Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_UiO-28-as_C _journal_coden_Cambridge 1145 _publ_contact_author_name 'Helmer Fjellvåg' _publ_contact_author_address ; Helmer Fjellvåg University of Oslo P.O Box 1033 Blindern N-0315 Oslo Norway ; _publ_contact_author_email helmer.fjellvag@kjemi.uio.no _publ_contact_author_fax '+47-22855565' _publ_contact_author_phone '+47-22855564' _publ_contact_letter ? _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Synthesis and characterization of the open framework magnesium aluminophosphate UiO-28 ; loop_ _publ_author_name _publ_author_address 'Kjell Ove Kongshaug' ; Department of Chemistry University of Oslo P.O Box 1033 Blindern N-0315 Oslo, Norway ; 'Fjellvag, Helmer' ; University of Oslo P.O. Box 1033 N-0315 Oslo, Norway ; 'Lillerud, Karl Petter' ; University of Oslo P.O. Box 1033 N-0315 Oslo, Norway ; _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ? _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? data_UiO-28-as _database_code_CSD 159627 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H16 Al3 Mg1 N3 O17 P4' _chemical_formula_weight 607.33 _chemical_melting_point ? _chemical_compound_source ? 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' '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 orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 9.2769(8) _cell_length_b 14.7984(13) _cell_length_c 14.6106(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2005.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 1370 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 22.48 _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type 'Empirical with SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens SMART CCD' _diffrn_measurement_method 'scanning' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13700 _diffrn_reflns_av_R_equivalents 0.1182 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 22.48 _reflns_number_total 1370 _reflns_number_observed 1104 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART CCD' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-95 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.1762P)^2^+8.6352P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1370 _refine_ls_number_parameters 171 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_obs 0.0877 _refine_ls_wR_factor_all 0.2779 _refine_ls_wR_factor_obs 0.2469 _refine_ls_goodness_of_fit_all 1.099 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.099 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.263 _refine_ls_shift/esd_mean 0.020 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.8765(3) 0.3430(2) 0.2500 0.0459(10) Uani 