# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2004


data_global

_journal_coden_Cambridge         1145

loop_
_publ_author_name
'Erhard Kemnitz'
'Michael Feist'
'Udo Grob'
'Hillary A. Prescott'
'Stephan K. Ruediger'
'S. Chandra Shekar'
'Sergey Troyanov'

_publ_contact_author_name        'ProfD Erhard Kemnitz'
_publ_contact_author_address     
;
Institute of Chemistry
Humboldt-University Berlin
Brook-Taylor-Str. 2
Berlin
12489
GERMANY
;

_publ_contact_author_email       ERHARD.KEMNITZ@CHEMIE.HU-BERLIN.DE

_publ_requested_journal          'Journal of Materials Chemistry'

_publ_section_title              
;
Non-aqueous synthesis of high surface area
aluminium fluoride - a mechanistic investigation
;

data_alprf2
_database_code_depnum_ccdc_archive 'CCDC 247809'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Al3 (i-OPr)8 F] (OSMe2)'
_chemical_formula_sum            'C26 H62 Al3 F O9 S'
_chemical_formula_weight         650.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0106 0.0060 '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'
Al Al 0.0645 0.0514 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.923(2)
_cell_length_b                   12.551(2)
_cell_length_c                   25.711(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3847.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    1191
_cell_measurement_theta_min      5
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    0.198
_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      175(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  IPDS(Stoe)
_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            20869
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.34
_reflns_number_total             6974
_reflns_number_gt                5248
_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 F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_number_reflns         6974
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0774
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_restrained_S_all      0.795
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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
Al1 Al 0.35207(6) 0.45873(6) 0.83719(2) 0.02324(16) Uani 1 1 d . . .
Al2 Al 0.35769(7) 0.60649(6) 0.92267(3) 0.02782(18) Uani 1 1 d . . .
Al3 Al 0.19667(7) 0.28526(6) 0.83068(3) 0.02855(18) Uani 1 1 d . . .
S S 0.45645(5) 0.65270(6) 0.77735(2) 0.03196(16) Uani 1 1 d . . .
O1 O 0.25533(14) 0.54716(14) 0.88102(6) 0.0260(4) Uani 1 1 d . . .
O2 O 0.45197(14) 0.52101(14) 0.88737(6) 0.0288(4) Uani 1 1 d . . .
O3 O 0.30022(15) 0.33404(14) 0.87520(6) 0.0304(4) Uani 1 1 d . . .
O4 O 0.23348(14) 0.40304(14) 0.79489(6) 0.0270(4) Uani 1 1 d . . .
