Thermal Generation and Structures of the Unsaturated Doubly Bridged Complex [Mo2Cp2Cl2(μ-SMe)2] and Its Quadruply Bridged Isomer [Mo2Cp2(μ-Cl)2(μ-SMe)2]
Ojo, Wilfried-Solo; McGrady, John E.; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Organometallics 30 (2011) 649–; doi:10.1021/om101061y

data_4063957
_publ_section_title
;
 Thermal Generation and Structures of the Unsaturated Doubly Bridged
 Complex [Mo2Cp2Cl2(\m-SMe)2] and Its Quadruply Bridged Isomer
 [Mo2Cp2(\m-Cl)2(\m-SMe)2]
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              649
_journal_paper_doi               10.1021/om101061y
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C12 H16 Cl2 Mo2 S2'
_chemical_formula_sum            'C12 H16 Cl2 Mo2 S2'
_chemical_formula_weight         487.15
_chemical_name_common            Mo2Cp2Cl2(\m-SMe)2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2010-10-26T14:58:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.560(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9955(3)
_cell_length_b                   14.5964(5)
_cell_length_c                   13.7702(4)
_cell_measurement_reflns_used    13809
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      44.797
_cell_measurement_theta_min      2.9535
_cell_volume                     1568.60(9)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method
;
        \w and \p scans:
4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.),
        detector angle 30 deg., phi 0, 90, 180, 270 deg.,
followed by 1 stepped phi-scan over 210 deg., detector angle 60 deg.
        step 0.75 deg., exposure time 40 s, detector distance 50 mm
;
_diffrn_orient_matrix_UB_11      0.0579589068
_diffrn_orient_matrix_UB_12      0.0344992961
_diffrn_orient_matrix_UB_13      0.0227298271
_diffrn_orient_matrix_UB_21      0.0079550769
_diffrn_orient_matrix_UB_22      0.0155059145
_diffrn_orient_matrix_UB_23      -0.0476044205
_diffrn_orient_matrix_UB_31      -0.0695614254
_diffrn_orient_matrix_UB_32      0.0304981082
_diffrn_orient_matrix_UB_33      -0.0015071147
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21301
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
flat short prism, axis [1 0 0],
lateral faces {0 1 1} and {0 0 1},
tip faces (-1 -1 0), (-1 0 1) and (-1 1 0) (other side brocken)
;
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method
'slow evaporation in cold (255 K) toluene solution'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.98
_refine_ls_R_factor_all          0.023
_refine_ls_R_factor_gt           0.0167
_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^)+(0.0223P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0385
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                4082
_reflns_number_total             4785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101061y_si_002.cif
_cod_data_source_block           ad4-1-b
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4063957