# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_JU92 #TrackingRef '17320_web_deposit_cif_file_0_YanyanWang_1359536091.JU92.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2.50 H10 Al3 Mg N O17.50 P4' _chemical_formula_weight 563.24 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2208(6) _cell_length_b 14.7180(11) _cell_length_c 14.2654(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.5330(10) _cell_angle_gamma 90.00 _cell_volume 1725.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4292 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 28.35 _exptl_crystal_description rod _exptl_crystal_colour white _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6503 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.00cm _diffrn_reflns_number 12541 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.35 _reflns_number_total 4292 _reflns_number_gt 3199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART Apex 2' _computing_cell_refinement 'Bruker SMART Apex 2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0713P)^2^+1.2518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4292 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.005 _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 0.11920(11) 0.21847(6) 0.90467(6) 0.0178(2) Uani 1 1 d . . . P2 P -0.61704(11) 0.66805(6) 1.23630(6) 0.0163(2) Uani 1 1 d . . . P3 P 0.17811(11) 0.36879(6) 1.57277(6) 0.0159(2) Uani 1 1 d . . . P4 P -0.12133(11) 0.44091(6) 1.21071(6) 0.0160(2) Uani 1 1 d . . . Al1 Al 0.00156(12) 0.36295(7) 1.76052(7) 0.0151(2) Uani 1 1 d . . . Al2 Al -0.04138(13) 0.27215(7) 1.09035(7) 0.0159(2) Uani 1 1 d . . . Al3 Al -0.01374(13) 0.32750(8) 1.38502(7) 0.0183(2) Uani 1 1 d . . . Mg1 Mg -0.44992(15) 0.48791(8) 1.32938(8) 0.0190(3) Uani 1 1 d . . . O1 O 0.0559(3) 0.27766(18) 0.98475(17) 0.0275(6) Uani 1 1 d . . . O2 O 0.0991(5) 0.2726(2) 0.81440(19) 0.0427(9) Uani 1 1 d . . . O3 O 0.0338(5) 0.1299(2) 0.8975(3) 0.0564(11) Uani 1 1 d . . . O4 O 0.2991(4) 0.2046(3) 0.9238(2) 0.0532(11) Uani 1 1 d . . . O5 O -0.5176(4) 0.5832(2) 1.23230(18) 0.0312(7) Uani 1 1 d . . . O6 O -0.5867(4) 0.7194(2) 1.32800(18) 0.0300(6) Uani 1 1 d . . . O7 O -0.5821(4) 0.7301(2) 1.15332(19) 0.0359(7) Uani 1 1 d . . . O8 O -0.7959(3) 0.6455(3) 1.2283(2) 0.0497(10) Uani 1 1 d . . . O9 O 0.0412(3) 0.36230(19) 1.64279(17) 0.0266(6) Uani 1 1 d . . . O10 O 0.0632(4) 0.46305(18) 1.81297(19) 0.0293(6) Uani 1 1 d . . . O11 O 0.2856(3) 0.44895(19) 1.59057(19) 0.0292(6) Uani 1 1 d . . . O12 O 0.0988(3) 0.37615(19) 1.47501(17) 0.0259(6) Uani 1 1 d . . . O13 O 0.2712(4) 0.27906(19) 1.5780(2) 0.0325(7) Uani 1 1 d . . . O14 O -0.0801(3) 