# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Ying Wei' ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; 'Bernd Marler' ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; 'Ling Zhang' ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; 'Zhijian Tian' ; Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics Chinese Academy of Sciences, 116023, Dalian P.R. China ; 'Heribert Graetsch' ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; 'Hermann Gies' ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; _publ_contact_author_address ; Institute of Geology, Mineralogy and Geophysics Ruhr-University-Bochum, D-44780, Bochum Germany ; _publ_contact_author_email hermann.gies@rub.de _publ_contact_author_fax '0049 0234 3214433' _publ_contact_author_phone '0049 0234 3223512' #TrackingRef '- RUB-A1.cif' _publ_contact_author_name 'Professor H. Gies' data_RUB-A1 _database_code_depnum_ccdc_archive 'CCDC 884903' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Al3 O16 P4, 2(C6 H11 N2), C H5 N' _chemical_formula_sum 'C13 H27 Al3 N5 O16 P4' _chemical_formula_weight 714 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 1 21/c 1' _symmetry_space_group_name_Hall '-P 2y b c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.991(2) _cell_length_b 16.979(2) _cell_length_c 14.863(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.191(19) _cell_angle_gamma 90.00 _cell_volume 2689.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1594 _cell_measurement_theta_min 2.7777 _cell_measurement_theta_max 42.4613 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.016 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type none _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 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean 8.2495 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47477 _diffrn_reflns_av_R_equivalents 0.174 _diffrn_reflns_av_sigmaI/netI 0.176 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4695 _reflns_number_gt 2238 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4695 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2015 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2300 _refine_ls_wR_factor_gt 0.1811 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _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 0.1668(2) 0.17622(13) 0.78100(17) 0.0126(6) Uani 1 1 d . . . P2 P 0.1799(2) 0.02551(14) 0.11587(16) 0.0137(6) Uani 1 1 d . . . P3 P 0.1700(2) -0.07123(13) 0.77691(18) 0.0161(6) Uani 1 1 d . . . P4 P 0.1756(2) 0.03099(15) 0.44681(18) 0.0185(6) Uani 1 1 d . . . Al1 Al 0.0778(3) 0.05712(16) 0.90262(19) 0.0152(7) Uani 1 1 d . . . Al2 