# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_DCsI3
_database_code_depnum_ccdc_archive 'CCDC 2381380'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_DCsI3               
;
PROBLEM: Check Calcd Positive Resid. Density on       Cs1       1.52 eA-3  
RESPONSE: Additional electron density is due to the heavy Cs+ ion
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(Cs0.33 I), 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cs I3 N2'
_chemical_formula_weight         627.80

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'
I I -0.4742 1.8119 '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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

_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, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   10.0382(2)
_cell_length_b                   10.0382(2)
_cell_length_c                   7.9849(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     696.81(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5252
_cell_measurement_theta_min      2.3380
_cell_measurement_theta_max      30.8860

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.992
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_min          0.172
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_max          0.434
_exptl_absorpt_coefficient_mu    9.267
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.17877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7018
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.343
_diffrn_reflns_theta_max         30.883
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             424
_reflns_number_gt                411
_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 1.171.40.23a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_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)+(0.0197P)²+1.5328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0102(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         424
_refine_ls_number_parameters     17
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0524
_refine_ls_wR_factor_gt          0.0522
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_restrained_S_all      1.293
_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
Cs1 Cs 0.000000 1.000000 0.500000 0.01502(19) Uani 1 12 d S T P . .
I1 I 0.18466(2) 0.81534(2) 0.250000 0.01505(17) Uani 1 4 d S T P . .
N1 N 0.333333 0.666667 0.5942(7) 0.0121(11) Uani 1 6 d S T P . .
H1 H 0.333333 0.666667 0.468956 0.014 Uiso 1 6 calc R U P . .
C1 C 0.4144(2) 0.5856(2) 0.6535(5) 0.0222(9) Uani 1 2 d S T P . .
H1A H 0.521461 0.638476 0.611090 0.027 Uiso 0.5 1 calc R U P . .
H1B H 0.361524 0.478539 0.611090 0.027 Uiso 0.5 1 calc R U P . .


_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
Cs1 I1 3.7806(3) 15_666 ?
Cs1 I1 3.7806(3) 3_465 ?
Cs1 I1 3.7806(3) 14_456 ?
Cs1 I1 3.7806(3) 2_675 ?
Cs1 I1 3.7806(3) . ?
Cs1 I1 3.7806(3) 13_576 ?
Cs1 Cs1 3.99245(10) 4_575 ?
Cs1 Cs1 3.99245(10) 4_574 ?
N1 C1 1.487(4) 2_665 ?
N1 C1 1.487(4) 3_565 ?
N1 C1 1.487(4) . ?
N1 H1 1.0000 . ?
C1 C1 1.542(9) 16_557 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
I1 Cs1 I1 180.0 15_666 3_465 ?
I1 Cs1 I1 94.692(4) 15_666 14_456 ?
I1 Cs1 I1 85.308(4) 3_465 14_456 ?
I1 Cs1 I1 85.308(4) 15_666 2_675 ?
I1 Cs1 I1 94.692(4) 3_465 2_675 ?
I1 Cs1 I1 180.0 14_456 2_675 ?
I1 Cs1 I1 85.308(4) 15_666 . ?
I1 Cs1 I1 94.692(4) 3_465 . ?
I1 Cs1 I1 85.308(4) 14_456 . ?
I1 Cs1 I1 94.692(4) 2_675 . ?
I1 Cs1 I1 94.692(4) 15_666 13_576 ?
I1 Cs1 I1 85.308(4) 3_465 13_576 ?
I1 Cs1 I1 94.692(4) 14_456 13_576 ?
I1 Cs1 I1 85.308(4) 2_675 13_576 ?
I1 Cs1 I1 180.0 . 13_576 ?
I1 Cs1 Cs1 58.129(3) 15_666 4_575 ?
I1 Cs1 Cs1 121.871(3) 3_465 4_575 ?
I1 Cs1 Cs1 58.129(3) 14_456 4_575 ?
I1 Cs1 Cs1 121.871(3) 2_675 4_575 ?
I1 Cs1 Cs1 121.871(3) . 4_575 ?
I1 Cs1 Cs1 58.129(3) 13_576 4_575 ?
I1 Cs1 Cs1 121.871(3) 15_666 4_574 ?
I1 Cs1 Cs1 58.129(3) 3_465 4_574 ?
I1 Cs1 Cs1 121.871(3) 14_456 4_574 ?
I1 Cs1 Cs1 58.129(3) 2_675 4_574 ?
I1 Cs1 Cs1 58.129(3) . 4_574 ?
I1 Cs1 Cs1 121.871(3) 13_576 4_574 ?
Cs1 Cs1 Cs1 180.0 4_575 4_574 ?
Cs1 I1 Cs1 63.742(6) 4_574 . ?
C1 N1 C1 110.4(3) 2_665 3_565 ?
C1 N1 C1 110.4(3) 2_665 . ?
C1 N1 C1 110.4(3) 3_565 . ?
C1 N1 H1 108.6 2_665 . ?
C1 N1 H1 108.6 3_565 . ?
C1 N1 H1 108.6 . . ?
N1 C1 C1 108.6(3) . 16_557 ?
N1 C1 H1A 110.0 . . ?
C1 C1 H1A 110.0 16_557 . ?
N1 C1 H1B 110.0 . . ?
C1 C1 H1B 110.0 16_557 . ?
H1A C1 H1B 108.4 . . ?

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
C1 N1 C1 C1 61.1(3) 2_665 . . 16_557 ?
C1 N1 C1 C1 -61.1(3) 3_565 . . 16_557 ?

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
N1 H1 I1 1.00 3.12 3.773(4) 124.1 . yes
N1 H1 I1 1.00 3.12 3.773(4) 124.1 2_665 yes
N1 H1 I1 1.00 3.12 3.773(4) 124.1 3_565 yes
C1 H1A I1 0.99 3.19 3.895(3) 129.6 14_556 yes
C1 H1A I1 0.99 3.27 3.925(4) 124.8 3_565 yes
C1 H1B I1 0.99 3.27 3.925(4) 124.8 2_665 yes
C1 H1B I1 0.99 3.19 3.895(3) 129.6 15_656 yes

_refine_diff_density_max         0.745
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.184

####################################################################### 
# 
# 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_DNaBr3
_database_code_depnum_ccdc_archive 'CCDC 2381382'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br3 Na, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Br3 N2 Na'
_chemical_formula_weight         376.91

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

_cell_length_a                   16.3508(2)
_cell_length_b                   16.3508(2)
_cell_length_c                   21.9979(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5093.19(13)
_cell_formula_units_Z            18
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10201
_cell_measurement_theta_min      3.6820
_cell_measurement_theta_max      78.7250

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_F_000             3240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.147
_exptl_absorpt_coefficient_mu    13.230
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10907
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         5.092
_diffrn_reflns_theta_max         79.053
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1207
_reflns_number_gt                1203
_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 1.171.40.23a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_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)+(0.0123P)²+22.9659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.000056(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1207
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0375
_refine_ls_wR_factor_gt          0.0375
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.64266(2) 0.46819(2) 0.41216(2) 0.01443(8) Uani 1 1 d . . . . .
Br2 Br 0.51739(2) 0.333333 0.583333 0.01713(9) Uani 1 2 d S T P . .
Na2 Na 0.666667 0.333333 0.333333 0.0156(4) Uani 1 6 d S T P . .
Na1 Na 0.666667 0.333333 0.50166(6) 0.0190(3) Uani 1 3 d S T P . .
N1 N 0.42062(12) 0.38309(12) 0.41566(8) 0.0156(3) Uani 1 1 d . . . . .
H1 H 0.491231 0.418377 0.414972 0.019 Uiso 1 1 calc R U . . .
C1 C 0.38594(14) 0.40805(14) 0.35974(9) 0.0167(4) Uani 1 1 d . . . . .
H1A H 0.406725 0.388346 0.323051 0.020 Uiso 1 1 calc R U . . .
H1B H 0.411831 0.477176 0.357797 0.020 Uiso 1 1 calc R U . . .
C2 C 0.38857(14) 0.41219(14) 0.47092(9) 0.0168(4) Uani 1 1 d . . . . .
H2B H 0.410339 0.480562 0.469074 0.020 Uiso 1 1 calc R U . . .
H2A H 0.415569 0.400098 0.507815 0.020 Uiso 1 1 calc R U . . .
C3 C 0.38741(15) 0.28027(15) 0.41723(11) 0.0227(5) Uani 1 1 d . . . . .
H3B H 0.410405 0.264512 0.454594 0.027 Uiso 1 1 calc R U . . .
H3A H 0.412233 0.262485 0.381645 0.027 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Na2 2.9814(2) . ?
Br1 Na1 3.1237(9) . ?
Br2 Na1 3.0308(8) . ?
Br2 Na1 3.0308(8) 16_545 ?
Na2 Na1 3.7028(13) . ?
Na2 Na1 3.7030(13) 31_655 ?
Na1 Na1 3.593(3) 16_545 ?
N1 C3 1.486(3) . ?
N1 C2 1.493(3) . ?
N1 C1 1.494(2) . ?
N1 H1 1.0000 . ?
C1 C2 1.529(3) 12 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 C3 1.532(4) 12 ?
C3 H3B 0.9900 . ?
C3 H3A 0.9900 . ?

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
Na2 Br1 Na1 74.635(19) . . ?
Na1 Br2 Na1 72.71(4) . 16_545 ?
Br1 Na2 Br1 180.0 3_665 33_545 ?
Br1 Na2 Br1 89.573(5) 3_665 2_655 ?
Br1 Na2 Br1 90.427(5) 33_545 2_655 ?
Br1 Na2 Br1 89.573(5) 3_665 . ?
Br1 Na2 Br1 90.427(5) 33_545 . ?
Br1 Na2 Br1 89.573(5) 2_655 . ?
Br1 Na2 Br1 90.427(6) 3_665 32 ?
Br1 Na2 Br1 89.573(5) 33_545 32 ?
Br1 Na2 Br1 180.0 2_655 32 ?
Br1 Na2 Br1 90.428(6) . 32 ?
Br1 Na2 Br1 90.427(5) 3_665 31_655 ?
Br1 Na2 Br1 89.573(5) 33_545 31_655 ?
Br1 Na2 Br1 90.427(6) 2_655 31_655 ?
Br1 Na2 Br1 180.0 . 31_655 ?
Br1 Na2 Br1 89.571(6) 32 31_655 ?
Br1 Na2 Na1 54.434(4) 3_665 . ?
Br1 Na2 Na1 125.566(4) 33_545 . ?
Br1 Na2 Na1 54.434(4) 2_655 . ?
Br1 Na2 Na1 54.434(4) . . ?
Br1 Na2 Na1 125.567(4) 32 . ?
Br1 Na2 Na1 125.566(4) 31_655 . ?
Br1 Na2 Na1 125.564(4) 3_665 31_655 ?
Br1 Na2 Na1 54.436(4) 33_545 31_655 ?
Br1 Na2 Na1 125.565(4) 2_655 31_655 ?
Br1 Na2 Na1 125.568(4) . 31_655 ?
Br1 Na2 Na1 54.434(4) 32 31_655 ?
Br1 Na2 Na1 54.432(4) 31_655 31_655 ?
Na1 Na2 Na1 180.0 . 31_655 ?
Br2 Na1 Br2 88.45(3) . 2_655 ?
Br2 Na1 Br2 88.45(3) . 3_665 ?
Br2 Na1 Br2 88.45(3) 2_655 3_665 ?
Br2 Na1 Br1 173.074(16) . 3_665 ?
Br2 Na1 Br1 98.048(5) 2_655 3_665 ?
Br2 Na1 Br1 89.322(5) 3_665 3_665 ?
Br2 Na1 Br1 98.047(5) . 2_655 ?
Br2 Na1 Br1 89.322(5) 2_655 2_655 ?
Br2 Na1 Br1 173.074(16) 3_665 2_655 ?
Br1 Na1 Br1 84.50(3) 3_665 2_655 ?
Br2 Na1 Br1 89.321(5) . . ?
Br2 Na1 Br1 173.074(16) 2_655 . ?
Br2 Na1 Br1 98.048(5) 3_665 . ?
Br1 Na1 Br1 84.50(3) 3_665 . ?
Br1 Na1 Br1 84.50(3) 2_655 . ?
Br2 Na1 Na1 53.65(2) . 16_545 ?
Br2 Na1 Na1 53.64(2) 2_655 16_545 ?
Br2 Na1 Na1 53.64(2) 3_665 16_545 ?
Br1 Na1 Na1 129.068(19) 3_665 16_545 ?
Br1 Na1 Na1 129.069(19) 2_655 16_545 ?
Br1 Na1 Na1 129.072(19) . 16_545 ?
Br2 Na1 Na2 126.36(2) . . ?
Br2 Na1 Na2 126.36(2) 2_655 . ?
Br2 Na1 Na2 126.36(2) 3_665 . ?
Br1 Na1 Na2 50.930(19) 3_665 . ?
Br1 Na1 Na2 50.931(19) 2_655 . ?
Br1 Na1 Na2 50.931(19) . . ?
Na1 Na1 Na2 180.0 16_545 . ?
C3 N1 C2 110.71(16) . . ?
C3 N1 C1 110.75(16) . . ?
C2 N1 C1 109.98(15) . . ?
C3 N1 H1 108.4 . . ?
C2 N1 H1 108.4 . . ?
C1 N1 H1 108.4 . . ?
N1 C1 C2 108.09(15) . 12 ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 12 . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 12 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 108.67(16) . 12 ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 12 . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 12 . ?
H2B C2 H2A 108.3 . . ?
N1 C3 C3 108.41(10) . 12 ?
N1 C3 H3B 110.0 . . ?
C3 C3 H3B 110.0 12 . ?
N1 C3 H3A 110.0 . . ?
C3 C3 H3A 110.0 12 . ?
H3B C3 H3A 108.4 . . ?

