# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1520110'
_audit_update_record             
;
2016-11-30 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H5 B7 Cs2 O14'
_chemical_formula_weight         570.53

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.356(10)
_cell_length_b                   11.971(14)
_cell_length_c                   14.109(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.520(12)
_cell_angle_gamma                90.00
_cell_volume                     1372(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1665
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.00

_exptl_crystal_description       blcok
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    5.382
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8199
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         27.51
_reflns_number_total             3135
_reflns_number_gt                2220
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00414(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3135
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0548
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B -0.0427(8) 0.3934(6) 0.7018(4) 0.0253(15) Uani 1 1 d . . .
B2 B -0.2638(7) 1.0843(5) 0.2845(4) 0.0223(14) Uani 1 1 d . . .
B3 B 0.4623(8) 1.2430(6) 0.5191(4) 0.0230(15) Uani 1 1 d . . .
B4 B 0.2652(7) 1.1954(6) 0.6224(4) 0.0247(15) Uani 1 1 d . . .
B5 B 0.4691(8) 0.6190(6) 0.5934(4) 0.0261(16) Uani 1 1 d . . .
B6 B 0.5539(7) 1.1841(6) 0.3686(4) 0.0223(14) Uani 1 1 d . . .
B7 B -0.0456(7) 0.7203(6) 0.8001(4) 0.0254(16) Uani 1 1 d . . .
Cs1 Cs 0.02650(4) 0.65870(4) 0.56622(2) 0.03501(13) Uani 1 1 d . . .
Cs2 Cs 0.22495(4) 0.98822(3) 0.41835(3) 0.03339(13) Uani 1 1 d . . .
H1 H 0.456(8) 0.474(6) 0.585(4) 0.040 Uiso 1 1 d . . .
H2 H -0.097(7) 1.042(6) 0.233(4) 0.040 Uiso 1 1 d . . .
H3 H -0.246(7) 0.746(5) 0.721(4) 0.040 Uiso 1 1 d . . .
H4 H -0.097(7) 0.834(6) 0.319(4) 0.040 Uiso 1 1 d . . .
H5 H -0.249(7) 0.390(5) 0.620(4) 0.040 Uiso 1 1 d . . .
O1 O 0.5056(4) 1.1625(3) 0.4564(2) 0.0218(8) Uani 1 1 d . . .
O2 O 0.4160(4) 0.7570(3) 0.3841(2) 0.0232(9) Uani 1 1 d . . .
O3 O 0.2958(4) 1.2197(3) 0.5357(2) 0.0225(9) Uani 1 1 d . . .
O4 O 0.1144(4) 0.4271(3) 0.7001(2) 0.0268(9) Uani 1 1 d . . .
O5 O -0.1081(5) 1.0521(4) 0.2830(3) 0.0360(11) Uani 1 1 d . . .
O6 O 0.4210(4) 1.1445(3) 0.2835(2) 0.0264(9) Uani 1 1 d . . .
O7 O -0.1087(5) 0.8246(4) 0.3716(3) 0.0409(12) Uani 1 1 d . . .
O8 O 0.4624(4) 1.3574(3) 0.4820(2) 0.0231(9) Uani 1 1 d . . .
O9 O 0.1110(4) 0.6905(4) 0.7948(2) 0.0339(11) Uani 1 1 d . . .
O10 O 0.4232(4) 0.6969(3) 0.6493(2) 0.0275(9) Uani 1 1 d . . .
O11 O 0.2927(4) 0.8754(3) 0.6331(2) 0.0276(10) Uani 1 1 d . . .
O12 O -0.1583(5) 0.7247(5) 0.7136(3) 0.0503(15) Uani 1 1 d . . .
O13 O -0.1572(5) 0.4064(4) 0.6162(3) 0.0421(13) Uani 1 1 d . . .
O14 O 0.4381(7) 0.5109(4) 0.6132(3) 0.0436(13) 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
B1 O6 1.337(7) 4_576 ?
B1 O13 1.363(7) . ?
B1 O4 1.379(7) . ?
B1 Cs1 3.821(8) . ?
B1 Cs1 3.866(7) 3_566 ?
B2 O11 1.333(7) 3_576 ?
B2 O5 1.362(7) . ?
B2 O4 1.380(6) 4_575 ?
B3 O1 1.411(7) . ?
B3 O8 1.465(7) . ?
B3 O3 1.490(7) . ?
B3 O2 1.500(6) 3_676 ?
B3 Cs2 3.733(7) . ?
B3 Cs2 3.768(7) 3_676 ?
B4 O3 1.339(7) . ?
B4 O7 1.351(7) 3_576 ?
B4 O9 1.369(6) 2_556 ?
B4 Cs1 3.611(7) 3_576 ?
B4 Cs2 3.755(7) . ?
B5 O10 1.334(7) . ?
B5 O8 1.350(7) 3_676 ?
B5 O14 1.362(8) . ?
B5 Cs1 3.659(8) . ?
B6 O1 1.414(6) . ?
B6 O10 1.467(8) 3_676 ?
B6 O11 1.471(7) 3_676 ?
B6 O6 1.508(6) . ?
B6 Cs2 3.757(7) 3_676 ?
B6 Cs2 3.801(7) . ?
B6 Cs1 3.896(7) 3_676 ?
B7 O2 1.327(6) 4_576 ?
B7 O12 1.358(6) . ?
B7 O9 1.375(7) . ?
B7 Cs1 3.567(7) . ?
B7 Cs2 3.766(7) 4_576 ?
Cs1 O12 2.972(4) . ?
Cs1 O3 3.104(4) 3_576 ?
Cs1 O13 3.121(5) 3_566 ?
Cs1 O9 3.158(5) . ?
Cs1 O10 3.280(5) . ?
Cs1 O4 3.338(5) . ?
Cs1 O7 3.363(5) . ?
Cs1 O11 3.404(5) . ?
Cs1 O13 3.533(6) . ?
Cs1 B4 3.611(7) 3_576 ?
Cs2 O5 3.081(5) . ?
Cs2 O1 3.091(4) . ?
Cs2 O1 3.096(4) 3_676 ?
Cs2 O3 3.211(5) . ?
Cs2 O11 3.244(5) . ?
Cs2 O2 3.287(5) . ?
Cs2 O7 3.345(5) . ?
Cs2 O6 3.356(4) . ?
Cs2 B6 3.757(7) 3_676 ?
Cs2 B7 3.766(7) 4_675 ?
O1 Cs2 3.096(4) 3_676 ?
O2 B7 1.327(6) 4_675 ?
O2 B3 1.500(6) 3_676 ?
O3 Cs1 3.104(4) 3_576 ?
O4 B2 1.380(6) 4_676 ?
O4 Cs1 3.807(5) 3_566 ?
O6 B1 1.337(7) 4_675 ?
O7 B4 1.351(7) 3_576 ?
O8 B5 1.350(7) 3_676 ?
O9 B4 1.369(6) 2_546 ?
O10 B6 1.467(8) 3_676 ?
O11 B2 1.333(7) 3_576 ?
O11 B6 1.471(7) 3_676 ?
O13 Cs1 3.121(5) 3_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 B1 O13 123.3(5) 4_576 . ?
O6 B1 O4 121.5(5) 4_576 . ?
O13 B1 O4 115.1(5) . . ?
O6 B1 Cs1 143.6(4) 4_576 . ?
O13 B1 Cs1 67.6(3) . . ?
O4 B1 Cs1 59.5(3) . . ?
O6 B1 Cs1 148.7(4) 4_576 3_566 ?
O13 B1 Cs1 47.9(3) . 3_566 ?
O4 B1 Cs1 77.2(3) . 3_566 ?
Cs1 B1 Cs1 66.44(12) . 3_566 ?
O11 B2 O5 119.0(5) 3_576 . ?
O11 B2 O4 122.7(5) 3_576 4_575 ?
