#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316761.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_4316761
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                 92.364(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3665(1)
_cell_length_b                   12.2759(2)
_cell_length_c                   11.8437(1)
_cell_measurement_reflns_used    28702
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      3.32
_cell_volume                     1651.19(3)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28702
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.514
_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    1.481
_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         0.361
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0672
_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+2.7512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                5610
_reflns_number_total             6276
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic101038z_si_001_3.cif
_cod_data_source_block           200K
_cod_database_code               4316761
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 0.4481(2) 0.7483(2) 0.0260(2) 0.0356(5) Uani 1 1 d . A .
C2 C 0.4320(3) 0.6419(3) -0.0103(3) 0.0429(6) Uani 1 1 d . . .
C3 C 0.4560(3) 0.6162(2) -0.1202(3) 0.0452(7) Uani 1 1 d . . .
C4 C 0.4961(3) 0.6960(2) -0.1913(2) 0.0379(6) Uani 1 1 d . . .
C5 C 0.5092(2) 0.8007(2) -0.1491(2) 0.0290(4) Uani 1 1 d . A .
C6 C 0.54588(19) 0.89537(19) -0.21406(19) 0.0263(4) Uani 1 1 d . A .
C7 C 0.60886(19) 1.0093(2) -0.33790(19) 0.0275(4) Uani 1 1 d . A .
C8 C 0.6528(2) 1.0539(2) -0.44284(19) 0.0292(4) Uani 1 1 d . . .
C9 C 0.6945(3) 1.1599(3) -0.4468(3) 0.0412(6) Uani 1 1 d . . .
C10 C 0.7337(3) 1.1973(3) -0.5490(3) 0.0499(8) Uani 1 1 d . . .
C11 C 0.7299(3) 1.1292(3) -0.6419(3) 0.0489(8) Uani 1 1 d . . .
C12 C 0.6879(3) 1.0253(3) -0.6288(2) 0.0436(7) Uani 1 1 d . . .
C15 C 1.0909(2) 0.8459(2) -0.10093(19) 0.0292(4) Uani 1 1 d . . .
C16 C 1.0000 1.0000 0.0000 0.0245(5) Uani 1 2 d S . .
N31 N 0.68792(17) 0.9837(2) 0.03530(19) 0.0347(5) Uani 1 1 d . . .
C131 C 0.7797(6) 0.9850(6) 0.0000(5) 0.0259(12) Uani 0.50 1 d P A 1
C141 C 0.8747(5) 0.9360(5) -0.1668(5) 0.0309(12) Uiso 0.50 1 d P A 1
N81 N 0.8545(8) 0.9020(13) -0.2558(8) 0.0444(19) Uani 0.50 1 d P A 1
N91 N 1.1578(5) 0.7814(5) -0.1168(4) 0.0399(11) Uani 0.50 1 d P B 1
C17 C 0.8864(4) 0.9743(4) -0.0545(4) 0.0267(9) Uani 0.50 1 d P A 1
C132 C 0.7847(6) 1.0086(6) 0.0321(5) 0.0243(11) Uani 0.50 1 d P A 2
C142 C 0.8944(5) 0.9103(5) -0.1632(5) 0.0301(12) Uiso 0.50 1 d P B 2
N82 N 0.8250(8) 0.8984(14) -0.2320(9) 0.049(2) Uani 0.50 1 d P B 2
N92 N 1.0998(5) 0.7655(5) -0.1446(5) 0.0420(12) Uani 0.50 1 d P B 2
C18 C 0.8998(4) 1.0505(4) 0.0441(4) 0.0247(8) Uani 0.50 1 d P . 2
C19 C 0.9947(4) 0.9208(4) -0.0843(3) 0.0253(8) Uani 0.50 1 d P . 2
N1 N 0.48579(16) 0.82729(17) -0.04148(17) 0.0281(4) Uani 1 1 d . . .
N2 N 0.54087(17) 0.99502(17) -0.17203(16) 0.0279(4) Uani 1 1 d . . .
N4 N 0.58058(17) 1.06739(17) -0.25003(16) 0.0281(4) Uani 1 1 d . A .
N5 N 0.58818(17) 0.90121(17) -0.31844(17) 0.0285(4) Uani 1 1 d . . .
N6 N 0.6172(2) 0.8090(2) -0.3833(2) 0.0393(5) Uani 1 1 d . A .
N7 N 0.64845(19) 0.9858(2) -0.53194(18) 0.0359(5) Uani 1 1 d . . .
