# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1443007'
_audit_update_record             
;
2015-12-22 deposited with the CCDC.
2016-03-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Al4.68 B8 La2 O22'
_chemical_formula_sum            'Al4.68 B8 La2 O22'
_chemical_formula_weight         842.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   p-62m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   4.6149(7)
_cell_length_b                   4.6149(7)
_cell_length_c                   18.720(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     345.27(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    153.1500
_cell_measurement_reflns_used    1354
_cell_measurement_theta_min      2.1759
_cell_measurement_theta_max      31.3481

_exptl_crystal_description       Chip
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2900
_exptl_crystal_size_mid          0.1800
_exptl_crystal_size_min          0.1650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             390.8
_exptl_absorpt_coefficient_mu    6.557
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153.1500
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Molybdenum
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3414
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         31.35
_reflns_number_total             475
_reflns_number_gt                403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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 > 2sigma(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)+(0.0843P)²+0.0910P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_number_reflns         475
_refine_ls_number_parameters     41
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1322
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_restrained_S_all      1.204
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.0000 0.0000 0.0000 0.0059(3) Uani 1 12 d S . .
La2 La 0.0000 0.0000 0.5000 0.0054(3) Uani 1 12 d S . .
Al1 Al 0.3896(11) 0.3896(11) 0.24972(6) 0.0086(8) Uani 0.78 2 d SP . .
O1 O 0.0000 0.0000 0.2525(5) 0.040(5) Uani 1 6 d S . .
O2 O 0.6667 0.3333 0.1873(3) 0.0025(7) Uani 1 3 d SU . .
O3 O 0.5760(8) 0.0000 0.08003(15) 0.0118(9) Uani 1 2 d S . .
O4 O 0.4294(7) 0.0000 0.41920(14) 0.0076(7) Uani 1 2 d SU . .
O5 O 0.6667 0.3333 0.3127(2) 0.0016(7) Uani 1 3 d SU . .
B1 B 0.6667 0.3333 0.1103(4) 0.0051(13) Uani 1 3 d S . .
B2 B 0.6667 0.3333 0.3880(4) 0.0027(9) Uani 1 3 d SU . .

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
La1 0.0063(4) 0.0063(4) 0.0052(4) 0.000 0.000 0.00316(19)
La2 0.0041(4) 0.0041(4) 0.0080(5) 0.000 0.000 0.00204(19)
Al1 0.0061(13) 0.0061(13) 0.0137(17) 0.0002(3) 0.0002(3) 0.0032(16)
O1 0.015(4) 0.015(4) 0.091(16) 0.000 0.000 0.007(2)
O2 0.0029(8) 0.0029(8) 0.0018(10) 0.000 0.000 0.0015(4)
O3 0.0151(17) 0.0112(14) 0.0079(13) 0.000 0.0053(11) 0.0056(7)
O4 0.0070(10) 0.0080(9) 0.0081(9) 0.000 0.0005(7) 0.0040(4)
O5 0.0018(8) 0.0018(8) 0.0011(10) 0.000 0.000 0.0009(4)
B1 0.006(2) 0.006(2) 0.003(3) 0.000 0.000 0.0032(10)
B2 0.0028(9) 0.0028(9) 0.0024(13) 0.000 0.000 0.0014(5)