0.38318(17) 1.12467(17) 0.0198(5) Uani 1 1 d . . . O15 O -0.0181(3) 0.40591(19) 1.29463(17) 0.0258(6) Uani 1 1 d . . . O16 O -0.2992(3) 0.43812(19) 1.22913(18) 0.0265(6) Uani 1 1 d . . . O17 O -0.6475(4) 0.5283(2) 1.41111(19) 0.0324(7) Uani 1 1 d . . . O18 O -0.6541(7) 0.4002(4) 1.2520(4) 0.0345(14) Uani 0.50 1 d P . . N1 N -0.5607(6) 0.4608(4) 1.0828(3) 0.0568(12) Uani 1 1 d . . . C1 C -0.4432(7) 0.4118(4) 1.0229(4) 0.0490(13) Uani 1 1 d . . . C2 C -0.3340(7) 0.4774(4) 0.9759(4) 0.0575(15) Uani 1 1 d . . . C3 C -0.6648(17) 0.3893(10) 1.1360(11) 0.085(5) Uani 0.50 1 d P . . 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 0.0213(5) 0.0149(5) 0.0173(4) 0.0033(3) 0.0064(3) 0.0053(4) P2 0.0167(4) 0.0168(5) 0.0155(4) 0.0000(3) -0.0002(3) -0.0014(3) P3 0.0195(4) 0.0157(5) 0.0126(4) -0.0005(3) -0.0013(3) 0.0000(3) P4 0.0222(4) 0.0121(4) 0.0138(4) -0.0016(3) 0.0011(3) -0.0004(3) Al1 0.0175(5) 0.0143(5) 0.0136(5) 0.0000(4) 0.0005(4) -0.0002(4) Al2 0.0202(5) 0.0134(5) 0.0141(5) -0.0013(4) 0.0019(4) 0.0008(4) Al3 0.0199(5) 0.0220(6) 0.0128(5) -0.0005(4) -0.0005(4) -0.0030(4) Mg1 0.0224(6) 0.0161(6) 0.0186(6) 0.0017(5) 0.0030(5) 0.0013(5) O1 0.0392(16) 0.0256(15) 0.0184(13) -0.0008(11) 0.0107(11) 0.0101(13) O2 0.082(2) 0.0268(16) 0.0188(14) 0.0034(12) 0.0007(15) 0.0261(17) O3 0.076(3) 0.0154(16) 0.081(3) -0.0101(16) 0.053(2) -0.0072(16) O4 0.0264(16) 0.088(3) 0.045(2) -0.0224(19) -0.0025(14) 0.0239(18) O5 0.0456(17) 0.0250(15) 0.0231(14) 0.0019(12) 0.0032(12) 0.0168(14) O6 0.0379(16) 0.0299(16) 0.0220(14) -0.0050(12) -0.0042(12) -0.0037(13) O7 0.065(2) 0.0205(15) 0.0223(14) 0.0071(11) 0.0016(14) -0.0064(14) O8 0.0177(14) 0.092(3) 0.0396(18) -0.0143(18) 0.0002(13) -0.0106(17) O9 0.0300(14) 0.0339(16) 0.0162(13) 0.0032(11) 0.0056(11) 0.0020(12) O10 0.0503(17) 0.0150(13) 0.0229(14) 0.0005(11) 0.0049(12) -0.0090(13) O11 0.0315(15) 0.0247(15) 0.0310(15) -0.0014(12) -0.0047(12) -0.0088(12) O12 0.0314(14) 0.0328(16) 0.0133(12) -0.0023(11) -0.0045(10) -0.0013(12) O13 0.0317(15) 0.0211(15) 0.0448(18) 0.0038(12) 0.0004(13) 0.0078(12) O14 0.0298(13) 0.0128(12) 0.0170(12) -0.0030(10) 0.0040(10) 0.0032(10) O15 0.0334(14) 0.0272(15) 0.0167(13) 0.0042(11) -0.0025(11) 0.0000(12) O16 0.0238(13) 0.0315(16) 0.0245(14) -0.0042(12) 0.0042(11) 0.0027(12) O17 0.0392(16) 0.0283(16) 0.0303(15) 0.0087(12) 0.0135(13) 0.0067(13) O18 0.034(3) 0.034(3) 0.035(3) -0.006(3) 0.000(2) -0.010(3) N1 0.059(3) 0.069(3) 0.042(3) -0.011(2) -0.004(2) 0.001(3) C1 0.060(3) 0.042(3) 0.045(3) -0.009(2) -0.007(2) 0.019(3) C2 0.058(3) 0.069(4) 0.045(3) -0.011(3) -0.009(3) 0.019(3) C3 0.063(8) 0.084(11) 0.109(12) -0.003(9) 