O5 B2 O4 118.3(5) . 4_575 ?
O1 B3 O8 113.1(4) . . ?
O1 B3 O3 110.9(5) . . ?
O8 B3 O3 108.1(5) . . ?
O1 B3 O2 110.6(5) . 3_676 ?
O8 B3 O2 105.5(5) . 3_676 ?
O3 B3 O2 108.4(4) . 3_676 ?
O1 B3 Cs2 52.8(3) . . ?
O8 B3 Cs2 132.2(3) . . ?
O3 B3 Cs2 58.3(3) . . ?
O2 B3 Cs2 122.2(4) 3_676 . ?
O1 B3 Cs2 51.6(3) . 3_676 ?
O8 B3 Cs2 135.4(4) . 3_676 ?
O3 B3 Cs2 116.6(4) . 3_676 ?
O2 B3 Cs2 60.1(3) 3_676 3_676 ?
Cs2 B3 Cs2 76.50(16) . 3_676 ?
O3 B4 O7 119.4(5) . 3_576 ?
O3 B4 O9 121.4(5) . 2_556 ?
O7 B4 O9 119.2(5) 3_576 2_556 ?
O3 B4 Cs1 57.5(3) . 3_576 ?
O7 B4 Cs1 68.6(3) 3_576 3_576 ?
O9 B4 Cs1 153.5(4) 2_556 3_576 ?
O3 B4 Cs2 56.3(3) . . ?
O7 B4 Cs2 91.0(4) 3_576 . ?
O9 B4 Cs2 122.7(4) 2_556 . ?
Cs1 B4 Cs2 80.24(14) 3_576 . ?
O10 B5 O8 123.6(6) . 3_676 ?
O10 B5 O14 116.6(5) . . ?
O8 B5 O14 119.8(6) 3_676 . ?
O10 B5 Cs1 63.1(3) . . ?
O8 B5 Cs1 119.6(4) 3_676 . ?
O14 B5 Cs1 84.7(4) . . ?
O1 B6 O10 113.8(5) . 3_676 ?
O1 B6 O11 110.7(5) . 3_676 ?
O10 B6 O11 108.5(4) 3_676 3_676 ?
O1 B6 O6 109.4(4) . . ?
O10 B6 O6 105.7(4) 3_676 . ?
O11 B6 O6 108.5(4) 3_676 . ?
O1 B6 Cs2 52.1(3) . 3_676 ?
O10 B6 Cs2 127.7(3) 3_676 3_676 ?
O11 B6 Cs2 58.6(2) 3_676 3_676 ?
O6 B6 Cs2 126.7(4) . 3_676 ?
O1 B6 Cs2 50.1(3) . . ?
O10 B6 Cs2 139.5(3) 3_676 . ?
O11 B6 Cs2 112.0(4) 3_676 . ?
O6 B6 Cs2 61.6(3) . . ?
Cs2 B6 Cs2 75.82(14) 3_676 . ?
O1 B6 Cs1 107.9(3) . 3_676 ?
O10 B6 Cs1 54.9(2) 3_676 3_676 ?
O11 B6 Cs1 59.9(3) 3_676 3_676 ?
O6 B6 Cs1 142.6(3) . 3_676 ?
Cs2 B6 Cs1 80.15(12) 3_676 3_676 ?
Cs2 B6 Cs1 154.71(17) . 3_676 ?
O2 B7 O12 122.3(5) 4_576 . ?
O2 B7 O9 122.3(5) 4_576 . ?
O12 B7 O9 115.4(5) . . ?
O2 B7 Cs1 175.8(4) 4_576 . ?
O12 B7 Cs1 53.7(3) . . ?
O9 B7 Cs1 61.8(2) . . ?
O2 B7 Cs2 59.0(3) 4_576 4_576 ?
O12 B7 Cs2 96.1(4) . 4_576 ?
O9 B7 Cs2 116.2(4) . 4_576 ?
Cs1 B7 Cs2 119.09(19) . 4_576 ?
O12 Cs1 O3 70.29(12) . 3_576 ?
O12 Cs1 O13 169.30(10) . 3_566 ?
O3 Cs1 O13 99.68(11) 3_576 3_566 ?
O12 Cs1 O9 44.15(11) . . ?
O3 Cs1 O9 112.28(9) 3_576 . ?
O13 Cs1 O9 146.54(10) 3_566 . ?
O12 Cs1 O10 111.11(12) . . ?
O3 Cs1 O10 142.70(11) 3_576 . ?
O13 Cs1 O10 79.06(11) 3_566 . ?
O9 Cs1 O10 69.66(8) . . ?
O12 Cs1 O4 84.64(13) . . ?
O3 Cs1 O4 134.76(9) 3_576 . ?
O13 Cs1 O4 100.72(12) 3_566 . ?
O9 Cs1 O4 63.59(11) . . ?
O10 Cs1 O4 80.98(9) . . ?
O12 Cs1 O7 106.49(14) . . ?
O3 Cs1 O7 41.85(9) 3_576 . ?
O13 Cs1 O7 65.77(13) 3_566 . ?
O9 Cs1 O7 135.62(13) . . ?
O10 Cs1 O7 109.15(9) . . ?
O4 Cs1 O7 160.03(10) . . ?
O12 Cs1 O11 90.93(13) . . ?
O3 Cs1 O11 102.19(12) 3_576 . ?
O13 Cs1 O11 94.99(11) 3_566 . ?
O9 Cs1 O11 69.49(9) . . ?
O10 Cs1 O11 41.77(9) . . ?
O4 Cs1 O11 115.65(10) . . ?
O7 Cs1 O11 81.34(11) . . ?
O12 Cs1 O13 76.51(14) . . ?
O3 Cs1 O13 97.07(12) 3_576 . ?
O13 Cs1 O13 101.72(10) 3_566 . ?
O9 Cs1 O13 84.43(10) . . ?
O10 Cs1 O13 119.86(9) . . ?
O4 Cs1 O13 39.24(10) . . ?
O7 Cs1 O13 126.10(10) . . ?
O11 Cs1 O13 151.93(9) . . ?
O12 Cs1 B7 21.60(11) . . ?
O3 Cs1 B7 90.90(13) 3_576 . ?
O13 Cs1 B7 169.08(12) 3_566 . ?
O9 Cs1 B7 22.56(11) . . ?
O10 Cs1 B7 90.91(12) . . ?
O4 Cs1 B7 73.18(14) . . ?
O7 Cs1 B7 122.42(15) . . ?
O11 Cs1 B7 80.02(13) . . ?
O13 Cs1 B7 79.45(14) . . ?
O12 Cs1 B4 90.87(15) . 3_576 ?
O3 Cs1 B4 21.32(11) 3_576 3_576 ?
O13 Cs1 B4 79.58(15) 3_566 3_576 ?
O9 Cs1 B4 130.19(13) . 3_576 ?
O10 Cs1 B4 130.36(13) . 3_576 ?
O4 Cs1 B4 147.14(12) . 3_576 ?
O7 Cs1 B4 21.98(11) . 3_576 ?
O11 Cs1 B4 96.93(14) . 3_576 ?
O13 Cs1 B4 108.10(14) . 3_576 ?
B7 Cs1 B4 110.54(16) . 3_576 ?
O12 Cs1 B5 129.71(13) . . ?
O3 Cs1 B5 148.87(13) 3_576 . ?
O13 Cs1 B5 60.93(12) 3_566 . ?
O9 Cs1 B5 85.95(11) . . ?
O10 Cs1 B5 21.27(12) . . ?
O4 Cs1 B5 75.50(13) . . ?
O7 Cs1 B5 107.50(12) . . ?
O11 Cs1 B5 59.38(14) . . ?
O13 Cs1 B5 110.11(14) . . ?
B7 Cs1 B5 108.36(14) . . ?
B4 Cs1 B5 129.17(15) 3_576 . ?
