# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_K2Al2O8H6
_database_code_depnum_ccdc_archive 'CCDC 1979081'
loop_
_audit_author_name
_audit_author_address
'Mateusz Dembowski'
;Pacific Northwest National Laboratory
United States of America
;
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         K2Al2O7H6
_chemical_formula_sum            'Al2 H6 K2 O7'
_chemical_formula_weight         250.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 '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'
Al Al 0.0406 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.1399 0.1562 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_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+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   10.1605(12)
_cell_length_b                   7.5416(8)
_cell_length_c                   9.9990(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     766.19(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    2593
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      26.77

_exptl_crystal_description       blocky
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_F_000             504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.745
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS (Krause 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9194
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.103
_diffrn_reflns_theta_max         26.939
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1687
_reflns_number_gt                1478
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_max     0.991
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1687
_refine_ls_number_parameters     63
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
K1 K 0.30153(6) 0.02766(8) 0.59783(6) 0.00989(12) Uani 1 1 d . . . . .
Al1 Al 0.49154(8) 0.20877(10) 0.86079(9) 0.00461(16) Uani 1 1 d . . . . .
O1 O 0.6432(2) 0.3220(2) 0.8575(3) 0.0091(4) Uani 1 1 d D . . . .
H1 H 0.718(3) 0.259(6) 0.827(6) 0.058(19) Uiso 1 1 d D . . . .
O2 O 0.3787(2) 0.3316(3) 0.7611(2) 0.0078(4) Uani 1 1 d D . . . .
H2 H 0.380(6) 0.446(3) 0.799(5) 0.054(18) Uiso 1 1 d D . . . .
O3 O 0.4299(2) 0.2183(3) 1.0253(2) 0.0103(4) Uani 1 1 d D . . . .
H3 H 0.469(7) 0.202(8) 1.111(4) 0.10(3) Uiso 1 1 d D . . . .
O4 O 0.500000 0.000000 0.7927(3) 0.0072(5) Uani 1 2 d S T P . .

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
K1 0.0100(2) 0.0108(2) 0.0089(2) 0.0011(3) 0.0005(3) 0.0012(2)
Al1 0.0050(4) 0.0042(3) 0.0047(4) -0.0005(4) -0.0006(4) 0.0001(3)
O1 0.0046(9) 0.0080(8) 0.0149(10) -0.0023(10) -0.0013(10) -0.0007(6)
O2 0.0069(10) 0.0071(9) 0.0094(10) 0.0005(7) -0.0027(8) 0.0008(7)
O3 0.0115(11) 0.0132(10) 0.0062(9) -0.0011(8) 0.0008(8) 0.0018(8)
O4 0.0109(14) 0.0028(12) 0.0078(12) 0.000 0.000 0.0003(10)

_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
K1 O1 2.716(3) 6_654 ?
K1 O3 2.770(2) 5_544 ?
K1 O4 2.812(2) . ?
K1 O3 2.850(2) 8_544 ?
K1 O2 2.865(2) 4_545 ?
K1 O2 2.921(2) . ?
K1 O1 3.259(3) 3_455 ?
K1 O3 3.412(2) 6_654 ?
K1 Al1 3.5365(11) . ?
K1 Al1 3.7402(11) 6_654 ?
K1 Al1 3.8097(11) 2_655 ?
K1 Al1 3.8895(11) 5_544 ?
Al1 O4 1.7177(15) . ?
Al1 O1 1.761(2) . ?
Al1 O3 1.762(3) . ?
Al1 O2 1.779(2) . ?

