A Bioctahedral Nb^IV^ Cluster with Bridging Sulfides: [Nb~2~(μ-S)~2~Cl~4~(thf)~4~]
Myungok Yoon; Victor Young Jr; Gordon J. Miller; .; Acta Crystallographica Section C 53 (1997) 1041–1043; doi:10.1107/S0108270197004277

data_2006387
_publ_contact_author
;
Professor Gordon J. Miller
Department of Chemistry
Iowa State University
Ames
IA 50010
USA
;
_publ_section_title
;
 A Bioctahedral Nb^IV^ Cluster with Bridging Sulfides:
 [Nb~2~(\m-S)~2~Cl~4~(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-\m-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       \w--2\q
_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/[\s^2^(Fo^2^)+(0.0457P)^2^+3.8139P] where P=(Fo^2^+2Fc^2^)/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