Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Lan-Chang Liang' 'Wei-Ying Lee' _publ_contact_author_name 'Prof Lan-Chang Liang' _publ_contact_author_address ; Department of Chemistry National Sun Yat-sen University Kaohsiung 80424 TAIWAN ; _publ_contact_author_email LCLIANG@MAIL.NSYSU.EDU.TW _publ_section_title ; Organoaluminum Complexes Incorporating an Amido Phosphine Chelate with a Pendant Amine Arm ; data_H[PNN] _database_code_depnum_ccdc_archive 'CCDC 264438' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H25 N2 P1' _chemical_formula_sum 'C22 H25 N2 P' _chemical_formula_weight 348.41 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2152(2) _cell_length_b 11.5571(3) _cell_length_c 23.8166(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1985.99(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14466 _cell_measurement_theta_min 1.697 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9613 _exptl_absorpt_correction_T_max 1.0049 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9678 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3473 _reflns_number_gt 2651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0903P)^2^+0.1139P] 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 -0.26(18) _refine_ls_number_reflns 3473 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.73254(13) 0.10077(8) 0.12805(4) 0.0371(3) Uani 1 1 d . . . N1 N 1.0076(4) 0.1602(2) 0.04023(13) 0.0386(8) Uani 1 1 d . . . H1 H 0.9207 0.0974 0.0422 0.046 Uiso 1 1 d R . . N2 N 1.1252(6) -0.0466(3) -0.00343(16) 0.0535(10) Uani 1 1 d . . . C1 C 0.8982(5) -0.0171(3) 0.14178(15) 0.0355(9) Uani 1 1 d . . . C2 C 1.0626(6) -0.0012(4) 0.17057(18) 0.0465(11) Uani 1 1 d . . . H2 H 1.0861 0.0746 0.1855 0.056 Uiso 1 1 d R . . C3 C 1.1830(6) -0.0935(4) 0.1799(2) 0.0557(11) Uani 1 1 d . . . H3 H 1.2973 -0.0792 0.1994 0.067 Uiso 1 1 d R . . C4 C 1.1411(7) -0.2019(4) 0.15948(19) 0.0545(12) Uani 1 1 d . . . H4 H 1.2289 -0.2630 0.1657 0.065 Uiso 1 1 d R . . C5 C 0.9794(7) -0.2178(4) 0.1303(2) 0.0559(12) Uani 1 1 d . . . H5 H 0.9472 -0.2934 0.1168 0.067 Uiso 1 1 d R . . C6 C 0.8591(6) -0.1269(3) 0.12135(18) 0.0477(10) Uani 1 1 d . . . H6 H 0.7470 -0.1401 0.1006 0.057 Uiso 1 1 d R . . C7 C 0.6089(5) 0.1135(3) 0.19481(15) 0.0374(9) Uani 1 1 d . . . C8 C 0.6379(5) 0.0413(3) 0.24087(17) 0.0425(10) Uani 1 1 d . . . H8 H 0.7486 -0.0048 0.2418 0.051 Uiso 1 1 d R . . C9 C 0.5277(6) 0.0500(4) 0.28847(17) 0.0525(12) Uani 1 1 d . . . H9 H 0.5370 -0.0052 0.3186 0.063 Uiso 1 1 d R . . C10 C 0.3885(6) 0.1322(4) 0.29145(19) 0.0546(12) Uani 1 1 d . . . H10 H 0.3180 0.1381 0.3256 0.065 Uiso 1 1 d R . . C11 C 0.3583(6) 0.2042(4) 0.2464(2) 0.0553(12) Uani 1 1 d . . . H11 H 0.2636 0.2619 0.2506 0.066 Uiso 1 1 d R . . C12 C 0.4647(6) 0.1942(4) 0.19816(19) 0.0478(11) Uani 1 1 d . . . H12 H 0.4275 0.2361 0.1652 0.057 Uiso 1 1 d R . . C13 C 0.8857(5) 0.2276(3) 0.12858(16) 0.0339(8) Uani 1 1 d . . . C14 C 0.8806(6) 0.3132(3) 0.16987(16) 0.0421(10) Uani 1 1 d . . . H14 H 0.8079 0.3003 0.2031 0.050 Uiso 1 1 d R . . C15 C 0.9861(6) 0.4135(4) 0.16455(17) 0.0461(10) Uani 1 1 d . . . H15 H 0.9688 0.4754 0.1909 0.055 Uiso 1 1 d R . . C16 C 1.0950(5) 0.4293(3) 0.11809(18) 0.0445(10) Uani 1 1 d . . . H16 H 1.1792 0.4935 0.1158 0.053 Uiso 1 1 d R . . C17 C 1.1059(5) 0.3450(3) 0.07686(17) 0.0405(9) Uani 1 1 d . . . H17 H 1.1808 0.3536 0.0439 0.049 Uiso 1 1 d R . . C18 C 1.0026(5) 0.2433(3) 0.08131(16) 0.0340(9) Uani 1 1 d . . . C19 C 1.1383(6) 0.1648(3) -0.00548(18) 0.0449(10) Uani 1 1 d . . . H19A H 1.1139 0.2324 -0.0277 0.054 Uiso 1 1 d R . . H19B H 1.2606 0.1697 0.0101 0.054 Uiso 1 1 d R . . C20 C 1.1206(6) 0.0554(3) -0.03948(18) 0.0468(10) Uani 1 1 d . . . H20A H 0.9977 0.0549 -0.0549 0.056 Uiso 1 1 d R . . H20B H 1.2096 0.0508 -0.0694 0.056 Uiso 1 1 d R . . C21 C 1.3077(8) -0.0667(5) 0.0186(2) 0.0813(17) Uani 1 1 d . . . H21A H 1.3074 -0.1342 0.0421 0.098 Uiso 1 1 d R . . H21B H 1.3454 -0.0007 0.0403 0.098 Uiso 1 1 d R . . H21C H 1.3927 -0.0780 -0.0119 0.098 Uiso 1 1 d R . . C22 C 1.0555(10) -0.1489(4) -0.0314(2) 0.095(2) Uani 1 1 d . . . H22A H 0.9333 -0.1340 -0.0456 0.114 Uiso 1 1 d R . . H22B H 1.0509 -0.2120 -0.0052 0.114 Uiso 1 1 d R . . H22C H 1.1363 -0.1686 -0.0620 0.114 Uiso 1 1 d 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 0.0413(6) 0.0339(5) 0.0360(5) 0.0012(5) -0.0024(4) -0.0033(5) N1 0.0420(18) 0.0306(17) 0.0433(19) -0.0034(15) 0.0105(15) -0.0048(15) N2 0.068(3) 0.037(2) 0.055(2) -0.0034(18) 0.019(2) 0.0035(19) C1 0.039(2) 0.038(2) 0.030(2) 0.0009(16) 0.0030(17) -0.0030(17) C2 0.051(3) 0.039(2) 0.050(3) 0.003(2) -0.007(2) -0.002(2) C3 0.052(2) 0.058(3) 0.058(3) 0.011(3) -0.008(2) 0.001(2) C4 0.057(3) 0.045(3) 0.062(3) 0.010(2) 0.006(2) 0.012(2) C5 0.064(3) 0.031(2) 0.072(3) -0.004(2) 0.009(3) 0.001(2) C6 0.049(2) 0.037(2) 0.057(3) -0.005(2) -0.002(2) -0.0054(19) C7 0.0346(19) 0.035(2) 0.043(2) 0.0000(18) -0.0013(16) -0.0048(19) C8 0.039(2) 0.046(2) 0.043(2) -0.001(2) -0.0007(19) 0.000(2) C9 0.062(3) 0.058(3) 0.038(2) 0.003(2) 0.004(2) -0.012(3) C10 0.049(3) 0.064(3) 0.050(3) -0.013(2) 0.009(2) -0.007(2) C11 0.047(3) 0.046(3) 0.072(3) -0.014(2) 0.009(2) 0.003(2) C12 0.045(2) 0.043(2) 0.056(3) 0.008(2) 0.001(2) 0.003(2) C13 0.037(2) 0.0296(18) 0.035(2) 0.0018(17) -0.0065(18) 0.0018(16) C14 0.048(2) 0.042(2) 0.037(2) 0.002(2) -0.0015(19) 0.000(2) C15 0.053(2) 0.040(2) 0.046(3) -0.007(2) -0.006(2) 0.000(2) C16 0.041(2) 0.031(2) 0.061(3) -0.0002(19) -0.009(2) -0.0060(17) C17 0.041(2) 0.033(2) 0.048(2) 0.0012(18) 0.0020(19) -0.0017(19) C18 0.034(2) 0.0278(19) 0.040(2) 0.0012(17) -0.0008(17) 0.0015(17) C19 0.053(2) 0.034(2) 0.048(2) 0.0029(19) 0.010(2) 0.004(2) C20 0.047(2) 0.048(2) 0.046(3) -0.001(2) 0.012(2) -0.001(2) C21 0.101(4) 0.068(4) 0.074(4) 0.019(3) 0.016(3) 0.031(3) C22 0.140(6) 0.050(3) 0.095(4) -0.026(3) 0.049(4) -0.027(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 C7 1.829(4) . ? P1 C13 1.836(4) . ? P1 C1 1.841(4) . ? N1 C18 1.372(5) . ? N1 C19 1.441(5) . ? N1 H1 0.9603 . ? N2 C21 1.437(7) . ? N2 C22 1.448(6) . ? N2 C20 1.459(5) . ? C1 C2 1.382(6) . ? C1 C6 1.388(5) . ? C2 C3 1.393(6) . ? C2 H2 0.9603 . ? C3 C4 1.378(7) . ? C3 H3 0.9608 . ? C4 C5 1.371(6) . ? C4 H4 0.9601 . ? C5 C6 1.379(6) . ? C5 H5 0.9595 . ? C6 H6 0.9602 . ? C7 C8 1.394(5) . ? C7 C12 1.400(6) . ? C8 C9 1.388(6) . ? C8 H8 0.9603 . ? C9 C10 1.384(6) . ? C9 H9 0.9620 . ? C10 C11 1.375(6) . ? C10 H10 0.9611 . ? C11 C12 1.388(6) . ? C11 H11 0.9600 . ? C12 H12 0.9614 . ? C13 C14 1.396(5) . ? C13 C18 1.418(5) . ? C14 C15 1.393(6) . ? C14 H14 0.9605 . ? C15 C16 1.369(6) . ? C15 H15 0.9606 . ? C16 C17 1.385(5) . ? C16 H16 0.9605 . ? C17 C18 1.397(5) . ? C17 H17 0.9590 . ? C19 C20 1.507(5) . ? C19 H19A 0.9596 . ? C19 H19B 0.9591 . ? C20 H20A 0.9596 . ? C20 H20B 0.9604 . ? C21 H21A 0.9601 . ? C21 H21B 0.9599 . ? C21 H21C 0.9599 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 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 C7 P1 C13 102.90(18) . . ? C7 P1 C1 102.81(17) . . ? C13 P1 C1 101.46(16) . . ? C18 N1 C19 122.0(3) . . ? C18 N1 H1 118.5 . . ? C19 N1 H1 119.5 . . ? C21 N2 C22 110.8(4) . . ? C21 N2 C20 111.6(4) . . ? C22 N2 C20 112.4(4) . . ? C2 C1 C6 118.0(4) . . ? C2 C1 P1 123.2(3) . . ? C6 C1 P1 118.8(3) . . ? C1 C2 C3 120.9(4) . . ? C1 C2 H2 117.1 . . ? C3 C2 H2 121.9 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 122.8 . . ? C3 C4 H4 118.0 . . ? C4 C5 C6 120.8(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 121.0(4) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 117.8(4) . . ? C8 C7 P1 124.2(3) . . ? C12 C7 P1 117.8(3) . . ? C9 C8 C7 120.9(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 118.3 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 117.9 . . ? C8 C9 H9 121.4 . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 122.2 . . ? C9 C10 H10 118.4 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 116.9 . . ? C12 C11 H11 122.6 . . ? C11 C12 C7 120.9(4) . . ? C11 C12 H12 118.8 . . ? C7 C12 H12 119.8 . . ? C14 C13 C18 119.0(3) . . ? C14 C13 P1 123.7(3) . . ? C18 C13 P1 117.0(3) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 119.0 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 117.8 . . ? C16 C17 C18 120.5(4) . . ? C16 C17 H17 122.7 . . ? C18 C17 H17 116.8 . . ? N1 C18 C17 121.5(3) . . ? N1 C18 C13 119.5(3) . . ? C17 C18 C13 119.0(3) . . ? N1 C19 C20 108.6(3) . . ? N1 C19 H19A 109.1 . . ? C20 C19 H19A 111.8 . . ? N1 C19 H19B 108.1 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 109.5 . . ? N2 C20 C19 111.1(3) . . ? N2 C20 H20A 103.9 . . ? C19 C20 H20A 106.8 . . ? N2 C20 H20B 112.1 . . ? C19 C20 H20B 112.8 . . ? H20A C20 H20B 109.5 . . ? N2 C21 H21A 110.0 . . ? N2 C21 H21B 109.1 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.3 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.3 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.340 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.116 data_3373 _database_code_depnum_ccdc_archive 'CCDC 264439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 Al1 N2 P1' _chemical_formula_sum 'C30 H42 Al N2 P' _chemical_formula_weight 488.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.1571(1) _cell_length_b 13.1017(2) _cell_length_c 20.6768(3) _cell_angle_alpha 73.4062(5) _cell_angle_beta 89.8788(6) _cell_angle_gamma 78.4122(6) _cell_volume 2832.70(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 37827 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9042 _exptl_absorpt_correction_T_max 1.0156 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33913 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.11 _reflns_number_total 9981 _reflns_number_gt 7515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1109P)^2^+0.5639P] 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 SHELXL _refine_ls_extinction_coef 0.035(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9981 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.35312(6) 0.27958(5) 0.41634(3) 0.02422(19) Uani 1 1 d . . . P2 P 0.75221(6) 0.70956(5) 0.08322(3) 0.02223(19) Uani 1 1 d . . . Al1 Al 0.29885(7) 0.29496(6) 0.28216(4) 0.0246(2) Uani 1 1 d . . . Al2 Al 0.69965(7) 0.69936(6) 0.21621(4) 0.0248(2) Uani 1 1 d . A . N1 N 0.2425(2) 0.36930(17) 0.17986(11) 0.0305(5) Uani 1 1 d . . . N2 N 0.2321(2) 0.43735(16) 0.28953(10) 0.0269(5) Uani 1 1 d . . . N3 N 0.6684(2) 0.62884(17) 0.31845(11) 0.0310(5) Uani 1 1 d . . . N4 N 0.7001(2) 0.55639(16) 0.21015(10) 0.0257(5) Uani 1 1 d . . . C1 C 0.2225(3) 0.2931(2) 0.14213(14) 0.0394(7) Uani 1 1 d . . . H1A H 0.1969 0.3332 0.0960 0.047 Uiso 1 1 d R . . H1B H 0.1605 0.2550 0.1623 0.047 Uiso 1 1 d R . . H1C H 0.2977 0.2416 0.1434 0.047 Uiso 1 1 d R . . C2 C 0.3268(3) 0.4365(2) 0.14268(14) 0.0379(7) Uani 1 1 d . . . H2A H 0.2963 0.4684 0.0964 0.045 Uiso 1 1 d R . . H2B H 0.4069 0.3918 0.1444 0.045 Uiso 1 1 d R . . H2C H 0.3316 0.4932 0.1629 0.045 Uiso 1 1 d R . . C3 C 0.1249(3) 0.4409(2) 0.18696(14) 0.0347(7) Uani 1 1 d . . . H3A H 0.0934 0.4879 0.1431 0.042 Uiso 1 1 d R . . H3B H 0.0672 0.3968 0.2061 0.042 Uiso 1 1 d R . . C4 C 0.1486(3) 0.5071(2) 0.23292(13) 0.0314(6) Uani 1 1 d . . . H4A H 0.0732 0.5360 0.2499 0.038 Uiso 1 1 d R . . H4B H 0.1854 0.5658 0.2083 0.038 Uiso 1 1 d R . . C5 C 0.2633(2) 0.4876(2) 0.33570(12) 0.0241(6) Uani 1 1 d . . . C6 C 0.2292(3) 0.6016(2) 0.32516(13) 0.0295(6) Uani 1 1 d . . . H6 H 0.1780 0.6466 0.2861 0.035 Uiso 1 1 d R . . C7 C 0.2654(3) 0.6501(2) 0.37125(14) 0.0315(6) Uani 1 1 d . . . H7 H 0.2435 0.7277 0.3624 0.038 Uiso 1 1 d R . . C8 C 0.3356(3) 0.5889(2) 0.42981(13) 0.0305(6) Uani 1 1 d . . . H8 H 0.3632 0.6219 0.4612 0.037 Uiso 1 1 d R . . C9 C 0.3669(2) 0.4772(2) 0.44223(13) 0.0262(6) Uani 1 1 d . . . H9 H 0.4131 0.4341 0.4835 0.031 Uiso 1 1 d R . . C10 C 0.3309(2) 0.42585(19) 0.39696(12) 0.0235(6) Uani 1 1 d . . . C11 C 0.4977(2) 0.2269(2) 0.46750(12) 0.0249(6) Uani 1 1 d . . . C12 C 0.6038(3) 0.2560(2) 0.43858(14) 0.0314(6) Uani 1 1 d . . . H12 H 0.5970 0.3075 0.3945 0.038 Uiso 1 1 d R . . C13 C 0.7179(3) 0.2123(2) 0.47213(15) 0.0344(7) Uani 1 1 d . . . H13 H 0.7896 0.2335 0.4514 0.041 Uiso 1 1 d R . . C14 C 0.7284(3) 0.1383(2) 0.53569(15) 0.0366(7) Uani 1 1 d . . . H14 H 0.8077 0.1066 0.5587 0.044 Uiso 1 1 d R . . C15 C 0.6246(3) 0.1092(2) 0.56589(15) 0.0366(7) Uani 1 1 d . . . H15 H 0.6320 0.0594 0.6106 0.044 Uiso 1 1 d R . . C16 C 0.5108(3) 0.1526(2) 0.53203(13) 0.0299(6) Uani 1 1 d . . . H16 H 0.4389 0.1324 0.5532 0.036 Uiso 1 1 d R . . C17 C 0.2358(2) 0.2455(2) 0.47637(13) 0.0301(6) Uani 1 1 d . . . C18 C 0.1515(3) 0.3234(3) 0.49565(15) 0.0392(7) Uani 1 1 d . . . H18 H 0.1570 0.3985 0.4793 0.047 Uiso 1 1 d R . . C19 C 0.0588(3) 0.2926(3) 0.53701(17) 0.0518(9) Uani 1 1 d . . . H19 H 0.0003 0.3457 0.5508 0.062 Uiso 1 1 d R . . C20 C 0.0516(3) 0.1840(3) 0.56003(18) 0.0606(11) Uani 1 1 d . . . H20 H -0.0121 0.1617 0.5886 0.073 Uiso 1 1 d R . . C21 C 0.1342(3) 0.1059(3) 0.54065(16) 0.0514(9) Uani 1 1 d . . . H21 H 0.1304 0.0303 0.5573 0.062 Uiso 1 1 d R . . C22 C 0.2243(3) 0.1370(2) 0.49859(14) 0.0380(7) Uani 1 1 d . . . H22 H 0.2790 0.0821 0.4843 0.046 Uiso 1 1 d R . . C23 C 0.4771(3) 0.2475(2) 0.27210(13) 0.0291(6) Uani 1 1 d . . . H23A H 0.4920 0.2575 0.2252 0.035 Uiso 1 1 d R . . H23B H 0.5212 0.2907 0.2896 0.035 Uiso 1 1 d R . . C24 C 0.5412(3) 0.1292(2) 0.30794(14) 0.0343(7) Uani 1 1 d . . . H24 H 0.5161 0.1123 0.3535 0.041 Uiso 1 1 d R . . C25 C 0.6800(3) 0.1158(3) 0.31063(18) 0.0516(9) Uani 1 1 d . . . H25A H 0.7161 0.0410 0.3331 0.062 Uiso 1 1 d R . . H25B H 0.7049 0.1614 0.3348 0.062 Uiso 1 1 d R . . H25C H 0.7067 0.1353 0.2654 0.062 Uiso 1 1 d R . . C26 C 0.5043(3) 0.0520(2) 0.27294(16) 0.0429(8) Uani 1 1 d . . . H26A H 0.5458 -0.0211 0.2962 0.052 Uiso 1 1 d R . . H26B H 0.5267 0.0706 0.2268 0.052 Uiso 1 1 d R . . H26C H 0.4173 0.0571 0.2741 0.052 Uiso 1 1 d R . . C27 C 0.1994(2) 0.1799(2) 0.30745(14) 0.0313(6) Uani 1 1 d . . . H27A H 0.2173 