# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2014slbrmlh1_ml

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2014-03-11
_chemical_name_systematic        
;
Tantalum pentachloride dimethyltelluride
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 Cl5 Ta Te'
_chemical_formula_sum            'C2 H6 Cl5 Ta Te'
_chemical_formula_weight         515.87

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'
Te Te -0.5308 1.6751 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'C mc21'
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   8.023(5)
_cell_length_b                   11.998(7)
_cell_length_c                   10.752(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1034.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1866
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    14.601
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_source                   'Rotating Anode'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            1827
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.1208
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.02
_reflns_number_total             929
_reflns_number_gt                864
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.

Weak data necessitated the use of DELU and SIMU restraints on all atoms, and the use
of the ISOR restraint on C1 to ensure appropriate anisotropic displacement parameters.

The largest residual electron density peak (3.24 e/Å3) is located 1.0 Å from Ta1, directly
between Ta1 and Cl2, and is most likely unassigned electron density from these heavy atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+97.1963P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_number_reflns         929
_refine_ls_number_parameters     49
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1645
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.121
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.0000 0.78977(10) 0.69580(7) 0.0227(4) Uani 1 2 d SU . .
Te1 Te 0.0000 0.55077(17) 0.6262(2) 0.0272(6) Uani 1 2 d SU . .
Cl1 Cl 0.0000 0.9751(7) 0.7465(9) 0.034(2) Uani 1 2 d SU . .
Cl2 Cl -0.2853(7) 0.7663(5) 0.6935(8) 0.0306(12) Uani 1 1 d U . .
Cl3 Cl 0.0000 0.8182(8) 0.4845(8) 0.035(2) Uani 1 2 d SU . .
Cl4 Cl 0.0000 0.7250(8) 0.8974(9) 0.035(2) Uani 1 2 d SU . .
C1 C -0.197(4) 0.549(2) 0.489(3) 0.032(5) Uani 1 1 d U . .
H1A H -0.3051 0.5501 0.5314 0.048 Uiso 1 1 calc R . .
H1B H -0.1876 0.4820 0.4382 0.048 Uiso 1 1 calc R . .
H1C H -0.1870 0.6153 0.4361 0.048 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ta1 0.0417(8) 0.0097(6) 0.0167(7) 0.0004(5) 0.000 0.000
Te1 0.0515(17) 0.0106(11) 0.0194(11) 0.0025(9) 0.000 0.000
Cl1 0.068(7) 0.010(3) 0.023(4) -0.001(3) 0.000 0.000
Cl2 0.033(3) 0.032(3) 0.026(3) -0.005(3) -0.003(4) -0.001(2)
Cl3 0.074(8) 0.013(4) 0.018(4) 0.000(3) 0.000 0.000
Cl4 0.070(7) 0.017(5) 0.018(4) 0.003(3) 0.000 0.000
C1 0.028(9) 0.033(9) 0.034(9) -0.007(7) 0.004(6) -0.004(8)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 Cl1 2.290(9) . ?
Ta1 Cl3 2.298(9) . ?
Ta1 Cl4 2.303(10) . ?
Ta1 Cl2 2.306(6) . ?
Ta1 Cl2 2.306(6) 4 ?
Ta1 Te1 2.964(3) . ?
Te1 C1 2.16(3) . ?
Te1 C1 2.16(3) 4 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 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
Cl1 Ta1 Cl3 95.2(3) . . ?
Cl1 Ta1 Cl4 95.9(3) . . ?
Cl3 Ta1 Cl4 168.8(3) . . ?
Cl1 Ta1 Cl2 96.95(15) . . ?
Cl3 Ta1 Cl2 90.4(2) . . ?
Cl4 Ta1 Cl2 88.2(2) . . ?
Cl1 Ta1 Cl2 96.95(15) . 4 ?
Cl3 Ta1 Cl2 90.4(2) . 4 ?
Cl4 Ta1 Cl2 88.2(2) . 4 ?
Cl2 Ta1 Cl2 165.9(3) . 4 ?
Cl1 Ta1 Te1 179.1(2) . . ?
Cl3 Ta1 Te1 83.9(2) . . ?
Cl4 Ta1 Te1 84.9(2) . . ?
Cl2 Ta1 Te1 83.06(15) . . ?
Cl2 Ta1 Te1 83.06(15) 4 . ?
C1 Te1 C1 94.0(16) . 4 ?
C1 Te1 Ta1 100.4(7) . . ?
C1 Te1 Ta1 100.4(7) 4 . ?
Te1 C1 H1A 109.5 . . ?
Te1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Te1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.240
_refine_diff_density_min         -3.689
_refine_diff_density_rms         0.448
_database_code_depnum_ccdc_archive 'CCDC 1022738'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2014slbRmlh2b
_audit_creation_date             2014-09-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_formula_moiety         'Cl6 Ta, C7 H15 Te2'
_chemical_formula_sum            'C7 H15 Cl6 Ta Te2'
_chemical_formula_weight         748.07
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Te -0.41592 1.76401 19.96440 19.01380 6.14487 2.52390 4.81742 0.42088 28.52840
70.84030 4.35200023651
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14874 0.16030 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ta -0.58482 6.58170 29.20240 15.22930 14.51350 4.76492 1.77333 9.37046 0.29598
63.36440 9.24353981018
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   7.433(1)
_cell_length_b                   9.1611(12)
_cell_length_c                   25.663(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.217(6)
_cell_angle_gamma                90
_cell_volume                     1747.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6499
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_exptl_absorpt_coefficient_mu    10.455
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.8432
_exptl_crystal_description       plate
_exptl_crystal_F_000             1342.5254
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.2056
_diffrn_reflns_av_unetI/netI     0.2260
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11709
_diffrn_reflns_theta_full        25.9994
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9189
_diffrn_measured_fraction_theta_max 0.9189
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -107.0000 - 73.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: -120.0000
	             XTD: 45.0000
	          2theta: -17.0000
scan:
	Number of images: 31
	           Slice: -71.0000 - -40.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -150.0000
	             XTD: 45.0000
	          2theta: -17.0000
scan:
	Number of images: 87
	           Slice: -107.0000 - -20.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: -150.0000
	             XTD: 45.0000
	          2theta: -17.0000
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.073260
_diffrn_orient_matrix_UB_12      -0.023161
_diffrn_orient_matrix_UB_13      -0.031700
_diffrn_orient_matrix_UB_21      0.040243
_diffrn_orient_matrix_UB_22      -0.104025
_diffrn_orient_matrix_UB_23      0.001932
_diffrn_orient_matrix_UB_31      -0.105420
_diffrn_orient_matrix_UB_32      -0.023615
_diffrn_orient_matrix_UB_33      0.022579
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                1564
_reflns_number_total             3163
_reflns_threshold_expression     I>=2u(I)
_reflns_special_details          
;
The data images collected were weak and showed evidence of twinning, 
which could not be resolved during integration and resulted in high Rint
and low data completeness. Solution and refinement allowed structure 
determination but positions of lighter atoms could not be determined exactly.
