# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_SGGR3
_database_code_depnum_ccdc_archive 'CCDC 1979258'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C27 H38 B4 N Nb2 O S'
_chemical_formula_sum            'C27 H38 B4 N Nb2 O S'
_chemical_formula_weight         653.70
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'
_space_group_IT_number           7
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   12.3639(14)
_cell_length_b                   9.6186(9)
_cell_length_c                   13.6552(14)
_cell_angle_alpha                90
_cell_angle_beta                 106.009(4)
_cell_angle_gamma                90
_cell_volume                     1560.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9988
_cell_measurement_theta_min      2.6100
_cell_measurement_theta_max      27.4734
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             666
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_T_max  0.968

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_av_r_equivalents  0.0439
_diffrn_reflns_av_uneti/neti     0.0634
_diffrn_reflns_number            15028
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.117
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             6903
_reflns_number_gt                6300
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_max     0.919
_reflns_Friedel_fraction_full    0.935

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2018)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0974P)²+8.4148P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6903
_refine_ls_number_parameters     234
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1876
_refine_ls_wR_factor_gt          0.1800
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.140
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(13)

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
S S 0.1246 0.1234 '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'
Nb Nb -2.0727 0.6215 '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'

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
Nb1 Nb 0.59622(7) 0.31005(10) 0.28479(7) 0.0222(2) Uani 1 1 d . . . . .
C1 C 0.7981(11) 0.3129(12) 0.3371(11) 0.0292(12) Uani 1 1 d . . . . .
C2 C 0.7607(11) 0.4273(13) 0.3836(9) 0.0292(12) Uani 1 1 d . . . . .
C3 C 0.7020(11) 0.5202(12) 0.3059(10) 0.0292(12) Uani 1 1 d . . . . .
C4 C 0.7021(11) 0.4572(13) 0.2099(10) 0.0292(12) Uani 1 1 d . . . . .
C5 C 0.7638(11) 0.3296(12) 0.2318(10) 0.0292(12) Uani 1 1 d . . . . .
C6 C 0.8731(13) 0.1932(17) 0.3960(13) 0.0464(16) Uani 1 1 d . . . . .
H6A H 0.860485 0.108978 0.353936 0.070 Uiso 1 1 calc R U . . .
H6B H 0.853461 0.174954 0.459596 0.070 Uiso 1 1 calc R U . . .
H6C H 0.952418 0.220185 0.411490 0.070 Uiso 1 1 calc R U . . .
C7 C 0.7861(13) 0.4595(17) 0.4962(12) 0.0464(16) Uani 1 1 d . . . . .
H7A H 0.827223 0.547599 0.510763 0.070 Uiso 1 1 calc R U . . .
H7B H 0.832120 0.384743 0.535596 0.070 Uiso 1 1 calc R U . . .
H7C H 0.715480 0.466944 0.515251 0.070 Uiso 1 1 calc R U . . .
C8 C 0.6569(14) 0.6593(17) 0.3194(13) 0.0464(16) Uani 1 1 d . . . . .
H8A H 0.621299 0.656089 0.375240 0.070 Uiso 1 1 calc R U . . .
H8B H 0.600994 0.686888 0.256363 0.070 Uiso 1 1 calc R U . . .
H8C H 0.718423 0.727107 0.335559 0.070 Uiso 1 1 calc R U . . .
C9 C 0.6658(13) 0.5255(17) 0.1074(12) 0.0464(16) Uani 1 1 d . . . . .
H9A H 0.721129 0.596112 0.102448 0.070 Uiso 1 1 calc R U . . .
H9B H 0.592259 0.569552 0.098647 0.070 Uiso 1 1 calc R U . . .
H9C H 0.660163 0.455380 0.054166 0.070 Uiso 1 1 calc R U . . .
C10 C 0.7933(13) 0.2366(18) 0.1540(13) 0.0464(16) Uani 1 1 d . . . . .
H10A H 0.735552 0.245335 0.088687 0.070 Uiso 1 1 calc R U . . .
H10B H 0.797079 0.139925 0.177225 0.070 Uiso 1 1 calc R U . . .
H10C H 0.866451 0.264299 0.145409 0.070 Uiso 1 1 calc R U . . .
Nb2 Nb 0.38193(7) 0.16621(9) 0.27407(6) 0.0214(2) Uani 1 1 d . . . . .
C11 C 0.1888(14) 0.129(2) 0.1915(13) 0.0491(17) Uani 1 1 d . . . . .
C12 C 0.2435(13) -0.0047(19) 0.2016(13) 0.0491(17) Uani 1 1 d . . . . .
C13 C 0.2793(13) -0.0322(19) 0.3112(13) 0.0491(17) Uani 1 1 d . . . . .
C14 C 0.2495(13) 0.077(2) 0.3573(13) 0.0491(17) Uani 1 1 d . . . . .
C15 C 0.1937(14) 0.1729(18) 0.2904(14) 0.0491(17) Uani 1 1 d . . . . .
C16 C 0.124(2) 0.186(3) 0.090(2) 0.098(4) Uani 1 1 d . . . . .
H16A H 0.168459 0.175630 0.041255 0.147 Uiso 1 1 calc R U . . .
H16B H 0.107671 0.284512 0.097166 0.147 Uiso 1 1 calc R U . . .
H16C H 0.053065 0.134600 0.065483 0.147 Uiso 1 1 calc R U . . .
C17 C 0.246(2) -0.105(3) 0.117(2) 0.098(4) Uani 1 1 d . . . . .
H17A H 0.321705 -0.142902 0.128444 0.147 Uiso 1 1 calc R U . . .
H17B H 0.223379 -0.056885 0.051540 0.147 Uiso 1 1 calc R U . . .
H17C H 0.192886 -0.181677 0.116752 0.147 Uiso 1 1 calc R U . . .
C18 C 0.325(2) -0.174(3) 0.352(3) 0.098(4) Uani 1 1 d . . . . .
H18A H 0.264048 -0.231720 0.361649 0.147 Uiso 1 1 calc R U . . .
H18B H 0.382866 -0.162239 0.416736 0.147 Uiso 1 1 calc R U . . .
H18C H 0.358776 -0.218772 0.302510 0.147 Uiso 1 1 calc R U . . .
C19 C 0.260(2) 0.077(3) 0.474(2) 0.098(4) Uani 1 1 d . . . . .
H19A H 0.264058 0.173050 0.498322 0.147 Uiso 1 1 calc R U . . .
H19B H 0.328034 0.026766 0.510162 0.147 Uiso 1 1 calc R U . . .
H19C H 0.193843 0.031264 0.485870 0.147 Uiso 1 1 calc R U . . .
C20 C 0.144(2) 0.310(3) 0.315(2) 0.098(4) Uani 1 1 d . . . . .
H20A H 0.141023 0.308681 0.386176 0.147 Uiso 1 1 calc R U . . .
H20B H 0.067248 0.320913 0.270091 0.147 Uiso 1 1 calc R U . . .
H20C H 0.190542 0.387578 0.304792 0.147 Uiso 1 1 calc R U . . .
S1 S 0.4370(3) 0.4884(3) 0.4731(2) 0.0316(6) Uani 1 1 d . . . . .
B21 B 0.4117(12) 0.4096(13) 0.2547(9) 0.0237(18) Uani 1 1 d . . . . .
H21 H 0.368889 0.491094 0.218082 0.028 Uiso 1 1 calc R U . . .
B22 B 0.4662(12) 0.3495(13) 0.3837(10) 0.0237(18) Uani 1 1 d . . . . .
C23 C 0.4622(10) 0.3921(11) 0.5846(9) 0.026(2) Uani 1 1 d . . . . .
N24 N 0.4813(10) 0.2616(12) 0.6004(9) 0.036(2) Uani 1 1 d . . . . .
C25 C 0.4892(11) 0.2437(15) 0.7040(11) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.5052(13) 0.1279(16) 0.7665(15) 0.049(4) Uani 1 1 d . . . . .
H26 H 0.514479 0.038051 0.741114 0.058 Uiso 1 1 calc R U . . .
C27 C 0.5072(14) 0.1470(18) 0.8641(15) 0.048(4) Uani 1 1 d . . . . .
H27 H 0.518812 0.067846 0.907331 0.058 Uiso 1 1 calc R U . . .
C28 C 0.4939(12) 0.2694(17) 0.9045(14) 0.044(3) Uani 1 1 d . . . . .
H28 H 0.496359 0.274821 0.974530 0.053 Uiso 1 1 calc R U . . .
C29 C 0.4761(13) 0.3926(15) 0.8442(12) 0.039(3) Uani 1 1 d . . . . .
H29 H 0.466317 0.481439 0.870868 0.046 Uiso 1 1 calc R U . . .
C30 C 0.4742(10) 0.3721(13) 0.7447(11) 0.031(3) Uani 1 1 d . . . . .
O31 O 0.4562(8) 0.4702(9) 0.6700(6) 0.0325(19) Uani 1 1 d . . . . .
B41 B 0.5104(12) 0.1204(13) 0.1760(10) 0.0260(19) Uani 1 1 d . . . . .
H41 H 0.507047 0.085344 0.106323 0.031 Uiso 1 1 calc R U . . .
B42 B 0.5676(12) 0.0656(13) 0.3042(11) 0.0260(19) Uani 1 1 d . . . . .
H42A H 0.494(12) 0.065(15) 0.364(11) 0.031 Uiso 1 1 d . U . . .
H42B H 0.600(12) -0.033(15) 0.308(11) 0.031 Uiso 1 1 d . U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Nb1 C4 2.346(12) . ?
Nb1 C3 2.381(12) . ?
Nb1 C5 2.383(13) . ?
Nb1 C2 2.390(12) . ?
Nb1 B22 2.398(14) . ?
Nb1 C1 2.400(13) . ?
Nb1 B21 2.402(14) . ?
Nb1 B42 2.404(13) . ?
Nb1 B41 2.407(13) . ?
Nb1 Nb2 2.9566(14) . ?
C1 C5 1.391(19) . ?
C1 C2 1.411(18) . ?
C1 C6 1.56(2) . ?
C2 C3 1.424(17) . ?
C2 C7 1.51(2) . ?
C3 C4 1.445(18) . ?
C3 C8 1.48(2) . ?
C4 C5 1.433(17) . ?
C4 C9 1.498(19) . ?
C5 C10 1.51(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Nb2 B22 2.362(13) . ?
Nb2 C11 2.369(16) . ?
Nb2 C12 2.382(16) . ?
Nb2 B41 2.383(15) . ?
Nb2 B21 2.395(13) . ?
Nb2 C14 2.396(16) . ?
Nb2 C15 2.400(17) . ?
Nb2 B42 2.420(15) . ?
Nb2 C13 2.422(16) . ?
Nb2 H42A 1.86(14) . ?
C11 C15 1.40(3) . ?
C11 C12 1.44(3) . ?
C11 C16 1.50(3) . ?
C12 C13 1.46(2) . ?
C12 C17 1.51(3) . ?
C13 C14 1.32(3) . ?
C13 C18 1.52(3) . ?
C14 C15 1.35(3) . ?
C14 C19 1.56(3) . ?
C15 C20 1.53(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
S1 C23 1.736(13) . ?
S1 B22 1.910(14) . ?
B21 B22 1.799(17) . ?
B21 H21 1.0000 . ?
C23 N24 1.285(16) . ?
C23 O31 1.406(13) . ?
N24 C25 1.401(18) . ?
C25 C26 1.38(2) . ?
C25 C30 1.388(18) . ?
C26 C27 1.34(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.33(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.43(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.37(2) . ?
C29 H29 0.9500 . ?
C30 O31 1.361(16) . ?
B41 B42 1.777(19) . ?
B41 H41 1.0000 . ?
B42 H42A 1.38(14) . ?
B42 H42B 1.03(14) . ?

