#------------------------------------------------------------------------------
#$Date: 2020-02-01 08:05:08 +0200 (Sat, 01 Feb 2020) $
#$Revision: 247438 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243263.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243263
loop_
_publ_author_name
'Wellm, Carsten'
'Näther, Christian'
_publ_section_title
;
 Crystal structure, synthesis and thermal properties of
 bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)bis(methanol-κN)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-κN)bis(isothiocyanato-κN)bis(methanol-κN)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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0694P)²+0.4300P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Fe Fe1 0.0000 0.0000 0.5000 0.02289(12) Uani d 1
N N1 -0.11410(12) 0.1948(2) 0.45147(10) 0.0371(3) Uani d 1
C C1 -0.19503(13) 0.2661(2) 0.42451(10) 0.0281(3) Uani d 1
S S1 -0.30854(4) 0.36594(7) 0.38796(3) 0.04332(15) Uani d 1
N N11 0.13430(11) 0.14836(18) 0.44116(8) 0.0258(3) Uani d 1
C C11 0.21746(13) 0.0529(2) 0.41200(10) 0.0277(3) Uani d 1
H H11 0.2228 -0.0756 0.4236 0.033 Uiso calc 1
C C12 0.29604(13) 0.1328(2) 0.36572(9) 0.0270(3) Uani d 1
H H12 0.3521 0.0594 0.3442 0.032 Uiso calc 1
C C13 0.29163(12) 0.3217(2) 0.35128(9) 0.0248(3) Uani d 1
C C14 0.20752(13) 0.4230(2) 0.38307(10) 0.0298(3) Uani d 1
H H14 0.2031 0.5529 0.3752 0.036 Uiso calc 1
C C15 0.13013(13) 0.3312(2) 0.42649(10) 0.0301(3) Uani d 1
H H15 0.0715 0.4006 0.4468 0.036 Uiso calc 1
C C16 0.37576(13) 0.4045(2) 0.29890(9) 0.0270(3) Uani d 1
C C17 0.43593(12) 0.5737(2) 0.32626(10) 0.0264(3) Uani d 1
C C18 0.49691(14) 0.6691(2) 0.27018(11) 0.0346(4) Uani d 1
H H18 0.4953 0.6297 0.2141 0.042 Uiso calc 1
C C19 0.55965(16) 0.8209(3) 0.29656(14) 0.0433(4) Uani d 1
H H19 0.6001 0.8871 0.2583 0.052 Uiso calc 1
C C20 0.56366(16) 0.8766(3) 0.37870(15) 0.0450(5) Uani d 1
H H20 0.6074 0.9802 0.3967 0.054 Uiso calc 1
C C21 0.50409(16) 0.7819(3) 0.43474(13) 0.0399(4) Uani d 1
H H21 0.5075 0.8202 0.4911 0.048 Uiso calc 1
C C22 0.43953(13) 0.6315(2) 0.40878(10) 0.0310(3) Uani d 1
H H22 0.3978 0.5679 0.4471 0.037 Uiso calc 1
O O11 0.39260(11) 0.32281(19) 0.23480(7) 0.0377(3) Uani d 1
C C23 0.1420(2) 0.2043(4) 0.64942(14) 0.0593(6) Uani d 1
H H23A 0.1367 0.2868 0.6970 0.089 Uiso calc 1
H H23B 0.1741 0.0861 0.6686 0.089 Uiso calc 1
H H23C 0.1892 0.2611 0.6101 0.089 Uiso calc 1
O O1 0.03337(11) 0.1736(2) 0.60921(7) 0.0384(3) Uani d 1
H H1 -0.0132 0.1745 0.6449 0.058 Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N1 3_556 . 180.00(8) y
N1 Fe1 O1 3_556 3_556 89.31(6) y
N1 Fe1 O1 . 3_556 90.69(6) y
N1 Fe1 O1 3_556 . 90.69(6) y
N1 Fe1 O1 . . 89.31(6) y
O1 Fe1 O1 3_556 . 180.00(4) y
N1 Fe1 N11 3_556 3_556 89.87(5) y
N1 Fe1 N11 . 3_556 90.13(5) y
O1 Fe1 N11 3_556 3_556 88.57(5) y
O1 Fe1 N11 . 3_556 91.43(5) y
N1 Fe1 N11 3_556 . 90.13(5) y
N1 Fe1 N11 . . 89.87(5) y
O1 Fe1 N11 3_556 . 91.43(5) y
O1 Fe1 N11 . . 88.57(5) y
N11 Fe1 N11 3_556 . 180.0 y
C1 N1 Fe1 . . 163.04(14) ?
