#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:07:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180026 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/20/7032033.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_7032033
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            'C47 H40 Fe3 N10 O9'
_chemical_formula_weight         1056.44
_chemical_name_systematic
;
  bis(m2-Cyano)-diaqua-tricyano-nitrosyl-bis(N,N'-(1,2-benzene)-
bis(salicylideneiminato)-N,N',O,O')-tri-iron(ii,iii)) methanole solvate
;
_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                99.960(3)
_cell_angle_beta                 116.960(4)
_cell_angle_gamma                105.062(3)
_cell_formula_units_Z            1
_cell_length_a                   10.8773(4)
_cell_length_b                   11.0243(4)
_cell_length_c                   11.6197(4)
_cell_measurement_reflns_used    9152
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.3066
_cell_measurement_theta_min      3.0536
_cell_volume                     1128.77(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10554
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.021
_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    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.582
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0350
_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)+(0.0553P)²+0.2833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                3407
_reflns_number_total             3948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02025a2.cif
_cod_data_source_block           ts_11_02
_cod_depositor_comments
'Adding full bibliography for 7032033--7032037.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7032033
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1520(2) 0.4622(2) 0.3416(2) 0.0116(5) Uani 1 1 d . A .
C2 C 0.0521(3) 0.4317(2) 0.2027(2) 0.0181(5) Uani 1 1 d . . .
H2 H -0.0133 0.4777 0.1750 0.022 Uiso 1 1 calc R . .
C3 C 0.0462(3) 0.3359(3) 0.1043(2) 0.0229(6) Uani 1 1 d . . .
H3 H -0.0233 0.3163 0.0099 0.027 Uiso 1 1 calc R . .
C4 C 0.1410(3) 0.2683(2) 0.1425(2) 0.0216(6) Uani 1 1 d . . .
H4 H 0.1358 0.2018 0.0746 0.026 Uiso 1 1 calc R . .
C5 C 0.2415(3) 0.2972(2) 0.2776(2) 0.0175(5) Uani 1 1 d . . .
H5 H 0.3065 0.2507 0.3027 0.021 Uiso 1 1 calc R . .
C6 C 0.2516(2) 0.3951(2) 0.3818(2) 0.0125(5) Uani 1 1 d . . .
C7 C 0.3619(2) 0.4173(2) 0.5201(2) 0.0124(5) Uani 1 1 d . . .
H7 H 0.4222 0.3662 0.5326 0.015 Uiso 1 1 calc R . .
C8 C 0.4997(2) 0.5119(2) 0.7633(2) 0.0127(5) Uani 1 1 d . . .
C9 C 0.5833(3) 0.4327(2) 0.7884(2) 0.0168(5) Uani 1 1 d . . .
H9 H 0.5664 0.3646 0.7142 0.020 Uiso 1 1 calc R . .
C10 C 0.6907(3) 0.4530(2) 0.9211(2) 0.0204(5) Uani 1 1 d . . .
H10 H 0.7473 0.3985 0.9380 0.025 Uiso 1 1 calc R . .
C11 C 0.7165(3) 0.5529(2) 1.0299(2) 0.0204(5) Uani 1 1 d . . .
H11 H 0.7918 0.5674 1.1209 0.024 Uiso 1 1 calc R . .
C12 C 0.6334(3) 0.6308(2) 1.0066(2) 0.0172(5) Uani 1 1 d . . .
H12 H 0.6515 0.6988 1.0816 0.021 Uiso 1 1 calc R . .
C13 C 0.5230(2) 0.6105(2) 0.8737(2) 0.0126(5) Uani 1 1 d . . .
C14 C 0.4269(2) 0.7650(2) 0.9332(2) 0.0143(5) Uani 1 1 d . . .
H14 H 0.5000 0.7816 1.0257 0.017 Uiso 1 1 calc R . .
C15 C 0.3296(3) 0.8360(2) 0.9113(2) 0.0142(5) Uani 1 1 d . . .
C16 C 0.3532(3) 0.9258(2) 1.0289(2) 0.0187(5) Uani 1 1 d . . .
H16 H 0.4313 0.9359 1.1168 0.022 Uiso 1 1 calc R . .
C17 C 0.2667(3) 0.9986(2) 1.0197(2) 0.0213(6) Uani 1 1 d . . .
H17 H 0.2853 1.0593 1.1000 0.026 Uiso 1 1 calc R . .
C18 C 0.1511(3) 0.9826(2) 0.8910(3) 0.0235(6) Uani 1 1 d . . .
H18 H 0.0903 1.0325 0.8838 0.028 Uiso 1 1 calc R . .
C19 C 0.1238(3) 0.8951(2) 0.7738(2) 0.0198(5) Uani 1 1 d . . .
H19 H 0.0441 0.8854 0.6869 0.024 Uiso 1 1 calc R . .
C20 C 0.2114(2) 0.8208(2) 0.7809(2) 0.0133(5) Uani 1 1 d . A .
C21 C 0.4558(3) 0.8633(2) 0.5750(2) 0.0150(5) Uani 1 1 d . A .
