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_2022930
_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_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)2 (H2 O)2], 2C6 H4 N2'
_chemical_formula_moiety         'C14 H12 Fe N6 O2 S2, 2(C6 H4 N2)'
_chemical_formula_sum            'C26 H20 Fe N10 O2 S2'
_chemical_formula_weight         624.49
_chemical_name_systematic
;
Diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile
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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                84.7650(10)
_cell_angle_beta                 77.7870(10)
_cell_angle_gamma                70.8260(10)
_cell_formula_units_Z            1
_cell_length_a                   8.10650(10)
_cell_length_b                   8.28800(10)
_cell_length_c                   11.4347(2)
_cell_measurement_reflns_used    25131
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.6570
_cell_measurement_theta_min      3.9450
_cell_volume                     709.021(18)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_collection
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CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
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CrysAlisPro 1.171.42.100a (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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_computing_structure_refinement
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<i>SHELXL2016/6</i> (Sheldrick, 2015a)
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_computing_structure_solution
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<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 0.995
_diffrn_measured_fraction_theta_max 0.968
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0089
_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       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29397
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.346
_diffrn_reflns_theta_min         3.957
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72660
_exptl_absorpt_correction_type   multi-scan
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;
(CrysalisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.245
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2016)
;
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0302P)^2^+0.2457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                2999
_reflns_number_total             2999
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2022929--2022930.cif.'
_cod_database_code               2022930
_cod_database_fobs_code          2022930
_shelx_hkl_checksum              918
_shelx_res_checksum              22852