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
C3 N1 C1 C2 63.4(2) . . . 12 ?
C2 N1 C1 C2 -59.30(19) . . . 12 ?
C3 N1 C2 C1 -58.8(2) . . . 12 ?
C1 N1 C2 C1 63.89(18) . . . 12 ?
C2 N1 C3 C3 63.0(3) . . . 12 ?
C1 N1 C3 C3 -59.2(3) . . . 12 ?

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
N1 H1 Br1 1.00 2.19 3.1734(16) 168.8 . yes
C1 H1A Br1 0.99 2.97 3.892(2) 155.8 33_545 yes
C1 H1B Br2 0.99 3.01 3.907(2) 152.0 19_666 yes
C2 H2B Br2 0.99 2.90 3.834(2) 158.4 19_666 yes
C2 H2A Br2 0.99 2.92 3.864(2) 159.2 . yes
C3 H3A Br1 0.99 3.03 3.559(2) 114.9 2_655 yes
C3 H3A Br1 0.99 3.11 3.997(2) 150.3 33_545 yes
N1 H1 Br1 1.00 2.19 3.1734(16) 168.8 . yes
C1 H1A Br1 0.99 2.97 3.892(2) 155.8 33_545 yes
C1 H1B Br2 0.99 3.01 3.907(2) 152.0 19_666 yes
C2 H2B Br2 0.99 2.90 3.834(2) 158.4 19_666 yes
C2 H2A Br2 0.99 2.92 3.864(2) 159.2 . yes
C3 H3A Br1 0.99 3.03 3.559(2) 114.9 2_655 yes
C3 H3A Br1 0.99 3.11 3.997(2) 150.3 33_545 yes

_refine_diff_density_max         0.355
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2381381'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-09-02 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 K, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cl3 K N2'
_chemical_formula_weight         259.64

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'

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

_cell_length_a                   16.0388(2)
_cell_length_b                   16.0388(2)
_cell_length_c                   22.2094(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4947.79(15)
_cell_formula_units_Z            18
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20222
_cell_measurement_theta_min      2.5370
_cell_measurement_theta_max      31.2820

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             2412.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10290
_exptl_crystal_size_mid          0.06209
_exptl_crystal_size_min          0.05525
_exptl_absorpt_coefficient_mu    1.164
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.97a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23980
_diffrn_reflns_av_unetI/netI     0.0067
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.348
_diffrn_reflns_theta_max         30.970
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1613
_reflns_number_gt                1563
_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 1.171.41.97a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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)+(0.0176P)²+4.8439P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1613
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0424
_refine_ls_wR_factor_gt          0.0422
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.000000 0.000000 0.000000 0.01262(8) Uani 1 6 d S T P . .
K2 K 0.000000 0.000000 0.16726(2) 0.01457(7) Uani 1 3 d S T P . .
Cl2 Cl 0.000000 -0.15795(2) 0.250000 0.01662(7) Uani 1 2 d S T P . .
Cl1 Cl -0.14305(2) -0.17019(2) 0.07857(2) 0.01373(6) Uani 1 1 d . . . . .
N1 N 0.03790(5) 0.42266(5) 0.58409(3) 0.01283(13) Uani 1 1 d . . . . .
C1 C -0.02337(6) 0.38743(6) 0.63929(4) 0.01554(16) Uani 1 1 d . . . . .
H1A H -0.068203 0.412969 0.640494 0.019 Uiso 1 1 calc R U . . .
H1B H 0.017593 0.409839 0.675741 0.019 Uiso 1 1 calc R U . . .
C2 C -0.02412(6) 0.38937(6) 0.52898(4) 0.01574(16) Uani 1 1 d . . . . .
H2B H 0.016185 0.415657 0.492487 0.019 Uiso 1 1 calc R U . . .
H2A H -0.070947 0.412470 0.529973 0.019 Uiso 1 1 calc R U . . .
C3 C 0.10884(6) 0.38855(7) 0.58305(5) 0.02197(19) Uani 1 1 d . . . . .
H3B H 0.151525 0.413377 0.618662 0.026 Uiso 1 1 calc R U . . .
H3A H 0.149156 0.412441 0.546389 0.026 Uiso 1 1 calc R U . . .
H1 H 0.0711(10) 0.4866(10) 0.5851(6) 0.028(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 Cl1 3.08170(19) 20 ?
K1 Cl1 3.08170(19) 2 ?
K1 Cl1 3.08170(19) 21 ?
K1 Cl1 3.08170(19) 3 ?
K1 Cl1 3.08169(19) 19 ?
K1 Cl1 3.08174(19) . ?
K1 K2 3.7147(3) . ?
K1 K2 3.7147(3) 19 ?
K2 Cl2 3.1296(3) . ?
K2 Cl2 3.1297(3) 2 ?
K2 Cl2 3.1297(3) 3 ?
K2 Cl1 3.2143(3) 3 ?
K2 Cl1 3.2143(3) 2 ?
K2 Cl1 3.2144(3) . ?
K2 K2 3.6753(6) 4 ?
N1 C3 1.4889(11) . ?
N1 C1 1.4943(10) . ?
N1 C2 1.4970(11) . ?
N1 H1 0.889(13) . ?
C1 C2 1.5305(12) 16 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 C3 1.5342(18) 16 ?
C3 H3B 0.9900 . ?
C3 H3A 0.9900 . ?

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
Cl1 K1 Cl1 180.0 20 2 ?
Cl1 K1 Cl1 91.093(5) 20 21 ?
Cl1 K1 Cl1 88.907(5) 2 21 ?
Cl1 K1 Cl1 88.907(5) 20 3 ?
Cl1 K1 Cl1 91.093(5) 2 3 ?
Cl1 K1 Cl1 180.0 21 3 ?
Cl1 K1 Cl1 91.093(5) 20 19 ?
Cl1 K1 Cl1 88.907(5) 2 19 ?
Cl1 K1 Cl1 91.093(5) 21 19 ?
Cl1 K1 Cl1 88.907(5) 3 19 ?
Cl1 K1 Cl1 88.907(5) 20 . ?
Cl1 K1 Cl1 91.093(5) 2 . ?
Cl1 K1 Cl1 88.907(5) 21 . ?
Cl1 K1 Cl1 91.093(5) 3 . ?
Cl1 K1 Cl1 180.0 19 . ?
Cl1 K1 K2 124.488(4) 20 . ?
Cl1 K1 K2 55.512(4) 2 . ?
Cl1 K1 K2 124.488(4) 21 . ?
Cl1 K1 K2 55.512(4) 3 . ?
Cl1 K1 K2 124.488(4) 19 . ?
Cl1 K1 K2 55.513(4) . . ?
Cl1 K1 K2 55.512(4) 20 19 ?
Cl1 K1 K2 124.488(4) 2 19 ?
Cl1 K1 K2 55.512(4) 21 19 ?
Cl1 K1 K2 124.488(4) 3 19 ?
Cl1 K1 K2 55.512(4) 19 19 ?
Cl1 K1 K2 124.487(4) . 19 ?
K2 K1 K2 180.0 . 19 ?
Cl2 K2 Cl2 89.017(7) . 2 ?
Cl2 K2 Cl2 89.017(7) . 3 ?
Cl2 K2 Cl2 89.017(7) 2 3 ?
Cl2 K2 Cl1 172.932(4) . 3 ?
Cl2 K2 Cl1 97.225(4) 2 3 ?
Cl2 K2 Cl1 87.782(4) 3 3 ?
Cl2 K2 Cl1 97.225(4) . 2 ?
Cl2 K2 Cl1 87.782(4) 2 2 ?
Cl2 K2 Cl1 172.932(4) 3 2 ?
Cl1 K2 Cl1 86.371(8) 3 2 ?
Cl2 K2 Cl1 87.782(4) . . ?
Cl2 K2 Cl1 172.932(4) 2 . ?
Cl2 K2 Cl1 97.224(4) 3 . ?
Cl1 K2 Cl1 86.372(8) 3 . ?
Cl1 K2 Cl1 86.372(8) 2 . ?
Cl2 K2 K2 54.043(5) . 4 ?
Cl2 K2 K2 54.044(5) 2 4 ?
Cl2 K2 K2 54.044(5) 3 4 ?
Cl1 K2 K2 127.793(5) 3 4 ?
Cl1 K2 K2 127.793(5) 2 4 ?
Cl1 K2 K2 127.792(5) . 4 ?
Cl2 K2 K1 125.957(5) . . ?
Cl2 K2 K1 125.956(5) 2 . ?
Cl2 K2 K1 125.956(5) 3 . ?
Cl1 K2 K1 52.207(5) 3 . ?
Cl1 K2 K1 52.207(5) 2 . ?
Cl1 K2 K1 52.208(5) . . ?
K2 K2 K1 180.0 4 . ?
K2 Cl2 K2 71.913(10) 4 . ?
K1 Cl1 K2 72.279(6) . . ?
C3 N1 C1 110.65(7) . . ?
C3 N1 C2 110.48(7) . . ?
C1 N1 C2 109.99(7) . . ?
C3 N1 H1 107.3(8) . . ?
C1 N1 H1 108.4(8) . . ?
C2 N1 H1 110.0(8) . . ?
N1 C1 C2 108.46(6) . 16 ?
N1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 16 . ?
N1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 16 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 108.60(6) . 16 ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 16 . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 16 . ?
H2B C2 H2A 108.3 . . ?
N1 C3 C3 108.55(4) . 16 ?
N1 C3 H3B 110.0 . . ?
C3 C3 H3B 110.0 16 . ?
N1 C3 H3A 110.0 . . ?
C3 C3 H3A 110.0 16 . ?
H3B C3 H3A 108.4 . . ?

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
C3 N1 C1 C2 -62.27(8) . . . 16 ?
C2 N1 C1 C2 60.07(8) . . . 16 ?
C3 N1 C2 C1 59.76(9) . . . 16 ?
C1 N1 C2 C1 -62.68(8) . . . 16 ?
C1 N1 C3 C3 59.80(12) . . . 16 ?
C2 N1 C3 C3 -62.25(12) . . . 16 ?

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
C1 H1A Cl2 0.99 2.88 3.7848(9) 152.1 8_455 yes
C1 H1B Cl1 0.99 2.85 3.7875(9) 157.8 13 yes
C2 H2B Cl2 0.99 2.79 3.7417(9) 161.9 32 yes
C2 H2A Cl2 0.99 2.82 3.7390(9) 155.6 8_455 yes
C3 H3B Cl1 0.99 2.98 3.5002(9) 113.7 33 yes
N1 H1 Cl1 0.889(13) 2.140(13) 3.0256(7) 174.6(12) 32 yes

_refine_diff_density_max         0.391
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2381383'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-09-02 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl2 Cs I, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cl2 Cs I N2'
_chemical_formula_weight         444.90

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'

_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, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   9.77000(10)
_cell_length_b                   9.77000(10)
_cell_length_c                   11.9653(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     989.11(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    23797
_cell_measurement_theta_min      2.4000
_cell_measurement_theta_max      31.0280

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_F_000             618.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_min          0.114
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_max          0.349
_exptl_absorpt_coefficient_mu    5.515
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31157
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.407
_diffrn_reflns_theta_max         30.901
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2095
_reflns_number_gt                1895
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_max     0.891
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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)+(0.0132P)²+0.6584P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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_abs_structure_details 
;
 Flack x determined using 749 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2095
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_ref         0.0357
_refine_ls_wR_factor_gt          0.0354
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.63252(3) 1.000000 0.333333 0.02254(7) Uani 1 2 d S T P . .
I1 I 0.77018(3) 0.77018(3) 0.500000 0.02317(8) Uani 1 2 d S T P . .
N1 N 0.6504(3) 0.9182(3) 0.9194(2) 0.0244(6) Uani 1 1 d . . . . .
H1 H 0.617141 0.852342 0.988833 0.029 Uiso 1 1 calc R U . . .
C3 C 0.8162(4) 0.9605(4) 0.8908(3) 0.0235(7) Uani 1 1 d . . . . .
H3A H 0.825559 0.864177 0.889249 0.028 Uiso 1 1 calc R U . . .
H3B H 0.890467 1.033628 0.947542 0.028 Uiso 1 1 calc R U . . .
C1 C 0.5777(4) 0.9347(5) 0.7267(3) 0.0292(8) Uani 1 1 d . . . . .
H1B H 0.583542 0.882350 0.657470 0.035 Uiso 1 1 calc R U . . .
H1A H 0.492728 0.961011 0.717683 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5422(5) 0.8251(4) 0.8261(3) 0.0328(8) Uani 1 1 d . . . . .
H2A H 0.430814 0.780928 0.849559 0.039 Uiso 1 1 calc R U . . .
H2B H 0.558986 0.736439 0.805546 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.54431(10) 0.72207(9) 0.13060(6) 0.02331(15) Uani 1 1 d . . . . .


