# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-4H2O
_database_code_depnum_ccdc_archive 'CCDC 1491307'
_audit_update_record             
;
2016-07-06 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT041_1-4H2O              
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: This alert arises because some hydrogen atoms of the water molecules were not located, but they were introduced in the formula of the compound.
;
_vrf_PLAT043_1-4H2O              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       3.02 Check
RESPONSE: This alert arises because some hydrogen atoms of the water molecules were not located, but they were introduced in the formula of the compound.
;
_vrf_PLAT068_1-4H2O              
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: This alert arises because some hydrogen atoms of the water molecules were not located, but they were introduced in the formula of the compound.
;
# Added during the CSD deposition process: Wednesday 06 July 2016 06:33 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10, C6 H8 O4, 4(H2 O)'
_chemical_formula_sum            'C28 H34 Fe N10 O8'
_chemical_formula_weight         694.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   8.07580(10)
_cell_length_b                   25.2815(3)
_cell_length_c                   16.1326(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.381(18)
_cell_angle_gamma                90.00
_cell_volume                     3045.65(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6950
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.0800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
'Goniometer Xcalibur, detector: Sapphire3 (Gemini Mo)'
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13393
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6963
_reflns_number_gt                4590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.28 (release 05-12-2008 CrysAlis171 .NET)
(compiled Dec  5 2008,16:01:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.28 (release 05-12-2008 CrysAlis171 .NET)
(compiled Dec  5 2008,16:01:47)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.28 (release 05-12-2008 CrysAlis171 .NET)
(compiled Dec  5 2008,16:01:47)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  
;
WinGX publication routines (Farrugia, 1999)
;

_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)+(0.1091P)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         6963
_refine_ls_number_parameters     457
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1890
_refine_ls_wR_factor_gt          0.1397
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_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
Fe1 Fe -0.08770(6) 0.141598(18) 0.84812(3) 0.01891(16) Uani 1 1 d . . .
N1 N -0.2879(4) 0.24415(12) 0.7585(2) 0.0259(6) Uani 1 1 d D . .
H1N H -0.317(5) 0.2333(15) 0.7030(15) 0.031 Uiso 1 1 d D . .
N2 N -0.1935(4) 0.21336(11) 0.82830(18) 0.0229(6) Uani 1 1 d . . .
N3 N -0.0093(4) 0.16628(11) 0.96936(18) 0.0223(6) Uani 1 1 d . . .
N4 N 0.0460(4) 0.07943(10) 0.91208(18) 0.0214(6) Uani 1 1 d . . .
N5 N 0.0844(4) 0.03064(11) 0.89202(19) 0.0225(6) Uani 1 1 d D . .
H5N H 0.049(5) 0.0172(14) 0.8375(15) 0.027 Uiso 1 1 d D . .
N6 N 0.2625(4) 0.19182(12) 0.8530(2) 0.0260(6) Uani 1 1 d D . .
H6N H 0.303(5) 0.2010(15) 0.9106(14) 0.031 Uiso 1 1 d D . .
N7 N 0.1095(3) 0.16499(11) 0.81452(18) 0.0211(6) Uani 1 1 d . . .
N8 N -0.1663(4) 0.11478(11) 0.72840(18) 0.0224(6) Uani 1 1 d . . .
N9 N -0.3132(4) 0.10793(11) 0.83777(19) 0.0233(6) Uani 1 1 d . . .
N10 N -0.4036(4) 0.09932(13) 0.8909(2) 0.0294(7) Uani 1 1 d D . .
H10N H -0.379(5) 0.1019(16) 0.9463(13) 0.035 Uiso 1 1 d D . .
C1 C -0.3220(5) 0.29125(15) 0.7881(3) 0.0322(8) Uani 1 1 d . . .
H1 H -0.3859 0.3190 0.7522 0.039 Uiso 1 1 calc R . .
C2 C -0.2469(5) 0.29141(14) 0.8798(3) 0.0307(8) Uani 1 1 d . . .
H2 H -0.2487 0.3186 0.9182 0.037 Uiso 1 1 calc R . .
C3 C -0.1669(4) 0.24169(13) 0.9030(2) 0.0250(7) Uani 1 1 d . . .
C4 C -0.0608(5) 0.21473(14) 0.9864(2) 0.0268(8) Uani 1 1 d . . .
C5 C -0.0128(6) 0.23266(15) 1.0732(3) 0.0387(10) Uani 1 1 d . . .
H5 H -0.0480 0.2660 1.0848 0.046 Uiso 1 1 calc R . .
C6 C 0.0890(6) 0.19984(16) 1.1426(3) 0.0430(10) Uani 1 1 d . . .
H6 H 0.1212 0.2110 1.2017 0.052 Uiso 1 1 calc R . .
C7 C 0.1430(6) 0.15073(15) 1.1249(3) 0.0373(9) Uani 1 1 d . . .
H7 H 0.2133 0.1290 1.1715 0.045 Uiso 1 1 calc R . .
C8 C 0.0915(5) 0.13440(14) 1.0373(2) 0.0260(8) Uani 1 1 d . . .
C9 C 0.1249(4) 0.08390(13) 1.0024(2) 0.0240(7) Uani 1 1 d . . .
C10 C 0.2161(5) 0.03689(14) 1.0391(2) 0.0302(8) Uani 1 1 d . . .
H10 H 0.2817 0.0294 1.0992 0.036 Uiso 1 1 calc R . .
C11 C 0.1866(5) 0.00438(14) 0.9665(2) 0.0291(8) Uani 1 1 d . . .
H11 H 0.2299 -0.0299 0.9685 0.035 Uiso 1 1 calc R . .
C12 C 0.3464(5) 0.19669(14) 0.7952(3) 0.0322(9) Uani 1 1 d . . .
H12 H 0.4554 0.2136 0.8073 0.039 Uiso 1 1 calc R . .
C13 C 0.2450(5) 0.17280(14) 0.7160(2) 0.0300(8) Uani 1 1 d . . .
H13 H 0.2693 0.1701 0.6643 0.036 Uiso 1 1 calc R . .
C14 C 0.0952(4) 0.15320(14) 0.7308(2) 0.0245(8) Uani 1 1 d . . .
C15 C -0.0653(4) 0.12279(14) 0.6790(2) 0.0244(7) Uani 1 1 d . . .
C16 C -0.1186(5) 0.10311(16) 0.5927(2) 0.0335(9) Uani 1 1 d . . .
H16 H -0.0499 0.1087 0.5586 0.040 Uiso 1 1 calc R . .
C17 C -0.2779(6) 0.07471(16) 0.5585(2) 0.0386(10) Uani 1 1 d . . .
H17 H -0.3159 0.0613 0.5006 0.046 Uiso 1 1 calc R . .
C18 C -0.3795(5) 0.06619(15) 0.6083(2) 0.0326(9) Uani 1 1 d . . .
H18 H -0.4861 0.0473 0.5847 0.039 Uiso 1 1 calc R . .
C19 C -0.3205(4) 0.08642(13) 0.6952(2) 0.0263(8) Uani 1 1 d . . .
C20 C -0.4018(4) 0.08215(13) 0.7609(2) 0.0255(8) Uani 1 1 d . . .
C21 C -0.5505(5) 0.05656(15) 0.7659(3) 0.0356(9) Uani 1 1 d . . .
H21 H -0.6339 0.0358 0.7221 0.043 Uiso 1 1 calc R . .
C22 C -0.5469(5) 0.06855(16) 0.8487(3) 0.0393(10) Uani 1 1 d . . .
H22 H -0.6298 0.0573 0.8722 0.047 Uiso 1 1 calc R . .
C23 C 0.1539(5) 0.46120(15) 0.7982(3) 0.0330(9) Uani 1 1 d . . .
C24 C 0.2232(5) 0.43201(16) 0.8881(3) 0.0366(9) Uani 1 1 d . . .
H24A H 0.3488 0.4235 0.9043 0.044 Uiso 1 1 calc R . .
H24B H 0.2136 0.4550 0.9342 0.044 Uiso 1 1 calc R . .
C25 C 0.1191(6) 0.38153(18) 0.8843(3) 0.0490(11) Uani 1 1 d . . .
H25A H 0.0998 0.3632 0.8285 0.059 Uiso 1 1 calc R . .
H25B H 0.0029 0.3904 0.8852 0.059 Uiso 1 1 calc R . .
C26 C 0.2185(6) 0.34477(18) 0.9633(3) 0.0429(10) Uani 1 1 d . . .
H26A H 0.2627 0.3653 1.0182 0.052 Uiso 1 1 calc R . .
H26B H 0.1353 0.3187 0.9689 0.052 Uiso 1 1 calc R . .
C27 C 0.3734(6) 0.31675(15) 0.9520(3) 0.0399(10) Uani 1 1 d . . .
H27A H 0.4592 0.3428 0.9490 0.048 Uiso 1 1 calc R . .
H27B H 0.3300 0.2974 0.8958 0.048 Uiso 1 1 calc R . .
C28 C 0.4674(5) 0.27827(15) 1.0288(3) 0.0333(9) Uani 1 1 d . . .
O1 O 0.2475(4) 0.46071(11) 0.75264(18) 0.0437(7) Uani 1 1 d . . .
O2 O 0.0043(4) 0.48447(11) 0.77492(17) 0.0385(7) Uani 1 1 d . . .
O3 O 0.4262(3) 0.23011(10) 1.01878(17) 0.0356(6) Uani 1 1 d . . .
O4 O 0.5806(5) 0.29760(12) 1.0984(2) 0.0605(10) Uani 1 1 d . . .
O1W O -0.3431(5) 0.14595(13) 1.0504(2) 0.0523(9) Uani 1 1 d D . .
H1A H -0.337(7) 0.1258(16) 1.091(3) 0.078 Uiso 1 1 d D . .
H1B H -0.409(6) 0.1693(15) 1.050(3) 0.078 Uiso 1 1 d D . .
O2W O -0.1346(4) 0.49485(15) 0.9118(2) 0.0500(8) Uani 1 1 d D . .
H2A H -0.099(7) 0.492(2) 0.874(2) 0.075 Uiso 1 1 d D . .
H2B H -0.059(8) 0.490(5) 0.9602(19) 0.075 Uiso 0.50 1 d PD . .
O3W O 0.5874(5) 0.42150(14) 0.8233(2) 0.0611(9) Uani 1 1 d D . .
H3A H 0.496(5) 0.440(2) 0.805(4) 0.092 Uiso 1 1 d D . .
O4W O 0.6956(5) 0.42653(17) 0.6808(2) 0.0683(10) Uani 1 1 d D . .
H4A H 0.807(3) 0.431(3) 0.705(3) 0.103 Uiso 1 1 d D . .
H4B H 0.663(7) 0.427(3) 0.724(3) 0.103 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
Fe1 N8 1.913(3) . ?
Fe1 N3 1.917(3) . ?
Fe1 N7 1.958(3) . ?
Fe1 N9 1.959(3) . ?
Fe1 N4 1.963(3) . ?
Fe1 N2 1.979(3) . ?
N1 N2 1.343(4) . ?
N1 C1 1.350(5) . ?
N1 H1N 0.879(18) . ?
N2 C3 1.347(4) . ?
N3 C8 1.354(4) . ?
N3 C4 1.355(4) . ?
N4 N5 1.341(4) . ?
N4 C9 1.354(4) . ?
N5 C11 1.346(4) . ?
N5 H5N 0.882(18) . ?
N6 N7 1.338(4) . ?
N6 C12 1.351(4) . ?
N6 H6N 0.890(18) . ?
N7 C14 1.345(4) . ?
N8 C15 1.355(4) . ?
N8 C19 1.358(4) . ?
N9 N10 1.338(4) . ?
N9 C20 1.342(4) . ?
N10 C22 1.345(5) . ?
N10 H10N 0.842(18) . ?
C1 C2 1.369(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.398(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.460(5) . ?
C4 C5 1.379(5) . ?
C5 C6 1.385(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.382(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.376(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.461(5) . ?
C9 C10 1.405(5) . ?
C10 C11 1.375(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.367(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.464(5) . ?
C15 C16 1.383(5) . ?
C16 C17 1.390(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.367(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.395(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.447(5) . ?
C20 C21 1.393(5) . ?
C21 C22 1.360(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O1 1.239(4) . ?
C23 O2 1.265(5) . ?
C23 C24 1.530(5) . ?
C24 C25 1.517(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.534(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.509(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.531(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 O4 1.246(5) . ?
C28 O3 1.256(4) . ?
O1W H1A 0.818(19) . ?
O1W H1B 0.793(19) . ?
O2W H2A 0.774(19) . ?
O2W H2B 0.80(2) . ?
O3W H3A 0.84(2) . ?
O4W H4A 0.84(2) . ?
O4W H4B 0.842(19) . ?

