#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:43:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179860 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/56/7015640.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_7015640
loop_
_publ_author_name
'Wragg, David S.'
'Fullerton, Grace M.'
'Byrne, Peter J.'
'Slawin, Alexandra M. Z.'
'Warren, John E.'
'Teat, Simon J.'
'Morris, Russell E.'
_publ_section_title
;
 Solvothermal aluminophosphate zeotype synthesis with ionic liquid
 precursors.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4926
_journal_page_last               4932
_journal_paper_doi               10.1039/c0dt01788d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'Al2 H O12 P3, C5 H6 N'
_chemical_formula_sum            'C5 H7 Al2 N O12 P3'
_chemical_formula_weight         419.99
_chemical_name_common            'compound 3'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 111.090(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.522(4)
_cell_length_b                   20.101(10)
_cell_length_c                   8.846(4)
_cell_measurement_reflns_used    619
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.73
_cell_measurement_theta_min      2.50
_cell_volume                     1413.8(12)
_computing_cell_refinement       'Bruker Apex'
_computing_data_collection       'Bruker Apex'
_computing_data_reduction        'Bruker Apex'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Platon, (Spek, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_source         'SRS daresbury laboratories'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69390
_diffrn_reflns_av_R_equivalents  0.1238
_diffrn_reflns_av_sigmaI/netI    0.1478
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8570
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0702P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                1662
_reflns_number_total             2882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01788d.txt
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7015640
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.4477(2) 0.59510(8) 0.91713(19) 0.0174(4) Uani 1 1 d . . .
P2 P -0.0490(2) 0.74849(8) 0.92788(19) 0.0176(4) Uani 1 1 d . . .
Al3 Al -0.3157(2) 0.78833(9) 0.5904(2) 0.0169(4) Uani 1 1 d . . .
Al4 Al 0.1897(2) 0.70862(9) 0.7588(2) 0.0171(4) Uani 1 1 d . . .
P5 P 0.4763(2) 0.80782(8) 0.82277(19) 0.0167(4) Uani 1 1 d . . .
O1 O -0.1536(5) 0.7924(2) 0.7880(5) 0.0210(10) Uani 1 1 d . . .
O2 O 0.3183(5) 0.6397(2) 0.7933(5) 0.0219(10) Uani 1 1 d . . .
O3 O 0.0590(5) 0.7019(2) 0.8692(5) 0.0191(10) Uani 1 1 d . . .
O4 O -0.1507(5) 0.7065(2) 0.9988(5) 0.0219(10) Uani 1 1 d . . .
O5 O 0.3018(5) 0.7825(2) 0.8088(5) 0.0219(10) Uani 1 1 d . . .
O6 O 0.4839(5) 0.5402(2) 0.8087(5) 0.0235(11) Uani 1 1 d . . .
O7 O -0.3943(5) 0.7113(2) 0.4854(5) 0.0218(10) Uani 1 1 d . . .
O8 O 0.0686(5) 0.7960(2) 1.0535(5) 0.0204(10) Uani 1 1 d . . .
O9 O -0.4850(5) 0.7832(2) 0.6796(5) 0.0196(10) Uani 1 1 d . . .
O10 O 0.6105(5) 0.6325(2) 1.0017(5) 0.0210(10) Uani 1 1 d . . .
O11 O 0.4704(6) 0.8853(2) 0.8248(5) 0.0216(10) Uani 1 1 d D . .
O12 O 0.3782(5) 0.5642(2) 1.0350(5) 0.0205(10) Uani 1 1 d . . .
N1 N 0.0448(11) 0.9267(4) 0.8231(10) 0.063(2) Uani 1 1 d . . .
H1 H 0.0091 0.8867 0.8242 0.076 Uiso 1 1 calc R . .
C2 C -0.0418(13) 0.9668(6) 0.7043(12) 0.061(3) Uani 1 1 d . . .
H2 H -0.1392 0.9516 0.6235 0.073 Uiso 1 1 calc R . .
C3 C 0.0110(12) 1.0294(6) 0.7004(10) 0.057(3) Uani 1 1 d . . .
H3 H -0.0506 1.0580 0.6178 0.069 Uiso 1 1 calc R . .
C4 C 0.1594(13) 1.0516(5) 0.8213(13) 0.058(3) Uani 1 1 d . . .
H4 H 0.1997 1.0944 0.8189 0.070 Uiso 1 1 calc R . .
C5 C 0.2440(10) 1.0078(6) 0.9443(10) 0.054(3) Uani 1 1 d . . .