1 d S . P2 P 0.6820(3) -0.0279(2) 0.2500 0.0413(9) Uani 1 d S . P3 P 1.1482(3) 0.13343(15) 0.1031(2) 0.0504(8) Uani 1 d . . Al1 Al 1.1426(3) 0.3470(2) 0.1150(2) 0.0484(9) Uani 0.82 d P . Mg1 Mg 1.1426(3) 0.3470(2) 0.1150(2) 0.0484(9) Uani 0.18 d P . Al2 Al 0.9015(4) 0.1356(2) 0.2500 0.0453(10) Uani 1 d S . Al3 Al 0.3323(4) 0.0204(2) 0.2500 0.0422(10) Uani 0.30 d SP . Mg3 Mg 0.3323(4) 0.0204(2) 0.2500 0.0422(10) Uani 0.70 d SP . O1 O 0.8256(10) 0.2444(5) 0.2500 0.059(2) Uani 1 d S . O2 O 0.7471(11) 0.4018(6) 0.2500 0.075(3) Uani 1 d S . O3 O 0.9667(8) 0.3592(4) 0.1638(5) 0.071(2) Uani 1 d . . O4 O 0.7559(13) 0.0616(7) 0.2500 0.093(4) Uani 1 d S . O5 O 0.5265(11) -0.0138(8) 0.2500 0.098(4) Uani 1 d S . O6 O 0.7279(9) -0.0783(6) 0.3337(6) 0.095(3) Uani 1 d . . O7 O 1.2562(9) 0.0668(5) 0.1397(5) 0.086(3) Uani 1 d . . O8 O 1.1270(10) 0.1149(5) 0.0007(4) 0.078(2) Uani 1 d . . O9 O 1.0026(8) 0.1206(4) 0.1490(5) 0.072(2) Uani 1 d . . O10 O 1.1983(7) 0.2308(4) 0.1167(5) 0.063(2) Uani 1 d . . OW1 O 0.4385(35) 0.1583(18) 0.2500 0.137(17) Uani 0.48(4) d SP . OW2 O 0.5019(46) 0.2552(38) 0.2500 0.349(54) Uani 0.53(4) d SP . N1 N 1.2130(12) -0.0840(8) 0.0054(7) 0.087(3) Uani 1 d . . N2 N 0.6248(26) 0.2425(14) 0.0481(17) 0.099(7) Uani 0.50 d P . C1 C 1.3689(18) -0.0966(13) -0.0138(13) 0.136(7) Uani 1 d . . C2 C 0.4356(19) -0.1743(12) 0.4729(14) 0.131(6) Uani 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 0.049(2) 0.034(2) 0.054(2) 0.000 0.000 0.0088(13) P2 0.041(2) 0.033(2) 0.050(2) 0.000 0.000 0.0016(12) P3 0.070(2) 0.0385(14) 0.0427(14) 0.0082(9) 0.0046(11) 0.0137(10) Al1 0.062(2) 0.037(2) 0.046(2) -0.0044(11) 0.0021(12) -0.0045(12) Mg1 0.062(2) 0.037(2) 0.046(2) -0.0044(11) 0.0021(12) -0.0045(12) Al2 0.050(2) 0.033(2) 0.052(2) 0.000 0.000 -0.0095(15) Al3 0.042(2) 0.038(2) 0.047(2) 0.000 0.000 0.006(2) Mg3 0.042(2) 0.038(2) 0.047(2) 0.000 0.000 0.006(2) O1 0.060(6) 0.039(5) 0.076(6) 0.000 0.000 0.002(4) O2 0.077(7) 0.045(5) 0.102(7) 0.000 0.000 0.025(5) O3 0.089(5) 0.056(4) 0.067(4) -0.001(3) 0.019(4) 0.008(3) O4 0.084(7) 0.065(7) 0.130(10) 0.000 0.000 -0.027(6) O5 0.057(6) 0.102(9) 0.135(11) 0.000 0.000 -0.001(6) O6 0.101(6) 0.098(6) 0.086(5) 0.033(5) 0.011(5) 0.039(5) O7 0.093(5) 0.085(5) 0.081(5) 0.027(4) 0.019(4) 0.038(4) O8 0.135(7) 0.053(4) 0.048(4) 0.004(3) 0.006(4) -0.001(4) O9 0.073(5) 0.068(4) 0.074(4) -0.002(3) 0.020(4) 0.000(3) O10 0.064(4) 0.059(4) 0.067(4) -0.005(3) -0.005(3) 0.004(3) OW1 0.118(25) 0.045(17) 0.247(42) 0.000 0.000 -0.015(14) OW2 0.088(27) 0.215(61) 0.744(162) 0.000 0.000 0.080(30) N1 0.077(6) 0.085(7) 0.097(7) -0.020(5) -0.006(5) 0.012(5) N2 0.114(17) 0.067(12) 0.116(17) -0.014(12) -0.002(14) 