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_4309794
_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            'C98 H137 Mo N7 O2 Ti'
_chemical_formula_weight         1588.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.657(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.290(3)
_cell_length_b                   13.1974(12)
_cell_length_c                   28.668(3)
_cell_measurement_temperature    193(2)
_cell_volume                     9244.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3488
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8998
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.078483
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         8998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.2109
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2942
_reflns_number_gt                4198
_reflns_number_total             8998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051320ssi20050803_105626.cif
_cod_data_source_block           002206m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        9244.5(15)
_cod_database_code               4309794