# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_MRT4C-2-H
_database_code_depnum_ccdc_archive 'CCDC 2335499'
loop_
_audit_author_name
_audit_author_address
'Carlos Gimenez-Saiz'
;University of Valencia
Spain
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_MRT4C-2-H           
;
PROBLEM: D-H Bond Without Acceptor O1W --H1W2 . Please Check 
RESPONSE: Although other alternative hydrogen bonding interactions 
are possible in this structure, all of them would yield at least one  
water hydrogen atom without a suitable acceptor. In the present 
model, H1W2 is located at 3.28 and 3.38 A from the centroids 
of a pyrazol and a pyridine ring, respectively, which are very long 
distances compared to typical O-H...pi acceptor interactions (lower 
than 2.50 Angstrom, see Angew. Chem. Int. Ed. 2002, 41, 48-76). 
However, such distances increase when more than one aromatic ring is 
involved. In particular, quite a few crystal structures can be found 
in the database in which water H atoms (with no other suitable 
hydrogen bond acceptors) are located at distances between 3.0-3.5 A 
from the centroids of two, or more, non-fused aromatic rings. The 
following CCDC numbers represent some examples of this: 705560, 
1409564, 916311, 763194, 1961549, 1561107, 1945990, 990239, 716966, 
2082126, 1539943, 1038130, 2097742.
;
_vrf_PLAT910_MRT4C-2-H           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).   12 Note
RESPONSE: Probably caused by the beamstop. It should not be a problem 
as we did not perform any solvent modelling refinement technique.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10 2+, C16 H8 O4 2-, 9(H2 O)'
_chemical_formula_sum            'C38 H44 Fe N10 O13'
_chemical_formula_weight         904.68

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   11.9374(2)
_cell_length_b                   14.5137(2)
_cell_length_c                   23.8247(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4127.77(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.00(10)
_cell_measurement_reflns_used    14889
_cell_measurement_theta_min      3.3830
_cell_measurement_theta_max      27.7400

