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_4326979
_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 H29 B F3 Fe N7 O2, C2 H3 N'
_chemical_formula_sum            'C24 H32 B F3 Fe N8 O2'
_chemical_formula_weight         588.24
_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     heavy
_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                 106.1061(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.32026(9)
_cell_length_b                   19.30082(13)
_cell_length_c                   13.78973(11)
_cell_measurement_reflns_used    19120
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      76.6127
_cell_measurement_theta_min      3.3331
_cell_volume                     2894.66(4)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
 1 omega -42.00 -11.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 125.0000 0.0000 31
 2 omega -106.00 -18.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 -37.0000 90.0000 88
 3 omega -66.00 36.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 37.0000 -90.0000 102
 4 omega 51.00 78.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - 40.6487 -125.0000 -90.0000 27
 5 omega 45.00 77.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 -150.0000 32
 6 omega 41.00 96.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -77.0000 -180.0000 55
 7 omega 98.00 124.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 -150.0000 26
 8 omega 40.00 67.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 -120.0000 27
 9 omega 40.00 68.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 60.0000 28
 10 omega 86.00 176.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 -120.0000 90
 11 omega 41.00 77.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 90.0000 36
 12 omega 43.00 76.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 0.0000 33
 13 omega 111.00 147.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -77.0000 -180.0000 36
 14 omega 138.00 177.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 90.0000 39
 15 omega 133.00 174.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 -150.0000 41
 16 omega 90.00 120.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 77.0000 60.0000 30
 17 omega 130.00 156.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 77.0000 60.0000 26
 18 omega 95.00 170.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 -180.0000 75
 19 omega 79.00 105.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 77.0000 -120.0000 26
 20 omega 153.00 178.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 77.0000 -120.0000 25
 21 omega 103.00 160.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 111.0000 90.0000 57
 22 omega -119.00 -7.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 -77.0000 -150.0000 112
 23 omega -119.00 -7.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 -77.0000 -60.0000 112
 24 omega -119.00 -7.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - -40.6487 -77.0000 30.0000 112
 25 omega 23.00 98.00 1.0000 4.1800
 omega____ theta____ kappa____ phi______ frames
 - 40.6487 -125.0000 60.0000 75
 26 omega -140.00 -28.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - -61.5000 -77.0000 120.0000 112
 27 omega -140.00 -28.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - -61.5000 -77.0000 -120.0000 112
 28 omega 85.00 178.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 120.0000 93
 29 omega 85.00 160.00 1.0000 63.2100
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 45.0000 60.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0385334
_diffrn_orient_matrix_UB_12      0.0047903
_diffrn_orient_matrix_UB_13      0.0985216
_diffrn_orient_matrix_UB_21      0.1043268
_diffrn_orient_matrix_UB_22      -0.0502336
_diffrn_orient_matrix_UB_23      0.0513838
_diffrn_orient_matrix_UB_31      0.0877724
_diffrn_orient_matrix_UB_32      0.0618326
_diffrn_orient_matrix_UB_33      0.0342196
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27495
_diffrn_reflns_theta_full        76.81
_diffrn_reflns_theta_max         76.81
_diffrn_reflns_theta_min         4.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.658
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   gaussian
_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)
 numerical absorption correction based on gaussian integration over
 a multifaceted crystal model
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.4566
_exptl_crystal_size_mid          0.1208
_exptl_crystal_size_min          0.0767
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.040
_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     402
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0384P)^2^+1.2116P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                5512
_reflns_number_total             6018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_02.cif
_cod_data_source_block           1acacF3
_cod_database_code               4326979