data_global _publ_contact_author_email amonge@icmm.csic.es _publ_contact_author_name 'Mrs Angeles Monge' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_address ; Madrid SPAIN ; _publ_contact_author_phone '34 91 334-9025' _publ_contact_author_fax '34 91 372-0623' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Solvothermal Synthesis and Structural Relations among Three Anionic Aluminophosphates; Catalytic Behaviour ; loop_ _publ_author_name _publ_author_address 'Manuela –Eloisa Medina' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Marta Iglesias' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Enrique Gutierrez Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'M. Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; data_mm23 _database_code_depnum_ccdc_archive 'CCDC 220244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H10 Al2 N2 O10 P2' _chemical_formula_weight 314.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4220(9) _cell_length_b 9.5705(9) _cell_length_c 9.9310(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 895.51(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.736 _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 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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3526 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 28.24 _reflns_number_total 1817 _reflns_number_gt 1630 _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^)+(0.0427P)^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 0.25(17) _refine_ls_number_reflns 1817 _refine_ls_number_parameters 164 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 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 0.57675(10) 0.79162(9) 0.64199(13) 0.0091(2) Uani 1 1 d . . . P2 P 0.58123(10) 0.48533(9) 0.36235(13) 0.0098(2) Uani 1 1 d . . . Al1 Al 0.39788(11) 0.76291(11) 0.35980(16) 0.0092(3) Uani 1 1 d . . . Al2 Al 0.34727(12) 0.97489(11) 0.82312(14) 0.0099(3) Uani 1 1 d . . . O1 O 0.5681(3) 0.6517(3) 0.7150(3) 0.0117(7) Uani 1 1 d . . . O2 O 0.7383(3) 0.5214(3) 0.3373(3) 0.0137(7) Uani 1 1 d . . . O3 O 0.5518(3) 0.4685(3) 0.5116(3) 0.0125(7) Uani 1 1 d . . . O4 O 0.5118(3) 0.7830(3) 0.5011(4) 0.0167(7) Uani 1 1 d . . . O5 O 0.4820(3) 0.5953(3) 0.3009(4) 0.0138(7) Uani 1 1 d . . . O6 O 0.5453(3) 0.3441(3) 0.2925(4) 0.0137(7) Uani 1 1 d . . . O7 O 0.5048(3) 0.9043(3) 0.7254(4) 0.0133(7) Uani 1 1 d . . . O8 O 0.7332(3) 0.8350(3) 0.6228(4) 0.0141(7) Uani 1 1 d . . . O9 O 0.3051(3) 0.9305(3) 0.4057(3) 0.0095(7) Uani 1 1 d D . . H9 H 0.276(10) 0.979(8) 0.488(5) 0.11(3) Uiso 1 1 d D . . O10 O 0.2810(2) 0.8018(2) 0.8606(3) 0.0053(6) Uani 1 1 d D . . H10 H 0.314(8) 0.827(8) 0.948(4) 0.10(3) Uiso 1 1 