#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316763.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_4316763
loop_
_publ_author_name
'Gaelle Dupouy'
'Smail Triki'
'Mathieu Marchivie'
'Nathalie Cosquer'
'Carlos J. Gómez-García'
'Sébastien Pillet'
'El-Eulmi Bendeif'
'Claude Lecomte'
'Saket Asthana'
'Jean-François Létard'
_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        ' Prof. Smail Triki'
_publ_contact_author_phone       +33298016146
_publ_section_title
;
 Cyanocarbanion-Based Spin-Crossover Materials: Photocrystallographic and
 Photomagnetic Studies of a New Iron(II) Neutral Chain
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9358
_journal_page_last               9368
_journal_paper_doi               10.1021/ic101038z
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H20 Fe1 N18'
_chemical_formula_sum            'C34 H20 Fe N18'
_chemical_formula_weight         736.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_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             2008-09-25T17:00:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.703(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2359(3)
_cell_length_b                   12.2079(2)
_cell_length_c                   11.8655(2)
_cell_measurement_reflns_used    10058
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.375
_cell_measurement_theta_min      2.5293
_cell_measurement_wavelength     0.71073
_cell_volume                     1626.83(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Oxford diffraction Xcalibur 2'
_diffrn_measurement_method       'phi scan and omega scan '
_diffrn_orient_matrix_UB_11      -0.0023615143
_diffrn_orient_matrix_UB_12      0.0478319269
_diffrn_orient_matrix_UB_13      0.0338721149
_diffrn_orient_matrix_UB_21      0.0133179744
_diffrn_orient_matrix_UB_22      0.0326651915
_diffrn_orient_matrix_UB_23      -0.0474935019
_diffrn_orient_matrix_UB_31      -0.0617441291
_diffrn_orient_matrix_UB_32      0.0052344172
_diffrn_orient_matrix_UB_33      -0.0133629364
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21459
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.96164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0417
_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)+(0.0247P)²+1.4140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                2353
_reflns_number_total             3234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101038z_si_001_5.cif
_cod_data_source_block           100K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4316763
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4495(2) 0.7521(2) 0.0318(2) 0.0333(6) Uani 1 1 d . A .
C2 C 0.4327(2) 0.6450(2) -0.0030(3) 0.0407(7) Uani 1 1 d . . .
C3 C 0.4558(3) 0.6175(2) -0.1126(3) 0.0396(7) Uani 1 1 d . . .
C4 C 0.4957(2) 0.6965(2) -0.1856(2) 0.0331(6) Uani 1 1 d . . .
C5 C 0.5095(2) 0.8023(2) -0.1448(2) 0.0281(6) Uani 1 1 d . A .
C6 C 0.5454(2) 0.8967(2) -0.2107(2) 0.0266(6) Uani 1 1 d . A .
C7 C 0.6083(2) 1.0116(2) -0.33547(19) 0.0268(5) Uani 1 1 d . A .
C8 C 0.6524(2) 1.0567(2) -0.4408(2) 0.0284(6) Uani 1 1 d . . .
C9 C 0.6949(2) 1.1631(2) -0.4462(2) 0.0338(6) Uani 1 1 d . . .
C10 C 0.7336(3) 1.2005(2) -0.5480(2) 0.0379(7) Uani 1 1 d . . .
C11 C 0.7302(2) 1.1322(2) -0.6404(2) 0.0376(7) Uani 1 1 d . . .
C12 C 0.6869(2) 1.0276(2) -0.6272(2) 0.0357(7) Uani 1 1 d . . .
C15 C 1.0920(2) 0.8434(2) -0.10019(19) 0.0260(6) Uani 1 1 d . . .
C16 C 1 1 0 0.0228(7) Uani 1 2 d S . .
N3 N 0.6821(2) 0.98781(18) 0.03217(17) 0.0322(5) Uani 1 1 d . . .
C131 C 0.7794(13) 0.9869(10) -0.0008(8) 0.021(2) Uani 0.505(5) 1 d P A 1
C141 C 0.8781(7) 0.9356(6) -0.1657(6) 0.027(2) Uiso 0.505(5) 1 d P A 1
N81 N 0.8574(9) 0.9011(13) -0.2547(10) 0.032(2) Uani 0.505(5) 1 d P A 1
N91 N 1.1566(6) 0.7767(6) -0.1152(5) 0.0308(15) Uani 0.505(5) 1 d P A 1
C17 C 0.8892(4) 0.9769(4) -0.0535(4) 0.0248(14) Uani 0.505(5) 1 d P A 1
C132 C 0.7788(12) 1.0116(9) 0.0305(9) 0.0160(19) Uani 0.495(5) 1 d P A 2
C142 C 0.8920(6) 0.9105(6) -0.1645(6) 0.023(2) Uiso 0.495(5) 1 d P A 2
N82 N 0.8218(10) 0.8993(13) -0.2321(11) 0.034(2) Uani 0.495(5) 1 d P A 2
N92 N 1.1031(6) 0.7632(6) -0.1424(6) 0.0289(15) Uani 0.495(5) 1 d P A 2
C18 C 0.8943(4) 1.0502(4) 0.0425(4) 0.0206(13) Uani 0.495(5) 1 d P . 2
C19 C 0.9915(4) 0.9185(4) -0.0847(4) 0.0235(13) Uani 0.505(5) 1 d P . 2
N1 N 0.48688(16) 0.83104(17) -0.03733(16) 0.0265(5) Uani 1 1 d . . .
