Preparation, Properties, and Reactivities of Unprecedented Oxo-Sulfido Nb(IV) Aqua Ions and Crystal Structure of (Me2NH2)6[Nb5(μ3-S)2(μ3-O)2(μ2-O)2(NCS)14]·3.5H2O
Ooi, Bee-Lean; Søtofte, Inger; Sokolov, Maxim N.; Kozlova, Svetlana G.; Rasmussen, Søren B.; Nielsen, Loa C.; Henriksen, Jonas; Inorganic Chemistry 45 (2006) 5008–5017; doi:10.1021/ic052145i

data_4332079
_publ_section_title
;
 Preparation, Properties, and Reactivities of Unprecedented Oxo-Sulfido
 Nb(IV) Aqua Ions and Crystal Structure of
 (Me2NH2)6[Nb5(\m3-S)2(\m3-O)2(\m2-O)2(NCS)14]&#x00B7;3.5H2O
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5008
_journal_page_last               5017
_journal_paper_doi               10.1021/ic052145i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C26 H55 N20 Nb5 O7.5 S16'
_chemical_formula_weight         1745.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 103.4590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4018(5)
_cell_length_b                   21.1932(8)
_cell_length_c                   22.0487(8)
_cell_measurement_temperature    120(2)
_cell_volume                     6999.3(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49468
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  no
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8494
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.883
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         16660
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+23.2989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                11434
_reflns_number_total             16660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052145isup1.cif
_cod_data_source_block           nb5k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C26 H55 N20 Nb5 O7.50 S16'
_cod_database_code               4332079