Insertion of SO2 into the S-S Bond of Cp2MoS2 and Cp2MoS2O To Give Molybdocene Dithiosulfate and Bis(O-alkylthiosulfates)
Andrzej Z. Rys; Anne-Marie Lebuis; Alan Shaver; David N. Harpp; Inorganic Chemistry 41 (2002) 3653–3655; doi:10.1021/ic011001a

data_4318186
_publ_section_title
;
 Insertion of SO2 into the S-S Bond of Cp2MoS2 and Cp2MoS2O To Give
 Molybdocene Dithiosulfate and Bis(O-alkylthiosulfates)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3653
_journal_page_last               3655
_journal_paper_doi               10.1021/ic011001a
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C12 H16 Mo O6 S4'
_chemical_formula_sum            'C12 H16 Mo O6 S4'
_chemical_formula_weight         480.43
_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           'SHELXL96 (Sheldrick, 1996)'
_cell_angle_alpha                87.803(11)
_cell_angle_beta                 77.758(11)
_cell_angle_gamma                86.383(12)
_cell_formula_units_Z            2
_cell_length_a                   8.3226(13)
_cell_length_b                   8.4736(11)
_cell_length_c                   12.3821(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      15
_cell_volume                     851.4(2)
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material
'NRCVAX (Gabe et al (1989) and SHELXL96 (Sheldrick (1996))'
_computing_structure_solution    'SHELXS96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           Mo
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6413
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        .5
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7978
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0364(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL96 (Sheldrick, 1996)'
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.2733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0694
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                2566
_reflns_number_total             2991
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic011001a_2.cif
_cod_data_source_block           compound_6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'psi scan' changed to
'psi-scan' 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:

'_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_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4318186