Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_AlaPrPO-I _database_code_CSD 165782 _journal_coden_Cambridge 186 _publ_contact_author_name 'Prof. Russell E. Morris' _publ_contact_author_address ; Prof R Morris School of Chemistry Purdie Building University of St Andrews St Andrews FIFE KY16 9ST UK ; _publ_contact_author_email 'REM1@ST-AND.AC.UK' loop_ _publ_author_name 'Attfield, Martin P.' 'Bull, Ivor' 'Morris, R.' 'Wheatley, Paul S.' 'Zakowsky, Nadja' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and structure of an aluminium 3-aminopropyl phosphonate sulphate hydrate ; # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-04-19 at 15:25:08 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1 # Request file : C:\Program Files\wingx\files\archive.dat # CIF files read : stan129a _audit_creation_date 2001-04-19T15:25:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum ? _chemical_formula_moiety 'Al(O3P(CH2)3NH3).SO4.3H2O' _chemical_formula_weight 315.16 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.3082(10) _cell_length_b 6.2577(6) _cell_length_c 16.486(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1063.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.828 _exptl_crystal_F_000 595 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.65 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.6887 _diffrn_radiation_monochromator Si(111) _diffrn_reflns_number 7189 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 29.34 _reflns_number_total 1632 _reflns_number_gt 1200 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1303P)^2^+3.0863P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 1632 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_gt 0.1929 _refine_ls_wR_factor_all 0.2124 _refine_ls_goodness_of_fit_gt 1.146 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_gt 1.146 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.641 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.259 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0643 0.0516 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1026 0.0946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1187 0.1163 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.36908(14) 0.25 0.58443(9) 0.0142(4) Uani 1 d S . S2 S -0.11949(11) 0.25 0.61767(7) 0.0167(3) Uani 1 d S . P1 P 0.56368(12) 0.25 0.42877(7) 0.0146(3) Uani 1 d S . O1 O 0.2469(4) 0.25 0.6736(2) 0.0176(7) Uani 1 d S . O2 O 0.2256(4) 0.25 0.5128(2) 0.0191(8) Uani 1 d S . O3 O 0.4997(3) 0.25 0.6664(2) 0.0171(7) Uani 1 d S . O4 O 0.5014(4) 0.25 0.5120(2) 0.0174(7) Uani 1 d S . O5 O 0.3521(2) -0.0521(4) 0.58399(14) 0.0156(5) Uani 1 d . . O8 O -0.0081(4) 0.25 0.6745(2) 0.0236(8) Uani 1 d S . O9 O -0.2393(4) 0.25 0.6661(2) 0.0336(11) Uani 