##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
ammonium oxonium dititanium(III,IV) tris(phosphate)
;
_chemical_name_common     ?
_chemical_formula_moiety     'O12 P3 Ti2, H4 N, H3 O'
_chemical_formula_sum     'H7 N O13 P3 Ti2'
_chemical_formula_structural     'N H4 +, O H3 +, P3 O12 Ti2 2-'
_chemical_formula_iupac     '(N H4) (H3 O) Ti2 (P O4)3'
_chemical_formula_weight     417.78
_chemical_melting_point     ?
_symmetry_cell_setting     Cubic
_symmetry_space_group_name_H-M     'P 21 3'
_symmetry_space_group_name_Hall     'P 2ac 2ab 3'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    'x+1/2, -y+1/2, -z'
    '-x, y+1/2, -z+1/2'
    'y, z, x'
    '-y+1/2, -z, x+1/2'
    'y+1/2, -z+1/2, -x'
    '-y, z+1/2, -x+1/2'
    'z, x, y'
    '-z, x+1/2, -y+1/2'
    '-z+1/2, -x, y+1/2'
    'z+1/2, -x+1/2, -y'
_cell_length_a     9.9384(4)
_cell_length_b     9.9384(4)
_cell_length_c     9.9384(4)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     981.63(4)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     8307
_cell_measurement_theta_min     3.4
_cell_measurement_theta_max     28.1
_cell_measurement_temperature     295(2)
_exptl_crystal_description     Block
_exptl_crystal_colour     Black
_exptl_crystal_size_max     0.19
_exptl_crystal_size_mid     0.19
_exptl_crystal_size_min     0.12
_exptl_crystal_density_diffrn     2.827
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     828
_exptl_absorpt_coefficient_mu     2.199
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.666
_exptl_absorpt_correction_T_max     0.778
_diffrn_ambient_temperature     295(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker APEX area-detector'
_diffrn_measurement_method     'φ and ω'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     10934
_diffrn_reflns_av_R_equivalents     0.026
_diffrn_reflns_av_sigmaI/netI     0.012
_diffrn_reflns_theta_min     2.9
_diffrn_reflns_theta_max     28.4
_diffrn_reflns_theta_full     28.4
_diffrn_measured_fraction_theta_max     0.99
_diffrn_measured_fraction_theta_full     0.99
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_h_max     13
_diffrn_reflns_limit_k_min     -13
_diffrn_reflns_limit_k_max     13
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_reflns_number_total     816
_reflns_number_gt     815
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.022
_refine_ls_R_factor_gt     0.022
_refine_ls_wR_factor_gt     0.065
_refine_ls_wR_factor_ref     0.065
_refine_ls_goodness_of_fit_ref     1.07
_refine_ls_restrained_S_all     1.07
_refine_ls_number_reflns     816
_refine_ls_number_parameters     68
_refine_ls_number_restraints     3
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0438P)²+1.2965P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.48
_refine_diff_density_min     -0.45
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details     'Flack (1983), 339 Friedel pairs'
_refine_ls_abs_structure_Flack     0.02(4)
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'
    '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'
    'Ti' 'Ti' 0.2776 0.4457
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Bruker, 2002)'
_computing_cell_refinement     'SAINT (Bruker, 2002)'
_computing_data_reduction     SAINT
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEPII (Johnson, 1976)'
_computing_publication_material     SHELXL97
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ti1 0.08490(5) 0.08490(5) 0.08490(5) 0.0071(2) Uani d S 1 . . Ti
    Ti2 0.35671(5) 0.35671(5) 0.35671(5) 0.0071(2) Uani d S 1 . . Ti
    P1 0.04433(7) 0.26610(7) 0.37696(7) 0.0076(2) Uani d . 1 . . P
    O1 0.0192(2) 0.1803(2) 0.2525(2) 0.0150(10)
                                              Uani d . 1 . . O
    O2 0.1946(2) 0.2620(2) 0.4174(2) 0.0120(10)
                                              Uani d . 1 . . O
    O3 -0.0021(2) 0.4103(2) 0.3520(2) 0.0140(10)
                                               Uani d . 1 . . O
    O4 -0.0365(2) 0.2042(2) 0.4940(2) 0.0140(10)
                                               Uani d . 1 . . O
    O5 0.2143(3) 0.2857(3) 0.7143(3) 0.0350(10)
