# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_[N(CH3)4][Br4F21]-BrF5
_database_code_depnum_ccdc_archive 'CCDC 2311055'
loop_
_audit_author_name
_audit_author_address
'Florian Kraus'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2023-11-29 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
'Tetramethylammonium (henicosafluoridotetrabromate(V))-bromine pentafluoride (1/1)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '5(Br F5), C4 H12 N, F'
_chemical_formula_sum            'C4 H12 Br5 F26 N'
_chemical_formula_weight         967.70

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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.389(4)
_cell_length_b                   13.389(4)
_cell_length_c                   13.389(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2400(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9797
_cell_measurement_theta_min      2.1512
_cell_measurement_theta_max      33.1300

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_F_000             1808
_exptl_transmission_factor_min   'not measured'
_exptl_transmission_factor_max   'not measured'
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.331
_exptl_absorpt_coefficient_mu    8.569
_shelx_estimated_absorpt_T_min   0.109
_shelx_estimated_absorpt_T_max   0.164
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0987
_exptl_absorpt_correction_T_max  0.2047
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec Microfocus'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            61002
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.151
_diffrn_reflns_theta_max         33.745
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3221
_reflns_number_gt                3042
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX3 v2018.7-2 (Bruker AXS)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Diamond V4.6.8 (Brandenburg, Crystal Impact)'
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+0.2842P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3221
_refine_ls_number_parameters     179
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0655
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.14698(2) 0.14698(2) 0.14698(2) 0.02843(14) Uani 1 3 d S T P . .
Br2 Br 0.36683(3) 0.36404(3) 0.14815(3) 0.02639(9) Uani 1 1 d . . . . .
Br3 Br 0.46870(3) 0.46870(3) 0.46870(3) 0.04010(19) Uani 1 3 d S T P . .
F1 F 0.25366(14) 0.25366(14) 0.25366(14) 0.0219(6) Uani 1 3 d S T P A .
F1A F 0.063(5) 0.068(7) 0.1003(16) 0.060(6) Uani 0.3333 1 d . . P A -1
F1B F 0.0745(18) 0.2406(15) 0.0737(17) 0.095(5) Uani 0.3333 1 d . U P A -1
F1C F 0.2078(15) 0.1291(14) 0.0320(11) 0.064(3) Uani 0.3333 1 d . U P A -1
F1D F 0.2104(15) 0.0518(9) 0.1995(13) 0.060(3) Uani 0.3333 1 d . U P A -1
F1E F 0.0635(17) 0.1600(18) 0.2447(14) 0.084(5) Uani 0.3333 1 d . U P A -1
F2A F 0.4714(3) 0.4090(3) 0.0926(4) 0.0652(11) Uani 1 1 d . . . . .
F2B F 0.4249(4) 0.2464(3) 0.1311(4) 0.0701(15) Uani 1 1 d . . . . .
F2C F 0.3197(6) 0.3578(6) 0.0270(4) 0.104(3) Uani 1 1 d . . . . .
F2D F 0.3326(4) 0.4912(3) 0.1526(4) 0.0709(15) Uani 1 1 d . . . . .
F2E F 0.4412(4) 0.3724(7) 0.2583(4) 0.089(2) Uani 1 1 d . . . . .
F3A F 0.540(5) 0.558(3) 0.524(3) 0.059(6) Uani 0.3333 1 d . U P B -1
F3B F 0.5094(14) 0.3800(14) 0.5603(13) 0.068(4) Uani 0.3333 1 d . U P B -1
F3C F 0.5874(12) 0.441(2) 0.4087(16) 0.083(5) Uani 0.3333 1 d . U P B -1
F3D F 0.440(2) 0.5670(15) 0.3977(15) 0.073(5) Uani 0.3333 1 d . U P B -1
F3E F 0.3747(13) 0.4948(19) 0.5498(12) 0.067(4) Uani 0.3333 1 d . U P B -1
N1 N 0.7352(3) 0.7352(3) 0.7352(3) 0.0259(9) Uani 1 3 d S T P . .
C1 C 0.6707(3) 0.6707(3) 0.6707(3) 0.0356(16) Uani 1 3 d S T P C .
H1A H 0.606095 0.660379 0.703476 0.053 Uiso 0.3333 1 calc R U P . .
H1B H 0.703476 0.606095 0.660379 0.053 Uiso 0.3333 1 calc R U P . .
H1C H 0.660379 0.703476 0.606095 0.053 Uiso 0.3333 1 calc R U P . .
C2 C 0.8380(8) 0.7201(12) 0.7011(12) 0.054(3) Uani 0.5 1 d . . P C 1
H2A H 0.881164 0.771676 0.730023 0.081 Uiso 0.5 1 calc R U P C 1
H2B H 0.840396 0.724519 0.628034 0.081 Uiso 0.5 1 calc R U P C 1
H2C H 0.861346 0.654055 0.722285 0.081 Uiso 0.5 1 calc R U P C 1
C3 C 0.8160(9) 0.7917(16) 0.6765(9) 0.062(4) Uani 0.5 1 d . . P C 2
H3A H 0.854520 0.833795 0.722373 0.093 Uiso 0.5 1 calc R U P C 2
H3B H 0.784289 0.833760 0.625653 0.093 Uiso 0.5 1 calc R U P C 2
H3C H 0.860688 0.743697 0.644068 0.093 Uiso 0.5 1 calc R U P C 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
Br1 F1A 1.668(8) . ?
Br1 F1D 1.685(13) . ?
Br1 F1E 1.730(17) . ?
Br1 F1C 1.759(13) . ?
Br1 F1B 1.864(16) . ?
Br1 F1 2.474(3) . ?
Br2 F2A 1.696(3) . ?
Br2 F2C 1.743(5) . ?
Br2 F2D 1.764(4) . ?
Br2 F2B 1.771(4) . ?
Br2 F2E 1.783(4) . ?
Br2 F1 2.5447(14) . ?
Br3 F3D 1.667(19) . ?
Br3 F3E 1.699(15) . ?
Br3 F3A 1.700(8) . ?
Br3 F3B 1.792(15) . ?
Br3 F3C 1.818(17) . ?
N1 C2 1.465(12) . ?
N1 C2 1.465(12) 9 ?
N1 C2 1.465(12) 5 ?
N1 C1 1.495(9) . ?
N1 C3 1.536(12) . ?
N1 C3 1.536(12) 9 ?
N1 C3 1.536(12) 5 ?