0.010(11) C1 0.099(11) 0.135(15) 0.174(17) 0.068(12) 0.029(10) 0.030(10) C2 0.105(11) 0.095(11) 0.192(17) -0.022(12) -0.015(12) 0.013(9) _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 1.482(9) . ? P1 O3 1.531(7) 6_556 ? P1 O3 1.531(7) . ? P1 O1 1.534(8) . ? P1 Mg1 3.160(4) 6_556 ? P1 Mg1 3.160(4) . ? P2 O5 1.458(11) . ? P2 O4 1.491(11) . ? P2 O6 1.494(7) 6_556 ? P2 O6 1.494(8) . ? P2 Mg1 3.156(3) 3_745 ? P2 Mg1 3.156(3) 8_755 ? P3 O7 1.504(7) . ? P3 O9 1.520(7) . ? P3 O10 1.526(7) . ? P3 O8 1.534(6) . ? P3 Mg1 3.166(3) . ? Al1 O8 1.788(6) 4 ? Al1 O3 1.789(7) . ? Al1 O6 1.796(8) 3_755 ? Al1 O10 1.797(7) . ? Mg1 O8 1.788(6) 4 ? Mg1 O3 1.789(7) . ? Mg1 O6 1.796(8) 3_755 ? Mg1 O10 1.797(7) . ? Mg1 P2 3.156(3) 3_755 ? Al2 O4 1.739(10) . ? Al2 O1 1.758(8) . ? Al2 O9 1.763(7) . ? Al2 O9 1.763(7) 6_556 ? Al3 O5 1.871(11) . ? Al3 O7 1.888(7) 6_456 ? Al3 O7 1.888(7) 1_455 ? Al3 O2 1.904(9) 3_645 ? Al3 OW1 2.27(3) . ? Mg3 O5 1.871(11) . ? Mg3 O7 1.888(7) 6_456 ? Mg3 O7 1.888(7) 1_455 ? Mg3 O2 1.904(9) 3_645 ? Mg3 OW1 2.27(3) . ? O2 Mg3 1.904(9) 3_655 ? O2 Al3 1.904(9) 3_655 ? O6 Mg1 1.796(8) 3_745 ? O6 Al1 1.796(8) 3_745 ? O7 Mg3 1.888(7) 1_655 ? O7 Al3 1.888(7) 1_655 ? O8 Mg1 1.788(6) 4 ? O8 Al1 1.788(6) 4 ? OW1 OW2 1.55(6) . ? N1 C1 1.48(2) . ? N2 C2 1.39(3) 3_655 ? N2 N2 1.42(5) 4 ? N2 C2 1.59(3) 2_654 ? C1 C2 1.44(2) 6_656 ? C2 N2 1.39(3) 3_645 ? C2 C1 1.44(2) 6_456 ? C2 N2 1.59(3) 2_655 ? 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 O3 110.6(4) . 6_556 ? O2 P1 O3 110.6(4) . . ? O3 P1 O3 110.7(6) 6_556 . ? O2 P1 O1 108.0(6) . . ? O3 P1 O1 108.5(3) 6_556 . ? O3 P1 O1 108.5(3) . . ? O2 P1 Mg1 128.5(3) . 6_556 ? O3 P1 Mg1 19.4(3) 6_556 6_556 ? O3 P1 Mg1 94.8(3) . 6_556 ? O1 P1 Mg1 105.0(3) . 6_556 ? O2 P1 Mg1 128.5(3) . . ? O3 P1 Mg1 94.8(3) 6_556 . ? O3 P1 Mg1 19.4(3) . . ? O1 P1 Mg1 105.0(3) . . ? Mg1 P1 Mg1 77.22(12) 6_556 . ? O5 P2 O4 109.1(7) . . ? O5 P2 O6 110.7(4) . 6_556 ? O4 P2 O6 108.2(5) . 6_556 ? O5 P2 O6 110.7(4) . . ? O4 P2 O6 108.2(5) . . ? O6 P2 O6 109.9(7) 6_556 . ? O5 P2 Mg1 126.5(3) . 3_745 ? O4 P2 Mg1 106.5(4) . 3_745 ? O6 P2 Mg1 94.2(3) 6_556 3_745 ? O6 P2 Mg1 18.1(3) . 3_745 ? O5 P2 Mg1 126.5(3) . 8_755 ? O4 P2 Mg1 106.5(4) . 8_755 ? O6 P2 Mg1 18.1(3) 6_556 8_755 ? O6 P2 Mg1 94.2(3) . 8_755 ? Mg1 P2 Mg1 77.34(11) 3_745 8_755 ? O7 P3 O9 110.7(4) . . ? O7 P3 O10 111.7(5) . . ? O9 P3 O10 109.3(4) . . ? O7 P3 O8 108.4(5) . . ? O9 P3 O8 107.1(5) . . ? O10 P3 O8 109.6(4) . . ? O7 P3 Mg1 130.2(4) . . ? O9 P3 Mg1 94.9(3) . . ? O10 P3 Mg1 19.2(3) . . ? O8 P3 Mg1 103.3(3) . . ? O8 Al1 O3 105.7(4) 4 . ? O8 Al1 O6 104.7(4) 4 3_755 ? O3 Al1 O6 112.5(4) . 