_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
Cs1 Cl1 3.3827(8) 6_665 ?
Cs1 Cl1 3.3828(8) 2_665 ?
Cs1 Cl1 3.4148(7) . ?
Cs1 Cl1 3.4148(7) 5_675 ?
Cs1 I1 3.72116(19) . ?
Cs1 I1 3.72118(19) 3_674 ?
N1 C2 1.493(4) . ?
N1 C1 1.495(5) 5_676 ?
N1 C3 1.498(4) . ?
N1 H1 1.0000 . ?
C3 C3 1.529(7) 5_676 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 C2 1.520(5) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?

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
Cl1 Cs1 Cl1 79.75(3) 6_665 2_665 ?
Cl1 Cs1 Cl1 95.132(5) 6_665 . ?
Cl1 Cs1 Cl1 97.67(2) 2_665 . ?
Cl1 Cs1 Cl1 97.67(2) 6_665 5_675 ?
Cl1 Cs1 Cl1 95.133(5) 2_665 5_675 ?
Cl1 Cs1 Cl1 163.30(3) . 5_675 ?
Cl1 Cs1 I1 171.413(15) 6_665 . ?
Cl1 Cs1 I1 91.662(14) 2_665 . ?
Cl1 Cs1 I1 85.673(14) . . ?
Cl1 Cs1 I1 83.273(14) 5_675 . ?
Cl1 Cs1 I1 91.661(14) 6_665 3_674 ?
Cl1 Cs1 I1 171.411(15) 2_665 3_674 ?
Cl1 Cs1 I1 83.273(14) . 3_674 ?
Cl1 Cs1 I1 85.674(14) 5_675 3_674 ?
I1 Cs1 I1 96.923(10) . 3_674 ?
Cs1 I1 Cs1 166.102(10) 2_765 . ?
C2 N1 C1 110.4(3) . 5_676 ?
C2 N1 C3 109.6(3) . . ?
C1 N1 C3 109.8(3) 5_676 . ?
C2 N1 H1 109.0 . . ?
C1 N1 H1 109.0 5_676 . ?
C3 N1 H1 109.0 . . ?
N1 C3 C3 108.08(17) . 5_676 ?
N1 C3 H3A 110.1 . . ?
C3 C3 H3A 110.1 5_676 . ?
N1 C3 H3B 110.1 . . ?
C3 C3 H3B 110.1 5_676 . ?
H3A C3 H3B 108.4 . . ?
N1 C1 C2 108.3(3) 5_676 . ?
N1 C1 H1B 110.0 5_676 . ?
C2 C1 H1B 110.0 . . ?
N1 C1 H1A 110.0 5_676 . ?
C2 C1 H1A 110.0 . . ?
H1B C1 H1A 108.4 . . ?
N1 C2 C1 108.3(3) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
Cs1 Cl1 Cs1 159.91(3) 3_564 . ?

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
C2 N1 C3 C3 52.5(4) . . . 5_676 ?
C1 N1 C3 C3 -69.0(4) 5_676 . . 5_676 ?
C1 N1 C2 C1 51.5(4) 5_676 . . . ?
C3 N1 C2 C1 -69.5(4) . . . . ?
N1 C1 C2 N1 14.3(4) 5_676 . . . ?

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
N1 H1 Cl1 1.00 2.02 3.024(3) 177.9 1_556 yes
C3 H3A Cl1 0.99 2.77 3.702(3) 156.6 4_556 yes
C3 H3B I1 0.99 3.11 4.040(3) 158.0 3_675 yes
C1 H1B I1 0.99 3.17 4.062(3) 150.1 . yes
C1 H1A I1 0.99 3.10 3.969(3) 146.7 2_665 yes
C2 H2A Cl1 0.99 2.96 3.602(4) 123.7 3_565 yes

_refine_diff_density_max         0.512
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_DCsBr3
_database_code_depnum_ccdc_archive 'CCDC 2381390'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2025-02-17 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br3 Cs, C6 H14 N2'
_chemical_formula_sum            'C6 H14 Br3 Cs N2'
_chemical_formula_weight         486.83

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'
Cs Cs -0.3680 2.1192 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

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

_cell_length_a                   9.8044(2)
_cell_length_b                   9.8273(3)
_cell_length_c                   27.3662(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2636.75(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9474
_cell_measurement_theta_min      2.4950
_cell_measurement_theta_max      31.0530

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.077
_exptl_absorpt_coefficient_mu    11.862
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.30776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20554
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.077
_diffrn_reflns_theta_max         30.866
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.777
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.777
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             3387
_reflns_number_gt                2981
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+6.3540P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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         3387
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.500000 1.00937(4) 0.250000 0.01613(11) Uani 1 2 d S T P . .
Cs2 Cs 0.500000 1.000000 0.500000 0.01807(11) Uani 1 2 d S . P . .
N2 N 0.5669(4) 0.4326(4) 0.40488(14) 0.0246(9) Uani 1 1 d . . . . .
H2 H 0.614273 0.379434 0.430993 0.030 Uiso 1 1 calc R U . . .
N1 N 0.4502(5) 0.5643(5) 0.34017(15) 0.0328(10) Uani 1 1 d . . . . .
H1 H 0.403383 0.618658 0.314212 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5925(5) 0.5807(6) 0.41285(18) 0.0308(12) Uani 1 1 d . . . . .
H4A H 0.691326 0.597325 0.417274 0.037 Uiso 1 1 calc R U . . .
H4B H 0.544201 0.612137 0.442544 0.037 Uiso 1 1 calc R U . . .
C2 C 0.5340(6) 0.4566(6) 0.31674(16) 0.0288(11) Uani 1 1 d . . . . .
H2A H 0.592517 0.496779 0.291033 0.035 Uiso 1 1 calc R U . . .
H2B H 0.474151 0.387603 0.301403 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6219(5) 0.3905(5) 0.35584(17) 0.0247(10) Uani 1 1 d . . . . .
H1A H 0.618891 0.290217 0.352549 0.030 Uiso 1 1 calc R U . . .
H1B H 0.717845 0.420497 0.352380 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3462(6) 0.5030(7) 0.3726(2) 0.0417(17) Uani 1 1 d . . . . .
H6A H 0.276979 0.454275 0.352936 0.050 Uiso 1 1 calc R U . . .
H6B H 0.299539 0.575021 0.391624 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4174(5) 0.4039(6) 0.4072(2) 0.0340(12) Uani 1 1 d . . . . .
H5A H 0.383472 0.416461 0.440979 0.041 Uiso 1 1 calc R U . . .
H5B H 0.398949 0.308889 0.397110 0.041 Uiso 1 1 calc R U . . .
C3 C 0.5414(8) 0.6559(7) 0.3690(2) 0.0434(15) Uani 1 1 d . . . . .
H3A H 0.490438 0.737890 0.379407 0.052 Uiso 1 1 calc R U . . .
H3B H 0.619289 0.685418 0.348539 0.052 Uiso 1 1 calc R U . . .
Br3A Br 0.69477(5) 1.30577(5) 0.50203(2) 0.02297(15) Uani 0.9712(15) 1 d . . P
A 1
Br3B Br 0.7250(18) 1.2764(19) 0.5249(8) 0.02297(15) Uani 0.0288(15) 1 d . . P A
2
Br2A Br 0.53086(6) 1.03537(6) 0.37551(2) 0.02244(15) Uani 0.9795(13) 1 d . . P
A 1
Br2B Br 0.532(3) 0.935(3) 0.3760(7) 0.02244(15) Uani 0.0205(13) 1 d . . P A 2
Br1A Br 0.27396(9) 0.73585(7) 0.26215(5) 0.0238(2) Uani 0.976(4) 1 d . . P A 1
Br1B Br 0.243(4) 0.753(3) 0.2792(17) 0.0238(2) Uani 0.024(4) 1 d . . P A 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
Cs1 Br2A 3.4574(4) . ?
Cs1 Br2A 3.4575(4) 3_655 ?
Cs1 Br1B 3.47(2) 6_666 ?
Cs1 Br1B 3.47(2) 8_665 ?
Cs1 Br1A 3.4996(6) . ?
Cs1 Br1A 3.4996(6) 3_655 ?
Cs1 Br1A 3.5042(6) 6_666 ?
Cs1 Br1A 3.5042(6) 8_665 ?
Cs1 Br2B 3.54(2) . ?
Cs1 Br2B 3.54(2) 3_655 ?
Cs1 Br1B 3.65(3) 3_655 ?
Cs1 Br1B 3.65(3) . ?
Cs2 Br2A 3.4378(4) 5_676 ?
Cs2 Br2A 3.4379(4) . ?
Cs2 Br2B 3.466(19) 5_676 ?
Cs2 Br2B 3.467(19) . ?
Cs2 Br3B 3.545(17) 8_755 ?
Cs2 Br3B 3.545(17) 4_476 ?
Cs2 Br3A 3.5500(5) 8_755 ?
Cs2 Br3A 3.5500(5) 4_476 ?
Cs2 Br3A 3.5608(5) . ?
Cs2 Br3A 3.5608(5) 5_676 ?
Cs2 Br3B 3.564(17) . ?
Cs2 Br3B 3.564(17) 5_676 ?
N2 C4 1.492(7) . ?
N2 C5 1.494(7) . ?
N2 C1 1.505(6) . ?
N2 H2 1.0000 . ?
N1 C6 1.480(7) . ?
N1 C2 1.486(7) . ?
N1 C3 1.494(8) . ?
N1 H1 1.0000 . ?
C4 C3 1.496(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 C1 1.519(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C6 C5 1.527(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

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
Br2A Cs1 Br2A 171.52(2) . 3_655 ?
Br2A Cs1 Br1B 96.8(8) . 6_666 ?
Br2A Cs1 Br1B 77.3(8) 3_655 6_666 ?
Br2A Cs1 Br1B 77.3(8) . 8_665 ?
Br2A Cs1 Br1B 96.8(8) 3_655 8_665 ?
Br1B Cs1 Br1B 92.6(10) 6_666 8_665 ?
Br2A Cs1 Br1A 91.02(2) . . ?
Br2A Cs1 Br1A 95.50(2) 3_655 . ?
Br2A Cs1 Br1A 95.49(2) . 3_655 ?
Br2A Cs1 Br1A 91.02(2) 3_655 3_655 ?
Br1A Cs1 Br1A 79.64(4) . 3_655 ?
Br2A Cs1 Br1A 88.87(2) . 6_666 ?
Br2A Cs1 Br1A 85.75(2) 3_655 6_666 ?
Br1A Cs1 Br1A 169.20(3) . 6_666 ?
Br1A Cs1 Br1A 89.623(5) 3_655 6_666 ?
Br2A Cs1 Br1A 85.75(2) . 8_665 ?
Br2A Cs1 Br1A 88.87(2) 3_655 8_665 ?
Br1A Cs1 Br1A 89.623(5) . 8_665 ?
Br1A Cs1 Br1A 169.20(3) 3_655 8_665 ?
Br1A Cs1 Br1A 101.14(3) 6_666 8_665 ?
Br1B Cs1 Br2B 107.8(10) 6_666 . ?
Br1B Cs1 Br2B 88.8(9) 8_665 . ?
Br2A Cs1 Br2B 172.3(5) . 3_655 ?
Br2A Cs1 Br2B 16.2(5) 3_655 3_655 ?
Br1A Cs1 Br2B 83.0(5) . 3_655 ?
Br1A Cs1 Br2B 78.8(5) 3_655 3_655 ?
Br1A Cs1 Br2B 96.1(5) 6_666 3_655 ?
Br1A Cs1 Br2B 98.9(5) 8_665 3_655 ?
Br2A Cs1 Br1B 102.0(6) . 3_655 ?
Br2A Cs1 Br1B 83.9(7) 3_655 3_655 ?
Br1A Cs1 Br1B 85.9(7) . 3_655 ?
Br1A Cs1 Br1B 9.1(8) 3_655 3_655 ?
Br1A Cs1 Br1B 83.5(6) 6_666 3_655 ?
Br1A Cs1 Br1B 171.1(4) 8_665 3_655 ?
Br1B Cs1 Br1B 179.3(6) 6_666 . ?
Br1B Cs1 Br1B 87.2(3) 8_665 . ?
Br2B Cs1 Br1B 72.9(8) . . ?
Br2B Cs1 Br1B 90.5(9) 3_655 . ?
Br1B Cs1 Br1B 92.9(14) 3_655 . ?
Br2A Cs2 Br2A 179.999(19) 5_676 . ?
Br2A Cs2 Br2B 16.4(5) 5_676 5_676 ?
Br2A Cs2 Br2B 163.6(5) . 5_676 ?
Br2B Cs2 Br2B 180.0(8) 5_676 . ?
Br2A Cs2 Br3B 79.3(3) 5_676 8_755 ?
Br2A Cs2 Br3B 100.7(3) . 8_755 ?
Br2A Cs2 Br3B 100.7(3) 5_676 4_476 ?
Br2A Cs2 Br3B 79.3(3) . 4_476 ?
Br2A Cs2 Br3A 90.248(13) 5_676 8_755 ?
Br2A Cs2 Br3A 89.752(13) . 8_755 ?
Br2A Cs2 Br3A 89.752(13) 5_676 4_476 ?
Br2A Cs2 Br3A 90.248(13) . 4_476 ?
Br3A Cs2 Br3A 180.0 8_755 4_476 ?
Br2A Cs2 Br3A 96.723(13) 5_676 . ?
Br2A Cs2 Br3A 83.277(13) . . ?
Br3A Cs2 Br3A 90.081(4) 8_755 . ?
Br3A Cs2 Br3A 89.919(4) 4_476 . ?
Br2A Cs2 Br3A 83.277(13) 5_676 5_676 ?
Br2A Cs2 Br3A 96.723(13) . 5_676 ?
Br3A Cs2 Br3A 89.919(4) 8_755 5_676 ?
Br3A Cs2 Br3A 90.081(4) 4_476 5_676 ?
Br3A Cs2 Br3A 180.0 . 5_676 ?
Br2B Cs2 Br3B 74.3(6) 5_676 . ?
Br2B Cs2 Br3B 105.7(6) . . ?
Br3B Cs2 Br3B 88.00(14) 8_755 . ?
Br3B Cs2 Br3B 92.00(14) 4_476 . ?
Br2A Cs2 Br3B 93.3(3) 5_676 5_676 ?
Br2A Cs2 Br3B 86.7(3) . 5_676 ?
Br3A Cs2 Br3B 96.6(3) 8_755 5_676 ?
Br3A Cs2 Br3B 83.4(3) 4_476 5_676 ?
Br3A Cs2 Br3B 167.9(4) . 5_676 ?
Br3A Cs2 Br3B 12.1(4) 5_676 5_676 ?
C4 N2 C5 110.1(4) . . ?
C4 N2 C1 109.8(4) . . ?
C5 N2 C1 109.8(4) . . ?
C4 N2 H2 109.1 . . ?
C5 N2 H2 109.1 . . ?
C1 N2 H2 109.1 . . ?
C6 N1 C2 110.5(5) . . ?
C6 N1 C3 109.9(4) . . ?
C2 N1 C3 109.0(5) . . ?
C6 N1 H1 109.1 . . ?
C2 N1 H1 109.1 . . ?
C3 N1 H1 109.1 . . ?
N2 C4 C3 107.9(4) . . ?
N2 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
N2 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N1 C2 C1 108.3(4) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
N2 C1 C2 107.9(4) . . ?
N2 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N2 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
N1 C6 C5 108.5(4) . . ?
N1 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N1 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N2 C5 C6 107.5(4) . . ?
N2 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
N2 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
N1 C3 C4 109.0(5) . . ?
N1 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
Cs2 Br3A Cs2 154.905(17) 4_576 . ?
Cs2 Br3B Cs2 155.0(6) 4_576 . ?
Cs2 Br2A Cs1 165.761(19) . . ?
Cs2 Br2B Cs1 155.1(10) . . ?
Cs1 Br1A Cs1 164.632(19) . 6_556 ?
Cs1 Br1B Cs1 154.1(15) 6_556 . ?