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
O1 K1 O3 91.30(7) 6_654 5_544 ?
O1 K1 O4 119.71(7) 6_654 . ?
O3 K1 O4 77.35(6) 5_544 . ?
O1 K1 O3 74.64(7) 6_654 8_544 ?
O3 K1 O3 138.32(8) 5_544 8_544 ?
O4 K1 O3 143.66(6) . 8_544 ?
O1 K1 O2 148.45(7) 6_654 4_545 ?
O3 K1 O2 90.88(7) 5_544 4_545 ?
O4 K1 O2 91.44(6) . 4_545 ?
O3 K1 O2 82.99(7) 8_544 4_545 ?
O1 K1 O2 96.40(7) 6_654 . ?
O3 K1 O2 132.91(7) 5_544 . ?
O4 K1 O2 58.56(5) . . ?
O3 K1 O2 88.16(6) 8_544 . ?
O2 K1 O2 104.94(8) 4_545 . ?
O1 K1 O1 131.44(7) 6_654 3_455 ?
O3 K1 O1 137.25(6) 5_544 3_455 ?
O4 K1 O1 80.09(6) . 3_455 ?
O3 K1 O1 67.65(6) 8_544 3_455 ?
O2 K1 O1 53.83(5) 4_545 3_455 ?
O2 K1 O1 54.13(6) . 3_455 ?
O1 K1 O3 53.98(6) 6_654 6_654 ?
O3 K1 O3 92.34(7) 5_544 6_654 ?
O4 K1 O3 67.38(5) . 6_654 ?
O3 K1 O3 108.82(4) 8_544 6_654 ?
O2 K1 O3 157.24(7) 4_545 6_654 ?
O2 K1 O3 57.56(6) . 6_654 ?
O1 K1 O3 111.64(6) 3_455 6_654 ?
O1 K1 Al1 112.55(5) 6_654 . ?
O3 K1 Al1 105.24(6) 5_544 . ?
O4 K1 Al1 28.59(2) . . ?
O3 K1 Al1 116.41(5) 8_544 . ?
O2 K1 Al1 97.15(5) 4_545 . ?
O2 K1 Al1 30.10(5) . . ?
O1 K1 Al1 62.79(4) 3_455 . ?
O3 K1 Al1 60.30(4) 6_654 . ?
O1 K1 Al1 25.98(5) 6_654 6_654 ?
O3 K1 Al1 90.98(5) 5_544 6_654 ?
O4 K1 Al1 94.32(4) . 6_654 ?
O3 K1 Al1 91.98(5) 8_544 6_654 ?
O2 K1 Al1 174.21(5) 4_545 6_654 ?
O2 K1 Al1 77.67(5) . 6_654 ?
O1 K1 Al1 126.70(4) 3_455 6_654 ?
O3 K1 Al1 28.04(4) 6_654 6_654 ?
Al1 K1 Al1 87.650(16) . 6_654 ?
O1 K1 Al1 133.78(5) 6_654 2_655 ?
O3 K1 Al1 61.74(5) 5_544 2_655 ?
O4 K1 Al1 24.664(17) . 2_655 ?
O3 K1 Al1 150.12(5) 8_544 2_655 ?
O2 K1 Al1 73.60(5) 4_545 2_655 ?
O2 K1 Al1 80.40(5) . 2_655 ?
O1 K1 Al1 83.42(4) 3_455 2_655 ?
O3 K1 Al1 88.17(4) 6_654 2_655 ?
Al1 K1 Al1 50.68(3) . 2_655 ?
Al1 K1 Al1 112.08(3) 6_654 2_655 ?
O1 K1 Al1 67.44(5) 6_654 5_544 ?
O3 K1 Al1 23.91(5) 5_544 5_544 ?
O4 K1 Al1 91.16(4) . 5_544 ?
O3 K1 Al1 124.50(5) 8_544 5_544 ?
O2 K1 Al1 110.21(5) 4_545 5_544 ?
O2 K1 Al1 133.83(5) . 5_544 ?
O1 K1 Al1 161.07(4) 3_455 5_544 ?
O3 K1 Al1 79.68(4) 6_654 5_544 ?
Al1 K1 Al1 114.89(3) . 5_544 ?
Al1 K1 Al1 70.33(3) 6_654 5_544 ?
Al1 K1 Al1 81.793(14) 2_655 5_544 ?
O4 Al1 O1 113.15(9) . . ?
O4 Al1 O3 115.17(12) . . ?
O1 Al1 O3 107.97(13) . . ?
O4 Al1 O2 106.69(11) . . ?
O1 Al1 O2 107.52(11) . . ?
O3 Al1 O2 105.83(11) . . ?
O4 Al1 K1 51.57(7) . . ?
O1 Al1 K1 130.60(10) . . ?
O3 Al1 K1 121.06(8) . . ?
O2 Al1 K1 55.44(7) . . ?
O4 Al1 K1 135.26(6) . 6_655 ?
O1 Al1 K1 42.49(9) . 6_655 ?
O3 Al1 K1 65.57(8) . 6_655 ?
O2 Al1 K1 116.14(8) . 6_655 ?
K1 Al1 K1 169.51(3) . 6_655 ?
O4 Al1 K1 43.08(6) . 2_655 ?
O1 Al1 K1 74.41(8) . 2_655 ?
O3 Al1 K1 149.28(8) . 2_655 ?
O2 Al1 K1 102.29(8) . 2_655 ?
K1 Al1 K1 66.88(3) . 2_655 ?
K1 Al1 K1 112.08(3) 6_655 2_655 ?
O4 Al1 K1 146.44(6) . 5 ?
O1 Al1 K1 98.38(8) . 5 ?
O3 Al1 K1 39.60(7) . 5 ?
O2 Al1 K1 72.51(8) . 5 ?
K1 Al1 K1 114.89(3) . 5 ?
K1 Al1 K1 64.17(2) 6_655 5 ?
K1 Al1 K1 169.71(3) 2_655 5 ?
Al1 O1 K1 111.53(12) . 6_655 ?
Al1 O1 K1 127.98(12) . 3 ?
K1 O1 K1 117.22(7) 6_655 3 ?
Al1 O2 K1 179.30(13) . 4 ?
Al1 O2 K1 94.46(9) . . ?
K1 O2 K1 85.12(6) 4 . ?
Al1 O3 K1 116.49(11) . 5 ?
Al1 O3 K1 120.69(11) . 8_545 ?
K1 O3 K1 88.26(6) 5 8_545 ?
Al1 O3 K1 86.39(9) . 6_655 ?
K1 O3 K1 81.25(6) 5 6_655 ?
K1 O3 K1 152.75(9) 8_545 6_655 ?
Al1 O4 Al1 133.26(19) . 2_655 ?
Al1 O4 K1 112.25(6) . 2_655 ?
Al1 O4 K1 99.84(6) 2_655 2_655 ?
Al1 O4 K1 99.84(6) . . ?
Al1 O4 K1 112.25(6) 2_655 . ?
K1 O4 K1 92.28(10) 2_655 . ?