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
N8 Fe1 N3 178.22(12) . . ?
N8 Fe1 N7 79.62(11) . . ?
N3 Fe1 N7 101.35(11) . . ?
N8 Fe1 N9 79.61(12) . . ?
N3 Fe1 N9 99.41(11) . . ?
N7 Fe1 N9 159.22(12) . . ?
N8 Fe1 N4 98.72(11) . . ?
N3 Fe1 N4 79.77(12) . . ?
N7 Fe1 N4 92.57(11) . . ?
N9 Fe1 N4 90.24(11) . . ?
N8 Fe1 N2 101.83(11) . . ?
N3 Fe1 N2 79.68(12) . . ?
N7 Fe1 N2 91.43(11) . . ?
N9 Fe1 N2 93.11(11) . . ?
N4 Fe1 N2 159.45(12) . . ?
N2 N1 C1 110.0(3) . . ?
N2 N1 H1N 121(3) . . ?
C1 N1 H1N 129(3) . . ?
N1 N2 C3 106.8(3) . . ?
N1 N2 Fe1 137.7(2) . . ?
C3 N2 Fe1 115.5(2) . . ?
C8 N3 C4 120.7(3) . . ?
C8 N3 Fe1 119.7(2) . . ?
C4 N3 Fe1 119.6(2) . . ?
N5 N4 C9 106.2(3) . . ?
N5 N4 Fe1 137.8(2) . . ?
C9 N4 Fe1 116.0(2) . . ?
N4 N5 C11 111.0(3) . . ?
N4 N5 H5N 125(2) . . ?
C11 N5 H5N 124(2) . . ?
N7 N6 C12 110.1(3) . . ?
N7 N6 H6N 122(2) . . ?
C12 N6 H6N 128(2) . . ?
N6 N7 C14 106.8(3) . . ?
N6 N7 Fe1 136.8(2) . . ?
C14 N7 Fe1 116.3(2) . . ?
C15 N8 C19 121.0(3) . . ?
C15 N8 Fe1 119.9(2) . . ?
C19 N8 Fe1 119.1(2) . . ?
N10 N9 C20 106.5(3) . . ?
N10 N9 Fe1 137.1(2) . . ?
C20 N9 Fe1 116.2(2) . . ?
N9 N10 C22 110.1(3) . . ?
N9 N10 H10N 135(3) . . ?
C22 N10 H10N 113(3) . . ?
N1 C1 C2 108.6(3) . . ?
N1 C1 H1 125.7 . . ?
C2 C1 H1 125.7 . . ?
C1 C2 C3 104.8(3) . . ?
C1 C2 H2 127.6 . . ?
C3 C2 H2 127.6 . . ?
N2 C3 C2 109.8(3) . . ?
N2 C3 C4 114.5(3) . . ?
C2 C3 C4 135.7(3) . . ?
N3 C4 C5 120.9(3) . . ?
N3 C4 C3 110.7(3) . . ?
C5 C4 C3 128.4(3) . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 120.5(4) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C6 119.1(4) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N3 C8 C7 120.4(3) . . ?
N3 C8 C9 110.5(3) . . ?
C7 C8 C9 129.0(3) . . ?
N4 C9 C10 109.9(3) . . ?
N4 C9 C8 114.0(3) . . ?
C10 C9 C8 136.1(3) . . ?
C11 C10 C9 104.7(3) . . ?
C11 C10 H10 127.7 . . ?
C9 C10 H10 127.7 . . ?
N5 C11 C10 108.3(3) . . ?
N5 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
N6 C12 C13 109.0(3) . . ?
N6 C12 H12 125.5 . . ?
C13 C12 H12 125.5 . . ?
C12 C13 C14 104.2(3) . . ?
C12 C13 H13 127.9 . . ?
C14 C13 H13 127.9 . . ?
N7 C14 C13 109.9(3) . . ?
N7 C14 C15 114.1(3) . . ?
C13 C14 C15 135.9(3) . . ?
N8 C15 C16 120.7(3) . . ?
N8 C15 C14 110.1(3) . . ?
C16 C15 C14 129.2(3) . . ?
C15 C16 C17 118.2(3) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 118.8(3) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N8 C19 C18 120.1(3) . . ?
N8 C19 C20 110.8(3) . . ?
C18 C19 C20 129.2(3) . . ?
N9 C20 C21 109.9(3) . . ?
N9 C20 C19 114.2(3) . . ?
C21 C20 C19 135.9(3) . . ?
C22 C21 C20 104.9(3) . . ?
C22 C21 H21 127.5 . . ?
C20 C21 H21 127.5 . . ?
N10 C22 C21 108.6(3) . . ?
N10 C22 H22 125.7 . . ?
C21 C22 H22 125.7 . . ?
O1 C23 O2 123.9(4) . . ?
O1 C23 C24 118.1(4) . . ?
O2 C23 C24 118.0(3) . . ?
C25 C24 C23 111.7(3) . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
C24 C25 C26 111.7(4) . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
C26 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C27 C26 C25 112.3(3) . . ?
C27 C26 H26A 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C26 C27 C28 112.2(3) . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
O4 C28 O3 124.3(4) . . ?
O4 C28 C27 116.6(3) . . ?
O3 C28 C27 119.1(3) . . ?
H1A O1W H1B 108(3) . . ?
H2A O2W H2B 113(4) . . ?
H4A O4W H4B 103(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.805
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.273
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol/water'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-2MeOH-H2O
_database_code_depnum_ccdc_archive 'CCDC 1491308'
_audit_update_record             
;
2016-07-06 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10, C8 H4 O4, 2(C H4 O), H2 O'
_chemical_formula_sum            'C32 H32 Fe N10 O7'
_chemical_formula_weight         724.53

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.0628(4)
_cell_length_b                   16.4572(7)
_cell_length_c                   24.6825(11)
_cell_angle_alpha                98.352(4)
_cell_angle_beta                 90.601(4)
_cell_angle_gamma                93.125(4)
_cell_volume                     3235.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    128(1)
_cell_measurement_reflns_used    3029
_cell_measurement_theta_min      2.6430
_cell_measurement_theta_max      27.8450

