Synthesis and Characterization of a Dinuclear Iron(II) Spin Crossover Complex with Wide Hysteresis
Birgit Weber; Eike S. Kaps; Jaroslava Obel; Klaus Achterhold; Fritz G. Parak; Inorganic Chemistry 47 (2008) 10779–10787; doi:10.1021/ic801388a

data_4306565
_publ_contact_author_address
;
Department Chemie und Biochemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus F)
D-81377 M\"unchen
Germany
;
_publ_contact_author_email       bwmch@cup.uni-muenchen.de
_publ_contact_author_fax         '+49 89 218077407'
_publ_contact_author_name        'Birgit Weber'
_publ_contact_author_phone       '+49 89 218077772'
_publ_section_title
;
Synthesis and Characterization of a Dinuclear Iron(II) Spin Crossover
Complex with Wide Hysteresis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10779
_journal_page_last               10787
_journal_paper_doi               10.1021/ic801388a
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source
;
The complex [Fe5b(MeOH)2] was dissolved in hot N-methylimidazole. After
cooling black crystals were obtained. 
;
_chemical_formula_moiety         'C26 H30 Fe N6 O4, C4 H6 N2'
_chemical_formula_sum            'C30 H36 Fe N8 O4'
_chemical_formula_weight         628.52
_chemical_name_common            Fe5bmeim3HS
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_author_name               'Weber, B.'
_audit_block_code                Fe_L5b_N-Methylimidazole_3_mo115_weber
_audit_creation_date
;
'Mon May 19 14:19:17 2008'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             30-june-08
_cell_angle_alpha                73.24(3)
_cell_angle_beta                 78.177(17)
_cell_angle_gamma                73.33(3)
_cell_formula_units_Z            2
_cell_length_a                   11.781(3)
_cell_length_b                   11.905(5)
_cell_length_c                   11.951(2)
_cell_measurement_reflns_used    4730
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.9975
_cell_measurement_theta_min      3.7956
_cell_volume                     1523.8(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics
;
ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
Plot Program for Crystal Structure Illustrations, Oak Ridge National
Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
Germany, 1995).
;
_computing_publication_material
;
PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
--- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_UB_11      0.0148394742
_diffrn_orient_matrix_UB_12      0.0556275098
_diffrn_orient_matrix_UB_13      -0.0074329894
_diffrn_orient_matrix_UB_21      0.0185725403
_diffrn_orient_matrix_UB_22      -0.0207290330
_diffrn_orient_matrix_UB_23      0.0568143101
_diffrn_orient_matrix_UB_31      0.0587869571
_diffrn_orient_matrix_UB_32      -0.0243044061
_diffrn_orient_matrix_UB_33      -0.0250593625
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10195
_diffrn_reflns_theta_full        24.9975
_diffrn_reflns_theta_max         24.9975
_diffrn_reflns_theta_min         3.80
_diffrn_source_current           45
_diffrn_source_power             2.48
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.8631
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.3697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                3558
_reflns_number_total             5226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801388a_si_002_1.cif
_cod_data_source_block           mo115
_cod_database_code               4306565