d D . . O11 O 0.7452(4) 0.0870(4) 0.8152(5) 0.0343(10) Uani 1 1 d . . . N1 N 0.4744(5) 0.1616(4) 0.5070(5) 0.0319(12) Uani 1 1 d D . . H13 H 0.475(8) 0.173(7) 0.596(2) 0.097 Uiso 1 1 d D . . H12 H 0.496(8) 0.071(3) 0.491(7) 0.147 Uiso 1 1 d D . . H11 H 0.539(6) 0.213(7) 0.468(7) 0.128 Uiso 1 1 d D . . H14 H 0.389(4) 0.179(8) 0.477(7) 0.123 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 0.0075(4) 0.0079(4) 0.0119(7) -0.0004(4) 0.0002(5) 0.0002(3) P2 0.0099(4) 0.0073(4) 0.0122(7) -0.0007(4) 0.0005(5) 0.0006(3) Al1 0.0086(5) 0.0076(5) 0.0113(8) 0.0002(5) -0.0007(5) -0.0010(4) Al2 0.0091(5) 0.0084(5) 0.0123(9) 0.0005(5) -0.0004(5) 0.0006(4) O1 0.0128(13) 0.0081(12) 0.014(2) 0.0017(11) 0.0010(13) 0.0013(10) O2 0.0101(13) 0.0160(13) 0.015(2) -0.0043(13) 0.0017(12) -0.0022(10) O3 0.0112(13) 0.0141(12) 0.012(2) -0.0018(12) -0.0007(12) -0.0008(10) O4 0.0191(15) 0.0184(15) 0.013(2) 0.0001(13) -0.0056(14) 0.0021(11) O5 0.0162(13) 0.0094(13) 0.016(2) 0.0011(12) -0.0006(13) 0.0052(10) O6 0.0164(14) 0.0075(12) 0.017(2) -0.0027(11) 0.0035(13) -0.0027(10) O7 0.0126(13) 0.0107(13) 0.017(2) -0.0017(11) 0.0015(13) 0.0018(10) O8 0.0079(12) 0.0098(12) 0.025(2) 0.0007(12) 0.0004(13) 0.0009(10) O9 0.0073(12) 0.0071(12) 0.014(2) -0.0005(11) 0.0018(11) 0.0025(9) O10 0.0071(11) 0.0006(10) 0.008(2) 0.0007(11) 0.0003(12) 0.000 O11 0.0319(18) 0.035(2) 0.036(3) 0.0006(17) -0.0012(19) 0.0005(15) N1 0.040(2) 0.030(2) 0.026(4) 0.005(2) -0.001(2) -0.0147(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O7 1.519(3) . ? P1 O1 1.525(3) . ? P1 O4 1.529(4) . ? P1 O8 1.543(3) . ? P2 O3 1.516(4) . ? P2 O5 1.534(3) . ? P2 O2 1.540(3) . ? P2 O6 1.557(3) . ? Al1 O4 1.777(4) . ? Al1 O6 1.783(4) 3_655 ? Al1 O8 1.821(3) 4_466 ? Al1 O5 1.882(3) . ? Al1 O9 1.883(3) . ? Al2 O10 1.809(3) . ? Al2 O9 1.885(3) 2_575 ? Al2 O2 1.895(3) 4_466 ? Al2 O7 1.898(3) . ? Al2 O3 1.898(4) 3_656 ? Al2 O1 1.909(3) 3_656 ? Al2 H10 1.91(7) . ? O1 Al2 1.909(3) 3_646 ? O2 Al2 1.895(3) 4_566 ? O3 Al2 1.898(4) 3_646 ? O6 Al1 1.783(4) 3_645 ? O8 Al1 1.821(3) 4_566 ? O9 Al2 1.885(3) 2_574 ? O9 H9 0.98(2) . ? O10 H10 0.95(2) . ? N1 H13 0.891(18) . ? N1 H12 0.904(18) . ? N1 H11 0.873(18) . ? N1 H14 0.873(18) . ? 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 O1 109.88(19) . . ? O7 P1 O4 111.00(18) . . ? O1 P1 O4 111.49(17) . . ? O7 P1 O8 107.61(16) . . ? O1 P1 O8 110.26(15) . . ? O4 P1 O8 106.48(19) . . ? O3 P2 O5 110.50(18) . . ? O3 P2 O2 110.97(18) . . ? O5 P2 O2 111.55(16) . . ? O3 P2 O6 107.66(18) . . ? O5 P2 O6 106.62(18) . . ? O2 P2 O6 109.37(16) . . ? O4 Al1 O6 116.19(15) . 3_655 ? O4 Al1 O8 119.70(18) . 