# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_2_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 2087567'
_audit_update_record             
;
2021-06-02 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;

_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            'B12 H12 Na O27 Rb5'
_chemical_formula_weight         1024.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2 :H'
_space_group_name_Hall           'R 3 2"'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   11.1487(4)
_cell_length_b                   11.1487(4)
_cell_length_c                   20.6785(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2225.9(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3873
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      29.49

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_F_000             1452
_exptl_transmission_factor_min   0.4867
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    8.300
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7441
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.887
_diffrn_reflns_theta_max         25.911
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             965
_reflns_number_gt                935
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.992

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0366P)²+5.6390P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         965
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
Rb Rb 0.40574(7) 0.22196(7) 0.46565(3) 0.0262(2) Uani 0.8333 1 d . . P . .
Na Na 0.000000 0.000000 0.500000 0.0223(11) Uani 1 6 d S T P . .
O4 O 0.333333 0.1900(5) 0.666667 0.0181(10) Uani 1 2 d S T P . .
O5 O 0.1917(4) 0.1169(4) 0.57146(18) 0.0225(8) Uani 1 1 d . . . . .
H5 H 0.139248 0.139629 0.590829 0.027 Uiso 1 1 d R U . . .
O3 O 0.3727(4) 0.0632(4) 0.5830(2) 0.0230(8) Uani 1 1 d . . . . .
O2 O 0.4979(4) 0.1126(4) 0.68315(18) 0.0221(8) Uani 1 1 d . . . . .
O1 O 0.5874(4) 0.0710(5) 0.5876(2) 0.0350(11) Uani 1 1 d . . . . .
H1 H 0.659896 0.097313 0.609739 0.042 Uiso 1 1 d R U . . .
B1 B 0.4845(6) 0.0820(6) 0.6185(3) 0.0203(13) Uani 1 1 d . . . . .
B2 B 0.2663(6) 0.0817(6) 0.6184(3) 0.0176(12) 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
Rb O3 2.916(4) . ?
Rb O3 2.976(4) 5_556 ?
Rb O5 3.009(4) . ?
Rb O1 3.083(5) 6_666 ?
Rb O2 3.110(4) 14_544 ?
Rb O1 3.128(4) 3_665 ?
Rb O5 3.160(4) 4_556 ?
Rb B2 3.495(6) 5_556 ?
Rb B2 3.522(6) . ?
Rb B1 3.793(6) 5_556 ?
Rb Rb 3.8224(13) 4_556 ?
Rb Na 3.9870(7) . ?
Na O5 2.380(4) 6_556 ?
Na O5 2.380(4) . ?
Na O5 2.380(4) 3 ?
Na O5 2.380(4) 4_556 ?
Na O5 2.380(4) 5_556 ?
Na O5 2.380(4) 2 ?
Na H5 2.4381 . ?
O4 B2 1.453(7) 12_556 ?
O4 B2 1.453(7) . ?
O5 B2 1.453(7) . ?
O5 H5 0.8458 . ?
O3 B1 1.369(8) . ?
O3 B2 1.494(7) . ?
O2 B1 1.370(7) . ?
O2 B2 1.489(7) 12_556 ?
O1 B1 1.371(8) . ?
O1 H1 0.8434 . ?

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 Rb O3 76.34(13) . 5_556 ?
O3 Rb O5 47.47(11) . . ?
O3 Rb O5 92.16(11) 5_556 . ?
O3 Rb O1 143.86(12) . 6_666 ?
O3 Rb O1 135.66(11) 5_556 6_666 ?
O5 Rb O1 105.53(12) . 6_666 ?
O3 Rb O2 115.26(11) . 14_544 ?
O3 Rb O2 46.68(10) 5_556 14_544 ?
O5 Rb O2 99.65(11) . 14_544 ?
O1 Rb O2 89.80(11) 6_666 14_544 ?
O3 Rb O1 69.49(11) . 3_665 ?
O3 Rb O1 145.83(12) 5_556 3_665 ?
O5 Rb O1 64.85(12) . 3_665 ?
O1 Rb O1 77.18(14) 6_666 3_665 ?
O2 Rb O1 155.38(12) 14_544 3_665 ?
O3 Rb O5 108.95(10) . 4_556 ?
O3 Rb O5 90.02(10) 5_556 4_556 ?
O5 Rb O5 64.39(13) . 4_556 ?
O1 Rb O5 63.64(10) 6_666 4_556 ?
O2 Rb O5 54.42(10) 14_544 4_556 ?
O1 Rb O5 100.96(11) 3_665 4_556 ?
O3 Rb B2 90.67(13) . 5_556 ?
O3 Rb B2 25.10(12) 5_556 5_556 ?
O5 Rb B2 86.92(13) . 5_556 ?
O1 Rb B2 114.25(13) 6_666 5_556 ?
O2 Rb B2 25.19(12) 14_544 5_556 ?
O1 Rb B2 151.72(13) 3_665 5_556 ?
O5 Rb B2 65.68(12) 4_556 5_556 ?
O3 Rb B2 24.61(12) . . ?
O3 Rb B2 89.16(13) 5_556 . ?
O5 Rb B2 24.10(12) . . ?
O1 Rb B2 122.48(13) 6_666 . ?
O2 Rb B2 114.14(12) 14_544 . ?
O1 Rb B2 59.31(12) 3_665 . ?
O5 Rb B2 88.29(12) 4_556 . ?
B2 Rb B2 94.28(15) 5_556 . ?
O3 Rb B1 84.10(13) . 5_556 ?
O3 Rb B1 18.82(12) 5_556 5_556 ?
O5 Rb B1 109.52(13) . 5_556 ?
O1 Rb B1 131.76(14) 6_666 5_556 ?
O2 Rb B1 52.79(12) 14_544 5_556 ?
O1 Rb B1 148.44(13) 3_665 5_556 ?
O5 Rb B1 103.85(12) 4_556 5_556 ?
B2 Rb B1 38.71(14) 5_556 5_556 ?
B2 Rb B1 102.11(14) . 5_556 ?
O3 Rb Rb 94.44(8) . 4_556 ?
O3 Rb Rb 134.00(7) 5_556 4_556 ?
O5 Rb Rb 53.51(8) . 4_556 ?
O1 Rb Rb 52.55(9) 6_666 4_556 ?
O2 Rb Rb 104.07(8) 14_544 4_556 ?
O1 Rb Rb 51.48(9) 3_665 4_556 ?
O5 Rb Rb 49.96(7) 4_556 4_556 ?
B2 Rb Rb 113.35(9) 5_556 4_556 ?
B2 Rb Rb 70.65(10) . 4_556 ?
B1 Rb Rb 151.77(10) 5_556 4_556 ?
O3 Rb Na 73.46(8) . . ?
O3 Rb Na 72.91(7) 5_556 . ?
O5 Rb Na 36.51(7) . . ?
O1 Rb Na 97.73(8) 6_666 . ?
O2 Rb Na 63.78(8) 14_544 . ?
O1 Rb Na 96.97(9) 3_665 . ?
O5 Rb Na 36.65(7) 4_556 . ?
B2 Rb Na 56.99(10) 5_556 . ?
B2 Rb Na 56.81(9) . . ?
B1 Rb Na 91.50(10) 5_556 . ?
Rb Rb Na 61.357(9) 4_556 . ?
O5 Na O5 168.7(2) 6_556 . ?
O5 Na O5 102.74(19) 6_556 3 ?
O5 Na O5 85.52(13) . 3 ?
O5 Na O5 85.52(13) 6_556 4_556 ?
O5 Na O5 87.43(19) . 4_556 ?
O5 Na O5 168.7(2) 3 4_556 ?
O5 Na O5 85.52(13) 6_556 5_556 ?
O5 Na O5 102.74(19) . 5_556 ?
O5 Na O5 87.43(19) 3 5_556 ?
O5 Na O5 85.52(13) 4_556 5_556 ?
O5 Na O5 87.43(19) 6_556 2 ?
O5 Na O5 85.52(13) . 2 ?
O5 Na O5 85.52(13) 3 2 ?
O5 Na O5 102.74(19) 4_556 2 ?
O5 Na O5 168.7(2) 5_556 2 ?
O5 Na Rb 130.42(9) 6_556 . ?
O5 Na Rb 48.79(9) . . ?
O5 Na Rb 116.58(10) 3 . ?
O5 Na Rb 52.42(10) 4_556 . ?
O5 Na Rb 68.27(10) 5_556 . ?
O5 Na Rb 122.90(10) 2 . ?
O5 Na Rb 116.58(10) 6_556 4_556 ?
O5 Na Rb 52.42(10) . 4_556 ?
O5 Na Rb 130.42(9) 3 4_556 ?
O5 Na Rb 48.79(9) 4_556 4_556 ?
O5 Na Rb 122.90(10) 5_556 4_556 ?
O5 Na Rb 68.27(10) 2 4_556 ?
Rb Na Rb 57.288(18) . 4_556 ?
O5 Na Rb 68.27(10) 6_556 3 ?
O5 Na Rb 122.90(10) . 3 ?
O5 Na Rb 48.79(9) 3 3 ?
O5 Na Rb 130.42(9) 4_556 3 ?
O5 Na Rb 52.42(10) 5_556 3 ?
O5 Na Rb 116.58(10) 2 3 ?
Rb Na Rb 116.897(5) . 3 ?
Rb Na Rb 173.878(18) 4_556 3 ?
O5 Na Rb 48.79(9) 6_556 6_556 ?
O5 Na Rb 130.42(9) . 6_556 ?
O5 Na Rb 68.27(10) 3 6_556 ?
O5 Na Rb 122.90(10) 4_556 6_556 ?
O5 Na Rb 116.58(10) 5_556 6_556 ?
O5 Na Rb 52.42(10) 2 6_556 ?
Rb Na Rb 173.878(18) . 6_556 ?
Rb Na Rb 116.898(5) 4_556 6_556 ?
Rb Na Rb 68.982(18) 3 6_556 ?
O5 Na Rb 52.42(10) 6_556 2 ?
O5 Na Rb 116.58(10) . 2 ?
O5 Na Rb 122.90(10) 3 2 ?
O5 Na Rb 68.27(10) 4_556 2 ?
O5 Na Rb 130.42(9) 5_556 2 ?
O5 Na Rb 48.79(9) 2 2 ?
Rb Na Rb 116.898(5) . 2 ?
Rb Na Rb 68.982(18) 4_556 2 ?
Rb Na Rb 116.897(6) 3 2 ?
Rb Na Rb 57.287(18) 6_556 2 ?
O5 Na Rb 122.90(10) 6_556 5_556 ?
O5 Na Rb 68.27(10) . 5_556 ?
O5 Na Rb 52.42(10) 3 5_556 ?
O5 Na Rb 116.58(10) 4_556 5_556 ?
O5 Na Rb 48.79(9) 5_556 5_556 ?
O5 Na Rb 130.42(9) 2 5_556 ?
Rb Na Rb 68.981(18) . 5_556 ?
Rb Na Rb 116.897(6) 4_556 5_556 ?
Rb Na Rb 57.287(18) 3 5_556 ?
Rb Na Rb 116.898(6) 6_556 5_556 ?
Rb Na Rb 173.878(18) 2 5_556 ?
O5 Na H5 151.1 6_556 . ?
O5 Na H5 20.2 . . ?
O5 Na H5 85.4 3 . ?
O5 Na H5 91.0 4_556 . ?
O5 Na H5 122.8 5_556 . ?
O5 Na H5 65.4 2 . ?
Rb Na H5 65.1 . . ?
Rb Na H5 45.8 4_556 . ?
Rb Na H5 131.6 3 . ?
Rb Na H5 112.8 6_556 . ?
Rb Na H5 99.8 2 . ?
Rb Na H5 84.2 5_556 . ?
B2 O4 B2 110.0(6) 12_556 . ?
B2 O5 Na 138.2(3) . . ?
B2 O5 Rb 98.1(3) . . ?
Na O5 Rb 94.70(12) . . ?
B2 O5 Rb 130.8(3) . 4_556 ?
Na O5 Rb 90.93(12) . 4_556 ?
Rb O5 Rb 76.52(9) . 4_556 ?
B2 O5 H5 109.8 . . ?
Na O5 H5 83.8 . . ?
Rb O5 H5 139.5 . . ?
Rb O5 H5 63.1 4_556 . ?
B1 O3 B2 116.2(5) . . ?
B1 O3 Rb 121.6(3) . . ?
B2 O3 Rb 101.0(3) . . ?
B1 O3 Rb 116.7(3) . 5_556 ?
B2 O3 Rb 97.3(3) . 5_556 ?
Rb O3 Rb 100.05(12) . 5_556 ?
B1 O2 B2 119.7(4) . 12_556 ?
B1 O2 Rb 128.6(3) . 9 ?
B2 O2 Rb 92.0(3) 12_556 9 ?
B1 O1 Rb 131.0(4) . 6_656 ?
B1 O1 Rb 140.4(4) . 2_655 ?
Rb O1 Rb 75.96(9) 6_656 2_655 ?
B1 O1 H1 114.6 . . ?
Rb O1 H1 93.1 6_656 . ?
Rb O1 H1 87.6 2_655 . ?
O3 B1 O2 122.6(5) . . ?
O3 B1 O1 118.4(5) . . ?
O2 B1 O1 119.0(5) . . ?
O3 B1 Rb 44.5(3) . 5_556 ?
O2 B1 Rb 127.4(4) . 5_556 ?
O1 B1 Rb 96.5(3) . 5_556 ?
O5 B2 O4 111.2(5) . . ?
O5 B2 O2 109.6(4) . 12_556 ?
O4 B2 O2 110.0(5) . 12_556 ?
O5 B2 O3 108.1(4) . . ?
O4 B2 O3 109.7(4) . . ?
O2 B2 O3 108.1(5) 12_556 . ?
O5 B2 Rb 91.2(3) . 5_556 ?
O4 B2 Rb 157.4(4) . 5_556 ?
O2 B2 Rb 62.8(3) 12_556 5_556 ?
O3 B2 Rb 57.6(3) . 5_556 ?
O5 B2 Rb 57.8(2) . . ?
O4 B2 Rb 108.5(3) . . ?
O2 B2 Rb 141.3(4) 12_556 . ?
O3 B2 Rb 54.4(3) . . ?
Rb B2 Rb 80.11(13) 5_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O4 0.84 1.90 2.735(5) 173.7 2_655 yes
O1 H1 O4 0.84 1.90 2.735(5) 173.7 2_655 yes
O1 H1 O4 0.84 1.90 2.735(5) 173.7 2_655 yes