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
F1A Br1 F1D 91(4) . . ?
F1A Br1 F1E 84.8(16) . . ?
F1D Br1 F1E 95.0(8) . . ?
F1A Br1 F1C 84.3(12) . . ?
F1D Br1 F1C 91.7(9) . . ?
F1E Br1 F1C 167.3(9) . . ?
F1A Br1 F1B 83(4) . . ?
F1D Br1 F1B 172.1(8) . . ?
F1E Br1 F1B 89.6(11) . . ?
F1C Br1 F1B 82.6(8) . . ?
F1A Br1 F1 166.6(5) . . ?
F1D Br1 F1 84.5(6) . . ?
F1E Br1 F1 83.0(7) . . ?
F1C Br1 F1 108.5(6) . . ?
F1B Br1 F1 102.5(6) . . ?
F2A Br2 F2C 84.7(3) . . ?
F2A Br2 F2D 83.5(2) . . ?
F2C Br2 F2D 89.1(3) . . ?
F2A Br2 F2B 84.1(2) . . ?
F2C Br2 F2B 89.8(4) . . ?
F2D Br2 F2B 167.6(2) . . ?
F2A Br2 F2E 83.1(3) . . ?
F2C Br2 F2E 167.2(3) . . ?
F2D Br2 F2E 93.3(3) . . ?
F2B Br2 F2E 85.2(3) . . ?
F2A Br2 F1 160.26(18) . . ?
F2C Br2 F1 105.9(3) . . ?
F2D Br2 F1 112.77(14) . . ?
F2B Br2 F1 79.43(14) . . ?
F2E Br2 F1 84.8(3) . . ?
F3D Br3 F3E 91.9(8) . . ?
F3D Br3 F3A 79.8(10) . . ?
F3E Br3 F3A 90(3) . . ?
F3D Br3 F3B 169.3(7) . . ?
F3E Br3 F3B 85.6(8) . . ?
F3A Br3 F3B 89.8(9) . . ?
F3D Br3 F3C 96.2(9) . . ?
F3E Br3 F3C 166.3(8) . . ?
F3A Br3 F3C 81(3) . . ?
F3B Br3 F3C 84.4(8) . . ?
Br1 F1 Br2 111.01(7) . 5 ?
Br1 F1 Br2 111.01(7) . . ?
Br2 F1 Br2 107.89(7) 5 . ?
C2 N1 C2 112.3(5) . 9 ?
C2 N1 C2 112.3(5) . 5 ?
C2 N1 C2 112.3(5) 9 5 ?
C2 N1 C1 106.4(6) . . ?
C2 N1 C1 106.4(6) 9 . ?
C2 N1 C1 106.4(6) 5 . ?
C1 N1 C3 113.3(5) . . ?
C2 N1 C3 71.7(9) . 9 ?
C2 N1 C3 41.1(9) 9 9 ?
C2 N1 C3 137.0(8) 5 9 ?
C1 N1 C3 113.3(5) . 9 ?
C3 N1 C3 105.4(6) . 9 ?
C2 N1 C3 137.0(8) . 5 ?
C2 N1 C3 71.7(9) 9 5 ?
C2 N1 C3 41.1(9) 5 5 ?
C1 N1 C3 113.3(5) . 5 ?
C3 N1 C3 105.4(6) . 5 ?
C3 N1 C3 105.4(6) 9 5 ?

_refine_diff_density_max         0.450
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.091



# start Validation Reply Form
_vrf_PLAT434_NCH34Br4F21-BrF5    
;
PROBLEM: Short Inter HL..HL Contact Br1      ..F1       .       2.47 Ang.  
RESPONSE: BR1 is bound to F1 by a strongly polar covalent bond of 2.47 
Ang.
;
_vrf_PLAT242_NCH34Br4F21-BrF5    
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Br2 Check 
RESPONSE: The neighboring light fluorine atoms exhibit a stronger 
vibrational displacement than the heavier Br atom.
;
_vrf_PLAT034_NCH34Br4F21-BrF5    
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do !  
RESPONSE: Twinning involves inversion, so Flack parameter cannot be 
determined. TWIN 0 -1 0 -1 0 0 0 0 1, BASF 0.465(2)
;
# end Validation Reply Form
_chemical_properties_physical    Moisture-sensitive
