# Supplementary Information (SI) for ChemComm.
# 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_Et4F4
_database_code_depnum_ccdc_archive 'CCDC 2388131'
loop_
_audit_author_name
_audit_author_address
'Bernd M. Schmidt'
;Heinrich Heine University Dusseldorf
Germany
;
_audit_update_record             
;
2024-11-04 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT084_Et4F4               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.37 Report
RESPONSE: This compound is a hollow structure, and since it consists
 of light elements bonded by covalent bonds, a lack of precision in
 the analysis is unavoidable.
;
_vrf_PLAT934_Et4F4               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 32 Check
RESPONSE: Diffuse scattering was observered that's difficult to model accurately.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C725.60 H557.62 Cl88.80 F192 N48 O24 '
_chemical_formula_weight         17129.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           203
_space_group_name_H-M_alt        'F d -3'
_space_group_name_Hall           '-F 2uv 2vw 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'

_cell_length_a                   35.6730(4)
_cell_length_b                   35.6730(4)
_cell_length_c                   35.6730(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     45396.1(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    6418
_cell_measurement_theta_min      3.4980
_cell_measurement_theta_max      67.0080

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             17354
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    3.220
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      101(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20096
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         4.110
_diffrn_reflns_theta_max         79.271
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3991
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'

_reflns_number_gt                2631
_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       
'CrysAlisPro system (CCD 42.58a 64-bit (release 31-05-2022))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3991
_refine_ls_number_parameters     290
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.1199
_refine_ls_wR_factor_ref         0.3703
_refine_ls_wR_factor_gt          0.3399
_refine_ls_goodness_of_fit_ref   1.436
_refine_ls_restrained_S_all      1.441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cl1 Cl 0.36050(8) 0.58985(8) 0.32346(7) 0.1009(8) Uani 0.5 1 d . . P A 1
Cl5 Cl 0.28115(8) 0.57190(9) 0.31590(9) 0.1140(9) Uani 0.5 1 d . . P A 1
Cl7 Cl 0.30495(9) 0.64892(9) 0.32169(10) 0.1235(11) Uani 0.5 1 d . . P A 1
F002 F 0.24077(9) 0.61216(8) 0.55455(7) 0.1004(9) Uani 1 1 d . . . . .
F003 F 0.24093(9) 0.67912(7) 0.43971(8) 0.1014(9) Uani 1 1 d . . . . .
F004 F 0.26765(8) 0.55273(7) 0.52019(8) 0.0979(8) Uani 1 1 d . . . . .
F005 F 0.26631(10) 0.61957(8) 0.40508(7) 0.1079(10) Uani 1 1 d . . . . .
N008 N 0.30306(12) 0.54956(11) 0.41523(11) 0.0946(11) Uani 1 1 d . . . . .
C009 C 0.24714(13) 0.64760(12) 0.46037(12) 0.0848(11) Uani 1 1 d . . . . .
C00A C 0.24008(11) 0.64789(11) 0.49844(12) 0.0789(10) Uani 1 1 d . . . . .
C00B C 0.26827(12) 0.58381(13) 0.46146(13) 0.0844(11) Uani 1 1 d . . . . .
C00C C 0.24723(12) 0.61485(13) 0.51745(12) 0.0851(11) Uani 1 1 d . . . . .
C00D C 0.26124(12) 0.58379(12) 0.49954(12) 0.0832(11) Uani 1 1 d . . . . .
C00E C 0.24492(12) 0.69490(12) 0.54933(12) 0.0826(10) Uani 1 1 d . . . . .
H00E H 0.266418 0.682008 0.558321 0.099 Uiso 1 1 calc R U . . .
C00F C 0.26088(13) 0.61700(13) 0.44245(13) 0.0886(11) Uani 1 1 d . . . . .
C00G C 0.22652(12) 0.68212(11) 0.51788(12) 0.0806(10) Uani 1 1 d . . . . .
C00H C 0.33226(14) 0.47089(13) 0.45724(13) 0.0950(13) Uani 1 1 d D . . . .
C00I C 0.28396(13) 0.54928(14) 0.44510(14) 0.0935(12) Uani 1 1 d . . . . .
