# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sad2 _database_code_depnum_ccdc_archive 'CCDC 878404' #TrackingRef '- Compound4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 429 _chemical_formula_moiety ? _chemical_formula_sum 'C44 H69 Al P2' _chemical_formula_weight 686.91 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 10.4075(2) _cell_length_b 12.0576(2) _cell_length_c 18.1948(3) _cell_angle_alpha 95.6010(10) _cell_angle_beta 94.7320(10) _cell_angle_gamma 109.1340(10) _cell_volume 2130.84(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description oktaeder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.312 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7886 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_process_details SADABS _exptl_special_details ; The measurement was carried out with copper radiation. The completeness in such measurements is generally lower than the completeness in measurements with Mo radiation, particularly when the crystal symmetry (redundancy within the measurement) is low (triclinic in our case). Furthermore, the problem is aggravated when the measurement is carried out to angles in 2 theta well above the requied minimum of 135 degrees. We always carry our measurements to the physical maximum of 150. When tested, our data showed a substancial increase in completeness when reduced to the required minimum in 2 theta. Since we are primarily interested in maximum crystallographic information and not maximized statistics, we used the complete measurement for the structure determination. ; _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 12351 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 67.48 _reflns_number_total 6929 _reflns_number_gt 5516 _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^)+(0.1046P)^2^+1.6918P] 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 6929 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.004 _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 0.64388(7) 0.76391(6) 0.31317(4) 0.02376(19) Uani 1 1 d . . . C11 C 0.7065(3) 0.6946(2) 0.38759(15) 0.0275(6) Uani 1 1 d . . . C12 C 0.8031(3) 0.6374(3) 0.37331(17) 0.0337(7) Uani 1 1 d . . . C121 C 0.8838(3) 0.6519(3) 0.3078(2) 0.0472(8) Uani 1 1 d . . . H12A H 0.9629 0.6291 0.3180 0.057 Uiso 1 1 calc R . . H12B H 0.9124 0.7332 0.2991 0.057 Uiso 1 1 calc R . . H12C H 0.8274 0.6027 0.2645 0.057 Uiso 1 1 calc R . . C13 C 0.8282(3) 0.5648(3) 0.42342(19) 0.0413(8) Uani 1 1 d . . . H13 H 0.8926 0.5253 0.4132 0.050 Uiso 1 1 calc R . . C14 C 0.7650(3) 0.5468(3) 0.48704(19) 0.0422(8) Uani 1 1 d . . . C141 C 0.7956(4) 0.4675(3) 0.5401(2) 0.0620(11) Uani 1 1 d . . . H14A H 0.8795 0.5100 0.5716 0.074 Uiso 1 1 calc R . . H14B H 0.8045 0.3990 0.5124 0.074 Uiso 1 1 calc R . . H14C H 0.7221 0.4431 0.5701 0.074 Uiso 1 1 calc R . . C15 C 0.6784(3) 0.6091(3) 0.50279(17) 0.0373(7) Uani 1 1 d . . . H15 H 0.6362 0.6003 0.5478 0.045 Uiso 1 1 calc R . . C16 C 0.6503(3) 0.6845(2) 0.45532(16) 0.0312(6) Uani 1 1 d . . . C161 C 0.5666(3) 0.7571(3) 0.48349(17) 0.0415(7) Uani 1 1 d . . . H16A H 0.6216 0.8395 0.4907 0.050 Uiso 1 1 calc R . . H16B H 0.5369 0.7339 0.5299 0.050 Uiso 1 1 calc R . . H16C H 0.4882 0.7442 0.4478 0.050 Uiso 1 1 calc R . . C31 C 0.6279(3) 0.6797(2) 0.22470(15) 0.0258(6) Uani 1 1 d . . . C32 C 0.7056(3) 0.7386(2) 0.17618(16) 0.0285(6) Uani 1 1 d . . . C33 C 0.7012(3) 0.6845(3) 0.09563(18) 0.0406(7) Uani 1 1 d . . . C331 C 0.6461(4) 0.5494(3) 0.08834(19) 0.0455(8) Uani 1 1 d . . . H33A H 0.6997 0.5228 0.1235 0.055 Uiso 1 1 calc R . . H33B H 0.6517 0.5170 0.0388 0.055 Uiso 1 1 calc R . . H33C H 0.5523 0.5233 0.0981 0.055 Uiso 1 1 calc R . . C332 C 0.6066(5) 0.7235(3) 0.0429(2) 0.0673(12) Uani 1 1 d . . . H33D H 0.5168 0.7014 0.0585 0.081 Uiso 1 1 calc R . . H33E H 0.6012 0.6856 -0.0068 0.081 Uiso 1 1 calc R . . H33F H 0.6426 0.8079 0.0438 0.081 Uiso 1 1 calc R . . C333 C 0.8459(5) 0.7209(4) 0.0716(3) 0.0785(16) Uani 1 1 d . . . H33G H 0.8794 0.8048 0.0701 0.094 Uiso 1 1 calc R . . H33H H 0.8426 0.6800 0.0231 0.094 Uiso 1 1 calc R . . H33I H 0.9059 0.7005 0.1066 0.094 Uiso 1 1 calc R . . C41 C 0.7757(3) 0.9042(2) 0.30204(15) 0.0266(6) Uani 1 1 d . . . C42 C 0.8242(3) 0.9897(2) 0.36011(16) 0.0293(6) Uani 1 1 d . . . H42 H 0.7788 0.9711 0.4034 0.035 Uiso 1 1 calc R . . C43 C 0.9365(3) 1.1102(2) 0.37139(18) 0.0344(7) Uani 1 1 d . . . C431 C 0.8678(5) 1.2017(3) 0.3748(4) 0.097(2) Uani 1 1 d . . . H43A H 0.9335 1.2773 0.3956 0.117 Uiso 1 1 calc R . . H43B H 0.7951 1.1801 0.4055 0.117 Uiso 1 1 calc R . . H43C H 0.8310 1.2065 0.3256 0.117 Uiso 1 1 calc R . . C432 C 1.0188(5) 1.1214(5) 0.4462(3) 0.100(2) Uani 1 1 d . . . H43D H 1.0712 1.0691 0.4430 0.120 Uiso 1 1 calc R . . H43E H 0.9576 1.1005 0.4832 0.120 Uiso 1 1 calc R . . H43F H 1.0795 1.2015 0.4596 0.120 Uiso 1 1 calc R . . C433 C 1.0326(4) 1.1290(4) 0.3134(3) 0.0732(14) Uani 1 1 d . . . H43G H 0.9856 1.1355 0.2672 0.088 Uiso 1 1 calc R . . H43H H 1.0649 1.0632 0.3068 0.088 Uiso 1 1 calc R . . H43I H 1.1090 1.2005 0.3290 0.088 Uiso 1 1 calc R . . C51 C 0.4612(3) 0.7192(2) 0.31203(15) 0.0273(6) Uani 1 1 d . . . C52 C 0.3636(3) 0.7652(2) 0.32440(16) 0.0331(6) Uani 1 1 d . . . H52 H 0.2740 0.7070 0.3109 0.040 Uiso 1 1 calc R . . C53 C 0.3552(3) 0.8844(3) 0.35400(18) 0.0363(7) Uani 1 1 d . . . C533 C 0.4938(3) 0.9807(3) 0.37998(19) 0.0383(7) Uani 1 1 d . . . H53A H 0.5398 0.9576 0.4206 0.046 Uiso 1 1 calc R . . H53B H 0.4800 1.0537 0.3961 0.046 Uiso 1 1 calc R . . H53C H 0.5487 0.9911 0.3396 0.046 Uiso 1 1 calc R . . C532 C 0.2709(3) 0.8665(3) 0.4202(2) 0.0459(8) Uani 1 1 d . . . H53D H 0.1836 0.8058 0.4048 0.055 Uiso 1 1 calc R . . H53E H 0.2573 0.9392 0.4374 0.055 Uiso 1 1 calc R . . H53F H 0.3192 0.8433 0.4598 0.055 Uiso 1 1 calc R . . C531 C 0.2775(4) 0.9243(3) 0.2922(2) 0.0503(9) Uani 1 1 d . . . H53G H 0.3271 0.9329 0.2497 0.060 Uiso 1 1 calc R . . H53H H 0.2687 0.9988 0.3099 0.060 Uiso 1 1 calc R . . H53I H 0.1881 0.8660 0.2783 0.060 Uiso 1 1 calc R . . P2 P 0.84015(7) 0.88370(6) 0.21198(4) 0.0289(2) Uani 1 1 d . . . C21 C 0.8101(3) 0.9884(2) 0.15069(16) 0.0314(6) Uani 1 1 d . . . C22 C 0.9203(3) 1.0477(3) 0.11296(17) 0.0383(7) Uani 1 1 d . . . C221 C 1.0623(3) 1.0391(3) 0.1255(2) 0.0489(8) Uani 1 1 d . . . H22A H 1.1017 1.0432 0.0795 0.059 Uiso 1 1 calc R . . H22B H 1.0561 0.9652 0.1431 0.059 Uiso 1 1 calc R . . H22C H 1.1191 1.1034 0.1618 0.059 Uiso 1 1 calc R . . C23 C 0.9001(4) 1.1200(3) 0.06073(19) 0.0483(9) Uani 1 1 d . . . H23 H 0.9754 1.1600 0.0350 0.058 Uiso 1 1 calc R . . C24 C 0.7762(4) 1.1359(3) 0.0449(2) 0.0497(9) Uani 1 1 d . . . C241 C 0.7568(5) 1.2128(4) -0.0131(3) 0.0772(14) Uani 1 1 d . . . H24A H 0.6689 1.1755 -0.0421 0.093 Uiso 1 1 calc R . . H24B H 0.8275 1.2231 -0.0451 0.093 Uiso 1 1 calc R . . H24C H 0.7616 1.2887 0.0112 0.093 Uiso 1 1 calc R . . C25 C 0.6693(4) 1.0789(3) 0.08343(19) 0.0456(8) Uani 1 1 d . . . H25 H 0.5826 1.0898 0.0734 0.055 Uiso 1 1 calc R . . C26 C 0.6837(3) 1.0065(3) 0.13610(17) 0.0355(7) Uani 1 1 d . . . C261 C 0.5613(3) 0.9495(3) 0.17496(18) 0.0428(8) Uani 1 1 d . . . H26A H 0.4866 0.9742 0.1576 0.051 Uiso 1 1 calc R . . H26B H 0.5843 0.9730 0.2276 0.051 Uiso 1 1 calc R . . H26C H 0.5348 0.8649 0.1644 0.051 Uiso 1 1 calc R . . Al1 Al 0.43928(8) 0.56588(7) 0.23888(4) 0.0271(2) Uani 1 1 d . . . C61 C 0.4495(3) 0.4312(2) 0.29093(17) 0.0343(7) Uani 1 1 d . . . H61A H 0.4973 0.4625 0.3399 0.041 Uiso 1 1 calc R . . H61B H 0.3579 0.3832 0.2967 0.041 Uiso 1 1 calc R . . C62 C 0.5194(4) 0.3511(3) 0.2535(2) 0.0505(9) Uani 1 1 d . . . H62 H 0.6048 0.4013 0.2406 0.061 Uiso 1 1 calc R . . C621 C 0.5516(6) 0.2703(4) 0.3050(3) 0.0817(15) Uani 1 1 d . . . H62A H 0.4679 0.2184 0.3187 0.098 Uiso 1 1 calc R . . H62B H 0.6085 0.3171 0.3489 0.098 Uiso 1 1 calc R . . H62C H 0.5988 0.2242 0.2802 0.098 Uiso 1 1 calc R . . C622 C 0.4367(6) 0.2797(4) 0.1831(3) 0.0791(14) Uani 1 1 d . . . H62D H 0.4876 0.2362 0.1591 0.095 Uiso 1 1 calc R . . H62E H 0.4171 0.3317 0.1505 0.095 Uiso 1 1 calc R . . H62F H 0.3523 0.2254 0.1944 0.095 Uiso 1 1 calc R . . C71 C 0.2886(3) 0.5374(3) 0.15664(17) 0.0379(7) Uani 1 1 d . . . H71A H 0.3062 0.6094 0.1347 0.045 Uiso 1 1 calc R . . H71B H 0.2969 0.4788 0.1194 0.045 Uiso 1 1 calc R . . C72 C 0.1449(4) 0.4996(7) 0.1711(3) 0.107(2) Uani 1 1 d . . . H72 H 0.1427 0.5760 0.1903 0.129 Uiso 1 1 calc R . . C721 C 0.0413(4) 0.4766(5) 0.1020(3) 0.0774(14) Uani 1 1 d . . . H72A H 0.0056 0.3933 0.0847 0.093 Uiso 1 1 calc R . . H72B H 0.0856 0.5184 0.0637 0.093 Uiso 1 1 calc R . . H72C H -0.0323 0.5037 0.1142 0.093 Uiso 1 1 calc R . . C722 C 0.0954(5) 0.4412(6) 0.2286(3) 0.0941(18) Uani 1 1 d . . . H72D H 0.0937 0.3609 0.2197 0.113 Uiso 1 1 calc R . . H72E H 0.0043 0.4416 0.2328 0.113 Uiso 1 1 calc R . . H72F H 0.1535 0.4798 0.2740 0.113 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 0.0231(3) 0.0207(3) 0.0229(4) -0.0022(3) 0.0004(3) 0.0033(2) C11 0.0251(13) 0.0215(12) 0.0280(14) -0.0012(11) -0.0051(11) 0.0006(10) C12 0.0310(15) 0.0306(14) 0.0343(16) -0.0027(13) -0.0059(13) 0.0080(12) C121 0.0394(18) 0.061(2) 0.049(2) 0.0055(17) 0.0042(16) 0.0283(16) C13 0.0357(17) 0.0329(16) 0.053(2) 0.0019(15) -0.0096(15) 0.0130(13) C14 0.0417(18) 0.0290(15) 0.0440(19) 0.0056(14) -0.0135(15) 0.0005(13) C141 0.064(3) 0.049(2) 0.068(3) 0.024(2) -0.009(2) 0.0127(18) C15 0.0366(16) 0.0322(15) 0.0302(15) 0.0047(13) -0.0052(13) -0.0035(12) C16 0.0274(14) 0.0294(14) 0.0268(14) -0.0007(12) -0.0042(12) -0.0007(11) C161 0.0445(18) 0.0526(19) 0.0270(15) 0.0019(15) 0.0044(14) 0.0168(15) C31 0.0244(13) 0.0240(13) 0.0251(14) -0.0043(11) -0.0007(11) 0.0060(10) C32 0.0281(14) 0.0250(13) 0.0283(15) -0.0036(12) 0.0034(12) 0.0057(11) C33 0.0475(18) 0.0323(15) 0.0337(17) -0.0042(14) 0.0132(14) 0.0028(13) C331 0.053(2) 0.0365(17) 0.0374(18) -0.0114(15) 0.0125(16) 0.0050(14) C332 0.114(4) 0.048(2) 0.0260(18) -0.0067(16) -0.011(2) 0.016(2) C333 0.079(3) 0.056(2) 0.074(3) -0.029(2) 0.053(3) -0.012(2) C41 0.0237(13) 0.0228(13) 0.0298(15) 0.0019(11) 0.0018(11) 0.0041(10) C42 0.0270(14) 0.0283(14) 0.0295(15) -0.0011(12) 0.0022(12) 0.0070(11) C43 0.0309(15) 0.0240(13) 0.0395(17) -0.0051(13) 0.0026(13) 0.0004(11) C431 0.061(3) 0.033(2) 0.191(7) 0.002(3) 0.035(3) 0.0066(19) C432 0.081(3) 0.090(3) 0.069(3) 0.012(3) -0.027(3) -0.042(3) C433 0.058(2) 0.048(2) 0.087(3) -0.014(2) 0.025(2) -0.0147(18) C51 0.0283(14) 0.0248(13) 0.0233(13) -0.0016(11) 0.0005(11) 0.0038(10) C52 0.0286(14) 0.0314(15) 0.0329(16) -0.0025(13) -0.0001(12) 0.0044(11) C53 0.0352(16) 0.0357(16) 0.0396(17) -0.0007(14) 0.0067(14) 0.0153(13) C533 0.0413(17) 0.0288(15) 0.0440(18) -0.0043(14) 0.0067(14) 0.0128(13) C532 0.0418(18) 0.0415(17) 0.054(2) -0.0061(16) 0.0116(16) 0.0157(14) C531 0.0410(19) 0.057(2) 0.058(2) 0.0088(18) 0.0034(17) 0.0244(16) P2 0.0266(4) 0.0258(4) 0.0293(4) -0.0001(3) 0.0057(3) 0.0028(3) C21 0.0372(16) 0.0271(14) 0.0239(14) -0.0001(12) 0.0053(12) 0.0036(11) C22 0.0414(17) 0.0303(15) 0.0327(16) -0.0007(13) 0.0065(14) -0.0009(12) C221 0.0374(18) 0.052(2) 0.049(2) 0.0082(17) 0.0167(16) 0.0008(15) C23 0.054(2) 0.0414(18) 0.0347(18) 0.0056(15) 0.0081(16) -0.0036(15) C24 0.063(2) 0.0389(18) 0.0367(18) 0.0077(15) -0.0009(16) 0.0044(16) C241 0.089(3) 0.071(3) 0.058(3) 0.029(2) -0.008(2) 0.007(2) C25 0.053(2) 0.0414(18) 0.0382(18) 0.0003(15) -0.0043(16) 0.0143(15) C26 0.0392(17) 0.0312(15) 0.0313(15) -0.0019(13) 0.0027(13) 0.0075(12) C261 0.0369(17) 0.058(2) 0.0357(17) 0.0078(16) 0.0028(14) 0.0189(15) Al1 0.0262(4) 0.0237(4) 0.0246(4) -0.0021(3) -0.0008(3) 0.0016(3) C61 0.0358(16) 0.0268(14) 0.0320(16) 0.0019(12) -0.0016(13) 0.0013(12) C62 0.054(2) 0.0381(18) 0.058(2) 0.0053(17) 0.0009(18) 0.0156(15) C621 0.100(4) 0.059(3) 0.089(4) 0.006(2) -0.016(3) 0.038(3) C622 0.125(4) 0.054(2) 0.058(3) -0.013(2) -0.004(3) 0.039(3) C71 0.0356(16) 0.0415(17) 0.0290(16) -0.0015(13) -0.0054(13) 0.0069(13) C72 0.036(2) 0.200(7) 0.060(3) 0.051(4) -0.012(2) -0.001(3) C721 0.044(2) 0.110(4) 0.066(3) 0.014(3) -0.019(2) 0.015(2) C722 0.040(2) 0.153(5) 0.083(3) 0.047(4) 0.007(2) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C31 1.782(3) . ? P1 C51 1.795(3) . ? P1 C41 1.837(3) . ? P1 C11 1.841(3) . ? P1 Al1 2.7613(10) . ? C11 C16 1.406(4) . ? C11 C12 1.421(4) . ? C12 C13 1.390(4) . ? C12 C121 1.505(5) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C13 C14 1.378(5) . ? C13 H13 0.9600 . ? C14 C15 1.380(5) . ? C14 C141 1.509(5) . ? C141 H14A 0.9599 . ? C141 H14B 0.9599 . ? C141 H14C 0.9599 . ? C15 C16 1.394(4) . ? C15 H15 0.9600 . ? C16 C161 1.507(4) . ? C161 H16A 0.9599 . ? C161 H16B 0.9599 . ? C161 H16C 0.9599 . ? C31 C32 1.342(4) . ? C31 Al1 2.047(3) . ? C32 C33 1.536(4) . ? C32 P2 1.862(3) . ? C33 C331 1.528(4) . ? C33 C332 1.532(5) . ? C33 C333 1.537(5) . ? C331 H33A 0.9599 . ? C331 H33B 0.9599 . ? C331 H33C 0.9599 . ? C332 H33D 0.9599 . ? C332 H33E 0.9599 . ? C332 H33F 0.9599 . ? C333 H33G 0.9599 . ? C333 H33H 0.9599 . ? C333 H33I 0.9599 . ? C41 C42 1.338(4) . ? C41 P2 1.846(3) . ? C42 C43 1.519(4) . ? C42 H42 0.9600 . ? C43 C433 1.496(5) . ? C43 C431 1.498(5) . ? C43 C432 1.516(5) . ? C431 H43A 0.9599 . ? C431 H43B 0.9599 . ? C431 H43C 0.9599 . ? C432 H43D 0.9599 . ? C432 H43E 0.9599 . ? C432 H43F 0.9599 . ? C433 H43G 0.9599 . ? C433 H43H 0.9599 . ? C433 H43I 0.9599 . ? C51 C52 1.332(4) . ? C51 Al1 2.106(3) . ? C52 C53 1.518(4) . ? C52 H52 0.9600 . ? C53 C533 1.527(4) . ? C53 C531 1.536(5) . ? C53 C532 1.540(4) . ? C533 H53A 0.9599 . ? C533 H53B 0.9599 . ? C533 H53C 0.9599 . ? C532 H53D 0.9599 . ? C532 H53E 0.9599 . ? C532 H53F 0.9599 . ? C531 H53G 0.9599 . ? C531 H53H 0.9599 . ? C531 H53I 0.9599 . ? P2 C21 1.847(3) . ? C21 C22 1.410(4) . ? C21 C26 1.411(4) . ? C22 C23 1.398(5) . ? C22 C221 1.516(5) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C23 C24 1.376(5) . ? C23 H23 0.9600 . ? C24 C25 1.387(5) . ? C24 C241 1.514(5) . ? C241 H24A 0.9599 . ? C241 H24B 0.9599 . ? C241 H24C 0.9599 . ? C25 C26 1.388(5) . ? C25 H25 0.9600 . ? C26 C261 1.505(4) . ? C261 H26A 0.9599 . ? C261 H26B 0.9599 . ? C261 H26C 0.9599 . ? Al1 C61 1.985(3) . ? Al1 C71 1.994(3) . ? C61 C62 1.530(5) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C62 C622 1.497(6) . ? C62 C621 1.510(6) . ? C62 H62 0.9600 . ? C621 H62A 0.9599 . ? C621 H62B 0.9599 . ? C621 H62C 0.9599 . ? C622 H62D 0.9599 . ? C622 H62E 0.9599 . ? C622 H62F 0.9599 . ? C71 C72 1.468(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C72 C722 1.362(7) . ? C72 C721 1.526(5) . ? C72 H72 0.9600 . ? C721 H72A 0.9599 . ? C721 H72B 0.9599 . ? C721 H72C 0.9599 . ? C722 H72D 0.9599 . ? C722 H72E 0.9599 . ? C722 H72F 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 C31 P1 C51 91.87(12) . . ? C31 P1 C41 101.39(13) . . ? C51 P1 C41 133.12(12) . . ? C31 P1 C11 110.70(12) . . ? C51 P1 C11 106.52(13) . . ? C41 P1 C11 110.08(12) . . ? C31 P1 Al1 47.80(9) . . ? C51 P1 Al1 49.70(9) . . ? C41 P1 Al1 144.67(9) . . ? C11 P1 Al1 98.83(8) . . ? C16 C11 C12 118.4(3) . . ? C16 C11 P1 122.0(2) . . ? C12 C11 P1 119.2(2) . . ? C13 C12 C11 118.6(3) . . ? C13 C12 C121 117.0(3) . . ? C11 C12 C121 124.3(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 123.1(3) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C13 C14 C15 117.6(3) . . ? C13 C14 C141 121.4(3) . . ? C15 C14 C141 120.9(3) . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C14 C15 C16 122.0(3) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 119.7(3) . . ? C15 C16 C161 116.3(3) . . ? C11 C16 C161 123.9(3) . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C32 C31 P1 114.5(2) . . ? C32 C31 Al1 145.5(2) . . ? P1 C31 Al1 92.03(12) . . ? C31 C32 C33 122.8(2) . . ? C31 C32 P2 118.0(2) . . ? C33 C32 P2 118.6(2) . . ? C331 C33 C332 107.8(3) . . ? C331 C33 C32 110.6(3) . . ? C332 C33 C32 110.5(3) . . ? C331 C33 C333 107.4(3) . . ? C332 C33 C333 109.9(4) . . ? C32 C33 C333 110.6(3) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C42 C41 P1 119.6(2) . . ? C42 C41 P2 131.4(2) . . ? P1 C41 P2 107.77(13) . . ? C41 C42 C43 133.0(3) . . ? C41 C42 H42 113.5 . . ? C43 C42 H42 113.5 . . ? C433 C43 C431 110.7(4) . . ? C433 C43 C432 108.3(4) . . ? C431 C43 C432 108.7(4) . . ? C433 C43 C42 114.7(3) . . ? C431 C43 C42 107.2(3) . . ? C432 C43 C42 107.0(3) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C52 C51 P1 140.3(2) . . ? C52 C51 Al1 126.3(2) . . ? P1 C51 Al1 89.75(12) . . ? C51 C52 C53 137.4(3) . . ? C51 C52 H52 111.3 . . ? C53 C52 H52 111.3 . . ? C52 C53 C533 114.5(2) . . ? C52 C53 C531 107.7(3) . . ? C533 C53 C531 109.7(3) . . ? C52 C53 C532 107.7(3) . . ? C533 C53 C532 108.5(3) . . ? C531 C53 C532 108.5(3) . . ? C53 C533 H53A 109.5 . . ? C53 C533 H53B 109.5 . . ? H53A C533 H53B 109.5 . . ? C53 C533 H53C 109.5 . . ? H53A C533 H53C 109.5 . . ? H53B C533 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C53 C531 H53G 109.5 . . ? C53 C531 H53H 109.5 . . ? H53G C531 H53H 109.5 . . ? C53 C531 H53I 109.5 . . ? H53G C531 H53I 109.5 . . ? H53H C531 H53I 109.5 . . ? C41 P2 C21 110.54(12) . . ? C41 P2 C32 96.39(12) . . ? C21 P2 C32 105.16(13) . . ? C22 C21 C26 118.9(3) . . ? C22 C21 P2 116.4(2) . . ? C26 C21 P2 124.6(2) . . ? C23 C22 C21 119.1(3) . . ? C23 C22 C221 116.8(3) . . ? C21 C22 C221 124.1(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 . . ? C24 C23 C22 122.4(3) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 118.0(3) . . ? C23 C24 C241 121.1(4) . . ? C25 C24 C241 120.9(4) . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C24 C25 C26 122.2(3) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 119.5(3) . . ? C25 C26 C261 117.7(3) . . ? C21 C26 C261 122.8(3) . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C61 Al1 C71 119.00(13) . . ? C61 Al1 C31 112.97(12) . . ? C71 Al1 C31 116.74(13) . . ? C61 Al1 C51 113.24(12) . . ? C71 Al1 C51 110.83(12) . . ? C31 Al1 C51 76.48(10) . . ? C61 Al1 P1 105.94(9) . . ? C71 Al1 P1 134.84(10) . . ? C31 Al1 P1 40.17(7) . . ? C51 Al1 P1 40.56(8) . . ? C62 C61 Al1 116.4(2) . . ? C62 C61 H61A 108.2 . . ? Al1 C61 H61A 108.2 . . ? C62 C61 H61B 108.2 . . ? Al1 C61 H61B 108.2 . . ? H61A C61 H61B 107.3 . . ? C622 C62 C621 110.0(3) . . ? C622 C62 C61 112.1(3) . . ? C621 C62 C61 112.1(3) . . ? C622 C62 H62 107.4 . . ? C621 C62 H62 107.4 . . ? C61 C62 H62 107.4 . . ? C62 C621 H62A 109.5 . . ? C62 C621 H62B 109.5 . . ? H62A C621 H62B 109.5 . . ? C62 C621 H62C 109.5 . . ? H62A C621 H62C 109.5 . . ? H62B C621 H62C 109.5 . . ? C62 C622 H62D 109.5 . . ? C62 C622 H62E 109.5 . . ? H62D C622 H62E 109.5 . . ? C62 C622 H62F 109.5 . . ? H62D C622 H62F 109.5 . . ? H62E C622 H62F 109.5 . . ? C72 C71 Al1 120.8(3) . . ? C72 C71 H71A 107.1 . . ? Al1 C71 H71A 107.1 . . ? C72 C71 H71B 107.1 . . ? Al1 C71 H71B 107.1 . . ? H71A C71 H71B 106.8 . . ? C722 C72 C71 125.1(4) . . ? C722 C72 C721 115.1(4) . . ? C71 C72 C721 114.5(4) . . ? C722 C72 H72 97.7 . . ? C71 C72 H72 97.7 . . ? C721 C72 H72 97.7 . . ? C72 C721 H72A 109.5 . . ? C72 C721 H72B 109.5 . . ? H72A C721 H72B 109.5 . . ? C72 C721 H72C 109.5 . . ? H72A C721 H72C 109.5 . . ? H72B C721 H72C 109.5 . . ? C72 C722 H72D 109.5 . . ? C72 C722 H72E 109.5 . . ? H72D C722 H72E 109.5 . . ? C72 C722 H72F 109.5 . . ? H72D C722 H72F 109.5 . . ? H72E C722 H72F 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 C31 P1 C11 C16 -136.9(2) . . . . ? C51 P1 C11 C16 -38.4(2) . . . . ? C41 P1 C11 C16 111.8(2) . . . . ? Al1 P1 C11 C16 -88.8(2) . . . . ? C31 P1 C11 C12 35.6(2) . . . . ? C51 P1 C11 C12 134.1(2) . . . . ? C41 P1 C11 C12 -75.7(2) . . . . ? Al1 P1 C11 C12 83.7(2) . . . . ? C16 C11 C12 C13 6.0(4) . . . . ? P1 C11 C12 C13 -166.8(2) . . . . ? C16 C11 C12 C121 -172.6(3) . . . . ? P1 C11 C12 C121 14.7(4) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? C121 C12 C13 C14 177.8(3) . . . . ? C12 C13 C14 C15 -3.4(5) . . . . ? C12 C13 C14 C141 -179.8(3) . . . . ? C13 C14 C15 C16 2.5(4) . . . . ? C141 C14 C15 C16 178.9(3) . . . . ? C14 C15 C16 C11 2.7(4) . . . . ? C14 C15 C16 C161 -173.4(3) . . . . ? C12 C11 C16 C15 -6.9(4) . . . . ? P1 C11 C16 C15 165.6(2) . . . . ? C12 C11 C16 C161 168.9(3) . . . . ? P1 C11 C16 C161 -18.5(4) . . . . ? C51 P1 C31 C32 131.9(2) . . . . ? C41 P1 C31 C32 -2.8(2) . . . . ? C11 P1 C31 C32 -119.6(2) . . . . ? Al1 P1 C31 C32 157.3(3) . . . . ? C51 P1 C31 Al1 -25.40(12) . . . . ? C41 P1 C31 Al1 -160.17(11) . . . . ? C11 P1 C31 Al1 83.05(13) . . . . ? P1 C31 C32 C33 -176.6(2) . . . . ? Al1 C31 C32 C33 -39.5(5) . . . . ? P1 C31 C32 P2 11.8(3) . . . . ? Al1 C31 C32 P2 148.9(3) . . . . ? C31 C32 C33 C331 -22.2(4) . . . . ? P2 C32 C33 C331 149.4(2) . . . . ? C31 C32 C33 C332 97.1(4) . . . . ? P2 C32 C33 C332 -91.4(3) . . . . ? C31 C32 C33 C333 -141.0(3) . . . . ? P2 C32 C33 C333 30.6(4) . . . . ? C31 P1 C41 C42 -175.1(2) . . . . ? C51 P1 C41 C42 81.4(3) . . . . ? C11 P1 C41 C42 -57.8(3) . . . . ? Al1 P1 C41 C42 159.17(17) . . . . ? C31 P1 C41 P2 -6.63(16) . . . . ? C51 P1 C41 P2 -110.19(17) . . . . ? C11 P1 C41 P2 110.60(15) . . . . ? Al1 P1 C41 P2 -32.4(2) . . . . ? P1 C41 C42 C43 175.6(2) . . . . ? P2 C41 C42 C43 10.3(5) . . . . ? C41 C42 C43 C433 -15.3(5) . . . . ? C41 C42 C43 C431 108.2(4) . . . . ? C41 C42 C43 C432 -135.4(4) . . . . ? C31 P1 C51 C52 -132.7(4) . . . . ? C41 P1 C51 C52 -25.2(4) . . . . ? C11 P1 C51 C52 115.0(4) . . . . ? Al1 P1 C51 C52 -157.4(4) . . . . ? C31 P1 C51 Al1 24.62(12) . . . . ? C41 P1 C51 Al1 132.17(14) . . . . ? C11 P1 C51 Al1 -87.62(12) . . . . ? P1 C51 C52 C53 -7.1(6) . . . . ? Al1 C51 C52 C53 -158.5(3) . . . . ? C51 C52 C53 C533 -2.6(5) . . . . ? C51 C52 C53 C531 119.7(4) . . . . ? C51 C52 C53 C532 -123.4(4) . . . . ? C42 C41 P2 C21 -73.6(3) . . . . ? P1 C41 P2 C21 119.82(14) . . . . ? C42 C41 P2 C32 177.6(3) . . . . ? P1 C41 P2 C32 10.98(15) . . . . ? C31 C32 P2 C41 -14.7(2) . . . . ? C33 C32 P2 C41 173.4(2) . . . . ? C31 C32 P2 C21 -128.0(2) . . . . ? C33 C32 P2 C21 60.0(3) . . . . ? C41 P2 C21 C22 134.8(2) . . . . ? C32 P2 C21 C22 -122.2(2) . . . . ? C41 P2 C21 C26 -49.3(3) . . . . ? C32 P2 C21 C26 53.7(3) . . . . ? C26 C21 C22 C23 -1.8(4) . . . . ? P2 C21 C22 C23 174.3(2) . . . . ? C26 C21 C22 C221 177.9(3) . . . . ? P2 C21 C22 C221 -6.0(4) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C221 C22 C23 C24 -179.5(3) . . . . ? C22 C23 C24 C25 1.0(5) . . . . ? C22 C23 C24 C241 -178.8(3) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? C241 C24 C25 C26 179.1(3) . . . . ? C24 C25 C26 C21 -0.8(5) . . . . ? C24 C25 C26 C261 179.7(3) . . . . ? C22 C21 C26 C25 2.1(4) . . . . ? P2 C21 C26 C25 -173.7(2) . . . . ? C22 C21 C26 C261 -178.5(3) . . . . ? P2 C21 C26 C261 5.8(4) . . . . ? C32 C31 Al1 C61 130.6(4) . . . . ? P1 C31 Al1 C61 -87.73(14) . . . . ? C32 C31 Al1 C71 -12.9(4) . . . . ? P1 C31 Al1 C71 128.84(13) . . . . ? C32 C31 Al1 C51 -119.6(4) . . . . ? P1 C31 Al1 C51 22.08(11) . . . . ? C32 C31 Al1 P1 -141.7(4) . . . . ? C52 C51 Al1 C61 -110.2(3) . . . . ? P1 C51 Al1 C61 87.59(14) . . . . ? C52 C51 Al1 C71 26.5(3) . . . . ? P1 C51 Al1 C71 -135.70(13) . . . . ? C52 C51 Al1 C31 140.3(3) . . . . ? P1 C51 Al1 C31 -21.90(11) . . . . ? C52 C51 Al1 P1 162.2(3) . . . . ? C31 P1 Al1 C61 106.90(15) . . . . ? C51 P1 Al1 C61 -107.30(15) . . . . ? C41 P1 Al1 C61 142.00(18) . . . . ? C11 P1 Al1 C61 -3.09(14) . . . . ? C31 P1 Al1 C71 -78.79(18) . . . . ? C51 P1 Al1 C71 67.00(18) . . . . ? C41 P1 Al1 C71 -43.7(2) . . . . ? C11 P1 Al1 C71 171.22(16) . . . . ? C51 P1 Al1 C31 145.79(17) . . . . ? C41 P1 Al1 C31 35.10(19) . . . . ? C11 P1 Al1 C31 -109.99(15) . . . . ? C31 P1 Al1 C51 -145.79(17) . . . . ? C41 P1 Al1 C51 -110.70(19) . . . . ? C11 P1 Al1 C51 104.21(15) . . . . ? C71 Al1 C61 C62 83.0(3) . . . . ? C31 Al1 C61 C62 -59.5(3) . . . . ? C51 Al1 C61 C62 -144.1(2) . . . . ? P1 Al1 C61 C62 -101.6(2) . . . . ? Al1 C61 C62 C622 -69.1(4) . . . . ? Al1 C61 C62 C621 166.5(3) . . . . ? C61 Al1 C71 C72 63.7(5) . . . . ? C31 Al1 C71 C72 -155.2(4) . . . . ? C51 Al1 C71 C72 -70.2(4) . . . . ? P1 Al1 C71 C72 -110.1(4) . . . . ? Al1 C71 C72 C722 -24.8(9) . . . . ? Al1 C71 C72 C721 -177.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 67.49 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.785 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.075 data_sad2a _database_code_depnum_ccdc_archive 'CCDC 878405' #TrackingRef '- Compound7b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H86 Al N P2' _chemical_formula_weight 814.14 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' 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 '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 16.0252(9) _cell_length_b 22.6102(10) _cell_length_c 16.4534(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.003(4) _cell_angle_gamma 90.00 _cell_volume 5358.