Fe^III^ in a low-spin state in caesium bis[3-ethoxysalicylaldehyde 4-methylthiosemicarbazonato(2‒)-κ^3^<i>O</i>^2^,<i>N</i>^1^,<i>S</i>]ferrate(III) methanol monosolvate
Powell, Robyn E.; Schwalbe, Carl H.; Tizzard, Graham J.; van Koningsbruggen, Petra J.; Acta Crystallographica Section C 70 (2014) 595–598; doi:10.1107/S2053229614008158

data_2019554
_publ_section_title
;
 Fe^III^ in a low-spin state in caesium bis[3-ethoxysalicylaldehyde
 4-methylthiosemicarbazonato(2--)-\k^3^<i>O</i>^2^,<i>N</i>^1^,<i>S</i>]ferrate(III)
 methanol monosolvate
;
_journal_coeditor_code           SF3227
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              595
_journal_page_last               598
_journal_paper_doi               10.1107/S2053229614008158
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Cs [Fe (C11 H13 N3 O2 S1)2], C H4 O'
_chemical_formula_moiety         'Cs +, C22 H26 Fe N6 O4 S2 -, C H4 O'
_chemical_formula_sum            'C23 H30 Cs Fe N6 O5 S2'
_chemical_formula_weight         723.40
_chemical_name_systematic
'Caesium bis{[2-(3-ethoxy-2-oxidobenzylidene)hydrazin-1-ylidene](methylamino)methanethiolato-\k^2^<i>O</i>^2^,<i>N</i>^1^,<i>S</i>}ferrate(III) methanol monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                100.629(5)
_cell_angle_beta                 91.549(5)
_cell_angle_gamma                113.674(5)
_cell_formula_units_Z            2
_cell_length_a                   8.486(3)
_cell_length_b                   9.078(3)
_cell_length_c                   19.875(7)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     1369.5(8)
_computing_cell_refinement       'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_data_collection       'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert (Rigaku, 2013)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007; Palatinus & van der Lee,
2008;
Palatinus <i>et al.</i>, 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 four-circle \k diffractometer'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15188
_diffrn_reflns_theta_full        25.0692
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.503
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear-SM Expert; Rigaku, 2013)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       plate
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.844
_refine_diff_density_min         -0.617
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                3414
_reflns_number_total             4844
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3227sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019554.cif.'
_cod_original_formula_sum        'C23 H30 Cs1 Fe1 N6 O5 S2'
_cod_database_code               2019554
_cod_database_fobs_code          2019554
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.980
_shelx_hkl_checksum              48058
_shelx_res_checksum              90137