H00I H 0.279579 0.526056 0.457373 0.112 Uiso 1 1 calc R U . . .
C00J C 0.31008(13) 0.47943(13) 0.42592(13) 0.0935(13) Uani 1 1 d D . . . .
C00K C 0.31870(15) 0.51372(14) 0.40253(15) 0.0997(14) Uani 1 1 d . . . . .
H00A H 0.346283 0.516421 0.401121 0.120 Uiso 1 1 calc R U . . .
H00B H 0.309560 0.509031 0.376753 0.120 Uiso 1 1 calc R U . . .
C00L C 0.36428(14) 0.49718(16) 0.46883(18) 0.1066(15) Uani 1 1 d . . . . .
H00C H 0.367017 0.496580 0.496439 0.128 Uiso 1 1 calc R U . . .
H00D H 0.357859 0.523156 0.461468 0.128 Uiso 1 1 calc R U . . .
C00N C 0.40182(18) 0.4862(2) 0.4506(2) 0.131(2) Uani 1 1 d . . . . .
H00F H 0.399220 0.486617 0.423302 0.197 Uiso 1 1 calc R U . . .
H00G H 0.408881 0.460919 0.458782 0.197 Uiso 1 1 calc R U . . .
H00H H 0.421261 0.504036 0.458278 0.197 Uiso 1 1 calc R U . . .
C00O C 0.3147(3) 0.6018(3) 0.3358(3) 0.101(3) Uani 0.5 1 d . . P A 1
H00O H 0.312383 0.600295 0.363682 0.121 Uiso 0.5 1 calc R U P A 1
C4 C 0.1575(7) 0.5925(7) 0.5925(7) 0.088(9) Uani 0.1 3 d DS TU P . .
H4 H 0.173675 0.576325 0.576324 0.106 Uiso 0.1 3 calc R U P . .
Cl4 Cl 0.1407(5) 0.6326(4) 0.5691(5) 0.127(5) Uani 0.1 1 d D . P . .
C6 C 0.3563(3) 0.3937(3) 0.3937(3) 0.078(7) Uani 0.25 3 d DS T P . .
H6 H 0.340097 0.409903 0.409902 0.094 Uiso 0.25 3 calc R U P . .
Cl6 Cl 0.39014(13) 0.37185(13) 0.42185(14) 0.0927(11) Uani 0.25 1 d D . P . .
O8 O 0.4265(4) 0.6775(5) 0.4291(4) 0.079(3) Uani 0.1667 1 d D U P B -1
H8 H 0.417567 0.698740 0.433823 0.118 Uiso 0.1667 1 calc R U P B -1
C3 C 0.4180(7) 0.6676(7) 0.3913(5) 0.089(3) Uani 0.1667 1 d D U P B -1
H3A H 0.437662 0.677269 0.374671 0.133 Uiso 0.1667 1 calc R U P B -1
H3B H 0.393827 0.678498 0.384133 0.133 Uiso 0.1667 1 calc R U P B -1
H3C H 0.416758 0.640247 0.388986 0.133 Uiso 0.1667 1 calc R U P B -1
C9 C 0.3523(7) 0.6478(6) 0.4187(9) 0.089(4) Uani 0.1667 1 d D U P C -3
H9A H 0.329970 0.645739 0.402764 0.134 Uiso 0.1667 1 calc R U P C -3
H9B H 0.368845 0.667331 0.408686 0.134 Uiso 0.1667 1 calc R U P C -3
H9C H 0.344694 0.654460 0.444233 0.134 Uiso 0.1667 1 calc R U P C -3
O7 O 0.3717(5) 0.6126(5) 0.4192(6) 0.094(4) Uani 0.1667 1 d D U P C -3
H7 H 0.356178 0.595080 0.421139 0.142 Uiso 0.1667 1 calc R U P C -3
O5 O 0.3471(5) 0.6660(5) 0.4043(6) 0.090(3) Uani 0.1667 1 d D U P D -2
H5 H 0.333161 0.676907 0.419904 0.134 Uiso 0.1667 1 calc R U P D -2
C1 C 0.3689(7) 0.6927(6) 0.3853(8) 0.091(3) Uani 0.1667 1 d D U P D -2
H1A H 0.354930 0.702267 0.363658 0.137 Uiso 0.1667 1 calc R U P D -2
H1B H 0.392230 0.681019 0.376687 0.137 Uiso 0.1667 1 calc R U P D -2
H1C H 0.374819 0.713498 0.402270 0.137 Uiso 0.1667 1 calc R U P D -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C00O 1.745(10) . ?
Cl5 C00O 1.753(13) . ?
Cl7 C00O 1.789(10) . ?
F002 C00C 1.347(5) . ?
F003 C009 1.362(5) . ?
F004 C00D 1.350(5) . ?
F005 C00F 1.350(5) . ?
N008 C00I 1.265(6) . ?
N008 C00K 1.467(6) . ?
C009 C00F 1.357(6) . ?
C009 C00A 1.381(6) . ?
C00A C00C 1.384(6) . ?
C00A C00G 1.485(5) . ?
C00B C00D 1.381(6) . ?
C00B C00F 1.390(7) . ?
C00B C00I 1.474(6) . ?
C00C C00D 1.373(6) . ?
C00E C00G 1.377(6) . ?
C00E C00G 1.385(6) 44_556 ?
C00E H00E 0.9500 . ?
C00H C00J 1.390(5) 43 ?
C00H C00J 1.402(5) . ?
C00H C00L 1.535(8) . ?
C00I H00I 0.9500 . ?
C00J C00K 1.512(7) . ?
C00K H00A 0.9900 . ?
C00K H00B 0.9900 . ?
C00L C00N 1.539(7) . ?
C00L H00C 0.9900 . ?
C00L H00D 0.9900 . ?
C00N H00F 0.9800 . ?
C00N H00G 0.9800 . ?
C00N H00H 0.9800 . ?
C00O H00O 1.0000 . ?
C4 Cl4 1.761(10) 43 ?
C4 Cl4 1.761(10) 34 ?
C4 Cl4 1.761(10) . ?
C4 H4 1.0000 . ?
C6 Cl6 1.753(6) . ?
C6 Cl6 1.753(6) 43 ?
C6 Cl6 1.753(6) 34 ?
C6 H6 1.0000 . ?
O8 C3 1.427(8) . ?
O8 H8 0.8400 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C9 O7 1.435(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O7 H7 0.8400 . ?
O5 C1 1.406(10) . ?
O5 H5 0.8400 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?