0.010(8) -0.039(8) _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 1.482(3) . ? P1 O4 1.511(3) . ? P1 O2 1.520(3) . ? P1 O1 1.538(3) . ? P2 O5 1.495(3) . ? P2 O8 1.509(3) . ? P2 O6 1.526(3) . ? P2 O7 1.529(3) . ? P3 O11 1.492(3) . ? P3 O12 1.528(3) . ? P3 O13 1.527(3) . ? P3 O9 1.528(3) . ? P4 O16 1.494(3) . ? P4 O10 1.533(3) 3_568 ? P4 O14 1.538(2) . ? P4 O15 1.538(3) . ? Al1 O8 1.707(3) 3_468 ? Al1 O9 1.719(3) . ? Al1 O10 1.722(3) . ? Al1 O2 1.723(3) 1_556 ? Al2 O13 1.720(3) 4_565 ? Al2 O1 1.726(3) . ? Al2 O6 1.733(3) 2_447 ? Al2 O14 1.738(3) . ? Al3 O4 1.715(3) 4_566 ? Al3 O12 1.718(3) . ? Al3 O15 1.730(3) . ? Al3 O7 1.731(3) 2_447 ? Mg1 O11 1.977(3) 3_568 ? Mg1 O3 1.995(3) 4_566 ? Mg1 O5 2.038(3) . ? Mg1 O16 2.052(3) . ? Mg1 O17 2.110(3) . ? Mg1 O18 2.367(6) . ? O2 Al1 1.723(3) 1_554 ? O3 Mg1 1.995(3) 4_665 ? O4 Al3 1.715(3) 4_665 ? O6 Al2 1.733(3) 2_457 ? O7 Al3 1.731(3) 2_457 ? O8 Al1 1.707(3) 3_468 ? O10 P4 1.533(3) 3_568 ? O11 Mg1 1.977(3) 3_568 ? O13 Al2 1.720(3) 4_666 ? O18 C3 1.662(17) . ? N1 C1 1.492(7) . ? N1 C2 1.496(7) 3_467 ? N1 C3 1.567(14) . ? C1 C2 1.490(9) . ? C2 N1 1.496(7) 3_467 ? 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 O4 110.7(2) . . ? O3 P1 O2 111.3(2) . . ? O4 P1 O2 107.9(2) . . ? O3 P1 O1 112.32(17) . . ? O4 P1 O1 106.90(18) . . ? O2 P1 O1 107.51(16) . . ? O5 P2 O8 110.2(2) . . ? O5 P2 O6 111.68(16) . . ? O8 P2 O6 108.10(17) . . ? O5 P2 O7 110.83(17) . . ? O8 P2 O7 106.0(2) . . ? O6 P2 O7 109.77(17) . . ? O11 P3 O12 109.63(16) . . ? O11 P3 O13 112.44(17) . . ? O12 P3 O13 107.86(17) . . ? O11 P3 O9 112.43(16) . . ? O12 P3 O9 107.30(16) . . ? O13 P3 O9 106.94(16) . . ? O16 P4 O10 112.13(17) . 3_568 ? O16 P4 O14 111.27(15) . . ? O10 P4 O14 104.90(15) 3_568 . ? O16 P4 O15 112.12(15) . . ? O10 P4 O15 108.16(16) 3_568 . ? O14 P4 O15 107.90(15) . . ? O8 Al1 O9 107.75(15) 3_468 . ? O8 Al1 O10 107.59(17) 3_468 . ? O9 Al1 O10 111.58(14) . . ? O8 Al1 O2 110.7(2) 3_468 1_556 ? O9 Al1 O2 109.47(14) . 1_556 ? O10 Al1 O2 109.76(16) . 1_556 ? O13 Al2 O1 111.44(15) 4_565 . ? O13 Al2 O6 113.52(15) 4_565 2_447 ? O1 Al2 O6 108.68(14) . 2_447 ? O13 Al2 O14 105.70(14) 4_565 . ? O1 Al2 O14 107.11(13) . . ? O6 Al2 O14 110.17(14) 2_447 . ? O4 Al3 O12 110.07(16) 4_566 . ? O4 Al3 O15 115.07(16) 4_566 . ? O12 Al3 O15 106.19(14) . . ? O4 Al3 O7 107.05(19) 4_566 2_447 ? O12 Al3 O7 109.92(15) . 2_447 ? O15 Al3 O7 108.50(14) . 2_447 ? O11 Mg1 O3 100.42(16) 3_568 4_566 ? O11 Mg1 O5 103.84(13) 3_568 . ? O3 Mg1 O5 155.36(17) 4_566 . ? O11 Mg1 O16 98.89(12) 3_568 . ? O3 Mg1 O16 94.51(13) 4_566 . ? O5 Mg1 O16 86.05(12) . . ? O11 Mg1 O17 94.18(13) 3_568 . ? O3 Mg1 O17 84.99(13) 4_566 . ? O5 Mg1 O17 88.94(12) . . ? O16 Mg1 O17 166.78(13) . . ? O11 Mg1 O18 172.13(18) 3_568 . ? O3 Mg1 O18 72.4(2) 4_566 . ? O5 Mg1 O18 83.15(19) . . ? O16 Mg1 O18 85.06(17) . . ? O17 Mg1 O18 82.20(18) . . ? P1 O1 Al2 142.67(19) . . ? P1 O2 Al1 145.2(2) . 