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_4321664
_publ_section_title
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 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
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_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         'C10 H17 Cl4 Mo O'
_chemical_formula_sum            'C10 H17 Cl4 Mo O'
_chemical_formula_weight         390.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   13.9735(10)
_cell_length_b                   11.9079(4)
_cell_length_c                   8.4183(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      9.9
_cell_volume                     1400.76(14)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 Diffractometer'
_diffrn_measurement_method       'omega/2theta scans'
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2653
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.5562
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1251
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      0.994
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_obs          0.0334
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0837
_refine_ls_wR_factor_obs         0.0788
_reflns_number_observed          1135
_reflns_number_total             1251
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000591u_1.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] 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^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321664