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 17982 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 28.17 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9674 _exptl_absorpt_correction_T_max 0.9949 _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 38443 _diffrn_reflns_av_R_equivalents 0.1224 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.01 _reflns_number_total 12832 _reflns_number_gt 6660 _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^)+(0.0716P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12832 _refine_ls_number_parameters 569 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.973 _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 0.11713(6) 0.50257(4) 0.29173(5) 0.02762(19) Uani 1 1 d . . . C11 C -0.0059(2) 0.51108(16) 0.2141(2) 0.0316(7) Uani 1 1 d . . . C12 C -0.0697(3) 0.46366(17) 0.1973(2) 0.0342(8) Uani 1 1 d . . . C121 C -0.0484(3) 0.40688(18) 0.2503(3) 0.0442(9) Uani 1 1 d . . . H12A H -0.1046 0.3825 0.2291 0.053 Uiso 1 1 calc R . . H12B H -0.0268 0.4158 0.3147 0.053 Uiso 1 1 calc R . . H12C H 0.0002 0.3853 0.2416 0.053 Uiso 1 1 calc R . . C13 C -0.1602(3) 0.47127(18) 0.1306(2) 0.0391(8) Uani 1 1 d . . . H13 H -0.2030 0.4390 0.1181 0.047 Uiso 1 1 calc R . . C14 C -0.1914(3) 0.52275(19) 0.0815(2) 0.0407(9) Uani 1 1 d . . . C141 C -0.2893(3) 0.5286(2) 0.0076(3) 0.0560(12) Uani 1 1 d . . . H14A H -0.3250 0.4932 0.0068 0.067 Uiso 1 1 calc R . . H14B H -0.2877 0.5327 -0.0510 0.067 Uiso 1 1 calc R . . H14C H -0.3188 0.5635 0.0190 0.067 Uiso 1 1 calc R . . C15 C -0.1302(3) 0.56980(19) 0.1039(2) 0.0404(9) Uani 1 1 d . . . H15 H -0.1516 0.6067 0.0729 0.048 Uiso 1 1 calc R . . C16 C -0.0386(2) 0.56553(16) 0.1698(2) 0.0334(8) Uani 1 1 d . . . C161 C 0.0140(3) 0.62340(16) 0.1918(2) 0.0395(9) Uani 1 1 d . . . H16A H -0.0065 0.6475 0.1369 0.047 Uiso 1 1 calc R . . H16B H 0.0807 0.6155 0.2153 0.047 Uiso 1 1 calc R . . H16C H 0.0021 0.6448 0.2375 0.047 Uiso 1 1 calc R . . P2 P 0.14153(6) 0.46913(4) 0.47139(6) 0.0298(2) Uani 1 1 d . . . C21 C 0.2424(2) 0.47908(15) 0.5830(2) 0.0310(7) Uani 1 1 d . . . C22 C 0.3318(2) 0.49617(16) 0.5968(2) 0.0340(7) Uani 1 1 d . . . C221 C 0.3571(3) 0.50839(18) 0.5198(2) 0.0392(8) Uani 1 1 d . . . H22A H 0.3459 0.5502 0.5027 0.047 Uiso 1 1 calc R . . H22B H 0.3189 0.4837 0.4677 0.047 Uiso 1 1 calc R . . H22C H 0.4228 0.4992 0.5391 0.047 Uiso 1 1 calc R . . C23 C 0.4003(3) 0.50384(18) 0.6842(2) 0.0398(8) Uani 1 1 d . . . H23 H 0.4612 0.5158 0.6931 0.048 Uiso 1 1 calc R . . C24 C 0.3836(3) 0.4947(2) 0.7597(2) 0.0452(9) Uani 1 1 d . . . C241 C 0.4595(3) 0.5047(3) 0.8541(3) 0.0673(14) Uani 1 1 d . . . H24A H 0.4327 0.5217 0.8921 0.081 Uiso 1 1 calc R . . H24B H 0.5058 0.5321 0.8514 0.081 Uiso 1 1 calc R . . H24C H 0.4894 0.4670 0.8798 0.081 Uiso 1 1 calc R . . C25 C 0.2956(3) 0.47705(18) 0.7452(2) 0.0426(9) Uani 1 1 d . . . H25 H 0.2833 0.4699 0.7965 0.051 Uiso 1 1 calc R . . C26 C 0.2242(2) 0.46927(16) 0.6590(2) 0.0342(8) Uani 1 1 d . . . C261 C 0.1297(3) 0.45200(18) 0.6514(2) 0.0394(9) Uani 1 1 d . . . H26A H 0.1329 0.4486 0.7121 0.047 Uiso 1 1 calc R . . H26B H 0.1111 0.4139 0.6202 0.047 Uiso 1 1 calc R . . H26C H 0.0841 0.4823 0.6171 0.047 Uiso 1 1 calc R . . C31 C 0.1576(2) 0.42851(15) 0.3191(2) 0.0296(7) Uani 1 1 d . . . C32 C 0.1764(2) 0.41505(15) 0.4060(2) 0.0307(7) Uani 1 1 d . . . C33 C 0.2118(3) 0.35428(15) 0.4496(2) 0.0364(8) Uani 1 1 d . . . C331 C 0.1920(3) 0.30650(16) 0.3781(2) 0.0420(9) Uani 1 1 d . . . H33A H 0.1253 0.3058 0.3376 0.050 Uiso 1 1 calc R . . H33B H 0.2111 0.2679 0.4076 0.050 Uiso 1 1 calc R . . H33C H 0.2266 0.3151 0.3430 0.050 Uiso 1 1 calc R . . C332 C 0.3174(3) 0.35600(19) 0.5094(3) 0.0520(11) Uani 1 1 d . . . H33D H 0.3391 0.3165 0.5343 0.062 Uiso 1 1 calc R . . H33E H 0.3313 0.3841 0.5591 0.062 Uiso 1 1 calc R . . H33F H 0.3490 0.3685 0.4730 0.062 Uiso 1 1 calc R . . C333 C 0.1621(4) 0.33561(18) 0.5073(3) 0.0550(12) Uani 1 1 d . . . H33G H 0.0948 0.3359 0.4697 0.066 Uiso 1 1 calc R . . H33H H 0.1780 0.3633 0.5576 0.066 Uiso 1 1 calc R . . H33I H 0.1820 0.2957 0.5310 0.066 Uiso 1 1 calc R . . C41 C 0.1385(2) 0.53322(16) 0.4015(2) 0.0293(7) Uani 1 1 d . . . C42 C 0.1398(2) 0.59204(16) 0.4140(2) 0.0315(7) Uani 1 1 d . . . H42 H 0.1367 0.6139 0.3635 0.038 Uiso 1 1 calc R . . C43 C 0.1450(3) 0.63132(16) 0.4908(2) 0.0363(8) Uani 1 1 d . . . C431 C 0.1123(3) 0.60254(18) 0.5552(3) 0.0428(9) Uani 1 1 d . . . H43A H 0.0521 0.5836 0.5204 0.051 Uiso 1 1 calc R . . H43B H 0.1062 0.6327 0.5950 0.051 Uiso 1 1 calc R . . H43C H 0.1577 0.5728 0.5918 0.051 Uiso 1 1 calc R . . C432 C 0.2461(3) 0.6529(2) 0.5429(3) 0.0579(12) Uani 1 1 d . . . H43D H 0.2861 0.6194 0.5741 0.069 Uiso 1 1 calc R . . H43E H 0.2495 0.6827 0.5874 0.069 Uiso 1 1 calc R . . H43F H 0.2670 0.6702 0.5004 0.069 Uiso 1 1 calc R . . C433 C 0.0826(4) 0.68455(19) 0.4470(3) 0.0586(13) Uani 1 1 d . . . H43G H 0.1037 0.7044 0.4064 0.070 Uiso 1 1 calc R . . H43H H 0.0857 0.7122 0.4941 0.070 Uiso 1 1 calc R . . H43I H 0.0184 0.6711 0.4124 0.070 Uiso 1 1 calc R . . C51 C 0.1836(2) 0.53580(15) 0.2376(2) 0.0285(7) Uani 1 1 d . . . C52 C 0.2577(2) 0.56882(15) 0.2875(2) 0.0316(7) Uani 1 1 d . . . H52 H 0.2648 0.5759 0.3471 0.038 Uiso 1 1 calc R . . C53 C 0.3324(3) 0.59712(17) 0.2680(2) 0.0374(8) Uani 1 1 d . . . C531 C 0.3517(3) 0.56469(19) 0.1963(3) 0.0462(10) Uani 1 1 d . . . H53A H 0.3636 0.5228 0.2126 0.055 Uiso 1 1 calc R . . H53B H 0.4061 0.5822 0.1931 0.055 Uiso 1 1 calc R . . H53C H 0.2977 0.5684 0.1374 0.055 Uiso 1 1 calc R . . C532 C 0.4219(3) 0.5973(2) 0.3571(3) 0.0547(11) Uani 1 1 d . . . H53D H 0.4108 0.6181 0.4036 0.066 Uiso 1 1 calc R . . H53E H 0.4713 0.6174 0.3479 0.066 Uiso 1 1 calc R . . H53F H 0.4407 0.5565 0.3765 0.066 Uiso 1 1 calc R . . C533 C 0.3041(4) 0.66139(18) 0.2389(3) 0.0547(11) Uani 1 1 d . . . H53G H 0.2461 0.6619 0.1830 0.066 Uiso 1 1 calc R . . H53H H 0.3531 0.6811 0.2286 0.066 Uiso 1 1 calc R . . H53I H 0.2950 0.6822 0.2867 0.066 Uiso 1 1 calc R . . C61 C 0.1462(2) 0.51600(15) 0.1410(2) 0.0300(7) Uani 1 1 d . . . C62 C 0.1175(3) 0.55588(16) 0.0740(2) 0.0368(8) Uani 1 1 d . . . H62A H 0.0852 0.5431 0.0122 0.044 Uiso 1 1 calc R . . H62B H 0.1291 0.5972 0.0877 0.044 Uiso 1 1 calc R . . N1 N 0.1345(2) 0.45585(13) 0.1317(2) 0.0348(7) Uani 1 1 d . . . H1 H 0.098(3) 0.4456(18) 0.075(3) 0.044(11) Uiso 1 1 d . . . Al1 Al 0.18288(8) 0.39317(5) 0.21490(7) 0.0309(2) Uani 1 1 d . . . C71 C 0.3212(3) 0.39079(16) 0.2590(3) 0.0388(8) Uani 1 1 d . . . H71A H 0.3324 0.4015 0.2062 0.047 Uiso 1 1 calc R . . H71B H 0.3461 0.4239 0.3024 0.047 Uiso 1 1 calc R . . C72 C 0.3851(3) 0.33757(17) 0.3037(3) 0.0446(9) Uani 1 1 d . . . H72 H 0.3707 0.3232 0.3536 0.054 Uiso 1 1 calc R . . C721 C 0.3679(4) 0.2877(2) 0.2393(4) 0.0650(13) Uani 1 1 d . . . H72A H 0.3802 0.3006 0.1888 0.078 Uiso 1 1 calc R . . H72B H 0.3031 0.2749 0.2163 0.078 Uiso 1 1 calc R . . H72C H 0.4090 0.2546 0.2705 0.078 Uiso 1 1 calc R . . C722 C 0.4879(3) 0.3544(2) 0.3457(4) 0.0724(15) Uani 1 1 d . . . H72D H 0.5256 0.3198 0.3759 0.087 Uiso 1 1 calc R . . H72E H 0.4994 0.3861 0.3900 0.087 Uiso 1 1 calc R . . H72F H 0.5045 0.3681 0.2982 0.087 Uiso 1 1 calc R . . C81 C 0.1010(3) 0.32443(16) 0.1523(2) 0.0393(9) Uani 1 1 d . . . H81A H 0.1345 0.2880 0.1828 0.047 Uiso 1 1 calc R . . H81B H 0.0453 0.3271 0.1635 0.047 Uiso 1 1 calc R . . C82 C 0.0671(3) 0.31539(17) 0.0501(2) 0.0410(9) Uani 1 1 d . . . H82 H 0.0499 0.3550 0.0202 0.049 Uiso 1 1 calc R . . C821 C 0.1439(3) 0.2897(2) 0.0298(3) 0.0549(12) Uani 1 1 d . . . H82A H 0.1634 0.2514 0.0602 0.066 Uiso 1 1 calc R . . H82B H 0.1969 0.3168 0.0517 0.066 Uiso 1 1 calc R . . H82C H 0.1206 0.2842 -0.0356 0.066 Uiso 1 1 calc R . . C822 C -0.0182(4) 0.2759(2) 0.0094(3) 0.0650(14) Uani 1 1 d . . . H82D H -0.0389 0.2727 -0.0560 0.078 Uiso 1 1 calc R . . H82E H -0.0680 0.2930 0.0212 0.078 Uiso 1 1 calc R . . H82F H -0.0026 0.2365 0.0368 0.078 Uiso 1 1 calc R . . C1 C 0.171(3) 0.8260(14) 0.635(2) 0.139(13) Uiso 0.25 1 d PD A 1 H1A H 0.1351 0.8618 0.6216 0.139 Uiso 0.25 1 calc PR A 1 H1B H 0.1450 0.8000 0.5835 0.139 Uiso 0.25 1 calc PR A 1 H1C H 0.2339 0.8353 0.6472 0.139 Uiso 0.25 1 calc PR A 1 C2 C 0.169(3) 0.796(2) 0.717(3) 0.26(4) Uiso 0.25 1 d PD A 1 H2A H 0.1056 0.7856 0.7009 0.262 Uiso 0.25 1 calc PR A 1 H2B H 0.1861 0.8252 0.7638 0.262 Uiso 0.25 1 calc PR A 1 C3 C 0.2272(16) 0.7404(13) 0.761(2) 0.125(11) Uiso 0.25 1 d PD A 1 H3A H 0.2205 0.7334 0.8159 0.125 Uiso 0.25 1 calc PR A 1 H3B H 0.1973 0.7079 0.7217 0.125 Uiso 0.25 1 calc PR A 1 C4 C 0.3310(16) 0.7350(12) 0.7870(18) 0.091(8) Uiso 0.25 1 d PD A 1 H4A H 0.3602 0.7704 0.8189 0.091 Uiso 0.25 1 calc PR A 1 H4B H 0.3372 0.7351 0.7316 0.091 Uiso 0.25 1 calc PR A 1 C5 C 0.389(3) 0.682(2) 0.844(3) 0.24(3) Uiso 0.25 1 d PD A 1 H5A H 0.3821 0.6503 0.8030 0.239 Uiso 0.25 1 calc PR A 1 H5B H 0.4531 0.6938 0.8699 0.239 Uiso 0.25 1 calc PR A 1 C6 C 0.371(3) 0.6563(13) 0.922(2) 0.124(11) Uiso 0.25 1 d PD A 1 H6A H 0.4139 0.6250 0.9509 0.124 Uiso 0.25 1 calc PR A 1 H6B H 0.3084 0.6410 0.8975 0.124 Uiso 0.25 1 calc PR A 1 H6C H 0.3778 0.6869 0.9648 0.124 Uiso 0.25 1 calc PR A 1 C1A C 0.105(2) 0.819(2) 0.634(3) 0.161(11) Uiso 0.25 1 d PD B 2 H1A1 H 0.0583 0.8100 0.6537 0.161 Uiso 0.25 1 calc PR B 2 H1A2 H 0.0930 0.7980 0.5796 0.161 Uiso 0.25 1 calc PR B 2 H1A3 H 0.1043 0.8610 0.6229 0.161 Uiso 0.25 1 calc PR B 2 C2A C 0.2004(14) 0.8017(13) 0.7078(18) 0.084(8) Uiso 0.25 1 d PD B 2 H2A1 H 0.1922 0.7615 0.7215 0.084 Uiso 0.25 1 calc PR B 2 H2A2 H 0.2064 0.8243 0.7595 0.084 Uiso 0.25 1 calc PR B 2 C3A C 0.2982(14) 0.8025(10) 0.7133(17) 0.081(7) Uiso 0.25 1 d PD B 2 H3A1 H 0.2902 0.8057 0.6521 0.081 Uiso 0.25 1 calc PR B 2 H3A2 H 0.3260 0.8389 0.7427 0.081 Uiso 0.25 1 calc PR B 2 C4A C 0.3709(18) 0.7548(14) 0.757(3) 0.146(14) Uiso 0.25 1 d PD B 2 H4A1 H 0.4256 0.7748 0.7998 0.146 Uiso 0.25 1 calc PR B 2 H4A2 H 0.3857 0.7396 0.7109 0.146 Uiso 0.25 1 calc PR B 2 C5A C 0.359(3) 0.7006(18) 0.808(4) 0.19(2) Uiso 0.25 1 d PD B 2 H5A1 H 0.4122 0.6977 0.8648 0.189 Uiso 0.25 1 calc PR B 2 H5A2 H 0.3575 0.6659 0.7733 0.189 Uiso 0.25 1 calc PR B 2 C6A C 0.272(3) 0.6996(18) 0.825(3) 0.161(11) Uiso 0.25 1 d PD B 2 H6A1 H 0.2743 0.6660 0.8616 0.161 Uiso 0.25 1 calc PR B 2 H6A2 H 0.2171 0.6969 0.7681 0.161 Uiso 0.25 1 calc PR B 2 H6A3 H 0.2692 0.7352 0.8554 0.161 Uiso 0.25 1 calc PR B 2 C1B C 0.426(2) 0.2752(13) 0.7474(15) 0.108(9) Uiso 0.25 1 d PD C 3 H1B1 H 0.3609 0.2716 0.7099 0.108 Uiso 0.25 1 calc PR C 3 H1B2 H 0.4502 0.2382 0.7774 0.108 Uiso 0.25 1 calc PR C 3 H1B3 H 0.4572 0.2853 0.7107 0.108 Uiso 0.25 1 calc PR C 3 C2B C 0.444(3) 0.3235(16) 0.8178(15) 0.20(3) Uiso 0.25 1 d PD C 3 H2B1 H 0.3871 0.3276 0.8238 0.200 Uiso 0.25 1 calc PR C 3 H2B2 H 0.4518 0.3596 0.7914 0.200 Uiso 0.25 1 calc PR C 3 C3B C 0.5225(16) 0.3216(12) 0.9144(14) 0.095(8) Uiso 0.25 1 d PD C 3 H3B1 H 0.5395 0.2807 0.9278 0.095 Uiso 0.25 1 calc PR C 3 H3B2 H 0.5749 0.3410 0.9125 0.095 Uiso 0.25 1 calc PR C 3 C4B C 0.512(3) 0.347(2) 0.9962(15) 0.18(2) Uiso 0.25 1 d PD C 3 H4B1 H 0.5278 0.3882 0.9990 0.184 Uiso 0.25 1 calc PR C 3 H4B2 H 0.4475 0.3451 0.9815 0.184 Uiso 0.25 1 calc PR C 3 C5B C 0.564(3) 0.323(2) 1.0926(15) 0.28(4) Uiso 0.25 1 d PD C 3 H5B1 H 0.5761 0.2822 1.0871 0.282 Uiso 0.25 1 calc PR C 3 H5B2 H 0.5209 0.3245 1.1186 0.282 Uiso 0.25 1 calc PR C 3 C6B C 0.655(2) 0.3495(19) 1.163(2) 0.146(14) Uiso 0.25 1 d PD C 3 H6B1 H 0.6569 0.3461 1.2222 0.146 Uiso 0.25 1 calc PR C 3 H6B2 H 0.6589 0.3904 1.1498 0.146 Uiso 0.25 1 calc PR C 3 H6B3 H 0.7066 0.3283 1.1623 0.146 Uiso 0.25 1 calc PR C 3 C1C C 0.253(2) 0.285(2) 0.779(3) 0.20(2) Uiso 0.25 1 d PD D 4 H1C1 H 0.1955 0.2794 0.7258 0.201 Uiso 0.25 1 calc PR D 4 H1C2 H 0.2551 0.3247 0.8011 0.201 Uiso 0.25 1 calc PR D 4 H1C3 H 0.2582 0.2573 0.8243 0.201 Uiso 0.25 1 calc PR D 4 C2C C 0.335(3) 0.277(3) 0.754(3) 0.23(3) Uiso 0.25 1 d PD D 4 H2C1 H 0.3180 0.2967 0.6973 0.228 Uiso 0.25 1 calc PR D 4 H2C2 H 0.3367 0.2352 0.7418 0.228 Uiso 0.25 1 calc PR D 4 C3C C 0.435(2) 0.295(3) 0.817(3) 0.22(3) Uiso 0.25 1 d PD D 4 H3C1 H 0.4708 0.2597 0.8364 0.223 Uiso 0.25 1 calc PR D 4 H3C2 H 0.4581 0.3164 0.7804 0.223 Uiso 0.25 1 calc PR D 4 C4C C 0.4583(17) 0.3328(15) 0.902(2) 0.128(12) Uiso 0.25 1 d PD D 4 H4C1 H 0.4601 0.3730 0.8837 0.128 Uiso 0.25 1 calc PR D 4 H4C2 H 0.4056 0.3298 0.9144 0.128 Uiso 0.25 1 calc PR D 4 C5C C 0.544(2) 0.325(2) 0.9921(19) 0.21(2) Uiso 0.25 1 d PD D 4 H5C1 H 0.5471 0.2835 1.0061 0.211 Uiso 0.25 1 calc PR D 4 H5C2 H 0.5298 0.3448 1.0364 0.211 Uiso 0.25 1 calc PR D 4 C6C C 0.6419(17) 0.3440(15) 1.010(2) 0.119(10) Uiso 0.25 1 d PD D 4 H6C1 H 0.6820 0.3410 1.0738 0.119 Uiso 0.25 1 calc PR D 4 H6C2 H 0.6408 0.3842 0.9910 0.119 Uiso 0.25 1 calc PR D 4 H6C3 H 0.6645 0.3187 0.9774 0.119 Uiso 0.25 1 calc PR D 4 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 0.0288(4) 0.0288(4) 0.0210(4) 0.0008(3) 0.0070(3) 0.0020(4) C11 0.0322(18) 0.0380(19) 0.0207(14) -0.0032(14) 0.0079(13) 0.0002(15) C12 0.0344(19) 0.041(2) 0.0258(16) -0.0051(15) 0.0120(14) -0.0004(16) C121 0.039(2) 0.045(2) 0.043(2) 0.0029(18) 0.0132(18) -0.0065(18) C13 0.0329(19) 0.051(2) 0.0295(17) -0.0087(17) 0.0102(15) -0.0047(17) C14 0.0315(19) 0.061(3) 0.0238(16) -0.0043(17) 0.0068(15) 0.0055(18) C141 0.037(2) 0.082(3) 0.033(2) -0.002(2) 0.0003(17) 0.004(2) C15 0.037(2) 0.052(2) 0.0267(17) 0.0058(17) 0.0091(16) 0.0121(18) C16 0.0309(18) 0.041(2) 0.0248(16) -0.0017(15) 0.0094(14) 0.0025(16) C161 0.045(2) 0.037(2) 0.0322(18) 0.0065(16) 0.0126(17) 0.0103(17) P2 0.0305(5) 0.0323(4) 0.0227(4) 0.0000(4) 0.0082(4) 0.0016(4) C21 0.0319(18) 0.0344(18) 0.0238(15) 0.0031(13) 0.0096(14) 0.0034(14) C22 0.0328(18) 0.0359(18) 0.0289(16) -0.0006(15) 0.0095(14) 0.0019(16) C221 0.0313(18) 0.052(2) 0.0307(17) 0.0021(17) 0.0100(15) 0.0024(18) C23 0.0323(18) 0.048(2) 0.0337(17) -0.0005(18) 0.0098(15) 0.0051(18) C24 0.040(2) 0.061(3) 0.0266(17) -0.0040(18) 0.0064(15) 0.005(2) C241 0.048(3) 0.107(4) 0.032(2) -0.015(3) 0.0036(19) 0.000(3) C25 0.044(2) 0.056(2) 0.0243(16) 0.0008(16) 0.0123(16) 0.0091(19) C26 0.0354(19) 0.0390(19) 0.0252(16) 0.0013(15) 0.0105(15) 0.0051(16) C261 0.041(2) 0.050(2) 0.0289(17) 0.0001(16) 0.0170(16) -0.0003(18) C31 0.0282(17) 0.0322(17) 0.0231(15) 0.0021(14) 0.0063(14) 0.0009(14) C32 0.0304(18) 0.0325(18) 0.0264(16) -0.0007(14) 0.0097(14) 0.0005(15) C33 0.045(2) 0.0301(18) 0.0281(17) 0.0034(15) 0.0104(16) 0.0058(16) C331 0.053(3) 0.0340(19) 0.0317(18) 0.0033(16) 0.0123(18) 0.0043(18) C332 0.057(3) 0.043(2) 0.038(2) -0.0013(18) 0.0032(19) 0.017(2) C333 0.089(4) 0.035(2) 0.053(3) 0.0081(19) 0.041(3) 0.004(2) C41 0.0249(16) 0.0378(18) 0.0229(15) -0.0025(14) 0.0084(13) 0.0010(15) C42 0.0310(18) 0.0368(19) 0.0243(16) -0.0013(14) 0.0097(14) -0.0015(15) C43 0.046(2) 0.0299(18) 0.0315(18) -0.0059(15) 0.0157(17) -0.0018(16) C431 0.051(2) 0.042(2) 0.037(2) -0.0052(17) 0.0213(19) 0.0027(19) C432 0.058(3) 0.064(3) 0.053(3) -0.025(2) 0.026(2) -0.021(2) C433 0.089(4) 0.041(2) 0.051(3) 0.000(2) 0.035(3) 0.015(2) C51 0.0290(17) 0.0286(16) 0.0246(15) 0.0029(13) 0.0087(14) 0.0032(14) C52 0.0350(19) 0.0303(17) 0.0273(16) 0.0014(14) 0.0116(15) 0.0035(15) C53 0.036(2) 0.039(2) 0.0383(19) 0.0001(16) 0.0168(17) -0.0040(16) C531 0.044(2) 0.051(2) 0.050(2) -0.004(2) 0.027(2) -0.0034(19) C532 0.036(2) 0.076(3) 0.050(2) -0.001(2) 0.016(2) -0.010(2) C533 0.065(3) 0.037(2) 0.066(3) 0.003(2) 0.033(3) -0.007(2) C61 0.0326(18) 0.0326(18) 0.0254(15) 0.0012(13) 0.0132(14) 0.0039(14) C62 0.045(2) 0.0324(18) 0.0303(18) 0.0018(15) 0.0138(16) 0.0044(16) N1 0.0413(18) 0.0326(16) 0.0231(14) -0.0033(12) 0.0074(13) 0.0003(13) Al1 0.0355(6) 0.0295(5) 0.0241(5) -0.0009(4) 0.0098(4) 0.0030(5) C71 0.038(2) 0.0315(18) 0.043(2) 0.0003(16) 0.0138(17) 0.0003(16) C72 0.039(2) 0.039(2) 0.049(2) 0.0044(18) 0.0127(19) 0.0028(17) C721 0.058(3) 0.051(3) 0.071(3) -0.005(2) 0.015(3) 0.016(2) C722 0.042(3) 0.064(3) 0.090(4) 0.010(3) 0.010(3) 0.003(2) C81 0.049(2) 0.0336(19) 0.0333(18) -0.0049(15) 0.0158(17) -0.0056(17) C82 0.053(2) 0.0320(19) 0.0297(18) -0.0046(15) 0.0105(17) -0.0020(17) C821 0.071(3) 0.051(3) 0.036(2) -0.0001(19) 0.017(2) 0.012(2) C822 0.074(4) 0.057(3) 0.046(3) -0.010(2) 0.010(2) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C31 1.781(3) . ? P1 C41 1.822(3) . ? P1 C51 1.824(3) . ? P1 C11 1.830(4) . ? C11 C16 1.409(5) . ? C11 C12 1.423(5) . ? C12 C13 1.393(5) . ? C12 C121 1.505(5) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C13 C14 1.380(6) . ? C13 H13 0.9600 . ? C14 C15 1.383(6) . ? C14 C141 1.512(5) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C15 C16 1.395(5) . ? C15 H15 0.9600 . ? C16 C161 1.512(5) . ? C161 H16A 0.9800 . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? P2 C41 1.837(4) . ? P2 C21 1.853(3) . ? P2 C32 1.869(3) . ? C21 C22 1.402(5) . ? C21 C26 1.420(5) . ? C22 C23 1.385(5) . ? C22 C221 1.516(5) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C23 C24 1.397(5) . ? C23 H23 0.9600 . ? C24 C25 1.382(6) . ? C24 C241 1.512(5) . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C25 C26 1.388(5) . ? C25 H25 0.9600 . ? C26 C261 1.515(5) . ? C261 H26A 0.9800 . ? C261 H26B 0.9800 . ? C261 H26C 0.9800 . ? C31 C32 1.360(4) . ? C31 Al1 2.085(3) . ? C32 C33 1.539(5) . ? C33 C331 1.525(5) . ? C33 C332 1.540(6) . ? C33 C333 1.541(6) . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C332 H33F 0.9800 . ? C333 H33G 0.9800 . ? C333 H33H 0.9800 . ? C333 H33I 0.9800 . ? C41 C42 1.345(5) . ? C42 C43 1.516(5) . ? C42 H42 0.9500 . ? C43 C431 1.518(5) . ? C43 C433 1.528(6) . ? C43 C432 1.543(6) . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C432 H43F 0.9800 . ? C433 H43G 0.9800 . ? C433 H43H 0.9800 . ? C433 H43I 0.9800 . ? C51 C52 1.336(5) . ? C51 C61 1.500(4) . ? C52 C53 1.512(5) . ? C52 H52 0.9500 . ? C53 C531 1.530(5) . ? C53 C533 1.535(6) . ? C53 C532 1.537(6) . ? C531 H53A 0.9800 . ? C531 H53B 0.9800 . ? C531 H53C 0.9800 . ? C532 H53D 0.9800 . ? C532 H53E 0.9800 . ? C532 H53F 0.9800 . ? C533 H53G 0.9800 . ? C533 H53H 0.9800 . ? C533 H53I 0.9800 . ? C61 C62 1.340(5) . ? C61 N1 1.372(4) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? N1 Al1 1.885(3) . ? N1 H1 0.89(4) . ? Al1 C81 2.003(4) . ? Al1 C71 2.009(4) . ? C71 C72 1.542(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C721 1.488(6) . ? C72 C722 1.528(6) . ? C72 H72 1.0000 . ? C721 H72A 0.9800 . ? C721 H72B 0.9800 . ? C721 H72C 0.9800 . ? C722 H72D 0.9800 . ? C722 H72E 0.9800 . ? C722 H72F 0.9800 . ? C81 C82 1.537(5) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C822 1.520(6) . ? C82 C821 1.525(6) . ? C82 H82 1.0000 . ? C821 H82A 0.9800 . ? C821 H82B 0.9800 . ? C821 H82C 0.9800 . ? C822 H82D 0.9800 . ? C822 H82E 0.9800 . ? C822 H82F 0.9800 . ? C1 C2 1.535(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.538(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C3 C4 1.532(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C4 C5 1.553(9) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C5 C6 1.545(9) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C1A C2A 1.528(9) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C3A 1.528(9) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C3A C4A 1.519(8) . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C4A C5A 1.537(9) . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C5A C6A 1.539(9) . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C1B C2B 1.527(9) . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C2B C3B 1.537(9) . ? C2B H2B1 0.9600 . ? C2B H2B2 0.9600 . ? C3B C4B 1.537(9) . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C4B C5B 1.529(9) . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C5B C6B 1.532(9) . ? C5B H5B1 0.9600 . ? C5B H5B2 0.9600 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C1C C2C 1.543(9) . ? C1C H1C1 0.9600 . ? C1C H1C2 0.9600 . ? C1C H1C3 0.9600 . ? C2C C3C 1.543(9) . ? C2C H2C1 0.9600 . ? C2C H2C2 0.9600 . ? C3C C4C 1.528(9) . ? C3C H3C1 0.9600 . ? C3C H3C2 0.9600 . ? C4C C5C 1.527(9) . ? C4C H4C1 0.9600 . ? C4C H4C2 0.9600 . ? C5C C6C 1.531(9) . ? C5C H5C1 0.9600 . ? C5C H5C2 0.9600 . ? C6C H6C1 0.9600 . ? C6C H6C2 0.9600 . ? C6C H6C3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 P1 C41 102.59(15) . . ? C31 P1 C51 106.54(16) . . ? C41 P1 C51 115.56(16) . . ? C31 P1 C11 115.91(16) . . ? C41 P1 C11 109.18(15) . . ? C51 P1 C11 107.30(15) . . ? C16 C11 C12 119.0(3) . . ? C16 C11 P1 119.7(3) . . ? C12 C11 P1 121.3(3) . . ? C13 C12 C11 118.1(3) . . ? C13 C12 C121 117.1(3) . . ? C11 C12 C121 124.7(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 123.4(4) . . ? C14 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? C13 C14 C15 117.4(3) . . ? C13 C14 C141 121.8(4) . . ? C15 C14 C141 120.8(4) . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C14 C15 C16 122.4(4) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 119.3(3) . . ? C15 C16 C161 114.4(3) . . ? C11 C16 C161 126.2(3) . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C41 P2 C21 107.25(15) . . ? C41 P2 C32 95.06(15) . . ? C21 P2 C32 107.38(16) . . ? C22 C21 C26 119.4(3) . . ? C22 C21 P2 125.4(2) . . ? C26 C21 P2 115.2(3) . . ? C23 C22 C21 119.4(3) . . ? C23 C22 C221 117.6(3) . . ? C21 C22 C221 123.0(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 C23 C24 122.1(4) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C241 121.5(4) . . ? C23 C24 C241 120.6(4) . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C24 C25 C26 122.3(3) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 118.9(3) . . ? C25 C26 C261 117.5(3) . . ? C21 C26 C261 123.5(3) . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C32 C31 P1 111.4(3) . . ? C32 C31 Al1 138.2(3) . . ? P1 C31 Al1 109.47(16) . . ? C31 C32 C33 123.8(3) . . ? C31 C32 P2 118.3(3) . . ? C33 C32 P2 117.2(2) . . ? C331 C33 C32 111.3(3) . . ? C331 C33 C332 108.1(3) . . ? C32 C33 C332 110.6(3) . . ? C331 C33 C333 107.0(3) . . ? C32 C33 C333 110.3(3) . . ? C332 C33 C333 109.5(3) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C42 C41 P1 120.8(3) . . ? C42 C41 P2 133.6(3) . . ? P1 C41 P2 105.21(18) . . ? C41 C42 C43 134.3(3) . . ? C41 C42 H42 112.8 . . ? C43 C42 H42 112.8 . . ? C42 C43 C431 114.8(3) . . ? C42 C43 C433 106.4(3) . . ? C431 C43 C433 108.2(3) . . ? C42 C43 C432 108.0(3) . . ? C431 C43 C432 110.3(3) . . ? C433 C43 C432 108.9(4) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C52 C51 C61 130.8(3) . . ? C52 C51 P1 118.8(2) . . ? C61 C51 P1 110.3(2) . . ? C51 C52 C53 132.7(3) . . ? C51 C52 H52 113.6 . . ? C53 C52 H52 113.6 . . ? C52 C53 C531 114.0(3) . . ? C52 C53 C533 108.2(3) . . ? C531 C53 C533 110.2(3) . . ? C52 C53 C532 107.0(3) . . ? C531 C53 C532 108.5(3) . . ? C533 C53 C532 108.6(4) . . ? C53 C531 H53A 109.5 . . ? C53 C531 H53B 109.5 . . ? H53A C531 H53B 109.5 . . ? C53 C531 H53C 109.5 . . ? H53A C531 H53C 109.5 . . ? H53B C531 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C53 C533 H53G 109.5 . . ? C53 C533 H53H 109.5 . . ? H53G C533 H53H 109.5 . . ? C53 C533 H53I 109.5 . . ? H53G C533 H53I 109.5 . . ? H53H C533 H53I 109.5 . . ? C62 C61 N1 126.5(3) . . ? C62 C61 C51 120.3(3) . . ? N1 C61 C51 112.7(3) . . ? C61 C62 H62A 120.0 . . ? C61 C62 H62B 120.0 . . ? H62A C62 H62B 120.0 . . ? C61 N1 Al1 132.2(2) . . ? C61 N1 H1 112(3) . . ? Al1 N1 H1 116(3) . . ? N1 Al1 C81 104.01(15) . . ? N1 Al1 C71 108.62(16) . . ? C81 Al1 C71 122.36(17) . . ? N1 Al1 C31 98.20(14) . . ? C81 Al1 C31 113.62(16) . . ? C71 Al1 C31 107.16(15) . . ? C72 C71 Al1 126.1(3) . . ? C72 C71 H71A 105.8 . . ? Al1 C71 H71A 105.8 . . ? C72 C71 H71B 105.8 . . ? Al1 C71 H71B 105.8 . . ? H71A C71 H71B 106.2 . . ? C721 C72 C722 109.7(4) . . ? C721 C72 C71 112.0(3) . . ? C722 C72 C71 112.3(3) . . ? C721 C72 H72 107.5 . . ? C722 C72 H72 107.5 . . ? C71 C72 H72 107.5 . . ? C72 C721 H72A 109.5 . . ? C72 C721 H72B 109.5 . . ? H72A C721 H72B 109.5 . . ? C72 C721 H72C 109.5 . . ? H72A C721 H72C 109.5 . . ? H72B C721 H72C 109.5 . . ? C72 C722 H72D 109.5 . . ? C72 C722 H72E 109.5 . . ? H72D C722 H72E 109.5 . . ? C72 C722 H72F 109.5 . . ? H72D C722 H72F 109.5 . . ? H72E C722 H72F 109.5 . . ? C82 C81 Al1 120.2(3) . . ? C82 C81 H81A 107.3 . . ? Al1 C81 H81A 107.3 . . ? C82 C81 H81B 107.3 . . ? Al1 C81 H81B 107.3 . . ? H81A C81 H81B 106.9 . . ? C822 C82 C821 109.6(4) . . ? C822 C82 C81 112.2(3) . . ? C821 C82 C81 111.0(3) . . ? C822 C82 H82 108.0 . . ? C821 C82 H82 108.0 . . ? C81 C82 H82 108.0 . . ? 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 . . ? C82 C822 H82D 109.5 . . ? C82 C822 H82E 109.5 . . ? H82D C822 H82E 109.5 . . ? C82 C822 H82F 109.5 . . ? H82D C822 H82F 109.5 . . ? H82E C822 H82F 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 122.6(11) . . ? C1 C2 H2A 106.7 . . ? C3 C2 H2A 106.7 . . ? C1 C2 H2B 106.7 . . ? C3 C2 H2B 106.7 . . ? H2A C2 H2B 106.6 . . ? C4 C3 C2 123.6(11) . . ? C4 C3 H3A 106.4 . . ? C2 C3 H3A 106.4 . . ? C4 C3 H3B 106.4 . . ? C2 C3 H3B 106.4 . . ? H3A C3 H3B 106.5 . . ? C3 C4 C5 121.2(10) . . ? C3 C4 H4A 107.0 . . ? C5 C4 H4A 107.0 . . ? C3 C4 H4B 107.0 . . ? C5 C4 H4B 107.0 . . ? H4A C4 H4B 106.8 . . ? C6 C5 C4 120.6(10) . . ? C6 C5 H5A 107.2 . . ? C4 C5 H5A 107.2 . . ? C6 C5 H5B 107.2 . . ? C4 C5 H5B 107.2 . . ? H5A C5 H5B 106.