#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:35:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179414 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/11/4331146.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_4331146
loop_
_publ_author_name
'Ivan Šalitroš'
'Roman Boča'
'Radovan Herchel'
'Ján Moncol'
'Ivan Nemec'
'Mario Ruben'
'Franz Renz'
_publ_section_title
;
 Mixed-Valence Heptanuclear Iron Complexes with Ferromagnetic Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12755
_journal_page_last               12767
_journal_paper_doi               10.1021/ic3015833
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C21 H25 Cl Fe N3 O4'
_chemical_formula_sum            'C21 H25 Cl Fe N3 O4'
_chemical_formula_weight         474.74
_chemical_name_systematic
;
 chlorido-(N,N'-bis(2-oxy-3-methoxy-benzylidene)
-1,6-diamino-4-azahexane)-iron(iii)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.064(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9099(7)
_cell_length_b                   20.5346(12)
_cell_length_c                   10.9418(8)
_cell_measurement_reflns_used    6706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.2808
_cell_measurement_theta_min      2.9369
_cell_volume                     2104.5(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)'
_diffrn_measurement_method
;
Rotation method data acquisition using omega and phi 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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16738
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29743
_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    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                2362
_reflns_number_total             3697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3015833_si_002_2.cif
_cod_data_source_block           2c
_cod_original_cell_volume        2104.5(2)
_cod_database_code               4331146
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.7235(3) 0.11248(14) 0.6455(3) 0.0136(7) Uani 1 1 d .
C2 C 0.6857(3) 0.05757(15) 0.5622(3) 0.0178(7) Uani 1 1 d .
C3 C 0.5938(3) 0.06337(15) 0.4381(3) 0.0232(8) Uani 1 1 d .
H3 H 0.5724 0.0263 0.3832 0.028 Uiso 1 1 calc R
C4 C 0.5319(3) 0.12288(16) 0.3922(3) 0.0275(8) Uani 1 1 d .
H4 H 0.4672 0.1262 0.3065 0.033 Uiso 1 1 calc R
C5 C 0.5632(3) 0.17676(15) 0.4693(3) 0.0211(7) Uani 1 1 d .
H5 H 0.5182 0.2171 0.4377 0.025 Uiso 1 1 calc R
C6 C 0.6621(3) 0.17312(15) 0.5959(3) 0.0146(7) Uani 1 1 d .
C7 C 0.7010(3) 0.23327(15) 0.6658(3) 0.0164(7) Uani 1 1 d .
H7 H 0.6493 0.2711 0.6276 0.020 Uiso 1 1 calc R
C8 C 0.8325(3) 0.30404(14) 0.8369(3) 0.0166(7) Uani 1 1 d .
H8A H 0.7925 0.3076 0.9086 0.020 Uiso 1 1 calc R
H8B H 0.7904 0.3389 0.7735 0.020 Uiso 1 1 calc R
C9 C 0.9927(3) 0.31085(14) 0.8881(3) 0.0192(7) Uani 1 1 d .
H9A H 1.0312 0.3133 0.8153 0.023 Uiso 1 1 calc R
H9B H 1.0194 0.3513 0.9397 0.023 Uiso 1 1 calc R
C10 C 1.2107(3) 0.25325(15) 1.0098(3) 0.0185(7) Uani 1 1 d .
H10A H 1.2473 0.2952 1.0521 0.022 Uiso 1 1 calc R
H10B H 1.2399 0.2496 0.9318 0.022 Uiso 1 1 calc R
C11 C 1.2787(3) 0.19829(14) 1.1017(3) 0.0184(7) Uani 1 1 d .
H11A H 1.2498 0.2026 1.1798 0.022 Uiso 1 1 calc R
H11B H 1.3837 0.2036 1.1291 0.022 Uiso 1 1 calc R
C12 C 1.2416(3) 0.12960(15) 1.0476(3) 0.0167(7) Uani 1 1 d .
H12A H 1.2630 0.1254 0.9656 0.020 Uiso 1 1 calc R
H12B H 1.3007 0.0975 1.1098 0.020 Uiso 1 1 calc R
C13 C 1.0580(3) 0.07534(13) 1.1003(2) 0.0138(7) Uani 1 1 d .
H13 H 1.1339 0.0513 1.1585 0.017 Uiso 1 1 calc R
C14 C 0.9155(3) 0.06346(13) 1.1036(3) 0.0126(7) Uani 1 1 d .
C15 C 0.8931(3) 0.00919(14) 1.1724(3) 0.0159(7) Uani 1 1 d .
