#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/60/4306027.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_4306027
loop_
_publ_author_name
'Gaelle Dupouy'
'Mathieu Marchivie'
'Smail Triki'
'Jean Sala-Pala'
'Jean-Yves Salaün'
'Carlos J. Gómez-García'
'Philippe Guionneau'
_publ_contact_author_address
;UMR CNRS 6521, Université de Bretagne Occidentale,
 BP 809, 29285 Brest Cedex (France)'
;
_publ_contact_author_email       triki@univ-brest.fr
_publ_contact_author_fax         +33298017001
_publ_contact_author_name        'TRIKI Smail'
_publ_contact_author_phone       +33298016146
_publ_section_title
;
The Key Role of the Intermolecular π-π Interactions in the Presence of
Spin Crossover in Neutral [Fe(abpt)2A2] Complexes (A = Terminal Monoanion N
Ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8921
_journal_page_last               8931
_journal_paper_doi               10.1021/ic800955r
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H20 Fe1 N18'
_chemical_formula_sum            'C32 H20 Fe N18'
_chemical_formula_weight         712.51
_chemical_name_systematic
;
 [Fe(abpt)2(tcm)2] 400 K
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-02-22T15:37:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.101(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2941(7)
_cell_length_b                   10.8508(8)
_cell_length_c                   16.7503(11)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     1688.9(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      400(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7507
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.5
_exptl_absorpt_correction_T_max  0.9517
_exptl_absorpt_correction_T_min  0.8644
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.086
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.8592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                2018
_reflns_number_total             3108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800955r_si_001_2.cif
_cod_data_source_block           struct1_400k
_cod_original_formula_sum        'C32 H20 Fe1 N18'
_cod_database_code               4306027
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0 0 0.5 0.0523(2) Uani 1 2 d S . .
N1 N -0.1289(2) 0.0842(2) 0.40396(14) 0.0560(6) Uani 1 1 d . . .
C7 C -0.3895(3) -0.2092(3) 0.51711(18) 0.0550(7) Uani 1 1 d . . .
N6 N -0.5311(3) -0.1321(3) 0.3973(2) 0.0770(9) Uani 1 1 d D . .
C8 C -0.5127(3) 0.3042(3) 0.45409(18) 0.0580(7) Uani 1 1 d . . .
N4 N -0.2640(3) -0.1831(2) 0.55063(15) 0.0643(7) Uani 1 1 d . . .
N5 N -0.4131(2) -0.1350(2) 0.45190(14) 0.0549(6) Uani 1 1 d . . .
N2 N -0.2044(2) -0.0911(2) 0.50573(14) 0.0577(6) Uani 1 1 d . . .
C6 C -0.2949(3) -0.0625(3) 0.44687(17) 0.0521(7) Uani 1 1 d . . .
N7 N -0.3769(3) 0.3009(2) 0.48274(16) 0.0723(7) Uani 1 1 d . . .
C5 C -0.2595(3) 0.0332(3) 0.38914(18) 0.0557(7) Uani 1 1 d . . .
C14 C -0.1458(3) 0.3100(3) 0.6744(2) 0.0687(9) Uani 1 1 d . . .
C13 C -0.1014(3) 0.2161(3) 0.6236(2) 0.0638(8) Uani 1 1 d . . .
C2 C -0.1704(4) 0.2206(3) 0.2951(2) 0.0802(10) Uani 1 1 d . . .
H2 H -0.1386 0.286 0.2642 0.096 Uiso 1 1 calc R . .
N3 N -0.0664(3) 0.1388(3) 0.58212(18) 0.0796(8) Uani 1 1 d . . .
C1 C -0.0879(3) 0.1773(3) 0.3581(2) 0.0699(9) Uani 1 1 d . . .
H1 H 0.0003 0.2147 0.369 0.084 Uiso 1 1 calc R . .
C9 C -0.5610(4) 0.3916(3) 0.4006(2) 0.0751(9) Uani 1 1 d . . .
H9 H -0.6558 0.3908 0.3818 0.09 Uiso 1 1 calc R . .
C16 C -0.2357(5) 0.2811(4) 0.7372(3) 0.0891(12) Uani 1 1 d . . .
C4 C -0.3463(4) 0.0717(3) 0.3270(2) 0.0784(10) Uani 1 1 d . . .
H4 H -0.4352 0.0347 0.3173 0.094 Uiso 1 1 calc R . .
C15 C 0.1010(4) 0.5683(4) 0.3403(2) 0.0853(11) Uani 1 1 d . . .
C3 C -0.2993(4) 0.1662(4) 0.2791(2) 0.0925(12) Uani 1 1 d . . .
H3 H -0.3557 0.1926 0.2359 0.111 Uiso 1 1 calc R . .
C11 C -0.3267(5) 0.4781(4) 0.4034(3) 0.0912(12) Uani 1 1 d . . .
H11 H -0.2604 0.5365 0.3868 0.109 Uiso 1 1 calc R . .
C12 C -0.2871(4) 0.3876(4) 0.4564(2) 0.0865(11) Uani 1 1 d . . .
H12 H -0.1923 0.3864 0.4752 0.104 Uiso 1 1 calc R . .
