#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:14:00 +0200 (lun 06 de sep de 2021) $
#$Revision: 268895 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/08/7060833.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_7060833
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                 100.972(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3795(5)
_cell_length_b                   9.4118(7)
_cell_length_c                   12.4288(7)
_cell_measurement_reflns_used    6033
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      41.602
_cell_measurement_theta_min      4.466
_cell_volume                     1306.81(14)
_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 0.568
_diffrn_measured_fraction_theta_max 0.483
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.568
_diffrn_reflns_Laue_measured_fraction_max 0.483
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19633
_diffrn_reflns_point_group_measured_fraction_full 0.568
_diffrn_reflns_point_group_measured_fraction_max 0.483
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.605
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec Ag I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0839 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.8651.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.648
_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         0.297
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         1928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0369
_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)+(0.0600P)²+0.5084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1429
_reflns_number_total             1928
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj02607k2.cif
_cod_data_source_block           B_9kbar
_cod_depositor_comments
'Adding full bibliography for 7060820--7060846.cif.'
_cod_database_code               7060833
_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   0.960
_shelx_estimated_absorpt_t_min   0.908
_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 0.0236(2) Uani 1 2 d S T P . .
S1 S 0.47454(6) 0.71629(11) 0.13795(7) 0.0318(3) Uani 1 1 d . . . . .
N1 N 0.5056(2) 0.5967(4) 0.3468(2) 0.0349(9) Uani 1 1 d . . . . .
N2 N 0.54196(18) 0.7097(3) 0.5763(2) 0.0272(7) Uani 1 1 d . . . . .
N3 N 0.32954(17) 0.6023(3) 0.4883(2) 0.0261(7) Uani 1 1 d . . . . .
N4 N 0.21435(18) 0.5706(3) 0.4355(2) 0.0288(7) Uani 1 1 d . . . . .
N5 N 0.22511(17) 0.7963(3) 0.4860(2) 0.0228(7) Uani 1 1 d . . . . .
N6 N 0.1943(2) 0.9342(4) 0.5133(3) 0.0351(8) Uani 1 1 d . . . . .
H6A H 0.149(3) 0.924(5) 0.560(3) 0.042 Uiso 1 1 d R . . . .
H6B H 0.157(3) 0.987(5) 0.452(3) 0.042 Uiso 1 1 d R . . . .
N7 N -0.00573(19) 0.8352(3) 0.3476(2) 0.0308(8) Uani 1 1 d . . . . .
C1 C 0.4923(2) 0.6462(4) 0.2605(3) 0.0259(8) Uani 1 1 d . . . . .
C2 C 0.6509(2) 0.7560(4) 0.6235(3) 0.0335(10) Uani 1 1 d . . . . .
H2 H 0.715907 0.695456 0.625461 0.040 Uiso 1 1 calc R . . . .
C3 C 0.6710(2) 0.8896(5) 0.6693(3) 0.0363(11) Uani 1 1 d . . . . .
H3 H 0.747878 0.917497 0.702113 0.044 Uiso 1 1 calc R . . . .
C4 C 0.5762(2) 0.9806(4) 0.6658(3) 0.0361(10) Uani 1 1 d . . . . .
H4 H 0.587721 1.071239 0.695692 0.043 Uiso 1 1 calc R . . . .
C5 C 0.4621(2) 0.9345(4) 0.6165(3) 0.0297(9) Uani 1 1 d . . . . .
H5 H 0.396197 0.993781 0.613490 0.036 Uiso 1 1 calc R . . . .
C6 C 0.4486(2) 0.8009(4) 0.5728(2) 0.0236(8) Uani 1 1 d . . . . .
C7 C 0.3352(2) 0.7345(4) 0.5183(2) 0.0226(8) Uani 1 1 d . . . . .
C8 C 0.1536(2) 0.6878(4) 0.4354(2) 0.0244(8) Uani 1 1 d . . . . .
C9 C 0.0255(2) 0.7076(4) 0.3873(2) 0.0229(8) Uani 1 1 d . . . . .
C10 C -0.1218(2) 0.8563(4) 0.3063(3) 0.0368(9) Uani 1 1 d . . . . .
H10 H -0.145261 0.944275 0.275485 0.044 Uiso 1 1 calc R . . . .
C11 C -0.2082(2) 0.7542(5) 0.3070(3) 0.0369(11) Uani 1 1 d . . . . .
