# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1451632'
_audit_update_record             
;
2016-02-03 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F6 H6  N Na3 O5 S Ti'
_chemical_formula_weight         362.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   12.925(13)
_cell_length_b                   7.971(8)
_cell_length_c                   9.546(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     983.5(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1208
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5716
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1208
_reflns_number_gt                1014
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0449P)²+0.3672P] 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       0.0053(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1208
_refine_ls_number_parameters     105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
Ti1 Ti 0.09799(4) 0.7500 0.32533(6) 0.01399(18) Uani 1 2 d S . .
Na1 Na 0.29589(9) 0.95787(14) 0.13729(11) 0.0323(3) Uani 1 1 d . . .
Na2 Na 0.0000 1.0000 0.0000 0.0213(3) Uani 1 2 d S . .
S1 S 0.18972(6) 0.7500 -0.15417(8) 0.0135(2) Uani 1 2 d S . .
F1 F 0.09251(12) 0.91794(19) 0.19261(15) 0.0268(4) Uani 1 1 d . . .
F2 F 0.10948(11) 0.91194(18) 0.46429(15) 0.0257(3) Uani 1 1 d . . .
F3 F -0.04434(16) 0.7500 0.3434(2) 0.0304(5) Uani 1 2 d S . .
F4 F 0.24219(14) 0.7500 0.2986(2) 0.0222(5) Uani 1 2 d S . .
O1 O 0.12526(14) 0.9008(2) -0.16071(18) 0.0254(4) Uani 1 1 d . . .
O2 O 0.25827(18) 0.7500 -0.2786(2) 0.0230(5) Uani 1 2 d S . .
O3 O 0.25293(18) 0.7500 -0.0268(2) 0.0223(5) Uani 1 2 d S . .
O4 O 0.1010(2) 1.2500 0.0016(3) 0.0245(6) Uani 1 2 d S . .
H4A H 0.137(3) 1.2500 -0.066(5) 0.037 Uiso 1 2 d S . .
H4B H 0.135(4) 1.2500 0.050(5) 0.037 Uiso 1 2 d S . .
N5 N 0.4597(3) 0.7500 0.8413(4) 0.0256(7) Uani 1 2 d S . .
H5B H 0.498(4) 0.7500 0.764(5) 0.038 Uiso 1 2 d S . .
H5C H 0.469(4) 0.826(7) 0.891(5) 0.13(2) Uiso 1 1 d . . .
H5A H 0.403(6) 0.7500 0.820(7) 0.10(3) Uiso 1 2 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
Ti1 F1 1.8445(19) 7_575 ?
Ti1 F1 1.8445(19) . ?
Ti1 F3 1.848(3) . ?
Ti1 F2 1.8569(19) . ?
Ti1 F2 1.8569(19) 7_575 ?
Ti1 F4 1.881(3) . ?
Ti1 Na1 3.537(2) . ?
Ti1 Na1 3.537(2) 7_575 ?
Na1 F2 2.302(2) 2_574 ?
Na1 O3 2.347(2) . ?
Na1 F4 2.366(2) . ?
Na1 O1 2.455(3) 2_575 ?
Na1 O2 2.561(3) 2_575 ?
Na1 F3 2.654(3) 6_656 ?
Na1 F1 2.700(3) . ?
Na1 S1 3.069(2) 2_575 ?
Na1 Na1 3.314(4) 7_575 ?
Na1 Na2 4.057(4) . ?
Na2 F1 2.289(2) 5_575 ?
Na2 F1 2.289(2) . ?
Na2 O1 2.366(2) 5_575 ?
Na2 O1 2.366(2) . ?
Na2 O4 2.383(2) 5_575 ?
Na2 O4 2.383(2) . ?
Na2 Na2 3.986(4) 3_545 ?
Na2 Na2 3.986(4) 3 ?
Na2 Na1 4.057(4) 5_575 ?
S1 O1 1.464(2) 7_575 ?
S1 O1 1.464(2) . ?
S1 O3 1.465(3) . ?
S1 O2 1.482(3) . ?
S1 Na1 3.069(2) 8_655 ?
S1 Na1 3.069(2) 2_574 ?
F2 Na1 2.302(2) 2_575 ?
F3 Na1 2.654(3) 4_465 ?
F3 Na1 2.654(3) 6_556 ?
F4 Na1 2.366(2) 7_575 ?
O1 Na1 2.455(3) 2_574 ?
O2 Na1 2.561(3) 8_655 ?
O2 Na1 2.561(3) 2_574 ?
O3 Na1 2.347(2) 7_575 ?
O4 Na2 2.383(2) 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
F1 Ti1 F1 93.06(12) 7_575 . ?
F1 Ti1 F3 91.48(7) 7_575 . ?
F1 Ti1 F3 91.48(7) . . ?
F1 Ti1 F2 176.64(7) 7_575 . ?
F1 Ti1 F2 89.38(11) . . ?
F3 Ti1 F2 90.75(7) . . ?
F1 Ti1 F2 89.38(11) 7_575 7_575 ?
