# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_293K
_database_code_depnum_ccdc_archive 'CCDC 1988358'
loop_
_audit_author_name
_audit_author_address
'Wei-Xiong Zhang'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2020-02-22
_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         'B3 F12 K, C5 H14 N2'
_chemical_formula_sum            'C5 H14 B3 F12 K N2'
_chemical_formula_weight         401.71
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P b c 21'
_space_group_name_Hall           'P 2c -2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, z'
'x, -y+1/2, z+1/2'

_cell_length_a                   10.27920(10)
_cell_length_b                   9.37590(10)
_cell_length_c                   14.5388(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1401.20(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10778
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.3710
_cell_measurement_theta_min      3.0130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12104
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         77.665
_diffrn_reflns_theta_min         4.301
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2520
_reflns_number_total             2563
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.085
_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)+(0.0614P)²+0.6601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1019
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.94(2)
 0.06(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
K1 K 0.25378(6) 0.70587(6) 0.70117(9) 0.0365(2) Uani 1 1 d . . . . .
F11 F 0.0759(2) 0.9041(3) 0.7415(2) 0.0540(7) Uani 1 1 d . . . . .
F12 F 0.0176(3) 0.8973(3) 0.59118(18) 0.0551(7) Uani 1 1 d . . . . .
F13 F -0.1359(2) 0.9252(3) 0.7004(2) 0.0512(6) Uani 1 1 d . . . . .
F14 F 0.0037(3) 1.1036(2) 0.6714(2) 0.0497(6) Uani 1 1 d . . . . .
F21 F 0.1516(3) 0.6419(3) 0.4895(2) 0.0612(8) Uani 1 1 d . . . . .
F22 F 0.2994(3) 0.8125(4) 0.5176(2) 0.0678(9) Uani 1 1 d . . . . .
F23 F 0.3150(3) 0.6793(3) 0.3884(2) 0.0606(8) Uani 1 1 d . . . . .
F24 F 0.1558(4) 0.8415(3) 0.4032(3) 0.0681(9) Uani 1 1 d . . . . .
F31 F 0.4237(3) 0.5036(3) 0.79367(19) 0.0468(6) Uani 1 1 d . . . . .
F32 F 0.4223(2) 0.4985(3) 0.63863(17) 0.0434(6) Uani 1 1 d . . . . .
F33 F 0.4532(3) 0.2933(2) 0.7190(2) 0.0588(8) Uani 1 1 d . . . . .
F34 F 0.6109(2) 0.4609(2) 0.7157(2) 0.0418(5) Uani 1 1 d . . . . .
B1 B -0.0104(4) 0.9563(4) 0.6765(3) 0.0327(9) Uani 1 1 d . . . . .
B2 B 0.2311(4) 0.7453(7) 0.4494(4) 0.0360(8) Uani 1 1 d . . . . .
B3 B 0.4772(4) 0.4397(4) 0.7161(3) 0.0299(8) Uani 1 1 d . . . . .
N1 N 0.3079(4) 0.1436(4) 0.8645(3) 0.0491(10) Uani 1 1 d . . . . .
H1A H 0.3152 0.0551 0.8430 0.059 Uiso 1 1 calc R . . . .
H1B H 0.3409 0.2022 0.8223 0.059 Uiso 1 1 calc R . . . .
N2 N 0.1410(3) 0.3573(4) 0.9984(3) 0.0449(9) Uani 1 1 d . . . . .
H2A H 0.0751 0.3107 1.0243 0.054 Uiso 1 1 calc R . . . .
H2B H 0.1254 0.4499 1.0059 0.054 Uiso 1 1 calc R . . . .
C1 C 0.1646(5) 0.1776(5) 0.8759(4) 0.0532(12) Uani 1 1 d . . . . .
H1C H 0.1200 0.1546 0.8190 0.064 Uiso 1 1 calc R . . . .
H1D H 0.1292 0.1166 0.9237 0.064 Uiso 1 1 calc R . . . .
C2 C 0.1364(4) 0.3280(5) 0.8999(3) 0.0446(9) Uani 1 1 d . . . . .
H2C H 0.1989 0.3889 0.8690 0.054 Uiso 1 1 calc R . . . .
H2D H 0.0506 0.3525 0.8770 0.054 Uiso 1 1 calc R . . . .
C3 C 0.2598(4) 0.3227(6) 1.0521(3) 0.0422(10) Uani 1 1 d . . . . .
H3A H 0.2431 0.2377 1.0882 0.051 Uiso 1 1 calc R . . . .
H3B H 0.2767 0.4002 1.0947 0.051 Uiso 1 1 calc R . . . .
C4 C 0.3804(4) 0.2983(5) 0.9946(3) 0.0395(9) Uani 1 1 d . . . . .
H4A H 0.3844 0.3713 0.9474 0.047 Uiso 1 1 calc R . . . .
H4B H 0.4562 0.3097 1.0337 0.047 Uiso 1 1 calc R . . . .
C5 C 0.3873(5) 0.1557(6) 0.9494(4) 0.0552(12) Uani 1 1 d . . . . .
H5A H 0.4773 0.1354 0.9343 0.066 Uiso 1 1 calc R . . . .
H5B H 0.3585 0.0838 0.9929 0.066 Uiso 1 1 calc R . . . .


_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 F11 2.672(3) . ?
K1 F13 2.897(3) 3_545 ?
K1 F14 2.848(3) 3_545 ?
K1 F21 3.306(4) . ?
K1 F22 2.888(4) . ?
K1 F23 2.994(4) 4_565 ?
K1 F24 3.136(4) 4_565 ?
K1 F31 2.908(3) . ?
K1 F32 2.758(3) . ?
K1 F33 3.132(3) 3_655 ?
K1 F34 2.774(2) 3_655 ?
K1 B3 3.398(4) . ?
F11 B1 1.386(5) . ?
F12 B1 1.389(5) . ?
F13 K1 2.897(3) 3 ?
F13 B1 1.367(5) . ?
F14 K1 2.848(3) 3 ?
F14 B1 1.391(4) . ?
F21 B2 1.395(6) . ?
F22 B2 1.369(6) . ?
F23 K1 2.994(4) 4_564 ?
F23 B2 1.383(6) . ?
F24 K1 3.136(4) 4_564 ?
F24 B2 1.365(6) . ?
F31 B3 1.390(5) . ?
