Two Novel Iron(II) Materials Based on Dianionic N4O2 Schiff Bases: Structural Properties and Spin-Crossover Characteristics in the Series [Fe(3-X,5-NO2-sal-N(1,4,7,10)] (X = H, 3-MeO, 3-EtO)
Lionel Salmon; Azzedine Bousseksou; Bruno Donnadieu; Jean-Pierre Tuchagues; Inorganic Chemistry 44 (2005) 1763–1773; doi:10.1021/ic048387k

data_4300804
_publ_contact_author             'Pr Jean-Pierre Tuchagues'
_publ_contact_author_address
;

Laboratoire de Chimie de Coordination

UPR-CNRS 8241

205, route de Narbonne

31077 Toulouse cedex, France 

;
_publ_contact_author_email       tuchague@lcc-toulouse.fr
_publ_section_title
;

Two Novel Iron(II) Materials Based on Dianionic N4O2 Schiff Bases:

Structural Properties and Spin-Crossover Characteristics in the Series

[Fe(3-X,5-NO2-sal-N(1,4,7,10)] (X = H, 3-MeO, 3-EtO)

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1763
_journal_page_last               1773
_journal_paper_doi               10.1021/ic048387k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C22 H26 Fe N6 O8'
_chemical_formula_weight         558.34
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ab'
_symmetry_space_group_name_H-M   'P b n b'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4810(9)
_cell_length_b                   14.7704(14)
_cell_length_c                   18.769(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.1
_cell_volume                     2351.2(4)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97.1990, (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14163
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details
;

'DIFABS - Walker, N. & Stuart, D. (1983) 

Acta Cryst. A39, 158-166.

Farrugia, L. J., ORTEP3 for Windows, 

J. Appl. Crystallogr. 1997, 30, 565.'

;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.049
_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     191
_refine_ls_number_reflns         1879
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0415P)^2^+1.3697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                1556
_reflns_number_total             1879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048387ksi20041116_110205_2.cif
_cod_data_source_block           (1_160K)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C22 H26 Fe1 N6 O8'
_cod_database_code               4300804