#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:07:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180026 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/20/7032035.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_7032035
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 Fe Mn2 N10 O11'
_chemical_formula_weight         1070.66
_chemical_name_systematic
;
bis(m-Cyano)-diaqua-tricyano-nitrosyl-bis(N,N'-ethylene-bis(3-
ethoxysalicylideneiminato)-N,N',O,O')-iron(ii)-di-manganese(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                 116.958(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2000(11)
_cell_length_b                   13.1797(8)
_cell_length_c                   14.860(2)
_cell_measurement_reflns_used    5279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.3356
_cell_measurement_theta_min      3.0697
_cell_volume                     2304.3(4)
_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  0.0943
_diffrn_reflns_av_sigmaI/netI    0.1145
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.923
_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            brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0469
_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)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                2390
_reflns_number_total             4058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02025a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7032033--7032037.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7032035
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe2 Fe 1.0000 0.0000 1.0000 0.0298(3) Uani 1 2 d S . .
Mn1 Mn 0.68099(5) 0.01952(4) 0.63857(4) 0.01312(17) Uani 1 1 d . . .
O1 O 0.5999(2) -0.10286(17) 0.60840(18) 0.0143(6) Uani 1 1 d . . .
O2 O 0.5594(2) 0.09420(17) 0.63807(18) 0.0147(6) Uani 1 1 d . . .
O3 O 0.6324(2) 0.04272(17) 0.47363(17) 0.0164(6) Uani 1 1 d . . .
H1 H 0.5811 0.0876 0.4518 0.025 Uiso 1 1 d R . .
H2 H 0.6029 -0.0112 0.4427 0.025 Uiso 1 1 d R . .
O4 O 0.4528(2) -0.24593(17) 0.57317(18) 0.0172(6) Uani 1 1 d . . .
O5 O 0.3724(2) 0.15798(18) 0.63893(19) 0.0188(6) Uani 1 1 d . . .
N1 N 0.8149(2) -0.0463(2) 0.6368(2) 0.0137(7) Uani 1 1 d . . .
N2 N 0.7804(3) 0.1407(2) 0.6738(2) 0.0152(7) Uani 1 1 d . . .
N3 N 0.7665(3) -0.0129(2) 0.8124(2) 0.0177(7) Uani 1 1 d . . .
N5 N 1.0930(3) -0.0744(2) 0.8546(2) 0.0216(8) Uani 1 1 d . . .
C1 C 0.6365(3) -0.1960(3) 0.6058(3) 0.0144(9) Uani 1 1 d . . .
C2 C 0.5571(3) -0.2759(3) 0.5862(3) 0.0137(9) Uani 1 1 d . . .
C3 C 0.5888(3) -0.3754(3) 0.5829(3) 0.0200(10) Uani 1 1 d . . .
H3 H 0.5358 -0.4286 0.5716 0.024 Uiso 1 1 calc R . .
C4 C 0.6984(3) -0.3985(3) 0.5961(3) 0.0229(10) Uani 1 1 d . . .
H4 H 0.7188 -0.4668 0.5919 0.027 Uiso 1 1 calc R . .
C5 C 0.7755(3) -0.3224(3) 0.6151(3) 0.0205(10) Uani 1 1 d . . .
H5 H 0.8501 -0.3387 0.6253 0.025 Uiso 1 1 calc R . .
C6 C 0.7464(3) -0.2189(3) 0.6197(3) 0.0157(9) Uani 1 1 d . . .
C7 C 0.8286(3) -0.1421(3) 0.6314(3) 0.0178(9) Uani 1 1 d . . .
H7 H 0.8991 -0.1640 0.6354 0.021 Uiso 1 1 calc R . .
C8 C 0.8978(3) 0.0263(3) 0.6343(3) 0.0192(9) Uani 1 1 d . . .
H8A H 0.8767 0.0463 0.5638 0.023 Uiso 1 1 calc R . .
H8B H 0.9744 -0.0047 0.6636 0.023 Uiso 1 1 calc R . .
C9 C 0.8979(3) 0.1185(3) 0.6956(3) 0.0182(9) Uani 1 1 d . . .
H9A H 0.9439 0.1047 0.7685 0.022 Uiso 1 1 calc R . .
H9B H 0.9313 0.1774 0.6773 0.022 Uiso 1 1 calc R . .
C10 C 0.7503(3) 0.2316(3) 0.6819(3) 0.0188(9) Uani 1 1 d . . .
H10 H 0.8050 0.2837 0.6948 0.023 Uiso 1 1 calc R . .
C11 C 0.6422(3) 0.2618(3) 0.6734(3) 0.0158(9) Uani 1 1 d . . .
C12 C 0.6292(4) 0.3654(3) 0.6926(3) 0.0223(10) Uani 1 1 d . . .
