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_4326310
_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         'C36 H42 Fe2 N16 O6, 4(N O3), 2(H2 O)'
_chemical_formula_sum            'C36 H46 Fe2 N20 O20'
_chemical_formula_weight         1190.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5604(10)
_cell_length_b                   14.6757(10)
_cell_length_c                   13.9671(10)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.870
_cell_measurement_theta_min      3.327
_cell_volume                     4826.2(5)
_computing_cell_refinement       DIRAX
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'EvalCCD and TWINABS'
_computing_molecular_graphics    PLATON
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4782
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4782
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+22.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                3900
_reflns_number_total             4782
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200332y_si_002_2.cif
_cod_data_source_block           s3241a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326310