# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2016_0505r2
_database_code_depnum_ccdc_archive 'CCDC 1542832'
_audit_update_record             
;
2017-04-07 deposited with the CCDC.
2017-06-26 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         'C4 H10 Cl3 Nb S3'
_chemical_formula_sum            'C4 H10 Cl3 Nb S3'
_chemical_formula_weight         353.56

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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   7.2010(3)
_cell_length_b                   11.3494(4)
_cell_length_c                   7.8693(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.502(7)
_cell_angle_gamma                90
_cell_volume                     580.47(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4775
_cell_measurement_theta_min      2.8360
_cell_measurement_theta_max      32.2020

_exptl_crystal_description       Chip
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_F_000             348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    2.209
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            5010
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.868
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2251
_reflns_number_gt                2212
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_max     0.984
_reflns_Friedel_fraction_full    0.987

_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       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²+0.2849P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1010 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.06(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2251
_refine_ls_number_parameters     102
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0425
_refine_ls_wR_factor_gt          0.0423
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.81578(5) 0.76017(3) 0.73224(4) 0.01682(10) Uani 1 1 d . U . . .
Cl1 Cl 0.50200(14) 0.85946(9) 0.56567(14) 0.0231(2) Uani 1 1 d . . . . .
Cl2 Cl 1.02554(14) 0.90758(8) 0.73787(14) 0.0205(2) Uani 1 1 d . . . . .
Cl3 Cl 1.06770(13) 0.65239(8) 0.98192(13) 0.01653(19) Uani 1 1 d . . . . .
S1 S 0.74804(14) 0.86683(8) 1.01273(13) 0.01526(18) Uani 1 1 d . U . . .
S2 S 0.59161(14) 0.59422(8) 0.81021(15) 0.0167(2) Uani 1 1 d . . . . .
S3 S 0.79355(18) 0.64069(11) 0.50249(15) 0.0283(3) Uani 1 1 d . . . . .
C1 C 0.9689(6) 0.8486(4) 1.2362(5) 0.0184(8) Uani 1 1 d . . . . .
H1A H 1.0019 0.7646 1.2592 0.028 Uiso 1 1 calc R U . . .
H1B H 0.9380 0.8806 1.3368 0.028 Uiso 1 1 calc R U . . .
H1C H 1.0867 0.8906 1.2340 0.028 Uiso 1 1 calc R U . . .
C2 C 0.5588(5) 0.7743(4) 1.0384(5) 0.0164(8) Uani 1 1 d . . . . .
H2A H 0.5555 0.7926 1.1601 0.020 Uiso 1 1 calc R U . . .
H2B H 0.4218 0.7935 0.9369 0.020 Uiso 1 1 calc R U . . .
C3 C 0.5978(6) 0.6430(4) 1.0314(6) 0.0170(8) Uani 1 1 d . . . . .
H3A H 0.4926 0.5988 1.0550 0.020 Uiso 1 1 calc R U . . .
H3B H 0.7340 0.6236 1.1340 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3238(6) 0.6085(4) 0.6523(6) 0.0228(9) Uani 1 1 d . . . . .
H4A H 0.2818 0.6910 0.6478 0.034 Uiso 1 1 calc R U . . .
H4B H 0.2419 0.5593 0.6969 0.034 Uiso 1 1 calc R U . . .
H4C H 0.3015 0.5829 0.5260 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 S3 2.2100(12) . ?
Nb1 Cl2 2.2416(10) . ?
Nb1 Cl1 2.3543(10) . ?
Nb1 Cl3 2.3619(9) . ?
Nb1 S2 2.7171(10) . ?
Nb1 S1 2.7390(11) . ?
S1 C2 1.799(4) . ?
S1 C1 1.805(4) . ?
S2 C4 1.796(4) . ?
S2 C3 1.809(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.522(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S3 Nb1 Cl2 106.56(4) . . ?
S3 Nb1 Cl1 97.13(4) . . ?
Cl2 Nb1 Cl1 97.52(4) . . ?
S3 Nb1 Cl3 97.00(4) . . ?
Cl2 Nb1 Cl3 95.76(4) . . ?
Cl1 Nb1 Cl3 156.97(4) . . ?
S3 Nb1 S2 85.33(4) . . ?
Cl2 Nb1 S2 166.83(4) . . ?
Cl1 Nb1 S2 86.36(3) . . ?
Cl3 Nb1 S2 76.78(3) . . ?
S3 Nb1 S1 162.77(4) . . ?
Cl2 Nb1 S1 90.37(4) . . ?
Cl1 Nb1 S1 77.05(4) . . ?
Cl3 Nb1 S1 84.15(3) . . ?
S2 Nb1 S1 78.18(3) . . ?
C2 S1 C1 102.47(18) . . ?
C2 S1 Nb1 103.82(13) . . ?
C1 S1 Nb1 110.29(14) . . ?
C4 S2 C3 102.27(19) . . ?
C4 S2 Nb1 110.29(15) . . ?
C3 S2 Nb1 103.56(13) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 S1 114.0(3) . . ?
C3 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 S2 113.9(3) . . ?
C2 C3 H3A 108.8 . . ?
S2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
S2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
S2 C4 H4A 109.5 . . ?
S2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         0.384
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_2016_1407r2
_database_code_depnum_ccdc_archive 'CCDC 1542834'
_audit_update_record             
;
2017-04-07 deposited with the CCDC.
2017-06-26 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         'C5 H12 Cl3 Nb S Se2'
_chemical_formula_sum            'C5 H12 Cl3 Nb S Se2'
_chemical_formula_weight         461.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   10.00610(10)
_cell_length_b                   10.00610(10)
_cell_length_c                   26.1100(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2614.19(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6364
_cell_measurement_theta_min      2.1890
_cell_measurement_theta_max      32.1700