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             1888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2448
_exptl_crystal_size_mid          0.0738
_exptl_crystal_size_min          0.0333
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
'SuperNova, Single source at offset, Sapphire3'
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            100177
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.285
_diffrn_reflns_theta_max         29.923
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_orient_matrix_UB_11      -0.0338553000
_diffrn_orient_matrix_UB_12      -0.0235491000
_diffrn_orient_matrix_UB_13      0.0198145000
_diffrn_orient_matrix_UB_21      -0.0402597000
_diffrn_orient_matrix_UB_22      0.0358637000
_diffrn_orient_matrix_UB_23      -0.0014358000
_diffrn_orient_matrix_UB_31      -0.0276290000
_diffrn_orient_matrix_UB_32      -0.0234016000
_diffrn_orient_matrix_UB_33      -0.0221743000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00  28.00   1.00   22.50    --  -20.96 -19.00  60.00  123
  2  ω    -92.00  11.00   1.00   22.50    --  -20.96 -77.00-120.00  103
  3  ω    -90.00   1.00   1.00   22.50    --  -20.96 -57.00   0.00   91
  4  ω    -20.00  65.00   1.00   22.50    --   21.90 -99.00 150.00   85
  5  ω    -20.00  65.00   1.00   22.50    --   21.90 -99.00  30.00   85
  6  ω    -20.00  65.00   1.00   22.50    --   21.90 -99.00 -30.00   85
  7  ω    -99.00 -35.00   1.00   22.50    --  -20.96-178.00 120.00   64
  8  ω    -48.00  52.00   1.00   22.50    --  -20.96  38.00-120.00  100
  9  ω    -90.00   1.00   1.00   22.50    --  -20.96 -57.00 -90.00   91
 10  ω    -10.00  93.00   1.00   22.50    --   21.90  77.00 150.00  103
 11  ω     35.00 100.00   1.00   22.50    --   21.90 178.00 150.00   65
 12  ω    -49.00  15.00   1.00   22.50    --   21.90 -77.00-180.00   64
 13  ω      0.00  91.00   1.00   22.50    --   21.90  57.00 -90.00   91
;
_reflns_number_total             11400
_reflns_number_gt                9136
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.927
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²+2.0430P] 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_abs_structure_details 
;
 Flack x determined using 3126 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11400
_refine_ls_number_parameters     629
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1238
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.075
_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_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
Fe1 Fe 0.53791(5) 0.67608(4) 0.86568(2) 0.01555(13) Uani 1 1 d . . . . .
C1 C 0.3103(4) 0.4879(3) 0.93265(19) 0.0228(10) Uani 1 1 d . . . . .
H1 H 0.275230 0.452209 0.961109 0.027 Uiso 1 1 calc R U . . .
C2 C 0.2968(4) 0.4765(3) 0.87575(18) 0.0239(10) Uani 1 1 d . . . . .
H2 H 0.250831 0.432824 0.856989 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3655(4) 0.5435(3) 0.85173(16) 0.0182(9) Uani 1 1 d . . . . .
C4 C 0.4014(4) 0.5645(3) 0.79471(17) 0.0181(9) Uani 1 1 d . . . . .
C5 C 0.3623(4) 0.5282(3) 0.74477(17) 0.0215(9) Uani 1 1 d . . . . .
H5 H 0.301597 0.485906 0.744597 0.026 Uiso 1 1 calc R U . . .
C6 C 0.4135(4) 0.5545(3) 0.69468(18) 0.0239(10) Uani 1 1 d . . . . .
H6 H 0.387601 0.530338 0.659978 0.029 Uiso 1 1 calc R U . . .
C7 C 0.5020(4) 0.6161(3) 0.69565(17) 0.0224(10) Uani 1 1 d . . . . .
H7 H 0.537828 0.634012 0.661755 0.027 Uiso 1 1 calc R U . . .
C8 C 0.5379(4) 0.6515(3) 0.74689(16) 0.0180(8) Uani 1 1 d . . . . .
C9 C 0.6285(4) 0.7157(3) 0.75812(17) 0.0172(8) Uani 1 1 d . . . . .
C10 C 0.7106(4) 0.7594(3) 0.72499(18) 0.0206(9) Uani 1 1 d . . . . .
H10 H 0.719957 0.756412 0.685435 0.025 Uiso 1 1 calc R U . . .
C11 C 0.7741(4) 0.8076(3) 0.76336(18) 0.0215(9) Uani 1 1 d . . . . .
H11 H 0.837169 0.844945 0.754898 0.026 Uiso 1 1 calc R U . . .
C12 C 0.7419(4) 0.4558(3) 0.9114(2) 0.0300(11) Uani 1 1 d . . . . .
H12 H 0.773299 0.395767 0.908860 0.036 Uiso 1 1 calc R U . . .
C13 C 0.7588(4) 0.5169(3) 0.9540(2) 0.0294(11) Uani 1 1 d . . . . .
H13 H 0.803717 0.508627 0.986527 0.035 Uiso 1 1 calc R U . . .
C14 C 0.6959(4) 0.5945(3) 0.93943(18) 0.0205(9) Uani 1 1 d . . . . .
C15 C 0.6689(3) 0.6829(3) 0.96541(16) 0.0181(8) Uani 1 1 d . . . . .
C16 C 0.7092(4) 0.7173(3) 1.01598(18) 0.0223(9) Uani 1 1 d . . . . .
H16 H 0.762669 0.684164 1.037537 0.027 Uiso 1 1 calc R U . . .
C17 C 0.6684(4) 0.8025(3) 1.03389(17) 0.0194(9) Uani 1 1 d . . . . .
H17 H 0.693227 0.827587 1.068543 0.023 Uiso 1 1 calc R U . . .
C18 C 0.5916(4) 0.8507(3) 1.00147(16) 0.0186(9) Uani 1 1 d . . . . .
H18 H 0.564962 0.909302 1.013179 0.022 Uiso 1 1 calc R U . . .
C19 C 0.5547(3) 0.8119(3) 0.95179(16) 0.0169(8) Uani 1 1 d . . . . .
C20 C 0.4736(4) 0.8483(3) 0.91160(15) 0.0156(8) Uani 1 1 d . . . . .
C21 C 0.4138(4) 0.9310(3) 0.90598(17) 0.0201(9) Uani 1 1 d . . . . .
H21 H 0.416983 0.983551 0.929664 0.024 Uiso 1 1 calc R U . . .
C22 C 0.3497(4) 0.9192(3) 0.85879(18) 0.0219(9) Uani 1 1 d . . . . .
H22 H 0.298565 0.962615 0.843562 0.026 Uiso 1 1 calc R U . . .
C23 C 0.0087(4) 1.0201(3) 0.84151(18) 0.0248(10) Uani 1 1 d . . . . .
H23 H -0.039078 1.037383 0.871606 0.030 Uiso 1 1 calc R U . . .
C24 C 0.0579(4) 1.0871(3) 0.80965(18) 0.0280(11) Uani 1 1 d . . . . .
H24 H 0.044960 1.150117 0.818145 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1282(4) 1.0631(3) 0.76404(19) 0.0251(10) Uani 1 1 d . . . . .
H25 H 0.163234 1.110152 0.742579 0.030 Uiso 1 1 calc R U . . .
C26 C 0.1455(4) 0.9734(3) 0.75087(17) 0.0205(9) Uani 1 1 d . . . . .
H26 H 0.190773 0.958601 0.719320 0.025 Uiso 1 1 calc R U . . .
C27 C 0.1036(4) 0.6427(3) 0.79616(19) 0.0222(9) Uani 1 1 d . . . . .
H27 H 0.154207 0.626489 0.767015 0.027 Uiso 1 1 calc R U . . .
C28 C 0.0577(4) 0.5759(3) 0.82846(19) 0.0259(10) Uani 1 1 d . . . . .
H28 H 0.077330 0.513391 0.822020 0.031 Uiso 1 1 calc R U . . .
C29 C -0.0190(4) 0.5980(3) 0.87172(18) 0.0268(10) Uani 1 1 d . . . . .
H29 H -0.052226 0.550088 0.893237 0.032 Uiso 1 1 calc R U . . .
C30 C -0.0455(4) 0.6872(3) 0.88259(16) 0.0224(9) Uani 1 1 d . . . . .
H30 H -0.097101 0.700943 0.911761 0.027 Uiso 1 1 calc R U . . .
C31 C -0.0179(3) 0.8545(3) 0.86344(17) 0.0179(8) Uani 1 1 d . . . . .
C32 C 0.1197(3) 0.8076(3) 0.77144(16) 0.0159(8) Uani 1 1 d . . . . .
C33 C 0.0279(4) 0.9244(3) 0.83038(16) 0.0181(8) Uani 1 1 d . . . . .
C34 C 0.0977(4) 0.9004(3) 0.78315(16) 0.0174(9) Uani 1 1 d . . . . .
C35 C 0.0028(4) 0.7608(3) 0.85106(16) 0.0184(9) Uani 1 1 d . . . . .
C36 C 0.0764(3) 0.7378(3) 0.80559(17) 0.0171(8) Uani 1 1 d . . . . .
C37 C -0.0894(4) 0.8802(3) 0.91385(18) 0.0240(10) Uani 1 1 d . . . . .
C38 C 0.1965(4) 0.7842(3) 0.72354(18) 0.0193(9) Uani 1 1 d . . . . .
N1 N 0.3813(3) 0.5579(3) 0.94097(15) 0.0204(8) Uani 1 1 d D . . . .
H1N H 0.399(4) 0.585(3) 0.9726(14) 0.033(15) Uiso 1 1 d D . . . .
N2 N 0.4165(3) 0.5934(2) 0.89199(14) 0.0174(7) Uani 1 1 d . . . . .
N3 N 0.4864(3) 0.6256(2) 0.79557(13) 0.0173(7) Uani 1 1 d . . . . .
N4 N 0.6431(3) 0.7359(2) 0.81290(14) 0.0185(7) Uani 1 1 d . . . . .
N5 N 0.7313(3) 0.7926(2) 0.81510(15) 0.0185(7) Uani 1 1 d D . . . .
H5N H 0.758(4) 0.818(3) 0.8467(14) 0.032(14) Uiso 1 1 d D . . . .
N6 N 0.6729(3) 0.4950(3) 0.87358(16) 0.0251(9) Uani 1 1 d D . . . .
H6N H 0.640(4) 0.464(3) 0.8458(17) 0.040(16) Uiso 1 1 d D . . . .
N7 N 0.6447(3) 0.5803(2) 0.88998(14) 0.0187(7) Uani 1 1 d . . . . .
N8 N 0.5929(3) 0.7283(2) 0.93467(14) 0.0165(7) Uani 1 1 d . . . . .
N9 N 0.4483(3) 0.7902(2) 0.86910(14) 0.0174(7) Uani 1 1 d . . . . .
N10 N 0.3726(3) 0.8341(3) 0.83760(14) 0.0187(7) Uani 1 1 d D . . . .
H10N H 0.344(3) 0.813(3) 0.8058(13) 0.018(12) Uiso 1 1 d D . . . .
O1 O -0.1938(3) 0.8752(2) 0.90922(13) 0.0252(7) Uani 1 1 d . . . . .
O2 O -0.0379(3) 0.9053(2) 0.95675(12) 0.0337(8) Uani 1 1 d . . . . .
O3 O 0.1571(3) 0.7809(2) 0.67518(12) 0.0254(7) Uani 1 1 d . . . . .
O4 O 0.2991(3) 0.7707(2) 0.73626(12) 0.0220(7) Uani 1 1 d . . . . .
O1W O 0.5431(3) 0.3668(3) 0.81718(15) 0.0369(8) Uani 1 1 d D . . . .
H1W1 H 0.585(4) 0.331(4) 0.800(2) 0.055 Uiso 1 1 d D U . . .
H1W2 H 0.490(3) 0.376(4) 0.798(2) 0.055 Uiso 1 1 d D U . . .
O2W O -0.0587(3) 0.8421(3) 0.63093(17) 0.0406(9) Uani 1 1 d D . . . .
H2W1 H -0.001(3) 0.820(4) 0.646(2) 0.061 Uiso 1 1 d D U . . .
H2W2 H -0.034(5) 0.864(4) 0.6020(16) 0.061 Uiso 1 1 d D U . . .
O3W O 0.3204(3) 0.5360(2) 0.55851(16) 0.0334(8) Uani 1 1 d D . . . .
H3W1 H 0.287(4) 0.492(2) 0.566(3) 0.050 Uiso 1 1 d D U . . .
H3W2 H 0.284(4) 0.582(2) 0.560(3) 0.050 Uiso 1 1 d D U . . .
O4W O 0.5423(4) 0.3054(3) 0.93113(17) 0.0540(11) Uani 1 1 d D . . . .
H4W1 H 0.474(4) 0.278(5) 0.933(3) 0.081 Uiso 1 1 d D U . . .
H4W2 H 0.540(6) 0.316(5) 0.8949(12) 0.081 Uiso 1 1 d D U . . .
O5W O -0.0148(4) 0.9189(3) 0.52263(16) 0.0458(10) Uani 1 1 d D . . . .
H5W1 H -0.061(4) 0.922(5) 0.495(2) 0.069 Uiso 1 1 d D U . . .
H5W2 H 0.028(5) 0.880(4) 0.505(2) 0.069 Uiso 1 1 d D U . . .
O6W O 0.0488(6) 1.0913(3) 0.96954(19) 0.0800(18) Uani 1 1 d D . . . .
H6W1 H 0.031(9) 1.108(5) 1.0019(19) 0.120 Uiso 1 1 d D U . . .
H6W2 H 0.047(9) 1.0347(18) 0.971(3) 0.120 Uiso 1 1 d D U . . .
O7W O 0.2511(4) 0.7111(3) 0.57983(17) 0.0478(11) Uani 1 1 d D . . . .
H7W1 H 0.315(3) 0.732(3) 0.573(2) 0.072 Uiso 1 1 d D U . . .
H7W2 H 0.238(5) 0.725(5) 0.6129(14) 0.072 Uiso 1 1 d D U . . .
O8W O 0.1315(4) 0.7807(3) 0.48698(17) 0.0529(12) Uani 1 1 d D . . . .
H8W1 H 0.190(2) 0.780(4) 0.4669(15) 0.079 Uiso 1 1 d D U . . .
H8W2 H 0.159(4) 0.759(4) 0.5181(15) 0.079 Uiso 1 1 d D U . . .
O9W O 0.1999(4) 0.2010(3) 0.90987(19) 0.0546(12) Uani 1 1 d D . . . .
H9W1 H 0.160(4) 0.158(3) 0.925(2) 0.082 Uiso 1 1 d D U . . .
H9W2 H 0.152(5) 0.244(3) 0.916(3) 0.082 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
Fe1 N3 1.925(3) . ?
Fe1 N8 1.925(3) . ?
Fe1 N7 1.973(4) . ?
Fe1 N9 1.974(3) . ?
Fe1 N4 1.978(4) . ?
Fe1 N2 1.984(4) . ?
C1 N1 1.339(6) . ?
C1 C2 1.375(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.395(6) . ?
C2 H2 0.9500 . ?
C3 N2 1.347(5) . ?
C3 C4 1.457(6) . ?
C4 N3 1.347(6) . ?
C4 C5 1.382(6) . ?
C5 C6 1.394(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(5) . ?
C7 H7 0.9500 . ?
C8 N3 1.366(5) . ?
C8 C9 1.452(6) . ?
C9 N4 1.349(5) . ?
C9 C10 1.409(6) . ?
C10 C11 1.378(6) . ?
C10 H10 0.9500 . ?
C11 N5 1.352(5) . ?
C11 H11 0.9500 . ?
C12 N6 1.347(6) . ?
C12 C13 1.363(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.397(6) . ?
C13 H13 0.9500 . ?
C14 N7 1.344(5) . ?
C14 C15 1.460(6) . ?
C15 N8 1.340(5) . ?
C15 C16 1.390(6) . ?
C16 C17 1.395(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(5) . ?
C18 H18 0.9500 . ?
C19 N8 1.359(5) . ?
C19 C20 1.461(6) . ?
C20 N9 1.351(5) . ?
C20 C21 1.403(6) . ?
C21 C22 1.370(6) . ?
C21 H21 0.9500 . ?
C22 N10 1.362(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.366(6) . ?
C23 C33 1.433(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.415(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.356(6) . ?
C25 H25 0.9500 . ?
C26 C34 1.427(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.353(6) . ?
C27 C36 1.436(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.416(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.358(6) . ?
C29 H29 0.9500 . ?
C30 C35 1.427(6) . ?
C30 H30 0.9500 . ?
C31 C33 1.396(6) . ?
C31 C35 1.413(6) . ?
C31 C37 1.519(6) . ?
C32 C36 1.398(6) . ?
C32 C34 1.401(6) . ?
C32 C38 1.503(6) . ?
C33 C34 1.443(6) . ?
C35 C36 1.434(6) . ?
C37 O2 1.247(5) . ?
C37 O1 1.253(6) . ?
C38 O3 1.246(5) . ?
C38 O4 1.277(5) . ?
N1 N2 1.343(5) . ?
N1 H1N 0.88(2) . ?
N4 N5 1.337(5) . ?
N5 H5N 0.90(2) . ?
N6 N7 1.342(5) . ?
N6 H6N 0.89(3) . ?
N9 N10 1.336(5) . ?
N10 H10N 0.89(2) . ?
O1W H1W1 0.82(2) . ?
O1W H1W2 0.80(2) . ?
O2W H2W1 0.84(3) . ?
O2W H2W2 0.81(3) . ?
O3W H3W1 0.78(2) . ?
O3W H3W2 0.79(2) . ?
O4W H4W1 0.91(3) . ?
O4W H4W2 0.88(3) . ?
O5W H5W1 0.86(3) . ?
O5W H5W2 0.86(3) . ?
O6W H6W1 0.83(3) . ?
O6W H6W2 0.82(3) . ?
O7W H7W1 0.84(3) . ?
O7W H7W2 0.83(3) . ?
O8W H8W1 0.85(2) . ?
O8W H8W2 0.87(2) . ?
O9W H9W1 0.86(3) . ?
O9W H9W2 0.86(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
N3 Fe1 N8 178.36(16) . . ?
N3 Fe1 N7 101.12(14) . . ?
N8 Fe1 N7 78.85(15) . . ?
N3 Fe1 N9 100.48(14) . . ?
N8 Fe1 N9 79.59(14) . . ?
N7 Fe1 N9 158.37(14) . . ?
N3 Fe1 N4 79.54(15) . . ?
N8 Fe1 N4 98.82(15) . . ?
N7 Fe1 N4 94.91(15) . . ?
N9 Fe1 N4 90.12(14) . . ?
N3 Fe1 N2 79.06(14) . . ?
N8 Fe1 N2 102.57(14) . . ?
N7 Fe1 N2 87.30(14) . . ?
N9 Fe1 N2 95.66(15) . . ?
N4 Fe1 N2 158.51(14) . . ?
N1 C1 C2 108.1(4) . . ?
N1 C1 H1 125.9 . . ?
C2 C1 H1 125.9 . . ?
C1 C2 C3 104.6(4) . . ?
C1 C2 H2 127.7 . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 110.4(4) . . ?
N2 C3 C4 114.7(4) . . ?
C2 C3 C4 134.6(4) . . ?
N3 C4 C5 121.2(4) . . ?
N3 C4 C3 110.2(4) . . ?
C5 C4 C3 128.6(4) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C8 119.2(4) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
N3 C8 C7 120.3(4) . . ?
N3 C8 C9 110.8(3) . . ?
C7 C8 C9 128.9(4) . . ?
N4 C9 C10 110.7(4) . . ?
N4 C9 C8 114.5(4) . . ?
C10 C9 C8 134.7(4) . . ?
C11 C10 C9 103.8(4) . . ?
C11 C10 H10 128.1 . . ?
C9 C10 H10 128.1 . . ?
N5 C11 C10 108.4(4) . . ?
N5 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
N6 C12 C13 108.3(4) . . ?
N6 C12 H12 125.9 . . ?
C13 C12 H12 125.9 . . ?
C12 C13 C14 105.1(4) . . ?
C12 C13 H13 127.5 . . ?
C14 C13 H13 127.5 . . ?
N7 C14 C13 109.8(4) . . ?
N7 C14 C15 114.0(4) . . ?
C13 C14 C15 136.2(4) . . ?
N8 C15 C16 122.1(4) . . ?
N8 C15 C14 110.5(3) . . ?
C16 C15 C14 127.4(4) . . ?
C15 C16 C17 117.6(4) . . ?
C15 C16 H16 121.2 . . ?
C17 C16 H16 121.2 . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 C17 118.8(4) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
N8 C19 C18 120.9(4) . . ?
N8 C19 C20 110.4(3) . . ?
C18 C19 C20 128.7(4) . . ?
N9 C20 C21 110.4(4) . . ?
N9 C20 C19 114.5(3) . . ?
C21 C20 C19 135.2(4) . . ?
C22 C21 C20 104.8(4) . . ?
C22 C21 H21 127.6 . . ?
C20 C21 H21 127.6 . . ?
N10 C22 C21 107.8(4) . . ?
N10 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
C24 C23 C33 121.2(4) . . ?
C24 C23 H23 119.4 . . ?
C33 C23 H23 119.4 . . ?
C23 C24 C25 120.5(4) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C34 121.8(4) . . ?
C25 C26 H26 119.1 . . ?
C34 C26 H26 119.1 . . ?
C28 C27 C36 120.5(4) . . ?
C28 C27 H27 119.7 . . ?
C36 C27 H27 119.7 . . ?
C27 C28 C29 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C35 121.3(4) . . ?
C29 C30 H30 119.3 . . ?
C35 C30 H30 119.3 . . ?
C33 C31 C35 120.9(4) . . ?
C33 C31 C37 119.1(4) . . ?
C35 C31 C37 120.0(4) . . ?
C36 C32 C34 120.8(4) . . ?
C36 C32 C38 120.2(4) . . ?
C34 C32 C38 118.9(4) . . ?
C31 C33 C23 122.6(4) . . ?
C31 C33 C34 119.4(4) . . ?
C23 C33 C34 118.0(4) . . ?
C32 C34 C26 122.1(4) . . ?
C32 C34 C33 119.7(4) . . ?
C26 C34 C33 118.2(4) . . ?
C31 C35 C30 122.6(4) . . ?
C31 C35 C36 119.2(4) . . ?
C30 C35 C36 118.1(4) . . ?
C32 C36 C35 119.8(4) . . ?
C32 C36 C27 121.5(4) . . ?
C35 C36 C27 118.7(4) . . ?
O2 C37 O1 125.4(4) . . ?
O2 C37 C31 116.3(4) . . ?
O1 C37 C31 118.3(4) . . ?
O3 C38 O4 125.2(4) . . ?
O3 C38 C32 118.7(4) . . ?
O4 C38 C32 116.1(4) . . ?
C1 N1 N2 111.1(4) . . ?
C1 N1 H1N 129(3) . . ?
N2 N1 H1N 120(4) . . ?
N1 N2 C3 105.8(3) . . ?
N1 N2 Fe1 137.3(3) . . ?
C3 N2 Fe1 115.5(3) . . ?
C4 N3 C8 120.5(3) . . ?
C4 N3 Fe1 120.3(3) . . ?
C8 N3 Fe1 119.2(3) . . ?
N5 N4 C9 105.9(3) . . ?
N5 N4 Fe1 138.2(3) . . ?
C9 N4 Fe1 115.9(3) . . ?
N4 N5 C11 111.1(4) . . ?
N4 N5 H5N 125(3) . . ?
C11 N5 H5N 124(3) . . ?
N7 N6 C12 110.4(4) . . ?
N7 N6 H6N 124(4) . . ?
C12 N6 H6N 124(4) . . ?
N6 N7 C14 106.4(4) . . ?
N6 N7 Fe1 136.6(3) . . ?
C14 N7 Fe1 116.3(3) . . ?
C15 N8 C19 120.2(4) . . ?
C15 N8 Fe1 120.3(3) . . ?
C19 N8 Fe1 119.6(3) . . ?
N10 N9 C20 106.0(3) . . ?
N10 N9 Fe1 138.0(3) . . ?
C20 N9 Fe1 115.6(3) . . ?
N9 N10 C22 111.0(3) . . ?
N9 N10 H10N 125(3) . . ?
C22 N10 H10N 124(3) . . ?
H1W1 O1W H1W2 108(4) . . ?
H2W1 O2W H2W2 103(4) . . ?
H3W1 O3W H3W2 114(4) . . ?
H4W1 O4W H4W2 95(3) . . ?
H5W1 O5W H5W2 93(3) . . ?
H6W1 O6W H6W2 104(4) . . ?
H7W1 O7W H7W2 105(4) . . ?
H8W1 O8W H8W2 99(3) . . ?
H9W1 O9W H9W2 95(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N O2 0.88(2) 1.85(3) 2.675(5) 156(5) 3_567 yes
N5 H5N O1 0.90(2) 1.80(3) 2.696(5) 177(5) 1_655 yes
N6 H6N O1W 0.89(3) 1.95(3) 2.769(5) 152(5) . yes
N10 H10N O4 0.89(2) 1.84(3) 2.728(4) 174(4) . yes
O1W H1W1 O4 0.82(2) 1.86(3) 2.667(5) 167(6) 4_646 yes
O2W H2W1 O3 0.84(3) 2.09(3) 2.921(5) 171(5) . yes
O2W H2W2 O5W 0.81(3) 2.06(3) 2.859(6) 166(6) . yes
O3W H3W1 O1 0.78(2) 2.11(3) 2.884(5) 177(6) 4_546 yes
O3W H3W2 O7W 0.79(2) 1.98(3) 2.721(5) 156(5) . yes
O4W H4W1 O8W 0.91(3) 2.00(4) 2.763(6) 141(6) 2_565 yes
O4W H4W2 O1W 0.88(3) 1.99(3) 2.857(6) 169(7) . yes
O5W H5W1 O3W 0.86(3) 2.00(3) 2.836(6) 164(6) 3_466 yes
O5W H5W2 O8W 0.86(3) 1.95(3) 2.791(6) 165(6) . yes
O6W H6W1 O4W 0.83(3) 2.04(5) 2.803(6) 152(9) 3_467 yes
O6W H6W2 O2 0.82(3) 2.16(6) 2.908(6) 151(10) . yes
O7W H7W1 O4W 0.84(3) 2.01(3) 2.833(7) 167(4) 4_656 yes
O7W H7W2 O3 0.83(3) 1.95(3) 2.728(5) 157(7) . yes
O8W H8W1 O9W 0.85(2) 1.91(3) 2.738(6) 165(6) 2_564 yes
O8W H8W2 O7W 0.87(2) 1.96(3) 2.820(6) 168(5) . yes
O9W H9W1 O6W 0.86(3) 1.96(3) 2.795(7) 163(6) 1_545 yes
O9W H9W2 O2W 0.86(3) 2.13(5) 2.825(6) 137(7) 4_546 yes