3_755 ? O8 Al1 O10 109.8(3) 4 . ? O3 Al1 O10 110.7(3) . . ? O6 Al1 O10 113.0(4) 3_755 . ? O8 Mg1 O3 105.7(4) 4 . ? O8 Mg1 O6 104.7(4) 4 3_755 ? O3 Mg1 O6 112.5(4) . 3_755 ? O8 Mg1 O10 109.8(3) 4 . ? O3 Mg1 O10 110.7(3) . . ? O6 Mg1 O10 113.0(4) 3_755 . ? O8 Mg1 P2 116.6(3) 4 3_755 ? O3 Mg1 P2 99.3(3) . 3_755 ? O6 Mg1 P2 15.0(3) 3_755 3_755 ? O10 Mg1 P2 113.9(2) . 3_755 ? O8 Mg1 P1 122.2(3) 4 . ? O3 Mg1 P1 16.5(2) . . ? O6 Mg1 P1 105.9(3) 3_755 . ? O10 Mg1 P1 101.4(2) . . ? P2 Mg1 P1 91.37(9) 3_755 . ? O8 Mg1 P3 105.3(3) 4 . ? O3 Mg1 P3 97.9(2) . . ? O6 Mg1 P3 128.8(3) 3_755 . ? O10 Mg1 P3 16.2(2) . . ? P2 Mg1 P3 127.68(11) 3_755 . ? P1 Mg1 P3 91.64(9) . . ? O4 Al2 O1 105.4(5) . . ? O4 Al2 O9 109.5(3) . . ? O1 Al2 O9 109.1(3) . . ? O4 Al2 O9 109.5(3) . 6_556 ? O1 Al2 O9 109.1(3) . 6_556 ? O9 Al2 O9 113.7(5) . 6_556 ? O5 Al3 O7 117.3(3) . 6_456 ? O5 Al3 O7 117.3(3) . 1_455 ? O7 Al3 O7 117.1(5) 6_456 1_455 ? O5 Al3 O2 97.1(5) . 3_645 ? O7 Al3 O2 101.0(3) 6_456 3_645 ? O7 Al3 O2 101.0(3) 1_455 3_645 ? O5 Al3 OW1 79.9(9) . . ? O7 Al3 OW1 80.5(5) 6_456 . ? O7 Al3 OW1 80.5(5) 1_455 . ? O2 Al3 OW1 177.0(9) 3_645 . ? O5 Mg3 O7 117.3(3) . 6_456 ? O5 Mg3 O7 117.3(3) . 1_455 ? O7 Mg3 O7 117.1(5) 6_456 1_455 ? O5 Mg3 O2 97.1(5) . 3_645 ? O7 Mg3 O2 101.0(3) 6_456 3_645 ? O7 Mg3 O2 101.0(3) 1_455 3_645 ? O5 Mg3 OW1 79.9(9) . . ? O7 Mg3 OW1 80.5(5) 6_456 . ? O7 Mg3 OW1 80.5(5) 1_455 . ? O2 Mg3 OW1 177.0(9) 3_645 . ? P1 O1 Al2 138.5(6) . . ? P1 O2 Mg3 148.6(7) . 3_655 ? P1 O2 Al3 148.6(7) . 3_655 ? Mg3 O2 Al3 0.0(2) 3_655 3_655 ? P1 O3 Mg1 144.1(5) . . ? P1 O3 Al1 144.1(5) . . ? Mg1 O3 Al1 0.0(2) . . ? P2 O4 Al2 156.4(9) . . ? P2 O5 Mg3 172.6(9) . . ? P2 O5 Al3 172.6(9) . . ? Mg3 O5 Al3 0.0(2) . . ? P2 O6 Mg1 147.0(6) . 3_745 ? P2 O6 Al1 147.0(6) . 3_745 ? Mg1 O6 Al1 0.0(3) 3_745 3_745 ? P3 O7 Mg3 142.3(5) . 1_655 ? P3 O7 Al3 142.3(5) . 1_655 ? Mg3 O7 Al3 0.0(3) 1_655 1_655 ? P3 O8 Mg1 148.8(5) . 4 ? P3 O8 Al1 148.8(5) . 4 ? Mg1 O8 Al1 0.0(2) 4 4 ? P3 O9 Al2 145.8(5) . . ? P3 O10 Mg1 144.5(5) . . ? P3 O10 Al1 144.5(5) . . ? Mg1 O10 Al1 0.0(2) . . ? OW2 OW1 Al3 176.5(25) . . ? OW2 OW1 Mg3 176.5(25) . . ? Al3 OW1 Mg3 0.0(2) . . ? C2 N2 N2 69.1(17) 3_655 4 ? C2 N2 C2 105.5(19) 3_655 2_654 ? N2 N2 C2 54.4(14) 4 2_654 ? C2 C1 N1 116.2(14) 6_656 . ? N2 C2 C1 128.9(19) 3_645 6_456 ? N2 C2 N2 56.5(19) 3_645 2_655 ? C1 C2 N2 93.9(17) 6_456 2_655 ? _refine_diff_density_max 0.919 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.158 #==========END data_ UiO-28-175_P _database_code_CSD 159628 _journal_coden_Cambridge 1145 _audit_creation_date Oct 26 20:08:11 2000 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_update_record ; Oct 26 20:08:11 2000 Initial CIF as