# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_TrisSbClGreen_100
_database_code_depnum_ccdc_archive 'CCDC 2017736'
loop_
_audit_author_name
_audit_author_address
'Rajesh G Gonnade'
;National Chemical Laboratory Pune 
India
;
_audit_update_record             
;
2020-09-03 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_TrisSbClGreen_100   
;
PROBLEM: Short Inter D-H..H-D H1OA ..H2OB . 2.09 Ang.
RESPONSE: The short contact between the H-atoms is due to the strong 
H-bonding between the water molecules which are loacated in the 
channel across the inversion center.
;
# 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         
'C6 H22 N4, SbCl5, 0.5(SbCl3), Cl, (H2O)(H2.5O)'
_chemical_formula_sum            'C6 H26.50 Cl9 N4 O2 Sb1.50'
_chemical_formula_weight         688.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.116(4)
_cell_length_b                   10.249(6)
_cell_length_c                   13.343(5)
_cell_angle_alpha                97.69(2)
_cell_angle_beta                 101.372(16)
_cell_angle_gamma                119.379(13)
_cell_volume                     1138.0(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5197
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      33.80

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    2.858
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            24249
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.426
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5453
_reflns_number_gt                5172
_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0231P)²+5.4717P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5453
_refine_ls_number_parameters     220
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0916
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Sb1 Sb 0.500000 1.000000 1.000000 0.00770(8) Uani 1 2 d S . P . .
Sb2 Sb 0.90868(3) 0.14286(3) 0.50581(2) 0.00939(8) Uani 1 1 d . . . . .
Cl1 Cl 0.66139(12) 1.20385(12) 0.90262(9) 0.0233(2) Uani 1 1 d . . . . .
Cl2 Cl 0.22897(11) 0.96622(11) 0.90194(8) 0.01907(19) Uani 1 1 d . . . . .
Cl3 Cl 0.44705(12) 0.77371(12) 0.84703(10) 0.0288(3) Uani 1 1 d . . . . .
Cl4 Cl 1.02795(13) 0.04229(12) 0.35503(8) 0.0207(2) Uani 1 1 d . . . . .
Cl5 Cl 0.62868(11) -0.07668(11) 0.40446(8) 0.0218(2) Uani 1 1 d . . . . .
Cl6 Cl 0.79489(10) 0.21475(10) 0.63759(7) 0.01399(17) Uani 1 1 d . . . . .
Cl7 Cl 1.20994(10) 0.39102(10) 0.63800(7) 0.01461(17) Uani 1 1 d . . . . .
Cl8 Cl 0.87881(12) 0.30921(11) 0.40293(8) 0.0203(2) Uani 1 1 d . . . . .
Cl9 Cl 0.86001(10) 0.68686(9) 0.05948(6) 0.01071(16) Uani 1 1 d . . . . .
N1 N 0.7485(3) 0.6000(3) 0.8099(2) 0.0075(5) Uani 1 1 d . . . . .
H1 H 0.783636 0.630788 0.889291 0.009 Uiso 1 1 calc R U . . .
N2 N 0.3490(4) 0.2613(3) 0.8050(3) 0.0118(6) Uani 1 1 d . . . . .
H2NA H 0.295757 0.248180 0.737277 0.018 Uiso 1 1 calc R U . . .
H2NB H 0.285770 0.251100 0.847105 0.018 Uiso 1 1 calc R U . . .
H2NC H 0.375096 0.188116 0.805934 0.018 Uiso 1 1 calc R U . . .
N3 N 0.7975(4) 0.9902(3) 0.8112(3) 0.0133(6) Uani 1 1 d . . . . .
H3NA H 0.816757 0.993370 0.747482 0.020 Uiso 1 1 calc R U . . .
H3NB H 0.863769 1.085998 0.858017 0.020 Uiso 1 1 calc R U . . .
H3NC H 0.694600 0.961448 0.802857 0.020 Uiso 1 1 calc R U . . .
N4 N 1.0853(4) 0.5339(4) 0.8089(3) 0.0119(6) Uani 1 1 d . . . . .
H4NA H 1.038331 0.472953 0.740805 0.018 Uiso 1 1 calc R U . . .
H4NB H 1.125879 0.490183 0.850031 0.018 Uiso 1 1 calc R U . . .
H4NC H 1.165213 0.629978 0.810829 0.018 Uiso 1 1 calc R U . . .
C1 C 0.5992(4) 0.4390(4) 0.7718(3) 0.0093(6) Uani 1 1 d . . . . .
H1A H 0.628817 0.360041 0.770232 0.011 Uiso 1 1 calc R U . . .
H1B H 0.537820 0.422831 0.698814 0.011 Uiso 1 1 calc R U . . .
C2 C 0.4965(4) 0.4189(4) 0.8450(3) 0.0105(6) Uani 1 1 d . . . . .
H2A H 0.556673 0.432357 0.917783 0.013 Uiso 1 1 calc R U . . .
H2B H 0.468398 0.498932 0.847879 0.013 Uiso 1 1 calc R U . . .
C3 C 0.7148(4) 0.7167(4) 0.7728(3) 0.0094(6) Uani 1 1 d . . . . .
H3A H 0.602752 0.683295 0.765999 0.011 Uiso 1 1 calc R U . . .
H3B H 0.730634 0.722506 0.702308 0.011 Uiso 1 1 calc R U . . .
C4 C 0.8260(4) 0.8761(4) 0.8523(3) 0.0116(6) Uani 1 1 d . . . . .
H4A H 0.805742 0.872358 0.921766 0.014 Uiso 1 1 calc R U . . .
H4B H 0.938203 0.907354 0.862345 0.014 Uiso 1 1 calc R U . . .
C5 C 0.8821(4) 0.6020(4) 0.7737(3) 0.0096(6) Uani 1 1 d . . . . .
H5A H 0.959417 0.708595 0.772130 0.012 Uiso 1 1 calc R U . . .
H5B H 0.838497 0.532412 0.701045 0.012 Uiso 1 1 calc R U . . .
C6 C 0.9656(4) 0.5478(4) 0.8496(3) 0.0105(6) Uani 1 1 d . . . . .
H6A H 1.018498 0.623361 0.920615 0.013 Uiso 1 1 calc R U . . .
H6B H 0.886246 0.445865 0.856868 0.013 Uiso 1 1 calc R U . . .
O1 O 0.5077(4) 0.8180(5) 0.6067(3) 0.0345(8) Uani 1 1 d D . . . .
H1OA H 0.532788 0.869168 0.563316 0.052 Uiso 1 1 d DG U . . .
H1OB H 0.441651 0.819246 0.634257 0.052 Uiso 1 1 d DG U . . .
O2 O 0.4001(5) 0.5355(5) 0.4931(3) 0.0455(11) Uani 1 1 d D . . . .
H2OA H 0.337469 0.478421 0.522494 0.068 Uiso 1 1 d DG U . . .
H2OB H 0.435418 0.630324 0.512445 0.068 Uiso 1 1 d DG U . . .
H20C H 0.500000 0.500000 0.500000 0.068 Uiso 1 2 d S 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
Sb1 Cl2 2.6233(14) 2_677 ?
Sb1 Cl2 2.6233(14) . ?
Sb1 Cl3 2.6295(16) 2_677 ?
Sb1 Cl3 2.6295(16) . ?
Sb1 Cl1 2.6336(13) 2_677 ?
Sb1 Cl1 2.6336(13) . ?
Sb2 Cl8 2.4189(14) . ?
Sb2 Cl6 2.4986(11) . ?
Sb2 Cl5 2.5172(15) . ?
Sb2 Cl7 2.8181(16) . ?
Sb2 Cl4 2.8616(13) . ?
N1 C3 1.511(4) . ?
N1 C1 1.513(4) . ?
N1 C5 1.515(4) . ?
N1 H1 1.0000 . ?
N2 C2 1.487(4) . ?
N2 H2NA 0.9100 . ?
N2 H2NB 0.9100 . ?
N2 H2NC 0.9100 . ?
N3 C4 1.480(4) . ?
N3 H3NA 0.9100 . ?
N3 H3NB 0.9100 . ?
N3 H3NC 0.9100 . ?
N4 C6 1.480(4) . ?
N4 H4NA 0.9100 . ?
N4 H4NB 0.9100 . ?
N4 H4NC 0.9100 . ?
C1 C2 1.523(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.524(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.523(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O1 H1OA 0.827(19) . ?
O1 H1OB 0.8285 . ?
O2 H2OA 0.833(19) . ?
O2 H2OB 0.8335 . ?
O2 H20C 1.223(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Sb1 Cl2 180.0 2_677 . ?
Cl2 Sb1 Cl3 90.09(4) 2_677 2_677 ?
Cl2 Sb1 Cl3 89.91(4) . 2_677 ?
Cl2 Sb1 Cl3 89.91(4) 2_677 . ?
Cl2 Sb1 Cl3 90.09(4) . . ?
Cl3 Sb1 Cl3 180.0 2_677 . ?
Cl2 Sb1 Cl1 93.22(4) 2_677 2_677 ?
Cl2 Sb1 Cl1 86.78(4) . 2_677 ?
Cl3 Sb1 Cl1 89.79(6) 2_677 2_677 ?
Cl3 Sb1 Cl1 90.21(6) . 2_677 ?
Cl2 Sb1 Cl1 86.78(4) 2_677 . ?
Cl2 Sb1 Cl1 93.22(4) . . ?