_refine_diff_density_max         1.108
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_MRT5cgs9_corr_2
_database_code_depnum_ccdc_archive 'CCDC 2335500'
loop_
_audit_author_name
_audit_author_address
'Carlos Gimenez-Saiz'
;University of Valencia
Spain
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_MRT5cgs9_corr_2     
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O5       - H5O      .       1.13 Ang.
RESPONSE: This corresponds to a short strong hydrogen bond between two carboxylate groups of different trimesic anions. The distance between the heteroatoms, O5 and O1, is 2.499(4).In this type of hydrogen bonds the X-H distance lengthens up to 0.25 Angstrom (see, for example Angew. Chem. Int. Ed. 2002, 41, 48-76). No geometrical restraints were applied to this H atom.
;
_vrf_RINTA01_MRT5cgs9_corr_2     
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The overall quality of the data is poor, probably due to  the crystal quality. There is reasonable confidence that the unit  cell, the crystal system, the Laue group, and the space group are  correct. The non-centrosymmetric space group P21 has been tested but  does not improve the Rint value.
;
_vrf_PLAT020_MRT5cgs9_corr_2     
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.239 Report
RESPONSE: See response to RINTA01.
;
_vrf_PLAT919_MRT5cgs9_corr_2     
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check
RESPONSE: This should not be a problem as we did not perform any solvent modelling refinement in this structure.
;
# Added during the CSD deposition process: Tuesday 27 February 2024 12:15 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10 2+, C9 H4 O6 1-, 5(H2 O)'
_chemical_formula_sum            'C31 H32 Fe N10 O11'
_chemical_formula_weight         776.51

