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_4326980
_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         'C27 H31 B F3 Fe N7 O2, C2 H3 N'
_chemical_formula_sum            'C29 H34 B F3 Fe N8 O2'
_chemical_formula_weight         650.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-04-20
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.273(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3762(7)
_cell_length_b                   12.3527(9)
_cell_length_c                   16.0614(6)
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      73.7837
_cell_measurement_theta_min      3.4957
_cell_volume                     3174.8(3)
_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 0.971
_diffrn_measurement_details
;
  1 omega  -67.00   34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737   37.0000 -180.0000 101

  2 omega  -86.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  125.0000    0.0000 84

  3 omega  -43.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  125.0000  -90.0000 32

  4 omega   32.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000  -60.0000 71

  5 omega   32.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   30.0000 25

  6 omega   32.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  120.0000 43

  7 omega  140.00  168.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  -60.0000 28

  8 omega   89.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  -60.0000 27

  9 omega   45.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -180.0000 25

 10 omega   64.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000 -120.0000 113

 11 omega  107.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000  -60.0000 34

 12 omega   33.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -30.0000 26

 13 omega   49.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  150.0000 26

 14 omega   42.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -150.0000 34

 15 omega -119.00  -61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7737  -77.0000   60.0000 58
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0287259000
_diffrn_orient_matrix_UB_12      0.0776845000
_diffrn_orient_matrix_UB_13      0.0630053000
_diffrn_orient_matrix_UB_21      -0.0881387000
_diffrn_orient_matrix_UB_22      0.0032172000
_diffrn_orient_matrix_UB_23      -0.0574357000
_diffrn_orient_matrix_UB_31      -0.0258560000
_diffrn_orient_matrix_UB_32      -0.0971896000
_diffrn_orient_matrix_UB_33      0.0484599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13228
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.22
_diffrn_reflns_theta_min         4.52
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.555
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2043
_exptl_crystal_size_mid          0.1736
_exptl_crystal_size_min          0.1203
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+1.0250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                5784
_reflns_number_total             6281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_03.cif
_cod_data_source_block           1acacPhF3
_cod_database_code               4326980
_chemical_oxdiff_formula         'Fe C29 H33 N8 O2 F3 B'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97