0.056(2) 0.053(2) 0.0085(17) 0.0004(17) 0.0079(18) C33 0.102(3) 0.134(4) 0.070(3) 0.000(3) 0.009(2) 0.044(3) C34 0.106(3) 0.065(3) 0.067(2) 0.005(2) -0.006(2) 0.002(2) C35 0.085(3) 0.086(3) 0.066(2) -0.016(2) -0.001(2) -0.011(2) _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 Al1 N1 1.901(3) . ? Al1 N2 1.925(2) . ? Al1 C34 1.947(4) . ? Al1 C35 1.961(3) . ? P1 N2 1.622(2) . ? P1 C1 1.741(3) . ? P1 C21 1.794(3) . ? P1 C15 1.798(3) . ? N1 C2 1.382(4) . ? N1 C9 1.430(4) . ? N2 C27 1.428(4) . ? C1 C2 1.362(4) . ? C1 H1 0.9300 . ? C2 C3 1.489(4) . ? C3 C8 1.371(4) . ? C3 C4 1.390(4) . ? C4 C5 1.354(5) . ? C4 H4 0.9300 . ? C5 C6 1.369(6) . ? C5 H5 0.9300 . ? C6 C7 1.377(6) . ? C6 H6 0.9300 . ? C7 C8 1.379(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C14 1.376(5) . ? C9 C10 1.384(5) . ? C10 C11 1.425(6) . ? C10 H10 0.9300 . ? C11 C12 1.368(7) . ? C11 H11 0.9300 . ? C12 C13 1.346(7) . ? C12 H12 0.9300 . ? C13 C14 1.381(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.358(5) . ? C15 C20 1.382(4) . ? C16 C17 1.395(5) . ? C16 H16 0.9300 . ? C17 C18 1.347(6) . ? C17 H17 0.9300 . ? C18 C19 1.353(6) . ? C18 H18 0.9300 . ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.367(5) . ? C21 C26 1.390(5) . ? C22 C23 1.393(5) . ? C22 H22 0.9300 . ? C23 C24 1.362(6) . ? C23 H23 0.9300 . ? C24 C25 1.347(6) . ? C24 H24 0.9300 . ? C25 C26 1.361(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.378(4) . ? C27 C32 1.389(4) . ? C28 C29 1.374(4) . ? C28 H28 0.9300 . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 C31 1.373(4) . ? C30 C33 1.508(4) . ? C31 C32 1.371(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 Al1 N2 99.34(11) . . ? N1 Al1 C34 108.33(14) . . ? N2 Al1 C34 110.47(14) . . ? N1 Al1 C35 111.05(14) . . ? N2 Al1 C35 107.26(14) . . ? C34 Al1 C35 118.67(16) . . ? N2 P1 C1 110.35(14) . . ? N2 P1 C21 112.70(15) . . ? C1 P1 C21 105.98(15) . . ? N2 P1 C15 110.67(13) . . ? C1 P1 C15 108.11(15) . . ? C21 P1 C15 108.82(16) . . ? C2 N1 C9 115.7(3) . . ? C2 N1 Al1 119.1(2) . . ? C9 N1 Al1 125.0(2) . . ? C27 N2 P1 123.3(2) . . ? C27 N2 Al1 120.02(18) . . ? P1 N2 Al1 116.51(13) . . ? C2 C1 P1 122.4(2) . . ? C2 C1 H1 118.8 . . ? P1 C1 H1 118.8 . . ? C1 C2 N1 119.9(3) . . ? C1 C2 C3 120.4(3) . . ? N1 C2 C3 119.6(3) . . ? C8 C3 C4 118.4(3) . . ? C8 C3 C2 121.7(3) . . ? C4 C3 C2 119.8(3) . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 118.9(4) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C8 C7 120.4(4) . . ? C3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C14 C9 C10 119.7(4) . . ? C14 C9 N1 120.8(3) . . ? C10 C9 N1 119.6(4) . . ? C9 C10 C11 119.0(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 117.8(5) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C13 C12 C11 123.9(6) . . ? C13 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C12 C13 C14 117.9(6) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C9 C14 C13 121.7(5) . . ? C9 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C16 C15 C20 118.7(3) . . ? C16 C15 P1 118.0(3) . . ? C20 C15 P1 123.1(3) . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 119.1(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 121.4(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C15 120.4(4) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C22 C21 C26 117.4(3) . . ? C22 C21 P1 120.9(3) . . ? C26 C21 P1 121.3(3) . . ? C21 C22 C23 121.7(4) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 118.3(5) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 120.1(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.2(4) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C28 C27 C32 116.9(3) . . ? C28 C27 N2 118.9(3) . . ? C32 C27 N2 124.2(3) . . ? C29 C28 C27 121.3(3) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 122.2(3) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 116.1(3) . . ? C31 C30 C33 121.7(3) . . ? C29 C30 C33 122.1(3) . . ? C32 C31 C30 122.8(3) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C31 C32 C27 120.6(3) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al1 C34 H34A 109.5 . . ? Al1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Al1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Al1 C35 H35A 109.5 . . ? Al1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Al1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 N2 Al1 N1 C2 -53.1(2) . . . . ? C34 Al1 N1 C2 62.2(3) . . . . ? C35 Al1 N1 C2 -165.8(2) . . . . ? N2 Al1 N1 C9 132.2(3) . . . . ? C34 Al1 N1 C9 -112.4(3) . . . . ? C35 Al1 N1 C9 19.6(3) . . . . ? C1 P1 N2 C27 -163.7(2) . . . . ? C21 