_refine_diff_density_max         1.485
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.095



####################################################################### 
# 
# 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_3_a
_database_code_depnum_ccdc_archive 'CCDC 2087568'
_audit_update_record             
;
2021-06-02 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;

_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            'B12 H4 O22 Rb4'
_chemical_formula_weight         827.63

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'
B B 0.0013 0.0007 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.1540(5)
_cell_length_b                   6.6585(4)
_cell_length_c                   18.6325(11)
_cell_angle_alpha                90
_cell_angle_beta                 117.594(2)
_cell_angle_gamma                90
_cell_volume                     1006.50(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2957
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      26.89

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.731
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   0.4579
_exptl_transmission_factor_max   0.7463
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    9.776
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10929
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.467
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2197
_reflns_number_gt                1854
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0301P)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_number_reflns         2197
_refine_ls_number_parameters     180
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_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 0.33257(4) 1.11220(5) 0.34574(2) 0.01929(11) Uani 1 1 d . . . . .
Rb2 Rb 0.89048(4) 1.18560(5) 0.37652(2) 0.02240(11) Uani 1 1 d . . . . .
O2 O 0.5338(3) 0.7547(3) 0.39084(14) 0.0141(5) Uani 1 1 d . . . . .
O5 O 0.8231(3) 0.7895(3) 0.42369(14) 0.0144(5) Uani 1 1 d . . . . .
O10 O 0.8598(3) 0.1389(3) 0.59503(14) 0.0132(5) Uani 1 1 d . . . . .
O3 O 0.6413(3) 0.5818(4) 0.31378(14) 0.0164(5) Uani 1 1 d . . . . .
O4 O 0.7449(3) 0.7311(3) 0.52883(14) 0.0151(5) Uani 1 1 d . . . . .
O7 O 0.8395(3) 0.4874(3) 0.62858(13) 0.0158(5) Uani 1 1 d . . . . .
O11 O 0.6834(3) 0.0451(3) 0.45726(13) 0.0139(5) Uani 1 1 d . . . . .
O9 O 0.9256(3) 0.2446(4) 0.73009(15) 0.0185(5) Uani 1 1 d . . . . .
O6 O 0.8955(3) 0.6608(4) 0.32441(15) 0.0218(6) Uani 1 1 d . . . . .
O8 O 0.7248(3) 0.3827(3) 0.49122(14) 0.0177(5) Uani 1 1 d . . . . .
O1 O 0.3676(3) 0.5323(4) 0.28543(17) 0.0246(6) Uani 1 1 d D . . . .
B6 B 0.7573(5) 0.1816(5) 0.5158(2) 0.0100(7) Uani 1 1 d . . . . .
B4 B 0.7682(4) 0.5344(5) 0.5485(2) 0.0114(7) Uani 1 1 d . . . . .
B5 B 0.9321(5) 0.2964(5) 0.6564(2) 0.0117(8) Uani 1 1 d . . . . .
B2 B 0.6962(5) 0.8259(6) 0.4508(2) 0.0118(8) Uani 1 1 d . . . . .
B1 B 0.5161(5) 0.6250(6) 0.3326(2) 0.0133(8) Uani 1 1 d . . . . .
B3 B 0.7918(5) 0.6822(6) 0.3566(2) 0.0131(8) Uani 1 1 d . . . . .
H9 H 0.984(5) 0.154(6) 0.751(2) 0.018(11) Uiso 1 1 d . . . . .
H1 H 0.310(5) 0.570(7) 0.304(3) 0.049(15) Uiso 1 1 d 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
Rb1 O2 2.887(2) . ?
Rb1 O6 2.895(3) 2_655 ?
Rb1 O4 2.930(2) 3_676 ?
Rb1 O11 2.941(2) 1_565 ?
Rb1 O10 2.986(2) 3_666 ?
Rb1 O1 3.086(3) 1_565 ?
Rb1 O3 3.097(2) 2_655 ?
Rb1 O9 3.183(3) 3_666 ?
Rb1 O7 3.242(2) 3_676 ?
Rb1 B3 3.428(4) 2_655 ?
Rb1 B4 3.458(4) 3_676 ?
Rb1 O9 3.463(3) 4_475 ?
Rb2 O9 2.928(2) 4_575 ?
Rb2 O5 2.934(2) . ?
Rb2 O10 3.008(2) 3_766 ?
Rb2 O4 3.018(2) 3_776 ?
Rb2 O1 3.021(3) 2_655 ?
Rb2 O11 3.062(2) 1_565 ?
Rb2 O6 3.316(3) 1_565 ?
Rb2 O3 3.326(2) 1_565 ?
Rb2 O7 3.328(2) 3_776 ?
Rb2 B4 3.339(4) 3_776 ?
Rb2 B6 3.340(4) 1_565 ?
Rb2 B3 3.403(4) 1_565 ?
O2 B1 1.337(4) . ?
O2 B2 1.464(4) . ?
O5 B3 1.350(5) . ?
O5 B2 1.486(4) . ?
O10 B6 1.363(4) . ?
O10 B5 1.465(4) . ?
O3 B1 1.376(4) . ?
O3 B3 1.401(4) . ?
O4 B4 1.350(4) . ?
O4 B2 1.453(4) . ?
O7 B4 1.360(4) . ?
O7 B5 1.483(4) . ?
O11 B6 1.338(4) . ?
O11 B2 1.474(4) 1_545 ?
O9 B5 1.444(4) . ?
O9 H9 0.78(4) . ?
O6 B3 1.345(4) . ?
O6 B5 1.475(4) 3_766 ?
O8 B4 1.387(4) . ?
O8 B6 1.402(4) . ?
O1 B1 1.376(5) . ?
O1 H1 0.796(19) . ?

