#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:03:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179877 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/73/7017346.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_7017346
loop_
_publ_author_name
'Herchel, Radovan'
'Pavelek, Lubomír'
'Trávníček, Zdeněk'
_publ_section_title
;
 Dinuclear and 1D iron(iii) Schiff base complexes bridged by
 4-salicylideneamino-1,2,4-triazolate: X-ray structures and magnetic
 properties.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11896
_journal_page_last               11903
_journal_paper_doi               10.1039/c1dt11127b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C52 H46 Fe2 N12 O6'
_chemical_formula_weight         1046.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.421(2)
_cell_angle_beta                 106.585(3)
_cell_angle_gamma                104.783(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1712(3)
_cell_length_b                   11.4950(3)
_cell_length_c                   13.7935(4)
_cell_measurement_reflns_used    9125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.2742
_cell_measurement_theta_min      2.9923
_cell_volume                     1148.17(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10611
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.8727
_exptl_absorpt_correction_T_min  0.7917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0475
_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)+(0.0729P)²+1.4322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                3421
_reflns_number_total             4050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11127b.txt
_cod_data_source_block           r2
_cod_original_cell_volume        1148.17(6)
_cod_database_code               7017346
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.25470(5) 0.22606(4) -0.14726(3) 0.01822(16) Uani 1 1 d .
O1 O 0.2673(3) 0.30223(18) -0.00604(16) 0.0185(4) Uani 1 1 d .
O2 O 0.2996(3) 0.3642(2) -0.20677(16) 0.0235(5) Uani 1 1 d .
O3 O -0.0082(3) 0.17948(18) -0.20560(17) 0.0222(5) Uani 1 1 d .
N1 N 0.2232(4) 0.0522(2) -0.1142(2) 0.0329(7) Uani 1 1 d .
N2 N 0.2649(4) 0.1117(3) -0.2833(2) 0.0390(8) Uani 1 1 d .
N3 N 0.4493(3) 0.7236(2) 0.0699(2) 0.0217(6) Uani 1 1 d .
N4 N 0.3392(3) 0.7862(2) 0.0991(2) 0.0218(6) Uani 1 1 d .
N5 N 0.1742(3) 0.6263(2) -0.0422(2) 0.0193(5) Uani 1 1 d .
N6 N 0.0268(3) 0.5518(2) -0.1353(2) 0.0224(6) Uani 1 1 d .
C1 C -0.1169(4) 0.2174(3) -0.2740(2) 0.0203(6) Uani 1 1 d .
C2 C -0.2395(4) 0.1316(3) -0.3704(3) 0.0283(7) Uani 1 1 d .
H2A H -0.2439 0.0463 -0.3858 0.034 Uiso 1 1 calc R
C3 C -0.3539(5) 0.1682(3) -0.4434(3) 0.0358(8) Uani 1 1 d .
H3A H -0.4355 0.1081 -0.5084 0.043 Uiso 1 1 calc R
C4 C -0.3513(4) 0.2923(3) -0.4230(3) 0.0325(8) Uani 1 1 d .
H4A H -0.4299 0.3173 -0.4738 0.039 Uiso 1 1 calc R
C5 C -0.2335(4) 0.3782(3) -0.3286(3) 0.0253(7) Uani 1 1 d .
H5A H -0.2320 0.4628 -0.3144 0.030 Uiso 1 1 calc R
C6 C -0.1156(4) 0.3434(3) -0.2528(2) 0.0194(6) Uani 1 1 d .
C7 C 0.0123(4) 0.4347(3) -0.1551(2) 0.0186(6) Uani 1 1 d .
H7A H 0.0874 0.4076 -0.1043 0.022 Uiso 1 1 calc R
C8 C 0.1767(4) 0.7267(3) 0.0303(2) 0.0202(6) Uani 1 1 d .
H8A H 0.0735 0.7501 0.0307 0.024 Uiso 1 1 calc R
C9 C 0.3474(4) 0.6282(3) -0.0150(2) 0.0206(6) Uani 1 1 d .
H9A H 0.3893 0.5698 -0.0514 0.025 Uiso 1 1 calc R
C10 C 0.2874(4) 0.2600(3) 0.0773(2) 0.0190(6) Uani 1 1 d .
C11 C 0.3334(4) 0.3454(3) 0.1764(2) 0.0239(7) Uani 1 1 d .
H11A H 0.3524 0.4319 0.1822 0.029 Uiso 1 1 calc R
C12 C 0.3517(5) 0.3057(4) 0.2659(3) 0.0342(8) Uani 1 1 d .
H12A H 0.3846 0.3651 0.3326 0.041 Uiso 1 1 calc R
C13 C 0.3222(6) 0.1787(4) 0.2588(3) 0.0413(9) Uani 1 1 d .
H13A H 0.3331 0.1517 0.3204 0.050 Uiso 1 1 calc R
C14 C 0.2779(5) 0.0939(3) 0.1636(3) 0.0384(9) Uani 1 1 d .
