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_4322992
_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_sum            'C24 H64 Cl26 Nb6 O2 S8'
_chemical_formula_weight         2120.39
_chemical_name_systematic
;
 ?
;
_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'
_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                 110.8830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.658(2)
_cell_length_b                   14.3090(10)
_cell_length_c                   19.8430(10)
_cell_measurement_reflns_used    5807
_cell_measurement_temperature    295(2)
_cell_volume                     7337.2(8)
_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/CCD'
_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  0.058
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39346
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         0.79
_diffrn_standards_interval_time  '6 hours'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.320
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       plates
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.000078(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.882
_refine_ls_goodness_of_fit_obs   1.023
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         15083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_restrained_S_obs      1.023
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_obs          0.0404
_refine_ls_shift/esd_max         0.530
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0784
_refine_ls_wR_factor_obs         0.0654
_reflns_number_observed          8135
_reflns_number_total             15086
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980150z_2.cif
_cod_data_source_block           nibb(4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] 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^)+(0.0270P)^2^+0.0000P] 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               4322992