Oxygen Activation by Nonheme Iron(II) Complexes: α-Keto Carboxylate versus Carboxylate
Mark P. Mehn; Kiyoshi Fujisawa; Eric L. Hegg; Lawrence Que; Journal of the American Chemical Society 125 (2003) 7828–7842; doi:10.1021/ja028867f

data_4113841
_publ_section_title
;
 Oxygen Activation by Nonheme Iron(II) Complexes: \a-Keto Carboxylate
 versus Carboxylate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7828
_journal_page_last               7842
_journal_paper_doi               10.1021/ja028867f
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C48 H37 B Fe N6 O3'
_chemical_formula_sum            'C48 H37 B Fe N6 O3'
_chemical_formula_weight         812.49
_chemical_name_common            01119
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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            8
_cell_length_a                   18.125(1)
_cell_length_b                   16.326(1)
_cell_length_c                   27.145(2)
_cell_measurement_reflns_used    2476
_cell_measurement_temperature    173(2)
_cell_volume                     8032.4(9)
_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    SHELXS-97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.1519
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45542
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.678892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         13993
_refine_ls_number_restraints     755
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0633
_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 
 [0.00000+1.00000exp(1.20(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0661P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                6300
_reflns_number_total             13993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028867fsi20021008_062216_1.cif
_cod_data_source_block           01119
_cod_original_cell_volume        8032.3(9)
_cod_database_code               4113841