Caesium bis(5-bromosalicylaldehyde thiosemicarbazonato-κ3O,N,S)ferrate(III): supramolecular arrangement of low-spin FeIIIcomplex anions mediated by Cs+cations
Powell, Robyn Elizabeth; Schwalbe, Carl H.; Tizzard, Graham J.; Koningsbruggen, Petra J. van; Acta Crystallographica Section C Structural Chemistry 71 (2015) –; doi:10.1107/S2053229615001928

data_2019840
_publ_section_title
;
 Caesium bis(5-bromosalicylaldehyde
 thiosemicarbazonato-\k3O,N,S)ferrate(III): supramolecular arrangement of
 low-spin FeIIIcomplex anions mediated by Cs+cations
;
_journal_coeditor_code           KY3069
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229615001928
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'Cs [Fe (C8 H6 Br1 N3 O1 S1)2]'
_chemical_formula_moiety         'Cs +, C16 H12 Br2 Fe N6 O2 S2 -'
_chemical_formula_sum            'C16 H12 Br2 Cs Fe N6 O2 S2'
_chemical_formula_weight         733.02
_chemical_name_systematic
'Caesium bis(5-bromosalicylaldehyde thiosemicarbazonato-\k^3^<i>O</i>,<i>N</i>,<i>S</i>)ferrate(III)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2500(14)
_cell_length_b                   12.0868(8)
_cell_length_c                   9.0389(5)
_cell_measurement_reflns_used    26513
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2212.3(2)
_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 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
ROTAX (Cooper <i>et al.</i>,  2002), SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC12 four-circle Kappa'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29088
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    6.131
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.6398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrystalClear-SM Expert</i>; Rigaku, 2013)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.852
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0451P)^2^+1.5804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                4211
_reflns_number_total             5073
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ky3069sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019840
_cod_database_fobs_code          2019840