#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:00:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/20/7702097.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7702097
loop_
_publ_author_name
'Chang, Yao-Pang'
'Levason, William'
'Light, Mark E.'
'Reid, Gillian'
_publ_section_title
;
 Niobium tetrachloride complexes with thio-, seleno- and telluro-ether
 coordination - synthesis and structures.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16262
_journal_page_last               16274
_journal_paper_doi               10.1039/c6dt02979e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C4 H12 Cl8 Nb2 S2'
_chemical_formula_sum            'C4 H12 Cl8 Nb2 S2'
_chemical_formula_weight         593.68
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.499(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4589(2)
_cell_length_b                   10.1598(4)
_cell_length_c                   13.1644(5)
_cell_measurement_reflns_used    3983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9990
_cell_measurement_theta_min      2.4850
_cell_volume                     861.20(5)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5264
_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         25.987
_diffrn_reflns_theta_min         2.535
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68615
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0288P)²+0.9127P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1570
_reflns_number_total             1690
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2016_0505r1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7702097
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.911
_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
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'
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
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)
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'
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
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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 .