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2004
_exptl_crystal_size_mid          0.0706
_exptl_crystal_size_min          0.0501
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 2 0.0359 0.0000 1.0000 2.0000 0.0530 -0.0019 -0.0567
0 2 1 0.0374 -0.0000 2.0000 1.0000 0.0211 -0.0003 -0.0936
0 -2 -1 0.0374 0.0000 -2.0000 -1.0000 -0.0211 0.0003 0.0936
0 -2 1 0.0323 0.0000 -2.0000 1.0000 0.0354 -0.0022 0.0804
0 2 -1 0.0323 -0.0000 2.0000 -1.0000 -0.0354 0.0022 -0.0804
0 0 -1 0.0251 -0.0000 -0.0000 -1.0000 -0.0283 0.0012 0.0066
0 0 1 0.0251 0.0000 0.0000 1.0000 0.0283 -0.0012 -0.0066
1 0 6 0.0380 1.0000 0.0000 6.0000 0.1662 -0.0951 -0.0452
-1 0 -6 0.0165 -1.0000 -0.0000 -6.0000 -0.1662 0.0951 0.0452
1 0 1 0.0958 1.0000 -0.0000 1.0000 0.0249 -0.0891 -0.0123
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      128(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29084
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.1885
_diffrn_orient_matrix_UB_11      -0.0034121000
_diffrn_orient_matrix_UB_12      -0.0035597000
_diffrn_orient_matrix_UB_13      0.0282679000
_diffrn_orient_matrix_UB_21      -0.0878676000
_diffrn_orient_matrix_UB_22      0.0004808000
_diffrn_orient_matrix_UB_23      -0.0012134000
_diffrn_orient_matrix_UB_31      -0.0057004000
_diffrn_orient_matrix_UB_32      -0.0434836000
_diffrn_orient_matrix_UB_33      -0.0065849000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00   43.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550  -45.0000  300.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega   -4.00   47.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550  -45.0000  150.0000 51

#__ type_ start__ end____ width___ exp.time_
  3 omega   38.00   92.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550   77.0000  180.0000 54

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   51.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550  -77.0000   90.0000 101

#__ type_ start__ end____ width___ exp.time_
  5 omega   -1.00   53.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550  -77.0000  210.0000 54

#__ type_ start__ end____ width___ exp.time_
  6 omega    6.00   49.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0550  -77.0000  270.0000 43

#__ type_ start__ end____ width___ exp.time_
  7 omega  -41.00    6.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6956  -77.0000    0.0000 47

#__ type_ start__ end____ width___ exp.time_
  8 omega   10.00   40.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6956   45.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
  9 omega  -26.00   -1.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6956   45.0000   60.0000 25

