# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_taseg1
_database_code_depnum_ccdc_archive 'CCDC 1882534'
loop_
_audit_author_name
_audit_author_address
'Babu Varghese'
;SAIF, IIT Madras
India
;
_audit_update_record             
;
2019-02-05 deposited with the CCDC.	2019-02-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H47 Cl2 Se7 Ta3'
_chemical_formula_weight         1586.15

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -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'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   15.9449(6)
_cell_length_b                   17.1036(6)
_cell_length_c                   16.1118(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4393.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4566
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      24.5

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_F_000             2896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    13.392
_shelx_estimated_absorpt_T_min   0.135
_shelx_estimated_absorpt_T_max   0.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_T_max  0.27
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12872
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.746
_diffrn_reflns_theta_max         25.231
_diffrn_reflns_theta_full        25.231
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3571
_reflns_number_gt                3290
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'

_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)+(0.0438P)²+6.1121P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3571
_refine_ls_number_parameters     254
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.046
_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
C1 C 0.2175(17) 0.8404(12) 0.2713(15) 0.129(12) Uani 1 1 d D . . . .
H1A H 0.186431 0.828811 0.320822 0.194 Uiso 1 1 calc R U . . .
H1B H 0.275157 0.849707 0.285254 0.194 Uiso 1 1 calc R U . . .
H1C H 0.194462 0.886091 0.245279 0.194 Uiso 1 1 calc R U . . .
C2 C 0.2120(10) 0.7734(9) 0.2135(11) 0.061(5) Uani 1 1 d D . . . .
C3 C 0.2486(11) 0.7670(9) 0.1345(12) 0.078(8) Uani 1 1 d D . . . .
C4 C 0.2350(9) 0.6903(10) 0.1064(9) 0.060(5) Uani 1 1 d D . . . .
C5 C 0.1883(11) 0.6485(7) 0.1649(11) 0.066(6) Uani 1 1 d D . . . .
C6 C 0.1736(11) 0.7011(8) 0.2313(9) 0.057(5) Uani 1 1 d D . . . .
C7 C 0.3035(12) 0.8223(15) 0.0856(19) 0.121(10) Uani 1 1 d D . . . .
H7A H 0.317462 0.799044 0.033176 0.182 Uiso 1 1 calc R U . . .
H7B H 0.273932 0.870452 0.076365 0.182 Uiso 1 1 calc R U . . .
H7C H 0.353971 0.832668 0.116169 0.182 Uiso 1 1 calc R U . . .
C8 C 0.2717(16) 0.6492(16) 0.0338(11) 0.126(12) Uani 1 1 d D . . . .
H8A H 0.301556 0.686065 -0.000081 0.189 Uiso 1 1 calc R U . . .
H8B H 0.309582 0.609458 0.052747 0.189 Uiso 1 1 calc R U . . .
H8C H 0.227635 0.625658 0.001809 0.189 Uiso 1 1 calc R U . . .
C9 C 0.1727(17) 0.5632(9) 0.163(2) 0.130(11) Uani 1 1 d D . . . .
H9A H 0.138981 0.548832 0.210279 0.195 Uiso 1 1 calc R U . . .
H9B H 0.143714 0.549667 0.113097 0.195 Uiso 1 1 calc R U . . .
H9C H 0.225177 0.535828 0.165557 0.195 Uiso 1 1 calc R U . . .
C10 C 0.1409(15) 0.6878(17) 0.3174(12) 0.128(11) Uani 1 1 d D . . . .
H10A H 0.116504 0.636631 0.320929 0.192 Uiso 1 1 calc R U . . .
H10B H 0.186154 0.691987 0.356467 0.192 Uiso 1 1 calc R U . . .
H10C H 0.099038 0.726421 0.330045 0.192 Uiso 1 1 calc R U . . .
C11 C 0.000000 1.0554(10) -0.0657(14) 0.071(9) Uani 1 2 d DS T P . .
H11A H -0.056725 1.070863 -0.054294 0.106 Uiso 0.5 1 calc R U P . .
H11B H 0.030196 1.050157 -0.014488 0.106 Uiso 0.5 1 calc R U P . .
H11C H 0.026528 1.094432 -0.099606 0.106 Uiso 0.5 1 calc R U P . .
C12 C 0.000000 0.9783(9) -0.1110(12) 0.040(5) Uani 1 2 d DS T P . .
C13 C -0.0709(7) 0.9367(7) -0.1383(8) 0.035(3) Uani 1 1 d D . . . .
C14 C -0.0447(8) 0.8693(7) -0.1817(7) 0.035(3) Uani 1 1 d D . . . .
C15 C -0.1615(8) 0.9625(10) -0.1290(10) 0.055(5) Uani 1 1 d D . . . .
H15A H -0.197801 0.923720 -0.152810 0.083 Uiso 1 1 calc R U . . .
H15B H -0.174508 0.968625 -0.071179 0.083 Uiso 1 1 calc R U . . .
H15C H -0.169529 1.011414 -0.157084 0.083 Uiso 1 1 calc R U . . .
C16 C -0.1000(11) 0.8198(10) -0.2335(10) 0.060(5) Uani 1 1 d D . . . .
H16A H -0.068026 0.777460 -0.256589 0.091 Uiso 1 1 calc R U . . .
H16B H -0.144518 0.799143 -0.199960 0.091 Uiso 1 1 calc R U . . .
H16C H -0.123237 0.850667 -0.277626 0.091 Uiso 1 1 calc R U . . .
Se1 Se 0.12047(10) 0.75851(7) -0.04208(10) 0.0377(3) Uani 1 1 d . . . . .
Se2 Se 0.10905(9) 0.90416(8) 0.06906(9) 0.0343(3) Uani 1 1 d . . . . .
Se3 Se 0.0608(2) 0.99567(17) 0.1571(2) 0.0495(8) Uani 0.5 1 d . . P . .
Se4 Se 0.000000 0.63796(11) 0.09561(14) 0.0439(6) Uani 1 2 d S T P . .
Se5 Se 0.000000 0.80744(11) 0.22390(11) 0.0348(5) Uani 1 2 d S T P . .
Ta1 Ta 0.000000 0.85007(4) -0.03818(4) 0.02331(18) Uani 1 2 d S T P . .
Ta2 Ta 0.09674(3) 0.75199(3) 0.11421(5) 0.02852(15) Uani 1 1 d . . . . .
C17 C 0.000000 0.570(4) -0.122(3) 0.154(12) Uani 0.699(15) 2 d DS TU P A 1
Cl1 Cl -0.1038(14) 0.5346(12) -0.1098(14) 0.138(8) Uani 0.349(7) 1 d D U P A 1
Cl2 Cl 0.000000 0.5895(11) -0.2278(13) 0.178(8) Uani 0.699(15) 2 d DS TU P A 1
C17A C 0.000000 0.576(4) -0.445(5) 0.08(3) Uani 0.096(17) 2 d DS TU P B 2
Cl1A Cl 0.000000 0.605(4) -0.342(4) 0.08(3) Uani 0.096(17) 2 d DS TU P B 2
Cl2A Cl 0.000000 0.658(4) -0.506(4) 0.07(2) Uani 0.096(17) 2 d DS TU P B 2
C17B C 0.000000 0.629(3) -0.531(4) 0.11(3) Uani 0.21(2) 2 d DS TU P C 3
Cl1B Cl 0.000000 0.571(3) -0.445(4) 0.14(2) Uani 0.21(2) 2 d DS TU P C 3
Cl2B Cl 0.000000 0.725(2) -0.499(3) 0.107(17) Uani 0.21(2) 2 d DS TU P C 3