P1 N2 C27 78.1(3) . . . . ? C15 P1 N2 C27 -44.0(3) . . . . ? C1 P1 N2 Al1 21.6(2) . . . . ? C21 P1 N2 Al1 -96.66(17) . . . . ? C15 P1 N2 Al1 141.22(17) . . . . ? N1 Al1 N2 C27 -157.3(2) . . . . ? C34 Al1 N2 C27 89.0(2) . . . . ? C35 Al1 N2 C27 -41.7(3) . . . . ? N1 Al1 N2 P1 17.62(18) . . . . ? C34 Al1 N2 P1 -96.06(18) . . . . ? C35 Al1 N2 P1 133.23(17) . . . . ? N2 P1 C1 C2 -50.9(3) . . . . ? C21 P1 C1 C2 71.4(3) . . . . ? C15 P1 C1 C2 -172.1(3) . . . . ? P1 C1 C2 N1 19.7(4) . . . . ? P1 C1 C2 C3 -164.1(2) . . . . ? C9 N1 C2 C1 -147.9(3) . . . . ? Al1 N1 C2 C1 36.9(4) . . . . ? C9 N1 C2 C3 35.9(4) . . . . ? Al1 N1 C2 C3 -139.3(2) . . . . ? C1 C2 C3 C8 49.1(4) . . . . ? N1 C2 C3 C8 -134.7(3) . . . . ? C1 C2 C3 C4 -127.6(3) . . . . ? N1 C2 C3 C4 48.6(4) . . . . ? C8 C3 C4 C5 -1.3(5) . . . . ? C2 C3 C4 C5 175.5(3) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C4 C5 C6 C7 -0.4(7) . . . . ? C5 C6 C7 C8 -0.9(7) . . . . ? C4 C3 C8 C7 0.0(5) . . . . ? C2 C3 C8 C7 -176.7(3) . . . . ? C6 C7 C8 C3 1.0(6) . . . . ? C2 N1 C9 C14 52.4(4) . . . . ? Al1 N1 C9 C14 -132.8(3) . . . . ? C2 N1 C9 C10 -128.7(3) . . . . ? Al1 N1 C9 C10 46.2(4) . . . . ? C14 C9 C10 C11 0.4(6) . . . . ? N1 C9 C10 C11 -178.6(4) . . . . ? C9 C10 C11 C12 -1.6(7) . . . . ? C10 C11 C12 C13 1.9(9) . . . . ? C11 C12 C13 C14 -0.8(9) . . . . ? C10 C9 C14 C13 0.7(6) . . . . ? N1 C9 C14 C13 179.7(3) . . . . ? C12 C13 C14 C9 -0.5(7) . . . . ? N2 P1 C15 C16 -68.8(3) . . . . ? C1 P1 C15 C16 52.2(3) . . . . ? C21 P1 C15 C16 166.9(3) . . . . ? N2 P1 C15 C20 106.3(3) . . . . ? C1 P1 C15 C20 -132.7(3) . . . . ? C21 P1 C15 C20 -18.0(3) . . . . ? C20 C15 C16 C17 0.5(6) . . . . ? P1 C15 C16 C17 175.8(3) . . . . ? C15 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C19 0.0(7) . . . . ? C17 C18 C19 C20 -0.6(7) . . . . ? C18 C19 C20 C15 1.2(6) . . . . ? C16 C15 C20 C19 -1.1(5) . . . . ? P1 C15 C20 C19 -176.2(3) . . . . ? N2 P1 C21 C22 11.8(3) . . . . ? C1 P1 C21 C22 -109.0(3) . . . . ? C15 P1 C21 C22 135.0(3) . . . . ? N2 P1 C21 C26 -175.9(3) . . . . ? C1 P1 C21 C26 63.3(3) . . . . ? C15 P1 C21 C26 -52.7(3) . . . . ? C26 C21 C22 C23 0.6(6) . . . . ? P1 C21 C22 C23 173.1(3) . . . . ? C21 C22 C23 C24 0.8(7) . . . . ? C22 C23 C24 C25 -1.9(8) . . . . ? C23 C24 C25 C26 1.6(9) . . . . ? C24 C25 C26 C21 -0.1(8) . . . . ? C22 C21 C26 C25 -0.9(6) . . . . ? P1 C21 C26 C25 -173.5(4) . . . . ? P1 N2 C27 C28 145.8(3) . . . . ? Al1 N2 C27 C28 -39.7(4) . . . . ? P1 N2 C27 C32 -35.5(4) . . . . ? Al1 N2 C27 C32 139.0(3) . . . . ? C32 C27 C28 C29 -1.5(5) . . . . ? N2 C27 C28 C29 177.3(3) . . . . ? C27 C28 C29 C30 1.1(6) . . . . ? C28 C29 C30 C31 -0.5(6) . . . . ? C28 C29 C30 C33 179.9(4) . . . . ? C29 C30 C31 C32 0.3(5) . . . . ? C33 C30 C31 C32 180.0(3) . . . . ? C30 C31 C32 C27 -0.8(5) . . . . ? C28 C27 C32 C31 1.3(5) . . . . ? N2 C27 C32 C31 -177.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.297 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.051 # Attachment '- 14.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 803994' #TrackingRef '- 14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H50 Al N3 P2, 0.13(C8 H16 O2)' _chemical_formula_sum 'C55.04 H52.08 Al N3 O0.26 P2' _chemical_formula_weight 848.67 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7891(12) _cell_length_b 15.4618(14) _cell_length_c 17.1493(18) _cell_angle_alpha 63.402(8) _cell_angle_beta 72.448(9) _cell_angle_gamma 89.894(9) _cell_volume 2409.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6062 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9654 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20945 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.80 _reflns_number_total 11148 _reflns_number_gt 5786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11148 _refine_ls_number_parameters 566 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _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 P1 P 0.34377(7) 0.69434(5) 0.74476(5) 0.03870(19) Uani 1 1 d . . . P2 P 0.43138(8) 0.21991(5) 0.79593(5) 0.0463(2) Uani 1 1 d . . . Al1 Al 0.52329(7) 0.57291(6) 0.67322(5) 0.0391(2) Uani 1 1 d . . . N1 N 0.4927(2) 0.68838(16) 0.69020(14) 0.0413(5) Uani 1 1 d . . . N2 N 0.3533(2) 0.49673(16) 0.74830(14) 0.0397(5) Uani 1 1 d . . . N3 N 0.3063(2) 0.13906(17) 0.84735(15) 0.0512(6) Uani 1 1 d . . . C1 C 0.6046(3) 0.75356(19) 0.67169(18) 0.0439(6) Uani 1 1 d . . . C2 C 0.7207(3) 0.7667(2) 0.60025(19) 0.0519(7) Uani 1 1 d . . . H2 H 0.7210 0.7378 0.5629 0.062 Uiso 1 1 calc R . . C3 C 0.8349(3) 0.8220(2) 0.5843(2) 0.0599(8) Uani 1 1 d . . . H3 H 0.9104 0.8293 0.5365 0.072 Uiso 1 1 calc R . . C4 C 0.8397(3) 0.8669(2) 0.6377(2) 0.0602(9) Uani 1 1 d . . . C5 C 0.7240(3) 0.8572(2) 0.7051(2) 0.0634(9) Uani 1 1 d . . . H5 H 0.7233 0.8891 0.7401 0.076 Uiso 1 1 calc R . . C6 C 0.6078(3) 0.8016(2) 0.7230(2) 0.0556(8) Uani 1 1 d . . . H6 H 0.5319 0.7965 0.7697 0.067 Uiso 1 1 calc R . . C7 C 0.9667(4) 0.9224(3) 0.6227(3) 0.0843(12) Uani 1 1 d . . . H7A H 1.0365 0.9181 0.5748 0.126 Uiso 1 1 calc R . . H7B H 0.9868 0.8947 0.6791 0.126 Uiso 1 1 calc R . . H7C H 0.9576 0.9899 0.6045 0.126 Uiso 1 1 calc R . . C8 C 0.3166(2) 0.8198(2) 0.70341(18) 0.0408(6) Uani 1 1 d . . . C9 C 0.3550(3) 0.8786(2) 0.60795(18) 0.0485(7) Uani 1 1 d . . . H9 H 0.3947 0.8529 0.5685 0.058 Uiso 1 1 calc R . . C10 C 0.3344(3) 0.9750(2) 0.5715(2) 0.0571(8) Uani 1 1 d . . . H10 H 0.3594 1.0137 0.5077 0.069 Uiso 1 1 calc R . . C11 C 0.2770(3) 1.0137(2) 0.6293(2) 0.0638(9) Uani 1 1 d . . . H11 H 0.2633 1.0786 0.6045 0.077 Uiso 1 1 calc R . . C12 C 0.2394(4) 0.9563(3) 0.7245(3) 0.0689(9) Uani 1 1 d . . . H12 H 0.2014 0.9830 0.7635 0.083 Uiso 1 1 calc R . . C13 C 0.2584(3) 0.8589(2) 0.7619(2) 0.0544(8) Uani 1 1 d . . . H13 H 0.2322 0.8201 0.8258 0.065 Uiso 1 1 calc R . . C14 C 0.3006(3) 0.6382(2) 0.86942(17) 0.0432(6) Uani 1 1 d . . . C15 C 0.3960(3) 0.6148(2) 0.9105(2) 0.0570(8) Uani 1 1 d . . . H15 H 0.4840 0.6255 0.8746 0.068 Uiso 1 1 calc R . . C16 C 0.3598(4) 0.5749(3) 1.0063(2) 0.0747(11) Uani 1 1 d . . . H16 H 0.4241 0.5598 1.0342 0.090 Uiso 1 1 calc R . . C17 C 0.2305(4) 0.5578(3) 1.0597(2) 0.0736(11) Uani 1 1 d . . . H17 H 0.2075 0.5319 1.1235 0.088 Uiso 1 1 calc R . . C18 C 0.1346(3) 0.5787(3) 1.0192(2) 0.0680(10) Uani 1 1 d . . . H18 H 0.0466 0.5660 1.0557 0.082 Uiso 1 1 calc R . . C19 C 0.1685(3) 0.6183(2) 0.92511(19) 0.0552(8) Uani 1 1 d . . . H19 H 0.1032 0.6320 0.8980 0.066 Uiso 1 1 calc R . . C20 C 0.2280(2) 0.63170(19) 0.72386(16) 0.0377(6) Uani 1 1 d . . . C21 C 0.1171(3) 0.6735(2) 0.70741(18) 0.0473(7) Uani 1 1 d . . . H21 H 0.1113 0.7374 0.6976 0.057 Uiso 1 1 calc R . . C22 C 0.0161(3) 0.6200(2) 0.7058(2) 0.0562(8) Uani 1 1 d . . . H22 H -0.0580 0.6472 0.6956 0.067 Uiso 1 1 calc R . . C23 C 0.0267(3) 0.5256(2) 0.7195(2) 0.0551(8) Uani 1 1 d . . . H23 H -0.0410 0.4898 0.7180 0.066 Uiso 1 1 calc R . . C24 C 0.1343(3) 0.4834(2) 0.73512(18) 0.0480(7) Uani 1 1 d . . . H24 H 0.1383 0.4196 0.7442 0.058 Uiso 1 1 calc R . . C25 C 0.2391(2) 0.53544(19) 0.73768(16) 0.0380(6) Uani 1 1 d . . . C26 C 0.3417(3) 0.3930(2) 0.79337(18) 0.0422(6) Uani 1 1 d . . . C27 C 0.4115(3) 0.3466(2) 0.74794(18) 0.0452(7) Uani 1 1 d . . . H27 H 0.4540 0.3848 0.6846 0.054 Uiso 1 1 calc R . . C28 C 0.2586(3) 0.3422(2) 0.89335(19) 0.0478(7) Uani 1 1 d . . . C29 C 0.2893(4) 0.3668(3) 0.9540(2) 0.0689(10) Uani 1 1 d . . . H29 H 0.3581 0.4171 0.9316 0.083 Uiso 1 1 calc R . . C30 C 0.2187(5) 0.3173(3) 1.0480(3) 0.0910(13) Uani 1 1 d . . . H30 H 0.2420 0.3330 1.0887 0.109 Uiso 1 1 calc R . . C31 C 0.1158(5) 0.2460(3) 1.0806(3) 0.0979(15) Uani 1 1 d . . . H31 H 0.0685 0.2133 1.1437 0.117 Uiso 1 1 calc R . . C32 C 0.0813(4) 0.2221(3) 1.0227(3) 0.0831(12) Uani 1 1 d . . . H32 H 0.0097 0.1737 1.0458 0.100 Uiso 1 1 calc R . . C33 C 0.1520(3) 0.2691(2) 0.9289(2) 0.0615(8) Uani 1 1 d . . . H33 H 0.1282 0.2517 0.8894 0.074 Uiso 1 1 calc R . . C34 C 0.2037(3) 0.1349(2) 0.81530(19) 0.0483(7) Uani 1 1 d . . . C35 C 0.2000(3) 0.1942(2) 0.7267(2) 0.0627(9) Uani 1 1 d . . . H35 H 0.2715 0.2421 0.6823 0.075 Uiso 1 1 calc R . . C36 C 0.0902(4) 0.1822(3) 0.7043(3) 0.0814(11) Uani 1 1 d . . . H36 H 0.0900 0.2227 0.6447 0.098 Uiso 1 1 calc R . . C37 C -0.0196(4) 0.1120(3) 0.7676(3) 0.0790(11) Uani 1 1 d . . . C38 C -0.0162(4) 0.0548(3) 0.8540(3) 0.0749(10) Uani 1 1 d . . . H38 H -0.0886 0.0078 0.8983 0.090 Uiso 1 1 calc R . . C39 C 0.0923(3) 0.0648(3) 0.8775(2) 0.0637(9) Uani 1 1 d . . . H39 H 0.0914 0.0232 0.9371 0.076 Uiso 1 1 calc R . . C40 C -0.1420(5) 0.0983(4) 0.7437(4) 0.139(2) Uani 1 1 d . . . H40A H -0.1701 0.0298 0.7674 0.209 Uiso 1 1 calc R . . H40B H -0.1210 0.1312 0.6777 0.209 Uiso 1 1 calc R . . H40C H -0.2115 0.1255 0.7711 0.209 Uiso 1 1 calc R . . C41 C 0.5152(4) 0.1938(2) 0.8786(2) 0.0594(8) Uani 1 1 d . . . C42 C 0.4496(5) 0.1301(4) 0.9713(3) 0.1059(16) Uani 1 1 d . . . H42 H 0.3625 0.1021 0.9905 0.127 Uiso 1 1 calc R . . C43 C 0.5137(8) 0.1079(5) 1.0358(4) 0.153(3) Uani 1 1 d . . . H43 H 0.4692 0.0658 1.0981 0.184 Uiso 1 1 calc R . . C44 C 0.6406(8) 0.1477(5) 1.0079(5) 0.144(3) Uani 1 1 d . . . H44 H 0.6834 0.1318 1.0510 0.173 Uiso 1 1 calc R . . C45 C 0.7078(6) 