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
C5 N2 C4 C3 -69.9(5) . . . . ?
C1 N2 C4 C3 51.0(6) . . . . ?
C6 N1 C2 C1 -69.2(5) . . . . ?
C3 N1 C2 C1 51.7(6) . . . . ?
C4 N2 C1 C2 -68.9(5) . . . . ?
C5 N2 C1 C2 52.2(5) . . . . ?
N1 C2 C1 N2 14.2(6) . . . . ?
C2 N1 C6 C5 51.7(6) . . . . ?
C3 N1 C6 C5 -68.7(6) . . . . ?
C4 N2 C5 C6 51.5(5) . . . . ?
C1 N2 C5 C6 -69.5(5) . . . . ?
N1 C6 C5 N2 15.0(6) . . . . ?
C6 N1 C3 C4 50.7(7) . . . . ?
C2 N1 C3 C4 -70.6(6) . . . . ?
N2 C4 C3 N1 15.7(7) . . . . ?

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
N2 H2 Br3A^a 1.00 2.22 3.193(4) 164.1 1_545 yes
N2 H2 Br3B^b 1.00 2.97 3.94(2) 165.3 1_545 yes
N1 H1 Br1A^a 1.00 2.23 3.222(4) 172.4 . yes
N1 H1 Br1B^b 1.00 2.27 3.22(3) 158.4 . yes
C4 H4A Br2A^a 0.99 3.02 3.857(5) 143.5 8_755 yes
C4 H4B Br3A^a 0.99 2.91 3.822(5) 154.3 5_676 yes
C4 H4B Br3B^b 0.99 2.99 3.817(18) 141.3 5_676 yes
C2 H2A Br1A^a 0.99 3.06 3.967(6) 153.2 3_655 yes
C2 H2B Br1A^a 0.99 3.05 4.007(6) 163.2 8_655 yes
C2 H2B Br1B^b 0.99 2.57 3.52(5) 160.1 8_655 yes
C1 H1A Br2A^a 0.99 2.72 3.642(5) 154.7 1_545 yes
C1 H1B Br2A^a 0.99 2.78 3.729(5) 160.0 8_755 yes
C1 H1B Br2B^b 0.99 2.54 3.46(3) 155.4 8_755 yes
C6 H6A Br2B^b 0.99 3.10 3.77(3) 126.0 8_655 yes
C6 H6A Br1B^b 0.99 2.83 3.65(5) 140.6 8_655 yes
C6 H6B Br3A^a 0.99 3.14 3.932(6) 138.2 5_676 yes
C6 H6B Br3B^b 0.99 2.72 3.613(19) 149.9 5_676 yes
C5 H5A Br3B^b 0.99 2.62 3.19(2) 116.2 4_466 yes
C5 H5B Br2A^a 0.99 3.04 3.887(6) 144.1 1_545 yes
C3 H3A Br2A^a 0.99 2.95 3.735(6) 136.7 . yes
C3 H3A Br2B^b 0.99 1.98 2.75(3) 132.7 . yes
N2 H2 Br3A^a 1.00 2.22 3.193(4) 164.1 1_545 yes
N2 H2 Br3B^b 1.00 2.97 3.94(2) 165.3 1_545 yes
N1 H1 Br1A^a 1.00 2.23 3.222(4) 172.4 . yes
N1 H1 Br1B^b 1.00 2.27 3.22(3) 158.4 . yes
C4 H4A Br2A^a 0.99 3.02 3.857(5) 143.5 8_755 yes
C4 H4B Br3A^a 0.99 2.91 3.822(5) 154.3 5_676 yes
C4 H4B Br3B^b 0.99 2.99 3.817(18) 141.3 5_676 yes
C2 H2A Br1A^a 0.99 3.06 3.967(6) 153.2 3_655 yes
C2 H2B Br1A^a 0.99 3.05 4.007(6) 163.2 8_655 yes
C2 H2B Br1B^b 0.99 2.57 3.52(5) 160.1 8_655 yes
C1 H1A Br2A^a 0.99 2.72 3.642(5) 154.7 1_545 yes
C1 H1B Br2A^a 0.99 2.78 3.729(5) 160.0 8_755 yes
C1 H1B Br2B^b 0.99 2.54 3.46(3) 155.4 8_755 yes
C6 H6A Br2B^b 0.99 3.10 3.77(3) 126.0 8_655 yes
C6 H6A Br1B^b 0.99 2.83 3.65(5) 140.6 8_655 yes
C6 H6B Br3A^a 0.99 3.14 3.932(6) 138.2 5_676 yes
C6 H6B Br3B^b 0.99 2.72 3.613(19) 149.9 5_676 yes
C5 H5A Br3B^b 0.99 2.62 3.19(2) 116.2 4_466 yes
C5 H5B Br2A^a 0.99 3.04 3.887(6) 144.1 1_545 yes
C3 H3A Br2A^a 0.99 2.95 3.735(6) 136.7 . yes
C3 H3A Br2B^b 0.99 1.98 2.75(3) 132.7 . yes

_refine_diff_density_max         1.393
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.188

####################################################################### 
# 
# 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_DKBr3
_database_code_depnum_ccdc_archive 'CCDC 2381387'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br3 K, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Br3 K N2'
_chemical_formula_weight         392.99

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

_cell_length_a                   16.5223(3)
_cell_length_b                   16.5223(3)
_cell_length_c                   23.0126(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5440.5(2)
_cell_formula_units_Z            18
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11216
_cell_measurement_theta_min      2.4590
_cell_measurement_theta_max      31.0390

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_F_000             3384
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.131
_exptl_absorpt_coefficient_mu    10.312
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15695
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.271
_diffrn_reflns_theta_max         30.907
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1716
_reflns_number_gt                1599
_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 1.171.40.23a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_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)+(0.0266P)²+6.1566P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.000196(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1716
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0500
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.18568(2) 0.49416(2) 0.24526(2) 0.01394(7) Uani 1 1 d . . . . .
Br2 Br 0.333333 0.50557(2) 0.416667 0.01673(8) Uani 1 2 d S T P . .
K2 K 0.333333 0.666667 0.166667 0.01353(17) Uani 1 6 d S T P . .
K1 K 0.333333 0.666667 0.33349(3) 0.01561(13) Uani 1 3 d S T P . .
N1 N 0.28276(11) 0.36928(11) 0.24854(6) 0.0146(3) Uani 1 1 d . . . . .
H1 H 0.247980 0.404361 0.247395 0.017 Uiso 1 1 calc R U . . .
C3 C 0.25388(13) 0.30965(13) 0.30190(7) 0.0171(3) Uani 1 1 d . . . . .
H3A H 0.186084 0.263958 0.300479 0.021 Uiso 1 1 calc R U . . .
H3B H 0.266547 0.349060 0.336900 0.021 Uiso 1 1 calc R U . . .
C1 C 0.25825(13) 0.30944(13) 0.19527(7) 0.0171(3) Uani 1 1 d . . . . .
H1A H 0.277281 0.349052 0.159999 0.021 Uiso 1 1 calc R U . . .
H1B H 0.189913 0.266190 0.193579 0.021 Uiso 1 1 calc R U . . .
C2 C 0.38446(14) 0.43790(13) 0.25031(10) 0.0252(4) Uani 1 1 d . . . . .
H2A H 0.399807 0.476347 0.285970 0.030 Uiso 1 1 calc R U . . .
H2B H 0.402404 0.479999 0.216246 0.030 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 K2 3.22380(17) . ?
Br1 K1 3.3533(4) . ?
Br2 K1 3.2784(4) . ?
Br2 K1 3.2786(4) 10_455 ?
K2 K1 3.8390(6) 25_565 ?
K2 K1 3.8391(6) . ?
K1 K1 3.8283(12) 10_455 ?
N1 C2 1.485(2) . ?
N1 C3 1.495(2) . ?
N1 C1 1.498(2) . ?
N1 H1 1.0000 . ?
C3 C1 1.532(2) 4 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.529(4) 4 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?

