#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/63/2006387.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006387
loop_
_publ_author_name
'Myungok Yoon'
'Victor Young Jr'
'Gordon J. Miller'
.
_publ_contact_author
;
Professor Gordon J. Miller
Department of Chemistry
Iowa State University
Ames
IA 50010
USA
;
_publ_section_title
;
 A Bioctahedral NbIV Cluster with Bridging Sulfides:
 [Nb₂(μ-S)₂Cl₄(thf)₄]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1041
_journal_page_last               1043
_journal_paper_doi               10.1107/S0108270197004277
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Nb2 Cl4 S2 (C4 H8 O)4]'
_chemical_formula_sum            'C16 H32 Cl4 Nb2 O4 S2'
_chemical_formula_weight         680.16
_chemical_name_systematic
;
Tetrachlorotetrakis(tetrahydrofuran)di-μ-thioxodiniobium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5400(10)
_cell_length_b                   15.605(2)
_cell_length_c                   10.4450(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      10.3
_cell_volume                     2605.3(5)
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6000
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        12
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type
'empirical via \y scans (XPREP in SHELXTL-Plus; Sheldrick, 1990)'
_exptl_crystal_colour            brown--green
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    'H atoms riding with C-H = 0.96 \%A'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          .0416
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0457P)²+3.8139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1112
_refine_ls_wR_factor_obs         .0972
_reflns_number_observed          3226
_reflns_number_total             4572
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            fr1039.cif
_cod_data_source_block           str495
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0457P)^2^+3.8139P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0457P)^2^+3.8139P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2605.3(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2006387
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Nb1 .48190(3) .44236(3) .09594(5) .0392(2) Uani d . 1 . Nb
S1 .59482(10) .43875(10) .0000(2) .0521(4) Uani d . 1 . S
Cl1 .39665(10) .34110(10) -.0465(2) .0613(4) Uani d . 1 . Cl
Cl2 .55480(10) .50786(10) .29788(14) .0583(4) Uani d . 1 . Cl
O11 .5426(2) .3167(3) .2117(4) .0583(11) Uani d . 1 . O
C11 .6301(5) .3127(5) .2839(8) .084(2) Uani d . 1 . C
H11A .6362(5) .3217(5) .3768(8) .080 Uiso d R 1 . H
H11B .6616(5) .3557(5) .2522(8) .080 Uiso d R 1 . H
C12 .6589(6) .2309(6) .2606(15) .164(6) Uani d . 1 . C
