Oxidation of Sulfide, Phosphine, and Benzyl Substrates Tethered to N-Donor Pyridine Ligands in Carboxylate-Bridged Diiron(II) Complexes
Emily C. Carson; Stephen J. Lippard; Journal of the American Chemical Society 126 (2004) 3412–3413; doi:10.1021/ja031806c

data_4112330
_publ_section_title
;
 Oxidation of Sulfide, Phosphine, and Benzyl Substrates Tethered to
 N-Donor Pyridine Ligands in Carboxylate-Bridged Diiron(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3412
_journal_page_last               3413
_journal_paper_doi               10.1021/ja031806c
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C101 H82 Fe2 N O8 P'
_chemical_formula_weight         1580.35
_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                96.150(5)
_cell_angle_beta                 90.847(6)
_cell_angle_gamma                112.399(3)
_cell_formula_units_Z            2
_cell_length_a                   12.810(2)
_cell_length_b                   15.785(3)
_cell_length_c                   21.780(4)
_cell_measurement_reflns_used    967
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.64
_cell_volume                     4040.9(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35186
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         18026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                13036
_reflns_number_total             18026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja031806csi20031218_113942.cif
_cod_data_source_block           '[FE2(m-O2CArTol)3(O2CArTol)(2-Ph2Ppy)]'
_cod_original_cell_volume        4041.0(12)
_cod_database_code               4112330