0.1327 0.2792 0.038 Uiso 1 1 d R . . H27B H 0.2191 0.1383 0.3539 0.038 Uiso 1 1 d R . . C28 C 0.0583(3) 0.1998(2) 0.30600(17) 0.0419(8) Uani 1 1 d . . . H28 H 0.0300 0.2303 0.2593 0.050 Uiso 1 1 d R . . C29 C 0.0016(3) 0.2789(3) 0.34452(16) 0.0461(8) Uani 1 1 d . . . H29A H -0.0860 0.2885 0.3414 0.055 Uiso 1 1 d R . . H29B H 0.0240 0.3480 0.3261 0.055 Uiso 1 1 d R . . H29C H 0.0310 0.2490 0.3911 0.055 Uiso 1 1 d R . . C30 C 0.0170(3) 0.0923(3) 0.3343(3) 0.0790(14) Uani 1 1 d . . . H30A H -0.0708 0.1052 0.3327 0.095 Uiso 1 1 d R . . H30B H 0.0489 0.0594 0.3803 0.095 Uiso 1 1 d R . . H30C H 0.0476 0.0443 0.3078 0.095 Uiso 1 1 d R . . C31 C 0.6086(3) 0.7077(2) 0.35327(14) 0.0389(7) Uani 1 1 d . . . H31A H 0.5974 0.6700 0.3993 0.047 Uiso 1 1 d R . . H31B H 0.5303 0.7455 0.3307 0.047 Uiso 1 1 d R . . H31C H 0.6594 0.7592 0.3524 0.047 Uiso 1 1 d R . . C32 C 0.7801(3) 0.5609(2) 0.35986(14) 0.0395(7) Uani 1 1 d . . . H32A H 0.7589 0.5318 0.4055 0.047 Uiso 1 1 d R . . H32B H 0.8403 0.6041 0.3594 0.047 Uiso 1 1 d R . . H32C H 0.8130 0.5021 0.3416 0.047 Uiso 1 1 d R . . C33 C 0.5856(3) 0.5579(2) 0.30991(14) 0.0354(7) Uani 1 1 d . . . H33A H 0.5721 0.5124 0.3535 0.042 Uiso 1 1 d R . . H33B H 0.5087 0.6019 0.2884 0.042 Uiso 1 1 d R . . C34 C 0.6450(3) 0.4885(2) 0.26626(13) 0.0327(7) Uani 1 1 d . . . H34A H 0.5851 0.4587 0.2485 0.039 Uiso 1 1 d R . . H34B H 0.7079 0.4303 0.2927 0.039 Uiso 1 1 d R . . C35 C 0.7588(2) 0.5031(2) 0.16630(12) 0.0242(6) Uani 1 1 d . . . C36 C 0.7784(2) 0.3891(2) 0.17825(13) 0.0279(6) Uani 1 1 d . . . H36 H 0.7466 0.3459 0.2174 0.033 Uiso 1 1 d R . . C37 C 0.8410(2) 0.3386(2) 0.13398(13) 0.0282(6) Uani 1 1 d . . . H37 H 0.8545 0.2606 0.1454 0.034 Uiso 1 1 d R . . C38 C 0.8858(2) 0.3974(2) 0.07565(13) 0.0282(6) Uani 1 1 d . . . H38 H 0.9305 0.3632 0.0450 0.034 Uiso 1 1 d R . . C39 C 0.8641(2) 0.5096(2) 0.06165(12) 0.0262(6) Uani 1 1 d . . . H39 H 0.8909 0.5533 0.0209 0.031 Uiso 1 1 d R . . C40 C 0.8011(2) 0.56340(19) 0.10493(12) 0.0236(6) Uani 1 1 d . . . C41 C 0.6222(2) 0.7381(2) 0.02266(12) 0.0256(6) Uani 1 1 d . . . C42 C 0.5703(2) 0.6568(2) 0.01053(14) 0.0301(6) Uani 1 1 d . . . H42 H 0.6069 0.5816 0.0316 0.036 Uiso 1 1 d R . . C43 C 0.4648(3) 0.6818(2) -0.03104(15) 0.0378(7) Uani 1 1 d . . . H43 H 0.4293 0.6242 -0.0374 0.045 Uiso 1 1 d R . . C44 C 0.4101(3) 0.7889(3) -0.06272(15) 0.0398(7) Uani 1 1 d . . . H44 H 0.3395 0.8060 -0.0934 0.048 Uiso 1 1 d R . . C45 C 0.4592(3) 0.8710(2) -0.05093(15) 0.0366(7) Uani 1 1 d . . . H45 H 0.4203 0.9455 -0.0724 0.044 Uiso 1 1 d R . . C46 C 0.5626(3) 0.8467(2) -0.00782(13) 0.0300(6) Uani 1 1 d . . . H46 H 0.5937 0.9048 0.0012 0.036 Uiso 1 1 d R . . C47 C 0.8751(2) 0.76293(19) 0.03444(12) 0.0242(6) Uani 1 1 d . . . C48 C 0.8570(3) 0.8381(2) -0.02933(13) 0.0312(6) Uani 1 1 d . . . H48 H 0.7781 0.8556 -0.0529 0.037 Uiso 1 1 d R . . C49 C 0.9529(3) 0.8851(2) -0.05914(15) 0.0417(8) Uani 1 1 d . . . H49 H 0.9399 0.9382 -0.1028 0.050 Uiso 1 1 d R . . C50 C 1.0661(3) 0.8585(2) -0.02576(17) 0.0425(8) Uani 1 1 d . . . H50 H 1.1298 0.8939 -0.0465 0.051 Uiso 1 1 d R . . C51 C 1.0866(3) 0.7824(2) 0.03680(15) 0.0364(7) Uani 1 1 d . . . H51 H 1.1664 0.7622 0.0597 0.044 Uiso 1 1 d R . . C52 C 0.9916(2) 0.7359(2) 0.06655(13) 0.0298(6) Uani 1 1 d . . . H52 H 1.0070 0.6833 0.1104 0.036 Uiso 1 1 d R . . C53 C 0.5488(3) 0.8165(2) 0.18714(14) 0.0306(6) Uani 1 1 d . . . H53A H 0.5455 0.8674 0.2129 0.037 Uiso 1 1 d R . . H53B H 0.5505 0.8538 0.1400 0.037 Uiso 1 1 d R . . C54 C 0.4156(3) 0.8006(2) 0.18948(15) 0.0382(7) Uani 1 1 d . . . H54 H 0.4022 0.7714 0.2364 0.046 Uiso 1 1 d R . . C55 C 0.3940(3) 0.7214(2) 0.15118(16) 0.0426(8) Uani 1 1 d . . . H55A H 0.3104 0.7134 0.1547 0.051 Uiso 1 1 d R . . H55B H 0.4477 0.6518 0.1702 0.051 Uiso 1 1 d R . . H55C H 0.4098 0.7496 0.1045 0.051 Uiso 1 1 d R . . C56 C 0.3239(3) 0.9081(3) 0.16208(19) 0.0557(9) Uani 1 1 d . . . H56A H 0.2421 0.8951 0.1649 0.067 Uiso 1 1 d R . . H56B H 0.3391 0.9400 0.1157 0.067 Uiso 1 1 d R . . H56C H 0.3329 0.9570 0.1878 0.067 Uiso 1 1 d R . . C57 C 0.8571(3) 0.7418(2) 0.23076(13) 0.0294(6) Uani 1 1 d . . . H57A H 0.8920 0.7021 0.2755 0.035 Uiso 1 1 d R A . H57B H 0.9126 0.7247 0.1981 0.035 Uiso 1 1 d R . . C58 C 0.8596(5) 0.8585(4) 0.2302(4) 0.0311(14) Uani 0.634(8) 1 d P A 1 H58 H 0.8022 0.8774 0.2630 0.037 Uiso 0.634(8) 1 calc PR A 1 C59 C 0.8159(5) 0.9382(4) 0.1612(3) 0.0446(18) Uani 0.634(8) 1 d P A 1 H59A H 0.8175 1.0108 0.1621 0.067 Uiso 0.634(8) 1 calc PR A 1 H59B H 0.7338 0.9343 0.1502 0.067 Uiso 0.634(8) 1 calc PR A 1 H59C H 0.8689 0.9199 0.1277 0.067 Uiso 0.634(8) 1 calc PR A 1 C60 C 0.9845(6) 0.8728(5) 0.2505(3) 0.0520(18) Uani 0.634(8) 1 d P A 1 H60A H 1.0118 0.8233 0.2944 0.078 Uiso 0.634(8) 1 calc PR A 1 H60B H 0.9787 0.9463 0.2519 0.078 Uiso 0.634(8) 1 calc PR A 1 H60C H 1.0420 0.8580 0.2181 0.078 Uiso 0.634(8) 1 calc PR A 1 C58A C 0.8787(9) 0.8543(7) 0.1925(6) 0.032(2) Uani 0.366(8) 1 d P A 2 H58A H 0.8647 0.8653 0.1440 0.039 Uiso 0.366(8) 1 calc PR A 2 C59A C 0.7979(9) 0.9453(7) 0.2112(5) 0.043(3) Uani 0.366(8) 1 d P A 2 H59D H 0.8158 1.0133 0.1850 0.064 Uiso 0.366(8) 1 calc PR A 2 H59E H 0.8121 0.9366 0.2584 0.064 Uiso 0.366(8) 1 calc PR A 2 H59F H 0.7138 0.9446 0.2021 0.064 Uiso 0.366(8) 1 calc PR A 2 C60A C 1.0129(7) 0.8547(7) 0.2065(5) 0.040(3) Uani 0.366(8) 1 d P A 2 H60D H 1.0645 0.7963 0.1940 0.061 Uiso 0.366(8) 1 calc PR A 2 H60E H 1.0277 0.8452 0.2538 0.061 Uiso 0.366(8) 1 calc PR A 2 H60F H 1.0308 0.9229 0.1807 0.061 Uiso 0.366(8) 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 0.0275(4) 0.0235(4) 0.0207(4) -0.0040(3) -0.0006(3) -0.0068(3) P2 0.0254(4) 0.0217(3) 0.0191(3) -0.0050(3) 0.0034(3) -0.0052(3) Al1 0.0290(5) 0.0214(4) 0.0221(4) -0.0048(3) -0.0017(3) -0.0048(3) Al2 0.0328(5) 0.0207(4) 0.0222(4) -0.0065(3) 0.0065(3) -0.0082(3) N1 0.0405(14) 0.0273(12) 0.0231(12) -0.0085(10) -0.0046(10) -0.0038(10) N2 0.0348(13) 0.0227(11) 0.0209(11) -0.0039(9) -0.0052(10) -0.0040(10) N3 0.0454(15) 0.0245(12) 0.0235(12) -0.0079(10) 0.0106(11) -0.0070(10) N4 0.0362(13) 0.0216(11) 0.0207(11) -0.0058(9) 0.0096(10) -0.0097(10) C1 0.057(2) 0.0321(16) 0.0283(15) -0.0127(13) -0.0101(14) -0.0005(14) C2 0.055(2) 0.0324(16) 0.0237(14) -0.0046(12) 0.0008(13) -0.0088(14) C3 0.0406(18) 0.0310(15) 0.0276(15) -0.0053(12) -0.0116(13) -0.0010(13) C4 0.0370(17) 0.0260(14) 0.0259(14) -0.0043(11) -0.0067(12) 0.0009(12) C5 0.0275(14) 0.0254(13) 0.0210(13) -0.0081(11) 0.0048(11) -0.0070(11) C6 0.0324(16) 0.0266(14) 0.0267(14) -0.0057(11) 0.0018(12) -0.0029(12) C7 0.0362(16) 0.0252(14) 0.0353(16) -0.0136(12) 0.0054(13) -0.0044(12) C8 0.0334(16) 0.0339(15) 0.0309(15) -0.0177(13) 0.0059(12) -0.0103(12) C9 0.0286(15) 0.0310(14) 0.0199(13) -0.0075(11) 0.0013(11) -0.0080(12) C10 0.0237(14) 0.0251(13) 0.0218(13) -0.0070(11) 0.0035(11) -0.0052(11) C11 0.0308(15) 0.0235(13) 0.0227(13) -0.0103(11) 0.0007(11) -0.0057(11) C12 0.0364(17) 0.0296(15) 0.0299(15) -0.0090(12) 0.0002(13) -0.0100(13) C13 0.0307(16) 