# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1693

data_vp55p_t #(STA-6)


_audit_creation_method            SHELXL
_chemical_name_systematic          ?

_chemical_formula_sum             'Mg3 Al13 P16 O64.1.5(C14 N4 H34). 2.5H2O'
_chemical_formula_weight          

;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_melting_point           ?
_chemical_compound_source         ?

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 '-x+1/2, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 'y+1/2, x+1/2, -z+1/2'
 '-y+1/2, -x+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z'
 '-y, x, -z'
 'x-1/2, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z-1/2'
 '-y-1/2, -x-1/2, z-1/2'
 'y-1/2, x-1/2, z-1/2'

_cell_length_a                    14.322(2)
_cell_length_b                    14.322(2)
_cell_length_c                    10.424(1)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2138.2(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     295(1)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        ?
_exptl_crystal_colour             white
_exptl_crystal_size_max          '80 microns'
_exptl_crystal_size_mid           '25 microns'
_exptl_crystal_size_min           '25 microns'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.841
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1184
_exptl_absorpt_coefficient_mu     0.591
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       295(1)
_diffrn_radiation_wavelength      0.68850
_diffrn_radiation_type            ?
_diffrn_radiation_source          'X-ray synchrotron, 9.8 Daresbury'

_diffrn_measurement_device        'SMART CCD area detector'
_diffrn_measurement_method        ?

_diffrn_standards_interval_time   '3 seconds/frame'
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             14131
_diffrn_reflns_av_R_equivalents   0.0579
_diffrn_reflns_av_sigmaI/netI     0.0328
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          2.33
_diffrn_reflns_theta_max          29.27
_reflns_number_total              1640
_reflns_number_observed           1097
_reflns_observed_criterion        >2sigma(I)

_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ?


_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^)+(0.1704P)^2^+10.2166P] 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     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1640
_refine_ls_number_parameters      64
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1155
_refine_ls_R_factor_obs           0.0843
_refine_ls_wR_factor_all          0.2878
_refine_ls_wR_factor_obs          0.2671
_refine_ls_goodness_of_fit_all    0.961
_refine_ls_goodness_of_fit_obs    1.088
_refine_ls_restrained_S_all       0.961
_refine_ls_restrained_S_obs       1.088
_refine_ls_shift/esd_max          -0.021
_refine_ls_shift/esd_mean         0.007

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
Al1 Al 0.26889(13) 0.10907(12) 0.0000 0.0210(5) Uani 1 d S .
P2 P 0.26657(12) -0.11369(11) 0.0000 0.0241(5) Uani 1 d S .
Al2 Al 0.39072(11) -0.10928(11) -0.2500 0.0314(6) Uani 1 d S .
P1 P 0.61008(8) -0.11008(8) -0.2500 0.0305(5) Uani 1 d S .
O1 O 0.2414(4) -0.0114(3) 0.0000 0.0380(13) Uani 1 d S .
O2 O 0.3209(3) -0.1397(3) -0.1174(4) 0.0491(12) Uani 1 d . .
O3 O 0.5093(3) -0.1278(3) -0.2135(5) 0.0495(11) Uani 1 d . .
O4 O 0.1750(4) -0.1661(4) 0.0000 0.0427(14) Uani 1 d S .
O5 O 0.6683(3) -0.1381(3) -0.1386(5) 0.064(2) Uani 1 d . .
N1 N 0.5595 0.6718 0.0547 0.300 Uiso 0.09 d P .
N2 N 0.5368 0.3621 0.0000 0.300 Uiso 0.09 d SP .
N3 N 0.4221 0.5146 0.2956 0.300 Uiso 0.09 d P .
N4 N 0.4938 0.5105 0.7902 0.300 Uiso 0.09 d P .
C1 C 0.4937 0.7371 1.0000 0.300 Uiso 0.09 d SP .
C2 C 0.6187 0.3376 0.0918 0.300 Uiso 0.09 d P .
C3 C 0.4966 0.4748 0.3812 0.300 Uiso 0.09 d P .
C4 C 0.4092 0.5505 0.7258 0.300 Uiso 0.09 d P .
C5 C 0.4451 0.3200 0.0477 0.300 Uiso 0.09 d P .
C6 C 0.4066 0.3480 0.1815 0.300 Uiso 0.09 d P .
C7 C 0.3685 0.4473 0.2101 0.300 Uiso 0.09 d P .
C8 C 0.4508 0.6050 0.2332 0.300 Uiso 0.09 d P .
C9 C 0.5145 0.5906 0.1159 0.300 Uiso 0.09 d P .
C10 C 0.6460 0.6501 0.9782 0.300 Uiso 0.09 d P .
C11 C 0.6480 0.5692 0.8802 0.300 Uiso 0.09 d P .
C12 C 0.5810 0.5662 0.7643 0.300 Uiso 0.09 d P .
C13 C 0.5025 0.4061 0.7672 0.300 Uiso 0.09 d P .
C14 C 0.5593 0.3481 0.8665 0.300 Uiso 0.09 d P .

