#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:14:00 +0200 (lun 06 de sep de 2021) $
#$Revision: 268895 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/08/7060823.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_7060823
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         'C26 H20 Fe N14 S2'
_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 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-07-12
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.984(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3439(6)
_cell_length_b                   9.3494(9)
_cell_length_c                   12.3371(9)
_cell_measurement_reflns_used    5469
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.000
_cell_measurement_theta_min      2.244
_cell_volume                     1284.49(17)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.587
_diffrn_measured_fraction_theta_max 0.487
_diffrn_measurement_device       'Xiphos II 4-circle 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  0.0512
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.587
_diffrn_reflns_Laue_measured_fraction_max 0.487
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17152
_diffrn_reflns_point_group_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.487
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.673
_diffrn_reflns_theta_min         2.139
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec Ag I\ms'
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8658.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0362
_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)+(0.0372P)²+0.6967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1439
_reflns_number_total             1924
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj02607k2.cif
_cod_data_source_block           B_11_5kbar
_cod_depositor_comments
'Adding full bibliography for 7060820--7060846.cif.'
_cod_database_code               7060823
_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.
;
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_exptl_crystal_mounting_method
'Crystal was mounted inside a Diamond Anvil Cell'
_olex2_submission_special_instructions 'No special instructions were received'
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_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 0.500000 0.500000 0.500000 0.02189(17) Uani 1 2 d S T P . .
S1 S 0.47478(6) 0.71735(10) 0.13652(6) 0.0309(2) Uani 1 1 d . . . . .
N1 N 0.5055(2) 0.5983(3) 0.3473(2) 0.0319(7) Uani 1 1 d . . . . .
N2 N 0.54297(17) 0.7086(3) 0.57739(19) 0.0263(6) Uani 1 1 d . . . . .
N3 N 0.33052(17) 0.6008(3) 0.48870(19) 0.0260(6) Uani 1 1 d . . . . .
N4 N 0.21499(17) 0.5696(3) 0.43522(19) 0.0270(6) Uani 1 1 d . . . . .
N5 N 0.22585(17) 0.7964(3) 0.48622(18) 0.0223(6) Uani 1 1 d . . . . .
N6 N 0.1955(2) 0.9357(4) 0.5138(3) 0.0334(7) Uani 1 1 d . . . . .
H6A H 0.147(3) 0.926(4) 0.557(3) 0.040 Uiso 1 1 d R . . . .
H6B H 0.160(3) 0.983(4) 0.455(3) 0.040 Uiso 1 1 d R . . . .
N7 N -0.00521(19) 0.8366(3) 0.3460(2) 0.0294(7) Uani 1 1 d . . . . .
C1 C 0.4923(2) 0.6477(4) 0.2600(2) 0.0252(7) Uani 1 1 d . . . . .
C2 C 0.6530(2) 0.7545(4) 0.6243(2) 0.0306(8) Uani 1 1 d . . . . .
H2 H 0.717963 0.693135 0.626713 0.037 Uiso 1 1 calc R . . . .
C3 C 0.6730(2) 0.8898(4) 0.6692(2) 0.0351(9) Uani 1 1 d . . . . .
H3 H 0.750266 0.918196 0.701557 0.042 Uiso 1 1 calc R . . . .
C4 C 0.5787(2) 0.9815(4) 0.6656(2) 0.0351(8) Uani 1 1 d . . . . .
H4 H 0.591048 1.072779 0.695656 0.042 Uiso 1 1 calc R . . . .
C5 C 0.4639(2) 0.9368(4) 0.6166(2) 0.0297(7) Uani 1 1 d . . . . .
H5 H 0.398266 0.997429 0.612894 0.036 Uiso 1 1 calc R . . . .
C6 C 0.4500(2) 0.8010(3) 0.5737(2) 0.0226(7) Uani 1 1 d . . . . .
C7 C 0.3358(2) 0.7349(3) 0.5188(2) 0.0225(7) Uani 1 1 d . . . . .
C8 C 0.1540(2) 0.6885(3) 0.4349(2) 0.0231(7) Uani 1 1 d . . . . .
C9 C 0.0253(2) 0.7075(3) 0.3866(2) 0.0226(7) Uani 1 1 d . . . . .
C10 C -0.1221(2) 0.8580(4) 0.3057(2) 0.0349(8) Uani 1 1 d . . . . .
H10 H -0.145761 0.947069 0.275703 0.042 Uiso 1 1 calc R . . . .
C11 C -0.2086(2) 0.7560(4) 0.3063(3) 0.0357(9) Uani 1 1 d . . . . .
