# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ts_11_02

_audit_creation_method           SHELXL-97
_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
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H40 Fe3 N10 O9'
_chemical_formula_weight         1056.44

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8773(4)
_cell_length_b                   11.0243(4)
_cell_length_c                   11.6197(4)
_cell_angle_alpha                99.960(3)
_cell_angle_beta                 116.960(4)
_cell_angle_gamma                105.062(3)
_cell_volume                     1128.77(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9152
_cell_measurement_theta_min      3.0536
_cell_measurement_theta_max      33.3066

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             542
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.6888
_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_special_details           
;
 face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_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_detector_area_resol_mean 8.3611
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10554
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3948
_reflns_number_gt                3407
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0553P)²+0.2833P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3948
_refine_ls_number_parameters     320
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 . ?

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
_geom_angle_publ_flag
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 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.582
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 998967'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelx

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(m-Cyano)-diaqua-tricyano-nitrosyl-bis(N,N'-ethylene-bis(3-
ethoxysalicylideneiminato)-N,N',O,O')-tri-iron(ii,iii))
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H48 Fe3 N10 O11'
_chemical_formula_weight         1072.48

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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'

_cell_length_a                   23.0051(7)
_cell_length_b                   13.7936(4)
_cell_length_c                   14.7860(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.407(3)
_cell_angle_gamma                90.00
_cell_volume                     4662.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13307
_cell_measurement_theta_min      2.9974
_cell_measurement_theta_max      33.2886

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    0.993
__exptl_absorpt_correction_type  multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.6888
_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_special_details           
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_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_detector_area_resol_mean 8.3611
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16257
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4091
_reflns_number_gt                3529
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0420P)²+0.4280P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4091
_refine_ls_number_parameters     322
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.25411(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 . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 ?

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
_geom_angle_publ_flag
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 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 998968'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelx

_audit_creation_method           SHELXL-97
_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))
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H48 Fe Mn2 N10 O11'
_chemical_formula_weight         1070.66

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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'

_cell_length_a                   13.2000(11)
_cell_length_b                   13.1797(8)
_cell_length_c                   14.860(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.958(8)
_cell_angle_gamma                90.00
_cell_volume                     2304.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5279
_cell_measurement_theta_min      3.0697
_cell_measurement_theta_max      33.3356

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.6888
_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_special_details           
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_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_detector_area_resol_mean 8.3611
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18371
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_sigmaI/netI    0.1145
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4058
_reflns_number_gt                2390
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4058
_refine_ls_number_parameters     315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0890
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_restrained_S_all      0.875
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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) . ?

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
_geom_angle_publ_flag
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) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 998969'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(m2-Cyano)-diaqua-tricyano-nitrosyl-bis(N,N'-(1,2-propylene-bis(3-
ethoxysalicylideneiminato)-N,N',O,O')-tri-iron(ii,iii))
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H52 Fe3 N10 O11'
_chemical_formula_weight         1100.54

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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'

_cell_length_a                   13.651(5)
_cell_length_b                   13.387(5)
_cell_length_c                   15.434(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.29(2)
_cell_angle_gamma                90.00
_cell_volume                     2435.5(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12035
_cell_measurement_theta_min      2.9832
_cell_measurement_theta_max      33.3691

