Reaction Mechanism of the C\τbN Triple Bond Cleavage of β-Ketonitriles on a Molybdenum(0) Center1
Yoshiaki Tanabe; Hidetake Seino; Youichi Ishii; Masanobu Hidai; Journal of the American Chemical Society 122 (2000) 1690–1699; doi:10.1021/ja9921928

data_4115931
_publ_contact_author_address
;
    Department of Chemistry and Biotechnology, Graduate School of Engineering,
The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113-8656, Japan
;
_publ_contact_author_email       ' hidai@chembio.t.u-tokyo.ac.jp '
_publ_contact_author_fax         ' +81-3-5841-7265 '
_publ_contact_author_name        ' Masanobu Hidai'
_publ_contact_author_phone       ' +81-3-5841-7261 '
_publ_section_title
;
 Reaction Mechanism of the C\\tbN Triple Bond Cleavage of \b-Ketonitriles
 on a Molybdenum(0) Center1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1690
_journal_page_last               1699
_journal_paper_doi               10.1021/ja9921928
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C60 H57 Cl3 Mo N3 O P4'
_chemical_formula_weight         1162.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Thu Jun  3 20:55:34 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.19(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.982(5)
_cell_length_b                   18.416(4)
_cell_length_c                   22.753(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      17.8
_cell_measurement_theta_min      13.9
_cell_volume                     5766(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06760
_diffrn_orient_matrix_UB_12      0.00174
_diffrn_orient_matrix_UB_13      -0.00871
_diffrn_orient_matrix_UB_21      -0.02661
_diffrn_orient_matrix_UB_22      0.00131
_diffrn_orient_matrix_UB_23      -0.04378
_diffrn_orient_matrix_UB_31      -0.00153
_diffrn_orient_matrix_UB_32      0.05426
_diffrn_orient_matrix_UB_33      0.00133
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.160
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10594
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        -3.09
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2396.00
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.632
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     649
_refine_ls_number_reflns         4451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.4790
_refine_ls_shift/su_mean         0.0130
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0350
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                4451
_reflns_number_total             10151
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja9921928_1.cif
_cod_data_source_block
'[Mo(N)(NCC(CN)COCH3)(dppe)2].5C2H4Cl2_(Compound_4h.5C2H4Cl2)'
_cod_original_cell_volume        5766(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C60 H57 Cl3 N3 Mo O P4 '
_cod_database_code               4115931