# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1494381'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.07.05 svn.r3305 for OlexSys, GUI svn.r5199)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H32 Cl4 Nb2 Se6'
_chemical_formula_sum            'C32 H32 Cl4 Nb2 Se6'
_chemical_formula_weight         1217.95
_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'
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'
Se Se -0.0929 2.2259 '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                   10.6850(5)
_cell_length_b                   12.3759(5)
_cell_length_c                   14.1909(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.821(5)
_cell_angle_gamma                90
_cell_volume                     1796.26(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.039
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   "CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'"
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1156
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by slow evaporation'
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.028
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         2.999
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_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                3334
_reflns_number_total             4644
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        "CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'"
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4644
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²+5.9443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1052
_refine_special_details          
;
There are some difficulties with the interpretation of the electron 
density peaks pertaining to the bridging Se positions, however, it 
is clear that the major species comprises 2 single mu2 Se bridges.


The molecule exhibits inversion symmetry at the centre of the 
Nb2Cl2Se4+x core -- the discussions below are with reference to 
the asymmetric unit.
Initial refinements proceed as expected with the large electron 
density peak refined as a single Se atom, this has the expected 
geometry for such a species forming a mu2 bridge. However, 
significant electron density remains asymmetrically above 
(1.302A) and below (0.982A) this site and free refinement of 
the occupancies give the values below, and the geometry of the 
2 new positions is consistent with an Se2 unit. The difficulty 
of interpretation arises from the occupancy sum of 1.0 so that 
a mixture of single bridge and double bridge situations cannot 
exist without also involving a partially vacant bridge site. 

Refined occupancies of the electron density peaks:
The difference peaks appear to represent real electron density 
(not Fourier truncation peaks).
Refined occupancies (EADP constraints) -- 0.057, 0.89, 0.057
Refined occupancies (no ADP constraints) -- 0.056, 0.89, 0.059

;

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Se3B) = Uanis(Se3) = Uanis(Se3A)
3. Others
 Fixed Sof: Se3(0.9) Se3A(0.05) Se3B(0.05)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.41965(5) 0.07014(4) 0.04021(4) 0.01607(13) Uani 1 1 d . . . . .
Se1 Se 0.40498(6) 0.16002(5) 0.21981(5) 0.02373(16) Uani 1 1 d . . . . .
Se2 Se 0.17794(6) 0.17908(5) -0.02486(5) 0.02375(16) Uani 1 1 d . . . . .
Se3 Se 0.62591(6) -0.01602(6) 0.13262(5) 0.02518(17) Uani 0.9 1 d . . P . .
Se3A Se 0.6861(11) 0.0675(10) 0.1105(10) 0.02518(17) Uani 0.05 1 d . . P . .
Se3B Se 0.5836(12) -0.0818(11) 0.1473(10) 0.02518(17) Uani 0.05 1 d . . P . .
Cl1 Cl 0.27315(13) -0.05076(12) 0.08541(12) 0.0261(3) Uani 1 1 d . . . . .
Cl2 Cl 0.49981(14) 0.24536(12) 0.02221(12) 0.0264(3) Uani 1 1 d . . . . .
C1 C 0.5725(6) 0.2331(5) 0.2809(5) 0.0292(15) Uani 1 1 d . . . . .
H1A H 0.6054 0.2689 0.2303 0.035 Uiso 1 1 calc R . . . .
H1B H 0.5627 0.2880 0.3290 0.035 Uiso 1 1 calc R . . . .
C2 C 0.6633(6) 0.1443(5) 0.3312(5) 0.0236(13) Uani 1 1 d . . . . .
C3 C 0.7986(7) 0.1509(6) 0.3511(5) 0.0343(17) Uani 1 1 d . . . . .
H3 H 0.8378 0.2163 0.3388 0.041 Uiso 1 1 calc R . . . .
C4 C 0.8728(6) 0.0661(6) 0.3870(6) 0.0379(18) Uani 1 1 d . . . . .
H4 H 0.9647 0.0710 0.3980 0.046 Uiso 1 1 calc R . . . .
C5 C 0.8186(7) -0.0315(6) 0.4092(6) 0.0380(17) Uani 1 1 d . . . . .
H5 H 0.8730 -0.0920 0.4335 0.046 Uiso 1 1 calc R . . . .
C6 C 0.6850(6) -0.0374(5) 0.3951(5) 0.0296(15) Uani 1 1 d . . . . .
H6 H 0.6473 -0.0998 0.4149 0.036 Uiso 1 1 calc R . . . .
C7 C 0.6071(6) 0.0489(5) 0.3518(5) 0.0230(13) Uani 1 1 d . . . . .
C8 C 0.4606(6) 0.0458(5) 0.3207(5) 0.0273(14) Uani 1 1 d . . . . .
H8A H 0.4267 0.0604 0.3774 0.033 Uiso 1 1 calc R . . . .
H8B H 0.4284 -0.0258 0.2928 0.033 Uiso 1 1 calc R . . . .
C9 C 0.1797(6) 0.2637(5) -0.1407(5) 0.0318(15) Uani 1 1 d . . . . .
H9A H 0.1729 0.3418 -0.1279 0.038 Uiso 1 1 calc R . . . .
H9B H 0.2617 0.2508 -0.1582 0.038 Uiso 1 1 calc R . . . .
C10 C 0.0629(6) 0.2266(5) -0.2230(5) 0.0246(14) Uani 1 1 d . . . . .
C11 C 0.0157(6) 0.2818(5) -0.3121(5) 0.0255(14) Uani 1 1 d . . . . .
H11 H 0.0584 0.3455 -0.3241 0.031 Uiso 1 1 calc R . . . .
C12 C -0.0911(7) 0.2443(6) -0.3814(5) 0.0407(18) Uani 1 1 d . . . . .
H12 H -0.1244 0.2826 -0.4415 0.049 Uiso 1 1 calc R . . . .
C13 C -0.1543(7) 0.1469(6) -0.3641(6) 0.0410(18) Uani 1 1 d . . . . .
H13 H -0.2292 0.1205 -0.4127 0.049 Uiso 1 1 calc R . . . .
C14 C -0.1075(6) 0.0941(5) -0.2803(5) 0.0307(16) Uani 1 1 d . . . . .
H14 H -0.1486 0.0290 -0.2696 0.037 Uiso 1 1 calc R . . . .
C15 C 0.0009(6) 0.1320(5) -0.2072(5) 0.0251(14) Uani 1 1 d . . . . .
C16 C 0.0558(6) 0.0754(5) -0.1098(5) 0.0313(15) Uani 1 1 d . . . . .
H16A H 0.1022 0.0085 -0.1183 0.038 Uiso 1 1 calc R . . . .
H16B H -0.0150 0.0562 -0.0807 0.038 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
Nb1 0.0156(2) 0.0185(3) 0.0142(3) -0.0017(2) 0.0044(2) 0.00037(19)
Se1 0.0243(3) 0.0269(3) 0.0202(4) -0.0032(3) 0.0066(3) 0.0031(2)
Se2 0.0209(3) 0.0288(3) 0.0216(4) 0.0035(3) 0.0061(3) 0.0045(2)
Se3 0.0226(3) 0.0332(4) 0.0168(4) -0.0058(3) 0.0011(3) 0.0088(3)
Se3A 0.0226(3) 0.0332(4) 0.0168(4) -0.0058(3) 0.0011(3) 0.0088(3)
Se3B 0.0226(3) 0.0332(4) 0.0168(4) -0.0058(3) 0.0011(3) 0.0088(3)
Cl1 0.0198(6) 0.0266(8) 0.0278(9) 0.0075(6) 0.0005(6) -0.0050(5)
Cl2 0.0287(7) 0.0248(7) 0.0266(9) -0.0001(6) 0.0093(7) -0.0064(6)
C1 0.038(4) 0.022(3) 0.024(4) 0.000(3) 0.002(3) -0.006(3)
C2 0.025(3) 0.028(3) 0.017(4) -0.005(3) 0.005(3) -0.010(2)
C3 0.041(4) 0.037(4) 0.029(4) -0.010(3) 0.016(3) -0.017(3)
C4 0.019(3) 0.059(5) 0.035(5) -0.006(4) 0.007(3) -0.003(3)
C5 0.035(4) 0.040(4) 0.031(5) -0.001(3) -0.002(3) 0.017(3)
C6 0.039(4) 0.023(3) 0.021(4) -0.003(3) 0.000(3) -0.012(3)
C7 0.029(3) 0.023(3) 0.015(3) -0.004(3) 0.003(3) 0.000(2)
C8 0.031(3) 0.026(3) 0.027(4) -0.001(3) 0.013(3) -0.005(3)
C9 0.031(3) 0.036(4) 0.029(4) 0.007(3) 0.009(3) -0.005(3)
C10 0.024(3) 0.025(3) 0.025(4) -0.001(3) 0.007(3) 0.006(2)
C11 0.023(3) 0.027(3) 0.028(4) 0.007(3) 0.010(3) 0.003(2)
C12 0.057(5) 0.040(4) 0.018(4) 0.010(3) 0.001(4) 0.014(4)
C13 0.035(4) 0.055(5) 0.025(4) -0.012(4) -0.005(3) 0.017(3)
C14 0.033(3) 0.024(3) 0.038(5) -0.002(3) 0.015(3) -0.001(3)
C15 0.024(3) 0.027(3) 0.024(4) 0.001(3) 0.005(3) 0.004(2)
C16 0.023(3) 0.031(4) 0.038(5) 0.006(3) 0.005(3) 0.000(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Nb1 2.8980(9) 3_655 ?
Nb1 Se1 2.8266(8) . ?
Nb1 Se2 2.8214(7) . ?
Nb1 Se3 2.4514(9) 3_655 ?
Nb1 Se3 2.4579(8) . ?
Nb1 Se3A 2.731(12) . ?
Nb1 Se3A 2.712(13) 3_655 ?
Nb1 Se3B 2.654(13) 3_655 ?
Nb1 Se3B 2.715(13) . ?
Nb1 Cl1 2.3836(14) . ?
Nb1 Cl2 2.3724(15) . ?
Se1 C1 1.968(6) . ?
Se1 C8 1.977(6) . ?
Se2 C9 1.953(7) . ?
Se2 C16 1.973(7) . ?
Se3 Nb1 2.4514(9) 3_655 ?
Se3 Se3A 1.302(13) . ?
Se3 Se3B 0.982(15) . ?
Se3A Nb1 2.712(13) 3_655 ?
Se3A Se3B 2.28(2) . ?
Se3B Nb1 2.654(13) 3_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.503(9) . ?
C2 C3 1.393(8) . ?
C2 C7 1.393(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.324(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.414(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(9) . ?
C7 C8 1.499(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.513(9) . ?
C10 C11 1.397(9) . ?
C10 C15 1.395(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.355(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.438(11) . ?
C13 H13 0.9500 . ?
C13 C14 1.322(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.394(9) . ?
C15 C16 1.509(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 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
Se1 Nb1 Nb1 141.68(3) . 3_655 ?
Se2 Nb1 Nb1 138.42(3) . 3_655 ?
Se2 Nb1 Se1 79.79(2) . . ?
Se3 Nb1 Nb1 53.93(2) 3_655 3_655 ?
Se3 Nb1 Nb1 53.72(2) . 3_655 ?
Se3 Nb1 Se1 164.34(3) 3_655 . ?
Se3 Nb1 Se1 87.98(3) . . ?
Se3 Nb1 Se2 84.56(3) 3_655 . ?
Se3 Nb1 Se2 167.54(3) . . ?
Se3 Nb1 Se3 107.64(3) 3_655 . ?
Se3 Nb1 Se3A 104.3(3) 3_655 . ?
Se3 Nb1 Se3A 104.6(2) . 3_655 ?
Se3 Nb1 Se3A 28.6(3) 3_655 3_655 ?
Se3 Nb1 Se3A 28.5(3) . . ?
Se3 Nb1 Se3B 106.2(3) 3_655 . ?
Se3 Nb1 Se3B 21.7(3) 3_655 3_655 ?
Se3 Nb1 Se3B 21.2(3) . . ?
Se3 Nb1 Se3B 107.9(2) . 3_655 ?
Se3A Nb1 Nb1 58.1(2) 3_655 3_655 ?
Se3A Nb1 Nb1 57.5(3) . 3_655 ?
Se3A Nb1 Se1 147.1(3) 3_655 . ?
Se3A Nb1 Se1 89.9(3) . . ?
Se3A Nb1 Se2 84.8(2) 3_655 . ?
Se3A Nb1 Se2 152.1(3) . . ?
Se3A Nb1 Se3A 115.7(3) 3_655 . ?
Se3A Nb1 Se3B 93.5(4) 3_655 . ?
Se3B Nb1 Nb1 58.3(3) 3_655 3_655 ?
Se3B Nb1 Nb1 56.3(3) . 3_655 ?
Se3B Nb1 Se1 87.9(3) . . ?
Se3B Nb1 Se1 153.4(3) 3_655 . ?
Se3B Nb1 Se2 153.5(3) . . ?
Se3B Nb1 Se2 84.3(2) 3_655 . ?
Se3B Nb1 Se3A 94.4(4) 3_655 . ?
Se3B Nb1 Se3A 49.6(4) . . ?
Se3B Nb1 Se3A 50.4(4) 3_655 3_655 ?
Se3B Nb1 Se3B 114.7(3) 3_655 . ?
Cl1 Nb1 Nb1 103.89(4) . 3_655 ?
Cl1 Nb1 Se1 78.01(4) . . ?
Cl1 Nb1 Se2 77.16(4) . . ?
Cl1 Nb1 Se3 98.16(5) . 3_655 ?
Cl1 Nb1 Se3 98.13(4) . . ?
Cl1 Nb1 Se3A 126.2(3) . . ?
Cl1 Nb1 Se3A 70.2(3) . 3_655 ?
Cl1 Nb1 Se3B 77.4(3) . . ?
Cl1 Nb1 Se3B 119.0(3) . 3_655 ?
Cl2 Nb1 Nb1 103.39(4) . 3_655 ?
Cl2 Nb1 Se1 81.56(4) . . ?
Cl2 Nb1 Se2 81.53(4) . . ?
Cl2 Nb1 Se3 96.63(5) . 3_655 ?
Cl2 Nb1 Se3 99.09(4) . . ?
Cl2 Nb1 Se3A 71.3(3) . . ?
Cl2 Nb1 Se3A 124.8(3) . 3_655 ?
Cl2 Nb1 Se3B 119.9(3) . . ?
Cl2 Nb1 Se3B 75.1(3) . 3_655 ?
Cl2 Nb1 Cl1 152.68(6) . . ?
C1 Se1 Nb1 107.3(2) . . ?
C1 Se1 C8 88.0(3) . . ?
C8 Se1 Nb1 106.74(19) . . ?
C9 Se2 Nb1 107.50(19) . . ?
C9 Se2 C16 90.0(3) . . ?
C16 Se2 Nb1 105.67(18) . . ?
Nb1 Se3 Nb1 72.36(3) 3_655 . ?
Se3A Se3 Nb1 87.5(5) . . ?
Se3A Se3 Nb1 86.9(6) . 3_655 ?
Se3B Se3 Nb1 94.3(7) . . ?
Se3B Se3 Nb1 90.9(8) . 3_655 ?
Se3B Se3 Se3A 176.5(8) . . ?
Nb1 Se3A Nb1 64.3(3) 3_655 . ?
Se3 Se3A Nb1 64.5(5) . 3_655 ?
Se3 Se3A Nb1 64.1(5) . . ?
Se3 Se3A Se3B 1.5(4) . . ?
Se3B Se3A Nb1 64.9(4) . . ?
Se3B Se3A Nb1 63.5(4) . 3_655 ?
Nb1 Se3B Nb1 65.3(3) 3_655 . ?
Se3 Se3B Nb1 64.5(7) . . ?
Se3 Se3B Nb1 67.4(7) . 3_655 ?
Se3 Se3B Se3A 2.0(5) . . ?
Se3A Se3B Nb1 66.1(5) . 3_655 ?
Se3A Se3B Nb1 65.6(5) . . ?
Se1 C1 H1A 110.8 . . ?
Se1 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
C2 C1 Se1 104.7(4) . . ?
C2 C1 H1A 110.8 . . ?
C2 C1 H1B 110.8 . . ?
C3 C2 C1 122.9(5) . . ?
C3 C2 C7 119.5(6) . . ?
C7 C2 C1 117.4(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(6) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.6(6) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 120.5 . . ?
C6 C5 C4 119.0(6) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 H6 120.5 . . ?
C7 C6 C5 119.0(6) . . ?
C7 C6 H6 120.5 . . ?
C2 C7 C8 115.9(5) . . ?
C6 C7 C2 120.5(6) . . ?
C6 C7 C8 123.5(5) . . ?
Se1 C8 H8A 110.7 . . ?
Se1 C8 H8B 110.7 . . ?
C7 C8 Se1 105.3(4) . . ?
C7 C8 H8A 110.7 . . ?
C7 C8 H8B 110.7 . . ?
H8A C8 H8B 108.8 . . ?
Se2 C9 H9A 110.5 . . ?
Se2 C9 H9B 110.5 . . ?
H9A C9 H9B 108.7 . . ?
C10 C9 Se2 106.3(4) . . ?
C10 C9 H9A 110.5 . . ?
C10 C9 H9B 110.5 . . ?
C11 C10 C9 123.5(6) . . ?
C15 C10 C9 117.1(6) . . ?
C15 C10 C11 119.5(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.8(6) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.1(6) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(7) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.3(6) . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C16 117.4(6) . . ?
C14 C15 C10 119.7(6) . . ?
C14 C15 C16 123.0(6) . . ?
Se2 C16 H16A 110.6 . . ?
Se2 C16 H16B 110.6 . . ?
C15 C16 Se2 105.7(4) . . ?
C15 C16 H16A 110.6 . . ?
C15 C16 H16B 110.6 . . ?
H16A C16 H16B 108.7 . . ?