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.6888
_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_special_details           
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_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_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19415
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.043
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4240
_reflns_number_gt                3360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0581P)²+0.4420P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4240
_refine_ls_number_parameters     364
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0861
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.36933(17) 0.79600(14) 0.39883(14) 0.0172(4) Uani 1 1 d . . . . .
C2 C 0.44785(17) 0.71915(14) 0.41671(15) 0.0192(5) Uani 1 1 d . . . . .
C3 C 0.42411(19) 0.62129(15) 0.42646(16) 0.0267(5) Uani 1 1 d . . . . .
H3 H 0.4777 0.5703 0.4379 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3208(2) 0.59724(16) 0.41947(17) 0.0301(6) Uani 1 1 d . . . . .
H4 H 0.3044 0.5298 0.4266 0.036 Uiso 1 1 calc R U . . .
C5 C 0.24346(19) 0.67007(15) 0.40251(17) 0.0275(5) Uani 1 1 d . . . . .
H5 H 0.1734 0.6525 0.3976 0.033 Uiso 1 1 calc R U . . .
C6 C 0.26515(17) 0.77090(15) 0.39214(16) 0.0210(5) Uani 1 1 d . . . . .
C7 C 0.18089(18) 0.84347(16) 0.37853(17) 0.0258(5) Uani 1 1 d . . . . .
H7 H 0.1149 0.8192 0.3775 0.031 Uiso 1 1 calc R U . . .
C8A C 0.1106(5) 1.0115(5) 0.3811(5) 0.0257(14) Uani 0.538(5) 1 d D . P A 1
H8A H 0.1528 1.0354 0.4521 0.031 Uiso 0.538(5) 1 calc R U P A 1
C9B C 0.1272(5) 1.1040(4) 0.3737(6) 0.0254(14) Uani 0.462(5) 1 d D . P A 2
H9B H 0.1637 1.1039 0.4485 0.030 Uiso 0.462(5) 1 calc R U P A 2
C9A C 0.0946(4) 1.1001(3) 0.3141(5) 0.0221(11) Uani 0.538(5) 1 d . . P A 1
H9A1 H 0.0501 1.0810 0.2425 0.027 Uiso 0.538(5) 1 calc R U P A 1
H9A2 H 0.0552 1.1554 0.3267 0.027 Uiso 0.538(5) 1 calc R U P A 1
C10 C 0.23193(18) 1.22077(16) 0.32895(17) 0.0273(5) Uani 1 1 d . . . . .
H10 H 0.1758 1.2686 0.3192 0.033 Uiso 1 1 calc R U . . .
C11 C 0.33062(17) 1.25716(15) 0.32746(15) 0.0203(5) Uani 1 1 d . . . . .
C12 C 0.33229(19) 1.35960(16) 0.30647(16) 0.0280(5) Uani 1 1 d . . . . .
H12 H 0.2710 1.4013 0.2963 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4208(2) 1.39953(16) 0.30059(17) 0.0303(5) Uani 1 1 d . . . . .
H13 H 0.4200 1.4683 0.2852 0.036 Uiso 1 1 calc R U . . .
C14 C 0.51214(19) 1.33990(15) 0.31710(16) 0.0272(5) Uani 1 1 d . . . . .
H14 H 0.5739 1.3683 0.3137 0.033 Uiso 1 1 calc R U . . .
C15 C 0.51321(17) 1.23942(14) 0.33848(15) 0.0208(5) Uani 1 1 d . . . . .
C16 C 0.42180(16) 1.19627(14) 0.34353(14) 0.0173(4) Uani 1 1 d . . . . .
C17A C -0.0035(4) 0.9674(3) 0.3615(4) 0.0354(13) Uani 0.538(5) 1 d D . P A 1
H17A H 0.0094 0.9264 0.4189 0.053 Uiso 0.538(5) 1 calc R U P A 1
H17B H -0.0363 0.9260 0.3009 0.053 Uiso 0.538(5) 1 calc R U P A 1
H17C H -0.0559 1.0218 0.3523 0.053 Uiso 0.538(5) 1 calc R U P A 1
C18 C 0.69488(18) 1.21487(17) 0.35497(17) 0.0288(5) Uani 1 1 d . . . . .
H18A H 0.7342 1.2630 0.4108 0.035 Uiso 1 1 calc R U . . .
H18B H 0.6716 1.2502 0.2911 0.035 Uiso 1 1 calc R U . . .
C19 C 0.7720(2) 1.12981(19) 0.3676(2) 0.0402(6) Uani 1 1 d . . . . .
H19A H 0.7859 1.0898 0.4259 0.060 Uiso 1 1 calc R U . . .
H19B H 0.8442 1.1559 0.3778 0.060 Uiso 1 1 calc R U . . .
H19C H 0.7365 1.0879 0.3073 0.060 Uiso 1 1 calc R U . . .
C20B C 0.62031(19) 0.67679(15) 0.41980(17) 0.0272(5) Uani 1 1 d . . . . .
H20A H 0.5790 0.6352 0.3587 0.033 Uiso 1 1 calc R U . . .
H20B H 0.6492 0.6328 0.4793 0.033 Uiso 1 1 calc R U . . .
C21 C 0.71662(19) 0.73000(17) 0.41961(18) 0.0309(5) Uani 1 1 d . . . . .
H21C H 0.6866 0.7806 0.3664 0.046 Uiso 1 1 calc R U . . .
H21A H 0.7625 0.6818 0.4076 0.046 Uiso 1 1 calc R U . . .
H21B H 0.7638 0.7625 0.4847 0.046 Uiso 1 1 calc R U . . .
C22 C 0.14238(19) 0.99046(14) 0.12518(17) 0.0206(5) Uani 1 1 d . . . . .
C23 C 0.07576(17) 1.04253(15) -0.06794(16) 0.0205(5) Uani 1 1 d . . . . .
Fe1 Fe 0.31978(2) 1.01039(2) 0.36375(2) 0.01577(11) Uani 1 1 d . . . . .
Fe2 Fe 0.0000 1.0000 0.0000 0.03241(15) Uani 1 2 d S . P . .
N1 N 0.18641(14) 0.93794(12) 0.36762(13) 0.0239(4) Uani 1 1 d D . . . .
N2 N 0.21304(14) 1.13014(12) 0.34224(15) 0.0264(4) Uani 1 1 d D . . . .
N3 N 0.22292(15) 0.98987(12) 0.20281(14) 0.0224(4) Uani 1 1 d . . . . .
N4 N 0.11928(16) 1.07073(14) -0.10999(15) 0.0315(5) Uani 1 1 d . . . . .
O1 O 0.39712(11) 0.88761(9) 0.38855(10) 0.0186(3) Uani 1 1 d . . . . .
O2 O 0.42740(11) 1.09949(9) 0.36379(10) 0.0181(3) Uani 1 1 d . . . . .
O3 O 0.38337(12) 1.03022(11) 0.52106(11) 0.0210(3) Uani 1 1 d D . . . .
O4 O 0.54600(11) 0.75144(9) 0.42232(11) 0.0216(3) Uani 1 1 d . . . . .
O5 O 0.59746(11) 1.17440(10) 0.35454(11) 0.0252(3) Uani 1 1 d . . . . .
C17B C 0.0266(4) 1.1780(4) 0.3264(4) 0.0376(16) Uani 0.462(5) 1 d D . P A 2
H17D H -0.0282 1.1604 0.3473 0.056 Uiso 0.462(5) 1 calc R U P A 2
H17E H 0.0545 1.2460 0.3487 0.056 Uiso 0.462(5) 1 calc R U P A 2
H17F H -0.0104 1.1745 0.2531 0.056 Uiso 0.462(5) 1 calc R U P A 2
C8B C 0.0840(6) 1.0001(6) 0.3312(6) 0.0261(16) Uani 0.462(5) 1 d D . P A 2
H8B1 H 0.0343 0.9738 0.3554 0.031 Uiso 0.462(5) 1 calc R U P A 2
H8B2 H 0.0406 1.0019 0.2569 0.031 Uiso 0.462(5) 1 calc R U P A 2
N5 N -0.00971(16) 1.21275(15) 0.05134(16) 0.0479(5) Uani 0.5 1 d . . P B 1
C24 C -0.00847(16) 1.13117(15) 0.03050(15) 0.0265(5) Uani 0.5 1 d . . P B 1
O6 O -0.00971(16) 1.21275(15) 0.05134(16) 0.0479(5) Uani 0.5 1 d . . P B 2
N6 N -0.00847(16) 1.13117(15) 0.03050(15) 0.0265(5) Uani 0.5 1 d . . P B 2
H1O3 H 0.4263(16) 1.0782(12) 0.5458(17) 0.032 Uiso 1 1 d D U . . .
H2O3 H 0.4140(18) 0.9772(11) 0.5526(17) 0.032 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.317(2) . ?
C1 C2 1.409(3) . ?
C1 C6 1.414(3) . ?
C2 O4 1.368(2) . ?
C2 C3 1.376(3) . ?
C3 C4 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.408(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.438(3) . ?
C7 N1 1.283(3) . ?
C7 H7 0.9500 . ?
C8A C9A 1.515(9) . ?
C8A N1 1.517(7) . ?
C8A C17A 1.546(7) . ?
C8A H8A 1.0000 . ?
C9B N2 1.519(6) . ?
C9B C8B 1.524(10) . ?
C9B C17B 1.546(7) . ?
C9B H9B 1.0000 . ?
C9A N2 1.502(5) . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
C10 N2 1.278(3) . ?
C10 C11 1.444(3) . ?
C10 H10 0.9500 . ?
C11 C16 1.401(3) . ?
C11 C12 1.412(3) . ?
C12 C13 1.366(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 O5 1.362(2) . ?
C15 C16 1.412(3) . ?
C16 O2 1.326(2) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C18 O5 1.433(2) . ?
C18 C19 1.495(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20B O4 1.438(2) . ?
C20B C21 1.497(3) . ?
C20B H20A 0.9900 . ?
C20B H20B 0.9900 . ?
C21 H21C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 N3 1.147(3) . ?
C22 Fe2 1.934(2) . ?
C23 N4 1.143(3) . ?
C23 Fe2 1.894(2) . ?
Fe1 O1 1.8854(14) . ?
Fe1 O2 1.8921(14) . ?
Fe1 N2 2.0773(17) . ?
Fe1 N1 2.0901(18) . ?
Fe1 O3 2.1430(16) . ?
Fe1 N3 2.164(2) . ?
Fe2 N6 1.837(2) 3_575 ?
Fe2 C24 1.837(2) 3_575 ?
Fe2 C24 1.837(2) . ?
Fe2 C23 1.894(2) 3_575 ?
Fe2 C22 1.934(2) 3_575 ?
N1 C8B 1.474(7) . ?
O3 H1O3 0.822(10) . ?
O3 H2O3 0.843(10) . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
N5 C24 1.141(3) . ?

