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_4308447
_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_sum            'C100 H96 B2 Cl2 Fe2 N8 O3'
_chemical_formula_weight         1662.07
_chemical_name_common            04151b
_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                89.414(3)
_cell_angle_beta                 78.086(3)
_cell_angle_gamma                87.962(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1918(18)
_cell_length_b                   16.306(2)
_cell_length_c                   22.117(3)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.27
_cell_volume                     4299.4(10)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30569
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.895
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         15055
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1238P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                8991
_reflns_number_total             15055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048427ksi20041110_032456_1.cif
_cod_data_source_block           04151b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4299.5(11)
_cod_database_code               4308447