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 0.0208(9) 0.0177(9) 0.0245(10) 0.000 0.000 0.0037(7)
P2 0.0275(9) 0.0214(8) 0.0232(8) 0.000 0.000 -0.0061(6)
Al2 0.0322(7) 0.0322(7) 0.0298(12) -0.0073(6) 0.0073(6) 0.0010(8)
P1 0.0283(6) 0.0283(6) 0.0350(10) -0.0130(5) -0.0130(5) 0.0077(6)
O1 0.052(3) 0.013(2) 0.049(3) 0.000 0.000 -0.002(2)
O2 0.057(3) 0.045(2) 0.046(2) -0.007(2) 0.027(2) -0.005(2)
O3 0.035(2) 0.057(3) 0.056(3) -0.006(2) 0.001(2) 0.005(2)
O4 0.041(3) 0.035(3) 0.052(3) 0.000 0.000 -0.019(2)
O5 0.080(3) 0.046(2) 0.067(3) -0.005(2) -0.056(3) 0.011(2)

_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 O5 1.758(4) 9_655 ?
Al1 O5 1.758(4) 2_655 ?
Al1 O4 1.756(5) 3 ?
Al1 O1 1.777(5) . ?
P2 O2 1.503(4) . ?
P2 O2 1.503(4) 10 ?
P2 O1 1.515(5) . ?
P2 O4 1.518(5) . ?
Al2 O3 1.767(4) 7_544 ?
Al2 O3 1.767(4) . ?
Al2 O2 1.768(4) 7_544 ?
Al2 O2 1.768(4) . ?
P1 O5 1.491(4) 8_554 ?
P1 O5 1.491(4) . ?
P1 O3 1.521(4) . ?
P1 O3 1.521(4) 8_554 ?
O4 Al1 1.756(5) 11 ?
O5 Al1 1.758(4) 9_655 ?

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
O5 Al1 O5 111.1(4) 9_655 2_655 ?
O5 Al1 O4 107.7(2) 9_655 3 ?
O5 Al1 O4 107.7(2) 2_655 3 ?
O5 Al1 O1 110.2(2) 9_655 . ?
O5 Al1 O1 110.2(2) 2_655 . ?
O4 Al1 O1 109.8(3) 3 . ?
O2 P2 O2 109.6(4) . 10 ?
O2 P2 O1 111.5(2) . . ?
O2 P2 O1 111.5(2) 10 . ?
O2 P2 O4 109.1(2) . . ?
O2 P2 O4 109.1(2) 10 . ?
O1 P2 O4 106.0(4) . . ?
O3 Al2 O3 109.7(3) 7_544 . ?
O3 Al2 O2 109.9(2) 7_544 7_544 ?
O3 Al2 O2 108.8(2) . 7_544 ?
O3 Al2 O2 108.8(2) 7_544 . ?
O3 Al2 O2 109.9(2) . . ?
O2 Al2 O2 109.5(3) 7_544 . ?
O5 P1 O5 107.9(4) 8_554 . ?
O5 P1 O3 111.1(3) 8_554 . ?
O5 P1 O3 107.1(3) . . ?
O5 P1 O3 107.1(3) 8_554 8_554 ?
O5 P1 O3 111.1(3) . 8_554 ?
O3 P1 O3 112.5(4) . 8_554 ?
P2 O1 Al1 153.4(4) . . ?
P2 O2 Al2 151.0(3) . . ?
P1 O3 Al2 147.1(4) . . ?
P2 O4 Al1 152.5(5) . 11 ?
P1 O5 Al1 150.4(3) . 9_655 ?

_refine_diff_density_max    1.080
_refine_diff_density_min   -0.733
_refine_diff_density_rms    0.146