data_global
_audit_creation_method           'form.cif (version 2.0)'
_journal_data_validation_number  ?
_journal_date_recd_electronic    ?
_journal_date_to_coeditor        ?
_journal_date_from_coeditor      ?
_journal_date_accepted           ?
_journal_date_printers_first     ?
_journal_date_printers_final     ?
_journal_date_proofs_out         ?
_journal_date_proofs_in          ?
_journal_coeditor_name           ?
_journal_coeditor_code           ?
_journal_coeditor_notes          ' ?'
_journal_techeditor_code         ?
_journal_techeditor_notes        ' ?'
_journal_coden_ASTM              ?
_journal_name_full               ?
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?
_journal_paper_category          ?
_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?
_publ_contact_author_name        'Vincent MAISONNEUVE'
_publ_contact_author_address
;
Laboratoire des Fluorures - UPRES-A 6010 
Facult\'e des Sciences, Universit\'e du Maine, Avenue Olivier-Messiaen,
 72085 LE MANS Cedex 9, FRANCE
;
_publ_contact_author_phone       '(33) 2 43 83 35 61'
_publ_contact_author_fax         '(33) 2 43 83 35 06'
_publ_contact_author_email       vincent.maisonneuve@univ-lemans.fr
_publ_contact_letter
;
Please consider this CIF submission for publication as a full paper in
Acta Crystallographica C. The figures and structure factors listings
will be sent by normal mailing.
;
_publ_requested_journal          'Acta Crystallographica C'
_publ_requested_coeditor_name    ?
_publ_section_title
;
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H, a One-Dimensional Aluminophosphate
;
loop_
_publ_author_name
_publ_author_address
'S. PHAN THANH'
;
Laboratoire des Fluorures - UPRES-A 6010 Facult\'e des Sciences, 
Universit\'e du Maine, Avenue Olivier-Messiaen, 72085 LE MANS Cedex 9, FRANCE
;
'J. MARROT'
;
Institut Lavoisier, IREM, UMR CNRS C 8637,
Universit\'e  de Versailles Saint-Quentin-en-Yvelines,
45 Avenue des Etats Unis, 75035 Versailles Cedex, FRANCE
;
'J. RENAUDIN'
;
Laboratoire des Fluorures - UPRES-A 6010 Facult\'e des Sciences, 
Universit\'e du Maine, Avenue Olivier-Messiaen, 72085 LE MANS Cedex 9, FRANCE
;
'V. MAISONNEUVE'
;
Laboratoire des Fluorures - UPRES-A 6010 Facult\'e des Sciences, 
Universit\'e du Maine, Avenue Olivier-Messiaen, 72085 LE MANS Cedex 9, FRANCE
;
_publ_section_synopsis
; The structure of the title compound, obtained solvothermally at 473 K, has 
been determined by single-crystal X-ray diffraction. It consists of 
one-dimensional [AlP~2~O~8~H]^2-^ macroanions, connected each other by 
pentanediammonium cations. 
;
_publ_section_abstract
;
The structure of the title compound, obtained solvothermally at 473 K, has 
been determined by single-crystal X-ray diffraction. It consists of 
one-dimensional [AlP~2~O~8~H]^2-^ macroanions, connected each other by 
pentanediammonium cations. Contrary to the referred similar compounds with 
P/Al = 2, the  three-dimensionality is mainly obtained via the network of 
hydrogen bonds. 
;
_publ_section_comment
;
The investigation of the system Al~2~O~3~-H~3~PO~4~-aliphatic 
diamine-EtOH led to a new one-dimensional aluminophosphate templated 
by 1,5-diaminopentane. The structure of [H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H 
consists of inorganic chains, formulated [AlP~2~O~8~H]^2-^, separated by 
organic molecules (Fig. 1, top). The inorganic part is built up from 
tetrahedral AlO~4~ and PO~4~ units, in which all AlO~4~ vertices are 
connected. This arrangement forms a corner-shared Al~2~P~2~ four-membered 
ring, with PO~4~H groups. The Al-O distances, ranging from 1.727 (3) to 
1.731 (3) \%A, and the O-Al-O angles, lying between 106.4 (2) and 111.3 (2)\%, 
are consistent with those found in the mineral Berlinite. On the contrary, the 
P-O distances vary from 1.490 (3) to 1.539 (3) \%A  and from 1.499 (3) to 1.546 
(3) \%A for the P1 and P2 phosphate groups respectively. This dispersion is 
attributable to multiple bond character. 1,5-diaminopentane molecules, which 
must be protonated to balance the negative charges, ensure the cohesion between 
inorganic chains via hydrogen bonds. All the protons of ammonium cations are 
linked to terminal O atoms of PO~4~H group. Owing to N-H...O hydrogen bond 
lengths for the two amine functions, the N1 terminal group is more anchored to 
the inorganic chains. Details of the hydrogen bonding are given in Table 2. 
[H~3~N(CH~2~)~5~NH~3~]^2+^ cations present a bent 
conformation for a size reason. In this case, the atomic displacement 
parameters of the carbon atoms are rather large, especially in the central 
part (atoms C3 and C4) of the molecule (Fig. 2). This situation is 
the complete opposite of that observed in [H~3~N(CH~2~)~6~NH~3~].AlF~5~ 
(Phan Thanh, Renaudin & Maisonneuve, 2000) where the diammonium cation 
exhibits a stretched conformation between (AlF~5~) inorganic chains. In 
addition, it can be observed in the compound called ULM13 both the bent and 
stretched conformations for the 1,6-diaminohexane molecules (Renaudin, 
F\'erey, 1995).