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.345
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    7.216
_shelx_estimated_absorpt_T_min   0.621
_shelx_estimated_absorpt_T_max   0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.39267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            11648
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.102
_diffrn_reflns_theta_max         32.295
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2242
_reflns_number_gt                1882
_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       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+6.1134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2242
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Nb1 Nb 0.0000 0.7500 0.11484(2) 0.01683(9) Uani 1 2 d S T P . .
Se1 Se 0.10129(2) 0.59686(3) 0.19978(2) 0.01326(8) Uani 1 1 d . . . . .
Cl1 Cl -0.0949(7) 0.9136(6) 0.06431(13) 0.0126(7) Uani 0.5 1 d . . P . .
Cl2 Cl 0.20178(6) 0.86508(7) 0.13232(2) 0.01712(13) Uani 1 1 d . . . . .
S1 S 0.0737(8) 0.5969(6) 0.06157(14) 0.0126(7) Uani 0.5 1 d . . P . .
C1 C 0.0456(3) 0.4156(3) 0.18385(11) 0.0193(5) Uani 1 1 d . . . . .
H1A H 0.0640 0.3574 0.2132 0.029 Uiso 1 1 calc R U . . .
H1B H 0.0950 0.3833 0.1539 0.029 Uiso 1 1 calc R U . . .
H1C H -0.0504 0.4146 0.1764 0.029 Uiso 1 1 calc R U . . .
C2 C -0.0309(3) 0.6259(3) 0.25448(10) 0.0190(5) Uani 1 1 d . . . . .
H2A H -0.1208 0.6351 0.2390 0.023 Uiso 1 1 calc R U . . .
H2B H -0.0323 0.5470 0.2773 0.023 Uiso 1 1 calc R U . . .
C3 C 0.0000 0.7500 0.28592(16) 0.0218(8) Uani 1 2 d S T P . .
H3A H 0.0775 0.7307 0.3083 0.026 Uiso 0.5 1 calc R U P . .
H3B H -0.0775 0.7693 0.3083 0.026 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 S1 2.197(8) 6_464 ?
Nb1 S1 2.197(8) . ?
Nb1 Cl1 2.308(7) . ?
Nb1 Cl1 2.308(7) 6_464 ?
Nb1 Cl2 2.3686(6) . ?
Nb1 Cl2 2.3686(6) 6_464 ?
Nb1 Se1 2.8799(4) 6_464 ?
Nb1 Se1 2.8799(4) . ?
Se1 C1 1.943(3) . ?
Se1 C2 1.968(3) . ?
Cl1 S1 0.247(13) 6_464 ?
S1 Cl1 0.247(13) 6_464 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.520(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.520(4) 6_464 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Nb1 S1 101.44(16) 6_464 . ?
S1 Nb1 Cl1 5.6(2) 6_464 . ?
S1 Nb1 Cl1 105.73(5) . . ?
S1 Nb1 Cl1 105.74(5) 6_464 6_464 ?
S1 Nb1 Cl1 5.6(2) . 6_464 ?
Cl1 Nb1 Cl1 110.25(13) . 6_464 ?
S1 Nb1 Cl2 93.97(18) 6_464 . ?
S1 Nb1 Cl2 100.06(18) . . ?
Cl1 Nb1 Cl2 96.67(15) . . ?
Cl1 Nb1 Cl2 95.98(15) 6_464 . ?
S1 Nb1 Cl2 100.06(18) 6_464 6_464 ?
S1 Nb1 Cl2 93.97(18) . 6_464 ?
Cl1 Nb1 Cl2 95.98(15) . 6_464 ?
Cl1 Nb1 Cl2 96.67(15) 6_464 6_464 ?
Cl2 Nb1 Cl2 157.79(4) . 6_464 ?
S1 Nb1 Se1 89.90(8) 6_464 6_464 ?
S1 Nb1 Se1 167.64(11) . 6_464 ?
Cl1 Nb1 Se1 85.29(6) . 6_464 ?
Cl1 Nb1 Se1 164.32(7) 6_464 6_464 ?
Cl2 Nb1 Se1 83.856(18) . 6_464 ?
Cl2 Nb1 Se1 79.068(18) 6_464 6_464 ?
S1 Nb1 Se1 167.64(11) 6_464 . ?
S1 Nb1 Se1 89.90(8) . . ?
Cl1 Nb1 Se1 164.32(7) . . ?
Cl1 Nb1 Se1 85.29(6) 6_464 . ?
Cl2 Nb1 Se1 79.067(18) . . ?
Cl2 Nb1 Se1 83.855(18) 6_464 . ?
Se1 Nb1 Se1 79.274(13) 6_464 . ?
C1 Se1 C2 95.77(12) . . ?
C1 Se1 Nb1 103.35(9) . . ?
C2 Se1 Nb1 104.10(8) . . ?
S1 Cl1 Nb1 61(3) 6_464 . ?
Cl1 S1 Nb1 114(2) 6_464 . ?
Se1 C1 H1A 109.5 . . ?
Se1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Se1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 Se1 112.08(18) . . ?
C3 C2 H2A 109.2 . . ?
Se1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
Se1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C2 C3 C2 114.6(3) . 6_464 ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 6_464 . ?
C2 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 6_464 . ?
H3A C3 H3B 107.6 . . ?

