# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Dr. Werner Uhl' _publ_contact_author_email Uhlw@uni-muenster.de loop_ _publ_author_name S.Roters C.Appelt H.Westenberg A.Hepp J.C.Slootweg ; K.Lammertsma ; W.Uhl data_sr1712m _database_code_depnum_ccdc_archive 'CCDC 861398' #TrackingRef 'Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34 Al P' _chemical_formula_weight 356.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 10.8370(2) _cell_length_b 12.5241(2) _cell_length_c 17.2299(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.2810(10) _cell_angle_gamma 90.00 _cell_volume 2220.48(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4319 _cell_measurement_theta_min 4.2965 _cell_measurement_theta_max 71.7705 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8678 _exptl_absorpt_correction_T_max 0.9176 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12377 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.30 _diffrn_reflns_theta_max 66.00 _reflns_number_total 3839 _reflns_number_gt 3000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _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^)+(0.0979P)^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 3839 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 P1 P 0.52851(6) 0.99027(5) 0.11636(4) 0.0215(2) Uani 1 1 d . . . Al1 Al 0.58700(7) 1.14991(5) 0.04805(4) 0.0222(2) Uani 1 1 d . . . C4 C 0.5381(3) 1.26422(19) 0.11241(15) 0.0294(6) Uani 1 1 d . . . H4A H 0.4460 1.2598 0.1026 0.035 Uiso 1 1 calc R . . H4B H 0.5793 1.2488 0.1693 0.035 Uiso 1 1 calc R . . C41 C 0.5705(3) 1.38054(19) 0.09723(18) 0.0382(7) Uani 1 1 d . . . H41A H 0.6615 1.3863 0.1035 0.046 Uiso 1 1 calc R . . H41B H 0.5496 1.4265 0.1359 0.046 Uiso 1 1 calc R . . H41C H 0.5207 1.4013 0.0428 0.046 Uiso 1 1 calc R . . C5 C 0.7764(2) 1.13523(19) 0.06679(15) 0.0281(6) Uani 1 1 d . . . H5A H 0.7992 1.0612 0.0757 0.034 Uiso 1 1 calc R . . H5B H 0.7946 1.1569 0.0181 0.034 Uiso 1 1 calc R . . C51 C 0.8633(3) 1.1997(3) 0.13889(19) 0.0488(8) Uani 1 1 d . . . H51A H 0.8430 1.2743 0.1301 0.059 Uiso 1 1 calc R . . H51B H 0.9528 1.1883 0.1432 0.059 Uiso 1 1 calc R . . H51C H 0.8485 1.1771 0.1884 0.059 Uiso 1 1 calc R . . C1 C 0.3631(2) 0.99274(18) 0.12237(15) 0.0236(5) Uani 1 1 d . . . C11 C 0.3292(3) 0.9254(2) 0.17653(16) 0.0326(6) Uani 1 1 d . . . H11 H 0.3927 0.8781 0.2111 0.039 Uiso 1 1 calc R . . C12 C 0.2035(3) 0.9267(2) 0.18055(18) 0.0389(7) Uani 1 1 d . . . H12 H 0.1803 0.8806 0.2183 0.047 Uiso 1 1 calc R . . C13 C 0.1118(3) 0.9936(2) 0.13078(18) 0.0384(7) Uani 1 1 d . . . H13 H 0.0246 0.9933 0.1334 0.046 Uiso 1 1 calc R . . C14 C 0.1447(2) 1.0608(2) 0.07730(17) 0.0336(6) Uani 1 1 d . . . H14 H 0.0804 1.1075 0.0428 0.040 Uiso 1 1 calc R . . C15 C 0.2705(2) 1.06152(19) 0.07304(15) 0.0270(6) Uani 1 1 d . . . H15 H 0.2936 1.1092 0.0362 0.032 Uiso 1 1 calc R . . C2 C 0.6209(2) 1.00499(19) 0.22031(15) 0.0266(6) Uani 1 1 d . . . C21 C 0.6851(3) 1.0273(2) 0.28823(16) 0.0300(6) Uani 1 1 d . . . C22 C 0.7649(3) 1.0520(2) 0.37318(16) 0.0395(7) Uani 1 1 d . . . C221 C 0.6845(4) 1.1264(3) 0.4117(2) 0.0677(11) Uani 1 1 d . . . H22A H 0.6664 1.1923 0.3819 0.081 Uiso 1 1 calc R . . H22B H 0.7334 1.1407 0.4677 0.081 Uiso 1 1 calc R . . H22C H 0.6043 1.0920 0.4094 0.081 Uiso 1 1 calc R . . C222 C 0.8854(3) 1.1121(3) 0.3728(2) 0.0743(12) Uani 1 1 d . . . H22D H 0.9357 1.0688 0.3479 0.089 Uiso 1 1 calc R . . H22E H 0.9364 1.1286 0.4279 0.089 Uiso 1 1 calc R . . H22F H 0.8609 1.1771 0.3423 0.089 Uiso 1 1 calc R . . C223 C 0.7962(4) 0.9512(3) 0.4225(2) 0.0688(11) Uani 1 1 d . . . H22G H 0.7174 0.9127 0.4173 0.083 Uiso 1 1 calc R . . H22H H 0.8381 0.9687 0.4789 0.083 Uiso 1 1 calc R . . H22I H 0.8531 0.9077 0.4029 0.083 Uiso 1 1 calc R . . C3 C 0.5375(2) 0.86467(18) 0.06735(14) 0.0216(5) Uani 1 1 d . . . C31 C 0.6182(2) 0.78123(18) 0.08998(15) 0.0241(5) Uani 1 1 d . . . H31 H 0.6017 0.7272 0.0485 0.029 Uiso 1 1 calc R . . C32 C 0.7299(2) 0.75172(19) 0.16598(15) 0.0280(6) Uani 1 1 d . . . C321 C 0.8395(2) 0.8340(2) 0.18200(17) 0.0367(7) Uani 1 1 d . . . H32A H 0.8072 0.9029 0.1904 0.044 Uiso 1 1 calc R . . H32B H 0.8711 0.8368 0.1358 0.044 Uiso 1 1 calc R . . H32C H 0.9091 0.8138 0.2298 0.044 Uiso 1 1 calc R . . C322 C 0.6804(3) 0.7402(2) 0.23997(16) 0.0353(6) Uani 1 1 d . . . H32D H 0.6444 0.8069 0.2499 0.042 Uiso 1 1 calc R . . H32E H 0.7512 0.7205 0.2872 0.042 Uiso 1 1 calc R . . H32F H 0.6145 0.6860 0.2289 0.042 Uiso 1 1 calc R . . C323 C 0.7834(3) 0.6436(2) 0.15038(18) 0.0414(7) Uani 1 1 d . . . H32G H 0.8553 0.6239 0.1971 0.050 Uiso 1 1 calc R . . H32H H 0.8121 0.6486 0.1032 0.050 Uiso 1 1 calc R . . H32I H 0.7165 0.5905 0.1411 0.050 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 P1 0.0207(3) 0.0189(3) 0.0219(3) 0.0002(2) 0.0026(3) 0.0004(2) Al1 0.0225(4) 0.0171(4) 0.0242(4) -0.0012(3) 0.0034(3) 0.0006(3) C4 0.0348(14) 0.0217(13) 0.0305(14) -0.0055(11) 0.0083(12) 0.0026(11) C41 0.0468(17) 0.0237(14) 0.0422(16) -0.0069(12) 0.0111(14) 0.0016(12) C5 0.0260(13) 0.0248(13) 0.0315(14) -0.0019(11) 0.0059(11) -0.0004(10) C51 0.0257(14) 0.059(2) 0.0523(19) -0.0219(16) -0.0016(14) 0.0002(14) C1 0.0223(12) 0.0212(12) 0.0258(13) -0.0075(10) 0.0054(11) -0.0014(10) C11 0.0340(15) 0.0265(13) 0.0377(15) -0.0001(12) 0.0116(13) -0.0001(11) C12 0.0398(16) 0.0340(15) 0.0487(18) -0.0010(14) 0.0220(15) -0.0066(13) C13 0.0259(14) 0.0372(15) 0.0535(19) -0.0156(14) 0.0143(14) -0.0049(12) C14 0.0242(13) 0.0319(14) 0.0394(16) -0.0101(13) 0.0026(12) 0.0027(11) C15 0.0255(13) 0.0268(13) 0.0273(13) -0.0032(11) 0.0063(11) -0.0008(10) C2 0.0252(13) 0.0231(12) 0.0283(14) -0.0007(11) 0.0037(12) -0.0013(10) C21 0.0285(14) 0.0279(13) 0.0321(15) 0.0017(12) 0.0073(12) -0.0018(11) C22 0.0382(16) 0.0445(17) 0.0277(15) 0.0002(13) -0.0013(13) -0.0101(13) C221 0.077(3) 0.074(3) 0.050(2) -0.0250(19) 0.017(2) -0.014(2) C222 0.054(2) 0.112(3) 0.045(2) 0.002(2) -0.0021(18) -0.042(2) C223 0.069(3) 0.072(3) 0.042(2) 0.0162(19) -0.0153(18) -0.011(2) C3 0.0215(12) 0.0188(11) 0.0225(12) -0.0006(10) 0.0041(10) -0.0026(9) C31 0.0235(12) 0.0201(12) 0.0287(13) -0.0006(10) 0.0079(11) 0.0005(10) C32 0.0260(13) 0.0239(12) 0.0313(14) 0.0052(11) 0.0050(12) 0.0048(10) C321 0.0256(14) 0.0388(15) 0.0413(16) 0.0072(13) 0.0043(13) 0.0017(12) C322 0.0373(15) 0.0302(14) 0.0345(15) 0.0085(12) 0.0056(13) 0.0053(12) C323 0.0370(16) 0.0354(15) 0.0448(17) 0.0050(13) 0.0030(14) 0.0140(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C2 1.766(3) . ? P1 C3 1.802(2) . ? P1 C1 1.828(2) . ? P1 Al1 2.5004(9) . ? Al1 C4 1.982(2) . ? Al1 C5 1.984(3) . ? Al1 C3 2.031(2) 3_675 ? C4 C41 1.540(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C41 H41A 0.9599 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? C5 C51 1.533(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C51 H51A 0.9599 . ? C51 H51B 0.9599 . ? C51 H51C 0.9599 . ? C1 C11 1.390(4) . ? C1 C15 1.391(3) . ? C11 C12 1.385(4) . ? C11 H11 0.9600 . ? C12 C13 1.375(4) . ? C12 H12 0.9600 . ? C13 C14 1.375(4) . ? C13 H13 0.9600 . ? C14 C15 1.388(3) . ? C14 H14 0.9600 . ? C15 H15 0.9600 . ? C2 C21 1.192(4) . ? C21 C22 1.481(4) . ? C22 C223 1.500(4) . ? C22 C222 1.509(4) . ? C22 C221 1.559(4) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C3 C31 1.339(3) . ? C3 Al1 2.031(2) 3_675 ? C31 C32 1.524(3) . ? C31 H31 0.9600 . ? C32 C321 1.531(4) . ? C32 C323 1.529(3) . ? C32 C322 1.537(4) . ? C321 H32A 0.9599 . ? C321 H32B 0.9599 . ? C321 H32C 0.9599 . ? C322 H32D 0.9599 . ? C322 H32E 0.9599 . ? C322 H32F 0.9599 . ? C323 H32G 0.9599 . ? C323 H32H 0.9599 . ? C323 H32I 0.9599 . ? 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 C2 P1 C3 117.99(11) . . ? C2 P1 C1 101.25(11) . . ? C3 P1 C1 103.85(10) . . ? C2 P1 Al1 104.30(8) . . ? C3 P1 Al1 114.73(8) . . ? C1 P1 Al1 114.27(8) . . ? C4 Al1 C5 114.87(11) . . ? C4 Al1 C3 113.60(10) . 3_675 ? C5 Al1 C3 119.13(10) . 3_675 ? C4 Al1 P1 99.34(8) . . ? C5 Al1 P1 104.56(8) . . ? C3 Al1 P1 101.55(7) 3_675 . ? C41 C4 Al1 118.20(18) . . ? C41 C4 H4A 107.8 . . ? Al1 C4 H4A 107.8 . . ? C41 C4 H4B 107.8 . . ? Al1 C4 H4B 107.8 . . ? H4A C4 H4B 107.1 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C51 C5 Al1 115.11(18) . . ? C51 C5 H5A 108.5 . . ? Al1 C5 H5A 108.5 . . ? C51 C5 H5B 108.5 . . ? Al1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C11 C1 C15 119.6(2) . . ? C11 C1 P1 119.88(19) . . ? C15 C1 P1 120.51(18) . . ? C12 C11 C1 119.8(3) . . ? C12 C11 H11 120.1 . . ? C1 C11 H11 120.1 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C1 C15 C14 119.7(2) . . ? C1 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C21 C2 P1 172.2(2) . . ? C2 C21 C22 178.5(3) . . ? C21 C22 C223 110.1(2) . . ? C21 C22 C222 109.8(2) . . ? C223 C22 C222 112.3(3) . . ? C21 C22 C221 108.3(2) . . ? C223 C22 C221 108.6(3) . . ? C222 C22 C221 107.7(3) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C22 C223 H22G 109.5 . . ? C22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C31 C3 P1 132.13(19) . . ? C31 C3 Al1 112.79(17) . 3_675 ? P1 C3 Al1 114.84(12) . 3_675 ? C3 C31 C32 135.2(2) . . ? C3 C31 H31 112.4 . . ? C32 C31 H31 112.4 . . ? C31 C32 C321 110.7(2) . . ? C31 C32 C323 107.9(2) . . ? C321 C32 C323 108.1(2) . . ? C31 C32 C322 110.2(2) . . ? C321 C32 C322 111.5(2) . . ? C323 C32 C322 108.2(2) . . ? C32 C321 H32A 109.5 . . ? C32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C32 C322 H32D 109.5 . . ? C32 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? C32 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? C32 C323 H32G 109.5 . . ? C32 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? C32 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 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 C2 P1 Al1 C4 -57.30(11) . . . . ? C3 P1 Al1 C4 172.11(11) . . . . ? C1 P1 Al1 C4 52.32(12) . . . . ? C2 P1 Al1 C5 61.59(11) . . . . ? C3 P1 Al1 C5 -68.99(11) . . . . ? C1 P1 Al1 C5 171.21(11) . . . . ? C2 P1 Al1 C3 -173.90(11) . . . 3_675 ? C3 P1 Al1 C3 55.51(13) . . . 3_675 ? C1 P1 Al1 C3 -64.28(11) . . . 3_675 ? C5 Al1 C4 C41 63.0(2) . . . . ? C3 Al1 C4 C41 -79.0(2) 3_675 . . . ? P1 Al1 C4 C41 173.90(19) . . . . ? C4 Al1 C5 C51 10.2(2) . . . . ? C3 Al1 C5 C51 150.0(2) 3_675 . . . ? P1 Al1 C5 C51 -97.6(2) . . . . ? C2 P1 C1 C11 -51.5(2) . . . . ? C3 P1 C1 C11 71.3(2) . . . . ? Al1 P1 C1 C11 -162.97(17) . . . . ? C2 P1 C1 C15 128.6(2) . . . . ? C3 P1 C1 C15 -108.6(2) . . . . ? Al1 P1 C1 C15 17.1(2) . . . . ? C15 C1 C11 C12 0.5(4) . . . . ? P1 C1 C11 C12 -179.45(19) . . . . ? C1 C11 C12 C13 0.5(4) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C11 C1 C15 C14 -1.2(4) . . . . ? P1 C1 C15 C14 178.76(18) . . . . ? C13 C14 C15 C1 0.9(4) . . . . ? C3 P1 C2 C21 145.7(17) . . . . ? C1 P1 C2 C21 -101.8(17) . . . . ? Al1 P1 C2 C21 17.1(18) . . . . ? P1 C2 C21 C22 -171(9) . . . . ? C2 C21 C22 C223 -1(11) . . . . ? C2 C21 C22 C222 123(11) . . . . ? C2 C21 C22 C221 -119(11) . . . . ? C2 P1 C3 C31 -12.5(3) . . . . ? C1 P1 C3 C31 -123.6(2) . . . . ? Al1 P1 C3 C31 111.0(2) . . . . ? C2 P1 C3 Al1 173.59(11) . . . 3_675 ? C1 P1 C3 Al1 62.57(14) . . . 3_675 ? Al1 P1 C3 Al1 -62.86(13) . . . 3_675 ? P1 C3 C31 C32 4.0(4) . . . . ? Al1 C3 C31 C32 178.0(2) 3_675 . . . ? C3 C31 C32 C321 -60.5(4) . . . . ? C3 C31 C32 C323 -178.6(3) . . . . ? C3 C31 C32 C322 63.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 66.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.650 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.068 # Attachment 'Compound2.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 861399' #TrackingRef 'Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 Al2 P2' _chemical_formula_weight 608.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 10.22660(10) _cell_length_b 19.4900(2) _cell_length_c 9.66150(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.2750(10) _cell_angle_gamma 90.00 _cell_volume 1817.75(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6810 _cell_measurement_theta_min 4.5375 _cell_measurement_theta_max 71.288 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7270 _exptl_absorpt_correction_T_max 0.8758 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10480 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 68.99 _reflns_number_total 3315 _reflns_number_gt 2966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _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^)+(0.0691P)^2^+0.4069P] 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 3315 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 P1 P 0.61348(4) 0.077177(18) 0.06240(4) 0.01658(14) Uani 1 1 d . . . C1 C 0.70552(15) 0.15589(8) 0.13884(17) 0.0201(3) Uani 1 1 d . . . C11 C 0.67249(18) 0.21747(8) 0.06278(19) 0.0280(4) Uani 1 1 d . . . H11 H 0.5977 0.2191 -0.0288 0.034 Uiso 1 1 calc R . . C12 C 0.7469(2) 0.27652(9) 0.1184(2) 0.0342(4) Uani 1 1 d . . . H12 H 0.7230 0.3190 0.0656 0.041 Uiso 1 1 calc R . . C13 C 0.85515(19) 0.27445(9) 0.2492(2) 0.0332(4) Uani 1 1 d . . . H13 H 0.9062 0.3155 0.2877 0.040 Uiso 1 1 calc R . . C14 C 0.89014(19) 0.21344(9) 0.3248(2) 0.0323(4) Uani 1 1 d . . . H14 H 0.9661 0.2120 0.4154 0.039 Uiso 1 1 calc R . . C15 C 0.81593(17) 0.15435(8) 0.27037(18) 0.0262(4) Uani 1 1 d . . . H15 H 0.8406 0.1120 0.3235 0.031 Uiso 1 1 calc R . . C2 C 0.42904(15) 0.09116(7) -0.02699(16) 0.0176(3) Uani 1 1 d . . . C21 C 0.34045(16) 0.12710(8) 0.02207(17) 0.0221(3) Uani 1 1 d . . . H21 H 0.2494 0.1283 -0.0497 0.027 Uiso 1 1 calc R . . C22 C 0.34509(17) 0.16645(8) 0.16045(18) 0.0251(4) Uani 1 1 d . . . C221 C 0.3516(2) 0.24366(10) 0.1344(2) 0.0427(5) Uani 1 1 d . . . H22A H 0.4395 0.2549 0.1245 0.051 Uiso 1 1 calc R . . H22B H 0.3408 0.2683 0.2160 0.051 Uiso 1 1 calc R . . H22C H 0.2786 0.2562 0.0464 0.051 Uiso 1 1 calc R . . C222 C 0.46263(19) 0.14492(10) 0.29760(19) 0.0331(4) Uani 1 1 d . . . H22D H 0.4629 0.0959 0.3070 0.040 Uiso 1 1 calc R . . H22E H 0.4495 0.1656 0.3823 0.040 Uiso 1 1 calc R . . H22F H 0.5495 0.1597 0.2898 0.040 Uiso 1 1 calc R . . C223 C 0.2076(2) 0.15099(12) 0.1863(2) 0.0445(5) Uani 1 1 d . . . H22G H 0.1317 0.1652 0.1023 0.053 Uiso 1 1 calc R . . H22H H 0.2043 0.1755 0.2713 0.053 Uiso 1 1 calc R . . H22I H 0.2008 0.1026 0.2015 0.053 Uiso 1 1 calc R . . C3 C 0.67365(16) 0.06587(8) -0.09630(17) 0.0218(3) Uani 1 1 d . . . H3A H 0.6356 0.0240 -0.1454 0.026 Uiso 1 1 calc R . . H3B H 0.6381 0.1029 -0.1638 0.026 Uiso 1 1 calc R . . C31 C 0.83050(17) 0.06365(10) -0.0575(2) 0.0324(4) Uani 1 1 d . . . H31A H 0.8697 0.1057 -0.0100 0.039 Uiso 1 1 calc R . . H31B H 0.8537 0.0581 -0.1454 0.039 Uiso 1 1 calc R . . H31C H 0.8670 0.0258 0.0072 0.039 Uiso 1 1 calc R . . Al1 Al 0.32756(4) 0.03328(2) -0.20576(5) 0.01707(14) Uani 1 1 d . . . C4 C 0.12319(15) 0.04577(8) -0.26580(18) 0.0241(3) Uani 1 1 d . . . H4A H 0.0780 0.0053 -0.3157 0.029 Uiso 1 1 calc R . . H4B H 0.0968 0.0518 -0.1800 0.029 Uiso 1 1 calc R . . C41 C 0.07531(17) 0.10802(9) -0.3669(2) 0.0312(4) Uani 1 1 d . . . H41A H 0.1161 0.1489 -0.3152 0.037 Uiso 1 1 calc R . . H41B H -0.0238 0.1115 -0.3971 0.037 Uiso 1 1 calc R . . H41C H 0.1036 0.1026 -0.4516 0.037 Uiso 1 1 calc R . . C5 C 0.37916(16) 0.03352(8) -0.38653(17) 0.0238(3) Uani 1 1 d . . . H5A H 0.3793 0.0800 -0.4191 0.029 Uiso 1 1 calc R . . H5B H 0.4717 0.0161 -0.3632 0.029 Uiso 1 1 calc R . . C51 C 0.28255(17) -0.00913(10) -0.51273(18) 0.0296(4) Uani 1 1 d . . . H51A H 0.2973 -0.0570 -0.4899 0.036 Uiso 1 1 calc R . . H51B H 0.3020 0.0006 -0.6014 0.036 Uiso 1 1 calc R . . H51C H 0.1880 0.0024 -0.5257 0.036 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 P1 0.0170(2) 0.0148(2) 0.0144(2) -0.00007(13) 0.00036(16) -0.00072(13) C1 0.0205(7) 0.0189(8) 0.0194(8) -0.0017(6) 0.0043(6) -0.0030(6) C11 0.0314(9) 0.0229(9) 0.0236(9) 0.0037(6) 0.0008(7) -0.0018(7) C12 0.0460(11) 0.0193(8) 0.0328(10) 0.0045(7) 0.0068(8) -0.0048(7) C13 0.0412(10) 0.0238(9) 0.0327(10) -0.0065(7) 0.0097(8) -0.0129(7) C14 0.0329(9) 0.0304(9) 0.0248(9) -0.0031(7) -0.0022(7) -0.0083(7) C15 0.0282(8) 0.0210(8) 0.0230(9) 0.0013(6) -0.0003(7) -0.0031(6) C2 0.0174(7) 0.0158(7) 0.0154(8) 0.0016(5) -0.0003(6) -0.0002(5) C21 0.0214(7) 0.0206(8) 0.0196(8) -0.0001(6) 0.0004(6) 0.0022(6) C22 0.0263(8) 0.0235(8) 0.0236(9) -0.0044(6) 0.0058(7) 0.0040(6) C221 0.0612(13) 0.0244(10) 0.0428(12) -0.0046(8) 0.0178(10) 0.0097(9) C222 0.0380(10) 0.0378(10) 0.0204(9) -0.0055(7) 0.0058(7) 0.0067(8) C223 0.0349(10) 0.0638(14) 0.0372(12) -0.0150(10) 0.0153(9) -0.0036(9) C3 0.0235(8) 0.0233(8) 0.0167(8) -0.0009(6) 0.0042(6) -0.0014(6) C31 0.0252(9) 0.0443(11) 0.0279(10) 0.0040(8) 0.0089(7) 0.0002(7) Al1 0.0161(2) 0.0177(2) 0.0138(3) -0.00014(15) 0.00008(18) 0.00076(15) C4 0.0176(7) 0.0258(8) 0.0241(9) -0.0011(6) 0.0004(6) 0.0009(6) C41 0.0259(8) 0.0320(10) 0.0296(10) 0.0019(7) 0.0009(7) 0.0095(7) C5 0.0243(8) 0.0273(9) 0.0172(8) -0.0004(6) 0.0032(6) -0.0013(6) C51 0.0293(8) 0.0364(10) 0.0200(9) -0.0056(7) 0.0039(7) -0.0004(7) _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 C2 1.8173(15) . ? P1 C1 1.8236(15) . ? P1 C3 1.8442(16) . ? P1 Al1 2.5230(5) 3_655 ? C1 C11 1.390(2) . ? C1 C15 1.394(2) . ? C11 C12 1.387(2) . ? C11 H11 0.9600 . ? C12 C13 1.379(3) . ? C12 H12 0.9600 . ? C13 C14 1.380(3) . ? C13 H13 0.9600 . ? C14 C15 1.384(2) . ? C14 H14 0.9600 . ? C15 H15 0.9600 . ? C2 C21 1.349(2) . ? C2 Al1 2.0370(15) . ? C21 C22 1.528(2) . ? C21 H21 0.9600 . ? C22 C222 1.525(2) . ? C22 C221 1.531(3) . ? C22 C223 1.537(2) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C3 C31 1.523(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C31 H31A 0.9599 . ? C31 H31B 0.9599 . ? C31 H31C 0.9599 . ? Al1 C5 1.9842(16) . ? Al1 C4 1.9909(16) . ? Al1 P1 2.5230(5) 3_655 ? C4 C41 1.533(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C41 H41A 0.9599 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? C5 C51 1.536(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C51 H51A 0.9599 . ? C51 H51B 0.9599 . ? C51 H51C 0.9599 . ? 