#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:07:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180026 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/20/7032034.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_7032034
loop_
_publ_author_name
'Nemec, Ivan'
'Herchel, Radovan'
'Silha, Tomáš'
'Trávníček, Zdeněk'
_publ_section_title
;
 Towards a better understanding of magnetic exchange mediated by hydrogen
 bonds in Mn(iii)/Fe(iii) salen-type supramolecular dimers.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15602
_journal_page_last               15616
_journal_paper_doi               10.1039/c4dt02025a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C45 H48 Fe3 N10 O11'
_chemical_formula_weight         1072.48
_chemical_name_systematic
;
bis(m-Cyano)-diaqua-tricyano-nitrosyl-bis(N,N'-ethylene-bis(3-
ethoxysalicylideneiminato)-N,N',O,O')-tri-iron(ii,iii))
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.407(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.0051(7)
_cell_length_b                   13.7936(4)
_cell_length_c                   14.7860(4)
_cell_measurement_reflns_used    13307
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.2886
_cell_measurement_theta_min      2.9974
_cell_volume                     4662.6(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16257
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.6888
_exptl_absorpt_correction_T_min  0.5730
_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    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0238
_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)+(0.0420P)²+0.4280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                3529
_reflns_number_total             4091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02025a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:
'__exptl_absorpt_correction_type' tag replaced with
'_exptl_absorpt_correction_type'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

 Adding full bibliography for 7032033--7032037.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7032034
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.25411(7) 0.06268(12) 0.14357(11) 0.0143(4) Uani 1 1 d .
C2 C 0.30946(7) 0.05504(13) 0.19499(11) 0.0173(4) Uani 1 1 d .
C3 C 0.33056(8) -0.03385(14) 0.22683(12) 0.0239(4) Uani 1 1 d .
H3 H 0.3680 -0.0382 0.2609 0.029 Uiso 1 1 calc R
C4 C 0.29684(8) -0.11721(14) 0.20888(12) 0.0275(4) Uani 1 1 d .
H4 H 0.3114 -0.1782 0.2310 0.033 Uiso 1 1 calc R
C5 C 0.24312(8) -0.11155(13) 0.15979(12) 0.0229(4) Uani 1 1 d .
H5 H 0.2207 -0.1689 0.1479 0.027 Uiso 1 1 calc R
C6 C 0.22029(7) -0.02179(12) 0.12631(11) 0.0164(4) Uani 1 1 d .
C7 C 0.16136(7) -0.02140(12) 0.08032(11) 0.0164(4) Uani 1 1 d .
H7 H 0.1416 -0.0819 0.0738 0.020 Uiso 1 1 calc R
C8 C 0.07137(7) 0.04553(12) 0.01216(12) 0.0160(4) Uani 1 1 d .
H8A H 0.0466 0.0551 0.0621 0.019 Uiso 1 1 calc R
H8B H 0.0633 -0.0198 -0.0140 0.019 Uiso 1 1 calc R
C9 C 0.05740(7) 0.12236(12) -0.06067(12) 0.0175(4) Uani 1 1 d .
H9A H 0.0717 0.1014 -0.1183 0.021 Uiso 1 1 calc R
H9B H 0.0146 0.1320 -0.0720 0.021 Uiso 1 1 calc R
C10 C 0.06165(7) 0.29531(12) -0.04710(11) 0.0150(4) Uani 1 1 d .
H10 H 0.0229 0.2945 -0.0771 0.018 Uiso 1 1 calc R
C11 C 0.08770(7) 0.38943(12) -0.02586(11) 0.0147(4) Uani 1 1 d .
C12 C 0.05452(8) 0.47157(13) -0.05549(12) 0.0208(4) Uani 1 1 d .
H12 H 0.0161 0.4635 -0.0853 0.025 Uiso 1 1 calc R
C13 C 0.07707(8) 0.56293(13) -0.04173(12) 0.0236(4) Uani 1 1 d .
H13 H 0.0538 0.6175 -0.0613 0.028 Uiso 1 1 calc R
C14 C 0.13344(8) 0.57682(13) 0.00042(11) 0.0210(4) Uani 1 1 d .
H14 H 0.1487 0.6406 0.0091 0.025 Uiso 1 1 calc R
C15 C 0.16737(7) 0.49775(12) 0.02969(11) 0.0154(4) Uani 1 1 d .
C16 C 0.14512(7) 0.40251(12) 0.01770(11) 0.0138(4) Uani 1 1 d .
C17 C 0.39377(7) 0.14231(15) 0.26330(12) 0.0243(4) Uani 1 1 d .
H17A H 0.4231 0.1099 0.2295 0.029 Uiso 1 1 calc R
H17B H 0.3919 0.1077 0.3215 0.029 Uiso 1 1 calc R
C18 C 0.41011(9) 0.24656(16) 0.28067(14) 0.0319(5) Uani 1 1 d .