;
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         28.67
_reflns_number_total             14486
_reflns_number_gt                7205
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0258P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14486
_refine_ls_number_parameters     953
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.016
_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
Fe1 Fe 0.01546(9) 0.33503(4) 0.73929(3) 0.01698(18) Uani 1 1 d . . .
N1 N -0.3306(5) 0.4024(2) 0.76777(16) 0.0190(10) Uani 1 1 d D . .
H1N H -0.332(7) 0.398(3) 0.8040(9) 0.043(17) Uiso 1 1 d D . .
N2 N -0.2102(5) 0.3744(2) 0.73384(15) 0.0157(9) Uani 1 1 d . . .
N3 N -0.0197(5) 0.3178(2) 0.66127(15) 0.0167(9) Uani 1 1 d . . .
N4 N 0.2225(5) 0.2828(2) 0.71395(15) 0.0163(9) Uani 1 1 d . . .
N5 N 0.3566(5) 0.2549(2) 0.73694(17) 0.0212(10) Uani 1 1 d D . .
H5N H 0.375(6) 0.270(2) 0.7732(9) 0.021(14) Uiso 1 1 d D . .
N6 N -0.1399(5) 0.1591(2) 0.74256(17) 0.0222(10) Uani 1 1 d D . .
H6N H -0.134(5) 0.141(2) 0.7064(8) 0.010(12) Uiso 1 1 d D . .
N7 N -0.0692(5) 0.2330(2) 0.76482(16) 0.0183(9) Uani 1 1 d . . .
N8 N 0.0525(5) 0.3622(2) 0.81705(15) 0.0170(9) Uani 1 1 d . . .
N9 N 0.1150(5) 0.4472(2) 0.74410(15) 0.0175(9) Uani 1 1 d . . .
N10 N 0.1559(5) 0.5006(2) 0.70936(17) 0.0207(10) Uani 1 1 d D . .
H10N H 0.156(8) 0.488(3) 0.6726(9) 0.07(2) Uiso 1 1 d D . .
C1 C -0.4585(6) 0.4253(3) 0.7392(2) 0.0215(12) Uani 1 1 d . . .
H1 H -0.5554 0.4465 0.7540 0.026 Uiso 1 1 calc R . .
C2 C -0.4230(6) 0.4124(3) 0.6846(2) 0.0213(12) Uani 1 1 d . . .
H2 H -0.4884 0.4229 0.6555 0.026 Uiso 1 1 calc R . .
C3 C -0.2665(6) 0.3799(3) 0.68254(18) 0.0168(11) Uani 1 1 d . . .
C4 C -0.1570(6) 0.3466(3) 0.63945(19) 0.0184(11) Uani 1 1 d . . .
C5 C -0.1797(7) 0.3412(3) 0.58386(19) 0.0253(12) Uani 1 1 d . . .
H5 H -0.2731 0.3618 0.5694 0.030 Uiso 1 1 calc R . .
C6 C -0.0604(7) 0.3045(3) 0.5493(2) 0.0277(13) Uani 1 1 d . . .
H6 H -0.0744 0.3001 0.5115 0.033 Uiso 1 1 calc R . .
C7 C 0.0782(6) 0.2748(3) 0.57121(19) 0.0230(12) Uani 1 1 d . . .
H7 H 0.1576 0.2498 0.5484 0.028 Uiso 1 1 calc R . .
C8 C 0.0972(6) 0.2826(3) 0.62727(19) 0.0204(11) Uani 1 1 d . . .
C9 C 0.2333(6) 0.2592(3) 0.65948(19) 0.0191(11) Uani 1 1 d . . .
C10 C 0.3783(6) 0.2168(3) 0.6481(2) 0.0226(12) Uani 1 1 d . . .
H10 H 0.4164 0.1944 0.6141 0.027 Uiso 1 1 calc R . .
C11 C 0.4510(7) 0.2160(3) 0.6981(2) 0.0252(13) Uani 1 1 d . . .
H11 H 0.5502 0.1923 0.7043 0.030 Uiso 1 1 calc R . .
C12 C -0.1802(6) 0.1138(3) 0.7822(2) 0.0267(13) Uani 1 1 d . . .
H12 H -0.2292 0.0607 0.7766 0.032 Uiso 1 1 calc R . .
C13 C -0.1373(7) 0.1583(3) 0.8318(2) 0.0278(13) Uani 1 1 d . . .
H13 H -0.1511 0.1426 0.8662 0.033 Uiso 1 1 calc R . .
C14 C -0.0680(6) 0.2326(3) 0.81917(19) 0.0187(11) Uani 1 1 d . . .
C15 C 0.0058(6) 0.3074(3) 0.85083(18) 0.0183(11) Uani 1 1 d . . .
C16 C 0.0316(6) 0.3264(3) 0.90715(19) 0.0235(12) Uani 1 1 d . . .
H16 H 0.0028 0.2879 0.9301 0.028 Uiso 1 1 calc R . .
C17 C 0.1007(6) 0.4034(3) 0.9285(2) 0.0259(13) Uani 1 1 d . . .
H17 H 0.1167 0.4173 0.9662 0.031 Uiso 1 1 calc R . .
C18 C 0.1460(6) 0.4597(3) 0.8939(2) 0.0242(12) Uani 1 1 d . . .
H18 H 0.1922 0.5116 0.9080 0.029 Uiso 1 1 calc R . .
C19 C 0.1215(6) 0.4378(3) 0.8381(2) 0.0187(11) Uani 1 1 d . . .
C20 C 0.1571(6) 0.4867(3) 0.7949(2) 0.0192(11) Uani 1 1 d . . .
C21 C 0.2247(6) 0.5656(3) 0.7917(2) 0.0229(12) Uani 1 1 d . . .
H21 H 0.2636 0.6053 0.8204 0.028 Uiso 1 1 calc R . .
C22 C 0.2211(6) 0.5717(3) 0.7365(2) 0.0240(12) Uani 1 1 d . . .
H22 H 0.2576 0.6174 0.7209 0.029 Uiso 1 1 calc R . .
Fe2 Fe 0.01902(9) 0.83426(4) 0.77321(3) 0.01730(18) Uani 1 1 d . . .
N11 N 0.3687(5) 0.7622(2) 0.76816(17) 0.0195(10) Uani 1 1 d D . .
H11N H 0.388(7) 0.765(3) 0.8047(9) 0.06(2) Uiso 1 1 d D . .
N12 N 0.2339(5) 0.7922(2) 0.74675(15) 0.0163(9) Uani 1 1 d . . .
N13 N 0.0018(5) 0.8421(2) 0.69697(15) 0.0158(9) Uani 1 1 d . . .
N14 N -0.2023(5) 0.8771(2) 0.76986(15) 0.0164(9) Uani 1 1 d . . .
N15 N -0.3258(5) 0.8986(2) 0.80448(17) 0.0204(10) Uani 1 1 d D . .
H15N H -0.340(6) 0.883(2) 0.8386(11) 0.028(15) Uiso 1 1 d D . .
N16 N -0.1304(5) 0.6582(2) 0.73653(17) 0.0215(10) Uani 1 1 d D . .
H16N H -0.124(6) 0.653(3) 0.7003(8) 0.024(15) Uiso 1 1 d D . .
N17 N -0.0733(5) 0.7219(2) 0.77341(16) 0.0191(10) Uani 1 1 d . . .
N18 N 0.0266(5) 0.8274(2) 0.85027(15) 0.0189(9) Uani 1 1 d . . .
N19 N 0.1183(5) 0.9442(2) 0.80219(15) 0.0180(9) Uani 1 1 d . . .
N20 N 0.1746(5) 1.0134(2) 0.78300(18) 0.0213(10) Uani 1 1 d D . .
H20N H 0.172(8) 1.021(3) 0.7485(10) 0.07(2) Uiso 1 1 d D . .
C23 C 0.4738(6) 0.7367(3) 0.72821(19) 0.0203(11) Uani 1 1 d . . .
H23 H 0.5747 0.7136 0.7330 0.024 Uiso 1 1 calc R . .
C24 C 0.4076(6) 0.7503(3) 0.67924(19) 0.0223(12) Uani 1 1 d . . .
H24 H 0.4531 0.7387 0.6447 0.027 Uiso 1 1 calc R . .
C25 C 0.2570(6) 0.7856(3) 0.69245(19) 0.0184(11) Uani 1 1 d . . .
C26 C 0.1240(6) 0.8169(3) 0.66212(19) 0.0199(11) Uani 1 1 d . . .
C27 C 0.1146(6) 0.8225(3) 0.60696(19) 0.0232(12) Uani 1 1 d . . .
H27 H 0.1990 0.8043 0.5836 0.028 Uiso 1 1 calc R . .
C28 C -0.0239(7) 0.8558(3) 0.5872(2) 0.0255(13) Uani 1 1 d . . .
H28 H -0.0316 0.8612 0.5503 0.031 Uiso 1 1 calc R . .
C29 C -0.1519(6) 0.8815(3) 0.62205(19) 0.0220(12) Uani 1 1 d . . .
H29 H -0.2460 0.9028 0.6087 0.026 Uiso 1 1 calc R . .
C30 C -0.1352(6) 0.8744(3) 0.67693(19) 0.0185(11) Uani 1 1 d . . .
C31 C -0.2514(6) 0.8965(3) 0.72059(18) 0.0155(11) Uani 1 1 d . . .
C32 C -0.4065(6) 0.9312(3) 0.7248(2) 0.0201(11) Uani 1 1 d . . .
H32 H -0.4666 0.9503 0.6973 0.024 Uiso 1 1 calc R . .
C33 C -0.4500(6) 0.9308(3) 0.77844(19) 0.0200(11) Uani 1 1 d . . .
H33 H -0.5478 0.9495 0.7942 0.024 Uiso 1 1 calc R . .
C34 C -0.1853(6) 0.5945(3) 0.7614(2) 0.0272(13) Uani 1 1 d . . .
H34 H -0.2295 0.5440 0.7439 0.033 Uiso 1 1 calc R . .
C35 C -0.1650(6) 0.6168(3) 0.8166(2) 0.0261(13) Uani 1 1 d . . .
H35 H -0.1917 0.5854 0.8440 0.031 Uiso 1 1 calc R . .
C36 C -0.0955(6) 0.6974(3) 0.8230(2) 0.0212(12) Uani 1 1 d . . .
C37 C -0.0343(6) 0.7581(3) 0.86837(19) 0.0194(11) Uani 1 1 d . . .
C38 C -0.0333(7) 0.7518(3) 0.9239(2) 0.0287(13) Uani 1 1 d . . .
H38 H -0.0725 0.7038 0.9364 0.034 Uiso 1 1 calc R . .
C39 C 0.0278(7) 0.8191(3) 0.9601(2) 0.0322(14) Uani 1 1 d . . .
H39 H 0.0280 0.8164 0.9975 0.039 Uiso 1 1 calc R . .
C40 C 0.0884(7) 0.8903(3) 0.9420(2) 0.0295(13) Uani 1 1 d . . .
H40 H 0.1297 0.9353 0.9666 0.035 Uiso 1 1 calc R . .
C41 C 0.0859(6) 0.8926(3) 0.8862(2) 0.0220(12) Uani 1 1 d . . .
C42 C 0.1407(6) 0.9597(3) 0.85758(18) 0.0170(11) Uani 1 1 d . . .
C43 C 0.2139(6) 1.0384(3) 0.8725(2) 0.0267(13) Uani 1 1 d . . .
H43 H 0.2432 1.0641 0.9077 0.032 Uiso 1 1 calc R . .
C44 C 0.2339(6) 1.0705(3) 0.8244(2) 0.0264(13) Uani 1 1 d . . .
H44 H 0.2802 1.1224 0.8210 0.032 Uiso 1 1 calc R . .
O1 O 0.3981(5) 0.7521(2) 0.87165(14) 0.0339(9) Uani 1 1 d . . .
O2 O 0.6086(5) 0.8436(2) 0.90070(13) 0.0307(9) Uani 1 1 d . . .
O3 O 0.3541(5) 0.6259(2) 1.12945(13) 0.0296(9) Uani 1 1 d . . .
O4 O 0.5707(5) 0.7144(2) 1.15710(14) 0.0337(9) Uani 1 1 d . . .
C45 C 0.4886(7) 0.7614(3) 0.9633(2) 0.0233(12) Uani 1 1 d . . .
C46 C 0.3655(7) 0.7046(3) 0.9746(2) 0.0254(13) Uani 1 1 d . . .
H46 H 0.2870 0.6839 0.9475 0.030 Uiso 1 1 calc R . .
C47 C 0.3562(7) 0.6777(3) 1.0251(2) 0.0267(13) Uani 1 1 d . . .
H47 H 0.2723 0.6396 1.0317 0.032 Uiso 1 1 calc R . .
C48 C 0.4724(7) 0.7079(3) 1.06584(19) 0.0217(12) Uani 1 1 d . . .
C49 C 0.5964(7) 0.7644(3) 1.05526(19) 0.0245(12) Uani 1 1 d . . .
H49 H 0.6747 0.7847 1.0825 0.029 Uiso 1 1 calc R . .
C50 C 0.6060(6) 0.7914(3) 1.00471(19) 0.0233(12) Uani 1 1 d . . .
H50 H 0.6903 0.8294 0.9982 0.028 Uiso 1 1 calc R . .
C51 C 0.4989(7) 0.7884(3) 0.9074(2) 0.0265(13) Uani 1 1 d . . .
C52 C 0.4656(7) 0.6802(3) 1.1217(2) 0.0266(13) Uani 1 1 d . . .
O5 O -0.3229(4) 0.10406(19) 0.58356(13) 0.0265(9) Uani 1 1 d . . .
O6 O -0.0953(4) 0.10410(19) 0.63634(13) 0.0261(9) Uani 1 1 d . . .
O7 O 0.2034(5) 0.6030(2) 0.59359(15) 0.0428(11) Uani 1 1 d . . .
O8 O 0.1936(5) 0.4702(2) 0.60427(14) 0.0380(10) Uani 1 1 d . . .
C53 C -0.0838(6) 0.0430(3) 0.54348(18) 0.0187(11) Uani 1 1 d . . .
C54 C -0.1724(6) -0.0063(3) 0.50123(19) 0.0195(11) Uani 1 1 d . . .
H54 H -0.2878 -0.0107 0.5017 0.023 Uiso 1 1 calc R . .
C55 C 0.0885(6) 0.0491(3) 0.54177(19) 0.0205(12) Uani 1 1 d . . .
H55 H 0.1485 0.0823 0.5698 0.025 Uiso 1 1 calc R . .
C56 C -0.1733(7) 0.0875(3) 0.5916(2) 0.0234(12) Uani 1 1 d . . .
C57 C 0.3787(6) 0.5144(3) 0.53959(19) 0.0242(12) Uani 1 1 d . . .
C58 C 0.4429(7) 0.5775(3) 0.51338(19) 0.0264(13) Uani 1 1 d . . .
H58 H 0.4040 0.6299 0.5222 0.032 Uiso 1 1 calc R . .
C59 C 0.4352(7) 0.4358(3) 0.52596(19) 0.0284(13) Uani 1 1 d . . .
H59 H 0.3920 0.3926 0.5429 0.034 Uiso 1 1 calc R . .
C60 C 0.2446(7) 0.5299(3) 0.5821(2) 0.0302(14) Uani 1 1 d . . .
O1S O -0.2247(5) 0.5201(2) 0.93118(16) 0.0381(10) Uani 1 1 d . . .
H1S H -0.2402 0.4750 0.9124 0.057 Uiso 1 1 calc R . .
C1S C -0.3791(7) 0.5566(3) 0.9411(2) 0.0487(18) Uani 1 1 d . . .
H1S1 H -0.4539 0.5196 0.9569 0.073 Uiso 1 1 calc R . .
H1S2 H -0.4256 0.5677 0.9071 0.073 Uiso 1 1 calc R . .
H1S3 H -0.3622 0.6071 0.9658 0.073 Uiso 1 1 calc R . .
O2S O 0.5822(5) 0.1311(2) 0.48270(15) 0.0457(11) Uani 1 1 d . . .
H2S H 0.6032 0.1171 0.5124 0.069 Uiso 1 1 calc R . .
C2S C 0.4722(7) 0.1949(3) 0.4899(2) 0.0376(15) Uani 1 1 d . . .
H2S1 H 0.5136 0.2369 0.5187 0.056 Uiso 1 1 calc R . .
H2S2 H 0.3650 0.1735 0.4994 0.056 Uiso 1 1 calc R . .
H2S3 H 0.4626 0.2178 0.4565 0.056 Uiso 1 1 calc R . .
O3S O -0.0851(5) 0.6441(2) 0.62994(15) 0.0390(10) Uani 1 1 d . . .
H3S H 0.0082 0.6327 0.6195 0.059 Uiso 1 1 calc R . .
C3S C -0.1997(11) 0.6032(5) 0.5944(3) 0.109(3) Uani 1 1 d U . .
H3S1 H -0.2919 0.6369 0.5916 0.164 Uiso 1 1 calc R . .
H3S2 H -0.2377 0.5532 0.6073 0.164 Uiso 1 1 calc R . .
H3S3 H -0.1511 0.5903 0.5591 0.164 Uiso 1 1 calc R . .
O4S O -0.2588(7) 0.9895(3) 0.9550(2) 0.089(2) Uani 1 1 d . . .
H4S H -0.2888 0.9427 0.9408 0.134 Uiso 1 1 calc R . .
C4S C -0.3680(8) 1.0431(4) 0.9412(3) 0.062(2) Uani 1 1 d . . .
H4S1 H -0.4734 1.0325 0.9574 0.093 Uiso 1 1 calc R . .
H4S2 H -0.3813 1.0364 0.9021 0.093 Uiso 1 1 calc R . .
H4S3 H -0.3269 1.0983 0.9545 0.093 Uiso 1 1 calc R . .
O1W O 0.1675(5) 0.0266(2) 0.67790(14) 0.0326(10) Uani 1 1 d D . .
H1WA H 0.242(4) 0.016(3) 0.6559(16) 0.039 Uiso 1 1 d D . .
H1WB H 0.103(5) 0.053(3) 0.6621(17) 0.039 Uiso 1 1 d D . .
O2W O 0.4363(5) -0.0122(2) 0.61125(14) 0.0327(9) Uani 1 1 d D . .
H2WA H 0.435(7) -0.0467(19) 0.5827(13) 0.039 Uiso 1 1 d D . .
H2WB H 0.480(6) 0.0293(17) 0.6026(18) 0.039 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
Fe1 N3 1.921(4) . ?
Fe1 N8 1.923(4) . ?
Fe1 N9 1.959(4) . ?
Fe1 N7 1.968(4) . ?
Fe1 N2 1.974(4) . ?
Fe1 N4 1.985(4) . ?
N1 N2 1.346(5) . ?
N1 C1 1.345(6) . ?
N2 C3 1.358(5) . ?
N3 C4 1.363(6) . ?
N3 C8 1.365(5) . ?
N4 N5 1.348(5) . ?
N4 C9 1.349(5) . ?
N5 C11 1.341(6) . ?
N6 C12 1.345(6) . ?
N6 N7 1.353(5) . ?
N7 C14 1.342(5) . ?
N8 C15 1.356(5) . ?
N8 C19 1.363(6) . ?
N9 N10 1.345(5) . ?
N9 C20 1.356(6) . ?
N10 C22 1.339(6) . ?
C1 C2 1.367(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.454(6) . ?
C4 C5 1.372(6) . ?
C5 C6 1.396(6) . ?
C6 C7 1.380(6) . ?
C7 C8 1.377(6) . ?
C8 C9 1.450(6) . ?
C9 C10 1.403(6) . ?
C10 C11 1.363(6) . ?
C12 C13 1.363(7) . ?
C13 C14 1.395(6) . ?
C14 C15 1.453(6) . ?
C15 C16 1.390(6) . ?
C16 C17 1.385(6) . ?
C17 C18 1.388(6) . ?
C18 C19 1.381(6) . ?
C19 C20 1.448(6) . ?
C20 C21 1.393(6) . ?
C21 C22 1.380(6) . ?
Fe2 N13 1.909(4) . ?
Fe2 N18 1.922(4) . ?
Fe2 N17 1.956(4) . ?
Fe2 N14 1.960(4) . ?
Fe2 N19 1.970(4) . ?
Fe2 N12 1.982(4) . ?
N11 C23 1.343(6) . ?
N11 N12 1.352(5) . ?
N12 C25 1.345(5) . ?
N13 C26 1.357(6) . ?
N13 C30 1.371(6) . ?
N14 N15 1.347(5) . ?
N14 C31 1.362(5) . ?
N15 C33 1.357(6) . ?
N16 N17 1.342(5) . ?
N16 C34 1.346(6) . ?
N17 C36 1.354(5) . ?
N18 C41 1.350(6) . ?
N18 C37 1.354(5) . ?
N19 N20 1.353(5) . ?
N19 C42 1.362(5) . ?
N20 C44 1.347(6) . ?
C23 C24 1.369(6) . ?
C24 C25 1.396(6) . ?
C25 C26 1.460(6) . ?
C26 C27 1.380(6) . ?
C27 C28 1.385(6) . ?
C28 C29 1.394(6) . ?
C29 C30 1.382(6) . ?
C30 C31 1.454(6) . ?
C31 C32 1.401(6) . ?
C32 C33 1.375(6) . ?
C34 C35 1.366(7) . ?
C35 C36 1.397(6) . ?
C36 C37 1.451(7) . ?
C37 C38 1.390(6) . ?
C38 C39 1.382(7) . ?
C39 C40 1.379(7) . ?
C40 C41 1.385(6) . ?
C41 C42 1.447(6) . ?
C42 C43 1.392(6) . ?
C43 C44 1.375(6) . ?
O1 C51 1.255(6) . ?
O2 C51 1.262(6) . ?
O3 C52 1.269(6) . ?
O4 C52 1.260(6) . ?
C45 C46 1.385(7) . ?
C45 C50 1.402(7) . ?
C45 C51 1.512(7) . ?
C46 C47 1.385(6) . ?
C47 C48 1.385(7) . ?
C48 C49 1.381(7) . ?
C48 C52 1.515(6) . ?
C49 C50 1.385(6) . ?
O5 C56 1.271(6) . ?
O6 C56 1.252(6) . ?
O7 C60 1.259(6) . ?
O8 C60 1.246(6) . ?
C53 C54 1.390(6) . ?
C53 C55 1.389(7) . ?
C53 C56 1.514(6) . ?
C54 C55 1.389(6) 2_556 ?
C55 C54 1.389(6) 2_556 ?
C57 C58 1.382(7) . ?
C57 C59 1.391(6) . ?
C57 C60 1.519(7) . ?
C58 C59 1.392(7) 2_666 ?
C59 C58 1.392(7) 2_666 ?
O1S C1S 1.419(6) . ?
O2S C2S 1.403(5) . ?
O3S C3S 1.349(8) . ?
O4S C4S 1.354(6) . ?

