# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Ayi Ayi' _publ_contact_author_email clearfield@chem.tamu.edu _publ_section_title ; Linear chain aluminium(III) carboxymethylphosphonate with encapsulated ammonium ions ; loop_ _publ_author_name 'Ayi, Ayi' A.Clearfield T.Kinnibrugh data_p-1 _database_code_depnum_ccdc_archive 'CCDC 842302' #TrackingRef '- cif file for manuscript ID DT-COM-08-2011-011620.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 Al O10 P2, 2(H4 N)' _chemical_formula_sum 'C2 H6.50 Al0.50 N O5 P' _chemical_formula_weight 169.04 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.757(2) _cell_length_b 8.231(4) _cell_length_c 8.524(4) _cell_angle_alpha 61.184(4) _cell_angle_beta 79.059(5) _cell_angle_gamma 85.228(5) _cell_volume 287.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2019 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.97 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 174 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8959 _exptl_absorpt_correction_T_max 0.9749 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3192 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.00 _reflns_number_total 1235 _reflns_number_gt 1143 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT+ 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^)+(0.0405P)^2^+0.1345P] 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 1235 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _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 Al1 Al 0.0000 1.0000 0.0000 0.00699(16) Uani 1 2 d S . . P1 P 0.40755(8) 0.94203(5) 0.26359(5) 0.00677(13) Uani 1 1 d . . . N1 N -0.1048(3) 0.3061(2) 0.2201(2) 0.0123(3) Uani 1 1 d . . . H4N H -0.120(5) 0.195(4) 0.324(4) 0.032(6) Uiso 1 1 d . . . H3N H 0.049(6) 0.367(4) 0.219(3) 0.034(6) Uiso 1 1 d . . . H2N H -0.091(5) 0.295(3) 0.119(4) 0.033(6) Uiso 1 1 d . . . H1N H -0.260(5) 0.367(3) 0.230(3) 0.020(5) Uiso 1 1 d . . . C1 C 0.2658(3) 0.7096(2) 0.3632(2) 0.0093(3) Uani 1 1 d . . . H1A H 0.3803 0.6268 0.4485 0.011 Uiso 1 1 d . . . H1B H 0.0777 0.7051 0.4278 0.011 Uiso 1 1 d . . . O1 O 0.7308(2) 0.93886(15) 0.21358(14) 0.0098(2) Uani 1 1 d . . . O2 O 0.3255(2) 1.00307(15) 0.41071(14) 0.0097(2) Uani 1 1 d . . . H2O H 0.4701 0.9965 0.4766 0.029(11) Uiso 0.50 1 d PR . . C2 C 0.2540(3) 0.6428(2) 0.2266(2) 0.0094(3) Uani 1 1 d . . . O3 O 0.2588(2) 1.06221(15) 0.10219(14) 0.0084(2) Uani 1 1 d . . . O4 O 0.3543(2) 0.48909(15) 0.25194(16) 0.0129(3) Uani 1 1 d . . . O5 O 0.1236(2) 0.74579(15) 0.09360(14) 0.0092(2) Uani 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 Al1 0.0062(3) 0.0085(3) 0.0075(3) -0.0046(3) -0.0017(2) 0.0003(2) P1 0.0060(2) 0.0084(2) 0.0069(2) -0.00425(16) -0.00164(15) 0.00025(14) N1 0.0123(7) 0.0127(7) 0.0139(7) -0.0081(6) -0.0020(6) 0.0007(5) C1 0.0103(7) 0.0094(7) 0.0080(7) -0.0036(6) -0.0027(6) 0.0001(6) O1 0.0073(5) 0.0136(5) 0.0088(5) -0.0055(4) -0.0019(4) 0.0009(4) O2 0.0091(5) 0.0139(6) 0.0097(5) -0.0080(4) -0.0031(4) 0.0013(4) C2 0.0065(7) 0.0105(7) 