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
_geom_angle_publ_flag
O1 C1 C2 117.83(17) . . ?
O1 C1 C6 123.57(18) . . ?
C2 C1 C6 118.60(17) . . ?
O4 C2 C3 124.81(18) . . ?
O4 C2 C1 113.93(16) . . ?
C3 C2 C1 121.25(19) . . ?
C2 C3 C4 119.7(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.30(19) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 118.75(19) . . ?
C5 C6 C7 117.76(19) . . ?
C1 C6 C7 123.46(18) . . ?
N1 C7 C6 126.13(19) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
C9A C8A N1 106.7(4) . . ?
C9A C8A C17A 112.5(5) . . ?
N1 C8A C17A 114.5(4) . . ?
C9A C8A H8A 107.6 . . ?
N1 C8A H8A 107.6 . . ?
C17A C8A H8A 107.6 . . ?
N2 C9B C8B 105.4(5) . . ?
N2 C9B C17B 110.3(4) . . ?
C8B C9B C17B 108.8(5) . . ?
N2 C9B H9B 110.7 . . ?
C8B C9B H9B 110.7 . . ?
C17B C9B H9B 110.7 . . ?
N2 C9A C8A 104.4(4) . . ?
N2 C9A H9A1 110.9 . . ?
C8A C9A H9A1 110.9 . . ?
N2 C9A H9A2 110.9 . . ?
C8A C9A H9A2 110.9 . . ?
H9A1 C9A H9A2 108.9 . . ?
N2 C10 C11 126.03(19) . . ?
N2 C10 H10 117.0 . . ?
C11 C10 H10 117.0 . . ?
C16 C11 C12 119.34(19) . . ?
C16 C11 C10 123.62(18) . . ?
C12 C11 C10 117.03(19) . . ?
C13 C12 C11 120.8(2) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 120.3(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.2(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
O5 C15 C14 124.84(19) . . ?
O5 C15 C16 114.65(17) . . ?
C14 C15 C16 120.50(19) . . ?
O2 C16 C11 123.40(18) . . ?
O2 C16 C15 117.72(17) . . ?
C11 C16 C15 118.88(18) . . ?
C8A C17A H17A 109.5 . . ?
C8A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
C8A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
O5 C18 C19 107.67(18) . . ?
O5 C18 H18A 110.2 . . ?
C19 C18 H18A 110.2 . . ?
O5 C18 H18B 110.2 . . ?
C19 C18 H18B 110.2 . . ?
H18A C18 H18B 108.5 . . ?
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 C20B C21 107.55(16) . . ?
O4 C20B H20A 110.2 . . ?
C21 C20B H20A 110.2 . . ?
O4 C20B H20B 110.2 . . ?
C21 C20B H20B 110.2 . . ?
H20A C20B H20B 108.5 . . ?
C20B C21 H21C 109.5 . . ?
C20B C21 H21A 109.5 . . ?
H21C C21 H21A 109.5 . . ?
C20B C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C22 Fe2 174.31(18) . . ?
N4 C23 Fe2 177.85(19) . . ?
O1 Fe1 O2 101.20(6) . . ?
O1 Fe1 N2 168.81(6) . . ?
O2 Fe1 N2 89.74(7) . . ?
O1 Fe1 N1 89.79(6) . . ?
O2 Fe1 N1 168.49(6) . . ?
N2 Fe1 N1 79.15(7) . . ?
O1 Fe1 O3 90.73(6) . . ?
O2 Fe1 O3 92.91(6) . . ?
N2 Fe1 O3 86.34(7) . . ?
N1 Fe1 O3 83.46(7) . . ?
O1 Fe1 N3 94.46(6) . . ?
O2 Fe1 N3 96.04(6) . . ?
N2 Fe1 N3 86.63(7) . . ?
N1 Fe1 N3 86.39(7) . . ?
O3 Fe1 N3 168.58(6) . . ?
C24 Fe2 C24 180.00(13) 3_575 . ?
N6 Fe2 C23 88.68(9) 3_575 3_575 ?
C24 Fe2 C23 88.68(9) 3_575 3_575 ?
C24 Fe2 C23 91.32(9) . 3_575 ?
N6 Fe2 C23 91.32(9) 3_575 . ?
C24 Fe2 C23 91.32(9) 3_575 . ?
C24 Fe2 C23 88.69(9) . . ?
C23 Fe2 C23 180.0 3_575 . ?
N6 Fe2 C22 88.20(8) 3_575 3_575 ?
C24 Fe2 C22 88.20(8) 3_575 3_575 ?
C24 Fe2 C22 91.80(8) . 3_575 ?
C23 Fe2 C22 91.07(9) 3_575 3_575 ?
C23 Fe2 C22 88.93(9) . 3_575 ?
N6 Fe2 C22 91.80(8) 3_575 . ?
C24 Fe2 C22 91.80(8) 3_575 . ?
C24 Fe2 C22 88.20(8) . . ?
C23 Fe2 C22 88.93(9) 3_575 . ?
C23 Fe2 C22 91.07(9) . . ?
C22 Fe2 C22 180.0 3_575 . ?
C7 N1 C8B 120.0(3) . . ?
C7 N1 C8A 122.2(3) . . ?
C7 N1 Fe1 124.80(15) . . ?
C8B N1 Fe1 113.5(3) . . ?
C8A N1 Fe1 111.5(2) . . ?
C10 N2 C9A 118.8(2) . . ?
C10 N2 C9B 121.4(3) . . ?
C10 N2 Fe1 125.18(15) . . ?
C9A N2 Fe1 113.9(2) . . ?
C9B N2 Fe1 111.3(2) . . ?
C22 N3 Fe1 155.12(16) . . ?
C1 O1 Fe1 132.11(12) . . ?
C16 O2 Fe1 131.57(13) . . ?
Fe1 O3 H1O3 114.1(17) . . ?
Fe1 O3 H2O3 110.4(17) . . ?
H1O3 O3 H2O3 111(2) . . ?
C2 O4 C20B 117.41(15) . . ?
C15 O5 C18 117.12(16) . . ?
C9B C17B H17D 109.5 . . ?
C9B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
C9B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N1 C8B C9B 105.3(5) . . ?
N1 C8B H8B1 110.7 . . ?
C9B C8B H8B1 110.7 . . ?
N1 C8B H8B2 110.7 . . ?
C9B C8B H8B2 110.7 . . ?
H8B1 C8B H8B2 108.8 . . ?
N5 C24 Fe2 177.62(19) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.063

