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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1952328'
_audit_update_record             
;
2019-09-16 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_audit_creation_date             2019-09-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(B8 Ba2 F12 H8 O12)'
_chemical_formula_sum            'B4 H4 Ba F6 O6'
_chemical_formula_weight         394.61
_chemical_melting_point          ?
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   6.803(2)
_cell_length_b                   7.008(2)
_cell_length_c                   9.588(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.960(4)
_cell_angle_gamma                90
_cell_volume                     456.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1380
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      4.18
_shelx_estimated_absorpt_T_max   0.642
_shelx_estimated_absorpt_T_min   0.504
_exptl_absorpt_coefficient_mu    4.461
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0659 before and 0.0286 after correction.
The Ratio of minimum to maximum transmission is 0.8761.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.109
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1398
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         4.178
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                565
_reflns_number_total             565
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0144
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0334
_refine_ls_wR_factor_ref         0.0334
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ba1 Ba 0.5000 1.0000 1.0000 0.00826(9) Uani 1 4 d S T P . .
B1 B 0.7584(5) 0.5000 0.6154(3) 0.0154(7) Uani 1 2 d S T P . .
B2 B 0.5430(4) 0.5000 0.8158(3) 0.0106(6) Uani 1 2 d S T P . .
O1 O 0.7721(3) 0.5000 0.4742(2) 0.0256(6) Uani 1 2 d S T P . .
H1 H 0.657(6) 0.5000 0.432(4) 0.031 Uiso 1 2 d RS T P . .
O2 O 0.9262(3) 0.5000 0.7016(2) 0.0184(5) Uani 1 2 d S T P . .
H2 H 1.032(6) 0.5000 0.658(4) 0.022 Uiso 1 2 d RS T P . .
O3 O 0.5773(3) 0.5000 0.6710(2) 0.0136(4) Uani 1 2 d S T P . .
F1 F 0.63102(17) 0.66149(16) 0.88545(12) 0.0139(2) Uani 1 1 d . . . . .
F2 F 0.3421(2) 0.5000 0.83473(16) 0.0141(3) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ba1 0.00586(12) 0.01054(13) 0.00838(12) 0.000 0.00030(8) 0.000
B1 0.0111(15) 0.0239(17) 0.0113(14) 0.000 0.0025(12) 0.000
B2 0.0065(14) 0.0156(15) 0.0098(13) 0.000 0.0012(11) 0.000
O1 0.0078(10) 0.0591(17) 0.0098(10) 0.000 -0.0007(8) 0.000
O2 0.0083(10) 0.0388(13) 0.0082(9) 0.000 0.0011(8) 0.000
O3 0.0076(9) 0.0247(11) 0.0084(9) 0.000 0.0003(7) 0.000
F1 0.0132(6) 0.0143(6) 0.0140(5) -0.0024(5) 0.0007(5) -0.0009(5)
F2 0.0076(8) 0.0228(9) 0.0121(8) 0.000 0.0036(6) 0.000

_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
Ba1 O2 2.879(2) 7_667 ?
Ba1 O2 2.879(2) 3_455 ?
Ba1 F1 2.7802(13) . ?
Ba1 F1 2.9160(14) 4_657 ?
Ba1 F1 2.7802(13) 5_677 ?
Ba1 F1 2.9160(14) 7_667 ?
Ba1 F1 2.7802(13) 6_575 ?
Ba1 F1 2.9160(14) 3_455 ?
Ba1 F1 2.9160(14) 8_465 ?
Ba1 F1 2.7802(13) 2_657 ?
Ba1 F2 2.8822(19) 7_567 ?
Ba1 F2 2.8822(19) 3 ?
B1 O1 1.362(4) . ?
B1 O2 1.375(4) . ?
B1 O3 1.367(4) . ?
B2 O3 1.421(4) . ?
B2 F1 1.429(2) . ?
B2 F1 1.429(2) 6_565 ?
B2 F2 1.388(3) . ?
O2 Ba1 2.879(2) 3_545 ?
F1 Ba1 2.9160(14) 3_545 ?
F2 Ba1 2.8822(19) 3_445 ?

