# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_kong1111
_audit_block_doi                 10.5517/ccdc.csd.cc201gn6
_database_code_depnum_ccdc_archive 'CCDC 1848457'
_audit_update_record             
;
2018-06-11 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B9 F K Li3 O15'
_chemical_formula_weight         416.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   11.974(4)
_cell_length_b                   11.974(4)
_cell_length_c                   15.998(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1986.4(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3709
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.35

_exptl_crystal_description       chip
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1212
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_type   none
_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         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3709
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.35
_reflns_number_total             1002
_reflns_number_gt                908
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

_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)+(0.0324P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_number_reflns         1002
_refine_ls_number_parameters     89
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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 0.0000 0.0000 0.15237(7) 0.0243(3) Uani 1 3 d S . .
O2 O 0.10834(17) 0.27308(18) 0.13699(11) 0.0182(4) Uani 1 1 d . . .
F1 F 0.0000 0.0000 -0.01302(16) 0.0181(6) Uani 1 3 d S . .
O1 O 0.17436(17) 0.20640(18) 0.25275(11) 0.0215(5) Uani 1 1 d . . .
B1 B 0.2063(3) 0.2969(3) 0.18870(18) 0.0155(6) Uani 1 1 d . . .
O3 O 0.32947(17) 0.39557(16) 0.18117(10) 0.0152(4) Uani 1 1 d . . .
B3 B 0.0980(3) 0.3550(3) 0.07328(17) 0.0131(6) Uani 1 1 d . . .
B2 B 0.2691(3) 0.2023(3) 0.29928(18) 0.0140(6) Uani 1 1 d . . .
O4 O 0.06284(17) 0.44458(17) 0.11351(11) 0.0159(4) Uani 1 1 d . . .
O5 O 0.22978(18) 0.11554(16) 0.36237(10) 0.0138(4) Uani 1 1 d . . .
Li1 Li -0.1541(4) -0.1193(5) -0.0555(3) 0.0207(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0224(4) 0.0224(4) 0.0280(5) 0.000 0.000 0.01120(18)
O2 0.0142(10) 0.0176(10) 0.0188(8) 0.0046(7) -0.0022(7) 0.0049(8)
F1 0.0161(9) 0.0161(9) 0.0221(14) 0.000 0.000 0.0081(4)
O1 0.0131(10) 0.0234(11) 0.0230(10) 0.0111(8) -0.0005(8) 0.0054(8)
B1 0.0152(15) 0.0155(15) 0.0146(13) -0.0011(11) -0.0019(12) 0.0069(13)
O3 0.0140(9) 0.0125(9) 0.0157(8) 0.0010(7) -0.0036(7) 0.0040(8)
B3 0.0142(15) 0.0123(14) 0.0130(13) -0.0003(11) 0.0012(11) 0.0069(13)
B2 0.0130(15) 0.0117(14) 0.0155(13) -0.0010(11) 0.0004(11) 0.0048(12)
O4 0.0134(9) 0.0149(9) 0.0179(8) -0.0052(7) 0.0002(7) 0.0059(8)
O5 0.0133(9) 0.0128(9) 0.0146(8) 0.0031(7) 0.0016(7) 0.0061(7)
Li1 0.017(2) 0.019(2) 0.027(2) -0.0017(18) 0.006(2) 0.009(2)

_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 F1 2.646(3) . ?
K1 O1 2.808(2) . ?
K1 O1 2.808(2) 3 ?
K1 O1 2.808(2) 2 ?
K1 O2 2.862(2) 3 ?
K1 O2 2.862(2) 2 ?
K1 O2 2.862(2) . ?
K1 B1 3.209(3) . ?
K1 B1 3.209(3) 3 ?
K1 B1 3.209(3) 2 ?
K1 Li1 3.723(5) 2 ?
K1 Li1 3.723(5) 3 ?
O2 B1 1.344(3) . ?
O2 B3 1.462(3) . ?
F1 Li1 1.808(5) . ?
F1 Li1 1.808(5) 2 ?
F1 Li1 1.808(5) 3 ?
O1 B2 1.378(3) . ?
O1 B1 1.399(3) . ?