Cl3 Sb1 Cl1 90.21(6) 2_677 . ?
Cl3 Sb1 Cl1 89.79(6) . . ?
Cl1 Sb1 Cl1 180.0 2_677 . ?
Cl8 Sb2 Cl6 92.00(4) . . ?
Cl8 Sb2 Cl5 90.38(5) . . ?
Cl6 Sb2 Cl5 87.12(5) . . ?
Cl8 Sb2 Cl7 91.54(5) . . ?
Cl6 Sb2 Cl7 86.96(5) . . ?
Cl5 Sb2 Cl7 173.84(3) . . ?
Cl8 Sb2 Cl4 90.38(4) . . ?
Cl6 Sb2 Cl4 176.70(3) . . ?
Cl5 Sb2 Cl4 90.58(5) . . ?
Cl7 Sb2 Cl4 95.26(5) . . ?
Sb2 Cl4 Sb2 89.99(4) . 2_756 ?
C3 N1 C1 110.7(3) . . ?
C3 N1 C5 110.7(3) . . ?
C1 N1 C5 111.3(3) . . ?
C3 N1 H1 108.0 . . ?
C1 N1 H1 108.0 . . ?
C5 N1 H1 108.0 . . ?
C2 N2 H2NA 109.5 . . ?
C2 N2 H2NB 109.5 . . ?
H2NA N2 H2NB 109.5 . . ?
C2 N2 H2NC 109.5 . . ?
H2NA N2 H2NC 109.5 . . ?
H2NB N2 H2NC 109.5 . . ?
C4 N3 H3NA 109.5 . . ?
C4 N3 H3NB 109.5 . . ?
H3NA N3 H3NB 109.5 . . ?
C4 N3 H3NC 109.5 . . ?
H3NA N3 H3NC 109.5 . . ?
H3NB N3 H3NC 109.5 . . ?
C6 N4 H4NA 109.5 . . ?
C6 N4 H4NB 109.5 . . ?
H4NA N4 H4NB 109.5 . . ?
C6 N4 H4NC 109.5 . . ?
H4NA N4 H4NC 109.5 . . ?
H4NB N4 H4NC 109.5 . . ?
N1 C1 C2 110.5(3) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 109.6(3) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 109.8(3) . . ?
N1 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 108.8(3) . . ?
N3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
N3 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C6 109.5(3) . . ?
N1 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N4 C6 C5 109.9(3) . . ?
N4 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N4 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
H1OA O1 H1OB 118.3 . . ?
H2OA O2 H2OB 117.0 . . ?
H2OA O2 H20C 104(5) . . ?
H2OB O2 H20C 115.8 . . ?

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 -82.0(3) . . . . ?
C5 N1 C1 C2 154.4(3) . . . . ?
N1 C1 C2 N2 178.8(3) . . . . ?
C1 N1 C3 C4 150.3(3) . . . . ?
C5 N1 C3 C4 -85.7(3) . . . . ?
N1 C3 C4 N3 176.6(3) . . . . ?
C3 N1 C5 C6 153.6(3) . . . . ?
C1 N1 C5 C6 -82.8(3) . . . . ?
N1 C5 C6 N4 174.2(3) . . . . ?

_refine_diff_density_max         1.686
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.170

####################################################################### 
# 
# 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_TrisSbClRed_0m
_database_code_depnum_ccdc_archive 'CCDC 2017737'
loop_
_audit_author_name
_audit_author_address
'Rajesh G Gonnade'
;National Chemical Laboratory Pune 
India
;
_audit_update_record             
;
2020-09-03 deposited with the CCDC.	2020-11-16 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         'C6 H22 N4, SbCl6, Cl, 1.5(H2 O)'
_chemical_formula_sum            'C6 H25 Cl7 N4 O1.50 Sb'
_chemical_formula_weight         547.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   10.3972(5)
_cell_length_b                   15.6011(8)
_cell_length_c                   12.0441(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.622(2)
_cell_angle_gamma                90
_cell_volume                     1944.25(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      33.22

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.382
_shelx_estimated_absorpt_T_min   0.449
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            39790
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.362
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             11149
_reflns_number_gt                10777
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.991

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-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)+(0.0364P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11149
_refine_ls_number_parameters     377
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Sb2 Sb 0.46448(2) 0.79241(2) 0.00669(2) 0.00756(7) Uani 1 1 d . . . . .
Cl12 Cl 0.66490(9) 0.66884(7) -0.04805(9) 0.01372(19) Uani 1 1 d . . . . .
Cl10 Cl 0.42255(9) 0.79376(7) 0.25310(8) 0.01215(18) Uani 1 1 d . . . . .
Sb1 Sb 0.96073(2) 0.22105(2) 0.50515(2) 0.00763(7) Uani 1 1 d . . . . .
Cl1 Cl 0.78791(9) 0.11532(7) 0.51694(9) 0.01299(19) Uani 1 1 d . . . . .
Cl2 Cl 1.17129(9) 0.32934(7) 0.45160(9) 0.01213(19) Uani 1 1 d . . . . .
Cl3 Cl 1.12810(9) 0.08930(7) 0.53889(9) 0.01325(19) Uani 1 1 d . . . . .
Cl4 Cl 0.96174(10) 0.18662(7) 0.30693(9) 0.0150(2) Uani 1 1 d . . . . .
Cl5 Cl 0.78753(10) 0.33233(7) 0.45504(10) 0.0166(2) Uani 1 1 d . . . . .
Cl6 Cl 0.95198(9) 0.21630(7) 0.76628(9) 0.01302(18) Uani 1 1 d . . . . .
N1 N 0.5586(3) 0.5786(2) 0.6687(3) 0.0085(6) Uani 1 1 d . . . . .
H1 H 0.536753 0.552479 0.593362 0.010 Uiso 1 1 calc R U . . .
N2 N 0.2261(3) 0.5254(2) 0.7534(3) 0.0116(7) Uani 1 1 d . . . . .
H2NA H 0.234806 0.506822 0.825367 0.017 Uiso 1 1 calc R U . . .
H2NB H 0.160811 0.496158 0.714270 0.017 Uiso 1 1 calc R U . . .
H2NC H 0.207603 0.582417 0.751732 0.017 Uiso 1 1 calc R U . . .
N3 N 0.5937(3) 0.7076(2) 0.4537(3) 0.0128(7) Uani 1 1 d . . . . .
H3NA H 0.675696 0.727900 0.453451 0.019 Uiso 1 1 calc R U . . .
H3NB H 0.540599 0.736038 0.401513 0.019 Uiso 1 1 calc R U . . .
H3NC H 0.592376 0.650620 0.437545 0.019 Uiso 1 1 calc R U . . .
N4 N 0.8238(3) 0.4154(2) 0.7401(3) 0.0097(7) Uani 1 1 d . . . . .
H4NA H 0.854289 0.434814 0.808870 0.015 Uiso 1 1 calc R U . . .
H4NB H 0.890982 0.396798 0.703325 0.015 Uiso 1 1 calc R U . . .
H4NC H 0.767970 0.371244 0.747319 0.015 Uiso 1 1 calc R U . . .
C1 C 0.4361(4) 0.5891(3) 0.7241(4) 0.0107(8) Uani 1 1 d . . . . .
H1A H 0.389526 0.640957 0.694809 0.013 Uiso 1 1 calc R U . . .
H1B H 0.457341 0.596553 0.805502 0.013 Uiso 1 1 calc R U . . .
C2 C 0.3493(4) 0.5103(3) 0.7022(4) 0.0107(8) Uani 1 1 d . . . . .
H2A H 0.330989 0.500842 0.620924 0.013 Uiso 1 1 calc R U . . .
H2B H 0.393205 0.458677 0.735421 0.013 Uiso 1 1 calc R U . . .
C3 C 0.6209(4) 0.6647(3) 0.6542(3) 0.0087(7) Uani 1 1 d . . . . .
H3A H 0.709790 0.655469 0.633840 0.010 Uiso 1 1 calc R U . . .
H3B H 0.627386 0.695315 0.726539 0.010 Uiso 1 1 calc R U . . .
C4 C 0.5484(4) 0.7212(3) 0.5659(4) 0.0130(8) Uani 1 1 d . . . . .
H4A H 0.454804 0.708313 0.562465 0.016 Uiso 1 1 calc R U . . .
H4B H 0.560755 0.782069 0.587495 0.016 Uiso 1 1 calc R U . . .
C5 C 0.6467(4) 0.5179(3) 0.7386(3) 0.0096(7) Uani 1 1 d . . . . .
H5A H 0.683222 0.547821 0.807085 0.011 Uiso 1 1 calc R U . . .
H5B H 0.595804 0.468449 0.761379 0.011 Uiso 1 1 calc R U . . .
C6 C 0.7552(4) 0.4861(3) 0.6756(4) 0.0134(8) Uani 1 1 d . . . . .
H6A H 0.720342 0.465081 0.601151 0.016 Uiso 1 1 calc R U . . .
H6B H 0.816231 0.533498 0.665071 0.016 Uiso 1 1 calc R U . . .
Cl7 Cl 0.66416(10) 0.89697(7) 0.05928(9) 0.0175(2) Uani 1 1 d . . . . .
Cl8 Cl 0.47934(10) 0.82892(7) -0.18944(9) 0.0153(2) Uani 1 1 d . . . . .
Cl9 Cl 0.27474(9) 0.68880(7) -0.04966(10) 0.0176(2) Uani 1 1 d . . . . .
