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_4318185
_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         'C10 H10 Mo O2 S3'
_chemical_formula_sum            'C10 H10 Mo O2 S3'
_chemical_formula_weight         354.30
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 92.040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6782(6)
_cell_length_b                   14.580(3)
_cell_length_c                   10.2730(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      27.5
_cell_volume                     1149.3(3)
_computing_cell_refinement
'MSC/AFC (Molecular Structure Corporation 1985)'
_computing_data_collection
'MSC/AFC (Molecular Structure Corporation 1985)'
_computing_data_reduction
'NRCVAX-89 DATRD2 (Gabe, LePage Charland, Lee & White 1989)'
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material  'SHELXL96 (Sheldrick (1996))'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.012
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1845
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         5.27
_diffrn_standards_decay_%        0.53
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.278
_exptl_absorpt_correction_T_max  0.996197
_exptl_absorpt_correction_T_min  0.409213
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'ABSN in NRCVAX, (Gabe et al (1989)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'diamond shaped'
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.00223(18)
_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   1.075
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0435P)^2^+5.4751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0952
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                1466
_reflns_number_total             1705
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic011001a_1.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 '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 
;
_cod_database_code               4318185