Mono- and Dinuclear Iron Complexes of Bis(1-methylimidazol-2-yl)ketone (bik): Structure, Magnetic Properties, and Catalytic Oxidation Studies
Pieter C. A. Bruijnincx; Inge L. C. Buurmans; Yuxing Huang; Gergely Juhász; Marta Viciano-Chumillas; Manuel Quesada; Jan Reedijk; Martin Lutz; Anthony L. Spek; Eckard Münck; Emile L. Bominaar; Robertus J. M. Klein Gebbink; Inorganic Chemistry 50 (2011) 9243–9255; doi:10.1021/ic200332y

data_4326309
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Mono- and Dinuclear Iron Complexes of Bis(1-methylimidazol-2-yl)ketone
 (bik): Structure, Magnetic Properties, and Catalytic Oxidation Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9243
_journal_page_last               9255
_journal_paper_doi               10.1021/ic200332y
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C27 H30 Fe N12 O3, 2(C F3 O3 S), C H4 O'
_chemical_formula_sum            'C30 H34 F6 Fe N12 O10 S2'
_chemical_formula_weight         956.66
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.85847(1)
_cell_length_b                   50.00278(10)
_cell_length_c                   11.81363(2)
_cell_measurement_reflns_used    29582
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.94
_cell_volume                     15274.97(4)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            65769
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       plate
_exptl_crystal_F_000             7840
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         8742
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0293P)^2^+18.3550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                7881
_reflns_number_total             8742
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200332y_si_002_1.cif
_cod_data_source_block           s3561a
_cod_database_code               4326309