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 Se3 Se3A Nb1 72.46(4) 3_655 . . . ?
Nb1 Se3 Se3A Nb1 -72.46(4) . . . 3_655 ?
Nb1 Se3 Se3A Se3B -121(16) . . . . ?
Nb1 Se3 Se3A Se3B -49(16) 3_655 . . . ?
Nb1 Se3 Se3B Nb1 -72.37(6) 3_655 . . . ?
Nb1 Se3 Se3B Nb1 72.37(6) . . . 3_655 ?
Nb1 Se3 Se3B Se3A 49(16) 3_655 . . . ?
Nb1 Se3 Se3B Se3A 121(16) . . . . ?
Se1 C1 C2 C3 155.1(5) . . . . ?
Se1 C1 C2 C7 -20.1(7) . . . . ?
Se2 C9 C10 C11 167.1(5) . . . . ?
Se2 C9 C10 C15 -13.0(7) . . . . ?
C1 C2 C3 C4 -173.5(7) . . . . ?
C1 C2 C7 C6 177.9(6) . . . . ?
C1 C2 C7 C8 0.1(8) . . . . ?
C2 C3 C4 C5 -2.1(11) . . . . ?
C2 C7 C8 Se1 19.9(7) . . . . ?
C3 C2 C7 C6 2.5(9) . . . . ?
C3 C2 C7 C8 -175.3(6) . . . . ?
C3 C4 C5 C6 -1.5(11) . . . . ?
C4 C5 C6 C7 5.5(10) . . . . ?
C5 C6 C7 C2 -6.1(10) . . . . ?
C5 C6 C7 C8 171.6(6) . . . . ?
C6 C7 C8 Se1 -157.8(5) . . . . ?
C7 C2 C3 C4 1.6(10) . . . . ?
C9 C10 C11 C12 -178.7(6) . . . . ?
C9 C10 C15 C14 179.8(5) . . . . ?
C9 C10 C15 C16 0.0(8) . . . . ?
C10 C11 C12 C13 -1.2(10) . . . . ?
C10 C15 C16 Se2 12.8(6) . . . . ?
C11 C10 C15 C14 -0.3(9) . . . . ?
C11 C10 C15 C16 179.9(5) . . . . ?
C11 C12 C13 C14 0.0(10) . . . . ?
C12 C13 C14 C15 1.1(10) . . . . ?
C13 C14 C15 C10 -0.9(9) . . . . ?
C13 C14 C15 C16 178.8(6) . . . . ?
C14 C15 C16 Se2 -166.9(5) . . . . ?
C15 C10 C11 C12 1.4(9) . . . . ?

_shelx_res_file                  
;
    shelx.res created by SHELXL-2014/7

TITL shelx in P21/c #14
REM reset to P21/c #14
rem EADP Se3A Se3 Se3B
CELL 0.71073 10.685 12.37588 14.190876 90 106.8211 90
ZERR 2 0.000499 0.000511 0.000747 0 0.0053 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Nb Se
UNIT 64 64 8 4 12
EADP Se3B Se3 Se3A

L.S. 5
PLAN  20
TEMP -173(2)
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
SHEL 7 0.74
REM <olex2.extras>
REM <HklSrc "%.\\2016_0402r2.hkl">
REM </olex2.extras>

WGHT    0.038100    5.944300
FVAR       1.68051
NB1   4    0.419647    0.070136    0.040205    11.00000    0.01558    0.01847 =
         0.01422   -0.00174    0.00440    0.00037
SE1   5    0.404985    0.160018    0.219814    11.00000    0.02426    0.02690 =
         0.02016   -0.00317    0.00663    0.00312
SE2   5    0.177943    0.179080   -0.024863    11.00000    0.02086    0.02877 =
         0.02158    0.00353    0.00608    0.00453
SE3   5    0.625913   -0.016019    0.132616    10.90000    0.02263    0.03316 =
         0.01682   -0.00584    0.00109    0.00880
SE3A  5    0.686055    0.067484    0.110542    10.05000    0.02263    0.03316 =
         0.01682   -0.00584    0.00109    0.00880
SE3B  5    0.583554   -0.081792    0.147254    10.05000    0.02263    0.03316 =
         0.01682   -0.00584    0.00109    0.00880
CL1   3    0.273152   -0.050765    0.085407    11.00000    0.01976    0.02660 =
         0.02781    0.00748    0.00053   -0.00500
CL2   3    0.499809    0.245362    0.022212    11.00000    0.02871    0.02484 =
         0.02657   -0.00011    0.00935   -0.00642
C1    1    0.572464    0.233095    0.280859    11.00000    0.03799    0.02158 =
         0.02377   -0.00014    0.00222   -0.00582
AFIX  23
H1A   2    0.605405    0.268883    0.230338    11.00000   -1.20000
H1B   2    0.562744    0.287957    0.329027    11.00000   -1.20000
AFIX   0
C2    1    0.663322    0.144318    0.331229    11.00000    0.02517    0.02765 =
         0.01734   -0.00539    0.00495   -0.01018
C3    1    0.798618    0.150871    0.351077    11.00000    0.04112    0.03660 =
         0.02869   -0.00952    0.01573   -0.01707
AFIX  43
H3    2    0.837774    0.216277    0.338836    11.00000   -1.20000
AFIX   0
C4    1    0.872800    0.066123    0.386976    11.00000    0.01879    0.05889 =
         0.03542   -0.00586    0.00674   -0.00318
AFIX  43
H4    2    0.964660    0.071006    0.398036    11.00000   -1.20000
AFIX   0
C5    1    0.818579   -0.031466    0.409244    11.00000    0.03543    0.03982 =
         0.03130   -0.00138   -0.00193    0.01729
AFIX  43
H5    2    0.872997   -0.092023    0.433515    11.00000   -1.20000
AFIX   0
C6    1    0.684970   -0.037445    0.395143    11.00000    0.03890    0.02347 =
         0.02081   -0.00294   -0.00037   -0.01204
AFIX  43
H6    2    0.647321   -0.099848    0.414931    11.00000   -1.20000
AFIX   0
C7    1    0.607125    0.048917    0.351767    11.00000    0.02930    0.02270 =
         0.01480   -0.00414    0.00303   -0.00018
C8    1    0.460616    0.045759    0.320699    11.00000    0.03096    0.02627 =
         0.02745   -0.00127    0.01271   -0.00503
AFIX  23
H8A   2    0.426672    0.060406    0.377375    11.00000   -1.20000
H8B   2    0.428438   -0.025785    0.292803    11.00000   -1.20000
AFIX   0
C9    1    0.179707    0.263678   -0.140665    11.00000    0.03053    0.03574 =
         0.02911    0.00718    0.00854   -0.00527
AFIX  23
H9A   2    0.172926    0.341776   -0.127855    11.00000   -1.20000
H9B   2    0.261673    0.250833   -0.158181    11.00000   -1.20000
AFIX   0
C10   1    0.062889    0.226627   -0.222953    11.00000    0.02355    0.02531 =
         0.02506   -0.00075    0.00722    0.00610
C11   1    0.015705    0.281835   -0.312114    11.00000    0.02325    0.02669 =
         0.02831    0.00735    0.01039    0.00278
AFIX  43
H11   2    0.058417    0.345473   -0.324109    11.00000   -1.20000
AFIX   0
C12   1   -0.091113    0.244348   -0.381392    11.00000    0.05723    0.04045 =
         0.01793    0.00990    0.00068    0.01438
AFIX  43
H12   2   -0.124351    0.282553   -0.441527    11.00000   -1.20000
AFIX   0
C13   1   -0.154300    0.146855   -0.364109    11.00000    0.03493    0.05455 =
         0.02495   -0.01176   -0.00501    0.01669
AFIX  43
H13   2   -0.229227    0.120529   -0.412656    11.00000   -1.20000
AFIX   0
C14   1   -0.107532    0.094061   -0.280274    11.00000    0.03299    0.02448 =
         0.03758   -0.00220    0.01477   -0.00050
AFIX  43
H14   2   -0.148644    0.029002   -0.269626    11.00000   -1.20000
AFIX   0
C15   1    0.000896    0.131983   -0.207220    11.00000    0.02372    0.02650 =
         0.02371    0.00121    0.00480    0.00421
C16   1    0.055796    0.075387   -0.109804    11.00000    0.02260    0.03137 =
         0.03772    0.00615    0.00521   -0.00017
AFIX  23
H16A  2    0.102247    0.008541   -0.118324    11.00000   -1.20000
H16B  2   -0.015036    0.056199   -0.080733    11.00000   -1.20000
AFIX   0
HKLF 4

REM  shelx in P21/c #14
REM R1 =  0.0498 for    3334 Fo > 4sig(Fo)  and  0.0854 for all    4644 data
REM    205 parameters refined using      0 restraints

END

WGHT      0.0381      5.9125

REM Highest difference peak  1.008,  deepest hole -0.858,  1-sigma level  0.185
Q1    1   0.2420  0.2053 -0.0438  11.00000  0.05    1.01
Q2    1   0.0858  0.1262 -0.0602  11.00000  0.05    0.97
Q3    1  -0.1767  0.1027 -0.3298  11.00000  0.05    0.91
Q4    1   0.5758  0.2324  0.0174  11.00000  0.05    0.86
Q5    1   0.5745 -0.0664  0.1663  11.00000  0.05    0.76
Q6    1  -0.1329  0.1262 -0.3845  11.00000  0.05    0.73
Q7    1   0.3196  0.1947  0.2237  11.00000  0.05    0.72
Q8    1  -0.0650  0.0610 -0.3364  11.00000  0.05    0.69
Q9    1   0.4791  0.1698  0.0589  11.00000  0.05    0.69
Q10   1  -0.1303  0.1870 -0.4239  11.00000  0.05    0.68
Q11   1   0.4867  0.2036  0.2293  11.00000  0.05    0.67
Q12   1   0.6402  0.0077  0.4152  11.00000  0.05    0.67
Q13   1   0.6306 -0.1014  0.1250  11.00000  0.05    0.66
Q14   1   0.1867  0.0966 -0.0291  11.00000  0.05    0.66
Q15   1   0.6000  0.0606  0.1159  11.00000  0.05    0.65
Q16   1   0.3440  0.0952  0.0460  11.00000  0.05    0.63
Q17   1   0.0982  0.1369 -0.2437  11.00000  0.05    0.63
Q18   1  -0.1058  0.0616 -0.2704  11.00000  0.05    0.62
Q19   1   0.4208  0.1027  0.0578  11.00000  0.05    0.62
Q20   1   0.6395  0.1991 -0.0133  11.00000  0.05    0.62
;
_shelx_res_checksum              69901
_shelx_SHELXL_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_0505r1
_database_code_depnum_ccdc_archive 'CCDC 1494382'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 H12 Cl8 Nb2 S2'
_chemical_formula_sum            'C4 H12 Cl8 Nb2 S2'
_chemical_formula_weight         593.68

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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.4589(2)
_cell_length_b                   10.1598(4)
_cell_length_c                   13.1644(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.499(4)
_cell_angle_gamma                90
_cell_volume                     861.20(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3983
_cell_measurement_theta_min      2.4850
_cell_measurement_theta_max      31.9990

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_F_000             572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    2.787
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68615
_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            5264
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.535
_diffrn_reflns_theta_max         25.987
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1690
_reflns_number_gt                1570
_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)+(0.0288P)²+0.9127P] 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         1690
_refine_ls_number_parameters     75
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0521
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 1.05339(3) 0.14902(2) 0.49580(2) 0.01023(9) Uani 1 1 d . . . . .
Cl1 Cl 1.31913(9) 0.29477(6) 0.56126(5) 0.01819(15) Uani 1 1 d . . . . .
Cl2 Cl 0.84323(9) 0.19683(6) 0.62515(4) 0.01472(14) Uani 1 1 d . . . . .
Cl3 Cl 1.18366(10) 0.12871(6) 0.33767(5) 0.01646(15) Uani 1 1 d . . . . .
Cl4 Cl 1.25630(9) -0.02464(6) 0.58104(5) 0.01371(14) Uani 1 1 d . . . . .
S1 S 0.88772(10) 0.36936(6) 0.42503(5) 0.01289(14) Uani 1 1 d . . . . .
C1 C 1.0547(4) 0.4439(3) 0.3383(2) 0.0185(6) Uani 1 1 d . . . . .
H1A H 1.0678 0.3852 0.2801 0.028 Uiso 1 1 calc R U . . .
H1B H 1.1921 0.4591 0.3734 0.028 Uiso 1 1 calc R U . . .
H1C H 0.9952 0.5280 0.3142 0.028 Uiso 1 1 calc R U . . .
C2 C 0.6663(4) 0.3360(3) 0.3380(2) 0.0211(6) Uani 1 1 d . . . . .
H2A H 0.6114 0.4188 0.3088 0.032 Uiso 1 1 calc R U . . .
H2B H 0.5589 0.2922 0.3744 0.032 Uiso 1 1 calc R U . . .
H2C H 0.7075 0.2786 0.2832 0.032 Uiso 1 1 calc R U . . .

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 0.00984(13) 0.01078(14) 0.01009(13) 0.00020(8) 0.00099(9) 0.00055(8)
Cl1 0.0143(3) 0.0156(3) 0.0240(3) -0.0012(3) -0.0030(2) -0.0019(3)
Cl2 0.0169(3) 0.0152(3) 0.0126(3) 0.0000(2) 0.0044(2) 0.0020(3)
Cl3 0.0210(3) 0.0145(3) 0.0149(3) 0.0006(2) 0.0078(2) 0.0007(2)
Cl4 0.0121(3) 0.0128(3) 0.0157(3) 0.0010(2) -0.0024(2) 0.0005(2)
S1 0.0147(3) 0.0119(3) 0.0122(3) 0.0012(2) 0.0014(2) 0.0010(2)
C1 0.0217(14) 0.0160(14) 0.0186(13) 0.0037(11) 0.0060(11) -0.0002(11)
C2 0.0166(14) 0.0207(15) 0.0247(15) 0.0051(11) -0.0062(11) 0.0009(11)

_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 Cl2 2.3110(6) . ?
Nb1 Cl3 2.3149(6) . ?
Nb1 Cl1 2.3768(7) . ?
Nb1 Cl4 2.4205(6) . ?
Nb1 Cl4 2.5107(6) 3_756 ?
Nb1 S1 2.6207(7) . ?
Nb1 Nb1 3.1094(5) 3_756 ?
Cl4 Nb1 2.5107(6) 3_756 ?
S1 C2 1.794(3) . ?
S1 C1 1.798(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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
Cl2 Nb1 Cl3 163.19(3) . . ?
Cl2 Nb1 Cl1 92.93(2) . . ?
Cl3 Nb1 Cl1 94.50(2) . . ?
Cl2 Nb1 Cl4 98.03(2) . . ?
Cl3 Nb1 Cl4 97.48(2) . . ?
Cl1 Nb1 Cl4 86.37(2) . . ?
Cl2 Nb1 Cl4 84.68(2) . 3_756 ?
Cl3 Nb1 Cl4 85.82(2) . 3_756 ?
Cl1 Nb1 Cl4 171.68(2) . 3_756 ?
Cl4 Nb1 Cl4 101.84(2) . 3_756 ?
Cl2 Nb1 S1 80.52(2) . . ?
Cl3 Nb1 S1 85.61(2) . . ?
Cl1 Nb1 S1 81.94(2) . . ?
Cl4 Nb1 S1 168.12(2) . . ?
Cl4 Nb1 S1 89.80(2) 3_756 . ?
Cl2 Nb1 Nb1 91.935(18) . 3_756 ?
Cl3 Nb1 Nb1 92.431(18) . 3_756 ?
Cl1 Nb1 Nb1 138.56(2) . 3_756 ?
Cl4 Nb1 Nb1 52.210(16) . 3_756 ?
Cl4 Nb1 Nb1 49.631(15) 3_756 3_756 ?
S1 Nb1 Nb1 139.374(19) . 3_756 ?
Nb1 Cl4 Nb1 78.16(2) . 3_756 ?
C2 S1 C1 99.33(13) . . ?
C2 S1 Nb1 110.39(10) . . ?
C1 S1 Nb1 109.69(9) . . ?
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 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_refine_diff_density_max         0.570
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.096

_shelx_res_file                  
; 
  
    2016_0505r1.res created by SHELXL-2014/7 
  
  
TITL 2016_0505r1 in P2(1)/n 
CELL 0.71073   6.4589  10.1598  13.1644  90.000  94.499  90.000 
ZERR    2.00   0.0002   0.0004   0.0005   0.000   0.004   0.000 
LATT 1 
SYMM 0.5-X, 0.5+Y, 0.5-Z 
SFAC C  H  S  Cl Nb 
UNIT 8 24 4 16 4 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.137 0.072 0.034 
TEMP -173 
WGHT    0.028800    0.912700 
FVAR       0.12508 
MOLE 1 
NB1   5    1.053386    0.149018    0.495802    11.00000    0.00984    0.01078 = 
         0.01009    0.00020    0.00099    0.00055 
CL1   4    1.319131    0.294765    0.561262    11.00000    0.01425    0.01560 = 
         0.02400   -0.00121   -0.00304   -0.00187 
CL2   4    0.843227    0.196826    0.625149    11.00000    0.01691    0.01520 = 
         0.01256   -0.00003    0.00438    0.00196 
CL3   4    1.183662    0.128705    0.337670    11.00000    0.02103    0.01449 = 
         0.01487    0.00060    0.00777    0.00068 
CL4   4    1.256300   -0.024641    0.581037    11.00000    0.01205    0.01277 = 
         0.01575    0.00099   -0.00238    0.00054 
S1    3    0.887717    0.369361    0.425030    11.00000    0.01468    0.01190 = 
         0.01216    0.00119    0.00140    0.00096 
C1    1    1.054718    0.443890    0.338294    11.00000    0.02166    0.01596 = 
         0.01857    0.00368    0.00602   -0.00024 
AFIX 137 
H1A   2    1.067850    0.385191    0.280077    11.00000   -1.50000 
H1B   2    1.192140    0.459061    0.373360    11.00000   -1.50000 
H1C   2    0.995173    0.528034    0.314176    11.00000   -1.50000 
AFIX   0 
C2    1    0.666260    0.335955    0.337996    11.00000    0.01663    0.02074 = 
         0.02470    0.00513   -0.00623    0.00087 
AFIX 137 
H2A   2    0.611394    0.418827    0.308847    11.00000   -1.50000 
H2B   2    0.558876    0.292161    0.374368    11.00000   -1.50000 
H2C   2    0.707507    0.278625    0.283218    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_0505r1 in P2(1)/n 
REM R1 =  0.0205 for    1570 Fo > 4sig(Fo)  and  0.0233 for all    1690 data 
REM     75 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0288      0.9126 
  