F32 B3 1.375(5) . ?
F33 K1 3.132(3) 3_645 ?
F33 B3 1.395(4) . ?
F34 K1 2.774(2) 3_645 ?
F34 B3 1.389(4) . ?
B1 K1 3.444(4) 3 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.516(7) . ?
N1 C5 1.484(7) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.459(6) . ?
N2 C3 1.484(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.481(6) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.513(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.492(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

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
F11 K1 F13 110.27(8) . 3_545 ?
F11 K1 F14 68.39(8) . 3_545 ?
F11 K1 F21 96.51(9) . . ?
F11 K1 F22 94.20(10) . . ?
F11 K1 F23 72.18(9) . 4_565 ?
F11 K1 F24 70.92(10) . 4_565 ?
F11 K1 F31 139.72(10) . . ?
F11 K1 F32 172.90(10) . . ?
F11 K1 F33 117.22(8) . 3_655 ?
F11 K1 F34 74.14(7) . 3_655 ?
F11 K1 B3 163.54(11) . . ?
F13 K1 F21 72.47(8) 3_545 . ?
F13 K1 F23 114.72(9) 3_545 4_565 ?
F13 K1 F24 74.97(9) 3_545 4_565 ?
F13 K1 F31 70.17(7) 3_545 . ?
F13 K1 F33 129.82(6) 3_545 3_655 ?
F13 K1 B3 67.41(8) 3_545 . ?
F14 K1 F13 45.98(6) 3_545 3_545 ?
F14 K1 F21 60.16(8) 3_545 . ?
F14 K1 F22 97.29(9) 3_545 . ?
F14 K1 F23 117.03(9) 3_545 4_565 ?
F14 K1 F24 78.24(9) 3_545 4_565 ?
F14 K1 F31 114.15(8) 3_545 . ?
F14 K1 F33 173.89(8) 3_545 3_655 ?
F14 K1 B3 113.00(8) 3_545 . ?
F21 K1 B3 98.09(9) . . ?
F22 K1 F13 112.25(9) . 3_545 ?
F22 K1 F21 41.78(8) . . ?
F22 K1 F23 132.95(7) . 4_565 ?
F22 K1 F24 165.11(9) . 4_565 ?
F22 K1 F31 123.75(9) . . ?
F22 K1 F33 80.21(9) . 3_655 ?
F22 K1 B3 101.74(11) . . ?
F23 K1 F21 167.99(8) 4_565 . ?
F23 K1 F24 42.88(8) 4_565 4_565 ?
F23 K1 F33 68.18(8) 4_565 3_655 ?
F23 K1 B3 93.67(10) 4_565 . ?
F24 K1 F21 138.06(7) 4_565 . ?
F24 K1 B3 93.05(10) 4_565 . ?
F31 K1 F21 120.20(8) . . ?
F31 K1 F23 71.81(8) . 4_565 ?
F31 K1 F24 70.58(9) . 4_565 ?
F31 K1 F33 63.56(7) . 3_655 ?
F31 K1 B3 23.89(9) . . ?
F32 K1 F13 67.73(7) . 3_545 ?
F32 K1 F14 107.24(8) . 3_545 ?
F32 K1 F21 76.39(8) . . ?
F32 K1 F22 80.64(9) . . ?
F32 K1 F23 114.91(9) . 4_565 ?
F32 K1 F24 114.24(9) . 4_565 ?
F32 K1 F31 46.81(7) . . ?
F32 K1 F33 66.92(7) . 3_655 ?
F32 K1 F34 108.54(7) . 3_655 ?
F32 K1 B3 22.93(9) . . ?
F33 K1 F21 115.47(9) 3_655 . ?
F33 K1 F24 105.56(9) 3_655 4_565 ?
F33 K1 B3 62.43(7) 3_655 . ?
F34 K1 F13 173.15(8) 3_655 3_545 ?
F34 K1 F14 140.13(7) 3_655 3_545 ?
F34 K1 F21 112.74(8) 3_655 . ?
F34 K1 F22 71.99(9) 3_655 . ?
F34 K1 F23 61.00(8) 3_655 4_565 ?
F34 K1 F24 102.22(9) 3_655 4_565 ?
F34 K1 F31 103.04(8) 3_655 . ?
F34 K1 F33 44.43(6) 3_655 3_655 ?
F34 K1 B3 106.81(8) 3_655 . ?
B1 F11 K1 122.3(2) . . ?
B1 F13 K1 101.7(2) . 3 ?
B1 F14 K1 103.2(2) . 3 ?
B2 F21 K1 94.5(3) . . ?
B2 F22 K1 115.3(3) . . ?
B2 F23 K1 106.9(3) . 4_564 ?
B2 F24 K1 100.6(3) . 4_564 ?
B3 F31 K1 98.2(2) . . ?
B3 F32 K1 105.7(2) . . ?
B3 F33 K1 94.9(2) . 3_645 ?
B3 F34 K1 111.92(18) . 3_645 ?
F11 B1 K1 129.4(3) . 3 ?
F11 B1 F12 109.6(3) . . ?
F11 B1 F14 108.7(3) . . ?
F12 B1 K1 120.9(3) . 3 ?
F12 B1 F14 109.0(3) . . ?
F13 B1 K1 55.47(17) . 3 ?
F13 B1 F11 110.9(3) . . ?
F13 B1 F12 109.7(4) . . ?
F13 B1 F14 108.9(3) . . ?
F14 B1 K1 53.62(17) . 3 ?
F22 B2 F21 108.5(4) . . ?
F22 B2 F23 110.5(3) . . ?
F23 B2 F21 108.8(5) . . ?
F24 B2 F21 109.5(3) . . ?
F24 B2 F22 110.0(5) . . ?
F24 B2 F23 109.5(4) . . ?
F31 B3 F33 109.2(3) . . ?
F32 B3 F31 109.2(3) . . ?
F32 B3 F33 110.3(3) . . ?
F32 B3 F34 110.2(3) . . ?
F34 B3 F31 109.4(3) . . ?
F34 B3 F33 108.4(3) . . ?
H1A N1 H1B 107.5 . . ?
C1 N1 H1A 108.5 . . ?
C1 N1 H1B 108.5 . . ?
C5 N1 H1A 108.5 . . ?
C5 N1 H1B 108.5 . . ?
C5 N1 C1 115.3(4) . . ?