O5 Cs2 O1 118.63(13) . . ?
O5 Cs2 O1 158.32(12) . 3_676 ?
O1 Cs2 O1 82.71(13) . 3_676 ?
O5 Cs2 O3 97.85(11) . . ?
O1 Cs2 O3 44.52(9) . . ?
O1 Cs2 O3 100.76(11) 3_676 . ?
O5 Cs2 O11 128.12(10) . . ?
O1 Cs2 O11 99.15(9) . . ?
O1 Cs2 O11 43.90(9) 3_676 . ?
O3 Cs2 O11 84.65(12) . . ?
O5 Cs2 O2 121.15(10) . . ?
O1 Cs2 O2 102.65(12) . . ?
O1 Cs2 O2 43.92(9) 3_676 . ?
O3 Cs2 O2 139.90(9) . . ?
O11 Cs2 O2 78.56(10) . . ?
O5 Cs2 O7 55.42(13) . . ?
O1 Cs2 O7 173.39(10) . . ?
O1 Cs2 O7 103.46(13) 3_676 . ?
O3 Cs2 O7 130.68(10) . . ?
O11 Cs2 O7 84.01(10) . . ?
O2 Cs2 O7 83.62(13) . . ?
O5 Cs2 O6 90.02(12) . . ?
O1 Cs2 O6 43.20(9) . . ?
O1 Cs2 O6 105.20(11) 3_676 . ?
O3 Cs2 O6 75.86(11) . . ?
O11 Cs2 O6 139.46(9) . . ?
O2 Cs2 O6 93.90(11) . . ?
O7 Cs2 O6 135.21(10) . . ?
O5 Cs2 B3 110.84(15) . . ?
O1 Cs2 B3 21.31(11) . . ?
O1 Cs2 B3 90.47(14) 3_676 . ?
O3 Cs2 B3 23.26(11) . . ?
O11 Cs2 B3 91.35(13) . . ?
O2 Cs2 B3 120.72(14) . . ?
O7 Cs2 B3 153.86(13) . . ?
O6 Cs2 B3 58.26(13) . . ?
O5 Cs2 B4 102.55(13) . . ?
O1 Cs2 B4 59.51(12) . . ?
O1 Cs2 B4 91.40(13) 3_676 . ?
O3 Cs2 B4 20.29(11) . . ?
O11 Cs2 B4 66.06(15) . . ?
O2 Cs2 B4 135.18(11) . . ?
O7 Cs2 B4 117.33(13) . . ?
O6 Cs2 B4 95.64(14) . . ?
B3 Cs2 B4 39.12(14) . . ?
O5 Cs2 B6 146.76(13) . 3_676 ?
O1 Cs2 B6 91.16(13) . 3_676 ?
O1 Cs2 B6 21.12(10) 3_676 3_676 ?
O3 Cs2 B6 93.68(14) . 3_676 ?
O11 Cs2 B6 22.79(10) . 3_676 ?
O2 Cs2 B6 59.34(12) . 3_676 ?
O7 Cs2 B6 93.88(13) . 3_676 ?
O6 Cs2 B6 123.08(13) . 3_676 ?
B3 Cs2 B6 91.48(15) . 3_676 ?
B4 Cs2 B6 79.05(16) . 3_676 ?
O5 Cs2 B7 111.69(13) . 4_675 ?
O1 Cs2 B7 94.59(14) . 4_675 ?
O1 Cs2 B7 59.27(13) 3_676 4_675 ?
O3 Cs2 B7 138.47(13) . 4_675 ?
O11 Cs2 B7 98.15(13) . 4_675 ?
O2 Cs2 B7 20.25(11) . 4_675 ?
O7 Cs2 B7 90.67(15) . 4_675 ?
O6 Cs2 B7 75.63(14) . 4_675 ?
B3 Cs2 B7 115.46(16) . 4_675 ?
B4 Cs2 B7 144.46(14) . 4_675 ?
B6 Cs2 B7 77.54(15) 3_676 4_675 ?
B3 O1 B6 126.3(5) . . ?
B3 O1 Cs2 105.9(3) . . ?
B6 O1 Cs2 109.4(3) . . ?
B3 O1 Cs2 107.4(3) . 3_676 ?
B6 O1 Cs2 106.8(3) . 3_676 ?
Cs2 O1 Cs2 97.29(13) . 3_676 ?
B7 O2 B3 124.0(4) 4_675 3_676 ?
B7 O2 Cs2 100.7(4) 4_675 . ?
B3 O2 Cs2 96.6(3) 3_676 . ?
B4 O3 B3 124.7(4) . . ?
B4 O3 Cs1 101.2(3) . 3_576 ?
B3 O3 Cs1 125.4(3) . 3_576 ?
B4 O3 Cs2 103.4(4) . . ?
B3 O3 Cs2 98.5(3) . . ?
Cs1 O3 Cs2 97.49(10) 3_576 . ?
B1 O4 B2 118.0(4) . 4_676 ?
B1 O4 Cs1 99.7(3) . . ?
B2 O4 Cs1 126.2(3) 4_676 . ?
B1 O4 Cs1 82.1(3) . 3_566 ?
B2 O4 Cs1 145.1(3) 4_676 3_566 ?
Cs1 O4 Cs1 71.90(9) . 3_566 ?
B2 O5 Cs2 142.1(3) . . ?
B1 O6 B6 121.3(4) 4_675 . ?
B1 O6 Cs2 122.6(4) 4_675 . ?
B6 O6 Cs2 95.2(3) . . ?
B4 O7 Cs2 150.0(4) 3_576 . ?
B4 O7 Cs1 89.4(3) 3_576 . ?
Cs2 O7 Cs1 94.56(11) . . ?
B5 O8 B3 120.8(5) 3_676 . ?
B4 O9 B7 118.7(4) 2_546 . ?
B4 O9 Cs1 145.2(3) 2_546 . ?
B7 O9 Cs1 95.7(3) . . ?
B5 O10 B6 120.7(4) . 3_676 ?
B5 O10 Cs1 95.6(3) . . ?
B6 O10 Cs1 103.6(3) 3_676 . ?
B2 O11 B6 121.7(4) 3_576 3_676 ?
B2 O11 Cs2 129.5(3) 3_576 . ?
B6 O11 Cs2 98.6(3) 3_676 . ?
B2 O11 Cs1 106.1(3) 3_576 . ?
B6 O11 Cs1 98.2(3) 3_676 . ?
Cs2 O11 Cs1 95.64(9) . . ?
B7 O12 Cs1 104.7(3) . . ?
B1 O13 Cs1 113.2(3) . 3_566 ?
B1 O13 Cs1 91.6(4) . . ?
Cs1 O13 Cs1 78.28(10) 3_566 . ?
B5 O14 Cs1 74.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.166
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1520113'
_audit_update_record             
;
2016-11-30 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B4 H6 K2 O10'
_chemical_formula_weight         287.49

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1742(3)
_cell_length_b                   7.8472(4)
_cell_length_c                   8.9702(4)
_cell_angle_alpha                68.551(2)
_cell_angle_beta                 88.368(2)
_cell_angle_gamma                74.877(2)
_cell_volume                     452.49(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5452
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             288
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7366
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.51
_reflns_number_total             2043
_reflns_number_gt                1917
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0442P)²+0.1967P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2043
_refine_ls_number_parameters     158
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0743
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.087
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.20675(4) 1.09022(5) 0.19990(4) 0.02355(9) Uani 1 1 d . . .
K2 K 0.09244(5) 0.61773(5) 0.19963(4) 0.02563(9) Uani 1 1 d . . .
B1 B 0.5434(2) 0.2327(2) 0.34782(18) 0.0151(3) Uani 1 1 d . . .
B2 B 0.2581(2) 0.6171(2) -0.14919(19) 0.0160(3) Uani 1 1 d . . .