B1 O3 1.358(3) . ?
O3 B3 1.481(3) 18_554 ?
O3 Li1 1.982(5) 17_554 ?
B3 O5 1.464(3) 15_554 ?
B3 O4 1.481(3) . ?
B3 O3 1.481(3) 12_454 ?
B2 O5 1.353(3) . ?
B2 O4 1.372(3) 18_554 ?
B2 Li1 2.813(6) 4 ?
O4 B2 1.372(3) 12_454 ?
O4 Li1 1.962(5) 18_554 ?
O5 B3 1.464(3) 8 ?
O5 Li1 2.074(5) 4 ?
Li1 O4 1.962(5) 12_454 ?
Li1 O3 1.982(5) 11_444 ?
Li1 O5 2.074(5) 4_554 ?
Li1 B2 2.813(6) 4_554 ?
Li1 Li1 2.903(8) 2 ?
Li1 Li1 2.903(8) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 K1 O1 124.88(4) . . ?
F1 K1 O1 124.88(4) . 3 ?
O1 K1 O1 90.54(6) . 3 ?
F1 K1 O1 124.88(4) . 2 ?
O1 K1 O1 90.54(6) . 2 ?
O1 K1 O1 90.54(6) 3 2 ?
F1 K1 O2 85.07(4) . 3 ?
O1 K1 O2 94.04(5) . 3 ?
O1 K1 O2 48.01(5) 3 3 ?
O1 K1 O2 138.26(6) 2 3 ?
F1 K1 O2 85.07(4) . 2 ?
O1 K1 O2 138.26(6) . 2 ?
O1 K1 O2 94.04(5) 3 2 ?
O1 K1 O2 48.01(5) 2 2 ?
O2 K1 O2 119.269(13) 3 2 ?
F1 K1 O2 85.07(4) . . ?
O1 K1 O2 48.01(5) . . ?
O1 K1 O2 138.26(6) 3 . ?
O1 K1 O2 94.04(5) 2 . ?
O2 K1 O2 119.269(13) 3 . ?
O2 K1 O2 119.269(13) 2 . ?
F1 K1 B1 100.43(6) . . ?
O1 K1 B1 25.79(6) . . ?
O1 K1 B1 113.86(7) 3 . ?
O1 K1 B1 100.67(7) 2 . ?
O2 K1 B1 101.21(7) 3 . ?
O2 K1 B1 139.50(7) 2 . ?
O2 K1 B1 24.75(7) . . ?
F1 K1 B1 100.43(6) . 3 ?
O1 K1 B1 100.67(7) . 3 ?
O1 K1 B1 25.79(6) 3 3 ?
O1 K1 B1 113.86(7) 2 3 ?
O2 K1 B1 24.75(7) 3 3 ?
O2 K1 B1 101.21(7) 2 3 ?
O2 K1 B1 139.50(7) . 3 ?
B1 K1 B1 116.80(3) . 3 ?
F1 K1 B1 100.43(6) . 2 ?
O1 K1 B1 113.86(7) . 2 ?
O1 K1 B1 100.67(7) 3 2 ?
O1 K1 B1 25.79(6) 2 2 ?
O2 K1 B1 139.50(7) 3 2 ?
O2 K1 B1 24.75(7) 2 2 ?
O2 K1 B1 101.21(7) . 2 ?
B1 K1 B1 116.80(3) . 2 ?
B1 K1 B1 116.80(3) 3 2 ?
F1 K1 Li1 26.75(7) . 2 ?
O1 K1 Li1 116.81(9) . 2 ?
O1 K1 Li1 102.99(8) 3 2 ?
O1 K1 Li1 148.87(9) 2 2 ?
O2 K1 Li1 58.85(8) 3 2 ?
O2 K1 Li1 102.48(9) 2 2 ?
O2 K1 Li1 94.06(8) . 2 ?
B1 K1 Li1 99.19(9) . 2 ?
B1 K1 Li1 77.25(9) 3 2 ?
B1 K1 Li1 123.10(10) 2 2 ?
F1 K1 Li1 26.75(7) . 3 ?
O1 K1 Li1 102.99(8) . 3 ?
O1 K1 Li1 148.87(9) 3 3 ?