H2A N2 H2B 106.9 . . ?
C2 N2 H2A 107.3 . . ?
C2 N2 H2B 107.3 . . ?
C2 N2 C3 120.1(3) . . ?
C3 N2 H2A 107.3 . . ?
C3 N2 H2B 107.3 . . ?
N1 C1 H1C 108.6 . . ?
N1 C1 H1D 108.6 . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 N1 114.6(4) . . ?
C2 C1 H1C 108.6 . . ?
C2 C1 H1D 108.6 . . ?
N2 C2 C1 113.8(4) . . ?
N2 C2 H2C 108.8 . . ?
N2 C2 H2D 108.8 . . ?
C1 C2 H2C 108.8 . . ?
C1 C2 H2D 108.8 . . ?
H2C C2 H2D 107.7 . . ?
N2 C3 H3A 108.6 . . ?
N2 C3 H3B 108.6 . . ?
N2 C3 C4 114.6(4) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 C3 114.7(4) . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
N1 C5 C4 114.1(4) . . ?
N1 C5 H5A 108.7 . . ?
N1 C5 H5B 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?

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
N1 H1A F23 0.89 2.29 3.048(5) 142.4 4
N1 H1A F34 0.89 2.19 2.882(4) 134.7 3_645
N1 H1B F33 0.89 2.08 2.945(5) 164.4 .
N2 H2A F12 0.89 2.38 3.190(5) 151.7 2_565
N2 H2A F21 0.89 2.43 3.011(5) 123.7 2_565
N2 H2B F12 0.89 2.20 2.953(4) 142.8 4_565
N2 H2B F24 0.89 2.48 3.149(5) 132.3 4_565
C5 H5B F32 0.97 2.35 3.128(6) 137.0 4

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.94(2)
2 0.06(2)

####################################################################### 
# 
# 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_400K
_database_code_depnum_ccdc_archive 'CCDC 1988360'
loop_
_audit_author_name
_audit_author_address
'Wei-Xiong Zhang'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2020-02-22
_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(B6 F24 K2), 0.5(C10 H28 N4)'
_chemical_formula_sum            'C5 H14 B3 F12 K N2'
_chemical_formula_weight         401.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
B B 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0220 0.0130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2370 0.3140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0080 0.0040 '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      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   10.568(2)
_cell_length_b                   9.929(2)
_cell_length_c                   14.249(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1495.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39189
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.49
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2585
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        27.705
_diffrn_reflns_theta_max         28.983
_diffrn_reflns_theta_min         3.443
_diffrn_ambient_temperature      400(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77487
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                759
_reflns_number_total             805
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.25(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         805
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0772
_refine_ls_restrained_S_all      1.075
_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)+(0.2500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2423
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 B2-F21 = B2-F22 = B2-F23 = B2-F24
 1.36 with sigma of 0.04
 B1-F11 = B1-F12 = B1-F13 = B1-F14 = B1-F11A = B1-F12A = B1-F13A = B1-F14A
 1.36 with sigma of 0.04
 C5-C4 = C4-C3 = C2-C1
 1.53 with sigma of 0.02
 N1-C5 = N1-C1 = N2-C3 = N2-C2
 1.49 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
F21 \\sim F22 \\sim F23 \\sim F24 \\sim B2: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=0.5*(1-FVAR(2))
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=0.5*FVAR(2)
 Fixed Sof: F21(0.25) F22(0.25) F23(0.25) F24(0.25) N1(0.25) H1C(0.25)
 H1D(0.25) N2(0.25) H2A(0.25) H2B(0.25) C1(0.25) H1A(0.25) H1B(0.25) C2(0.25)
 H2C(0.25) H2D(0.25) C3(0.25) H3A(0.25) H3B(0.25) C4(0.25) H4A(0.25) H4B(0.25)
 C5(0.25) H5A(0.25) H5B(0.25)
5.a Riding coordinates:
 N1(H1C,H1D), N2(H2A,H2B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_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
K1 K 0.5000 0.53964(8) 0.7500 0.0890(9) Uani 1 4 d S T P . .
F11 F 0.2740(17) 0.9399(9) 0.7714(17) 0.197(8) Uani 0.347(7) 1 d D U . A -1
F11A F 0.369(3) 0.900(4) 0.729(4) 0.218(11) Uani 0.153(7) 1 d D U . A -2
F12 F 0.1400(7) 0.7826(11) 0.755(2) 0.169(4) Uani 0.347(7) 1 d D U . A -1
F12A F 0.195(3) 0.889(4) 0.707(3) 0.196(9) Uani 0.153(7) 1 d D U . A -2
F13 F 0.334(2) 0.745(2) 0.8190(16) 0.183(6) Uani 0.347(7) 1 d D U . A -1
F13A F 0.310(4) 0.705(4) 0.716(3) 0.188(8) Uani 0.153(7) 1 d D U . A -2
F14 F 0.2963(17) 0.765(2) 0.6618(15) 0.186(6) Uani 0.347(7) 1 d D U . A -1
F14A F 0.235(4) 0.856(5) 0.839(3) 0.200(9) Uani 0.153(7) 1 d D U . A -2
F21 F 0.417(3) 0.389(3) 0.484(3) 0.230(11) Uani 0.25 1 d D U . A -1
F22 F 0.4337(18) 0.576(3) 0.5604(9) 0.155(5) Uani 0.25 1 d D U . A -1
F23 F 0.5945(19) 0.474(3) 0.5658(16) 0.168(6) Uani 0.25 1 d D U . A -1
F24 F 0.561(2) 0.573(4) 0.4381(18) 0.216(12) Uani 0.25 1 d D U . A -1
B1 B 0.2692(6) 0.8122(6) 0.7500 0.1187(16) Uani 1 2 d DS T P . .
B2 B 0.5000 0.5000 0.5000 0.135(3) Uani 1 4 d DS TU P A .