H12 H 0.6886 0.4121 0.7039 0.027 Uiso 1 1 calc R . .
C13 C 0.5331(4) 0.3985(3) 0.6949(3) 0.0241(10) Uani 1 1 d . . .
H13 H 0.5260 0.4678 0.7088 0.029 Uiso 1 1 calc R . .
C14 C 0.4449(4) 0.3310(3) 0.6771(3) 0.0228(10) Uani 1 1 d . . .
H14 H 0.3778 0.3544 0.6790 0.027 Uiso 1 1 calc R . .
C15 C 0.4544(3) 0.2293(3) 0.6566(3) 0.0168(9) Uani 1 1 d . . .
C16 C 0.5543(3) 0.1930(3) 0.6554(3) 0.0142(9) Uani 1 1 d . . .
C17 C 0.8504(3) -0.0100(3) 0.8855(3) 0.0148(9) Uani 1 1 d . . .
C18 C 0.2687(3) 0.1912(3) 0.6379(3) 0.0222(10) Uani 1 1 d . . .
H18A H 0.2304 0.2412 0.5830 0.027 Uiso 1 1 calc R . .
H18B H 0.2848 0.2241 0.7029 0.027 Uiso 1 1 calc R . .
C19 C 0.1936(3) 0.1005(3) 0.6213(3) 0.0278(10) Uani 1 1 d . . .
H19A H 0.2297 0.0538 0.6785 0.042 Uiso 1 1 calc R . .
H19B H 0.1822 0.0659 0.5590 0.042 Uiso 1 1 calc R . .
H19C H 0.1200 0.1225 0.6156 0.042 Uiso 1 1 calc R . .
C20 C 0.3756(3) -0.3221(3) 0.5739(3) 0.0188(9) Uani 1 1 d . . .
H20A H 0.4118 -0.3627 0.6366 0.023 Uiso 1 1 calc R . .
H20B H 0.3544 -0.3682 0.5155 0.023 Uiso 1 1 calc R . .
C21 C 0.2724(3) -0.2695(3) 0.5679(3) 0.0207(10) Uani 1 1 d . . .
H21A H 0.2321 -0.2363 0.5020 0.031 Uiso 1 1 calc R . .
H21B H 0.2952 -0.2185 0.6215 0.031 Uiso 1 1 calc R . .
H21C H 0.2221 -0.3194 0.5762 0.031 Uiso 1 1 calc R . .
C22 C 1.0619(3) -0.0439(3) 0.9100(3) 0.0183(9) Uani 1 1 d . . .
N4 N 1.0042(3) 0.2174(2) 0.9511(2) 0.0286(8) Uani 0.50 1 d P A 1
C23 C 1.0056(3) 0.1326(3) 0.9694(2) 0.0168(8) Uani 0.50 1 d P A 1
O6 O 1.0042(3) 0.2174(2) 0.9511(2) 0.0286(8) Uani 0.50 1 d P A 2
N6 N 1.0056(3) 0.1326(3) 0.9694(2) 0.0168(8) Uani 0.50 1 d P A 2
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
N6 Fe2 C23 0.0(2) 3_757 3_757
N6 Fe2 C23 180.000(1) 3_757 .
C23 Fe2 C23 180.000(1) 3_757 .
N6 Fe2 C17 90.77(15) 3_757 .
C23 Fe2 C17 90.77(15) 3_757 .
C23 Fe2 C17 89.23(15) . .
N6 Fe2 C17 89.23(15) 3_757 3_757
C23 Fe2 C17 89.23(15) 3_757 3_757
C23 Fe2 C17 90.77(15) . 3_757
C17 Fe2 C17 180.000(1) . 3_757
N6 Fe2 C22 87.89(15) 3_757 .
C23 Fe2 C22 87.89(15) 3_757 .
C23 Fe2 C22 92.11(15) . .
C17 Fe2 C22 87.39(14) . .
C17 Fe2 C22 92.61(14) 3_757 .
N6 Fe2 C22 92.11(15) 3_757 3_757
C23 Fe2 C22 92.11(15) 3_757 3_757
C23 Fe2 C22 87.89(15) . 3_757
C17 Fe2 C22 92.61(14) . 3_757
C17 Fe2 C22 87.39(14) 3_757 3_757
C22 Fe2 C22 180.00(12) . 3_757
O1 Mn1 O2 93.20(10) . .
O1 Mn1 N1 92.05(11) . .
O2 Mn1 N1 174.37(11) . .
O1 Mn1 N2 174.30(12) . .
O2 Mn1 N2 92.36(11) . .
N1 Mn1 N2 82.45(12) . .
O1 Mn1 O3 90.37(10) . .
O2 Mn1 O3 95.93(9) . .
N1 Mn1 O3 82.00(10) . .
N2 Mn1 O3 90.33(10) . .