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 C2 P1 C1 112.48(7) . . ? C2 P1 C3 101.63(7) . . ? C1 P1 C3 99.66(7) . . ? C2 P1 Al1 114.29(5) . 3_655 ? C1 P1 Al1 119.84(5) . 3_655 ? C3 P1 Al1 105.64(5) . 3_655 ? C11 C1 C15 118.88(14) . . ? C11 C1 P1 120.64(12) . . ? C15 C1 P1 120.37(12) . . ? C12 C11 C1 120.37(15) . . ? C12 C11 H11 119.8 . . ? C1 C11 H11 119.8 . . ? C13 C12 C11 120.19(16) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.00(16) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.15(16) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C1 120.41(15) . . ? C14 C15 H15 119.8 . . ? C1 C15 H15 119.8 . . ? C21 C2 P1 128.53(12) . . ? C21 C2 Al1 111.86(11) . . ? P1 C2 Al1 118.57(8) . . ? C2 C21 C22 137.51(14) . . ? C2 C21 H21 111.2 . . ? C22 C21 H21 111.2 . . ? C222 C22 C21 114.21(13) . . ? C222 C22 C221 110.41(15) . . ? C21 C22 C221 109.87(15) . . ? C222 C22 C223 107.81(15) . . ? C21 C22 C223 106.13(14) . . ? C221 C22 C223 108.14(16) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C22 C223 H22G 109.5 . . ? C22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C31 C3 P1 114.36(11) . . ? C31 C3 H3A 108.7 . . ? P1 C3 H3A 108.7 . . ? C31 C3 H3B 108.7 . . ? P1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 Al1 C4 107.57(7) . . ? C5 Al1 C2 122.41(7) . . ? C4 Al1 C2 111.80(7) . . ? C5 Al1 P1 113.60(5) . 3_655 ? C4 Al1 P1 107.57(5) . 3_655 ? C2 Al1 P1 92.55(4) . 3_655 ? C41 C4 Al1 111.48(11) . . ? C41 C4 H4A 109.3 . . ? Al1 C4 H4A 109.3 . . ? C41 C4 H4B 109.3 . . ? Al1 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C51 C5 Al1 114.15(11) . . ? C51 C5 H5A 108.7 . . ? Al1 C5 H5A 108.7 . . ? C51 C5 H5B 108.7 . . ? Al1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 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 C2 P1 C1 C11 -40.04(16) . . . . ? C3 P1 C1 C11 66.92(15) . . . . ? Al1 P1 C1 C11 -178.68(12) 3_655 . . . ? C2 P1 C1 C15 143.93(13) . . . . ? C3 P1 C1 C15 -109.10(14) . . . . ? Al1 P1 C1 C15 5.30(16) 3_655 . . . ? C15 C1 C11 C12 -1.0(3) . . . . ? P1 C1 C11 C12 -177.12(14) . . . . ? C1 C11 C12 C13 0.5(3) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C1 0.1(3) . . . . ? C11 C1 C15 C14 0.7(3) . . . . ? P1 C1 C15 C14 176.83(13) . . . . ? C1 P1 C2 C21 -46.17(17) . . . . ? C3 P1 C2 C21 -151.87(15) . . . . ? Al1 P1 C2 C21 94.87(15) 3_655 . . . ? C1 P1 C2 Al1 146.50(8) . . . . ? C3 P1 C2 Al1 40.80(10) . . . . ? Al1 P1 C2 Al1 -72.46(8) 3_655 . . . ? P1 C2 C21 C22 -3.2(3) . . . . ? Al1 C2 C21 C22 164.85(17) . . . . ? C2 C21 C22 C222 -22.8(3) . . . . ? C2 C21 C22 C221 101.9(2) . . . . ? C2 C21 C22 C223 -141.4(2) . . . . ? C2 P1 C3 C31 171.25(12) . . . . ? C1 P1 C3 C31 55.71(13) . . . . ? Al1 P1 C3 C31 -69.17(12) 3_655 . . . ? C21 C2 Al1 C5 130.91(12) . . . . ? P1 C2 Al1 C5 -59.74(11) . . . . ? C21 C2 Al1 C4 1.19(14) . . . . ? P1 C2 Al1 C4 170.54(8) . . . . ? C21 C2 Al1 P1 -108.89(11) . . . 3_655 ? P1 C2 Al1 P1 60.46(8) . . . 3_655 ? C5 Al1 C4 C41 -51.57(13) . . . . ? C2 Al1 C4 C41 85.50(13) . . . . ? P1 Al1 C4 C41 -174.31(10) 3_655 . . . ? C4 Al1 C5 C51 -43.88(14) . . . . ? C2 Al1 C5 C51 -175.36(11) . . . . ? P1 Al1 C5 C51 75.07(12) 3_655 . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 68.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.553 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.053 # Attachment 'Compound3.cif' data_sad1 _database_code_depnum_ccdc_archive 'CCDC 861400' #TrackingRef 'Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Al2 P2' _chemical_formula_weight 692.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.44900(10) _cell_length_b 15.3975(2) _cell_length_c 13.6643(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.3260(10) _cell_angle_gamma 90.00 _cell_volume 2109.78(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5940 _cell_measurement_theta_min 4.429 _cell_measurement_theta_max 71,3725 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8629 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10998 _diffrn_reflns_av_R_equivalents 0.1898 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.43 _diffrn_reflns_theta_max 61.48 _reflns_number_total 3099 _reflns_number_gt 2673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _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^)+(0.0837P)^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 3099 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.009 _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 0.39669(5) 0.01488(3) 0.35145(4) 0.0154(2) Uani 1 1 d . . . C1 C 0.3349(2) 0.03367(13) 0.21274(15) 0.0191(5) Uani 1 1 d . . . C11 C 0.2249(2) 0.08884(13) 0.17441(16) 0.0230(5) Uani 1 1 d . . . C111 C 0.1635(2) 0.14184(17) 0.24227(18) 0.0348(6) Uani 1 1 d . . . H11A H 0.1016 0.1827 0.2016 0.042 Uiso 1 1 calc R . . H11B H 0.2323 0.1725 0.2916 0.042 Uiso 1 1 calc R . . H11C H 0.1175 0.1040 0.2769 0.042 Uiso 1 1 calc R . . C12 C 0.1662(2) 0.09414(14) 0.07002(17) 0.0257(5) Uani 1 1 d . . . H12 H 0.0906 0.1315 0.0450 0.031 Uiso 1 1 calc R . . C13 C 0.2131(2) 0.04727(14) 0.00042(17) 0.0243(5) Uani 1 1 d . . . C131 C 0.1430(2) 0.05066(17) -0.11150(17) 0.0327(6) Uani 1 1 d . . . H13A H 0.0992 -0.0038 -0.1328 0.039 Uiso 1 1 calc R . . H13B H 0.2068 0.0615 -0.1487 0.039 Uiso 1 1 calc R . . H13C H 0.0781 0.0965 -0.1246 0.039 Uiso 1 1 calc R . . C14 C 0.3246(2) -0.00475(13) 0.03919(16) 0.0223(5) Uani 1 1 d . . . H14 H 0.3610 -0.0358 -0.0078 0.027 Uiso 1 1 calc R . . C15 C 0.3854(2) -0.01377(13) 0.14281(16) 0.0204(5) Uani 1 1 d . . . C151 C 0.5001(2) -0.07761(15) 0.17380(17) 0.0262(5) Uani 1 1 d . . . H15A H 0.4668 -0.1336 0.1856 0.031 Uiso 1 1 calc R . . H15B H 0.5634 -0.0577 0.2351 0.031 Uiso 1 1 calc R . . H15C H 0.5428 -0.0820 0.1203 0.031 Uiso 1 1 calc R . . C2 C 0.5767(2) 0.00745(12) 0.40067(15) 0.0151(4) Uani 1 1 d . . . C21 C 0.6675(2) 0.06646(13) 0.38984(15) 0.0189(5) Uani 1 1 d . . . H21 H 0.7557 0.0502 0.4291 0.023 Uiso 1 1 calc R . . C22 C 0.6700(2) 0.15180(14) 0.33296(17) 0.0255(5) Uani 1 1 d . . . C221 C 0.5367(2) 0.19672(15) 0.2905(2) 0.0351(6) Uani 1 1 d . . . H22A H 0.4815 0.1625 0.2361 0.042 Uiso 1 1 calc R . . H22B H 0.5506 0.2530 0.2650 0.042 Uiso 1 1 calc R . . H22C H 0.4936 0.2031 0.3435 0.042 Uiso 1 1 calc R . . C222 C 0.7313(3) 0.13183(18) 0.2465(2) 0.0516(8) Uani 1 1 d . . . H22D H 0.6712 0.0960 0.1966 0.062 Uiso 1 1 calc R . . H22E H 0.8142 0.1018 0.2732 0.062 Uiso 1 1 calc R . . H22F H 0.7469 0.1851 0.2152 0.062 Uiso 1 1 calc R . . C223 C 0.7641(3) 0.21286(16) 0.4086(2) 0.0405(7) Uani 1 1 d . . . H22G H 0.7782 0.2646 0.3737 0.049 Uiso 1 1 calc R . . H22H H 0.8479 0.1843 0.4373 0.049 Uiso 1 1 calc R . . H22I H 0.7251 0.2280 0.4621 0.049 Uiso 1 1 calc R . . C3 C 0.3357(2) -0.09671(13) 0.35442(16) 0.0206(5) Uani 1 1 d . . . H3A H 0.3813 -0.1342 0.3191 0.025 Uiso 1 1 calc R . . H3B H 0.3566 -0.1159 0.4240 0.025 Uiso 1 1 calc R . . C31 C 0.1855(2) -0.10467(15) 0.3057(2) 0.0328(6) Uani 1 1 d . . . H31A H 0.1394 -0.0661 0.3394 0.039 Uiso 1 1 calc R . . H31B H 0.1579 -0.1633 0.3122 0.039 Uiso 1 1 calc R . . H31C H 0.1647 -0.0895 0.2348 0.039 Uiso 1 1 calc R . . Al1 Al 0.33394(5) 0.08801(4) 0.49899(4) 0.0157(2) Uani 1 1 d . . . C4 C 0.4034(2) 0.20903(13) 0.52608(18) 0.0269(5) Uani 1 1 d . . . H4A H 0.4293 0.2180 0.5985 0.032 Uiso 1 1 calc R . . H4B H 0.4827 0.2134 0.5041 0.032 Uiso 1 1 calc R . . C41 C 0.3098(3) 0.28367(15) 0.4764(2) 0.0376(6) Uani 1 1 d . . . H41A H 0.3008 0.2849 0.4046 0.045 Uiso 1 1 calc R . . H41B H 0.3464 0.3378 0.5064 0.045 Uiso 1 1 calc R . . H41C H 0.2239 0.2749 0.4873 0.045 Uiso 1 1 calc R . . C5 C 0.1401(2) 0.09126(14) 0.48756(17) 0.0224(5) Uani 1 1 d . . . H5A H 0.0965 0.1328 0.4367 0.027 Uiso 1 1 calc R . . H5B H 0.1012 0.0353 0.4673 0.027 Uiso 1 1 calc R . . C51 C 0.1211(3) 0.11659(16) 0.59126(19) 0.0333(6) Uani 1 1 d . . . H51A H 0.1460 0.0687 0.6377 0.040 Uiso 1 1 calc R . . H51B H 0.0293 0.1311 0.5829 0.040 Uiso 1 1 calc R . . H51C H 0.1761 0.1658 0.6180 0.040 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 P1 0.0145(3) 0.0147(3) 0.0172(3) 0.00085(18) 0.0049(2) 0.00164(19) C1 0.0169(10) 0.0206(10) 0.0201(11) 0.0021(8) 0.0058(9) 0.0005(8) C11 0.0233(11) 0.0223(11) 0.0236(13) 0.0043(8) 0.0070(10) 0.0033(9) C111 0.0343(13) 0.0418(15) 0.0277(13) 0.0055(10) 0.0077(10) 0.0226(11) C12 0.0216(11) 0.0262(12) 0.0274(13) 0.0080(9) 0.0037(9) 0.0037(9) C13 0.0243(11) 0.0232(12) 0.0232(12) 0.0038(9) 0.0032(9) -0.0046(9) C131 0.0350(13) 0.0361(14) 0.0225(13) 0.0031(10) 0.0009(10) 0.0005(11) C14 0.0258(11) 0.0219(11) 0.0200(12) -0.0005(8) 0.0075(9) -0.0027(9) C15 0.0205(10) 0.0189(11) 0.0220(12) -0.0005(8) 0.0066(9) -0.0012(8) C151 0.0277(11) 0.0290(12) 0.0225(12) -0.0026(9) 0.0081(10) 0.0071(10) C2 0.0160(10) 0.0129(10) 0.0162(11) -0.0009(7) 0.0041(8) 0.0012(8) C21 0.0200(10) 0.0174(10) 0.0198(11) 0.0008(8) 0.0067(9) 0.0012(8) C22 0.0274(11) 0.0183(11) 0.0339(13) 0.0065(9) 0.0139(10) -0.0009(9) C221 0.0324(12) 0.0202(12) 0.0505(16) 0.0136(10) 0.0078(11) 0.0001(10) C222 0.077(2) 0.0344(15) 0.0615(19) 0.0176(13) 0.0497(17) 0.0102(14) C223 0.0332(13) 0.0202(13) 0.0635(18) 0.0094(11) 0.0061(12) -0.0038(10) C3 0.0219(11) 0.0178(10) 0.0226(12) -0.0025(8) 0.0071(9) -0.0020(8) C31 0.0239(12) 0.0302(13) 0.0445(15) -0.0055(10) 0.0097(11) -0.0073(10) Al1 0.0147(3) 0.0126(3) 0.0203(4) 0.0006(2) 0.0060(3) 0.0018(2) C4 0.0252(11) 0.0169(11) 0.0373(14) -0.0012(9) 0.0067(10) 0.0011(9) C41 0.0378(13) 0.0153(11) 0.0565(17) 0.0017(11) 0.0081(12) 0.0027(10) C5 0.0178(10) 0.0226(11) 0.0275(12) 0.0021(8) 0.0076(9) 0.0029(8) C51 0.0324(12) 0.0357(13) 0.0373(14) -0.0008(10) 0.0185(11) 0.0080(11) _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 C2 1.815(2) . ? P1 C3 1.837(2) . ? P1 C1 1.845(2) . ? P1 Al1 2.5505(7) . ? C1 C11 1.407(3) . ? C1 C15 1.417(3) . ? C11 C12 1.388(3) . ? C11 C111 1.507(3) . ? C111 H11A 0.9599 . ? C111 H11B 0.9599 . ? C111 H11C 0.9599 . ? C12 C13 1.388(3) . ? C12 H12 0.9600 . ? C13 C14 1.390(3) . ? C13 C131 1.499(3) . ? C131 H13A 0.9599 . ? C131 H13B 0.9599 . ? C131 H13C 0.9599 . ? C14 C15 1.386(3) . ? C14 H14 0.9600 . ? C15 C151 1.516(3) . ? C151 H15A 0.9599 . ? C151 H15B 0.9599 . ? C151 H15C 0.9599 . ? C2 C21 1.351(3) . ? C2 Al1 2.048(2) 3_656 ? C21 C22 1.531(3) . ? C21 H21 0.9600 . ? C22 C221 1.517(3) . ? C22 C222 1.525(4) . ? C22 C223 1.532(3) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C3 C31 1.528(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C31 H31A 0.9599 . ? C31 H31B 0.9599 . ? C31 H31C 0.9599 . ? Al1 C5 1.988(2) . ? Al1 C4 1.996(2) . ? Al1 C2 2.048(2) 3_656 ? C4 C41 1.538(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C41 H41A 0.9599 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? C5 C51 1.536(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C51 H51A 0.9599 . ? C51 H51B 0.9599 . ? C51 H51C 0.9599 . ? 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 C2 P1 C3 105.24(9) . . ? C2 P1 C1 114.67(9) . . ? C3 P1 C1 98.39(10) . . ? C2 P1 Al1 101.83(6) . . ? C3 P1 Al1 103.15(7) . . ? C1 P1 Al1 130.49(7) . . ? C11 C1 C15 118.71(19) . . ? C11 C1 P1 119.36(16) . . ? C15 C1 P1 121.52(16) . . ? C12 C11 C1 119.8(2) . . ? C12 C11 C111 117.34(19) . . ? C1 C11 C111 122.85(19) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C11 C12 C13 122.3(2) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 117.2(2) . . ? C14 C13 C131 121.7(2) . . ? C12 C13 C131 121.0(2) . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C15 C14 C13 122.8(2) . . ? C15 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C14 C15 C1 119.10(19) . . ? C14 C15 C151 116.73(19) . . ? C1 C15 C151 124.12(19) . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C21 C2 P1 127.12(16) . . ? C21 C2 Al1 110.74(15) . 3_656 ? P1 C2 Al1 121.56(10) . 3_656 ? C2 C21 C22 138.21(19) . . ? C2 C21 H21 110.9 . . ? C22 C21 H21 110.9 . . ? C221 C22 C222 109.6(2) . . ? C221 C22 C21 116.14(18) . . ? C222 C22 C21 106.93(18) . . ? C221 C22 C223 108.93(19) . . ? C222 C22 C223 108.5(2) . . ? C21 C22 C223 106.49(18) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C22 C223 H22G 109.5 . . ? C22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C31 C3 P1 112.69(15) . . ? C31 C3 H3A 109.1 . . ? P1 C3 H3A 109.1 . . ? C31 C3 H3B 109.1 . . ? P1 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 Al1 C4 107.48(9) . . ? C5 Al1 C2 109.48(9) . 3_656 ? C4 Al1 C2 118.19(9) . 3_656 ? C5 Al1 P1 115.58(7) . . ? C4 Al1 P1 113.44(7) . . ? C2 Al1 P1 92.42(6) 3_656 . ? C41 C4 Al1 117.57(16) . . ? C41 C4 H4A 107.9 . . ? Al1 C4 H4A 107.9 . . ? C41 C4 H4B 107.9 . . ? Al1 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C51 C5 Al1 109.10(16) . . ? C51 C5 H5A 109.9 . . ? Al1 C5 H5A 109.9 . . ? C51 C5 H5B 109.9 . . ? Al1 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 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 C2 P1 C1 C11 -142.10(16) . . . . ? C3 P1 C1 C11 106.79(17) . . . . ? Al1 P1 C1 C11 -8.6(2) . . . . ? C2 P1 C1 C15 45.4(2) . . . . ? C3 P1 C1 C15 -65.75(19) . . . . ? Al1 P1 C1 C15 178.88(13) . . . . ? C15 C1 C11 C12 1.6(3) . . . . ? P1 C1 C11 C12 -171.17(16) . . . . ? C15 C1 C11 C111 179.8(2) . . . . ? P1 C1 C11 C111 7.1(3) . . . . ? C1 C11 C12 C13 -0.7(3) . . . . ? C111 C11 C12 C13 -179.1(2) . . . . ? C11 C12 C13 C14 -1.3(3) . . . . ? C11 C12 C13 C131 176.6(2) . . . . ? C12 C13 C14 C15 2.7(3) . . . . ? C131 C13 C14 C15 -175.3(2) . . . . ? C13 C14 C15 C1 -1.8(3) . . . . ? C13 C14 C15 C151 175.9(2) . . . . ? C11 C1 C15 C14 -0.3(3) . . . . ? P1 C1 C15 C14 172.25(15) . . . . ? C11 C1 C15 C151 -177.9(2) . . . . ? P1 C1 C15 C151 -5.3(3) . . . . ? C3 P1 C2 C21 161.90(18) . . . . ? C1 P1 C2 C21 54.9(2) . . . . ? Al1 P1 C2 C21 -90.76(18) . . . . ? C3 P1 C2 Al1 -27.67(13) . . . 3_656 ? C1 P1 C2 Al1 -134.62(11) . . . 3_656 ? Al1 P1 C2 Al1 79.67(10) . . . 3_656 ? P1 C2 C21 C22 -6.2(4) . . . . ? Al1 C2 C21 C22 -177.5(2) 3_656 . . . ? C2 C21 C22 C221 15.1(4) . . . . ? C2 C21 C22 C222 -107.6(3) . . . . ? C2 C21 C22 C223 136.6(3) . . . . ? C2 P1 C3 C31 -174.45(15) . . . . ? C1 P1 C3 C31 -55.93(17) . . . . ? Al1 P1 C3 C31 79.18(16) . . . . ? C2 P1 Al1 C5 -170.00(9) . . . . ? C3 P1 Al1 C5 -61.05(10) . . . . ? C1 P1 Al1 C5 52.31(12) . . . . ? C2 P1 Al1 C4 65.22(10) . . . . ? C3 P1 Al1 C4 174.17(10) . . . . ? C1 P1 Al1 C4 -72.47(12) . . . . ? C2 P1 Al1 C2 -57.03(10) . . . 3_656 ? C3 P1 Al1 C2 51.92(9) . . . 3_656 ? C1 P1 Al1 C2 165.28(10) . . . 3_656 ? C5 Al1 C4 C41 -34.1(2) . . . . ? C2 Al1 C4 C41 -158.53(17) 3_656 . . . ? P1 Al1 C4 C41 94.93(18) . . . . ? C4 Al1 C5 C51 -65.63(17) . . . . ? C2 Al1 C5 C51 63.91(17) 3_656 . . . ? P1 Al1 C5 C51 166.55(13) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 61.48 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.571 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.081 # Attachment 'Compound4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 861401' #TrackingRef 'Compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H76 Al2 P2' _chemical_formula_weight 624.