N1 N -0.1215(15) 0.569(3) 0.5447(17) 0.111(5) Uani 0.25 1 d D U . B -1
H1C H -0.1256 0.6303 0.4990 0.133 Uiso 0.25 1 d R . . B -1
H1D H -0.1850 0.5851 0.5842 0.133 Uiso 0.25 1 d R . . B -1
N2 N 0.152(2) 0.485(3) 0.479(2) 0.146(7) Uani 0.25 1 d D U . B -1
H2A H 0.2148 0.5085 0.4407 0.176 Uiso 0.25 1 d R . . B -1
H2B H 0.1872 0.4446 0.5284 0.176 Uiso 0.25 1 d R . . B -1
C1 C 0.000(3) 0.585(2) 0.5953(12) 0.133(5) Uani 0.25 1 d DS TU P B -1
H1A H -0.0040 0.6617 0.6374 0.159 Uiso 0.25 1 d R . . B -1
H1B H 0.0230 0.5051 0.6306 0.159 Uiso 0.25 1 d R . . B -1
C2 C 0.095(3) 0.613(3) 0.519(2) 0.155(7) Uani 0.25 1 d D U . B -1
H2C H 0.1625 0.6691 0.5440 0.186 Uiso 0.25 1 d R . . B -1
H2D H 0.0543 0.6631 0.4687 0.186 Uiso 0.25 1 d R . . B -1
C3 C 0.068(3) 0.387(2) 0.428(2) 0.144(7) Uani 0.25 1 d D U . B -1
H3A H 0.1058 0.3646 0.3677 0.173 Uiso 0.25 1 d R . . B -1
H3B H 0.0604 0.3048 0.4639 0.173 Uiso 0.25 1 d R . . B -1
C4 C -0.061(3) 0.443(3) 0.411(2) 0.148(8) Uani 0.25 1 d D U . B -1
H4A H -0.0981 0.3926 0.3598 0.178 Uiso 0.25 1 d R . . B -1
H4B H -0.0543 0.5368 0.3926 0.178 Uiso 0.25 1 d R . . B -1
C5 C -0.137(3) 0.432(3) 0.503(2) 0.128(6) Uani 0.25 1 d D U . B -1
H5A H -0.2254 0.4121 0.4912 0.153 Uiso 0.25 1 d R . . B -1
H5B H -0.1022 0.3634 0.5443 0.153 Uiso 0.25 1 d R . . B -1


_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 F13 2.861(16) . ?
K1 F13A 2.64(3) . ?
K1 F14 3.35(2) . ?
K1 F22 2.814(16) . ?
K1 F23 2.88(2) . ?
K1 B2 3.5839(7) . ?
K1 B2 3.5839(7) 2_665 ?
F11 B1 1.305(11) . ?
F11A B1 1.40(2) . ?
F12 B1 1.398(10) . ?
F12A B1 1.25(2) . ?
F13 B1 1.374(19) . ?
F13A B1 1.25(2) . ?
F14 B1 1.372(18) . ?
F14A B1 1.38(3) . ?
F21 B2 1.43(3) . ?
F22 B2 1.344(17) . ?
F23 B2 1.40(2) . ?
F24 B2 1.31(2) . ?
B2 K1 3.5839(7) 9_666 ?
N1 H1C 0.8900 . ?
N1 H1D 0.8899 . ?
N1 C1 1.48(2) . ?
N1 C5 1.493(18) . ?
N2 H2A 0.8906 . ?
N2 H2B 0.8897 . ?
N2 C2 1.52(2) . ?
N2 C3 1.507(19) . ?
C1 H1A 0.9703 . ?
C1 H1B 0.9699 . ?
C1 C2 1.510(19) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9699 . ?
C3 H3B 0.9701 . ?
C3 C4 1.49(2) . ?
C4 H4A 0.9698 . ?
C4 H4B 0.9697 . ?
C4 C5 1.54(2) . ?
C5 H5A 0.9698 . ?
C5 H5B 0.9699 . ?

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
F13 K1 F14 42.3(3) . . ?
F13 K1 F23 133.4(7) . . ?
F13 K1 B2 74.7(4) . 2_665 ?
F13 K1 B2 114.8(4) . . ?
F13A K1 B2 83.4(8) . . ?
F13A K1 B2 104.6(9) . 2_665 ?
F14 K1 B2 116.5(3) . 2_665 ?
F14 K1 B2 72.6(3) . . ?
F22 K1 F13 94.9(6) . . ?
F22 K1 F14 52.7(6) . . ?
F22 K1 F23 40.7(5) . . ?
F22 K1 B2 20.0(5) . . ?
F22 K1 B2 165.5(4) . 2_665 ?
F23 K1 F14 91.9(6) . . ?
F23 K1 B2 151.6(5) . 2_665 ?
F23 K1 B2 21.6(4) . . ?
B2 K1 B2 167.39(2) . 2_665 ?
B1 F13 K1 114.0(11) . . ?
B1 F13A K1 136(2) . . ?
B1 F14 K1 91.1(10) . . ?
B2 F22 K1 114.4(13) . . ?
B2 F23 K1 108.7(11) . . ?
F11 B1 F12 103.3(10) . . ?
F11 B1 F13 106.6(14) . . ?
F11 B1 F14 122.6(15) . . ?
F12A B1 F11A 89(2) . . ?
F12A B1 F14A 95(4) . . ?
F13 B1 F12 110.7(15) . . ?
F13A B1 F11A 101(3) . . ?
F13A B1 F12A 123(3) . . ?
F13A B1 F14A 136(3) . . ?
F14 B1 F12 100.2(16) . . ?
F14 B1 F13 112.6(12) . . ?
F14A B1 F11A 101(3) . . ?
K1 B2 K1 180.0 . 9_666 ?
F21 B2 K1 75.8(18) . 9_666 ?
F21 B2 K1 104.2(18) . . ?
F22 B2 K1 45.7(9) . . ?
F22 B2 K1 134.3(9) . 9_666 ?
F22 B2 F21 102.8(13) . . ?
F22 B2 F23 92.7(12) . . ?
F23 B2 K1 49.6(9) . . ?
F23 B2 K1 130.4(9) . 9_666 ?
F23 B2 F21 113.7(16) . . ?
F24 B2 K1 52.7(18) . 9_666 ?
F24 B2 K1 127.3(18) . . ?
F24 B2 F21 128(2) . . ?
F24 B2 F22 111.9(17) . . ?
F24 B2 F23 101.7(15) . . ?
H1C N1 H1D 107.8 . . ?
C1 N1 H1C 109.1 . . ?
C1 N1 H1D 109.1 . . ?
C1 N1 C5 113(2) . . ?
C5 N1 H1C 109.1 . . ?
C5 N1 H1D 109.1 . . ?
H2A N2 H2B 107.1 . . ?
