#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316762.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_4316762
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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.401(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3439(2)
_cell_length_b                   12.2258(2)
_cell_length_c                   11.8418(2)
_cell_measurement_reflns_used    13426
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      3.33
_cell_volume                     1640.88(5)
_computing_cell_refinement       'DENZO (Otwinowski, 1996)'
_computing_data_collection       'COLLECT (Otwinowski, 1996)'
_computing_data_reduction        'SORTAV (Blessing, 1989)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Xcalibur CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13426
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Absorption correction were performed using CRYSALIS Oxford Diffraction (2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.364
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.364
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0739
_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)+(0.0000P)²+3.4277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                5592
_reflns_number_total             6239
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic101038z_si_001_4.cif
_cod_data_source_block           150K
_cod_original_cell_volume        1640.89(3)
_cod_database_code               4316762
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 0.4476(2) 0.7479(3) 0.0269(3) 0.0292(5) Uani 1 1 d . A .
C2 C 0.4312(3) 0.6409(3) -0.0095(3) 0.0358(7) Uani 1 1 d . . .
C3 C 0.4551(3) 0.6151(3) -0.1194(3) 0.0374(7) Uani 1 1 d . . .
C4 C 0.4955(3) 0.6950(2) -0.1909(3) 0.0311(6) Uani 1 1 d . . .
C5 C 0.5089(2) 0.8003(2) -0.1485(2) 0.0240(5) Uani 1 1 d . A .
C6 C 0.5458(2) 0.8952(2) -0.2137(2) 0.0224(4) Uani 1 1 d . A .
C7 C 0.6090(2) 1.0096(2) -0.3376(2) 0.0232(4) Uani 1 1 d . A .
C8 C 0.6529(2) 1.0539(2) -0.4429(2) 0.0237(5) Uani 1 1 d . . .
C9 C 0.6957(3) 1.1603(3) -0.4468(3) 0.0328(6) Uani 1 1 d . . .
C10 C 0.7347(3) 1.1974(3) -0.5494(3) 0.0399(7) Uani 1 1 d . . .
C11 C 0.7297(3) 1.1288(3) -0.6424(3) 0.0386(7) Uani 1 1 d . . .
C12 C 0.6867(3) 1.0244(3) -0.6292(3) 0.0350(7) Uani 1 1 d . . .
C15 C 1.0911(2) 0.8453(2) -0.1013(2) 0.0237(5) Uani 1 1 d . . .
C16 C 1.0000 1.0000 0.0000 0.0199(6) Uani 1 2 d S . .
N31 N 0.68723(19) 0.9840(2) 0.0354(2) 0.0290(5) Uani 1 1 d . . .
C131 C 0.7798(7) 0.9853(6) 0.0004(5) 0.0203(12) Uani 0.50 1 d P A 1
C141 C 0.8743(6) 0.9349(5) -0.1662(5) 0.0238(12) Uiso 0.50 1 d P A 1
N81 N 0.8548(7) 0.8994(11) -0.2552(8) 0.0349(17) Uani 0.50 1 d P A 1
N91 N 1.1578(5) 0.7801(5) -0.1170(4) 0.0317(11) Uani 0.50 1 d P B 1
C17 C 0.8869(4) 0.9748(4) -0.0546(4) 0.0218(9) Uani 0.50 1 d P A 1
C132 C 0.7835(6) 1.0086(6) 0.0322(5) 0.0190(12) Uani 0.50 1 d P A 2
C142 C 0.8941(6) 0.9100(5) -0.1641(5) 0.0236(12) Uiso 0.50 1 d P B 2
N82 N 0.8234(7) 0.8994(12) -0.2326(8) 0.0376(19) Uani 0.50 1 d P B 2
N92 N 1.1006(5) 0.7643(5) -0.1450(5) 0.0325(11) Uani 0.50 1 d P B 2
C18 C 0.8986(4) 1.0503(4) 0.0441(4) 0.0194(8) Uani 0.50 1 d P . 2
C19 C 0.9939(4) 0.9202(4) -0.0845(4) 0.0195(8) Uani 0.50 1 d P . 2
N1 N 0.48568(18) 0.82715(19) -0.04085(19) 0.0233(4) Uani 1 1 d . . .
N2 N 0.54109(18) 0.99544(19) -0.17150(18) 0.0234(4) Uani 1 1 d . . .
N4 N 0.58082(19) 1.06807(19) -0.24965(18) 0.0228(4) Uani 1 1 d . A .
N5 N 0.58807(19) 0.90080(19) -0.31802(19) 0.0243(4) Uani 1 1 d . . .
