#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024382.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_7024382
loop_
_publ_author_name
'Jura, Marek'
'Levason, William'
'Ratnani, Raju'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Six- and eight-coordinate thio- and seleno-ether complexes of NbF5 and
 some comparisons with NbCl5 and NbBr5 adducts.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              883
_journal_page_last               891
_journal_paper_doi               10.1039/b916336k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C16 H36 F4 Nb S4 1+, F6 Nb1 1-'
_chemical_formula_structural     '((C8 H18 S2)2 (F4 Nb)) (F6 Nb)'
_chemical_formula_sum            'C16 H36 F10 Nb2 S4'
_chemical_formula_weight         732.51
_chemical_name_common
;Tetrafluorobis(1,2-bis(isopropylthio)ethane-S,S')niobium(V)
hexafluoroniobate(V)
;
_chemical_name_systematic
;
Tetrafluorobis(1,2-bis(isopropylthio)ethane-S,S')niobium(V)
hexafluoroniobate(V)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-02-17
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                115.206(7)
_cell_angle_beta                 90.596(10)
_cell_angle_gamma                110.136(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2850(10)
_cell_length_b                   11.6895(15)
_cell_length_c                   13.5404(15)
_cell_measurement_reflns_used    49250
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1359.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27957
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0470
_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)+(0.0312P)²+5.7487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                5146
_reflns_number_total             6180
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b916336k.txt
_cod_data_source_block           09mj07
_cod_database_code               7024382
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb1 Nb 0.86971(4) 0.59002(4) 0.31573(3) 0.01678(10) Uani 1 1 d .
Nb2 Nb 0.0000 0.0000 0.0000 0.03102(16) Uani 1 2 d S
Nb3 Nb 0.5000 1.0000 0.5000 0.02636(14) Uani 1 2 d S
F1 F 1.0161(2) 0.5263(2) 0.3191(2) 0.0210(5) Uani 1 1 d .
F2 F 0.6769(2) 0.5555(2) 0.3273(2) 0.0199(5) Uani 1 1 d .
F3 F 0.8251(2) 0.5265(2) 0.16043(19) 0.0205(5) Uani 1 1 d .
F4 F 0.9589(3) 0.7489(2) 0.45523(19) 0.0219(5) Uani 1 1 d .
F5 F -0.0811(4) -0.1684(3) 0.0049(3) 0.0495(8) Uani 1 1 d .
F6 F 0.1802(4) -0.0018(4) 0.0188(4) 0.0662(11) Uani 1 1 d .
F7 F 0.0168(4) 0.0932(4) 0.1556(3) 0.0594(10) Uani 1 1 d .
F8 F 0.4501(3) 0.8253(3) 0.3785(3) 0.0441(8) Uani 1 1 d .
F9 F 0.4029(4) 1.0498(4) 0.4164(3) 0.0550(9) Uani 1 1 d .
F10 F 0.6651(4) 1.0651(3) 0.4484(3) 0.0486(8) Uani 1 1 d .
S1 S 0.84225(10) 0.52194(10) 0.48698(8) 0.0189(2) Uani 1 1 d .
S2 S 0.75756(11) 0.30985(11) 0.21831(9) 0.0209(2) Uani 1 1 d .
S3 S 0.81235(11) 0.80072(11) 0.31967(9) 0.0212(2) Uani 1 1 d .
S4 S 1.10712(11) 0.74737(11) 0.27437(9) 0.0232(2) Uani 1 1 d .
C1 C 0.6779(5) 0.5189(6) 0.6453(4) 0.0325(11) Uani 1 1 d .
H1A H 0.7636 0.5733 0.7024 0.049 Uiso 1 1 calc R
H1B H 0.6608 0.4214 0.6151 0.049 Uiso 1 1 calc R
H1C H 0.5976 0.5353 0.6782 0.049 Uiso 1 1 calc R
C2 C 0.7270(5) 0.7120(5) 0.5943(4) 0.0278(10) Uani 1 1 d .