                                              Uani d SD 1 . . O
    N1 -0.0733(3) 0.4267(3) 0.0733(3) 0.0150(10)
                                               Uani d SD 1 . . N
    H1 -0.038(4) 0.427(5) 0.152(2) 0.030(10)
                                           Uiso d D 1 . . H
    H2 -0.0240(10)
                 0.4760(10)
                          0.0240(10)
                                   0.05(3) Uiso d SD 1 . . H
    H3 0.219(8) 0.234(6) 0.645(5) 0.10(3) Uiso d D 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ti1 0.0071(2) 0.0071(2) 0.0071(2) 0.0000(2) 0.0000(2) 0.0000(2)
    Ti2 0.0071(2) 0.0071(2) 0.0071(2) 0.0000(2) 0.0000(2) 0.0000(2)
    P1 0.0076(3) 0.0080(3) 0.0070(3) 0.0001(2) 0.0006(2) -0.0002(2)
    O1 0.0160(10)
                0.0170(10)
                         0.0110(10)
                                  -0.0010(10)
                                            0.0010(10)
                                                     -0.0040(10)
    O2 0.0080(10)
                0.0130(10)
                         0.0140(10)
                                  -0.0010(10)
                                            -0.0010(10)
                                                      0.0020(10)
    O3 0.0130(10)
                0.0100(10)
                         0.0180(10)
                                  0.0040(10)
                                           0.0020(10)
                                                    0.0030(10)
    O4 0.0150(10)
                0.0160(10)
                         0.0130(10)
                                  0.0000(10)
                                           0.0060(10)
                                                    0.0040(10)
    O5 0.0350(10)
                0.0350(10)
                         0.0350(10)
                                  -0.0020(10)
                                            0.0020(10)
                                                     -0.0020(10)
    N1 0.0150(10)
                0.0150(10)
                         0.0150(10)
                                  -0.0010(10)
                                            0.0010(10)
                                                     0.0010(10)
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ti1 O1 . 2.025(2) yes
    Ti1 O1 5 2.025(2) n
    Ti1 O1 9 2.025(2) n
    Ti1 O3 4_545 2.020(2) yes
    Ti1 O3 7_455 2.020(2) n
    Ti1 O3 11_554 2.020(2) n
    Ti2 O2 . 1.961(2) yes
    Ti2 O2 5 1.961(2) n
    Ti2 O2 9 1.961(2) n
    Ti2 O4 3_556 1.922(2) yes
    Ti2 O4 6_565 1.922(2) n
    Ti2 O4 10_655 1.922(2) n
    P1 O1 . 1.523(2) no
    P1 O2 . 1.547(2) no
    P1 O3 . 1.526(2) no
    P1 O4 . 1.542(2) no
    O3 Ti1 4 2.020(2) no
    O4 Ti2 3_456 1.922(2) no
    O5 H3 . 0.860(10)
                    no
    N1 H1 . 0.860(10)
                    no
    N1 H2 . 0.850(10)
                    no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 Ti1 O1 . 5 91.80(10)
                          n
    O1 Ti1 O1 . 9 91.80(10)
                          no
    O1 Ti1 O3 . 4_545 90.90(10)
                              n
    O1 Ti1 O3 . 7_455 85.00(10)
                              n
    O1 Ti1 O3 . 11_554 175.90(10)
                                n
    O1 Ti1 O1 5 9 91.80(10)
                          no
    O1 Ti1 O3 5 4_545 175.90(10)
                               no
    O1 Ti1 O3 5 7_455 90.90(10)
                              no
    O1 Ti1 O3 5 11_554 85.00(10)
                               no
    O1 Ti1 O3 9 4_545 85.00(10)
                              no
    O1 Ti1 O3 9 7_455 175.90(10)
                               no
    O1 Ti1 O3 9 11_554 90.90(10)
                               no
    O3 Ti1 O3 4_545 7_455 92.50(10)
                                  n
    O3 Ti1 O3 4_545 11_554 92.50(10)
                                   no
    O3 Ti1 O3 7_455 11_554 92.50(10)
                                   no
    O2 Ti2 O2 . 5 90.40(10)
                          n
    O2 Ti2 O2 . 9 90.40(10)
                          no
    O2 Ti2 O4 . 3_556 93.70(10)
                              n