Al 0.1007(2) 0.13747(15) 0.26667(19) 0.0137(7) Uani 1 1 d . . . Al3 Al 0.0781(3) 0.05457(17) 0.62351(19) 0.0186(7) Uani 1 1 d . . . O1 O -0.0648(6) 0.1336(4) 0.2420(5) 0.0290(17) Uani 1 1 d . . . O2 O 0.3028(6) 0.1560(4) 0.8094(5) 0.0281(18) Uani 1 1 d . . . O3 O 0.1574(7) 0.0904(4) 0.1809(4) 0.0285(17) Uani 1 1 d . . . O4 O 0.2963(6) -0.1070(4) 0.8069(5) 0.0311(18) Uani 1 1 d . . . O5 O 0.1655(7) 0.0943(4) 0.3723(5) 0.0328(19) Uani 1 1 d . . . O6 O 0.0808(6) -0.0403(4) 0.1132(5) 0.0234(16) Uani 1 1 d . . . O7 O 0.1578(7) -0.0229(4) 0.6862(5) 0.0310(17) Uani 1 1 d . . . O8 O 0.1003(6) 0.1422(4) 0.6856(4) 0.0222(16) Uani 1 1 d . . . O9 O 0.3033(6) 0.0006(5) 0.4805(6) 0.047(2) Uani 1 1 d . . . O10 O 0.3068(6) -0.0080(4) 0.1438(5) 0.0360(19) Uani 1 1 d . . . O11 O 0.0812(7) -0.0352(4) 0.4053(5) 0.038(2) Uani 1 1 d . . . O12 O 0.1532(7) 0.0626(4) 0.0176(4) 0.0282(18) Uani 1 1 d . . . O13 O 0.0950(6) 0.1478(3) 0.8518(4) 0.0208(16) Uani 1 1 d . . . O14 O 0.1486(6) -0.0150(4) 0.8515(5) 0.0326(18) Uani 1 1 d . . . O15 O 0.1474(6) 0.2655(3) 0.7726(4) 0.0209(16) Uani 1 1 d . . . O16 O 0.1261(9) 0.0700(4) 0.5237(5) 0.051(3) Uani 1 1 d . . . N1 N 0.4498(8) 0.0247(5) 0.8723(6) 0.031(2) Uani 1 1 d . . . H1A H 0.4124 0.0671 0.8426 0.04(3) Uiso 1 1 calc R . . H1B H 0.4021 -0.0175 0.8540 0.06(4) Uiso 1 1 calc R . . H1C H 0.5240 0.0180 0.8594 0.07(5) Uiso 1 1 calc R . . C1 C 0.4678(10) 0.0357(7) 0.9737(7) 0.035(3) Uani 1 1 d . . . H1D H 0.3870 0.0435 0.9877 0.086(10) Uiso 1 1 calc R . . H1E H 0.5184 0.0822 0.9935 0.086(10) Uiso 1 1 calc R . . N21 N 0.5778(11) 0.3235(7) 0.8959(9) 0.070(4) Uani 1 1 d . . . N22 N 0.7620(11) 0.2699(8) 0.9303(10) 0.076(4) Uani 1 1 d . . . C21 C 0.6973(16) 0.3366(9) 0.9247(12) 0.080(5) Uani 1 1 d . . . H21 H 0.7330 0.3861 0.9394 0.086(10) Uiso 1 1 calc R . . C22 C 0.6788(15) 0.2093(9) 0.9027(10) 0.066(4) Uani 1 1 d . . . H22 H 0.6982 0.1562 0.8993 0.086(10) Uiso 1 1 calc R . . C23 C 0.5635(15) 0.2419(9) 0.8816(11) 0.071(5) Uani 1 1 d . . . H23 H 0.4879 0.2151 0.8611 0.086(10) Uiso 1 1 calc R . . C24 C 0.4802(14) 0.3855(10) 0.8687(16) 0.138(10) Uani 1 1 d . . . H24A H 0.3991 0.3613 0.8488 0.086(10) Uiso 1 1 calc R . . H24B H 0.4968 0.4162 0.8187 0.086(10) Uiso 1 1 calc R . . H24C H 0.4816 0.4191 0.9208 0.086(10) Uiso 1 1 calc R . . C25 C 0.8970(18) 0.2659(11) 0.9530(12) 0.090(6) Uani 1 1 d . . . H25A H 0.9256 0.2440 0.9015 0.086(10) Uiso 1 1 calc R . . H25B H 0.9329 0.3180 0.9665 0.086(10) Uiso 1 1 calc R . . C26 C 0.9326(16) 0.2177(12) 1.0305(13) 0.098(6) Uani 1 1 d . . . H26A H 0.9003 0.1656 1.0151 0.086(10) Uiso 1 1 calc R . . H26B H 0.8997 0.2384 1.0797 0.086(10) Uiso 1 1 calc