0.2118(5) 0.9154(4) 0.1227(19) Uani 1 1 d . . . H45 H 0.7951 0.2391 0.8965 0.147 Uiso 1 1 calc R . . C46 C 0.6434(4) 0.2346(3) 0.8518(3) 0.0852(12) Uani 1 1 d . . . H46 H 0.6876 0.2783 0.7899 0.102 Uiso 1 1 calc R . . C47 C 0.5473(3) 0.2123(2) 0.6970(2) 0.0504(7) Uani 1 1 d . . . C48 C 0.5346(3) 0.1232(3) 0.6965(2) 0.0628(9) Uani 1 1 d . . . H48 H 0.4694 0.0722 0.7444 0.075 Uiso 1 1 calc R . . C49 C 0.6189(4) 0.1098(3) 0.6248(3) 0.0793(11) Uani 1 1 d . . . H49 H 0.6112 0.0496 0.6253 0.095 Uiso 1 1 calc R . . C50 C 0.7127(4) 0.1849(4) 0.5541(3) 0.0873(13) Uani 1 1 d . . . H50 H 0.7691 0.1754 0.5065 0.105 Uiso 1 1 calc R . . C51 C 0.7257(4) 0.2738(4) 0.5515(3) 0.0868(13) Uani 1 1 d . . . H51 H 0.7895 0.3247 0.5020 0.104 Uiso 1 1 calc R . . C52 C 0.6426(3) 0.2883(3) 0.6237(2) 0.0696(10) Uani 1 1 d . . . H52 H 0.6515 0.3488 0.6224 0.084 Uiso 1 1 calc R . . C53 C 0.5579(3) 0.6067(3) 0.5431(2) 0.0687(10) Uani 1 1 d . . . H53A H 0.5551 0.5478 0.5373 0.103 Uiso 1 1 calc R . . H53B H 0.6433 0.6457 0.5063 0.103 Uiso 1 1 calc R . . H53C H 0.4922 0.6432 0.5219 0.103 Uiso 1 1 calc R . . C54 C 0.6534(3) 0.5128(2) 0.7335(2) 0.0603(8) Uani 1 1 d . . . H54A H 0.6087 0.4592 0.7937 0.090 Uiso 1 1 calc R . . H54B H 0.7004 0.5609 0.7395 0.090 Uiso 1 1 calc R . . H54C H 0.7143 0.4893 0.6965 0.090 Uiso 1 1 calc R . . C57 C 0.0453(17) 0.5762(12) 0.4313(9) 0.116(7) Uiso 0.25 1 d PD . . H57A H 0.0321 0.5675 0.3822 0.139 Uiso 0.25 1 d PR . . H57B H 0.0934 0.6403 0.4061 0.139 Uiso 0.25 1 d PR . . C56 C 0.1177(10) 0.4949(13) 0.4867(10) 0.093(5) Uiso 0.25 1 d PD . . H56A H 0.1729 0.5200 0.5089 0.112 Uiso 0.25 1 d PR . . H56B H 0.1707 0.4695 0.4481 0.112 Uiso 0.25 1 d PR . . C55 C 0.0070(15) 0.4155(9) 0.5684(10) 0.091(6) Uiso 0.25 1 d PD . . H55A H 0.0311 0.3871 0.6232 0.109 Uiso 0.25 1 d PR . . H55B H -0.0105 0.3647 0.5538 0.109 Uiso 0.25 1 d PR . . O1 O -0.1096(10) 0.4619(9) 0.5834(6) 0.099(4) Uiso 0.25 1 d PD . . C58 C -0.0844(13) 0.5606(9) 0.5068(9) 0.072(4) Uiso 0.25 1 d PD . . H58A H -0.1546 0.5705 0.4816 0.086 Uiso 0.25 1 d PR . . H58B H -0.0817 0.6070 0.5295 0.086 Uiso 0.25 1 d PR . . 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 P1 0.0366(4) 0.0387(4) 0.0440(4) -0.0222(3) -0.0134(3) 0.0089(3) P2 0.0523(5) 0.0402(4) 0.0521(4) -0.0250(3) -0.0197(4) 0.0141(3) Al1 0.0352(4) 0.0400(5) 0.0452(4) -0.0221(4) -0.0141(3) 0.0096(3) N1 0.0333(11) 0.0372(12) 0.0525(12) -0.0227(10) -0.0107(10) 0.0021(9) N2 0.0353(11) 0.0347(12) 0.0513(12) -0.0209(10) -0.0163(10) 0.0078(9) N3 0.0560(15) 0.0402(14) 0.0545(14) -0.0215(11) -0.0159(12) 0.0084(11) C1 0.0394(15) 0.0351(14) 0.0558(16) -0.0194(12) -0.0174(13) 0.0046(12) C2 0.0469(17) 0.0464(17) 0.0536(16) -0.0202(14) -0.0105(13) 0.0042(14) C3 0.0439(17) 0.0500(19) 0.0652(19) -0.0164(15) -0.0077(14) -0.0019(14) C4 0.0541(19) 0.0407(17) 0.075(2) -0.0136(15) -0.0292(17) -0.0017(14) C5 0.065(2) 0.057(2) 0.081(2) -0.0380(18) -0.0313(18) 0.0019(17) C6 0.0455(17) 0.059(2) 0.0695(19) -0.0385(16) -0.0151(15) 0.0037(14) C7 0.064(2) 0.073(3) 0.103(3) -0.027(2) -0.035(2) -0.0117(19) C8 0.0361(14) 0.0398(15) 0.0527(15) -0.0278(12) -0.0136(12) 0.0091(11) C9 0.0511(17) 0.0447(17) 0.0510(16) -0.0243(13) -0.0159(13) 0.0112(13) C10 0.0587(19) 0.0446(18) 0.0615(18) -0.0207(15) -0.0183(15) 0.0078(15) C11 0.067(2) 0.0385(17) 0.083(2) -0.0258(17) -0.0255(18) 0.0111(15) C12 0.079(2) 0.058(2) 0.091(2) -0.055(2) -0.026(2) 0.0241(18) C13 0.063(2) 0.0492(18) 0.0565(17) -0.0325(15) -0.0148(15) 0.0114(15) C14 0.0450(16) 0.0430(16) 0.0449(14) -0.0227(12) -0.0159(12) 0.0101(12) C15 0.0486(17) 0.073(2) 0.0526(17) -0.0305(16) -0.0197(14) 0.0119(16) C16 0.072(2) 0.100(3) 0.059(2) -0.0353(19) -0.0345(18) 0.016(2) C17 0.074(2) 0.098(3) 0.0456(17) -0.0342(18) -0.0162(17) 0.017(2) C18 0.057(2) 0.087(3) 0.0518(18) -0.0322(18) -0.0076(16) 0.0113(18) C19 0.0470(17) 0.067(2) 0.0466(16) -0.0230(15) -0.0144(13) 0.0097(15) C20 0.0314(13) 0.0401(15) 0.0395(13) -0.0191(11) -0.0087(10) 0.0049(11) C21 0.0413(15) 0.0444(16) 0.0542(16) -0.0204(13) -0.0179(13) 0.0123(13) C22 0.0381(16) 0.062(2) 0.0674(19) -0.0248(16) -0.0247(14) 0.0129(14) C23 0.0401(16) 0.062(2) 0.0644(18) -0.0271(16) -0.0238(14) 0.0026(14) C24 0.0437(16) 0.0481(17) 0.0563(16) -0.0262(14) -0.0196(13) 0.0049(13) C25 0.0324(13) 0.0410(15) 0.0380(13) -0.0176(11) -0.0099(11) 0.0049(11) C26 0.0401(14) 0.0374(15) 0.0529(15) -0.0217(12) -0.0196(12) 0.0083(12) C27 0.0451(16) 0.0384(15) 0.0502(15) -0.0204(12) -0.0139(13) 0.0069(12) C28 0.0518(17) 0.0341(15) 0.0529(16) -0.0198(13) -0.0124(13) 0.0122(13) C29 0.082(3) 0.063(2) 0.0562(19) -0.0247(17) -0.0213(18) 