_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
C1 C2 1.479(16) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.404(16) . ?
C2 C6 1.408(16) . ?
C2 Ta2 2.463(17) . ?
C3 C4 1.405(15) . ?
C3 C7 1.511(17) . ?
C3 Ta2 2.457(17) . ?
C4 C5 1.398(16) . ?
C4 C8 1.484(16) . ?
C4 Ta2 2.447(14) . ?
C5 C6 1.417(15) . ?
C5 C9 1.480(16) . ?
C5 Ta2 2.435(15) . ?
C6 C10 1.501(17) . ?
C6 Ta2 2.412(15) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.508(17) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 H11A 0.9600 4 ?
C11 H11B 0.9600 4 ?
C11 H11C 0.9599 4 ?
C12 C13 1.407(13) 4 ?
C12 C13 1.407(13) . ?
C12 Ta1 2.487(17) . ?
C13 C14 1.412(14) . ?
C13 C15 1.518(15) . ?
C13 Ta1 2.465(12) . ?
C14 C14 1.42(3) 4 ?
C14 C16 1.480(15) . ?
C14 Ta1 2.441(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
Se1 Ta1 2.4790(14) . ?
Se1 Ta2 2.5488(17) . ?
Se2 Se3 2.248(3) . ?
Se2 Ta1 2.6201(15) . ?
Se2 Ta2 2.7095(13) . ?
Se3 Se3 1.938(7) 4 ?
Se4 Ta2 2.5045(16) . ?
Se4 Ta2 2.5045(16) 4 ?
Se5 Ta2 2.5303(16) . ?
Se5 Ta2 2.5303(16) 4 ?
Ta1 Ta2 3.3499(9) . ?
Ta1 Ta2 3.3499(9) 4 ?
Ta2 Ta2 3.0850(11) 4 ?
C17 Cl2 1.74(4) . ?
C17 Cl1 1.78(2) 4 ?
C17 Cl1 1.78(2) . ?
C17A Cl2A 1.72(4) . ?
C17A Cl1A 1.73(4) . ?
C17B Cl1B 1.71(4) . ?
C17B Cl2B 1.72(4) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C6 107.3(13) . . ?
C3 C2 C1 127.3(19) . . ?
C6 C2 C1 125.2(19) . . ?
C3 C2 Ta2 73.2(10) . . ?
C6 C2 Ta2 71.2(9) . . ?
C1 C2 Ta2 124.6(13) . . ?
C2 C3 C4 107.5(13) . . ?
C2 C3 C7 131.7(19) . . ?
C4 C3 C7 120(2) . . ?
C2 C3 Ta2 73.7(10) . . ?
C4 C3 Ta2 72.9(9) . . ?
C7 C3 Ta2 124.5(13) . . ?
C5 C4 C3 110.0(12) . . ?
C5 C4 C8 120.0(19) . . ?
C3 C4 C8 129(2) . . ?
C5 C4 Ta2 72.9(9) . . ?
C3 C4 Ta2 73.8(9) . . ?
C8 C4 Ta2 126.9(12) . . ?
C4 C5 C6 105.8(11) . . ?
C4 C5 C9 125.6(19) . . ?
C6 C5 C9 127.7(19) . . ?
C4 C5 Ta2 73.8(8) . . ?
C6 C5 Ta2 72.1(9) . . ?
C9 C5 Ta2 127.6(13) . . ?
C2 C6 C5 109.4(12) . . ?
C2 C6 C10 118.2(18) . . ?
C5 C6 C10 131.2(17) . . ?
C2 C6 Ta2 75.2(9) . . ?
C5 C6 Ta2 73.9(9) . . ?
C10 C6 Ta2 127.0(13) . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.47(4) . 4 ?
H11A C11 H11A 140.8 . 4 ?
H11B C11 H11A 52.3 . 4 ?
H11C C11 H11A 60.2 . 4 ?
C12 C11 H11B 109.5(9) . 4 ?
H11A C11 H11B 52.3 . 4 ?
H11B C11 H11B 60.2 . 4 ?
H11C C11 H11B 140.8 . 4 ?
H11A C11 H11B 109.5 4 4 ?
C12 C11 H11C 109.5(10) . 4 ?
H11A C11 H11C 60.2 . 4 ?
H11B C11 H11C 140.8 . 4 ?
H11C C11 H11C 52.3 . 4 ?
H11A C11 H11C 109.5 4 4 ?
H11B C11 H11C 109.5 4 4 ?
C13 C12 C13 107.0(14) 4 . ?
C13 C12 C11 126.4(7) 4 . ?
C13 C12 C11 126.4(7) . . ?
C13 C12 Ta1 72.7(8) 4 . ?
C13 C12 Ta1 72.7(8) . . ?
C11 C12 Ta1 123.0(13) . . ?
C12 C13 C14 109.2(11) . . ?
C12 C13 C15 126.0(12) . . ?
C14 C13 C15 124.7(12) . . ?
C12 C13 Ta1 74.3(8) . . ?
C14 C13 Ta1 72.3(7) . . ?
C15 C13 Ta1 123.1(9) . . ?
C13 C14 C14 107.3(7) . 4 ?
C13 C14 C16 124.7(13) . . ?
C14 C14 C16 126.6(9) 4 . ?
C13 C14 Ta1 74.2(7) . . ?
C14 C14 Ta1 73.0(3) 4 . ?
C16 C14 Ta1 129.1(9) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Ta1 Se1 Ta2 83.55(5) . . ?
Se3 Se2 Ta1 115.76(11) . . ?
Se3 Se2 Ta2 118.33(11) . . ?
Ta1 Se2 Ta2 77.86(4) . . ?
Se3 Se3 Se2 110.03(9) 4 . ?
Ta2 Se4 Ta2 76.03(6) . 4 ?
Ta2 Se5 Ta2 75.12(6) . 4 ?
C14 Ta1 C14 33.9(6) 4 . ?
C14 Ta1 C13 55.5(4) 4 . ?
C14 Ta1 C13 33.4(3) . . ?
C14 Ta1 C13 33.4(3) 4 4 ?
C14 Ta1 C13 55.5(4) . 4 ?
C13 Ta1 C13 54.6(6) . 4 ?
C14 Ta1 Se1 80.5(3) 4 . ?
C14 Ta1 Se1 106.7(3) . . ?
C13 Ta1 Se1 135.9(3) . . ?
C13 Ta1 Se1 90.4(3) 4 . ?
C14 Ta1 Se1 106.7(3) 4 4 ?
C14 Ta1 Se1 80.5(3) . 4 ?
C13 Ta1 Se1 90.4(3) . 4 ?
C13 Ta1 Se1 135.9(3) 4 4 ?
Se1 Ta1 Se1 101.58(8) . 4 ?
C14 Ta1 C12 55.6(5) 4 . ?
C14 Ta1 C12 55.6(5) . . ?
C13 Ta1 C12 33.0(3) . . ?
C13 Ta1 C12 33.0(3) 4 . ?
Se1 Ta1 C12 123.03(17) . . ?
Se1 Ta1 C12 123.03(17) 4 . ?
C14 Ta1 Se2 140.4(3) 4 4 ?
C14 Ta1 Se2 112.6(3) . 4 ?
C13 Ta1 Se2 85.1(3) . 4 ?
C13 Ta1 Se2 121.6(3) 4 4 ?
Se1 Ta1 Se2 138.93(6) . 4 ?
Se1 Ta1 Se2 74.07(5) 4 4 ?
C12 Ta1 Se2 90.0(3) . 4 ?
C14 Ta1 Se2 112.6(3) 4 . ?
C14 Ta1 Se2 140.4(3) . . ?
C13 Ta1 Se2 121.6(3) . . ?
C13 Ta1 Se2 85.1(3) 4 . ?
Se1 Ta1 Se2 74.07(5) . . ?
Se1 Ta1 Se2 138.93(6) 4 . ?
C12 Ta1 Se2 90.0(3) . . ?
Se2 Ta1 Se2 83.15(7) 4 . ?
C14 Ta1 Ta2 128.8(3) 4 . ?
C14 Ta1 Ta2 153.6(3) . . ?
C13 Ta1 Ta2 172.7(3) . . ?
C13 Ta1 Ta2 124.7(3) 4 . ?
Se1 Ta1 Ta2 49.12(4) . . ?
Se1 Ta1 Ta2 93.38(4) 4 . ?
C12 Ta1 Ta2 141.9(3) . . ?
Se2 Ta1 Ta2 89.94(4) 4 . ?
Se2 Ta1 Ta2 52.26(3) . . ?
C14 Ta1 Ta2 153.6(3) 4 4 ?
C14 Ta1 Ta2 128.8(3) . 4 ?
C13 Ta1 Ta2 124.7(3) . 4 ?
C13 Ta1 Ta2 172.7(3) 4 4 ?
Se1 Ta1 Ta2 93.39(4) . 4 ?
Se1 Ta1 Ta2 49.12(4) 4 4 ?
C12 Ta1 Ta2 141.9(3) . 4 ?
Se2 Ta1 Ta2 52.26(3) 4 4 ?
Se2 Ta1 Ta2 89.94(4) . 4 ?
Ta2 Ta1 Ta2 54.83(2) . 4 ?
C6 Ta2 C5 34.0(4) . . ?
C6 Ta2 C4 55.0(5) . . ?
C5 Ta2 C4 33.3(4) . . ?
C6 Ta2 C3 55.4(6) . . ?
C5 Ta2 C3 56.0(5) . . ?
C4 Ta2 C3 33.3(4) . . ?
C6 Ta2 C2 33.6(4) . . ?
C5 Ta2 C2 56.2(5) . . ?
C4 Ta2 C2 54.9(5) . . ?
C3 Ta2 C2 33.2(4) . . ?
C6 Ta2 Se4 97.2(4) . . ?
C5 Ta2 Se4 81.0(4) . . ?
C4 Ta2 Se4 102.3(4) . . ?
C3 Ta2 Se4 134.8(4) . . ?
C2 Ta2 Se4 130.8(4) . . ?
C6 Ta2 Se5 84.2(4) . . ?
C5 Ta2 Se5 113.8(4) . . ?
C4 Ta2 Se5 138.3(3) . . ?
C3 Ta2 Se5 117.9(5) . . ?
C2 Ta2 Se5 86.9(4) . . ?
Se4 Ta2 Se5 90.00(6) . . ?
C6 Ta2 Se1 135.5(4) . . ?
C5 Ta2 Se1 105.9(4) . . ?
C4 Ta2 Se1 80.5(3) . . ?
C3 Ta2 Se1 88.9(5) . . ?
C2 Ta2 Se1 121.6(4) . . ?
Se4 Ta2 Se1 90.42(7) . . ?
Se5 Ta2 Se1 139.83(5) . . ?
C6 Ta2 Se2 121.3(4) . . ?
C5 Ta2 Se2 138.1(4) . . ?
C4 Ta2 Se2 109.6(4) . . ?
C3 Ta2 Se2 82.2(4) . . ?
C2 Ta2 Se2 88.7(4) . . ?
Se4 Ta2 Se2 139.51(6) . . ?
Se5 Ta2 Se2 82.62(5) . . ?
Se1 Ta2 Se2 71.46(5) . . ?
C6 Ta2 Ta2 120.5(4) . 4 ?
C5 Ta2 Ta2 126.8(4) . 4 ?
C4 Ta2 Ta2 154.3(4) . 4 ?
C3 Ta2 Ta2 170.3(4) . 4 ?
C2 Ta2 Ta2 138.2(4) . 4 ?
Se4 Ta2 Ta2 51.98(3) . 4 ?
Se5 Ta2 Ta2 52.44(3) . 4 ?
Se1 Ta2 Ta2 98.54(4) . 4 ?
Se2 Ta2 Ta2 94.15(3) . 4 ?
C6 Ta2 Ta1 171.1(4) . . ?
C5 Ta2 Ta1 152.3(4) . . ?
C4 Ta2 Ta1 126.4(4) . . ?
C3 Ta2 Ta1 119.9(4) . . ?
C2 Ta2 Ta1 138.2(4) . . ?
Se4 Ta2 Ta1 91.07(5) . . ?
Se5 Ta2 Ta1 92.50(4) . . ?
Se1 Ta2 Ta1 47.34(3) . . ?
Se2 Ta2 Ta1 49.88(3) . . ?
Ta2 Ta2 Ta1 62.584(12) 4 . ?
Cl2 C17 Cl1 99.9(17) . 4 ?
Cl2 C17 Cl1 99.9(17) . . ?
Cl1 C17 Cl1 138(4) 4 . ?
Cl2A C17A Cl1A 109(3) . . ?
Cl1B C17B Cl2B 107(3) . . ?