H12A .6793(6) .2012(6) .3431(15) .080 Uiso d R 1 . H
H12B .7037(6) .2350(6) .2178(15) .080 Uiso d R 1 . H
C13 .5914(6) .1826(5) .1805(10) .105(3) Uani d . 1 . C
H13A .5908(6) .1239(5) .2079(10) .080 Uiso d R 1 . H
H13B .5929(6) .1845(5) .0893(10) .080 Uiso d R 1 . H
C14 .5180(5) .2290(4) .1941(9) .091(3) Uani d . 1 . C
H14A .4703(5) .2223(4) .1197(9) .080 Uiso d R 1 . H
H14B .5036(5) .2089(4) .2723(9) .080 Uiso d R 1 . H
O21 .3848(2) .4213(3) .2144(4) .0533(10) Uani d . 1 . O
C21 .2962(4) .4386(6) .1696(7) .087(3) Uani d . 1 . C
H21A .2712(4) .4035(6) .0944(7) .080 Uiso d R 1 . H
H21B .2872(4) .4977(6) .1442(7) .080 Uiso d R 1 . H
C22 .2615(5) .4208(8) .2795(9) .153(6) Uani d . 1 . C
H22A .2150(5) .3825(8) .2506(9) .080 Uiso d R 1 . H
H22B .2417(5) .4726(8) .3106(9) .080 Uiso d R 1 . H
C23 .3206(4) .3830(6) .3804(7) .087(3) Uani d . 1 . C
H23A .3057(4) .3246(6) .3917(7) .080 Uiso d R 1 . H
H23B .3241(4) .4130(6) .4619(7) .080 Uiso d R 1 . H
C24 .3997(5) .3847(6) .3436(7) .098(3) Uani d . 1 . C
H24A .4383(5) .4203(6) .4055(7) .080 Uiso d R 1 . H
H24B .4230(5) .3283(6) .3453(7) .080 Uiso d R 1 . H
Nb1' .98201(3) .54478(3) .10917(5) .0395(2) Uani d . 1 . Nb
S1' 1.10604(9) .54553(10) .04253(15) .0483(4) Uani d . 1 . S
Cl1' 1.02107(10) .43760(10) .27691(14) .0578(4) Uani d . 1 . Cl
Cl2' .93014(10) .67582(10) .0034(2) .0589(4) Uani d . 1 . Cl
O1' 1.0489(3) .6348(3) .2827(4) .0578(11) Uani d . 1 . O
C11' 1.0631(6) .6222(6) .4235(7) .107(3) Uani d . 1 . C
H11C 1.0690(6) .5621(6) .4439(7) .080 Uiso d R 1 . H
H11D 1.0176(6) .6449(6) .4543(7) .080 Uiso d R 1 . H
C12' 1.1401(6) .6696(6) .4819(8) .113(3) Uani d . 1 . C
H12C 1.1878(6) .6334(6) .4868(8) .080 Uiso d R 1 . H
H12D 1.1415(6) .6898(6) .5693(8) .080 Uiso d R 1 . H
C13' 1.1417(6) .7392(6) .3934(9) .107(3) Uani d . 1 . C
H13C 1.1979(6) .7538(6) .3920(9) .080 Uiso d R 1 . H
H13D 1.1162(6) .7886(6) .4216(9) .080 Uiso d R 1 . H
C14' 1.0913(6) .7126(5) .2639(8) .091(3) Uani d . 1 . C
H14C 1.0521(6) .7561(5) .2229(8) .080 Uiso d R 1 . H
H14D 1.1279(6) .7010(5) .2079(8) .080 Uiso d R 1 . H
O21' .8761(3) .5690(3) .2111(4) .0570(11) Uani d . 1 . O
C21' .8462(5) .6503(5) .2453(8) .083(2) Uani d . 1 . C
H21C .8089(5) .6748(5) .1681(8) .080 Uiso d R 1 . H
H21D .8917(5) .6893(5) .2786(8) .080 Uiso d R 1 . H
C22' .7998(5) .6313(6) .3464(8) .091(3) Uani d . 1 . C
H22C .7495(5) .6646(6) .3325(8) .080 Uiso d R 1 . H
H22D .8347(5) .6436(6) .4331(8) .080 Uiso d R 1 . H
C23' .7784(6) .5421(5) .3309(9) .099(3) Uani d . 1 . C
H23C .7189(6) .5343(5) .3050(9) .080 Uiso d R 1 . H
H23D .8001(6) .5139(5) .4143(9) .080 Uiso d R 1 . H
C24' .8182(5) .5045(5) .2324(7) .076(2) Uani d . 1 . C
H24C .8471(5) .4522(5) .2636(7) .080 Uiso d R 1 . H