created by GSAS2CIF ; _publ_contact_author_name 'Helmer Fjellvåg' _publ_contact_author_address ; Helmer Fjellvåg University of Oslo P.O Box 1033 Blindern N-0315 Oslo Norway ; _publ_contact_author_email helmer.fjellvag@kjemi.uio.no _publ_contact_author_fax '+47-22855565' _publ_contact_author_phone '+47-22855564' _publ_contact_letter ? _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Synthesis and characterization of the open framework magnesium aluminophosphate UiO-28 ; loop_ _publ_author_name _publ_author_address 'Kjell Ove Kongshaug' ; Department of Chemistry University of Oslo P.O Box 1033 Blindern N-0315 Oslo, Norway ; 'Fjellvag, Helmer' ; University of Oslo P.O. Box 1033 N-0315 Oslo, Norway ; 'Lillerud, Karl Petter' ; University of Oslo P.O. Box 1033 N-0315 Oslo, Norway ; _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ? _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _refine_ls_shift/esd_max ? _refine_ls_shift/esd_mean ? _computing_structure_refinement GSAS _refine_ls_number_parameters 90 _refine_ls_goodness_of_fit_all 2.88 _refine_ls_number_restraints 28 _pd_proc_ls_prof_R_factor 0.0590 _pd_proc_ls_prof_wR_factor 0.0624 _pd_proc_ls_prof_F2_factor 0.0790 _cell_length_a 9.2187(4) _cell_length_b 14.8652(4) _cell_length_c 14.5811(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 1998.1(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.001 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c m' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y+1/2,+z +x,-y+1/2,+z+1/2 -x,-y,+z+1/2 -x,-y,-z +x,-y+1/2,-z -x,+y+1/2,-z+1/2 +x,+y,-z+1/2 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity P1 0.8890(14) 0.3347(7) 0.25 1.0 Uiso 0.0304(23) 4 P2 0.6851(15) -0.0362(7) 0.25 1.0 Uiso 0.0304(23) 4 P3 1.1548(9) 0.1356(5) 0.1041(6) 1.0 Uiso 0.0304(23) 8 Al1 1.1480(10) 0.3479(5) 0.1145(7) 0.82 Uiso 0.0398(24) 8 Mg1 1.1480(10) 0.3479(5) 0.1145(7) 0.18 Uiso 0.0398(24) 8 Al2 0.8989(15) 0.1353(8) 0.25 1.0 Uiso 0.0398(24) 4 Al3 0.3291(19) 0.0190(8) 0.25 0.3 Uiso 0.0398(24) 4 Mg3 0.3291(19) 0.0190(8) 0.25 0.7 Uiso 0.0398(24) 4 O1 0.8144(16) 0.2430(10) 0.25 1.0 Uiso 0.0549(22) 4 O2 0.7572(19) 0.3946(12) 0.25 1.0 Uiso 0.0549(22) 4 O3 0.9725(13) 0.3597(8) 0.1628(8) 1.0 Uiso 0.0549(22) 8 O4 0.7563(21) 0.0537(10) 0.25 1.0 Uiso 0.0549(22) 4 O5 0.5315(18) -0.0061(17) 0.25 1.0 Uiso 0.0549(22) 4 O6 0.7280(15) -0.0737(8) 0.3398(7) 1.0 Uiso 0.0549(22) 8 O7 1.2674(16) 0.0695(8) 0.1364(9) 1.0 Uiso 0.0549(22) 8 O8 1.1269(13) 0.1116(6) 0.0026(8) 1.0 Uiso 0.0549(22) 8 O9 1.0134(13) 0.1191(8) 0.1526(9) 1.0 Uiso 0.0549(22) 8 O10 1.2102(11) 0.2328(7) 0.1187(7) 1.0 Uiso 0.0549(22) 8 N1 1.2174(14) -0.0856(9) -0.0038(18) 