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
C6 C2 C3 C4 -2(2) . . . . ?
C1 C2 C3 C4 173.3(18) . . . . ?
Ta2 C2 C3 C4 -65.6(12) . . . . ?
C6 C2 C3 C7 -175(2) . . . . ?
C1 C2 C3 C7 1(3) . . . . ?
Ta2 C2 C3 C7 122(2) . . . . ?
C6 C2 C3 Ta2 63.5(12) . . . . ?
C1 C2 C3 Ta2 -121(2) . . . . ?
C2 C3 C4 C5 1.7(19) . . . . ?
C7 C3 C4 C5 175.1(17) . . . . ?
Ta2 C3 C4 C5 -64.4(12) . . . . ?
C2 C3 C4 C8 -169.2(17) . . . . ?
C7 C3 C4 C8 4(3) . . . . ?
Ta2 C3 C4 C8 124.7(17) . . . . ?
C2 C3 C4 Ta2 66.1(13) . . . . ?
C7 C3 C4 Ta2 -120.5(18) . . . . ?
C3 C4 C5 C6 -0.5(19) . . . . ?
C8 C4 C5 C6 171.3(15) . . . . ?
Ta2 C4 C5 C6 -65.5(11) . . . . ?
C3 C4 C5 C9 -170.1(18) . . . . ?
C8 C4 C5 C9 2(3) . . . . ?
Ta2 C4 C5 C9 124.9(19) . . . . ?
C3 C4 C5 Ta2 64.9(12) . . . . ?
C8 C4 C5 Ta2 -123.2(15) . . . . ?
C3 C2 C6 C5 2(2) . . . . ?
C1 C2 C6 C5 -173.7(18) . . . . ?
Ta2 C2 C6 C5 66.7(12) . . . . ?
C3 C2 C6 C10 170.9(17) . . . . ?
C1 C2 C6 C10 -5(3) . . . . ?
Ta2 C2 C6 C10 -124.4(16) . . . . ?
C3 C2 C6 Ta2 -64.8(13) . . . . ?
C1 C2 C6 Ta2 119.6(19) . . . . ?
C4 C5 C6 C2 -0.8(19) . . . . ?
C9 C5 C6 C2 168.5(18) . . . . ?
Ta2 C5 C6 C2 -67.5(12) . . . . ?
C4 C5 C6 C10 -168(2) . . . . ?
C9 C5 C6 C10 1(3) . . . . ?
Ta2 C5 C6 C10 125(2) . . . . ?
C4 C5 C6 Ta2 66.7(11) . . . . ?
C9 C5 C6 Ta2 -124(2) . . . . ?
C13 C12 C13 C14 1(2) 4 . . . ?
C11 C12 C13 C14 177.0(17) . . . . ?
Ta1 C12 C13 C14 -64.4(9) . . . . ?
C13 C12 C13 C15 -175.1(9) 4 . . . ?
C11 C12 C13 C15 1(3) . . . . ?
Ta1 C12 C13 C15 119.8(13) . . . . ?
C13 C12 C13 Ta1 65.0(12) 4 . . . ?
C11 C12 C13 Ta1 -118.6(19) . . . . ?
C12 C13 C14 C14 -0.4(12) . . . 4 ?
C15 C13 C14 C14 175.4(10) . . . 4 ?
Ta1 C13 C14 C14 -66.1(3) . . . 4 ?
C12 C13 C14 C16 -167.3(14) . . . . ?
C15 C13 C14 C16 9(2) . . . . ?
Ta1 C13 C14 C16 127.0(13) . . . . ?
C12 C13 C14 Ta1 65.7(11) . . . . ?
C15 C13 C14 Ta1 -118.5(12) . . . . ?