O5 O 0.36998(16) 0.74001(15) 0.90925(7) 0.0379(5) Uani 1 1 d . . .
O6 O 0.3569(2) 0.57357(19) 0.98616(6) 0.0561(6) Uani 1 1 d . . .
O7 O 0.23838(16) 0.16957(16) 0.80100(7) 0.0418(5) Uani 1 1 d . . .
O8 O 0.06182(17) 0.2892(2) 0.85061(8) 0.0562(6) Uani 1 1 d . . .
O9 O 0.36049(15) 0.57565(14) 0.78952(6) 0.0325(4) Uani 1 1 d . . .
F1 F 0.46052(12) 0.39158(12) 0.80699(5) 0.0361(4) Uani 1 1 d . . .
C1 C 0.1357(2) 0.5657(2) 0.87778(10) 0.0327(6) Uani 1 1 d . . .
H1 H 0.099(2) 0.499(3) 0.8652(10) 0.039 Uiso 1 1 calc . . .
C2 C 0.1118(3) 0.6531(3) 0.83885(13) 0.0608(10) Uani 1 1 d . . .
H2A H 0.1467 0.7195 0.8506 0.091 Uiso 1 1 calc R . .
H2B H 0.0306 0.6632 0.8358 0.091 Uiso 1 1 calc R . .
H2C H 0.1427 0.6330 0.8049 0.091 Uiso 1 1 calc R . .
C3 C 0.0900(3) 0.5913(3) 0.93090(12) 0.0585(10) Uani 1 1 d . . .
H3A H 0.1098 0.5340 0.9551 0.088 Uiso 1 1 calc R . .
H3B H 0.0082 0.5979 0.9290 0.088 Uiso 1 1 calc R . .
H3C H 0.1222 0.6586 0.9431 0.088 Uiso 1 1 calc R . .
C4 C 0.5729(2) 0.5118(3) 0.89100(12) 0.0426(7) Uani 1 1 d . . .
H4 H 0.602(2) 0.485(3) 0.8570(12) 0.051 Uiso 1 1 calc . . .
C5 C 0.6253(3) 0.6187(3) 0.90206(14) 0.0556(9) Uani 1 1 d . . .
H5A H 0.6031 0.6695 0.8750 0.083 Uiso 1 1 calc R . .
H5B H 0.7071 0.6116 0.9024 0.083 Uiso 1 1 calc R . .
H5C H 0.5996 0.6445 0.9360 0.083 Uiso 1 1 calc R . .
C6 C 0.6032(3) 0.4322(4) 0.9328(2) 0.111(2) Uani 1 1 d . . .
H6A H 0.5674 0.4529 0.9656 0.167 Uiso 1 1 calc R . .
H6B H 0.6848 0.4309 0.9373 0.167 Uiso 1 1 calc R . .
H6C H 0.5770 0.3613 0.9225 0.167 Uiso 1 1 calc R . .
C7 C 0.3301(3) 0.2954(2) 0.92619(9) 0.0377(7) Uani 1 1 d . . .
H7 H 0.373(2) 0.353(3) 0.9446(11) 0.045 Uiso 1 1 calc . . .
C8 C 0.4057(4) 0.1996(3) 0.92113(13) 0.0760(13) Uani 1 1 d . . .
H8A H 0.3641 0.1410 0.9049 0.114 Uiso 1 1 calc R . .
H8B H 0.4315 0.1777 0.9557 0.114 Uiso 1 1 calc R . .
H8C H 0.4705 0.2179 0.8995 0.114 Uiso 1 1 calc R . .
C9 C 0.2239(4) 0.2723(4) 0.95691(12) 0.0806(14) Uani 1 1 d . . .
H9A H 0.1771 0.3365 0.9581 0.121 Uiso 1 1 calc R . .
H9B H 0.2439 0.2510 0.9924 0.121 Uiso 1 1 calc R . .
H9C H 0.1822 0.2146 0.9400 0.121 Uiso 1 1 calc R . .
C10 C 0.2082(2) 0.4250(2) 0.74077(9) 0.0324(6) Uani 1 1 d . . .
H10 H 0.212(2) 0.504(3) 0.7352(10) 0.039 Uiso 1 1 calc . . .
C11 C 0.2954(3) 0.3723(3) 0.70627(10) 0.0473(8) Uani 1 1 d . . .
H11A H 0.3699 0.4001 0.7150 0.071 Uiso 1 1 calc R . .
H11B H 0.2786 0.3878 0.6697 0.071 Uiso 1 1 calc R . .
H11C H 0.2940 0.2951 0.7118 0.071 Uiso 1 1 calc R . .
C12 C 0.0903(2) 0.3873(3) 0.72860(11) 0.0521(9) Uani 1 1 d . . .
H12A H 0.0869 0.3095 0.7316 0.078 Uiso 1 1 calc R . .
H12B H 0.0703 0.4084 0.6931 0.078 Uiso 1 1 calc R . .
H12C H 0.0375 0.4196 0.7532 0.078 Uiso 1 1 calc R . .
C13 C 0.4080(3) 0.8236(3) 0.94226(11) 0.0439(8) Uani 1 1 d . . .
