# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_u150408man3
_database_code_depnum_ccdc_archive 'CCDC 1053538'
_audit_update_record             
;
2015-04-16 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            AlTfO-G3
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H56 Al2 F12 O26 S4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1218.92

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 4/n c c'
_space_group_name_Hall           '-P 4a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y, x, z-1/2'

_cell_length_a                   17.8177(2)
_cell_length_b                   17.8177(2)
_cell_length_c                   16.8493(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5349.15(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9937
_cell_measurement_theta_min      2.4798
_cell_measurement_theta_max      68.1487
_cell_measurement_temperature    223

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2520

_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_T_max  0.52

_exptl_special_details           'SADABS (Sheldrick 1996)'

_diffrn_ambient_temperature      223

_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              ?

_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'

_diffrn_measurement_device_type  'Bruker APEXII Ultra CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            17591
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_theta_min         3.508
_diffrn_reflns_theta_max         68.163
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19

_refine_special_details          
;
;

_reflns_number_total             2453
_reflns_number_gt                2295
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1687
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_number_reflns         2453
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1016P)²+3.1923P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C6 0.3927(3) 0.2104(3) 0.7190(3) 0.0813(14) Uani d . P . 0.75 A 1
H H6A 0.4389 0.1909 0.6952 0.098 Uiso calc U P R 0.75 A 1
H H6B 0.3926 0.196 0.7752 0.098 Uiso calc U P R 0.75 A 1
C C7 0.3929(3) 0.2921(3) 0.7134(3) 0.0780(13) Uani d . P . 0.75 A 1
H H7A 0.4342 0.3062 0.6779 0.094 Uiso calc U P R 0.75 A 1
H H7B 0.4055 0.3117 0.766 0.094 Uiso calc U P R 0.75 A 1
C C16 0.4044(9) 0.1458(8) 0.7454(8) 0.074(3) Uani d . P . 0.25 A -2
H H16A 0.4437 0.1229 0.7138 0.111 Uiso calc U P R 0.25 A -2
H H16B 0.3832 0.1086 0.7811 0.111 Uiso calc U P R 0.25 A -2
H H16C 0.4252 0.1868 0.7762 0.111 Uiso calc U P R 0.25 A -2
C C17 0.3511(9) 0.0999(9) 0.6890(8) 0.076(3) Uani d . P . 0.25 A -3
H H17A 0.405 0.0922 0.6908 0.114 Uiso calc U P R 0.25 A -3
H H17B 0.3305 0.0746 0.6429 0.114 Uiso calc U P R 0.25 A -3
H H17C 0.3285 0.0795 0.7367 0.114 Uiso calc U P R 0.25 A -3
O O18 0.3238(3) 0.1648(3) 0.7491(3) 0.0838(14) Uani d . P . 0.5 A 4
O O8 0.3352(4) 0.1795(3) 0.6840(3) 0.0875(16) Uani d . P . 0.5 . .
