data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Jones
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Al H12 O10 S'
_chemical_formula_weight          231.14
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'S'  'S'   0.1246   0.1234
 '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            Monoclinic
_symmetry_space_group_name_H-M    C2/c
_symmetry_space_group_name_hall   '-C 2yc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    10.0144(3)
_cell_length_b                    7.2114(2)
_cell_length_c                    24.3118(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  98.868(2)
_cell_angle_gamma                 90.00
_cell_volume                      1734.76(9)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     2662
_cell_measurement_theta_min       5.11
_cell_measurement_theta_max       23.24
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.26
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.770
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              968
_exptl_absorpt_coefficient_mu     0.504
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8553
_exptl_absorpt_correction_T_max   0.9328
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             4886
_diffrn_reflns_av_R_equivalents   0.0386
_diffrn_reflns_av_sigmaI/netI     0.0353
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          3.39
_diffrn_reflns_theta_max          27.47
_reflns_number_total              1844
_reflns_number_gt                 1693
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_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)+(0.0521P)²+1.3116P] 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        0.0025(7)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1844
_refine_ls_number_parameters      160
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0293
_refine_ls_R_factor_gt            0.0262
_refine_ls_wR_factor_ref          0.0804
_refine_ls_wR_factor_gt           0.0775
_refine_ls_goodness_of_fit_ref    0.989
_refine_ls_restrained_S_all       0.989
_refine_ls_shift/su_max           0.042
_refine_ls_shift/su_mean          0.008
 
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
H5A H 0.337(2) -0.108(3) 0.3041(9) 0.023(5) Uiso 1 1 d . . .
H5B H 0.419(2) -0.232(4) 0.2928(10) 0.039(7) Uiso 1 1 d . . .
H6A H 0.412(2) 0.351(4) 0.2951(10) 0.037(6) Uiso 1 1 d . . .
H6B H 0.320(3) 0.279(3) 0.2730(9) 0.025(7) Uiso 1 1 d . . .
H7A H 0.662(2) 0.151(3) 0.3364(9) 0.024(5) Uiso 1 1 d . . .
H7B H 0.655(2) -0.034(3) 0.3415(9) 0.022(5) Uiso 1 1 d . . .
H8A H 0.354(2) -0.195(3) 0.4240(10) 0.033(6) Uiso 1 1 d . . .
H8B H 0.451(2) -0.298(4) 0.4453(9) 0.031(6) Uiso 1 1 d . . .
H9A H 0.502(3) 0.270(4) 0.4328(10) 0.039(7) Uiso 1 1 d . . .
H9B H 0.390(2) 0.188(3) 0.4122(9) 0.029(5) Uiso 1 1 d . . .
H10A H 0.302(2) 0.121(3) 0.5460(9) 0.022(5) Uiso 1 1 d . . .
H10B H 0.248(3) 0.029(3) 0.5009(12) 0.036(7) Uiso 1 1 d . . .
Al1 Al 0.5000 0.06127(8) 0.2500 0.01432(18) Uani 1 2 d S . .
O5 O 0.38615(11) -0.14372(15) 0.28196(4) 0.0111(2) Uani 1 1 d . . .
O6 O 0.38405(14) 0.25864(15) 0.28065(5) 0.0135(2) Uani 1 1 d . . .
O7 O 0.64181(12) 0.05941(15) 0.32066(4) 0.0137(2) Uani 1 1 d . . .
Al2 Al 0.5000 0.0000 0.5000 0.01560(18) Uani 1 2 d S . .
O8 O 0.41273(12) -0.21606(15) 0.45313(4) 0.0140(2) Uani 1 1 d . . .
O9 O 0.46462(13) 0.17515(17) 0.43274(5) 0.0194(3) Uani 1 1 d . . .
O10 O 0.31162(12) 0.05219(16) 0.52129(5) 0.0172(3) Uani 1 1 d . . .
O1 O 0.08978(11) 0.01149(14) 0.43159(4) 0.0121(2) Uani 1 1 d . . .
O2 O 0.20035(10) 0.23533(13) 0.38090(4) 0.0113(2) Uani 1 1 d . . .
O3 O 0.22500(10) -0.09292(13) 0.36405(4) 0.0116(2) Uani 1 1 d . . .
O4 O 0.01158(11) 0.05898(13) 0.33364(4) 0.0156(3) Uani 1 1 d . . .
S1 S 0.13095(3) 0.05375(4) 0.376943(12) 0.00833(14) Uani 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
Al1 0.0165(4) 0.0124(3) 0.0139(3) 0.000 0.0021(2) 0.000
O5 0.0129(6) 0.0081(5) 0.0126(5) 0.0014(4) 0.0030(4) 0.0013(4)
O6 0.0117(6) 0.0108(5) 0.0174(5) -0.0050(4) 0.0002(4) 0.0019(5)
O7 0.0202(6) 0.0076(5) 0.0116(5) 0.0003(4) -0.0028(4) -0.0011(4)
Al2 0.0163(4) 0.0142(3) 0.0161(3) -0.0006(2) 0.0015(2) 0.0002(3)
O8 0.0137(6) 0.0109(5) 0.0163(5) -0.0050(4) -0.0014(4) 0.0027(4)
O9 0.0181(6) 0.0166(6) 0.0205(5) 0.0092(4) -0.0066(4) -0.0081(5)
O10 0.0116(6) 0.0223(6) 0.0172(5) -0.0108(4) 0.0003(4) 0.0011(4)
O1 0.0149(6) 0.0092(5) 0.0132(5) 0.0003(4) 0.0056(4) 0.0003(4)
O2 0.0129(5) 0.0070(5) 0.0139(4) 0.0008(3) 0.0011(4) -0.0015(4)
O3 0.0138(6) 0.0084(4) 0.0130(4) -0.0011(4) 0.0032(4) 0.0026(4)
O4 0.0167(6) 0.0095(5) 0.0176(5) -0.0016(4) -0.0070(4) 0.0012(4)
S1 0.0101(2) 0.00564(19) 0.00873(19) -0.00036(10) 0.00003(13) 0.00044(11)
 