B3 B -0.2905(2) 1.0684(2) 0.17250(19) 0.0161(3) Uani 1 1 d . . .
B4 B -0.1482(2) 1.2625(2) 0.43229(19) 0.0185(3) Uani 1 1 d . . .
O1 O 0.25165(6) 0.44839(13) -0.01373(9) 0.0196(2) Uani 1 1 d D . .
O2 O -0.25739(5) 0.92183(12) 0.11603(13) 0.0227(2) Uani 1 1 d D . .
O8 O 0.58991(14) 1.06616(13) 0.29473(12) 0.0182(2) Uani 1 1 d . . .
O10 O 0.20260(14) 0.78993(14) -0.10377(12) 0.0180(2) Uani 1 1 d . . .
O9 O 0.54812(13) 0.40078(13) 0.21010(11) 0.01508(19) Uani 1 1 d . . .
O6 O 0.30633(14) 0.80329(15) 0.52406(12) 0.0198(2) Uani 1 1 d . . .
O7 O -0.11244(14) 1.35243(15) 0.27766(12) 0.0198(2) Uani 1 1 d . . .
O3 O 0.35511(14) 0.25189(8) 0.41312(10) 0.0203(2) Uani 1 1 d D . .
O5 O 0.45708(10) 0.73315(6) 0.24948(6) 0.0302(3) Uani 1 1 d D . .
O4 O 0.01826(5) 0.76566(17) 0.44406(13) 0.0311(3) Uani 1 1 d D . .
H3 H 0.376(3) 0.1515(7) 0.5068(5) 0.037 Uiso 1 1 d D . .
H2 H -0.3421(4) 0.8501(8) 0.161(2) 0.037 Uiso 1 1 d D . .
H1 H 0.35505(19) 0.37712(15) 0.06845(9) 0.037 Uiso 1 1 d D . .
H52 H 0.5199 0.6446 0.2050 0.037 Uiso 1 1 d RD . .
H51 H 0.4940 0.6936 0.3484 0.037 Uiso 1 1 d RD . .
H4 H -0.0969(3) 0.7400(18) 0.4902(14) 0.053(7) 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
K1 O5 2.7898(6) . ?
K1 O8 2.8391(11) . ?
K1 O1 2.8590(9) 1_565 ?
K1 O2 2.8795(11) 2_575 ?
K1 O10 2.8918(10) 2_575 ?
K1 O7 2.9093(11) . ?
K1 O6 2.9200(10) . ?
K1 O3 2.9993(10) 1_565 ?
K1 O4 3.2651(12) . ?
K1 B1 3.3938(15) 1_565 ?
K1 B2 3.4541(15) 2_575 ?
K1 B4 3.5459(17) 2_576 ?
K2 O7 2.7308(10) 1_545 ?
K2 O10 2.7573(10) . ?
K2 O1 2.7707(10) . ?
K2 O4 2.8126(12) . ?
K2 O2 2.8686(7) . ?
K2 O3 2.9702(7) . ?
K2 O5 3.0761(8) . ?
K2 O9 3.2543(10) . ?
K2 O1 3.2680(8) 2_565 ?
K2 K1 3.8168(5) 2_575 ?
K2 K1 4.0036(5) 1_545 ?
B1 O9 1.4481(17) . ?
B1 O3 1.4503(17) . ?
B1 O6 1.4959(17) 2_666 ?
B1 O8 1.5045(18) 1_545 ?
B1 K1 3.3938(15) 1_545 ?
B2 O1 1.4435(17) . ?
B2 O9 1.4701(18) 2_665 ?
B2 O7 1.4881(18) 2_575 ?
B2 O10 1.5091(18) . ?
B2 K1 3.4541(15) 2_575 ?
B3 O10 1.3623(18) 2_575 ?
B3 O8 1.3709(19) 1_455 ?
B3 O2 1.3829(18) . ?
B3 K1 3.5720(15) 1_455 ?
B4 O6 1.3564(19) 2_576 ?
B4 O7 1.3586(19) . ?
B4 O4 1.3856(18) 2_576 ?
B4 K1 3.5459(17) 2_576 ?
O1 K1 2.8590(9) 1_545 ?
O1 K2 3.2680(8) 2_565 ?
O2 K1 2.8795(11) 2_575 ?
O8 B3 1.3709(19) 1_655 ?
O8 B1 1.5045(18) 1_565 ?
O10 B3 1.3623(18) 2_575 ?
O10 K1 2.8918(10) 2_575 ?
O9 B2 1.4701(18) 2_665 ?
O6 B4 1.3564(19) 2_576 ?
O6 B1 1.4959(17) 2_666 ?
O7 B2 1.4881(18) 2_575 ?
O7 K2 2.7308(10) 1_565 ?
O3 K1 2.9993(10) 1_545 ?
O4 B4 1.3856(18) 2_576 ?

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
O5 K1 O8 68.35(3) . . ?
O5 K1 O1 126.47(2) . 1_565 ?
O8 K1 O1 78.71(2) . 1_565 ?
O5 K1 O2 74.88(2) . 2_575 ?
O8 K1 O2 100.76(2) . 2_575 ?
O1 K1 O2 71.24(3) 1_565 2_575 ?
O5 K1 O10 126.07(3) . 2_575 ?
O8 K1 O10 165.58(3) . 2_575 ?
O1 K1 O10 90.82(2) 1_565 2_575 ?
O2 K1 O10 84.95(2) 2_575 2_575 ?
O5 K1 O7 154.13(3) . . ?
O8 K1 O7 118.26(3) . . ?
O1 K1 O7 78.85(3) 1_565 . ?
O2 K1 O7 124.26(3) 2_575 . ?
O10 K1 O7 49.09(3) 2_575 . ?
O5 K1 O6 59.61(2) . . ?
O8 K1 O6 72.04(3) . . ?
O1 K1 O6 144.33(3) 1_565 . ?
O2 K1 O6 133.56(3) 2_575 . ?
O10 K1 O6 113.55(3) 2_575 . ?
O7 K1 O6 97.26(3) . . ?
O5 K1 O3 108.24(2) . 1_565 ?
O8 K1 O3 48.80(3) . 1_565 ?
O1 K1 O3 75.36(2) 1_565 1_565 ?
O2 K1 O3 138.88(2) 2_575 1_565 ?
O10 K1 O3 119.13(3) 2_575 1_565 ?
O7 K1 O3 70.03(3) . 1_565 ?
O6 K1 O3 70.12(3) . 1_565 ?
O5 K1 O4 71.34(2) . . ?
O8 K1 O4 115.14(2) . . ?
O1 K1 O4 161.78(2) 1_565 . ?
O2 K1 O4 114.98(3) 2_575 . ?
O10 K1 O4 73.30(2) 2_575 . ?
O7 K1 O4 83.91(3) . . ?
O6 K1 O4 43.83(2) . . ?
O3 K1 O4 104.24(3) 1_565 . ?
O5 K1 B1 93.18(3) . 1_565 ?
O8 K1 B1 26.04(3) . 1_565 ?
O1 K1 B1 67.57(3) 1_565 1_565 ?
O2 K1 B1 116.28(3) 2_575 1_565 ?
O10 K1 B1 139.98(3) 2_575 1_565 ?
O7 K1 B1 92.51(3) . 1_565 ?
O6 K1 B1 77.29(3) . 1_565 ?
O3 K1 B1 25.27(3) 1_565 1_565 ?
O4 K1 B1 119.44(3) . 1_565 ?
O5 K1 B2 149.93(3) . 2_575 ?
O8 K1 B2 140.32(3) . 2_575 ?
O1 K1 B2 77.72(3) 1_565 2_575 ?
O2 K1 B2 101.25(3) 2_575 2_575 ?
O10 K1 B2 25.60(3) 2_575 2_575 ?
O7 K1 B2 25.23(3) . 2_575 ?