    O2 Ti2 O4 . 6_565 86.70(10)
                              n
    O2 Ti2 O4 . 10_655 175.00(10)
                                n
    O2 Ti2 O2 5 9 90.40(10)
                          no
    O2 Ti2 O4 5 3_556 175.00(10)
                               no
    O2 Ti2 O4 5 6_565 93.70(10)
                              no
    O2 Ti2 O4 5 10_655 86.70(10)
                               no
    O2 Ti2 O4 9 3_556 86.70(10)
                              no
    O2 Ti2 O4 9 6_565 175.00(10)
                               no
    O2 Ti2 O4 9 10_655 93.70(10)
                               no
    O4 Ti2 O4 3_556 6_565 89.50(10)
                                  yes
    O4 Ti2 O4 3_556 10_655 89.50(10)
                                   no
    O4 Ti2 O4 10_655 6_565 89.50(10)
                                   no
    O1 P1 O3 . . 110.10(10)
                          no
    O1 P1 O4 . . 107.70(10)
                          no
    O3 P1 O4 . . 109.90(10)
                          no
    O1 P1 O2 . . 110.80(10)
                          no
    O3 P1 O2 . . 111.00(10)
                          no
    O4 P1 O2 . . 107.30(10)
                          no
    P1 O1 Ti1 . . 151.30(10)
                           y
    P1 O2 Ti2 . . 134.50(10)
                           y
    P1 O3 Ti1 . 4 151.60(10)
                           y
    P1 O4 Ti2 . 3_456 174.7(2) y
    H1 N1 H2 . . 107(3) no
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O3 P1 O1 Ti1 . . . . 103.0(3) no
    O4 P1 O1 Ti1 . . . . -137.2(3) no
    O2 P1 O1 Ti1 . . . . -20.2(3) no
    O3 Ti1 O1 P1 7_455 . . . -141.6(3) no
    O3 Ti1 O1 P1 4_545 . . . 126.0(3) no
    O1 Ti1 O1 P1 5 . . . -50.8(2) no
    O1 Ti1 O1 P1 9 . . . 41.0(3) no
    O1 P1 O2 Ti2 . . . . 81.8(2) no
    O3 P1 O2 Ti2 . . . . -40.9(2) no
    O4 P1 O2 Ti2 . . . . -160.9(2) no
    O4 Ti2 O2 P1 3_556 . . . 167.9(2) no
    O4 Ti2 O2 P1 6_565 . . . 78.7(2) no
    O2 Ti2 O2 P1 9 . . . -105.40(10)
                                   no
    O2 Ti2 O2 P1 5 . . . -15.1(2) no
    O1 P1 O3 Ti1 . . . 4 144.4(3) no
    O4 P1 O3 Ti1 . . . 4 26.0(3) no
    O2 P1 O3 Ti1 . . . 4 -92.5(3) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O5 H3 O2 . 0.860(10)
                       2.30(5) 2.966(4) 135(6) yes
    N1 H1 O3 . 0.860(10)
                       2.030(10)
                               2.864(3) 165(4) yes
    N1 H2 O4 5 0.850(10)
                       2.350(10)
                               3.039(4) 138.0(10)
                                               yes
    N1 H2 O4 4 0.850(10)
                       2.350(10)
                               3.039(4) 138.0(10)
                                               yes
    N1 H2 O4 12_455 0.850(10)
                            2.350(10)
                                    3.039(4) 138.0(10)
                                                    yes
data_global
_journal_date_recd_electronic     2005-07-04
_journal_date_accepted     2005-07-05
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2005
_journal_volume     61
_journal_issue      8
_journal_page_first     i158
_journal_page_last     i159
_journal_paper_category     EI
_journal_coeditor_code     HB6237
_publ_contact_author_name     'Ng, Seik Weng'
_publ_contact_author_address
;
      Department of Chemistry
      University of Malaya
      50603 Kuala Lumpur
      Malaysia
;
_publ_contact_author_email     seikweng@um.edu.my
_publ_contact_author_fax     603-7967-6778
_publ_contact_author_phone     603-7967-6778
_publ_section_title
;
Langbeinite-type mixed-valence (NH₄)(H₃O)TiIIITiIV(PO₄)₃
;
loop_
    _publ_author_name
    _publ_author_address
    'Fu, Yun-Long'
;
School of Chemistry and Materials Science
Shanxi Normal University
Linfen 041004
People's Republic of China
;
    'Xu, Zhi-Wei'
;
School of Chemistry and Materials Science
Shanxi Normal University
Linfen 041004
People's Republic of China
;
    'Ren, Jia-Lin'
;
School of Chemistry and Materials Science
Shanxi Normal University
Linfen 041004
People's Republic of China
;
    'Ng, Seik Weng'
;
Department of Chemistry
University of Malaya
50603 Kuala Lumpur
Malaysia
;