C22 C 0.3363(3) 0.8925(2) 0.3368(2) 0.0210(5) Uani 0.50 1 d P A 1
N4 N 0.3363(3) 0.8925(2) 0.3368(2) 0.0210(5) Uani 0.50 1 d P A 2
C23 C 0.6207(3) 0.9235(2) 0.4561(3) 0.0218(6) Uani 1 1 d . A .
Fe1 Fe 0.26950(3) 0.62433(3) 0.62866(3) 0.00965(12) Uani 1 1 d . A .
Fe2 Fe 0.5000 1.0000 0.5000 0.03557(18) Uani 1 2 d S . .
N1 N 0.38804(19) 0.50033(17) 0.63056(18) 0.0106(4) Uani 1 1 d . . .
N2 N 0.4253(2) 0.68033(17) 0.83931(18) 0.0114(4) Uani 1 1 d . . .
N3 N 0.4225(2) 0.77942(18) 0.61318(19) 0.0150(4) Uani 1 1 d . . .
O3 O 0.13180(17) 0.47272(15) 0.64802(16) 0.0126(3) Uani 1 1 d D . .
N5 N 0.2315(3) 0.8209(2) 0.2363(2) 0.0448(6) Uani 0.50 1 d P A 1
O6 O 0.2315(3) 0.8209(2) 0.2363(2) 0.0448(6) Uani 0.50 1 d P A 2
N6 N 0.6924(3) 0.8773(2) 0.4308(3) 0.0338(6) Uani 1 1 d . . .
O1 O 0.15039(17) 0.55266(15) 0.43250(15) 0.0134(3) Uani 1 1 d . . .
O2 O 0.18060(17) 0.73815(15) 0.66548(15) 0.0153(4) Uani 1 1 d . . .
H1O3 H 0.137(3) 0.3986(19) 0.634(3) 0.018 Uiso 1 1 d D . .
H2O3 H 0.043(2) 0.465(2) 0.622(2) 0.018 Uiso 1 1 d D . .
C1S C 0.9952(3) 0.8473(3) 0.3862(3) 0.0273(6) Uani 1 1 d . . .
H1C1 H 0.9868 0.9297 0.3690 0.033 Uiso 1 1 calc R . .
H2C1 H 1.0253 0.8045 0.3279 0.033 Uiso 1 1 calc R . .
H3C1 H 1.0703 0.8686 0.4828 0.033 Uiso 1 1 calc R . .
O1S O 0.85509(19) 0.75941(16) 0.3555(2) 0.0284(4) Uani 1 1 d . . .
H1O1 H 0.8017 0.8027 0.3549 0.034 Uiso 1 1 calc R . .
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'
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
O1 C1 C2 118.89(19) . .
O1 C1 C6 122.19(19) . .
C2 C1 C6 118.9(2) . .
C3 C2 C1 121.2(2) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 120.3(2) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C5 C4 C3 119.9(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 121.7(2) . .
C4 C5 H5 119.2 . .
C6 C5 H5 119.2 . .
C5 C6 C1 118.0(2) . .
C5 C6 C7 116.63(19) . .
C1 C6 C7 125.3(2) . .
N1 C7 C6 126.6(2) . .
N1 C7 H7 116.7 . .
C6 C7 H7 116.7 . .
C9 C8 C13 119.7(2) . .
C9 C8 N1 124.4(2) . .
C13 C8 N1 115.87(18) . .
C10 C9 C8 120.1(2) . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
C9 C10 C11 120.2(2) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C12 C11 C10 120.3(2) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.3(2) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C12 C13 C8 119.4(2) . .
C12 C13 N2 124.7(2) . .
C8 C13 N2 115.88(19) . .
N2 C14 C15 126.5(2) . .
N2 C14 H14 116.8 . .
C15 C14 H14 116.8 . .
C16 C15 C20 118.4(2) . .
C16 C15 C14 117.0(2) . .
C20 C15 C14 124.6(2) . .
C17 C16 C15 121.8(2) . .
C17 C16 H16 119.1 . .
C15 C16 H16 119.1 . .
C16 C17 C18 119.1(2) . .
C16 C17 H17 120.5 . .
C18 C17 H17 120.5 . .
C19 C18 C17 120.8(2) . .
C19 C18 H18 119.6 . .
C17 C18 H18 119.6 . .
C18 C19 C20 121.0(2) . .
C18 C19 H19 119.5 . .
C20 C19 H19 119.5 . .
O2 C20 C19 118.7(2) . .
O2 C20 C15 122.4(2) . .
C19 C20 C15 118.9(2) . .
N3 C21 Fe2 176.4(2) . .
N5 C22 Fe2 177.1(2) . .
N6 C23 Fe2 179.4(2) . .
O2 Fe1 O1 101.00(6) . .
O2 Fe1 O3 90.30(7) . .
O1 Fe1 O3 92.41(7) . .
O2 Fe1 N2 90.68(7) . .