1_554 ? P1 O3 Mg1 139.5(2) . 4_665 ? P1 O4 Al3 149.4(2) . 4_665 ? P2 O5 Mg1 133.54(17) . . ? P2 O6 Al2 151.8(2) . 2_457 ? P2 O7 Al3 146.7(2) . 2_457 ? P2 O8 Al1 167.1(3) . 3_468 ? P3 O9 Al1 143.19(19) . . ? P4 O10 Al1 141.53(18) 3_568 . ? P3 O11 Mg1 149.59(19) . 3_568 ? P3 O12 Al3 149.4(2) . . ? P3 O13 Al2 146.1(2) . 4_666 ? P4 O14 Al2 142.21(17) . . ? P4 O15 Al3 143.48(19) . . ? P4 O16 Mg1 136.47(17) . . ? C3 O18 Mg1 122.4(5) . . ? C1 N1 C2 110.4(4) . 3_467 ? C1 N1 C3 108.8(7) . . ? C2 N1 C3 111.4(7) 3_467 . ? C2 C1 N1 110.6(5) . . ? C1 C2 N1 107.4(5) . 3_467 ? N1 C3 O18 113.7(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.819 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 922472' ####################################################################### # # 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_JU92-300 #TrackingRef '17321_web_deposit_cif_file_1_YanyanWang_1359536091.JU92-300.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2.50 H7 Al3 Mg N O16 P4' _chemical_formula_weight 536.22 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' Mg Mg 0.0486 0.0363 '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 8.4084(5) _cell_length_b 14.4558(9) _cell_length_c 16.3592(8) _cell_angle_alpha 90.00 _cell_angle_beta 120.037(2) _cell_angle_gamma 90.00 _cell_volume 1721.42(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4274 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 28.31 _exptl_crystal_description rod _exptl_crystal_colour white _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8042 _exptl_absorpt_correction_T_max 0.8825 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.0cm _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12471 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4274 _reflns_number_gt 3470 _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 '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^)+(0.0475P)^2^+3.4908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4274 _refine_ls_number_parameters 262 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.85310(11) 0.66451(6) 0.24313(6) 0.01511(18) Uani 1 1 d . . . P2 P 1.21497(11) 0.71085(6) 0.60391(6) 0.01425(17) Uani 1 1 d . . . P3 P 0.70107(12) 0.94568(6) 0.29470(6) 0.01675(18) Uani 1 1 d . . . P4 P 0.59773(12) 0.64195(6) 0.43013(6) 0.01600(18) Uani 1 1 d . . . Al1 Al 0.86474(13) 0.77199(6) 0.41543(7) 0.0145(2) Uani 1 1 d . . . Al2 Al 