C−C, C−S, and C−N Coupling versus Dealkylation Processes in the Cationic Tris(thiolato)dimolybdenum(III) Complexes [Mo2Cp2(μ-SMe)3L2]+(L = xylNC,t-BuNC, CO, MeCN)
Ojo, Wilfried-Solo; Pétillon, François Y.; Schollhammer, P.; Talarmin, Jean; Organometallics 27 (2008) 4207–; doi:10.1021/om8003702

data_4071768
_publ_section_title
;
 C&#x2212;C, C&#x2212;S, and C&#x2212;N Coupling versus Dealkylation
 Processes in the Cationic Tris(thiolato)dimolybdenum(III) Complexes
 [Mo2Cp2(\m-SMe)3L2]+(L = xylNC,t-BuNC, CO, MeCN)
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4207
_journal_paper_doi               10.1021/om8003702
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety
;
       2(C48 H52 Mo2 N4 S2), 4(B C24 H20), C4 H10 O
;
_chemical_formula_sum            'C196 H194 B4 Mo4 N8 O S4'
_chemical_formula_weight         3232.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-03-10T15:12:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.078(2)
_cell_angle_beta                 95.249(3)
_cell_angle_gamma                93.064(3)
_cell_formula_units_Z            1
_cell_length_a                   15.6411(6)
_cell_length_b                   15.8771(4)
_cell_length_c                   17.5708(5)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.9173
_cell_measurement_theta_min      2.5594
_cell_volume                     4331.4(2)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR2'
_diffrn_measurement_method
;
        stepped phi-scan over 360 deg
        step 1 deg, exposure time 90 s
        detector distance 45 mm
        detector angle 20 deg.
;
_diffrn_orient_matrix_UB_11      -0.0250372365
_diffrn_orient_matrix_UB_12      -0.0188681041
_diffrn_orient_matrix_UB_13      0.026903917
_diffrn_orient_matrix_UB_21      0.035428179
_diffrn_orient_matrix_UB_22      -0.0232298247
_diffrn_orient_matrix_UB_23      0.0130140104
_diffrn_orient_matrix_UB_31      0.0141063401
_diffrn_orient_matrix_UB_32      0.0333596439
_diffrn_orient_matrix_UB_33      0.027493288
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24348
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate // (0 1 0)'
_exptl_crystal_F_000             1686
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                7516
_reflns_number_total             11345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8003702-file005.cif
_cod_data_source_block           bisxyl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4071768