# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 1421016'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Si3 Al2 O12 Na2 H4'
_chemical_formula_sum            'Si3 Al2 O12 Na2 H4'
_chemical_formula_weight         380.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   F2dd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z'
'x+1/4, -y+1/4, z+1/4'
'x+1/4, y+1/4, -z+1/4'
'x, y+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/4, -y+3/4, z+3/4'
'x+1/4, y+3/4, -z+3/4'
'x+1/2, y, z+1/2'
'x+1/2, -y, -z+1/2'
'x+3/4, -y+1/4, z+3/4'
'x+3/4, y+1/4, -z+3/4'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'x+3/4, -y+3/4, z+1/4'
'x+3/4, y+3/4, -z+1/4'

_cell_length_a                   6.5880(2)
_cell_length_b                   18.2780(2)
_cell_length_c                   18.6130(2)
_cell_angle_alpha                90.0000(12)
_cell_angle_beta                 90.0000(12)
_cell_angle_gamma                90.0000(12)
_cell_volume                     2241.29(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10189
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      50.58

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_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  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16556
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         50.56
_reflns_number_total             5590
_reflns_number_gt                5195
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0294P)²+8.5658P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_number_reflns         5590
_refine_ls_number_parameters     95
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0807
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0.001
_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
Si1 Si 0.70390(4) 0.402879(13) 0.038318(13) 0.00407(4) Uani 1 1 d . . .
Si2 Si 0.33114(6) 0.5000 0.0000 0.00415(5) Uani 1 2 d S . .
Al3 Al 0.94652(5) 0.463068(15) -0.094197(14) 0.00393(4) Uani 1 1 d . . .
Na1 Na 0.94882(9) 0.27928(2) -0.03061(2) 0.00807(6) Uani 1 1 d . . .
O1 O 0.83274(13) 0.40158(4) -0.03547(4) 0.00703(9) Uani 1 1 d . . .
O2 O 0.47099(12) 0.42986(4) 0.02221(4) 0.00783(10) Uani 1 1 d . . .
O3 O 0.69116(13) 0.31933(3) 0.06744(3) 0.00565(8) Uani 1 1 d . . .
O4 O 0.80656(12) 0.45602(4) 0.09755(4) 0.00681(9) Uani 1 1 d . . .
O5 O 0.19758(13) 0.52226(4) 0.06911(4) 0.00755(9) Uani 1 1 d . . .
O1W O 1.19243(16) 0.30621(5) 0.06025(4) 0.01037(10) Uani 1 1 d . . .
H1 H 1.246(5) 0.3437(16) 0.0595(16) 0.026(7) Uiso 1 1 d . . .
H2 H 1.138(4) 0.3025(16) 0.0981(15) 0.023(7) Uiso 1 1 d . . .

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
Si1 0.00453(9) 0.00371(7) 0.00396(7) 0.00023(6) 0.00011(7) -0.00004(7)
Si2 0.00351(12) 0.00436(11) 0.00458(11) 0.00026(9) 0.000 0.000
Al3 0.00434(10) 0.00384(8) 0.00362(8) -0.00008(7) -0.00001(8) -0.00009(8)
Na1 0.00943(17) 0.00741(13) 0.00736(13) -0.00045(11) 0.00089(14) 0.00082(14)
O1 0.0092(3) 0.0061(2) 0.00578(19) 0.00096(15) 0.00267(18) -0.00008(19)
O2 0.0064(3) 0.0068(2) 0.0103(2) 0.00085(17) -0.00110(18) 0.00133(18)
O3 0.0081(2) 0.00422(17) 0.00459(17) 0.00074(14) 0.00006(17) -0.00006(19)
O4 0.0084(3) 0.00601(19) 0.0061(2) -0.00114(16) -0.00010(17) -0.00185(18)
O5 0.0061(2) 0.0100(2) 0.00649(18) -0.00101(16) 0.00096(19) 0.0005(2)
O1W 0.0101(3) 0.0112(2) 0.0099(2) -0.00096(19) 0.0006(2) -0.0001(2)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Si1 O1 1.6147(7) . ?