0.0086(19) C30 0.122(4) 0.090(3) 0.058(2) -0.031(2) -0.033(2) 0.025(3) C31 0.115(4) 0.074(3) 0.059(2) -0.012(2) 0.002(2) 0.031(3) C32 0.072(3) 0.058(2) 0.080(3) -0.022(2) 0.011(2) 0.0058(19) C33 0.0553(19) 0.0476(19) 0.069(2) -0.0287(16) -0.0021(16) 0.0082(15) C34 0.0534(18) 0.0406(16) 0.0535(16) -0.0265(13) -0.0142(14) 0.0095(13) C35 0.073(2) 0.051(2) 0.0623(19) -0.0233(16) -0.0247(17) 0.0115(16) C36 0.108(3) 0.075(3) 0.088(3) -0.045(2) -0.057(3) 0.037(2) C37 0.068(2) 0.085(3) 0.121(3) -0.070(3) -0.046(2) 0.030(2) C38 0.059(2) 0.076(3) 0.094(3) -0.048(2) -0.016(2) 0.0048(19) C39 0.064(2) 0.061(2) 0.0626(19) -0.0327(17) -0.0108(16) 0.0055(17) C40 0.127(4) 0.148(5) 0.244(6) -0.134(5) -0.128(5) 0.064(4) C41 0.078(2) 0.0541(19) 0.069(2) -0.0380(16) -0.0400(18) 0.0291(17) C42 0.118(4) 0.118(4) 0.082(3) -0.032(3) -0.058(3) 0.009(3) C43 0.195(7) 0.168(6) 0.098(4) -0.033(4) -0.096(5) 0.022(5) C44 0.187(7) 0.161(6) 0.158(6) -0.087(5) -0.136(6) 0.063(5) C45 0.119(4) 0.145(5) 0.163(5) -0.090(4) -0.098(4) 0.040(4) C46 0.088(3) 0.090(3) 0.105(3) -0.054(2) -0.057(2) 0.023(2) C47 0.0520(17) 0.0530(18) 0.0565(17) -0.0313(15) -0.0232(14) 0.0210(14) C48 0.070(2) 0.067(2) 0.074(2) -0.0471(18) -0.0309(17) 0.0235(17) C49 0.092(3) 0.095(3) 0.095(3) -0.073(3) -0.044(2) 0.040(2) C50 0.080(3) 0.130(4) 0.087(3) -0.077(3) -0.033(2) 0.044(3) C51 0.074(3) 0.109(4) 0.068(2) -0.043(2) -0.0104(19) 0.023(3) C52 0.064(2) 0.070(2) 0.069(2) -0.0342(18) -0.0125(17) 0.0165(18) C53 0.072(2) 0.080(3) 0.0604(19) -0.0369(18) -0.0239(17) 0.0107(19) C54 0.0459(17) 0.057(2) 0.079(2) -0.0288(16) -0.0272(15) 0.0132(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 P1 N1 1.623(2) . ? P1 C20 1.792(3) . ? P1 C8 1.801(3) . ? P1 C14 1.811(3) . ? P2 N3 1.569(2) . ? P2 C27 1.795(3) . ? P2 C41 1.803(3) . ? P2 C47 1.832(3) . ? Al1 N2 1.906(2) . ? Al1 N1 1.946(2) . ? Al1 C53 1.962(3) . ? Al1 C54 1.978(3) . ? N1 C1 1.436(3) . ? N2 C25 1.394(3) . ? N2 C26 1.420(3) . ? N3 C34 1.389(4) . ? C1 C6 1.390(4) . ? C1 C2 1.401(4) . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.375(5) . ? C4 C7 1.508(4) . ? C5 C6 1.393(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C13 1.388(4) . ? C8 C9 1.392(4) . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.372(4) . ? C10 H10 0.9300 . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 C13 1.391(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.377(4) . ? C14 C19 1.398(4) . ? C15 C16 1.391(4) . ? C15 H15 0.9300 . ? C16 C17 1.366(5) . ? C16 H16 0.9300 . ? C17 C18 1.375(5) . ? C17 H17 0.9300 . ? C18 C19 1.368(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.402(4) . ? C20 C25 1.409(4) . ? C21 C22 1.384(4) . ? C21 H21 0.9300 . ? C22 C23 1.380(4) . ? C22 H22 0.9300 . ? C23 C24 1.369(4) . ? C23 H23 0.9300 . ? C24 C25 1.412(4) . ? C24 H24 0.9300 . ? C26 C27 1.354(4) . ? C26 C28 1.493(4) . ? C27 H27 0.9300 . ? C28 C29 1.377(4) . ? C28 C33 1.392(4) . ? C29 C30 1.387(5) . ? C29 H29 0.9300 . ? C30 C31 1.356(6) . ? C30 H30 0.9300 . ? C31 C32 1.349(6) . ? C31 H31 0.9300 . ? C32 C33 1.382(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.393(4) . ? C34 C39 1.398(4) . ? C35 C36 1.388(5) . ? C35 H35 0.9300 . ? C36 C37 1.390(5) . ? C36 H36 0.9300 . ? C37 C38 1.356(5) . ? C37 C40 1.537(5) . ? C38 C39 1.378(5) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C46 1.372(5) . ? C41 C42 1.386(5) . ? C42 C43 1.394(6) . ? C42 H42 0.9300 . ? C43 C44 1.351(8) . ? C43 H43 0.9300 . ? C44 C45 1.387(8) . ? C44 H44 0.9300 . ? C45 C46 1.382(6) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.386(4) . ? C47 C48 1.388(4) . ? C48 C49 1.391(5) . ? C48 H48 0.9300 . ? C49 C50 1.359(6) . ? C49 H49 0.9300 . ? C50 C51 1.360(6) . ? C50 H50 0.9300 . ? C51 C52 1.402(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C57 C55 0.58(2) 2_566 ? C57 O1 0.958(19) 2_566 ? C57 C58 1.524(9) . ? C57 C56 1.570(9) . ? C57 C56 1.847(19) 2_566 ? C57 C58 2.01(2) 2_566 ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C56 C58 0.88(2) 2_566 ? C56 O1 1.114(16) 2_566 ? C56 C55 1.534(9) . ? C56 C57 1.847(19) 2_566 ? C56 H56A 0.9600 . ? C56 H56B 0.9599 . ? C55 C57 0.58(2) 2_566 ? C55 C58 1.193(18) 2_566 ? C55 O1 1.460(8) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? O1 C57 0.958(19) 2_566 ? O1 C56 1.114(16) 2_566 ? O1 C58 1.456(8) . ? C58 C56 0.88(2) 2_566 ? C58 C55 1.193(18) 2_566 ? C58 C57 2.01(2) 2_566 ? C58 H58A 0.9599 . ? C58 H58B 0.9600 . ? 