
data_cc

_publ_section_exptl_refinement
;
Disorder of the organic strucutre directing agent 
(OSDA) caused difficulties locating the linking
carbon atoms between the DABCO cages as well as
the terminal nitrogen atoms (N2). High thermal 
parameters and the differences between 
neighbouring atoms are also attributed to the
disordered nature of the OSDA.
No significant electron density was found at 
end of the final refinement cycles.
;

_vrf_PLAT340_cc
;
RESPONSE:
Due to the nature of the template and the resulting disorder.
See _publ_section_exptl_refinement for further comments.
;

_vrf_RFACR01_cc
;
RESPONSE:
The disordered nature of the template, charge balancing 
hydroxide and flexibility within the framework cause a
comparably high wR2 value.
;

_vrf_PLAT084_cc
;
RESPONSE:
see _vrf_RFACR01_cc
;

_vrf_PLAT201_cc
;
RESPONSE:
see _publ_section_exptl_refinement
;

_vrf_PLAT242_cc
;
RESPONSE:
Disorder of C atoms surrounding N1 atom.
;


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'AlPO STA-2, as-prepared'
_chemical_melting_point           ?
_chemical_formula_moiety          '6(Al2 O8.33 P2), C15.98 H24 N4'
_chemical_formula_sum
 'C16 H24 Al12 N4 O50 P12'
_chemical_formula_weight          1767.23

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.2130   0.2455
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            hexagonal
_symmetry_space_group_name_H-M    'R-3'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                    13.0310(6)
_cell_length_b                    13.0310(6)
_cell_length_c                    29.4980(16)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      4337.89(4)
_cell_formula_units_Z             3
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     1071
_cell_measurement_theta_min       21.3
_cell_measurement_theta_max       68.1

_exptl_crystal_description        'Prism'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_size_max           0.03
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.029
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2820.0
_exptl_absorpt_coefficient_mu     6.368
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_max   0.826
_exptl_absorpt_correction_T_min   0.826
_exptl_absorpt_process_details    ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      1.54187
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   
;
Rigaku Saturn92 (2x2 bin mode)
;
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  22.2222
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             20137
_diffrn_reflns_av_R_equivalents   0.1636
_diffrn_reflns_av_sigmaI/netI     0.0822
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        35
_diffrn_reflns_theta_min          21.9
_diffrn_reflns_theta_max          68.07
_reflns_number_total              1760
_reflns_number_gt                 1145
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_reduction         
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/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      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1760
_refine_ls_number_parameters      131
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.1716
_refine_ls_R_factor_gt            0.1126
_refine_ls_wR_factor_ref          0.3568
_refine_ls_wR_factor_gt           0.2973
_refine_ls_goodness_of_fit_ref    1.250
_refine_ls_restrained_S_all       1.250
_refine_ls_shift/su_max           0.067
_refine_ls_shift/su_mean          0.011
 
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 0.5721(2) 0.9073(2) 0.11592(10) 0.0563(9) Uani 1 1 d . . .
P2 P 0.42180(19) 1.09390(18) 0.04090(8) 0.0397(8) Uani 1 1 d . . .
Al1 Al 0.6588(2) 1.0902(2) 0.03641(15) 0.0645(12) Uani 1 1 d . . .
Al2 Al 0.5661(3) 0.9008(3) 0.22158(15) 0.0714(13) Uani 1 1 d . . .
O1 O 0.6046(7) 0.9386(8) 0.1646(2) 0.076(2) Uani 1 1 d . . .
O2 O 0.4403(5) 0.8596(6) 0.1086(2) 0.0589(19) Uani 1 1 d . . .
O3 O 0.5520(5) 1.1299(6) 0.0396(3) 0.0575(18) Uani 1 1 d . . .
O4 O 0.6002(6) 0.8123(6) 0.1016(2) 0.0592(18) Uani 1 1 d . . .
O5 O 0.6966(6) 0.9966(5) 0.2488(2) 0.0560(19) Uani 1 1 d . . .
O6 O 0.8002(5) 1.2071(5) 0.0386(3) 0.064(2) Uani 1 1 d . . .
O7 O 0.6432(7) 0.9844(7) -0.0009(2) 0.074(2) Uani 1 1 d . . .
O8 O 0.6465(6) 1.0179(6) 0.0884(3) 0.072(2) Uani 1 1 d . . .
O100 O 0.6628(17) 1.1537(17) -0.0359(6) 0.058(5) Uiso 0.33 1 d P . .
N1 N 0.0000 0.0000 0.1066(6) 0.083(5) Uiso 1 3 d SD . .
N2 N 0.0000 0.0000 0.1893(16) 0.231(17) Uiso 1 3 d S . .
C3 C -0.0617(19) 0.0542(19) 0.1193(8) 0.162(8) Uiso 1 1 d . . .
H3A H -0.1417 0.0114 0.1073 0.194 Uiso 1 1 calc R . .
H3B H -0.0234 0.1346 0.1078 0.194 Uiso 1 1 calc R . .
C4 C -0.064(2) 0.055(3) 0.1688(9) 0.212(12) Uiso 1 1 d . . .
H4A H -0.0295 0.1359 0.1794 0.254 Uiso 1 1 calc R . .
H4B H -0.1462 0.0122 0.1789 0.254 Uiso 1 1 calc R . .
C1 C 0.0000 0.0000 0.0244(16) 0.21(2) Uiso 1 3 d SD . .
C2 C -0.077(4) -0.037(8) 0.0642(12) 0.20(3) Uiso 0.33 1 d PD . .
 