Cl11 Cl 0.31306(10) 0.91099(7) 0.01177(9) 0.0148(2) Uani 1 1 d . . . . .
N5 N 0.0577(3) 0.4326(2) 0.1625(3) 0.0080(6) Uani 1 1 d . . . . .
H5 H 0.033753 0.463638 0.090837 0.010 Uiso 1 1 calc R U . . .
N6 N -0.2702(3) 0.4814(2) 0.2575(3) 0.0121(7) Uani 1 1 d . . . . .
H6NA H -0.305610 0.431973 0.228214 0.018 Uiso 1 1 calc R U . . .
H6NB H -0.326843 0.525328 0.242762 0.018 Uiso 1 1 calc R U . . .
H6NC H -0.252623 0.475443 0.332596 0.018 Uiso 1 1 calc R U . . .
N7 N 0.3193(3) 0.5967(2) 0.2321(3) 0.0121(7) Uani 1 1 d . . . . .
H7NA H 0.260873 0.639709 0.236340 0.018 Uiso 1 1 calc R U . . .
H7NB H 0.387405 0.616197 0.197254 0.018 Uiso 1 1 calc R U . . .
H7NC H 0.347782 0.578757 0.302126 0.018 Uiso 1 1 calc R U . . .
N8 N 0.0440(3) 0.2165(2) 0.0238(3) 0.0131(7) Uani 1 1 d . . . . .
H8NA H 0.128259 0.200187 0.035258 0.020 Uiso 1 1 calc R U . . .
H8NB H 0.010085 0.198546 -0.044818 0.020 Uiso 1 1 calc R U . . .
H8NC H -0.001104 0.192631 0.077004 0.020 Uiso 1 1 calc R U . . .
C7 C -0.0637(3) 0.4204(3) 0.2204(4) 0.0096(7) Uani 1 1 d . . . . .
H7A H -0.040122 0.409290 0.300697 0.012 Uiso 1 1 calc R U . . .
H7B H -0.112156 0.370193 0.188224 0.012 Uiso 1 1 calc R U . . .
C8 C -0.1487(4) 0.4999(3) 0.2067(4) 0.0097(8) Uani 1 1 d . . . . .
H8A H -0.103862 0.549491 0.244312 0.012 Uiso 1 1 calc R U . . .
H8B H -0.168017 0.513810 0.126556 0.012 Uiso 1 1 calc R U . . .
C9 C 0.1523(4) 0.4876(3) 0.2342(3) 0.0096(7) Uani 1 1 d . . . . .
H9A H 0.193057 0.452808 0.296820 0.012 Uiso 1 1 calc R U . . .
H9B H 0.105221 0.535363 0.266080 0.012 Uiso 1 1 calc R U . . .
C10 C 0.2571(4) 0.5240(3) 0.1678(4) 0.0127(8) Uani 1 1 d . . . . .
H10A H 0.322030 0.479242 0.156250 0.015 Uiso 1 1 calc R U . . .
H10B H 0.218755 0.544017 0.093904 0.015 Uiso 1 1 calc R U . . .
C11 C 0.1117(4) 0.3462(3) 0.1351(4) 0.0102(7) Uani 1 1 d . . . . .
H11A H 0.105061 0.306157 0.198030 0.012 Uiso 1 1 calc R U . . .
H11B H 0.204024 0.351901 0.122621 0.012 Uiso 1 1 calc R U . . .
C12 C 0.0353(4) 0.3114(3) 0.0301(4) 0.0111(8) Uani 1 1 d . . . . .
H12A H -0.056475 0.328448 0.029885 0.013 Uiso 1 1 calc R U . . .
H12B H 0.069101 0.336931 -0.036438 0.013 Uiso 1 1 calc R U . . .
Cl13 Cl 0.99728(9) 0.51809(6) 0.93076(9) 0.01111(18) Uani 1 1 d . . . . .
Cl14 Cl 0.50829(9) 0.51143(7) 0.42835(9) 0.01255(19) Uani 1 1 d . . . . .
O1 O 0.0387(3) 0.4458(2) 0.6122(3) 0.0148(6) Uani 1 1 d D . . . .
H1OA H 0.001928 0.486293 0.578239 0.022 Uiso 1 1 d DG U . . .
H1OB H 0.078385 0.411049 0.574630 0.022 Uiso 1 1 d DG U . . .
O2 O 0.5789(3) 0.6162(2) 0.1763(3) 0.0176(6) Uani 1 1 d D . . . .
H2OA H 0.586154 0.617359 0.109194 0.026 Uiso 1 1 d DG U . . .
H2OB H 0.615619 0.655402 0.215824 0.026 Uiso 1 1 d DG U . . .
O3 O 0.7413(3) 0.7470(3) 0.2563(3) 0.0223(8) Uani 1 1 d D . . . .
H3OA H 0.818358 0.727300 0.265630 0.034 Uiso 1 1 d DG U . . .
H3OB H 0.731778 0.790080 0.216263 0.034 Uiso 1 1 d DG 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
Sb2 Cl11 2.4339(10) . ?
Sb2 Cl8 2.4495(11) . ?
Sb2 Cl9 2.5890(10) . ?
Sb2 Cl7 2.6674(10) . ?
Sb2 Cl12 2.9601(10) . ?
Sb2 Cl10 3.0417(10) . ?
Sb1 Cl4 2.4481(11) . ?
Sb1 Cl1 2.4535(10) . ?
Sb1 Cl5 2.5314(10) . ?
Sb1 Cl3 2.6982(10) . ?
Sb1 Cl2 2.8878(10) . ?
Sb1 Cl6 3.1562(11) . ?
N1 C1 1.504(5) . ?
N1 C3 1.508(5) . ?
N1 C5 1.515(5) . ?
N1 H1 1.0000 . ?
N2 C2 1.494(5) . ?
N2 H2NA 0.9100 . ?
N2 H2NB 0.9100 . ?
N2 H2NC 0.9100 . ?
N3 C4 1.490(5) . ?
N3 H3NA 0.9100 . ?
N3 H3NB 0.9100 . ?
N3 H3NC 0.9100 . ?
N4 C6 1.490(5) . ?
N4 H4NA 0.9100 . ?
N4 H4NB 0.9100 . ?
N4 H4NC 0.9100 . ?
C1 C2 1.533(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.504(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N5 C11 1.509(5) . ?
N5 C9 1.512(5) . ?
N5 C7 1.512(5) . ?
N5 H5 1.0000 . ?
N6 C8 1.485(5) . ?
N6 H6NA 0.9100 . ?
N6 H6NB 0.9100 . ?
N6 H6NC 0.9100 . ?
N7 C10 1.486(5) . ?
N7 H7NA 0.9100 . ?
N7 H7NB 0.9100 . ?
N7 H7NC 0.9100 . ?
N8 C12 1.486(5) . ?
N8 H8NA 0.9100 . ?
N8 H8NB 0.9100 . ?
N8 H8NC 0.9100 . ?
C7 C8 1.522(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.523(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.525(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O1 H1OA 0.83(2) . ?
O1 H1OB 0.8398 . ?
O2 H2OA 0.82(2) . ?
O2 H2OB 0.8433 . ?
O3 H3OA 0.86(2) . ?
O3 H3OB 0.8273 . ?

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
Cl11 Sb2 Cl8 87.11(4) . . ?
Cl11 Sb2 Cl9 90.17(4) . . ?
Cl8 Sb2 Cl9 90.62(4) . . ?
Cl11 Sb2 Cl7 91.11(4) . . ?
Cl8 Sb2 Cl7 88.03(4) . . ?
Cl9 Sb2 Cl7 178.09(3) . . ?
Cl11 Sb2 Cl12 166.37(4) . . ?
Cl8 Sb2 Cl12 79.89(3) . . ?
Cl9 Sb2 Cl12 94.01(3) . . ?
Cl7 Sb2 Cl12 84.42(3) . . ?
Cl11 Sb2 Cl10 79.36(3) . . ?
Cl8 Sb2 Cl10 165.45(3) . . ?
Cl9 Sb2 Cl10 94.69(3) . . ?
Cl7 Sb2 Cl10 86.94(3) . . ?
Cl12 Sb2 Cl10 113.15(3) . . ?
Cl4 Sb1 Cl1 88.97(4) . . ?
Cl4 Sb1 Cl5 89.37(4) . . ?
Cl1 Sb1 Cl5 88.11(4) . . ?
Cl4 Sb1 Cl3 85.14(3) . . ?
Cl1 Sb1 Cl3 86.81(3) . . ?
Cl5 Sb1 Cl3 172.58(4) . . ?
Cl4 Sb1 Cl2 80.49(3) . . ?
Cl1 Sb1 Cl2 169.04(3) . . ?
Cl5 Sb1 Cl2 94.74(3) . . ?
Cl3 Sb1 Cl2 89.28(3) . . ?
Cl4 Sb1 Cl6 165.91(3) . . ?
Cl1 Sb1 Cl6 80.43(3) . . ?
Cl5 Sb1 Cl6 99.46(3) . . ?
Cl3 Sb1 Cl6 85.02(3) . . ?
Cl2 Sb1 Cl6 109.44(3) . . ?
C1 N1 C3 110.3(3) . . ?
C1 N1 C5 108.3(3) . . ?
C3 N1 C5 112.2(3) . . ?
C1 N1 H1 108.7 . . ?