O1 Mn1 N3 92.54(10) . .
O2 Mn1 N3 94.78(11) . .
N1 Mn1 N3 87.01(11) . .
N2 Mn1 N3 85.72(11) . .
O3 Mn1 N3 168.73(10) . .
C1 O1 Mn1 128.9(2) . .
C16 O2 Mn1 128.9(2) . .
Mn1 O3 H1 107.2 . .
Mn1 O3 H2 108.2 . .
H1 O3 H2 106.9 . .
C2 O4 C20 118.2(3) . .
C15 O5 C18 117.5(3) . .
C7 N1 C8 120.8(3) . .
C7 N1 Mn1 125.8(2) . .
C8 N1 Mn1 113.3(2) . .
C10 N2 C9 120.5(3) . .
C10 N2 Mn1 125.5(3) . .
C9 N2 Mn1 113.9(2) . .
C17 N3 Mn1 144.4(3) . .
O1 C1 C6 124.1(3) . .
O1 C1 C2 116.6(3) . .
C6 C1 C2 119.2(3) . .
O4 C2 C3 124.9(3) . .
O4 C2 C1 114.8(3) . .
C3 C2 C1 120.2(3) . .
C2 C3 C4 120.6(4) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C5 C4 C3 119.7(4) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 121.3(4) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C1 C6 C5 118.8(3) . .
C1 C6 C7 122.7(3) . .
C5 C6 C7 118.3(3) . .
N1 C7 C6 125.5(3) . .
N1 C7 H7 117.2 . .
C6 C7 H7 117.2 . .
N1 C8 C9 107.7(3) . .
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 108.4(3) . .
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 126.1(3) . .
N2 C10 H10 117.0 . .
C11 C10 H10 117.0 . .
C16 C11 C12 119.7(3) . .
C16 C11 C10 123.0(3) . .
C12 C11 C10 117.1(3) . .
C13 C12 C11 120.9(4) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C12 C13 C14 120.0(4) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C15 C14 C13 120.5(4) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
O5 C15 C14 124.3(3) . .
O5 C15 C16 115.3(3) . .
C14 C15 C16 120.4(4) . .
O2 C16 C11 124.0(3) . .
O2 C16 C15 117.5(3) . .
C11 C16 C15 118.5(3) . .
N3 C17 Fe2 173.7(3) . .
O5 C18 C19 108.3(3) . .
O5 C18 H18A 110.0 . .
C19 C18 H18A 110.0 . .
O5 C18 H18B 110.0 . .
C19 C18 H18B 110.0 . .
H18A C18 H18B 108.4 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O4 C20 C21 107.9(3) . .
O4 C20 H20A 110.1 . .
C21 C20 H20A 110.1 . .
O4 C20 H20B 110.1 . .
C21 C20 H20B 110.1 . .
H20A C20 H20B 108.4 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
N5 C22 Fe2 175.6(3) . .
N4 C23 Fe2 176.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe2 N6 1.815(4) 3_757
Fe2 C23 1.815(4) 3_757
Fe2 C23 1.815(4) .
Fe2 C17 1.940(4) .
Fe2 C17 1.940(4) 3_757
Fe2 C22 1.945(4) .
Fe2 C22 1.945(4) 3_757
Mn1 O1 1.874(2) .
Mn1 O2 1.880(2) .
Mn1 N1 1.980(3) .
Mn1 N2 1.981(3) .
Mn1 O3 2.256(2) .
Mn1 N3 2.343(3) .
O1 C1 1.326(4) .
O2 C16 1.336(4) .
O3 H1 0.8449 .
O3 H2 0.8400 .
O4 C2 1.359(4) .
O4 C20 1.433(4) .
O5 C15 1.366(4) .
O5 C18 1.430(4) .
N1 C7 1.282(5) .
N1 C8 1.467(4) .
N2 C10 1.285(5) .
N2 C9 1.463(5) .
N3 C17 1.148(4) .
N5 C22 1.146(4) .
C1 C6 1.403(5) .
C1 C2 1.419(5) .
C2 C3 1.384(5) .
C3 C4 1.402(5) .
C3 H3 0.9500 .
C4 C5 1.364(5) .
C4 H4 0.9500 .
C5 C6 1.427(5) .
C5 H5 0.9500 .
C6 C7 1.436(5) .
C7 H7 0.9500 .
C8 C9 1.518(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.431(5) .
C10 H10 0.9500 .
C11 C16 1.399(5) .
C11 C12 1.421(5) .
C12 C13 1.357(5) .
C12 H12 0.9500 .
C13 C14 1.392(5) .
C13 H13 0.9500 .
C14 C15 1.392(5) .
C14 H14 0.9500 .
C15 C16 1.411(5) .
C18 C19 1.501(5) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.494(5) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
N4 C23 1.149(4) .