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.1212(2)
_cell_length_b                   31.2063(8)
_cell_length_c                   13.5547(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.059(3)
_cell_angle_gamma                90
_cell_volume                     3416.01(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.00(14)
_cell_measurement_reflns_used    4493
_cell_measurement_theta_min      2.4660
_cell_measurement_theta_max      21.1290

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1961
_exptl_crystal_size_mid          0.0924
_exptl_crystal_size_min          0.0090
_exptl_absorpt_coefficient_mu    0.518
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      120.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
'SuperNova, Single source at offset, Sapphire3'
;
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            82571
_diffrn_reflns_av_unetI/netI     0.2012
_diffrn_reflns_av_R_equivalents  0.2391
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.997
_diffrn_reflns_theta_max         29.919
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_orient_matrix_UB_11      0.0116577000
_diffrn_orient_matrix_UB_12      0.0221660000
_diffrn_orient_matrix_UB_13      0.0100840000
_diffrn_orient_matrix_UB_21      0.0648218000
_diffrn_orient_matrix_UB_22      -0.0049391000
_diffrn_orient_matrix_UB_23      0.0375093000
_diffrn_orient_matrix_UB_31      0.0580821000
_diffrn_orient_matrix_UB_32      0.0010711000
_diffrn_orient_matrix_UB_33      -0.0354979000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00  -11.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575  141.0000   16.0000 77

#__ type_ start__ end____ width___ exp.time_
  2 omega  -81.00   -5.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575  129.0000 -155.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega    5.00   82.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950 -129.0000  130.0000 77

#__ type_ start__ end____ width___ exp.time_
  4 omega   11.00   89.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950 -141.0000  -41.0000 78

#__ type_ start__ end____ width___ exp.time_
  5 omega  -48.00   52.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575   38.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega  -99.00  -35.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575 -178.0000   90.0000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -90.00    1.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575  -57.0000  -90.0000 91

#__ type_ start__ end____ width___ exp.time_
  8 omega  -99.00  -35.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575 -178.0000 -120.0000 64

#__ type_ start__ end____ width___ exp.time_
  9 omega    0.00   91.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950   57.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
 10 omega  -28.00   96.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950   19.0000   90.0000 124

#__ type_ start__ end____ width___ exp.time_
 11 omega  -48.00    3.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9575   38.0000   60.0000 51

#__ type_ start__ end____ width___ exp.time_
 12 omega  -10.00   93.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950   77.0000   30.0000 103

#__ type_ start__ end____ width___ exp.time_
 13 omega   35.00  100.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950  178.0000 -150.0000 65

#__ type_ start__ end____ width___ exp.time_
 14 omega    0.00   91.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       21.8950   57.0000 -120.0000 91

;
_reflns_number_total             9255
_reflns_number_gt                4236
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
;
_computing_data_reduction        
;
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
;
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0747P)²] 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         9255
_refine_ls_number_parameters     528
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1994
_refine_ls_R_factor_gt           0.0750
_refine_ls_wR_factor_ref         0.2055
_refine_ls_wR_factor_gt          0.1474
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.989
_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_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 -0.0034(6) 0.18933(15) 0.6504(3) 0.0312(11) Uani 1 1 d . . . . .
H1 H -0.102479 0.204280 0.628577 0.037 Uiso 1 1 calc R U . . .
C2 C 0.0426(5) 0.17493(14) 0.7457(3) 0.0290(11) Uani 1 1 d . . . . .
H2 H -0.016261 0.177852 0.802330 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1956(5) 0.15508(13) 0.7399(3) 0.0222(9) Uani 1 1 d . . . . .
C4 C 0.3164(5) 0.13268(13) 0.8099(3) 0.0224(9) Uani 1 1 d . . . . .
C5 C 0.3003(6) 0.12306(14) 0.9087(3) 0.0311(11) Uani 1 1 d . . . . .
H5 H 0.205237 0.131563 0.939049 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4292(6) 0.10044(14) 0.9616(3) 0.0302(11) Uani 1 1 d . . . . .
H6 H 0.422269 0.093379 1.029236 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5675(5) 0.08816(13) 0.9162(3) 0.0259(10) Uani 1 1 d . . . . .
H7 H 0.655150 0.072574 0.951740 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5740(5) 0.09936(13) 0.8170(3) 0.0243(10) Uani 1 1 d . . . . .
C9 C 0.7040(5) 0.08956(13) 0.7544(3) 0.0249(10) Uani 1 1 d . . . . .
C10 C 0.8544(6) 0.06739(14) 0.7672(4) 0.0337(12) Uani 1 1 d . . . . .
H10 H 0.905052 0.054117 0.825816 0.040 Uiso 1 1 calc R U . . .
C11 C 0.9124(6) 0.06927(15) 0.6747(4) 0.0343(12) Uani 1 1 d . . . . .
H11 H 1.012302 0.056840 0.657481 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6681(5) 0.25627(14) 0.6581(3) 0.0261(10) Uani 1 1 d . . . . .
H12 H 0.714439 0.280726 0.692344 0.031 Uiso 1 1 calc R U . . .
C13 C 0.6411(5) 0.25153(14) 0.5573(3) 0.0276(10) Uani 1 1 d . . . . .
H13 H 0.665107 0.271592 0.508132 0.033 Uiso 1 1 calc R U . . .
C14 C 0.5701(5) 0.21059(14) 0.5421(3) 0.0233(10) Uani 1 1 d . . . . .
C15 C 0.5145(5) 0.18409(14) 0.4568(3) 0.0237(10) Uani 1 1 d . . . . .
C16 C 0.5170(5) 0.19376(15) 0.3576(3) 0.0276(10) Uani 1 1 d . . . . .
H16 H 0.554742 0.220933 0.337784 0.033 Uiso 1 1 calc R U . . .
C17 C 0.4634(6) 0.16307(15) 0.2872(3) 0.0303(11) Uani 1 1 d . . . . .
H17 H 0.466238 0.168992 0.218645 0.036 Uiso 1 1 calc R U . . .
C18 C 0.4056(6) 0.12363(15) 0.3171(3) 0.0317(11) Uani 1 1 d . . . . .
H18 H 0.367277 0.102451 0.269793 0.038 Uiso 1 1 calc R U . . .
C19 C 0.4057(5) 0.11621(14) 0.4181(3) 0.0249(10) Uani 1 1 d . . . . .
C20 C 0.3539(5) 0.07730(14) 0.4656(3) 0.0270(10) Uani 1 1 d . . . . .
C21 C 0.2939(6) 0.03738(14) 0.4333(4) 0.0333(11) Uani 1 1 d . . . . .
H21 H 0.271673 0.027685 0.366780 0.040 Uiso 1 1 calc R U . . .
C22 C 0.2739(6) 0.01500(15) 0.5186(4) 0.0346(12) Uani 1 1 d . . . . .
H22 H 0.235593 -0.013667 0.522086 0.042 Uiso 1 1 calc R U . . .
C23 C 0.9312(5) 0.20544(14) 0.3345(3) 0.0252(10) Uani 1 1 d . . . . .
C24 C 0.8923(5) 0.18550(13) 0.2341(3) 0.0224(10) Uani 1 1 d . . . . .
C25 C 0.9688(5) 0.14681(13) 0.2154(3) 0.0230(10) Uani 1 1 d . . . . .
H25 H 1.035478 0.132892 0.267610 0.028 Uiso 1 1 calc R U . . .
C26 C 0.9494(5) 0.12821(13) 0.1219(3) 0.0206(9) Uani 1 1 d . . . . .
C27 C 1.0269(6) 0.08533(14) 0.1052(3) 0.0272(10) Uani 1 1 d . . . . .
C28 C 0.8518(5) 0.14863(13) 0.0462(3) 0.0233(10) Uani 1 1 d . . . . .
H28 H 0.841767 0.136747 -0.018647 0.028 Uiso 1 1 calc R U . . .
C29 C 0.7684(5) 0.18623(13) 0.0638(3) 0.0211(9) Uani 1 1 d . . . . .
C30 C 0.6602(6) 0.20512(14) -0.0209(3) 0.0263(10) Uani 1 1 d . . . . .
C31 C 0.7869(5) 0.20447(14) 0.1585(3) 0.0229(10) Uani 1 1 d . . . . .
H31 H 0.727829 0.229776 0.171448 0.028 Uiso 1 1 calc R U . . .
Fe1 Fe 0.45892(8) 0.13330(2) 0.62594(4) 0.02219(18) Uani 1 1 d . . . . .
N1 N 0.1169(5) 0.17844(11) 0.5939(3) 0.0247(8) Uani 1 1 d D . . . .
H1N H 0.105(7) 0.1855(17) 0.5292(18) 0.07(2) Uiso 1 1 d D . . . .
N2 N 0.2398(4) 0.15709(11) 0.6463(2) 0.0232(8) Uani 1 1 d . . . . .
N3 N 0.4496(4) 0.12087(11) 0.7650(3) 0.0245(8) Uani 1 1 d . . . . .
N4 N 0.6746(4) 0.10464(11) 0.6605(3) 0.0247(8) Uani 1 1 d . . . . .
N5 N 0.8038(5) 0.09157(12) 0.6137(3) 0.0297(9) Uani 1 1 d D . . . .
H5N H 0.816(6) 0.1008(15) 0.552(2) 0.052(17) Uiso 1 1 d D . . . .
N6 N 0.6169(5) 0.21974(12) 0.7006(3) 0.0262(9) Uani 1 1 d D . . . .
H6N H 0.631(6) 0.2160(15) 0.7664(15) 0.046(16) Uiso 1 1 d D . . . .
N7 N 0.5557(4) 0.19157(11) 0.6310(2) 0.0237(8) Uani 1 1 d . . . . .
N8 N 0.4595(4) 0.14579(11) 0.4861(3) 0.0233(8) Uani 1 1 d . . . . .
N9 N 0.3675(4) 0.07943(11) 0.5659(3) 0.0253(8) Uani 1 1 d . . . . .
N10 N 0.3185(5) 0.04104(12) 0.5968(3) 0.0284(9) Uani 1 1 d D . . . .
H10N H 0.312(5) 0.0349(13) 0.6613(16) 0.025(12) Uiso 1 1 d D . . . .
O1 O 0.8796(4) 0.24299(9) 0.3482(2) 0.0277(7) Uani 1 1 d . . . . .
O2 O 1.0168(4) 0.18383(10) 0.3989(2) 0.0398(9) Uani 1 1 d . . . . .
O3 O 1.1142(4) 0.06827(10) 0.1770(2) 0.0336(8) Uani 1 1 d . . . . .
O4 O 0.9964(4) 0.06887(9) 0.0207(2) 0.0320(8) Uani 1 1 d . . . . .
O5 O 0.5339(4) 0.22692(10) 0.0019(2) 0.0290(7) Uani 1 1 d . . . . .
H5O H 0.463(8) 0.2404(19) -0.067(5) 0.09(2) Uiso 1 1 d . . . . .
O6 O 0.6938(4) 0.19865(10) -0.1067(2) 0.0354(8) Uani 1 1 d . . . . .
O1W O 0.6630(4) -0.00942(12) 0.2174(2) 0.0358(8) Uani 1 1 d D . . . .
H1W1 H 0.712(5) -0.0113(17) 0.169(3) 0.054 Uiso 1 1 d D U . . .
H1W2 H 0.568(3) -0.0015(17) 0.199(3) 0.054 Uiso 1 1 d D U . . .
O2W O 0.8144(4) -0.00706(10) 0.0497(3) 0.0358(8) Uani 1 1 d D . . . .
H2W1 H 0.871(4) -0.0268(9) 0.031(3) 0.054 Uiso 1 1 d D U . . .
H2W2 H 0.876(5) 0.0137(9) 0.051(4) 0.054 Uiso 1 1 d D U . . .
O3W O 0.8267(5) 0.11093(12) 0.4263(3) 0.0474(10) Uani 1 1 d D . . . .
H3W1 H 0.840(7) 0.0916(12) 0.386(3) 0.071 Uiso 1 1 d D U . . .
H3W2 H 0.889(6) 0.1302(12) 0.412(4) 0.071 Uiso 1 1 d D U . . .
O4W O 0.9010(5) 0.04303(12) 0.3175(3) 0.0457(10) Uani 1 1 d D . . . .
H4W1 H 0.820(4) 0.0316(17) 0.284(3) 0.069 Uiso 1 1 d D U . . .
H4W2 H 0.960(5) 0.0505(17) 0.274(3) 0.069 Uiso 1 1 d D U . . .
O5W O 0.3749(5) 0.02001(14) 0.1360(3) 0.0500(10) Uani 1 1 d D . . . .
H5W1 H 0.295(5) 0.0339(16) 0.154(3) 0.075 Uiso 1 1 d D U . . .
H5W2 H 0.339(6) 0.0125(17) 0.080(2) 0.075 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 N1 1.347(5) . ?
C1 C2 1.382(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.398(6) . ?
C2 H2 0.9500 . ?
C3 N2 1.356(5) . ?
C3 C4 1.468(6) . ?
C4 N3 1.347(5) . ?
C4 C5 1.392(6) . ?
C5 C6 1.396(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(6) . ?
C7 H7 0.9500 . ?
C8 N3 1.349(5) . ?
C8 C9 1.455(6) . ?
C9 N4 1.353(5) . ?
C9 C10 1.398(6) . ?
C10 C11 1.387(6) . ?
C10 H10 0.9500 . ?
C11 N5 1.339(6) . ?
C11 H11 0.9500 . ?
C12 N6 1.362(5) . ?
C12 C13 1.368(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.408(6) . ?
C13 H13 0.9500 . ?
C14 N7 1.360(5) . ?
C14 C15 1.453(6) . ?
C15 N8 1.350(5) . ?
C15 C16 1.381(6) . ?
C16 C17 1.389(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(6) . ?
C18 H18 0.9500 . ?
C19 N8 1.344(5) . ?
C19 C20 1.457(6) . ?
C20 N9 1.354(5) . ?
C20 C21 1.391(6) . ?
C21 C22 1.375(6) . ?
C21 H21 0.9500 . ?
C22 N10 1.354(6) . ?
C22 H22 0.9500 . ?
C23 O2 1.254(5) . ?
C23 O1 1.265(5) . ?
C23 C24 1.499(6) . ?
C24 C25 1.393(6) . ?
C24 C31 1.396(6) . ?
C25 C26 1.387(5) . ?
C25 H25 0.9500 . ?
C26 C28 1.384(6) . ?
C26 C27 1.506(6) . ?
C27 O4 1.256(5) . ?
C27 O3 1.260(5) . ?
C28 C29 1.388(6) . ?
C28 H28 0.9500 . ?
C29 C31 1.399(6) . ?
C29 C30 1.490(6) . ?
C30 O6 1.240(5) . ?
C30 O5 1.295(5) . ?
C31 H31 0.9500 . ?
Fe1 N3 1.934(3) . ?
Fe1 N8 1.936(4) . ?
Fe1 N2 1.974(3) . ?
Fe1 N9 1.978(4) . ?
Fe1 N4 1.978(4) . ?
Fe1 N7 1.979(4) . ?
N1 N2 1.340(5) . ?
N1 H1N 0.901(19) . ?
N4 N5 1.346(5) . ?
N5 H5N 0.901(19) . ?
N6 N7 1.346(5) . ?
N6 H6N 0.895(19) . ?
N9 N10 1.343(5) . ?
N10 H10N 0.901(18) . ?
O5 H5O 1.12(7) . ?
O1W H1W1 0.802(18) . ?
O1W H1W2 0.824(19) . ?
O2W H2W1 0.825(18) . ?
O2W H2W2 0.818(18) . ?
O3W H3W1 0.832(19) . ?
O3W H3W2 0.823(19) . ?
O4W H4W1 0.838(19) . ?
O4W H4W2 0.832(19) . ?
O5W H5W1 0.839(19) . ?
O5W H5W2 0.821(18) . ?