This data allowed structural identification but structural parameters were not
analysed due to these limitations.
;
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         4.9476
_refine_diff_density_min         -4.8853
_refine_diff_density_rms         1.1828
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.4423
_refine_ls_goodness_of_fit_ref   1.0588
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3163
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.2054
_refine_ls_R_factor_gt           0.1048
_refine_ls_restrained_S_all      1.0449
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0790P)²+50.1550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2439
_refine_special_details          
;
DELU, SIMU and ISOR restraints were used for all C atoms. Several large residual electron
density peaks (max 4.95 e/Å3) remain after refinement, but could not be modelled chemically
and are often in close proximity to heavy atoms. Their presence was attributed to the poor 
data quality.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C6, C4, C7, C5, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C4 \\sim C7 \\sim C5 \\sim C1 \\sim C2 \\sim C3: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b)
4.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C7(H7a,H7b,H7c), C6(H6a,H6b,H6c)
;
_atom_sites_solution_primary     heavy
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_refinement_flags_posn
_atom_site_refinement_flags_adp
Ta1 Ta 0.03894(18) 1.70259(16) 0.36736(5) 0.0327(4) Uani 1.000000 . .
Te1 Te 0.6568(3) 1.1938(3) 0.47551(9) 0.0421(7) Uani 1.000000 . .
Te2 Te 0.5160(3) 1.0677(3) 0.38930(9) 0.0376(6) Uani 1.000000 . .
Cl3 Cl -0.0747(12) 1.5409(10) 0.4282(3) 0.047(2) Uani 1.000000 . .
Cl1 Cl 0.0926(12) 1.5161(10) 0.3089(3) 0.045(2) Uani 1.000000 . .
Cl2 Cl -0.2437(11) 1.7413(10) 0.3311(4) 0.049(2) Uani 1.000000 . .
Cl4 Cl 0.1674(11) 1.8766(9) 0.3107(3) 0.037(2) Uani 1.000000 . .
Cl5 Cl -0.0172(12) 1.8947(10) 0.4273(3) 0.043(2) Uani 1.000000 . .
Cl6 Cl 0.3293(11) 1.6704(10) 0.4034(3) 0.045(2) Uani 1.000000 . .
C4 C 0.619(4) 1.206(4) 0.3265(13) 0.040(5) Uani 1.000000 . U
C3 C 0.259(4) 1.195(4) 0.4044(13) 0.043(6) Uani 1.000000 . U
C5 C 0.596(4) 1.367(4) 0.3332(13) 0.040(5) Uani 1.000000 . U
H5a H 0.473(9) 1.395(5) 0.323(7) 0.060(8) Uiso 1.000000 GR .
H5b H 0.62(3) 1.393(5) 0.370(2) 0.060(8) Uiso 1.000000 GR .
H5c H 0.682(18) 1.419(4) 0.311(6) 0.060(8) Uiso 1.000000 GR .
C1 C 0.409(4) 1.307(4) 0.4815(14) 0.048(6) Uani 1.000000 . U
H1a H 0.383(4) 1.325(4) 0.5188(14) 0.057(8) Uiso 1.000000 R .
H1b H 0.421(4) 1.403(4) 0.4643(14) 0.057(8) Uiso 1.000000 R .
C7 C 0.528(5) 1.141(4) 0.2763(13) 0.044(5) Uani 1.000000 . U
H7a H 0.55(2) 1.036(5) 0.275(4) 0.066(8) Uiso 1.000000 GR .
H7b H 0.399(6) 1.162(19) 0.277(4) 0.066(8) Uiso 1.000000 GR .
H7c H 0.582(19) 1.186(16) 0.2453(13) 0.066(8) Uiso 1.000000 GR .
C2 C 0.256(5) 1.228(4) 0.4579(14) 0.046(6) Uani 1.000000 . U
C6 C 0.820(4) 1.162(4) 0.3238(14) 0.042(5) Uani 1.000000 . U
H6a H 0.881(7) 1.19(2) 0.356(3) 0.064(8) Uiso 1.000000 GR .
H6b H 0.830(4) 1.057(5) 0.319(8) 0.064(8) Uiso 1.000000 GR .
H6c H 0.877(8) 1.213(18) 0.295(5) 0.064(8) Uiso 1.000000 GR .
H2a H 0.146(5) 1.287(4) 0.4644(14) 0.056(7) Uiso 1.000000 R .
H2b H 0.241(5) 1.135(4) 0.4771(14) 0.056(7) Uiso 1.000000 R .
H3a H 0.258(4) 1.285(4) 0.3834(13) 0.051(7) Uiso 1.000000 R .
H3b H 0.153(4) 1.135(4) 0.3947(13) 0.051(7) Uiso 1.000000 R .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ta1 0.0300(8) 0.0461(9) 0.0218(8) -0.0037(7) -0.0103(6) -0.0006(7)
Te1 0.0395(14) 0.0556(16) 0.0311(14) -0.0051(12) -0.0152(10) 0.0046(12)
Te2 0.0383(13) 0.0488(15) 0.0255(12) -0.0053(11) -0.0096(10) 0.0001(11)
Cl3 0.055(6) 0.055(6) 0.030(5) -0.011(5) 0.006(4) 0.004(4)
Cl1 0.045(5) 0.053(6) 0.036(5) 0.001(4) -0.015(4) -0.002(4)
Cl2 0.030(5) 0.061(7) 0.057(6) 0.001(4) -0.016(4) -0.006(5)
Cl4 0.034(5) 0.049(5) 0.029(5) -0.002(4) -0.004(4) 0.003(4)
Cl5 0.054(5) 0.051(6) 0.025(5) -0.002(4) -0.002(4) -0.006(4)
Cl6 0.040(5) 0.057(6) 0.038(5) 0.001(4) -0.021(4) 0.000(4)
C4 0.040(7) 0.041(7) 0.040(7) -0.001(3) -0.003(3) 0.002(3)
C3 0.039(9) 0.042(9) 0.046(8) -0.001(4) -0.002(4) 0.004(4)
C5 0.039(8) 0.041(7) 0.040(8) -0.002(4) -0.001(4) 0.004(4)
C1 0.045(9) 0.051(9) 0.047(8) -0.001(4) -0.000(4) 0.000(4)
C7 0.046(8) 0.044(8) 0.042(8) -0.000(4) -0.003(4) 0.000(4)
C2 0.044(8) 0.047(8) 0.048(8) -0.000(3) 0.000(3) 0.002(3)
C6 0.043(7) 0.043(8) 0.041(8) 0.000(4) -0.003(4) 0.001(4)

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 Cl3 2.314(8) . ?