_refine_diff_density_max         0.463
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.124

_shelx_res_file                  
;
TITL new in Aba2
    K2Al2O8H6.res
    created by SHELXL-2016/6 at 14:41:17 on 03-Mar-2019
CELL 0.56086  10.16050   7.54160   9.99900  90.0000  90.0000  90.0000
ZERR    4.00   0.00120   0.00080   0.00120   0.0000   0.0000   0.0000
LATT -5
SYMM -X, -Y, Z
SYMM 0.5+X, 0.5-Y, Z
SYMM 0.5-X, 0.5+Y, Z
SFAC O H AL K
UNIT 28 24 8 8
TEMP -127.110

L.S. 10
BOND
FMAP 2
PLAN 10
ACTA
DFIX 0.96 0.01 O1 H1 o2 H2 O3 H3
WGHT    0.024100
FVAR       0.15929
K1    4    0.301528    0.027657    0.597828    11.00000    0.01004    0.01076 =
         0.00887    0.00112    0.00049    0.00120
AL1   3    0.491543    0.208769    0.860791    11.00000    0.00498    0.00416 =
         0.00470   -0.00053   -0.00057    0.00008
O1    1    0.643153    0.321951    0.857519    11.00000    0.00459    0.00795 =
         0.01490   -0.00229   -0.00135   -0.00068
H1    2    0.718499    0.259454    0.827441    11.00000    0.05799
O2    1    0.378679    0.331552    0.761147    11.00000    0.00691    0.00714 =
         0.00939    0.00051   -0.00274    0.00082
H2    2    0.379669    0.446404    0.798860    11.00000    0.05359
O3    1    0.429920    0.218252    1.025322    11.00000    0.01149    0.01323 =
         0.00624   -0.00108    0.00077    0.00177
H3    2    0.468582    0.201810    1.111102    11.00000    0.10177
O4    1    0.500000    0.000000    0.792656    10.50000    0.01094    0.00276 =
         0.00780    0.00000    0.00000    0.00034

HKLF 4




REM  new in Aba2
REM R1 =  0.0367 for    1478 Fo > 4sig(Fo)  and  0.0503 for all    1687 data
REM     63 parameters refined using      4 restraints

END

WGHT      0.0259      0.7175

REM Highest difference peak  0.463,  deepest hole -0.530,  1-sigma level  0.124
Q1    1   0.5257  0.1893  1.0899  11.00000  0.05    0.46
Q2    1   0.3270  0.2967  0.7362  11.00000  0.05    0.42
Q3    1   0.4836  0.5458  0.8740  11.00000  0.05    0.41
Q4    1   0.2748  0.2522  0.5984  11.00000  0.05    0.40
Q5    1   0.4818  0.1250  1.0806  11.00000  0.05    0.40
Q6    1   0.4607  0.1398  1.2141  11.00000  0.05    0.39
Q7    1   0.5291  0.0893  0.9916  11.00000  0.05    0.39
Q8    1   0.2980  0.1981  1.0993  11.00000  0.05    0.38
Q9    1   0.3279  0.5119  0.8727  11.00000  0.05    0.38
Q10   1   0.6562  0.3337  0.7766  11.00000  0.05    0.37
;
_shelx_res_checksum              52068
####################################################################### 
# 
# 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_Rb2Al2O8H6
_database_code_depnum_ccdc_archive 'CCDC 1979082'
loop_
_audit_author_name
_audit_author_address
'Mateusz Dembowski'
;Pacific Northwest National Laboratory
United States of America
;
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         Rb2Al2O7H6
_chemical_formula_sum            'Al2 H6 O7 Rb2'
_chemical_formula_weight         342.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 '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'
Al Al 0.0406 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb 0.0068 2.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_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+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   10.3511(8)
_cell_length_b                   7.6823(7)
_cell_length_c                   10.2481(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     814.93(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5220
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      28.60

_exptl_crystal_description       blocky
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.795
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    6.579
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   'SADABS (Krause 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17980
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         31.839
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2754
_reflns_number_gt                2057
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_max     0.936
_reflns_Friedel_fraction_full    0.991

