# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1967 data_yh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H16 Al2 N2 O11 P2' _chemical_formula_weight 372.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 10.001(3) _cell_length_b 6.7120(13) _cell_length_c 18.633(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1250.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour none _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2716 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 23.21 _reflns_number_total 1642 _reflns_number_gt 1523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material '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^)+(0.0431P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.37(13) _refine_ls_number_reflns 1642 _refine_ls_number_parameters 232 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.047 _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 0.52715(9) 0.35466(14) 0.07521(6) 0.0157(2) Uani 1 1 d . . . P2 P 0.66117(9) 1.14870(14) -0.12846(6) 0.0158(2) Uani 1 1 d . . . Al1 Al 0.80165(10) 0.40273(16) -0.00730(7) 0.0175(3) Uani 1 1 d . . . Al2 Al 0.88820(10) 0.90279(16) -0.04647(7) 0.0150(3) Uani 1 1 d . . . O1 O 0.4390(3) 0.5301(4) 0.05371(17) 0.0244(7) Uani 1 1 d . . . O2 O 0.4883(3) 0.1691(4) 0.03153(15) 0.0204(7) Uani 1 1 d . . . O3 O 0.5139(3) 0.3184(4) 0.15512(16) 0.0255(7) Uani 1 1 d . . . O4 O 0.6749(3) 0.4081(4) 0.06044(17) 0.0238(7) Uani 1 1 d . . . O5 O 0.8078(3) 0.6550(5) -0.0469(2) 0.0321(8) Uani 1 1 d D . . O6 O 0.8747(3) 1.1503(4) -0.00502(19) 0.0355(9) Uani 1 1 d D . . O7 O 0.7537(3) 0.9774(4) -0.10863(17) 0.0290(7) Uani 1 1 d . . . O8 O 0.6701(3) 1.1867(4) -0.20838(17) 0.0310(8) Uani 1 1 d . . . O9 O 0.5165(3) 1.0849(5) -0.11302(16) 0.0291(8) Uani 1 1 d . . . O10 O 0.6945(3) 1.3349(4) -0.08504(15) 0.0228(7) Uani 1 1 d . . . O1W O 1.0257(7) 0.3556(10) -0.1564(4) 0.069(2) Uiso 0.60 1 d P . . O1W' O 0.9745(12) 0.3826(16) -0.1013(7) 0.076(3) Uiso 0.40 1 d P . . N1 N 0.7735(5) -0.4866(5) 0.2088(2) 0.0280(9) Uani 1 1 d . . . N2 N 0.5856(5) -0.0054(6) 0.2382(2) 0.0271(9) Uani 1 1 d . . . C1 C 0.6995(5) -0.3240(7) 0.2463(3) 0.0294(10) Uani 1 1 d . . . C2 C 0.6342(5) -0.1787(7) 0.1950(3) 0.0374(12) Uani 1 1 d . . . H2 H 0.5549 -0.2451 0.1754 0.080 Uiso 1 1 calc . . . C3 C 0.7136(6) -0.1091(8) 0.1337(3) 0.0503(16) Uani 1 1 d . . . H1A H 0.795(4) -0.606(7) 0.242(3) 0.029(12) Uiso 1 1 d . . . H1B H 0.732(6) -0.514(8) 0.170(3) 0.050(17) Uiso 1 1 d . . . H1C H 0.860(8) -0.467(13) 0.196(5) 0.13(4) Uiso 1 1 d . . . H1D H 0.636(4) -0.386(6) 0.271(3) 0.034(13) Uiso 1 1 d . . . H1E H 0.763(5) -0.258(8) 