Ta1 Cl1 2.310(9) . ?
Ta1 Cl2 2.322(9) . ?
Ta1 Cl4 2.362(8) . ?
Ta1 Cl5 2.376(8) . ?
Ta1 Cl6 2.363(8) . ?
Te1 Te2 2.703(3) . ?
Te1 C1 2.12(3) . ?
Te2 C4 2.19(3) . ?
Te2 C3 2.27(3) . ?
C4 C5 1.50(4) . ?
C4 C7 1.57(5) . ?
C4 C6 1.55(4) . ?
C3 C2 1.41(4) . ?
C3 H3a 0.9900 . ?
C3 H3b 0.9900 . ?
C5 H5a 0.9800 . ?
C5 H5b 0.9800 . ?
C5 H5c 0.9800 . ?
C1 H1a 0.9900 . ?
C1 H1b 0.9900 . ?
C1 C2 1.48(5) . ?
C7 H7a 0.9800 . ?
C7 H7b 0.9800 . ?
C7 H7c 0.9800 . ?
C2 H2a 0.9900 . ?
C2 H2b 0.9900 . ?
C6 H6a 0.9800 . ?
C6 H6b 0.9800 . ?
C6 H6c 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
Cl1 Ta1 Cl3 91.7(3) . . ?
Cl2 Ta1 Cl3 92.1(3) . . ?
Cl2 Ta1 Cl1 90.6(3) . . ?
Cl4 Ta1 Cl3 175.5(3) . . ?
Cl4 Ta1 Cl1 91.6(3) . . ?
Cl4 Ta1 Cl2 91.0(3) . . ?
Cl5 Ta1 Cl3 88.4(3) . . ?
Cl5 Ta1 Cl1 179.8(3) . . ?
Cl5 Ta1 Cl2 89.2(3) . . ?
Cl5 Ta1 Cl4 88.4(3) . . ?
Cl6 Ta1 Cl3 89.5(3) . . ?
Cl6 Ta1 Cl1 90.1(3) . . ?
Cl6 Ta1 Cl2 178.2(3) . . ?
Cl6 Ta1 Cl4 87.4(3) . . ?
Cl6 Ta1 Cl5 90.1(3) . . ?
C1 Te1 Te2 86.3(10) . . ?
C4 Te2 Te1 102.7(9) . . ?
C3 Te2 Te1 88.0(9) . . ?
C3 Te2 C4 97.2(12) . . ?
C5 C4 Te2 116(2) . . ?
C7 C4 Te2 104(2) . . ?
C7 C4 C5 115(3) . . ?
C6 C4 Te2 103(2) . . ?
C6 C4 C5 112(3) . . ?
C6 C4 C7 106(3) . . ?
C2 C3 Te2 107(2) . . ?
H3a C3 Te2 110.2(9) . . ?
H3a C3 C2 110(2) . . ?
H3b C3 Te2 110.2(9) . . ?
H3b C3 C2 110.2(19) . . ?
H3b C3 H3a 108.51830603(2) . . ?
H5a C5 C4 109.5 . . ?
H5b C5 C4 109.5 . . ?
H5b C5 H5a 109.5 . . ?
H5c C5 C4 109.5 . . ?
H5c C5 H5a 109.5 . . ?
H5c C5 H5b 109.5 . . ?
H1a C1 Te1 108.9(10) . . ?
H1b C1 Te1 108.9(10) . . ?
H1b C1 H1a 107.70747193(3) . . ?
C2 C1 Te1 114(2) . . ?
C2 C1 H1a 108.9(19) . . ?
C2 C1 H1b 109(2) . . ?
H7a C7 C4 109.5 . . ?
H7b C7 C4 109.5 . . ?
H7b C7 H7a 109.5 . . ?
H7c C7 C4 109.5 . . ?
H7c C7 H7a 109.5 . . ?
H7c C7 H7b 109.5 . . ?
C1 C2 C3 119(3) . . ?
H2a C2 C3 107.5(19) . . ?
H2a C2 C1 107.5(19) . . ?
H2b C2 C3 107(2) . . ?
H2b C2 C1 107(2) . . ?
H2b C2 H2a 106.987676771(15) . . ?
H6a C6 C4 109.5 . . ?
H6b C6 C4 109.5 . . ?
H6b C6 H6a 109.5 . . ?
H6c C6 C4 109.5 . . ?
H6c C6 H6a 109.5 . . ?
H6c C6 H6b 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
C4 0.0100
C3 0.0100
C5 0.0100
C1 0.0100
C7 0.0100
C2 0.0100
C6 0.0100

loop_
_restr_U_rigid_atom_site_label_1
_restr_U_rigid_atom_site_label_2
_restr_U_rigid_target_weight_param
_restr_U_rigid_U_parallel
_restr_U_rigid_diff
C4 C5 0.0100 0.0421 -0.0005
C4 C7 0.0100 0.0395 -0.0018
C4 C6 0.0100 0.0421 -0.0015
C3 C1 0.0100 0.0456 -0.0019
C3 C2 0.0100 0.0483 -0.0008
C5 C7 0.0100 0.0429 0.0006
C5 C6 0.0100 0.0430 -0.0007
C1 C2 0.0100 0.0459 -0.0004
C7 C6 0.0100 0.0406 0.0023

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
C4 C5 0.0100
C4 C7 0.0100
C4 C6 0.0100
C3 C2 0.0100
C1 C2 0.0100
_database_code_depnum_ccdc_archive 'CCDC 1022739'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2013slbkmlh2x

_audit_creation_method           'SHELXL-97  hand edit'
_audit_creation_date             2013-10-22
_chemical_name_systematic        
;
alpha,alpha-bis(ethylthio)-o-xylene di(tantalum pentachloride)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H18 Cl10 S2 Ta2'
_chemical_formula_sum            'C12 H18 Cl10 S2 Ta2'
_chemical_formula_weight         942.78

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   12.437(5)
_cell_length_b                   17.574(3)
_cell_length_c                   11.745(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.859(7)
_cell_angle_gamma                90.00
_cell_volume                     2536.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11807
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    9.840
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_source                   'Rotating Anode'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            12901
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5770
_reflns_number_gt                5218
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.

The largest residual electron density peaks indicate a small amount 
of disorder around the Ta centre, similar to that seen in the 
isomorphous structure reported for M = Nb in this nmanuscript (data_ypc2x).
In the present case a satisfactory structure was obtained without modelling 
this very minor disorder component, the size of the residual peaks being small enough to suggest a very 
low occupancy of the second part. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0349P)²+37.0643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         5770
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.369548(19) 0.343781(13) 0.79534(2) 0.01188(8) Uani 1 1 d . . .
Ta2 Ta -0.15612(2) 0.154100(15) 0.89130(2) 0.01926(8) Uani 1 1 d . . .