H13 H 0.456(3) 0.792(3) 0.9701(12) 0.053 Uiso 1 1 calc . . .
C14 C 0.3087(3) 0.8769(3) 0.96747(14) 0.0670(10) Uani 1 1 d . . .
H14A H 0.2585 0.9047 0.9405 0.101 Uiso 1 1 calc R . .
H14B H 0.3347 0.9357 0.9894 0.101 Uiso 1 1 calc R . .
H14C H 0.2682 0.8250 0.9889 0.101 Uiso 1 1 calc R . .
C15 C 0.4770(3) 0.9020(3) 0.91118(14) 0.0601(9) Uani 1 1 d . . .
H15A H 0.5388 0.8643 0.8941 0.090 Uiso 1 1 calc R . .
H15B H 0.5074 0.9566 0.9345 0.090 Uiso 1 1 calc R . .
H15C H 0.4295 0.9358 0.8848 0.090 Uiso 1 1 calc R . .
C16 C 0.3388(7) 0.5741(6) 1.03498(15) 0.174(5) Uani 1 1 d . . .
H16 H 0.284(8) 0.634(8) 1.037(3) 0.209 Uiso 1 1 calc . . .
C17 C 0.2776(4) 0.4946(4) 1.06164(14) 0.0885(14) Uani 1 1 d . . .
H17A H 0.2138 0.4720 1.0403 0.133 Uiso 1 1 calc R . .
H17B H 0.2502 0.5234 1.0947 0.133 Uiso 1 1 calc R . .
H17C H 0.3265 0.4333 1.0684 0.133 Uiso 1 1 calc R . .
C18 C 0.4310(9) 0.6188(9) 1.06654(18) 0.251(7) Uani 1 1 d . . .
H18A H 0.4857 0.6533 1.0436 0.377 Uiso 1 1 calc R . .
H18B H 0.4678 0.5614 1.0860 0.377 Uiso 1 1 calc R . .
H18C H 0.4007 0.6713 1.0910 0.377 Uiso 1 1 calc R . .
C19 C 0.1752(3) 0.0786(2) 0.78474(12) 0.0449(8) Uani 1 1 d . . .
H19 H 0.094(3) 0.099(3) 0.7818(11) 0.054 Uiso 1 1 calc . . .
C20 C 0.2163(4) 0.0444(3) 0.73230(14) 0.0751(12) Uani 1 1 d . . .
H20A H 0.2089 0.1037 0.7077 0.113 Uiso 1 1 calc R . .
H20B H 0.1717 -0.0162 0.7201 0.113 Uiso 1 1 calc R . .
H20C H 0.2953 0.0234 0.7348 0.113 Uiso 1 1 calc R . .
C21 C 0.1858(3) -0.0078(3) 0.82525(15) 0.0641(10) Uani 1 1 d . . .
H21A H 0.2653 -0.0241 0.8309 0.096 Uiso 1 1 calc R . .
H21B H 0.1468 -0.0720 0.8132 0.096 Uiso 1 1 calc R . .
H21C H 0.1522 0.0166 0.8579 0.096 Uiso 1 1 calc R . .
C22 C -0.0364(4) 0.2582(6) 0.86524(18) 0.129(3) Uani 1 1 d . . .
H22 H -0.017(6) 0.186(5) 0.879(2) 0.155 Uiso 1 1 calc . . .
C23 C -0.1189(3) 0.2268(4) 0.82645(16) 0.0761(12) Uani 1 1 d . . .
H23A H -0.1628 0.2891 0.8160 0.114 Uiso 1 1 calc R . .
H23B H -0.1690 0.1728 0.8412 0.114 Uiso 1 1 calc R . .
H23C H -0.0804 0.1972 0.7960 0.114 Uiso 1 1 calc R . .
C24 C -0.0813(4) 0.3074(5) 0.91301(17) 0.1045(18) Uani 1 1 d . . .
H24A H -0.0194 0.3234 0.9368 0.157 Uiso 1 1 calc R . .
H24B H -0.1336 0.2580 0.9298 0.157 Uiso 1 1 calc R . .
H24C H -0.1206 0.3734 0.9041 0.157 Uiso 1 1 calc R . .
C25 C 0.3886(3) 0.7782(2) 0.77748(12) 0.0441(7) Uani 1 1 d . . .
H25A H 0.3195 0.7738 0.7570 0.066 Uiso 1 1 calc R . .
H25B H 0.4385 0.8318 0.7622 0.066 Uiso 1 1 calc R . .
H25C H 0.3703 0.7983 0.8133 0.066 Uiso 1 1 calc R . .
C26 C 0.4788(3) 0.6389(3) 0.70925(10) 0.0492(8) Uani 1 1 d . . .
H26A H 0.5087 0.5677 0.7019 0.074 Uiso 1 1 calc R . .
H26B H 0.5326 0.6928 0.6975 0.074 Uiso 1 1 calc R . .
H26C H 0.4076 0.6485 0.6908 0.074 Uiso 1 1 calc R . .