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 0.0462(15) 0.0558(17) 0.0675(19) -0.0114(12) -0.0162(12) 0.0260(13)
P2 0.0429(13) 0.0338(12) 0.0490(15) 0.0097(9) 0.0098(10) 0.0242(10)
Al1 0.0306(15) 0.0306(15) 0.128(3) -0.0216(15) -0.0144(16) 0.0122(12)
Al2 0.064(2) 0.0553(19) 0.108(3) -0.0422(18) -0.0481(19) 0.0396(16)
O1 0.082(5) 0.098(6) 0.052(5) -0.026(4) -0.030(4) 0.048(5)
O2 0.045(4) 0.068(4) 0.062(5) -0.006(3) -0.013(3) 0.026(3)
O3 0.041(4) 0.053(4) 0.084(5) 0.007(3) 0.013(3) 0.027(3)
O4 0.058(4) 0.052(4) 0.070(5) 0.001(3) 0.008(3) 0.029(3)
O5 0.062(4) 0.049(4) 0.045(4) 0.001(3) -0.024(3) 0.020(3)
O6 0.044(4) 0.029(3) 0.095(5) -0.003(3) -0.032(3) 0.000(3)
O7 0.071(5) 0.094(6) 0.056(5) -0.023(4) -0.004(4) 0.040(4)
O8 0.067(5) 0.047(4) 0.088(5) 0.013(4) -0.014(4) 0.017(4)
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
P1 O1 1.495(7) . ?
P1 O8 1.510(8) . ?
P1 O4 1.516(7) . ?
P1 O2 1.521(6) . ?
P2 O6 1.488(6) 3_575 ?
P2 O5 1.505(6) 15 ?
P2 O7 1.513(7) 10_675 ?
P2 O3 1.518(6) . ?
Al1 O7 1.694(8) . ?
Al1 O6 1.708(6) . ?
Al1 O3 1.712(6) . ?
Al1 O8 1.764(8) . ?
Al1 O100 2.28(2) . ?
Al2 O5 1.725(7) . ?
Al2 O4 1.732(7) 15 ?
Al2 O2 1.734(7) 14_455 ?
Al2 O1 1.753(9) . ?
Al2 O100 2.354(19) 5_665 ?
O2 Al2 1.734(7) 15 ?
O4 Al2 1.732(7) 14_455 ?
O5 P2 1.505(6) 14_455 ?
O6 P2 1.488(6) 2_775 ?
O7 P2 1.513(7) 10_675 ?
O100 Al2 2.354(19) 9_564 ?
N1 C3 1.36(2) 3 ?
N1 C3 1.36(2) . ?
N1 C3 1.36(2) 2 ?
N1 C2 1.52(2) 2 ?
N1 C2 1.52(2) 3 ?
N1 C2 1.52(2) . ?
N2 C4 1.47(3) 2 ?
N2 C4 1.47(3) 3 ?
N2 C4 1.47(3) . ?
C3 C4 1.46(3) . ?
C3 C2 1.96(6) . ?
C3 C2 2.02(7) 3 ?
C1 C2 1.46(4) . ?
C1 C2 1.46(4) 2 ?
C1 C2 1.46(4) 3 ?
C1 C1 1.44(10) 10 ?
C2 C2 1.51(8) 2 ?
C2 C2 1.51(8) 3 ?
C2 C3 2.02(7) 2 ?
 