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 Rb1 O6 116.76(7) . 2_655 ?
O2 Rb1 O4 114.78(7) . 3_676 ?
O6 Rb1 O4 121.02(7) 2_655 3_676 ?
O2 Rb1 O11 47.80(6) . 1_565 ?
O6 Rb1 O11 142.02(6) 2_655 1_565 ?
O4 Rb1 O11 94.53(7) 3_676 1_565 ?
O2 Rb1 O10 80.62(6) . 3_666 ?
O6 Rb1 O10 102.58(7) 2_655 3_666 ?
O4 Rb1 O10 60.18(6) 3_676 3_666 ?
O11 Rb1 O10 106.97(6) 1_565 3_666 ?
O2 Rb1 O1 133.91(7) . 1_565 ?
O6 Rb1 O1 69.13(7) 2_655 1_565 ?
O4 Rb1 O1 94.12(7) 3_676 1_565 ?
O11 Rb1 O1 97.55(7) 1_565 1_565 ?
O10 Rb1 O1 145.15(6) 3_666 1_565 ?
O2 Rb1 O3 84.43(6) . 2_655 ?
O6 Rb1 O3 45.04(6) 2_655 2_655 ?
O4 Rb1 O3 160.63(6) 3_676 2_655 ?
O11 Rb1 O3 97.11(6) 1_565 2_655 ?
O10 Rb1 O3 129.73(6) 3_666 2_655 ?
O1 Rb1 O3 69.05(7) 1_565 2_655 ?
O2 Rb1 O9 75.89(7) . 3_666 ?
O6 Rb1 O9 65.60(7) 2_655 3_666 ?
O4 Rb1 O9 102.46(6) 3_676 3_666 ?
O11 Rb1 O9 122.92(7) 1_565 3_666 ?
O10 Rb1 O9 45.77(6) 3_666 3_666 ?
O1 Rb1 O9 134.10(7) 1_565 3_666 ?
O3 Rb1 O9 84.07(6) 2_655 3_666 ?
O2 Rb1 O7 157.39(6) . 3_676 ?
O6 Rb1 O7 85.21(6) 2_655 3_676 ?
O4 Rb1 O7 43.63(6) 3_676 3_676 ?
O11 Rb1 O7 117.82(6) 1_565 3_676 ?
O10 Rb1 O7 89.76(6) 3_666 3_676 ?
O1 Rb1 O7 56.49(6) 1_565 3_676 ?
O3 Rb1 O7 117.00(6) 2_655 3_676 ?
O9 Rb1 O7 111.58(6) 3_666 3_676 ?
O2 Rb1 B3 105.92(8) . 2_655 ?
O6 Rb1 B3 22.60(8) 2_655 2_655 ?
O4 Rb1 B3 138.49(8) 3_676 2_655 ?
O11 Rb1 B3 119.70(8) 1_565 2_655 ?
O10 Rb1 B3 122.04(8) 3_666 2_655 ?
O1 Rb1 B3 60.91(8) 1_565 2_655 ?
O3 Rb1 B3 24.12(7) 2_655 2_655 ?
O9 Rb1 B3 79.24(8) 3_666 2_655 ?
O7 Rb1 B3 96.54(8) 3_676 2_655 ?
O2 Rb1 B4 134.27(8) . 3_676 ?
O6 Rb1 B4 107.50(8) 2_655 3_676 ?
O4 Rb1 B4 22.51(8) 3_676 3_676 ?
O11 Rb1 B4 101.12(8) 1_565 3_676 ?
O10 Rb1 B4 79.14(7) 3_666 3_676 ?
O1 Rb1 B4 71.99(8) 1_565 3_676 ?
O3 Rb1 B4 138.68(8) 2_655 3_676 ?
O9 Rb1 B4 114.95(8) 3_666 3_676 ?
O7 Rb1 B4 23.13(7) 3_676 3_676 ?
B3 Rb1 B4 119.60(9) 2_655 3_676 ?
O2 Rb1 O9 139.97(7) . 4_475 ?
O6 Rb1 O9 42.76(6) 2_655 4_475 ?
O4 Rb1 O9 79.06(6) 3_676 4_475 ?
O11 Rb1 O9 171.62(6) 1_565 4_475 ?
O10 Rb1 O9 74.65(6) 3_666 4_475 ?
O1 Rb1 O9 77.71(6) 1_565 4_475 ?
O3 Rb1 O9 87.70(6) 2_655 4_475 ?
O9 Rb1 O9 64.27(3) 3_666 4_475 ?
O7 Rb1 O9 53.81(6) 3_676 4_475 ?
B3 Rb1 O9 64.20(7) 2_655 4_475 ?
B4 Rb1 O9 70.93(7) 3_676 4_475 ?
O9 Rb2 O5 123.41(7) 4_575 . ?
O9 Rb2 O10 82.87(7) 4_575 3_766 ?
O5 Rb2 O10 63.24(6) . 3_766 ?
O9 Rb2 O4 86.92(7) 4_575 3_776 ?
O5 Rb2 O4 108.62(6) . 3_776 ?
O10 Rb2 O4 58.97(6) 3_766 3_776 ?
O9 Rb2 O1 59.69(7) 4_575 2_655 ?
O5 Rb2 O1 79.62(7) . 2_655 ?
O10 Rb2 O1 96.44(7) 3_766 2_655 ?
O4 Rb2 O1 141.94(7) 3_776 2_655 ?
O9 Rb2 O11 150.04(7) 4_575 1_565 ?
O5 Rb2 O11 46.72(6) . 1_565 ?
O10 Rb2 O11 106.67(6) 3_766 1_565 ?
O4 Rb2 O11 122.56(6) 3_776 1_565 ?
O1 Rb2 O11 90.68(7) 2_655 1_565 ?
O9 Rb2 O6 63.48(7) 4_575 1_565 ?
O5 Rb2 O6 168.11(6) . 1_565 ?
O10 Rb2 O6 128.64(6) 3_766 1_565 ?
O4 Rb2 O6 80.45(6) 3_776 1_565 ?
O1 Rb2 O6 98.07(7) 2_655 1_565 ?
O11 Rb2 O6 122.07(6) 1_565 1_565 ?
O9 Rb2 O3 84.26(7) 4_575 1_565 ?
O5 Rb2 O3 127.82(6) . 1_565 ?
O10 Rb2 O3 166.67(6) 3_766 1_565 ?
O4 Rb2 O3 116.90(6) 3_776 1_565 ?
O1 Rb2 O3 79.93(6) 2_655 1_565 ?
O11 Rb2 O3 86.28(6) 1_565 1_565 ?
O6 Rb2 O3 40.57(6) 1_565 1_565 ?
O9 Rb2 O7 57.73(6) 4_575 3_776 ?
O5 Rb2 O7 149.13(6) . 3_776 ?
O10 Rb2 O7 87.77(6) 3_766 3_776 ?
O4 Rb2 O7 42.38(6) 3_776 3_776 ?
O1 Rb2 O7 116.10(6) 2_655 3_776 ?
O11 Rb2 O7 148.32(6) 1_565 3_776 ?
O6 Rb2 O7 41.96(5) 1_565 3_776 ?
O3 Rb2 O7 82.45(5) 1_565 3_776 ?
O9 Rb2 B4 79.40(8) 4_575 3_776 ?
O5 Rb2 B4 131.48(8) . 3_776 ?
O10 Rb2 B4 80.78(8) 3_766 3_776 ?
O4 Rb2 B4 23.84(8) 3_776 3_776 ?
O1 Rb2 B4 138.94(8) 2_655 3_776 ?
O11 Rb2 B4 129.60(8) 1_565 3_776 ?
O6 Rb2 B4 56.81(8) 1_565 3_776 ?
O3 Rb2 B4 93.48(7) 1_565 3_776 ?
O7 Rb2 B4 23.54(7) 3_776 3_776 ?
O9 Rb2 B6 164.23(9) 4_575 1_565 ?
O5 Rb2 B6 63.71(8) . 1_565 ?
O10 Rb2 B6 112.23(8) 3_766 1_565 ?
O4 Rb2 B6 104.51(8) 3_776 1_565 ?
O1 Rb2 B6 112.05(8) 2_655 1_565 ?
O11 Rb2 B6 23.61(8) 1_565 1_565 ?
O6 Rb2 B6 107.14(8) 1_565 1_565 ?
O3 Rb2 B6 80.89(8) 1_565 1_565 ?
O7 Rb2 B6 124.81(7) 3_776 1_565 ?
B4 Rb2 B6 106.68(9) 3_776 1_565 ?
O9 Rb2 B3 83.25(9) 4_575 1_565 ?
O5 Rb2 B3 145.49(8) . 1_565 ?
O10 Rb2 B3 149.18(8) 3_766 1_565 ?
O4 Rb2 B3 92.92(8) 3_776 1_565 ?
O1 Rb2 B3 100.03(8) 2_655 1_565 ?
O11 Rb2 B3 99.02(8) 1_565 1_565 ?
O6 Rb2 B3 23.05(7) 1_565 1_565 ?
O3 Rb2 B3 24.00(7) 1_565 1_565 ?
O7 Rb2 B3 61.60(7) 3_776 1_565 ?
B4 Rb2 B3 69.68(9) 3_776 1_565 ?
B6 Rb2 B3 85.32(9) 1_565 1_565 ?
B1 O2 B2 121.8(3) . . ?
B1 O2 Rb1 118.4(2) . . ?
B2 O2 Rb1 103.92(18) . . ?
B3 O5 B2 122.4(3) . . ?
B3 O5 Rb2 100.5(2) . . ?
B2 O5 Rb2 105.15(18) . . ?
B3 O5 Rb2 139.4(2) . 3_776 ?
B2 O5 Rb2 87.04(18) . 3_776 ?
Rb2 O5 Rb2 96.94(6) . 3_776 ?
B6 O10 B5 122.1(3) . . ?
B6 O10 Rb1 106.78(19) . 3_666 ?
B5 O10 Rb1 104.07(18) . 3_666 ?
B6 O10 Rb2 115.3(2) . 3_766 ?
B5 O10 Rb2 110.19(19) . 3_766 ?
Rb1 O10 Rb2 93.61(6) 3_666 3_766 ?
B1 O3 B3 118.1(3) . . ?
B1 O3 Rb1 132.5(2) . 2_645 ?
B3 O3 Rb1 91.3(2) . 2_645 ?
B1 O3 Rb2 126.4(2) . 1_545 ?
B3 O3 Rb2 81.09(18) . 1_545 ?
Rb1 O3 Rb2 92.52(6) 2_645 1_545 ?
B4 O4 B2 129.0(3) . . ?
B4 O4 Rb1 101.27(19) . 3_676 ?
B2 O4 Rb1 124.62(19) . 3_676 ?
B4 O4 Rb2 91.53(19) . 3_776 ?
B2 O4 Rb2 104.38(18) . 3_776 ?
Rb1 O4 Rb2 94.54(7) 3_676 3_776 ?
B4 O7 B5 119.1(3) . . ?
B4 O7 Rb1 87.35(18) . 3_676 ?
B5 O7 Rb1 153.1(2) . 3_676 ?
B4 O7 Rb2 78.66(18) . 3_776 ?
B5 O7 Rb2 105.00(18) . 3_776 ?
Rb1 O7 Rb2 83.36(5) 3_676 3_776 ?
B6 O11 B2 135.2(3) . 1_545 ?
B6 O11 Rb1 116.6(2) . 1_545 ?
B2 O11 Rb1 101.24(18) 1_545 1_545 ?
B6 O11 Rb2 89.94(19) . 1_545 ?
B2 O11 Rb2 99.87(18) 1_545 1_545 ?
Rb1 O11 Rb2 109.18(7) 1_545 1_545 ?
B5 O9 Rb2 156.8(2) . 4_576 ?
B5 O9 Rb1 96.05(19) . 3_666 ?
Rb2 O9 Rb1 98.79(7) 4_576 3_666 ?
B5 O9 Rb1 91.11(19) . 4_676 ?
Rb2 O9 Rb1 85.83(6) 4_576 4_676 ?
Rb1 O9 Rb1 147.68(9) 3_666 4_676 ?
B5 O9 H9 109(3) . . ?
Rb2 O9 H9 91(3) 4_576 . ?
Rb1 O9 H9 81(3) 3_666 . ?
Rb1 O9 H9 67(3) 4_676 . ?
B3 O6 B5 140.2(3) . 3_766 ?
B3 O6 Rb1 101.6(2) . 2_645 ?
B5 O6 Rb1 115.8(2) 3_766 2_645 ?
B3 O6 Rb2 82.1(2) . 1_545 ?
B5 O6 Rb2 105.75(19) 3_766 1_545 ?
Rb1 O6 Rb2 96.50(7) 2_645 1_545 ?
B3 O6 Rb2 71.33(19) . . ?
B5 O6 Rb2 83.92(17) 3_766 . ?
Rb1 O6 Rb2 107.96(8) 2_645 . ?
Rb2 O6 Rb2 146.71(8) 1_545 . ?
B4 O8 B6 120.2(3) . . ?
B4 O8 Rb2 135.4(2) . 1_545 ?
B6 O8 Rb2 75.43(18) . 1_545 ?
B1 O1 Rb2 124.8(2) . 2_645 ?
B1 O1 Rb1 114.3(2) . 1_545 ?
Rb2 O1 Rb1 120.33(8) 2_645 1_545 ?
B1 O1 H1 104(4) . . ?
Rb2 O1 H1 87(4) 2_645 . ?
Rb1 O1 H1 86(4) 1_545 . ?
O11 B6 O10 125.2(3) . . ?
O11 B6 O8 115.6(3) . . ?
O10 B6 O8 119.3(3) . . ?
O11 B6 Rb2 66.45(18) . 1_545 ?
O10 B6 Rb2 121.8(2) . 1_545 ?
O8 B6 Rb2 80.60(19) . 1_545 ?
O11 B6 Rb1 91.04(19) . 3_666 ?
O10 B6 Rb1 52.10(16) . 3_666 ?
O8 B6 Rb1 131.7(2) . 3_666 ?
Rb2 B6 Rb1 147.43(11) 1_545 3_666 ?
O11 B6 Rb1 44.75(16) . 1_545 ?
O10 B6 Rb1 144.8(2) . 1_545 ?
O8 B6 Rb1 82.02(19) . 1_545 ?
Rb2 B6 Rb1 87.30(9) 1_545 1_545 ?
Rb1 B6 Rb1 92.69(8) 3_666 1_545 ?
O11 B6 Rb2 88.77(19) . 3_766 ?
O10 B6 Rb2 45.79(16) . 3_766 ?
O8 B6 Rb2 141.9(2) . 3_766 ?
Rb2 B6 Rb2 83.64(8) 1_545 3_766 ?
Rb1 B6 Rb2 72.14(7) 3_666 3_766 ?
Rb1 B6 Rb2 131.62(10) 1_545 3_766 ?
O4 B4 O7 117.1(3) . . ?
O4 B4 O8 123.0(3) . . ?
O7 B4 O8 119.8(3) . . ?
O4 B4 Rb2 64.63(17) . 3_776 ?
O7 B4 Rb2 77.81(18) . 3_776 ?
O8 B4 Rb2 127.4(2) . 3_776 ?
O4 B4 Rb1 56.22(16) . 3_676 ?
O7 B4 Rb1 69.52(17) . 3_676 ?
O8 B4 Rb1 151.3(2) . 3_676 ?
Rb2 B4 Rb1 80.01(8) 3_776 3_676 ?
O9 B5 O10 111.6(3) . . ?
O9 B5 O6 109.1(3) . 3_766 ?
O10 B5 O6 111.9(3) . 3_766 ?
O9 B5 O7 105.6(3) . . ?
O10 B5 O7 111.3(3) . . ?
O6 B5 O7 107.1(3) 3_766 . ?
O9 B5 Rb1 60.66(17) . 3_666 ?
O10 B5 Rb1 52.90(15) . 3_666 ?
O6 B5 Rb1 141.3(2) 3_766 3_666 ?
O7 B5 Rb1 111.6(2) . 3_666 ?
O9 B5 Rb2 99.33(19) . 3_766 ?
O10 B5 Rb2 48.45(14) . 3_766 ?
O6 B5 Rb2 73.20(17) 3_766 3_766 ?
O7 B5 Rb2 153.2(2) . 3_766 ?
Rb1 B5 Rb2 72.31(7) 3_666 3_766 ?
O9 B5 Rb1 66.43(18) . 4_676 ?
O10 B5 Rb1 137.4(2) . 4_676 ?
O6 B5 Rb1 43.64(15) 3_766 4_676 ?
O7 B5 Rb1 109.8(2) . 4_676 ?
Rb1 B5 Rb1 119.00(10) 3_666 4_676 ?
Rb2 B5 Rb1 89.10(8) 3_766 4_676 ?
O4 B2 O2 110.8(3) . . ?
O4 B2 O11 110.3(3) . 1_565 ?
O2 B2 O11 107.0(3) . 1_565 ?
O4 B2 O5 110.1(3) . . ?
O2 B2 O5 111.4(3) . . ?
O11 B2 O5 107.1(3) 1_565 . ?
O4 B2 Rb1 124.2(2) . . ?
O2 B2 Rb1 52.39(15) . . ?
O11 B2 Rb1 54.63(15) 1_565 . ?
O5 B2 Rb1 125.7(2) . . ?
O4 B2 Rb2 133.9(2) . . ?
O2 B2 Rb2 115.3(2) . . ?
O11 B2 Rb2 56.47(16) 1_565 . ?
O5 B2 Rb2 51.51(15) . . ?
Rb1 B2 Rb2 86.27(9) . . ?
O4 B2 Rb2 53.00(15) . 3_776 ?
O2 B2 Rb2 159.2(2) . 3_776 ?
O11 B2 Rb2 92.16(18) 1_565 3_776 ?
O5 B2 Rb2 69.05(16) . 3_776 ?
Rb1 B2 Rb2 145.32(11) . 3_776 ?
Rb2 B2 Rb2 81.89(8) . 3_776 ?
O2 B1 O1 121.4(3) . . ?
O2 B1 O3 122.7(3) . . ?
O1 B1 O3 115.9(3) . . ?
O2 B1 Rb1 43.16(16) . . ?
O1 B1 Rb1 95.2(2) . . ?
O3 B1 Rb1 130.9(2) . . ?
O6 B3 O5 125.3(3) . . ?
O6 B3 O3 114.0(3) . . ?
O5 B3 O3 120.7(3) . . ?
O6 B3 Rb2 74.87(19) . 1_545 ?
O5 B3 Rb2 118.8(2) . 1_545 ?
O3 B3 Rb2 74.91(18) . 1_545 ?
O6 B3 Rb1 55.83(18) . 2_645 ?
O5 B3 Rb1 155.5(2) . 2_645 ?
O3 B3 Rb1 64.57(18) . 2_645 ?
Rb2 B3 Rb1 85.63(9) 1_545 2_645 ?
O6 B3 Rb2 87.0(2) . . ?
O5 B3 Rb2 56.84(17) . . ?
O3 B3 Rb2 131.7(2) . . ?
Rb2 B3 Rb2 152.91(12) 1_545 . ?
Rb1 B3 Rb2 100.81(10) 2_645 . ?