N6 N 0.6171(3) 0.8081(2) -0.3829(2) 0.0324(5) Uani 1 1 d . A .
N7 N 0.6474(2) 0.9856(2) -0.53196(19) 0.0294(5) Uani 1 1 d . . .
Fe01 Fe 0.5000 1.0000 0.0000 0.02101(11) Uani 1 2 d S . .
H1 H 0.434(3) 0.770(3) 0.099(3) 0.039(10) Uiso 1 1 d . . .
H1N H 0.613(4) 0.829(4) -0.451(4) 0.053(13) Uiso 1 1 d . . .
H2 H 0.398(4) 0.588(4) 0.040(4) 0.054(12) Uiso 1 1 d . . .
H2N H 0.704(4) 0.793(4) -0.360(4) 0.059(13) Uiso 1 1 d . . .
H3 H 0.445(3) 0.540(3) -0.150(3) 0.047(11) Uiso 1 1 d . . .
H4 H 0.510(3) 0.682(3) -0.269(3) 0.029(9) Uiso 1 1 d . . .
H5 H 0.680(3) 0.974(3) -0.691(3) 0.045(11) Uiso 1 1 d . . .
H6 H 0.757(4) 1.152(4) -0.708(4) 0.077(16) Uiso 1 1 d . . .
H7 H 0.765(4) 1.268(4) -0.558(4) 0.069(15) Uiso 1 1 d . . .
H8 H 0.703(3) 1.204(3) -0.382(3) 0.036(10) 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 0.0000 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 122.5(3) . . ?
N1 C1 H1 115(2) . . ?
C2 C1 H1 123(2) . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 H2 121(3) . . ?
C1 C2 H2 120(3) . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 122(2) . . ?
C4 C3 H3 118(2) . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 H4 123(2) . . ?
C5 C4 H4 119(2) . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 C6 112.0(2) . . ?
C4 C5 C6 125.0(2) . . ?
N2 C6 N5 108.7(2) . . ?
N2 C6 C5 121.1(2) . . ?
N5 C6 C5 130.1(2) . . ?
N4 C7 N5 110.1(2) . . ?
N4 C7 C8 125.1(2) . . ?
N5 C7 C8 124.7(2) . . ?
N7 C8 C9 124.1(3) . . ?
N7 C8 C7 115.5(2) . . ?
C9 C8 C7 120.4(2) . . ?
C10 C9 C8 117.3(3) . . ?
C10 C9 H8 121(2) . . ?
C8 C9 H8 121(2) . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H7 118(3) . . ?
C9 C10 H7 122(3) . . ?
C12 C11 C10 118.3(3) . . ?
C12 C11 H6 122(3) . . ?
C10 C11 H6 119(3) . . ?
N7 C12 C11 123.9(3) . . ?
N7 C12 H5 114(2) . . ?
C11 C12 H5 122(2) . . ?
N91 C15 N92 38.6(4) . . ?
N91 C15 C18 131.6(5) . 3_775 ?
N92 C15 C18 169.9(4) . 3_775 ?
N91 C15 C19 173.2(5) . . ?
N92 C15 C19 134.9(4) . . ?
C18 C15 C19 55.0(3) 3_775 . ?
C19 C16 C19 180.0(4) . 3_775 ?
C19 C16 C18 123.2(3) . . ?
C19 C16 C18 56.8(3) 3_775 . ?
C19 C16 C18 56.8(3) . 3_775 ?
C19 C16 C18 123.2(3) 3_775 3_775 ?
C18 C16 C18 180.000(1) . 3_775 ?
C19 C16 C17 60.9(3) . . ?
C19 C16 C17 119.1(3) 3_775 . ?
C18 C16 C17 62.7(3) . . ?
C18 C16 C17 117.3(3) 3_775 . ?
C19 C16 C17 119.1(3) . 3_775 ?
C19 C16 C17 60.9(3) 3_775 3_775 ?
C18 C16 C17 117.3(3) . 3_775 ?
C18 C16 C17 62.7(3) 3_775 3_775 ?
C17 C16 C17 180.000(1) . 3_775 ?
C132 N31 C131 24.0(3) . . ?
C132 N31 Fe01 155.6(4) . . ?
C131 N31 Fe01 147.1(4) . . ?
N31 C131 C17 171.2(6) . . ?
N81 C141 C17 174.4(7) . . ?
C131 C17 C141 114.1(5) . . ?
C131 C17 C16 122.7(4) . . ?
C141 C17 C16 123.1(4) . . ?
N31 C132 C18 170.3(6) . . ?
N82 C142 C19 174.0(7) . . ?
C19 C18 C132 164.2(5) 3_775 . ?