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
C4 Nb1 C3 35.6(4) . . ?
C4 Nb1 C5 35.3(4) . . ?
C3 Nb1 C5 58.4(4) . . ?
C4 Nb1 C2 58.1(4) . . ?
C3 Nb1 C2 34.7(4) . . ?
C5 Nb1 C2 57.2(4) . . ?
C4 Nb1 B22 133.8(4) . . ?
C3 Nb1 B22 103.2(4) . . ?
C5 Nb1 B22 158.8(4) . . ?
C2 Nb1 B22 101.8(4) . . ?
C4 Nb1 C1 57.5(4) . . ?
C3 Nb1 C1 57.5(4) . . ?
C5 Nb1 C1 33.8(4) . . ?
C2 Nb1 C1 34.3(4) . . ?
B22 Nb1 C1 129.4(5) . . ?
C4 Nb1 B21 107.6(4) . . ?
C3 Nb1 B21 98.4(4) . . ?
C5 Nb1 B21 141.3(4) . . ?
C2 Nb1 B21 121.9(4) . . ?
B22 Nb1 B21 44.0(4) . . ?
C1 Nb1 B21 155.1(4) . . ?
C4 Nb1 B42 139.0(5) . . ?
C3 Nb1 B42 155.5(5) . . ?
C5 Nb1 B42 106.1(5) . . ?
C2 Nb1 B42 121.8(4) . . ?
B22 Nb1 B42 87.2(5) . . ?
C1 Nb1 B42 98.7(5) . . ?
B21 Nb1 B42 104.3(5) . . ?
C4 Nb1 B41 113.1(5) . . ?
C3 Nb1 B41 148.5(5) . . ?
C5 Nb1 B41 98.3(5) . . ?
C2 Nb1 B41 150.2(5) . . ?
B22 Nb1 B41 102.6(5) . . ?
C1 Nb1 B41 116.0(5) . . ?
B21 Nb1 B41 87.7(5) . . ?
B42 Nb1 B41 43.3(5) . . ?
C4 Nb1 Nb2 149.4(3) . . ?
C3 Nb1 Nb2 149.1(3) . . ?
C5 Nb1 Nb2 149.8(3) . . ?
C2 Nb1 Nb2 149.3(3) . . ?
B22 Nb1 Nb2 51.0(3) . . ?
C1 Nb1 Nb2 149.8(3) . . ?
B21 Nb1 Nb2 51.9(3) . . ?
B42 Nb1 Nb2 52.4(4) . . ?
B41 Nb1 Nb2 51.5(4) . . ?
C5 C1 C2 109.4(11) . . ?
C5 C1 C6 126.0(13) . . ?
C2 C1 C6 124.5(13) . . ?
C5 C1 Nb1 72.4(8) . . ?
C2 C1 Nb1 72.5(7) . . ?
C6 C1 Nb1 124.6(9) . . ?
C1 C2 C3 108.5(11) . . ?
C1 C2 C7 128.0(12) . . ?
C3 C2 C7 123.3(12) . . ?
C1 C2 Nb1 73.2(7) . . ?
C3 C2 Nb1 72.3(7) . . ?
C7 C2 Nb1 125.2(9) . . ?
C2 C3 C4 106.6(11) . . ?
C2 C3 C8 127.3(13) . . ?
C4 C3 C8 125.9(12) . . ?
C2 C3 Nb1 73.0(7) . . ?
C4 C3 Nb1 70.9(7) . . ?
C8 C3 Nb1 124.7(9) . . ?
C5 C4 C3 107.7(11) . . ?
C5 C4 C9 125.2(12) . . ?
C3 C4 C9 126.0(12) . . ?
C5 C4 Nb1 73.8(7) . . ?
C3 C4 Nb1 73.5(7) . . ?
C9 C4 Nb1 127.7(9) . . ?
C1 C5 C4 107.9(11) . . ?
C1 C5 C10 126.6(12) . . ?
C4 C5 C10 125.4(12) . . ?
C1 C5 Nb1 73.7(8) . . ?
C4 C5 Nb1 70.9(7) . . ?
C10 C5 Nb1 124.5(9) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
B22 Nb2 C11 128.7(6) . . ?
B22 Nb2 C12 156.8(5) . . ?
C11 Nb2 C12 35.3(6) . . ?
B22 Nb2 B41 104.4(5) . . ?
C11 Nb2 B41 116.4(5) . . ?
C12 Nb2 B41 98.8(5) . . ?
B22 Nb2 B21 44.4(4) . . ?
C11 Nb2 B21 105.1(6) . . ?
C12 Nb2 B21 138.0(6) . . ?
B41 Nb2 B21 88.4(5) . . ?
B22 Nb2 C14 102.0(5) . . ?
C11 Nb2 C14 56.0(6) . . ?
C12 Nb2 C14 56.1(6) . . ?
B41 Nb2 C14 148.0(6) . . ?
B21 Nb2 C14 123.4(6) . . ?
B22 Nb2 C15 101.0(5) . . ?
C11 Nb2 C15 34.1(6) . . ?
C12 Nb2 C15 56.8(6) . . ?
B41 Nb2 C15 150.6(6) . . ?
B21 Nb2 C15 99.6(5) . . ?
C14 Nb2 C15 32.7(6) . . ?
B22 Nb2 B42 87.7(5) . . ?
C11 Nb2 B42 143.6(6) . . ?
C12 Nb2 B42 109.5(5) . . ?
B41 Nb2 B42 43.4(5) . . ?
B21 Nb2 B42 104.0(5) . . ?
C14 Nb2 B42 121.1(6) . . ?
C15 Nb2 B42 153.4(5) . . ?
B22 Nb2 C13 128.4(5) . . ?
C11 Nb2 C13 57.5(6) . . ?
C12 Nb2 C13 35.4(6) . . ?
B41 Nb2 C13 116.1(5) . . ?
B21 Nb2 C13 154.0(6) . . ?
C14 Nb2 C13 31.9(6) . . ?
C15 Nb2 C13 54.8(6) . . ?
B42 Nb2 C13 100.2(5) . . ?
B22 Nb2 Nb1 52.2(4) . . ?
C11 Nb2 Nb1 150.0(4) . . ?
C12 Nb2 Nb1 151.0(4) . . ?
B41 Nb2 Nb1 52.2(3) . . ?
B21 Nb2 Nb1 52.1(3) . . ?
C14 Nb2 Nb1 149.9(4) . . ?
C15 Nb2 Nb1 149.5(4) . . ?
B42 Nb2 Nb1 51.9(3) . . ?
C13 Nb2 Nb1 150.8(4) . . ?
B22 Nb2 H42A 82(4) . . ?
C11 Nb2 H42A 135(4) . . ?
C12 Nb2 H42A 103(4) . . ?
B41 Nb2 H42A 77(4) . . ?
B21 Nb2 H42A 118(4) . . ?
C14 Nb2 H42A 89(4) . . ?
C15 Nb2 H42A 121(4) . . ?
B42 Nb2 H42A 34(4) . . ?
C13 Nb2 H42A 78(4) . . ?
Nb1 Nb2 H42A 74(4) . . ?
C15 C11 C12 106.4(16) . . ?
C15 C11 C16 131(2) . . ?
C12 C11 C16 122.1(18) . . ?
C15 C11 Nb2 74.1(9) . . ?
C12 C11 Nb2 72.8(9) . . ?
C16 C11 Nb2 126.7(13) . . ?
C11 C12 C13 105.1(15) . . ?
C11 C12 C17 127.2(19) . . ?
C13 C12 C17 126.9(19) . . ?
C11 C12 Nb2 71.8(9) . . ?
C13 C12 Nb2 73.8(9) . . ?
C17 C12 Nb2 126.7(12) . . ?
C14 C13 C12 107.4(17) . . ?
C14 C13 C18 131(2) . . ?
C12 C13 C18 120.7(19) . . ?
C14 C13 Nb2 73.0(10) . . ?
C12 C13 Nb2 70.8(9) . . ?
C18 C13 Nb2 128.1(13) . . ?
C13 C14 C15 112.2(17) . . ?
C13 C14 C19 122(2) . . ?
C15 C14 C19 125(2) . . ?
C13 C14 Nb2 75.1(10) . . ?
C15 C14 Nb2 73.8(10) . . ?
C19 C14 Nb2 127.4(12) . . ?
C14 C15 C11 108.9(17) . . ?
C14 C15 C20 127(2) . . ?
C11 C15 C20 124(2) . . ?
C14 C15 Nb2 73.5(10) . . ?
C11 C15 Nb2 71.7(9) . . ?
C20 C15 Nb2 120.3(12) . . ?
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 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 S1 B22 99.6(5) . . ?
B22 B21 Nb2 66.8(6) . . ?
B22 B21 Nb1 67.9(6) . . ?
Nb2 B21 Nb1 76.1(4) . . ?
B22 B21 H21 138.2 . . ?
Nb2 B21 H21 138.2 . . ?
Nb1 B21 H21 138.2 . . ?
B21 B22 S1 108.4(8) . . ?
B21 B22 Nb2 68.8(6) . . ?
S1 B22 Nb2 143.1(8) . . ?
B21 B22 Nb1 68.1(6) . . ?
S1 B22 Nb1 138.1(7) . . ?
Nb2 B22 Nb1 76.8(4) . . ?
N24 C23 O31 115.6(11) . . ?
N24 C23 S1 130.5(9) . . ?
O31 C23 S1 113.9(8) . . ?
C23 N24 C25 104.3(11) . . ?
C26 C25 C30 118.8(15) . . ?
C26 C25 N24 132.8(14) . . ?
C30 C25 N24 108.4(13) . . ?
C27 C26 C25 117.6(15) . . ?
C27 C26 H26 121.2 . . ?
C25 C26 H26 121.2 . . ?
C28 C27 C26 124.4(17) . . ?
C28 C27 H27 117.8 . . ?
C26 C27 H27 117.8 . . ?
C27 C28 C29 120.9(18) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C30 C29 C28 114.4(14) . . ?
C30 C29 H29 122.8 . . ?
C28 C29 H29 122.8 . . ?
O31 C30 C29 126.8(12) . . ?
O31 C30 C25 109.2(12) . . ?
C29 C30 C25 124.0(13) . . ?
C30 O31 C23 102.5(9) . . ?
B42 B41 Nb2 69.4(7) . . ?
B42 B41 Nb1 68.2(6) . . ?
Nb2 B41 Nb1 76.2(4) . . ?
B42 B41 H41 137.6 . . ?
Nb2 B41 H41 137.6 . . ?
Nb1 B41 H41 137.6 . . ?
B41 B42 Nb1 68.4(6) . . ?
B41 B42 Nb2 67.2(6) . . ?
Nb1 B42 Nb2 75.6(4) . . ?
B41 B42 H42A 116(6) . . ?
Nb1 B42 H42A 102(6) . . ?
Nb2 B42 H42A 50(6) . . ?
B41 B42 H42B 111(8) . . ?
Nb1 B42 H42B 148(8) . . ?
Nb2 B42 H42B 136(8) . . ?
H42A B42 H42B 106(10) . . ?

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 -0.7(15) . . . . ?
C6 C1 C2 C3 175.5(12) . . . . ?
Nb1 C1 C2 C3 -64.2(9) . . . . ?
C5 C1 C2 C7 -174.6(13) . . . . ?
C6 C1 C2 C7 2(2) . . . . ?
Nb1 C1 C2 C7 121.9(13) . . . . ?
C5 C1 C2 Nb1 63.5(9) . . . . ?
C6 C1 C2 Nb1 -120.3(12) . . . . ?
C1 C2 C3 C4 1.5(14) . . . . ?
C7 C2 C3 C4 175.7(12) . . . . ?
Nb1 C2 C3 C4 -63.4(8) . . . . ?
C1 C2 C3 C8 -174.2(13) . . . . ?
C7 C2 C3 C8 0(2) . . . . ?
Nb1 C2 C3 C8 121.0(14) . . . . ?
C1 C2 C3 Nb1 64.8(9) . . . . ?
C7 C2 C3 Nb1 -120.9(12) . . . . ?
C2 C3 C4 C5 -1.7(13) . . . . ?
C8 C3 C4 C5 174.0(13) . . . . ?
Nb1 C3 C4 C5 -66.4(8) . . . . ?
C2 C3 C4 C9 -170.2(12) . . . . ?
C8 C3 C4 C9 6(2) . . . . ?
Nb1 C3 C4 C9 125.0(13) . . . . ?
C2 C3 C4 Nb1 64.8(8) . . . . ?
C8 C3 C4 Nb1 -119.5(13) . . . . ?
C2 C1 C5 C4 -0.4(14) . . . . ?
C6 C1 C5 C4 -176.5(12) . . . . ?
Nb1 C1 C5 C4 63.2(9) . . . . ?
C2 C1 C5 C10 175.2(12) . . . . ?
C6 C1 C5 C10 -1(2) . . . . ?
Nb1 C1 C5 C10 -121.2(13) . . . . ?
C2 C1 C5 Nb1 -63.5(9) . . . . ?
C6 C1 C5 Nb1 120.4(13) . . . . ?
C3 C4 C5 C1 1.3(14) . . . . ?
C9 C4 C5 C1 169.9(13) . . . . ?
Nb1 C4 C5 C1 -65.0(9) . . . . ?
C3 C4 C5 C10 -174.4(12) . . . . ?
C9 C4 C5 C10 -6(2) . . . . ?
Nb1 C4 C5 C10 119.3(13) . . . . ?
C3 C4 C5 Nb1 66.3(8) . . . . ?
C9 C4 C5 Nb1 -125.1(13) . . . . ?
C15 C11 C12 C13 -0.3(16) . . . . ?
C16 C11 C12 C13 -170.2(16) . . . . ?
Nb2 C11 C12 C13 66.8(10) . . . . ?
C15 C11 C12 C17 170.2(17) . . . . ?
C16 C11 C12 C17 0(3) . . . . ?
Nb2 C11 C12 C17 -122.7(18) . . . . ?
C15 C11 C12 Nb2 -67.1(10) . . . . ?
C16 C11 C12 Nb2 123.0(16) . . . . ?
C11 C12 C13 C14 -1.1(17) . . . . ?
C17 C12 C13 C14 -171.6(17) . . . . ?
Nb2 C12 C13 C14 64.3(11) . . . . ?
C11 C12 C13 C18 171.0(16) . . . . ?
C17 C12 C13 C18 1(3) . . . . ?
Nb2 C12 C13 C18 -123.5(16) . . . . ?
C11 C12 C13 Nb2 -65.5(10) . . . . ?
C17 C12 C13 Nb2 124.1(17) . . . . ?
C12 C13 C14 C15 2.2(18) . . . . ?
C18 C13 C14 C15 -168.8(18) . . . . ?
Nb2 C13 C14 C15 65.1(12) . . . . ?
C12 C13 C14 C19 172.0(15) . . . . ?
C18 C13 C14 C19 1(3) . . . . ?
Nb2 C13 C14 C19 -125.1(16) . . . . ?
C12 C13 C14 Nb2 -62.9(10) . . . . ?
C18 C13 C14 Nb2 126(2) . . . . ?
C13 C14 C15 C11 -2.4(19) . . . . ?
C19 C14 C15 C11 -171.8(16) . . . . ?
Nb2 C14 C15 C11 63.5(11) . . . . ?
C13 C14 C15 C20 178.2(17) . . . . ?
C19 C14 C15 C20 9(3) . . . . ?
Nb2 C14 C15 C20 -115.9(18) . . . . ?
C13 C14 C15 Nb2 -65.9(12) . . . . ?
C19 C14 C15 Nb2 124.7(17) . . . . ?
C12 C11 C15 C14 1.6(17) . . . . ?
C16 C11 C15 C14 170.3(19) . . . . ?
Nb2 C11 C15 C14 -64.6(11) . . . . ?
C12 C11 C15 C20 -179.1(16) . . . . ?
C16 C11 C15 C20 -10(3) . . . . ?
Nb2 C11 C15 C20 114.7(16) . . . . ?
C12 C11 C15 Nb2 66.2(10) . . . . ?
C16 C11 C15 Nb2 -125.0(19) . . . . ?
Nb2 B21 B22 S1 -140.8(8) . . . . ?
Nb1 B21 B22 S1 135.4(7) . . . . ?
Nb1 B21 B22 Nb2 -83.8(3) . . . . ?
Nb2 B21 B22 Nb1 83.8(3) . . . . ?
B22 S1 C23 N24 -7.5(14) . . . . ?
B22 S1 C23 O31 175.1(9) . . . . ?
O31 C23 N24 C25 0.3(15) . . . . ?
S1 C23 N24 C25 -176.9(10) . . . . ?
C23 N24 C25 C26 177.7(16) . . . . ?
C23 N24 C25 C30 -0.5(15) . . . . ?
C30 C25 C26 C27 -1(2) . . . . ?
N24 C25 C26 C27 -179.1(15) . . . . ?
C25 C26 C27 C28 1(3) . . . . ?
C26 C27 C28 C29 0(3) . . . . ?
C27 C28 C29 C30 0(2) . . . . ?
C28 C29 C30 O31 178.4(12) . . . . ?
C28 C29 C30 C25 -1(2) . . . . ?
C26 C25 C30 O31 -178.0(12) . . . . ?
N24 C25 C30 O31 0.5(15) . . . . ?
C26 C25 C30 C29 1(2) . . . . ?
N24 C25 C30 C29 179.6(13) . . . . ?
C29 C30 O31 C23 -179.4(14) . . . . ?
C25 C30 O31 C23 -0.3(13) . . . . ?
N24 C23 O31 C30 0.0(14) . . . . ?
S1 C23 O31 C30 177.7(8) . . . . ?
Nb2 B41 B42 Nb1 -82.9(3) . . . . ?
Nb1 B41 B42 Nb2 82.9(3) . . . . ?