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
C00I N008 C00K 117.3(4) . . ?
C00F C009 F003 117.9(4) . . ?
C00F C009 C00A 122.3(4) . . ?
F003 C009 C00A 119.8(4) . . ?
C009 C00A C00C 116.2(4) . . ?
C009 C00A C00G 121.6(4) . . ?
C00C C00A C00G 122.1(4) . . ?
C00D C00B C00F 116.5(4) . . ?
C00D C00B C00I 117.3(4) . . ?
C00F C00B C00I 126.2(4) . . ?
F002 C00C C00D 117.5(4) . . ?
F002 C00C C00A 120.7(4) . . ?
C00D C00C C00A 121.8(4) . . ?
F004 C00D C00C 118.0(4) . . ?
F004 C00D C00B 120.4(4) . . ?
C00C C00D C00B 121.5(4) . . ?
C00G C00E C00G 120.1(4) . 44_556 ?
C00G C00E H00E 119.9 . . ?
C00G C00E H00E 119.9 44_556 . ?
F005 C00F C009 117.5(4) . . ?
F005 C00F C00B 120.8(4) . . ?
C009 C00F C00B 121.6(4) . . ?
C00E C00G C00E 119.9(4) . 35_465 ?
C00E C00G C00A 119.8(4) . . ?
C00E C00G C00A 120.2(4) 35_465 . ?
C00J C00H C00J 120.5(5) 43 . ?
C00J C00H C00L 119.2(5) 43 . ?
C00J C00H C00L 120.1(5) . . ?
N008 C00I C00B 122.1(5) . . ?
N008 C00I H00I 118.9 . . ?
C00B C00I H00I 118.9 . . ?
C00H C00J C00H 119.5(5) 34 . ?
C00H C00J C00K 120.4(5) 34 . ?
C00H C00J C00K 120.0(5) . . ?
N008 C00K C00J 117.2(4) . . ?
N008 C00K H00A 108.0 . . ?
C00J C00K H00A 108.0 . . ?
N008 C00K H00B 108.0 . . ?
C00J C00K H00B 108.0 . . ?
H00A C00K H00B 107.2 . . ?
C00H C00L C00N 112.2(5) . . ?
C00H C00L H00C 109.2 . . ?
C00N C00L H00C 109.2 . . ?
C00H C00L H00D 109.2 . . ?
C00N C00L H00D 109.2 . . ?
H00C C00L H00D 107.9 . . ?
C00L C00N H00F 109.5 . . ?
C00L C00N H00G 109.5 . . ?
H00F C00N H00G 109.5 . . ?
C00L C00N H00H 109.5 . . ?
H00F C00N H00H 109.5 . . ?
H00G C00N H00H 109.5 . . ?
Cl1 C00O Cl5 112.9(6) . . ?
Cl1 C00O Cl7 109.9(6) . . ?
Cl5 C00O Cl7 109.0(6) . . ?
Cl1 C00O H00O 108.3 . . ?
Cl5 C00O H00O 108.3 . . ?
Cl7 C00O H00O 108.3 . . ?
Cl4 C4 Cl4 105.6(15) 43 34 ?
Cl4 C4 Cl4 105.6(15) 43 . ?
Cl4 C4 Cl4 105.6(15) 34 . ?
Cl4 C4 H4 113.1 43 . ?
Cl4 C4 H4 113.1 34 . ?
Cl4 C4 H4 113.1 . . ?
C4 Cl4 C4 116(2) . 2_565 ?
Cl6 C6 Cl6 110.0(6) . 43 ?
Cl6 C6 Cl6 110.0(6) . 34 ?
Cl6 C6 Cl6 110.0(6) 43 34 ?
Cl6 C6 H6 108.9 . . ?
Cl6 C6 H6 108.9 43 . ?
Cl6 C6 H6 108.9 34 . ?
C6 Cl6 C6 78.0(16) 5 . ?
C6 Cl6 H6 44.8(4) 5 38 ?
C6 Cl6 H6 122.2(12) . 38 ?
C3 O8 H8 109.5 . . ?
O8 C3 H3A 109.5 . . ?
O8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O7 C9 H9A 109.5 . . ?
O7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C9 O7 H7 109.5 . . ?
C1 O5 H5 109.5 . . ?
O5 C1 H1A 109.5 . . ?
O5 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O5 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