_refine_diff_density_max         1.336
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.166

# start Validation Reply Form
_vrf_PLAT260_taseg1              
;
PROBLEM: Large Average Ueq of Residue Including       Cl2      0.157 Check 
RESPONSE:The solvent DCM seems to be disordered with apparent electron 
density diffused over a region. This has led to apparently large 
thermal parameters.
;
_vrf_PLAT342_taseg1              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02188 Ang.  
RESPONSE: This could be due to large thermal libration of Cp* moiety.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_BABU
_database_code_depnum_ccdc_archive 'CCDC 1886852'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar'
;IIT Madras
India
;
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-02-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 Nb3 S6'
_chemical_formula_weight         831.39

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'

_cell_length_a                   20.2903(12)
_cell_length_b                   20.2903(12)
_cell_length_c                   15.0268(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5357.6(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2197
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.809

_exptl_crystal_description       flake
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             2394
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.338
_shelx_estimated_absorpt_T_min   0.824
_shelx_estimated_absorpt_T_max   0.878
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6101
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.783
_diffrn_reflns_theta_max         26.809
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2545
_reflns_number_gt                1273
_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       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1828P)²+179.2492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0014(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2545
_refine_ls_number_parameters     210
_refine_ls_number_restraints     1106
_refine_ls_R_factor_all          0.2374
_refine_ls_R_factor_gt           0.1562
_refine_ls_wR_factor_ref         0.4604
_refine_ls_wR_factor_gt          0.4160
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.8323(19) 0.7726(12) 0.260(2) 0.099(8) Uani 0.49(3) 1 d D U P A 1
C2 C 0.880(2) 0.7725(11) 0.327(2) 0.098(8) Uani 0.49(3) 1 d D U P A 1
C3 C 0.9444(19) 0.7764(12) 0.286(2) 0.098(8) Uani 0.49(3) 1 d D U P A 1
C4 C 0.936(2) 0.7790(14) 0.194(2) 0.099(8) Uani 0.49(3) 1 d D U P A 1
C5 C 0.867(2) 0.7767(15) 0.177(2) 0.099(8) Uani 0.49(3) 1 d D U P A 1
C6 C 0.756(2) 0.769(2) 0.274(4) 0.105(11) Uani 0.49(3) 1 d D U P A 1
C7 C 0.865(3) 0.769(2) 0.427(2) 0.103(11) Uani 0.49(3) 1 d D U P A 1
C8 C 1.012(2) 0.778(2) 0.334(3) 0.100(11) Uani 0.49(3) 1 d D U P A 1
C9 C 0.993(2) 0.783(2) 0.123(3) 0.102(11) Uani 0.49(3) 1 d D U P A 1
C10 C 0.835(3) 0.778(2) 0.086(2) 0.101(11) Uani 0.49(3) 1 d D U P A 1
S1 S 0.8999(8) 0.9456(7) 0.1302(11) 0.044(4) Uiso 0.60(3) 1 d . . P B 1
S2 S 0.9031(8) 0.9476(7) 0.3706(10) 0.041(4) Uiso 0.60(3) 1 d . . P B 1
C1' C 0.8505(19) 0.7703(11) 0.312(2) 0.100(8) Uani 0.51(3) 1 d D U P A 2
C2' C 0.9194(19) 0.7698(10) 0.310(2) 0.099(8) Uani 0.51(3) 1 d D U P A 2
C3' C 0.9391(18) 0.7702(12) 0.220(2) 0.099(8) Uani 0.51(3) 1 d D U P A 2
C4' C 0.883(2) 0.7710(14) 0.1673(19) 0.099(8) Uani 0.51(3) 1 d D U P A 2
C5' C 0.8276(18) 0.7711(14) 0.224(2) 0.099(8) Uani 0.51(3) 1 d D U P A 2
C6' C 0.808(3) 0.7701(19) 0.396(2) 0.102(11) Uani 0.51(3) 1 d D U P A 2
C7' C 0.965(2) 0.7690(18) 0.390(3) 0.094(10) Uani 0.51(3) 1 d D U P A 2
C8' C 1.010(2) 0.770(2) 0.186(3) 0.099(10) Uani 0.51(3) 1 d D U P A 2
C9' C 0.880(3) 0.771(2) 0.065(2) 0.108(11) Uani 0.51(3) 1 d D U P A 2
C10' C 0.756(2) 0.772(2) 0.195(3) 0.103(11) Uani 0.51(3) 1 d D U P A 2
S1' S 0.8833(11) 0.9398(10) 0.1604(16) 0.039(5) Uiso 0.40(3) 1 d . . P A 2
S2' S 0.8788(10) 0.9374(9) 0.3367(13) 0.032(5) Uiso 0.40(3) 1 d . . P A 2
Nb1 Nb 0.94991(14) 0.89671(10) 0.25008(16) 0.0380(9) 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
C1 C5 1.407(15) . ?
C1 C2 1.406(15) . ?
C1 C6 1.530(16) . ?
C1 Nb1 2.46(2) . ?
C2 C3 1.404(16) . ?
C2 C7 1.531(16) . ?
C2 Nb1 2.48(2) . ?
C3 C4 1.405(15) . ?
C3 C8 1.532(16) . ?
C3 Nb1 2.45(3) . ?
C4 C5 1.404(15) . ?
C4 C9 1.533(16) . ?
C4 Nb1 2.42(3) . ?
C5 C10 1.529(15) . ?
C5 Nb1 2.42(3) . ?
S1 Nb1 2.504(13) . ?
S1 Nb1 2.574(14) 3_675 ?
S2 Nb1 2.495(12) . ?
S2 Nb1 2.559(12) 3_675 ?
C1' C2' 1.405(15) . ?
C1' C5' 1.407(15) . ?
C1' C6' 1.527(16) . ?
C1' Nb1 2.52(2) . ?
C2' C3' 1.404(16) . ?
C2' C7' 1.528(16) . ?
C2' Nb1 2.49(2) . ?
C3' C4' 1.402(15) . ?
C3' C8' 1.530(16) . ?
C3' Nb1 2.51(3) . ?
C4' C5' 1.405(15) . ?
C4' C9' 1.532(16) . ?
C4' Nb1 2.54(3) . ?
C5' C10' 1.529(15) . ?
C5' Nb1 2.55(3) . ?
S1' Nb1 2.367(18) 3_675 ?
S1' Nb1 2.364(18) . ?
S2' Nb1 2.382(15) 3_675 ?
S2' Nb1 2.376(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C1 C2 107.9(8) . . ?
C5 C1 C6 126.2(9) . . ?
C2 C1 C6 125.9(9) . . ?
C5 C1 Nb1 71.8(10) . . ?
C2 C1 Nb1 74.1(10) . . ?
