A Cycle for Organic Nitrile Synthesis via Dinitrogen Cleavage
John J. Curley; Emma L. Sceats; Christopher C. Cummins; Journal of the American Chemical Society 128 (2006) 14036–14037; doi:10.1021/ja066090a

data_4111044
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology 
77 Massachusetts Av. 
Cambridge, MA 02139
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 A Cycle for Organic Nitrile Synthesis via Dinitrogen Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14036
_journal_page_last               14037
_journal_paper_doi               10.1021/ja066090a
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C46 H68 Mo N4 O Si'
_chemical_formula_weight         817.07
_chemical_name_common            Ph(Me3SiO)C=NMo(N[t-Bu](3,5-C6H3Me2)
_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                103.380(7)
_cell_angle_beta                 103.203(6)
_cell_angle_gamma                97.163(6)
_cell_formula_units_Z            2
_cell_length_a                   9.5296(16)
_cell_length_b                   12.337(3)
_cell_length_c                   20.531(4)
_cell_measurement_reflns_used    7076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2245.6(8)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            46636
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.9809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         11152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0440P)^2^+1.0415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                9950
_reflns_number_total             11152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066090asi20060915_111623.cif
_cod_data_source_block           05148
_cod_database_code               4111044