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_4326984
_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         'C50 H38 B F3 Fe N6 O2, 0.867(C H2 Cl2)'
_chemical_formula_sum            'C50.87 H39.73 B Cl1.73 F3 Fe N6 O2'
_chemical_formula_weight         952.17
_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                 94.637(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9620(3)
_cell_length_b                   33.2844(10)
_cell_length_c                   13.5814(4)
_cell_measurement_reflns_used    10919
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      70.595
_cell_measurement_theta_min      3.2598
_cell_volume                     4488.6(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
1 omega -122.00   46.00   1.0000    8.6900
omega____ theta____ kappa____ phi______ frames
-      -40.7737    0.0000 -150.0000 168

2 omega   46.00   82.00   1.0000    8.6900
omega____ theta____ kappa____ phi______ frames
-       40.7737 -125.0000    0.0000 36

3 omega   26.00   73.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000  150.0000 47

4 omega   29.00   71.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000  -30.0000 42

5 omega   97.00  139.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  125.0000   90.0000 42

6 omega  119.00  155.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756   45.0000   30.0000 36

7 omega   36.00   63.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000 -120.0000 27

8 omega   34.00   77.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000   90.0000 43

9 omega   36.00   63.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000   60.0000 27

10 omega   22.00  130.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -77.0000 -120.0000 108

11 omega   95.00  169.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  125.0000 -150.0000 74

12 omega   26.00   54.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000  -90.0000 28

13 omega -117.00  -14.00   1.0000    8.6900
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -37.0000  120.0000 103

14 omega -117.00  -14.00   1.0000    8.6900
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -37.0000   30.0000 103

15 omega   23.00   98.00   1.0000    8.6900
omega____ theta____ kappa____ phi______ frames
-       40.7737 -125.0000  -60.0000 75

16 omega   39.00   90.00   1.0000   65.5100
omega____ theta____ kappa____ phi______ frames
-      100.5756   15.0000 -150.0000 51
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0425383
_diffrn_orient_matrix_UB_12      0.033648
_diffrn_orient_matrix_UB_13      0.0688899
_diffrn_orient_matrix_UB_21      -0.1202403
_diffrn_orient_matrix_UB_22      -0.025653
_diffrn_orient_matrix_UB_23      0.0272871
_diffrn_orient_matrix_UB_31      0.0882995
_diffrn_orient_matrix_UB_32      -0.018715
_diffrn_orient_matrix_UB_33      0.0864594
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.2268
_diffrn_reflns_av_unetI/netI     0.1396
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25772
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.99
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.153
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.91688
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.638
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0804
_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^)+(0.1313P)^2^+0.6279P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2217
_reflns_number_gt                6076
_reflns_number_total             8377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_07.cif
_cod_data_source_block           2acacF3
_cod_database_code               4326984