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
N1 C1 C2 108.0(4) . . ?
N1 C1 H1 126.0 . . ?
C2 C1 H1 126.0 . . ?
C1 C2 C3 104.2(4) . . ?
C1 C2 H2 127.9 . . ?
C3 C2 H2 127.9 . . ?
N2 C3 C2 111.0(4) . . ?
N2 C3 C4 113.7(4) . . ?
C2 C3 C4 135.4(4) . . ?
N3 C4 C5 122.5(4) . . ?
N3 C4 C3 110.6(4) . . ?
C5 C4 C3 126.9(4) . . ?
C4 C5 C6 117.5(4) . . ?
C4 C5 H5 121.2 . . ?
C6 C5 H5 121.2 . . ?
C7 C6 C5 120.6(4) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 118.2(4) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
N3 C8 C7 121.7(4) . . ?
N3 C8 C9 110.5(4) . . ?
C7 C8 C9 127.8(4) . . ?
N4 C9 C10 110.8(4) . . ?
N4 C9 C8 114.1(4) . . ?
C10 C9 C8 135.1(4) . . ?
C11 C10 C9 104.0(4) . . ?
C11 C10 H10 128.0 . . ?
C9 C10 H10 128.0 . . ?
N5 C11 C10 108.4(4) . . ?
N5 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
N6 C12 C13 107.9(4) . . ?
N6 C12 H12 126.0 . . ?
C13 C12 H12 126.0 . . ?
C12 C13 C14 105.4(4) . . ?
C12 C13 H13 127.3 . . ?
C14 C13 H13 127.3 . . ?
N7 C14 C13 109.8(4) . . ?
N7 C14 C15 114.1(4) . . ?
C13 C14 C15 136.2(4) . . ?
N8 C15 C16 121.2(4) . . ?
N8 C15 C14 110.8(4) . . ?
C16 C15 C14 127.9(4) . . ?
C15 C16 C17 118.9(4) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
C16 C17 C18 120.0(4) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 118.0(4) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
N8 C19 C18 121.8(4) . . ?
N8 C19 C20 111.0(4) . . ?
C18 C19 C20 127.2(4) . . ?
N9 C20 C21 110.4(4) . . ?
N9 C20 C19 113.9(4) . . ?
C21 C20 C19 135.7(4) . . ?
C22 C21 C20 105.0(4) . . ?
C22 C21 H21 127.5 . . ?
C20 C21 H21 127.5 . . ?
N10 C22 C21 107.9(4) . . ?
N10 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
O2 C23 O1 124.3(4) . . ?
O2 C23 C24 117.2(4) . . ?
O1 C23 C24 118.5(4) . . ?
C25 C24 C31 119.0(4) . . ?
C25 C24 C23 118.0(4) . . ?
C31 C24 C23 123.0(4) . . ?
C26 C25 C24 121.3(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C28 C26 C25 119.0(4) . . ?
C28 C26 C27 120.9(4) . . ?
C25 C26 C27 120.0(4) . . ?
O4 C27 O3 124.9(4) . . ?
O4 C27 C26 117.1(4) . . ?
O3 C27 C26 118.0(4) . . ?
C26 C28 C29 121.0(4) . . ?
C26 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C28 C29 C31 119.6(4) . . ?
C28 C29 C30 117.5(4) . . ?
C31 C29 C30 122.9(4) . . ?
O6 C30 O5 124.6(4) . . ?
O6 C30 C29 119.2(4) . . ?
O5 C30 C29 116.2(4) . . ?
C24 C31 C29 120.0(4) . . ?
C24 C31 H31 120.0 . . ?
C29 C31 H31 120.0 . . ?
N3 Fe1 N8 177.89(15) . . ?
N3 Fe1 N2 79.07(14) . . ?
N8 Fe1 N2 99.01(14) . . ?
N3 Fe1 N9 100.30(15) . . ?
N8 Fe1 N9 78.91(15) . . ?
N2 Fe1 N9 94.15(14) . . ?
N3 Fe1 N4 78.64(14) . . ?
N8 Fe1 N4 103.28(14) . . ?
N2 Fe1 N4 157.71(14) . . ?
N9 Fe1 N4 89.88(15) . . ?
N3 Fe1 N7 101.94(14) . . ?
N8 Fe1 N7 78.88(14) . . ?
N2 Fe1 N7 90.58(14) . . ?
N9 Fe1 N7 157.75(14) . . ?
N4 Fe1 N7 93.94(14) . . ?
N2 N1 C1 111.7(4) . . ?
N2 N1 H1N 130(4) . . ?
C1 N1 H1N 119(4) . . ?
N1 N2 C3 105.2(3) . . ?
N1 N2 Fe1 138.2(3) . . ?
C3 N2 Fe1 116.5(3) . . ?
C4 N3 C8 119.5(4) . . ?
C4 N3 Fe1 120.1(3) . . ?
C8 N3 Fe1 120.3(3) . . ?
N5 N4 C9 105.6(4) . . ?
N5 N4 Fe1 137.7(3) . . ?
C9 N4 Fe1 116.4(3) . . ?
C11 N5 N4 111.2(4) . . ?
C11 N5 H5N 128(3) . . ?
N4 N5 H5N 121(3) . . ?
N7 N6 C12 110.9(4) . . ?
N7 N6 H6N 128(3) . . ?
C12 N6 H6N 121(3) . . ?
N6 N7 C14 106.0(3) . . ?
N6 N7 Fe1 137.8(3) . . ?
C14 N7 Fe1 116.2(3) . . ?
C19 N8 C15 120.0(4) . . ?
C19 N8 Fe1 119.9(3) . . ?
C15 N8 Fe1 120.0(3) . . ?
N10 N9 C20 105.9(4) . . ?
N10 N9 Fe1 137.8(3) . . ?
C20 N9 Fe1 116.3(3) . . ?
N9 N10 C22 110.8(4) . . ?
N9 N10 H10N 123(3) . . ?
C22 N10 H10N 127(3) . . ?
C30 O5 H5O 110(3) . . ?
H1W1 O1W H1W2 108(3) . . ?
H2W1 O2W H2W2 104(3) . . ?
H3W1 O3W H3W2 104(3) . . ?
H4W1 O4W H4W2 103(3) . . ?
H5W1 O5W H5W2 102(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N O2 0.901(19) 1.83(3) 2.688(5) 157(5) 1_455 yes
N5 H5N O3W 0.901(19) 1.74(2) 2.637(5) 171(5) . yes
N6 H6N O6 0.895(19) 1.82(2) 2.702(5) 166(5) 1_556 yes
N10 H10N O1W 0.901(18) 1.82(2) 2.694(5) 163(4) 3_656 yes
O5 H5O O1 1.12(7) 1.38(7) 2.499(4) 179(6) 4_565 yes
O1W H1W1 O2W 0.802(18) 1.90(2) 2.697(4) 171(5) . yes
O1W H1W2 O5W 0.824(19) 1.83(2) 2.644(5) 169(5) . yes
O2W H2W1 O4 0.825(18) 1.88(2) 2.702(4) 176(4) 3_755 yes
O2W H2W2 O4 0.818(18) 2.04(2) 2.842(4) 166(6) . yes
O3W H3W1 O4W 0.832(19) 1.87(2) 2.686(5) 167(6) . yes
O3W H3W2 O2 0.823(19) 1.987(19) 2.796(5) 168(5) . yes
O4W H4W1 O1W 0.838(19) 1.96(2) 2.775(5) 164(6) . yes
O4W H4W2 O3 0.832(19) 1.987(19) 2.818(5) 177(5) . yes
O5W H5W1 O3 0.839(19) 1.87(2) 2.703(5) 172(5) 1_455 yes
O5W H5W2 O2W 0.821(18) 2.05(2) 2.836(5) 160(4) 3_655 yes