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
K2 Br1 K1 71.392(9) . . ?
K1 Br2 K1 71.443(18) . 10_455 ?
Br1 K2 Br1 91.601(4) 26_455 25_565 ?
Br1 K2 Br1 88.400(4) 26_455 . ?
Br1 K2 Br1 180.0 25_565 . ?
Br1 K2 Br1 180.0 26_455 2_665 ?
Br1 K2 Br1 88.400(4) 25_565 2_665 ?
Br1 K2 Br1 91.599(4) . 2_665 ?
Br1 K2 Br1 88.398(4) 26_455 3_565 ?
Br1 K2 Br1 88.399(4) 25_565 3_565 ?
Br1 K2 Br1 91.599(4) . 3_565 ?
Br1 K2 Br1 91.600(4) 2_665 3_565 ?
Br1 K2 Br1 91.600(4) 26_455 27 ?
Br1 K2 Br1 91.600(4) 25_565 27 ?
Br1 K2 Br1 88.401(4) . 27 ?
Br1 K2 Br1 88.401(4) 2_665 27 ?
Br1 K2 Br1 180.0 3_565 27 ?
Br1 K2 K1 55.874(3) 26_455 25_565 ?
Br1 K2 K1 55.876(3) 25_565 25_565 ?
Br1 K2 K1 124.126(3) . 25_565 ?
Br1 K2 K1 124.128(3) 2_665 25_565 ?
Br1 K2 K1 124.122(3) 3_565 25_565 ?
Br1 K2 K1 55.876(3) 27 25_565 ?
Br1 K2 K1 124.124(3) 26_455 . ?
Br1 K2 K1 124.124(3) 25_565 . ?
Br1 K2 K1 55.874(3) . . ?
Br1 K2 K1 55.874(3) 2_665 . ?
Br1 K2 K1 55.876(3) 3_565 . ?
Br1 K2 K1 124.126(3) 27 . ?
K1 K2 K1 180.0 25_565 . ?
Br2 K1 Br2 89.354(12) 3_565 2_665 ?
Br2 K1 Br2 89.352(12) 3_565 . ?
Br2 K1 Br2 89.352(12) 2_665 . ?
Br2 K1 Br1 96.194(4) 3_565 . ?
Br2 K1 Br1 173.654(5) 2_665 . ?
Br2 K1 Br1 87.638(4) . . ?
Br2 K1 Br1 173.656(5) 3_565 2_665 ?
Br2 K1 Br1 87.637(3) 2_665 2_665 ?
Br2 K1 Br1 96.195(4) . 2_665 ?
Br1 K1 Br1 87.136(12) . 2_665 ?
Br2 K1 Br1 87.638(3) 3_565 3_565 ?
Br2 K1 Br1 96.196(4) 2_665 3_565 ?
Br2 K1 Br1 173.655(5) . 3_565 ?
Br1 K1 Br1 87.135(12) . 3_565 ?
Br1 K1 Br1 87.136(12) 2_665 3_565 ?
Br2 K1 K1 54.277(9) 3_565 10_455 ?
Br2 K1 K1 54.280(9) 2_665 10_455 ?
Br2 K1 K1 54.281(9) . 10_455 ?
Br1 K1 K1 127.266(8) . 10_455 ?
Br1 K1 K1 127.268(9) 2_665 10_455 ?
Br1 K1 K1 127.264(9) 3_565 10_455 ?
Br2 K1 K2 125.721(9) 3_565 . ?
Br2 K1 K2 125.720(9) 2_665 . ?
Br2 K1 K2 125.721(9) . . ?
Br1 K1 K2 52.734(9) . . ?
Br1 K1 K2 52.734(9) 2_665 . ?
Br1 K1 K2 52.734(8) 3_565 . ?
K1 K1 K2 180.0 10_455 . ?
C2 N1 C3 110.30(14) . . ?
C2 N1 C1 110.83(15) . . ?
C3 N1 C1 110.20(14) . . ?
C2 N1 H1 108.5 . . ?
C3 N1 H1 108.5 . . ?
C1 N1 H1 108.5 . . ?
N1 C3 C1 108.53(13) . 4 ?
N1 C3 H3A 110.0 . . ?
C1 C3 H3A 110.0 4 . ?
N1 C3 H3B 110.0 . . ?
C1 C3 H3B 110.0 4 . ?
H3A C3 H3B 108.4 . . ?
N1 C1 C3 108.22(13) . 4 ?
N1 C1 H1A 110.1 . . ?
C3 C1 H1A 110.1 4 . ?
N1 C1 H1B 110.1 . . ?
C3 C1 H1B 110.1 4 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C2 108.57(10) . 4 ?
N1 C2 H2A 110.0 . . ?
C2 C2 H2A 110.0 4 . ?
N1 C2 H2B 110.0 . . ?
C2 C2 H2B 110.0 4 . ?
H2A C2 H2B 108.4 . . ?

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
C2 N1 C3 C1 -59.52(18) . . . 4 ?
C1 N1 C3 C1 63.17(16) . . . 4 ?
C2 N1 C1 C3 62.53(18) . . . 4 ?
C3 N1 C1 C3 -59.85(17) . . . 4 ?
C3 N1 C2 C2 63.5(2) . . . 4 ?
C1 N1 C2 C2 -58.8(3) . . . 4 ?

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
C3 H3A Br2 0.99 2.91 3.8407(19) 157.1 31 yes
C3 H3B Br2 0.99 2.90 3.8636(18) 164.1 . yes
C1 H1A Br1 0.99 2.94 3.8838(19) 159.2 27 yes
C1 H1B Br2 0.99 3.02 3.9169(19) 151.8 31 yes
C2 H2B Br1 0.99 3.10 3.6319(19) 115.1 2_665 yes
N1 H1 Br1 1.00 2.19 3.1852(14) 174.2 . yes
C3 H3A Br2 0.99 2.91 3.8407(19) 157.1 31 yes
C3 H3B Br2 0.99 2.90 3.8636(18) 164.1 . yes
C1 H1A Br1 0.99 2.94 3.8838(19) 159.2 27 yes
C1 H1B Br2 0.99 3.02 3.9169(19) 151.8 31 yes
C2 H2B Br1 0.99 3.10 3.6319(19) 115.1 2_665 yes

_refine_diff_density_max         0.508
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_DKI3
_database_code_depnum_ccdc_archive 'CCDC 2381385'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2025-03-19 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT034_shelx               
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do !  
RESPONSE: Twinning involves inversion, so Flack parameter cannot be determined.
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor  N1       --H1       .     Please Check 
RESPONSE: N1 is involved in H bonding, the lengths exceed ShelX definition.
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(I K0.33), 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 I3 K N2'
_chemical_formula_weight         533.99

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2 :H'
_space_group_name_Hall           'R 3 2"'

_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, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   9.6698(7)
_cell_length_b                   9.6698(7)
_cell_length_c                   12.2899(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     995.21(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    3301
_cell_measurement_theta_min      2.9080
_cell_measurement_theta_max      30.4760

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.673
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    7.342
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4000
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.943
_diffrn_reflns_theta_max         30.897
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             608
_reflns_number_gt                594
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_max     0.908
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+89.3544P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_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_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         608
_refine_ls_number_parameters     17
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_restrained_S_all      1.296
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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
I1 I 0.52841(18) 0.52841(18) 0.500000 0.0381(7) Uani 1 2 d S T P . .
K1 K 0.666667 0.333333 0.333333 0.0196(18) Uani 1 6 d S T P . .
N1 N 0.333333 0.666667 0.268(2) 0.031(4) Uani 1 3 d S T P . .
H1 H 0.333334 0.666667 0.349387 0.037 Uiso 1 3 calc R U P . .
C1 C 0.320(3) 0.516(3) 0.2288(16) 0.031(4) Uani 1 1 d . . . . .
H1A H 0.212575 0.425103 0.245889 0.037 Uiso 1 1 calc R U . . .
H1B H 0.400656 0.497495 0.264920 0.037 Uiso 1 1 calc R U . . .


_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
I1 K1 3.4732(2) . ?
I1 K1 3.4733(2) 7_455 ?
N1 C1 1.48(2) 3_565 ?
N1 C1 1.48(2) 2_665 ?
N1 C1 1.48(2) . ?
C1 C1 1.54(4) 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
K1 I1 K1 170.93(6) . 7_455 ?
I1 K1 I1 97.93(4) 3_665 14_654 ?
I1 K1 I1 170.93(6) 3_665 15_554 ?
I1 K1 I1 88.756(5) 14_654 15_554 ?
I1 K1 I1 88.756(5) 3_665 2_655 ?
I1 K1 I1 170.93(6) 14_654 2_655 ?
I1 K1 I1 85.29(4) 15_554 2_655 ?
I1 K1 I1 88.756(5) 3_665 . ?
I1 K1 I1 85.29(4) 14_654 . ?
I1 K1 I1 97.94(4) 15_554 . ?
I1 K1 I1 88.757(5) 2_655 . ?
I1 K1 I1 85.29(4) 3_665 13_544 ?
I1 K1 I1 88.755(5) 14_654 13_544 ?
I1 K1 I1 88.755(5) 15_554 13_544 ?
I1 K1 I1 97.93(4) 2_655 13_544 ?
I1 K1 I1 170.93(6) . 13_544 ?
C1 N1 C1 109.9(13) 3_565 2_665 ?
C1 N1 C1 109.9(13) 3_565 . ?
C1 N1 C1 109.9(13) 2_665 . ?
N1 C1 C1 108.1(14) . 12 ?

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
C1 H1A I1 0.99 3.14 4.01(2) 147.6 13_444 yes
C1 H1B I1 0.99 3.10 3.87(2) 135.5 . yes
C1 H1A I1 0.99 3.14 4.01(2) 147.6 13_444 yes
C1 H1B I1 0.99 3.10 3.87(2) 135.5 . yes

_refine_diff_density_max         1.954
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.360

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2381389'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 Na, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cl3 N2 Na'
_chemical_formula_weight         243.53
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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

_cell_length_a                   15.87470(10)
_cell_length_b                   15.87470(10)
_cell_length_c                   21.1921(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4625.04(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    149.98(10)
_cell_measurement_reflns_used    21668
_cell_measurement_theta_min      5.2450
_cell_measurement_theta_max      76.0790

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_F_000             2268.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    8.077
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.98(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29780
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         5.270
_diffrn_reflns_theta_max         74.370
_diffrn_reflns_theta_full        67.684
_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             1061
_reflns_number_gt                1045
_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_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_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)+(0.0626P)²+3.4787P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1061
_refine_ls_number_parameters     61
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.35959(2) 0.53695(2) 0.58789(2) 0.01669(17) Uani 1 1 d . . . . .
N1 N 0.57641(9) 0.61612(9) 0.58366(5) 0.0157(3) Uani 1 1 d . . . . .
Cl2 Cl 0.333333 0.81231(3) 0.416667 0.01979(18) Uani 1 2 d S T P . .
Na2 Na 0.333333 0.666667 0.666667 0.0162(3) Uani 1 6 d S T P . .
Na1 Na 0.333333 0.666667 0.49781(4) 0.0193(2) Uani 1 3 d S T P . .
C2 C 0.61126(10) 0.58948(10) 0.64161(6) 0.0184(3) Uani 1 1 d . . . . .
H2B H 0.586104 0.519829 0.642679 0.022 Uiso 1 1 calc R U . . .
H2A H 0.588579 0.607521 0.678946 0.022 Uiso 1 1 calc R U . . .
C1 C 0.61060(10) 0.58767(10) 0.52628(6) 0.0188(3) Uani 1 1 d . . . . .
H1A H 0.585073 0.601928 0.488715 0.023 Uiso 1 1 calc R U . . .
H1B H 0.587569 0.518409 0.527099 0.023 Uiso 1 1 calc R U . . .
C3 C 0.61098(11) 0.72239(11) 0.58288(8) 0.0228(3) Uani 1 1 d . . . . .
H3B H 0.586164 0.739810 0.619439 0.027 Uiso 1 1 calc R U . . .
H3A H 0.587608 0.738952 0.545228 0.027 Uiso 1 1 calc R U . . .
H1 H 0.5096(16) 0.5840(13) 0.5856(8) 0.031(5) Uiso 1 1 d . . . . .


_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 Na2 2.8389(3) . ?
Cl1 Na1 2.9861(6) . ?
N1 C2 1.4924(17) . ?
N1 C3 1.4905(18) . ?
N1 C1 1.4906(17) . ?
N1 H1 0.92(2) . ?
Cl2 Na1 2.8812(6) 10_455 ?
Cl2 Na1 2.8813(6) . ?
Na2 Na1 3.5785(9) . ?
Na2 Na1 3.5786(9) 25_566 ?
Na1 Na1 3.4390(17) 10_455 ?
C2 C1 1.5330(19) 18_655 ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C3 1.531(3) 18_655 ?
C3 H3B 0.9700 . ?
C3 H3A 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na2 Cl1 Na1 75.761(15) . . ?
C2 N1 C3 110.55(11) . . ?
C2 N1 C1 110.04(11) . . ?
C3 N1 C1 110.49(11) . . ?
C2 N1 H1 107.2(12) . . ?
C3 N1 H1 107.3(12) . . ?
C1 N1 H1 111.2(11) . . ?
Na1 Cl2 Na1 73.28(3) 10_455 . ?
Cl1 Na2 Cl1 91.074(10) 27_556 2_665 ?
Cl1 Na2 Cl1 91.074(10) 27_556 . ?
Cl1 Na2 Cl1 88.926(10) 2_665 . ?
Cl1 Na2 Cl1 88.925(10) 27_556 25_566 ?
Cl1 Na2 Cl1 91.075(10) 2_665 25_566 ?
Cl1 Na2 Cl1 180.0 . 25_566 ?
Cl1 Na2 Cl1 88.925(10) 27_556 26_456 ?
Cl1 Na2 Cl1 180.0 2_665 26_456 ?
Cl1 Na2 Cl1 91.075(10) . 26_456 ?
Cl1 Na2 Cl1 88.924(10) 25_566 26_456 ?
Cl1 Na2 Cl1 180.0 27_556 3_565 ?
Cl1 Na2 Cl1 88.925(10) 2_665 3_565 ?
Cl1 Na2 Cl1 88.927(10) . 3_565 ?
Cl1 Na2 Cl1 91.075(10) 25_566 3_565 ?
Cl1 Na2 Cl1 91.076(10) 26_456 3_565 ?
Cl1 Na2 Na1 126.020(7) 27_556 . ?
Cl1 Na2 Na1 53.980(7) 2_665 . ?
Cl1 Na2 Na1 53.980(7) . . ?
Cl1 Na2 Na1 126.022(7) 25_566 . ?
Cl1 Na2 Na1 126.022(7) 26_456 . ?
Cl1 Na2 Na1 53.980(7) 3_565 . ?
Cl1 Na2 Na1 53.981(7) 27_556 25_566 ?
Cl1 Na2 Na1 126.020(7) 2_665 25_566 ?
Cl1 Na2 Na1 126.023(7) . 25_566 ?
Cl1 Na2 Na1 53.976(7) 25_566 25_566 ?
Cl1 Na2 Na1 53.978(7) 26_456 25_566 ?
Cl1 Na2 Na1 126.019(7) 3_565 25_566 ?
Na1 Na2 Na1 180.0 . 25_566 ?
Cl2 Na1 Cl2 88.04(2) . 3_565 ?
Cl2 Na1 Cl2 88.04(2) . 2_665 ?
Cl2 Na1 Cl2 88.04(2) 3_565 2_665 ?
Cl2 Na1 Cl1 89.590(7) . 2_665 ?
Cl2 Na1 Cl1 99.257(7) 3_565 2_665 ?
Cl2 Na1 Cl1 172.248(13) 2_665 2_665 ?
Cl2 Na1 Cl1 172.249(13) . . ?
Cl2 Na1 Cl1 89.590(7) 3_565 . ?
Cl2 Na1 Cl1 99.259(7) 2_665 . ?
Cl1 Na1 Cl1 83.51(2) 2_665 . ?
Cl2 Na1 Cl1 99.256(7) . 3_565 ?
Cl2 Na1 Cl1 172.250(13) 3_565 3_565 ?
Cl2 Na1 Cl1 89.590(7) 2_665 3_565 ?
Cl1 Na1 Cl1 83.51(2) 2_665 3_565 ?
Cl1 Na1 Cl1 83.51(2) . 3_565 ?
Cl2 Na1 Na1 53.358(15) . 10_455 ?
Cl2 Na1 Na1 53.362(15) 3_565 10_455 ?
Cl2 Na1 Na1 53.359(15) 2_665 10_455 ?
Cl1 Na1 Na1 129.740(14) 2_665 10_455 ?
Cl1 Na1 Na1 129.742(14) . 10_455 ?
Cl1 Na1 Na1 129.737(14) 3_565 10_455 ?
Cl2 Na1 Na2 126.640(15) . . ?
Cl2 Na1 Na2 126.640(15) 3_565 . ?
Cl2 Na1 Na2 126.641(15) 2_665 . ?
Cl1 Na1 Na2 50.260(14) 2_665 . ?
Cl1 Na1 Na2 50.260(14) . . ?
Cl1 Na1 Na2 50.261(14) 3_565 . ?
Na1 Na1 Na2 180.0 10_455 . ?
N1 C2 C1 108.31(11) . 18_655 ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 18_655 . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 18_655 . ?
H2B C2 H2A 108.4 . . ?
N1 C1 C2 108.76(10) . 18_655 ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 18_655 . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 18_655 . ?
H1A C1 H1B 108.3 . . ?
N1 C3 C3 108.58(7) . 18_655 ?
N1 C3 H3B 110.0 . . ?
C3 C3 H3B 110.0 18_655 . ?
N1 C3 H3A 110.0 . . ?
C3 C3 H3A 110.0 18_655 . ?
H3B C3 H3A 108.4 . . ?