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
C00F C009 C00A C00C -1.0(7) . . . . ?
F003 C009 C00A C00C -179.7(4) . . . . ?
C00F C009 C00A C00G 177.4(4) . . . . ?
F003 C009 C00A C00G -1.3(7) . . . . ?
C009 C00A C00C F002 -179.1(4) . . . . ?
C00G C00A C00C F002 2.5(7) . . . . ?
C009 C00A C00C C00D 1.2(7) . . . . ?
C00G C00A C00C C00D -177.2(4) . . . . ?
F002 C00C C00D F004 -0.1(6) . . . . ?
C00A C00C C00D F004 179.6(4) . . . . ?
F002 C00C C00D C00B 179.2(4) . . . . ?
C00A C00C C00D C00B -1.1(7) . . . . ?
C00F C00B C00D F004 -180.0(4) . . . . ?
C00I C00B C00D F004 -1.9(7) . . . . ?
C00F C00B C00D C00C 0.8(7) . . . . ?
C00I C00B C00D C00C 178.9(4) . . . . ?
F003 C009 C00F F005 -2.1(7) . . . . ?
C00A C009 C00F F005 179.2(4) . . . . ?
F003 C009 C00F C00B 179.5(4) . . . . ?
C00A C009 C00F C00B 0.8(8) . . . . ?
C00D C00B C00F F005 -178.9(4) . . . . ?
C00I C00B C00F F005 3.2(8) . . . . ?
C00D C00B C00F C009 -0.6(7) . . . . ?
C00I C00B C00F C009 -178.5(5) . . . . ?
C00G C00E C00G C00E -0.8(9) 44_556 . . 35_465 ?
C00G C00E C00G C00A -179.1(3) 44_556 . . . ?
C009 C00A C00G C00E -128.1(5) . . . . ?
C00C C00A C00G C00E 50.3(6) . . . . ?
C009 C00A C00G C00E 53.6(6) . . . 35_465 ?
C00C C00A C00G C00E -128.1(5) . . . 35_465 ?
C00K N008 C00I C00B 177.2(5) . . . . ?
C00D C00B C00I N008 -155.1(5) . . . . ?
C00F C00B C00I N008 22.8(8) . . . . ?
C00J C00H C00J C00H 1.8(8) 43 . . 34 ?
C00L C00H C00J C00H -174.2(3) . . . 34 ?
C00J C00H C00J C00K 178.5(3) 43 . . . ?
C00L C00H C00J C00K 2.6(6) . . . . ?
C00I N008 C00K C00J 1.0(7) . . . . ?
C00H C00J C00K N008 92.0(6) 34 . . . ?
C00H C00J C00K N008 -84.7(6) . . . . ?
C00J C00H C00L C00N 92.5(6) 43 . . . ?
C00J C00H C00L C00N -91.5(6) . . . . ?
Cl4 C4 Cl4 C4 -77.1(9) 43 . . 2_565 ?
Cl4 C4 Cl4 C4 35(2) 34 . . 2_565 ?
Cl6 C6 Cl6 C6 50.5(9) 43 . . 5 ?
Cl6 C6 Cl6 C6 -70.8(6) 34 . . 5 ?