C6 C1 Nb1 119.9(10) . . ?
C1 C2 C3 108.0(8) . . ?
C1 C2 C7 125.8(9) . . ?
C3 C2 C7 126.2(9) . . ?
C1 C2 Nb1 72.8(10) . . ?
C3 C2 Nb1 72.4(10) . . ?
C7 C2 Nb1 120.6(9) . . ?
C4 C3 C2 108.1(8) . . ?
C4 C3 C8 126.0(9) . . ?
C2 C3 C8 125.9(9) . . ?
C4 C3 Nb1 71.9(10) . . ?
C2 C3 Nb1 74.5(10) . . ?
C8 C3 Nb1 119.5(10) . . ?
C5 C4 C3 108.0(8) . . ?
C5 C4 C9 126.1(9) . . ?
C3 C4 C9 125.9(9) . . ?
C5 C4 Nb1 73.3(11) . . ?
C3 C4 Nb1 74.5(10) . . ?
C9 C4 Nb1 118.1(9) . . ?
C4 C5 C1 108.0(8) . . ?
C4 C5 C10 126.0(8) . . ?
C1 C5 C10 125.9(8) . . ?
C4 C5 Nb1 72.9(11) . . ?
C1 C5 Nb1 74.7(9) . . ?
C10 C5 Nb1 118.4(9) . . ?
Nb1 S1 Nb1 76.5(4) . 3_675 ?
Nb1 S2 Nb1 76.9(4) . 3_675 ?
C2' C1' C5' 107.9(8) . . ?
C2' C1' C6' 126.2(9) . . ?
C5' C1' C6' 125.9(9) . . ?
C2' C1' Nb1 72.7(10) . . ?
C5' C1' Nb1 74.9(9) . . ?
C6' C1' Nb1 118.3(8) . . ?
C1' C2' C3' 108.0(8) . . ?
C1' C2' C7' 126.0(9) . . ?
C3' C2' C7' 126.0(9) . . ?
C1' C2' Nb1 74.7(9) . . ?
C3' C2' Nb1 74.1(9) . . ?
C7' C2' Nb1 117.2(9) . . ?
C4' C3' C2' 108.1(8) . . ?
C4' C3' C8' 125.8(9) . . ?
C2' C3' C8' 126.0(9) . . ?
C4' C3' Nb1 75.1(10) . . ?
C2' C3' Nb1 73.3(8) . . ?
C8' C3' Nb1 117.6(9) . . ?
C5' C4' C3' 108.0(8) . . ?
C5' C4' C9' 125.7(9) . . ?
C3' C4' C9' 126.3(9) . . ?
C5' C4' Nb1 74.3(9) . . ?
C3' C4' Nb1 72.6(9) . . ?
C9' C4' Nb1 119.1(8) . . ?
C4' C5' C1' 107.9(8) . . ?
C4' C5' C10' 126.0(8) . . ?
C1' C5' C10' 126.1(8) . . ?
C4' C5' Nb1 73.6(9) . . ?
C1' C5' Nb1 72.9(8) . . ?
C10' C5' Nb1 119.4(9) . . ?
Nb1 S1' Nb1 83.3(6) 3_675 . ?
Nb1 S2' Nb1 82.7(5) 3_675 . ?
S2' Nb1 S1' 142.0(5) 2_765 . ?
S1' Nb1 S1' 97.3(12) 2_765 . ?
S2' Nb1 S2' 101.6(11) 2_765 . ?
S1' Nb1 S2' 142.1(5) 2_765 . ?
S1' Nb1 S2' 68.0(8) . . ?
C3 Nb1 C2 33.1(4) . . ?
C3 Nb1 C4 33.6(5) . . ?
C2 Nb1 C4 55.4(5) . . ?
C3 Nb1 C1 55.2(5) . . ?
C2 Nb1 C1 33.1(4) . . ?
C4 Nb1 C1 55.6(6) . . ?
S2' Nb1 C4' 125.7(10) 2_765 . ?
S1' Nb1 C4' 92.9(9) 2_765 . ?
S1' Nb1 C4' 88.4(9) . . ?
S2' Nb1 C4' 120.2(10) . . ?
S2' Nb1 C3' 93.7(9) 2_765 . ?
S1' Nb1 C3' 83.7(8) 2_765 . ?
S1' Nb1 C3' 120.2(9) . . ?
S2' Nb1 C3' 134.2(8) . . ?
C4' Nb1 C3' 32.3(4) . . ?
C3 Nb1 C5 55.6(6) . . ?
C2 Nb1 C5 55.3(5) . . ?
C4 Nb1 C5 33.7(5) . . ?
C1 Nb1 C5 33.5(5) . . ?
S2' Nb1 C5' 137.3(8) 2_765 . ?
S1' Nb1 C5' 124.6(9) 2_765 . ?
S1' Nb1 C5' 80.3(8) . . ?
S2' Nb1 C5' 88.6(9) . . ?
C4' Nb1 C5' 32.1(4) . . ?
C3' Nb1 C5' 53.4(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 0.0(2) . . . . ?
C6 C1 C2 C3 180.0(3) . . . . ?
Nb1 C1 C2 C3 -64.3(10) . . . . ?
C5 C1 C2 C7 -180.0(3) . . . . ?
C6 C1 C2 C7 0.1(4) . . . . ?
Nb1 C1 C2 C7 115.7(10) . . . . ?
C5 C1 C2 Nb1 64.3(10) . . . . ?
C6 C1 C2 Nb1 -115.7(10) . . . . ?
C1 C2 C3 C4 0.0(2) . . . . ?
C7 C2 C3 C4 179.9(4) . . . . ?
Nb1 C2 C3 C4 -64.6(10) . . . . ?
C1 C2 C3 C8 180.0(3) . . . . ?
C7 C2 C3 C8 -0.1(4) . . . . ?
Nb1 C2 C3 C8 115.4(10) . . . . ?
C1 C2 C3 Nb1 64.6(10) . . . . ?
C7 C2 C3 Nb1 -115.5(10) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C8 C3 C4 C5 -180.0(4) . . . . ?
Nb1 C3 C4 C5 -66.2(10) . . . . ?
C2 C3 C4 C9 -179.9(4) . . . . ?
C8 C3 C4 C9 0.1(7) . . . . ?
Nb1 C3 C4 C9 113.8(11) . . . . ?
C2 C3 C4 Nb1 66.3(10) . . . . ?
C8 C3 C4 Nb1 -113.7(10) . . . . ?
C3 C4 C5 C1 0.0(5) . . . . ?
C9 C4 C5 C1 179.9(5) . . . . ?
Nb1 C4 C5 C1 -67.0(9) . . . . ?
C3 C4 C5 C10 -179.9(5) . . . . ?
C9 C4 C5 C10 0.1(9) . . . . ?
Nb1 C4 C5 C10 113.1(10) . . . . ?
C3 C4 C5 Nb1 67.0(9) . . . . ?
C9 C4 C5 Nb1 -113.0(10) . . . . ?
C2 C1 C5 C4 0.0(5) . . . . ?
C6 C1 C5 C4 -180.0(4) . . . . ?
Nb1 C1 C5 C4 65.8(11) . . . . ?
C2 C1 C5 C10 179.9(4) . . . . ?
C6 C1 C5 C10 -0.1(7) . . . . ?
Nb1 C1 C5 C10 -114.3(11) . . . . ?
C2 C1 C5 Nb1 -65.8(10) . . . . ?
C6 C1 C5 Nb1 114.2(10) . . . . ?
C5' C1' C2' C3' -0.1(2) . . . . ?
C6' C1' C2' C3' 179.9(3) . . . . ?
Nb1 C1' C2' C3' -67.3(9) . . . . ?
C5' C1' C2' C7' 180.0(4) . . . . ?
C6' C1' C2' C7' 0.0(4) . . . . ?
Nb1 C1' C2' C7' 112.8(9) . . . . ?
C5' C1' C2' Nb1 67.2(9) . . . . ?
C6' C1' C2' Nb1 -112.8(9) . . . . ?
C1' C2' C3' C4' 0.0(2) . . . . ?
C7' C2' C3' C4' -180.0(4) . . . . ?
Nb1 C2' C3' C4' -67.6(10) . . . . ?
C1' C2' C3' C8' 180.0(3) . . . . ?
C7' C2' C3' C8' 0.0(4) . . . . ?
Nb1 C2' C3' C8' 112.3(10) . . . . ?
C1' C2' C3' Nb1 67.7(9) . . . . ?
C7' C2' C3' Nb1 -112.4(10) . . . . ?
C2' C3' C4' C5' 0.0(5) . . . . ?
C8' C3' C4' C5' -180.0(4) . . . . ?
Nb1 C3' C4' C5' -66.4(9) . . . . ?
C2' C3' C4' C9' -179.8(4) . . . . ?
C8' C3' C4' C9' 0.2(7) . . . . ?
Nb1 C3' C4' C9' 113.8(10) . . . . ?
C2' C3' C4' Nb1 66.4(8) . . . . ?
C8' C3' C4' Nb1 -113.6(8) . . . . ?
C3' C4' C5' C1' 0.0(5) . . . . ?
C9' C4' C5' C1' 179.8(5) . . . . ?
Nb1 C4' C5' C1' -65.3(9) . . . . ?
C3' C4' C5' C10' -179.9(5) . . . . ?
C9' C4' C5' C10' -0.1(9) . . . . ?
Nb1 C4' C5' C10' 114.8(10) . . . . ?
C3' C4' C5' Nb1 65.3(9) . . . . ?
C9' C4' C5' Nb1 -114.9(10) . . . . ?
C2' C1' C5' C4' 0.0(5) . . . . ?
C6' C1' C5' C4' -180.0(4) . . . . ?
Nb1 C1' C5' C4' 65.8(10) . . . . ?
C2' C1' C5' C10' 179.9(4) . . . . ?
C6' C1' C5' C10' -0.1(7) . . . . ?
Nb1 C1' C5' C10' -114.3(10) . . . . ?
C2' C1' C5' Nb1 -65.8(9) . . . . ?
C6' C1' C5' Nb1 114.2(9) . . . . ?

