# Supplementary Information (SI) for Dalton Transactions.
# 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_mo_ZubJu2_a
_database_code_depnum_ccdc_archive 'CCDC 2374510'
loop_
_audit_author_name
_audit_author_address
'Julian Zuber'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2024-11-08 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V144 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;

loop_
_publ_author_phone
08928954134
08928954134
08928954134
0498275218
''
'089 289 54101'
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
'Calix[4]imidazolium[2]dibromo-pyrazole tetrakis(hexafluorophosphate)'
_chemical_name_common            H6LBr2(PF6)4
_chemical_formula_sum            'C24 H26 Br2 F24 N12 P4'
_chemical_formula_moiety         ?
_chemical_formula_weight         1222.27
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_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.
;
_vrf_PLAT088_mo_ZubJu2_a         
;PROBLEM: Poor Data / Parameter Ratio ....................       2.36 Note  
RESPONSE: This is caused by heavy disorder of the macrocylic cation and the PF6 
anions at ambient temperature.
;
_vrf_THETM01_mo_ZubJu2_a         
;PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals (and other compound specimen from different crystal 
growth attempts) were poorly diffracting beyond a certain resolution limit (<1.2
 A). Only a relatively imprecise diffraction dataset with limited resolution 
could be obtained.
;

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

_cell_length_a                   10.703(6)
_cell_length_b                   24.950(16)
_cell_length_c                   18.538(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.850(9)
_cell_angle_gamma                90
_cell_volume                     4826(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6665
_cell_measurement_theta_min      2.1865
_cell_measurement_theta_max      25.3475
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    1.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5539
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.515
_shelx_estimated_absorpt_T_max   0.806
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;Diffractometer operator             T. Pickl
scanspeed                           25 s per frame
dx                                  89 mm
2642 frames measured in 5 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      296(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'IMS microsource'
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           1.0
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 7.5
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Duo'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            31189
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_theta_min         1.984
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_full        20.816
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2533
_reflns_number_gt                1611
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;
_computing_data_collection       'Bruker BIS V6.2.12/2019-08-12'
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL (Sheldrick, 2015), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²+50.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         2533
_refine_ls_number_parameters     1072
_refine_ls_number_restraints     4872
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0985
_refine_ls_wR_factor_ref         0.3090
_refine_ls_wR_factor_gt          0.2648
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      0.638
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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
C9_1 C 0.801(9) 0.3029(18) 0.610(4) 0.072(7) Uani 0.182(3) 1 d D U P A -1
N5_1 N 0.848(7) 0.314(2) 0.551(3) 0.073(7) Uani 0.182(3) 1 d D U P A -1
C10_1 C 0.777(4) 0.3518(15) 0.6405(19) 0.078(7) Uani 0.182(3) 1 d D U P A -1
N6_1 N 0.855(6) 0.368(2) 0.543(3) 0.074(8) Uani 0.182(3) 1 d D U P A -1
H6_1 H 0.883517 0.383616 0.509029 0.088 Uiso 0.182(3) 1 calc R U P A -1
C16_1 C 0.54(2) 0.535(3) 0.758(9) 0.062(7) Uani 0.182(3) 1 d D U P A -1
H16A_1 H 0.610717 0.556116 0.788556 0.074 Uiso 0.182(3) 1 calc R U P A -1
H16B_1 H 0.479867 0.558754 0.729470 0.074 Uiso 0.182(3) 1 calc R U P A -1
C8_1 C 0.820(7) 0.251(3) 0.650(5) 0.068(7) Uani 0.182(3) 1 d D U P A -1
H8A_1 H 0.866716 0.255245 0.701216 0.081 Uiso 0.182(3) 1 calc R U P A -1
H8B_1 H 0.862411 0.224722 0.625668 0.081 Uiso 0.182(3) 1 calc R U P A -1
C11_1 C 0.812(7) 0.3920(19) 0.597(3) 0.076(7) Uani 0.182(3) 1 d D U P A -1
C12_1 C 0.788(9) 0.451(2) 0.590(5) 0.074(7) Uani 0.182(3) 1 d D U P A -1
H12A_1 H 0.739355 0.461382 0.541582 0.088 Uiso 0.182(3) 1 calc R U P A -1
H12B_1 H 0.866421 0.471925 0.603297 0.088 Uiso 0.182(3) 1 calc R U P A -1
C20_1 C 0.228(7) 0.461(2) 0.886(5) 0.063(7) Uani 0.182(3) 1 d D U P A -1
H20A_1 H 0.217449 0.481272 0.929045 0.076 Uiso 0.182(3) 1 calc R U P A -1
H20B_1 H 0.165238 0.473677 0.843395 0.076 Uiso 0.182(3) 1 calc R U P A -1
Br1_1 Br 0.7077(18) 0.3621(8) 0.7258(10) 0.107(6) Uani 0.182(3) 1 d D U P A -1
N7_1 N 0.710(6) 0.452(3) 0.649(3) 0.069(7) Uani 0.182(3) 1 d D U P A -1
N8_1 N 0.597(6) 0.499(3) 0.709(4) 0.065(7) Uani 0.182(3) 1 d D U P A -1
C13_1 C 0.715(5) 0.489(3) 0.701(4) 0.067(8) Uani 0.182(3) 1 d D U P A -1
H13_1 H 0.789481 0.505442 0.727842 0.080 Uiso 0.182(3) 1 calc R U P A -1
C14_1 C 0.582(7) 0.437(3) 0.622(3) 0.069(8) Uani 0.182(3) 1 d D U P A -1
H14_1 H 0.551871 0.411994 0.585649 0.083 Uiso 0.182(3) 1 calc R U P A -1
C15_1 C 0.511(5) 0.467(3) 0.659(4) 0.068(8) Uani 0.182(3) 1 d D U P A -1
H15_1 H 0.422553 0.466205 0.652740 0.081 Uiso 0.182(3) 1 calc R U P A -1
N10_1 N 0.363(7) 0.468(4) 0.874(6) 0.060(7) Uani 0.182(3) 1 d D U P A -1
N9_1 N 0.484(9) 0.499(3) 0.805(4) 0.060(7) Uani 0.182(3) 1 d D U P A -1
C17_1 C 0.370(8) 0.504(4) 0.821(6) 0.060(7) Uani 0.182(3) 1 d D U P A -1
H17_1 H 0.305401 0.527819 0.799827 0.072 Uiso 0.182(3) 1 calc R U P A -1
C19_1 C 0.478(8) 0.440(2) 0.892(4) 0.060(8) Uani 0.182(3) 1 d D U P A -1
H19_1 H 0.497756 0.412516 0.926542 0.073 Uiso 0.182(3) 1 calc R U P A -1
C18_1 C 0.554(6) 0.460(3) 0.849(4) 0.060(8) Uani 0.182(3) 1 d D U P A -1
H18_1 H 0.636986 0.448609 0.848969 0.072 Uiso 0.182(3) 1 calc R U P A -1
N4_1 N 0.680(7) 0.236(5) 0.646(6) 0.064(7) Uani 0.182(3) 1 d D U P A -1
C7_1 C 0.557(8) 0.256(3) 0.616(4) 0.064(8) Uani 0.182(3) 1 d D U P A -1
H7_1 H 0.534401 0.281260 0.578768 0.077 Uiso 0.182(3) 1 calc R U P A -1
C5_1 C 0.674(8) 0.201(5) 0.698(6) 0.062(7) Uani 0.182(3) 1 d D U P A -1
H5_1 H 0.742632 0.182280 0.726896 0.075 Uiso 0.182(3) 1 calc R U P A -1
C6_1 C 0.477(7) 0.230(4) 0.652(4) 0.062(8) Uani 0.182(3) 1 d D U P A -1
H6A_1 H 0.388564 0.234777 0.643254 0.074 Uiso 0.182(3) 1 calc R U P A -1
N3_1 N 0.552(10) 0.196(4) 0.703(5) 0.061(7) Uani 0.182(3) 1 d D U P A -1
C4_1 C 0.533(10) 0.163(3) 0.766(4) 0.061(7) Uani 0.182(3) 1 d D U P A -1
H4A_1 H 0.507603 0.126686 0.748729 0.073 Uiso 0.182(3) 1 calc R U P A -1
H4B_1 H 0.612061 0.160309 0.803253 0.073 Uiso 0.182(3) 1 calc R U P A -1
N2_1 N 0.431(8) 0.187(3) 0.798(3) 0.058(7) Uani 0.182(3) 1 d D U P A -1
C1_1 C 0.315(7) 0.206(4) 0.796(5) 0.057(7) Uani 0.182(3) 1 d D U P A -1
H1_1 H 0.243999 0.202631 0.756914 0.069 Uiso 0.182(3) 1 calc R U P A -1
C3_1 C 0.513(6) 0.201(3) 0.865(4) 0.057(8) Uani 0.182(3) 1 d D U P A -1
H3_1 H 0.599318 0.193472 0.880455 0.069 Uiso 0.182(3) 1 calc R U P A -1
C2_1 C 0.441(7) 0.229(3) 0.904(4) 0.058(8) Uani 0.182(3) 1 d D U P A -1
H2_1 H 0.468008 0.243471 0.950786 0.069 Uiso 0.182(3) 1 calc R U P A -1
N1_1 N 0.317(6) 0.232(4) 0.859(5) 0.057(7) Uani 0.182(3) 1 d D U P A -1
C24_1 C 0.199(7) 0.255(2) 0.881(7) 0.058(7) Uani 0.182(3) 1 d D U P A -1
H24A_1 H 0.126345 0.247345 0.841259 0.070 Uiso 0.182(3) 1 calc R U P A -1
H24B_1 H 0.187393 0.235488 0.924081 0.070 Uiso 0.182(3) 1 calc R U P A -1
C23_1 C 0.193(9) 0.3132(18) 0.899(3) 0.061(7) Uani 0.182(3) 1 d D U P A -1
C22_1 C 0.211(5) 0.3570(14) 0.8556(18) 0.063(7) Uani 0.182(3) 1 d D U P A -1
Br2_1 Br 0.2395(18) 0.3543(9) 0.7578(9) 0.054(4) Uani 0.182(3) 1 d D U P A -1
C21_1 C 0.207(8) 0.4025(18) 0.898(2) 0.064(7) Uani 0.182(3) 1 d D U P A -1
N11_1 N 0.188(8) 0.386(2) 0.964(2) 0.064(7) Uani 0.182(3) 1 d D U P A -1
H11_1 H 0.184106 0.406847 1.000270 0.077 Uiso 0.182(3) 1 calc R U P A -1
N12_1 N 0.178(9) 0.332(2) 0.964(3) 0.062(7) Uani 0.182(3) 1 d D U P A -1
C9_2 C 0.809(7) 0.3135(14) 0.6029(17) 0.076(6) Uani 0.318(3) 1 d D U P B -2
N5_2 N 0.793(5) 0.3240(16) 0.5300(18) 0.076(7) Uani 0.318(3) 1 d D U P B -2
C10_2 C 0.793(3) 0.3603(11) 0.6411(15) 0.082(6) Uani 0.318(3) 1 d D U P B -2
N6_2 N 0.763(3) 0.3767(16) 0.5200(16) 0.075(7) Uani 0.318(3) 1 d D U P B -2
H6_2 H 0.746684 0.393322 0.478241 0.090 Uiso 0.318(3) 1 calc R U P B -2
C16_2 C 0.460(13) 0.5343(18) 0.748(4) 0.064(6) Uani 0.318(3) 1 d D U P B -2
H16A_2 H 0.383980 0.554644 0.725721 0.077 Uiso 0.318(3) 1 calc R U P B -2
H16B_2 H 0.526630 0.559533 0.769729 0.077 Uiso 0.318(3) 1 calc R U P B -2
C8_2 C 0.832(5) 0.2568(18) 0.626(5) 0.070(6) Uani 0.318(3) 1 d D U P B -2
H8A_2 H 0.902133 0.254082 0.668845 0.084 Uiso 0.318(3) 1 calc R U P B -2
H8B_2 H 0.852535 0.235730 0.585997 0.084 Uiso 0.318(3) 1 calc R U P B -2
C11_2 C 0.762(4) 0.3989(13) 0.5863(14) 0.077(6) Uani 0.318(3) 1 d D U P B -2
C12_2 C 0.739(4) 0.4580(15) 0.589(3) 0.075(6) Uani 0.318(3) 1 d D U P B -2
H12A_2 H 0.723553 0.472604 0.539725 0.090 Uiso 0.318(3) 1 calc R U P B -2
H12B_2 H 0.814818 0.475109 0.618521 0.090 Uiso 0.318(3) 1 calc R U P B -2
C20_2 C 0.172(3) 0.4404(13) 0.875(3) 0.070(6) Uani 0.318(3) 1 d D U P B -2
H20A_2 H 0.142478 0.459568 0.914029 0.084 Uiso 0.318(3) 1 calc R U P B -2
H20B_2 H 0.109546 0.446436 0.829459 0.084 Uiso 0.318(3) 1 calc R U P B -2
Br1_2 Br 0.806(2) 0.3667(5) 0.7447(9) 0.115(5) Uani 0.318(3) 1 d D U P B -2
N7_2 N 0.625(4) 0.471(2) 0.623(3) 0.068(6) Uani 0.318(3) 1 d D U P B -2
N8_2 N 0.502(5) 0.504(2) 0.690(3) 0.064(6) Uani 0.318(3) 1 d D U P B -2
C13_2 C 0.622(5) 0.500(3) 0.683(3) 0.066(6) Uani 0.318(3) 1 d D U P B -2
H13_2 H 0.693208 0.515151 0.715375 0.079 Uiso 0.318(3) 1 calc R U P B -2
C14_2 C 0.500(4) 0.4559(17) 0.590(2) 0.067(7) Uani 0.318(3) 1 d D U P B -2
H14_2 H 0.475074 0.435298 0.547220 0.080 Uiso 0.318(3) 1 calc R U P B -2
C15_2 C 0.423(4) 0.4764(17) 0.631(2) 0.066(6) Uani 0.318(3) 1 d D U P B -2
H15_2 H 0.334044 0.473192 0.622418 0.080 Uiso 0.318(3) 1 calc R U P B -2
N10_2 N 0.300(3) 0.4651(15) 0.868(2) 0.068(6) Uani 0.318(3) 1 d D U P B -2
N9_2 N 0.431(4) 0.500(2) 0.807(2) 0.065(6) Uani 0.318(3) 1 d D U P B -2
C17_2 C 0.309(3) 0.4958(18) 0.811(2) 0.066(6) Uani 0.318(3) 1 d D U P B -2
H17_2 H 0.240107 0.512060 0.778201 0.079 Uiso 0.318(3) 1 calc R U P B -2
C19_2 C 0.423(4) 0.4494(17) 0.904(2) 0.070(6) Uani 0.318(3) 1 d D U P B -2
H19_2 H 0.444509 0.426935 0.944744 0.084 Uiso 0.318(3) 1 calc R U P B -2
C18_2 C 0.505(3) 0.4727(19) 0.868(2) 0.069(7) Uani 0.318(3) 1 d D U P B -2
H18_2 H 0.594308 0.471179 0.881311 0.082 Uiso 0.318(3) 1 calc R U P B -2
N4_2 N 0.707(4) 0.238(3) 0.644(3) 0.064(6) Uani 0.318(3) 1 d D U P B -2
C7_2 C 0.586(4) 0.250(3) 0.601(3) 0.063(7) Uani 0.318(3) 1 d D U P B -2
H7_2 H 0.567647 0.269828 0.558013 0.076 Uiso 0.318(3) 1 calc R U P B -2
C5_2 C 0.696(5) 0.207(3) 0.700(4) 0.063(6) Uani 0.318(3) 1 d D U P B -2
H5_2 H 0.763679 0.193135 0.736172 0.075 Uiso 0.318(3) 1 calc R U P B -2
C6_2 C 0.501(4) 0.227(3) 0.636(3) 0.062(7) Uani 0.318(3) 1 d D U P B -2
H6A_2 H 0.412125 0.228075 0.621048 0.074 Uiso 0.318(3) 1 calc R U P B -2
N3_2 N 0.573(5) 0.200(2) 0.697(3) 0.061(6) Uani 0.318(3) 1 d D U P B -2
C4_2 C 0.523(8) 0.1626(16) 0.747(4) 0.061(6) Uani 0.318(3) 1 d D U P B -2
H4A_2 H 0.591352 0.138524 0.771040 0.073 Uiso 0.318(3) 1 calc R U P B -2
H4B_2 H 0.454170 0.141219 0.718650 0.073 Uiso 0.318(3) 1 calc R U P B -2
N2_2 N 0.476(4) 0.194(2) 0.804(2) 0.059(6) Uani 0.318(3) 1 d D U P B -2
C1_2 C 0.350(4) 0.197(2) 0.795(3) 0.058(6) Uani 0.318(3) 1 d D U P B -2
H1_2 H 0.289842 0.181893 0.756271 0.070 Uiso 0.318(3) 1 calc R U P B -2
C3_2 C 0.534(4) 0.220(3) 0.870(3) 0.060(7) Uani 0.318(3) 1 d D U P B -2
H3_2 H 0.621211 0.222471 0.890197 0.072 Uiso 0.318(3) 1 calc R U P B -2
C2_2 C 0.438(5) 0.241(3) 0.898(3) 0.061(7) Uani 0.318(3) 1 d D U P B -2
H2_2 H 0.447395 0.261476 0.940311 0.073 Uiso 0.318(3) 1 calc R U P B -2
N1_2 N 0.324(4) 0.226(2) 0.850(3) 0.060(6) Uani 0.318(3) 1 d D U P B -2
C24_2 C 0.196(4) 0.2353(13) 0.871(3) 0.062(6) Uani 0.318(3) 1 d D U P B -2
H24A_2 H 0.126182 0.225937 0.829949 0.075 Uiso 0.318(3) 1 calc R U P B -2
H24B_2 H 0.189528 0.213255 0.913207 0.075 Uiso 0.318(3) 1 calc R U P B -2
C23_2 C 0.188(5) 0.2927(11) 0.8897(15) 0.063(6) Uani 0.318(3) 1 d D U P B -2
C22_2 C 0.179(3) 0.3385(9) 0.8464(14) 0.069(6) Uani 0.318(3) 1 d D U P B -2
Br2_2 Br 0.177(2) 0.3424(5) 0.7436(7) 0.107(4) Uani 0.318(3) 1 d D U P B -2
C21_2 C 0.174(5) 0.3819(11) 0.8927(14) 0.068(6) Uani 0.318(3) 1 d D U P B -2
N11_2 N 0.188(5) 0.3624(13) 0.9614(15) 0.064(6) Uani 0.318(3) 1 d D U P B -2
H11_2 H 0.194679 0.381460 1.000756 0.076 Uiso 0.318(3) 1 calc R U P B -2
N12_2 N 0.191(5) 0.3081(13) 0.9594(15) 0.064(6) Uani 0.318(3) 1 d D U P B -2
P1_3 P 0.4123(13) 0.3558(6) 0.3969(7) 0.081(4) Uani 0.535(4) 1 d D U P C 1
F1_3 F 0.493(2) 0.3342(9) 0.4729(10) 0.114(7) Uani 0.535(4) 1 d D U P C 1
F2_3 F 0.2859(19) 0.3464(13) 0.4246(18) 0.154(8) Uani 0.535(4) 1 d D U P C 1
F3_3 F 0.332(2) 0.3777(7) 0.3201(9) 0.122(7) Uani 0.535(4) 1 d D U P C 1
F4_3 F 0.5401(18) 0.3621(11) 0.3691(13) 0.135(7) Uani 0.535(4) 1 d D U P C 1
F5_3 F 0.442(2) 0.4139(6) 0.4284(13) 0.120(8) Uani 0.535(4) 1 d D U P C 1
F6_3 F 0.411(3) 0.2992(8) 0.3614(15) 0.135(9) Uani 0.535(4) 1 d D U P C 1
P1_4 P 0.404(2) 0.3545(10) 0.3988(15) 0.080(8) Uani 0.229(4) 1 d D U P D 2
F1_4 F 0.495(4) 0.3115(14) 0.445(2) 0.111(12) Uani 0.229(4) 1 d D U P D 2
F2_4 F 0.359(5) 0.3708(18) 0.471(2) 0.115(11) Uani 0.229(4) 1 d D U P D 2
F3_4 F 0.308(4) 0.3959(15) 0.352(3) 0.126(12) Uani 0.229(4) 1 d D U P D 2
F4_4 F 0.455(5) 0.3399(19) 0.3285(19) 0.111(10) Uani 0.229(4) 1 d D U P D 2
F5_4 F 0.514(4) 0.3973(16) 0.414(3) 0.109(11) Uani 0.229(4) 1 d D U P D 2
F6_4 F 0.294(4) 0.3117(16) 0.380(3) 0.104(11) Uani 0.229(4) 1 d D U P D 2
P1_5 P 0.401(2) 0.3549(12) 0.4102(15) 0.093(8) Uani 0.237(4) 1 d D U P E 3
F1_5 F 0.353(5) 0.3338(17) 0.479(2) 0.132(12) Uani 0.237(4) 1 d D U P E 3
F2_5 F 0.260(3) 0.3659(19) 0.367(2) 0.105(9) Uani 0.237(4) 1 d D U P E 3
F3_5 F 0.449(4) 0.3774(17) 0.342(2) 0.118(11) Uani 0.237(4) 1 d D U P E 3
F4_5 F 0.544(3) 0.345(2) 0.453(3) 0.120(12) Uani 0.237(4) 1 d D U P E 3
F5_5 F 0.364(5) 0.4132(13) 0.432(3) 0.114(11) Uani 0.237(4) 1 d D U P E 3
F6_5 F 0.364(6) 0.2999(16) 0.369(3) 0.108(12) Uani 0.237(4) 1 d D U P E 3
P1_6 P 1.0793(13) 0.5536(5) 0.6207(7) 0.095(4) Uani 0.538(4) 1 d D U P F 1
F1_6 F 1.105(2) 0.4953(6) 0.6502(13) 0.131(8) Uani 0.538(4) 1 d D U P F 1
F2_6 F 0.979(2) 0.5330(9) 0.5510(10) 0.153(7) Uani 0.538(4) 1 d D U P F 1
F3_6 F 1.0519(19) 0.6132(6) 0.5917(11) 0.109(6) Uani 0.538(4) 1 d D U P F 1
F4_6 F 1.173(2) 0.5768(7) 0.6920(11) 0.113(7) Uani 0.538(4) 1 d D U P F 1
F5_6 F 0.966(2) 0.5576(8) 0.6616(12) 0.127(7) Uani 0.538(4) 1 d D U P F 1
F6_6 F 1.189(3) 0.5509(8) 0.5763(15) 0.134(7) Uani 0.538(4) 1 d D U P F 1
P1_7 P 1.131(2) 0.5325(10) 0.6283(15) 0.102(7) Uani 0.254(4) 1 d D U P G 2
F1_7 F 1.233(3) 0.4903(13) 0.668(2) 0.126(11) Uani 0.254(4) 1 d D U P G 2
F2_7 F 1.028(3) 0.4867(14) 0.614(3) 0.141(12) Uani 0.254(4) 1 d D U P G 2
F3_7 F 1.031(3) 0.5743(15) 0.587(2) 0.133(12) Uani 0.254(4) 1 d D U P G 2
F4_7 F 1.234(3) 0.5778(14) 0.653(3) 0.134(12) Uani 0.254(4) 1 d D U P G 2
F5_7 F 1.080(5) 0.540(2) 0.701(2) 0.149(12) Uani 0.254(4) 1 d D U P G 2
F6_7 F 1.181(5) 0.526(2) 0.555(2) 0.138(13) Uani 0.254(4) 1 d D U P G 2
P1_8 P 1.116(3) 0.5446(17) 0.6308(18) 0.106(9) Uani 0.207(4) 1 d D U P H 3
F1_8 F 1.143(5) 0.562(3) 0.7146(19) 0.117(14) Uani 0.207(4) 1 d D U P H 3
F2_8 F 1.159(8) 0.486(2) 0.655(3) 0.133(13) Uani 0.207(4) 1 d D U P H 3
F3_8 F 1.088(5) 0.528(2) 0.5469(19) 0.129(13) Uani 0.207(4) 1 d D U P H 3
F4_8 F 1.128(6) 0.6050(17) 0.608(3) 0.124(13) Uani 0.207(4) 1 d D U P H 3
F5_8 F 0.970(3) 0.559(3) 0.623(3) 0.126(13) Uani 0.207(4) 1 d D U P H 3
F6_8 F 1.263(3) 0.546(3) 0.633(3) 0.131(12) Uani 0.207(4) 1 d D U P H 3