C3 N1 H1 108.7 . . ?
C5 N1 H1 108.7 . . ?
C2 N2 H2NA 109.5 . . ?
C2 N2 H2NB 109.5 . . ?
H2NA N2 H2NB 109.5 . . ?
C2 N2 H2NC 109.5 . . ?
H2NA N2 H2NC 109.5 . . ?
H2NB N2 H2NC 109.5 . . ?
C4 N3 H3NA 109.5 . . ?
C4 N3 H3NB 109.5 . . ?
H3NA N3 H3NB 109.5 . . ?
C4 N3 H3NC 109.5 . . ?
H3NA N3 H3NC 109.5 . . ?
H3NB N3 H3NC 109.5 . . ?
C6 N4 H4NA 109.5 . . ?
C6 N4 H4NB 109.5 . . ?
H4NA N4 H4NB 109.5 . . ?
C6 N4 H4NC 109.5 . . ?
H4NA N4 H4NC 109.5 . . ?
H4NB N4 H4NC 109.5 . . ?
N1 C1 C2 110.2(3) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 108.4(3) . . ?
N2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
N1 C3 C4 114.0(3) . . ?
N1 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.6 . . ?
N3 C4 C3 111.9(3) . . ?
N3 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 N1 111.6(3) . . ?
C6 C5 H5A 109.3 . . ?
N1 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
N1 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
N4 C6 C5 109.0(3) . . ?
N4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C11 N5 C9 113.4(3) . . ?
C11 N5 C7 109.6(3) . . ?
C9 N5 C7 109.5(3) . . ?
C11 N5 H5 108.1 . . ?
C9 N5 H5 108.1 . . ?
C7 N5 H5 108.1 . . ?
C8 N6 H6NA 109.5 . . ?
C8 N6 H6NB 109.5 . . ?
H6NA N6 H6NB 109.5 . . ?
C8 N6 H6NC 109.5 . . ?
H6NA N6 H6NC 109.5 . . ?
H6NB N6 H6NC 109.5 . . ?
C10 N7 H7NA 109.5 . . ?
C10 N7 H7NB 109.5 . . ?
H7NA N7 H7NB 109.5 . . ?
C10 N7 H7NC 109.5 . . ?
H7NA N7 H7NC 109.5 . . ?
H7NB N7 H7NC 109.5 . . ?
C12 N8 H8NA 109.5 . . ?
C12 N8 H8NB 109.5 . . ?
H8NA N8 H8NB 109.5 . . ?
C12 N8 H8NC 109.5 . . ?
H8NA N8 H8NC 109.5 . . ?
H8NB N8 H8NC 109.5 . . ?
N5 C7 C8 110.5(3) . . ?
N5 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
N5 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N6 C8 C7 107.8(3) . . ?
N6 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
N6 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N5 C9 C10 111.8(3) . . ?
N5 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N5 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
N7 C10 C9 108.0(3) . . ?
N7 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
N7 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N5 C11 C12 108.9(3) . . ?
N5 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
N5 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N8 C12 C11 111.6(3) . . ?
N8 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
N8 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
H1OA O1 H1OB 117.0 . . ?
H2OA O2 H2OB 117.4 . . ?
H3OA O3 H3OB 115.2 . . ?

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
C3 N1 C1 C2 159.9(3) . . . . ?
C5 N1 C1 C2 -77.0(4) . . . . ?
N1 C1 C2 N2 -177.0(3) . . . . ?
C1 N1 C3 C4 -71.2(4) . . . . ?
C5 N1 C3 C4 168.1(3) . . . . ?
N1 C3 C4 N3 -90.3(4) . . . . ?
C1 N1 C5 C6 165.4(4) . . . . ?
C3 N1 C5 C6 -72.7(4) . . . . ?
N1 C5 C6 N4 -169.8(3) . . . . ?
C11 N5 C7 C8 -156.8(3) . . . . ?
C9 N5 C7 C8 78.3(4) . . . . ?
N5 C7 C8 N6 175.7(3) . . . . ?
C11 N5 C9 C10 74.3(4) . . . . ?
C7 N5 C9 C10 -163.0(3) . . . . ?
N5 C9 C10 N7 162.6(3) . . . . ?
C9 N5 C11 C12 -157.8(3) . . . . ?
C7 N5 C11 C12 79.6(4) . . . . ?
N5 C11 C12 N8 -156.7(3) . . . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.142

####################################################################### 
# 
# 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_TRIS_YELLO_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2017738'
loop_
_audit_author_name
_audit_author_address
'Rajesh G Gonnade'
;National Chemical Laboratory Pune 
India
;
_audit_update_record             
;
2020-09-03 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_TRIS_YELLO_0m_a     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O2 Check
RESPONSE: The isolated O atoms are the oxygens of the water molecules.
The H-atoms bound to these O atoms could not be located in the difference
Fourier map and hence left them isolated. However, the H-atoms were incorporated
in the SFAC unit for correct molecular formula, molecular weight, crystal density
and F(000) calculations.
;
_vrf_PLAT911_TRIS_YELLO_0m_a     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 805 Report
RESPONSE: These reflections were probably affected by deviations
in their intensities values for symmetry equivalent measurements and 
hence omitted during data reduction.
;
_vrf_PLAT934_TRIS_YELLO_0m_a     
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 2 Check
RESPONSE: CheckCIF uses a different method of calculating these than does SHELXL.
The most disagreeable reflections from lst file does not indicate any such issue.

;
# 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         '4(C6 H22 N4), 3(SbCl6), Cl7, 4(H2O)'
_chemical_formula_sum            'C24 H96 Cl25 N16 O4 Sb3'
_chemical_formula_weight         1924.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.229(4)
_cell_length_b                   10.266(4)
_cell_length_c                   40.365(16)
_cell_angle_alpha                86.054(17)
_cell_angle_beta                 88.191(17)
_cell_angle_gamma                60.550(15)
_cell_volume                     3682(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    301(2)
_cell_measurement_reflns_used    9762
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      30.65

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.042
_shelx_estimated_absorpt_T_min   0.438
_shelx_estimated_absorpt_T_max   0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4297
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      301(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            68358
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.283
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.939
_reflns_number_total             13650
_reflns_number_gt                13263
_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+43.2975P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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       0.0093(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13650
_refine_ls_number_parameters     712
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.2026
_refine_ls_wR_factor_gt          0.2018
_refine_ls_goodness_of_fit_ref   1.364
_refine_ls_restrained_S_all      1.364
_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
N1 N 0.6649(7) 0.1381(8) 0.05758(18) 0.0215(14) Uani 1 1 d . . . . .
H1 H 0.667410 0.149962 0.033307 0.026 Uiso 1 1 calc R U . . .
N2 N 1.0651(8) 0.0575(10) 0.0697(2) 0.0321(17) Uani 1 1 d . . . . .
H2A H 1.042736 0.147311 0.076107 0.048 Uiso 1 1 calc R U . . .
H2B H 1.145447 0.023585 0.056571 0.048 Uiso 1 1 calc R U . . .
H2C H 1.084429 -0.005715 0.087396 0.048 Uiso 1 1 calc R U . . .
N3 N 0.6116(9) -0.2030(9) 0.0550(2) 0.0320(17) Uani 1 1 d . . . . .
H3A H 0.707795 -0.270615 0.052584 0.048 Uiso 1 1 calc R U . . .
H3B H 0.555278 -0.223116 0.042206 0.048 Uiso 1 1 calc R U . . .
H3C H 0.585115 -0.206172 0.076151 0.048 Uiso 1 1 calc R U . . .
N4 N 0.3436(9) 0.5351(9) 0.0641(2) 0.0327(18) Uani 1 1 d . . . . .
H4A H 0.267876 0.517702 0.068961 0.049 Uiso 1 1 calc R U . . .
H4B H 0.311379 0.616757 0.050402 0.049 Uiso 1 1 calc R U . . .
H4C H 0.378444 0.549134 0.082666 0.049 Uiso 1 1 calc R U . . .
C1 C 0.7946(9) 0.1476(10) 0.0715(2) 0.0254(17) Uani 1 1 d . . . . .
H1D H 0.814695 0.102635 0.093977 0.030 Uiso 1 1 calc R U . . .
H1E H 0.766953 0.252170 0.072436 0.030 Uiso 1 1 calc R U . . .
C2 C 0.9361(10) 0.0698(11) 0.0511(2) 0.0289(19) Uani 1 1 d . . . . .
H2D H 0.954597 -0.029437 0.046510 0.035 Uiso 1 1 calc R U . . .
H2E H 0.924049 0.126329 0.030079 0.035 Uiso 1 1 calc R U . . .
C3 C 0.6832(10) -0.0154(9) 0.0671(2) 0.0236(17) Uani 1 1 d . . . . .
H3D H 0.788051 -0.090628 0.065127 0.028 Uiso 1 1 calc R U . . .
H3E H 0.653828 -0.018907 0.090077 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5890(11) -0.0514(11) 0.0452(2) 0.0291(19) Uani 1 1 d . . . . .
H4D H 0.483817 0.022367 0.047404 0.035 Uiso 1 1 calc R U . . .
H4E H 0.617469 -0.047473 0.022175 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5164(9) 0.2628(9) 0.0696(2) 0.0213(16) Uani 1 1 d . . . . .
H5D H 0.440794 0.231793 0.069473 0.026 Uiso 1 1 calc R U . . .
