#------------------------------------------------------------------------------
#$Date: 2021-09-06 15:14:00 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268895 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/08/7060826.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7060826
loop_
_publ_author_name
'Mason, Helen E.'
'Musselle-Sexton, Jake R. C.'
'Howard, Judith A. K.'
'Probert, Michael R.'
'Sparkes, Hazel A.'
_publ_section_title
;
 Structural studies into the spin crossover behaviour of Fe(abpt)2(NCS)2
 polymorphs B and D
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14014
_journal_page_last               14023
_journal_paper_doi               10.1039/D1NJ02607K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '2(C13 H10 Fe0.5 N7 S)'
_chemical_formula_sum            'C26 H20 Fe N14 S2'
_chemical_formula_weight         648.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.567(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7361(7)
_cell_length_b                   15.4827(17)
_cell_length_c                   16.6888(11)
_cell_measurement_reflns_used    7785
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.388
_cell_measurement_theta_min      2.603
_cell_volume                     2644.7(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.576
_diffrn_measured_fraction_theta_max 0.576
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.576
_diffrn_reflns_Laue_measured_fraction_max 0.576
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23039
_diffrn_reflns_point_group_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.576
_diffrn_reflns_theta_full        19.524
_diffrn_reflns_theta_max         19.524
_diffrn_reflns_theta_min         1.448
_diffrn_source                   'microfocus sealed X-ray tube Ag'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms Ag'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.6147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.8258.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0467
_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)+(0.0367P)²+7.6101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2123
_reflns_number_total             2697
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj02607k2.cif
_cod_data_source_block           polyd_7_5kbar
_cod_depositor_comments
'Adding full bibliography for 7060820--7060846.cif.'
_cod_database_code               7060826
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C25(H25), C26(H26), C13(H13), C12(H12), C10(H10), C11(H11)
;
_olex2_exptl_crystal_mounting_method
'Crystal was mounted within a diamond anvil cell'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.000000 0.500000 0.000000 0.0232(3) Uani 1 2 d S TU P . .
Fe2 Fe 0.000000 0.500000 0.500000 0.0215(3) Uani 1 2 d S TU P . .
S1 S -0.17432(13) 0.43197(12) 0.22675(10) 0.0380(5) Uani 1 1 d . U . . .
N1 N -0.0437(4) 0.4634(4) 0.1097(3) 0.0368(15) Uani 1 1 d . U . . .
N2 N 0.1313(4) 0.5998(4) 0.0702(3) 0.0265(13) Uani 1 1 d . U . . .
N3 N 0.1871(4) 0.4391(4) 0.0389(3) 0.0281(13) Uani 1 1 d . U . . .
N4 N 0.2352(4) 0.3631(4) 0.0206(3) 0.0350(15) Uani 1 1 d . U . . .
N5 N 0.3982(3) 0.4510(4) 0.0791(3) 0.0274(12) Uani 1 1 d . U . . .
N6 N 0.5249(4) 0.4879(4) 0.1142(4) 0.0435(17) Uani 1 1 d . U . . .
H6A H 0.547(5) 0.474(5) 0.177(4) 0.052 Uiso 1 1 d R . . . .
H6B H 0.579(6) 0.454(5) 0.094(4) 0.052 Uiso 1 1 d R . . . .
N8 N 0.1811(4) 0.5238(4) 0.5716(3) 0.0323(14) Uani 1 1 d . U . . .
N9 N 0.0069(4) 0.6035(4) 0.4271(3) 0.0262(13) Uani 1 1 d . U . . .
N10 N 0.0787(4) 0.4447(4) 0.4178(3) 0.0259(13) Uani 1 1 d . U . . .
N11 N 0.1238(4) 0.3651(4) 0.4050(3) 0.0295(13) Uani 1 1 d . U . . .
N12 N 0.1734(4) 0.4585(4) 0.3205(3) 0.0260(12) Uani 1 1 d . U . . .
N13 N 0.2185(5) 0.5017(4) 0.2599(4) 0.0386(16) Uani 1 1 d . U . . .
H13A H 0.164(6) 0.494(5) 0.210(4) 0.046 Uiso 1 1 d R . . . .
H13B H 0.288(6) 0.484(5) 0.260(4) 0.046 Uiso 1 1 d R . . . .