1 d S . O11 O -0.1109(3) 0.0594(6) 0.5680(2) 0.0403(9) Uani 1 d . . N1 N 0.0860(5) -0.25 0.6200(3) 0.0238(10) Uani 1 d S . C2 C 0.3734(5) 0.25 0.2072(3) 0.0201(10) Uani 1 d S . H2A H 0.3203(5) 0.1248 0.2174(3) 0.03 Uiso 1 calc R . H2B H 0.3203(5) 0.3752 0.2174(3) 0.03 Uiso 1 calc R . C3 C 0.4872(5) 0.25 0.2663(3) 0.0164(9) Uani 1 d S . H3A H 0.5405(5) 0.3756 0.2572(3) 0.025 Uiso 1 calc R . H3B H 0.5405(5) 0.1244 0.2572(3) 0.025 Uiso 1 calc R . C6 C 0.4371(5) 0.25 0.3532(3) 0.0158(9) Uani 1 d S . H6A H 0.3830(5) 0.1249 0.3612(3) 0.024 Uiso 1 calc R . H6B H 0.3830(5) 0.3751 0.3612(3) 0.024 Uiso 1 calc R . 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 Al1 0.0145(7) 0.0137(7) 0.0145(7) 0 0.0003(5) 0 S2 0.0161(6) 0.0194(6) 0.0145(6) 0 -0.0010(4) 0 P1 0.0155(6) 0.0146(6) 0.0136(6) 0 0.0001(4) 0 O1 0.017(2) 0.021(2) 0.015(2) 0 0.0026(13) 0 O2 0.020(2) 0.017(2) 0.020(2) 0 -0.0062(14) 0 O3 0.016(2) 0.021(2) 0.014(2) 0 0.0005(13) 0 O4 0.020(2) 0.017(2) 0.015(2) 0 0.0039(13) 0 O5 0.0158(11) 0.0147(11) 0.0165(11) 0.0017(9) 0.0006(8) 0.0003(9) O8 0.016(2) 0.037(2) 0.018(2) 0 -0.0002(14) 0 O9 0.018(2) 0.065(3) 0.018(2) 0 -0.0015(15) 0 O11 0.033(2) 0.037(2) 0.051(2) -0.026(2) -0.0082(14) 0.0000(14) N1 0.023(2) 0.033(3) 0.015(2) 0 0.002(2) 0 C2 0.019(2) 0.022(3) 0.020(2) 0 -0.002(2) 0 C3 0.018(2) 0.018(2) 0.013(2) 0 0.001(2) 0 C6 0.016(2) 0.016(2) 0.015(2) 0 0.003(2) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al1 O4 1.813(4) . ? Al1 O2 1.893(4) . ? Al1 O5 1.898(3) . ? Al1 O5 1.898(3) 7_565 ? Al1 O3 1.908(4) . ? Al1 O1 1.935(4) . ? S2 O11 1.449(3) . ? S2 O11 1.449(3) 7_565 ? S2 O9 1.470(4) . ? S2 O8 1.482(4) . ? P1 O4 1.514(4) . ? P1 O5 1.527(3) 3_656 ? P1 O5 1.527(3) 5_656 ? P1 C6 1.804(5) . ? O5 P1 1.527(3) 5_656 ? N1 C2 1.498(7) 2 ? C2 N1 1.498(7) 2_554 ? C2 C3 1.525(7) . ? C3 C6 1.524(6) . ? 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 O4 Al1 O2 100.2(2) . . ? O4 Al1 O5 93.82(9) . . ? O2 Al1 O5 85.74(9) . . ? O4 Al1 O5 93.82(9) . 7_565 ? O2 Al1 O5 85.74(9) . 7_565 ? O5 Al1 O5 169.4(2) . 7_565 ? O4 Al1 O3 86.3(2) . . ? O2 Al1 O3 173.5(2) . . ? O5 Al1 O3 93.88(9) . . ? O5 Al1 O3 93.88(9) 7_565 . ? O4 Al1 O1 171.8(2) . . ? O2 Al1 O1 88.0(2) . . ? O5 Al1 O1 86.74(9) . . ? O5 Al1 O1 86.74(9) 7_565 . ? O3 Al1 O1 85.5(2) . . ? O11 S2 O11 110.7(4) . 7_565 ? O11 S2 O9 111.0(2) . . ? O11 S2 O9 111.0(2) 7_565 . ? O11 S2 O8 108.1(2) . . ? O11 S2 O8 108.1(2) 7_565 . ? O9 S2 O8 107.9(2) . . ? O4 P1 O5 111.45(13) . 3_656 ? O4 P1 O5 111.45(12) . 5_656 ? O5 P1 O5 108.4(2) 3_656 5_656 ? O4 P1 C6 108.6(2) . . ? O5 P1 C6 108.43(13) 3_656 . ? O5 P1 C6 108.43(13) 5_656 . ? P1 O4 Al1 156.3(3) . . ? P1 O5 Al1 139.1(2) 5_656 . ? N1 C2 C3 113.5(4) 2_554 . ? C2 C3 C6 109.8(4) . . ? C3 C6 P1 113.8(3) . . ?