Molybdenum Nitride Complexes with Ph3SiO Ligands Are Exceedingly Practical and Tolerant Precatalysts for Alkyne Metathesis and Efficient Nitrogen Transfer Agents
Martin Bindl; Robert Stade; Eike K. Heilmann; Alexandre Picot; Richard Goddard; Alois Fürstner; Journal of the American Chemical Society 131 (2009) 9468–9470; doi:10.1021/ja903259g

data_4104673
_publ_section_title
;
 Molybdenum Nitride Complexes with Ph3SiO Ligands Are Exceedingly
 Practical and Tolerant Precatalysts for Alkyne Metathesis and Efficient
 Nitrogen Transfer Agents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9468
_journal_page_last               9470
_journal_paper_doi               10.1021/ja903259g
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        toluene
_chemical_formula_moiety         'C59 H50 MO N2 O3 Si3, C7 H8'
_chemical_formula_sum            'C66 H58 Mo N2 O3 Si3'
_chemical_formula_weight         1107.35
_chemical_name_systematic
; 
 N-pyridine-tris(triphenylsiloxy)-molybdenum-nitride
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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_block_code                BMA-BC-117-01
_audit_creation_date             2008-07-23
_cell_angle_alpha                87.206(1)
_cell_angle_beta                 77.527(1)
_cell_angle_gamma                64.003(1)
_cell_formula_units_Z            2
_cell_length_a                   13.0697(2)
_cell_length_b                   13.5755(3)
_cell_length_c                   18.2169(3)
_cell_measurement_reflns_used    71022
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.91
_cell_volume                     2832.69(9)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86247
_diffrn_reflns_theta_full        31.59
_diffrn_reflns_theta_max         31.59
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.94306
_exptl_absorpt_correction_T_min  0.86938
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.420
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         18892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0690P)^2^+5.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                14883
_reflns_number_total             18892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903259g_si_001.cif
_cod_data_source_block           6300
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4104673