H18A H 0.4043 0.2828 0.2234 0.048 Uiso 1 1 calc R
H18B H 0.4513 0.2507 0.3060 0.048 Uiso 1 1 calc R
H18C H 0.3854 0.2743 0.3240 0.048 Uiso 1 1 calc R
C19 C 0.24780(8) 0.59522(13) 0.09523(12) 0.0233(4) Uani 1 1 d .
H19A H 0.2226 0.6299 0.1347 0.028 Uiso 1 1 calc R
H19B H 0.2505 0.6346 0.0399 0.028 Uiso 1 1 calc R
C20 C 0.30735(8) 0.57981(14) 0.14471(13) 0.0294(5) Uani 1 1 d .
H20A H 0.3044 0.5387 0.1981 0.044 Uiso 1 1 calc R
H20B H 0.3244 0.6425 0.1644 0.044 Uiso 1 1 calc R
H20C H 0.3324 0.5481 0.1041 0.044 Uiso 1 1 calc R
C21 C 0.07352(7) 0.21055(11) 0.19900(11) 0.0122(3) Uani 1 1 d .
C22 C 0.0000 0.07715(18) 0.2500 0.0157(5) Uani 1 2 d S
C23 C 0.03969(7) 0.20283(11) 0.37295(12) 0.0143(4) Uani 1 1 d .
N1 N 0.13356(6) 0.05374(10) 0.04757(9) 0.0139(3) Uani 1 1 d .
N2 N 0.08612(6) 0.21353(10) -0.02915(9) 0.0125(3) Uani 1 1 d .
O6 O 0.19842(5) 0.17533(9) -0.07742(8) 0.0153(3) Uani 1 1 d D
N4 N 0.11573(6) 0.21008(10) 0.16425(9) 0.0138(3) Uani 1 1 d .
N5 N 0.06216(7) 0.19378(10) 0.44589(10) 0.0198(3) Uani 1 1 d .
N6 N 0.0000 -0.00578(16) 0.2500 0.0260(5) Uani 1 2 d S
N7 N 0.0000 0.33833(15) 0.2500 0.0149(4) Uani 1 2 d S
O1 O 0.23627(5) 0.15024(8) 0.11609(8) 0.0145(3) Uani 1 1 d .
O2 O 0.17966(5) 0.33006(8) 0.04667(7) 0.0130(2) Uani 1 1 d .
O3 O 0.33762(5) 0.14203(9) 0.21065(8) 0.0199(3) Uani 1 1 d .
O4 O 0.22352(5) 0.50151(8) 0.07096(8) 0.0182(3) Uani 1 1 d .
O5 O 0.0000 0.42106(13) 0.2500 0.0294(4) Uani 1 2 d S
Fe1 Fe 0.166072(10) 0.194717(17) 0.050908(15) 0.01064(8) Uani 1 1 d .
Fe2 Fe 0.0000 0.21845(2) 0.2500 0.01101(9) Uani 1 2 d S
H1O6 H 0.2025(8) 0.2297(8) -0.1011(11) 0.013 Uiso 1 1 d D
H2O6 H 0.2293(5) 0.1436(11) -0.0708(12) 0.013 Uiso 1 1 d 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_1
_geom_angle_site_symmetry_3
O1 C1 C6 123.56(15) . .
O1 C1 C2 117.58(15) . .
C6 C1 C2 118.84(15) . .
O3 C2 C3 125.29(16) . .
O3 C2 C1 113.97(14) . .
C3 C2 C1 120.73(17) . .
C2 C3 C4 119.96(17) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.36(17) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C6 121.07(18) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C1 C6 C5 119.03(16) . .
C1 C6 C7 123.47(15) . .
C5 C6 C7 117.39(16) . .
N1 C7 C6 125.55(16) . .
N1 C7 H7 117.2 . .
C6 C7 H7 117.2 . .
N1 C8 C9 108.59(13) . .
N1 C8 H8A 110.0 . .
C9 C8 H8A 110.0 . .
N1 C8 H8B 110.0 . .
C9 C8 H8B 110.0 . .
H8A C8 H8B 108.4 . .
N2 C9 C8 108.62(13) . .
N2 C9 H9A 110.0 . .
C8 C9 H9A 110.0 . .
N2 C9 H9B 110.0 . .
C8 C9 H9B 110.0 . .
H9A C9 H9B 108.3 . .
N2 C10 C11 125.79(15) . .
N2 C10 H10 117.1 . .
C11 C10 H10 117.1 . .
C12 C11 C16 119.02(16) . .
C12 C11 C10 117.15(15) . .
C16 C11 C10 123.72(15) . .
C13 C12 C11 120.72(17) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C12 C13 C14 120.89(17) . .
C12 C13 H13 119.6 . .
C14 C13 H13 119.6 . .
C15 C14 C13 119.89(17) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
O4 C15 C14 125.62(16) . .
O4 C15 C16 113.72(15) . .
C14 C15 C16 120.66(16) . .
O2 C16 C15 117.84(15) . .