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2754
_refine_ls_number_parameters     63
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Rb1 Rb 0.20111(3) 0.97386(4) 0.35079(4) 0.00902(6) Uani 1 1 d . . . . .
Al1 Al 0.00211(11) 0.79223(14) 0.08628(11) 0.00433(19) Uani 1 1 d . . . . .
O1 O 0.1157(3) 0.6689(3) 0.1785(3) 0.0078(5) Uani 1 1 d D . . . .
O2 O 0.0558(3) 0.7775(4) -0.0766(3) 0.0108(5) Uani 1 1 d D . . . .
O3 O -0.1470(3) 0.6832(4) 0.0991(3) 0.0094(5) Uani 1 1 d D . . . .
O4 O 0.000000 1.000000 0.1489(4) 0.0076(7) Uani 1 2 d S T P . .
H2 H 0.010(5) 0.808(7) -0.155(3) 0.033(16) Uiso 1 1 d D . . . .
H1 H 0.119(7) 0.548(3) 0.156(6) 0.027(17) Uiso 1 1 d D . . . .
H3 H -0.213(7) 0.765(10) 0.079(13) 0.11(4) Uiso 1 1 d 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
Rb1 0.00935(11) 0.00892(11) 0.00880(11) 0.0012(2) 0.00087(19) 0.00096(11)
Al1 0.0053(4) 0.0021(4) 0.0056(5) -0.0003(4) 0.0002(4) 0.0003(4)
O1 0.0069(11) 0.0050(11) 0.0114(12) 0.0004(9) -0.0030(10) 0.0007(9)
O2 0.0120(14) 0.0138(14) 0.0065(12) -0.0006(9) 0.0008(10) 0.0024(11)
O3 0.0068(11) 0.0062(12) 0.0151(13) -0.0019(10) -0.0001(11) -0.0005(8)
O4 0.0125(17) 0.0026(17) 0.0077(15) 0.000 0.000 0.0010(12)