0.0359(16) 0.0409(17) -0.0167(14) 0.0038(13) -0.0090(13) C14 0.0313(17) 0.0322(16) 0.0457(18) -0.0172(14) -0.0109(14) 0.0033(13) C15 0.0384(18) 0.0340(16) 0.0301(15) -0.0043(13) -0.0046(13) 0.0019(13) C16 0.0326(16) 0.0297(14) 0.0258(14) -0.0081(12) 0.0016(12) -0.0024(12) C17 0.0291(15) 0.0363(16) 0.0228(14) -0.0022(12) -0.0039(11) -0.0114(12) C18 0.0352(17) 0.0524(19) 0.0356(17) -0.0161(14) 0.0060(14) -0.0173(15) C19 0.0368(19) 0.080(3) 0.051(2) -0.0305(19) 0.0159(16) -0.0250(18) C20 0.053(2) 0.099(3) 0.045(2) -0.022(2) 0.0163(18) -0.050(2) C21 0.056(2) 0.062(2) 0.0358(18) 0.0022(16) -0.0009(16) -0.0361(19) C22 0.0419(18) 0.0405(17) 0.0288(15) 0.0004(13) -0.0044(13) -0.0175(14) C23 0.0379(16) 0.0263(14) 0.0248(14) -0.0069(11) 0.0009(12) -0.0111(12) C24 0.0376(17) 0.0333(15) 0.0299(15) -0.0094(12) -0.0001(13) -0.0024(13) C25 0.043(2) 0.050(2) 0.064(2) -0.0274(17) -0.0115(17) 0.0022(15) C26 0.0460(19) 0.0325(16) 0.053(2) -0.0154(14) 0.0076(16) -0.0098(14) C27 0.0311(16) 0.0291(15) 0.0330(15) -0.0074(12) -0.0049(12) -0.0068(12) C28 0.0298(17) 0.0395(17) 0.0499(19) -0.0005(15) -0.0055(14) -0.0107(14) C29 0.0299(17) 0.061(2) 0.0395(18) -0.0038(16) -0.0002(14) -0.0078(15) C30 0.037(2) 0.054(2) 0.135(4) -0.002(2) -0.006(2) -0.0239(18) C31 0.062(2) 0.0294(15) 0.0276(15) -0.0110(12) 0.0184(14) -0.0101(14) C32 0.061(2) 0.0310(16) 0.0234(15) -0.0037(12) 0.0040(14) -0.0079(14) C33 0.0514(19) 0.0254(14) 0.0293(15) -0.0039(12) 0.0184(14) -0.0140(13) C34 0.0464(18) 0.0255(14) 0.0285(15) -0.0076(12) 0.0147(13) -0.0137(13) C35 0.0255(14) 0.0249(13) 0.0229(13) -0.0075(11) -0.0002(11) -0.0060(11) C36 0.0353(16) 0.0244(14) 0.0257(14) -0.0076(11) 0.0029(12) -0.0099(12) C37 0.0313(15) 0.0233(13) 0.0306(15) -0.0099(12) -0.0030(12) -0.0042(11) C38 0.0312(15) 0.0293(14) 0.0267(14) -0.0139(12) 0.0018(12) -0.0041(12) C39 0.0279(15) 0.0310(14) 0.0195(13) -0.0073(11) 0.0011(11) -0.0052(12) C40 0.0235(14) 0.0244(13) 0.0224(13) -0.0059(11) 0.0011(11) -0.0056(11) C41 0.0252(14) 0.0306(14) 0.0221(13) -0.0085(11) 0.0041(11) -0.0071(11) C42 0.0273(15) 0.0301(15) 0.0346(15) -0.0121(12) 0.0055(12) -0.0064(12) C43 0.0295(16) 0.0448(18) 0.0466(18) -0.0223(15) 0.0024(14) -0.0115(14) C44 0.0265(16) 0.0523(19) 0.0404(17) -0.0171(15) -0.0029(13) -0.0026(14) C45 0.0318(16) 0.0335(16) 0.0386(17) -0.0074(13) -0.0027(13) 0.0022(13) C46 0.0318(16) 0.0278(14) 0.0292(15) -0.0071(12) 0.0016(12) -0.0054(12) C47 0.0284(15) 0.0219(13) 0.0230(13) -0.0085(11) 0.0057(11) -0.0043(11) C48 0.0320(16) 0.0305(15) 0.0281(15) -0.0041(12) 0.0028(12) -0.0065(12) C49 0.0432(19) 0.0354(17) 0.0367(17) 0.0057(13) 0.0100(15) -0.0098(14) C50 0.0382(19) 0.0394(17) 0.055(2) -0.0163(16) 0.0210(16) -0.0163(14) C51 0.0278(16) 0.0454(17) 0.0409(17) -0.0194(14) 0.0043(13) -0.0091(13) C52 0.0282(15) 0.0355(15) 0.0249(14) -0.0089(12) 0.0016(12) -0.0050(12) C53 0.0384(17) 0.0266(14) 0.0280(14) -0.0089(12) 0.0094(12) -0.0080(12) C54 0.0361(17) 0.0356(16) 0.0400(17) -0.0060(13) 0.0116(14) -0.0079(13) C55 0.0351(18) 0.0481(18) 0.0453(18) -0.0094(15) 0.0054(14) -0.0166(14) C56 0.0354(19) 0.047(2) 0.075(3) -0.0077(18) 0.0097(18) -0.0013(15) C57 0.0381(16) 0.0286(14) 0.0204(13) -0.0048(11) 0.0028(12) -0.0083(12) C58 0.035(3) 0.027(3) 0.036(4) -0.012(3) 0.004(2) -0.012(2) C59 0.044(3) 0.029(3) 0.056(4) -0.002(3) -0.007(3) -0.012(2) C60 0.057(4) 0.048(3) 0.058(4) -0.019(3) -0.005(3) -0.023(3) C58A 0.042(5) 0.032(5) 0.025(5) -0.007(4) 0.002(4) -0.010(4) C59A 0.045(6) 0.041(6) 0.044(6) -0.014(5) 0.004(4) -0.014(5) C60A 0.032(5) 0.039(5) 0.051(7) -0.012(4) 0.008(4) -0.010(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 C10 1.807(2) . ? P1 C11 1.827(3) . ? P1 C17 1.834(3) . ? P1 Al1 2.7827(10) . ? P2 C40 1.804(2) . ? P2 C41 1.826(3) . ? P2 C47 1.834(2) . ? P2 Al2 2.7818(9) . ? Al1 N2 1.914(2) . ? Al1 C23 1.990(3) . ? Al1 C27 1.998(3) . ? Al1 N1 2.098(2) . ? Al2 N4 1.912(2) . ? Al2 C57 1.994(3) . ? Al2 C53 1.997(3) . ? Al2 N3 2.111(2) . ? N1 C1 1.480(3) . ? N1 C3 1.485(4) . ? N1 C2 1.481(4) . ? N2 C5 1.385(3) . ? N2 C4 1.457(3) . ? N3 C33 1.479(4) . ? N3 C31 1.476(3) . ? N3 C32 1.484(4) . ? N4 C35 1.383(3) . ? N4 C34 1.464(3) . ? C1 H1A 0.9597 . ? C1 H1B 0.9595 . ? C1 H1C 0.9603 . ? C2 H2A 0.9604 . ? C2 H2B 0.9597 . ? C2 H2C 0.9605 . ? C3 C4 1.513(4) . ? C3 H3A 0.9601 . ? C3 H3B 0.9603 . ? C4 H4A 0.9599 . ? C4 H4B 0.9599 . ? C5 C6 1.418(3) . ? C5 C10 1.415(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9602 . ? C7 C8 1.385(4) . ? C7 H7 0.9596 . ? C8 C9 1.382(4) . ? C8 H8 0.9581 . ? C9 C10 1.400(3) . ? C9 H9 0.9609 . ? C11 C12 1.397(4) . ? C11 C16 1.397(4) . ? C12 C13 1.383(4) . ? C12 H12 0.9596 . ? C13 C14 1.381(4) . ? C13 H13 0.9593 . ? C14 C15 1.384(4) . ? C14 H14 0.9606 . ? C15 C16 1.382(4) . ? C15 H15 0.9597 . ? C16 H16 0.9609 . ? C17 C18 1.389(4) . ? C17 C22 1.396(4) . ? C18 C19 1.390(4) . ? C18 H18 0.9593 . ? C19 C20 1.384(5) . ? C19 H19 0.9600 . ? C20 C21 1.383(5) . ? C20 H20 0.9608 . ? C21 C22 1.375(4) . ? C21 H21 0.9610 . ? C22 H22 0.9601 . ? C23 C24 1.538(4) . ? C23 H23A 0.9595 . ? C23 H23B 0.9607 . ? C24 C25 1.521(4) . ? C24 C26 1.518(4) . ? C24 H24 0.9597 . ? C25 H25A 0.9596 . ? C25 H25B 0.9605 . ? C25 H25C 0.9594 . ? C26 H26A 0.9607 . ? C26 H26B 0.9598 . ? C26 H26C 0.9602 . ? C27 C28 1.542(4) . ? C27 H27A 0.9582 . ? C27 H27B 0.9609 . ? C28 C30 1.526(4) . ? C28 C29 1.521(4) . ? C28 H28 0.9602 . ? C29 H29A 0.9599 . ? C29 H29B 0.9595 . ? C29 H29C 0.9611 . ? C30 H30A 0.9590 . ? C30 H30B 0.9606 . ? C30 H30C 0.9603 . ? C31 H31A 0.9593 . ? C31 H31B 0.9605 . ? C31 H31C 0.9609 . ? C32 H32A 0.9593 . ? C32 H32B 0.9597 . ? C32 H32C 0.9611 . ? C33 C34 1.519(3) . ? C33 H33A 0.9588 . ? C33 H33B 0.9605 . ? C34 H34A 0.9604 . ? C34 H34B 0.9596 . ? C35 C36 1.413(3) . ? C35 C40 1.426(3) . ? C36 C37 1.386(4) . ? C36 H36 0.9595 . ? C37 C38 1.386(4) . ? C37 H37 0.9609 . ? C38 C39 1.385(3) . ? C38 H38 0.9611 . ? C39 C40 1.397(3) . ? C39 H39 0.9596 . ? C41 C42 1.391(4) . ? C41 C46 1.405(4) . ? C42 C43 1.385(4) . ? C42 H42 0.9599 . ? C43 C44 1.380(4) . ? C43 H43 0.9598 . ? C44 C45 1.380(4) . ? C44 H44 0.9610 . ? C45 C46 1.386(4) . ? C45 H45 0.9600 . ? C46 H46 0.9601 . ? C47 C48 1.389(4) . ? C47 C52 1.392(4) . ? C48 C49 1.396(4) . ? C48 H48 0.9604 . ? C49 C50 1.371(4) . ? C49 H49 0.9605 . ? C50 C51 1.376(4) . ? C50 H50 0.9598 . ? C51 C52 1.385(4) . ? C51 H51 0.9605 . ? C52 H52 0.9598 . ? C53 C54 1.540(4) . ? C53 H53A 0.9612 . ? C53 H53B 0.9589 . ? C54 C56 1.524(4) . ? C54 C55 1.528(4) . ? C54 H54 0.9590 . ? C55 H55A 0.9596 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9601 . ? C56 H56B 0.9606 . ? C56 H56C 0.9610 . ? C57 C58A 1.528(9) . ? C57 C58 1.531(5) . ? C57 H57A 0.9602 . ? C57 H57B 0.9591 . ? C58 C59 1.521(9) . ? C58 C60 1.518(7) . ? C58 H58 0.9800 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C58A C59A 1.487(15) . ? C58A C60A 1.527(12) . ? C58A H58A 0.9800 . ? C59A H59D 0.9600 . ? C59A H59E 0.9600 . ? C59A H59F 0.9600 . ? C60A H60D 0.9600 . ? C60A H60E 0.9600 . ? C60A H60F 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 C10 P1 C11 104.65(11) . . ? C10 P1 C17 103.59(12) . . ? C11 P1 C17 104.35(12) . . ? C10 P1 Al1 91.53(8) . . ? C11 P1 Al1 130.52(8) . . ? C17 P1 Al1 116.90(9) . . ? C40 P2 C41 102.99(12) . . ? C40 P2 C47 104.96(11) . . ? C41 P2 C47 106.02(11) . . ? C40 P2 Al2 91.56(8) . . ? C41 P2 Al2 117.08(8) . . ? C47 P2 Al2 128.75(8) . . ? N2 Al1 C23 121.17(10) . . ? N2 Al1 C27 119.51(11) . . ? C23 Al1 C27 117.60(11) . . ? N2 Al1 N1 82.84(9) . . ? C23 Al1 N1 98.81(10) . . ? C27 Al1 N1 101.59(11) . . ? N2 Al1 P1 75.67(7) . . ? C23 Al1 P1 88.69(8) . . ? C27 Al1 P1 92.95(9) . . ? N1 Al1 P1 158.05(7) . . ? N4 Al2 C57 120.11(11) . . ? N4 Al2 C53 119.93(11) . . ? C57 Al2 C53 118.47(11) . . ? N4 Al2 N3 82.93(8) . . ? C57 Al2 N3 98.07(10) . . ? C53 Al2 N3 101.19(10) . . ? N4 Al2 P2 75.37(6) . . ? C57 Al2 P2 90.47(8) . . ? C53 Al2 P2 92.20(8) . . ? N3 Al2 P2 158.12(7) . . ? C1 N1 C3 111.0(2) . . ? C1 N1 C2 108.5(2) . . ? C3 N1 C2 109.7(2) . . ? C1 N1 Al1 114.53(17) . . ? C3 N1 Al1 99.85(15) . . ? C2 N1 Al1 113.03(17) . . ? C5 N2 C4 115.6(2) . . ? C5 N2 Al1 129.38(18) . . ? C4 N2 Al1 114.38(16) . . ? C33 N3 C31 111.0(2) . . ? C33 N3 C32 109.4(2) . . ? C31 N3 C32 108.3(2) . . ? C33 N3 Al2 99.69(15) . . ? C31 N3 Al2 114.30(16) . . ? C32 N3 Al2 113.93(16) . . ? C35 N4 C34 115.19(19) . . ? C35 N4 Al2 129.67(16) . . ? C34 N4 Al2 114.49(16) . . ? N1 C1 H1A 109.4 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.3 . . ? H1A C1 H1C 109.4 . . ? H1B C1 H1C 109.4 . . ? N1 C2 H2A 109.2 . . ? N1 C2 H2B 109.8 . . ? H2A C2 H2B 109.3 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 108.6(2) . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3A 110.5 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 109.4 . . ? N2 C4 C3 109.2(2) . . ? N2 C4 H4A 109.2 . . ? C3 C4 H4A 110.2 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 109.5 . . ? N2 C5 C6 122.8(2) . . ? N2 C5 C10 120.8(2) . . ? C6 C5 C10 116.5(2) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 121.3(2) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 118.3(2) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 121.9 . . ? C8 C9 C10 121.6(2) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 120.7(2) . . ? C9 C10 P1 122.78(19) . . ? C5 C10 P1 116.23(18) . . ? C12 C11 C16 117.5(3) . . ? C12 C11 P1 118.20(19) . . ? C16 C11 P1 124.1(2) . . ? C13 C12 C11 121.5(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 121.2(3) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 118.9 . . ? C18 C17 C22 118.7(3) . . ? C18 C17 P1 123.2(2) . . ? C22 C17 P1 117.8(2) . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 120.8 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.5 . . ? C21 C22 C17 121.4(3) . . ? C21 C22 H22 118.2 . . ? C17 C22 H22 120.4 . . ? C24 C23 Al1 119.07(18) . . ? C24 C23 H23A 104.9 . . ? Al1 C23 H23A 109.7 . . ? C24 C23 H23B 104.4 . . ? Al1 C23 H23B 108.9 . . ? H23A C23 H23B 109.5 . . ? C25 C24 C26 109.8(2) . . ? C25 C24 C23 111.4(2) . . ? C26 C24 C23 110.7(2) . . ? C25 C24 H24 107.9 . . ? C26 C24 H24 109.9 . . ? C23 C24 H24 107.1 . . ? C24 C25 H25A 108.6 . . ? C24 C25 H25B 110.6 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.2 . . ? H25A C25 H25C 109.6 . . ? H25B C25 H25C 109.4 . . ? C24 C26 H26A 108.9 . . ? C24 C26 H26B 109.9 . . ? H26A C26 H26B 109.6 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.4 . . ? H26B C26 H26C 109.6 . . ? C28 C27 Al1 125.89(19) . . ? C28 C27 H27A 101.2 . . ? Al1 C27 H27A 109.6 . . ? C28 C27 H27B 100.1 . . ? Al1 C27 H27B 109.4 . . ? H27A C27 H27B 109.5 . . ? C30 C28 C29 109.3(3) . . ? C30 C28 C27 110.3(3) . . ? C29 C28 C27 113.3(2) . . ? C30 C28 H28 108.9 . . ? C29 C28 H28 108.6 . . ? C27 C28 H28 106.3 . . ? C28 C29 H29A 109.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 108.6 . . ? H29A C29 H29C 109.4 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.8 . . ? C28 C30 H30B 109.3 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.4 . . ? N3 C31 H31A 109.6 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.2 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.2 . . ? N3 C32 H32B 110.1 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.1 . . ? H32A C32 H32C 109.4 . . ? H32B C32 H32C 109.5 . . ? N3 C33 C34 108.8(2) . . ? N3 C33 H33A 109.0 . . ? C34 C33 H33A 110.2 . . ? N3 C33 H33B 109.7 . . ? C34 C33 H33B 109.6 . . ? H33A C33 H33B 109.5 . . ? N4 C34 C33 108.9(2) . . ? N4 C34 H34A 109.2 . . ? C33 C34 H34A 110.5 . . ? N4 C34 H34B 109.0 . . ? C33 C34 H34B 109.7 . . ? H34A C34 H34B 109.5 . . ? N4 C35 C36 123.3(2) . . ? N4 C35 C40 120.2(2) . . ? C36 C35 C40 116.5(2) . . ? C37 C36 C35 121.4(2) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 121.7(2) . . ? C36 C37 H37 118.0 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 118.0(2) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 122.4 . . ? C38 C39 C40 121.9(2) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 117.6 . . ? C39 C40 C35 120.3(2) . . ? C39 C40 P2 123.27(18) . . ? C35 C40 P2 115.98(18) . . ? C42 C41 C46 117.6(3) . . ? C42 C41 P2 122.9(2) . . ? C46 C41 P2 119.15(19) . . ? C43 C42 C41 121.3(3) . . ? C43 C42 H42 118.6 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.3(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 119.4(3) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.4 . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 120.7(3) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.8 . . ? C48 C47 C52 117.7(2) . . ? C48 C47 P2 124.3(2) . . ? C52 C47 P2 117.59(19) . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 120.8 . . ? C50 C49 C48 120.6(3) . . ? C50 C49 H49 119.0 . . ? C48 C49 H49 120.4 . . ? C49 C50 C51 119.9(3) . . ? C49 C50 H50 119.2 . . ? C51 C50 H50 121.0 . . ? C50 C51 C52 119.6(3) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.4 . . ? C51 C52 C47 121.8(3) . . ? C51 C52 H52 118.8 . . ? C47 C52 H52 119.5 . . ? C54 C53 Al2 126.38(19) . . ? C54 C53 H53A 100.9 . . ? Al2 C53 H53A 109.6 . . ? C54 C53 H53B 100.0 . . ? Al2 C53 H53B 109.4 . . ? H53A C53 H53B 109.4 . . ? C56 C54 C55 109.3(3) . . ? C56 C54 C53 112.0(2) . . ? C55 C54 C53 112.3(2) . . ? C56 C54 H54 107.9 . . ? C55 C54 H54 109.4 . . ? C53 C54 H54 105.8 . . ? C54 C55 H55A 109.1 . . ? C54 C55 H55B 109.9 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.4 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.4 . . ? C54 C56 H56A 109.6 . . ? C54 C56 H56B 108.7 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 110.2 . . ? H56A C56 H56C 109.4 . . ? H56B C56 H56C 109.4 . . ? C58A C57 C58 31.2(3) . . ? C58A C57 Al2 120.6(4) . . ? C58 C57 Al2 120.9(2) . . ? C58A C57 H57A 123.4 . . ? C58 C57 H57A 100.7 . . ? Al2 C57 H57A 109.5 . . ? C58A C57 H57B 78.5 . . ? C58 C57 H57B 106.7 . . ? Al2 C57 H57B 109.0 . . ? H57A C57 H57B 109.5 . . ? C59 C58 C57 110.8(5) . . ? C59 C58 C60 109.3(4) . . ? C57 C58 C60 113.7(4) . . ? C59 C58 H58 107.6 . . ? C57 C58 H58 107.6 . . ? C60 C58 H58 107.6 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59A C58A C57 113.9(9) . . ? C59A C58A C60A 109.9(8) . . ? C57 C58A C60A 107.5(6) . . ? C59A C58A H58A 108.5 . . ? C57 C58A H58A 108.5 . . ? C60A C58A H58A 108.5 . . ? C58A C59A H59D 109.5 . . ? C58A C59A H59E 109.5 . . ? H59D C59A H59E 109.5 . . ? C58A C59A H59F 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C58A C60A H60D 109.5 . . ? C58A C60A H60E 109.5 . . ? H60D C60A H60E 109.5 . . ? C58A C60A H60F 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.669 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.189 data_3211 _database_code_depnum_ccdc_archive 'CCDC 264440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 Al1 N2 P1' _chemical_formula_sum 'C24 H30 Al N2 P' _chemical_formula_weight 404.