#------------------------------------------------------------------------------
#$Date: 2016-04-05 21:27:14 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181752 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/52/7055284.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_7055284
loop_
_publ_author_name
'Mason, Helen E.'
'Li, Wei'
'Carpenter, Michael A.'
'Hamilton, Michelle L.'
'Howard, Judith A. K.'
'Sparkes, Hazel A.'
_publ_section_title
;
 Structural and spectroscopic characterisation of the spin crossover in
 [Fe(abpt)2(NCS)2] polymorph A
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2466
_journal_paper_doi               10.1039/C5NJ02359A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C26 H20 Fe N14 S2'
_chemical_formula_sum            'C26 H20 Fe N14 S2'
_chemical_formula_weight         648.53
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3913(4)
_cell_length_b                   10.0025(5)
_cell_length_c                   16.2339(8)
_cell_measurement_reflns_used    4455
_cell_measurement_temperature    165
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.39
_cell_volume                     1360.29(12)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      165
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9138
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G. Sheldrick, 1998)'
_exptl_crystal_colour            reddish
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.6067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                2660
_reflns_number_total             3374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02359a2.cif
_cod_data_source_block           165k
_cod_depositor_comments
'Adding full bibliography for 7055281--7055291.cif.'
_cod_database_code               7055284
_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)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.5000 0.5000 0.5000 0.01745(9) Uani 1 2 d S
S1 S 0.26449(6) 0.71416(5) 0.26122(3) 0.03202(13) Uani 1 1 d .
N1 N 0.39981(17) 0.57055(14) 0.39666(9) 0.0227(3) Uani 1 1 d .
N2 N 0.71060(17) 0.58347(14) 0.47344(9) 0.0224(3) Uani 1 1 d .
N3 N 0.47653(17) 0.67900(14) 0.54839(9) 0.0217(3) Uani 1 1 d .
N4 N 0.35606(17) 0.74994(14) 0.58036(9) 0.0218(3) Uani 1 1 d .
N5 N 0.57022(17) 0.87659(14) 0.58029(9) 0.0215(3) Uani 1 1 d .
N6 N 0.68232(19) 0.98254(16) 0.59362(11) 0.0281(3) Uani 1 1 d .
H6A H 0.625(3) 1.053(2) 0.6071(13) 0.034 Uiso 1 1 d .
H6B H 0.736(3) 0.962(2) 0.6442(14) 0.034 Uiso 1 1 d .
N7 N 0.39286(18) 1.09413(14) 0.64648(9) 0.0253(3) Uani 1 1 d .
C1 C 0.34307(19) 0.62882(17) 0.34044(11) 0.0215(3) Uani 1 1 d .
C2 C 0.8207(2) 0.52947(18) 0.42713(11) 0.0261(4) Uani 1 1 d .
H2 H 0.7988 0.4456 0.4015 0.031 Uiso 1 1 calc R
C3 C 0.9656(2) 0.5913(2) 0.41508(12) 0.0303(4) Uani 1 1 d .
H3 H 1.0401 0.5509 0.3809 0.036 Uiso 1 1 calc R
C4 C 1.0005(2) 0.7116(2) 0.45310(12) 0.0314(4) Uani 1 1 d .
H4 H 1.1006 0.7538 0.4469 0.038 Uiso 1 1 calc R
C5 C 0.8872(2) 0.7707(2) 0.50075(11) 0.0280(4) Uani 1 1 d .
H5 H 0.9081 0.8537 0.5277 0.034 Uiso 1 1 calc R
C6 C 0.7431(2) 0.70546(17) 0.50786(10) 0.0223(4) Uani 1 1 d .
C7 C 0.6049(2) 0.75556(17) 0.54752(10) 0.0220(4) Uani 1 1 d .
C8 C 0.4142(2) 0.86876(17) 0.60013(10) 0.0218(4) Uani 1 1 d .
C9 C 0.3233(2) 0.97393(16) 0.63930(10) 0.0221(4) Uani 1 1 d .
C10 C 0.3134(2) 1.18870(18) 0.68564(11) 0.0277(4) Uani 1 1 d .
H10 H 0.3615 1.2743 0.6925 0.033 Uiso 1 1 calc R
C11 C 0.1651(2) 1.16878(18) 0.71668(11) 0.0264(4) Uani 1 1 d .
H11 H 0.1136 1.2390 0.7443 0.032 Uiso 1 1 calc R
C12 C 0.0933(2) 1.04526(19) 0.70689(11) 0.0274(4) Uani 1 1 d .
H12 H -0.0091 1.0293 0.7269 0.033 Uiso 1 1 calc R
C13 C 0.1733(2) 0.94482(18) 0.66734(11) 0.0253(4) Uani 1 1 d .
