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_4326571
_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            'C78 H94 I4 Mo N2'
_chemical_formula_weight         1663.10
_chemical_name_common            trans-MoI4(CNArDipp2)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 126.228(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.601(5)
_cell_length_b                   16.167(4)
_cell_length_c                   15.491(7)
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.45
_cell_volume                     4162(2)
_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 0.998
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19075
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_platon_squeeze_details
; 
SQUEEZE was employed to account for severely disordered molecules of Tol 
(C7H8).  A total of 221 electrons in a solvent accessible void of 
724.0 Ang^3 were accounted for.  This corresponds to roughly 4 
disordered molecules of Tol per unit cell. 
;
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+4.8892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                3822
_reflns_number_total             4747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015868_si_001_06.cif
_cod_data_source_block           jfig217
_cod_depositor_comments
;

2021-04-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         831.55
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C39 H47 I2 Mo0.50 N'
_cod_database_code               4326571