Cl1 Cl 0.27136(13) 0.33982(9) 0.61252(13) 0.0196(3) Uani 1 1 d . . .
Cl2 Cl 0.52249(12) 0.31105(9) 0.71690(13) 0.0184(3) Uani 1 1 d . . .
Cl3 Cl 0.46585(12) 0.31713(9) 0.97898(12) 0.0164(3) Uani 1 1 d . . .
Cl4 Cl 0.40076(14) 0.47109(9) 0.80958(15) 0.0219(3) Uani 1 1 d . . .
Cl5 Cl 0.20593(13) 0.34799(9) 0.86941(14) 0.0199(3) Uani 1 1 d . . .
Cl6 Cl -0.05990(15) 0.24855(11) 0.81337(19) 0.0324(4) Uani 1 1 d . . .
Cl7 Cl -0.27570(14) 0.14902(11) 0.71849(16) 0.0275(4) Uani 1 1 d . . .
Cl8 Cl -0.23190(16) 0.04105(10) 0.94671(16) 0.0299(4) Uani 1 1 d . . .
Cl9 Cl -0.01283(14) 0.14110(11) 1.04206(16) 0.0271(4) Uani 1 1 d . . .
Cl10 Cl -0.26158(15) 0.23084(12) 0.98224(19) 0.0352(4) Uani 1 1 d . . .
S1 S 0.33234(12) 0.19499(8) 0.81464(13) 0.0128(3) Uani 1 1 d . . .
S2 S -0.03596(14) 0.05158(10) 0.79332(17) 0.0253(4) Uani 1 1 d . . .
C1 C 0.4600(6) 0.0730(4) 0.9025(6) 0.0245(14) Uani 1 1 d . . .
H1A H 0.4442 0.0879 0.9786 0.037 Uiso 1 1 calc R . .
H1B H 0.5314 0.0482 0.9109 0.037 Uiso 1 1 calc R . .
H1C H 0.4041 0.0376 0.8665 0.037 Uiso 1 1 calc R . .
C2 C 0.4608(5) 0.1438(4) 0.8267(6) 0.0164(12) Uani 1 1 d . . .
H2A H 0.4740 0.1285 0.7489 0.020 Uiso 1 1 calc R . .
H2B H 0.5208 0.1778 0.8602 0.020 Uiso 1 1 calc R . .
C3 C 0.2592(5) 0.1603(3) 0.6771(5) 0.0155(12) Uani 1 1 d . . .
H3A H 0.1869 0.1849 0.6611 0.019 Uiso 1 1 calc R . .
H3B H 0.3003 0.1738 0.6142 0.019 Uiso 1 1 calc R . .
C4 C 0.2453(5) 0.0749(3) 0.6808(5) 0.0145(12) Uani 1 1 d . . .
C5 C 0.3092(5) 0.0302(4) 0.6189(5) 0.0170(12) Uani 1 1 d . . .
H5 H 0.3556 0.0542 0.5726 0.020 Uiso 1 1 calc R . .
C6 C 0.3058(5) -0.0488(4) 0.6240(6) 0.0193(13) Uani 1 1 d . . .
H6 H 0.3493 -0.0786 0.5812 0.023 Uiso 1 1 calc R . .
C7 C 0.2387(5) -0.0839(4) 0.6920(6) 0.0191(13) Uani 1 1 d . . .
H7 H 0.2377 -0.1378 0.6977 0.023 Uiso 1 1 calc R . .
C8 C 0.1733(5) -0.0404(4) 0.7513(6) 0.0178(12) Uani 1 1 d . . .
H8 H 0.1260 -0.0652 0.7958 0.021 Uiso 1 1 calc R . .
C9 C 0.1747(5) 0.0389(4) 0.7476(6) 0.0156(12) Uani 1 1 d . . .
C10 C 0.1041(5) 0.0853(4) 0.8144(6) 0.0193(13) Uani 1 1 d . . .
H10A H 0.1053 0.1392 0.7898 0.023 Uiso 1 1 calc R . .
H10B H 0.1342 0.0830 0.8974 0.023 Uiso 1 1 calc R . .
C11 C -0.0735(6) 0.0457(5) 0.6401(8) 0.0353(19) Uani 1 1 d . . .
H11A H -0.0356 0.0016 0.6121 0.042 Uiso 1 1 calc R . .
H11B H -0.1526 0.0355 0.6227 0.042 Uiso 1 1 calc R . .
C12 C -0.0480(7) 0.1168(6) 0.5721(7) 0.039(2) Uani 1 1 d . . .
H12A H -0.0738 0.1623 0.6078 0.059 Uiso 1 1 calc R . .
H12B H -0.0848 0.1127 0.4923 0.059 Uiso 1 1 calc R . .
H12C H 0.0307 0.1205 0.5730 0.059 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ta1 0.01160(13) 0.01082(12) 0.01293(13) 0.00073(8) 0.00091(9) -0.00021(9)
Ta2 0.01399(14) 0.01747(14) 0.02747(16) 0.00357(10) 0.00688(11) 0.00311(10)
Cl1 0.0219(8) 0.0190(7) 0.0156(7) 0.0036(5) -0.0036(6) -0.0005(6)
Cl2 0.0149(7) 0.0215(7) 0.0201(7) -0.0029(6) 0.0066(6) -0.0022(6)
Cl3 0.0155(7) 0.0193(7) 0.0136(6) 0.0014(5) -0.0003(5) 0.0013(6)
Cl4 0.0248(8) 0.0108(7) 0.0292(8) 0.0010(6) 0.0008(6) -0.0024(6)
Cl5 0.0127(7) 0.0226(8) 0.0249(8) -0.0022(6) 0.0047(6) 0.0018(6)
Cl6 0.0230(8) 0.0257(9) 0.0497(11) 0.0096(8) 0.0094(8) -0.0033(7)
Cl7 0.0163(7) 0.0343(9) 0.0316(9) 0.0116(7) 0.0027(7) 0.0055(7)
Cl8 0.0332(9) 0.0225(8) 0.0315(9) 0.0039(7) -0.0025(7) -0.0074(7)
Cl9 0.0198(8) 0.0336(9) 0.0279(9) -0.0010(7) 0.0034(7) 0.0002(7)
Cl10 0.0204(8) 0.0345(10) 0.0517(12) -0.0198(9) 0.0084(8) 0.0015(7)
S1 0.0122(7) 0.0114(6) 0.0149(7) 0.0016(5) 0.0021(5) 0.0006(5)
S2 0.0203(8) 0.0211(8) 0.0346(10) 0.0005(7) 0.0045(7) 0.0001(7)
C1 0.028(4) 0.022(3) 0.022(3) 0.003(3) -0.001(3) 0.010(3)
C2 0.008(3) 0.015(3) 0.025(3) -0.002(2) -0.001(2) 0.004(2)
C3 0.017(3) 0.013(3) 0.015(3) 0.001(2) -0.001(2) 0.000(2)
C4 0.014(3) 0.013(3) 0.015(3) 0.000(2) -0.003(2) 0.001(2)
C5 0.018(3) 0.017(3) 0.016(3) -0.002(2) 0.001(2) -0.001(2)
C6 0.019(3) 0.016(3) 0.023(3) -0.005(2) 0.003(3) 0.004(2)
C7 0.021(3) 0.009(3) 0.024(3) -0.002(2) -0.005(3) 0.002(2)
C8 0.017(3) 0.015(3) 0.021(3) 0.004(2) 0.001(2) -0.003(2)
C9 0.011(3) 0.015(3) 0.021(3) -0.002(2) 0.003(2) -0.001(2)
C10 0.010(3) 0.021(3) 0.027(3) -0.006(3) 0.002(2) -0.002(2)
C11 0.017(3) 0.035(4) 0.049(5) -0.019(4) -0.012(3) 0.003(3)
C12 0.031(4) 0.053(6) 0.031(4) -0.001(4) -0.004(3) 0.005(4)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 Cl4 2.2726(16) . ?