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR SGGR3                                                  #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
####################################################################### 
# 
# 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_SGGBB3
_audit_block_doi                 10.5517/ccdc.csd.cc26s69j
_database_code_depnum_ccdc_archive 'CCDC 2049047'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2020-12-21 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 26 novembre 2018                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C17 H19 Cl3 N S2 Ta'
_chemical_formula_sum            'C17 H19 Cl3 N S2 Ta'
_chemical_formula_weight         588.75
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.1531(19)
_cell_length_b                   8.2431(10)
_cell_length_c                   16.1868(17)
_cell_angle_alpha                90
_cell_angle_beta                 116.994(3)
_cell_angle_gamma                90
_cell_volume                     1920.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9310
_cell_measurement_theta_min      2.8304
_cell_measurement_theta_max      27.5035
_cell_measurement_wavelength     0.71073


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0263694
_diffrn_orient_matrix_UB_21      -0.0502944
_diffrn_orient_matrix_UB_31      0.0400272
_diffrn_orient_matrix_UB_12      0.1101077
_diffrn_orient_matrix_UB_22      0.0499873
_diffrn_orient_matrix_UB_32      -0.0097283
_diffrn_orient_matrix_UB_13      0.0008650
_diffrn_orient_matrix_UB_23      0.0114031
_diffrn_orient_matrix_UB_33      0.0683828


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1136
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_T_max  0.641

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.1/2016-03-01                           #
# Number of scans            :        3                                        #
# Total number of frames [*] :      244                                        #
# Total length of scans  [*] :   244.00 (deg.)                                 #
# Rotation speed         [*] :     8.00 sec./deg.                              #
# Total exposition time  [*] :         32.5 min.                               #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
# Measurement mode           : shutterless mode                                #
#                                                                              #
#   Scan   Time(s)  Width  DX (mm)  Frames  Theta  Omega    Phi    Chi   T(K)  #
#                                                                              #
#  1 Phi       8.0   1.00     34.0     184   0.27 270.94  28.00  23.00 150.00  #
#  2 Omega     8.0   1.00     34.0      60   0.63   0.82 237.22 303.68 150.00  #
#  3 Fast      1.0   1.00     34.0     180   0.00 360.00   0.00  54.74 150.00  #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0359
_diffrn_reflns_av_r_equivalents  0.0423
_diffrn_reflns_number            18536
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.410
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             4396
_reflns_number_gt                4074
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.

;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0183P)²+3.7717P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4396
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0592
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.149

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
S S 0.1246 0.1234 '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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ta1 Ta 0.23355(2) 0.82302(2) 0.50334(2) 0.01054(5) Uani 1 1 d . . . . .
Cl1 Cl 0.38055(6) 0.68206(11) 0.56748(7) 0.02017(19) Uani 1 1 d . . . . .
Cl2 Cl 0.14147(6) 1.06633(11) 0.46893(7) 0.01784(18) Uani 1 1 d . . . . .
Cl3 Cl 0.26242(7) 0.86471(13) 0.66076(6) 0.0226(2) Uani 1 1 d . . . . .
S1 S 0.26384(6) 0.89558(12) 0.36843(6) 0.01513(18) Uani 1 1 d . . . . .
S2 S 0.42198(7) 1.15501(12) 0.44217(7) 0.0190(2) Uani 1 1 d . . . . .
C1 C 0.0694(3) 0.7277(5) 0.4155(3) 0.0195(8) Uani 1 1 d . . . . .
C2 C 0.1055(3) 0.6648(5) 0.5067(3) 0.0180(8) Uani 1 1 d . . . . .
C3 C 0.1788(3) 0.5539(4) 0.5205(3) 0.0152(7) Uani 1 1 d . . . . .
C4 C 0.1881(3) 0.5497(4) 0.4369(3) 0.0158(7) Uani 1 1 d . . . . .
C5 C 0.1218(3) 0.6592(5) 0.3729(3) 0.0189(8) Uani 1 1 d . . . . .
C6 C -0.0180(3) 0.8234(5) 0.3658(3) 0.0314(11) Uani 1 1 d . . . . .
H6A H -0.070105 0.749377 0.332246 0.047 Uiso 1 1 calc R U . . .
H6B H -0.011479 0.897335 0.321654 0.047 Uiso 1 1 calc R U . . .
H6C H -0.029758 0.886300 0.410734 0.047 Uiso 1 1 calc R U . . .
C7 C 0.0645(3) 0.6937(6) 0.5718(3) 0.0282(10) Uani 1 1 d . . . . .
H7A H 0.050576 0.809340 0.571945 0.042 Uiso 1 1 calc R U . . .
H7B H 0.109030 0.660096 0.634430 0.042 Uiso 1 1 calc R U . . .
H7C H 0.007211 0.630579 0.551546 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2297(3) 0.4508(5) 0.6049(3) 0.0232(8) Uani 1 1 d . . . . .
H8A H 0.197427 0.346805 0.596535 0.035 Uiso 1 1 calc R U . . .
H8B H 0.231681 0.506585 0.659233 0.035 Uiso 1 1 calc R U . . .
H8C H 0.293160 0.431554 0.614100 0.035 Uiso 1 1 calc R U . . .
C9 C 0.2477(3) 0.4371(5) 0.4149(3) 0.0231(9) Uani 1 1 d . . . . .
H9A H 0.298026 0.395912 0.472712 0.035 Uiso 1 1 calc R U . . .
H9B H 0.274152 0.495300 0.379665 0.035 Uiso 1 1 calc R U . . .
H9C H 0.210058 0.346036 0.377994 0.035 Uiso 1 1 calc R U . . .
C10 C 0.0982(3) 0.6728(5) 0.2722(3) 0.0290(10) Uani 1 1 d . . . . .
H10A H 0.153749 0.650538 0.264179 0.044 Uiso 1 1 calc R U . . .
H10B H 0.075900 0.782671 0.250249 0.044 Uiso 1 1 calc R U . . .
H10C H 0.049631 0.594063 0.236413 0.044 Uiso 1 1 calc R U . . .
C11 C 0.3413(3) 1.0261(5) 0.4501(3) 0.0160(7) Uani 1 1 d . . . . .
N12 N 0.3406(2) 1.0228(4) 0.5311(2) 0.0147(6) Uani 1 1 d . . . . .
C13 C 0.4073(2) 1.1262(4) 0.5949(2) 0.0129(7) Uani 1 1 d . . . . .
C14 C 0.4263(3) 1.1525(5) 0.6873(3) 0.0202(8) Uani 1 1 d . . . . .
H14 H 0.391479 1.098741 0.713312 0.024 Uiso 1 1 calc R U . . .
C15 C 0.4967(3) 1.2583(5) 0.7396(3) 0.0244(9) Uani 1 1 d . . . . .
H15 H 0.510240 1.277927 0.802254 0.029 Uiso 1 1 calc R U . . .
C16 C 0.5484(3) 1.3370(5) 0.7025(3) 0.0249(9) Uani 1 1 d . . . . .
H16 H 0.597444 1.407278 0.740951 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5305(3) 1.3156(5) 0.6119(3) 0.0225(9) Uani 1 1 d . . . . .
H17 H 0.565335 1.371560 0.586778 0.027 Uiso 1 1 calc R U . . .
C18 C 0.4592(3) 1.2086(5) 0.5577(3) 0.0171(8) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Ta1 N12 2.280(3) . ?
Ta1 Cl3 2.3978(9) . ?
Ta1 Cl2 2.4068(9) . ?
Ta1 Cl1 2.4143(9) . ?
Ta1 C3 2.450(4) . ?
Ta1 C4 2.461(4) . ?
Ta1 C5 2.466(4) . ?
Ta1 C2 2.467(4) . ?
Ta1 C1 2.500(4) . ?
Ta1 S1 2.5172(9) . ?
S1 C11 1.723(4) . ?
S2 C11 1.731(4) . ?
S2 C18 1.741(4) . ?
C1 C2 1.417(6) . ?
C1 C5 1.430(6) . ?
C1 C6 1.494(6) . ?
C2 C3 1.431(5) . ?
C2 C7 1.495(6) . ?
C3 C4 1.427(5) . ?
C3 C8 1.499(5) . ?
C4 C5 1.424(5) . ?
C4 C9 1.492(5) . ?
C5 C10 1.499(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N12 1.316(5) . ?
N12 C13 1.394(5) . ?
C13 C14 1.401(5) . ?
C13 C18 1.410(5) . ?
C14 C15 1.377(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.371(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(5) . ?
C17 H17 0.9500 . ?

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
N12 Ta1 Cl3 85.57(8) . . ?
N12 Ta1 Cl2 77.15(8) . . ?
Cl3 Ta1 Cl2 85.88(3) . . ?
N12 Ta1 Cl1 75.69(8) . . ?
Cl3 Ta1 Cl1 86.16(4) . . ?
Cl2 Ta1 Cl1 152.18(3) . . ?
N12 Ta1 C3 155.79(12) . . ?
Cl3 Ta1 C3 85.16(9) . . ?
Cl2 Ta1 C3 124.32(9) . . ?
Cl1 Ta1 C3 81.41(9) . . ?
N12 Ta1 C4 142.80(12) . . ?
Cl3 Ta1 C4 118.11(9) . . ?
Cl2 Ta1 C4 129.16(9) . . ?
Cl1 Ta1 C4 77.72(9) . . ?
C3 Ta1 C4 33.80(12) . . ?
N12 Ta1 C5 139.37(12) . . ?
Cl3 Ta1 C5 134.63(10) . . ?
Cl2 Ta1 C5 97.07(10) . . ?
Cl1 Ta1 C5 107.41(10) . . ?
C3 Ta1 C5 55.93(13) . . ?
C4 Ta1 C5 33.61(12) . . ?
N12 Ta1 C2 161.10(12) . . ?
Cl3 Ta1 C2 79.21(10) . . ?
Cl2 Ta1 C2 90.53(9) . . ?
Cl1 Ta1 C2 114.02(10) . . ?
C3 Ta1 C2 33.84(12) . . ?
C4 Ta1 C2 55.86(12) . . ?
C5 Ta1 C2 55.56(13) . . ?
N12 Ta1 C1 148.55(12) . . ?
Cl3 Ta1 C1 107.10(10) . . ?
Cl2 Ta1 C1 75.27(9) . . ?
Cl1 Ta1 C1 132.51(10) . . ?
C3 Ta1 C1 55.63(13) . . ?
C4 Ta1 C1 55.57(12) . . ?
C5 Ta1 C1 33.46(13) . . ?
C2 Ta1 C1 33.14(13) . . ?
N12 Ta1 S1 64.58(8) . . ?
Cl3 Ta1 S1 150.14(3) . . ?
Cl2 Ta1 S1 86.81(3) . . ?
Cl1 Ta1 S1 86.95(3) . . ?
C3 Ta1 S1 122.39(9) . . ?
C4 Ta1 S1 88.59(9) . . ?
C5 Ta1 S1 75.04(10) . . ?
C2 Ta1 S1 129.79(10) . . ?
C1 Ta1 S1 98.92(10) . . ?
C11 S1 Ta1 80.90(13) . . ?
C11 S2 C18 88.89(18) . . ?
C2 C1 C5 107.8(3) . . ?
C2 C1 C6 126.6(4) . . ?
C5 C1 C6 124.8(4) . . ?
C2 C1 Ta1 72.2(2) . . ?
C5 C1 Ta1 72.0(2) . . ?
C6 C1 Ta1 129.7(3) . . ?
C1 C2 C3 108.4(3) . . ?
C1 C2 C7 124.9(4) . . ?
C3 C2 C7 126.3(4) . . ?
C1 C2 Ta1 74.7(2) . . ?
C3 C2 Ta1 72.4(2) . . ?
C7 C2 Ta1 125.1(3) . . ?
C4 C3 C2 107.7(3) . . ?
C4 C3 C8 126.9(3) . . ?
C2 C3 C8 125.2(3) . . ?
C4 C3 Ta1 73.5(2) . . ?
C2 C3 Ta1 73.7(2) . . ?
C8 C3 Ta1 122.7(3) . . ?
C5 C4 C3 107.9(3) . . ?
C5 C4 C9 125.0(4) . . ?
C3 C4 C9 126.7(4) . . ?
C5 C4 Ta1 73.4(2) . . ?
C3 C4 Ta1 72.7(2) . . ?
C9 C4 Ta1 125.3(3) . . ?
C4 C5 C1 108.2(3) . . ?
C4 C5 C10 125.1(4) . . ?
C1 C5 C10 125.5(4) . . ?
C4 C5 Ta1 73.0(2) . . ?
C1 C5 Ta1 74.6(2) . . ?
C10 C5 Ta1 128.0(3) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N12 C11 S1 114.9(3) . . ?
N12 C11 S2 115.7(3) . . ?
S1 C11 S2 129.4(2) . . ?
C11 N12 C13 111.9(3) . . ?
C11 N12 Ta1 99.6(2) . . ?
C13 N12 Ta1 148.1(3) . . ?
N12 C13 C14 127.4(3) . . ?
N12 C13 C18 112.7(3) . . ?
C14 C13 C18 119.8(3) . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 121.4(4) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 121.6(4) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 117.8(4) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
C17 C18 C13 121.1(4) . . ?
C17 C18 S2 128.2(3) . . ?
C13 C18 S2 110.8(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
C5 C1 C2 C3 -1.5(4) . . . . ?
C6 C1 C2 C3 168.2(4) . . . . ?
Ta1 C1 C2 C3 -65.1(3) . . . . ?
C5 C1 C2 C7 -174.0(4) . . . . ?
C6 C1 C2 C7 -4.3(6) . . . . ?
Ta1 C1 C2 C7 122.4(4) . . . . ?
C5 C1 C2 Ta1 63.6(3) . . . . ?
C6 C1 C2 Ta1 -126.7(4) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C7 C2 C3 C4 172.8(4) . . . . ?
Ta1 C2 C3 C4 -66.2(3) . . . . ?
C1 C2 C3 C8 -174.5(4) . . . . ?
C7 C2 C3 C8 -2.1(6) . . . . ?
Ta1 C2 C3 C8 118.9(4) . . . . ?
C1 C2 C3 Ta1 66.6(3) . . . . ?
C7 C2 C3 Ta1 -121.0(4) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C8 C3 C4 C5 175.7(4) . . . . ?
Ta1 C3 C4 C5 -65.5(3) . . . . ?
C2 C3 C4 C9 -172.2(4) . . . . ?
C8 C3 C4 C9 2.6(6) . . . . ?
Ta1 C3 C4 C9 121.5(4) . . . . ?
C2 C3 C4 Ta1 66.4(3) . . . . ?
C8 C3 C4 Ta1 -118.8(4) . . . . ?
C3 C4 C5 C1 -1.8(4) . . . . ?
C9 C4 C5 C1 171.4(4) . . . . ?
Ta1 C4 C5 C1 -66.8(3) . . . . ?
C3 C4 C5 C10 -170.1(4) . . . . ?
C9 C4 C5 C10 3.1(6) . . . . ?
Ta1 C4 C5 C10 124.9(4) . . . . ?
C3 C4 C5 Ta1 65.0(3) . . . . ?
C9 C4 C5 Ta1 -121.8(4) . . . . ?
C2 C1 C5 C4 2.0(4) . . . . ?
C6 C1 C5 C4 -167.9(4) . . . . ?
Ta1 C1 C5 C4 65.8(3) . . . . ?
C2 C1 C5 C10 170.2(4) . . . . ?
C6 C1 C5 C10 0.3(6) . . . . ?
Ta1 C1 C5 C10 -126.0(4) . . . . ?
C2 C1 C5 Ta1 -63.7(3) . . . . ?
C6 C1 C5 Ta1 126.3(4) . . . . ?
Ta1 S1 C11 N12 -2.3(3) . . . . ?
Ta1 S1 C11 S2 175.2(3) . . . . ?
C18 S2 C11 N12 0.5(3) . . . . ?
C18 S2 C11 S1 -177.0(3) . . . . ?
S1 C11 N12 C13 177.6(3) . . . . ?
S2 C11 N12 C13 -0.3(4) . . . . ?
S1 C11 N12 Ta1 2.5(3) . . . . ?
S2 C11 N12 Ta1 -175.35(19) . . . . ?
C11 N12 C13 C14 -179.7(4) . . . . ?
Ta1 N12 C13 C14 -8.9(7) . . . . ?
C11 N12 C13 C18 -0.2(5) . . . . ?
Ta1 N12 C13 C18 170.6(3) . . . . ?
N12 C13 C14 C15 178.8(4) . . . . ?
C18 C13 C14 C15 -0.6(6) . . . . ?
C13 C14 C15 C16 -0.4(6) . . . . ?
C14 C15 C16 C17 1.4(7) . . . . ?
C15 C16 C17 C18 -1.4(6) . . . . ?
C16 C17 C18 C13 0.3(6) . . . . ?
C16 C17 C18 S2 -179.0(3) . . . . ?
N12 C13 C18 C17 -178.9(3) . . . . ?
C14 C13 C18 C17 0.6(6) . . . . ?
N12 C13 C18 S2 0.6(4) . . . . ?
C14 C13 C18 S2 -179.9(3) . . . . ?
C11 S2 C18 C17 178.8(4) . . . . ?
C11 S2 C18 C13 -0.6(3) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_SGGAH11
_audit_block_doi                 10.5517/ccdc.csd.cc26s6dm
_database_code_depnum_ccdc_archive 'CCDC 2049050'
loop_
_audit_author_name
_audit_author_address
'Thierry ROISNEL'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2020-12-08 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 25 septembre 2019                                        #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C26 H46 B4 Nb2 Se'
_chemical_formula_sum            'C26 H46 B4 Nb2 Se'
_chemical_formula_weight         666.65
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'