_refine_diff_density_max         0.637
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.118



####################################################################### 
# 
# 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_3_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2087569'
_audit_update_record             
;
2021-06-02 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;

_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            'B12 H4 Ba O22 Rb2'
_chemical_formula_weight         794.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.058(3)
_cell_length_b                   6.620(2)
_cell_length_c                   18.294(6)
_cell_angle_alpha                90
_cell_angle_beta                 117.603(7)
_cell_angle_gamma                90
_cell_volume                     972.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1532
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      24.20

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.713
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   0.4460
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    7.128
_shelx_estimated_absorpt_T_min   0.815
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5934
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.513
_diffrn_reflns_theta_max         24.611
_diffrn_reflns_theta_full        24.611
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1618
_reflns_number_gt                1247
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0649P)²+11.2632P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1618
_refine_ls_number_parameters     172
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.051
_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
Rb Rb 0.10689(13) 0.68306(14) 0.12205(7) 0.0369(3) Uani 1 1 d . . . . .
Ba Ba 0.67082(16) -0.10375(18) 0.65623(8) 0.0347(4) Uani 0.5 1 d . . P . .
O2 O 0.1447(6) 0.8603(7) 0.4066(3) 0.0124(11) Uani 1 1 d . U . . .
O7 O 0.1803(6) 0.2081(7) 0.5769(3) 0.0135(12) Uani 1 1 d . . . . .
O9 O 0.3591(7) 0.4235(8) 0.6875(3) 0.0167(12) Uani 1 1 d . . . . .
O4 O 0.3278(7) 0.9519(7) 0.5458(3) 0.0148(12) Uani 1 1 d . U . . .
O10 O 0.4737(6) 0.2459(8) 0.6122(3) 0.0149(12) Uani 1 1 d . . . . .
O3 O 0.1628(7) 0.5106(7) 0.3702(3) 0.0157(12) Uani 1 1 d . . . . .
O1 O 0.0748(7) 0.7579(8) 0.2676(3) 0.0195(13) Uani 1 1 d D . . . .
H1 H 0.007148 0.849029 0.248393 0.023 Uiso 1 1 d DR U . . .
O5 O 0.2852(7) 0.6139(8) 0.5102(3) 0.0171(12) Uani 1 1 d . U . . .
O8 O 0.1032(7) 0.3403(9) 0.6758(4) 0.0230(14) Uani 1 1 d . . . . .
O6 O 0.2629(7) 0.2640(7) 0.4710(3) 0.0159(12) Uani 1 1 d . U . . .
O11 O 0.6329(7) 0.4844(9) 0.7147(4) 0.0252(14) Uani 1 1 d D . . . .
H11 H 0.702024 0.436950 0.702460 0.030 Uiso 1 1 d DR U . . .
B3 B 0.2385(11) 0.4616(12) 0.4514(6) 0.0134(19) Uani 1 1 d . U . . .
B4 B 0.3114(12) 0.1707(13) 0.5504(6) 0.0156(19) Uani 1 1 d . . . . .
B2 B 0.2492(11) 0.8160(13) 0.4854(6) 0.0148(19) Uani 1 1 d . . . . .
B1 B 0.0691(11) 0.7038(12) 0.3432(5) 0.0115(18) Uani 1 1 d . . . . .
B5 B 0.2090(12) 0.3179(13) 0.6438(6) 0.017(2) Uani 1 1 d . . . . .
B6 B 0.4856(12) 0.3841(13) 0.6687(6) 0.017(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
Rb O1 2.853(6) . ?
Rb O7 2.887(5) 4_565 ?
Rb O2 2.988(5) 2_545 ?
Rb O6 3.020(6) 2 ?
Rb O11 3.030(7) 3_666 ?
Rb O4 3.055(5) 4_575 ?
Rb O9 3.302(6) 4_575 ?
Rb B2 3.302(9) 4_575 ?
Rb O8 3.309(6) 4_575 ?
Rb O3 3.318(5) 2 ?
Rb B3 3.332(8) 2 ?
Rb O7 3.357(6) 2 ?
Rb H1 3.0497 . ?
Ba O10 2.804(5) . ?
Ba O8 2.818(6) 2_646 ?
Ba O4 2.837(6) 1_545 ?
Ba O6 2.864(6) 3_656 ?
Ba O2 2.914(5) 3_666 ?
Ba O9 3.000(6) 2_646 ?
Ba O11 3.006(6) 1_545 ?
Ba O1 3.085(6) 3_666 ?
Ba O3 3.230(5) 3_656 ?
Ba B5 3.338(10) 2_646 ?
Ba B3 3.415(9) 3_656 ?
Ba B4 3.436(9) . ?
O2 B2 1.340(11) . ?
O2 B1 1.467(10) . ?
O7 B5 1.342(11) . ?
O7 B4 1.497(10) . ?
O9 B6 1.365(11) . ?
O9 B5 1.403(11) . ?
O4 B2 1.345(11) . ?
O4 B4 1.463(10) 1_565 ?
O10 B6 1.347(11) . ?
O10 B4 1.466(11) . ?
O3 B3 1.356(11) . ?
O3 B1 1.487(10) . ?
O1 B1 1.451(10) . ?
O1 H1 0.8146 . ?
O5 B3 1.390(10) . ?
O5 B2 1.402(10) . ?
O8 B5 1.341(11) . ?
O8 B1 1.464(10) 3_566 ?
O6 B3 1.347(10) . ?
O6 B4 1.446(11) . ?
O11 B6 1.374(11) . ?
O11 H11 0.8190 . ?