_refine_diff_density_max         4.538
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.400

####################################################################### 
# 
# 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_NBSH
_database_code_depnum_ccdc_archive 'CCDC 1882536'
loop_
_audit_author_name
_audit_author_address
'Babu Varghese'
;SAIF, IIT Madras
India
;
_audit_update_record             
;
2019-02-05 deposited with the CCDC.	2019-02-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C30 H45 B Nb3 S7) + 0.5(CH2Cl2)'
_chemical_formula_sum            'C30.50 H46 B Cl Nb3 S7'
_chemical_formula_weight         962.08

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -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'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   15.7274(5)
_cell_length_b                   16.7472(5)
_cell_length_c                   15.8653(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4178.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6788
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      24.8

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             1944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.242
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker Apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17535
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.776
_diffrn_reflns_theta_max         26.771
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             4459
_reflns_number_gt                4151
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_max     0.928
_reflns_Friedel_fraction_full    0.956

_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       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'


_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)+(0.0516P)²] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4459
_refine_ls_number_parameters     254
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.074
_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
S5 S 0.0697(2) 0.4844(2) 0.3092(2) 0.0374(7) Uani 0.5 1 d . . P . .
B1 B -0.0295(8) 0.4261(9) 0.3335(8) 0.029(3) Uani 0.5 1 d . . P . .
C1 C 0.2159(4) 0.2782(5) 0.3653(5) 0.0423(17) Uani 1 1 d . . . . .
C2 C 0.1771(4) 0.2054(5) 0.3870(4) 0.0420(17) Uani 1 1 d . . . . .
C3 C 0.1931(5) 0.1505(5) 0.3199(6) 0.051(2) Uani 1 1 d . . . . .
C4 C 0.2393(4) 0.1909(5) 0.2579(5) 0.0479(19) Uani 1 1 d . . . . .
C5 C 0.2538(4) 0.2687(5) 0.2850(4) 0.0453(19) Uani 1 1 d . . . . .
C6 C 0.3090(5) 0.3296(7) 0.2428(7) 0.086(3) Uani 1 1 d . . . . .
H6A H 0.303322 0.379940 0.271296 0.130 Uiso 1 1 calc R U . . .
H6B H 0.291909 0.335491 0.185074 0.130 Uiso 1 1 calc R U . . .
H6C H 0.367253 0.312557 0.245066 0.130 Uiso 1 1 calc R U . . .
C7 C 0.2232(6) 0.3508(6) 0.4215(7) 0.076(3) Uani 1 1 d . . . . .
H7A H 0.174756 0.353359 0.458231 0.114 Uiso 1 1 calc R U . . .
H7B H 0.225196 0.398109 0.387293 0.114 Uiso 1 1 calc R U . . .
H7C H 0.274148 0.347193 0.454525 0.114 Uiso 1 1 calc R U . . .
C8 C 0.1365(6) 0.1895(8) 0.4704(6) 0.081(3) Uani 1 1 d . . . . .
H8A H 0.179282 0.173593 0.510173 0.121 Uiso 1 1 calc R U . . .
H8B H 0.095337 0.147528 0.464545 0.121 Uiso 1 1 calc R U . . .
H8C H 0.108892 0.237067 0.490038 0.121 Uiso 1 1 calc R U . . .
C9 C 0.1746(7) 0.0625(5) 0.3230(8) 0.093(4) Uani 1 1 d . . . . .
H9A H 0.181853 0.039926 0.267820 0.139 Uiso 1 1 calc R U . . .
H9B H 0.117198 0.054159 0.341508 0.139 Uiso 1 1 calc R U . . .
H9C H 0.213083 0.037085 0.361609 0.139 Uiso 1 1 calc R U . . .
C10 C 0.2778(7) 0.1494(8) 0.1834(6) 0.094(4) Uani 1 1 d . . . . .
H10A H 0.287607 0.187411 0.139144 0.141 Uiso 1 1 calc R U . . .
H10B H 0.239560 0.108751 0.163653 0.141 Uiso 1 1 calc R U . . .
H10C H 0.330720 0.125382 0.199559 0.141 Uiso 1 1 calc R U . . .
C11 C 0.0455(4) 0.3700(4) -0.0257(4) 0.0314(14) Uani 1 1 d . . . . .
C12 C 0.0725(4) 0.4367(4) 0.0215(4) 0.0300(14) Uani 1 1 d . . . . .
C13 C 0.000000 0.4798(5) 0.0493(5) 0.0296(19) Uani 1 2 d S T P . .
C14 C 0.000000 0.5574(6) 0.0954(7) 0.051(3) Uani 1 2 d S T P . .
H14A H -0.037181 0.594306 0.067354 0.076 Uiso 0.5 1 calc R U P . .
H14B H 0.056631 0.578794 0.096461 0.076 Uiso 0.5 1 calc R U P . .
H14C H -0.019450 0.549143 0.152101 0.076 Uiso 0.5 1 calc R U P . .
C15 C 0.1639(4) 0.4630(5) 0.0315(5) 0.050(2) Uani 1 1 d . . . . .
H15A H 0.200175 0.416951 0.033001 0.075 Uiso 1 1 calc R U . . .
H15B H 0.169939 0.492496 0.083062 0.075 Uiso 1 1 calc R U . . .
H15C H 0.179652 0.496365 -0.015194 0.075 Uiso 1 1 calc R U . . .
C16 C 0.0992(5) 0.3174(5) -0.0779(5) 0.052(2) Uani 1 1 d . . . . .
H16A H 0.114422 0.344568 -0.128988 0.079 Uiso 1 1 calc R U . . .
H16B H 0.068381 0.269593 -0.091344 0.079 Uiso 1 1 calc R U . . .