H5E H 0.527557 0.281971 0.092269 0.026 Uiso 1 1 calc R U . . .
C6 C 0.4661(10) 0.4040(10) 0.0477(2) 0.0282(19) Uani 1 1 d . . . . .
H6D H 0.550438 0.420993 0.043279 0.034 Uiso 1 1 calc R U . . .
H6E H 0.430313 0.393002 0.026688 0.034 Uiso 1 1 calc R U . . .
N5 N 0.0212(8) 0.7172(8) 0.19410(18) 0.0240(15) Uani 1 1 d . . . . .
H5 H 0.022468 0.760752 0.171786 0.029 Uiso 1 1 calc R U . . .
N6 N 0.3362(11) 0.7035(12) 0.1675(2) 0.045(2) Uani 1 1 d . . . . .
H6A H 0.255191 0.764779 0.155339 0.068 Uiso 1 1 calc R U . . .
H6B H 0.413718 0.654360 0.154078 0.068 Uiso 1 1 calc R U . . .
H6C H 0.357063 0.756635 0.180718 0.068 Uiso 1 1 calc R U . . .
N7 N -0.1485(10) 0.4942(10) 0.1610(2) 0.0361(19) Uani 1 1 d . . . . .
H7A H -0.062676 0.409497 0.158632 0.054 Uiso 1 1 calc R U . . .
H7B H -0.208882 0.511105 0.143962 0.054 Uiso 1 1 calc R U . . .
H7C H -0.192683 0.486204 0.179836 0.054 Uiso 1 1 calc R U . . .
N8 N -0.2506(10) 1.1025(10) 0.2220(2) 0.0391(19) Uani 1 1 d . . . . .
H8A H -0.321779 1.119695 0.207443 0.059 Uiso 1 1 calc R U . . .
H8B H -0.245486 1.185859 0.223639 0.059 Uiso 1 1 calc R U . . .
H8C H -0.272500 1.074003 0.241735 0.059 Uiso 1 1 calc R U . . .
C7 C 0.1708(10) 0.6675(12) 0.2104(2) 0.031(2) Uani 1 1 d . . . . .
H7D H 0.183428 0.597172 0.228936 0.038 Uiso 1 1 calc R U . . .
H7E H 0.168328 0.754154 0.219235 0.038 Uiso 1 1 calc R U . . .
C8 C 0.3071(10) 0.5945(12) 0.1879(3) 0.034(2) Uani 1 1 d . . . . .
H8D H 0.394843 0.530190 0.201445 0.041 Uiso 1 1 calc R U . . .
H8E H 0.292571 0.531685 0.173181 0.041 Uiso 1 1 calc R U . . .
C9 C -0.0074(10) 0.5867(10) 0.1906(2) 0.0289(19) Uani 1 1 d . . . . .
H9D H -0.048062 0.567525 0.211243 0.035 Uiso 1 1 calc R U . . .
H9E H 0.086785 0.497351 0.186374 0.035 Uiso 1 1 calc R U . . .
C10 C -0.1174(11) 0.6204(11) 0.1622(2) 0.0306(19) Uani 1 1 d . . . . .
H10D H -0.210108 0.712425 0.165787 0.037 Uiso 1 1 calc R U . . .
H10E H -0.074594 0.633407 0.141330 0.037 Uiso 1 1 calc R U . . .
C11 C -0.1065(9) 0.8370(10) 0.2133(2) 0.0241(17) Uani 1 1 d . . . . .
H11D H -0.201455 0.853170 0.204924 0.029 Uiso 1 1 calc R U . . .
H11E H -0.098650 0.802308 0.236546 0.029 Uiso 1 1 calc R U . . .
C12 C -0.1043(11) 0.9825(11) 0.2106(3) 0.034(2) Uani 1 1 d . . . . .
H12D H -0.023944 0.974829 0.224146 0.041 Uiso 1 1 calc R U . . .
H12E H -0.086997 1.005664 0.187715 0.041 Uiso 1 1 calc R U . . .
N9 N 0.5787(8) 0.5308(9) 0.31830(19) 0.0282(16) Uani 1 1 d . . . . .
H9 H 0.573740 0.502391 0.341798 0.034 Uiso 1 1 calc R U . . .
N10 N 0.9830(9) 0.2234(11) 0.3188(3) 0.043(2) Uani 1 1 d . . . . .
H10A H 1.018337 0.243921 0.299889 0.064 Uiso 1 1 calc R U . . .
H10B H 1.026952 0.124526 0.322859 0.064 Uiso 1 1 calc R U . . .
H10C H 1.002465 0.264230 0.335353 0.064 Uiso 1 1 calc R U . . .
N11 N 0.3540(10) 0.3351(10) 0.3058(2) 0.0374(19) Uani 1 1 d . . . . .
H11A H 0.266415 0.418064 0.308016 0.056 Uiso 1 1 calc R U . . .
H11B H 0.351420 0.258054 0.316682 0.056 Uiso 1 1 calc R U . . .
H11C H 0.371254 0.317433 0.284341 0.056 Uiso 1 1 calc R U . . .
N12 N 0.4217(10) 0.9204(9) 0.2788(2) 0.0357(18) Uani 1 1 d . . . . .
H12A H 0.328051 0.936457 0.280615 0.054 Uiso 1 1 calc R U . . .
H12B H 0.433499 0.957092 0.258957 0.054 Uiso 1 1 calc R U . . .
H12C H 0.439520 0.965815 0.294615 0.054 Uiso 1 1 calc R U . . .
C13 C 0.7439(10) 0.4540(10) 0.3095(2) 0.0295(19) Uani 1 1 d . . . . .
H13D H 0.793921 0.492838 0.322466 0.035 Uiso 1 1 calc R U . . .
H13E H 0.754630 0.477478 0.286215 0.035 Uiso 1 1 calc R U . . .
C14 C 0.8195(10) 0.2854(11) 0.3159(3) 0.032(2) Uani 1 1 d . . . . .
H14D H 0.780880 0.260947 0.336202 0.039 Uiso 1 1 calc R U . . .
H14E H 0.797709 0.241591 0.297752 0.039 Uiso 1 1 calc R U . . .
C15 C 0.4852(11) 0.4821(11) 0.2999(2) 0.0289(19) Uani 1 1 d . . . . .
H15D H 0.529950 0.449117 0.278338 0.035 Uiso 1 1 calc R U . . .
H15E H 0.385119 0.566513 0.296215 0.035 Uiso 1 1 calc R U . . .
C16 C 0.4749(11) 0.3544(11) 0.3194(3) 0.033(2) Uani 1 1 d . . . . .
H16D H 0.569778 0.262121 0.318145 0.039 Uiso 1 1 calc R U . . .
H16E H 0.454771 0.376801 0.342592 0.039 Uiso 1 1 calc R U . . .
C17 C 0.5127(11) 0.6969(11) 0.3160(2) 0.0308(19) Uani 1 1 d . . . . .
H17D H 0.562125 0.724264 0.332115 0.037 Uiso 1 1 calc R U . . .
H17E H 0.407231 0.742552 0.321855 0.037 Uiso 1 1 calc R U . . .
C18 C 0.5273(13) 0.7585(12) 0.2822(3) 0.039(2) Uani 1 1 d . . . . .
H18D H 0.629169 0.740341 0.278995 0.047 Uiso 1 1 calc R U . . .
H18E H 0.506189 0.708321 0.265352 0.047 Uiso 1 1 calc R U . . .
N13 N 0.3197(7) 0.8581(8) 0.44079(17) 0.0212(14) Uani 1 1 d . . . . .
H13 H 0.318773 0.854245 0.465122 0.025 Uiso 1 1 calc R U . . .
N14 N 0.6630(9) 0.9106(11) 0.4400(2) 0.039(2) Uani 1 1 d . . . . .
H14A H 0.732927 0.814487 0.439794 0.058 Uiso 1 1 calc R U . . .
H14B H 0.691736 0.957053 0.453430 0.058 Uiso 1 1 calc R U . . .
H14C H 0.650379 0.953291 0.419535 0.058 Uiso 1 1 calc R U . . .
N15 N 0.3908(10) 0.4602(10) 0.4415(2) 0.039(2) Uani 1 1 d . . . . .
H15A H 0.298835 0.471486 0.441279 0.059 Uiso 1 1 calc R U . . .
H15B H 0.450327 0.379101 0.454241 0.059 Uiso 1 1 calc R U . . .
H15C H 0.426837 0.449643 0.420864 0.059 Uiso 1 1 calc R U . . .
N16 N -0.0719(9) 1.1957(10) 0.4381(2) 0.041(2) Uani 1 1 d . . . . .
H16A H -0.042793 1.264548 0.436547 0.061 Uiso 1 1 calc R U . . .
H16B H -0.148809 1.223795 0.452103 0.061 Uiso 1 1 calc R U . . .
H16C H -0.099993 1.186112 0.418194 0.061 Uiso 1 1 calc R U . . .
C19 C 0.4683(9) 0.8449(11) 0.4292(2) 0.0260(18) Uani 1 1 d . . . . .
H19D H 0.543610 0.739828 0.428819 0.031 Uiso 1 1 calc R U . . .
H19E H 0.457124 0.889786 0.406800 0.031 Uiso 1 1 calc R U . . .
C20 C 0.5199(11) 0.9221(12) 0.4520(3) 0.033(2) Uani 1 1 d . . . . .
H20D H 0.444015 1.026832 0.452689 0.040 Uiso 1 1 calc R U . . .
