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_4326575
_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            'C66 H82 I3 Mo N2 O'
_chemical_formula_weight         1395.98
_chemical_name_common            MoI3(THF)(CNArDipp2)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.956(6)
_cell_length_b                   17.956(6)
_cell_length_c                   41.03(2)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.19
_cell_volume                     13229(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.1729
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            99709
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.29
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  0.8405
_exptl_absorpt_correction_T_min  0.7913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
; 
SQUEEZE was employed to account for severely disordered molecules of THF 
(C4H8O).  A total of 352 electrons in a solvent accessible void of 
1285.8 Ang^3 were accounted for.  This corresponds to roughly 8 
disordered molecules of THF per unit cell. 
;
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.97(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         14759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                12071
_reflns_number_total             14759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015868_si_001_10.cif
_cod_data_source_block           MoI3(THF)(CNArDipp2)2
_cod_database_code               4326575