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_4326985
_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         'C55 H40 B F3 Fe N6 O2, C H2 Cl2'
_chemical_formula_sum            'C56 H42 B Cl2 F3 Fe N6 O2'
_chemical_formula_weight         1025.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2011-04-21
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.429(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9045(7)
_cell_length_b                   35.733(2)
_cell_length_c                   13.4769(9)
_cell_measurement_reflns_used    6548
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      74.4721
_cell_measurement_theta_min      3.2795
_cell_volume                     4765.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega  -65.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237   37.0000 -180.0000 100

  2 omega  -83.00  -57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  125.0000   90.0000 26

  3 omega  -71.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237   77.0000   30.0000 36

  4 omega  -53.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237   37.0000  -90.0000 84

  5 omega   32.00   72.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -30.0000 40

  6 omega   34.00  166.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -15.0000   90.0000 132

  7 omega   33.00   60.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   90.0000 27

  8 omega   34.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   60.0000 31

  9 omega   34.00  133.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000 -120.0000 99

 10 omega   46.00  140.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000   60.0000 94

 11 omega -117.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  -37.0000 -180.0000 103

 12 omega    7.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237   77.0000  -30.0000 112

 13 omega    7.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237   77.0000   90.0000 112

 14 omega   46.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000 -150.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0725049000
_diffrn_orient_matrix_UB_12      0.0071228000
_diffrn_orient_matrix_UB_13      -0.1015802000
_diffrn_orient_matrix_UB_21      -0.1365068000
_diffrn_orient_matrix_UB_22      -0.0091864000
_diffrn_orient_matrix_UB_23      0.0452945000
_diffrn_orient_matrix_UB_31      -0.0171760000
_diffrn_orient_matrix_UB_32      0.0415038000
_diffrn_orient_matrix_UB_33      0.0274348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26605
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.090
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.3686
_exptl_crystal_size_mid          0.1889
_exptl_crystal_size_min          0.0566
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0429P)^2^+15.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                7234
_reflns_number_total             9427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_08.cif
_cod_data_source_block           2acacPhF3
_cod_database_code               4326985
_chemical_oxdiff_formula         'Fe C56 H42 N6 O2 F3 Cl2 B'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97