Theoretical, Thermodynamic, Spectroscopic, and Structural Studies of the Consequences of One-Electron Oxidation on the Fe-X Bonds in 17- and 18-Electron Cp*Fe(dppe)X Complexes (X = F, Cl, Br, I, H, CH3)
Mats Tilset; Irene Fjeldahl; Jean-René Hamon; Paul Hamon; Loïc Toupet; Jean-Yves Saillard; Karine Costuas; Anthony Haynes; Journal of the American Chemical Society 123 (2001) 9984–10000; doi:10.1021/ja0106927

data_4115717
_publ_contact_author
;
Toupet Loic
G.M.C.M.-UMR6626
Universite de Rennes
Campus de Beaulieu
35042 RENNES cedex , FRANCE
;
_publ_contact_author_email       loic.toupet@univ-rennes1.fr
_publ_contact_author_fax         '(33) 2 99 28 67 17'
_publ_contact_author_phone       '(33) 2 99 28 60 65'
_publ_section_title
;
 Theoretical, Thermodynamic, Spectroscopic, and Structural Studies of the
 Consequences of One-Electron Oxidation on the Fe-X Bonds in 17- and
 18-Electron Cp*Fe(dppe)X Complexes (X = F, Cl, Br, I, H, CH3)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9984
_journal_page_last               10000
_journal_paper_doi               10.1021/ja0106927
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C36 H39 Cl F6 Fe P3'
_chemical_formula_weight         769.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   12.763(3)
_cell_length_b                   13.877(7)
_cell_length_c                   19.551(7)
_cell_measurement_temperature    293(2)
_cell_volume                     3463(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3406
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.710
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       prism
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_coef       0.0059(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.613
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                2423
_reflns_number_total             3406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0106927_2.cif
_cod_data_source_block           compound2
_cod_database_code               4115717