Fe01 Fe 0.5000 1.0000 0.0000 0.02555(11) Uani 1 2 d S . .
H1 H 0.433(3) 0.771(3) 0.097(3) 0.042(9) Uiso 1 1 d . . .
H1N H 0.614(3) 0.829(3) -0.452(4) 0.066(13) Uiso 1 1 d . . .
H2 H 0.400(3) 0.588(3) 0.041(3) 0.063(11) Uiso 1 1 d . . .
H2N H 0.703(3) 0.794(3) -0.356(3) 0.062(11) Uiso 1 1 d . . .
H3 H 0.446(3) 0.541(3) -0.149(3) 0.055(10) Uiso 1 1 d . . .
H4 H 0.510(3) 0.684(2) -0.269(3) 0.036(8) Uiso 1 1 d . . .
H5 H 0.685(3) 0.973(3) -0.690(3) 0.050(10) Uiso 1 1 d . . .
H6 H 0.758(4) 1.152(4) -0.708(4) 0.089(15) Uiso 1 1 d . . .
H7 H 0.767(4) 1.266(4) -0.552(4) 0.091(16) Uiso 1 1 d . . .
H8 H 0.703(3) 1.204(3) -0.382(3) 0.047(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 122.6(3) . . ?
N1 C1 H1 114(2) . . ?
C2 C1 H1 123(2) . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 H2 122(2) . . ?
C1 C2 H2 120(2) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 121(2) . . ?
C4 C3 H3 119(2) . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 H4 123.4(19) . . ?
C5 C4 H4 118.3(19) . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 C6 112.0(2) . . ?
C4 C5 C6 125.2(2) . . ?
N2 C6 N5 108.6(2) . . ?
N2 C6 C5 121.3(2) . . ?
N5 C6 C5 130.1(2) . . ?
N4 C7 N5 110.1(2) . . ?
N4 C7 C8 125.0(2) . . ?
N5 C7 C8 124.9(2) . . ?
N7 C8 C9 123.9(2) . . ?
N7 C8 C7 115.5(2) . . ?
C9 C8 C7 120.5(2) . . ?
C10 C9 C8 117.6(3) . . ?
C10 C9 H8 120(2) . . ?
C8 C9 H8 122(2) . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H7 121(3) . . ?
C9 C10 H7 119(3) . . ?
C12 C11 C10 118.2(3) . . ?
C12 C11 H6 121(3) . . ?
C10 C11 H6 120(3) . . ?
N7 C12 C11 124.3(3) . . ?
N7 C12 H5 114(2) . . ?
C11 C12 H5 122(2) . . ?
N91 C15 N92 39.1(3) . . ?
N91 C15 C18 131.8(4) . 3_775 ?
N92 C15 C18 170.6(4) . 3_775 ?
N91 C15 C19 173.7(5) . . ?
N92 C15 C19 134.8(4) . . ?
C18 C15 C19 54.4(3) 3_775 . ?
C19 C16 C19 180.0(4) 3_775 . ?
C19 C16 C18 56.0(2) 3_775 . ?
C19 C16 C18 124.0(2) . . ?
C19 C16 C18 124.0(2) 3_775 3_775 ?
C19 C16 C18 56.0(2) . 3_775 ?
C18 C16 C18 180.0(3) . 3_775 ?
C19 C16 C17 118.8(2) 3_775 . ?
C19 C16 C17 61.2(2) . . ?
C18 C16 C17 63.0(2) . . ?
C18 C16 C17 117.0(2) 3_775 . ?
C19 C16 C17 61.2(2) 3_775 3_775 ?
C19 C16 C17 118.8(2) . 3_775 ?
C18 C16 C17 117.0(2) . 3_775 ?
C18 C16 C17 63.0(2) 3_775 3_775 ?
C17 C16 C17 180.000(1) . 3_775 ?
C131 N31 C132 24.3(3) . . ?
C131 N31 Fe01 146.8(4) . . ?
C132 N31 Fe01 155.5(4) . . ?
N31 C131 C17 171.4(6) . . ?
N81 C141 C17 173.5(7) . . ?
C131 C17 C141 114.5(5) . . ?
C131 C17 C16 123.0(4) . . ?
C141 C17 C16 122.5(4) . . ?
N31 C132 C18 170.2(6) . . ?
N82 C142 C19 172.7(7) . . ?
C19 C18 C132 163.9(5) 3_775 . ?
C19 C18 C16 61.1(3) 3_775 . ?
C132 C18 C16 124.1(4) . . ?
