Synthesis and characterisation of monocyclopentadienyl dithiolato complexes of niobium and tantalum; crystal structures of [Nb2(μ-O)(μ-η2∶η2-S2C2H4)(η5-C5H4Me)2Cl4] and [Nb2(μ-η1∶η2-S2C2H4)2(η5-C5H4Me)2O(S2C2H4)] †
Lindsell, W. Edward; Rosair, Georgina M.; Spence, Malcolm A.; Journal of the Chemical Society, Dalton Transactions  (1998) 3281–; doi:10.1039/a804808h

data_7028146
_publ_section_title
;
 Synthesis and characterisation of monocyclopentadienyl dithiolato
 complexes of niobium and tantalum; crystal structures of
 [Nb2(\m-O)(\m-\h2&#x2236;\h2-S2C2H4)(\h5-C5H4Me)2Cl4] and
 [Nb2(\m-\h1&#x2236;\h2-S2C2H4)2(\h5-C5H4Me)2O(S2C2H4)]&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3281
_journal_paper_doi               10.1039/a804808h
_journal_year                    1998
_chemical_formula_sum            'C7 H9 Cl2 Nb O0.5 S'
_chemical_formula_weight         297.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.489(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.7436(15)
_cell_length_b                   9.4404(13)
_cell_length_c                   18.031(2)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      5.06
_cell_volume                     1916.8(4)
_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      160(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2195
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.36
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_obs          0.0293
_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^)+(0.0424P)^2^+1.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0841
_refine_ls_wR_factor_obs         0.0785
_reflns_number_observed          1495
_reflns_number_total             1668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            h804808sup1.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.0790P] 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^)+(0.0424P)^2^+1.0790P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C7 H9 Cl2 Nb O0.50 S'
_cod_database_code               7028146