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_4075583
_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           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-02-10T11:43:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2946(8)
_cell_length_b                   13.4907(6)
_cell_length_c                   16.0487(7)
_cell_measurement_reflns_used    9201
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      1.89
_cell_volume                     3527.9(3)
_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      300(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
  1 omega  -54.00   60.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       25.0000  -79.0000    0.0000    0.0000    0.0000 153

  2 omega  -54.00   60.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       25.0000  -79.0000   90.0000    0.0000    0.0000 153

  3 omega  -54.00   60.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       25.0000  -79.0000  180.0000    0.0000    0.0000 153

  4 omega  -54.00   60.75   0.7500   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       25.0000  -79.0000  270.0000    0.0000    0.0000 153
;
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD 4-circle diffractometer'
_diffrn_measurement_method
;
omega-scans with kappa = -79%  and phi = 0, 90, 180, 270%
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35546
_diffrn_reflns_theta_full        31.18
_diffrn_reflns_theta_max         31.18
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.86
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.6731
_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    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
'fragment of rhombic plate, main face // (010)'
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.1
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8842
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                6223
_reflns_number_total             8842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060383vsi20060503_095347.cif
_cod_data_source_block           5b2
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4075583