Al Al1 0.25 0.25 0.46533(6) 0.0285(3) Uani d T P S 1 . .
Al Al2 0.25 0.75 0.25 0.0660(5) Uani d T P S 1 . .
C C1 0.44170(18) 0.09492(18) 0.4732(2) 0.0713(10) Uani d . . . 1 . .
C C2 0.3166(3) 0.9014(3) 0.3561(4) 0.123(2) Uani d . . . 1 . .
H H2A 0.3161 0.9196 0.4103 0.185 Uiso calc U . R 1 . .
H H2B 0.2725 0.9197 0.3284 0.185 Uiso calc U . R 1 . .
H H2C 0.3614 0.9194 0.3294 0.185 Uiso calc U . R 1 . .
C C3 0.3800(2) 0.7941(3) 0.3955(2) 0.0943(13) Uani d . . . 1 . .
H H3A 0.3777 0.8077 0.4518 0.113 Uiso calc U . R 1 . .
H H3B 0.4255 0.8165 0.373 0.113 Uiso calc U . R 1 . .
C C4 0.3840(2) 0.7128(3) 0.3881(2) 0.0939(12) Uani d . . . 1 . .
H H4A 0.431 0.6947 0.4116 0.113 Uiso calc U . R 1 . .
H H4B 0.3422 0.6898 0.4171 0.113 Uiso calc U . R 1 . .
C C5 0.3965(2) 0.6171(2) 0.2908(3) 0.0867(11) Uani d . . . 1 . .
H H5A 0.3648 0.584 0.323 0.104 Uiso calc U . R 1 . .
H H5B 0.4491 0.606 0.3032 0.104 Uiso calc U . R 1 . .
F F1 0.51456(11) 0.08626(12) 0.47548(16) 0.0994(9) Uani d . . . 1 . .
F F2 0.41313(19) 0.06513(16) 0.5377(2) 0.1463(15) Uani d . . . 1 . .
F F3 0.41745(16) 0.05771(14) 0.4131(2) 0.1439(15) Uani d . . . 1 . .
O O1 0.33650(10) 0.18988(9) 0.46494(11) 0.0496(5) Uani d . . . 1 . .
O O2 0.44847(14) 0.22685(14) 0.53493(13) 0.0784(8) Uani d . . . 1 . .
O O3 0.44959(13) 0.21733(14) 0.39346(14) 0.0798(7) Uani d . . . 1 . .
O O4 0.25 0.25 0.57656(19) 0.0537(9) Uani d T P S 1 . .
H H4 0.2846 0.2771 0.593 0.081 Uiso calc U P R 0.25 . .
O O5 0.25 0.25 0.35415(18) 0.0507(8) Uani d T P S 1 . .
H H5 0.2251 0.2862 0.3377 0.076 Uiso calc U P R 0.25 . .
O O6 0.31635(13) 0.82351(15) 0.35611(17) 0.0860(8) Uani d . . . 1 . .
O O7 0.38080(15) 0.69192(13) 0.30930(15) 0.0814(7) Uani d . . . 1 . .
S S1 0.41846(3) 0.19380(3) 0.46589(3) 0.0390(3) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C6 O8 . 1.304(8) ?
C6 C7 . 1.460(8) ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C7 O8 3 1.581(8) ?
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C16 O8 . 1.717(15) ?
C16 H16A . 0.97 ?
C16 H16B . 0.97 ?
C16 H16C . 0.97 ?
C17 O8 . 1.449(17) ?
C17 H17A . 0.97 ?
C17 H17B . 0.97 ?
C17 H17C . 0.97 ?
O18 O8 . 1.147(7) ?
O8 C7 4 1.581(8) ?
Al1 O5 . 1.873(3) ?
Al1 O4 . 1.874(3) ?
Al1 O1 . 1.8769(17) ?
Al1 O1 4 1.8770(17) ?
Al1 O1 3 1.8770(17) ?
Al1 O1 2 1.8770(17) ?
Al2 O6 . 2.512(2) ?
Al2 O7 . 2.739(3) ?
C1 F3 . 1.286(4) ?
C1 F1 . 1.308(4) ?
C1 F2 . 1.312(4) ?
C1 S1 . 1.814(3) ?
C2 O6 . 1.388(5) ?
C2 H2A . 0.97 ?
C2 H2B . 0.97 ?
C2 H2C . 0.97 ?
C3 O6 . 1.415(5) ?
C3 C4 . 1.457(6) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C4 O7 . 1.381(5) ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C5 O7 . 1.397(4) ?
C5 C5 8_665 1.418(9) ?
C5 H5A . 0.98 ?
C5 H5B . 0.98 ?
O1 S1 . 1.4620(18) ?
O2 S1 . 1.409(2) ?
O3 S1 . 1.405(2) ?
O4 H4 . 0.83 ?
O5 H5 . 0.83 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O8 C6 C7 . . 113.1(5) ?
O8 C6 H6A . . 109.0 ?
