# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1510859'
_audit_update_record             
;
2016-10-20 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Al3 O (H2 O)2 (O H) (C16 H6 N2 O8)1.5, 1.5(H2 O)'
_chemical_formula_sum            'C24 H17 Al3 N3 O17.50'
_chemical_formula_weight         708.34

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'
Al Al 0.2130 0.2455 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   21.4934(5)
_cell_length_b                   21.4934(5)
_cell_length_c                   21.4934(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9929.2(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    9196
_cell_measurement_theta_min      4.11
_cell_measurement_theta_max      67.35

_exptl_crystal_description       'square pyramid'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.948
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    1.182
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0669 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.8672.
The λ/2 correction factor is 0.00150.
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\ms'
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            34324
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         5.040
_diffrn_reflns_theta_max         66.524
_diffrn_reflns_theta_full        66.524
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2916
_reflns_number_gt                2806
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_max     0.986
_reflns_Friedel_fraction_full    0.986

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material  
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'

_refine_special_details          
;A full list of restraints and constraints is contained
 within the CIF file. Water hydrogen atoms were found from the difference
 Fourier map and refined isotropically with Uiso(H) = 1.5 Ueq(O).
 O6-H and H6a...H6b distances were restrained to 0.87(1) and 1.42(1) A,
 respectively. H6a and H6b occupancies were fixed at 1 and 2/3 (H6a is present
 in the case of O6 is water or hydroxyl group atom; H6b is present only
 in the case when O6 is a water oxygen atom),, SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0644P)²+1.4289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1235 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2916
_refine_ls_number_parameters     154
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.26072(3) 0.19852(3) 0.31923(3) 0.02086(19) Uani 1 1 d . . . . .
C1 C 0.45670(11) 0.21435(14) 0.33007(13) 0.0342(6) Uani 1 1 d . . . . .
C2 C 0.51089(11) 0.21889(12) 0.29435(13) 0.0321(6) Uani 1 1 d . . . . .
H2 H 0.5089 0.2301 0.2516 0.038 Uiso 1 1 calc R U . . .
C3 C 0.56837(11) 0.20653(13) 0.32299(13) 0.0353(6) Uani 1 1 d . . . . .
C4 C 0.57052(13) 0.1952(2) 0.38539(14) 0.0633(11) Uani 1 1 d . . . . .
H4 H 0.6096 0.1887 0.4050 0.076 Uiso 1 1 calc R U . . .
C5 C 0.51682(13) 0.1930(3) 0.42029(15) 0.0755(14) Uani 1 1 d . . . . .
C6 C 0.45909(12) 0.2023(2) 0.39172(13) 0.0619(11) Uani 1 1 d . . . . .
H6 H 0.4219 0.2003 0.4155 0.074 Uiso 1 1 calc R U . . .
C7 C 0.39346(10) 0.22341(11) 0.30089(12) 0.0282(5) Uani 1 1 d . . . . .
C8 C 0.62813(10) 0.20719(11) 0.28809(12) 0.0259(5) Uani 1 1 d . . . . .
N1 N 0.52400(12) 0.1912(2) 0.48586(13) 0.0911(14) Uani 1 1 d . . . . .
O1 O 0.34830(7) 0.19978(8) 0.33058(8) 0.0324(4) Uani 1 1 d . . . . .
O2 O 0.38945(7) 0.25297(8) 0.25128(9) 0.0329(4) Uani 1 1 d . . . . .
O3 O 0.67323(7) 0.18120(9) 0.31413(8) 0.0338(4) Uani 1 1 d . . . . .
O4 O 0.62961(7) 0.23320(9) 0.23604(9) 0.0322(4) Uani 1 1 d . . . . .
O5 O 0.25938(7) 0.25938(7) 0.25938(7) 0.0165(5) Uani 1 3 d S T P . .
O6 O 0.26163(9) 0.13362(10) 0.38139(9) 0.0415(5) Uani 1 1 d D . . . .
H6A H 0.2872(14) 0.1272(17) 0.4139(12) 0.062 Uiso 1 1 d D U . . .
H6B H 0.237(2) 0.1008(16) 0.381(2) 0.062 Uiso 0.6667 1 d D U P . .
O1W O 0.3045(4) 0.1436(6) 0.5081(4) 0.155(5) Uani 0.5 1 d . . P . .


_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 1.8348(6) . ?
Al1 O2 1.8952(19) 12 ?
Al1 O1 1.8982(16) . ?
Al1 O3 1.9002(16) 21_455 ?
Al1 O4 1.903(2) 4_545 ?
Al1 O6 1.9318(17) . ?
C1 C6 1.351(4) . ?
C1 C2 1.398(4) . ?
C1 C7 1.510(3) . ?
C2 C3 1.406(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.364(4) . ?
C3 C8 1.487(3) . ?
C4 C5 1.377(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(4) . ?
C5 N1 1.418(4) . ?
C6 H6 0.9500 . ?
C7 O2 1.244(3) . ?
C7 O1 1.268(3) . ?
C8 O4 1.251(3) . ?
C8 O3 1.251(3) . ?
N1 N1 1.197(6) 9_656 ?
O2 Al1 1.8952(19) 11 ?
O3 Al1 1.9001(16) 21 ?
O4 Al1 1.903(2) 2 ?
O5 Al1 1.8348(6) 12 ?
O5 Al1 1.8348(6) 11 ?
O6 H6A 0.899(13) . ?
O6 H6B 0.879(13) . ?

