Iron Coordination Chemistry of Phenylpyruvate: An Unexpected κ3-Bridging Mode That Leads to Oxidative Cleavage of the C2-C3 Bond
Tapan K. Paine; Hui Zheng; Lawrence Que; Inorganic Chemistry 44 (2005) 474–476; doi:10.1021/ic048427k

data_4308448
_publ_contact_author_name        'Lawrence Que Jr.'
_publ_section_title
;
Iron Coordination Chemistry of Phenylpyruvate: An Unexpected \k3-Bridging
Mode That Leads to Oxidative Cleavage of the C2-C3 Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              474
_journal_page_last               476
_journal_paper_doi               10.1021/ic048427k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '2(C H2 Cl2), C54 H41 B Fe N6 O3'
_chemical_formula_sum            'C56 H45 B Cl4 Fe N6 O3'
_chemical_formula_weight         1058.44
_chemical_name_common            03267
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.223(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.056(3)
_cell_length_b                   37.072(9)
_cell_length_c                   13.409(3)
_cell_measurement_reflns_used    1015
_cell_measurement_temperature    173(2)
_cell_volume                     4999(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48025
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         0.55
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.838955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8797
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+6.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                7265
_reflns_number_total             8797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048427ksi20041110_032456_2.cif
_cod_data_source_block           03267
_cod_database_code               4308448