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
C9_1 N5_1 1.34(2) . ?
C9_1 C10_1 1.39(2) . ?
C9_1 C8_1 1.49(3) . ?
N5_1 N6_1 1.35(3) . ?
C10_1 C11_1 1.39(2) . ?
C10_1 Br1_1 1.91(2) . ?
N6_1 C11_1 1.34(2) . ?
N6_1 H6_1 0.8600 . ?
C16_1 N9_1 1.48(2) . ?
C16_1 N8_1 1.48(2) . ?
C16_1 H16A_1 0.9700 . ?
C16_1 H16B_1 0.9700 . ?
C8_1 N4_1 1.52(2) . ?
C8_1 H8A_1 0.9700 . ?
C8_1 H8B_1 0.9700 . ?
C11_1 C12_1 1.49(3) . ?
C12_1 N7_1 1.53(2) . ?
C12_1 H12A_1 0.9700 . ?
C12_1 H12B_1 0.9700 . ?
C20_1 C21_1 1.50(3) . ?
C20_1 N10_1 1.53(2) . ?
C20_1 H20A_1 0.9700 . ?
C20_1 H20B_1 0.9700 . ?
N7_1 C13_1 1.32(2) . ?
N7_1 C14_1 1.40(2) . ?
N8_1 C13_1 1.33(2) . ?
N8_1 C15_1 1.40(2) . ?
C13_1 H13_1 0.9300 . ?
C14_1 C15_1 1.35(2) . ?
C14_1 H14_1 0.9300 . ?
C15_1 H15_1 0.9300 . ?
N10_1 C17_1 1.33(2) . ?
N10_1 C19_1 1.39(2) . ?
N9_1 C17_1 1.33(2) . ?
N9_1 C18_1 1.40(2) . ?
C17_1 H17_1 0.9300 . ?
C19_1 C18_1 1.35(2) . ?
C19_1 H19_1 0.9300 . ?
C18_1 H18_1 0.9300 . ?
N4_1 C5_1 1.33(2) . ?
N4_1 C7_1 1.395(19) . ?
C7_1 C6_1 1.35(2) . ?
C7_1 H7_1 0.9300 . ?
C5_1 N3_1 1.33(2) . ?
C5_1 H5_1 0.9300 . ?
C6_1 N3_1 1.396(19) . ?
C6_1 H6A_1 0.9300 . ?
N3_1 C4_1 1.49(2) . ?
C4_1 N2_1 1.48(2) . ?
C4_1 H4A_1 0.9700 . ?
C4_1 H4B_1 0.9700 . ?
N2_1 C1_1 1.33(2) . ?
N2_1 C3_1 1.40(2) . ?
C1_1 N1_1 1.330(19) . ?
C1_1 H1_1 0.9300 . ?
C3_1 C2_1 1.35(2) . ?
C3_1 H3_1 0.9300 . ?
C2_1 N1_1 1.393(19) . ?
C2_1 H2_1 0.9300 . ?
N1_1 C24_1 1.52(2) . ?
C24_1 C23_1 1.49(3) . ?
C24_1 H24A_1 0.9700 . ?
C24_1 H24B_1 0.9700 . ?
C23_1 N12_1 1.34(2) . ?
C23_1 C22_1 1.39(2) . ?
C22_1 C21_1 1.39(2) . ?
C22_1 Br2_1 1.90(2) . ?
C21_1 N11_1 1.34(2) . ?
N11_1 N12_1 1.35(3) . ?
N11_1 H11_1 0.8600 . ?
C9_2 N5_2 1.35(2) . ?
C9_2 C10_2 1.39(2) . ?
C9_2 C8_2 1.48(2) . ?
N5_2 N6_2 1.36(3) . ?
C10_2 C11_2 1.38(2) . ?
C10_2 Br1_2 1.90(2) . ?
N6_2 C11_2 1.35(2) . ?
N6_2 H6_2 0.8600 . ?
C16_2 N8_2 1.47(2) . ?
C16_2 N9_2 1.48(2) . ?
C16_2 H16A_2 0.9700 . ?
C16_2 H16B_2 0.9700 . ?
C8_2 N4_2 1.52(2) . ?
C8_2 H8A_2 0.9700 . ?
C8_2 H8B_2 0.9700 . ?
C11_2 C12_2 1.50(3) . ?
C12_2 N7_2 1.53(2) . ?
C12_2 H12A_2 0.9700 . ?
C12_2 H12B_2 0.9700 . ?
C20_2 C21_2 1.50(3) . ?
C20_2 N10_2 1.53(2) . ?
C20_2 H20A_2 0.9700 . ?
C20_2 H20B_2 0.9700 . ?
N7_2 C13_2 1.332(19) . ?
N7_2 C14_2 1.394(19) . ?
N8_2 C13_2 1.322(19) . ?
N8_2 C15_2 1.396(19) . ?
C13_2 H13_2 0.9300 . ?
C14_2 C15_2 1.35(2) . ?
C14_2 H14_2 0.9300 . ?
C15_2 H15_2 0.9300 . ?
N10_2 C17_2 1.332(19) . ?
N10_2 C19_2 1.395(19) . ?
N9_2 C17_2 1.330(19) . ?
N9_2 C18_2 1.401(19) . ?
C17_2 H17_2 0.9300 . ?
C19_2 C18_2 1.35(2) . ?
C19_2 H19_2 0.9300 . ?
C18_2 H18_2 0.9300 . ?
N4_2 C5_2 1.326(18) . ?
N4_2 C7_2 1.391(19) . ?
C7_2 C6_2 1.35(2) . ?
C7_2 H7_2 0.9300 . ?
C5_2 N3_2 1.326(18) . ?
C5_2 H5_2 0.9300 . ?
C6_2 N3_2 1.396(18) . ?
C6_2 H6A_2 0.9300 . ?
N3_2 C4_2 1.49(2) . ?
C4_2 N2_2 1.49(2) . ?
C4_2 H4A_2 0.9700 . ?
C4_2 H4B_2 0.9700 . ?
N2_2 C1_2 1.329(18) . ?
N2_2 C3_2 1.394(18) . ?
C1_2 N1_2 1.334(18) . ?
C1_2 H1_2 0.9300 . ?
C3_2 C2_2 1.35(2) . ?
C3_2 H3_2 0.9300 . ?
C2_2 N1_2 1.391(18) . ?
C2_2 H2_2 0.9300 . ?
N1_2 C24_2 1.52(2) . ?
C24_2 C23_2 1.48(3) . ?
C24_2 H24A_2 0.9700 . ?
C24_2 H24B_2 0.9700 . ?
C23_2 N12_2 1.34(2) . ?
C23_2 C22_2 1.39(2) . ?
C22_2 C21_2 1.39(2) . ?
C22_2 Br2_2 1.91(2) . ?
C21_2 N11_2 1.34(2) . ?
N11_2 N12_2 1.36(3) . ?
N11_2 H11_2 0.8600 . ?
P1_3 F6_3 1.558(14) . ?
P1_3 F2_3 1.566(14) . ?
P1_3 F5_3 1.568(14) . ?
P1_3 F1_3 1.573(13) . ?
P1_3 F4_3 1.574(15) . ?
P1_3 F3_3 1.588(14) . ?
P1_4 F4_4 1.565(17) . ?
P1_4 F2_4 1.566(17) . ?
P1_4 F1_4 1.568(17) . ?
P1_4 F6_4 1.569(17) . ?
P1_4 F5_4 1.569(17) . ?
P1_4 F3_4 1.574(17) . ?
P1_5 F1_5 1.567(17) . ?
P1_5 F3_5 1.568(17) . ?
P1_5 F2_5 1.568(17) . ?
P1_5 F4_5 1.570(17) . ?
P1_5 F6_5 1.578(17) . ?
P1_5 F5_5 1.580(17) . ?
P1_6 F1_6 1.557(14) . ?
P1_6 F5_6 1.571(14) . ?
P1_6 F2_6 1.571(14) . ?
P1_6 F6_6 1.577(14) . ?
P1_6 F4_6 1.580(14) . ?
P1_6 F3_6 1.586(14) . ?
P1_7 F3_7 1.564(17) . ?
P1_7 F5_7 1.568(17) . ?
P1_7 F2_7 1.568(17) . ?
P1_7 F1_7 1.571(16) . ?
P1_7 F4_7 1.572(17) . ?
P1_7 F6_7 1.576(17) . ?
P1_8 F6_8 1.568(17) . ?
P1_8 F3_8 1.569(17) . ?
P1_8 F2_8 1.571(17) . ?
P1_8 F5_8 1.572(17) . ?
P1_8 F1_8 1.575(17) . ?
P1_8 F4_8 1.579(17) . ?

