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_4075582
_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            'C35 H43 Mo2 N3 O S2'
_chemical_formula_weight         777.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_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_creation_date             2006-02-09T15:42:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.796(11)
_cell_angle_beta                 86.048(9)
_cell_angle_gamma                68.941(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9768(9)
_cell_length_b                   13.2860(16)
_cell_length_c                   13.9137(18)
_cell_measurement_reflns_used    1591
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      33.1708
_cell_measurement_theta_min      3.2871
_cell_volume                     1682.2(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_details
;
  1 phi      0.00  270.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
   0.0000   30.0000    0.0000     -        0.0000    0.0000 270

  2 phi    270.00  296.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
   0.0000   30.0000    0.0000     -        0.0000    0.0000 26
;
_diffrn_measurement_device_type  'X-calibur-2 CCD 4-circle diffractometer'
_diffrn_measurement_method       phi-scan
_diffrn_orient_matrix_UB_11      0.0162217027
_diffrn_orient_matrix_UB_12      0.0466619591
_diffrn_orient_matrix_UB_13      -0.0247178541
_diffrn_orient_matrix_UB_21      0.0303654178
_diffrn_orient_matrix_UB_22      0.0017471539
_diffrn_orient_matrix_UB_23      0.0439644876
_diffrn_orient_matrix_UB_31      0.0679633711
_diffrn_orient_matrix_UB_32      -0.0350621274
_diffrn_orient_matrix_UB_33      -0.0132922049
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8920
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.29
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_correction_T_min  0.9314
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                3592
_reflns_number_total             5516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060383vsi20060503_095347.cif
_cod_data_source_block           5b1
_cod_original_cell_volume        1682.2(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075582