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 Ba1 O2 180.0 3_455 7_667 ?
O2 Ba1 F1 118.48(5) 3_455 7_667 ?
O2 Ba1 F1 61.52(5) 3_455 3_455 ?
O2 Ba1 F1 118.48(5) 3_455 4_657 ?
O2 Ba1 F1 61.52(5) 7_667 7_667 ?
O2 Ba1 F1 61.52(5) 7_667 4_657 ?
O2 Ba1 F1 118.48(5) 7_667 3_455 ?
O2 Ba1 F1 118.48(5) 7_667 8_465 ?
O2 Ba1 F1 61.52(5) 3_455 8_465 ?
O2 Ba1 F2 116.24(6) 3_455 7_567 ?
O2 Ba1 F2 63.76(6) 7_667 7_567 ?
O2 Ba1 F2 63.76(6) 3_455 3 ?
O2 Ba1 F2 116.24(6) 7_667 3 ?
F1 Ba1 O2 110.46(3) . 7_667 ?
F1 Ba1 O2 69.54(3) . 3_455 ?
F1 Ba1 O2 69.54(3) 6_575 3_455 ?
F1 Ba1 O2 110.46(3) 2_657 3_455 ?
F1 Ba1 O2 69.54(3) 2_657 7_667 ?
F1 Ba1 O2 69.54(3) 5_677 7_667 ?
F1 Ba1 O2 110.46(3) 6_575 7_667 ?
F1 Ba1 O2 110.46(3) 5_677 3_455 ?
F1 Ba1 F1 61.99(4) 6_575 4_657 ?
F1 Ba1 F1 101.11(3) . 4_657 ?
F1 Ba1 F1 134.33(5) 4_657 3_455 ?
F1 Ba1 F1 78.89(3) 5_677 4_657 ?
F1 Ba1 F1 180.0 4_657 8_465 ?
F1 Ba1 F1 117.14(5) 5_677 2_657 ?
F1 Ba1 F1 78.89(3) . 8_465 ?
F1 Ba1 F1 101.11(3) 2_657 3_455 ?
F1 Ba1 F1 78.89(3) 2_657 7_667 ?
F1 Ba1 F1 78.89(3) 6_575 3_455 ?
F1 Ba1 F1 117.14(5) 6_575 . ?
F1 Ba1 F1 45.67(5) 8_465 3_455 ?
F1 Ba1 F1 62.86(5) 2_657 . ?
F1 Ba1 F1 45.67(5) 4_657 7_667 ?
F1 Ba1 F1 134.33(5) 8_465 7_667 ?
F1 Ba1 F1 61.99(4) 5_677 3_455 ?
F1 Ba1 F1 61.99(4) 2_657 8_465 ?
F1 Ba1 F1 101.11(3) 6_575 7_667 ?
F1 Ba1 F1 62.86(5) 5_677 6_575 ?
F1 Ba1 F1 180.0 6_575 2_657 ?
F1 Ba1 F1 61.99(4) . 7_667 ?
F1 Ba1 F1 180.0 7_667 3_455 ?
F1 Ba1 F1 118.01(4) 5_677 7_667 ?
F1 Ba1 F1 118.01(4) 6_575 8_465 ?
F1 Ba1 F1 118.01(4) . 3_455 ?
F1 Ba1 F1 101.11(3) 5_677 8_465 ?
F1 Ba1 F1 118.01(4) 2_657 4_657 ?
F1 Ba1 F1 180.0 5_677 . ?
F1 Ba1 F2 59.89(3) 5_677 7_567 ?
F1 Ba1 F2 120.11(3) 5_677 3 ?
F1 Ba1 F2 120.11(3) 6_575 7_567 ?
F1 Ba1 F2 59.89(3) . 3 ?
F1 Ba1 F2 59.89(3) 2_657 7_567 ?
F1 Ba1 F2 59.89(3) 6_575 3 ?
F1 Ba1 F2 120.11(3) 2_657 3 ?
F1 Ba1 F2 120.11(3) . 7_567 ?
F2 Ba1 F1 60.22(4) 3 7_667 ?
F2 Ba1 F1 60.22(4) 7_567 8_465 ?
F2 Ba1 F1 119.78(4) 7_567 7_667 ?
F2 Ba1 F1 119.78(4) 7_567 4_657 ?
F2 Ba1 F1 60.22(4) 3 4_657 ?
F2 Ba1 F1 60.22(4) 7_567 3_455 ?
F2 Ba1 F1 119.78(4) 3 3_455 ?
F2 Ba1 F1 119.78(4) 3 8_465 ?
F2 Ba1 F2 180.0 7_567 3 ?
O1 B1 O2 120.0(3) . . ?
O1 B1 O3 119.8(3) . . ?
O3 B1 O2 120.2(3) . . ?
O3 B2 F1 111.74(16) . . ?
O3 B2 F1 111.74(16) . 6_565 ?
F1 B2 F1 104.7(2) . 6_565 ?
F2 B2 O3 109.9(2) . . ?
F2 B2 F1 109.31(17) . . ?
F2 B2 F1 109.31(17) . 6_565 ?
B1 O2 Ba1 133.99(19) . 3_545 ?
B1 O3 B2 125.3(2) . . ?
Ba1 F1 Ba1 118.01(4) . 3_545 ?
B2 F1 Ba1 136.45(13) . . ?
B2 F1 Ba1 101.56(11) . 3_545 ?
B2 F2 Ba1 154.18(15) . 3_445 ?