Ta1 Cl1 2.3019(16) . ?
Ta1 Cl2 2.3102(16) . ?
Ta1 Cl5 2.3341(17) . ?
Ta1 Cl3 2.3473(15) . ?
Ta1 S1 2.6713(15) . ?
Ta2 Cl10 2.2607(18) . ?
Ta2 Cl6 2.3158(18) . ?
Ta2 Cl9 2.3219(19) . ?
Ta2 Cl7 2.3258(19) . ?
Ta2 Cl8 2.3341(18) . ?
Ta2 S2 2.7081(19) . ?
S1 C2 1.819(6) . ?
S1 C3 1.831(6) . ?
S2 C11 1.791(9) . ?
S2 C10 1.820(6) . ?
C1 C2 1.531(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.512(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.399(9) . ?
C4 C9 1.413(9) . ?
C5 C6 1.391(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.381(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.396(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.504(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.542(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
Cl4 Ta1 Cl1 99.12(6) . . ?
Cl4 Ta1 Cl2 97.63(6) . . ?
Cl1 Ta1 Cl2 88.37(6) . . ?
Cl4 Ta1 Cl5 95.17(6) . . ?
Cl1 Ta1 Cl5 88.91(6) . . ?
Cl2 Ta1 Cl5 167.18(6) . . ?
Cl4 Ta1 Cl3 94.11(6) . . ?
Cl1 Ta1 Cl3 166.74(6) . . ?
Cl2 Ta1 Cl3 88.95(6) . . ?
Cl5 Ta1 Cl3 90.84(6) . . ?
Cl4 Ta1 S1 170.88(5) . . ?
Cl1 Ta1 S1 88.60(5) . . ?
Cl2 Ta1 S1 87.37(5) . . ?
Cl5 Ta1 S1 80.04(5) . . ?
Cl3 Ta1 S1 78.30(5) . . ?
Cl10 Ta2 Cl6 97.58(8) . . ?
Cl10 Ta2 Cl9 97.55(7) . . ?
Cl6 Ta2 Cl9 89.39(7) . . ?
Cl10 Ta2 Cl7 95.49(7) . . ?
Cl6 Ta2 Cl7 89.00(7) . . ?
Cl9 Ta2 Cl7 166.96(7) . . ?
Cl10 Ta2 Cl8 95.02(8) . . ?
Cl6 Ta2 Cl8 167.36(7) . . ?
Cl9 Ta2 Cl8 89.95(7) . . ?
Cl7 Ta2 Cl8 88.81(7) . . ?
Cl10 Ta2 S2 174.81(7) . . ?
Cl6 Ta2 S2 87.50(7) . . ?
Cl9 Ta2 S2 81.35(6) . . ?
Cl7 Ta2 S2 85.65(6) . . ?
Cl8 Ta2 S2 79.93(7) . . ?
C2 S1 C3 102.4(3) . . ?
C2 S1 Ta1 109.2(2) . . ?
C3 S1 Ta1 108.7(2) . . ?
C11 S2 C10 104.6(4) . . ?
C11 S2 Ta2 112.9(3) . . ?
C10 S2 Ta2 107.7(2) . . ?
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 . . ?
C1 C2 S1 111.3(5) . . ?
C1 C2 H2A 109.4 . . ?
S1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
S1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 S1 110.4(4) . . ?
C4 C3 H3A 109.6 . . ?
S1 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
S1 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C9 119.3(6) . . ?
C5 C4 C3 117.7(6) . . ?
C9 C4 C3 122.9(6) . . ?
C6 C5 C4 120.9(6) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C5 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C8 C7 C6 119.9(6) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 121.7(6) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C4 118.4(6) . . ?
C8 C9 C10 120.9(6) . . ?
C4 C9 C10 120.6(6) . . ?
C9 C10 S2 112.1(4) . . ?
C9 C10 H10A 109.2 . . ?
S2 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
S2 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 S2 115.5(6) . . ?
C12 C11 H11A 108.4 . . ?
S2 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
S2 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         5.609
_refine_diff_density_min         -3.103
_refine_diff_density_rms         0.226
_database_code_depnum_ccdc_archive 'CCDC 1022740'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ypc2x
_audit_creation_date             13-10-17
_audit_creation_method           
;
Rigaku CrystalClear-SM Expert 2.0 r11
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H18 Cl10 Nb2 S2'
_chemical_formula_sum            'C12 H18 Cl10 Nb2 S2'
_chemical_formula_weight         766.70
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.4305(10)
_cell_length_b                   17.5222(10)
_cell_length_c                   11.7030(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.150(7)
_cell_angle_gamma                90
_cell_volume                     2516.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11213
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.831
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.216
_diffrn_ambient_temperature      100.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
scan:
	Number of images: 128
	           Slice: -110.0000 - 18.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 135.0000
	             XTD: 45.0217
	          2theta: -19.9971
scan:
	Number of images: 71
	           Slice: -110.0000 - -39.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -30.0000
	             Phi: 270.0000
	             XTD: 45.0217
	          2theta: -19.9971
scan:
	Number of images: 24
	           Slice: -34.0000 - -10.0000
	     Image width: 1.0000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 70.0000
	             Phi: 90.0000
	             XTD: 45.0217
	          2theta: -19.9971
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.016580
_diffrn_orient_matrix_UB_12      -0.055907
_diffrn_orient_matrix_UB_13      0.007350
_diffrn_orient_matrix_UB_21      0.072528
_diffrn_orient_matrix_UB_22      0.011148
_diffrn_orient_matrix_UB_23      0.051847
_diffrn_orient_matrix_UB_31      -0.044222
_diffrn_orient_matrix_UB_32      -0.002677
_diffrn_orient_matrix_UB_33      0.062430
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4258
_reflns_number_total             4924
_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.