REM Highest difference peak  0.570,  deepest hole -0.582,  1-sigma level  0.096 
Q1    1   0.7761  0.3595  0.3818  11.00000  0.05    0.57 
Q2    1   1.0574  0.2369  0.4935  11.00000  0.05    0.49 
Q3    1   1.1822  0.1496  0.5270  11.00000  0.05    0.48 
Q4    1   0.9581  0.2033  0.6464  11.00000  0.05    0.42 
Q5    1   1.1798  0.1440  0.4174  11.00000  0.05    0.42 
;
_shelx_res_checksum              92062

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_1604r1
_database_code_depnum_ccdc_archive 'CCDC 1494383'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 H12 Cl8 Nb2 Se2'
_chemical_formula_sum            'C4 H12 Cl8 Nb2 Se2'
_chemical_formula_weight         687.48

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

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

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

_cell_length_a                   10.4725(8)
_cell_length_b                   7.2592(5)
_cell_length_c                   22.5009(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1710.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2802
_cell_measurement_theta_min      1.8230
_cell_measurement_theta_max      32.1190

_exptl_crystal_description       Chip
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.669
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    6.818
_shelx_estimated_absorpt_T_min   0.727
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70713
_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            5388
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.810
_diffrn_reflns_theta_max         25.988
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             888
_reflns_number_gt                763
_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] 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         888
_refine_ls_number_parameters     44
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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 0.5000 0.03576(7) 0.43316(2) 0.01067(17) Uani 1 2 d S T P . .
Se1 Se 0.5000 0.35278(8) 0.36610(2) 0.01460(18) Uani 1 2 d S T P . .
Cl1 Cl 0.28284(11) 0.07819(15) 0.42927(4) 0.0150(3) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 -0.1318(2) 0.34196(5) 0.0162(3) Uani 1 2 d S T P . .
Cl3 Cl 0.5000 -0.25681(18) 0.48329(5) 0.0127(3) Uani 1 2 d S T P . .
C1 C 0.3630(5) 0.3190(6) 0.30963(17) 0.0199(10) Uani 1 1 d . . . . .
H1A H 0.3724 0.4077 0.2771 0.030 Uiso 1 1 calc R U . . .
H1B H 0.2809 0.3386 0.3295 0.030 Uiso 1 1 calc R U . . .
H1C H 0.3663 0.1935 0.2937 0.030 Uiso 1 1 calc R U . . .

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 0.0146(3) 0.0108(3) 0.0066(3) -0.00034(19) 0.000 0.000
Se1 0.0218(4) 0.0130(3) 0.0090(3) 0.0016(2) 0.000 0.000
Cl1 0.0157(6) 0.0164(5) 0.0129(5) 0.0002(4) -0.0006(4) 0.0000(5)
Cl2 0.0230(9) 0.0176(8) 0.0082(6) -0.0034(5) 0.000 0.000
Cl3 0.0190(8) 0.0106(7) 0.0086(6) -0.0007(5) 0.000 0.000
C1 0.022(3) 0.024(2) 0.013(2) 0.0052(17) -0.0051(18) 0.001(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 2.2966(12) 12_655 ?
Nb1 Cl1 2.2966(12) . ?
Nb1 Cl2 2.3854(13) . ?
Nb1 Cl3 2.4048(14) . ?
Nb1 Cl3 2.4715(13) 9_656 ?
Nb1 Se1 2.7518(8) . ?
Nb1 Nb1 3.0524(9) 9_656 ?
Se1 C1 1.932(4) 12_655 ?
Se1 C1 1.932(4) . ?
Cl3 Nb1 2.4716(13) 9_656 ?
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 Nb1 Cl1 163.98(6) 12_655 . ?
Cl1 Nb1 Cl2 92.04(3) 12_655 . ?
Cl1 Nb1 Cl2 92.04(3) . . ?
Cl1 Nb1 Cl3 97.83(3) 12_655 . ?
Cl1 Nb1 Cl3 97.83(3) . . ?
Cl2 Nb1 Cl3 87.32(5) . . ?
Cl1 Nb1 Cl3 86.67(3) 12_655 9_656 ?
Cl1 Nb1 Cl3 86.67(3) . 9_656 ?
Cl2 Nb1 Cl3 170.17(5) . 9_656 ?
Cl3 Nb1 Cl3 102.51(4) . 9_656 ?
Cl1 Nb1 Se1 82.36(3) 12_655 . ?
Cl1 Nb1 Se1 82.36(3) . . ?
Cl2 Nb1 Se1 87.40(4) . . ?
Cl3 Nb1 Se1 174.72(4) . . ?
Cl3 Nb1 Se1 82.77(4) 9_656 . ?
Cl1 Nb1 Nb1 93.46(2) 12_655 9_656 ?
Cl1 Nb1 Nb1 93.46(2) . 9_656 ?
Cl2 Nb1 Nb1 139.55(5) . 9_656 ?
Cl3 Nb1 Nb1 52.23(3) . 9_656 ?
Cl3 Nb1 Nb1 50.28(3) 9_656 9_656 ?
Se1 Nb1 Nb1 133.05(3) . 9_656 ?
C1 Se1 C1 95.9(3) 12_655 . ?
C1 Se1 Nb1 104.73(13) 12_655 . ?
C1 Se1 Nb1 104.73(13) . . ?
Nb1 Cl3 Nb1 77.49(4) . 9_656 ?
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 . . ?

_refine_diff_density_max         0.649
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.158

_shelx_res_file                  
; 
  
    2016_1604r1.res created by SHELXL-2014/7 
  
  
TITL 2016_1604r1 in Cmce 
CELL 0.71073  10.472544   7.259181  22.500915  90.0000  90.0000  90.0000 
ZERR    4.   0.000821   0.000540   0.001153   0.0000   0.0000   0.0000 
LATT 7 
SYMM -x,-y+1/2, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x,-y,-z 
SFAC C  H  Cl Se Nb 
UNIT 16 48 32 8 8 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
TEMP -173 
SIZE 0.05 0.03 0.02 
WGHT    0.030800 
FVAR       1.17365 
MOLE 1 
NB1   5    0.500000    0.035764    0.433160    10.50000    0.01462    0.01079 = 
         0.00661   -0.00034    0.00000    0.00000 
SE1   4    0.500000    0.352781    0.366104    10.50000    0.02183    0.01301 = 
         0.00896    0.00158    0.00000    0.00000 
CL1   3    0.282842    0.078187    0.429273    11.00000    0.01565    0.01638 = 
         0.01286    0.00016   -0.00065    0.00005 
CL2   3    0.500000   -0.131778    0.341963    10.50000    0.02299    0.01756 = 
         0.00815   -0.00339    0.00000    0.00000 
CL3   3    0.500000   -0.256806    0.483291    10.50000    0.01897    0.01062 = 
         0.00860   -0.00074    0.00000    0.00000 
C1    1    0.363015    0.318963    0.309633    11.00000    0.02172    0.02447 = 
         0.01336    0.00521   -0.00509    0.00104 
AFIX 137 
H1A   2    0.372400    0.407682    0.277097    11.00000   -1.50000 
H1B   2    0.280863    0.338590    0.329504    11.00000   -1.50000 
H1C   2    0.366299    0.193464    0.293655    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_1604r1 in Cmce 
REM R1 =  0.0291 for     763 Fo > 4sig(Fo)  and  0.0391 for all     888 data 
REM     44 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0311      0.0000 
  
REM Highest difference peak  0.649,  deepest hole -0.692,  1-sigma level  0.158 
Q1    1   0.5000 -0.2295  0.2716  10.50000  0.05    0.65 
Q2    1   0.3949  0.0534  0.4589  11.00000  0.05    0.64 
Q3    1   0.5000 -0.1200  0.4332  10.50000  0.05    0.58 
Q4    1   0.5000  0.4989  0.3701  10.50000  0.05    0.58 
Q5    1   0.4041  0.0565  0.4041  11.00000  0.05    0.58 
;
_shelx_res_checksum              28006

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_1905k4
_database_code_depnum_ccdc_archive 'CCDC 1494384'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 H24 Cl8 Nb2 Te4'
_chemical_formula_sum            'C8 H24 Cl8 Nb2 Te4'
_chemical_formula_weight         1100.09

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'
Nb Nb -2.0727 0.6215 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'

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

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

_cell_length_a                   10.48350(10)
_cell_length_b                   10.48350(10)
_cell_length_c                   12.0612(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1325.57(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10097
_cell_measurement_theta_min      2.5440
_cell_measurement_theta_max      31.9530

_exptl_crystal_description       block
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_F_000             996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    5.979
_shelx_estimated_absorpt_T_min   0.444
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70589
_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 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            8870
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.748
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1315
_reflns_number_gt                1310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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)+(0.0170P)²+0.4852P] 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 501 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.016(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1315
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0120
_refine_ls_R_factor_gt           0.0119
_refine_ls_wR_factor_ref         0.0295
_refine_ls_wR_factor_gt          0.0295
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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 0.40487(3) 0.59513(3) 1.0000 0.00786(9) Uani 1 2 d S T P . .
Te1 Te 0.43926(2) 0.81917(2) 0.85380(2) 0.01167(7) Uani 1 1 d . . . . .
Cl1 Cl 0.20471(7) 0.59929(8) 0.88859(6) 0.01211(16) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.5000 0.82338(8) 0.0111(2) Uani 1 2 d S T P . .
Cl3 Cl 0.64285(7) 0.64285(7) 1.0000 0.0106(2) Uani 1 2 d S T P . .
C1 C 0.3906(4) 0.7625(3) 0.6897(3) 0.0182(7) Uani 1 1 d . . . . .
H1A H 0.3087 0.7173 0.6907 0.027 Uiso 1 1 calc R U . . .
H1B H 0.4569 0.7058 0.6605 0.027 Uiso 1 1 calc R U . . .
H1C H 0.3837 0.8381 0.6424 0.027 Uiso 1 1 calc R U . . .
C2 C 0.2675(3) 0.9238(3) 0.8773(3) 0.0179(7) Uani 1 1 d . . . . .
H2A H 0.2549 0.9821 0.8147 0.027 Uiso 1 1 calc R U . . .
H2B H 0.2732 0.9730 0.9462 0.027 Uiso 1 1 calc R U . . .
H2C H 0.1954 0.8645 0.8817 0.027 Uiso 1 1 calc R U . . .

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 0.00750(13) 0.00750(13) 0.00859(18) -0.00015(11) -0.00015(11) 0.00014(15)
Te1 0.01194(11) 0.00946(11) 0.01360(11) 0.00222(8) -0.00042(8) -0.00001(8)
Cl1 0.0102(4) 0.0132(4) 0.0130(4) -0.0005(3) -0.0024(3) 0.0004(3)
Cl2 0.0120(6) 0.0118(6) 0.0096(5) 0.000 0.000 0.0009(4)
Cl3 0.0089(3) 0.0089(3) 0.0140(5) 0.0003(3) -0.0003(3) -0.0010(4)
C1 0.025(2) 0.0163(18) 0.0128(15) 0.0020(13) -0.0007(14) 0.0022(16)
C2 0.0184(18) 0.0128(17) 0.0225(18) 0.0041(14) 0.0021(15) 0.0057(15)

_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 2.4922(8) . ?
Nb1 Cl1 2.4922(8) 8_667 ?
Nb1 Cl3 2.5445(9) 2_665 ?
Nb1 Cl3 2.5445(9) . ?
Nb1 Cl2 2.5548(9) . ?
Nb1 Cl2 2.5548(9) 7_557 ?
Nb1 Nb1 2.8208(8) 2_665 ?
Nb1 Te1 2.9591(3) . ?
Nb1 Te1 2.9591(3) 8_667 ?
Te1 C2 2.127(3) . ?
Te1 C1 2.128(3) . ?
Cl2 Nb1 2.5548(9) 2_665 ?
Cl3 Nb1 2.5445(9) 2_665 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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 Cl1 105.14(4) . 8_667 ?
Cl1 Nb1 Cl3 81.47(2) . 2_665 ?
Cl1 Nb1 Cl3 145.299(19) 8_667 2_665 ?
Cl1 Nb1 Cl3 145.299(19) . . ?
Cl1 Nb1 Cl3 81.47(2) 8_667 . ?
Cl3 Nb1 Cl3 112.68(3) 2_665 . ?
Cl1 Nb1 Cl2 83.45(2) . . ?
Cl1 Nb1 Cl2 141.729(19) 8_667 . ?
Cl3 Nb1 Cl2 72.182(11) 2_665 . ?
Cl3 Nb1 Cl2 72.182(11) . . ?
Cl1 Nb1 Cl2 141.729(19) . 7_557 ?
Cl1 Nb1 Cl2 83.45(2) 8_667 7_557 ?
Cl3 Nb1 Cl2 72.182(11) 2_665 7_557 ?
Cl3 Nb1 Cl2 72.183(11) . 7_557 ?
Cl2 Nb1 Cl2 112.99(3) . 7_557 ?
Cl1 Nb1 Nb1 127.43(2) . 2_665 ?
Cl1 Nb1 Nb1 127.43(2) 8_667 2_665 ?
Cl3 Nb1 Nb1 56.338(15) 2_665 2_665 ?
Cl3 Nb1 Nb1 56.339(15) . 2_665 ?
Cl2 Nb1 Nb1 56.493(14) . 2_665 ?
Cl2 Nb1 Nb1 56.493(14) 7_557 2_665 ?
Cl1 Nb1 Te1 76.55(2) . . ?
Cl1 Nb1 Te1 69.825(19) 8_667 . ?
Cl3 Nb1 Te1 143.341(5) 2_665 . ?
Cl3 Nb1 Te1 74.008(11) . . ?
Cl2 Nb1 Te1 76.432(10) . . ?
Cl2 Nb1 Te1 139.392(5) 7_557 . ?
Nb1 Nb1 Te1 118.367(8) 2_665 . ?
Cl1 Nb1 Te1 69.824(19) . 8_667 ?
Cl1 Nb1 Te1 76.55(2) 8_667 8_667 ?
Cl3 Nb1 Te1 74.009(11) 2_665 8_667 ?
Cl3 Nb1 Te1 143.342(5) . 8_667 ?
Cl2 Nb1 Te1 139.392(5) . 8_667 ?
Cl2 Nb1 Te1 76.432(10) 7_557 8_667 ?
Nb1 Nb1 Te1 118.368(8) 2_665 8_667 ?
Te1 Nb1 Te1 123.264(16) . 8_667 ?
C2 Te1 C1 93.72(14) . . ?
C2 Te1 Nb1 103.12(10) . . ?
C1 Te1 Nb1 107.65(10) . . ?
Nb1 Cl2 Nb1 67.02(3) . 2_665 ?
Nb1 Cl3 Nb1 67.32(3) . 2_665 ?
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 . . ?
Te1 C2 H2A 109.5 . . ?
Te1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Te1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.075

_shelx_res_file                  
; 
  
    2016_1905k4.res created by SHELXL-2014/7 
  
  
TITL 2016_1905k4 in P4(2)2(1)2 
CELL 0.71073  10.4835  10.4835  12.0612  90.000  90.000  90.000 
ZERR   2.0   0.0001   0.0001   0.0002   0.000   0.000   0.000 
LATT -1 
SYMM -X, -Y, Z 
SYMM 0.5-Y, 0.5+X, 0.5+Z 
SYMM 0.5+Y, 0.5-X, 0.5+Z 
SYMM 0.5-X, 0.5+Y, 0.5-Z 
SYMM 0.5+X, 0.5-Y, 0.5-Z 
SYMM Y, X, -Z 
SYMM -Y, -X, -Z 
SFAC C  H  Cl Nb Te 
UNIT 16 48 16 4 8 
OMIT  0   1   1 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND 
BOND $H 
FMAP 2 
PLAN 3 
SIZE 0.162 0.154 0.042 
TEMP -173 
WGHT    0.017000    0.485200 
FVAR       2.69666 
MOLE 1 
NB1   4    0.404872    0.595128    1.000000    10.50000    0.00750    0.00750 = 
         0.00859   -0.00015   -0.00015    0.00014 
TE1   5    0.439257    0.819173    0.853797    11.00000    0.01194    0.00946 = 
         0.01360    0.00222   -0.00042   -0.00001 
CL1   3    0.204705    0.599286    0.888589    11.00000    0.01019    0.01317 = 
         0.01297   -0.00045   -0.00243    0.00039 
CL2   3    0.500000    0.500000    0.823382    10.50000    0.01199    0.01178 = 
         0.00955    0.00000    0.00000    0.00090 
CL3   3    0.642848    0.642848    1.000000    10.50000    0.00893    0.00893 = 
         0.01397    0.00025   -0.00025   -0.00101 
C1    1    0.390599    0.762462    0.689742    11.00000    0.02533    0.01631 = 
         0.01281    0.00202   -0.00065    0.00218 
AFIX 137 
H1A   2    0.308746    0.717326    0.690742    11.00000   -1.50000 
H1B   2    0.456945    0.705824    0.660538    11.00000   -1.50000 
H1C   2    0.383700    0.838121    0.642400    11.00000   -1.50000 
AFIX   0 
C2    1    0.267547    0.923804    0.877263    11.00000    0.01842    0.01276 = 
         0.02251    0.00412    0.00213    0.00567 
AFIX 137 
H2A   2    0.254922    0.982081    0.814687    11.00000   -1.50000 
H2B   2    0.273171    0.972994    0.946183    11.00000   -1.50000 
H2C   2    0.195430    0.864548    0.881731    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_1905k4 in P4(2)2(1)2 
REM R1 =  0.0119 for    1310 Fo > 4sig(Fo)  and  0.0120 for all    1315 data 
REM     54 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0170      0.4852 
  