Si1 O4 1.6175(7) . ?
Si1 O3 1.6226(7) . ?
Si1 O2 1.6394(8) . ?
Si1 Na1 3.0584(5) . ?
Si2 O5 1.6107(8) 2_565 ?
Si2 O5 1.6107(8) . ?
Si2 O2 1.6320(8) 2_565 ?
Si2 O2 1.6320(8) . ?
Al3 O1 1.7378(7) . ?
Al3 O5 1.7394(9) 2_665 ?
Al3 O4 1.7440(8) 2_565 ?
Al3 O3 1.7485(7) 7_554 ?
Al3 Na1 3.0915(6) 12_454 ?
Al3 Na1 3.5618(5) . ?
Na1 O1 2.3643(8) . ?
Na1 O1W 2.3662(11) 14_455 ?
Na1 O1W 2.3829(11) . ?
Na1 O4 2.3914(8) 7_554 ?
Na1 O3 2.5035(9) 14 ?
Na1 O3 2.5977(9) . ?
Na1 Al3 3.0915(6) 8_544 ?
Na1 Na1 3.6461(4) 14_455 ?
Na1 Na1 3.6461(4) 14 ?
O3 Al3 1.7485(7) 15_455 ?
O3 Na1 2.5035(9) 14_455 ?
O4 Al3 1.7440(8) 2_565 ?
O4 Na1 2.3914(8) 15_455 ?
O5 Al3 1.7394(9) 2_465 ?
O1W Na1 2.3662(11) 14 ?
O1W H1 0.77(3) . ?
O1W H2 0.79(3) . ?

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
O1 Si1 O4 111.64(4) . . ?
O1 Si1 O3 107.30(4) . . ?
O4 Si1 O3 111.04(4) . . ?
O1 Si1 O2 109.93(4) . . ?
O4 Si1 O2 109.60(4) . . ?
O3 Si1 O2 107.21(4) . . ?
O1 Si1 Na1 49.83(3) . . ?
O4 Si1 Na1 120.59(3) . . ?
O3 Si1 Na1 58.14(3) . . ?
O2 Si1 Na1 129.74(3) . . ?
O5 Si2 O5 113.78(6) 2_565 . ?
O5 Si2 O2 107.73(4) 2_565 2_565 ?
O5 Si2 O2 108.20(4) . 2_565 ?
O5 Si2 O2 108.20(4) 2_565 . ?
O5 Si2 O2 107.73(4) . . ?
O2 Si2 O2 111.25(6) 2_565 . ?
O1 Al3 O5 109.94(4) . 2_665 ?
O1 Al3 O4 110.06(4) . 2_565 ?
O5 Al3 O4 112.43(4) 2_665 2_565 ?
O1 Al3 O3 111.34(4) . 7_554 ?
O5 Al3 O3 108.90(4) 2_665 7_554 ?
O4 Al3 O3 104.06(4) 2_565 7_554 ?
O1 Al3 Na1 119.97(3) . 12_454 ?
O5 Al3 Na1 130.08(3) 2_665 12_454 ?
O4 Al3 Na1 50.35(3) 2_565 12_454 ?
O3 Al3 Na1 54.05(3) 7_554 12_454 ?
O1 Al3 Na1 35.20(3) . . ?
O5 Al3 Na1 92.99(3) 2_665 . ?
O4 Al3 Na1 144.49(3) 2_565 . ?
O3 Al3 Na1 89.61(2) 7_554 . ?
Na1 Al3 Na1 128.455(17) 12_454 . ?
O1 Na1 O1W 112.62(4) . 14_455 ?
O1 Na1 O1W 92.84(3) . . ?
O1W Na1 O1W 141.51(2) 14_455 . ?
O1 Na1 O4 87.33(3) . 7_554 ?
O1W Na1 O4 93.73(3) 14_455 7_554 ?
O1W Na1 O4 116.74(4) . 7_554 ?
O1 Na1 O3 151.22(3) . 14 ?
O1W Na1 O3 85.18(3) 14_455 14 ?
O1W Na1 O3 85.04(3) . 14 ?
O4 Na1 O3 68.41(3) 7_554 14 ?