O6 K1 B2 113.11(3) . 2_575 ?
O3 K1 B2 94.28(3) 1_565 2_575 ?
O4 K1 B2 84.19(3) . 2_575 ?
B1 K1 B2 114.42(4) 1_565 2_575 ?
O5 K1 B4 67.33(3) . 2_576 ?
O8 K1 B4 93.59(3) . 2_576 ?
O1 K1 B4 157.93(3) 1_565 2_576 ?
O2 K1 B4 130.79(3) 2_575 2_576 ?
O10 K1 B4 92.54(3) 2_575 2_576 ?
O7 K1 B4 86.95(3) . 2_576 ?
O6 K1 B4 21.55(3) . 2_576 ?
O3 K1 B4 83.98(3) 1_565 2_576 ?
O4 K1 B4 23.00(3) . 2_576 ?
B1 K1 B4 96.59(4) 1_565 2_576 ?
B2 K1 B4 96.46(4) 2_575 2_576 ?
O7 K2 O10 124.64(3) 1_545 . ?
O7 K2 O1 83.50(3) 1_545 . ?
O10 K2 O1 52.13(3) . . ?
O7 K2 O4 103.02(3) 1_545 . ?
O10 K2 O4 127.76(3) . . ?
O1 K2 O4 167.021(19) . . ?
O7 K2 O2 91.41(3) 1_545 . ?
O10 K2 O2 87.67(3) . . ?
O1 K2 O2 122.02(3) . . ?
O4 K2 O2 69.55(3) . . ?
O7 K2 O3 72.87(3) 1_545 . ?
O10 K2 O3 117.88(3) . . ?
O1 K2 O3 77.14(2) . . ?
O4 K2 O3 93.89(3) . . ?
O2 K2 O3 154.37(3) . . ?
O7 K2 O5 149.81(3) 1_545 . ?
O10 K2 O5 74.19(2) . . ?
O1 K2 O5 94.63(2) . . ?
O4 K2 O5 74.042(18) . . ?
O2 K2 O5 114.43(2) . . ?
O3 K2 O5 77.33(2) . . ?
O7 K2 O9 108.12(3) 1_545 . ?
O10 K2 O9 75.03(3) . . ?
O1 K2 O9 55.20(2) . . ?
O4 K2 O9 111.85(2) . . ?
O2 K2 O9 159.00(3) . . ?
O3 K2 O9 45.00(2) . . ?
O5 K2 O9 49.78(2) . . ?
O7 K2 O1 45.65(3) 1_545 2_565 ?
O10 K2 O1 85.19(3) . 2_565 ?
O1 K2 O1 70.540(17) . 2_565 ?
O4 K2 O1 122.02(2) . 2_565 ?
O2 K2 O1 65.62(3) . 2_565 ?
O3 K2 O1 111.76(3) . 2_565 ?
O5 K2 O1 159.297(19) . 2_565 ?
O9 K2 O1 123.25(2) . 2_565 ?
O7 K2 K1 92.28(2) 1_545 2_575 ?
O10 K2 K1 49.00(2) . 2_575 ?
O1 K2 K1 73.931(15) . 2_575 ?
O4 K2 K1 116.48(2) . 2_575 ?
O2 K2 K1 48.52(2) . 2_575 ?
O3 K2 K1 148.78(2) . 2_575 ?
O5 K2 K1 116.242(13) . 2_575 ?
O9 K2 K1 120.89(2) . 2_575 ?
O1 K2 K1 46.809(16) 2_565 2_575 ?
O7 K2 K1 154.06(3) 1_545 . ?
O10 K2 K1 74.48(2) . . ?
O1 K2 K1 121.63(2) . . ?
O4 K2 K1 53.90(2) . . ?
O2 K2 K1 70.465(18) . . ?
O3 K2 K1 116.20(2) . . ?
O5 K2 K1 44.056(11) . . ?
O9 K2 K1 93.103(19) . . ?
O1 K2 K1 132.007(19) 2_565 . ?
K1 K2 K1 89.244(10) 2_575 . ?
O7 K2 K1 46.61(2) 1_545 1_545 ?
O10 K2 K1 97.60(2) . 1_545 ?
O1 K2 K1 45.565(19) . 1_545 ?
O4 K2 K1 133.00(3) . 1_545 ?
O2 K2 K1 131.41(2) . 1_545 ?
O3 K2 K1 48.190(18) . 1_545 ?
O5 K2 K1 113.443(14) . 1_545 ?
O9 K2 K1 64.095(18) . 1_545 ?
O1 K2 K1 66.777(17) 2_565 1_545 ?
K1 K2 K1 101.720(10) 2_575 1_545 ?
K1 K2 K1 157.191(13) . 1_545 ?
O9 B1 O3 111.55(11) . . ?
O9 B1 O6 110.02(11) . 2_666 ?
O3 B1 O6 109.02(11) . 2_666 ?
O9 B1 O8 107.98(11) . 1_545 ?
O3 B1 O8 109.71(10) . 1_545 ?
O6 B1 O8 108.51(11) 2_666 1_545 ?
O9 B1 K1 99.49(8) . 1_545 ?
O3 B1 K1 61.97(6) . 1_545 ?
O6 B1 K1 150.14(9) 2_666 1_545 ?
O8 B1 K1 55.93(6) 1_545 1_545 ?
O1 B2 O9 111.28(11) . 2_665 ?
O1 B2 O7 108.47(11) . 2_575 ?
O9 B2 O7 110.04(11) 2_665 2_575 ?
O1 B2 O10 110.69(11) . . ?
O9 B2 O10 109.21(11) 2_665 . ?
O7 B2 O10 107.05(11) 2_575 . ?
O1 B2 K1 103.78(7) . 2_575 ?
O9 B2 K1 144.93(9) 2_665 2_575 ?
O7 B2 K1 56.45(6) 2_575 2_575 ?
O10 B2 K1 55.89(6) . 2_575 ?
O10 B3 O8 122.51(13) 2_575 1_455 ?
O10 B3 O2 118.44(13) 2_575 . ?
O8 B3 O2 119.05(12) 1_455 . ?
O10 B3 K1 129.93(9) 2_575 1_455 ?
O8 B3 K1 47.80(7) 1_455 1_455 ?
O2 B3 K1 91.92(7) . 1_455 ?
O6 B4 O7 124.02(13) 2_576 . ?
O6 B4 O4 116.41(13) 2_576 2_576 ?
O7 B4 O4 119.57(13) . 2_576 ?
O6 B4 K1 52.27(7) 2_576 2_576 ?
O7 B4 K1 162.85(11) . 2_576 ?
O4 B4 K1 67.05(8) 2_576 2_576 ?
B2 O1 K2 98.92(8) . . ?
B2 O1 K1 166.90(8) . 1_545 ?
K2 O1 K1 90.65(2) . 1_545 ?
B2 O1 K2 91.55(7) . 2_565 ?
K2 O1 K2 109.460(17) . 2_565 ?
K1 O1 K2 76.74(2) 1_545 2_565 ?
B3 O2 K2 122.90(7) . . ?
B3 O2 K1 132.70(8) . 2_575 ?
K2 O2 K1 83.21(2) . 2_575 ?
B3 O8 B1 118.80(11) 1_655 1_565 ?
B3 O8 K1 111.24(8) 1_655 . ?
B1 O8 K1 98.03(7) 1_565 . ?
B3 O10 B2 118.70(11) 2_575 . ?
B3 O10 K2 135.00(9) 2_575 . ?
B2 O10 K2 97.74(7) . . ?
B3 O10 K1 112.34(8) 2_575 2_575 ?
B2 O10 K1 98.51(7) . 2_575 ?
K2 O10 K1 84.98(3) . 2_575 ?
B1 O9 B2 111.05(10) . 2_665 ?
B1 O9 K2 95.37(7) . . ?
B2 O9 K2 153.53(8) 2_665 . ?