_diffrn_orient_matrix_UB_11      0.0423051
_diffrn_orient_matrix_UB_21      -0.0484156
_diffrn_orient_matrix_UB_31      -0.1129327
_diffrn_orient_matrix_UB_12      0.0488540
_diffrn_orient_matrix_UB_22      -0.0892164
_diffrn_orient_matrix_UB_32      0.0203906
_diffrn_orient_matrix_UB_13      -0.0383333
_diffrn_orient_matrix_UB_23      -0.0376016
_diffrn_orient_matrix_UB_33      -0.0069685

_cell_length_a                   8.0962(8)
_cell_length_b                   10.3403(11)
_cell_length_c                   19.0685(19)
_cell_angle_alpha                101.994(3)
_cell_angle_beta                 94.204(3)
_cell_angle_gamma                106.275(4)
_cell_volume                     1484.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    9736
_cell_measurement_theta_min      2.6063
_cell_measurement_theta_max      27.5052
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.070
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             676
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.869

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_reflns_av_r_equivalents  0.0320
_diffrn_reflns_av_uneti/neti     0.0315
_diffrn_reflns_number            26480
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.113
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             6760
_reflns_number_gt                6181
_reflns_threshold_expression     >2sigma(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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²+1.3288P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6760
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0590
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.081

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Se Se -0.0929 2.2259 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Nb1 Nb 0.46774(2) 0.59978(2) 0.76209(2) 0.01372(5) Uani 1 1 d . . . . .
C1 C 0.7137(3) 0.7086(2) 0.85537(11) 0.0228(4) Uani 1 1 d . . . . .
C2 C 0.7267(3) 0.7865(2) 0.80102(10) 0.0204(4) Uani 1 1 d . . . . .
C3 C 0.5870(3) 0.84467(19) 0.80169(10) 0.0194(4) Uani 1 1 d . . . . .
C4 C 0.4859(3) 0.8009(2) 0.85547(10) 0.0202(4) Uani 1 1 d . . . . .
C5 C 0.5646(3) 0.7162(2) 0.88834(10) 0.0226(4) Uani 1 1 d . . . . .
C6 C 0.8432(4) 0.6401(3) 0.87754(15) 0.0404(6) Uani 1 1 d . . . . .
H6A H 0.932845 0.706512 0.915523 0.061 Uiso 1 1 calc R U . . .
H6B H 0.897280 0.608788 0.835561 0.061 Uiso 1 1 calc R U . . .
H6C H 0.783837 0.560150 0.895983 0.061 Uiso 1 1 calc R U . . .
C7 C 0.8751(3) 0.8188(2) 0.75777(13) 0.0315(5) Uani 1 1 d . . . . .
H7A H 0.832471 0.832509 0.711259 0.047 Uiso 1 1 calc R U . . .
H7B H 0.924426 0.741450 0.749192 0.047 Uiso 1 1 calc R U . . .
H7C H 0.964838 0.903462 0.784720 0.047 Uiso 1 1 calc R U . . .
C8 C 0.5577(4) 0.9433(2) 0.75764(12) 0.0309(5) Uani 1 1 d . . . . .
H8A H 0.639838 1.035819 0.778278 0.046 Uiso 1 1 calc R U . . .
H8B H 0.438550 0.947998 0.758381 0.046 Uiso 1 1 calc R U . . .
H8C H 0.575519 0.910462 0.707584 0.046 Uiso 1 1 calc R U . . .
C9 C 0.3372(3) 0.8501(3) 0.87974(13) 0.0334(5) Uani 1 1 d . . . . .
H9A H 0.381664 0.934767 0.918657 0.050 Uiso 1 1 calc R U . . .
H9B H 0.256835 0.778038 0.897567 0.050 Uiso 1 1 calc R U . . .
H9C H 0.275925 0.869773 0.838866 0.050 Uiso 1 1 calc R U . . .
C10 C 0.5051(4) 0.6540(3) 0.95024(12) 0.0394(6) Uani 1 1 d . . . . .
H10A H 0.531162 0.565945 0.945889 0.059 Uiso 1 1 calc R U . . .
H10B H 0.379518 0.637553 0.949008 0.059 Uiso 1 1 calc R U . . .
H10C H 0.565713 0.718154 0.996158 0.059 Uiso 1 1 calc R U . . .
Nb2 Nb 0.25805(2) 0.35666(2) 0.64781(2) 0.01339(5) Uani 1 1 d . . . . .
C11 C 0.1483(3) 0.1124(2) 0.60320(11) 0.0243(4) Uani 1 1 d . . . . .
C12 C 0.2394(3) 0.1655(2) 0.54905(11) 0.0237(4) Uani 1 1 d . . . . .
C13 C 0.1492(3) 0.2483(2) 0.52100(10) 0.0200(4) Uani 1 1 d . . . . .
C14 C 0.0037(3) 0.2479(2) 0.55807(10) 0.0208(4) Uani 1 1 d . . . . .
C15 C 0.0037(3) 0.1648(2) 0.60958(11) 0.0235(4) Uani 1 1 d . . . . .
C16 C 0.1924(4) 0.0113(2) 0.64194(14) 0.0394(6) Uani 1 1 d . . . . .
H16A H 0.135103 -0.083533 0.613355 0.059 Uiso 1 1 calc R U . . .
H16B H 0.152401 0.023157 0.689464 0.059 Uiso 1 1 calc R U . . .
H16C H 0.318557 0.028472 0.648271 0.059 Uiso 1 1 calc R U . . .
C17 C 0.3906(4) 0.1268(3) 0.52036(14) 0.0398(6) Uani 1 1 d . . . . .
H17A H 0.468485 0.120069 0.560368 0.060 Uiso 1 1 calc R U . . .
H17B H 0.453842 0.197887 0.496945 0.060 Uiso 1 1 calc R U . . .
H17C H 0.348615 0.037129 0.484966 0.060 Uiso 1 1 calc R U . . .
C18 C 0.1937(3) 0.3173(3) 0.45943(12) 0.0342(5) Uani 1 1 d . . . . .
H18A H 0.121573 0.258400 0.414350 0.051 Uiso 1 1 calc R U . . .
H18B H 0.316626 0.330868 0.454422 0.051 Uiso 1 1 calc R U . . .
H18C H 0.171771 0.407449 0.469575 0.051 Uiso 1 1 calc R U . . .
C19 C -0.1315(3) 0.3156(3) 0.54220(14) 0.0359(5) Uani 1 1 d . . . . .
H19A H -0.075884 0.403789 0.530044 0.054 Uiso 1 1 calc R U . . .
H19B H -0.189676 0.332990 0.584915 0.054 Uiso 1 1 calc R U . . .
H19C H -0.217210 0.254414 0.501279 0.054 Uiso 1 1 calc R U . . .
C20 C -0.1346(3) 0.1277(3) 0.65699(13) 0.0391(6) Uani 1 1 d . . . . .
H20A H -0.188984 0.201848 0.667583 0.059 Uiso 1 1 calc R U . . .
H20B H -0.081921 0.116385 0.702372 0.059 Uiso 1 1 calc R U . . .
H20C H -0.222927 0.040679 0.631846 0.059 Uiso 1 1 calc R U . . .
Se1 Se 0.33751(3) 0.24009(2) 0.84167(2) 0.02312(6) Uani 1 1 d . . . . .
C21 C 0.1177(3) 0.2195(2) 0.87688(10) 0.0216(4) Uani 1 1 d . . . . .
C22 C 0.0109(3) 0.3002(2) 0.86670(13) 0.0311(5) Uani 1 1 d . . . . .
H22 H 0.047600 0.372919 0.842629 0.037 Uiso 1 1 calc R U . . .
C23 C -0.1503(4) 0.2749(3) 0.89170(15) 0.0368(6) Uani 1 1 d . . . . .
H23 H -0.223617 0.329385 0.883849 0.044 Uiso 1 1 calc R U . . .
C24 C -0.2038(3) 0.1703(3) 0.92799(12) 0.0325(5) Uani 1 1 d . . . . .
H24 H -0.312667 0.154120 0.945622 0.039 Uiso 1 1 calc R U . . .
C25 C -0.0982(3) 0.0904(2) 0.93826(12) 0.0299(5) Uani 1 1 d . . . . .
H25 H -0.134877 0.018132 0.962652 0.036 Uiso 1 1 calc R U . . .
C26 C 0.0613(3) 0.1146(2) 0.91325(11) 0.0258(4) Uani 1 1 d . . . . .
H26 H 0.133308 0.059019 0.920950 0.031 Uiso 1 1 calc R U . . .
B31 B 0.3363(3) 0.3669(2) 0.77358(11) 0.0170(4) Uani 1 1 d . . . . .
H31A H 0.200(3) 0.323(2) 0.7371(12) 0.020 Uiso 1 1 d . U . . .
H31B H 0.334(3) 0.479(2) 0.8111(12) 0.020 Uiso 1 1 d . U . . .
B32 B 0.5183(3) 0.3769(2) 0.72589(12) 0.0189(4) Uani 1 1 d . . . . .
H32A H 0.600(3) 0.316(2) 0.7414(13) 0.023 Uiso 1 1 d . U . . .
H32B H 0.617(3) 0.493(2) 0.7331(13) 0.023 Uiso 1 1 d . U . . .
H32C H 0.486(3) 0.339(2) 0.6613(13) 0.023 Uiso 1 1 d . U . . .
B33 B 0.2073(3) 0.5780(2) 0.68494(12) 0.0208(4) Uani 1 1 d . . . . .
H33A H 0.130(3) 0.640(3) 0.6689(13) 0.025 Uiso 1 1 d . U . . .
H33B H 0.109(3) 0.463(3) 0.6786(13) 0.025 Uiso 1 1 d . U . . .
H33C H 0.240(3) 0.619(2) 0.7500(13) 0.025 Uiso 1 1 d . U . . .
B34 B 0.3901(3) 0.5892(2) 0.63616(12) 0.0211(4) Uani 1 1 d . . . . .
H34A H 0.395(3) 0.655(3) 0.5990(13) 0.025 Uiso 1 1 d . U . . .
H34C H 0.403(3) 0.476(3) 0.5994(13) 0.025 Uiso 1 1 d . U . . .
H34B H 0.531(3) 0.635(2) 0.6741(13) 0.025 Uiso 1 1 d . U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Nb1 C2 2.362(2) . ?
Nb1 C3 2.3755(19) . ?
Nb1 C4 2.4016(19) . ?
Nb1 C1 2.406(2) . ?
Nb1 B31 2.407(2) . ?
Nb1 B33 2.409(2) . ?
Nb1 B34 2.409(2) . ?
Nb1 C5 2.4186(19) . ?
Nb1 B32 2.422(2) . ?
Nb1 Nb2 2.9563(3) . ?
Nb1 H31B 1.87(2) . ?
Nb1 H32B 1.89(2) . ?
Nb1 H33C 1.92(3) . ?
Nb1 H34B 1.87(2) . ?
C1 C5 1.415(3) . ?
C1 C2 1.431(3) . ?
C1 C6 1.502(3) . ?
C2 C3 1.422(3) . ?
C2 C7 1.507(3) . ?
C3 C4 1.427(3) . ?
C3 C8 1.505(3) . ?
C4 C5 1.431(3) . ?
C4 C9 1.500(3) . ?
C5 C10 1.505(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Nb2 C15 2.365(2) . ?
Nb2 C11 2.373(2) . ?
Nb2 C12 2.392(2) . ?
Nb2 B34 2.406(2) . ?
Nb2 B31 2.408(2) . ?
Nb2 B33 2.410(2) . ?
Nb2 C14 2.412(2) . ?
Nb2 B32 2.422(2) . ?
Nb2 C13 2.4263(19) . ?
Nb2 H31A 1.87(2) . ?
Nb2 H32C 1.91(3) . ?
Nb2 H33B 1.90(3) . ?
Nb2 H34C 1.89(2) . ?
C11 C15 1.424(3) . ?
C11 C12 1.425(3) . ?
C11 C16 1.502(3) . ?
C12 C13 1.427(3) . ?
C12 C17 1.497(3) . ?
C13 C14 1.418(3) . ?
C13 C18 1.511(3) . ?
C14 C15 1.433(3) . ?
C14 C19 1.500(3) . ?
C15 C20 1.507(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Se1 C21 1.920(2) . ?
Se1 B31 2.030(2) . ?
C21 C22 1.389(3) . ?
C21 C26 1.395(3) . ?
C22 C23 1.396(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
B31 B32 1.778(3) . ?
B31 H31A 1.18(2) . ?
B31 H31B 1.23(2) . ?
B32 H32A 1.10(2) . ?
B32 H32B 1.21(2) . ?
B32 H32C 1.20(2) . ?
B33 B34 1.794(3) . ?
B33 H33A 1.08(3) . ?
B33 H33B 1.21(2) . ?
B33 H33C 1.21(2) . ?
B34 H34A 1.07(2) . ?
B34 H34C 1.27(2) . ?
B34 H34B 1.22(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
C2 Nb1 C3 34.92(7) . . ?
C2 Nb1 C4 57.76(7) . . ?
