Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Xiang, Shouhe' 'Li, N.' _publ_contact_author_name 'Prof Shouhe Xiang' _publ_contact_author_address ; Nankai University Institute of Chemistry,Nankai unive Tianjin 300071 CHINA ; _publ_contact_author_email 'SHXIANG@PUBLIC.TPT.TJ.CN' _publ_section_title ; Hydrothermal synthesis and crystal structure of two novel aluminophosphites containing infinite Al-O-Al chain ; data_010214a _database_code_CSD 162456 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H11 Al N0 O10 P2' _chemical_formula_weight 260.01 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' '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 6.949(2) _cell_length_b 17.398(6) _cell_length_c 7.903(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 955.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.578 _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 298(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_% ? _diffrn_reflns_number 1714 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 25.01 _reflns_number_total 432 _reflns_number_gt 317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0522P)^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 432 _refine_ls_number_parameters 51 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.552 _refine_ls_shift/su_mean 0.054 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 0.0000 0.37651(7) 0.16642(18) 0.0141(4) Uani 1 2 d S . . Al1 Al 0.2500 0.2500 0.0000 0.0111(5) Uani 1 4 d S . . O1 O 0.1807(3) 0.32737(13) 0.1606(3) 0.0198(7) Uani 1 1 d . . . O2 O 0.5000 0.2500 0.0907(6) 0.0142(11) Uani 1 4 d SD . . O3 O 0.0000 0.43079(19) 0.3132(5) 0.0210(9) Uani 1 2 d S . . O4 O 0.0000 0.5901(2) 0.3377(7) 0.0410(12) Uani 1 2 d SD . . O5 O 0.1244(12) 0.7500 0.4707(11) 0.039(2) Uani 0.50 2 d SP . . H1 H 0.5000 0.2500 0.2044(15) 0.04(3) Uiso 1 4 d SD . . H2 H 0.123(12) 0.604(15) 0.32(3) 0.50(15) Uiso 1 1 d D . . H3 H 0.0000 0.442(14) 0.05(4) 0.50(14) Uiso 1 2 d S . . 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 0.0125(7) 0.0132(7) 0.0165(7) -0.0018(6) 0.000 0.000 Al1 0.0066(10) 0.0108(10) 0.0159(11) 0.000 0.0007(10) 0.000 O1 0.0138(14) 0.0223(14) 0.0234(15) -0.0091(12) -0.0011(12) 0.0003(10) O2 0.009(3) 0.023(3) 0.010(3) 0.000 0.000 0.000 O3 0.028(2) 0.0161(18) 0.0193(19) -0.0075(16) 0.000 0.000 O4 0.041(3) 0.034(2) 0.048(3) -0.003(2) 0.000 0.000 O5 0.039(5) 0.035(4) 0.044(6) 0.000 -0.006(5) 0.000 _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 1.496(4) . ? P1 O1 1.520(2) 12 ? P1 O1 1.520(2) . ? Al1 O2 1.879(2) . ? Al1 O2 1.879(2) 13 ? Al1 O1 1.912(2) 13 ? Al1 O1 1.912(2) 7_545 ? Al1 O1 1.912(2) . ? Al1 O1 1.912(2) 11_565 ? O2 Al1 1.879(2) 2_655 ? O5 O5 1.729(16) 2_565 ? O5 O5 1.806(16) 13_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 P1 O1 112.26(13) . 12 ? O3 P1 O1 112.26(13) . . ? O1 P1 O1 111.43(19) 12 . ? O2 Al1 O2 180.0 . 13 ? O2 Al1 O1 91.17(12) . 13 ? O2 Al1 O1 88.83(12) 13 13 ? O2 Al1 O1 91.17(12) . 7_545 ? O2 Al1 O1 88.83(12) 13 7_545 ? O1 Al1 O1 89.53(15) 13 7_545 ? O2 Al1 O1 88.83(12) . . ? O2 Al1 O1 91.17(12) 13 . ? O1 Al1 O1 180.00(9) 13 . ? O1 Al1 O1 90.47(15) 7_545 . ? O2 Al1 O1 88.83(12) . 11_565 ? O2 Al1 O1 91.17(12) 13 11_565 ? O1 Al1 O1 90.47(15) 13 11_565 ? O1 Al1 O1 180.00(9) 7_545 11_565 ? O1 Al1 O1 89.53(15) . 11_565 ? P1 O1 Al1 128.64(16) . . ? Al1 O2 Al1 135.1(3) . 2_655 ? O5 O5 O5 165.1(6) 2_565 13_566 ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.336 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.087 data_010609f _database_code_CSD 181566 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H21 Al N2 O7 P2' _chemical_formula_weight 322.