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
Al1 0.0277(4) 0.0201(4) 0.0220(3) -0.0002(3) 0.0008(3) 0.0016(3)
Al2 0.0329(4) 0.0275(5) 0.0231(3) -0.0034(3) 0.0006(3) 0.0011(4)
Al3 0.0347(4) 0.0234(5) 0.0276(4) -0.0004(3) 0.0027(3) -0.0036(3)
S 0.0303(3) 0.0317(4) 0.0339(3) 0.0054(3) -0.0004(3) -0.0049(3)
O1 0.0249(9) 0.0224(10) 0.0308(9) -0.0036(7) 0.0016(7) 0.0030(7)
O2 0.0259(9) 0.0278(11) 0.0328(9) -0.0053(7) -0.0039(7) 0.0033(8)
O3 0.0438(10) 0.0227(10) 0.0247(8) 0.0051(7) -0.0045(7) -0.0017(9)
O4 0.0332(10) 0.0268(10) 0.0211(7) 0.0012(7) -0.0019(7) -0.0019(8)
O5 0.0470(12) 0.0277(12) 0.0389(10) -0.0075(8) -0.0049(9) -0.0020(9)
O6 0.0628(14) 0.0804(18) 0.0250(9) 0.0026(9) 0.0023(10) -0.0019(13)
O7 0.0453(12) 0.0251(11) 0.0550(11) -0.0102(9) -0.0005(9) -0.0052(9)
O8 0.0387(12) 0.0782(18) 0.0516(12) -0.0051(11) 0.0130(9) -0.0100(12)
O9 0.0350(10) 0.0282(11) 0.0342(9) 0.0104(7) 0.0008(8) -0.0068(8)
F1 0.0372(8) 0.0354(9) 0.0356(7) -0.0089(7) 0.0026(6) 0.0085(7)
C1 0.0238(14) 0.0318(18) 0.0426(14) -0.0037(12) 0.0000(11) 0.0031(12)
C2 0.0465(19) 0.072(3) 0.064(2) 0.0132(19) 0.0024(15) 0.0262(18)
C3 0.0394(18) 0.083(3) 0.0526(18) -0.0014(17) 0.0135(14) 0.0155(18)
C4 0.0258(15) 0.049(2) 0.0533(18) -0.0088(15) -0.0004(13) 0.0041(13)
C5 0.0383(18) 0.062(3) 0.0666(19) -0.0038(17) -0.0133(15) -0.0072(16)
C6 0.039(2) 0.093(4) 0.201(5) 0.068(4) -0.031(3) 0.009(2)
C7 0.057(2) 0.0324(18) 0.0233(12) 0.0047(12) -0.0053(12) -0.0023(14)
C8 0.135(4) 0.041(2) 0.0514(18) 0.0009(16) -0.032(2) 0.039(2)
C9 0.085(3) 0.121(4) 0.0355(17) 0.033(2) -0.0021(18) -0.027(3)
C10 0.0391(16) 0.0350(18) 0.0230(11) 0.0041(10) -0.0071(11) -0.0014(13)
C11 0.0511(18) 0.065(2) 0.0253(12) -0.0012(13) -0.0003(12) 0.0041(17)
C12 0.0435(17) 0.078(3) 0.0342(14) 0.0032(15) -0.0100(13) -0.0035(17)
C13 0.0573(19) 0.0295(19) 0.0448(16) -0.0120(13) -0.0098(14) 0.0032(14)
C14 0.082(3) 0.050(3) 0.069(2) -0.0205(17) 0.0186(19) 0.007(2)
C15 0.056(2) 0.037(2) 0.087(2) -0.0119(18) 0.0012(18) -0.0118(17)
C16 0.271(10) 0.223(9) 0.0277(19) 0.027(3) -0.021(3) -0.165(8)
C17 0.117(4) 0.097(4) 0.051(2) 0.007(2) 0.022(2) 0.003(3)
C18 0.364(12) 0.339(13) 0.050(3) 0.038(4) -0.052(5) -0.268(11)
C19 0.0459(19) 0.0312(19) 0.0576(18) -0.0102(14) -0.0029(14) -0.0058(13)
C20 0.093(3) 0.058(3) 0.075(2) -0.032(2) 0.010(2) -0.028(2)
C21 0.064(2) 0.037(2) 0.092(3) 0.0105(18) -0.012(2) -0.0052(17)
C22 0.042(2) 0.267(9) 0.079(3) -0.061(4) 0.020(2) -0.045(4)
C23 0.044(2) 0.100(3) 0.084(3) 0.001(2) -0.0007(18) -0.022(2)
C24 0.068(3) 0.152(5) 0.093(3) -0.034(3) 0.048(2) -0.016(3)
C25 0.0560(19) 0.0264(17) 0.0499(15) 0.0038(13) 0.0085(14) -0.0045(14)
C26 0.055(2) 0.050(2) 0.0429(16) -0.0042(14) 0.0184(14) -0.0103(16)