0.283(3) 0.048(14) Uiso 1 1 d . . . H2A H 0.648(5) 0.057(8) 0.260(3) 0.041(16) Uiso 1 1 d . . . H2B H 0.510(6) -0.043(8) 0.263(3) 0.058(18) Uiso 1 1 d . . . H2C H 0.554(4) 0.102(7) 0.218(3) 0.029(13) Uiso 1 1 d . . . H3A H 0.741(9) -0.217(12) 0.114(5) 0.13(3) Uiso 1 1 d . . . H3B H 0.666(5) 0.015(9) 0.103(3) 0.061(16) Uiso 1 1 d . . . H3C H 0.813(4) -0.027(7) 0.158(3) 0.034(12) Uiso 1 1 d . . . H5 H 0.758(4) 0.653(7) -0.077(2) 0.031(15) Uiso 1 1 d D . . H6 H 0.926(4) 1.151(7) 0.027(2) 0.031(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0140(5) 0.0147(5) 0.0184(5) 0.0003(5) -0.0034(4) -0.0002(4) P2 0.0145(5) 0.0148(5) 0.0180(6) -0.0006(5) -0.0014(4) 0.0001(4) Al1 0.0178(6) 0.0133(5) 0.0214(7) -0.0004(5) -0.0035(5) -0.0001(5) Al2 0.0144(6) 0.0120(5) 0.0185(7) -0.0001(5) -0.0007(5) 0.0005(4) O1 0.0217(16) 0.0166(14) 0.0350(19) -0.0031(13) -0.0079(14) 0.0001(12) O2 0.0209(16) 0.0151(15) 0.0250(19) 0.0008(12) -0.0076(12) 0.0038(12) O3 0.0297(16) 0.0234(16) 0.0233(17) -0.0003(13) -0.0012(13) -0.0007(13) O4 0.0183(16) 0.0262(16) 0.0268(18) -0.0064(14) -0.0026(13) -0.0025(12) O5 0.0405(19) 0.0240(17) 0.032(2) 0.0101(17) -0.0208(17) -0.0155(13) O6 0.046(2) 0.0209(16) 0.040(2) -0.0117(17) -0.0299(19) 0.0144(13) O7 0.0284(17) 0.0222(14) 0.0364(19) -0.0115(14) -0.0177(15) 0.0091(14) O8 0.0427(18) 0.0257(17) 0.0247(18) 0.0023(15) -0.0010(13) -0.0085(14) O9 0.0186(16) 0.0364(18) 0.032(2) -0.0146(15) 0.0058(14) -0.0081(13) O10 0.0228(15) 0.0196(14) 0.0259(18) -0.0010(12) -0.0062(12) 0.0011(12) N1 0.036(3) 0.0221(19) 0.026(2) -0.0012(19) -0.006(2) 0.0025(18) N2 0.027(2) 0.028(2) 0.026(2) 0.0046(18) 0.0045(18) 0.0076(19) C1 0.037(3) 0.024(2) 0.027(2) 0.004(2) 0.007(2) 0.006(2) C2 0.045(3) 0.033(3) 0.034(3) -0.001(2) 0.007(2) 0.009(2) C3 0.076(4) 0.043(3) 0.032(3) 0.010(2) 0.018(3) 0.032(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 O3 1.515(3) . ? P1 O1 1.524(3) . ? P1 O2 1.538(3) . ? P1 O4 1.546(3) . ? P2 O8 1.514(3) . ? P2 O7 1.522(3) . ? P2 O10 1.526(3) . ? P2 O9 1.536(3) . ? Al1 O4 1.789(3) . ? Al1 O1 1.839(3) 3_565 ? Al1 O6 1.846(3) 1_545 ? Al1 O5 1.848(3) . ? Al1 O10 1.858(3) 1_545 ? Al2 O9 1.787(3) 3_575 ? Al2 O2 1.830(3) 3_565 ? Al2 O6 1.837(3) . ? Al2 O7 1.844(3) . ? Al2 O5 1.848(3) . ? O1 Al1 1.839(3) 3_465 ? O2 Al2 1.830(3) 3_465 ? O5 H5 0.75(3) . ? O6 Al1 1.846(3) 1_565 ? O6 H6 0.78(3) . ? O9 Al2 1.787(3) 3_475 ? O10 Al1 1.858(3) 1_565 ? O1W O1W' 1.161(14) . ? N1 C1 1.493(6) . ? N1 H1A 1.04(5) . ? N1 H1B 0.86(6) . ? N1 H1C 0.91(8) . ? N2 C2 1.496(6) . ? N2 H2A 0.85(5) . ? N2 H2B 0.92(6) . ? N2 H2C 0.87(5) . ? C1 C2 1.514(7) . ? C1 H1D 0.89(5) . ? C1 H1E 1.03(5) . ? C2 C3 1.468(7) . ? C2 H2 0.9800 . ? C3 H3A 0.86(8) . ? C3 H3B 1.12(6) . ? C3 H3C 1.22(5) . ? 