C19 C18 C15 63.2(3) 3_775 3_775 ?
C132 C18 C15 114.8(4) . 3_775 ?
C16 C18 C15 121.0(3) . 3_775 ?
C18 C19 C16 62.8(3) 3_775 . ?
C18 C19 C15 62.5(3) 3_775 . ?
C16 C19 C15 122.0(3) . . ?
C18 C19 C142 159.2(5) 3_775 . ?
C16 C19 C142 122.3(4) . . ?
C15 C19 C142 115.7(4) . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Fe01 126.34(18) . . ?
C5 N1 Fe01 115.54(16) . . ?
C6 N2 N4 108.97(18) . . ?
C6 N2 Fe01 113.89(15) . . ?
N4 N2 Fe01 136.35(16) . . ?
C7 N4 N2 106.3(2) . . ?
C6 N5 C7 106.0(2) . . ?
C6 N5 N6 123.8(2) . . ?
C7 N5 N6 129.7(2) . . ?
N5 N6 H1N 107(3) . . ?
N5 N6 H2N 102(2) . . ?
H1N N6 H2N 111(3) . . ?
C12 N7 C8 116.4(3) . . ?
N2 Fe01 N2 180.0 3_675 . ?
N2 Fe01 N31 85.93(8) 3_675 3_675 ?
N2 Fe01 N31 94.07(8) . 3_675 ?
N2 Fe01 N31 94.07(8) 3_675 . ?
N2 Fe01 N31 85.93(8) . . ?
N31 Fe01 N31 180.00(13) 3_675 . ?
N2 Fe01 N1 76.79(8) 3_675 3_675 ?
N2 Fe01 N1 103.21(8) . 3_675 ?
N31 Fe01 N1 90.97(8) 3_675 3_675 ?
N31 Fe01 N1 89.03(8) . 3_675 ?
N2 Fe01 N1 103.21(8) 3_675 . ?
N2 Fe01 N1 76.79(8) . . ?
N31 Fe01 N1 89.03(8) 3_675 . ?
N31 Fe01 N1 90.97(8) . . ?
N1 Fe01 N1 180.0 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 1.338(3) . ?
C1 C2 1.385(4) . ?
C1 H1 0.91(3) . ?
C2 C3 1.377(5) . ?
C2 H2 0.98(4) . ?
C3 C4 1.381(4) . ?
C3 H3 0.99(4) . ?
C4 C5 1.385(4) . ?
C4 H4 0.96(3) . ?
C5 N1 1.353(3) . ?
C5 C6 1.464(3) . ?
C6 N2 1.323(3) . ?
C6 N5 1.347(3) . ?
C7 N4 1.312(3) . ?
C7 N5 1.369(3) . ?
C7 C8 1.465(3) . ?
C8 N7 1.345(3) . ?
C8 C9 1.386(4) . ?
C9 C10 1.386(4) . ?
C9 H8 0.94(3) . ?
C10 C11 1.381(5) . ?
C10 H7 0.92(5) . ?
C11 C12 1.372(5) . ?
C11 H6 0.91(4) . ?
C12 N7 1.339(3) . ?
C12 H5 0.97(3) . ?
C15 N91 1.120(6) . ?
C15 N92 1.121(6) . ?
C15 C18 1.440(5) 3_775 ?
C15 C19 1.449(5) . ?
C16 C19 1.393(5) 3_775 ?
C16 C19 1.393(5) . ?
C16 C18 1.416(4) . ?
C16 C18 1.416(4) 3_775 ?
C16 C17 1.454(4) . ?
C16 C17 1.454(4) 3_775 ?
N31 C131 1.140(8) . ?
N31 C132 1.144(7) . ?
N31 Fe01 2.169(2) . ?
C131 C17 1.403(8) . ?
C141 N81 1.148(13) . ?
C141 C17 1.412(7) . ?
C132 C18 1.407(8) . ?
C142 N82 1.120(13) . ?
C142 C19 1.450(7) . ?
C18 C19 1.320(6) 3_775 ?
C18 C15 1.440(5) 3_775 ?
C19 C18 1.320(6) 3_775 ?
N1 Fe01 2.181(2) . ?
N2 N4 1.371(3) . ?
N2 Fe01 2.1093(19) . ?
N5 N6 1.415(3) . ?
N6 H1N 0.85(4) . ?
N6 H2N 1.03(4) . ?
Fe01 N2 2.1093(19) 3_675 ?
Fe01 N31 2.169(2) 3_675 ?
Fe01 N1 2.181(2) 3_675 ?