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 Rb O7 124.00(15) . 4_565 ?
O1 Rb O2 83.60(16) . 2_545 ?
O7 Rb O2 64.30(15) 4_565 2_545 ?
O1 Rb O6 85.96(16) . 2 ?
O7 Rb O6 109.87(14) 4_565 2 ?
O2 Rb O6 58.10(14) 2_545 2 ?
O1 Rb O11 60.83(15) . 3_666 ?
O7 Rb O11 77.11(15) 4_565 3_666 ?
O2 Rb O11 95.33(15) 2_545 3_666 ?
O6 Rb O11 140.69(15) 2 3_666 ?
O1 Rb O4 148.04(16) . 4_575 ?
O7 Rb O4 47.23(14) 4_565 4_575 ?
O2 Rb O4 108.57(14) 2_545 4_575 ?
O6 Rb O4 125.76(15) 2 4_575 ?
O11 Rb O4 88.17(15) 3_666 4_575 ?
O1 Rb O9 82.95(15) . 4_575 ?
O7 Rb O9 126.79(14) 4_565 4_575 ?
O2 Rb O9 166.20(15) 2_545 4_575 ?
O6 Rb O9 117.69(13) 2 4_575 ?
O11 Rb O9 80.78(14) 3_666 4_575 ?
O4 Rb O9 84.64(14) 4_575 4_575 ?
O1 Rb B2 162.0(2) . 4_575 ?
O7 Rb B2 64.07(18) 4_565 4_575 ?
O2 Rb B2 113.72(19) 2_545 4_575 ?
O6 Rb B2 107.0(2) 2 4_575 ?
O11 Rb B2 110.4(2) 3_666 4_575 ?
O4 Rb B2 24.03(18) 4_575 4_575 ?
O9 Rb B2 79.96(19) 4_575 4_575 ?
O1 Rb O8 62.48(15) . 4_575 ?
O7 Rb O8 167.22(14) 4_565 4_575 ?
O2 Rb O8 128.48(14) 2_545 4_575 ?
O6 Rb O8 80.63(14) 2 4_575 ?
O11 Rb O8 99.58(15) 3_666 4_575 ?
O4 Rb O8 120.87(13) 4_575 4_575 ?
O9 Rb O8 40.59(13) 4_575 4_575 ?
B2 Rb O8 106.51(18) 4_575 4_575 ?
O1 Rb O3 56.70(14) . 2 ?
O7 Rb O3 150.44(14) 4_565 2 ?
O2 Rb O3 87.60(13) 2_545 2 ?
O6 Rb O3 42.45(14) 2 2 ?
O11 Rb O3 116.66(14) 3_666 2 ?
O4 Rb O3 149.50(13) 4_575 2 ?
O9 Rb O3 82.43(13) 4_575 2 ?
B2 Rb O3 125.79(18) 4_575 2 ?
O8 Rb O3 41.88(13) 4_575 2 ?
O1 Rb B3 78.3(2) . 2 ?
O7 Rb B3 132.73(19) 4_565 2 ?
O2 Rb B3 80.08(18) 2_545 2 ?
O6 Rb B3 23.85(18) 2 2 ?
O11 Rb B3 139.1(2) 3_666 2 ?
O4 Rb B3 132.01(19) 4_575 2 ?
O9 Rb B3 94.14(18) 4_575 2 ?
B2 Rb B3 108.5(2) 4_575 2 ?
O8 Rb B3 56.99(18) 4_575 2 ?
O3 Rb B3 23.53(19) 2 2 ?
O1 Rb O7 129.85(15) . 2 ?
O7 Rb O7 84.23(14) 4_565 2 ?
O2 Rb O7 72.56(13) 2_545 2 ?
O6 Rb O7 43.95(13) 2 2 ?
O11 Rb O7 160.89(14) 3_666 2 ?
O4 Rb O7 82.06(14) 4_575 2 ?
O9 Rb O7 114.36(13) 4_575 2 ?
B2 Rb O7 63.71(19) 4_575 2 ?
O8 Rb O7 99.53(13) 4_575 2 ?
O3 Rb O7 78.37(13) 2 2 ?
B3 Rb O7 54.86(19) 2 2 ?
O1 Rb H1 15.4 . . ?
O7 Rb H1 136.7 4_565 . ?
O2 Rb H1 85.5 2_545 . ?
O6 Rb H1 73.9 2 . ?
O11 Rb H1 75.7 3_666 . ?
O4 Rb H1 159.7 4_575 . ?
O9 Rb H1 80.7 4_575 . ?
B2 Rb H1 158.4 4_575 . ?
O8 Rb H1 52.0 4_575 . ?
O3 Rb H1 41.4 2 . ?
B3 Rb H1 63.5 2 . ?
O7 Rb H1 116.8 2 . ?
O10 Ba O8 117.74(17) . 2_646 ?
O10 Ba O4 49.24(14) . 1_545 ?
O8 Ba O4 142.71(16) 2_646 1_545 ?
O10 Ba O6 114.70(16) . 3_656 ?
O8 Ba O6 121.20(16) 2_646 3_656 ?
O4 Ba O6 92.43(16) 1_545 3_656 ?
O10 Ba O2 80.52(15) . 3_666 ?
O8 Ba O2 104.09(16) 2_646 3_666 ?
O4 Ba O2 106.64(15) 1_545 3_666 ?
O6 Ba O2 60.64(15) 3_656 3_666 ?
O10 Ba O9 84.11(15) . 2_646 ?
O8 Ba O9 46.29(15) 2_646 2_646 ?
O4 Ba O9 96.78(15) 1_545 2_646 ?
O6 Ba O9 160.50(15) 3_656 2_646 ?
O2 Ba O9 131.62(15) 3_666 2_646 ?
O10 Ba O11 133.51(16) . 1_545 ?
O8 Ba O11 68.77(17) 2_646 1_545 ?
O4 Ba O11 95.91(15) 1_545 1_545 ?
O6 Ba O11 93.14(15) 3_656 1_545 ?
O2 Ba O11 145.39(15) 3_666 1_545 ?
O9 Ba O11 68.89(15) 2_646 1_545 ?
O10 Ba O1 76.10(15) . 3_666 ?
O8 Ba O1 65.93(16) 2_646 3_666 ?
O4 Ba O1 124.57(15) 1_545 3_666 ?
O6 Ba O1 104.35(15) 3_656 3_666 ?
O2 Ba O1 47.37(15) 3_666 3_666 ?
O9 Ba O1 84.45(15) 2_646 3_666 ?
O11 Ba O1 134.20(16) 1_545 3_666 ?
O10 Ba O3 157.61(16) . 3_656 ?
O8 Ba O3 84.27(16) 2_646 3_656 ?
O4 Ba O3 115.76(15) 1_545 3_656 ?
O6 Ba O3 44.07(14) 3_656 3_656 ?
O2 Ba O3 90.56(14) 3_666 3_656 ?
O9 Ba O3 116.55(14) 2_646 3_656 ?
O11 Ba O3 55.60(14) 1_545 3_656 ?
O1 Ba O3 112.57(15) 3_666 3_656 ?
O10 Ba B5 106.5(2) . 2_646 ?
O8 Ba B5 23.3(2) 2_646 2_646 ?
O4 Ba B5 119.6(2) 1_545 2_646 ?
O6 Ba B5 138.4(2) 3_656 2_646 ?
O2 Ba B5 124.23(19) 3_666 2_646 ?
O9 Ba B5 24.85(19) 2_646 2_646 ?
O11 Ba B5 60.15(19) 1_545 2_646 ?
O1 Ba B5 79.89(18) 3_666 2_646 ?
O3 Ba B5 95.52(19) 3_656 2_646 ?
O10 Ba B3 134.3(2) . 3_656 ?
O8 Ba B3 106.9(2) 2_646 3_656 ?
O4 Ba B3 98.98(19) 1_545 3_656 ?
O6 Ba B3 22.68(18) 3_656 3_656 ?
O2 Ba B3 79.71(17) 3_666 3_656 ?
O9 Ba B3 138.01(19) 2_646 3_656 ?
O11 Ba B3 70.94(19) 1_545 3_656 ?
O1 Ba B3 116.52(18) 3_666 3_656 ?
O3 Ba B3 23.34(18) 3_656 3_656 ?
B5 Ba B3 118.7(2) 2_646 3_656 ?
O10 Ba B4 24.60(19) . . ?
O8 Ba B4 134.7(2) 2_646 . ?
O4 Ba B4 24.68(18) 1_545 . ?
O6 Ba B4 103.8(2) 3_656 . ?
O2 Ba B4 92.98(18) 3_666 . ?
O9 Ba B4 91.44(19) 2_646 . ?
O11 Ba B4 116.45(19) 1_545 . ?
O1 Ba B4 100.16(19) 3_666 . ?
O3 Ba B4 137.95(19) 3_656 . ?
B5 Ba B4 116.3(2) 2_646 . ?
B3 Ba B4 117.4(2) 3_656 . ?
B2 O2 B1 122.3(6) . . ?
B2 O2 Ba 107.3(5) . 3_666 ?
B1 O2 Ba 102.8(4) . 3_666 ?
B2 O2 Rb 116.5(5) . 2 ?
B1 O2 Rb 109.1(4) . 2 ?
Ba O2 Rb 93.75(14) 3_666 2 ?
B5 O7 B4 122.5(7) . . ?
B5 O7 Rb 101.4(5) . 4_566 ?
B4 O7 Rb 105.5(4) . 4_566 ?
B5 O7 Rb 137.9(5) . 2_545 ?
B4 O7 Rb 88.5(5) . 2_545 ?
Rb O7 Rb 95.77(14) 4_566 2_545 ?
B6 O9 B5 117.8(7) . . ?
B6 O9 Ba 133.2(5) . 2_656 ?
B5 O9 Ba 91.2(5) . 2_656 ?
B6 O9 Rb 125.4(5) . 4_576 ?
B5 O9 Rb 82.1(4) . 4_576 ?
Ba O9 Rb 92.30(14) 2_656 4_576 ?
B2 O4 B4 132.8(7) . 1_565 ?
B2 O4 Ba 119.1(5) . 1_565 ?
B4 O4 Ba 101.2(5) 1_565 1_565 ?
B2 O4 Rb 88.3(4) . 4_576 ?
B4 O4 Rb 99.1(4) 1_565 4_576 ?
Ba O4 Rb 111.71(18) 1_565 4_576 ?
B6 O10 B4 121.2(6) . . ?
B6 O10 Ba 121.8(5) . . ?
B4 O10 Ba 102.6(4) . . ?
B3 O3 B1 119.4(6) . . ?
B3 O3 Ba 86.0(4) . 3_656 ?
B1 O3 Ba 154.4(5) . 3_656 ?
B3 O3 Rb 78.8(4) . 2_545 ?
B1 O3 Rb 105.0(4) . 2_545 ?
Ba O3 Rb 82.26(12) 3_656 2_545 ?
B1 O1 Rb 155.5(4) . . ?
B1 O1 Ba 95.8(4) . 3_666 ?
Rb O1 Ba 99.93(16) . 3_666 ?
B1 O1 H1 104.0 . . ?
Rb O1 H1 96.1 . . ?
Ba O1 H1 84.3 3_666 . ?
B3 O5 B2 120.1(7) . . ?
B3 O5 Rb 133.7(5) . 4_576 ?
B2 O5 Rb 73.4(4) . 4_576 ?
B5 O8 B1 140.7(7) . 3_566 ?
B5 O8 Ba 100.7(5) . 2_656 ?
B1 O8 Ba 116.1(5) 3_566 2_656 ?
B5 O8 Rb 82.5(5) . 4_576 ?
B1 O8 Rb 106.1(4) 3_566 4_576 ?
Ba O8 Rb 95.53(16) 2_656 4_576 ?
B5 O8 Rb 71.1(5) . 4_566 ?
B1 O8 Rb 83.5(4) 3_566 4_566 ?
Ba O8 Rb 109.25(19) 2_656 4_566 ?
Rb O8 Rb 146.37(19) 4_576 4_566 ?
B3 O6 B4 128.2(7) . . ?
B3 O6 Ba 102.3(5) . 3_656 ?
B4 O6 Ba 125.2(4) . 3_656 ?
B3 O6 Rb 91.2(5) . 2_545 ?
B4 O6 Rb 103.4(5) . 2_545 ?
Ba O6 Rb 94.09(16) 3_656 2_545 ?
B6 O11 Ba 117.3(5) . 1_565 ?
B6 O11 Rb 121.2(5) . 3_666 ?
Ba O11 Rb 121.17(18) 1_565 3_666 ?
B6 O11 H11 107.2 . . ?
Ba O11 H11 91.3 1_565 . ?
Rb O11 H11 77.6 3_666 . ?
O6 B3 O3 117.5(7) . . ?
O6 B3 O5 123.0(8) . . ?
O3 B3 O5 119.5(7) . . ?
O6 B3 Rb 65.0(4) . 2_545 ?
O3 B3 Rb 77.7(4) . 2_545 ?
O5 B3 Rb 127.3(5) . 2_545 ?
O6 B3 Ba 55.1(4) . 3_656 ?
O3 B3 Ba 70.7(4) . 3_656 ?
O5 B3 Ba 151.8(5) . 3_656 ?
Rb B3 Ba 79.35(19) 2_545 3_656 ?
O6 B4 O4 111.0(7) . 1_545 ?
O6 B4 O10 111.1(7) . . ?
O4 B4 O10 106.8(7) 1_545 . ?
O6 B4 O7 109.7(7) . . ?
O4 B4 O7 107.4(6) 1_545 . ?
O10 B4 O7 110.9(7) . . ?
O6 B4 Ba 124.0(5) . . ?
O4 B4 Ba 54.1(4) 1_545 . ?
O10 B4 Ba 52.8(4) . . ?
O7 B4 Ba 126.3(5) . . ?
O6 B4 Rb 132.6(5) . 4_566 ?
O4 B4 Rb 57.2(4) 1_545 4_566 ?
O10 B4 Rb 116.3(5) . 4_566 ?
O7 B4 Rb 50.8(3) . 4_566 ?
Ba B4 Rb 87.9(2) . 4_566 ?
O6 B4 Rb 53.8(4) . 2_545 ?
O4 B4 Rb 93.8(5) 1_545 2_545 ?
O10 B4 Rb 158.6(5) . 2_545 ?
O7 B4 Rb 67.2(4) . 2_545 ?
Ba B4 Rb 146.6(3) . 2_545 ?
Rb B4 Rb 79.92(19) 4_566 2_545 ?
O2 B2 O4 125.4(7) . . ?
O2 B2 O5 119.9(7) . . ?
O4 B2 O5 114.7(8) . . ?
O2 B2 Rb 119.0(5) . 4_576 ?
O4 B2 Rb 67.6(4) . 4_576 ?
O5 B2 Rb 82.6(5) . 4_576 ?
O2 B2 Rb 45.0(4) . 2 ?
O4 B2 Rb 89.8(5) . 2 ?
O5 B2 Rb 142.7(5) . 2 ?
Rb B2 Rb 81.61(19) 4_576 2 ?
O1 B1 O8 109.2(7) . 3_566 ?
O1 B1 O2 111.7(6) . . ?
O8 B1 O2 112.6(6) 3_566 . ?
O1 B1 O3 105.2(6) . . ?
O8 B1 O3 106.8(6) 3_566 . ?
O2 B1 O3 111.1(6) . . ?
O1 B1 Rb 99.1(4) . 2 ?
O8 B1 Rb 73.6(4) 3_566 2 ?
O2 B1 Rb 49.1(3) . 2 ?
O3 B1 Rb 153.8(5) . 2 ?
O8 B5 O7 125.6(8) . . ?
O8 B5 O9 113.3(8) . . ?
O7 B5 O9 121.1(8) . . ?
O8 B5 Ba 56.1(4) . 2_656 ?
O7 B5 Ba 155.7(6) . 2_656 ?
O9 B5 Ba 64.0(4) . 2_656 ?
O8 B5 Rb 74.5(5) . 4_576 ?
O7 B5 Rb 119.5(5) . 4_576 ?
O9 B5 Rb 73.9(4) . 4_576 ?
Ba B5 Rb 84.9(2) 2_656 4_576 ?
O8 B5 Rb 87.1(5) . 4_566 ?
O7 B5 Rb 55.9(4) . 4_566 ?
O9 B5 Rb 133.5(5) . 4_566 ?
Ba B5 Rb 102.2(2) 2_656 4_566 ?
Rb B5 Rb 152.2(3) 4_576 4_566 ?
O10 B6 O9 123.0(8) . . ?
O10 B6 O11 120.5(8) . . ?
O9 B6 O11 116.4(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O11 H11 O1 0.82 2.24 2.982(8) 150.6 3_666 yes
O11 H11 O3 0.82 2.21 2.915(8) 144.1 3_666 yes
O11 H11 O3 0.82 2.21 2.915(8) 144.1 3_666 yes
O11 H11 O1 0.82 2.24 2.982(8) 150.6 3_666 yes

_refine_diff_density_max         0.767
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.174



####################################################################### 
# 
# 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_1_a
_database_code_depnum_ccdc_archive 'CCDC 2087570'
_audit_update_record             
;
2021-06-02 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;

_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            'B5 H O9 Rb2'
_chemical_formula_weight         370.00

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'
B B 0.0013 0.0007 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -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+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   8.5942(9)
_cell_length_b                   7.6284(8)
_cell_length_c                   13.1321(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     860.94(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5085
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      30.83

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.855
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   0.419
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    11.395
_shelx_estimated_absorpt_T_min   0.659
_shelx_estimated_absorpt_T_max   0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11051
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.670
_diffrn_reflns_theta_max         31.544
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2665
_reflns_number_gt                2442
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.889
_reflns_Friedel_fraction_full    0.988