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9523(2) _cell_length_b 11.1101(3) _cell_length_c 11.7142(3) _cell_angle_alpha 80.2789(9) _cell_angle_beta 74.9271(9) _cell_angle_gamma 65.7727(9) _cell_volume 1137.63(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8058 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9322 _exptl_absorpt_correction_T_max 0.9941 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11107 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3992 _reflns_number_gt 2773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0900P)^2^+0.0227P] 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 SHELXL _refine_ls_extinction_coef 0.038(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3992 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.89392(7) 0.33171(6) 0.73496(6) 0.0418(3) Uani 1 1 d . . . Al1 Al 0.86157(9) 0.58417(8) 0.76323(7) 0.0463(3) Uani 1 1 d . . . N1 N 0.7904(3) 0.7633(2) 0.8465(2) 0.0577(7) Uani 1 1 d . . . N2 N 0.7415(2) 0.5384(2) 0.90461(19) 0.0456(6) Uani 1 1 d . . . C1 C 0.7699(4) 0.6561(3) 0.6229(3) 0.0736(10) Uani 1 1 d . . . H1A H 0.6630 0.6791 0.6464 0.110 Uiso 1 1 calc R . . H1B H 0.8126 0.5906 0.5657 0.110 Uiso 1 1 calc R . . H1C H 0.7897 0.7335 0.5884 0.110 Uiso 1 1 calc R . . C2 C 1.0803(3) 0.5276(3) 0.7464(3) 0.0604(8) Uani 1 1 d . . . H2A H 1.1061 0.4954 0.8223 0.091 Uiso 1 1 calc R . . H2B H 1.1090 0.6014 0.7158 0.091 Uiso 1 1 calc R . . H2C H 1.1326 0.4584 0.6927 0.091 Uiso 1 1 calc R . . C3 C 0.7886(5) 0.8815(3) 0.7667(4) 0.0900(12) Uani 1 1 d . . . H3A H 0.8901 0.8713 0.7285 0.135 Uiso 1 1 calc R . . H3B H 0.7421 0.9583 0.8117 0.135 Uiso 1 1 calc R . . H3C H 0.7324 0.8918 0.7078 0.135 Uiso 1 1 calc R . . C4 C 0.8796(4) 0.7473(4) 0.9360(3) 0.0760(10) Uani 1 1 d . . . H4A H 0.8814 0.6704 0.9883 0.114 Uiso 1 1 calc R . . H4B H 0.8342 0.8241 0.9809 0.114 Uiso 1 1 calc R . . H4C H 0.9808 0.7369 0.8965 0.114 Uiso 1 1 calc R . . C5 C 0.6352(3) 0.7770(3) 0.9063(3) 0.0650(9) Uani 1 1 d . . . H5A H 0.5912 0.8493 0.9565 0.078 Uiso 1 1 d R . . H5B H 0.5769 0.7945 0.8473 0.078 Uiso 1 1 d R . . C6 C 0.6391(3) 0.6492(3) 0.9773(3) 0.0561(8) Uani 1 1 d . . . H6A H 0.5409 0.6455 0.9983 0.067 Uiso 1 1 d R . . H6B H 0.6747 0.6412 1.0480 0.067 Uiso 1 1 d R . . C7 C 0.7545(3) 0.4144(2) 0.9587(2) 0.0416(6) Uani 1 1 d . . . C8 C 0.6898(3) 0.3927(3) 1.0787(3) 0.0524(7) Uani 1 1 d . . . H8 H 0.6303 0.4673 1.1256 0.063 Uiso 1 1 d R . . C9 C 0.7099(3) 0.2678(3) 1.1304(3) 0.0602(8) Uani 1 1 d . . . H9 H 0.6650 0.2560 1.2124 0.072 Uiso 1 1 d R . . C10 C 0.7934(3) 0.1566(3) 1.0665(3) 0.0597(8) Uani 1 1 d . . . H10 H 0.8120 0.0684 1.1020 0.072 Uiso 1 1 d R . . C11 C 0.8538(3) 0.1747(3) 0.9475(3) 0.0533(7) Uani 1 1 d . . . H11 H 0.9093 0.0979 0.9027 0.064 Uiso 1 1 d R . . C12 C 0.8347(3) 0.3003(2) 0.8925(2) 0.0418(6) Uani 1 1 d . . . C13 C 0.7495(3) 0.3188(2) 0.6735(2) 0.0445(7) Uani 1 1 d . . . C14 C 0.6327(3) 0.2849(3) 0.7413(3) 0.0598(8) Uani 1 1 d . . . H14 H 0.6295 0.2613 0.8244 0.072 Uiso 1 1 d R . . C15 C 0.5217(3) 0.2844(3) 0.6903(3) 0.0727(10) Uani 1 1 d . . . H15 H 0.4396 0.2621 0.7377 0.087 Uiso 1 1 d R . . C16 C 0.5273(4) 0.3161(3) 0.5718(3) 0.0689(10) Uani 1 1 d . . . H16 H 0.4503 0.3164 0.5365 0.083 Uiso 1 1 d R . . C17 C 0.6441(4) 0.3478(3) 0.5025(3) 0.0673(9) Uani 1 1 d . . . H17 H 0.6492 0.3679 0.4188 0.081 Uiso 1 1 d R . . C18 C 0.7538(4) 0.3508(3) 0.5526(3) 0.0565(8) Uani 1 1 d . . . H18 H 0.8352 0.3737 0.5045 0.068 Uiso 1 1 d R . . C19 C 1.0608(3) 0.1844(2) 0.6877(2) 0.0438(6) Uani 1 1 d . . . C20 C 1.0623(4) 0.0902(3) 0.6236(3) 0.0673(9) Uani 1 1 d . . . H20 H 0.9689 0.0969 0.6089 0.081 Uiso 1 1 d R . . C21 C 1.1941(4) -0.0139(3) 0.5836(3) 0.0828(11) Uani 1 1 d . . . H21 H 1.1919 -0.0763 0.5372 0.099 Uiso 1 1 d R . . C22 C 1.3265(4) -0.0269(3) 0.6068(3) 0.0700(10) Uani 1 1 d . . . H22 H 1.4176 -0.0995 0.5774 0.084 Uiso 1 1 d R . . C23 C 1.3283(3) 0.0627(3) 0.6715(3) 0.0695(9) Uani 1 1 d . . . H23 H 1.4200 0.0538 0.6910 0.083 Uiso 1 1 d R . . C24 C 1.1960(3) 0.1690(3) 0.7116(3) 0.0600(8) Uani 1 1 d . . . H24 H 1.1982 0.2331 0.7560 0.072 Uiso 1 1 d 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 0.0403(4) 0.0438(4) 0.0436(5) -0.0039(3) -0.0094(3) -0.0177(3) Al1 0.0462(5) 0.0508(5) 0.0460(5) 0.0030(4) -0.0151(4) -0.0220(4) N1 0.0619(16) 0.0526(14) 0.0670(17) -0.0015(11) -0.0202(13) -0.0275(12) N2 0.0431(13) 0.0448(12) 0.0496(14) -0.0073(10) -0.0081(11) -0.0172(10) C1 0.097(3) 0.0601(19) 0.073(2) 0.0081(15) -0.044(2) -0.0286(18) C2 0.0529(18) 0.0714(19) 0.062(2) -0.0013(15) -0.0096(15) -0.0323(15) C3 0.118(3) 0.058(2) 0.102(3) 0.0057(18) -0.025(3) -0.045(2) C4 0.076(2) 0.092(2) 0.080(3) -0.0230(19) -0.024(2) -0.041(2) C5 0.058(2) 0.0494(17) 0.085(2) -0.0160(16) -0.0145(18) -0.0141(15) C6 0.0463(17) 0.0590(17) 0.0597(19) -0.0163(14) -0.0013(14) -0.0184(14) C7 0.0357(14) 0.0531(16) 0.0407(16) -0.0033(12) -0.0105(12) -0.0203(12) C8 0.0490(17) 0.0662(18) 0.0452(18) -0.0051(13) -0.0064(13) -0.0269(14) C9 0.0583(19) 0.085(2) 0.0425(18) 0.0068(16) -0.0096(15) -0.0381(17) C10 0.060(2) 0.0653(19) 0.058(2) 0.0155(15) -0.0177(16) -0.0327(16) C11 0.0534(18) 0.0503(16) 0.057(2) 0.0007(13) -0.0173(15) -0.0192(14) C12 0.0382(14) 0.0469(15) 0.0428(16) 0.0021(11) -0.0119(12) -0.0189(11) C13 0.0422(16) 0.0429(14) 0.0489(17) -0.0101(11) -0.0135(13) -0.0120(12) C14 0.0490(18) 0.079(2) 0.0561(19) -0.0163(15) -0.0060(15) -0.0275(15) C15 0.0475(19) 0.098(2) 0.082(3) -0.034(2) -0.0071(17) -0.0311(17) C16 0.052(2) 0.069(2) 0.089(3) -0.0299(18) -0.0320(19) -0.0061(16) C17 0.082(2) 0.0586(19) 0.063(2) -0.0072(15) -0.0370(19) -0.0138(17) C18 0.067(2) 0.0526(17) 0.056(2) -0.0006(13) -0.0212(16) -0.0256(14) C19 0.0450(16) 0.0427(14) 0.0428(16) -0.0002(11) -0.0085(12) -0.0174(12) C20 0.057(2) 0.0561(18) 0.087(3) -0.0188(16) -0.0255(18) -0.0094(15) C21 0.079(3) 0.060(2) 0.099(3) -0.0309(19) -0.027(2) -0.0016(18) C22 0.057(2) 0.0552(19) 0.074(2) -0.0077(16) -0.0022(17) -0.0047(15) C23 0.0417(18) 0.064(2) 0.097(3) -0.0019(18) -0.0148(17) -0.0159(15) C24 0.0504(18) 0.0589(18) 0.072(2) -0.0087(15) -0.0125(16) -0.0213(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C12 