C3 Nb1 C4 34.75(6) . . ?
C2 Nb1 C1 34.91(7) . . ?
C3 Nb1 C1 57.74(7) . . ?
C4 Nb1 C1 57.20(7) . . ?
C2 Nb1 B31 140.99(7) . . ?
C3 Nb1 B31 156.56(7) . . ?
C4 Nb1 B31 122.67(7) . . ?
C1 Nb1 B31 108.27(7) . . ?
C2 Nb1 B33 130.67(8) . . ?
C3 Nb1 B33 101.38(7) . . ?
C4 Nb1 B33 101.45(8) . . ?
C1 Nb1 B33 157.67(7) . . ?
B31 Nb1 B33 88.35(8) . . ?
C2 Nb1 B34 105.53(7) . . ?
C3 Nb1 B34 97.39(7) . . ?
C4 Nb1 B34 121.68(8) . . ?
C1 Nb1 B34 138.67(8) . . ?
B31 Nb1 B34 104.22(7) . . ?
B33 Nb1 B34 43.73(8) . . ?
C2 Nb1 C5 57.63(7) . . ?
C3 Nb1 C5 57.69(7) . . ?
C4 Nb1 C5 34.55(7) . . ?
C1 Nb1 C5 34.11(8) . . ?
B31 Nb1 C5 99.81(7) . . ?
B33 Nb1 C5 130.29(8) . . ?
B34 Nb1 C5 154.64(7) . . ?
C2 Nb1 B32 113.20(8) . . ?
C3 Nb1 B32 147.97(8) . . ?
C4 Nb1 B32 149.28(7) . . ?
C1 Nb1 B32 97.78(7) . . ?
B31 Nb1 B32 43.21(8) . . ?
B33 Nb1 B32 104.55(8) . . ?
B34 Nb1 B32 88.70(8) . . ?
C5 Nb1 B32 114.76(7) . . ?
C2 Nb1 Nb2 148.35(5) . . ?
C3 Nb1 Nb2 148.33(5) . . ?
C4 Nb1 Nb2 149.99(5) . . ?
C1 Nb1 Nb2 150.16(5) . . ?
B31 Nb1 Nb2 52.13(5) . . ?
B33 Nb1 Nb2 52.17(5) . . ?
B34 Nb1 Nb2 52.08(5) . . ?
C5 Nb1 Nb2 150.95(5) . . ?
B32 Nb1 Nb2 52.39(5) . . ?
C2 Nb1 H31B 131.8(7) . . ?
C3 Nb1 H31B 127.6(7) . . ?
C4 Nb1 H31B 92.9(7) . . ?
C1 Nb1 H31B 97.9(7) . . ?
B31 Nb1 H31B 30.3(7) . . ?
B33 Nb1 H31B 89.1(8) . . ?
B34 Nb1 H31B 122.7(7) . . ?
C5 Nb1 H31B 76.4(7) . . ?
B32 Nb1 H31B 71.6(7) . . ?
Nb2 Nb1 H31B 74.7(7) . . ?
C2 Nb1 H32B 85.0(8) . . ?
C3 Nb1 H32B 119.0(8) . . ?
C4 Nb1 H32B 136.0(8) . . ?
C1 Nb1 H32B 78.9(7) . . ?
B31 Nb1 H32B 71.3(7) . . ?
B33 Nb1 H32B 121.5(7) . . ?
B34 Nb1 H32B 88.1(7) . . ?
C5 Nb1 H32B 107.4(7) . . ?
B32 Nb1 H32B 29.5(7) . . ?
Nb2 Nb1 H32B 73.4(7) . . ?
H31B Nb1 H32B 96.5(10) . . ?
C2 Nb1 H33C 124.6(7) . . ?
C3 Nb1 H33C 89.7(7) . . ?
C4 Nb1 H33C 76.5(7) . . ?
C1 Nb1 H33C 132.9(7) . . ?
B31 Nb1 H33C 88.4(7) . . ?
B33 Nb1 H33C 29.7(7) . . ?
B34 Nb1 H33C 71.9(7) . . ?
C5 Nb1 H33C 101.0(7) . . ?
B32 Nb1 H33C 121.9(7) . . ?
Nb2 Nb1 H33C 73.9(7) . . ?
H31B Nb1 H33C 74.6(10) . . ?
H32B Nb1 H33C 147.3(11) . . ?
C2 Nb1 H34B 78.4(8) . . ?
C3 Nb1 H34B 82.1(8) . . ?
C4 Nb1 H34B 115.4(8) . . ?
C1 Nb1 H34B 109.3(8) . . ?
B31 Nb1 H34B 121.3(8) . . ?
B33 Nb1 H34B 72.1(8) . . ?
B34 Nb1 H34B 29.8(8) . . ?
C5 Nb1 H34B 135.3(8) . . ?
B32 Nb1 H34B 88.2(8) . . ?
Nb2 Nb1 H34B 73.5(8) . . ?
H31B Nb1 H34B 148.2(11) . . ?
H32B Nb1 H34B 73.5(11) . . ?
H33C Nb1 H34B 97.3(11) . . ?
C5 C1 C2 108.15(18) . . ?
C5 C1 C6 125.8(2) . . ?
C2 C1 C6 125.9(2) . . ?
C5 C1 Nb1 73.44(12) . . ?
C2 C1 Nb1 70.87(11) . . ?
C6 C1 Nb1 124.96(14) . . ?
C3 C2 C1 108.07(18) . . ?
C3 C2 C7 125.09(19) . . ?
C1 C2 C7 126.3(2) . . ?
C3 C2 Nb1 73.05(11) . . ?
C1 C2 Nb1 74.21(11) . . ?
C7 C2 Nb1 125.09(14) . . ?
C2 C3 C4 107.78(17) . . ?
C2 C3 C8 126.36(19) . . ?
C4 C3 C8 125.7(2) . . ?
C2 C3 Nb1 72.03(11) . . ?
C4 C3 Nb1 73.63(11) . . ?
C8 C3 Nb1 123.37(14) . . ?
C3 C4 C5 108.06(19) . . ?
C3 C4 C9 125.6(2) . . ?
C5 C4 C9 125.86(19) . . ?
C3 C4 Nb1 71.62(11) . . ?
C5 C4 Nb1 73.38(11) . . ?
C9 C4 Nb1 126.65(15) . . ?
C1 C5 C4 107.91(17) . . ?
C1 C5 C10 126.3(2) . . ?
C4 C5 C10 125.7(2) . . ?
C1 C5 Nb1 72.45(11) . . ?
C4 C5 Nb1 72.08(11) . . ?
C10 C5 Nb1 124.06(15) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C15 Nb2 C11 34.98(8) . . ?
C15 Nb2 C12 57.82(8) . . ?
C11 Nb2 C12 34.81(7) . . ?
C15 Nb2 B34 142.75(8) . . ?
C11 Nb2 B34 153.68(7) . . ?
C12 Nb2 B34 119.20(8) . . ?
C15 Nb2 B31 104.74(7) . . ?
C11 Nb2 B31 99.30(7) . . ?
C12 Nb2 B31 125.28(7) . . ?
B34 Nb2 B31 104.29(7) . . ?
C15 Nb2 B33 114.84(8) . . ?
C11 Nb2 B33 149.81(8) . . ?
C12 Nb2 B33 146.20(7) . . ?
B34 Nb2 B33 43.75(8) . . ?
B31 Nb2 B33 88.32(7) . . ?
C15 Nb2 C14 34.88(7) . . ?
C11 Nb2 C14 57.78(7) . . ?
C12 Nb2 C14 57.24(7) . . ?
B34 Nb2 C14 109.08(7) . . ?
B31 Nb2 C14 136.69(7) . . ?
B33 Nb2 C14 97.05(8) . . ?
C15 Nb2 B32 128.48(8) . . ?
C11 Nb2 B32 100.81(8) . . ?
C12 Nb2 B32 103.57(7) . . ?
B34 Nb2 B32 88.76(8) . . ?
B31 Nb2 B32 43.20(8) . . ?
B33 Nb2 B32 104.53(8) . . ?
C14 Nb2 B32 158.26(7) . . ?
C15 Nb2 C13 57.49(7) . . ?
C11 Nb2 C13 57.57(7) . . ?
C12 Nb2 C13 34.44(7) . . ?
B34 Nb2 C13 98.25(7) . . ?
B31 Nb2 C13 156.87(7) . . ?
B33 Nb2 C13 112.00(7) . . ?
C14 Nb2 C13 34.07(7) . . ?
B32 Nb2 C13 133.66(7) . . ?
C15 Nb2 Nb1 148.74(5) . . ?
C11 Nb2 Nb1 149.56(5) . . ?
C12 Nb2 Nb1 150.36(5) . . ?
B34 Nb2 Nb1 52.17(5) . . ?
B31 Nb2 Nb1 52.11(5) . . ?
B33 Nb2 Nb1 52.15(6) . . ?
C14 Nb2 Nb1 149.13(5) . . ?
B32 Nb2 Nb1 52.38(5) . . ?
C13 Nb2 Nb1 150.06(5) . . ?
C15 Nb2 H31A 79.1(7) . . ?
C11 Nb2 H31A 85.6(7) . . ?
C12 Nb2 H31A 119.5(7) . . ?
B34 Nb2 H31A 120.7(7) . . ?
B31 Nb2 H31A 28.7(8) . . ?
B33 Nb2 H31A 87.6(7) . . ?
C14 Nb2 H31A 108.4(8) . . ?
B32 Nb2 H31A 70.5(8) . . ?
C13 Nb2 H31A 136.5(8) . . ?
Nb1 Nb2 H31A 72.5(7) . . ?
C15 Nb2 H32C 123.5(7) . . ?
C11 Nb2 H32C 88.8(7) . . ?
C12 Nb2 H32C 78.6(7) . . ?
B34 Nb2 H32C 88.0(7) . . ?
B31 Nb2 H32C 71.0(7) . . ?
B33 Nb2 H32C 121.2(7) . . ?
C14 Nb2 H32C 135.7(7) . . ?
B32 Nb2 H32C 29.1(7) . . ?
C13 Nb2 H32C 105.0(7) . . ?
Nb1 Nb2 H32C 73.0(7) . . ?
H31A Nb2 H32C 95.7(10) . . ?
C15 Nb2 H33B 86.5(8) . . ?
C11 Nb2 H33B 121.1(8) . . ?
C12 Nb2 H33B 135.0(8) . . ?
B34 Nb2 H33B 72.1(7) . . ?
B31 Nb2 H33B 87.2(7) . . ?
B33 Nb2 H33B 29.6(7) . . ?
C14 Nb2 H33B 77.8(8) . . ?
B32 Nb2 H33B 120.7(8) . . ?
C13 Nb2 H33B 104.9(7) . . ?
Nb1 Nb2 H33B 73.0(8) . . ?
H31A Nb2 H33B 73.0(10) . . ?
H32C Nb2 H33B 146.1(11) . . ?
C15 Nb2 H34C 133.8(8) . . ?
C11 Nb2 H34C 123.7(7) . . ?
C12 Nb2 H34C 88.9(7) . . ?
B34 Nb2 H34C 31.6(8) . . ?
B31 Nb2 H34C 121.1(8) . . ?
B33 Nb2 H34C 74.1(8) . . ?
C14 Nb2 H34C 101.5(8) . . ?
B32 Nb2 H34C 87.1(8) . . ?
C13 Nb2 H34C 76.8(7) . . ?
Nb1 Nb2 H34C 74.3(8) . . ?
H31A Nb2 H34C 146.7(11) . . ?
H32C Nb2 H34C 71.8(10) . . ?
H33B Nb2 H34C 99.9(11) . . ?
C15 C11 C12 107.67(18) . . ?
C15 C11 C16 127.0(2) . . ?
C12 C11 C16 125.2(2) . . ?
C15 C11 Nb2 72.23(11) . . ?
C12 C11 Nb2 73.32(11) . . ?
C16 C11 Nb2 123.35(15) . . ?
C11 C12 C13 108.29(19) . . ?
C11 C12 C17 125.6(2) . . ?
C13 C12 C17 125.7(2) . . ?
C11 C12 Nb2 71.87(11) . . ?
C13 C12 Nb2 74.11(11) . . ?
C17 C12 Nb2 125.50(15) . . ?
C14 C13 C12 108.01(18) . . ?
C14 C13 C18 125.6(2) . . ?
C12 C13 C18 126.3(2) . . ?
C14 C13 Nb2 72.43(11) . . ?
C12 C13 Nb2 71.45(11) . . ?
C18 C13 Nb2 124.65(14) . . ?
C13 C14 C15 107.94(19) . . ?
C13 C14 C19 125.35(19) . . ?
C15 C14 C19 126.6(2) . . ?
C13 C14 Nb2 73.50(11) . . ?
C15 C14 Nb2 70.76(11) . . ?
C19 C14 Nb2 124.28(15) . . ?
C11 C15 C14 108.08(18) . . ?
C11 C15 C20 125.7(2) . . ?
C14 C15 C20 126.0(2) . . ?
C11 C15 Nb2 72.79(11) . . ?
C14 C15 Nb2 74.36(11) . . ?
C20 C15 Nb2 123.27(15) . . ?
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 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 Se1 B31 103.19(9) . . ?
C22 C21 C26 118.6(2) . . ?
C22 C21 Se1 123.90(16) . . ?
C26 C21 Se1 117.51(17) . . ?
C21 C22 C23 120.2(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 121.0(2) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
B32 B31 Se1 108.99(13) . . ?
B32 B31 Nb1 68.83(10) . . ?
Se1 B31 Nb1 142.14(10) . . ?
B32 B31 Nb2 68.82(10) . . ?
Se1 B31 Nb2 140.59(10) . . ?
Nb1 B31 Nb2 75.76(6) . . ?
B32 B31 H31A 115.3(12) . . ?
Se1 B31 H31A 106.7(11) . . ?
Nb1 B31 H31A 107.9(11) . . ?
Nb2 B31 H31A 49.7(11) . . ?
B32 B31 H31B 114.6(12) . . ?
Se1 B31 H31B 106.6(11) . . ?
Nb1 B31 H31B 49.9(11) . . ?
Nb2 B31 H31B 109.7(11) . . ?
H31A B31 H31B 104.1(17) . . ?
B31 B32 Nb1 67.96(10) . . ?
B31 B32 Nb2 67.98(10) . . ?
Nb1 B32 Nb2 75.23(7) . . ?
B31 B32 H32A 113.2(13) . . ?
Nb1 B32 H32A 142.1(13) . . ?
Nb2 B32 H32A 142.1(13) . . ?
B31 B32 H32B 115.3(12) . . ?
Nb1 B32 H32B 50.3(12) . . ?
Nb2 B32 H32B 107.9(12) . . ?
H32A B32 H32B 105.1(18) . . ?
B31 B32 H32C 115.9(12) . . ?
Nb1 B32 H32C 108.0(12) . . ?
Nb2 B32 H32C 50.9(12) . . ?
H32A B32 H32C 104.9(17) . . ?
H32B B32 H32C 101.1(16) . . ?
B34 B33 Nb1 68.14(11) . . ?
B34 B33 Nb2 68.02(11) . . ?
Nb1 B33 Nb2 75.68(7) . . ?
B34 B33 H33A 110.7(13) . . ?
Nb1 B33 H33A 141.0(13) . . ?
Nb2 B33 H33A 142.1(13) . . ?
B34 B33 H33B 116.2(12) . . ?
Nb1 B33 H33B 108.1(12) . . ?
Nb2 B33 H33B 51.0(12) . . ?
H33A B33 H33B 106.7(19) . . ?
B34 B33 H33C 116.5(13) . . ?
Nb1 B33 H33C 51.9(13) . . ?
Nb2 B33 H33C 110.2(12) . . ?
H33A B33 H33C 103.9(17) . . ?
H33B B33 H33C 101.6(16) . . ?
B33 B34 Nb2 68.23(10) . . ?
B33 B34 Nb1 68.13(10) . . ?
Nb2 B34 Nb1 75.74(6) . . ?
B33 B34 H34A 112.6(14) . . ?
Nb2 B34 H34A 142.2(13) . . ?
Nb1 B34 H34A 141.4(13) . . ?
B33 B34 H34C 116.7(12) . . ?
Nb2 B34 H34C 51.1(11) . . ?
Nb1 B34 H34C 107.6(11) . . ?
H34A B34 H34C 105.6(17) . . ?
B33 B34 H34B 114.7(12) . . ?
Nb2 B34 H34B 108.1(11) . . ?
Nb1 B34 H34B 49.7(11) . . ?
H34A B34 H34B 105.2(18) . . ?
H34C B34 H34B 100.6(17) . . ?

