Synthesis and Characterization of Fe(II) β-Diketonato Complexes with Relevance to Acetylacetone Dioxygenase: Insights into the Electronic Properties of the 3-Histidine Facial Triad
Heaweon Park; Jacob S. Baus; Sergey V. Lindeman; Adam T. Fiedler; Inorganic Chemistry 50 (2011) 11978–11989; doi:10.1021/ic201115s

data_4326987
_publ_section_title
;
 Synthesis and Characterization of Fe(II) \b-Diketonato Complexes with
 Relevance to Acetylacetone Dioxygenase: Insights into the Electronic
 Properties of the 3-Histidine Facial Triad
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11978
_journal_page_last               11989
_journal_paper_doi               10.1021/ic201115s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H25 F3 Fe N6 O2 P, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C34 H27 Cl2 F6 Fe N6 O5 P S'
_chemical_formula_weight         903.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-04-25
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                85.8018(19)
_cell_angle_beta                 71.277(2)
_cell_angle_gamma                87.183(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9737(3)
_cell_length_b                   12.6383(3)
_cell_length_c                   14.6113(3)
_cell_measurement_reflns_used    44442
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.4949
_cell_measurement_theta_min      3.4421
_cell_volume                     1913.33(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
  1 omega  -65.00   45.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000   30.0000 110

  2 omega    6.00   88.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   77.0000  120.0000 82

  3 omega  -81.00   21.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697  -77.0000 -120.0000 102

  4 omega    9.00   75.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134 -136.0000   -6.0000 66

  5 omega  -67.00   45.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000 -180.0000 112

  6 omega  -65.00   38.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -37.0000   60.0000 103

  7 omega  -15.00   88.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   37.0000  150.0000 103

  8 omega  -22.00   90.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   77.0000    0.0000 112

  9 omega  -73.00  -27.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697  132.0000   59.0000 46

 10 omega  -15.00   88.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   37.0000  -90.0000 103

 11 omega  -67.00   45.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000    0.0000 112

 12 omega    9.00   75.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134 -136.0000  -57.0000 66

 13 omega  -73.00  -27.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697  132.0000    9.0000 46

 14 omega  -73.00  -27.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697  132.0000 -120.0000 46

 15 omega  -28.00   64.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697   37.0000 -120.0000 92

 16 omega  -78.00  101.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000 -180.0000 179

 17 omega  -78.00    2.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000 -150.0000 80

 18 omega  -67.00   45.00   1.0000   20.4000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000 -150.0000 112
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0011541000
_diffrn_orient_matrix_UB_12      0.0198116000
_diffrn_orient_matrix_UB_13      -0.0464140000
_diffrn_orient_matrix_UB_21      -0.0526751000
_diffrn_orient_matrix_UB_22      0.0344289000
_diffrn_orient_matrix_UB_23      0.0219692000
_diffrn_orient_matrix_UB_31      0.0434194000
_diffrn_orient_matrix_UB_32      0.0398907000
_diffrn_orient_matrix_UB_33      -0.0003095000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            86437
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.4949
_diffrn_reflns_theta_min         3.4421
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         10144
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0623P)^2^+0.2798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                8159
_reflns_number_total             10144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_10.cif
_cod_data_source_block           3acacF3
_cod_original_cell_volume        1913.32(8)
_cod_database_code               4326987
_chemical_oxdiff_formula         'Fe C32 H25 N6 O2 P F3'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32