REM Highest difference peak  0.298,  deepest hole -0.236,  1-sigma level  0.075 
Q1    1   0.5201  0.6108  0.9956  11.00000  0.05    0.30 
Q2    1   0.4437  0.7133  0.8485  11.00000  0.05    0.28 
Q3    1   0.5000  0.5000  1.0000  10.25000  0.05    0.28 
;
_shelx_res_checksum              86614

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1494385'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 H20 Cl4 Nb S4'
_chemical_formula_sum            'C8 H20 Cl4 Nb S4'
_chemical_formula_weight         479.19

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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

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

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

_cell_length_a                   9.1410(4)
_cell_length_b                   9.1410(4)
_cell_length_c                   20.5742(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1719.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3796
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_F_000             964
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    1.786
_shelx_estimated_absorpt_T_min   0.859
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_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            7720
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.438
_diffrn_reflns_theta_max         25.989
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1691
_reflns_number_gt                1534
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.614
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0220P)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 547 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.01(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1691
_refine_ls_number_parameters     80
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 0.00706(4) 1.00706(4) 0.0000 0.01256(14) Uani 1 2 d S T P . .
Cl1 Cl 0.07994(13) 1.05085(12) 0.11512(4) 0.0182(3) Uani 1 1 d . . . . .
Cl2 Cl -0.22590(13) 1.12257(12) 0.03693(4) 0.0178(3) Uani 1 1 d . . . . .
S1 S 0.29835(12) 1.04125(13) 0.00809(4) 0.0178(2) Uani 1 1 d . . . . .
S2 S -0.09234(13) 0.78261(13) 0.07065(5) 0.0173(2) Uani 1 1 d . . . . .
C1 C 0.3901(5) 1.0177(6) -0.06890(18) 0.0254(12) Uani 1 1 d . . . . .
H1A H 0.3471 1.0839 -0.1011 0.038 Uiso 1 1 calc R U . . .
H1B H 0.3786 0.9163 -0.0836 0.038 Uiso 1 1 calc R U . . .
H1C H 0.4943 1.0399 -0.0638 0.038 Uiso 1 1 calc R U . . .
C2 C 0.3311(5) 1.2347(5) 0.02158(18) 0.0220(11) Uani 1 1 d . . . . .
H2A H 0.3116 1.2581 0.0678 0.026 Uiso 1 1 calc R U . . .
H2B H 0.4352 1.2567 0.0126 0.026 Uiso 1 1 calc R U . . .
C3 C -0.2171(6) 0.8347(5) 0.13408(19) 0.0251(12) Uani 1 1 d . . . . .
H3A H -0.3035 0.8813 0.1149 0.038 Uiso 1 1 calc R U . . .
H3B H -0.1687 0.9037 0.1635 0.038 Uiso 1 1 calc R U . . .
H3C H -0.2471 0.7476 0.1584 0.038 Uiso 1 1 calc R U . . .
C4 C -0.2174(5) 0.6820(5) 0.01888(19) 0.0215(11) Uani 1 1 d . . . . .
H4A H -0.1605 0.6215 -0.0120 0.026 Uiso 1 1 calc R U . . .
H4B H -0.2770 0.6152 0.0460 0.026 Uiso 1 1 calc R U . . .

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 0.01108(18) 0.01108(18) 0.0155(2) 0.00011(14) -0.00011(14) 0.0002(2)
Cl1 0.0213(7) 0.0161(6) 0.0172(4) -0.0004(4) -0.0027(4) 0.0009(5)
Cl2 0.0152(6) 0.0161(6) 0.0222(4) -0.0008(4) 0.0023(4) 0.0032(5)
S1 0.0134(6) 0.0186(6) 0.0214(4) 0.0035(4) -0.0013(4) -0.0019(5)
S2 0.0167(6) 0.0140(6) 0.0212(4) 0.0022(4) 0.0020(4) 0.0005(5)
C1 0.017(2) 0.032(3) 0.027(2) 0.008(2) 0.0057(18) 0.001(2)
C2 0.019(3) 0.021(3) 0.0265(19) 0.0019(19) -0.0019(19) -0.005(2)
C3 0.024(3) 0.025(3) 0.0264(19) 0.004(2) 0.008(2) -0.001(2)
C4 0.019(3) 0.017(3) 0.028(2) -0.0001(18) 0.0001(19) -0.003(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 2.4928(9) 7_465 ?
Nb1 Cl1 2.4928(9) . ?
Nb1 Cl2 2.4954(11) . ?
Nb1 Cl2 2.4954(11) 7_465 ?
Nb1 S2 2.6736(12) . ?
Nb1 S2 2.6736(12) 7_465 ?
Nb1 S1 2.6861(12) . ?
Nb1 S1 2.6861(12) 7_465 ?
S1 C1 1.805(4) . ?
S1 C2 1.814(5) . ?
S2 C3 1.797(4) . ?
S2 C4 1.814(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C2 1.530(8) 7_465 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C4 1.515(9) 7_465 ?
C4 H4A 0.9900 . ?
C4 H4B 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
Cl1 Nb1 Cl1 144.78(6) 7_465 . ?
Cl1 Nb1 Cl2 108.25(3) 7_465 . ?
Cl1 Nb1 Cl2 82.58(4) . . ?
Cl1 Nb1 Cl2 82.58(4) 7_465 7_465 ?
Cl1 Nb1 Cl2 108.26(3) . 7_465 ?
Cl2 Nb1 Cl2 144.58(6) . 7_465 ?
Cl1 Nb1 S2 140.92(4) 7_465 . ?
Cl1 Nb1 S2 72.39(3) . . ?
Cl2 Nb1 S2 82.48(4) . . ?
Cl2 Nb1 S2 69.79(4) 7_465 . ?
Cl1 Nb1 S2 72.39(3) 7_465 7_465 ?
Cl1 Nb1 S2 140.92(4) . 7_465 ?
Cl2 Nb1 S2 69.79(4) . 7_465 ?
Cl2 Nb1 S2 82.48(4) 7_465 7_465 ?
S2 Nb1 S2 76.94(5) . 7_465 ?
Cl1 Nb1 S1 82.45(3) 7_465 . ?
Cl1 Nb1 S1 69.97(3) . . ?
Cl2 Nb1 S1 141.06(4) . . ?
Cl2 Nb1 S1 72.47(4) 7_465 . ?
S2 Nb1 S1 113.11(3) . . ?
S2 Nb1 S1 146.50(3) 7_465 . ?
Cl1 Nb1 S1 69.97(3) 7_465 7_465 ?
Cl1 Nb1 S1 82.45(3) . 7_465 ?
Cl2 Nb1 S1 72.47(4) . 7_465 ?
Cl2 Nb1 S1 141.06(4) 7_465 7_465 ?
S2 Nb1 S1 146.51(3) . 7_465 ?
S2 Nb1 S1 113.11(3) 7_465 7_465 ?
S1 Nb1 S1 76.89(5) . 7_465 ?
C1 S1 C2 100.0(2) . . ?
C1 S1 Nb1 113.08(16) . . ?
C2 S1 Nb1 106.64(16) . . ?
C3 S2 C4 99.3(2) . . ?
C3 S2 Nb1 114.01(16) . . ?
C4 S2 Nb1 106.52(14) . . ?
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 . . ?
C2 C2 S1 112.2(2) 7_465 . ?
C2 C2 H2A 109.2 7_465 . ?
S1 C2 H2A 109.2 . . ?
C2 C2 H2B 109.2 7_465 . ?
S1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C4 S2 112.1(2) 7_465 . ?
C4 C4 H4A 109.2 7_465 . ?
S2 C4 H4A 109.2 . . ?
C4 C4 H4B 109.2 7_465 . ?
S2 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.074

_shelx_res_file                  
; 
  
    shelx.res created by SHELXL-2014/7 
  
  
TITL shelx in P4(3)2(1)2 
CELL 0.71073   9.1410   9.1410  20.5742  90.000  90.000  90.000 
ZERR    4.00   0.0004   0.0004   0.0018   0.000   0.000   0.000 
LATT -1 
SYMM -X, -Y, 0.5+Z 
SYMM 0.5-Y, 0.5+X, 0.75+Z 
SYMM 0.5+Y, 0.5-X, 0.25+Z 
SYMM 0.5-X, 0.5+Y, 0.75-Z 
SYMM 0.5+X, 0.5-Y, 0.25-Z 
SYMM Y, X, -Z 
SYMM -Y, -X, 0.5-Z 
SFAC C  H  S  Cl Nb 
UNIT 32 80 16 16 4 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND 
FMAP 2 
PLAN 5 
BOND $H 
SIZE 0.088 0.064 0.034 
TEMP -173 
WGHT    0.022000 
FVAR       0.33914 
MOLE 1 
NB1   5    0.007064    1.007064    0.000000    10.50000    0.01108    0.01108 = 
         0.01550    0.00011   -0.00011    0.00015 
CL1   4    0.079945    1.050846    0.115121    11.00000    0.02129    0.01613 = 
         0.01718   -0.00044   -0.00273    0.00094 
CL2   4   -0.225901    1.122571    0.036931    11.00000    0.01521    0.01606 = 
         0.02221   -0.00080    0.00228    0.00320 
S1    3    0.298347    1.041254    0.008092    11.00000    0.01338    0.01862 = 
         0.02140    0.00348   -0.00133   -0.00189 
S2    3   -0.092345    0.782614    0.070654    11.00000    0.01667    0.01404 = 
         0.02116    0.00222    0.00200    0.00050 
C1    1    0.390063    1.017665   -0.068900    11.00000    0.01715    0.03184 = 
         0.02733    0.00844    0.00570    0.00057 
AFIX 137 
H1A   2    0.347096    1.083945   -0.101106    11.00000   -1.50000 
H1B   2    0.378574    0.916312   -0.083566    11.00000   -1.50000 
H1C   2    0.494311    1.039930   -0.063827    11.00000   -1.50000 
AFIX   0 
C2    1    0.331083    1.234664    0.021584    11.00000    0.01859    0.02085 = 
         0.02646    0.00191   -0.00188   -0.00548 
AFIX  23 
H2A   2    0.311616    1.258148    0.067754    11.00000   -1.20000 
H2B   2    0.435189    1.256709    0.012636    11.00000   -1.20000 
AFIX   0 
C3    1   -0.217103    0.834741    0.134085    11.00000    0.02434    0.02464 = 
         0.02644    0.00360    0.00847   -0.00118 
AFIX 137 
H3A   2   -0.303466    0.881275    0.114873    11.00000   -1.50000 
H3B   2   -0.168745    0.903748    0.163534    11.00000   -1.50000 
H3C   2   -0.247120    0.747621    0.158431    11.00000   -1.50000 
AFIX   0 
C4    1   -0.217432    0.681951    0.018876    11.00000    0.01921    0.01691 = 
         0.02845   -0.00005    0.00007   -0.00262 
AFIX  23 
H4A   2   -0.160490    0.621521   -0.012019    11.00000   -1.20000 
H4B   2   -0.277044    0.615216    0.045983    11.00000   -1.20000 
  
AFIX   0 
HKLF 4 
  
REM  shelx in P4(3)2(1)2 
REM R1 =  0.0266 for    1534 Fo > 4sig(Fo)  and  0.0326 for all    1691 data 
REM     80 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0220      0.0000 
  
REM Highest difference peak  0.402,  deepest hole -0.294,  1-sigma level  0.074 
Q1    1   0.3088  1.3088  0.0000  10.50000  0.05    0.40 
Q2    1   0.1804  1.0689  0.0012  11.00000  0.05    0.30 
Q3    1  -0.2073  1.0724 -0.0107  11.00000  0.05    0.29 
Q4    1  -0.0906  0.5000 -0.0086  11.00000  0.05    0.28 
Q5    1  -0.2123  0.7877  0.0000  10.50000  0.05    0.28 
;
_shelx_res_checksum              72266

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_2801r2
_database_code_depnum_ccdc_archive 'CCDC 1494386'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_2016_2801r2         
;
PROBLEM: Check Calcd Residual Density  0.67A From     Nb1       2.07 eA-3  
RESPONSE: The maximun Q peaks are all within 1 angstrom of the heavy Nb 
atom, due to imperfect absorption correction.
;
# end Validation Reply Form

_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 Cl4 Nb S2'
_chemical_formula_sum            'C8 H18 Cl4 Nb S2'
_chemical_formula_weight         413.05

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                   8.7424(4)
_cell_length_b                   9.2175(3)
_cell_length_c                   19.6381(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.649(4)
_cell_angle_gamma                90
_cell_volume                     1564.49(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4510
_cell_measurement_theta_min      2.1810
_cell_measurement_theta_max      29.7200

_exptl_crystal_description       Chip
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    1.690
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64661
_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            10862
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.446
_diffrn_reflns_theta_max         29.903
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4029
_reflns_number_gt                2763
_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)+(0.0455P)²+8.5153P] 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         4029
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1403
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.19525(6) 0.76594(6) 0.14409(3) 0.02757(17) Uani 1 1 d . . . . .
S2 S 0.16572(15) 1.04619(15) 0.10916(7) 0.0175(3) Uani 1 1 d . . . . .
Cl4 Cl -0.03730(15) 0.82637(16) 0.18267(7) 0.0228(3) Uani 1 1 d . . . . .
S1 S 0.33853(15) 0.88347(15) 0.26280(7) 0.0197(3) Uani 1 1 d . . . . .
Cl1 Cl 0.45000(17) 0.79022(17) 0.12083(8) 0.0305(4) Uani 1 1 d . . . . .
Cl3 Cl 0.2275(2) 0.53870(18) 0.19317(10) 0.0450(5) Uani 1 1 d . . . . .
Cl2 Cl 0.0917(2) 0.6841(2) 0.03932(9) 0.0492(5) Uani 1 1 d . . . . .
C8 C 0.2772(7) 1.0372(7) -0.0098(3) 0.0266(13) Uani 1 1 d . . . . .
H8A H 0.1739 1.0677 -0.0316 0.040 Uiso 1 1 calc R U . . .
H8B H 0.2791 0.9315 -0.0042 0.040 Uiso 1 1 calc R U . . .
H8C H 0.3538 1.0661 -0.0389 0.040 Uiso 1 1 calc R U . . .
C6 C 0.3150(6) 1.1084(6) 0.0597(3) 0.0206(12) Uani 1 1 d . . . . .
H6 H 0.4183 1.0733 0.0826 0.025 Uiso 1 1 calc R U . . .
C5 C 0.2174(7) 1.1309(6) 0.1926(3) 0.0257(13) Uani 1 1 d . . . . .
H5A H 0.2342 1.2358 0.1858 0.031 Uiso 1 1 calc R U . . .
H5B H 0.1293 1.1211 0.2186 0.031 Uiso 1 1 calc R U . . .
C3 C 0.2738(7) 0.9984(7) 0.3869(3) 0.0281(13) Uani 1 1 d . . . . .
H3A H 0.2098 0.9924 0.4238 0.042 Uiso 1 1 calc R U . . .
H3B H 0.2718 1.0979 0.3692 0.042 Uiso 1 1 calc R U . . .
H3C H 0.3805 0.9713 0.4052 0.042 Uiso 1 1 calc R U . . .
C2 C 0.2101(6) 0.8947(6) 0.3285(3) 0.0224(12) Uani 1 1 d . . . . .
H2 H 0.1054 0.9285 0.3067 0.027 Uiso 1 1 calc R U . . .
C1 C 0.1983(8) 0.7416(7) 0.3550(3) 0.0315(14) Uani 1 1 d . . . . .
H1A H 0.3011 0.7079 0.3758 0.047 Uiso 1 1 calc R U . . .
H1B H 0.1576 0.6776 0.3167 0.047 Uiso 1 1 calc R U . . .
H1C H 0.1286 0.7401 0.3897 0.047 Uiso 1 1 calc R U . . .
C4 C 0.3602(7) 1.0689(6) 0.2356(3) 0.0267(13) Uani 1 1 d . . . . .
H4A H 0.3879 1.1303 0.2769 0.032 Uiso 1 1 calc R U . . .
H4B H 0.4470 1.0734 0.2085 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3180(8) 1.2728(7) 0.0549(3) 0.0332(15) Uani 1 1 d . . . . .
H7A H 0.3910 1.3022 0.0242 0.050 Uiso 1 1 calc R U . . .
H7B H 0.3504 1.3139 0.1008 0.050 Uiso 1 1 calc R U . . .
H7C H 0.2143 1.3083 0.0365 0.050 Uiso 1 1 calc R U . . .