H11 H -0.288962 0.776722 0.278906 0.043 Uiso 1 1 calc R . . . .
C12 C -0.1754(2) 0.6236(4) 0.3475(3) 0.0390(9) Uani 1 1 d . . . . .
H12 H -0.232815 0.553370 0.350244 0.047 Uiso 1 1 calc R . . . .
C13 C -0.0539(2) 0.5951(4) 0.3855(2) 0.0317(8) Uani 1 1 d . . . . .
H13 H -0.027325 0.504201 0.409085 0.038 Uiso 1 1 calc R . . . .
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'
Fe Fe 0.2886 0.5448 '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'
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_666 ?
N1 Fe1 N2 87.66(10) 3_666 3_666 ?
N1 Fe1 N2 92.34(10) . 3_666 ?
N1 Fe1 N2 92.34(10) 3_666 . ?
N1 Fe1 N2 87.66(10) . . ?
N1 Fe1 N3 94.11(9) . 3_666 ?
N1 Fe1 N3 94.11(9) 3_666 . ?
N1 Fe1 N3 85.89(9) 3_666 3_666 ?
N1 Fe1 N3 85.89(9) . . ?
N2 Fe1 N2 180.00(6) 3_666 . ?
N3 Fe1 N2 75.90(9) 3_666 3_666 ?
N3 Fe1 N2 104.10(9) 3_666 . ?
N3 Fe1 N2 104.10(9) . 3_666 ?
N3 Fe1 N2 75.90(9) . . ?
N3 Fe1 N3 180.00(12) 3_666 . ?
C1 N1 Fe1 170.8(2) . . ?
C2 N2 Fe1 125.8(2) . . ?
C2 N2 C6 117.6(3) . . ?
C6 N2 Fe1 116.50(16) . . ?
N4 N3 Fe1 134.7(2) . . ?
C7 N3 Fe1 114.57(16) . . ?
C7 N3 N4 109.1(2) . . ?
C8 N4 N3 105.9(2) . . ?
C7 N5 N6 124.9(2) . . ?
C7 N5 C8 104.8(3) . . ?
C8 N5 N6 129.9(2) . . ?
N5 N6 H6A 106(3) . . ?
N5 N6 H6B 111(3) . . ?
H6A N6 H6B 109(3) . . ?
C9 N7 C10 116.4(3) . . ?
N1 C1 S1 179.5(3) . . ?
N2 C2 H2 118.9 . . ?
N2 C2 C3 122.2(3) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 123.0(2) . . ?
N2 C6 C7 110.9(3) . . ?
C5 C6 C7 126.1(3) . . ?
N3 C7 N5 109.3(2) . . ?
N3 C7 C6 121.4(2) . . ?
N5 C7 C6 129.2(3) . . ?
N4 C8 N5 110.9(2) . . ?
N4 C8 C9 125.7(3) . . ?
N5 C8 C9 123.4(3) . . ?
N7 C9 C8 115.3(3) . . ?
N7 C9 C13 124.5(2) . . ?
C13 C9 C8 120.2(3) . . ?
N7 C10 H10 118.2 . . ?
N7 C10 C11 123.6(3) . . ?
C11 C10 H10 118.2 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.1(3) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C13 118.9(3) . . ?
C13 C12 H12 120.5 . . ?
C9 C13 C12 117.3(3) . . ?
C9 C13 H13 121.4 . . ?
C12 C13 H13 121.4 . . ?
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 2.107(3) . ?
Fe1 N1 2.107(3) 3_666 ?
Fe1 N2 2.185(3) . ?
Fe1 N2 2.185(3) 3_666 ?
Fe1 N3 2.122(2) 3_666 ?
Fe1 N3 2.122(2) . ?
S1 C1 1.634(3) . ?
N1 C1 1.155(4) . ?
N2 C2 1.342(3) . ?
N2 C6 1.357(3) . ?
N3 N4 1.381(3) . ?
N3 C7 1.306(4) . ?
N4 C8 1.309(4) . ?
N5 N6 1.406(4) . ?
N5 C7 1.362(3) . ?
N5 C8 1.373(4) . ?
N6 H6A 0.84(3) . ?
N6 H6B 0.88(3) . ?
N7 C9 1.327(4) . ?
N7 C10 1.339(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.382(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.365(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.373(4) . ?
C6 C7 1.478(3) . ?
C8 C9 1.479(3) . ?
C9 C13 1.381(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.370(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.364(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(4) . ?
C13 H13 0.9300 . ?
