Activation of Organonitriles toward β-Electrophilic Attack. Synthesis and Characterization of Methyleneamide (Azavinylidene) Complexes of Rhenium
M. Fátima C. Guedes da Silva; João J. R. Fraústo da Silva; Armando J. L. Pombeiro; Inorganic Chemistry 41 (2002) 219–228; doi:10.1021/ic010841m

data_4317434
_publ_section_title
;
 Activation of Organonitriles toward \b-Electrophilic Attack. Synthesis
 and Characterization of Methyleneamide (Azavinylidene) Complexes of
 Rhenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              219
_journal_page_last               228
_journal_paper_doi               10.1021/ic010841m
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C120 H110 B2 Cl6 F10 N2 P8 Re2'
_chemical_formula_weight         2624.58
_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                84.55(2)
_cell_angle_beta                 74.64(2)
_cell_angle_gamma                65.82(2)
_cell_formula_units_Z            1
_cell_length_a                   12.881(3)
_cell_length_b                   14.767(3)
_cell_length_c                   17.785(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2975.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10951
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.338
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_refine_diff_density_max         2.845
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.249
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+7.8504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                7889
_reflns_number_total             10440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010841m.cif
_cod_data_source_block           2transb
_cod_original_cell_volume        2975.6(11)
_cod_database_code               4317434