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 0.0275(3) 0.0230(3) 0.0366(3) -0.0004(3) 0.0192(2) -0.0007(2)
S2 0.0186(6) 0.0192(7) 0.0158(6) 0.0027(5) 0.0058(5) 0.0029(5)
Cl4 0.0189(6) 0.0285(7) 0.0225(7) -0.0006(6) 0.0086(5) -0.0040(5)
S1 0.0189(6) 0.0232(7) 0.0169(6) 0.0047(6) 0.0024(5) -0.0032(6)
Cl1 0.0252(7) 0.0311(8) 0.0392(9) 0.0139(7) 0.0177(6) 0.0109(6)
Cl3 0.0609(12) 0.0223(8) 0.0583(12) 0.0026(8) 0.0295(9) 0.0007(8)
Cl2 0.0501(11) 0.0648(13) 0.0332(9) -0.0026(9) 0.0080(8) -0.0050(9)
C8 0.028(3) 0.036(4) 0.018(3) 0.002(3) 0.008(2) -0.004(3)
C6 0.020(3) 0.025(3) 0.018(3) 0.005(2) 0.006(2) 0.000(2)
C5 0.047(4) 0.014(3) 0.019(3) 0.000(2) 0.016(3) 0.001(3)
C3 0.032(3) 0.029(3) 0.023(3) 0.001(3) 0.006(3) -0.001(3)
C2 0.022(3) 0.028(3) 0.018(3) 0.001(2) 0.004(2) -0.003(2)
C1 0.041(4) 0.032(4) 0.024(3) 0.000(3) 0.014(3) -0.014(3)
C4 0.035(3) 0.030(3) 0.015(3) 0.001(2) 0.003(2) -0.013(3)
C7 0.042(4) 0.024(3) 0.035(4) 0.006(3) 0.009(3) -0.005(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl2 2.2500(19) . ?
Nb1 Cl3 2.3052(17) . ?
Nb1 Cl4 2.3411(14) . ?
Nb1 Cl1 2.3505(15) . ?
Nb1 S2 2.6752(15) . ?
Nb1 S1 2.7016(15) . ?
S2 C5 1.811(6) . ?
S2 C6 1.832(5) . ?
S1 C4 1.809(6) . ?
S1 C2 1.837(6) . ?
C8 C6 1.507(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C6 C7 1.519(8) . ?
C6 H6 1.0000 . ?
C5 C4 1.510(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C3 C2 1.532(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C2 C1 1.513(8) . ?
C2 H2 1.0000 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 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
Cl2 Nb1 Cl3 94.86(8) . . ?
Cl2 Nb1 Cl4 97.24(6) . . ?
Cl3 Nb1 Cl4 97.95(6) . . ?
Cl2 Nb1 Cl1 96.72(7) . . ?
Cl3 Nb1 Cl1 96.20(6) . . ?
Cl4 Nb1 Cl1 159.16(6) . . ?
Cl2 Nb1 S2 94.55(7) . . ?
Cl3 Nb1 S2 170.26(6) . . ?
Cl4 Nb1 S2 78.36(5) . . ?
Cl1 Nb1 S2 85.18(5) . . ?
Cl2 Nb1 S1 173.81(6) . . ?
Cl3 Nb1 S1 89.54(6) . . ?
Cl4 Nb1 S1 86.44(5) . . ?
Cl1 Nb1 S1 78.44(5) . . ?
S2 Nb1 S1 81.28(4) . . ?
C5 S2 C6 104.1(3) . . ?
C5 S2 Nb1 100.54(19) . . ?
C6 S2 Nb1 112.89(19) . . ?
C4 S1 C2 104.9(3) . . ?
C4 S1 Nb1 100.32(18) . . ?
C2 S1 Nb1 112.08(18) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C8 C6 C7 112.4(5) . . ?
C8 C6 S2 105.5(4) . . ?
C7 C6 S2 111.4(4) . . ?
C8 C6 H6 109.1 . . ?
C7 C6 H6 109.1 . . ?
S2 C6 H6 109.1 . . ?
C4 C5 S2 114.5(4) . . ?
C4 C5 H5A 108.6 . . ?
S2 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
S2 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
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 . . ?
C1 C2 C3 111.2(5) . . ?
C1 C2 S1 105.6(4) . . ?
C3 C2 S1 111.7(4) . . ?
C1 C2 H2 109.4 . . ?
C3 C2 H2 109.4 . . ?
S1 C2 H2 109.4 . . ?
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 . . ?
C5 C4 S1 114.1(4) . . ?
C5 C4 H4A 108.7 . . ?
S1 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
S1 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         2.370
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.166

_shelx_res_file                  
; 
  
    2016_2801r2.res created by SHELXL-2014/7 
  
  
TITL 2016_2801r2 in P2(1)/c 
CELL 0.71073   8.742372   9.217481  19.638078  90.0000  98.6485  90.0000 
ZERR   4.00   0.000381   0.000349   0.000857   0.0000   0.0041   0.0000 
LATT 1 
SYMM -x, y+1/2,-z+1/2 
SFAC C  H  S  Cl Nb 
UNIT 32 72 8 16 4 
OMIT 1 0 0 
OMIT 0 0 2 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.123 0.088 0.032 
TEMP -173 
WGHT    0.045500    8.515302 
FVAR       2.68919 
MOLE 1 
NB1   5    0.195251    0.765944    0.144092    11.00000    0.02752    0.02305 = 
         0.03657   -0.00045    0.01920   -0.00065 
S2    3    0.165721    1.046189    0.109161    11.00000    0.01856    0.01922 = 
         0.01581    0.00275    0.00584    0.00288 
CL4   4   -0.037303    0.826374    0.182670    11.00000    0.01894    0.02852 = 
         0.02250   -0.00061    0.00864   -0.00397 
S1    3    0.338530    0.883468    0.262800    11.00000    0.01892    0.02325 = 
         0.01689    0.00469    0.00242   -0.00319 
CL1   4    0.450004    0.790220    0.120834    11.00000    0.02519    0.03113 = 
         0.03916    0.01389    0.01773    0.01091 
CL3   4    0.227474    0.538703    0.193175    11.00000    0.06088    0.02226 = 
         0.05828    0.00259    0.02945    0.00068 
CL2   4    0.091684    0.684069    0.039319    11.00000    0.05011    0.06480 = 
         0.03315   -0.00262    0.00804   -0.00498 
C8    1    0.277171    1.037186   -0.009834    11.00000    0.02811    0.03555 = 
         0.01750    0.00208    0.00763   -0.00378 
AFIX 137 
H8A   2    0.173945    1.067686   -0.031623    11.00000   -1.50000 
H8B   2    0.279112    0.931521   -0.004239    11.00000   -1.50000 
H8C   2    0.353827    1.066060   -0.038884    11.00000   -1.50000 
AFIX   0 
C6    1    0.315037    1.108357    0.059731    11.00000    0.01969    0.02512 = 
         0.01794    0.00452    0.00588   -0.00007 
AFIX  13 
H6    2    0.418335    1.073338    0.082644    11.00000   -1.20000 
AFIX   0 
C5    1    0.217442    1.130915    0.192649    11.00000    0.04670    0.01436 = 
         0.01946    0.00002    0.01565    0.00051 
AFIX  23 
H5A   2    0.234162    1.235795    0.185773    11.00000   -1.20000 
H5B   2    0.129345    1.121069    0.218638    11.00000   -1.20000 
AFIX   0 
C3    1    0.273781    0.998431    0.386939    11.00000    0.03242    0.02945 = 
         0.02293    0.00063    0.00572   -0.00149 
AFIX 137 
H3A   2    0.209787    0.992435    0.423755    11.00000   -1.50000 
H3B   2    0.271848    1.097916    0.369227    11.00000   -1.50000 
H3C   2    0.380467    0.971288    0.405188    11.00000   -1.50000 
AFIX   0 
C2    1    0.210061    0.894709    0.328547    11.00000    0.02226    0.02760 = 
         0.01775    0.00084    0.00433   -0.00345 
AFIX  13 
H2    2    0.105405    0.928500    0.306713    11.00000   -1.20000 
AFIX   0 
C1    1    0.198301    0.741564    0.355014    11.00000    0.04135    0.03179 = 
         0.02396   -0.00002    0.01381   -0.01351 
AFIX 137 
H1A   2    0.301099    0.707866    0.375798    11.00000   -1.50000 
H1B   2    0.157606    0.677567    0.316692    11.00000   -1.50000 
H1C   2    0.128583    0.740069    0.389696    11.00000   -1.50000 
AFIX   0 
C4    1    0.360204    1.068858    0.235555    11.00000    0.03467    0.02992 = 
         0.01532    0.00142    0.00317   -0.01311 
AFIX  23 
H4A   2    0.387905    1.130282    0.276927    11.00000   -1.20000 
H4B   2    0.447014    1.073384    0.208547    11.00000   -1.20000 
AFIX   0 
C7    1    0.317951    1.272804    0.054853    11.00000    0.04217    0.02387 = 
         0.03474    0.00556    0.00922   -0.00502 
AFIX 137 
H7A   2    0.391025    1.302206    0.024170    11.00000   -1.50000 
H7B   2    0.350414    1.313945    0.100768    11.00000   -1.50000 
H7C   2    0.214293    1.308339    0.036475    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_2801r2 in P2(1)/c 
REM R1 =  0.0614 for    2763 Fo > 4sig(Fo)  and  0.1053 for all    4029 data 
REM    140 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0455      8.5151 
  
REM Highest difference peak  2.370,  deepest hole -1.881,  1-sigma level  0.166 
Q1    1   0.1507  0.7667  0.1115  11.00000  0.05    2.37 
Q2    1   0.2114  0.6928  0.1525  11.00000  0.05    1.74 
Q3    1   0.1097  0.7632  0.0687  11.00000  0.05    1.26 
Q4    1   0.2169  0.7920  0.1528  11.00000  0.05    1.17 
Q5    1   0.2634  0.6207  0.1930  11.00000  0.05    0.69 
;
_shelx_res_checksum              75787

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1494387'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 Cl4 Nb S2'
_chemical_formula_sum            'C5 H12 Cl4 Nb S2'
_chemical_formula_weight         370.98

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      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'

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

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

_cell_length_a                   9.964(3)
_cell_length_b                   9.964(3)
_cell_length_c                   25.113(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2493(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2212
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      27.4

_exptl_crystal_description       Chip
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.027
_exptl_absorpt_coefficient_mu    2.108
_shelx_estimated_absorpt_T_min   0.863
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_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            3934
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.199
_diffrn_reflns_theta_max         25.992
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1225
_reflns_number_gt                841
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0618P)²+1.5104P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.1(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1225
_refine_ls_number_parameters     58
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 0.5000 1.00018(4) 0.0374(4) Uani 1 2 d S T P . .
S1 S 0.0890(5) 0.6554(4) 0.92322(10) 0.0581(11) Uani 1 1 d . . . . .
Cl1 Cl -0.0693(4) 0.3420(4) 1.06393(8) 0.0555(10) Uani 1 1 d . . . . .
Cl2 Cl 0.2074(4) 0.3957(4) 0.98830(12) 0.0660(10) Uani 1 1 d . . . . .
C1 C 0.0455(18) 0.8246(12) 0.9379(4) 0.068(5) Uani 1 1 d . . . . .
H1A H 0.0956 0.8850 0.9144 0.101 Uiso 1 1 calc R U . . .
H1B H 0.0680 0.8444 0.9751 0.101 Uiso 1 1 calc R U . . .
H1C H -0.0510 0.8375 0.9324 0.101 Uiso 1 1 calc R U . . .
C2 C -0.0279(19) 0.6246(14) 0.8679(4) 0.075(5) Uani 1 1 d . . . . .
H2A H -0.1201 0.6190 0.8825 0.090 Uiso 1 1 calc R U . . .
H2B H -0.0249 0.7025 0.8435 0.090 Uiso 1 1 calc R U . . .
C3 C 0.0000 0.5000 0.8366(6) 0.061(5) Uani 1 2 d S T P . .
H3A H 0.0781 0.5175 0.8133 0.073 Uiso 0.5 1 calc R U P . .
H3B H -0.0781 0.4825 0.8133 0.073 Uiso 0.5 1 calc R U P . .

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 0.0456(9) 0.0483(9) 0.0183(5) 0.000 0.000 -0.0079(8)
S1 0.085(3) 0.056(2) 0.0327(11) 0.0073(15) 0.0136(16) -0.003(2)
Cl1 0.081(3) 0.059(2) 0.0258(9) 0.0059(14) 0.0025(14) -0.023(2)
Cl2 0.0514(19) 0.088(3) 0.0583(15) 0.0115(18) 0.0058(15) 0.009(2)
C1 0.120(14) 0.035(7) 0.048(5) 0.003(6) 0.021(8) -0.010(9)
C2 0.130(16) 0.066(9) 0.028(4) 0.012(6) -0.008(7) 0.021(12)
C3 0.093(16) 0.056(12) 0.033(7) 0.000 0.000 0.015(16)

_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 Cl2 2.332(4) . ?
Nb1 Cl2 2.332(4) 2_565 ?
Nb1 Cl1 2.349(3) 2_565 ?
Nb1 Cl1 2.349(3) . ?
Nb1 S1 2.630(3) 2_565 ?
Nb1 S1 2.630(3) . ?
S1 C1 1.780(13) . ?
S1 C2 1.838(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.496(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.496(15) 2_565 ?
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
Cl2 Nb1 Cl2 165.30(16) . 2_565 ?
Cl2 Nb1 Cl1 97.22(15) . 2_565 ?
Cl2 Nb1 Cl1 92.80(15) 2_565 2_565 ?
Cl2 Nb1 Cl1 92.79(15) . . ?
Cl2 Nb1 Cl1 97.22(15) 2_565 . ?
Cl1 Nb1 Cl1 94.08(15) 2_565 . ?
Cl2 Nb1 S1 86.69(14) . 2_565 ?
Cl2 Nb1 S1 82.51(14) 2_565 2_565 ?
Cl1 Nb1 S1 173.88(13) 2_565 2_565 ?
Cl1 Nb1 S1 90.42(10) . 2_565 ?
Cl2 Nb1 S1 82.51(14) . . ?
Cl2 Nb1 S1 86.69(14) 2_565 . ?
Cl1 Nb1 S1 90.42(10) 2_565 . ?
Cl1 Nb1 S1 173.88(13) . . ?
S1 Nb1 S1 85.41(16) 2_565 . ?
C1 S1 C2 99.2(7) . . ?
C1 S1 Nb1 108.8(4) . . ?
C2 S1 Nb1 104.1(5) . . ?
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 114.6(10) . . ?
C3 C2 H2A 108.6 . . ?
S1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
S1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 C2 116.6(12) . 2_565 ?
C2 C3 H3A 108.1 . . ?
C2 C3 H3A 108.1 2_565 . ?
C2 C3 H3B 108.1 . . ?
C2 C3 H3B 108.1 2_565 . ?
H3A C3 H3B 107.3 . . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.120

_shelx_res_file                  
; 
  
    shelx.res created by SHELXL-2014/7 
  
  
TITL shelx in I-42d 
CELL 0.71073   9.9644   9.9644  25.1132  90.000  90.000  90.000 
ZERR    8.00   0.0034   0.0034   0.0118   0.000   0.000   0.000 
LATT -2 
SYMM -X, -Y, Z 
SYMM Y, -X, -Z 
SYMM -Y, X, -Z 
SYMM 0.5-X, Y, 0.75-Z 
SYMM 0.5+X, -Y, 0.75-Z 
SYMM 0.5-Y, -X, 0.75+Z 
SYMM 0.5+Y, X, 0.75+Z 
SFAC C  H  S  Cl Nb 
UNIT 40 96 16 32 8 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
TWIN 
SIZE 0.072 0.048 0.027 
TEMP -173 
WGHT    0.061800    1.510400 
BASF   0.13637 
FVAR       0.17661 
MOLE 1 
NB1   5    0.000000    0.500000    1.000181    10.50000    0.04564    0.04829 = 
         0.01825    0.00000    0.00000   -0.00794 
S1    3    0.088971    0.655354    0.923218    11.00000    0.08530    0.05645 = 
         0.03269    0.00730    0.01363   -0.00281 
CL1   4   -0.069254    0.341975    1.063933    11.00000    0.08138    0.05932 = 
         0.02577    0.00593    0.00255   -0.02331 
CL2   4    0.207361    0.395702    0.988300    11.00000    0.05137    0.08835 = 
         0.05829    0.01153    0.00577    0.00919 
C1    1    0.045525    0.824569    0.937935    11.00000    0.12037    0.03451 = 
         0.04802    0.00287    0.02068   -0.01028 
AFIX 137 
H1A   2    0.095598    0.885016    0.914422    11.00000   -1.50000 
H1B   2    0.068022    0.844416    0.975099    11.00000   -1.50000 
H1C   2   -0.050969    0.837459    0.932389    11.00000   -1.50000 
AFIX   0 
C2    1   -0.027944    0.624644    0.867930    11.00000    0.13014    0.06555 = 
         0.02812    0.01199   -0.00759    0.02139 
AFIX  23 
H2A   2   -0.120122    0.618976    0.882466    11.00000   -1.20000 
H2B   2   -0.024915    0.702493    0.843466    11.00000   -1.20000 
AFIX   0 
C3    1    0.000000    0.500000    0.836647    10.50000    0.09304    0.05565 = 
         0.03328    0.00000    0.00000    0.01524 
AFIX  23 
H3A   2    0.078090    0.517506    0.813286    10.50000   -1.20000 
H3B   2   -0.078091    0.482491    0.813286    10.50000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  shelx in I-42d 
REM R1 =  0.0521 for     841 Fo > 4sig(Fo)  and  0.0821 for all    1225 data 
REM     58 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0617      1.5471 
  
REM Highest difference peak  0.867,  deepest hole -0.533,  1-sigma level  0.120 
Q1    1  -0.0175  0.6778  0.9213  11.00000  0.05    0.87 
Q2    1   0.1722  0.4402  0.9615  11.00000  0.05    0.71 
Q3    1  -0.0743  0.4978  0.9981  11.00000  0.05    0.63 
Q4    1  -0.0011  0.5824  1.0007  11.00000  0.05    0.58 
Q5    1   0.0000  0.5000  1.0271  10.50000  0.05    0.53 
;
_shelx_res_checksum              55139

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_2002r1
_database_code_depnum_ccdc_archive 'CCDC 1494388'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 Cl4 Nb S2'
_chemical_formula_sum            'C4 H10 Cl4 Nb S2'
_chemical_formula_weight         356.95

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                   7.2443(3)
_cell_length_b                   11.2723(4)
_cell_length_c                   7.9616(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.177(5)
_cell_angle_gamma                90
_cell_volume                     583.46(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3686
_cell_measurement_theta_min      2.8440
_cell_measurement_theta_max      32.1650

_exptl_crystal_description       Chip
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_F_000             350
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.248
_shelx_estimated_absorpt_T_min   0.823
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82060
_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            3485
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.851
_diffrn_reflns_theta_max         25.997
_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 0.877
_diffrn_reflns_point_group_measured_fraction_full 0.885
_reflns_number_total             2002
_reflns_number_gt                1984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.667
_reflns_Friedel_fraction_max     0.741
_reflns_Friedel_fraction_full    0.757