B4 O6 B1 118.62(11) 2_576 2_666 ?
B4 O6 K1 106.18(8) 2_576 . ?
B1 O6 K1 132.09(8) 2_666 . ?
B4 O7 B2 117.61(11) . 2_575 ?
B4 O7 K2 121.28(9) . 1_565 ?
B2 O7 K2 114.32(8) 2_575 1_565 ?
B4 O7 K1 107.00(9) . . ?
B2 O7 K1 98.32(8) 2_575 . ?
K2 O7 K1 90.39(3) 1_565 . ?
B1 O3 K2 107.88(7) . . ?
B1 O3 K1 92.76(7) . 1_545 ?
K2 O3 K1 84.24(2) . 1_545 ?
K1 O5 K2 85.88(2) . . ?
B4 O4 K2 126.66(8) 2_576 . ?
B4 O4 K1 89.95(8) 2_576 . ?
K2 O4 K1 81.99(3) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1520112'
_audit_update_record             
;
2016-11-30 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            ' B4 H11.25 K2 O12.63'
_chemical_formula_weight         334.78

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   11.150(3)
_cell_length_b                   13.064(3)
_cell_length_c                   16.411(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2390.4(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3559
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      26.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1362
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_process_details   face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13713
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         27.84
_reflns_number_total             2795
_reflns_number_gt                2129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0932P)²+2.7644P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2795
_refine_ls_number_parameters     185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1670
_refine_ls_wR_factor_gt          0.1539
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.44496(7) 0.52521(6) 0.63056(5) 0.0432(2) Uani 1 1 d . . .
K2 K 0.0000 0.58478(10) 0.2500 0.0621(4) Uani 1 2 d S . .
K3 K 0.57312(15) 0.25215(13) 0.75597(9) 0.0479(4) Uani 0.50 1 d P . .
B1 B 0.2561(2) 0.7228(2) 0.57132(18) 0.0208(6) Uani 1 1 d . . .
B2 B 0.1391(2) 0.5645(2) 0.56147(19) 0.0222(6) Uani 1 1 d . . .
B3 B 0.6267(2) 0.3144(2) 0.55175(18) 0.0214(6) Uani 1 1 d . . .
B4 B 0.1553(2) 0.6846(2) 0.44491(18) 0.0201(6) Uani 1 1 d . . .
O1 O 0.17005(15) 0.75948(13) 0.51096(11) 0.0204(4) Uani 1 1 d . . .
O2 O 0.07106(15) 0.71739(14) 0.38353(11) 0.0232(4) Uani 1 1 d . . .
H2 H 0.0446 0.7765 0.3955 0.028 Uiso 1 1 d R . .
O4 O 0.11211(16) 0.58589(13) 0.48190(11) 0.0239(4) Uani 1 1 d . . .
O5 O 0.52112(16) 0.31820(16) 0.59419(12) 0.0292(4) Uani 1 1 d . . .
H5 H 0.4627 0.3110 0.5614 0.035 Uiso 1 1 d R . .
O6 O 0.72841(15) 0.33293(14) 0.59490(11) 0.0237(4) Uani 1 1 d . . .
O7 O 0.37261(15) 0.70586(14) 0.53008(11) 0.0229(4) Uani 1 1 d . . .
O8 O 0.27113(17) 0.79225(15) 0.63922(11) 0.0283(4) Uani 1 1 d . . .
H8 H 0.3044 0.8512 0.6278 0.034 Uiso 1 1 d R . .
O9 O 0.21324(16) 0.62381(14) 0.60659(11) 0.0250(4) Uani 1 1 d . . .
O10 O 0.09168(18) 0.52220(15) 0.09740(13) 0.0309(5) Uani 1 1 d . . .
H10 H 0.0247 0.5489 0.0722 0.037 Uiso 1 1 d R . .
O11 O 0.6487(2) 0.54066(17) 0.53249(17) 0.0483(6) Uani 1 1 d . . .
H11A H 0.7081 0.5812 0.5358 0.058 Uiso 1 1 d R . .
H11B H 0.5904 0.5738 0.5121 0.058 Uiso 1 1 d R . .
O12 O 0.3539(4) 0.6592(2) 0.7641(2) 0.0879(12) Uani 1 1 d . . .
H12A H 0.2985 0.6764 0.7312 0.106 Uiso 1 1 d R . .
H12B H 0.3318 0.6047 0.7880 0.106 Uiso 1 1 d R . .
O13 O 0.3714(4) 0.3900(4) 0.7508(3) 0.0448(11) Uani 0.50 1 d P . .
H13A H 0.2352 0.4611 0.7780 0.054 Uiso 0.50 1 d PR . .
H13B H 0.3117 0.3965 0.8031 0.054 Uiso 1 1 d R . .
H14A H 0.3285 0.3441 0.7123 0.054 Uiso 0.50 1 d PR . .
O14 O 0.3124(8) 0.4551(5) 0.7693(3) 0.080(2) Uani 0.50 1 d P . .
O15 O -0.1380(9) 0.4406(8) 0.1823(7) 0.069(3) Uiso 0.30 1 d P . .
H15A H -0.1027 0.3999 0.1651 0.083 Uiso 0.30 1 d PR . .
H15B H -0.1501 0.4372 0.2249 0.083 Uiso 0.30 1 d PR . .
O16 O 0.6073(10) 0.1138(8) 0.7305(7) 0.070(3) Uiso 0.30 1 d PD . .
H16A H 0.6631 0.1356 0.7153 0.084 Uiso 0.30 1 d PR . .
H16B H 0.6487 0.0645 0.7109 0.084 Uiso 0.30 1 d PRD . .


_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 O13 2.772(5) . ?
K1 O11 2.791(3) . ?
K1 O14 2.866(6) . ?
K1 O5 2.897(2) . ?
K1 O9 2.914(2) . ?
K1 O12 2.982(4) . ?
K1 O7 2.990(2) . ?
K1 O11 2.998(3) 5_666 ?
K1 O14 3.295(9) 3_656 ?
K1 O12 3.329(4) 3_656 ?
K1 O13 3.332(5) 3_656 ?
K1 B1 3.471(3) . ?
K2 O15 2.674(11) . ?
K2 O15 2.674(11) 3 ?
K2 O10 2.826(2) . ?
K2 O10 2.826(2) 3 ?
K2 O16 2.875(11) 2_554 ?
K2 O16 2.875(11) 4_456 ?
K2 O2 2.904(2) . ?
K2 O2 2.904(2) 3 ?
K2 K3 4.477(2) 2_554 ?
K2 K3 4.477(2) 4_456 ?
K3 K3 1.642(3) 3_656 ?
K3 O16 1.893(11) . ?
K3 O13 1.908(6) 3_656 ?
K3 O16 2.713(11) 3_656 ?
K3 O5 2.810(3) 3_656 ?
K3 O8 2.847(3) 6_657 ?
K3 O5 2.851(3) . ?
K3 O13 2.883(6) . ?
K3 O15 2.885(11) 2 ?
K3 O14 2.971(7) 3_656 ?
K3 O9 3.215(2) 6_657 ?
K3 O6 3.331(3) . ?
B1 O8 1.447(3) . ?
B1 O1 1.460(3) . ?
B1 O7 1.482(3) . ?
B1 O9 1.495(3) . ?
B1 K3 3.513(3) 6_567 ?
B2 O9 1.354(3) . ?
B2 O4 1.369(4) . ?
B2 O10 1.382(3) 7_566 ?
B3 O6 1.359(3) . ?
B3 O5 1.368(3) . ?
B3 O7 1.369(3) 5_666 ?
B4 O2 1.442(3) . ?
B4 O1 1.469(3) . ?
B4 O6 1.470(3) 5_666 ?
B4 O4 1.504(3) . ?
O5 K3 2.810(3) 3_656 ?
O6 B4 1.470(3) 5_666 ?