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
N5_1 C9_1 C10_1 107(3) . . ?
N5_1 C9_1 C8_1 124(4) . . ?
C10_1 C9_1 C8_1 125(4) . . ?
C9_1 N5_1 N6_1 108.9(17) . . ?
C11_1 C10_1 C9_1 107(3) . . ?
C11_1 C10_1 Br1_1 126.2(19) . . ?
C9_1 C10_1 Br1_1 126.5(19) . . ?
C11_1 N6_1 N5_1 110.0(18) . . ?
C11_1 N6_1 H6_1 125.0 . . ?
N5_1 N6_1 H6_1 125.0 . . ?
N9_1 C16_1 N8_1 106(7) . . ?
N9_1 C16_1 H16A_1 110.4 . . ?
N8_1 C16_1 H16A_1 110.4 . . ?
N9_1 C16_1 H16B_1 110.4 . . ?
N8_1 C16_1 H16B_1 110.4 . . ?
H16A_1 C16_1 H16B_1 108.6 . . ?
C9_1 C8_1 N4_1 99(6) . . ?
C9_1 C8_1 H8A_1 112.0 . . ?
N4_1 C8_1 H8A_1 112.0 . . ?
C9_1 C8_1 H8B_1 112.0 . . ?
N4_1 C8_1 H8B_1 112.0 . . ?
H8A_1 C8_1 H8B_1 109.7 . . ?
N6_1 C11_1 C10_1 107(3) . . ?
N6_1 C11_1 C12_1 118(3) . . ?
C10_1 C11_1 C12_1 134(3) . . ?
C11_1 C12_1 N7_1 94(4) . . ?
C11_1 C12_1 H12A_1 112.9 . . ?
N7_1 C12_1 H12A_1 112.9 . . ?
C11_1 C12_1 H12B_1 112.9 . . ?
N7_1 C12_1 H12B_1 112.9 . . ?
H12A_1 C12_1 H12B_1 110.3 . . ?
C21_1 C20_1 N10_1 109(6) . . ?
C21_1 C20_1 H20A_1 110.0 . . ?
N10_1 C20_1 H20A_1 110.0 . . ?
C21_1 C20_1 H20B_1 110.0 . . ?
N10_1 C20_1 H20B_1 110.0 . . ?
H20A_1 C20_1 H20B_1 108.4 . . ?
C13_1 N7_1 C14_1 109.4(16) . . ?
C13_1 N7_1 C12_1 127(6) . . ?
C14_1 N7_1 C12_1 113(6) . . ?
C13_1 N8_1 C15_1 109.1(16) . . ?
C13_1 N8_1 C16_1 133(10) . . ?
C15_1 N8_1 C16_1 118(10) . . ?
N7_1 C13_1 N8_1 108.3(17) . . ?
N7_1 C13_1 H13_1 125.9 . . ?
N8_1 C13_1 H13_1 125.9 . . ?
C15_1 C14_1 N7_1 106.5(12) . . ?
C15_1 C14_1 H14_1 126.8 . . ?
N7_1 C14_1 H14_1 126.7 . . ?
C14_1 C15_1 N8_1 106.7(12) . . ?
C14_1 C15_1 H15_1 126.7 . . ?
N8_1 C15_1 H15_1 126.7 . . ?
C17_1 N10_1 C19_1 109.1(16) . . ?
C17_1 N10_1 C20_1 113(7) . . ?
C19_1 N10_1 C20_1 136(6) . . ?
C17_1 N9_1 C18_1 109.3(16) . . ?
C17_1 N9_1 C16_1 129(9) . . ?
C18_1 N9_1 C16_1 121(10) . . ?
N9_1 C17_1 N10_1 108.3(17) . . ?
N9_1 C17_1 H17_1 125.9 . . ?
N10_1 C17_1 H17_1 125.9 . . ?
C18_1 C19_1 N10_1 106.9(12) . . ?
C18_1 C19_1 H19_1 126.6 . . ?
N10_1 C19_1 H19_1 126.6 . . ?
C19_1 C18_1 N9_1 106.5(12) . . ?
C19_1 C18_1 H18_1 126.7 . . ?
N9_1 C18_1 H18_1 126.7 . . ?
C5_1 N4_1 C7_1 109.0(15) . . ?
C5_1 N4_1 C8_1 109(7) . . ?
C7_1 N4_1 C8_1 140(7) . . ?
C6_1 C7_1 N4_1 106.8(12) . . ?
C6_1 C7_1 H7_1 126.6 . . ?
N4_1 C7_1 H7_1 126.6 . . ?
N3_1 C5_1 N4_1 108.3(17) . . ?
N3_1 C5_1 H5_1 125.8 . . ?
N4_1 C5_1 H5_1 125.8 . . ?
C7_1 C6_1 N3_1 106.8(12) . . ?
C7_1 C6_1 H6A_1 126.6 . . ?
N3_1 C6_1 H6A_1 126.6 . . ?
C5_1 N3_1 C6_1 109.1(15) . . ?
C5_1 N3_1 C4_1 114(6) . . ?
C6_1 N3_1 C4_1 136(6) . . ?
N2_1 C4_1 N3_1 109(7) . . ?
N2_1 C4_1 H4A_1 109.9 . . ?
N3_1 C4_1 H4A_1 109.9 . . ?
N2_1 C4_1 H4B_1 109.9 . . ?
N3_1 C4_1 H4B_1 109.9 . . ?
H4A_1 C4_1 H4B_1 108.3 . . ?
C1_1 N2_1 C3_1 109.3(15) . . ?
C1_1 N2_1 C4_1 155(6) . . ?
C3_1 N2_1 C4_1 96(6) . . ?
N2_1 C1_1 N1_1 108.2(17) . . ?
N2_1 C1_1 H1_1 125.9 . . ?
N1_1 C1_1 H1_1 125.9 . . ?
C2_1 C3_1 N2_1 106.5(12) . . ?
C2_1 C3_1 H3_1 126.7 . . ?
N2_1 C3_1 H3_1 126.7 . . ?
C3_1 C2_1 N1_1 106.9(12) . . ?
C3_1 C2_1 H2_1 126.5 . . ?
N1_1 C2_1 H2_1 126.5 . . ?
C1_1 N1_1 C2_1 109.0(15) . . ?
C1_1 N1_1 C24_1 124(7) . . ?
C2_1 N1_1 C24_1 126(7) . . ?
C23_1 C24_1 N1_1 121(7) . . ?
C23_1 C24_1 H24A_1 107.1 . . ?
N1_1 C24_1 H24A_1 107.1 . . ?
C23_1 C24_1 H24B_1 107.1 . . ?
N1_1 C24_1 H24B_1 107.1 . . ?
H24A_1 C24_1 H24B_1 106.8 . . ?
N12_1 C23_1 C22_1 108(3) . . ?
N12_1 C23_1 C24_1 124(6) . . ?
C22_1 C23_1 C24_1 128(6) . . ?
C21_1 C22_1 C23_1 107(3) . . ?
C21_1 C22_1 Br2_1 127.0(19) . . ?
C23_1 C22_1 Br2_1 126.2(19) . . ?
N11_1 C21_1 C22_1 107(3) . . ?
N11_1 C21_1 C20_1 119(4) . . ?
C22_1 C21_1 C20_1 133(4) . . ?
C21_1 N11_1 N12_1 109.6(18) . . ?
C21_1 N11_1 H11_1 125.2 . . ?
N12_1 N11_1 H11_1 125.2 . . ?
C23_1 N12_1 N11_1 108.8(18) . . ?
N5_2 C9_2 C10_2 110(2) . . ?
N5_2 C9_2 C8_2 117(4) . . ?
C10_2 C9_2 C8_2 133(4) . . ?
C9_2 N5_2 N6_2 107.3(16) . . ?
C11_2 C10_2 C9_2 104(2) . . ?
C11_2 C10_2 Br1_2 129.3(17) . . ?
C9_2 C10_2 Br1_2 126.4(17) . . ?
C11_2 N6_2 N5_2 108.7(16) . . ?
C11_2 N6_2 H6_2 125.6 . . ?
N5_2 N6_2 H6_2 125.6 . . ?
N8_2 C16_2 N9_2 113(4) . . ?
N8_2 C16_2 H16A_2 109.0 . . ?
N9_2 C16_2 H16A_2 109.0 . . ?
N8_2 C16_2 H16B_2 109.0 . . ?
N9_2 C16_2 H16B_2 109.0 . . ?
H16A_2 C16_2 H16B_2 107.8 . . ?
C9_2 C8_2 N4_2 105(4) . . ?
C9_2 C8_2 H8A_2 110.7 . . ?
N4_2 C8_2 H8A_2 110.7 . . ?
C9_2 C8_2 H8B_2 110.7 . . ?
N4_2 C8_2 H8B_2 110.7 . . ?
H8A_2 C8_2 H8B_2 108.8 . . ?
N6_2 C11_2 C10_2 110(2) . . ?
N6_2 C11_2 C12_2 118(3) . . ?
C10_2 C11_2 C12_2 132(3) . . ?
C11_2 C12_2 N7_2 113(4) . . ?
C11_2 C12_2 H12A_2 109.0 . . ?
N7_2 C12_2 H12A_2 109.0 . . ?
C11_2 C12_2 H12B_2 109.0 . . ?
N7_2 C12_2 H12B_2 109.0 . . ?
H12A_2 C12_2 H12B_2 107.8 . . ?
C21_2 C20_2 N10_2 116(3) . . ?
C21_2 C20_2 H20A_2 108.2 . . ?
N10_2 C20_2 H20A_2 108.2 . . ?
C21_2 C20_2 H20B_2 108.2 . . ?
N10_2 C20_2 H20B_2 108.2 . . ?
H20A_2 C20_2 H20B_2 107.4 . . ?
C13_2 N7_2 C14_2 109.1(14) . . ?
C13_2 N7_2 C12_2 129(4) . . ?
C14_2 N7_2 C12_2 122(4) . . ?
C13_2 N8_2 C15_2 109.6(14) . . ?
C13_2 N8_2 C16_2 124(6) . . ?
C15_2 N8_2 C16_2 126(6) . . ?
N8_2 C13_2 N7_2 108.0(16) . . ?
N8_2 C13_2 H13_2 126.0 . . ?
N7_2 C13_2 H13_2 126.0 . . ?
C15_2 C14_2 N7_2 106.9(12) . . ?
C15_2 C14_2 H14_2 126.6 . . ?
N7_2 C14_2 H14_2 126.6 . . ?
C14_2 C15_2 N8_2 106.4(12) . . ?
C14_2 C15_2 H15_2 126.8 . . ?
N8_2 C15_2 H15_2 126.8 . . ?
C17_2 N10_2 C19_2 108.4(15) . . ?
C17_2 N10_2 C20_2 122(4) . . ?
C19_2 N10_2 C20_2 128(3) . . ?
C17_2 N9_2 C18_2 108.4(15) . . ?
C17_2 N9_2 C16_2 117(6) . . ?
C18_2 N9_2 C16_2 135(6) . . ?
N9_2 C17_2 N10_2 108.9(16) . . ?
N9_2 C17_2 H17_2 125.5 . . ?
N10_2 C17_2 H17_2 125.5 . . ?
C18_2 C19_2 N10_2 107.3(12) . . ?
C18_2 C19_2 H19_2 126.4 . . ?
N10_2 C19_2 H19_2 126.4 . . ?
C19_2 C18_2 N9_2 106.8(12) . . ?
C19_2 C18_2 H18_2 126.6 . . ?
N9_2 C18_2 H18_2 126.6 . . ?
C5_2 N4_2 C7_2 109.7(14) . . ?
C5_2 N4_2 C8_2 126(4) . . ?
C7_2 N4_2 C8_2 124(4) . . ?
C6_2 C7_2 N4_2 106.4(12) . . ?
C6_2 C7_2 H7_2 126.8 . . ?
N4_2 C7_2 H7_2 126.8 . . ?
N3_2 C5_2 N4_2 108.0(16) . . ?
N3_2 C5_2 H5_2 126.0 . . ?
N4_2 C5_2 H5_2 126.0 . . ?
C7_2 C6_2 N3_2 106.5(12) . . ?
C7_2 C6_2 H6A_2 126.7 . . ?
N3_2 C6_2 H6A_2 126.7 . . ?
C5_2 N3_2 C6_2 109.4(15) . . ?
C5_2 N3_2 C4_2 123(5) . . ?
C6_2 N3_2 C4_2 127(5) . . ?
N3_2 C4_2 N2_2 110(4) . . ?
N3_2 C4_2 H4A_2 109.7 . . ?
N2_2 C4_2 H4A_2 109.7 . . ?
N3_2 C4_2 H4B_2 109.7 . . ?
N2_2 C4_2 H4B_2 109.7 . . ?
H4A_2 C4_2 H4B_2 108.2 . . ?
C1_2 N2_2 C3_2 108.9(14) . . ?
C1_2 N2_2 C4_2 116(5) . . ?
C3_2 N2_2 C4_2 135(5) . . ?
N2_2 C1_2 N1_2 108.4(15) . . ?
N2_2 C1_2 H1_2 125.8 . . ?
N1_2 C1_2 H1_2 125.8 . . ?
C2_2 C3_2 N2_2 106.9(11) . . ?
C2_2 C3_2 H3_2 126.6 . . ?
N2_2 C3_2 H3_2 126.6 . . ?
C3_2 C2_2 N1_2 106.9(11) . . ?
C3_2 C2_2 H2_2 126.6 . . ?
N1_2 C2_2 H2_2 126.6 . . ?
C1_2 N1_2 C2_2 108.9(14) . . ?
C1_2 N1_2 C24_2 129(3) . . ?
C2_2 N1_2 C24_2 121(3) . . ?
C23_2 C24_2 N1_2 108(3) . . ?
C23_2 C24_2 H24A_2 110.1 . . ?
N1_2 C24_2 H24A_2 110.1 . . ?
C23_2 C24_2 H24B_2 110.1 . . ?
N1_2 C24_2 H24B_2 110.1 . . ?
H24A_2 C24_2 H24B_2 108.4 . . ?
N12_2 C23_2 C22_2 108(2) . . ?
N12_2 C23_2 C24_2 121(3) . . ?
C22_2 C23_2 C24_2 132(3) . . ?
C23_2 C22_2 C21_2 107(2) . . ?
C23_2 C22_2 Br2_2 127.2(16) . . ?
C21_2 C22_2 Br2_2 125.9(16) . . ?
N11_2 C21_2 C22_2 107(2) . . ?
N11_2 C21_2 C20_2 123(3) . . ?
C22_2 C21_2 C20_2 129(3) . . ?
C21_2 N11_2 N12_2 109.5(16) . . ?
C21_2 N11_2 H11_2 125.2 . . ?
N12_2 N11_2 H11_2 125.2 . . ?
C23_2 N12_2 N11_2 108.4(15) . . ?
F6_3 P1_3 F2_3 94.4(18) . . ?
F6_3 P1_3 F5_3 167.8(19) . . ?
F2_3 P1_3 F5_3 97.7(18) . . ?
F6_3 P1_3 F1_3 91.0(13) . . ?
F2_3 P1_3 F1_3 89.8(13) . . ?
F5_3 P1_3 F1_3 87.6(11) . . ?
F6_3 P1_3 F4_3 82.9(16) . . ?
F2_3 P1_3 F4_3 177.1(18) . . ?
F5_3 P1_3 F4_3 84.9(15) . . ?
F1_3 P1_3 F4_3 89.1(12) . . ?
F6_3 P1_3 F3_3 89.0(12) . . ?
F2_3 P1_3 F3_3 90.5(13) . . ?
F5_3 P1_3 F3_3 92.3(11) . . ?
F1_3 P1_3 F3_3 179.7(16) . . ?
F4_3 P1_3 F3_3 90.6(12) . . ?
F4_4 P1_4 F2_4 177(3) . . ?
F4_4 P1_4 F1_4 90.0(16) . . ?
F2_4 P1_4 F1_4 89.5(16) . . ?
F4_4 P1_4 F6_4 93(3) . . ?
F2_4 P1_4 F6_4 90(3) . . ?
F1_4 P1_4 F6_4 90.1(16) . . ?
F4_4 P1_4 F5_4 85(3) . . ?
F2_4 P1_4 F5_4 92(3) . . ?
F1_4 P1_4 F5_4 90.8(16) . . ?
F6_4 P1_4 F5_4 178(3) . . ?
F4_4 P1_4 F3_4 90.2(16) . . ?
F2_4 P1_4 F3_4 90.4(17) . . ?
F1_4 P1_4 F3_4 177.8(19) . . ?
F6_4 P1_4 F3_4 87.7(16) . . ?
F5_4 P1_4 F3_4 91.4(16) . . ?
F1_5 P1_5 F3_5 179(2) . . ?
F1_5 P1_5 F2_5 91.1(16) . . ?
F3_5 P1_5 F2_5 88.5(16) . . ?
F1_5 P1_5 F4_5 90.2(16) . . ?
F3_5 P1_5 F4_5 90.3(16) . . ?
F2_5 P1_5 F4_5 179(3) . . ?
F1_5 P1_5 F6_5 90.4(17) . . ?
F3_5 P1_5 F6_5 90.7(17) . . ?
F2_5 P1_5 F6_5 78(3) . . ?
F4_5 P1_5 F6_5 102(4) . . ?
F1_5 P1_5 F5_5 87.7(16) . . ?
F3_5 P1_5 F5_5 91.0(16) . . ?
F2_5 P1_5 F5_5 73(3) . . ?
F4_5 P1_5 F5_5 107(3) . . ?
F6_5 P1_5 F5_5 151(4) . . ?
F1_6 P1_6 F5_6 89.3(11) . . ?
F1_6 P1_6 F2_6 91.1(11) . . ?
F5_6 P1_6 F2_6 87.5(13) . . ?
F1_6 P1_6 F6_6 92.7(12) . . ?
F5_6 P1_6 F6_6 177.3(16) . . ?
F2_6 P1_6 F6_6 90.6(16) . . ?
F1_6 P1_6 F4_6 91.0(11) . . ?
F5_6 P1_6 F4_6 89.2(15) . . ?
F2_6 P1_6 F4_6 176.1(16) . . ?
F6_6 P1_6 F4_6 92.6(16) . . ?
F1_6 P1_6 F3_6 179.1(12) . . ?
F5_6 P1_6 F3_6 89.9(10) . . ?
F2_6 P1_6 F3_6 89.3(11) . . ?
F6_6 P1_6 F3_6 88.1(10) . . ?
F4_6 P1_6 F3_6 88.6(10) . . ?
F3_7 P1_7 F5_7 90.5(16) . . ?
F3_7 P1_7 F2_7 91.4(16) . . ?
F5_7 P1_7 F2_7 82(3) . . ?
F3_7 P1_7 F1_7 178.5(19) . . ?
F5_7 P1_7 F1_7 91.0(16) . . ?
F2_7 P1_7 F1_7 88.7(15) . . ?
F3_7 P1_7 F4_7 91.2(16) . . ?
F5_7 P1_7 F4_7 91(3) . . ?
F2_7 P1_7 F4_7 173(4) . . ?
F1_7 P1_7 F4_7 88.9(16) . . ?
F3_7 P1_7 F6_7 88.4(16) . . ?
F5_7 P1_7 F6_7 179(2) . . ?
F2_7 P1_7 F6_7 98(3) . . ?
F1_7 P1_7 F6_7 90.0(16) . . ?
F4_7 P1_7 F6_7 89(3) . . ?
F6_8 P1_8 F3_8 90.0(17) . . ?
F6_8 P1_8 F2_8 77(4) . . ?
F3_8 P1_8 F2_8 91.5(17) . . ?
F6_8 P1_8 F5_8 165(5) . . ?
F3_8 P1_8 F5_8 89.8(16) . . ?
F2_8 P1_8 F5_8 117(4) . . ?
F6_8 P1_8 F1_8 90.3(17) . . ?
F3_8 P1_8 F1_8 179(2) . . ?
F2_8 P1_8 F1_8 89.4(17) . . ?
F5_8 P1_8 F1_8 89.8(16) . . ?
F6_8 P1_8 F4_8 81(4) . . ?
F3_8 P1_8 F4_8 89.5(17) . . ?
F2_8 P1_8 F4_8 159(4) . . ?
F5_8 P1_8 F4_8 84(4) . . ?
F1_8 P1_8 F4_8 89.7(17) . . ?