_refine_diff_density_max         0.808
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.129



####################################################################### 
# 
# 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_Et4H4
_database_code_depnum_ccdc_archive 'CCDC 2388132'
loop_
_audit_author_name
_audit_author_address
'Bernd M. Schmidt'
;Heinrich Heine University Dusseldorf
Germany
;
_audit_update_record             
;
2024-11-04 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_Et4H4               
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of . 1069 Ang**3
RESPONSE: This crystal is a cage-like compound, which might be partially hollow or containing disordered highly disordered solvent. Therefore, this alert makes sense.
;
_vrf_PLAT049_Et4H4               
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 ......... 0.9800 Check
RESPONSE: This is related to PLAT601, so the apparent density appears lower than it 
should be. This alert is unavoidable.
;
_vrf_PLAT340_Et4H4               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0102 Ang.
RESPONSE: This compound is a hollow structure, and since it consists 
of light elements bonded by covalent bonds, a lack of precision in 
the analysis is unavoidable.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C350.54 H326.54 Cl45 N24'
_chemical_formula_weight         6470.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_H-M_alt        'F -4 3 c'
_space_group_name_Hall           'F -4c 2 3'

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

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

_cell_length_a                   35.2652(8)
_cell_length_b                   35.2652(8)
_cell_length_c                   35.2652(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     43857(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2961
_cell_measurement_theta_min      4.3640
_cell_measurement_theta_max      68.9520

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_F_000             13452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.179
_exptl_absorpt_coefficient_mu    2.889
_shelx_estimated_absorpt_T_min   0.551
_shelx_estimated_absorpt_T_max   0.626
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12329
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.506
_diffrn_reflns_theta_max         66.959
_diffrn_reflns_theta_full        66.959
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             3155
_reflns_number_gt                2092
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_max     0.919
_reflns_Friedel_fraction_full    0.919