_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
Rb1 O3 2.871(3) 6_565 ?
Rb1 O2 2.874(3) 5 ?
Rb1 O4 2.942(3) . ?
Rb1 O1 2.993(3) 4 ?
Rb1 O2 3.027(3) 8_545 ?
Rb1 O1 3.064(3) . ?
Rb1 O3 3.253(3) 3_565 ?
Rb1 O2 3.369(3) 6_565 ?
Rb1 Al1 3.6794(12) . ?
Rb1 Al1 3.7985(13) 6_565 ?
Rb1 Al1 3.8733(12) 2_575 ?
Rb1 Rb1 3.9722(4) 4_545 ?
Al1 O4 1.7203(18) . ?
Al1 O3 1.761(3) . ?
Al1 O2 1.763(3) . ?
Al1 O1 1.781(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
O3 Rb1 O2 90.56(8) 6_565 5 ?
O3 Rb1 O4 120.94(7) 6_565 . ?
O2 Rb1 O4 75.89(7) 5 . ?
O3 Rb1 O1 148.95(8) 6_565 4 ?
O2 Rb1 O1 94.48(8) 5 4 ?
O4 Rb1 O1 89.95(7) . 4 ?
O3 Rb1 O2 74.62(8) 6_565 8_545 ?
O2 Rb1 O2 140.91(10) 5 8_545 ?
O4 Rb1 O2 142.67(7) . 8_545 ?
O1 Rb1 O2 82.40(8) 4 8_545 ?
O3 Rb1 O1 97.65(8) 6_565 . ?
O2 Rb1 O1 128.23(8) 5 . ?
O4 Rb1 O1 56.13(5) . . ?
O1 Rb1 O1 103.03(9) 4 . ?
O2 Rb1 O1 90.03(8) 8_545 . ?
O3 Rb1 O3 129.87(9) 6_565 3_565 ?
O2 Rb1 O3 139.41(8) 5 3_565 ?
O4 Rb1 O3 79.02(7) . 3_565 ?
O1 Rb1 O3 53.96(7) 4 3_565 ?
O2 Rb1 O3 66.94(7) 8_545 3_565 ?
O1 Rb1 O3 53.04(7) . 3_565 ?
O3 Rb1 O2 53.82(7) 6_565 6_565 ?
O2 Rb1 O2 89.71(8) 5 6_565 ?
O4 Rb1 O2 68.66(6) . 6_565 ?
O1 Rb1 O2 156.50(7) 4 6_565 ?
O2 Rb1 O2 108.44(3) 8_545 6_565 ?
O1 Rb1 O2 57.41(7) . 6_565 ?
O3 Rb1 O2 110.11(7) 3_565 6_565 ?
O3 Rb1 Al1 112.61(6) 6_565 . ?
O2 Rb1 Al1 101.86(6) 5 . ?
O4 Rb1 Al1 27.33(2) . . ?
O1 Rb1 Al1 96.30(6) 4 . ?
O2 Rb1 Al1 117.23(6) 8_545 . ?
O1 Rb1 Al1 28.83(5) . . ?
O3 Rb1 Al1 62.97(5) 3_565 . ?
O2 Rb1 Al1 60.23(5) 6_565 . ?
O3 Rb1 Al1 26.21(6) 6_565 6_565 ?
O2 Rb1 Al1 88.99(6) 5 6_565 ?
O4 Rb1 Al1 95.26(5) . 6_565 ?
O1 Rb1 Al1 174.32(6) 4 6_565 ?
O2 Rb1 Al1 92.07(6) 8_545 6_565 ?
O1 Rb1 Al1 78.16(6) . 6_565 ?
O3 Rb1 Al1 124.88(5) 3_565 6_565 ?
O2 Rb1 Al1 27.66(5) 6_565 6_565 ?
Al1 Rb1 Al1 87.361(9) . 6_565 ?
O3 Rb1 Al1 135.18(6) 6_565 2_575 ?
O2 Rb1 Al1 61.33(6) 5 2_575 ?
O4 Rb1 Al1 24.74(2) . 2_575 ?
O1 Rb1 Al1 72.48(6) 4 2_575 ?
O2 Rb1 Al1 148.73(6) 8_545 2_575 ?
O1 Rb1 Al1 78.16(5) . 2_575 ?
O3 Rb1 Al1 83.08(5) 3_565 2_575 ?
O2 Rb1 Al1 89.53(5) 6_565 2_575 ?
Al1 Rb1 Al1 49.93(3) . 2_575 ?
Al1 Rb1 Al1 113.17(3) 6_565 2_575 ?
O3 Rb1 Rb1 69.10(6) 6_565 4_545 ?
O2 Rb1 Rb1 156.68(6) 5 4_545 ?
O4 Rb1 Rb1 104.258(15) . 4_545 ?
O1 Rb1 Rb1 108.82(5) 4 4_545 ?
O2 Rb1 Rb1 46.07(6) 8_545 4_545 ?
O1 Rb1 Rb1 48.25(5) . 4_545 ?
O3 Rb1 Rb1 61.19(5) 3_565 4_545 ?
O2 Rb1 Rb1 69.32(5) 6_565 4_545 ?
Al1 Rb1 Rb1 77.051(18) . 4_545 ?
Al1 Rb1 Rb1 67.710(17) 6_565 4_545 ?
Al1 Rb1 Rb1 125.946(17) 2_575 4_545 ?
O4 Al1 O3 113.71(11) . . ?
O4 Al1 O2 114.61(16) . . ?
O3 Al1 O2 108.43(16) . . ?
O4 Al1 O1 107.72(14) . . ?
O3 Al1 O1 106.63(14) . . ?
O2 Al1 O1 105.08(15) . . ?
O4 Al1 Rb1 51.73(9) . . ?
O3 Al1 Rb1 128.04(11) . . ?
O2 Al1 Rb1 123.07(11) . . ?
O1 Al1 Rb1 56.05(9) . . ?
O4 Al1 Rb1 136.81(8) . 6_564 ?
O3 Al1 Rb1 46.05(10) . 6_564 ?
O2 Al1 Rb1 62.50(11) . 6_564 ?
O1 Al1 Rb1 114.59(10) . 6_564 ?
Rb1 Al1 Rb1 169.18(3) . 6_564 ?
O4 Al1 Rb1 45.71(8) . 2_575 ?
O3 Al1 Rb1 72.08(10) . 2_575 ?
O2 Al1 Rb1 149.71(11) . 2_575 ?
O1 Al1 Rb1 103.54(10) . 2_575 ?
Rb1 Al1 Rb1 67.20(2) . 2_575 ?
Rb1 Al1 Rb1 113.18(3) 6_564 2_575 ?
O4 Al1 Rb1 142.90(8) . 5_544 ?
O3 Al1 Rb1 101.85(10) . 5_544 ?
O2 Al1 Rb1 39.51(10) . 5_544 ?
O1 Al1 Rb1 69.83(10) . 5_544 ?
Rb1 Al1 Rb1 112.80(3) . 5_544 ?
Rb1 Al1 Rb1 64.75(2) 6_564 5_544 ?
Rb1 Al1 Rb1 169.77(3) 2_575 5_544 ?
O4 Al1 Rb1 85.08(9) . 8_544 ?
O3 Al1 Rb1 148.48(11) . 8_544 ?
O2 Al1 Rb1 40.31(10) . 8_544 ?
O1 Al1 Rb1 89.93(10) . 8_544 ?
Rb1 Al1 Rb1 83.48(2) . 8_544 ?
Rb1 Al1 Rb1 102.80(3) 6_564 8_544 ?
Rb1 Al1 Rb1 130.79(3) 2_575 8_544 ?
Rb1 Al1 Rb1 58.273(17) 5_544 8_544 ?
Al1 O1 Rb1 175.84(15) . 4_545 ?
Al1 O1 Rb1 95.12(11) . . ?
Rb1 O1 Rb1 81.95(7) 4_545 . ?
Al1 O2 Rb1 117.52(14) . 5_544 ?
Al1 O2 Rb1 117.56(14) . 8_544 ?
Rb1 O2 Rb1 84.58(8) 5_544 8_544 ?
Al1 O2 Rb1 89.84(12) . 6_564 ?
Rb1 O2 Rb1 83.73(7) 5_544 6_564 ?
Rb1 O2 Rb1 152.56(10) 8_544 6_564 ?
Al1 O3 Rb1 107.74(13) . 6_564 ?
Al1 O3 Rb1 131.23(14) . 3_465 ?
Rb1 O3 Rb1 116.91(9) 6_564 3_465 ?
Al1 O4 Al1 136.2(2) . 2_575 ?
Al1 O4 Rb1 100.95(7) . . ?
Al1 O4 Rb1 109.55(8) 2_575 . ?
Al1 O4 Rb1 109.54(8) . 2_575 ?
Al1 O4 Rb1 100.95(7) 2_575 2_575 ?
Rb1 O4 Rb1 90.61(10) . 2_575 ?

