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_4112333
_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            'C96 H79 Cl Fe2 N O8 S'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.483(5)
_cell_angle_gamma                113.723(4)
_cell_formula_units_Z            2
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_cell_length_b                   15.545(5)
_cell_length_c                   21.915(6)
_cell_measurement_reflns_used    974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.53
_cell_volume                     3905(2)
_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 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0763
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34415
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             1622
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         17575
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_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1023
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja031806csi20040129_032030.cif
_cod_data_source_block           '[Fe2(m-O2CArTol)3(O2CArTol)(2-PhSpy)]'
_cod_original_cell_volume        3904.5(19)
_cod_database_code               4112333