N1 C1 S1 . . 179.32(16) ?
C11 N11 C15 . . 117.66(13) ?
C11 N11 Fe1 . . 119.92(10) ?
C15 N11 Fe1 . . 122.13(10) ?
N11 C11 C12 . . 123.04(15) ?
N11 C11 H11 . . 118.5 ?
C12 C11 H11 . . 118.5 ?
C11 C12 C13 . . 118.94(14) ?
C11 C12 H12 . . 120.5 ?
C13 C12 H12 . . 120.5 ?
C12 C13 C14 . . 118.52(13) ?
C12 C13 C16 . . 117.99(14) ?
C14 C13 C16 . . 123.44(14) ?
C15 C14 C13 . . 118.83(15) ?
C15 C14 H14 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
N11 C15 C14 . . 122.95(14) ?
N11 C15 H15 . . 118.5 ?
C14 C15 H15 . . 118.5 ?
O11 C16 C17 . . 122.83(14) ?
O11 C16 C13 . . 116.92(14) ?
C17 C16 C13 . . 120.23(13) ?
C22 C17 C18 . . 119.69(15) ?
C22 C17 C16 . . 120.78(14) ?
C18 C17 C16 . . 119.34(15) ?
C19 C18 C17 . . 119.90(17) ?
C19 C18 H18 . . 120.1 ?
C17 C18 H18 . . 120.1 ?
C18 C19 C20 . . 120.13(17) ?
C18 C19 H19 . . 119.9 ?
C20 C19 H19 . . 119.9 ?
C19 C20 C21 . . 120.28(17) ?
C19 C20 H20 . . 119.9 ?
C21 C20 H20 . . 119.9 ?
C22 C21 C20 . . 120.13(18) ?
C22 C21 H21 . . 119.9 ?
C20 C21 H21 . . 119.9 ?
C21 C22 C17 . . 119.86(16) ?
C21 C22 H22 . . 120.1 ?
C17 C22 H22 . . 120.1 ?
O1 C23 H23A . . 109.5 ?
O1 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
O1 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C23 O1 Fe1 . . 123.95(12) ?
C23 O1 H1 . . 109.2 ?
Fe1 O1 H1 . . 118.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 3_556 2.0823(15) y
Fe1 N1 . 2.0823(15) y
Fe1 O1 3_556 2.1780(12) y
Fe1 O1 . 2.1780(12) y
Fe1 N11 3_556 2.2270(12) y
Fe1 N11 . 2.2270(12) y
N1 C1 . 1.160(2) ?
C1 S1 . 1.6209(17) ?
N11 C11 . 1.339(2) ?
N11 C15 . 1.345(2) ?
C11 C12 . 1.385(2) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.388(2) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.388(2) ?
C13 C16 . 1.502(2) ?
C14 C15 . 1.386(2) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 O11 . 1.225(2) ?
C16 C17 . 1.474(2) ?
C17 C22 . 1.396(2) ?
C17 C18 . 1.398(2) ?
C18 C19 . 1.383(3) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.385(3) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.386(3) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.385(2) ?
C21 H21 . 0.9500 ?
C22 H22 . 0.9500 ?
C23 O1 . 1.436(3) ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
O1 H1 . 0.8401 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 O11 4_566 0.84 1.92 2.7574(16) 174.3

_cod_database_fobs_code 2243263
