# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_KPreAFY
_database_code_depnum_ccdc_archive 'CCDC 1987816'
loop_
_audit_author_name
_audit_author_address
'Kazuyuki Maeda'
;Tokyo University of Agriculture and Technology
Japan
;
_audit_update_record             
;
2020-03-03 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_KPreAFY             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        Ow7 Check
RESPONSE: H atoms are not included in the Rietveld refinement.
;
_vrf_DENSD01_KPreAFY             
;
PROBLEM: The ratio of the submitted crystal density and that
RESPONSE: Use of virtual atoms Ow7, Ow8, and Ow9 representing H2O makes small inconsistency between the compositional formula and the refined composition.
;
_vrf_PLAT046_KPreAFY             
;
PROBLEM: Reported Z, MW and D(calc) are Inconsistent ....      1.890 Check
RESPONSE: Use of virtual atoms Ow7, Ow8, and Ow9 representing H2O makes small inconsistency between the compositional formula and the refined composition.
;
# Added during the CSD deposition process: Tuesday 03 March 2020 11:37 AM
# end Validation Reply Form



_symmetry_space_group_name_hall  '-P 3'
#Added by publCIF




_exptl_absorpt_correction_T_min  ?
#Added by publCIF




_refine_ls_structure_factor_coef ?
#Added by publCIF




_pd_proc_info_excluded_regions   none
#Added by publCIF




_diffrn_radiation_monochromator  none
#Added by publCIF



# 5. CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            K-PreAFY
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety         '2(Al3 O16 P4), 6(O1.48), 0.50(O), 6(K)'
_chemical_formula_sum            'Al6 K6 O41.38 P8'
_chemical_formula_weight         1306.32


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0715 0.0658 'International Tables for Crystallography, Vol. C'
K K 0.2137 0.3152 'International Tables for Crystallography, Vol. C'
O O 0.0113 0.0079 'International Tables for Crystallography, Vol. C'
P P 0.1127 0.1202 'International Tables for Crystallography, Vol. C'
H H -0.0006 0.0000 'International Tables for Crystallography, Vol. C'
C C 0.0033 0.0021 'International Tables for Crystallography, Vol. C'

#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
_space_group_IT_number           147

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,-z
5 y,-x+y,-z
6 x-y,x,-z

_cell_length_a                   12.925(1)
_cell_length_b                   12.925(1)
_cell_length_c                   7.9339(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1147.8(2)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z            1
_cell_measurement_temperature    300
_exptl_crystal_density_diffrn    1.9175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             661.95
_exptl_crystal_description       powder

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              20.0 # perpendicular to
# equatorial plane

_pd_spec_size_equat              0.05 # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              0.05 # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; 'Lindemann glass capillary'
;
_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder

_pd_char_colour                  colorless

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
K-PreAFY was obtained by a cation exchange of [BuNH3]3[Al3P4O16] with 
potassium acetate in a 1:1 (v/v) CH3OH/CH3CN mixed solvent.  Since the 
resulting K-PreAFY powder considerably lost the crystallinity without the 
solvent, it was stored with the mother liquor prior to the measurement.  
;
# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; BL02B2, SPring-8 (Japan) 
;
_diffrn_ambient_temperature      300
_diffrn_source                   'Synchrotron radiation'
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'Multiple Si microstrip detectors'
_diffrn_detector_type            'MYTHEN detector'

_pd_meas_scan_method             step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;
K-PreAFY stored in the mother liquor was used for the measurement.  The sample 
with the mother liquor was loaded in a 0.5 mm Lindemann glass capillary, the 
powder was deposited in the end of capillary, and the capillary was sealed 
with the liquid.  
;
_diffrn_radiation_wavelength     0.79940

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        12686
_pd_meas_2theta_range_min        2.1000
_pd_meas_2theta_range_max        78.2100
_pd_meas_2theta_range_inc        0.0060

#===============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      ?

# The next three items are given as text.

_pd_calc_method                  'Rietveld Refinement'

_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     ?
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)

_pd_proc_ls_prof_R_factor        0.05092
_pd_proc_ls_prof_wR_factor       0.07065
_pd_proc_ls_prof_wR_expected     0.01089
_refine_ls_R_I_factor            0.01792
_refine_ls_R_Fsqd_factor         0.00851
_refine_ls_R_factor_all          0.00859

_refine_special_details          
; 
The virtual chemical species Ow (1O and 2H) were introduced for Ow7, Ow8, 
and Ow9 to simulate water molecules.  However, also methanol or acetonitrile 
molecules should be actually included in the mother liquor, though the 
composition cannot be readily determined.  Therefore, no geometrical 
restraints were given for their coordinates and the displacement parameters 
for these species were fixed at Biso = 4.  According to the final coordinates, 
the distance of Ow7-Ow9 is 1.35 angstrom, which can be regarded as C-O 
distance of a methanol molecule.  However, the inconsistency is left as it is 
because of no information on the composition.