H2A H 0.6478 0.7322 0.6264 0.042 Uiso 1 1 calc R
H2B H 0.7404 0.7350 0.5326 0.042 Uiso 1 1 calc R
H2C H 0.8128 0.7664 0.6513 0.042 Uiso 1 1 calc R
C3 C 0.6960(4) 0.5605(5) 0.5521(4) 0.0222(9) Uani 1 1 d .
H3 H 0.6074 0.5059 0.4950 0.027 Uiso 1 1 calc R
C4 C 0.7743(5) 0.3367(4) 0.4328(4) 0.0233(9) Uani 1 1 d .
H4A H 0.8118 0.3135 0.4862 0.028 Uiso 1 1 calc R
H4B H 0.6703 0.3006 0.4239 0.028 Uiso 1 1 calc R
C5 C 0.8159(5) 0.2702(4) 0.3217(4) 0.0234(9) Uani 1 1 d .
H5A H 0.7757 0.1696 0.2938 0.028 Uiso 1 1 calc R
H5B H 0.9198 0.3007 0.3326 0.028 Uiso 1 1 calc R
C6 C 0.5658(4) 0.2481(4) 0.2078(4) 0.0226(9) Uani 1 1 d .
H6 H 0.5423 0.3076 0.2778 0.027 Uiso 1 1 calc R
C7 C 0.5063(5) 0.2604(5) 0.1111(4) 0.0290(10) Uani 1 1 d .
H7A H 0.5286 0.2017 0.0422 0.043 Uiso 1 1 calc R
H7B H 0.5482 0.3558 0.1241 0.043 Uiso 1 1 calc R
H7C H 0.4039 0.2317 0.1045 0.043 Uiso 1 1 calc R
C8 C 0.5050(5) 0.1001(5) 0.1896(4) 0.0315(10) Uani 1 1 d .
H8A H 0.4019 0.0643 0.1716 0.047 Uiso 1 1 calc R
H8B H 0.5336 0.0970 0.2574 0.047 Uiso 1 1 calc R
H8C H 0.5404 0.0441 0.1281 0.047 Uiso 1 1 calc R
C9 C 0.7095(6) 0.8841(5) 0.1854(4) 0.0353(11) Uani 1 1 d .
H9A H 0.6624 0.8613 0.1123 0.053 Uiso 1 1 calc R
H9B H 0.8034 0.9562 0.2042 0.053 Uiso 1 1 calc R
H9C H 0.6538 0.9166 0.2414 0.053 Uiso 1 1 calc R
C10 C 0.5779(5) 0.6446(5) 0.1577(4) 0.0334(11) Uani 1 1 d .
H10A H 0.5270 0.6758 0.2180 0.050 Uiso 1 1 calc R
H10B H 0.5885 0.5617 0.1514 0.050 Uiso 1 1 calc R
H10C H 0.5250 0.6243 0.0877 0.050 Uiso 1 1 calc R
C11 C 0.7231(5) 0.7565(5) 0.1827(4) 0.0256(9) Uani 1 1 d .
H11 H 0.7787 0.7222 0.1249 0.031 Uiso 1 1 calc R
C12 C 0.9827(5) 0.9321(5) 0.3397(4) 0.0312(10) Uani 1 1 d .
H12A H 0.9682 1.0084 0.3334 0.037 Uiso 1 1 calc R
H12B H 1.0340 0.9688 0.4158 0.037 Uiso 1 1 calc R
C13 C 1.0713(5) 0.8813(5) 0.2578(4) 0.0308(10) Uani 1 1 d .
H13A H 1.1611 0.9578 0.2704 0.037 Uiso 1 1 calc R
H13B H 1.0211 0.8442 0.1813 0.037 Uiso 1 1 calc R
C14 C 1.1306(5) 0.6510(5) 0.1323(4) 0.0265(9) Uani 1 1 d .
H14 H 1.0415 0.6156 0.0793 0.032 Uiso 1 1 calc R
C15 C 1.2496(6) 0.7460(5) 0.1038(4) 0.0344(11) Uani 1 1 d .