O7 B3 1.369(3) 5_666 ?
O8 K3 2.847(3) 6_567 ?
O9 K3 3.215(2) 6_567 ?
O10 B2 1.382(3) 7_565 ?
O11 K1 2.998(3) 5_666 ?
O12 K1 3.329(3) 3_656 ?
O12 K3 3.374(4) 6_567 ?
O13 O14 1.117(8) . ?
O13 K3 1.908(6) 3_656 ?
O13 K1 3.332(5) 3_656 ?
O14 K3 2.971(7) 3_656 ?
O14 K1 3.295(9) 3_656 ?
O15 O16 1.117(14) 2_554 ?
O15 K3 2.885(11) 2_554 ?
O16 O15 1.117(14) 2 ?
O16 K3 2.713(11) 3_656 ?
O16 K2 2.875(11) 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
O13 K1 O11 134.21(12) . . ?
O13 K1 O14 22.77(15) . . ?
O11 K1 O14 154.31(18) . . ?
O13 K1 O5 68.81(12) . . ?
O11 K1 O5 73.15(6) . . ?
O14 K1 O5 90.94(13) . . ?
O13 K1 O9 96.62(12) . . ?
O11 K1 O9 127.72(7) . . ?
O14 K1 O9 77.96(17) . . ?
O5 K1 O9 130.16(6) . . ?
O13 K1 O12 75.54(13) . . ?
O11 K1 O12 131.16(10) . . ?
O14 K1 O12 55.13(14) . . ?
O5 K1 O12 143.04(8) . . ?
O9 K1 O12 62.47(8) . . ?
O13 K1 O7 144.64(12) . . ?
O11 K1 O7 81.05(6) . . ?
O14 K1 O7 123.48(16) . . ?
O5 K1 O7 134.62(6) . . ?
O9 K1 O7 48.50(5) . . ?
O12 K1 O7 81.37(7) . . ?
O13 K1 O11 110.44(11) . 5_666 ?
O11 K1 O11 77.85(8) . 5_666 ?
O14 K1 O11 115.97(17) . 5_666 ?
O5 K1 O11 69.53(6) . 5_666 ?
O9 K1 O11 72.40(6) . 5_666 ?
O12 K1 O11 134.87(9) . 5_666 ?
O7 K1 O11 68.93(6) . 5_666 ?
O13 K1 O14 73.20(17) . 3_656 ?
O11 K1 O14 68.87(13) . 3_656 ?
O14 K1 O14 86.5(3) . 3_656 ?
O5 K1 O14 66.57(11) . 3_656 ?
O9 K1 O14 156.68(11) . 3_656 ?
O12 K1 O14 94.39(12) . 3_656 ?
O7 K1 O14 135.73(13) . 3_656 ?
O11 K1 O14 130.61(11) 5_666 3_656 ?
O13 K1 O12 99.47(12) . 3_656 ?
O11 K1 O12 73.34(9) . 3_656 ?
O14 K1 O12 95.89(17) . 3_656 ?
O5 K1 O12 113.60(7) . 3_656 ?
O9 K1 O12 115.78(8) . 3_656 ?
O12 K1 O12 62.55(14) . 3_656 ?
O7 K1 O12 93.05(7) . 3_656 ?
O11 K1 O12 148.10(8) 5_666 3_656 ?
O14 K1 O12 48.26(12) 3_656 3_656 ?
O13 K1 O13 55.13(18) . 3_656 ?
O11 K1 O13 82.83(10) . 3_656 ?
O14 K1 O13 71.5(2) . 3_656 ?
O5 K1 O13 56.32(9) . 3_656 ?
O9 K1 O13 149.11(10) . 3_656 ?
O12 K1 O13 95.22(11) . 3_656 ?
O7 K1 O13 155.01(10) . 3_656 ?
O11 K1 O13 125.69(10) 5_666 3_656 ?
O14 K1 O13 19.39(13) 3_656 3_656 ?
O12 K1 O13 63.97(11) 3_656 3_656 ?
O13 K1 B1 119.58(12) . . ?
O11 K1 B1 106.18(7) . . ?
O14 K1 B1 98.48(16) . . ?
O5 K1 B1 144.55(7) . . ?
O9 K1 B1 25.20(6) . . ?
O12 K1 B1 64.06(8) . . ?
O7 K1 B1 25.13(6) . . ?
O11 K1 B1 75.65(7) 5_666 . ?
O14 K1 B1 147.65(12) 3_656 . ?
O12 K1 B1 99.40(8) 3_656 . ?
O13 K1 B1 158.56(10) 3_656 . ?
O15 K2 O15 90.4(5) . 3 ?
O15 K2 O10 68.7(2) . . ?
O15 K2 O10 87.5(2) 3 . ?
O15 K2 O10 87.5(2) . 3 ?
O15 K2 O10 68.7(2) 3 3 ?
O10 K2 O10 146.37(10) . 3 ?
O15 K2 O16 22.8(3) . 2_554 ?
O15 K2 O16 69.5(3) 3 2_554 ?
O10 K2 O16 77.9(2) . 2_554 ?
O10 K2 O16 71.8(2) 3 2_554 ?
O15 K2 O16 69.5(3) . 4_456 ?
O15 K2 O16 22.8(3) 3 4_456 ?
O10 K2 O16 71.8(2) . 4_456 ?
O10 K2 O16 77.9(2) 3 4_456 ?
O16 K2 O16 51.0(4) 2_554 4_456 ?
O15 K2 O2 153.0(2) . . ?
O15 K2 O2 87.1(2) 3 . ?
O10 K2 O2 137.97(6) . . ?
O10 K2 O2 66.58(5) 3 . ?
O16 K2 O2 137.4(2) 2_554 . ?
O16 K2 O2 109.9(2) 4_456 . ?
O15 K2 O2 87.1(2) . 3 ?
O15 K2 O2 153.0(2) 3 3 ?
O10 K2 O2 66.58(5) . 3 ?
O10 K2 O2 137.97(6) 3 3 ?
O16 K2 O2 109.9(2) 2_554 3 ?
O16 K2 O2 137.4(2) 4_456 3 ?
O2 K2 O2 106.74(8) . 3 ?
O15 K2 K3 38.0(2) . 2_554 ?
O15 K2 K3 53.4(2) 3 2_554 ?
O10 K2 K3 78.51(5) . 2_554 ?
O10 K2 K3 68.30(5) 3 2_554 ?
O16 K2 K3 16.2(2) 2_554 2_554 ?
O16 K2 K3 35.5(2) 4_456 2_554 ?
O2 K2 K3 128.29(5) . 2_554 ?
O2 K2 K3 123.60(5) 3 2_554 ?
O15 K2 K3 53.4(2) . 4_456 ?
O15 K2 K3 38.0(2) 3 4_456 ?
O10 K2 K3 68.30(5) . 4_456 ?
O10 K2 K3 78.51(5) 3 4_456 ?
O16 K2 K3 35.5(2) 2_554 4_456 ?
O16 K2 K3 16.2(2) 4_456 4_456 ?
O2 K2 K3 123.60(5) . 4_456 ?
O2 K2 K3 128.29(5) 3 4_456 ?
K3 K2 K3 21.14(4) 2_554 4_456 ?
K3 K3 O16 100.0(3) 3_656 . ?
K3 K3 O13 108.37(15) 3_656 3_656 ?
O16 K3 O13 145.4(4) . 3_656 ?
K3 K3 O16 43.4(2) 3_656 3_656 ?
O16 K3 O16 62.1(5) . 3_656 ?
O13 K3 O16 150.9(3) 3_656 3_656 ?
K3 K3 O5 74.52(11) 3_656 3_656 ?
O16 K3 O5 124.2(3) . 3_656 ?
O13 K3 O5 83.23(16) 3_656 3_656 ?
O16 K3 O5 81.7(2) 3_656 3_656 ?