1.0 Uiso 0.080(4) 8 N2 0.6458(26) 0.2208(16) 0.0528(19) 0.5 Uiso 0.080(4) 8 C1 1.3775(16) -0.1031(10) -0.0106(25) 1.0 Uiso 0.080(4) 8 C2 0.4177(18) -0.1908(12) 0.4627(17) 1.0 Uiso 0.080(4) 8 loop_ _atom_type_symbol _atom_type_number_in_cell P 16.0 AL 11.76 MG 4.24 O 64.0 N 12.0 C 16.0 _chemical_formula_structural 'MgAl3(PO4)4C4N3H14' _chemical_formula_sum 'C4 H14 Al3 Mg1 N3 O16 P4' _chemical_formula_weight 597.96 _diffrn_ambient_temperature 298 _diffrn_ambient_environment 'air' _diffrn_ambient_pressure '1 atm' _diffrn_radiation_source Cu _diffrn_radiation_detector 'Braun linear PSD' _pd_meas_info_author_name ? _pd_meas_info_author_email ? _pd_meas_info_author_address ? _pd_meas_info_author_telephone ? _pd_meas_datetime_initiated ? #loop_ _pd_phase_id ? _pd_phase_block_id PHASE_1 _pd_instr_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.83 _diffrn_radiation_wavelength 1.540598 _diffrn_radiation_type 'Cu K\a~1~' _pd_proc_info_datetime 'Oct 26 20:08:14 2000' _pd_calc_method 'Rietveld Refinement' _pd_meas_2theta_range_min 8.000 _pd_meas_2theta_range_max 89.8829 _pd_meas_2theta_range_inc 0.015576 _pd_proc_2theta_range_min 8.000 _pd_proc_2theta_range_max 89.8829 _pd_proc_2theta_range_inc 0.015576 _reflns_number_observed 883 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _reflns_d_resolution_high 1.091 _reflns_d_resolution_low 9.219 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 O1 1.528(10) P1 O2 1.506(11) P1 O3 1.532(7) P1 O3 1.532(7) P2 O4 1.490(10) P2 O5 1.485(11) P2 O6 1.477(7) P2 O6 1.477(7) P3 O7 1.504(9) P3 O8 1.545(9) P3 O9 1.503(9) P3 O10 1.547(9) Al1 O3 1.773(9) Al1 O6 1.764(9) Al1 O8 1.820(9) Al1 O10 1.806(8) Al2 O1 1.780(10) Al2 O4 1.788(10) Al2 O9 1.786(7) Al2 O9 1.786(7) Mg3 O2 2.014(15) Mg3 O5 1.903(15) Mg3 O7 1.905(10) Mg3 O7 1.905(10) N1 C1 1.502(11) N2 N2 1.77(6) N2 C2 1.506(11) N2 C2 1.456(12) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 P1 O2 99.5(12) O1 P1 O3 116.2(8) O1 P1 O3 116.2(8) O2 P1 O3 105.2(9) O2 P1 O3 105.2(9) O3 P1 O3 112.2(14) O4 P2 O5 98.6(14) O4 P2 O6 102.7(9) O4 P2 O6 102.7(9) O5 P2 O6 111.7(9) O5 P2 O6 111.7(9) O6 P2 O6 124.9(14) O7 P3 O8 105.3(9) O7 P3 O9 110.2(10) O7 P3 O10 109.9(9) O8 P3 O9 105.6(9) O8 P3 O10 113.7(7) O9 P3 O10 112.0(8) O3 Al1 O6 112.1(8) O3 Al1 O8 104.0(8) O3 Al1 O10 111.7(7) O6 Al1 O8 101.8(7) O6 Al1 O10 114.0(9) O8 Al1 O10 112.3(6) O1 Al2 O4 106.7(11) O1 Al2 O9 112.3(7) O1 Al2 O9 112.3(7) O4 Al2 O9 110.1(8) O4 Al2 O9 110.1(8) O9 Al2 O9 105.4(13) O2 Mg3 O5 102.0(11) O2 Mg3 O7 104.1(8) O2 Mg3 O7 104.1(8) O5 Mg3 O7 111.7(8) O5 Mg3 O7 111.7(8) O7 Mg3 O7 120.8(12) C2 N2 C2 88.6(22) N1 C1 C2 110.8(16) N2 C2 C1 76.1(15) N2 C2 C1 138.1(22)