_refine_diff_density_max         0.727
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.146

####################################################################### 
# 
# 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_2016_2804r3
_database_code_depnum_ccdc_archive 'CCDC 1542831'
_audit_update_record             
;
2017-04-07 deposited with the CCDC.
2017-06-26 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         'C2 H6 Cl3 Nb1 S2'
_chemical_formula_sum            'C2 H6 Cl3 Nb S2'
_chemical_formula_weight         293.45

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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   7.2513(5)
_cell_length_b                   13.0295(6)
_cell_length_c                   9.8715(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.075(7)
_cell_angle_gamma                90
_cell_volume                     886.64(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4910
_cell_measurement_theta_min      2.6540
_cell_measurement_theta_max      31.9800

_exptl_crystal_description       Chip
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.641
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            7662
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.170
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3468
_reflns_number_gt                3159
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.986
_reflns_Friedel_fraction_full    0.991

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

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0385P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1313 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.14(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3468
_refine_ls_number_parameters     149
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0725
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.71536(11) 0.25361(5) 0.96161(8) 0.0174(2) Uani 1 1 d . . . . .
Nb2 Nb 0.28051(11) 0.28810(5) 0.56396(8) 0.0175(2) Uani 1 1 d . . . . .
S1 S 1.0198(3) 0.24049(17) 1.0613(3) 0.0226(5) Uani 1 1 d . . . . .
S2 S 0.7007(3) 0.05920(16) 0.8767(2) 0.0171(5) Uani 1 1 d . . . . .
S3 S -0.0174(3) 0.25839(18) 0.4573(2) 0.0231(5) Uani 1 1 d . . . . .
S4 S 0.3722(3) 0.09412(16) 0.5331(2) 0.0177(5) Uani 1 1 d . . . . .
Cl1 Cl 0.6989(3) 0.28055(15) 0.7156(2) 0.0178(4) Uani 1 1 d . . . . .
Cl2 Cl 0.6563(3) 0.42628(16) 0.9904(2) 0.0240(5) Uani 1 1 d . . . . .
Cl3 Cl 0.5900(3) 0.18643(17) 1.1306(2) 0.0226(5) Uani 1 1 d . . . . .
Cl4 Cl 0.3049(3) 0.23107(15) 0.8006(2) 0.0191(5) Uani 1 1 d . . . . .
Cl5 Cl 0.2852(3) 0.46091(16) 0.6242(2) 0.0217(5) Uani 1 1 d . . . . .
Cl6 Cl 0.4102(3) 0.31135(15) 0.3785(2) 0.0211(5) Uani 1 1 d . . . . .
C1 C 0.8730(12) 0.0438(6) 0.7820(9) 0.0200(19) Uani 1 1 d . . . . .
H1A H 0.9952 0.0771 0.8352 0.030 Uiso 1 1 calc R U . . .
H1B H 0.8223 0.0754 0.6876 0.030 Uiso 1 1 calc R U . . .
H1C H 0.8958 -0.0294 0.7714 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8221(12) -0.0136(6) 1.0345(9) 0.023(2) Uani 1 1 d . . . . .
H2A H 0.8091 -0.0871 1.0123 0.035 Uiso 1 1 calc R U . . .
