Halogenation and Alkylation at a MoIII2(μ-S) Site. Crystal Structure of the Metal-Sulfenyl Halide Complex [Mo2(η5-C5Me5)2(μ-SMe)2(μ-SI)(CO)2]I5
P. Schollhammer; F. Y. Pétillon; J. Talarmin; K. W. Muir; H. K. Fun; K. Chinnakali; Inorganic Chemistry 39 (2000) 5879–5882; doi:10.1021/ic000591u

data_4321665
_publ_section_title
;
 Halogenation and Alkylation at a MoIII2(\m-S) Site. Crystal Structure of
 the Metal-Sulfenyl Halide Complex
 [Mo2(\h5-C5Me5)2(\m-SMe)2(\m-SI)(CO)2]I5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5879
_journal_page_last               5882
_journal_paper_doi               10.1021/ic000591u
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'synthesis by authors'
_chemical_formula_moiety         'C24 H36 I6 Mo2 O2 S3'
_chemical_formula_sum            'C24 H36 I6 Mo2 O2 S3'
_chemical_formula_weight         1405.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7079(3)
_cell_length_b                   14.4213(2)
_cell_length_c                   14.5978(2)
_cell_measurement_reflns_used    6844
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3727.85(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART CCD diffractometer'
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28463
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    5.831
_exptl_absorpt_correction_T_max  0.7298
_exptl_absorpt_correction_T_min  0.5063
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.641
_refine_diff_density_min         -2.995
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+29.4195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1378
_refine_ls_wR_factor_obs         0.1141
_reflns_number_observed          3405
_reflns_number_total             4805
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000591u_2.cif
_cod_data_source_block           kwm1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+29.4195P] 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^)+(0.0498P)^2^+29.4195P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321665