N14 N 0.3030(4) 0.3267(4) 0.2566(3) 0.0345(15) Uani 1 1 d . U . . .
C1 C -0.0997(4) 0.4500(4) 0.1578(3) 0.0251(15) Uani 1 1 d . U . . .
C2 C 0.0963(5) 0.6775(5) 0.0904(4) 0.0324(16) Uani 1 1 d . U . . .
H2 H 0.007747 0.691041 0.074085 0.039 Uiso 1 1 calc R . . . .
C3 C 0.1827(5) 0.7385(5) 0.1335(4) 0.0420(18) Uani 1 1 d . U . . .
H3 H 0.153995 0.792502 0.144860 0.050 Uiso 1 1 calc R . . . .
C4 C 0.3139(6) 0.7176(6) 0.1598(5) 0.053(2) Uani 1 1 d . U . . .
H4 H 0.375073 0.757004 0.190655 0.063 Uiso 1 1 calc R . . . .
C5 C 0.3527(5) 0.6391(6) 0.1404(4) 0.047(2) Uani 1 1 d . U . . .
H5 H 0.441012 0.625032 0.156460 0.057 Uiso 1 1 calc R . . . .
C6 C 0.2605(4) 0.5798(4) 0.0964(3) 0.0263(14) Uani 1 1 d . U . . .
C7 C 0.2846(4) 0.4934(4) 0.0727(3) 0.0241(14) Uani 1 1 d . U . . .
C8 C 0.3643(4) 0.3717(5) 0.0467(3) 0.0269(14) Uani 1 1 d . U . . .
C14 C 0.2874(5) 0.5313(4) 0.6122(4) 0.0309(16) Uani 1 1 d . U . . .
C15 C -0.0404(5) 0.6811(5) 0.4325(4) 0.0309(16) Uani 1 1 d . U . . .
H15 H -0.084114 0.690586 0.472064 0.037 Uiso 1 1 calc R . . . .
C16 C -0.0279(5) 0.7487(5) 0.3819(4) 0.0330(16) Uani 1 1 d . U . . .
H16 H -0.061079 0.802960 0.387960 0.040 Uiso 1 1 calc R . . . .
C17 C 0.0340(5) 0.7347(5) 0.3226(4) 0.0373(18) Uani 1 1 d . U . . .
H17 H 0.043598 0.779693 0.288018 0.045 Uiso 1 1 calc R . . . .
C18 C 0.0815(5) 0.6551(5) 0.3139(4) 0.0329(17) Uani 1 1 d . U . . .
H18 H 0.123179 0.645071 0.273366 0.040 Uiso 1 1 calc R . . . .
C19 C 0.0669(4) 0.5884(5) 0.3670(4) 0.0276(15) Uani 1 1 d . U . . .
C20 C 0.1087(4) 0.5025(5) 0.3676(3) 0.0250(14) Uani 1 1 d . U . . .
C21 C 0.1812(5) 0.3757(5) 0.3453(4) 0.0268(14) Uani 1 1 d . U . . .
C22 C 0.2391(4) 0.3040(5) 0.3106(4) 0.0258(15) Uani 1 1 d . U . . .
C23 C 0.3515(6) 0.2600(6) 0.2231(4) 0.046(2) Uani 1 1 d . U . . .
H23 H 0.398356 0.273046 0.186052 0.055 Uiso 1 1 calc R . . . .
C24 C 0.3371(6) 0.1766(6) 0.2393(4) 0.049(2) Uani 1 1 d . U . . .
H24 H 0.369361 0.133658 0.211991 0.059 Uiso 1 1 calc R . . . .
C25 C 0.2737(5) 0.1555(6) 0.2971(4) 0.0454(19) Uani 1 1 d . U . . .
H25 H 0.264114 0.098203 0.310948 0.054 Uiso 1 1 calc R . . . .
C26 C 0.2249(5) 0.2216(5) 0.3338(4) 0.0354(17) Uani 1 1 d . U . . .
H26 H 0.182794 0.210008 0.373783 0.043 Uiso 1 1 calc R . . . .
N7 N 0.5752(4) 0.3267(4) 0.0433(3) 0.0433(16) Uani 1 1 d . U . . .
C9 C 0.4537(5) 0.3020(5) 0.0388(4) 0.0325(15) Uani 1 1 d . U . . .
