Coordination-Mode Control of Bound Nitrile Radical Complex Reactivity: Intercepting End-on Nitrile-Mo(III) Radicals at Low Temperature
Meaghan E. Germain; Manuel Temprado; Annie Castonguay; Olga P. Kryatova; Elena V. Rybak-Akimova; John J. Curley; Arjun Mendiratta; Yi-Chou Tsai; Christopher C. Cummins; Rajeev Prabhakar; James E. McDonough; Carl D. Hoff; Journal of the American Chemical Society 131 (2009) 15412–15423; doi:10.1021/ja905849a

data_4105185
_publ_contact_author_address
;Department of Chemistry
University of Miami
1301 Memorial Drive
Coral Gables, Florida 33146
;
_publ_contact_author_email       c.hoff@miami.edu
_publ_contact_author_name        'Carl D. Hoff'
_publ_section_title
;
 Coordination-Mode Control of Bound Nitrile Radical Complex Reactivity:
 Intercepting End-on Nitrile-Mo(III) Radicals at Low Temperature
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15412
_journal_page_last               15423
_journal_paper_doi               10.1021/ja905849a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C45 H65 Mo N5 S'
_chemical_formula_weight         804.02
_chemical_name_common            (Ar[tBu]N)3Mo(N=c(NMe2)(SPh))
_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                 91.6090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8313(7)
_cell_length_b                   14.4109(7)
_cell_length_c                   22.1159(10)
_cell_measurement_reflns_used    5869
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.39
_cell_volume                     4406.4(4)
_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      80(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33529
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9278
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                9327
_reflns_number_total             11082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905849a_si_002.cif
_cod_data_source_block           04091
_cod_database_code               4105185