_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
Al1 F1 1.7278(16) . ?
Al1 O9 1.9146(17) . ?
Al1 O4 1.9158(18) . ?
Al1 O2 1.9220(18) . ?
Al1 O3 1.9458(19) . ?
Al1 O1 1.9576(18) . ?
Al1 Al3 2.8638(11) . ?
Al1 Al2 2.8764(10) . ?
Al2 O6 1.6838(19) . ?
Al2 O5 1.717(2) . ?
Al2 O1 1.7862(18) . ?
Al2 O2 1.7996(18) . ?
Al3 O8 1.688(2) . ?
Al3 O7 1.714(2) . ?
Al3 O3 1.7916(19) . ?
Al3 O4 1.7958(19) . ?
S O9 1.5305(18) . ?
S C25 1.770(3) . ?
S C26 1.779(3) . ?
O1 C1 1.448(3) . ?
O2 C4 1.450(3) . ?
O3 C7 1.442(3) . ?
O4 C10 1.450(3) . ?
O5 C13 1.423(3) . ?
O6 C16 1.274(5) . ?
O7 C19 1.430(3) . ?
O8 C22 1.290(5) . ?
C1 C3 1.505(4) . ?
C1 C2 1.511(4) . ?
C4 C5 1.506(5) . ?
C4 C6 1.511(5) . ?
C7 C8 1.509(5) . ?
C7 C9 1.520(5) . ?
C10 C12 1.515(4) . ?
C10 C11 1.518(4) . ?
C13 C14 1.507(5) . ?
C13 C15 1.511(5) . ?
C16 C17 1.413(7) . ?
C16 C18 1.477(9) . ?
C19 C20 1.497(5) . ?
C19 C21 1.509(5) . ?
C22 C23 1.455(6) . ?
C22 C24 1.475(6) . ?