O2 C16 C11 123.33(15) . .
C15 C16 C11 118.82(15) . .
O3 C17 C18 106.80(15) . .
O3 C17 H17A 110.4 . .
C18 C17 H17A 110.4 . .
O3 C17 H17B 110.4 . .
C18 C17 H17B 110.4 . .
H17A C17 H17B 108.6 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O4 C19 C20 107.68(15) . .
O4 C19 H19A 110.2 . .
C20 C19 H19A 110.2 . .
O4 C19 H19B 110.2 . .
C20 C19 H19B 110.2 . .
H19A C19 H19B 108.5 . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
N4 C21 Fe2 175.43(14) . .
N6 C22 Fe2 180.0 . .
N5 C23 Fe2 178.86(15) . .
C7 N1 C8 119.71(14) . .
C7 N1 Fe1 125.62(12) . .
C8 N1 Fe1 114.37(10) . .
C10 N2 C9 121.17(14) . .
C10 N2 Fe1 124.61(11) . .
C9 N2 Fe1 114.14(10) . .
Fe1 O6 H1O6 109.1(13) . .
Fe1 O6 H2O6 109.9(12) . .
H1O6 O6 H2O6 112.8(18) . .
C21 N4 Fe1 154.81(12) . .
O5 N7 Fe2 180.0 . .
C1 O1 Fe1 132.12(11) . .
C16 O2 Fe1 131.45(11) . .
C2 O3 C17 118.34(13) . .
C15 O4 C19 117.84(14) . .
O1 Fe1 O2 101.66(5) . .
O1 Fe1 N1 89.61(5) . .
O2 Fe1 N1 168.36(5) . .
O1 Fe1 N2 167.99(5) . .
O2 Fe1 N2 89.82(5) . .
N1 Fe1 N2 79.13(5) . .
O1 Fe1 O6 92.86(5) . .
O2 Fe1 O6 91.08(5) . .
N1 Fe1 O6 91.26(5) . .
N2 Fe1 O6 83.33(5) . .
O1 Fe1 N4 97.96(5) . .
O2 Fe1 N4 91.94(5) . .
N1 Fe1 N4 83.53(5) . .
N2 Fe1 N4 84.99(5) . .
O6 Fe1 N4 167.93(5) . .
N7 Fe2 C21 93.23(5) . .
N7 Fe2 C21 93.23(5) . 2
C21 Fe2 C21 173.53(10) . 2
N7 Fe2 C22 180.0 . .
C21 Fe2 C22 86.77(5) . .
C21 Fe2 C22 86.77(5) 2 .
N7 Fe2 C23 96.33(5) . 2
C21 Fe2 C23 88.23(7) . 2
C21 Fe2 C23 91.06(7) 2 2
C22 Fe2 C23 83.67(5) . 2
N7 Fe2 C23 96.33(5) . .
C21 Fe2 C23 91.06(7) . .
C21 Fe2 C23 88.23(7) 2 .
C22 Fe2 C23 83.67(5) . .
C23 Fe2 C23 167.33(9) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.3246(19) .
C1 C6 1.408(2) .
C1 C2 1.412(2) .
C2 O3 1.371(2) .
C2 C3 1.382(2) .
C3 C4 1.396(3) .
C3 H3 0.9500 .
C4 C5 1.364(3) .
C4 H4 0.9500 .
C5 C6 1.413(2) .
C5 H5 0.9500 .
C6 C7 1.447(2) .
C7 N1 1.284(2) .
C7 H7 0.9500 .
C8 N1 1.472(2) .
C8 C9 1.520(2) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 N2 1.472(2) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 N2 1.275(2) .
C10 C11 1.450(2) .
C10 H10 0.9500 .
C11 C12 1.408(2) .
C11 C16 1.415(2) .
C12 C13 1.369(3) .
C12 H12 0.9500 .
C13 C14 1.388(3) .
C13 H13 0.9500 .
C14 C15 1.382(2) .
C14 H14 0.9500 .
C15 O4 1.367(2) .
C15 C16 1.414(2) .
C16 O2 1.3181(19) .
C17 O3 1.432(2) .
C17 C18 1.501(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 O4 1.438(2) .
C19 C20 1.495(3) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 N4 1.148(2) .
C21 Fe2 1.9302(17) .
C22 N6 1.144(3) .
C22 Fe2 1.949(2) .
C23 N5 1.150(2) .
C23 Fe2 1.9530(18) .
N1 Fe1 2.0821(14) .
N2 Fe1 2.0894(14) .
O6 Fe1 2.1309(12) .
O6 H1O6 0.837(9) .
O6 H2O6 0.832(9) .
N4 Fe1 2.1512(14) .
N7 O5 1.141(3) .
N7 Fe2 1.654(2) .
O1 Fe1 1.8884(11) .
O2 Fe1 1.8950(11) .
Fe2 C21 1.9302(17) 2
Fe2 C23 1.9530(18) 2