H14A H 0.2566 0.0075 0.1595 0.046 Uiso 1 1 calc R
C15 C 0.2626(4) 0.1312(3) 0.0710(3) 0.0279(7) Uani 1 1 d .
C16 C 0.2270(5) 0.0353(3) -0.0253(3) 0.0367(9) Uani 1 1 d .
H16A H 0.2040 -0.0487 -0.0217 0.044 Uiso 1 1 calc R
C17 C 0.1772(7) -0.0548(4) -0.2095(4) 0.0621(13) Uani 1 1 d .
H17A H 0.0465 -0.0752 -0.2521 0.074 Uiso 1 1 calc R
C18 C 0.2822(8) -0.0093(4) -0.2736(4) 0.0693(15) Uani 1 1 d .
H18A H 0.4111 0.0006 -0.2392 0.083 Uiso 1 1 calc R
H18B H 0.2360 -0.0708 -0.3446 0.083 Uiso 1 1 calc R
C19 C 0.2019(8) -0.1736(4) -0.1940(4) 0.0632(13) Uani 1 1 d .
H19A H 0.1307 -0.2048 -0.1525 0.095 Uiso 1 1 calc R
H19B H 0.3302 -0.1586 -0.1563 0.095 Uiso 1 1 calc R
H19C H 0.1611 -0.2363 -0.2630 0.095 Uiso 1 1 calc R
C20 C 0.2389(5) 0.1391(4) -0.3721(3) 0.0470(11) Uani 1 1 d .
H20A H 0.2281 0.0757 -0.4317 0.056 Uiso 1 1 calc R
C21 C 0.2250(5) 0.2549(4) -0.3890(3) 0.0386(9) Uani 1 1 d .
C22 C 0.1788(6) 0.2629(5) -0.4958(3) 0.0585(14) Uani 1 1 d .
H22A H 0.1575 0.1912 -0.5517 0.070 Uiso 1 1 calc R
C23 C 0.1648(6) 0.3707(6) -0.5186(4) 0.0601(14) Uani 1 1 d .
H23A H 0.1340 0.3741 -0.5896 0.072 Uiso 1 1 calc R
C24 C 0.1954(5) 0.4736(5) -0.4387(3) 0.0515(12) Uani 1 1 d .
H24A H 0.1866 0.5492 -0.4541 0.062 Uiso 1 1 calc R
C25 C 0.2391(4) 0.4696(4) -0.3357(3) 0.0384(9) Uani 1 1 d .
H25A H 0.2588 0.5427 -0.2816 0.046 Uiso 1 1 calc R
C26 C 0.2554(4) 0.3613(3) -0.3078(3) 0.0299(8) Uani 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'
O O 0.0106 0.0060 '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_3
O2 Fe1 O1 104.68(9) .
O2 Fe1 O3 94.73(9) .
O1 Fe1 O3 93.04(9) .
O2 Fe1 N2 87.67(11) .
O1 Fe1 N2 165.75(11) .
O3 Fe1 N2 92.99(11) .
O2 Fe1 N1 165.21(11) .
O1 Fe1 N1 89.40(10) .
O3 Fe1 N1 88.94(10) .
N2 Fe1 N1 77.82(12) .
O2 Fe1 N3 88.53(9) 2_665
O1 Fe1 N3 83.33(9) 2_665
O3 Fe1 N3 175.65(9) 2_665
N2 Fe1 N3 90.01(11) 2_665
N1 Fe1 N3 88.62(10) 2_665
C10 O1 Fe1 130.99(18) .
C26 O2 Fe1 128.7(2) .
C1 O3 Fe1 132.33(18) .
C16 N1 C17 121.9(3) .
C16 N1 Fe1 124.8(2) .
C17 N1 Fe1 113.0(3) .
C20 N2 C18 122.1(3) .
C20 N2 Fe1 123.4(3) .
C18 N2 Fe1 114.1(3) .
C9 N3 N4 107.9(2) .
C9 N3 Fe1 125.0(2) 2_665
N4 N3 Fe1 127.03(18) 2_665
C8 N4 N3 106.3(2) .
C9 N5 C8 105.3(2) .
C9 N5 N6 128.0(2) .
C8 N5 N6 125.9(2) .
C7 N6 N5 112.1(2) .
O3 C1 C2 119.9(3) .
O3 C1 C6 122.1(3) .
C2 C1 C6 117.9(3) .
C3 C2 C1 121.4(3) .
C3 C2 H2A 119.3 .
C1 C2 H2A 119.3 .
C2 C3 C4 120.7(3) .
C2 C3 H3A 119.7 .
C4 C3 H3A 119.7 .
C5 C4 C3 119.2(3) .
C5 C4 H4A 120.4 .
C3 C4 H4A 120.4 .
C4 C5 C6 121.4(3) .
C4 C5 H5A 119.3 .
C6 C5 H5A 119.3 .
C5 C6 C1 119.5(3) .
C5 C6 C7 121.3(3) .
C1 C6 C7 119.2(3) .
N6 C7 C6 121.5(3) .