# start Validation Reply Form
_vrf_PLAT413_shelxl              
;
RESPONSE: The alert is connected to disorder of the amine part of the ligand.
The hydrogen atoms on C19 and C21 atoms were located from Fourier maps and were refined
using torsion angles derived from the electron density. However, the hydrogen atoms on 
C8A/C9A atom were not possible to locate from Fourier maps and they were put into
 calculated positions (AFIX13/AFIX 23).
;
_database_code_depnum_ccdc_archive 'CCDC 998970'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(aqua-methanole(N,N'-(ethane-1,2-diylbis(nitrilomethylylidene))dinaphthalen-2-
olato-N,N')-manganesse(iii) (m-Cyano)-methanole-tricyano-nitrosyl(N,N'-(ethane-
1,2-diylbis(nitrilomethylylidene))dinaphthalen-2-olato-N,N')-iron(ii) methanole 
solvate monohydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62.50 H50 Fe Mn2 N10 O10.50'
_chemical_formula_weight         1274.85

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6373(3)
_cell_length_b                   15.3822(4)
_cell_length_c                   18.2505(5)
_cell_angle_alpha                78.980(2)
_cell_angle_beta                 79.305(2)
_cell_angle_gamma                73.460(2)
_cell_volume                     2782.45(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14234
_cell_measurement_theta_min      2.9249
_cell_measurement_theta_max      33.1964