N2 N 0.54063(16) 0.99689(17) -0.16812(15) 0.0262(4) Uani 1 1 d . . .
N4 N 0.57971(18) 1.07010(16) -0.24649(16) 0.0279(5) Uani 1 1 d . A .
N5 N 0.58722(18) 0.90303(16) -0.31613(17) 0.0283(5) Uani 1 1 d . . .
N6 N 0.6161(2) 0.81001(18) -0.3815(2) 0.0357(6) Uani 1 1 d . A .
N7 N 0.64725(18) 0.98843(18) -0.53008(16) 0.0323(5) Uani 1 1 d . . .
Fe Fe 0.5 1 0 0.02325(15) Uani 1 2 d S . .
H1 H 0.435(2) 0.774(2) 0.106(2) 0.036(7) Uiso 1 1 d . . .
H1N H 0.612(2) 0.831(2) -0.451(3) 0.047(9) Uiso 1 1 d . . .
H2 H 0.407(2) 0.593(2) 0.051(2) 0.049(8) Uiso 1 1 d . . .
H2N H 0.701(3) 0.800(2) -0.361(2) 0.050(9) Uiso 1 1 d . . .
H3 H 0.446(2) 0.544(2) -0.140(2) 0.040(8) Uiso 1 1 d . . .
H4 H 0.510(2) 0.683(2) -0.263(2) 0.034(7) Uiso 1 1 d . . .
H5 H 0.683(2) 0.976(2) -0.686(2) 0.027(7) Uiso 1 1 d . . .
H6 H 0.755(3) 1.155(2) -0.707(3) 0.055(9) Uiso 1 1 d . . .
H7 H 0.763(2) 1.267(2) -0.559(2) 0.039(8) Uiso 1 1 d . . .
H8 H 0.696(2) 1.206(2) -0.389(2) 0.036(8) Uiso 1 1 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
N1 C1 C2 122.6(3) . . ?
C3 C2 C1 119.1(3) . . ?
C2 C3 C4 119.8(3) . . ?
C3 C4 C5 117.8(3) . . ?
N1 C5 C4 123.2(2) . . ?
N1 C5 C6 111.3(2) . . ?
C4 C5 C6 125.4(2) . . ?
N2 C6 N5 108.6(2) . . ?
N2 C6 C5 120.7(2) . . ?
N5 C6 C5 130.6(2) . . ?
N4 C7 N5 110.0(2) . . ?
N4 C7 C8 125.0(2) . . ?
N5 C7 C8 124.9(2) . . ?
N7 C8 C9 123.4(2) . . ?
N7 C8 C7 115.5(2) . . ?
C9 C8 C7 121.2(2) . . ?
C10 C9 C8 118.1(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C11 C10 118.2(3) . . ?
N7 C12 C11 123.9(3) . . ?
N91 C15 N92 36.4(3) . . ?
N91 C15 C19 170.7(5) . . ?
N92 C15 C19 134.8(5) . . ?
N91 C15 C18 131.4(5) . 3_775 ?
N92 C15 C18 167.5(5) . 3_775 ?
C19 C15 C18 57.5(3) . 3_775 ?
C17 C16 C17 180.0000(10) . 3_775 ?
C17 C16 C19 120.1(3) . 3_775 ?
C17 C16 C19 59.9(3) 3_775 3_775 ?
C17 C16 C19 59.9(3) . . ?
C17 C16 C19 120.1(3) 3_775 . ?
C19 C16 C19 180.0(4) 3_775 . ?
C17 C16 C18 61.1(3) . . ?
C17 C16 C18 118.9(3) 3_775 . ?
C19 C16 C18 59.4(3) 3_775 . ?
C19 C16 C18 120.6(3) . . ?
C17 C16 C18 118.9(3) . 3_775 ?
C17 C16 C18 61.1(3) 3_775 3_775 ?
C19 C16 C18 120.6(3) 3_775 3_775 ?
