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_4075581
_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            'C39 H43 Mo2 N3 O S2'
_chemical_formula_weight         825.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_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_creation_date             2006-02-09T13:25:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.892(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8718(15)
_cell_length_b                   14.3618(9)
_cell_length_c                   16.2998(16)
_cell_measurement_reflns_used    4615
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      19.6
_cell_measurement_theta_min      1.97
_cell_volume                     3695.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.671
_diffrn_measured_fraction_theta_max 0.671
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD-4-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9730
_diffrn_reflns_theta_full        20.65
_diffrn_reflns_theta_max         20.65
_diffrn_reflns_theta_min         3.1
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.7897
_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    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
hexagonal plate // {100}, sides {001}, {011}
;
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.824
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         2545
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1489P)^2^+32.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2261
_reflns_number_gt                2176
_reflns_number_total             2545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060383vsi20060503_095347.cif
_cod_data_source_block           5a1
_cod_database_code               4075581