#------------------------------------------------------------------------------
#$Date: 2016-04-05 21:27:14 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181752 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/52/7055287.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_7055287
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                 93.1120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3411(4)
_cell_length_b                   9.9442(5)
_cell_length_c                   16.1668(8)
_cell_measurement_reflns_used    3875
_cell_measurement_temperature    30.0
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.41
_cell_volume                     1338.99(11)
_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      30.0
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0467
_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            9018
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.787
_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    1.609
_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         0.727
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0341
_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)+(0.0416P)²+0.3980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                2600
_reflns_number_total             3318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02359a2.cif
_cod_data_source_block           30kls
_cod_depositor_comments
'Adding full bibliography for 7055281--7055291.cif.'
_cod_database_code               7055287
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.014) H6B(0.014) H2(0.013) H3(0.013) H4(0.014) H5(0.014)
 H10(0.014) H11(0.014) H12(0.014) H13(0.013)
 Fixed X: Fe1(0.5) H2(0.7991) H3(1.0425) H4(1.1053) H5(0.9123) H10(0.3616)
 H11(0.1128) H12(-0.0126) H13(0.1251)
 Fixed Y: Fe1(0.5) H2(0.4426) H3(0.5477) H4(0.752) H5(0.8529) H10(1.2789)
 H11(1.2432) H12(1.032) H13(0.8602)
 Fixed Z: Fe1(0.5) H2(0.4002) H3(0.3785) H4(0.4457) H5(0.5269) H10(0.6919)
 H11(0.7453) H12(0.7276) H13(0.6595)
;
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 0.00706(10) Uani 1 2 d S
S1 S 0.26557(6) 0.71425(5) 0.26020(3) 0.01196(12) Uani 1 1 d .
N1 N 0.40060(18) 0.57073(15) 0.39687(10) 0.0095(3) Uani 1 1 d .
N2 N 0.71135(19) 0.58159(15) 0.47304(9) 0.0095(3) Uani 1 1 d .
N3 N 0.47686(19) 0.67903(15) 0.54830(9) 0.0097(3) Uani 1 1 d .
N4 N 0.35481(19) 0.75030(15) 0.58002(10) 0.0093(3) Uani 1 1 d .
N5 N 0.57166(19) 0.87759(15) 0.57979(10) 0.0091(3) Uani 1 1 d .
N6 N 0.6845(2) 0.98395(16) 0.59319(11) 0.0117(3) Uani 1 1 d .
H6A H 0.629(3) 1.058(2) 0.6028(13) 0.014 Uiso 1 1 d .
H6B H 0.734(3) 0.964(2) 0.6421(15) 0.014 Uiso 1 1 d .
N7 N 0.3928(2) 1.09724(15) 0.64599(10) 0.0112(3) Uani 1 1 d .
C1 C 0.3440(2) 0.62913(18) 0.34030(12) 0.0096(4) Uani 1 1 d .
C2 C 0.8218(2) 0.52683(18) 0.42595(12) 0.0105(4) Uani 1 1 d .
H2 H 0.7991 0.4426 0.4002 0.013 Uiso 1 1 calc R
C3 C 0.9681(2) 0.58844(19) 0.41330(12) 0.0112(4) Uani 1 1 d .
H3 H 1.0425 0.5477 0.3785 0.013 Uiso 1 1 calc R
C4 C 1.0043(2) 0.71000(18) 0.45192(12) 0.0119(4) Uani 1 1 d .
H4 H 1.1053 0.7520 0.4457 0.014 Uiso 1 1 calc R
C5 C 0.8908(2) 0.76947(19) 0.49988(12) 0.0113(4) Uani 1 1 d .
H5 H 0.9123 0.8529 0.5269 0.014 Uiso 1 1 calc R
C6 C 0.7449(2) 0.70432(18) 0.50754(11) 0.0091(4) Uani 1 1 d .
C7 C 0.6065(2) 0.75545(18) 0.54719(11) 0.0095(4) Uani 1 1 d .
C8 C 0.4140(2) 0.86982(18) 0.59943(11) 0.0102(4) Uani 1 1 d .
C9 C 0.3224(2) 0.97599(18) 0.63883(12) 0.0103(4) Uani 1 1 d .
C10 C 0.3132(2) 1.19283(19) 0.68542(12) 0.0115(4) Uani 1 1 d .
H10 H 0.3616 1.2789 0.6919 0.014 Uiso 1 1 calc R
C11 C 0.1641(2) 1.17263(19) 0.71719(12) 0.0114(4) Uani 1 1 d .
H11 H 0.1128 1.2432 0.7453 0.014 Uiso 1 1 calc R
C12 C 0.0906(2) 1.04788(19) 0.70740(11) 0.0113(4) Uani 1 1 d .