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 2374511'
loop_
_audit_author_name
_audit_author_address
'Julian Zuber'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2024-10-10 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

#===============================================================================

# start Validation Reply Form
_vrf_PLAT020_I                   
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.206 Report
RESPONSE: The Rint value is acceptable for electron diffraction data.
;
_vrf_PLAT082_I                   
;
PROBLEM: High R1 Value ..................................       0.26 Report
RESPONSE: The R1 value is acceptable for electron diffraction data.
;
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.62 Report  
RESPONSE: The wR2 value is acceptable for electron diffraction data.
;
_vrf_PLAT341_I                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.06 Ang.  
RESPONSE: This is due to the generally lower quality of electron diffraction
 data as compared to X-ray diffraction data regarding resolution,
 completeness, redundancy, and accuracy of unit cell parameters.
;
_vrf_PLAT601_I                   
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        179 Ang**3
RESPONSE: As the measurements were performed under high vacuum solvent
 molecules were removed from the voids (except for a small amount of
 residuals that could not be properly modelled).
;
_vrf_THETM01_I                   
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.4530
RESPONSE: The resolution of electron diffraction data is commonly lower than
 for X-ray diffraction data.
;
# end Validation Reply Form

# 5. CHEMICAL DATA

_chemical_name_systematic        
'Calix[4]imidazolium[2]dibromo-pyrazole tetrakis(triflate)'
_chemical_name_common            H6LBr2(OTf)4
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 Br2 N12, 4(C F3 O3 S)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C28 H26 Br2 F12 N12 O12 S4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1238.65
_chemical_compound_source        'see text'


#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_Int_Tables_number      61

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,1/2+y,1/2-z
5 -x,-y,-z
6 1/2+x,y,1/2-z
7 1/2-x,1/2+y,z
8 x,1/2-y,1/2+z

_cell_length_a                   12.8(3)
_cell_length_b                   19.7(4)
_cell_length_c                   20.2(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5094
_cell_formula_units_Z            4
_cell_measurement_temperature    293
_cell_measurement_reflns_used    123
_cell_measurement_theta_min      0.2935
_cell_measurement_theta_max      0.5563
_cell_special_details            
;
;

_exptl_crystal_description       nanocrystals
_exptl_crystal_colour            colourless

_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             0
_exptl_absorpt_coefficient_mu    ?
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2413
_exptl_absorpt_correction_T_max  0.5321
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker 2016)'
_exptl_absorpt_special_details   ?

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
;
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     0.02851
_diffrn_radiation_type           electron
_diffrn_radiation_source         LaB~6~
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       'ELDICO ED-1'
_diffrn_measurement_device_type  'electron diffractometer'
_diffrn_measurement_method       'continuous rotation 3D ED'
_diffrn_detector                 'Dectris QUADRO'
_diffrn_detector_area_resol_mean 13.33

# number of measured reflections (redundant set)
_diffrn_reflns_number            5874
_diffrn_reflns_av_R_equivalents  0.2062
_diffrn_reflns_av_unetI/netI     0.2750
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         0.09
_diffrn_reflns_theta_max         0.74
_diffrn_reflns_theta_full        0.74
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measured_fraction_theta_full 0.787
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             1578
# number of observed reflections (> n sig(I))
_reflns_number_gt                818
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Eldix (ELDICO 2023)'
_computing_cell_refinement       'SAINT (Bruker 2019)'
_computing_data_reduction        'SAINT (Bruker 2019)'
_computing_structure_solution    'SHELXD (Sheldrick 2008)'
_computing_structure_refinement  
'SHELXL (Sheldrick 2015), ShelXle (Huebschle 2011)'
_computing_molecular_graphics    'Mercury (Macrae 2008)'
_computing_publication_material  'EnCIFer (Allen 2004), PLATON (Spek 2009)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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.
 Electron scattering factors (Peng 1999).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.4769P)²+2.1600P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     XD
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom


_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         1578
_refine_ls_number_parameters     317
_refine_ls_number_restraints     499
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.3074
_refine_ls_R_factor_gt           0.2586
_refine_ls_wR_factor_ref         0.6211
_refine_ls_wR_factor_gt          0.5711
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      0.944
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.056

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br Uani 0.6314(10) 0.5782(5) 0.7316(9) 1.000 0.138(7) d U . .
S1 S Uani 0.4636(9) 0.7912(6) 0.3679(10) 1.000 0.094(7) d DU . .
S2 S Uani 0.9150(10) 0.6005(9) 0.4088(12) 1.000 0.140(8) d DU . .
N1 N Uani 0.7265(18) 0.6324(13) 0.555(2) 1.000 0.101(9) d U . .
F1 F Uani 0.6217(19) 0.7179(13) 0.3938(19) 1.000 0.112(9) d DU . .
N2 N Uani 0.648(3) 0.6754(14) 0.564(3) 1.000 0.113(12) d U . .
F2 F Uani 0.620(2) 0.7539(15) 0.301(2) 1.000 0.121(9) d DU . .
N3 N Uani 0.7933(15) 0.4732(10) 0.5952(19) 1.000 0.073(8) d DU . .
F3 F Uani 0.517(2) 0.6712(14) 0.328(2) 1.000 0.126(12) d DU . .
N4 N Uani 0.7794(18) 0.3774(12) 0.5443(18) 1.000 0.080(8) d DU . .
N5 N Uani 0.719(2) 0.3334(13) 0.4432(18) 1.000 0.095(9) d DU . .
N6 N Uani 0.5845(17) 0.3141(12) 0.381(2) 1.000 0.093(9) d DU . .
O1 O Uani 0.408(2) 0.8042(15) 0.3114(17) 1.000 0.123(10) d DU . .
C1 C Uani 0.655(2) 0.6137(13) 0.649(2) 1.000 0.098(9) d U . .
C2 C Uani 0.740(2) 0.5953(14) 0.606(2) 1.000 0.092(9) d U . .
O2 O Uani 0.5231(17) 0.8496(11) 0.3856(18) 1.000 0.101(8) d DU . .
O3 O Uani 0.409(2) 0.7571(13) 0.4182(18) 1.000 0.118(9) d DU . .
C3 C Uani 0.605(2) 0.6636(15) 0.612(3) 1.000 0.098(9) d U . .
C4 C Uani 0.8196(18) 0.5407(10) 0.609(2) 1.000 0.093(8) d DU . .
C5 C Uani 0.8154(16) 0.4435(12) 0.539(2) 1.000 0.078(8) d U . .
C6 C Uani 0.746(2) 0.4319(14) 0.639(2) 1.000 0.102(9) d U . .
C7 C Uani 0.7360(19) 0.3668(14) 0.603(2) 1.000 0.087(9) d U . .
C8 C Uani 0.7914(19) 0.3284(12) 0.4951(14) 1.000 0.085(8) d DU . .
C9 C Uani 0.625(2) 0.3016(14) 0.440(2) 1.000 0.096(9) d U . .
C10 C Uani 0.739(2) 0.3621(17) 0.381(3) 1.000 0.116(10) d U . .
C11 C Uani 0.656(3) 0.3503(18) 0.348(3) 1.000 0.126(11) d U . .
C12 C Uani 0.4867(16) 0.2900(12) 0.361(2) 1.000 0.091(12) d DU . .
F4 F Uani 0.879(3) 0.664(2) 0.304(3) 1.000 0.202(14) d DU . .
F5 F Uani 0.952(3) 0.575(2) 0.290(2) 1.000 0.210(14) d DU . .
F6 F Uani 0.786(3) 0.577(2) 0.313(3) 1.000 0.202(13) d DU . .
O4 O Uani 1.009(2) 0.6348(16) 0.409(2) 1.000 0.156(12) d DU . .
O5 O Uani 0.927(3) 0.5318(16) 0.427(3) 1.000 0.175(13) d DU . .
O6 O Uani 0.831(2) 0.6398(17) 0.434(2) 1.000 0.168(13) d DU . .
C13 C Uani 0.564(2) 0.7232(16) 0.342(2) 1.000 0.112(9) d DU . .
C14 C Uani 0.874(3) 0.601(2) 0.316(2) 1.000 0.191(13) d DU . .
H1 H Uiso 0.77011 0.62933 0.51299 1.000 0.1190 c RU . .
H4A H Uiso 0.88186 0.55478 0.57456 1.000 0.1100 c RU . .
H4B H Uiso 0.85340 0.54174 0.65820 1.000 0.1100 c RU . .
H5 H Uiso 0.85422 0.46601 0.49711 1.000 0.0940 c RU . .
H6 H Uiso 0.72216 0.44344 0.68911 1.000 0.1220 c RU . .
H7 H Uiso 0.70059 0.32057 0.62072 1.000 0.1050 c RU . .
H8A H Uiso 0.78403 0.27842 0.51766 1.000 0.1020 c RU . .
H8B H Uiso 0.87020 0.33234 0.47479 1.000 0.1020 c RU . .
H9 H Uiso 0.58998 0.27149 0.47876 1.000 0.1140 c RU . .
H10 H Uiso 0.80849 0.38832 0.36510 1.000 0.1370 c RU . .
H11 H Uiso 0.64478 0.36820 0.29836 1.000 0.1520 c RU . .
H12A H Uiso 0.47616 0.23862 0.37959 1.000 0.1080 c RU . .
H12B H Uiso 0.48343 0.28809 0.30716 1.000 0.1080 c RU . .