H11 H -0.288412 0.774585 0.280335 0.044 Uiso 1 1 calc R . . . .
C12 C -0.1744(3) 0.6224(5) 0.3475(3) 0.0397(11) Uani 1 1 d . . . . .
H12 H -0.231218 0.551786 0.349306 0.048 Uiso 1 1 calc R . . . .
C13 C -0.0538(2) 0.5957(4) 0.3858(3) 0.0322(9) Uani 1 1 d . . . . .
H13 H -0.027035 0.505662 0.409761 0.039 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 87.76(11) 3_666 3_666 ?
N1 Fe1 N2 92.24(11) 3_666 . ?
N1 Fe1 N2 92.24(11) . 3_666 ?
N1 Fe1 N2 87.76(11) . . ?
N1 Fe1 N3 94.15(10) 3_666 . ?
N1 Fe1 N3 85.85(10) 3_666 3_666 ?
N1 Fe1 N3 94.15(10) . 3_666 ?
N1 Fe1 N3 85.85(10) . . ?
N2 Fe1 N2 180.00(7) 3_666 . ?
N3 Fe1 N2 75.29(9) . . ?
N3 Fe1 N2 104.71(9) 3_666 . ?
N3 Fe1 N2 104.71(9) . 3_666 ?
N3 Fe1 N2 75.29(9) 3_666 3_666 ?
N3 Fe1 N3 180.00(14) . 3_666 ?
C1 N1 Fe1 170.9(2) . . ?
C2 N2 Fe1 125.9(2) . . ?
C2 N2 C6 117.5(3) . . ?
C6 N2 Fe1 116.61(18) . . ?
N4 N3 Fe1 134.3(2) . . ?
C7 N3 Fe1 114.62(17) . . ?
C7 N3 N4 109.5(2) . . ?
C8 N4 N3 105.8(3) . . ?
C7 N5 N6 125.4(3) . . ?
C7 N5 C8 104.2(3) . . ?
C8 N5 N6 130.0(2) . . ?
N5 N6 H6A 106(3) . . ?
N5 N6 H6B 113(3) . . ?
H6A N6 H6B 112(3) . . ?
C9 N7 C10 117.0(3) . . ?
N1 C1 S1 179.6(3) . . ?
N2 C2 H2 118.6 . . ?
N2 C2 C3 122.9(3) . . ?
C3 C2 H2 118.6 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(3) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.5 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
N2 C6 C5 122.7(2) . . ?
N2 C6 C7 110.9(3) . . ?
C5 C6 C7 126.4(3) . . ?
N3 C7 N5 109.3(2) . . ?
N3 C7 C6 121.9(2) . . ?
N5 C7 C6 128.7(3) . . ?
N4 C8 N5 111.1(2) . . ?
N4 C8 C9 126.2(3) . . ?
N5 C8 C9 122.7(3) . . ?
N7 C9 C8 116.1(3) . . ?
N7 C9 C13 124.0(3) . . ?
C13 C9 C8 120.0(3) . . ?
N7 C10 H10 118.4 . . ?
N7 C10 C11 123.3(3) . . ?
C11 C10 H10 118.4 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.0(3) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.8(3) . . ?
C13 C12 H12 120.6 . . ?
C9 C13 C12 117.8(3) . . ?
C9 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
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 2.123(3) 3_666 ?
Fe1 N1 2.123(3) . ?
Fe1 N2 2.203(3) . ?
Fe1 N2 2.203(3) 3_666 ?
Fe1 N3 2.146(2) . ?
Fe1 N3 2.146(2) 3_666 ?
S1 C1 1.637(3) . ?
N1 C1 1.152(4) . ?
N2 C2 1.339(3) . ?
N2 C6 1.359(4) . ?
N3 N4 1.382(3) . ?
N3 C7 1.297(4) . ?
N4 C8 1.301(4) . ?
N5 N6 1.402(4) . ?
N5 C7 1.370(3) . ?
N5 C8 1.381(4) . ?
N6 H6A 0.85(3) . ?
N6 H6B 0.94(4) . ?
N7 C9 1.321(5) . ?
N7 C10 1.338(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.372(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.395(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.367(5) . ?
C6 C7 1.478(4) . ?
C8 C9 1.479(3) . ?
C9 C13 1.384(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.376(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.366(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(4) . ?
C13 H13 0.9300 . ?
