Synthesis of Molybdenum Nitrido Complexes for Triple-Bond Metathesis of Alkynes and Nitriles
Eric S. Wiedner; Kimberley J. Gallagher; Marc J. A. Johnson; Jeff W. Kampf; Inorganic Chemistry 50 (2011) 5936–5945; doi:10.1021/ic1024247

data_4325468
_publ_section_title
;
 Synthesis of Molybdenum Nitrido Complexes for Triple-Bond Metathesis of
 Alkynes and Nitriles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5936
_journal_page_last               5945
_journal_paper_doi               10.1021/ic1024247
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C44 H56 Mo N2 O3, 0.5(C7 H8)'
_chemical_formula_sum            'C47.5 H50 Mo N2 O3'
_chemical_formula_weight         792.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                87.778(2)
_cell_angle_beta                 85.186(2)
_cell_angle_gamma                78.835(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9987(16)
_cell_length_b                   12.6721(18)
_cell_length_c                   14.715(2)
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.17
_cell_volume                     2004.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40336
_diffrn_reflns_theta_full        26.54
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.9098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0542P)^2^+7.6769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                6223
_reflns_number_total             8251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1024247_si_002_2.cif
_cod_data_source_block           ew1352
_cod_original_formula_sum        'C47.50 H50 Mo N2 O3'
_cod_database_code               4325468