Heterobimetallic Reductive Cross-Coupling of Benzonitrile with Carbon Dioxide, Pyridine, and Benzophenone
Arjun Mendiratta; Christopher C. Cummins; Inorganic Chemistry 44 (2005) 7319–7321; doi:10.1021/ic051320s

data_4309793
_publ_section_title
;
Heterobimetallic Reductive Cross-Coupling of Benzonitrile with Carbon
Dioxide, Pyridine, and Benzophenone
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7319
_journal_page_last               7321
_journal_paper_doi               10.1021/ic051320s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C79 H101 Mo N7 O2 Ti'
_chemical_formula_weight         1324.51
_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                112.2270(10)
_cell_angle_beta                 94.7310(10)
_cell_angle_gamma                100.7660(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4158(5)
_cell_length_b                   18.4340(8)
_cell_length_c                   20.0106(9)
_cell_measurement_temperature    293(2)
_cell_volume                     3774.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16339
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.320
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          5.024
_refine_ls_shift/su_mean         0.164
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                7721
_reflns_number_total             9855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051320ssi20050803_105606.cif
_cod_data_source_block           003289m
_cod_database_code               4309793