Spin crossover and high spin electroneutral mononuclear iron(iii) Schiff base complexes involving terminal pseudohalido ligands
Masárová, Petra; Zoufalý, Pavel; Moncol, Ján; Nemec, Ivan; Pavlik, Ján; Gembický, Milan; Trávníček, Zdeněk; Boča, Roman; Šalitroš, Ivan; New J. Chem. 39 (2015) 508–; doi:10.1039/C4NJ01363H

data_7054505
_publ_section_title
;
 Spin crossover and high spin electroneutral mononuclear iron(iii) Schiff
 base complexes involving terminal pseudohalido ligands
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              508
_journal_paper_doi               10.1039/C4NJ01363H
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C20 H19 Fe N6 O6 S'
_chemical_formula_weight         527.32
_chemical_name_systematic
(isothiocyanato)-(N,N'-bis(5-nitro-2-oxido-benzylidene)-1,6-diamino-4-azahexane)-iron(iii)
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   15.9030(5)
_cell_length_b                   14.2180(5)
_cell_length_c                   19.6342(5)
_cell_measurement_reflns_used    17074
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.2587
_cell_measurement_theta_min      2.9234
_cell_volume                     4439.5(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40122
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.8794
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0443P)^2^+3.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                3038
_reflns_number_total             3907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01363h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7054500--7054508.cif.'
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7054505