1.806(3) . ? P1 C19 1.827(3) . ? P1 C13 1.829(3) . ? P1 Al1 2.7564(10) . ? Al1 N2 1.901(2) . ? Al1 C2 1.967(3) . ? Al1 C1 1.978(3) . ? Al1 N1 2.134(2) . ? N1 C3 1.475(4) . ? N1 C5 1.476(4) . ? N1 C4 1.486(4) . ? N2 C7 1.384(3) . ? N2 C6 1.467(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.510(4) . ? C5 H5A 0.9591 . ? C5 H5B 0.9605 . ? C6 H6A 0.9601 . ? C6 H6B 0.9598 . ? C7 C8 1.410(4) . ? C7 C12 1.423(4) . ? C8 C9 1.373(4) . ? C8 H8 0.9598 . ? C9 C10 1.386(4) . ? C9 H9 0.9601 . ? C10 C11 1.383(4) . ? C10 H10 0.9597 . ? C11 C12 1.393(4) . ? C11 H11 0.9603 . ? C13 C14 1.379(4) . ? C13 C18 1.394(4) . ? C14 C15 1.387(4) . ? C14 H14 0.9601 . ? C15 C16 1.366(5) . ? C15 H15 0.9597 . ? C16 C17 1.373(5) . ? C16 H16 0.9594 . ? C17 C18 1.381(4) . ? C17 H17 0.9608 . ? C18 H18 0.9601 . ? C19 C20 1.380(4) . ? C19 C24 1.381(4) . ? C20 C21 1.377(4) . ? C20 H20 0.9598 . ? C21 C22 1.360(5) . ? C21 H21 0.9605 . ? C22 C23 1.358(5) . ? C22 H22 0.9604 . ? C23 C24 1.393(4) . ? C23 H23 0.9599 . ? C24 H24 0.9603 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 P1 C19 105.25(12) . . ? C12 P1 C13 103.54(13) . . ? C19 P1 C13 103.45(12) . . ? C12 P1 Al1 91.84(8) . . ? C19 P1 Al1 131.60(9) . . ? C13 P1 Al1 116.20(8) . . ? N2 Al1 C2 120.80(12) . . ? N2 Al1 C1 117.89(14) . . ? C2 Al1 C1 120.08(15) . . ? N2 Al1 N1 83.11(9) . . ? C2 Al1 N1 98.30(12) . . ? C1 Al1 N1 99.47(12) . . ? N2 Al1 P1 75.77(7) . . ? C2 Al1 P1 91.43(10) . . ? C1 Al1 P1 91.69(10) . . ? N1 Al1 P1 158.84(8) . . ? C3 N1 C5 110.4(3) . . ? C3 N1 C4 108.9(3) . . ? C5 N1 C4 110.0(3) . . ? C3 N1 Al1 116.1(2) . . ? C5 N1 Al1 99.40(16) . . ? C4 N1 Al1 111.67(18) . . ? C7 N2 C6 114.8(2) . . ? C7 N2 Al1 129.20(17) . . ? C6 N2 Al1 114.97(17) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 109.3(2) . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5A 110.9 . . ? N1 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 109.5 . . ? N2 C6 C5 108.7(2) . . ? N2 C6 H6A 108.3 . . ? C5 C6 H6A 111.0 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 109.4 . . ? N2 C7 C8 123.6(2) . . ? N2 C7 C12 120.1(2) . . ? C8 C7 C12 116.3(2) . . ? C9 C8 C7 121.9(3) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 118.5 . . ? C11 C10 C9 118.2(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 122.5 . . ? C10 C11 C12 121.6(3) . . ? C10 C11 H11 118.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C7 120.5(2) . . ? C11 C12 P1 123.6(2) . . ? C7 C12 P1 115.72(19) . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P1 123.5(2) . . ? C18 C13 P1 118.3(2) . . ? C13 C14 C15 120.7(3) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 120.2 . . ? C17 C18 C13 120.7(3) . . ? C17 C18 H18 120.5 . . ? C13 C18 H18 118.9 . . ? C20 C19 C24 117.4(3) . . ? C20 C19 P1 123.9(2) . . ? C24 C19 P1 118.5(2) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 118.8 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 119.1 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 118.8 . . ? C19 C24 C23 120.9(3) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.302 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.094 data_4047 _database_code_depnum_ccdc_archive 'CCDC 264441' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H28 Al1 N2 P1' _chemical_formula_sum 'C26 H34 Al N2 P' _chemical_formula_weight 432.50 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2620(3) _cell_length_b 29.0657(14) _cell_length_c 9.8432(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.149(3) _cell_angle_gamma 90.00 _cell_volume 2471.35(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 73001 _cell_measurement_theta_min 1.455 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 1.1003 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11346 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3909 _reflns_number_gt 2536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1067P)^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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3909 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.33290(12) 0.11088(3) 0.42557(10) 0.0363(3) Uani 1 1 d . . . Al1 Al 0.13387(14) 0.11681(3) 0.14088(12) 0.0417(4) Uani 1 1 d . . . N1 N 0.1276(4) 0.17718(9) 0.2197(3) 0.0432(8) Uani 1 1 d . . . N2 N -0.0409(5) 0.14473(11) -0.0443(4) 0.0597(10) Uani 1 1 d . . . C1 C 0.5293(4) 0.12603(11) 0.4433(4) 0.0378(9) Uani 1 1 d . . . C2 C 0.6247(5) 0.09193(13) 0.4203(5) 0.0508(11) Uani 1 1 d . . . H2 H 0.5887 0.0607 0.4062 0.061 Uiso 1 1 d R . . C3 C 0.7671(5) 0.10296(15) 0.4161(5) 0.0611(12) Uani 1 1 d . . . H3 H 0.8341 0.0791 0.4059 0.073 Uiso 1 1 d R . . C4 C 0.8177(5) 0.14799(15) 0.4307(5) 0.0613(12) Uani 1 1 d . . . H4 H 0.9154 0.1557 0.4233 0.074 Uiso 1 1 d R . . C5 C 0.7251(5) 0.18154(14) 0.4519(5) 0.0567(12) Uani 1 1 d . . . H5 H 0.7599 0.2129 0.4621 0.068 Uiso 1 1 d R . . C6 C 0.5824(5) 0.17123(12) 0.4587(4) 0.0478(11) Uani 1 1 d . . . H6 H 0.5173 0.1948 0.4743 0.057 Uiso 1 1 d R . . C7 C 0.3544(5) 0.07076(11) 0.5746(4) 0.0410(10) Uani 1 1 d . . . C8 C 0.4925(6) 0.05806(13) 0.6802(4) 0.0541(11) Uani 1 1 d . . . H8 H 0.5857 0.0707 0.6740 0.065 Uiso 1 1 d R . . C9 C 0.4932(7) 0.02704(15) 0.7884(5) 0.0676(14) Uani 1 1 d . . . H9 H 0.5889 0.0178 0.8622 0.081 Uiso 1 1 d R . . C10 C 0.3596(8) 0.00959(14) 0.7934(6) 0.0691(15) Uani 1 1 d . . . H10 H 0.3611 -0.0113 0.8693 0.083 Uiso 1 1 d R . . C11 C 0.2218(7) 0.02196(14) 0.6909(6) 0.0665(14) Uani 1 1 d . . . H11 H 0.1279 0.0097 0.6966 0.080 Uiso 1 1 d R . . C12 C 0.2189(6) 0.05191(13) 0.5821(5) 0.0582(12) Uani 1 1 d . . . H12 H 0.1224 0.0598 0.5070 0.070 Uiso 1 1 d R . . C13 C 0.2569(4) 0.16204(11) 0.4792(4) 0.0334(9) Uani 1 1 d . . . C14 C 0.2841(5) 0.17363(12) 0.6237(4) 0.0462(10) Uani 1 1 d . . . H14 H 0.3444 0.1536 0.7008 0.055 Uiso 1 1 d R . . C15 C 0.2228(5) 0.21361(12) 0.6591(5) 0.0511(11) Uani 1 1 d . . . H15 H 0.2405 0.2207 0.7591 0.061 Uiso 1 1 d R . . C16 C 0.1371(5) 0.24237(12) 0.5472(5) 0.0516(12) Uani 1 1 d . . . H16 H 0.0958 0.2707 0.5682 0.062 Uiso 1 1 d R . . C17 C 0.1086(5) 0.23194(11) 0.4043(5) 0.0465(10) Uani 1 1 d . . . H17 H 0.0514 0.2531 0.3294 0.056 Uiso 1 1 d R . . C18 C 0.1630(4) 0.19035(10) 0.3633(4) 0.0373(9) Uani 1 1 d . . . C19 C 0.0469(6) 0.21153(12) 0.1115(5) 0.0603(12) Uani 1 1 d . . . H19A H -0.0512 0.2177 0.1204 0.072 Uiso 1 1 d R . . H19B H 0.1068 0.2393 0.1285 0.072 Uiso 1 1 d R . . C20 C 0.0172(6) 0.19280(13) -0.0380(5) 0.0696(14) Uani 1 1 d . . . H20A H 0.1123 0.1925 -0.0562 0.084 Uiso 1 1 d R . . H20B H -0.0585 0.2107 -0.1116 0.084 Uiso 1 1 d R . . C21 C -0.1945(6) 0.14403(16) -0.0297(6) 0.0779(15) Uani 1 1 d . . . H21A H -0.2706 0.1571 -0.1152 0.093 Uiso 1 1 d R . . H21B H -0.1905 0.1616 0.0542 0.093 Uiso 1 1 d R . . H21C H -0.2220 0.1128 -0.0185 0.093 Uiso 1 1 d R . . C22 C -0.0515(7) 0.12358(17) -0.1846(5) 0.0869(17) Uani 1 1 d . . . H22A H -0.1324 0.1382 -0.2633 0.104 Uiso 1 1 d R . . H22B H -0.0746 0.0914 -0.1823 0.104 Uiso 1 1 d R . . H22C H 0.0452 0.1271 -0.1988 0.104 