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 P1 C20 109.81(12) . . ? N1 P1 C8 110.52(12) . . ? C20 P1 C8 107.43(12) . . ? N1 P1 C14 114.71(12) . . ? C20 P1 C14 105.81(12) . . ? C8 P1 C14 108.22(13) . . ? N3 P2 C27 119.26(13) . . ? N3 P2 C41 105.51(15) . . ? C27 P2 C41 109.33(14) . . ? N3 P2 C47 112.78(14) . . ? C27 P2 C47 103.06(13) . . ? C41 P2 C47 106.28(15) . . ? N2 Al1 N1 98.39(10) . . ? N2 Al1 C53 110.66(13) . . ? N1 Al1 C53 109.91(13) . . ? N2 Al1 C54 109.46(12) . . ? N1 Al1 C54 106.46(12) . . ? C53 Al1 C54 119.76(15) . . ? C1 N1 P1 122.25(19) . . ? C1 N1 Al1 118.34(17) . . ? P1 N1 Al1 118.09(12) . . ? C25 N2 C26 116.6(2) . . ? C25 N2 Al1 121.37(17) . . ? C26 N2 Al1 118.97(17) . . ? C34 N3 P2 126.73(19) . . ? C6 C1 C2 117.2(3) . . ? C6 C1 N1 124.2(3) . . ? C2 C1 N1 118.5(3) . . ? C3 C2 C1 121.1(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C7 122.2(3) . . ? C3 C4 C7 121.1(3) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 120.3(3) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 119.5(3) . . ? C13 C8 P1 123.2(2) . . ? C9 C8 P1 117.3(2) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 119.7(3) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C19 119.2(2) . . ? C15 C14 P1 121.0(2) . . ? C19 C14 P1 119.8(2) . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 120.4(3) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C21 C20 C25 120.7(2) . . ? C21 C20 P1 119.2(2) . . ? C25 C20 P1 119.46(18) . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.2(3) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 121.7(3) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? N2 C25 C20 120.2(2) . . ? N2 C25 C24 122.3(3) . . ? C20 C25 C24 117.4(2) . . ? C27 C26 N2 120.2(2) . . ? C27 C26 C28 123.8(3) . . ? N2 C26 C28 115.8(2) . . ? C26 C27 P2 127.5(2) . . ? C26 C27 H27 116.3 . . ? P2 C27 H27 116.3 . . ? C29 C28 C33 118.0(3) . . ? C29 C28 C26 119.1(3) . . ? C33 C28 C26 122.8(3) . . ? C28 C29 C30 120.6(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.7(4) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.3(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? N3 C34 C35 126.5(3) . . ? N3 C34 C39 117.5(3) . . ? C35 C34 C39 116.1(3) . . ? C36 C35 C34 120.3(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 122.5(4) . . ? C35 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 117.1(3) . . ? C38 C37 C40 119.9(4) . . ? C36 C37 C40 123.0(4) . . ? C37 C38 C39 121.3(4) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C34 122.6(3) . . ? C38 C39 H39 118.7 . . ? C34 C39 H39 118.7 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 119.0(3) . . ? C46 C41 P2 121.5(3) . . ? C42 C41 P2 119.4(3) . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 120.0(6) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.7(5) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 119.2(5) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C41 C46 C45 121.0(4) . . ? C41 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C52 C47 C48 118.9(3) . . ? C52 C47 P2 125.0(3) . . ? C48 C47 P2 116.0(2) . . ? C47 C48 C49 120.4(4) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 119.7(4) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 121.4(4) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C50 C51 C52 119.7(4) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? C47 C52 C51 119.9(4) . . ? C47 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? Al1 C53 H53A 109.5 . . ? Al1 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Al1 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Al1 C54 H54A 109.5 . . ? Al1 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Al1 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C55 C57 O1 143(5) 2_566 2_566 ? C55 C57 C58 45(2) 2_566 . ? O1 C57 C58 138.4(14) 2_566 . ? C55 C57 C56 141(2) 2_566 . ? O1 C57 C56 44.6(10) 2_566 . ? C58 C57 C56 101.7(6) . . ? C55 C57 C56 49.3(17) 2_566 2_566 ? O1 C57 C56 114.9(18) 2_566 2_566 ? C58 C57 C56 28.2(8) . 2_566 ? C56 C57 C56 91.7(7) . 2_566 ? C55 C57 C58 123(3) 2_566 2_566 ? O1 C57 C58 42.6(9) 2_566 2_566 ? C58 C57 C58 96.1(7) . 2_566 ? C56 C57 C58 24.7(7) . 2_566 ? C56 C57 C58 76.9(7) 2_566 2_566 ? C55 C57 H57A 74.0 2_566 . ? O1 C57 H57A 73.3 2_566 . ? C58 C57 H57A 111.9 . . ? C56 C57 H57A 112.0 . . ? C56 C57 H57A 92.3 2_566 . ? C58 C57 H57A 92.6 2_566 . ? C55 C57 H57B 102.2 2_566 . ? O1 C57 H57B 105.2 2_566 . ? C58 C57 H57B 110.9 . . ? C56 C57 H57B 110.9 . . ? C56 C57 H57B 138.5 2_566 . ? C58 C57 H57B 134.3 2_566 . ? H57A C57 H57B 109.2 . . ? C58 C56 O1 93.1(17) 2_566 2_566 ? C58 C56 C55 50.8(12) 2_566 . ? O1 C56 C55 122.8(14) 2_566 . ? C58 C56 C57 106.9(17) 2_566 . ? O1 C56 C57 37.1(10) 2_566 . ? C55 C56 C57 104.9(6) . . ? C58 C56 C57 55.1(12) 2_566 2_566 ? O1 C56 C57 108.7(13) 2_566 2_566 ? C55 C56 C57 16.6(7) . 