_refine_diff_density_max         1.135
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.289

_shelx_res_file                  
;
TITL md in Aba2
    Rb2Al2O8H6.res
    created by SHELXL-2016/6 at 14:39:15 on 03-Mar-2019
CELL 0.56086  10.35110   7.68230  10.24810  90.0000  90.0000  90.0000
ZERR    4.00   0.00080   0.00070   0.00080   0.0000   0.0000   0.0000
LATT -5
SYMM -X, -Y, Z
SYMM 0.5+X, 0.5-Y, Z
SYMM 0.5-X, 0.5+Y, Z
SFAC O H AL RB
UNIT 28 24 8 8
TEMP -117.860

L.S. 10
BOND
FMAP 2
PLAN 10
ACTA
DFIX 0.96 0.01 O1 H1 o2 H2 O3 H3
WGHT    0.018200
FVAR       0.09959
RB1   4    0.201111    0.973861    0.350790    11.00000    0.00935    0.00892 =
         0.00880    0.00119    0.00087    0.00096
AL1   3    0.002114    0.792228    0.086285    11.00000    0.00529    0.00210 =
         0.00561   -0.00030    0.00021    0.00030
O1    1    0.115707    0.668857    0.178468    11.00000    0.00687    0.00504 =
         0.01135    0.00036   -0.00300    0.00070
O2    1    0.055764    0.777521   -0.076622    11.00000    0.01203    0.01382 =
         0.00650   -0.00061    0.00079    0.00242
O3    1   -0.147046    0.683227    0.099090    11.00000    0.00678    0.00620 =
         0.01510   -0.00190   -0.00006   -0.00053
O4    1    0.000000    1.000000    0.148867    10.50000    0.01253    0.00256 =
         0.00767    0.00000    0.00000    0.00102
H2    2    0.010351    0.807834   -0.154678    11.00000    0.03263
H1    2    0.119367    0.548309    0.156117    11.00000    0.02725
H3    2   -0.213420    0.765151    0.079449    11.00000    0.11385

HKLF 4




REM  md in Aba2
REM R1 =  0.0426 for    2057 Fo > 4sig(Fo)  and  0.0791 for all    2754 data
REM     63 parameters refined using      4 restraints

END

WGHT      0.0177      0.0000

REM Highest difference peak  1.135,  deepest hole -1.494,  1-sigma level  0.289
Q1    1  -0.1068  0.9638 -0.1483  11.00000  0.05    1.14
Q2    1   0.1425  0.7215  0.3156  11.00000  0.05    1.10
Q3    1   0.0000  1.0000 -0.0568  10.50000  0.05    1.10
Q4    1   0.2111  0.7393  0.3501  11.00000  0.05    1.06
Q5    1   0.2962  0.9291  0.3514  11.00000  0.05    0.99
Q6    1   0.1408  0.5603  0.2536  11.00000  0.05    0.99
Q7    1  -0.1716  0.6456  0.0862  11.00000  0.05    0.96
Q8    1   0.1991  0.8556  0.2555  11.00000  0.05    0.95
Q9    1   0.0495  0.9540  0.3479  11.00000  0.05    0.95
Q10   1   0.0798  0.9536  0.2588  11.00000  0.05    0.94
;
_shelx_res_checksum              3047
####################################################################### 
# 
# 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_CsAlOH4
_database_code_depnum_ccdc_archive 'CCDC 1979083'
loop_
_audit_author_name
_audit_author_address
'Mateusz Dembowski'
;Pacific Northwest National Laboratory
United States of America
;
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         CsAlO6H8
_chemical_formula_sum            'Al Cs H8 O6'
_chemical_formula_weight         245.94

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'
Al Al 0.0406 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.7527 1.3916 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   10.4124(15)
_cell_length_b                   6.6986(10)
_cell_length_c                   6.2156(10)
_cell_angle_alpha                90
_cell_angle_beta                 126.129(4)
_cell_angle_gamma                90
_cell_volume                     350.16(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3749
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      21.70

_exptl_crystal_description       Acicular
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_F_000             228
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    2.833
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS (Krause 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            527
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.068
_diffrn_reflns_theta_max         21.702
_diffrn_reflns_theta_full        21.702
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.540
_diffrn_reflns_point_group_measured_fraction_full 0.540
_reflns_number_total             527
_reflns_number_gt                527
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_reflns_special_details          
;
 _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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0539P)²] 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 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -0.03(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         527
_refine_ls_number_parameters     39
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0786
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_restrained_S_all      1.205
_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
Cs1 Cs 0.500000 0.17830(9) 0.500000 0.0100(2) Uani 1 2 d S T P . .
Al1 Al 0.500000 0.662(3) 1.000000 0.007(2) Uani 1 2 d S T P . .
O1 O 0.3636(10) 0.5095(12) 0.7282(14) 0.0138(14) Uani 1 1 d . . . . .
O2 O 0.5884(10) 0.8230(12) 0.9015(16) 0.0133(15) Uani 1 1 d . . . . .
O1W O 0.2690(9) 0.2201(11) 0.7680(13) 0.017(2) 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
Cs1 0.0101(4) 0.0092(4) 0.0118(3) 0.000 0.0070(3) 0.000
Al1 0.0081(14) 0.008(6) 0.0050(13) 0.000 0.0036(11) 0.000
O1 0.022(4) 0.009(3) 0.007(3) -0.001(3) 0.007(3) -0.006(3)
O2 0.020(4) 0.006(3) 0.018(3) -0.003(3) 0.014(3) -0.005(3)
O1W 0.021(4) 0.017(8) 0.014(3) 0.003(2) 0.011(3) 0.008(3)

