Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
Müller-Meinhard, Asmus; Jess, Inke; Näther, Christian; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 1173–1178; doi:10.1107/S205698902300988X

data_2022948
_publ_section_title
;
 Synthesis, crystal structure and properties of
 chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
;
_journal_coeditor_code           NX2002
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1173
_journal_page_last               1178
_journal_paper_doi               10.1107/S205698902300988X
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Fe Cl (N C S) (C6 H4 N2)4]'
_chemical_formula_moiety         'C25 H16 Cl Fe N9 S'
_chemical_formula_sum            'C25 H16 Cl Fe N9 S'
_chemical_formula_weight         565.83
_chemical_name_systematic
;
Chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.79412(6)
_cell_length_b                   10.79412(6)
_cell_length_c                   11.15065(11)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6630
_cell_measurement_theta_min      5.6860
_cell_volume                     1299.196(16)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(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 0.999
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11711
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.863
_diffrn_reflns_theta_min         5.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.345
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 652 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.0059(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1411
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0384P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                1406
_reflns_number_total             1411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2002sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022948.cif.'
_cod_original_cell_volume        1299.20(2)
_cod_database_code               2022948
_cod_database_fobs_code          2022948
_shelx_hkl_checksum              13585
_shelx_res_checksum              59468