C7 C6 H6A . . 109.0 ?
O8 C6 H6B . . 109.0 ?
C7 C6 H6B . . 109.0 ?
H6A C6 H6B . . 107.8 ?
C6 C7 O8 . 3 120.2(4) ?
C6 C7 H7A . . 107.3 ?
O8 C7 H7A 3 . 107.3 ?
C6 C7 H7B . . 107.3 ?
O8 C7 H7B 3 . 107.3 ?
H7A C7 H7B . . 106.9 ?
O8 C16 H16A . . 109.5 ?
O8 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
O8 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O8 C17 H17A . . 109.5 ?
O8 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
O8 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C6 O8 C7 . 4 125.7(4) ?
O5 Al1 O4 . . 180.0 ?
O5 Al1 O1 . . 89.80(7) ?
O4 Al1 O1 . . 90.20(7) ?
O5 Al1 O1 . 4 89.80(7) ?
O4 Al1 O1 . 4 90.20(7) ?
O1 Al1 O1 . 4 90.0010(10) ?
O5 Al1 O1 . 3 89.80(7) ?
O4 Al1 O1 . 3 90.20(7) ?
O1 Al1 O1 . 3 89.9970(10) ?
O1 Al1 O1 4 3 179.60(13) ?
O5 Al1 O1 . 2 89.80(7) ?
O4 Al1 O1 . 2 90.20(7) ?
O1 Al1 O1 . 2 179.60(13) ?
O1 Al1 O1 4 2 89.9990(10) ?
O1 Al1 O1 3 2 89.9990(10) ?
O6 Al2 O7 . . 62.41(8) ?
F3 C1 F1 . . 107.2(3) ?
F3 C1 F2 . . 108.3(4) ?
F1 C1 F2 . . 108.3(3) ?
F3 C1 S1 . . 111.7(3) ?
F1 C1 S1 . . 110.1(2) ?
F2 C1 S1 . . 111.2(2) ?
O6 C2 H2A . . 109.5 ?
O6 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
O6 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
O6 C3 C4 . . 111.6(3) ?
O6 C3 H3A . . 109.3 ?
C4 C3 H3A . . 109.3 ?
O6 C3 H3B . . 109.3 ?
C4 C3 H3B . . 109.3 ?
H3A C3 H3B . . 108.0 ?
O7 C4 C3 . . 110.4(4) ?
O7 C4 H4A . . 109.6 ?
C3 C4 H4A . . 109.6 ?
O7 C4 H4B . . 109.6 ?
C3 C4 H4B . . 109.6 ?
H4A C4 H4B . . 108.1 ?
O7 C5 C5 . 8_665 110.2(3) ?
O7 C5 H5A . . 109.6 ?
C5 C5 H5A 8_665 . 109.6 ?
O7 C5 H5B . . 109.6 ?
C5 C5 H5B 8_665 . 109.6 ?
H5A C5 H5B . . 108.1 ?
S1 O1 Al1 . . 142.46(11) ?
Al1 O4 H4 . . 109.5 ?
Al1 O5 H5 . . 109.5 ?
C2 O6 C3 . . 111.6(3) ?
C2 O6 Al2 . . 121.5(3) ?
C3 O6 Al2 . . 121.2(2) ?
C4 O7 C5 . . 117.6(3) ?
C4 O7 Al2 . . 106.5(2) ?
C5 O7 Al2 . . 116.7(2) ?
O3 S1 O2 . . 116.27(18) ?
O3 S1 O1 . . 113.53(13) ?
O2 S1 O1 . . 114.07(13) ?
O3 S1 C1 . . 105.02(16) ?
O2 S1 C1 . . 105.24(16) ?
O1 S1 C1 . . 100.51(12) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O8 C6 C7 O8 . . . 3 12.5(6) ?
C7 C6 O8 C7 . . . 4 -144.3(6) ?
O6 C3 C4 O7 . . . . 53.9(5) ?
O5 Al1 O1 S1 . . . . 91.3(2) ?
O4 Al1 O1 S1 . . . . -88.7(2) ?
O1 Al1 O1 S1 4 . . . -178.92(14) ?
O1 Al1 O1 S1 3 . . . 1.5(3) ?
C4 C3 O6 C2 . . . . -173.8(4) ?
C4 C3 O6 Al2 . . . . -20.0(5) ?
C3 C4 O7 C5 . . . . 169.6(3) ?
C3 C4 O7 Al2 . . . . -57.3(4) ?
C5 C5 O7 C4 8_665 . . . 173.7(4) ?
C5 C5 O7 Al2 8_665 . . . 45.3(5) ?
Al1 O1 S1 O3 . . . . -73.4(2) ?
Al1 O1 S1 O2 . . . . 62.9(3) ?
Al1 O1 S1 C1 . . . . 175.0(2) ?
F3 C1 S1 O3 . . . . -56.6(3) ?
F1 C1 S1 O3 . . . . 62.4(3) ?
F2 C1 S1 O3 . . . . -177.7(3) ?
F3 C1 S1 O2 . . . . -179.8(3) ?
F1 C1 S1 O2 . . . . -60.9(3) ?
F2 C1 S1 O2 . . . . 59.1(3) ?
F3 C1 S1 O1 . . . . 61.5(3) ?
F1 C1 S1 O1 . . . . -179.6(3) ?
F2 C1 S1 O1 . . . . -59.6(3) ?

_chemical_properties_physical    Hygroscopic