_refine_diff_density_max         0.599
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_MRT14c-6
_database_code_depnum_ccdc_archive 'CCDC 2335503'
loop_
_audit_author_name
_audit_author_address
'Carlos Gimenez-Saiz'
;University of Valencia
Spain
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_MRT14c-6            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 16 Note 
RESPONSE: Probably caused by the beamstop. This should not be a problem as 
we did not perform any solvent modelling refinement in this structure.
;
_vrf_PLAT242_MRT14c-6            
;
PROBLEM: Low ?MainMol? Ueq as Compared to Neighbors of C30 Check 
RESPONSE: C30 is bonded to O3, which has a large U(eq) (both belonging to a 
carboxylate group). O3 is forming a hydrogen bond with a water molecule (O6W) 
with a refined occupancy close to 0.5, possibly due to a partial dehydration 
of the crystal during the preparation of the sample. Such partial dehydration 
could cause the high U(eq) in O3 and, therefore, the alert.  
;
_vrf_PLAT250_MRT14c-6            
;
PROBLEM: Large U3/U1 Ratio for <U(i,j)> Tensor(Resd 3) 2.5 Note 
RESPONSE: See response to PLAT242. This alert probably arises for the same 
reason.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Fe N10 2+, C14 H8 O4 2-, 5(H2 O)'
_chemical_formula_sum            'C36 H36 Fe N10 O9'
_chemical_formula_weight         808.60

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   28.8805(5)
_cell_length_b                   15.3810(2)
_cell_length_c                   8.49297(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3772.67(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.00(10)
_cell_measurement_reflns_used    18200
_cell_measurement_theta_min      3.4420
_cell_measurement_theta_max      24.9870