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1A C2A C3A 133(2) . . ? C1A C2A H2A1 103.9 . . ? C3A C2A H2A1 103.9 . . ? C1A C2A H2A2 103.9 . . ? C3A C2A H2A2 103.9 . . ? H2A1 C2A H2A2 105.4 . . ? C4A C3A C2A 124.9(16) . . ? C4A C3A H3A1 106.1 . . ? C2A C3A H3A1 106.1 . . ? C4A C3A H3A2 106.1 . . ? C2A C3A H3A2 106.1 . . ? H3A1 C3A H3A2 106.3 . . ? C3A C4A C5A 124.8(18) . . ? C3A C4A H4A1 106.1 . . ? C5A C4A H4A1 106.1 . . ? C3A C4A H4A2 106.1 . . ? C5A C4A H4A2 106.1 . . ? H4A1 C4A H4A2 106.3 . . ? C4A C5A C6A 116.8(19) . . ? C4A C5A H5A1 108.1 . . ? C6A C5A H5A1 108.1 . . ? C4A C5A H5A2 108.1 . . ? C6A C5A H5A2 108.1 . . ? H5A1 C5A H5A2 107.3 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C1B C2B C3B 123.9(11) . . ? C1B C2B H2B1 106.3 . . ? C3B C2B H2B1 106.3 . . ? C1B C2B H2B2 106.3 . . ? C3B C2B H2B2 106.3 . . ? H2B1 C2B H2B2 106.4 . . ? C4B C3B C2B 122.8(11) . . ? C4B C3B H3B1 106.6 . . ? C2B C3B H3B1 106.6 . . ? C4B C3B H3B2 106.6 . . ? C2B C3B H3B2 106.6 . . ? H3B1 C3B H3B2 106.6 . . ? C5B C4B C3B 124.0(11) . . ? C5B C4B H4B1 106.3 . . ? C3B C4B H4B1 106.3 . . ? C5B C4B H4B2 106.3 . . ? C3B C4B H4B2 106.3 . . ? H4B1 C4B H4B2 106.4 . . ? C4B C5B C6B 123.6(12) . . ? C4B C5B H5B1 106.4 . . ? C6B C5B H5B1 106.4 . . ? C4B C5B H5B2 106.4 . . ? C6B C5B H5B2 106.4 . . ? H5B1 C5B H5B2 106.5 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2C C1C H1C1 109.5 . . ? C2C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C2C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C1C C2C C3C 122.6(11) . . ? C1C C2C H2C1 106.7 . . ? C3C C2C H2C1 106.7 . . ? C1C C2C H2C2 106.7 . . ? C3C C2C H2C2 106.7 . . ? H2C1 C2C H2C2 106.6 . . ? C4C C3C C2C 122.3(10) . . ? C4C C3C H3C1 106.8 . . ? C2C C3C H3C1 106.8 . . ? C4C C3C H3C2 106.8 . . ? C2C C3C H3C2 106.8 . . ? H3C1 C3C H3C2 106.6 . . ? C5C C4C C3C 125.6(12) . . ? C5C C4C H4C1 105.9 . . ? C3C C4C H4C1 105.9 . . ? C5C C4C H4C2 105.9 . . ? C3C C4C H4C2 105.9 . . ? H4C1 C4C H4C2 106.3 . . ? C4C C5C C6C 124.2(11) . . ? C4C C5C H5C1 106.3 . . ? C6C C5C H5C1 106.3 . . ? C4C C5C H5C2 106.3 . . ? C6C C5C H5C2 106.3 . . ? H5C1 C5C H5C2 106.4 . . ? C5C C6C H6C1 109.5 . . ? C5C C6C H6C2 109.5 . . ? H6C1 C6C H6C2 109.5 . . ? C5C C6C H6C3 109.5 . . ? H6C1 C6C H6C3 109.5 . . ? H6C2 C6C H6C3 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 C31 P1 C11 C16 -163.0(2) . . . . ? C41 P1 C11 C16 81.8(3) . . . . ? C51 P1 C11 C16 -44.1(3) . . . . ? C31 P1 C11 C12 17.0(3) . . . . ? C41 P1 C11 C12 -98.2(3) . . . . ? C51 P1 C11 C12 135.8(3) . . . . ? C16 C11 C12 C13 6.5(5) . . . . ? P1 C11 C12 C13 -173.5(3) . . . . ? C16 C11 C12 C121 -169.7(3) . . . . ? P1 C11 C12 C121 10.4(5) . . . . ? C11 C12 C13 C14 -1.4(5) . . . . ? C121 C12 C13 C14 175.0(3) . . . . ? C12 C13 C14 C15 -3.5(5) . . . . ? C12 C13 C14 C141 178.0(4) . . . . ? C13 C14 C15 C16 3.4(5) . . . . ? C141 C14 C15 C16 -178.1(4) . . . . ? C14 C15 C16 C11 1.6(5) . . . . ? C14 C15 C16 C161 -173.6(3) . . . . ? C12 C11 C16 C15 -6.6(5) . . . . ? P1 C11 C16 C15 173.4(3) . . . . ? C12 C11 C16 C161 168.0(3) . . . . ? P1 C11 C16 C161 -12.0(5) . . . . ? C41 P2 C21 C22 -45.8(3) . . . . ? C32 P2 C21 C22 55.4(3) . . . . ? C41 P2 C21 C26 132.9(3) . . . . ? C32 P2 C21 C26 -125.9(3) . . . . ? C26 C21 C22 C23 -0.8(5) . . . . ? P2 C21 C22 C23 177.9(3) . . . . ? C26 C21 C22 C221 -179.1(3) . . . . ? P2 C21 C22 C221 -0.5(5) . . . . ? C21 C22 C23 C24 0.5(6) . . . . ? C221 C22 C23 C24 179.0(4) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C22 C23 C24 C241 -178.7(4) . . . . ? C23 C24 C25 C26 -1.0(6) . . . . ? C241 C24 C25 C26 178.0(4) . . . . ? C24 C25 C26 C21 0.7(6) . . . . ? C24 C25 C26 C261 -177.8(4) . . . . ? C22 C21 C26 C25 0.2(5) . . . . ? P2 C21 C26 C25 -178.6(3) . . . . ? C22 C21 C26 C261 178.6(3) . . . . ? P2 C21 C26 C261 -0.1(5) . . . . ? C41 P1 C31 C32 9.9(3) . . . . ? C51 P1 C31 C32 131.7(3) . . . . ? C11 P1 C31 C32 -109.0(3) . . . . ? C41 P1 C31 Al1 -160.68(16) . . . . ? C51 P1 C31 Al1 -38.8(2) . . . . ? C11 P1 C31 Al1 80.4(2) . . . . ? P1 C31 C32 C33 179.5(3) . . . . ? Al1 C31 C32 C33 -13.9(6) . . . . ? P1 C31 C32 P2 8.7(4) . . . . ? Al1 C31 C32 P2 175.3(2) . . . . ? C41 P2 C32 C31 -22.7(3) . . . . ? C21 P2 C32 C31 -132.5(3) . . . . ? C41 P2 C32 C33 165.9(3) . . . . ? C21 P2 C32 C33 56.1(3) . . . . ? C31 C32 C33 C331 -19.4(5) . . . . ? P2 C32 C33 C331 151.5(3) . . . . ? C31 C32 C33 C332 100.7(4) . . . . ? P2 C32 C33 C332 -88.4(3) . . . . ? C31 C32 C33 C333 -138.0(4) . . . . ? P2 C32 C33 C333 32.9(4) . . . . ? C31 P1 C41 C42 162.7(3) . . . . ? C51 P1 C41 C42 47.2(3) . . . . ? C11 P1 C41 C42 -73.8(3) . . . . ? C31 P1 C41 P2 -23.5(2) . . . . ? C51 P1 C41 P2 -138.96(16) . . . . ? C11 P1 C41 P2 100.01(18) . . . . ? C21 P2 C41 C42 -52.1(4) . . . . ? C32 P2 C41 C42 -162.1(4) . . . . ? C21 P2 C41 P1 135.22(17) . . . . ? C32 P2 C41 P1 25.25(19) . . . . ? P1 C41 C42 C43 172.4(3) . . . . ? P2 C41 C42 C43 0.6(7) . . . . ? C41 C42 C43 C431 -23.1(6) . . . . ? C41 C42 C43 C433 -142.8(4) . . . . ? C41 C42 C43 C432 100.4(5) . . . . ? C31 P1 C51 C52 -97.2(3) . . . . ? C41 P1 C51 C52 16.0(3) . . . . ? C11 P1 C51 C52 138.0(3) . . . . ? C31 P1 C51 C61 78.5(2) . . . . ? C41 P1 C51 C61 -168.3(2) . . . . ? C11 P1 C51 C61 -46.3(3) . . . . ? C61 C51 C52 C53 -1.9(7) . . . . ? P1 C51 C52 C53 172.8(3) . . . . ? C51 C52 C53 C531 -27.9(6) . . . . ? C51 C52 C53 C533 95.2(5) . . . . ? C51 C52 C53 C532 -147.9(4) . . . . ? C52 C51 C61 C62 -61.9(5) . . . . ? P1 C51 C61 C62 123.0(3) . . . . ? C52 C51 C61 N1 126.0(4) . . . . ? P1 C51 C61 N1 -49.0(3) . . . . ? C62 C61 N1 Al1 170.6(3) . . . . ? C51 C61 N1 Al1 -17.9(5) . . . . ? C61 N1 Al1 C81 163.8(3) . . . . ? C61 N1 Al1 C71 -64.4(4) . . . . ? C61 N1 Al1 C31 46.8(4) . . . . ? C32 C31 Al1 N1 -173.8(4) . . . . ? P1 C31 Al1 N1 -7.0(2) . . . . ? C32 C31 Al1 C81 77.0(4) . . . . ? P1 C31 Al1 C81 -116.26(19) . . . . ? C32 C31 Al1 C71 -61.3(4) . . . . ? P1 C31 Al1 C71 105.46(19) . . . . ? N1 Al1 C71 C72 -160.4(3) . . . . ? C81 Al1 C71 C72 -39.3(4) . . . . ? C31 Al1 C71 C72 94.5(3) . . . . ? Al1 C71 C72 C721 67.3(5) . . . . ? Al1 C71 C72 C722 -168.7(3) . . . . ? N1 Al1 C81 C82 38.9(4) . . . . ? C71 Al1 C81 C82 -84.3(4) . . . . ? C31 Al1 C81 C82 144.6(3) . . . . ? Al1 C81 C82 C822 -160.0(3) . . . . ? Al1 C81 C82 C821 77.1(4) . . . . ? C1 C2 C3 C4 49(6) . . . . ? C2 C3 C4 C5 171(3) . . . . ? C3 C4 C5 C6 -37(6) . . . . ? C1A C2A C3A C4A -141(4) . . . . ? C2A C3A C4A C5A -3(6) . . . . ? C3A C4A C5A C6A -9(7) . . . . ? C1B C2B C3B C4B -146(4) . . . . ? C2B C3B C4B C5B 150(4) . . . . ? C3B C4B C5B C6B 96(4) . . . . ? C1C C2C C3C C4C -10(10) . . . . ? C2C C3C C4C C5C 141(5) . . . . ? C3C C4C C5C C6C 75(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.636 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.060 data_sad1c _database_code_depnum_ccdc_archive 'CCDC 878406' #TrackingRef '- Compound7a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 456 _chemical_formula_moiety ? _chemical_formula_sum 'C60 H104 Al N P2' _chemical_formula_weight 928.36 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' 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 '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 29.4289(13) _cell_length_b 16.7690(8) _cell_length_c 24.9350(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.663(2) _cell_angle_gamma 90.00 _cell_volume 12130.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9819 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9648 _exptl_absorpt_correction_T_max 0.9763 _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 'micro source' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'kappa geometry' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107198 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 29.57 _reflns_number_total 16956 _reflns_number_gt 12697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1196P)^2^+9.6057P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16956 _refine_ls_number_parameters 693 _refine_ls_number_restraints 442 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.2040 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.067 _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 0.345153(15) 0.53332(3) 0.490633(17) 0.02460(11) Uani 1 1 d . . . C11 C 0.38929(6) 0.61115(11) 0.49714(7) 0.0283(3) Uani 1 1 d . . . C12 C 0.39156(6) 0.66518(11) 0.45388(8) 0.0321(4) Uani 1 1 d . . . C121 C 0.35642(8) 0.67090(13) 0.40288(9) 0.0412(5) Uani 1 1 d . . . H12A H 0.3257 0.6776 0.4125 0.062 Uiso 1 1 calc R . . H12B H 0.3571 0.6220 0.3815 0.062 Uiso 1 1 calc R . . H12C H 0.3635 0.7168 0.3814 0.062 Uiso 1 1 calc R . . C13 C 0.42737(7) 0.72043(12) 0.45949(9) 0.0387(4) Uani 1 1 d . . . H13 H 0.4292 0.7558 0.4302 0.046 Uiso 1 1 calc R . . C14 C 0.46042(7) 0.72614(13) 0.50594(10) 0.0416(5) Uani 1 1 d . . . C141 C 0.49883(8) 0.78623(16) 0.51032(14) 0.0587(7) Uani 1 1 d . . . H14A H 0.4951 0.8187 0.4772 0.088 Uiso 1 1 calc R . . H14B H 0.5285 0.7584 0.5148 0.088 Uiso 1 1 calc R . . H14C H 0.4979 0.8208 0.5418 0.088 Uiso 1 1 calc R . . C15 C 0.45634(7) 0.67611(13) 0.54851(10) 0.0396(5) Uani 1 1 d . . . H15 H 0.4781 0.6806 0.5811 0.047 Uiso 1 1 calc R . . C16 C 0.42150(6) 0.61902(12) 0.54587(8) 0.0323(4) Uani 1 1 d . . . C161 C 0.42049(7) 0.57447(14) 0.59824(8) 0.0400(4) Uani 1 1 d . . . H16A H 0.4521 0.5653 0.6169 0.060 Uiso 1 1 calc R . . H16B H 0.4049 0.5231 0.5902 0.060 Uiso 1 1 calc R . . H16C H 0.4038 0.6060 0.6217 0.060 Uiso 1 1 calc R . . P2 P 0.253150(15) 0.60099(3) 0.468243(18) 0.02544(11) Uani 1 1 d . . . C21 C 0.19796(6) 0.56142(11) 0.48206(7) 0.0280(3) Uani 1 1 d . . . C22 C 0.19071(6) 0.48203(11) 0.49749(8) 0.0321(4) Uani 1 1 d . . . C221 C 0.22750(7) 0.41938(12) 0.50401(9) 0.0361(4) Uani 1 1 d . . . H22A H 0.2442 0.4200 0.5415 0.054 Uiso 1 1 calc R . . H22B H 0.2490 0.4302 0.4789 0.054 Uiso 1 1 calc R . . H22C H 0.2134 0.3669 0.4959 0.054 Uiso 1 1 calc R . . C23 C 0.14741(7) 0.46017(14) 0.50812(10) 0.0438(5) Uani 1 1 d . . . H23 H 0.1426 0.4067 0.5184 0.053 Uiso 1 1 calc R . . C24 C 0.11130(8) 0.51338(16) 0.50418(12) 0.0514(6) Uani 1 1 d . . . C241 C 0.06496(10) 0.4872(2) 0.51647(19) 0.0860(12) Uani 1 1 d . . . H24A H 0.0440 0.5314 0.5117 0.103 Uiso 0.50 1 d P A -2 H24B H 0.0684 0.4685 0.5533 0.103 Uiso 0.50 1 d P B -2 H24C H 0.0530 0.4449 0.4921 0.103 Uiso 0.50 1 d P C -2 H24D H 0.0663 0.4318 0.5264 0.103 Uiso 0.50 1 d P D -1 H24E H 0.0418 0.4947 0.4847 0.103 Uiso 0.50 1 d P E -1 H24F H 0.0573 0.5183 0.5459 0.103 Uiso 0.50 1 d P F -1 C25 C 0.11857(7) 0.59079(14) 0.48867(10) 0.0435(5) Uani 1 1 d . . . H25 H 0.0938 0.6278 0.4856 0.052 Uiso 1 1 calc R . . C26 C 0.16100(6) 0.61636(11) 0.47745(8) 0.0318(4) Uani 1 1 d . . . C261 C 0.16535(7) 0.70284(12) 0.46278(9) 0.0368(4) Uani 1 1 d . . . H26A H 0.1350 0.7283 0.4583 0.055 Uiso 1 1 calc R . . H26B H 0.1776 0.7067 0.4286 0.055 Uiso 1 1 calc R . . H26C H 0.1864 0.7298 0.4918 0.055 Uiso 1 1 calc R . . C31 C 0.31686(6) 0.51152(11) 0.42306(7) 0.0270(3) Uani 1 1 d . . . C32 C 0.27242(6) 0.53687(11) 0.41499(7) 0.0273(3) Uani 1 1 d . . . C33 C 0.23830(6) 0.52721(13) 0.36129(8) 0.0337(4) Uani 1 1 d . . . C331 C 0.20550(8) 0.45713(16) 0.36514(9) 0.0451(5) Uani 1 1 d . . . H33A H 0.1850 0.4503 0.3302 0.068 Uiso 1 1 calc R . . H33B H 0.1871 0.4680 0.3936 0.068 Uiso 1 1 calc R . . H33C H 0.2235 0.4083 0.3741 0.068 Uiso 1 1 calc R . . C332 C 0.26362(7) 0.51141(15) 0.31362(8) 0.0400(5) Uani 1 1 d . . . H33D H 0.2414 0.5101 0.2797 0.060 Uiso 1 1 calc R . . H33E H 0.2796 0.4600 0.3189 0.060 Uiso 1 1 calc R . . H33F H 0.2861 0.5540 0.3117 0.060 Uiso 1 1 calc R . . C333 C 0.21013(9) 0.60396(16) 0.34802(9) 0.0491(6) Uani 1 1 d . . . H33G H 0.2311 0.6494 0.3485 0.074 Uiso 1 1 calc R . . H33H H 0.1901 0.6121 0.3752 0.074 Uiso 1 1 calc R . . H33I H 0.1912 0.5993 0.3119 0.074 Uiso 1 1 calc R . . C41 C 0.29804(6) 0.56725(10) 0.52341(7) 0.0256(3) Uani 1 1 d . . . C42 C 0.30335(6) 0.57095(11) 0.57802(7) 0.0296(4) Uani 1 1 d . . . H42 H 0.3316 0.5483 0.5954 0.036 Uiso 1 1 calc R . . C43 C 0.27441(7) 0.60317(12) 0.61784(8) 0.0348(4) Uani 1 1 d . . . C431 C 0.23865(7) 0.66456(13) 0.59444(8) 0.0387(4) Uani 1 1 d . . . H43A H 0.2528 0.7040 0.5734 0.058 Uiso 1 1 calc R . . H43B H 0.2268 0.6914 0.6241 0.058 Uiso 1 1 calc R . . H43C H 0.2132 0.6380 0.5707 0.058 Uiso 1 1 calc R . . C432 C 0.30798(9) 0.64302(19) 0.66327(10) 0.0588(7) Uani 1 1 d . . . H43D H 0.3304 0.6036 0.6805 0.088 Uiso 1 1 calc R . . H43E H 0.2909 0.6648 0.6905 0.088 Uiso 1 1 calc R . . H43F H 0.3242 0.6863 0.6480 0.088 Uiso 1 1 calc R . . C433 C 0.25132(12) 0.53236(16) 0.64108(12) 0.0630(8) Uani 1 1 d . . . H43G H 0.2292 0.5075 0.6121 0.095 Uiso 1 1 calc R . . H43H H 0.2352 0.5510 0.6700 0.095 Uiso 1 1 calc R . . H43I H 0.2748 0.4932 0.6559 0.095 Uiso 1 1 calc R . . C51 C 0.37251(6) 0.44103(11) 0.51777(7) 0.0282(3) Uani 1 1 d . . . C52 C 0.35063(7) 0.39595(11) 0.54952(7) 0.0306(4) Uani 1 1 d . . . H52 H 0.3237 0.4202 0.5585 0.037 Uiso 1 1 calc R . . C53 C 0.36029(8) 0.31352(12) 0.57411(8) 0.0383(4) Uani 1 1 d . . . C531 C 0.31385(10) 0.27669(15) 0.57861(13) 0.0594(7) Uani 1 1 d . . . H53A H 0.2976 0.3111 0.6009 0.089 Uiso 1 1 calc R . . H53B H 0.3186 0.2240 0.5957 0.089 Uiso 1 1 calc R . . H53C H 0.2955 0.2712 0.5422 0.089 Uiso 1 1 calc R . . C532 C 0.38562(12) 0.25834(15) 0.54138(12) 0.0626(8) Uani 1 1 d . . . H53D H 0.3691 0.2555 0.5039 0.094 Uiso 1 1 calc R . . H53E H 0.3874 0.2050 0.5576 0.094 Uiso 1 1 calc R . . H53F H 0.4168 0.2787 0.5414 0.094 Uiso 1 1 calc R . . C533 C 0.38747(11) 0.32480(17) 0.63195(10) 0.0595(7) Uani 1 1 d . . . H53G H 0.4177 0.3481 0.6299 0.089 Uiso 1 1 calc R . . H53H H 0.3917 0.2730 0.6503 0.089 Uiso 1 1 calc R . . H53I H 0.3704 0.3605 0.6525 0.089 Uiso 1 1 calc R . . C61 C 0.41637(7) 0.42821(12) 0.49643(8) 0.0316(4) Uani 1 1 d . . . C62 C 0.45619(7) 0.41746(14) 0.53099(9) 0.0406(5) Uani 1 1 d . . . H62A H 0.4846 0.4171 0.5177 0.049 Uiso 1 1 calc R . . H62B H 0.4559 0.4103 0.5687 0.049 Uiso 1 1 calc R . . N1 N 0.41147(6) 0.43930(11) 0.44105(7) 0.0348(4) Uani 1 1 d . . . H1 H 0.4396(11) 0.4412(18) 0.4312(12) 0.060(8) Uiso 1 1 d . . . Al1 Al 0.359459(19) 0.43785(4) 0.38591(2) 0.03004(14) Uani 1 1 d . . . C71 C 0.32632(7) 0.33289(13) 0.38352(9) 0.0375(4) Uani 1 1 d . . . H71A H 0.3244 0.3196 0.4218 0.045 Uiso 1 1 calc R . . H71B H 0.2944 0.3435 0.3652 0.045 Uiso 1 1 calc R . . C72 C 0.34113(8) 0.25579(13) 0.35807(8) 0.0380(4) Uani 1 1 d . . . C721 C 0.39107(9) 0.23595(16) 0.38150(11) 0.0521(6) Uani 1 1 d . . . H72A H 0.4111 0.2794 0.3733 0.078 Uiso 1 1 calc R . . H72B H 0.3999 0.1864 0.3652 0.078 Uiso 1 1 calc R . . H72C H 0.3943 0.2294 0.4210 0.078 Uiso 1 1 calc R . . C722 C 0.31043(10) 0.18597(15) 0.36947(11) 0.0540(6) Uani 1 1 d . . . H72D H 0.3125 0.1793 0.4089 0.081 Uiso 1 1 calc R . . H72E H 0.3208 0.1370 0.3538 0.081 Uiso 1 1 calc R . . H72F H 0.2784 0.1970 0.3531 0.081 Uiso 1 1 calc R . . C723 C 0.33625(11) 0.26520(17) 0.29640(9) 0.0553(6) Uani 1 1 d . . . H72G H 0.3044 0.2799 0.2814 0.083 Uiso 1 1 calc R . . H72H H 0.3440 0.2147 0.2803 0.083 Uiso 1 1 calc R . . H72I H 0.3572 0.3071 0.2880 0.083 Uiso 1 1 calc R . . C81 C 0.37637(7) 0.48236(13) 0.31678(8) 0.0339(4) Uani 1 1 d . . . H81A H 0.3599 0.4489 0.2870 0.041 Uiso 1 1 calc R . . H81B H 0.3619 0.5357 0.3121 0.041 Uiso 1 1 calc R . . C82 C 0.42576(7) 0.49309(14) 0.30428(8) 0.0379(4) Uani 1 1 d . . . C821 C 0.42312(8) 0.52037(18) 0.24526(9) 0.0515(6) Uani 1 1 d . . . H82A H 0.4062 0.5709 0.2399 0.077 Uiso 1 1 calc R . . H82B H 0.4071 0.4799 0.2208 0.077 Uiso 1 1 calc R . . H82C H 0.4544 0.5278 0.2374 0.077 Uiso 1 1 calc R . . C822 C 0.45164(9) 0.55698(17) 0.34120(10) 0.0507(6) Uani 1 1 d . . . H82D H 0.4830 0.5622 0.3334 0.076 Uiso 1 1 calc R . . H82E H 0.4529 0.5416 0.3793 0.076 Uiso 1 1 calc R . . H82F H 0.4356 0.6081 0.3345 0.076 Uiso 1 1 calc R . . C823 C 0.45245(8) 0.41495(16) 0.31164(10) 0.0475(5) Uani 1 1 d . . . H82G H 0.4836 0.4233 0.3036 0.071 Uiso 1 1 calc R . . H82H H 0.4365 0.3747 0.2868 0.071 Uiso 1 1 calc R . . H82I H 0.4545 0.3966 0.3493 0.071 Uiso 1 1 calc R . . C1 C 0.3045(7) 0.7083(9) 0.2459(8) 0.153(6) Uani 0.520(10) 1 d PDU G -1 H1A H 0.2729 0.6992 0.2300 0.153 Uiso 0.520(10) 1 calc PR G -1 H1B H 0.3098 0.6897 0.2828 0.153 Uiso 0.520(10) 1 calc PR G -1 H1C H 0.3242 0.6800 0.2254 0.153 Uiso 0.520(10) 1 calc PR G -1 C2 C 0.3144(4) 0.7930(7) 0.2449(5) 0.144(4) Uani 0.520(10) 1 d PDU G -1 H2A H 0.2875 0.8205 0.2522 0.144 Uiso 0.520(10) 1 calc PR G -1 H2B H 0.3177 0.8061 0.2082 0.144 Uiso 0.520(10) 1 calc PR G -1 C3 C 0.3553(6) 0.8288(10) 0.2817(8) 0.170(7) Uani 0.520(10) 1 d PDU G -1 H3A H 0.3514 0.8169 0.3183 0.170 Uiso 0.520(10) 1 calc PR G -1 H3B H 0.3819 0.7996 0.2753 0.170 Uiso 0.520(10) 1 calc PR G -1 C4 C 0.3674(6) 0.9140(9) 0.2807(5) 0.160(5) Uani 0.520(10) 1 d PDU G -1 H4A H 0.3414 0.9469 0.2842 0.160 Uiso 0.520(10) 1 calc PR G -1 H4B H 0.3780 0.9275 0.2475 0.160 Uiso 0.520(10) 1 calc PR G -1 C5 C 0.4070(7) 0.9250(17) 0.3310(10) 0.293(11) Uani 0.520(10) 1 d PDU G -1 H5A H 0.4130 0.8763 0.3512 0.293 Uiso 0.520(10) 1 calc PR G -1 H5B H 0.4349 0.9435 0.3201 0.293 Uiso 0.520(10) 1 calc PR G -1 C6 C 0.3870(9) 0.9854(18) 0.3622(12) 0.326(15) Uani 0.520(10) 1 d PDU G -1 H6A H 0.4090 0.9997 0.3937 0.326 Uiso 0.520(10) 1 calc PR G -1 H6B H 0.3597 0.9645 0.3734 0.326 Uiso 0.520(10) 1 calc PR G -1 H6C H 0.3793 1.0318 0.3400 0.326 Uiso 0.520(10) 1 calc PR G -1 C1A C 0.3065(7) 0.7276(12) 0.2554(8) 0.169(7) Uani 0.480(10) 1 d PDU G -2 H1A1 H 0.3067 0.6820 0.2322 0.169 Uiso 0.480(10) 1 calc PR G -2 H1A2 H 0.2796 0.7592 0.2431 0.169 Uiso 0.480(10) 1 calc PR G -2 H1A3 H 0.3061 0.7101 0.2920 0.169 Uiso 0.480(10) 1 calc PR G -2 C2A C 0.3486(8) 0.7764(10) 0.2540(8) 0.184(5) Uani 0.480(10) 1 d PDU G -2 H2A1 H 0.3510 0.7892 0.2170 0.184 Uiso 0.480(10) 1 calc PR G -2 H2A2 H 0.3756 0.7467 0.2694 0.184 Uiso 0.480(10) 1 calc PR G -2 C3A C 0.3459(4) 0.8538(9) 0.2867(5) 0.120(4) Uani 0.480(10) 1 d PDU G -2 H3A1 H 0.3199 0.8848 0.2700 0.120 Uiso 0.480(10) 1 calc PR G -2 H3A2 H 0.3416 0.8409 0.3230 0.120 Uiso 0.480(10) 1 calc PR G -2 C4A C 0.3888(7) 0.9013(11) 0.2887(10) 0.202(8) Uani 0.480(10) 1 d PDU G -2 H4A1 H 0.3942 0.9145 0.2528 0.202 Uiso 0.480(10) 1 calc PR G -2 H4A2 H 0.4151 0.8735 0.3079 0.202 Uiso 0.480(10) 1 calc PR G -2 C5A C 0.3775(6) 0.9768(12) 0.3202(8) 0.198(7) Uani 0.480(10) 1 d PDU G -2 H5A1 H 0.3475 0.9964 0.3050 0.198 Uiso 0.480(10) 1 calc PR G -2 H5A2 H 0.3775 0.9636 0.3577 0.198 Uiso 0.480(10) 1 calc PR G -2 C6A C 0.4102(6) 1.0346(9) 0.3167(7) 0.184(5) Uani 0.480(10) 1 d PDU G -2 H6A1 H 0.4045 1.0800 0.3381 0.184 Uiso 0.480(10) 1 calc PR G -2 H6A2 H 0.4085 1.0505 0.2794 0.184 Uiso 0.480(10) 1 calc PR G -2 H6A3 H 0.4403 1.0137 0.3301 0.184 Uiso 0.480(10) 1 calc PR G -2 C01 C 0.0728(5) 0.7168(8) 0.3120(7) 0.204(6) Uani 0.767(8) 1 d PDU H -3 H01A H 0.0613 0.7703 0.3128 0.204 Uiso 0.767(8) 1 calc PR H -3 H01B H 0.0737 0.7017 0.2751 0.204 Uiso 0.767(8) 1 calc PR H -3 H01C H 0.1033 0.7141 0.3328 0.204 Uiso 0.767(8) 1 calc PR H -3 C02 C 0.0420(5) 0.6616(8) 0.3356(5) 0.224(5) Uani 0.767(8) 1 d PDU H -3 H02A H 0.0110 0.6637 0.3160 0.224 Uiso 0.767(8) 1 calc PR H -3 H02B H 0.0418 0.6733 0.3733 0.224 Uiso 0.767(8) 1 calc PR H -3 C03 C 0.0650(7) 0.5790(8) 0.3285(9) 0.272(5) Uani 0.767(8) 1 d PDU H -3 H03A H 0.0646 0.5678 0.2906 0.272 Uiso 0.767(8) 1 calc PR H -3 H03B H 0.0964 0.5787 0.3469 0.272 Uiso 0.767(8) 1 calc PR H -3 C04 C 0.0371(5) 0.5186(8) 0.3529(5) 0.234(6) Uani 0.767(8) 1 d PDU H -3 H04A H 0.0071 0.5149 0.3309 0.234 Uiso 0.767(8) 1 calc PR H -3 H04B H 0.0331 0.5363 0.3884 0.234 Uiso 0.767(8) 1 calc PR H -3 C05 C 0.0601(5) 0.4337(8) 0.3577(6) 0.231(6) Uani 0.767(8) 1 d PDU H -3 H05A H 0.0773 0.4274 0.3285 0.231 Uiso 0.767(8) 1 calc PR H -3 H05B H 0.0815 0.4312 0.3912 0.231 Uiso 0.767(8) 1 calc PR H -3 C06 C 0.0277(5) 0.3665(8) 0.3562(7) 0.272(5) Uani 0.767(8) 1 d PDU H -3 H06A H 0.0444 0.3172 0.3578 0.272 Uiso 0.767(8) 1 calc PR H -3 H06B H 0.0058 0.3686 0.3230 0.272 Uiso 0.767(8) 1 calc PR H -3 H06C H 0.0117 0.3700 0.3867 0.272 Uiso 0.767(8) 1 calc PR H -3 C0A C 0.052(2) 0.7287(18) 0.3078(17) 0.240(19) Uani 0.233(8) 1 d PDU H -4 H0A1 H 0.0648 0.7708 0.2888 0.240 Uiso 0.233(8) 1 calc PR H -4 H0A2 H 0.0595 0.7378 0.3463 0.240 Uiso 0.233(8) 1 calc PR H -4 H0A3 H 0.0192 0.7279 0.2970 0.240 Uiso 0.233(8) 1 calc PR H -4 C0B C 0.0712(15) 0.6523(18) 0.2944(14) 0.194(10) Uani 0.233(8) 1 d PDU H -4 H0B1 H 0.1040 0.6575 0.2970 0.194 Uiso 0.233(8) 1 calc PR H -4 H0B2 H 0.0586 0.6384 0.2576 0.194 Uiso 0.233(8) 1 calc PR H -4 C0C C 0.0607(16) 0.5855(18) 0.3325(10) 0.175(8) Uani 0.233(8) 1 d PDU H -4 H0C1 H 0.0789 0.5945 0.3677 0.175 Uiso 0.233(8) 1 calc PR H -4 H0C2 H 0.0289 0.5895 0.3365 0.175 Uiso 0.233(8) 1 calc PR H -4 C0D C 0.0693(13) 0.5037(18) 0.3157(19) 0.238(10) Uani 0.233(8) 1 d PDU H -4 H0D1 H 0.0907 0.4783 0.3439 0.238 Uiso 0.233(8) 1 calc PR H -4 H0D2 H 0.0831 0.5054 0.2835 0.238 Uiso 0.233(8) 1 calc PR H -4 C0E C 0.0239(17) 0.453(3) 0.304(2) 0.281(12) Uani 0.233(8) 1 d PDU H -4 H0E1 H 0.0080 0.4633 0.2679 0.281 Uiso 0.233(8) 1 calc PR H -4 H0E2 H 0.0312 0.3972 0.3071 0.281 Uiso 0.233(8) 1 calc PR H -4 C0F C -0.0051(15) 0.475(3) 0.344(2) 0.281(12) Uani 0.233(8) 1 d PDU H -4 H0F1 H -0.0302 0.4386 0.3424 0.281 Uiso 0.233(8) 1 calc PR H -4 H0F2 H -0.0169 0.5283 0.3365 0.281 Uiso 0.233(8) 1 calc PR H -4 H0F3 H 0.0130 0.4742 0.3800 0.281 Uiso 0.233(8) 1 calc PR H -4 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 0.0221(2) 0.0276(2) 0.0250(2) -0.00040(16) 0.00676(15) 0.00260(16) C11 0.0223(8) 0.0296(8) 0.0342(9) -0.0023(7) 0.0083(6) 0.0021(6) C12 0.0286(9) 0.0313(9) 0.0390(9) -0.0007(7) 0.0132(7) 0.0022(7) C121 0.0431(11) 0.0406(11) 0.0403(11) 0.0102(9) 0.0081(8) -0.0033(9) C13 0.0330(10) 0.0347(10) 0.0526(12) 0.0032(9) 0.0193(9) 0.0004(8) C14 0.0243(9) 0.0364(10) 0.0670(14) -0.0048(10) 0.0157(9) -0.0005(7) C141 0.0327(11) 0.0510(14) 0.094(2) -0.0033(14) 0.0164(12) -0.0108(10) C15 0.0233(9) 0.0408(11) 0.0539(12) -0.0088(9) 0.0043(8) 0.0017(8) C16 0.0234(8) 0.0353(9) 0.0385(9) -0.0046(8) 0.0062(7) 0.0044(7) C161 0.0330(10) 0.0484(12) 0.0364(10) -0.0033(9) -0.0008(8) -0.0007(8) P2 0.0219(2) 0.0267(2) 0.0291(2) -0.00021(16) 0.00803(16) 0.00127(16) C21 0.0222(8) 0.0308(9) 0.0322(8) -0.0015(7) 0.0079(6) -0.0013(6) C22 0.0285(9) 0.0317(9) 0.0361(9) -0.0012(7) 0.0060(7) -0.0024(7) C221 0.0353(10) 0.0279(9) 0.0461(11) 0.0016(8) 0.0096(8) -0.0009(7) C23 0.0337(10) 0.0387(11) 0.0603(14) 0.0070(10) 0.0115(9) -0.0077(8) C24 0.0268(10) 0.0522(13) 0.0769(17) 0.0081(12) 0.0136(10) -0.0064(9) C241 0.0321(13) 0.075(2) 0.155(4) 0.029(2) 0.0296(17) -0.0084(13) C25 0.0233(9) 0.0447(12) 0.0638(14) 0.0015(10) 0.0113(9) 0.0013(8) C26 0.0247(8) 0.0326(9) 0.0391(9) -0.0016(7) 0.0078(7) 0.0013(7) C261 0.0300(9) 0.0321(9) 0.0500(11) 0.0017(8) 0.0112(8) 0.0067(7) C31 0.0261(8) 0.0314(8) 0.0245(8) 0.0011(6) 0.0074(6) 0.0032(6) C32 0.0259(8) 0.0295(8) 0.0273(8) 0.0001(6) 0.0073(6) 0.0014(6) C33 0.0266(9) 0.0446(11) 0.0295(9) -0.0036(8) 0.0038(7) 0.0044(8) C331 0.0334(10) 0.0610(14) 0.0404(11) -0.0119(10) 0.0045(8) -0.0082(10) C332 0.0348(10) 0.0575(13) 0.0275(9) -0.0028(8) 0.0044(7) 0.0054(9) C333 0.0474(12) 0.0629(15) 0.0341(10) -0.0011(10) -0.0013(9) 0.0224(11) C41 0.0240(8) 0.0251(8) 0.0290(8) -0.0016(6) 0.0084(6) 0.0003(6) C42 0.0289(9) 0.0310(9) 0.0301(8) -0.0013(7) 0.0082(7) 0.0024(7) C43 0.0378(10) 0.0398(10) 0.0294(9) -0.0027(7) 0.0132(7) 0.0056(8) C431 0.0361(10) 0.0457(11) 0.0364(10) -0.0065(8) 0.0120(8) 0.0071(8) C432 0.0538(14) 0.0837(19) 0.0364(11) -0.0216(12) 0.0000(10) 0.0213(13) C433 0.088(2) 0.0507(14) 0.0634(16) 0.0106(12) 0.0513(16) 0.0075(14) C51 0.0279(8) 0.0305(8) 0.0262(8) -0.0015(6) 0.0046(6) 0.0059(7) C52 0.0359(9) 0.0291(9) 0.0273(8) -0.0016(7) 0.0062(7) 0.0032(7) C53 0.0517(12) 0.0307(9) 0.0327(9) 0.0028(7) 0.0077(8) 0.0046(8) C531 0.0670(17) 0.0382(12) 0.0723(17) 0.0147(12) 0.0096(13) -0.0069(11) C532 0.099(2) 0.0334(11) 0.0622(16) 0.0064(11) 0.0314(15) 0.0220(13) C533 0.0823(19) 0.0527(14) 0.0381(12) 0.0104(10) -0.0051(12) 0.0036(13) C61 0.0317(9) 0.0331(9) 0.0311(9) -0.0001(7) 0.0083(7) 0.0082(7) C62 0.0328(10) 0.0512(12) 0.0378(10) 0.0034(9) 0.0062(8) 0.0148(9) N1 0.0285(8) 0.0474(10) 0.0302(8) 0.0003(7) 0.0095(6) 0.0069(7) Al1 0.0282(3) 0.0370(3) 0.0266(3) -0.0011(2) 0.0095(2) 0.0048(2) C71 0.0370(10) 0.0388(10) 0.0393(10) 0.0019(8) 0.0141(8) 0.0040(8) C72 0.0427(11) 0.0376(10) 0.0346(9) 0.0002(8) 0.0090(8) 0.0011(8) C721 0.0474(13) 0.0520(14) 0.0584(14) 0.0010(11) 0.0128(11) 0.0151(11) C722 0.0613(15) 0.0432(13) 0.0596(15) 0.0050(11) 0.0161(12) -0.0051(11) C723 0.0770(18) 0.0548(14) 0.0353(11) -0.0049(10) 0.0123(11) -0.0110(13) C81 0.0287(9) 0.0460(11) 0.0289(8) 0.0003(8) 0.0100(7) 0.0032(8) C82 0.0301(9) 0.0552(12) 0.0304(9) 0.0022(8) 0.0108(7) 0.0002(9) C821 0.0399(12) 0.0814(18) 0.0360(11) 0.0102(11) 0.0147(9) -0.0016(11) C822 0.0416(12) 0.0656(16) 0.0460(12) 0.0010(11) 0.0101(10) -0.0124(11) C823 0.0350(11) 0.0647(15) 0.0462(12) 0.0011(11) 0.0164(9) 0.0088(10) C1 0.126(11) 0.184(10) 0.162(14) 0.081(10) 0.067(10) 0.016(9) C2 0.123(8) 0.168(8) 0.149(10) 0.082(8) 0.046(7) 0.062(6) C3 0.135(11) 0.201(12) 0.176(13) 0.113(10) 0.035(8) 0.004(10) C4 0.163(13) 0.204(10) 0.123(8) 0.091(7) 0.053(8) 0.020(9) C5 0.27(2) 0.38(2) 0.220(19) -0.034(17) 0.011(14) -0.077(17) C6 0.29(3) 0.34(3) 0.34(3) -0.09(2) 0.04(3) -0.12(2) C1A 0.152(12) 0.242(17) 0.090(9) 0.007(11) -0.047(9) 0.064(10) C2A 0.204(11) 0.216(11) 0.139(9) -0.022(8) 0.053(9) 0.056(8) C3A 0.096(6) 0.220(12) 0.056(5) 0.022(6) 0.045(4) 0.069(6) C4A 0.159(14) 0.265(14) 0.174(15) -0.030(13) 0.010(13) 0.002(11) C5A 0.109(10) 0.336(17) 0.158(13) -0.085(14) 0.047(10) 0.007(10) C6A 0.204(11) 0.216(11) 0.139(9) -0.022(8) 0.053(9) 0.056(8) C01 0.154(10) 0.241(11) 0.216(14) -0.077(11) 0.024(8) -0.046(9) C02 0.322(16) 0.217(10) 0.118(7) 0.034(8) -0.006(9) -0.016(10) C03 0.253(11) 0.254(9) 0.288(12) 0.052(10) -0.011(10) -0.010(8) C04 0.264(14) 0.237(9) 0.164(10) 0.042(9) -0.071(9) -0.039(9) C05 0.274(15) 0.229(10) 0.188(12) -0.024(10) 0.035(11) -0.023(9) C06 0.253(11) 0.254(9) 0.288(12) 0.052(10) -0.011(10) -0.010(8) C0A 0.35(5) 0.217(18) 0.17(3) -0.146(18) 0.08(3) -0.01(3) C0B 0.26(2) 0.174(16) 0.140(19) -0.022(15) 0.023(19) 0.015(19) C0C 0.22(2) 0.260(16) 0.053(9) -0.055(11) 0.034(12) -0.059(17) C0D 0.27(2) 0.197(15) 0.23(2) 0.027(17) -0.021(19) -0.011(17) C0E 0.32(2) 0.23(2) 0.29(3) 0.01(2) 0.03(2) -0.069(19) C0F 0.32(2) 0.23(2) 0.29(3) 0.01(2) 0.03(2) -0.069(19) _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 C31 1.7873(18) . ? P1 C41 1.8151(17) . ? P1 C51 1.8215(18) . ? P1 C11 1.8292(19) . ? C11 C16 1.416(3) . ? C11 C12 1.419(3) . ? C12 C13 1.392(3) . ? C12 C121 1.501(3) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.374(3) . ? C14 C141 1.504(3) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C161 1.509(3) . ? C161 H16A 0.9800 . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? P2 C41 1.8297(18) . ? P2 C21 1.8397(18) . ? P2 C32 1.8691(18) . ? C21 C22 1.412(3) . ? C21 C26 1.415(2) . ? C22 C23 1.394(3) . ? C22 C221 1.498(3) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C23 C24 1.378(3) . ? C23 H23 0.9500 . ? C24 C25 1.381(3) . ? C24 C241 1.512(3) . ? C241 H24A 0.9593 . ? C241 H24B 0.9590 . ? C241 H24C 0.9618 . ? C241 H24D 0.9608 . ? C241 H24E 0.9611 . ? C241 H24F 0.9583 . ? C25 C26 1.392(3) . ? C25 H25 0.9500 . ? C26 C261 1.506(3) . ? C261 H26A 0.9800 . ? C261 H26B 0.9800 . ? C261 H26C 0.9800 . ? C31 C32 1.358(2) . ? C31 Al1 2.0847(18) . ? C32 C33 1.542(3) . ? C33 C332 1.528(3) . ? C33 C331 1.534(3) . ? C33 C333 1.537(3) . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C332 H33F 0.9800 . ? C333 H33G 0.9800 . ? C333 H33H 0.9800 . ? C333 H33I 0.9800 . ? C41 C42 1.346(2) . ? C42 C43 1.512(2) . ? C42 H42 0.9500 . ? C43 C431 1.517(3) . ? C43 C432 1.526(3) . ? C43 C433 1.530(3) . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C432 H43F 0.9800 . ? C433 H43G 0.9800 . ? C433 H43H 0.9800 . ? C433 H43I 0.9800 . ? C51 C52 1.336(3) . ? C51 C61 1.492(3) . ? C52 C53 1.519(3) . ? C52 H52 0.9500 . ? C53 C532 1.511(3) . ? C53 C531 1.521(4) . ? C53 C533 1.539(3) . ? C531 H53A 0.9800 . ? C531 H53B 0.9800 . ? C531 H53C 0.9800 . ? C532 H53D 0.9800 . ? C532 H53E 0.9800 . ? C532 H53F 0.9800 . ? C533 H53G 0.9800 . ? C533 H53H 0.9800 . ? C533 H53I 0.9800 . ? C61 C62 1.345(3) . ? C61 N1 1.377(2) . ? C62 H62A 0.9500 . ? C62 H62B 0.9500 . ? N1 Al1 1.8783(18) . ? N1 H1 0.90(3) . ? Al1 C71 2.008(2) . ? Al1 C81 2.0160(19) . ? C71 C72 1.535(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C721 1.525(3) . ? C72 C723 1.528(3) . ? C72 C722 1.534(3) . ? C721 H72A 0.9800 . ? C721 H72B 0.9800 . ? C721 H72C 0.9800 . ? C722 H72D 0.9800 . ? C722 H72E 0.9800 . ? C722 H72F 0.9800 . ? C723 H72G 0.9800 . ? C723 H72H 0.9800 . ? C723 H72I 0.9800 . ? C81 C82 1.547(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C823 1.523(3) . ? C82 C822 1.530(3) . ? C82 C821 1.530(3) . ? C821 H82A 0.9800 . ? C821 H82B 0.9800 . ? C821 H82C 0.9800 . ? C822 H82D 0.9800 . ? C822 H82E 0.9800 . ? C822 H82F 0.9800 . ? C823 H82G 0.9800 . ? C823 H82H 0.9800 . ? C823 H82I 0.9800 . ? C1 C2 1.451(14) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.509(13) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C3 C4 1.474(15) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C4 C5 1.572(15) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C5 C6 1.459(17) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C1A C2A 1.492(15) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C3A 1.542(13) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C3A C4A 1.486(16) . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C4A C5A 1.556(15) . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C5A C6A 1.379(15) . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C01 C02 1.484(13) . ? C01 H01A 0.9600 . ? C01 H01B 0.9600 . ? C01 H01C 0.9600 . ? C02 C03 1.566(14) . ? C02 H02A 0.9600 . ? C02 H02B 0.9600 . ? C03 C04 1.497(15) . ? C03 H03A 0.9600 . ? C03 H03B 0.9600 . ? C04 C05 1.573(13) . ? C04 H04A 0.9600 . ? C04 H04B 0.9600 . ? C05 C06 1.473(12) . ? C05 H05A 0.9600 . ? C05 H05B 0.9600 . ? C06 H06A 0.9600 . ? C06 H06B 0.9600 . ? C06 H06C 0.9600 . ? C0A C0B 1.461(17) . ? C0A H0A1 0.9600 . ? C0A H0A2 0.9600 . ? C0A H0A3 0.9600 . ? C0B C0C 1.534(16) . ? C0B H0B1 0.9600 . ? C0B H0B2 0.9600 . ? C0C C0D 1.468(18) . ? C0C H0C1 0.9600 . ? C0C H0C2 0.9600 . ? C0D C0E 1.568(17) . ? C0D H0D1 0.9600 . ? C0D H0D2 0.9600 . ? C0E C0F 1.469(17) . ? C0E H0E1 0.9600 . ? C0E H0E2 0.9600 . ? C0F H0F1 0.9600 . ? C0F H0F2 0.9600 . ? C0F H0F3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 P1 C41 102.62(8) . . ? C31 P1 C51 106.45(8) . . ? C41 P1 C51 114.99(8) . . ? C31 P1 C11 116.17(8) . . ? C41 P1 C11 108.73(8) . . ? C51 P1 C11 108.08(8) . . ? C16 C11 C12 118.85(17) . . ? C16 C11 P1 120.37(14) . . ? C12 C11 P1 120.78(14) . . ? C13 C12 C11 118.69(18) . . ? C13 C12 C121 116.40(18) . . ? C11 C12 C121 124.82(17) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 122.9(2) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C15 C14 C13 117.61(19) . . ? C15 C14 C141 121.0(2) . . ? C13 C14 C141 121.4(2) . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C14 C15 C16 122.8(2) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C11 119.00(19) . . ? C15 C16 C161 114.81(18) . . ? C11 C16 C161 126.07(17) . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C41 P2 C21 107.24(8) . . ? C41 P2 C32 95.13(8) . . ? C21 P2 C32 107.95(8) . . ? C22 C21 C26 119.12(16) . . ? C22 C21 P2 124.73(14) . . ? C26 C21 P2 116.15(14) . . ? C23 C22 C21 119.00(18) . . ? C23 C22 C221 117.54(18) . . ? C21 C22 C221 123.46(17) . . ? 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 . . ? C24 C23 C22 122.3(2) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C25 118.32(19) . . ? C23 C24 C241 120.6(2) . . ? C25 C24 C241 121.1(2) . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.6 . . ? C24 C241 H24C 109.4 . . ? H24A C241 H24C 109.4 . . ? H24B C241 H24C 109.4 . . ? C24 C241 H24D 109.4 . . ? H24A C241 H24D 141.0 . . ? H24B C241 H24D 56.3 . . ? H24C C241 H24D 56.2 . . ? C24 C241 H24E 109.4 . . ? H24A C241 H24E 56.2 . . ? H24B C241 H24E 141.0 . . ? H24C C241 H24E 56.2 . . ? H24D C241 H24E 109.3 . . ? C24 C241 H24F 109.6 . . ? H24A C241 H24F 56.3 . . ? H24B C241 H24F 56.3 . . ? H24C C241 H24F 141.0 . . ? H24D C241 H24F 109.6 . . ? H24E C241 H24F 109.5 . . ? C24 C25 C26 122.1(2) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 119.09(18) . . ? C25 C26 C261 117.45(17) . . ? C21 C26 C261 123.42(16) . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C32 C31 P1 111.13(13) . . ? C32 C31 Al1 139.10(14) . . ? P1 C31 Al1 108.69(9) . . ? C31 C32 C33 124.51(16) . . ? C31 C32 P2 118.32(13) . . ? C33 C32 P2 116.53(12) . . ? C332 C33 C331 108.06(18) . . ? C332 C33 C333 107.08(18) . . ? C331 C33 C333 109.44(18) . . ? C332 C33 C32 111.24(15) . . ? C331 C33 C32 110.55(16) . . ? C333 C33 C32 110.37(16) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C42 C41 P1 120.16(14) . . ? C42 C41 P2 133.87(14) . . ? P1 C41 P2 105.55(9) . . ? C41 C42 C43 134.29(17) . . ? C41 C42 H42 112.9 . . ? C43 C42 H42 112.9 . . ? C42 C43 C431 114.87(16) . . ? C42 C43 C432 106.14(17) . . ? C431 C43 C432 108.01(18) . . ? C42 C43 C433 107.83(17) . . ? C431 C43 C433 110.4(2) . . ? C432 C43 C433 109.4(2) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C52 C51 C61 131.44(17) . . ? C52 C51 P1 118.29(14) . . ? C61 C51 P1 110.18(13) . . ? C51 C52 C53 132.67(18) . . ? C51 C52 H52 113.7 . . ? C53 C52 H52 113.7 . . ? C532 C53 C52 114.53(18) . . ? C532 C53 C531 108.8(2) . . ? C52 C53 C531 106.82(18) . . ? C532 C53 C533 110.8(2) . . ? C52 C53 C533 107.40(18) . . ? C531 C53 C533 108.2(2) . . ? C53 C531 H53A 109.5 . . ? C53 C531 H53B 109.5 . . ? H53A C531 H53B 109.5 . . ? C53 C531 H53C 109.5 . . ? H53A C531 H53C 109.5 . . ? H53B C531 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C53 C533 H53G 109.5 . . ? C53 C533 H53H 109.5 . . ? H53G C533 H53H 109.5 . . ? C53 C533 H53I 109.5 . . ? H53G C533 H53I 109.5 . . ? H53H C533 H53I 109.5 . . ? C62 C61 N1 126.43(18) . . ? C62 C61 C51 120.24(17) . . ? N1 C61 C51 112.78(16) . . ? C61 C62 H62A 120.0 . . ? C61 C62 H62B 120.0 . . ? H62A C62 H62B 120.0 . . ? C61 N1 Al1 131.89(14) . . ? C61 N1 H1 109.4(19) . . ? Al1 N1 H1 118.2(19) . . ? N1 Al1 C71 111.42(9) . . ? N1 Al1 C81 109.47(8) . . ? C71 Al1 C81 119.17(9) . . ? N1 Al1 C31 98.28(7) . . ? C71 Al1 C31 101.97(8) . . ? C81 Al1 C31 114.44(8) . . ? C72 C71 Al1 125.47(14) . . ? C72 C71 H71A 106.0 . . ? Al1 C71 H71A 106.0 . . ? C72 C71 H71B 106.0 . . ? Al1 C71 H71B 106.0 . . ? H71A C71 H71B 106.3 . . ? C721 C72 C723 109.3(2) . . ? C721 C72 C722 108.8(2) . . ? C723 C72 C722 107.8(2) . . ? C721 C72 C71 110.34(19) . . ? C723 C72 C71 110.10(19) . . ? C722 C72 C71 110.44(18) . . ? C72 C721 H72A 109.5 . . ? C72 C721 H72B 109.5 . . ? H72A C721 H72B 109.5 . . ? C72 C721 H72C 109.5 . . ? H72A C721 H72C 109.5 . . ? H72B C721 H72C 109.5 . . ? C72 C722 H72D 109.5 . . ? C72 C722 H72E 109.5 . . ? H72D C722 H72E 109.5 . . ? C72 C722 H72F 109.5 . . ? H72D C722 H72F 109.5 . . ? H72E C722 H72F 109.5 . . ? C72 C723 H72G 109.5 . . ? C72 C723 H72H 109.5 . . ? H72G C723 H72H 109.5 . . ? C72 C723 H72I 109.5 . . ? H72G C723 H72I 109.5 . . ? H72H C723 H72I 109.5 . . ? C82 C81 Al1 126.18(14) . . ? C82 C81 H81A 105.8 . . ? Al1 C81 H81A 105.8 . . ? C82 C81 H81B 105.8 . . ? Al1 C81 H81B 105.8 . . ? H81A C81 H81B 106.2 . . ? C823 C82 C822 109.61(19) . . ? C823 C82 C821 108.36(19) . . ? C822 C82 C821 108.0(2) . . ? C823 C82 C81 111.01(18) . . ? C822 C82 C81 110.48(17) . . ? C821 C82 C81 109.31(17) . . ? 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 . . ? C82 C822 H82D 109.5 . . ? C82 C822 H82E 109.5 . . ? H82D C822 H82E 109.5 . . ? C82 C822 H82F 109.5 . . ? H82D C822 H82F 109.5 . . ? H82E C822 H82F 109.5 . . ? C82 C823 H82G 109.5 . . ? C82 C823 H82H 109.5 . . ? H82G C823 H82H 109.5 . . ? C82 C823 H82I 109.5 . . ? H82G C823 H82I 109.5 . . ? H82H C823 H82I 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 121.4(12) . . ? C1 C2 H2A 107.0 . . ? C3 C2 H2A 107.0 . . ? C1 C2 H2B 107.0 . . ? C3 C2 H2B 107.0 . . ? H2A C2 H2B 106.7 . . ? C4 C3 C2 123.1(14) . . ? C4 C3 H3A 106.6 . . ? C2 C3 H3A 106.6 . . ? C4 C3 H3B 106.6 . . ? C2 C3 H3B 106.6 . . ? H3A C3 H3B 106.5 . . ? C3 C4 C5 104.4(14) . . ? C3 C4 H4A 110.9 . . ? C5 C4 H4A 110.9 . . ? C3 C4 H4B 110.9 . . ? C5 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? C6 C5 C4 101.3(17) . . ? C6 C5 H5A 111.5 . . ? C4 C5 H5A 111.5 . . ? C6 C5 H5B 111.5 . . ? C4 C5 H5B 111.5 . . ? H5A C5 H5B 109.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1A C2A C3A 109.4(14) . . ? C1A C2A H2A1 109.8 . . ? C3A C2A H2A1 109.8 . . ? C1A C2A H2A2 109.8 . . ? C3A C2A H2A2 109.8 . . ? H2A1 C2A H2A2 108.2 . . ? C4A C3A C2A 110.4(12) . . ? C4A C3A H3A1 109.6 . . ? C2A C3A H3A1 109.6 . . ? C4A C3A H3A2 109.6 . . ? C2A C3A H3A2 109.6 . . ? H3A1 C3A H3A2 108.1 . . ? C3A C4A C5A 101.6(14) . . ? C3A C4A H4A1 111.5 . . ? C5A C4A H4A1 111.5 . . ? C3A C4A H4A2 111.5 . . ? C5A C4A H4A2 111.5 . . ? H4A1 C4A H4A2 109.3 . . ? C6A C5A C4A 109.3(13) . . ? C6A C5A H5A1 109.8 . . ? C4A C5A H5A1 109.8 . . ? C6A C5A H5A2 109.8 . . ? C4A C5A H5A2 109.8 . . ? H5A1 C5A H5A2 108.3 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C02 C01 H01A 109.5 . . ? C02 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? C02 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? C01 C02 C03 101.7(12) . . ? C01 C02 H02A 111.4 . . ? C03 C02 H02A 111.4 . . ? C01 C02 H02B 111.4 . . ? C03 C02 H02B 111.4 . . ? H02A C02 H02B 109.3 . . ? C04 C03 C02 105.9(14) . . ? C04 C03 H03A 110.5 . . ? C02 C03 H03A 110.5 . . ? C04 C03 H03B 110.5 . . ? C02 C03 H03B 110.5 . . ? H03A C03 H03B 108.7 . . ? C03 C04 C05 112.6(14) . . ? C03 C04 H04A 109.1 . . ? C05 C04 H04A 109.1 . . ? C03 C04 H04B 109.1 . . ? C05 C04 H04B 109.1 . . ? H04A C04 H04B 107.8 . . ? C06 C05 C04 115.0(12) . . ? C06 C05 H05A 108.5 . . ? C04 C05 H05A 108.5 . . ? C06 C05 H05B 108.5 . . ? C04 C05 H05B 108.5 . . ? H05A C05 H05B 107.5 . . ? C05 C06 H06A 109.5 . . ? C05 C06 H06B 109.5 . . ? H06A C06 H06B 109.5 . . ? C05 C06 H06C 109.5 . . ? H06A C06 H06C 109.5 . . ? H06B C06 H06C 109.5 . . ? C0B C0A H0A1 109.5 . . ? C0B C0A H0A2 109.5 . . ? H0A1 C0A H0A2 109.5 . . ? C0B C0A H0A3 109.5 . . ? H0A1 C0A H0A3 109.5 . . ? H0A2 C0A H0A3 109.5 . . ? C0A C0B C0C 112(2) . . ? C0A C0B H0B1 109.2 . . ? C0C C0B H0B1 109.2 . . ? C0A C0B H0B2 109.2 . . ? C0C C0B H0B2 109.2 . . ? H0B1 C0B H0B2 107.9 . . ? C0D C0C C0B 116(2) . . ? C0D C0C H0C1 108.2 . . ? C0B C0C H0C1 108.2 . . ? C0D C0C H0C2 108.2 . . ? C0B C0C H0C2 108.2 . . ? H0C1 C0C H0C2 107.4 . . ? C0C C0D C0E 112(2) . . ? C0C C0D H0D1 109.2 . . ? C0E C0D H0D1 109.2 . . ? C0C C0D H0D2 109.2 . . ? C0E C0D H0D2 109.2 . . ? H0D1 C0D H0D2 107.9 . . ? C0F C0E C0D 108(2) . . ? C0F C0E H0E1 110.1 . . ? C0D C0E H0E1 110.1 . . ? C0F C0E H0E2 110.1 . . ? C0D C0E H0E2 110.1 . . ? H0E1 C0E H0E2 108.4 . . ? C0E C0F H0F1 109.5 . . ? C0E C0F H0F2 109.5 . . ? H0F1 C0F H0F2 109.5 . . ? C0E C0F H0F3 109.5 . . ? H0F1 C0F H0F3 109.5 . . ? H0F2 C0F H0F3 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 C31 P1 C11 C16 -163.81(14) . . . . ? C41 P1 C11 C16 81.12(16) . . . . ? C51 P1 C11 C16 -44.32(16) . . . . ? C31 P1 C11 C12 16.94(18) . . . . ? C41 P1 C11 C12 -98.12(15) . . . . ? C51 P1 C11 C12 136.44(14) . . . . ? C16 C11 C12 C13 4.4(3) . . . . ? P1 C11 C12 C13 -176.31(14) . . . . ? C16 C11 C12 C121 -171.89(18) . . . . ? P1 C11 C12 C121 7.4(3) . . . . ? C11 C12 C13 C14 -1.4(3) . . . . ? C121 C12 C13 C14 175.28(19) . . . . ? C12 C13 C14 C15 -1.9(3) . . . . ? C12 C13 C14 C141 179.5(2) . . . . ? C13 C14 C15 C16 2.1(3) . . . . ? C141 C14 C15 C16 -179.3(2) . . . . ? C14 C15 C16 C11 1.0(3) . . . . ? C14 C15 C16 C161 -175.24(19) . . . . ? C12 C11 C16 C15 -4.3(3) . . . . ? P1 C11 C16 C15 176.48(14) . . . . ? C12 C11 C16 C161 171.48(18) . . . . ? P1 C11 C16 C161 -7.8(3) . . . . ? C41 P2 C21 C22 -46.31(18) . . . . ? C32 P2 C21 C22 55.17(18) . . . . ? C41 P2 C21 C26 132.55(14) . . . . ? C32 P2 C21 C26 -125.97(14) . . . . ? C26 C21 C22 C23 -0.4(3) . . . . ? P2 C21 C22 C23 178.38(16) . . . . ? C26 C21 C22 C221 -179.48(18) . . . . ? P2 C21 C22 C221 -0.6(3) . . . . ? C21 C22 C23 C24 -0.1(4) . . . . ? C221 C22 C23 C24 179.0(2) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C22 C23 C24 C241 -179.6(3) . . . . ? C23 C24 C25 C26 -0.5(4) . . . . ? C241 C24 C25 C26 179.6(3) . . . . ? C24 C25 C26 C21 0.0(4) . . . . ? C24 C25 C26 C261 -177.9(2) . . . . ? C22 C21 C26 C25 0.5(3) . . . . ? P2 C21 C26 C25 -178.43(17) . . . . ? C22 C21 C26 C261 178.28(18) . . . . ? P2 C21 C26 C261 -0.7(3) . . . . ? C41 P1 C31 C32 8.73(15) . . . . ? C51 P1 C31 C32 129.89(14) . . . . ? C11 P1 C31 C32 -109.74(14) . . . . ? C41 P1 C31 Al1 -161.70(8) . . . . ? C51 P1 C31 Al1 -40.54(11) . . . . ? C11 P1 C31 Al1 79.83(11) . . . . ? P1 C31 C32 C33 -179.83(15) . . . . ? Al1 C31 C32 C33 -13.7(3) . . . . ? P1 C31 C32 P2 9.69(19) . . . . ? Al1 C31 C32 P2 175.77(12) . . . . ? C41 P2 C32 C31 -23.07(16) . . . . ? C21 P2 C32 C31 -133.06(15) . . . . ? C41 P2 C32 C33 165.69(14) . . . . ? C21 P2 C32 C33 55.70(15) . . . . ? C31 C32 C33 C332 -18.7(3) . . . . ? P2 C32 C33 C332 151.97(15) . . . . ? C31 C32 C33 C331 101.4(2) . . . . ? P2 C32 C33 C331 -87.97(18) . . . . ? C31 C32 C33 C333 -137.4(2) . . . . ? P2 C32 C33 C333 33.3(2) . . . . ? C31 P1 C41 C42 163.76(15) . . . . ? C51 P1 C41 C42 48.64(18) . . . . ? C11 P1 C41 C42 -72.66(17) . . . . ? C31 P1 C41 P2 -22.70(10) . . . . ? C51 P1 C41 P2 -137.82(9) . . . . ? C11 P1 C41 P2 100.88(10) . . . . ? C21 P2 C41 C42 -52.2(2) . . . . ? C32 P2 C41 C42 -162.80(19) . . . . ? C21 P2 C41 P1 135.56(9) . . . . ? C32 P2 C41 P1 24.96(10) . . . . ? P1 C41 C42 C43 172.59(18) . . . . ? P2 C41 C42 C43 1.2(4) . . . . ? C41 C42 C43 C431 -20.9(3) . . . . ? C41 C42 C43 C432 -140.1(2) . . . . ? C41 C42 C43 C433 102.7(3) . . . . ? C31 P1 C51 C52 -97.77(16) . . . . ? C41 P1 C51 C52 15.12(18) . . . . ? C11 P1 C51 C52 136.78(15) . . . . ? C31 P1 C51 C61 79.16(14) . . . . ? C41 P1 C51 C61 -167.96(12) . . . . ? C11 P1 C51 C61 -46.30(15) . . . . ? C61 C51 C52 C53 -3.1(4) . . . . ? P1 C51 C52 C53 173.00(17) . . . . ? C51 C52 C53 C532 -28.9(3) . . . . ? C51 C52 C53 C531 -149.4(2) . . . . ? C51 C52 C53 C533 94.6(3) . . . . ? C52 C51 C61 C62 -58.9(3) . . . . ? P1 C51 C61 C62 124.67(19) . . . . ? C52 C51 C61 N1 129.0(2) . . . . ? P1 C51 C61 N1 -47.4(2) . . . . ? C62 C61 N1 Al1 168.09(18) . . . . ? C51 C61 N1 Al1 -20.5(3) . . . . ? C61 N1 Al1 C71 -58.3(2) . . . . ? C61 N1 Al1 C81 167.73(18) . . . . ? C61 N1 Al1 C31 48.1(2) . . . . ? C32 C31 Al1 N1 -172.3(2) . . . . ? P1 C31 Al1 N1 -5.98(11) . . . . ? C32 C31 Al1 C71 -58.2(2) . . . . ? P1 C31 Al1 C71 108.10(10) . . . . ? C32 C31 Al1 C81 71.9(2) . . . . ? P1 C31 Al1 C81 -121.84(10) . . . . ? N1 Al1 C71 C72 -78.49(19) . . . . ? C81 Al1 C71 C72 50.5(2) . . . . ? C31 Al1 C71 C72 177.56(17) . . . . ? Al1 C71 C72 C721 53.5(2) . . . . ? Al1 C71 C72 C723 -67.2(2) . . . . ? Al1 C71 C72 C722 173.85(17) . . . . ? N1 Al1 C81 C82 16.8(2) . . . . ? C71 Al1 C81 C82 -113.07(19) . . . . ? C31 Al1 C81 C82 125.97(18) . . . . ? Al1 C81 C82 C823 54.6(2) . . . . ? Al1 C81 C82 C822 -67.3(2) . . . . ? Al1 C81 C82 C821 174.03(17) . . . . ? C1 C2 C3 C4 178.0(16) . . . . ? C2 C3 C4 C5 171.9(19) . . . . ? C3 C4 C5 C6 -121(2) . . . . ? C1A C2A C3A C4A 176.6(18) . . . . ? C2A C3A C4A C5A 177.2(17) . . . . ? C3A C4A C5A C6A -168.4(19) . . . . ? C01 C02 C03 C04 178.3(14) . . . . ? C02 C03 C04 C05 -170.8(12) . . . . ? C03 C04 C05 C06 -152.5(15) . . . . ? C0A C0B C0C C0D 167(4) . . . . ? C0B C0C C0D C0E -116(5) . . . . ? C0C C0D C0E C0F -38(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.546 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.123 data_sad1d _database_code_depnum_ccdc_archive 'CCDC 878407' #TrackingRef '- Compound8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H80 Al F2 N P2' _chemical_formula_weight 870.11 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' F F 0.0727 0.0534 '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 12.0290(3) _cell_length_b 13.5846(3) _cell_length_c 18.2054(4) _cell_angle_alpha 76.0130(10) _cell_angle_beta 85.9320(10) _cell_angle_gamma 63.7400(10) _cell_volume 2586.59(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6263 _cell_measurement_theta_min 2.504 _cell_measurement_theta_max 72.150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.241 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8965 _exptl_absorpt_correction_T_max 0.9637 _exptl_absorpt_process_details SADABS _exptl_special_details ; The measurement was carried out with copper radiation. The completeness in such measurements is generally lower than the completeness in measurements with Mo radiation, particularly when the crystal symmetry (redundancy within the measurement) is low (triclinic in our case). Furthermore, the problem is aggravated when the measurement is carried out to angles in 2 theta well above the requied minimum of 135 degrees. We always carry our measurements to the physical maximum of 150. When tested, our data showed a substancial increase in completeness when reduced to the required minimum in 2 theta. Since we are primarily interested in maximum crystallographic information and not maximized statistics, we used the complete measurement for the structure determination. ; _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 14529 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 65.00 _reflns_number_total 8002 _reflns_number_gt 5840 _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^)+(0.1024P)^2^+1.7856P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8002 _refine_ls_number_parameters 529 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.014 _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 0.10688(7) 0.80393(7) 0.22027(5) 0.0211(2) Uani 1 1 d . . . C11 C 0.1030(3) 0.9444(3) 0.19067(18) 0.0222(7) Uani 1 1 d . . . C12 C 0.2001(3) 0.9560(3) 0.14587(19) 0.0254(7) Uani 1 1 d . . . C121 C 0.3066(3) 0.8616(3) 0.1197(2) 0.0306(8) Uani 1 1 d . . . H12A H 0.3593 0.8907 0.0898 0.037 Uiso 1 1 calc R . . H12B H 0.2750 0.8298 0.0896 0.037 Uiso 1 1 calc R . . H12C H 0.3534 0.8043 0.1629 0.037 Uiso 1 1 calc R . . C13 C 0.2000(3) 1.0619(3) 0.1249(2) 0.0290(8) Uani 1 1 d . . . H13 H 0.2653 1.0699 0.0944 0.035 Uiso 1 1 calc R . . C14 C 0.1097(3) 1.1556(3) 0.1463(2) 0.0306(8) Uani 1 1 d . . . C141 C 0.1127(4) 1.2687(3) 0.1240(2) 0.0434(10) Uani 1 1 d . . . H14A H 0.0510 1.3178 0.0843 0.052 Uiso 1 1 calc R . . H14B H 0.1932 1.2590 0.1063 0.052 Uiso 1 1 calc R . . H14C H 0.0958 1.3015 0.1671 0.052 Uiso 1 1 calc R . . C15 C 0.0157(3) 1.1429(3) 0.1889(2) 0.0293(8) Uani 1 1 d . . . H15 H -0.0487 1.2079 0.2030 0.035 Uiso 1 1 calc R . . C16 C 0.0099(3) 1.0398(3) 0.21258(19) 0.0254(7) Uani 1 1 d . . . C161 C -0.0968(3) 1.0400(3) 0.2612(2) 0.0377(9) Uani 1 1 d . . . H16A H -0.0657 0.9953 0.3113 0.045 Uiso 1 1 calc R . . H16B H -0.1408 1.0088 0.2396 0.045 Uiso 1 1 calc R . . H16C H -0.1520 1.1161 0.2636 0.045 Uiso 1 1 calc R . . P2 P 0.34334(7) 0.59673(7) 0.21956(5) 0.0242(2) Uani 1 1 d . . . C21 C 0.3823(3) 0.4564(3) 0.2838(2) 0.0278(8) Uani 1 1 d . . . C22 C 0.5082(3) 0.3763(3) 0.2853(2) 0.0316(8) Uani 1 1 d . . . C221 C 0.6026(3) 0.3968(3) 0.2330(3) 0.0443(10) Uani 1 1 d . . . H22A H 0.6817 0.3321 0.2444 0.053 Uiso 1 1 calc R . . H22B H 0.6092 0.4619 0.2397 0.053 Uiso 1 1 calc R . . H22C H 0.5770 0.4094 0.1814 0.053 Uiso 1 1 calc R . . C23 C 0.5461(4) 0.2709(3) 0.3352(2) 0.0401(10) Uani 1 1 d . . . H23 H 0.6309 0.2161 0.3356 0.048 Uiso 1 1 calc R . . C24 C 0.4672(4) 0.2421(3) 0.3841(2) 0.0428(10) Uani 1 1 d . . . C241 C 0.5115(5) 0.1265(4) 0.4385(3) 0.0653(15) Uani 1 1 d . . . H24A H 0.5095 0.0735 0.4126 0.078 Uiso 1 1 calc R . . H24B H 0.4581 0.1311 0.4806 0.078 Uiso 1 1 calc R . . H24C H 0.5948 0.1019 0.4565 0.078 Uiso 1 1 calc R . . C25 C 0.3440(4) 0.3206(3) 0.3809(2) 0.0425(10) Uani 1 1 d . . . H25 H 0.2873 0.3011 0.4139 0.051 Uiso 1 1 calc R . . C26 C 0.2998(3) 0.4267(3) 0.3313(2) 0.0334(9) Uani 1 1 d . . . C261 C 0.1646(3) 0.5059(3) 0.3302(3) 0.0443(11) Uani 1 1 d . . . H26A H 0.1214 0.4666 0.3606 0.053 Uiso 1 1 calc R . . H26B H 0.1311 0.5334 0.2791 0.053 Uiso 1 1 calc R . . H26C H 0.1547 0.5683 0.3503 0.053 Uiso 1 1 calc R . . C31 C 0.1245(3) 0.7418(3) 0.14023(18) 0.0222(7) Uani 1 1 d . . . C32 C 0.2192(3) 0.6365(3) 0.14764(19) 0.0242(7) Uani 1 1 d . . . C33 C 0.2482(3) 0.5604(3) 0.0914(2) 0.0312(8) Uani 1 1 d . . . C331 C 0.1324(4) 0.5833(4) 0.0470(2) 0.0420(10) Uani 1 1 d . . . H33A H 0.0704 0.5777 0.0818 0.050 Uiso 1 1 calc R . . H33B H 0.1536 0.5289 0.0169 0.050 Uiso 1 1 calc R . . H33C H 0.1004 0.6579 0.0145 0.050 Uiso 1 1 calc R . . C332 C 0.3429(4) 0.5791(4) 0.0355(3) 0.0488(11) Uani 1 1 d . . . H33D H 0.3053 0.6543 0.0041 0.059 Uiso 1 1 calc R . . H33E H 0.3688 0.5256 0.0043 0.059 Uiso 1 1 calc R . . H33F H 0.4136 0.5691 0.0632 0.059 Uiso 1 1 calc R . . C333 C 0.3052(5) 0.4352(3) 0.1318(3) 0.0531(12) Uani 1 1 d . . . H33G H 0.3833 0.4147 0.1560 0.064 Uiso 1 1 calc R . . H33H H 0.3180 0.3907 0.0955 0.064 Uiso 1 1 calc R . . H33I H 0.2501 0.4216 0.1692 0.064 Uiso 1 1 calc R . . C41 C 0.2544(3) 0.7083(3) 0.27019(18) 0.0221(7) Uani 1 1 d . . . C42 C 0.2849(3) 0.7427(3) 0.32557(19) 0.0281(8) Uani 1 1 d . . . H42 H 0.2212 0.8133 0.3329 0.034 Uiso 1 1 calc R . . C43 C 0.3963(3) 0.6957(3) 0.3789(2) 0.0362(9) Uani 1 1 d . . . C431 C 0.4512(4) 0.7813(4) 0.3606(3) 0.0578(13) Uani 1 1 d . . . H43A H 0.5173 0.7589 0.3967 0.069 Uiso 1 1 calc R . . H43B H 0.3877 0.8547 0.3629 0.069 Uiso 1 1 calc R . . H43C H 0.4828 0.7839 0.3106 0.069 Uiso 1 1 calc R . . C432 C 0.4966(4) 0.5800(4) 0.3726(3) 0.0520(12) Uani 1 1 d . . . H43D H 0.4650 0.5248 0.3885 0.062 Uiso 1 1 calc R . . H43E H 0.5675 0.5596 0.4043 0.062 Uiso 1 1 calc R . . H43F H 0.5203 0.5828 0.3209 0.062 Uiso 1 1 calc R . . C433 C 0.3496(5) 0.6912(5) 0.4596(2) 0.0662(15) Uani 1 1 d . . . H43G H 0.3120 0.6402 0.4713 0.079 Uiso 1 1 calc R . . H43H H 0.2895 0.7653 0.4633 0.079 Uiso 1 1 calc R . . H43I H 0.4181 0.6652 0.4948 0.079 Uiso 1 1 calc R . . C51 C -0.0254(3) 0.7950(3) 0.26939(18) 0.0227(7) Uani 1 1 d . . . C52 C -0.0118(3) 0.7704(3) 0.3456(2) 0.0312(8) Uani 1 1 d . . . H52 H 0.0661 0.7608 0.3640 0.037 Uiso 1 1 calc R . . C53 C -0.0984(4) 0.7557(3) 0.4067(2) 0.0348(9) Uani 1 1 d . . . C531 C -0.1707(4) 0.8667(4) 0.4299(2) 0.0519(12) Uani 1 1 d . . . H53A H -0.1138 0.8904 0.4457 0.062 Uiso 1 1 calc R . . H53B H -0.2221 0.8568 0.4711 0.062 Uiso 1 1 calc R . . H53C H -0.2217 0.9230 0.3877 0.062 Uiso 1 1 calc R . . C532 C -0.0227(4) 0.6657(4) 0.4749(2) 0.0518(11) Uani 1 1 d . . . H53D H 0.0216 0.5949 0.4609 0.062 Uiso 1 1 calc R . . H53E H -0.0772 0.6584 0.5148 0.062 Uiso 1 1 calc R . . H53F H 0.0352 0.6870 0.4922 0.062 Uiso 1 1 calc R . . C533 C -0.1898(4) 0.7181(4) 0.3820(2) 0.0515(12) Uani 1 1 d . . . H53G H -0.2444 0.7765 0.3419 0.062 Uiso 1 1 calc R . . H53H H -0.2375 0.7039 0.4242 0.062 Uiso 1 1 calc R . . H53I H -0.1446 0.6503 0.3643 0.062 Uiso 1 1 calc R . . N1 N -0.0856(3) 0.8748(3) 0.10383(19) 0.0300(7) Uani 1 1 d . . . H1 H -0.124(3) 0.924(3) 0.0729(18) 0.007(8) Uiso 1 1 d . . . C61 C 0.0326(3) 0.8237(3) 0.07796(19) 0.0246(7) Uani 1 1 d . . . C62 C 0.0696(3) 0.8538(3) 0.0088(2) 0.0330(8) Uani 1 1 d . . . H62A H 0.0119 0.9162 -0.0281 0.040 Uiso 1 1 calc R . . H62B H 0.1540 0.8131 -0.0041 0.040 Uiso 1 1 calc R . . Al1 Al -0.15813(9) 0.82369(8) 0.18981(6) 0.0252(3) Uani 1 1 d . . . C71 C -0.3246(3) 0.9437(3) 0.2094(2) 0.0283(8) Uani 1 1 d . . . H71A H -0.3743 0.9045 0.2283 0.034 Uiso 1 1 calc R . . H71B H -0.3096 0.9684 0.2513 0.034 Uiso 1 1 calc R . . C72 C -0.4107(3) 1.0525(3) 0.1527(2) 0.0353(9) Uani 1 1 d . . . C721 C -0.4388(4) 1.0259(3) 0.0815(2) 0.0459(10) Uani 1 1 d . . . H72A H -0.3631 0.9913 0.0566 0.055 Uiso 1 1 calc R . . H72B H -0.4945 1.0946 0.0479 0.055 Uiso 1 1 calc R . . H72C H -0.4765 0.9752 0.0951 0.055 Uiso 1 1 calc R . . C722 C -0.5341(4) 1.1110(4) 0.1902(3) 0.0512(12) Uani 1 1 d . . . H72D H -0.5722 1.0606 0.2047 0.061 Uiso 1 1 calc R . . H72E H -0.5885 1.1781 0.1549 0.061 Uiso 1 1 calc R . . H72F H -0.5184 1.1307 0.2343 0.061 Uiso 1 1 calc R . . C723 C -0.3535(4) 1.1358(3) 0.1307(3) 0.0508(12) Uani 1 1 d . . . H72G H -0.3444 1.1591 0.1747 0.061 Uiso 1 1 calc R . . H72H H -0.4067 1.2005 0.0933 0.061 Uiso 1 1 calc R . . H72I H -0.2736 1.0998 0.1103 0.061 Uiso 1 1 calc R . . C81 C -0.1451(3) 0.6705(3) 0.1914(2) 0.0300(8) Uani 1 1 d . . . H81A H -0.0624 0.6270 0.1773 0.036 Uiso 1 1 calc R . . H81B H -0.1508 0.6363 0.2433 0.036 Uiso 1 1 calc R . . C82 C -0.2323(3) 0.6512(3) 0.1447(2) 0.0324(8) Uani 1 1 d . . . C821 C -0.2416(4) 0.7156(4) 0.0621(2) 0.0541(12) Uani 1 1 d . . . H82A H -0.2888 0.6966 0.0323 0.065 Uiso 1 1 calc R . . H82B H -0.1599 0.6952 0.0430 0.065 Uiso 1 1 calc R . . H82C H -0.2820 0.7953 0.0590 0.065 Uiso 1 1 calc R . . C822 C -0.3598(4) 0.6898(4) 0.1769(3) 0.0540(12) Uani 1 1 d . . . H82D H -0.4128 0.6764 0.1476 0.065 Uiso 1 1 calc R . . H82E H -0.3939 0.7691 0.1750 0.065 Uiso 1 1 calc R . . H82F H -0.3539 0.6486 0.2285 0.065 Uiso 1 1 calc R . . C823 C -0.1823(4) 0.5262(3) 0.1450(3) 0.0494(11) Uani 1 1 d . . . H82G H -0.1723 0.4827 0.1963 0.059 Uiso 1 1 calc R . . H82H H -0.1036 0.5017 0.1217 0.059 Uiso 1 1 calc R . . H82I H -0.2396 0.5157 0.1173 0.059 Uiso 1 1 calc R . . F1 F 0.1074(16) -0.0151(10) 0.4227(11) 0.261(9) Uiso 0.583(9) 1 d PD A 1 F2 F 0.2404(9) 0.0790(8) 0.3583(6) 0.152(4) Uiso 0.583(9) 1 d PD A 1 C1 C 0.0475(4) 0.1052(3) 0.3935(3) 0.059(2) Uiso 0.583(9) 1 d PGD A 1 C2 C 0.1200(5) 0.1574(4) 0.3576(4) 0.083(3) Uiso 0.583(9) 1 d PGD A 1 C3 C 0.0670(6) 0.2739(4) 0.3301(4) 0.069(3) Uiso 0.583(9) 1 d PGD A 1 H3 H 0.1171 0.3099 0.3053 0.083 Uiso 0.583(9) 1 calc PR A 1 C4 C -0.0585(7) 0.3383(3) 0.3387(4) 0.076(3) Uiso 0.583(9) 1 d PGD A 1 H4 H -0.0951 0.4188 0.3197 0.091 Uiso 0.583(9) 1 calc PR A 1 C5 C -0.1310(5) 0.2862(3) 0.3746(4) 0.076(3) Uiso 0.583(9) 1 d PGD A 1 H5 H -0.2177 0.3307 0.3805 0.091 Uiso 0.583(9) 1 calc PR A 1 C6 C -0.0780(4) 0.1696(3) 0.4020(3) 0.063(2) Uiso 0.583(9) 1 d PGD A 1 H6 H -0.1281 0.1336 0.4269 0.076 Uiso 0.583(9) 1 calc PR A 1 F1A F -0.1253(4) 0.1274(4) 0.4271(4) 0.131(5) Uiso 0.417(9) 1 d PGD A 2 F2A F 0.1009(5) -0.0082(3) 0.4184(4) 0.065(3) Uiso 0.417(9) 1 d PGD A 2 C1A C -0.0293(9) 0.1642(7) 0.3907(5) 0.065(4) Uiso 0.417(9) 1 d PGD A 2 C2A C 0.0947(10) 0.0897(5) 0.3875(6) 0.087(5) Uiso 0.417(9) 1 d PGD A 2 C3A C 0.1777(8) 0.1299(7) 0.3521(7) 0.121(7) Uiso 0.417(9) 1 d PGD A 2 H3A H 0.2634 0.0785 0.3498 0.145 Uiso 0.417(9) 1 calc PR A 2 C4A C 0.1368(8) 0.2445(8) 0.3199(6) 0.065(4) Uiso 0.417(9) 1 d PGD A 2 H4A H 0.1942 0.2723 0.2955 0.078 Uiso 0.417(9) 1 calc PR A 2 C5A C 0.0129(9) 0.3190(6) 0.3232(5) 0.045(3) Uiso 0.417(9) 1 d PGD A 2 H5A H -0.0154 0.3982 0.3010 0.054 Uiso 0.417(9) 1 calc PR A 2 C6A C -0.0702(7) 0.2789(7) 0.3586(5) 0.072(4) Uiso 0.417(9) 1 d PGD A 2 H6A H -0.1558 0.3303 0.3608 0.087 Uiso 0.417(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0173(4) 0.0202(4) 0.0247(4) -0.0054(3) -0.0002(3) -0.0070(3) C11 0.0204(16) 0.0211(16) 0.0252(17) -0.0059(14) -0.0061(14) -0.0079(13) C12 0.0238(16) 0.0224(17) 0.0272(18) -0.0036(15) -0.0040(14) -0.0081(14) C121 0.0246(17) 0.0256(18) 0.040(2) -0.0035(16) 0.0043(16) -0.0119(15) C13 0.0270(17) 0.0281(18) 0.0308(19) -0.0027(16) -0.0015(15) -0.0129(15) C14 0.0360(19) 0.0241(18) 0.0320(19) -0.0031(16) -0.0076(16) -0.0139(16) C141 0.052(2) 0.028(2) 0.053(3) -0.0112(19) 0.006(2) -0.0195(18) C15 0.0273(17) 0.0235(18) 0.035(2) -0.0124(16) -0.0016(16) -0.0066(14) C16 0.0235(16) 0.0270(18) 0.0261(17) -0.0080(15) -0.0034(14) -0.0100(14) C161 0.0307(19) 0.030(2) 0.056(2) -0.0207(19) 0.0100(18) -0.0119(16) P2 0.0191(4) 0.0200(4) 0.0311(5) -0.0037(4) 0.0005(4) -0.0074(3) C21 0.0290(18) 0.0177(16) 0.0325(19) -0.0037(15) -0.0001(16) -0.0074(14) C22 0.0266(18) 0.0244(18) 0.040(2) -0.0062(16) -0.0001(16) -0.0084(15) C221 0.0245(18) 0.032(2) 0.067(3) -0.006(2) 0.0035(19) -0.0072(16) C23 0.0313(19) 0.0258(19) 0.052(2) -0.0049(18) -0.0002(19) -0.0041(16) C24 0.044(2) 0.0247(19) 0.047(2) 0.0009(18) 0.001(2) -0.0078(17) C241 0.066(3) 0.033(2) 0.068(3) 0.011(2) 0.004(3) -0.008(2) C25 0.047(2) 0.032(2) 0.043(2) -0.0015(18) 0.013(2) -0.0164(18) C26 0.034(2) 0.0235(18) 0.036(2) -0.0021(16) 0.0038(17) -0.0094(15) C261 0.033(2) 0.032(2) 0.058(3) 0.002(2) 0.012(2) -0.0127(17) C31 0.0200(15) 0.0215(16) 0.0251(17) -0.0039(14) 0.0023(14) -0.0103(13) C32 0.0208(16) 0.0243(17) 0.0276(18) -0.0038(15) 0.0036(14) -0.0116(14) C33 0.0280(18) 0.0292(19) 0.038(2) -0.0131(17) 0.0031(16) -0.0113(15) C331 0.037(2) 0.048(2) 0.049(2) -0.030(2) 0.0040(19) -0.0170(19) C332 0.041(2) 0.058(3) 0.056(3) -0.035(2) 0.021(2) -0.021(2) C333 0.073(3) 0.028(2) 0.055(3) -0.016(2) -0.009(2) -0.015(2) C41 0.0165(15) 0.0213(16) 0.0269(17) -0.0019(14) 0.0007(14) -0.0088(13) C42 0.0249(17) 0.0283(18) 0.0305(19) -0.0051(16) 0.0000(15) -0.0119(15) C43 0.0300(19) 0.041(2) 0.036(2) -0.0079(18) -0.0092(17) -0.0129(17) C431 0.040(2) 0.059(3) 0.083(4) -0.027(3) -0.012(2) -0.022(2) C432 0.040(2) 0.048(3) 0.058(3) -0.010(2) -0.022(2) -0.008(2) C433 0.059(3) 0.082(4) 0.037(2) -0.011(3) -0.015(2) -0.012(3) C51 0.0194(15) 0.0206(16) 0.0260(17) -0.0041(14) 0.0017(14) -0.0077(13) C52 0.0256(17) 0.0299(19) 0.036(2) -0.0085(16) -0.0010(16) -0.0091(15) C53 0.037(2) 0.040(2) 0.0284(19) -0.0091(17) 0.0032(16) -0.0175(17) C531 0.055(3) 0.062(3) 0.037(2) -0.019(2) 0.017(2) -0.023(2) C532 0.048(3) 0.062(3) 0.037(2) -0.003(2) 0.008(2) -0.022(2) C533 0.047(2) 0.082(3) 0.036(2) -0.012(2) 0.012(2) -0.040(2) N1 0.0215(14) 0.0278(16) 0.0310(17) 0.0016(15) -0.0042(14) -0.0057(13) C61 0.0247(17) 0.0226(17) 0.0274(18) -0.0091(14) 0.0011(15) -0.0096(14) C62 0.0300(18) 0.031(2) 0.0277(19) -0.0036(16) 0.0011(16) -0.0059(15) Al1 0.0187(5) 0.0257(5) 0.0294(5) -0.0056(4) 0.0006(4) -0.0086(4) C71 0.0236(17) 0.0295(18) 0.0345(19) -0.0098(16) 0.0024(15) -0.0131(15) C72 0.0246(18) 0.0268(19) 0.048(2) -0.0089(18) -0.0010(17) -0.0054(15) C721 0.035(2) 0.039(2) 0.048(2) -0.002(2) -0.0116(19) -0.0041(18) C722 0.030(2) 0.040(2) 0.074(3) -0.021(2) -0.001(2) -0.0026(18) C723 0.046(2) 0.027(2) 0.069(3) 0.002(2) -0.005(2) -0.0127(18) C81 0.0257(17) 0.0307(19) 0.0319(19) -0.0102(16) 0.0030(15) -0.0096(15) C82 0.0267(18) 0.0298(19) 0.042(2) -0.0145(17) 0.0028(16) -0.0104(15) C821 0.057(3) 0.065(3) 0.045(3) -0.014(2) -0.012(2) -0.028(2) C822 0.033(2) 0.052(3) 0.093(4) -0.038(3) 0.016(2) -0.024(2) C823 0.041(2) 0.043(2) 0.069(3) -0.027(2) 0.001(2) -0.015(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 C51 1.807(3) . ? P1 C31 1.809(3) . ? P1 C41 1.811(3) . ? P1 C11 1.833(3) . ? C11 C16 1.412(5) . ? C11 C12 1.421(5) . ? C12 C13 1.396(5) . ? C12 C121 1.506(5) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C13 C14 1.381(5) . ? C13 H13 0.9600 . ? C14 C15 1.376(5) . ? C14 C141 1.507(5) . ? C141 H14A 0.9599 . ? C141 H14B 0.9599 . ? C141 H14C 0.9599 . ? C15 C16 1.394(5) . ? C15 H15 0.9600 . ? C16 C161 1.506(5) . ? C161 H16A 0.9599 . ? C161 H16B 0.9599 . ? C161 H16C 0.9599 . ? P2 C41 1.842(3) . ? P2 C21 1.853(3) . ? P2 C32 1.860(3) . ? C21 C26 1.399(5) . ? C21 C22 1.419(5) . ? C22 C23 1.392(5) . ? C22 C221 1.507(5) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C23 C24 1.373(6) . ? C23 H23 0.9600 . ? C24 C25 1.386(5) . ? C24 C241 1.521(5) . ? C241 H24A 0.9599 . ? C241 H24B 0.9599 . ? C241 H24C 0.9599 . ? C25 C26 1.391(5) . ? C25 H25 0.9600 . ? C26 C261 1.500(5) . ? C261 H26A 0.9599 . ? C261 H26B 0.9599 . ? C261 H26C 0.9599 . ? C31 C32 1.360(4) . ? C31 C61 1.491(4) . ? C32 C33 1.543(5) . ? C33 C333 1.529(5) . ? C33 C331 1.531(5) . ? C33 C332 1.538(5) . ? C331 H33A 0.9599 . ? C331 H33B 0.9599 . ? C331 H33C 0.9599 . ? C332 H33D 0.9599 . ? C332 H33E 0.9599 . ? C332 H33F 0.9599 . ? C333 H33G 0.9599 . ? C333 H33H 0.9599 . ? C333 H33I 0.9599 . ? C41 C42 1.342(5) . ? C42 C43 1.509(5) . ? C42 H42 0.9600 . ? C43 C432 1.526(6) . ? C43 C433 1.532(6) . ? C43 C431 1.537(6) . ? C431 H43A 0.9599 . ? C431 H43B 0.9599 . ? C431 H43C 0.9599 . ? C432 H43D 0.9599 . ? C432 H43E 0.9599 . ? C432 H43F 0.9599 . ? C433 H43G 0.9599 . ? C433 H43H 0.9599 . ? C433 H43I 0.9599 . ? C51 C52 1.351(5) . ? C51 Al1 2.075(3) . ? C52 C53 1.509(5) . ? C52 H52 0.9600 . ? C53 C531 1.518(6) . ? C53 C532 1.518(5) . ? C53 C533 1.533(6) . ? C531 H53A 0.9599 . ? C531 H53B 0.9599 . ? C531 H53C 0.9599 . ? C532 H53D 0.9599 . ? C532 H53E 0.9599 . ? C532 H53F 0.9599 . ? C533 H53G 0.9599 . ? C533 H53H 0.9599 . ? C533 H53I 0.9599 . ? N1 C61 1.384(4) . ? N1 Al1 1.874(3) . ? N1 H1 0.75(3) . ? C61 C62 1.336(5) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? Al1 C81 2.010(4) . ? Al1 C71 2.022(3) . ? C71 C72 1.543(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C72 C721 1.524(6) . ? C72 C723 1.531(5) . ? C72 C722 1.541(5) . ? C721 H72A 0.9599 . ? C721 H72B 0.9599 . ? C721 H72C 0.9599 . ? C722 H72D 0.9599 . ? C722 H72E 0.9599 . ? C722 H72F 0.9599 . ? C723 H72G 0.9599 . ? C723 H72H 0.9599 . ? C723 H72I 0.9599 . ? C81 C82 1.539(5) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C82 C822 1.510(5) . ? C82 C823 1.528(5) . ? C82 C821 1.531(6) . ? C821 H82A 0.9599 . ? C821 H82B 0.9599 . ? C821 H82C 0.9599 . ? C822 H82D 0.9599 . ? C822 H82E 0.9599 . ? C822 H82F 0.9599 . ? C823 H82G 0.9599 . ? C823 H82H 0.9599 . ? C823 H82I 0.9599 . ? F1 C1 1.437(13) . ? F2 C2 1.365(10) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9600 . ? C4 C5 1.3900 . ? C4 H4 0.9600 . ? C5 C6 1.3900 . ? C5 H5 0.9600 . ? C6 H6 0.9600 . ? F1A C1A 1.506(7) . ? F2A C2A 1.285(7) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C3A H3A 0.9600 . ? C4A C5A 1.3900 . ? C4A H4A 0.9600 . ? C5A C6A 1.3900 . ? C5A H5A 0.9600 . ? C6A H6A 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C51 P1 C31 106.29(15) . . ? C51 P1 C41 114.01(15) . . ? C31 P1 C41 99.40(15) . . ? C51 P1 C11 116.82(15) . . ? C31 P1 C11 111.28(15) . . ? C41 P1 C11 107.68(14) . . ? C16 C11 C12 119.2(3) . . ? C16 C11 P1 122.6(3) . . ? C12 C11 P1 118.2(2) . . ? C13 C12 C11 118.6(3) . . ? C13 C12 C121 116.3(3) . . ? C11 C12 C121 125.1(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 122.6(3) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C15 C14 C13 117.9(3) . . ? C15 C14 C141 120.5(3) . . ? C13 C14 C141 121.7(3) . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C14 C15 C16 122.9(3) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C11 118.8(3) . . ? C15 C16 C161 116.0(3) . . ? C11 C16 C161 125.2(3) . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C41 P2 C21 109.72(15) . . ? C41 P2 C32 96.80(15) . . ? C21 P2 C32 112.15(15) . . ? C26 C21 C22 119.3(3) . . ? C26 C21 P2 125.5(3) . . ? C22 C21 P2 115.2(3) . . ? C23 C22 C21 118.6(3) . . ? C23 C22 C221 117.7(3) . . ? C21 C22 C221 123.6(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 . . ? C24 C23 C22 122.7(3) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 118.0(3) . . ? C23 C24 C241 121.5(4) . . ? C25 C24 C241 120.5(4) . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C24 C25 C26 122.1(4) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 119.3(3) . . ? C25 C26 C261 118.8(3) . . ? C21 C26 C261 121.9(3) . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C32 C31 C61 134.3(3) . . ? C32 C31 P1 115.4(3) . . ? C61 C31 P1 110.3(2) . . ? C31 C32 C33 126.1(3) . . ? C31 C32 P2 115.3(3) . . ? C33 C32 P2 116.9(2) . . ? C333 C33 C331 106.4(3) . . ? C333 C33 C332 107.5(3) . . ? C331 C33 C332 109.2(3) . . ? C333 C33 C32 111.7(3) . . ? C331 C33 C32 112.6(3) . . ? C332 C33 C32 109.1(3) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C42 C41 P1 115.7(3) . . ? C42 C41 P2 133.1(3) . . ? P1 C41 P2 109.87(18) . . ? C41 C42 C43 134.6(3) . . ? C41 C42 H42 112.7 . . ? C43 C42 H42 112.7 . . ? C42 C43 C432 114.5(3) . . ? C42 C43 C433 107.5(3) . . ? C432 C43 C433 110.5(4) . . ? C42 C43 C431 106.5(3) . . ? C432 C43 C431 109.2(3) . . ? C433 C43 C431 108.3(4) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C52 C51 P1 113.9(3) . . ? C52 C51 Al1 137.5(3) . . ? P1 C51 Al1 108.64(16) . . ? C51 C52 C53 130.8(3) . . ? C51 C52 H52 114.6 . . ? C53 C52 H52 114.6 . . ? C52 C53 C531 108.9(3) . . ? C52 C53 C532 109.2(3) . . ? C531 C53 C532 109.1(3) . . ? C52 C53 C533 113.2(3) . . ? C531 C53 C533 109.2(4) . . ? C532 C53 C533 107.3(4) . . ? C53 C531 H53A 109.5 . . ? C53 C531 H53B 109.5 . . ? H53A C531 H53B 109.5 . . ? C53 C531 H53C 109.5 . . ? H53A C531 H53C 109.5 . . ? H53B C531 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C53 C533 H53G 109.5 . . ? C53 C533 H53H 109.5 . . ? H53G C533 H53H 109.5 . . ? C53 C533 H53I 109.5 . . ? H53G C533 H53I 109.5 . . ? H53H C533 H53I 109.5 . . ? C61 N1 Al1 129.8(3) . . ? C61 N1 H1 108(2) . . ? Al1 N1 H1 121(2) . . ? C62 C61 N1 125.9(3) . . ? C62 C61 C31 120.9(3) . . ? N1 C61 C31 112.3(3) . . ? C61 C62 H62A 120.0 . . ? C61 C62 H62B 120.0 . . ? H62A C62 H62B 120.0 . . ? N1 Al1 C81 110.71(15) . . ? N1 Al1 C71 112.88(14) . . ? C81 Al1 C71 118.02(15) . . ? N1 Al1 C51 97.44(14) . . ? C81 Al1 C51 105.38(14) . . ? C71 Al1 C51 110.16(14) . . ? C72 C71 Al1 127.5(3) . . ? C72 C71 H71A 105.4 . . ? Al1 C71 H71A 105.4 . . ? C72 C71 H71B 105.4 . . ? Al1 C71 H71B 105.4 . . ? H71A C71 H71B 106.0 . . ? C721 C72 C723 109.3(4) . . ? C721 C72 C722 108.3(3) . . ? C723 C72 C722 107.5(3) . . ? C721 C72 C71 111.1(3) . . ? C723 C72 C71 111.3(3) . . ? C722 C72 C71 109.1(3) . . ? C72 C721 H72A 109.5 . . ? C72 C721 H72B 109.5 . . ? H72A C721 H72B 109.5 . . ? C72 C721 H72C 109.5 . . ? H72A C721 H72C 109.5 . . ? H72B C721 H72C 109.5 . . ? C72 C722 H72D 109.5 . . ? C72 C722 H72E 109.5 . . ? H72D C722 H72E 109.5 . . ? C72 C722 H72F 109.5 . . ? H72D C722 H72F 109.5 . . ? H72E C722 H72F 109.5 . . ? C72 C723 H72G 109.5 . . ? C72 C723 H72H 109.5 . . ? H72G C723 H72H 109.5 . . ? C72 C723 H72I 109.5 . . ? H72G C723 H72I 109.5 . . ? H72H C723 H72I 109.5 . . ? C82 C81 Al1 123.8(2) . . ? C82 C81 H81A 106.4 . . ? Al1 C81 H81A 106.4 . . ? C82 C81 H81B 106.4 . . ? Al1 C81 H81B 106.4 . . ? H81A C81 H81B 106.5 . . ? C822 C82 C823 108.6(3) . . ? C822 C82 C821 109.6(4) . . ? C823 C82 C821 107.1(3) . . ? C822 C82 C81 110.5(3) . . ? C823 C82 C81 110.9(3) . . ? C821 C82 C81 110.1(3) . . ? 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 . . ? C82 C822 H82D 109.5 . . ? C82 C822 H82E 109.5 . . ? H82D C822 H82E 109.5 . . ? C82 C822 H82F 109.5 . . ? H82D C822 H82F 109.5 . . ? H82E C822 H82F 109.5 . . ? C82 C823 H82G 109.5 . . ? C82 C823 H82H 109.5 . . ? H82G C823 H82H 109.5 . . ? C82 C823 H82I 109.5 . . ? H82G C823 H82I 109.5 . . ? H82H C823 H82I 109.5 . . ? C2 C1 C6 120.0 . . ? C2 C1 F1 117.8(9) . . ? C6 C1 F1 122.2(9) . . ? F2 C2 C1 110.0(5) . . ? F2 C2 C3 130.0(5) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C2A C1A C6A 120.0 . . ? C2A C1A F1A 123.3(6) . . ? C6A C1A F1A 116.7(6) . . ? F2A C2A C3A 135.2(7) . . ? F2A C2A C1A 104.7(7) . . ? C3A C2A C1A 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? 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 C51 P1 C11 C16 7.7(3) . . . . ? C31 P1 C11 C16 130.0(3) . . . . ? C41 P1 C11 C16 -122.1(3) . . . . ? C51 P1 C11 C12 -174.3(2) . . . . ? C31 P1 C11 C12 -52.0(3) . . . . ? C41 P1 C11 C12 55.9(3) . . . . ? C16 C11 C12 C13 -0.1(5) . . . . ? P1 C11 C12 C13 -178.1(3) . . . . ? C16 C11 C12 C121 178.7(3) . . . . ? P1 C11 C12 C121 0.6(5) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C121 C12 C13 C14 -178.5(3) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C12 C13 C14 C141 179.1(3) . . . . ? C13 C14 C15 C16 1.6(5) . . . . ? C141 C14 C15 C16 -178.5(3) . . . . ? C14 C15 C16 C11 -1.3(5) . . . . ? C14 C15 C16 C161 177.9(3) . . . . ? C12 C11 C16 C15 0.5(5) . . . . ? P1 C11 C16 C15 178.5(2) . . . . ? C12 C11 C16 C161 -178.6(3) . . . . ? P1 C11 C16 C161 -0.7(5) . . . . ? C41 P2 C21 C26 46.0(4) . . . . ? C32 P2 C21 C26 -60.4(4) . . . . ? C41 P2 C21 C22 -131.5(3) . . . . ? C32 P2 C21 C22 122.1(3) . . . . ? C26 C21 C22 C23 -1.1(6) . . . . ? P2 C21 C22 C23 176.5(3) . . . . ? C26 C21 C22 C221 175.9(4) . . . . ? P2 C21 C22 C221 -6.5(5) . . . . ? C21 C22 C23 C24 -1.2(6) . . . . ? C221 C22 C23 C24 -178.4(4) . . . . ? C22 C23 C24 C25 2.5(7) . . . . ? C22 C23 C24 C241 -179.6(4) . . . . ? C23 C24 C25 C26 -1.4(7) . . . . ? C241 C24 C25 C26 -179.3(4) . . . . ? C24 C25 C26 C21 -0.9(6) . . . . ? C24 C25 C26 C261 178.8(4) . . . . ? C22 C21 C26 C25 2.2(6) . . . . ? P2 C21 C26 C25 -175.2(3) . . . . ? C22 C21 C26 C261 -177.5(4) . . . . ? P2 C21 C26 C261 5.1(6) . . . . ? C51 P1 C31 C32 -104.5(3) . . . . ? C41 P1 C31 C32 14.1(3) . . . . ? C11 P1 C31 C32 127.3(3) . . . . ? C51 P1 C31 C61 78.6(2) . . . . ? C41 P1 C31 C61 -162.8(2) . . . . ? C11 P1 C31 C61 -49.6(3) . . . . ? C61 C31 C32 C33 -9.5(6) . . . . ? P1 C31 C32 C33 174.5(3) . . . . ? C61 C31 C32 P2 155.4(3) . . . . ? P1 C31 C32 P2 -20.6(3) . . . . ? C41 P2 C32 C31 16.6(3) . . . . ? C21 P2 C32 C31 131.2(3) . . . . ? C41 P2 C32 C33 -177.0(2) . . . . ? C21 P2 C32 C33 -62.5(3) . . . . ? C31 C32 C33 C333 -148.1(4) . . . . ? P2 C32 C33 C333 47.2(4) . . . . ? C31 C32 C33 C331 -28.4(5) . . . . ? P2 C32 C33 C331 166.9(3) . . . . ? C31 C32 C33 C332 93.1(4) . . . . ? P2 C32 C33 C332 -71.6(3) . . . . ? C51 P1 C41 C42 -80.7(3) . . . . ? C31 P1 C41 C42 166.6(3) . . . . ? C11 P1 C41 C42 50.6(3) . . . . ? C51 P1 C41 P2 110.50(18) . . . . ? C31 P1 C41 P2 -2.14(19) . . . . ? C11 P1 C41 P2 -118.17(17) . . . . ? C21 P2 C41 C42 71.1(4) . . . . ? C32 P2 C41 C42 -172.4(3) . . . . ? C21 P2 C41 P1 -122.83(17) . . . . ? C32 P2 C41 P1 -6.33(18) . . . . ? P1 C41 C42 C43 -177.3(3) . . . . ? P2 C41 C42 C43 -11.8(6) . . . . ? C41 C42 C43 C432 -3.5(6) . . . . ? C41 C42 C43 C433 -126.8(5) . . . . ? C41 C42 C43 C431 117.3(5) . . . . ? C31 P1 C51 C52 141.7(3) . . . . ? C41 P1 C51 C52 33.3(3) . . . . ? C11 P1 C51 C52 -93.4(3) . . . . ? C31 P1 C51 Al1 -37.32(19) . . . . ? C41 P1 C51 Al1 -145.77(15) . . . . ? C11 P1 C51 Al1 87.53(19) . . . . ? P1 C51 C52 C53 179.9(3) . . . . ? Al1 C51 C52 C53 -1.5(6) . . . . ? C51 C52 C53 C531 -95.4(5) . . . . ? C51 C52 C53 C532 145.7(4) . . . . ? C51 C52 C53 C533 26.2(6) . . . . ? Al1 N1 C61 C62 165.2(3) . . . . ? Al1 N1 C61 C31 -25.3(4) . . . . ? C32 C31 C61 C62 -52.6(6) . . . . ? P1 C31 C61 C62 123.5(3) . . . . ? C32 C31 C61 N1 137.3(4) . . . . ? P1 C31 C61 N1 -46.6(3) . . . . ? C61 N1 Al1 C81 -54.6(3) . . . . ? C61 N1 Al1 C71 170.6(3) . . . . ? C61 N1 Al1 C51 55.0(3) . . . . ? C52 C51 Al1 N1 170.2(4) . . . . ? P1 C51 Al1 N1 -11.15(18) . . . . ? C52 C51 Al1 C81 -75.9(4) . . . . ? P1 C51 Al1 C81 102.79(17) . . . . ? C52 C51 Al1 C71 52.4(4) . . . . ? P1 C51 Al1 C71 -128.90(16) . . . . ? N1 Al1 C71 C72 19.4(4) . . . . ? C81 Al1 C71 C72 -111.8(3) . . . . ? C51 Al1 C71 C72 127.2(3) . . . . ? Al1 C71 C72 C721 54.0(4) . . . . ? Al1 C71 C72 C723 -68.2(4) . . . . ? Al1 C71 C72 C722 173.4(3) . . . . ? N1 Al1 C81 C82 -79.8(3) . . . . ? C71 Al1 C81 C82 52.4(3) . . . . ? C51 Al1 C81 C82 175.8(3) . . . . ? Al1 C81 C82 C822 -71.6(4) . . . . ? Al1 C81 C82 C823 168.0(3) . . . . ? Al1 C81 C82 C821 49.6(4) . . . . ? C6 C1 C2 F2 177.6(6) . . . . ? F1 C1 C2 F2 -0.8(11) . . . . ? C6 C1 C2 C3 0.0 . . . . ? F1 C1 C2 C3 -178.3(12) . . . . ? F2 C2 C3 C4 -177.0(8) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C2 C1 C6 C5 0.0 . . . . ? F1 C1 C6 C5 178.2(13) . . . . ? C6A C1A C2A F2A -177.1(11) . . . . ? F1A C1A C2A F2A 2.1(10) . . . . ? C6A C1A C2A C3A 0.0 . . . . ? F1A C1A C2A C3A 179.2(9) . . . . ? F2A C2A C3A C4A 176.0(14) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C2A C1A C6A C5A 0.0 . . . . ? F1A C1A C6A C5A -179.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.888 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.065 data_sad1a _database_code_depnum_ccdc_archive 'CCDC 878408' #TrackingRef '- Compound6cis.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 423 _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Al2 P2' _chemical_formula_weight 712.88 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' 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 '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 17.8586(7) _cell_length_b 10.4392(4) _cell_length_c 24.8146(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.8410(10) _cell_angle_gamma 90.00 _cell_volume 4471.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6709 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.705 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9791 _exptl_absorpt_correction_T_max 0.9951 _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 '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 44425 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.87 _reflns_number_total 10642 _reflns_number_gt 7262 _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^)+(0.0938P)^2^+2.4860P] 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 10642 _refine_ls_number_parameters 480 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _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 0.24334(3) 0.56142(6) 0.09605(2) 0.02654(15) Uani 1 1 d . . . C11 C 0.16544(14) 0.4558(2) 0.10113(10) 0.0311(5) Uani 1 1 d . . . C12 C 0.18256(16) 0.3378(3) 0.12719(12) 0.0396(6) Uani 1 1 d . . . H12 H 0.2353 0.3161 0.1451 0.048 Uiso 1 1 calc R . . C13 C 0.12388(19) 0.2512(3) 0.12741(15) 0.0532(8) Uani 1 1 d . . . H13 H 0.1357 0.1705 0.1462 0.064 Uiso 1 1 calc R . . C14 C 0.0486(2) 0.2813(4) 0.10056(15) 0.0579(9) Uani 1 1 d . . . H14 H 0.0081 0.2206 0.1001 0.070 Uiso 1 1 calc R . . C15 C 0.03086(17) 0.3980(4) 0.07429(14) 0.0527(8) Uani 1 1 d . . . H15 H -0.0219 0.4182 0.0559 0.063 Uiso 1 1 calc R . . C16 C 0.08931(15) 0.4866(3) 0.07440(11) 0.0385(6) Uani 1 1 d . . . H16 H 0.0771 0.5680 0.0562 0.046 Uiso 1 1 calc R . . C41 C 0.28136(14) 0.5001(2) 0.04022(10) 0.0289(5) Uani 1 1 d . . . C42 C 0.23159(14) 0.4631(2) -0.00697(10) 0.0299(5) Uani 1 1 d . . . H42 H 0.1786 0.4618 -0.0050 0.036 Uiso 1 1 calc R . . C43 C 0.24248(16) 0.4228(3) -0.06295(11) 0.0381(6) Uani 1 1 d . . . C431 C 0.31720(19) 0.4705(4) -0.07411(13) 0.0557(9) Uani 1 1 d . . . H43A H 0.3219 0.5611 -0.0673 0.067 Uiso 1 1 calc R . . H43B H 0.3167 0.4535 -0.1122 0.067 Uiso 1 1 calc R . . H43C H 0.3603 0.4273 -0.0499 0.067 Uiso 1 1 calc R . . C432 C 0.1758(2) 0.4756(5) -0.10753(14) 0.0822(14) Uani 1 1 d . . . H43D H 0.1278 0.4468 -0.1010 0.099 Uiso 1 1 calc R . . H43E H 0.1796 0.4462 -0.1434 0.099 Uiso 1 1 calc R . . H43F H 0.1775 0.5675 -0.1066 0.099 Uiso 1 1 calc R . . C433 C 0.2420(3) 0.2756(4) -0.06391(19) 0.0852(14) Uani 1 1 d . . . H43G H 0.2856 0.2439 -0.0359 0.102 Uiso 1 1 calc R . . H43H H 0.2452 0.2461 -0.0999 0.102 Uiso 1 1 calc R . . H43I H 0.1949 0.2448 -0.0566 0.102 Uiso 1 1 calc R . . P2 P 0.38660(4) 0.51657(7) 0.06137(3) 0.03161(17) Uani 1 1 d . . . C21 C 0.41951(15) 0.3483(3) 0.06453(11) 0.0389(6) Uani 1 1 d . . . C22 C 0.47234(18) 0.3134(4) 0.03462(15) 0.0583(9) Uani 1 1 d . . . H22 H 0.4894 0.3753 0.0117 0.070 Uiso 1 1 calc R . . C23 C 0.5006(2) 0.1880(5) 0.03807(19) 0.0803(14) Uani 1 1 d . . . H23 H 0.5367 0.1638 0.0171 0.096 Uiso 1 1 calc R . . C24 C 0.4775(3) 0.1000(4) 0.0708(2) 0.0877(16) Uani 1 1 d . . . H24 H 0.4972 0.0142 0.0726 0.105 Uiso 1 1 calc R . . C25 C 0.4260(3) 0.1331(4) 0.10149(18) 0.0741(11) Uani 1 1 d . . . H25 H 0.4103 0.0707 0.1249 0.089 Uiso 1 1 calc R . . C26 C 0.39676(19) 0.2577(3) 0.09834(14) 0.0518(8) Uani 1 1 d . . . H26 H 0.3608 0.2810 0.1196 0.062 Uiso 1 1 calc R . . C31 C 0.32569(14) 0.5577(2) 0.15420(10) 0.0268(5) Uani 1 1 d . . . C32 C 0.39135(14) 0.5445(2) 0.13640(10) 0.0287(5) Uani 1 1 d . . . C33 C 0.47296(14) 0.5655(3) 0.17478(11) 0.0354(6) Uani 1 1 d D . . C331 C 0.53875(15) 0.5330(3) 0.14788(13) 0.0474(7) Uani 1 1 d D . . H33A H 0.5876 0.5533 0.1733 0.057 Uiso 1 1 calc R . . H33B H 0.5328 0.5820 0.1143 0.057 Uiso 1 1 calc R . . H33C H 0.5372 0.4433 0.1391 0.057 Uiso 1 1 calc R . . C332 C 0.48524(16) 0.4839(3) 0.22732(12) 0.0465(7) Uani 1 1 d D . . H33D H 0.4805 0.3949 0.2172 0.056 Uiso 1 1 calc R . . H33E H 0.4470 0.5056 0.2468 0.056 Uiso 1 1 calc R . . H33F H 0.5360 0.4998 0.2510 0.056 Uiso 1 1 calc R . . C333 C 0.47911(17) 0.7089(3) 0.18918(14) 0.0506(8) Uani 1 1 d D . . H33G H 0.5293 0.7267 0.2133 0.061 Uiso 1 1 calc R . . H33H H 0.4399 0.7315 0.2076 0.061 Uiso 1 1 calc R . . H33I H 0.4720 0.7581 0.1556 0.061 Uiso 1 1 calc R . . Al1 Al 0.17977(5) 0.80497(8) 0.15154(3) 0.0400(2) Uani 1 1 d . . . C71 C 0.07019(19) 0.8617(4) 0.13814(15) 0.0588(9) Uani 1 1 d . . . H71A H 0.0576 0.8596 0.1735 0.071 Uiso 1 1 calc R . . H71B H 0.0685 0.9500 0.1270 0.071 Uiso 1 1 calc R . . C72 C 0.0069(2) 0.7953(5) 0.0977(2) 0.0847(13) Uani 1 1 d . . . H72A H 0.0136 0.8057 0.0608 0.102 Uiso 1 1 calc R . . H72B H -0.0420 0.8313 0.0993 0.102 Uiso 1 1 calc R . . H72C H 0.0078 0.7058 0.1067 0.102 Uiso 1 1 calc R . . C81 C 0.2528(2) 0.9418(3) 0.18931(14) 0.0543(8) Uani 1 1 d . . . H81A H 0.3045 0.9076 0.1993 0.065 Uiso 1 1 calc R . . H81B H 0.2518 1.0106 0.1635 0.065 Uiso 1 1 calc R . . C82 C 0.2341(3) 0.9954(4) 0.24165(15) 0.0716(11) Uani 1 1 d . . . H82A H 0.1811 1.0232 0.2328 0.086 Uiso 1 1 calc R . . H82B H 0.2675 1.0668 0.2553 0.086 Uiso 1 1 calc R . . H82C H 0.2419 0.9300 0.2697 0.086 Uiso 1 1 calc R . . Al2 Al 0.30403(4) 0.57094(7) 0.23132(3) 0.02883(18) Uani 1 1 d . . . C91 C 0.35894(16) 0.6948(3) 0.28896(11) 0.0392(6) Uani 1 1 d . . . H91A H 0.4113 0.6662 0.3035 0.047 Uiso 1 1 calc R . . H91B H 0.3607 0.7765 0.2716 0.047 Uiso 1 1 calc R . . C92 C 0.32103(18) 0.7116(3) 0.33763(12) 0.0489(7) Uani 1 1 d . . . H92A H 0.2692 0.7430 0.3237 0.059 Uiso 1 1 calc R . . H92B H 0.3506 0.7716 0.3640 0.059 Uiso 1 1 calc R . . H92C H 0.3197 0.6305 0.3556 0.059 Uiso 1 1 calc R . . C101 C 0.30308(17) 0.3913(3) 0.25868(12) 0.0402(6) Uani 1 1 d . . . H10A H 0.2505 0.3613 0.2490 0.048 Uiso 1 1 calc R . . H10B H 0.3316 0.3387 0.2392 0.048 Uiso 1 1 calc R . . C102 C 0.3367(2) 0.3713(3) 0.32137(13) 0.0562(9) Uani 1 1 d . . . H10C H 0.3875 0.4082 0.3325 0.067 Uiso 1 1 calc R . . H10D H 0.3398 0.2812 0.3295 0.067 Uiso 1 1 calc R . . H10E H 0.3038 0.4118 0.3414 0.067 Uiso 1 1 calc R . . C51 C 0.20840(14) 0.7231(2) 0.08521(11) 0.0324(5) Uani 