_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)+(0.0293P)²+0.2907P] 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 
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.03(6)
_chemical_absolute_configuration 'flack(1983),1096 Friedel Pair'
_refine_ls_number_reflns         2002
_refine_ls_number_parameters     102
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0177
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.005
_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 0.69286(5) 0.22470(3) 0.24990(4) 0.01318(10) Uani 1 1 d . . . . .
Cl1 Cl 0.70056(16) 0.10858(9) 0.49550(13) 0.0219(2) Uani 1 1 d . . . . .
Cl2 Cl 0.47016(14) 0.37145(8) 0.26797(13) 0.0176(2) Uani 1 1 d . . . . .
Cl3 Cl 0.99618(14) 0.32939(9) 0.41952(14) 0.0217(2) Uani 1 1 d . . . . .
Cl4 Cl 0.43294(14) 0.11705(8) 0.01104(12) 0.0163(2) Uani 1 1 d . . . . .
S1 S 0.91189(15) 0.06001(8) 0.18831(13) 0.0150(2) Uani 1 1 d . . . . .
S2 S 0.74266(14) 0.33241(8) -0.02352(13) 0.01397(19) Uani 1 1 d . . . . .
C1 C 1.1803(6) 0.0775(4) 0.3453(6) 0.0203(8) Uani 1 1 d . . . . .
H1A H 1.2623 0.0256 0.3057 0.030 Uiso 1 1 calc R U . . .
H1B H 1.2039 0.0563 0.4726 0.030 Uiso 1 1 calc R U . . .
H1C H 1.2210 0.1602 0.3432 0.030 Uiso 1 1 calc R U . . .
C2 C 0.9024(6) 0.1069(4) -0.0329(5) 0.0158(8) Uani 1 1 d . . . . .
H2A H 1.0093 0.0633 -0.0535 0.019 Uiso 1 1 calc R U . . .
H2B H 0.7671 0.0843 -0.1346 0.019 Uiso 1 1 calc R U . . .
C3 C 0.9343(6) 0.2393(4) -0.0465(5) 0.0161(8) Uani 1 1 d . . . . .
H3A H 0.9338 0.2558 -0.1689 0.019 Uiso 1 1 calc R U . . .
H3B H 1.0716 0.2613 0.0524 0.019 Uiso 1 1 calc R U . . .
C4 C 0.5197(6) 0.3128(4) -0.2460(5) 0.0177(8) Uani 1 1 d . . . . .
H4A H 0.5441 0.3512 -0.3449 0.027 Uiso 1 1 calc R U . . .
H4B H 0.3993 0.3488 -0.2405 0.027 Uiso 1 1 calc R U . . .
H4C H 0.4948 0.2280 -0.2733 0.027 Uiso 1 1 calc R U . . .

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 0.00954(15) 0.01234(16) 0.01546(15) -0.00119(14) 0.00352(11) 0.00005(13)
Cl1 0.0243(5) 0.0235(5) 0.0186(4) 0.0030(4) 0.0100(4) 0.0034(4)
Cl2 0.0160(4) 0.0165(4) 0.0204(5) 0.0002(4) 0.0083(4) 0.0042(4)
Cl3 0.0124(4) 0.0209(5) 0.0259(5) -0.0080(4) 0.0029(4) -0.0029(4)
Cl4 0.0125(4) 0.0167(4) 0.0181(4) -0.0035(4) 0.0053(4) -0.0048(4)
S1 0.0130(4) 0.0129(4) 0.0183(5) 0.0017(4) 0.0062(4) 0.0018(4)
S2 0.0131(4) 0.0115(4) 0.0170(4) 0.0005(4) 0.0064(3) 0.0004(4)
C1 0.0130(18) 0.025(2) 0.0198(19) 0.0007(17) 0.0040(15) 0.0026(18)
C2 0.0161(18) 0.0156(19) 0.0166(18) -0.0012(16) 0.0080(15) 0.0003(16)
C3 0.0121(16) 0.016(2) 0.0209(17) 0.0022(17) 0.0083(14) 0.0008(17)
C4 0.0152(18) 0.021(2) 0.0142(17) 0.0026(16) 0.0042(15) 0.0020(17)

_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 Cl3 2.3295(10) . ?
Nb1 Cl1 2.3332(10) . ?
Nb1 Cl4 2.3399(9) . ?
Nb1 Cl2 2.3590(9) . ?
Nb1 S1 2.6250(10) . ?
Nb1 S2 2.6525(10) . ?
S1 C1 1.800(4) . ?
S1 C2 1.811(4) . ?
S2 C4 1.809(4) . ?
S2 C3 1.813(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.522(5) . ?
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
Cl3 Nb1 Cl1 97.51(4) . . ?
Cl3 Nb1 Cl4 161.61(3) . . ?
Cl1 Nb1 Cl4 95.93(4) . . ?
Cl3 Nb1 Cl2 96.03(4) . . ?
Cl1 Nb1 Cl2 96.11(4) . . ?
Cl4 Nb1 Cl2 94.96(3) . . ?
Cl3 Nb1 S1 88.47(3) . . ?
Cl1 Nb1 S1 88.10(3) . . ?
Cl4 Nb1 S1 79.48(3) . . ?
Cl2 Nb1 S1 173.37(3) . . ?
Cl3 Nb1 S2 78.98(4) . . ?
Cl1 Nb1 S2 169.41(4) . . ?
Cl4 Nb1 S2 85.55(3) . . ?
Cl2 Nb1 S2 94.20(3) . . ?
S1 Nb1 S2 81.85(3) . . ?
C1 S1 C2 102.09(19) . . ?
C1 S1 Nb1 110.46(14) . . ?
C2 S1 Nb1 102.05(13) . . ?
C4 S2 C3 102.90(18) . . ?
C4 S2 Nb1 111.22(13) . . ?
C3 S2 Nb1 101.85(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 114.4(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 114.4(3) . . ?
C2 C3 H3A 108.7 . . ?
S2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
S2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
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         0.453
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.064

_shelx_res_file                  
; 
  
    2016_2002r1.res created by SHELXL-2014/7 
  
  
TITL 2016_2002r1 in P2(1) 
CELL 0.71073   7.2443  11.2723   7.9616  90.000 116.177  90.000 
ZERR    2.00   0.0003   0.0004   0.0003   0.000   0.005   0.000 
LATT -1 
SYMM -X, 0.5+Y, -Z 
SFAC C  H  S  Cl Nb 
UNIT 8 20 4 8 2 
L.S. 4 
BOND $H 
FMAP 2 
TEMP -173 
SIZE 0.09 0.04 0.03 
PLAN 5 
MERG 2 
OMIT -4 52 
ACTA 
WGHT    0.029300    0.290700 
FVAR       0.27641 
MOLE 1 
NB1   5    0.692855    0.224701    0.249897    11.00000    0.00954    0.01234 = 
         0.01546   -0.00119    0.00352    0.00005 
CL1   4    0.700557    0.108577    0.495505    11.00000    0.02429    0.02345 = 
         0.01859    0.00296    0.01005    0.00342 
CL2   4    0.470159    0.371455    0.267966    11.00000    0.01603    0.01652 = 
         0.02043    0.00016    0.00831    0.00422 
CL3   4    0.996182    0.329390    0.419519    11.00000    0.01235    0.02086 = 
         0.02591   -0.00796    0.00289   -0.00286 
CL4   4    0.432943    0.117054    0.011036    11.00000    0.01248    0.01669 = 
         0.01814   -0.00345    0.00527   -0.00475 
S1    3    0.911888    0.060013    0.188311    11.00000    0.01301    0.01292 = 
         0.01830    0.00169    0.00622    0.00177 
S2    3    0.742656    0.332412   -0.023519    11.00000    0.01312    0.01152 = 
         0.01701    0.00048    0.00641    0.00042 
C1    1    1.180322    0.077537    0.345328    11.00000    0.01302    0.02456 = 
         0.01978    0.00072    0.00400    0.00261 
AFIX 137 
H1A   2    1.262297    0.025600    0.305686    11.00000   -1.50000 
H1B   2    1.203873    0.056320    0.472591    11.00000   -1.50000 
H1C   2    1.220979    0.160236    0.343215    11.00000   -1.50000 
AFIX   0 
C2    1    0.902368    0.106856   -0.032930    11.00000    0.01613    0.01557 = 
         0.01656   -0.00119    0.00799    0.00031 
AFIX  23 
H2A   2    1.009330    0.063332   -0.053524    11.00000   -1.20000 
H2B   2    0.767096    0.084345   -0.134609    11.00000   -1.20000 
AFIX   0 
C3    1    0.934273    0.239320   -0.046531    11.00000    0.01212    0.01630 = 
         0.02090    0.00219    0.00825    0.00079 
AFIX  23 
H3A   2    0.933769    0.255848   -0.168857    11.00000   -1.20000 
H3B   2    1.071566    0.261315    0.052437    11.00000   -1.20000 
AFIX   0 
C4    1    0.519659    0.312834   -0.246049    11.00000    0.01524    0.02119 = 
         0.01416    0.00255    0.00424    0.00199 
AFIX 137 
H4A   2    0.544064    0.351161   -0.344924    11.00000   -1.50000 
H4B   2    0.399295    0.348778   -0.240501    11.00000   -1.50000 
H4C   2    0.494805    0.227955   -0.273281    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_2002r1 in P2(1) 
REM R1 =  0.0177 for    1984 Fo > 4sig(Fo)  and  0.0178 for all    2002 data 
REM    102 parameters refined using      1 restraints 
  
END 
  
WGHT      0.0293      0.2900 
  
REM Highest difference peak  0.453,  deepest hole -0.321,  1-sigma level  0.064 
Q1    1   0.6761  0.2211  0.3331  11.00000  0.05    0.45 
Q2    1   0.8559  0.1035  0.2132  11.00000  0.05    0.32 
Q3    1   0.8378  0.2797 -0.0503  11.00000  0.05    0.32 
Q4    1   0.4746  0.2145  0.0042  11.00000  0.05    0.27 
Q5    1   0.4588  0.1582  0.1081  11.00000  0.05    0.24 
;
_shelx_res_checksum              79489

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_1802r3
_database_code_depnum_ccdc_archive 'CCDC 1494389'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 Cl4 Nb Se2'
_chemical_formula_sum            'C5 H12 Cl4 Nb Se2'
_chemical_formula_weight         464.78

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'
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                   9.9381(2)
_cell_length_b                   9.9381(2)
_cell_length_c                   26.2651(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2594.09(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6180
_cell_measurement_theta_min      2.2060
_cell_measurement_theta_max      32.0750

_exptl_crystal_description       Chip
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_F_000             1752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.317
_shelx_estimated_absorpt_T_min   0.668
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46954
_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            8738
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.551
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1281
_reflns_number_gt                1219
_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          'Refined as a 2-component twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+0.5224P] 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         1281
_refine_ls_number_parameters     58
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0697
_refine_ls_wR_factor_gt          0.0689
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 0.5000 0.7500 0.37878(2) 0.01383(16) Uani 1 2 d S T P . .
Se1 Se 0.60292(5) 0.59473(4) 0.30059(2) 0.01458(14) Uani 1 1 d . . . . .
Cl1 Cl 0.42081(12) 0.90676(12) 0.43926(5) 0.0222(3) Uani 1 1 d . . . . .
Cl2 Cl 0.29764(12) 0.63481(13) 0.36593(5) 0.0193(3) Uani 1 1 d . . . . .
C1 C 0.5453(5) 0.4126(4) 0.3167(2) 0.0202(11) Uani 1 1 d . . . . .
H1A H 0.4471 0.4106 0.3203 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5870 0.3839 0.3487 0.030 Uiso 1 1 calc R U . . .
H1C H 0.5727 0.3517 0.2893 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4715(5) 0.6235(4) 0.2459(2) 0.0186(10) Uani 1 1 d . . . . .
H2A H 0.4722 0.5444 0.2229 0.022 Uiso 1 1 calc R U . . .
H2B H 0.3805 0.6305 0.2610 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5000 0.7500 0.2147(3) 0.0239(17) Uani 1 2 d S T P . .
H3A H 0.4216 0.7676 0.1924 0.029 Uiso 0.5 1 calc R U P . .
H3B H 0.5784 0.7324 0.1924 0.029 Uiso 0.5 1 calc R U P . .

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 0.0135(3) 0.0142(3) 0.0138(3) 0.000 0.000 -0.0009(2)
Se1 0.0130(2) 0.0152(2) 0.0156(3) -0.00019(18) 0.00034(18) 0.00187(19)
Cl1 0.0277(6) 0.0198(5) 0.0190(7) -0.0032(5) 0.0055(5) 0.0015(4)
Cl2 0.0141(5) 0.0212(6) 0.0227(7) 0.0009(5) 0.0008(4) -0.0032(4)
C1 0.029(3) 0.013(2) 0.019(3) -0.002(2) 0.001(2) -0.004(2)
C2 0.018(2) 0.020(2) 0.018(2) -0.002(2) -0.0065(19) 0.0033(19)
C3 0.030(4) 0.028(4) 0.014(4) 0.000 0.000 0.013(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl2 2.3386(12) . ?
Nb1 Cl2 2.3386(12) 6_564 ?
Nb1 Cl1 2.3600(13) . ?
Nb1 Cl1 2.3601(13) 6_564 ?
Nb1 Se1 2.7647(7) 6_564 ?
Nb1 Se1 2.7648(7) . ?
Se1 C1 1.945(4) . ?
Se1 C2 1.963(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.527(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.527(6) 6_564 ?
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
Cl2 Nb1 Cl2 163.40(7) . 6_564 ?
Cl2 Nb1 Cl1 97.67(4) . . ?
Cl2 Nb1 Cl1 93.49(4) 6_564 . ?
Cl2 Nb1 Cl1 93.49(4) . 6_564 ?
Cl2 Nb1 Cl1 97.67(4) 6_564 6_564 ?
Cl1 Nb1 Cl1 95.39(7) . 6_564 ?
Cl2 Nb1 Se1 81.25(3) . 6_564 ?
Cl2 Nb1 Se1 86.43(4) 6_564 6_564 ?
Cl1 Nb1 Se1 90.47(3) . 6_564 ?
Cl1 Nb1 Se1 172.62(3) 6_564 6_564 ?
Cl2 Nb1 Se1 86.43(4) . . ?
Cl2 Nb1 Se1 81.25(3) 6_564 . ?
Cl1 Nb1 Se1 172.62(3) . . ?
Cl1 Nb1 Se1 90.47(3) 6_564 . ?
Se1 Nb1 Se1 84.07(3) 6_564 . ?
C1 Se1 C2 95.7(2) . . ?
C1 Se1 Nb1 104.40(15) . . ?
C2 Se1 Nb1 102.50(15) . . ?
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 112.9(3) . . ?
C3 C2 H2A 109.0 . . ?
Se1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
Se1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C2 C3 C2 115.1(6) . 6_564 ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 6_564 . ?
C2 C3 H3B 108.5 . . ?
C2 C3 H3B 108.5 6_564 . ?
H3A C3 H3B 107.5 . . ?

_refine_diff_density_max         0.836
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.154

_shelx_res_file                  
; 
  
    2016_1802r3.res created by SHELXL-2014/7 
  
  
TITL 2016_1802r3 in I4(1)/a 
CELL 0.71073   9.9381   9.9381  26.2651  90.000  90.000  90.000 
ZERR    8.00   0.0002   0.0002   0.0011   0.000   0.000   0.000 
LATT 2 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM 0.75-Y, 0.25+X, 0.25+Z 
SYMM 0.75+Y, 0.75-X, 0.75+Z 
SFAC C  H  Cl Se Nb 
UNIT 40 96 32 16 8 
OMIT 0   1   1 
OMIT 0 4 6 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.06 0.05 0.03 
TWIN -1 0 0 0 1 0 0 0 -1 
TEMP -173 
WGHT    0.043300    0.522400 
BASF   0.45461 
FVAR       0.14716 
NB1   5    0.500000    0.750000    0.378779    10.50000    0.01354    0.01418 = 
         0.01378    0.00000    0.00000   -0.00092 
SE1   4    0.602924    0.594733    0.300595    11.00000    0.01299    0.01520 = 
         0.01555   -0.00019    0.00034    0.00187 
CL1   3    0.420807    0.906758    0.439259    11.00000    0.02769    0.01977 = 
         0.01903   -0.00319    0.00547    0.00149 
CL2   3    0.297638    0.634811    0.365925    11.00000    0.01408    0.02122 = 
         0.02270    0.00085    0.00083   -0.00319 
C1    1    0.545257    0.412617    0.316715    11.00000    0.02884    0.01252 = 
         0.01915   -0.00200    0.00116   -0.00399 
AFIX 137 
H1A   2    0.447113    0.410557    0.320254    11.00000   -1.50000 
H1B   2    0.586952    0.383883    0.348732    11.00000   -1.50000 
H1C   2    0.572652    0.351655    0.289280    11.00000   -1.50000 
AFIX   0 
C2    1    0.471521    0.623451    0.245887    11.00000    0.01762    0.02017 = 
         0.01804   -0.00238   -0.00648    0.00331 
AFIX  23 
H2A   2    0.472204    0.544414    0.222945    11.00000   -1.20000 
H2B   2    0.380481    0.630475    0.260955    11.00000   -1.20000 
AFIX   0 
C3    1    0.500000    0.750000    0.214704    10.50000    0.02963    0.02829 = 
         0.01375    0.00000    0.00000    0.01310 
AFIX  23 
H3A   2    0.421623    0.767639    0.192417    10.50000   -1.20000 
H3B   2    0.578376    0.732362    0.192417    10.50000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  2016_1802r3 in I4(1)/a 
REM R1 =  0.0281 for    1219 Fo > 4sig(Fo)  and  0.0302 for all    1281 data 
REM     58 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0432      0.5384 
  