_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
Cs1 O2 3.167(8) 2_646 ?
Cs1 O2 3.167(8) 1_545 ?
Cs1 O1 3.360(9) 4_546 ?
Cs1 O1 3.360(9) 3_545 ?
Cs1 O1 3.366(9) . ?
Cs1 O1 3.366(9) 2_656 ?
Cs1 O1W 3.656(7) 2_656 ?
Cs1 O1W 3.656(7) . ?
Cs1 O1W 3.696(6) 2_657 ?
Cs1 O1W 3.696(6) 1_554 ?
Cs1 O2 3.788(8) 4_647 ?
Cs1 O2 3.788(8) 3_444 ?
Al1 O2 1.747(15) . ?
Al1 O2 1.747(15) 2_657 ?
Al1 O1 1.756(14) . ?
Al1 O1 1.756(14) 2_657 ?

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
O2 Cs1 O2 82.6(3) 2_646 1_545 ?
O2 Cs1 O1 71.52(19) 2_646 4_546 ?
O2 Cs1 O1 79.13(19) 1_545 4_546 ?
O2 Cs1 O1 79.13(19) 2_646 3_545 ?
O2 Cs1 O1 71.52(19) 1_545 3_545 ?
O1 Cs1 O1 140.7(3) 4_546 3_545 ?
O2 Cs1 O1 146.0(2) 2_646 . ?
O2 Cs1 O1 99.33(18) 1_545 . ?
O1 Cs1 O1 75.48(12) 4_546 . ?
O1 Cs1 O1 134.0(2) 3_545 . ?
O2 Cs1 O1 99.33(18) 2_646 2_656 ?
O2 Cs1 O1 146.0(2) 1_545 2_656 ?
O1 Cs1 O1 134.0(2) 4_546 2_656 ?
O1 Cs1 O1 75.48(12) 3_545 2_656 ?
O1 Cs1 O1 97.5(2) . 2_656 ?
O2 Cs1 O1W 70.25(18) 2_646 2_656 ?
O2 Cs1 O1W 116.94(18) 1_545 2_656 ?
O1 Cs1 O1W 135.53(16) 4_546 2_656 ?
O1 Cs1 O1W 48.54(17) 3_545 2_656 ?
O1 Cs1 O1W 134.11(17) . 2_656 ?
O1 Cs1 O1W 37.14(18) 2_656 2_656 ?
O2 Cs1 O1W 116.94(18) 2_646 . ?
O2 Cs1 O1W 70.25(18) 1_545 . ?
O1 Cs1 O1W 48.54(17) 4_546 . ?
O1 Cs1 O1W 135.54(16) 3_545 . ?
O1 Cs1 O1W 37.14(18) . . ?
O1 Cs1 O1W 134.11(17) 2_656 . ?
O1W Cs1 O1W 171.2(2) 2_656 . ?
O2 Cs1 O1W 134.65(18) 2_646 2_657 ?
O2 Cs1 O1W 53.93(19) 1_545 2_657 ?
O1 Cs1 O1W 107.38(17) 4_546 2_657 ?
O1 Cs1 O1W 75.66(17) 3_545 2_657 ?
O1 Cs1 O1W 63.97(17) . 2_657 ?
O1 Cs1 O1W 109.80(17) 2_656 2_657 ?
O1W Cs1 O1W 115.4(2) 2_656 2_657 ?
O1W Cs1 O1W 63.8(2) . 2_657 ?
O2 Cs1 O1W 53.93(19) 2_646 1_554 ?
O2 Cs1 O1W 134.65(18) 1_545 1_554 ?
O1 Cs1 O1W 75.66(17) 4_546 1_554 ?
O1 Cs1 O1W 107.38(16) 3_545 1_554 ?
O1 Cs1 O1W 109.80(17) . 1_554 ?
O1 Cs1 O1W 63.97(17) 2_656 1_554 ?
O1W Cs1 O1W 63.8(2) 2_656 1_554 ?
O1W Cs1 O1W 115.4(2) . 1_554 ?
O1W Cs1 O1W 171.3(2) 2_657 1_554 ?
O2 Cs1 O2 126.9(2) 2_646 4_647 ?
O2 Cs1 O2 77.50(14) 1_545 4_647 ?
O1 Cs1 O2 147.30(16) 4_546 4_647 ?
O1 Cs1 O2 47.98(17) 3_545 4_647 ?
O1 Cs1 O2 86.08(18) . 4_647 ?
O1 Cs1 O2 74.39(18) 2_656 4_647 ?
O1W Cs1 O2 76.14(16) 2_656 4_647 ?
O1W Cs1 O2 101.56(16) . 4_647 ?
O1W Cs1 O2 39.94(16) 2_657 4_647 ?
O1W Cs1 O2 136.71(17) 1_554 4_647 ?
O2 Cs1 O2 77.50(14) 2_646 3_444 ?
O2 Cs1 O2 126.9(2) 1_545 3_444 ?
O1 Cs1 O2 47.98(17) 4_546 3_444 ?
O1 Cs1 O2 147.30(16) 3_545 3_444 ?
O1 Cs1 O2 74.39(18) . 3_444 ?
O1 Cs1 O2 86.09(18) 2_656 3_444 ?
O1W Cs1 O2 101.56(16) 2_656 3_444 ?
O1W Cs1 O2 76.14(16) . 3_444 ?
O1W Cs1 O2 136.71(17) 2_657 3_444 ?
O1W Cs1 O2 39.94(16) 1_554 3_444 ?
O2 Cs1 O2 150.3(2) 4_647 3_444 ?
O2 Al1 O2 103.6(12) . 2_657 ?
O2 Al1 O1 108.4(3) . . ?
O2 Al1 O1 113.7(4) 2_657 . ?
O2 Al1 O1 113.7(4) . 2_657 ?
O2 Al1 O1 108.4(3) 2_657 2_657 ?
O1 Al1 O1 109.0(12) . 2_657 ?
O2 Al1 Cs1 64.2(3) . 3_556 ?
O2 Al1 Cs1 113.8(5) 2_657 3_556 ?
O1 Al1 Cs1 132.3(6) . 3_556 ?
O1 Al1 Cs1 50.0(3) 2_657 3_556 ?
O2 Al1 Cs1 113.8(5) . 3_455 ?
O2 Al1 Cs1 64.2(3) 2_657 3_455 ?
O1 Al1 Cs1 50.0(3) . 3_455 ?
O1 Al1 Cs1 132.3(6) 2_657 3_455 ?
Cs1 Al1 Cs1 177.0(5) 3_556 3_455 ?
Al1 O1 Cs1 106.4(5) . 3_455 ?
Al1 O1 Cs1 119.0(5) . . ?
Cs1 O1 Cs1 134.0(2) 3_455 . ?
Al1 O2 Cs1 140.6(5) . 1_565 ?
Al1 O2 Cs1 91.3(4) . 3_556 ?
Cs1 O2 Cs1 126.9(2) 1_565 3_556 ?
Cs1 O1W Cs1 115.4(2) . 1_556 ?