1 1 d . . . C52 C 0.21367(17) 0.7692(3) 0.03513(12) 0.0451(7) Uani 1 1 d . A . H52 H 0.2286 0.7058 0.0118 0.054 Uiso 1 1 calc R . . C53 C 0.2010(2) 0.8981(3) 0.00937(13) 0.0542(8) Uani 1 1 d D . . C531 C 0.1922(7) 1.0079(7) 0.0467(3) 0.075(3) Uani 0.540(8) 1 d PDU A -1 H53A H 0.2391 1.0178 0.0756 0.090 Uiso 0.540(8) 1 calc PR A -1 H53B H 0.1500 0.9906 0.0630 0.090 Uiso 0.540(8) 1 calc PR A -1 H53C H 0.1818 1.0853 0.0251 0.090 Uiso 0.540(8) 1 calc PR A -1 C532 C 0.2640(6) 0.9285(8) -0.0200(4) 0.095(4) Uani 0.540(8) 1 d PDU A -1 H53D H 0.2475 0.9015 -0.0582 0.114 Uiso 0.540(8) 1 calc PR A -1 H53E H 0.3107 0.8841 -0.0018 0.114 Uiso 0.540(8) 1 calc PR A -1 H53F H 0.2736 1.0191 -0.0186 0.114 Uiso 0.540(8) 1 calc PR A -1 C533 C 0.1221(6) 0.8850(8) -0.0384(3) 0.085(3) Uani 0.540(8) 1 d PDU A -1 H53G H 0.1157 0.9586 -0.0623 0.102 Uiso 0.540(8) 1 calc PR A -1 H53H H 0.0793 0.8794 -0.0217 0.102 Uiso 0.540(8) 1 calc PR A -1 H53I H 0.1240 0.8091 -0.0598 0.102 Uiso 0.540(8) 1 calc PR A -1 C53A C 0.1781(6) 0.8941(8) -0.0507(3) 0.064(3) Uani 0.460(8) 1 d PDU A -2 H53J H 0.2209 0.8650 -0.0643 0.077 Uiso 0.460(8) 1 calc PR A -2 H53K H 0.1630 0.9783 -0.0650 0.077 Uiso 0.460(8) 1 calc PR A -2 H53L H 0.1353 0.8364 -0.0628 0.077 Uiso 0.460(8) 1 calc PR A -2 C53B C 0.1387(7) 0.9749(10) 0.0313(4) 0.076(3) Uani 0.460(8) 1 d PDU A -2 H53M H 0.1330 1.0592 0.0154 0.092 Uiso 0.460(8) 1 calc PR A -2 H53N H 0.1552 0.9813 0.0712 0.092 Uiso 0.460(8) 1 calc PR A -2 H53O H 0.0899 0.9309 0.0207 0.092 Uiso 0.460(8) 1 calc PR A -2 C53C C 0.2809(6) 0.9663(10) 0.0325(4) 0.091(4) Uani 0.460(8) 1 d PDU A -2 H53P H 0.3207 0.9192 0.0214 0.109 Uiso 0.460(8) 1 calc PR A -2 H53Q H 0.2927 0.9697 0.0725 0.109 Uiso 0.460(8) 1 calc PR A -2 H53R H 0.2784 1.0518 0.0179 0.109 Uiso 0.460(8) 1 calc PR A -2 C61 C 0.18981(15) 0.6493(3) 0.20687(10) 0.0358(6) Uani 1 1 d . . . C62 C 0.14408(15) 0.6091(3) 0.23105(11) 0.0370(6) Uani 1 1 d . . . C63 C 0.08641(17) 0.5614(4) 0.26029(12) 0.0512(8) Uani 1 1 d . . . C631 C 0.0746(4) 0.6633(7) 0.3006(2) 0.139(3) Uani 1 1 d . . . H63A H 0.0395 0.6321 0.3211 0.166 Uiso 1 1 calc R . . H63B H 0.0534 0.7388 0.2802 0.166 Uiso 1 1 calc R . . H63C H 0.1235 0.6836 0.3260 0.166 Uiso 1 1 calc R . . C632 C 0.0102(2) 0.5398(7) 0.21923(19) 0.115(2) Uani 1 1 d . . . H63D H 0.0133 0.4648 0.1975 0.138 Uiso 1 1 calc R . . H63E H -0.0024 0.6127 0.1950 0.138 Uiso 1 1 calc R . . H63F H -0.0292 0.5279 0.2388 0.138 Uiso 1 1 calc R . . C633 C 0.1159(3) 0.4470(7) 0.2934(3) 0.163(4) Uani 1 1 d . . . H63G H 0.1205 0.3779 0.2689 0.196 Uiso 1 1 calc R . . H63H H 0.0807 0.4230 0.3151 0.196 Uiso 1 1 calc R . . H63I H 0.1658 0.4653 0.3178 0.196 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 0.0261(3) 0.0306(3) 0.0250(3) 0.0004(2) 0.0104(2) 0.0015(2) C11 0.0298(12) 0.0380(14) 0.0285(12) -0.0068(10) 0.0132(10) -0.0043(10) C12 0.0370(14) 0.0371(15) 0.0470(16) 0.0009(12) 0.0149(12) -0.0016(12) C13 0.0552(19) 0.0448(17) 0.066(2) -0.0010(15) 0.0266(17) -0.0113(15) C14 0.0514(19) 0.063(2) 0.065(2) -0.0097(17) 0.0261(17) -0.0256(17) C15 0.0279(14) 0.078(2) 0.0517(18) -0.0098(17) 0.0103(13) -0.0090(14) C16 0.0316(13) 0.0523(17) 0.0339(14) -0.0002(12) 0.0123(11) 0.0002(12) C41 0.0323(12) 0.0291(12) 0.0297(12) 0.0019(10) 0.0160(10) 0.0007(10) C42 0.0301(12) 0.0338(13) 0.0294(12) 0.0007(10) 0.0140(10) -0.0004(10) C43 0.0422(15) 0.0445(15) 0.0317(13) -0.0063(11) 0.0172(11) -0.0065(12) C431 0.0499(18) 0.088(3) 0.0349(15) -0.0028(16) 0.0218(14) -0.0108(17) C432 0.057(2) 0.160(4) 0.0286(17) -0.004(2) 0.0086(15) 0.018(3) C433 0.137(4) 0.059(2) 0.081(3) -0.030(2) 0.067(3) -0.028(2) P2 0.0289(3) 0.0382(4) 0.0315(3) -0.0030(3) 0.0148(3) -0.0031(3) C21 0.0308(13) 0.0441(15) 0.0396(14) -0.0122(12) 0.0050(11) 0.0039(12) C22 0.0392(16) 0.077(2) 0.057(2) -0.0270(18) 0.0109(14) 0.0089(16) C23 0.054(2) 0.095(3) 0.083(3) -0.048(3) 0.001(2) 0.031(2) C24 0.083(3) 0.061(3) 0.098(3) -0.034(2) -0.016(3) 0.033(2) C25 0.085(3) 0.044(2) 0.080(3) -0.0045(18) -0.003(2) 0.0164(19) C26 0.0510(18) 0.0424(17) 0.0567(19) -0.0067(14) 0.0038(15) 0.0070(14) C31 0.0282(12) 0.0263(12) 0.0263(11) 0.0000(9) 0.0077(9) -0.0004(9) C32 0.0290(12) 0.0275(12) 0.0308(12) -0.0006(10) 0.0100(10) -0.0004(9) C33 0.0256(12) 0.0440(15) 0.0369(14) -0.0059(11) 0.0090(10) -0.0009(11) C331 0.0267(13) 0.069(2) 0.0484(17) -0.0130(15) 0.0136(12) -0.0041(13) C332 0.0314(14) 0.066(2) 0.0408(16) 0.0054(14) 0.0063(12) 0.0082(13) C333 0.0372(16) 0.0513(18) 0.065(2) -0.0167(15) 0.0156(14) -0.0109(13) Al1 0.0418(5) 0.0426(5) 0.0349(4) -0.0040(4) 0.0085(3) 0.0131(4) C71 0.0510(19) 0.069(2) 0.057(2) 0.0023(17) 0.0152(16) 0.0207(17) C72 0.053(2) 0.102(3) 0.097(3) -0.020(3) 0.016(2) 0.019(2) C81 0.069(2) 0.0432(17) 0.0477(18) 0.0010(14) 0.0088(16) 0.0062(16) C82 0.102(3) 0.054(2) 0.052(2) -0.0128(17) 0.007(2) 0.006(2) Al2 0.0288(4) 0.0337(4) 0.0254(4) 0.0024(3) 0.0095(3) 0.0012(3) C91 0.0345(14) 0.0486(16) 0.0334(14) -0.0039(12) 0.0067(11) 0.0007(12) C92 0.0530(18) 0.0566(19) 0.0380(16) -0.0099(14) 0.0132(14) -0.0010(15) C101 0.0409(15) 0.0387(15) 0.0454(16) 0.0083(12) 0.0193(12) 0.0044(12) C102 0.074(2) 0.0522(19) 0.0498(18) 0.0207(15) 0.0296(17) 0.0197(17) C51 0.0301(13) 0.0334(13) 0.0333(13) 0.0027(10) 0.0073(10) 0.0020(10) C52 0.0463(17) 0.0462(17) 0.0414(16) 0.0041(13) 0.0086(13) -0.0039(13) C53 0.074(2) 0.0466(17) 0.0405(16) 0.0062(14) 0.0114(15) -0.0138(16) C531 0.132(9) 0.038(4) 0.059(5) 0.003(3) 0.034(5) 0.004(5) C532 0.162(10) 0.061(5) 0.086(7) 0.000(4) 0.075(7) -0.028(5) C533 0.110(8) 0.081(6) 0.055(5) 0.010(4) 0.004(5) 0.007(5) C53A 0.077(6) 0.066(5) 0.048(4) 0.019(4) 0.013(4) -0.006(5) C53B 0.121(10) 0.054(6) 0.056(6) 0.011(4) 0.025(6) 0.013(6) C53C 0.106(8) 0.075(6) 0.085(8) 0.019(5) 0.011(6) -0.039(6) C61 0.0314(13) 0.0475(16) 0.0304(13) -0.0081(11) 0.0112(11) 0.0008(11) C62 0.0299(13) 0.0510(16) 0.0295(13) -0.0055(12) 0.0064(10) 0.0058(12) C63 0.0364(15) 0.086(2) 0.0361(15) 0.0001(15) 0.0180(12) -0.0037(15) C631 0.135(5) 0.201(7) 0.119(4) -0.064(5) 0.104(4) -0.043(5) C632 0.055(2) 0.228(7) 0.065(3) -0.001(3) 0.019(2) -0.057(3) C633 0.088(4) 0.209(7) 0.227(8) 0.151(7) 0.102(5) 0.045(4) _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 C31 1.778(2) . ? P1 C51 1.796(3) . ? P1 C11 1.805(3) . ? P1 C41 1.809(2) . ? C11 C12 1.388(4) . ? C11 C16 1.389(4) . ? C12 C13 1.385(4) . ? C12 H12 0.9600 . ? C13 C14 1.375(5) . ? C13 H13 0.9600 . ? C14 C15 1.380(5) . ? C14 H14 0.9600 . ? C15 C16 1.395(4) . ? C15 H15 0.9600 . ? C16 H16 0.9600 . ? C41 C42 1.333(3) . ? C41 P2 1.825(3) . ? C42 C43 1.511(3) . ? C42 H42 0.9600 . ? C43 C432 1.507(5) . ? C43 C431 1.515(4) . ? C43 C433 1.537(5) . ? C431 H43A 0.9599 . ? C431 H43B 0.9599 . ? C431 H43C 0.9599 . ? C432 H43D 0.9599 . ? C432 H43E 0.9599 . ? C432 H43F 0.9599 . ? C433 H43G 0.9599 . ? C433 H43H 0.9599 . ? C433 H43I 0.9599 . ? P2 C21 1.848(3) . ? P2 C32 1.865(3) . ? C21 C22 1.390(4) . ? C21 C26 1.392(4) . ? C22 C23 1.397(6) . ? C22 H22 0.9600 . ? C23 C24 1.359(7) . ? C23 H23 0.9600 . ? C24 C25 1.379(7) . ? C24 H24 0.9600 . ? C25 C26 1.396(5) . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? C31 C32 1.362(3) . ? C31 Al2 2.052(2) . ? C32 C33 1.539(3) . ? C33 C332 1.526(4) . ? C33 C331 1.531(4) . ? C33 C333 1.536(4) . ? C331 H33A 0.9599 . ? C331 H33B 0.9599 . ? C331 H33C 0.9599 . ? C332 H33D 0.9599 . ? C332 H33E 0.9599 . ? C332 H33F 0.9599 . ? C333 H33G 0.9599 . ? C333 H33H 0.9599 . ? C333 H33I 0.9599 . ? Al1 C71 1.989(3) . ? Al1 C81 1.999(3) . ? Al1 C51 2.033(3) . ? Al1 C61 2.105(3) . ? C71 C72 1.479(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C72 H72A 0.9599 . ? C72 H72B 0.9599 . ? C72 H72C 0.9599 . ? C81 C82 1.528(5) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C82 H82A 0.9599 . ? C82 H82B 0.9599 . ? C82 H82C 0.9599 . ? Al2 C91 1.990(3) . ? Al2 C101 1.996(3) . ? Al2 C61 2.137(3) . ? C91 C92 1.538(4) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C92 H92A 0.9599 . ? C92 H92B 0.9599 . ? C92 H92C 0.9599 . ? C101 C102 1.532(4) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C102 H10C 0.9599 . ? C102 H10D 0.9599 . ? C102 H10E 0.9599 . ? C51 C52 1.358(4) . ? C52 C53 1.483(4) . ? C52 H52 0.9600 . ? C53 C53A 1.442(7) . ? C53 C531 1.506(7) . ? C53 C532 1.524(8) . ? C53 C53C 1.567(8) . ? C53 C53B 1.576(9) . ? C53 C533 1.597(8) . ? C531 H53A 0.9599 . ? C531 H53B 0.9599 . ? C531 H53C 0.9599 . ? C532 H53D 0.9599 . ? C532 H53E 0.9599 . ? C532 H53F 0.9599 . ? C533 H53G 0.9599 . ? C533 H53H 0.9599 . ? C533 H53I 0.9599 . ? C53A H53J 0.9599 . ? C53A H53K 0.9599 . ? C53A H53L 0.9599 . ? C53B H53M 0.9599 . ? C53B H53N 0.9599 . ? C53B H53O 0.9599 . ? C53C H53P 0.9599 . ? C53C H53Q 0.9599 . ? C53C H53R 0.9599 . ? C61 C62 1.206(4) . ? C62 C63 1.489(4) . ? C63 C633 1.469(6) . ? C63 C632 1.493(5) . ? C63 C631 1.510(6) . ? C631 H63A 0.9599 . ? C631 H63B 0.9599 . ? C631 H63C 0.9599 . ? C632 H63D 0.9599 . ? C632 H63E 0.9599 . ? C632 H63F 0.9599 . ? C633 H63G 0.9599 . ? C633 H63H 0.9599 . ? C633 H63I 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 C31 P1 C51 109.01(11) . . ? C31 P1 C11 114.97(11) . . ? C51 P1 C11 109.90(12) . . ? C31 P1 C41 102.65(11) . . ? C51 P1 C41 113.72(11) . . ? C11 P1 C41 106.51(11) . . ? C12 C11 C16 120.0(2) . . ? C12 C11 P1 119.5(2) . . ? C16 C11 P1 120.2(2) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 119.2(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C42 C41 P1 118.60(18) . . ? C42 C41 P2 133.28(19) . . ? P1 C41 P2 107.89(13) . . ? C41 C42 C43 132.4(2) . . ? C41 C42 H42 113.8 . . ? C43 C42 H42 113.8 . . ? C432 C43 C42 108.0(2) . . ? C432 C43 C431 108.2(3) . . ? C42 C43 C431 113.8(2) . . ? C432 C43 C433 110.8(3) . . ? C42 C43 C433 106.9(2) . . ? C431 C43 C433 109.1(3) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C41 P2 C21 102.43(12) . . ? C41 P2 C32 94.70(11) . . ? C21 P2 C32 99.99(12) . . ? C22 C21 C26 119.1(3) . . ? C22 C21 P2 118.6(3) . . ? C26 C21 P2 122.2(2) . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C21 C26 C25 120.3(3) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C32 C31 P1 109.94(18) . . ? C32 C31 Al2 133.87(19) . . ? P1 C31 Al2 116.18(12) . . ? C31 C32 C33 122.8(2) . . ? C31 C32 P2 121.13(19) . . ? C33 C32 P2 115.71(17) . . ? C332 C33 C331 106.9(2) . . ? C332 C33 C333 111.1(2) . . ? C331 C33 C333 107.5(2) . . ? C332 C33 C32 110.8(2) . . ? C331 C33 C32 114.2(2) . . ? C333 C33 C32 106.4(2) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C71 Al1 C81 111.20(15) . . ? C71 Al1 C51 115.50(13) . . ? C81 Al1 C51 114.25(13) . . ? C71 Al1 C61 104.75(14) . . ? C81 Al1 C61 108.03(12) . . ? C51 Al1 C61 101.92(10) . . ? C72 C71 Al1 121.5(3) . . ? C72 C71 H71A 107.0 . . ? Al1 C71 H71A 107.0 . . ? C72 C71 H71B 107.0 . . ? Al1 C71 H71B 107.0 . . ? H71A C71 H71B 106.7 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C82 C81 Al1 113.7(3) . . ? C82 C81 H81A 108.8 . . ? Al1 C81 H81A 108.8 . . ? C82 C81 H81B 108.8 . . ? Al1 C81 H81B 108.8 . . ? H81A C81 H81B 107.7 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C91 Al2 C101 114.30(12) . . ? C91 Al2 C31 122.57(11) . . ? C101 Al2 C31 105.89(11) . . ? C91 Al2 C61 102.37(11) . . ? C101 Al2 C61 111.46(12) . . ? C31 Al2 C61 98.93(10) . . ? C92 C91 Al2 113.8(2) . . ? C92 C91 H91A 108.8 . . ? Al2 C91 H91A 108.8 . . ? C92 C91 H91B 108.8 . . ? Al2 C91 H91B 108.8 . . ? H91A C91 H91B 107.7 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C102 C101 Al2 116.0(2) . . ? C102 C101 H10A 108.3 . . ? Al2 C101 H10A 108.3 . . ? C102 C101 H10B 108.3 . . ? Al2 C101 H10B 108.3 . . ? H10A C101 H10B 107.4 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C52 C51 P1 111.5(2) . . ? C52 C51 Al1 133.0(2) . . ? P1 C51 Al1 115.07(13) . . ? C51 C52 C53 132.6(3) . . ? C51 C52 H52 113.7 . . ? C53 C52 H52 113.7 . . ? C53A C53 C52 113.0(4) . . ? C53A C53 C531 127.7(5) . . ? C52 C53 C531 117.0(4) . . ? C53A C53 C532 63.8(5) . . ? C52 C53 C532 110.2(4) . . ? C531 C53 C532 110.0(5) . . ? C53A C53 C53C 112.4(6) . . ? C52 C53 C53C 103.3(4) . . ? C531 C53 C53C 70.0(6) . . ? C532 C53 C53C 50.6(5) . . ? C53A C53 C53B 109.5(6) . . ? C52 C53 C53B 110.9(4) . . ? C531 C53 C53B 37.6(4) . . ? C532 C53 C53B 137.1(6) . . ? C53C C53 C53B 107.5(7) . . ? C53A C53 C533 43.0(4) . . ? C52 C53 C533 104.5(4) . . ? C531 C53 C533 108.1(6) . . ? C532 C53 C533 106.4(6) . . ? C53C C53 C533 149.1(5) . . ? C53B C53 C533 74.6(6) . . ? C53 C531 H53A 109.5 . . ? C53 C531 H53B 109.5 . . ? C53 C531 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? C53 C533 H53G 109.5 . . ? C53 C533 H53H 109.5 . . ? C53 C533 H53I 109.5 . . ? C53 C53A H53J 109.5 . . ? C53 C53A H53K 109.5 . . ? H53J C53A H53K 109.5 . . ? C53 C53A H53L 109.5 . . ? H53J C53A H53L 109.5 . . ? H53K C53A H53L 109.5 . . ? C53 C53B H53M 109.5 . . ? C53 C53B H53N 109.5 . . ? H53M C53B H53N 109.5 . . ? C53 C53B H53O 109.5 . . ? H53M C53B H53O 109.5 . . ? H53N C53B H53O 109.5 . . ? C53 C53C H53P 109.5 . . ? C53 C53C H53Q 109.5 . . ? H53P C53C H53Q 109.5 . . ? C53 C53C H53R 109.5 . . ? H53P C53C H53R 109.5 . . ? H53Q C53C H53R 109.5 . . ? C62 C61 Al1 129.6(2) . . ? C62 C61 Al2 116.4(2) . . ? Al1 C61 Al2 113.36(12) . . ? C61 C62 C63 178.8(3) . . ? C633 C63 C62 110.5(3) . . ? C633 C63 C632 113.1(5) . . ? C62 C63 C632 109.9(3) . . ? C633 C63 C631 107.0(5) . . ? C62 C63 C631 108.6(3) . . ? C632 C63 C631 107.5(4) . . ? C63 C631 H63A 109.5 . . ? C63 C631 H63B 109.5 . . ? H63A C631 H63B 109.5 . . ? C63 C631 H63C 109.5 . . ? H63A C631 H63C 109.5 . . ? H63B C631 H63C 109.5 . . ? C63 C632 H63D 109.5 . . ? C63 C632 H63E 109.5 . . ? H63D C632 H63E 109.5 . . ? C63 C632 H63F 109.5 . . ? H63D C632 H63F 109.5 . . ? H63E C632 H63F 109.5 . . ? C63 C633 H63G 109.5 . . ? C63 C633 H63H 109.5 . . ? H63G C633 H63H 109.5 . . ? C63 C633 H63I 109.5 . . ? H63G C633 H63I 109.5 . . ? H63H C633 H63I 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 C31 P1 C11 C12 -35.3(2) . . . . ? C51 P1 C11 C12 -158.7(2) . . . . ? C41 P1 C11 C12 77.6(2) . . . . ? C31 P1 C11 C16 151.0(2) . . . . ? C51 P1 C11 C16 27.6(2) . . . . ? C41 P1 C11 C16 -96.0(2) . . . . ? C16 C11 C12 C13 -1.0(4) . . . . ? P1 C11 C12 C13 -174.7(2) . . . . ? C11 C12 C13 C14 1.5(5) . . . . ? C12 C13 C14 C15 -1.2(5) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C12 C11 C16 C15 0.1(4) . . . . ? P1 C11 C16 C15 173.8(2) . . . . ? C14 C15 C16 C11 0.2(4) . . . . ? C31 P1 C41 C42 165.3(2) . . . . ? C51 P1 C41 C42 -77.1(2) . . . . ? C11 P1 C41 C42 44.1(2) . . . . ? C31 P1 C41 P2 -19.46(15) . . . . ? C51 P1 C41 P2 98.14(14) . . . . ? C11 P1 C41 P2 -140.65(13) . . . . ? P1 C41 C42 C43 171.9(2) . . . . ? P2 C41 C42 C43 -1.8(5) . . . . ? C41 C42 C43 C432 -142.1(3) . . . . ? C41 C42 C43 C431 -21.9(4) . . . . ? C41 C42 C43 C433 98.7(4) . . . . ? C42 C41 P2 C21 -69.2(3) . . . . ? P1 C41 P2 C21 116.57(13) . . . . ? C42 C41 P2 C32 -170.5(3) . . . . ? P1 C41 P2 C32 15.25(14) . . . . ? C41 P2 C21 C22 126.4(2) . . . . ? C32 P2 C21 C22 -136.5(2) . . . . ? C41 P2 C21 C26 -57.5(3) . . . . ? C32 P2 C21 C26 39.6(3) . . . . ? C26 C21 C22 C23 1.2(5) . . . . ? P2 C21 C22 C23 177.4(3) . . . . ? C21 C22 C23 C24 -0.6(5) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 0.7(6) . . . . ? C22 C21 C26 C25 -0.8(5) . . . . ? P2 C21 C26 C25 -176.9(3) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C51 P1 C31 C32 -105.04(19) . . . . ? C11 P1 C31 C32 131.06(18) . . . . ? C41 P1 C31 C32 15.9(2) . . . . ? C51 P1 C31 Al2 75.76(15) . . . . ? C11 P1 C31 Al2 -48.13(16) . . . . ? C41 P1 C31 Al2 -163.34(12) . . . . ? P1 C31 C32 C33 167.09(19) . . . . ? Al2 C31 C32 C33 -13.9(4) . . . . ? P1 C31 C32 P2 -6.2(3) . . . . ? Al2 C31 C32 P2 172.78(14) . . . . ? C41 P2 C32 C31 -6.2(2) . . . . ? C21 P2 C32 C31 -109.7(2) . . . . ? C41 P2 C32 C33 -179.93(19) . . . . ? C21 P2 C32 C33 76.6(2) . . . . ? C31 C32 C33 C332 53.6(3) . . . . ? P2 C32 C33 C332 -132.8(2) . . . . ? C31 C32 C33 C331 174.3(2) . . . . ? P2 C32 C33 C331 -12.0(3) . . . . ? C31 C32 C33 C333 -67.3(3) . . . . ? P2 C32 C33 C333 106.4(2) . . . . ? C81 Al1 C71 C72 162.6(3) . . . . ? C51 Al1 C71 C72 30.3(4) . . . . ? C61 Al1 C71 C72 -81.0(4) . . . . ? C71 Al1 C81 C82 51.4(3) . . . . ? C51 Al1 C81 C82 -175.6(2) . . . . ? C61 Al1 C81 C82 -63.0(3) . . . . ? C32 C31 Al2 C91 51.2(3) . . . . ? P1 C31 Al2 C91 -129.86(14) . . . . ? C32 C31 Al2 C101 -82.4(3) . . . . ? P1 C31 Al2 C101 96.55(15) . . . . ? C32 C31 Al2 C61 162.1(2) . . . . ? P1 C31 Al2 C61 -18.90(15) . . . . ? C101 Al2 C91 C92 -63.7(2) . . . . ? C31 Al2 C91 C92 166.15(19) . . . . ? C61 Al2 C91 C92 57.0(2) . . . . ? C91 Al2 C101 C102 6.1(3) . . . . ? C31 Al2 C101 C102 144.0(2) . . . . ? C61 Al2 C101 C102 -109.4(2) . . . . ? C31 P1 C51 C52 116.6(2) . . . . ? C11 P1 C51 C52 -116.5(2) . . . . ? C41 P1 C51 C52 2.8(2) . . . . ? C31 P1 C51 Al1 -57.61(16) . . . . ? C11 P1 C51 Al1 69.23(16) . . . . ? C41 P1 C51 Al1 -171.47(12) . . . . ? C71 Al1 C51 C52 67.1(3) . . . . ? C81 Al1 C51 C52 -63.8(3) . . . . ? C61 Al1 C51 C52 -180.0(3) . . . . ? C71 Al1 C51 P1 -120.24(17) . . . . ? C81 Al1 C51 P1 108.89(16) . . . . ? C61 Al1 C51 P1 -7.34(16) . . . . ? P1 C51 C52 C53 -172.4(3) . . . . ? Al1 C51 C52 C53 0.4(5) . . . . ? C51 C52 C53 C53A -153.0(5) . . . . ? C51 C52 C53 C531 11.1(7) . . . . ? C51 C52 C53 C532 137.7(5) . . . . ? C51 C52 C53 C53C 85.2(6) . . . . ? C51 C52 C53 C53B -29.6(7) . . . . ? C51 C52 C53 C533 -108.3(5) . . . . ? C71 Al1 C61 C62 -7.6(3) . . . . ? C81 Al1 C61 C62 111.0(3) . . . . ? C51 Al1 C61 C62 -128.3(3) . . . . ? C71 Al1 C61 Al2 -178.10(14) . . . . ? C81 Al1 C61 Al2 -59.49(16) . . . . ? C51 Al1 C61 Al2 61.19(14) . . . . ? C91 Al2 C61 C62 -93.0(2) . . . . ? C101 Al2 C61 C62 29.6(3) . . . . ? C31 Al2 C61 C62 140.7(2) . . . . ? C91 Al2 C61 Al1 78.85(14) . . . . ? C101 Al2 C61 Al1 -158.55(13) . . . . ? C31 Al2 C61 Al1 -47.47(14) . . . . ? Al1 C61 C62 C63 3(15) . . . . ? Al2 C61 C62 C63 173(100) . . . . ? C61 C62 C63 C633 175(100) . . . . ? C61 C62 C63 C632 49(15) . . . . ? C61 C62 C63 C631 -68(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.965 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.069 data_sad1b _database_code_depnum_ccdc_archive 'CCDC 878409' #TrackingRef '- Compound6trans.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 418 _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Al2 P2' _chemical_formula_weight 712.88 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 17.9208(2) _cell_length_b 10.78390(10) _cell_length_c 24.2169(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.1110(10) _cell_angle_gamma 90.00 _cell_volume 4496.26(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6130 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 71.389 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7422 _exptl_absorpt_correction_T_max 0.7714 _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 25234 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 67.49 _reflns_number_total 7798 _reflns_number_gt 6323 _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^)+(0.1025P)^2^+0.5082P] 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 7798 _refine_ls_number_parameters 500 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.25565(3) 0.55374(5) 0.40490(2) 0.03003(15) Uani 1 1 d . . . C11 C 0.33218(11) 0.4479(2) 0.40077(9) 0.0340(5) Uani 1 1 d . . . C12 C 0.40948(12) 0.4767(2) 0.42679(10) 0.0411(5) Uani 1 1 d . . . H12 H 0.4235 0.5571 0.4434 0.049 Uiso 1 1 calc R . . C13 C 0.46648(13) 0.3879(3) 0.42858(11) 0.0532(7) Uani 1 1 d . . . H13 H 0.5199 0.4070 0.4471 0.064 Uiso 1 1 calc R . . C14 C 0.44715(15) 0.2738(3) 0.40429(12) 0.0567(7) Uani 1 1 d . . . H14 H 0.4870 0.2132 0.4060 0.068 Uiso 1 1 calc R . . C15 C 0.31312(13) 0.3324(2) 0.37563(12) 0.0469(6) Uani 1 1 d . . . H15 H 0.2598 0.3126 0.3570 0.056 Uiso 1 1 calc R . . C16 C 0.37081(15) 0.2454(3) 0.37732(14) 0.0584(7) Uani 1 1 d . . . H16 H 0.3575 0.1656 0.3597 0.070 Uiso 1 1 calc R . . C31 C 0.17262(11) 0.54791(17) 0.34431(9) 0.0300(4) Uani 1 1 d . A . C32 C 0.10690(11) 0.53209(18) 0.36176(9) 0.0313(4) Uani 1 1 d . . . C33 C 0.02469(12) 0.5510(2) 0.32146(10) 0.0378(5) Uani 1 1 d D . . C331 C -0.04035(13) 0.5136(3) 0.34817(12) 0.0533(7) Uani 1 1 d D . . H33A H -0.0356 0.5606 0.3826 0.064 Uiso 1 1 calc R . . H33B H -0.0362 0.4268 0.3572 0.064 Uiso 1 1 calc R . . H33C H -0.0899 0.5301 0.3213 0.064 Uiso 1 1 calc R . . C332 C 0.01259(13) 0.4759(3) 0.26649(11) 0.0533(6) Uani 1 1 d D . . H33D H -0.0398 0.4866 0.2430 0.064 Uiso 1 1 calc R . . H33E H 0.0218 0.3898 0.2759 0.064 Uiso 1 1 calc R . . H33F H 0.0481 0.5040 0.2459 0.064 Uiso 1 1 calc R . . C333 C 0.01677(14) 0.6892(2) 0.30809(14) 0.0580(7) Uani 1 1 d D . . H33G H 0.0577 0.7151 0.2921 0.070 Uiso 1 1 calc R . . H33H H 0.0202 0.7346 0.3428 0.070 Uiso 1 1 calc R . . H33I H -0.0326 0.7050 0.2809 0.070 Uiso 1 1 calc R . . C41 C 0.21837(12) 0.49316(18) 0.46165(9) 0.0324(4) Uani 1 1 d . . . C42 C 0.26909(12) 0.45221(19) 0.50997(10) 0.0365(5) Uani 1 1 d . . . H42 H 0.3224 0.4562 0.5094 0.044 Uiso 1 1 calc R . . C43 C 0.25756(13) 0.4009(2) 0.56518(10) 0.0437(5) Uani 1 1 d . . . C431 C 0.18657(16) 0.4545(3) 0.57977(12) 0.0555(7) Uani 1 1 d . . . H43A H 0.1914 0.5430 0.5829 0.067 Uiso 1 1 calc R . . H43B H 0.1831 0.4206 0.6156 0.067 Uiso 1 1 calc R . . H43C H 0.1406 0.4335 0.5499 0.067 Uiso 1 1 calc R . . C432 C 0.33068(17) 0.4307(3) 0.61394(12) 0.0623(7) Uani 1 1 d . . . H43D H 0.3757 0.4004 0.6040 0.075 Uiso 1 1 calc R . . H43E H 0.3272 0.3914 0.6487 0.075 Uiso 1 1 calc R . . H43F H 0.3349 0.5188 0.6196 0.075 Uiso 1 1 calc R . . C433 C 0.25013(18) 0.2590(2) 0.55835(13) 0.0580(7) Uani 1 1 d . . . H43G H 0.2048 0.2392 0.5277 0.070 Uiso 1 1 calc R . . H43H H 0.2456 0.2229 0.5935 0.070 Uiso 1 1 calc R . . H43I H 0.2954 0.2265 0.5495 0.070 Uiso 1 1 calc R . . C51 C 0.29542(12) 0.7043(2) 0.40797(10) 0.0378(5) Uani 1 1 d . A . C52 C 0.29909(15) 0.8025(2) 0.44253(12) 0.0528(6) Uani 1 1 d . . . H52 H 0.3252 0.8711 0.4308 0.063 Uiso 1 1 calc R . . C53 C 0.27310(15) 0.8339(2) 0.49496(12) 0.0536(6) Uani 1 1 d . . . C531 C 0.18627(17) 0.8067(3) 0.48518(15) 0.0707(9) Uani 1 1 d . . . H53A H 0.1570 0.8474 0.4507 0.085 Uiso 1 1 calc R . . H53B H 0.1700 0.8368 0.5173 0.085 Uiso 1 1 calc R . . H53C H 0.1776 0.7189 0.4814 0.085 Uiso 1 1 calc R . . C532 C 0.3195(2) 0.7595(3) 0.54677(14) 0.0706(8) Uani 1 1 d . . . H53D H 0.3121 0.6725 0.5387 0.085 Uiso 1 1 calc R . . H53E H 0.3019 0.7797 0.5797 0.085 Uiso 1 1 calc R . . H53F H 0.3736 0.7794 0.5545 0.085 Uiso 1 1 calc R . . C533 C 0.2860(2) 0.9720(3) 0.50815(18) 0.0870(11) Uani 1 1 d . . . H53G H 0.3406 0.9899 0.5183 0.104 Uiso 1 1 calc R . . H53H H 0.2656 0.9936 0.5396 0.104 Uiso 1 1 calc R . . H53I H 0.2598 1.0194 0.4749 0.104 Uiso 1 1 calc R . . P2 P 0.11234(3) 0.50264(5) 0.43856(2) 0.03509(16) Uani 1 1 d . . . C21 C 0.08364(12) 0.3377(2) 0.43455(10) 0.0414(5) Uani 1 1 d . . . C22 C 0.10928(14) 0.2518(2) 0.40148(11) 0.0481(6) Uani 1 1 d . . . H22 H 0.1438 0.2773 0.3796 0.058 Uiso 1 1 calc R . . C23 C 0.08540(18) 0.1287(3) 0.39970(14) 0.0638(8) Uani 1 1 d . . . H23 H 0.1037 0.0696 0.3768 0.077 Uiso 1 1 calc R . . C24 C 0.03593(19) 0.0918(3) 0.43058(17) 0.0771(10) Uani 1 1 d . . . H24 H 0.0199 0.0067 0.4295 0.093 Uiso 1 1 calc R . . C25 C 0.00920(16) 0.1756(3) 0.46310(16) 0.0751(10) Uani 1 1 d . . . H25 H -0.0257 0.1491 0.4845 0.090 Uiso 1 1 calc R . . C26 C 0.03259(14) 0.2998(3) 0.46517(13) 0.0565(7) Uani 1 1 d . . . H26 H 0.0134 0.3586 0.4877 0.068 Uiso 1 1 calc R . . Al1 Al 0.33725(5) 0.75514(7) 0.34146(3) 0.0544(2) Uani 1 1 d D . . C71 C 0.45277(19) 0.7695(4) 0.36678(14) 0.0902(13) Uani 1 1 d D A . H71A H 0.4738 0.6874 0.3744 0.108 Uiso 1 1 calc R . . H71B H 0.4693 0.8016 0.3351 0.108 Uiso 1 1 calc R . . C72 C 0.4886(2) 0.8481(5) 0.41829(16) 0.1075(16) Uani 1 1 d D . . H72A H 0.4701 0.9317 0.4111 0.129 Uiso 1 1 calc R A . H72B H 0.5441 0.8471 0.4258 0.129 Uiso 1 1 calc R . . H72C H 0.4747 0.8158 0.4510 0.129 Uiso 1 1 calc R . . C81 C 0.2736(7) 0.9061(9) 0.3095(5) 0.071(3) Uani 0.535(9) 1 d PDU A -1 H81A H 0.2200 0.8819 0.2975 0.085 Uiso 0.535(9) 1 calc PR A -1 H81B H 0.2793 0.9648 0.3402 0.085 Uiso 0.535(9) 1 calc PR A -1 C82 C 0.2926(6) 0.9730(6) 0.2587(3) 0.098(3) Uani 0.535(9) 1 d PDU A -1 H82A H 0.3473 0.9899 0.2683 0.118 Uiso 0.535(9) 1 calc PR A -1 H82B H 0.2643 1.0496 0.2511 0.118 Uiso 0.535(9) 1 calc PR A -1 H82C H 0.2781 0.9212 0.2252 0.118 Uiso 0.535(9) 1 calc PR A -1 C8A C 0.2985(9) 0.9088(11) 0.2988(7) 0.081(4) Uani 0.465(9) 1 d PDU A -2 H8A1 H 0.3398 0.9685 0.3064 0.097 Uiso 0.465(9) 1 calc PR A -2 H8A2 H 0.2840 0.8910 0.2584 0.097 Uiso 0.465(9) 1 calc PR A -2 C8B C 0.2320(5) 0.9633(8) 0.3136(4) 0.093(3) Uani 0.465(9) 1 d PDU A -2 H8B1 H 0.1903 0.9043 0.3061 0.111 Uiso 0.465(9) 1 calc PR A -2 H8B2 H 0.2155 1.0363 0.2908 0.111 Uiso 0.465(9) 1 calc PR A -2 H8B3 H 0.2466 0.9850 0.3536 0.111 Uiso 0.465(9) 1 calc PR A -2 C61 C 0.30888(12) 0.6093(2) 0.28340(10) 0.0406(5) Uani 1 1 d . A . C62 C 0.35708(13) 0.5715(2) 0.26105(10) 0.0409(5) Uani 1 1 d . . . C63 C 0.41464(14) 0.5209(3) 0.23373(11) 0.0534(6) Uani 1 1 d D A . C631 C 0.4761(6) 0.4493(12) 0.2765(5) 0.076(3) Uani 0.598(16) 1 d PDU A -3 H63A H 0.5045 0.5043 0.3061 0.091 Uiso 0.598(16) 1 calc PR A -3 H63B H 0.5110 0.4123 0.2575 0.091 Uiso 0.598(16) 1 calc PR A -3 H63C H 0.4522 0.3855 0.2934 0.091 Uiso 0.598(16) 1 calc PR A -3 C632 C 0.3721(5) 0.4451(10) 0.1818(3) 0.071(2) Uani 0.598(16) 1 d PDU A -3 H63D H 0.3461 0.3769 0.1940 0.086 Uiso 0.598(16) 1 calc PR A -3 H63E H 0.4087 0.4139 0.1628 0.086 Uiso 0.598(16) 1 calc PR A -3 H63F H 0.3346 0.4965 0.1557 0.086 Uiso 0.598(16) 1 calc PR A -3 C633 C 0.4540(5) 0.6325(8) 0.2116(4) 0.080(3) Uani 0.598(16) 1 d PDU A -3 H63G H 0.4147 