Synthesis of a Homoleptic Niobium(V) Thiolate Complex and the Preparation of Niobium Sulfide via Thio "Sol-Gel" and Vapor Phase Thin-Film Experiments
Claire J. Carmalt; Christopher W. Dinnage; Ivan P. Parkin; Andrew J. P. White; David J. Williams; Inorganic Chemistry 41 (2002) 3668–3672; doi:10.1021/ic020097l

data_4318207
_publ_section_title
;
 Synthesis of a Homoleptic Niobium(V) Thiolate Complex and the Preparation
 of Niobium Sulfide via Thio "Sol-Gel" and Vapor Phase Thin-Film
 Experiments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3668
_journal_page_last               3672
_journal_paper_doi               10.1021/ic020097l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H45 Nb S5'
_chemical_formula_weight         778.97
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                81.733(4)
_cell_angle_beta                 82.984(4)
_cell_angle_gamma                61.955(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6085(4)
_cell_length_b                   10.7974(4)
_cell_length_c                   19.0869(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      10.84
_cell_volume                     1905.80(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5998
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.329
_exptl_absorpt_correction_T_max  0.6686
_exptl_absorpt_correction_T_min  0.1999
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Very dark red'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00068(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   1.050
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_obs          0.0368
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0965
_refine_ls_wR_factor_obs         0.0905
_reflns_number_observed          5206
_reflns_number_total             5644
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020097l.cif
_cod_data_source_block           CC0102
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.7840P] 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^)+(0.0516P)^2^+1.7840P] 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        1905.80(15)
_cod_original_formula_sum        'C40 H45 S5 Nb'
_cod_database_code               4318207