C10 C -0.4663(5) 0.4805(3) 0.3752(2) 0.0920(12) Uani 1 1 d . . .
H10 H -0.4966 0.5413 0.3396 0.11 Uiso 1 1 calc R . .
N9 N -0.3107(5) 0.2582(4) 0.7871(3) 0.1402(17) Uani 1 1 d . . .
N8 N 0.0653(5) 0.4698(4) 0.3513(3) 0.1359(16) Uani 1 1 d . . .
H6 H -0.601(4) -0.172(3) 0.423(2) 0.126(16) Uiso 1 1 d D . .
H5 H -0.507(5) -0.183(4) 0.359(2) 0.16(2) Uiso 1 1 d D . .
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 0 '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'
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
_geom_angle_publ_flag
N3 Fe1 N3 180.00(12) 3_556 . ?
N3 Fe1 N2 88.34(10) 3_556 . ?
N3 Fe1 N2 91.66(10) . . ?
N3 Fe1 N2 91.66(10) 3_556 3_556 ?
N3 Fe1 N2 88.34(10) . 3_556 ?
N2 Fe1 N2 180 . 3_556 ?
N3 Fe1 N1 91.05(10) 3_556 3_556 ?
N3 Fe1 N1 88.95(10) . 3_556 ?
N2 Fe1 N1 104.35(9) . 3_556 ?
N2 Fe1 N1 75.65(9) 3_556 3_556 ?
N3 Fe1 N1 88.95(10) 3_556 . ?
N3 Fe1 N1 91.05(10) . . ?
N2 Fe1 N1 75.65(9) . . ?
N2 Fe1 N1 104.35(9) 3_556 . ?
N1 Fe1 N1 180.00(8) 3_556 . ?
C1 N1 C5 118.1(3) . . ?
C1 N1 Fe1 125.7(2) . . ?
C5 N1 Fe1 116.19(19) . . ?
N4 C7 N5 109.9(2) . . ?
N4 C7 C8 124.2(3) . 3_456 ?
N5 C7 C8 125.9(3) . 3_456 ?
N7 C8 C9 123.0(3) . . ?
N7 C8 C7 116.7(3) . 3_456 ?
C9 C8 C7 120.3(3) . 3_456 ?
C7 N4 N2 106.7(2) . . ?
C6 N5 C7 105.8(2) . . ?
C6 N5 N6 124.5(2) . . ?
C7 N5 N6 129.7(2) . . ?
C6 N2 N4 108.8(2) . . ?
C6 N2 Fe1 114.23(19) . . ?
N4 N2 Fe1 136.59(18) . . ?
N2 C6 N5 108.8(2) . . ?
N2 C6 C5 120.8(2) . . ?
N5 C6 C5 130.3(3) . . ?
C12 N7 C8 116.8(3) . . ?
N1 C5 C4 121.9(3) . . ?
N1 C5 C6 112.5(2) . . ?
C4 C5 C6 125.6(3) . . ?
C16 C14 C13 119.0(3) . . ?
C16 C14 C15 121.8(3) . 3_566 ?
C13 C14 C15 119.2(3) . 3_566 ?
N3 C13 C14 179.4(4) . . ?
C3 C2 C1 118.7(3) . . ?
C13 N3 Fe1 177.4(3) . . ?
N1 C1 C2 122.8(3) . . ?
C8 C9 C10 118.8(3) . . ?
N9 C16 C14 178.7(5) . . ?
C5 C4 C3 118.8(3) . . ?
N8 C15 C14 179.3(5) . 3_566 ?
C2 C3 C4 119.8(3) . . ?
C12 C11 C10 118.5(3) . . ?
N7 C12 C11 123.8(4) . . ?
C11 C10 C9 119.1(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 N3 2.139(3) 3_556 ?
Fe1 N3 2.139(3) . ?
Fe1 N2 2.145(2) . ?
Fe1 N2 2.145(2) 3_556 ?
Fe1 N1 2.187(2) 3_556 ?
Fe1 N1 2.187(2) . ?
N1 C1 1.330(4) . ?
N1 C5 1.352(3) . ?
C7 N4 1.316(4) . ?
C7 N5 1.372(3) . ?
C7 C8 1.462(4) 3_456 ?
N6 N5 1.415(3) . ?
C8 N7 1.342(4) . ?
C8 C9 1.374(4) . ?
C8 C7 1.462(4) 3_456 ?
N4 N2 1.373(3) . ?
N5 C6 1.355(3) . ?
N2 C6 1.321(3) . ?
C6 C5 1.461(4) . ?
N7 C12 1.338(4) . ?
C5 C4 1.370(4) . ?
C14 C16 1.393(5) . ?
C14 C13 1.395(4) . ?
C14 C15 1.407(5) 3_566 ?
C13 N3 1.140(4) . ?
C2 C3 1.358(5) . ?
C2 C1 1.375(4) . ?
C9 C10 1.378(5) . ?
C16 N9 1.126(5) . ?
C4 C3 1.378(5) . ?
C15 N8 1.135(5) . ?
C15 C14 1.407(5) 3_566 ?
C11 C12 1.369(5) . ?
C11 C10 1.372(5) . ?