H15A H 1.3356 0.7861 0.1588 0.052 Uiso 1 1 calc R
H15B H 1.2235 0.8192 0.1042 0.052 Uiso 1 1 calc R
H15C H 1.2665 0.6937 0.0299 0.052 Uiso 1 1 calc R
C16 C 1.1628(5) 0.5310(5) 0.1258(4) 0.0312(10) Uani 1 1 d .
H16A H 1.1853 0.4844 0.0528 0.047 Uiso 1 1 calc R
H16B H 1.0804 0.4667 0.1365 0.047 Uiso 1 1 calc R
H16C H 1.2434 0.5645 0.1839 0.047 Uiso 1 1 calc R
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'
F F 0.0171 0.0103 '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'
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
F3 Nb1 F1 99.35(10) . .
F3 Nb1 F2 90.69(10) . .
F1 Nb1 F2 143.70(10) . .
F3 Nb1 F4 144.48(10) . .
F1 Nb1 F4 91.73(11) . .
F2 Nb1 F4 100.10(11) . .
F3 Nb1 S3 81.26(8) . .
F1 Nb1 S3 144.32(8) . .
F2 Nb1 S3 71.52(8) . .
F4 Nb1 S3 70.57(8) . .
F3 Nb1 S4 77.45(8) . .
F1 Nb1 S4 70.37(8) . .
F2 Nb1 S4 145.87(8) . .
F4 Nb1 S4 74.75(8) . .
S3 Nb1 S4 75.07(4) . .
F3 Nb1 S2 72.74(8) . .
F1 Nb1 S2 70.83(8) . .
F2 Nb1 S2 79.25(8) . .
F4 Nb1 S2 142.39(8) . .
S3 Nb1 S2 140.34(4) . .
S4 Nb1 S2 125.47(4) . .
F3 Nb1 S1 146.30(8) . .
F1 Nb1 S1 75.26(8) . .
F2 Nb1 S1 77.18(8) . .
F4 Nb1 S1 69.18(8) . .
S3 Nb1 S1 122.58(3) . .
S4 Nb1 S1 128.54(3) . .
S2 Nb1 S1 74.14(3) . .
F6 Nb2 F6 180.0(3) . 2
F6 Nb2 F5 89.66(18) . 2
F6 Nb2 F5 90.34(18) 2 2
F6 Nb2 F5 90.34(18) . .
F6 Nb2 F5 89.66(18) 2 .
F5 Nb2 F5 180.0(3) 2 .
F6 Nb2 F7 90.0(2) . 2
F6 Nb2 F7 90.0(2) 2 2
F5 Nb2 F7 89.44(15) 2 2
F5 Nb2 F7 90.56(15) . 2
F6 Nb2 F7 90.0(2) . .
F6 Nb2 F7 90.0(2) 2 .
F5 Nb2 F7 90.56(15) 2 .
F5 Nb2 F7 89.44(15) . .
F7 Nb2 F7 180.0(2) 2 .
F8 Nb3 F8 180.00(17) 2_676 .
F8 Nb3 F10 90.06(15) 2_676 .
F8 Nb3 F10 89.94(15) . .
F8 Nb3 F10 89.94(15) 2_676 2_676
F8 Nb3 F10 90.06(15) . 2_676
F10 Nb3 F10 180.000(1) . 2_676
F8 Nb3 F9 90.20(16) 2_676 2_676
F8 Nb3 F9 89.80(16) . 2_676
F10 Nb3 F9 90.23(18) . 2_676
F10 Nb3 F9 89.77(18) 2_676 2_676
F8 Nb3 F9 89.80(16) 2_676 .
F8 Nb3 F9 90.20(16) . .
F10 Nb3 F9 89.77(18) . .
F10 Nb3 F9 90.23(18) 2_676 .
F9 Nb3 F9 180.000(1) 2_676 .
C4 S1 C3 100.9(2) . .
C4 S1 Nb1 110.17(15) . .
C3 S1 Nb1 108.85(14) . .
C5 S2 C6 103.7(2) . .
C5 S2 Nb1 103.93(15) . .