_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
La1 O3 2.464(3) 3_665 ?
La1 O3 2.464(3) 4_455 ?
La1 O3 2.464(3) 5_545 ?
La1 O3 2.464(3) 6_665 ?
La1 O3 2.464(3) 1_455 ?
La1 O3 2.464(3) 2_545 ?
La2 O4 2.493(3) 3 ?
La2 O4 2.493(3) 5_556 ?
La2 O4 2.493(3) 4_556 ?
La2 O4 2.493(3) 6_556 ?
La2 O4 2.493(3) . ?
La2 O4 2.493(3) 2 ?
Al1 O1 1.799(5) . ?
Al1 O2 1.844(3) 10 ?
Al1 O2 1.844(3) . ?
Al1 O5 1.851(3) 10 ?
Al1 O5 1.851(3) . ?
Al1 Al1 2.471(3) 3_665 ?
Al1 Al1 2.471(3) 2_665 ?
Al1 Al1 2.471(3) 2_655 ?
Al1 Al1 2.471(3) 3_565 ?
O1 Al1 1.799(5) 3 ?
O1 Al1 1.799(5) 2 ?
O2 B1 1.442(9) . ?
O2 Al1 1.844(3) 3_665 ?
O2 Al1 1.844(3) 2_655 ?
O3 B1 1.490(3) . ?
O3 B1 1.490(3) 10_545 ?
O3 La1 2.464(3) 1_655 ?
O4 B2 1.491(3) 10_545 ?
O4 B2 1.491(3) . ?
O5 B2 1.410(9) . ?
O5 Al1 1.851(3) 2_655 ?
O5 Al1 1.851(3) 3_665 ?
B1 O3 1.490(3) 2_655 ?
B1 O3 1.490(3) 3_665 ?
B2 O4 1.491(3) 2_655 ?
B2 O4 1.491(3) 3_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_3
_geom_angle_publ_flag
O3 La1 O3 133.22(5) 3_665 4_455 ?
O3 La1 O3 133.22(5) 3_665 5_545 ?
O3 La1 O3 86.88(11) 4_455 5_545 ?
O3 La1 O3 74.88(15) 3_665 6_665 ?
O3 La1 O3 86.88(11) 4_455 6_665 ?
O3 La1 O3 86.88(11) 5_545 6_665 ?
O3 La1 O3 86.88(11) 3_665 1_455 ?
O3 La1 O3 74.88(15) 4_455 1_455 ?
O3 La1 O3 133.22(5) 5_545 1_455 ?
O3 La1 O3 133.22(5) 6_665 1_455 ?
O3 La1 O3 86.88(11) 3_665 2_545 ?
O3 La1 O3 133.22(5) 4_455 2_545 ?
O3 La1 O3 74.88(15) 5_545 2_545 ?
O3 La1 O3 133.22(5) 6_665 2_545 ?
O3 La1 O3 86.88(11) 1_455 2_545 ?
O4 La2 O4 133.16(5) 3 5_556 ?
O4 La2 O4 133.16(5) 3 4_556 ?
O4 La2 O4 87.01(10) 5_556 4_556 ?
O4 La2 O4 74.71(14) 3 6_556 ?
O4 La2 O4 87.01(10) 5_556 6_556 ?
O4 La2 O4 87.01(10) 4_556 6_556 ?
O4 La2 O4 87.01(10) 3 . ?
O4 La2 O4 133.16(5) 5_556 . ?
O4 La2 O4 74.71(14) 4_556 . ?
O4 La2 O4 133.16(5) 6_556 . ?
O4 La2 O4 87.01(10) 3 2 ?
O4 La2 O4 74.71(14) 5_556 2 ?
O4 La2 O4 133.16(5) 4_556 2 ?
O4 La2 O4 133.16(5) 6_556 2 ?
O4 La2 O4 87.01(10) . 2 ?
O1 Al1 O2 107.1(2) . 10 ?
O1 Al1 O2 107.1(2) . . ?
O2 Al1 O2 92.5(2) 10 . ?
O1 Al1 O5 104.9(2) . 10 ?
O2 Al1 O5 78.9(2) 10 10 ?
O2 Al1 O5 148.0(3) . 10 ?
O1 Al1 O5 104.9(2) . . ?
O2 Al1 O5 148.0(3) 10 . ?
O2 Al1 O5 78.9(2) . . ?
O5 Al1 O5 92.1(2) 10 . ?
O1 Al1 Al1 140.91(18) . 3_665 ?
O2 Al1 Al1 103.9(3) 10 3_665 ?
O2 Al1 Al1 47.93(9) . 3_665 ?
O5 Al1 Al1 103.9(3) 10 3_665 ?
O5 Al1 Al1 48.12(9) . 3_665 ?
O1 Al1 Al1 140.91(18) . 2_665 ?
O2 Al1 Al1 47.93(9) 10 2_665 ?
O2 Al1 Al1 103.9(3) . 2_665 ?
O5 Al1 Al1 48.12(9) 10 2_665 ?
O5 Al1 Al1 103.9(3) . 2_665 ?
Al1 Al1 Al1 78.1(4) 3_665 2_665 ?
O1 Al1 Al1 80.94(18) . 2_655 ?
O2 Al1 Al1 139.22(12) 10 2_655 ?
O2 Al1 Al1 47.93(9) . 2_655 ?
O5 Al1 Al1 138.96(12) 10 2_655 ?
O5 Al1 Al1 48.12(9) . 2_655 ?
Al1 Al1 Al1 60.0 3_665 2_655 ?
Al1 Al1 Al1 138.1(4) 2_665 2_655 ?
O1 Al1 Al1 80.94(18) . 3_565 ?
O2 Al1 Al1 47.93(9) 10 3_565 ?
O2 Al1 Al1 139.22(12) . 3_565 ?
O5 Al1 Al1 48.12(9) 10 3_565 ?
O5 Al1 Al1 138.96(12) . 3_565 ?
Al1 Al1 Al1 138.1(4) 3_665 3_565 ?
Al1 Al1 Al1 60.0 2_665 3_565 ?
Al1 Al1 Al1 161.9(4) 2_655 3_565 ?
Al1 O1 Al1 119.92(3) . 3 ?
Al1 O1 Al1 119.92(3) . 2 ?
Al1 O1 Al1 119.92(3) 3 2 ?
B1 O2 Al1 129.31(12) . 3_665 ?
B1 O2 Al1 129.31(12) . 2_655 ?
Al1 O2 Al1 84.14(18) 3_665 2_655 ?
B1 O2 Al1 129.31(12) . . ?
Al1 O2 Al1 84.14(18) 3_665 . ?
Al1 O2 Al1 84.14(18) 2_655 . ?
B1 O3 B1 126.9(5) . 10_545 ?
B1 O3 La1 114.7(2) . 1_655 ?
B1 O3 La1 114.72(19) 10_545 1_655 ?
B2 O4 B2 126.7(5) 10_545 . ?
B2 O4 La2 114.29(19) 10_545 . ?
B2 O4 La2 114.29(19) . . ?
B2 O5 Al1 129.58(12) . 2_655 ?
B2 O5 Al1 129.58(12) . 3_665 ?
Al1 O5 Al1 83.75(17) 2_655 3_665 ?
B2 O5 Al1 129.58(12) . . ?
Al1 O5 Al1 83.75(17) 2_655 . ?
Al1 O5 Al1 83.75(17) 3_665 . ?
O2 B1 O3 112.4(3) . . ?
O2 B1 O3 112.4(3) . 2_655 ?
O3 B1 O3 106.4(3) . 2_655 ?
O2 B1 O3 112.4(3) . 3_665 ?
O3 B1 O3 106.4(3) . 3_665 ?
O3 B1 O3 106.4(3) 2_655 3_665 ?
O5 B2 O4 113.1(3) . 2_655 ?
O5 B2 O4 113.1(3) . . ?
O4 B2 O4 105.7(3) 2_655 . ?
O5 B2 O4 113.1(3) . 3_665 ?
O4 B2 O4 105.7(3) 2_655 3_665 ?
O4 B2 O4 105.7(3) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        31.35
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.620
_refine_diff_density_min         -3.258
_refine_diff_density_rms         0.343