C2 N2 H2A 107.4 . . ?
C2 N2 H2B 104.1 . . ?
C3 N2 H2A 108.4 . . ?
C3 N2 H2B 110.2 . . ?
C3 N2 C2 119(2) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 112.6 . . ?
N1 C1 C2 104(2) . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 111.0 . . ?
N2 C2 H2C 109.2 . . ?
N2 C2 H2D 109.2 . . ?
C1 C2 N2 112(2) . . ?
C1 C2 H2C 109.2 . . ?
C1 C2 H2D 109.2 . . ?
H2C C2 H2D 107.9 . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 N2 112(2) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 107.1 . . ?
C3 C4 H4B 109.6 . . ?
C3 C4 C5 108(3) . . ?
H4A C4 H4B 108.7 . . ?
C5 C4 H4A 113.3 . . ?
C5 C4 H4B 109.7 . . ?
N1 C5 C4 102(2) . . ?
N1 C5 H5A 111.3 . . ?
N1 C5 H5B 111.3 . . ?
C4 C5 H5A 111.3 . . ?
C4 C5 H5B 111.3 . . ?
H5A C5 H5B 109.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT088_400K                
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.28 Note  
RESPONSE: Because there are 22 non-hydrogen atoms per asymmetric 
unit in the disordered structure, the number of parameters for 
refinement is high and the I/sigma for data of high angle is low, which 
causes the poor data/parameter ratio.
;
_vrf_PLAT242_400K                
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of         K1 Check   
RESPONSE: The alert was caused by neighboring disordered cation and 
tetrafluorobrate in structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_338K
_database_code_depnum_ccdc_archive 'CCDC 1988359'
loop_
_audit_author_name
_audit_author_address
'Wei-Xiong Zhang'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2020-02-22
_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         '0.25(B12 F48 K4), C5 H14 N2'
_chemical_formula_sum            'C5 H14 B3 F12 K N2'
_chemical_formula_weight         401.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
B B 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0220 0.0130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2370 0.3140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0080 0.0040 '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      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, z'

_cell_length_a                   10.5005(4)
_cell_length_b                   9.7685(4)
_cell_length_c                   14.0216(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1438.25(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    338(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.49
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.3586
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12852
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.705
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.115
_diffrn_ambient_temperature      338
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77487
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1204
_reflns_number_total             1515
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1515
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.162
_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)+(0.1700P)²+0.2800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2297
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 F33A-B3 = F34-B3 = F34A-B3 = F31A-B3 = F32A-B3 = F31-B3 = F32-B3 = F33-B3
 1.36 with sigma of 0.04
 N1-C1 = N1-C5 = N2-C3 = N2-C2
 1.49 with sigma of 0.02
 C2-C1 = C4-C3 = C5-C4
 1.53 with sigma of 0.02
 F33A-F31A \\sim F33A-F34A \\sim F31A-F34A \\sim F33A-F32A \\sim F31A-F32A
\\sim F34A-F32A \\sim F32-
 F31 \\sim F32-F34 \\sim F31-F34 \\sim F32-F33 \\sim F31-F33 \\sim F34-F33
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F31 \\sim F31A \\sim F32 \\sim F32A \\sim F33 \\sim F33A \\sim F34 \\sim F34A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=0.5*(1-FVAR(2))
 Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=0.5*FVAR(2)
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) N2(0.5) H2A(0.5) H2B(0.5) C1(0.5)
 H1C(0.5) H1D(0.5) C2(0.5) H2C(0.5) H2D(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
K1 K 0.24593(6) 0.71263(8) 0.2500 0.0493(4) Uani 1 2 d S T P A .
F11 F 0.1110(3) 0.9721(3) 0.2500 0.0842(9) Uani 1 2 d S T P A .
F12 F -0.0340(4) 0.8089(3) 0.2500 0.1180(14) Uani 1 2 d S T P A .
F13 F -0.0727(2) 1.0057(2) 0.32880(17) 0.1034(9) Uani 1 1 d . . . . .
F21 F 0.1714(2) 0.8168(3) 0.43543(18) 0.1263(13) Uani 1 1 d . . . . .
F22 F 0.3222(2) 0.8373(3) 0.55169(18) 0.1103(9) Uani 1 1 d . . . . .
F31 F 0.3621(10) 0.4347(16) 0.248(2) 0.136(4) Uani 0.296(13) 1 d D U . A -1
F31A F 0.3771(19) 0.381(3) 0.2250(18) 0.142(7) Uani 0.204(13) 1 d D U . A -2
F32 F 0.5101(16) 0.5878(11) 0.249(2) 0.132(4) Uani 0.296(13) 1 d D U . A -1
F32A F 0.4650(19) 0.5827(18) 0.248(3) 0.131(4) Uani 0.204(13) 1 d D U . A -2
F33 F 0.552(3) 0.392(3) 0.175(2) 0.134(7) Uani 0.296(13) 1 d D U . A -1
F33A F 0.5912(18) 0.409(3) 0.2130(18) 0.121(6) Uani 0.204(13) 1 d D U . A -2
F34 F 0.542(3) 0.3884(17) 0.3299(18) 0.092(5) Uani 0.296(13) 1 d D U . A -1
F34A F 0.492(2) 0.413(3) 0.3523(13) 0.116(6) Uani 0.204(13) 1 d D U . A -2
B1 B -0.0179(5) 0.9472(5) 0.2500 0.0618(12) Uani 1 2 d S T P . .
B2 B 0.2463(4) 0.7500 0.5000 0.0762(16) Uani 1 2 d S T P A .
B3 B 0.4860(6) 0.4484(6) 0.2500 0.0777(16) Uani 1 2 d DS T P . .