F1 Ti1 F2 176.64(7) . 7_575 ?
F3 Ti1 F2 90.75(7) . 7_575 ?
F2 Ti1 F2 88.08(12) . 7_575 ?
F1 Ti1 F4 86.84(7) 7_575 . ?
F1 Ti1 F4 86.84(7) . . ?
F3 Ti1 F4 177.55(9) . . ?
F2 Ti1 F4 91.01(7) . . ?
F2 Ti1 F4 91.01(7) 7_575 . ?
F1 Ti1 Na1 91.10(8) 7_575 . ?
F1 Ti1 Na1 48.64(6) . . ?
F3 Ti1 Na1 140.12(6) . . ?
F2 Ti1 Na1 88.80(7) . . ?
F2 Ti1 Na1 129.08(7) 7_575 . ?
F4 Ti1 Na1 38.25(5) . . ?
F1 Ti1 Na1 48.64(6) 7_575 7_575 ?
F1 Ti1 Na1 91.10(8) . 7_575 ?
F3 Ti1 Na1 140.12(6) . 7_575 ?
F2 Ti1 Na1 129.08(7) . 7_575 ?
F2 Ti1 Na1 88.80(7) 7_575 7_575 ?
F4 Ti1 Na1 38.25(5) . 7_575 ?
Na1 Ti1 Na1 55.87(7) . 7_575 ?
F2 Na1 O3 88.01(10) 2_574 . ?
F2 Na1 F4 159.78(8) 2_574 . ?
O3 Na1 F4 82.56(10) . . ?
F2 Na1 O1 97.82(10) 2_574 2_575 ?
O3 Na1 O1 161.19(8) . 2_575 ?
F4 Na1 O1 86.10(10) . 2_575 ?
F2 Na1 O2 87.72(9) 2_574 2_575 ?
O3 Na1 O2 141.87(9) . 2_575 ?
F4 Na1 O2 110.65(9) . 2_575 ?
O1 Na1 O2 56.62(7) 2_575 2_575 ?
F2 Na1 F3 85.30(8) 2_574 6_656 ?
O3 Na1 F3 77.86(9) . 6_656 ?
F4 Na1 F3 75.27(8) . 6_656 ?
O1 Na1 F3 84.77(8) 2_575 6_656 ?
O2 Na1 F3 139.35(8) 2_575 6_656 ?
F2 Na1 F1 135.29(7) 2_574 . ?
O3 Na1 F1 79.45(8) . . ?
F4 Na1 F1 60.30(6) . . ?
O1 Na1 F1 107.74(8) 2_575 . ?
O2 Na1 F1 77.28(7) 2_575 . ?
F3 Na1 F1 132.09(8) 6_656 . ?
F2 Na1 S1 95.23(8) 2_574 2_575 ?
O3 Na1 S1 169.40(8) . 2_575 ?
F4 Na1 S1 97.29(9) . 2_575 ?
O1 Na1 S1 28.01(5) 2_575 2_575 ?
O2 Na1 S1 28.75(6) 2_575 2_575 ?
F3 Na1 S1 112.42(7) 6_656 2_575 ?
F1 Na1 S1 91.24(5) . 2_575 ?
F2 Na1 Na1 116.79(5) 2_574 7_575 ?
O3 Na1 Na1 45.08(6) . 7_575 ?
F4 Na1 Na1 45.55(6) . 7_575 ?
O1 Na1 Na1 117.32(6) 2_575 7_575 ?
O2 Na1 Na1 155.42(6) 2_575 7_575 ?
F3 Na1 Na1 51.37(5) 6_656 7_575 ?
F1 Na1 Na1 83.23(4) . 7_575 ?
S1 Na1 Na1 139.35(5) 2_575 7_575 ?
F2 Na1 Ti1 163.62(6) 2_574 . ?
O3 Na1 Ti1 80.61(8) . . ?
F4 Na1 Ti1 29.49(5) . . ?
O1 Na1 Ti1 96.69(8) 2_575 . ?
O2 Na1 Ti1 93.97(8) 2_575 . ?
F3 Na1 Ti1 103.58(8) 6_656 . ?
F1 Na1 Ti1 30.85(4) . . ?
S1 Na1 Ti1 94.02(6) 2_575 . ?
Na1 Na1 Ti1 62.07(3) 7_575 . ?
F2 Na1 Na2 103.40(8) 2_574 . ?
O3 Na1 Na2 67.65(6) . . ?
F4 Na1 Na2 89.52(7) . . ?
O1 Na1 Na2 127.38(6) 2_575 . ?
O2 Na1 Na2 76.60(6) 2_575 . ?
F3 Na1 Na2 143.87(6) 6_656 . ?
F1 Na1 Na2 32.34(5) . . ?
S1 Na1 Na2 101.76(4) 2_575 . ?
Na1 Na1 Na2 94.748(17) 7_575 . ?
Ti1 Na1 Na2 61.38(6) . . ?
F1 Na2 F1 180.00(7) 5_575 . ?