R . . H26C H 1.0225 0.2157 1.0501 0.086(10) Uiso 1 1 calc R . . N31 N 0.4724(9) 0.2105(6) 0.6373(7) 0.047(3) Uani 1 1 d . . . N32 N 0.6644(9) 0.1702(6) 0.6765(7) 0.038(2) Uani 1 1 d . . . C31 C 0.2911(17) 0.2581(9) 0.5291(12) 0.098(6) Uani 1 1 d . . . H31A H 0.2202 0.2929 0.5191 0.086(10) Uiso 1 1 calc R . . H31B H 0.2624 0.2048 0.5172 0.086(10) Uiso 1 1 calc R . . H31C H 0.3425 0.2720 0.4878 0.086(10) Uiso 1 1 calc R . . C32 C 0.3599(13) 0.2646(10) 0.6190(10) 0.069(4) Uani 1 1 d . . . H32A H 0.3074 0.2514 0.6607 0.086(10) Uiso 1 1 calc R . . H32B H 0.3879 0.3186 0.6312 0.086(10) Uiso 1 1 calc R . . C33 C 0.4718(13) 0.1296(8) 0.6318(10) 0.063(4) Uani 1 1 d . . . H33 H 0.4013 0.0975 0.6139 0.086(10) Uiso 1 1 calc R . . C34 C 0.5891(14) 0.1059(7) 0.6564(10) 0.058(4) Uani 1 1 d . . . H34 H 0.6161 0.0538 0.6594 0.086(10) Uiso 1 1 calc R . . C35 C 0.5892(11) 0.2317(7) 0.6620(9) 0.045(3) Uani 1 1 d . . . H35 H 0.6164 0.2838 0.6685 0.086(10) Uiso 1 1 calc R . . C36 C 0.8004(11) 0.1729(9) 0.7097(10) 0.059(4) Uani 1 1 d . . . H36A H 0.8275 0.2268 0.7169 0.086(10) Uiso 1 1 calc R . . H36B H 0.8381 0.1473 0.6657 0.086(10) Uiso 1 1 calc R . . H36C H 0.8253 0.1465 0.7685 0.086(10) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0146(13) 0.0095(12) 0.0145(13) -0.0017(11) 0.0050(10) -0.0006(10) P2 0.0162(13) 0.0142(13) 0.0106(13) 0.0005(10) 0.0032(10) -0.0003(10) P3 0.0190(13) 0.0103(13) 0.0198(14) 0.0012(11) 0.0064(11) 0.0017(10) P4 0.0236(15) 0.0171(14) 0.0161(14) 0.0021(11) 0.0075(11) -0.0025(11) Al1 0.0222(16) 0.0134(15) 0.0116(15) -0.0028(12) 0.0072(12) -0.0046(12) Al2 0.0193(16) 0.0099(14) 0.0121(15) 0.0001(12) 0.0042(13) -0.0023(12) Al3 0.0304(17) 0.0149(15) 0.0117(15) -0.0019(13) 0.0075(13) -0.0039(13) O1 0.030(4) 0.022(4) 0.035(5) 0.001(3) 0.007(3) -0.005(3) O2 0.028(4) 0.025(4) 0.033(4) -0.003(3) 0.011(3) 0.006(3) O3 0.040(4) 0.036(4) 0.014(4) -0.009(3) 0.015(3) -0.002(4) O4 0.031(4) 0.022(4) 0.044(5) -0.002(3) 0.015(4) 0.003(3) O5 0.053(5) 0.026(4) 0.017(4) 0.003(3) 0.005(4) -0.001(4) O6 0.020(4) 0.017(4) 0.035(4) 0.001(3) 0.012(3) -0.002(3) O7 0.035(4) 0.030(4) 0.027(4) 0.003(3) 0.006(3) 0.004(3) O8 0.032(4) 0.012(3) 0.021(4) -0.004(3) 0.004(3) -0.002(3) O9 0.021(4) 0.052(5) 0.064(6) 0.018(5) 0.001(4) 0.006(4) O10 0.021(4) 0.044(5) 0.045(5) -0.001(4) 0.014(4) 0.005(3) O11 0.037(5) 0.024(4) 0.047(5) -0.006(4) -0.002(4) -0.011(3) O12 0.048(5) 0.029(4) 0.008(4) 0.002(3) 0.008(3) -0.007(3) O13 0.029(4) 0.016(4) 0.022(4) 0.002(3) 0.015(3) 0.000(3) O14 0.039(5) 0.032(4) 0.030(4) -0.019(4) 0.015(4) 0.002(3) O15 0.023(4) 0.011(3) 0.029(4) 0.003(3) 0.006(3) 0.002(3) O16 0.108(8) 0.032(5) 0.029(5) 