Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-κ<i>N</i>)bis(isothiocyanato-κ<i>N</i>)bis(methanol-κ<i>N</i>)iron(II)
Wellm, Carsten; Näther, Christian; Acta Crystallographica Section E 76 (2020) 276–280; doi:10.1107/S2056989020001152

data_2243263
_publ_section_title
;
 Crystal structure, synthesis and thermal properties of
 bis(4-benzoylpyridine-\k<i>N</i>)bis(isothiocyanato-\k<i>N</i>)bis(methanol-\k<i>N</i>)iron(II)
;
_journal_coeditor_code           LH5944
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              276
_journal_page_last               280
_journal_paper_doi               10.1107/S2056989020001152
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Fe (N C S)2 (C12 H9 N O)2 (C H4 O)2]'
_chemical_formula_sum            'C28 H26 Fe N4 O4 S2'
_chemical_formula_weight         602.50
_chemical_name_systematic
Bis(4-benzoylpyridine-\k<i>N</i>)bis(isothiocyanato-\k<i>N</i>)bis(methanol-\k<i>N</i>)iron(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.730(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1111(8)
_cell_length_b                   7.2385(3)
_cell_length_c                   16.1716(12)
_cell_measurement_reflns_used    19758
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.109
_cell_measurement_theta_min      2.528
_cell_volume                     1412.87(15)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19758
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.109
_diffrn_reflns_theta_min         2.528
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.8339
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.510
_refine_ls_extinction_coef       0.033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0694P)^2^+0.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                3012
_reflns_number_total             3422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5944sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243263
_cod_database_fobs_code          2243263
_shelx_hkl_checksum              1759
_shelx_res_checksum              80988
_shelxl_version_number           2.014