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1310
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.6888
_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_special_details           
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_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_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24066
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9726
_reflns_number_gt                6678
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0544P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9726
_refine_ls_number_parameters     815
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.52803(4) 0.15135(3) 0.20407(2) 0.01193(12) Uani 1 1 d . . .
Fe1 Fe 0.83176(4) 0.35660(3) 0.22647(2) 0.01659(12) Uani 1 1 d . . .
Mn2 Mn 0.56982(4) 0.15414(3) 0.68651(2) 0.01307(12) Uani 1 1 d . . .
O6 O 0.54478(18) 0.11369(13) 0.79102(10) 0.0152(5) Uani 1 1 d . A .
O4 O 0.8191(2) 0.38584(17) 0.07173(13) 0.0370(6) Uani 1 1 d . . .
O2 O 0.49206(18) 0.10958(13) 0.30829(10) 0.0139(4) Uani 1 1 d . . .
C18 C 0.3179(3) 0.2911(2) 0.27530(16) 0.0144(7) Uani 1 1 d . . .
H18 H 0.2518 0.3476 0.2710 0.017 Uiso 1 1 calc R . .
C5 C 0.9533(3) -0.0872(2) -0.07562(17) 0.0195(7) Uani 1 1 d . . .
H5 H 1.0144 -0.1458 -0.0701 0.023 Uiso 1 1 calc R . .
O1 O 0.65475(18) 0.04108(13) 0.18445(10) 0.0140(4) Uani 1 1 d . . .
O7 O 0.4147(2) 0.07896(14) 0.67809(11) 0.0168(5) Uani 1 1 d D A .
C61 C 0.4606(3) 0.1032(2) 0.91845(15) 0.0137(7) Uani 1 1 d . A .
H61 H 0.5196 0.0440 0.9260 0.016 Uiso 1 1 calc R . .
C32 C 0.8130(3) 0.3253(2) 0.33551(18) 0.0181(7) Uani 1 1 d . . .
O3 O 0.3639(2) 0.09324(15) 0.18331(12) 0.0160(5) Uani 1 1 d . . .
C27 C 0.4254(3) 0.1104(2) 0.43701(15) 0.0139(7) Uani 1 1 d . . .
H27 H 0.4876 0.0527 0.4460 0.017 Uiso 1 1 calc R . .
N2 N 0.5509(2) 0.20546(16) 0.09703(12) 0.0121(5) Uani 1 1 d . . .
O8A O 0.7091(2) 0.23436(16) 0.70075(12) 0.0256(5) Uani 0.683(6) 1 d P A 1
O8B O 0.7091(2) 0.23436(16) 0.70075(12) 0.0256(5) Uani 0.317(6) 1 d PD A 2
H8A H 0.6923 0.2477 0.7447 0.031 Uiso 0.683(6) 1 calc PR A 1
N1 N 0.3956(2) 0.26960(16) 0.21306(12) 0.0123(5) Uani 1 1 d . . .
O5 O 0.70541(18) 0.04964(13) 0.66953(10) 0.0163(5) Uani 1 1 d . A .
C10 C 0.7145(3) 0.0733(2) 0.05027(16) 0.0132(6) Uani 1 1 d . . .
C20 C 0.2335(3) 0.2794(2) 0.41161(16) 0.0145(7) Uani 1 1 d . . .
C1 C 0.7272(3) 0.01809(19) 0.12061(15) 0.0124(6) Uani 1 1 d . . .
N9 N 0.5790(2) 0.20101(16) 0.57873(12) 0.0121(5) Uani 1 1 d . A .
C59 C 0.2902(3) 0.2260(2) 0.96988(15) 0.0132(6) Uani 1 1 d . A .
C12 C 0.4736(3) 0.2977(2) 0.08199(16) 0.0133(7) Uani 1 1 d . . .
N10 N 0.4276(2) 0.26776(16) 0.69569(12) 0.0120(5) Uani 1 1 d . A .
C50 C 0.3297(3) 0.4147(2) 0.61582(16) 0.0178(7) Uani 1 1 d . A .
H50 H 0.2742 0.4394 0.6581 0.021 Uiso 1 1 calc R . .
C9 C 0.7920(3) 0.0378(2) -0.01819(16) 0.0162(7) Uani 1 1 d . . .
C55 C 0.1873(3) 0.3632(2) 0.89089(17) 0.0187(7) Uani 1 1 d . A .
H55 H 0.1764 0.3983 0.8426 0.022 Uiso 1 1 calc R . .
C41 C 0.8472(3) 0.0197(2) 0.33254(16) 0.0179(7) Uani 1 1 d . . .
H41 H 0.8272 0.0468 0.2833 0.021 Uiso 1 1 calc R . .
N5 N 0.8010(3) 0.30638(18) 0.40002(15) 0.0244(6) Uani 1 1 d . . .
C3 C 0.8965(3) -0.0996(2) 0.06251(17) 0.0180(7) Uani 1 1 d . . .
H3 H 0.9601 -0.1573 0.0675 0.022 Uiso 1 1 calc R . .
C25 C 0.2514(3) 0.2344(2) 0.48562(15) 0.0144(7) Uani 1 1 d . . .
C52 C 0.3585(3) 0.2918(2) 0.75923(16) 0.0137(7) Uani 1 1 d . . .
H52 H 0.2964 0.3502 0.7564 0.016 Uiso 1 1 calc R A .
C38 C 0.9032(3) -0.0602(2) 0.47683(16) 0.0133(7) Uani 1 1 d . . .
C13 C 0.4758(3) 0.3522(2) 0.01228(16) 0.0167(7) Uani 1 1 d . . .
H13 H 0.5322 0.3289 -0.0303 0.020 Uiso 1 1 calc R . .
C24 C 0.1709(3) 0.2739(2) 0.54820(17) 0.0200(7) Uani 1 1 d . . .
H24 H 0.1852 0.2449 0.5979 0.024 Uiso 1 1 calc R . .
C49 C 0.3265(3) 0.4658(2) 0.54543(16) 0.0196(7) Uani 1 1 d . . .
H49 H 0.2695 0.5259 0.5392 0.024 Uiso 1 1 calc R . .
C19 C 0.3222(3) 0.2390(2) 0.34833(15) 0.0129(6) Uani 1 1 d . . .
C44 C 0.7395(3) 0.0672(2) 0.53424(15) 0.0130(6) Uani 1 1 d . A .
C48 C 0.4063(3) 0.4298(2) 0.48315(17) 0.0194(7) Uani 1 1 d . A .
H48 H 0.4028 0.4651 0.4345 0.023 Uiso 1 1 calc R . .
C17 C 0.3907(3) 0.3319(2) 0.14461(15) 0.0140(7) Uani 1 1 d . . .