4_466 ? O6 Al1 O8 124.10(17) 3_655 4_466 ? O4 Al1 O5 94.79(14) . . ? O6 Al1 O5 88.92(15) 3_655 . ? O8 Al1 O5 87.12(13) 4_466 . ? O4 Al1 O9 89.82(15) . . ? O6 Al1 O9 88.48(14) 3_655 . ? O8 Al1 O9 91.14(12) 4_466 . ? O5 Al1 O9 175.35(17) . . ? O10 Al2 O9 95.02(13) . 2_575 ? O10 Al2 O2 90.17(14) . 4_466 ? O9 Al2 O2 86.78(14) 2_575 4_466 ? O10 Al2 O7 92.80(13) . . ? O9 Al2 O7 171.57(15) 2_575 . ? O2 Al2 O7 90.05(15) 4_466 . ? O10 Al2 O3 88.01(14) . 3_656 ? O9 Al2 O3 91.20(15) 2_575 3_656 ? O2 Al2 O3 177.16(15) 4_466 3_656 ? O7 Al2 O3 92.22(15) . 3_656 ? O10 Al2 O1 175.48(13) . 3_656 ? O9 Al2 O1 88.78(13) 2_575 3_656 ? O2 Al2 O1 92.48(14) 4_466 3_656 ? O7 Al2 O1 83.54(13) . 3_656 ? O3 Al2 O1 89.47(14) 3_656 3_656 ? O10 Al2 H10 29.5(10) . . ? O9 Al2 H10 87(2) 2_575 . ? O2 Al2 H10 118.1(13) 4_466 . ? O7 Al2 H10 101(2) . . ? O3 Al2 H10 59.8(13) 3_656 . ? O1 Al2 H10 148.8(11) 3_656 . ? P1 O1 Al2 131.5(2) . 3_646 ? P2 O2 Al2 131.4(2) . 4_566 ? P2 O3 Al2 138.61(18) . 3_646 ? P1 O4 Al1 165.9(2) . . ? P2 O5 Al1 135.9(2) . . ? P2 O6 Al1 133.72(19) . 3_645 ? P1 O7 Al2 151.70(19) . . ? P1 O8 Al1 131.58(16) . 4_566 ? Al1 O9 Al2 131.11(19) . 2_574 ? Al1 O9 H9 137(5) . . ? Al2 O9 H9 86(6) 2_574 . ? Al2 O10 H10 81(5) . . ? H13 N1 H12 107(3) . . ? H13 N1 H11 111(3) . . ? H12 N1 H11 108(3) . . ? H13 N1 H14 109(3) . . ? H12 N1 H14 109(3) . . ? H11 N1 H14 112(3) . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 0.607 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.101 data_mm30 _database_code_depnum_ccdc_archive 'CCDC 220245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H12 Al2 N3 O12 P3' _chemical_formula_weight 392.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.261(3) _cell_length_b 10.255(2) _cell_length_c 8.8627(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.407(4) _cell_angle_gamma 90.00 _cell_volume 1122.2(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 prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.764 _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 '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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1867 _diffrn_reflns_av_R_equivalents 0.1037 _diffrn_reflns_av_sigmaI/netI 0.1702 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1129 _reflns_number_gt 670 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1129 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.29416(18) 0.62274(18) 0.3437(2) 0.0083(5) Uani 1 1 d . . . P2 P 0.0000 0.4948(3) 0.2500 0.0064(6) Uani 1 2 d S . . Al1 Al 0.16769(19) 0.4215(2) 0.0826(3) 0.0078(5) Uani 1 1 d . . . O1 O 0.2295(4) 0.2699(5) 0.1614(6) 0.0114(13) Uani 1 1 d . . . O2 O -0.0578(4) 0.5857(5) 0.1044(5) 0.0099(12) Uani 1 1 d . . . O3 O 0.2161(4) 0.5748(5) 0.1779(6) 0.0119(12) Uani 1 1 d . . . O4 O 0.0794(4) 0.4051(5) 0.2092(5) 0.0090(11) Uani 