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3441
_exptl_crystal_size_mid          0.1026
_exptl_crystal_size_min          0.0199
_exptl_absorpt_coefficient_mu    0.468
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
;
'SuperNova, Single source at offset, Sapphire3'
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            91426
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.391
_diffrn_reflns_theta_max         29.761
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0239881000
_diffrn_orient_matrix_UB_12      -0.0074385000
_diffrn_orient_matrix_UB_13      -0.0117143000
_diffrn_orient_matrix_UB_21      0.0026702000
_diffrn_orient_matrix_UB_22      -0.0087242000
_diffrn_orient_matrix_UB_23      0.0815186000
_diffrn_orient_matrix_UB_31      -0.0045175000
_diffrn_orient_matrix_UB_32      -0.0446681000
_diffrn_orient_matrix_UB_33      -0.0139601000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00  48.00   1.00   22.50    --  -22.59  57.00 -30.00   94
  2  ω    -93.00   1.00   1.00   22.50    --  -22.59 -57.00-180.00   94
  3  ω    -75.00   8.00   1.00   22.50    --  -22.59 113.00  52.00   83
  4  ω   -102.00 -35.00   1.00   22.50    --  -22.59-178.00  60.00   67
  5  ω   -102.00 -35.00   1.00   22.50    --  -22.59-178.00 -90.00   67
  6  ω    -46.00  48.00   1.00   22.50    --  -22.59  57.00 -60.00   94
  7  ω     -8.00  76.00   1.00   22.50    --   23.52-113.00 -39.00   84
  8  ω    -43.00  99.00   1.00   22.50    --   23.52  19.00   0.00  142
  9  ω    -93.00   1.00   1.00   22.50    --  -22.59 -57.00  30.00   94
 10  ω    -95.00 -70.00   1.00   22.50    --  -22.59 -77.00 120.00   25
 11  ω   -102.00 -35.00   1.00   22.50    --  -22.59-178.00 120.00   67
 12  ω    -95.00  10.00   1.00   22.50    --  -22.59 -77.00  90.00  105
 13  ω    -10.00  96.00   1.00   22.50    --   23.52  77.00   0.00  106
 14  ω      0.00  94.00   1.00   22.50    --   23.52  57.00 -90.00   94
;
_reflns_number_total             10240
_reflns_number_gt                8885
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_max     0.925
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+2.2793P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.083(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10240
_refine_ls_number_parameters     560
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1061
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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_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 0.81422(15) 0.2770(2) 0.2426(5) 0.0302(9) Uani 1 1 d . . . . .
H1 H 0.808197 0.298637 0.139837 0.036 Uiso 1 1 calc R U . . .
C2 C 0.85617(14) 0.2775(2) 0.3175(5) 0.0278(8) Uani 1 1 d . . . . .
H2 H 0.884830 0.298510 0.278033 0.033 Uiso 1 1 calc R U . . .
C3 C 0.84765(13) 0.2403(2) 0.4648(4) 0.0208(7) Uani 1 1 d . . . . .
C4 C 0.87819(13) 0.2202(2) 0.5972(4) 0.0190(7) Uani 1 1 d . . . . .
C5 C 0.92582(13) 0.2344(2) 0.6003(5) 0.0241(8) Uani 1 1 d . . . . .
H5 H 0.941125 0.260918 0.513677 0.029 Uiso 1 1 calc R U . . .
C6 C 0.95024(13) 0.2090(2) 0.7324(5) 0.0245(8) Uani 1 1 d . . . . .
H6 H 0.982791 0.217584 0.736136 0.029 Uiso 1 1 calc R U . . .
C7 C 0.92790(13) 0.1711(2) 0.8593(5) 0.0223(8) Uani 1 1 d . . . . .
H7 H 0.944506 0.154016 0.950818 0.027 Uiso 1 1 calc R U . . .
C8 C 0.88001(12) 0.1589(2) 0.8480(4) 0.0183(7) Uani 1 1 d . . . . .
C9 C 0.85143(12) 0.1158(2) 0.9678(4) 0.0185(7) Uani 1 1 d . . . . .
C10 C 0.86220(14) 0.0804(3) 1.1145(5) 0.0247(8) Uani 1 1 d . . . . .
H10 H 0.891599 0.077458 1.164356 0.030 Uiso 1 1 calc R U . . .
C11 C 0.81990(14) 0.0503(2) 1.1706(4) 0.0259(8) Uani 1 1 d . . . . .
H11 H 0.814633 0.023102 1.269450 0.031 Uiso 1 1 calc R U . . .
C12 C 0.82868(15) -0.0993(2) 0.4927(5) 0.0294(9) Uani 1 1 d . . . . .
H12 H 0.849663 -0.143130 0.459342 0.035 Uiso 1 1 calc R U . . .
C13 C 0.78150(15) -0.1028(2) 0.4832(4) 0.0277(8) Uani 1 1 d . . . . .
H13 H 0.763101 -0.148999 0.443255 0.033 Uiso 1 1 calc R U . . .
C14 C 0.76610(14) -0.0234(2) 0.5453(4) 0.0225(8) Uani 1 1 d . . . . .
C15 C 0.72020(14) 0.0121(2) 0.5733(4) 0.0229(8) Uani 1 1 d . . . . .
C16 C 0.67865(16) -0.0277(3) 0.5302(5) 0.0320(10) Uani 1 1 d . . . . .
H16 H 0.678459 -0.080438 0.471964 0.038 Uiso 1 1 calc R U . . .
C17 C 0.63802(15) 0.0118(3) 0.5749(6) 0.0371(11) Uani 1 1 d . . . . .
H17 H 0.609332 -0.014337 0.547438 0.045 Uiso 1 1 calc R U . . .
C18 C 0.63804(14) 0.0888(3) 0.6591(5) 0.0300(9) Uani 1 1 d . . . . .
H18 H 0.609931 0.115276 0.691914 0.036 Uiso 1 1 calc R U . . .
C19 C 0.68099(12) 0.1264(2) 0.6940(4) 0.0209(7) Uani 1 1 d . . . . .
C20 C 0.68758(12) 0.2083(2) 0.7788(4) 0.0200(7) Uani 1 1 d . . . . .
C21 C 0.65709(14) 0.2642(2) 0.8547(5) 0.0252(8) Uani 1 1 d . . . . .
H21 H 0.624374 0.259012 0.861751 0.030 Uiso 1 1 calc R U . . .
C22 C 0.68438(14) 0.3284(2) 0.9172(5) 0.0252(8) Uani 1 1 d . . . . .
H22 H 0.673907 0.376732 0.977033 0.030 Uiso 1 1 calc R U . . .
C23 C 0.67524(13) 0.9728(2) 0.0923(5) 0.0230(8) Uani 1 1 d . . . . .
C24 C 0.62296(12) 0.9816(2) 0.0936(5) 0.0216(7) Uani 1 1 d . . . . .
C25 C 0.60196(13) 1.0614(2) 0.0674(4) 0.0224(8) Uani 1 1 d . . . . .
H25 H 0.620555 1.111525 0.050973 0.027 Uiso 1 1 calc R U . . .
C26 C 0.55398(13) 1.0688(2) 0.0650(4) 0.0210(8) Uani 1 1 d . . . . .
H26 H 0.540226 1.123727 0.044383 0.025 Uiso 1 1 calc R U . . .
C27 C 0.52563(12) 0.9966(2) 0.0923(4) 0.0188(7) Uani 1 1 d . . . . .
C28 C 0.54740(13) 0.9169(2) 0.1226(4) 0.0226(8) Uani 1 1 d . . . . .
H28 H 0.529056 0.867059 0.144693 0.027 Uiso 1 1 calc R U . . .
C29 C 0.59529(13) 0.9094(2) 0.1208(5) 0.0242(8) Uani 1 1 d . . . . .
H29 H 0.609261 0.854354 0.138337 0.029 Uiso 1 1 calc R U . . .
C30 C 0.95818(18) 0.8191(3) 0.4083(5) 0.0360(10) Uani 1 1 d . . . . .
C31 C 0.97048(14) 0.7240(2) 0.4052(5) 0.0247(8) Uani 1 1 d . . . . .
C32 C 0.99420(16) 0.6877(3) 0.2781(5) 0.0323(9) Uani 1 1 d . . . . .
H32 H 1.002477 0.723250 0.191103 0.039 Uiso 1 1 calc R U . . .
C33 C 1.00581(14) 0.6003(2) 0.2776(5) 0.0293(9) Uani 1 1 d . . . . .
H33 H 1.021998 0.576623 0.190195 0.035 Uiso 1 1 calc R U . . .
C34 C 0.99411(14) 0.5472(2) 0.4029(5) 0.0243(8) Uani 1 1 d . . . . .
C35 C 0.97104(13) 0.5836(2) 0.5301(5) 0.0243(8) Uani 1 1 d . . . . .
H35 H 0.963208 0.548146 0.617743 0.029 Uiso 1 1 calc R U . . .
C36 C 0.95922(14) 0.6712(2) 0.5310(5) 0.0253(8) Uani 1 1 d . . . . .
H36 H 0.943277 0.694952 0.618932 0.030 Uiso 1 1 calc R U . . .
Fe1 Fe 0.78494(2) 0.15014(3) 0.70244(6) 0.01697(11) Uani 1 1 d . . . . .
N1 N 0.78302(13) 0.2405(2) 0.3399(3) 0.0248(7) Uani 1 1 d D . . . .
H1N H 0.7539(10) 0.226(3) 0.327(6) 0.047(15) Uiso 1 1 d D . . . .
N2 N 0.80269(11) 0.21744(19) 0.4784(4) 0.0204(6) Uani 1 1 d . . . . .
N3 N 0.85623(10) 0.18359(17) 0.7202(4) 0.0172(6) Uani 1 1 d . . . . .
N4 N 0.80618(10) 0.10737(18) 0.9351(4) 0.0185(6) Uani 1 1 d . . . . .
N5 N 0.78796(12) 0.06662(19) 1.0604(4) 0.0218(6) Uani 1 1 d D . . . .
H5N H 0.7585(11) 0.051(4) 1.072(8) 0.09(2) Uiso 1 1 d D . . . .
N6 N 0.83999(12) -0.0227(2) 0.5574(4) 0.0265(7) Uani 1 1 d D . . . .
H6N H 0.8669(10) -0.002(3) 0.574(6) 0.045(15) Uiso 1 1 d D . . . .
N7 N 0.80238(11) 0.02508(19) 0.5909(4) 0.0216(6) Uani 1 1 d . . . . .
N8 N 0.72065(11) 0.08822(18) 0.6516(3) 0.0202(6) Uani 1 1 d . . . . .
N9 N 0.73171(10) 0.23752(18) 0.7923(4) 0.0193(6) Uani 1 1 d . . . . .
N10 N 0.72855(11) 0.3110(2) 0.8789(4) 0.0217(7) Uani 1 1 d D . . . .
H10N H 0.7521(12) 0.346(3) 0.895(5) 0.038(13) Uiso 1 1 d D . . . .
O1 O 0.69803(9) 1.04277(17) 0.0921(4) 0.0319(7) Uani 1 1 d . . . . .
O2 O 0.69167(9) 0.89784(17) 0.0910(4) 0.0306(6) Uani 1 1 d . . . . .
O3 O 0.9676(2) 0.8647(2) 0.2931(5) 0.111(2) Uani 1 1 d . . . . .
O4 O 0.93898(11) 0.8485(2) 0.5268(4) 0.0401(7) Uani 1 1 d . . . . .
O1W O 0.69417(11) 0.1957(2) 0.2750(4) 0.0432(8) Uani 1 1 d D . . . .
H1W1 H 0.6907(18) 0.153(2) 0.222(6) 0.065 Uiso 1 1 d D U . . .
H1W2 H 0.6693(13) 0.223(3) 0.269(7) 0.065 Uiso 1 1 d D U . . .
O2W O 0.61471(12) 0.2968(2) 0.2183(5) 0.0494(9) Uani 1 1 d D . . . .
H2W1 H 0.5997(18) 0.309(4) 0.302(4) 0.074 Uiso 1 1 d D U . . .
H2W2 H 0.5937(16) 0.307(4) 0.150(5) 0.074 Uiso 1 1 d D U . . .
O3W O 1.06627(13) -0.0162(2) 0.5823(6) 0.0637(13) Uani 1 1 d D . . . .
H3W1 H 1.0601(14) 0.0361(18) 0.563(7) 0.096 Uiso 1 1 d D U . . .
H3W2 H 1.063(3) -0.041(4) 0.494(5) 0.096 Uiso 1 1 d D U . . .
O4W O 0.95973(14) 0.8447(3) 0.9741(4) 0.0576(10) Uani 1 1 d D . . . .
H4W1 H 0.957(2) 0.855(4) 1.070(3) 0.086 Uiso 1 1 d D U . . .
H4W2 H 0.959(2) 0.897(2) 0.935(7) 0.086 Uiso 1 1 d D U . . .
O5W O 1.000000 0.000000 0.8276(6) 0.0467(12) Uani 1 2 d DS T P . .
H5W1 H 1.0218(7) -0.010(4) 0.763(4) 0.070 Uiso 1 1 d D U . . .
O6W O 1.0429(2) -0.0489(4) 0.2972(10) 0.0491(19) Uani 0.5 1 d D . P . .
H6W1 H 1.023(3) -0.086(5) 0.298(16) 0.074 Uiso 0.5 1 d D U P . .
H6W2 H 1.031(3) -0.006(4) 0.263(15) 0.074 Uiso 0.5 1 d D U P . .


