Cooperative Iron(II) Spin Crossover Complexes with N4O2 Coordination Sphere
Birgit Weber; Eike Kaps; Jan Weigand; Chiara Carbonera; Jean-François Létard; Klaus Achterhold; Fritz G. Parak; Inorganic Chemistry 47 (2008) 487–496; doi:10.1021/ic070067o

data_4303949
_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
;
Cooperative Iron(II) Spin Crossover Complexes with N4O2 Coordination Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              487
_journal_page_last               496
_journal_paper_doi               10.1021/ic070067o
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source
;
iron acetate and ligand L heated to reflux in pyridine
;
_chemical_formula_moiety         'C18 H18 Fe N2 O4, 2(C5 H5 N)'
_chemical_formula_sum            'C28 H28 Fe N4 O4'
_chemical_formula_weight         540.391
_chemical_name_common            1
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                fe_L_py_2_HS
_audit_creation_date             27-Nov-03
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_audit_update_record             27-Oct-04
_cell_angle_alpha                90.00
_cell_angle_beta                 103.201(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9950(8)
_cell_length_b                   8.8100(5)
_cell_length_c                   24.9490(15)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.2
_cell_volume                     2566.8(3)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_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_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_orient_matrix_type
;first index: i in a~i~^*^, second: diffractometer xyz
 e.g. UB_21,UB_22,UB_23 are the xyz components of b^*^
;
_diffrn_orient_matrix_UB_11      0.020425
_diffrn_orient_matrix_UB_12      0.058298
_diffrn_orient_matrix_UB_13      0.059307
_diffrn_orient_matrix_UB_21      0.091667
_diffrn_orient_matrix_UB_22      0.029168
_diffrn_orient_matrix_UB_23      -0.060242
_diffrn_orient_matrix_UB_31      -0.019374
_diffrn_orient_matrix_UB_32      0.033894
_diffrn_orient_matrix_UB_33      -0.013070
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17760
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         2.13
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.9049
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.39840(16)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0405P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                3627
_reflns_number_total             4911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070067o-file001_2.cif
_cod_data_source_block           h149
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303949