1 1 d . . . O5 O 0.2698(4) 0.5563(5) 0.4802(5) 0.0105(12) Uani 1 1 d . . . O6 O 0.4103(4) 0.5946(5) 0.3646(6) 0.0180(14) Uani 1 1 d . . . N2 N 0.5000 0.6179(11) 0.7500 0.024(3) Uani 1 2 d S . . H5 H 0.454(8) 0.564(10) 0.777(12) 0.050 Uiso 1 1 d . . . H6 H 0.559(13) 0.623(13) 0.862(17) 0.13(6) Uiso 1 1 d . . . N1 N 0.3872(7) 0.7021(7) 0.0413(10) 0.0178(18) Uani 1 1 d . . . H1 H 0.358(10) 0.644(11) 0.016(14) 0.050 Uiso 1 1 d . . . H2 H 0.472(9) 0.668(9) 0.057(11) 0.050 Uiso 1 1 d . . . H3 H 0.369(8) 0.752(10) -0.042(12) 0.050 Uiso 1 1 d . . . H4 H 0.373(8) 0.758(10) 0.096(12) 0.050 Uiso 1 1 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 0.0103(11) 0.0073(11) 0.0097(9) -0.0005(8) 0.0063(8) -0.0008(9) P2 0.0042(16) 0.0106(16) 0.0052(13) 0.000 0.0027(12) 0.000 Al1 0.0083(13) 0.0098(13) 0.0056(10) -0.0005(10) 0.0028(9) -0.0007(11) O1 0.018(3) 0.003(3) 0.016(3) 0.006(2) 0.011(3) 0.007(2) O2 0.009(3) 0.008(3) 0.013(3) 0.007(2) 0.005(2) -0.002(2) O3 0.021(3) 0.008(3) 0.011(3) -0.003(2) 0.010(2) -0.001(3) O4 0.000(2) 0.017(3) 0.009(2) 0.000 0.001 0.000 O5 0.014(3) 0.010(3) 0.012(2) 0.000(2) 0.011(2) 0.002(2) O6 0.010(3) 0.021(3) 0.026(3) 0.002(2) 0.010(3) 0.002(3) N2 0.030(7) 0.024(7) 0.021(6) 0.000 0.014(6) 0.000 N1 0.020(5) 0.016(5) 0.022(4) 0.006(3) 0.012(4) 0.003(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 O6 1.510(5) . ? P1 O5 1.522(5) . ? P1 O3 1.537(5) . ? P1 O1 1.539(5) 4 ? P2 O4 1.537(5) 2 ? P2 O4 1.537(5) . ? P2 O2 1.549(5) 2 ? P2 O2 1.549(5) . ? Al1 O2 1.764(5) 5_565 ? Al1 O1 1.777(5) . ? Al1 O3 1.789(5) . ? Al1 O5 1.899(5) 6_565 ? Al1 O4 1.902(5) . ? O1 P1 1.539(5) 4_545 ? O2 Al1 1.764(5) 5_565 ? O5 Al1 1.899(5) 6_566 ? N2 H5 0.92(10) . ? N2 H6 1.02(15) . ? N1 H1 0.70(11) . ? N1 H2 1.14(11) . ? N1 H3 0.86(11) . ? N1 H4 0.82(10) . ? 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 O6 P1 O5 108.6(3) . . ? O6 P1 O3 111.0(3) . . ? O5 P1 O3 110.6(3) . . ? O6 P1 O1 112.2(3) . 4 ? O5 P1 O1 111.2(3) . 4 ? O3 P1 O1 103.1(3) . 4 ? O4 P2 O4 106.5(4) 2 . ? O4 P2 O2 109.7(2) 2 2 ? O4 P2 O2 112.5(2) . 2 ? O4 P2 O2 112.5(2) 2 . ? O4 P2 O2 109.7(2) . . ? O2 P2 O2 106.0(4) 2 . ? O2 Al1 O1 115.9(3) 5_565 . ? O2 Al1 O3 120.7(3) 5_565 . ? O1 Al1 O3 123.3(3) . . ? O2 Al1 O5 92.6(2) 5_565 6_565 ? O1 Al1 O5 89.2(2) . 6_565 ? O3 Al1 O5 85.7(2) . 6_565 ? O2 Al1 O4 94.3(2) 5_565 . ? O1 Al1 O4 89.2(2) . . ? O3 Al1 O4 89.5(2) . . ? O5 Al1 O4 173.0(2) 6_565 . ? P1 O1 Al1 141.9(4) 4_545 . ? P2 O2 Al1 138.2(3) . 5_565 ? P1 O3 Al1 137.1(3) . . ? P2 O4 Al1 135.0(3) . . ? P1 O5 Al1 136.2(3) . 