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 O2 97.49(9) . 12 ?
O5 Al1 O1 95.48(8) . . ?
O2 Al1 O1 88.64(8) 12 . ?
O5 Al1 O3 94.76(7) . 21_455 ?
O2 Al1 O3 90.14(8) 12 21_455 ?
O1 Al1 O3 169.75(8) . 21_455 ?
O5 Al1 O4 96.79(8) . 4_545 ?
O2 Al1 O4 165.65(8) 12 4_545 ?
O1 Al1 O4 91.34(9) . 4_545 ?
O3 Al1 O4 87.33(8) 21_455 4_545 ?
O5 Al1 O6 179.17(12) . . ?
O2 Al1 O6 83.24(9) 12 . ?
O1 Al1 O6 84.92(8) . . ?
O3 Al1 O6 84.84(8) 21_455 . ?
O4 Al1 O6 82.47(9) 4_545 . ?
C6 C1 C2 121.3(2) . . ?
C6 C1 C7 117.8(2) . . ?
C2 C1 C7 120.9(2) . . ?
C1 C2 C3 118.6(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.6(2) . . ?
C4 C3 C8 117.9(2) . . ?
C2 C3 C8 122.4(2) . . ?
C3 C4 C5 120.9(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 N1 116.8(3) . . ?
C6 C5 N1 122.4(3) . . ?
C1 C6 C5 119.5(3) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
O2 C7 O1 125.7(2) . . ?
O2 C7 C1 119.0(2) . . ?
O1 C7 C1 115.4(2) . . ?
O4 C8 O3 125.4(2) . . ?
O4 C8 C3 118.5(2) . . ?
O3 C8 C3 116.1(2) . . ?
N1 N1 C5 114.2(3) 9_656 . ?
C7 O1 Al1 134.45(16) . . ?
C7 O2 Al1 127.79(15) . 11 ?
C8 O3 Al1 134.83(16) . 21 ?
C8 O4 Al1 127.49(15) . 2 ?
Al1 O5 Al1 119.999(1) 12 11 ?
Al1 O5 Al1 120.001(1) 12 . ?
Al1 O5 Al1 120.0 11 . ?
Al1 O6 H6A 131(2) . . ?
Al1 O6 H6B 124(3) . . ?
H6A O6 H6B 105(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 4.2(5) . . . . ?
C7 C1 C2 C3 -176.4(2) . . . . ?
C1 C2 C3 C4 -4.9(4) . . . . ?
C1 C2 C3 C8 177.0(2) . . . . ?
C2 C3 C4 C5 2.8(6) . . . . ?
C8 C3 C4 C5 -179.0(4) . . . . ?
C3 C4 C5 C6 0.1(8) . . . . ?
C3 C4 C5 N1 -169.9(4) . . . . ?
C2 C1 C6 C5 -1.4(6) . . . . ?
C7 C1 C6 C5 179.3(4) . . . . ?
C4 C5 C6 C1 -0.9(8) . . . . ?
N1 C5 C6 C1 168.5(4) . . . . ?
C6 C1 C7 O2 157.5(3) . . . . ?
C2 C1 C7 O2 -21.9(4) . . . . ?
C6 C1 C7 O1 -22.0(4) . . . . ?
C2 C1 C7 O1 158.6(2) . . . . ?
C4 C3 C8 O4 -161.2(3) . . . . ?
C2 C3 C8 O4 16.9(4) . . . . ?
C4 C3 C8 O3 18.7(4) . . . . ?
C2 C3 C8 O3 -163.2(2) . . . . ?
C4 C5 N1 N1 177.9(4) . . . 9_656 ?
C6 C5 N1 N1 8.2(6) . . . 9_656 ?
O2 C7 O1 Al1 -2.2(4) . . . . ?
C1 C7 O1 Al1 177.28(18) . . . . ?
O5 Al1 O1 C7 -12.7(3) . . . . ?
O2 Al1 O1 C7 -110.1(2) 12 . . . ?
O3 Al1 O1 C7 166.7(5) 21_455 . . . ?
O4 Al1 O1 C7 84.3(2) 4_545 . . . ?
O6 Al1 O1 C7 166.6(2) . . . . ?
O1 C7 O2 Al1 -10.9(4) . . . 11 ?
C1 C7 O2 Al1 169.70(17) . . . 11 ?
O4 C8 O3 Al1 14.3(4) . . . 21 ?
C3 C8 O3 Al1 -165.59(19) . . . 21 ?
O3 C8 O4 Al1 1.7(4) . . . 2 ?
C3 C8 O4 Al1 -178.37(17) . . . 2 ?
O2 Al1 O5 Al1 -49.30(16) 12 . . 12 ?
O1 Al1 O5 Al1 -138.64(15) . . . 12 ?
O3 Al1 O5 Al1 41.47(17) 21_455 . . 12 ?
O4 Al1 O5 Al1 129.35(16) 4_545 . . 12 ?
O2 Al1 O5 Al1 130.24(15) 12 . . 11 ?
O1 Al1 O5 Al1 40.90(17) . . . 11 ?
O3 Al1 O5 Al1 -138.98(15) 21_455 . . 11 ?
O4 Al1 O5 Al1 -51.11(16) 4_545 . . 11 ?

_refine_diff_density_max         0.320
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.050

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 1002 331 ' '
2 -0.074 -0.045 0.461 3128 1193 ' '
3 0.500 0.500 0.500 1002 330 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_PLAT213_shelx               
;
PROBLEM: Atom C6              has ADP max/min Ratio .....        3.2 prolat
RESPONSE: This alert is caused by large thermal motions of flat ligand
 molecules towards the voids in the structure.
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.7 Note  
RESPONSE: This alert is caused by large thermal motions of flat ligand
 molecules towards the voids in the structure.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.595          8 Report
RESPONSE: These reflexes were excluded from the refinement
 due to the bad statistics.
;
# end Validation Reply Form