0.59388(13) 0.82161(7) 0.11784(7) 0.0159(2) Uani 1 1 d . . . Al3 Al 1.22885(13) 0.64492(6) 0.24416(7) 0.0137(2) Uani 1 1 d . . . Mg1 Mg 0.72830(16) 0.49272(8) 0.32343(8) 0.0180(2) Uani 1 1 d . . . O1 O 1.1483(4) 0.62153(17) 0.6217(2) 0.0289(6) Uani 1 1 d . . . O2 O 1.3627(3) 0.69446(19) 0.57710(18) 0.0276(6) Uani 1 1 d . . . O3 O 1.0599(3) 0.76657(18) 0.52366(17) 0.0268(6) Uani 1 1 d . . . O4 O 0.3900(3) 0.64354(19) 0.36261(17) 0.0264(6) Uani 1 1 d . . . O5 O 1.2977(3) 0.77336(17) 0.69143(17) 0.0238(5) Uani 1 1 d . . . O6 O 0.6938(3) 0.71327(17) 0.15887(18) 0.0268(6) Uani 1 1 d . . . O7 O 0.8024(4) 0.56502(17) 0.24614(19) 0.0289(6) Uani 1 1 d . . . O8 O 0.8264(3) 0.88856(16) 0.38356(16) 0.0222(5) Uani 1 1 d . . . O9 O 0.6892(4) 0.56402(18) 0.40990(19) 0.0300(6) Uani 1 1 d . . . O10 O 0.6287(3) 0.63689(19) 0.52985(17) 0.0274(6) Uani 1 1 d . . . O11 O 0.6734(4) 0.73527(18) 0.4195(2) 0.0302(6) Uani 1 1 d . . . O12 O 0.6960(4) 0.89933(18) 0.21001(17) 0.0297(6) Uani 1 1 d . . . O13 O 1.0167(4) 0.6720(2) 0.2287(2) 0.0318(6) Uani 1 1 d . . . O14 O 0.7980(4) 1.03875(17) 0.31025(18) 0.0316(6) Uani 1 1 d . . . O15 O 0.5132(4) 0.9562(2) 0.28160(19) 0.0325(6) Uani 1 1 d . . . O16 O 0.8995(4) 0.71370(19) 0.33416(18) 0.0340(7) Uani 1 1 d . . . N1 N 0.4114(12) 0.9871(6) 0.4416(6) 0.052(2) Uani 0.50 1 d P . . N2 N 0.2350(9) 0.9438(5) 0.4055(4) 0.0757(16) Uani 0.50 1 d P . . C1 C 0.4303(8) 1.0688(4) 0.5166(3) 0.0491(12) Uani 1 1 d U . . C2 C 0.2548(16) 1.0137(8) 0.4775(7) 0.053(2) Uani 0.50 1 d PU . . C3 C 0.385(2) 0.8845(8) 0.4409(9) 0.070(3) Uani 0.50 1 d PU . . C4 C 0.2350(9) 0.9438(5) 0.4055(4) 0.0757(16) Uani 0.50 1 d PU . . 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 0.0154(4) 0.0161(4) 0.0153(4) -0.0002(3) 0.0088(3) 0.0015(3) P2 0.0119(4) 0.0162(4) 0.0121(4) -0.0008(3) 0.0041(3) 0.0023(3) P3 0.0202(4) 0.0135(4) 0.0118(4) 0.0017(3) 0.0045(3) 0.0007(3) P4 0.0173(4) 0.0195(4) 0.0115(4) -0.0014(3) 0.0074(3) -0.0014(3) Al1 0.0146(5) 0.0139(5) 0.0124(4) 0.0011(3) 0.0047(4) 0.0013(4) Al2 0.0152(5) 0.0212(5) 0.0102(4) 0.0018(4) 0.0057(4) 0.0018(4) Al3 0.0130(5) 0.0137(5) 0.0123(4) 0.0002(3) 0.0049(4) -0.0002(3) Mg1 0.0231(6) 0.0156(5) 0.0170(5) -0.0001(4) 0.0113(5) 0.0003(4) O1 0.0269(14) 0.0193(13) 0.0378(15) 0.0055(11) 0.0142(12) 0.0006(10) O2 0.0184(13) 0.0415(16) 0.0252(13) -0.0102(11) 0.0126(11) -0.0017(11) O3 0.0221(13) 0.0290(14) 0.0167(12) 0.0036(10) 0.0003(11) 0.0071(10) O4 0.0207(13) 0.0402(16) 0.0131(12) 0.0027(10) 0.0044(10) -0.0087(11) O5 0.0214(13) 0.0279(14) 0.0176(12) -0.0076(10) 0.0065(10) 0.0042(10) O6 0.0200(13) 0.0223(13) 0.0254(14) 0.0002(10) 0.0017(11) 0.0062(10) O7 0.0407(16) 