0.0106(7) -0.0048(6) -0.0003(6) -0.0022(5) O3 0.0075(5) 0.0095(5) 0.0094(5) -0.0051(4) -0.0026(4) -0.0001(4) O4 0.0138(6) 0.0101(5) 0.0175(6) -0.0079(5) -0.0060(5) 0.0032(4) O5 0.0095(5) 0.0095(5) 0.0100(5) -0.0053(4) -0.0037(4) 0.0015(4) _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 O3 1.8650(12) 2_575 ? Al1 O3 1.8650(12) . ? Al1 O1 1.8834(13) 2_675 ? Al1 O1 1.8834(13) 1_455 ? Al1 O5 1.9301(14) . ? Al1 O5 1.9301(14) 2_575 ? P1 O1 1.5172(13) . ? P1 O3 1.5211(12) . ? P1 O2 1.5384(12) . ? P1 C1 1.8073(18) . ? N1 H4N 0.91(3) . ? N1 H3N 0.91(3) . ? N1 H2N 0.90(3) . ? N1 H1N 0.87(2) . ? C1 C2 1.519(2) . ? C1 H1A 0.9494 . ? C1 H1B 0.9507 . ? O1 Al1 1.8834(13) 1_655 ? O2 H2O 0.9500 . ? C2 O4 1.245(2) . ? C2 O5 1.2813(19) . ? 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 Al1 O3 179.999(1) 2_575 . ? O3 Al1 O1 88.42(6) 2_575 2_675 ? O3 Al1 O1 91.58(6) . 2_675 ? O3 Al1 O1 91.58(6) 2_575 1_455 ? O3 Al1 O1 88.42(6) . 1_455 ? O1 Al1 O1 180.000(1) 2_675 1_455 ? O3 Al1 O5 86.18(5) 2_575 . ? O3 Al1 O5 93.82(5) . . ? O1 Al1 O5 88.90(5) 2_675 . ? O1 Al1 O5 91.10(5) 1_455 . ? O3 Al1 O5 93.82(5) 2_575 2_575 ? O3 Al1 O5 86.18(5) . 2_575 ? O1 Al1 O5 91.10(5) 2_675 2_575 ? O1 Al1 O5 88.90(5) 1_455 2_575 ? O5 Al1 O5 180.0 . 2_575 ? O1 P1 O3 113.76(6) . . ? O1 P1 O2 110.16(6) . . ? O3 P1 O2 110.40(7) . . ? O1 P1 C1 109.32(7) . . ? O3 P1 C1 106.72(7) . . ? O2 P1 C1 106.15(7) . . ? H4N N1 H3N 106(2) . . ? H4N N1 H2N 113(2) . . ? H3N N1 H2N 113(2) . . ? H4N N1 H1N 107(2) . . ? H3N N1 H1N 109(2) . . ? H2N N1 H1N 108(2) . . ? C2 C1 P1 114.29(11) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? P1 O1 Al1 136.67(7) . 1_655 ? P1 O2 H2O 117.0 . . ? O4 C2 O5 122.72(14) . . ? O4 C2 C1 120.03(14) . . ? O5 C2 C1 117.13(13) . . ? P1 O3 Al1 130.83(7) . . ? C2 O5 Al1 131.67(10) . . ? 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 P1 C1 C2 -76.59(12) . . . . ? O3 P1 C1 C2 46.86(13) . . . . ? O2 P1 C1 C2 164.62(11) . . . . ? O3 P1 O1 Al1 -17.10(12) . . . 1_655 ? O2 P1 O1 Al1 -141.66(10) . . . 1_655 ? C1 P1 O1 Al1 102.07(11) . . . 1_655 ? P1 C1 C2 O4 130.20(13) . . . . ? P1 C1 C2 O5 -53.72(17) . . . . ? O1 P1 O3 Al1 116.16(9) . . . . ? O2 P1 O3 Al1 -119.41(9) . . . . ? C1 P1 O3 Al1 -4.48(11) . . . . ? O1 Al1 O3 P1 -112.48(9) 2_675 . . . ? O1 Al1 O3 P1 67.52(9) 1_455 . . . ? O5 Al1 O3 P1 -23.47(9) . . . . ? O5 Al1 O3 P1 156.53(9) 2_575 . . . ? O4 C2 O5 Al1 -169.26(11) . . . . ? C1 C2 O5 Al1 14.8(2) . . . . ? O3 Al1 O5 C2 -158.26(13) 2_575 . . . ? O3 Al1 O5 C2 21.74(13) . . . . ? O1 Al1 O5 C2 113.26(13) 2_675 . . . ? O1 Al1 O5 C2 -66.74(13) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.378 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.065 _publ_section_references ; Bruker (2005). SAINTP+ for NT. Data Reduction and Correction Program v. 7.56, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 2008.4 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SADABS-2008/1, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SHELXTL 2008/4, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;