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 9.9285(3) _cell_length_b 10.7738(4) _cell_length_c 21.3657(7) _cell_angle_alpha 79.662(2) _cell_angle_beta 84.097(2) _cell_angle_gamma 66.1080(10) _cell_volume 2054.52(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5997 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 63.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5769 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCd area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10609 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 63.00 _reflns_number_total 5997 _reflns_number_gt 5474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _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^)+(0.0460P)^2^+1.8568P] 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 5997 _refine_ls_number_parameters 435 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.74838(18) 0.6691(2) 0.20992(7) 0.0194(4) Uani 0.698(9) 1 d PU A 1 H1A H 0.8364 0.5432 0.2054 0.050 Uiso 0.70 1 d P A 1 P1A P 0.7039(10) 0.7331(13) 0.20747(17) 0.0465(19) Uani 0.302(9) 1 d PU A 2 H1AA H 0.5971 0.8942 0.1913 0.050 Uiso 0.30 1 d P A 2 C1 C 0.5922(3) 0.6747(2) 0.16457(11) 0.0299(5) Uani 1 1 d D . . C11 C 0.6362(3) 0.6678(4) 0.09447(13) 0.0522(8) Uani 1 1 d D A . H11A H 0.5560 0.6649 0.0723 0.078 Uiso 1 1 calc R . . H11B H 0.7254 0.5848 0.0905 0.078 Uiso 1 1 calc R . . H11C H 0.6555 0.7490 0.0755 0.078 Uiso 1 1 calc R . . C12 C 0.5704(4) 0.5455(3) 0.19586(16) 0.0561(8) Uani 1 1 d D A . H12A H 0.5442 0.5505 0.2411 0.084 Uiso 1 1 calc R . . H12B H 0.6620 0.4650 0.1915 0.084 Uiso 1 1 calc R . . H12C H 0.4911 0.5379 0.1751 0.084 Uiso 1 1 calc R . . C13 C 0.4504(3) 0.8002(3) 0.17014(15) 0.0522(8) Uani 1 1 d D A . H13A H 0.3751 0.7980 0.1446 0.078 Uiso 1 1 calc R . . H13B H 0.4686 0.8835 0.1546 0.078 Uiso 1 1 calc R . . H13C H 0.4160 0.8001 0.2148 0.078 Uiso 1 1 calc R . . P2 P 0.6196(3) 0.9953(3) 0.26943(6) 0.0288(7) Uani 0.698(9) 1 d PU A 3 H2A H 0.5333 0.9329 0.2589 0.050 Uiso 0.70 1 d P A 3 P2A P 0.6584(4) 1.0356(5) 0.27593(13) 0.0190(10) Uani 0.302(9) 1 d PU A 4 H2AA H 0.6993 1.1142 0.2896 0.050 Uiso 0.30 1 d P A 4 C2 C 0.4522(3) 1.1435(2) 0.28947(11) 0.0322(6) Uani 1 1 d D . . C21 C 0.3299(5) 1.1686(9) 0.2457(3) 0.0453(18) Uani 0.587(13) 1 d PDU A 3 H21A H 0.2446 1.2473 0.2552 0.054 Uiso 0.587(13) 1 calc PR A 3 H21B H 0.3055 1.0896 0.2521 0.054 Uiso 0.587(13) 1 calc PR A 3 H21C H 0.3622 1.1849 0.2023 0.054 Uiso 0.587(13) 1 calc PR A 3 C22 C 0.4856(9) 1.2764(6) 0.2763(4) 0.0404(16) Uani 0.587(13) 1 d PDU A 3 H22A H 0.5123 1.2934 0.2321 0.048 Uiso 0.587(13) 1 calc PR A 3 H22B H 0.5655 1.2640 0.3018 0.048 Uiso 0.587(13) 1 calc PR A 3 H22C H 0.3995 1.3532 0.2869 0.048 Uiso 0.587(13) 1 calc PR A 3 C23 C 0.400(2) 1.1228(18) 0.3589(4) 0.038(3) Uani 0.587(13) 1 d PDU A 3 H23A H 0.4776 1.1069 0.3864 0.046 Uiso 0.587(13) 1 calc PR A 3 H23B H 0.3729 1.0450 0.3666 0.046 Uiso 0.587(13) 1 calc PR A 3 H23C H 0.3157 1.2034 0.3674 0.046 Uiso 0.587(13) 1 calc PR A 3 C21A C 0.3550(10) 1.0822(14) 0.2613(4) 0.044(3) Uani 0.413(13) 1 d PDU A 4 H21D H 0.2526 1.1341 0.2704 0.052 Uiso 0.413(13) 1 calc PR A 4 H21E H 0.3811 0.9881 0.2802 0.052 Uiso 0.413(13) 1 calc PR A 4 H21F H 0.3723 1.0873 0.2160 0.052 Uiso 0.413(13) 1 calc PR A 4 C22A C 0.4257(13) 1.2830(8) 0.2551(5) 0.045(3) Uani 0.413(13) 1 d PDU A 4 H22D H 0.3219 1.3387 0.2557 0.054 Uiso 0.413(13) 1 calc PR A 4 H22E H 0.4618 1.2773 0.2118 0.054 Uiso 0.413(13) 1 calc PR A 4 H22F H 0.4763 1.3235 0.2754 0.054 Uiso 0.413(13) 1 calc PR A 4 C23A C 0.416(3) 1.139(3) 0.3599(5) 0.039(4) Uani 0.413(13) 1 d PDU A 4 H23D H 0.4682 1.1823 0.3777 0.046 Uiso 0.413(13) 1 calc PR A 4 H23E H 0.4456 1.0458 0.3800 0.046 Uiso 0.413(13) 1 calc PR A 4 H23F H 0.3121 1.1878 0.3667 0.046 Uiso 0.413(13) 1 calc PR A 4 Al1 Al 0.72335(7) 0.67982(7) 0.32942(3) 0.02930(18) Uani 1 1 d . . . C3 C 0.5482(3) 0.6524(3) 0.37878(12) 0.0406(6) Uani 1 1 d . A . C31 C 0.3966(3) 0.7391(4) 0.35123(17) 0.0643(9) Uani 1 1 d . . . H31A H 0.3201 0.7293 0.3821 0.096 Uiso 1 1 calc R A . H31B H 0.3892 0.7081 0.3118 0.096 Uiso 1 1 calc R . . H31C H 0.3833 0.8358 0.3421 0.096 Uiso 1 1 calc R . . C32 C 0.5639(4) 0.5025(3) 0.38956(15) 0.0565(8) Uani 1 1 d . . . H32A H 0.6542 0.4442 0.4124 0.085 Uiso 1 1 calc R A . H32B H 0.5688 0.4726 0.3484 0.085 Uiso 1 1 calc R . . H32C H 0.4786 0.4949 0.4148 0.085 Uiso 1 1 calc R . . C33 C 0.5477(4) 0.6922(3) 0.44444(13) 0.0564(8) Uani 1 1 d . . . H33A H 0.5325 0.7892 0.4394 0.085 Uiso 1 1 calc R A . H33B H 0.6423 0.6352 0.4642 0.085 Uiso 1 1 calc R . . H33C H 0.4679 0.6777 0.4715 0.085 Uiso 1 1 calc R . . C4 C 0.9224(3) 0.5237(3) 0.35053(11) 0.0361(6) Uani 1 1 d . A . C41 C 0.9375(3) 0.3915(3) 0.32684(14) 0.0516(7) Uani 1 1 d . . . H41A H 0.9341 0.4077 0.2803 0.077 Uiso 1 1 calc R A . H41B H 0.8562 0.3655 0.3451 0.077 Uiso 1 1 calc R . . H41C H 1.0316 0.3173 0.3401 0.077 Uiso 1 1 calc R . . C42 C 0.9484(3) 0.4827(3) 0.42239(13) 0.0518(8) Uani 1 1 d . . . H42A H 1.0459 0.4083 0.4295 0.078 Uiso 1 1 calc R A . H42B H 0.8725 0.4516 0.4432 0.078 Uiso 1 1 calc R . . H42C H 0.9433 0.5622 0.4403 0.078 Uiso 1 1 calc R . . C43 C 1.0473(3) 0.5646(3) 0.31958(14) 0.0487(7) Uani 1 1 d . . . H43A H 1.0438 0.6447 0.3364 0.073 Uiso 1 1 calc R A . H43B H 1.0361 0.5873 0.2734 0.073 Uiso 1 1 calc R . . H43C H 1.1422 0.4879 0.3291 0.073 Uiso 1 1 calc R . . Al2 Al 0.77522(7) 0.98873(7) 0.16489(3) 0.02883(18) Uani 1 1 d . . . C5 C 0.6593(3) 1.1101(3) 0.08768(11) 0.0346(6) Uani 1 1 d . A . C51 C 0.5100(3) 1.1062(4) 0.07985(15) 0.0635(10) Uani 1 1 d . . . H51A H 0.4650 1.1680 0.0413 0.095 Uiso 1 1 calc R A . H51B H 0.4454 1.1357 0.1169 0.095 Uiso 1 1 calc R . . H51C H 0.5236 1.0123 0.0763 0.095 Uiso 1 1 calc R . . C52 C 0.7546(3) 1.0571(3) 0.02903(12) 0.0448(7) Uani 1 1 d . . . H52A H 0.7652 0.9630 0.0282 0.067 Uiso 1 1 calc R A . H52B H 0.8521 1.0584 0.0313 0.067 Uiso 1 1 calc R . . H52C H 0.7072 1.1163 -0.0097 0.067 Uiso 1 1 calc R . . C53 C 0.6368(3) 1.2602(3) 0.08377(13) 0.0491(7) Uani 1 1 d . . . H53A H 0.5890 1.3128 0.0440 0.074 Uiso 1 1 calc R A . H53B H 0.7325 1.2659 0.0848 0.074 Uiso 1 1 calc R . . H53C H 0.5744 1.2982 0.1200 0.074 Uiso 1 1 calc R . . C6 C 0.9485(3) 1.0304(3) 0.18306(11) 0.0324(5) Uani 1 1 d . A . C61 C 1.0529(3) 1.0371(3) 0.12553(12) 0.0393(6) Uani 1 1 d . . . H61A H 1.1329 1.0574 0.1383 0.059 Uiso 1 1 calc R A . H61B H 0.9981 1.1095 0.0918 0.059 Uiso 1 1 calc R . . H61C H 1.0944 0.9486 0.1098 0.059 Uiso 1 1 calc R . . C62 C 0.8970(3) 1.1697(3) 0.20656(15) 0.0539(8) Uani 1 1 d . . . H62A H 0.8262 1.1735 0.2424 0.081 Uiso 1 1 calc R A . H62B H 0.8500 1.2437 0.1719 0.081 Uiso 1 1 calc R . . H62C H 0.9821 1.1808 0.2204 0.081 Uiso 1 1 calc R . . C63 C 1.0411(3) 0.9183(3) 0.23495(12) 0.0408(6) Uani 1 1 d . . . H63A H 1.0828 0.8297 0.2193 0.061 Uiso 1 1 calc R A . H63B H 0.9784 0.9126 0.2730 0.061 Uiso 1 1 calc R . . H63C H 1.1211 0.9412 0.2457 0.061 Uiso 1 1 calc R . . C71 C 0.8305(2) 0.7858(2) 0.16346(10) 0.0280(5) Uani 1 1 d . A . C72 C 0.9524(3) 0.7394(2) 0.12574(11) 0.0292(5) Uani 1 1 d . . . H72 H 0.9799 0.8133 0.1075 0.035 Uiso 1 1 calc R A . C73 C 1.0610(3) 0.6070(3) 0.10265(11) 0.0325(5) Uani 1 1 d . A . C731 C 1.0472(3) 0.4713(3) 0.12919(13) 0.0473(7) Uani 1 1 d . . . H73D H 1.0615 0.4511 0.1752 0.071 Uiso 1 1 calc R A . H73E H 1.1223 0.3975 0.1086 0.071 Uiso 1 1 calc R . . H73F H 0.9490 0.4781 0.1209 0.071 Uiso 1 1 calc R . . C732 C 1.0502(3) 0.6315(3) 0.02990(12) 0.0456(7) Uani 1 1 d . . . H73A H 1.1259 0.5533 0.0122 0.068 Uiso 1 1 calc R A . H73B H 1.0651 0.7155 0.0120 0.068 Uiso 1 1 calc R . . H73C H 0.9525 0.6413 0.0190 0.068 Uiso 1 1 calc R . . C733 C 1.2148(3) 0.5913(3) 0.11830(15) 0.0509(7) Uani 1 1 d . . . H73G H 1.2242 0.5741 0.1646 0.076 Uiso 1 1 calc R A . H73H H 1.2291 0.6758 0.1006 0.076 Uiso 1 1 calc R . . H73I H 1.2896 0.5140 0.0997 0.076 Uiso 1 1 calc R . . C81 C 0.7170(2) 0.8690(2) 0.33360(10) 0.0282(5) Uani 1 1 d . A . C82 C 0.7843(3) 0.8624(3) 0.38616(11) 0.0316(5) Uani 1 1 d . . . H82 H 0.8185 0.7712 0.4084 0.038 Uiso 1 1 calc R A . C83 C 0.8241(3) 0.9516(3) 0.42210(12) 0.0368(6) Uani 1 1 d . A . C831 C 0.7451(3) 0.9515(3) 0.48756(13) 0.0514(8) Uani 1 1 d . . . H83A H 0.6384 0.9984 0.4824 0.077 Uiso 1 1 calc R A . H83B H 0.7772 0.9996 0.5139 0.077 Uiso 1 1 calc R . . H83C H 0.7691 0.8566 0.5083 0.077 Uiso 1 1 calc R . . C832 C 0.9908(3) 0.8794(4) 0.43158(16) 0.0618(9) Uani 1 1 d . . . H83G H 1.0149 0.7844 0.4522 0.093 Uiso 1 1 calc R A . H83H H 1.0208 0.9279 0.4585 0.093 Uiso 1 1 calc R . . H83I H 1.0432 0.8799 0.3901 0.093 Uiso 1 1 calc R . . C833 C 0.7898(4) 1.0988(3) 0.39142(16) 0.0671(10) Uani 1 1 d . . . H83D H 0.8335 1.1001 0.3482 0.101 Uiso 1 1 calc R A . H83E H 0.8310 1.1419 0.4166 0.101 Uiso 1 1 calc R . . H83F H 0.6828 1.1497 0.3897 0.101 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 P1 0.0181(6) 0.0161(8) 0.0191(5) -0.0002(5) -0.0017(4) -0.0024(6) P1A 0.055(3) 0.080(5) 0.0256(14) -0.005(2) -0.0036(16) -0.049(4) C1 0.0277(12) 0.0313(13) 0.0333(13) -0.0050(10) -0.0080(10) -0.0125(10) C11 0.0489(17) 0.080(2) 0.0364(15) -0.0167(15) -0.0087(12) -0.0299(16) C12 0.075(2) 0.0412(17) 0.061(2) -0.0009(15) -0.0220(16) -0.0306(16) C13 0.0396(16) 0.0525(18) 0.0545(18) -0.0097(15) -0.0103(13) -0.0053(14) P2 0.0259(8) 0.0271(8) 0.0229(5) -0.0014(5) 0.0047(4) -0.0019(7) P2A 0.0179(13) 0.0220(14) 0.0205(11) -0.0033(9) 0.0007(8) -0.0117(11) C2 0.0261(12) 0.0311(13) 0.0291(13) -0.0016(10) 0.0053(9) -0.0034(11) C21 0.034(3) 0.038(4) 0.050(3) -0.009(3) -0.001(2) 0.001(3) C22 0.043(4) 0.023(3) 0.039(4) 0.000(2) 0.007(3) 0.000(3) C23 0.040(7) 0.035(5) 0.029(5) -0.012(3) 0.016(3) -0.005(4) C21A 0.038(4) 0.052(7) 0.044(4) -0.013(4) 0.006(3) -0.020(4) C22A 0.042(5) 0.032(4) 0.038(5) 0.005(4) 0.002(4) 0.002(4) C23A 0.024(6) 0.033(8) 0.048(8) 0.002(5) 0.005(5) -0.004(5) Al1 0.0292(4) 0.0339(4) 0.0210(3) -0.0009(3) 0.0015(3) -0.0105(3) C3 0.0426(15) 0.0375(15) 0.0357(14) 0.0040(12) 0.0093(11) -0.0160(12) C31 0.0411(17) 0.064(2) 0.074(2) 0.0121(18) 0.0087(15) -0.0187(16) C32 0.066(2) 0.0533(19) 0.0526(18) -0.0010(15) 0.0123(15) -0.0328(17) C33 0.068(2) 0.0555(19) 0.0412(16) -0.0098(14) 0.0259(14) -0.0257(17) C4 0.0372(14) 0.0341(14) 0.0296(13) -0.0082(11) -0.0015(10) -0.0051(11) C41 0.0536(18) 0.0434(17) 0.0524(18) -0.0170(14) 0.0003(14) -0.0103(14) C42 0.0584(18) 0.0367(15) 0.0405(16) -0.0029(13) -0.0143(13) 0.0032(14) C43 0.0353(15) 0.0534(18) 0.0517(17) -0.0179(14) 0.0003(12) -0.0080(13) Al2 0.0253(4) 0.0319(4) 0.0197(3) 0.0002(3) 0.0024(3) -0.0040(3) C5 0.0347(13) 0.0375(14) 0.0229(12) 0.0051(11) -0.0021(10) -0.0092(11) C51 0.0461(18) 0.084(2) 0.0504(18) 0.0297(18) -0.0168(14) -0.0285(17) C52 0.0548(17) 0.0443(16) 0.0246(13) 0.0005(12) -0.0020(11) -0.0108(14) C53 0.0578(18) 0.0375(16) 0.0355(15) 0.0006(12) -0.0065(13) -0.0032(14) C6 0.0294(12) 0.0353(14) 0.0273(12) -0.0082(10) 0.0026(10) -0.0070(11) C61 0.0354(14) 0.0425(15) 0.0395(14) -0.0037(12) 0.0038(11) -0.0172(12) C62 0.0514(18) 0.0477(18) 0.0559(18) -0.0216(15) -0.0076(14) -0.0056(15) C63 0.0332(14) 0.0485(17) 0.0336(13) -0.0039(12) -0.0013(11) -0.0097(12) C71 0.0258(12) 0.0370(13) 0.0189(11) -0.0006(10) -0.0040(9) -0.0107(10) C72 0.0307(12) 0.0293(13) 0.0268(12) -0.0013(10) -0.0019(9) -0.0120(10) C73 0.0311(13) 0.0337(14) 0.0331(13) -0.0088(11) 0.0037(10) -0.0129(11) C731 0.0598(18) 0.0375(15) 0.0427(16) -0.0035(13) -0.0003(13) -0.0185(14) C732 0.0567(18) 0.0451(16) 0.0349(14) -0.0115(12) 0.0104(12) -0.0205(14) C733 0.0308(14) 0.0502(18) 0.068(2) -0.0251(15) 0.0032(13) -0.0064(13) C81 0.0221(11) 0.0336(13) 0.0216(11) -0.0016(10) 0.0039(9) -0.0057(10) C82 0.0316(13) 0.0307(13) 0.0273(12) -0.0026(10) 0.0016(10) -0.0084(11) C83 0.0396(14) 0.0416(15) 0.0302(13) -0.0124(11) 0.0026(10) -0.0150(12) C831 0.0590(19) 0.066(2) 0.0346(15) -0.0187(14) 0.0071(13) -0.0281(16) C832 0.0459(17) 0.086(3) 0.063(2) -0.0393(19) -0.0007(15) -0.0240(17) C833 0.097(3) 0.0497(19) 0.058(2) -0.0103(16) 0.0118(19) -0.035(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 P1 C71 1.856(3) . ? P1 C1 1.886(3) . ? P1 Al1 2.5585(15) . ? P1 H1A 1.2970 . ? P1A C71 1.711(4) . ? P1A C1 1.856(4) . ? P1A Al1 2.575(4) . ? P1A H1AA 1.6205 . ? C1 C13 1.518(4) . ? C1 C12 1.520(4) . ? C1 C11 1.523(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? P2 C81 1.790(2) . ? P2 C2 1.855(2) . ? P2 Al2 2.5767(14) . ? P2 H2A 1.3408 . ? P2 H2AA 1.8818 . ? P2A C81 1.894(4) . ? P2A C2 1.923(4) . ? P2A Al2 2.572(3) . ? P2A H2AA 1.1658 . ? C2 C22A 1.481(8) . ? C2 C23A 1.507(12) . ? C2 C21 1.516(5) . ? C2 C23 1.530(8) . ? C2 C22 1.569(6) . ? C2 C21A 1.584(7) . ? C21 H21A 0.9599 . ? C21 H21B 0.9599 . ? C21 H21C 0.9599 . ? C22 H22A 0.9599 . ? C22 H22B 0.9599 . ? C22 H22C 0.9599 . ? C23 H23A 0.9599 . ? C23 H23B 0.9599 . ? C23 H23C 0.9599 . ? C21A H21D 0.9599 . ? C21A H21E 0.9599 . ? C21A H21F 0.9599 . ? C22A H22D 0.9599 . ? C22A H22E 0.9599 . ? C22A H22F 0.9599 . ? C23A H23D 0.9599 . ? C23A H23E 0.9599 . ? C23A H23F 0.9599 . ? Al1 C81 2.031(3) . ? Al1 C3 2.038(3) . ? Al1 C4 2.039(3) . ? C3 C31 1.526(4) . ? C3 C32 1.534(4) . ? C3 C33 1.538(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C4 C43 1.529(4) . ? C4 C42 1.538(4) . ? C4 C41 1.543(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? Al2 C71 2.032(3) . ? Al2 C6 2.034(3) . ? Al2 C5 2.038(2) . ? C5 C51 1.526(4) . ? C5 C53 1.529(4) . ? C5 C52 1.538(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C6 C61 1.535(3) . ? C6 C63 1.537(3) . ? C6 C62 1.537(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C71 C72 1.349(3) . ? C72 C73 1.528(3) . ? C72 H72 0.9500 . ? C73 C731 1.526(4) . ? C73 C733 1.532(4) . ? C73 C732 1.537(3) . ? C731 H73D 0.9800 . ? C731 H73E 0.9800 . ? C731 H73F 0.9800 . ? C732 H73A 0.9800 . ? C732 H73B 0.9800 . ? C732 H73C 0.9800 . ? C733 H73G 0.9800 . ? C733 H73H 0.9800 . ? C733 H73I 0.9800 . ? C81 C82 1.342(3) . ? C82 C83 1.519(4) . ? C82 H82 0.9500 . ? C83 C833 1.515(4) . ? C83 C831 1.532(3) . ? C83 C832 1.534(4) . ? C831 H83A 0.9800 . ? C831 H83B 0.9800 . ? C831 H83C 0.9800 . ? C832 H83G 0.9800 . ? C832 H83H 0.9800 . ? C832 H83I 0.9800 . ? C833 H83D 0.9800 . ? C833 H83E 0.9800 . ? C833 H83F 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 C71 P1 C1 109.12(13) . . ? C71 P1 Al1 113.39(10) . . ? C1 P1 Al1 121.68(10) . . ? C71 P1 H1A 108.8 . . ? C1 P1 H1A 97.2 . . ? Al1 P1 H1A 104.6 . . ? C71 P1A C1 117.4(2) . . ? C71 P1A Al1 118.47(19) . . ? C1 P1A Al1 122.2(2) . . ? C71 P1A H1AA 82.8 . . ? C1 P1A H1AA 94.1 . . ? Al1 P1A H1AA 106.2 . . ? C13 C1 C12 110.0(2) . . ? C13 C1 C11 109.1(2) . . ? C12 C1 C11 110.3(2) . . ? C13 C1 P1A 94.8(4) . . ? C12 C1 P1A 117.0(3) . . ? C11 C1 P1A 114.4(2) . . ? C13 C1 P1 113.76(19) . . ? C12 C1 P1 102.81(18) . . ? C11 C1 P1 110.77(18) . . ? P1A C1 P1 19.9(3) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C81 P2 C2 117.92(12) . . ? C81 P2 Al2 113.33(9) . . ? C2 P2 Al2 125.66(10) . . ? C81 P2 H2A 96.4 . . ? C2 P2 H2A 89.2 . . ? Al2 P2 H2A 102.3 . . ? C81 P2 H2AA 89.3 . . ? C2 P2 H2AA 77.7 . . ? Al2 P2 H2AA 86.3 . . ? H2A P2 H2AA 166.8 . . ? C81 P2A C2 109.9(2) . . ? C81 P2A Al2 109.76(18) . . ? C2 P2A Al2 122.66(18) . . ? C81 P2A H2AA 112.9 . . ? C2 P2A H2AA 95.6 . . ? Al2 P2A H2AA 105.2 . . ? C22A C2 C23A 113.5(10) . . ? C22A C2 C21 77.8(5) . . ? C23A C2 C21 118.1(11) . . ? C22A C2 C23 120.6(8) . . ? C23A C2 C23 11.0(15) . . ? C21 C2 C23 109.8(8) . . ? C22A C2 C22 28.6(4) . . ? C23A C2 C22 98.9(10) . . ? C21 C2 C22 106.4(3) . . ? C23 C2 C22 109.1(7) . . ? C22A C2 C21A 109.9(5) . . ? C23A C2 C21A 107.6(10) . . ? C21 C2 C21A 32.5(3) . . ? C23 C2 C21A 96.7(8) . . ? C22 C2 C21A 138.4(4) . . ? C22A C2 P2 119.7(4) . . ? C23A C2 P2 113.7(11) . . ? C21 C2 P2 109.6(3) . . ? C23 C2 P2 112.6(7) . . ? C22 C2 P2 109.2(3) . . ? C21A C2 P2 89.0(4) . . ? C22A C2 P2A 105.8(5) . . ? C23A C2 P2A 109.5(11) . . ? C21 C2 P2A 126.0(3) . . ? C23 C2 P2A 113.0(7) . . ? C22 C2 P2A 89.2(4) . . ? C21A C2 P2A 110.5(5) . . ? P2 C2 P2A 22.00(10) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? C2 C21A H21D 109.5 . . ? C2 C21A H21E 109.5 . . ? C2 C21A H21F 109.5 . . ? C2 C22A H22D 109.5 . . ? C2 C22A H22E 109.5 . . ? C2 C22A H22F 109.5 . . ? C2 C23A H23D 109.5 . . ? C2 C23A H23E 109.5 . . ? C2 C23A H23F 109.5 . . ? C81 Al1 C3 110.79(10) . . ? C81 Al1 C4 113.99(10) . . ? C3 Al1 C4 114.54(11) . . ? C81 Al1 P1 103.21(8) . . ? C3 Al1 P1 117.93(9) . . ? C4 Al1 P1 95.22(9) . . ? C81 Al1 P1A 91.7(2) . . ? C3 Al1 P1A 115.64(13) . . ? C4 Al1 P1A 108.2(3) . . ? P1 Al1 P1A 14.5(2) . . ? C31 C3 C32 106.7(3) . . ? C31 C3 C33 107.5(3) . . ? C32 C3 C33 107.4(2) . . ? C31 C3 Al1 116.58(18) . . ? C32 C3 Al1 113.09(19) . . ? C33 C3 Al1 105.06(19) . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C43 C4 C42 107.7(2) . . ? C43 C4 C41 108.3(2) . . ? C42 C4 C41 105.3(2) . . ? C43 C4 Al1 110.25(18) . . ? C42 C4 Al1 113.30(17) . . ? C41 C4 Al1 111.67(18) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C71 Al2 C6 112.95(10) . . ? C71 Al2 C5 112.40(10) . . ? C6 Al2 C5 114.40(10) . . ? C71 Al2 P2A 106.32(14) . . ? C6 Al2 P2A 91.17(17) . . ? C5 Al2 P2A 117.81(9) . . ? C71 Al2 P2 94.75(10) . . ? C6 Al2 P2 106.32(12) . . ? C5 Al2 P2 114.32(8) . . ? P2A Al2 P2 16.16(8) . . ? C51 C5 C53 108.0(2) . . ? C51 C5 C52 105.9(2) . . ? C53 C5 C52 107.1(2) . . ? C51 C5 Al2 116.89(17) . . ? C53 C5 Al2 112.38(18) . . ? C52 C5 Al2 105.96(16) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C61 C6 C63 107.1(2) . . ? C61 C6 C62 105.5(2) . . ? C63 C6 C62 108.2(2) . . ? C61 C6 Al2 114.74(17) . . ? C63 C6 Al2 109.31(17) . . ? C62 C6 Al2 111.70(18) . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C6 C62 H62A 109.5 . . ? C6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C6 C63 H63A 109.5 . . ? C6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C72 C71 P1A 141.2(5) . . ? C72 C71 P1 121.9(2) . . ? P1A C71 P1 20.4(4) . . ? C72 C71 Al2 108.49(17) . . ? P1A C71 Al2 110.2(4) . . ? P1 C71 Al2 129.31(14) . . ? C71 C72 C73 140.9(2) . . ? C71 C72 H72 109.6 . . ? C73 C72 H72 109.6 . . ? C731 C73 C72 119.6(2) . . ? C731 C73 C733 107.1(2) . . ? C72 C73 C733 106.3(2) . . ? C731 C73 C732 108.7(2) . . ? C72 C73 C732 106.3(2) . . ? C733 C73 C732 108.4(2) . . ? C73 C731 H73D 109.5 . . ? C73 C731 H73E 109.5 . . ? H73D C731 H73E 109.5 . . ? C73 C731 H73F 109.5 . . ? H73D C731 H73F 109.5 . . ? H73E C731 H73F 109.5 . . ? C73 C732 H73A 109.5 . . ? C73 C732 H73B 109.5 . . ? H73A C732 H73B 109.5 . . ? C73 C732 H73C 109.5 . . ? H73A C732 H73C 109.5 . . ? H73B C732 H73C 109.5 . . ? C73 C733 H73G 109.5 . . ? C73 C733 H73H 109.5 . . ? H73G C733 H73H 109.5 . . ? C73 C733 H73I 109.5 . . ? H73G C733 H73I 109.5 . . ? H73H C733 H73I 109.5 . . ? C82 C81 P2 138.5(2) . . ? C82 C81 P2A 117.5(3) . . ? P2 C81 P2A 22.44(9) . . ? C82 C81 Al1 108.74(17) . . ? P2 C81 Al1 112.66(18) . . ? P2A C81 Al1 133.3(2) . . ? C81 C82 C83 141.3(2) . . ? C81 C82 H82 109.4 . . ? C83 C82 H82 109.4 . . ? C833 C83 C82 117.4(2) . . ? C833 C83 C831 108.9(2) . . ? C82 C83 C831 107.3(2) . . ? C833 C83 C832 108.3(3) . . ? C82 C83 C832 106.2(2) . . ? C831 C83 C832 108.4(2) . . ? C83 C831 H83A 109.5 . . ? C83 C831 H83B 109.5 . . ? H83A C831 H83B 109.5 . . ? C83 C831 H83C 109.5 . . ? H83A C831 H83C 109.5 . . ? H83B C831 H83C 109.5 . . ? C83 C832 H83G 109.5 . . ? C83 C832 H83H 109.5 . . ? H83G C832 H83H 109.5 . . ? C83 C832 H83I 109.5 . . ? H83G C832 H83I 109.5 . . ? H83H C832 H83I 109.5 . . ? C83 C833 H83D 109.5 . . ? C83 C833 H83E 109.5 . . ? H83D C833 H83E 109.5 . . ? C83 C833 H83F 109.5 . . ? H83D C833 H83F 109.5 . . ? H83E C833 H83F 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 C71 P1A C1 C13 -108.1(7) . . . . ? Al1 P1A C1 C13 88.0(6) . . . . ? C71 P1A C1 C12 136.6(6) . . . . ? Al1 P1A C1 C12 -27.4(8) . . . . ? C71 P1A C1 C11 5.4(9) . . . . ? Al1 P1A C1 C11 -158.5(4) . . . . ? C71 P1A C1 P1 89.1(9) . . . . ? Al1 P1A C1 P1 -74.8(6) . . . . ? C71 P1 C1 C13 -78.8(2) . . . . ? Al1 P1 C1 C13 56.3(2) . . . . ? C71 P1 C1 C12 162.3(2) . . . . ? Al1 P1 C1 C12 -62.6(2) . . . . ? C71 P1 C1 C11 44.6(2) . . . . ? Al1 P1 C1 C11 179.59(18) . . . . ? C71 P1 C1 P1A -60.0(4) . . . . ? Al1 P1 C1 P1A 75.0(4) . . . . ? C81 P2 C2 C22A 138.4(7) . . . . ? Al2 P2 C2 C22A -20.3(7) . . . . ? C81 P2 C2 C23A -0.3(11) . . . . ? Al2 P2 C2 C23A -159.0(10) . . . . ? C81 P2 C2 C21 -134.8(4) . . . . ? Al2 P2 C2 C21 66.5(5) . . . . ? C81 P2 C2 C23 -12.3(8) . . . . ? Al2 P2 C2 C23 -170.9(8) . . . . ? C81 P2 C2 C22 109.1(4) . . . . ? Al2 P2 C2 C22 -49.6(4) . . . . ? C81 P2 C2 C21A -109.1(5) . . . . ? Al2 P2 C2 C21A 92.2(5) . . . . ? C81 P2 C2 P2A 83.3(3) . . . . ? Al2 P2 C2 P2A -75.3(3) . . . . ? C81 P2A C2 C22A 165.8(6) . . . . ? Al2 P2A C2 C22A -63.0(7) . . . . ? C81 P2A C2 C23A 43.1(11) . . . . ? Al2 P2A C2 C23A 174.3(10) . . . . ? C81 P2A C2 C21 -107.9(5) . . . . ? Al2 P2A C2 C21 23.2(7) . . . . ? C81 P2A C2 C23 31.9(8) . . . . ? Al2 P2A C2 C23 163.0(8) . . . . ? C81 P2A C2 C22 142.3(4) . . . . ? Al2 P2A C2 C22 -86.5(5) . . . . ? C81 P2A C2 C21A -75.2(5) . . . . ? Al2 P2A C2 C21A 55.9(6) . . . . ? C81 P2A C2 P2 -61.9(3) . . . . ? Al2 P2A C2 P2 69.3(4) . . . . ? C71 P1 Al1 C81 24.07(14) . . . . ? C1 P1 Al1 C81 -109.27(15) . . . . ? C71 P1 Al1 C3 146.55(13) . . . . ? C1 P1 Al1 C3 13.21(19) . . . . ? C71 P1 Al1 C4 -92.09(14) . . . . ? C1 P1 Al1 C4 134.58(16) . . . . ? C71 P1 Al1 P1A 61.9(4) . . . . ? C1 P1 Al1 P1A -71.4(4) . . . . ? C71 P1A Al1 C81 55.1(7) . . . . ? C1 P1A Al1 C81 -141.1(7) . . . . ? C71 P1A Al1 C3 169.2(5) . . . . ? C1 P1A Al1 C3 -27.1(8) . . . . ? C71 P1A Al1 C4 -60.9(7) . . . . ? C1 P1A Al1 C4 102.9(6) . . . . ? C71 P1A Al1 P1 -88.2(8) . . . . ? C1 P1A Al1 P1 75.6(7) . . . . ? C81 Al1 C3 C31 68.2(3) . . . . ? C4 Al1 C3 C31 -161.2(2) . . . . ? P1 Al1 C3 C31 -50.4(3) . . . . ? P1A Al1 C3 C31 -34.4(4) . . . . ? C81 Al1 C3 C32 -167.6(2) . . . . ? C4 Al1 C3 C32 -37.0(2) . . . . ? P1 Al1 C3 C32 73.8(2) . . . . ? P1A Al1 C3 C32 89.9(4) . . . . ? C81 Al1 C3 C33 -50.7(2) . . . . ? C4 Al1 C3 C33 79.9(2) . . . . ? P1 Al1 C3 C33 -169.29(17) . . . . ? P1A Al1 C3 C33 -153.3(4) . . . . ? C81 Al1 C4 C43 -41.6(2) . . . . ? C3 Al1 C4 C43 -170.69(18) . . . . ? P1 Al1 C4 C43 65.34(18) . . . . ? P1A Al1 C4 C43 58.7(2) . . . . ? C81 Al1 C4 C42 79.1(2) . . . . ? C3 Al1 C4 C42 -49.9(2) . . . . ? P1 Al1 C4 C42 -173.9(2) . . . . ? P1A Al1 C4 C42 179.5(2) . . . . ? C81 Al1 C4 C41 -162.12(18) . . . . ? C3 Al1 C4 C41 68.8(2) . . . . ? P1 Al1 C4 C41 -55.15(19) . . . . ? P1A Al1 C4 C41 -61.8(2) . . . . ? C81 P2A Al2 C71 20.7(3) . . . . ? C2 P2A Al2 C71 -110.5(3) . . . . ? C81 P2A Al2 C6 -93.6(3) . . . . ? C2 P2A Al2 C6 135.1(4) . . . . ? C81 P2A Al2 C5 147.8(2) . . . . ? C2 P2A Al2 C5 16.6(5) . . . . ? C81 P2A Al2 P2 66.2(4) . . . . ? C2 P2A Al2 P2 -65.0(4) . . . . ? C81 P2 Al2 C71 53.7(2) . . . . ? C2 P2 Al2 C71 -146.7(3) . . . . ? C81 P2 Al2 C6 -61.9(2) . . . . ? C2 P2 Al2 C6 97.7(3) . . . . ? C81 P2 Al2 C5 170.9(2) . . . . ? C2 P2 Al2 C5 -29.5(3) . . . . ? C81 P2 Al2 P2A -82.8(3) . . . . ? C2 P2 Al2 P2A 76.7(3) . . . . ? C71 Al2 C5 C51 62.5(2) . . . . ? C6 Al2 C5 C51 -167.0(2) . . . . ? P2A Al2 C5 C51 -61.6(3) . . . . ? P2 Al2 C5 C51 -44.1(3) . . . . ? C71 Al2 C5 C53 -171.81(18) . . . . ? C6 Al2 C5 C53 -41.3(2) . . . . ? P2A Al2 C5 C53 64.1(3) . . . . ? P2 Al2 C5 C53 81.7(2) . . . . ? C71 Al2 C5 C52 -55.2(2) . . . . ? C6 Al2 C5 C52 75.4(2) . . . . ? P2A Al2 C5 C52 -179.3(2) . . . . ? P2 Al2 C5 C52 -161.69(19) . . . . ? C71 Al2 C6 C61 79.73(19) . . . . ? C5 Al2 C6 C61 -50.5(2) . . . . ? P2A Al2 C6 C61 -171.98(19) . . . . ? P2 Al2 C6 C61 -177.70(17) . . . . ? C71 Al2 C6 C63 -40.58(19) . . . . ? C5 Al2 C6 C63 -170.85(16) . . . . ? P2A Al2 C6 C63 67.71(18) . . . . ? P2 Al2 C6 C63 61.99(17) . . . . ? C71 Al2 C6 C62 -160.29(18) . . . . ? C5 Al2 C6 C62 69.4(2) . . . . ? P2A Al2 C6 C62 -52.0(2) . . . . ? P2 Al2 C6 C62 -57.7(2) . . . . ? C1 P1A C71 C72 -60.9(10) . . . . ? Al1 P1A C71 C72 103.6(5) . . . . ? C1 P1A C71 P1 -83.1(8) . . . . ? Al1 P1A C71 P1 81.5(7) . . . . ? C1 P1A C71 Al2 115.5(6) . . . . ? Al1 P1A C71 Al2 -80.0(6) . . . . ? C1 P1 C71 C72 -97.2(2) . . . . ? Al1 P1 C71 C72 123.72(19) . . . . ? C1 P1 C71 P1A 66.6(4) . . . . ? Al1 P1 C71 P1A -72.4(4) . . . . ? C1 P1 C71 Al2 89.33(18) . . . . ? Al1 P1 C71 Al2 -49.74(19) . . . . ? C6 Al2 C71 C72 -49.31(18) . . . . ? C5 Al2 C71 C72 81.97(18) . . . . ? P2A Al2 C71 C72 -147.76(19) . . . . ? P2 Al2 C71 C72 -159.26(17) . . . . ? C6 Al2 C71 P1A 133.1(2) . . . . ? C5 Al2 C71 P1A -95.6(2) . . . . ? P2A Al2 C71 P1A 34.6(3) . . . . ? P2 Al2 C71 P1A 23.1(3) . . . . ? C6 Al2 C71 P1 124.84(15) . . . . ? C5 Al2 C71 P1 -103.88(16) . . . . ? P2A Al2 C71 P1 26.4(2) . . . . ? P2 Al2 C71 P1 14.89(18) . . . . ? P1A C71 C72 C73 -6.3(6) . . . . ? P1 C71 C72 C73 2.5(4) . . . . ? Al2 C71 C72 C73 177.2(3) . . . . ? C71 C72 C73 C731 -4.5(5) . . . . ? C71 C72 C73 C733 -125.8(3) . . . . ? C71 C72 C73 C732 118.9(3) . . . . ? C2 P2 C81 C82 -58.3(4) . . . . ? Al2 P2 C81 C82 102.9(3) . . . . ? C2 P2 C81 P2A -81.8(3) . . . . ? Al2 P2 C81 P2A 79.4(3) . . . . ? C2 P2 C81 Al1 118.5(2) . . . . ? Al2 P2 C81 Al1 -80.2(2) . . . . ? C2 P2A C81 C82 -98.9(4) . . . . ? Al2 P2A C81 C82 123.4(3) . . . . ? C2 P2A C81 P2 63.8(3) . . . . ? Al2 P2A C81 P2 -73.9(3) . . . . ? C2 P2A C81 Al1 90.0(3) . . . . ? Al2 P2A C81 Al1 -47.7(4) . . . . ? C3 Al1 C81 C82 87.07(18) . . . . ? C4 Al1 C81 C82 -43.87(19) . . . . ? P1 Al1 C81 C82 -145.79(15) . . . . ? P1A Al1 C81 C82 -154.6(2) . . . . ? C3 Al1 C81 P2 -90.73(15) . . . . ? C4 Al1 C81 P2 138.33(13) . . . . ? P1 Al1 C81 P2 36.41(15) . . . . ? P1A Al1 C81 P2 27.6(3) . . . . ? C3 Al1 C81 P2A -101.2(2) . . . . ? C4 Al1 C81 P2A 127.8(2) . . . . ? P1 Al1 C81 P2A 25.9(2) . . . . ? P1A Al1 C81 P2A 17.1(4) . . . . ? P2 C81 C82 C83 -2.9(5) . . . . ? P2A C81 C82 C83 7.0(4) . . . . ? Al1 C81 C82 C83 -179.8(3) . . . . ? C81 C82 C83 C833 -4.8(5) . . . . ? C81 C82 C83 C831 118.2(3) . . . . ? C81 C82 C83 C832 -126.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 63.00 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.398 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.043 # Attachment 'Compound5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 861402' #TrackingRef 'Compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H30 Al O2 P' _chemical_formula_weight 348.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' _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 7.7790(3) _cell_length_b 9.1298(3) _cell_length_c 15.9543(5) _cell_angle_alpha 91.206(3) _cell_angle_beta 91.247(3) _cell_angle_gamma 114.460(3) _cell_volume 1030.58(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 53595 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9289 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'imaging plate detector system' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9368 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4907 _reflns_number_gt 3990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _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^)+(0.0417P)^2^+0.0834P] 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 4907 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.66384(5) 0.22648(4) 0.159881(19) 0.02713(9) Uani 1 1 d . . . C11 C 0.72458(18) 0.41171(17) 0.10669(8) 0.0308(3) Uani 1 1 d . . . C111 C 0.7704(2) 0.55679(18) 0.15085(9) 0.0357(3) Uani 1 1 d . . . H111 H 0.7733 0.5597 0.2104 0.043 Uiso 1 1 calc R . . C112 C 0.8117(2) 0.69703(19) 0.10784(10) 0.0426(3) Uani 1 1 d . . . H112 H 0.8422 0.7958 0.1381 0.051 Uiso 1 1 calc R . . C113 C 0.8091(2) 0.6943(2) 0.02152(10) 0.0443(4) Uani 1 1 d . . . H113 H 0.8384 0.7910 -0.0076 0.053 Uiso 1 1 calc R . . C114 C 0.7638(3) 0.5512(2) -0.02257(10) 0.0527(4) Uani 1 1 d . . . H114 H 0.7614 0.5496 -0.0821 0.063 Uiso 1 1 calc R . . C115 C 0.7216(3) 0.4098(2) 0.01909(9) 0.0465(4) Uani 1 1 d . . . H115 H 0.6908 0.3115 -0.0118 0.056 Uiso 1 1 calc R . . C12 C 0.74041(17) 0.24910(15) 0.26649(7) 0.0265(3) Uani 1 1 d . . . C121 C 0.63058(18) 0.27988(16) 0.32180(8) 0.0294(3) Uani 1 1 d . . . H121 H 0.5209 0.2872 0.2987 0.035 Uiso 1 1 calc R . . C122 C 0.65897(19) 0.30427(18) 0.41566(8) 0.0331(3) Uani 1 1 d . . . C123 C 0.4742(2) 0.1926(2) 0.45530(10) 0.0492(4) Uani 1 1 d . . . H12A H 0.3704 0.2175 0.4343 0.074 Uiso 1 1 calc R . . H12B H 0.4870 0.2087 0.5164 0.074 Uiso 1 1 calc R . . H12C H 0.4474 0.0803 0.4405 0.074 Uiso 1 1 calc R . . C124 C 0.8220(2) 0.2697(2) 0.44990(9) 0.0430(4) Uani 1 1 d . . . H12D H 0.7986 0.1580 0.4356 0.064 Uiso 1 1 calc R . . H12E H 0.8326 0.2864 0.5110 0.064 Uiso 1 1 calc R . . H12F H 0.9398 0.3425 0.4251 0.064 Uiso 1 1 calc R . . C125 C 0.6965(2) 0.4797(2) 0.43664(9) 0.0435(4) Uani 1 1 d . . . H12G H 0.8145 0.5515 0.4116 0.065 Uiso 1 1 calc R . . H12H H 0.7071 0.4979 0.4977 0.065 Uiso 1 1 calc R . . H12I H 0.5918 0.5019 0.4141 0.065 Uiso 1 1 calc R . . C13 C 0.41834(19) 0.10143(18) 0.13647(9) 0.0372(3) Uani 1 1 d . . . H13A H 0.3411 0.1547 0.1598 0.045 Uiso 1 1 calc R . . H13B H 0.3965 0.0912 0.0748 0.045 Uiso 1 1 calc R . . C131 C 0.3529(2) -0.0656(2) 0.17156(11) 0.0511(4) Uani 1 1 d . . . H13C H 0.4321 -0.1176 0.1506 0.077 Uiso 1 1 calc R . . H13D H 0.2210 -0.1301 0.1537 0.077 Uiso 1 1 calc R . . H13E H 0.3633 -0.0570 0.2330 0.077 Uiso 1 1 calc R . . C14 C 0.80647(19) 0.12665(16) 0.11116(8) 0.0319(3) Uani 1 1 d . . . O11 O 0.95097(13) 0.14304(12) 0.15752(6) 0.0342(2) Uani 1 1 d . . . O12 O 0.75967(15) 0.05972(14) 0.04284(6) 0.0451(3) Uani 1 1 d . . . Al1 Al 0.97782(5) 0.20592(5) 0.27102(2) 0.03051(11) Uani 1 1 d . . . C15 C 0.9536(3) 0.0073(2) 0.32604(10) 0.0490(4) Uani 1 1 d . . . H15A H 1.0407 -0.0332 0.3001 0.059 Uiso 1 1 calc R . . H15B H 0.9922 0.0328 0.3860 0.059 Uiso 1 1 calc R . . C151 C 0.7528(3) -0.1250(2) 0.31941(13) 0.0653(5) Uani 1 1 d . . . H15C H 0.6669 -0.0881 0.3479 0.098 Uiso 1 1 calc R . . H15D H 0.7499 -0.2219 0.3458 0.098 Uiso 1 1 calc R . . H15E H 0.7129 -0.1497 0.2602 0.098 Uiso 1 1 calc R . . C16 C 1.2134(2) 0.40301(19) 0.28719(10) 0.0407(3) Uani 1 1 d . . . H16A H 1.2677 0.4015 0.3437 0.049 Uiso 1 1 calc R . . H16B H 1.3044 0.3985 0.2459 0.049 Uiso 1 1 calc R . . C161 C 1.1987(2) 0.5636(2) 0.27906(13) 0.0568(5) Uani 1 1 d . . . H16C H 1.1561 0.5720 0.2218 0.085 Uiso 1 1 calc R . . H16D H 1.3228 0.6519 0.2912 0.085 Uiso 1 1 calc R . . H16E H 1.1078 0.5701 0.3189 0.085 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 P1 0.03214(17) 0.03006(19) 0.02160(15) -0.00236(13) 0.00030(12) 0.01549(13) C11 0.0354(7) 0.0358(7) 0.0259(6) 0.0009(5) 0.0017(5) 0.0193(6) C111 0.0456(8) 0.0355(8) 0.0293(6) 0.0003(6) 0.0009(6) 0.0203(6) C112 0.0497(8) 0.0353(8) 0.0471(8) 0.0050(7) 0.0043(7) 0.0218(7) C113 0.0464(8) 0.0461(9) 0.0482(9) 0.0185(7) 0.0119(7) 0.0258(7) C114 0.0774(12) 0.0621(12) 0.0300(7) 0.0144(8) 0.0113(8) 0.0393(10) C115 0.0712(11) 0.0489(10) 0.0266(7) 0.0017(7) 0.0042(7) 0.0321(8) C12 0.0309(6) 0.0269(6) 0.0236(6) 0.0004(5) 0.0015(5) 0.0141(5) C121 0.0321(6) 0.0346(7) 0.0253(6) 0.0004(5) 0.0001(5) 0.0176(5) C122 0.0379(7) 0.0437(8) 0.0231(6) -0.0001(6) 0.0030(5) 0.0224(6) C123 0.0513(9) 0.0636(11) 0.0358(8) 0.0135(8) 0.0132(7) 0.0258(8) C124 0.0517(9) 0.0627(11) 0.0255(6) -0.0014(7) -0.0030(6) 0.0350(8) C125 0.0524(9) 0.0504(10) 0.0348(7) -0.0096(7) -0.0019(6) 0.0291(8) C13 0.0357(7) 0.0415(8) 0.0336(7) -0.0062(6) -0.0029(6) 0.0159(6) C131 0.0417(8) 0.0422(9) 0.0569(10) -0.0032(8) 0.0004(7) 0.0052(7) C14 0.0394(7) 0.0307(7) 0.0284(6) -0.0002(5) 0.0056(5) 0.0173(6) O11 0.0385(5) 0.0423(6) 0.0293(5) -0.0010(4) 0.0041(4) 0.0242(4) O12 0.0547(6) 0.0526(7) 0.0333(5) -0.0160(5) -0.0020(5) 0.0285(5) Al1 0.0329(2) 0.0366(2) 0.0279(2) 0.00208(17) 0.00226(15) 0.02014(17) C15 0.0659(11) 0.0563(11) 0.0430(8) 0.0104(8) 0.0115(8) 0.0425(9) C151 0.0900(14) 0.0424(10) 0.0670(12) 0.0160(9) 0.0296(11) 0.0291(10) C16 0.0323(7) 0.0505(9) 0.0405(8) 0.0009(7) -0.0010(6) 0.0185(6) C161 0.0424(9) 0.0421(10) 0.0787(13) 0.0031(9) 0.0000(8) 0.0103(7) _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 C12 1.7691(13) . ? P1 C11 1.7943(14) . ? P1 C13 1.7988(14) . ? P1 C14 1.8738(13) . ? C11 C111 1.3917(19) . ? C11 C115 1.3969(18) . ? C111 C112 1.385(2) . ? C111 H111 0.9500 . ? C112 C113 1.376(2) . ? C112 H112 0.9500 . ? C113 C114 1.377(2) . ? C113 H113 0.9500 . ? C114 C115 1.382(2) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C12 C121 1.3449(16) . ? C12 Al1 2.0420(12) . ? C121 C122 1.5071(17) . ? C121 H121 0.9500 . ? C122 C124 1.5216(19) . ? C122 C125 1.532(2) . ? C122 C123 1.536(2) . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 H12D 0.9800 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C13 C131 1.518(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C14 O12 1.2102(16) . ? C14 O11 1.2856(17) . ? O11 Al1 1.8688(10) . ? Al1 C15 1.9714(17) . ? Al1 C16 1.9730(16) . ? C15 C151 1.528(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C151 H15C 0.9800 . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C16 C161 1.525(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C161 H16C 0.9800 . ? C161 H16D 0.9800 . ? C161 H16E 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 C12 P1 C11 114.84(6) . . ? C12 P1 C13 117.02(6) . . ? C11 P1 C13 107.94(7) . . ? C12 P1 C14 102.45(6) . . ? C11 P1 C14 105.81(6) . . ? C13 P1 C14 107.85(6) . . ? C111 C11 C115 119.29(13) . . ? C111 C11 P1 121.36(10) . . ? C115 C11 P1 119.34(11) . . ? C112 C111 C11 119.94(13) . . ? C112 C111 H111 120.0 . . ? C11 C111 H111 120.0 . . ? C113 C112 C111 120.46(15) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C112 C113 C114 119.90(14) . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C113 C114 C115 120.59(14) . . ? C113 C114 H114 119.7 . . ? C115 C114 H114 119.7 . . ? C114 C115 C11 119.82(15) . . ? C114 C115 H115 120.1 . . ? C11 C115 H115 120.1 . . ? C121 C12 P1 116.46(10) . . ? C121 C12 Al1 136.94(10) . . ? P1 C12 Al1 106.49(6) . . ? C12 C121 C122 128.40(12) . . ? C12 C121 H121 115.8 . . ? C122 C121 H121 115.8 . . ? C121 C122 C124 113.20(10) . . ? C121 C122 C125 107.27(11) . . ? C124 C122 C125 109.64(13) . . ? C121 C122 C123 107.64(12) . . ? C124 C122 C123 109.83(12) . . ? C125 C122 C123 109.15(12) . . ? C122 C123 H12A 109.5 . . ? C122 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C122 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C122 C124 H12D 109.5 . . ? C122 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C131 C13 P1 113.27(11) . . ? C131 C13 H13A 108.9 . . ? P1 C13 H13A 108.9 . . ? C131 C13 H13B 108.9 . . ? P1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C131 H13C 109.5 . . ? C13 C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C13 C131 H13E 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? O12 C14 O11 127.85(12) . . ? O12 C14 P1 119.97(11) . . ? O11 C14 P1 112.17(9) . . ? C14 O11 Al1 123.26(8) . . ? O11 Al1 C15 102.11(6) . . ? O11 Al1 C16 108.12(6) . . ? C15 Al1 C16 119.63(7) . . ? O11 Al1 C12 92.61(5) . . ? C15 Al1 C12 115.95(6) . . ? C16 Al1 C12 113.46(6) . . ? C151 C15 Al1 112.90(12) . . ? C151 C15 H15A 109.0 . . ? Al1 C15 H15A 109.0 . . ? C151 C15 H15B 109.0 . . ? Al1 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C151 H15C 109.5 . . ? C15 C151 H15D 109.5 . . ? H15C C151 H15D 109.5 . . ? C15 C151 H15E 109.5 . . ? H15C C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? C161 C16 Al1 117.08(10) . . ? C161 C16 H16A 108.0 . . ? Al1 C16 H16A 108.0 . . ? C161 C16 H16B 108.0 . . ? Al1 C16 H16B 108.0 . . ? H16A C16 H16B 107.3 . . ? C16 C161 H16C 109.5 . . ? C16 C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C16 C161 H16E 109.5 . . ? H16C C161 H16E 109.5 . . ? H16D C161 H16E 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 C12 P1 C11 C111 -20.00(13) . . . . ? C13 P1 C11 C111 112.54(12) . . . . ? C14 P1 C11 C111 -132.21(11) . . . . ? C12 P1 C11 C115 161.48(11) . . . . ? C13 P1 C11 C115 -65.98(13) . . . . ? C14 P1 C11 C115 49.27(13) . . . . ? C115 C11 C111 C112 0.2(2) . . . . ? P1 C11 C111 C112 -178.28(11) . . . . ? C11 C111 C112 C113 -0.4(2) . . . . ? C111 C112 C113 C114 0.4(2) . . . . ? C112 C113 C114 C115 -0.3(3) . . . . ? C113 C114 C115 C11 0.1(3) . . . . ? C111 C11 C115 C114 -0.1(2) . . . . ? P1 C11 C115 C114 178.44(13) . . . . ? C11 P1 C12 C121 82.19(12) . . . . ? C13 P1 C12 C121 -45.91(13) . . . . ? C14 P1 C12 C121 -163.62(11) . . . . ? C11 P1 C12 Al1 -101.05(7) . . . . ? C13 P1 C12 Al1 130.85(7) . . . . ? C14 P1 C12 Al1 13.14(8) . . . . ? P1 C12 C121 C122 179.82(11) . . . . ? Al1 C12 C121 C122 4.4(2) . . . . ? C12 C121 C122 C124 -7.5(2) . . . . ? C12 C121 C122 C125 113.60(16) . . . . ? C12 C121 C122 C123 -129.06(15) . . . . ? C12 P1 C13 C131 -53.76(12) . . . . ? C11 P1 C13 C131 174.88(10) . . . . ? C14 P1 C13 C131 60.98(12) . . . . ? C12 P1 C14 O12 162.85(12) . . . . ? C11 P1 C14 O12 -76.51(13) . . . . ? C13 P1 C14 O12 38.80(14) . . . . ? C12 P1 C14 O11 -18.48(11) . . . . ? C11 P1 C14 O11 102.17(10) . . . . ? C13 P1 C14 O11 -142.52(10) . . . . ? O12 C14 O11 Al1 -165.29(12) . . . . ? P1 C14 O11 Al1 16.16(14) . . . . ? C14 O11 Al1 C15 110.84(12) . . . . ? C14 O11 Al1 C16 -122.13(11) . . . . ? C14 O11 Al1 C12 -6.40(11) . . . . ? C121 C12 Al1 O11 169.25(15) . . . . ? P1 C12 Al1 O11 -6.51(7) . . . . ? C121 C12 Al1 C15 64.44(17) . . . . ? P1 C12 Al1 C15 -111.32(8) . . . . ? C121 C12 Al1 C16 -79.71(16) . . . . ? P1 C12 Al1 C16 104.53(7) . . . . ? O11 Al1 C15 C151 -70.49(12) . . . . ? C16 Al1 C15 C151 170.31(11) . . . . ? C12 Al1 C15 C151 28.49(14) . . . . ? O11 Al1 C16 C161 90.73(13) . . . . ? C15 Al1 C16 C161 -153.17(12) . . . . ? C12 Al1 C16 C161 -10.47(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.314 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.038 # Attachment 'Compoundcis-7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 861403' #TrackingRef 'Compoundcis-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 Al N O P' _chemical_formula_weight 423.49 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' Al Al 0.0645 0.0514 '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' _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 8.3516(5) _cell_length_b 8.9767(5) _cell_length_c 17.3493(9) _cell_angle_alpha 81.019(4) _cell_angle_beta 76.329(4) _cell_angle_gamma 80.138(4) _cell_volume 1236.03(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 23959 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9761 _exptl_absorpt_correction_T_max 0.9777 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'imaging plate detector system' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11214 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.99 _reflns_number_total 5896 _reflns_number_gt 4711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _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^)+(0.0502P)^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 5896 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.75325(4) 0.84909(3) 0.227288(17) 0.01985(7) Uani 1 1 d . . . C11 C 0.94635(15) 0.90868(13) 0.17164(7) 0.0242(2) Uani 1 1 d . . . C111 C 1.09515(16) 0.81939(15) 0.18194(8) 0.0318(3) Uani 1 1 d . . . H111 H 1.0939 0.7286 0.2195 0.038 Uiso 1 1 calc R . . C112 C 1.24500(18) 0.86196(18) 0.13788(9) 0.0409(3) Uani 1 1 d . . . H112 H 1.3477 0.8004 0.1448 0.049 Uiso 1 1 calc R . . C113 C 1.2472(2) 0.99234(18) 0.08413(9) 0.0439(4) Uani 1 1 d . . . H113 H 1.3515 1.0217 0.0540 0.053 Uiso 1 1 calc R . . C114 C 1.1007(2) 1.08047(18) 0.07357(10) 0.0484(4) Uani 1 1 d . . . H114 H 1.1032 1.1712 0.0361 0.058 Uiso 1 1 calc R . . C115 C 0.94892(19) 1.03927(16) 0.11679(9) 0.0379(3) Uani 1 1 d . . . H115 H 0.8467 1.1005 0.1088 0.045 Uiso 1 1 calc R . . C12 C 0.77394(14) 0.71413(12) 0.31112(7) 0.0209(2) Uani 1 1 d . . . C121 C 0.80848(15) 0.72720(13) 0.38138(7) 0.0239(2) Uani 1 1 d . . . H121 H 0.8095 0.6326 0.4159 0.029 Uiso 1 1 calc R . . C122 C 0.84625(16) 0.85397(14) 0.41959(7) 0.0278(3) Uani 1 1 d . . . C123 C 0.7296(2) 0.85890(18) 0.50159(9) 0.0426(3) Uani 1 1 d . . . H12A H 0.6164 0.8820 0.4954 0.051 Uiso 1 1 calc R . . H12B H 0.7540 0.9360 0.5279 0.051 Uiso 1 1 calc R . . H12C H 0.7448 0.7617 0.5331 0.051 Uiso 1 1 calc R . . C124 C 0.8273(3) 1.01049(16) 0.37217(10) 0.0539(5) Uani 1 1 d . . . H12D H 0.9006 1.0086 0.3205 0.065 Uiso 1 1 calc R . . H12E H 0.8549 1.0837 0.4000 0.065 Uiso 1 1 calc R . . H12F H 0.7144 1.0382 0.3660 0.065 Uiso 1 1 calc R . . C125 C 1.0250(2) 0.8087(2) 0.43078(12) 0.0558(5) Uani 1 1 d . . . H12G H 1.0366 0.7082 0.4592 0.067 Uiso 1 1 calc R . . H12H H 1.0507 0.8796 0.4607 0.067 Uiso 1 1 calc R . . H12I H 1.1001 0.8100 0.3795 0.067 Uiso 1 1 calc R . . C13 C 0.59158(17) 1.01208(14) 0.23549(8) 0.0329(3) Uani 1 1 d . . . H13A H 0.6304 1.0923 0.2536 0.039 Uiso 1 1 calc R . . H13B H 0.5680 1.0486 0.1837 0.039 Uiso 1 1 calc R . . C131 C 0.4324(2) 0.97219(19) 0.29337(10) 0.0483(4) Uani 1 1 d . . . H13C H 0.3986 0.8862 0.2780 0.058 Uiso 1 1 calc R . . H13D H 0.3462 1.0577 0.2921 0.058 Uiso 1 1 calc R . . H13E H 0.4523 0.9475 0.3465 0.058 Uiso 1 1 calc R . . C14 C 0.68586(14) 0.74158(13) 0.15917(7) 0.0219(2) Uani 1 1 d . . . O1 O 0.65639(11) 0.81361(10) 0.09653(5) 0.02944(19) Uani 1 1 d . . . N1 N 0.67673(13) 0.59579(11) 0.18781(6) 0.0237(2) Uani 1 1 d . . . C17 C 0.63344(16) 0.50136(13) 0.13807(7) 0.0255(2) Uani 1 1 d . . . C171 C 0.74313(18) 0.46302(15) 0.06828(8) 0.0334(3) Uani 1 1 d . . . H171 H 0.8475 0.5022 0.0517 0.040 Uiso 1 1 calc R . . C172 C 0.7018(2) 0.36775(16) 0.02234(9) 0.0384(3) Uani 1 1 d . . . H172 H 0.7781 0.3411 -0.0259 0.046 Uiso 1 1 calc R . . C173 C 0.5514(2) 0.31108(15) 0.04557(9) 0.0369(3) Uani 1 1 d . . . H173 H 0.5228 0.2462 0.0133 0.044 Uiso 1 1 calc R . . C174 C 0.44295(19) 0.34832(15) 0.11528(9) 0.0367(3) Uani 1 1 d . . . H174 H 0.3390 0.3084 0.1318 0.044 Uiso 1 1 calc R . . C175 C 0.48332(17) 0.44358(14) 0.16183(8) 0.0313(3) Uani 1 1 d . . . H175 H 0.4073 0.4692 0.2103 0.038 Uiso 1 1 calc R . . Al1 Al 0.74901(5) 0.50837(4) 0.28478(2) 0.02218(9) Uani 1 1 d . . . C15 C 0.57122(18) 0.41738(14) 0.36558(8) 0.0331(3) Uani 1 1 d . . . H15A H 0.5369 0.3395 0.3435 0.040 Uiso 1 1 calc R . . H15B H 0.6157 0.3697 0.4110 0.040 Uiso 1 1 calc R . . C151 C 0.4185(2) 0.53255(17) 0.39358(10) 0.0456(4) Uani 1 1 d . . . H15C H 0.4505 0.6080 0.4183 0.055 Uiso 1 1 calc R . . H15D H 0.3361 0.4808 0.4315 0.055 Uiso 1 1 calc R . . H15E H 0.3732 0.5810 0.3485 0.055 Uiso 1 1 calc R . . C16 C 0.96961(18) 0.38440(14) 0.25528(8) 0.0336(3) Uani 1 1 d . . . H16A H 0.9536 0.2865 0.2450 0.040 Uiso 1 1 calc R . . H16B H 1.0308 0.4330 0.2066 0.040 Uiso 1 1 calc R . . C161 C 1.0736(2) 0.36102(18) 0.31893(11) 0.0464(4) Uani 1 1 d . . . H16C H 1.0884 0.4583 0.3305 0.056 Uiso 1 1 calc R . . H16D H 1.1803 0.3045 0.2996 0.056 Uiso 1 1 calc R . . H16E H 1.0174 0.3056 0.3667 0.056 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 P1 0.02199(15) 0.01734(13) 0.01917(14) -0.00086(10) -0.00282(11) -0.00334(10) C11 0.0284(6) 0.0255(5) 0.0199(5) -0.0032(4) -0.0025(4) -0.0108(4) C111 0.0276(6) 0.0362(6) 0.0303(6) -0.0027(5) -0.0022(5) -0.0079(5) C112 0.0274(7) 0.0549(9) 0.0412(8) -0.0138(7) 0.0002(6) -0.0118(6) C113 0.0414(8) 0.0547(9) 0.0379(8) -0.0163(7) 0.0105(6) -0.0296(7) C114 0.0593(10) 0.0421(8) 0.0390(8) 0.0053(6) 0.0061(7) -0.0267(7) C115 0.0417(8) 0.0337(7) 0.0351(7) 0.0072(6) -0.0035(6) -0.0136(6) C12 0.0238(5) 0.0174(5) 0.0205(5) -0.0012(4) -0.0024(4) -0.0047(4) C121 0.0294(6) 0.0203(5) 0.0221(5) -0.0009(4) -0.0042(5) -0.0071(4) C122 0.0348(7) 0.0278(6) 0.0233(6) -0.0063(5) -0.0049(5) -0.0105(5) C123 0.0526(9) 0.0437(8) 0.0325(7) -0.0158(6) 0.0015(6) -0.0139(7) C124 0.1056(15) 0.0284(7) 0.0367(8) -0.0035(6) -0.0198(9) -0.0281(8) C125 0.0379(9) 0.0678(11) 0.0732(12) -0.0378(10) -0.0154(8) -0.0080(8) C13 0.0369(7) 0.0236(6) 0.0339(7) -0.0031(5) -0.0063(6) 0.0054(5) C131 0.0344(8) 0.0512(9) 0.0479(9) -0.0093(7) 0.0028(7) 0.0116(7) C14 0.0191(5) 0.0256(5) 0.0205(5) -0.0017(4) -0.0036(4) -0.0035(4) O1 0.0344(5) 0.0312(4) 0.0238(4) 0.0047(3) -0.0110(4) -0.0082(4) N1 0.0296(5) 0.0227(4) 0.0204(5) -0.0020(4) -0.0072(4) -0.0056(4) C17 0.0335(6) 0.0222(5) 0.0234(6) -0.0014(4) -0.0125(5) -0.0037(4) C171 0.0371(7) 0.0352(7) 0.0298(6) -0.0076(5) -0.0080(6) -0.0057(5) C172 0.0514(9) 0.0358(7) 0.0299(7) -0.0113(5) -0.0121(6) -0.0001(6) C173 0.0548(9) 0.0255(6) 0.0379(7) -0.0058(5) -0.0245(7) -0.0043(6) C174 0.0438(8) 0.0301(6) 0.0429(8) -0.0028(6) -0.0193(6) -0.0108(5) C175 0.0363(7) 0.0287(6) 0.0315(6) -0.0040(5) -0.0102(5) -0.0079(5) Al1 0.02910(19) 0.01775(16) 0.02037(17) -0.00085(12) -0.00641(14) -0.00500(13) C15 0.0414(8) 0.0258(6) 0.0306(6) 0.0018(5) -0.0031(6) -0.0115(5) C151 0.0435(9) 0.0379(7) 0.0489(9) -0.0049(6) 0.0081(7) -0.0132(6) C16 0.0380(7) 0.0253(6) 0.0356(7) -0.0036(5) -0.0074(6) 0.0002(5) C161 0.0412(8) 0.0386(8) 0.0599(10) 0.0010(7) -0.0206(8) -0.0001(6) _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 C12 1.7635(11) . ? P1 C11 1.7937(12) . ? P1 C13 1.8115(12) . ? P1 C14 1.8712(12) . ? C11 C115 1.3896(17) . ? C11 C111 1.3920(18) . ? C111 C112 1.385(2) . ? C111 H111 0.9600 . ? C112 C113 1.378(2) . ? C112 H112 0.9600 . ? C113 C114 1.373(3) . ? C113 H113 0.9600 . ? C114 C115 1.389(2) . ? C114 H114 0.9600 . ? C115 H115 0.9600 . ? C12 C121 1.3436(16) . ? C12 Al1 2.0259(11) . ? C121 C122 1.5137(15) . ? C121 H121 0.9600 . ? C122 C124 1.5167(19) . ? C122 C123 1.5247(19) . ? C122 C125 1.529(2) . ? C123 H12A 0.9599 . ? C123 H12B 0.9599 . ? C123 H12C 0.9599 . ? C124 H12D 0.9599 . ? C124 H12E 0.9599 . ? C124 H12F 0.9599 . ? C125 H12G 0.9599 . ? C125 H12H 0.9599 . ? C125 H12I 0.9599 . ? C13 C131 1.524(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C131 H13C 0.9599 . ? C131 H13D 0.9599 . ? C131 H13E 0.9599 . ? C14 O1 1.2297(14) . ? C14 N1 1.3337(15) . ? N1 C17 1.4405(14) . ? N1 Al1 1.9277(10) . ? C17 C171 1.3862(18) . ? C17 C175 1.3865(18) . ? C171 C172 1.3893(18) . ? C171 H171 0.9600 . ? C172 C173 1.384(2) . ? C172 H172 0.9600 . ? C173 C174 1.378(2) . ? C173 H173 0.9600 . ? C174 C175 1.3930(17) . ? C174 H174 0.9600 . ? C175 H175 0.9600 . ? Al1 C15 1.9777(14) . ? Al1 C16 1.9810(14) . ? C15 C151 1.531(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C151 H15C 0.9599 . ? C151 H15D 0.9599 . ? C151 H15E 0.9599 . ? C16 C161 1.529(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C161 H16C 0.9599 . ? C161 H16D 0.9599 . ? C161 H16E 0.9599 . ? 