F1 Na2 O1 93.89(9) 5_575 5_575 ?
F1 Na2 O1 86.11(9) . 5_575 ?
F1 Na2 O1 86.11(9) 5_575 . ?
F1 Na2 O1 93.89(9) . . ?
O1 Na2 O1 180.0 5_575 . ?
F1 Na2 O4 87.00(8) 5_575 5_575 ?
F1 Na2 O4 93.00(8) . 5_575 ?
O1 Na2 O4 84.76(9) 5_575 5_575 ?
O1 Na2 O4 95.24(9) . 5_575 ?
F1 Na2 O4 93.00(8) 5_575 . ?
F1 Na2 O4 87.00(8) . . ?
O1 Na2 O4 95.24(9) 5_575 . ?
O1 Na2 O4 84.76(9) . . ?
O4 Na2 O4 180.0 5_575 . ?
F1 Na2 Na2 106.61(4) 5_575 3_545 ?
F1 Na2 Na2 73.39(4) . 3_545 ?
O1 Na2 Na2 109.53(5) 5_575 3_545 ?
O1 Na2 Na2 70.47(5) . 3_545 ?
O4 Na2 Na2 33.24(6) 5_575 3_545 ?
O4 Na2 Na2 146.76(6) . 3_545 ?
F1 Na2 Na2 73.39(4) 5_575 3 ?
F1 Na2 Na2 106.61(4) . 3 ?
O1 Na2 Na2 70.47(5) 5_575 3 ?
O1 Na2 Na2 109.53(5) . 3 ?
O4 Na2 Na2 146.76(6) 5_575 3 ?
O4 Na2 Na2 33.24(6) . 3 ?
Na2 Na2 Na2 180.0 3_545 3 ?
F1 Na2 Na1 39.13(4) 5_575 5_575 ?
F1 Na2 Na1 140.87(4) . 5_575 ?
O1 Na2 Na1 62.41(8) 5_575 5_575 ?
O1 Na2 Na1 117.59(8) . 5_575 ?
O4 Na2 Na1 63.28(7) 5_575 5_575 ?
O4 Na2 Na1 116.72(7) . 5_575 ?
Na2 Na2 Na1 94.748(17) 3_545 5_575 ?
Na2 Na2 Na1 85.252(17) 3 5_575 ?
F1 Na2 Na1 140.87(4) 5_575 . ?
F1 Na2 Na1 39.13(4) . . ?
O1 Na2 Na1 117.59(8) 5_575 . ?
O1 Na2 Na1 62.41(8) . . ?
O4 Na2 Na1 116.72(7) 5_575 . ?
O4 Na2 Na1 63.28(7) . . ?
Na2 Na2 Na1 85.252(16) 3_545 . ?
Na2 Na2 Na1 94.748(17) 3 . ?
Na1 Na2 Na1 180.0 5_575 . ?
O1 S1 O1 110.38(17) 7_575 . ?
O1 S1 O3 110.66(9) 7_575 . ?
O1 S1 O3 110.66(9) . . ?
O1 S1 O2 107.83(9) 7_575 . ?
O1 S1 O2 107.83(9) . . ?
O3 S1 O2 109.39(16) . . ?
O1 S1 Na1 51.97(9) 7_575 8_655 ?
O1 S1 Na1 129.03(9) . 8_655 ?
O3 S1 Na1 120.31(7) . 8_655 ?
O2 S1 Na1 56.21(6) . 8_655 ?
O1 S1 Na1 129.03(9) 7_575 2_574 ?
O1 S1 Na1 51.97(9) . 2_574 ?
O3 S1 Na1 120.31(7) . 2_574 ?
O2 S1 Na1 56.21(6) . 2_574 ?
Na1 S1 Na1 98.70(9) 8_655 2_574 ?
Ti1 F1 Na2 141.19(9) . . ?
Ti1 F1 Na1 100.52(7) . . ?
Na2 F1 Na1 108.53(8) . . ?
Ti1 F2 Na1 150.26(9) . 2_575 ?
Ti1 F3 Na1 141.37(5) . 4_465 ?
Ti1 F3 Na1 141.37(5) . 6_556 ?
Na1 F3 Na1 77.27(10) 4_465 6_556 ?
Ti1 F4 Na1 112.27(7) . 7_575 ?
Ti1 F4 Na1 112.27(7) . . ?
Na1 F4 Na1 88.90(11) 7_575 . ?
S1 O1 Na2 129.51(11) . . ?
S1 O1 Na1 100.02(11) . 2_574 ?
Na2 O1 Na1 129.78(9) . 2_574 ?
S1 O2 Na1 95.04(8) . 8_655 ?
S1 O2 Na1 95.04(8) . 2_574 ?
Na1 O2 Na1 130.84(12) 8_655 2_574 ?
S1 O3 Na1 133.31(7) . . ?
S1 O3 Na1 133.31(7) . 7_575 ?
Na1 O3 Na1 89.83(12) . 7_575 ?
Na2 O4 Na2 113.52(13) . 3 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.090