C13 C 0.4123(6) 0.2176(6) 0.0296(4) 0.0455(18) Uani 1 1 d . U . . .
H13 H 0.327760 0.203378 0.028751 0.055 Uiso 1 1 calc R . . . .
C12 C 0.4981(7) 0.1546(7) 0.0216(5) 0.062(2) Uani 1 1 d . U . . .
H12 H 0.472042 0.097133 0.013495 0.074 Uiso 1 1 calc R . . . .
C10 C 0.6572(6) 0.2627(7) 0.0373(5) 0.058(2) Uani 1 1 d . U . . .
H10 H 0.742815 0.277546 0.041279 0.070 Uiso 1 1 calc R . . . .
C11 C 0.6231(6) 0.1784(7) 0.0257(4) 0.062(2) Uani 1 1 d . U . . .
H11 H 0.683437 0.137274 0.020672 0.075 Uiso 1 1 calc R . . . .
S2A S 0.43932(13) 0.54652(15) 0.66929(11) 0.0542(6) Uani 1 1 d . U . A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2886 0.5448 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.0 3_565 . ?
N1 Fe1 N2 90.05(19) 3_565 3_565 ?
N1 Fe1 N2 89.95(19) . 3_565 ?
N1 Fe1 N2 89.95(19) 3_565 . ?
N1 Fe1 N2 90.05(19) . . ?
N1 Fe1 N3 86.98(19) 3_565 . ?
N1 Fe1 N3 93.02(19) 3_565 3_565 ?
N1 Fe1 N3 86.98(19) . 3_565 ?
N1 Fe1 N3 93.02(19) . . ?
N2 Fe1 N2 180.0 . 3_565 ?
N3 Fe1 N2 75.71(18) 3_565 3_565 ?
N3 Fe1 N2 75.71(18) . . ?
N3 Fe1 N2 104.29(18) . 3_565 ?
N3 Fe1 N2 104.29(18) 3_565 . ?
N3 Fe1 N3 180.0 . 3_565 ?
N8 Fe2 N8 180.0 3_566 . ?
N8 Fe2 N9 90.44(19) . . ?
N8 Fe2 N9 90.44(19) 3_566 3_566 ?
N8 Fe2 N9 89.56(19) . 3_566 ?
N8 Fe2 N9 89.56(19) 3_566 . ?
N8 Fe2 N10 92.70(18) 3_566 . ?
N8 Fe2 N10 92.70(18) . 3_566 ?
N8 Fe2 N10 87.30(19) . . ?
N8 Fe2 N10 87.30(18) 3_566 3_566 ?
N9 Fe2 N9 180.0(2) . 3_566 ?
N10 Fe2 N9 99.9(2) 3_566 . ?
N10 Fe2 N9 80.1(2) . . ?
N10 Fe2 N9 99.9(2) . 3_566 ?
N10 Fe2 N9 80.1(2) 3_566 3_566 ?
N10 Fe2 N10 180.00(16) . 3_566 ?
C1 N1 Fe1 162.2(4) . . ?
C2 N2 Fe1 126.1(4) . . ?
C2 N2 C6 117.5(5) . . ?
C6 N2 Fe1 116.4(4) . . ?
N4 N3 Fe1 134.6(4) . . ?
C7 N3 Fe1 113.5(4) . . ?
C7 N3 N4 109.9(4) . . ?
C8 N4 N3 105.7(6) . . ?
C7 N5 N6 124.1(5) . . ?
C8 N5 N6 129.6(4) . . ?
C8 N5 C7 106.3(4) . . ?
C14 N8 Fe2 175.0(5) . . ?
C15 N9 Fe2 126.5(4) . . ?
C15 N9 C19 118.8(5) . . ?
C19 N9 Fe2 114.6(4) . . ?
N11 N10 Fe2 137.2(4) . . ?
C20 N10 Fe2 112.1(5) . . ?
C20 N10 N11 110.1(5) . . ?
C21 N11 N10 105.8(5) . . ?
C20 N12 N13 121.0(6) . . ?
C21 N12 N13 131.9(5) . . ?
C21 N12 C20 107.0(5) . . ?
C22 N14 C23 114.7(8) . . ?
N1 C1 S1 178.5(5) . . ?
N2 C2 C3 123.9(5) . . ?
C2 C3 C4 118.1(7) . . ?
C5 C4 C3 119.5(7) . . ?