H16C H 0.149844 0.303764 -0.047284 0.079 Uiso 1 1 calc R U . . .
Nb1 Nb 0.09979(3) 0.25663(3) 0.26498(4) 0.02474(14) Uani 1 1 d . . . . .
Nb2 Nb 0.000000 0.34860(4) 0.12063(4) 0.02067(17) Uani 1 2 d S T P . .
S1 S 0.11492(10) 0.25594(9) 0.11547(11) 0.0333(4) Uani 1 1 d . . . . .
S2 S 0.10408(11) 0.40466(11) 0.22720(11) 0.0396(4) Uani 1 1 d . . . . .
S3 S 0.000000 0.31967(15) 0.37122(13) 0.0294(5) Uani 1 2 d S T P . .
S4 S 0.000000 0.15060(13) 0.27279(17) 0.0347(5) Uani 1 2 d S T P . .
Cl1 Cl 0.000000 -0.0799(11) 0.4504(10) 0.120(6) Uani 0.364(6) 2 d DS TU P A 1
Cl2 Cl -0.0821(12) -0.0058(10) 0.5855(10) 0.110(6) Uani 0.182(3) 1 d D U P A 1
C17 C 0.000000 -0.0711(19) 0.5609(17) 0.078(8) Uani 0.364(6) 2 d DS TU P A 1
Cl1' Cl 0.000000 0.0281(16) 0.609(2) 0.103(9) Uani 0.136(6) 2 d DS TU P B 2
Cl2' Cl -0.043(3) -0.063(2) 0.468(2) 0.077(8) Uani 0.068(3) 1 d D U P B 2
C17' C 0.000000 -0.068(3) 0.569(3) 0.083(10) Uani 0.136(6) 2 d DS TU P B 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
S5 B1 1.880(14) . ?
S5 S2 1.941(4) . ?
B1 S3 1.937(15) . ?
B1 S2 2.086(13) 4 ?
C1 C2 1.406(11) . ?
C1 C5 1.416(10) . ?
C1 C7 1.513(11) . ?
C1 Nb1 2.449(6) . ?
C2 C3 1.428(11) . ?
C2 C8 1.492(11) . ?
C2 Nb1 2.441(6) . ?
C3 C4 1.399(12) . ?
C3 C9 1.504(11) . ?
C3 Nb1 2.464(7) . ?
C4 C5 1.391(11) . ?
C4 C10 1.499(11) . ?
C4 Nb1 2.457(6) . ?
C5 C6 1.498(12) . ?
C5 Nb1 2.452(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.410(9) . ?
C11 C11 1.430(12) 4 ?
C11 C16 1.475(9) . ?
C11 Nb2 2.456(6) . ?
C12 C13 1.419(9) . ?
C12 C15 1.512(8) . ?
C12 Nb2 2.440(6) . ?
C13 C14 1.492(14) . ?
C13 Nb2 2.471(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 H14A 0.96(9) 4 ?
C14 H14B 0.96(3) 4 ?
C14 H14C 0.96(6) 4 ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
Nb1 S4 2.3732(16) . ?
Nb1 S1 2.3840(18) . ?
Nb1 S3 2.5336(18) . ?
Nb1 S2 2.5514(18) . ?
Nb1 Nb1 3.1390(9) 4 ?
Nb1 Nb2 3.1750(9) . ?
Nb2 S1 2.3837(15) . ?
Nb2 S1 2.3837(15) 4 ?
Nb2 S2 2.5337(17) 4 ?
Nb2 S2 2.5337(17) . ?
Cl1 C17 1.76(2) . ?
Cl2 C17 1.74(2) . ?
Cl1' C17' 1.73(3) . ?
Cl2' Cl2' 1.35(9) 4 ?
Cl2' C17' 1.74(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
B1 S5 S2 90.7(4) . . ?
S5 B1 S3 110.0(7) . . ?
S5 B1 S2 113.0(6) . 4 ?
S3 B1 S2 103.0(6) . 4 ?
C2 C1 C5 107.8(7) . . ?
C2 C1 C7 125.9(8) . . ?
C5 C1 C7 126.0(8) . . ?
C2 C1 Nb1 73.0(4) . . ?
C5 C1 Nb1 73.3(4) . . ?
C7 C1 Nb1 123.9(5) . . ?
C1 C2 C3 107.4(7) . . ?
C1 C2 C8 123.8(8) . . ?
C3 C2 C8 128.4(8) . . ?
C1 C2 Nb1 73.6(4) . . ?
C3 C2 Nb1 73.9(4) . . ?
C8 C2 Nb1 123.6(5) . . ?
C4 C3 C2 107.8(7) . . ?
C4 C3 C9 126.7(9) . . ?
C2 C3 C9 124.9(9) . . ?
C4 C3 Nb1 73.2(4) . . ?
C2 C3 Nb1 72.2(4) . . ?
C9 C3 Nb1 127.2(5) . . ?
C5 C4 C3 108.7(6) . . ?
C5 C4 C10 127.8(9) . . ?
C3 C4 C10 122.7(9) . . ?
C5 C4 Nb1 73.3(4) . . ?
C3 C4 Nb1 73.7(4) . . ?
C10 C4 Nb1 127.2(5) . . ?
C4 C5 C1 108.3(7) . . ?
C4 C5 C6 126.5(8) . . ?
C1 C5 C6 124.8(8) . . ?
C4 C5 Nb1 73.8(4) . . ?
C1 C5 Nb1 73.1(4) . . ?
C6 C5 Nb1 124.8(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C11 107.5(4) . 4 ?
C12 C11 C16 126.8(6) . . ?
C11 C11 C16 125.0(4) 4 . ?
C12 C11 Nb2 72.6(3) . . ?
C11 C11 Nb2 73.07(14) 4 . ?
C16 C11 Nb2 127.6(5) . . ?
C11 C12 C13 109.0(5) . . ?
C11 C12 C15 125.0(6) . . ?
C13 C12 C15 125.7(7) . . ?
C11 C12 Nb2 73.9(3) . . ?
C13 C12 Nb2 74.4(4) . . ?
C15 C12 Nb2 123.5(4) . . ?
C12 C13 C12 106.9(8) 4 . ?
C12 C13 C14 126.5(4) 4 . ?
C12 C13 C14 126.5(4) . . ?
C12 C13 Nb2 72.0(4) 4 . ?
C12 C13 Nb2 72.0(4) . . ?
C14 C13 Nb2 123.4(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5(19) . 4 ?
H14A C14 H14A 75.1 . 4 ?
H14B C14 H14A 37.2 . 4 ?
H14C C14 H14A 136.2 . 4 ?
C13 C14 H14B 109.5(7) . 4 ?
H14A C14 H14B 37.2 . 4 ?
H14B C14 H14B 136.2 . 4 ?
H14C C14 H14B 75.1 . 4 ?
H14A C14 H14B 109.5 4 4 ?
C13 C14 H14C 109.5(13) . 4 ?
H14A C14 H14C 136.2 . 4 ?
H14B C14 H14C 75.1 . 4 ?
H14C C14 H14C 37.2 . 4 ?
H14A C14 H14C 109.5 4 4 ?
H14B C14 H14C 109.5 4 4 ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S4 Nb1 S1 96.56(8) . . ?
S4 Nb1 C2 91.41(19) . . ?
S1 Nb1 C2 137.52(17) . . ?
S4 Nb1 C1 124.7(2) . . ?
S1 Nb1 C1 124.96(19) . . ?
C2 Nb1 C1 33.4(3) . . ?
S4 Nb1 C5 135.1(2) . . ?
S1 Nb1 C5 91.76(17) . . ?
C2 Nb1 C5 55.6(2) . . ?
C1 Nb1 C5 33.6(2) . . ?
S4 Nb1 C4 104.9(2) . . ?
S1 Nb1 C4 82.12(17) . . ?
C2 Nb1 C4 55.6(2) . . ?
C1 Nb1 C4 55.2(2) . . ?
C5 Nb1 C4 32.9(3) . . ?
S4 Nb1 C3 80.54(19) . . ?
S1 Nb1 C3 106.8(2) . . ?
C2 Nb1 C3 33.8(3) . . ?
C1 Nb1 C3 55.4(3) . . ?
C5 Nb1 C3 54.9(3) . . ?
C4 Nb1 C3 33.0(3) . . ?
S4 Nb1 S3 82.38(7) . . ?
S1 Nb1 S3 136.54(6) . . ?
C2 Nb1 S3 85.83(17) . . ?
C1 Nb1 S3 88.18(19) . . ?
C5 Nb1 S3 119.44(19) . . ?
C4 Nb1 S3 140.39(17) . . ?
C3 Nb1 S3 115.7(2) . . ?
S4 Nb1 S2 139.18(6) . . ?
S1 Nb1 S2 76.61(6) . . ?
