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_4326981
_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         'C22 H26 B F6 Fe N7 O2'
_chemical_formula_sum            'C22 H26 B F6 Fe N7 O2'
_chemical_formula_weight         601.16
_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             2011-05-27
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6456(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.72084(10)
_cell_length_b                   19.56928(16)
_cell_length_c                   11.95953(9)
_cell_measurement_reflns_used    40723
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      37.6382
_cell_measurement_theta_min      3.3770
_cell_volume                     2704.36(4)
_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      100.15
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega   -2.00   74.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808   77.0000   90.0000 76

  2 omega  -19.00   21.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808  -37.0000  120.0000 40

  3 omega  -48.00  118.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808    0.0000  -30.0000 166

  4 omega  -47.00   44.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808  -77.0000   60.0000 91

  5 omega   -2.00  110.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808   77.0000  -30.0000 112

  6 omega  -47.00   65.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -       31.4808  -77.0000  -60.0000 112

  7 omega -111.00    2.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -      -31.7933  -77.0000 -180.0000 113

  8 omega  -28.00   44.00   1.0000   38.9200
omega____ theta____ kappa____ phi______ frames
    -      -31.7933   37.0000 -120.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0056776000
_diffrn_orient_matrix_UB_12      0.0026548000
_diffrn_orient_matrix_UB_13      0.0598103000
_diffrn_orient_matrix_UB_21      -0.0580547000
_diffrn_orient_matrix_UB_22      -0.0110775000
_diffrn_orient_matrix_UB_23      -0.0030018000
_diffrn_orient_matrix_UB_31      0.0190884000
_diffrn_orient_matrix_UB_32      -0.0344266000
_diffrn_orient_matrix_UB_33      0.0055747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81670
_diffrn_reflns_theta_full        37.73
_diffrn_reflns_theta_max         37.73
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81873
_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            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         14031
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0501P)^2^+0.2473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                11230
_reflns_number_total             14031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_04.cif
_cod_data_source_block           1acacF6
_cod_database_code               4326981
_chemical_oxdiff_formula         'Fe C20 H23 N6 O2 F6 B'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23