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 C12 P1 C11 113.74(6) . . ? C12 P1 C13 120.65(6) . . ? C11 P1 C13 109.75(6) . . ? C12 P1 C14 103.96(5) . . ? C11 P1 C14 105.13(5) . . ? C13 P1 C14 101.43(6) . . ? C115 C11 C111 119.87(12) . . ? C115 C11 P1 120.97(10) . . ? C111 C11 P1 119.13(9) . . ? C112 C111 C11 119.76(13) . . ? C112 C111 H111 120.1 . . ? C11 C111 H111 120.1 . . ? C113 C112 C111 120.24(14) . . ? C113 C112 H112 119.9 . . ? C111 C112 H112 119.9 . . ? C114 C113 C112 120.21(14) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C115 120.48(14) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C114 C115 C11 119.44(14) . . ? C114 C115 H115 120.3 . . ? C11 C115 H115 120.3 . . ? C121 C12 P1 131.48(9) . . ? C121 C12 Al1 120.47(8) . . ? P1 C12 Al1 107.97(6) . . ? C12 C121 C122 135.87(11) . . ? C12 C121 H121 112.1 . . ? C122 C121 H121 112.1 . . ? C121 C122 C124 114.76(10) . . ? C121 C122 C123 107.89(10) . . ? C124 C122 C123 108.85(12) . . ? C121 C122 C125 106.25(11) . . ? C124 C122 C125 110.16(14) . . ? C123 C122 C125 108.75(13) . . ? C122 C123 H12A 109.5 . . ? C122 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C122 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C122 C124 H12D 109.5 . . ? C122 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C131 C13 P1 111.67(9) . . ? C131 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C131 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C131 H13C 109.5 . . ? C13 C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C13 C131 H13E 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? O1 C14 N1 130.17(11) . . ? O1 C14 P1 116.73(9) . . ? N1 C14 P1 113.10(8) . . ? C14 N1 C17 117.39(9) . . ? C14 N1 Al1 121.10(8) . . ? C17 N1 Al1 120.94(7) . . ? C171 C17 C175 119.72(11) . . ? C171 C17 N1 120.61(11) . . ? C175 C17 N1 119.62(11) . . ? C17 C171 C172 119.90(13) . . ? C17 C171 H171 120.0 . . ? C172 C171 H171 120.0 . . ? C173 C172 C171 120.47(14) . . ? C173 C172 H172 119.8 . . ? C171 C172 H172 119.8 . . ? C174 C173 C172 119.60(12) . . ? C174 C173 H173 120.2 . . ? C172 C173 H173 120.2 . . ? C173 C174 C175 120.38(14) . . ? C173 C174 H174 119.8 . . ? C175 C174 H174 119.8 . . ? C17 C175 C174 119.93(13) . . ? C17 C175 H175 120.0 . . ? C174 C175 H175 120.0 . . ? N1 Al1 C15 112.22(5) . . ? N1 Al1 C16 108.18(5) . . ? C15 Al1 C16 119.13(6) . . ? N1 Al1 C12 92.71(4) . . ? C15 Al1 C12 110.78(5) . . ? C16 Al1 C12 110.66(5) . . ? C151 C15 Al1 113.70(9) . . ? C151 C15 H15A 108.8 . . ? Al1 C15 H15A 108.8 . . ? C151 C15 H15B 108.8 . . ? Al1 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C151 H15C 109.5 . . ? C15 C151 H15D 109.5 . . ? H15C C151 H15D 109.5 . . ? C15 C151 H15E 109.5 . . ? H15C C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? C161 C16 Al1 114.12(10) . . ? C161 C16 H16A 108.7 . . ? Al1 C16 H16A 108.7 . . ? C161 C16 H16B 108.7 . . ? Al1 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C161 H16C 109.5 . . ? C16 C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C16 C161 H16E 109.5 . . ? H16C C161 H16E 109.5 . . ? H16D C161 H16E 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 C12 P1 C11 C115 -163.90(10) . . . . ? C13 P1 C11 C115 -25.35(12) . . . . ? C14 P1 C11 C115 83.02(11) . . . . ? C12 P1 C11 C111 18.27(11) . . . . ? C13 P1 C11 C111 156.82(10) . . . . ? C14 P1 C11 C111 -94.81(10) . . . . ? C115 C11 C111 C112 0.51(19) . . . . ? P1 C11 C111 C112 178.36(10) . . . . ? C11 C111 C112 C113 0.2(2) . . . . ? C111 C112 C113 C114 -0.4(2) . . . . ? C112 C113 C114 C115 -0.1(2) . . . . ? C113 C114 C115 C11 0.7(2) . . . . ? C111 C11 C115 C114 -0.9(2) . . . . ? P1 C11 C115 C114 -178.75(11) . . . . ? C11 P1 C12 C121 71.10(13) . . . . ? C13 P1 C12 C121 -62.51(14) . . . . ? C14 P1 C12 C121 -175.12(12) . . . . ? C11 P1 C12 Al1 -105.52(6) . . . . ? C13 P1 C12 Al1 120.87(7) . . . . ? C14 P1 C12 Al1 8.25(7) . . . . ? P1 C12 C121 C122 -1.1(2) . . . . ? Al1 C12 C121 C122 175.21(12) . . . . ? C12 C121 C122 C124 6.7(2) . . . . ? C12 C121 C122 C123 128.21(16) . . . . ? C12 C121 C122 C125 -115.31(17) . . . . ? C12 P1 C13 C131 -35.54(13) . . . . ? C11 P1 C13 C131 -170.76(10) . . . . ? C14 P1 C13 C131 78.41(11) . . . . ? C12 P1 C14 O1 177.32(9) . . . . ? C11 P1 C14 O1 -62.88(10) . . . . ? C13 P1 C14 O1 51.44(11) . . . . ? C12 P1 C14 N1 -2.30(10) . . . . ? C11 P1 C14 N1 117.50(9) . . . . ? C13 P1 C14 N1 -128.19(9) . . . . ? O1 C14 N1 C17 3.28(19) . . . . ? P1 C14 N1 C17 -177.17(8) . . . . ? O1 C14 N1 Al1 174.71(10) . . . . ? P1 C14 N1 Al1 -5.73(12) . . . . ? C14 N1 C17 C171 69.05(15) . . . . ? Al1 N1 C17 C171 -102.39(12) . . . . ? C14 N1 C17 C175 -113.42(13) . . . . ? Al1 N1 C17 C175 75.13(13) . . . . ? C175 C17 C171 C172 0.36(19) . . . . ? N1 C17 C171 C172 177.88(11) . . . . ? C17 C171 C172 C173 0.2(2) . . . . ? C171 C172 C173 C174 -0.7(2) . . . . ? C172 C173 C174 C175 0.6(2) . . . . ? C171 C17 C175 C174 -0.46(18) . . . . ? N1 C17 C175 C174 -178.00(11) . . . . ? C173 C174 C175 C17 -0.03(19) . . . . ? C14 N1 Al1 C15 123.62(10) . . . . ? C17 N1 Al1 C15 -65.25(11) . . . . ? C14 N1 Al1 C16 -102.93(10) . . . . ? C17 N1 Al1 C16 68.20(10) . . . . ? C14 N1 Al1 C12 9.85(10) . . . . ? C17 N1 Al1 C12 -179.01(10) . . . . ? C121 C12 Al1 N1 173.15(10) . . . . ? P1 C12 Al1 N1 -9.79(6) . . . . ? C121 C12 Al1 C15 58.13(11) . . . . ? P1 C12 Al1 C15 -124.80(6) . . . . ? C121 C12 Al1 C16 -76.26(11) . . . . ? P1 C12 Al1 C16 100.81(7) . . . . ? N1 Al1 C15 C151 -62.38(12) . . . . ? C16 Al1 C15 C151 169.78(10) . . . . ? C12 Al1 C15 C151 39.73(12) . . . . ? N1 Al1 C16 C161 156.61(10) . . . . ? C15 Al1 C16 C161 -73.69(12) . . . . ? C12 Al1 C16 C161 56.41(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.339 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.037 # Attachment 'Compoundtrans-7.cif' data_Compoundtrans-7 _database_code_depnum_ccdc_archive 'CCDC 861404' #TrackingRef 'Compoundtrans-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 Al N O P' _chemical_formula_weight 423.49 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' Al Al 0.0645 0.0514 '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' _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 12.8546(5) _cell_length_b 12.3967(9) _cell_length_c 16.4403(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.714(3) _cell_angle_gamma 90.00 _cell_volume 2450.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 36289 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9466 _exptl_absorpt_correction_T_max 0.9759 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'imaging plate detector system' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27512 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.02 _reflns_number_total 5885 _reflns_number_gt 4263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0921P)^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 5885 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.002 _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 0.15873(3) 0.22269(4) 0.21266(3) 0.03960(13) Uani 1 1 d . . . C11 C 0.17632(14) 0.27690(15) 0.11669(11) 0.0424(4) Uani 1 1 d . . . C111 C 0.08391(16) 0.31211(18) 0.04764(13) 0.0522(5) Uani 1 1 d . . . H111 H 0.0116 0.3046 0.0503 0.063 Uiso 1 1 calc R . . C112 C 0.09694(18) 0.35775(19) -0.02437(14) 0.0592(5) Uani 1 1 d . . . H112 H 0.0335 0.3814 -0.0714 0.071 Uiso 1 1 calc R . . C113 C 0.20167(18) 0.36939(18) -0.02865(14) 0.0573(5) Uani 1 1 d . . . H113 H 0.2105 0.4009 -0.0785 0.069 Uiso 1 1 calc R . . C114 C 0.29272(18) 0.3353(2) 0.03927(15) 0.0660(6) Uani 1 1 d . . . H114 H 0.3648 0.3435 0.0364 0.079 Uiso 1 1 calc R . . C115 C 0.28105(17) 0.2891(2) 0.11197(14) 0.0587(5) Uani 1 1 d . . . H115 H 0.3449 0.2657 0.1587 0.070 Uiso 1 1 calc R . . C12 C 0.02675(13) 0.16186(15) 0.19050(11) 0.0404(4) Uani 1 1 d . . . C121 C 0.01899(14) 0.05949(15) 0.16099(11) 0.0430(4) Uani 1 1 d . . . H121 H 0.0838 0.0312 0.1537 0.052 Uiso 1 1 calc R . . C122 C -0.07940(14) -0.01586(16) 0.13805(12) 0.0462(4) Uani 1 1 d . . . C123 C -0.17962(16) 0.03317(18) 0.15334(14) 0.0555(5) Uani 1 1 d . . . H12A H -0.1579 0.0567 0.2140 0.083 Uiso 1 1 calc R . . H12B H -0.2388 -0.0209 0.1412 0.083 Uiso 1 1 calc R . . H12C H -0.2067 0.0953 0.1147 0.083 Uiso 1 1 calc R . . C124 C -0.11052(17) -0.04681(19) 0.04210(14) 0.0586(5) Uani 1 1 d . . . H12D H -0.1326 0.0180 0.0059 0.088 Uiso 1 1 calc R . . H12E H -0.1726 -0.0980 0.0259 0.088 Uiso 1 1 calc R . . H12F H -0.0463 -0.0802 0.0331 0.088 Uiso 1 1 calc R . . C125 C -0.0413(2) -0.11721(19) 0.19399(17) 0.0652(6) Uani 1 1 d . . . H12G H 0.0234 -0.1482 0.1842 0.098 Uiso 1 1 calc R . . H12H H -0.1018 -0.1701 0.1780 0.098 Uiso 1 1 calc R . . H12I H -0.0211 -0.0981 0.2555 0.098 Uiso 1 1 calc R . . C13 C 0.27787(15) 0.14086(16) 0.27091(13) 0.0499(4) Uani 1 1 d . . . H13A H 0.2840 0.0811 0.2329 0.060 Uiso 1 1 calc R . . H13B H 0.3461 0.1853 0.2854 0.060 Uiso 1 1 calc R . . C131 C 0.27015(18) 0.0944(2) 0.35379(16) 0.0673(6) Uani 1 1 d . . . H13C H 0.2700 0.1533 0.3936 0.101 Uiso 1 1 calc R . . H13D H 0.3341 0.0473 0.3815 0.101 Uiso 1 1 calc R . . H13E H 0.2013 0.0527 0.3400 0.101 Uiso 1 1 calc R . . C14 C 0.15989(14) 0.34259(15) 0.28030(11) 0.0417(4) Uani 1 1 d . . . O2 O 0.24945(10) 0.38757(12) 0.31878(9) 0.0515(3) Uani 1 1 d . . . N1 N 0.05651(11) 0.36817(12) 0.27449(9) 0.0410(3) Uani 1 1 d . . . C17 C 0.04011(14) 0.46308(15) 0.31843(12) 0.0421(4) Uani 1 1 d . . . C171 C -0.03794(15) 0.53778(16) 0.27124(13) 0.0490(4) Uani 1 1 d . . . H171 H -0.0739 0.5286 0.2103 0.059 Uiso 1 1 calc R . . C172 C -0.06404(17) 0.62622(17) 0.31253(15) 0.0567(5) Uani 1 1 d . . . H172 H -0.1184 0.6767 0.2798 0.068 Uiso 1 1 calc R . . C173 C -0.01150(17) 0.64084(18) 0.40039(15) 0.0581(5) Uani 1 1 d . . . H173 H -0.0300 0.7006 0.4289 0.070 Uiso 1 1 calc R . . C174 C 0.06847(18) 0.56786(19) 0.44688(14) 0.0607(5) Uani 1 1 d . . . H174 H 0.1063 0.5787 0.5074 0.073 Uiso 1 1 calc R . . C175 C 0.09450(16) 0.47890(17) 0.40649(13) 0.0522(5) Uani 1 1 d . . . H175 H 0.1495 0.4291 0.4393 0.063 Uiso 1 1 calc R . . Al2 Al -0.06970(4) 0.26967(5) 0.22403(4) 0.04434(16) Uani 1 1 d . . . C16 C -0.10898(17) 0.23009(19) 0.32629(14) 0.0579(5) Uani 1 1 d . . . H16A H -0.1215 0.2968 0.3546 0.070 Uiso 1 1 calc R . . H16B H -0.1794 0.1888 0.3064 0.070 Uiso 1 1 calc R . . C161 C -0.0192(2) 0.1628(2) 0.39301(15) 0.0723(7) Uani 1 1 d . . . H16C H -0.0081 0.0955 0.3659 0.108 Uiso 1 1 calc R . . H16D H -0.0426 0.1462 0.4422 0.108 Uiso 1 1 calc R . . H16E H 0.0506 0.2036 0.4136 0.108 Uiso 1 1 calc R . . C15 C -0.18532(16) 0.33704(18) 0.12010(15) 0.0587(5) Uani 1 1 d . . . H15A H -0.1484 0.3924 0.0963 0.070 Uiso 1 1 calc R . . H15B H -0.2139 0.2807 0.0750 0.070 Uiso 1 1 calc R . . C151 C -0.28439(17) 0.3896(2) 0.13488(18) 0.0690(6) Uani 1 1 d . . . H15C H -0.3205 0.3368 0.1606 0.103 Uiso 1 1 calc R . . H15D H -0.3377 0.4146 0.0792 0.103 Uiso 1 1 calc R . . H15E H -0.2587 0.4511 0.1744 0.103 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 P1 0.0311(2) 0.0482(3) 0.0409(2) -0.00068(19) 0.01451(17) -0.00032(17) C11 0.0396(8) 0.0499(10) 0.0414(9) -0.0044(8) 0.0189(7) -0.0020(7) C111 0.0391(9) 0.0667(12) 0.0522(11) 0.0038(9) 0.0177(8) 0.0000(8) C112 0.0512(11) 0.0720(14) 0.0539(12) 0.0088(10) 0.0180(9) 0.0029(10) C113 0.0620(12) 0.0651(13) 0.0524(11) 0.0065(9) 0.0296(10) 0.0030(10) C114 0.0469(11) 0.0940(17) 0.0664(14) 0.0137(12) 0.0315(10) 0.0014(11) C115 0.0396(10) 0.0840(15) 0.0548(11) 0.0099(11) 0.0197(8) 0.0021(9) C12 0.0323(7) 0.0514(10) 0.0393(8) -0.0007(7) 0.0146(6) 0.0001(7) C121 0.0352(8) 0.0519(10) 0.0438(9) -0.0027(8) 0.0163(7) -0.0012(7) C122 0.0375(9) 0.0514(10) 0.0509(10) -0.0045(8) 0.0172(8) -0.0057(7) C123 0.0415(10) 0.0657(13) 0.0632(12) -0.0120(10) 0.0234(9) -0.0109(9) C124 0.0495(11) 0.0704(14) 0.0585(12) -0.0152(10) 0.0226(9) -0.0118(10) C125 0.0612(13) 0.0579(12) 0.0748(15) 0.0078(11) 0.0220(11) -0.0072(10) C13 0.0349(8) 0.0551(11) 0.0575(11) 0.0027(9) 0.0137(8) 0.0021(8) C131 0.0485(11) 0.0807(16) 0.0685(14) 0.0217(12) 0.0154(10) 0.0066(11) C14 0.0357(8) 0.0497(10) 0.0410(9) -0.0007(7) 0.0150(7) -0.0021(7) O2 0.0371(6) 0.0611(8) 0.0573(8) -0.0115(6) 0.0177(6) -0.0079(6) N1 0.0348(7) 0.0487(8) 0.0395(7) -0.0041(6) 0.0132(6) 0.0002(6) C17 0.0345(8) 0.0494(10) 0.0445(9) -0.0032(7) 0.0164(7) -0.0033(7) C171 0.0415(9) 0.0554(11) 0.0472(10) -0.0010(8) 0.0121(8) -0.0004(8) C172 0.0447(10) 0.0543(11) 0.0690(13) -0.0034(10) 0.0176(9) 0.0044(8) C173 0.0488(11) 0.0597(12) 0.0676(13) -0.0183(10) 0.0230(10) -0.0037(9) C174 0.0578(12) 0.0723(14) 0.0485(11) -0.0171(10) 0.0144(9) 0.0008(10) C175 0.0489(10) 0.0597(11) 0.0443(10) -0.0056(9) 0.0118(8) 0.0053(9) Al2 0.0318(3) 0.0542(3) 0.0477(3) -0.0072(2) 0.0149(2) -0.0007(2) C16 0.0495(11) 0.0714(14) 0.0620(12) -0.0162(11) 0.0309(10) -0.0105(10) C161 0.0696(15) 0.1007(19) 0.0545(13) -0.0004(13) 0.0318(11) -0.0107(13) C15 0.0421(10) 0.0586(12) 0.0671(13) -0.0081(10) 0.0090(9) 0.0031(9) C151 0.0419(11) 0.0713(14) 0.0923(17) 0.0098(13) 0.0219(11) 0.0032(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C12 1.7727(17) . ? P1 C11 1.8012(18) . ? P1 C13 1.8040(19) . ? P1 C14 1.8532(19) . ? C11 C115 1.384(3) . ? C11 C111 1.392(3) . ? C111 C112 1.375(3) . ? C111 H111 0.9500 . ? C112 C113 1.380(3) . ? C112 H112 0.9500 . ? C113 C114 1.368(3) . ? C113 H113 0.9500 . ? C114 C115 1.381(3) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C12 C121 1.350(3) . ? C12 Al2 2.0275(18) . ? C121 C122 1.509(2) . ? C121 H121 0.9500 . ? C122 C123 1.524(3) . ? C122 C125 1.531(3) . ? C122 C124 1.533(3) . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 H12D 0.9800 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C13 C131 1.514(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C14 O2 1.233(2) . ? C14 N1 1.336(2) . ? N1 C17 1.435(2) . ? N1 Al2 1.9645(15) . ? C17 C175 1.381(3) . ? C17 C171 1.384(3) . ? C171 C172 1.392(3) . ? C171 H171 0.9500 . ? C172 C173 1.373(3) . ? C172 H172 0.9500 . ? C173 C174 1.380(3) . ? C173 H173 0.9500 . ? C174 C175 1.388(3) . ? C174 H174 0.9500 . ? C175 H175 0.9500 . ? Al2 C16 1.981(2) . ? Al2 C15 2.007(2) . ? C16 C161 1.528(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C161 H16C 0.9800 . ? C161 H16D 0.9800 . ? C161 H16E 0.9800 . ? C15 C151 1.524(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C151 H15C 0.9800 . ? C151 H15D 0.9800 . ? C151 H15E 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 C12 P1 C11 112.72(8) . . ? C12 P1 C13 116.17(9) . . ? C11 P1 C13 109.19(9) . . ? C12 P1 C14 105.58(8) . . ? C11 P1 C14 104.45(8) . . ? C13 P1 C14 107.90(9) . . ? C115 C11 C111 119.11(17) . . ? C115 C11 P1 121.07(15) . . ? C111 C11 P1 119.75(13) . . ? C112 C111 C11 120.18(18) . . ? C112 C111 H111 119.9 . . ? C11 C111 H111 119.9 . . ? C111 C112 C113 120.3(2) . . ? C111 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C114 C113 C112 119.6(2) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C113 C114 C115 120.75(19) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C114 C115 C11 119.98(19) . . ? C114 C115 H115 120.0 . . ? C11 C115 H115 120.0 . . ? C121 C12 P1 114.68(13) . . ? C121 C12 Al2 137.99(13) . . ? P1 C12 Al2 107.25(9) . . ? C12 C121 C122 128.37(16) . . ? C12 C121 H121 115.8 . . ? C122 C121 H121 115.8 . . ? C121 C122 C123 113.25(16) . . ? C121 C122 C125 107.22(16) . . ? C123 C122 C125 109.74(17) . . ? C121 C122 C124 107.62(15) . . ? C123 C122 C124 109.97(16) . . ? C125 C122 C124 108.92(18) . . ? C122 C123 H12A 109.5 . . ? C122 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C122 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C122 C124 H12D 109.5 . . ? C122 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C122 C125 H12G 109.5 . . ? C122 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C122 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C131 C13 P1 112.19(14) . . ? C131 C13 H13A 109.2 . . ? P1 C13 H13A 109.2 . . ? C131 C13 H13B 109.2 . . ? P1 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C131 H13C 109.5 . . ? C13 C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C13 C131 H13E 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? O2 C14 N1 130.81(17) . . ? O2 C14 P1 118.58(13) . . ? N1 C14 P1 110.52(12) . . ? C14 N1 C17 118.56(14) . . ? C14 N1 Al2 122.32(12) . . ? C17 N1 Al2 118.42(11) . . ? C175 C17 C171 119.36(18) . . ? C175 C17 N1 122.29(17) . . ? C171 C17 N1 118.23(16) . . ? C17 C171 C172 120.39(18) . . ? C17 C171 H171 119.8 . . ? C172 C171 H171 119.8 . . ? C173 C172 C171 120.2(2) . . ? C173 C172 H172 119.9 . . ? C171 C172 H172 119.9 . . ? C172 C173 C174 119.3(2) . . ? C172 C173 H173 120.4 . . ? C174 C173 H173 120.4 . . ? C173 C174 C175 120.96(19) . . ? C173 C174 H174 119.5 . . ? C175 C174 H174 119.5 . . ? C17 C175 C174 119.74(19) . . ? C17 C175 H175 120.1 . . ? C174 C175 H175 120.1 . . ? N1 Al2 C16 102.47(8) . . ? N1 Al2 C15 110.68(8) . . ? C16 Al2 C15 119.43(10) . . ? N1 Al2 C12 91.80(7) . . ? C16 Al2 C12 115.56(9) . . ? C15 Al2 C12 112.50(9) . . ? C161 C16 Al2 112.96(14) . . ? C161 C16 H16A 109.0 . . ? Al2 C16 H16A 109.0 . . ? C161 C16 H16B 109.0 . . ? Al2 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C161 H16C 109.5 . . ? C16 C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C16 C161 H16E 109.5 . . ? H16C C161 H16E 109.5 . . ? H16D C161 H16E 109.5 . . ? C151 C15 Al2 116.80(18) . . ? C151 C15 H15A 108.1 . . ? Al2 C15 H15A 108.1 . . ? C151 C15 H15B 108.1 . . ? Al2 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C15 C151 H15C 109.5 . . ? C15 C151 H15D 109.5 . . ? H15C C151 H15D 109.5 . . ? C15 C151 H15E 109.5 . . ? H15C C151 H15E 109.5 . . ? H15D C151 H15E 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 C12 P1 C11 C115 -154.82(17) . . . . ? C13 P1 C11 C115 -24.1(2) . . . . ? C14 P1 C11 C115 91.07(18) . . . . ? C12 P1 C11 C111 28.38(19) . . . . ? C13 P1 C11 C111 159.07(16) . . . . ? C14 P1 C11 C111 -85.74(17) . . . . ? C115 C11 C111 C112 0.4(3) . . . . ? P1 C11 C111 C112 177.28(17) . . . . ? C11 C111 C112 C113 -0.2(3) . . . . ? C111 C112 C113 C114 -0.1(4) . . . . ? C112 C113 C114 C115 0.2(4) . . . . ? C113 C114 C115 C11 0.0(4) . . . . ? C111 C11 C115 C114 -0.3(3) . . . . ? P1 C11 C115 C114 -177.10(19) . . . . ? C11 P1 C12 C121 82.52(16) . . . . ? C13 P1 C12 C121 -44.56(17) . . . . ? C14 P1 C12 C121 -164.06(14) . . . . ? C11 P1 C12 Al2 -100.20(10) . . . . ? C13 P1 C12 Al2 132.73(10) . . . . ? C14 P1 C12 Al2 13.22(10) . . . . ? P1 C12 C121 C122 178.47(15) . . . . ? Al2 C12 C121 C122 2.3(3) . . . . ? C12 C121 C122 C123 -1.5(3) . . . . ? C12 C121 C122 C125 -122.7(2) . . . . ? C12 C121 C122 C124 120.3(2) . . . . ? C12 P1 C13 C131 -52.50(19) . . . . ? C11 P1 C13 C131 178.69(16) . . . . ? C14 P1 C13 C131 65.74(18) . . . . ? C12 P1 C14 O2 166.08(15) . . . . ? C11 P1 C14 O2 -74.85(16) . . . . ? C13 P1 C14 O2 41.25(17) . . . . ? C12 P1 C14 N1 -16.90(15) . . . . ? C11 P1 C14 N1 102.17(13) . . . . ? C13 P1 C14 N1 -141.73(13) . . . . ? O2 C14 N1 C17 0.3(3) . . . . ? P1 C14 N1 C17 -176.28(12) . . . . ? O2 C14 N1 Al2 -169.94(16) . . . . ? P1 C14 N1 Al2 13.51(18) . . . . ? C14 N1 C17 C175 -55.7(2) . . . . ? Al2 N1 C17 C175 114.90(17) . . . . ? C14 N1 C17 C171 128.15(18) . . . . ? Al2 N1 C17 C171 -61.3(2) . . . . ? C175 C17 C171 C172 -2.0(3) . . . . ? N1 C17 C171 C172 174.24(17) . . . . ? C17 C171 C172 C173 0.8(3) . . . . ? C171 C172 C173 C174 1.0(3) . . . . ? C172 C173 C174 C175 -1.5(3) . . . . ? C171 C17 C175 C174 1.5(3) . . . . ? N1 C17 C175 C174 -174.61(18) . . . . ? C173 C174 C175 C17 0.3(3) . . . . ? C14 N1 Al2 C16 112.13(15) . . . . ? C17 N1 Al2 C16 -58.09(15) . . . . ? C14 N1 Al2 C15 -119.46(15) . . . . ? C17 N1 Al2 C15 70.32(15) . . . . ? C14 N1 Al2 C12 -4.56(15) . . . . ? C17 N1 Al2 C12 -174.78(13) . . . . ? C121 C12 Al2 N1 169.6(2) . . . . ? P1 C12 Al2 N1 -6.76(9) . . . . ? C121 C12 Al2 C16 64.8(2) . . . . ? P1 C12 Al2 C16 -111.50(10) . . . . ? C121 C12 Al2 C15 -77.2(2) . . . . ? P1 C12 Al2 C15 106.53(10) . . . . ? N1 Al2 C16 C161 -67.13(17) . . . . ? C15 Al2 C16 C161 170.19(16) . . . . ? C12 Al2 C16 C161 31.00(19) . . . . ? N1 Al2 C15 C151 -98.24(18) . . . . ? C16 Al2 C15 C151 20.3(2) . . . . ? C12 Al2 C15 C151 160.65(16) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.350 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.055 # Attachment 'Compound8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 861405' #TrackingRef 'Compound8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52.50 Al F N O P' _chemical_formula_weight 688.