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

data_ITQ-54_as-made_RED
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'F0.50 O32.50 Si16' 
_chemical_formula_weight          978.78 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Si'  'Si'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-x, y, -z' 
 'x, -y, -z' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, y, -z' 
 'x, -y, z' 
 '-x, y, z' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x+1/2, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, z+1/2' 
 '-x+1/2, y+1/2, z+1/2' 
 
_cell_length_a                    26.5850(3) 
_cell_length_b                    24.9260(3) 
_cell_length_c                    15.9390(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      10562.1(3) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.231 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1269 
_exptl_absorpt_coefficient_mu     0.000 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       ? 
_diffrn_radiation_wavelength      0.0197 
_diffrn_radiation_type            'Electron 200kV' 
_diffrn_radiation_source          'LaB6' 
_diffrn_radiation_monochromator   ? 
_diffrn_measurement_device_type   ? 
_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             10593 
_diffrn_reflns_av_R_equivalents   0.3246 
_diffrn_reflns_av_sigmaI/netI     0.1295 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        26 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          1.12 
_diffrn_reflns_theta_max          20.79 
_reflns_number_total              1913 
_reflns_number_gt                 1472 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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)+(0.1000P)²+0.0000P] 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      SHELXL 
_refine_ls_extinction_coef        0.019(7) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1913 
_refine_ls_number_parameters      112 
_refine_ls_number_restraints      36 
_refine_ls_R_factor_all           0.3174 
_refine_ls_R_factor_gt            0.2892 
_refine_ls_wR_factor_ref          0.6068 
_refine_ls_wR_factor_gt           0.5607 
_refine_ls_goodness_of_fit_ref    3.133 
_refine_ls_restrained_S_all       3.132 
_refine_ls_shift/su_max           0.021 
_refine_ls_shift/su_mean          0.002 
 
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 0.4414(3) 0.2696(4) 0.0964(6) 0.052(3) Uiso 1 1 d D . . 
Si2 Si 0.2070(3) 0.1565(5) 0.2529(7) 0.069(3) Uiso 1 1 d D . . 
Si3 Si 0.2493(3) 0.2103(5) 0.0980(6) 0.061(3) Uiso 1 1 d D . . 
Si4 Si 0.0567(3) 0.1061(5) 0.4032(7) 0.066(3) Uiso 1 1 d D . . 
Si5 Si 0.1973(3) 0.3167(5) 0.1491(6) 0.069(3) Uiso 1 1 d D . . 
Si6 Si 0.1539(3) 0.0614(4) 0.3299(6) 0.063(3) Uiso 1 1 d D . . 
Si7 Si 0.3473(3) 0.2371(5) 0.1951(6) 0.058(3) Uiso 1 1 d D . . 
Si8 Si 0.2122(6) 0.0639(6) 0.5000 0.102(7) Uiso 1 2 d SD . . 
Si9 Si 0.1787(5) 0.3902(7) 0.0000 0.083(5) Uiso 1 2 d SD . . 
O1 O 0.4046(6) 0.2339(10) 0.1563(13) 0.111(7) Uiso 1 1 d D . . 
O2 O 0.2487(14) 0.1896(18) 0.0000 0.144(13) Uiso 1 2 d SD . . 
O3 O 0.2225(17) 0.0000 0.5000 0.124(15) Uiso 1 4 d SD . . 
O4 O 0.4335(12) 0.2497(17) 0.0000 0.132(12) Uiso 1 2 d SD . . 
O5 O 0.0000 0.0988(18) 0.3693(19) 0.114(10) Uiso 1 2 d SD . . 
O6 O 0.1653(7) 0.3537(11) 0.0822(13) 0.122(8) Uiso 1 1 d D . . 
O7 O 0.1810(10) 0.0806(12) 0.4165(12) 0.151(10) Uiso 1 1 d D . . 
O8 O 0.0940(6) 0.0708(12) 0.3424(16) 0.124(8) Uiso 1 1 d D . . 
O9 O 0.1772(9) 0.0985(9) 0.2533(15) 0.138(9) Uiso 1 1 d D . . 
O10 O 0.2237(14) 0.1634(13) 0.1551(15) 0.189(14) Uiso 1 1 d D . . 
O11 O 0.3094(7) 0.2130(16) 0.1228(19) 0.172(12) Uiso 1 1 d D . . 
O12 O 0.2229(14) 0.2691(10) 0.094(2) 0.189(13) Uiso 1 1 d D . . 
O13 O 0.0652(13) 0.0829(17) 0.5000 0.138(13) Uiso 1 2 d SD . . 
O14 O 0.5000 0.2588(17) 0.115(2) 0.117(10) Uiso 1 2 d SD . . 
O15 O 0.2628(9) 0.0970(19) 0.5000 0.156(15) Uiso 1 2 d SD . . 
O16 O 0.4250(9) 0.3322(7) 0.107(2) 0.136(9) Uiso 1 1 d D . . 
O17 O 0.2532(8) 0.1508(14) 0.3213(18) 0.162(11) Uiso 1 1 d D . . 
O18 O 0.1711(9) 0.0000 0.3093(19) 0.094(8) Uiso 1 2 d SD . . 
O19 O 0.1558(11) 0.3006(18) 0.2208(19) 0.191(14) Uiso 1 1 d D . . 
O20 O 0.1518(13) 0.4483(12) 0.0000 0.139(13) Uiso 1 2 d SD . . 
O21 O 0.3341(11) 0.3012(10) 0.207(3) 0.194(14) Uiso 1 1 d D . . 
F1 F 0.0000 0.171(4) 0.5000 0.20(3) Uiso 1 4 d S . . 
 