C6 S2 Nb1 109.63(14) . .
C12 S3 C11 103.9(2) . .
C12 S3 Nb1 105.06(16) . .
C11 S3 Nb1 111.14(15) . .
C13 S4 C14 99.0(2) . .
C13 S4 Nb1 108.40(16) . .
C14 S4 Nb1 109.48(15) . .
C3 C1 H1A 109.5 . .
C3 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C3 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 H2A 109.5 . .
C3 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C3 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C2 C3 C1 112.0(4) . .
C2 C3 S1 109.2(3) . .
C1 C3 S1 108.9(3) . .
C2 C3 H3 108.9 . .
C1 C3 H3 108.9 . .
S1 C3 H3 108.9 . .
C5 C4 S1 110.9(3) . .
C5 C4 H4A 109.5 . .
S1 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
S1 C4 H4B 109.5 . .
H4A C4 H4B 108.0 . .
C4 C5 S2 113.4(3) . .
C4 C5 H5A 108.9 . .
S2 C5 H5A 108.9 . .
C4 C5 H5B 108.9 . .
S2 C5 H5B 108.9 . .
H5A C5 H5B 107.7 . .
C7 C6 C8 111.1(4) . .
C7 C6 S2 107.0(3) . .
C8 C6 S2 111.0(3) . .
C7 C6 H6 109.3 . .
C8 C6 H6 109.3 . .
S2 C6 H6 109.3 . .
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 . .
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 . .
C11 C9 H9A 109.5 . .
C11 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C11 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C10 C11 C9 110.5(4) . .
C10 C11 S3 107.8(3) . .
C9 C11 S3 109.1(3) . .
C10 C11 H11 109.8 . .
C9 C11 H11 109.8 . .
S3 C11 H11 109.8 . .
C13 C12 S3 113.2(3) . .
C13 C12 H12A 108.9 . .
S3 C12 H12A 108.9 . .
C13 C12 H12B 108.9 . .
S3 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
C12 C13 S4 109.3(3) . .
C12 C13 H13A 109.8 . .
S4 C13 H13A 109.8 . .
C12 C13 H13B 109.8 . .
S4 C13 H13B 109.8 . .
H13A C13 H13B 108.3 . .
C15 C14 C16 111.3(4) . .
C15 C14 S4 109.2(3) . .
C16 C14 S4 108.7(3) . .
C15 C14 H14 109.2 . .
C16 C14 H14 109.2 . .
S4 C14 H14 109.2 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 F3 1.897(2) .
Nb1 F1 1.904(2) .
Nb1 F2 1.905(2) .
Nb1 F4 1.913(2) .
Nb1 S3 2.7030(11) .
Nb1 S4 2.7336(12) .
Nb1 S2 2.7357(12) .
Nb1 S1 2.7424(11) .
Nb2 F6 1.877(4) .
Nb2 F6 1.877(4) 2
Nb2 F5 1.886(3) 2
Nb2 F5 1.886(3) .
Nb2 F7 1.888(3) 2
Nb2 F7 1.888(3) .
Nb3 F8 1.881(3) 2_676
Nb3 F8 1.881(3) .
Nb3 F10 1.881(3) .
Nb3 F10 1.881(3) 2_676
Nb3 F9 1.885(3) 2_676
Nb3 F9 1.885(3) .
S1 C4 1.819(4) .
S1 C3 1.843(4) .
S2 C5 1.807(4) .
S2 C6 1.832(4) .
S3 C12 1.812(5) .
S3 C11 1.836(4) .
S4 C13 1.825(5) .
S4 C14 1.838(5) .
C1 C3 1.526(6) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.519(6) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3 1.0000 .
C4 C5 1.515(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.521(6) .
C6 C8 1.527(6) .
C6 H6 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C11 1.531(6) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.524(7) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11 1.0000 .
C12 C13 1.499(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.524(7) .
C14 C16 1.515(7) .
C14 H14 1.0000 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
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
S1 C4 C5 S2 -57.3(4)
S3 C12 C13 S4 -61.9(4)
