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_4326988
_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         'C37 H27 F3 Fe N6 O2 P, 4(C H2 Cl2), C F3 O3 S'
_chemical_formula_sum            'C42 H35 Cl8 F6 Fe N6 O5 P S'
_chemical_formula_weight         1220.24
_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             2011-04-25
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                85.0393(15)
_cell_angle_beta                 78.0672(17)
_cell_angle_gamma                83.3042(17)
_cell_formula_units_Z            2
_cell_length_a                   11.4327(3)
_cell_length_b                   12.8330(2)
_cell_length_c                   17.9561(3)
_cell_measurement_reflns_used    14001
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      73.8642
_cell_measurement_theta_min      3.4719
_cell_volume                     2554.66(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -58.00   35.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000   60.0000 93

  2 omega -107.00  -14.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -46.0000 -110.0000 93

  3 omega   46.00   75.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -125.0000  -90.0000 29

  4 omega  -29.00   72.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -       40.6487  -77.0000  150.0000 101

  5 omega   38.00  110.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -147.0000 -178.0000 72

  6 omega   32.00   74.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -120.0000 42

  7 omega   45.00   72.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -90.0000 27

  8 omega   80.00  168.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  -90.0000 88

  9 omega   33.00   69.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   90.0000 36

 10 omega   43.00   77.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000    0.0000 34

 11 omega   83.00  129.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000   90.0000 46

 12 omega   87.00  178.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -180.0000 91

 13 omega   61.00  118.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -124.0000  -13.0000 57

 14 omega   81.00  107.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  147.0000  178.0000 26

 15 omega   37.00   77.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -180.0000 40

 16 omega  114.00  140.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000    0.0000 26

 17 omega  133.00  163.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  120.0000 30

 18 omega   42.00   68.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -30.0000 26

 19 omega   67.00  118.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -124.0000  -66.0000 51

 20 omega  138.00  167.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  147.0000  178.0000 29

 21 omega   44.00   70.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  150.0000 26

 22 omega   40.00   66.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000   90.0000 26

 23 omega  102.00  169.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000  120.0000 67

 24 omega   28.00  109.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -104.0000  107.0000 81

 25 omega -119.00   -7.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -77.0000 -180.0000 112

 26 omega -115.00  -59.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487 -147.0000 -178.0000 56

 27 omega -119.00   -7.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -77.0000   30.0000 112

 28 omega -117.00  -14.00   1.0000    2.4100
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000   60.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0107772000
_diffrn_orient_matrix_UB_12      0.0608267000
_diffrn_orient_matrix_UB_13      -0.0785099000
_diffrn_orient_matrix_UB_21      0.0147470000
_diffrn_orient_matrix_UB_22      -0.1045766000
_diffrn_orient_matrix_UB_23      -0.0387978000
_diffrn_orient_matrix_UB_31      -0.1372171000
_diffrn_orient_matrix_UB_32      0.0058084000
_diffrn_orient_matrix_UB_33      0.0072464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23048
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.95
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.525
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.5506
_exptl_crystal_size_mid          0.4490
_exptl_crystal_size_min          0.2986
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1283P)^2^+1.5053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                9128
_reflns_number_total             10023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201115s_si_002_11.cif
_cod_data_source_block           3acacPhF3
_cod_database_code               4326988
_chemical_oxdiff_formula         'Fe C38 H27 N6 O5 P S F6'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97