 
data_kar
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Al6 Cl0 Na7.82 O24.13 S1.87 Si6' 
_chemical_formula_weight          956.23

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 
_space_group_crystal_system       cubic
_space_group_IT_number            218
_space_group_name_H-M_alt         'P -4 3 n'
_space_group_name_Hall            'P -4n 2 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'y+1/2, x+1/2, z+1/2'
 '-y+1/2, -x+1/2, z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 '-y+1/2, x+1/2, -z+1/2'
 'x+1/2, z+1/2, y+1/2'
 '-x+1/2, z+1/2, -y+1/2'
 '-x+1/2, -z+1/2, y+1/2'
 'x+1/2, -z+1/2, -y+1/2'
 'z+1/2, y+1/2, x+1/2'
 'z+1/2, -y+1/2, -x+1/2'
 '-z+1/2, y+1/2, -x+1/2'
 '-z+1/2, -y+1/2, x+1/2'
 
_cell_length_a                    8.91462(7)
_cell_length_b                    8.91462(7)
_cell_length_c                    8.91462(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      708.449(16)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     4538
_cell_measurement_theta_min       3.2150
_cell_measurement_theta_max       30.2270
 
_exptl_crystal_description        irregular
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.241          
_exptl_crystal_F_000              471
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.386
_exptl_crystal_size_mid           0.306
_exptl_crystal_size_min           0.229
_exptl_absorpt_coefficient_mu     0.836
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.86383
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type   'Xcalibur, Sapphire3'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.0630
_diffrn_reflns_number             10280
_diffrn_reflns_av_unetI/netI      0.0108
_diffrn_reflns_av_R_equivalents   0.0323
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.232
_diffrn_reflns_theta_max          30.801
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.982
_diffrn_reflns_point_group_measured_fraction_full  0.995
_reflns_number_total              374
_reflns_number_gt                 334
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.685
_reflns_Friedel_fraction_max      0.974
_reflns_Friedel_fraction_full     1.000
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0195P)²+0.0707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.5(3)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          374
_refine_ls_number_parameters      21
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0211
_refine_ls_R_factor_gt            0.0162
_refine_ls_wR_factor_ref          0.0413
_refine_ls_wR_factor_gt           0.0372
_refine_ls_goodness_of_fit_ref    1.176
_refine_ls_restrained_S_all       1.176
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S S 0.000000 0.000000 0.000000 0.0317(6) Uani 0.937(16) 12 d S T P . .
OW O 0.000000 0.000000 0.000000 0.0317(6) Uani 0.063(16) 12 d S T P . .
Na Na 0.18168(9) 0.18168(9) 0.18168(9) 0.0202(4) Uani 0.977(6) 3 d S T P . .
Si Si 0.250000 0.500000 0.000000 0.00721(17) Uani 1 4 d S T P . .
Al Al 0.250000 0.000000 0.500000 0.00705(18) Uani 1 4 d S T P . .
O1 O 0.13998(11) 0.14994(11) 0.44087(14) 0.0123(2) Uani 1 1 d . . . . .
 
 
_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
S Na 2.8053(14) . ?
S Na 2.8053(14) 2 ?
S Na 2.8053(14) 4 ?
S Na 2.8053(14) 3 ?
Na O1 2.3573(14) 5 ?
Na O1 2.3573(14) 9 ?
Na O1 2.3573(14) . ?
Na Al 3.3236(4) . ?
Na Si 3.3236(4) 5 ?
Na Si 3.3236(4) . ?
Na Al 3.3236(4) 5 ?
Na Al 3.3236(4) 9 ?
Na Si 3.3236(4) 9 ?
Si O1 1.6220(7) 16 ?
Si O1 1.6220(7) 11_565 ?
Si O1 1.6220(7) 14_554 ?
Si O1 1.6220(7) 9 ?
Al O1 1.7397(7) 19 ?
Al O1 1.7397(7) 4_556 ?
Al O1 1.7397(7) 18_545 ?
Al O1 1.7397(7) . ?
 