_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 
Si1 O4 1.629(14) . ? 
Si1 O1 1.630(16) . ? 
Si1 O16 1.629(16) . ? 
Si1 O14 1.607(11) . ? 
Si2 O10 1.630(18) . ? 
Si2 O9 1.649(17) . ? 
Si2 O17 1.648(17) . ? 
Si2 O21 1.645(17) 13 ? 
Si3 O12 1.625(18) . ? 
Si3 O2 1.646(15) . ? 
Si3 O10 1.632(18) . ? 
Si3 O11 1.646(16) . ? 
Si4 O13 1.663(15) . ? 
Si4 O8 1.641(16) . ? 
Si4 O16 1.624(16) 13 ? 
Si4 O5 1.611(13) . ? 
Si5 O12 1.624(17) . ? 
Si5 O6 1.645(15) . ? 
Si5 O17 1.617(18) 13 ? 
Si5 O19 1.639(17) . ? 
Si6 O18 1.631(12) . ? 
Si6 O9 1.652(17) . ? 
Si6 O7 1.629(16) . ? 
Si6 O8 1.622(15) . ? 
Si7 O19 1.639(18) 13 ? 
Si7 O21 1.647(18) . ? 
Si7 O11 1.646(17) . ? 
Si7 O1 1.647(15) . ? 
Si8 O7 1.622(13) . ? 
Si8 O7 1.622(13) 10_556 ? 
Si8 O3 1.615(16) . ? 
Si8 O15 1.580(18) . ? 
Si9 O6 1.633(13) 10 ? 
Si9 O6 1.633(13) . ? 
Si9 O20 1.614(19) . ? 
Si9 O15 1.587(17) 13 ? 
O2 Si3 1.646(15) 10 ? 
O3 Si8 1.615(16) 11 ? 
O4 Si1 1.629(14) 10 ? 
O5 Si4 1.611(13) 12 ? 
O13 Si4 1.663(15) 10_556 ? 
O14 Si1 1.607(11) 12_655 ? 
O15 Si9 1.587(17) 13 ? 
O16 Si4 1.624(16) 13 ? 
O17 Si5 1.617(18) 13 ? 
O18 Si6 1.631(12) 11 ? 
O19 Si7 1.639(18) 13 ? 
O21 Si2 1.645(17) 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 
O4 Si1 O1 108.0(15) . . ? 
O4 Si1 O16 111(2) . . ? 
O1 Si1 O16 107.4(13) . . ? 
O4 Si1 O14 104.1(19) . . ? 
O1 Si1 O14 112.6(15) . . ? 
O16 Si1 O14 113.6(17) . . ? 
O10 Si2 O9 103.1(14) . . ? 
O10 Si2 O17 116.0(19) . . ? 
O9 Si2 O17 106.2(15) . . ? 
O10 Si2 O21 119(2) . 13 ? 
O9 Si2 O21 104.0(16) . 13 ? 
O17 Si2 O21 107(2) . 13 ? 
O12 Si3 O2 104(2) . . ? 
O12 Si3 O10 119(2) . . ? 
O2 Si3 O10 107.4(18) . . ? 
O12 Si3 O11 113.1(19) . . ? 
O2 Si3 O11 104.5(17) . . ? 
O10 Si3 O11 107(2) . . ? 
O13 Si4 O8 106.3(16) . . ? 
O13 Si4 O16 113(2) . 13 ? 