N6 C7 H7A 119.2 .
C6 C7 H7A 119.2 .
N4 C8 N5 111.0(3) .
N4 C8 H8A 124.5 .
N5 C8 H8A 124.5 .
N3 C9 N5 109.5(3) .
N3 C9 H9A 125.2 .
N5 C9 H9A 125.2 .
O1 C10 C11 118.6(3) .
O1 C10 C15 122.9(3) .
C11 C10 C15 118.5(3) .
C12 C11 C10 120.9(3) .
C12 C11 H11A 119.5 .
C10 C11 H11A 119.5 .
C11 C12 C13 120.4(3) .
C11 C12 H12A 119.8 .
C13 C12 H12A 119.8 .
C14 C13 C12 119.9(3) .
C14 C13 H13A 120.0 .
C12 C13 H13A 120.0 .
C13 C14 C15 121.4(3) .
C13 C14 H14A 119.3 .
C15 C14 H14A 119.3 .
C14 C15 C10 118.8(3) .
C14 C15 C16 117.4(3) .
C10 C15 C16 123.8(3) .
N1 C16 C15 126.7(3) .
N1 C16 H16A 116.7 .
C15 C16 H16A 116.7 .
C18 C17 C19 109.3(4) .
C18 C17 N1 107.5(4) .
C19 C17 N1 118.5(4) .
C18 C17 H17A 107.0 .
C19 C17 H17A 107.0 .
N1 C17 H17A 107.0 .
N2 C18 C17 108.8(4) .
N2 C18 H18A 109.9 .
C17 C18 H18A 109.9 .
N2 C18 H18B 109.9 .
C17 C18 H18B 109.9 .
H18A C18 H18B 108.3 .
C17 C19 H19A 109.5 .
C17 C19 H19B 109.5 .
H19A C19 H19B 109.5 .
C17 C19 H19C 109.5 .
H19A C19 H19C 109.5 .
H19B C19 H19C 109.5 .
N2 C20 C21 126.3(3) .
N2 C20 H20A 116.8 .
C21 C20 H20A 116.8 .
C26 C21 C20 123.7(3) .
C26 C21 C22 118.4(4) .
C20 C21 C22 117.9(4) .
C23 C22 C21 121.6(4) .
C23 C22 H22A 119.2 .
C21 C22 H22A 119.2 .
C24 C23 C22 119.3(4) .
C24 C23 H23A 120.4 .
C22 C23 H23A 120.4 .
C23 C24 C25 120.9(5) .
C23 C24 H24A 119.6 .
C25 C24 H24A 119.6 .
C24 C25 C26 122.2(4) .
C24 C25 H25A 118.9 .
C26 C25 H25A 118.9 .
O2 C26 C25 119.1(3) .
O2 C26 C21 123.2(3) .
C25 C26 C21 117.6(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 1.929(2) .
Fe1 O1 1.933(2) .
Fe1 O3 1.951(2) .
Fe1 N2 2.104(3) .
Fe1 N1 2.105(3) .
Fe1 N3 2.211(2) 2_665
O1 C10 1.318(4) .
O2 C26 1.327(4) .
O3 C1 1.323(4) .
N1 C16 1.272(5) .
N1 C17 1.491(5) .
N2 C20 1.297(5) .
N2 C18 1.461(6) .
N3 C9 1.317(4) .
N3 N4 1.384(3) .
N3 Fe1 2.211(2) 2_665
N4 C8 1.300(4) .
N5 C9 1.350(4) .
N5 C8 1.360(4) .
N5 N6 1.410(3) .
N6 C7 1.287(4) .
C1 C2 1.401(4) .
C1 C6 1.416(4) .
C2 C3 1.377(5) .
C2 H2A 0.9500 .
C3 C4 1.392(5) .
C3 H3A 0.9500 .
C4 C5 1.374(5) .
C4 H4A 0.9500 .
C5 C6 1.403(4) .
C5 H5A 0.9500 .
C6 C7 1.444(4) .
C7 H7A 0.9500 .
C8 H8A 0.9500 .
C9 H9A 0.9500 .
C10 C11 1.399(4) .
C10 C15 1.424(4) .
C11 C12 1.381(5) .
C11 H11A 0.9500 .
C12 C13 1.395(5) .
C12 H12A 0.9500 .
C13 C14 1.359(5) .
C13 H13A 0.9500 .
C14 C15 1.410(5) .
C14 H14A 0.9500 .
C15 C16 1.449(5) .
C16 H16A 0.9500 .
C17 C18 1.476(7) .
C17 C19 1.477(6) .
C17 H17A 1.0000 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.422(6) .
C20 H20A 0.9500 .
C21 C26 1.399(5) .
C21 C22 1.441(6) .
C22 C23 1.362(7) .
C22 H22A 0.9500 .
C23 C24 1.361(7) .
C23 H23A 0.9500 .
C24 C25 1.376(5) .
C24 H24A 0.9500 .
C25 C26 1.400(5) .
C25 H25A 0.9500 .
