Formation of C−C, C−N, and C−O Links between Isonitrile, Cyclopentadienyl, and Hydroxide Ligands Bound to Molybdenum(III): Syntheses and Crystal Structures of μ-Aminocarbyne and μ-Amino-oxycarbene Dimolybdenum Complexes
Ojo, Wilfried-Solo; Paugam, Eddy; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Muir, Kenneth W.; Organometallics 25 (2006) 4009–; doi:10.1021/om060383v

data_4075585
_publ_section_title
;
 Formation of C&#x2212;C, C&#x2212;N, and C&#x2212;O Links between
 Isonitrile, Cyclopentadienyl, and Hydroxide Ligands Bound to
 Molybdenum(III):&#x00A0; Syntheses and Crystal Structures of
 \m-Aminocarbyne and \m-Amino-oxycarbene Dimolybdenum Complexes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4009
_journal_paper_doi               10.1021/om060383v
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C41 H47 Mo2 N3 O S2'
_chemical_formula_weight         853.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_date             2006-02-09T11:09:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(7)
_cell_angle_beta                 95.627(7)
_cell_angle_gamma                90.000(6)
_cell_formula_units_Z            4
_cell_length_a                   12.9957(10)
_cell_length_b                   18.5383(14)
_cell_length_c                   16.2894(15)
_cell_measurement_reflns_used    '4100 reflns out of 5564'
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.9474
_cell_measurement_theta_min      2.7387
_cell_volume                     3905.5(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
        (compiled Nov 14 2003,14:35:41)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
        (compiled Nov 14 2003,14:35:41)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
        (compiled Nov 14 2003,14:35:41)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -68.00   46.00   0.7500   45.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.0000  -79.0000    0.0000    0.0000    0.0000 152

  2 omega  -68.00   46.00   0.7500   45.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.0000  -79.0000   90.0000    0.0000    0.0000 152

  3 omega  -68.00   46.00   0.7500   45.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.0000  -79.0000  180.0000    0.0000    0.0000 152

  4 omega  -68.00   46.00   0.7500   45.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.0000  -79.0000  270.0000    0.0000    0.0000 152
;
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD-4-circle diffractometer'
_diffrn_orient_matrix_UB_11      0.0456502234
_diffrn_orient_matrix_UB_12      -0.0173629602
_diffrn_orient_matrix_UB_13      -0.0103344945
_diffrn_orient_matrix_UB_21      0.0272277665
_diffrn_orient_matrix_UB_22      0.0331126152
_diffrn_orient_matrix_UB_23      0.0050181119
_diffrn_orient_matrix_UB_31      0.0135108492
_diffrn_orient_matrix_UB_32      -0.0081247221
_diffrn_orient_matrix_UB_33      0.0422195098
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_unetI/netI     0.103
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19626
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         3.28
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.8589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
        Scale3 Abspack program including interframe scaling, empirical
        absorption correction (Blessing) and detector sensitivity correction.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment of twinned crystal'
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                2923
_reflns_number_total             4068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060383vsi20060503_095347.cif
_cod_data_source_block           6b
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4075585