C21 C 0.1295(3) 0.3587(2) 0.40336(17) 0.0198(7) Uani 1 1 d . . .
H21 H 0.1125 0.3884 0.3542 0.024 Uiso 1 1 calc R . .
C7 C 0.8485(3) 0.0458(2) -0.15364(17) 0.0220(8) Uani 1 1 d . . .
H7 H 0.8361 0.0785 -0.2026 0.026 Uiso 1 1 calc R . .
C26 C 0.3480(3) 0.1505(2) 0.49636(16) 0.0159(7) Uani 1 1 d . . .
H26 H 0.3596 0.1209 0.5462 0.019 Uiso 1 1 calc R . .
C56 C 0.1114(3) 0.3970(2) 0.95392(17) 0.0216(7) Uani 1 1 d . . .
H56 H 0.0484 0.4549 0.9485 0.026 Uiso 1 1 calc R . .
C51 C 0.4137(3) 0.3273(2) 0.62538(15) 0.0136(7) Uani 1 1 d . . .
C43 C 0.8078(3) 0.0252(2) 0.46694(15) 0.0127(6) Uani 1 1 d . . .
C60 C 0.3810(3) 0.1385(2) 0.97835(15) 0.0139(7) Uani 1 1 d . . .
H60 H 0.3862 0.1038 1.0272 0.017 Uiso 1 1 calc R . .
C58 C 0.2118(3) 0.2630(2) 1.03355(16) 0.0162(7) Uani 1 1 d . . .
H58 H 0.2195 0.2284 1.0823 0.019 Uiso 1 1 calc R . .
C28 C 0.4134(3) 0.1542(2) 0.36237(15) 0.0126(6) Uani 1 1 d . . .
C46 C 0.4951(3) 0.29103(19) 0.56250(15) 0.0122(6) Uani 1 1 d . A .
C2 C 0.8228(3) -0.0677(2) 0.12555(17) 0.0162(7) Uani 1 1 d . . .
H2 H 0.8353 -0.1033 0.1735 0.019 Uiso 1 1 calc R . .
C54 C 0.2811(3) 0.2772(2) 0.89688(15) 0.0139(7) Uani 1 1 d . . .
C47 C 0.4905(3) 0.3430(2) 0.49193(16) 0.0169(7) Uani 1 1 d . . .
H47 H 0.5456 0.3190 0.4493 0.020 Uiso 1 1 calc R A .
N3 N 0.6800(2) 0.21435(17) 0.22737(13) 0.0176(6) Uani 1 1 d . . .
C39 C 0.9698(3) -0.1026(2) 0.41306(16) 0.0159(7) Uani 1 1 d . . .
H39 H 1.0350 -0.1593 0.4197 0.019 Uiso 1 1 calc R . .
C37 C 0.9282(3) -0.1038(2) 0.55061(15) 0.0142(7) Uani 1 1 d . . .
H37 H 0.9936 -0.1604 0.5566 0.017 Uiso 1 1 calc R . .
C35 C 0.7650(3) 0.0192(2) 0.60577(15) 0.0122(6) Uani 1 1 d . . .
C36 C 0.8610(3) -0.0665(2) 0.61260(16) 0.0133(6) Uani 1 1 d . A .
H36 H 0.8784 -0.0981 0.6612 0.016 Uiso 1 1 calc R . .
N6 N 0.9870(3) 0.49178(18) 0.24342(15) 0.0255(7) Uani 1 1 d . . .
C62 C 0.4578(3) 0.1529(2) 0.84467(15) 0.0138(7) Uani 1 1 d . . .
C45 C 0.6523(3) 0.1557(2) 0.52472(16) 0.0136(7) Uani 1 1 d . . .
H45 H 0.6459 0.1855 0.4744 0.016 Uiso 1 1 calc R A .
C8 C 0.7794(3) 0.0846(2) -0.09157(16) 0.0179(7) Uani 1 1 d . . .
H8 H 0.7218 0.1445 -0.0983 0.021 Uiso 1 1 calc R . .
C16 C 0.3129(3) 0.4213(2) 0.13661(16) 0.0194(7) Uani 1 1 d . . .
H16 H 0.2579 0.4456 0.1791 0.023 Uiso 1 1 calc R . .
C40 C 0.9420(3) -0.0637(2) 0.34236(16) 0.0184(7) Uani 1 1 d . . .
H40 H 0.9869 -0.0932 0.3001 0.022 Uiso 1 1 calc R . .
C11 C 0.6292(3) 0.1631(2) 0.04268(16) 0.0153(7) Uani 1 1 d . . .
H11 H 0.6285 0.1963 -0.0069 0.018 Uiso 1 1 calc R . .
C34 C 0.9280(3) 0.4417(2) 0.23789(16) 0.0175(7) Uani 1 1 d . . .
C4 C 0.8819(3) -0.0497(2) -0.01063(16) 0.0155(7) Uani 1 1 d . . .
C15 C 0.3155(3) 0.4749(2) 0.06726(17) 0.0222(7) Uani 1 1 d . . .
H15 H 0.2617 0.5361 0.0619 0.027 Uiso 1 1 calc R . .
N4 N 0.5700(3) 0.5098(2) 0.24038(16) 0.0335(7) Uani 1 1 d . . .
C30 C 0.7370(3) 0.2656(2) 0.23098(16) 0.0163(7) Uani 1 1 d . . .
C53 C 0.3672(3) 0.2390(2) 0.83209(15) 0.0125(6) Uani 1 1 d . A .
C22 C 0.0516(3) 0.3944(2) 0.46509(17) 0.0245(8) Uani 1 1 d . . .
H22 H -0.0183 0.4483 0.4580 0.029 Uiso 1 1 calc R . .
C33 C 1.0012(3) 0.2649(2) 0.22514(15) 0.0135(7) Uani 1 1 d . . .
C14 C 0.3963(3) 0.4400(2) 0.00485(17) 0.0210(7) Uani 1 1 d . . .
H14 H 0.3965 0.4771 -0.0431 0.025 Uiso 1 1 calc R . .
C42 C 0.7821(3) 0.0635(2) 0.39338(15) 0.0149(7) Uani 1 1 d . . .
H42 H 0.7185 0.1208 0.3853 0.018 Uiso 1 1 calc R . .
C31 C 0.6655(3) 0.4510(2) 0.23989(18) 0.0217(7) Uani 1 1 d . . .
O1S O 1.1149(2) 0.63405(17) 0.20589(17) 0.0528(8) Uani 1 1 d . . .
H4S1 H 1.1124 0.5917 0.2423 0.063 Uiso 1 1 calc R . .
N7 N 1.1039(2) 0.21362(17) 0.22177(13) 0.0178(6) Uani 1 1 d . . .
C6 C 0.9364(3) -0.0409(2) -0.14611(17) 0.0218(8) Uani 1 1 d . . .
H6 H 0.9839 -0.0673 -0.1894 0.026 Uiso 1 1 calc R . .
C57 C 0.1257(3) 0.3473(2) 1.02606(16) 0.0189(7) Uani 1 1 d . . .
H57 H 0.0754 0.3725 1.0694 0.023 Uiso 1 1 calc R . .
C23 C 0.0736(3) 0.3526(2) 0.53785(17) 0.0239(8) Uani 1 1 d . . .
H23 H 0.0208 0.3790 0.5801 0.029 Uiso 1 1 calc R . .
C1S C 1.0164(3) 0.7132(2) 0.2224(2) 0.0387(10) Uani 1 1 d . . .
H3S1 H 0.9733 0.7025 0.2744 0.058 Uiso 1 1 calc R . .
H2S1 H 0.9505 0.7279 0.1878 0.058 Uiso 1 1 calc R . .