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
N3 Fe1 N8 175.08(15) . . ?
N3 Fe1 N9 96.12(16) . . ?
N8 Fe1 N9 79.21(16) . . ?
N3 Fe1 N7 105.91(16) . . ?
N8 Fe1 N7 78.76(16) . . ?
N9 Fe1 N7 157.97(16) . . ?
N3 Fe1 N2 79.17(16) . . ?
N8 Fe1 N2 99.28(15) . . ?
N9 Fe1 N2 91.46(15) . . ?
N7 Fe1 N2 92.26(16) . . ?
N3 Fe1 N4 78.62(16) . . ?
N8 Fe1 N4 103.11(15) . . ?
N9 Fe1 N4 93.93(16) . . ?
N7 Fe1 N4 90.85(15) . . ?
N2 Fe1 N4 157.58(16) . . ?
N2 N1 C1 110.5(4) . . ?
N1 N2 C3 105.8(4) . . ?
N1 N2 Fe1 138.1(3) . . ?
C3 N2 Fe1 116.0(3) . . ?
C4 N3 C8 119.5(4) . . ?
C4 N3 Fe1 119.6(3) . . ?
C8 N3 Fe1 120.7(3) . . ?
N5 N4 C9 106.2(4) . . ?
N5 N4 Fe1 137.2(3) . . ?
C9 N4 Fe1 116.2(3) . . ?
C11 N5 N4 110.2(4) . . ?
C12 N6 N7 110.2(4) . . ?
C14 N7 N6 105.6(4) . . ?
C14 N7 Fe1 116.7(3) . . ?
N6 N7 Fe1 137.6(3) . . ?
C15 N8 C19 120.3(4) . . ?
C15 N8 Fe1 120.2(3) . . ?
C19 N8 Fe1 119.5(3) . . ?
N10 N9 C20 105.9(4) . . ?
N10 N9 Fe1 137.2(3) . . ?
C20 N9 Fe1 116.9(3) . . ?
C22 N10 N9 110.9(4) . . ?
N1 C1 C2 108.9(4) . . ?
C1 C2 C3 104.6(4) . . ?
N2 C3 C2 110.3(4) . . ?
N2 C3 C4 113.8(4) . . ?
C2 C3 C4 135.8(4) . . ?
N3 C4 C5 121.3(4) . . ?
N3 C4 C3 110.6(4) . . ?
C5 C4 C3 128.2(5) . . ?
C4 C5 C6 119.0(5) . . ?
C7 C6 C5 120.0(5) . . ?
C8 C7 C6 119.1(5) . . ?
N3 C8 C7 121.2(4) . . ?
N3 C8 C9 109.7(4) . . ?
C7 C8 C9 129.1(4) . . ?
N4 C9 C10 109.8(4) . . ?
N4 C9 C8 114.6(4) . . ?
C10 C9 C8 135.6(4) . . ?
C11 C10 C9 104.6(4) . . ?
N5 C11 C10 109.1(5) . . ?
N6 C12 C13 108.9(4) . . ?
C12 C13 C14 104.4(4) . . ?
N7 C14 C13 110.8(4) . . ?
N7 C14 C15 114.2(4) . . ?
C13 C14 C15 135.0(4) . . ?
N8 C15 C16 120.8(4) . . ?
N8 C15 C14 110.1(4) . . ?
C16 C15 C14 129.1(4) . . ?
C17 C16 C15 118.9(5) . . ?
C16 C17 C18 120.1(5) . . ?
C19 C18 C17 119.1(5) . . ?
N8 C19 C18 120.8(4) . . ?
N8 C19 C20 110.8(4) . . ?
C18 C19 C20 128.4(5) . . ?
N9 C20 C21 110.1(4) . . ?
N9 C20 C19 113.6(4) . . ?
C21 C20 C19 136.3(5) . . ?
C22 C21 C20 104.7(4) . . ?
N10 C22 C21 108.3(4) . . ?
N13 Fe2 N18 177.57(17) . . ?
N13 Fe2 N17 100.38(16) . . ?
N18 Fe2 N17 79.27(16) . . ?
N13 Fe2 N14 79.67(16) . . ?
N18 Fe2 N14 97.93(16) . . ?
N17 Fe2 N14 92.26(16) . . ?
N13 Fe2 N19 101.00(15) . . ?
N18 Fe2 N19 79.37(16) . . ?
N17 Fe2 N19 158.62(16) . . ?
N14 Fe2 N19 91.53(15) . . ?
N13 Fe2 N12 78.74(16) . . ?
N18 Fe2 N12 103.65(16) . . ?
N17 Fe2 N12 90.70(15) . . ?
N14 Fe2 N12 158.39(15) . . ?
N19 Fe2 N12 93.48(16) . . ?
C23 N11 N12 110.1(4) . . ?
C25 N12 N11 106.4(4) . . ?
C25 N12 Fe2 116.1(3) . . ?
N11 N12 Fe2 137.4(3) . . ?
C26 N13 C30 119.1(4) . . ?
C26 N13 Fe2 121.2(3) . . ?
C30 N13 Fe2 119.7(3) . . ?
N15 N14 C31 105.6(4) . . ?
N15 N14 Fe2 137.9(3) . . ?
C31 N14 Fe2 116.3(3) . . ?
N14 N15 C33 110.9(4) . . ?
N17 N16 C34 111.0(4) . . ?
N16 N17 C36 105.7(4) . . ?
N16 N17 Fe2 137.5(3) . . ?
C36 N17 Fe2 116.7(3) . . ?
C41 N18 C37 120.4(4) . . ?
C41 N18 Fe2 120.1(3) . . ?
C37 N18 Fe2 119.5(3) . . ?
N20 N19 C42 106.0(4) . . ?
N20 N19 Fe2 138.5(3) . . ?
C42 N19 Fe2 115.5(3) . . ?
C44 N20 N19 110.6(4) . . ?
N11 C23 C24 108.6(5) . . ?
C23 C24 C25 105.0(4) . . ?
N12 C25 C24 109.9(4) . . ?
N12 C25 C26 114.4(4) . . ?
C24 C25 C26 135.7(4) . . ?
N13 C26 C27 122.1(4) . . ?
N13 C26 C25 109.5(4) . . ?
C27 C26 C25 128.4(4) . . ?
C26 C27 C28 118.3(5) . . ?
C27 C28 C29 120.7(5) . . ?
C30 C29 C28 118.3(5) . . ?
N13 C30 C29 121.4(4) . . ?
N13 C30 C31 110.4(4) . . ?
C29 C30 C31 128.2(5) . . ?
N14 C31 C32 110.4(4) . . ?
N14 C31 C30 113.6(4) . . ?
C32 C31 C30 135.9(4) . . ?
C33 C32 C31 104.8(4) . . ?
N15 C33 C32 108.2(4) . . ?
N16 C34 C35 108.3(5) . . ?
C34 C35 C36 104.9(4) . . ?
N17 C36 C35 110.1(4) . . ?
N17 C36 C37 113.5(4) . . ?
C35 C36 C37 136.3(5) . . ?
N18 C37 C38 120.9(5) . . ?
N18 C37 C36 110.9(4) . . ?
C38 C37 C36 128.3(5) . . ?
C39 C38 C37 118.0(5) . . ?
C40 C39 C38 121.5(5) . . ?
C39 C40 C41 117.9(5) . . ?
N18 C41 C40 121.4(5) . . ?
N18 C41 C42 110.5(4) . . ?
C40 C41 C42 128.1(5) . . ?
N19 C42 C43 109.7(4) . . ?
N19 C42 C41 114.6(4) . . ?
C43 C42 C41 135.8(4) . . ?
C44 C43 C42 105.6(4) . . ?
N20 C44 C43 108.1(5) . . ?
C46 C45 C50 118.1(5) . . ?
C46 C45 C51 120.8(5) . . ?
C50 C45 C51 121.0(5) . . ?
C45 C46 C47 121.6(5) . . ?
C48 C47 C46 119.8(5) . . ?
C49 C48 C47 119.3(5) . . ?
C49 C48 C52 119.5(5) . . ?
C47 C48 C52 121.2(5) . . ?
C50 C49 C48 121.1(5) . . ?
C49 C50 C45 120.1(5) . . ?
O1 C51 O2 126.3(5) . . ?
O1 C51 C45 116.0(5) . . ?
O2 C51 C45 117.6(5) . . ?
O4 C52 O3 125.4(5) . . ?
O4 C52 C48 116.7(5) . . ?
O3 C52 C48 117.9(5) . . ?
C54 C53 C55 119.1(4) . . ?
C54 C53 C56 120.6(5) . . ?
C55 C53 C56 120.3(5) . . ?
C55 C54 C53 120.0(5) 2_556 . ?
C54 C55 C53 120.9(5) 2_556 . ?
O6 C56 O5 125.1(5) . . ?
O6 C56 C53 117.7(5) . . ?
O5 C56 C53 117.2(4) . . ?
C58 C57 C59 119.4(5) . . ?
C58 C57 C60 120.5(5) . . ?
C59 C57 C60 120.0(5) . . ?
C57 C58 C59 121.2(5) . 2_666 ?
C58 C59 C57 119.3(5) 2_666 . ?
O8 C60 O7 126.5(5) . . ?
O8 C60 C57 116.9(5) . . ?
O7 C60 C57 116.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.869
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.104
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol/water'
_chemical_properties_physical    ', Efflorescent'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-5H2O
_database_code_depnum_ccdc_archive 'CCDC 1491309'
_audit_update_record             
;
2016-07-06 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RFACR01_2-5H2O              
;
PROBLEM: The value of the weighted R factor is > 0.35
RESPONSE: The quality of the single crystals is low giving rise to a poor diffraction pattern. The comparative analysis of this crystal structure and that of the compound ?2-2MeOH-H2O? suggests that these crystals may be obtained as a result of desolvation and subsequent rehydration of ?2-2MeOH-H2O?, although this hypothesis has not been proven unambiguously. A crystal-to-crystal transformation of this kind may result in the low quality of the singles crystals of ?2-5H2O?.
;
_vrf_PLAT043_2-5H2O              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      10.08 Check
RESPONSE: The difference between the calculated and reported molecular weight is due to hydrogen atoms, which were added to the formula of the compound but not located in the structural resolution.
;
_vrf_PLAT084_2-5H2O              
;
PROBLEM: High wR2 Value (i.e. &gt; 0.25) ...................       0.36 Report
RESPONSE: The quality of the single crystals is low giving rise to a poor diffraction pattern. The comparative analysis of this crystal structure and that of the compound ?2-2MeOH-H2O? suggests that these crystals may be obtained as a result of desolvation and subsequent rehydration of ?2-2MeOH-H2O?, although this hypothesis has not been proven unambiguously. A crystal-to-crystal transformation of this kind may result in the low quality of the singles crystals of ?2-5H2O?.
;
_vrf_PLAT250_2-5H2O              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.7 Note
RESPONSE: Due to the reasons stated before, the displacement ellipsoids do not behave properly. In addition, the structure exhibits disorder in one of the terephthalate anions.
;
_vrf_PLAT250_2-5H2O_2            
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.5 Note
RESPONSE: Due to the reasons stated before, the displacement ellipsoids do not behave properly. In addition, the structure exhibits disorder in one of the terephthalate anions.
;
_vrf_PLAT306_2-5H2O              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check
RESPONSE: The hydrogen atoms of the water molecules were not located.
;
_vrf_PLAT430_2-5H2O              
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O2W     ..       2.72 Ang.
RESPONSE: We consider that these distances are within reasonable range for hydrogen-bonded water molecules.
;
_vrf_PLAT430_2-5H2O_2            
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O2      ..       2.74 Ang.
RESPONSE: We consider that these distances are within reasonable range for hydrogen-bonded water molecules.
;
_vrf_CHEMW03_2-5H2O              
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The difference between the calculated and reported molecular weight is due to hydrogen atoms, which were added to the formula of the compound but not located in the structural resolution.
;
# Added during the CSD deposition process: Wednesday 06 July 2016 06:33 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10, C8 H4 O4, 5(H2 O)'
_chemical_formula_sum            'C30 H32 Fe N10 O9'
_chemical_formula_weight         732.51