_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0094(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2665
_refine_ls_number_parameters     150
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0449
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_restrained_S_all      0.927
_refine_ls_shift/su_max          0.001
_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
O8 O 0.6843(3) 0.4955(3) 0.0942(2) 0.0169(6) Uani 1 1 d . . . . .
B4 B 0.6893(4) 0.6731(5) 0.0653(3) 0.0103(7) Uani 1 1 d . . . . .
O7 O 0.5708(3) 0.5745(3) 0.25387(19) 0.0141(5) Uani 1 1 d . . . . .
O6 O 0.6524(3) 0.7971(3) 0.13511(18) 0.0115(5) Uani 1 1 d . . . . .
Rb2 Rb 0.80337(4) 0.36659(4) 0.38347(3) 0.02035(10) Uani 1 1 d . . . . .
Rb1 Rb 0.65971(4) 1.08481(6) 0.61611(3) 0.02292(10) Uani 1 1 d . . . . .
O4 O 0.7739(3) 0.7031(3) 0.46767(19) 0.0121(5) Uani 1 1 d . . . . .
O2 O 0.7276(3) 0.9954(3) 0.40538(18) 0.0117(5) Uani 1 1 d . . . . .
O3 O 0.5331(3) 0.8787(3) 0.29509(19) 0.0106(5) Uani 1 1 d . . . . .
O1 O 0.4865(3) 1.1246(3) 0.40680(18) 0.0110(5) Uani 1 1 d . . . . .
O5 O 0.7955(3) 0.7622(3) 0.29014(18) 0.0110(5) Uani 1 1 d . . . . .
O9 O 0.5516(3) 0.2847(3) 0.1866(2) 0.0217(6) Uani 1 1 d D . . . .
H9 H 0.477(4) 0.272(8) 0.224(4) 0.054(18) Uiso 1 1 d D . . . .
B1 B 0.5792(4) 0.9973(5) 0.3665(3) 0.0085(7) Uani 1 1 d . . . . .
B5 B 0.5985(5) 0.4545(5) 0.1808(3) 0.0129(8) Uani 1 1 d . . . . .
B2 B 0.8215(4) 0.8368(4) 0.3908(4) 0.0084(7) Uani 1 1 d . . . . .
B3 B 0.6433(4) 0.7550(5) 0.2462(3) 0.0107(7) 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
O8 B5 1.391(5) . ?
O8 B4 1.408(5) . ?
O8 Rb2 2.939(3) 4_654 ?
O8 Rb1 3.419(3) 4_644 ?
B4 O4 1.340(5) 4_654 ?
B4 O6 1.355(5) . ?
B4 Rb2 3.342(4) 4_654 ?
B4 Rb1 3.463(4) 4_654 ?
B4 Rb1 3.585(4) 2_674 ?
O7 B5 1.347(5) . ?
O7 B3 1.514(4) . ?
O7 Rb2 2.895(2) 3_465 ?
O7 Rb2 3.067(3) . ?
O6 B3 1.496(5) . ?
O6 Rb1 2.736(2) 4_654 ?
O6 Rb1 2.841(2) 2_674 ?
Rb2 O4 2.807(3) . ?
Rb2 O2 2.919(2) 1_545 ?
Rb2 O3 2.957(3) 3_565 ?
Rb2 O5 3.258(3) . ?
Rb2 B5 3.261(4) . ?
Rb2 O1 3.304(2) 1_545 ?
Rb2 B1 3.420(3) 1_545 ?
Rb2 O9 3.428(3) . ?
Rb1 O3 2.889(3) 2_675 ?
Rb1 O2 2.909(2) . ?
Rb1 O9 3.056(3) 4_665 ?
Rb1 O1 3.141(2) . ?
Rb1 B3 3.345(4) 2_675 ?
Rb1 O5 3.380(3) 4_655 ?
Rb1 B1 3.417(4) . ?
Rb1 O9 3.479(3) 2_665 ?
O4 B2 1.492(5) . ?
O2 B1 1.374(5) . ?
O2 B2 1.467(4) . ?
O3 B1 1.361(4) . ?
O3 B3 1.483(4) . ?
O1 B1 1.363(4) . ?
O1 B2 1.463(4) 3_475 ?
O5 B3 1.431(4) . ?
O5 B2 1.457(5) . ?
O9 B5 1.358(5) . ?
O9 H9 0.818(14) . ?