Disorder of the substituents around Nb2 was modelled as two parts whose 
occupancies were refined using a free variable. ADP values and bond distances 
of the two parts were linked using EADP and SADI restraints. While a second 
position for C12 is predicted for part 2 based on the geometry of around C11, 
a corresponding electron density peak could not be discerned due to the low 
occupancy (around 10%) of this part of a light atom. Cl7a, Cl8a and Cl9a were 
restrained using ISOR.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0306
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+7.2997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0681
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C11-C12
 with sigma of 0.02
 C10-S2 \\sim C10-S2A
 with sigma of 0.02
 Nb2-Cl7 \\sim Nb2-Cl7A
 with sigma of 0.01
 Nb2-Cl8 \\sim Nb2-Cl8A
 with sigma of 0.01
 Nb2-Cl9 \\sim Nb2-Cl9A
 with sigma of 0.01
 S2-Nb2 \\sim S2A-Nb2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl7A) \\sim Ueq, Uanis(Cl8A) \\sim Ueq, Uanis(Cl9A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl7) = Uanis(Cl7A)
Uanis(Cl8) = Uanis(Cl8A)
Uanis(Cl9) = Uanis(Cl9A)
Uanis(S2) = Uanis(S2A)
4. Others
 Sof(Cl7A)=Sof(Cl8A)=Sof(Cl9A)=Sof(S2A)=Sof(H10C)=Sof(H10D)=Sof(H11C)=
 Sof(H11D)=1-FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(S2)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C10(H10C,H10D), C11(H11A,H11B),
 C11(H11C,H11D)
5.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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 0.36975(2) 0.34546(2) 0.29428(2) 0.01117(8) Uani 1 1 d . . . . .
Nb2 Nb -0.15698(3) 0.15455(2) 0.39159(3) 0.01721(8) Uani 1 1 d . . . . .
Cl1 Cl 0.20550(7) 0.34847(5) 0.36736(7) 0.01846(18) Uani 1 1 d . . . . .
Cl2 Cl 0.27137(7) 0.34011(5) 0.11029(7) 0.01836(18) Uani 1 1 d . . . . .
Cl3 Cl 0.46570(7) 0.31714(5) 0.47918(7) 0.01547(17) Uani 1 1 d . . . . .
Cl4 Cl 0.52252(7) 0.31125(5) 0.21654(7) 0.01769(18) Uani 1 1 d . . . . .
Cl5 Cl 0.40191(7) 0.47306(5) 0.31068(8) 0.02059(19) Uani 1 1 d . . . . .
Cl6 Cl -0.01255(7) 0.14132(5) 0.54263(8) 0.0238(2) Uani 1 1 d . . . . .
Cl7 Cl -0.05921(8) 0.24777(6) 0.31156(11) 0.0216(2) Uani 0.8976(16) 1 d . . P A
1
Cl8 Cl -0.23209(10) 0.04078(6) 0.44637(9) 0.0193(2) Uani 0.8976(16) 1 d . . P A
1
Cl9 Cl -0.26301(9) 0.23283(7) 0.48034(11) 0.0247(3) Uani 0.8976(16) 1 d . . P A
1
Cl10 Cl -0.27561(7) 0.14903(6) 0.21696(8) 0.0243(2) Uani 1 1 d . . . . .
Cl7A Cl -0.0649(8) 0.2699(5) 0.3561(10) 0.0216(2) Uani 0.1024(16) 1 d . U P A 2
Cl8A Cl -0.1836(9) 0.0315(4) 0.4280(8) 0.0193(2) Uani 0.1024(16) 1 d . U P A 2
Cl9A Cl -0.2578(9) 0.2098(7) 0.5182(10) 0.0247(3) Uani 0.1024(16) 1 d . U P A 2
S1 S 0.33250(7) 0.19548(5) 0.31380(7) 0.01204(17) Uani 1 1 d . . . . .
S2 S -0.03568(8) 0.05120(5) 0.29335(9) 0.0159(2) Uani 0.8976(16) 1 d . . P A 1
S2A S -0.0182(6) 0.1127(5) 0.2521(7) 0.0159(2) Uani 0.1024(16) 1 d . . P A 2
C1 C 0.4606(3) 0.0735(2) 0.4025(3) 0.0222(8) Uani 1 1 d . . . . .
H1A H 0.5307 0.0470 0.4078 0.033 Uiso 1 1 calc R . . . .
H1B H 0.4489 0.0889 0.4801 0.033 Uiso 1 1 calc R . . . .
H1C H 0.4019 0.0392 0.3685 0.033 Uiso 1 1 calc R . . . .
C2 C 0.4614(3) 0.14379(19) 0.3268(3) 0.0156(7) Uani 1 1 d . . . . .
H2A H 0.4746 0.1282 0.2488 0.019 Uiso 1 1 calc R . . . .
H2B H 0.5217 0.1779 0.3605 0.019 Uiso 1 1 calc R . . . .
C3 C 0.2592(3) 0.16008(19) 0.1755(3) 0.0155(7) Uani 1 1 d . . . . .
H3A H 0.1867 0.1847 0.1589 0.019 Uiso 1 1 calc R . . . .
H3B H 0.3002 0.1736 0.1124 0.019 Uiso 1 1 calc R . . . .
C4 C 0.2456(3) 0.07490(18) 0.1796(3) 0.0119(7) Uani 1 1 d . . . . .
C5 C 0.3093(3) 0.0293(2) 0.1184(3) 0.0157(7) Uani 1 1 d . . . . .
H5 H 0.3559 0.0529 0.0719 0.019 Uiso 1 1 calc R . . . .
C6 C 0.3059(3) -0.0498(2) 0.1243(3) 0.0163(7) Uani 1 1 d . . . . .
H6 H 0.3490 -0.0799 0.0814 0.020 Uiso 1 1 calc R . . . .
C7 C 0.2393(3) -0.0844(2) 0.1930(3) 0.0176(7) Uani 1 1 d . . . . .
H7 H 0.2387 -0.1384 0.2000 0.021 Uiso 1 1 calc R . . . .
C8 C 0.1734(3) -0.0403(2) 0.2518(3) 0.0169(7) Uani 1 1 d . . . . .
H8 H 0.1263 -0.0645 0.2971 0.020 Uiso 1 1 calc R . . . .
C9 C 0.1754(3) 0.03939(19) 0.2455(3) 0.0132(7) Uani 1 1 d . . . . .
C10 C 0.1041(3) 0.0856(2) 0.3129(3) 0.0185(7) Uani 1 1 d . . . . .