0.6867 0.1891 0.096 Uiso 0.598(16) 1 calc PR A -3 H63H H 0.4855 0.6020 0.1883 0.096 Uiso 0.598(16) 1 calc PR A -3 H63I H 0.4860 0.6772 0.2438 0.096 Uiso 0.598(16) 1 calc PR A -3 C63A C 0.4153(13) 0.599(2) 0.1835(8) 0.139(9) Uani 0.402(16) 1 d PDU A -4 H63J H 0.3644 0.6001 0.1568 0.167 Uiso 0.402(16) 1 calc PR A -4 H63K H 0.4519 0.5664 0.1650 0.167 Uiso 0.402(16) 1 calc PR A -4 H63L H 0.4300 0.6825 0.1962 0.167 Uiso 0.402(16) 1 calc PR A -4 C63B C 0.3840(7) 0.3857(15) 0.2134(11) 0.113(7) Uani 0.402(16) 1 d PDU A -4 H63M H 0.3893 0.3336 0.2463 0.135 Uiso 0.402(16) 1 calc PR A -4 H63N H 0.4139 0.3519 0.1896 0.135 Uiso 0.402(16) 1 calc PR A -4 H63O H 0.3304 0.3900 0.1918 0.135 Uiso 0.402(16) 1 calc PR A -4 C63C C 0.4916(7) 0.505(2) 0.2763(7) 0.086(6) Uani 0.402(16) 1 d PDU A -4 H63P H 0.5118 0.5849 0.2906 0.103 Uiso 0.402(16) 1 calc PR A -4 H63Q H 0.5266 0.4656 0.2582 0.103 Uiso 0.402(16) 1 calc PR A -4 H63R H 0.4861 0.4548 0.3076 0.103 Uiso 0.402(16) 1 calc PR A -4 Al2 Al 0.19189(3) 0.55715(6) 0.26462(3) 0.03253(17) Uani 1 1 d . . . C91 C 0.18565(14) 0.3852(2) 0.23417(12) 0.0507(6) Uani 1 1 d . A . H91A H 0.2374 0.3524 0.2425 0.061 Uiso 1 1 calc R . . H91B H 0.1575 0.3355 0.2545 0.061 Uiso 1 1 calc R . . C92 C 0.1475(2) 0.3710(3) 0.17037(13) 0.0711(9) Uani 1 1 d . . . H92A H 0.0947 0.3995 0.1615 0.085 Uiso 1 1 calc R A . H92B H 0.1482 0.2853 0.1598 0.085 Uiso 1 1 calc R . . H92C H 0.1754 0.4193 0.1493 0.085 Uiso 1 1 calc R . . C101 C 0.13970(13) 0.6858(2) 0.20833(10) 0.0447(5) Uani 1 1 d . A . H10A H 0.0866 0.6616 0.1918 0.054 Uiso 1 1 calc R . . H10B H 0.1395 0.7624 0.2284 0.054 Uiso 1 1 calc R . . C102 C 0.17758(16) 0.7078(3) 0.15983(12) 0.0588(7) Uani 1 1 d . . . H10C H 0.2303 0.7346 0.1758 0.071 Uiso 1 1 calc R A . H10D H 0.1492 0.7705 0.1344 0.071 Uiso 1 1 calc R . . H10E H 0.1770 0.6322 0.1388 0.071 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 0.0252(3) 0.0298(3) 0.0366(3) -0.00167(19) 0.0110(2) 0.0008(2) C11 0.0285(10) 0.0418(12) 0.0338(12) 0.0024(8) 0.0121(9) 0.0062(9) C12 0.0307(11) 0.0564(14) 0.0355(13) -0.0047(10) 0.0081(9) 0.0038(10) C13 0.0298(11) 0.0789(19) 0.0471(15) -0.0059(13) 0.0044(10) 0.0127(12) C14 0.0443(14) 0.0644(17) 0.0609(17) -0.0045(13) 0.0138(13) 0.0254(12) C15 0.0325(11) 0.0443(13) 0.0647(17) -0.0090(11) 0.0146(11) 0.0023(10) C16 0.0492(14) 0.0461(15) 0.083(2) -0.0118(13) 0.0233(14) 0.0113(12) C31 0.0266(9) 0.0262(10) 0.0377(12) -0.0005(8) 0.0100(9) 0.0001(8) C32 0.0293(10) 0.0279(10) 0.0383(12) -0.0008(8) 0.0119(9) 0.0021(8) C33 0.0257(10) 0.0426(12) 0.0457(13) 0.0051(9) 0.0112(9) 0.0035(9) C331 0.0246(11) 0.0811(19) 0.0545(16) 0.0122(13) 0.0117(11) 0.0036(11) C332 0.0265(11) 0.0770(18) 0.0528(16) -0.0083(13) 0.0049(11) -0.0032(11) C333 0.0372(12) 0.0491(15) 0.086(2) 0.0166(13) 0.0137(13) 0.0135(11) C41 0.0306(10) 0.0299(11) 0.0404(12) -0.0019(8) 0.0157(9) 0.0026(8) C42 0.0323(10) 0.0359(12) 0.0434(13) -0.0024(9) 0.0139(10) 0.0034(9) C43 0.0439(12) 0.0502(14) 0.0381(13) 0.0013(10) 0.0135(10) 0.0095(11) C431 0.0569(16) 0.0729(18) 0.0432(15) 0.0055(12) 0.0246(13) 0.0146(13) C432 0.0572(16) 0.081(2) 0.0446(16) 0.0049(13) 0.0080(13) 0.0066(15) C433 0.0701(18) 0.0514(15) 0.0564(17) 0.0135(12) 0.0242(14) 0.0106(13) C51 0.0321(10) 0.0348(12) 0.0437(13) -0.0032(9) 0.0060(9) -0.0026(9) C52 0.0443(13) 0.0442(14) 0.0645(17) -0.0101(11) 0.0063(12) -0.0029(11) C53 0.0506(14) 0.0484(15) 0.0576(16) -0.0181(11) 0.0079(12) 0.0105(12) C531 0.0540(16) 0.072(2) 0.087(2) -0.0243(17) 0.0214(16) 0.0102(15) C532 0.074(2) 0.072(2) 0.0605(19) -0.0181(14) 0.0102(16) 0.0110(16) C533 0.097(3) 0.0583(19) 0.103(3) -0.0340(18) 0.024(2) -0.0018(18) P2 0.0285(3) 0.0397(3) 0.0402(3) 0.0016(2) 0.0148(2) 0.0049(2) C21 0.0275(10) 0.0459(13) 0.0490(14) 0.0115(10) 0.0077(10) -0.0005(9) C22 0.0436(13) 0.0416(13) 0.0565(16) 0.0056(10) 0.0098(12) -0.0023(10) C23 0.0626(17) 0.0421(15) 0.076(2) 0.0068(13) 0.0014(15) -0.0065(13) C24 0.0595(18) 0.0561(18) 0.099(3) 0.0341(18) -0.0058(18) -0.0190(15) C25 0.0438(15) 0.084(2) 0.093(2) 0.043(2) 0.0117(16) -0.0119(15) C26 0.0365(12) 0.0689(18) 0.0647(18) 0.0243(14) 0.0153(12) -0.0023(12) Al1 0.0646(5) 0.0514(5) 0.0435(4) -0.0008(3) 0.0086(4) -0.0319(4) C71 0.076(2) 0.146(3) 0.0561(19) -0.0233(19) 0.0312(17) -0.073(2) C72 0.076(2) 0.174(4) 0.073(2) -0.031(3) 0.021(2) -0.066(3) C81 0.132(9) 0.039(4) 0.044(5) 0.003(3) 0.029(5) -0.025(5) C82 0.181(9) 0.059(4) 0.059(4) 0.012(3) 0.043(5) -0.011(4) C8A 0.150(10) 0.044(5) 0.053(7) 0.002(4) 0.036(6) -0.029(5) C8B 0.088(6) 0.056(5) 0.110(7) 0.001(5) -0.013(5) 0.007(4) C61 0.0332(11) 0.0488(13) 0.0400(13) 0.0049(9) 0.0106(10) -0.0062(10) C62 0.0332(11) 0.0527(14) 0.0362(13) -0.0034(9) 0.0089(10) -0.0108(10) C63 0.0393(13) 0.0800(19) 0.0437(15) -0.0089(12) 0.0163(11) -0.0022(12) C631 0.054(5) 0.118(8) 0.058(4) -0.001(5) 0.019(4) 0.025(5) C632 0.054(3) 0.113(6) 0.052(4) -0.033(3) 0.022(3) -0.012(4) C633 0.071(5) 0.110(5) 0.077(6) 0.002(4) 0.049(4) -0.023(4) C63A 0.146(16) 0.23(2) 0.076(10) 0.061(12) 0.083(11) 0.081(15) C63B 0.043(5) 0.146(13) 0.156(16) -0.098(12) 0.040(8) -0.012(7) C63C 0.034(4) 0.161(17) 0.064(7) -0.034(9) 0.016(4) -0.005(7) Al2 0.0278(3) 0.0345(3) 0.0365(4) -0.0043(2) 0.0110(3) -0.0028(2) C91 0.0409(12) 0.0448(14) 0.0730(18) -0.0185(12) 0.0267(12) -0.0100(11) C92 0.088(2) 0.0664(19) 0.069(2) -0.0302(15) 0.0386(17) -0.0306(17) C101 0.0372(12) 0.0527(14) 0.0435(14) 0.0049(10) 0.0102(10) -0.0003(10) C102 0.0570(16) 0.0720(19) 0.0495(16) 0.0163(13) 0.0182(13) 0.0045(14) _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 C51 1.767(2) . ? P1 C31 1.778(2) . ? P1 C11 1.808(2) . ? P1 C41 1.809(2) . ? C11 C15 1.387(3) . ? C11 C12 1.389(3) . ? C12 C13 1.392(3) . ? C12 H12 0.9600 . ? C13 C14 1.366(4) . ? C13 H13 0.9600 . ? C14 C16 1.377(4) . ? C14 H14 0.9600 . ? C15 C16 1.389(3) . ? C15 H15 0.9600 . ? C16 H16 0.9600 . ? C31 C32 1.368(3) . ? C31 Al2 2.055(2) . ? C32 C33 1.538(3) . ? C32 P2 1.862(2) . ? C33 C332 1.521(3) . ? C33 C333 1.523(3) . ? C33 C331 1.535(3) . ? C331 H33A 0.9599 . ? C331 H33B 0.9599 . ? C331 H33C 0.9599 . ? C332 H33D 0.9599 . ? C332 H33E 0.9599 . ? C332 H33F 0.9599 . ? C333 H33G 0.9599 . ? C333 H33H 0.9599 . ? C333 H33I 0.9599 . ? C41 C42 1.342(3) . ? C41 P2 1.829(2) . ? C42 C43 1.513(3) . ? C42 H42 0.9600 . ? C43 C431 1.525(3) . ? C43 C432 1.535(4) . ? C43 C433 1.541(4) . ? C431 H43A 0.9599 . ? C431 H43B 0.9599 . ? C431 H43C 0.9599 . ? C432 H43D 0.9599 . ? C432 H43E 0.9599 . ? C432 H43F 0.9599 . ? C433 H43G 0.9599 . ? C433 H43H 0.9599 . ? C433 H43I 0.9599 . ? C51 C52 1.339(3) . ? C51 Al1 2.032(2) . ? C52 C53 1.507(4) . ? C52 H52 0.9600 . ? C53 C532 1.526(4) . ? C53 C533 1.528(4) . ? C53 C531 1.536(4) . ? C531 H53A 0.9599 . ? C531 H53B 0.9599 . ? C531 H53C 0.9599 . ? C532 H53D 0.9599 . ? C532 H53E 0.9599 . ? C532 H53F 0.9599 . ? C533 H53G 0.9599 . ? C533 H53H 0.9599 . ? C533 H53I 0.9599 . ? P2 C21 1.847(2) . ? C21 C22 1.384(3) . ? C21 C26 1.390(3) . ? C22 C23 1.391(4) . ? C22 H22 0.9600 . ? C23 C24 1.368(5) . ? C23 H23 0.9600 . ? C24 C25 1.369(5) . ? C24 H24 0.9600 . ? C25 C26 1.400(5) . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? Al1 C8A 1.973(7) . ? Al1 C71 1.995(3) . ? Al1 C81 2.014(6) . ? Al1 C61 2.076(3) . ? C71 C72 1.497(4) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C72 H72A 0.9599 . ? C72 H72B 0.9599 . ? C72 H72C 0.9599 . ? C81 C82 1.544(8) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C82 H82A 0.9599 . ? C82 H82B 0.9599 . ? C82 H82C 0.9599 . ? C8A C8B 1.458(11) . ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8B H8B1 0.9599 . ? C8B H8B2 0.9599 . ? C8B H8B3 0.9599 . ? C61 C62 1.211(3) . ? C61 Al2 2.095(2) . ? C62 C63 1.476(3) . ? C63 C63C 1.484(12) . ? C63 C63A 1.485(11) . ? C63 C631 1.500(9) . ? C63 C632 1.516(7) . ? C63 C633 1.563(7) . ? C63 C63B 1.587(11) . ? C631 H63A 0.9599 . ? C631 H63B 0.9599 . ? C631 H63C 0.9599 . ? C632 H63D 0.9599 . ? C632 H63E 0.9599 . ? C632 H63F 0.9599 . ? C633 H63G 0.9599 . ? C633 H63H 0.9599 . ? C633 H63I 0.9599 . ? C63A H63J 0.9599 . ? C63A H63K 0.9599 . ? C63A H63L 0.9599 . ? C63B H63M 0.9599 . ? C63B H63N 0.9599 . ? C63B H63O 0.9599 . ? C63C H63P 0.9599 . ? C63C H63Q 0.9599 . ? C63C H63R 0.9599 . ? Al2 C91 1.987(2) . ? Al2 C101 1.987(2) . ? C91 C92 1.514(4) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C92 H92A 0.9599 . ? C92 H92B 0.9599 . ? C92 H92C 0.9599 . ? C101 C102 1.530(3) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C102 H10C 0.9599 . ? C102 H10D 0.9599 . ? C102 H10E 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 C51 P1 C31 107.62(10) . . ? C51 P1 C11 106.22(10) . . ? C31 P1 C11 113.96(10) . . ? C51 P1 C41 121.98(10) . . ? C31 P1 C41 102.32(10) . . ? C11 P1 C41 105.06(9) . . ? C15 C11 C12 119.5(2) . . ? C15 C11 P1 119.54(16) . . ? C12 C11 P1 120.68(17) . . ? C11 C12 C13 119.4(2) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 120.7(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C16 120.3(2) . . ? C13 C14 H14 119.8 . . ? C16 C14 H14 119.8 . . ? C11 C15 C16 120.2(2) . . ? C11 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C14 C16 C15 119.8(2) . . ? C14 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C32 C31 P1 110.16(16) . . ? C32 C31 Al2 132.82(16) . . ? P1 C31 Al2 116.94(10) . . ? C31 C32 C33 122.85(19) . . ? C31 C32 P2 121.25(16) . . ? C33 C32 P2 115.58(14) . . ? C332 C33 C333 110.6(2) . . ? C332 C33 C331 106.8(2) . . ? C333 C33 C331 108.03(19) . . ? C332 C33 C32 111.31(17) . . ? C333 C33 C32 106.31(19) . . ? C331 C33 C32 113.77(19) . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C33 C333 H33G 109.5 . . ? C33 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C33 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C42 C41 P1 118.55(16) . . ? C42 C41 P2 132.85(16) . . ? P1 C41 P2 108.60(11) . . ? C41 C42 C43 131.7(2) . . ? C41 C42 H42 114.1 . . ? C43 C42 H42 114.1 . . ? C42 C43 C431 113.17(19) . . ? C42 C43 C432 107.9(2) . . ? C431 C43 C432 109.4(2) . . ? C42 C43 C433 107.29(19) . . ? C431 C43 C433 110.4(2) . . ? C432 C43 C433 108.7(2) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C43 C433 H43G 109.5 . . ? C43 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C43 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C52 C51 P1 134.6(2) . . ? C52 C51 Al1 108.50(18) . . ? P1 C51 Al1 116.60(12) . . ? C51 C52 C53 136.9(3) . . ? C51 C52 H52 111.5 . . ? C53 C52 H52 111.5 . . ? C52 C53 C532 110.4(2) . . ? C52 C53 C533 109.3(3) . . ? C532 C53 C533 109.0(3) . . ? C52 C53 C531 111.3(2) . . ? C532 C53 C531 108.9(3) . . ? C533 C53 C531 107.8(2) . . ? C53 C531 H53A 109.5 . . ? C53 C531 H53B 109.5 . . ? H53A C531 H53B 109.5 . . ? C53 C531 H53C 109.5 . . ? H53A C531 H53C 109.5 . . ? H53B C531 H53C 109.5 . . ? C53 C532 H53D 109.5 . . ? C53 C532 H53E 109.5 . . ? H53D C532 H53E 109.5 . . ? C53 C532 H53F 109.5 . . ? H53D C532 H53F 109.5 . . ? H53E C532 H53F 109.5 . . ? C53 C533 H53G 109.5 . . ? C53 C533 H53H 109.5 . . ? H53G C533 H53H 109.5 . . ? C53 C533 H53I 109.5 . . ? H53G C533 H53I 109.5 . . ? H53H C533 H53I 109.5 . . ? C41 P2 C21 102.29(9) . . ? C41 P2 C32 94.42(9) . . ? C21 P2 C32 100.08(10) . . ? C22 C21 C26 119.0(2) . . ? C22 C21 P2 122.88(17) . . ? C26 C21 P2 118.1(2) . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 119.8(3) . . ? C21 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C8A Al1 C71 106.3(5) . . ? C8A Al1 C81 16.5(4) . . ? C71 Al1 C81 118.9(4) . . ? C8A Al1 C51 119.2(4) . . ? C71 Al1 C51 110.91(12) . . ? C81 Al1 C51 103.2(3) . . ? C8A Al1 C61 107.3(6) . . ? C71 Al1 C61 107.77(13) . . ? C81 Al1 C61 110.2(4) . . ? C51 Al1 C61 104.94(9) . . ? C72 C71 Al1 118.0(3) . . ? C72 C71 H71A 107.8 . . ? Al1 C71 H71A 107.8 . . ? C72 C71 H71B 107.8 . . ? Al1 C71 H71B 107.8 . . ? H71A C71 H71B 107.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C82 C81 Al1 117.2(6) . . ? C82 C81 H81A 108.0 . . ? Al1 C81 H81A 108.0 . . ? C82 C81 H81B 108.0 . . ? Al1 C81 H81B 108.0 . . ? H81A C81 H81B 107.2 . . ? C8B C8A Al1 113.8(7) . . ? C8B C8A H8A1 108.8 . . ? Al1 C8A H8A1 108.8 . . ? C8B C8A H8A2 108.8 . . ? Al1 C8A H8A2 108.8 . . ? H8A1 C8A H8A2 107.7 . . ? C8A C8B H8B1 109.5 . . ? C8A C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C8A C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C62 C61 Al1 119.15(18) . . ? C62 C61 Al2 127.42(19) . . ? Al1 C61 Al2 113.12(11) . . ? C61 C62 C63 178.0(3) . . ? C62 C63 C63C 111.2(8) . . ? C62 C63 C63A 108.8(6) . . ? C63C C63 C63A 114.6(9) . . ? C62 C63 C631 110.6(5) . . ? C63C C63 C631 25.7(7) . . ? C63A C63 C631 133.5(8) . . ? C62 C63 C632 108.6(4) . . ? C63C C63 C632 132.1(8) . . ? C63A C63 C632 75.2(10) . . ? C631 C63 C632 113.6(6) . . ? C62 C63 C633 107.9(4) . . ? C63C C63 C633 84.6(7) . . ? C63A C63 C633 34.2(9) . . ? C631 C63 C633 108.6(5) . . ? C632 C63 C633 107.5(4) . . ? C62 C63 C63B 104.8(5) . . ? C63C C63 C63B 106.6(8) . . ? C63A C63 C63B 110.5(9) . . ? C631 C63 C63B 82.3(8) . . ? C632 C63 C63B 36.5(8) . . ? C633 C63 C63B 138.6(8) . . ? C63 C631 H63A 109.5 . . ? C63 C631 H63B 109.5 . . ? C63 C631 H63C 109.5 . . ? C63 C632 H63D 109.5 . . ? C63 C632 H63E 109.5 . . ? C63 C632 H63F 109.5 . . ? C63 C633 H63G 109.5 . . ? C63 C633 H63H 109.5 . . ? C63 C633 H63I 109.5 . . ? C63 C63A H63J 109.5 . . ? C63 C63A H63K 109.5 . . ? C63 C63A H63L 109.5 . . ? C63 C63B H63M 109.5 . . ? C63 C63B H63N 109.5 . . ? C63 C63B H63O 109.5 . . ? C63 C63C H63P 109.5 . . ? C63 C63C H63Q 109.5 . . ? C63 C63C H63R 109.5 . . ? C91 Al2 C101 115.43(12) . . ? C91 Al2 C31 107.25(10) . . ? C101 Al2 C31 120.55(9) . . ? C91 Al2 C61 106.32(10) . . ? C101 Al2 C61 102.33(9) . . ? C31 Al2 C61 103.18(9) . . ? C92 C91 Al2 115.9(2) . . ? C92 C91 H91A 108.3 . . ? Al2 C91 H91A 108.3 . . ? C92 C91 H91B 108.3 . . ? Al2 C91 H91B 108.3 . . ? H91A C91 H91B 107.4 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C102 C101 Al2 114.24(17) . . ? C102 C101 H10A 108.7 . . ? Al2 C101 H10A 108.7 . . ? C102 C101 H10B 108.7 . . ? Al2 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 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 C51 P1 C11 C15 -154.45(19) . . . . ? C31 P1 C11 C15 -36.1(2) . . . . ? C41 P1 C11 C15 75.0(2) . . . . ? C51 P1 C11 C12 31.1(2) . . . . ? C31 P1 C11 C12 149.41(18) . . . . ? C41 P1 C11 C12 -99.41(19) . . . . ? C15 C11 C12 C13 -1.7(3) . . . . ? P1 C11 C12 C13 172.74(18) . . . . ? C11 C12 C13 C14 1.0(4) . . . . ? C12 C13 C14 C16 0.4(4) . . . . ? C12 C11 C15 C16 1.1(4) . . . . ? P1 C11 C15 C16 -173.4(2) . . . . ? C13 C14 C16 C15 -1.0(4) . . . . ? C11 C15 C16 C14 0.3(4) . . . . ? C51 P1 C31 C32 -114.36(16) . . . . ? C11 P1 C31 C32 128.13(15) . . . . ? C41 P1 C31 C32 15.29(16) . . . . ? C51 P1 C31 Al2 68.38(13) . . . . ? C11 P1 C31 Al2 -49.13(14) . . . . ? C41 P1 C31 Al2 -161.96(10) . . . . ? P1 C31 C32 C33 166.57(15) . . . . ? Al2 C31 C32 C33 -16.8(3) . . . . ? P1 C31 C32 P2 -6.7(2) . . . . ? Al2 C31 C32 P2 169.97(11) . . . . ? C31 C32 C33 C332 52.6(3) . . . . ? P2 C32 C33 C332 -133.77(18) . . . . ? C31 C32 C33 C333 -68.0(3) . . . . ? P2 C32 C33 C333 105.67(19) . . . . ? C31 C32 C33 C331 173.3(2) . . . . ? P2 C32 C33 C331 -13.1(2) . . . . ? C51 P1 C41 C42 -78.0(2) . . . . ? C31 P1 C41 C42 161.90(17) . . . . ? C11 P1 C41 C42 42.6(2) . . . . ? C51 P1 C41 P2 101.86(13) . . . . ? C31 P1 C41 P2 -18.25(12) . . . . ? C11 P1 C41 P2 -137.53(11) . . . . ? P1 C41 C42 C43 177.78(19) . . . . ? P2 C41 C42 C43 -2.0(4) . . . . ? C41 C42 C43 C431 -30.5(4) . . . . ? C41 C42 C43 C432 -151.7(2) . . . . ? C41 C42 C43 C433 91.5(3) . . . . ? C31 P1 C51 C52 108.5(3) . . . . ? C11 P1 C51 C52 -129.0(3) . . . . ? C41 P1 C51 C52 -9.0(3) . . . . ? C31 P1 C51 Al1 -64.12(13) . . . . ? C11 P1 C51 Al1 58.30(14) . . . . ? C41 P1 C51 Al1 178.35(10) . . . . ? P1 C51 C52 C53 0.8(5) . . . . ? Al1 C51 C52 C53 173.9(3) . . . . ? C51 C52 C53 C532 68.4(4) . . . . ? C51 C52 C53 C533 -171.8(3) . . . . ? C51 C52 C53 C531 -52.7(4) . . . . ? C42 C41 P2 C21 -64.8(2) . . . . ? P1 C41 P2 C21 115.33(11) . . . . ? C42 C41 P2 C32 -166.2(2) . . . . ? P1 C41 P2 C32 13.99(11) . . . . ? C31 C32 P2 C41 -4.96(18) . . . . ? C33 C32 P2 C41 -178.69(15) . . . . ? C31 C32 P2 C21 -108.29(17) . . . . ? C33 C32 P2 C21 77.98(16) . . . . ? C41 P2 C21 C22 -55.9(2) . . . . ? C32 P2 C21 C22 40.9(2) . . . . ? C41 P2 C21 C26 125.6(2) . . . . ? C32 P2 C21 C26 -137.54(19) . . . . ? C26 C21 C22 C23 -1.1(4) . . . . ? P2 C21 C22 C23 -179.6(2) . . . . ? C21 C22 C23 C24 0.3(4) . . . . ? C22 C23 C24 C25 0.4(5) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C22 C21 C26 C25 1.3(4) . . . . ? P2 C21 C26 C25 179.8(2) . . . . ? C24 C25 C26 C21 -0.6(4) . . . . ? C52 C51 Al1 C8A -49.1(7) . . . . ? P1 C51 Al1 C8A 125.4(7) . . . . ? C52 C51 Al1 C71 74.7(2) . . . . ? P1 C51 Al1 C71 -110.79(17) . . . . ? C52 C51 Al1 C81 -53.7(5) . . . . ? P1 C51 Al1 C81 120.8(5) . . . . ? C52 C51 Al1 C61 -169.18(17) . . . . ? P1 C51 Al1 C61 5.31(15) . . . . ? C8A Al1 C71 C72 78.9(6) . . . . ? C81 Al1 C71 C72 67.3(5) . . . . ? C51 Al1 C71 C72 -52.0(4) . . . . ? C61 Al1 C71 C72 -166.4(3) . . . . ? C8A Al1 C81 C82 12(3) . . . . ? C71 Al1 C81 C82 54.5(11) . . . . ? C51 Al1 C81 C82 177.8(9) . . . . ? C61 Al1 C81 C82 -70.6(10) . . . . ? C71 Al1 C8A C8B -135.7(11) . . . . ? C81 Al1 C8A C8B 6(2) . . . . ? C51 Al1 C8A C8B -9.6(15) . . . . ? C61 Al1 C8A C8B 109.3(12) . . . . ? C8A Al1 C61 C62 96.6(4) . . . . ? C71 Al1 C61 C62 -17.5(3) . . . . ? C81 Al1 C61 C62 113.8(4) . . . . ? C51 Al1 C61 C62 -135.7(2) . . . . ? C8A Al1 C61 Al2 -77.5(4) . . . . ? C71 Al1 C61 Al2 168.47(14) . . . . ? C81 Al1 C61 Al2 -60.3(3) . . . . ? C51 Al1 C61 Al2 50.21(13) . . . . ? Al1 C61 C62 C63 148(7) . . . . ? Al2 C61 C62 C63 -38(7) . . . . ? C61 C62 C63 C63C -104(7) . . . . ? C61 C62 C63 C63A 129(7) . . . . ? C61 C62 C63 C631 -76(7) . . . . ? C61 C62 C63 C632 49(7) . . . . ? C61 C62 C63 C633 165(7) . . . . ? C61 C62 C63 C63B 11(7) . . . . ? C32 C31 Al2 C91 -76.1(2) . . . . ? P1 C31 Al2 C91 100.35(12) . . . . ? C32 C31 Al2 C101 58.7(2) . . . . ? P1 C31 Al2 C101 -124.80(12) . . . . ? C32 C31 Al2 C61 171.8(2) . . . . ? P1 C31 Al2 C61 -11.66(13) . . . . ? C62 C61 Al2 C91 27.2(3) . . . . ? Al1 C61 Al2 C91 -159.30(12) . . . . ? C62 C61 Al2 C101 -94.2(2) . . . . ? Al1 C61 Al2 C101 79.23(13) . . . . ? C62 C61 Al2 C31 139.9(2) . . . . ? Al1 C61 Al2 C31 -46.60(12) . . . . ? C101 Al2 C91 C92 4.6(2) . . . . ? C31 Al2 C91 C92 142.11(18) . . . . ? C61 Al2 C91 C92 -108.04(19) . . . . ? C91 Al2 C101 C102 -66.8(2) . . . . ? C31 Al2 C101 C102 161.81(18) . . . . ? C61 Al2 C101 C102 48.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 67.49 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.776 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.057 data_sade _database_code_depnum_ccdc_archive 'CCDC 878410' #TrackingRef '- Five-membered AlP2C2 ring.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H45 Al P2' _chemical_formula_weight 494.58 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.1692(3) _cell_length_b 16.6042(4) _cell_length_c 30.1940(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6101.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8428 _cell_measurement_theta_min 2.927 _cell_measurement_theta_max 71.944 _exptl_crystal_description block _exptl_crystal_colour pale _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8511 _exptl_absorpt_correction_T_max 0.9213 _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 35045 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 71.97 _reflns_number_total 11468 _reflns_number_gt 9385 _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^)+(0.0714P)^2^+0.4912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(18) _refine_ls_number_reflns 11468 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 P11 P 0.87836(6) 0.50012(4) 0.96112(3) 0.02946(17) Uani 1 1 d . . . C111 C 1.0136(2) 0.52915(19) 0.98033(11) 0.0318(7) Uani 1 1 d . . . C112 C 1.0221(3) 0.5882(2) 1.01266(12) 0.0417(8) Uani 1 1 d . . . H112 H 0.9567 0.6111 1.0253 0.050 Uiso 1 1 calc R . . C113 C 1.1239(3) 0.6145(2) 1.02686(13) 0.0504(9) Uani 1 1 d . . . H113 H 1.1291 0.6549 1.0495 0.060 Uiso 1 1 calc R . . C114 C 1.2192(3) 0.5821(3) 1.00826(14) 0.0534(10) Uani 1 1 d . . . H114 H 1.2901 0.6001 1.0180 0.064 Uiso 1 1 calc R . . C115 C 1.2105(3) 0.5243(2) 0.97601(13) 0.0477(9) Uani 1 1 d . . . H115 H 1.2760 0.5019 0.9633 0.057 Uiso 1 1 calc R . . C116 C 1.1090(3) 0.4978(2) 0.96157(11) 0.0383(7) Uani 1 1 d . . . H116 H 1.1042 0.4579 0.9387 0.046 Uiso 1 1 calc R . . C151 C 0.8916(3) 0.40294(18) 0.93419(11) 0.0362(7) Uani 1 1 d . . . H15A H 0.8215 0.3878 0.9223 0.043 Uiso 1 1 calc R . . H15B H 0.9419 0.4081 0.9098 0.043 Uiso 1 1 calc R . . C152 C 0.9321(3) 0.3359(2) 0.96470(14) 0.0505(10) Uani 1 1 d . . . H15C H 0.9984 0.3528 0.9792 0.061 Uiso 1 1 calc R . . H15D H 0.9465 0.2884 0.9476 0.061 Uiso 1 1 calc R . . H15E H 0.8769 0.3244 0.9865 0.061 Uiso 1 1 calc R . . C131 C 0.8280(2) 0.57367(18) 0.92194(9) 0.0295(6) Uani 1 1 d . . . C132 C 0.8967(3) 0.63349(18) 0.90972(10) 0.0318(7) Uani 1 1 d . . . H132 H 0.9698 0.6298 0.9214 0.038 Uiso 1 1 calc R . . C133 C 0.8753(3) 0.70599(18) 0.88008(11) 0.0357(7) Uani 1 1 d . . . C134 C 0.7954(4) 0.7622(2) 0.90356(14) 0.0553(11) Uani 1 1 d . . . H13A H 0.7279 0.7341 0.9093 0.066 Uiso 1 1 calc R . . H13B H 0.7809 0.8081 0.8851 0.066 Uiso 1 1 calc R . . H13C H 0.8270 0.7798 0.9310 0.066 Uiso 1 1 calc R . . C135 C 0.9861(3) 0.7502(2) 0.87378(14) 0.0544(10) Uani 1 1 d . . . H13D H 1.0132 0.7676 0.9021 0.065 Uiso 1 1 calc R . . H13E H 0.9756 0.7961 0.8550 0.065 Uiso 1 1 calc R . . H13F H 1.0382 0.7143 0.8604 0.065 Uiso 1 1 calc R . . C136 C 0.8311(4) 0.6819(2) 0.83500(13) 0.0572(11) Uani 1 1 d . . . H13G H 0.8837 0.6481 0.8203 0.069 Uiso 1 1 calc R . . H13H H 0.8185 0.7294 0.8175 0.069 Uiso 1 1 calc R . . H13I H 0.7633 0.6532 0.8386 0.069 Uiso 1 1 calc R . . C141 C 0.7802(3) 0.4893(2) 1.00485(11) 0.0366(8) Uani 1 1 d . . . C142 C 0.8246(3) 0.4665(2) 1.04339(11) 0.0409(8) Uani 1 1 d . . . H142 H 0.9033 0.4625 1.0434 0.049 Uiso 1 1 calc R . . C143 C 0.7699(3) 0.4459(3) 1.08690(12) 0.0540(10) Uani 1 1 d . . . C144 C 0.6485(4) 0.4501(5) 1.08564(17) 0.128(3) Uani 1 1 d . . . H14A H 0.6189 0.4259 1.1119 0.153 Uiso 1 1 calc R . . H14B H 0.6220 0.4217 1.0601 0.153 Uiso 1 1 calc R . . H14C H 0.6258 0.5054 1.0841 0.153 Uiso 1 1 calc R . . C145 C 0.8169(5) 0.5012(3) 1.12207(13) 0.0769(14) Uani 1 1 d . . . H14D H 0.7991 0.5561 1.1150 0.092 Uiso 1 1 calc R . . H14E H 0.8953 0.4950 1.1232 0.092 Uiso 1 1 calc R . . H14F H 0.7860 0.4877 1.1504 0.092 Uiso 1 1 calc R . . C146 C 0.8067(6) 0.3594(3) 1.09803(17) 0.104(2) Uani 1 1 d . . . H14G H 0.7765 0.3438 1.1261 0.125 Uiso 1 1 calc R . . H14H H 0.8854 0.3573 1.0994 0.125 Uiso 1 1 calc R . . H14I H 0.7809 0.3233 1.0755 0.125 Uiso 1 1 calc R . . P12 P 0.68139(7) 0.56140(5) 0.90872(3) 0.03366(18) Uani 1 1 d . . . C121 C 0.6849(3) 0.47907(18) 0.86830(10) 0.0316(7) Uani 1 1 d . . . C122 C 0.5917(3) 0.4321(2) 0.86233(11) 0.0362(7) Uani 1 1 d . . . H122 H 0.5287 0.4416 0.8807 0.043 Uiso 1 1 calc R . . C123 C 0.5870(3) 0.3723(2) 0.83080(12) 0.0404(8) Uani 1 1 d . . . H123 H 0.5219 0.3401 0.8279 0.048 Uiso 1 1 calc R . . C124 C 0.6768(3) 0.35860(19) 0.80307(11) 0.0405(8) Uani 1 1 d . . . H124 H 0.6740 0.3172 0.7809 0.049 Uiso 1 1 calc R . . C125 C 0.7693(3) 0.40534(19) 0.80805(12) 0.0374(8) Uani 1 1 d . . . H125 H 0.8318 0.3962 0.7893 0.045 Uiso 1 1 calc R . . C126 C 0.7731(3) 0.46470(19) 0.83948(11) 0.0343(7) Uani 1 1 d . . . H126 H 0.8379 0.4974 0.8419 0.041 Uiso 1 1 calc R . . Al11 Al 0.62438(8) 0.51314(7) 0.98226(3) 0.0424(3) Uani 1 1 d . . . C161 C 0.5655(4) 0.6136(3) 1.00933(16) 0.0722(14) Uani 1 1 d . . . H16A H 0.5106 0.6357 0.9900 0.087 Uiso 1 1 calc R . . H16B H 0.5300 0.6001 1.0367 0.087 Uiso 1 1 calc R . . C162 C 0.6517(5) 0.6783(3) 1.01836(19) 0.0937(19) Uani 1 1 d . . . H16C H 0.7025 0.6592 1.0403 0.112 Uiso 1 1 calc R . . H16D H 0.6163 0.7262 1.0289 0.112 Uiso 1 1 calc R . . H16E H 0.6907 0.6902 0.9915 0.112 Uiso 1 1 calc R . . C171 C 0.5221(3) 0.4203(3) 0.97895(14) 0.0602(12) Uani 1 1 d . . . H17A H 0.4831 0.4171 1.0065 0.072 Uiso 1 1 calc R . . H17B H 0.4690 0.4313 0.9562 0.072 Uiso 1 1 calc R . . C172 C 0.5718(4) 0.3391(3) 0.96975(17) 0.0738(14) Uani 1 1 d . . . H17C H 0.6094 0.3405 0.9418 0.089 Uiso 1 1 calc R . . H17D H 0.5148 0.2992 0.9688 0.089 Uiso 1 1 calc R . . H17E H 0.6231 0.3259 0.9928 0.089 Uiso 1 1 calc R . . P21 P 1.38833(6) 0.56467(5) 0.74420(3) 0.02890(17) Uani 1 1 d . . . C211 C 1.5241(2) 0.60664(18) 0.73498(10) 0.0282(6) Uani 1 1 d . . . C212 C 1.6180(3) 0.5639(2) 0.74570(10) 0.0355(7) Uani 1 1 d . . . H212 H 1.6124 0.5098 0.7566 0.043 Uiso 1 1 calc R . . C213 C 1.7203(3) 0.5998(2) 0.74058(12) 0.0381(8) Uani 1 1 d . . . H213 H 1.7857 0.5703 0.7479 0.046 Uiso 1 1 calc R . . C214 C 1.7284(3) 0.6778(2) 0.72497(11) 0.0388(8) Uani 1 1 d . . . H214 H 1.7993 0.7022 0.7212 0.047 Uiso 1 1 calc R . . C215 C 1.6351(3) 0.7206(2) 0.71489(12) 0.0398(8) Uani 1 1 d . . . H215 H 1.6408 0.7751 0.7045 0.048 Uiso 1 1 calc R . . C216 C 1.5324(3) 0.6851(2) 0.71963(11) 0.0363(7) Uani 1 1 d . . . H216 H 1.4673 0.7149 0.7123 0.044 Uiso 1 1 calc R . . C251 C 1.4008(3) 0.45652(17) 0.75049(11) 0.0352(7) Uani 1 1 d . . . H25A H 1.4532 0.4456 0.7735 0.042 Uiso 1 1 calc R . . H25B H 1.3312 0.4354 0.7599 0.042 Uiso 1 1 calc R . . C252 C 1.4364(3) 0.4121(2) 0.70874(13) 0.0484(9) Uani 1 1 d . . . H25C H 1.3817 0.4190 0.6862 0.058 Uiso 1 1 calc R . . H25D H 1.4448 0.3559 0.7152 0.058 Uiso 1 1 calc R . . H25E H 1.5052 0.4336 0.6986 0.058 Uiso 1 1 calc R . . C231 C 1.3322(2) 0.60539(18) 0.79499(10) 0.0301(7) Uani 1 1 d . . . C232 C 1.3917(3) 0.65662(18) 