#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C1 1.83(6) . . yes
S1 O1 1.37(5) . . yes
S1 O2 1.43(4) . . yes
S1 O3 1.40(5) . . yes
S1 C13 1.93(6) . . yes
S2 O4 1.38(4) . . yes
S2 O5 1.41(5) . . yes
S2 O6 1.42(5) . . yes
S2 C14 1.95(7) . . yes
N1 N2 1.33(5) . . yes
N1 C2 1.28(6) . . yes
F1 C13 1.29(6) . . yes
N2 C3 1.14(8) . . yes
F2 C13 1.25(6) . . yes
F3 C13 1.22(5) . . yes
N3 C6 1.35(5) . . yes
N3 C4 1.40(4) . . yes
N3 C5 1.31(6) . . yes
N4 C5 1.39(5) . . yes
N4 C7 1.33(6) . . yes
N4 C8 1.39(5) . . yes
N5 C8 1.40(5) . . yes
N5 C10 1.40(7) . . yes
N5 C9 1.36(5) . . yes
N6 C11 1.34(6) . . yes
N6 C12 1.40(5) . . yes
N6 C9 1.32(6) . . yes
C1 C3 1.39(6) . . no
N1 H1 1.0200 . . no
C1 C2 1.44(6) . . no
C2 C4 1.48(5) . . no
C3 C12 1.59(6) . 5_666 no
C6 C7 1.48(6) . . no
C10 C11 1.28(7) . . no
F4 C14 1.27(6) . . yes
C4 H4B 1.0800 . . no
C4 H4A 1.0900 . . no
C5 H5 1.0800 . . no
F5 C14 1.24(6) . . yes
C6 H6 1.0800 . . no
F6 C14 1.22(6) . . yes
C7 H7 1.0800 . . no
C8 H8B 1.0900 . . no
C8 H8A 1.0900 . . no
C9 H9 1.0800 . . no
C10 H10 1.0800 . . no
C11 H11 1.0700 . . no
C12 H12B 1.0900 . . no
C12 H12A 1.0900 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 C13 105(2) . . . yes
O2 S1 O3 118(3) . . . yes
O2 S1 C13 106(2) . . . yes
O3 S1 C13 101(2) . . . yes
O1 S1 O2 110(2) . . . yes
O1 S1 O3 116(2) . . . yes
O4 S2 O6 113(3) . . . yes
O5 S2 C14 107(3) . . . yes
O4 S2 C14 104(2) . . . yes
O5 S2 O6 121(3) . . . yes
O4 S2 O5 112(2) . . . yes
O6 S2 C14 98(2) . . . yes
N2 N1 C2 111(4) . . . yes
N1 N2 C3 111(4) . . . yes
C4 N3 C6 124(4) . . . yes
C5 N3 C6 113(3) . . . yes
C4 N3 C5 123(3) . . . yes
C7 N4 C8 125(3) . . . yes
C5 N4 C8 124(3) . . . yes
C5 N4 C7 111(3) . . . yes
C8 N5 C9 126(3) . . . yes
C9 N5 C10 108(3) . . . yes
C8 N5 C10 125(3) . . . yes
C9 N6 C12 123(3) . . . yes
C9 N6 C11 106(3) . . . yes
C11 N6 C12 131(4) . . . yes
Br1 C1 C3 133(3) . . . yes
N2 N1 H1 125.00 . . . no
C2 C1 C3 102(4) . . . no
Br1 C1 C2 125(2) . . . yes
C2 N1 H1 124.00 . . . no
N1 C2 C1 104(3) . . . yes
N1 C2 C4 123(3) . . . yes
C1 C2 C4 133(3) . . . no
N2 C3 C1 112(3) . . . yes
C1 C3 C12 124(5) . . 5_666 no
N2 C3 C12 122(4) . . 5_666 yes
N3 C4 C2 121(3) . . . yes
N3 C5 N4 106(3) . . . yes
N3 C6 C7 104(3) . . . yes
N4 C7 C6 106(3) . . . yes
N4 C8 N5 114(3) . . . yes
N5 C9 N6 108(3) . . . yes
N5 C10 C11 104(4) . . . yes
N6 C11 C10 114(5) . . . yes
N6 C12 C3 112(3) . . 5_666 yes
C2 C4 H4A 107.00 . . . no
C2 C4 H4B 107.00 . . . no
H4A C4 H4B 107.00 . . . no
N3 C4 H4A 107.00 . . . no
N3 C4 H4B 107.00 . . . no
N3 C5 H5 127.00 . . . no
N4 C5 H5 127.00 . . . no
N3 C6 H6 128.00 . . . no
C7 C6 H6 128.00 . . . no
C6 C7 H7 127.00 . . . no
N4 C7 H7 127.00 . . . no
N5 C8 H8B 109.00 . . . no
H8A C8 H8B 108.00 . . . no
N4 C8 H8A 109.00 . . . no
N4 C8 H8B 109.00 . . . no
N5 C8 H8A 109.00 . . . no
N6 C9 H9 126.00 . . . no
N5 C9 H9 126.00 . . . no
C11 C10 H10 128.00 . . . no
N5 C10 H10 128.00 . . . no
N6 C11 H11 123.00 . . . no
C10 C11 H11 123.00 . . . no
C3 C12 H12A 109.00 5_666 . . no
C3 C12 H12B 110.00 5_666 . . no
N6 C12 H12A 109.00 . . . no
N6 C12 H12B 110.00 . . . no
H12A C12 H12B 108.00 . . . no
F2 C13 F3 122(4) . . . yes
S1 C13 F1 103(3) . . . yes
S1 C13 F2 103(3) . . . yes
S1 C13 F3 109(3) . . . yes
F1 C13 F2 104(3) . . . yes
F1 C13 F3 114(3) . . . yes
S2 C14 F4 100(4) . . . yes
S2 C14 F5 101(3) . . . yes
S2 C14 F6 107(4) . . . yes
F4 C14 F5 107(4) . . . yes
F4 C14 F6 115(4) . . . yes
F5 C14 F6 124(5) . . . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 C13 F1 57(3) . . . . no
O2 S1 C13 F2 -51(3) . . . . no
O2 S1 C13 F3 178(3) . . . . no
O3 S1 C13 F1 -66(3) . . . . no
O3 S1 C13 F2 -175(3) . . . . no
O3 S1 C13 F3 54(4) . . . . no
O1 S1 C13 F2 65(3) . . . . no
O1 S1 C13 F3 -66(3) . . . . no
O1 S1 C13 F1 173(2) . . . . no
O4 S2 C14 F6 -174(3) . . . . no
O5 S2 C14 F5 -63(3) . . . . no
O5 S2 C14 F6 68(4) . . . . no
O5 S2 C14 F4 -172(3) . . . . no
O4 S2 C14 F4 -54(3) . . . . no
O4 S2 C14 F5 55(3) . . . . no
O6 S2 C14 F6 -57(3) . . . . no
O6 S2 C14 F4 62(3) . . . . no
O6 S2 C14 F5 172(3) . . . . no
C2 N1 N2 C3 -8(5) . . . . no
N2 N1 C2 C1 5(4) . . . . no
N2 N1 C2 C4 178(3) . . . . no
N1 N2 C3 C12 175(3) . . . 5_666 no
N1 N2 C3 C1 7(5) . . . . no
C6 N3 C4 C2 -80(5) . . . . no
C4 N3 C5 N4 179(2) . . . . no
C5 N3 C4 C2 103(4) . . . . no
C5 N3 C6 C7 -1(3) . . . . no
C6 N3 C5 N4 1(3) . . . . no
C4 N3 C6 C7 -179(2) . . . . no
C7 N4 C8 N5 103(3) . . . . no
C8 N4 C5 N3 -178(2) . . . . no
C5 N4 C8 N5 -80(3) . . . . no
C7 N4 C5 N3 0(3) . . . . no
C8 N4 C7 C6 177(2) . . . . no
C5 N4 C7 C6 -1(3) . . . . no
C8 N5 C9 N6 -174(3) . . . . no
C9 N5 C8 N4 -91(3) . . . . no
C9 N5 C10 C11 4(4) . . . . no
C10 N5 C9 N6 -5(3) . . . . no
C8 N5 C10 C11 174(3) . . . . no
C10 N5 C8 N4 101(4) . . . . no
C12 N6 C9 N5 -179(3) . . . . no
C9 N6 C12 C3 82(4) . . . 5_666 no
C11 N6 C9 N5 3(4) . . . . no
C11 N6 C12 C3 -101(5) . . . 5_666 no
C9 N6 C11 C10 0(4) . . . . no
C12 N6 C11 C10 -178(3) . . . . no
C2 C1 C3 N2 -4(4) . . . . no
C2 C1 C3 C12 -171(3) . . . 5_666 no
Br1 C1 C2 N1 -179(2) . . . . no
C3 C1 C2 C4 -173(3) . . . . no
Br1 C1 C3 N2 174(3) . . . . no
C3 C1 C2 N1 -1(3) . . . . no
Br1 C1 C3 C12 7(5) . . . 5_666 no
Br1 C1 C2 C4 9(5) . . . . no
N1 C2 C4 N3 -96(4) . . . . no
C1 C2 C4 N3 74(5) . . . . no
N2 C3 C12 N6 94(4) . . 5_666 5_666 no
C1 C3 C12 N6 -99(4) . . 5_666 5_666 no
N3 C6 C7 N4 1(3) . . . . no
N5 C10 C11 N6 -3(4) . . . . no

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
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
N1 H1 O6 1.0200 1.7900 2.79(8) 168.00 . yes
C5 H5 O5 1.0800 2.1300 3.19(10) 167.00 . yes
C6 H6 F6 1.0800 2.5400 3.54(11) 154.00 2_665 yes
C7 H7 O3 1.0800 2.2200 3.10(8) 137.00 5_666 yes
C8 H8A N2 1.0900 2.4000 3.41(9) 154.00 7_645 yes
C8 H8B O2 1.0900 2.2900 3.27(9) 149.00 7_645 yes
C9 H9 O3 1.0800 2.1600 3.12(9) 147.00 5_666 yes
C10 H10 Br1 1.0800 2.8800 3.64(10) 128.00 2_664 yes
C10 H10 O2 1.0800 2.3200 3.06(8) 124.00 7_645 yes
C12 H12A O4 1.0900 2.1400 3.21(9) 167.00 7_645 yes



#===END
####################################################################### 
# 
# 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_heial14_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 2374513'
loop_
_audit_author_name
_audit_author_address
'Julian Zuber'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2024-11-08 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V144 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;

loop_
_publ_author_phone
08928954134
08928954134
08928954134
0498275218
''
'089 289 54101'
_platon_squeeze_details          
;Solvent Accessible Volume =      3747
Electrons Found in S.A.V. =      1583
This correponds to about 9 solvent molecules (i.e. diethylether) ?in the asymm. unit
;
_platon_squeeze_void_probe_radius 1.20
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
Bis(calix[4]imidazolium[2]dibromo-pyrazolato)octakisgold(I)tetrakis(hexafluorophosphate)
_chemical_name_common            Au8(LBr2)2(PF6)4
_chemical_formula_sum            'C52 H46 Au8 Br4 F24 N26 P4 [+ 9(C4 H10 O)]'
_chemical_formula_moiety         
'C48 H40 Au8 Br4 N24, 4(F6 P), 2(C2 H3 N) [+ 9(C4 H10 O)]'
_chemical_formula_weight         3510.40
_chemical_melting_point          ?
_chemical_absolute_configuration ?
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
_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'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   14.3499(8)
_vrf_ABSMU01_heial14_0m_sq       
;PROBLEM: The ratio of given/expected absorption coefficient lies
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_CHEMW01_heial14_0m_sq       
;PROBLEM: The ratio of given/expected molecular weight as calculated
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMN02_heial14_0m_sq       
;PROBLEM: The minimum difference density is < -0.1*ZMAX*2.00
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMN03_heial14_0m_sq       
;PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMX02_heial14_0m_sq       
;PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_PLAT250_heial14_0m_sq       
;PROBLEM: Large U3/U1 Ratio for <U(i,j)> Tensor(Resd    2)        2.4 Note  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this meaningfully have been unsuccessful due 
to the lack of electron density on all light atoms of the cation. Additional min
 twin domain could not be found by CELLNOW (APEX5) or Platon.
;
_vrf_PLAT342_heial14_0m_sq       
;PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03154 Ang.  
RESPONSE: Whole molecule disorder and many heavy atoms.
;
_vrf_PLAT364_heial14_0m_sq       
;PROBLEM: Short  C(sp3)-C(sp)  Bond  C1M      - C2M      .       1.31 Ang.  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this meaningfully have been unsuccessful due 
to the lack of electron density on all light atoms of the cation. Additional min
 twin domain could not be found by CELLNOW (APEX5) or Platon.
;
_vrf_PLAT971_heial14_0m_sq       
;PROBLEM: Check Calcd Resid. Dens.  1.51Ang From Au1             2.50 eA-3  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this meaningfully have been unsuccessful due 
to the lack of electron density on all light atoms of the cation. Additional min
 twin domain could not be found by CELLNOW (APEX5) or Platon.
;
_vrf_PLAT972_heial14_0m_sq       
;PROBLEM: Check Calcd Resid. Dens.  1.58Ang From Au4            -2.81 eA-3  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this meaningfully have been unsuccessful due 
to the lack of electron density on all light atoms of the cation. Additional min
 twin domain could not be found by CELLNOW (APEX5) or Platon.
;
_vrf_PLAT977_heial14_0m_sq       
;PROBLEM: Check Negative Difference Density on H2MB      .      -0.43 eA-3  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this meaningfully have been unsuccessful due 
to the lack of electron density on all light atoms of the cation. Additional min
 twin domain could not be found by CELLNOW (APEX5) or Platon.
;
_vrf_STRVA01_heial14_0m_sq       
;PROBLEM: Flack test results are ambiguous.
RESPONSE: Since the compound is not chiral, the determination of the Flack 
parameter in this case is arbitrary.
;
_cell_length_b                   14.3499(8)
_cell_length_c                   51.556(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10616.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9218
_cell_measurement_theta_min      2.8165
_cell_measurement_theta_max      25.683
_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_F_000             6352
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    12.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'TWINABS 2012/1 (Bruker, 2012)'
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;Diffractometer operator             J. Zuber
scanspeed                           1-10 s per frame
dx                                  100 mm
12109 frames measured in 22 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      123(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'TXS rotating anode'
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           50.0
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_detector_area_resol_mean 16
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            231404
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_theta_min         2.007
_diffrn_reflns_theta_max         25.760
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_limit_l_max       62
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10144
_reflns_number_gt                9304
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_max     0.996
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker BIS V6.2.4/2016-09-30'
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_reduction        'SAINT V8.40A'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL (Sheldrick, 2015), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0118P)²+347.7684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         10144
_refine_ls_number_parameters     599
_refine_ls_number_restraints     1354
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1080
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.197
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

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'
P P 0.1023 0.0942 '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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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
Au2 Au 0.75462(6) 0.39962(6) 0.48222(2) 0.02336(17) Uani 1 1 d . U . . .
P1 P 1.1492(6) 0.9733(6) 0.41304(19) 0.067(2) Uani 1 1 d . U . . .
F1 F 1.0673(14) 0.9442(18) 0.3931(5) 0.096(5) Uani 1 1 d . U . . .
F1A F 1.1488(16) 1.0775(13) 0.4025(4) 0.090(5) Uani 1 1 d . U . . .
F1B F 1.2334(15) 1.0028(15) 0.4337(5) 0.089(5) Uani 1 1 d . U . . .
F1C F 1.1488(11) 0.8696(11) 0.4233(3) 0.062(4) Uani 1 1 d . U . . .
F1D F 1.0713(14) 1.0009(15) 0.4343(5) 0.086(5) Uani 1 1 d . U . . .
F1E F 1.2273(14) 0.9435(16) 0.3919(4) 0.089(5) Uani 1 1 d . U . . .
Au3 Au 0.90321(6) 0.54526(6) 0.51216(2) 0.02213(17) Uani 1 1 d . U . . .
Au4 Au 0.90313(6) 0.75446(6) 0.51384(2) 0.02226(17) Uani 1 1 d . U . . .
Br1 Br 0.98122(19) 0.66450(19) 0.40249(4) 0.0438(6) Uani 1 1 d . U . . .
Br2 Br 0.6646(2) 0.3084(2) 0.59308(4) 0.0486(7) Uani 1 1 d . U . . .
C4 C 0.5165(15) 0.3921(17) 0.4033(4) 0.030(3) Uani 1 1 d . U . . .
H4 H 0.540546 0.379203 0.386504 0.036 Uiso 1 1 calc R U . . .
C5 C 0.6436(15) 0.3184(13) 0.4301(4) 0.023(3) Uani 1 1 d . U . . .
H5A H 0.642689 0.263685 0.418426 0.027 Uiso 1 1 calc R U . . .
H5B H 0.643699 0.295131 0.448178 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7870(13) 0.4009(14) 0.4449(4) 0.020(3) Uani 1 1 d . U . . .
C7 C 0.7713(15) 0.3845(15) 0.4016(4) 0.028(3) Uani 1 1 d . U . . .
H7 H 0.747508 0.366005 0.385162 0.034 Uiso 1 1 calc R U . . .
C8 C 0.8493(18) 0.4274(15) 0.4058(4) 0.030(3) Uani 1 1 d . U . . .
H8 H 0.890967 0.448516 0.392698 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9428(15) 0.4770(14) 0.4454(4) 0.023(3) Uani 1 1 d . U . . .
H9A H 0.998169 0.469995 0.434076 0.028 Uiso 1 1 calc R U . . .
H9B H 0.954508 0.441676 0.461519 0.028 Uiso 1 1 calc R U . . .
C10 C 0.9305(14) 0.5770(14) 0.4518(4) 0.022(3) Uani 1 1 d . U . . .
C11 C 0.9452(14) 0.6613(15) 0.4374(3) 0.025(3) Uani 1 1 d . U . . .
C12 C 0.9304(15) 0.7357(15) 0.4539(3) 0.024(3) Uani 1 1 d . U . . .
C13 C 0.9422(15) 0.8333(15) 0.4488(4) 0.026(4) Uani 1 1 d . U . . .
H13A H 0.998236 0.841612 0.437862 0.031 Uiso 1 1 calc R U . . .
H13B H 0.953826 0.865552 0.465477 0.031 Uiso 1 1 calc R U . . .
C14 C 0.5799(14) 0.3635(15) 0.5438(4) 0.024(3) Uani 1 1 d . U . . .
C15 C 0.6574(15) 0.3475(16) 0.5582(3) 0.027(3) Uani 1 1 d . U . . .
C16 C 0.7337(14) 0.3657(15) 0.5425(4) 0.024(3) Uani 1 1 d . U . . .
C17 C 0.8333(13) 0.3533(16) 0.5471(3) 0.023(3) Uani 1 1 d . U . . .
H17A H 0.865044 0.343915 0.530236 0.028 Uiso 1 1 calc R U . . .
H17B H 0.842685 0.296221 0.557562 0.028 Uiso 1 1 calc R U . . .
C18 C 0.9087(15) 0.5061(14) 0.5492(4) 0.023(3) Uani 1 1 d . U . . .
C19 C 0.8939(17) 0.4345(15) 0.5872(4) 0.031(3) Uani 1 1 d . U . . .
H19 H 0.877534 0.387762 0.599412 0.037 Uiso 1 1 calc R U . . .
C20 C 0.9388(17) 0.5174(16) 0.5924(4) 0.033(4) Uani 1 1 d . U . . .
H20 H 0.959242 0.540051 0.608727 0.040 Uiso 1 1 calc R U . . .
C21 C 1.0015(14) 0.6451(17) 0.5650(4) 0.028(3) Uani 1 1 d . U . . .
H21A H 1.025835 0.647965 0.547017 0.034 Uiso 1 1 calc R U . . .
H21B H 1.055467 0.643251 0.576909 0.034 Uiso 1 1 calc R U . . .
C22 C 0.9105(15) 0.7848(15) 0.5515(4) 0.024(3) Uani 1 1 d . U . . .
C23 C 0.9394(18) 0.7733(17) 0.5937(4) 0.036(4) Uani 1 1 d . U . . .
H23 H 0.961716 0.750095 0.609789 0.043 Uiso 1 1 calc R U . . .
C24 C 0.8958(16) 0.8542(19) 0.5904(4) 0.034(3) Uani 1 1 d . U . . .
H24 H 0.879674 0.897829 0.603477 0.041 Uiso 1 1 calc R U . . .
N1 N 0.4317(12) 0.4389(13) 0.4354(3) 0.027(3) Uani 1 1 d . U . . .
N2 N 0.5602(12) 0.3723(12) 0.4259(3) 0.025(3) Uani 1 1 d . U . . .
N3 N 0.7283(12) 0.3704(12) 0.4256(3) 0.024(3) Uani 1 1 d . U . . .
N4 N 0.8626(12) 0.4377(12) 0.4323(3) 0.023(3) Uani 1 1 d . U . . .
N5 N 0.9060(11) 0.6071(12) 0.4757(3) 0.019(2) Uani 1 1 d . U . . .
N6 N 0.9076(12) 0.7015(12) 0.4772(3) 0.022(3) Uani 1 1 d . U . . .
N7 N 0.6073(12) 0.3874(11) 0.5198(3) 0.021(3) Uani 1 1 d . U . . .
N8 N 0.6988(12) 0.3877(12) 0.5186(3) 0.021(3) Uani 1 1 d . U . . .
N9 N 0.8769(12) 0.4321(12) 0.5605(3) 0.026(3) Uani 1 1 d . U . . .
N10 N 0.9476(13) 0.5607(12) 0.5681(3) 0.025(3) Uani 1 1 d . U . . .
N11 N 0.9473(13) 0.7285(13) 0.5701(3) 0.027(3) Uani 1 1 d . U . . .
N12 N 0.8785(11) 0.8623(13) 0.5642(3) 0.024(3) Uani 1 1 d . U . . .
N1M N 1.1572(16) 0.7931(15) 0.5534(4) 0.043(4) Uani 1 1 d . U . . .
C1M C 1.1645(15) 0.857(2) 0.5679(5) 0.043(5) Uani 1 1 d . U . . .
C2M C 1.167(2) 0.921(2) 0.5859(7) 0.070(8) Uani 1 1 d . U . . .
H2MA H 1.188204 0.979886 0.578288 0.105 Uiso 1 1 calc R U . . .
H2MB H 1.211129 0.901857 0.599528 0.105 Uiso 1 1 calc R U . . .
H2MC H 1.105199 0.928906 0.593402 0.105 Uiso 1 1 calc R U . . .
Au1 Au 0.54393(6) 0.39861(6) 0.48384(2) 0.02393(18) Uani 1 1 d . U . . .
C1 C 0.3501(18) 0.4776(15) 0.4491(4) 0.030(4) Uani 1 1 d . U . . .
H1A H 0.339124 0.441234 0.465165 0.036 Uiso 1 1 calc R U . . .
H1B H 0.294300 0.471236 0.437987 0.036 Uiso 1 1 calc R U . . .
C2 C 0.5041(14) 0.4001(15) 0.4468(4) 0.022(3) Uani 1 1 d . U . . .
C3 C 0.4360(15) 0.4319(17) 0.4081(4) 0.030(3) Uani 1 1 d . U . . .
H3 H 0.390599 0.451699 0.395853 0.037 Uiso 1 1 calc R U . . .
P1_1 P 1.1435(13) 0.6522(12) 0.6420(3) 0.034(2) Uani 0.529(16) 1 d D U P A 1
F1_1 F 1.144(2) 0.6171(19) 0.6707(4) 0.053(5) Uani 0.529(16) 1 d D U P A 1
F2_1 F 1.092(2) 0.5621(17) 0.6331(5) 0.062(5) Uani 0.529(16) 1 d D U P A 1
F3_1 F 1.142(2) 0.6874(18) 0.6129(3) 0.050(5) Uani 0.529(16) 1 d D U P A 1
F4_1 F 1.186(2) 0.7466(17) 0.6510(5) 0.057(5) Uani 0.529(16) 1 d D U P A 1
F5_1 F 1.0458(17) 0.699(2) 0.6462(5) 0.054(5) Uani 0.529(16) 1 d D U P A 1
F6_1 F 1.2405(16) 0.610(2) 0.6363(5) 0.049(5) Uani 0.529(16) 1 d D U P A 1
P1_2 P 1.1444(14) 0.6495(13) 0.6415(3) 0.035(2) Uani 0.471(16) 1 d D U P A 2
F1_2 F 1.153(2) 0.5673(17) 0.6611(5) 0.051(5) Uani 0.471(16) 1 d D U P A 2
F2_2 F 1.164(3) 0.7214(19) 0.6637(5) 0.052(5) Uani 0.471(16) 1 d D U P A 2
F3_2 F 1.138(2) 0.7324(18) 0.6216(5) 0.058(5) Uani 0.471(16) 1 d D U P A 2
F4_2 F 1.140(3) 0.5781(19) 0.6183(5) 0.062(5) Uani 0.471(16) 1 d D U P A 2
F5_2 F 1.2523(15) 0.653(2) 0.6384(7) 0.047(5) Uani 0.471(16) 1 d D U P A 2
F6_2 F 1.0354(15) 0.643(3) 0.6434(7) 0.053(5) Uani 0.471(16) 1 d D U P A 2