H13 H 0.1272 0.8587 0.6596 0.030 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 0.0033 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 N1 179.999(1) 3_666 .
N1 Fe1 N2 89.68(6) 3_666 .
N1 Fe1 N2 89.68(6) . 3_666
N1 Fe1 N2 90.32(6) . .
N1 Fe1 N2 90.32(6) 3_666 3_666
N1 Fe1 N3 91.93(6) . 3_666
N1 Fe1 N3 88.07(6) 3_666 3_666
N1 Fe1 N3 88.07(6) . .
N1 Fe1 N3 91.93(6) 3_666 .
N2 Fe1 N2 180.0 . 3_666
N3 Fe1 N2 79.55(6) 3_666 3_666
N3 Fe1 N2 100.45(6) . 3_666
N3 Fe1 N2 100.45(6) 3_666 .
N3 Fe1 N2 79.55(6) . .
N3 Fe1 N3 180.0 3_666 .
C1 N1 Fe1 170.90(14) . .
C2 N2 Fe1 126.37(12) . .
C2 N2 C6 117.59(15) . .
C6 N2 Fe1 116.03(11) . .
N4 N3 Fe1 135.98(11) . .
C7 N3 Fe1 114.94(12) . .
C7 N3 N4 108.99(14) . .
C8 N4 N3 106.88(14) . .
C7 N5 N6 124.52(15) . .
C7 N5 C8 105.69(14) . .
C8 N5 N6 129.70(15) . .
N5 N6 H6A 105.4(14) . .
N5 N6 H6B 104.3(13) . .
H6A N6 H6B 101.5(18) . .
C9 N7 C10 116.70(16) . .
N1 C1 S1 178.88(16) . .
N2 C2 H2 118.7 . .
N2 C2 C3 122.57(18) . .
C3 C2 H2 118.7 . .
C2 C3 H3 120.3 . .
C4 C3 C2 119.45(18) . .
C4 C3 H3 120.3 . .
C3 C4 H4 120.5 . .
C3 C4 C5 119.08(17) . .
C5 C4 H4 120.5 . .
C4 C5 H5 120.9 . .
C6 C5 C4 118.30(18) . .
C6 C5 H5 120.9 . .
N2 C6 C5 122.90(16) . .
N2 C6 C7 110.20(14) . .
C5 C6 C7 126.83(16) . .
N3 C7 N5 108.55(15) . .
N3 C7 C6 118.57(15) . .
N5 C7 C6 132.59(15) . .
N4 C8 N5 109.88(15) . .
N4 C8 C9 123.95(16) . .
N5 C8 C9 126.16(15) . .
N7 C9 C8 116.55(16) . .
N7 C9 C13 123.83(16) . .
C13 C9 C8 119.62(15) . .
N7 C10 H10 118.2 . .
N7 C10 C11 123.65(17) . .
C11 C10 H10 118.2 . .
C10 C11 H11 120.6 . .
C12 C11 C10 118.87(17) . .
C12 C11 H11 120.6 . .
C11 C12 H12 120.6 . .
C11 C12 C13 118.85(18) . .
C13 C12 H12 120.6 . .
C9 C13 H13 121.0 . .
C12 C13 C9 118.06(17) . .
C12 C13 H13 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9636(15) .
Fe1 N1 1.9636(15) 3_666
Fe1 N2 2.0234(14) .
Fe1 N2 2.0234(14) 3_666
Fe1 N3 1.9696(14) 3_666
Fe1 N3 1.9696(14) .
S1 C1 1.6490(18) .
N1 C1 1.161(2) .
N2 C2 1.338(2) .
N2 C6 1.363(2) .
N3 N4 1.3622(19) .
N3 C7 1.323(2) .
N4 C8 1.317(2) .
N5 N6 1.425(2) .
N5 C7 1.361(2) .
N5 C8 1.369(2) .
N6 H6A 0.89(2) .
N6 H6B 0.93(2) .
N7 C9 1.339(2) .
N7 C10 1.339(2) .
C2 H2 0.9500 .
C2 C3 1.388(3) .
C3 H3 0.9500 .
C3 C4 1.376(3) .
C4 H4 0.9500 .
C4 C5 1.392(3) .
C5 H5 0.9500 .
C5 C6 1.384(2) .
C6 C7 1.448(2) .
C8 C9 1.466(2) .
C9 C13 1.394(2) .
C10 H10 0.9500 .
C10 C11 1.384(3) .
C11 H11 0.9500 .
C11 C12 1.380(3) .
C12 H12 0.9500 .
C12 C13 1.386(3) .
C13 H13 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H6A N7 0.89(2) 2.13(2) 2.850(2) 138.4(19) .
N6 H6B S1 0.93(2) 2.59(2) 3.3958(18) 144.5(17) 4_676