REM Highest difference peak  0.836,  deepest hole -0.723,  1-sigma level  0.154 
Q1    1   0.5497  0.6736  0.3388  11.00000  0.05    0.84 
Q2    1   0.5823  0.8153  0.3795  11.00000  0.05    0.62 
Q3    1   0.6894  0.6654  0.3023  11.00000  0.05    0.62 
Q4    1   0.4928  0.6089  0.3138  11.00000  0.05    0.58 
Q5    1   0.4128  0.8205  0.3786  11.00000  0.05    0.54 
;
_shelx_res_checksum              36484

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_0602r3
_database_code_depnum_ccdc_archive 'CCDC 1494390'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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         'C12 H18 Cl4 Nb S2'
_chemical_formula_sum            'C12 H18 Cl4 Nb S2'
_chemical_formula_weight         461.09

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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   19.407(9)
_cell_length_b                   12.502(6)
_cell_length_c                   7.084(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1718.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3061
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Chip
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_F_000             924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.028
_exptl_absorpt_coefficient_mu    1.549
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_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            8916
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.061
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1768
_reflns_number_gt                1401
_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 XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0318P)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_number_reflns         1768
_refine_ls_number_parameters     92
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0681
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.11126(2) 0.2500 0.31388(6) 0.01693(13) Uani 1 2 d S T P . .
Cl1 Cl 0.22023(6) 0.2500 0.17556(17) 0.0231(3) Uani 1 2 d S T P . .
Cl2 Cl 0.03064(6) 0.2500 0.55702(17) 0.0217(3) Uani 1 2 d S T P . .
Cl3 Cl 0.06241(4) 0.11320(7) 0.12325(12) 0.0234(2) Uani 1 1 d . . . . .
S1 S 0.16510(4) 0.08570(6) 0.49928(12) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.11977(18) -0.1055(3) 0.6556(5) 0.0248(8) Uani 1 1 d . . . . .
H1A H 0.1444 -0.1433 0.5548 0.037 Uiso 1 1 calc R U . . .
H1B H 0.0803 -0.1485 0.6966 0.037 Uiso 1 1 calc R U . . .
H1C H 0.1509 -0.0941 0.7626 0.037 Uiso 1 1 calc R U . . .
C2 C 0.09468(17) 0.0014(3) 0.5827(5) 0.0226(8) Uani 1 1 d . . . . .
H2A H 0.0698 0.0391 0.6849 0.027 Uiso 1 1 calc R U . . .
H2B H 0.0618 -0.0107 0.4779 0.027 Uiso 1 1 calc R U . . .
C3 C 0.20140(18) 0.1286(3) 0.7252(5) 0.0213(7) Uani 1 1 d . . . . .
H3A H 0.1671 0.1720 0.7948 0.026 Uiso 1 1 calc R U . . .
H3B H 0.2128 0.0652 0.8029 0.026 Uiso 1 1 calc R U . . .
C4 C 0.26551(17) 0.1938(3) 0.6913(5) 0.0203(7) Uani 1 1 d . . . . .
C5 C 0.32738(18) 0.1401(3) 0.6593(5) 0.0224(7) Uani 1 1 d . . . . .
H5 H 0.3276 0.0641 0.6580 0.027 Uiso 1 1 calc R U . . .
C6 C 0.38843(18) 0.1946(3) 0.6292(5) 0.0249(8) Uani 1 1 d . . . . .
H6 H 0.4301 0.1564 0.6087 0.030 Uiso 1 1 calc R U . . .

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 0.0144(2) 0.0220(2) 0.0143(2) 0.000 -0.00006(18) 0.000
Cl1 0.0183(6) 0.0311(6) 0.0199(6) 0.000 0.0023(5) 0.000
Cl2 0.0176(6) 0.0257(6) 0.0217(6) 0.000 0.0045(5) 0.000
Cl3 0.0219(4) 0.0278(4) 0.0206(5) -0.0043(4) -0.0036(4) -0.0009(3)
S1 0.0170(4) 0.0213(4) 0.0170(5) 0.0007(3) 0.0002(3) 0.0001(3)
C1 0.0253(19) 0.0258(17) 0.023(2) 0.0020(15) -0.0001(16) -0.0018(14)
C2 0.0167(18) 0.0236(17) 0.027(2) 0.0034(15) 0.0019(15) -0.0027(13)
C3 0.0247(19) 0.0261(16) 0.0130(18) 0.0005(14) -0.0027(14) 0.0002(14)
C4 0.0221(18) 0.0286(17) 0.0101(16) 0.0021(15) -0.0038(15) 0.0006(13)
C5 0.0265(19) 0.0261(17) 0.0146(18) 0.0007(14) -0.0032(15) 0.0039(14)
C6 0.0162(17) 0.0409(19) 0.0174(18) -0.0011(16) -0.0030(15) 0.0052(14)

_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 Cl2 2.3269(14) . ?
Nb1 Cl1 2.3308(15) . ?
Nb1 Cl3 2.3763(11) 7_565 ?
Nb1 Cl3 2.3763(11) . ?
Nb1 S1 2.6524(11) . ?
Nb1 S1 2.6524(11) 7_565 ?
S1 C2 1.824(3) . ?
S1 C3 1.829(3) . ?
C1 C2 1.514(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.507(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.394(5) . ?
C4 C4 1.406(6) 7_565 ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C6 1.384(7) 7_565 ?
C6 H6 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Nb1 Cl1 157.11(5) . . ?
Cl2 Nb1 Cl3 98.77(4) . 7_565 ?
Cl1 Nb1 Cl3 97.07(4) . 7_565 ?
Cl2 Nb1 Cl3 98.77(4) . . ?
Cl1 Nb1 Cl3 97.07(4) . . ?
Cl3 Nb1 Cl3 92.05(5) 7_565 . ?
Cl2 Nb1 S1 84.17(4) . . ?
Cl1 Nb1 S1 81.41(3) . . ?
Cl3 Nb1 S1 174.76(3) 7_565 . ?
Cl3 Nb1 S1 83.18(4) . . ?
Cl2 Nb1 S1 84.17(4) . 7_565 ?
Cl1 Nb1 S1 81.41(3) . 7_565 ?
Cl3 Nb1 S1 83.18(4) 7_565 7_565 ?
Cl3 Nb1 S1 174.76(3) . 7_565 ?
S1 Nb1 S1 101.50(5) . 7_565 ?
C2 S1 C3 100.05(17) . . ?
C2 S1 Nb1 108.22(11) . . ?
C3 S1 Nb1 110.98(11) . . ?
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 112.3(2) . . ?
C1 C2 H2A 109.1 . . ?
S1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
S1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 S1 109.7(2) . . ?
C4 C3 H3A 109.7 . . ?
S1 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
S1 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 C4 118.8(2) . 7_565 ?
C5 C4 C3 118.5(3) . . ?
C4 C4 C3 122.75(18) 7_565 . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C6 C6 C5 119.5(2) 7_565 . ?
C6 C6 H6 120.2 7_565 . ?
C5 C6 H6 120.2 . . ?

_refine_diff_density_max         1.018
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.099

_shelx_res_file                  
; 
  
    0602r3.res created by SHELXL-2014/7 
  
  
TITL 0602r3 in Pnma 
CELL 0.71073  19.4067  12.5015   7.0839  90.000  90.000  90.000 
ZERR    4.00   0.0088   0.0056   0.0031   0.000   0.000   0.000 
LATT 1 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM -X, 0.5+Y, -Z 
SYMM 0.5+X, 0.5-Y, 0.5-Z 
SFAC C  H  S  Cl Nb 
UNIT 48 72 8 16 4 
OMIT 0 12 0 
OMIT 2 0 0 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.043 0.031 0.028 
TEMP -173 
WGHT    0.031800 
FVAR       0.16221 
MOLE 1 
NB1   5    0.111256    0.250000    0.313880    10.50000    0.01441    0.02205 = 
         0.01432    0.00000   -0.00006    0.00000 
CL1   4    0.220231    0.250000    0.175563    10.50000    0.01827    0.03111 = 
         0.01986    0.00000    0.00233    0.00000 
CL2   4    0.030636    0.250000    0.557024    10.50000    0.01763    0.02569 = 
         0.02172    0.00000    0.00447    0.00000 
CL3   4    0.062409    0.113203    0.123245    11.00000    0.02191    0.02775 = 
         0.02059   -0.00432   -0.00362   -0.00094 
S1    3    0.165097    0.085704    0.499279    11.00000    0.01695    0.02126 = 
         0.01698    0.00066    0.00021    0.00010 
C1    1    0.119774   -0.105545    0.655613    11.00000    0.02530    0.02575 = 
         0.02323    0.00199   -0.00009   -0.00181 
AFIX 137 
H1A   2    0.144376   -0.143293    0.554827    11.00000   -1.50000 
H1B   2    0.080267   -0.148485    0.696622    11.00000   -1.50000 
H1C   2    0.150922   -0.094089    0.762611    11.00000   -1.50000 
AFIX   0 
C2    1    0.094684    0.001402    0.582671    11.00000    0.01669    0.02358 = 
         0.02747    0.00337    0.00194   -0.00268 
AFIX  23 
H2A   2    0.069764    0.039092    0.684879    11.00000   -1.20000 
H2B   2    0.061845   -0.010716    0.477883    11.00000   -1.20000 
AFIX   0 
C3    1    0.201396    0.128589    0.725195    11.00000    0.02473    0.02610 = 
         0.01296    0.00052   -0.00267    0.00019 
AFIX  23 
H3A   2    0.167119    0.172018    0.794756    11.00000   -1.20000 
H3B   2    0.212773    0.065170    0.802871    11.00000   -1.20000 
AFIX   0 
C4    1    0.265507    0.193776    0.691342    11.00000    0.02206    0.02862 = 
         0.01012    0.00212   -0.00379    0.00056 
C5    1    0.327378    0.140101    0.659266    11.00000    0.02649    0.02607 = 
         0.01460    0.00074   -0.00321    0.00394 
AFIX  43 
H5    2    0.327625    0.064114    0.658039    11.00000   -1.20000 
AFIX   0 
C6    1    0.388431    0.194649    0.629174    11.00000    0.01624    0.04088 = 
         0.01744   -0.00106   -0.00298    0.00522 
AFIX  43 
H6    2    0.430056    0.156384    0.608659    11.00000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  0602r3 in Pnma 
REM R1 =  0.0328 for    1401 Fo > 4sig(Fo)  and  0.0486 for all    1768 data 
REM     92 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0321      0.0000 
  
REM Highest difference peak  1.018,  deepest hole -0.487,  1-sigma level  0.099 
Q1    1   0.1158  0.2500  0.9544  10.50000  0.05    1.02 
Q2    1   0.0681  0.2500  0.1641  10.50000  0.05    0.58 
Q3    1   0.0314  0.2500  0.6934  10.50000  0.05    0.48 
Q4    1   0.1705  0.0922  0.7940  11.00000  0.05    0.46 
Q5    1   0.3953  0.2500  0.5479  10.50000  0.05    0.45 
;
_shelx_res_checksum              13750

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_2015_0801ypc1
_database_code_depnum_ccdc_archive 'CCDC 1494391'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;





# start Validation Reply Form
_vrf_PLAT975_2015_0801ypc1       
;
PROBLEM: Check Calcd Residual Density  0.63A From      O1
RESPONSE: The oxygen forms a double bond with metal centre. (1.7 Angstrom)
          The oxidation state of metal centres are +5.
          The residuals are not hydrogen.
;
# end Validation Reply Form
_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 Nb O S'
_chemical_formula_sum            'C2 H6 Cl3 Nb O S'
_chemical_formula_weight         277.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   14.3522(11)
_cell_length_b                   14.9254(7)
_cell_length_c                   7.9099(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.049(7)
_cell_angle_gamma                90
_cell_volume                     1681.6(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4683
_cell_measurement_theta_min      2.7040
_cell_measurement_theta_max      29.3690

_exptl_crystal_description       Needle
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    2.548
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59489
_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            13175
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.729
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3295
_reflns_number_gt                2339
_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)+(0.0261P)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_number_reflns         3295
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0694
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 0.90516(4) 0.25568(3) 0.56478(6) 0.01056(14) Uani 1 1 d . . . . .
Nb2 Nb 0.37140(4) 0.24387(3) 0.35383(6) 0.01186(14) Uani 1 1 d . . . . .
Cl1 Cl 1.02463(11) 0.15180(9) 0.54159(16) 0.0183(3) Uani 1 1 d . . . . .
Cl2 Cl 0.99207(11) 0.38595(8) 0.56539(17) 0.0190(3) Uani 1 1 d . . . . .
Cl3 Cl 0.75707(10) 0.32452(8) 0.49949(17) 0.0174(3) Uani 1 1 d . . . . .
Cl4 Cl 0.21247(10) 0.21076(9) 0.28465(17) 0.0178(3) Uani 1 1 d . . . . .
Cl5 Cl 0.42600(11) 0.09633(9) 0.36047(18) 0.0220(4) Uani 1 1 d . . . . .
Cl6 Cl 0.51557(10) 0.31407(9) 0.33274(17) 0.0205(3) Uani 1 1 d . . . . .
O1 O 0.8993(3) 0.2434(2) 0.7825(4) 0.0136(8) Uani 1 1 d . . . . .
O2 O 0.3695(3) 0.2618(2) 0.5715(4) 0.0144(9) Uani 1 1 d . . . . .
S1 S 0.80478(11) 0.10642(9) 0.48076(17) 0.0165(3) Uani 1 1 d . . . . .
S2 S 0.30315(11) 0.40740(9) 0.26899(17) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.8416(4) 0.0281(3) 0.6489(7) 0.0229(15) Uani 1 1 d . . . . .
H1A H 0.8314 0.0543 0.7587 0.034 Uiso 1 1 calc R U . . .
H1B H 0.9084 0.0146 0.6491 0.034 Uiso 1 1 calc R U . . .
H1C H 0.8050 -0.0272 0.6303 0.034 Uiso 1 1 calc R U . . .
C2 C 0.6850(4) 0.1219(4) 0.5166(8) 0.0274(16) Uani 1 1 d . . . . .
H2A H 0.6524 0.0641 0.5075 0.041 Uiso 1 1 calc R U . . .
H2B H 0.6541 0.1633 0.4312 0.041 Uiso 1 1 calc R U . . .
H2C H 0.6828 0.1468 0.6307 0.041 Uiso 1 1 calc R U . . .
C3 C 0.3846(4) 0.4883(4) 0.3695(8) 0.0256(15) Uani 1 1 d . . . . .
H3A H 0.3562 0.5481 0.3594 0.038 Uiso 1 1 calc R U . . .
H3B H 0.4419 0.4880 0.3136 0.038 Uiso 1 1 calc R U . . .
H3C H 0.4003 0.4731 0.4901 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2072(4) 0.4260(4) 0.3908(7) 0.0215(15) Uani 1 1 d . . . . .
H4A H 0.2283 0.4155 0.5118 0.032 Uiso 1 1 calc R U . . .
H4B H 0.1558 0.3847 0.3523 0.032 Uiso 1 1 calc R U . . .
H4C H 0.1851 0.4879 0.3748 0.032 Uiso 1 1 calc R U . . .

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 0.0164(3) 0.0078(2) 0.0075(3) -0.0005(2) 0.0018(2) -0.0005(2)
Nb2 0.0166(3) 0.0109(2) 0.0082(3) 0.0007(2) 0.0021(2) 0.0005(2)
Cl1 0.0212(9) 0.0181(7) 0.0156(8) -0.0010(6) 0.0025(6) 0.0058(7)
Cl2 0.0235(9) 0.0139(7) 0.0196(8) 0.0010(6) 0.0021(7) -0.0060(7)
Cl3 0.0191(9) 0.0137(6) 0.0191(8) 0.0000(6) 0.0013(6) 0.0031(6)
Cl4 0.0178(9) 0.0152(6) 0.0201(8) -0.0019(6) 0.0011(6) -0.0029(6)
Cl5 0.0294(10) 0.0140(7) 0.0239(8) 0.0028(6) 0.0084(7) 0.0079(7)
Cl6 0.0157(8) 0.0239(7) 0.0220(8) 0.0013(6) 0.0026(6) -0.0024(7)
O1 0.021(2) 0.0101(18) 0.0099(19) 0.0004(16) 0.0010(17) 0.0028(18)
O2 0.023(2) 0.0132(19) 0.0079(19) -0.0008(16) 0.0032(17) 0.0000(18)
S1 0.0257(9) 0.0102(6) 0.0137(8) -0.0017(6) 0.0026(7) -0.0026(7)
S2 0.0229(9) 0.0131(7) 0.0144(8) 0.0001(6) 0.0051(7) 0.0007(7)
C1 0.033(4) 0.015(3) 0.020(3) 0.005(3) 0.003(3) -0.002(3)
C2 0.024(4) 0.015(3) 0.043(4) -0.005(3) 0.004(3) -0.011(3)
C3 0.021(4) 0.021(3) 0.034(4) -0.006(3) 0.001(3) -0.007(3)
C4 0.022(4) 0.020(3) 0.024(3) 0.003(3) 0.011(3) 0.004(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.744(3) . ?
Nb1 O1 2.224(3) 4_565 ?
Nb1 Cl2 2.3097(14) . ?
Nb1 Cl1 2.3355(14) . ?
Nb1 Cl3 2.3602(15) . ?
Nb1 S1 2.6917(15) . ?
Nb2 O2 1.746(3) . ?
Nb2 O2 2.232(3) 4_565 ?
Nb2 Cl4 2.3324(16) . ?
Nb2 Cl5 2.3357(14) . ?
Nb2 Cl6 2.3435(15) . ?
Nb2 S2 2.6844(14) . ?
O1 Nb1 2.224(3) 4_566 ?
O2 Nb2 2.232(3) 4_566 ?
S1 C2 1.792(6) . ?
S1 C1 1.800(5) . ?
S2 C4 1.797(5) . ?
S2 C3 1.797(6) . ?
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
O1 Nb1 O1 172.48(15) . 4_565 ?
O1 Nb1 Cl2 100.26(12) . . ?
O1 Nb1 Cl2 87.18(9) 4_565 . ?
O1 Nb1 Cl1 97.63(12) . . ?
O1 Nb1 Cl1 82.13(10) 4_565 . ?
Cl2 Nb1 Cl1 99.06(5) . . ?
O1 Nb1 Cl3 96.34(13) . . ?
O1 Nb1 Cl3 81.68(10) 4_565 . ?
Cl2 Nb1 Cl3 96.06(5) . . ?
Cl1 Nb1 Cl3 157.21(5) . . ?
O1 Nb1 S1 93.86(12) . . ?
O1 Nb1 S1 78.70(9) 4_565 . ?
Cl2 Nb1 S1 165.88(5) . . ?
Cl1 Nb1 S1 78.87(5) . . ?
Cl3 Nb1 S1 82.30(5) . . ?
O2 Nb2 O2 173.16(7) . 4_565 ?
O2 Nb2 Cl4 97.51(13) . . ?
O2 Nb2 Cl4 82.28(10) 4_565 . ?
O2 Nb2 Cl5 99.70(12) . . ?
O2 Nb2 Cl5 87.10(9) 4_565 . ?
Cl4 Nb2 Cl5 96.97(6) . . ?
O2 Nb2 Cl6 97.02(12) . . ?
O2 Nb2 Cl6 81.28(10) 4_565 . ?
Cl4 Nb2 Cl6 157.61(5) . . ?
Cl5 Nb2 Cl6 97.26(6) . . ?
O2 Nb2 S2 93.29(12) . . ?
O2 Nb2 S2 79.94(9) 4_565 . ?
Cl4 Nb2 S2 79.49(5) . . ?
Cl5 Nb2 S2 166.90(5) . . ?
Cl6 Nb2 S2 82.76(5) . . ?
Nb1 O1 Nb1 171.9(2) . 4_566 ?
Nb2 O2 Nb2 168.86(19) . 4_566 ?
C2 S1 C1 99.6(3) . . ?
C2 S1 Nb1 110.44(19) . . ?
C1 S1 Nb1 104.8(2) . . ?
C4 S2 C3 99.2(3) . . ?
C4 S2 Nb2 106.65(18) . . ?
C3 S2 Nb2 107.6(2) . . ?
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 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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         0.767
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.166

