Oxidative Decarbonylation of m-Terphenyl Isocyanide Complexes of Molybdenum and Tungsten: Precursors to Low-Coordinate Isocyanide Complexes
Treffly B. Ditri; Curtis E. Moore; Arnold L. Rheingold; Joshua S. Figueroa; Inorganic Chemistry 50 (2011) 10448–10459; doi:10.1021/ic2015868

data_4326576
_publ_section_title
;
 Oxidative Decarbonylation of m-Terphenyl Isocyanide Complexes of
 Molybdenum and Tungsten: Precursors to Low-Coordinate Isocyanide
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10448
_journal_page_last               10459
_journal_paper_doi               10.1021/ic2015868
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C142 H178 Mo2 N8 O Si2'
_chemical_formula_weight         2260.98
_chemical_name_common            (eta6-C6H6)Mo(N2)(CNArDipp2)2
_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                74.1840(10)
_cell_angle_beta                 74.6450(10)
_cell_angle_gamma                68.8530(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5493(10)
_cell_length_b                   12.7014(11)
_cell_length_c                   22.4890(19)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.32
_cell_volume                     3160.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43502
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.9112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       Block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.033
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+8.0014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                10245
_reflns_number_total             11568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015868_si_001_11.cif
_cod_data_source_block           (eta6-C6H6)Mo(N2)(CNArDipp2)2
_cod_database_code               4326576