# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Adrian Wright' 'Neal J. Checker' 'John Godber' 'Benson M. Kariuki' 'Steven Rishi' _publ_contact_author_name 'Adrian Wright' _publ_contact_author_address ; School of Chemistry University of Birmingham Edgbaston Birmingham B15 2TT UNITED KINGDOM ; _publ_contact_author_email A.J.WRIGHT@BHAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis and crystal structure of AlH2P3O10 2H2O; a new structure-type for layered acid phosphates. ; _publ_section_references ; PLATON- (a) Spek, A. L. (1990) Acta Cryst. A46, C34. (b) Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. SHELXTL, program suite for structure solution and refinement, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SMART, program for instrument control and data aquisition, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SAINTPLUS, program suite for data processing, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA ; data_altp121 _database_code_depnum_ccdc_archive 'CCDC 288341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Al H2 P3 O10, 2(H2 O)' _chemical_formula_sum 'Al H6 O12 P3' _chemical_formula_weight 317.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0492 0.0322 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 7.9659(8) _cell_length_b 4.9180(6) _cell_length_c 11.6355(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.851(7) _cell_angle_gamma 90.00 _cell_volume 453.46(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 579 _cell_measurement_theta_min 5.58 _cell_measurement_theta_max 68.91 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 7.724 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2813 _exptl_absorpt_correction_T_max 0.8608 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2051 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.58 _diffrn_reflns_theta_max 68.91 _reflns_number_total 742 _reflns_number_gt 579 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _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^)+(0.0972P)^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 742 _refine_ls_number_parameters 84 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.003 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 O1 O -0.3552(5) 0.3005(7) 0.5079(3) 0.0176(9) Uani 1 1 d . . . O2 O -0.5695(5) 0.0815(8) 0.6467(3) 0.0200(9) Uani 1 1 d . . . O3 O -0.3200(5) 0.7934(7) 0.5697(3) 0.0201(9) Uani 1 1 d . . . O4 O -0.0922(5) 0.4637(8) 0.6231(4) 0.0257(11) Uani 1 1 d D . . H1 H -0.0446(11) 0.630(3) 0.631(5) 0.031 Uiso 1 1 d D . . O5 O -0.3572(5) 0.4335(8) 0.7170(3) 0.0240(10) Uani 1 1 d . . . O6 O 0.0725(8) -0.0743(18) 0.6348(7) 0.092(2) Uani 1 1 d D . . H2 H 0.031(6) 0.092(7) 0.651(9) 0.110 Uiso 1 1 d D . . H3 H 0.165(8) -0.051(14) 0.596(8) 0.110 Uiso 1 1 d D . . Al1 Al -0.5000 0.0000 0.5000 0.0129(6) Uani 1 2 d S . . P1 P -0.28251(17) 0.5022(2) 0.59579(11) 0.0140(5) Uani 1 1 d D . . P2 P -0.5000 0.2373(4) 0.7500 0.0146(5) Uani 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 O1 0.025(2) 0.0117(18) 0.0169(18) -0.0025(15) 0.0051(16) -0.0040(16) O2 0.027(2) 0.022(2) 0.0116(17) -0.0018(17) 0.0026(15) -0.0064(17) O3 0.027(2) 0.012(2) 0.0203(19) -0.0006(16) -0.0013(16) -0.0048(17) O4 0.023(2) 0.017(2) 0.036(3) 0.0017(19) -0.0030(19) 0.0009(16) O5 0.037(2) 0.020(2) 0.0150(19) 0.0007(18) 0.0027(17) -0.0120(19) O6 0.036(4) 0.140(6) 0.102(5) -0.019(5) 0.019(3) -0.030(4) Al1 0.0196(12) 0.0077(11) 0.0113(11) -0.0012(9) 0.0014(9) -0.0022(8) P1 0.0179(7) 0.0093(8) 0.0146(8) 0.0018(6) 0.0002(5) -0.0019(5) P2 0.0228(10) 0.0101(10) 0.0111(9) 0.000 0.0027(7) 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 O1 P1 1.498(4) . ? O1 Al1 1.871(3) . ? O2 P2 1.485(4) . ? O2 Al1 1.890(4) . ? O3 P1 1.488(4) . ? O3 Al1 1.873(4) 1_565 ? O4 P1 1.529(4) . ? O5 P2 1.569(4) . ? O5 P1 1.621(4) . ? Al1 O1 1.871(3) 3_456 ? Al1 O3 1.873(4) 3_466 ? Al1 O3 1.873(4) 1_545 ? Al1 O2 1.890(4) 3_456 ? P2 O2 1.485(4) 2_456 ? P2 O5 1.569(4) 2_456 ? 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 P1 O1 Al1 138.6(2) . . ? P2 O2 Al1 136.2(2) . . ? P1 O3 Al1 137.7(2) . 1_565 ? P2 O5 P1 132.9(2) . . ? O1 Al1 O1 180.0(2) . 3_456 ? O1 Al1 O3 91.92(15) . 3_466 ? O1 Al1 O3 88.08(15) 3_456 3_466 ? O1 Al1 O3 88.08(15) . 1_545 ? O1 Al1 O3 91.92(15) 3_456 1_545 ? O3 Al1 O3 180.0(2) 3_466 1_545 ? O1 Al1 O2 88.62(16) . 3_456 ? O1 Al1 O2 91.38(16) 3_456 3_456 ? O3 Al1 O2 90.34(16) 3_466 3_456 ? O3 Al1 O2 89.66(16) 1_545 3_456 ? O1 Al1 O2 91.38(16) . . ? O1 Al1 O2 88.62(16) 3_456 . ? O3 Al1 O2 89.66(16) 3_466 . ? O3 Al1 O2 90.34(16) 1_545 . ? O2 Al1 O2 180.00(8) 3_456 . ? O3 P1 O1 116.2(2) . . ? O3 P1 O4 109.6(2) . . ? O1 P1 O4 111.5(2) . . ? O3 P1 O5 107.1(2) . . ? O1 P1 O5 107.8(2) . . ? O4 P1 O5 103.8(2) . . ? O2 P2 O2 117.8(3) . 2_456 ? O2 P2 O5 109.8(2) . . ? O2 P2 O5 107.2(2) 2_456 . ? O2 P2 O5 107.2(2) . 2_456 ? O2 P2 O5 109.8(2) 2_456 2_456 ? O5 P2 O5 104.1(3) . 2_456 ? 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 O4 H1 O6 0.904(10) 1.724(14) 2.620(9) 171(4) 1_565 O6 H2 O4 0.907(11) 2.09(4) 2.950(10) 159(9) . O6 H3 O2 0.908(11) 2.24(8) 2.942(7) 134(9) 1_655 O6 H3 O1 0.908(11) 2.37(4) 3.135(8) 141(6) 3_556 _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 68.91 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 0.642 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.141