O1 K1 Li1 116.81(9) 2 3 ?
O2 K1 Li1 102.48(9) 3 3 ?
O2 K1 Li1 94.06(8) 2 3 ?
O2 K1 Li1 58.85(8) . 3 ?
B1 K1 Li1 77.25(9) . 3 ?
B1 K1 Li1 123.10(10) 3 3 ?
B1 K1 Li1 99.19(9) 2 3 ?
Li1 K1 Li1 45.88(12) 2 3 ?
B1 O2 B3 130.1(2) . . ?
B1 O2 K1 92.20(16) . . ?
B3 O2 K1 133.19(15) . . ?
Li1 F1 Li1 106.77(18) . 2 ?
Li1 F1 Li1 106.77(18) . 3 ?
Li1 F1 Li1 106.77(18) 2 3 ?
Li1 F1 K1 112.06(16) . . ?
Li1 F1 K1 112.06(16) 2 . ?
Li1 F1 K1 112.06(16) 3 . ?
B2 O1 B1 120.8(2) . . ?
B2 O1 K1 122.74(17) . . ?
B1 O1 K1 93.32(15) . . ?
O2 B1 O3 125.7(3) . . ?
O2 B1 O1 114.5(2) . . ?
O3 B1 O1 119.8(2) . . ?
O2 B1 K1 63.05(14) . . ?
O3 B1 K1 148.0(2) . . ?
O1 B1 K1 60.89(13) . . ?
B1 O3 B3 121.1(2) . 18_554 ?
B1 O3 Li1 120.1(2) . 17_554 ?
B3 O3 Li1 116.92(19) 18_554 17_554 ?
O2 B3 O5 113.5(2) . 15_554 ?
O2 B3 O4 109.5(2) . . ?
O5 B3 O4 105.7(2) 15_554 . ?
O2 B3 O3 106.4(2) . 12_454 ?
O5 B3 O3 110.9(2) 15_554 12_454 ?
O4 B3 O3 111.0(2) . 12_454 ?
O5 B2 O4 123.7(2) . 18_554 ?
O5 B2 O1 117.0(2) . . ?
O4 B2 O1 119.4(2) 18_554 . ?
O5 B2 Li1 44.35(14) . 4 ?
O4 B2 Li1 134.1(2) 18_554 4 ?
O1 B2 Li1 90.11(18) . 4 ?
B2 O4 B3 118.5(2) 12_454 . ?
B2 O4 Li1 117.7(2) 12_454 18_554 ?
B3 O4 Li1 121.5(2) . 18_554 ?
B2 O5 B3 125.1(2) . 8 ?
B2 O5 Li1 108.5(2) . 4 ?
B3 O5 Li1 111.6(2) 8 4 ?
F1 Li1 O4 108.4(2) . 12_454 ?
F1 Li1 O3 118.2(3) . 11_444 ?
O4 Li1 O3 94.5(2) 12_454 11_444 ?
F1 Li1 O5 106.1(2) . 4_554 ?
O4 Li1 O5 136.1(3) 12_454 4_554 ?
O3 Li1 O5 92.4(2) 11_444 4_554 ?
F1 Li1 B2 128.1(2) . 4_554 ?
O4 Li1 B2 109.1(2) 12_454 4_554 ?
O3 Li1 B2 93.1(2) 11_444 4_554 ?
O5 Li1 B2 27.14(10) 4_554 4_554 ?
F1 Li1 Li1 36.62(9) . 2 ?
O4 Li1 Li1 140.4(3) 12_454 2 ?
O3 Li1 Li1 117.0(2) 11_444 2 ?
O5 Li1 Li1 69.55(19) 4_554 2 ?
B2 Li1 Li1 93.36(16) 4_554 2 ?
F1 Li1 Li1 36.62(9) . 3 ?
O4 Li1 Li1 80.4(3) 12_454 3 ?
O3 Li1 Li1 145.47(15) 11_444 3 ?
O5 Li1 Li1 115.02(15) 4_554 3 ?
B2 Li1 Li1 120.99(11) 4_554 3 ?
Li1 Li1 Li1 60.0 2 3 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.35
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.056