K3 K3 O8 147.34(13) 3_656 6_657 ?
O16 K3 O8 98.8(3) . 6_657 ?
O13 K3 O8 67.03(16) 3_656 6_657 ?
O16 K3 O8 130.4(2) 3_656 6_657 ?
O5 K3 O8 72.83(7) 3_656 6_657 ?
K3 K3 O5 71.76(10) 3_656 . ?
O16 K3 O5 97.1(3) . . ?
O13 K3 O5 74.11(16) 3_656 . ?
O16 K3 O5 97.3(2) 3_656 . ?
O5 K3 O5 130.23(9) 3_656 . ?
O8 K3 O5 131.64(8) 6_657 . ?
K3 K3 O13 38.90(10) 3_656 . ?
O16 K3 O13 138.3(3) . . ?
O13 K3 O13 70.2(2) 3_656 . ?
O16 K3 O13 80.8(3) 3_656 . ?
O5 K3 O13 62.76(11) 3_656 . ?
O8 K3 O13 120.52(12) 6_657 . ?
O5 K3 O13 67.96(11) . . ?
K3 K3 O15 101.5(2) 3_656 2 ?
O16 K3 O15 12.6(4) . 2 ?
O13 K3 O15 135.9(3) 3_656 2 ?
O16 K3 O15 68.8(3) 3_656 2 ?
O5 K3 O15 136.8(2) 3_656 2 ?
O8 K3 O15 102.7(2) 6_657 2 ?
O5 K3 O15 85.7(2) . 2 ?
O13 K3 O15 136.8(2) . 2 ?
K3 K3 O14 114.19(18) 3_656 3_656 ?
O16 K3 O14 137.2(4) . 3_656 ?
O13 K3 O14 8.2(2) 3_656 3_656 ?
O16 K3 O14 157.5(3) 3_656 3_656 ?
O5 K3 O14 90.52(13) 3_656 3_656 ?
O8 K3 O14 65.62(16) 6_657 3_656 ?
O5 K3 O14 71.77(14) . 3_656 ?
O13 K3 O14 76.9(2) . 3_656 ?
O15 K3 O14 127.8(3) 2 3_656 ?
K3 K3 O9 124.48(11) 3_656 6_657 ?
O16 K3 O9 63.9(3) . 6_657 ?
O13 K3 O9 112.05(16) 3_656 6_657 ?
O16 K3 O9 87.4(2) 3_656 6_657 ?
O5 K3 O9 74.21(6) 3_656 6_657 ?
O8 K3 O9 45.21(6) 6_657 6_657 ?
O5 K3 O9 155.48(8) . 6_657 ?
O13 K3 O9 136.52(11) . 6_657 ?
O15 K3 O9 73.6(2) 2 6_657 ?
O14 K3 O9 110.76(17) 3_656 6_657 ?
K3 K3 O6 114.92(11) 3_656 . ?
O16 K3 O6 91.3(3) . . ?
O13 K3 O6 59.09(15) 3_656 . ?
O16 K3 O6 131.4(2) 3_656 . ?
O5 K3 O6 142.32(8) 3_656 . ?
O8 K3 O6 91.03(7) 6_657 . ?
O5 K3 O6 43.20(5) . . ?
O13 K3 O6 100.61(11) . . ?
O15 K3 O6 79.3(2) 2 . ?
O14 K3 O6 51.92(12) 3_656 . ?
O9 K3 O6 117.98(7) 6_657 . ?
O8 B1 O1 113.2(2) . . ?
O8 B1 O7 110.1(2) . . ?
O1 B1 O7 108.4(2) . . ?
O8 B1 O9 106.3(2) . . ?
O1 B1 O9 109.7(2) . . ?
O7 B1 O9 109.1(2) . . ?
O8 B1 K1 100.38(15) . . ?
O1 B1 K1 146.40(16) . . ?
O7 B1 K1 58.97(12) . . ?
O9 B1 K1 56.08(12) . . ?
O8 B1 K3 51.51(12) . 6_567 ?
O1 B1 K3 97.49(14) . 6_567 ?
O7 B1 K3 153.38(17) . 6_567 ?
O9 B1 K3 66.21(12) . 6_567 ?
K1 B1 K3 101.98(8) . 6_567 ?
O9 B2 O4 122.6(2) . . ?
O9 B2 O10 118.0(2) . 7_566 ?
O4 B2 O10 119.4(2) . 7_566 ?
O6 B3 O5 116.5(2) . . ?
O6 B3 O7 122.7(2) . 5_666 ?
O5 B3 O7 120.8(2) . 5_666 ?
O2 B4 O1 113.0(2) . . ?
O2 B4 O6 108.1(2) . 5_666 ?
O1 B4 O6 109.43(19) . 5_666 ?
O2 B4 O4 109.2(2) . . ?
O1 B4 O4 108.0(2) . . ?
O6 B4 O4 109.2(2) 5_666 . ?
B1 O1 B4 110.84(19) . . ?
B4 O2 K2 121.83(15) . . ?
B2 O4 B4 119.3(2) . . ?
B3 O5 K3 139.10(17) . 3_656 ?
B3 O5 K3 106.74(16) . . ?
K3 O5 K3 33.72(7) 3_656 . ?
B3 O5 K1 113.01(16) . . ?
K3 O5 K1 89.81(7) 3_656 . ?
K3 O5 K1 98.64(7) . . ?
B3 O6 B4 118.5(2) . 5_666 ?
B3 O6 K3 85.59(15) . . ?
B4 O6 K3 139.62(15) 5_666 . ?
B3 O7 B1 118.8(2) 5_666 . ?
B3 O7 K1 112.76(15) 5_666 . ?
B1 O7 K1 95.89(14) . . ?
B1 O8 K3 105.06(15) . 6_567 ?
B2 O9 B1 118.6(2) . . ?
B2 O9 K1 111.25(16) . . ?
B1 O9 K1 98.72(14) . . ?
B2 O9 K3 112.66(16) . 6_567 ?
B1 O9 K3 88.61(14) . 6_567 ?
K1 O9 K3 124.52(7) . 6_567 ?
B2 O10 K2 138.91(18) 7_565 . ?
K1 O11 K1 102.15(8) . 5_666 ?
K1 O12 K1 81.01(9) . 3_656 ?
K1 O12 K3 117.10(10) . 6_567 ?
K1 O12 K3 149.86(13) 3_656 6_567 ?
O14 O13 K3 157.7(5) . 3_656 ?
O14 O13 K1 83.3(4) . . ?
K3 O13 K1 117.7(2) 3_656 . ?
O14 O13 K3 157.9(5) . . ?
K3 O13 K3 32.73(11) 3_656 . ?
K1 O13 K3 100.84(16) . . ?
O14 O13 K1 78.4(5) . 3_656 ?
K3 O13 K1 109.6(2) 3_656 3_656 ?
K1 O13 K1 84.05(13) . 3_656 ?
K3 O13 K1 80.47(12) . 3_656 ?
O13 O14 K1 73.9(4) . . ?
O13 O14 K3 14.1(3) . 3_656 ?
K1 O14 K3 87.3(2) . 3_656 ?
O13 O14 K1 82.2(5) . 3_656 ?
K1 O14 K1 83.3(2) . 3_656 ?
K3 O14 K1 88.0(2) 3_656 3_656 ?
O16 O15 K2 88.8(9) 2_554 . ?
O16 O15 K3 21.7(7) 2_554 2_554 ?
K2 O15 K3 107.3(4) . 2_554 ?
O15 O16 K3 145.7(11) 2 . ?
O15 O16 K3 135.2(10) 2 3_656 ?
K3 O16 K3 36.6(2) . 3_656 ?
O15 O16 K2 68.4(8) 2 2 ?
K3 O16 K2 138.8(5) . 2 ?
K3 O16 K2 106.5(4) 3_656 2 ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.84
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.087