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
O1 H1 O3 0.86(4) 1.83(4) 2.692(3) 176(4) 5_666
O1 H1 F2 0.86(4) 2.56(4) 3.023(3) 115(3) 5_666
O2 H2 O1 0.85(4) 1.89(4) 2.722(3) 168(3) 5_766

_shelx_res_file                  
;
    1.res created by SHELXL-2014/7

TITL 1_a.res in C2/m
REM Old TITL 1 in C2
REM SHELXT solution in C2/m: R1 0.033, Rweak 0.175, Alpha 0.057
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: B4 O4 F8 Ba
CELL 0.71073 6.8027 7.0079 9.5884 90 92.96 90
ZERR 2 0.0023 0.0023 0.0032 0 0.004 0
LATT 7
SYMM -X,+Y,-Z
SFAC B Ba F H O
UNIT 8 2 12 8 12
EQIV $1 1-X,1-Y,1-Z
EQIV $2 2-X,1-Y,1-Z

L.S. 4 0 0
PLAN  20
SIZE 0.178 0.123 0.109
TEMP -120.15
HTAB O1 O3_$1
HTAB O1 F2_$1
HTAB O2 O1_$2
list 6
HTAB
fmap 2 53
acta
OMIT -1 1 4
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.023200
FVAR       0.49251
BA1   2    0.500000    1.000000    1.000000    10.25000    0.00586    0.01054 =
         0.00838    0.00000    0.00030    0.00000
B1    1    0.758412    0.500000    0.615395    10.50000    0.01111    0.02390 =
         0.01126    0.00000    0.00250    0.00000
B2    1    0.542985    0.500000    0.815849    10.50000    0.00652    0.01562 =
         0.00979    0.00000    0.00118    0.00000
O1    5    0.772132    0.500000    0.474222    10.50000    0.00784    0.05910 =
         0.00984    0.00000   -0.00065    0.00000
H1    4    0.657427    0.500000    0.431866    10.50000   -1.20000
O2    5    0.926220    0.500000    0.701631    10.50000    0.00830    0.03883 =
         0.00820    0.00000    0.00110    0.00000
H2    4    1.031505    0.500000    0.657605    10.50000   -1.20000
O3    5    0.577314    0.500000    0.670957    10.50000    0.00761    0.02466 =
         0.00840    0.00000    0.00034    0.00000
F1    3    0.631018    0.661487    0.885447    11.00000    0.01321    0.01434 =
         0.01400   -0.00239    0.00072   -0.00086
F2    3    0.342071    0.500000    0.834732    10.50000    0.00765    0.02280 =
         0.01210    0.00000    0.00356    0.00000
HKLF 4

REM  1_a.res in C2/m
REM R1 =  0.0144 for     565 Fo > 4sig(Fo)  and  0.0144 for all     565 data
REM     54 parameters refined using      0 restraints

END

WGHT      0.0177      0.0000

REM Instructions for potential hydrogen bonds
HTAB O1 O3_$1
HTAB O1 F2_$1
HTAB O2 O1_$2

REM Highest difference peak  1.036,  deepest hole -0.535,  1-sigma level  0.103
Q1    1   0.5000  1.1335  1.0000  10.50000  0.05    1.04
Q2    1   0.6491  1.0000  0.9225  10.50000  0.05    0.45
Q3    1   0.5832  0.7921  0.9137  11.00000  0.05    0.33
Q4    1   0.5986  0.5720  0.8467  11.00000  0.05    0.33
Q5    1   0.5450  0.3863  0.6472  11.00000  0.05    0.32
Q6    1   0.5931  0.4732  0.7234  11.00000  0.05    0.30
Q7    1   0.9559  0.5000  0.7731  10.50000  0.05    0.29
Q8    1   0.6558  1.0811  1.0555  11.00000  0.05    0.29
Q9    1   0.4894  0.5000  0.6432  10.50000  0.05    0.29
Q10   1   1.1045  0.5000  0.5765  10.50000  0.05    0.26
Q11   1   0.5437  0.7410  0.8322  11.00000  0.05    0.26
Q12   1   0.6525  0.5000  0.6464  10.50000  0.05    0.26
Q13   1   0.1393  0.6171  0.8377  11.00000  0.05    0.24
Q14   1   0.9169  0.6109  0.6941  11.00000  0.05    0.23
Q15   1   0.4360  1.0000  0.8740  10.50000  0.05    0.23
Q16   1   0.4457  1.0000  0.9612  10.50000  0.05    0.22
Q17   1   0.5767  0.6250  0.5214  11.00000  0.05    0.22
Q18   1   0.8543  0.5000  0.6368  10.50000  0.05    0.22
Q19   1   0.4440  0.5000  0.7425  10.50000  0.05    0.21
Q20   1   0.9324  0.3371  0.6451  11.00000  0.05    0.20
;
_shelx_res_checksum              35625
_olex2_submission_special_instructions 'No special instructions were received'