Up to now, two types of chain architecture for the one-dimensional 
aluminophosphates, with a P/Al ratio of 2 in the formulation, have been 
reported in the literature. The former in [H~3~NCH~2~CH~2~NH~3~].AlP~2~O~8~H 
(Williams, Xu, Gao, Chen & Xu, 1997) shows a one-dimensional polymer chains 
consisting of edge-shared Al~2~P~2~ four-membered rings, with pendant PO~4~H 
side groups. The latter, in [H~3~NCH~2~CH~2~NH~3~].AlP~2~O~8~.H~2~O 
(Wang, Yu & Pang, 1990), [Et~3~NH].AlP~2~O~8~H~2~ (Jones, Thomas, Xu, Huo, Xu, 
Cheetham & Bieber, 1990) and [NH~4~][H~3~NCH~2~CH~2~NH~3~].AlP~2~O~8~ (Gao, 
Chen, Li, Xu, Thomas, Light & Hursthouse, 1996), present a linear arrangement 
of corner-shared Al~2~P~2~ four-membered rings similar to that 
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H. However, the higher size of the 
diammonium cation in [H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H led to a distorted 
inorganic chain. On one hand, the small size of the 
organic molecule in these four compounds leads to a three-dimensional 
organization ensured by a combination of van der Waals forces and hydrogen 
bonds. On the other hand, in the title compound, the structure accommodates 
the more significant length of the organic chain by a distortion of the 
organic part but also of the inorganic chain. Consequently, the three-
dimensional character is then obtained mainly by the set of hydrogen bonds 
(Fig. 1, bottom). It is also noticed that this involves a shortening of the 
O-H...O distance. The distance passes from 2.641 (2) \%A in 
[H~3~NCH~2~CH~2~NH~3~].AlP~2~O~8~H to 2.457 (4) \%A in 
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H.
;
_publ_section_exptl_prep
;
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H was prepared from a starting mixture 
Aluminum isopropoxide ([(CH~3~)~2~CHO]~3~Al)-H~3~PO~4~-1.5 diaminopentane-EtOH 
with the molar ratio 1:2:5:100 under solvothermal conditions (473 K, 7 days, 
autogenous pressure) in a Teflon lined autoclave. The resulting product was 
filtered and dried in air at 353 K for 1 h. A suitable single crystal was 
isolated by optical microscopy. The crystal cell of 
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H was obtained from long exposure rotation 
photographs. Systematic extinction conditions lead to P2~1~/n space group.
;
_publ_section_exptl_refinement
;
The structure was solved by direct methods of the program SHELXS86 
(Sheldrick, 1990) and successive refinements and difference Fourier maps using 
SHELXL93 program (Sheldrick, 1993). For the refinement of hydrogen atoms in 
the CH~2~ and NH~3~ groups, geometrical restraint conditions were used that 
implied equal distances and angles to the central atom (AFIX option). H atoms 
of each CH~2~ and NH~3~ groups were refined with a common isotropic thermal 
parameter. Fourier map showed a relatively large electron-density peak of 
1.36 e \%A^-3^ at distances of 0.94 and 1.28 \%A from H5A and C5 respectively.
;
_publ_section_references
; Berger-Hoff, G. (1996). DIAMOND. Visual Crystal Structure Information
 System, Gerhard-Domagk-Str.1, 53121 Bonn, Germany.