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 29.123(17) _cell_length_b 6.772(4) _cell_length_c 6.851(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.991(10) _cell_angle_gamma 90.00 _cell_volume 1349.3(14) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9035 _exptl_absorpt_correction_T_max 0.9796 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2365 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1065 _reflns_number_gt 719 _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^)+(0.0800P)^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 1065 _refine_ls_number_parameters 96 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.225 _refine_ls_shift/su_mean 0.024 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 0.43862(4) 0.21210(16) 0.75029(16) 0.0172(4) Uani 1 1 d D . . Al1 Al 0.5000 0.5000 0.5000 0.0119(4) Uani 1 2 d S . . O1 O 0.5000 0.6096(6) 0.7500 0.0177(9) Uani 1 2 d S . . O2 O 0.46129(12) 0.2943(5) 0.5737(4) 0.0284(8) Uani 1 1 d . . . O4 O 0.44596(11) 0.3494(5) 0.9253(4) 0.0288(9) Uani 1 1 d . . . O3 O 0.38963(11) 0.1563(5) 0.7119(5) 0.0281(8) Uani 1 1 d . . . N1 N 0.39125(13) 0.2516(6) 0.2473(6) 0.0234(9) Uani 1 1 d D . . C1 C 0.34384(16) 0.3293(8) 0.2471(8) 0.0332(12) Uani 1 1 d . . . H1A H 0.3439 0.4699 0.2199 0.040 Uiso 1 1 calc R . . H1B H 0.3315 0.3095 0.3745 0.040 Uiso 1 1 calc R . . C3 C 0.26523(16) 0.3023(9) 0.0778(8) 0.0394(14) Uani 1 1 d . . . H3A H 0.2661 0.4422 0.0477 0.047 Uiso 1 1 calc R . . H3B H 0.2518 0.2876 0.2036 0.047 Uiso 1 1 calc R . . C2 C 0.31390(17) 0.2223(8) 0.0915(8) 0.0355(12) Uani 1 1 d . . . H2A H 0.3274 0.2367 -0.0342 0.043 Uiso 1 1 calc R . . H2B H 0.3131 0.0826 0.1226 0.043 Uiso 1 1 calc R . . H1 H 0.4618(13) 0.061(4) 0.795(6) 0.025(12) Uiso 1 1 d D . . H3 H 0.381(3) 0.126(5) 0.253(13) 0.13(4) Uiso 1 1 d D . . H2 H 0.419(5) 0.23(2) 0.29(2) 0.20(6) 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 0.0189(6) 0.0188(6) 0.0139(6) 0.0005(4) 0.0002(4) -0.0032(5) Al1 0.0144(9) 0.0145(9) 0.0065(9) 0.0011(6) -0.0008(6) -0.0004(7) O1 0.018(2) 0.030(3) 0.0048(19) 0.000 -0.0007(15) 0.000 O2 0.042(2) 0.0304(19) 0.0130(17) -0.0030(13) 0.0044(13) -0.0119(15) O4 0.0307(18) 0.044(2) 0.0121(16) -0.0046(13) 0.0032(12) -0.0131(15) O3 0.0238(17) 0.0276(18) 0.0323(19) -0.0041(14) -0.0034(13) -0.0072(14) N1 0.0164(19) 0.028(2) 0.025(2) 0.0036(16) -0.0002(16) 0.0017(16) C1 0.023(2) 0.037(3) 0.039(3) -0.001(2) 0.001(2) 0.012(2) C3 0.019(2) 0.054(4) 0.045(3) -0.009(3) -0.004(2) 0.009(2) C2 0.026(3) 0.039(3) 0.041(3) -0.001(2) 0.000(2) -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 O3 1.486(3) . ? P1 O2 1.514(3) . ? P1 O4 1.523(3) . ? Al1 O1 1.8666(19) . ? Al1 O1 1.8666(19) 5_666 ? Al1 O2 1.878(3) . ? Al1 O2 1.878(3) 5_666 ? Al1 O4 1.922(3) 2_656 ? Al1 O4 1.922(3) 6_565 ? O1 Al1 1.8666(19) 2_656 ? O4 Al1 1.922(3) 2_656 ? N1 C1 1.478(6) . ? C1 C2 1.524(8) . ? C3 C2 1.516(7) . ? C3 C3 1.525(10) 7 ? 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 O2 114.00(19) . . ? O3 P1 O4 112.85(18) . . ? O2 P1 O4 110.83(18) . . ? O1 Al1 O1 180.000(1) . 5_666 ? O1 Al1 O2 91.12(13) . . ? O1 Al1 O2 88.88(13) 5_666 . ? O1 Al1 O2 88.88(13) . 5_666 ? O1 Al1 O2 91.12(13) 5_666 5_666 ? O2 Al1 O2 180.00(16) . 5_666 ? O1 Al1 O4 90.34(12) . 2_656 ? O1 Al1 O4 89.66(12) 5_666 2_656 ? O2 Al1 O4 91.69(15) . 2_656 ? O2 Al1 O4 88.31(15) 5_666 2_656 ? O1 Al1 O4 89.66(12) . 6_565 ? O1 Al1 O4 90.34(12) 5_666 6_565 ? O2 Al1 O4 88.31(15) . 6_565 ? O2 Al1 O4 91.69(15) 5_666 6_565 ? O4 Al1 O4 180.00(11) 2_656 6_565 ? Al1 O1 Al1 133.1(2) . 2_656 ? P1 O2 Al1 141.3(2) . . ? P1 O4 Al1 127.77(19) . 2_656 ? N1 C1 C2 109.4(4) . . ? C2 C3 C3 112.7(5) . 7 ? C3 C2 C1 111.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 O1 Al1 -114(100) 5_666 . . 2_656 ? O2 Al1 O1 Al1 36.85(11) . . . 2_656 ? O2 Al1 O1 Al1 -143.15(11) 5_666 . . 2_656 ? O4 Al1 O1 Al1 -54.85(11) 2_656 . . 2_656 ? O4 Al1 O1 Al1 125.15(11) 6_565 . . 2_656 ? O3 P1 O2 Al1 135.6(3) . . . . ? O4 P1 O2 Al1 7.0(4) . . . . ? O1 Al1 O2 P1 -4.6(4) . . . . ? O1 Al1 O2 P1 175.4(4) 5_666 . . . ? O2 Al1 O2 P1 -147(100) 5_666 . . . ? O4 Al1 O2 P1 85.8(4) 2_656 . . . ? O4 Al1 O2 P1 -94.2(4) 6_565 . . . ? O3 P1 O4 Al1 -166.9(2) . . . 2_656 ? O2 P1 O4 Al1 -37.6(3) . . . 2_656 ? C3 C3 C2 C1 179.8(6) 7 . . . ? N1 C1 C2 C3 -177.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 0.879 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.093