N1 N 0.8653(13) 0.8422(17) 0.5339(12) 0.147(6) Uani 0.5 1 d D U . B -1
H1A H 0.9313 0.8671 0.5697 0.176 Uiso 0.5 1 calc R . . B -1
H1B H 0.8553 0.9048 0.4884 0.176 Uiso 0.5 1 calc R . . B -1
N2 N 0.6826(12) 0.662(2) 0.4192(14) 0.191(9) Uani 0.5 1 d D U . B -1
H2A H 0.6525 0.6920 0.3638 0.230 Uiso 0.5 1 calc R . . B -1
H2B H 0.6653 0.5726 0.4204 0.230 Uiso 0.5 1 calc R . . B -1
C1 C 0.8924(9) 0.7071(15) 0.4893(12) 0.108(6) Uani 0.5 1 d D U . B -1
H1C H 0.9813 0.7062 0.4704 0.130 Uiso 0.5 1 calc R . . B -1
H1D H 0.8820 0.6373 0.5379 0.130 Uiso 0.5 1 calc R . . B -1
C2 C 0.8179(12) 0.668(2) 0.4085(14) 0.151(7) Uani 0.5 1 d D U . B -1
H2C H 0.8469 0.5784 0.3879 0.182 Uiso 0.5 1 calc R . . B -1
H2D H 0.8365 0.7316 0.3573 0.182 Uiso 0.5 1 calc R . . B -1
C3 C 0.6022(9) 0.7166(8) 0.4855(11) 0.113(6) Uani 0.5 1 d D U . B -1
H3A H 0.5933 0.6506 0.5368 0.135 Uiso 0.5 1 calc R . . B -1
H3B H 0.5191 0.7262 0.4560 0.135 Uiso 0.5 1 calc R . . B -1
C4 C 0.6358(14) 0.8510(14) 0.5292(13) 0.120(5) Uani 0.5 1 d D U . B -1
H4A H 0.5644 0.8843 0.5664 0.144 Uiso 0.5 1 calc R . . B -1
H4B H 0.6532 0.9170 0.4793 0.144 Uiso 0.5 1 calc R . . B -1
C5 C 0.7512(8) 0.8373(19) 0.5927(11) 0.099(4) Uani 0.5 1 d D U . B -1
H5A H 0.7527 0.9113 0.6388 0.119 Uiso 0.5 1 calc R . . B -1
H5B H 0.7478 0.7513 0.6271 0.119 Uiso 0.5 1 calc R . . B -1


_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 F11 2.903(3) . ?
K1 F12 3.086(4) . ?
K1 F13 2.935(2) 3_545 ?
K1 F13 2.935(2) 8 ?
K1 F21 2.900(3) . ?
K1 F21 2.900(3) 6_556 ?
K1 F22 2.934(3) 4_566 ?
K1 F22 2.934(3) 7_575 ?
K1 F31 2.977(13) . ?
K1 F32 3.030(16) . ?
K1 F32A 2.628(16) . ?
K1 B2 3.52436(15) . ?
F11 B1 1.375(6) . ?
F12 B1 1.362(6) . ?
F13 K1 2.935(2) 3 ?
F13 B1 1.371(3) . ?
F21 B2 1.365(3) . ?
F22 K1 2.934(3) 7_576 ?
F22 B2 1.374(3) . ?
F31 B3 1.308(13) . ?
F31A B3 1.368(16) . ?
F32 B3 1.386(12) . ?
F32A B3 1.330(17) . ?
F33 B3 1.376(17) . ?
F33A B3 1.279(17) . ?
F34 B3 1.396(14) . ?
F34A B3 1.476(18) . ?
B1 K1 3.529(4) 3 ?
B1 F13 1.371(3) 6_556 ?
B2 K1 3.52436(14) 7_576 ?
B2 F21 1.365(3) 4_566 ?
B2 F22 1.374(3) 4_566 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.488(13) . ?
N1 C5 1.455(14) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.430(16) . ?
N2 C3 1.365(15) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.429(16) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.491(15) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.509(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

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
F11 K1 F12 43.06(8) . . ?
F11 K1 F13 107.38(7) . 8 ?
F11 K1 F13 107.38(7) . 3_545 ?
F11 K1 F22 106.16(5) . 7_575 ?
F11 K1 F22 106.16(5) . 4_566 ?
F11 K1 F31 175.0(3) . . ?
F11 K1 F32 142.9(2) . . ?
F11 K1 B2 84.84(3) . . ?
F12 K1 B2 88.25(6) . . ?
F13 K1 F12 67.64(7) 8 . ?
F13 K1 F12 67.64(7) 3_545 . ?
F13 K1 F13 44.23(9) 3_545 8 ?
F13 K1 F31 67.8(3) 3_545 . ?
F13 K1 F31 68.3(4) 8 . ?
F13 K1 F32 107.0(3) 8 . ?
F13 K1 F32 106.7(3) 3_545 . ?
F13 K1 B2 72.40(6) 8 . ?
F13 K1 B2 116.51(6) 3_545 . ?
F21 K1 F11 64.03(5) . . ?
F21 K1 F11 64.03(5) 6_556 . ?
F21 K1 F12 68.66(5) . . ?
F21 K1 F12 68.66(5) 6_556 . ?
F21 K1 F13 74.74(8) . 8 ?
F21 K1 F13 114.33(8) 6_556 8 ?
F21 K1 F13 114.33(8) . 3_545 ?
F21 K1 F13 74.74(8) 6_556 3_545 ?
F21 K1 F21 127.45(10) . 6_556 ?
F21 K1 F22 44.14(7) . 4_566 ?
F21 K1 F22 169.01(7) 6_556 4_566 ?
F21 K1 F22 44.14(7) 6_556 7_575 ?
F21 K1 F22 169.01(7) . 7_575 ?
F21 K1 F31 114.9(6) 6_556 . ?
F21 K1 F31 116.1(6) . . ?
F21 K1 F32 113.2(6) . . ?
F21 K1 F32 112.5(6) 6_556 . ?
F21 K1 B2 148.85(6) 6_556 . ?
F21 K1 B2 21.89(7) . . ?
F22 K1 F12 108.09(5) 4_566 . ?
F22 K1 F12 108.09(5) 7_575 . ?
F22 K1 F13 72.41(7) 4_566 8 ?
F22 K1 F13 72.41(7) 7_575 3_545 ?
F22 K1 F13 114.28(7) 4_566 3_545 ?
F22 K1 F13 114.28(7) 7_575 8 ?
F22 K1 F22 142.73(9) 4_566 7_575 ?
F22 K1 F31 75.3(6) 4_566 . ?
F22 K1 F31 74.2(6) 7_575 . ?
F22 K1 F32 71.1(6) 7_575 . ?
F22 K1 F32 71.9(6) 4_566 . ?
F22 K1 B2 22.25(7) 4_566 . ?
F22 K1 B2 163.62(8) 7_575 . ?
F31 K1 F12 131.9(3) . . ?
F31 K1 F32 42.1(3) . . ?