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
B5 O8 B4 116.9(3) . . ?
B5 O8 Rb2 135.5(2) . 4_654 ?
B4 O8 Rb2 93.8(2) . 4_654 ?
B5 O8 Rb1 86.2(2) . 4_644 ?
B4 O8 Rb1 153.2(2) . 4_644 ?
Rb2 O8 Rb1 76.03(6) 4_654 4_644 ?
O4 B4 O6 125.6(3) 4_654 . ?
O4 B4 O8 115.5(3) 4_654 . ?
O6 B4 O8 118.9(3) . . ?
O4 B4 Rb2 55.38(18) 4_654 4_654 ?
O6 B4 Rb2 167.4(2) . 4_654 ?
O8 B4 Rb2 61.31(18) . 4_654 ?
O4 B4 Rb1 86.6(2) 4_654 4_654 ?
O6 B4 Rb1 47.48(16) . 4_654 ?
O8 B4 Rb1 146.3(2) . 4_654 ?
Rb2 B4 Rb1 139.90(12) 4_654 4_654 ?
O4 B4 Rb1 106.7(2) 4_654 2_674 ?
O6 B4 Rb1 47.04(16) . 2_674 ?
O8 B4 Rb1 114.8(2) . 2_674 ?
Rb2 B4 Rb1 120.60(11) 4_654 2_674 ?
Rb1 B4 Rb1 79.07(8) 4_654 2_674 ?
B5 O7 B3 119.9(3) . . ?
B5 O7 Rb2 131.6(2) . 3_465 ?
B3 O7 Rb2 102.97(18) . 3_465 ?
B5 O7 Rb2 85.9(2) . . ?
B3 O7 Rb2 103.82(18) . . ?
Rb2 O7 Rb2 105.75(8) 3_465 . ?
B4 O6 B3 121.5(3) . . ?
B4 O6 Rb1 111.1(2) . 4_654 ?
B3 O6 Rb1 106.99(18) . 4_654 ?
B4 O6 Rb1 112.5(2) . 2_674 ?
B3 O6 Rb1 95.97(18) . 2_674 ?
Rb1 O6 Rb1 107.15(8) 4_654 2_674 ?
O4 Rb2 O7 99.29(7) . 3_565 ?
O4 Rb2 O2 145.90(7) . 1_545 ?
O7 Rb2 O2 112.68(7) 3_565 1_545 ?
O4 Rb2 O8 47.64(7) . 4_655 ?
O7 Rb2 O8 118.24(7) 3_565 4_655 ?
O2 Rb2 O8 103.87(7) 1_545 4_655 ?
O4 Rb2 O3 142.52(7) . 3_565 ?
O7 Rb2 O3 48.50(6) 3_565 3_565 ?
O2 Rb2 O3 64.79(7) 1_545 3_565 ?
O8 Rb2 O3 123.86(7) 4_655 3_565 ?
O4 Rb2 O7 71.74(7) . . ?
O7 Rb2 O7 96.37(6) 3_565 . ?
O2 Rb2 O7 114.26(7) 1_545 . ?
O8 Rb2 O7 111.90(7) 4_655 . ?
O3 Rb2 O7 122.99(7) 3_565 . ?
O4 Rb2 O5 45.50(6) . . ?
O7 Rb2 O5 69.61(6) 3_565 . ?
O2 Rb2 O5 158.56(6) 1_545 . ?
O8 Rb2 O5 92.59(7) 4_655 . ?
O3 Rb2 O5 116.89(6) 3_565 . ?
O7 Rb2 O5 45.47(6) . . ?
O4 Rb2 B5 94.86(9) . . ?
O7 Rb2 B5 85.24(9) 3_565 . ?
O2 Rb2 B5 99.17(9) 1_545 . ?
O8 Rb2 B5 135.99(9) 4_655 . ?
O3 Rb2 B5 99.81(9) 3_565 . ?
O7 Rb2 B5 24.34(8) . . ?
O5 Rb2 B5 59.42(8) . . ?
O4 Rb2 O1 113.58(6) . 1_545 ?
O7 Rb2 O1 142.70(7) 3_565 1_545 ?
O2 Rb2 O1 42.71(6) 1_545 1_545 ?
O8 Rb2 O1 97.42(7) 4_655 1_545 ?
O3 Rb2 O1 103.48(6) 3_565 1_545 ?
O7 Rb2 O1 78.66(6) . 1_545 ?
O5 Rb2 O1 122.36(6) . 1_545 ?
B5 Rb2 O1 75.25(8) . 1_545 ?
O4 Rb2 B4 23.14(9) . 4_655 ?
O7 Rb2 B4 107.25(8) 3_565 4_655 ?
O2 Rb2 B4 127.74(8) 1_545 4_655 ?
O8 Rb2 B4 24.85(8) 4_655 4_655 ?
O3 Rb2 B4 135.27(8) 3_565 4_655 ?
O7 Rb2 B4 92.69(8) . 4_655 ?
O5 Rb2 B4 67.74(8) . 4_655 ?
B5 Rb2 B4 116.70(10) . 4_655 ?
O1 Rb2 B4 109.88(8) 1_545 4_655 ?
O4 Rb2 B1 136.74(8) . 1_545 ?
O7 Rb2 B1 122.45(8) 3_565 1_545 ?
O2 Rb2 B1 23.36(8) 1_545 1_545 ?
O8 Rb2 B1 110.94(8) 4_655 1_545 ?
O3 Rb2 B1 80.17(8) 3_565 1_545 ?
O7 Rb2 B1 91.29(8) . 1_545 ?
O5 Rb2 B1 136.61(7) . 1_545 ?
B5 Rb2 B1 79.15(9) . 1_545 ?
O1 Rb2 B1 23.31(7) 1_545 1_545 ?
B4 Rb2 B1 129.30(9) 4_655 1_545 ?
O4 Rb2 O9 114.00(7) . . ?
O7 Rb2 O9 94.93(7) 3_565 . ?
O2 Rb2 O9 75.93(7) 1_545 . ?
O8 Rb2 O9 142.54(7) 4_655 . ?
O3 Rb2 O9 90.58(7) 3_565 . ?
O7 Rb2 O9 42.65(7) . . ?
O5 Rb2 O9 82.64(6) . . ?
B5 Rb2 O9 23.25(9) . . ?
O1 Rb2 O9 56.50(6) 1_545 . ?
B4 Rb2 O9 132.69(8) 4_655 . ?
B1 Rb2 O9 56.31(8) 1_545 . ?
O6 Rb1 O6 143.48(6) 4_655 2_675 ?
O6 Rb1 O3 109.97(7) 4_655 2_675 ?
O6 Rb1 O3 49.94(7) 2_675 2_675 ?
O6 Rb1 O2 77.32(7) 4_655 . ?
O6 Rb1 O2 110.31(7) 2_675 . ?
O3 Rb1 O2 155.70(7) 2_675 . ?
O6 Rb1 O9 83.90(7) 4_655 4_665 ?
O6 Rb1 O9 125.57(7) 2_675 4_665 ?
O3 Rb1 O9 99.85(8) 2_675 4_665 ?
O2 Rb1 O9 104.03(7) . 4_665 ?
O6 Rb1 O1 115.91(7) 4_655 . ?
O6 Rb1 O1 66.34(6) 2_675 . ?
O3 Rb1 O1 115.52(7) 2_675 . ?
O2 Rb1 O1 44.37(6) . . ?
O9 Rb1 O1 126.99(7) 4_665 . ?
O6 Rb1 B3 134.89(8) 4_655 2_675 ?
O6 Rb1 B3 26.41(8) 2_675 2_675 ?
O3 Rb1 B3 26.23(8) 2_675 2_675 ?
O2 Rb1 B3 136.68(8) . 2_675 ?
O9 Rb1 B3 107.14(9) 4_665 2_675 ?
O1 Rb1 B3 92.46(8) . 2_675 ?
O6 Rb1 O5 44.54(6) 4_655 4_655 ?
O6 Rb1 O5 106.20(6) 2_675 4_655 ?
O3 Rb1 O5 65.51(6) 2_675 4_655 ?
O2 Rb1 O5 116.73(6) . 4_655 ?
O9 Rb1 O5 93.79(7) 4_665 4_655 ?
O1 Rb1 O5 135.73(6) . 4_655 ?
B3 Rb1 O5 90.53(8) 2_675 4_655 ?
O6 Rb1 B1 92.88(8) 4_655 . ?
O6 Rb1 B1 87.42(8) 2_675 . ?
O3 Rb1 B1 133.10(8) 2_675 . ?
O2 Rb1 B1 23.37(8) . . ?
O9 Rb1 B1 123.55(8) 4_665 . ?
O1 Rb1 B1 23.51(7) . . ?
B3 Rb1 B1 113.81(9) 2_675 . ?
O5 Rb1 B1 121.98(7) 4_655 . ?
O6 Rb1 O8 120.75(7) 4_655 4_665 ?
O6 Rb1 O8 94.99(6) 2_675 4_665 ?
O3 Rb1 O8 101.83(7) 2_675 4_665 ?
O2 Rb1 O8 93.21(7) . 4_665 ?
O9 Rb1 O8 41.41(6) 4_665 4_665 ?
O1 Rb1 O8 91.35(6) . 4_665 ?
B3 Rb1 O8 90.77(8) 2_675 4_665 ?
O5 Rb1 O8 132.78(6) 4_655 4_665 ?
B1 Rb1 O8 100.24(7) . 4_665 ?
O6 Rb1 B4 21.41(8) 4_655 4_655 ?
O6 Rb1 B4 131.17(8) 2_675 4_655 ?
O3 Rb1 B4 117.32(8) 2_675 4_655 ?
O2 Rb1 B4 61.91(8) . 4_655 ?
O9 Rb1 B4 101.94(8) 4_665 4_655 ?
O1 Rb1 B4 95.54(8) . 4_655 ?
B3 Rb1 B4 136.16(9) 2_675 4_655 ?
O5 Rb1 B4 55.07(8) 4_655 4_655 ?
B1 Rb1 B4 73.37(9) . 4_655 ?
O8 Rb1 B4 131.90(8) 4_665 4_655 ?
O6 Rb1 O9 68.52(7) 4_655 2_665 ?
O6 Rb1 O9 74.97(7) 2_675 2_665 ?
O3 Rb1 O9 64.04(7) 2_675 2_665 ?
O2 Rb1 O9 99.67(7) . 2_665 ?
O9 Rb1 O9 138.39(9) 4_665 2_665 ?
O1 Rb1 O9 93.66(6) . 2_665 ?
B3 Rb1 O9 75.75(8) 2_675 2_665 ?
O5 Rb1 O9 44.74(6) 4_655 2_665 ?
B1 Rb1 O9 89.50(8) . 2_665 ?
O8 Rb1 O9 165.79(7) 4_665 2_665 ?
B4 Rb1 O9 60.79(8) 4_655 2_665 ?
B4 O4 B2 134.4(3) 4_655 . ?
B4 O4 Rb2 101.5(2) 4_655 . ?
B2 O4 Rb2 109.5(2) . . ?
B4 O4 Rb1 71.8(2) 4_655 . ?
B2 O4 Rb1 83.64(19) . . ?
Rb2 O4 Rb1 165.31(9) . . ?
B1 O2 B2 118.1(2) . . ?
B1 O2 Rb1 99.5(2) . . ?
B2 O2 Rb1 115.3(2) . . ?
B1 O2 Rb2 99.23(17) . 1_565 ?
B2 O2 Rb2 131.63(19) . 1_565 ?
Rb1 O2 Rb2 84.91(6) . 1_565 ?
B1 O3 B3 122.4(3) . . ?
B1 O3 Rb1 131.5(2) . 2_674 ?
B3 O3 Rb1 94.32(19) . 2_674 ?
B1 O3 Rb2 110.1(2) . 3_465 ?
B3 O3 Rb2 101.15(19) . 3_465 ?
Rb1 O3 Rb2 89.85(7) 2_674 3_465 ?
B1 O1 B2 130.8(3) . 3_475 ?
B1 O1 Rb1 89.68(19) . . ?
B2 O1 Rb1 127.2(2) 3_475 . ?
B1 O1 Rb2 83.14(18) . 1_565 ?
B2 O1 Rb2 132.30(18) 3_475 1_565 ?
Rb1 O1 Rb2 75.20(5) . 1_565 ?
B3 O5 B2 121.4(3) . . ?
B3 O5 Rb2 97.74(19) . . ?
B2 O5 Rb2 90.98(18) . . ?
B3 O5 Rb1 81.94(19) . 4_654 ?
B2 O5 Rb1 108.18(19) . 4_654 ?
Rb2 O5 Rb1 157.86(8) . 4_654 ?
B5 O9 Rb1 102.6(2) . 4_644 ?
B5 O9 Rb2 71.4(2) . . ?
Rb1 O9 Rb2 78.88(7) 4_644 . ?
B5 O9 Rb1 155.9(2) . 2_664 ?
Rb1 O9 Rb1 86.49(6) 4_644 2_664 ?
Rb2 O9 Rb1 132.66(9) . 2_664 ?
B5 O9 H9 112(4) . . ?
Rb1 O9 H9 140(4) 4_644 . ?
Rb2 O9 H9 94(4) . . ?
Rb1 O9 H9 70(4) 2_664 . ?
O3 B1 O1 124.8(3) . . ?
O3 B1 O2 121.3(3) . . ?
O1 B1 O2 113.9(3) . . ?
O3 B1 Rb1 148.1(2) . . ?
O1 B1 Rb1 66.80(18) . . ?
O2 B1 Rb1 57.11(17) . . ?
O3 B1 Rb2 139.1(2) . 1_565 ?
O1 B1 Rb2 73.55(17) . 1_565 ?
O2 B1 Rb2 57.40(14) . 1_565 ?
Rb1 B1 Rb2 70.26(7) . 1_565 ?
O3 B1 Rb2 49.39(16) . 3_465 ?
O1 B1 Rb2 97.96(19) . 3_465 ?
O2 B1 Rb2 124.8(2) . 3_465 ?
Rb1 B1 Rb2 102.77(9) . 3_465 ?
Rb2 B1 Rb2 170.51(12) 1_565 3_465 ?
O7 B5 O9 123.8(3) . . ?
O7 B5 O8 121.5(3) . . ?
O9 B5 O8 114.6(3) . . ?
O7 B5 Rb2 69.8(2) . . ?
O9 B5 Rb2 85.3(2) . . ?
O8 B5 Rb2 115.3(2) . . ?
O7 B5 Rb1 143.3(3) . 4_644 ?
O9 B5 Rb1 55.81(19) . 4_644 ?
O8 B5 Rb1 71.17(19) . 4_644 ?
Rb2 B5 Rb1 73.75(8) . 4_644 ?
O5 B2 O1 110.9(3) . 3_575 ?
O5 B2 O2 110.8(3) . . ?
O1 B2 O2 110.4(3) 3_575 . ?
O5 B2 O4 107.7(3) . . ?
O1 B2 O4 107.9(3) 3_575 . ?
O2 B2 O4 109.0(3) . . ?
O5 B2 Rb2 65.10(16) . . ?
O1 B2 Rb2 104.28(18) 3_575 . ?
O2 B2 Rb2 143.5(2) . . ?
O4 B2 Rb2 47.44(15) . . ?
O5 B2 Rb1 148.2(2) . . ?
O1 B2 Rb1 98.3(2) 3_575 . ?
O2 B2 Rb1 44.14(18) . . ?
O4 B2 Rb1 73.2(2) . . ?
Rb2 B2 Rb1 120.36(11) . . ?
O5 B3 O3 112.6(3) . . ?
O5 B3 O6 109.7(3) . . ?
O3 B3 O6 108.6(3) . . ?
O5 B3 O7 112.6(3) . . ?
O3 B3 O7 106.7(3) . . ?
O6 B3 O7 106.3(3) . . ?
O5 B3 Rb1 154.6(2) . 2_674 ?
O3 B3 Rb1 59.45(16) . 2_674 ?
O6 B3 Rb1 57.62(15) . 2_674 ?
O7 B3 Rb1 92.63(19) . 2_674 ?
O5 B3 Rb1 74.04(18) . 4_654 ?
O3 B3 Rb1 93.61(19) . 4_654 ?
O6 B3 Rb1 48.74(15) . 4_654 ?
O7 B3 Rb1 152.8(2) . 4_654 ?
Rb1 B3 Rb1 82.18(9) 2_674 4_654 ?
O5 B3 Rb2 123.8(2) . 3_465 ?
O3 B3 Rb2 54.70(15) . 3_465 ?
O6 B3 Rb2 126.4(2) . 3_465 ?
O7 B3 Rb2 52.51(15) . 3_465 ?
Rb1 B3 Rb2 73.43(7) 2_674 3_465 ?
Rb1 B3 Rb2 146.83(12) 4_654 3_465 ?
O5 B3 Rb2 59.92(17) . . ?
O3 B3 Rb2 122.1(2) . . ?
O6 B3 Rb2 128.5(2) . . ?
O7 B3 Rb2 52.97(15) . . ?
Rb1 B3 Rb2 145.47(12) 2_674 . ?
Rb1 B3 Rb2 129.17(11) 4_654 . ?
Rb2 B3 Rb2 81.43(8) 3_465 . ?

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.100



####################################################################### 
# 
# 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_1_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2087571'
_audit_update_record             
;
2021-06-02 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;

_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            'B12 H3 Na2 O21 Rb'
_chemical_formula_weight         600.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Na Na 0.0362 0.0249 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'z, x, y'
'-z+1/2, -x, y+1/2'
'z+1/2, -x+1/2, -y'
'-z, x+1/2, -y+1/2'
'y, z, x'
'y+1/2, -z+1/2, -x'
'-y, z+1/2, -x+1/2'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'-z, -x, -y'
'z-1/2, x, -y-1/2'
'-z-1/2, x-1/2, y'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'-y-1/2, z-1/2, x'
'y, -z-1/2, x-1/2'
'y-1/2, z, -x-1/2'

_cell_length_a                   12.3596(11)
_cell_length_b                   12.3596(11)
_cell_length_c                   12.3596(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1888.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5140
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      27.85

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   0.6611
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.774
_shelx_estimated_absorpt_T_min   0.874
_shelx_estimated_absorpt_T_max   0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24211
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.686
_diffrn_reflns_theta_max         30.413
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             960
_reflns_number_gt                813
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0622P)²+0.7732P] 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_number_reflns         960
_refine_ls_number_parameters     72
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.124
_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
O1 O 0.29916(10) 0.52592(9) 0.29347(9) 0.0113(3) Uani 1 1 d . . . . .
O2 O 0.17547(9) 0.55556(9) 0.14747(10) 0.0121(3) Uani 1 1 d . . . . .
O3 O 0.19325(10) 0.38411(9) 0.23568(10) 0.0120(3) Uani 1 1 d . . . . .
O4 O 0.30581(8) 0.69419(8) 0.19419(8) 0.0057(4) Uani 1 3 d S T P . .
B1 B 0.22076(15) 0.48997(13) 0.22284(15) 0.0084(3) Uani 1 1 d . . . . .
B2 B 0.32974(13) 0.63939(13) 0.30270(13) 0.0066(3) Uani 1 1 d . . . . .
O5 O 0.4491(18) 0.941(2) 0.4492(15) 0.038(5) Uani 0.0833 1 d . U P . .
Rb Rb 0.500000 0.500000 0.500000 0.02394(18) Uani 1 6 d S T P . .
Na Na 0.65791(5) 0.65791(5) 0.65791(5) 0.0137(3) Uani 1 3 d S T P . .
O5A O 0.370(3) 1.0027(17) 0.484(2) 0.044(6) Uani 0.0833 1 d . U P . .


_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
O1 B1 1.378(2) . ?
O1 B2 1.4571(19) . ?
O1 Na 2.4093(12) 13_666 ?
O1 Rb 3.5750(12) . ?
O2 B1 1.356(2) . ?
O2 B2 1.4466(19) 6_564 ?
O2 Rb 2.9149(11) 2_564 ?
O3 B1 1.361(2) . ?
O3 B2 1.452(2) 24_556 ?
O3 Na 2.3203(14) 13_666 ?
O4 B2 1.5313(16) . ?
O4 B2 1.5314(16) 6_564 ?
O4 B2 1.5314(16) 11_655 ?
B1 Na 2.7860(19) 13_666 ?
B2 Rb 3.6527(17) . ?
O5 O5A 1.27(3) 22_765 ?
O5 O5A 1.32(3) . ?
O5 O5A 1.34(3) 8_656 ?
O5 O5 1.37(4) 22_765 ?
O5 O5 1.37(4) 20_575 ?
Rb Na 3.3804(12) 13_666 ?
Rb Na 3.3804(12) . ?