2_566 ? C57 C56 C57 88.3(7) . 2_566 ? C58 C56 H56A 140.9 2_566 . ? O1 C56 H56A 122.3 2_566 . ? C55 C56 H56A 110.1 . . ? C57 C56 H56A 111.4 . . ? C57 C56 H56A 118.0 2_566 . ? C58 C56 H56B 63.0 2_566 . ? O1 C56 H56B 73.3 2_566 . ? C55 C56 H56B 111.2 . . ? C57 C56 H56B 110.3 . . ? C57 C56 H56B 118.0 2_566 . ? H56A C56 H56B 108.9 . . ? C57 C55 C58 114(3) 2_566 2_566 ? C57 C55 O1 23(3) 2_566 . ? C58 C55 O1 122.5(11) 2_566 . ? C57 C55 C56 114(2) 2_566 . ? C58 C55 C56 34.8(10) 2_566 . ? O1 C55 C56 107.4(6) . . ? C57 C55 H55A 123.2 2_566 . ? C58 C55 H55A 122.4 2_566 . ? O1 C55 H55A 110.2 . . ? C56 C55 H55A 111.0 . . ? C57 C55 H55B 86.8 2_566 . ? C58 C55 H55B 75.0 2_566 . ? O1 C55 H55B 110.0 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.5 . . ? C57 O1 C56 98.2(15) 2_566 2_566 ? C57 O1 C58 111.0(11) 2_566 . ? C56 O1 C58 37.0(11) 2_566 . ? C57 O1 C55 14(2) 2_566 . ? C56 O1 C55 104.9(11) 2_566 . ? C58 O1 C55 108.8(5) . . ? C56 C58 C55 94.4(16) 2_566 2_566 ? C56 C58 O1 49.8(11) 2_566 . ? C55 C58 O1 123.2(11) 2_566 . ? C56 C58 C57 96.8(16) 2_566 . ? C55 C58 C57 20.2(12) 2_566 . ? O1 C58 C57 110.1(6) . . ? C56 C58 C57 48.4(12) 2_566 2_566 ? C55 C58 C57 97.1(11) 2_566 2_566 ? O1 C58 C57 26.4(5) . 2_566 ? C57 C58 C57 83.9(7) . 2_566 ? C56 C58 H58A 69.9 2_566 . ? C55 C58 H58A 89.6 2_566 . ? O1 C58 H58A 109.7 . . ? C57 C58 H58A 109.3 . . ? C57 C58 H58A 118.2 2_566 . ? C56 C58 H58B 151.2 2_566 . ? C55 C58 H58B 114.5 2_566 . ? O1 C58 H58B 109.1 . . ? C57 C58 H58B 110.3 . . ? C57 C58 H58B 123.3 2_566 . ? H58A C58 H58B 108.2 . . ? 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 C20 P1 N1 C1 161.79(19) . . . . ? C8 P1 N1 C1 43.4(2) . . . . ? C14 P1 N1 C1 -79.2(2) . . . . ? C20 P1 N1 Al1 -31.52(16) . . . . ? C8 P1 N1 Al1 -149.86(13) . . . . ? C14 P1 N1 Al1 87.46(16) . . . . ? N2 Al1 N1 C1 159.61(18) . . . . ? C53 Al1 N1 C1 -84.8(2) . . . . ? C54 Al1 N1 C1 46.4(2) . . . . ? N2 Al1 N1 P1 -7.61(14) . . . . ? C53 Al1 N1 P1 108.03(16) . . . . ? C54 Al1 N1 P1 -120.87(15) . . . . ? N1 Al1 N2 C25 50.2(2) . . . . ? C53 Al1 N2 C25 -64.8(2) . . . . ? C54 Al1 N2 C25 161.1(2) . . . . ? N1 Al1 N2 C26 -150.40(19) . . . . ? C53 Al1 N2 C26 94.5(2) . . . . ? C54 Al1 N2 C26 -39.5(2) . . . . ? C27 P2 N3 C34 49.1(3) . . . . ? C41 P2 N3 C34 172.5(2) . . . . ? C47 P2 N3 C34 -71.9(3) . . . . ? P1 N1 C1 C6 24.0(4) . . . . ? Al1 N1 C1 C6 -142.6(2) . . . . ? P1 N1 C1 C2 -159.1(2) . . . . ? Al1 N1 C1 C2 34.3(3) . . . . ? C6 C1 C2 C3 2.6(4) . . . . ? N1 C1 C2 C3 -174.5(3) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C2 C3 C4 C5 -2.6(5) . . . . ? C2 C3 C4 C7 176.7(3) . . . . ? C3 C4 C5 C6 2.9(5) . . . . ? C7 C4 C5 C6 -176.3(3) . . . . ? C2 C1 C6 C5 -2.2(4) . . . . ? N1 C1 C6 C5 174.7(3) . . . . ? C4 C5 C6 C1 -0.6(5) . . . . ? N1 P1 C8 C13 -132.8(2) . . . . ? C20 P1 C8 C13 107.4(3) . . . . ? C14 P1 C8 C13 -6.4(3) . . . . ? N1 P1 C8 C9 48.1(2) . . . . ? C20 P1 C8 C9 -71.7(2) . . . . ? C14 P1 C8 C9 174.5(2) . . . . ? C13 C8 C9 C10 -0.6(4) . . . . ? P1 C8 C9 C10 178.6(2) . . . . ? C8 C9 C10 C11 0.6(5) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C9 C8 C13 C12 -0.2(4) . . . . ? P1 C8 C13 C12 -179.3(2) . . . . ? C11 C12 C13 C8 0.8(5) . . . . ? N1 P1 C14 C15 14.9(3) . . . . ? C20 P1 C14 C15 136.1(3) . . . . ? C8 P1 C14 C15 -109.0(3) . . . . ? N1 P1 C14 C19 -165.1(2) . . . . ? C20 P1 C14 C19 -43.9(3) . . . . ? C8 P1 C14 C19 71.0(3) . . . . ? C19 C14 C15 C16 -2.2(5) . . . . ? P1 C14 C15 C16 177.8(3) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C18 0.8(6) . . . . ? C16 C17 C18 C19 -1.0(6) . . . . ? C17 C18 C19 C14 -0.4(5) . . . . ? C15 C14 C19 C18 2.0(5) . . . . ? P1 C14 C19 C18 -178.0(3) . . . . ? N1 P1 C20 C21 -138.4(2) . . . . ? C8 P1 C20 C21 -18.1(2) . . . . ? C14 P1 C20 C21 97.3(2) . . . . ? N1 P1 C20 C25 51.0(2) . . . . ? C8 P1 C20 C25 171.20(19) . . . . ? C14 P1 C20 C25 -73.4(2) . . . . ? C25 C20 C21 C22 0.9(4) . . . . ? P1 C20 C21 C22 -169.7(2) . . . . ? C20 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C26 N2 C25 C20 158.4(2) . . . . ? Al1 N2 C25 C20 -41.8(3) . . . . ? C26 N2 C25 C24 -25.2(4) . . . . ? Al1 N2 C25 C24 134.7(2) . . . . ? C21 C20 C25 N2 176.0(2) . . . . ? P1 C20 C25 N2 -13.4(3) . . . . ? C21 C20 C25 C24 -0.6(4) . . . . ? P1 C20 C25 C24 169.93(19) . . . . ? C23 C24 C25 N2 -176.3(2) . . . . ? C23 C24 C25 C20 0.2(4) . . . . ? C25 N2 C26 C27 118.2(3) . . . . ? Al1 N2 C26 C27 -42.2(3) . . . . ? C25 N2 C26 C28 -66.7(3) . . . . ? Al1 N2 C26 C28 133.0(2) . . . . ? N2 C26 