Uiso 1 1 d R . . C23 C 0.0191(5) 0.06168(11) 0.1679(5) 0.0487(11) Uani 1 1 d . . . H23A H -0.0126 0.0667 0.2494 0.058 Uiso 1 1 d R . . H23B H -0.0707 0.0573 0.0814 0.058 Uiso 1 1 d R . . C24 C 0.1156(6) 0.01782(13) 0.1964(5) 0.0685(14) Uani 1 1 d . . . H24A H 0.0549 -0.0076 0.2081 0.082 Uiso 1 1 d R . . H24B H 0.2055 0.0214 0.2833 0.082 Uiso 1 1 d R . . H24C H 0.1473 0.0120 0.1153 0.082 Uiso 1 1 d R . . C25 C 0.2981(5) 0.10238(14) 0.0639(5) 0.0569(12) Uani 1 1 d . . . H25A H 0.3671 0.0799 0.1253 0.068 Uiso 1 1 d R . . H25B H 0.2508 0.0902 -0.0326 0.068 Uiso 1 1 d R . . C26 C 0.4074(7) 0.13994(17) 0.0461(6) 0.0836(16) Uani 1 1 d . . . H26A H 0.4800 0.1276 0.0066 0.100 Uiso 1 1 d R . . H26B H 0.4624 0.1531 0.1401 0.100 Uiso 1 1 d R . . H26C H 0.3462 0.1633 -0.0178 0.100 Uiso 1 1 d 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 0.0391(7) 0.0256(5) 0.0468(6) -0.0006(4) 0.0184(5) -0.0005(4) Al1 0.0466(8) 0.0305(6) 0.0499(8) -0.0022(5) 0.0196(7) -0.0019(5) N1 0.054(2) 0.0271(15) 0.048(2) 0.0053(13) 0.0173(18) 0.0042(14) N2 0.068(3) 0.050(2) 0.053(2) -0.0019(16) 0.012(2) 0.0044(18) C1 0.037(3) 0.0343(18) 0.043(2) -0.0041(15) 0.016(2) 0.0013(17) C2 0.049(3) 0.037(2) 0.073(3) -0.0083(19) 0.030(2) -0.0024(19) C3 0.046(3) 0.062(3) 0.083(3) -0.011(2) 0.034(3) 0.004(2) C4 0.049(3) 0.069(3) 0.075(3) 0.001(2) 0.034(3) -0.012(2) C5 0.050(3) 0.046(2) 0.078(3) 0.006(2) 0.027(3) -0.010(2) C6 0.055(3) 0.0303(19) 0.063(3) 0.0010(17) 0.027(2) -0.0010(19) C7 0.051(3) 0.0269(18) 0.049(2) -0.0035(16) 0.023(2) -0.0003(18) C8 0.057(3) 0.049(2) 0.058(3) 0.007(2) 0.023(3) 0.003(2) C9 0.084(4) 0.059(3) 0.061(3) 0.019(2) 0.027(3) 0.023(3) C10 0.113(5) 0.038(2) 0.075(3) 0.012(2) 0.057(4) 0.003(3) C11 0.090(4) 0.046(3) 0.082(4) 0.007(2) 0.053(3) -0.011(3) C12 0.057(3) 0.048(2) 0.074(3) 0.010(2) 0.028(3) -0.002(2) C13 0.030(2) 0.0298(18) 0.042(2) -0.0027(15) 0.0150(19) -0.0034(15) C14 0.057(3) 0.035(2) 0.048(3) 0.0010(17) 0.021(2) -0.0013(18) C15 0.065(3) 0.040(2) 0.060(3) -0.0140(19) 0.036(3) -0.008(2) C16 0.055(3) 0.0271(19) 0.081(3) -0.012(2) 0.035(3) -0.0032(18) C17 0.048(3) 0.0248(18) 0.067(3) -0.0026(17) 0.021(2) 0.0020(17) C18 0.038(3) 0.0238(17) 0.054(3) -0.0002(16) 0.022(2) -0.0020(16) C19 0.071(4) 0.036(2) 0.065(3) 0.007(2) 0.014(3) 0.006(2) C20 0.096(4) 0.044(2) 0.056(3) 0.013(2) 0.011(3) 0.011(2) C21 0.051(4) 0.072(3) 0.089(4) -0.007(3) -0.001(3) 0.012(3) C22 0.121(5) 0.075(3) 0.053(3) -0.005(3) 0.016(3) 0.012(3) C23 0.052(3) 0.034(2) 0.059(3) -0.0095(17) 0.019(2) -0.0072(18) C24 0.087(4) 0.033(2) 0.094(4) -0.008(2) 0.043(3) -0.006(2) C25 0.062(3) 0.065(3) 0.048(3) -0.009(2) 0.024(3) -0.009(2) C26 0.083(4) 0.103(4) 0.079(4) 0.021(3) 0.047(3) -0.007(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 C13 1.804(3) . ? P1 C1 1.818(4) . ? P1 C7 1.827(4) . ? P1 Al1 2.7482(16) . ? Al1 N1 1.928(3) . ? Al1 C25 1.974(4) . ? Al1 C23 1.993(4) . ? Al1 N2 2.115(4) . ? N1 C18 1.385(4) . ? N1 C19 1.454(5) . ? N2 C21 1.481(6) . ? N2 C22 1.482(5) . ? N2 C20 1.490(5) . ? C1 C6 1.392(5) . ? C1 C2 1.400(5) . ? C2 C3 1.373(5) . ? C2 H2 0.9601 . ? C3 C4 1.380(6) . ? C3 H3 0.9600 . ? C4 C5 1.363(6) . ? C4 H4 0.9601 . ? C5 C6 1.380(5) . ? C5 H5 0.9599 . ? C6 H6 0.9600 . ? C7 C8 1.376(6) . ? C7 C12 1.396(5) . ? C8 C9 1.394(5) . ? C8 H8 0.9601 . ? C9 C10 1.354(7) . ? C9 H9 0.9599 . ? C10 C11 1.359(7) . ? C10 H10 0.9598 . ? C11 C12 1.373(6) . ? C11 H11 0.9600 . ? C12 H12 0.9598 . ? C13 C14 1.393(5) . ? C13 C18 1.421(5) . ? C14 C15 1.392(5) . ? C14 H14 0.9599 . ? C15 C16 1.383(6) . ? C15 H15 0.9598 . ? C16 C17 1.369(5) . ? C16 H16 0.9599 . ? C17 C18 1.423(5) . ? C17 H17 0.9599 . ? C19 C20 1.499(6) . ? C19 H19A 0.9599 . ? C19 H19B 0.9598 . ? C20 H20A 0.9599 . ? C20 H20B 0.9598 . ? C21 H21A 0.9597 . ? C21 H21B 0.9599 . ? C21 H21C 0.9599 . ? C22 H22A 0.9599 . ? C22 H22B 0.9601 . ? C22 H22C 0.9600 . ? C23 C24 1.524(5) . ? C23 H23A 0.9599 . ? C23 H23B 0.9598 . ? C24 H24A 0.9600 . ? C24 H24B 0.9598 . ? C24 H24C 0.9599 . ? C25 C26 1.541(6) . ? C25 H25A 0.9598 . ? C25 H25B 0.9597 . ? C26 H26A 0.9600 . ? C26 H26B 0.9598 . ? C26 H26C 0.9598 . ? 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 C13 P1 C1 104.79(15) . . ? C13 P1 C7 103.42(15) . . ? C1 P1 C7 105.18(18) . . ? C13 P1 Al1 93.31(12) . . ? C1 P1 Al1 111.25(12) . . ? C7 P1 Al1 134.20(14) . . ? N1 Al1 C25 119.15(16) . . ? N1 Al1 C23 125.67(15) . . ? C25 Al1 C23 113.73(16) . . ? N1 Al1 N2 82.69(13) . . ? C25 Al1 N2 101.95(18) . . ? C23 Al1 N2 98.30(17) . . ? N1 Al1 P1 75.71(10) . . ? C25 Al1 P1 92.96(14) . . ? C23 Al1 P1 90.43(13) . . ? N2 Al1 P1 157.85(10) . . ? C18 N1 C19 115.3(3) . . ? C18 N1 Al1 129.2(2) . . ? C19 N1 Al1 114.4(2) . . ? C21 N2 C22 110.0(4) . . ? C21 N2 C20 110.7(4) . . ? C22 N2 C20 109.2(3) . . ? C21 N2 Al1 112.0(3) . . ? C22 N2 Al1 114.6(3) . . ? C20 N2 Al1 99.9(3) . . ? C6 C1 C2 117.8(3) . . ? C6 C1 P1 122.8(3) . . ? C2 C1 P1 118.8(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 121.4 . . ? C1 C6 H6 118.1 . . ? C8 C7 C12 117.6(4) . . ? C8 C7 P1 125.5(3) . . ? C12 C7 P1 116.9(3) . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8 117.4 . . ? C9 C8 H8 122.7 . . ? C10 C9 C8 121.2(5) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 121.2 . . ? C11 C12 C7 121.7(5) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 118.1 . . ? C14 C13 C18 120.9(3) . . ? C14 C13 P1 123.5(3) . . ? C18 C13 P1 115.6(2) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 118.3(4) . . ? C16 C15 H15 121.5 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 121.8(3) . . ? C17 C16 H16 117.8 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.5(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 118.8 . . ? N1 C18 C13 120.7(3) . . ? N1 C18 C17 123.1(3) . . ? C13 C18 C17 116.2(3) . . ? N1 C19 C20 109.5(3) . . ? N1 C19 H19A 108.3 . . ? C20 C19 H19A 108.2 . . ? N1 C19 H19B 109.8 . . ? C20 C19 H19B 111.5 . . ? H19A C19 H19B 109.5 . . ? N2 C20 C19 108.5(3) . . ? N2 C20 H20A 108.9 . . ? C19 C20 H20A 109.4 . . ? N2 C20 H20B 108.9 . . ? C19 C20 H20B 111.7 . . ? H20A C20 H20B 109.5 . . ? N2 C21 H21A 109.7 . . ? N2 C21 H21B 109.6 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.1 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.8 . . ? N2 C22 H22B 108.8 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.8 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 Al1 113.0(3) . . ? C24 C23 H23A 108.0 . . ? Al1 C23 H23A 109.1 . . ? C24 C23 H23B 108.5 . . ? Al1 C23 H23B 108.7 . . ? H23A C23 H23B 109.5 . . ? C23 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.2 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Al1 121.5(3) . . ? C26 C25 H25A 103.8 . . ? Al1 C25 H25A 109.5 . . ? C26 C25 H25B 103.5 . . ? Al1 C25 H25B 108.6 . . ? H25A C25 H25B 109.5 . . ? C25 C26 H26A 111.5 . . ? C25 C26 H26B 108.3 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 108.6 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.320 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.101