H20E H 0.533231 0.875961 0.474309 0.040 Uiso 1 1 calc R U . . .
C21 C 0.3047(10) 0.7280(10) 0.4301(2) 0.0274(18) Uani 1 1 d . . . . .
H21D H 0.347985 0.701685 0.408153 0.033 Uiso 1 1 calc R U . . .
H21E H 0.199387 0.756354 0.428852 0.033 Uiso 1 1 calc R U . . .
C22 C 0.3850(11) 0.5937(10) 0.4547(2) 0.0297(19) Uani 1 1 d . . . . .
H22D H 0.486141 0.574995 0.458562 0.036 Uiso 1 1 calc R U . . .
H22E H 0.332102 0.614498 0.475754 0.036 Uiso 1 1 calc R U . . .
C23 C 0.1902(9) 1.0062(10) 0.4285(2) 0.0252(17) Uani 1 1 d . . . . .
H23D H 0.164955 0.998823 0.405985 0.030 Uiso 1 1 calc R U . . .
H23E H 0.219725 1.082771 0.428065 0.030 Uiso 1 1 calc R U . . .
C24 C 0.0533(10) 1.0515(11) 0.4505(2) 0.031(2) Uani 1 1 d . . . . .
H24D H 0.023541 0.975062 0.450954 0.038 Uiso 1 1 calc R U . . .
H24E H 0.078111 1.059440 0.472988 0.038 Uiso 1 1 calc R U . . .
Sb1 Sb 0.000000 0.500000 0.000000 0.0209(2) Uani 1 2 d S . P . .
Cl1 Cl -0.2122(3) 0.7579(3) -0.02627(7) 0.0414(6) Uani 1 1 d . . . . .
Cl2 Cl 0.2184(3) 0.5462(3) -0.02352(7) 0.0397(6) Uani 1 1 d . . . . .
Cl3 Cl -0.0122(3) 0.6261(3) 0.05631(7) 0.0425(6) Uani 1 1 d . . . . .
Sb2 Sb 0.000000 0.500000 0.500000 0.0255(2) Uani 1 2 d S . P . .
Cl4 Cl 0.000(2) 0.275(3) 0.5364(9) 0.079(6) Uani 0.56(5) 1 d . U P A 1
Cl5 Cl 0.227(2) 0.474(2) 0.5346(5) 0.055(4) Uani 0.56(5) 1 d . U P A 1
Cl6 Cl 0.164(2) 0.339(2) 0.4492(5) 0.057(3) Uani 0.56(5) 1 d . U P A 1
Cl4' Cl 0.013(2) 0.256(2) 0.5261(5) 0.041(4) Uani 0.44(5) 1 d . U P A 2
Cl5' Cl 0.250(3) 0.447(3) 0.5278(6) 0.043(4) Uani 0.44(5) 1 d . U P A 2
Cl6' Cl 0.196(2) 0.300(3) 0.4622(11) 0.068(6) Uani 0.44(5) 1 d . U P A 2
Sb3 Sb 0.95372(6) 0.79102(7) 0.33289(2) 0.02582(18) Uani 1 1 d . . . . .
Cl7 Cl 0.7932(3) 0.7192(3) 0.36839(7) 0.0451(6) Uani 1 1 d . . . . .
Cl8 Cl 1.1848(3) 0.5972(4) 0.36441(8) 0.0578(8) Uani 1 1 d . . . . .
Cl9 Cl 0.9135(4) 0.9941(4) 0.37616(8) 0.0549(8) Uani 1 1 d . . . . .
Cl10 Cl 0.6976(3) 0.9889(3) 0.29446(7) 0.0446(6) Uani 1 1 d . . . . .
Cl11 Cl 1.0028(3) 0.5830(3) 0.29190(6) 0.0409(6) Uani 1 1 d . . . . .
Cl12 Cl 1.1267(3) 0.8834(4) 0.28682(8) 0.0490(7) Uani 1 1 d . . . . .
Sb4 Sb 0.36797(6) 0.11801(7) 0.16597(2) 0.02453(18) Uani 1 1 d . . . . .
Cl13 Cl 0.3806(4) 0.2548(4) 0.23009(8) 0.0533(7) Uani 1 1 d . . . . .
Cl14 Cl 0.3731(3) -0.0156(3) 0.11747(6) 0.0397(6) Uani 1 1 d . . . . .
Cl15 Cl 0.2406(3) 0.3702(3) 0.12869(6) 0.0359(5) Uani 1 1 d . . . . .
Cl16 Cl 0.6339(3) 0.0821(4) 0.15063(6) 0.0441(7) Uani 1 1 d . . . . .
Cl17 Cl 0.5077(3) -0.1441(3) 0.20088(6) 0.0429(6) Uani 1 1 d . . . . .
Cl18 Cl 0.1054(3) 0.1399(4) 0.18033(9) 0.0567(8) Uani 1 1 d . . . . .
Cl19 Cl 0.6322(3) 0.4397(4) 0.39076(6) 0.0494(7) Uani 1 1 d . . . . .
Cl20 Cl 0.3278(3) 0.0803(3) 0.34704(6) 0.0412(6) Uani 1 1 d . . . . .
Cl21 Cl 0.7037(4) 0.4261(3) 0.22419(7) 0.0538(8) Uani 1 1 d . . . . .
Cl22 Cl 0.0570(3) 0.8220(3) 0.12269(6) 0.0454(6) Uani 1 1 d . . . . .
Cl23 Cl 0.5813(3) 0.5624(3) 0.11133(7) 0.0425(6) Uani 1 1 d . . . . .
Cl24 Cl 0.3236(3) 0.8224(3) 0.02030(5) 0.0311(5) Uani 1 1 d . . . . .
Cl25 Cl 0.6673(3) 0.1679(3) 0.48126(6) 0.0336(5) Uani 1 1 d . . . . .
O1 O 0.561(3) 1.113(3) 0.3874(8) 0.070(8) Uani 0.5 1 d . U P B 1
O1' O 0.518(3) 1.170(3) 0.3961(6) 0.057(6) Uani 0.5 1 d . U P C 2
O2 O 0.0006(12) 0.3468(12) 0.3792(3) 0.068(3) Uani 1 1 d . . . . .
O3 O 0.9714(9) 0.3353(10) 0.0969(2) 0.0470(19) Uani 1 1 d . . . . .
O4 O 0.121(16) 0.211(15) 0.2569(16) 0.075(17) Uani 0.4(3) 1 d . . P D 1
O4' O 0.068(14) 0.271(17) 0.2557(14) 0.081(18) Uani 0.6(3) 1 d . . P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.506(10) . ?
N1 C3 1.516(11) . ?
N1 C5 1.520(10) . ?
N1 H1 0.9800 . ?
N2 C2 1.485(12) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 C4 1.483(12) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N4 C6 1.494(12) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
C1 C2 1.512(12) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C3 C4 1.515(12) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C4 H4D 0.9700 . ?
C4 H4E 0.9700 . ?
C5 C6 1.506(12) . ?
C5 H5D 0.9700 . ?
C5 H5E 0.9700 . ?
C6 H6D 0.9700 . ?
C6 H6E 0.9700 . ?
N5 C7 1.510(11) . ?
N5 C11 1.520(11) . ?
N5 C9 1.521(12) . ?
N5 H5 0.9800 . ?
N6 C8 1.484(14) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N7 C10 1.482(12) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 H7C 0.8900 . ?
N8 C12 1.480(13) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 H8C 0.8900 . ?
C7 C8 1.522(13) . ?
C7 H7D 0.9700 . ?
C7 H7E 0.9700 . ?
C8 H8D 0.9700 . ?
C8 H8E 0.9700 . ?
C9 C10 1.531(12) . ?
C9 H9D 0.9700 . ?
C9 H9E 0.9700 . ?
C10 H10D 0.9700 . ?
C10 H10E 0.9700 . ?
C11 C12 1.501(13) . ?
C11 H11D 0.9700 . ?
C11 H11E 0.9700 . ?
C12 H12D 0.9700 . ?
C12 H12E 0.9700 . ?
N9 C17 1.490(12) . ?
N9 C15 1.512(11) . ?
N9 C13 1.515(11) . ?
N9 H9 0.9800 . ?
N10 C14 1.474(12) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 H10C 0.8900 . ?
N11 C16 1.473(12) . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 H11C 0.8900 . ?
N12 C18 1.470(13) . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N12 H12C 0.8900 . ?
C13 C14 1.515(13) . ?
C13 H13D 0.9700 . ?
C13 H13E 0.9700 . ?
C14 H14D 0.9700 . ?
C14 H14E 0.9700 . ?
C15 C16 1.530(13) . ?
C15 H15D 0.9700 . ?
C15 H15E 0.9700 . ?
C16 H16D 0.9700 . ?
C16 H16E 0.9700 . ?
C17 C18 1.500(13) . ?
C17 H17D 0.9700 . ?
C17 H17E 0.9700 . ?
C18 H18D 0.9700 . ?
C18 H18E 0.9700 . ?
N13 C23 1.506(10) . ?
N13 C21 1.510(11) . ?
N13 C19 1.519(10) . ?
N13 H13 0.9800 . ?
N14 C20 1.477(12) . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
N14 H14C 0.8900 . ?
N15 C22 1.480(13) . ?
N15 H15A 0.8900 . ?
N15 H15B 0.8900 . ?
N15 H15C 0.8900 . ?