0.81890(11) 0.0339(7) Uani 1 1 d . . . H232 H 1.4660 0.6635 0.8090 0.041 Uiso 1 1 calc R . . C233 C 1.3607(3) 0.7058(2) 0.85923(12) 0.0388(8) Uani 1 1 d . . . C234 C 1.4637(3) 0.7460(2) 0.87762(13) 0.0503(10) Uani 1 1 d . . . H23A H 1.4972 0.7783 0.8549 0.060 Uiso 1 1 calc R . . H23B H 1.5146 0.7055 0.8872 0.060 Uiso 1 1 calc R . . H23C H 1.4442 0.7796 0.9023 0.060 Uiso 1 1 calc R . . C235 C 1.2792(3) 0.7706(2) 0.84405(14) 0.0494(10) Uani 1 1 d . . . H23D H 1.2154 0.7453 0.8315 0.059 Uiso 1 1 calc R . . H23E H 1.3134 0.8042 0.8222 0.059 Uiso 1 1 calc R . . H23F H 1.2578 0.8029 0.8690 0.059 Uiso 1 1 calc R . . C236 C 1.3095(4) 0.6551(2) 0.89579(12) 0.0514(10) Uani 1 1 d . . . H23G H 1.2945 0.6886 0.9210 0.062 Uiso 1 1 calc R . . H23H H 1.3595 0.6131 0.9042 0.062 Uiso 1 1 calc R . . H23I H 1.2422 0.6317 0.8853 0.062 Uiso 1 1 calc R . . C241 C 1.2924(2) 0.58166(18) 0.70062(11) 0.0312(7) Uani 1 1 d . . . C242 C 1.3340(3) 0.60073(19) 0.66086(11) 0.0370(7) Uani 1 1 d . . . H242 H 1.4124 0.6067 0.6596 0.044 Uiso 1 1 calc R . . C243 C 1.2733(3) 0.6141(2) 0.61727(12) 0.0434(9) Uani 1 1 d . . . C244 C 1.1786(4) 0.5569(4) 0.61122(16) 0.099(2) Uani 1 1 d . . . H24A H 1.1498 0.5623 0.5818 0.118 Uiso 1 1 calc R . . H24B H 1.1221 0.5692 0.6323 0.118 Uiso 1 1 calc R . . H24C H 1.2036 0.5027 0.6157 0.118 Uiso 1 1 calc R . . C245 C 1.3521(4) 0.6028(4) 0.57923(15) 0.095(2) Uani 1 1 d . . . H24D H 1.4141 0.6378 0.5830 0.114 Uiso 1 1 calc R . . H24E H 1.3157 0.6154 0.5519 0.114 Uiso 1 1 calc R . . H24F H 1.3767 0.5479 0.5786 0.114 Uiso 1 1 calc R . . C246 C 1.2322(7) 0.6992(3) 0.61546(19) 0.118(3) Uani 1 1 d . . . H24G H 1.2932 0.7356 0.6174 0.142 Uiso 1 1 calc R . . H24H H 1.1830 0.7086 0.6398 0.142 Uiso 1 1 calc R . . H24I H 1.1940 0.7078 0.5880 0.142 Uiso 1 1 calc R . . P22 P 1.18484(7) 0.57822(5) 0.80213(3) 0.03269(18) Uani 1 1 d . . . Al21 Al 1.13807(7) 0.55720(6) 0.72369(3) 0.0347(2) Uani 1 1 d . . . C271 C 1.0899(3) 0.4446(2) 0.70986(12) 0.0440(8) Uani 1 1 d . . . H27A H 1.1255 0.4272 0.6831 0.053 Uiso 1 1 calc R . . H27B H 1.1135 0.4096 0.7333 0.053 Uiso 1 1 calc R . . C272 C 0.9669(3) 0.4362(3) 0.70419(16) 0.0635(12) Uani 1 1 d . . . H27C H 0.9302 0.4603 0.7290 0.076 Uiso 1 1 calc R . . H27D H 0.9479 0.3802 0.7025 0.076 Uiso 1 1 calc R . . H27E H 0.9446 0.4628 0.6774 0.076 Uiso 1 1 calc R . . C261 C 1.0263(3) 0.6421(2) 0.71498(14) 0.0461(9) Uani 1 1 d . . . H26A H 1.0100 0.6458 0.6839 0.055 Uiso 1 1 calc R . . H26B H 0.9601 0.6261 0.7298 0.055 Uiso 1 1 calc R . . C262 C 1.0590(3) 0.7256(2) 0.73160(14) 0.0535(10) Uani 1 1 d . . . H26C H 1.0820 0.7220 0.7619 0.064 Uiso 1 1 calc R . . H26D H 0.9972 0.7613 0.7294 0.064 Uiso 1 1 calc R . . H26E H 1.1183 0.7460 0.7139 0.064 Uiso 1 1 calc R . . C221 C 1.1909(3) 0.47983(19) 0.82919(10) 0.0334(7) Uani 1 1 d . . . C222 C 1.0966(3) 0.4316(2) 0.82746(11) 0.0418(8) Uani 1 1 d . . . H222 H 1.0346 0.4496 0.8104 0.050 Uiso 1 1 calc R . . C223 C 1.0901(3) 0.3583(2) 0.84976(13) 0.0475(9) Uani 1 1 d . . . H223 H 1.0246 0.3262 0.8481 0.057 Uiso 1 1 calc R . . C224 C 1.1790(4) 0.3323(2) 0.87431(13) 0.0516(10) Uani 1 1 d . . . H224 H 1.1754 0.2818 0.8897 0.062 Uiso 1 1 calc R . . C225 C 1.2724(3) 0.3784(2) 0.87677(13) 0.0472(9) Uani 1 1 d . . . H225 H 1.3339 0.3602 0.8940 0.057 Uiso 1 1 calc R . . C226 C 1.2783(3) 0.4516(2) 0.85428(11) 0.0377(8) Uani 1 1 d . . . H226 H 1.3443 0.4832 0.8562 0.045 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 P11 0.0281(4) 0.0328(4) 0.0274(4) -0.0012(3) -0.0008(3) -0.0022(3) C111 0.0264(16) 0.0373(16) 0.0317(17) 0.0014(14) -0.0021(13) -0.0033(12) C112 0.0382(19) 0.0453(19) 0.041(2) -0.0071(17) -0.0010(15) -0.0049(15) C113 0.050(2) 0.051(2) 0.050(2) -0.0108(18) -0.0082(19) -0.0122(18) C114 0.038(2) 0.070(3) 0.051(2) 0.003(2) -0.0101(17) -0.0182(18) C115 0.0303(19) 0.066(2) 0.047(2) 0.010(2) 0.0053(15) -0.0026(16) C116 0.0361(17) 0.0449(17) 0.0338(17) 0.0015(16) 0.0001(14) -0.0023(15) C151 0.0411(19) 0.0349(16) 0.0326(17) -0.0037(14) -0.0052(15) -0.0005(14) C152 0.062(2) 0.0349(18) 0.055(2) 0.0008(18) -0.012(2) 0.0029(16) C131 0.0305(15) 0.0357(16) 0.0223(14) -0.0050(13) 0.0009(12) 0.0036(13) C132 0.0300(17) 0.0385(16) 0.0270(16) -0.0050(14) 0.0005(13) 0.0026(13) C133 0.0425(18) 0.0316(15) 0.0330(18) -0.0007(14) 0.0032(15) -0.0013(14) C134 0.064(3) 0.041(2) 0.060(3) 0.000(2) 0.011(2) 0.0099(18) C135 0.051(2) 0.053(2) 0.059(3) 0.015(2) 0.006(2) -0.0084(18) C136 0.083(3) 0.052(2) 0.037(2) 0.0067(18) -0.007(2) -0.002(2) C141 0.0341(18) 0.0460(19) 0.0298(17) -0.0020(16) 0.0033(14) -0.0068(14) C142 0.0425(19) 0.0463(18) 0.0338(19) -0.0001(16) 0.0004(16) -0.0097(15) C143 0.060(2) 0.072(3) 0.0298(19) 0.004(2) -0.0012(17) -0.022(2) C144 0.064(3) 0.278(10) 0.042(3) 0.018(4) 0.017(2) -0.038(5) C145 0.109(4) 0.085(3) 0.037(2) -0.008(2) 0.006(3) -0.035(3) C146 0.177(7) 0.076(3) 0.059(3) 0.019(3) 0.027(4) -0.037(4) P12 0.0287(4) 0.0385(4) 0.0337(4) -0.0054(4) -0.0020(3) 0.0026(3) C121 0.0325(16) 0.0343(15) 0.0280(16) 0.0020(13) -0.0082(14) 0.0058(13) C122 0.0308(16) 0.0433(18) 0.0345(17) 0.0031(16) -0.0047(13) 0.0028(14) C123 0.040(2) 0.0384(18) 0.042(2) -0.0012(17) -0.0093(16) -0.0060(14) C124 0.052(2) 0.0355(17) 0.0340(18) -0.0078(15) -0.0070(17) 0.0057(15) C125 0.0392(18) 0.0391(17) 0.0341(19) 0.0002(16) -0.0007(15) 0.0041(14) C126 0.0315(16) 0.0359(16) 0.0356(19) 0.0038(15) -0.0034(14) 0.0000(12) Al11 0.0306(5) 0.0638(7) 0.0327(5) -0.0096(5) 0.0044(4) -0.0049(5) C161 0.066(3) 0.100(4) 0.050(3) -0.026(3) 0.002(2) 0.023(3) C162 0.136(5) 0.066(3) 0.079(4) -0.025(3) 0.043(4) 0.002(3) C171 0.045(2) 0.095(3) 0.041(2) -0.009(2) 0.0102(18) -0.029(2) C172 0.085(3) 0.077(3) 0.060(3) 0.015(3) -0.004(3) -0.031(3) P21 0.0249(4) 0.0322(4) 0.0296(4) 0.0019(3) -0.0001(3) 0.0027(3) C211 0.0261(15) 0.0351(16) 0.0234(15) -0.0003(13) 0.0003(11) 0.0013(12) C212 0.0321(16) 0.0400(16) 0.0344(17) 0.0051(16) -0.0019(14) 0.0010(14) C213 0.0273(17) 0.0469(19) 0.040(2) 0.0024(17) -0.0059(14) 0.0074(13) C214 0.0248(16) 0.059(2) 0.0323(19) -0.0038(18) 0.0001(14) -0.0054(14) C215 0.0409(19) 0.0413(18) 0.037(2) 0.0054(15) 0.0021(16) -0.0021(14) C216 0.0294(16) 0.0412(17) 0.0383(19) 0.0067(16) -0.0019(15) 0.0056(13) C251 0.0359(17) 0.0309(15) 0.0387(19) 0.0046(14) 0.0031(14) 0.0032(12) C252 0.057(2) 0.0400(19) 0.049(2) -0.0022(17) 0.0096(18) 0.0064(16) C231 0.0254(15) 0.0317(15) 0.0333(17) 0.0039(13) 0.0046(13) 0.0019(12) C232 0.0292(17) 0.0347(16) 0.0379(19) 0.0028(14) 0.0013(14) -0.0011(13) C233 0.042(2) 0.0389(17) 0.0355(19) -0.0045(15) 0.0058(15) -0.0068(14) C234 0.055(2) 0.054(2) 0.042(2) -0.0107(19) -0.0040(18) -0.0107(18) C235 0.043(2) 0.049(2) 0.056(3) -0.013(2) 0.0054(18) 0.0033(16) C236 0.065(3) 0.052(2) 0.037(2) -0.0081(17) 0.0074(19) -0.007(2) C241 0.0232(15) 0.0337(15) 0.0366(17) 0.0029(14) -0.0007(13) 0.0025(11) C242 0.0308(17) 0.0429(18) 0.0373(18) -0.0013(15) -0.0039(14) 0.0011(13) C243 0.045(2) 0.056(2) 0.0296(19) 0.0016(18) -0.0078(15) 0.0017(16) C244 0.077(3) 0.166(6) 0.052(3) 0.027(3) -0.026(3) -0.044(4) C245 0.077(4) 0.162(6) 0.046(3) -0.014(3) -0.010(2) 0.012(4) C246 0.205(8) 0.075(4) 0.075(4) 0.003(3) -0.071(5) 0.034(4) P22 0.0252(4) 0.0361(4) 0.0367(4) 0.0001(4) 0.0021(3) 0.0016(3) Al21 0.0265(4) 0.0387(5) 0.0388(5) 0.0019(5) -0.0027(4) -0.0014(4) C271 0.050(2) 0.0432(19) 0.039(2) -0.0041(17) -0.0024(16) -0.0028(16) C272 0.056(2) 0.055(2) 0.080(3) -0.006(2) 0.006(2) -0.018(2) C261 0.0306(18) 0.047(2) 0.061(3) 0.0081(19) -0.0063(17) 0.0066(14) C262 0.056(2) 0.050(2) 0.055(3) 0.005(2) -0.008(2) 0.0108(17) C221 0.0314(16) 0.0378(16) 0.0311(16) -0.0057(14) 0.0076(14) 0.0019(13) C222 0.0411(19) 0.0491(19) 0.0351(18) -0.0063(17) 0.0035(15) -0.0071(16) C223 0.056(2) 0.045(2) 0.042(2) -0.0097(18) 0.0177(18) -0.0132(17) C224 0.072(3) 0.0332(17) 0.050(2) 0.0031(17) 0.018(2) 0.0016(18) C225 0.057(2) 0.045(2) 0.040(2) 0.0026(18) 0.0072(17) 0.0098(17) C226 0.0371(18) 0.0400(18) 0.0360(19) -0.0012(16) 0.0047(15) -0.0004(14) _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 P11 C141 1.789(3) . ? P11 C131 1.807(3) . ? P11 C111 1.810(3) . ? P11 C151 1.814(3) . ? C111 C112 1.388(5) . ? C111 C116 1.393(4) . ? C112 C113 1.381(5) . ? C112 H112 0.9600 . ? C113 C114 1.396(5) . ? C113 H113 0.9600 . ? C114 C115 1.371(5) . ? C114 H114 0.9600 . ? C115 C116 1.383(5) . ? C115 H115 0.9600 . ? C116 H116 0.9600 . ? C151 C152 1.526(5) . ? C151 H15A 0.9600 . ? C151 H15B 0.9600 . ? C152 H15C 0.9599 . ? C152 H15D 0.9599 . ? C152 H15E 0.9599 . ? C131 C132 1.349(4) . ? C131 P12 1.840(3) . ? C132 C133 1.522(4) . ? C132 H132 0.9600 . ? C133 C136 1.517(5) . ? C133 C134 1.522(5) . ? C133 C135 1.547(5) . ? C134 H13A 0.9599 . ? C134 H13B 0.9599 . ? C134 H13C 0.9599 . ? C135 H13D 0.9599 . ? C135 H13E 0.9599 . ? C135 H13F 0.9599 . ? C136 H13G 0.9599 . ? C136 H13H 0.9599 . ? C136 H13I 0.9599 . ? C141 C142 1.338(5) . ? C141 Al11 2.054(3) . ? C142 C143 1.512(5) . ? C142 H142 0.9600 . ? C143 C144 1.480(6) . ? C143 C145 1.516(5) . ? C143 C146 1.541(7) . ? C144 H14A 0.9599 . ? C144 H14B 0.9599 . ? C144 H14C 0.9599 . ? C145 H14D 0.9599 . ? C145 H14E 0.9599 . ? C145 H14F 0.9599 . ? C146 H14G 0.9599 . ? C146 H14H 0.9599 . ? C146 H14I 0.9599 . ? P12 C121 1.833(3) . ? P12 Al11 2.4607(13) . ? C121 C122 1.388(4) . ? C121 C126 1.402(4) . ? C122 C123 1.377(5) . ? C122 H122 0.9600 . ? C123 C124 1.395(5) . ? C123 H123 0.9600 . ? C124 C125 1.376(5) . ? C124 H124 0.9600 . ? C125 C126 1.369(5) . ? C125 H125 0.9600 . ? C126 H126 0.9600 . ? Al11 C171 1.984(4) . ? Al11 C161 1.992(5) . ? C161 C162 1.526(7) . ? C161 H16A 0.9600 . ? C161 H16B 0.9600 . ? C162 H16C 0.9599 . ? C162 H16D 0.9599 . ? C162 H16E 0.9599 . ? C171 C172 1.502(6) . ? C171 H17A 0.9600 . ? C171 H17B 0.9600 . ? C172 H17C 0.9599 . ? C172 H17D 0.9599 . ? C172 H17E 0.9599 . ? P21 C241 1.781(3) . ? P21 C231 1.810(3) . ? P21 C251 1.812(3) . ? P21 C211 1.815(3) . ? C211 C212 1.383(4) . ? C211 C216 1.386(4) . ? C212 C213 1.389(4) . ? C212 H212 0.9600 . ? C213 C214 1.382(5) . ? C213 H213 0.9600 . ? C214 C215 1.373(5) . ? C214 H214 0.9600 . ? C215 C216 1.389(5) . ? C215 H215 0.9600 . ? C216 H216 0.9600 . ? C251 C252 1.523(5) . ? C251 H25A 0.9600 . ? C251 H25B 0.9600 . ? C252 H25C 0.9599 . ? C252 H25D 0.9599 . ? C252 H25E 0.9599 . ? C231 C232 1.330(4) . ? C231 P22 1.862(3) . ? C232 C233 1.513(5) . ? C232 H232 0.9600 . ? C233 C236 1.521(5) . ? C233 C234 1.525(5) . ? C233 C235 1.534(5) . ? C234 H23A 0.9599 . ? C234 H23B 0.9599 . ? C234 H23C 0.9599 . ? C235 H23D 0.9599 . ? C235 H23E 0.9599 . ? C235 H23F 0.9599 . ? C236 H23G 0.9599 . ? C236 H23H 0.9599 . ? C236 H23I 0.9599 . ? C241 C242 1.341(5) . ? C241 Al21 2.044(3) . ? C242 C243 1.526(5) . ? C242 H242 0.9600 . ? C243 C246 1.499(6) . ? C243 C244 1.504(6) . ? C243 C245 1.508(6) . ? C244 H24A 0.9599 . ? C244 H24B 0.9599 . ? C244 H24C 0.9599 . ? C245 H24D 0.9599 . ? C245 H24E 0.9599 . ? C245 H24F 0.9599 . ? C246 H24G 0.9599 . ? C246 H24H 0.9599 . ? C246 H24I 0.9599 . ? P22 C221 1.828(3) . ? P22 Al21 2.4607(13) . ? Al21 C261 1.977(3) . ? Al21 C271 2.003(4) . ? C271 C272 1.513(5) . ? C271 H27A 0.9600 . ? C271 H27B 0.9600 . ? C272 H27C 0.9599 . ? C272 H27D 0.9599 . ? C272 H27E 0.9599 . ? C261 C262 1.526(5) . ? C261 H26A 0.9600 . ? C261 H26B 0.9600 . ? C262 H26C 0.9599 . ? C262 H26D 0.9599 . ? C262 H26E 0.9599 . ? C221 C226 1.387(5) . ? C221 C222 1.401(4) . ? C222 C223 1.394(5) . ? C222 H222 0.9600 . ? C223 C224 1.380(6) . ? C223 H223 0.9600 . ? C224 C225 1.373(6) . ? C224 H224 0.9600 . ? C225 C226 1.394(5) . ? C225 H225 0.9600 . ? C226 H226 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C141 P11 C131 108.94(15) . . ? C141 P11 C111 113.39(15) . . ? C131 P11 C111 109.75(15) . . ? C141 P11 C151 107.52(16) . . ? C131 P11 C151 109.74(14) . . ? C111 P11 C151 107.43(16) . . ? C112 C111 C116 119.2(3) . . ? C112 C111 P11 118.8(3) . . ? C116 C111 P11 121.9(3) . . ? C113 C112 C111 120.5(3) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C112 C113 C114 119.9(3) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C115 C114 C113 119.5(3) . . ? C115 C114 H114 120.3 . . ? C113 C114 H114 120.3 . . ? C114 C115 C116 121.0(3) . . ? C114 C115 H115 119.5 . . ? C116 C115 H115 119.5 . . ? C115 C116 C111 119.9(3) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C152 C151 P11 114.0(2) . . ? C152 C151 H15A 108.8 . . ? P11 C151 H15A 108.8 . . ? C152 C151 H15B 108.8 . . ? P11 C151 H15B 108.8 . . ? H15A C151 H15B 107.6 . . ? C151 C152 H15C 109.5 . . ? C151 C152 H15D 109.5 . . ? H15C C152 H15D 109.5 . . ? C151 C152 H15E 109.5 . . ? H15C C152 H15E 109.5 . . ? H15D C152 H15E 109.5 . . ? C132 C131 P11 117.8(2) . . ? C132 C131 P12 128.5(2) . . ? P11 C131 P12 113.33(17) . . ? C131 C132 C133 129.6(3) . . ? C131 C132 H132 115.2 . . ? C133 C132 H132 115.2 . . ? C136 C133 C132 112.3(3) . . ? C136 C133 C134 110.7(3) . . ? C132 C133 C134 108.7(3) . . ? C136 C133 C135 108.9(3) . . ? C132 C133 C135 107.3(3) . . ? C134 C133 C135 108.8(3) . . ? C133 C134 H13A 109.5 . . ? C133 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C133 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? C133 C135 H13D 109.5 . . ? C133 C135 H13E 109.5 . . ? H13D C135 H13E 109.5 . . ? C133 C135 H13F 109.5 . . ? H13D C135 H13F 109.5 . . ? H13E C135 H13F 109.5 . . ? C133 C136 H13G 109.5 . . ? C133 C136 H13H 109.5 . . ? H13G C136 H13H 109.5 . . ? C133 C136 H13I 109.5 . . ? H13G C136 H13I 109.5 . . ? H13H C136 H13I 109.5 . . ? C142 C141 P11 113.6(3) . . ? C142 C141 Al11 135.7(3) . . ? P11 C141 Al11 110.60(17) . . ? C141 C142 C143 130.0(3) . . ? C141 C142 H142 115.0 . . ? C143 C142 H142 115.0 . . ? C144 C143 C142 114.0(4) . . ? C144 C143 C145 111.5(5) . . ? C142 C143 C145 107.8(3) . . ? C144 C143 C146 109.8(5) . . ? C142 C143 C146 105.8(4) . . ? C145 C143 C146 107.6(4) . . ? C143 C144 H14A 109.5 . . ? C143 C144 H14B 109.5 . . ? H14A C144 H14B 109.5 . . ? C143 C144 H14C 109.5 . . ? H14A C144 H14C 109.5 . . ? H14B C144 H14C 109.5 . . ? C143 C145 H14D 109.5 . . ? C143 C145 H14E 109.5 . . ? H14D C145 H14E 109.5 . . ? C143 C145 H14F 109.5 . . ? H14D C145 H14F 109.5 . . ? H14E C145 H14F 109.5 . . ? C143 C146 H14G 109.5 . . ? C143 C146 H14H 109.5 . . ? H14G C146 H14H 109.5 . . ? C143 C146 H14I 109.5 . . ? H14G C146 H14I 109.5 . . ? H14H C146 H14I 109.5 . . ? C121 P12 C131 101.79(14) . . ? C121 P12 Al11 111.38(11) . . ? C131 P12 Al11 96.52(10) . . ? C122 C121 C126 116.7(3) . . ? C122 C121 P12 119.1(3) . . ? C126 C121 P12 123.9(2) . . ? C123 C122 C121 121.9(3) . . ? C123 C122 H122 119.0 . . ? C121 C122 H122 119.0 . . ? C122 C123 C124 120.0(3) . . ? C122 C123 H123 120.0 . . ? C124 C123 H123 120.0 . . ? C125 C124 C123 118.9(3) . . ? C125 C124 H124 120.5 . . ? C123 C124 H124 120.5 . . ? C126 C125 C124 120.6(3) . . ? C126 C125 H125 119.7 . . ? C124 C125 H125 119.7 . . ? C125 C126 C121 121.8(3) . . ? C125 C126 H126 119.1 . . ? C121 C126 H126 119.1 . . ? C171 Al11 C161 116.5(2) . . ? C171 Al11 C141 116.50(18) . . ? C161 Al11 C141 110.95(17) . . ? C171 Al11 P12 112.61(13) . . ? C161 Al11 P12 101.47(16) . . ? C141 Al11 P12 95.86(10) . . ? C162 C161 Al11 114.5(3) . . ? C162 C161 H16A 108.6 . . ? Al11 C161 H16A 108.6 . . ? C162 C161 H16B 108.6 . . ? Al11 C161 H16B 108.6 . . ? H16A C161 H16B 107.6 . . ? C161 C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C162 H16E 109.5 . . ? H16C C162 H16E 109.5 . . ? H16D C162 H16E 109.5 . . ? C172 C171 Al11 117.0(3) . . ? C172 C171 H17A 108.1 . . ? Al11 C171 H17A 108.1 . . ? C172 C171 H17B 108.1 . . ? Al11 C171 H17B 108.1 . . ? H17A C171 H17B 107.3 . . ? C171 C172 H17C 109.5 . . ? C171 C172 H17D 109.5 . . ? H17C C172 H17D 109.5 . . ? C171 C172 H17E 109.5 . . ? H17C C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C241 P21 C231 108.65(14) . . ? C241 P21 C251 106.82(15) . . ? C231 P21 C251 108.25(15) . . ? C241 P21 C211 114.99(14) . . ? C231 P21 C211 109.26(14) . . ? C251 P21 C211 108.67(15) . . ? C212 C211 C216 120.0(3) . . ? C212 C211 P21 121.3(2) . . ? C216 C211 P21 118.6(2) . . ? C211 C212 C213 119.6(3) . . ? C211 C212 H212 120.2 . . ? C213 C212 H212 120.2 . . ? C214 C213 C212 120.2(3) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C215 C214 C213 120.1(3) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C214 C215 C216 120.1(3) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C211 C216 C215 119.9(3) . . ? C211 C216 H216 120.1 . . ? C215 C216 H216 120.1 . . ? C252 C251 P21 114.6(2) . . ? C252 C251 H25A 108.6 . . ? P21 C251 H25A 108.6 . . ? C252 C251 H25B 108.6 . . ? P21 C251 H25B 108.6 . . ? H25A C251 H25B 107.6 . . ? C251 C252 H25C 109.5 . . ? C251 C252 H25D 109.5 . . ? H25C C252 H25D 109.5 . . ? C251 C252 H25E 109.5 . . ? H25C C252 H25E 109.5 . . ? H25D C252 H25E 109.5 . . ? C232 C231 P21 119.6(2) . . ? C232 C231 P22 128.0(2) . . ? P21 C231 P22 111.78(16) . . ? C231 C232 C233 130.3(3) . . ? C231 C232 H232 114.9 . . ? C233 C232 H232 114.9 . . ? C232 C233 C236 112.8(3) . . ? C232 C233 C234 109.0(3) . . ? C236 C233 C234 108.3(3) . . ? C232 C233 C235 107.4(3) . . ? C236 C233 C235 109.9(3) . . ? C234 C233 C235 109.4(3) . . ? C233 C234 H23A 109.5 . . ? C233 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C233 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? C233 C235 H23D 109.5 . . ? C233 C235 H23E 109.5 . . ? H23D C235 H23E 109.5 . . ? C233 C235 H23F 109.5 . . ? H23D C235 H23F 109.5 . . ? H23E C235 H23F 109.5 . . ? C233 C236 H23G 109.5 . . ? C233 C236 H23H 109.5 . . ? H23G C236 H23H 109.5 . . ? C233 C236 H23I 109.5 . . ? H23G C236 H23I 109.5 . . ? H23H C236 H23I 109.5 . . ? C242 C241 P21 116.9(2) . . ? C242 C241 Al21 134.3(2) . . ? P21 C241 Al21 108.59(16) . . ? C241 C242 C243 128.6(3) . . ? C241 C242 H242 115.7 . . ? C243 C242 H242 115.7 . . ? C246 C243 C244 109.6(5) . . ? C246 C243 C245 107.6(5) . . ? C244 C243 C245 108.4(4) . . ? C246 C243 C242 109.3(3) . . ? C244 C243 C242 112.5(3) . . ? C245 C243 C242 109.3(3) . . ? C243 C244 H24A 109.5 . . ? C243 C244 H24B 109.5 . . ? H24A C244 H24B 109.5 . . ? C243 C244 H24C 109.5 . . ? H24A C244 H24C 109.5 . . ? H24B C244 H24C 109.5 . . ? C243 C245 H24D 109.5 . . ? C243 C245 H24E 109.5 . . ? H24D C245 H24E 109.5 . . ? C243 C245 H24F 109.5 . . ? H24D C245 H24F 109.5 . . ? H24E C245 H24F 109.5 . . ? C243 C246 H24G 109.5 . . ? C243 C246 H24H 109.5 . . ? H24G C246 H24H 109.5 . . ? C243 C246 H24I 109.5 . . ? H24G C246 H24I 109.5 . . ? H24H C246 H24I 109.5 . . ? C221 P22 C231 103.24(14) . . ? C221 P22 Al21 108.23(11) . . ? C231 P22 Al21 98.38(10) . . ? C261 Al21 C271 115.91(15) . . ? C261 Al21 C241 116.44(14) . . ? C271 Al21 C241 112.53(14) . . ? C261 Al21 P22 100.71(13) . . ? C271 Al21 P22 113.62(12) . . ? C241 Al21 P22 95.00(10) . . ? C272 C271 Al21 113.5(3) . . ? C272 C271 H27A 108.9 . . ? Al21 C271 H27A 108.9 . . ? C272 C271 H27B 108.9 . . ? Al21 C271 H27B 108.9 . . ? H27A C271 H27B 107.7 . . ? C271 C272 H27C 109.5 . . ? C271 C272 H27D 109.5 . . ? H27C C272 H27D 109.5 . . ? C271 C272 H27E 109.5 . . ? H27C C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C262 C261 Al21 115.1(2) . . ? C262 C261 H26A 108.5 . . ? Al21 C261 H26A 108.5 . . ? C262 C261 H26B 108.5 . . ? Al21 C261 H26B 108.5 . . ? H26A C261 H26B 107.5 . . ? C261 C262 H26C 109.5 . . ? C261 C262 H26D 109.5 . . ? H26C C262 H26D 109.5 . . ? C261 C262 H26E 109.5 . . ? H26C C262 H26E 109.5 . . ? H26D C262 H26E 109.5 . . ? C226 C221 C222 117.1(3) . . ? C226 C221 P22 125.2(3) . . ? C222 C221 P22 117.4(3) . . ? C223 C222 C221 121.9(3) . . ? C223 C222 H222 119.1 . . ? C221 C222 H222 119.1 . . ? C224 C223 C222 119.2(3) . . ? C224 C223 H223 120.4 . . ? C222 C223 H223 120.4 . . ? C225 C224 C223 120.2(3) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C224 C225 C226 120.2(4) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C221 C226 C225 121.4(3) . . ? C221 C226 H226 119.3 . . ? C225 C226 H226 119.3 . . ? 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 C141 P11 C111 C112 -42.9(3) . . . . ? C131 P11 C111 C112 79.2(3) . . . . ? C151 P11 C111 C112 -161.5(3) . . . . ? C141 P11 C111 C116 141.4(3) . . . . ? C131 P11 C111 C116 -96.5(3) . . . . ? C151 P11 C111 C116 22.8(3) . . . . ? C116 C111 C112 C113 -1.5(5) . . . . ? P11 C111 C112 C113 -177.3(3) . . . . ? C111 C112 C113 C114 0.7(6) . . . . ? C112 C113 C114 C115 0.0(6) . . . . ? C113 C114 C115 C116 0.1(6) . . . . ? C114 C115 C116 C111 -0.9(5) . . . . ? C112 C111 C116 C115 1.5(5) . . . . ? P11 C111 C116 C115 177.2(3) . . . . ? C141 P11 C151 C152 -60.8(3) . . . . ? C131 P11 C151 C152 -179.1(3) . . . . ? C111 P11 C151 C152 61.6(3) . . . . ? C141 P11 C131 C132 130.0(2) . . . . ? C111 P11 C131 C132 5.3(3) . . . . ? C151 P11 C131 C132 -112.6(3) . . . . ? C141 P11 C131 P12 -43.8(2) . . . . ? C111 P11 C131 P12 -168.50(15) . . . . ? C151 P11 C131 P12 73.66(19) . . . . ? P11 C131 C132 C133 -175.6(3) . . . . ? P12 C131 C132 C133 -2.9(5) . . . . ? C131 C132 C133 C136 -55.0(5) . . . . ? C131 C132 C133 C134 67.9(4) . . . . ? C131 C132 C133 C135 -174.6(3) . . . . ? C131 P11 C141 C142 -152.4(3) . . . . ? C111 P11 C141 C142 -29.8(3) . . . . ? C151 P11 C141 C142 88.8(3) . . . . ? C131 P11 C141 Al11 28.9(2) . . . . ? C111 P11 C141 Al11 151.47(15) . . . . ? C151 P11 C141 Al11 -89.92(19) . . . . ? P11 C141 C142 C143 -175.7(3) . . . . ? Al11 C141 C142 C143 2.5(6) . . . . ? C141 C142 C143 C144 1.7(7) . . . . ? C141 C142 C143 C145 -122.6(4) . . . . ? C141 C142 C143 C146 122.5(5) . . . . ? C132 C131 P12 C121 107.1(3) . . . . ? P11 C131 P12 C121 -79.94(17) . . . . ? C132 C131 P12 Al11 -139.4(3) . . . . ? P11 C131 P12 Al11 33.56(15) . . . . ? C131 P12 C121 C122 156.3(2) . . . . ? Al11 P12 C121 C122 54.4(3) . . . . ? C131 P12 C121 C126 -30.1(3) . . . . ? Al11 P12 C121 C126 -132.0(2) . . . . ? C126 C121 C122 C123 2.3(5) . . . . ? P12 C121 C122 C123 176.3(3) . . . . ? C121 C122 C123 C124 -1.4(5) . . . . ? C122 C123 C124 C125 0.4(5) . . . . ? C123 C124 C125 C126 -0.4(5) . . . . ? C124 C125 C126 C121 1.5(5) . . . . ? C122 C121 C126 C125 -2.4(5) . . . . ? P12 C121 C126 C125 -176.1(2) . . . . ? C142 C141 Al11 C171 -67.1(4) . . . . ? P11 C141 Al11 C171 111.2(2) . . . . ? C142 C141 Al11 C161 69.3(4) . . . . ? P11 C141 Al11 C161 -112.4(2) . . . . ? C142 C141 Al11 P12 174.0(4) . . . . ? P11 C141 Al11 P12 -7.73(17) . . . . ? C121 P12 Al11 C171 -30.8(2) . . . . ? C131 P12 Al11 C171 -136.16(18) . . . . ? C121 P12 Al11 C161 -156.05(18) . . . . ? C131 P12 Al11 C161 98.55(18) . . . . ? C121 P12 Al11 C141 91.14(15) . . . . ? C131 P12 Al11 C141 -14.26(14) . . . . ? C171 Al11 C161 C162 170.1(4) . . . . ? C141 Al11 C161 C162 33.6(4) . . . . ? P12 Al11 C161 C162 -67.3(4) . . . . ? C161 Al11 C171 C172 -164.8(3) . . . . ? C141 Al11 C171 C172 -30.7(4) . . . . ? P12 Al11 C171 C172 78.6(4) . . . . ? C241 P21 C211 C212 -138.0(3) . . . . ? C231 P21 C211 C212 99.5(3) . . . . ? C251 P21 C211 C212 -18.4(3) . . . . ? C241 P21 C211 C216 46.3(3) . . . . ? C231 P21 C211 C216 -76.2(3) . . . . ? C251 P21 C211 C216 165.9(3) . . . . ? C216 C211 C212 C213 -0.6(5) . . . . ? P21 C211 C212 C213 -176.3(3) . . . . ? C211 C212 C213 C214 0.2(5) . . . . ? C212 C213 C214 C215 0.7(5) . . . . ? C213 C214 C215 C216 -1.1(5) . . . . ? C212 C211 C216 C215 0.2(5) . . . . ? P21 C211 C216 C215 176.0(3) . . . . ? C214 C215 C216 C211 0.6(5) . . . . ? C241 P21 C251 C252 57.4(3) . . . . ? C231 P21 C251 C252 174.2(3) . . . . ? C211 P21 C251 C252 -67.2(3) . . . . ? C241 P21 C231 C232 -127.2(3) . . . . ? C251 P21 C231 C232 117.1(3) . . . . ? C211 P21 C231 C232 -1.0(3) . . . . ? C241 P21 C231 P22 44.7(2) . . . . ? C251 P21 C231 P22 -70.98(19) . . . . ? C211 P21 C231 P22 170.84(15) . . . . ? P21 C231 C232 C233 172.6(3) . . . . ? P22 C231 C232 C233 2.2(5) . . . . ? C231 C232 C233 C236 52.0(5) . . . . ? C231 C232 C233 C234 172.3(3) . . . . ? C231 C232 C233 C235 -69.2(4) . . . . ? C231 P21 C241 C242 142.3(3) . . . . ? C251 P21 C241 C242 -101.2(3) . . . . ? C211 P21 C241 C242 19.5(3) . . . . ? C231 P21 C241 Al21 -42.41(19) . . . . ? C251 P21 C241 Al21 74.15(18) . . . . ? C211 P21 C241 Al21 -165.19(14) . . . . ? P21 C241 C242 C243 176.5(3) . . . . ? Al21 C241 C242 C243 2.7(6) . . . . ? C241 C242 C243 C246 84.0(5) . . . . ? C241 C242 C243 C244 -38.0(6) . . . . ? C241 C242 C243 C245 -158.5(4) . . . . ? C232 C231 P22 C221 -102.5(3) . . . . ? P21 C231 P22 C221 86.49(18) . . . . ? C232 C231 P22 Al21 146.4(3) . . . . ? P21 C231 P22 Al21 -24.58(15) . . . . ? C242 C241 Al21 C261 -58.1(4) . . . . ? P21 C241 Al21 C261 127.78(18) . . . . ? C242 C241 Al21 C271 79.2(4) . . . . ? P21 C241 Al21 C271 -94.94(18) . . . . ? C242 C241 Al21 P22 -162.6(3) . . . . ? P21 C241 Al21 P22 23.20(15) . . . . ? C221 P22 Al21 C261 135.59(15) . . . . ? C231 P22 Al21 C261 -117.41(15) . . . . ? C221 P22 Al21 C271 10.98(16) . . . . ? C231 P22 Al21 C271 117.97(15) . . . . ? C221 P22 Al21 C241 -106.28(14) . . . . ? C231 P22 Al21 C241 0.71(13) . . . . ? C261 Al21 C271 C272 -12.8(4) . . . . ? C241 Al21 C271 C272 -150.3(3) . . . . ? P22 Al21 C271 C272 103.1(3) . . . . ? C271 Al21 C261 C262 172.0(3) . . . . ? C241 Al21 C261 C262 -52.2(4) . . . . ? P22 Al21 C261 C262 48.9(3) . . . . ? C231 P22 C221 C226 24.1(3) . . . . ? Al21 P22 C221 C226 127.7(3) . . . . ? C231 P22 C221 C222 -161.3(3) . . . . ? Al21 P22 C221 C222 -57.7(3) . . . . ? C226 C221 C222 C223 -0.2(5) . . . . ? P22 C221 C222 C223 -175.2(3) . . . . ? C221 C222 C223 C224 0.1(5) . . . . ? C222 C223 C224 C225 0.2(6) . . . . ? C223 C224 C225 C226 -0.3(6) . . . . ? C222 C221 C226 C225 0.0(5) . . . . ? P22 C221 C226 C225 174.7(3) . . . . ? C224 C225 C226 C221 0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 71.97 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.566 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.053