H24D .7762(5) .4931(5) .1518(7) .080 Uiso d R 1 . H
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O21 Nb1 S1 . 3_665 88.08(11) no
O21 Nb1 S1 . . 167.89(11) no
S1 Nb1 S1 3_665 . 104.02(5) yes
O21 Nb1 Cl1 . . 81.76(11) no
S1 Nb1 Cl1 3_665 . 95.21(6) no
S1 Nb1 Cl1 . . 97.29(6) no
O21 Nb1 Cl2 . . 81.27(11) no
S1 Nb1 Cl2 3_665 . 97.80(6) no
S1 Nb1 Cl2 . . 96.43(6) no
Cl1 Nb1 Cl2 . . 158.20(6) yes
O21 Nb1 O11 . . 82.55(14) yes
S1 Nb1 O11 3_665 . 170.60(11) no
S1 Nb1 O11 . . 85.35(11) no
Cl1 Nb1 O11 . . 82.81(11) no
Cl2 Nb1 O11 . . 81.51(11) no
O21 Nb1 Nb1 . 3_665 140.27(10) no
S1 Nb1 Nb1 3_665 3_665 52.20(4) no
S1 Nb1 Nb1 . 3_665 51.83(4) no
Cl1 Nb1 Nb1 . 3_665 100.19(5) no
Cl2 Nb1 Nb1 . 3_665 101.61(5) no
O11 Nb1 Nb1 . 3_665 137.18(10) no
Nb1 S1 Nb1 3_665 . 75.97(5) yes
C14 O11 C11 . . 103.8(5) no
C14 O11 Nb1 . . 130.9(4) no
C11 O11 Nb1 . . 122.2(4) no
C12 C11 O11 . . 106.7(7) no
C11 C12 C13 . . 109.4(7) no
C12 C13 C14 . . 103.1(7) no
O11 C14 C13 . . 105.8(6) no
C24 O21 C21 . . 107.1(5) no
C24 O21 Nb1 . . 126.5(4) no
C21 O21 Nb1 . . 126.3(4) no
C22 C21 O21 . . 106.5(6) no
C23 C22 C21 . . 110.2(7) no
C22 C23 C24 . . 107.5(6) no
O21 C24 C23 . . 108.0(6) no
O21' Nb1' S1' . . 165.97(11) no
O21' Nb1' S1' . 3_765 89.83(11) no
S1' Nb1' S1' . 3_765 104.14(5) yes
O21' Nb1' O1' . . 78.88(15) yes
S1' Nb1' O1' . . 87.20(11) no
S1' Nb1' O1' 3_765 . 168.58(11) no
O21' Nb1' Cl2' . . 81.22(11) no
S1' Nb1' Cl2' . . 95.57(6) no
S1' Nb1' Cl2' 3_765 . 96.68(6) no
O1' Nb1' Cl2' . . 83.42(11) no
O21' Nb1' Cl1' . . 82.53(11) no
S1' Nb1' Cl1' . . 97.46(6) no
S1' Nb1' Cl1' 3_765 . 94.54(6) no
O1' Nb1' Cl1' . . 82.38(11) no
Cl2' Nb1' Cl1' . . 160.19(6) yes
O21' Nb1' Nb1' . 3_765 141.86(11) no
S1' Nb1' Nb1' . 3_765 52.08(4) no
S1' Nb1' Nb1' 3_765 3_765 52.05(4) no
O1' Nb1' Nb1' . 3_765 139.25(11) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nb1 O21 . 2.289(4) yes
Nb1 S1 3_665 2.324(2) yes
Nb1 S1 . 2.336(2) yes
Nb1 Cl1 . 2.370(2) yes
Nb1 Cl2 . 2.3747(15) yes
Nb1 O11 . 2.385(4) yes
Nb1 Nb1 3_665 2.8685(10) yes
S1 Nb1 3_665 2.324(2) no
O11 C14 . 1.426(7) no
O11 C11 . 1.451(7) no
C11 C12 . 1.405(11) no
C12 C13 . 1.426(12) no
C13 C14 . 1.452(10) no
O21 C24 . 1.428(7) no
O21 C21 . 1.446(7) no
C21 C22 . 1.435(10) no
C22 C23 . 1.372(10) no
C23 C24 . 1.455(9) no
Nb1' O21' . 2.303(4) yes
Nb1' S1' . 2.330(2) yes
Nb1' S1' 3_765 2.331(2) yes
Nb1' O1' . 2.335(4) yes
Nb1' Cl2' . 2.377(2) yes
Nb1' Cl1' . 2.3879(15) yes
Nb1' Nb1' 3_765 2.8647(10) yes
S1' Nb1' 3_765 2.330(2) no
O1' C14' . 1.440(8) no
O1' C11' . 1.442(8) no
C11' C12' . 1.464(11) no
C12' C13' . 1.431(11) no
C13' C14' . 1.456(10) no
O21' C21' . 1.440(8) no
O21' C24' . 1.445(7) no
C21' C22' . 1.486(9) no
C22' C23' . 1.434(11) no
C23' C24' . 1.478(9) no