_refine_diff_density_max         0.937
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.243

_shelx_res_file                  
;
TITL md_c.res in C2
    CsAlOH4.res
    created by SHELXL-2016/6 at 15:12:07 on 01-May-2019
CELL  0.56086  10.4124   6.6986   6.2156   90.000  126.129   90.000
ZERR    2.000   0.0015   0.0010   0.0010    0.000    0.004    0.000
LATT -7
SYMM -X, Y, -Z
SFAC H AL CS O
UNIT 12 2 2 10
TEMP -173.110
L.S. 10
BOND $H
LIST 6
FMAP 2
PLAN 10
ACTA 52
WGHT    0.053900
BASF   0.33178
FVAR       0.70053
CS1   3    0.500000    0.178300    0.500000    10.50000    0.01006    0.00922 =
         0.01178    0.00000    0.00699    0.00000
AL1   2    0.500000    0.661792    1.000000    10.50000    0.00815    0.00767 =
         0.00499    0.00000    0.00357    0.00000
O1    4    0.363587    0.509537    0.728220    11.00000    0.02190    0.00880 =
         0.00710   -0.00119    0.00656   -0.00565
O2    4    0.588356    0.822997    0.901467    11.00000    0.02019    0.00647 =
         0.01779   -0.00342    0.01376   -0.00523
O1W   4    0.269010    0.220137    0.768014    11.00000    0.02068    0.01681 =
         0.01395    0.00282    0.01116    0.00789

HKLF 5




REM  md_c.res in C2
REM R1 =  0.0274 for     527 Fo > 4sig(Fo)  and  0.0274 for all     527 data
REM     39 parameters refined using      1 restraints

END

WGHT      0.0541      0.0000

REM Highest difference peak  0.937,  deepest hole -1.025,  1-sigma level  0.243
Q1    1   0.3222  0.3822  0.6006  11.00000  0.05    0.94
Q2    1   0.1785  0.4655  0.4025  11.00000  0.05    0.91
Q3    1   0.2451  0.4501  0.3791  11.00000  0.05    0.80
Q4    1   0.2554  0.4077  0.6176  11.00000  0.05    0.78
Q5    1   0.3540  0.0768  0.9992  11.00000  0.05    0.77
Q6    1   0.1284  0.1793  0.6635  11.00000  0.05    0.70
Q7    1   0.4233  0.1742  0.9848  11.00000  0.05    0.63
Q8    1   0.1454  0.2859  0.5430  11.00000  0.05    0.61
Q9    1   0.6583  0.8684  0.8455  11.00000  0.05    0.60
Q10   1   0.2402  0.1223  0.8911  11.00000  0.05    0.58
;
_shelx_res_checksum              50594