O8 Si4 O16 105.4(15) . 13 ? 
O13 Si4 O5 113.5(19) . . ? 
O8 Si4 O5 107.9(14) . . ? 
O16 Si4 O5 110.7(18) 13 . ? 
O12 Si5 O6 106.1(17) . . ? 
O12 Si5 O17 100(2) . 13 ? 
O6 Si5 O17 109.2(16) . 13 ? 
O12 Si5 O19 119(2) . . ? 
O6 Si5 O19 104.1(12) . . ? 
O17 Si5 O19 118(2) 13 . ? 
O18 Si6 O9 105.7(14) . . ? 
O18 Si6 O7 108.8(16) . . ? 
O9 Si6 O7 107.2(14) . . ? 
O18 Si6 O8 115.9(14) . . ? 
O9 Si6 O8 112.2(16) . . ? 
O7 Si6 O8 106.7(14) . . ? 
O19 Si7 O21 117(2) 13 . ? 
O19 Si7 O11 109(2) 13 . ? 
O21 Si7 O11 108(2) . . ? 
O19 Si7 O1 109.0(13) 13 . ? 
O21 Si7 O1 106.8(14) . . ? 
O11 Si7 O1 106.6(13) . . ? 
O7 Si8 O7 110(2) . 10_556 ? 
O7 Si8 O3 109.8(15) . . ? 
O7 Si8 O3 109.8(15) 10_556 . ? 
O7 Si8 O15 107.5(15) . . ? 
O7 Si8 O15 107.5(15) 10_556 . ? 
O3 Si8 O15 112(3) . . ? 
O6 Si9 O6 107(2) 10 . ? 
O6 Si9 O20 113.8(13) 10 . ? 
O6 Si9 O20 113.8(13) . . ? 
O6 Si9 O15 109.0(13) 10 13 ? 
O6 Si9 O15 109.0(13) . 13 ? 
O20 Si9 O15 105(2) . 13 ? 
Si1 O1 Si7 138.4(16) . . ? 
Si3 O2 Si3 143(3) . 10 ? 
Si8 O3 Si8 160(3) . 11 ? 
Si1 O4 Si1 141(3) 10 . ? 
Si4 O5 Si4 139(2) . 12 ? 
Si9 O6 Si5 136.0(14) . . ? 
Si8 O7 Si6 148(2) . . ? 
Si4 O8 Si6 138.0(16) . . ? 
Si6 O9 Si2 132.3(17) . . ? 
Si2 O10 Si3 136(2) . . ? 
Si7 O11 Si3 141(2) . . ? 
Si3 O12 Si5 145(2) . . ? 
Si4 O13 Si4 136(3) . 10_556 ? 
Si1 O14 Si1 152(3) . 12_655 ? 
Si8 O15 Si9 160(4) . 13 ? 
Si4 O16 Si1 144.7(17) 13 . ? 
Si5 O17 Si2 139(2) 13 . ? 
Si6 O18 Si6 139.6(18) . 11 ? 
Si7 O19 Si5 138(2) 13 . ? 
Si7 O21 Si2 144(2) . 13 ? 
 
_diffrn_measured_fraction_theta_max    0.627 
_diffrn_reflns_theta_full              20.79 
_diffrn_measured_fraction_theta_full   0.627 
_refine_diff_density_max    0.307 
_refine_diff_density_min   -0.286 
_refine_diff_density_rms    0.059 