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
Au2 C6 1.979(19) . ?
Au2 N8 2.048(16) . ?
Au2 Au1 3.0246(11) . ?
Au2 Au3 3.3610(11) . ?
P1 F1C 1.580(17) . ?
P1 F1A 1.590(18) . ?
P1 F1D 1.62(2) . ?
P1 F1 1.62(2) . ?
P1 F1E 1.62(2) . ?
P1 F1B 1.67(2) . ?
Au3 C18 1.993(19) . ?
Au3 N5 2.079(15) . ?
Au3 Au4 3.0032(11) . ?
Au4 C22 1.995(19) . ?
Au4 N6 2.039(15) . ?
Au4 Au4 3.3376(16) 7_556 ?
Br1 C11 1.874(18) . ?
Br2 C15 1.889(18) . ?
C4 C3 1.31(3) . ?
C4 N2 1.35(3) . ?
C4 H4 0.9500 . ?
C5 N2 1.44(3) . ?
C5 N3 1.44(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N4 1.37(3) . ?
C6 N3 1.37(3) . ?
C7 C8 1.30(3) . ?
C7 N3 1.40(3) . ?
C7 H7 0.9500 . ?
C8 N4 1.39(3) . ?
C8 H8 0.9500 . ?
C9 N4 1.45(3) . ?
C9 C10 1.48(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N5 1.35(2) . ?
C10 C11 1.44(3) . ?
C11 C12 1.38(3) . ?
C12 N6 1.34(2) . ?
C12 C13 1.43(3) . ?
C13 N12 1.48(3) 7_556 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N7 1.35(2) . ?
C14 C15 1.35(3) . ?
C14 C1 1.52(3) 7_556 ?
C15 C16 1.39(3) . ?
C16 N8 1.36(2) . ?
C16 C17 1.46(3) . ?
C17 N9 1.47(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 N9 1.29(3) . ?
C18 N10 1.37(3) . ?
C19 C20 1.38(3) . ?
C19 N9 1.40(2) . ?
C19 H19 0.9500 . ?
C20 N10 1.40(3) . ?
C20 H20 0.9500 . ?
C21 N10 1.45(3) . ?
C21 N11 1.45(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N11 1.36(3) . ?
C22 N12 1.37(3) . ?
C23 C24 1.33(4) . ?
C23 N11 1.38(3) . ?
C23 H23 0.9500 . ?
C24 N12 1.38(2) . ?
C24 H24 0.9500 . ?
N1 C2 1.32(3) . ?
N1 C3 1.41(3) . ?
N1 C1 1.48(3) . ?
N2 C2 1.40(3) . ?
N5 N6 1.36(2) . ?
N7 N8 1.31(2) . ?
N7 Au1 2.070(16) . ?
N1M C1M 1.18(3) . ?
C1M C2M 1.31(4) . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
Au1 C2 1.992(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 H3 0.9500 . ?
P1_1 F6_1 1.544(17) . ?
P1_1 F2_1 1.554(17) . ?
P1_1 F4_1 1.558(17) . ?
P1_1 F1_1 1.567(16) . ?
P1_1 F5_1 1.570(17) . ?
P1_1 F3_1 1.582(16) . ?
P1_2 F5_2 1.557(17) . ?
P1_2 F1_2 1.558(17) . ?
P1_2 F2_2 1.567(17) . ?
P1_2 F6_2 1.571(17) . ?
P1_2 F3_2 1.573(17) . ?
P1_2 F4_2 1.576(17) . ?

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
C6 Au2 N8 169.6(8) . . ?
C6 Au2 Au1 105.2(6) . . ?
N8 Au2 Au1 65.4(5) . . ?
C6 Au2 Au3 107.0(6) . . ?
N8 Au2 Au3 83.0(5) . . ?
Au1 Au2 Au3 128.64(3) . . ?
F1C P1 F1A 179.5(15) . . ?
F1C P1 F1D 90.0(10) . . ?
F1A P1 F1D 89.9(12) . . ?
F1C P1 F1 88.1(12) . . ?
F1A P1 F1 91.4(13) . . ?
F1D P1 F1 89.6(13) . . ?
F1C P1 F1E 88.9(11) . . ?
F1A P1 F1E 91.2(12) . . ?
F1D P1 F1E 178.9(12) . . ?
F1 P1 F1E 90.3(12) . . ?
F1C P1 F1B 91.6(11) . . ?
F1A P1 F1B 88.9(12) . . ?
F1D P1 F1B 90.3(12) . . ?
F1 P1 F1B 179.6(13) . . ?
F1E P1 F1B 89.8(13) . . ?
C18 Au3 N5 170.5(8) . . ?
C18 Au3 Au4 104.7(6) . . ?
N5 Au3 Au4 66.4(5) . . ?
C18 Au3 Au2 106.9(6) . . ?
N5 Au3 Au2 82.1(5) . . ?
Au4 Au3 Au2 129.39(3) . . ?
C22 Au4 N6 169.5(8) . . ?
C22 Au4 Au3 104.3(6) . . ?
N6 Au4 Au3 66.4(5) . . ?
C22 Au4 Au4 108.1(6) . 7_556 ?
N6 Au4 Au4 82.1(5) . 7_556 ?
Au3 Au4 Au4 128.82(3) . 7_556 ?
C3 C4 N2 110(2) . . ?
C3 C4 H4 125.2 . . ?
N2 C4 H4 125.2 . . ?
N2 C5 N3 113.4(15) . . ?
N2 C5 H5A 108.9 . . ?
N3 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N3 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N3 105.4(16) . . ?
N4 C6 Au2 130.5(15) . . ?
N3 C6 Au2 123.8(14) . . ?
C8 C7 N3 107.6(18) . . ?
C8 C7 H7 126.2 . . ?
N3 C7 H7 126.2 . . ?
C7 C8 N4 109(2) . . ?
C7 C8 H8 125.3 . . ?
N4 C8 H8 125.3 . . ?
N4 C9 C10 112.8(17) . . ?
N4 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N4 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N5 C10 C11 103.9(17) . . ?
N5 C10 C9 123.0(18) . . ?
C11 C10 C9 132.9(17) . . ?
C12 C11 C10 108.1(15) . . ?
C12 C11 Br1 127.9(16) . . ?
C10 C11 Br1 124.0(15) . . ?
N6 C12 C11 107.8(18) . . ?
N6 C12 C13 123.5(17) . . ?
C11 C12 C13 128.6(18) . . ?
C12 C13 N12 114.8(18) . 7_556 ?
C12 C13 H13A 108.6 . . ?
N12 C13 H13A 108.6 7_556 . ?
C12 C13 H13B 108.6 . . ?
N12 C13 H13B 108.6 7_556 . ?
H13A C13 H13B 107.5 . . ?
N7 C14 C15 107.8(18) . . ?
N7 C14 C1 122.2(18) . 7_556 ?
C15 C14 C1 129.8(18) . 7_556 ?
C14 C15 C16 107.3(16) . . ?
C14 C15 Br2 128.0(16) . . ?
C16 C15 Br2 124.7(15) . . ?
N8 C16 C15 106.3(17) . . ?
N8 C16 C17 122.3(17) . . ?
C15 C16 C17 130.9(18) . . ?
C16 C17 N9 113.6(18) . . ?
C16 C17 H17A 108.8 . . ?
N9 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
N9 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N9 C18 N10 107.1(17) . . ?
N9 C18 Au3 130.4(16) . . ?
N10 C18 Au3 122.4(15) . . ?
C20 C19 N9 107.1(18) . . ?
C20 C19 H19 126.5 . . ?
N9 C19 H19 126.5 . . ?
C19 C20 N10 104.5(19) . . ?
C19 C20 H20 127.8 . . ?
N10 C20 H20 127.8 . . ?
N10 C21 N11 112.6(16) . . ?
N10 C21 H21A 109.1 . . ?
N11 C21 H21A 109.1 . . ?
N10 C21 H21B 109.1 . . ?
N11 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
N11 C22 N12 106.1(16) . . ?
N11 C22 Au4 125.3(15) . . ?
N12 C22 Au4 128.6(15) . . ?
C24 C23 N11 109(2) . . ?
C24 C23 H23 125.3 . . ?
N11 C23 H23 125.3 . . ?
C23 C24 N12 107(2) . . ?
C23 C24 H24 126.7 . . ?
N12 C24 H24 126.7 . . ?
C2 N1 C3 112.4(17) . . ?
C2 N1 C1 124.7(17) . . ?
C3 N1 C1 122.6(17) . . ?
C4 N2 C2 109.7(17) . . ?
C4 N2 C5 128.8(17) . . ?
C2 N2 C5 120.9(16) . . ?
C6 N3 C7 109.0(16) . . ?
C6 N3 C5 124.4(16) . . ?
C7 N3 C5 125.9(17) . . ?
C6 N4 C8 108.5(17) . . ?
C6 N4 C9 124.1(16) . . ?
C8 N4 C9 127.4(18) . . ?
C10 N5 N6 111.5(16) . . ?
C10 N5 Au3 133.8(14) . . ?
N6 N5 Au3 112.1(11) . . ?
C12 N6 N5 108.7(16) . . ?
C12 N6 Au4 134.6(15) . . ?
N5 N6 Au4 115.1(12) . . ?
N8 N7 C14 109.5(16) . . ?
N8 N7 Au1 113.5(12) . . ?
C14 N7 Au1 135.8(15) . . ?
N7 N8 C16 109.0(16) . . ?
N7 N8 Au2 115.6(12) . . ?
C16 N8 Au2 134.5(14) . . ?
C18 N9 C19 111.2(18) . . ?
C18 N9 C17 124.8(17) . . ?
C19 N9 C17 123.9(17) . . ?
C18 N10 C20 110.1(18) . . ?
C18 N10 C21 128.3(17) . . ?
C20 N10 C21 121.2(18) . . ?
C22 N11 C23 108.1(18) . . ?
C22 N11 C21 124.6(17) . . ?
C23 N11 C21 126.2(18) . . ?
C22 N12 C24 109.7(18) . . ?
C22 N12 C13 124.2(15) . 7_556 ?
C24 N12 C13 126.1(18) . 7_556 ?
N1M C1M C2M 173(3) . . ?
C1M C2M H2MA 109.5 . . ?
C1M C2M H2MB 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
C1M C2M H2MC 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C2 Au1 N7 169.8(7) . . ?
C2 Au1 Au2 105.1(6) . . ?
N7 Au1 Au2 65.5(5) . . ?
N1 C1 C14 112.1(19) . 7_556 ?
N1 C1 H1A 109.2 . . ?
C14 C1 H1A 109.2 7_556 . ?
N1 C1 H1B 109.2 . . ?
C14 C1 H1B 109.2 7_556 . ?
H1A C1 H1B 107.9 . . ?
N1 C2 N2 103.2(17) . . ?
N1 C2 Au1 131.2(15) . . ?
N2 C2 Au1 124.7(14) . . ?
C4 C3 N1 104.9(19) . . ?
C4 C3 H3 127.6 . . ?
N1 C3 H3 127.6 . . ?
F6_1 P1_1 F2_1 93(2) . . ?
F6_1 P1_1 F4_1 92(2) . . ?
F2_1 P1_1 F4_1 175(2) . . ?
F6_1 P1_1 F1_1 93.0(14) . . ?
F2_1 P1_1 F1_1 90.7(14) . . ?
F4_1 P1_1 F1_1 89.8(14) . . ?
F6_1 P1_1 F5_1 176.2(17) . . ?
F2_1 P1_1 F5_1 89(2) . . ?
F4_1 P1_1 F5_1 86(2) . . ?
F1_1 P1_1 F5_1 90.5(14) . . ?
F6_1 P1_1 F3_1 87.7(14) . . ?
F2_1 P1_1 F3_1 88.8(14) . . ?
F4_1 P1_1 F3_1 90.7(14) . . ?
F1_1 P1_1 F3_1 179.2(17) . . ?
F5_1 P1_1 F3_1 88.8(13) . . ?
F5_2 P1_2 F1_2 90.5(15) . . ?
F5_2 P1_2 F2_2 83(2) . . ?
F1_2 P1_2 F2_2 90.6(14) . . ?
F5_2 P1_2 F6_2 177(2) . . ?
F1_2 P1_2 F6_2 89.8(15) . . ?
F2_2 P1_2 F6_2 100(2) . . ?
F5_2 P1_2 F3_2 88.3(15) . . ?
F1_2 P1_2 F3_2 178.8(18) . . ?
F2_2 P1_2 F3_2 89.3(15) . . ?
F6_2 P1_2 F3_2 91.4(15) . . ?
F5_2 P1_2 F4_2 89(2) . . ?
F1_2 P1_2 F4_2 90.2(15) . . ?
F2_2 P1_2 F4_2 172(3) . . ?
F6_2 P1_2 F4_2 88(2) . . ?
F3_2 P1_2 F4_2 89.7(15) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.128 -0.119 0.000 645 287 ' '
2 -0.183 0.312 0.250 645 286 ' '
3 0.112 0.227 0.500 646 288 ' '
4 0.150 0.684 0.750 645 287 ' '
5 0.156 0.843 0.250 285 92 ' '
6 0.343 0.343 0.000 285 88 ' '
7 0.656 0.657 0.500 283 91 ' '
8 0.843 0.157 0.750 284 88 ' '