F31 K1 B2 96.0(6) . . ?
F32 K1 F12 174.0(2) . . ?
F32 K1 B2 92.7(6) . . ?
F32A K1 F11 148.1(5) . . ?
F32A K1 F12 168.8(5) . . ?
F32A K1 F13 101.9(6) . 3_545 ?
F32A K1 F13 102.3(6) . 8 ?
F32A K1 F21 114.4(10) . . ?
F32A K1 F21 113.5(10) . 6_556 ?
F32A K1 F22 71.9(10) . 4_566 ?
F32A K1 F22 70.9(10) . 7_575 ?
F32A K1 B2 93.3(10) . . ?
B1 F11 K1 109.0(3) . . ?
B1 F12 K1 100.6(3) . . ?
B1 F13 K1 104.12(19) . 3 ?
B2 F21 K1 105.76(17) . . ?
B2 F22 K1 103.79(16) . 7_576 ?
B3 F31 K1 108.3(9) . . ?
B3 F32 K1 103.2(9) . . ?
B3 F32A K1 128.4(13) . . ?
F11 B1 K1 122.5(3) . 3 ?
F12 B1 K1 130.2(3) . 3 ?
F12 B1 F11 107.3(4) . . ?
F12 B1 F13 111.2(3) . 6_556 ?
F12 B1 F13 111.2(3) . . ?
F13 B1 K1 53.75(17) . 3 ?
F13 B1 K1 53.75(17) 6_556 3 ?
F13 B1 F11 109.8(3) . . ?
F13 B1 F11 109.8(3) 6_556 . ?
F13 B1 F13 107.4(3) 6_556 . ?
K1 B2 K1 179.88(13) 7_576 . ?
F21 B2 K1 52.35(13) . . ?
F21 B2 K1 127.56(18) 4_566 . ?
F21 B2 K1 127.56(18) . 7_576 ?
F21 B2 K1 52.35(13) 4_566 7_576 ?
F21 B2 F21 109.7(4) 4_566 . ?
F21 B2 F22 112.8(2) . . ?
F21 B2 F22 106.3(2) . 4_566 ?
F21 B2 F22 106.3(2) 4_566 . ?
F21 B2 F22 112.8(2) 4_566 4_566 ?
F22 B2 K1 53.96(12) 4_566 . ?
F22 B2 K1 126.12(17) 4_566 7_576 ?
F22 B2 K1 53.96(12) . 7_576 ?
F22 B2 K1 126.13(17) . . ?
F22 B2 F22 109.1(4) . 4_566 ?
F31 B3 F32 106.4(7) . . ?
F31 B3 F33 116.5(15) . . ?
F31 B3 F34 113.4(16) . . ?
F31A B3 F34A 100.0(13) . . ?
F32 B3 F34 110.3(12) . . ?
F32A B3 F31A 109.6(11) . . ?
F32A B3 F34A 104.7(18) . . ?
F33 B3 F32 106.7(15) . . ?
F33 B3 F34 103.4(7) . . ?
F33A B3 F31A 118.2(12) . . ?
F33A B3 F32A 115.6(16) . . ?
F33A B3 F34A 106.6(10) . . ?
H1A N1 H1B 108.0 . . ?
C1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
C5 N1 H1A 109.3 . . ?
C5 N1 H1B 109.3 . . ?
C5 N1 C1 111.5(11) . . ?
H2A N2 H2B 105.6 . . ?
C2 N2 H2A 104.2 . . ?
C2 N2 H2B 104.2 . . ?
C3 N2 H2A 104.2 . . ?
C3 N2 H2B 104.2 . . ?
C3 N2 C2 132.0(15) . . ?
N1 C1 H1C 107.9 . . ?
N1 C1 H1D 107.9 . . ?
H1C C1 H1D 107.2 . . ?
C2 C1 N1 117.7(15) . . ?
C2 C1 H1C 107.9 . . ?
C2 C1 H1D 107.9 . . ?
N2 C2 H2C 107.8 . . ?
N2 C2 H2D 107.8 . . ?
C1 C2 N2 118.2(16) . . ?
C1 C2 H2C 107.8 . . ?
C1 C2 H2D 107.8 . . ?
H2C C2 H2D 107.1 . . ?
N2 C3 H3A 107.7 . . ?
N2 C3 H3B 107.7 . . ?
N2 C3 C4 118.6(15) . . ?
H3A C3 H3B 107.1 . . ?
C4 C3 H3A 107.7 . . ?
C4 C3 H3B 107.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 C5 110.8(12) . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
N1 C5 C4 108.9(14) . . ?
N1 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
C4 C5 H5A 109.9 . . ?
C4 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT088_338K                
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.61 Note  
RESPONSE: Because there are 24 non-hydrogen atoms per asymmetric 
unit in the disordered structure, the number of parameters for 
refinement is high and the I/sigma for data of high angle is low, which 
causes the poor data/parameter ratio.
;
_vrf_PLAT241_338K                
;
PROBLEM: High   MainMol Ueq as Compared to Neighbors of        F21 Check   
RESPONSE: The alert was caused by neighboring disordered cation and 
tetrafluorobrate in structure.
;
_vrf_PLAT242_338K                
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of         K1 Check   
RESPONSE: The alert was caused by neighboring disordered cation and 
tetrafluorobrate in structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_463K
_database_code_depnum_ccdc_archive 'CCDC 1988361'
loop_
_audit_author_name
_audit_author_address
'Wei-Xiong Zhang'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2020-03-03
_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         'B3 F12 K1, 1(C5 H14 N2)'
_chemical_formula_sum            'C5 H14 B3 F12 K N2'
_chemical_formula_weight         401.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'

_cell_length_a                   7.2964(17)
_cell_length_b                   7.2964(17)
_cell_length_c                   7.2964(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     388.4(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    45
_cell_measurement_temperature    463.0(2)
_cell_measurement_theta_max      17.0240
_cell_measurement_theta_min      6.2220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1925
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            415
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.095
_diffrn_reflns_theta_min         3.950
_diffrn_ambient_temperature      463.0(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'multiwire proportional'
_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                33
_reflns_number_total             139
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         139
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0793
_refine_ls_restrained_S_all      0.413
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.2237
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.36 with sigma of 0.02
 C1-C2 = C3-C4 = C4-C5
 1.53 with sigma of 0.04
 C2-N2 = N2-C3 = C5-N1 = N1-C1
 1.5 with sigma of 0.04
 C1-N2 = C2-C3 = N2-C4 = C3-C5 = C4-N1 = C5-C1 = N1-C2
 2.5 with sigma of 0.04
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim B1: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms of
0.16
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: F1(0.0625) F2(0.0625) F3(0.0625) F4(0.0625) B1(0.0625) N1(0.02083)
 H1A(0.02083) H1B(0.02083) N2(0.02083) H2A(0.02083) H2B(0.02083) C1(0.02083)
 H1C(0.02083) H1D(0.02083) C2(0.02083) H2C(0.02083) H2D(0.02083) C3(0.02083)
 H3A(0.02083) H3B(0.02083) C4(0.02083) H4A(0.02083) H4B(0.02083) C5(0.02083)
 H5A(0.02083) H5B(0.02083)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
K1 K 1.0000 1.0000 0.0000 0.164(6) Uani 1 48 d S T P . .