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 1.3(2) . . . . ?
C6 C1 C2 C3 -174.42(19) . . . . ?
Nb1 C1 C2 C3 65.73(13) . . . . ?
C5 C1 C2 C7 173.29(19) . . . . ?
C6 C1 C2 C7 -2.4(3) . . . . ?
Nb1 C1 C2 C7 -122.2(2) . . . . ?
C5 C1 C2 Nb1 -64.46(14) . . . . ?
C6 C1 C2 Nb1 119.8(2) . . . . ?
C1 C2 C3 C4 -1.0(2) . . . . ?
C7 C2 C3 C4 -173.18(19) . . . . ?
Nb1 C2 C3 C4 65.47(13) . . . . ?
C1 C2 C3 C8 174.85(19) . . . . ?
C7 C2 C3 C8 2.7(3) . . . . ?
Nb1 C2 C3 C8 -118.6(2) . . . . ?
C1 C2 C3 Nb1 -66.51(13) . . . . ?
C7 C2 C3 Nb1 121.36(19) . . . . ?
C2 C3 C4 C5 0.4(2) . . . . ?
C8 C3 C4 C5 -175.51(19) . . . . ?
Nb1 C3 C4 C5 64.82(13) . . . . ?
C2 C3 C4 C9 173.20(19) . . . . ?
C8 C3 C4 C9 -2.7(3) . . . . ?
Nb1 C3 C4 C9 -122.4(2) . . . . ?
C2 C3 C4 Nb1 -64.41(13) . . . . ?
C8 C3 C4 Nb1 119.7(2) . . . . ?
C2 C1 C5 C4 -1.0(2) . . . . ?
C6 C1 C5 C4 174.69(19) . . . . ?
Nb1 C1 C5 C4 -63.81(13) . . . . ?
C2 C1 C5 C10 -177.44(19) . . . . ?
C6 C1 C5 C10 -1.7(3) . . . . ?
Nb1 C1 C5 C10 119.8(2) . . . . ?
C2 C1 C5 Nb1 62.79(13) . . . . ?
C6 C1 C5 Nb1 -121.5(2) . . . . ?
C3 C4 C5 C1 0.4(2) . . . . ?
C9 C4 C5 C1 -172.4(2) . . . . ?
Nb1 C4 C5 C1 64.05(14) . . . . ?
C3 C4 C5 C10 176.82(19) . . . . ?
C9 C4 C5 C10 4.1(3) . . . . ?
Nb1 C4 C5 C10 -119.5(2) . . . . ?
C3 C4 C5 Nb1 -63.68(13) . . . . ?
C9 C4 C5 Nb1 123.6(2) . . . . ?
C15 C11 C12 C13 -1.1(2) . . . . ?
C16 C11 C12 C13 174.91(19) . . . . ?
Nb2 C11 C12 C13 -65.69(14) . . . . ?
C15 C11 C12 C17 -174.3(2) . . . . ?
C16 C11 C12 C17 1.7(3) . . . . ?
Nb2 C11 C12 C17 121.1(2) . . . . ?
C15 C11 C12 Nb2 64.55(13) . . . . ?
C16 C11 C12 Nb2 -119.4(2) . . . . ?
C11 C12 C13 C14 0.6(2) . . . . ?
C17 C12 C13 C14 173.7(2) . . . . ?
Nb2 C12 C13 C14 -63.65(14) . . . . ?
C11 C12 C13 C18 -175.92(19) . . . . ?
C17 C12 C13 C18 -2.8(3) . . . . ?
Nb2 C12 C13 C18 119.8(2) . . . . ?
C11 C12 C13 Nb2 64.23(13) . . . . ?
C17 C12 C13 Nb2 -122.6(2) . . . . ?
C12 C13 C14 C15 0.2(2) . . . . ?
C18 C13 C14 C15 176.75(19) . . . . ?
Nb2 C13 C14 C15 -62.80(13) . . . . ?
C12 C13 C14 C19 -176.3(2) . . . . ?
C18 C13 C14 C19 0.2(3) . . . . ?
Nb2 C13 C14 C19 120.7(2) . . . . ?
C12 C13 C14 Nb2 63.01(13) . . . . ?
C18 C13 C14 Nb2 -120.5(2) . . . . ?
C12 C11 C15 C14 1.3(2) . . . . ?
C16 C11 C15 C14 -174.7(2) . . . . ?
Nb2 C11 C15 C14 66.55(14) . . . . ?
C12 C11 C15 C20 175.7(2) . . . . ?
C16 C11 C15 C20 -0.2(3) . . . . ?
Nb2 C11 C15 C20 -119.0(2) . . . . ?
C12 C11 C15 Nb2 -65.27(14) . . . . ?
C16 C11 C15 Nb2 118.8(2) . . . . ?
C13 C14 C15 C11 -0.9(2) . . . . ?
C19 C14 C15 C11 175.5(2) . . . . ?
Nb2 C14 C15 C11 -65.51(13) . . . . ?
C13 C14 C15 C20 -175.4(2) . . . . ?
C19 C14 C15 C20 1.1(3) . . . . ?
Nb2 C14 C15 C20 120.1(2) . . . . ?
C13 C14 C15 Nb2 64.58(14) . . . . ?
C19 C14 C15 Nb2 -118.9(2) . . . . ?
C26 C21 C22 C23 -0.8(3) . . . . ?
Se1 C21 C22 C23 177.53(19) . . . . ?
C21 C22 C23 C24 1.1(4) . . . . ?
C22 C23 C24 C25 -1.0(4) . . . . ?
C23 C24 C25 C26 0.6(4) . . . . ?
C24 C25 C26 C21 -0.4(3) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
Se1 C21 C26 C25 -177.97(16) . . . . ?
Se1 B31 B32 Nb1 -139.65(11) . . . . ?
Nb2 B31 B32 Nb1 82.36(5) . . . . ?
Se1 B31 B32 Nb2 137.99(11) . . . . ?
Nb1 B31 B32 Nb2 -82.36(5) . . . . ?
Nb1 B33 B34 Nb2 82.80(6) . . . . ?
Nb2 B33 B34 Nb1 -82.80(6) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_BMBT
_database_code_depnum_ccdc_archive 'CCDC 1979259'
loop_
_audit_author_name
_audit_author_address
'P. K. SUTHADEVI ANTHARJANAM'
;Technical Officer, SAIF IIT Madras
India
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2021-03-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H45 B4 N Nb2 S2'
_chemical_formula_sum            'C27 H45 B4 N Nb2 S2'
_chemical_formula_weight         676.82

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'
N N 0.0061 0.0033 '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      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                   10.6906(2)
_cell_length_b                   11.8702(2)
_cell_length_c                   14.5084(3)
_cell_angle_alpha                109.764(3)
_cell_angle_beta                 108.139(3)
_cell_angle_gamma                94.319(4)
_cell_volume                     1612.63(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.89

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.857
_shelx_estimated_absorpt_T_min   0.919
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7001
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43653
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.447
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5657
_reflns_number_gt                4146
_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       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'


