Rearrangement of Molybdocene Tetraoxotetrasulfide Cp2MoS4O4to Give [(Cp2MoS2H)2](HSO4)2: A Novel Proton-Stabilized Molybdocene Disulfide Dimer
Rys, Andrzej Z.; Lebuis, Anne-Marie; Shaver, Alan; Inorganic Chemistry 45 (2006) 341–344; doi:10.1021/ic051332d

data_4331664
_publ_section_title
;
 Rearrangement of Molybdocene Tetraoxotetrasulfide Cp2MoS4O4to Give
 [(Cp2MoS2H)2](HSO4)2:&#x00A0; A Novel Proton-Stabilized Molybdocene
 Disulfide Dimer
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              341
_journal_page_last               344
_journal_paper_doi               10.1021/ic051332d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C20 H28 Mo2 O10 S6'
_chemical_formula_sum            'C20 H28 Mo2 O10 S6'
_chemical_formula_weight         812.68
_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-97
_cell_angle_alpha                109.95(3)
_cell_angle_beta                 96.11(3)
_cell_angle_gamma                108.22(3)
_cell_formula_units_Z            1
_cell_length_a                   6.751(2)
_cell_length_b                   9.865(4)
_cell_length_c                   11.549(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     666.9(5)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRC-2, NRC-2A (Ahmed et al, 1973)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'ENRAF-NONIUS CAD-4'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Cu k\a'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21647
_diffrn_reflns_theta_full        69.81
_diffrn_reflns_theta_max         69.81
_diffrn_reflns_theta_min         4.19
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    12.689
_exptl_absorpt_correction_T_max  0.3384
_exptl_absorpt_correction_T_min  0.0929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.685
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                2263
_reflns_number_total             2529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051332dsup1.cif
_cod_data_source_block           harp67
_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.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' 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 
;
_cod_original_cell_volume        666.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331664