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_4300806
_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            'C28 H38 Fe N6 O9'
_chemical_formula_weight         658.49
_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_creation_method           SHELXL-97
_cell_angle_alpha                84.18(4)
_cell_angle_beta                 70.53(5)
_cell_angle_gamma                88.95(5)
_cell_formula_units_Z            2
_cell_length_a                   10.265(4)
_cell_length_b                   10.861(4)
_cell_length_c                   14.181(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.2
_cell_volume                     1482.7(11)
_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 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.1815
_diffrn_reflns_av_sigmaI/netI    0.1616
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9204
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.470
_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    1.475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         3378
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2411
_reflns_number_gt                2331
_reflns_number_total             3378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048387ksi20041116_110205_1.cif
_cod_data_source_block           (2)
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1482.6(10)
_cod_database_code               4300806