Synthesis, crystal structure and properties of tetra-kis-(pyridine-3-carbo-nitrile)-dithio-cyanatoiron(II) and of diaqua-bis-(pyridine-3-carbo-nitrile)-di-thio-cyanatoiron(II) pyridine-3-carbo-nitrile monosolvate.
Näther, Christian; Müller-Meinhard, Asmus; Jess, Inke; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 1093–1099; doi:10.1107/S205698902300909X

data_2022929
_publ_section_title
;
 Synthesis, crystal structure and properties of
 tetra-kis-(pyridine-3-carbo-nitrile)-dithio-cyanatoiron(II) and of
 diaqua-bis-(pyridine-3-carbo-nitrile)-di-thio-cyanatoiron(II)
 pyridine-3-carbo-nitrile monosolvate.
;
_journal_coeditor_code           HB8079
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1093
_journal_page_last               1099
_journal_paper_doi               10.1107/S205698902300909X
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Fe (N C S)2 (C6 H4 N2)4]'
_chemical_formula_moiety         'C26 H16 Fe N10 S2'
_chemical_formula_sum            'C26 H16 Fe N10 S2'
_chemical_formula_weight         588.46
_chemical_name_systematic
;
Tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
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;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
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_cell_formula_units_Z            4
_cell_length_a                   20.3549(2)
_cell_length_b                   10.20840(10)
_cell_length_c                   13.03100(10)
_cell_measurement_reflns_used    22008
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.6930
_cell_measurement_theta_min      4.3390
_cell_volume                     2707.72(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_collection
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CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
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CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
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_computing_molecular_graphics
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DIAMOND (Brandenburg & Putz, 1999)
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;
Publcif (Westrip, 2010)
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<i>SHELXL2016/6</i> (Sheldrick, 2015a)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_min         4.344
_diffrn_source                   'micro-focus sealed X-ray tube'
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_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
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_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.293
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.7383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                5676
_reflns_number_total             5727
_reflns_threshold_expression     'I > 2\s(I)'
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'Adding full bibliography for 2022929--2022930.cif.'
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