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.1799(4)
_cell_length_b                   8.0776(4)
_cell_length_c                   25.9260(12)
_cell_angle_alpha                90.532(4)
_cell_angle_beta                 93.150(4)
_cell_angle_gamma                89.370(4)
_cell_volume                     1710.28(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    120.00(10)
_cell_measurement_reflns_used    3434
_cell_measurement_theta_min      3.4470
_cell_measurement_theta_max      21.9420

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1197
_exptl_crystal_size_mid          0.0807
_exptl_crystal_size_min          0.0256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0128 -0.0004 0.0000 -0.9990 0.0082 0.0147 -0.0216
0 0 1 0.0128 0.0004 -0.0000 0.9990 -0.0082 -0.0147 0.0216
-1 0 0 0.0337 -0.9990 0.0001 0.0035 0.0741 0.0237 0.0384
1 0 0 0.0469 0.9990 -0.0001 -0.0035 -0.0741 -0.0237 -0.0384
0 -1 -1 0.0596 -0.0004 -0.9992 -0.9987 -0.0323 0.0857 0.0106
0 1 1 0.0457 0.0004 0.9992 0.9987 0.0323 -0.0857 -0.0106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22391
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_sigmaI/netI    0.1489
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         30.01
_diffrn_orient_matrix_UB_11      -0.0741551000
_diffrn_orient_matrix_UB_12      0.0405351000
_diffrn_orient_matrix_UB_13      -0.0082008000
_diffrn_orient_matrix_UB_21      -0.0238323000
_diffrn_orient_matrix_UB_22      -0.0709687000
_diffrn_orient_matrix_UB_23      -0.0147525000
_diffrn_orient_matrix_UB_31      -0.0384142000
_diffrn_orient_matrix_UB_32      -0.0321353000
_diffrn_orient_matrix_UB_33      0.0215852000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -95.00  -35.00   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777 -178.0000  -90.0000 80