Gao, Q., Chen, J., Li, S., Xu, R., Thomas, J. M., Light, M. & Hursthouse,
 M. B. (1996). J. Solid State Chem. 127, 145-150.

Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565.

Jones, R. H., Thomas, J. M., Xu, R., Huo, Q., Xu, Y., Cheetham, A. K. & 
Bieber, D. (1990). J. Chem. Soc., Chem. Commun. 1170-1172.

Phan Thanh, S., Renaudin, J. & Maisonneuve, V. (2000). Solid State Sciences, 
in press.

Renaudin, J. & F\'erey, G. (1995). J. Solid State Chem.  120, 197-203.

Sheldrick, G.M. (1990), Acta Cryst. A46 , 467-473.

Sheldrick, G.M. (1993). SHELXL93. Program for the Refinement of Crystal 
Structures, University of G\"ottingen, Germany.

Sheldrick, G.M. (1996). SADABS. University of G\"ottingen, Germany.

Siemens (1996). SMART and SAINT. Area Detector Control and Integration
 Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Wang, T., Yu, L. & Pang, W. (1990). J. Solid State Chem. 89, 392-395.

Williams, I. D., XU, J., Gao, Q., Chen, J. & Xu, R. (1997). Chem. Commun.
 1273-1274.
;
_publ_section_figure_captions
;
Fig. 1.  Projection of [H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H along the c-axis 
showing its one-dimensional character and the bent conformation of the 
diammonium cation (top) and along the a-axis (bottom). PO~4~ tetrahedra are 
hatched.

Fig. 2.  Ortep view (Farrugia, 1997) of pentanediammonium cation in 
[H~3~N(CH~2~)~5~NH~3~].AlP~2~O~8~H. Displacement ellipsoids are shown at the 
50% probability level.
;
_publ_section_acknowledgements
; The authors thank Professor M. Leblanc and R. Retoux for useful counsels to 
this manuscript and Dr T. Loiseau for his help.
;
_publ_section_table_legends
;
Table 1. Selected bond distances (\%A) and angles (\%)