The model was refined in the Rietveld method with soft geometrical restraints 
[prescribed distances/angstrom: Al-O 1.73(3), P-O 1.52(3); prescribed 
angles/: C-C-C(H) 120.0(9), O-Al(P)-O 109(3), Al-O-P 145(13)].  To 
stabilize the refinement, the displacement parameters for all the framework 
atoms (Al, P and framework O) were constrained to be the same.  An anisotropic 
profile broadening parameters Ue and Pe on the 001 axis were also refined.
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/yi
# The following line must be commented out in the absence of H atoms.
#_refine_ls_hydrogen_treatment      none
_refine_ls_extinction_method     none
_refine_ls_number_parameters     68
_refine_ls_number_restraints     34
_refine_ls_number_constraints    8

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   6.4863

# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max          0.0
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         0.0
_refine_diff_density_min         0.0

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        3.0060
_pd_proc_2theta_range_max        39.9960
_pd_proc_2theta_range_inc        0.0060


# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       ?

# The following items are used to identify the programs used.

_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_structure_solution    'EXPO-2014 (Altomare et al., 2013)'
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Al1 0.4750(5) 0.3206(7) 0.008(1) 1 6 g Uiso 0.001(1) Al
K1 0.1303(7) 0.4461(7) 0.524(1) 1 6 g Uiso 0.070(3) K
P1 0.4309(7) 0.0931(5) 0.179(1) 1 6 g Uiso 0.001(1) P
P2 0.33333 0.66667 0.241(2) 1 2 d Uiso 0.001(1) P
O1 0.0113(6) 0.370(1) 0.068(1) 1 6 g Uiso 0.001(1) O
O2 0.242(1) 0.5493(8) 0.171(1) 1 6 g Uiso 0.001(1) O
O3 0.407(1) 0.193(1) 0.124(2) 1 6 g Uiso 0.001(1) O
O4 0.565(1) 0.138(1) 0.146(2) 1 6 g Uiso 0.001(1) O
O5 0.403(1) 0.062(1) 0.368(2) 1 6 g Uiso 0.001(1) O
O6 0.33333 0.66667 0.429(2) 1 2 d Uiso 0.001(1) O
Ow7 0.216(1) 0.084(2) 0.650(2) 1 6 g Uiso 0.05066 O
Ow8 0 0 0 0.50(4) 1 a Uiso 0.05066 O
Ow9 0.287(3) 0.050(2) 0.727(4) 0.48(1) 6 g Uiso 0.05066 O

#===============================================================================

#10. GEOMETRICAL PARAMETERS

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O3 1.70(2) . 1_555 ?
Al1 O1 1.765(2) . 5_555 ?
Al1 O4 1.765(4) . 3_665 ?
Al1 O2 1.767(1) . 5_555 ?
P1 O1 1.49(1) . 3_555 ?
P1 O3 1.53(2) . 1_555 ?
P1 O5 1.55(2) . 1_555 ?
P1 O4 1.552(5) . 1_555 ?
P2 O6 1.490(3) . 1_555 ?
P2 O2 1.490(2) . 1_555 ?
P2 O2 1.490(2) . 3_565 ?
P2 O2 1.490(2) . 2_665 ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Al1 O1 111.0(8) 1_555 . 5_555 ?
O3 Al1 O4 106.5(9) 1_555 . 3_665 ?
O3 Al1 O2 112.4(8) 1_555 . 5_555 ?
O1 Al1 O4 107.9(8) 5_555 . 3_665 ?
O1 Al1 O2 106.5(7) 5_555 . 5_555 ?
O4 Al1 O2 112.5(8) 3_665 . 5_555 ?
O1 P1 O3 107(1) 3_555 . 1_555 ?
O1 P1 O5 112.470(7) 3_555 . 1_555 ?
O1 P1 O4 108(1) 3_555 . 1_555 ?
O3 P1 O5 112(1) 1_555 . 1_555 ?
O3 P1 O4 107.1(8) 1_555 . 1_555 ?
O5 P1 O4 109.3(9) 1_555 . 1_555 ?
O6 P2 O2 111.9(7) 1_555 . 1_555 ?
O6 P2 O2 111.9(7) 1_555 . 3_565 ?
O6 P2 O2 111.9(7) 1_555 . 2_665 ?
O2 P2 O2 106.9(7) 1_555 . 3_565 ?
O2 P2 O2 106.9(7) 1_555 . 2_665 ?
O2 P2 O2 106.9(7) 3_565 . 2_665 ?
P1 O1 Al1 151(1) 2_555 . 6_555 ?
P2 O2 Al1 145(1) 1_555 . 6_555 ?
P1 O3 Al1 139(1) 1_555 . 1_555 ?
P1 O4 Al1 150(1) 1_555 . 2_655 ?