0.0198(13) 0.0329(15) 0.0009(10) 0.0233(13) -0.0053(11) O8 0.0280(13) 0.0141(11) 0.0155(11) 0.0040(9) 0.0042(10) 0.0020(9) O9 0.0426(17) 0.0267(14) 0.0293(14) -0.0016(11) 0.0245(13) 0.0064(12) O10 0.0220(13) 0.0476(17) 0.0119(11) -0.0016(10) 0.0079(10) 0.0051(11) O11 0.0248(14) 0.0231(14) 0.0432(17) 0.0000(11) 0.0174(13) -0.0050(10) O12 0.0417(16) 0.0276(14) 0.0175(13) -0.0044(10) 0.0131(12) 0.0000(12) O13 0.0200(13) 0.0440(17) 0.0373(16) 0.0063(13) 0.0188(13) 0.0034(11) O14 0.0381(16) 0.0160(13) 0.0245(14) 0.0041(10) 0.0034(12) -0.0051(11) O15 0.0263(14) 0.0430(17) 0.0266(14) 0.0106(12) 0.0119(12) 0.0107(12) O16 0.0494(18) 0.0334(15) 0.0201(13) -0.0058(11) 0.0181(13) 0.0055(13) N1 0.049(5) 0.073(6) 0.045(5) 0.037(4) 0.031(4) 0.032(4) N2 0.071(4) 0.089(4) 0.060(3) 0.015(3) 0.027(3) -0.010(3) C1 0.058(3) 0.059(3) 0.036(2) 0.012(2) 0.028(2) 0.025(2) C2 0.062(6) 0.059(6) 0.033(5) -0.003(4) 0.019(4) 0.011(5) C3 0.098(8) 0.045(6) 0.062(6) 0.013(5) 0.036(6) 0.027(5) C4 0.071(4) 0.089(4) 0.060(3) 0.015(3) 0.027(3) -0.010(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 O7 1.508(3) . ? P1 O13 1.511(3) . ? P1 O16 1.515(3) . ? P1 O6 1.531(3) . ? P2 O1 1.493(3) . ? P2 O2 1.528(2) . ? P2 O5 1.534(2) . ? P2 O3 1.536(2) . ? P2 Mg1 3.1198(14) 3_766 ? P3 O15 1.492(3) . ? P3 O12 1.520(3) . ? P3 O14 1.527(3) . ? P3 O8 1.540(2) . ? P4 O9 1.492(3) . ? P4 O10 1.520(2) . ? P4 O4 1.529(3) . ? P4 O11 1.538(3) . ? Al1 O3 1.710(3) . ? Al1 O16 1.718(3) . ? Al1 O11 1.726(3) . ? Al1 O8 1.746(2) . ? Al2 O10 1.715(2) 4_575 ? Al2 O12 1.725(3) . ? Al2 O2 1.726(3) 4_475 ? Al2 O6 1.745(3) . ? Al3 O13 1.717(3) . ? Al3 O4 1.721(3) 1_655 ? Al3 O5 1.725(2) 4_575 ? Al3 O14 1.731(3) 2_745 ? Mg1 O9 1.907(3) . ? Mg1 O1 1.918(3) 3_766 ? Mg1 O15 1.965(3) 2_645 ? Mg1 O7 1.967(3) . ? Mg1 P2 3.1198(14) 3_766 ? O1 Mg1 1.918(3) 3_766 ? O2 Al2 1.726(3) 4_676 ? O4 Al3 1.721(3) 1_455 ? O5 Al3 1.725(2) 4_576 ? O10 Al2 1.715(2) 4_576 ? O14 Al3 1.731(3) 2_755 ? O15 Mg1 1.965(3) 2_655 ? N1 C1 1.408(9) 3_676 ? N1 N2 1.437(11) . ? N1 C3 1.499(15) . ? N1 C1 1.652(11) . ? N1 C2 1.732(13) . ? N1 N1 1.778(19) 3_676 ? N2 C3 1.387(13) . ? N2 C2 1.496(12) . ? C1 N1 1.408(9) 3_676 ? C1 C3 1.508(16) 3_676 ? C1 C2 1.509(13) . ? C3 C1 1.508(16) 3_676 ? 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 O7 P1 O13 111.60(16) . . ? O7 P1 O16 110.70(16) . . ? O13 P1 O16 108.24(17) . . ? O7 P1 O6 109.53(16) . . ? O13 P1 O6 106.32(16) . . ? O16 P1 O6 110.35(15) . . ? O1 P2 O2 111.11(16) . . ? O1 P2 O5 111.51(15) . . ? O2 P2 O5 107.78(14) . . ? O1 P2 O3 112.27(16) . . ? O2 P2 O3 107.46(15) . . ? O5 P2 O3 106.45(14) . . ? O1 P2 Mg1 27.23(11) . 3_766 ? O2 P2 Mg1 88.39(11) . 