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_4306566
_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 [Fe5b8MeOH)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         628.503
_chemical_name_common            Fe5bmeim3LS
_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               'P. Mayer'
_audit_block_code                Fe_L5b_N-Methylimidazole_3_mo116_weber
_audit_creation_date
;
'Wed Jul 23 14:35:28 2008'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             24-jule-08
_cell_angle_alpha                77.356(11)
_cell_angle_beta                 72.901(17)
_cell_angle_gamma                72.642(10)
_cell_formula_units_Z            2
_cell_length_a                   11.676(3)
_cell_length_b                   11.7660(14)
_cell_length_c                   11.8250(17)
_cell_measurement_reflns_used    7169
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      24.3981
_cell_measurement_theta_min      3.7509
_cell_volume                     1466.6(5)
_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      135(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_UB_11      0.0571122719
_diffrn_orient_matrix_UB_12      -0.0082819387
_diffrn_orient_matrix_UB_13      0.0143869816
_diffrn_orient_matrix_UB_21      -0.0209619539
_diffrn_orient_matrix_UB_22      0.0580252234
_diffrn_orient_matrix_UB_23      0.0182790845
_diffrn_orient_matrix_UB_31      -0.0247898938
_diffrn_orient_matrix_UB_32      -0.0256746658
_diffrn_orient_matrix_UB_33      0.0591917026
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13322
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         3.75
_diffrn_source_current           45
_diffrn_source_power             2.48
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_correction_T_min  0.8184
_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    1.4233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                2815
_reflns_number_total             3786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801388a_si_002_2.cif
_cod_data_source_block           mo116
_cod_database_code               4306566