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.2157(4) _cell_length_b 14.10780(10) _cell_length_c 15.6568(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.3050(10) _cell_angle_gamma 90.00 _cell_volume 7809.60(14) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5961 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 67.50 _exptl_crystal_description octahedral _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2948 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7805 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21955 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 67.50 _reflns_number_total 6803 _reflns_number_gt 5961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker SAINT+' _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^)+(0.0873P)^2^+11.7288P] 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 6803 _refine_ls_number_parameters 478 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.055 _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 C1 C 0.16349(6) 0.27635(15) 0.27542(15) 0.0279(4) Uani 1 1 d . . . C2 C 0.19755(6) 0.30903(16) 0.28352(16) 0.0316(5) Uani 1 1 d . . . H2 H 0.2027 0.3744 0.3010 0.038 Uiso 1 1 calc R . . C31 C 0.22798(6) 0.25624(16) 0.26872(17) 0.0341(5) Uani 1 1 d . . . C32 C 0.26387(7) 0.2979(2) 0.2970(2) 0.0469(6) Uani 1 1 d . . . H32 H 0.2684 0.3581 0.3280 0.056 Uiso 1 1 calc R . . C33 C 0.29288(8) 0.2527(2) 0.2806(3) 0.0621(9) Uani 1 1 d . . . H33 H 0.3174 0.2816 0.3004 0.074 Uiso 1 1 calc R . . C34 C 0.28660(9) 0.1665(2) 0.2359(2) 0.0629(10) Uani 1 1 d . . . H34 H 0.3068 0.1355 0.2245 0.075 Uiso 1 1 calc R . . C35 C 0.25127(9) 0.1246(2) 0.2074(2) 0.0567(8) Uani 1 1 d . . . H35 H 0.2470 0.0645 0.1764 0.068 Uiso 1 1 calc R . . C36 C 0.22216(8) 0.16920(18) 0.22369(19) 0.0426(6) Uani 1 1 d . . . H36 H 0.1977 0.1398 0.2037 0.051 Uiso 1 1 calc R . . Al1 Al 0.140023(17) 0.14286(4) 0.26699(4) 0.02717(18) Uani 1 1 d . . . C4 C 0.16938(6) 0.04819(16) 0.36444(17) 0.0353(5) Uani 1 1 d . . . C41 C 0.18772(8) 0.09690(19) 0.45815(18) 0.0487(7) Uani 1 1 d . . . H41A H 0.2001 0.0504 0.5045 0.058 Uiso 1 1 calc R . . H41B H 0.1686 0.1285 0.4735 0.058 Uiso 1 1 calc R . . H41C H 0.2059 0.1424 0.4553 0.058 Uiso 1 1 calc R . . C42 C 0.13982(7) -0.02172(18) 0.3720(2) 0.0456(6) Uani 1 1 d . . . H42A H 0.1519 -0.0659 0.4211 0.055 Uiso 1 1 calc R . . H42B H 0.1284 -0.0555 0.3149 0.055 Uiso 1 1 calc R . . H42C H 0.1207 0.0126 0.3848 0.055 Uiso 1 1 calc R . . C43 C 0.19970(7) -0.00961(19) 0.3464(2) 0.0473(6) Uani 1 1 d . . . H43A H 0.2197 0.0317 0.3468 0.057 Uiso 1 1 calc R . . H43B H 0.1888 -0.0401 0.2873 0.057 Uiso 1 1 calc R . . H43C H 0.2097 -0.0567 0.3937 0.057 Uiso 1 1 calc R . . C5 C 0.11252(6) 0.09626(17) 0.13671(16) 0.0357(5) Uani 1 1 d . . . C51 C 0.12814(8) 0.00201(18) 0.11695(19) 0.0442(6) Uani 1 1 d . . . H51A H 0.1128 -0.0193 0.0560 0.053 Uiso 1 1 calc R . . H51B H 0.1278 -0.0446 0.1613 0.053 Uiso 1 1 calc R . . H51C H 0.1537 0.0110 0.1212 0.053 Uiso 1 1 calc R . . C52 C 0.07078(7) 0.0807(2) 0.1208(2) 0.0525(7) Uani 1 1 d . . . H52A H 0.0599 0.1393 0.1299 0.063 Uiso 1 1 calc R . . H52B H 0.0689 0.0342 0.1636 0.063 Uiso 1 1 calc R . . H52C H 0.0574 0.0587 0.0588 0.063 Uiso 1 1 calc R . . C53 C 0.11400(9) 0.1681(2) 0.06437(18) 0.0502(7) Uani 1 1 d . . . H53A H 0.1398 0.1784 0.0719 0.060 Uiso 1 1 calc R . . H53B H 0.1030 0.2270 0.0724 0.060 Uiso 1 1 calc R . . H53C H 0.1001 0.1438 0.0036 0.060 Uiso 1 1 calc R . . O1 O 0.10580(4) 0.18765(10) 0.31566(10) 0.0290(3) Uani 1 1 d . . . C6 C 0.10743(6) 0.27481(14) 0.34623(15) 0.0269(4) Uani 1 1 d . . . N1 N 0.09762(5) 0.31045(12) 0.40853(13) 0.0301(4) Uani 1 1 d . . . C71 C 0.07951(7) 0.25547(15) 0.45581(17) 0.0353(5) Uani 1 1 d . . . C72 C 0.05347(7) 0.18381(19) 0.41515(19) 0.0415(6) Uani 1 1 d . . . H72 H 0.0488 0.1644 0.3530 0.050 Uiso 1 1 calc R . . C73 C 0.03413(8) 0.1401(2) 0.4636(2) 0.0502(7) Uani 1 1 d . . . H73 H 0.0159 0.0917 0.4342 0.060 Uiso 1 1 calc R . . C74 C 0.04074(11) 0.1651(2) 0.5521(3) 0.0655(10) Uani 1 1 d . . . H74 H 0.0271 0.1350 0.5850 0.079 Uiso 1 1 calc R . . C75 C 0.06727(15) 0.2342(2) 0.5944(3) 0.0910(15) Uani 1 1 d . . . H75 H 0.0729 0.2504 0.6578 0.109 Uiso 1 1 calc R . . C76 C 0.08597(12) 0.2805(2) 0.5452(2) 0.0690(10) Uani 1 1 d . . . H76 H 0.1035 0.3305 0.5742 0.083 Uiso 1 1 calc R . . P1 P 0.129309(14) 0.35616(3) 0.28886(4) 0.02520(16) Uani 1 1 d . . . C81 C 0.14655(6) 0.46173(14) 0.35899(15) 0.0273(4) Uani 1 1 d . . . C82 C 0.12834(6) 0.55085(15) 0.33450(15) 0.0300(5) Uani 1 1 d . . . C83 C 0.14651(7) 0.63077(16) 0.38368(17) 0.0348(5) Uani 1 1 d . . . H83 H 0.1344 0.6914 0.3669 0.042 Uiso 1 1 calc R . . C84 C 0.18150(7) 0.62576(17) 0.45606(17) 0.0368(5) Uani 1 1 d . . . C85 C 0.19699(7) 0.53711(17) 0.48441(17) 0.0362(5) Uani 1 1 d . . . H85 H 0.2203 0.5325 0.5373 0.043 Uiso 1 1 calc R . . C86 C 0.17999(6) 0.45418(16) 0.43895(16) 0.0310(5) Uani 1 1 d . . . C821 C 0.08927(7) 0.56575(17) 0.26183(18) 0.0393(5) Uani 1 1 d . . . H82A H 0.0785 0.6223 0.2756 0.047 Uiso 1 1 calc R . . H82B H 0.0736 0.5124 0.2613 0.047 Uiso 1 1 calc R . . H82C H 0.0909 0.5720 0.2024 0.047 Uiso 1 1 calc R . . C841 C 0.20136(9) 0.71433(19) 0.5042(2) 0.0543(7) Uani 1 1 d . . . H84A H 0.2214 0.6975 0.5613 0.065 Uiso 1 1 calc R . . H84B H 0.1836 0.7547 0.5167 0.065 Uiso 1 1 calc R . . H84C H 0.2117 0.7472 0.4654 0.065 Uiso 1 1 calc R . . C861 C 0.19732(7) 0.36168(16) 0.48336(18) 0.0388(6) Uani 1 1 d . . . H86A H 0.2185 0.3469 0.4671 0.047 Uiso 1 1 calc R . . H86B H 0.1788 0.3121 0.4620 0.047 Uiso 1 1 calc R . . H86C H 0.2056 0.3672 0.5492 0.047 Uiso 1 1 calc R . . C91 C 0.09612(6) 0.38463(15) 0.17224(15) 0.0287(5) Uani 1 1 d . . . C92 C 0.05727(6) 0.36209(15) 0.13892(16) 0.0323(5) Uani 1 1 d . . . C93 C 0.03510(7) 0.38359(19) 0.04735(17) 0.0426(6) Uani 1 1 d . . . H93 H 0.0088 0.3663 0.0239 0.051 Uiso 1 1 calc R . . C94 C 0.04927(8) 0.4287(2) -0.01129(17) 0.0502(7) Uani 1 1 d . . . C95 C 0.08726(8) 0.45271(19) 0.02358(18) 0.0452(6) Uani 1 1 d . . . H95 H 0.0975 0.4848 -0.0158 0.054 Uiso 1 1 calc R . . C96 C 0.11100(7) 0.43193(16) 0.11345(16) 0.0352(5) Uani 1 1 d . . . C921 C 0.03661(6) 0.32134(17) 0.19559(17) 0.0377(5) Uani 1 1 d . . . H92A H 0.0099 0.3208 0.1595 0.045 Uiso 1 1 calc R . . H92B H 0.0416 0.3595 0.2497 0.045 Uiso 1 1 calc R . . H92C H 0.0452 0.2578 0.2136 0.045 Uiso 1 1 calc R . . C941 C 0.02404(11) 0.4543(3) -0.1084(2) 0.0844(13) Uani 1 1 d . . . H94A H 0.0286 0.4116 -0.1508 0.101 Uiso 1 1 calc R . . H94B H 0.0293 0.5180 -0.1214 0.101 Uiso 1 1 calc R . . H94C H -0.0019 0.4497 -0.1150 0.101 Uiso 1 1 calc R . . C961 C 0.15124(8) 0.46557(17) 0.14290(19) 0.0424(6) Uani 1 1 d . . . H96A H 0.1667 0.4150 0.1357 0.051 Uiso 1 1 calc R . . H96B H 0.1604 0.4847 0.2065 0.051 Uiso 1 1 calc R . . H96C H 0.1523 0.5184 0.1053 0.051 Uiso 1 1 calc R . . C01 C 0.00705(10) -0.19827(18) 0.2402(3) 0.085(2) Uani 0.50 1 d PGU . 1 C02 C 0.03785(11) -0.1462(3) 0.2977(2) 0.084(2) Uani 0.50 1 d PGU . 1 C03 C 0.03381(17) -0.0501(3) 0.3116(3) 0.078(3) Uani 0.50 1 d PGU . 1 C04 C -0.0010(2) -0.0062(2) 0.2681(3) 0.060(2) Uani 0.50 1 d PGU . 1 C05 C -0.03183(16) -0.0584(3) 0.2106(4) 0.067(2) Uani 0.50 1 d PGU . 1 C06 C -0.02779(11) -0.1544(3) 0.1967(3) 0.087(3) Uani 0.50 1 d PGU . 1 F01 F 0.00982(13) -0.30290(19) 0.2127(4) 0.144(2) Uani 0.50 1 d PGU . 1 F02 F 0.06688(11) -0.1943(4) 0.3253(3) 0.064(2) Uani 0.25 1 d PGU . 1 F06 F -0.05069(10) -0.2216(4) 0.1407(5) 0.183(9) Uani 0.25 1 d PGU . 1 H03A H 0.0552 -0.0131 0.3507 0.120 Uiso 0.50 1 d P A 1 H04A H -0.0038 0.0608 0.2775 0.120 Uiso 0.50 1 d P B 1 H05A H -0.0559 -0.0277 0.1811 0.120 Uiso 0.50 1 d P C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0270(11) 0.0252(10) 0.0315(11) -0.0026(8) 0.0109(9) 0.0013(8) C2 0.0302(12) 0.0275(11) 0.0385(13) -0.0020(9) 0.0146(9) 0.0012(8) C31 0.0312(12) 0.0344(12) 0.0407(13) 0.0077(10) 0.0180(10) 0.0053(9) C32 0.0344(13) 0.0485(15) 0.0620(17) 0.0120(13) 0.0231(12) 0.0029(11) C33 0.0376(15) 0.071(2) 0.088(2) 0.0338(18) 0.0361(16) 0.0157(14) C34 0.0599(19) 0.068(2) 0.084(2) 0.0394(18) 0.0532(18) 0.0376(16) C35 0.074(2) 0.0438(15) 0.070(2) 0.0144(14) 0.0467(17) 0.0268(14) C36 0.0460(15) 0.0385(13) 0.0516(16) 0.0041(11) 0.0276(12) 0.0086(11) Al1 0.0250(3) 0.0224(3) 0.0336(4) -0.0027(2) 0.0105(3) 0.0007(2) C4 0.0328(12) 0.0274(11) 0.0427(13) 0.0030(9) 0.0109(10) 0.0022(9) C41 0.0521(16) 0.0376(14) 0.0430(15) 0.0050(11) 0.0028(12) 0.0034(11) C42 0.0459(15) 0.0332(13) 0.0581(17) 0.0081(11) 0.0200(13) -0.0017(11) C43 0.0384(14) 0.0379(13) 0.0622(17) 0.0117(12) 0.0155(12) 0.0118(11) C5 0.0329(12) 0.0327(12) 0.0394(13) -0.0098(10) 0.0112(10) -0.0003(9) C51 0.0451(14) 0.0395(14) 0.0468(15) -0.0135(11) 0.0164(11) 0.0018(11) C52 0.0357(14) 0.0546(17) 0.0604(18) -0.0263(14) 0.0107(12) -0.0048(12) C53 0.0645(18) 0.0443(15) 0.0364(14) -0.0058(11) 0.0131(12) 0.0031(13) O1 0.0281(8) 0.0224(7) 0.0386(9) -0.0019(6) 0.0149(6) -0.0011(6) C6 0.0225(10) 0.0241(10) 0.0322(11) 0.0008(8) 0.0082(8) 0.0001(8) N1 0.0319(10) 0.0255(9) 0.0363(10) 0.0014(7) 0.0166(8) 0.0014(7) C71 0.0417(13) 0.0253(11) 0.0467(14) 0.0064(9) 0.0255(11) 0.0084(9) C72 0.0316(12) 0.0467(14) 0.0467(15) 0.0104(11) 0.0152(11) -0.0006(10) C73 0.0412(15) 0.0443(15) 0.071(2) 0.0173(13) 0.0284(14) 0.0035(11) C74 0.099(3) 0.0347(15) 0.098(3) 0.0107(15) 0.077(2) 0.0045(15) C75 0.188(5) 0.0446(18) 0.088(3) -0.0167(17) 0.105(3) -0.028(2) C76 0.132(3) 0.0349(15) 0.068(2) -0.0165(14) 0.069(2) -0.0257(17) P1 0.0242(3) 0.0211(3) 0.0315(3) -0.00105(19) 0.0119(2) -0.00039(18) C81 0.0280(11) 0.0230(10) 0.0344(12) -0.0027(8) 0.0158(9) -0.0020(8) C82 0.0345(12) 0.0260(11) 0.0360(12) -0.0006(9) 0.0208(10) 0.0006(9) C83 0.0420(13) 0.0250(11) 0.0456(14) -0.0010(9) 0.0257(11) -0.0012(9) C84 0.0393(13) 0.0327(12) 0.0461(14) -0.0102(10) 0.0250(11) -0.0090(10) C85 0.0309(12) 0.0387(13) 0.0393(13) -0.0072(10) 0.0139(10) -0.0051(9) C86 0.0286(11) 0.0308(11) 0.0358(12) -0.0029(9) 0.0148(9) -0.0016(9) C821 0.0424(14) 0.0296(12) 0.0457(14) -0.0007(10) 0.0165(11) 0.0102(10) C841 0.0556(17) 0.0371(14) 0.073(2) -0.0205(13) 0.0271(15) -0.0137(12) C861 0.0353(13) 0.0351(13) 0.0389(14) -0.0006(10) 0.0062(10) 0.0025(10) C91 0.0335(11) 0.0216(10) 0.0314(11) -0.0019(8) 0.0128(9) 0.0036(8) C92 0.0328(12) 0.0264(11) 0.0359(12) -0.0035(9) 0.0112(9) 0.0055(8) C93 0.0372(13) 0.0479(14) 0.0371(14) -0.0057(11) 0.0077(10) 0.0128(11) C94 0.0598(18) 0.0591(17) 0.0319(14) 0.0030(12) 0.0174(12) 0.0277(14) C95 0.0626(18) 0.0430(14) 0.0399(14) 0.0091(11) 0.0305(13) 0.0202(12) C96 0.0469(14) 0.0263(11) 0.0395(13) -0.0008(9) 0.0244(11) 0.0062(10) C921 0.0253(11) 0.0373(13) 0.0459(14) 0.0029(10) 0.0082(10) 0.0000(9) C941 0.083(2) 0.133(4) 0.0356(17) 0.0149(19) 0.0204(16) 0.056(2) C961 0.0546(16) 0.0318(12) 0.0530(16) 0.0051(11) 0.0339(13) -0.0010(11) C01 0.055(5) 0.076(4) 0.141(7) 0.060(4) 0.055(4) 0.032(3) C02 0.060(4) 0.142(7) 0.062(5) 0.022(4) 0.038(3) 0.043(4) C03 0.053(4) 0.130(6) 0.046(4) 0.004(4) 0.013(3) 0.033(5) C04 0.066(3) 0.079(4) 0.016(5) 0.013(2) -0.007(4) 0.010(3) C05 0.047(4) 0.074(4) 0.064(5) 0.035(3) 0.003(3) 0.032(4) C06 0.029(3) 0.061(4) 0.162(9) 0.009(5) 0.028(4) -0.013(3) F01 0.156(6) 0.093(4) 0.193(7) 0.046(4) 0.079(5) 0.038(4) F02 0.069(5) 0.074(5) 0.034(3) -0.006(3) 0.001(3) 0.046(4) F06 0.101(9) 0.051(5) 0.30(2) 0.010(8) -0.034(10) -0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.341(3) . ? C1 P1 1.796(2) . ? C1 Al1 2.068(2) . ? C2 C31 1.472(3) . ? C2 H2 0.9600 . ? C31 C36 1.391(4) . ? C31 C32 1.401(3) . ? C32 C33 1.385(4) . ? C32 H32 0.9600 . ? C33 C34 1.379(5) . ? C33 H33 0.9600 . ? C34 C35 1.383(5) . ? C34 H34 0.9600 . ? C35 C36 1.383(4) . ? C35 H35 0.9600 . ? C36 H36 0.9600 . ? Al1 O1 1.8565(15) . ? Al1 C5 2.018(2) . ? Al1 C4 2.018(2) . ? C4 C41 1.528(4) . ? C4 C43 1.529(3) . ? C4 C42 1.538(3) . ? C41 H41A 0.9599 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? C42 H42A 0.9599 . ? C42 H42B 0.9599 . ? C42 H42C 0.9599 . ? C43 H43A 0.9599 . ? C43 H43B 0.9599 . ? C43 H43C 0.9599 . ? C5 C52 1.534(4) . ? C5 C51 1.536(3) . ? C5 C53 1.537(4) . ? C51 H51A 0.9599 . ? C51 H51B 0.9599 . ? C51 H51C 0.9599 . ? C52 H52A 0.9599 . ? C52 H52B 0.9599 . ? C52 H52C 0.9599 . ? C53 H53A 0.9599 . ? C53 H53B 0.9599 . ? C53 H53C 0.9599 . ? O1 C6 1.312(3) . ? C6 N1 1.274(3) . ? C6 P1 1.842(2) . ? N1 C71 1.421(3) . ? C71 C76 1.372(4) . ? C71 C72 1.392(4) . ? C72 C73 1.388(4) . ? C72 H72 0.9600 . ? C73 C74 1.358(5) . ? C73 H73 0.9600 . ? C74 C75 1.381(5) . ? C74 H74 0.9600 . ? C75 C76 1.396(4) . ? C75 H75 0.9600 . ? C76 H76 0.9600 . ? P1 C81 1.819(2) . ? P1 C91 1.829(2) . ? C81 C86 1.413(3) . ? C81 C82 1.418(3) . ? C82 C83 1.393(3) . ? C82 C821 1.509(3) . ? C83 C84 1.388(4) . ? C83 H83 0.9600 . ? C84 C85 1.383(4) . ? C84 C841 1.507(3) . ? C85 C86 1.395(3) . ? C85 H85 0.9600 . ? C86 C861 1.508(3) . ? C821 H82A 0.9599 . ? C821 H82B 0.9599 . ? C821 H82C 0.9599 . ? C841 H84A 0.9599 . ? C841 H84B 0.9599 . ? C841 H84C 0.9599 . ? C861 H86A 0.9599 . ? C861 H86B 0.9599 . ? C861 H86C 0.9599 . ? C91 C92 1.410(3) . ? C91 C96 1.419(3) . ? C92 C93 1.394(3) . ? C92 C921 1.508(3) . ? C93 C94 1.385(4) . ? C93 H93 0.9600 . ? C94 C95 1.385(4) . ? C94 C941 1.503(4) . ? C95 C96 1.386(4) . ? C95 H95 0.9600 . ? C96 C961 1.505(4) . ? C921 H92A 0.9599 . ? C921 H92B 0.9599 . ? C921 H92C 0.9599 . ? C941 H94A 0.9599 . ? C941 H94B 0.9599 . ? C941 H94C 0.9599 . ? C961 H96A 0.9599 . ? C961 H96B 0.9599 . ? C961 H96C 0.9599 . ? C01 C01 0.714(6) 2 ? C01 C06 1.180(6) 2 ? C01 C02 1.3900 . ? C01 C06 1.3900 . ? C01 F01 1.5526 . ? C01 C02 1.751(7) 2 ? C01 F01 1.871(6) 2 ? C02 C06 0.441(8) 2 ? C02 F02 1.2305 . ? C02 C05 1.257(2) 2 ? C02 C03 1.3900 . ? C02 F06 1.395(5) 2 ? C02 C01 1.751(7) 2 ? C03 C05 0.348(8) 2 ? C03 C04 1.3900 . ? C03 C06 1.4866(12) 2 ? C03 C04 1.525(11) 2 ? C03 H03A 0.9672 . ? C04 C04 0.601(10) 2 ? C04 C05 1.383(10) 2 ? C04 C05 1.3900 . ? C04 C03 1.525(10) 2 ? C04 H04A 0.9686 . ? C05 C03 0.348(10) 2 ? C05 C02 1.2575(14) 2 ? C05 C04 1.383(12) 2 ? C05 C06 1.3900 . ? C05 H05A 0.9616 . ? C06 C02 0.441(8) 2 ? C06 C01 1.180(7) 2 ? C06 F06 1.3605 . ? C06 C03 1.4866(17) 2 ? C06 F02 1.509(6) 2 ? F01 F01 1.611(11) 2 ? F01 C01 1.871(5) 2 ? F02 F06 1.032(10) 2 ? F02 C06 1.509(8) 2 ? F06 F02 1.032(12) 2 ? F06 C02 1.395(7) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 P1 119.76(16) . . ? C2 C1 Al1 134.50(16) . . ? P1 C1 Al1 105.15(10) . . ? C1 C2 C31 127.4(2) . . ? C1 C2 H2 116.3 . . ? C31 C2 H2 116.3 . . ? C36 C31 C32 118.7(2) . . ? C36 C31 C2 122.9(2) . . ? C32 C31 C2 118.4(2) . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.6(3) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? O1 Al1 C5 110.37(9) . . ? O1 Al1 C4 101.02(9) . . ? C5 Al1 C4 118.40(10) . . ? O1 Al1 C1 91.13(8) . . ? C5 Al1 C1 114.08(10) . . ? C4 Al1 C1 116.83(9) . . ? C41 C4 C43 108.3(2) . . ? C41 C4 C42 107.3(2) . . ? C43 C4 C42 107.6(2) . . ? C41 C4 Al1 110.43(16) . . ? C43 C4 Al1 117.14(17) . . ? C42 C4 Al1 105.60(16) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C52 C5 C51 107.6(2) . . ? C52 C5 C53 107.5(2) . . ? C51 C5 C53 107.3(2) . . ? C52 C5 Al1 108.77(17) . . ? C51 C5 Al1 113.11(17) . . ? C53 C5 Al1 112.30(16) . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C6 O1 Al1 121.68(13) . . ? N1 C6 O1 131.5(2) . . ? N1 C6 P1 116.58(16) . . ? O1 C6 P1 111.93(15) . . ? C6 N1 C71 121.79(19) . . ? C76 C71 C72 118.3(2) . . ? C76 C71 N1 117.1(2) . . ? C72 C71 N1 124.3(2) . . ? C73 C72 C71 120.6(3) . . ? C73 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C74 C73 C72 120.8(3) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C75 119.4(3) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C74 C75 C76 120.2(3) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C71 C76 C75 120.7(3) . . ? C71 C76 H76 119.6 . . ? C75 C76 H76 119.6 . . ? C1 P1 C81 118.10(10) . . ? C1 P1 C91 106.27(10) . . ? C81 P1 C91 112.20(10) . . ? C1 P1 C6 98.71(10) . . ? C81 P1 C6 110.08(10) . . ? C91 P1 C6 110.63(10) . . ? C86 C81 C82 119.51(19) . . ? C86 C81 P1 118.14(16) . . ? C82 C81 P1 122.33(17) . . ? C83 C82 C81 118.5(2) . . ? C83 C82 C821 116.5(2) . . ? C81 C82 C821 124.8(2) . . ? C84 C83 C82 122.3(2) . . ? C84 C83 H83 118.9 . . ? C82 C83 H83 118.9 . . ? C85 C84 C83 118.1(2) . . ? C85 C84 C841 121.1(2) . . ? C83 C84 C841 120.8(2) . . ? C84 C85 C86 122.4(2) . . ? C84 C85 H85 118.8 . . ? C86 C85 H85 118.8 . . ? C85 C86 C81 118.6(2) . . ? C85 C86 C861 116.9(2) . . ? C81 C86 C861 124.4(2) . . ? C82 C821 H82A 109.5 . . ? C82 C821 H82B 109.5 . . ? H82A C821 H82B 109.5 . . ? C82 C821 H82C 109.5 . . ? H82A C821 H82C 109.5 . . ? H82B C821 H82C 109.5 . . ? C84 C841 H84A 109.5 . . ? C84 C841 H84B 109.5 . . ? H84A C841 H84B 109.5 . . ? C84 C841 H84C 109.5 . . ? H84A C841 H84C 109.5 . . ? H84B C841 H84C 109.5 . . ? C86 C861 H86A 109.5 . . ? C86 C861 H86B 109.5 . . ? H86A C861 H86B 109.5 . . ? C86 C861 H86C 109.5 . . ? H86A C861 H86C 109.5 . . ? H86B C861 H86C 109.5 . . ? C92 C91 C96 119.4(2) . . ? C92 C91 P1 123.61(17) . . ? C96 C91 P1 116.99(17) . . ? C93 C92 C91 118.4(2) . . ? C93 C92 C921 116.0(2) . . ? C91 C92 C921 125.5(2) . . ? C94 C93 C92 122.9(3) . . ? C94 C93 H93 118.5 . . ? C92 C93 H93 118.5 . . ? C95 C94 C93 117.8(2) . . ? C95 C94 C941 120.9(3) . . ? C93 C94 C941 121.2(3) . . ? C94 C95 C96 122.2(2) . . ? C94 C95 H95 118.9 . . ? C96 C95 H95 118.9 . . ? C95 C96 C91 119.3(2) . . ? C95 C96 C961 116.3(2) . . ? C91 C96 C961 124.4(2) . . ? C92 C921 H92A 109.5 . . ? C92 C921 H92B 109.5 . . ? H92A C921 H92B 109.5 . . ? C92 C921 H92C 109.5 . . ? H92A C921 H92C 109.5 . . ? H92B C921 H92C 109.5 . . ? C94 C941 H94A 109.5 . . ? C94 C941 H94B 109.5 . . ? H94A C941 H94B 109.5 . . ? C94 C941 H94C 109.5 . . ? H94A C941 H94C 109.5 . . ? H94B C941 H94C 109.5 . . ? C96 C961 H96A 109.5 . . ? C96 C961 H96B 109.5 . . ? H96A C961 H96B 109.5 . . ? C96 C961 H96C 109.5 . . ? H96A C961 H96C 109.5 . . ? H96B C961 H96C 109.5 . . ? C01 C01 C06 91.0(6) 2 2 ? C01 C01 C02 108.3(6) 2 . ? C06 C01 C02 17.4(4) 2 . ? C01 C01 C06 58.1(6) 2 . ? C06 C01 C06 113.0(3) 2 . ? C02 C01 C06 120.0 . . ? C01 C01 F01 105.15(19) 2 . ? C06 C01 F01 129.5(2) 2 . ? C02 C01 F01 123.5 . . ? C06 C01 F01 116.2 . . ? C01 C01 C02 48.9(4) 2 2 ? C06 C01 C02 108.9(3) 2 2 ? C02 C01 C02 118.53(19) . 2 ? C06 C01 C02 9.4(4) . 2 ? F01 C01 C02 117.80(17) . 2 ? C01 C01 F01 53.24(19) 2 2 ? C06 C01 F01 107.8(5) 2 2 ? C02 C01 F01 119.7(4) . 2 ? C06 C01 F01 97.8(3) . 2 ? F01 C01 F01 55.2(3) . 2 ? C02 C01 F01 91.4(3) 2 2 ? C06 C02 F02 121.5(6) 2 . ? C06 C02 C05 98.1(8) 2 2 ? F02 C02 C05 133.2(5) . 2 ? C06 C02 C03 93.9(3) 2 . ? F02 C02 C03 128.4 . . ? C05 C02 C03 14.0(4) 2 . ? C06 C02 C01 53.3(8) 2 . ? F02 C02 C01 111.4 . . ? C05 C02 C01 112.2(5) 2 . ? C03 C02 C01 120.0 . . ? C06 C02 F06 76.4(6) 2 2 ? F02 C02 F06 45.8(4) . 2 ? C05 C02 F06 145.7(6) 2 2 ? C03 C02 F06 131.7(3) . 2 ? C01 C02 F06 91.9(3) . 2 ? C06 C02 C01 30.8(7) 2 2 ? F02 C02 C01 121.63(11) . 2 ? C05 C02 C01 105.2(6) 2 2 ? C03 C02 C01 108.04(11) . 2 ? C01 C02 C01 22.8(2) . 2 ? F06 C02 C01 87.5(3) 2 2 ? C05 C03 C02 60.8(6) 2 . ? C05 C03 C04 81.6(16) 2 . ? C02 C03 C04 120.0 . . ? C05 C03 C06 67.3(4) 2 2 ? C02 C03 C06 17.2(3) . 2 ? C04 C03 C06 108.1(3) . 2 ? C05 C03 C04 61.0(13) 2 2 ? C02 C03 C04 111.90(17) . 2 ? C04 C03 C04 23.2(4) . 2 ? C06 C03 C04 106.2(5) 2 2 ? C05 C03 H03A 128.6 2 . ? C02 C03 H03A 120.5 . . ? C04 C03 H03A 119.5 . . ? C06 C03 H03A 130.9 2 . ? C04 C03 H03A 122.2 2 . ? C04 C04 C05 78.2(11) 2 2 ? C04 C04 C05 76.8(11) 2 . ? C05 C04 C05 110.1(3) 2 . ? C04 C04 C03 91.1(12) 2 . ? C05 C04 C03 14.4(3) 2 . ? C05 C04 C03 120.0 . . ? C04 C04 C03 65.7(10) 2 2 ? C05 C04 C03 111.7(3) 2 2 ? C05 C04 C03 12.6(3) . 2 ? C03 C04 C03 123.9(3) . 2 ? C04 C04 H04A 101.8 2 . ? C05 C04 H04A 128.6 2 . ? C05 C04 H04A 120.0 . . ? C03 C04 H04A 120.0 . . ? C03 C04 H04A 114.7 2 . ? C03 C05 C02 105.3(11) 2 2 ? C03 C05 C04 84.0(16) 2 2 ? C02 C05 C04 131.5(6) 2 2 ? C03 C05 C04 106.3(15) 2 . ? C02 C05 C04 131.7(4) 2 . ? C04 C05 C04 25.1(4) 2 . ? C03 C05 C06 99.4(7) 2 . ? C02 C05 C06 18.3(4) 2 . ? C04 C05 C06 114.3(3) 2 . ? C04 C05 C06 120.0 . . ? C03 C05 H05A 64.1 2 . ? C02 C05 H05A 106.8 2 . ? C04 C05 H05A 119.6 2 . ? C04 C05 H05A 119.6 . . ? C06 C05 H05A 120.4 . . ? C02 C06 C01 109.3(14) 2 2 ? C02 C06 F06 85.2(9) 2 . ? C01 C06 F06 103.7(2) 2 . ? C02 C06 C05 63.6(3) 2 . ? C01 C06 C05 117.3(3) 2 . ? F06 C06 C05 134.2 . . ? C02 C06 C01 139.9(13) 2 . ? C01 C06 C01 30.9(3) 2 . ? F06 C06 C01 105.5 . . ? C05 C06 C01 120.0 . . ? C02 C06 C03 68.9(3) 2 2 ? C01 C06 C03 128.7(6) 2 2 ? F06 C06 C03 126.3(4) . 2 ? C05 C06 C03 13.3(4) . 2 ? C01 C06 C03 124.8(4) . 2 ? C02 C06 F02 44.1(6) 2 2 ? C01 C06 F02 106.7(5) 2 2 ? F06 C06 F02 41.8(5) . 2 ? C05 C06 F02 103.88(16) . 2 ? C01 C06 F02 128.8(2) . 2 ? C03 C06 F02 104.0(5) 2 2 ? C01 F01 F01 72.5 . 2 ? C01 F01 C01 21.61(16) . 2 ? F01 F01 C01 52.32(16) 2 2 ? F06 F02 C02 75.5(4) 2 . ? F06 F02 C06 61.4(4) 2 2 ? C02 F02 C06 14.44(17) . 2 ? F02 F06 C06 76.8(4) 2 . ? F02 F06 C02 58.7(5) 2 2 ? C06 F06 C02 18.4(3) . 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 P1 C1 C2 C31 -175.55(18) . . . . ? Al1 C1 C2 C31 14.7(4) . . . . ? C1 C2 C31 C36 15.0(4) . . . . ? C1 C2 C31 C32 -168.4(2) . . . . ? C36 C31 C32 C33 -0.3(4) . . . . ? C2 C31 C32 C33 -177.0(2) . . . . ? C31 C32 C33 C34 0.3(4) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C31 -0.1(4) . . . . ? C32 C31 C36 C35 0.2(4) . . . . ? C2 C31 C36 C35 176.8(2) . . . . ? C2 C1 Al1 O1 153.8(2) . . . . ? P1 C1 Al1 O1 -16.90(10) . . . . ? C2 C1 Al1 C5 -93.2(2) . . . . ? P1 C1 Al1 C5 96.07(12) . . . . ? C2 C1 Al1 C4 50.9(3) . . . . ? P1 C1 Al1 C4 -119.85(11) . . . . ? O1 Al1 C4 C41 -58.84(19) . . . . ? C5 Al1 C4 C41 -179.40(17) . . . . ? C1 Al1 C4 C41 38.1(2) . . . . ? O1 Al1 C4 C43 176.60(17) . . . . ? C5 Al1 C4 C43 56.0(2) . . . . ? C1 Al1 C4 C43 -86.5(2) . . . . ? O1 Al1 C4 C42 56.83(17) . . . . ? C5 Al1 C4 C42 -63.73(19) . . . . ? C1 Al1 C4 C42 153.78(16) . . . . ? O1 Al1 C5 C52 -17.3(2) . . . . ? C4 Al1 C5 C52 98.32(19) . . . . ? C1 Al1 C5 C52 -118.20(18) . . . . ? O1 Al1 C5 C51 -136.82(17) . . . . ? C4 Al1 C5 C51 -21.2(2) . . . . ? C1 Al1 C5 C51 122.28(18) . . . . ? O1 Al1 C5 C53 101.61(18) . . . . ? C4 Al1 C5 C53 -142.76(18) . . . . ? C1 Al1 C5 C53 0.7(2) . . . . ? C5 Al1 O1 C6 -122.24(16) . . . . ? C4 Al1 O1 C6 111.66(16) . . . . ? C1 Al1 O1 C6 -5.97(16) . . . . ? Al1 O1 C6 N1 -151.2(2) . . . . ? Al1 O1 C6 P1 26.7(2) . . . . ? O1 C6 N1 C71 -4.0(4) . . . . ? P1 C6 N1 C71 178.19(16) . . . . ? C6 N1 C71 C76 149.4(3) . . . . ? C6 N1 C71 C72 -36.2(3) . . . . ? C76 C71 C72 C73 1.1(4) . . . . ? N1 C71 C72 C73 -173.3(2) . . . . ? C71 C72 C73 C74 -1.3(4) . . . . ? C72 C73 C74 C75 -0.6(5) . . . . ? C73 C74 C75 C76 2.6(6) . . . . ? C72 C71 C76 C75 0.9(5) . . . . ? N1 C71 C76 C75 175.7(3) . . . . ? C74 C75 C76 C71 -2.8(6) . . . . ? C2 C1 P1 C81 -25.9(2) . . . . ? Al1 C1 P1 C81 146.48(10) . . . . ? C2 C1 P1 C91 101.09(19) . . . . ? Al1 C1 P1 C91 -86.50(11) . . . . ? C2 C1 P1 C6 -144.32(19) . . . . ? Al1 C1 P1 C6 28.09(11) . . . . ? N1 C6 P1 C1 143.20(17) . . . . ? O1 C6 P1 C1 -35.06(16) . . . . ? N1 C6 P1 C81 18.9(2) . . . . ? O1 C6 P1 C81 -159.34(14) . . . . ? N1 C6 P1 C91 -105.66(18) . . . . ? O1 C6 P1 C91 76.08(16) . . . . ? C1 P1 C81 C86 -37.3(2) . . . . ? C91 P1 C81 C86 -161.42(16) . . . . ? C6 P1 C81 C86 74.91(18) . . . . ? C1 P1 C81 C82 140.66(17) . . . . ? C91 P1 C81 C82 16.5(2) . . . . ? C6 P1 C81 C82 -107.13(18) . . . . ? C86 C81 C82 C83 7.8(3) . . . . ? P1 C81 C82 C83 -170.10(16) . . . . ? C86 C81 C82 C821 -168.5(2) . . . . ? P1 C81 C82 C821 13.6(3) . . . . ? C81 C82 C83 C84 -0.7(3) . . . . ? C821 C82 C83 C84 176.0(2) . . . . ? C82 C83 C84 C85 -5.5(3) . . . . ? C82 C83 C84 C841 176.5(2) . . . . ? C83 C84 C85 C86 4.5(4) . . . . ? C841 C84 C85 C86 -177.5(2) . . . . ? C84 C85 C86 C81 2.5(3) . . . . ? C84 C85 C86 C861 -173.1(2) . . . . ? C82 C81 C86 C85 -8.7(3) . . . . ? P1 C81 C86 C85 169.27(17) . . . . ? C82 C81 C86 C861 166.5(2) . . . . ? P1 C81 C86 C861 -15.5(3) . . . . ? C1 P1 C91 C92 117.60(18) . . . . ? C81 P1 C91 C92 -111.93(18) . . . . ? C6 P1 C91 C92 11.4(2) . . . . ? C1 P1 C91 C96 -62.36(18) . . . . ? C81 P1 C91 C96 68.11(18) . . . . ? C6 P1 C91 C96 -168.53(16) . . . . ? C96 C91 C92 C93 2.8(3) . . . . ? P1 C91 C92 C93 -177.14(17) . . . . ? C96 C91 C92 C921 -173.3(2) . . . . ? P1 C91 C92 C921 6.7(3) . . . . ? C91 C92 C93 C94 -2.1(4) . . . . ? C921 C92 C93 C94 174.4(2) . . . . ? C92 C93 C94 C95 0.3(4) . . . . ? C92 C93 C94 C941 -177.4(3) . . . . ? C93 C94 C95 C96 0.8(4) . . . . ? C941 C94 C95 C96 178.5(3) . . . . ? C94 C95 C96 C91 -0.1(4) . . . . ? C94 C95 C96 C961 -177.7(2) . . . . ? C92 C91 C96 C95 -1.8(3) . . . . ? P1 C91 C96 C95 178.19(17) . . . . ? C92 C91 C96 C961 175.7(2) . . . . ? P1 C91 C96 C961 -4.4(3) . . . . ? C01 C01 C02 C06 7.4(4) 2 . . 2 ? C06 C01 C02 C06 70.6(7) . . . 2 ? F01 C01 C02 C06 -115.9(7) . . . 2 ? C02 C01 C02 C06 60.0(6) 2 . . 2 ? F01 C01 C02 C06 -50.1(7) 2 . . 2 ? C01 C01 C02 F02 121.5(4) 2 . . . ? C06 C01 C02 F02 114.1(7) 2 . . . ? C06 C01 C02 F02 -175.4 . . . . ? F01 C01 C02 F02 -1.9 . . . . ? C02 C01 C02 F02 174.0(4) 2 . . . ? F01 C01 C02 F02 64.0(3) 2 . . . ? C01 C01 C02 C05 -76.0(6) 2 . . 2 ? C06 C01 C02 C05 -83.4(9) 2 . . 2 ? C06 C01 C02 C05 -12.9(5) . . . 2 ? F01 C01 C02 C05 160.6(5) . . . 2 ? C02 C01 C02 C05 -23.5(6) 2 . . 2 ? F01 C01 C02 C05 -133.6(5) 2 . . 2 ? C01 C01 C02 C03 -63.2(4) 2 . . . ? C06 C01 C02 C03 -70.6(7) 2 . . . ? C06 C01 C02 C03 0.0 . . . . ? F01 C01 C02 C03 173.5 . . . . ? C02 C01 C02 C03 -10.6(4) 2 . . . ? F01 C01 C02 C03 -120.7(3) 2 . . . ? C01 C01 C02 F06 78.9(5) 2 . . 2 ? C06 C01 C02 F06 71.5(7) 2 . . 2 ? C06 C01 C02 F06 142.0(4) . . . 2 ? F01 C01 C02 F06 -44.4(4) . . . 2 ? C02 C01 C02 F06 131.5(5) 2 . . 2 ? F01 C01 C02 F06 21.4(3) 2 . . 2 ? C06 C01 C02 C01 -7.4(4) 2 . . 2 ? C06 C01 C02 C01 63.2(4) . . . 2 ? F01 C01 C02 C01 -123.3(4) . . . 2 ? C02 C01 C02 C01 52.6(3) 2 . . 2 ? F01 C01 C02 C01 -57.5(4) 2 . . 2 ? C06 C02 C03 C05 -108(3) 2 . . 2 ? F02 C02 C03 C05 116(2) . . . 2 ? C01 C02 C03 C05 -59(2) . . . 2 ? F06 C02 C03 C05 177(2) 2 . . 2 ? C01 C02 C03 C05 -80(2) 2 . . 2 ? C06 C02 C03 C04 -49.2(9) 2 . . . ? F02 C02 C03 C04 174.5 . . . . ? C05 C02 C03 C04 59(2) 2 . . . ? C01 C02 C03 C04 0.0 . . . . ? F06 C02 C03 C04 -124.5(6) 2 . . . ? C01 C02 C03 C04 -21.3(3) 2 . . . ? F02 C02 C03 C06 -136.2(9) . . . 2 ? C05 C02 C03 C06 108(3) 2 . . 2 ? C01 C02 C03 C06 49.2(9) . . . 2 ? F06 C02 C03 C06 -75.3(9) 2 . . 2 ? C01 C02 C03 C06 27.9(7) 2 . . 2 ? C06 C02 C03 C04 -73.5(11) 2 . . 2 ? F02 C02 C03 C04 150.2(5) . . . 2 ? C05 C02 C03 C04 34.6(18) 2 . . 2 ? C01 C02 C03 C04 -24.3(5) . . . 2 ? F06 C02 C03 C04 -148.8(8) 2 . . 2 ? C01 C02 C03 C04 -45.6(5) 2 . . 2 ? C05 C03 C04 C04 -26.3(7) 2 . . 2 ? C02 C03 C04 C04 -75.3(6) . . . 2 ? C06 C03 C04 C04 -89.0(6) 2 . . 2 ? C02 C03 C04 C05 -49.1(11) . . . 2 ? C06 C03 C04 C05 -62.7(10) 2 . . 2 ? C04 C03 C04 C05 26.3(7) 2 . . 2 ? C05 C03 C04 C05 49.1(11) 2 . . . ? C02 C03 C04 C05 0.0 . . . . ? C06 C03 C04 C05 -13.6(3) 2 . . . ? C04 C03 C04 C05 75.3(6) 2 . . . ? C05 C03 C04 C03 34.9(10) 2 . . 2 ? C02 C03 C04 C03 -14.2(5) . . . 2 ? C06 C03 C04 C03 -27.8(5) 2 . . 2 ? C04 C03 C04 C03 61.1(6) 2 . . 2 ? C04 C04 C05 C03 -27.9(10) 2 . . 2 ? C05 C04 C05 C03 -99.9(17) 2 . . 2 ? C03 C04 C05 C03 -111.4(16) . . . 2 ? C04 C04 C05 C02 101.0(11) 2 . . 2 ? C05 C04 C05 C02 29.0(7) 2 . . 2 ? C03 C04 C05 C02 17.5(6) . . . 2 ? C03 C04 C05 C02 129(2) 2 . . 2 ? C05 C04 C05 C04 -71.9(9) 2 . . 2 ? C03 C04 C05 C04 -83.5(7) . . . 2 ? C03 C04 C05 C04 27.9(10) 2 . . 2 ? C04 C04 C05 C06 83.5(7) 2 . . . ? C05 C04 C05 C06 11.5(4) 2 . . . ? C03 C04 C05 C06 0.0 . . . . ? C03 C04 C05 C06 111.4(16) 2 . . . ? C03 C05 C06 C02 -111(3) 2 . . 2 ? C04 C05 C06 C02 161.8(18) 2 . . 2 ? C04 C05 C06 C02 134.3(16) . . . 2 ? C03 C05 C06 C01 150(2) 2 . . 2 ? C02 C05 C06 C01 -99.1(17) 2 . . 2 ? C04 C05 C06 C01 62.7(5) 2 . . 2 ? C04 C05 C06 C01 35.2(3) . . . 2 ? C03 C05 C06 F06 -58(2) 2 . . . ? C02 C05 C06 F06 52.1(16) 2 . . . ? C04 C05 C06 F06 -146.1(4) 2 . . . ? C04 C05 C06 F06 -173.6 . . . . ? C03 C05 C06 C01 115(2) 2 . . . ? C02 C05 C06 C01 -134.3(16) 2 . . . ? C04 C05 C06 C01 27.5(4) 2 . . . ? C04 C05 C06 C01 0.0 . . . . ? C02 C05 C06 C03 111(3) 2 . . 2 ? C04 C05 C06 C03 -88(2) 2 . . 2 ? C04 C05 C06 C03 -115(2) . . . 2 ? C03 C05 C06 F02 -92(2) 2 . . 2 ? C02 C05 C06 F02 18.4(10) 2 . . 2 ? C04 C05 C06 F02 -179.8(8) 2 . . 2 ? C04 C05 C06 F02 152.7(6) . . . 2 ? C01 C01 C06 C02 10.3(5) 2 . . 2 ? C06 C01 C06 C02 -65.7(8) 2 . . 2 ? C02 C01 C06 C02 -83.6(8) . . . 2 ? F01 C01 C06 C02 102.5(8) . . . 2 ? F01 C01 C06 C02 47.5(7) 2 . . 2 ? C06 C01 C06 C01 -76.0(6) 2 . . 2 ? C02 C01 C06 C01 -93.9(5) . . . 2 ? F01 C01 C06 C01 92.1(5) . . . 2 ? C02 C01 C06 C01 -10.3(5) 2 . . 2 ? F01 C01 C06 C01 37.2(3) 2 . . 2 ? C01 C01 C06 F06 -90.9(5) 2 . . . ? C06 C01 C06 F06 -166.9(3) 2 . . . ? C02 C01 C06 F06 175.2 . . . . ? F01 C01 C06 F06 1.3 . . . . ? C02 C01 C06 F06 -101.2(8) 2 . . . ? F01 C01 C06 F06 -53.7(4) 2 . . . ? C01 C01 C06 C05 93.9(5) 2 . . . ? C06 C01 C06 C05 17.9(3) 2 . . . ? C02 C01 C06 C05 0.0 . . . . ? F01 C01 C06 C05 -174.0 . . . . ? C02 C01 C06 C05 83.6(8) 2 . . . ? F01 C01 C06 C05 131.1(4) 2 . . . ? C01 C01 C06 C03 108.6(8) 2 . . 2 ? C06 C01 C06 C03 32.6(5) 2 . . 2 ? C02 C01 C06 C03 14.7(5) . . . 2 ? F01 C01 C06 C03 -159.2(5) . . . 2 ? C02 C01 C06 C03 98.3(11) 2 . . 2 ? F01 C01 C06 C03 145.8(7) 2 . . 2 ? C01 C01 C06 F02 -51.2(5) 2 . . 2 ? C06 C01 C06 F02 -127.2(8) 2 . . 2 ? C02 C01 C06 F02 -145.1(8) . . . 2 ? F01 C01 C06 F02 40.9(8) . . . 2 ? C02 C01 C06 F02 -61.6(7) 2 . . 2 ? F01 C01 C06 F02 -14.0(5) 2 . . 2 ? C01 C01 F01 F01 -19.4(4) 2 . . 2 ? C06 C01 F01 F01 84.9(6) 2 . . 2 ? C02 C01 F01 F01 105.3(5) . . . 2 ? C06 C01 F01 F01 -81.0(5) . . . 2 ? C02 C01 F01 F01 -70.6(4) 2 . . 2 ? C06 C01 F01 C01 104.3(8) 2 . . 2 ? C02 C01 F01 C01 124.7(7) . . . 2 ? C06 C01 F01 C01 -61.5(7) . . . 2 ? C02 C01 F01 C01 -51.2(5) 2 . . 2 ? F01 C01 F01 C01 19.4(4) 2 . . 2 ? C06 C02 F02 F06 -11.5(6) 2 . . 2 ? C05 C02 F02 F06 131.8(7) 2 . . 2 ? C03 C02 F02 F06 114.5(4) . . . 2 ? C01 C02 F02 F06 -70.7(4) . . . 2 ? C01 C02 F02 F06 -47.8(2) 2 . . 2 ? C05 C02 F02 C06 143.3(13) 2 . . 2 ? C03 C02 F02 C06 126.0(9) . . . 2 ? C01 C02 F02 C06 -59.1(9) . . . 2 ? F06 C02 F02 C06 11.5(6) 2 . . 2 ? C01 C02 F02 C06 -36.3(7) 2 . . 2 ? C02 C06 F06 F02 -8.9(5) 2 . . 2 ? C01 C06 F06 F02 99.9(8) 2 . . 2 ? C05 C06 F06 F02 -54.0(6) . . . 2 ? C01 C06 F06 F02 131.8(6) . . . 2 ? C03 C06 F06 F02 -68.1(6) 2 . . 2 ? C01 C06 F06 C02 108.7(13) 2 . . 2 ? C05 C06 F06 C02 -45.1(11) . . . 2 ? C01 C06 F06 C02 140.6(11) . . . 2 ? C03 C06 F06 C02 -59.3(9) 2 . . 2 ? F02 C06 F06 C02 8.9(5) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.954 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.065