H2B H 0.7633 0.0017 1.1093 0.035 Uiso 1 1 calc R U . . .
H2C H 0.9598 0.0050 1.0678 0.035 Uiso 1 1 calc R U . . .
C3 C 0.2585(13) 0.0648(7) 0.3472(10) 0.026(2) Uani 1 1 d . . . . .
H3A H 0.2780 -0.0080 0.3304 0.040 Uiso 1 1 calc R U . . .
H3B H 0.3166 0.1070 0.2890 0.040 Uiso 1 1 calc R U . . .
H3C H 0.1193 0.0793 0.3213 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2285(12) 0.0133(6) 0.6084(10) 0.023(2) Uani 1 1 d . . . . .
H4A H 0.0907 0.0290 0.5637 0.034 Uiso 1 1 calc R U . . .
H4B H 0.2636 0.0258 0.7112 0.034 Uiso 1 1 calc R U . . .
H4C H 0.2526 -0.0588 0.5913 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 S1 2.127(2) . ?
Nb1 Cl3 2.305(2) . ?
Nb1 Cl2 2.324(2) . ?
Nb1 Cl1 2.420(2) . ?
Nb1 S2 2.660(2) . ?
Nb1 Cl4 2.921(2) . ?
Nb2 S3 2.124(2) . ?
Nb2 Cl6 2.323(2) . ?
Nb2 Cl5 2.326(2) . ?
Nb2 Cl4 2.405(2) . ?
Nb2 S4 2.655(2) . ?
Nb2 Cl1 2.939(2) . ?
S2 C1 1.789(8) . ?
S2 C2 1.803(9) . ?
S4 C4 1.797(8) . ?
S4 C3 1.804(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Nb1 Cl3 102.72(9) . . ?
S1 Nb1 Cl2 103.03(9) . . ?
Cl3 Nb1 Cl2 98.64(8) . . ?
S1 Nb1 Cl1 101.37(8) . . ?
Cl3 Nb1 Cl1 150.86(9) . . ?
Cl2 Nb1 Cl1 91.64(8) . . ?
S1 Nb1 S2 90.21(8) . . ?
Cl3 Nb1 S2 83.11(7) . . ?
Cl2 Nb1 S2 165.82(9) . . ?
Cl1 Nb1 S2 80.64(7) . . ?
S1 Nb1 Cl4 168.43(8) . . ?
Cl3 Nb1 Cl4 77.98(7) . . ?
Cl2 Nb1 Cl4 88.20(7) . . ?
Cl1 Nb1 Cl4 75.16(6) . . ?
S2 Nb1 Cl4 78.37(6) . . ?
S3 Nb2 Cl6 103.38(9) . . ?
S3 Nb2 Cl5 103.59(9) . . ?
Cl6 Nb2 Cl5 95.63(8) . . ?
S3 Nb2 Cl4 100.49(8) . . ?
Cl6 Nb2 Cl4 151.64(8) . . ?
Cl5 Nb2 Cl4 93.43(8) . . ?
S3 Nb2 S4 91.27(9) . . ?
Cl6 Nb2 S4 81.76(7) . . ?
Cl5 Nb2 S4 165.11(9) . . ?
Cl4 Nb2 S4 82.63(7) . . ?
S3 Nb2 Cl1 167.58(8) . . ?
Cl6 Nb2 Cl1 78.42(7) . . ?
Cl5 Nb2 Cl1 88.36(7) . . ?
Cl4 Nb2 Cl1 75.03(6) . . ?
S4 Nb2 Cl1 76.75(6) . . ?
C1 S2 C2 99.2(4) . . ?
C1 S2 Nb1 107.8(3) . . ?
C2 S2 Nb1 105.5(3) . . ?
C4 S4 C3 99.0(4) . . ?
C4 S4 Nb2 108.2(3) . . ?
C3 S4 Nb2 105.5(3) . . ?
Nb1 Cl1 Nb2 103.75(6) . . ?
Nb2 Cl4 Nb1 104.65(7) . . ?
S2 C1 H1A 109.5 . . ?
S2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S2 C2 H2A 109.5 . . ?
S2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S4 C3 H3A 109.5 . . ?
S4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S4 C4 H4A 109.5 . . ?
S4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         0.807
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_2016_1407r1
_database_code_depnum_ccdc_archive 'CCDC 1542833'
_audit_update_record             
;
2017-04-07 deposited with the CCDC.
2017-06-26 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         'C8 H18 Cl3 Nb S3'
_chemical_formula_sum            'C8 H18 Cl3 Nb S3'
_chemical_formula_weight         409.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   8.7791(2)
_cell_length_b                   9.1658(2)
_cell_length_c                   19.6825(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.753(2)
_cell_angle_gamma                90
_cell_volume                     1565.36(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7205
_cell_measurement_theta_min      2.1630
_cell_measurement_theta_max      32.2310

