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_7028147
_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            'C19 H28 Cl2 Nb2 O S6'
_chemical_formula_weight         721.49
_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                98.609(7)
_cell_angle_beta                 96.039(9)
_cell_angle_gamma                90.532(5)
_cell_formula_units_Z            4
_cell_length_a                   10.2778(7)
_cell_length_b                   11.3022(8)
_cell_length_c                   23.120(2)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.45
_cell_volume                     2639.8(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      293(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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10987
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        9.70
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  0.6700
_exptl_absorpt_correction_T_min  0.4685
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+2.1316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1198
_refine_ls_wR_factor_obs         0.0953
_reflns_number_observed          6563
_reflns_number_total             9279
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            h804808sup1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0463P)^2^+2.1316P] 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^)+(0.0463P)^2^+2.1316P] 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      P-1
_cod_database_code               7028147