Synthesis, Structure, Hydrolysis, and Film Deposition Studies of Complexes of the Formula [NbCl4(S2R2)2][NbCl6]
Peggy J. McKarns; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 37 (1998) 4743–4747; doi:10.1021/ic980150z

data_4322991
_publ_section_title
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 Synthesis, Structure, Hydrolysis, and Film Deposition Studies of
 Complexes of the Formula [NbCl4(S2R2)2][NbCl6]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4743
_journal_page_last               4747
_journal_paper_doi               10.1021/ic980150z
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '[Nb(Cl)4(S2(CH3)2)2]+[Nb(Cl)6]-'
_chemical_formula_sum            'C4 H12 Cl10 Nb2 S4'
_chemical_formula_weight         728.70
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8960(10)
_cell_length_b                   12.4030(10)
_cell_length_c                   15.2580(10)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    295(2)
_cell_volume                     2212.8(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  Shelxl-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens P4/CD'
_diffrn_measurement_method       'SMART CCD'
_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  0.09
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12125
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_time  '6 hours'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.607
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       'Cut fragment'
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL-93
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.198
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.198
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         -0.120
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1387
_refine_ls_wR_factor_obs         0.1190
_reflns_number_observed          2748
_reflns_number_total             4735
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980150z_1.cif
_cod_data_source_block           neco(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.8441P] 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^)+(0.0602P)^2^+1.8441P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322991