####################################################################### 
# 
# 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_mo_heial12_0ma_sq
_database_code_depnum_ccdc_archive 'CCDC 2374512'
loop_
_audit_author_name
_audit_author_address
'Julian Zuber'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2024-11-08 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V144 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;

loop_
_publ_author_phone
08928954134
08928954134
08928954134
0498275218
''
'089 289 54101'
_platon_squeeze_details          
;Solvent Accessible Volume =      6020
Electrons Found in S.A.V. =      2119
This correponds to about 13 disordered solvent molecules per asymm unit ?(i.e. diethylether)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
Bis(calix[4]imidazolium[2]dibromo-pyrazolato)octakissilver(I)tetrakis(hexafluorophosphate)
_chemical_name_common            Ag8(LBr2)2(PF6)4
_chemical_formula_sum            'C48 H40 Ag8 Br4 F24 N24 P4 [+ 13(C4 H10 O)]'
_chemical_formula_moiety         
'C48 H40 Ag8 Br4 N24, 4(F6 P), [+ 13(C4 H10 O)]'
_chemical_formula_weight         2715.52
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_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.
;
_vrf_ABSMU01_mo_heial12_0ma_sq   
;PROBLEM: The ratio of given/expected absorption coefficient lies
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_CHEMW01_mo_heial12_0ma_sq   
;PROBLEM: The ratio of given/expected molecular weight as calculated
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMN02_mo_heial12_0ma_sq   
;PROBLEM: The minimum difference density is < -0.1*ZMAX*2.00
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMN03_mo_heial12_0ma_sq   
;PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_DIFMX02_mo_heial12_0ma_sq   
;PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: This error originates from the differing chemical formula, since the 
formula of the disordered solvent molecules treated by Platon SQUEEZE has been 
included into the overall chemical sum formula.
;
_vrf_PLAT097_mo_heial12_0ma_sq   
;PROBLEM: Large Reported Max.  (Positive) Residual Density       5.42 eA-3  
RESPONSE: see PLAT 971
;
_vrf_PLAT971_mo_heial12_0ma_sq   
;PROBLEM: Check Calcd Resid. Dens.  0.88Ang From Ag4             5.07 eA-3  
RESPONSE: Whole molecule disorder of the pillarplex cation is strongly indicated
 by large residual density peaks close to heavy atoms in the structure. 
Unfortunately, attempts to resolve this in a meaningful manner have been 
unsuccessful due to the lack of electron density on all light atoms of the 
cation. Possible minor twin domain could not be found by CELLNOW or Platon.
;
_vrf_PLAT973_mo_heial12_0ma_sq   
;PROBLEM: Check Calcd Positive Resid. Density on       Ag2       1.61 eA-3  
RESPONSE: see PLAT 971
;

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

_cell_length_a                   24.1945(15)
_cell_length_b                   24.0406(15)
_cell_length_c                   20.9494(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12185.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9310
_cell_measurement_theta_min      2.282
_cell_measurement_theta_max      26.17
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             5152
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.167
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6425
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.662
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           
;Diffractometer operator             J. Zuber
scanspeed                           2-20 s per frame
dx                                  60 mm
2229 frames measured in 7 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'IMS microsource'
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           1.0
_diffrn_detector                 CPAD
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_detector_area_resol_mean 7.5
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Duo'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            270041
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_theta_min         1.944
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12302
_reflns_number_gt                9028
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_computing_data_collection       'Bruker BIS V6.2.12/2019-08-12'
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL (Sheldrick, 2015), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1280P)²+214.7278P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         12302
_refine_ls_number_parameters     706
_refine_ls_number_restraints     2568
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2738
_refine_ls_wR_factor_gt          0.2334
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         5.424
_refine_diff_density_min         -2.549
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
P P 0.1023 0.0942 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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
C5 C 0.6116(5) 0.3811(6) 0.8402(5) 0.057(2) Uani 1 1 d . U . . .
H5 H 0.638165 0.367095 0.869398 0.068 Uiso 1 1 calc R U . . .
C6 C 0.5637(5) 0.4070(6) 0.8544(6) 0.059(2) Uani 1 1 d . U . . .
H6 H 0.549833 0.415156 0.895783 0.070 Uiso 1 1 calc R U . . .
C7 C 0.4876(4) 0.4518(6) 0.7926(6) 0.058(2) Uani 1 1 d . U . . .
H7A H 0.489817 0.483418 0.822798 0.070 Uiso 1 1 calc R U . . .
H7B H 0.484433 0.467381 0.748997 0.070 Uiso 1 1 calc R U . . .
C8 C 0.4009(4) 0.4011(6) 0.7639(6) 0.061(2) Uani 1 1 d . U . . .
C9 C 0.4197(5) 0.4088(7) 0.8685(7) 0.071(3) Uani 1 1 d . U . . .
H9 H 0.438534 0.417103 0.907153 0.085 Uiso 1 1 calc R U . . .
C10 C 0.3705(5) 0.3842(7) 0.8631(7) 0.070(3) Uani 1 1 d . U . . .
H10 H 0.346931 0.372472 0.896698 0.085 Uiso 1 1 calc R U . . .
C11 C 0.3092(4) 0.3539(6) 0.7724(7) 0.064(2) Uani 1 1 d . U . . .
H11A H 0.279259 0.358808 0.804128 0.077 Uiso 1 1 calc R U . . .
H11B H 0.298386 0.374145 0.733278 0.077 Uiso 1 1 calc R U . . .
C12 C 0.3140(4) 0.2948(6) 0.7573(6) 0.059(2) Uani 1 1 d . U . . .
Ag3 Ag 0.41375(3) 0.40261(4) 0.66570(4) 0.0571(3) Uani 1 1 d . . . . .
Ag4 Ag 0.32120(4) 0.31508(4) 0.60752(4) 0.0556(3) Uani 1 1 d . . . . .
Br1 Br 0.68407(6) 0.250000 0.84728(8) 0.0578(4) Uani 1 2 d S T P . .
Br2 Br 0.29093(8) 0.250000 0.88426(11) 0.0862(7) Uani 1 2 d S T P . .
Br3 Br 0.45661(6) 0.45060(6) 0.38734(6) 0.0683(4) Uani 1 1 d . . . . .
Ag1 Ag 0.62887(4) 0.31524(3) 0.57401(4) 0.0478(2) Uani 1 1 d . . . . .
Ag2 Ag 0.54373(3) 0.40317(4) 0.65268(4) 0.0500(2) Uani 1 1 d . . . . .
N1 N 0.6412(3) 0.2789(4) 0.6644(4) 0.0400(16) Uani 1 1 d . U . . .
N2 N 0.6140(3) 0.3792(4) 0.7731(4) 0.0481(17) Uani 1 1 d . U . . .
N3 N 0.5387(4) 0.4194(5) 0.7969(5) 0.0542(19) Uani 1 1 d . U . . .
N4 N 0.4386(4) 0.4201(5) 0.8064(5) 0.060(2) Uani 1 1 d . U . . .
N5 N 0.3612(3) 0.3795(5) 0.7985(5) 0.063(2) Uani 1 1 d . U . . .
N6 N 0.3252(3) 0.2781(4) 0.6979(5) 0.055(2) Uani 1 1 d . U . . .
N7 N 0.6296(5) 0.2996(4) 0.4282(4) 0.059(2) Uani 1 1 d . U . . .
N8 N 0.5917(5) 0.3776(4) 0.4521(4) 0.0563(19) Uani 1 1 d . U . . .
N9 N 0.5002(4) 0.4074(4) 0.5667(4) 0.0489(17) Uani 1 1 d . U . . .
N10 N 0.4445(4) 0.4070(4) 0.5723(5) 0.0505(18) Uani 1 1 d . U . . .
N11 N 0.3345(4) 0.3772(4) 0.4791(5) 0.0575(19) Uani 1 1 d . U . . .
N12 N 0.2922(4) 0.3000(4) 0.4649(5) 0.059(2) Uani 1 1 d . U . . .
C1 C 0.6648(5) 0.250000 0.7612(7) 0.044(3) Uani 1 2 d S TU P . .
C2 C 0.6552(4) 0.2963(5) 0.7224(5) 0.0445(18) Uani 1 1 d . U . . .
C3 C 0.6607(4) 0.3559(5) 0.7378(5) 0.0474(19) Uani 1 1 d . U . . .
H3A H 0.694753 0.361313 0.763250 0.057 Uiso 1 1 calc R U . . .
H3B H 0.665134 0.376967 0.697497 0.057 Uiso 1 1 calc R U . . .
C4 C 0.5690(4) 0.4007(5) 0.7468(5) 0.0454(19) Uani 1 1 d . U . . .
C13 C 0.3064(7) 0.250000 0.7960(9) 0.063(3) Uani 1 2 d S TU P . .
C14 C 0.6612(8) 0.250000 0.4348(7) 0.054(3) Uani 1 2 d S TU P . .
H14A H 0.679134 0.249999 0.477248 0.065 Uiso 1 2 calc R U P . .
H14B H 0.690811 0.250000 0.402141 0.065 Uiso 1 2 calc R U P . .
C15 C 0.6173(5) 0.3351(5) 0.4791(5) 0.055(2) Uani 1 1 d . U . . .
C16 C 0.6127(6) 0.3235(5) 0.3710(6) 0.067(3) Uani 1 1 d . U . . .
H16 H 0.617902 0.308452 0.329474 0.080 Uiso 1 1 calc R U . . .
C17 C 0.5875(6) 0.3721(5) 0.3853(6) 0.066(2) Uani 1 1 d . U . . .
H17 H 0.570473 0.397256 0.356360 0.079 Uiso 1 1 calc R U . . .
C18 C 0.5719(5) 0.4272(4) 0.4850(5) 0.053(2) Uani 1 1 d . U . . .
H18A H 0.575124 0.459628 0.456096 0.063 Uiso 1 1 calc R U . . .
H18B H 0.595382 0.434286 0.522793 0.063 Uiso 1 1 calc R U . . .
C19 C 0.5139(5) 0.4212(4) 0.5055(5) 0.0497(18) Uani 1 1 d . U . . .
C20 C 0.4634(5) 0.4291(4) 0.4747(6) 0.051(2) Uani 1 1 d . U . . .
C21 C 0.4215(5) 0.4211(5) 0.5167(6) 0.0532(19) Uani 1 1 d . U . . .
C22 C 0.3605(5) 0.4261(5) 0.5088(6) 0.057(2) Uani 1 1 d . U . . .
H22A H 0.343548 0.432176 0.551222 0.069 Uiso 1 1 calc R U . . .
H22B H 0.352443 0.459164 0.482261 0.069 Uiso 1 1 calc R U . . .
C23 C 0.3168(5) 0.3328(5) 0.5107(6) 0.057(2) Uani 1 1 d . U . . .
C24 C 0.3234(6) 0.3736(6) 0.4142(7) 0.066(2) Uani 1 1 d . U . . .
H24 H 0.331809 0.400230 0.382144 0.080 Uiso 1 1 calc R U . . .
C25 C 0.2979(6) 0.3234(5) 0.4067(6) 0.063(2) Uani 1 1 d . U . . .
H25 H 0.286192 0.307732 0.367310 0.076 Uiso 1 1 calc R U . . .
C26 C 0.2616(7) 0.250000 0.4785(8) 0.056(3) Uani 1 2 d S TU P . .
H26A H 0.250910 0.250001 0.524106 0.067 Uiso 1 2 calc R U P . .
H26B H 0.227250 0.250000 0.452818 0.067 Uiso 1 2 calc R U P . .
P1_1 P 0.6753(5) 0.2482(9) 0.2090(4) 0.091(4) Uani 0.373(13) 1 d D U P A -1
F1_1 F 0.6125(7) 0.2353(12) 0.2261(10) 0.101(7) Uani 0.373(13) 1 d D U P A -1
F2_1 F 0.6633(10) 0.2379(13) 0.1356(6) 0.105(7) Uani 0.373(13) 1 d D U P A -1
F3_1 F 0.7389(7) 0.2600(11) 0.1955(10) 0.101(7) Uani 0.373(13) 1 d D U P A -1
F4_1 F 0.6873(8) 0.256(2) 0.2835(7) 0.091(7) Uani 0.373(13) 1 d D U P A -1
F5_1 F 0.6637(13) 0.3126(9) 0.2180(16) 0.102(7) Uani 0.373(13) 1 d D U P A -1
F6_1 F 0.6863(12) 0.1831(9) 0.2030(16) 0.102(7) Uani 0.373(13) 1 d D U P A -1
P1_2 P 0.6486(14) 0.248(2) 0.1938(15) 0.101(10) Uani 0.127(13) 1 d D U P A -2
F1_2 F 0.612(2) 0.258(3) 0.1321(19) 0.110(13) Uani 0.127(13) 1 d D U P A -2
F2_2 F 0.665(4) 0.188(3) 0.169(4) 0.104(12) Uani 0.127(13) 1 d D U P A -2
F3_2 F 0.686(2) 0.239(3) 0.256(2) 0.102(12) Uani 0.127(13) 1 d D U P A -2
F4_2 F 0.630(4) 0.307(3) 0.220(3) 0.102(12) Uani 0.127(13) 1 d D U P A -2
F5_2 F 0.702(2) 0.269(3) 0.156(3) 0.108(13) Uani 0.127(13) 1 d D U P A -2
F6_2 F 0.5953(19) 0.233(4) 0.234(3) 0.107(12) Uani 0.127(13) 1 d D U P A -2
P1_3 P 0.2711(7) 0.5480(6) 0.4159(9) 0.060(4) Uani 0.47(6) 1 d D U P B 1
F1_3 F 0.2657(11) 0.4832(6) 0.4295(18) 0.074(6) Uani 0.47(6) 1 d D U P B 1
F2_3 F 0.3317(9) 0.5375(15) 0.3877(18) 0.075(6) Uani 0.47(6) 1 d D U P B 1
F3_3 F 0.2767(13) 0.6126(8) 0.4026(17) 0.068(6) Uani 0.47(6) 1 d D U P B 1
F4_3 F 0.2116(8) 0.5571(12) 0.4466(15) 0.069(6) Uani 0.47(6) 1 d D U P B 1
F5_3 F 0.2429(14) 0.5395(13) 0.3478(13) 0.078(6) Uani 0.47(6) 1 d D U P B 1
F6_3 F 0.2977(12) 0.5562(11) 0.4851(10) 0.062(5) Uani 0.47(6) 1 d D U P B 1
P1_4 P 0.2742(6) 0.5471(7) 0.4046(11) 0.077(4) Uani 0.53(6) 1 d D U P B 2
F1_4 F 0.2114(7) 0.5412(14) 0.4254(18) 0.088(6) Uani 0.53(6) 1 d D U P B 2
F2_4 F 0.2788(11) 0.4812(7) 0.4022(19) 0.089(6) Uani 0.53(6) 1 d D U P B 2
F3_4 F 0.3371(7) 0.5523(11) 0.3831(13) 0.070(5) Uani 0.53(6) 1 d D U P B 2
F4_4 F 0.2684(12) 0.6128(8) 0.4078(16) 0.075(5) Uani 0.53(6) 1 d D U P B 2
F5_4 F 0.2558(10) 0.5475(11) 0.3317(12) 0.078(6) Uani 0.53(6) 1 d D U P B 2
F6_4 F 0.2927(12) 0.5429(17) 0.4775(12) 0.090(6) Uani 0.53(6) 1 d D U P B 2
P1_5 P 0.5033(12) 0.5082(9) 0.9942(12) 0.085(4) Uani 0.5 1 d D U P C -1
F1_5 F 0.5133(13) 0.4971(10) 1.0676(12) 0.102(6) Uani 0.5 1 d D U P C -1
F2_5 F 0.5034(16) 0.4429(10) 0.9828(13) 0.096(6) Uani 0.5 1 d D U P C -1
F3_5 F 0.4969(14) 0.5210(13) 0.9201(13) 0.119(7) Uani 0.5 1 d D U P C -1
F4_5 F 0.5039(19) 0.5738(10) 1.0056(15) 0.100(7) Uani 0.5 1 d D U P C -1
F5_5 F 0.4386(12) 0.5086(13) 1.0024(14) 0.105(7) Uani 0.5 1 d D U P C -1
F6_5 F 0.5682(12) 0.5109(14) 0.9842(15) 0.120(7) Uani 0.5 1 d D U P C -1