#__ type_ start__ end____ width___ exp.time_
  2 omega  -96.00  -34.50   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777  178.0000 -120.0000 82

#__ type_ start__ end____ width___ exp.time_
  3 omega  -96.00  -34.50   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777  178.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   42.00   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -       20.8840  -57.0000 -180.0000 120

#__ type_ start__ end____ width___ exp.time_
  5 omega  -52.00   65.00   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -       20.8840  -19.0000 -120.0000 156

#__ type_ start__ end____ width___ exp.time_
  6 omega  -95.00  -35.00   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777 -178.0000    0.0000 80

#__ type_ start__ end____ width___ exp.time_
  7 omega  -90.00  -48.75   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777  -77.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
  8 omega  -90.00   10.50   0.7500   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.4777  -77.0000  -90.0000 134

;
_reflns_number_total             8562
_reflns_number_gt                4987
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1281P)²+12.1176P] 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         8562
_refine_ls_number_parameters     533
_refine_ls_number_restraints     161
_refine_ls_R_factor_all          0.1966
_refine_ls_R_factor_gt           0.1275
_refine_ls_wR_factor_ref         0.3580
_refine_ls_wR_factor_gt          0.3066
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_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
Fe1 Fe 0.01094(11) 0.05617(12) -0.24766(4) 0.0203(3) Uani 1 1 d . . .
N1 N -0.3392(7) 0.2050(7) -0.2472(3) 0.0302(14) Uani 1 1 d D . .
H1N H -0.353(10) 0.206(10) -0.2816(9) 0.036 Uiso 1 1 d D . .
N2 N -0.1969(7) 0.1489(7) -0.2247(2) 0.0251(12) Uani 1 1 d . . .
N3 N 0.0487(8) 0.0530(8) -0.1739(2) 0.0334(14) Uani 1 1 d . . .
N4 N 0.2334(6) -0.0359(7) -0.2414(2) 0.0248(12) Uani 1 1 d . . .
N5 N 0.3488(7) -0.0869(8) -0.2739(3) 0.0353(15) Uani 1 1 d D . .
H5N H 0.334(11) -0.069(11) -0.3080(11) 0.042 Uiso 1 1 d D . .
N6 N 0.1636(8) 0.4056(8) -0.2417(4) 0.048(2) Uani 1 1 d D . .
H6N H 0.160(13) 0.418(13) -0.2077(10) 0.058 Uiso 1 1 d D . .
N7 N 0.0931(6) 0.2758(7) -0.2657(3) 0.0285(13) Uani 1 1 d . . .
N8 N -0.0264(8) 0.0523(8) -0.3212(2) 0.0307(14) Uani 1 1 d . . .
N9 N -0.0850(7) -0.1638(7) -0.2574(2) 0.0233(12) Uani 1 1 d . . .
N10 N -0.1211(7) -0.2908(7) -0.2277(3) 0.0305(14) Uani 1 1 d D . .
H10N H -0.117(10) -0.296(10) -0.1933(9) 0.037 Uiso 1 1 d D . .
C1 C -0.4394(10) 0.2587(10) -0.2108(4) 0.043(2) Uani 1 1 d . . .
H1 H -0.5439 0.3029 -0.2173 0.051 Uiso 1 1 calc R . .
C2 C -0.3640(11) 0.2385(11) -0.1633(4) 0.050(2) Uani 1 1 d . . .
H2 H -0.4043 0.2661 -0.1314 0.060 Uiso 1 1 calc R . .
C3 C -0.2082(10) 0.1647(10) -0.1732(3) 0.0388(19) Uani 1 1 d . . .
C4 C -0.0669(11) 0.1101(12) -0.1429(3) 0.044(2) Uani 1 1 d . . .
C5 C -0.0448(16) 0.1032(18) -0.0900(4) 0.080(4) Uani 1 1 d . . .
H5 H -0.1268 0.1414 -0.0693 0.096 Uiso 1 1 calc R . .
C6 C 0.0940(18) 0.042(2) -0.0684(4) 0.094(5) Uani 1 1 d . . .
H6 H 0.1092 0.0367 -0.0326 0.112 Uiso 1 1 calc R . .
C7 C 0.2180(14) -0.0153(16) -0.1001(4) 0.070(3) Uani 1 1 d . . .
H7 H 0.3172 -0.0544 -0.0855 0.084 Uiso 1 1 calc R . .
C8 C 0.1902(10) -0.0125(10) -0.1527(3) 0.0398(19) Uani 1 1 d . . .
C9 C 0.2954(9) -0.0654(10) -0.1931(3) 0.0366(18) Uani 1 1 d . . .
C10 C 0.4519(10) -0.1369(11) -0.1937(4) 0.046(2) Uani 1 1 d . . .
H10 H 0.5204 -0.1700 -0.1659 0.055 Uiso 1 1 calc R . .
C11 C 0.4793(9) -0.1462(9) -0.2442(4) 0.044(2) Uani 1 1 d . . .
H11 H 0.5751 -0.1877 -0.2574 0.053 Uiso 1 1 calc R . .
C12 C 0.2095(11) 0.5162(11) -0.2755(6) 0.067(4) Uani 1 1 d . . .
H12 H 0.2608 0.6160 -0.2673 0.080 Uiso 1 1 calc R . .
C13 C 0.1701(13) 0.4606(12) -0.3230(6) 0.065(3) Uani 1 1 d . . .
H13 H 0.1885 0.5118 -0.3541 0.078 Uiso 1 1 calc R . .
C14 C 0.0944(10) 0.3075(10) -0.3159(4) 0.042(2) Uani 1 1 d . . .
C15 C 0.0187(13) 0.1793(11) -0.3490(3) 0.051(2) Uani 1 1 d U . .
C16 C -0.012(2) 0.1773(17) -0.4026(4) 0.103(5) Uani 1 1 d U . .
H16 H 0.0143 0.2680 -0.4222 0.123 Uiso 1 1 calc R . .
C17 C -0.0814(19) 0.0401(18) -0.4258(4) 0.090(3) Uani 1 1 d U . .
H17 H -0.0983 0.0353 -0.4616 0.108 Uiso 1 1 calc R . .
C18 C -0.126(2) -0.0889(16) -0.3965(4) 0.096(5) Uani 1 1 d U . .
H18 H -0.1758 -0.1809 -0.4120 0.116 Uiso 1 1 calc R . .
C19 C -0.0955(12) -0.0821(11) -0.3439(3) 0.047(2) Uani 1 1 d U . .
C20 C -0.1304(9) -0.2058(9) -0.3066(3) 0.0316(16) Uani 1 1 d . . .
C21 C -0.1988(10) -0.3659(10) -0.3070(4) 0.042(2) Uani 1 1 d . . .
H21 H -0.2409 -0.4255 -0.3355 0.050 Uiso 1 1 calc R . .
C22 C -0.1902(9) -0.4135(9) -0.2572(4) 0.043(2) Uani 1 1 d . . .
H22 H -0.2258 -0.5142 -0.2451 0.052 Uiso 1 1 calc R . .
C23 C 0.3705(16) 0.872(2) -0.4091(4) 0.082(4) Uani 1 1 d . A 1
O1 O 0.3242(13) 0.7194(11) -0.4073(3) 0.096(3) Uani 1 1 d . A 1
O2 O 0.3553(10) 0.9682(11) -0.3718(3) 0.073(2) Uani 1 1 d . A 1
C24 C 0.4310(15) 0.9367(14) -0.4558(4) 0.061(3) Uani 1 1 d . A 1
C25 C 0.5061(15) 0.8329(14) -0.4905(4) 0.062(3) Uani 1 1 d . . 1
H25 H 0.5086 0.7195 -0.4845 0.075 Uiso 1 1 calc R . 1
C26 C 0.4220(15) 1.1074(14) -0.4660(4) 0.064(3) Uani 1 1 d . . 1
H26 H 0.3690 1.1793 -0.4440 0.076 Uiso 1 1 calc R . 1
O3A O 0.9839(18) 0.6868(14) -0.1272(4) 0.0469(13) Uani 0.50 1 d PU B 2
O4A O 0.7262(17) 0.6995(14) -0.1010(4) 0.0462(14) Uani 0.50 1 d PU B 2
C27A C 0.871(3) 0.662(2) -0.0943(6) 0.0467(12) Uani 0.50 1 d PU B 2
C28A C 0.934(3) 0.585(2) -0.0457(7) 0.0467(12) Uani 0.50 1 d PU B 2
C29A C 1.103(3) 0.582(2) -0.0303(6) 0.0466(12) Uani 0.50 1 d PU . 2
H29A H 1.1758 0.6362 -0.0506 0.056 Uiso 0.50 1 calc PR . 2
C30A C 0.838(3) 0.498(2) -0.0134(6) 0.0465(13) Uani 0.50 1 d PU . 2
H30A H 0.7257 0.4926 -0.0218 0.056 Uiso 0.50 1 calc PR . 2
O3B O 1.1384(18) 0.4921(15) -0.1342(4) 0.0478(15) Uani 0.50 1 d PU C 1
O4B O 0.8909(18) 0.6348(15) -0.1315(4) 0.0472(13) Uani 0.50 1 d PU C 1
C27B C 1.009(3) 0.554(2) -0.1105(6) 0.0469(12) Uani 0.50 1 d PU C 1
C28B C 0.999(3) 0.537(2) -0.0509(7) 0.0467(12) Uani 0.50 1 d PU C 1
C29B C 1.091(2) 0.399(2) -0.0311(6) 0.0467(13) Uani 0.50 1 d PU . 1
H29B H 1.1465 0.3272 -0.0524 0.056 Uiso 0.50 1 calc PR . 1
C30B C 0.9080(5) 0.6219(5) -0.02284(14) 0.0466(12) Uani 0.50 1 d PU . 1
H30B H 0.8381 0.7009 -0.0382 0.056 Uiso 0.50 1 calc PR . 1
O1W O 0.5853(5) 0.2048(5) -0.34795(14) 0.076(2) Uani 1 1 d R . .
O2W O 0.5906(5) 0.4733(5) -0.41064(14) 0.058(3) Uani 0.60 1 d PRU . .
O3W O 0.1684(5) 0.5320(5) -0.49326(14) 0.045(3) Uani 0.50 1 d PRU . 1
O4W O 0.5798(5) 0.9238(5) -0.02458(14) 0.051(4) Uani 0.40 1 d PR . 1
O5W O 0.5501(5) 0.5777(5) -0.09303(14) 0.057(5) Uani 0.40 1 d PR . 1
O6W O 0.3912(5) 0.7011(5) 0.02084(14) 0.039(4) Uani 0.30 1 d PRU . 1
O7W O 0.5078(5) 0.7528(5) 0.00335(14) 0.061(4) Uani 0.50 1 d PR . 2
O8W O 0.4392(5) 0.5222(5) -0.07425(14) 0.043(3) Uani 0.50 1 d PR . 2
O9W O 1.2471(5) 0.4691(5) -0.14865(14) 0.065(4) Uani 0.50 1 d PR . 2
O10W O 0.6604(5) 0.9575(5) -0.04678(14) 0.043(5) Uani 0.30 1 d PR . 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
Fe1 N8 1.915(6) . ?
Fe1 N3 1.922(6) . ?
Fe1 N9 1.958(5) . ?
Fe1 N4 1.957(5) . ?
Fe1 N2 1.970(5) . ?
Fe1 N7 1.973(6) . ?
N1 C1 1.349(10) . ?
N1 N2 1.348(8) . ?
N2 C3 1.349(9) . ?
N3 C4 1.348(10) . ?
N3 C8 1.358(10) . ?
N4 C9 1.348(10) . ?
N4 N5 1.357(8) . ?
N5 C11 1.366(10) . ?
N6 C12 1.328(14) . ?
N6 N7 1.335(8) . ?
N7 C14 1.329(11) . ?
N8 C15 1.326(10) . ?
N8 C19 1.345(10) . ?
N9 N10 1.333(8) . ?
N9 C20 1.352(9) . ?
N10 C22 1.356(10) . ?
C1 C2 1.358(14) . ?
C2 C3 1.436(11) . ?
C3 C4 1.429(12) . ?
C4 C5 1.376(12) . ?
C5 C6 1.331(17) . ?
C6 C7 1.412(17) . ?
C7 C8 1.370(12) . ?
C8 C9 1.449(12) . ?
C9 C10 1.399(11) . ?
C10 C11 1.342(13) . ?
C12 C13 1.331(17) . ?
C13 C14 1.407(12) . ?
C14 C15 1.460(13) . ?
C15 C16 1.399(14) . ?
C16 C17 1.370(18) . ?
C17 C18 1.359(18) . ?
C18 C19 1.375(12) . ?
C19 C20 1.438(12) . ?
C20 C21 1.414(10) . ?
C21 C22 1.347(13) . ?
C23 O2 1.245(16) . ?
C23 O1 1.297(16) . ?
C23 C24 1.437(15) . ?
C24 C25 1.388(15) . ?
C24 C26 1.406(15) . ?
C25 C26 1.393(14) 2_674 ?
C26 C25 1.393(14) 2_674 ?
O3A C27A 1.31(2) . ?
O4A C27A 1.22(2) . ?
C27A C28A 1.48(2) . ?
C28A C30A 1.38(3) . ?
C28A C29A 1.42(3) . ?
C29A C30A 1.37(2) 2_765 ?
C30A C29A 1.37(2) 2_765 ?
O3B C27B 1.34(2) . ?
O4B C27B 1.26(2) . ?
C27B C28B 1.56(2) . ?
C28B C30B 1.26(2) . ?
C28B C29B 1.42(3) . ?
C29B C30B 1.410(16) 2_765 ?
C30B C29B 1.410(16) 2_765 ?