H15 H 0.9710 -0.0187 1.2142 0.019 Uiso 1 1 calc R
C16 C 0.7607(3) -0.00418(15) 1.1803(3) 0.0180(7) Uani 1 1 d .
H16 H 0.7466 -0.0409 1.2275 0.022 Uiso 1 1 calc R
C17 C 0.6478(3) 0.03667(14) 1.1183(3) 0.0160(7) Uani 1 1 d .
H17 H 0.5555 0.0269 1.1217 0.019 Uiso 1 1 calc R
C18 C 0.6660(3) 0.09111(13) 1.0520(3) 0.0126(7) Uani 1 1 d .
C19 C 0.8027(3) 0.10754(13) 1.0462(3) 0.0122(7) Uani 1 1 d .
C20 C 0.7501(4) -0.05158(16) 0.5314(3) 0.0333(9) Uani 1 1 d .
H20A H 0.6518 -0.0637 0.4819 0.050 Uiso 1 1 calc R
H20B H 0.7994 -0.0891 0.5817 0.050 Uiso 1 1 calc R
H20C H 0.8001 -0.0378 0.4719 0.050 Uiso 1 1 calc R
C21 C 0.5133(3) 0.13927(15) 0.8599(3) 0.0203(7) Uani 1 1 d .
H21A H 0.5802 0.1698 0.8414 0.030 Uiso 1 1 calc R
H21B H 0.4160 0.1565 0.8246 0.030 Uiso 1 1 calc R
H21C H 0.5187 0.0971 0.8199 0.030 Uiso 1 1 calc R
N1 N 0.7993(2) 0.24024(11) 0.7751(2) 0.0138(5) Uani 1 1 d .
N2 N 1.0527(2) 0.25378(11) 0.9696(2) 0.0155(6) Uani 1 1 d .
H1N2 H 1.0304 0.2594 1.0452 0.019 Uiso 1 1 calc R
N3 N 1.0902(2) 0.11604(11) 1.0243(2) 0.0118(5) Uani 1 1 d .
O1 O 0.81097(19) 0.10419(9) 0.76360(17) 0.0156(5) Uani 1 1 d .
O2 O 0.82250(18) 0.16310(9) 0.99414(16) 0.0129(4) Uani 1 1 d .
O3 O 0.7489(2) 0.00059(10) 0.61669(18) 0.0215(5) Uani 1 1 d .
O4 O 0.54984(19) 0.13122(9) 0.99740(18) 0.0172(5) Uani 1 1 d .
Cl1 Cl 1.07660(7) 0.16821(4) 0.73430(6) 0.01803(18) Uani 1 1 d .
Fe1 Fe 0.93559(4) 0.16642(2) 0.87623(4) 0.01294(13) 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'
Cl Cl 0.1484 0.1585 '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
O1 C1 C6 123.8(3)
O1 C1 C2 118.7(3)
C6 C1 C2 117.5(3)
O3 C2 C3 124.6(3)
O3 C2 C1 114.3(2)
C3 C2 C1 121.2(3)
C2 C3 C4 120.5(3)
C2 C3 H3 119.7
C4 C3 H3 119.7
C5 C4 C3 120.4(3)
C5 C4 H4 119.8
C3 C4 H4 119.8
C4 C5 C6 120.5(3)
C4 C5 H5 119.7
C6 C5 H5 119.7
C5 C6 C1 119.8(3)
C5 C6 C7 117.1(3)
C1 C6 C7 123.0(3)
N1 C7 C6 125.7(3)
N1 C7 H7 117.2
C6 C7 H7 117.2
N1 C8 C9 107.8(2)
N1 C8 H8A 110.2
C9 C8 H8A 110.2
N1 C8 H8B 110.2
C9 C8 H8B 110.2
H8A C8 H8B 108.5
N2 C9 C8 108.6(2)
N2 C9 H9A 110.0
C8 C9 H9A 110.0
N2 C9 H9B 110.0
C8 C9 H9B 110.0
H9A C9 H9B 108.4
N2 C10 C11 113.6(2)
N2 C10 H10A 108.8
C11 C10 H10A 108.8
N2 C10 H10B 108.8
C11 C10 H10B 108.8
H10A C10 H10B 107.7
C10 C11 C12 115.6(2)
C10 C11 H11A 108.4
C12 C11 H11A 108.4
C10 C11 H11B 108.4
C12 C11 H11B 108.4
H11A C11 H11B 107.4