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
C3 N1 C2 C1 -62.19(14) . . . 18_655 ?
C1 N1 C2 C1 60.14(13) . . . 18_655 ?
C2 N1 C1 C2 -62.55(13) . . . 18_655 ?
C3 N1 C1 C2 59.81(14) . . . 18_655 ?
C2 N1 C3 C3 60.04(19) . . . 18_655 ?
C1 N1 C3 C3 -62.02(19) . . . 18_655 ?

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
C2 H2B Cl2 0.97 2.89 3.7797(14) 152.9 21_656 yes
C2 H2A Cl1 0.97 2.91 3.8035(15) 154.3 27_556 yes
C1 H1A Cl2 0.97 2.82 3.7356(15) 157.6 3_565 yes
C1 H1B Cl2 0.97 2.84 3.7476(15) 156.1 21_656 yes
C3 H3B Cl1 0.97 2.93 3.4345(15) 113.8 2_665 yes
N1 H1 Cl1 0.92(2) 2.11(2) 3.0180(12) 169.1(17) . yes

_refine_diff_density_max         0.261
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.052

####################################################################### 
# 
# 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_DCsCl3
_database_code_depnum_ccdc_archive 'CCDC 2381386'
loop_
_audit_author_name
_audit_author_address
'Melanie Rademeyer'
;University of Pretoria
South Africa
;
_audit_update_record             
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl12 Cs4, 4(C6 H14 N2)'
_chemical_formula_sum            'C24 H56 Cl12 Cs4 N8'
_chemical_formula_weight         1413.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;

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                   41.1638(16)
_cell_length_b                   9.48990(10)
_cell_length_c                   32.6647(13)
_cell_angle_alpha                90
_cell_angle_beta                 131.638(7)
_cell_angle_gamma                90
_cell_volume                     9536.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    149.99(10)
_cell_measurement_reflns_used    47010
_cell_measurement_theta_min      2.2840
_cell_measurement_theta_max      31.0460

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             5440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.735
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.99(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            135520
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.981
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13501
_reflns_number_gt                11485
_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 1.171.40.23a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_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)+(0.0261P)²+14.1687P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.000053(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13501
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.003
_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
Cs1 Cs 0.000000 0.000000 0.500000 0.01662(5) Uani 1 2 d S . P . .
Cs3 Cs -0.24893(2) 0.99898(2) 0.12508(2) 0.01635(4) Uani 1 1 d . . . . .
Cs5 Cs -0.500000 -0.00842(2) -0.250000 0.01630(5) Uani 1 2 d S T P . .
Cs2 Cs -0.12375(2) 0.49488(2) 0.31283(2) 0.01618(4) Uani 1 1 d . . . . .
Cs4 Cs -0.37176(2) 0.48660(2) -0.05989(2) 0.01625(4) Uani 1 1 d . . . . .
Cl12 Cl -0.44859(2) 0.28064(4) -0.16833(2) 0.01784(9) Uani 1 1 d . . . . .
Cl7 Cl -0.17233(2) 0.79576(4) 0.23728(2) 0.01876(9) Uani 1 1 d . . . . .
Cl5 Cl -0.19732(2) 0.30133(4) 0.19778(2) 0.01912(9) Uani 1 1 d . . . . .
Cl1 Cl -0.06657(2) -0.26992(4) 0.41754(2) 0.02031(9) Uani 1 1 d . . . . .
Cl2 Cl 0.07677(2) -0.03371(5) 0.48936(2) 0.01902(9) Uani 1 1 d . . . . .
Cl4 Cl -0.19928(2) 0.45793(5) 0.32617(2) 0.02195(9) Uani 1 1 d . . . . .
Cl9 Cl -0.29819(2) 0.74107(5) 0.02702(2) 0.02124(9) Uani 1 1 d . . . . .
Cl11 Cl -0.43773(2) 0.75860(4) -0.14353(2) 0.02050(9) Uani 1 1 d . . . . .
Cl8 Cl -0.17831(2) 1.04672(4) 0.10803(2) 0.01921(9) Uani 1 1 d . . . . .
Cl6 Cl -0.06137(2) 0.53911(5) 0.28266(2) 0.02056(10) Uani 1 1 d . . . . .
Cl3 Cl -0.05379(2) 0.24227(5) 0.39947(2) 0.02730(11) Uani 1 1 d . . . . .
Cl10 Cl -0.32747(2) 1.20745(5) 0.02310(2) 0.02684(10) Uani 1 1 d . . . . .
N8 N -0.72196(5) 0.50394(15) -0.20631(6) 0.0184(3) Uani 1 1 d . . . . .
H8 H -0.748406 0.501979 -0.245167 0.022 Uiso 1 1 calc R U . . .
N4 N -0.47000(5) 0.56669(16) 0.20822(6) 0.0189(3) Uani 1 1 d . . . . .
H4 H -0.494350 0.619304 0.199675 0.023 Uiso 1 1 calc R U . . .
N3 N -0.40824(5) 0.43388(16) 0.23001(6) 0.0193(3) Uani 1 1 d . . . . .
H3 H -0.383883 0.381374 0.238522 0.023 Uiso 1 1 calc R U . . .
N1 N -0.43806(5) 1.05673(17) 0.00106(7) 0.0234(3) Uani 1 1 d . . . . .
H1 H -0.436064 1.110631 0.028261 0.028 Uiso 1 1 calc R U . . .
N2 N -0.44226(6) 0.92124(17) -0.06682(7) 0.0240(4) Uani 1 1 d . . . . .
H2 H -0.443697 0.867860 -0.093671 0.029 Uiso 1 1 calc R U . . .
N5 N -0.68551(5) -0.06502(17) 0.12435(6) 0.0206(3) Uani 1 1 d . . . . .
H5 H -0.687032 -0.118702 0.148670 0.025 Uiso 1 1 calc R U . . .
N6 N -0.68183(5) 0.07075(16) 0.06284(6) 0.0203(3) Uani 1 1 d . . . . .
H6 H -0.680468 0.124887 0.038466 0.024 Uiso 1 1 calc R U . . .
N7 N -0.65520(6) 0.50949(18) -0.10835(7) 0.0253(4) Uani 1 1 d . . . . .
H7 H -0.628651 0.510224 -0.069538 0.030 Uiso 1 1 calc R U . . .
C23 C -0.64379(6) -0.09919(19) 0.13810(7) 0.0202(4) Uani 1 1 d . . . . .
H23A H -0.640647 -0.200466 0.138015 0.024 Uiso 1 1 calc R U . . .
H23B H -0.619411 -0.063667 0.174265 0.024 Uiso 1 1 calc R U . . .
C10 C -0.43170(7) 0.66286(19) 0.23560(8) 0.0239(4) Uani 1 1 d . . . . .
H10A H -0.419605 0.685339 0.272362 0.029 Uiso 1 1 calc R U . . .
H10B H -0.440537 0.749977 0.215084 0.029 Uiso 1 1 calc R U . . .
C11 C -0.45813(6) 0.44765(19) 0.24602(7) 0.0195(4) Uani 1 1 d . . . . .
H11A H -0.480558 0.375847 0.226578 0.023 Uiso 1 1 calc R U . . .
H11B H -0.455346 0.481453 0.276249 0.023 Uiso 1 1 calc R U . . .
C12 C -0.41499(6) 0.38620(18) 0.26754(7) 0.0186(4) Uani 1 1 d . . . . .
H12A H -0.391408 0.419188 0.304510 0.022 Uiso 1 1 calc R U . . .
H12B H -0.415810 0.284112 0.268104 0.022 Uiso 1 1 calc R U . . .
C14 C -0.70982(6) 0.65412(18) -0.18783(7) 0.0191(4) Uani 1 1 d . . . . .
H14A H -0.734017 0.703180 -0.195477 0.023 Uiso 1 1 calc R U . . .
H14B H -0.702680 0.701502 -0.207294 0.023 Uiso 1 1 calc R U . . .
C4 C -0.47715(6) 0.87007(19) -0.06809(7) 0.0194(4) Uani 1 1 d . . . . .
H4A H -0.472216 0.772025 -0.056973 0.023 Uiso 1 1 calc R U . . .
H4B H -0.505257 0.877720 -0.104896 0.023 Uiso 1 1 calc R U . . .
C7 C -0.48300(7) 0.5102(2) 0.15643(8) 0.0240(4) Uani 1 1 d . . . . .
H7A H -0.485336 0.586445 0.134814 0.029 Uiso 1 1 calc R U . . .
H7B H -0.510986 0.463595 0.134886 0.029 Uiso 1 1 calc R U . . .
C8 C -0.44826(7) 0.4057(2) 0.17190(8) 0.0248(4) Uani 1 1 d . . . . .
H8A H -0.458170 0.309907 0.168128 0.030 Uiso 1 1 calc R U . . .
H8B H -0.442180 0.417413 0.148048 0.030 Uiso 1 1 calc R U . . .
C9 C -0.39789(6) 0.5875(2) 0.23777(8) 0.0232(4) Uani 1 1 d . . . . .
H9A H -0.398857 0.622387 0.209066 0.028 Uiso 1 1 calc R U . . .
H9B H -0.368987 0.603940 0.272842 0.028 Uiso 1 1 calc R U . . .
C15 C -0.73037(7) 0.4285(2) -0.17408(8) 0.0238(4) Uani 1 1 d . . . . .
H15A H -0.740864 0.333926 -0.188293 0.029 Uiso 1 1 calc R U . . .
H15B H -0.752203 0.478202 -0.176541 0.029 Uiso 1 1 calc R U . . .
C3 C -0.47616(6) 0.96136(19) -0.02849(8) 0.0210(4) Uani 1 1 d . . . . .
H3A H -0.502695 1.016117 -0.048693 0.025 Uiso 1 1 calc R U . . .
H3B H -0.473964 0.901911 -0.002589 0.025 Uiso 1 1 calc R U . . .
C19 C -0.64461(7) -0.0300(2) 0.09502(8) 0.0236(4) Uani 1 1 d . . . . .
H19A H -0.617544 0.019547 0.112732 0.028 Uiso 1 1 calc R U . . .
H19B H -0.648164 -0.101211 0.070994 0.028 Uiso 1 1 calc R U . . .
C24 C -0.68700(8) 0.0878(2) 0.13286(9) 0.0325(5) Uani 1 1 d . . . . .
H24A H -0.665164 0.110441 0.171525 0.039 Uiso 1 1 calc R U . . .
H24B H -0.715307 0.112434 0.120111 0.039 Uiso 1 1 calc R U . . .
C21 C -0.72401(7) -0.0065(2) 0.02897(8) 0.0274(4) Uani 1 1 d . . . . .
H21A H -0.728057 -0.060147 0.000594 0.033 Uiso 1 1 calc R U . . .
H21B H -0.747878 0.059685 0.011570 0.033 Uiso 1 1 calc R U . . .
C22 C -0.72310(6) -0.1051(2) 0.06650(8) 0.0258(4) Uani 1 1 d . . . . .
H22A H -0.749993 -0.097087 0.059304 0.031 Uiso 1 1 calc R U . . .
H22B H -0.720025 -0.201952 0.059992 0.031 Uiso 1 1 calc R U . . .
C2 C -0.39863(7) 0.9016(2) -0.01187(10) 0.0323(5) Uani 1 1 d . . . . .
H2A H -0.376621 0.942418 -0.011088 0.039 Uiso 1 1 calc R U . . .
H2B H -0.392483 0.801839 -0.003718 0.039 Uiso 1 1 calc R U . . .
C16 C -0.68622(7) 0.4316(2) -0.19907(8) 0.0241(4) Uani 1 1 d . . . . .
H16A H -0.692698 0.332001 -0.207307 0.029 Uiso 1 1 calc R U . . .
H16B H -0.683190 0.471752 -0.223688 0.029 Uiso 1 1 calc R U . . .
C13 C -0.67079(7) 0.6555(2) -0.12666(8) 0.0299(5) Uani 1 1 d . . . . .
H13A H -0.647888 0.713460 -0.118995 0.036 Uiso 1 1 calc R U . . .
H13B H -0.678977 0.694672 -0.107190 0.036 Uiso 1 1 calc R U . . .
C20 C -0.67841(8) 0.1701(2) 0.10096(9) 0.0318(5) Uani 1 1 d . . . . .
H20A H -0.699522 0.245390 0.080405 0.038 Uiso 1 1 calc R U . . .
H20B H -0.649601 0.211607 0.125937 0.038 Uiso 1 1 calc R U . . .
C5 C -0.44277(8) 1.1563(2) -0.03761(10) 0.0350(5) Uani 1 1 d . . . . .
H5A H -0.416821 1.213729 -0.018318 0.042 Uiso 1 1 calc R U . . .
H5B H -0.467352 1.218173 -0.053484 0.042 Uiso 1 1 calc R U . . .
C1 C -0.39770(8) 0.9717(3) 0.02982(9) 0.0416(6) Uani 1 1 d . . . . .
H1A H -0.395935 0.901208 0.052745 0.050 Uiso 1 1 calc R U . . .
H1B H -0.372396 1.032228 0.053033 0.050 Uiso 1 1 calc R U . . .
C6 C -0.44964(9) 1.0735(2) -0.08213(9) 0.0407(6) Uani 1 1 d . . . . .
H6A H -0.479010 1.087523 -0.116724 0.049 Uiso 1 1 calc R U . . .
H6B H -0.429498 1.104979 -0.086200 0.049 Uiso 1 1 calc R U . . .
C17 C -0.64514(8) 0.4511(3) -0.14099(11) 0.0555(8) Uani 1 1 d . . . . .
H17A H -0.630401 0.361252 -0.125750 0.067 Uiso 1 1 calc R U . . .
H17B H -0.625974 0.514851 -0.139529 0.067 Uiso 1 1 calc R U . . .
C18 C -0.68828(11) 0.4226(4) -0.11553(11) 0.0699(11) Uani 1 1 d . . . . .
H18A H -0.692802 0.456738 -0.091650 0.084 Uiso 1 1 calc R U . . .
H18B H -0.678284 0.325786 -0.105545 0.084 Uiso 1 1 calc R U . . .