H1S1 H 1.0567 0.7645 0.2165 0.058 Uiso 1 1 calc R . .
N8 N 0.8321(2) 0.37689(18) 0.13393(15) 0.0223(6) Uani 1 1 d . . .
C63 C 0.7426(5) 0.3115(4) 0.6443(3) 0.0300(15) Uani 0.683(6) 1 d P A 1
H63A H 0.8048 0.3356 0.6629 0.045 Uiso 0.683(6) 1 calc PR A 1
H63B H 0.6617 0.3603 0.6368 0.045 Uiso 0.683(6) 1 calc PR A 1
H63C H 0.7832 0.2892 0.5964 0.045 Uiso 0.683(6) 1 calc PR A 1
O2S O 0.6356(2) 0.33307(16) 0.81870(14) 0.0317(6) Uani 1 1 d D . .
O3S O 0.7951(8) 0.3125(5) 0.5641(5) 0.038(3) Uani 0.317(6) 1 d PD A 2
H3SA H 0.761(11) 0.362(5) 0.583(6) 0.046 Uiso 0.317(6) 1 d PD A 2
H3SB H 0.805(12) 0.310(8) 0.5176(19) 0.046 Uiso 0.317(6) 1 d PD A 2
H7A H 0.439(4) 0.0255(15) 0.670(2) 0.046 Uiso 1 1 d D . .
H7B H 0.358(3) 0.079(2) 0.7162(15) 0.046 Uiso 1 1 d D . .
H3A H 0.366(4) 0.044(3) 0.193(2) 0.046 Uiso 1 1 d . . .
H3B H 0.287(4) 0.126(3) 0.2003(19) 0.046 Uiso 1 1 d . . .
H2SA H 0.578(3) 0.3809(18) 0.8004(19) 0.046 Uiso 1 1 d D . .
H2SB H 0.698(3) 0.355(2) 0.818(2) 0.046 Uiso 1 1 d D . .
H8C H 0.742(11) 0.250(7) 0.656(3) 0.046 Uiso 0.317(6) 1 d PD A 2
H8B H 0.684(11) 0.278(5) 0.727(5) 0.046 Uiso 0.317(6) 1 d PD A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 1.8904(19) . ?
Mn1 O2 1.8920(18) . ?
Mn1 N2 1.971(2) . ?
Mn1 N1 1.972(2) . ?
Mn1 N3 2.245(3) . ?
Mn1 O3 2.292(2) . ?
Fe1 N8 1.657(3) . ?
Fe1 C30 1.927(3) . ?
Fe1 C34 1.937(3) . ?
Fe1 C32 1.942(3) . ?
Fe1 C33 1.946(3) . ?
Fe1 C31 1.952(3) . ?
Mn2 O5 1.8613(19) . ?
Mn2 O6 1.8836(18) . ?
Mn2 N9 1.956(2) . ?
Mn2 N10 1.971(2) . ?
Mn2 O8A 2.256(2) . ?
Mn2 O7 2.309(2) . ?
O6 C62 1.323(3) . ?
O4 N8 1.146(3) . ?
O2 C28 1.331(3) . ?
C18 N1 1.313(3) . ?
C18 C19 1.419(4) . ?
C18 H18 0.9500 . ?
C5 C6 1.363(4) . ?
C5 C4 1.412(4) . ?
C5 H5 0.9500 . ?
O1 C1 1.321(3) . ?
O7 H7A 0.824(18) . ?
O7 H7B 0.834(18) . ?
C61 C60 1.352(4) . ?
C61 C62 1.416(4) . ?
C61 H61 0.9500 . ?
C32 N5 1.150(4) . ?
O3 H3A 0.73(4) . ?
O3 H3B 0.87(4) . ?
C27 C26 1.366(4) . ?
C27 C28 1.411(4) . ?
C27 H27 0.9500 . ?
N2 C11 1.316(3) . ?
N2 C12 1.427(4) . ?
O8A C63 1.494(6) . ?
O8A H8C 0.839(19) . ?
O8A H8B 0.84(2) . ?
N1 C17 1.421(3) . ?
O5 C35 1.320(3) . ?
C10 C1 1.404(4) . ?
C10 C11 1.418(4) . ?
C10 C9 1.470(4) . ?
C20 C21 1.398(4) . ?
C20 C25 1.415(4) . ?
C20 C19 1.465(4) . ?
C1 C2 1.417(4) . ?
N9 C45 1.317(3) . ?
N9 C46 1.428(4) . ?
C59 C58 1.412(4) . ?
C59 C60 1.415(4) . ?
C59 C54 1.417(4) . ?
C12 C13 1.384(4) . ?
C12 C17 1.397(4) . ?
N10 C52 1.310(3) . ?
N10 C51 1.432(3) . ?
C50 C49 1.372(4) . ?
C50 C51 1.386(4) . ?
C50 H50 0.9500 . ?
C9 C8 1.405(4) . ?
C9 C4 1.411(4) . ?
C55 C56 1.375(4) . ?
C55 C54 1.411(4) . ?
C55 H55 0.9500 . ?
C41 C42 1.379(4) . ?
C41 C40 1.391(4) . ?
C41 H41 0.9500 . ?
C3 C2 1.357(4) . ?
C3 C4 1.419(4) . ?
C3 H3 0.9500 . ?
C25 C26 1.408(4) . ?
C25 C24 1.419(4) . ?
C52 C53 1.424(4) . ?
C52 H52 0.9500 . ?
C38 C39 1.416(4) . ?
C38 C43 1.416(4) . ?
C38 C37 1.421(4) . ?
C13 C14 1.370(4) . ?
C13 H13 0.9500 . ?
C24 C23 1.358(4) . ?
C24 H24 0.9500 . ?
C49 C48 1.391(4) . ?
C49 H49 0.9500 . ?
C19 C28 1.397(4) . ?
C44 C35 1.405(4) . ?
C44 C45 1.412(4) . ?
C44 C43 1.469(4) . ?
C48 C47 1.378(4) . ?
C48 H48 0.9500 . ?
C17 C16 1.386(4) . ?
C21 C22 1.374(4) . ?
C21 H21 0.9500 . ?
C7 C8 1.371(4) . ?
C7 C6 1.392(4) . ?
C7 H7 0.9500 . ?
C26 H26 0.9500 . ?
C56 C57 1.401(4) . ?
C56 H56 0.9500 . ?
C51 C46 1.407(4) . ?
C43 C42 1.403(4) . ?
C60 H60 0.9500 . ?
C58 C57 1.357(4) . ?
C58 H58 0.9500 . ?
C46 C47 1.382(4) . ?
C2 H2 0.9500 . ?
C54 C53 1.463(4) . ?
C47 H47 0.9500 . ?
N3 C30 1.139(4) . ?
C39 C40 1.363(4) . ?
C39 H39 0.9500 . ?
C37 C36 1.354(4) . ?
C37 H37 0.9500 . ?
C35 C36 1.419(4) . ?
C36 H36 0.9500 . ?
N6 C34 1.151(4) . ?
C62 C53 1.406(4) . ?
C45 H45 0.9500 . ?
C8 H8 0.9500 . ?
C16 C15 1.372(4) . ?
C16 H16 0.9500 . ?
C40 H40 0.9500 . ?
C11 H11 0.9500 . ?
C15 C14 1.390(4) . ?
C15 H15 0.9500 . ?
N4 C31 1.152(4) . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C33 N7 1.150(4) . ?
C14 H14 0.9500 . ?
C42 H42 0.9500 . ?
O1S C1S 1.403(4) . ?
O1S H4S1 0.8400 . ?
C6 H6 0.9500 . ?
C57 H57 0.9500 . ?
C23 H23 0.9500 . ?
C1S H3S1 0.9800 . ?
C1S H2S1 0.9800 . ?
C1S H1S1 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
O2S H2SA 0.865(18) . ?
O2S H2SB 0.824(18) . ?
O3S H3SA 0.85(2) . ?
O3S H3SB 0.84(2) . ?