_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 N1 1.345(5) . ?
C1 C2 1.368(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.397(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.350(5) . ?
C3 C4 1.462(5) . ?
C4 N3 1.346(4) . ?
C4 C5 1.393(5) . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(5) . ?
C7 H7 0.9500 . ?
C8 N3 1.339(4) . ?
C8 C9 1.467(5) . ?
C9 N4 1.342(4) . ?
C9 C10 1.395(5) . ?
C10 C11 1.391(6) . ?
C10 H10 0.9500 . ?
C11 N5 1.338(5) . ?
C11 H11 0.9500 . ?
C12 N6 1.340(5) . ?
C12 C13 1.366(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(5) . ?
C13 H13 0.9500 . ?
C14 N7 1.343(5) . ?
C14 C15 1.453(6) . ?
C15 N8 1.346(5) . ?
C15 C16 1.396(5) . ?
C16 C17 1.375(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.400(5) . ?
C18 H18 0.9500 . ?
C19 N8 1.336(5) . ?
C19 C20 1.464(5) . ?
C20 N9 1.356(4) . ?
C20 C21 1.389(5) . ?
C21 C22 1.371(5) . ?
C21 H21 0.9500 . ?
C22 N10 1.344(5) . ?
C22 H22 0.9500 . ?
C23 O2 1.246(4) . ?
C23 O1 1.262(5) . ?
C23 C24 1.516(5) . ?
C24 C29 1.387(5) . ?
C24 C25 1.387(5) . ?
C25 C26 1.391(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.401(5) . ?
C27 C27 1.484(7) 2_675 ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 O3 1.234(6) . ?
C30 O4 1.235(5) . ?
C30 C31 1.506(6) . ?
C31 C36 1.381(5) . ?
C31 C32 1.395(6) . ?
C32 C33 1.385(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(5) . ?
C34 C34 1.492(7) 2_765 ?
C35 C36 1.390(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
Fe1 N3 2.128(3) . ?
Fe1 N8 2.131(3) . ?
Fe1 N4 2.171(3) . ?
Fe1 N9 2.180(3) . ?
Fe1 N7 2.203(3) . ?
Fe1 N2 2.226(3) . ?
N1 N2 1.354(4) . ?
N1 H1N 0.87(2) . ?
N4 N5 1.342(4) . ?
N5 H5N 0.89(3) . ?
N6 N7 1.342(4) . ?
N6 H6N 0.85(2) . ?
N9 N10 1.351(4) . ?
N10 H10N 0.88(2) . ?
O1W H1W1 0.81(2) . ?
O1W H1W2 0.83(2) . ?
O2W H2W1 0.85(2) . ?
O2W H2W2 0.86(2) . ?
O3W H3W1 0.84(2) . ?
O3W H3W2 0.84(3) . ?
O4W H4W1 0.83(3) . ?
O4W H4W2 0.87(2) . ?
O5W H5W1 0.85(2) . ?
O5W H5W1 0.85(2) 2_755 ?
O6W H6W1 0.81(3) . ?
O6W H6W2 0.80(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
N1 C1 C2 108.0(3) . . ?
N1 C1 H1 126.0 . . ?
C2 C1 H1 126.0 . . ?
C1 C2 C3 105.0(3) . . ?
C1 C2 H2 127.5 . . ?
C3 C2 H2 127.5 . . ?
N2 C3 C2 110.6(3) . . ?
N2 C3 C4 117.3(3) . . ?
C2 C3 C4 132.0(3) . . ?
N3 C4 C5 121.1(3) . . ?
N3 C4 C3 113.7(3) . . ?
C5 C4 C3 125.2(3) . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C5 C6 C7 120.9(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 117.6(3) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
N3 C8 C7 121.6(3) . . ?
N3 C8 C9 113.7(3) . . ?
C7 C8 C9 124.7(3) . . ?
N4 C9 C10 111.3(3) . . ?
N4 C9 C8 116.6(3) . . ?
C10 C9 C8 132.1(3) . . ?
C11 C10 C9 103.9(3) . . ?
C11 C10 H10 128.0 . . ?
C9 C10 H10 128.0 . . ?
N5 C11 C10 107.6(3) . . ?
N5 C11 H11 126.2 . . ?
C10 C11 H11 126.2 . . ?
N6 C12 C13 107.6(4) . . ?
N6 C12 H12 126.2 . . ?
C13 C12 H12 126.2 . . ?
C12 C13 C14 105.0(3) . . ?
C12 C13 H13 127.5 . . ?
C14 C13 H13 127.5 . . ?
N7 C14 C13 110.1(4) . . ?
N7 C14 C15 117.1(3) . . ?
C13 C14 C15 132.7(4) . . ?
N8 C15 C16 121.3(4) . . ?
N8 C15 C14 113.5(3) . . ?
C16 C15 C14 125.2(3) . . ?
C17 C16 C15 117.9(4) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
C16 C17 C18 121.4(4) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C19 117.6(4) . . ?
C17 C18 H18 121.2 . . ?
C19 C18 H18 121.2 . . ?
N8 C19 C18 121.4(3) . . ?
N8 C19 C20 113.5(3) . . ?
C18 C19 C20 125.1(3) . . ?
N9 C20 C21 110.6(3) . . ?
N9 C20 C19 116.7(3) . . ?
C21 C20 C19 132.7(3) . . ?
C22 C21 C20 105.1(3) . . ?
C22 C21 H21 127.4 . . ?
C20 C21 H21 127.4 . . ?
N10 C22 C21 108.0(3) . . ?
N10 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
O2 C23 O1 126.2(4) . . ?
O2 C23 C24 117.5(3) . . ?
O1 C23 C24 116.3(3) . . ?
C29 C24 C25 118.9(3) . . ?
C29 C24 C23 120.2(3) . . ?
C25 C24 C23 120.9(3) . . ?
C24 C25 C26 120.7(3) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C27 121.0(3) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 117.5(3) . . ?
C26 C27 C27 121.8(4) . 2_675 ?
C28 C27 C27 120.7(4) . 2_675 ?
C29 C28 C27 121.1(3) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C24 C29 C28 120.7(3) . . ?
C24 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
O3 C30 O4 122.5(4) . . ?
O3 C30 C31 119.1(4) . . ?
O4 C30 C31 118.4(4) . . ?
C36 C31 C32 118.6(4) . . ?
C36 C31 C30 120.2(4) . . ?
C32 C31 C30 121.2(4) . . ?
C33 C32 C31 120.7(4) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 120.7(4) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 118.6(3) . . ?
C33 C34 C34 121.3(3) . 2_765 ?
C35 C34 C34 120.2(3) . 2_765 ?
C34 C35 C36 120.9(4) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.6 . . ?
C31 C36 C35 120.5(4) . . ?
C31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
N3 Fe1 N8 164.94(11) . . ?
N3 Fe1 N4 74.64(11) . . ?
N8 Fe1 N4 107.17(11) . . ?
N3 Fe1 N9 120.56(11) . . ?
N8 Fe1 N9 74.46(11) . . ?
N4 Fe1 N9 93.86(11) . . ?
N3 Fe1 N7 91.17(11) . . ?
N8 Fe1 N7 73.85(12) . . ?
N4 Fe1 N7 93.58(11) . . ?
N9 Fe1 N7 148.25(11) . . ?
N3 Fe1 N2 74.06(11) . . ?
N8 Fe1 N2 103.61(11) . . ?
N4 Fe1 N2 148.63(11) . . ?
N9 Fe1 N2 100.08(11) . . ?
N7 Fe1 N2 89.18(11) . . ?
C1 N1 N2 111.2(3) . . ?
C1 N1 H1N 132(3) . . ?
N2 N1 H1N 116(3) . . ?
C3 N2 N1 105.1(3) . . ?
C3 N2 Fe1 114.6(2) . . ?
N1 N2 Fe1 140.2(3) . . ?
C8 N3 C4 120.4(3) . . ?
C8 N3 Fe1 119.0(2) . . ?
C4 N3 Fe1 120.1(2) . . ?
N5 N4 C9 105.3(3) . . ?
N5 N4 Fe1 138.8(2) . . ?
C9 N4 Fe1 115.7(2) . . ?
C11 N5 N4 111.8(3) . . ?
C11 N5 H5N 122(5) . . ?
N4 N5 H5N 126(5) . . ?
C12 N6 N7 111.8(3) . . ?
C12 N6 H6N 128(3) . . ?
N7 N6 H6N 120(3) . . ?
N6 N7 C14 105.5(3) . . ?
N6 N7 Fe1 139.0(2) . . ?
C14 N7 Fe1 115.5(2) . . ?
C19 N8 C15 120.4(3) . . ?
C19 N8 Fe1 119.7(2) . . ?
C15 N8 Fe1 119.8(3) . . ?
N10 N9 C20 105.1(3) . . ?
N10 N9 Fe1 138.9(2) . . ?
C20 N9 Fe1 115.4(2) . . ?
C22 N10 N9 111.3(3) . . ?
C22 N10 H10N 125(3) . . ?
N9 N10 H10N 123(3) . . ?
H1W1 O1W H1W2 105(4) . . ?
H2W1 O2W H2W2 100(3) . . ?
H3W1 O3W H3W2 103(4) . . ?
H4W1 O4W H4W2 101(4) . . ?
H5W1 O5W H5W1 100(4) . 2_755 ?
H6W1 O6W H6W2 106(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N O1W 0.87(2) 1.84(3) 2.713(5) 173(5) . yes
N5 H5N O1 0.89(3) 1.76(3) 2.637(4) 169(6) 1_546 yes
N6 H6N O3W 0.85(2) 1.95(3) 2.781(5) 165(5) 2_755 yes
N10 H10N O2 0.88(2) 1.81(3) 2.676(4) 166(5) 4_646 yes
O1W H1W1 O1 0.81(2) 2.03(2) 2.821(4) 167(5) 1_545 yes
O1W H1W2 O2W 0.83(2) 1.99(3) 2.814(5) 170(6) . yes
O2W H2W1 O4 0.85(2) 1.93(3) 2.779(5) 172(6) 4_646 yes
O2W H2W2 O4W 0.86(2) 1.96(3) 2.799(6) 169(5) 4_646 yes
O3W H3W1 O4 0.84(2) 1.80(3) 2.626(5) 167(4) 2_765 yes
O3W H3W2 O6W 0.84(3) 1.77(4) 2.564(10) 156(6) . yes
O4W H4W1 O3 0.83(3) 1.93(3) 2.736(6) 163(7) 1_556 yes
O4W H4W2 O5W 0.87(2) 2.18(4) 2.934(5) 146(6) 1_565 yes
O5W H5W1 O3W 0.85(2) 2.00(3) 2.840(6) 168(4) . yes
O6W H6W1 O3 0.81(3) 1.77(5) 2.550(9) 160(10) 1_545 yes
O6W H6W2 O3 0.80(3) 2.18(7) 2.849(7) 141(11) 2_765 yes

_refine_diff_density_max         0.931
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.066