N3 C12 C11 110.3(2)
N3 C12 H12A 109.6
C11 C12 H12A 109.6
N3 C12 H12B 109.6
C11 C12 H12B 109.6
H12A C12 H12B 108.1
N3 C13 C14 125.1(3)
N3 C13 H13 117.5
C14 C13 H13 117.5
C15 C14 C19 120.4(2)
C15 C14 C13 118.3(3)
C19 C14 C13 121.1(2)
C16 C15 C14 121.0(3)
C16 C15 H15 119.5
C14 C15 H15 119.5
C15 C16 C17 119.0(3)
C15 C16 H16 120.5
C17 C16 H16 120.5
C18 C17 C16 121.7(3)
C18 C17 H17 119.1
C16 C17 H17 119.1
C17 C18 O4 118.5(2)
C17 C18 C19 120.6(3)
O4 C18 C19 120.8(2)
O2 C19 C14 122.5(2)
O2 C19 C18 120.3(2)
C14 C19 C18 117.1(2)
O3 C20 H20A 109.5
O3 C20 H20B 109.5
H20A C20 H20B 109.5
O3 C20 H20C 109.5
H20A C20 H20C 109.5
H20B C20 H20C 109.5
O4 C21 H21A 109.5
O4 C21 H21B 109.5
H21A C21 H21B 109.5
O4 C21 H21C 109.5
H21A C21 H21C 109.5
H21B C21 H21C 109.5
C7 N1 C8 121.3(3)
C7 N1 Fe1 125.2(2)
C8 N1 Fe1 113.34(18)
C9 N2 C10 111.3(2)
C9 N2 Fe1 108.64(17)
C10 N2 Fe1 118.56(16)
C9 N2 H1N2 105.8
C10 N2 H1N2 105.8
Fe1 N2 H1N2 105.8
C13 N3 C12 117.8(2)
C13 N3 Fe1 122.96(19)
C12 N3 Fe1 119.22(17)
C1 O1 Fe1 128.76(18)
C19 O2 Fe1 120.72(16)
C2 O3 C20 117.3(2)
C18 O4 C21 114.2(2)
O1 Fe1 O2 90.75(8)
O1 Fe1 N1 88.51(8)
O2 Fe1 N1 87.97(8)
O1 Fe1 N3 108.74(9)
O2 Fe1 N3 84.58(8)
N1 Fe1 N3 161.24(9)
O1 Fe1 N2 166.66(8)
O2 Fe1 N2 92.91(8)
N1 Fe1 N2 78.82(9)
N3 Fe1 N2 84.38(9)
O1 Fe1 Cl1 89.04(6)
O2 Fe1 Cl1 178.68(6)
N1 Fe1 Cl1 93.33(6)
N3 Fe1 Cl1 94.25(6)
N2 Fe1 Cl1 87.58(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.310(3)
C1 C6 1.414(4)
C1 C2 1.422(4)
C2 O3 1.369(3)
C2 C3 1.370(4)
C3 C4 1.386(4)
C3 H3 0.9500
C4 C5 1.364(4)
C4 H4 0.9500
C5 C6 1.413(4)
C5 H5 0.9500
C6 C7 1.438(4)
C7 N1 1.280(3)
C7 H7 0.9500
C8 N1 1.462(4)
C8 C9 1.508(4)
C8 H8A 0.9900
C8 H8B 0.9900
C9 N2 1.475(3)
C9 H9A 0.9900
C9 H9B 0.9900
C10 N2 1.481(3)
C10 C11 1.515(4)
C10 H10A 0.9900
C10 H10B 0.9900
C11 C12 1.527(4)
C11 H11A 0.9900
C11 H11B 0.9900
C12 N3 1.465(3)
C12 H12A 0.9900
C12 H12B 0.9900
C13 N3 1.290(3)
C13 C14 1.446(4)
C13 H13 0.9500
C14 C15 1.402(4)
C14 C19 1.416(4)
C15 C16 1.370(4)
C15 H15 0.9500
C16 C17 1.385(4)
C16 H16 0.9500
C17 C18 1.376(4)
C17 H17 0.9500
C18 O4 1.383(3)
C18 C19 1.417(4)
C19 O2 1.318(3)
C20 O3 1.423(3)
C20 H20A 0.9800
C20 H20B 0.9800
C20 H20C 0.9800
C21 O4 1.437(3)
C21 H21A 0.9800
C21 H21B 0.9800
C21 H21C 0.9800
N1 Fe1 2.090(2)
N2 Fe1 2.199(2)
N2 H1N2 0.9300
N3 Fe1 2.102(2)
O1 Fe1 1.9190(19)
O2 Fe1 1.9671(16)
Cl1 Fe1 2.4049(7)