0.000(4) 0.049(5) -0.007(4) N1 0.014(5) 0.028(5) 0.051(6) -0.001(5) 0.009(4) 0.000(4) C1 0.023(6) 0.052(8) 0.030(7) 0.006(6) 0.004(5) 0.009(5) N21 0.052(8) 0.062(8) 0.107(11) -0.038(7) 0.041(7) -0.030(7) N22 0.031(7) 0.071(9) 0.130(12) -0.057(8) 0.027(7) -0.012(6) C21 0.067(11) 0.043(10) 0.139(16) -0.041(10) 0.043(11) -0.022(8) C22 0.058(10) 0.056(10) 0.084(12) -0.014(8) 0.018(9) -0.026(8) C23 0.063(11) 0.069(11) 0.092(12) -0.030(9) 0.041(9) -0.038(9) C24 0.042(10) 0.091(15) 0.29(3) -0.091(16) 0.047(14) 0.015(9) C25 0.106(16) 0.095(14) 0.072(12) 0.011(11) 0.030(11) 0.015(11) C26 0.071(12) 0.122(17) 0.098(15) -0.041(13) 0.013(11) 0.012(11) N31 0.040(7) 0.027(6) 0.066(8) 0.008(5) -0.003(5) -0.002(5) N32 0.032(6) 0.034(6) 0.045(6) -0.010(5) 0.006(5) 0.000(5) C31 0.104(14) 0.058(11) 0.098(15) 0.020(10) -0.038(11) 0.017(10) C32 0.056(10) 0.093(12) 0.059(10) -0.003(9) 0.018(8) 0.019(9) C33 0.038(9) 0.051(9) 0.088(12) 0.010(8) -0.007(8) -0.020(7) C34 0.071(11) 0.018(7) 0.079(11) -0.003(7) 0.007(8) -0.006(6) C35 0.034(7) 0.030(7) 0.066(9) 0.021(6) 0.004(7) 0.002(6) C36 0.030(8) 0.069(10) 0.079(11) -0.012(8) 0.018(7) -0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.491(7) . ? P1 O15 1.531(6) . ? P1 O13 1.539(6) . ? P1 O8 1.540(7) . ? P2 O10 1.469(7) . ? P2 O3 1.525(7) . ? P2 O12 1.551(6) . ? P2 O6 1.554(6) . ? P3 O4 1.480(7) . ? P3 O14 1.524(7) . ? P3 O1 1.542(7) 3_556 ? P3 O7 1.557(7) . ? P4 O9 1.464(7) . ? P4 O5 1.528(7) . ? P4 O16 1.532(7) . ? P4 O11 1.551(7) . ? Al1 O12 1.709(7) 1_556 ? Al1 O14 1.724(7) . ? Al1 O6 1.725(7) 3_556 ? Al1 O13 1.746(6) . ? Al2 O5 1.721(7) . ? Al2 O15 1.722(6) 4_565 ? Al2 O3 1.744(7) . ? Al2 O1 1.767(7) . ? Al3 O16 1.711(7) . ? Al3 O7 1.721(7) . ? Al3 O11 1.729(7) 3_556 ? Al3 O8 1.736(7) . ? O1 P3 1.542(7) 3_556 ? O6 Al1 1.725(7) 3_556 ? O11 Al3 1.729(7) 3_556 ? O12 Al1 1.709(7) 1_554 ? O15 Al2 1.722(6) 4_566 ? N1 C1 1.483(13) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 C1 1.52(2) 3_657 ? C1 H1D 0.9700 . ? C1 H1E 0.9700 . ? N21 C21 1.297(17) . ? N21 C23 1.404(17) . ? N21 C24 1.49(2) . ? N22 C21 1.328(18) . ? N22 C22 1.372(16) . ? N22 C25 1.44(2) . ? C21 H21 0.9300 . ? C22 C23 1.35(2) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.39(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9599 . ? C26 H26B 0.9599 . ? C26 H26C 0.9599 . ? N31 C35 1.297(14) . ? N31 C33 1.376(16) . ? N31 C32 1.511(16) . ? N32 C35 1.317(14) . ? N32 C34 1.358(15) . ? N32 C36 1.456(14) . ? C31 C32 1.369(17) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.314(17) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9599 . ? C36 H36B 0.9599 . ? C36 H36C 0.9599 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 O15 111.1(4) . . ? O2 P1 O13 112.4(4) . . ? O15 P1 O13 106.4(4) . . ? O2 P1 O8 113.0(4) . . ? O15 P1 O8 105.8(4) . . ? O13 P1 O8 107.7(4) . . ? O10 P2 O3 113.0(4) . . ? O10 P2 O12 111.8(4) . . ? O3 P2 O12 106.3(4) . . ? O10 P2 O6 109.8(4) . . ? O3 P2 O6 108.3(4) . . ? O12 P2 O6 107.4(4) . . ? O4 P3 O14 109.8(4) . . ? O4 P3 O1 112.3(4) . 