Table 2. Hydrogen-bonding geometry (\%A, \%)
;
data_C5H17AlN2O8P2
_audit_creation_method           SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C5 H17 Al N2 O8 P2'
_chemical_formula_weight         322.13
_chemical_melting_point          ?
_chemical_compound_source        ?
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2~1~/n
_cell_length_a                   7.8783(2)
_cell_length_b                   10.46890(10)
_cell_length_c                   16.0680(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1470(10)
_cell_angle_gamma                90.00
_cell_volume                     1319.90(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5007
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      29.83
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_T_max  0.978
_exptl_special_details
;
'Blessing, Acta Cryst. (1995) A51 33-38'
;
_diffrn_ambient_temperature      296(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       'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8939
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         29.83
_reflns_number_total             3421
_reflns_number_gt                1901
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Siemens SMART'
_computing_cell_refinement       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'DIAMOND (Berger-Hoff, 1996)'
_computing_publication_material  'Siemens SHELXTL'
_refine_special_details
; Refinement on F^2^ for ALL reflections except for 900 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^)+(0.0573P)^2^+3.0698P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0130(77)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2521
_refine_ls_number_parameters     167
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_all         0.2069
_refine_ls_wR_factor_ref         0.1362
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.370
_refine_ls_restrained_S_obs      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/esd_mean        0.000
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'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
P1 P 0.55909(13) 0.78402(9) 0.02396(7) 0.0280(3) Uani 1 d . .
P2 P 0.09646(13) 1.05563(11) 0.13485(6) 0.0290(3) Uani 1 d . .
Al1 Al 0.24723(13) 0.95928(11) -0.02995(7) 0.0246(4) Uani 1 d . .
O1 O 0.1684(4) 0.9724(3) 0.0667(2) 0.0379(7) Uani 1 d . .
O2 O 0.6564(4) 0.7078(3) -0.0386(2) 0.0373(7) Uani 1 d . .
O3 O 0.0882(4) 0.9116(3) -0.1048(2) 0.0381(7) Uani 1 d . .
O4 O 0.1982(4) 1.1793(3) 0.1459(2) 0.0467(9) Uani 1 d . .
O5 O 0.4005(4) 0.8408(3) -0.0252(2) 0.0435(8) Uani 1 d . .
O6 O 0.5116(4) 0.6993(3) 0.0927(2) 0.0466(8) Uani 1 d . .
O7 O 0.1067(5) 0.9814(4) 0.2149(2) 0.0521(9) Uani 1 d . .
O8 O 0.6701(4) 0.8956(3) 0.0585(2) 0.0398(8) Uani 1 d . .
N1 N 0.5653(6) 0.4525(4) 0.1464(2) 0.0438(10) Uani 1 d . .
N2 N 1.2290(5) 0.7318(4) 0.1793(3) 0.0439(9) Uani 1 d . .
C1 C 0.7372(9) 0.3936(7) 0.1518(5) 0.077(2) Uani 1 d D .
C2 C 0.8618(10) 0.4488(8) 0.2194(5) 0.088(2) Uani 1 d D .
C3 C 0.8903(13) 0.5913(9) 0.2175(5) 0.110(3) Uani 1 d D .
C4 C 0.9232(15) 0.6711(14) 0.1428(8) 0.153(5) Uani 1 d D .
C5 C 1.1025(11) 0.6688(10) 0.1213(5) 0.099(3) Uani 1 d D .
H2 H 0.7123 0.7571 -0.0649 0.056 Uiso 1 calc R .
H1A H 0.4934 0.4053 0.1133 0.066 Uiso 1 calc R .
H1B H 0.5704 0.5309 0.1254 0.066 Uiso 1 calc R .
H1C H 0.5288 0.4565 0.1972 0.066 Uiso 1 calc R .
H1D H 0.7840 0.4038 0.0984 0.092 Uiso 1 calc R .
H1E H 0.7258 0.3028 0.1618 0.092 Uiso 1 calc R .
H2A H 0.8225 0.4271 0.2732 0.105 Uiso 1 calc R .
H2B H 0.9709 0.4071 0.2162 0.105 Uiso 1 calc R .
H3A H 0.7912 0.6290 0.2395 0.132 Uiso 1 calc R .
H3B H 0.9855 0.6077 0.2587 0.132 Uiso 1 calc R .
H4A H 0.8502 0.6411 0.0950 0.184 Uiso 1 calc R .
H4B H 0.8917 0.7587 0.1534 0.184 Uiso 1 calc R .
H5A H 1.1363 0.5802 0.1162 0.118 Uiso 1 calc R .
H5B H 1.1062 0.7081 0.0669 0.118 Uiso 1 calc R .
H2C H 1.3301 0.7296 0.1586 0.066 Uiso 1 calc R .
H2D H 1.2357 0.6916 0.2283 0.066 Uiso 1 calc R .
H2E H 1.1984 0.8127 0.1863 0.066 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
P1 0.0276(5) 0.0230(5) 0.0341(6) 0.0016(4) 0.0063(4) 0.0016(4)
P2 0.0259(5) 0.0418(6) 0.0193(5) -0.0034(4) 0.0019(4) -0.0018(4)
Al1 0.0218(6) 0.0289(6) 0.0233(6) -0.0027(4) 0.0024(4) 0.0004(4)
O1 0.041(2) 0.048(2) 0.0262(15) -0.0020(13) 0.0096(12) 0.0047(14)
O2 0.036(2) 0.0285(15) 0.049(2) -0.0019(13) 0.0141(13) 0.0033(12)
O3 0.0279(15) 0.049(2) 0.037(2) -0.0117(13) -0.0009(12) -0.0003(13)
O4 0.042(2) 0.060(2) 0.039(2) -0.016(2) 0.0100(14) -0.019(2)
O5 0.036(2) 0.046(2) 0.047(2) -0.0090(14) -0.0034(14) 0.0153(14)
O6 0.055(2) 0.032(2) 0.056(2) 0.0116(14) 0.022(2) -0.0010(14)
O7 0.060(2) 0.073(2) 0.024(2) 0.0063(15) 0.0098(14) 0.015(2)
O8 0.045(2) 0.036(2) 0.038(2) -0.0015(13) 0.0052(13) -0.0117(14)
N1 0.067(3) 0.030(2) 0.037(2) -0.003(2) 0.016(2) -0.006(2)
C1 0.080(4) 0.070(4) 0.080(5) -0.026(3) 0.000(4) 0.012(3)
C2 0.073(4) 0.123(7) 0.067(4) -0.005(4) 0.008(3) -0.002(4)
C3 0.097(6) 0.158(10) 0.077(5) -0.002(6) 0.015(4) -0.056(6)
C4 0.169(13) 0.130(10) 0.153(12) 0.010(8) -0.024(10) -0.019(9)
C5 0.099(6) 0.134(7) 0.063(4) -0.007(4) 0.004(4) -0.075(5)
N2 0.041(2) 0.052(2) 0.039(2) 0.012(2) 0.006(2) -0.002(2)