_shelx_res_file                  
; 
  
    2015_0801ypc1.res created by SHELXL-2014/7 
  
  
TITL 2015_0801ypc1 in P2(1)/c 
CELL 0.71073  14.352232  14.925446   7.909869  90.0000  97.0492  90.0000 
ZERR   8.0   0.001133   0.000743   0.000537   0.0000   0.0068   0.0000 
LATT 1 
SYMM -x, y+1/2,-z+1/2 
SFAC C  H  O  S  Cl Nb 
UNIT 16 48 8 8 24 8 
OMIT 1   1   0 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.173 0.028 0.024 
TEMP -173 
WGHT    0.026100 
FVAR       0.15116 
MOLE 1 
NB1   6    0.905164    0.255678    0.564783    11.00000    0.01642    0.00784 = 
         0.00749   -0.00053    0.00182   -0.00047 
NB2   6    0.371401    0.243867    0.353826    11.00000    0.01663    0.01087 = 
         0.00823    0.00072    0.00214    0.00049 
CL1   5    1.024626    0.151799    0.541588    11.00000    0.02117    0.01812 = 
         0.01562   -0.00103    0.00250    0.00576 
CL2   5    0.992071    0.385949    0.565395    11.00000    0.02346    0.01394 = 
         0.01960    0.00102    0.00214   -0.00600 
CL3   5    0.757075    0.324519    0.499489    11.00000    0.01912    0.01374 = 
         0.01912   -0.00004    0.00128    0.00313 
CL4   5    0.212474    0.210761    0.284645    11.00000    0.01784    0.01520 = 
         0.02013   -0.00192    0.00109   -0.00288 
CL5   5    0.425998    0.096331    0.360473    11.00000    0.02941    0.01404 = 
         0.02388    0.00277    0.00839    0.00793 
CL6   5    0.515574    0.314074    0.332743    11.00000    0.01574    0.02389 = 
         0.02198    0.00133    0.00261   -0.00238 
O1    3    0.899268    0.243383    0.782484    11.00000    0.02062    0.01011 = 
         0.00987    0.00036    0.00102    0.00275 
O2    3    0.369496    0.261847    0.571498    11.00000    0.02251    0.01323 = 
         0.00786   -0.00084    0.00318   -0.00001 
S1    4    0.804782    0.106419    0.480760    11.00000    0.02573    0.01017 = 
         0.01374   -0.00167    0.00263   -0.00260 
S2    4    0.303149    0.407399    0.268994    11.00000    0.02287    0.01308 = 
         0.01442    0.00006    0.00515    0.00075 
C1    1    0.841583    0.028113    0.648862    11.00000    0.03314    0.01507 = 
         0.02023    0.00481    0.00254   -0.00170 
AFIX 137 
H1A   2    0.831364    0.054320    0.758685    11.00000   -1.50000 
H1B   2    0.908421    0.014609    0.649098    11.00000   -1.50000 
H1C   2    0.804998   -0.027221    0.630316    11.00000   -1.50000 
AFIX   0 
C2    1    0.684957    0.121908    0.516587    11.00000    0.02395    0.01521 = 
         0.04300   -0.00494    0.00375   -0.01058 
AFIX 137 
H2A   2    0.652378    0.064084    0.507506    11.00000   -1.50000 
H2B   2    0.654114    0.163283    0.431168    11.00000   -1.50000 
H2C   2    0.682846    0.146827    0.630679    11.00000   -1.50000 
AFIX   0 
C3    1    0.384640    0.488336    0.369468    11.00000    0.02136    0.02098 = 
         0.03374   -0.00553    0.00073   -0.00682 
AFIX 137 
H3A   2    0.356156    0.548073    0.359440    11.00000   -1.50000 
H3B   2    0.441928    0.487969    0.313617    11.00000   -1.50000 
H3C   2    0.400266    0.473096    0.490128    11.00000   -1.50000 
AFIX   0 
C4    1    0.207155    0.425982    0.390810    11.00000    0.02208    0.02038 = 
         0.02417    0.00313    0.01105    0.00368 
AFIX 137 
H4A   2    0.228261    0.415497    0.511760    11.00000   -1.50000 
H4B   2    0.155801    0.384701    0.352337    11.00000   -1.50000 
H4C   2    0.185053    0.487881    0.374764    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2015_0801ypc1 in P2(1)/c 
REM R1 =  0.0409 for    2339 Fo > 4sig(Fo)  and  0.0743 for all    3295 data 
REM    149 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0261      0.0000 
  
REM Highest difference peak  0.767,  deepest hole -0.711,  1-sigma level  0.166 
Q1    1   0.8232  0.2732  0.5263  11.00000  0.05    0.77 
Q2    1   0.4049  0.1646  0.3914  11.00000  0.05    0.72 
Q3    1   0.2852  0.2279  0.3329  11.00000  0.05    0.70 
Q4    1   0.9486  0.3207  0.5994  11.00000  0.05    0.68 
Q5    1   0.3690  0.2353  0.2399  11.00000  0.05    0.65 
;
_shelx_res_checksum              1291

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_1405r3
_database_code_depnum_ccdc_archive 'CCDC 1494392'
_audit_update_record             
;
2016-07-18 deposited with the CCDC.
2016-09-13 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 O S2'
_chemical_formula_sum            'C4 H10 Cl3 Nb O S2'
_chemical_formula_weight         337.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   6.7898(3)
_cell_length_b                   6.9745(3)
_cell_length_c                   7.2523(4)
_cell_angle_alpha                108.917(4)
_cell_angle_beta                 99.404(4)
_cell_angle_gamma                113.677(4)
_cell_volume                     279.93(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6549
_cell_measurement_theta_min      3.1020
_cell_measurement_theta_max      32.1680

_exptl_crystal_description       Chip
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_F_000             166
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.112
_shelx_estimated_absorpt_T_min   0.959
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66440
_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            6650
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.156
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2205
_reflns_number_gt                2156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_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)+(0.0459P)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 1030 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.03(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2205
_refine_ls_number_parameters     102
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0628
_refine_ls_wR_factor_gt          0.0624
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.071
_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 0.47326(3) 0.87591(3) 0.74330(3) 0.01528(14) Uani 1 1 d . . . . .
Cl1 Cl 0.2952(2) 0.4950(2) 0.4724(2) 0.0193(3) Uani 1 1 d . . . . .
Cl2 Cl 0.2873(2) 1.0047(2) 0.5521(2) 0.0210(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5755(2) 1.1720(2) 1.0749(2) 0.0216(3) Uani 1 1 d . . . . .
S1 S 0.5349(2) 0.6331(2) 0.9428(2) 0.0165(3) Uani 1 1 d . . . . .
S2 S 0.0664(2) 0.7160(2) 0.8455(2) 0.0172(3) Uani 1 1 d . . . . .
O1 O 0.7410(7) 0.9741(7) 0.7229(6) 0.0214(9) Uani 1 1 d . . . . .
C1 C 0.6917(11) 0.8139(11) 1.2156(10) 0.0243(13) Uani 1 1 d . . . . .
H1A H 0.6151 0.8989 1.2747 0.036 Uiso 1 1 calc R U . . .
H1B H 0.8474 0.9244 1.2347 0.036 Uiso 1 1 calc R U . . .
H1C H 0.6976 0.7166 1.2858 0.036 Uiso 1 1 calc R U . . .
C2 C 0.2534(9) 0.4537(9) 0.9417(9) 0.0173(11) Uani 1 1 d . . . . .
H2A H 0.1609 0.3287 0.7999 0.021 Uiso 1 1 calc R U . . .
H2B H 0.2694 0.3793 1.0344 0.021 Uiso 1 1 calc R U . . .
C3 C 0.1248(10) 0.5832(10) 1.0098(10) 0.0198(12) Uani 1 1 d . . . . .
H3A H 0.2152 0.7057 1.1529 0.024 Uiso 1 1 calc R U . . .
H3B H -0.0221 0.4736 1.0121 0.024 Uiso 1 1 calc R U . . .
C4 C -0.1582(10) 0.4681(10) 0.6173(9) 0.0240(13) Uani 1 1 d . . . . .
H4A H -0.1075 0.3542 0.5648 0.036 Uiso 1 1 calc R U . . .
H4B H -0.1942 0.5180 0.5106 0.036 Uiso 1 1 calc R U . . .
H4C H -0.2949 0.3975 0.6524 0.036 Uiso 1 1 calc R U . . .

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 0.0157(2) 0.0158(2) 0.0136(2) 0.00615(17) 0.00353(18) 0.00765(18)
Cl1 0.0244(7) 0.0186(6) 0.0159(7) 0.0064(5) 0.0065(6) 0.0121(5)
Cl2 0.0255(7) 0.0197(6) 0.0180(7) 0.0074(5) 0.0036(6) 0.0131(6)
Cl3 0.0250(7) 0.0177(6) 0.0155(7) 0.0034(5) 0.0011(6) 0.0097(6)
S1 0.0164(7) 0.0205(6) 0.0154(7) 0.0085(5) 0.0048(5) 0.0110(5)
S2 0.0153(6) 0.0184(6) 0.0168(7) 0.0059(5) 0.0044(5) 0.0090(5)
O1 0.018(2) 0.026(2) 0.018(2) 0.0082(17) 0.0048(17) 0.0106(17)
C1 0.021(3) 0.029(3) 0.017(3) 0.008(2) -0.002(2) 0.011(3)
C2 0.018(3) 0.017(3) 0.017(3) 0.009(2) 0.005(2) 0.008(2)
C3 0.021(3) 0.023(3) 0.019(3) 0.010(2) 0.010(2) 0.011(2)
C4 0.015(3) 0.026(3) 0.018(3) 0.002(2) -0.001(2) 0.007(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 O1 1.718(4) . ?
Nb1 Cl2 2.3389(13) . ?
Nb1 Cl3 2.3693(13) . ?
Nb1 Cl1 2.3746(13) . ?
Nb1 S1 2.6642(13) . ?
Nb1 S2 2.8559(14) . ?
S1 C1 1.804(6) . ?
S1 C2 1.813(6) . ?
S2 C4 1.804(6) . ?
S2 C3 1.814(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.519(8) . ?
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
O1 Nb1 Cl2 105.17(15) . . ?
O1 Nb1 Cl3 97.22(14) . . ?
Cl2 Nb1 Cl3 97.03(5) . . ?
O1 Nb1 Cl1 98.34(14) . . ?
Cl2 Nb1 Cl1 93.59(5) . . ?
Cl3 Nb1 Cl1 158.15(5) . . ?
O1 Nb1 S1 93.95(14) . . ?
Cl2 Nb1 S1 159.99(5) . . ?
Cl3 Nb1 S1 86.16(4) . . ?
Cl1 Nb1 S1 77.56(4) . . ?
O1 Nb1 S2 169.79(14) . . ?
Cl2 Nb1 S2 83.98(5) . . ?
Cl3 Nb1 S2 76.86(5) . . ?
Cl1 Nb1 S2 85.38(4) . . ?
S1 Nb1 S2 77.50(4) . . ?
C1 S1 C2 102.4(3) . . ?
C1 S1 Nb1 111.9(2) . . ?
C2 S1 Nb1 105.04(18) . . ?
C4 S2 C3 102.2(3) . . ?
C4 S2 Nb1 107.7(2) . . ?
C3 S2 Nb1 102.4(2) . . ?
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 114.6(4) . . ?
C3 C2 H2A 108.6 . . ?
S1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
S1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 S2 114.1(4) . . ?
C2 C3 H3A 108.7 . . ?
S2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
S2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
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 . . ?

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
C1 S1 C2 C3 68.3(5) . . . . ?
Nb1 S1 C2 C3 -48.8(5) . . . . ?
S1 C2 C3 S2 61.7(5) . . . . ?
C4 S2 C3 C2 73.6(5) . . . . ?
Nb1 S2 C3 C2 -37.9(5) . . . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.093

_shelx_res_file                  
; 
  
    2016_1405r3.res created by SHELXL-2014/7 
  
  
TITL 2016_1405r3 in P1 
CELL 0.71073   6.7898   6.9745   7.2523 108.917  99.404 113.677 
ZERR    1.00   0.0003   0.0003   0.0004   0.004   0.004   0.004 
LATT -1 
SFAC C  H  O  S  Cl Nb 
UNIT 4 10 1 2 3 1 
OMIT  0  -1   3 
OMIT   0   1   4 
OMIT  0   1  -3 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
CONF 
SIZE 0.02 0.02 0.02 
TEMP -173 
WGHT    0.045900 
FVAR       0.66795 
MOLE 1 
NB1   6    0.473259    0.875911    0.743296    11.00000    0.01569    0.01579 = 
         0.01358    0.00615    0.00353    0.00765 
CL1   5    0.295182    0.495003    0.472445    11.00000    0.02438    0.01856 = 
         0.01592    0.00636    0.00654    0.01214 
CL2   5    0.287253    1.004685    0.552098    11.00000    0.02548    0.01968 = 
         0.01797    0.00736    0.00363    0.01311 
CL3   5    0.575504    1.171989    1.074938    11.00000    0.02498    0.01772 = 
         0.01550    0.00343    0.00115    0.00967 
S1    4    0.534875    0.633094    0.942845    11.00000    0.01640    0.02051 = 
         0.01537    0.00854    0.00476    0.01103 
S2    4    0.066371    0.715988    0.845501    11.00000    0.01530    0.01844 = 
         0.01679    0.00586    0.00436    0.00899 
O1    3    0.741026    0.974108    0.722851    11.00000    0.01774    0.02642 = 
         0.01798    0.00818    0.00481    0.01058 
C1    1    0.691651    0.813907    1.215647    11.00000    0.02100    0.02918 = 
         0.01666    0.00820   -0.00196    0.01131 
AFIX 137 
H1A   2    0.615113    0.898920    1.274657    11.00000   -1.50000 
H1B   2    0.847423    0.924441    1.234689    11.00000   -1.50000 
H1C   2    0.697595    0.716596    1.285812    11.00000   -1.50000 
AFIX   0 
C2    1    0.253359    0.453701    0.941736    11.00000    0.01762    0.01717 = 
         0.01740    0.00932    0.00493    0.00771 
AFIX  23 
H2A   2    0.160877    0.328705    0.799911    11.00000   -1.20000 
H2B   2    0.269423    0.379341    1.034413    11.00000   -1.20000 
AFIX   0 
C3    1    0.124776    0.583180    1.009775    11.00000    0.02060    0.02272 = 
         0.01901    0.01005    0.00979    0.01104 
AFIX  23 
H3A   2    0.215204    0.705671    1.152941    11.00000   -1.20000 
H3B   2   -0.022057    0.473641    1.012115    11.00000   -1.20000 
AFIX   0 
C4    1   -0.158202    0.468121    0.617259    11.00000    0.01500    0.02561 = 
         0.01850    0.00158   -0.00074    0.00702 
AFIX 137 
H4A   2   -0.107521    0.354235    0.564808    11.00000   -1.50000 
H4B   2   -0.194187    0.518002    0.510573    11.00000   -1.50000 
H4C   2   -0.294859    0.397510    0.652439    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_1405r3 in P1 
REM R1 =  0.0252 for    2156 Fo > 4sig(Fo)  and  0.0266 for all    2205 data 
REM    102 parameters refined using      3 restraints 
  
END 
  
WGHT      0.0459      0.0000 
  
REM Highest difference peak  0.695,  deepest hole -0.331,  1-sigma level  0.093 
Q1    1   0.3433  0.8140  0.7826  11.00000  0.05    0.69 
Q2    1   0.6117  0.9277  0.7066  11.00000  0.05    0.59 
Q3    1   0.5897  0.9973  0.8531  11.00000  0.05    0.48 
Q4    1   0.2005  0.7777  0.8138  11.00000  0.05    0.44 
Q5    1   0.3960  0.7633  0.6047  11.00000  0.05    0.42 
;
_shelx_res_checksum              1063

_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