O1 Na1 O3 63.19(2) . . ?
O1W Na1 O3 83.31(3) 14_455 . ?
O1W Na1 O3 83.29(3) . . ?
O4 Na1 O3 145.94(3) 7_554 . ?
O3 Na1 O3 144.29(2) 14 . ?
O1 Na1 Si1 31.457(18) . . ?
O1W Na1 Si1 102.06(3) 14_455 . ?
O1W Na1 Si1 84.55(3) . . ?
O4 Na1 Si1 118.12(2) 7_554 . ?
O3 Na1 Si1 169.47(3) 14 . ?
O3 Na1 Si1 32.041(16) . . ?
O1 Na1 Al3 120.80(2) . 8_544 ?
O1W Na1 Al3 86.71(3) 14_455 8_544 ?
O1W Na1 Al3 105.09(3) . 8_544 ?
O4 Na1 Al3 34.163(19) 7_554 8_544 ?
O3 Na1 Al3 34.428(16) 14 8_544 ?
O3 Na1 Al3 170.00(3) . 8_544 ?
Si1 Na1 Al3 152.109(18) . 8_544 ?
O1 Na1 Al3 25.066(19) . . ?
O1W Na1 Al3 122.84(3) 14_455 . ?
O1W Na1 Al3 92.51(3) . . ?
O4 Na1 Al3 65.17(2) 7_554 . ?
O3 Na1 Al3 126.21(2) 14 . ?
O3 Na1 Al3 87.984(19) . . ?
Si1 Na1 Al3 55.973(10) . . ?
Al3 Na1 Al3 96.948(13) 8_544 . ?
O1 Na1 Na1 89.84(3) . 14_455 ?
O1W Na1 Na1 40.02(2) 14_455 14_455 ?
O1W Na1 Na1 116.57(3) . 14_455 ?
O4 Na1 Na1 126.69(3) 7_554 14_455 ?
O3 Na1 Na1 116.77(3) 14 14_455 ?
O3 Na1 Na1 43.351(19) . 14_455 ?
Si1 Na1 Na1 66.989(14) . 14_455 ?
Al3 Na1 Na1 126.69(2) 8_544 14_455 ?
Al3 Na1 Na1 112.138(17) . 14_455 ?
O1 Na1 Na1 125.57(3) . 14 ?
O1W Na1 Na1 121.60(3) 14_455 14 ?
O1W Na1 Na1 39.68(2) . 14 ?
O4 Na1 Na1 93.51(2) 7_554 14 ?
O3 Na1 Na1 45.42(2) 14 14 ?
O3 Na1 Na1 116.97(3) . 14 ?
Si1 Na1 Na1 124.22(2) . 14 ?
Al3 Na1 Na1 69.132(13) 8_544 14 ?
Al3 Na1 Na1 112.614(17) . 14 ?
Na1 Na1 Na1 129.22(3) 14_455 14 ?
Si1 O1 Al3 138.78(5) . . ?
Si1 O1 Na1 98.71(3) . . ?
Al3 O1 Na1 119.74(4) . . ?
Si2 O2 Si1 144.20(5) . . ?
Si1 O3 Al3 129.20(4) . 15_455 ?
Si1 O3 Na1 128.25(4) . 14_455 ?
Al3 O3 Na1 91.52(3) 15_455 14_455 ?
Si1 O3 Na1 89.82(3) . . ?
Al3 O3 Na1 123.52(4) 15_455 . ?
Na1 O3 Na1 91.23(2) 14_455 . ?
Si1 O4 Al3 134.90(5) . 2_565 ?
Si1 O4 Na1 126.14(4) . 15_455 ?
Al3 O4 Na1 95.48(3) 2_565 15_455 ?
Si2 O5 Al3 140.60(5) . 2_465 ?
Na1 O1W Na1 100.30(3) 14 . ?
Na1 O1W H1 105(2) 14 . ?
Na1 O1W H1 119(2) . . ?
Na1 O1W H2 118(2) 14 . ?
Na1 O1W H2 108(2) . . ?
H1 O1W H2 107(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        50.56
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.129
