Syntheses, crystal structures and properties of tetrakis(3-methylpyridine-κ<i>N</i>)bis(isothiocyanato-κ<i>N</i>)manganese(II) and tetrakis(3-methylpyridine-κ<i>N</i>)bis(isothiocyanato-κ<i>N</i>)iron(II)
Ceglarska, Magdalena; Krebs, Christoph; Näther, Christian; Acta Crystallographica Section E 78 (2022) 755–760; doi:10.1107/S2056989022006491

data_2244120
_publ_section_title
;
 Syntheses, crystal structures and properties of
 tetrakis(3-methylpyridine-\k<i>N</i>)bis(isothiocyanato-\k<i>N</i>)manganese(II)
 and
 tetrakis(3-methylpyridine-\k<i>N</i>)bis(isothiocyanato-\k<i>N</i>)iron(II)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              755
_journal_page_last               760
_journal_paper_doi               10.1107/S2056989022006491
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Fe (N C S)2 (C6 H7 N)4]'
_chemical_formula_moiety         'C26 H28 Fe N6 S2'
_chemical_formula_sum            'C26 H28 Fe N6 S2'
_chemical_formula_weight         544.51
_chemical_name_systematic
Tetrakis(3-methylpyridine-\k<i>N</i>)bis(isothiocyanato-\k<i>N</i>)iron(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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            4
_cell_length_a                   17.37330(10)
_cell_length_b                   8.94119(5)
_cell_length_c                   17.24862(10)
_cell_measurement_reflns_used    17643
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.3300
_cell_measurement_theta_min      2.5960
_cell_volume                     2679.37(3)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_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      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 0.983
_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  0.0200
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22225
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.767
_diffrn_reflns_theta_min         5.092
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'intense colourless'
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.284
_refine_ls_extinction_coef       0.00049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016/6 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0401P)^2^+1.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                2804
_reflns_number_total             2875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8024sup1.cif
_cod_data_source_block           2
_cod_database_code               2244120
_shelx_hkl_checksum              89447
_shelx_res_checksum              21293
_cod_database_fobs_code 2244120