3_766 ? O5 P2 Mg1 106.77(11) . 3_766 ? O3 P2 Mg1 136.29(11) . 3_766 ? O15 P3 O12 111.69(16) . . ? O15 P3 O14 111.86(17) . . ? O12 P3 O14 108.02(16) . . ? O15 P3 O8 111.44(15) . . ? O12 P3 O8 108.51(15) . . ? O14 P3 O8 105.02(14) . . ? O9 P4 O10 111.81(15) . . ? O9 P4 O4 112.35(16) . . ? O10 P4 O4 107.24(14) . . ? O9 P4 O11 110.40(16) . . ? O10 P4 O11 107.79(16) . . ? O4 P4 O11 107.00(15) . . ? O3 Al1 O16 109.38(14) . . ? O3 Al1 O11 112.09(14) . . ? O16 Al1 O11 113.67(15) . . ? O3 Al1 O8 106.94(13) . . ? O16 Al1 O8 108.65(13) . . ? O11 Al1 O8 105.79(13) . . ? O10 Al2 O12 106.64(14) 4_575 . ? O10 Al2 O2 110.83(13) 4_575 4_475 ? O12 Al2 O2 113.37(14) . 4_475 ? O10 Al2 O6 112.66(14) 4_575 . ? O12 Al2 O6 108.37(13) . . ? O2 Al2 O6 105.08(13) 4_475 . ? O13 Al3 O4 110.06(14) . 1_655 ? O13 Al3 O5 110.74(13) . 4_575 ? O4 Al3 O5 107.38(13) 1_655 4_575 ? O13 Al3 O14 105.56(15) . 2_745 ? O4 Al3 O14 113.26(14) 1_655 2_745 ? O5 Al3 O14 109.87(14) 4_575 2_745 ? O9 Mg1 O1 111.83(13) . 3_766 ? O9 Mg1 O15 107.91(13) . 2_645 ? O1 Mg1 O15 104.97(13) 3_766 2_645 ? O9 Mg1 O7 114.67(12) . . ? O1 Mg1 O7 119.17(13) 3_766 . ? O15 Mg1 O7 95.83(13) 2_645 . ? O9 Mg1 P2 106.11(9) . 3_766 ? O1 Mg1 P2 20.87(8) 3_766 3_766 ? O15 Mg1 P2 88.50(10) 2_645 3_766 ? O7 Mg1 P2 135.15(9) . 3_766 ? P2 O1 Mg1 131.90(17) . 3_766 ? P2 O2 Al2 146.08(18) . 4_676 ? P2 O3 Al1 150.82(18) . . ? P4 O4 Al3 141.65(17) . 1_455 ? P2 O5 Al3 139.60(17) . 4_576 ? P1 O6 Al2 142.72(17) . . ? P1 O7 Mg1 135.53(17) . . ? P3 O8 Al1 137.41(16) . . ? P4 O9 Mg1 150.72(19) . . ? P4 O10 Al2 151.04(19) . 4_576 ? P4 O11 Al1 136.07(18) . . ? P3 O12 Al2 149.1(2) . . ? P1 O13 Al3 157.0(2) . . ? P3 O14 Al3 140.73(18) . 2_755 ? P3 O15 Mg1 135.18(17) . 2_655 ? P1 O16 Al1 158.6(2) . . ? C1 N1 N2 118.6(8) 3_676 . ? C1 N1 C3 62.4(7) 3_676 . ? N2 N1 C3 56.3(7) . . ? C1 N1 C1 109.5(6) 3_676 . ? N2 N1 C1 108.2(6) . . ? C3 N1 C1 132.1(7) . . ? C1 N1 C2 131.0(6) 3_676 . ? N2 N1 C2 55.4(5) . . ? C3 N1 C2 94.9(8) . . ? C1 N1 C2 52.9(5) . . ? C1 N1 N1 61.2(5) 3_676 3_676 ? N2 N1 N1 132.1(8) . 3_676 ? C3 N1 N1 104.9(8) . 3_676 ? C1 N1 N1 48.3(5) . 3_676 ? C2 N1 N1 87.7(7) . 3_676 ? C3 N2 N1 64.1(7) . . ? C3 N2 C2 111.6(8) . . ? N1 N2 C2 72.4(7) . . ? N1 C1 C3 61.8(6) 3_676 3_676 ? N1 C1 C2 112.8(7) 3_676 . ? C3 C1 C2 174.6(7) 3_676 . ? N1 C1 N1 70.5(6) 3_676 . ? C3 C1 N1 110.9(6) 3_676 . ? C2 C1 N1 66.3(5) . . ? N2 C2 C1 113.0(8) . . ? N2 C2 N1 52.2(5) . . ? C1 C2 N1 60.8(6) . . ? N2 C3 N1 59.6(6) . . ? N2 C3 C1 115.3(9) . 3_676 ? N1 C3 C1 55.8(6) . 3_676 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.768 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 922473'