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
Na S Na 109.5 . 2 ?
Na S Na 109.5 . 4 ?
Na S Na 109.5 2 4 ?
Na S Na 109.5 . 3 ?
Na S Na 109.5 2 3 ?
Na S Na 109.5 4 3 ?
O1 Na O1 104.67(5) 5 9 ?
O1 Na O1 104.67(5) 5 . ?
O1 Na O1 104.67(5) 9 . ?
O1 Na S 113.92(4) 5 . ?
O1 Na S 113.92(4) 9 . ?
O1 Na S 113.92(4) . . ?
O1 Na Al 81.14(2) 5 . ?
O1 Na Al 129.37(5) 9 . ?
O1 Na Al 29.951(16) . . ?
S Na Al 108.50(2) . . ?
O1 Na Si 127.52(5) 5 5 ?
O1 Na Si 84.06(2) 9 5 ?
O1 Na Si 26.912(16) . 5 ?
S Na Si 108.50(2) . 5 ?
Al Na Si 56.608(8) . 5 ?
O1 Na Si 84.06(2) 5 . ?
O1 Na Si 26.912(16) 9 . ?
O1 Na Si 127.52(5) . . ?
S Na Si 108.50(2) . . ?
Al Na Si 142.99(4) . . ?
Si Na Si 110.42(2) 5 . ?
O1 Na Al 29.951(16) 5 5 ?
O1 Na Al 81.14(2) 9 5 ?
O1 Na Al 129.37(5) . 5 ?
S Na Al 108.50(2) . 5 ?
Al Na Al 110.42(2) . 5 ?
Si Na Al 142.99(4) 5 5 ?
Si Na Al 56.608(8) . 5 ?
O1 Na Al 129.37(5) 5 9 ?
O1 Na Al 29.951(16) 9 9 ?
O1 Na Al 81.14(2) . 9 ?
S Na Al 108.50(2) . 9 ?
Al Na Al 110.42(2) . 9 ?
Si Na Al 56.608(8) 5 9 ?
Si Na Al 56.608(8) . 9 ?
Al Na Al 110.42(2) 5 9 ?
O1 Na Si 26.912(16) 5 9 ?
O1 Na Si 127.52(5) 9 9 ?
O1 Na Si 84.06(2) . 9 ?
S Na Si 108.50(2) . 9 ?
Al Na Si 56.608(8) . 9 ?
Si Na Si 110.42(2) 5 9 ?
Si Na Si 110.42(2) . 9 ?
Al Na Si 56.608(8) 5 9 ?
Al Na Si 142.99(4) 9 9 ?
O1 Si O1 107.60(4) 16 11_565 ?
O1 Si O1 113.27(8) 16 14_554 ?
O1 Si O1 107.60(4) 11_565 14_554 ?
O1 Si O1 107.60(4) 16 9 ?
O1 Si O1 113.27(8) 11_565 9 ?
O1 Si O1 107.60(4) 14_554 9 ?
O1 Si Na 41.13(4) 16 16 ?
O1 Si Na 126.82(5) 11_565 16 ?
O1 Si Na 123.48(5) 14_554 16 ?
O1 Si Na 66.56(4) 9 16 ?
O1 Si Na 123.48(5) 16 14_554 ?
O1 Si Na 66.56(4) 11_565 14_554 ?
O1 Si Na 41.13(4) 14_554 14_554 ?
O1 Si Na 126.82(5) 9 14_554 ?
Na Si Na 158.88(3) 16 14_554 ?
O1 Si Na 66.56(4) 16 4_565 ?
O1 Si Na 41.13(4) 11_565 4_565 ?
O1 Si Na 126.82(5) 14_554 4_565 ?
O1 Si Na 123.48(5) 9 4_565 ?
Na Si Na 91.924(4) 16 4_565 ?
Na Si Na 91.924(4) 14_554 4_565 ?
O1 Si Na 126.82(5) 16 . ?
O1 Si Na 123.48(5) 11_565 . ?
O1 Si Na 66.56(4) 14_554 . ?
O1 Si Na 41.13(4) 9 . ?
Na Si Na 91.925(4) 16 . ?
Na Si Na 91.924(4) 14_554 . ?
Na Si Na 158.88(2) 4_565 . ?
O1 Al O1 108.53(4) 19 4_556 ?
O1 Al O1 111.37(8) 19 18_545 ?
O1 Al O1 108.53(4) 4_556 18_545 ?
O1 Al O1 108.53(4) 19 . ?
O1 Al O1 111.37(8) 4_556 . ?
O1 Al O1 108.53(4) 18_545 . ?
O1 Al Na 42.57(4) 19 14 ?
O1 Al Na 127.71(5) 4_556 14 ?
O1 Al Na 122.00(5) 18_545 14 ?
O1 Al Na 66.11(4) . 14 ?
O1 Al Na 122.00(5) 19 16_545 ?
O1 Al Na 66.11(4) 4_556 16_545 ?
O1 Al Na 42.57(4) 18_545 16_545 ?
O1 Al Na 127.71(5) . 16_545 ?
Na Al Na 158.88(3) 14 16_545 ?
O1 Al Na 66.11(4) 19 4_556 ?
O1 Al Na 42.57(4) 4_556 4_556 ?
O1 Al Na 127.71(5) 18_545 4_556 ?
O1 Al Na 121.99(5) . 4_556 ?
Na Al Na 91.924(5) 14 4_556 ?
Na Al Na 91.924(5) 16_545 4_556 ?
O1 Al Na 127.71(5) 19 . ?
O1 Al Na 121.99(5) 4_556 . ?
O1 Al Na 66.11(4) 18_545 . ?
O1 Al Na 42.57(4) . . ?
Na Al Na 91.925(5) 14 . ?
Na Al Na 91.924(5) 16_545 . ?
Na Al Na 158.88(2) 4_556 . ?
Si O1 Al 139.27(8) 5 . ?
Si O1 Na 111.95(5) 5 . ?
Al O1 Na 107.48(5) . . ?
 
_refine_diff_density_max    0.191
_refine_diff_density_min   -0.147
_refine_diff_density_rms    0.046