_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)+(0.0407P)²+0.6934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5657
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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 0.4957(4) 0.8441(4) 0.0560(3) 0.0410(10) Uani 1 1 d . . . . .
C2 C 0.4265(4) 0.9363(4) 0.0928(3) 0.0420(11) Uani 1 1 d . . . . .
C3 C 0.4993(4) 1.0049(3) 0.2011(3) 0.0412(10) Uani 1 1 d . . . . .
C4 C 0.6140(4) 0.9533(4) 0.2312(3) 0.0396(10) Uani 1 1 d . . . . .
C5 C 0.6127(4) 0.8549(4) 0.1415(3) 0.0412(10) Uani 1 1 d . . . . .
C6 C 0.7214(5) 0.7824(5) 0.1353(4) 0.0664(14) Uani 1 1 d . . . . .
H6A H 0.6956 0.7212 0.0658 0.100 Uiso 1 1 calc R U . . .
H6B H 0.8036 0.8361 0.1511 0.100 Uiso 1 1 calc R U . . .
H6C H 0.7345 0.7437 0.1850 0.100 Uiso 1 1 calc R U . . .
C7 C 0.4585(6) 0.7574(4) -0.0571(3) 0.0662(15) Uani 1 1 d . . . . .
H7A H 0.5211 0.7037 -0.0615 0.099 Uiso 1 1 calc R U . . .
H7B H 0.3694 0.7101 -0.0817 0.099 Uiso 1 1 calc R U . . .
H7C H 0.4615 0.8035 -0.0997 0.099 Uiso 1 1 calc R U . . .
C8 C 0.3029(5) 0.9623(5) 0.0264(4) 0.0670(15) Uani 1 1 d . . . . .
H8A H 0.2753 1.0290 0.0695 0.101 Uiso 1 1 calc R U . . .
H8B H 0.3220 0.9836 -0.0268 0.101 Uiso 1 1 calc R U . . .
H8C H 0.2322 0.8910 -0.0063 0.101 Uiso 1 1 calc R U . . .
C9 C 0.4665(5) 1.1163(4) 0.2687(4) 0.0626(14) Uani 1 1 d . . . . .
H9A H 0.5314 1.1452 0.3388 0.094 Uiso 1 1 calc R U . . .
H9B H 0.4687 1.1789 0.2409 0.094 Uiso 1 1 calc R U . . .
H9C H 0.3785 1.0962 0.2698 0.094 Uiso 1 1 calc R U . . .
C10 C 0.7268(5) 1.0045(4) 0.3372(3) 0.0608(14) Uani 1 1 d . . . . .
H10A H 0.7034 1.0705 0.3846 0.091 Uiso 1 1 calc R U . . .
H10B H 0.7409 0.9414 0.3646 0.091 Uiso 1 1 calc R U . . .
H10C H 0.8078 1.0340 0.3297 0.091 Uiso 1 1 calc R U . . .
C11 C 0.2206(4) 0.5852(4) 0.3722(3) 0.0412(10) Uani 1 1 d . . . . .
C12 C 0.2462(4) 0.4779(4) 0.3055(4) 0.0431(11) Uani 1 1 d . . . . .
C13 C 0.1425(5) 0.4399(4) 0.2053(3) 0.0489(12) Uani 1 1 d . . . . .
C14 C 0.0546(4) 0.5222(4) 0.2121(3) 0.0478(12) Uani 1 1 d . . . . .
C15 C 0.1028(4) 0.6128(4) 0.3139(3) 0.0460(11) Uani 1 1 d . . . . .
C16 C 0.0343(5) 0.7153(5) 0.3568(4) 0.0758(16) Uani 1 1 d . . . . .
H16A H 0.0885 0.7645 0.4285 0.114 Uiso 1 1 calc R U . . .
H16B H 0.0233 0.7651 0.3158 0.114 Uiso 1 1 calc R U . . .
H16C H -0.0522 0.6811 0.3531 0.114 Uiso 1 1 calc R U . . .
C17 C -0.0783(5) 0.5084(6) 0.1271(4) 0.0868(19) Uani 1 1 d . . . . .
H17A H -0.0885 0.4398 0.0646 0.130 Uiso 1 1 calc R U . . .
H17B H -0.1507 0.4954 0.1506 0.130 Uiso 1 1 calc R U . . .
H17C H -0.0797 0.5813 0.1122 0.130 Uiso 1 1 calc R U . . .
C18 C 0.1230(6) 0.3242(4) 0.1114(4) 0.089(2) Uani 1 1 d . . . . .
H18A H 0.1975 0.2847 0.1271 0.133 Uiso 1 1 calc R U . . .
H18B H 0.0412 0.2702 0.0958 0.133 Uiso 1 1 calc R U . . .
H18C H 0.1179 0.3446 0.0519 0.133 Uiso 1 1 calc R U . . .
C19 C 0.3572(6) 0.4127(5) 0.3375(5) 0.0828(18) Uani 1 1 d . . . . .
H19A H 0.3524 0.3429 0.2777 0.124 Uiso 1 1 calc R U . . .
H19B H 0.4424 0.4672 0.3640 0.124 Uiso 1 1 calc R U . . .
H19C H 0.3476 0.3865 0.3911 0.124 Uiso 1 1 calc R U . . .
C20 C 0.2978(5) 0.6486(5) 0.4882(3) 0.0693(15) Uani 1 1 d . . . . .
H20A H 0.3737 0.6120 0.5080 0.104 Uiso 1 1 calc R U . . .
H20B H 0.3285 0.7336 0.5046 0.104 Uiso 1 1 calc R U . . .
H20C H 0.2406 0.6406 0.5261 0.104 Uiso 1 1 calc R U . . .
C21 C 0.7350(4) 0.6364(4) 0.4095(3) 0.0376(10) Uani 1 1 d . . . . .
C22 C 0.9008(4) 0.6772(4) 0.5592(3) 0.0415(10) Uani 1 1 d . . . . .
C23 C 1.0124(4) 0.6600(5) 0.6311(4) 0.0541(12) Uani 1 1 d . . . . .
H23 H 1.0459 0.5889 0.6128 0.065 Uiso 1 1 calc R U . . .
C24 C 1.0708(5) 0.7501(5) 0.7284(4) 0.0657(14) Uani 1 1 d . . . . .
H24 H 1.1460 0.7403 0.7764 0.079 Uiso 1 1 calc R U . . .
C25 C 1.0209(5) 0.8560(5) 0.7577(4) 0.0676(15) Uani 1 1 d . . . . .
H25 H 1.0624 0.9153 0.8251 0.081 Uiso 1 1 calc R U . . .
C26 C 0.9106(5) 0.8745(5) 0.6881(4) 0.0612(13) Uani 1 1 d . . . . .
H26 H 0.8769 0.9454 0.7074 0.073 Uiso 1 1 calc R U . . .
C27 C 0.8519(4) 0.7841(4) 0.5889(3) 0.0447(11) Uani 1 1 d . . . . .
B1 B 0.3098(5) 0.8562(4) 0.3056(4) 0.0388(12) Uani 1 1 d . . . . .
B2 B 0.1964(5) 0.7901(5) 0.1735(4) 0.0433(12) Uani 1 1 d . . . . .
B3 B 0.4975(4) 0.6483(4) 0.2539(4) 0.0321(10) Uani 1 1 d . . . . .
B4 B 0.3862(5) 0.5807(4) 0.1210(4) 0.0354(11) Uani 1 1 d . . . . .
N1 N 0.8319(3) 0.5944(3) 0.4575(3) 0.0402(8) Uani 1 1 d . . . . .
S1 S 0.71388(12) 0.78039(11) 0.48470(9) 0.0497(3) Uani 1 1 d . . . . .
S2 S 0.63614(11) 0.55842(10) 0.27739(9) 0.0438(3) Uani 1 1 d . . . . .
Nb1 Nb 0.26721(3) 0.63757(3) 0.24154(3) 0.02917(11) Uani 1 1 d . . . . .
Nb2 Nb 0.42572(3) 0.80101(3) 0.18493(3) 0.02928(11) Uani 1 1 d . . . . .
H1A H 0.282(3) 0.932(3) 0.356(3) 0.036(10) Uiso 1 1 d . . . . .
H2A H 0.115(4) 0.837(4) 0.161(3) 0.054(12) Uiso 1 1 d . . . . .
H4A H 0.419(4) 0.504(4) 0.078(3) 0.045(11) Uiso 1 1 d . . . . .
H1B H 0.320(3) 0.791(3) 0.350(2) 0.027(9) Uiso 1 1 d . . . . .
H1C H 0.429(4) 0.893(3) 0.319(3) 0.048(11) Uiso 1 1 d . . . . .
H2B H 0.152(4) 0.687(3) 0.146(3) 0.038(10) Uiso 1 1 d . . . . .
H3A H 0.553(4) 0.756(3) 0.279(3) 0.041(10) Uiso 1 1 d . . . . .
H2C H 0.243(3) 0.783(3) 0.104(3) 0.037(10) Uiso 1 1 d . . . . .
H3B H 0.451(4) 0.651(3) 0.317(3) 0.040(10) Uiso 1 1 d . . . . .
H4C H 0.370(3) 0.649(3) 0.076(3) 0.038(10) Uiso 1 1 d . . . . .
H4B H 0.270(4) 0.545(3) 0.110(3) 0.052(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.414(6) . ?
C1 C5 1.422(6) . ?
C1 C7 1.517(6) . ?
C1 Nb2 2.404(4) . ?
C2 C3 1.420(6) . ?
C2 C8 1.497(6) . ?
C2 Nb2 2.413(4) . ?
C3 C4 1.426(6) . ?
C3 C9 1.496(6) . ?
C3 Nb2 2.398(4) . ?
C4 C5 1.420(6) . ?
C4 C10 1.514(6) . ?
C4 Nb2 2.358(4) . ?
C5 C6 1.504(6) . ?
C5 Nb2 2.381(4) . ?
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 C15 1.412(6) . ?
C11 C12 1.420(6) . ?
C11 C20 1.505(6) . ?
C11 Nb1 2.360(4) . ?
C12 C13 1.423(6) . ?
C12 C19 1.503(6) . ?
C12 Nb1 2.400(4) . ?
C13 C14 1.406(6) . ?
C13 C18 1.517(6) . ?
C13 Nb1 2.412(4) . ?
C14 C15 1.405(6) . ?
C14 C17 1.518(6) . ?
C14 Nb1 2.399(4) . ?
C15 C16 1.520(6) . ?
C15 Nb1 2.357(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N1 1.292(5) . ?
C21 S2 1.743(4) . ?
C21 S1 1.764(4) . ?
C22 N1 1.385(5) . ?
C22 C27 1.392(6) . ?
C22 C23 1.399(6) . ?
C23 C24 1.363(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.388(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.381(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.382(6) . ?
C26 H26 0.9300 . ?
C27 S1 1.739(4) . ?
B1 B2 1.775(7) . ?
B1 Nb2 2.393(5) . ?
B1 Nb1 2.394(5) . ?
B1 H1A 1.07(4) . ?
B1 H1B 1.15(3) . ?
B1 H1C 1.25(4) . ?
B2 Nb2 2.395(5) . ?
B2 Nb1 2.403(5) . ?
B2 H2A 1.07(4) . ?
B2 H2B 1.16(4) . ?
B2 H2C 1.24(3) . ?
B3 B4 1.777(6) . ?
B3 S2 1.903(4) . ?
B3 Nb1 2.402(4) . ?
B3 Nb2 2.415(4) . ?
B3 H3A 1.24(4) . ?
B3 H3B 1.16(4) . ?
B4 Nb2 2.414(5) . ?
B4 Nb1 2.418(5) . ?
B4 H4A 1.07(4) . ?
B4 H4C 1.20(4) . ?
B4 H4B 1.23(4) . ?
Nb1 Nb2 2.9597(5) . ?
Nb1 H1B 1.87(3) . ?
Nb1 H2B 1.84(3) . ?
Nb1 H3B 1.89(4) . ?
Nb1 H4B 1.87(4) . ?
Nb2 H1C 1.87(4) . ?
Nb2 H3A 1.86(3) . ?
Nb2 H2C 1.89(3) . ?
Nb2 H4C 1.85(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
C2 C1 C5 108.1(4) . . ?
C2 C1 C7 125.7(4) . . ?
C5 C1 C7 126.0(4) . . ?
C2 C1 Nb2 73.3(2) . . ?
C5 C1 Nb2 71.8(2) . . ?
C7 C1 Nb2 125.2(3) . . ?
C1 C2 C3 108.6(4) . . ?
C1 C2 C8 125.4(4) . . ?
C3 C2 C8 125.9(4) . . ?
C1 C2 Nb2 72.6(2) . . ?
C3 C2 Nb2 72.3(2) . . ?
C8 C2 Nb2 124.5(3) . . ?
C2 C3 C4 107.3(4) . . ?
C2 C3 C9 126.1(4) . . ?
C4 C3 C9 126.5(4) . . ?
C2 C3 Nb2 73.4(2) . . ?
C4 C3 Nb2 71.0(2) . . ?
C9 C3 Nb2 124.2(3) . . ?
C5 C4 C3 108.4(3) . . ?
C5 C4 C10 125.6(4) . . ?
C3 C4 C10 125.6(4) . . ?
C5 C4 Nb2 73.4(2) . . ?
C3 C4 Nb2 74.1(2) . . ?
C10 C4 Nb2 124.2(3) . . ?
C4 C5 C1 107.7(4) . . ?
C4 C5 C6 126.2(4) . . ?
C1 C5 C6 125.9(4) . . ?
C4 C5 Nb2 71.7(2) . . ?
C1 C5 Nb2 73.6(2) . . ?
C6 C5 Nb2 124.4(3) . . ?
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 . . ?
C15 C11 C12 108.5(4) . . ?
C15 C11 C20 126.3(4) . . ?
C12 C11 C20 124.8(4) . . ?
C15 C11 Nb1 72.5(2) . . ?
C12 C11 Nb1 74.2(2) . . ?
C20 C11 Nb1 124.7(3) . . ?
C11 C12 C13 107.2(4) . . ?
C11 C12 C19 126.0(4) . . ?
C13 C12 C19 126.7(4) . . ?
C11 C12 Nb1 71.1(2) . . ?
C13 C12 Nb1 73.2(2) . . ?
C19 C12 Nb1 124.0(3) . . ?
C14 C13 C12 107.8(4) . . ?
C14 C13 C18 126.2(5) . . ?
C12 C13 C18 125.8(5) . . ?
C14 C13 Nb1 72.5(2) . . ?
C12 C13 Nb1 72.4(2) . . ?
C18 C13 Nb1 125.4(3) . . ?
C15 C14 C13 109.0(4) . . ?
C15 C14 C17 125.2(5) . . ?
C13 C14 C17 125.6(5) . . ?
C15 C14 Nb1 71.2(2) . . ?
C13 C14 Nb1 73.5(2) . . ?
C17 C14 Nb1 126.1(3) . . ?
C14 C15 C11 107.6(4) . . ?
C14 C15 C16 126.3(4) . . ?
C11 C15 C16 125.9(4) . . ?
C14 C15 Nb1 74.5(2) . . ?
C11 C15 Nb1 72.7(2) . . ?
C16 C15 Nb1 122.7(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C11 C20 H20A 109.5 . . ?
C11 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C11 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 S2 122.0(3) . . ?
N1 C21 S1 115.7(3) . . ?
S2 C21 S1 122.3(2) . . ?
N1 C22 C27 115.5(4) . . ?
N1 C22 C23 124.9(4) . . ?
C27 C22 C23 119.6(4) . . ?
C24 C23 C22 118.4(5) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C23 C24 C25 121.6(4) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 117.7(5) . . ?
C25 C26 H26 121.1 . . ?
C27 C26 H26 121.1 . . ?
C26 C27 C22 121.8(4) . . ?
C26 C27 S1 128.7(4) . . ?
C22 C27 S1 109.5(3) . . ?
B2 B1 Nb2 68.3(2) . . ?
B2 B1 Nb1 68.6(2) . . ?
Nb2 B1 Nb1 76.36(15) . . ?
B2 B1 H1A 115.1(19) . . ?
Nb2 B1 H1A 143.9(19) . . ?
Nb1 B1 H1A 139.6(19) . . ?
B2 B1 H1B 114.6(16) . . ?
Nb2 B1 H1B 109.7(16) . . ?
Nb1 B1 H1B 49.7(16) . . ?
H1A B1 H1B 101(2) . . ?
B2 B1 H1C 116.1(17) . . ?
Nb2 B1 H1C 50.6(17) . . ?
Nb1 B1 H1C 108.1(17) . . ?
H1A B1 H1C 105(3) . . ?
H1B B1 H1C 103(2) . . ?
B1 B2 Nb2 68.2(2) . . ?
B1 B2 Nb1 68.0(2) . . ?
Nb2 B2 Nb1 76.16(15) . . ?
B1 B2 H2A 111(2) . . ?
Nb2 B2 H2A 143(2) . . ?
Nb1 B2 H2A 140(2) . . ?
B1 B2 H2B 113.9(17) . . ?
Nb2 B2 H2B 105.3(18) . . ?
Nb1 B2 H2B 47.9(17) . . ?
H2A B2 H2B 108(3) . . ?
B1 B2 H2C 117.5(17) . . ?
Nb2 B2 H2C 51.6(16) . . ?
Nb1 B2 H2C 107.5(16) . . ?
H2A B2 H2C 107(3) . . ?
H2B B2 H2C 98(2) . . ?
B4 B3 S2 110.0(3) . . ?
B4 B3 Nb1 68.8(2) . . ?
S2 B3 Nb1 139.2(2) . . ?
B4 B3 Nb2 68.4(2) . . ?
S2 B3 Nb2 143.7(2) . . ?
Nb1 B3 Nb2 75.81(13) . . ?
B4 B3 H3A 113.1(16) . . ?
S2 B3 H3A 107.0(17) . . ?
Nb1 B3 H3A 110.5(17) . . ?
Nb2 B3 H3A 49.3(16) . . ?
B4 B3 H3B 116.3(18) . . ?
S2 B3 H3B 104.4(18) . . ?
Nb1 B3 H3B 50.6(18) . . ?
Nb2 B3 H3B 108.4(18) . . ?
H3A B3 H3B 105(2) . . ?
B3 B4 Nb2 68.5(2) . . ?
B3 B4 Nb1 67.9(2) . . ?
Nb2 B4 Nb1 75.56(14) . . ?
B3 B4 H4A 111(2) . . ?
Nb2 B4 H4A 142(2) . . ?
Nb1 B4 H4A 141(2) . . ?
B3 B4 H4C 114.3(17) . . ?
Nb2 B4 H4C 48.3(16) . . ?
Nb1 B4 H4C 105.8(17) . . ?
H4A B4 H4C 109(3) . . ?
B3 B4 H4B 114.2(18) . . ?
Nb2 B4 H4B 107.2(18) . . ?
Nb1 B4 H4B 49.3(18) . . ?
H4A B4 H4B 107(3) . . ?
H4C B4 H4B 101(2) . . ?
C21 N1 C22 110.7(3) . . ?
C27 S1 C21 88.5(2) . . ?
C21 S2 B3 103.99(19) . . ?
C15 Nb1 C11 34.85(14) . . ?
C15 Nb1 B1 97.15(16) . . ?
C11 Nb1 B1 105.96(16) . . ?
C15 Nb1 C14 34.34(15) . . ?
C11 Nb1 C14 57.03(14) . . ?
B1 Nb1 C14 121.15(17) . . ?
C15 Nb1 C12 57.78(15) . . ?
C11 Nb1 C12 34.70(14) . . ?
B1 Nb1 C12 138.97(16) . . ?
C14 Nb1 C12 56.89(15) . . ?
C15 Nb1 B3 148.70(16) . . ?
C11 Nb1 B3 114.12(15) . . ?
B1 Nb1 B3 88.03(16) . . ?
C14 Nb1 B3 150.48(16) . . ?
C12 Nb1 B3 98.98(15) . . ?
C15 Nb1 B2 100.68(17) . . ?
C11 Nb1 B2 130.23(17) . . ?
B1 Nb1 B2 43.42(17) . . ?
C14 Nb1 B2 101.01(17) . . ?
C12 Nb1 B2 156.94(17) . . ?
B3 Nb1 B2 104.08(17) . . ?
C15 Nb1 C13 57.33(15) . . ?
C11 Nb1 C13 57.30(14) . . ?
B1 Nb1 C13 153.86(17) . . ?
C14 Nb1 C13 33.98(15) . . ?
C12 Nb1 C13 34.40(15) . . ?
B3 Nb1 C13 116.51(16) . . ?
B2 Nb1 C13 129.24(18) . . ?
C15 Nb1 B4 156.84(16) . . ?
C11 Nb1 B4 141.28(16) . . ?
B1 Nb1 B4 103.96(17) . . ?
C14 Nb1 B4 123.23(16) . . ?
C12 Nb1 B4 108.68(15) . . ?
B3 Nb1 B4 43.26(15) . . ?
B2 Nb1 B4 88.48(17) . . ?
C13 Nb1 B4 100.48(15) . . ?
C15 Nb1 Nb2 147.59(11) . . ?
C11 Nb1 Nb2 149.23(10) . . ?
B1 Nb1 Nb2 51.80(12) . . ?
C14 Nb1 Nb2 149.33(11) . . ?
C12 Nb1 Nb2 151.26(10) . . ?
B3 Nb1 Nb2 52.29(11) . . ?
B2 Nb1 Nb2 51.80(13) . . ?
C13 Nb1 Nb2 151.20(10) . . ?
B4 Nb1 Nb2 52.16(11) . . ?
C15 Nb1 H1B 82.4(10) . . ?
C11 Nb1 H1B 80.2(10) . . ?
B1 Nb1 H1B 28.1(10) . . ?
C14 Nb1 H1B 115.0(10) . . ?
C12 Nb1 H1B 111.2(10) . . ?
B3 Nb1 H1B 88.3(10) . . ?
B2 Nb1 H1B 70.0(10) . . ?
C13 Nb1 H1B 136.3(10) . . ?
B4 Nb1 H1B 120.7(10) . . ?
Nb2 Nb1 H1B 72.5(10) . . ?
C15 Nb1 H2B 91.7(11) . . ?
C11 Nb1 H2B 126.5(11) . . ?
B1 Nb1 H2B 70.4(12) . . ?
C14 Nb1 H2B 78.9(11) . . ?
C12 Nb1 H2B 134.7(12) . . ?
B3 Nb1 H2B 118.9(11) . . ?
B2 Nb1 H2B 28.0(11) . . ?
C13 Nb1 H2B 102.2(12) . . ?
B4 Nb1 H2B 86.5(11) . . ?
Nb2 Nb1 H2B 70.8(11) . . ?
H1B Nb1 H2B 94.7(15) . . ?
C15 Nb1 H3B 120.8(11) . . ?
C11 Nb1 H3B 87.2(11) . . ?
B1 Nb1 H3B 87.3(11) . . ?
C14 Nb1 H3B 137.9(11) . . ?
C12 Nb1 H3B 81.1(11) . . ?
B3 Nb1 H3B 28.2(11) . . ?
B2 Nb1 H3B 120.1(11) . . ?
C13 Nb1 H3B 109.8(11) . . ?
B4 Nb1 H3B 70.2(11) . . ?
Nb2 Nb1 H3B 72.3(11) . . ?
H1B Nb1 H3B 74.7(14) . . ?
H2B Nb1 H3B 143.1(16) . . ?
C15 Nb1 H4B 128.4(13) . . ?
C11 Nb1 H4B 133.0(12) . . ?
B1 Nb1 H4B 121.0(12) . . ?
C14 Nb1 H4B 94.1(13) . . ?
C12 Nb1 H4B 99.4(12) . . ?
B3 Nb1 H4B 71.7(13) . . ?
B2 Nb1 H4B 87.9(12) . . ?
C13 Nb1 H4B 77.9(12) . . ?
B4 Nb1 H4B 29.8(12) . . ?
Nb2 Nb1 H4B 73.4(12) . . ?
H1B Nb1 H4B 145.9(16) . . ?
H2B Nb1 H4B 72.7(16) . . ?
H3B Nb1 H4B 96.1(17) . . ?
C4 Nb2 C5 34.87(14) . . ?
C4 Nb2 B1 112.10(16) . . ?
C5 Nb2 B1 146.90(16) . . ?
C4 Nb2 B2 137.73(17) . . ?
C5 Nb2 B2 153.66(16) . . ?
B1 Nb2 B2 43.51(17) . . ?
C4 Nb2 C3 34.88(14) . . ?
C5 Nb2 C3 57.76(14) . . ?
B1 Nb2 C3 96.16(16) . . ?
B2 Nb2 C3 104.73(17) . . ?
C4 Nb2 C1 57.59(14) . . ?
C5 Nb2 C1 34.57(14) . . ?
B1 Nb2 C1 147.88(16) . . ?
B2 Nb2 C1 120.58(16) . . ?
C3 Nb2 C1 57.27(14) . . ?
C4 Nb2 C2 57.39(14) . . ?
C5 Nb2 C2 57.21(14) . . ?
B1 Nb2 C2 113.75(16) . . ?
B2 Nb2 C2 96.95(16) . . ?
C3 Nb2 C2 34.33(14) . . ?
C1 Nb2 C2 34.14(14) . . ?
C4 Nb2 B4 133.48(16) . . ?
C5 Nb2 B4 103.93(16) . . ?
B1 Nb2 B4 104.11(17) . . ?
B2 Nb2 B4 88.76(18) . . ?
C3 Nb2 B4 159.59(16) . . ?
C1 Nb2 B4 102.76(15) . . ?
C2 Nb2 B4 130.24(15) . . ?
C4 Nb2 B3 109.25(15) . . ?
C5 Nb2 B3 100.99(15) . . ?
B1 Nb2 B3 87.77(16) . . ?
B2 Nb2 B3 103.94(17) . . ?
C3 Nb2 B3 141.94(15) . . ?
C1 Nb2 B3 124.13(15) . . ?
C2 Nb2 B3 157.36(15) . . ?
B4 Nb2 B3 43.18(15) . . ?
C4 Nb2 Nb1 150.34(10) . . ?
C5 Nb2 Nb1 151.77(10) . . ?
B1 Nb2 Nb1 51.83(12) . . ?
B2 Nb2 Nb1 52.04(12) . . ?
C3 Nb2 Nb1 147.87(10) . . ?
C1 Nb2 Nb1 150.11(10) . . ?
C2 Nb2 Nb1 147.94(10) . . ?
B4 Nb2 Nb1 52.28(12) . . ?
B3 Nb2 Nb1 51.90(11) . . ?
C4 Nb2 H1C 83.3(12) . . ?
C5 Nb2 H1C 117.0(12) . . ?
B1 Nb2 H1C 31.0(12) . . ?
B2 Nb2 H1C 73.3(12) . . ?
C3 Nb2 H1C 78.4(11) . . ?
C1 Nb2 H1C 135.3(12) . . ?
C2 Nb2 H1C 108.1(11) . . ?
B4 Nb2 H1C 120.7(11) . . ?
B3 Nb2 H1C 86.4(11) . . ?
Nb1 Nb2 H1C 73.7(12) . . ?
C4 Nb2 H3A 80.5(11) . . ?
C5 Nb2 H3A 83.0(11) . . ?
B1 Nb2 H3A 89.5(11) . . ?
B2 Nb2 H3A 123.2(11) . . ?
C3 Nb2 H3A 111.6(11) . . ?
C1 Nb2 H3A 115.7(11) . . ?
C2 Nb2 H3A 136.7(11) . . ?
B4 Nb2 H3A 71.4(11) . . ?
B3 Nb2 H3A 30.4(11) . . ?
Nb1 Nb2 H3A 75.2(11) . . ?
H1C Nb2 H3A 73.0(16) . . ?
C4 Nb2 H2C 130.5(10) . . ?
C5 Nb2 H2C 125.5(11) . . ?
B1 Nb2 H2C 73.5(11) . . ?
B2 Nb2 H2C 31.0(11) . . ?
C3 Nb2 H2C 97.0(10) . . ?
C1 Nb2 H2C 90.9(11) . . ?
C2 Nb2 H2C 75.0(11) . . ?
B4 Nb2 H2C 86.7(10) . . ?
B3 Nb2 H2C 120.2(10) . . ?
Nb1 Nb2 H2C 73.2(11) . . ?
H1C Nb2 H2C 100.8(16) . . ?
H3A Nb2 H2C 148.2(16) . . ?
C4 Nb2 H4C 127.7(11) . . ?
C5 Nb2 H4C 92.8(11) . . ?
B1 Nb2 H4C 120.1(11) . . ?
B2 Nb2 H4C 87.4(11) . . ?
C3 Nb2 H4C 134.6(11) . . ?
C1 Nb2 H4C 78.7(11) . . ?
C2 Nb2 H4C 101.8(11) . . ?
B4 Nb2 H4C 28.9(11) . . ?
B3 Nb2 H4C 71.0(11) . . ?
Nb1 Nb2 H4C 72.3(11) . . ?
H1C Nb2 H4C 145.9(16) . . ?
H3A Nb2 H4C 96.1(16) . . ?
H2C Nb2 H4C 71.3(15) . . ?