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 Al1 O9 92.69(8) . . ?
F1 Al1 O4 96.85(8) . . ?
O9 Al1 O4 87.41(8) . . ?
F1 Al1 O2 92.08(8) . . ?
O9 Al1 O2 94.90(8) . . ?
O4 Al1 O2 170.67(8) . . ?
F1 Al1 O3 94.09(8) . . ?
O9 Al1 O3 162.67(9) . . ?
O4 Al1 O3 75.95(7) . . ?
O2 Al1 O3 100.77(8) . . ?
F1 Al1 O1 167.48(8) . . ?
O9 Al1 O1 87.99(8) . . ?
O4 Al1 O1 95.67(8) . . ?
O2 Al1 O1 75.41(7) . . ?
O3 Al1 O1 88.84(8) . . ?
F1 Al1 Al3 95.00(6) . . ?
O9 Al1 Al3 125.39(7) . . ?
O4 Al1 Al3 38.00(5) . . ?
O2 Al1 Al3 138.54(6) . . ?
O3 Al1 Al3 38.04(5) . . ?
O1 Al1 Al3 94.79(6) . . ?
F1 Al1 Al2 129.83(6) . . ?
O9 Al1 Al2 89.64(6) . . ?
O4 Al1 Al2 133.33(6) . . ?
O2 Al1 Al2 37.86(5) . . ?
O3 Al1 Al2 98.18(6) . . ?
O1 Al1 Al2 37.66(5) . . ?
Al3 Al1 Al2 123.36(3) . . ?
O6 Al2 O5 115.76(11) . . ?
O6 Al2 O1 118.35(11) . . ?
O5 Al2 O1 110.17(9) . . ?
O6 Al2 O2 110.25(11) . . ?
O5 Al2 O2 115.29(9) . . ?
O1 Al2 O2 82.87(8) . . ?
O6 Al2 Al1 125.61(9) . . ?
O5 Al2 Al1 118.54(7) . . ?
O1 Al2 Al1 42.03(6) . . ?
O2 Al2 Al1 40.96(6) . . ?
O8 Al3 O7 115.85(12) . . ?
O8 Al3 O3 116.90(10) . . ?
O7 Al3 O3 111.96(10) . . ?
O8 Al3 O4 111.37(11) . . ?
O7 Al3 O4 113.48(9) . . ?
O3 Al3 O4 82.97(8) . . ?
O8 Al3 Al1 125.19(10) . . ?
O7 Al3 Al1 118.84(8) . . ?
O3 Al3 Al1 42.01(6) . . ?
O4 Al3 Al1 41.06(5) . . ?
O9 S C25 102.73(13) . . ?
O9 S C26 104.59(13) . . ?
C25 S C26 99.05(15) . . ?
C1 O1 Al2 129.84(16) . . ?
C1 O1 Al1 129.69(15) . . ?
Al2 O1 Al1 100.31(8) . . ?
C4 O2 Al2 129.52(17) . . ?
C4 O2 Al1 128.86(17) . . ?
Al2 O2 Al1 101.18(9) . . ?
C7 O3 Al3 129.49(17) . . ?
C7 O3 Al1 130.42(17) . . ?
Al3 O3 Al1 99.96(8) . . ?
C10 O4 Al3 126.65(16) . . ?
C10 O4 Al1 128.99(16) . . ?
Al3 O4 Al1 100.94(8) . . ?
C13 O5 Al2 128.81(18) . . ?
C16 O6 Al2 162.8(5) . . ?
C19 O7 Al3 130.80(18) . . ?
C22 O8 Al3 160.8(4) . . ?
S O9 Al1 130.88(11) . . ?
O1 C1 C3 109.8(2) . . ?
O1 C1 C2 109.9(2) . . ?
C3 C1 C2 112.2(3) . . ?
O2 C4 C5 110.7(3) . . ?
O2 C4 C6 109.6(3) . . ?
C5 C4 C6 110.8(3) . . ?
O3 C7 C8 109.7(2) . . ?
O3 C7 C9 109.3(2) . . ?
C8 C7 C9 113.0(3) . . ?
O4 C10 C12 109.4(2) . . ?
O4 C10 C11 109.6(2) . . ?
C12 C10 C11 112.3(2) . . ?
O5 C13 C14 109.5(3) . . ?
O5 C13 C15 109.8(2) . . ?
C14 C13 C15 111.5(3) . . ?
O6 C16 C17 124.2(5) . . ?
O6 C16 C18 114.7(6) . . ?
C17 C16 C18 112.7(4) . . ?
O7 C19 C20 108.6(3) . . ?
O7 C19 C21 109.1(3) . . ?
C20 C19 C21 112.8(3) . . ?
O8 C22 C23 119.7(4) . . ?
O8 C22 C24 116.5(5) . . ?
C23 C22 C24 116.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.041