H10A H 0.1043 0.1396 0.2877 0.022 Uiso 0.8976(16) 1 calc R . P A 1
H10B H 0.1350 0.0837 0.3962 0.022 Uiso 0.8976(16) 1 calc R . P A 1
H10C H 0.1452 0.1323 0.3402 0.022 Uiso 0.1024(16) 1 calc R . P A 2
H10D H 0.0954 0.0557 0.3826 0.022 Uiso 0.1024(16) 1 calc R . P A 2
C11 C -0.0744(3) 0.0458(2) 0.1378(4) 0.0322(10) Uani 1 1 d . . . . .
H11A H -0.0373 0.0013 0.1093 0.039 Uiso 0.8976(16) 1 calc R . P A 1
H11B H -0.1539 0.0363 0.1201 0.039 Uiso 0.8976(16) 1 calc R . P A 1
H11C H -0.0295 0.0001 0.1293 0.039 Uiso 0.1024(16) 1 calc R . P A 2
H11D H -0.1528 0.0337 0.1332 0.039 Uiso 0.1024(16) 1 calc R . P A 2
C12 C -0.0481(4) 0.1169(3) 0.0704(4) 0.0354(10) Uani 1 1 d . . . . .
H12A H 0.0311 0.1235 0.0794 0.053 Uiso 1 1 calc GR . . . .
H12B H -0.0808 0.1620 0.1007 0.053 Uiso 1 1 calc GR . . . .
H12C H -0.0778 0.1106 -0.0117 0.053 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.01024(15) 0.01049(15) 0.01267(14) 0.00064(11) 0.00148(11) -0.00018(11)
Nb2 0.01197(16) 0.01604(16) 0.02487(17) 0.00297(13) 0.00677(13) 0.00253(12)
Cl1 0.0115(4) 0.0216(4) 0.0230(4) -0.0012(3) 0.0049(3) 0.0020(3)
Cl2 0.0197(4) 0.0185(4) 0.0152(4) 0.0022(3) -0.0024(3) -0.0006(3)
Cl3 0.0144(4) 0.0184(4) 0.0130(4) 0.0012(3) 0.0002(3) 0.0013(3)
Cl4 0.0138(4) 0.0214(4) 0.0189(4) -0.0031(3) 0.0060(3) -0.0019(3)
Cl5 0.0226(5) 0.0109(4) 0.0272(5) 0.0013(3) 0.0008(4) -0.0019(3)
Cl6 0.0167(4) 0.0305(5) 0.0243(4) -0.0001(4) 0.0036(3) -0.0003(4)
Cl7 0.0175(5) 0.0163(5) 0.0329(6) 0.0011(4) 0.0099(4) -0.0014(4)
Cl8 0.0167(6) 0.0188(5) 0.0225(5) 0.0021(4) 0.0035(4) -0.0039(4)
Cl9 0.0161(5) 0.0222(6) 0.0367(7) -0.0090(5) 0.0071(5) 0.0026(5)
Cl10 0.0144(4) 0.0310(5) 0.0274(5) 0.0099(4) 0.0025(3) 0.0039(4)
Cl7A 0.0175(5) 0.0163(5) 0.0329(6) 0.0011(4) 0.0099(4) -0.0014(4)
Cl8A 0.0167(6) 0.0188(5) 0.0225(5) 0.0021(4) 0.0035(4) -0.0039(4)
Cl9A 0.0161(5) 0.0222(6) 0.0367(7) -0.0090(5) 0.0071(5) 0.0026(5)
S1 0.0106(4) 0.0114(4) 0.0141(4) 0.0005(3) 0.0017(3) 0.0008(3)
S2 0.0103(4) 0.0131(4) 0.0247(5) 0.0001(4) 0.0038(4) -0.0006(4)
S2A 0.0103(4) 0.0131(4) 0.0247(5) 0.0001(4) 0.0038(4) -0.0006(4)
C1 0.022(2) 0.0215(19) 0.0223(19) 0.0028(15) 0.0013(15) 0.0083(16)
C2 0.0077(16) 0.0152(17) 0.0226(17) 0.0003(14) -0.0013(13) 0.0021(13)
C3 0.0151(17) 0.0153(17) 0.0149(16) 0.0002(13) -0.0015(13) -0.0011(14)
C4 0.0094(16) 0.0107(15) 0.0139(16) 0.0008(12) -0.0038(13) -0.0002(13)
C5 0.0156(17) 0.0181(17) 0.0138(16) 0.0014(13) 0.0040(13) 0.0003(14)
C6 0.0114(16) 0.0181(17) 0.0186(17) -0.0055(14) -0.0001(13) 0.0032(14)
C7 0.0147(17) 0.0124(17) 0.0239(18) -0.0006(14) -0.0021(14) -0.0002(14)
C8 0.0124(17) 0.0161(17) 0.0217(18) -0.0001(14) 0.0008(14) -0.0037(14)
C9 0.0090(16) 0.0139(16) 0.0155(16) 0.0012(13) -0.0019(13) 0.0029(13)
C10 0.0093(16) 0.0199(18) 0.0268(19) -0.0051(15) 0.0042(14) -0.0037(14)
C11 0.016(2) 0.032(2) 0.045(3) -0.016(2) -0.0054(18) 0.0038(17)
C12 0.028(2) 0.050(3) 0.025(2) 0.000(2) -0.0033(18) 0.002(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl1 2.3363(9) . ?
Nb1 Cl2 2.3029(9) . ?
Nb1 Cl3 2.3516(8) . ?
Nb1 Cl4 2.3115(9) . ?
Nb1 Cl5 2.2740(9) . ?
Nb1 S1 2.6844(9) . ?
Nb2 Cl6 2.3221(10) . ?
Nb2 Cl7 2.3205(10) . ?
Nb2 Cl8 2.3339(10) . ?
Nb2 Cl9 2.2656(10) . ?
Nb2 Cl10 2.3242(10) . ?
Nb2 Cl7A 2.390(7) . ?
Nb2 Cl8A 2.233(7) . ?
Nb2 Cl9A 2.301(8) . ?
Nb2 S2 2.7251(10) . ?
Nb2 S2A 2.660(6) . ?
S1 C2 1.826(3) . ?
S1 C3 1.835(3) . ?
S2 C10 1.819(3) . ?
S2 C11 1.810(4) . ?
S2A C10 1.642(8) . ?
S2A C11 1.832(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.518(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.504(4) . ?
C4 C5 1.400(5) . ?
C4 C9 1.399(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(5) . ?
C9 C10 1.512(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 C12 1.537(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
Cl1 Nb1 Cl3 90.73(3) . . ?
Cl1 Nb1 S1 79.54(3) . . ?
Cl2 Nb1 Cl1 88.75(3) . . ?
Cl2 Nb1 Cl3 165.47(3) . . ?
Cl2 Nb1 Cl4 88.21(3) . . ?
Cl2 Nb1 S1 88.09(3) . . ?
Cl3 Nb1 S1 77.54(3) . . ?
