#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/47/7204750.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204750
loop_
_publ_author_name
'M. Eloísa Medina'
'M. Iglesias'
'E. Gutiérrez-Puebla'
'M. Angeles Monge'
_publ_section_title
;
 Solvothermal synthesis and structural relations among three anionic
 aluminophosphates; catalytic behaviour
;
_journal_issue                   5
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              845
_journal_page_last               850
_journal_paper_doi               10.1039/b311618b
_journal_volume                  14
_journal_year                    2004
_chemical_formula_sum            'Al2 H12 N3 O12 P3'
_chemical_formula_weight         392.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.407(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.261(3)
_cell_length_b                   10.255(2)
_cell_length_c                   8.8627(19)
_cell_measurement_temperature    293(2)
_cell_volume                     1122.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.809
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_sigmaI/netI    0.1702
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1867
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0529P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                670
_reflns_number_total             1129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311618b.txt
_cod_data_source_block           mm30
_cod_original_cell_volume        1122.2(4)
_cod_original_formula_sum        'H12 Al2 N3 O12 P3'
_cod_database_code               7204750
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.29416(18) 0.62274(18) 0.3437(2) 0.0083(5) Uani 1 1 d . . .
P2 P 0.0000 0.4948(3) 0.2500 0.0064(6) Uani 1 2 d S . .
Al1 Al 0.16769(19) 0.4215(2) 0.0826(3) 0.0078(5) Uani 1 1 d . . .
O1 O 0.2295(4) 0.2699(5) 0.1614(6) 0.0114(13) Uani 1 1 d . . .
O2 O -0.0578(4) 0.5857(5) 0.1044(5) 0.0099(12) Uani 1 1 d . . .
O3 O 0.2161(4) 0.5748(5) 0.1779(6) 0.0119(12) Uani 1 1 d . . .
O4 O 0.0794(4) 0.4051(5) 0.2092(5) 0.0090(11) Uani 1 1 d . . .
O5 O 0.2698(4) 0.5563(5) 0.4802(5) 0.0105(12) Uani 1 1 d . . .
O6 O 0.4103(4) 0.5946(5) 0.3646(6) 0.0180(14) Uani 1 1 d . . .
N2 N 0.5000 0.6179(11) 0.7500 0.024(3) Uani 1 2 d S . .
H5 H 0.454(8) 0.564(10) 0.777(12) 0.050 Uiso 1 1 d . . .
H6 H 0.559(13) 0.623(13) 0.862(17) 0.13(6) Uiso 1 1 d . . .
N1 N 0.3872(7) 0.7021(7) 0.0413(10) 0.0178(18) Uani 1 1 d . . .
H1 H 0.358(10) 0.644(11) 0.016(14) 0.050 Uiso 1 1 d . . .
H2 H 0.472(9) 0.668(9) 0.057(11) 0.050 Uiso 1 1 d . . .
H3 H 0.369(8) 0.752(10) -0.042(12) 0.050 Uiso 1 1 d . . .
H4 H 0.373(8) 0.758(10) 0.096(12) 0.050 Uiso 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
P1 0.0103(11) 0.0073(11) 0.0097(9) -0.0005(8) 0.0063(8) -0.0008(9)
P2 0.0042(16) 0.0106(16) 0.0052(13) 0.000 0.0027(12) 0.000
Al1 0.0083(13) 0.0098(13) 0.0056(10) -0.0005(10) 0.0028(9) -0.0007(11)
O1 0.018(3) 0.003(3) 0.016(3) 0.006(2) 0.011(3) 0.007(2)
O2 0.009(3) 0.008(3) 0.013(3) 0.007(2) 0.005(2) -0.002(2)
O3 0.021(3) 0.008(3) 0.011(3) -0.003(2) 0.010(2) -0.001(3)
O4 0.000(2) 0.017(3) 0.009(2) 0.000 0.001 0.000
O5 0.014(3) 0.010(3) 0.012(2) 0.000(2) 0.011(2) 0.002(2)
O6 0.010(3) 0.021(3) 0.026(3) 0.002(2) 0.010(3) 0.002(3)
N2 0.030(7) 0.024(7) 0.021(6) 0.000 0.014(6) 0.000
N1 0.020(5) 0.016(5) 0.022(4) 0.006(3) 0.012(4) 0.003(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'
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
O6 P1 O5 108.6(3) . . ?
O6 P1 O3 111.0(3) . . ?
O5 P1 O3 110.6(3) . . ?
O6 P1 O1 112.2(3) . 4 ?
O5 P1 O1 111.2(3) . 4 ?
O3 P1 O1 103.1(3) . 4 ?
O4 P2 O4 106.5(4) 2 . ?
O4 P2 O2 109.7(2) 2 2 ?
O4 P2 O2 112.5(2) . 2 ?
O4 P2 O2 112.5(2) 2 . ?
O4 P2 O2 109.7(2) . . ?
O2 P2 O2 106.0(4) 2 . ?
O2 Al1 O1 115.9(3) 5_565 . ?
O2 Al1 O3 120.7(3) 5_565 . ?
O1 Al1 O3 123.3(3) . . ?
O2 Al1 O5 92.6(2) 5_565 6_565 ?
O1 Al1 O5 89.2(2) . 6_565 ?
O3 Al1 O5 85.7(2) . 6_565 ?
O2 Al1 O4 94.3(2) 5_565 . ?
O1 Al1 O4 89.2(2) . . ?
O3 Al1 O4 89.5(2) . . ?
O5 Al1 O4 173.0(2) 6_565 . ?
P1 O1 Al1 141.9(4) 4_545 . ?
P2 O2 Al1 138.2(3) . 5_565 ?
P1 O3 Al1 137.1(3) . . ?
P2 O4 Al1 135.0(3) . . ?
P1 O5 Al1 136.2(3) . 6_566 ?
H5 N2 H6 97(9) . . ?
H1 N1 H2 101(10) . . ?
H1 N1 H3 106(10) . . ?
H2 N1 H3 104(8) . . ?
H1 N1 H4 124(10) . . ?
H2 N1 H4 125(9) . . ?
H3 N1 H4 92(9) . . ?
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 O6 1.510(5) . ?
P1 O5 1.522(5) . ?
P1 O3 1.537(5) . ?
P1 O1 1.539(5) 4 ?
P2 O4 1.537(5) 2 ?
P2 O4 1.537(5) . ?
P2 O2 1.549(5) 2 ?
P2 O2 1.549(5) . ?
Al1 O2 1.764(5) 5_565 ?
Al1 O1 1.777(5) . ?
Al1 O3 1.789(5) . ?
Al1 O5 1.899(5) 6_565 ?
Al1 O4 1.902(5) . ?
O1 P1 1.539(5) 4_545 ?
O2 Al1 1.764(5) 5_565 ?
O5 Al1 1.899(5) 6_566 ?
N2 H5 0.92(10) . ?
N2 H6 1.02(15) . ?
N1 H1 0.70(11) . ?
N1 H2 1.14(11) . ?
N1 H3 0.86(11) . ?
N1 H4 0.82(10) . ?