_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 O6 2.0484(12) 2_655 ?
Al1 O6 2.0484(12) . ?
Al1 O7 2.0533(11) . ?
Al1 O7 2.0533(11) 2_655 ?
Al1 O5 2.0885(11) 2_655 ?
Al1 O5 2.0885(11) . ?
O5 H5A 0.82(2) . ?
O5 H5B 0.75(3) . ?
O6 H6A 0.79(3) . ?
O6 H6B 0.66(3) . ?
O7 H7A 0.78(2) . ?
O7 H7B 0.84(2) . ?
Al2 O8 2.0452(10) 5_656 ?
Al2 O8 2.0452(10) . ?
Al2 O9 2.0534(11) 5_656 ?
Al2 O9 2.0534(11) . ?
Al2 O10 2.0663(12) 5_656 ?
Al2 O10 2.0663(12) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.75(3) . ?
O9 H9A 0.78(3) . ?
O9 H9B 0.84(2) . ?
O10 H10A 0.80(2) . ?
O10 H10B 0.76(3) . ?
O1 S1 1.4822(10) . ?
O2 S1 1.4787(10) . ?
O3 S1 1.4816(10) . ?
O4 S1 1.4665(11) . ?
 
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
O6 Al1 O6 91.97(7) 2_655 . ?
O6 Al1 O7 87.20(5) 2_655 . ?
O6 Al1 O7 93.32(5) . . ?
O6 Al1 O7 93.32(5) 2_655 2_655 ?
O6 Al1 O7 87.20(5) . 2_655 ?
O7 Al1 O7 179.25(7) . 2_655 ?
O6 Al1 O5 89.08(5) 2_655 2_655 ?
O6 Al1 O5 178.57(5) . 2_655 ?
O7 Al1 O5 87.70(4) . 2_655 ?
O7 Al1 O5 91.77(4) 2_655 2_655 ?
O6 Al1 O5 178.57(5) 2_655 . ?
O6 Al1 O5 89.08(5) . . ?
O7 Al1 O5 91.78(4) . . ?
O7 Al1 O5 87.70(4) 2_655 . ?
O5 Al1 O5 89.89(7) 2_655 . ?
Al1 O5 H5A 115.8(15) . . ?
Al1 O5 H5B 119.6(19) . . ?
H5A O5 H5B 108(2) . . ?
Al1 O6 H6A 124.5(17) . . ?
Al1 O6 H6B 129(2) . . ?
H6A O6 H6B 102(3) . . ?
Al1 O7 H7A 120.3(15) . . ?
Al1 O7 H7B 122.4(14) . . ?
H7A O7 H7B 112(2) . . ?
O8 Al2 O8 180.0 5_656 . ?
O8 Al2 O9 91.06(5) 5_656 5_656 ?
O8 Al2 O9 88.94(5) . 5_656 ?
O8 Al2 O9 88.94(5) 5_656 . ?
O8 Al2 O9 91.06(5) . . ?
O9 Al2 O9 180.00(4) 5_656 . ?
O8 Al2 O10 87.14(5) 5_656 5_656 ?
O8 Al2 O10 92.86(5) . 5_656 ?
O9 Al2 O10 92.02(5) 5_656 5_656 ?
O9 Al2 O10 87.98(5) . 5_656 ?
O8 Al2 O10 92.86(5) 5_656 . ?
O8 Al2 O10 87.14(5) . . ?
O9 Al2 O10 87.98(5) 5_656 . ?
O9 Al2 O10 92.02(5) . . ?
O10 Al2 O10 180.00(6) 5_656 . ?
Al2 O8 H8A 120.4(16) . . ?
Al2 O8 H8B 123.7(18) . . ?
H8A O8 H8B 104(2) . . ?
Al2 O9 H9A 120.8(17) . . ?
Al2 O9 H9B 125.0(16) . . ?
H9A O9 H9B 107(2) . . ?
Al2 O10 H10A 121.9(15) . . ?
Al2 O10 H10B 120(2) . . ?
H10A O10 H10B 116(2) . . ?
O4 S1 O2 110.30(6) . . ?
O4 S1 O3 109.93(6) . . ?
O2 S1 O3 109.77(6) . . ?
O4 S1 O1 109.89(6) . . ?
O2 S1 O1 108.46(6) . . ?
O3 S1 O1 108.46(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.935
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.935
_refine_diff_density_max    0.290
_refine_diff_density_min   -0.465
_refine_diff_density_rms    0.061