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
_geom_angle_publ_flag
O1 Mn1 O2 93.85(8) . . ?
O1 Mn1 N2 91.70(9) . . ?
O2 Mn1 N2 174.40(9) . . ?
O1 Mn1 N1 174.01(9) . . ?
O2 Mn1 N1 91.93(9) . . ?
N2 Mn1 N1 82.50(9) . . ?
O1 Mn1 N3 93.11(8) . . ?
O2 Mn1 N3 89.91(8) . . ?
N2 Mn1 N3 90.53(9) . . ?
N1 Mn1 N3 88.44(9) . . ?
O1 Mn1 O3 89.95(8) . . ?
O2 Mn1 O3 89.07(8) . . ?
N2 Mn1 O3 90.20(9) . . ?
N1 Mn1 O3 88.59(9) . . ?
N3 Mn1 O3 176.83(8) . . ?
N8 Fe1 C30 88.16(12) . . ?
N8 Fe1 C34 100.38(13) . . ?
C30 Fe1 C34 171.41(12) . . ?
N8 Fe1 C32 172.57(12) . . ?
C30 Fe1 C32 84.77(12) . . ?
C34 Fe1 C32 86.73(12) . . ?
N8 Fe1 C33 96.15(12) . . ?
C30 Fe1 C33 92.16(12) . . ?
C34 Fe1 C33 86.09(12) . . ?
C32 Fe1 C33 86.40(11) . . ?
N8 Fe1 C31 90.39(13) . . ?
C30 Fe1 C31 90.89(12) . . ?
C34 Fe1 C31 89.94(12) . . ?
C32 Fe1 C31 87.47(13) . . ?
C33 Fe1 C31 172.87(12) . . ?
O5 Mn2 O6 92.16(8) . . ?
O5 Mn2 N9 92.00(9) . . ?
O6 Mn2 N9 174.96(9) . . ?
O5 Mn2 N10 175.42(9) . . ?
O6 Mn2 N10 92.41(9) . . ?
N9 Mn2 N10 83.42(9) . . ?
O5 Mn2 O8A 93.65(9) . . ?
O6 Mn2 O8A 91.25(8) . . ?
N9 Mn2 O8A 91.33(9) . . ?
N10 Mn2 O8A 86.59(9) . . ?
O5 Mn2 O7 90.31(8) . . ?
O6 Mn2 O7 86.49(8) . . ?
N9 Mn2 O7 90.64(8) . . ?
N10 Mn2 O7 89.64(9) . . ?
O8A Mn2 O7 175.52(8) . . ?
C62 O6 Mn2 129.49(18) . . ?
C28 O2 Mn1 129.38(17) . . ?
N1 C18 C19 126.9(3) . . ?
N1 C18 H18 116.5 . . ?
C19 C18 H18 116.5 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C1 O1 Mn1 130.06(18) . . ?
Mn2 O7 H7A 120(3) . . ?
Mn2 O7 H7B 113(3) . . ?
H7A O7 H7B 105(3) . . ?
C60 C61 C62 121.4(3) . . ?
C60 C61 H61 119.3 . . ?
C62 C61 H61 119.3 . . ?
N5 C32 Fe1 179.4(3) . . ?
Mn1 O3 H3A 122(3) . . ?
Mn1 O3 H3B 110(2) . . ?
H3A O3 H3B 110(4) . . ?
C26 C27 C28 120.4(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C11 N2 C12 121.2(2) . . ?
C11 N2 Mn1 125.0(2) . . ?
C12 N2 Mn1 113.75(17) . . ?
C63 O8A Mn2 124.3(2) . . ?
Mn2 O8A H8C 104(8) . . ?
C63 O8A H8B 79(7) . . ?
Mn2 O8A H8B 122(8) . . ?
H8C O8A H8B 113(9) . . ?
C18 N1 C17 121.7(2) . . ?
C18 N1 Mn1 124.7(2) . . ?
C17 N1 Mn1 113.57(17) . . ?
C35 O5 Mn2 130.15(18) . . ?
C1 C10 C11 122.2(3) . . ?
C1 C10 C9 119.5(3) . . ?
C11 C10 C9 118.4(3) . . ?
C21 C20 C25 117.8(3) . . ?
C21 C20 C19 124.0(3) . . ?
C25 C20 C19 118.2(3) . . ?
O1 C1 C10 123.9(2) . . ?
O1 C1 C2 116.5(2) . . ?
C10 C1 C2 119.6(3) . . ?
C45 N9 C46 121.6(2) . . ?
C45 N9 Mn2 125.0(2) . . ?
C46 N9 Mn2 113.37(17) . . ?
C58 C59 C60 120.5(3) . . ?
C58 C59 C54 120.2(3) . . ?
C60 C59 C54 119.3(3) . . ?
C13 C12 C17 120.2(3) . . ?
C13 C12 N2 125.2(3) . . ?
C17 C12 N2 114.6(2) . . ?
C52 N10 C51 121.9(2) . . ?
C52 N10 Mn2 125.0(2) . . ?
C51 N10 Mn2 112.91(17) . . ?
C49 C50 C51 120.1(3) . . ?
C49 C50 H50 119.9 . . ?
C51 C50 H50 119.9 . . ?
C8 C9 C4 117.4(3) . . ?
C8 C9 C10 123.9(3) . . ?
C4 C9 C10 118.6(3) . . ?
C56 C55 C54 121.0(3) . . ?
C56 C55 H55 119.5 . . ?
C54 C55 H55 119.5 . . ?
C42 C41 C40 120.8(3) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C2 C3 C4 122.2(3) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C26 C25 C20 119.7(3) . . ?
C26 C25 C24 120.7(3) . . ?
C20 C25 C24 119.6(3) . . ?
N10 C52 C53 126.4(3) . . ?
N10 C52 H52 116.8 . . ?
C53 C52 H52 116.8 . . ?
C39 C38 C43 119.5(3) . . ?
C39 C38 C37 120.6(3) . . ?
C43 C38 C37 119.9(2) . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C23 C24 C25 120.7(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C50 C49 C48 120.3(3) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C28 C19 C18 122.4(3) . . ?
C28 C19 C20 119.3(2) . . ?
C18 C19 C20 118.1(3) . . ?
C35 C44 C45 122.1(3) . . ?
C35 C44 C43 119.1(3) . . ?
C45 C44 C43 118.7(3) . . ?
C47 C48 C49 120.2(3) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C16 C17 C12 119.4(3) . . ?
C16 C17 N1 125.2(3) . . ?
C12 C17 N1 115.3(2) . . ?
C22 C21 C20 121.2(3) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C8 C7 C6 121.1(3) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C27 C26 C25 121.8(3) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C55 C56 C57 120.9(3) . . ?
C55 C56 H56 119.5 . . ?
C57 C56 H56 119.5 . . ?
C50 C51 C46 119.7(3) . . ?
C50 C51 N10 125.6(3) . . ?
C46 C51 N10 114.7(2) . . ?
C42 C43 C38 117.8(3) . . ?
C42 C43 C44 123.9(3) . . ?
C38 C43 C44 118.3(2) . . ?
C61 C60 C59 121.5(3) . . ?
C61 C60 H60 119.3 . . ?
C59 C60 H60 119.3 . . ?
C57 C58 C59 120.9(3) . . ?
C57 C58 H58 119.5 . . ?
C59 C58 H58 119.5 . . ?
O2 C28 C19 123.6(2) . . ?
O2 C28 C27 116.0(2) . . ?
C19 C28 C27 120.4(3) . . ?
C47 C46 C51 119.6(3) . . ?
C47 C46 N9 125.3(3) . . ?
C51 C46 N9 115.1(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C55 C54 C59 117.4(3) . . ?
C55 C54 C53 123.4(3) . . ?
C59 C54 C53 119.2(3) . . ?
C48 C47 C46 120.2(3) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C30 N3 Mn1 162.9(2) . . ?
C40 C39 C38 121.2(3) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C36 C37 C38 121.6(3) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 H37 119.2 . . ?
O5 C35 C44 123.7(3) . . ?
O5 C35 C36 116.0(2) . . ?
C44 C35 C36 120.3(2) . . ?
C37 C36 C35 120.8(3) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
O6 C62 C53 123.9(3) . . ?
O6 C62 C61 116.1(2) . . ?
C53 C62 C61 120.0(3) . . ?
N9 C45 C44 126.4(3) . . ?
N9 C45 H45 116.8 . . ?
C44 C45 H45 116.8 . . ?
C7 C8 C9 121.4(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C15 C16 C17 120.0(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C39 C40 C41 119.5(3) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
N2 C11 C10 126.9(3) . . ?
N2 C11 H11 116.5 . . ?
C10 C11 H11 116.5 . . ?
N6 C34 Fe1 178.6(3) . . ?
C9 C4 C5 119.8(3) . . ?
C9 C4 C3 119.1(3) . . ?
C5 C4 C3 121.1(3) . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
N3 C30 Fe1 174.2(3) . . ?
C62 C53 C52 122.7(3) . . ?
C62 C53 C54 118.6(2) . . ?
C52 C53 C54 118.6(3) . . ?
C21 C22 C23 121.0(3) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
N7 C33 Fe1 176.7(3) . . ?
C13 C14 C15 120.3(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C41 C42 C43 121.3(3) . . ?
C41 C42 H42 119.4 . . ?
C43 C42 H42 119.4 . . ?
N4 C31 Fe1 173.3(3) . . ?
C1S O1S H4S1 109.5 . . ?
C5 C6 C7 118.9(3) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C58 C57 C56 119.5(3) . . ?
C58 C57 H57 120.3 . . ?
C56 C57 H57 120.3 . . ?
C24 C23 C22 119.6(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
O1S C1S H3S1 109.5 . . ?
O1S C1S H2S1 109.5 . . ?
H3S1 C1S H2S1 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
H3S1 C1S H1S1 109.5 . . ?
H2S1 C1S H1S1 109.5 . . ?
O4 N8 Fe1 171.3(2) . . ?
O8A C63 H63A 109.5 . . ?
O8A C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
O8A C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O8A C63 H3SA 161(4) . . ?
H63A C63 H3SA 88.0 . . ?
H63B C63 H3SA 70.3 . . ?
H63C C63 H3SA 55.2 . . ?
H63A C63 H8C 121.4 . . ?
H63B C63 H8C 122.1 . . ?
H63C C63 H8C 79.0 . . ?
H3SA C63 H8C 133(4) . . ?
H63A C63 H8B 91.6 . . ?
H63B C63 H8B 92.2 . . ?
H63C C63 H8B 141.4 . . ?
H3SA C63 H8B 161(4) . . ?
H8C C63 H8B 62(4) . . ?
H2SA O2S H2SB 101(3) . . ?
H3SA O3S H3SB 123(10) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.080

# start Validation Reply Form
_vrf_PLAT041_shelxl              
;
RESPONSE: All reported problems with calc. and report. formula originate in 
CH3OH/H2O disorder. 
;
_database_code_depnum_ccdc_archive 'CCDC 998971'