C19 C18 C16 60.7(3) 3_775 . ?
C132 C18 C16 124.7(4) . . ?
C19 C18 C15 62.8(3) 3_775 3_775 ?
C132 C18 C15 115.1(4) . 3_775 ?
C16 C18 C15 120.2(3) . 3_775 ?
C18 C19 C16 62.6(3) 3_775 . ?
C18 C19 C142 158.5(5) 3_775 . ?
C16 C19 C142 122.7(4) . . ?
C18 C19 C15 62.2(3) 3_775 . ?
C16 C19 C15 121.5(3) . . ?
C142 C19 C15 115.7(4) . . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Fe01 126.4(2) . . ?
C5 N1 Fe01 115.49(17) . . ?
C6 N2 N4 108.9(2) . . ?
C6 N2 Fe01 113.74(17) . . ?
N4 N2 Fe01 136.58(18) . . ?
C7 N4 N2 106.3(2) . . ?
C6 N5 C7 106.0(2) . . ?
C6 N5 N6 123.9(2) . . ?
C7 N5 N6 129.7(2) . . ?
N5 N6 H1N 106(3) . . ?
N5 N6 H2N 104(3) . . ?
H1N N6 H2N 109(4) . . ?
C12 N7 C8 116.6(3) . . ?
N2 Fe01 N2 180.00(13) . 3_675 ?
N2 Fe01 N31 85.92(9) . . ?
N2 Fe01 N31 94.08(9) 3_675 . ?
N2 Fe01 N31 94.08(9) . 3_675 ?
N2 Fe01 N31 85.92(9) 3_675 3_675 ?
N31 Fe01 N31 180.0 . 3_675 ?
N2 Fe01 N1 77.10(8) . . ?
N2 Fe01 N1 102.90(8) 3_675 . ?
N31 Fe01 N1 91.08(9) . . ?
N31 Fe01 N1 88.92(9) 3_675 . ?
N2 Fe01 N1 102.90(8) . 3_675 ?
N2 Fe01 N1 77.10(8) 3_675 3_675 ?
N31 Fe01 N1 88.92(9) . 3_675 ?
N31 Fe01 N1 91.08(9) 3_675 3_675 ?
N1 Fe01 N1 180.00(11) . 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 1.341(3) . ?
C1 C2 1.387(5) . ?
C1 H1 0.91(4) . ?
C2 C3 1.377(5) . ?
C2 H2 0.97(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.99(4) . ?
C4 C5 1.387(4) . ?
C4 H4 0.96(3) . ?
C5 N1 1.353(3) . ?
C5 C6 1.465(4) . ?
C6 N2 1.325(3) . ?
C6 N5 1.346(3) . ?
C7 N4 1.314(3) . ?
C7 N5 1.372(3) . ?
C7 C8 1.465(3) . ?
C8 N7 1.345(3) . ?
C8 C9 1.391(4) . ?
C9 C10 1.387(4) . ?
C9 H8 0.93(4) . ?
C10 C11 1.383(5) . ?
C10 H7 0.93(5) . ?
C11 C12 1.377(5) . ?
C11 H6 0.90(5) . ?
C12 N7 1.339(4) . ?
C12 H5 0.96(4) . ?
C15 N91 1.120(6) . ?
C15 N92 1.125(6) . ?
C15 C18 1.447(6) 3_775 ?
C15 C19 1.454(5) . ?
C16 C19 1.397(5) . ?
C16 C19 1.397(5) 3_775 ?
C16 C18 1.423(5) . ?
C16 C18 1.423(5) 3_775 ?
C16 C17 1.445(5) . ?
C16 C17 1.445(5) 3_775 ?
N31 C132 1.134(8) . ?
N31 C131 1.145(8) . ?
N31 Fe01 2.156(2) . ?
C131 C17 1.408(9) . ?
C141 N81 1.153(12) . ?
C141 C17 1.411(8) . ?
C132 C18 1.404(9) . ?
C142 N82 1.123(12) . ?
C142 C19 1.448(8) . ?
C18 C19 1.340(6) 3_775 ?
C18 C15 1.447(6) 3_775 ?
C19 C18 1.340(6) 3_775 ?
N1 Fe01 2.172(2) . ?
N2 N4 1.372(3) . ?
N2 Fe01 2.103(2) . ?
N5 N6 1.416(3) . ?
N6 H1N 0.84(4) . ?
N6 H2N 1.02(5) . ?
Fe01 N2 2.103(2) 3_675 ?
Fe01 N31 2.156(2) 3_675 ?
Fe01 N1 2.172(2) 3_675 ?
