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_4071767
_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
;
        C48 H51 Mo2 N4 S2 1+, Br 1-, 2(C H2 Cl2)
;
_chemical_formula_sum            'C50 H55 Br Cl4 Mo2 N4 S2'
_chemical_formula_weight         1189.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2008-03-25T13:58:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.814(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2743(6)
_cell_length_b                   18.2217(6)
_cell_length_c                   19.7904(8)
_cell_measurement_reflns_used    18695
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      1.87
_cell_volume                     5244.0(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)''PARST (Nardel'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)''SIR-92 (Al'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR2'
_diffrn_measurement_method
;
        1 stepped phi-scan over 360 deg with kappa 0
4 stepped omega-scans over 115 deg, with kappa -79 deg (chi -58.3 deg),
        phi 0, 90, 180, 270 deg
        step 0.75 deg, exposure time 15 s
        detector distance 45 mm
        detector angle 30 deg
;
_diffrn_orient_matrix_UB_11      0.011929548
_diffrn_orient_matrix_UB_12      -0.0135247745
_diffrn_orient_matrix_UB_13      -0.0295923167
_diffrn_orient_matrix_UB_21      0.0253004636
_diffrn_orient_matrix_UB_22      0.0324849877
_diffrn_orient_matrix_UB_23      -0.0004887049
_diffrn_orient_matrix_UB_31      0.0398676387
_diffrn_orient_matrix_UB_32      -0.0165645097
_diffrn_orient_matrix_UB_33      0.0231933042
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.039
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            100367
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.70511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.856
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         15988
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+6.9583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                10873
_reflns_number_total             15988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8003702-file004.cif
_cod_data_source_block           xylcarbb
_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_cell_volume        5244.0(3)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4071767