Cl4 Nb1 Cl1 166.04(3) . . ?
Cl4 Nb1 Cl3 88.81(3) . . ?
Cl4 Nb1 S1 86.75(3) . . ?
Cl5 Nb1 Cl1 95.68(3) . . ?
Cl5 Nb1 Cl2 100.31(3) . . ?
Cl5 Nb1 Cl3 94.19(3) . . ?
Cl5 Nb1 Cl4 98.26(3) . . ?
Cl5 Nb1 S1 170.30(3) . . ?
Cl6 Nb2 Cl8 90.02(4) . . ?
Cl6 Nb2 Cl10 166.12(4) . . ?
Cl6 Nb2 Cl7A 83.3(3) . . ?
Cl6 Nb2 S2 80.92(3) . . ?
Cl6 Nb2 S2A 86.63(18) . . ?
Cl7 Nb2 Cl6 89.22(4) . . ?
Cl7 Nb2 Cl8 165.98(4) . . ?
Cl7 Nb2 Cl10 88.52(4) . . ?
Cl7 Nb2 S2 86.39(4) . . ?
Cl8 Nb2 S2 79.67(4) . . ?
Cl9 Nb2 Cl6 98.47(4) . . ?
Cl9 Nb2 Cl7 97.99(4) . . ?
Cl9 Nb2 Cl8 95.97(4) . . ?
Cl9 Nb2 Cl10 95.41(4) . . ?
Cl9 Nb2 S2 175.58(4) . . ?
Cl10 Nb2 Cl8 88.88(4) . . ?
Cl10 Nb2 Cl7A 97.9(3) . . ?
Cl10 Nb2 S2 85.28(3) . . ?
Cl10 Nb2 S2A 80.31(18) . . ?
Cl7A Nb2 S2A 75.6(3) . . ?
Cl8A Nb2 Cl6 83.0(3) . . ?
Cl8A Nb2 Cl10 92.0(2) . . ?
Cl8A Nb2 Cl7A 159.9(4) . . ?
Cl8A Nb2 Cl9A 99.9(4) . . ?
Cl8A Nb2 S2A 88.9(3) . . ?
Cl9A Nb2 Cl6 89.2(3) . . ?
Cl9A Nb2 Cl10 104.4(3) . . ?
Cl9A Nb2 Cl7A 94.6(4) . . ?
Cl9A Nb2 S2A 169.8(4) . . ?
C2 S1 Nb1 109.37(11) . . ?
C2 S1 C3 102.23(16) . . ?
C3 S1 Nb1 108.91(11) . . ?
C10 S2 Nb2 107.94(12) . . ?
C11 S2 Nb2 112.49(14) . . ?
C11 S2 C10 103.88(18) . . ?
C10 S2A Nb2 117.4(4) . . ?
C10 S2A C11 110.5(4) . . ?
C11 S2A Nb2 114.5(3) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
S1 C2 H2A 109.4 . . ?
S1 C2 H2B 109.4 . . ?
C1 C2 S1 111.3(2) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
S1 C3 H3A 109.6 . . ?
S1 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 S1 110.5(2) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C5 C4 C3 118.3(3) . . ?
C9 C4 C3 122.9(3) . . ?
C9 C4 C5 118.8(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.5(3) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 120.9(3) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C8 119.4(3) . . ?
C4 C9 C10 121.2(3) . . ?
C8 C9 C10 119.4(3) . . ?
S2 C10 H10A 109.1 . . ?
S2 C10 H10B 109.1 . . ?
S2A C10 H10C 107.2 . . ?
S2A C10 H10D 107.2 . . ?
C9 C10 S2 112.6(2) . . ?
C9 C10 S2A 120.5(4) . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C9 C10 H10C 107.2 . . ?
C9 C10 H10D 107.2 . . ?
H10A C10 H10B 107.8 . . ?
H10C C10 H10D 106.8 . . ?
S2 C11 H11A 108.4 . . ?
S2 C11 H11B 108.4 . . ?
S2A C11 H11C 115.8 . . ?
S2A C11 H11D 115.8 . . ?
H11A C11 H11B 107.5 . . ?
H11C C11 H11D 112.8 . . ?
C12 C11 S2 115.4(3) . . ?
C12 C11 S2A 76.6(3) . . ?
C12 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
C12 C11 H11C 115.8 . . ?
C12 C11 H11D 115.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nb1 S1 C2 C1 147.4(2) . . . . ?
Nb1 S1 C3 C4 175.0(2) . . . . ?
Nb2 S2 C10 S2A -59.8(4) . . . . ?
Nb2 S2 C10 C9 -170.9(2) . . . . ?
Nb2 S2 C11 S2A 63.0(3) . . . . ?
Nb2 S2 C11 C12 68.3(3) . . . . ?
Nb2 S2A C10 S2 71.6(4) . . . . ?
Nb2 S2A C10 C9 161.5(3) . . . . ?
Nb2 S2A C11 S2 -68.0(3) . . . . ?
Nb2 S2A C11 C12 116.8(4) . . . . ?
S1 C3 C4 C5 -106.6(3) . . . . ?
S1 C3 C4 C9 70.7(4) . . . . ?
C2 S1 C3 C4 59.3(3) . . . . ?
C3 S1 C2 C1 -97.3(3) . . . . ?
C3 C4 C5 C6 175.9(3) . . . . ?
C3 C4 C9 C8 -175.1(3) . . . . ?
C3 C4 C9 C10 3.0(5) . . . . ?
C4 C5 C6 C7 -0.8(5) . . . . ?
C4 C9 C10 S2 133.8(3) . . . . ?
C4 C9 C10 S2A 88.8(5) . . . . ?
C5 C4 C9 C8 2.2(5) . . . . ?
C5 C4 C9 C10 -179.6(3) . . . . ?
C5 C6 C7 C8 2.5(5) . . . . ?
C6 C7 C8 C9 -1.8(5) . . . . ?
C7 C8 C9 C4 -0.6(5) . . . . ?
C7 C8 C9 C10 -178.7(3) . . . . ?
C8 C9 C10 S2 -48.1(4) . . . . ?
C8 C9 C10 S2A -93.0(5) . . . . ?
C9 C4 C5 C6 -1.6(5) . . . . ?
C10 S2 C11 S2A -53.4(4) . . . . ?
C10 S2 C11 C12 -48.2(3) . . . . ?
C10 S2A C11 S2 67.2(4) . . . . ?
C10 S2A C11 C12 -107.9(5) . . . . ?
C11 S2 C10 S2A 59.8(4) . . . . ?
C11 S2 C10 C9 -51.3(3) . . . . ?
C11 S2A C10 S2 -62.3(4) . . . . ?
C11 S2A C10 C9 27.7(6) . . . . ?
#===END
_database_code_depnum_ccdc_archive 'CCDC 1022741'
