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_4326978
_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 H32 B Fe N7 O2, 2(C2 H3 N)'
_chemical_formula_sum            'C26 H38 B Fe N9 O2'
_chemical_formula_weight         575.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-04-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                91.901(2)
_cell_angle_beta                 98.880(2)
_cell_angle_gamma                97.026(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8894(2)
_cell_length_b                   12.1386(3)
_cell_length_c                   16.3511(4)
_cell_measurement_reflns_used    29728
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.7662
_cell_measurement_theta_min      3.3048
_cell_volume                     1533.33(7)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
1 omega  -34.00   55.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376  -86.0000   34.0000 89

2 omega   -3.00   98.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376   77.0000  150.0000 101

3 omega  -14.00   79.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376   77.0000  -60.0000 93

4 omega  -47.00   -3.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376  -77.0000  -90.0000 44

5 omega  -16.00   10.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939  -77.0000  150.0000 26

6 omega  -99.00  -73.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939  -77.0000  150.0000 26

7 omega  -59.00   53.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376  -77.0000 -180.0000 112

8 omega  -34.00   16.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939  -86.0000   27.0000 50

9 omega  -28.00   56.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939   37.0000  120.0000 84

10 omega  -56.00   14.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939   86.0000  -34.0000 70

11 omega  -28.00   56.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939   37.0000  -90.0000 84

12 omega  -14.00   98.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376   77.0000    0.0000 112

13 omega  -59.00   53.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376  -77.0000  -90.0000 112

14 omega  -59.00   53.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376  -77.0000   90.0000 112

15 omega  -14.00   98.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376   77.0000 -150.0000 112

16 omega  -28.00   56.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939   37.0000  -30.0000 84

17 omega   -7.00   96.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-       19.7376   37.0000  120.0000 103

18 omega  -56.00    3.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939   86.0000  152.0000 59

19 omega  -34.00   16.00   1.0000   21.9200
omega____ theta____ kappa____ phi______ frames
-      -19.8939  -86.0000 -145.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0905511
_diffrn_orient_matrix_UB_12      0.0151074
_diffrn_orient_matrix_UB_13      0.0029207
_diffrn_orient_matrix_UB_21      0.0024377
_diffrn_orient_matrix_UB_22      0.0270448
_diffrn_orient_matrix_UB_23      0.0393676
_diffrn_orient_matrix_UB_31      0.0146655
_diffrn_orient_matrix_UB_32      -0.0501646
_diffrn_orient_matrix_UB_33      0.01936
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71038
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.84
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.40884
_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    1.246
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         10798
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0478P)^2^+0.2981P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                8616
_reflns_number_total             10798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_01.cif
_cod_data_source_block           1acac
_cod_database_code               4326978