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
O1 P1 O8 107.3(5) . . ?
O1 P1 O4 109.9(4) . . ?
O8 P1 O4 109.2(4) . . ?
O1 P1 O2 110.8(4) . . ?
O8 P1 O2 111.6(4) . . ?
O4 P1 O2 108.2(4) . . ?
O6 P2 O5 107.7(4) 3_575 15 ?
O6 P2 O7 107.6(5) 3_575 10_675 ?
O5 P2 O7 110.1(4) 15 10_675 ?
O6 P2 O3 110.9(4) 3_575 . ?
O5 P2 O3 110.0(4) 15 . ?
O7 P2 O3 110.6(4) 10_675 . ?
O7 Al1 O6 112.8(4) . . ?
O7 Al1 O3 119.8(4) . . ?
O6 Al1 O3 114.0(3) . . ?
O7 Al1 O8 100.8(4) . . ?
O6 Al1 O8 102.3(4) . . ?
O3 Al1 O8 104.0(4) . . ?
O7 Al1 O100 70.1(6) . . ?
O6 Al1 O100 83.8(6) . . ?
O3 Al1 O100 79.5(6) . . ?
O8 Al1 O100 170.7(6) . . ?
O5 Al2 O4 112.8(4) . 15 ?
O5 Al2 O2 114.7(4) . 14_455 ?
O4 Al2 O2 116.4(4) 15 14_455 ?
O5 Al2 O1 101.7(4) . . ?
O4 Al2 O1 104.7(4) 15 . ?
O2 Al2 O1 104.4(4) 14_455 . ?
O5 Al2 O100 79.3(6) . 5_665 ?
O4 Al2 O100 76.6(5) 15 5_665 ?
O2 Al2 O100 73.4(5) 14_455 5_665 ?
O1 Al2 O100 177.7(6) . 5_665 ?
P1 O1 Al2 147.4(6) . . ?
P1 O2 Al2 142.5(5) . 15 ?
P2 O3 Al1 149.3(5) . . ?
P1 O4 Al2 144.0(5) . 14_455 ?
P2 O5 Al2 139.6(4) 14_455 . ?
P2 O6 Al1 164.2(5) 2_775 . ?
P2 O7 Al1 148.7(5) 10_675 . ?
P1 O8 Al1 145.1(5) . . ?
Al1 O100 Al2 141.4(9) . 9_564 ?
C3 N1 C3 112.7(11) 3 . ?
C3 N1 C3 112.7(11) 3 2 ?
C3 N1 C3 112.7(11) . 2 ?
C3 N1 C2 89(4) 3 2 ?
C3 N1 C2 141(3) . 2 ?
C3 N1 C2 86(3) 2 2 ?
C3 N1 C2 86(3) 3 3 ?
C3 N1 C2 89(4) . 3 ?
C3 N1 C2 141(3) 2 3 ?
C2 N1 C2 59(3) 2 3 ?
C3 N1 C2 141(3) 3 . ?
C3 N1 C2 86(3) . . ?
C3 N1 C2 89(4) 2 . ?
C2 N1 C2 59(3) 2 . ?
C2 N1 C2 59(3) 3 . ?
C4 N2 C4 104(3) 2 3 ?
C4 N2 C4 104(3) 2 . ?
C4 N2 C4 104(3) 3 . ?
N1 C3 C4 107(2) . . ?
N1 C3 C2 51(2) . . ?
C4 C3 C2 147(3) . . ?
N1 C3 C2 49(2) . 3 ?
C4 C3 C2 145(3) . 3 ?
C2 C3 C2 44(3) . 3 ?
N2 C4 C3 113(3) . . ?
C2 C1 C2 62(3) . 2 ?
C2 C1 C2 62(3) . 3 ?
C2 C1 C2 62(3) 2 3 ?
C2 C1 C1 143.4(19) . 10 ?
C2 C1 C1 143.4(19) 2 10 ?
C2 C1 C1 143.4(19) 3 10 ?
C1 C2 C2 58.9(16) . 2 ?
C1 C2 C2 58.9(16) . 3 ?
C2 C2 C2 60.000(3) 2 3 ?
C1 C2 N1 108(4) . . ?
C2 C2 N1 60.3(17) 2 . ?
C2 C2 N1 60.3(17) 3 . ?
C1 C2 C3 128(5) . . ?
C2 C2 C3 102(3) 2 . ?
C2 C2 C3 70(4) 3 . ?
N1 C2 C3 43.8(16) . . ?
C1 C2 C3 124(5) . 2 ?
C2 C2 C3 66(4) 2 2 ?
C2 C2 C3 100(3) 3 2 ?
N1 C2 C3 42.3(17) . 2 ?
C3 C2 C3 69.3(18) . 2 ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              67.00
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    1.176
_refine_diff_density_min   -0.756
_refine_diff_density_rms    0.221