N16 C24 1.468(13) . ?
N16 H16A 0.8900 . ?
N16 H16B 0.8900 . ?
N16 H16C 0.8900 . ?
C19 C20 1.515(13) . ?
C19 H19D 0.9700 . ?
C19 H19E 0.9700 . ?
C20 H20D 0.9700 . ?
C20 H20E 0.9700 . ?
C21 C22 1.522(13) . ?
C21 H21D 0.9700 . ?
C21 H21E 0.9700 . ?
C22 H22D 0.9700 . ?
C22 H22E 0.9700 . ?
C23 C24 1.518(12) . ?
C23 H23D 0.9700 . ?
C23 H23E 0.9700 . ?
C24 H24D 0.9700 . ?
C24 H24E 0.9700 . ?
Sb1 Cl1 2.637(2) . ?
Sb1 Cl1 2.637(2) 2_565 ?
Sb1 Cl2 2.639(2) 2_565 ?
Sb1 Cl2 2.639(2) . ?
Sb1 Cl3 2.662(3) 2_565 ?
Sb1 Cl3 2.662(3) . ?
Sb2 Cl4' 2.593(18) . ?
Sb2 Cl4' 2.593(18) 2_566 ?
Sb2 Cl6' 2.602(15) . ?
Sb2 Cl6' 2.602(15) 2_566 ?
Sb2 Cl5' 2.61(2) . ?
Sb2 Cl5' 2.61(2) 2_566 ?
Sb2 Cl5 2.641(17) . ?
Sb2 Cl5 2.641(17) 2_566 ?
Sb2 Cl4 2.657(18) 2_566 ?
Sb2 Cl4 2.657(18) . ?
Sb2 Cl6 2.697(12) . ?
Sb2 Cl6 2.697(12) 2_566 ?
Sb3 Cl7 2.488(3) . ?
Sb3 Cl8 2.526(3) . ?
Sb3 Cl11 2.633(3) . ?
Sb3 Cl9 2.679(3) . ?
Sb3 Cl10 2.826(3) . ?
Sb3 Cl12 2.948(3) . ?
Sb4 Cl14 2.451(3) . ?
Sb4 Cl16 2.619(3) . ?
Sb4 Cl18 2.632(3) . ?
Sb4 Cl15 2.634(3) . ?
Sb4 Cl17 2.663(3) . ?
Sb4 Cl13 3.064(3) . ?

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
C1 N1 C3 109.1(6) . . ?
C1 N1 C5 110.7(6) . . ?
C3 N1 C5 111.8(6) . . ?
C1 N1 H1 108.4 . . ?
C3 N1 H1 108.4 . . ?
C5 N1 H1 108.4 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C2 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N3 H3A 109.5 . . ?
C4 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C4 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C6 N4 H4A 109.5 . . ?
C6 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C6 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
N1 C1 C2 112.8(7) . . ?
N1 C1 H1D 109.0 . . ?
C2 C1 H1D 109.0 . . ?
N1 C1 H1E 109.0 . . ?
C2 C1 H1E 109.0 . . ?
H1D C1 H1E 107.8 . . ?
N2 C2 C1 109.6(8) . . ?
N2 C2 H2D 109.8 . . ?
C1 C2 H2D 109.8 . . ?
N2 C2 H2E 109.8 . . ?
C1 C2 H2E 109.8 . . ?
H2D C2 H2E 108.2 . . ?
C4 C3 N1 111.6(7) . . ?
C4 C3 H3D 109.3 . . ?
N1 C3 H3D 109.3 . . ?
C4 C3 H3E 109.3 . . ?
N1 C3 H3E 109.3 . . ?
H3D C3 H3E 108.0 . . ?
N3 C4 C3 109.9(7) . . ?
N3 C4 H4D 109.7 . . ?
C3 C4 H4D 109.7 . . ?
N3 C4 H4E 109.7 . . ?
C3 C4 H4E 109.7 . . ?
H4D C4 H4E 108.2 . . ?
C6 C5 N1 110.6(7) . . ?
C6 C5 H5D 109.5 . . ?
N1 C5 H5D 109.5 . . ?
C6 C5 H5E 109.5 . . ?
N1 C5 H5E 109.5 . . ?
H5D C5 H5E 108.1 . . ?
N4 C6 C5 110.5(7) . . ?
N4 C6 H6D 109.6 . . ?
C5 C6 H6D 109.6 . . ?
N4 C6 H6E 109.6 . . ?
C5 C6 H6E 109.6 . . ?
H6D C6 H6E 108.1 . . ?
C7 N5 C11 111.1(7) . . ?
C7 N5 C9 112.0(7) . . ?
C11 N5 C9 109.6(7) . . ?
C7 N5 H5 108.0 . . ?
C11 N5 H5 108.0 . . ?
C9 N5 H5 108.0 . . ?
C8 N6 H6A 109.5 . . ?
C8 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C8 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C10 N7 H7A 109.5 . . ?
C10 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C10 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C12 N8 H8A 109.5 . . ?
C12 N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
C12 N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
N5 C7 C8 115.5(8) . . ?
N5 C7 H7D 108.4 . . ?
C8 C7 H7D 108.4 . . ?
N5 C7 H7E 108.4 . . ?
C8 C7 H7E 108.4 . . ?
H7D C7 H7E 107.5 . . ?
N6 C8 C7 113.7(9) . . ?
N6 C8 H8D 108.8 . . ?
C7 C8 H8D 108.8 . . ?
N6 C8 H8E 108.8 . . ?
C7 C8 H8E 108.8 . . ?
H8D C8 H8E 107.7 . . ?
N5 C9 C10 111.0(7) . . ?
N5 C9 H9D 109.4 . . ?
C10 C9 H9D 109.4 . . ?
N5 C9 H9E 109.4 . . ?
C10 C9 H9E 109.4 . . ?
H9D C9 H9E 108.0 . . ?
N7 C10 C9 109.1(8) . . ?
N7 C10 H10D 109.9 . . ?
C9 C10 H10D 109.9 . . ?
N7 C10 H10E 109.9 . . ?
C9 C10 H10E 109.9 . . ?
H10D C10 H10E 108.3 . . ?
C12 C11 N5 111.9(7) . . ?
C12 C11 H11D 109.2 . . ?
N5 C11 H11D 109.2 . . ?
C12 C11 H11E 109.2 . . ?
N5 C11 H11E 109.2 . . ?
H11D C11 H11E 107.9 . . ?
N8 C12 C11 108.7(8) . . ?
N8 C12 H12D 109.9 . . ?
C11 C12 H12D 109.9 . . ?
N8 C12 H12E 109.9 . . ?
C11 C12 H12E 109.9 . . ?
H12D C12 H12E 108.3 . . ?
C17 N9 C15 111.9(7) . . ?
C17 N9 C13 110.9(7) . . ?
C15 N9 C13 115.3(7) . . ?
C17 N9 H9 106.0 . . ?
C15 N9 H9 106.0 . . ?
C13 N9 H9 106.0 . . ?
C14 N10 H10A 109.5 . . ?
C14 N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
C14 N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
C16 N11 H11A 109.5 . . ?
C16 N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
C16 N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
C18 N12 H12A 109.5 . . ?
C18 N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
C18 N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
N9 C13 C14 112.4(7) . . ?
N9 C13 H13D 109.1 . . ?
C14 C13 H13D 109.1 . . ?
N9 C13 H13E 109.1 . . ?
C14 C13 H13E 109.1 . . ?
H13D C13 H13E 107.9 . . ?
N10 C14 C13 109.7(8) . . ?
N10 C14 H14D 109.7 . . ?
C13 C14 H14D 109.7 . . ?
N10 C14 H14E 109.7 . . ?
C13 C14 H14E 109.7 . . ?
H14D C14 H14E 108.2 . . ?
N9 C15 C16 111.0(7) . . ?
N9 C15 H15D 109.4 . . ?
C16 C15 H15D 109.4 . . ?
N9 C15 H15E 109.4 . . ?
C16 C15 H15E 109.4 . . ?
H15D C15 H15E 108.0 . . ?
N11 C16 C15 110.0(8) . . ?
N11 C16 H16D 109.7 . . ?
C15 C16 H16D 109.7 . . ?
N11 C16 H16E 109.7 . . ?
C15 C16 H16E 109.7 . . ?
H16D C16 H16E 108.2 . . ?
N9 C17 C18 113.2(8) . . ?
N9 C17 H17D 108.9 . . ?
C18 C17 H17D 108.9 . . ?
N9 C17 H17E 108.9 . . ?
C18 C17 H17E 108.9 . . ?
H17D C17 H17E 107.7 . . ?
N12 C18 C17 109.9(8) . . ?
N12 C18 H18D 109.7 . . ?
C17 C18 H18D 109.7 . . ?
N12 C18 H18E 109.7 . . ?
C17 C18 H18E 109.7 . . ?
H18D C18 H18E 108.2 . . ?
C23 N13 C21 111.6(6) . . ?
C23 N13 C19 110.8(6) . . ?
C21 N13 C19 110.6(7) . . ?
C23 N13 H13 107.9 . . ?
C21 N13 H13 107.9 . . ?
C19 N13 H13 107.9 . . ?
C20 N14 H14A 109.5 . . ?
C20 N14 H14B 109.5 . . ?
H14A N14 H14B 109.5 . . ?
C20 N14 H14C 109.5 . . ?
H14A N14 H14C 109.5 . . ?