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 O3 P1 O1 109.37(17) . . ? O3 P1 O2 111.60(15) . . ? O1 P1 O2 109.89(15) . . ? O3 P1 O4 107.23(16) . . ? O1 P1 O4 109.07(16) . . ? O2 P1 O4 109.61(17) . . ? O8 P2 O7 109.29(19) . . ? O8 P2 O10 111.75(16) . . ? O7 P2 O10 110.94(15) . . ? O8 P2 O9 106.69(18) . . ? O7 P2 O9 108.46(18) . . ? O10 P2 O9 109.57(17) . . ? O4 Al1 O1 95.06(15) . 3_565 ? O4 Al1 O6 106.42(16) . 1_545 ? O1 Al1 O6 85.15(14) 3_565 1_545 ? O4 Al1 O5 106.67(16) . . ? O1 Al1 O5 89.87(14) 3_565 . ? O6 Al1 O5 146.84(19) 1_545 . ? O4 Al1 O10 98.42(13) . 1_545 ? O1 Al1 O10 166.52(15) 3_565 1_545 ? O6 Al1 O10 91.21(14) 1_545 1_545 ? O5 Al1 O10 86.09(14) . 1_545 ? O9 Al2 O2 99.82(13) 3_575 3_565 ? O9 Al2 O6 107.64(16) 3_575 . ? O2 Al2 O6 86.84(14) 3_565 . ? O9 Al2 O7 94.34(15) 3_575 . ? O2 Al2 O7 165.80(16) 3_565 . ? O6 Al2 O7 87.99(14) . . ? O9 Al2 O5 110.56(16) 3_575 . ? O2 Al2 O5 90.25(14) 3_565 . ? O6 Al2 O5 141.63(19) . . ? O7 Al2 O5 85.63(14) . . ? P1 O1 Al1 141.60(18) . 3_465 ? P1 O2 Al2 140.58(17) . 3_465 ? P1 O4 Al1 143.0(2) . . ? Al2 O5 Al1 146.8(2) . . ? Al2 O5 H5 108(4) . . ? Al1 O5 H5 105(4) . . ? Al2 O6 Al1 148.2(2) . 1_565 ? Al2 O6 H6 106(4) . . ? Al1 O6 H6 106(4) 1_565 . ? P2 O7 Al2 143.24(18) . . ? P2 O9 Al2 142.6(2) . 3_475 ? P2 O10 Al1 137.73(18) . 1_565 ? C1 N1 H1A 113(3) . . ? C1 N1 H1B 108(4) . . ? H1A N1 H1B 116(4) . . ? C1 N1 H1C 119(5) . . ? H1A N1 H1C 94(6) . . ? H1B N1 H1C 106(6) . . ? C2 N2 H2A 114(4) . . ? C2 N2 H2B 109(3) . . ? H2A N2 H2B 120(5) . . ? C2 N2 H2C 122(3) . . ? H2A N2 H2C 93(4) . . ? H2B N2 H2C 99(4) . . ? N1 C1 C2 112.9(4) . . ? N1 C1 H1D 105(3) . . ? C2 C1 H1D 108(3) . . ? N1 C1 H1E 109(3) . . ? C2 C1 H1E 114(3) . . ? H1D C1 H1E 108(4) . . ? C3 C2 N2 110.3(4) . . ? C3 C2 C1 117.6(4) . . ? N2 C2 C1 107.5(4) . . ? C3 C2 H2 107.0 . . ? N2 C2 H2 107.0 . . ? C1 C2 H2 107.0 . . ? C2 C3 H3A 104(6) . . ? C2 C3 H3B 114(3) . . ? H3A C3 H3B 122(7) . . ? C2 C3 H3C 107(2) . . ? H3A C3 H3C 106(6) . . ? H3B C3 H3C 101(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O8 1.04(5) 1.71(5) 2.740(5) 175(4) 4_635 N1 H1B O4 0.86(6) 2.18(6) 3.018(5) 166(5) 1_545 N1 H1B O3 0.86(6) 2.47(6) 3.074(5) 129(5) 1_545 N1 H1C O3 0.91(8) 1.98(9) 2.838(5) 156(8) 3 N2 H2A O8 0.85(5) 2.10(6) 2.936(6) 166(5) 4_645 N2 H2B O8 0.92(6) 2.11(6) 3.002(5) 162(5) 2_665 N2 H2B O9 0.92(6) 2.34(6) 3.002(5) 128(4) 2_665 N2 H2C O3 0.87(5) 1.91(5) 2.764(5) 166(4) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.261 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.055