3_556 ? O14 P3 O1 108.7(4) . 3_556 ? O4 P3 O7 110.6(4) . . ? O14 P3 O7 107.7(4) . . ? O1 P3 O7 107.6(4) 3_556 . ? O9 P4 O5 112.9(4) . . ? O9 P4 O16 112.6(5) . . ? O5 P4 O16 105.1(4) . . ? O9 P4 O11 111.8(5) . . ? O5 P4 O11 107.4(4) . . ? O16 P4 O11 106.6(4) . . ? O12 Al1 O14 108.6(4) 1_556 . ? O12 Al1 O6 111.8(3) 1_556 3_556 ? O14 Al1 O6 111.9(4) . 3_556 ? O12 Al1 O13 107.9(3) 1_556 . ? O14 Al1 O13 109.1(3) . . ? O6 Al1 O13 107.5(3) 3_556 . ? O5 Al2 O15 108.0(3) . 4_565 ? O5 Al2 O3 109.3(4) . . ? O15 Al2 O3 108.7(3) 4_565 . ? O5 Al2 O1 110.4(4) . . ? O15 Al2 O1 109.0(3) 4_565 . ? O3 Al2 O1 111.4(4) . . ? O16 Al3 O7 111.2(4) . . ? O16 Al3 O11 108.8(4) . 3_556 ? O7 Al3 O11 109.8(4) . 3_556 ? O16 Al3 O8 107.2(4) . . ? O7 Al3 O8 112.4(3) . . ? O11 Al3 O8 107.2(3) 3_556 . ? P3 O1 Al2 138.7(5) 3_556 . ? P2 O3 Al2 159.5(5) . . ? P4 O5 Al2 154.3(5) . . ? P2 O6 Al1 143.3(4) . 3_556 ? P3 O7 Al3 142.8(5) . . ? P1 O8 Al3 141.7(4) . . ? P4 O11 Al3 140.7(5) . 3_556 ? P2 O12 Al1 148.5(5) . 1_554 ? P1 O13 Al1 134.5(4) . . ? P3 O14 Al1 158.8(5) . . ? P1 O15 Al2 170.1(4) . 4_566 ? P4 O16 Al3 145.2(5) . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 C1 110.7(11) . 3_657 ? N1 C1 H1D 109.5 . . ? C1 C1 H1D 109.5 3_657 . ? N1 C1 H1E 109.5 . . ? C1 C1 H1E 109.5 3_657 . ? H1D C1 H1E 108.1 . . ? C21 N21 C23 106.7(13) . . ? C21 N21 C24 124.9(13) . . ? C23 N21 C24 127.6(13) . . ? C21 N22 C22 108.3(13) . . ? C21 N22 C25 124.1(13) . . ? C22 N22 C25 127.4(14) . . ? N21 C21 N22 110.9(12) . . ? N21 C21 H21 124.5 . . ? N22 C21 H21 124.5 . . ? C23 C22 N22 106.3(14) . . ? C23 C22 H22 126.8 . . ? N22 C22 H22 126.8 . . ? C22 C23 N21 107.8(13) . . ? C22 C23 H23 126.1 . . ? N21 C23 H23 126.1 . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N22 106.7(15) . . ? C26 C25 H25A 110.4 . . ? N22 C25 H25A 110.4 . . ? C26 C25 H25B 110.4 . . ? N22 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C35 N31 C33 106.5(10) . . ? C35 N31 C32 126.3(11) . . ? C33 N31 C32 127.2(11) . . ? C35 N32 C34 106.2(10) . . ? C35 N32 C36 125.5(10) . . ? C34 N32 C36 128.3(11) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C31 C32 N31 111.0(13) . . ? C31 C32 H32A 109.4 . . ? N31 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? N31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 