C4 C5 C6 119.9(6) . . ?
N2 C6 C5 121.1(6) . . ?
N2 C6 C7 111.9(5) . . ?
C5 C6 C7 127.0(5) . . ?
N3 C7 N5 107.6(5) . . ?
N3 C7 C6 121.4(4) . . ?
N5 C7 C6 131.1(5) . . ?
N4 C8 N5 110.6(5) . . ?
N4 C8 C9 122.7(7) . . ?
N5 C8 C9 126.7(5) . . ?
N8 C14 S2A 177.5(6) . . ?
N9 C15 C16 122.7(7) . . ?
C17 C16 C15 118.9(7) . . ?
C18 C17 C16 120.1(6) . . ?
C17 C18 C19 119.0(6) . . ?
N9 C19 C18 120.5(7) . . ?
N9 C19 C20 112.2(5) . . ?
C18 C19 C20 127.3(6) . . ?
N10 C20 N12 106.7(6) . . ?
N10 C20 C19 120.2(5) . . ?
N12 C20 C19 133.0(5) . . ?
N11 C21 N12 110.4(5) . . ?
N11 C21 C22 123.1(7) . . ?
N12 C21 C22 126.4(6) . . ?
N14 C22 C21 115.5(7) . . ?
N14 C22 C26 124.5(6) . . ?
C26 C22 C21 120.1(6) . . ?
C24 C23 N14 124.9(7) . . ?
C23 C24 C25 118.8(6) . . ?
C26 C25 C24 118.0(9) . . ?
C22 C26 C25 119.0(8) . . ?
C9 N7 C10 115.6(7) . . ?
N7 C9 C8 115.7(7) . . ?
N7 C9 C13 123.7(6) . . ?
C13 C9 C8 120.5(5) . . ?
C9 C13 C12 118.8(7) . . ?
C11 C12 C13 118.5(10) . . ?
N7 C10 C11 124.4(7) . . ?
C10 C11 C12 119.0(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.100(5) 3_565 ?
Fe1 N1 2.100(5) . ?
Fe1 N2 2.179(5) 3_565 ?
Fe1 N2 2.179(5) . ?
Fe1 N3 2.135(4) . ?
Fe1 N3 2.135(4) 3_565 ?
Fe2 N8 1.985(4) . ?
Fe2 N8 1.985(4) 3_566 ?
Fe2 N9 2.026(6) 3_566 ?
Fe2 N9 2.026(6) . ?
Fe2 N10 2.007(5) 3_566 ?
Fe2 N10 2.007(5) . ?
S1 C1 1.613(5) . ?
N1 C1 1.157(6) . ?
N2 C2 1.335(8) . ?
N2 C6 1.359(6) . ?
N3 N4 1.357(7) . ?
N3 C7 1.328(7) . ?
N4 C8 1.327(6) . ?
N5 N6 1.427(6) . ?
N5 C7 1.360(6) . ?
N5 C8 1.348(8) . ?
N8 C14 1.144(7) . ?
N9 C15 1.318(9) . ?
N9 C19 1.366(7) . ?
N10 N11 1.365(8) . ?
N10 C20 1.331(8) . ?
N11 C21 1.331(7) . ?
N12 N13 1.415(7) . ?
N12 C20 1.375(8) . ?
N12 C21 1.342(8) . ?
N14 C22 1.335(8) . ?
N14 C23 1.352(10) . ?
C2 C3 1.366(9) . ?
C3 C4 1.382(8) . ?
C4 C5 1.356(11) . ?
C5 C6 1.386(9) . ?
C6 C7 1.441(9) . ?
C8 C9 1.476(8) . ?
C14 S2A 1.638(6) . ?
C15 C16 1.376(9) . ?
C16 C17 1.366(9) . ?
C17 C18 1.357(10) . ?
C18 C19 1.400(9) . ?
C19 C20 1.403(9) . ?
C21 C22 1.473(9) . ?
C22 C26 1.354(10) . ?
C23 C24 1.337(11) . ?
C24 C25 1.378(10) . ?
C25 C26 1.375(11) . ?
N7 C9 1.339(7) . ?
N7 C10 1.350(9) . ?
C9 C13 1.373(10) . ?
C13 C12 1.377(10) . ?
C12 C11 1.373(11) . ?
C10 C11 1.354(12) . ?