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
B1 O1 B2 122.85(13) . . ?
B1 O1 Na 90.51(10) . 13_666 ?
B2 O1 Na 146.20(10) . 13_666 ?
B1 O1 Rb 155.76(10) . . ?
B2 O1 Rb 81.38(8) . . ?
Na O1 Rb 65.45(4) 13_666 . ?
B1 O2 B2 123.81(13) . 6_564 ?
B1 O2 Rb 126.58(9) . 2_564 ?
B2 O2 Rb 109.05(9) 6_564 2_564 ?
B1 O3 B2 135.68(14) . 24_556 ?
B1 O3 Na 94.77(10) . 13_666 ?
B2 O3 Na 121.60(9) 24_556 13_666 ?
B2 O4 B2 118.11(4) . 6_564 ?
B2 O4 B2 118.10(4) . 11_655 ?
B2 O4 B2 118.11(4) 6_564 11_655 ?
O2 B1 O3 123.49(15) . . ?
O2 B1 O1 122.20(14) . . ?
O3 B1 O1 114.31(16) . . ?
O2 B1 Na 167.95(12) . 13_666 ?
O3 B1 Na 56.09(9) . 13_666 ?
O1 B1 Na 59.85(9) . 13_666 ?
O2 B2 O3 112.63(13) 11_655 19_665 ?
O2 B2 O1 109.59(13) 11_655 . ?
O3 B2 O1 110.55(12) 19_665 . ?
O2 B2 O4 108.79(11) 11_655 . ?
O3 B2 O4 107.25(13) 19_665 . ?
O1 B2 O4 107.88(12) . . ?
O2 B2 Rb 48.96(7) 11_655 . ?
O3 B2 Rb 94.27(8) 19_665 . ?
O1 B2 Rb 75.39(8) . . ?
O4 B2 Rb 154.76(10) . . ?
O5A O5 O5A 111(2) 22_765 . ?
O5A O5 O5A 109(2) 22_765 8_656 ?
O5A O5 O5A 134(2) . 8_656 ?
O5A O5 O5 60(2) 22_765 22_765 ?
O5A O5 O5 134(2) . 22_765 ?
O5A O5 O5 55.8(13) 8_656 22_765 ?
O5A O5 O5 61(2) 22_765 20_575 ?
O5A O5 O5 56.4(13) . 20_575 ?
O5A O5 O5 133.2(18) 8_656 20_575 ?
O5 O5 O5 86(2) 22_765 20_575 ?
O2 Rb O2 180.0 23_566 11_655 ?
O2 Rb O2 115.928(15) 23_566 19_665 ?
O2 Rb O2 64.072(15) 11_655 19_665 ?
O2 Rb O2 64.072(15) 23_566 7_556 ?
O2 Rb O2 115.928(15) 11_655 7_556 ?
O2 Rb O2 180.0 19_665 7_556 ?
O2 Rb O2 115.928(15) 23_566 14_656 ?
O2 Rb O2 64.072(15) 11_655 14_656 ?
O2 Rb O2 115.928(15) 19_665 14_656 ?
O2 Rb O2 64.072(15) 7_556 14_656 ?
O2 Rb O2 64.072(15) 23_566 2_565 ?
O2 Rb O2 115.928(15) 11_655 2_565 ?
O2 Rb O2 64.072(15) 19_665 2_565 ?
O2 Rb O2 115.928(15) 7_556 2_565 ?
O2 Rb O2 180.0 14_656 2_565 ?
O2 Rb Na 101.80(2) 23_566 13_666 ?
O2 Rb Na 78.20(2) 11_655 13_666 ?
O2 Rb Na 101.80(2) 19_665 13_666 ?
O2 Rb Na 78.20(2) 7_556 13_666 ?
O2 Rb Na 101.80(2) 14_656 13_666 ?
O2 Rb Na 78.20(2) 2_565 13_666 ?
O2 Rb Na 78.20(2) 23_566 . ?
O2 Rb Na 101.80(2) 11_655 . ?
O2 Rb Na 78.20(2) 19_665 . ?
O2 Rb Na 101.80(2) 7_556 . ?
O2 Rb Na 78.20(2) 14_656 . ?
O2 Rb Na 101.80(2) 2_565 . ?
Na Rb Na 180.0 13_666 . ?
O2 Rb O1 92.81(3) 23_566 9 ?
O2 Rb O1 87.19(3) 11_655 9 ?
O2 Rb O1 138.66(3) 19_665 9 ?
O2 Rb O1 41.34(3) 7_556 9 ?
O2 Rb O1 70.57(3) 14_656 9 ?
O2 Rb O1 109.43(3) 2_565 9 ?
Na Rb O1 40.412(19) 13_666 9 ?
Na Rb O1 139.588(19) . 9 ?
O2 Rb O1 109.43(3) 23_566 17_666 ?
O2 Rb O1 70.57(3) 11_655 17_666 ?
O2 Rb O1 87.19(3) 19_665 17_666 ?
O2 Rb O1 92.81(3) 7_556 17_666 ?
O2 Rb O1 41.34(3) 14_656 17_666 ?
O2 Rb O1 138.66(3) 2_565 17_666 ?
Na Rb O1 139.588(19) 13_666 17_666 ?
Na Rb O1 40.412(19) . 17_666 ?
O1 Rb O1 111.69(3) 9 17_666 ?
O2 Rb O1 70.57(3) 23_566 5 ?
O2 Rb O1 109.43(3) 11_655 5 ?
O2 Rb O1 92.81(3) 19_665 5 ?
O2 Rb O1 87.19(3) 7_556 5 ?
O2 Rb O1 138.66(3) 14_656 5 ?
O2 Rb O1 41.34(3) 2_565 5 ?
Na Rb O1 40.412(19) 13_666 5 ?
Na Rb O1 139.588(19) . 5 ?
O1 Rb O1 68.31(3) 9 5 ?
O1 Rb O1 180.0 17_666 5 ?
O2 Rb O1 41.34(3) 23_566 13_666 ?
O2 Rb O1 138.66(3) 11_655 13_666 ?
O2 Rb O1 109.43(3) 19_665 13_666 ?
O2 Rb O1 70.57(3) 7_556 13_666 ?
O2 Rb O1 87.19(3) 14_656 13_666 ?
O2 Rb O1 92.81(3) 2_565 13_666 ?
Na Rb O1 139.588(19) 13_666 13_666 ?
Na Rb O1 40.412(19) . 13_666 ?
O1 Rb O1 111.69(3) 9 13_666 ?
O1 Rb O1 68.31(3) 17_666 13_666 ?
O1 Rb O1 111.69(3) 5 13_666 ?
O3 Na O3 81.66(5) 21_666 17_666 ?
O3 Na O3 81.66(5) 21_666 13_666 ?
O3 Na O3 81.66(5) 17_666 13_666 ?
O3 Na O1 112.71(4) 21_666 13_666 ?
O3 Na O1 132.74(5) 17_666 13_666 ?
O3 Na O1 58.19(4) 13_666 13_666 ?
O3 Na O1 58.19(4) 21_666 21_666 ?
O3 Na O1 112.71(4) 17_666 21_666 ?
O3 Na O1 132.74(5) 13_666 21_666 ?
O1 Na O1 112.83(3) 13_666 21_666 ?
O3 Na O1 132.74(5) 21_666 17_666 ?
O3 Na O1 58.19(4) 17_666 17_666 ?
O3 Na O1 112.71(4) 13_666 17_666 ?
O1 Na O1 112.83(3) 13_666 17_666 ?
O1 Na O1 112.83(3) 21_666 17_666 ?
O3 Na B1 29.13(4) 21_666 21_666 ?
O3 Na B1 94.18(5) 17_666 21_666 ?
O3 Na B1 109.48(6) 13_666 21_666 ?
O1 Na B1 120.61(5) 13_666 21_666 ?
O1 Na B1 29.64(5) 21_666 21_666 ?
O1 Na B1 123.69(5) 17_666 21_666 ?
O3 Na B1 109.48(6) 21_666 17_666 ?
O3 Na B1 29.13(4) 17_666 17_666 ?
O3 Na B1 94.18(5) 13_666 17_666 ?
O1 Na B1 123.69(5) 13_666 17_666 ?
O1 Na B1 120.61(5) 21_666 17_666 ?
O1 Na B1 29.64(5) 17_666 17_666 ?
B1 Na B1 114.55(3) 21_666 17_666 ?
O3 Na B1 94.18(5) 21_666 13_666 ?
O3 Na B1 109.48(6) 17_666 13_666 ?
O3 Na B1 29.13(4) 13_666 13_666 ?
O1 Na B1 29.64(5) 13_666 13_666 ?
O1 Na B1 123.69(5) 21_666 13_666 ?
O1 Na B1 120.61(5) 17_666 13_666 ?
B1 Na B1 114.55(3) 21_666 13_666 ?
B1 Na B1 114.55(3) 17_666 13_666 ?
O3 Na Rb 130.98(4) 21_666 . ?
O3 Na Rb 130.98(4) 17_666 . ?
O3 Na Rb 130.98(4) 13_666 . ?
O1 Na Rb 74.14(4) 13_666 . ?
O1 Na Rb 74.14(4) 21_666 . ?
O1 Na Rb 74.14(4) 17_666 . ?
B1 Na Rb 103.74(4) 21_666 . ?
B1 Na Rb 103.74(4) 17_666 . ?
B1 Na Rb 103.74(4) 13_666 . ?
O5 O5A O5 64(2) 20_575 . ?
O5 O5A O5 63(2) 20_575 10_466 ?
O5 O5A O5 89(3) . 10_466 ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
B2 O2 B1 O3 174.41(15) 6_564 . . . ?
Rb O2 B1 O3 4.0(2) 2_564 . . . ?
B2 O2 B1 O1 -5.5(3) 6_564 . . . ?
Rb O2 B1 O1 -175.92(11) 2_564 . . . ?
B2 O2 B1 Na -101.6(6) 6_564 . . 13_666 ?
Rb O2 B1 Na 87.9(6) 2_564 . . 13_666 ?
B2 O3 B1 O2 18.6(3) 24_556 . . . ?
Na O3 B1 O2 165.51(15) 13_666 . . . ?
B2 O3 B1 O1 -161.54(15) 24_556 . . . ?
Na O3 B1 O1 -14.60(15) 13_666 . . . ?
B2 O3 B1 Na -146.94(19) 24_556 . . 13_666 ?
B2 O1 B1 O2 8.2(3) . . . . ?
Na O1 B1 O2 -166.11(15) 13_666 . . . ?
Rb O1 B1 O2 -173.15(15) . . . . ?
B2 O1 B1 O3 -171.73(13) . . . . ?
Na O1 B1 O3 14.00(14) 13_666 . . . ?
Rb O1 B1 O3 7.0(4) . . . . ?
B2 O1 B1 Na 174.27(16) . . . 13_666 ?
Rb O1 B1 Na -7.0(2) . . . 13_666 ?
B1 O1 B2 O2 -144.93(15) . . . 11_655 ?
Na O1 B2 O2 24.7(2) 13_666 . . 11_655 ?
Rb O1 B2 O2 35.62(10) . . . 11_655 ?
B1 O1 B2 O3 90.34(17) . . . 19_665 ?
Na O1 B2 O3 -99.99(18) 13_666 . . 19_665 ?
Rb O1 B2 O3 -89.11(10) . . . 19_665 ?
B1 O1 B2 O4 -26.6(2) . . . . ?
Na O1 B2 O4 143.03(14) 13_666 . . . ?
Rb O1 B2 O4 153.91(11) . . . . ?
B1 O1 B2 Rb 179.45(15) . . . . ?
Na O1 B2 Rb -10.88(16) 13_666 . . . ?
B2 O4 B2 O2 163.93(11) 6_564 . . 11_655 ?
B2 O4 B2 O2 -43.1(2) 11_655 . . 11_655 ?
B2 O4 B2 O3 -73.98(18) 6_564 . . 19_665 ?
B2 O4 B2 O3 78.98(17) 11_655 . . 19_665 ?
B2 O4 B2 O1 45.1(2) 6_564 . . . ?
B2 O4 B2 O1 -161.92(12) 11_655 . . . ?
B2 O4 B2 Rb 138.71(16) 6_564 . . . ?
B2 O4 B2 Rb -68.3(3) 11_655 . . . ?
O5A O5 O5A O5 -29(3) 22_765 . . 20_575 ?
O5A O5 O5A O5 120(3) 8_656 . . 20_575 ?
O5 O5 O5A O5 39(3) 22_765 . . 20_575 ?
O5A O5 O5A O5 -89(2) 22_765 . . 10_466 ?
O5A O5 O5A O5 60(4) 8_656 . . 10_466 ?
O5 O5 O5A O5 -22(4) 22_765 . . 10_466 ?
O5 O5 O5A O5 -60.5(17) 20_575 . . 10_466 ?

_refine_diff_density_max         0.660
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.127