N31 107.4(11) . . ? C34 C33 H33 126.3 . . ? N31 C33 H33 126.3 . . ? C33 C34 N32 108.6(11) . . ? C33 C34 H34 125.7 . . ? N32 C34 H34 125.7 . . ? N31 C35 N32 111.3(11) . . ? N31 C35 H35 124.4 . . ? N32 C35 H35 124.4 . . ? N32 C36 H36A 109.5 . . ? N32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.556 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.117 # Attachment '- RUB-A2.cif' data_RUB-A2 _database_code_depnum_ccdc_archive 'CCDC 884904' #TrackingRef '- RUB-A2.cif' # start Validation Reply Form _vrf_PLAT075_global ; PROBLEM: Occupancy 1. greater than 1.0 for ...... C1 RESPONSE: To include the scattering power of the hydrogen atoms which could not be located, the occupancy factor of the carbon, nitrogen and oxygen atoms was increased by a factor largeer than 1.0 ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C12 H32 Al3 N4 O17 P4' _chemical_formula_weight 711 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source al 6.42020 3.03870 1.90020 0.74260 1.59360 31.54720 1.96460 85.08860 1.11510 0.20400 0.24600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 p 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x,-y,-z _cell_length_a 12.9165(2) _cell_length_b 13.0460(2) _cell_length_c 9.8873(2) _cell_angle_alpha 70.585(1) _cell_angle_beta 99.547(2) _cell_angle_gamma 119.438(2) _cell_volume 1368.46(4) _cell_formula_units_Z 2 _cell_measurement_temperature 297 _cell_special_details ? _pd_spec_mounting ; glass capillary with 0.3mm diameter ; _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_char_particle_morphology plate _pd_char_colour white _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature 297 _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ; No correction is applied. ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_special_details ? _pd_instr_location ? _pd_calibration_special_details # description of the method used # to calibrate the instrument ? _diffrn_ambient_temperature 297 _diffrn_source 'sealed X-ray tube' _diffrn_radiation_type 'Cu K\a1' _diffrn_source_target ? # Put here the chemical symbol of the anode _diffrn_radiation_wavelength 1.540600 _diffrn_radiation_monochromator germanium _diffrn_measurement_device_type 'Siemens D5000 powder diffractometer' _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step _pd_meas_special_details ? _pd_meas_number_of_points 11133 _pd_meas_2theta_range_min 7.05400 _pd_meas_2theta_range_max 94.99680 _pd_meas_2theta_range_inc 0.007903 _refine_special_details ? _pd_proc_ls_special_details ? _pd_proc_ls_profile_function ; Thompson--Cox--Hastings pseudo-Voigt Axial divergence asymmetry ; _pd_proc_ls_background_function ; Linear Interpolation of background points ; _pd_proc_ls_prof_R_factor 1.9097 _pd_proc_ls_prof_wR_factor 2.5357 _pd_proc_ls_prof_wR_expected 1.6656 _pd_proc_ls_prof_cR_factor 7.0796 _pd_proc_ls_prof_cwR_factor 7.2602 _pd_proc_ls_prof_cwR_expected 4.7689 _pd_proc_ls_prof_chi2 2.3178 _pd_proc_ls_prof_echi2 2.3178 _refine_ls_R_I_factor 2.3784 _refine_ls_number_reflns 2674 _refine_ls_number_parameters 145 _refine_ls_number_restraints 121 _refine_ls_goodness_of_fit_all 1.522 _refine_ls_hydrogen_treatment noref _refine_diff_density_max 0.116 _refine_diff_density_min -0.115 _pd_proc_2theta_range_min 7.0856 _pd_proc_2theta_range_max 95.0284 _pd_proc_2theta_range_inc 0.007903 _pd_proc_wavelength 1.540600 _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction FULLPROF loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Al1 0.145(1) 0.969(1) 0.520(1) 0.0222(8) 1.00000 Uiso Al P1 0.341(1) 0.899(1) 0.656(1) 0.0222(8) 1.00000 Uiso P P2 0.325(1) 0.207(1) 0.305(1) 0.0222(8) 1.00000 Uiso P Al2 0.669(1) 0.650(1) 0.505(1) 0.0222(8) 1.00000 Uiso Al Al3 0.521(1) 0.165(1) 0.509(1) 0.0222(8) 1.00000 Uiso Al P3 0.091(1) 0.131(1) 0.647(1) 0.0222(8) 1.00000 Uiso P P4 0.568(1) 0.360(1) 0.640(1) 0.0222(8) 1.00000 Uiso P O1 0.778(2) -0.084(2) 0.625(2) 0.031(2) 1.00000 Uiso O O2 0.872(2) -0.039(2) 0.371(2) 0.031(2) 1.00000 Uiso O O3 0.989(2) 0.124(2) 0.534(2) 0.031(2) 1.00000 Uiso O O4 0.781(2) 0.112(2) 0.402(3) 0.031(2) 1.00000 Uiso O O5 0.565(2) 0.669(2) 0.380(2) 0.031(2) 1.00000 Uiso O O6 0.633(2) 0.499(2) 0.546(2) 0.031(2) 1.00000 Uiso O O7 0.680(2) 0.693(2) 0.649(2) 0.031(2) 1.00000 Uiso O O8 0.803(2) 0.735(2) 0.417(3) 0.031(2) 1.00000 Uiso O O9 0.441(2) 0.199(2) 0.361(2) 0.031(2) 1.00000 Uiso O O10 0.620(2) 0.145(2) 0.444(3) 0.031(2) 1.00000 Uiso O O11 0.594(2) 0.285(2) 0.574(3) 0.031(2) 1.00000 Uiso O O12 0.424(2) 0.039(2) 0.636(2) 0.031(2) 1.00000 Uiso O O13 0.665(2) 0.172(2) 0.192(2) 0.031(2) 1.00000 Uiso O O14 0.601(2) 0.338(2) -0.204(2) 0.031(2) 1.00000 Uiso O O15 0.322(3) 0.232(2) 0.141(2) 0.031(2) 1.00000 Uiso O O16 0.936(2) -0.107(2) 0.200(2) 0.031(2) 1.00000 Uiso O C1 -0.121(3) 0.485(5) 0.598(5) 0.39(2) 1.33333 Uiso C C2 0.049(3) 0.444(5) 0.289(4) 0.39(2) 1.33333 Uiso C N1 -0.062(3) 0.374(4) 0.366(4) 0.39(2) 1.28571 Uiso N C3 0.052(4) 0.559(2) 0.459(8) 0.39(2) 1.33333 Uiso C C4 0.384(3) 0.078(2) -0.012(3) 0.136(8) 1.33333 Uiso C C5 0.338(3) -0.018(2) 0.136(2) 0.136(8) 1.33333 Uiso C N2 0.097(3) 0.146(3) 0.040(4) 0.136(8) 1.28571 Uiso N C6 -0.065(3) 0.7850(4) -0.100(3) 0.136(8) 1.33333 Uiso C C7 0.122(2) 0.855(3) 0.066(5) 0.136(8) 1.33333 Uiso C C8 0.250(2) 0.861(3) 0.103(4) 