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_4075584
_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_moiety         'C40 H45 Mo2 N3 O1 S3, 0.143(O1)'
_chemical_formula_sum            'C40 H45 Mo2 N3 O1.143 S2'
_chemical_formula_weight         842.10
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.36000(10)
_cell_length_b                   16.9560(2)
_cell_length_c                   26.1569(4)
_cell_measurement_reflns_used    137299
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     3697.36(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.148
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39623
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724.6
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                4520
_reflns_number_total             6477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060383vsi20060503_095347.cif
_cod_data_source_block           6a
_cod_database_code               4075584