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
C5 C6 1.349(17) . ?
C5 N2 1.406(14) . ?
C5 H5 0.9500 . ?
C6 N3 1.379(15) . ?
C6 H6 0.9500 . ?
C7 N4 1.439(16) . ?
C7 N3 1.465(14) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N5 1.312(16) . ?
C8 N4 1.355(15) . ?
C8 Ag3 2.080(13) . ?
C9 C10 1.334(18) . ?
C9 N4 1.404(17) . ?
C9 H9 0.9500 . ?
C10 N5 1.377(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.458(19) . ?
C11 N5 1.502(15) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N6 1.336(16) . ?
C12 C13 1.361(18) . ?
Ag3 N10 2.095(10) . ?
Ag3 Ag2 3.1567(12) . ?
Ag3 Ag4 3.3057(13) . ?
Ag4 C23 2.075(13) . ?
Ag4 N6 2.094(10) . ?
Ag4 Ag4 3.129(2) 7_565 ?
Br1 C1 1.864(14) . ?
Br2 C13 1.89(2) . ?
Br3 C20 1.910(12) . ?
Ag1 C15 2.064(12) . ?
Ag1 N1 2.106(8) . ?
Ag1 Ag1 3.1368(16) 7_565 ?
Ag2 C4 2.065(11) . ?
Ag2 N9 2.089(9) . ?
N1 C2 1.329(13) . ?
N1 N1 1.390(17) 7_565 ?
N2 C4 1.326(13) . ?
N2 C3 1.462(12) . ?
N3 C4 1.357(13) . ?
N6 N6 1.35(2) 7_565 ?
N7 C16 1.391(16) . ?
N7 C15 1.399(14) . ?
N7 C14 1.423(15) . ?
N8 C15 1.321(15) . ?
N8 C17 1.410(15) . ?
N8 C18 1.458(14) . ?
N9 N10 1.352(13) . ?
N9 C19 1.365(15) . ?
N10 C21 1.335(15) . ?
N11 C23 1.326(16) . ?
N11 C24 1.388(16) . ?
N11 C22 1.470(15) . ?
N12 C25 1.352(17) . ?
N12 C23 1.376(15) . ?
N12 C26 1.441(14) . ?
C1 C2 1.397(14) 7_565 ?
C1 C2 1.397(14) . ?
C2 C3 1.476(16) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.351(18) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.475(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.392(16) . ?
C20 C21 1.356(17) . ?
C21 C22 1.491(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 C25 1.364(18) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
P1_1 F2_1 1.584(12) . ?
P1_1 F5_1 1.586(13) . ?
P1_1 F3_1 1.590(12) . ?
P1_1 F6_1 1.592(13) . ?
P1_1 F1_1 1.593(12) . ?
P1_1 F4_1 1.601(12) . ?
P1_2 F1_2 1.584(13) . ?
P1_2 F2_2 1.587(14) . ?
P1_2 F4_2 1.589(14) . ?
P1_2 F5_2 1.589(14) . ?
P1_2 F6_2 1.592(14) . ?
P1_2 F3_2 1.594(13) . ?
P1_3 F3_3 1.583(11) . ?
P1_3 F1_3 1.590(12) . ?
P1_3 F4_3 1.592(12) . ?
P1_3 F5_3 1.594(12) . ?
P1_3 F6_3 1.598(12) . ?
P1_3 F2_3 1.600(12) . ?
P1_4 F1_4 1.586(11) . ?
P1_4 F2_4 1.587(12) . ?
P1_4 F4_4 1.587(12) . ?
P1_4 F5_4 1.589(12) . ?
P1_4 F3_4 1.594(11) . ?
P1_4 F6_4 1.597(12) . ?
P1_5 F5_5 1.574(12) . ?
P1_5 F1_5 1.578(12) . ?
P1_5 F6_5 1.586(12) . ?
P1_5 F2_5 1.588(12) . ?
P1_5 F3_5 1.590(12) . ?
P1_5 F4_5 1.595(12) . ?

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
C6 C5 N2 105.8(10) . . ?
C6 C5 H5 127.1 . . ?
N2 C5 H5 127.1 . . ?
C5 C6 N3 106.4(10) . . ?
C5 C6 H6 126.8 . . ?
N3 C6 H6 126.8 . . ?
N4 C7 N3 113.6(11) . . ?
N4 C7 H7A 108.8 . . ?
N3 C7 H7A 108.8 . . ?
N4 C7 H7B 108.8 . . ?
N3 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N5 C8 N4 105.2(11) . . ?
N5 C8 Ag3 131.5(9) . . ?
N4 C8 Ag3 123.0(9) . . ?
C10 C9 N4 107.3(12) . . ?
C10 C9 H9 126.4 . . ?
N4 C9 H9 126.4 . . ?
C9 C10 N5 105.5(12) . . ?
C9 C10 H10 127.2 . . ?
N5 C10 H10 127.2 . . ?
C12 C11 N5 114.3(10) . . ?
C12 C11 H11A 108.7 . . ?
N5 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
N5 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N6 C12 C13 110.1(13) . . ?
N6 C12 C11 120.7(13) . . ?
C13 C12 C11 129.1(13) . . ?
C8 Ag3 N10 167.6(4) . . ?
C8 Ag3 Ag2 103.5(3) . . ?
N10 Ag3 Ag2 64.2(3) . . ?
C8 Ag3 Ag4 104.6(4) . . ?
N10 Ag3 Ag4 85.9(3) . . ?
Ag2 Ag3 Ag4 130.22(4) . . ?
C23 Ag4 N6 166.8(4) . . ?
C23 Ag4 Ag4 101.9(3) . 7_565 ?
N6 Ag4 Ag4 64.9(3) . 7_565 ?
C23 Ag4 Ag3 105.3(3) . . ?
N6 Ag4 Ag3 84.5(2) . . ?
Ag4 Ag4 Ag3 129.53(2) 7_565 . ?
C15 Ag1 N1 168.9(4) . . ?
C15 Ag1 Ag1 103.4(3) . 7_565 ?
N1 Ag1 Ag1 65.5(2) . 7_565 ?
C4 Ag2 N9 166.9(4) . . ?
C4 Ag2 Ag3 102.3(3) . . ?
N9 Ag2 Ag3 64.7(3) . . ?
C2 N1 N1 108.3(6) . 7_565 ?
C2 N1 Ag1 136.7(8) . . ?
N1 N1 Ag1 114.5(2) 7_565 . ?
C4 N2 C5 111.6(9) . . ?
C4 N2 C3 125.0(9) . . ?
C5 N2 C3 123.4(9) . . ?
C4 N3 C6 111.6(9) . . ?
C4 N3 C7 125.8(10) . . ?
C6 N3 C7 122.5(9) . . ?
C8 N4 C9 109.0(11) . . ?
C8 N4 C7 126.9(11) . . ?
C9 N4 C7 123.8(10) . . ?
C8 N5 C10 112.9(10) . . ?
C8 N5 C11 125.1(11) . . ?
C10 N5 C11 121.9(11) . . ?
C12 N6 N6 107.5(8) . 7_565 ?
C12 N6 Ag4 134.9(9) . . ?
N6 N6 Ag4 115.1(3) 7_565 . ?
C16 N7 C15 110.0(10) . . ?
C16 N7 C14 126.0(11) . . ?
C15 N7 C14 123.6(11) . . ?
C15 N8 C17 112.7(10) . . ?
C15 N8 C18 125.7(10) . . ?
C17 N8 C18 121.4(10) . . ?
N10 N9 C19 109.0(9) . . ?
N10 N9 Ag2 115.3(7) . . ?
C19 N9 Ag2 134.4(8) . . ?
C21 N10 N9 109.7(10) . . ?
C21 N10 Ag3 132.8(8) . . ?
N9 N10 Ag3 115.8(7) . . ?
C23 N11 C24 112.1(11) . . ?
C23 N11 C22 124.7(10) . . ?
C24 N11 C22 123.1(11) . . ?
C25 N12 C23 110.3(11) . . ?
C25 N12 C26 125.3(11) . . ?
C23 N12 C26 124.2(12) . . ?
C2 C1 C2 105.6(13) 7_565 . ?
C2 C1 Br1 127.2(6) 7_565 . ?
C2 C1 Br1 127.2(6) . . ?
N1 C2 C1 108.9(10) . . ?
N1 C2 C3 121.9(10) . . ?
C1 C2 C3 129.2(10) . . ?
N2 C3 C2 114.5(9) . . ?
N2 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
N2 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
N2 C4 N3 104.5(9) . . ?
N2 C4 Ag2 130.6(7) . . ?
N3 C4 Ag2 124.7(7) . . ?
C12 C13 C12 104.8(18) 7_565 . ?
C12 C13 Br2 127.6(9) 7_565 . ?
C12 C13 Br2 127.6(9) . . ?
N7 C14 N7 113.7(16) . 7_565 ?
N7 C14 H14A 108.8 . . ?
N7 C14 H14A 108.8 7_565 . ?
N7 C14 H14B 108.8 . . ?
N7 C14 H14B 108.8 7_565 . ?
H14A C14 H14B 107.7 . . ?
N8 C15 N7 104.2(10) . . ?
N8 C15 Ag1 131.0(8) . . ?
N7 C15 Ag1 124.3(9) . . ?
C17 C16 N7 107.4(11) . . ?
C17 C16 H16 126.3 . . ?
N7 C16 H16 126.3 . . ?
C16 C17 N8 105.6(12) . . ?
C16 C17 H17 127.2 . . ?
N8 C17 H17 127.2 . . ?
N8 C18 C19 111.8(9) . . ?
N8 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
N8 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
N9 C19 C20 104.8(10) . . ?
N9 C19 C18 121.8(10) . . ?
C20 C19 C18 133.3(11) . . ?
C21 C20 C19 109.6(10) . . ?
C21 C20 Br3 126.6(9) . . ?
C19 C20 Br3 123.8(10) . . ?
N10 C21 C20 106.9(10) . . ?
N10 C21 C22 122.0(12) . . ?
C20 C21 C22 131.1(11) . . ?
N11 C22 C21 114.0(10) . . ?
N11 C22 H22A 108.7 . . ?
C21 C22 H22A 108.7 . . ?
N11 C22 H22B 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
N11 C23 N12 104.6(11) . . ?
N11 C23 Ag4 129.5(9) . . ?
N12 C23 Ag4 125.8(9) . . ?
C25 C24 N11 104.8(12) . . ?
C25 C24 H24 127.6 . . ?
N11 C24 H24 127.6 . . ?
N12 C25 C24 108.0(11) . . ?
N12 C25 H25 126.0 . . ?
C24 C25 H25 126.0 . . ?
N12 C26 N12 113.1(15) 7_565 . ?
N12 C26 H26A 108.9 7_565 . ?
N12 C26 H26A 108.9 . . ?
N12 C26 H26B 108.9 7_565 . ?
N12 C26 H26B 108.9 . . ?
H26A C26 H26B 107.8 . . ?
F2_1 P1_1 F5_1 104(2) . . ?
F2_1 P1_1 F3_1 91.9(9) . . ?
F5_1 P1_1 F3_1 91.0(12) . . ?
F2_1 P1_1 F6_1 78.5(19) . . ?
F5_1 P1_1 F6_1 177.5(16) . . ?
F3_1 P1_1 F6_1 90.0(11) . . ?
F2_1 P1_1 F1_1 90.7(10) . . ?
F5_1 P1_1 F1_1 89.6(12) . . ?
F3_1 P1_1 F1_1 177.1(12) . . ?
F6_1 P1_1 F1_1 89.2(12) . . ?
F2_1 P1_1 F4_1 178(3) . . ?
F5_1 P1_1 F4_1 78(3) . . ?
F3_1 P1_1 F4_1 88.6(9) . . ?
F6_1 P1_1 F4_1 100(3) . . ?
F1_1 P1_1 F4_1 88.7(9) . . ?
F1_2 P1_2 F2_2 90.3(14) . . ?
F1_2 P1_2 F4_2 89.8(14) . . ?
F2_2 P1_2 F4_2 178(6) . . ?
F1_2 P1_2 F5_2 90.2(14) . . ?
F2_2 P1_2 F5_2 85(5) . . ?
F4_2 P1_2 F5_2 97(5) . . ?
F1_2 P1_2 F6_2 90.9(13) . . ?
F2_2 P1_2 F6_2 100(6) . . ?
F4_2 P1_2 F6_2 78(6) . . ?
F5_2 P1_2 F6_2 175(6) . . ?
F1_2 P1_2 F3_2 179.5(19) . . ?
F2_2 P1_2 F3_2 90.0(14) . . ?
F4_2 P1_2 F3_2 89.9(14) . . ?
F5_2 P1_2 F3_2 89.4(13) . . ?
F6_2 P1_2 F3_2 89.4(13) . . ?
F3_3 P1_3 F1_3 179.7(16) . . ?
F3_3 P1_3 F4_3 90.8(10) . . ?
F1_3 P1_3 F4_3 89.3(9) . . ?
F3_3 P1_3 F5_3 90.3(12) . . ?
F1_3 P1_3 F5_3 90.0(10) . . ?
F4_3 P1_3 F5_3 89.5(13) . . ?
F3_3 P1_3 F6_3 90.3(12) . . ?
F1_3 P1_3 F6_3 89.4(10) . . ?
F4_3 P1_3 F6_3 88.9(13) . . ?
F5_3 P1_3 F6_3 178.3(15) . . ?
F3_3 P1_3 F2_3 90.7(11) . . ?
F1_3 P1_3 F2_3 89.2(10) . . ?
F4_3 P1_3 F2_3 177.6(15) . . ?
F5_3 P1_3 F2_3 92.4(17) . . ?
F6_3 P1_3 F2_3 89.2(16) . . ?
F1_4 P1_4 F2_4 89.3(10) . . ?
F1_4 P1_4 F4_4 89.6(10) . . ?
F2_4 P1_4 F4_4 178.8(13) . . ?
F1_4 P1_4 F5_4 89.9(10) . . ?
F2_4 P1_4 F5_4 89.8(12) . . ?
F4_4 P1_4 F5_4 90.6(15) . . ?
F1_4 P1_4 F3_4 179.3(14) . . ?
F2_4 P1_4 F3_4 90.1(10) . . ?
F4_4 P1_4 F3_4 91.0(10) . . ?
F5_4 P1_4 F3_4 89.7(10) . . ?
F1_4 P1_4 F6_4 90.0(11) . . ?
F2_4 P1_4 F6_4 87.1(14) . . ?
F4_4 P1_4 F6_4 92.6(15) . . ?
F5_4 P1_4 F6_4 176.8(16) . . ?
F3_4 P1_4 F6_4 90.3(11) . . ?
F5_5 P1_5 F1_5 92.8(11) . . ?
F5_5 P1_5 F6_5 177.0(18) . . ?
F1_5 P1_5 F6_5 89.0(11) . . ?
F5_5 P1_5 F2_5 91.5(18) . . ?
F1_5 P1_5 F2_5 88.8(11) . . ?
F6_5 P1_5 F2_5 91.0(17) . . ?
F5_5 P1_5 F3_5 90.5(11) . . ?
F1_5 P1_5 F3_5 176.5(14) . . ?
F6_5 P1_5 F3_5 87.7(11) . . ?
F2_5 P1_5 F3_5 92.6(11) . . ?
F5_5 P1_5 F4_5 89.2(17) . . ?
F1_5 P1_5 F4_5 91.2(11) . . ?
F6_5 P1_5 F4_5 88(2) . . ?
F2_5 P1_5 F4_5 179(3) . . ?
F3_5 P1_5 F4_5 87.4(11) . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.672 0.015 -0.008 6040 2127 ' '

