Synthesis, structure and redox properties of bis(cyclopentadienyl)dithiolene complexes of molybdenum and tungsten.
Whalley, Alexandra L.; Blake, Alexander J.; Collison, David; Davies, E. Stephen; Disley, Helen J.; Helliwell, Madeleine; Mabbs, Frank E.; McMaster, Jonathan; Wilson, Claire; Garner, C. David; Dalton transactions (Cambridge, England : 2003) 40 (2011) 10457–10472; doi:10.1039/c1dt10663e

data_7016738
_publ_section_title
;
 Synthesis, structure and redox properties of
 bis(cyclopentadienyl)dithiolene complexes of molybdenum and tungsten.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10457
_journal_page_last               10472
_journal_paper_doi               10.1039/c1dt10663e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C18 H16 Mo S2 +, B F4 -'
_chemical_formula_sum            'C18 H16 B F4 Mo S2'
_chemical_formula_weight         479.20
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.2730(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7275(5)
_cell_length_b                   14.586(1)
_cell_length_c                   18.307(10)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.25
_cell_volume                     1777.7(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL(Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_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  0.101
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15612
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker 1999'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Sphenoid
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.94
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.081P)^2^+1.457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.129
_refine_ls_wR_factor_ref         0.138
_reflns_number_gt                3265
_reflns_number_total             4343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10663e.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1777.7(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7016738