_exptl_crystal_description       block
_exptl_crystal_colour            'Yellow Green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.083
_exptl_absorpt_coefficient_mu    1.652
_shelx_estimated_absorpt_T_min   0.756
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            14369
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.347
_diffrn_reflns_theta_max         32.323
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5181
_reflns_number_gt                4254
_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       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+1.2705P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5181
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Nb1 Nb 0.30719(3) 0.74925(2) 0.35846(2) 0.02090(7) Uani 1 1 d . . . . .
Cl1 Cl 0.27103(9) 0.96344(7) 0.30276(4) 0.03082(15) Uani 1 1 d . . . . .
Cl2 Cl 0.53605(6) 0.67979(7) 0.31798(3) 0.01977(12) Uani 1 1 d . . . . .
Cl3 Cl 0.05194(7) 0.71679(7) 0.38004(3) 0.02328(13) Uani 1 1 d . . . . .
S1 S 0.16050(7) 0.62013(7) 0.23818(3) 0.01744(12) Uani 1 1 d . . . . .
S2 S 0.33464(7) 0.45840(6) 0.39160(3) 0.01587(12) Uani 1 1 d . . . . .
S3 S 0.40943(8) 0.81178(8) 0.46405(3) 0.02853(15) Uani 1 1 d . . . . .
C1 C 0.2248(3) 0.5016(3) 0.11543(12) 0.0225(5) Uani 1 1 d . . . . .
H1A H 0.1203 0.5318 0.0958 0.034 Uiso 1 1 calc R U . . .
H1B H 0.2219 0.4026 0.1341 0.034 Uiso 1 1 calc R U . . .
H1C H 0.2909 0.5029 0.0796 0.034 Uiso 1 1 calc R U . . .
C2 C 0.2888(3) 0.6061(3) 0.17270(12) 0.0194(5) Uani 1 1 d . . . . .
H2 H 0.3928 0.5718 0.1947 0.023 Uiso 1 1 calc R U . . .
C3 C 0.3013(4) 0.7601(3) 0.14545(14) 0.0290(6) Uani 1 1 d . . . . .
H3A H 0.3716 0.7605 0.1112 0.044 Uiso 1 1 calc R U . . .
H3B H 0.3412 0.8253 0.1835 0.044 Uiso 1 1 calc R U . . .
H3C H 0.1993 0.7937 0.1241 0.044 Uiso 1 1 calc R U . . .
C4 C 0.1410(3) 0.4337(3) 0.26582(12) 0.0229(5) Uani 1 1 d . . . . .
H4A H 0.0557 0.4286 0.2934 0.027 Uiso 1 1 calc R U . . .
H4B H 0.1128 0.3713 0.2248 0.027 Uiso 1 1 calc R U . . .
C5 C 0.2857(3) 0.3734(3) 0.30810(12) 0.0223(5) Uani 1 1 d . . . . .
H5A H 0.3728 0.3865 0.2821 0.027 Uiso 1 1 calc R U . . .
H5B H 0.2721 0.2674 0.3146 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1771(3) 0.2291(3) 0.44154(15) 0.0270(6) Uani 1 1 d . . . . .
H6A H 0.2789 0.1911 0.4606 0.040 Uiso 1 1 calc R U . . .