H12 H -0.0126 1.0320 0.7276 0.014 Uiso 1 1 calc R
C13 C 0.1715(2) 0.94682(19) 0.66731(11) 0.0107(4) Uani 1 1 d .
H13 H 0.1251 0.8602 0.6595 0.013 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 180.0 3_666 .
N1 Fe1 N2 90.35(6) 3_666 3_666
N1 Fe1 N2 90.35(6) . .
N1 Fe1 N2 89.65(6) . 3_666
N1 Fe1 N2 89.65(6) 3_666 .
N1 Fe1 N3 91.92(6) . 3_666
N1 Fe1 N3 88.08(6) 3_666 3_666
N1 Fe1 N3 88.08(6) . .
N1 Fe1 N3 91.92(6) 3_666 .
N2 Fe1 N2 180.00(8) 3_666 .
N3 Fe1 N2 100.02(6) 3_666 .
N3 Fe1 N2 79.98(6) . .
N3 Fe1 N2 79.98(6) 3_666 3_666
N3 Fe1 N2 100.02(6) . 3_666
N3 Fe1 N3 179.998(1) 3_666 .
C1 N1 Fe1 171.09(15) . .
C2 N2 Fe1 126.62(13) . .
C2 N2 C6 117.56(16) . .
C6 N2 Fe1 115.81(12) . .
N4 N3 Fe1 135.61(12) . .
C7 N3 Fe1 114.76(13) . .
C7 N3 N4 109.52(15) . .
C8 N4 N3 106.28(15) . .
C7 N5 N6 124.62(16) . .
C7 N5 C8 105.47(15) . .
C8 N5 N6 129.82(15) . .
N5 N6 H6A 107.2(15) . .
N5 N6 H6B 104.0(15) . .
H6A N6 H6B 104(2) . .
C10 N7 C9 116.87(17) . .
N1 C1 S1 179.07(18) . .
N2 C2 H2 118.7 . .
N2 C2 C3 122.66(17) . .
C3 C2 H2 118.7 . .
C2 C3 H3 120.3 . .
C4 C3 C2 119.31(18) . .
C4 C3 H3 120.3 . .
C3 C4 H4 120.5 . .
C3 C4 C5 118.97(18) . .
C5 C4 H4 120.5 . .
C4 C5 H5 120.7 . .
C4 C5 C6 118.57(17) . .
C6 C5 H5 120.7 . .
N2 C6 C5 122.80(17) . .
N2 C6 C7 110.19(16) . .
C5 C6 C7 126.92(17) . .
N3 C7 N5 108.40(16) . .
N3 C7 C6 118.55(16) . .
N5 C7 C6 132.74(17) . .
N4 C8 N5 110.32(16) . .
N4 C8 C9 123.66(17) . .
N5 C8 C9 126.00(17) . .
N7 C9 C8 116.57(17) . .
N7 C9 C13 123.81(17) . .
C13 C9 C8 119.61(17) . .
N7 C10 H10 118.3 . .
N7 C10 C11 123.45(18) . .
C11 C10 H10 118.3 . .
C10 C11 H11 120.4 . .
C10 C11 C12 119.12(17) . .
C12 C11 H11 120.4 . .
C11 C12 H12 120.8 . .
C11 C12 C13 118.45(18) . .
C13 C12 H12 120.8 . .
C9 C13 H13 120.9 . .
C12 C13 C9 118.26(18) . .
C12 C13 H13 120.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9523(16) .
Fe1 N1 1.9523(16) 3_666
Fe1 N2 2.0098(16) 3_666
Fe1 N2 2.0098(16) .
Fe1 N3 1.9577(15) .
Fe1 N3 1.9577(15) 3_666
S1 C1 1.652(2) .
N1 C1 1.162(2) .
N2 C2 1.342(2) .
N2 C6 1.365(2) .
N3 N4 1.363(2) .
N3 C7 1.322(2) .
N4 C8 1.318(2) .
N5 N6 1.424(2) .
N5 C7 1.362(2) .
N5 C8 1.371(2) .
N6 H6A 0.88(2) .
N6 H6B 0.89(2) .
N7 C9 1.343(2) .
N7 C10 1.341(2) .
C2 H2 0.9500 .
C2 C3 1.390(3) .
C3 H3 0.9500 .
C3 C4 1.386(3) .
C4 H4 0.9500 .
C4 C5 1.388(3) .
C5 H5 0.9500 .
C5 C6 1.390(3) .
C6 C7 1.443(3) .
C8 C9 1.469(3) .
C9 C13 1.395(3) .
C10 H10 0.9500 .
C10 C11 1.386(3) .
C11 H11 0.9500 .
C11 C12 1.389(3) .
C12 H12 0.9500 .
C12 C13 1.390(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 0.88(2) 2.16(2) 2.853(2) 134.5(19) .
N6 H6B S1 0.89(2) 2.61(2) 3.3814(18) 145.0(19) 4_676