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H5 of C5, H20 of C20, H13 of C13, H8 of C8, H11 of C11,
  H4 of C4, H7 of C7, H10 of C10
 At 1.5 times of:
  All C(H,H,H) groups, H21 of C21
2. Restrained distances
 C21-H21
 1.1 with sigma of 0.02
 H21-C21
 1.1 with sigma of 0.02
3. Rigid bond restraints
 Cl1, Cl2, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C21 \\sim Cl4: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C20) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C20)=Sof(H20)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
 Sof(C21)=Sof(H21)=0.25*FVAR(3)
 Sof(Cl4)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 741 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3155
_refine_ls_number_parameters     186
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.1258
_refine_ls_wR_factor_ref         0.3455
_refine_ls_wR_factor_gt          0.3244
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_restrained_S_all      1.373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N1 N 0.32072(18) 0.42297(18) 0.70893(18) 0.0991(17) Uani 1 1 d . . . . .
C1 C 0.3684(3) 0.3459(3) 0.7424(2) 0.115(2) Uani 1 1 d D . . . .
H1A H 0.395542 0.340454 0.737524 0.138 Uiso 1 1 calc R U . . .
H1B H 0.365640 0.373570 0.746080 0.138 Uiso 1 1 calc R U . . .
C2 C 0.34512(19) 0.33361(16) 0.7084(2) 0.096(2) Uani 1 1 d D . . . .
C3 C 0.31324(19) 0.3562(2) 0.69876(18) 0.099(2) Uani 1 1 d D . . . .
C4 C 0.3030(3) 0.3891(2) 0.7216(2) 0.107(2) Uani 1 1 d . . . . .
H4A H 0.275126 0.392462 0.720713 0.128 Uiso 1 1 calc R U . . .
H4B H 0.310247 0.384337 0.748254 0.128 Uiso 1 1 calc R U . . .
C5 C 0.3013(2) 0.4511(2) 0.6992(2) 0.0972(19) Uani 1 1 d . . . . .
H5 H 0.274454 0.449161 0.700887 0.117 Uiso 1 1 calc R U . A .
C6 C 0.31761(16) 0.48722(17) 0.6854(2) 0.0905(18) Uani 1 1 d D . . A -1
C7 C 0.35649(17) 0.4931(2) 0.6846(2) 0.101(2) Uani 1 1 d D . . . .
H7 H 0.373292 0.474059 0.693563 0.122 Uiso 1 1 calc R U . A .
C8 C 0.3706(2) 0.5269(2) 0.6708(3) 0.109(2) Uani 1 1 d D . . . .
H8 H 0.397138 0.531298 0.671121 0.131 Uiso 1 1 calc R U . . .
C9 C 0.34669(17) 0.5546(2) 0.6565(2) 0.097(2) Uani 1 1 d D . . . .
C10 C 0.30797(19) 0.5487(2) 0.6581(2) 0.105(2) Uani 1 1 d D . . . .
H10 H 0.291274 0.567895 0.649149 0.126 Uiso 1 1 calc R U . . .
C11 C 0.2933(2) 0.51549(19) 0.6723(2) 0.102(2) Uani 1 1 d D . . . .
H11 H 0.266608 0.511846 0.673301 0.122 Uiso 1 1 calc R U . A .
C12 C 0.3629(2) 0.5886(2) 0.6389(2) 0.099(2) Uani 1 1 d . . . . .
C13 C 0.3465(2) 0.6045(2) 0.6066(2) 0.0963(19) Uani 1 1 d . . . . .
H13 H 0.324462 0.592925 0.596285 0.116 Uiso 1 1 calc R U . . .
C14 C 0.3559(5) 0.3254(7) 0.7778(4) 0.228(9) Uani 1 1 d D . . . .
H14A H 0.377106 0.310531 0.787915 0.343 Uiso 1 1 calc R U . . .
H14B H 0.334744 0.308459 0.771774 0.343 Uiso 1 1 calc R U . . .
H14C H 0.347757 0.343970 0.796853 0.343 Uiso 1 1 calc R U . . .
C20 C 0.4788(4) 0.4231(6) 0.6883(5) 0.189(10) Uani 0.549(16) 1 d D U P B 1
H20 H 0.488131 0.402199 0.671632 0.227 Uiso 0.549(16) 1 calc R U P B 1
Cl1 Cl 0.4402(3) 0.4065(3) 0.7172(5) 0.257(6) Uani 0.549(16) 1 d D U P B 1
Cl2 Cl 0.4580(4) 0.4597(4) 0.6601(4) 0.285(8) Uani 0.549(16) 1 d D U P B 1
Cl3 Cl 0.5152(3) 0.4361(3) 0.7220(4) 0.241(6) Uani 0.549(16) 1 d D U P B 1
C21 C 0.250000 0.250000 0.750000 0.151(10) Uani 0.68(3) 12 d DS TU P . .
H21 H 0.2680(3) 0.2680(3) 0.7320(3) 0.226 Uiso 0.171(7) 3 d DS U P C 2
Cl4 Cl 0.2035(2) 0.2667(2) 0.7544(2) 0.108(4) Uani 0.228(10) 1 d D U P C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C5 1.254(10) . ?
N1 C4 1.421(10) . ?
C1 C14 1.510(11) . ?
C1 C2 1.516(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.418(7) . ?
C2 C3 1.427(6) 11_566 ?
C3 C4 1.458(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.480(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(7) . ?
C6 C11 1.393(7) . ?
C7 C8 1.380(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(8) . ?
C9 C12 1.469(10) . ?
C10 C11 1.377(8) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.395(12) . ?
C12 C13 1.409(12) 10_656 ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C20 Cl2 1.786(13) . ?
C20 Cl1 1.800(13) . ?
C20 Cl3 1.806(13) . ?
C20 H20 1.0000 . ?
C21 Cl4 1.750(7) . ?
C21 H21 1.10(2) . ?