O1 Fe1 N2 168.30(6) . .
O3 Fe1 N2 88.28(7) . .
O2 Fe1 N1 168.08(7) . .
O1 Fe1 N1 90.38(7) . .
O3 Fe1 N1 85.63(7) . .
N2 Fe1 N1 78.02(7) . .
O2 Fe1 N3 92.04(7) . .
O1 Fe1 N3 88.84(7) . .
O3 Fe1 N3 177.09(7) . .
N2 Fe1 N3 89.97(7) . .
N1 Fe1 N3 91.74(7) . .
N4 Fe2 C22 0.00(15) 2_676 2_676
N4 Fe2 C22 180.000(1) 2_676 .
C22 Fe2 C22 180.000(1) 2_676 .
N4 Fe2 C21 91.95(10) 2_676 .
C22 Fe2 C21 91.95(10) 2_676 .
C22 Fe2 C21 88.05(10) . .
N4 Fe2 C21 88.05(10) 2_676 2_676
C22 Fe2 C21 88.05(10) 2_676 2_676
C22 Fe2 C21 91.95(10) . 2_676
C21 Fe2 C21 180.000(1) . 2_676
N4 Fe2 C23 90.36(10) 2_676 2_676
C22 Fe2 C23 90.36(10) 2_676 2_676
C22 Fe2 C23 89.64(10) . 2_676
C21 Fe2 C23 89.54(10) . 2_676
C21 Fe2 C23 90.46(10) 2_676 2_676
N4 Fe2 C23 89.64(10) 2_676 .
C22 Fe2 C23 89.64(10) 2_676 .
C22 Fe2 C23 90.36(10) . .
C21 Fe2 C23 90.46(10) . .
C21 Fe2 C23 89.54(10) 2_676 .
C23 Fe2 C23 180.00(16) 2_676 .
C7 N1 C8 121.41(18) . .
C7 N1 Fe1 123.60(15) . .
C8 N1 Fe1 114.99(13) . .
C14 N2 C13 121.51(19) . .
C14 N2 Fe1 123.22(15) . .
C13 N2 Fe1 115.09(13) . .
C21 N3 Fe1 155.42(18) . .
Fe1 O3 H1O3 118.7(18) . .
Fe1 O3 H2O3 120.3(17) . .
H1O3 O3 H2O3 111(2) . .
C1 O1 Fe1 131.88(13) . .
C20 O2 Fe1 132.55(14) . .
O1S C1S H1C1 109.5 . .
O1S C1S H2C1 109.5 . .
H1C1 C1S H2C1 109.5 . .
O1S C1S H3C1 109.5 . .
H1C1 C1S H3C1 109.5 . .
H2C1 C1S H3C1 109.5 . .
C1S O1S H1O1 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.331(3) .
C1 C2 1.389(3) .
C1 C6 1.420(3) .
C2 C3 1.382(3) .
C2 H2 0.9500 .
C3 C4 1.383(3) .
C3 H3 0.9500 .
C4 C5 1.360(3) .
C4 H4 0.9500 .
C5 C6 1.417(3) .
C5 H5 0.9500 .
C6 C7 1.430(3) .
C7 N1 1.301(3) .
C7 H7 0.9500 .
C8 C9 1.390(3) .
C8 C13 1.404(3) .
C8 N1 1.422(3) .
C9 C10 1.380(3) .
C9 H9 0.9500 .
C10 C11 1.388(3) .
C10 H10 0.9500 .
C11 C12 1.375(3) .
C11 H11 0.9500 .
C12 C13 1.391(3) .
C12 H12 0.9500 .
C13 N2 1.424(3) .
C14 N2 1.297(3) .
C14 C15 1.434(3) .
C14 H14 0.9500 .
C15 C16 1.413(3) .
C15 C20 1.418(3) .
C16 C17 1.368(3) .
C16 H16 0.9500 .
C17 C18 1.391(3) .
C17 H17 0.9500 .
C18 C19 1.379(3) .
C18 H18 0.9500 .
C19 C20 1.394(3) .
C19 H19 0.9500 .
C20 O2 1.324(3) .
C21 N3 1.138(3) .
C21 Fe2 1.929(2) .
C22 N5 1.137(3) .
C22 Fe2 1.799(2) .
C23 N6 1.147(3) .
C23 Fe2 1.931(2) .
Fe1 O2 1.8742(15) .
Fe1 O1 1.9145(15) .
Fe1 O3 2.0548(16) .
Fe1 N2 2.1016(18) .
Fe1 N1 2.1054(17) .
Fe1 N3 2.151(2) .
Fe2 N4 1.799(2) 2_676
Fe2 C22 1.799(2) 2_676
Fe2 C21 1.929(2) 2_676
Fe2 C23 1.931(2) 2_676
O3 H1O3 0.826(16) .
O3 H2O3 0.851(16) .
C1S O1S 1.418(3) .
C1S H1C1 0.9800 .
C1S H2C1 0.9800 .
C1S H3C1 0.9800 .
O1S H1O1 0.8400 .
