# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'R. E. Morris' _publ_section_abstract ? _publ_contact_author_address ; School of Chemistry Purdie Building North Haugh St. Andrews Fife Scotland KY16 9ST UNITED KINGDOM ; _publ_contact_author_email rem1@st-andrews.ac.uk _publ_contact_author_phone 01334463818 _publ_contact_author_fax 01334463808 loop_ _publ_author_name _publ_author_address R.E.Morris ;School of Chemistry Purdie Building North Haugh St. Andrews Fife Scotland KY16 9ST ; E.R.Parnham ;School of Chemistry Purdie Building North Haugh St. Andrews Fife Scotland KY16 9ST ; _publ_section_title ; Ionothermal synthesis using a hydrophobic ionic liquid as solvent in the preparation of a novel aluminophosphate chain structure ; data_Al[H2PO4]F _database_code_depnum_ccdc_archive 'CCDC 616055' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Al F H4 O8 P2' _chemical_formula_sum 'Al F H4 O8 P2' _chemical_formula_weight 239.95 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 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1000 0.0917 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0625 0.0500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4494(17) _cell_length_b 4.7836(10) _cell_length_c 15.767(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.491(3) _cell_angle_gamma 90.00 _cell_volume 628.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.001 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.730 _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 150(2) _diffrn_radiation_wavelength 0.69990 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4222 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.84 _reflns_number_total 1261 _reflns_number_gt 1001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXL-97 _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^)+(0.0705P)^2^+0.9311P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1261 _refine_ls_number_parameters 124 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.031 _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 0.63314(15) 0.2151(3) 0.63683(8) 0.0021(3) Uani 1 1 d . . . Al1 Al 0.86262(17) -0.2789(3) 0.70032(9) 0.0018(4) Uani 1 1 d . . . P2 P 0.86331(15) -0.0347(3) 0.88523(8) 0.0029(3) Uani 1 1 d . . . F1 F 1.0410(3) -0.0663(6) 0.73247(17) 0.0042(6) Uani 1 1 d . . . O1 O 0.6848(4) 0.4998(7) 0.6680(2) 0.0052(8) Uani 1 1 d U . . O2 O 0.7641(4) 0.0052(7) 0.6321(2) 0.0041(7) Uani 1 1 d . . . O3 O 0.5313(4) 0.2471(7) 0.5440(2) 0.0074(8) Uani 1 1 d D . . H3A H 0.527(14) 0.397(13) 0.514(6) 0.011 Uiso 0.50 1 d PD . . H3B H 0.541(13) 0.084(10) 0.522(7) 0.011 Uiso 0.50 1 d PD . . O4 O 0.5156(4) 0.0851(7) 0.6931(2) 0.0078(8) Uani 1 1 d DU . . H4 H 0.449(5) 0.188(9) 0.715(3) 0.012 Uiso 1 1 d D . . O5 O 0.7883(4) -0.1503(7) 0.7992(2) 0.0046(7) Uani 1 1 d . . . O6 O 1.0323(4) 0.0844(7) 0.8904(2) 0.0046(7) Uani 1 1 d U . . O7 O 0.7510(4) 0.1846(8) 0.9165(2) 0.0107(8) Uani 1 1 d D . . H7 H 0.783(7) 0.355(4) 0.920(4) 0.016 Uiso 1 1 d D . . O8 O 0.8656(4) -0.2842(7) 0.9501(2) 0.0057(8) Uani 1 1 d DU . . H8 H 0.877(7) -0.245(11) 1.0040(8) 0.009 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 0.0013(6) 0.0034(7) 0.0018(7) 0.0000(5) 0.0003(5) 0.0000(5) Al1 0.0015(7) 0.0024(8) 0.0018(8) -0.0003(6) 0.0012(6) -0.0006(6) P2 0.0038(6) 0.0026(7) 0.0027(7) -0.0009(5) 0.0015(5) -0.0010(5) F1 0.0054(15) 0.0044(15) 0.0036(14) -0.0014(11) 0.0034(11) -0.0012(11) O1 0.0042(15) 0.0027(16) 0.0087(16) -0.0018(13) 0.0011(13) 0.0009(12) O2 0.0045(17) 0.0032(18) 0.0046(18) 0.0017(13) 0.0010(14) -0.0001(13) O3 0.0073(19) 0.010(2) 0.004(2) 0.0008(14) -0.0016(15) 0.0020(16) O4 0.0071(16) 0.0070(17) 0.0113(17) 0.0017(13) 0.0077(13) 0.0034(13) O5 0.0027(16) 0.0076(18) 0.0033(17) -0.0007(14) -0.0005(13) -0.0001(14) O6 0.0049(14) 0.0065(16) 0.0028(14) 0.0016(12) 0.0021(12) -0.0015(12) O7 0.011(2) 0.0063(19) 0.016(2) -0.0048(16) 0.0081(16) -0.0008(16) O8 0.0080(16) 0.0071(17) 0.0022(16) 0.0011(12) 0.0013(13) -0.0032(13) _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 O1 1.488(4) . ? P1 O2 1.505(3) . ? P1 O4 1.565(4) . ? P1 O3 1.578(4) . ? Al1 F1 1.820(3) . ? Al1 O1 1.840(4) 1_545 ? Al1 F1 1.841(3) 2_746 ? Al1 O2 1.845(4) . ? Al1 O5 1.878(4) . ? Al1 O6 1.918(4) 2_746 ? P2 O5 1.504(3) . ? P2 O6 1.527(3) . ? P2 O7 1.548(4) . ? P2 O8 1.569(4) . ? O3 H3A 0.860(3) . ? O3 H3B 0.860(3) . ? O4 H4 0.86(3) . ? O7 H7 0.86(3) . ? O8 H8 0.860(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 O1 P1 O2 116.7(2) . . ? O1 P1 O4 110.8(2) . . ? O2 P1 O4 107.7(2) . . ? O1 P1 O3 107.64(19) . . ? O2 P1 O3 108.14(19) . . ? O4 P1 O3 105.3(2) . . ? F1 Al1 O1 178.86(16) . 1_545 ? F1 Al1 F1 89.41(8) . 2_746 ? O1 Al1 F1 89.61(15) 1_545 2_746 ? F1 Al1 O2 91.37(15) . . ? O1 Al1 O2 89.61(16) 1_545 . ? F1 Al1 O2 179.16(16) 2_746 . ? F1 Al1 O5 87.74(14) . . ? O1 Al1 O5 92.79(16) 1_545 . ? F1 Al1 O5 86.75(15) 2_746 . ? O2 Al1 O5 93.59(16) . . ? F1 Al1 O6 86.23(14) . 2_746 ? O1 Al1 O6 93.15(16) 1_545 2_746 ? F1 Al1 O6 87.67(14) 2_746 2_746 ? O2 Al1 O6 92.07(16) . 2_746 ? O5 Al1 O6 171.83(16) . 2_746 ? O5 P2 O6 115.85(19) . . ? O5 P2 O7 110.3(2) . . ? O6 P2 O7 110.3(2) . . ? O5 P2 O8 105.4(2) . . ? O6 P2 O8 109.77(19) . . ? O7 P2 O8 104.5(2) . . ? Al1 F1 Al1 147.66(16) . 2_756 ? P1 O1 Al1 143.0(2) . 1_565 ? P1 O2 Al1 136.6(2) . . ? P1 O3 H3A 124(8) . . ? P1 O3 H3B 102(7) . . ? H3A O3 H3B 123(10) . . ? P1 O4 H4 121(4) . . ? P2 O5 Al1 136.1(2) . . ? P2 O6 Al1 129.2(2) . 2_756 ? P2 O7 H7 117(4) . . ? P2 O8 H8 118(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O6 0.860(18) 1.88(2) 2.697(5) 158(5) 3_757 O4 H4 O5 0.86(4) 2.13(3) 2.883(5) 146(5) 2_656 O7 H7 O8 0.86(3) 1.89(3) 2.740(5) 169(6) 1_565 O3 H3A O3 0.860(3) 1.95(3) 2.796(7) 166(11) 3_666 O3 H3B O3 0.860(3) 1.94(4) 2.748(7) 156(10) 3_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.691 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.169