H5 H 0.3408 1.0213 1.0282 0.065 Uiso 1 1 calc R . .
C6 C 0.1861(13) 0.9458(5) 0.9420(11) 0.058(3) Uani 1 1 d . . .
H6 H 0.2440 0.9159 1.0232 0.070 Uiso 1 1 calc R . .
H11 H 0.411(11) 0.905(4) 0.723(7) 0.07(3) Uiso 1 1 d D . .
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_
_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
O12 P1 O10 112.4(2) . . ?
O12 P1 O2 112.1(3) . . ?
O10 P1 O2 110.9(3) . . ?
O12 P1 O6 110.3(3) . . ?
O10 P1 O6 107.7(3) . . ?
O2 P1 O6 103.0(2) . . ?
O4 P2 O1 114.2(3) . . ?
O4 P2 O3 107.8(2) . . ?
O1 P2 O3 109.1(3) . . ?
O4 P2 O8 111.9(3) . . ?
O1 P2 O8 105.5(2) . . ?
O3 P2 O8 108.2(2) . . ?
O10 Al3 O1 114.3(2) 4_475 . ?
O10 Al3 O7 122.1(2) 4_475 . ?
O1 Al3 O7 123.5(2) . . ?
O10 Al3 O4 87.7(2) 4_475 4_575 ?
O1 Al3 O4 89.1(2) . 4_575 ?
O7 Al3 O4 91.3(2) . 4_575 ?
O10 Al3 O9 91.8(2) 4_475 . ?
O1 Al3 O9 91.8(2) . . ?
O7 Al3 O9 88.3(2) . . ?
O4 Al3 O9 179.1(2) 4_575 . ?
O2 Al4 O3 109.5(2) . . ?
O2 Al4 O5 112.7(2) . . ?
O3 Al4 O5 109.3(2) . . ?
O2 Al4 O8 104.0(2) . 4_575 ?
O3 Al4 O8 108.9(2) . 4_575 ?
O5 Al4 O8 112.2(2) . 4_575 ?
O9 P5 O7 114.3(3) 1_655 4_676 ?
O9 P5 O5 108.8(2) 1_655 . ?
O7 P5 O5 110.2(3) 4_676 . ?
O9 P5 O11 110.9(3) 1_655 . ?
O7 P5 O11 105.0(2) 4_676 . ?
O5 P5 O11 107.3(3) . . ?
P2 O1 Al3 141.7(3) . . ?
P1 O2 Al4 147.6(3) . . ?
P2 O3 Al4 137.0(3) . . ?
P2 O4 Al3 142.3(3) . 4_576 ?
P5 O5 Al4 137.2(3) . . ?
P5 O7 Al3 135.7(3) 4_475 . ?
P2 O8 Al4 135.3(3) . 4_576 ?
P5 O9 Al3 140.4(3) 1_455 . ?
P1 O10 Al3 140.6(3) . 4_676 ?
P5 O11 H11 115(5) . . ?
C2 N1 C6 122.5(9) . . ?
C2 N1 H1 118.7 . . ?
C6 N1 H1 118.7 . . ?
N1 C2 C3 119.8(9) . . ?
N1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 119.8(8) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 117.9(9) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
C6 C5 C4 119.8(8) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 N1 120.1(8) . . ?
C5 C6 H6 119.9 . . ?
N1 C6 H6 119.9 . . ?
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 O12 1.506(5) . ?
P1 O10 1.518(4) . ?
P1 O2 1.533(4) . ?
P1 O6 1.565(5) . ?
P2 O4 1.500(5) . ?
P2 O1 1.521(4) . ?
P2 O3 1.529(5) . ?
P2 O8 1.533(4) . ?
Al3 O10 1.785(5) 4_475 ?
Al3 O1 1.798(4) . ?
Al3 O7 1.805(5) . ?
Al3 O4 1.861(5) 4_575 ?
Al3 O9 1.880(5) . ?
Al4 O2 1.724(5) . ?
Al4 O3 1.732(5) . ?
Al4 O5 1.734(5) . ?
Al4 O8 1.739(4) 4_575 ?
P5 O9 1.503(5) 1_655 ?
P5 O7 1.514(4) 4_676 ?
P5 O5 1.535(5) . ?
P5 O11 1.559(5) . ?
O11 H11 0.94(4) . ?
N1 C2 1.319(12) . ?
N1 C6 1.339(12) . ?
N1 H1 0.8600 . ?
C2 C3 1.342(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.403(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.337(14) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11 O12 0.94(4) 1.70(6) 2.602(6) 158(9) 4_575