6_566 ? H5 N2 H6 97(9) . . ? H1 N1 H2 101(10) . . ? H1 N1 H3 106(10) . . ? H2 N1 H3 104(8) . . ? H1 N1 H4 124(10) . . ? H2 N1 H4 125(9) . . ? H3 N1 H4 92(9) . . ? _diffrn_measured_fraction_theta_max 0.809 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.809 _refine_diff_density_max 0.730 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.175 data_mm19 _database_code_depnum_ccdc_archive 'CCDC 220246' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H12 Al N3 O8 P2' _chemical_formula_weight 271.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9998(9) _cell_length_b 9.9790(10) _cell_length_c 11.1099(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.645(2) _cell_angle_gamma 90.00 _cell_volume 997.71(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismat _exptl_crystal_colour transparent _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.551 _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 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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3491 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1839 _reflns_number_gt 1155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1839 _refine_ls_number_parameters 175 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.19317(14) 0.54985(12) 0.40696(12) 0.0198(4) Uani 1 1 d . . . P2 P 0.25673(15) 0.14081(12) 0.65843(13) 0.0217(4) Uani 1 1 d . . . Al1 Al 0.13824(16) 0.42756(13) 0.65049(13) 0.0161(4) Uani 1 1 d . . . O1 O 0.2622(4) 0.0456(3) 0.7690(3) 0.0266(9) Uani 1 1 d . . . O2 O 0.0515(4) 0.5471(4) 0.3285(3) 0.0313(10) Uani 1 1 d . . . O3 O 0.1800(4) 0.4307(3) 0.4975(3) 0.0260(10) Uani 1 1 d . . . O4 O 0.3257(4) 0.5237(4) 0.3279(3) 0.0294(10) Uani 1 1 d . . . O5 O 0.1807(4) 0.2691(3) 0.7060(3) 0.0316(10) Uani 1 1 d . . . O6 O 0.2025(4) 0.6793(3) 0.4768(3) 0.0270(9) Uani 1 1 d . . . O7 O 0.4126(5) 0.1751(5) 0.6204(5) 0.0664(17) Uani 1 1 d . . . O8 O 0.1634(6) 0.0795(4) 0.5622(4) 0.0520(14) Uani 1 1 d . . . N1 N 0.4996(7) 0.3137(6) 0.4137(6) 0.0336(14) Uani 1 1 d . . . H11 H 0.445(8) 0.272(7) 0.450(6) 0.05(2) Uiso 1 1 d . . . H12 H 0.451(10) 0.406(9) 0.386(8) 0.09(3) Uiso 1 1 d . . . H13 H 0.499(8) 0.262(7) 0.344(7) 0.06(2) Uiso 1 1 d . . . H14 H 0.586(8) 0.318(6) 0.425(7) 0.04(2) Uiso 1 1 d . . . N3 N 0.0129(6) 0.8375(5) 0.6302(5) 0.0367(13) Uani 1 1 d D . . H31 H 0.080(5) 0.916(4) 0.626(6) 0.038(17) Uiso 1 1 d D . . H32 H -0.088(7) 0.836(11) 0.665(12) 0.18(5) Uiso 1 1 d D . . H33 H 0.073(9) 0.764(6) 0.597(8) 0.11(3) Uiso 1 1 d D . . H34 H -0.054(8) 0.861(9) 0.562(5) 0.10(3) Uiso 1 1 d D . . N2 N 0.2017(7) 0.4171(5) 0.1147(5) 0.0329(14) Uani 1 1 d . . . H21 H 0.242(7) 0.339(7) 0.092(6) 0.046(18) Uiso 1 1 d . . . H22 H 0.100(9) 0.405(6) 0.115(7) 0.06(2) Uiso 1 1 d . . . H23 H 0.208(8) 0.458(6) 0.069(6) 0.04(2) Uiso 1 1 d . . . H24 H 0.245(12) 0.495(11) 0.204(11) 0.15(4) Uiso 1 1 