#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320461.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_4320461
loop_
_publ_author_name
'Jiyang Li'
'Jihong Yu'
'Kaixue Wang'
'Guangshan Zhu'
'Ruren Xu'
_publ_section_title
;
 A Simulation Study on the Topotactic Transformations from
 Aluminophosphate AlPO4-21 to AlPO4-25
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5812
_journal_page_last               5817
_journal_paper_doi               10.1021/ic010292k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         Al3P3O13H.C2NH8
_chemical_formula_sum            'C2 H9 Al3 N O13 P3'
_chemical_formula_weight         428.95
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.604(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6868(19)
_cell_length_b                   17.428(5)
_cell_length_c                   9.1589(17)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.34
_cell_volume                     1306.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXP'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2722
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.7831
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1748
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0380
_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)+(0.0410P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                1184
_reflns_number_total             1748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010292k.cif
_cod_data_source_block           lijy
_cod_original_cell_volume        1306.3(5)
_cod_database_code               4320461
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_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
H3 H 0.950(5) 0.288(4) 0.602(5) 0.05(2) Uiso 1 1 d D . .
P2 P 0.79627(17) 0.21168(8) 0.97278(18) 0.0153(4) Uani 1 1 d . . .
P1 P 0.34018(17) 0.07040(8) 0.86820(18) 0.0140(4) Uani 1 1 d . . .
P3 P 1.24792(16) 0.33769(8) 1.00510(18) 0.0149(4) Uani 1 1 d . . .
Al1 Al 0.50970(18) 0.16886(9) 0.6897(2) 0.0161(4) Uani 1 1 d . . .
Al2 Al 0.63827(19) 0.11132(9) 1.16384(19) 0.0130(4) Uani 1 1 d . . .
Al3 Al 1.06466(19) 0.20402(9) 0.7973(2) 0.0145(4) Uani 1 1 d . . .
O1 O 0.2806(4) -0.01181(19) 0.8400(4) 0.0157(9) Uani 1 1 d . . .
O4 O 0.6353(4) 0.2267(2) 0.8379(4) 0.0207(10) Uani 1 1 d . . .
O6 O 0.8357(4) 0.28363(19) 1.0745(4) 0.0191(9) Uani 1 1 d . . .
O7 O 0.9329(4) 0.1945(2) 0.9107(4) 0.0210(10) Uani 1 1 d . . .
O8 O 1.1901(4) 0.1211(2) 0.8195(4) 0.0188(9) Uani 1 1 d . . .
O2 O 0.4468(4) 0.0889(2) 0.7680(4) 0.0203(10) Uani 1 1 d . . .
O12 O 1.2333(4) 0.39074(19) 0.8698(4) 0.0178(9) Uani 1 1 d . . .
O11 O 1.2267(4) 0.25376(19) 0.9553(4) 0.0181(9) Uani 1 1 d . . .
O10 O 1.0420(4) 0.2901(2) 0.6788(5) 0.0181(10) Uani 1 1 d D . .
O9 O 0.9149(4) 0.15096(19) 0.6278(4) 0.0179(9) Uani 1 1 d . . .
O5 O 0.7741(4) 0.1438(2) 1.0681(4) 0.0189(9) Uani 1 1 d . . .
O3 O 0.4406(4) 0.08320(19) 1.0376(4) 0.0157(9) Uani 1 1 d . . .
O13 O 1.1173(4) 0.3628(2) 1.0732(4) 0.0244(10) Uani 1 1 d . . .
C1 C 0.1294(9) 0.0641(4) 0.4091(9) 0.059(2) Uani 1 1 d . . .
H1A H 0.0617 0.0595 0.4727 0.080 Uiso 1 1 calc . . .
H1B H 0.1244 0.1157 0.3714 0.080 Uiso 1 1 calc . . .
H1C H 0.2402 0.0516 0.4692 0.080 Uiso 1 1 calc . . .
N1 N 0.0709(6) 0.0111(3) 0.2774(6) 0.0319(14) Uani 1 1 d . . .
H1D H -0.0338 0.0222 0.2227 0.080 Uiso 1 1 calc . . .
H1E H 0.0742 -0.0372 0.3133 0.080 Uiso 1 1 calc . . .
C2 C 0.1696(10) 0.0155(5) 0.1743(9) 0.066(2) Uani 1 1 d . . .
H2A H 0.1276 -0.0201 0.0903 0.080 Uiso 1 1 calc . . .
H2B H 0.2811 0.0028 0.2318 0.080 Uiso 1 1 calc . . .
H2C H 0.1644 0.0666 0.1338 0.080 Uiso 1 1 calc . . .
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
O7 P2 O5 109.2(2) . . ?
O7 P2 O6 110.4(2) . . ?
O5 P2 O6 109.5(2) . . ?
O7 P2 O4 110.3(2) . . ?
O5 P2 O4 109.6(2) . . ?
O6 P2 O4 107.8(2) . . ?