F1 F 0.966(14) 0.616(13) -0.080(17) 0.21(4) Uani 0.0625 1 d D U . A -1
F2 F 0.957(10) 0.614(17) 0.224(16) 0.22(4) Uani 0.0625 1 d D U . A -1
F3 F 1.175(10) 0.451(17) 0.078(9) 0.22(5) Uani 0.0625 1 d D U . A -1
F4 F 0.882(15) 0.356(8) 0.069(16) 0.19(4) Uani 0.0625 1 d D U . A -1
B1 B 0.995(10) 0.508(11) 0.072(11) 0.21(4) Uani 0.0625 1 d D U . A -1
N1 N 0.39(3) 0.60(2) 0.345(9) 0.038(18) Uani 0.0208 1 d D U . B -1
H1A H 0.3289 0.6166 0.2410 0.045 Uiso 0.0208 1 calc R . . B -1
H1B H 0.4516 0.7044 0.3681 0.045 Uiso 0.0208 1 calc R . . B -1
N2 N 0.412(17) 0.356(14) 0.727(11) 0.04(2) Uani 0.0208 1 d D U . B -1
H2A H 0.3098 0.2899 0.7320 0.050 Uiso 0.0208 1 calc R . . B -1
H2B H 0.4591 0.3588 0.8393 0.050 Uiso 0.0208 1 calc R . . B -1
C1 C 0.258(10) 0.565(12) 0.50(2) 0.039(19) Uani 0.0208 1 d D U . B -1
H1C H 0.1885 0.4542 0.4726 0.046 Uiso 0.0208 1 calc R . . B -1
H1D H 0.1727 0.6659 0.5094 0.046 Uiso 0.0208 1 calc R . . B -1
C2 C 0.36(2) 0.542(14) 0.676(13) 0.04(2) Uani 0.0208 1 d D U . B -1
H2C H 0.4749 0.6131 0.6672 0.046 Uiso 0.0208 1 calc R . . B -1
H2D H 0.2903 0.5936 0.7741 0.046 Uiso 0.0208 1 calc R . . B -1
C3 C 0.55(2) 0.257(12) 0.605(12) 0.04(2) Uani 0.0208 1 d D U . B -1
H3A H 0.4812 0.1673 0.5304 0.048 Uiso 0.0208 1 calc R . . B -1
H3B H 0.6355 0.1924 0.6789 0.048 Uiso 0.0208 1 calc R . . B -1
C4 C 0.642(11) 0.398(15) 0.481(18) 0.037(19) Uani 0.0208 1 d D U . B -1
H4A H 0.6693 0.5066 0.5523 0.045 Uiso 0.0208 1 calc R . . B -1
H4B H 0.7563 0.3468 0.4376 0.045 Uiso 0.0208 1 calc R . . B -1
C5 C 0.52(3) 0.449(17) 0.322(9) 0.038(19) Uani 0.0208 1 d D U . B -1
H5A H 0.6051 0.4802 0.2207 0.046 Uiso 0.0208 1 calc R . . B -1
H5B H 0.4565 0.3403 0.2848 0.046 Uiso 0.0208 1 calc R . . B -1


_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 2.87(10) . ?
K1 F2 3.27(15) . ?
F1 B1 1.38(4) . ?
F2 B1 1.38(4) . ?
F3 B1 1.38(4) . ?
F4 B1 1.38(4) . ?
N1 C1 1.51(8) . ?
N1 C5 1.49(7) . ?
N2 C2 1.45(7) . ?
N2 C3 1.50(6) . ?
C1 C2 1.51(8) . ?
C3 C4 1.54(8) . ?
C4 C5 1.49(8) . ?

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 F2 41.7(18) . . ?
B1 F1 K1 112(7) . . ?
B1 F2 K1 94(5) . . ?
F2 B1 F1 107(4) . . ?
F2 B1 F4 110(4) . . ?
F3 B1 F1 110(5) . . ?
F3 B1 F2 110(4) . . ?
F3 B1 F4 109(4) . . ?
F4 B1 F1 111(5) . . ?
C5 N1 C1 112(8) . . ?
C2 N2 C3 117(5) . . ?
N1 C1 C2 109(6) . . ?
N2 C2 C1 117(8) . . ?
N2 C3 C4 109(6) . . ?
C5 C4 C3 111(7) . . ?
N1 C5 C4 118(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_RINTA01_463K                
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The alert was caused by the low data quality. The diffraction 
intensities were weakened and the crystal quality was reduced when the single 
crystal was heated to 463 K.
;
_vrf_PLAT026_463K                
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        24% Check 
RESPONSE: The alert was caused by the low I/sigma of data.  The diffraction 
intensities were weakened when the single crystal was heated to 463 K. 
;
_vrf_PLAT088_463K                
;
PROBLEM: Poor Data / Parameter Ratio ....................       1.26 Note  
RESPONSE: There are two main reasons for the poor data/parameter ratio. On 
the one hand, the number of unique reflections is low because of the systematic 
absence in high-symmetric cubic cell. On the other hand, the I/sigma of data is 
low, because the diffraction intensities were weakened when the single crystal 
was heated to 463 K. 
;
_vrf_PLAT020_463K                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.192 Report
RESPONSE: The alert was caused by the low data quality. The diffraction 
intensities were weakened and the crystal quality was reduced when the single 
crystal was heated to 463 K.
;
# end Validation Reply Form