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
C5 N1 C4 120.7(7) . . ?
C14 C1 C2 111.1(11) . . ?
C14 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
C14 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C3 122.4(8) . 11_566 ?
C3 C2 C1 117.3(6) . . ?
C3 C2 C1 120.2(7) 11_566 . ?
C2 C3 C2 117.6(8) . 8_656 ?
C2 C3 C4 120.7(7) . . ?
C2 C3 C4 121.7(7) 8_656 . ?
N1 C4 C3 112.8(7) . . ?
N1 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N1 C5 C6 123.9(6) . . ?
N1 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
C7 C6 C11 119.7(6) . . ?
C7 C6 C5 121.3(6) . . ?
C11 C6 C5 119.0(6) . . ?
C8 C7 C6 119.5(6) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 121.2(6) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C10 C9 C8 118.8(6) . . ?
C10 C9 C12 121.6(6) . . ?
C8 C9 C12 119.6(6) . . ?
C11 C10 C9 120.9(7) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C6 119.9(6) . . ?
C10 C11 H11 120.1 . . ?
C6 C11 H11 120.1 . . ?
C13 C12 C13 117.2(7) . 10_656 ?
C13 C12 C9 120.8(7) . . ?
C13 C12 C9 122.0(7) 10_656 . ?
C12 C13 C12 122.8(7) . 7_665 ?
C12 C13 H13 118.6 . . ?
C12 C13 H13 118.6 7_665 . ?
C1 C14 H14A 109.5 . . ?
C1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Cl2 C20 Cl1 103.8(11) . . ?
Cl2 C20 Cl3 118.4(13) . . ?
Cl1 C20 Cl3 104.3(10) . . ?
Cl2 C20 H20 109.9 . . ?
Cl1 C20 H20 109.9 . . ?
Cl3 C20 H20 109.9 . . ?

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
C14 C1 C2 C3 94.8(12) . . . . ?
C14 C1 C2 C3 -87.1(12) . . . 11_566 ?
C3 C2 C3 C2 0.9(13) 11_566 . . 8_656 ?
C1 C2 C3 C2 178.9(5) . . . 8_656 ?
C3 C2 C3 C4 -179.8(5) 11_566 . . . ?
C1 C2 C3 C4 -1.8(9) . . . . ?
C5 N1 C4 C3 121.8(8) . . . . ?
C2 C3 C4 N1 90.0(9) . . . . ?
C2 C3 C4 N1 -90.8(9) 8_656 . . . ?
C4 N1 C5 C6 -179.3(7) . . . . ?
N1 C5 C6 C7 -4.5(11) . . . . ?
N1 C5 C6 C11 174.6(8) . . . . ?
C11 C6 C7 C8 -0.3(12) . . . . ?
C5 C6 C7 C8 178.8(8) . . . . ?
C6 C7 C8 C9 -2.2(13) . . . . ?
C7 C8 C9 C10 3.4(13) . . . . ?
C7 C8 C9 C12 -174.4(8) . . . . ?
C8 C9 C10 C11 -2.2(13) . . . . ?
C12 C9 C10 C11 175.5(8) . . . . ?
C9 C10 C11 C6 -0.1(13) . . . . ?
C7 C6 C11 C10 1.4(12) . . . . ?
C5 C6 C11 C10 -177.7(7) . . . . ?
C10 C9 C12 C13 -36.7(12) . . . . ?
C8 C9 C12 C13 141.1(8) . . . . ?
C10 C9 C12 C13 143.4(8) . . . 10_656 ?
C8 C9 C12 C13 -38.9(11) . . . 10_656 ?
C13 C12 C13 C12 0.2(15) 10_656 . . 7_665 ?
C9 C12 C13 C12 -179.8(5) . . . 7_665 ?

_refine_diff_density_max         0.507
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.093