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
N8 Fe1 N3 178.3(3) . . ?
N8 Fe1 N9 79.8(2) . . ?
N3 Fe1 N9 98.6(3) . . ?
N8 Fe1 N4 100.1(3) . . ?
N3 Fe1 N4 79.2(3) . . ?
N9 Fe1 N4 92.1(2) . . ?
N8 Fe1 N2 102.1(3) . . ?
N3 Fe1 N2 78.5(3) . . ?
N9 Fe1 N2 91.6(2) . . ?
N4 Fe1 N2 157.7(3) . . ?
N8 Fe1 N7 79.1(3) . . ?
N3 Fe1 N7 102.5(3) . . ?
N9 Fe1 N7 158.9(3) . . ?
N4 Fe1 N7 91.6(2) . . ?
N2 Fe1 N7 92.8(2) . . ?
C1 N1 N2 110.1(7) . . ?
N1 N2 C3 107.2(6) . . ?
N1 N2 Fe1 136.9(5) . . ?
C3 N2 Fe1 115.9(5) . . ?
C4 N3 C8 119.8(7) . . ?
C4 N3 Fe1 120.4(5) . . ?
C8 N3 Fe1 119.8(5) . . ?
C9 N4 N5 106.6(6) . . ?
C9 N4 Fe1 116.4(5) . . ?
N5 N4 Fe1 137.0(5) . . ?
N4 N5 C11 107.5(7) . . ?
C12 N6 N7 111.1(9) . . ?
C14 N7 N6 105.7(7) . . ?
C14 N7 Fe1 115.8(5) . . ?
N6 N7 Fe1 138.2(6) . . ?
C15 N8 C19 121.1(7) . . ?
C15 N8 Fe1 120.0(6) . . ?
C19 N8 Fe1 118.8(5) . . ?
N10 N9 C20 107.2(6) . . ?
N10 N9 Fe1 137.2(5) . . ?
C20 N9 Fe1 115.6(5) . . ?
N9 N10 C22 110.0(7) . . ?
N1 C1 C2 109.5(7) . . ?
C1 C2 C3 104.5(7) . . ?
N2 C3 C4 114.9(7) . . ?
N2 C3 C2 108.7(8) . . ?
C4 C3 C2 136.4(8) . . ?
N3 C4 C5 121.3(9) . . ?
N3 C4 C3 110.3(7) . . ?
C5 C4 C3 128.4(9) . . ?
C6 C5 C4 120.0(10) . . ?
C5 C6 C7 119.6(9) . . ?
C8 C7 C6 119.2(9) . . ?
N3 C8 C7 120.1(9) . . ?
N3 C8 C9 110.1(7) . . ?
C7 C8 C9 129.7(8) . . ?
N4 C9 C10 111.0(8) . . ?
N4 C9 C8 114.3(6) . . ?
C10 C9 C8 134.6(8) . . ?
C11 C10 C9 103.4(8) . . ?
C10 C11 N5 111.4(7) . . ?
N6 C12 C13 108.7(8) . . ?
C12 C13 C14 105.0(10) . . ?
N7 C14 C13 109.5(9) . . ?
N7 C14 C15 114.0(7) . . ?
C13 C14 C15 136.5(10) . . ?
N8 C15 C16 119.7(10) . . ?
N8 C15 C14 110.9(7) . . ?
C16 C15 C14 129.4(9) . . ?
C17 C16 C15 119.2(11) . . ?
C18 C17 C16 119.9(11) . . ?
C17 C18 C19 119.4(11) . . ?
N8 C19 C18 120.5(9) . . ?
N8 C19 C20 111.7(6) . . ?
C18 C19 C20 127.8(9) . . ?
N9 C20 C21 108.6(7) . . ?
N9 C20 C19 114.0(6) . . ?
C21 C20 C19 137.3(7) . . ?
C22 C21 C20 105.4(7) . . ?
C21 C22 N10 108.9(7) . . ?
O2 C23 O1 121.2(11) . . ?
O2 C23 C24 118.5(13) . . ?
O1 C23 C24 120.2(13) . . ?
C25 C24 C26 118.8(10) . . ?
C25 C24 C23 120.6(11) . . ?
C26 C24 C23 120.6(11) . . ?
C26 C25 C24 122.3(10) 2_674 . ?
C25 C26 C24 118.9(11) 2_674 . ?
O4A C27A O3A 125.4(15) . . ?
O4A C27A C28A 121.0(19) . . ?
O3A C27A C28A 113.7(18) . . ?
C30A C28A C29A 114.0(16) . . ?
C30A C28A C27A 123.8(19) . . ?
C29A C28A C27A 122.0(18) . . ?
C30A C29A C28A 122.0(19) 2_765 . ?
C29A C30A C28A 124.0(19) 2_765 . ?
O4B C27B O3B 126.2(15) . . ?
O4B C27B C28B 113.3(18) . . ?
O3B C27B C28B 120.5(15) . . ?
C30B C28B C29B 121.8(16) . . ?
C30B C28B C27B 125.8(16) . . ?
C29B C28B C27B 112.1(17) . . ?
C30B C29B C28B 115.6(16) 2_765 . ?
C28B C30B C29B 122.0(11) . 2_765 ?

_diffrn_measured_fraction_theta_max 0.856
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.084
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.156





_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol/water'
_chemical_properties_physical    ', Efflorescent'
_exptl_crystal_preparation       ', Magnetic properties'