_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
Cs1 Cl3 3.3630(5) . ?
Cs1 Cl3 3.3630(5) 5_556 ?
Cs1 Cl1 3.3937(5) . ?
Cs1 Cl1 3.3938(5) 5_556 ?
Cs1 Cl2 3.4162(5) . ?
Cs1 Cl2 3.4163(5) 5_556 ?
Cs3 Cl8 3.3343(5) . ?
Cs3 Cl10 3.3392(6) . ?
Cs3 Cl5 3.4179(5) 1_565 ?
Cs3 Cl9 3.4252(5) . ?
Cs3 Cl7 3.4259(5) . ?
Cs3 Cl4 3.4269(5) 4_455 ?
Cs5 Cl6 3.3444(4) 8_455 ?
Cs5 Cl6 3.3444(4) 7_455 ?
Cs5 Cl12 3.4085(5) . ?
Cs5 Cl12 3.4086(5) 2_454 ?
Cs5 Cl11 3.4216(5) 2_444 ?
Cs5 Cl11 3.4216(5) 1_545 ?
Cs2 Cl6 3.3324(4) . ?
Cs2 Cl3 3.3496(5) . ?
Cs2 Cl1 3.3946(5) 1_565 ?
Cs2 Cl5 3.3977(5) . ?
Cs2 Cl7 3.4183(5) . ?
Cs2 Cl4 3.4321(5) . ?
Cs4 Cl10 3.3351(5) 1_545 ?
Cs4 Cl8 3.3362(5) 7_465 ?
Cs4 Cl12 3.3887(5) . ?
Cs4 Cl9 3.4113(5) . ?
Cs4 Cl11 3.4121(5) . ?
Cs4 Cl2 3.4356(5) 8_455 ?
N8 C15 1.492(2) . ?
N8 C16 1.493(2) . ?
N8 C14 1.498(2) . ?
N8 H8 0.9800 . ?
N4 C7 1.494(2) . ?
N4 C11 1.496(2) . ?
N4 C10 1.498(2) . ?
N4 H4 0.9800 . ?
N3 C9 1.493(2) . ?
N3 C8 1.494(2) . ?
N3 C12 1.496(2) . ?
N3 H3 0.9800 . ?
N1 C3 1.483(2) . ?
N1 C5 1.484(3) . ?
N1 C1 1.490(3) . ?
N1 H1 0.9800 . ?
N2 C2 1.483(3) . ?
N2 C4 1.490(2) . ?
N2 C6 1.492(3) . ?
N2 H2 0.9800 . ?
N5 C24 1.485(3) . ?
N5 C22 1.492(2) . ?
N5 C23 1.494(2) . ?
N5 H5 0.9800 . ?
N6 C21 1.491(3) . ?
N6 C20 1.492(2) . ?
N6 C19 1.492(2) . ?
N6 H6 0.9800 . ?
N7 C18 1.472(3) . ?
N7 C13 1.476(3) . ?
N7 C17 1.484(3) . ?
N7 H7 0.9800 . ?
C23 C19 1.533(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C10 C9 1.524(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.526(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 C13 1.519(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 C3 1.535(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 C8 1.524(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C15 C18 1.503(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C24 C20 1.520(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C21 C22 1.523(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C2 C1 1.493(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C16 C17 1.493(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C5 C6 1.505(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Cs1 Cl3 179.999(19) . 5_556 ?
Cl3 Cs1 Cl1 94.616(13) . . ?
Cl3 Cs1 Cl1 85.385(14) 5_556 . ?
Cl3 Cs1 Cl1 85.385(14) . 5_556 ?
Cl3 Cs1 Cl1 94.614(13) 5_556 5_556 ?
Cl1 Cs1 Cl1 179.999(18) . 5_556 ?
Cl3 Cs1 Cl2 91.032(13) . . ?
Cl3 Cs1 Cl2 88.967(13) 5_556 . ?
Cl1 Cs1 Cl2 99.343(11) . . ?
Cl1 Cs1 Cl2 80.657(11) 5_556 . ?
Cl3 Cs1 Cl2 88.968(12) . 5_556 ?
Cl3 Cs1 Cl2 91.033(13) 5_556 5_556 ?
Cl1 Cs1 Cl2 80.657(11) . 5_556 ?
Cl1 Cs1 Cl2 99.343(11) 5_556 5_556 ?
Cl2 Cs1 Cl2 180.0 . 5_556 ?
Cl8 Cs3 Cl10 97.269(13) . . ?
Cl8 Cs3 Cl5 78.079(11) . 1_565 ?
Cl10 Cs3 Cl5 86.483(14) . 1_565 ?
Cl8 Cs3 Cl9 88.912(12) . . ?
Cl10 Cs3 Cl9 84.909(14) . . ?
Cl5 Cs3 Cl9 163.361(11) 1_565 . ?
Cl8 Cs3 Cl7 88.290(12) . . ?
Cl10 Cs3 Cl7 173.483(12) . . ?
Cl5 Cs3 Cl7 91.366(13) 1_565 . ?
Cl9 Cs3 Cl7 98.647(13) . . ?
Cl8 Cs3 Cl4 166.817(12) . 4_455 ?
Cl10 Cs3 Cl4 92.413(13) . 4_455 ?
Cl5 Cs3 Cl4 93.674(11) 1_565 4_455 ?
Cl9 Cs3 Cl4 100.885(12) . 4_455 ?
Cl7 Cs3 Cl4 81.578(11) . 4_455 ?
Cl6 Cs5 Cl6 170.009(17) 8_455 7_455 ?
Cl6 Cs5 Cl12 91.617(11) 8_455 . ?
Cl6 Cs5 Cl12 96.427(11) 7_455 . ?
Cl6 Cs5 Cl12 96.426(11) 8_455 2_454 ?
Cl6 Cs5 Cl12 91.618(11) 7_455 2_454 ?
Cl12 Cs5 Cl12 72.821(16) . 2_454 ?
Cl6 Cs5 Cl11 93.059(12) 8_455 2_444 ?
Cl6 Cs5 Cl11 80.451(12) 7_455 2_444 ?
Cl12 Cs5 Cl11 166.360(11) . 2_444 ?
Cl12 Cs5 Cl11 93.914(12) 2_454 2_444 ?
Cl6 Cs5 Cl11 80.451(12) 8_455 1_545 ?
Cl6 Cs5 Cl11 93.059(12) 7_455 1_545 ?
Cl12 Cs5 Cl11 93.915(13) . 1_545 ?
Cl12 Cs5 Cl11 166.361(11) 2_454 1_545 ?
Cl11 Cs5 Cl11 99.493(17) 2_444 1_545 ?
Cl6 Cs2 Cl3 86.623(13) . . ?
Cl6 Cs2 Cl1 93.471(12) . 1_565 ?
Cl3 Cs2 Cl1 89.310(14) . 1_565 ?
Cl6 Cs2 Cl5 92.098(12) . . ?
Cl3 Cs2 Cl5 100.471(14) . . ?
Cl1 Cs2 Cl5 169.015(12) 1_565 . ?
Cl6 Cs2 Cl7 82.955(11) . . ?
Cl3 Cs2 Cl7 165.923(12) . . ?
Cl1 Cs2 Cl7 81.928(13) 1_565 . ?
Cl5 Cs2 Cl7 89.375(13) . . ?
Cl6 Cs2 Cl4 172.520(11) . . ?
Cl3 Cs2 Cl4 99.353(13) . . ?
Cl1 Cs2 Cl4 91.110(12) 1_565 . ?
Cl5 Cs2 Cl4 82.435(12) . . ?
Cl7 Cs2 Cl4 91.849(12) . . ?
Cl10 Cs4 Cl8 97.616(12) 1_545 7_465 ?
Cl10 Cs4 Cl12 91.031(13) 1_545 . ?
Cl8 Cs4 Cl12 83.822(11) 7_465 . ?
Cl10 Cs4 Cl9 100.501(14) 1_545 . ?
Cl8 Cs4 Cl9 88.536(12) 7_465 . ?
Cl12 Cs4 Cl9 166.932(11) . . ?
Cl10 Cs4 Cl11 165.055(13) 1_545 . ?
Cl8 Cs4 Cl11 96.114(11) 7_465 . ?
Cl12 Cs4 Cl11 84.597(13) . . ?
Cl9 Cs4 Cl11 85.700(14) . . ?
Cl10 Cs4 Cl2 84.085(12) 1_545 8_455 ?
Cl8 Cs4 Cl2 177.962(11) 7_465 8_455 ?
Cl12 Cs4 Cl2 97.294(11) . 8_455 ?
Cl9 Cs4 Cl2 90.051(11) . 8_455 ?
Cl11 Cs4 Cl2 82.314(11) . 8_455 ?
Cs4 Cl12 Cs5 160.951(15) . . ?
Cs2 Cl7 Cs3 157.469(15) . . ?
Cs2 Cl5 Cs3 155.242(14) . 1_545 ?
Cs1 Cl1 Cs2 161.737(15) . 1_545 ?
Cs1 Cl2 Cs4 159.284(15) . 8_556 ?
Cs3 Cl4 Cs2 160.575(16) 4_445 . ?
Cs4 Cl9 Cs3 158.545(16) . . ?
Cs4 Cl11 Cs5 164.339(15) . 1_565 ?
Cs3 Cl8 Cs4 161.119(15) . 7_465 ?
Cs2 Cl6 Cs5 167.730(16) . 7_455 ?
Cs2 Cl3 Cs1 162.351(18) . . ?
Cs4 Cl10 Cs3 157.745(18) 1_565 . ?
C15 N8 C16 109.49(14) . . ?
C15 N8 C14 110.13(14) . . ?
C16 N8 C14 110.11(15) . . ?
C15 N8 H8 109.0 . . ?
C16 N8 H8 109.0 . . ?
C14 N8 H8 109.0 . . ?
C7 N4 C11 109.78(14) . . ?
C7 N4 C10 109.73(15) . . ?
C11 N4 C10 109.29(15) . . ?
C7 N4 H4 109.3 . . ?
C11 N4 H4 109.3 . . ?
C10 N4 H4 109.3 . . ?
C9 N3 C8 109.88(15) . . ?
C9 N3 C12 110.11(14) . . ?
C8 N3 C12 109.79(15) . . ?
C9 N3 H3 109.0 . . ?
C8 N3 H3 109.0 . . ?
C12 N3 H3 109.0 . . ?
C3 N1 C5 110.54(16) . . ?
C3 N1 C1 109.49(17) . . ?
C5 N1 C1 109.98(17) . . ?
C3 N1 H1 108.9 . . ?
C5 N1 H1 108.9 . . ?
C1 N1 H1 108.9 . . ?
C2 N2 C4 111.25(16) . . ?
C2 N2 C6 109.92(16) . . ?
C4 N2 C6 109.16(17) . . ?
C2 N2 H2 108.8 . . ?
C4 N2 H2 108.8 . . ?
C6 N2 H2 108.8 . . ?
C24 N5 C22 110.44(16) . . ?
C24 N5 C23 109.74(16) . . ?
C22 N5 C23 110.06(15) . . ?
C24 N5 H5 108.9 . . ?
C22 N5 H5 108.9 . . ?
C23 N5 H5 108.9 . . ?
C21 N6 C20 110.36(17) . . ?
C21 N6 C19 110.60(15) . . ?
C20 N6 C19 109.50(16) . . ?
C21 N6 H6 108.8 . . ?
C20 N6 H6 108.8 . . ?
C19 N6 H6 108.8 . . ?
C18 N7 C13 110.7(2) . . ?
C18 N7 C17 110.3(2) . . ?
C13 N7 C17 108.27(19) . . ?
C18 N7 H7 109.2 . . ?
C13 N7 H7 109.2 . . ?
C17 N7 H7 109.2 . . ?
N5 C23 C19 108.15(15) . . ?
N5 C23 H23A 110.1 . . ?
C19 C23 H23A 110.1 . . ?
N5 C23 H23B 110.1 . . ?
C19 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
N4 C10 C9 107.95(14) . . ?
N4 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
N4 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N4 C11 C12 108.10(14) . . ?
N4 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
N4 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N3 C12 C11 107.45(14) . . ?
N3 C12 H12A 110.2 . . ?
C11 C12 H12A 110.2 . . ?
N3 C12 H12B 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
N8 C14 C13 108.43(14) . . ?
N8 C14 H14A 110.0 . . ?
C13 C14 H14A 110.0 . . ?
N8 C14 H14B 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
N2 C4 C3 107.89(14) . . ?
N2 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
N2 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N4 C7 C8 107.86(15) . . ?
N4 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N4 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N3 C8 C7 107.70(15) . . ?
N3 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
N3 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N3 C9 C10 107.56(15) . . ?
N3 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
N3 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N8 C15 C18 107.71(16) . . ?
N8 C15 H15A 110.2 . . ?
C18 C15 H15A 110.2 . . ?
N8 C15 H15B 110.2 . . ?
C18 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
N1 C3 C4 108.53(15) . . ?
N1 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
N1 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N6 C19 C23 107.88(15) . . ?
N6 C19 H19A 110.1 . . ?
C23 C19 H19A 110.1 . . ?
N6 C19 H19B 110.1 . . ?
C23 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
N5 C24 C20 108.44(15) . . ?
N5 C24 H24A 110.0 . . ?
C20 C24 H24A 110.0 . . ?
N5 C24 H24B 110.0 . . ?
C20 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
N6 C21 C22 108.13(16) . . ?
N6 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
N6 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
N5 C22 C21 108.23(16) . . ?
N5 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
N5 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
N2 C2 C1 108.92(17) . . ?
N2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
N2 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C17 C16 N8 108.01(16) . . ?
C17 C16 H16A 110.1 . . ?
N8 C16 H16A 110.1 . . ?
C17 C16 H16B 110.1 . . ?
N8 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
N7 C13 C14 108.67(15) . . ?
N7 C13 H13A 110.0 . . ?
C14 C13 H13A 110.0 . . ?
N7 C13 H13B 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.3 . . ?
N6 C20 C24 108.12(16) . . ?
N6 C20 H20A 110.1 . . ?
C24 C20 H20A 110.1 . . ?
N6 C20 H20B 110.1 . . ?
C24 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
N1 C5 C6 108.95(16) . . ?
N1 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1 C2 108.93(18) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C6 C5 108.41(16) . . ?
N2 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N2 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N7 C17 C16 109.76(19) . . ?
N7 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
N7 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N7 C18 C15 110.12(18) . . ?
N7 C18 H18A 109.6 . . ?
C15 C18 H18A 109.6 . . ?
N7 C18 H18B 109.6 . . ?
C15 C18 H18B 109.6 . . ?
H18A C18 H18B 108.2 . . ?