H6B H 0.1468 0.1910 0.3949 0.040 Uiso 1 1 calc R U . . .
H6C H 0.1016 0.1986 0.4706 0.040 Uiso 1 1 calc R U . . .
C7 C 0.1831(3) 0.3941(3) 0.43916(12) 0.0181(4) Uani 1 1 d . . . . .
H7 H 0.0812 0.4318 0.4162 0.022 Uiso 1 1 calc R U . . .
C8 C 0.2199(3) 0.4611(3) 0.51047(12) 0.0239(5) Uani 1 1 d . . . . .
H8A H 0.1442 0.4278 0.5389 0.036 Uiso 1 1 calc R U . . .
H8B H 0.2159 0.5677 0.5067 0.036 Uiso 1 1 calc R U . . .
H8C H 0.3233 0.4309 0.5317 0.036 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 S3 2.2105(7) . ?
Nb1 Cl1 2.2475(7) . ?
Nb1 Cl2 2.3588(6) . ?
Nb1 Cl3 2.3623(6) . ?
Nb1 S2 2.7464(6) . ?
Nb1 S1 2.7813(6) . ?
S1 C4 1.810(3) . ?
S1 C2 1.841(2) . ?
S2 C5 1.810(2) . ?
S2 C7 1.837(2) . ?
C1 C2 1.520(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.520(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.513(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.514(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.521(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S3 Nb1 Cl1 103.84(3) . . ?
S3 Nb1 Cl2 98.20(2) . . ?
Cl1 Nb1 Cl2 97.78(2) . . ?
S3 Nb1 Cl3 97.13(3) . . ?
Cl1 Nb1 Cl3 97.49(3) . . ?
Cl2 Nb1 Cl3 155.07(2) . . ?
S3 Nb1 S2 91.14(2) . . ?
Cl1 Nb1 S2 164.70(2) . . ?
Cl2 Nb1 S2 76.69(2) . . ?
Cl3 Nb1 S2 83.48(2) . . ?
S3 Nb1 S1 168.47(2) . . ?
Cl1 Nb1 S1 86.78(2) . . ?
Cl2 Nb1 S1 84.58(2) . . ?
Cl3 Nb1 S1 76.73(2) . . ?
S2 Nb1 S1 78.559(18) . . ?
C4 S1 C2 103.91(12) . . ?
C4 S1 Nb1 101.47(8) . . ?
C2 S1 Nb1 111.85(8) . . ?
C5 S2 C7 103.55(12) . . ?
C5 S2 Nb1 101.64(8) . . ?
C7 S2 Nb1 112.86(8) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 111.2(2) . . ?
C3 C2 S1 105.48(18) . . ?
C1 C2 S1 111.51(17) . . ?
C3 C2 H2 109.5 . . ?
C1 C2 H2 109.5 . . ?
S1 C2 H2 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 S1 113.57(17) . . ?
C5 C4 H4A 108.9 . . ?
S1 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
S1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C4 C5 S2 113.95(17) . . ?
C4 C5 H5A 108.8 . . ?
S2 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
S2 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 C7 C8 112.2(2) . . ?
C6 C7 S2 111.57(18) . . ?
C8 C7 S2 105.79(16) . . ?
C6 C7 H7 109.1 . . ?
C8 C7 H7 109.1 . . ?
S2 C7 H7 109.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_refine_diff_density_max         0.659
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.123