H14B N14 H14C 109.5 . . ?
C22 N15 H15A 109.5 . . ?
C22 N15 H15B 109.5 . . ?
H15A N15 H15B 109.5 . . ?
C22 N15 H15C 109.5 . . ?
H15A N15 H15C 109.5 . . ?
H15B N15 H15C 109.5 . . ?
C24 N16 H16A 109.5 . . ?
C24 N16 H16B 109.5 . . ?
H16A N16 H16B 109.5 . . ?
C24 N16 H16C 109.5 . . ?
H16A N16 H16C 109.5 . . ?
H16B N16 H16C 109.5 . . ?
C20 C19 N13 111.0(7) . . ?
C20 C19 H19D 109.4 . . ?
N13 C19 H19D 109.4 . . ?
C20 C19 H19E 109.4 . . ?
N13 C19 H19E 109.4 . . ?
H19D C19 H19E 108.0 . . ?
N14 C20 C19 110.2(8) . . ?
N14 C20 H20D 109.6 . . ?
C19 C20 H20D 109.6 . . ?
N14 C20 H20E 109.6 . . ?
C19 C20 H20E 109.6 . . ?
H20D C20 H20E 108.1 . . ?
N13 C21 C22 109.9(7) . . ?
N13 C21 H21D 109.7 . . ?
C22 C21 H21D 109.7 . . ?
N13 C21 H21E 109.7 . . ?
C22 C21 H21E 109.7 . . ?
H21D C21 H21E 108.2 . . ?
N15 C22 C21 109.6(8) . . ?
N15 C22 H22D 109.8 . . ?
C21 C22 H22D 109.8 . . ?
N15 C22 H22E 109.8 . . ?
C21 C22 H22E 109.8 . . ?
H22D C22 H22E 108.2 . . ?
N13 C23 C24 111.4(7) . . ?
N13 C23 H23D 109.4 . . ?
C24 C23 H23D 109.4 . . ?
N13 C23 H23E 109.4 . . ?
C24 C23 H23E 109.4 . . ?
H23D C23 H23E 108.0 . . ?
N16 C24 C23 110.7(8) . . ?
N16 C24 H24D 109.5 . . ?
C23 C24 H24D 109.5 . . ?
N16 C24 H24E 109.5 . . ?
C23 C24 H24E 109.5 . . ?
H24D C24 H24E 108.1 . . ?
Cl1 Sb1 Cl1 180.0 . 2_565 ?
Cl1 Sb1 Cl2 86.67(8) . 2_565 ?
Cl1 Sb1 Cl2 93.33(8) 2_565 2_565 ?
Cl1 Sb1 Cl2 93.33(8) . . ?
Cl1 Sb1 Cl2 86.67(8) 2_565 . ?
Cl2 Sb1 Cl2 180.0 2_565 . ?
Cl1 Sb1 Cl3 89.28(9) . 2_565 ?
Cl1 Sb1 Cl3 90.72(9) 2_565 2_565 ?
Cl2 Sb1 Cl3 92.27(9) 2_565 2_565 ?
Cl2 Sb1 Cl3 87.73(9) . 2_565 ?
Cl1 Sb1 Cl3 90.72(9) . . ?
Cl1 Sb1 Cl3 89.28(9) 2_565 . ?
Cl2 Sb1 Cl3 87.73(9) 2_565 . ?
Cl2 Sb1 Cl3 92.27(9) . . ?
Cl3 Sb1 Cl3 180.0 2_565 . ?
Cl4' Sb2 Cl6' 78.2(11) . . ?
Cl4' Sb2 Cl6' 101.8(11) 2_566 . ?
Cl4' Sb2 Cl6' 101.8(11) . 2_566 ?
Cl4' Sb2 Cl6' 78.2(11) 2_566 2_566 ?
Cl6' Sb2 Cl6' 180.0 . 2_566 ?
Cl4' Sb2 Cl5' 93.7(6) . . ?
Cl4' Sb2 Cl5' 86.3(6) 2_566 . ?
Cl6' Sb2 Cl5' 79.3(13) . . ?
Cl6' Sb2 Cl5' 100.7(13) 2_566 . ?
Cl5 Sb2 Cl5 180.0(8) . 2_566 ?
Cl5 Sb2 Cl4 89.0(8) . 2_566 ?
Cl5 Sb2 Cl4 91.0(7) 2_566 2_566 ?
Cl5 Sb2 Cl4 91.0(7) . . ?
Cl5 Sb2 Cl4 89.0(7) 2_566 . ?
Cl4 Sb2 Cl4 180.0 2_566 . ?
Cl5 Sb2 Cl6 96.6(8) . . ?
Cl5 Sb2 Cl6 83.4(8) 2_566 . ?
Cl4 Sb2 Cl6 83.0(12) 2_566 . ?
Cl4 Sb2 Cl6 97.0(12) . . ?
Cl5 Sb2 Cl6 83.4(8) . 2_566 ?
Cl5 Sb2 Cl6 96.6(8) 2_566 2_566 ?
Cl4 Sb2 Cl6 97.0(12) 2_566 2_566 ?
Cl4 Sb2 Cl6 83.0(12) . 2_566 ?
Cl6 Sb2 Cl6 180.0(9) . 2_566 ?
Cl7 Sb3 Cl8 90.56(12) . . ?
Cl7 Sb3 Cl11 90.85(9) . . ?
Cl8 Sb3 Cl11 87.46(10) . . ?
Cl7 Sb3 Cl9 89.02(11) . . ?
Cl8 Sb3 Cl9 90.15(11) . . ?
Cl11 Sb3 Cl9 177.60(9) . . ?
Cl7 Sb3 Cl10 88.92(10) . . ?
Cl8 Sb3 Cl10 175.31(10) . . ?
Cl11 Sb3 Cl10 87.89(9) . . ?
Cl9 Sb3 Cl10 94.50(10) . . ?
Cl7 Sb3 Cl12 175.64(9) . . ?
Cl8 Sb3 Cl12 93.32(11) . . ?
Cl11 Sb3 Cl12 87.34(9) . . ?
Cl9 Sb3 Cl12 92.96(10) . . ?
Cl10 Sb3 Cl12 87.05(9) . . ?
Cl14 Sb4 Cl16 90.40(9) . . ?
Cl14 Sb4 Cl18 87.21(10) . . ?
Cl16 Sb4 Cl18 176.99(11) . . ?
Cl14 Sb4 Cl15 88.75(9) . . ?
Cl16 Sb4 Cl15 90.37(9) . . ?
Cl18 Sb4 Cl15 91.41(10) . . ?
Cl14 Sb4 Cl17 88.97(10) . . ?
Cl16 Sb4 Cl17 87.36(9) . . ?
Cl18 Sb4 Cl17 90.77(10) . . ?
Cl15 Sb4 Cl17 176.77(9) . . ?
Cl14 Sb4 Cl13 174.37(9) . . ?
Cl16 Sb4 Cl13 88.71(9) . . ?
Cl18 Sb4 Cl13 93.49(10) . . ?
Cl15 Sb4 Cl13 96.82(9) . . ?
Cl17 Sb4 Cl13 85.44(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 C2 78.7(9) . . . . ?
C5 N1 C1 C2 -157.9(7) . . . . ?
N1 C1 C2 N2 -168.9(7) . . . . ?
C1 N1 C3 C4 -161.2(7) . . . . ?
C5 N1 C3 C4 75.9(9) . . . . ?
N1 C3 C4 N3 179.3(7) . . . . ?
C1 N1 C5 C6 85.1(8) . . . . ?
C3 N1 C5 C6 -153.0(7) . . . . ?
N1 C5 C6 N4 -165.5(7) . . . . ?
C11 N5 C7 C8 -158.4(8) . . . . ?
C9 N5 C7 C8 78.7(10) . . . . ?
N5 C7 C8 N6 82.8(11) . . . . ?
C7 N5 C9 C10 -155.4(8) . . . . ?
C11 N5 C9 C10 80.9(9) . . . . ?
N5 C9 C10 N7 -176.8(7) . . . . ?
C7 N5 C11 C12 69.5(9) . . . . ?
C9 N5 C11 C12 -166.3(7) . . . . ?
N5 C11 C12 N8 165.2(7) . . . . ?
C17 N9 C13 C14 172.4(8) . . . . ?
C15 N9 C13 C14 -59.0(10) . . . . ?
N9 C13 C14 N10 -159.5(8) . . . . ?
C17 N9 C15 C16 -139.4(8) . . . . ?
C13 N9 C15 C16 92.6(9) . . . . ?
N9 C15 C16 N11 165.4(8) . . . . ?
C15 N9 C17 C18 -71.6(10) . . . . ?
C13 N9 C17 C18 58.7(10) . . . . ?
N9 C17 C18 N12 162.3(8) . . . . ?
C23 N13 C19 C20 83.1(9) . . . . ?
C21 N13 C19 C20 -152.7(8) . . . . ?
N13 C19 C20 N14 -178.9(7) . . . . ?
C23 N13 C21 C22 -152.8(7) . . . . ?
C19 N13 C21 C22 83.4(9) . . . . ?
N13 C21 C22 N15 -171.1(7) . . . . ?
C21 N13 C23 C24 80.8(9) . . . . ?
C19 N13 C23 C24 -155.6(7) . . . . ?
N13 C23 C24 N16 -179.9(8) . . . . ?

_refine_diff_density_max         1.068
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.153

