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_4326986
_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 H28 Fe N6 O2 P, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C35 H31 F3 Fe N7 O5 P S'
_chemical_formula_weight         805.55
_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             2011-05-04
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                87.443(2)
_cell_angle_beta                 71.223(2)
_cell_angle_gamma                89.004(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8489(3)
_cell_length_b                   12.6264(3)
_cell_length_c                   14.4290(4)
_cell_measurement_reflns_used    19230
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.4600
_cell_measurement_theta_min      3.4452
_cell_volume                     1869.46(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_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 0.917
_diffrn_measurement_details
;
  1 omega    1.00   90.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697   77.0000 -120.0000 89

  2 omega  -22.00   86.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697   77.0000   30.0000 108

  3 omega  -45.00   66.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   77.0000  120.0000 111

  4 omega  -17.00   56.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -103.0000  102.0000 73

  5 omega  -64.00   38.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -37.0000  -90.0000 102

  6 omega  -15.00   88.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000 -150.0000 103

  7 omega  -15.00   88.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000   90.0000 103

  8 omega  -17.00   56.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -103.0000  -23.0000 73

  9 omega  -56.00   -5.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  103.0000 -156.0000 51

 10 omega  -28.00    0.00   1.0000    7.0300
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   37.0000 -180.0000 28
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0506097000
_diffrn_orient_matrix_UB_12      0.0081916000
_diffrn_orient_matrix_UB_13      0.0446229000
_diffrn_orient_matrix_UB_21      0.0237491000
_diffrn_orient_matrix_UB_22      -0.0431023000
_diffrn_orient_matrix_UB_23      0.0226736000
_diffrn_orient_matrix_UB_31      0.0405378000
_diffrn_orient_matrix_UB_32      0.0351729000
_diffrn_orient_matrix_UB_33      0.0139684000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42236
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.4600
_diffrn_reflns_theta_min         3.4452
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.4708
_exptl_crystal_size_mid          0.2386
_exptl_crystal_size_min          0.0789
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0342P)^2^+1.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                7894
_reflns_number_total             9554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_09.cif
_cod_data_source_block           3acac
_cod_original_cell_volume        1869.46(8)
_cod_database_code               4326986
_chemical_oxdiff_formula         'Fe C33 H28 N6 O5 P S F3'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32