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 -0.1(4) . . . . ?
C7 C1 C2 C3 -174.6(4) . . . . ?
Nb2 C1 C2 C3 63.7(3) . . . . ?
C5 C1 C2 C8 175.8(4) . . . . ?
C7 C1 C2 C8 1.3(7) . . . . ?
Nb2 C1 C2 C8 -120.4(4) . . . . ?
C5 C1 C2 Nb2 -63.8(3) . . . . ?
C7 C1 C2 Nb2 121.7(4) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C8 C2 C3 C4 -176.4(4) . . . . ?
Nb2 C2 C3 C4 63.4(3) . . . . ?
C1 C2 C3 C9 175.4(4) . . . . ?
C8 C2 C3 C9 -0.4(7) . . . . ?
Nb2 C2 C3 C9 -120.6(4) . . . . ?
C1 C2 C3 Nb2 -64.0(3) . . . . ?
C8 C2 C3 Nb2 120.2(4) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
C9 C3 C4 C5 -175.0(4) . . . . ?
Nb2 C3 C4 C5 66.0(3) . . . . ?
C2 C3 C4 C10 174.0(4) . . . . ?
C9 C3 C4 C10 -2.0(7) . . . . ?
Nb2 C3 C4 C10 -121.0(4) . . . . ?
C2 C3 C4 Nb2 -65.0(3) . . . . ?
C9 C3 C4 Nb2 119.0(4) . . . . ?
C3 C4 C5 C1 -1.0(4) . . . . ?
C10 C4 C5 C1 -174.1(4) . . . . ?
Nb2 C4 C5 C1 65.4(3) . . . . ?
C3 C4 C5 C6 173.9(4) . . . . ?
C10 C4 C5 C6 0.9(7) . . . . ?
Nb2 C4 C5 C6 -119.7(4) . . . . ?
C3 C4 C5 Nb2 -66.4(3) . . . . ?
C10 C4 C5 Nb2 120.6(4) . . . . ?
C2 C1 C5 C4 0.7(4) . . . . ?
C7 C1 C5 C4 175.2(4) . . . . ?
Nb2 C1 C5 C4 -64.1(3) . . . . ?
C2 C1 C5 C6 -174.3(4) . . . . ?
C7 C1 C5 C6 0.2(7) . . . . ?
Nb2 C1 C5 C6 120.9(4) . . . . ?
C2 C1 C5 Nb2 64.8(3) . . . . ?
C7 C1 C5 Nb2 -120.7(4) . . . . ?
C15 C11 C12 C13 0.0(4) . . . . ?
C20 C11 C12 C13 173.5(4) . . . . ?
Nb1 C11 C12 C13 -64.9(3) . . . . ?
C15 C11 C12 C19 -176.4(4) . . . . ?
C20 C11 C12 C19 -2.9(7) . . . . ?
Nb1 C11 C12 C19 118.8(4) . . . . ?
C15 C11 C12 Nb1 64.9(3) . . . . ?
C20 C11 C12 Nb1 -121.6(4) . . . . ?
C11 C12 C13 C14 -0.9(5) . . . . ?
C19 C12 C13 C14 175.5(4) . . . . ?
Nb1 C12 C13 C14 -64.3(3) . . . . ?
C11 C12 C13 C18 -175.2(4) . . . . ?
C19 C12 C13 C18 1.1(7) . . . . ?
Nb1 C12 C13 C18 121.3(4) . . . . ?
C11 C12 C13 Nb1 63.4(3) . . . . ?
C19 C12 C13 Nb1 -120.2(4) . . . . ?
C12 C13 C14 C15 1.5(5) . . . . ?
C18 C13 C14 C15 175.8(4) . . . . ?
Nb1 C13 C14 C15 -62.8(3) . . . . ?
C12 C13 C14 C17 -172.8(4) . . . . ?
C18 C13 C14 C17 1.5(7) . . . . ?
Nb1 C13 C14 C17 123.0(4) . . . . ?
C12 C13 C14 Nb1 64.2(3) . . . . ?
C18 C13 C14 Nb1 -121.5(4) . . . . ?
C13 C14 C15 C11 -1.5(5) . . . . ?
C17 C14 C15 C11 172.8(4) . . . . ?
Nb1 C14 C15 C11 -65.7(3) . . . . ?
C13 C14 C15 C16 -176.3(4) . . . . ?
C17 C14 C15 C16 -2.0(7) . . . . ?
Nb1 C14 C15 C16 119.5(4) . . . . ?
C13 C14 C15 Nb1 64.2(3) . . . . ?
C17 C14 C15 Nb1 -121.5(4) . . . . ?
C12 C11 C15 C14 0.9(5) . . . . ?
C20 C11 C15 C14 -172.5(4) . . . . ?
Nb1 C11 C15 C14 66.9(3) . . . . ?
C12 C11 C15 C16 175.7(4) . . . . ?
C20 C11 C15 C16 2.3(7) . . . . ?
Nb1 C11 C15 C16 -118.3(4) . . . . ?
C12 C11 C15 Nb1 -66.0(3) . . . . ?
C20 C11 C15 Nb1 120.6(4) . . . . ?
N1 C22 C23 C24 179.4(4) . . . . ?
C27 C22 C23 C24 -0.6(7) . . . . ?
C22 C23 C24 C25 1.1(8) . . . . ?
C23 C24 C25 C26 -0.9(8) . . . . ?
C24 C25 C26 C27 0.1(8) . . . . ?
C25 C26 C27 C22 0.4(7) . . . . ?
C25 C26 C27 S1 -179.7(4) . . . . ?
N1 C22 C27 C26 179.9(4) . . . . ?
C23 C22 C27 C26 -0.1(7) . . . . ?
N1 C22 C27 S1 0.0(5) . . . . ?
C23 C22 C27 S1 180.0(3) . . . . ?
Nb1 B1 B2 Nb2 -83.32(13) . . . . ?
Nb2 B1 B2 Nb1 83.32(13) . . . . ?
S2 B3 B4 Nb2 -141.1(3) . . . . ?
Nb1 B3 B4 Nb2 82.58(11) . . . . ?
S2 B3 B4 Nb1 136.3(3) . . . . ?
Nb2 B3 B4 Nb1 -82.58(11) . . . . ?
S2 C21 N1 C22 175.7(3) . . . . ?
S1 C21 N1 C22 -1.8(4) . . . . ?
C27 C22 N1 C21 1.1(5) . . . . ?
C23 C22 N1 C21 -178.8(4) . . . . ?
C26 C27 S1 C21 179.4(5) . . . . ?
C22 C27 S1 C21 -0.8(3) . . . . ?
N1 C21 S1 C27 1.5(3) . . . . ?
S2 C21 S1 C27 -176.0(3) . . . . ?
N1 C21 S2 B3 172.4(3) . . . . ?
S1 C21 S2 B3 -10.3(3) . . . . ?

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.077

# start Validation Reply Form
_vrf_PLAT910_BMBT                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: Intensity of these reflections are cut by the beamstop. Hence
omitted from refinement. 
;
# end Validation Reply Form