C19 C16 C18 59.4(3) . 3_775 ?
C18 C16 C18 180.0000(10) . 3_775 ?
C132 N3 C131 23.9(5) . . ?
C132 N3 Fe 157.7(7) . . ?
C131 N3 Fe 149.7(6) . . ?
N3 C131 C17 171.7(9) . . ?
N81 C141 C17 173.4(8) . . ?
C131 C17 C16 123.9(5) . . ?
C131 C17 C141 113.1(6) . . ?
C16 C17 C141 122.9(4) . . ?
N3 C132 C18 171.4(8) . . ?
N82 C142 C19 173.8(9) . . ?
C132 C18 C19 164.9(6) . 3_775 ?
C132 C18 C16 126.8(5) . . ?
C19 C18 C16 59.4(3) 3_775 . ?
C132 C18 C15 115.7(5) . 3_775 ?
C19 C18 C15 61.1(3) 3_775 3_775 ?
C16 C18 C15 117.5(3) . 3_775 ?
C16 C19 C18 61.2(3) . 3_775 ?
C16 C19 C142 123.2(4) . . ?
C18 C19 C142 157.5(5) 3_775 . ?
C16 C19 C15 119.4(3) . . ?
C18 C19 C15 61.4(3) 3_775 . ?
C142 C19 C15 117.2(5) . . ?
C1 N1 C5 117.4(2) . . ?
C1 N1 Fe 126.45(18) . . ?
C5 N1 Fe 115.87(16) . . ?
C6 N2 N4 109.01(19) . . ?
C6 N2 Fe 113.49(16) . . ?
N4 N2 Fe 136.83(16) . . ?
C7 N4 N2 106.24(19) . . ?
C6 N5 C7 106.1(2) . . ?
C6 N5 N6 123.5(2) . . ?
C7 N5 N6 129.9(2) . . ?
C12 N7 C8 116.7(2) . . ?
N2 Fe N2 180.00(12) . 3_675 ?
N2 Fe N3 93.95(7) . 3_675 ?
N2 Fe N3 86.05(7) 3_675 3_675 ?
N2 Fe N3 86.05(7) . . ?
N2 Fe N3 93.95(7) 3_675 . ?
N3 Fe N3 180.00(12) 3_675 . ?
N2 Fe N1 101.82(8) . 3_675 ?
N2 Fe N1 78.18(8) 3_675 3_675 ?
N3 Fe N1 91.77(8) 3_675 3_675 ?
N3 Fe N1 88.23(8) . 3_675 ?
N2 Fe N1 78.18(8) . . ?
N2 Fe N1 101.82(8) 3_675 . ?
N3 Fe N1 88.23(8) 3_675 . ?
N3 Fe N1 91.77(8) . . ?
N1 Fe N1 180.00(10) 3_675 . ?
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
C1 N1 1.342(3) . ?
C1 C2 1.382(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.386(4) . ?
C5 N1 1.354(3) . ?
C5 C6 1.456(3) . ?
C6 N2 1.325(3) . ?
C6 N5 1.352(3) . ?
C7 N4 1.322(3) . ?
C7 N5 1.367(3) . ?
C7 C8 1.465(3) . ?
C8 N7 1.348(3) . ?
C8 C9 1.386(4) . ?
C9 C10 1.374(4) . ?
C10 C11 1.378(4) . ?
C11 C12 1.377(4) . ?
C12 N7 1.337(3) . ?
C15 N91 1.108(7) . ?
C15 N92 1.108(7) . ?
C15 C19 1.471(5) . ?
C15 C18 1.474(5) 3_775 ?
C16 C17 1.409(5) . ?
C16 C17 1.409(5) 3_775 ?
C16 C19 1.415(5) 3_775 ?
C16 C19 1.415(5) . ?
C16 C18 1.441(4) . ?
C16 C18 1.441(4) 3_775 ?
N3 C132 1.126(14) . ?
N3 C131 1.172(14) . ?
N3 Fe 2.075(2) . ?
C131 C17 1.405(14) . ?
C141 N81 1.154(16) . ?
C141 C17 1.426(9) . ?
C132 C18 1.384(14) . ?
C142 N82 1.117(17) . ?
C142 C19 1.447(9) . ?
C18 C19 1.417(6) 3_775 ?
C18 C15 1.474(5) 3_775 ?
C19 C18 1.417(6) 3_775 ?
N1 Fe 2.114(2) . ?
N2 N4 1.371(3) . ?
N2 Fe 2.0600(18) . ?
N5 N6 1.418(3) . ?
Fe N2 2.0600(18) 3_675 ?
Fe N3 2.075(2) 3_675 ?
Fe N1 2.114(2) 3_675 ?