C2 Nb1 S2 121.0(2) . . ?
C1 Nb1 S2 89.43(19) . . ?
C5 Nb1 S2 85.6(2) . . ?
C4 Nb1 S2 113.6(2) . . ?
C3 Nb1 S2 140.20(19) . . ?
S3 Nb1 S2 76.57(7) . . ?
S4 Nb1 Nb1 48.60(4) . 4 ?
S1 Nb1 Nb1 95.73(4) . 4 ?
C2 Nb1 Nb1 119.85(17) . 4 ?
C1 Nb1 Nb1 138.22(18) . 4 ?
C5 Nb1 Nb1 171.16(19) . 4 ?
C4 Nb1 Nb1 153.2(2) . 4 ?
C3 Nb1 Nb1 126.5(2) . 4 ?
S3 Nb1 Nb1 51.72(3) . 4 ?
S2 Nb1 Nb1 91.52(4) . 4 ?
S4 Nb1 Nb2 94.23(5) . . ?
S1 Nb1 Nb2 48.24(4) . . ?
C2 Nb1 Nb2 171.31(19) . . ?
C1 Nb1 Nb2 140.00(19) . . ?
C5 Nb1 Nb2 122.81(17) . . ?
C4 Nb1 Nb2 128.72(18) . . ?
C3 Nb1 Nb2 154.1(2) . . ?
S3 Nb1 Nb2 88.37(4) . . ?
S2 Nb1 Nb2 51.12(4) . . ?
Nb1 Nb1 Nb2 60.373(11) 4 . ?
S1 Nb2 S1 98.62(9) . 4 ?
S1 Nb2 C12 91.00(16) . . ?
S1 Nb2 C12 136.54(15) 4 . ?
S1 Nb2 C12 136.54(15) . 4 ?
S1 Nb2 C12 91.00(16) 4 4 ?
C12 Nb2 C12 55.7(3) . 4 ?
S1 Nb2 C11 80.89(15) . . ?
S1 Nb2 C11 106.46(16) 4 . ?
C12 Nb2 C11 33.5(2) . . ?
C12 Nb2 C11 55.81(19) 4 . ?
S1 Nb2 C11 106.46(16) . 4 ?
S1 Nb2 C11 80.89(15) 4 4 ?
C12 Nb2 C11 55.81(19) . 4 ?
C12 Nb2 C11 33.5(2) 4 4 ?
C11 Nb2 C11 33.9(3) . 4 ?
S1 Nb2 C13 124.27(9) . . ?
S1 Nb2 C13 124.26(9) 4 . ?
C12 Nb2 C13 33.59(19) . . ?
C12 Nb2 C13 33.58(19) 4 . ?
C11 Nb2 C13 55.8(2) . . ?
C11 Nb2 C13 55.8(2) 4 . ?
S1 Nb2 S2 138.94(6) . 4 ?
S1 Nb2 S2 76.96(6) 4 4 ?
C12 Nb2 S2 120.53(17) . 4 ?
C12 Nb2 S2 84.51(14) 4 4 ?
C11 Nb2 S2 139.90(15) . 4 ?
C11 Nb2 S2 112.87(15) 4 4 ?
C13 Nb2 S2 88.64(16) . 4 ?
S1 Nb2 S2 76.96(6) . . ?
S1 Nb2 S2 138.95(6) 4 . ?
C12 Nb2 S2 84.51(14) . . ?
C12 Nb2 S2 120.53(17) 4 . ?
C11 Nb2 S2 112.87(15) . . ?
C11 Nb2 S2 139.90(15) 4 . ?
C13 Nb2 S2 88.64(16) . . ?
S2 Nb2 S2 80.49(9) 4 . ?
S1 Nb2 Nb1 94.81(5) . 4 ?
S1 Nb2 Nb1 48.25(4) 4 4 ?
C12 Nb2 Nb1 171.71(16) . 4 ?
C12 Nb2 Nb1 121.85(14) 4 4 ?
C11 Nb2 Nb1 153.73(16) . 4 ?
C11 Nb2 Nb1 127.50(14) 4 4 ?
C13 Nb2 Nb1 139.61(13) . 4 ?
S2 Nb2 Nb1 51.62(4) 4 4 ?
S2 Nb2 Nb1 91.02(5) . 4 ?
S1 Nb2 Nb1 48.25(4) . . ?
S1 Nb2 Nb1 94.81(5) 4 . ?
C12 Nb2 Nb1 121.85(14) . . ?
C12 Nb2 Nb1 171.70(16) 4 . ?
C11 Nb2 Nb1 127.50(14) . . ?
C11 Nb2 Nb1 153.73(16) 4 . ?
C13 Nb2 Nb1 139.61(13) . . ?
S2 Nb2 Nb1 91.02(5) 4 . ?
S2 Nb2 Nb1 51.61(4) . . ?
Nb1 Nb2 Nb1 59.25(2) 4 . ?
Nb2 S1 Nb1 83.51(5) . . ?
S5 S2 B1 35.2(4) . 4 ?
S5 S2 Nb2 121.48(13) . . ?
B1 S2 Nb2 103.9(4) 4 . ?
S5 S2 Nb1 120.24(14) . . ?
B1 S2 Nb1 87.9(4) 4 . ?
Nb2 S2 Nb1 77.27(5) . . ?
B1 S3 B1 27.7(8) 4 . ?
B1 S3 Nb1 91.7(4) 4 . ?
B1 S3 Nb1 109.1(4) . . ?
B1 S3 Nb1 109.1(4) 4 4 ?
B1 S3 Nb1 91.7(4) . 4 ?
Nb1 S3 Nb1 76.56(6) . 4 ?
Nb1 S4 Nb1 82.80(7) 4 . ?
Cl2 C17 Cl2 96(2) 4 . ?
Cl2 C17 Cl1 106.1(13) 4 . ?
Cl2 C17 Cl1 106.1(13) . . ?
Cl2' Cl2' C17' 67.1(17) 4 . ?
Cl1' C17' Cl2' 107(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
S2 S5 B1 S3 58.1(5) . . . . ?
S2 S5 B1 S2 -56.5(6) . . . 4 ?
C5 C1 C2 C3 1.3(8) . . . . ?
C7 C1 C2 C3 -173.4(7) . . . . ?
Nb1 C1 C2 C3 66.8(5) . . . . ?
C5 C1 C2 C8 174.7(6) . . . . ?
C7 C1 C2 C8 0.1(11) . . . . ?
Nb1 C1 C2 C8 -119.8(7) . . . . ?
C5 C1 C2 Nb1 -65.5(5) . . . . ?
C7 C1 C2 Nb1 119.9(7) . . . . ?
C1 C2 C3 C4 -1.4(8) . . . . ?
C8 C2 C3 C4 -174.5(7) . . . . ?
Nb1 C2 C3 C4 65.1(5) . . . . ?
C1 C2 C3 C9 170.1(7) . . . . ?
C8 C2 C3 C9 -2.9(12) . . . . ?
Nb1 C2 C3 C9 -123.3(7) . . . . ?
C1 C2 C3 Nb1 -66.6(5) . . . . ?
C8 C2 C3 Nb1 120.4(7) . . . . ?
C2 C3 C4 C5 1.1(8) . . . . ?
C9 C3 C4 C5 -170.3(7) . . . . ?
Nb1 C3 C4 C5 65.5(5) . . . . ?
C2 C3 C4 C10 171.4(7) . . . . ?
C9 C3 C4 C10 0.1(11) . . . . ?
Nb1 C3 C4 C10 -124.1(7) . . . . ?
C2 C3 C4 Nb1 -64.4(5) . . . . ?
C9 C3 C4 Nb1 124.2(8) . . . . ?
C3 C4 C5 C1 -0.3(7) . . . . ?
C10 C4 C5 C1 -170.0(7) . . . . ?
Nb1 C4 C5 C1 65.5(5) . . . . ?
C3 C4 C5 C6 172.6(7) . . . . ?
C10 C4 C5 C6 2.8(12) . . . . ?
Nb1 C4 C5 C6 -121.6(7) . . . . ?
C3 C4 C5 Nb1 -65.8(5) . . . . ?
C10 C4 C5 Nb1 124.5(8) . . . . ?
C2 C1 C5 C4 -0.6(7) . . . . ?
C7 C1 C5 C4 174.0(7) . . . . ?
Nb1 C1 C5 C4 -65.9(5) . . . . ?
C2 C1 C5 C6 -173.6(7) . . . . ?
C7 C1 C5 C6 1.0(11) . . . . ?
Nb1 C1 C5 C6 121.1(7) . . . . ?
C2 C1 C5 Nb1 65.3(5) . . . . ?
C7 C1 C5 Nb1 -120.1(7) . . . . ?
C11 C11 C12 C13 -1.5(6) 4 . . . ?
C16 C11 C12 C13 168.9(7) . . . . ?
Nb2 C11 C12 C13 -66.7(5) . . . . ?
C11 C11 C12 C15 -174.8(5) 4 . . . ?
C16 C11 C12 C15 -4.4(10) . . . . ?
Nb2 C11 C12 C15 120.0(6) . . . . ?
C11 C11 C12 Nb2 65.25(15) 4 . . . ?
C16 C11 C12 Nb2 -124.4(7) . . . . ?
C11 C12 C13 C12 2.3(9) . . . 4 ?
C15 C12 C13 C12 175.6(4) . . . 4 ?
Nb2 C12 C13 C12 -64.0(5) . . . 4 ?
C11 C12 C13 C14 -175.0(8) . . . . ?
C15 C12 C13 C14 -1.7(12) . . . . ?
Nb2 C12 C13 C14 118.6(9) . . . . ?
C11 C12 C13 Nb2 66.3(4) . . . . ?
C15 C12 C13 Nb2 -120.4(6) . . . . ?
Cl2' Cl2' C17' Cl1' 97.4(12) 4 . . . ?

_refine_diff_density_max         0.862
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.103

