Six- and eight-coordinate thio- and seleno-ether complexes of NbF5 and some comparisons with NbCl5 and NbBr5 adducts.
Jura, Marek; Levason, William; Ratnani, Raju; Reid, Gillian; Webster, Michael; Dalton transactions (Cambridge, England : 2003) 39 (2010) 883–891; doi:10.1039/b916336k

data_7024382
_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 \k-goniostat'
_diffrn_measurement_method       '\f & \w 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/[\s^2^(Fo^2^)+(0.0312P)^2^+5.7487P] where P=(Fo^2^+2Fc^2^)/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