O8 P1 O1 106.9(2) 1_455 . ?
O8 P1 O3 111.0(2) 1_455 . ?
O1 P1 O3 111.0(2) . . ?
O8 P1 O2 109.4(2) 1_455 . ?
O1 P1 O2 109.6(2) . . ?
O3 P1 O2 108.9(2) . . ?
O12 P3 O9 108.8(2) . 4_666 ?
O12 P3 O11 111.8(2) . . ?
O9 P3 O11 109.6(2) 4_666 . ?
O12 P3 O13 106.7(2) . . ?
O9 P3 O13 108.4(2) 4_666 . ?
O11 P3 O13 111.4(2) . . ?
O13 Al1 O6 108.54(19) 4_565 4_565 ?
O13 Al1 O2 107.99(19) 4_565 . ?
O6 Al1 O2 107.65(18) 4_565 . ?
O13 Al1 O4 109.73(19) 4_565 . ?
O6 Al1 O4 112.72(19) 4_565 . ?
O2 Al1 O4 110.08(19) . . ?
O5 Al2 O3 114.81(18) . . ?
O5 Al2 O12 112.23(18) . 4_566 ?
O3 Al2 O12 132.88(19) . 4_566 ?
O5 Al2 O1 88.24(17) . 3_657 ?
O3 Al2 O1 91.13(16) . 3_657 ?
O12 Al2 O1 87.60(17) 4_566 3_657 ?
O5 Al2 O10 97.22(18) . 4_566 ?
O3 Al2 O10 86.86(16) . 4_566 ?
O12 Al2 O10 90.04(18) 4_566 4_566 ?
O1 Al2 O10 174.52(17) 3_657 4_566 ?
O8 Al3 O7 110.12(18) . . ?
O8 Al3 O10 132.50(19) . . ?
O7 Al3 O10 117.31(18) . . ?
O8 Al3 O11 90.86(17) . . ?
O7 Al3 O11 93.18(17) . . ?
O10 Al3 O11 88.99(18) . . ?
O8 Al3 O9 85.59(17) . . ?
O7 Al3 O9 91.91(17) . . ?
O10 Al3 O9 90.37(18) . . ?
O11 Al3 O9 174.56(18) . . ?
P1 O1 Al2 140.2(2) . 3_657 ?
P2 O4 Al1 133.2(2) . . ?
P2 O6 Al1 137.1(2) . 4_666 ?
P2 O7 Al3 159.4(3) . . ?
P1 O8 Al3 160.3(2) 1_655 . ?
P1 O2 Al1 138.5(2) . . ?
P3 O12 Al2 137.1(2) . 4_665 ?
P3 O11 Al3 131.6(2) . . ?
Al3 O10 Al2 144.0(2) . 4_665 ?
Al3 O10 H3 110(4) . . ?
Al2 O10 H3 106(4) 4_665 . ?
P3 O9 Al3 139.7(2) 4_565 . ?
P2 O5 Al2 139.6(2) . . ?
P1 O3 Al2 143.0(2) . . ?
P3 O13 Al1 142.1(3) . 4_666 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 N1 C2 112.2(6) . . ?
C1 N1 H1D 109.2 . . ?
C2 N1 H1D 109.2 . . ?
C1 N1 H1E 109.2 . . ?
C2 N1 H1E 109.2 . . ?
H1D N1 H1E 107.9 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
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
P2 O7 1.508(4) . ?
P2 O5 1.520(4) . ?
P2 O6 1.531(4) . ?
P2 O4 1.546(4) . ?
P1 O8 1.513(4) 1_455 ?
P1 O1 1.516(4) . ?
P1 O3 1.520(4) . ?
P1 O2 1.541(4) . ?
P3 O12 1.517(4) . ?
P3 O9 1.521(3) 4_666 ?
P3 O11 1.525(4) . ?
P3 O13 1.531(4) . ?
Al1 O13 1.728(4) 4_565 ?
Al1 O6 1.736(4) 4_565 ?
Al1 O2 1.737(4) . ?
Al1 O4 1.748(4) . ?
Al2 O5 1.783(4) . ?
Al2 O3 1.787(4) . ?
Al2 O12 1.788(4) 4_566 ?
Al2 O1 1.877(4) 3_657 ?
Al2 O10 1.936(4) 4_566 ?
Al3 O8 1.780(4) . ?
Al3 O7 1.793(4) . ?
Al3 O10 1.823(4) . ?
Al3 O11 1.861(4) . ?
Al3 O9 1.898(4) . ?
O1 Al2 1.877(4) 3_657 ?
O6 Al1 1.736(4) 4_666 ?
O8 P1 1.513(4) 1_655 ?
O12 Al2 1.788(4) 4_665 ?
O10 Al2 1.936(4) 4_665 ?
O10 H3 0.87(2) . ?
O9 P3 1.521(3) 4_565 ?
O13 Al1 1.728(4) 4_666 ?
C1 N1 1.468(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
N1 C2 1.475(8) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