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 0.0200(6) 0.0231(6) 0.0165(8) 0.0018(5) 0.0009(7) 0.0007(5) P2 0.0281(7) 0.0198(6) 0.0173(8) 0.0028(6) 0.0018(7) 0.0053(5) Al1 0.0205(8) 0.0147(7) 0.0130(8) 0.0000(6) -0.0027(7) 0.0002(5) O1 0.032(2) 0.0223(18) 0.025(2) 0.0100(15) 0.002(2) 0.0063(14) O2 0.0199(18) 0.052(2) 0.022(2) -0.0029(18) -0.0018(19) 0.0033(16) O3 0.044(2) 0.0156(17) 0.019(2) -0.0001(14) 0.007(2) 0.0018(14) O4 0.0231(19) 0.042(2) 0.024(2) 0.0027(17) 0.007(2) 0.0029(15) O5 0.057(3) 0.0168(18) 0.021(2) 0.0025(16) -0.001(2) 0.0102(16) O6 0.036(2) 0.0230(18) 0.022(2) -0.0008(16) -0.005(2) 0.0015(15) O7 0.037(2) 0.080(3) 0.083(4) 0.052(3) 0.027(3) 0.019(2) O8 0.097(4) 0.031(2) 0.027(3) -0.002(2) -0.034(3) 0.010(2) N1 0.030(3) 0.040(3) 0.031(3) 0.008(3) 0.006(3) 0.004(2) N3 0.035(3) 0.044(3) 0.031(3) 0.004(3) -0.007(3) 0.000(2) N2 0.042(3) 0.025(3) 0.032(3) 0.002(3) 0.011(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O6 1.509(4) . ? P1 O4 1.512(3) . ? P1 O2 1.537(4) . ? P1 O3 1.563(3) . ? P2 O8 1.484(5) . ? P2 O7 1.509(4) . ? P2 O5 1.547(3) . ? P2 O1 1.554(4) . ? Al1 O1 1.724(4) 2_556 ? Al1 O5 1.738(4) . ? Al1 O2 1.745(4) 3_566 ? Al1 O3 1.745(3) . ? O1 Al1 1.724(4) 2_546 ? O2 Al1 1.745(4) 3_566 ? N1 H11 0.76(7) . ? N1 H12 1.06(10) . ? N1 H13 0.93(8) . ? N1 H14 0.79(7) . ? N3 H31 0.99(2) . ? N3 H32 0.99(2) . ? N3 H33 0.99(2) . ? N3 H34 1.00(2) . ? N2 H21 0.90(7) . ? N2 H22 0.92(8) . ? N2 H23 0.66(6) . ? N2 H24 1.31(13) . ? 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 O6 P1 O4 114.0(2) . . ? O6 P1 O2 110.4(2) . . ? O4 P1 O2 108.8(2) . . ? O6 P1 O3 108.9(2) . . ? O4 P1 O3 108.0(2) . . ? O2 P1 O3 106.4(2) . . ? O8 P2 O7 114.3(3) . . ? O8 P2 O5 109.8(3) . . ? O7 P2 O5 108.9(3) . . ? O8 P2 O1 109.3(2) . . ? O7 P2 O1 109.8(2) . . ? O5 P2 O1 104.24(19) . . ? O1 Al1 O5 109.1(2) 2_556 . ? O1 Al1 O2 109.59(18) 2_556 3_566 ? O5 Al1 O2 107.21(19) . 3_566 ? O1 Al1 O3 112.12(18) 2_556 . ? O5 Al1 O3 108.23(17) . . ? O2 Al1 O3 110.5(2) 3_566 . ? P2 O1 Al1 147.1(2) . 2_546 ? P1 O2 Al1 136.8(2) . 3_566 ? P1 O3 Al1 131.2(2) . . ? P2 O5 Al1 136.7(2) . . ? H11 N1 H12 111(7) . . ? H11 N1 H13 98(6) . . ? H12 N1 H13 104(7) . . ? H11 N1 H14 126(7) . . ? H12 N1 H14 114(7) . . ? H13 N1 H14 99(6) . . ? H31 N3 H32 126(7) . . ? H31 N3 H33 104(6) . . ? H32 N3 H33 130(8) . . ? H31 N3 H34 98(6) . . ? H32 N3 H34 75(8) . . ? H33 N3 H34 103(7) . . ? H21 N2 H22 107(6) . . ? H21 N2 H23 106(7) . . ? H22 N2 H23 101(8) . . ? H21 N2 H24 128(7) . . ? H22 N2 H24 111(6) . . ? H23 N2 H24 101(7) . . ? _diffrn_measured_fraction_theta_max 0.743 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.743 _refine_diff_density_max 0.747 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.140 #===END