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_4326982
_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 H41 B Fe N6 O2'
_chemical_formula_sum            'C50 H41 B Fe N6 O2'
_chemical_formula_weight         824.55
_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             2011-04-18
_audit_creation_method
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
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_cell_angle_alpha                90.00
_cell_angle_beta                 112.1370(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.88320(12)
_cell_length_b                   18.87572(15)
_cell_length_c                   16.93576(18)
_cell_measurement_reflns_used    30246
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.7608
_cell_measurement_theta_min      3.2818
_cell_volume                     4110.95(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
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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
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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 0.927
_diffrn_measurement_details
;
1 omega  -12.00   43.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376   77.0000  150.0000 55

2 omega  -50.00   46.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376  -37.0000  120.0000 96

3 omega   -7.00   85.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376   37.0000  -60.0000 92

4 omega   -7.00   96.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376   37.0000   90.0000 103

5 omega  -56.00   46.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376  -37.0000    0.0000 102

6 omega  -59.00  -34.00   1.0000   50.6300
omega____ theta____ kappa____ phi______ frames
-       19.7376  -77.0000 -120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.031178
_diffrn_orient_matrix_UB_12      -0.0020993
_diffrn_orient_matrix_UB_13      0.0440888
_diffrn_orient_matrix_UB_21      0.0438205
_diffrn_orient_matrix_UB_22      0.0114724
_diffrn_orient_matrix_UB_23      -0.0084643
_diffrn_orient_matrix_UB_31      -0.0122255
_diffrn_orient_matrix_UB_32      0.0357274
_diffrn_orient_matrix_UB_33      0.0053046
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59544
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         32.84
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.81481
_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    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         14181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.7078P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                10683
_reflns_number_total             14181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_05.cif
_cod_data_source_block           2acac
_cod_database_code               4326982