0.136(8) 1.33333 Uiso C N3 0.522(2) 0.813(2) 0.972(3) 0.136(8) 1.28571 Uiso N C9 0.024(3) 0.752(3) 0.003(4) 0.136(8) 1.33333 Uiso C N4 0.377(3) 0.451(5) 0.890(3) 0.118(5) 0.50000 Uiso N N5 0.528(5) 0.51(1) 1.033(5) 0.12(1) 0.50000 Uiso N C10 0.286(4) 0.460(4) 0.787(5) 0.12(1) 0.66667 Uiso C C11 0.291(5) 0.575(4) 0.793(5) 0.12(1) 0.75000 Uiso C C12 0.471(4) 0.47(1) 0.824(5) 0.12(1) 0.58333 Uiso C C13 0.579(5) 0.49(1) 1.006(8) 0.12(1) 0.58333 Uiso C C14 0.412(5) 0.500(8) 0.827(4) 0.12(1) 0.75000 Uiso C C15 0.436(5) 0.51(1) 1.071(8) 0.12(1) 0.58333 Uiso C OW 0.208(2) 0.609(2) 0.003(3) 0.15(1) 1.25000 Uiso O _geom_special_details ? 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 Al1 O1 1.69(2) 2_666 ? Al1 O2 1.73(4) 2_666 ? Al1 O3 1.68(2) 2_666 ? Al1 O4 1.69(3) 2_666 ? P1 O4 1.55(3) 2_666 ? P1 O10 1.54(4) 2_666 ? P1 O12 1.56(2) 1_565 ? P1 O13 1.47(2) 2_666 ? P2 O1 1.52(2) 2_656 ? P2 O7 1.54(4) 2_666 ? P2 O9 1.55(3) . ? P2 O15 1.54(2) . ? Al2 O5 1.72(2) . ? Al2 O6 1.70(2) . ? Al2 O7 1.65(3) . ? Al2 O8 1.72(2) . ? Al3 O9 1.72(3) . ? Al3 O10 1.69(4) . ? Al3 O11 1.66(3) . ? Al3 O12 1.72(2) . ? P3 O2 1.56(4) 2_656 ? P3 O3 1.56(2) 1_455 ? P3 O8 1.60(2) 2_666 ? P3 O16 1.50(3) 2_656 ? P4 O5 1.56(2) 2_666 ? P4 O6 1.58(2) . ? P4 O11 1.52(4) . ? P4 O14 1.51(2) 1_556 ? 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 O1 Al1 O2 106(2) 5_666 6_666 ? O1 Al1 O3 109(2) 5_666 7_666 ? O1 Al1 O4 109(2) 5_666 8_666 ? O2 Al1 O3 109(2) 6_666 7_666 ? O2 Al1 O4 114(3) 6_666 8_666 ? O3 Al1 O4 109(2) 7_666 8_666 ? O4 P1 O10 104(3) 4_666 5_666 ? O4 P1 O12 105(2) 4_666 6_565 ? O4 P1 O13 112(2) 4_666 7_666 ? O10 P1 O12 110(3) 5_666 6_565 ? O10 P1 O13 114(3) 5_666 7_666 ? O12 P1 O13 111(2) 6_565 7_666 ? O1 P2 O7 108(3) 4_656 5_666 ? O1 P2 O9 107(2) 4_656 6_555 ? O1 P2 O15 111(2) 4_656 7_555 ? O7 P2 O9 110(3) 5_666 6_555 ? O7 P2 O15 114(3) 5_666 7_555 ? O9 P2 O15 107(2) 6_555 7_555 ? O5 Al2 O6 105(2) 5_555 6_555 ? O5 Al2 O7 116(2) 5_555 7_555 ? O5 Al2 O8 106(2) 5_555 8_555 ? O6 Al2 O7 113(3) 6_555 7_555 ? O6 Al2 O8 107(2) 6_555 8_555 ? O7 Al2 O8 110(3) 7_555 8_555 ? O9 Al3 O10 104(3) 5_555 6_555 ? O9 Al3 O11 110(2) 5_555 7_555 ? O9 Al3 O12 108(2) 5_555 8_555 ? O10 Al3 O11 109(3) 6_555 7_555 ? O10 Al3 O12 116(2) 6_555 8_555 ? O11 Al3 O12 110(2) 7_555 8_555 ? O2 P3 O3 104(3) 4_656 5_455 ? O2 P3 O8 106(2) 4_656 6_666 ? O2 P3 O16 112(3) 4_656 7_656 ? O3 P3 O8 104(2) 5_455 6_666 ? O3 P3 O16 118(2) 5_455 7_656 ? O8 P3 O16 112(2) 6_666 7_656 ? O5 P4 O6 102(2) 4_666 5_555 ? O5 P4 O11 112(3) 4_666 6_555 ? O5 P4 O14 110(2) 4_666 7_556 ? O6 P4 O11 108(2) 5_555 6_555 ? O6 P4 O14 115(2) 5_555 7_556 ? O11 P4 O14 111(3) 6_555 7_556 ?