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
C24 N5 C23 C19 -68.35(19) . . . . ?
C22 N5 C23 C19 53.39(19) . . . . ?
C7 N4 C10 C9 -48.7(2) . . . . ?
C11 N4 C10 C9 71.70(18) . . . . ?
C7 N4 C11 C12 71.15(18) . . . . ?
C10 N4 C11 C12 -49.24(18) . . . . ?
C9 N3 C12 C11 71.48(18) . . . . ?
C8 N3 C12 C11 -49.63(18) . . . . ?
N4 C11 C12 N3 -18.20(19) . . . . ?
C15 N8 C14 C13 56.3(2) . . . . ?
C16 N8 C14 C13 -64.6(2) . . . . ?
C2 N2 C4 C3 63.70(19) . . . . ?
C6 N2 C4 C3 -57.78(19) . . . . ?
C11 N4 C7 C8 -48.9(2) . . . . ?
C10 N4 C7 C8 71.23(19) . . . . ?
C9 N3 C8 C7 -49.3(2) . . . . ?
C12 N3 C8 C7 71.90(19) . . . . ?
N4 C7 C8 N3 -18.7(2) . . . . ?
C8 N3 C9 C10 71.83(19) . . . . ?
C12 N3 C9 C10 -49.2(2) . . . . ?
N4 C10 C9 N3 -19.0(2) . . . . ?
C16 N8 C15 C18 56.1(2) . . . . ?
C14 N8 C15 C18 -65.2(2) . . . . ?
C5 N1 C3 C4 64.29(19) . . . . ?
C1 N1 C3 C4 -57.0(2) . . . . ?
N2 C4 C3 N1 -6.0(2) . . . . ?
C21 N6 C19 C23 -68.06(19) . . . . ?
C20 N6 C19 C23 53.8(2) . . . . ?
N5 C23 C19 N6 12.2(2) . . . . ?
C22 N5 C24 C20 -68.2(2) . . . . ?
C23 N5 C24 C20 53.3(2) . . . . ?
C20 N6 C21 C22 -68.3(2) . . . . ?
C19 N6 C21 C22 53.0(2) . . . . ?
C24 N5 C22 C21 52.6(2) . . . . ?
C23 N5 C22 C21 -68.7(2) . . . . ?
N6 C21 C22 N5 13.1(2) . . . . ?
C4 N2 C2 C1 -54.9(2) . . . . ?
C6 N2 C2 C1 66.1(2) . . . . ?
C15 N8 C16 C17 -67.6(2) . . . . ?
C14 N8 C16 C17 53.7(2) . . . . ?
C18 N7 C13 C14 -64.2(2) . . . . ?
C17 N7 C13 C14 56.8(2) . . . . ?
N8 C14 C13 N7 7.1(2) . . . . ?
C21 N6 C20 C24 52.8(2) . . . . ?
C19 N6 C20 C24 -69.2(2) . . . . ?
N5 C24 C20 N6 12.9(3) . . . . ?
C3 N1 C5 C6 -55.6(2) . . . . ?
C1 N1 C5 C6 65.4(2) . . . . ?
C3 N1 C1 C2 66.9(2) . . . . ?
C5 N1 C1 C2 -54.7(3) . . . . ?
N2 C2 C1 N1 -9.3(3) . . . . ?
C2 N2 C6 C5 -55.1(2) . . . . ?
C4 N2 C6 C5 67.2(2) . . . . ?
N1 C5 C6 N2 -8.9(3) . . . . ?
C18 N7 C17 C16 52.6(3) . . . . ?
C13 N7 C17 C16 -68.7(3) . . . . ?
N8 C16 C17 N7 11.1(3) . . . . ?
C13 N7 C18 C15 55.6(3) . . . . ?
C17 N7 C18 C15 -64.2(3) . . . . ?
N8 C15 C18 N7 8.2(3) . . . . ?

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
N8 H8 Cl4 0.98 2.05 3.0171(17) 167.8 5_465 yes
N4 H4 Cl12 0.98 2.07 3.0374(16) 170.4 5_465 yes
N3 H3 Cl7 0.98 2.05 3.0248(16) 171.9 4_445 yes
N1 H1 Cl1 0.98 2.04 3.0227(16) 177.4 4_465 yes
N2 H2 Cl11 0.98 2.08 3.0523(16) 172.3 . yes
N5 H5 Cl5 0.98 2.06 3.0242(16) 168.8 3_445 yes
N6 H6 Cl9 0.98 2.11 3.0453(16) 158.1 5_465 yes
N7 H7 Cl2 0.98 2.04 3.0038(17) 167.3 4_455 yes
C23 H23A Cl8 0.97 2.66 3.5243(19) 147.9 3_435 yes
C23 H23B Cl6 0.97 2.82 3.7738(19) 167.7 3_445 yes
C10 H10A Cl12 0.97 2.89 3.677(2) 138.9 6_566 yes
C10 H10B Cl6 0.97 2.74 3.5999(19) 147.4 4_455 yes
C11 H11A Cl11 0.97 2.86 3.787(2) 160.5 5_465 yes
C11 H11B Cl12 0.97 2.79 3.6292(19) 145.3 6_566 yes
C12 H12A Cl8 0.97 2.64 3.5843(19) 164.7 4_445 yes
C12 H12B Cl6 0.97 2.64 3.5163(18) 150.5 4_445 yes
C14 H14A Cl5 0.97 2.78 3.6396(19) 148.4 5_465 yes
C14 H14B Cl7 0.97 2.80 3.6891(19) 152.5 8_465 yes
C4 H4A Cl2 0.97 2.72 3.6197(19) 153.9 8_455 yes
C4 H4B Cl6 0.97 2.86 3.7510(19) 153.3 8_465 yes
C7 H7A Cl3 0.97 2.90 3.762(2) 148.0 4_455 yes
C8 H8A Cl6 0.97 2.85 3.699(2) 146.7 4_445 yes
C8 H8B Cl1 0.97 2.98 3.7490(19) 136.6 4_455 yes
C9 H9A Cl3 0.97 2.91 3.790(2) 151.0 4_455 yes
C9 H9B Cl5 0.97 2.90 3.5978(19) 129.9 4_455 yes
C15 H15B Cl5 0.97 2.69 3.602(2) 155.9 5_465 yes
C3 H3A Cl3 0.97 2.80 3.697(2) 154.9 8_465 yes
C19 H19A Cl11 0.97 2.75 3.674(2) 158.7 5_465 yes
C19 H19B Cl10 0.97 2.72 3.626(2) 156.6 5_465 yes
C24 H24A Cl7 0.97 2.94 3.627(2) 128.9 3_445 yes
C24 H24B Cl9 0.97 2.93 3.740(2) 141.6 3_445 yes
C21 H21B Cl9 0.97 2.98 3.820(2) 145.2 3_445 yes
C22 H22B Cl8 0.97 2.74 3.582(2) 145.3 3_435 yes
C2 H2A Cl10 0.97 2.94 3.724(2) 138.3 . yes
C2 H2B Cl2 0.97 2.78 3.642(2) 148.0 8_455 yes
C16 H16B Cl7 0.97 2.73 3.595(2) 148.9 8_465 yes
C13 H13A Cl1 0.97 2.76 3.666(2) 156.1 8_455 yes
C13 H13B Cl10 0.97 2.74 3.669(2) 160.5 5_475 yes
C20 H20A Cl8 0.97 2.95 3.581(2) 123.7 3_445 yes
C5 H5A Cl10 0.97 2.96 3.767(2) 141.6 . yes
C5 H5B Cl3 0.97 2.81 3.682(2) 149.9 8_465 yes
C6 H6A Cl6 0.97 2.99 3.848(3) 148.3 8_465 yes
C6 H6B Cl12 0.97 2.79 3.458(2) 126.5 1_565 yes
C17 H17A Cl3 0.97 2.85 3.557(2) 130.2 8_455 yes

_refine_diff_density_max         1.256
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.143

