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_4326983
_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
'C53 H47 B Fe N6 O2, 0.5(C4 H8 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C56 H52.5 B Fe N6.5 O2.5'
_chemical_formula_weight         923.20
_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             2011-05-04
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0112(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.75151(12)
_cell_length_b                   35.2674(4)
_cell_length_c                   13.67554(17)
_cell_measurement_reflns_used    8953
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      70.7277
_cell_measurement_theta_min      3.4709
_cell_volume                     4691.64(10)
_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 0.991
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
1 omega -106.00  -18.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -77.0000 -150.0000 88

2 omega -111.00  -26.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -37.0000   90.0000 85

3 omega   73.00   98.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-       40.7737 -125.0000   30.0000 25

4 omega   28.00   77.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000 -150.0000 49

5 omega   34.00   60.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000  -90.0000 26

6 omega   21.00  161.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -15.0000 -120.0000 140

7 omega   27.00   65.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000   30.0000 38

8 omega   37.00   76.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000  -60.0000 39

9 omega   27.00  130.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -77.0000   30.0000 103

10 omega   31.00   76.00   1.0000   97.5700
omega____ theta____ kappa____ phi______ frames
-      100.5756  -45.0000   60.0000 45

11 omega  -96.00   -2.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-      -40.7737  125.0000 -180.0000 94

12 omega  -95.00  -17.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -77.0000  -60.0000 78

13 omega -117.00  -85.00   1.0000   12.6700
omega____ theta____ kappa____ phi______ frames
-      -40.7737  -37.0000  -30.0000 32
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0040733
_diffrn_orient_matrix_UB_12      0.0006244
_diffrn_orient_matrix_UB_13      -0.1124118
_diffrn_orient_matrix_UB_21      -0.1491017
_diffrn_orient_matrix_UB_22      0.0147033
_diffrn_orient_matrix_UB_23      -0.0097131
_diffrn_orient_matrix_UB_31      0.0533265
_diffrn_orient_matrix_UB_32      0.0411114
_diffrn_orient_matrix_UB_33      0.0053254
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22809
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.86
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.81094
_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    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                6059
_reflns_number_total             8776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_06.cif
_cod_data_source_block           2acactBu
_cod_original_cell_volume        4691.63(10)
_cod_original_formula_sum        'C56 H52.50 B Fe N6.50 O2.50'
_cod_database_code               4326983