C27 P2 169.64(19) . . . . ? C28 C26 C27 P2 -5.1(4) . . . . ? N3 P2 C27 C26 58.6(3) . . . . ? C41 P2 C27 C26 -62.9(3) . . . . ? C47 P2 C27 C26 -175.6(3) . . . . ? C27 C26 C28 C29 118.1(3) . . . . ? N2 C26 C28 C29 -56.9(4) . . . . ? C27 C26 C28 C33 -60.6(4) . . . . ? N2 C26 C28 C33 124.4(3) . . . . ? C33 C28 C29 C30 2.3(5) . . . . ? C26 C28 C29 C30 -176.4(3) . . . . ? C28 C29 C30 C31 -2.1(6) . . . . ? C29 C30 C31 C32 0.4(7) . . . . ? C30 C31 C32 C33 1.0(7) . . . . ? C31 C32 C33 C28 -0.6(6) . . . . ? C29 C28 C33 C32 -1.0(5) . . . . ? C26 C28 C33 C32 177.7(3) . . . . ? P2 N3 C34 C35 9.0(4) . . . . ? P2 N3 C34 C39 -170.7(2) . . . . ? N3 C34 C35 C36 -179.6(3) . . . . ? C39 C34 C35 C36 0.2(5) . . . . ? C34 C35 C36 C37 0.0(6) . . . . ? C35 C36 C37 C38 0.4(6) . . . . ? C35 C36 C37 C40 179.8(4) . . . . ? C36 C37 C38 C39 -1.0(6) . . . . ? C40 C37 C38 C39 179.6(4) . . . . ? C37 C38 C39 C34 1.3(6) . . . . ? N3 C34 C39 C38 179.0(3) . . . . ? C35 C34 C39 C38 -0.8(5) . . . . ? N3 P2 C41 C46 164.4(3) . . . . ? C27 P2 C41 C46 -66.2(3) . . . . ? C47 P2 C41 C46 44.4(3) . . . . ? N3 P2 C41 C42 -14.7(4) . . . . ? C27 P2 C41 C42 114.7(3) . . . . ? C47 P2 C41 C42 -134.7(3) . . . . ? C46 C41 C42 C43 -0.2(7) . . . . ? P2 C41 C42 C43 178.9(4) . . . . ? C41 C42 C43 C44 -0.8(9) . . . . ? C42 C43 C44 C45 1.0(11) . . . . ? C43 C44 C45 C46 -0.2(10) . . . . ? C42 C41 C46 C45 1.1(6) . . . . ? P2 C41 C46 C45 -178.0(3) . . . . ? C44 C45 C46 C41 -0.9(8) . . . . ? N3 P2 C47 C52 159.2(3) . . . . ? C27 P2 C47 C52 29.2(3) . . . . ? C41 P2 C47 C52 -85.7(3) . . . . ? N3 P2 C47 C48 -19.6(3) . . . . ? C27 P2 C47 C48 -149.5(2) . . . . ? C41 P2 C47 C48 95.5(3) . . . . ? C52 C47 C48 C49 1.8(5) . . . . ? P2 C47 C48 C49 -179.3(3) . . . . ? C47 C48 C49 C50 -1.1(5) . . . . ? C48 C49 C50 C51 -0.3(6) . . . . ? C49 C50 C51 C52 1.1(6) . . . . ? C48 C47 C52 C51 -1.1(5) . . . . ? P2 C47 C52 C51 -179.8(3) . . . . ? C50 C51 C52 C47 -0.4(6) . . . . ? C55 C57 C56 C58 51(7) 2_566 . . 2_566 ? O1 C57 C56 C58 -72.2(19) 2_566 . . 2_566 ? C58 C57 C56 C58 79(2) . . . 2_566 ? C56 C57 C56 C58 52.6(14) 2_566 . . 2_566 ? C55 C57 C56 O1 123(8) 2_566 . . 2_566 ? C58 C57 C56 O1 151(3) . . . 2_566 ? C56 C57 C56 O1 125(3) 2_566 . . 2_566 ? C58 C57 C56 O1 72.2(19) 2_566 . . 2_566 ? C55 C57 C56 C55 -2(8) 2_566 . . . ? O1 C57 C56 C55 -125(2) 2_566 . . . ? C58 C57 C56 C55 26(2) . . . . ? C56 C57 C56 C55 -0.4(15) 2_566 . . . ? C58 C57 C56 C55 -53.0(13) 2_566 . . . ? C55 C57 C56 C57 -2(6) 2_566 . . 2_566 ? O1 C57 C56 C57 -125(3) 2_566 . . 2_566 ? C58 C57 C56 C57 26.5(9) . . . 2_566 ? C56 C57 C56 C57 -0.001(2) 2_566 . . 2_566 ? C58 C57 C56 C57 -52.6(14) 2_566 . . 2_566 ? C58 C56 C55 C57 -98(5) 2_566 . . 2_566 ? O1 C56 C55 C57 -34(5) 2_566 . . 2_566 ? C57 C56 C55 C57 1(5) . . . 2_566 ? O1 C56 C55 C58 63.9(17) 2_566 . . 2_566 ? C57 C56 C55 C58 100(2) . . . 2_566 ? C57 C56 C55 C58 98(5) 2_566 . . 2_566 ? C58 C56 C55 O1 -122(2) 2_566 . . . ? O1 C56 C55 O1 -59(2) 2_566 . . . ? C57 C56 C55 O1 -23(2) . . . . ? C57 C56 C55 O1 -24(4) 2_566 . . . ? C58 C55 O1 C57 76(5) 2_566 . . 2_566 ? C56 C55 O1 C57 111(5) . . . 2_566 ? C57 C55 O1 C56 -63(4) 2_566 . . 2_566 ? C58 C55 O1 C56 13(2) 2_566 . . 2_566 ? C56 C55 O1 C56 48(2) . . . 2_566 ? C57 C55 O1 C58 -101(4) 2_566 . . . ? C58 C55 O1 C58 -25(2) 2_566 . . . ? C56 C55 O1 C58 9.4(18) . . . . ? C57 O1 C58 C56 75(2) 2_566 . . 2_566 ? C55 O1 C58 C56 89.9(18) . . . 2_566 ? C57 O1 C58 C55 11(3) 2_566 . . 2_566 ? C56 O1 C58 C55 -64.3(18) 2_566 . . 2_566 ? C55 O1 C58 C55 26(3) . . . 2_566 ? C57 O1 C58 C57 -6(3) 2_566 . . . ? C56 O1 C58 C57 -82(2) 2_566 . . . ? C55 O1 C58 C57 8.3(17) . . . . ? C56 O1 C58 C57 -75(2) 2_566 . . 2_566 ? C55 O1 C58 C57 15(2) . . . 2_566 ? C55 C57 C58 C56 84(4) 2_566 . . 2_566 ? O1 C57 C58 C56 -41(4) 2_566 . . 2_566 ? C56 C57 C58 C56 -71(2) . . . 2_566 ? C58 C57 C58 C56 -46.7(14) 2_566 . . 2_566 ? O1 C57 C58 C55 -125(7) 2_566 . . 2_566 ? C56 C57 C58 C55 -155(5) . . . 2_566 ? C56 C57 C58 C55 -84(4) 2_566 . . 2_566 ? C58 C57 C58 C55 -131(5) 2_566 . . 2_566 ? C55 C57 C58 O1 134(4) 2_566 . . . ? O1 C57 C58 O1 9(4) 2_566 . . . ? C56 C57 C58 O1 -22(2) . . . . ? C56 C57 C58 O1 49.6(13) 2_566 . . . ? C58 C57 C58 O1 2.8(14) 2_566 . . . ? C55 C57 C58 C57 131(5) 2_566 . . 2_566 ? O1 C57 C58 C57 6(3) 2_566 . . 2_566 ? C56 C57 C58 C57 -24.4(9) . . . 2_566 ? C56 C57 C58 C57 46.8(14) 2_566 . . 2_566 ? C58 C57 C58 C57 0.002(2) 2_566 . . 2_566 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.80 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.739 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.063