An Unprecedented Tetranuclear Niobium Aqua Ion with a Capping μ4-Sulfido Ligand
Bee-Lean Ooi; Inger Søtofte; Maja F. Bendtsen; Astrid Munch; Loa C. Nielsen; Jonas Henriksen; Inorganic Chemistry 44 (2005) 480–482; doi:10.1021/ic048659j

data_4308523
_publ_contact_author_name        'Bee-Lean Ooi'
_publ_section_title
;
An Unprecedented Tetranuclear Niobium Aqua Ion with a Capping \m4-Sulfido
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              480
_journal_page_last               482
_journal_paper_doi               10.1021/ic048659j
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         Cs4.26,Na1.74,Nb4SO5(NCS)10,0.33H2O
_chemical_formula_sum            'C10 H0.67 Cs4.26 N10 Na1.74 Nb4 O5.33 S11'
_chemical_formula_weight         1676.70
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.8033(6)
_cell_length_b                   20.8033(6)
_cell_length_c                   18.1398(8)
_cell_measurement_temperature    120(2)
_cell_volume                     6798.7(4)
_computing_cell_refinement       'SAINT (Bruker AXS,1998)'
_computing_data_collection       'SMART (Bruker AXS,1998)'
_computing_data_reduction        'SAINT (Bruker AXS,1998)'
_computing_molecular_graphics    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_refinement  'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_solution    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART CCD Platform'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48479
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  no
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    4.917
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             4601
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.295
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+70.4794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                4411
_reflns_number_total             5657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048659jsi20041217_044017.cif
_cod_data_source_block           nbR
_cod_database_code               4308523