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_7054503
_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_absolute_configuration unk
_chemical_formula_sum            'C28 H25 Fe N4 O2 S'
_chemical_formula_weight         537.45
_chemical_name_systematic
(isothiocyanato)-(N,N'-bis((2-oxido-1-naphthyl)methylene)-1,6-diamino-4-azahexane)-iron(iii)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5011(6)
_cell_length_b                   13.0676(10)
_cell_length_c                   24.704(3)
_cell_measurement_reflns_used    4554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.2245
_cell_measurement_theta_min      2.9264
_cell_volume                     2421.5(4)
_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  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.988
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8399
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.924
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.777
_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    1.474
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 1057 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                3084
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4nj01363h2.cif
_cod_data_source_block           2@100K
_cod_depositor_comments
'Adding full bibliography for 7054500--7054508.cif.'
_cod_database_code               7054503
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2014-3
_shelx_res_checksum              37808